Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2002 data_global #============================================================================== _audit_creation_date '2001-06-23' _audit_creation_method 'by teXsan for Windows v1.06' _audit_update_record ; ? ; #============================================================================== _journal_coden_Cambridge 186 loop_ _publ_author_name 'Zhang, Shi-Wei' 'Liu, Guang' 'Tang, You-Qi' _publ_contact_author_name 'Prof Shi-Wei Zhang' _publ_contact_author_address ; College of Chemistry and Molecular Engineering Peking University Beijing CHINA ; _publ_requested_coeditor_name ? _publ_contact_author_phone ' (8610)62751492 ' _publ_contact_author_fax ' (8610)62751725 ' _publ_contact_author_email ' zsw@chem.pku.edu.cn ' # SUBMISSION DETAILS _publ_requested_journal ' J. Chem. Soc., Dalton Trans.' _publ_requested_category ' CHOOSE FI FM FO CI CM CO or AD' _publ_section_title ; Synthesis and characterization of a novel ring-like decamolybdate ; _publ_section_title_footnote ; Paper Ref.: B108997H ; _publ_section_references ; ENTER OTHER REFERENCES Molecular Structure Corporation. (1997-1999). teXsan for Windows. Single Crystal Structure Analysis Software. Version 1.06. MSC, 9009 New Trails Drive, The Woodlands, TX 77381, USA. ; data_Mo10Y2-1_ _database_code_CSD 166172 #============================================================================== _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan for Windows version 1.06 (MSC, 1997-1999)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'teXsan for Windows version 1.06 (MSC, 1997-1999)' #------------------------------------------------------------------------------ _cell_length_a 24.345(5) _cell_length_b 16.580(3) _cell_length_c 15.355(3) _cell_angle_alpha 90.00 _cell_angle_beta 101.16(3) _cell_angle_gamma 90.00 _cell_volume 6081(2) _cell_formula_units_Z 4 _cell_measurement_temperature 173 _cell_measurement_reflns_used 34563 _cell_measurement_theta_min 1.5 _cell_measurement_theta_max 27.5 #------------------------------------------------------------------------------ _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c ' _symmetry_Int_Tables_number 15 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' ' -x, +y,1/2-z' ' -x, -y, -z' ' +x, -y,1/2+z' '1/2+x,1/2+y, +z' '1/2-x,1/2+y,1/2-z' '1/2-x,1/2-y, -z' '1/2+x,1/2-y,1/2+z' #------------------------------------------------------------------------------ _publ_section_exptl_prep ; ENTER EXPERIMENTAL SECTION ; _exptl_crystal_description 'chip' _exptl_crystal_colour 'red' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_diffrn 2.580 _exptl_crystal_density_meas 'not measured' _chemical_formula_weight 2361.88 _chemical_formula_analytical ? _chemical_formula_sum 'C8 H72 Mo10 O66 Y2 ' _chemical_formula_moiety 'C8 H72 Mo10 O66 Y2 ' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 4584 _exptl_absorpt_coefficient_mu 4.005 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_max 1.222 _exptl_absorpt_correction_T_min 0.643 _exptl_special_details ; ? ; #============================================================================== # EXPERIMENTAL DATA _diffrn_special_details ; ? ; _diffrn_ambient_temperature 173.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Rigaku rotating anode' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'Imaging Plate' _diffrn_measurement_device 'Rigaku RAXIS-RAPID' _diffrn_detector_area_resol_mean ? _diffrn_measurement_method ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_decay_% 0.00 loop_ _diffrn_standard_refln_index_h ? _diffrn_standard_refln_index_k ? _diffrn_standard_refln_index_l ? _diffrn_reflns_number 6943 _reflns_number_total 6943 _reflns_number_gt 5052 _reflns_threshold_expression I>2.00\s(I) _diffrn_reflns_av_R_equivalents 0.0504 _diffrn_reflns_av_sigmaI/netI 0.0673 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_max 0.481 _diffrn_measured_fraction_theta_full 0.481 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 