Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2004 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Prof Zhao-Hui Zhou' _publ_contact_author_address ; Department of Chemistry Xiamen University State Key Laboratory for Physical C Xiamen 361005 CHINA ; _publ_contact_author_email ZHZHOU@XMU.EDU.CN _publ_section_title ; Peroxomolybdate(VI)-Citrate and Malate Complexes Interconversions by pH-Dependence. Synthetic, Structural and Spectroscopic studies ; loop_ _publ_author_name 'Zhao-Hui Zhou' 'Shu-Ya Hou' 'Huilin Wan' data_sad_3 _database_code_depnum_ccdc_archive 'CCDC 225098' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'Potassium polymeric diperoxo malato oxomolybdenum(VI)' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C4 H6 K2 Mo O11' _chemical_formula_weight 404.23 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' K K 0.2009 0.2494 '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 'P 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 7.2393(6) _cell_length_b 10.7555(9) _cell_length_c 7.5130(6) _cell_angle_alpha 90.00 _cell_angle_beta 94.407(1) _cell_angle_gamma 90.00 _cell_volume 583.25(8) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 2.72 _cell_measurement_theta_max 28.16 _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.302 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 396 _exptl_absorpt_coefficient_mu 1.888 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.7396 _exptl_absorpt_correction_T_max 0.8951 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX area-detector diffractometer' _diffrn_measurement_method '\f and \w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 3503 _diffrn_reflns_av_R_equivalents 0.0875 _diffrn_reflns_av_sigmaI/netI 0.0641 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 2.72 _diffrn_reflns_theta_max 28.16 _reflns_number_total 2059 _reflns_number_gt 1971 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 1998)' _computing_cell_refinement 'SAINT (Bruker, 1998)' _computing_data_reduction 'SAINT (Bruker, 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-II (Johnson, 1976)' _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^)+(0.0375P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.06(6) _refine_ls_number_reflns 2059 _refine_ls_number_parameters 172 _refine_ls_number_restraints 5 _refine_ls_R_factor_all 0.0360 _refine_ls_R_factor_gt 0.0346 _refine_ls_wR_factor_ref 0.0785 _refine_ls_wR_factor_gt 0.0777 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_restrained_S_all 1.029 _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 Mo1 Mo 0.41437(5) 0.97519(4) 0.22756(5) 0.02149(12) Uani 1 1 d . . . K1 K 0.41953(16) 1.07389(15) 0.71525(16) 0.0338(3) Uani 1 1 d . . . K2 K 0.86608(17) 0.84201(14) 0.00463(17) 0.0351(3) Uani 1 1 d . . . O1 O 0.5477(5) 1.1123(4) 0.3666(5) 0.0253(8) Uani 1 1 d . . . O2 O 0.6187(5) 1.0551(4) 0.0422(5) 0.0254(8) Uani 1 1 d . . . O3 O 0.8419(5) 1.1967(4) 0.0298(5) 0.0302(9) Uani 1 1 d . . . O4 O 0.7864(6) 1.1340(6) 0.6961(5) 0.0504(14) Uani 1 1 d D . . H4 H 0.800(11) 1.154(8) 0.806(3) 0.060 Uiso 1 1 d D . . O5 O 1.0723(6) 1.1851(6) 0.6620(6) 0.0611(16) Uani 1 1 d . . . O6 O 0.6354(5) 0.8711(4) 0.2841(5) 0.0334(9) Uani 1 1 d . . . O7 O 0.5023(5) 0.8159(4) 0.1464(6) 0.0361(10) Uani 1 1 d . . . O8 O 0.2374(4) 0.9741(6) 0.0198(5) 0.0355(8) Uani 1 1 d . . . O9 O 0.2584(6) 1.1015(4) 0.1003(6) 0.0361(10) Uani 1 1 d . . . O10 O 0.2835(5) 0.9375(4) 0.3969(5) 0.0350(10) Uani 1 1 d . . . O1W O 0.6647(7) 0.8375(5) -0.3219(6) 0.0524(13) Uani 1 1 d D . . H1W1 H 0.691(10) 0.874(6) -0.417(5) 0.063 Uiso 1 1 d D . . H1W2 H 0.591(9) 0.777(5) -0.349(8) 0.063 Uiso 1 1 d D . . C1 C 0.7136(7) 1.1620(5) 0.3122(6) 0.0232(11) Uani 1 1 d . . . H1A H 0.7138 1.2520 0.3333 0.028 Uiso 1 1 calc R . . C2 C 0.7264(6) 1.1388(5) 0.1115(7) 0.0207(10) Uani 1 1 d . . . C3 C 0.8908(7) 1.1055(6) 0.4100(7) 0.0295(12) Uani 1 1 d . . . H3A H 0.8808 1.0156 0.4066 0.035 Uiso 1 1 calc R . . H3B H 0.9968 1.1286 0.3456 0.035 Uiso 1 1 calc R . . C4 C 0.9258(7) 1.1461(6) 0.6013(7) 0.0287(12) 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 Mo1 0.01909(18) 0.0247(2) 0.02072(19) 0.0009(2) 0.00193(13) -0.0003(2) K1 0.0261(6) 0.0510(9) 0.0238(6) -0.0020(5) -0.0007(5) -0.0035(5) K2 0.0285(6) 0.0407(8) 0.0362(7) -0.0052(6) 0.0026(5) 0.0086(5) O1 0.0198(17) 0.034(2) 0.0218(18) -0.0039(16) 0.0010(14) -0.0008(15) O2 0.0300(19) 0.028(2) 0.0177(17) -0.0043(15) -0.0007(14) -0.0060(15) O3 0.027(2) 0.045(3) 0.0193(18) -0.0011(17) 0.0010(15) -0.0127(17) O4 0.031(2) 0.099(4) 0.022(2) -0.014(3) 0.0064(18) -0.027(2) O5 0.034(3) 0.113(5) 0.036(2) -0.023(3) 0.001(2) -0.026(3) O6 0.035(2) 0.034(2) 0.031(2) 0.0059(18) 0.0026(17) 0.0082(19) O7 0.040(2) 0.026(2) 0.043(2) -0.0078(18) 0.0100(19) -0.0012(18) O8 0.0341(18) 0.034(2) 0.0358(19) -0.005(3) -0.0107(14) -0.006(3) O9 0.033(2) 0.029(2) 0.044(3) 0.000(2) -0.0105(18) 0.0033(17) O10 0.0302(19) 0.043(3) 0.033(2) 0.0061(17) 0.0102(16) -0.0027(16) O1W 0.069(4) 0.053(3) 0.034(2) 0.009(2) -0.007(2) -0.022(3) C1 0.025(3) 0.032(3) 0.013(2) -0.004(2) 0.0038(19) -0.001(2) C2 0.019(2) 0.025(3) 0.017(2) -0.001(2) -0.0017(18) 0.005(2) C3 0.023(2) 0.043(4) 0.023(3) -0.003(2) 0.003(2) -0.001(2) C4 0.023(3) 0.040(3) 0.022(2) 0.002(2) -0.003(2) 0.000(2) _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 O10 1.693(4) . ? Mo1 O8 1.942(3) . ? Mo1 O7 1.942(4) . ? Mo1 O9 1.967(4) . ? Mo1 O6 1.972(4) . ? Mo1 O1 2.011(4) . ? Mo1 O2 2.277(4) . ? Mo1 K1 3.9956(13) 1_554 ? K1 O4 2.748(4) . ? K1 O2 2.758(4) 1_556 ? K1 O5 2.785(6) 1_455 ? K1 O7 2.844(5) 2_656 ? K1 O1 2.875(4) . ? K1 O10 2.912(4) . ? K1 O8 2.931(4) 1_556 ? K1 O1W 3.126(6) 1_556 ? K1 O9 3.215(5) 1_556 ? K1 O6 3.221(5) 2_656 ? K2 O3 2.658(4) 2_745 ? K2 O1W 2.756(5) . ? K2 O6 2.799(4) . ? K2 O9 2.832(4) 2_645 ? K2 O7 2.929(4) . ? K2 O2 2.936(4) . ? K2 O5 3.025(5) 2_746 ? K2 O8 3.035(4) 1_655 ? K2 K1 4.5074(19) 1_554 ? O1 C1 1.404(6) . ? O1 K1 2.875(4) 1 ? O2 C2 1.275(6) . ? O2 K1 2.758(4) 1_554 ? O3 C2 1.242(6) . ? O3 K2 2.658(4) 2_755 ? O4 C4 1.286(7) . ? O4 K1 2.748(4) 1 ? O5 C4 1.198(7) . ? O5 K1 2.785(6) 1_655 ? O5 K2 3.025(5) 2_756 ? O6 O7 1.482(6) . ? O6 K1 3.221(5) 2_646 ? O7 K1 2.844(5) 2_646 ? O8 O9 1.501(7) . ? O8 K1 2.931(4) 1_554 ? O8 K2 3.035(4) 1_455 ? O9 K2 2.832(4) 2_655 ? O9 K1 3.215(5) 1_554 ? O10 K1 2.912(4) 1 ? O1W K1 3.126(6) 1_554 ? C1 C2 1.538(6) . ? C1 C3 1.552(7) . ? C3 C4 1.505(7) . ? 