# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2014 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_3 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H32 Ag3 Al Mo6 N2 O34' _chemical_formula_weight 1722.67 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' Ag Ag -0.8971 1.1015 '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' Mo Mo -1.6832 0.6857 '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' _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 10.0978(8) _cell_length_b 10.5238(8) _cell_length_c 10.7062(8) _cell_angle_alpha 87.9400(10) _cell_angle_beta 73.8280(10) _cell_angle_gamma 63.0990(10) _cell_volume 969.05(13) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5533 _cell_measurement_theta_min 1.99 _cell_measurement_theta_max 25.00 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.952 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 820 _exptl_absorpt_coefficient_mu 3.494 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.577 _exptl_absorpt_correction_T_max 0.635 _exptl_absorpt_process_details 'ABSCOR by T.Higashi 8 March, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart Apex CCD' _diffrn_measurement_method \w-2\q _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 5533 _diffrn_reflns_av_R_equivalents 0.0122 _diffrn_reflns_av_unetI/netI 0.0210 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 1.99 _diffrn_reflns_theta_max 25.00 _reflns_number_total 3356 _reflns_number_gt 3183 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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 command 'omit-3 50' was used to omit the weak reflections above 50 degree. The hydrogen atoms of OW1, OW2 and OW3 are located from the residual peak. The restraint command 'dfix' was used to restrain the distances between O atoms and hydrogen atoms, and angles on water molecules. All these restrained refinement led to a restraint value of 9. ; _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^)+(0.0341P)^2^+1.3220P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens . _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3356 _refine_ls_number_parameters 307 _refine_ls_number_restraints 9 _refine_ls_R_factor_all 0.0244 _refine_ls_R_factor_gt 0.0226 _refine_ls_wR_factor_ref 0.0611 _refine_ls_wR_factor_gt 0.0599 _refine_ls_goodness_of_fit_ref 1.076 _refine_ls_restrained_S_all 1.075 _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 -0.40732(4) 0.76038(3) 0.70604(3) 0.01313(9) Uani 1 1 d . . . Mo2 Mo -0.14884(3) 0.72003(3) 0.41827(3) 0.01364(9) Uani 1 1 d . . . Mo3 Mo -0.24581(4) 0.96424(3) 0.21489(3) 0.01358(9) Uani 1 1 d . . . Ag1 Ag 0.24109(4) 0.60262(4) 0.48517(3) 0.03304(11) Uani 1 1 d . . . Ag2 Ag -0.5000 1.0000 1.0000 0.02850(12) Uani 1 2 d S . . Al1 Al -0.5000 1.0000 0.5000 0.0109(3) Uani 1 2 d S . . O1 O -0.5066(3) 0.9939(2) 0.6777(2) 0.0121(5) Uani 1 1 d . . . O2 O -0.4123(3) 0.7968(3) 0.4904(2) 0.0130(5) Uani 1 1 d . . . O3 O -0.2894(3) 0.9682(3) 0.4362(2) 0.0137(5) Uani 1 1 d . . . O4 O -0.6259(3) 0.8291(3) 0.7396(2) 0.0157(5) Uani 1 1 d . . . O5 O -0.2160(3) 0.7585(3) 0.6074(2) 0.0149(5) Uani 1 1 d . . . O6 O -0.1898(3) 0.7701(3) 0.2548(2) 0.0157(5) Uani 1 1 d . . . O7 O -0.3954(3) 0.7872(3) 0.8587(3) 0.0202(6) Uani 1 1 d . . . O8 O -0.3564(3) 0.5813(3) 0.6821(3) 0.0200(6) Uani 1 1 d . . . O9 O -0.1063(3) 0.5437(3) 0.4017(3) 0.0207(6) Uani 1 1 d . . . O10 O 0.0248(3) 0.7248(3) 0.3950(3) 0.0221(6) Uani 1 1 d . . . O11 O -0.0729(3) 0.9672(3) 0.1864(3) 0.0223(6) Uani 1 1 d . . . O12 O -0.7334(3) 1.0548(3) 0.9364(3) 0.0208(6) Uani 1 1 d . . . O13 O -0.6086(3) 0.8858(3) 1.2145(3) 0.0230(6) Uani 1 1 d . . . O14 O -0.5224(3) 0.6978(3) 1.3282(3) 0.0263(6) Uani 1 1 d . . . C1 C -0.5844(4) 0.7600(4) 1.2422(4) 0.0181(8) Uani 1 1 d . . . C2 C -0.6348(5) 0.6806(4) 1.1687(4) 0.0209(8) Uani 1 1 d . . . H2A H -0.6063 0.5849 1.1811 0.025 Uiso 1 1 calc R . . C3 C -0.7175(4) 0.7389(4) 1.0872(4) 0.0186(8) Uani 1 1 d . . . H3A H -0.7413 0.8332 1.0716 0.022 Uiso 1 1 calc R . . C4 C -0.7746(4) 0.6640(4) 1.0192(4) 0.0176(8) Uani 1 1 d . . . C5 C -0.8773(5) 0.7418(4) 0.9496(4) 0.0207(8) Uani 1 1 d . . . H5A H -0.9100 0.8397 0.9480 0.025 Uiso 1 1 calc R . . C6 C -0.8858(5) 0.5374(5) 0.8802(4) 0.0260(9) Uani 1 1 d . . . H6A H -0.9226 0.4963 0.8315 0.031 Uiso 1 1 calc R . . C7 C -0.7859(5) 0.4545(5) 0.9479(4) 0.0266(9) Uani 1 1 d . . . H7A H -0.7550 0.3567 0.9464 0.032 Uiso 1 1 calc R . . C8 C -0.7314(5) 0.5172(4) 1.0188(4) 0.0220(9) Uani 1 1 d . . . H8A H -0.6653 0.4615 1.0666 0.026 Uiso 1 1 calc R . . N1 N -0.9299(4) 0.6774(4) 0.8845(3) 0.0232(8) Uani 1 1 d . . . H1A H -0.9952 0.7289 0.8437 0.028 Uiso 1 1 calc R . . OW1 O 0.3450(4) 0.5902(3) 0.6504(3) 0.0296(7) Uani 1 1 d D . . OW2 O -0.1373(4) 1.1188(4) 0.4707(4) 0.0376(8) Uani 1 1 d D . . OW3 O 0.0938(3) 0.1351(3) 0.2627(3) 0.0269(7) Uani 1 1 d D . . H1 H 0.406(5) 0.509(2) 0.662(5) 0.042(16) Uiso 1 1 d D . . H2 H 0.364(5) 0.659(3) 0.656(5) 0.030(13) Uiso 1 1 d D . . H3 H -0.080(5) 1.106(6) 0.393(2) 0.054(18) Uiso 1 1 d D . . H4 H -0.098(7) 1.111(8) 0.532(4) 0.10(3) Uiso 1 1 d D . . H5 H 0.111(6) 0.192(5) 0.299(6) 0.07(2) Uiso 1 1 d D . . H6 H 0.164(5) 0.060(3) 0.220(5) 0.051(18) 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 0.01807(17) 0.01051(16) 0.01262(17) 0.00220(12) -0.00666(13) -0.00695(13) Mo2 0.01462(17) 0.01178(17) 0.01406(17) 0.00102(12) -0.00578(13) -0.00478(13) Mo3 0.01561(17) 0.01398(17) 0.01200(17) 0.00185(12) -0.00455(13) -0.00727(13) Ag1 0.0406(2) 0.02595(19) 0.0330(2) -0.00261(15) -0.01735(16) -0.01149(16) Ag2 0.0316(3) 0.0278(3) 0.0253(2) -0.00582(19) -0.0136(2) -0.0094(2) Al1 0.0132(7) 0.0095(7) 0.0109(7) 0.0017(6) -0.0048(6) -0.0053(6) O1 0.0167(12) 0.0099(12) 0.0115(12) 0.0018(10) -0.0060(10) -0.0066(10) O2 0.0168(12) 0.0103(12) 0.0119(12) 0.0010(10) -0.0057(10) -0.0054(10) O3 0.0147(12) 0.0132(13) 0.0138(13) 0.0014(10) -0.0049(10) -0.0065(10) O4 0.0178(13) 0.0129(13) 0.0186(14) 0.0021(11) -0.0052(11) -0.0088(11) O5 0.0163(13) 0.0163(13) 0.0136(13) 0.0024(10) -0.0072(10) -0.0072(11) O6 0.0211(13) 0.0121(13) 0.0138(13) 0.0011(10) -0.0075(11) -0.0061(11) O7 0.0283(15) 0.0188(14) 0.0149(14) 0.0012(11) -0.0099(12) -0.0099(12) O8 