31 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.50 _diffrn_reflns_theta_max 27.48 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 0.03012 _diffrn_orient_matrix_UB_12 -0.00666 _diffrn_orient_matrix_UB_13 -0.03541 _diffrn_orient_matrix_UB_21 -0.02627 _diffrn_orient_matrix_UB_22 -0.03177 _diffrn_orient_matrix_UB_23 -0.04542 _diffrn_orient_matrix_UB_31 -0.01247 _diffrn_orient_matrix_UB_32 0.05084 _diffrn_orient_matrix_UB_33 -0.03302 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Mo 0 40 -1.825 0.688 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Y 0 8 -2.951 3.542 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; O 0 320 0.008 0.006 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; H 0 160 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; C 0 32 0.002 0.002 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; N 0 16 0.004 0.003 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mo1 Mo 0.246935(19) 0.17596(3) 0.07522(3) 0.01249(10) Uani 1 d . . . Mo2 Mo 0.366297(19) 0.42552(3) 0.01630(3) 0.01424(10) Uani 1 d . . . Mo3 Mo 0.27608(2) 0.01200(3) -0.03011(3) 0.01436(11) Uani 1 d . . . Mo4 Mo 0.41288(2) 0.25434(3) -0.04459(3) 0.01488(11) Uani 1 d . . . Mo5 Mo 0.392833(19) 0.11247(3) 0.01136(3) 0.01450(11) Uani 1 d . . . Y1 Y 0.19370(2) 0.14950(3) -0.22191(3) 0.01434(12) Uani 1 d . . . O1 O 0.38869(15) 0.5246(2) 0.0182(2) 0.0179(8) Uani 1 d . . . O2 O 0.34978(15) 0.0099(2) -0.0384(2) 0.0169(8) Uani 1 d . . . O3 O 0.31221(15) -0.0117(2) 0.1182(2) 0.0158(8) Uani 1 d . . . O4 O 0.37133(15) 0.1628(2) -0.1046(2) 0.0170(8) Uani 1 d . . . O5 O 0.25746(15) 0.1455(2) 0.1818(2) 0.0177(8) Uani 1 d . . . O6 O 0.16853(15) 0.1878(2) 0.0406(2) 0.0139(7) Uani 1 d . . . O7 O 0.47903(16) 0.2409(2) -0.0601(2) 0.0216(9) Uani 1 d . . . O8 O 0.41083(15) 0.2144(2) 0.0730(2) 0.0159(8) Uani 1 d . . . O9 O 0.35977(15) 0.4059(2) 0.1247(2) 0.0166(8) Uani 1 d . . . O10 O 0.45574(16) 0.0693(2) 0.0124(2) 0.0204(8) Uani 1 d . . . O11 O 0.30500(15) 0.1282(2) 0.0268(2) 0.0147(8) Uani 1 d . . . O12 O 0.26937(14) 0.2780(2) 0.0865(2) 0.0127(7) Uani 1 d . . . O13 O 0.39187(15) 0.3151(2) -0.1701(2) 0.0183(8) Uani 1 d . . . O14 O 0.39105(15) 0.0626(2) 0.1397(2) 0.0169(8) Uani 1 d . . . O15 O 0.43045(14) 0.3691(2) 0.0105(2) 0.0140(7) Uani 1 d . . . O16 O 0.25914(16) -0.0892(2) -0.0316(2) 0.0200(8) Uani 1 d . . . O17 O 0.28492(15) 0.4425(2) -0.0264(2) 0.0146(8) Uani 1 d . . . O18 O 0.24518(16) 0.0482(2) -0.1346(2) 0.0172(8) Uani 1 d . . . O19 O 0.36268(16) 0.4368(2) -0.1339(2) 0.0185(8) Uani 1 d . . . C1 C 0.3537(2) 0.0211(3) 0.1672(3) 0.0173(11) Uani 1 d . . . C2 C 0.3595(2) 0.0122(4) 0.2664(3) 0.0232(13) Uani 1 d . . . H2A H 0.3926 0.0399 0.2957 0.035 Uiso 1 calc R . . H2B H 0.3624 -0.0439 0.2819 0.035 Uiso 1 calc R . . H2C H 0.3274 0.0351 0.2847 0.035 Uiso 1 calc R . . C3 C 0.3716(2) 0.3844(3) -0.1894(3) 0.0175(11) Uani 1 d . . . C4 C 0.3577(3) 0.4069(4) -0.2864(3) 0.0330(16) Uani 1 d . . . H4A H 0.3428 0.4606 -0.2924 0.049 Uiso 1 calc R . . H4B H 0.3305 0.3698 -0.3175 0.049 Uiso 1 calc R . . H4C H 0.3911 0.4045 -0.3109 0.049 Uiso 1 calc R . . OW1 O 0.21821(16) 0.0565(2) -0.3233(2) 0.0190(8) Uani 1 d . . . OW2 O 0.11286(16) 0.1006(2) -0.3193(2) 0.0228(9) Uani 1 d . . . OW3 O 0.12776(16) 0.2485(2) -0.2153(2) 0.0207(9) Uani 1 d . . . OW4 O 0.28425(16) 0.1842(2) -0.2331(2) 0.0193(8) Uani 1 d . . . OW5 O 0.18949(17) 0.2375(2) -0.3473(2) 0.0242(9) Uani 1 d . . . OW6 O 0.01024(17) 0.1643(3) -0.3347(3) 0.0278(9) Uani 1 d . . . OW7 O 0.05262(18) 0.3158(3) -0.3517(3) 0.0346(11) Uani 1 d . . . OW8 O 0.5000 0.0811(4) 0.2500 0.0410(17) Uani 1 d S . . OW9 O 0.3219(4) 0.1955(6) -0.3921(7) 0.024(2) Uani 0.67 d P . . OW10 O 0.3012(13) 0.2148(15) -0.4068(16) 0.067(10) Uani 0.33 d P . . OW11 O 0.5025(3) 0.4224(5) -0.1113(5) 0.0257(17) Uani 0.67 d P . . OW12 O 0.4948(10) 0.4487(13) -0.0973(15) 0.057(7) Uiso 0.33 d P . . OW13 O 0.5000 0.3083(5) -0.2500 0.065(2) Uani 1 d S . . OW14 O 0.4213(3) -0.1183(3) 0.0071(3) 0.071(2) Uani 1 d . . . OW15 O 0.4237(8) 0.1654(11) -0.2645(9) 0.041(4) Uani 0.50 d P . . OW16 O 0.4290(8) 0.1657(11) -0.3047(9) 0.047(4) Uani 0.50 d P . . OW17 O 0.1693(4) 0.1740(5) -0.5058(5) 0.031(2) Uani 0.50 d P . . OW18 O 0.3862(5) 0.2998(6) -0.4892(6) 0.057(3) Uani 0.50 d P . . OW19 O 0.4993(5) -0.0725(7) 0.1549(8) 0.179(5) Uani 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mo1 0.0150(2) 0.0108(2) 0.0104(2) -0.00048(16) -0.00072(16) 0.00115(18) Mo2 0.0157(2) 0.0131(2) 0.0125(2) 0.00052(17) -0.00086(17) -0.00021(19) Mo3 0.0189(2) 0.0114(2) 0.0115(2) -0.00029(16) -0.00047(17) 0.00259(19) Mo4 0.0165(2) 0.0147(2) 0.0123(2) 0.00160(17) 0.00007(17) 0.00238(19) Mo5 0.0168(2) 0.0141(2) 0.0116(2) 0.00086(17) 0.00007(17) 0.00293(19) Y1 0.0177(3) 0.0136(3) 0.0105(2) -0.00056(19) -0.00034(19) 0.0017(2) O1 0.017(2) 0.0144(19) 0.0212(19) 0.0020(15) 0.0004(15) -0.0047(16) O2 0.020(2) 0.0135(19) 0.0166(18) -0.0017(14) 0.0011(15) 0.0032(16) O3 0.0151(19) 0.0158(19) 0.0141(17) -0.0005(14) -0.0034(14) 0.0012(16) O4 0.019(2) 0.0157(19) 0.0150(17) -0.0024(14) -0.0009(14) 0.0035(16) O5 0.016(2) 0.021(2) 0.0155(18) 0.0002(15) 0.0017(14) -0.0009(16) O6 0.0167(19) 0.0110(18) 0.0136(17) 0.0017(13) 0.0022(14) 0.0016(15) O7 0.025(2) 0.019(2) 0.0201(19) 0.0021(15) 0.0026(16) 0.0081(18) O8 0.016(2) 0.0165(19) 0.0127(17) 0.0013(14) -0.0020(14) 0.0014(16) O9 0.016(2) 0.019(2) 0.0122(17) 0.0014(14) -0.0022(14) 0.0008(16) O10 0.020(2) 0.017(2) 0.0231(19) 0.0016(15) 0.0024(16) 0.0044(17) O11 0.016(2) 0.0141(18) 0.0128(17) -0.0003(14) 0.0002(14) -0.0010(15) O12 0.0139(19) 0.0096(17) 0.0130(16) -0.0011(13) -0.0014(14) 0.0023(15) O13 0.021(2) 0.019(2) 0.0147(17) 0.0016(15) 0.0023(15) 0.0047(17) O14 0.017(2) 0.0179(19) 0.0139(17) 0.0031(14) -0.0007(15) -0.0006(16) O15 0.0117(18) 0.0143(19) 0.0150(17) -0.0010(14) -0.0003(14) -0.0009(15) O16 0.030(2) 0.0115(19) 0.0172(18) -0.0018(14) 0.0006(16) -0.0018(17) O17 0.018(2) 0.0133(18) 0.0109(16) 0.0000(14) -0.0013(14) 0.0036(15) O18 0.023(2) 0.0136(19) 0.0145(18) 0.0009(14) 0.0009(15) 0.0056(16) O19 0.025(2) 0.0157(19) 0.0145(18) 0.0023(15) 0.0029(15) 0.0034(17) C1 0.022(3) 0.014(3) 0.016(3) 0.003(2) 0.002(2) 0.010(2) C2 0.026(3) 0.029(3) 0.013(3) 0.002(2) -0.001(2) -0.001(3) C3 0.017(3) 0.019(3) 0.016(3) 0.004(2) 0.001(2) -0.001(2) C4 0.057(5) 0.030(4) 0.012(3) 0.004(2) 0.007(3) 0.013(3) OW1 0.022(2) 0.018(2) 0.0157(18) -0.0060(15) 0.0010(15) 0.0014(16) OW2 0.023(2) 0.024(2) 0.0192(19) -0.0071(16) -0.0023(16) 0.0014(18) OW3 0.024(2) 0.021(2) 0.0157(18) -0.0001(15) 0.0002(16) 0.0093(18) OW4 0.022(2) 0.019(2) 0.0159(18) -0.0010(15) 0.0024(15) 0.0002(17) OW5 0.030(2) 0.024(2) 0.0182(19) 0.0100(16) 0.0025(16) 0.0050(19) OW6 0.022(2) 0.032(2) 0.026(2) -0.0034(18) -0.0017(17) 0.0014(19) OW7 0.023(2) 0.036(3) 0.040(2) 0.007(2) -0.0054(19) 0.001(2) OW8 0.046(4) 0.038(4) 0.034(4) 0.000 -0.005(3) 0.000 OW9 0.033(5) 0.019(5) 0.018(5) 0.002(3) 0.002(3) 0.002(4) OW10 0.16(3) 0.027(12) 0.012(9) -0.001(8) -0.002(14) 0.009(15) OW11 0.034(4) 0.019(4) 0.028(4) -0.013(3) 0.017(3) -0.009(3) OW13 0.054(5) 0.074(6) 0.071(5) 0.000 0.023(4) 0.000 OW14 0.118(6) 0.039(3) 0.051(3) -0.005(3) 0.001(3) 0.045(4) OW15 0.038(7) 0.039(7) 0.048(9) -0.021(8) 0.010(8) 0.003(5) OW16 0.051(9) 0.029(6) 0.054(10) -0.002(8) -0.005(8) 0.003(6) OW17 0.055(6) 0.022(5) 0.017(4) -0.007(3) 0.009(4) -0.005(4) OW18 0.096(10) 0.044(6) 0.026(5) 0.002(4) 0.002(5) -0.023(7) OW19 0.165(11) 0.180(11) 0.208(11) -0.017(9) 0.075(9) -0.021(9) #============================================================================== # REFINEMENT DATA _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^)+(0.0400P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6943 _refine_ls_number_parameters 420 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0552 _refine_ls_R_factor_gt 0.0350 _refine_ls_wR_factor_ref 0.0816 _refine_ls_wR_factor_gt 0.0772 _refine_ls_goodness_of_fit_ref 0.953 _refine_ls_restrained_S_all 0.953 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 1.165 _refine_diff_density_min -0.942 _refine_diff_density_rms 0.175 #============================================================================== # MOLECULAR GEOMETRY _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 O5 1.685(3) . ? Mo1 O12 1.777(3) . ? Mo1 O6 1.890(4) . ? Mo1 O11 1.893(4) . ? Mo1 O17 2.190(3) 7 ? Mo2 O1 1.729(4) . ? Mo2 O9 1.733(3) . ? Mo2 O15 1.838(4) . ? Mo2 O17 1.983(4) . ? Mo2 O6 2.173(3) 7 ? Mo2 O19 2.299(3) . ? Mo3 O16 1.728(4) . ? Mo3 O18 1.741(3) . ? Mo3 O2 1.823(4) . ? Mo3 O17 2.007(4) 7 ? Mo3 O11 2.176(3) . ? Mo3 O3 2.311(3) . ? Mo4 O7 1.688(4) . ? Mo4 O8 1.934(3) . ? Mo4 O4 1.953(4) . ? Mo4 O15 2.092(3) . ? Mo4 O13 2.146(3) . ? Mo4 O6 2.214(3) 7 ? Mo4 Mo5 2.5829(8) . ? Mo5 O10 1.688(4) . ? Mo5 O4 1.944(3) . ? Mo5 O8 1.945(4) . ? Mo5 O2 2.065(4) . ? Mo5 O14 2.146(3) . ? Mo5 O11 2.212(4) . ? Y1 OW3 2.311(4) . ? Y1 OW4 2.317(4) . ? Y1 O9 2.349(4) 7 ? Y1 OW1 2.349(4) . ? Y1 O18 2.354(3) . ? Y1 OW2 2.372(4) . ? Y1 OW5 2.401(4) . ? Y1 O12 2.419(3) 7 ? O3 C1 1.261(6) . ? O6 Mo2 2.173(3) 7 ? O6 Mo4 2.214(3) 7 ? O9 Y1 2.349(4) 7 ? O12 Y1 2.419(3) 7 ? O13 C3 1.263(6) . ? O14 C1 1.276(6) . ? O17 Mo3 2.007(4) 7 ? O17 Mo1 2.190(3) 7 ? O19 C3 1.265(6) . ? C1 C2 1.509(7) . ? C3 C4 1.508(7) . ? OW9 OW10 0.60(2) . ? OW11 OW12 0.53(2) . ? OW15 OW16 0.655(15) . ? OW17 OW18 1.407(15) 7_554 ? OW18 OW17 1.407(15) 7_554 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O5 Mo1 O12 101.83(16) . . ? O5 Mo1 O6 105.08(16) . . ? O12 Mo1 O6 101.73(15) . . ? O5 Mo1 O11 105.76(16) . . ? O12 Mo1 O11 101.39(15) . . ? O6 Mo1 O11 136.29(14) . . ? O5 Mo1 O17 92.34(15) . 7 ? O12 Mo1 O17 165.83(13) . 7 ? O6 Mo1 O17 74.05(14) . 7 ? O11 Mo1 O17 74.49(14) . 7 ? O1 Mo2 O9 104.41(17) . . ? O1 Mo2 O15 102.51(17) . . ? O9 Mo2 O15 100.82(16) . . ? O1 Mo2 O17 99.34(16) . . ? O9 Mo2 O17 94.19(15) . . ? O15 Mo2 O17 149.36(14) . . ? O1 Mo2 O6 157.71(14) . 7 ? O9 Mo2 O6 97.03(15) . 7 ? O15 Mo2 O6 79.01(14) . 7 ? O17 Mo2 O6 72.71(13) . 7 ? O1 Mo2 O19 83.72(15) . . ? O9 Mo2 O19 170.43(15) . . ? O15 Mo2 O19 82.00(14) . . ? O17 Mo2 O19 79.31(14) . . ? O6 Mo2 O19 74.42(12) 7 . ? O16 Mo3 O18 105.26(16) . . ? O16 Mo3 O2 102.48(17) . . ? O18 Mo3 O2 101.42(17) . . ? O16 Mo3 O17 100.14(16) . 7 ? O18 Mo3 O17 92.58(15) . 7 ? O2 Mo3 O17 149.08(15) . 7 ? O16 Mo3 O11 157.47(14) . . ? O18 Mo3 O11 96.50(15) . . ? O2 Mo3 O11 78.39(15) . . ? O17 Mo3 O11 72.69(13) 7 . ? O16 Mo3 O3 83.79(14) . . ? O18 Mo3 O3 168.74(15) . . ? O2 Mo3 O3 82.73(14) . . ? O17 Mo3 O3 79.04(13) 7 . ? O11 Mo3 O3 73.93(12) . . ? O7 Mo4 O8 106.51(16) . . ? O7 Mo4 O4 104.60(17) . . ? O8 Mo4 O4 94.00(15) . . ? O7 Mo4 O15 92.94(16) . . ? O8 Mo4 O15 88.52(14) . . ? O4 Mo4 O15 160.71(14) . . ? O7 Mo4 O13 90.21(16) . . ? O8 Mo4 O13 162.66(15) . . ? O4 Mo4 O13 85.96(14) . . ? O15 Mo4 O13 86.03(13) . . ? O7 Mo4 O6 160.95(16) . 7 ? O8 Mo4 O6 86.40(14) . 7 ? O4 Mo4 O6 88.00(14) . 7 ? O15 Mo4 O6 73.06(13) . 7 ? O13 Mo4 O6 76.26(13) . 7 ? O7 Mo4 Mo5 99.99(13) . . ? O8 Mo4 Mo5 48.43(10) . . ? O4 Mo4 Mo5 48.35(10) . . ? O15 Mo4 Mo5 136.93(9) . . ? O13 Mo4 Mo5 134.30(10) . . ? O6 Mo4 Mo5 99.06(9) 7 . ? O10 Mo5 O4 105.90(16) . . ? O10 Mo5 O8 104.19(17) . . ? O4 Mo5 O8 93.91(14) . . ? O10 Mo5 O2 92.81(17) . . ? O4 Mo5 O2 89.28(14) . . ? O8 Mo5 O2 161.07(15) . . ? O10 Mo5 O14 90.42(16) . . ? O4 Mo5 O14 163.13(15) . . ? O8 Mo5 O14 86.01(14) . . ? O2 Mo5 O14 85.60(14) . . ? O10 Mo5 O11 160.61(16) . . ? O4 Mo5 O11 87.30(14) . . ? O8 Mo5 O11 88.66(14) . . ? O2 Mo5 O11 72.84(14) . . ? O14 Mo5 O11 75.84(13) . . ? O10 Mo5 Mo4 99.20(13) . . ? O4 Mo5 Mo4 48.63(11) . . ? O8 Mo5 Mo4 48.06(10) . . ? O2 Mo5 Mo4 137.90(10) . . ? O14 Mo5 Mo4 134.06(10) . . ? O11 Mo5 Mo4 100.19(9) . . ? OW3 Y1 OW4 120.37(13) . . ? OW3 Y1 O9 76.99(13) . 7 ? OW4 Y1 O9 142.82(12) . 7 ? OW3 Y1 OW1 139.69(13) . . ? OW4 Y1 OW1 75.31(13) . . ? O9 Y1 OW1 114.06(13) 7 . ? OW3 Y1 O18 141.21(13) . . ? OW4 Y1 O18 79.08(13) . . ? O9 Y1 O18 70.02(13) 7 . ? OW1 Y1 O18 74.57(12) . . ? OW3 Y1 OW2 76.79(13) . . ? OW4 Y1 OW2 136.33(13) . . ? O9 Y1 OW2 76.86(12) 7 . ? OW1 Y1 OW2 69.15(13) . . ? O18 Y1 OW2 113.62(13) . . ? OW3 Y1 OW5 71.44(13) . . ? OW4 Y1 OW5 71.51(13) . . ? O9 Y1 OW5 143.51(13) 7 . ? OW1 Y1 OW5 81.02(13) . . ? O18 Y1 OW5 145.64(14) . . ? OW2 Y1 OW5 78.50(14) . . ? OW3 Y1 O12 75.85(12) . 