# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Enbo Wang' _publ_contact_author_email WANGENBO@PUBLIC.CC.JL.CN _publ_section_title ; Polyoxometalate-Based {MnIII2}-Schiff Base Composite Materials Exhibiting Single-Molecule Magnet Behaviour ; loop_ _publ_author_name 'Enbo Wang.' 'Rodolphe Clerac' 'Yang-Guang Li.' 'Ying Lu.' 'Yong-Hui Wang.' ; Qiong Wu ; # Attachment 'AlMo6-compound1.cif' data_1 _database_code_depnum_ccdc_archive 'CCDC 709702' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ; 2(C16H16N2O3Mn)+,Na+,(H6AlMo6O24)3-,20(H2O) ; _chemical_formula_sum 'C32 H78 Al Mn2 Mo6 N4 Na O50' _chemical_formula_weight 2054.47 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 '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 10.860(2) _cell_length_b 11.219(2) _cell_length_c 15.377(3) _cell_angle_alpha 105.62(3) _cell_angle_beta 98.15(3) _cell_angle_gamma 109.04(3) _cell_volume 1650.4(6) _cell_formula_units_Z 1 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 15754 _cell_measurement_theta_min 3.05 _cell_measurement_theta_max 27.50 _exptl_crystal_description block _exptl_crystal_colour brown _exptl_crystal_size_max 0.29 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.067 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1024 _exptl_absorpt_coefficient_mu 1.606 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6531 _exptl_absorpt_correction_T_max 0.6992 _exptl_absorpt_process_details 'ABSCOR by T.Higashi 8 March, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Rotation anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku R-AXIS RAPID IP' _diffrn_measurement_method Oscillation _diffrn_detector_area_resol_mean 0.01 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% none _diffrn_reflns_number 12709 _diffrn_reflns_av_R_equivalents 0.0571 _diffrn_reflns_av_sigmaI/netI 0.0757 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.06 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5566 _reflns_number_gt 4177 _reflns_threshold_expression >2sigma(I) _computing_data_collection PROCESS-AUTO _computing_cell_refinement PROCESS-AUTO _computing_data_reduction CrystalStructure _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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. During the refinement, the 'omit-3 50' command was used to omit the weak reflection data above 50 degree. The restraint command 'isor' was used to refine some O and C atoms with ADP problems, these atoms are as follows: C16, O37, o37a, o38, o38a, o39 and o39a. Furthermore, all the H atoms on OH and water molecules are found from the residual peaks and the O-H bonds are further fixed with the command 'DFIX 0.85 0.01 OXX HXX'. All these restraint refinement led to a relatively high restraint value 69. ; _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^)+(0.0150P)^2^+11.1244P] 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 5566 _refine_ls_number_parameters 520 _refine_ls_number_restraints 69 _refine_ls_R_factor_all 0.0719 _refine_ls_R_factor_gt 0.0470 _refine_ls_wR_factor_ref 0.1086 _refine_ls_wR_factor_gt 0.0975 _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_restrained_S_all 1.044 _refine_ls_shift/su_max 0.001 _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 0.70156(6) 0.52613(6) 0.36085(4) 0.01646(15) Uani 1 1 d . . . Mo2 Mo 0.81632(6) 0.72235(6) 0.58255(4) 0.01716(16) Uani 1 1 d . . . Mo3 Mo 0.61034(6) 0.69759(6) 0.72185(4) 0.01755(16) Uani 1 1 d . . . Al1 Al 0.5000 0.5000 0.5000 0.0121(6) Uani 1 2 d S . . O11 O 0.5929(5) 0.6848(4) 0.5690(3) 0.0156(10) Uani 1 1 d D . . H11A H 0.555(6) 0.736(6) 0.557(5) 0.019 Uiso 1 1 d D . . O12 O 0.4995(5) 0.5200(5) 0.3814(3) 0.0164(10) Uani 1 1 d D . . H12A H 0.482(7) 0.582(5) 0.367(5) 0.020 Uiso 1 1 d D . . O13 O 0.6750(5) 0.4995(4) 0.4994(3) 0.0150(10) Uani 1 1 d D . . H13A H 0.690(7) 0.436(5) 0.512(5) 0.018 Uiso 1 1 d D . . O14 O 0.8456(5) 0.4928(5) 0.3683(3) 0.0204(11) Uani 1 1 d . . . O15 O 0.9574(5) 0.6853(5) 0.5865(3) 0.0230(11) Uani 1 1 d . . . O16 O 0.5787(5) 0.3394(5) 0.3107(3) 0.0194(10) Uani 1 1 d . . . O17 O 0.6264(5) 0.6509(5) 0.8190(3) 0.0252(11) Uani 1 1 d . . . O18 O 0.6660(5) 0.8674(5) 0.7610(3) 0.0244(11) Uani 1 1 d . . . O19 O 0.8723(5) 0.8925(5) 0.6264(3) 0.0242(11) Uani 1 1 d . . . O20 O 0.7665(5) 0.6717(5) 0.6866(3) 0.0207(11) Uani 1 1 d . . . O21 O 0.6822(5) 0.5711(5) 0.2643(3) 0.0226(11) Uani 1 1 d . . . O22 O 0.7680(5) 0.7031(4) 0.4529(3) 0.0192(10) Uani 1 1 d . . . Mn1 Mn 0.93307(10) 0.61446(10) 1.01953(7) 0.0153(2) Uani 1 1 d . . . O1W O 0.7305(5) 0.6147(6) 0.9859(4) 0.0285(12) Uani 1 1 d D . . H111 H 0.682(6) 0.629(8) 1.023(3) 0.034 Uiso 1 1 d D . . H112 H 0.696(6) 0.612(8) 0.932(2) 0.034 Uiso 1 1 d D . . O1 O 0.8674(4) 0.4247(4) 0.9553(3) 0.0157(10) Uani 1 1 d . . . O2 O 0.9709(5) 0.6648(4) 0.9170(3) 0.0192(10) Uani 1 1 d . . . N1 N 0.9153(6) 0.5820(6) 1.1374(4) 0.0186(13) Uani 1 1 d . . . N2 N 1.0175(6) 0.8019(6) 1.1052(4) 0.0186(13) Uani 1 1 d . . . C1 C 0.7605(7) 0.3405(7) 0.9726(5) 0.0180(15) Uani 1 1 d . . . C2 C 0.6704(7) 0.2271(7) 0.9005(5) 0.0184(15) Uani 1 1 d . . . H2A H 0.6836 0.2105 0.8393 0.022 Uiso 1 1 calc R . . C3 C 0.5622(8) 0.1385(8) 0.9171(6) 0.0302(18) Uani 1 1 d . . . H3A H 0.5001 0.0627 0.8667 0.036 Uiso 1 1 calc R . . C4 C 0.5420(7) 0.1578(8) 1.0061(6) 0.0263(17) Uani 1 1 d . . . H4A H 0.4660 0.0968 1.0165 0.032 Uiso 1 1 calc R . . C5 C 0.6338(7) 0.2668(8) 1.0792(5) 0.0241(16) Uani 1 1 d . . . H5A H 0.6230 0.2788 1.1408 0.029 Uiso 1 1 calc R . . C6 C 0.7423(7) 0.3596(7) 1.0638(5) 0.0233(16) Uani 1 1 d . . . C7 C 0.8345(7) 0.4717(7) 1.1438(5) 0.0193(15) Uani 1 1 d . . . H7A H 0.8362 0.4643 1.2041 0.023 Uiso 1 1 calc R . . C8 C 1.0018(8) 0.6953(7) 1.2210(5) 0.0238(16) Uani 1 1 d . . . H8A H 1.0951 0.6986 1.2327 0.029 Uiso 1 1 calc R . . H8B H 0.9674 0.6885 1.2765 0.029 Uiso 1 1 calc R . . C9 C 0.9970(8) 0.8190(7) 1.1998(5) 0.0216(16) Uani 1 1 d . . . H9A H 0.9088 0.8258 1.2020 0.026 Uiso 1 1 calc R . . H9B H 1.0687 0.9012 1.2457 0.026 Uiso 1 1 calc R . . C10 C 1.0820(7) 0.9047(7) 1.0844(5) 0.0226(16) Uani 1 1 d . . . H10A H 1.1199 0.9890 1.1332 0.027 Uiso 1 1 calc R . . C11 C 1.1013(7) 0.9026(7) 0.9935(5) 0.0205(15) Uani 1 1 d . . . C12 C 1.1800(7) 1.0242(7) 0.9843(5) 0.0230(16) Uani 1 1 d . . . H12B H 1.2190 1.1027 1.0379 0.028 Uiso 1 1 calc R . . C13 C 1.2014(7) 1.0318(8) 0.9007(6) 0.0259(17) Uani 1 1 d . . . H13B H 1.2558 1.1141 0.8957 0.031 Uiso 1 1 calc R . . C14 C 1.1414(7) 0.9153(8) 0.8221(6) 0.0274(18) Uani 1 1 d . . . H14A H 1.1528 0.9204 0.7629 0.033 Uiso 1 1 calc R . . C15 C 1.0668(7) 0.7945(7) 0.8279(5) 0.0193(15) Uani 1 1 d . . . H15A H 1.0298 0.7167 0.7737 0.023 Uiso 1 1 calc R . . C16 C 1.0452(6) 0.7859(7) 0.9141(5) 0.0177(14) Uani 1 1 d U . . Na1 Na 1.0000 0.5000 0.5000 0.0291(10) Uani 1 2 d S . . O31 O 0.8327(6) 0.3702(6) 0.5574(4) 0.0309(13) Uani 1 1 d D . . H311 H 0.848(8) 0.403(6) 0.6166(11) 0.037 Uiso 1 1 d D . . H312 H 0.823(9) 0.288(3) 0.541(4) 0.037 Uiso 1 1 d D . . O32 O 0.8681(5) 0.9270(6) 0.3998(4) 0.0312(13) Uani 1 1 d D . . H321 H 0.857(6) 0.873(7) 0.430(5) 0.037 Uiso 1 1 d D . . H322 H 0.946(4) 0.949(8) 0.390(6) 0.037 Uiso 1 1 d D . . O33 O 0.8172(5) 0.4759(5) 0.7416(3) 0.0241(11) Uani 1 1 d D . . H331 H 0.865(6) 0.515(5) 0.797(2) 0.029 Uiso 1 1 d D . . H332 H 0.791(7) 0.528(5) 0.721(4) 0.029 Uiso 1 1 d D . . O34 O 0.5784(7) 0.6290(7) 1.1105(4) 0.0400(15) Uani 1 1 d D . . H341 H 0.595(9) 0.590(8) 1.148(4) 0.048 Uiso 1 1 d D . . H342 H 0.544(9) 0.684(7) 1.133(5) 0.048 Uiso 1 1 d D . . O35 O 0.6282(6) 0.8752(6) 0.2765(4) 0.0375(14) Uani 1 1 d D . . H351 H 0.701(5) 0.880(7) 0.309(5) 0.045 Uiso 1 1 d D . . H352 H 0.614(7) 0.946(5) 0.298(5) 0.045 Uiso 1 1 d D . . O36 O 0.5620(5) 0.2840(6) 0.6574(4) 0.0284(12) Uani 1 1 d D . . H361 H 0.502(4) 0.243(7) 0.680(4) 0.034 Uiso 1 1 d D . . H362 H 0.637(3) 0.329(7) 0.698(3) 0.034 Uiso 1 1 d D . . O37 O 0.5322(8) 0.1559(8) 0.4751(6) 0.026(2) Uani 0.70 1 d PU A 1 O37A O 0.463(2) 0.1148(19) 0.4669(14) 0.025(4) Uani 0.30 1 d PU B 2 O38 O 0.7035(9) 0.1725(9) 0.3520(6) 0.036(2) Uani 0.73 1 d PU C 1 O38A O 0.631(3) 0.123(2) 0.3511(16) 0.035(6) Uani 0.27 1 d PU D 2 O39 O 0.8621(10) 1.1325(11) 0.5534(7) 0.037(2) Uani 0.74 1 d PU E 1 O39A O 0.802(3) 1.113(3) 0.549(3) 0.043(9) Uani 0.26 1 d PU F 2 O40 O 0.6815(8) 1.0629(7) 0.6649(6) 0.067(2) Uani 1 1 d D . . H401 H 0.733(9) 1.086(10) 0.630(7) 0.080 Uiso 1 1 d D . . H402 H 0.691(10) 0.997(8) 0.679(8) 0.080 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 0.0176(3) 0.0229(3) 0.0135(3) 0.0079(3) 0.0055(2) 0.0114(3) Mo2 0.0167(3) 0.0183(3) 0.0156(3) 0.0060(3) 0.0024(2) 0.0060(3) Mo3 0.0207(3) 0.0196(3) 0.0113(3) 0.0039(2) 0.0022(2) 0.0082(3) Al1 0.0141(14) 0.0124(13) 0.0108(14) 0.0032(11) 0.0025(11) 0.0071(12) O11 0.019(2) 0.013(2) 0.017(3) 0.005(2) 0.002(2) 0.010(2) O12 0.020(2) 0.019(2) 0.014(2) 0.005(2) 0.005(2) 0.012(2) O13 0.018(2) 0.016(2) 0.013(2) 0.003(2) 0.0025(19) 0.010(2) O14 0.021(3) 0.026(3) 0.019(3) 0.007(2) 0.006(2) 0.015(2) O15 0.016(2) 0.031(3) 0.025(3) 0.012(2) 0.005(2) 0.010(2) O16 0.020(2) 0.025(3) 0.016(3) 0.004(2) 0.006(2) 0.014(2) O17 0.027(3) 0.036(3) 0.016(3) 0.009(2) 0.005(2) 0.017(2) O18 0.029(3) 0.019(3) 0.021(3) 0.005(2) 0.002(2) 0.007(2) O19 0.025(3) 0.016(2) 0.019(3) 0.003(2) -0.002(2) -0.002(2) O20 0.021(3) 0.022(3) 0.016(3) 0.002(2) -0.001(2) 0.011(2) O21 0.024(3) 0.029(3) 0.019(3) 0.010(2) 0.008(2) 0.014(2) O22 0.024(3) 0.016(2) 0.015(3) 0.006(2) 0.001(2) 0.004(2) Mn1 0.0175(5) 0.0149(5) 0.0128(5) 0.0038(4) 0.0031(4) 0.0064(4) O1W 0.030(3) 0.045(3) 0.025(3) 0.018(3) 0.010(2) 0.026(3) O1 0.014(2) 0.016(2) 0.014(2) 0.004(2) 0.0009(19) 0.003(2) O2 0.021(3) 0.016(2) 0.016(3) 0.003(2) 0.002(2) 0.006(2) N1 0.018(3) 0.019(3) 0.018(3) 0.003(3) 0.003(3) 0.010(3) N2 0.023(3) 0.019(3) 0.018(3) 0.006(3) 0.007(3) 0.013(3) C1 0.013(3) 0.022(4) 0.024(4) 0.011(3) 0.005(3) 0.011(3) C2 0.016(3) 0.020(4) 0.020(4) 0.009(3) 0.002(3) 0.008(3) C3 0.024(4) 0.025(4) 0.033(5) 0.012(4) -0.006(3) 0.002(4) C4 0.016(4) 0.026(4) 0.043(5) 0.021(4) 0.012(3) 0.005(3) C5 0.025(4) 0.033(4) 0.029(4) 0.020(4) 0.016(3) 0.019(4) C6 0.022(4) 0.026(4) 0.032(4) 0.017(4) 0.010(3) 0.014(3) C7 0.015(3) 0.027(4) 0.021(4) 