0.0252(14) 0.0124(13) 0.0231(15) 0.0024(11) -0.0079(12) -0.0087(11) O9 0.0261(14) 0.0138(14) 0.0195(14) 0.0008(11) -0.0076(12) -0.0063(12) O10 0.0186(14) 0.0268(15) 0.0225(15) 0.0039(12) -0.0077(12) -0.0109(12) O11 0.0191(14) 0.0212(15) 0.0259(15) 0.0029(12) -0.0048(12) -0.0099(12) O12 0.0251(14) 0.0203(14) 0.0151(14) -0.0004(11) -0.0066(11) -0.0084(12) O13 0.0340(16) 0.0184(15) 0.0273(15) 0.0060(12) -0.0188(13) -0.0157(13) O14 0.0401(17) 0.0223(15) 0.0258(16) 0.0053(12) -0.0212(14) -0.0158(13) C1 0.0175(18) 0.021(2) 0.0165(19) -0.0019(16) -0.0037(15) -0.0098(16) C2 0.030(2) 0.020(2) 0.021(2) 0.0056(17) -0.0113(17) -0.0177(18) C3 0.0220(19) 0.0159(19) 0.021(2) 0.0025(16) -0.0087(16) -0.0102(16) C4 0.024(2) 0.020(2) 0.0138(19) 0.0002(15) -0.0058(16) -0.0137(17) C5 0.023(2) 0.021(2) 0.019(2) 0.0015(16) -0.0064(16) -0.0108(17) C6 0.031(2) 0.036(3) 0.019(2) -0.0061(18) -0.0022(18) -0.024(2) C7 0.034(2) 0.023(2) 0.027(2) -0.0016(18) -0.0043(19) -0.0188(19) C8 0.026(2) 0.021(2) 0.022(2) 0.0046(17) -0.0083(17) -0.0125(18) N1 0.0239(18) 0.035(2) 0.0172(17) 0.0046(15) -0.0106(14) -0.0164(16) OW1 0.0365(18) 0.0242(18) 0.0385(19) 0.0051(15) -0.0200(15) -0.0177(15) OW2 0.045(2) 0.051(2) 0.032(2) -0.0007(17) -0.0097(17) -0.0345(18) OW3 0.0287(16) 0.0275(18) 0.0301(17) -0.0021(14) -0.0158(14) -0.0133(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mo1 O7 1.714(3) . ? Mo1 O8 1.722(3) . ? Mo1 O4 1.912(2) . ? Mo1 O5 1.918(2) . ? Mo1 O1 2.241(2) . ? Mo1 O2 2.337(2) . ? Mo2 O9 1.708(3) . ? Mo2 O10 1.725(3) . ? Mo2 O6 1.910(2) . ? Mo2 O5 1.941(2) . ? Mo2 O2 2.298(2) . ? Mo2 O3 2.324(2) . ? Mo3 O11 1.702(3) . ? Mo3 O12 1.720(3) 2_476 ? Mo3 O6 1.924(2) . ? Mo3 O4 1.954(2) 2_476 ? Mo3 O1 2.281(2) 2_476 ? Mo3 O3 2.284(2) . ? Ag1 OW1 2.267(3) . ? Ag1 O8 2.314(3) 2_566 ? Ag1 O10 2.429(3) . ? Ag1 O9 2.557(3) 2_566 ? Ag2 O7 2.374(3) 2_477 ? Ag2 O7 2.374(3) . ? Ag2 O12 2.447(3) 2_477 ? Ag2 O12 2.447(3) . ? Al1 O1 1.885(2) . ? Al1 O1 1.885(2) 2_476 ? Al1 O2 1.903(2) . ? Al1 O2 1.903(2) 2_476 ? Al1 O3 1.914(2) 2_476 ? Al1 O3 1.914(2) . ? O1 Mo3 2.281(2) 2_476 ? O4 Mo3 1.954(2) 2_476 ? O8 Ag1 2.314(3) 2_566 ? O9 Ag1 2.557(3) 2_566 ? O12 Mo3 1.720(3) 2_476 ? O13 C1 1.272(5) . ? O14 C1 1.255(5) . ? C1 C2 1.494(5) . ? C2 C3 1.319(6) . ? C2 H2A 0.9300 . ? C3 C4 1.473(5) . ? C3 H3A 0.9300 . ? C4 C5 1.386(5) . ? C4 C8 1.401(6) . ? C5 N1 1.339(5) . ? C5 H5A 0.9300 . ? C6 N1 1.331(6) . ? C6 C7 1.368(6) . ? C6 H6A 0.9300 . ? C7 C8 1.383(6) . ? C7 H7A 0.9300 . ? C8 H8A 0.9300 . ? N1 H1A 0.8600 . ? OW1 H1 0.832(19) . ? OW1 H2 0.836(19) . ? OW2 H3 0.844(19) . ? OW2 H4 0.84(2) . ? OW3 H5 0.827(19) . ? OW3 H6 0.825(19) . ? 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 O7 Mo1 O8 105.98(13) . . ? O7 Mo1 O4 101.67(12) . . ? O8 Mo1 O4 96.33(12) . . ? O7 Mo1 O5 97.38(12) . . ? O8 Mo1 O5 99.89(12) . . ? O4 Mo1 O5 150.46(10) . . ? O7 Mo1 O1 93.61(11) . . ? O8 Mo1 O1 159.56(11) . . ? O4 Mo1 O1 73.61(9) . . ? O5 Mo1 O1 82.90(10) . . ? O7 Mo1 O2 159.71(11) . . ? O8 Mo1 O2 92.83(11) . . ? O4 Mo1 O2 83.34(10) . . ? O5 Mo1 O2 71.40(9) . . ? O1 Mo1 O2 68.70(9) . . ? O9 Mo2 O10 106.92(13) . . ? O9 Mo2 O6 98.30(12) . . ? O10 Mo2 O6 102.04(12) . . ? O9 Mo2 O5 100.70(12) . . ? O10 Mo2 O5 95.69(12) . . ? O6 Mo2 O5 148.92(10) . . ? O9 Mo2 O2 93.24(11) . . ? O10 Mo2 O2 158.20(11) . . ? O6 Mo2 O2 82.68(10) . . ? O5 Mo2 O2 71.93(9) . . ? O9 Mo2 O3 159.80(11) . . ? O10 Mo2 O3 92.83(11) . . ? O6 Mo2 O3 72.84(9) . . ? O5 Mo2 O3 81.04(10) . . ? O2 Mo2 O3 67.98(8) . . ? O11 Mo3 O12 106.06(13) . 2_476 ? O11 Mo3 O6 101.10(12) . . ? O12 Mo3 O6 97.34(12) 2_476 . ? O11 Mo3 O4 95.51(12) . 2_476 ? O12 Mo3 O4 100.58(12) 2_476 2_476 ? O6 Mo3 O4 151.11(11) . 2_476 ? O11 Mo3 O1 158.92(11) . 2_476 ? O12 Mo3 O1 93.11(11) 2_476 2_476 ? O6 Mo3 O1 84.69(10) . 2_476 ? O4 Mo3 O1 71.93(9) 2_476 2_476 ? O11 Mo3 O3 94.03(12) . . ? O12 Mo3 O3 159.33(11) 2_476 . ? O6 Mo3 O3 73.56(10) . . ? O4 Mo3 O3 81.90(10) 2_476 . ? O1 Mo3 O3 67.95(9) 2_476 . ? OW1 Ag1 O8 121.55(11) . 2_566 ? OW1 Ag1 O10 148.59(11) . . ? O8 Ag1 O10 89.50(9) 2_566 . ? OW1 Ag1 O9 91.54(10) . 2_566 ? O8 Ag1 O9 83.25(9) 2_566 2_566 ? O10 Ag1 O9 87.30(9) . 2_566 ? O7 Ag2 O7 180.00(11) 2_477 . ? O7 Ag2 O12 82.79(9) 2_477 2_477 ? O7 Ag2 O12 97.21(9) . 2_477 ? O7 Ag2 O12 97.21(9) 2_477 . ? O7 Ag2 O12 82.79(9) . . ? O12 Ag2 O12 180.000(1) 2_477 . ? O1 Al1 O1 180.0 . 2_476 ? O1 Al1 O2 86.05(10) . . ? O1 Al1 O2 93.95(10) 2_476 . ? O1 Al1 O2 93.95(10) . 2_476 ? O1 Al1 O2 86.05(10) 2_476 2_476 ? O2 Al1 O2 180.0 . 2_476 ? O1 Al1 O3 84.37(10) . 2_476 ? O1 Al1 O3 95.63(10) 2_476 2_476 ? O2 Al1 O3 94.77(10) . 2_476 ? O2 Al1 O3 85.23(10) 2_476 2_476 ? O1 Al1 O3 95.63(10) . . ? O1 Al1 O3 84.37(10) 2_476 . ? O2 Al1 O3 85.23(10) . . ? O2 Al1 O3 94.77(10) 2_476 . ? O3 Al1 O3 180.0 2_476 . ? Al1 O1 Mo1 104.66(11) . . ? Al1 O1 Mo3 104.35(11) . 2_476 ? Mo1 O1 Mo3 92.77(9) . 2_476 ? Al1 O2 Mo2 104.05(11) . . ? Al1 O2 Mo1 100.59(10) . . ? Mo2 O2 Mo1 91.89(9) . . ? Al1 O3 Mo3 103.30(10) . . ? Al1 O3 Mo2 102.72(10) . . ? Mo3 O3 Mo2 91.05(9) . . ? Mo1 O4 Mo3 115.76(12) . 2_476 ? Mo1 O5 Mo2 119.34(13) . . ? Mo2 O6 Mo3 118.07(13) . . ? Mo1 O7 Ag2 131.22(14) . . ? Mo1 O8 Ag1 140.19(15) . 2_566 ? Mo2 O9 Ag1 134.16(14) . 2_566 ? Mo2 O10 Ag1 133.57(14) . . ? Mo3 O12 Ag2 130.19(14) 2_476 . ? O14 C1 O13 124.7(4) . . ? O14 C1 C2 117.2(3) . . ? O13 C1 C2 118.0(3) . . ? C3 C2 C1 123.6(4) . . ? C3 C2 H2A 118.2 . . ? C1 C2 H2A 118.2 . . ? C2 C3 C4 124.1(4) . . ? C2 C3 H3A 118.0 . . ? C4 C3 H3A 118.0 . . ? C5 C4 C8 116.8(4) . . ? C5 C4 C3 118.7(3) . . ? C8 C4 C3 124.5(4) . . ? N1 C5 C4 120.6(4) . . ? N1 C5 H5A 119.7 . . ? C4 C5 H5A 119.7 . . ? N1 C6 C7 119.3(4) . . ? N1 C6 H6A 120.3 . . ? C7 C6 H6A 120.3 . . ? C6 C7 C8 119.5(4) . . ? C6 C7 H7A 120.2 . . ? C8 C7 H7A 120.2 . . ? C7 C8 C4 120.6(4) . . ? C7 C8 H8A 119.7 . . ? C4 C8 H8A 119.7 . . ? C6 N1 C5 123.0(4) . . ? C6 N1 H1A 118.5 . . ? C5 N1 H1A 118.5 . . ? Ag1 OW1 H1 116(3) . . ? Ag1 OW1 H2 112(3) . . ? H1 OW1 H2 120(3) . . ? H3 OW2 H4 118(4) . . ? H5 OW3 H6 122(4) . . ? 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 O1 Al1 O1 Mo1 -152(100) 2_476 . . . ? O2 Al1 O1 Mo1 0.12(10) . . . . ? O2 Al1 O1 Mo1 -179.88(10) 2_476 . . . ? O3 Al1 O1 Mo1 95.32(11) 2_476 . . . ? O3 Al1 O1 Mo1 -84.68(11) . . . . ? O1 Al1 O1 Mo3 111(100) 2_476 . . 