7 ? OW4 Y1 O12 74.93(12) . 7 ? O9 Y1 O12 78.89(12) 7 7 ? OW1 Y1 O12 142.76(12) . 7 ? O18 Y1 O12 78.25(11) . 7 ? OW2 Y1 O12 146.76(13) . 7 ? OW5 Y1 O12 109.80(12) . 7 ? Mo3 O2 Mo5 113.21(17) . . ? C1 O3 Mo3 128.6(3) . . ? Mo5 O4 Mo4 83.02(13) . . ? Mo1 O6 Mo2 108.52(16) . 7 ? Mo1 O6 Mo4 153.90(18) . 7 ? Mo2 O6 Mo4 95.98(14) 7 7 ? Mo4 O8 Mo5 83.51(13) . . ? Mo2 O9 Y1 148.07(19) . 7 ? Mo1 O11 Mo3 108.64(16) . . ? Mo1 O11 Mo5 154.45(18) . . ? Mo3 O11 Mo5 95.55(14) . . ? Mo1 O12 Y1 127.79(16) . 7 ? C3 O13 Mo4 130.7(3) . . ? C1 O14 Mo5 130.9(3) . . ? Mo2 O15 Mo4 111.94(16) . . ? Mo2 O17 Mo3 133.30(17) . 7 ? Mo2 O17 Mo1 104.52(15) . 7 ? Mo3 O17 Mo1 104.03(16) 7 7 ? Mo3 O18 Y1 149.13(19) . . ? C3 O19 Mo2 129.9(3) . . ? O3 C1 O14 125.1(5) . . ? O3 C1 C2 118.0(5) . . ? O14 C1 C2 116.9(5) . . ? O13 C3 O19 125.2(5) . . ? O13 C3 C4 117.4(5) . . ? O19 C3 C4 117.4(5) . . ? #============================================================================== data_Mo10Y2-2_ _database_code_CSD 166173 #============================================================================== _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan for Windows version 1.06 (MSC, 1997-1999)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'teXsan for Windows version 1.06 (MSC, 1997-1999)' #------------------------------------------------------------------------------ _cell_length_a 10.950(2) _cell_length_b 22.531(5) _cell_length_c 13.043(3) _cell_angle_alpha 90.00 _cell_angle_beta 114.79(3) _cell_angle_gamma 90.00 _cell_volume 2921.4(11) _cell_formula_units_Z 2 _cell_measurement_temperature 173 _cell_measurement_reflns_used 17901 _cell_measurement_theta_min 2.2 _cell_measurement_theta_max 27.5 #------------------------------------------------------------------------------ _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_Int_Tables_number 14 _symmetry_space_group_name_Hall ? 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' #------------------------------------------------------------------------------ _publ_section_exptl_prep ; ENTER EXPERIMENTAL SECTION ; _exptl_crystal_description 'needle' _exptl_crystal_colour 'red' _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_diffrn 2.685 _exptl_crystal_density_meas 'not measured' _chemical_formula_weight 2361.88 _chemical_formula_analytical ? _chemical_formula_sum 'C8 H72 Mo10 O66 Y2' _chemical_formula_moiety 'C8 H72 Mo10 O66 Y2' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 2292 _exptl_absorpt_coefficient_mu 4.168 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_max 1.258 _exptl_absorpt_correction_T_min 0.845 _exptl_special_details ; ? ; #============================================================================== # EXPERIMENTAL DATA _diffrn_special_details ; ? ; _diffrn_ambient_temperature 173.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Rigaku rotating anode' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'Imaging Plate' _diffrn_measurement_device 'Rigaku RAXIS-RAPID' _diffrn_detector_area_resol_mean ? _diffrn_measurement_method ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_decay_% 0.00 loop_ _diffrn_standard_refln_index_h ? _diffrn_standard_refln_index_k ? _diffrn_standard_refln_index_l ? _diffrn_reflns_number 12088 _reflns_number_total 6587 _reflns_number_gt 4254 _reflns_threshold_expression I>2.00\s(I) _diffrn_reflns_av_R_equivalents 0.0610 _diffrn_reflns_av_sigmaI/netI 0.1183 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_max 0.960 _diffrn_measured_fraction_theta_full 0.960 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 0.90 _diffrn_reflns_theta_max 27.48 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 -0.04355 _diffrn_orient_matrix_UB_12 0.03464 _diffrn_orient_matrix_UB_13 -0.05391 _diffrn_orient_matrix_UB_21 0.00297 _diffrn_orient_matrix_UB_22 -0.01738 _diffrn_orient_matrix_UB_23 -0.08249 _diffrn_orient_matrix_UB_31 -0.07229 _diffrn_orient_matrix_UB_32 -0.02163 _diffrn_orient_matrix_UB_33 -0.02019 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C 0 81 0.002 0.002 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; H 0 117 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; O 0 45 0.008 0.006 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; Mo 0 9 -1.825 0.688 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Y 0 9 -2.951 3.542 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mo1 Mo 0.97396(7) 0.02535(4) 0.61546(7) 0.0142(2) Uani 1 d . . . Mo2 Mo 0.76523(8) -0.11565(4) 0.26108(7) 0.0153(2) Uani 1 d . . . Mo3 Mo 0.89888(8) 0.16647(4) 0.54986(7) 0.0150(2) Uani 1 d . . . Mo4 Mo 0.63832(8) 0.01705(4) 0.22328(7) 0.0152(2) Uani 1 d . . . Mo5 Mo 0.64379(8) 0.09197(4) 0.37452(7) 0.0145(2) Uani 1 d . . . Y1 Y 1.15987(9) 0.13459(4) 0.41876(8) 0.0165(2) Uani 1 d . . . O1 O 0.7344(6) -0.1792(3) 0.1805(6) 0.0201(15) Uani 1 d . . . O2 O 0.7294(7) 0.1736(3) 0.4334(6) 0.0211(15) Uani 1 d . . . O3 O 0.7779(6) 0.1418(3) 0.6508(6) 0.0223(16) Uani 1 d . . . O4 O 0.7269(6) 0.0943(3) 0.2688(6) 0.0213(15) Uani 1 d . . . O5 O 0.9213(6) 0.0152(3) 0.7192(6) 0.0211(15) Uani 1 d . . . O6 O 1.1627(6) 0.0255(3) 0.6859(5) 0.0145(13) Uani 1 d . . . O7 O 0.4846(6) 0.0340(3) 0.1240(6) 0.0213(16) Uani 1 d . . . O8 O 0.6190(6) 0.0075(3) 0.3643(5) 0.0162(14) Uani 1 d . . . O9 O 0.7555(6) -0.1384(3) 0.3861(6) 0.0214(16) Uani 1 d . . . O10 O 0.4867(6) 0.1204(3) 0.3051(6) 0.0199(15) Uani 1 d . . . O11 O 0.8435(6) 0.0749(3) 0.5082(5) 0.0158(14) Uani 1 d . . . O12 O 0.9391(6) -0.0439(3) 0.5451(5) 0.0150(14) Uani 1 d . . . O13 O 0.7250(6) 0.0173(3) 0.1040(6) 0.0205(15) Uani 1 d . . . O14 O 0.6059(6) 0.0880(3) 0.5240(5) 0.0177(14) Uani 1 d . . . O15 O 0.6104(6) -0.0728(3) 0.1945(6) 0.0189(15) Uani 1 d . . . O16 O 0.9156(6) 0.2328(3) 0.6195(6) 0.0190(15) Uani 1 d . . . O17 O 0.9666(6) -0.1181(3) 0.3282(6) 0.0197(15) Uani 1 d . . . O18 O 1.0001(6) 0.1746(3) 0.4764(6) 0.0195(15) Uani 1 d . . . O19 O 0.8063(6) -0.0748(3) 0.1159(6) 0.0198(15) Uani 1 d . . . C1 C 0.6758(10) 0.1092(5) 0.6231(9) 0.022(2) Uani 1 d . . . C2 C 0.6233(11) 0.0945(5) 0.7101(10) 0.031(3) Uani 1 d . . . H2A H 0.5456 0.0694 0.6768 0.080 Uiso 1 calc R . . H2B H 0.5991 0.1305 0.7365 0.080 Uiso 1 calc R . . H2C H 0.6918 0.0742 0.7725 0.080 Uiso 1 calc R . . C3 C 0.7804(9) -0.0235(5) 0.0733(8) 0.022(2) Uani 1 d . . . C4 C 0.8284(11) -0.0079(5) -0.0162(9) 0.027(2) Uani 1 d . . . H4A H 0.8682 -0.0422 -0.0334 0.080 Uiso 1 calc R . . H4B H 0.8940 0.0233 0.0111 0.080 Uiso 1 calc R . . H4C H 0.7535 0.0052 -0.0831 0.080 Uiso 1 calc R . . OW1 O 1.1082(7) 0.2319(3) 0.3440(8) 0.036(2) Uani 1 d . . . OW2 O 1.3619(7) 0.1896(3) 0.4880(6) 0.0272(17) Uani 1 d . . . OW3 O 1.3287(6) 0.0623(3) 0.4604(6) 0.0195(15) Uani 1 d . . . OW4 O 0.9595(7) 0.1177(3) 0.2583(6) 0.0218(16) Uani 1 d . . . OW5 O 1.2189(7) 0.1349(4) 0.2641(6) 0.0284(18) Uani 1 d . . . OW6 O 0.5310(7) 0.2514(3) 0.4181(6) 0.0250(17) Uani 1 d . . . OW7 O 0.9777(8) 0.1453(4) 0.8773(7) 0.038(2) Uani 1 d . . . OW8 O 1.5928(10) 0.1296(4) 0.9892(9) 0.059(3) Uani 1 d . . . OW9 O 1.4755(12) 0.2440(4) 0.6895(7) 0.062(3) Uani 1 d . . . OW10 O 1.1674(12) 0.2070(6) 0.0788(12) 0.088(4) Uani 1 d . . . OW11 O 0.7251(13) 0.2715(5) 0.7174(11) 0.082(4) Uani 1 d . . . OW12 O 0.8637(11) 0.1485(6) 1.0330(10) 0.068(3) Uani 1 d . . . OW13 O 1.422(2) 0.3417(10) 0.5708(19) 0.064(6) Uiso 0.50 d P . . OW14 O 1.330(3) 0.3469(11) 0.567(2) 0.072(7) Uiso 0.50 d P . . OW15 O 0.993(3) 0.1600(16) 1.084(2) 0.256(17) Uani 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mo1 0.0080(4) 0.0110(4) 0.0196(4) 0.0001(3) 0.0018(3) 0.0002(3) Mo2 0.0087(4) 0.0125(4) 0.0201(4) -0.0023(3) 0.0017(3) -0.0011(3) Mo3 0.0090(4) 0.0106(4) 0.0211(4) -0.0004(3) 0.0022(3) -0.0001(3) Mo4 0.0088(4) 0.0128(4) 0.0195(4) -0.0007(3) 0.0014(3) -0.0005(3) Mo5 