0.005(3) 0.005(3) 0.016(3) C8 0.026(4) 0.026(4) 0.015(4) 0.002(3) -0.002(3) 0.012(3) C9 0.031(4) 0.022(4) 0.017(4) 0.006(3) 0.008(3) 0.015(3) C10 0.018(4) 0.026(4) 0.028(4) 0.007(3) 0.006(3) 0.014(3) C11 0.017(4) 0.022(4) 0.023(4) 0.008(3) 0.001(3) 0.009(3) C12 0.020(4) 0.016(4) 0.033(4) 0.010(3) 0.003(3) 0.006(3) C13 0.020(4) 0.025(4) 0.039(5) 0.022(4) 0.010(3) 0.007(3) C14 0.025(4) 0.038(5) 0.030(5) 0.026(4) 0.009(3) 0.013(4) C15 0.018(3) 0.019(4) 0.020(4) 0.009(3) 0.001(3) 0.005(3) C16 0.010(3) 0.023(3) 0.022(3) 0.007(3) 0.000(2) 0.011(3) Na1 0.030(2) 0.047(3) 0.028(2) 0.023(2) 0.017(2) 0.026(2) O31 0.036(3) 0.033(3) 0.036(3) 0.019(3) 0.013(3) 0.021(3) O32 0.030(3) 0.037(3) 0.037(3) 0.023(3) 0.014(3) 0.015(3) O33 0.032(3) 0.028(3) 0.015(3) 0.006(2) 0.001(2) 0.018(3) O34 0.053(4) 0.060(4) 0.034(4) 0.027(3) 0.019(3) 0.042(4) O35 0.025(3) 0.042(3) 0.052(4) 0.029(3) 0.003(3) 0.013(3) O36 0.024(3) 0.033(3) 0.031(3) 0.016(3) 0.003(2) 0.011(3) O37 0.016(4) 0.014(4) 0.042(5) 0.011(3) 0.001(4) -0.002(3) O37A 0.038(9) 0.012(8) 0.028(8) 0.011(6) 0.003(7) 0.011(7) O38 0.042(5) 0.032(5) 0.039(5) 0.008(4) 0.014(4) 0.023(4) O38A 0.042(9) 0.032(9) 0.033(9) 0.010(7) 0.008(7) 0.019(8) O39 0.042(5) 0.037(5) 0.039(5) 0.015(4) 0.011(5) 0.022(5) O39A 0.041(12) 0.039(11) 0.056(12) 0.016(8) 0.013(9) 0.022(9) O40 0.077(6) 0.049(5) 0.078(6) 0.031(4) 0.025(5) 0.019(4) _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 O21 1.700(5) . ? Mo1 O14 1.719(5) . ? Mo1 O22 1.931(5) . ? Mo1 O16 1.944(5) . ? Mo1 O12 2.243(5) . ? Mo1 O13 2.273(4) . ? Mo2 O19 1.704(5) . ? Mo2 O15 1.711(5) . ? Mo2 O22 1.922(5) . ? Mo2 O20 1.926(5) . ? Mo2 O11 2.291(5) . ? Mo2 O13 2.336(5) . ? Mo3 O18 1.698(5) . ? Mo3 O17 1.716(5) . ? Mo3 O16 1.918(5) 2_666 ? Mo3 O20 1.937(5) . ? Mo3 O11 2.293(5) . ? Mo3 O12 2.319(5) 2_666 ? Al1 O11 1.895(5) . ? Al1 O11 1.895(5) 2_666 ? Al1 O12 1.896(4) 2_666 ? Al1 O12 1.896(4) . ? Al1 O13 1.904(5) . ? Al1 O13 1.904(5) 2_666 ? O11 H11A 0.846(10) . ? O12 Mo3 2.319(5) 2_666 ? O12 H12A 0.847(10) . ? O13 H13A 0.846(10) . ? O14 Na1 2.404(5) . ? O15 Na1 2.370(5) . ? O16 Mo3 1.918(5) 2_666 ? Mn1 O2 1.867(5) . ? Mn1 O1 1.922(5) . ? Mn1 N1 1.966(6) . ? Mn1 N2 1.976(6) . ? Mn1 O1W 2.189(5) . ? Mn1 O1 2.348(5) 2_767 ? O1W H111 0.848(10) . ? O1W H112 0.850(10) . ? O1 C1 1.349(8) . ? O1 Mn1 2.348(5) 2_767 ? O2 C16 1.351(8) . ? N1 C7 1.301(9) . ? N1 C8 1.466(9) . ? N2 C10 1.288(9) . ? N2 C9 1.473(8) . ? C1 C2 1.388(10) . ? C1 C6 1.412(10) . ? C2 C3 1.376(10) . ? C2 H2A 0.9500 . ? C3 C4 1.387(11) . ? C3 H3A 0.9500 . ? C4 C5 1.378(11) . ? C4 H4A 0.9500 . ? C5 C6 1.393(10) . ? C5 H5A 0.9500 . ? C6 C7 1.447(10) . ? C7 H7A 0.9500 . ? C8 C9 1.524(9) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 C11 1.437(10) . ? C10 H10A 0.9500 . ? C11 C16 1.409(10) . ? C11 C12 1.410(9) . ? C12 C13 1.358(10) . ? C12 H12B 0.9500 . ? C13 C14 1.402(11) . ? C13 H13B 0.9500 . ? C14 C15 1.368(10) . ? C14 H14A 0.9500 . ? C15 C16 1.401(9) . ? C15 H15A 0.9500 . ? Na1 O15 2.370(5) 2_766 ? Na1 O31 2.372(5) . ? Na1 O31 2.372(5) 2_766 ? Na1 O14 2.404(5) 2_766 ? O31 H311 0.852(10) . ? O31 H312 0.851(10) . ? O32 H321 0.849(10) . ? O32 H322 0.852(10) . ? O33 H331 0.848(10) . ? O33 H332 0.846(10) . ? O34 H341 0.848(10) . ? O34 H342 0.848(10) . ? O35 H351 0.851(10) . ? O35 H352 0.851(10) . ? O36 H361 0.847(10) . ? O36 H362 0.849(11) . ? O40 H401 0.853(11) . ? O40 H402 0.853(10) . ? 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 O21 Mo1 O14 105.9(2) . . ? O21 Mo1 O22 97.7(2) . . ? O14 Mo1 O22 100.8(2) . . ? O21 Mo1 O16 100.3(2) . . ? O14 Mo1 O16 95.3(2) . . ? O22 Mo1 O16 151.53(19) . . ? O21 Mo1 O12 93.2(2) . . ? O14 Mo1 O12 159.22(18) . . ? O22 Mo1 O12 84.30(19) . . ? O16 Mo1 O12 72.91(18) . . ? O21 Mo1 O13 160.1(2) . . ? O14 Mo1 O13 93.26(19) . . ? O22 Mo1 O13 72.95(17) . . ? O16 Mo1 O13 82.85(18) . . ? O12 Mo1 O13 68.76(16) . . ? O19 Mo2 O15 106.0(2) . . ? O19 Mo2 O22 97.4(2) . . ? O15 Mo2 O22 100.1(2) . . ? O19 Mo2 O20 102.1(2) . . ? O15 Mo2 O20 97.7(2) . . ? O22 Mo2 O20 148.7(2) . . ? O19 Mo2 O11 95.7(2) . . ? O15 Mo2 O11 157.59(19) . . ? O22 Mo2 O11 82.20(18) . . ? O20 Mo2 O11 71.80(18) . . ? O19 Mo2 O13 160.3(2) . . ? O15 Mo2 O13 92.3(2) . . ? O22 Mo2 O13 71.63(17) . . ? O20 Mo2 O13 82.20(18) . . ? O11 Mo2 O13 67.11(16) . . ? O18 Mo3 O17 106.4(2) . . ? O18 Mo3 O16 97.6(2) . 2_666 ? O17 Mo3 O16 101.8(2) . 2_666 ? O18 Mo3 O20 100.9(2) . . ? O17 Mo3 O20 96.3(2) . . ? O16 Mo3 O20 149.2(2) 2_666 . ? O18 Mo3 O11 93.1(2) . . ? O17 Mo3 O11 158.9(2) . . ? O16 Mo3 O11 83.18(18) 2_666 . ? O20 Mo3 O11 71.58(18) . . ? O18 Mo3 O12 158.2(2) . 2_666 ? O17 Mo3 O12 94.6(2) . 2_666 ? O16 Mo3 O12 71.57(19) 2_666 2_666 ? O20 Mo3 O12 82.39(19) . 2_666 ? O11 Mo3 O12 67.27(16) . 2_666 ? O11 Al1 O11 180.000(1) . 2_666 ? O11 Al1 O12 84.74(19) . 2_666 ? O11 Al1 O12 95.26(19) 2_666 2_666 ? O11 Al1 O12 95.26(19) . . ? O11 Al1 O12 84.74(19) 2_666 . ? O12 Al1 O12 180.000(1) 2_666 . ? O11 Al1 O13 84.7(2) . . ? O11 Al1 O13 95.3(2) 2_666 . ? O12 Al1 O13 95.67(19) 2_666 . ? O12 Al1 O13 84.33(19) . . ? O11 Al1 O13 95.3(2) . 