# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_email zhzhou@xmu.edu.cn _publ_contact_author_name 'Zhao-Hui Zhou' loop_ _publ_author_name 'Q.L. Chen' 'Y.D. Lin' 'H.L. Wan' 'Z.H. Zhou' # Attachment 'Cif2.cif' data_sad2 _database_code_depnum_ccdc_archive 'CCDC 847782' #TrackingRef 'Cif2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H28 Mo8 N12 O26' _chemical_formula_weight 1596.04 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' Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.3045(3) _cell_length_b 10.5573(5) _cell_length_c 12.4212(4) _cell_angle_alpha 106.644(4) _cell_angle_beta 103.017(3) _cell_angle_gamma 109.367(4) _cell_volume 1031.34(7) _cell_formula_units_Z 1 _cell_measurement_temperature 446(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.570 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 764 _exptl_absorpt_coefficient_mu 2.454 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.7915 _exptl_absorpt_correction_T_max 0.9300 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 446(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12699 _diffrn_reflns_av_R_equivalents 0.0420 _diffrn_reflns_av_sigmaI/netI 0.0512 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.12 _diffrn_reflns_theta_max 26.99 _reflns_number_total 4446 _reflns_number_gt 3859 _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 ? _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. ; _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^)+(0.0300P)^2^+11.8816P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4446 _refine_ls_number_parameters 289 _refine_ls_number_restraints 546 _refine_ls_R_factor_all 0.0604 _refine_ls_R_factor_gt 0.0492 _refine_ls_wR_factor_ref 0.1046 _refine_ls_wR_factor_gt 0.1001 _refine_ls_goodness_of_fit_ref 1.074 _refine_ls_restrained_S_all 1.031 _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 0.69156(7) 0.20596(6) 0.18834(5) 0.01299(14) Uani 1 1 d . . . Mo2 Mo 0.93139(7) 0.19822(6) 0.47906(5) 0.01257(14) Uani 1 1 d . . . Mo3 Mo 1.11240(6) 0.44616(6) 0.75407(5) 0.01205(13) Uani 1 1 d . . . Mo4 Mo 0.79719(6) 0.45228(6) 0.47400(5) 0.01024(13) Uani 1 1 d . . . O1 O 0.7048(5) 0.4245(5) 0.3119(4) 0.0141(8) Uani 1 1 d U . . O6 O 0.7753(6) 0.1064(6) 0.5187(4) 0.0206(10) Uani 1 1 d U . . O2 O 0.9698(5) 0.4326(5) 0.5765(4) 0.0120(8) Uani 1 1 d U . . O12 O 0.6333(5) 0.3733(5) 0.5095(4) 0.0186(10) Uani 1 1 d U . . O9 O 0.9419(5) 0.3665(5) 0.7852(4) 0.0172(10) Uani 1 1 d U . . O10 O 1.1200(5) 0.6420(5) 0.8074(4) 0.0145(9) Uani 1 1 d U . . O11 O 1.2709(6) 0.4672(5) 0.8669(4) 0.0187(10) Uani 1 1 d U . . O3 O 0.5509(6) 0.1988(6) 0.0686(4) 0.0210(10) Uani 1 1 d U . . O7 O 1.1021(5) 0.2770(5) 0.6321(4) 0.0149(9) Uani 1 1 d U . . O13 O 0.8028(5) 0.2507(5) 0.3690(4) 0.0142(9) Uani 1 1 d U . . O5 O 0.8544(5) 0.6383(5) 0.5501(4) 0.0140(9) Uani 1 1 d U . . O8 O 0.9685(6) 0.0659(6) 0.3912(5) 0.0232(11) Uani 1 1 d U . . O4 O 0.7330(6) 0.0603(6) 0.1353(5) 0.0239(11) Uani 1 1 d U . . N1 N 0.4725(7) 0.0997(7) 0.2283(5) 0.0174(10) Uani 