0.0082(4) 0.0107(4) 0.0203(4) -0.0005(3) 0.0017(3) 0.0002(3) Y1 0.0099(4) 0.0141(5) 0.0225(5) 0.0013(4) 0.0040(4) -0.0005(4) O1 0.015(3) 0.013(4) 0.030(4) -0.008(3) 0.007(3) -0.002(3) O2 0.021(3) 0.012(4) 0.029(4) 0.002(3) 0.009(3) 0.003(3) O3 0.012(3) 0.017(4) 0.030(4) -0.005(3) 0.002(3) -0.007(3) O4 0.012(3) 0.020(4) 0.028(4) -0.007(3) 0.004(3) 0.001(3) O5 0.016(3) 0.014(4) 0.026(4) -0.002(3) 0.002(3) -0.003(3) O6 0.012(3) 0.007(3) 0.019(3) -0.001(3) 0.002(3) -0.002(2) O7 0.015(3) 0.024(4) 0.019(4) -0.006(3) 0.002(3) 0.002(3) O8 0.013(3) 0.017(4) 0.018(3) 0.000(3) 0.006(3) -0.003(3) O9 0.006(3) 0.020(4) 0.028(4) 0.006(3) -0.003(3) 0.003(3) O10 0.010(3) 0.020(4) 0.025(4) -0.004(3) 0.002(3) 0.000(3) O11 0.019(3) 0.006(3) 0.021(3) -0.002(3) 0.007(3) -0.001(3) O12 0.007(3) 0.016(3) 0.016(3) 0.001(3) -0.001(3) 0.000(3) O13 0.015(3) 0.016(4) 0.024(4) 0.003(3) 0.003(3) 0.002(3) O14 0.010(3) 0.022(4) 0.019(3) -0.001(3) 0.004(3) -0.002(3) O15 0.012(3) 0.016(4) 0.027(4) -0.004(3) 0.006(3) -0.003(3) O16 0.013(3) 0.012(3) 0.026(4) -0.001(3) 0.001(3) 0.002(3) O17 0.011(3) 0.016(4) 0.027(4) -0.001(3) 0.003(3) -0.001(3) O18 0.009(3) 0.019(4) 0.025(4) 0.000(3) 0.002(3) 0.001(3) O19 0.014(3) 0.023(4) 0.021(4) 0.001(3) 0.006(3) 0.002(3) C1 0.018(5) 0.023(6) 0.027(5) -0.003(5) 0.012(5) 0.005(4) C2 0.022(5) 0.036(7) 0.033(6) -0.003(5) 0.009(5) -0.006(5) C3 0.012(4) 0.029(6) 0.019(5) -0.001(4) 0.002(4) -0.005(4) C4 0.025(6) 0.032(7) 0.021(5) 0.005(5) 0.005(5) 0.003(5) OW1 0.017(4) 0.021(4) 0.067(6) 0.018(4) 0.014(4) 0.003(3) OW2 0.016(3) 0.032(4) 0.030(4) -0.005(3) 0.006(3) -0.011(3) OW3 0.011(3) 0.017(4) 0.027(4) 0.005(3) 0.004(3) 0.003(3) OW4 0.018(3) 0.018(4) 0.027(4) 0.003(3) 0.007(3) -0.001(3) OW5 0.018(4) 0.048(5) 0.020(4) 0.012(4) 0.009(3) 0.002(3) OW6 0.027(4) 0.018(4) 0.034(4) -0.001(3) 0.016(4) 0.003(3) OW7 0.018(4) 0.046(6) 0.038(5) -0.009(4) 0.000(4) 0.010(4) OW8 0.042(5) 0.041(6) 0.069(7) 0.016(5) 0.000(5) -0.009(5) OW9 0.105(9) 0.039(6) 0.033(5) -0.008(4) 0.021(6) -0.038(6) OW10 0.068(8) 0.080(9) 0.105(10) 0.022(8) 0.025(8) 0.021(7) OW11 0.106(10) 0.054(7) 0.123(10) -0.049(7) 0.085(9) -0.046(7) OW12 0.037(6) 0.084(9) 0.069(8) -0.001(6) 0.009(6) -0.005(6) OW15 0.23(3) 0.43(5) 0.18(2) -0.04(3) 0.15(2) -0.11(3) #============================================================================== # REFINEMENT DATA _refine_special_details ; ? ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0809P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00006(12) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 6587 _refine_ls_number_parameters 388 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.1031 _refine_ls_R_factor_gt 0.0607 _refine_ls_wR_factor_ref 0.1511 _refine_ls_wR_factor_gt 0.1377 _refine_ls_goodness_of_fit_ref 0.956 _refine_ls_restrained_S_all 0.956 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 3.756 _refine_diff_density_min -1.221 _refine_diff_density_rms 0.313 #============================================================================== # MOLECULAR GEOMETRY _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 O5 1.694(7) . ? Mo1 O12 1.768(7) . ? Mo1 O6 1.877(6) . ? Mo1 O11 1.890(6) . ? Mo1 O17 2.221(7) 3_756 ? Mo2 O1 1.724(7) . ? Mo2 O9 1.754(7) . ? Mo2 O15 1.824(7) . ? Mo2 O17 2.003(6) . ? Mo2 O6 2.185(6) 3_756 ? Mo2 O19 2.313(7) . ? Mo3 O16 1.719(7) . ? Mo3 O18 1.752(7) . ? Mo3 O2 1.848(7) . ? Mo3 O17 1.981(7) 3_756 ? Mo3 O11 2.154(6) . ? Mo3 O3 2.293(7) . ? Mo4 O7 1.681(6) . ? Mo4 O8 1.949(7) . ? Mo4 O4 1.960(7) . ? Mo4 O15 2.059(7) . ? Mo4 O13 2.135(7) . ? Mo4 O6 2.214(6) 3_756 ? Mo4 Mo5 2.5779(13) . ? Mo5 O10 1.698(6) . ? Mo5 O8 1.919(7) . ? Mo5 O4 1.946(7) . ? Mo5 O2 2.060(7) . ? Mo5 O14 2.158(7) . ? Mo5 O11 2.184(6) . ? Y1 O9 2.317(7) 3_756 ? Y1 OW4 2.342(7) . ? Y1 OW3 2.351(6) . ? Y1 O18 2.354(7) . ? Y1 OW2 2.360(7) . ? Y1 OW5 2.363(7) . ? Y1 OW1 2.370(8) . ? Y1 O12 2.450(7) 3_756 ? O3 C1 1.257(12) . ? O6 Mo2 2.185(6) 3_756 ? O6 Mo4 2.214(6) 3_756 ? O9 Y1 2.317(7) 3_756 ? O12 Y1 2.450(7) 3_756 ? O13 C3 1.255(12) . ? O14 C1 1.286(12) . ? O17 Mo3 1.981(7) 3_756 ? O17 Mo1 2.221(7) 3_756 ? O19 C3 1.263(12) . ? C1 C2 1.509(15) . ? C3 C4 1.508(15) . ? OW12 OW15 1.31(3) . ? OW13 OW14 1.00(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O5 Mo1 O12 103.0(3) . . ? O5 Mo1 O6 106.5(3) . . ? O12 Mo1 O6 102.1(3) . . ? O5 Mo1 O11 105.4(3) . . ? O12 Mo1 O11 101.9(3) . . ? O6 Mo1 O11 134.2(3) . . ? O5 Mo1 O17 90.7(3) . 