2_666 ? O11 Al1 O13 84.7(2) 2_666 2_666 ? O12 Al1 O13 84.33(19) 2_666 2_666 ? O12 Al1 O13 95.67(19) . 2_666 ? O13 Al1 O13 180.000(1) . 2_666 ? Al1 O11 Mo2 105.1(2) . . ? Al1 O11 Mo3 104.50(19) . . ? Mo2 O11 Mo3 92.39(17) . . ? Al1 O11 H11A 116(5) . . ? Mo2 O11 H11A 125(5) . . ? Mo3 O11 H11A 110(5) . . ? Al1 O12 Mo1 104.1(2) . . ? Al1 O12 Mo3 103.48(19) . 2_666 ? Mo1 O12 Mo3 92.72(17) . 2_666 ? Al1 O12 H12A 123(5) . . ? Mo1 O12 H12A 111(5) . . ? Mo3 O12 H12A 118(5) 2_666 . ? Al1 O13 Mo1 102.76(19) . . ? Al1 O13 Mo2 103.12(19) . . ? Mo1 O13 Mo2 91.93(16) . . ? Al1 O13 H13A 115(5) . . ? Mo1 O13 H13A 119(5) . . ? Mo2 O13 H13A 121(5) . . ? Mo1 O14 Na1 131.1(2) . . ? Mo2 O15 Na1 133.0(3) . . ? Mo3 O16 Mo1 117.5(2) 2_666 . ? Mo2 O20 Mo3 117.8(2) . . ? Mo2 O22 Mo1 118.7(2) . . ? O2 Mn1 O1 96.0(2) . . ? O2 Mn1 N1 172.4(2) . . ? O1 Mn1 N1 90.0(2) . . ? O2 Mn1 N2 92.2(2) . . ? O1 Mn1 N2 169.1(2) . . ? N1 Mn1 N2 81.3(2) . . ? O2 Mn1 O1W 90.9(2) . . ? O1 Mn1 O1W 91.5(2) . . ? N1 Mn1 O1W 93.7(2) . . ? N2 Mn1 O1W 95.5(2) . . ? O2 Mn1 O1 91.21(18) . 2_767 ? O1 Mn1 O1 79.05(19) . 2_767 ? N1 Mn1 O1 85.3(2) . 2_767 ? N2 Mn1 O1 93.7(2) . 2_767 ? O1W Mn1 O1 170.5(2) . 2_767 ? Mn1 O1W H111 128(4) . . ? Mn1 O1W H112 121(4) . . ? H111 O1W H112 111.0(19) . . ? C1 O1 Mn1 120.5(4) . . ? C1 O1 Mn1 115.9(4) . 2_767 ? Mn1 O1 Mn1 100.95(19) . 2_767 ? C16 O2 Mn1 129.5(4) . . ? C7 N1 C8 121.2(6) . . ? C7 N1 Mn1 124.8(5) . . ? C8 N1 Mn1 114.1(4) . . ? C10 N2 C9 120.0(6) . . ? C10 N2 Mn1 126.2(5) . . ? C9 N2 Mn1 113.8(4) . . ? O1 C1 C2 119.5(6) . . ? O1 C1 C6 121.7(7) . . ? C2 C1 C6 118.7(6) . . ? C3 C2 C1 120.4(7) . . ? C3 C2 H2A 119.8 . . ? C1 C2 H2A 119.8 . . ? C2 C3 C4 121.3(8) . . ? C2 C3 H3A 119.4 . . ? C4 C3 H3A 119.4 . . ? C5 C4 C3 119.0(7) . . ? C5 C4 H4A 120.5 . . ? C3 C4 H4A 120.5 . . ? C4 C5 C6 120.7(7) . . ? C4 C5 H5A 119.6 . . ? C6 C5 H5A 119.6 . . ? C5 C6 C1 119.8(7) . . ? C5 C6 C7 117.7(7) . . ? C1 C6 C7 122.5(6) . . ? N1 C7 C6 123.3(6) . . ? N1 C7 H7A 118.4 . . ? C6 C7 H7A 118.4 . . ? N1 C8 C9 105.0(6) . . ? N1 C8 H8A 110.8 . . ? C9 C8 H8A 110.8 . . ? N1 C8 H8B 110.8 . . ? C9 C8 H8B 110.8 . . ? H8A C8 H8B 108.8 . . ? N2 C9 C8 106.0(6) . . ? N2 C9 H9A 110.5 . . ? C8 C9 H9A 110.5 . . ? N2 C9 H9B 110.5 . . ? C8 C9 H9B 110.5 . . ? H9A C9 H9B 108.7 . . ? N2 C10 C11 125.4(7) . . ? N2 C10 H10A 117.3 . . ? C11 C10 H10A 117.3 . . ? C16 C11 C12 118.9(7) . . ? C16 C11 C10 123.2(7) . . ? C12 C11 C10 117.8(7) . . ? C13 C12 C11 121.8(7) . . ? C13 C12 H12B 119.1 . . ? C11 C12 H12B 119.1 . . ? C12 C13 C14 118.3(7) . . ? C12 C13 H13B 120.8 . . ? C14 C13 H13B 120.8 . . ? C15 C14 C13 122.1(7) . . ? C15 C14 H14A 119.0 . . ? C13 C14 H14A 119.0 . . ? C14 C15 C16 119.8(7) . . ? C14 C15 H15A 120.1 . . ? C16 C15 H15A 120.1 . . ? O2 C16 C15 118.0(6) . . ? O2 C16 C11 122.9(6) . . ? C15 C16 C11 119.1(6) . . ? O15 Na1 O15 180.000(1) . 2_766 ? O15 Na1 O31 85.63(18) . . ? O15 Na1 O31 94.37(18) 2_766 . ? O15 Na1 O31 94.37(18) . 2_766 ? O15 Na1 O31 85.63(18) 2_766 2_766 ? O31 Na1 O31 180.000(1) . 2_766 ? O15 Na1 O14 93.89(17) . 2_766 ? O15 Na1 O14 86.11(16) 2_766 2_766 ? O31 Na1 O14 84.42(17) . 2_766 ? O31 Na1 O14 95.58(18) 2_766 2_766 ? O15 Na1 O14 86.11(16) . . ? O15 Na1 O14 93.89(17) 2_766 . ? O31 Na1 O14 95.58(18) . . ? O31 Na1 O14 84.42(17) 2_766 . ? O14 Na1 O14 180.000(1) 2_766 . ? Na1 O31 H311 112(5) . . ? Na1 O31 H312 113(5) . . ? H311 O31 H312 110.4(18) . . ? H321 O32 H322 110.6(19) . . ? H331 O33 H332 111.6(19) . . ? H341 O34 H342 111.2(19) . . ? H351 O35 H352 110.5(19) . . ? H361 O36 H362 111.3(19) . . ? H401 O40 H402 110.8(19) . . ? 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 O11 H11A O37A 0.846(10) 1.87(3) 2.681(19) 159(7) 2_666 O11 H11A O37 0.846(10) 1.888(15) 2.733(10) 178(8) 2_666 O12 H12A O36 0.847(10) 1.835(13) 2.682(7) 177(7) 2_666 O13 H13A O31 0.846(10) 2.04(4) 2.779(7) 146(7) . O1W H111 O34 0.848(10) 1.872(19) 2.707(7) 168(7) . O1W H112 O17 0.850(10) 2.01(2) 2.841(7) 167(8) . O31 H311 O33 0.852(10) 2.00(3) 2.812(8) 160(8) . O31 H312 O39A 0.851(10) 1.95(4) 2.76(4) 160(6) 1_545 O31 H312 O39 0.851(10) 1.98(4) 2.773(12) 155(7) 1_545 O32 H321 O22 0.849(10) 1.99(3) 2.781(7) 156(8) . O32 H322 O19 0.852(10) 2.28(4) 3.042(7) 149(6) 2_776 O32 H322 O39 0.852(10) 2.66(5) 3.238(12) 127(5) 2_776 O33 H331 O2 0.848(10) 2.00(3) 2.809(7) 159(5) . O33 H332 O20 0.846(10) 1.903(18) 2.739(6) 169(6) . O34 H341 O21 0.848(10) 2.00(4) 2.799(7) 158(8) 1_556 O34 H342 O35 0.848(10) 2.43(7) 3.045(9) 130(7) 1_556 O35 H351 O32 0.851(10) 1.94(2) 2.781(8) 168(7) . O35 H352 O38A 0.851(10) 1.86(3) 2.69(2) 165(8) 1_565 O35 H352 O38 0.851(10) 2.26(5) 3.001(10) 146(7) 1_565 O36 H361 O35 0.847(10) 1.926(18) 2.766(8) 171(8) 2_666 O36 H362 O33 0.849(11) 1.98(3) 2.753(8) 150(6) . O40 H401 O39A 0.853(11) 1.58(4) 2.43(3) 168(13) . O40 H401 O39 0.853(11) 1.990(19) 2.841(13) 175(8) . O40 H402 O18 0.853(10) 2.15(4) 2.932(8) 153(8) . _diffrn_measured_fraction_theta_max 0.957 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.957 _refine_diff_density_max 0.811 _refine_diff_density_min -0.958 _refine_diff_density_rms 0.161 # Attachment 'CrMo6-Compound_2.cif' data_2 _database_code_depnum_ccdc_archive 'CCDC 709703' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ; 2(C16H16N2O3Mn)+,Na+,(H6CrMo6O24)3-,20(H2O) ; _chemical_formula_sum 'C32 H78 Cr Mn2 Mo6 N4 Na O50' _chemical_formula_weight 2079.49 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cr Cr 0.3209 0.6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 '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' Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.896(2) _cell_length_b 11.223(2) _cell_length_c 15.417(3) _cell_angle_alpha 105.47(3) _cell_angle_beta 98.24(3) _cell_angle_gamma 109.18(3) _cell_volume 1660.0(6) _cell_formula_units_Z 1 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour brown _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.23 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.080 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1035 _exptl_absorpt_coefficient_mu 1.738 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6418 _exptl_absorpt_correction_T_max 0.6906 _exptl_absorpt_process_details 'ABSCOR by T.Higashi 8 March, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Rotation anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku R-AXIS RAPID IP' _diffrn_measurement_method Oscillation _diffrn_detector_area_resol_mean 0.01 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% none _diffrn_reflns_number 12844 _diffrn_reflns_av_R_equivalents 0.0240 _diffrn_reflns_av_sigmaI/netI 0.0336 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.05 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5772 _reflns_number_gt 5064 _reflns_threshold_expression >2sigma(I) _computing_data_collection PROCESS-AUTO _computing_cell_refinement PROCESS-AUTO _computing_data_reduction CrystalStructure _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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. The restraint command 'isor' was used to refine some O atoms with ADP problems, these atoms are as follows: O37, o37a, o38, o38a, o39 and o39a. Furthermore, all the H atoms on OH and water molecules are found from the residual peaks and the O-H bonds are further fixed with the command 'DFIX 0.85 0.01 OXX HXX'. All these restraint refinement lead to a relatively high restraint value 63. ; _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^)+(0.0275P)^2^+2.8651P] 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 5772 _refine_ls_number_parameters 520 _refine_ls_number_restraints 63 _refine_ls_R_factor_all 0.0333 _refine_ls_R_factor_gt 0.0266 _refine_ls_wR_factor_ref 0.0681 _refine_ls_wR_factor_gt 0.0654 _refine_ls_goodness_of_fit_ref 1.063 _refine_ls_restrained_S_all 1.061 _refine_ls_shift/su_max 0.001 _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 0.11101(3) 0.19851(3) 0.722757(18) 0.01685(8) Uani 1 1 d . . . Mo2 Mo -0.20271(3) -0.02654(3) 0.639634(18) 0.01575(8) Uani 1 1 d . . . Mo3 Mo 0.31793(3) 0.22336(3) 0.582884(19) 0.01621(8) Uani 1 1 d . . . Cr1 Cr 0.0000 0.0000 0.5000 0.01249(15) Uani 1 2 d S . . O11 O -0.1810(2) -0.0004(2) 0.50037(15) 0.0152(5) Uani 1 1 d D . . H111 H -0.203(4) 0.060(3) 0.488(3) 0.018 Uiso 1 1 d D . . O12 O 0.0006(2) -0.0202(2) 0.62303(15) 0.0145(5) Uani 1 1 d D . . H121 H 0.027(4) -0.077(3) 0.636(2) 0.017 Uiso 1 1 d D . . O13 O 0.0972(2) 0.1920(2) 0.57196(15) 0.0154(5) Uani 1 1 d D . . H131 H 0.067(4) 0.247(3) 0.560(2) 0.019 Uiso 1 1 d D . . O14 O -0.0784(2) 0.1602(2) 0.68989(15) 0.0181(5) Uani 1 1 d . . . O15 O -0.1855(3) -0.0730(2) 0.73615(16) 0.0236(5) Uani 1 1 d . . . O16 O 0.2682(2) 0.2030(2) 0.45246(15) 0.0193(5) Uani 1 1 d . . . O17 O 0.3751(3) 0.3934(2) 0.62590(17) 0.0252(6) Uani 1 1 d . . . O18 O 0.1277(3) 0.1521(3) 0.81969(16) 0.0272(6) Uani 1 1 d . . . O19 O -0.3450(3) 0.0082(2) 0.63224(16) 0.0231(5) Uani 1 1 d . . . O20 O 0.1671(3) 0.3687(2) 0.76260(17) 0.0274(6) Uani 1 1 d . . . O21 O 0.4587(3) 0.1863(2) 0.58740(16) 0.0236(5) Uani 1 1 d . . . O22 O 0.2666(2) 0.1725(2) 0.68614(15) 0.0192(5) Uani 1 1 d . . . Mn1 Mn 0.43332(5) 0.11451(5) 1.01925(3) 0.01506(12) Uani 1 1 d . . . O1W O 0.2313(3) 0.1161(3) 0.98636(18) 0.0282(6) Uani 1 1 d D . . H1WA H 0.190(3) 0.114(4) 0.9346(13) 0.034 Uiso 1 1 d D . . H1WB H 0.186(3) 0.122(4) 1.0260(18) 0.034 Uiso 1 1 d D . . O1 O 0.4709(2) 0.1652(2) 0.91620(15) 0.0193(5) Uani 1 1 d . . . O2 O 0.3674(2) -0.0751(2) 0.95510(15) 0.0162(5) Uani 1 1 d . . . N1 N 0.5175(3) 0.3023(3) 1.10413(18) 0.0181(6) Uani 1 1 d . . . N2 N 0.4146(3) 0.0813(3) 1.13719(19) 0.0178(6) Uani 1 1 d . . . C1 C 0.6017(4) 0.4017(3) 0.9923(2) 0.0205(7) Uani 1 1 d . . . C2 C 0.5445(3) 0.2846(3) 0.9133(2) 0.0179(7) Uani 1 1 d . . . C3 C 0.5669(4) 0.2942(4) 0.8275(3) 0.0242(8) Uani 1 1 d . . . H3A H 0.5298 0.2165 0.7734 0.029 Uiso 1 1 calc R . . C4 C 0.6428(4) 0.4161(4) 0.8213(3) 0.0277(8) Uani 1 1 d . . . H4A H 0.6556 0.4212 0.7625 0.033 Uiso 1 1 calc R . . C5 C 0.7008(4) 0.5314(4) 0.8994(3) 0.0288(8) Uani 1 1 d . . . H5A H 0.7545 0.6140 0.8944 0.035 Uiso 1 1 calc R . . C6 C 0.6796(4) 0.5242(3) 0.9834(3) 0.0257(8) Uani 1 1 d . . . H6A H 0.7179 0.6029 1.0368 0.031 Uiso 1 1 calc R . . C7 