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 Mo1 O8 103.3(2) . . ? O10 Mo1 O7 103.9(2) . . ? O8 Mo1 O7 87.4(2) . . ? O10 Mo1 O9 101.4(2) . . ? O8 Mo1 O9 45.1(2) . . ? O7 Mo1 O9 130.3(2) . . ? O10 Mo1 O6 101.2(2) . . ? O8 Mo1 O6 130.1(2) . . ? O7 Mo1 O6 44.5(2) . . ? O9 Mo1 O6 157.3(2) . . ? O10 Mo1 O1 93.4(2) . . ? O8 Mo1 O1 133.1(2) . . ? O7 Mo1 O1 130.9(2) . . ? O9 Mo1 O1 88.9(2) . . ? O6 Mo1 O1 87.5(2) . . ? O10 Mo1 O2 167.8(2) . . ? O8 Mo1 O2 86.0(2) . . ? O7 Mo1 O2 84.1(2) . . ? O9 Mo1 O2 79.5(2) . . ? O6 Mo1 O2 78.0(2) . . ? O1 Mo1 O2 74.5(1) . . ? O10 Mo1 K1 146.6(1) . 1_554 ? O8 Mo1 K1 44.1(1) . 1_554 ? O7 Mo1 K1 84.5(1) . 1_554 ? O9 Mo1 K1 52.8(1) . 1_554 ? O6 Mo1 K1 106.9(1) . 1_554 ? O1 Mo1 K1 105.4(1) . 1_554 ? O2 Mo1 K1 41.91(9) . 1_554 ? O4 K1 O2 67.8(1) . 1_556 ? K1 K1 O5 0(10) 1 1_455 ? O4 K1 O5 139.2(2) . 1_455 ? O2 K1 O5 124.3(1) 1_556 1_455 ? O4 K1 O7 68.8(1) . 2_656 ? O2 K1 O7 70.5(1) 1_556 2_656 ? O5 K1 O7 79.1(2) 1_455 2_656 ? O4 K1 O1 62.5(1) . . ? O2 K1 O1 129.7(1) 1_556 . ? O5 K1 O1 99.1(1) 1_455 . ? O7 K1 O1 97.6(1) 2_656 . ? O4 K1 O10 110.2(1) . . ? O2 K1 O10 144.6(1) 1_556 . ? O5 K1 O10 81.6(1) 1_455 . ? O7 K1 O10 143.8(1) 2_656 . ? O1 K1 O10 55.7(1) . . ? O4 K1 O8 128.4(1) . 1_556 ? O2 K1 O8 60.9(1) 1_556 1_556 ? O5 K1 O8 79.3(1) 1_455 1_556 ? O7 K1 O8 98.0(1) 2_656 1_556 ? O1 K1 O8 163.7(1) . 1_556 ? O10 K1 O8 108.2(1) . 1_556 ? O4 K1 O1W 68.2(2) . 1_556 ? O2 K1 O1W 76.0(1) 1_556 1_556 ? O5 K1 O1W 148.1(2) 1_455 1_556 ? O7 K1 O1W 132.8(1) 2_656 1_556 ? O1 K1 O1W 79.1(1) . 1_556 ? O10 K1 O1W 71.1(1) . 1_556 ? O8 K1 O1W 93.7(1) 1_556 1_556 ? O4 K1 O9 116.4(1) . 1_556 ? O2 K1 O9 53.6(1) 1_556 1_556 ? O5 K1 O9 72.8(1) 1_455 1_556 ? O7 K1 O9 70.3(1) 2_656 1_556 ? O1 K1 O9 166.2(1) . 1_556 ? O10 K1 O9 131.5(1) . 1_556 ? O8 K1 O9 27.8(1) 1_556 1_556 ? O1W K1 O9 113.8(1) 1_556 1_556 ? O4 K1 O6 83.5(2) . 2_656 ? O2 K1 O6 97.3(1) 1_556 2_656 ? O5 K1 O6 57.6(2) 1_455 2_656 ? O7 K1 O6 27.4(1) 2_656 2_656 ? O1 K1 O6 84.7(1) . 2_656 ? O10 K1 O6 117.9(1) . 2_656 ? O8 K1 O6 107.4(1) 1_556 2_656 ? O1W K1 O6 151.5(1) 1_556 2_656 ? O9 K1 O6 81.6(1) 1_556 2_656 ? O3 K2 O1W 105.9(2) 2_745 . ? O3 K2 O6 131.6(1) 2_745 . ? O1W K2 O6 111.4(1) . . ? O3 K2 O9 71.0(1) 2_745 2_645 ? O1W K2 O9 66.5(1) . 2_645 ? O6 K2 O9 96.6(1) . 2_645 ? O3 K2 O7 136.3(1) 2_745 . ? O1W K2 O7 83.9(1) . . ? O6 K2 O7 29.9(1) . . ? O9 K2 O7 74.8(1) 2_645 . ? O3 K2 O2 164.6(1) 2_745 . ? O1W K2 O2 79.3(2) . . ? O6 K2 O2 55.7(1) . . ? O9 K2 O2 123.8(1) 2_645 . ? O7 K2 O2 57.8(1) . . ? O3 K2 O5 71.6(1) 2_745 2_746 ? O1W K2 O5 140.0(2) . 2_746 ? O6 K2 O5 60.0(1) . 2_746 ? O9 K2 O5 75.2(2) 2_645 2_746 ? O7 K2 O5 74.0(1) . 2_746 ? O2 K2 O5 114.1(1) . 2_746 ? O3 K2 O8 64.5(1) 2_745 1_655 ? O1W K2 O8 116.6(1) . 1_655 ? O6 K2 O8 119.8(1) . 1_655 ? O9 K2 O8 134.5(1) 2_645 1_655 ? O7 K2 O8 148.2(1) . 1_655 ? O2 K2 O8 100.1(1) . 1_655 ? O5 K2 O8 99.0(1) 2_746 1_655 ? O3 K2 K1 145.57(9) 2_745 1_554 ? O1W K2 K1 43.1(1) . 1_554 ? O6 K2 K1 81.54(9) . 1_554 ? O9 K2 K1 99.79(9) 2_645 1_554 ? O7 K2 K1 66.23(9) . 1_554 ? O2 K2 K1 36.31(7) . 1_554 ? O5 K2 K1 139.7(1) 2_746 1_554 ? O8 K2 K1 111.1(1) 1_655 1_554 ? C1 O1 Mo1 121.0(3) . . ? C1 O1 K1 131.5(3) . 1 ? Mo1 O1 K1 101.1(2) . 1 ? C1 O1 K1 131.5(3) . . ? Mo1 O1 K1 101.1(2) . . ? C2 O2 Mo1 115.0(3) . . ? C2 O2 K1 125.0(3) . 1_554 ? Mo1 O2 K1 104.6(1) . 1_554 ? C2 O2 K2 103.4(3) . . ? Mo1 O2 K2 101.2(1) . . ? K1 O2 K2 104.6(1) 1_554 . ? C2 O3 K2 156.0(3) . 2_755 ? C4 O4 K1 148.8(4) . 1 ? C4 O4 K1 148.8(4) . . ? C4 O5 K1 131.9(5) . 1_655 ? C4 O5 K2 125.5(4) . 2_756 ? K1 O5 K2 92.7(1) 1_655 2_756 ? O7 O6 Mo1 66.7(2) . . ? O7 O6 K2 79.9(2) . . ? Mo1 O6 K2 115.0(2) . . ? O7 O6 K1 62.0(2) . 2_646 ? Mo1 O6 K1 117.7(2) . 2_646 ? K2 O6 K1 88.4(1) . 2_646 ? O6 O7 Mo1 68.9(2) . . ? O6 O7 K1 90.6(3) . 2_646 ? Mo1 O7 K1 138.9(2) . 2_646 ? O6 O7 K2 70.2(2) . . ? Mo1 O7 K2 110.8(2) . . ? K1 O7 K2 93.5(1) 2_646 . ? O9 O8 Mo1 68.3(2) . . ? O9 O8 K1 86.7(3) . 1_554 ? Mo1 O8 K1 108.5(2) . 1_554 ? O9 O8 K2 120.3(2) . 1_455 ? Mo1 O8 K2 124.1(2) . 1_455 ? K1 O8 K2 126.3(1) 1_554 1_455 ? O8 O9 Mo1 66.6(2) . . ? O8 O9 K2 134.6(3) . 2_655 ? Mo1 O9 K2 157.7(2) . 2_655 ? O8 O9 K1 65.5(2) . 1_554 ? Mo1 O9 K1 98.0(2) . 1_554 ? K2 O9 K1 87.9(1) 2_655 1_554 ? Mo1 O10 K1 108.9(2) . 1 ? Mo1 O10 K1 108.9(2) . . ? K1 O10 K1 0.00(3) 1 . ? K2 O1W K1 99.9(2) . 