1 1 d U . . N2 N 0.3071(7) 0.0118(7) 0.3147(5) 0.0214(12) Uani 1 1 d U . . H2A H 0.2732 -0.0134 0.3676 0.026 Uiso 1 1 calc R . . C1 C 0.4606(8) 0.0725(8) 0.3241(6) 0.0189(12) Uani 1 1 d U . . H1A H 0.5491 0.0935 0.3898 0.023 Uiso 1 1 calc R . . C2 C 0.3146(8) 0.0492(8) 0.1526(7) 0.0212(13) Uani 1 1 d U . . H2B H 0.2845 0.0517 0.0769 0.025 Uiso 1 1 calc R . . C3 C 0.2106(9) -0.0042(9) 0.2052(7) 0.0252(14) Uani 1 1 d U . . H3A H 0.0974 -0.0437 0.1741 0.030 Uiso 1 1 calc R . . C6 C 0.4019(7) 0.3913(7) 0.2000(6) 0.0103(11) Uani 1 1 d U . . H6A H 0.5082 0.4066 0.2375 0.012 Uiso 1 1 calc R . . N5 N 1.3595(8) 0.2172(7) 0.7108(6) 0.0284(13) Uani 1 1 d U . . H5A H 1.2592 0.1988 0.6776 0.034 Uiso 1 1 calc R . . C4 C 0.1502(7) 0.3485(8) 0.1643(6) 0.0148(12) Uani 1 1 d U . . H4A H 0.0493 0.3285 0.1730 0.018 Uiso 1 1 calc R . . C9 C 1.6093(8) 0.2751(8) 0.7398(7) 0.0217(14) Uani 1 1 d U . . H9A H 1.7088 0.3039 0.7286 0.026 Uiso 1 1 calc R . . N3 N 0.1847(8) 0.3651(8) 0.0673(6) 0.0331(15) Uani 1 1 d U . . H3B H 0.1181 0.3595 0.0037 0.040 Uiso 1 1 calc R . . C5 C 0.3421(8) 0.3919(8) 0.0890(6) 0.0189(13) Uani 1 1 d U . . H5B H 0.3996 0.4078 0.0382 0.023 Uiso 1 1 calc R . . N4 N 0.2852(8) 0.3656(8) 0.2455(6) 0.0302(13) Uani 1 1 d U . . H4B H 0.2941 0.3608 0.3145 0.036 Uiso 1 1 calc R . . C7 C 1.4749(10) 0.2560(9) 0.6687(8) 0.0291(15) Uani 1 1 d U . . H7A H 1.4613 0.2681 0.5964 0.035 Uiso 1 1 calc R . . C8 C 1.4274(10) 0.2111(9) 0.8185(8) 0.0305(15) Uani 1 1 d U . . H8A H 1.3742 0.1868 0.8696 0.037 Uiso 1 1 calc R . . N6 N 1.5822(10) 0.2462(9) 0.8348(8) 0.052(2) Uani 1 1 d U . . H6C H 1.6536 0.2502 0.8949 0.062 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mo1 0.0118(3) 0.0150(3) 0.0097(3) 0.0049(2) 0.0038(2) 0.0026(2) Mo2 0.0125(3) 0.0145(3) 0.0146(3) 0.0096(2) 0.0056(2) 0.0064(2) Mo3 0.0103(3) 0.0158(3) 0.0139(3) 0.0099(2) 0.0060(2) 0.0055(2) Mo4 0.0085(2) 0.0141(3) 0.0107(3) 0.0077(2) 0.0042(2) 0.0047(2) O1 0.0125(18) 0.018(2) 0.0152(19) 0.0110(16) 0.0044(15) 0.0066(15) O6 0.017(2) 0.022(3) 0.020(2) 0.012(2) 0.0054(19) 0.0041(19) O2 0.0116(18) 0.016(2) 0.0121(19) 0.0082(16) 0.0052(15) 0.0071(16) O12 0.012(2) 0.021(3) 0.021(2) 0.008(2) 0.0083(18) 0.0034(18) O9 0.015(2) 0.023(3) 0.020(2) 0.014(2) 0.0115(19) 0.0079(19) O10 0.012(2) 0.018(2) 0.013(2) 0.0067(18) 0.0059(17) 0.0048(17) O11 0.017(2) 0.021(3) 0.021(2) 0.011(2) 0.0073(19) 0.0084(19) O3 0.018(2) 0.024(3) 0.016(2) 0.010(2) 0.0041(19) 0.002(2) O7 0.0163(19) 0.016(2) 0.019(2) 0.0123(17) 0.0070(16) 0.0095(16) O13 0.0149(19) 0.012(2) 0.016(2) 0.0069(16) 0.0060(16) 0.0053(16) O5 0.015(2) 0.015(2) 0.014(2) 0.0062(18) 0.0070(17) 0.0064(17) O8 0.026(3) 0.023(3) 0.021(3) 0.007(2) 0.007(2) 0.011(2) O4 0.027(3) 0.020(3) 0.023(3) 0.008(2) 0.011(2) 0.008(2) N1 0.015(2) 0.019(2) 0.016(2) 0.0080(19) 0.0063(18) 0.0045(18) N2 0.019(2) 0.025(3) 0.018(3) 0.010(2) 0.009(2) 0.002(2) C1 0.016(2) 0.021(3) 0.019(3) 0.009(2) 0.005(2) 0.005(2) C2 0.015(2) 0.026(3) 0.019(3) 0.009(2) 0.004(2) 0.004(2) C3 0.017(3) 0.029(3) 0.025(3) 