C 0.5811(4) 0.4046(3) 1.0828(2) 0.0211(7) Uani 1 1 d . . . H7A H 0.6177 0.4893 1.1309 0.025 Uiso 1 1 calc R . . C8 C 0.2428(4) -0.1400(3) 1.0634(2) 0.0205(7) Uani 1 1 d . . . C9 C 0.2609(3) -0.1589(3) 0.9726(2) 0.0181(7) Uani 1 1 d . . . C10 C 0.1693(4) -0.2725(3) 0.9003(2) 0.0231(8) Uani 1 1 d . . . H10A H 0.1812 -0.2888 0.8389 0.028 Uiso 1 1 calc R . . C11 C 0.0613(4) -0.3613(4) 0.9177(3) 0.0295(9) Uani 1 1 d . . . H11A H -0.0011 -0.4375 0.8678 0.035 Uiso 1 1 calc R . . C12 C 0.0424(4) -0.3407(4) 1.0071(3) 0.0305(9) Uani 1 1 d . . . H12A H -0.0330 -0.4014 1.0181 0.037 Uiso 1 1 calc R . . C13 C 0.1340(4) -0.2320(4) 1.0791(3) 0.0265(8) Uani 1 1 d . . . H13A H 0.1231 -0.2191 1.1405 0.032 Uiso 1 1 calc R . . C14 C 0.3358(4) -0.0270(3) 1.1431(2) 0.0197(7) Uani 1 1 d . . . H14A H 0.3378 -0.0345 1.2032 0.024 Uiso 1 1 calc R . . C15 C 0.4984(4) 0.3189(3) 1.1990(2) 0.0247(8) Uani 1 1 d . . . H15A H 0.4110 0.3266 1.2020 0.030 Uiso 1 1 calc R . . H15B H 0.5709 0.4008 1.2445 0.030 Uiso 1 1 calc R . . C16 C 0.5022(4) 0.1956(3) 1.2204(2) 0.0221(8) Uani 1 1 d . . . H16A H 0.5951 0.1984 1.2318 0.027 Uiso 1 1 calc R . . H16B H 0.4684 0.1894 1.2759 0.027 Uiso 1 1 calc R . . Na1 Na 0.5000 0.0000 0.5000 0.0288(5) Uani 1 2 d S . . O31 O 0.3327(3) -0.1309(3) 0.55817(19) 0.0312(6) Uani 1 1 d D . . H311 H 0.327(5) -0.2109(18) 0.542(2) 0.037 Uiso 1 1 d D . . H312 H 0.340(5) -0.100(3) 0.6163(10) 0.037 Uiso 1 1 d D . . O32 O 0.0624(3) -0.2163(3) 0.65833(19) 0.0301(6) Uani 1 1 d D . . H321 H 0.1391(19) -0.168(4) 0.696(2) 0.036 Uiso 1 1 d D . . H322 H 0.012(3) -0.266(3) 0.682(2) 0.036 Uiso 1 1 d D . . O33 O 0.0781(4) 0.1281(3) 1.1099(2) 0.0437(8) Uani 1 1 d D . . H331 H 0.110(5) 0.102(4) 1.152(2) 0.052 Uiso 1 1 d D . . H332 H 0.071(5) 0.202(3) 1.135(3) 0.052 Uiso 1 1 d D . . O34 O 0.3664(3) 0.4272(3) 0.3996(2) 0.0347(6) Uani 1 1 d D . . H341 H 0.349(4) 0.356(3) 0.414(3) 0.042 Uiso 1 1 d D . . H342 H 0.4491(15) 0.463(4) 0.403(3) 0.042 Uiso 1 1 d D . . O35 O 0.3172(3) -0.0232(3) 0.74104(17) 0.0276(6) Uani 1 1 d D . . H351 H 0.363(4) 0.006(3) 0.7961(12) 0.033 Uiso 1 1 d D . . H352 H 0.289(4) 0.033(3) 0.728(2) 0.033 Uiso 1 1 d D . . O36 O 0.1263(3) 0.3753(3) 0.2772(2) 0.0439(8) Uani 1 1 d D . . H361 H 0.204(2) 0.386(4) 0.306(3) 0.053 Uiso 1 1 d D . . H362 H 0.114(4) 0.448(3) 0.290(3) 0.053 Uiso 1 1 d D . . O37 O 0.3610(6) 0.6334(6) 0.5535(4) 0.0425(13) Uani 0.72 1 d PU A 1 O37A O 0.2912(17) 0.6022(16) 0.5425(13) 0.056(5) Uani 0.28 1 d PU B 2 O38 O 0.0311(5) -0.3459(5) 0.4738(4) 0.0319(12) Uani 0.70 1 d PU C 1 O38A O -0.0340(14) -0.3832(11) 0.4687(9) 0.032(3) Uani 0.30 1 d PU D 2 O39 O 0.2020(6) -0.3263(5) 0.3519(4) 0.0428(12) Uani 0.72 1 d PU E 1 O39A O 0.1323(16) -0.3768(13) 0.3501(10) 0.044(3) Uani 0.28 1 d PU F 2 O40 O -0.1831(5) -0.5647(4) 0.3336(3) 0.0778(13) Uani 1 1 d D . . H401 H -0.186(6) -0.502(4) 0.311(3) 0.078 Uiso 1 1 d D . . H402 H -0.127(5) -0.525(4) 0.388(2) 0.078 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 0.01977(17) 0.01926(15) 0.01036(14) 0.00281(11) 0.00225(11) 0.00844(12) Mo2 0.01749(16) 0.02161(15) 0.01233(14) 0.00735(12) 0.00589(11) 0.01051(12) Mo3 0.01677(16) 0.01637(14) 0.01458(14) 0.00516(11) 0.00318(11) 0.00562(12) Cr1 0.0154(4) 0.0141(3) 0.0094(3) 0.0039(3) 0.0032(3) 0.0076(3) O11 0.0182(13) 0.0167(11) 0.0149(11) 0.0075(9) 0.0046(9) 0.0101(10) O12 0.0169(12) 0.0182(11) 0.0125(10) 0.0070(9) 0.0039(9) 0.0102(10) O13 0.0194(13) 0.0146(11) 0.0146(11) 0.0055(9) 0.0026(9) 0.0095(10) O14 0.0223(13) 0.0199(11) 0.0140(11) 0.0035(9) 0.0049(9) 0.0122(10) O15 0.0277(15) 0.0327(13) 0.0180(12) 0.0132(11) 0.0085(10) 0.0162(12) O16 0.0214(13) 0.0216(12) 0.0172(11) 0.0095(10) 0.0054(10) 0.0083(10) O17 0.0255(15) 0.0201(12) 0.0244(12) 0.0055(10) 0.0041(11) 0.0041(11) O18 0.0291(15) 0.0402(15) 0.0158(12) 0.0110(11) 0.0052(10) 0.0167(12) O19 0.0213(14) 0.0323(13) 0.0211(12) 0.0119(11) 0.0078(10) 0.0136(11) O20 0.0302(16) 0.0206(12) 0.0238(13) 0.0002(10) 0.0016(11) 0.0084(11) O21 0.0190(14) 0.0296(13) 0.0212(12) 0.0077(11) 0.0032(10) 0.0095(11) O22 0.0177(13) 0.0254(12) 0.0149(11) 0.0071(10) 0.0018(9) 0.0098(10) Mn1 0.0186(3) 0.0135(2) 0.0117(2) 0.00366(19) 0.00396(19) 0.0049(2) O1W 0.0272(16) 0.0445(16) 0.0240(13) 0.0192(13) 0.0086(11) 0.0204(13) O1 0.0239(14) 0.0168(11) 0.0151(11) 0.0064(9) 0.0056(10) 0.0042(10) O2 0.0167(13) 0.0150(10) 0.0160(11) 0.0053(9) 0.0061(9) 0.0041(9) N1 0.0212(16) 0.0179(13) 0.0147(13) 0.0034(11) 0.0027(11) 0.0091(12) N2 0.0196(16) 0.0200(14) 0.0156(13) 0.0054(12) 0.0046(11) 0.0103(12) C1 0.0163(18) 0.0202(16) 0.0251(17) 0.0093(15) 0.0026(14) 0.0070(14) C2 0.0138(17) 0.0186(16) 0.0234(17) 0.0103(14) 0.0032(13) 0.0069(14) C3 0.023(2) 0.0253(18) 0.0246(18) 0.0115(15) 0.0056(15) 0.0079(15) C4 0.023(2) 0.035(2) 0.032(2) 0.0225(18) 0.0079(16) 0.0093(17) C5 0.022(2) 0.0242(18) 0.044(2) 0.0195(18) 0.0099(17) 0.0066(16) C6 0.021(2) 0.0169(16) 0.036(2) 0.0075(15) 0.0026(16) 0.0058(15) C7 0.0193(19) 0.0169(16) 0.0231(17) 0.0020(14) 0.0017(14) 0.0075(14) C8 0.0216(19) 0.0232(17) 0.0233(17) 0.0117(15) 0.0089(14) 0.0123(15) C9 0.0154(18) 0.0166(15) 0.0235(17) 