1_554 ? O1 C1 C2 109.9(4) . . ? O1 C1 C3 114.1(4) . . ? C2 C1 C3 106.9(4) . . ? O3 C2 O2 124.4(5) . . ? O3 C2 C1 119.8(4) . . ? O2 C2 C1 115.8(4) . . ? C4 C3 C1 114.2(5) . . ? O5 C4 O4 122.3(5) . . ? O5 C4 C3 122.9(5) . . ? O4 C4 C3 114.7(5) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O4 H4 O3 0.849(10) 1.749(13) 2.597(6) 177(8) 1_556 O1W H1W2 O1 0.856(10) 2.035(19) 2.874(7) 166(7) 2_645 _diffrn_measured_fraction_theta_max 0.935 _diffrn_reflns_theta_full 28.16 _diffrn_measured_fraction_theta_full 0.935 _refine_diff_density_max 0.585 _refine_diff_density_min -1.161 _refine_diff_density_rms 0.178 data_sad_2 _database_code_depnum_ccdc_archive 'CCDC 225099' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'Potassium dimeric diperoxo hydrogen citrato oxomolybdenum(VI)' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H23 K5 Mo2 O30' _chemical_formula_weight 1034.68 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' K K 0.2009 0.2494 '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 7.9131(5) _cell_length_b 9.4755(6) _cell_length_c 11.3561(7) _cell_angle_alpha 72.314(1) _cell_angle_beta 77.384(1) _cell_angle_gamma 72.276(1) _cell_volume 765.26(8) _cell_formula_units_Z 1 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 1.90 _cell_measurement_theta_max 28.20 _exptl_crystal_description needle _exptl_crystal_colour 'light yellow' _exptl_crystal_size_max 0.39 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.245 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 514 _exptl_absorpt_coefficient_mu 1.617 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.5711 _exptl_absorpt_correction_T_max 0.9381 _exptl_absorpt_process_details 'SADABS (Bruker, 2002)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX area-detector diffractometer' _diffrn_measurement_method '\f and \w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 4626 _diffrn_reflns_av_R_equivalents 0.0504 _diffrn_reflns_av_sigmaI/netI 0.0451 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.90 _diffrn_reflns_theta_max 28.20 _reflns_number_total 3326 _reflns_number_gt 3146 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 1998)' _computing_cell_refinement 'SAINT (Bruker, 1998)' _computing_data_reduction 'SAINT (Bruker, 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-II (Johnson, 1976)' _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^)+(0.0443P)^2^+1.0861P] 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 3326 _refine_ls_number_parameters 246 _refine_ls_number_restraints 10 _refine_ls_R_factor_all 0.0373 _refine_ls_R_factor_gt 0.0354 _refine_ls_wR_factor_ref 0.0914 _refine_ls_wR_factor_gt 0.0896 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.033 _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 Mo1 Mo 0.26027(3) 0.07590(3) 0.24859(2) 0.02087(10) Uani 1 1 d . . . K1 K 0.57833(10) -0.25437(8) 0.09902(7) 0.02893(17) Uani 1 1 d . . . K2 K 0.93359(11) 0.23730(10) -0.09314(8) 0.03430(19) Uani 1 1 d . . . O1 O 0.4461(3) 0.1075(2) 0.32993(19) 0.0199(4) Uani 1 1 d . . . O2 O 0.5124(3) 0.0388(3) 0.1208(2) 0.0215(4) Uani 1 1 d . . . O3 O 0.8040(3) 0.0258(3) 0.0890(2) 0.0277(5) Uani 1 1 d . . . O4 O 0.6288(4) -0.2541(3) 0.4997(2) 0.0303(5) Uani 1 1 d D . . O5 O 0.7382(4) -0.2615(3) 0.3067(2) 0.0324(6) Uani 1 1 d . . . O6 O 0.5976(3) 0.3808(3) 0.0593(2) 0.0323(6) Uani 1 1 d . . . O7 O 0.4785(4) 0.4784(3) 0.2231(3) 0.0388(6) Uani 1 1 d . . . O8 O 0.0977(3) 0.1153(3) 0.3661(2) 0.0348(6) Uani 1 1 d . . . O9 O 0.3458(3) -0.1482(3) 0.3131(3) 0.0334(6) Uani 1 1 d . . . O10 O 0.2203(4) -0.1013(3) 0.2207(3) 0.0365(6) Uani 1 1 d . . . O11 O 0.1449(3) 0.1905(3) 0.1026(2) 0.0339(6) Uani 1 1 d . . . O12 O 0.2325(3) 0.2859(3) 0.1381(2) 0.0313(5) Uani 1 1 d . . . O1W O 0.8987(4) -0.4811(3) 0.1480(3) 0.0494(8) Uani 1 1 d D . . O2W O 0.8837(5) 0.4661(6) -0.3229(4) 0.0747(12) Uani 1 1 d D . . C1 C 0.6289(4) 0.0874(3) 0.2762(3) 0.0177(6) Uani 1 1 d . . . C2 C 0.6541(4) 0.0477(3) 0.1514(3) 0.0196(6) Uani 1 1 d . . . C3 C 0.7476(4) -0.0428(4) 0.3658(3) 0.0214(6) Uani 1 1 d . . . H3A H 0.8727 -0.0516 0.3310 0.026 Uiso 1 1 calc R . . H3B H 0.7291 -0.0175 0.4451 0.026 Uiso 1 1 calc R . . C4 C 0.7053(4) -0.1943(4) 0.3874(3) 0.0222(6) Uani 1 1 d . . . C5 C 0.6897(4) 0.2342(4) 0.2556(3) 0.0233(6) Uani 1 1 d . . . H5A H 0.6849 0.2519 0.3362 0.028 Uiso 1 1 calc R . . H5B H 0.8134 0.2182 0.2162 0.028 Uiso 1 1 calc R . . C6 C 0.5781(4) 0.3753(4) 0.1762(3) 0.0268(7) Uani 1 1 d . . . H1 H 0.615(6) -0.205(4) 0.554(3) 0.032 Uiso 1 1 d D . . H2 H 0.5000 0.5000 0.0000 0.032 Uiso 1 2 d S . . H1W1 H 0.986(4) -0.553(3) 0.128(3) 0.032 Uiso 1 1 d D . . H1W2 H 0.898(5) -0.482(4) 0.2230(17) 0.032 Uiso 1 1 d D . . H2W1 H 0.775(2) 0.494(5) -0.289(3) 0.032 Uiso 1 1 d D . . H2W2 H 0.886(5) 0.423(5) -0.379(3) 0.032 Uiso 1 1 d D . . O3W O 0.8660(9) 0.3572(6) 0.4802(7) 0.0989(17) Uani 1 1 d D . . K3 K 0.5000 0.5000 0.5000 0.1054(10) Uani 1 2 d S . . H3W1 H 0.952(8) 0.323(10) 0.428(8) 0.18(5) Uiso 1 1 d D . . H3W2 H 0.789(4) 0.306(4) 0.499(4) 0.024(11) Uiso 1 1 d 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 0.01666(15) 0.02807(16) 0.01864(15) -0.00817(11) -0.00140(10) -0.00534(10) K1 0.0343(4) 0.0259(4) 0.0253(4) -0.0070(3) -0.0020(3) -0.0069(3) K2 0.0346(4) 0.0363(4) 0.0319(4) -0.0060(3) -0.0024(3) -0.0132(3) O1 0.0170(10) 0.0284(11) 0.0157(10) -0.0095(8) 0.0008(8) -0.0062(8) O2 0.0211(11) 0.0283(11) 0.0166(10) -0.0084(9) -0.0029(8) -0.0055(9) O3 0.0217(11) 0.0374(13) 0.0196(11) -0.0084(10) 0.0042(9) -0.0051(10) O4 0.0461(15) 0.0266(12) 0.0193(11) -0.0072(9) 0.0036(10) -0.0151(11) O5 0.0445(15) 0.0282(12) 0.0233(12) -0.0130(10) -0.0039(11) -0.0017(11) O6 0.0368(14) 0.0246(12) 0.0297(13) -0.0034(10) -0.0072(11) -0.0013(10) O7 0.0393(15) 0.0263(13) 0.0419(15) -0.0103(11) 0.0096(12) -0.0047(11) O8 0.0230(12) 0.0568(17) 0.0236(12) -0.0148(12) 0.0029(9) -0.0085(11) O9 0.0341(14) 0.0300(13) 0.0368(14) -0.0033(11) -0.0093(11) -0.0110(11) O10 0.0361(14) 0.0439(15) 0.0388(15) -0.0134(12) -0.0081(11) -0.0188(12) O11 0.0301(13) 0.0438(15) 0.0283(13) -0.0080(11) -0.0109(10) -0.0068(11) O12 0.0316(13) 0.0286(13) 0.0306(13) -0.0076(10) -0.0057(10) -0.0024(10) O1W 0.0416(17) 0.0376(16) 0.068(2) -0.0198(15) -0.0101(16) 0.0003(13) O2W 0.044(2) 0.099(3) 0.064(3) -0.026(2) -0.0065(18) 0.010(2) C1 0.0175(14) 0.0201(14) 0.0144(13) -0.0038(11) -0.0010(10) -0.0047(11) C2 0.0235(15) 0.0160(13) 0.0155(14) -0.0024(11) -0.0028(11) -0.0012(11) C3 0.0216(15) 0.0253(15) 0.0163(14) -0.0024(11) -0.0059(11) -0.0050(12) C4 0.0214(15) 0.0224(15) 0.0187(14) -0.0039(12) -0.0053(11) 0.0006(12) C5 0.0263(16) 0.0246(15) 0.0222(15) -0.0073(12) -0.0023(12) -0.0107(13) C6 0.0234(16) 0.0221(16) 