3_756 ? O12 Mo1 O17 166.3(3) . 3_756 ? O6 Mo1 O17 74.2(2) . 3_756 ? O11 Mo1 O17 73.4(3) . 3_756 ? O1 Mo2 O9 104.5(3) . . ? O1 Mo2 O15 104.1(3) . . ? O9 Mo2 O15 101.0(3) . . ? O1 Mo2 O17 98.1(3) . . ? O9 Mo2 O17 94.0(3) . . ? O15 Mo2 O17 148.9(3) . . ? O1 Mo2 O6 156.7(3) . 3_756 ? O9 Mo2 O6 97.6(3) . 3_756 ? O15 Mo2 O6 78.4(3) . 3_756 ? O17 Mo2 O6 72.7(3) . 3_756 ? O1 Mo2 O19 83.5(3) . . ? O9 Mo2 O19 170.3(3) . . ? O15 Mo2 O19 82.0(3) . . ? O17 Mo2 O19 79.2(3) . . ? O6 Mo2 O19 73.8(2) 3_756 . ? O16 Mo3 O18 104.3(3) . . ? O16 Mo3 O2 102.0(3) . . ? O18 Mo3 O2 100.9(3) . . ? O16 Mo3 O17 100.1(3) . 3_756 ? O18 Mo3 O17 93.9(3) . 3_756 ? O2 Mo3 O17 149.4(3) . 3_756 ? O16 Mo3 O11 157.3(3) . . ? O18 Mo3 O11 97.9(3) . . ? O2 Mo3 O11 78.2(3) . . ? O17 Mo3 O11 73.3(3) 3_756 . ? O16 Mo3 O3 82.3(3) . . ? O18 Mo3 O3 171.6(3) . . ? O2 Mo3 O3 82.5(3) . . ? O17 Mo3 O3 79.6(3) 3_756 . ? O11 Mo3 O3 75.1(2) . . ? O7 Mo4 O8 106.4(3) . . ? O7 Mo4 O4 103.9(3) . . ? O8 Mo4 O4 92.7(3) . . ? O7 Mo4 O15 93.4(3) . . ? O8 Mo4 O15 89.8(3) . . ? O4 Mo4 O15 161.0(3) . . ? O7 Mo4 O13 92.6(3) . . ? O8 Mo4 O13 160.9(3) . . ? O4 Mo4 O13 84.5(3) . . ? O15 Mo4 O13 87.0(3) . . ? O7 Mo4 O6 162.3(3) . 3_756 ? O8 Mo4 O6 85.3(3) . 3_756 ? O4 Mo4 O6 88.3(2) . 3_756 ? O15 Mo4 O6 73.1(2) . 3_756 ? O13 Mo4 O6 75.7(2) . 3_756 ? O7 Mo4 Mo5 97.8(2) . . ? O8 Mo4 Mo5 47.7(2) . . ? O4 Mo4 Mo5 48.5(2) . . ? O15 Mo4 Mo5 137.5(2) . . ? O13 Mo4 Mo5 132.94(19) . . ? O6 Mo4 Mo5 99.89(17) 3_756 . ? O10 Mo5 O8 104.8(3) . . ? O10 Mo5 O4 106.4(3) . . ? O8 Mo5 O4 94.1(3) . . ? O10 Mo5 O2 93.6(3) . . ? O8 Mo5 O2 160.0(3) . . ? O4 Mo5 O2 88.0(3) . . ? O10 Mo5 O14 87.8(3) . . ? O8 Mo5 O14 87.0(3) . . ? O4 Mo5 O14 164.9(3) . . ? O2 Mo5 O14 86.0(3) . . ? O10 Mo5 O11 160.6(3) . . ? O8 Mo5 O11 86.9(3) . . ? O4 Mo5 O11 87.8(3) . . ? O2 Mo5 O11 73.3(3) . . ? O14 Mo5 O11 77.2(2) . . ? O10 Mo5 Mo4 98.4(2) . . ? O8 Mo5 Mo4 48.71(19) . . ? O4 Mo5 Mo4 48.9(2) . . ? O2 Mo5 Mo4 136.9(2) . . ? O14 Mo5 Mo4 135.44(19) . . ? O11 Mo5 Mo4 100.95(17) . . ? O9 Y1 OW4 141.3(2) 3_756 . ? O9 Y1 OW3 81.9(2) 3_756 . ? OW4 Y1 OW3 116.5(2) . . ? O9 Y1 O18 69.1(2) 3_756 . ? OW4 Y1 O18 78.7(2) . . ? OW3 Y1 O18 144.0(2) . . ? O9 Y1 OW2 71.4(2) 3_756 . ? OW4 Y1 OW2 143.5(3) . . ? OW3 Y1 OW2 75.8(2) . . ? O18 Y1 OW2 112.3(2) . . ? O9 Y1 OW5 144.3(2) 3_756 . ? OW4 Y1 OW5 74.1(2) . . ? OW3 Y1 OW5 74.3(3) . . ? O18 Y1 OW5 141.1(2) . . ? OW2 Y1 OW5 77.1(3) . . ? O9 Y1 OW1 109.5(3) 3_756 . ? OW4 Y1 OW1 79.1(3) . . ? OW3 Y1 OW1 139.9(2) . . ? O18 Y1 OW1 72.3(3) . . ? OW2 Y1 OW1 72.2(3) . . ? OW5 Y1 OW1 75.5(3) . . ? O9 Y1 O12 79.9(2) 3_756 3_756 ? OW4 Y1 O12 73.3(2) . 3_756 ? OW3 Y1 O12 75.3(2) . 3_756 ? O18 Y1 O12 79.0(2) . 3_756 ? OW2 Y1 O12 141.6(2) . 3_756 ? OW5 Y1 O12 117.9(3) . 3_756 ? OW1 Y1 O12 143.4(2) . 3_756 ? Mo3 O2 Mo5 111.9(3) . . ? C1 O3 Mo3 129.4(7) . . ? Mo5 O4 Mo4 82.6(3) . . ? Mo1 O6 Mo2 109.5(3) . 3_756 ? Mo1 O6 Mo4 153.6(3) . 3_756 ? Mo2 O6 Mo4 95.1(2) 3_756 3_756 ? Mo5 O8 Mo4 83.6(3) . . ? Mo2 O9 Y1 149.1(4) . 3_756 ? Mo1 O11 Mo3 109.5(3) . . ? Mo1 O11 Mo5 152.6(3) . . ? Mo3 O11 Mo5 96.6(3) . . ? Mo1 O12 Y1 130.7(3) . 3_756 ? C3 O13 Mo4 130.7(7) . . ? C1 O14 Mo5 129.3(6) . . ? Mo2 O15 Mo4 113.3(3) . . ? Mo3 O17 Mo2 132.7(4) 3_756 . ? Mo3 O17 Mo1 103.6(3) 3_756 3_756 ? Mo2 O17 Mo1 103.6(3) . 3_756 ? Mo3 O18 Y1 149.3(4) . . ? C3 O19 Mo2 129.8(6) . . ? O3 C1 O14 126.0(10) . . ? O3 C1 C2 119.0(10) . . ? O14 C1 C2 114.9(9) . . ? O13 C3 O19 125.4(10) . . ? O13 C3 C4 116.6(10) . . ? O19 C3 C4 117.8(10) . . ? #------------------------------------------------------------------------------ #===end