0.0078(14) 0.0048(14) 0.0070(14) C10 0.022(2) 0.0209(17) 0.0224(17) 0.0063(15) -0.0001(14) 0.0065(15) C11 0.020(2) 0.0224(18) 0.037(2) 0.0102(16) -0.0034(16) 0.0013(15) C12 0.019(2) 0.030(2) 0.046(2) 0.0216(18) 0.0099(17) 0.0061(16) C13 0.026(2) 0.0264(18) 0.036(2) 0.0159(17) 0.0162(17) 0.0121(16) C14 0.024(2) 0.0251(18) 0.0179(16) 0.0093(14) 0.0116(14) 0.0150(15) C15 0.035(2) 0.0235(17) 0.0150(16) 0.0020(14) 0.0048(15) 0.0141(16) C16 0.029(2) 0.0256(17) 0.0111(15) 0.0039(14) 0.0049(14) 0.0117(16) Na1 0.0275(12) 0.0444(12) 0.0281(10) 0.0183(10) 0.0116(9) 0.0239(10) O31 0.0401(18) 0.0338(14) 0.0316(14) 0.0159(12) 0.0138(13) 0.0230(14) O32 0.0289(16) 0.0311(14) 0.0350(15) 0.0191(12) 0.0061(12) 0.0119(12) O33 0.060(2) 0.065(2) 0.0350(16) 0.0302(16) 0.0219(16) 0.0455(19) O34 0.0281(16) 0.0314(15) 0.0446(16) 0.0194(13) 0.0083(13) 0.0065(13) O35 0.0330(16) 0.0278(13) 0.0210(12) 0.0062(11) -0.0006(11) 0.0153(12) O36 0.0349(19) 0.0488(18) 0.0540(19) 0.0321(16) 0.0057(15) 0.0140(15) O37 0.053(4) 0.037(3) 0.041(3) 0.015(2) 0.012(3) 0.018(3) O37A 0.054(8) 0.039(7) 0.083(8) 0.023(6) 0.019(7) 0.026(6) O38 0.031(3) 0.025(3) 0.038(2) 0.013(2) 0.002(2) 0.009(2) O38A 0.054(7) 0.018(5) 0.033(5) 0.014(4) 0.013(6) 0.020(5) O39 0.053(3) 0.038(3) 0.045(3) 0.014(2) 0.015(3) 0.026(2) O39A 0.060(8) 0.040(6) 0.051(6) 0.021(5) 0.018(6) 0.035(6) O40 0.083(4) 0.060(2) 0.082(3) 0.022(2) 0.003(3) 0.026(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 O20 1.703(2) . ? Mo1 O18 1.714(2) . ? Mo1 O14 1.924(2) . ? Mo1 O22 1.946(2) . ? Mo1 O13 2.288(2) . ? Mo1 O12 2.314(2) . ? Mo2 O15 1.709(2) . ? Mo2 O19 1.715(2) . ? Mo2 O16 1.930(2) 2_556 ? Mo2 O14 1.948(3) . ? Mo2 O12 2.246(2) . ? Mo2 O11 2.278(2) . ? Mo3 O17 1.702(2) . ? Mo3 O21 1.713(3) . ? Mo3 O22 1.924(2) . ? Mo3 O16 1.936(2) . ? Mo3 O13 2.287(2) . ? Mo3 O11 2.328(3) 2_556 ? Cr1 O12 1.969(2) 2_556 ? Cr1 O12 1.969(2) . ? Cr1 O13 1.970(2) . ? Cr1 O13 1.970(2) 2_556 ? Cr1 O11 1.971(2) 2_556 ? Cr1 O11 1.971(2) . ? O11 Mo3 2.328(3) 2_556 ? O11 H111 0.846(10) . ? O12 H121 0.843(10) . ? O13 H131 0.845(10) . ? O16 Mo2 1.930(2) 2_556 ? O19 Na1 2.414(3) 1_455 ? O21 Na1 2.383(3) . ? Mn1 O1 1.879(2) . ? Mn1 O2 1.921(2) . ? Mn1 N2 1.976(3) . ? Mn1 N1 1.977(3) . ? Mn1 O1W 2.194(3) . ? Mn1 O2 2.355(2) 2_657 ? O1W H1WA 0.850(10) . ? O1W H1WB 0.843(10) . ? O1 C2 1.333(4) . ? O2 C9 1.346(4) . ? O2 Mn1 2.355(2) 2_657 ? N1 C7 1.285(5) . ? N1 C15 1.478(4) . ? N2 C14 1.272(4) . ? N2 C16 1.473(4) . ? C1 C2 1.411(5) . ? C1 C6 1.412(5) . ? C1 C7 1.439(5) . ? C2 C3 1.404(5) . ? C3 C4 1.384(5) . ? C3 H3A 0.9500 . ? C4 C5 1.392(6) . ? C4 H4A 0.9500 . ? C5 C6 1.367(6) . ? C5 H5A 0.9500 . ? C6 H6A 0.9500 . ? C7 H7A 0.9500 . ? C8 C13 1.394(5) . ? C8 C9 1.411(5) . ? C8 C14 1.453(5) . ? C9 C10 1.397(5) . ? C10 C11 1.383(5) . ? C10 H10A 0.9500 . ? C11 C12 1.393(6) . ? C11 H11A 0.9500 . ? C12 C13 1.369(6) . ? C12 H12A 0.9500 . ? C13 H13A 0.9500 . ? C14 H14A 0.9500 . ? C15 C16 1.517(5) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? Na1 O21 2.383(3) 2_656 ? Na1 O31 2.387(3) 2_656 ? Na1 O31 2.387(3) . ? Na1 O19 2.414(3) 2_556 ? Na1 O19 2.414(3) 1_655 ? O31 H311 0.843(10) . ? O31 H312 0.852(10) . ? O32 H321 0.849(10) . ? O32 H322 0.848(10) . ? O33 H331 0.852(10) . ? O33 H332 0.851(10) . ? O34 H341 0.851(10) . ? O34 H342 0.845(10) . ? O35 H351 0.839(10) . ? O35 H352 0.843(10) . ? O36 H361 0.846(10) . ? O36 H362 0.845(10) . ? O40 H401 0.874(10) . ? O40 H402 0.869(10) . ? 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 O20 Mo1 O18 105.89(13) . . ? O20 Mo1 O14 98.01(12) . . ? O18 Mo1 O14 101.92(12) . . ? O20 Mo1 O22 101.11(12) . . ? O18 Mo1 O22 96.64(11) . . ? O14 Mo1 O22 148.50(9) . . ? O20 Mo1 O13 92.03(11) . . ? O18 Mo1 O13 160.03(10) . . ? O14 Mo1 O13 83.82(9) . . ? O22 Mo1 O13 70.77(9) . . ? O20 Mo1 O12 159.68(10) . . ? O18 Mo1 O12 93.39(11) . . ? O14 Mo1 O12 71.22(9) . . ? O22 Mo1 O12 82.56(9) . . ? O13 Mo1 O12 70.13(8) . . ? O15 Mo2 O19 105.66(12) . . ? O15 Mo2 O16 97.60(11) . 2_556 ? O19 Mo2 O16 101.50(12) . 2_556 ? O15 Mo2 O14 100.68(11) . . ? O19 Mo2 O14 95.15(11) . . ? O16 Mo2 O14 150.90(10) 2_556 . ? O15 Mo2 O12 92.34(11) . . ? O19 Mo2 O12 159.92(10) . . ? O16 Mo2 O12 84.51(10) 2_556 . ? O14 Mo2 O12 72.36(9) . . ? O15 Mo2 O11 161.41(10) . . ? O19 Mo2 O11 91.90(10) . . ? O16 Mo2 O11 72.43(9) 2_556 . ? O14 Mo2 O11 83.42(9) . . ? O12 Mo2 O11 71.46(9) . . ? O17 Mo3 O21 105.58(13) . . ? O17 Mo3 O22 102.58(11) . . ? O21 Mo3 O22 97.95(11) . . ? O17 Mo3 O16 97.43(11) . . ? O21 Mo3 O16 100.52(11) . . ? O22 Mo3 O16 147.92(10) . . ? O17 Mo3 O13 94.57(11) . . ? O21 Mo3 O13 158.93(10) . . ? O22 Mo3 O13 71.15(9) . . ? O16 Mo3 O13 82.56(10) . . ? O17 Mo3 O11 161.47(11) . 2_556 ? O21 Mo3 O11 91.14(11) . 2_556 ? O22 Mo3 O11 82.50(9) . 2_556 ? O16 Mo3 O11 71.18(9) . 2_556 ? O13 Mo3 O11 69.95(8) . 2_556 ? O12 Cr1 O12 180.000(1) 2_556 . ? O12 Cr1 O13 95.70(10) 2_556 . ? O12 Cr1 O13 84.30(10) . . ? O12 Cr1 O13 84.30(10) 2_556 2_556 ? O12 Cr1 O13 95.70(10) . 2_556 ? O13 Cr1 O13 180.0 . 2_556 ? O12 Cr1 O11 84.22(10) 2_556 2_556 ? O12 Cr1 O11 95.78(10) . 2_556 ? O13 Cr1 O11 84.31(10) . 