0.0337(18) -0.0039(13) -0.0008(13) -0.0094(12) O3W 0.094(4) 0.081(4) 0.128(5) -0.058(3) -0.038(4) 0.014(3) K3 0.0582(11) 0.0998(16) 0.198(3) -0.1093(19) 0.0372(14) -0.0441(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mo1 O8 1.684(2) . ? Mo1 O10 1.926(3) . ? Mo1 O11 1.930(2) . ? Mo1 O9 1.975(3) . ? Mo1 O12 1.980(2) . ? Mo1 O1 2.034(2) . ? Mo1 O2 2.197(2) . ? Mo1 K1 3.8898(8) 2_655 ? Mo1 K1 3.9472(8) . ? K1 O2 2.744(2) . ? K1 O7 2.754(3) 1_545 ? K1 O2 2.777(2) 2_655 ? K1 O1W 2.815(3) . ? K1 O12 2.835(3) 2_655 ? K1 O11 2.860(3) 2_655 ? K1 O5 2.885(3) . ? K1 O9 2.952(3) . ? K1 O10 3.008(3) . ? K1 O6 3.166(3) 2_655 ? K1 C2 3.338(3) . ? K1 C6 3.349(3) 1_545 ? K2 O3 2.675(3) . ? K2 O3 2.710(3) 2_755 ? K2 O10 2.846(3) 2_655 ? K2 O1W 2.849(3) 2_755 ? K2 O2W 2.856(5) . ? K2 O11 2.917(3) 1_655 ? K2 O6 3.022(3) . ? K2 O5 3.154(3) 2_755 ? K2 K1 3.8998(12) 2_755 ? K2 K1 4.0191(12) 2_655 ? K2 K2 4.2564(17) 2_755 ? O1 C1 1.421(4) . ? O2 C2 1.277(4) . ? O2 K1 2.777(2) 2_655 ? O3 C2 1.235(4) . ? O3 K2 2.710(3) 2_755 ? O4 C4 1.322(4) . ? O4 K3 2.812(2) 1_545 ? O5 C4 1.209(4) . ? O5 K2 3.154(3) 2_755 ? O5 K3 3.354(3) 1_545 ? O6 C6 1.290(4) . ? O6 K1 3.166(3) 2_655 ? O7 C6 1.234(4) . ? O7 K1 2.754(3) 1_565 ? O7 K3 3.256(3) . ? O9 O10 1.480(4) . ? O9 K3 3.386(2) 1_545 ? O10 K2 2.846(3) 2_655 ? O11 O12 1.479(4) . ? O11 K1 2.860(3) 2_655 ? O11 K2 2.917(3) 1_455 ? O12 K1 2.835(3) 2_655 ? O1W K2 2.849(3) 2_755 ? C1 C2 1.531(4) . ? C1 C5 1.543(4) . ? C1 C3 1.546(4) . ? C2 K1 3.466(3) 2_655 ? C3 C4 1.509(4) . ? C4 K3 3.518(3) 1_545 ? C5 C6 1.508(5) . ? C6 K1 3.349(3) 1_565 ? O3W K3 2.790(6) . ? K3 O3W 2.790(6) 2_666 ? K3 O4 2.812(2) 1_565 ? K3 O4 2.812(2) 2_656 ? K3 O7 3.256(3) 2_666 ? K3 O5 3.354(3) 1_565 ? K3 O5 3.354(3) 2_656 ? K3 O9 3.386(2) 1_565 ? K3 O9 3.386(2) 2_656 ? K3 C4 3.518(3) 1_565 ? K3 C4 3.518(3) 2_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 O8 Mo1 O10 103.2(1) . . ? O8 Mo1 O11 102.6(1) . . ? O10 Mo1 O11 85.8(1) . . ? O8 Mo1 O9 99.8(1) . . ? O10 Mo1 O9 44.6(1) . . ? O11 Mo1 O9 129.1(1) . . ? O8 Mo1 O12 98.6(1) . . ? O10 Mo1 O12 129.1(1) . . ? O11 Mo1 O12 44.4(1) . . ? O9 Mo1 O12 161.6(1) . . ? O8 Mo1 O1 91.7(1) . . ? O10 Mo1 O1 133.7(1) . . ? O11 Mo1 O1 133.6(1) . . ? O9 Mo1 O1 90.1(1) . . ? O12 Mo1 O1 90.3(1) . . ? O8 Mo1 O2 165.9(1) . . ? O10 Mo1 O2 87.7(1) . . ? O11 Mo1 O2 87.0(1) . . ? O9 Mo1 O2 81.6(1) . . ? O12 Mo1 O2 80.81(9) . . ? O1 Mo1 O2 74.18(8) . . ? O8 Mo1 K1 140.82(9) . 2_655 ? O10 Mo1 K1 95.92(9) . 2_655 ? O11 Mo1 K1 44.68(8) . 2_655 ? O9 Mo1 K1 117.54(8) . 2_655 ? O12 Mo1 K1 44.35(8) . 2_655 ? O1 Mo1 K1 99.33(6) . 2_655 ? O2 Mo1 K1 44.24(6) . 2_655 ? O8 Mo1 K1 144.5(1) . . ? O10 Mo1 K1 47.65(8) . . ? O11 Mo1 K1 95.53(8) . . ? O9 Mo1 K1 46.32(8) . . ? O12 Mo1 K1 115.44(8) . . ? O1 Mo1 K1 97.50(6) . . ? O2 Mo1 K1 42.05(6) . . ? K1 Mo1 K1 71.22(2) 2_655 . ? O2 K1 O7 139.47(8) . 1_545 ? O2 K1 O2 68.50(7) . 2_655 ? O7 K1 O2 131.40(9) 1_545 2_655 ? O2 K1 O1W 123.71(9) . . ? O7 K1 O1W 74.12(9) 1_545 . ? O2 K1 O1W 130.19(9) 2_655 . ? O2 K1 O12 111.67(7) . 2_655 ? O7 K1 O12 108.15(8) 1_545 2_655 ? O2 K1 O12 57.80(7) 2_655 2_655 ? O1W K1 O12 74.53(9) . 2_655 ? O2 K1 O11 88.39(7) . 2_655 ? O7 K1 O11 131.64(8) 1_545 2_655 ? O2 K1 O11 60.62(7) 2_655 2_655 ? O1W K1 O11 71.10(9) . 2_655 ? O12 K1 O11 30.09(7) 2_655 2_655 ? O2 K1 O5 70.82(7) . . ? O7 K1 O5 92.34(9) 1_545 . ? O2 K1 O5 135.12(7) 2_655 . ? O1W K1 O5 62.95(9) . . ? O12 K1 O5 125.20(8) 2_655 . ? O11 K1 O5 100.52(8) 2_655 . ? O2 K1 O9 57.16(7) . . ? O7 K1 O9 82.35(8) 1_545 . ? O2 K1 O9 109.15(7) 2_655 . ? O1W K1 O9 117.13(9) . . ? O12 K1 O9 166.66(8) 2_655 . ? O11 K1 O9 143.94(8) 2_655 . ? O5 K1 O9 60.78(7) . . ? O2 K1 O10 59.50(7) . . ? O7 K1 O10 84.50(8) 1_545 . ? O2 K1 O10 86.20(7) 2_655 . ? O1W K1 O10 143.4(1) . . ? O12 K1 O10 141.47(8) 2_655 . ? O11 K1 O10 141.39(8) 2_655 . ? O5 K1 O10 89.17(7) . . ? O9 K1 O10 28.73(7) . . ? O2 K1 O6 129.38(7) . 2_655 ? O7 K1 O6 64.80(8) 1_545 2_655 ? O2 K1 O6 68.17(6) 2_655 2_655 ? O1W K1 O6 104.03(8) . 2_655 ? O12 K1 O6 63.02(7) 2_655 2_655 ? O11 K1 O6 92.36(7) 2_655 2_655 ? O5 K1 O6 156.70(7) . 2_655 ? O9 K1 O6 116.86(7) . 2_655 ? O10 K1 O6 92.78(7) . 2_655 ? O2 K1 C2 21.53(7) . . ? O7 K1 C2 141.40(8) 1_545 . ? O2 K1 C2 80.95(7) 2_655 . ? O1W K1 C2 102.20(9) . . ? O12 K1 C2 107.62(8) 2_655 . ? O11 K1 C2 79.10(8) 2_655 . ? O5 K1 C2 54.66(7) . . ? O9 K1 C2 64.91(7) . . ? O10 K1 C2 76.48(7) . . ? O6 K1 C2 148.00(7) 2_655 . ? O2 K1 C6 159.33(8) . 1_545 ? O7 K1 C6 20.50(8) 1_545 1_545 ? O2 K1 C6 126.43(8) 2_655 1_545 ? O1W K1 C6 60.55(9) . 1_545 ? O12 K1 C6 89.00(8) 2_655 1_545 ? O11 K1 C6 111.13(8) 2_655 1_545 ? O5 K1 C6 97.96(8) . 1_545 ? O9 K1 C6 102.31(8) . 1_545 ? O10 K1 C6 104.24(8) . 1_545 ? O6 K1 C6 59.07(8) 2_655 1_545 ? C2 K1 C6 152.58(8) . 1_545 ? O3 K2 O3 75.55(8) . 2_755 ? O3 K2 O10 76.11(8) . 2_655 ? O3 K2 O10 81.54(8) 2_755 2_655 ? O3 K2 O1W 145.0(1) . 2_755 ? O3 K2 O1W 107.67(8) 2_755 2_755 ? O10 K2 O1W 138.7(1) 2_655 2_755 ? O3 K2 O2W 147.2(1) . . ? O3 K2 O2W 119.9(1) 2_755 . ? O10 K2 O2W 77.9(1) 2_655 . ? O1W K2 O2W 62.5(1) 2_755 . ? O3 K2 O11 78.79(8) . 1_655 ? O3 K2 O11 71.80(8) 2_755 1_655 ? O10 K2 O11 147.10(8) 2_655 1_655 ? O1W K2 O11 69.81(9) 2_755 1_655 ? O2W K2 O11 132.2(1) . 1_655 ? O3 K2 O6 68.29(7) . . ? O3 K2 O6 142.35(7) 2_755 . ? O10 K2 O6 99.23(8) 2_655 . ? O1W K2 O6 96.42(9) 2_755 . ? O2W K2 O6 96.71(9) . . ? O11 K2 O6 90.80(8) 1_655 . ? O3 K2 O5 139.94(7) . 2_755 ? O3 K2 O5 64.76(7) 2_755 2_755 ? O10 K2 O5 92.41(8) 2_655 2_755 ? O1W K2 O5 59.19(8) 2_755 2_755 ? O2W K2 O5 60.50(9) . 2_755 ? O11 K2 O5 93.28(7) 1_655 2_755 ? O6 K2 O5 151.67(7) . 2_755 ? O3 K2 K1 118.19(6) . 2_755 ? O3 K2 K1 62.71(6) 2_755 2_755 ? O10 K2 K1 133.48(6) 2_655 2_755 ? O1W K2 K1 46.13(6) 2_755 2_755 ? O2W K2 K1 94.31(9) . 2_755 ? O11 K2 K1 46.93(6) 1_655 2_755 ? O6 K2 K1 127.28(6) . 