2_476 ? O2 Al1 O1 Mo3 -96.68(11) . . . 2_476 ? O2 Al1 O1 Mo3 83.32(11) 2_476 . . 2_476 ? O3 Al1 O1 Mo3 -1.49(10) 2_476 . . 2_476 ? O3 Al1 O1 Mo3 178.51(10) . . . 2_476 ? O7 Mo1 O1 Al1 169.65(12) . . . . ? O8 Mo1 O1 Al1 -26.7(4) . . . . ? O4 Mo1 O1 Al1 -89.24(12) . . . . ? O5 Mo1 O1 Al1 72.65(12) . . . . ? O2 Mo1 O1 Al1 -0.11(9) . . . . ? O7 Mo1 O1 Mo3 -84.74(11) . . . 2_476 ? O8 Mo1 O1 Mo3 79.0(3) . . . 2_476 ? O4 Mo1 O1 Mo3 16.37(9) . . . 2_476 ? O5 Mo1 O1 Mo3 178.26(10) . . . 2_476 ? O2 Mo1 O1 Mo3 105.50(10) . . . 2_476 ? O1 Al1 O2 Mo2 -94.79(11) . . . . ? O1 Al1 O2 Mo2 85.21(11) 2_476 . . . ? O2 Al1 O2 Mo2 8(100) 2_476 . . . ? O3 Al1 O2 Mo2 -178.79(10) 2_476 . . . ? O3 Al1 O2 Mo2 1.21(10) . . . . ? O1 Al1 O2 Mo1 -0.12(10) . . . . ? O1 Al1 O2 Mo1 179.88(10) 2_476 . . . ? O2 Al1 O2 Mo1 103(100) 2_476 . . . ? O3 Al1 O2 Mo1 -84.12(11) 2_476 . . . ? O3 Al1 O2 Mo1 95.88(11) . . . . ? O9 Mo2 O2 Al1 -173.44(12) . . . . ? O10 Mo2 O2 Al1 28.7(3) . . . . ? O6 Mo2 O2 Al1 -75.47(12) . . . . ? O5 Mo2 O2 Al1 86.36(12) . . . . ? O3 Mo2 O2 Al1 -1.07(9) . . . . ? O9 Mo2 O2 Mo1 85.15(11) . . . . ? O10 Mo2 O2 Mo1 -72.7(3) . . . . ? O6 Mo2 O2 Mo1 -176.88(10) . . . . ? O5 Mo2 O2 Mo1 -15.05(9) . . . . ? O3 Mo2 O2 Mo1 -102.48(10) . . . . ? O7 Mo1 O2 Al1 -30.7(4) . . . . ? O8 Mo1 O2 Al1 171.12(12) . . . . ? O4 Mo1 O2 Al1 75.07(11) . . . . ? O5 Mo1 O2 Al1 -89.39(12) . . . . ? O1 Mo1 O2 Al1 0.11(9) . . . . ? O7 Mo1 O2 Mo2 74.0(3) . . . . ? O8 Mo1 O2 Mo2 -84.21(11) . . . . ? O4 Mo1 O2 Mo2 179.74(10) . . . . ? O5 Mo1 O2 Mo2 15.28(9) . . . . ? O1 Mo1 O2 Mo2 104.78(10) . . . . ? O1 Al1 O3 Mo3 178.52(10) . . . . ? O1 Al1 O3 Mo3 -1.48(10) 2_476 . . . ? O2 Al1 O3 Mo3 92.98(11) . . . . ? O2 Al1 O3 Mo3 -87.02(11) 2_476 . . . ? O3 Al1 O3 Mo3 6(100) 2_476 . . . ? O1 Al1 O3 Mo2 84.36(11) . . . . ? O1 Al1 O3 Mo2 -95.64(11) 2_476 . . . ? O2 Al1 O3 Mo2 -1.19(10) . . . . ? O2 Al1 O3 Mo2 178.81(10) 2_476 . . . ? O3 Al1 O3 Mo2 -88(100) 2_476 . . . ? O11 Mo3 O3 Al1 170.04(13) . . . . ? O12 Mo3 O3 Al1 -23.5(4) 2_476 . . . ? O6 Mo3 O3 Al1 -89.57(12) . . . . ? O4 Mo3 O3 Al1 75.03(11) 2_476 . . . ? O1 Mo3 O3 Al1 1.31(9) 2_476 . . . ? O11 Mo3 O3 Mo2 -86.63(11) . . . . ? O12 Mo3 O3 Mo2 79.9(3) 2_476 . . . ? O6 Mo3 O3 Mo2 13.77(9) . . . . ? O4 Mo3 O3 Mo2 178.37(10) 2_476 . . . ? O1 Mo3 O3 Mo2 104.65(10) 2_476 . . . ? O9 Mo2 O3 Al1 23.6(4) . . . . ? O10 Mo2 O3 Al1 -168.30(13) . . . . ? O6 Mo2 O3 Al1 89.97(12) . . . . ? O5 Mo2 O3 Al1 -72.99(11) . . . . ? O2 Mo2 O3 Al1 1.06(9) . . . . ? O9 Mo2 O3 Mo3 -80.2(3) . . . . ? O10 Mo2 O3 Mo3 87.81(11) . . . . ? O6 Mo2 O3 Mo3 -13.92(9) . . . . ? O5 Mo2 O3 Mo3 -176.88(10) . . . . ? O2 Mo2 O3 Mo3 -102.83(10) . . . . ? O7 Mo1 O4 Mo3 68.97(15) . . . 2_476 ? O8 Mo1 O4 Mo3 176.77(14) . . . 2_476 ? O5 Mo1 O4 Mo3 -60.1(3) . . . 2_476 ? O1 Mo1 O4 Mo3 -21.40(12) . . . 2_476 ? O2 Mo1 O4 Mo3 -91.10(13) . . . 2_476 ? O7 Mo1 O5 Mo2 176.43(15) . . . . ? O8 Mo1 O5 Mo2 68.71(16) . . . . ? O4 Mo1 O5 Mo2 -53.6(3) . . . . ? O1 Mo1 O5 Mo2 -90.82(14) . . . . ? O2 Mo1 O5 Mo2 -20.96(12) . . . . ? O9 Mo2 O5 Mo1 -68.67(16) . . . . ? O10 Mo2 O5 Mo1 -177.12(15) . . . . ? O6 Mo2 O5 Mo1 58.0(3) . . . . ? O2 Mo2 O5 Mo1 21.26(12) . . . . ? O3 Mo2 O5 Mo1 90.90(14) . . . . ? O9 Mo2 O6 Mo3 -179.76(15) . . . . ? O10 Mo2 O6 Mo3 -70.38(16) . . . . ? O5 Mo2 O6 Mo3 53.0(3) . . . . ? O2 Mo2 O6 Mo3 88.02(14) . . . . ? O3 Mo2 O6 Mo3 18.88(12) . . . . ? O11 Mo3 O6 Mo2 71.82(17) . . . . ? O12 Mo3 O6 Mo2 179.84(15) 2_476 . . . ? O4 Mo3 O6 Mo2 -52.1(3) 2_476 . . . ? O1 Mo3 O6 Mo2 -87.69(14) 2_476 . . . ? O3 Mo3 O6 Mo2 -19.15(12) . . . . ? O8 Mo1 O7 Ag2 -162.53(17) . . . . ? O4 Mo1 O7 Ag2 -62.38(19) . . . . ? O5 Mo1 O7 Ag2 94.92(18) . . . . ? O1 Mo1 O7 Ag2 11.61(18) . . . . ? O2 Mo1 O7 Ag2 40.2(4) . . . . ? O7 Ag2 O7 Mo1 -65(100) 2_477 . . . ? O12 Ag2 O7 Mo1 -135.30(19) 2_477 . . . ? O12 Ag2 O7 Mo1 44.70(19) . . . . ? O7 Mo1 O8 Ag1 -149.9(2) . . . 2_566 ? O4 Mo1 O8 Ag1 106.0(2) . . . 2_566 ? O5 Mo1 O8 Ag1 -49.2(2) . . . 2_566 ? O1 Mo1 O8 Ag1 47.1(5) . . . 2_566 ? O2 Mo1 O8 Ag1 22.4(2) . . . 2_566 ? O10 Mo2 O9 Ag1 143.18(18) . . . 2_566 ? O6 Mo2 O9 Ag1 -111.47(19) . . . 2_566 ? O5 Mo2 O9 Ag1 43.8(2) . . . 2_566 ? O2 Mo2 O9 Ag1 -28.40(19) . . . 2_566 ? O3 Mo2 O9 Ag1 -49.3(4) . . . 2_566 ? O9 Mo2 O10 Ag1 -49.9(2) . . . . ? O6 Mo2 O10 Ag1 -152.55(18) . . . . ? O5 Mo2 O10 Ag1 53.1(2) . . . . ? O2 Mo2 O10 Ag1 106.9(3) . . . . ? O3 Mo2 O10 Ag1 134.39(19) . . . . ? OW1 Ag1 O10 Mo2 -82.5(3) . . . . ? O8 Ag1 O10 Mo2 89.3(2) 2_566 . . . ? O9 Ag1 O10 Mo2 6.0(2) 2_566 . . . ? O7 Ag2 O12 Mo3 135.79(18) 2_477 . . 2_476 ? O7 Ag2 O12 Mo3 -44.21(18) . . . 2_476 ? O12 Ag2 O12 Mo3 -26(100) 2_477 . . 2_476 ? O14 C1 C2 C3 171.7(4) . . . . ? O13 C1 C2 C3 -7.5(6) . . . . ? C1 C2 C3 C4 -176.8(4) . . . . ? C2 C3 C4 C5 171.6(4) . . . . ? C2 C3 C4 C8 -8.9(6) . . . . ? C8 C4 C5 N1 -0.7(6) . . . . ? C3 C4 C5 N1 178.8(3) . . . . ? N1 C6 C7 C8 -0.6(6) . . . . ? C6 C7 C8 C4 -1.5(6) . . . . ? C5 C4 C8 C7 2.1(6) . . . . ? C3 C4 C8 C7 -177.4(4) . . . . ? C7 C6 N1 C5 2.1(6) . . . . ? C4 C5 N1 C6 -1.4(6) . . . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 0.741 _refine_diff_density_min -0.752 _refine_diff_density_rms 0.110 _database_code_depnum_ccdc_archive 'CCDC 954134' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H34 Ag2 Al Mo6 N3 O33' _chemical_formula_weight 1710.90 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' Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Fddd loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+3/4, -y+3/4, z' '-x+3/4, y, -z+3/4' 'x, -y+3/4, -z+3/4' 'x, y+1/2, z+1/2' '-x+3/4, -y+5/4, z+1/2' '-x+3/4, y+1/2, -z+5/4' 'x, -y+5/4, -z+5/4' 'x+1/2, y, z+1/2' '-x+5/4, -y+3/4, z+1/2' '-x+5/4, y, -z+5/4' 'x+1/2, -y+3/4, -z+5/4' 'x+1/2, y+1/2, z' '-x+5/4, -y+5/4, z' '-x+5/4, y+1/2, -z+3/4' 'x+1/2, -y+5/4, -z+3/4' '-x, -y, -z' 'x-3/4, y-3/4, -z' 'x-3/4, -y, z-3/4' '-x, y-3/4, z-3/4' '-x, -y+1/2, -z+1/2' 'x-3/4, y-1/4, -z+1/2' 'x-3/4, -y+1/2, z-1/4' '-x, y-1/4, z-1/4' '-x+1/2, -y, -z+1/2' 'x-1/4, y-3/4, -z+1/2' 'x-1/4, -y, z-1/4' '-x+1/2, y-3/4, z-1/4' '-x+1/2, -y+1/2, -z' 