2_556 ? O13 Cr1 O11 95.69(10) 2_556 2_556 ? O12 Cr1 O11 95.78(10) 2_556 . ? O12 Cr1 O11 84.22(10) . . ? O13 Cr1 O11 95.69(10) . . ? O13 Cr1 O11 84.31(10) 2_556 . ? O11 Cr1 O11 180.0 2_556 . ? Cr1 O11 Mo2 101.56(10) . . ? Cr1 O11 Mo3 102.13(10) . 2_556 ? Mo2 O11 Mo3 92.80(9) . 2_556 ? Cr1 O11 H111 121(3) . . ? Mo2 O11 H111 116(3) . . ? Mo3 O11 H111 119(3) 2_556 . ? Cr1 O12 Mo2 102.75(10) . . ? Cr1 O12 Mo1 102.36(10) . . ? Mo2 O12 Mo1 93.61(9) . . ? Cr1 O12 H121 120(3) . . ? Mo2 O12 H121 118(3) . . ? Mo1 O12 H121 116(3) . . ? Cr1 O13 Mo3 103.61(10) . . ? Cr1 O13 Mo1 103.21(10) . . ? Mo3 O13 Mo1 93.54(9) . . ? Cr1 O13 H131 119(3) . . ? Mo3 O13 H131 121(3) . . ? Mo1 O13 H131 112(3) . . ? Mo1 O14 Mo2 118.29(12) . . ? Mo2 O16 Mo3 119.22(12) 2_556 . ? Mo2 O19 Na1 130.96(12) . 1_455 ? Mo3 O21 Na1 132.57(13) . . ? Mo3 O22 Mo1 118.90(12) . . ? O1 Mn1 O2 95.90(10) . . ? O1 Mn1 N2 172.72(12) . . ? O2 Mn1 N2 89.94(11) . . ? O1 Mn1 N1 92.04(11) . . ? O2 Mn1 N1 169.50(11) . . ? N2 Mn1 N1 81.66(12) . . ? O1 Mn1 O1W 90.87(11) . . ? O2 Mn1 O1W 91.86(11) . . ? N2 Mn1 O1W 93.29(11) . . ? N1 Mn1 O1W 94.89(12) . . ? O1 Mn1 O2 91.48(10) . 2_657 ? O2 Mn1 O2 79.04(10) . 2_657 ? N2 Mn1 O2 85.34(10) . 2_657 ? N1 Mn1 O2 93.92(11) . 2_657 ? O1W Mn1 O2 170.79(10) . 2_657 ? Mn1 O1W H1WA 126(2) . . ? Mn1 O1W H1WB 123(2) . . ? H1WA O1W H1WB 111.1(18) . . ? C2 O1 Mn1 129.5(2) . . ? C9 O2 Mn1 120.26(19) . . ? C9 O2 Mn1 115.84(19) . 2_657 ? Mn1 O2 Mn1 100.96(10) . 2_657 ? C7 N1 C15 120.4(3) . . ? C7 N1 Mn1 126.1(2) . . ? C15 N1 Mn1 113.5(2) . . ? C14 N2 C16 121.9(3) . . ? C14 N2 Mn1 124.7(2) . . ? C16 N2 Mn1 113.4(2) . . ? C2 C1 C6 119.7(3) . . ? C2 C1 C7 123.1(3) . . ? C6 C1 C7 117.2(3) . . ? O1 C2 C3 118.5(3) . . ? O1 C2 C1 123.2(3) . . ? C3 C2 C1 118.4(3) . . ? C4 C3 C2 120.4(3) . . ? C4 C3 H3A 119.8 . . ? C2 C3 H3A 119.8 . . ? C3 C4 C5 121.3(3) . . ? C3 C4 H4A 119.3 . . ? C5 C4 H4A 119.3 . . ? C6 C5 C4 119.1(3) . . ? C6 C5 H5A 120.4 . . ? C4 C5 H5A 120.4 . . ? C5 C6 C1 121.1(3) . . ? C5 C6 H6A 119.4 . . ? C1 C6 H6A 119.4 . . ? N1 C7 C1 125.5(3) . . ? N1 C7 H7A 117.2 . . ? C1 C7 H7A 117.2 . . ? C13 C8 C9 120.1(3) . . ? C13 C8 C14 117.8(3) . . ? C9 C8 C14 122.1(3) . . ? O2 C9 C10 119.5(3) . . ? O2 C9 C8 121.9(3) . . ? C10 C9 C8 118.5(3) . . ? C11 C10 C9 120.2(3) . . ? C11 C10 H10A 119.9 . . ? C9 C10 H10A 119.9 . . ? C10 C11 C12 121.1(3) . . ? C10 C11 H11A 119.5 . . ? C12 C11 H11A 119.5 . . ? C13 C12 C11 119.2(4) . . ? C13 C12 H12A 120.4 . . ? C11 C12 H12A 120.4 . . ? C12 C13 C8 120.9(4) . . ? C12 C13 H13A 119.6 . . ? C8 C13 H13A 119.6 . . ? N2 C14 C8 123.9(3) . . ? N2 C14 H14A 118.0 . . ? C8 C14 H14A 118.0 . . ? N1 C15 C16 106.6(3) . . ? N1 C15 H15A 110.4 . . ? C16 C15 H15A 110.4 . . ? N1 C15 H15B 110.4 . . ? C16 C15 H15B 110.4 . . ? H15A C15 H15B 108.6 . . ? N2 C16 C15 105.3(3) . . ? N2 C16 H16A 110.7 . . ? C15 C16 H16A 110.7 . . ? N2 C16 H16B 110.7 . . ? C15 C16 H16B 110.7 . . ? H16A C16 H16B 108.8 . . ? O21 Na1 O21 180.000(1) . 2_656 ? O21 Na1 O31 94.32(9) . 2_656 ? O21 Na1 O31 85.68(9) 2_656 2_656 ? O21 Na1 O31 85.68(9) . . ? O21 Na1 O31 94.32(9) 2_656 . ? O31 Na1 O31 180.00(12) 2_656 . ? O21 Na1 O19 86.70(9) . 2_556 ? O21 Na1 O19 93.30(9) 2_656 2_556 ? O31 Na1 O19 84.25(9) 2_656 2_556 ? O31 Na1 O19 95.75(9) . 2_556 ? O21 Na1 O19 93.30(9) . 1_655 ? O21 Na1 O19 86.70(9) 2_656 1_655 ? O31 Na1 O19 95.75(9) 2_656 1_655 ? O31 Na1 O19 84.25(9) . 1_655 ? O19 Na1 O19 180.000(1) 2_556 1_655 ? Na1 O31 H311 111(3) . . ? Na1 O31 H312 116(3) . . ? H311 O31 H312 111.0(18) . . ? H321 O32 H322 111.3(17) . . ? H331 O33 H332 110.0(17) . . ? H341 O34 H342 110.5(18) . . ? H351 O35 H352 112.7(18) . . ? H361 O36 H362 111.5(18) . . ? H401 O40 H402 106.7(17) . . ? 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 O11 H111 O31 0.846(10) 1.97(2) 2.757(4) 154(4) 2_556 O12 H121 O32 0.843(10) 1.827(12) 2.665(3) 173(4) . O13 H131 O38A 0.845(10) 1.820(17) 2.654(12) 169(4) 2_556 O13 H131 O38 0.845(10) 1.882(14) 2.719(6) 170(4) 2_556 O1W H1WA O18 0.850(10) 2.006(14) 2.840(4) 166(4) . O1W H1WB O33 0.843(10) 1.869(11) 2.711(4) 177(4) . O31 H312 O35 0.852(10) 1.974(14) 2.809(4) 166(4) . O31 H311 O37 0.843(10) 1.95(2) 2.746(6) 158(4) 1_545 O31 H311 O37A 0.843(10) 2.00(2) 2.815(16) 161(3) 1_545 O32 H321 O35 0.849(10) 1.959(16) 2.755(4) 156(3) . O32 H322 O36 0.848(10) 1.904(12) 2.742(4) 169(4) 2_556 O33 H331 O15 0.852(10) 1.959(14) 2.802(4) 170(4) 2_557 O33 H332 O36 0.851(10) 2.35(3) 3.076(5) 143(3) 1_556 O34 H341 O16 0.851(10) 1.948(13) 2.778(4) 165(4) . O34 H342 O17 0.845(10) 2.251(18) 3.026(4) 153(3) 2_666 O35 H351 O1 0.839(10) 2.06(2) 2.811(4) 149(3) . O35 H352 O22 0.843(10) 1.915(15) 2.738(4) 165(4) . O36 H361 O34 0.846(10) 1.956(17) 2.783(4) 165(5) . O36 H362 O39A 0.845(10) 1.87(2) 2.684(13) 162(4) 1_565 O36 H362 O39 0.845(10) 2.26(3) 3.013(6) 149(4) 1_565 O40 H401 O20 0.874(10) 2.080(18) 2.939(5) 167(6) 2_556 O40 H402 O38A 0.869(10) 1.62(3) 2.391(13) 147(5) . O40 H402 O38 0.869(10) 2.10(3) 2.847(7) 144(5) . _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 0.667 _refine_diff_density_min -0.775 _refine_diff_density_rms 0.107