2_755 ? O5 K2 K1 46.81(5) 2_755 2_755 ? O3 K2 K1 65.61(5) . 2_655 ? O3 K2 K1 121.30(6) 2_755 2_655 ? O10 K2 K1 48.34(6) 2_655 2_655 ? O1W K2 K1 129.54(6) 2_755 2_655 ? O2W K2 K1 82.12(9) . 2_655 ? O11 K2 K1 134.65(6) 1_655 2_655 ? O6 K2 K1 51.08(5) . 2_655 ? O5 K2 K1 132.05(5) 2_755 2_655 ? K1 K2 K1 175.62(3) 2_755 2_655 ? O3 K2 K2 38.07(5) . 2_755 ? O3 K2 K2 37.48(5) 2_755 2_755 ? O10 K2 K2 75.85(6) 2_655 2_755 ? O1W K2 K2 135.06(7) 2_755 2_755 ? O2W K2 K2 147.7(1) . 2_755 ? O11 K2 K2 71.28(6) 1_655 2_755 ? O6 K2 K2 105.77(5) . 2_755 ? O5 K2 K2 102.09(5) 2_755 2_755 ? K1 K2 K2 90.28(3) 2_755 2_755 ? K1 K2 K2 94.09(3) 2_655 2_755 ? C1 O1 Mo1 122.2(2) . . ? C2 O2 Mo1 118.9(2) . . ? C2 O2 K1 106.4(2) . . ? Mo1 O2 K1 105.52(9) . . ? C2 O2 K1 112.1(2) . 2_655 ? Mo1 O2 K1 102.26(8) . 2_655 ? K1 O2 K1 111.50(7) . 2_655 ? C2 O3 K2 125.7(2) . . ? C2 O3 K2 129.8(2) . 2_755 ? K2 O3 K2 104.45(8) . 2_755 ? C4 O4 K3 111.5(2) . 1_545 ? C4 O5 K1 138.1(2) . . ? C4 O5 K2 121.9(2) . 2_755 ? K1 O5 K2 80.31(6) . 2_755 ? C4 O5 K3 87.6(2) . 1_545 ? K1 O5 K3 90.50(7) . 1_545 ? K2 O5 K3 144.32(8) 2_755 1_545 ? C6 O6 K2 126.3(2) . . ? C6 O6 K1 133.9(2) . 2_655 ? K2 O6 K1 80.96(7) . 2_655 ? C6 O7 K1 108.1(2) . 1_565 ? C6 O7 K3 123.0(2) . . ? K1 O7 K3 94.97(9) 1_565 . ? O10 O9 Mo1 66.0(1) . . ? O10 O9 K1 77.7(2) . . ? Mo1 O9 K1 104.7(1) . . ? O10 O9 K3 128.8(2) . 1_545 ? Mo1 O9 K3 162.7(1) . 1_545 ? K1 O9 K3 88.75(7) . 1_545 ? O9 O10 Mo1 69.5(2) . . ? O9 O10 K2 139.3(2) . 2_655 ? Mo1 O10 K2 151.2(1) . 2_655 ? O9 O10 K1 73.6(2) . . ? Mo1 O10 K1 104.1(1) . . ? K2 O10 K1 86.67(8) 2_655 . ? O12 O11 Mo1 69.6(1) . . ? O12 O11 K1 74.0(2) . 2_655 ? Mo1 O11 K1 107.0(1) . 2_655 ? O12 O11 K2 135.2(2) . 1_455 ? Mo1 O11 K2 155.2(1) . 1_455 ? K1 O11 K2 84.91(7) 2_655 1_455 ? O11 O12 Mo1 66.0(1) . . ? O11 O12 K1 75.9(2) . 2_655 ? Mo1 O12 K1 106.4(1) . 2_655 ? K1 O1W K2 87.02(9) . 2_755 ? O1 C1 C2 109.5(2) . . ? O1 C1 C5 110.7(2) . . ? C2 C1 C5 109.7(2) . . ? O1 C1 C3 109.7(2) . . ? C2 C1 C3 109.9(2) . . ? C5 C1 C3 107.3(2) . . ? O3 C2 O2 124.9(3) . . ? O3 C2 C1 119.9(3) . . ? O2 C2 C1 115.2(3) . . ? O3 C2 K1 91.4(2) . . ? O2 C2 K1 52.0(2) . . ? C1 C2 K1 128.1(2) . . ? O3 C2 K1 96.0(2) . 2_655 ? O2 C2 K1 47.9(1) . 2_655 ? C1 C2 K1 126.9(2) . 2_655 ? K1 C2 K1 84.22(7) . 2_655 ? C4 C3 C1 111.6(2) . . ? O5 C4 O4 119.5(3) . . ? O5 C4 C3 122.8(3) . . ? O4 C4 C3 117.7(3) . . ? O5 C4 K3 72.3(2) . 1_545 ? O4 C4 K3 48.1(2) . 1_545 ? C3 C4 K3 162.7(2) . 1_545 ? C6 C5 C1 113.9(3) . . ? O7 C6 O6 123.7(3) . . ? O7 C6 C5 120.4(3) . . ? O6 C6 C5 115.9(3) . . ? O7 C6 K1 51.4(2) . 1_565 ? O6 C6 K1 89.3(2) . 1_565 ? C5 C6 K1 132.2(2) . 1_565 ? O3W K3 O3W 180.0(3) . 2_666 ? O3W K3 O4 81.0(1) . 1_565 ? O3W K3 O4 99.0(1) 2_666 1_565 ? O3W K3 O4 99.0(1) . 2_656 ? O3W K3 O4 81.0(1) 2_666 2_656 ? O4 K3 O4 180.000(1) 1_565 2_656 ? O3W K3 O7 88.2(1) . 2_666 ? O3W K3 O7 91.9(1) 2_666 2_666 ? O4 K3 O7 65.83(7) 1_565 2_666 ? O4 K3 O7 114.17(7) 2_656 2_666 ? O3W K3 O7 91.9(1) . . ? O3W K3 O7 88.2(1) 2_666 . ? O4 K3 O7 114.17(7) 1_565 . ? O4 K3 O7 65.83(7) 2_656 . ? O7 K3 O7 180.0 2_666 . ? O3W K3 O5 68.83(16) . 1_565 ? O3W K3 O5 111.17(16) 2_666 1_565 ? O4 K3 O5 40.37(6) 1_565 1_565 ? O4 K3 O5 139.63(6) 2_656 1_565 ? O7 K3 O5 104.05(6) 2_666 1_565 ? O7 K3 O5 75.95(6) . 1_565 ? O3W K3 O5 111.17(16) . 2_656 ? O3W K3 O5 68.83(16) 2_666 2_656 ? O4 K3 O5 139.63(6) 1_565 2_656 ? O4 K3 O5 40.37(6) 2_656 2_656 ? O7 K3 O5 75.95(6) 2_666 2_656 ? O7 K3 O5 104.05(6) . 2_656 ? O5 K3 O5 180.0 1_565 2_656 ? O3W K3 O9 120.3(2) . 1_565 ? O3W K3 O9 59.7(2) 2_666 1_565 ? O4 K3 O9 60.26(7) 1_565 1_565 ? O4 K3 O9 119.74(7) 2_656 1_565 ? O7 K3 O9 111.08(6) 2_666 1_565 ? O7 K3 O9 68.92(6) . 1_565 ? O5 K3 O9 51.97(6) 1_565 1_565 ? O5 K3 O9 128.03(6) 2_656 1_565 ? O3W K3 O9 59.7(2) . 2_656 ? O3W K3 O9 120.3(2) 2_666 2_656 ? O4 K3 O9 119.74(7) 1_565 2_656 ? O4 K3 O9 60.26(7) 2_656 2_656 ? O7 K3 O9 68.92(6) 2_666 2_656 ? O7 K3 O9 111.08(6) . 2_656 ? O5 K3 O9 128.03(6) 1_565 2_656 ? O5 K3 O9 51.97(6) 2_656 2_656 ? O9 K3 O9 180.0 1_565 2_656 ? O3W K3 C4 75.9(2) . 1_565 ? O3W K3 C4 104.1(2) 2_666 1_565 ? O4 K3 C4 20.47(7) 1_565 1_565 ? O4 K3 C4 159.53(7) 2_656 1_565 ? O7 K3 C4 85.73(7) 2_666 1_565 ? O7 K3 C4 94.27(7) . 1_565 ? O5 K3 C4 20.09(7) 1_565 1_565 ? O5 K3 C4 159.91(7) 2_656 1_565 ? O9 K3 C4 51.67(6) 1_565 1_565 ? O9 K3 C4 128.33(6) 2_656 1_565 ? O3W K3 C4 104.1(2) . 2_656 ? O3W K3 C4 75.9(2) 2_666 2_656 ? O4 K3 C4 159.53(7) 1_565 2_656 ? O4 K3 C4 20.47(7) 2_656 2_656 ? O7 K3 C4 94.27(7) 2_666 2_656 ? O7 K3 C4 85.73(7) . 2_656 ? O5 K3 C4 159.91(7) 1_565 2_656 ? O5 K3 C4 20.09(7) 2_656 2_656 ? O9 K3 C4 128.33(6) 1_565 2_656 ? O9 K3 C4 51.67(6) 2_656 2_656 ? C4 K3 C4 180.000(1) 1_565 2_656 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O6 H2 O6 1.249(2) 1.249(2) 2.497(5) 180.0(3) 2_665 O4 H1 O1 0.848(10) 1.738(12) 2.580(3) 171(4) 2_656 O1W H1W2 O5 0.849(10) 2.44(3) 2.977(4) 122(3) . O1W H1W1 O12 0.852(10) 2.082(18) 2.887(4) 157(3) 1_645 O1W H1W2 O2W 0.849(10) 2.32(3) 2.957(5) 132(4) 2_755 O2W H2W1 O7 0.856(10) 1.951(14) 2.793(5) 168(3) 2_665 _diffrn_measured_fraction_theta_max 0.880 _diffrn_reflns_theta_full 28.20 _diffrn_measured_fraction_theta_full 0.880 _refine_diff_density_max 1.419 _refine_diff_density_min -1.095 _refine_diff_density_rms 0.108 data_sad_1 _database_code_depnum_ccdc_archive 'CCDC 225100' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'Potassium diperoxo citrato oxomolybdenum(VI) tetrahydrate' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C6 H12 K4 Mo O16' _chemical_formula_weight 592.50 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' K K 0.2009 0.2494 '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 Orthorhombic _symmetry_space_group_name_H-M 'P nma' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z+1/2' '-x, y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z-1/2' 