'x-1/4, y-1/4, -z' 'x-1/4, -y+1/2, z-3/4' '-x+1/2, y-1/4, z-3/4' _cell_length_a 15.892(2) _cell_length_b 29.617(4) _cell_length_c 37.798(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 17790(5) _cell_formula_units_Z 16 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 21439 _cell_measurement_theta_min 2.16 _cell_measurement_theta_max 25.00 _exptl_crystal_description rod _exptl_crystal_colour colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.555 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 13152 _exptl_absorpt_coefficient_mu 2.624 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.573 _exptl_absorpt_correction_T_max 0.749 _exptl_absorpt_process_details 'ABSCOR by T.Higashi 8 March, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart Apex CCD' _diffrn_measurement_method \w-2\q _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 21439 _diffrn_reflns_av_R_equivalents 0.0325 _diffrn_reflns_av_unetI/netI 0.0237 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -34 _diffrn_reflns_limit_k_max 35 _diffrn_reflns_limit_l_min -44 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.16 _diffrn_reflns_theta_max 25.00 _reflns_number_total 3926 _reflns_number_gt 3517 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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 command 'omit-3 50' was used to omit the weak reflections above 50 degree. The carboxyl oxygen atoms (O13, O13a, O15), pyridyl nitrogen atoms (N1, N2) and carbon atoms (C9 C10 C11 C12 C13 C14 C15 C16) of organic molecules are restrained with the command isor so as to avoid their extensive NPD and ADP problems. The disordered crystal water molecules (OW2, OW3) are also retrained with the command 'isor'.The hydrogen atoms of OW1 are located from the residual peak, and hydrogen atoms of disordered water molecules (OW2, OW3) failed to be picked out. Futhermore, the restraint command 'dfix' was used to restrain the distance of neighboring carbon atoms, and 'eadp' was used to restrain the disordered carboxyl oxygen atoms. All these restrained refinement led to a restraint value of 91. ; _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^)+(0.0317P)^2^+573.2908P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens . _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3926 _refine_ls_number_parameters 365 _refine_ls_number_restraints 91 _refine_ls_R_factor_all 0.0415 _refine_ls_R_factor_gt 0.0359 _refine_ls_wR_factor_ref 0.0914 _refine_ls_wR_factor_gt 0.0882 _refine_ls_goodness_of_fit_ref 1.129 _refine_ls_restrained_S_all 1.122 _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 -0.13454(3) -0.021574(17) -0.063994(13) 0.02079(14) Uani 1 1 d . . . Mo2 Mo 0.06984(3) -0.023418(17) -0.080874(13) 0.02097(14) Uani 1 1 d . . . Mo3 Mo 0.20565(3) -0.001786(17) -0.016884(13) 0.01929(14) Uani 1 1 d . . . Ag1 Ag -0.03649(5) -0.1250 -0.1250 0.02925(18) Uani 1 2 d S . . Ag2 Ag -0.1250 0.3750 -0.03868(3) 0.0597(3) Uani 1 2 d S . . Al1 Al 0.0000 0.0000 0.0000 0.0150(5) Uani 1 2 d S . . O1 O -0.0982(2) 0.02710(12) -0.01932(10) 0.0173(8) Uani 1 1 d . . . O2 O -0.0170(2) -0.04543(12) -0.03434(10) 0.0171(8) Uani 1 1 d . . . O3 O 0.0753(2) 0.02613(12) -0.03375(10) 0.0174(8) Uani 1 1 d . . . O4 O -0.1904(3) -0.04142(13) -0.02073(11) 0.0228(9) Uani 1 1 d . . . O5 O -0.0396(3) 0.00394(14) -0.08718(10) 0.0236(9) Uani 1 1 d . . . O6 O 0.1562(2) -0.04375(13) -0.04905(11) 0.0218(9) Uani 1 1 d . . . O7 O -0.1484(3) -0.07129(15) -0.08663(12) 0.0314(10) Uani 1 1 d . . . O8 O -0.2083(3) 0.01533(17) -0.07907(12) 0.0328(11) Uani 1 1 d . . . O9 O 0.0572(3) -0.07304(15) -0.10346(12) 0.0324(11) Uani 1 1 d . . . O10 O 0.1261(3) 0.01150(16) -0.10780(12) 0.0316(10) Uani 1 1 d . . . O11 O 0.2599(3) 0.03279(15) -0.04489(11) 0.0282(10) Uani 1 1 d . . . O12 O 0.2797(3) -0.03721(15) 0.00162(12) 0.0304(10) Uani 1 1 d . . . O13 O -0.2754(5) 0.1145(3) -0.0362(2) 0.051(2) Uani 0.719(10) 1 d PU A 1 O13A O -0.2712(12) 0.1011(7) -0.0641(6) 0.051(2) Uani 0.281(10) 1 d PU A 2 O14 O -0.1402(4) 0.11569(16) -0.03162(16) 0.0480(14) Uani 1 1 d . A . C1 C -0.2033(6) 0.1341(3) -0.0376(2) 0.052(2) Uani 1 1 d . . . C2 C -0.2070(5) 0.1847(3) -0.0412(2) 0.0450(19) Uani 1 1 d . A . H2A H -0.1569 0.2007 -0.0393 0.054 Uiso 1 1 calc R . . C3 C -0.2738(6) 0.2067(3) -0.0466(2) 0.049(2) Uani 1 1 d . . . H3A H -0.3232 0.1901 -0.0488 0.059 Uiso 1 1 calc R A . C4 C -0.2809(4) 0.2557(2) -0.04981(17) 0.0294(14) Uani 1 1 d . A . C5 C -0.2177(4) 0.2862(2) -0.04224(17) 0.0282(14) Uani 1 1 d . . . H5A H -0.1658 0.2751 -0.0350 0.034 Uiso 1 1 calc R A . C6 C -0.3025(5) 0.3465(2) -0.05556(19) 0.0389(17) Uani 1 1 d . . . H6A H -0.3099 0.3776 -0.0578 0.047 Uiso 1 1 calc R A . C7 C -0.3684(5) 0.3188(3) -0.0635(2) 0.0411(18) Uani 1 1 d . A . H7A H -0.4198 0.3308 -0.0707 0.049 Uiso 1 1 calc R . . C8 C -0.3579(5) 0.2732(3) -0.06066(19) 0.0371(17) Uani 1 1 d . . . H8A H -0.4022 0.2539 -0.0660 0.045 Uiso 1 1 calc R A . O15 O -0.0712(13) 0.3280(8) -0.1179(7) 0.043(6) Uani 0.50 1 d PU B -1 O16 O -0.2075(12) 0.3353(8) -0.1320(8) 0.051(5) Uani 0.50 1 d P B -1 C9 C -0.1425(11) 0.3123(5) -0.1261(8) 0.034(5) Uani 0.50 1 d PU B -1 C10 C -0.1549(9) 0.2616(5) -0.1289(4) 0.032(3) Uani 0.50 1 d PU B -1 H10A H -0.2072 0.2505 -0.1357 0.038 Uiso 0.50 1 calc PR B -1 C11 C -0.0936(8) 0.2329(3) -0.1219(3) 0.026(3) Uani 0.50 1 d PDU B -1 H11A H -0.0423 0.2454 -0.1154 0.032 Uiso 0.50 1 calc PR B -1 C12 C -0.0975(6) 0.1838(2) -0.1233(3) 0.027(3) Uani 0.50 1 d PGDU B -1 C13 C -0.0285(4) 0.1582(3) -0.1128(3) 0.045(4) Uani 0.50 1 d PGU B -1 H13A H 0.0202 0.1725 -0.1050 0.054 Uiso 0.50 1 calc PR B -1 C15 C -0.0323(5) 0.1114(3) -0.1140(4) 0.060(5) Uani 0.50 1 d PGU B -1 H15A H 0.0139 0.0943 -0.1070 0.071 Uiso 0.50 1 calc PR B -1 C14 C -0.1051(6) 0.0900(2) -0.1257(4) 0.035(4) Uani 0.50 1 d PGU B -1 H14A H -0.1076 0.0587 -0.1265 0.042 Uiso 0.50 1 calc PR B -1 N2 N -0.1741(4) 0.1156(3) -0.1362(3) 0.045(3) Uani 0.50 1 d PGU B -1 H2B H -0.2191 0.1024 -0.1434 0.054 Uiso 0.50 1 calc PR B -1 C16 C -0.1703(5) 0.1624(3) -0.1350(3) 0.042(4) Uani 0.50 1 d PGU B -1 H16A H -0.2165 0.1795 -0.1420 0.050 Uiso 0.50 1 calc PR B -1 N1 N -0.2275(4) 0.33103(18) -0.04477(15) 0.0319(13) Uani 1 1 d U A . OW1 O 0.0080(5) 0.12685(19) 0.00356(18) 0.072(2) Uani 1 1 d . . . H1 H 0.0389 0.1149 -0.0100 0.086 Uiso 1 1 d R . . H2 H -0.0432 0.1309 -0.0038 0.086 Uiso 1 1 d R . . OW2 O 0.1250 0.1250 -0.0510(5) 0.071(5) Uani 0.50 2 d SPU . . OW3 O -0.3080(14) 0.1087(6) -0.1909(5) 0.041(5) Uani 0.25 1 d PU . . 