'x, -y-1/2, z' _cell_length_a 22.361(2) _cell_length_b 10.3537(8) _cell_length_c 7.8268(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1812.1(2) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 2325 _cell_measurement_theta_min 2.7 _cell_measurement_theta_max 24.6 _exptl_crystal_description Block _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.172 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1176 _exptl_absorpt_coefficient_mu 1.72 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.668 _exptl_absorpt_correction_T_max 0.889 _exptl_absorpt_process_details 'SADABS (Bruker, 2002)' _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX area-detector diffractometer' _diffrn_measurement_method '\f and \w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 10442 _diffrn_reflns_av_R_equivalents 0.044 _diffrn_reflns_av_sigmaI/netI 0.037 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -7 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 1.8 _diffrn_reflns_theta_max 27.5 _reflns_number_total 2179 _reflns_number_gt 1749 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'SMART (Bruker, 1998)' _computing_cell_refinement 'SAINT (Bruker, 1998)' _computing_data_reduction 'SAINT (Bruker, 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-II (Johnson, 1976)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0470P)^2^] 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 2179 _refine_ls_number_parameters 155 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.042 _refine_ls_R_factor_gt 0.031 _refine_ls_wR_factor_ref 0.079 _refine_ls_wR_factor_gt 0.075 _refine_ls_goodness_of_fit_ref 1.01 _refine_ls_restrained_S_all 1.01 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean <0.001 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 0.63017(1) 0.2500 0.39077(4) 0.0188(1) Uani 1 2 d S . . K1 K 0.75182(3) 0.51668(8) 0.52382(9) 0.0383(2) Uani 1 1 d . . . K2 K 0.46759(4) 0.2500 0.4971(1) 0.0310(2) Uani 1 2 d S . . K3 K 0.57719(5) -0.2500 0.9929(1) 0.0398(3) Uani 1 2 d S . . O1 O 0.7007(1) 0.2500 0.5927(3) 0.027(1) Uani 1 2 d S . . O2 O 0.7154(1) 0.2500 0.8728(4) 0.033(1) Uani 1 2 d S . . O3 O 0.5861(1) 0.2500 0.6088(3) 0.020(1) Uani 1 2 d S . . O4 O 0.6598(1) -0.0363(2) 0.7792(3) 0.035(1) Uani 1 1 d . . . O5 O 0.5623(1) -0.0635(2) 0.7413(3) 0.033(1) Uani 1 1 d . . . O6 O 0.6791(1) 0.1230(2) 0.2759(3) 0.033(1) Uani 1 1 d . . . O7 O 0.6420(1) 0.0605(2) 0.4085(2) 0.030(1) Uani 1 1 d . . . O8 O 0.5671(1) 0.2500 0.2723(3) 0.026(1) Uani 1 2 d S . . O1w O 0.3415(2) 0.2500 0.4409(4) 0.041(1) Uani 1 2 d SD . . O2w O 0.6723(2) -0.2500 1.1918(8) 0.116(2) Uani 1 2 d SD . . O3w O 0.5475(1) -0.0706(2) 1.2371(3) 0.039(1) Uani 1 1 d D . . C1 C 0.6822(2) 0.2500 0.7476(5) 0.023(1) Uani 1 2 d S . . C2 C 0.6139(2) 0.2500 0.7710(4) 0.018(1) Uani 1 2 d S . . C3 C 0.5947(1) 0.1310(3) 0.8742(3) 0.022(1) Uani 1 1 d . . . C4 C 0.6062(1) 0.0014(3) 0.7897(3) 0.024(1) Uani 1 1 d . . . H1w1 H 0.338(2) 0.317(1) 0.379(2) 0.04(1) Uiso 1 1 d D . . H2w1 H 0.693(1) -0.317(1) 1.210(6) 0.07(2) Uiso 1 1 d D . . H3w1 H 0.574(1) -0.024(3) 1.285(5) 0.09(2) Uiso 1 1 d D . . H3w2 H 0.515(1) -0.028(3) 1.232(5) 0.08(2) Uiso 1 1 d D . . H3a H 0.6154 0.1325 0.9830 0.027 Uiso 1 1 calc R . . H3b H 0.5522 0.1380 0.8977 0.027 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 0.0192(2) 0.0214(2) 0.0159(2) 0.000 0.0001(1) 0.000 K1 0.0360(4) 0.0517(5) 0.0272(4) -0.0043(3) 0.0029(3) -0.0181(3) K2 0.0295(5) 0.0365(6) 0.0271(5) 0.000 -0.0014(4) 0.000 K3 0.0620(7) 0.0271(6) 0.0301(5) 0.000 0.0000(5) 0.000 O1 0.019(1) 0.038(2) 0.023(2) 0.000 0.000(1) 0.000 O2 0.023(2) 0.049(2) 0.027(2) 0.000 -0.010(1) 0.000 O3 0.017(1) 0.028(2) 0.014(1) 0.000 -0.001(1) 0.000 O4 0.034(1) 0.029(1) 0.043(1) -0.003(1) -0.005(1) 0.009(1) O5 0.035(1) 0.022(1) 0.043(1) -0.008(1) -0.003(1) -0.004(1) O6 0.035(1) 0.036(1) 0.028(1) -0.005(1) 0.008(1) 0.009(1) O7 0.037(1) 0.025(1) 0.029(1) 0.000(1) 0.001(1) 0.005(1) O8 0.025(1) 0.034(2) 0.018(1) 0.000 -0.004(1) 0.000 O1w 0.047(2) 0.034(2) 0.044(2) 0.000 0.017(2) 0.000 O2w 0.030(2) 0.248(8) 0.071(4) 0.000 -0.006(2) 0.000 O3w 0.038(1) 0.031(1) 0.048(1) -0.007(1) -0.006(1) -0.002(1) C1 0.023(2) 0.021(2) 0.024(2) 0.000 -0.003(2) 0.000 C2 0.020(2) 0.019(2) 0.014(2) 0.000 -0.003(1) 0.000 C3 0.026(1) 0.021(1) 0.021(1) 0.001(1) 0.002(1) -0.001(1) C4 0.033(2) 0.019(1) 0.019(1) 0.005(1) -0.001(1) 0.001(1) 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 O1 2.232(3) . yes Mo1 O3 1.971(2) . yes Mo1 O6 1.933(2) . yes Mo1 O6 1.933(2) 8_565 no Mo1 O7 1.985(2) . yes Mo1 O7 1.985(2) 8_565 no Mo1 O8 1.688(3) . yes K1 O7 2.736(2) 8_565 no K1 O6 2.737(2) 7_766 no K1 O2 2.788(2) 2_664 no K1 O4 2.806(2) 7_765 no K1 O4 2.876(2) 8_565 no K1 O6 2.915(2) 8_565 no K1 O1 3.037(1) . no K1 O1w 3.204(3) 5_666 no K2 O5 2.767(2) 5_656 no K2 O5 2.767(2) 4_656 no K2 O3 2.790(3) . no K2 O3w 2.810(3) 4_657 no K2 O3w 2.810(3) 5_657 no K2 O8 2.837(3) . no K2 O1w 2.854(4) . no K3 O2w 2.636(5) . no K3 O3w 2.747(2) 8 no K3 O3w 2.747(2) . no K3 O5 2.778(2) 8 no K3 O5 2.778(2) . no K3 O4 3.333(2) . no K3 O4 3.333(2) 8 no O1 C1 1.281(5) . no O2 C1 1.230(5) . no O3 C2 1.414(4) . no O4 C4 1.263(3) . no O5 C4 1.248(3) . no O6 O7 1.478(3) . no C1 C2 1.536(5) . no C2 C3 1.535(3) . no C2 C3 1.535(3) 8_565 no C3 C4 1.518(4) . no O1w H1w1 0.85(1) . no O2w H2w1 0.85(1) . no O3w H3w1 0.85(1) . no O3w H3w2 0.86(1) . no C3 H3a 0.97 . no C3 H3b 0.97 . no 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 O1 Mo1 O3 75.0(1) . . yes O1 Mo1 O6 86.0(1) . . yes O1 Mo1 O6 86.0(1) . 8_565 no O1 Mo1 O7 81.8(1) . . yes O1 Mo1 O7 81.8(1) . 8_565 no O1 Mo1 O8 168.2(1) . . yes O3 Mo1 O6 133.3(1) . . yes O3 Mo1 O6 133.3(1) . 8_565 no O3 Mo1 O7 90.4(1) . . yes O3 Mo1 O7 90.4(1) . 8_565 no O3 Mo1 O8 93.3(1) . . yes O6 Mo1 O6 85.8(1) . 8_565 yes O6 Mo1 O7 44.3(1) . . yes O6 Mo1 O7 129.0(1) . 8_565 yes O6 Mo1 O8 102.6(1) . . yes O6 Mo1 O7 129.0(1) 8_565 . no O6 Mo1 O7 44.3(1) 8_565 8_565 no O6 Mo1 O8 102.6(1) 8_565 . no O7 Mo1 O7 162.7(1) . 8_565 yes O7 Mo1 O8 98.6(1) . . yes O7 Mo1 O8 98.6(1) 8_565 . no O7 K1 O6 149.5(1) 8_565 7_766 no O7 K1 O2 110.4(1) 8_565 2_664 no O6 K1 O2 79.0(1) 7_766 2_664 no O7 K1 O4 110.5(1) 8_565 7_765 no O6 K1 O4 100.0(1) 7_766 7_765 no O2 K1 O4 72.2(1) 2_664 7_765 no O7 K1 O4 66.9(1) 8_565 8_565 no O6 K1 O4 82.8(1) 7_766 8_565 no O2 K1 O4 115.0(1) 2_664 8_565 no O4 K1 O4 172.8(1) 7_765 8_565 no O7 K1 O6 30.1(1) 8_565 8_565 no O6 K1 O6 173.7(1) 7_766 8_565 no O2 K1 O6 107.1(1) 2_664 8_565 no O4 K1 O6 80.9(1) 7_765 8_565 no O4 K1 O6 95.7(1) 8_565 8_565 no O7 K1 O1 57.0(1) 8_565 . no O6 K1 O1 116.8(1) 7_766 . no O2 K1 O1 164.2(1) 2_664 . no O4 K1 O1 102.1(1) 7_765 . no O4 K1 O1 70.8(1) 8_565 . no O6 K1 O1 57.1(1) 8_565 . no O7 K1 O1w 70.4(1) 8_565 5_666 no O6 K1 O1w 90.1(1) 7_766 5_666 no O2 K1 O1w 63.5(1) 2_664 5_666 no O4 K1 O1w 131.7(1) 7_765 5_666 no O4 K1 O1w 54.6(1) 8_565 5_666 no O6 K1 O1w 93.9(1) 8_565 5_666 no O1 K1 O1w 115.2(1) . 5_666 no O5 K2 O5 88.5(1) 5_656 4_656 no O5 K2 O3 116.1(1) 5_656 . no O5 K2 O3 116.1(1) 4_656 . no O5 K2 O3w 158.7(1) 5_656 4_657 no O5 K2 O3w 90.5(1) 4_656 4_657 no O3 K2 O3w 83.2(1) . 4_657 no O5 K2 O3w 90.5(1) 5_656 5_657 no O5 K2 O3w 158.7(1) 4_656 5_657 no O3 K2 O3w 83.2(1) . 5_657 no O3w K2 O3w 82.8(1) 4_657 5_657 no O5 K2 O8 76.8(1) 5_656 . no O5 K2 O8 76.8(1) 4_656 . no O3 K2 O8 56.6(1) . . no O3w K2 O8 123.6(1) 4_657 . no O3w K2 O8 123.6(1) 5_657 . no O5 K2 O1w 70.0(1) 5_656 . no O5 K2 O1w 70.0(1) 4_656 . no O3 K2 O1w 170.6(1) . . no O3w K2 O1w 89.8(1) 4_657 . no O3w K2 O1w 89.8(1) 5_657 . no O8 K2 O1w 132.8(1) . . no O8 K2 K3 66.3(1) . 5_656 no O5 K2 K3 126.5(1) 5_656 5_657 no O8 K2 K3 142.4(1) . 5_657 no O2w K3 O3w 77.6(1) . 8 no O2w K3 O3w 77.6(1) . . no O3w K3 O3w 85.1(1) 8 . no O2w K3 O5 121.0(1) . 8 no O3w K3 O5 89.7(1) 8 8 no O3w K3 O5 159.1(1) . 8 no O2w K3 O5 121.0(1) . . no O3w K3 O5 159.1(1) 8 . no O3w K3 O5 89.7(1) . . no O5 K3 O5 88.1(1) 8 . no O2w K3 O4 81.3(1) . . no O3w K3 O4 158.8(1) 8 . no O3w K3 O4 92.0(1) . . no O5 K3 O4 99.9(1) 8 . no O5 K3 O4 41.3(1) . . no O2w K3 O4 81.3(1) . 8 no O3w K3 O4 92.0(1) 8 8 no O3w K3 O4 158.8(1) . 8 no O5 K3 O4 41.3(1) 8 8 no O5 K3 O4 99.9(1) . 8 no O4 K3 O4 83.2(1) . 8 no O5 K3 K1 122.7(1) 8 7_756 no C1 O1 Mo1 116.2(2) . . no C1 O1 K1 106.8(1) . . no Mo1 O1 K1 98.1(1) . . no C1 O1 K1 106.8(1) . 8_565 no Mo1 O1 K1 98.1(1) . 8_565 no K1 O1 K1 130.8(1) . 8_565 no C1 O2 K1 119.8(1) . 2_665 no C1 O2 K1 119.8(1) . 7_756 no K1 O2 K1 120.1(1) 2_665 7_756 no C2 O3 Mo1 123.8(2) . . no C2 O3 K2 134.5(2) . . no Mo1 O3 K2 101.8(1) . . no C4 O4 K1 124.3(2) . 7_756 no C4 O4 K1 134.6(2) . 8_565 no K1 O4 K1 87.5(1) 7_756 8_565 no C4 O4 K3 69.3(2) . . no K1 O4 K3 100.2(1) 7_756 . no K1 O4 K3 142.4(1) 8_565 . no C4 O5 K2 140.3(2) . 5_656 no C4 O5 K3 93.7(2) . . no K2 O5 K3 91.2(1) 5_656 . no O7 O6 Mo1 69.7(1) . . no O7 O6 K1 130.3(2) . 7_755 no Mo1 O6 K1 158.2(1) . 7_755 no O7 O6 K1 68.2(1) . 8_565 no Mo1 O6 K1 110.1(1) . 8_565 no K1 O6 K1 88.0(1) 7_755 8_565 no O6 O7 Mo1 66.0(1) . . no O6 O7 K1 81.7(1) . 8_565 no Mo1 O7 K1 115.5(1) . 8_565 no Mo1 O8 K2 108.4(1) . . no K2 O1w K1 129.1(1) . 4_646 no K2 O1w K1 129.1(1) . 5_666 no K1 O1w K1 97.9(1) 4_646 5_666 no K3 O3w K2 95.6(1) . 5_657 no O2 C1 O1 124.0(4) . . no O2 C1 C2 120.3(3) . . no O1 C1 C2 115.7(3) . . no O3 C2 C3 110.4(2) . . no O3 C2 C3 110.4(2) . 8_565 no C3 C2 C3 106.8(3) . 8_565 no O3 C2 C1 109.3(3) . . no C3 C2 C1 110.0(2) . . no C3 C2 C1 110.0(2) 8_565 . no C4 C3 C2 115.6(2) . . no O5 C4 O4 124.1(3) . . no O5 C4 C3 118.3(3) . . no O4 C4 C3 117.6(3) . . no K2 O1w H1w1 100(2) . . no K1 O1w H1w1 128(2) 4_646 . no K1 O1w H1w1 52(2) 5_666 . no K3 O2w H2w1 123(2) . . no K3 O3w H3w1 121(3) . . no K2 O3w H3w1 97(3) 5_657 . no K3 O3w H3w2 122(3) . . no K2 O3w H3w2 106(3) 5_657 . no H3w1 O3w H3w2 109(2) . . no C4 C3 H3a 108.4 . . no C2 C3 H3a 108.4 . . no C4 C3 H3b 108.4 . . no C2 C3 H3b 108.4 . . no H3a C3 H3b 107.4 . . no 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 O8 Mo1 O1 C1 0.0 . . . . no O6 Mo1 O1 C1 137.0(1) 8_565 . . . no O6 Mo1 O1 C1 -137.0(1) . . . . no O3 Mo1 O1 C1 0.0 . . . . no O7 Mo1 O1 C1 92.6(1) 8_565 . . . no O7 Mo1 O1 C1 -92.6(1) . . . . no O8 Mo1 O1 K1 -113.3(1) . . . . no O6 Mo1 O1 K1 23.7(1) 8_565 . . . no O6 Mo1 O1 K1 109.7(1) . . . . no O3 Mo1 O1 K1 -113.3(1) . . . . no O7 Mo1 O1 K1 -20.7(1) 8_565 . . . no O7 Mo1 O1 K1 154.1(1) . . . . no O8 Mo1 O1 K1 113.3(1) . . . 8_565 no O6 Mo1 O1 K1 -109.7(1) 8_565 . . 8_565 no O6 Mo1 O1 K1 -23.7(1) . . . 8_565 no O3 Mo1 O1 K1 113.3(1) . . . 8_565 no O7 Mo1 O1 K1 -154.1(1) 8_565 . . 8_565 no O7 Mo1 O1 K1 20.7(1) . . . 8_565 no O7 K1 O1 C1 -103.0(2) 8_565 . . . no O6 K1 O1 C1 42.5(2) 7_766 . . . no O2 K1 O1 C1 -142.8(3) 2_664 . . . no O4 K1 O1 C1 150.3(2) 7_765 . . . no O4 K1 O1 C1 -28.6(2) 8_565 . . . no O6 K1 O1 C1 -139.0(2) 8_565 . . . no O1w K1 O1 C1 -61.4(2) 5_666 . . . no O7 K1 O1 Mo1 17.64(7) 8_565 . . . no O6 K1 O1 Mo1 163.1(1) 7_766 . . . no O2 K1 O1 Mo1 -22.2(3) 2_664 . . . no O4 K1 O1 Mo1 -89.1(1) 7_765 . . . no O4 K1 O1 Mo1 92.0(1) 8_565 . . . no O6 K1 O1 Mo1 -18.4(1) 8_565 . . . no O1w K1 O1 Mo1 59.2(1) 5_666 . . . no O7 K1 O1 K1 125.7(1) 8_565 . . 8_565 no O6 K1 O1 K1 -88.9(1) 7_766 . . 8_565 no O2 K1 O1 K1 85.8(3) 2_664 . . 8_565 no O4 K1 O1 K1 18.9(1) 7_765 . . 8_565 no O4 K1 O1 K1 -160.0(1) 8_565 . . 8_565 no O6 K1 O1 K1 89.6(1) 8_565 . . 8_565 no O1w K1 O1 K1 167.3(1) 5_666 . . 