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 0.0187(3) 0.0256(3) 0.0181(3) -0.0035(2) -0.0012(2) -0.0047(2) Mo2 0.0204(3) 0.0238(3) 0.0188(3) -0.0063(2) 0.0023(2) -0.0027(2) Mo3 0.0165(3) 0.0205(3) 0.0209(3) -0.0020(2) 0.0021(2) -0.0031(2) Ag1 0.0282(4) 0.0203(3) 0.0392(4) 0.0039(3) 0.000 0.000 Ag2 0.0672(6) 0.0606(6) 0.0511(6) 0.000 0.000 -0.0449(5) Al1 0.0157(11) 0.0136(11) 0.0157(12) -0.0042(9) 0.0010(9) -0.0030(9) O1 0.017(2) 0.0176(19) 0.017(2) -0.0012(16) 0.0002(16) -0.0008(16) O2 0.018(2) 0.0144(19) 0.019(2) -0.0038(15) 0.0010(16) -0.0016(16) O3 0.016(2) 0.0166(19) 0.019(2) -0.0005(16) 0.0003(16) -0.0014(16) O4 0.021(2) 0.023(2) 0.024(2) -0.0063(17) 0.0018(17) -0.0091(17) O5 0.024(2) 0.029(2) 0.018(2) 0.0002(17) 0.0013(17) -0.0025(18) O6 0.021(2) 0.018(2) 0.027(2) -0.0039(17) 0.0003(17) 0.0004(17) O7 0.032(3) 0.036(3) 0.027(2) -0.009(2) -0.002(2) -0.012(2) O8 0.023(2) 0.047(3) 0.028(2) 0.008(2) -0.0021(19) -0.001(2) O9 0.030(2) 0.036(3) 0.032(2) -0.017(2) -0.002(2) -0.004(2) O10 0.027(2) 0.041(3) 0.027(2) 0.001(2) 0.005(2) -0.007(2) O11 0.027(2) 0.030(2) 0.027(2) -0.0001(19) 0.0058(19) -0.0074(19) O12 0.023(2) 0.035(2) 0.033(3) 0.003(2) -0.002(2) 0.0001(19) O13 0.043(4) 0.039(4) 0.072(5) 0.002(3) -0.018(4) 0.008(3) O13A 0.043(4) 0.039(4) 0.072(5) 0.002(3) -0.018(4) 0.008(3) O14 0.054(4) 0.023(3) 0.067(4) -0.003(2) 0.001(3) 0.001(2) C1 0.058(6) 0.037(4) 0.060(5) 0.005(4) 0.014(5) 0.001(4) C2 0.039(4) 0.051(5) 0.045(5) -0.003(4) 0.000(4) -0.007(4) C3 0.066(6) 0.036(4) 0.046(5) 0.006(4) 0.003(4) -0.001(4) C4 0.038(4) 0.022(3) 0.028(3) 0.002(3) 0.006(3) -0.004(3) C5 0.020(3) 0.031(3) 0.034(4) 0.006(3) 0.004(3) 0.003(3) C6 0.053(5) 0.024(3) 0.040(4) -0.001(3) 0.002(4) 0.007(3) C7 0.031(4) 0.050(5) 0.042(4) 0.007(4) -0.005(3) 0.010(3) C8 0.030(4) 0.044(4) 0.037(4) 0.000(3) 0.002(3) -0.012(3) O15 0.041(10) 0.037(9) 0.050(8) 0.002(6) -0.004(8) 0.002(7) O16 0.043(12) 0.038(10) 0.072(10) -0.004(7) 0.005(10) 0.003(9) C9 0.037(12) 0.032(6) 0.033(6) -0.003(7) 0.004(9) -0.001(6) C10 0.035(6) 0.028(6) 0.033(6) -0.002(6) 0.003(6) -0.002(5) C11 0.037(6) 0.022(5) 0.020(5) 0.001(5) -0.003(5) 0.003(5) C12 0.037(7) 0.023(6) 0.022(5) 0.000(5) 0.000(6) 0.002(5) C13 0.045(7) 0.037(7) 0.051(7) -0.005(6) -0.012(7) 0.000(6) C15 0.058(9) 0.052(8) 0.068(9) 0.002(7) -0.006(8) 0.006(7) C14 0.041(10) 0.027(5) 0.037(6) -0.004(6) 0.006(8) 0.002(5) N2 0.046(7) 0.036(6) 0.053(7) -0.001(5) -0.002(6) 0.002(6) C16 0.045(8) 0.031(7) 0.050(8) -0.001(6) -0.004(7) 0.008(7) N1 0.033(3) 0.027(3) 0.036(3) 0.002(2) 0.001(2) -0.009(2) OW1 0.098(5) 0.035(3) 0.082(5) 0.020(3) -0.043(4) -0.023(3) OW2 0.076(9) 0.070(9) 0.067(9) 0.000 0.000 0.028(8) OW3 0.053(9) 0.027(7) 0.043(8) -0.015(7) 0.004(7) -0.007(7) _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 1.701(5) . ? Mo1 O7 1.717(4) . ? Mo1 O5 1.901(4) . ? Mo1 O4 1.951(4) . ? Mo1 O2 2.291(4) . ? Mo1 O1 2.294(4) . ? Mo2 O10 1.705(4) . ? Mo2 O9 1.712(4) . ? Mo2 O6 1.922(4) . ? Mo2 O5 1.934(4) . ? Mo2 O3 2.309(4) . ? Mo2 O2 2.329(4) . ? Mo3 O11 1.706(4) . ? Mo3 O12 1.725(4) . ? Mo3 O6 1.908(4) . ? Mo3 O4 1.928(4) 17 ? Mo3 O1 2.313(4) 17 ? Mo3 O3 2.320(4) . ? Ag1 O9 2.290(4) . ? Ag1 O9 2.290(4) 4_544 ? Ag1 O7 2.389(4) 2_445 ? Ag1 O7 2.389(4) 3_454 ? Ag1 Ag1 2.8131(15) 2_445 ? Ag2 N1 2.098(5) 2_455 ? Ag2 N1 2.098(5) . ? Al1 O2 1.889(4) 17 ? Al1 O2 1.889(4) . ? Al1 O1 1.901(4) 17 ? Al1 O1 1.901(4) . ? Al1 O3 1.913(4) . ? Al1 O3 1.913(4) 17 ? O1 Mo3 2.313(4) 17 ? O4 Mo3 1.928(4) 17 ? O7 Ag1 2.389(4) 2_445 ? O13 C1 1.284(11) . ? O13A C1 1.77(2) . ? O14 C1 1.164(10) . ? C1 C2 1.506(11) . ? C2 C3 1.262(11) . ? C3 C4 1.461(10) . ? C4 C5 1.381(9) . ? C4 C8 1.392(10) . ? C5 N1 1.340(8) . ? C6 N1 1.340(9) . ? C6 C7 1.366(11) . ? C7 C8 1.364(10) . ? O15 C9 1.27(3) . ? O16 C9 1.26(3) . ? C9 C10 1.52(2) . ? C10 C11 1.319(16) . ? C11 C12 1.458(8) . ? C12 C13 1.3900 . ? C12 C16 1.3900 . ? C13 C15 1.3900 . ? C15 C14 1.3900 . ? C14 N2 1.3900 . ? N2 C16 1.3900 . ? OW2 OW3 1.21(2) 16_544 ? OW2 OW3 1.21(2) 3_454 ? OW3 OW2 1.21(2) 3_454 ? 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 O7 107.2(2) . . ? O8 Mo1 O5 97.9(2) . . ? O7 Mo1 O5 102.28(19) . . ? O8 Mo1 O4 99.3(2) . . ? O7 Mo1 O4 95.80(19) . . ? O5 Mo1 O4 150.10(17) . . ? O8 Mo1 O2 157.57(19) . . ? O7 Mo1 O2 94.81(18) . . ? O5 Mo1 O2 72.61(16) . . ? O4 Mo1 O2 82.41(16) . . ? O8 Mo1 O1 90.95(19) . . ? O7 Mo1 O1 159.69(18) . . ? O5 Mo1 O1 83.67(15) . . ? O4 Mo1 O1 71.75(15) . . ? O2 Mo1 O1 68.18(13) . . ? O10 Mo2 O9 106.6(2) . . ? O10 Mo2 O6 100.9(2) . . ? O9 Mo2 O6 97.3(2) . . ? O10 Mo2 O5 98.3(2) . . ? O9 Mo2 O5 101.1(2) . . ? O6 Mo2 O5 148.32(17) . . ? O10 Mo2 O3 93.17(18) . . ? O9 Mo2 O3 159.18(19) . . ? O6 Mo2 O3 71.93(15) . . ? O5 Mo2 O3 82.10(15) . . ? O10 Mo2 O2 158.72(18) . . ? O9 Mo2 O2 93.81(18) . . ? O6 Mo2 O2 82.11(15) . . ? O5 Mo2 O2 71.19(15) . . ? O3 Mo2 O2 67.51(13) . . ? O11 Mo3 O12 105.8(2) . . ? O11 Mo3 O6 101.74(19) . . ? O12 Mo3 O6 98.2(2) . . ? O11 Mo3 O4 97.05(19) . 17 ? O12 Mo3 O4 101.0(2) . 17 ? O6 Mo3 O4 148.26(17) . 17 ? O11 Mo3 O1 159.11(18) . 17 ? O12 Mo3 O1 93.82(18) . 17 ? O6 Mo3 O1 82.06(15) . 17 ? O4 Mo3 O1 71.70(15) 17 17 ? O11 Mo3 O3 93.81(18) . . ? O12 Mo3 O3 159.64(18) . . ? O6 Mo3 O3 71.91(15) . . ? O4 Mo3 O3 81.58(16) 17 . ? O1 Mo3 O3 67.59(13) 17 . ? O9 Ag1 O9 99.0(2) . 4_544 ? O9 Ag1 O7 120.87(16) . 2_445 ? O9 Ag1 O7 92.87(17) 4_544 2_445 ? O9 Ag1 O7 92.87(17) . 3_454 ? O9 Ag1 O7 120.87(16) 4_544 3_454 ? O7 Ag1 O7 128.6(2) 2_445 3_454 ? O9 Ag1 Ag1 130.52(11) . 2_445 ? O9 Ag1 Ag1 130.52(11) 4_544 2_445 ? O7 Ag1 Ag1 64.32(11) 2_445 2_445 ? O7 Ag1 Ag1 64.32(11) 3_454 2_445 ? N1 Ag2 N1 167.4(3) 2_455 . ? O2 Al1 O2 180.0(2) 17 . ? O2 Al1 O1 85.39(16) 17 17 ? O2 Al1 O1 94.61(16) . 17 ? O2 Al1 O1 94.61(16) 17 . ? O2 Al1 O1 85.39(16) . . ? O1 Al1 O1 180.0(3) 17 . ? O2 Al1 O3 94.63(16) 17 . ? O2 Al1 O3 85.37(16) . . ? O1 Al1 O3 85.05(16) 17 . ? O1 Al1 O3 94.95(16) . . ? O2 Al1 O3 85.37(16) 17 17 ? O2 Al1 O3 94.63(16) . 17 ? O1 Al1 O3 94.95(16) 17 17 ? O1 Al1 O3 85.05(16) . 17 ? O3 Al1 O3 180.0(3) . 17 ? Al1 O1 Mo1 102.95(16) . . ? Al1 O1 Mo3 104.00(16) . 17 ? Mo1 O1 Mo3 92.62(13) . 17 ? Al1 O2 Mo1 103.47(16) . . ? Al1 O2 Mo2 103.59(16) . . ? Mo1 O2 Mo2 91.56(14) . . ? Al1 O3 Mo2 103.52(16) . . ? Al1 O3 Mo3 103.36(16) . . ? Mo2 O3 Mo3 91.08(13) . . ? Mo3 O4 Mo1 118.4(2) 17 . ? Mo1 O5 Mo2 119.4(2) . . ? Mo3 O6 Mo2 119.3(2) . . ? Mo1 O7 Ag1 158.3(3) . 2_445 ? Mo2 O9 Ag1 146.2(3) . . ? O14 C1 O13 123.4(8) . . ? O14 C1 C2 121.1(8) . . ? O13 C1 C2 114.7(8) . . ? O14 C1 O13A 112.2(9) . . ? O13 C1 O13A 39.6(8) . . ? C2 C1 O13A 118.4(9) . . ? C3 C2 C1 124.1(8) . . ? C2 C3 C4 126.2(9) . . ? C5 C4 C8 117.1(6) . . ? C5 C4 C3 125.3(7) . . ? C8 C4 C3 117.6(7) . . ? N1 C5 C4 123.4(6) . . ? N1 C6 C7 122.9(6) . . ? C8 C7 C6 119.0(7) . . ? C7 C8 C4 120.0(7) . . ? O16 C9 O15 125.4(15) . . ? O16 C9 C10 114.7(18) . . ? O15 C9 C10 119.9(18) . . ? C11 C10 C9 121.9(13) . . ? C10 C11 C12 127.2(11) . . ? C13 C12 C16 120.0 . . ? C13 C12 C11 120.0(7) . . ? C16 C12 C11 120.0(7) . . ? C12 C13 C15 120.0 . . ? C13 C15 C14 120.0 . . ? N2 C14 C15 120.0 . . ? C16 N2 C14 120.0 . . ? N2 C16 C12 120.0 . . ? C5 N1 C6 117.7(6) . . ? C5 N1 Ag2 121.1(5) . . ? C6 N1 Ag2 120.7(5) . . ? OW3 OW2 OW3 151(3) 16_544 3_454 ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.998 _refine_diff_density_min -1.308 _refine_diff_density_rms 0.138 _database_code_depnum_ccdc_archive 'CCDC 954135' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H49 Ag2 Al Mo6 N4 Na2 O40' _chemical_formula_weight 1994.09 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' Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 '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 Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 9.8882(2) _cell_length_b 24.4954(5) _cell_length_c 12.1347(2) _cell_angle_alpha 90.00 _cell_angle_beta 101.6530(10) _cell_angle_gamma 90.00 _cell_volume 2878.63(10) _cell_formula_units_Z 2 _cell_measurement_temperature 220 _cell_measurement_reflns_used 19102 _cell_measurement_theta_min 1.90 _cell_measurement_theta_max 25.00 _exptl_crystal_description 'triangular block' _exptl_crystal_colour colorless _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.301 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1940 _exptl_absorpt_coefficient_mu 2.068 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.780 _exptl_absorpt_correction_T_max 0.848 _exptl_absorpt_process_details 'ABSCOR by T.Higashi 8 March, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 220 _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 Smart Apex CCD' _diffrn_measurement_method \w-2\q _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 19102 _diffrn_reflns_av_R_equivalents 0.0258 _diffrn_reflns_av_unetI/netI 0.0221 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.90 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5064 _reflns_number_gt 4827 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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 command 'omit-3 50' was used to omit the weak reflections above 50 degree. The C9, C10, C11 and O15 atoms of one pyridylacrylic acid ligand are respectively disordered into two parts, and their occupancies are refined using free variables. The carbon atoms C9, C9A, C10, C10A, C11 and C11A are restrained with the command isor so as to avoid their extensive NPD and ADP problems. The disorder of these carbon atoms of the pyridylacrylic acid ligand causes some bond lengths and bond angles deviate from the standard values, such as C(11A)-C(12) 1.68(2) A, C(11A)-C(12)-C(13) 103.7(9) degree and C(11A)-C(12)-C(16) 139.2(9) degree. The similar disorder phenomenon has been observed by Vittal et al.(Cryst. Growth Des. 2012, 12, 326). The crystal water molecules (OW5, OW6, OW7, OW8) and partial coordinated water (OW1, OW2) are also retrained with the command 'isor'. The restraint command 'simu' was used to restrain the coordinated water molecules (OW1, OW2) on Na1 centers. Furthermore, the restraint command 'dfix' was used to restrain the distance between Na atom and disordered water molecules (OW1). All these restrained refinement led to a restraint value of 79. ; _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^)+(0.0403P)^2^+14.5822P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens . _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5064 _refine_ls_number_parameters 468 _refine_ls_number_restraints 79 _refine_ls_R_factor_all 0.0372 _refine_ls_R_factor_gt 0.0354 _refine_ls_wR_factor_ref 0.0939 _refine_ls_wR_factor_gt 0.0926 _refine_ls_goodness_of_fit_ref 1.096 _refine_ls_restrained_S_all 1.109 _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 1.11553(4) 0.100867(17) 0.36331(4) 0.02471(12) Uani 1 1 d . . . Mo2 Mo 0.87625(5) 0.016487(17) 0.22759(3) 0.02513(12) Uani 1 1 d . . . Mo3 Mo 0.76202(4) -0.085087(17) 0.36678(4) 0.02490(12) Uani 1 1 d . . . Ag1 Ag 0.81273(5) -0.26057(2) 0.72124(4) 0.04008(14) Uani 1 1 d . A . Al1 Al 1.0000 0.0000 0.5000 0.0169(4) Uani 1 2 d S . . O1 O 1.1706(3) 0.02798(13) 0.4817(3) 0.0211(7) Uani 1 1 d . . . O2 O 0.9217(3) 0.05748(13) 0.4022(3) 0.0213(7) Uani 1 1 d . . . O3 O 0.9709(3) -0.04384(13) 0.3658(3) 0.0214(7) Uani 1 1 d . . . O4 O 1.1298(4) 0.12753(13) 0.5138(3) 0.0277(7) Uani 1 1 d . . . O5 O 1.0612(4) 0.04342(14) 0.2521(3) 0.0277(7) Uani 1 1 d . . . O6 O 0.7285(4) -0.01705(14) 0.2852(3) 0.0274(7) Uani 1 1 d . . . O7 O 1.2819(4) 0.10872(16) 0.3471(3) 0.0357(9) Uani 1 1 d . B . O8 O 1.0266(4) 0.15487(15) 0.2947(3) 0.0352(8) Uani 1 1 d . . . O9 O 0.7844(4) 0.07306(15) 0.1714(3) 0.0323(8) Uani 1 1 d . . . O10 O 0.8846(4) -0.02588(16) 0.1173(3) 0.0382(9) Uani 1 1 d . . . O11 O 0.7703(4) -0.12992(16) 0.2602(3) 0.0385(9) Uani 1 1 d . . . O12 O 0.6007(4) -0.09337(16) 0.3951(4) 0.0389(9) Uani 1 1 d . . . O13 O 0.3168(5) -0.33381(17) 1.2475(4) 0.0466(11) Uani 1 1 d . . . O14 O 0.3110(4) -0.37839(16) 1.0871(3) 0.0380(9) Uani 1 1 d . . . O16 O 1.1750(5) -0.1072(2) 0.3066(4) 0.0468(11) Uani 1 1 d . . . C1 C 0.3441(5) -0.3383(2) 1.1451(4) 0.0289(11) Uani 