8_565 no O8 Mo1 O3 C2 180.0 . . . . no O6 Mo1 O3 C2 -69.3(1) 8_565 . . . no O6 Mo1 O3 C2 69.3(1) . . . . no O7 Mo1 O3 C2 -81.4(1) 8_565 . . . no O7 Mo1 O3 C2 81.4(1) . . . . no O1 Mo1 O3 C2 0.0 . . . . no O8 Mo1 O3 K2 0.0 . . . . no O6 Mo1 O3 K2 110.7(1) 8_565 . . . no O6 Mo1 O3 K2 -110.7(1) . . . . no O7 Mo1 O3 K2 98.6(1) 8_565 . . . no O7 Mo1 O3 K2 -98.6(1) . . . . no O1 Mo1 O3 K2 180.0 . . . . no O5 K2 O3 C2 -129.0(1) 5_656 . . . no O5 K2 O3 C2 129.0(1) 4_656 . . . no O3w K2 O3 C2 41.8(1) 4_657 . . . no O3w K2 O3 C2 -41.8(1) 5_657 . . . no O8 K2 O3 C2 180.0 . . . . no O1w K2 O3 C2 0.0 . . . . no O5 K2 O3 Mo1 51.0(1) 5_656 . . . no O5 K2 O3 Mo1 -51.0(1) 4_656 . . . no O3w K2 O3 Mo1 -138.2(1) 4_657 . . . no O3w K2 O3 Mo1 138.2(1) 5_657 . . . no O8 K2 O3 Mo1 0.0 . . . . no O1w K2 O3 Mo1 180.0 . . . . no O2w K3 O4 C4 -136.8(2) . . . . no O3w K3 O4 C4 -141.2(2) 8 . . . no O3w K3 O4 C4 -59.7(2) . . . . no O5 K3 O4 C4 103.0(2) 8 . . . no O5 K3 O4 C4 27.5(2) . . . . no O4 K3 O4 C4 141.0(2) 8 . . . no O2w K3 O4 K1 -13.8(1) . . . 7_756 no O3w K3 O4 K1 -18.3(2) 8 . . 7_756 no O3w K3 O4 K1 63.3(1) . . . 7_756 no O5 K3 O4 K1 -134.0(1) 8 . . 7_756 no O5 K3 O4 K1 150.5(1) . . . 7_756 no O4 K3 O4 K1 -96.0(1) 8 . . 7_756 no O2w K3 O4 K1 85.5(2) . . . 8_565 no O3w K3 O4 K1 81.0(2) 8 . . 8_565 no O3w K3 O4 K1 162.6(1) . . . 8_565 no O5 K3 O4 K1 -34.7(1) 8 . . 8_565 no O5 K3 O4 K1 -110.2(2) . . . 8_565 no O4 K3 O4 K1 3.3(2) 8 . . 8_565 no O2w K3 O5 C4 -7.8(2) . . . . no O3w K3 O5 C4 142.6(2) 8 . . . no O3w K3 O5 C4 67.4(2) . . . . no O5 K3 O5 C4 -133.4(2) 8 . . . no O4 K3 O5 C4 -26.0(2) . . . . no O4 K3 O5 C4 -93.6(2) 8 . . . no O2w K3 O5 K2 132.8(1) . . . 5_656 no O3w K3 O5 K2 -76.8(2) 8 . . 5_656 no O3w K3 O5 K2 -152.0(1) . . . 5_656 no O5 K3 O5 K2 7.2(1) 8 . . 5_656 no O4 K3 O5 K2 114.6(1) . . . 5_656 no O4 K3 O5 K2 47.0(1) 8 . . 5_656 no O8 Mo1 O6 O7 -89.5(1) . . . . no O6 Mo1 O6 O7 168.6(1) 8_565 . . . no O3 Mo1 O6 O7 17.5(2) . . . . no O7 Mo1 O6 O7 158.3(2) 8_565 . . . no O1 Mo1 O6 O7 82.4(1) . . . . no O8 Mo1 O6 K1 69.5(3) . . . 7_755 no O6 Mo1 O6 K1 -32.4(3) 8_565 . . 7_755 no O3 Mo1 O6 K1 176.5(2) . . . 7_755 no O7 Mo1 O6 K1 -42.7(3) 8_565 . . 7_755 no O7 Mo1 O6 K1 159.0(4) . . . 7_755 no O1 Mo1 O6 K1 -118.7(3) . . . 7_755 no O8 Mo1 O6 K1 -145.7(1) . . . 8_565 no O6 Mo1 O6 K1 112.4(2) 8_565 . . 8_565 no O3 Mo1 O6 K1 -38.7(2) . . . 8_565 no O7 Mo1 O6 K1 102.1(1) 8_565 . . 8_565 no O7 Mo1 O6 K1 -56.2(1) . . . 8_565 no O1 Mo1 O6 K1 26.15(8) . . . 8_565 no K1 O6 O7 Mo1 -170.0(2) 7_755 . . . no K1 O6 O7 Mo1 122.8(1) 8_565 . . . no Mo1 O6 O7 K1 -122.8(1) . . . 8_565 no K1 O6 O7 K1 67.2(2) 7_755 . . 8_565 no O8 Mo1 O7 O6 99.2(1) . . . . no O6 Mo1 O7 O6 -14.7(1) 8_565 . . . no O3 Mo1 O7 O6 -167.4(1) . . . . no O7 Mo1 O7 O6 -75.1(4) 8_565 . . . no O1 Mo1 O7 O6 -92.7(1) . . . . no O8 Mo1 O7 K1 166.3(1) . . . 8_565 no O6 Mo1 O7 K1 52.4(1) 8_565 . . 8_565 no O6 Mo1 O7 K1 67.1(1) . . . 8_565 no O3 Mo1 O7 K1 -100.3(1) . . . 8_565 no O7 Mo1 O7 K1 -7.9(4) 8_565 . . 8_565 no O1 Mo1 O7 K1 -25.5(1) . . . 8_565 no O6 Mo1 O8 K2 -135.8(1) 8_565 . . . no O6 Mo1 O8 K2 135.8(1) . . . . no O3 Mo1 O8 K2 0.0 . . . . no O7 Mo1 O8 K2 -90.9(1) 8_565 . . . no O7 Mo1 O8 K2 90.9(1) . . . . no O1 Mo1 O8 K2 0.0 . . . . no O5 K2 O8 Mo1 -134.2(1) 5_656 . . . no O5 K2 O8 Mo1 134.2(1) 4_656 . . . no O3 K2 O8 Mo1 0.0 . . . . no O3w K2 O8 Mo1 52.5(1) 4_657 . . . no O3w K2 O8 Mo1 -52.5(1) 5_657 . . . no O1w K2 O8 Mo1 180.0 . . . . no O5 K2 O1w K1 55.8(1) 5_656 . . 4_646 no O5 K2 O1w K1 151.8(2) 4_656 . . 4_646 no O3 K2 O1w K1 -76.2(1) . . . 4_646 no O3w K2 O1w K1 -117.6(1) 4_657 . . 4_646 no O3w K2 O1w K1 -34.8(1) 5_657 . . 4_646 no O8 K2 O1w K1 103.8(1) . . . 4_646 no O5 K2 O1w K1 -151.8(2) 5_656 . . 5_666 no O5 K2 O1w K1 -55.8(1) 4_656 . . 5_666 no O3 K2 O1w K1 76.2(1) . . . 5_666 no O3w K2 O1w K1 34.8(1) 4_657 . . 5_666 no O3w K2 O1w K1 117.6(1) 5_657 . . 5_666 no O8 K2 O1w K1 -103.8(1) . . . 5_666 no O2w K3 O3w K2 -70.8(1) . . . 5_657 no O3w K3 O3w K2 7.5(1) 8 . . 5_657 no O5 K3 O3w K2 83.6(2) 8 . . 5_657 no O5 K3 O3w K2 167.3(1) . . . 5_657 no O4 K3 O3w K2 -151.5(1) . . . 5_657 no O4 K3 O3w K2 -75.3(2) 8 . . 5_657 no K1 O2 C1 O1 93.1(2) 2_665 . . . no K1 O2 C1 O1 -93.1(2) 7_756 . . . no K1 O2 C1 C2 -86.9(2) 2_665 . . . no K1 O2 C1 C2 86.9(2) 7_756 . . . no Mo1 O1 C1 O2 180.0 . . . . no K1 O1 C1 O2 -71.8(1) . . . . no K1 O1 C1 O2 71.8(1) 8_565 . . . no Mo1 O1 C1 C2 0.0 . . . . no K1 O1 C1 C2 108.2(1) . . . . no K1 O1 C1 C2 -108.2(1) 8_565 . . . no Mo1 O3 C2 C3 -121.1(2) . . . . no K2 O3 C2 C3 58.9(2) . . . . no Mo1 O3 C2 C3 121.1(2) . . . 8_565 no K2 O3 C2 C3 -58.9(2) . . . 8_565 no Mo1 O3 C2 C1 0.0 . . . . no K2 O3 C2 C1 180.0 . . . . no O2 C1 C2 O3 180.0 . . . . no O1 C1 C2 O3 0.0 . . . . no O2 C1 C2 C3 -58.7(2) . . . . no O1 C1 C2 C3 121.3(2) . . . . no O2 C1 C2 C3 58.7(2) . . . 8_565 no O1 C1 C2 C3 -121.3(2) . . . 8_565 no O3 C2 C3 C4 56.5(3) . . . . no C3 C2 C3 C4 176.5(2) 8_565 . . . no C1 C2 C3 C4 -64.2(3) . . . . no K2 O5 C4 O4 -29.1(4) 5_656 . . . no K3 O5 C4 O4 67.3(3) . . . . no K2 O5 C4 C3 153.9(2) 5_656 . . . no K3 O5 C4 C3 -109.6(2) . . . . no K1 O4 C4 O5 -143.5(2) 7_756 . . . no K1 O4 C4 O5 89.6(3) 8_565 . . . no K3 O4 C4 O5 -55.1(2) . . . . no K1 O4 C4 C3 33.4(3) 7_756 . . . no K1 O4 C4 C3 -93.4(3) 8_565 . . . no K3 O4 C4 C3 121.8(2) . . . . no C2 C3 C4 O5 -111.3(3) . . . . no C2 C3 C4 O4 71.5(3) . . . . no loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A _geom_hbond_publ_flag O1w H1w1 O4 0.85(1) 1.96(1) 2.804(3) 173(3) 4_656 yes O2w H2w1 O1 0.85(1) 2.63(3) 2.944(6) 103(2) 2_655 yes O2w H2w1 O2 0.85(1) 2.50(2) 2.883(6) 108(2) 2_655 yes O3w H3w2 O5 0.86(1) 1.97(1) 2.824(3) 171(4) 5_657 yes O3w H3w1 O7 0.85(1) 2.01(1) 2.847(3) 172(4) 1_556 yes _diffrn_measured_fraction_theta_max 0.99 _diffrn_reflns_theta_full 27.5 _diffrn_measured_fraction_theta_full 0.99 _refine_diff_density_max 0.57 _refine_diff_density_min -0.84 _refine_diff_density_rms 0.20