1 1 d . . . C2 C 0.4166(5) -0.2912(2) 1.1110(4) 0.0295(11) Uani 1 1 d . . . H2A H 0.4216 -0.2587 1.1514 0.035 Uiso 1 1 calc R . . C3 C 0.4756(5) -0.2950(2) 1.0215(4) 0.0289(11) Uani 1 1 d . . . H3A H 0.4678 -0.3285 0.9849 0.035 Uiso 1 1 calc R . . C4 C 0.5515(5) -0.2524(2) 0.9741(4) 0.0282(11) Uani 1 1 d . . . C5 C 0.6210(5) -0.2669(2) 0.8905(4) 0.0299(11) Uani 1 1 d . A . H5A H 0.6179 -0.3033 0.8679 0.036 Uiso 1 1 calc R . . C6 C 0.6931(6) -0.1793(2) 0.8713(5) 0.0398(13) Uani 1 1 d . A . H6A H 0.7409 -0.1541 0.8364 0.048 Uiso 1 1 calc R . . C7 C 0.6256(7) -0.1610(3) 0.9535(6) 0.0473(15) Uani 1 1 d . . . H7A H 0.6284 -0.1243 0.9734 0.057 Uiso 1 1 calc R . . C8 C 0.5540(6) -0.1979(2) 1.0053(5) 0.0387(13) Uani 1 1 d . . . H8A H 0.5077 -0.1864 1.0607 0.046 Uiso 1 1 calc R . . O15 O 1.2801(14) -0.1766(5) 0.2636(10) 0.045(3) Uani 0.60(2) 1 d P A 1 C9 C 1.1900(14) -0.1512(6) 0.3142(11) 0.033(3) Uani 0.60(2) 1 d PU A 1 C10 C 1.1130(12) -0.1864(6) 0.3807(9) 0.032(3) Uani 0.60(2) 1 d PU A 1 C11 C 1.1366(10) -0.2397(5) 0.3926(8) 0.031(3) Uani 0.60(2) 1 d PU A 1 O15A O 1.3251(17) -0.1654(6) 0.2253(14) 0.051(4) Uani 0.40(2) 1 d P A 2 C9A C 1.233(3) -0.1605(9) 0.2872(18) 0.028(5) Uani 0.40(2) 1 d PU A 2 C10A C 1.1886(15) -0.2115(6) 0.3350(11) 0.034(5) Uani 0.40(2) 1 d PU A 2 C11A C 1.1043(18) -0.2106(9) 0.4048(15) 0.028(4) Uani 0.40(2) 1 d PU A 2 C12 C 1.0687(7) -0.2694(3) 0.4641(5) 0.0499(17) Uani 1 1 d . . . C13 C 0.9861(6) -0.2532(2) 0.5389(4) 0.0351(12) Uani 1 1 d . A . H13A H 0.9683 -0.2162 0.5458 0.042 Uiso 1 1 calc R . . C14 C 0.9566(7) -0.3420(3) 0.5903(5) 0.0438(14) Uani 1 1 d . A . H14A H 0.9171 -0.3672 0.6317 0.053 Uiso 1 1 calc R . . C15 C 1.0401(8) -0.3604(3) 0.5190(6) 0.059(2) Uani 1 1 d . . . H15A H 1.0571 -0.3976 0.5143 0.071 Uiso 1 1 calc R A . C16 C 1.0957(8) -0.3256(4) 0.4576(6) 0.064(2) Uani 1 1 d . A . H16A H 1.1524 -0.3382 0.4105 0.076 Uiso 1 1 calc R . . N1 N 0.9313(5) -0.28884(19) 0.6010(4) 0.0325(10) Uani 1 1 d . . . N2 N 0.6929(5) -0.23162(19) 0.8398(4) 0.0326(10) Uani 1 1 d . . . Na1 Na 1.4867(3) 0.06125(13) 0.4288(3) 0.0695(8) Uani 1 1 d D . . OW1 O 1.4896(13) 0.0283(4) 0.2856(8) 0.062(3) Uani 0.50 1 d PDU B 3 OW2 O 1.4823(13) 0.0479(5) 0.2445(12) 0.061(3) Uani 0.50 1 d PU B 4 OW3 O 1.3546(14) -0.0331(6) 0.4067(9) 0.034(3) Uani 0.50 1 d P . 5 OW4 O 1.3841(15) -0.0278(6) 0.4583(13) 0.052(4) Uani 0.50 1 d P . 6 OW5 O 1.2313(12) -0.0007(5) 0.1130(10) 0.044(3) Uani 0.50 1 d PU . . OW6 O 1.2412(14) 0.0281(6) 0.1091(12) 0.067(4) Uani 0.50 1 d PU . . OW7 O 1.389(2) -0.0816(8) 0.1351(19) 0.106(6) Uani 0.50 1 d PU . . OW8 O 1.409(2) -0.1064(8) 0.1639(15) 0.093(5) Uani 0.50 1 d PU . . 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 0.0307(2) 0.0182(2) 0.0283(2) 0.00666(16) 0.01321(18) 0.00393(16) Mo2 0.0335(2) 0.0232(2) 0.0192(2) 0.00212(16) 0.00650(17) 0.00587(17) Mo3 0.0279(2) 0.0194(2) 0.0282(2) -0.00371(16) 0.00763(17) -0.00101(16) Ag1 0.0398(3) 0.0528(3) 0.0315(2) 0.00285(19) 0.01654(18) 0.0062(2) Al1 0.0196(9) 0.0135(9) 0.0186(9) 0.0019(7) 0.0065(7) 0.0027(7) O1 0.0251(17) 0.0177(15) 0.0222(16) 0.0021(12) 0.0090(13) 0.0018(13) O2 0.0262(17) 0.0161(15) 0.0229(16) 0.0028(12) 0.0082(13) 0.0048(13) O3 0.0284(17) 0.0163(15) 0.0208(15) 0.0001(12) 0.0080(13) 0.0033(13) O4 0.037(2) 0.0167(16) 0.0323(18) 0.0016(14) 0.0133(15) 0.0039(14) O5 0.036(2) 0.0269(18) 0.0231(16) 0.0014(14) 0.0137(14) 0.0042(15) O6 0.0271(18) 0.0272(18) 0.0275(18) 0.0002(14) 0.0043(14) 0.0023(14) O7 0.036(2) 0.035(2) 0.041(2) 0.0061(17) 0.0181(17) -0.0018(16) O8 0.046(2) 0.0239(18) 0.036(2) 0.0076(15) 0.0103(17) 0.0079(16) O9 0.038(2) 0.032(2) 0.0267(18) 0.0061(15) 0.0045(15) 0.0080(16) O10 0.053(2) 0.037(2) 0.0256(18) -0.0040(16) 0.0098(17) 0.0051(18) O11 0.046(2) 0.032(2) 0.038(2) -0.0120(17) 0.0080(17) -0.0024(17) O12 0.032(2) 0.028(2) 0.059(3) -0.0041(18) 0.0159(18) -0.0038(16) O13 0.063(3) 0.042(2) 0.043(2) -0.0149(19) 0.029(2) -0.019(2) O14 0.050(2) 0.033(2) 0.035(2) -0.0065(17) 0.0185(18) -0.0137(18) O16 0.045(3) 0.057(3) 0.043(2) 0.000(2) 0.0188(19) -0.005(2) C1 0.026(3) 0.031(3) 0.032(3) -0.005(2) 0.011(2) -0.002(2) C2 0.026(3) 0.027(3) 0.037(3) -0.005(2) 0.010(2) -0.002(2) C3 0.026(3) 0.026(3) 0.035(3) -0.003(2) 0.007(2) 0.000(2) C4 0.024(2) 0.030(3) 0.032(3) 0.004(2) 0.008(2) 0.002(2) C5 0.028(3) 0.030(3) 0.033(3) 0.001(2) 0.008(2) 0.004(2) C6 0.047(3) 0.036(3) 0.039(3) 0.012(2) 0.016(3) -0.004(3) C7 0.061(4) 0.028(3) 0.060(4) 0.000(3) 0.027(3) -0.002(3) C8 0.044(3) 0.032(3) 0.046(3) -0.002(2) 0.022(3) 0.000(2) O15 0.053(7) 0.048(6) 0.040(6) -0.003(4) 0.022(5) 0.021(5) C9 0.025(5) 0.044(7) 0.030(5) -0.006(5) 0.007(4) 0.009(5) C10 0.037(5) 0.032(6) 0.028(5) 0.002(4) 0.008(4) 0.001(5) C11 0.035(5) 0.033(6) 0.027(5) -0.005(4) 0.005(4) 0.004(4) O15A 0.070(9) 0.044(8) 0.055(8) 0.002(6) 0.049(7) 0.009(6) C9A 0.034(9) 0.023(8) 0.029(8) -0.002(6) 0.009(7) -0.002(7) C10A 0.040(7) 0.034(7) 0.032(7) 0.001(5) 0.015(5) 0.005(5) C11A 0.031(7) 0.024(8) 0.028(7) -0.003(6) 0.006(5) -0.004(6) C12 0.039(3) 0.090(5) 0.021(3) 0.000(3) 0.006(2) -0.008(3) C13 0.043(3) 0.033(3) 0.030(3) 0.001(2) 0.007(2) -0.001(2) C14 0.055(4) 0.035(3) 0.039(3) 0.001(3) 0.005(3) 0.005(3) C15 0.063(5) 0.055(4) 0.055(4) -0.022(4) 0.002(4) 0.021(4) C16 0.049(4) 0.101(7) 0.041(4) -0.032(4) 0.011(3) 0.014(4) N1 0.038(3) 0.033(2) 0.027(2) 0.0009(18) 0.0099(19) 0.004(2) N2 0.033(2) 0.036(3) 0.031(2) 0.0075(19) 0.0111(19) 0.0027(19) Na1 0.0499(16) 0.0649(19) 0.093(2) 0.0151(17) 0.0140(15) -0.0044(14) OW1 0.037(5) 0.044(6) 0.109(8) 0.030(5) 0.024(5) 0.010(5) OW2 0.044(5) 0.035(5) 0.104(7) -0.012(5) 0.015(6) 0.010(5) OW3 0.028(5) 0.034(6) 0.040(6) -0.009(5) 0.010(5) 0.010(4) OW4 0.048(9) 0.025(5) 0.095(11) -0.012(8) 0.044(9) 0.004(5) OW5 0.044(5) 0.050(5) 0.040(5) 0.001(5) 0.009(4) 0.011(5) OW6 0.052(6) 0.100(8) 0.052(6) -0.010(7) 0.020(5) -0.003(7) OW7 0.105(9) 0.102(10) 0.124(10) -0.004(8) 0.055(8) 0.018(8) OW8 0.090(8) 0.116(10) 0.086(8) -0.029(7) 0.046(7) -0.027(8) _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 O7 1.706(4) . ? Mo1 O8 1.709(4) . ? Mo1 O4 1.918(3) . ? Mo1 O5 1.948(3) . ? Mo1 O1 2.287(3) . ? Mo1 O2 2.322(3) . ? Mo2 O10 1.709(4) . ? Mo2 O9 1.721(4) . ? Mo2 O5 1.911(4) . ? Mo2 O6 1.926(4) . ? Mo2 O3 2.289(3) . ? Mo2 O2 2.306(3) . ? Mo3 O12 1.710(4) . ? Mo3 O11 1.711(4) . ? Mo3 O4 1.923(3) 3_756 ? Mo3 O6 1.933(3) . ? Mo3 O1 2.299(3) 3_756 ? Mo3 O3 2.301(3) . ? Ag1 N2 2.160(4) . ? Ag1 N1 2.162(4) . ? Al1 O1 1.875(3) 3_756 ? Al1 O1 1.875(3) . ? Al1 O2 1.902(3) 3_756 ? Al1 O2 1.902(3) . ? Al1 O3 1.923(3) 3_756 ? Al1 O3 1.923(3) . ? O1 Mo3 2.299(3) 3_756 ? O4 Mo3 1.923(3) 3_756 ? O7 Na1 2.372(5) . ? O12 Na1 2.584(5) 3_756 ? O13 C1 1.328(6) . ? O14 C1 1.214(6) . ? O14 Na1 2.526(5) 2_746 ? O16 C9 1.090(15) . ? O16 C9A 1.46(3) . ? C1 C2 1.461(7) . ? C2 C3 1.337(7) . ? C3 C4 1.469(7) . ? C4 C5 1.383(7) . ? C4 C8 1.385(8) . ? C5 N2 1.344(7) . ? C6 N2 1.337(8) . ? C6 C7 1.382(8) . ? C7 C8 1.376(8) . ? O15 C9 1.334(14) . ? C9 C10 1.49(2) . ? C10 C11 1.331(19) . ? C11 C12 1.402(12) . ? O15A C9A 1.30(3) . ? C9A C10A 1.48(2) . ? C10A C11A 1.30(2) . ? C11A C12 1.68(2) . ? C12 C13 1.396(8) . ? C12 C16 1.408(11) . ? C13 N1 1.337(7) . ? C14 N1 1.336(8) . ? C14 C15 1.387(10) . ? C15 C16 1.323(12) . ? Na1 OW4 1.865(17) 3_856 ? Na1 OW1 1.922(9) . ? Na1 OW2 2.252(15) . ? Na1 OW3 2.379(12) 3_856 ? Na1 OW4 2.462(15) . ? Na1 O14 2.526(5) 2_756 ? Na1 O12 2.584(5) 3_756 ? Na1 OW3 2.641(15) . ? Na1 Na1 3.446(6) 3_856 ? OW3 Na1 2.379(12) 3_856 ? OW4 Na1 1.865(17) 3_856 ? OW5 OW6 0.713(15) . ? OW7 OW8 0.71(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O7 Mo1 O8 105.64(18) . . ? O7 Mo1 O4 100.64(17) . . ? O8 Mo1 O4 97.56(16) . . ? O7 Mo1 O5 97.97(17) . . ? O8 Mo1 O5 100.33(17) . . ? O4 Mo1 O5 149.58(14) . . ? O7 Mo1 O1 92.74(15) . . ? O8 Mo1 O1 160.73(15) . . ? O4 Mo1 O1 72.86(12) . . ? O5 Mo1 O1 82.44(13) . . ? O7 Mo1 O2 158.36(15) . . ? O8 Mo1 O2 95.10(15) . . ? O4 Mo1 O2 82.35(13) . . ? O5 Mo1 O2 71.76(12) . . ? O1 Mo1 O2 67.45(11) . . ? O10 Mo2 O9 106.49(18) . . ? O10 Mo2 O5 97.78(17) . . ? O9 Mo2 O5 101.30(17) . . ? O10 Mo2 O6 100.69(18) . . ? O9 Mo2 O6 96.24(16) . . ? O5 Mo2 O6 149.68(14) . . ? O10 Mo2 O3 96.00(15) . . ? O9 Mo2 O3 156.27(14) . . ? O5 Mo2 O3 82.64(13) . . ? O6 Mo2 O3 71.73(13) . . ? O10 Mo2 O2 162.38(16) . . ? O9 Mo2 O2 90.16(14) . . ? O5 Mo2 O2 72.76(12) . . ? O6 Mo2 O2 82.74(13) . . ? O3 Mo2 O2 68.45(11) . . ? O12 Mo3 O11 105.36(19) . . ? O12 Mo3 O4 100.60(18) . 3_756 ? O11 Mo3 O4 96.77(17) . 3_756 ? O12 Mo3 O6 97.76(17) . . ? O11 Mo3 O6 101.29(17) . . ? O4 Mo3 O6 149.76(15) 3_756 . ? O12 Mo3 O1 92.45(16) . 3_756 ? O11 Mo3 O1 160.81(16) . 3_756 ? O4 Mo3 O1 72.50(13) 3_756 3_756 ? O6 Mo3 O1 82.94(13) . 3_756 ? O12 Mo3 O3 158.05(15) . . ? O11 Mo3 O3 95.61(16) . . ? O4 Mo3 O3 82.99(13) 3_756 . ? O6 Mo3 O3 71.34(13) . . ? O1 Mo3 O3 67.77(11) 3_756 . ? N2 Ag1 N1 179.29(17) . . ? O1 Al1 O1 180.00(18) 3_756 . ? O1 Al1 O2 85.31(13) 3_756 3_756 ? O1 Al1 O2 94.69(13) . 3_756 ? O1 Al1 O2 94.69(13) 3_756 . ? O1 Al1 O2 85.31(13) . . ? O2 Al1 O2 180.00(16) 3_756 . ? O1 Al1 O3 95.07(13) 3_756 3_756 ? O1 Al1 O3 84.93(13) . 3_756 ? O2 Al1 O3 85.00(13) 3_756 3_756 ? O2 Al1 O3 95.00(13) . 3_756 ? O1 Al1 O3 84.93(13) 3_756 . ? O1 Al1 O3 95.07(13) . . ? O2 Al1 O3 95.00(13) 3_756 . ? O2 Al1 O3 85.00(13) . . ? O3 Al1 O3 180.00(15) 3_756 . ? Al1 O1 Mo1 104.71(14) . . ? Al1 O1 Mo3 104.48(13) . 3_756 ? Mo1 O1 Mo3 91.21(11) . 3_756 ? Al1 O2 Mo2 103.30(13) . . ? Al1 O2 Mo1 102.53(14) . . ? Mo2 O2 Mo1 91.60(11) . . ? Al1 O3 Mo2 103.24(13) . . ? Al1 O3 Mo3 102.82(13) . . ? Mo2 O3 Mo3 93.03(12) . . ? Mo1 O4 Mo3 117.12(17) . 3_756 ? Mo2 O5 Mo1 118.60(17) . . ? Mo2 O6 Mo3 119.31(17) . . ? Mo1 O7 Na1 131.1(2) . . ? Mo3 O12 Na1 127.7(2) . 3_756 ? C1 O14 Na1 113.2(4) . 2_746 ? C9 O16 C9A 23.1(9) . . ? O14 C1 O13 121.8(5) . . ? O14 C1 C2 124.4(5) . . ? O13 C1 C2 113.8(4) . . ? C3 C2 C1 119.7(5) . . ? C2 C3 C4 127.6(5) . . ? C5 C4 C8 117.7(5) . . ? C5 C4 C3 118.2(5) . . ? C8 C4 C3 124.0(5) . . ? N2 C5 C4 123.8(5) . . ? N2 C6 C7 123.0(5) . . ? C8 C7 C6 119.0(6) . . ? C7 C8 C4 119.4(5) . . ? O16 C9 O15 121.0(13) . . ? O16 C9 C10 122.8(14) . . ? O15 C9 C10 116.2(14) . . ? C11 C10 C9 122.0(11) . . ? C10 C11 C12 118.7(10) . . ? O15A C9A O16 121.2(13) . . ? O15A C9A C10A 116(2) . . ? O16 C9A C10A 122(2) . . ? C11A C10A C9A 121.2(19) . . ? C10A C11A C12 118.7(17) . . ? C13 C12 C11 132.2(8) . . ? C13 C12 C16 117.1(6) . . ? C11 C12 C16 110.6(8) . . ? C13 C12 C11A 103.7(9) . . ? C11 C12 C11A 28.6(6) . . ? C16 C12 C11A 139.2(9) . . ? N1 C13 C12 122.6(6) . . ? N1 C14 C15 121.7(6) . . ? C16 C15 C14 120.6(7) . . ? C15 C16 C12 119.6(6) . . ? C14 N1 C13 118.4(5) . . ? C14 N1 Ag1 121.0(4) . . ? C13 N1 Ag1 120.5(4) . . ? C6 N2 C5 117.1(5) . . ? C6 N2 Ag1 122.4(4) . . ? C5 N2 Ag1 120.4(4) . . ? OW4 Na1 OW1 110.3(6) 3_856 . ? OW4 Na1 OW2 122.6(5) 3_856 . ? OW1 Na1 OW2 16.6(3) . . ? OW4 Na1 O7 157.5(5) 3_856 . ? OW1 Na1 O7 89.8(4) . . ? OW2 Na1 O7 79.2(3) . . ? OW4 Na1 OW3 10.7(6) 3_856 3_856 ? OW1 Na1 OW3 120.6(5) . 3_856 ? OW2 Na1 OW3 131.9(5) . 3_856 ? O7 Na1 OW3 148.9(4) . 3_856 ? OW4 Na1 OW4 75.2(6) 3_856 . ? OW1 Na1 OW4 80.9(5) . . ? OW2 Na1 OW4 95.2(5) . . ? O7 Na1 OW4 98.8(4) . . ? OW3 Na1 OW4 80.9(6) 3_856 . ? OW4 Na1 O14 83.0(5) 3_856 2_756 ? OW1 Na1 O14 91.2(4) . 2_756 ? OW2 Na1 O14 82.3(4) . 2_756 ? O7 Na1 O14 107.68(17) . 2_756 ? OW3 Na1 O14 80.5(4) 3_856 2_756 ? OW4 Na1 O14 152.3(4) . 2_756 ? OW4 Na1 O12 79.6(4) 3_856 3_756 ? OW1 Na1 O12 160.8(4) . 3_756 ? OW2 Na1 O12 157.4(4) . 3_756 ? O7 Na1 O12 78.26(16) . 3_756 ? OW3 Na1 O12 70.6(3) 3_856 3_756 ? OW4 Na1 O12 86.2(3) . 3_756 ? O14 Na1 O12 106.69(17) 2_756 3_756 ? OW4 Na1 OW3 86.6(6) 3_856 . ? OW1 Na1 OW3 68.8(4) . . ? OW2 Na1 OW3 82.1(4) . . ? O7 Na1 OW3 91.3(3) . . ? OW3 Na1 OW3 93.5(4) 3_856 . ? OW4 Na1 OW3 14.0(4) . . ? O14 Na1 OW3 152.5(3) 2_756 . ? O12 Na1 OW3 96.3(3) 3_756 . ? OW4 Na1 Na1 43.7(5) 3_856 3_856 ? OW1 Na1 Na1 94.2(4) . 3_856 ? OW2 Na1 Na1 110.8(4) . 3_856 ? O7 Na1 Na1 127.51(18) . 3_856 ? OW3 Na1 Na1 49.9(4) 3_856 3_856 ? OW4 Na1 Na1 31.5(4) . 3_856 ? O14 Na1 Na1 124.49(17) 2_756 3_856 ? O12 Na1 Na1 81.66(15) 3_756 3_856 ? OW3 Na1 Na1 43.6(3) . 3_856 ? Na1 OW3 Na1 86.5(4) 3_856 . ? Na1 OW4 Na1 104.8(6) 3_856 . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.473 _refine_diff_density_min -1.495 _refine_diff_density_rms 0.127 _database_code_depnum_ccdc_archive 'CCDC 954136'