0.012(3) 0.006(2) 0.003(2) C6 0.008(2) 0.017(2) 0.012(2) 0.0068(19) 0.0081(18) 0.0087(18) N5 0.022(3) 0.022(3) 0.036(3) 0.007(2) 0.007(2) 0.009(2) C4 0.008(2) 0.021(3) 0.020(3) 0.008(2) 0.008(2) 0.009(2) C9 0.017(3) 0.017(3) 0.037(3) 0.012(3) 0.016(2) 0.008(2) N3 0.027(3) 0.031(3) 0.031(3) 0.011(3) 0.003(2) 0.008(2) C5 0.018(2) 0.021(3) 0.021(3) 0.009(2) 0.011(2) 0.010(2) N4 0.027(2) 0.029(3) 0.027(2) 0.008(2) 0.008(2) 0.008(2) C7 0.036(3) 0.018(3) 0.033(3) 0.012(3) 0.015(3) 0.009(2) C8 0.038(3) 0.021(3) 0.033(3) 0.011(3) 0.021(3) 0.007(2) N6 0.049(3) 0.029(3) 0.051(4) 0.004(3) -0.011(3) 0.015(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mo1 O4 1.695(5) . ? Mo1 O3 1.711(5) . ? Mo1 O10 1.922(4) 2_766 ? Mo1 O13 2.087(5) . ? Mo1 N1 2.217(5) . ? Mo1 O1 2.323(5) . ? Mo2 O8 1.696(5) . ? Mo2 O6 1.718(5) . ? Mo2 O7 1.920(5) . ? Mo2 O13 1.935(5) . ? Mo2 O2 2.285(5) . ? Mo2 O5 2.342(4) 2_766 ? Mo3 O11 1.692(5) . ? Mo3 O9 1.718(4) . ? Mo3 O7 1.940(5) . ? Mo3 O10 1.954(5) . ? Mo3 O2 2.240(4) . ? Mo3 O1 2.271(4) 2_766 ? Mo4 O12 1.699(4) . ? Mo4 O5 1.747(5) . ? Mo4 O1 1.895(4) . ? Mo4 O2 1.923(4) . ? Mo4 O13 2.179(5) . ? Mo4 O2 2.423(4) 2_766 ? O1 Mo3 2.271(4) 2_766 ? O2 Mo4 2.423(4) 2_766 ? O10 Mo1 1.922(4) 2_766 ? O5 Mo2 2.342(4) 2_766 ? N1 C1 1.322(9) . ? N1 C2 1.377(9) . ? N2 C1 1.318(9) . ? N2 C3 1.380(10) . ? N2 H2A 0.8600 . ? C1 H1A 0.9300 . ? C2 C3 1.347(10) . ? C2 H2B 0.9300 . ? C3 H3A 0.9300 . ? C6 N4 1.319(8) . ? C6 C5 1.368(9) . ? C6 H6A 0.9300 . ? N5 C7 1.294(10) . ? N5 C8 1.374(11) . ? N5 H5A 0.8600 . ? C4 N4 1.343(9) . ? C4 N3 1.357(9) . ? C4 H4A 0.9300 . ? C9 C7 1.272(11) . ? C9 N6 1.356(12) . ? C9 H9A 0.9300 . ? N3 C5 1.342(9) . ? N3 H3B 0.8600 . ? C5 H5B 0.9300 . ? N4 H4B 0.8600 . ? C7 H7A 0.9300 . ? C8 N6 1.314(11) . ? C8 H8A 0.9300 . ? N6 H6C 0.8600 . ? 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 O4 Mo1 O3 106.0(3) . . ? O4 Mo1 O10 99.8(2) . 2_766 ? O3 Mo1 O10 98.2(2) . 2_766 ? O4 Mo1 O13 94.9(2) . . ? O3 Mo1 O13 155.2(2) . . ? O10 Mo1 O13 91.02(18) 2_766 . ? O4 Mo1 N1 99.5(2) . . ? O3 Mo1 N1 82.8(2) . . ? O10 Mo1 N1 159.5(2) 2_766 . ? O13 Mo1 N1 80.70(19) . . ? O4 Mo1 O1 162.2(2) . . ? O3 Mo1 O1 91.5(2) . . ? O10 Mo1 O1 73.80(17) 2_766 . ? O13 Mo1 O1 68.94(16) . . ? N1 Mo1 O1 85.71(19) . . ? O8 Mo2 O6 104.9(2) . . ? O8 Mo2 O7 103.9(2) . . ? O6 Mo2 O7 97.1(2) . . ? O8 Mo2 O13 105.4(2) . . ? O6 Mo2 O13 96.3(2) . . ? O7 Mo2 O13 143.2(2) . . ? O8 Mo2 O2 155.3(2) . . ? O6 Mo2 O2 99.9(2) . . ? O7 Mo2 O2 72.70(17) . . ? O13 Mo2 O2 71.30(17) . . ? O8 Mo2 O5 85.5(2) . 2_766 ? O6 Mo2 O5 169.5(2) . 2_766 ? O7 Mo2 O5 78.73(18) . 2_766 ? O13 Mo2 O5 81.97(17) . 2_766 ? O2 Mo2 O5 69.78(15) . 2_766 ? O11 Mo3 O9 105.4(2) . . ? O11 Mo3 O7 97.6(2) . . ? O9 Mo3 O7 100.4(2) . . ? O11 Mo3 O10 101.2(2) . . ? O9 Mo3 O10 95.6(2) . . ? O7 Mo3 O10 151.14(19) . . ? O11 Mo3 O2 160.04(19) . . ? O9 Mo3 O2 93.90(19) . . ? O7 Mo3 O2 73.38(17) . . ? O10 Mo3 O2 81.73(18) . . ? O11 Mo3 O1 88.4(2) . 2_766 ? O9 Mo3 O1 164.55(19) . 2_766 ? O7 Mo3 O1 84.41(18) . 2_766 ? O10 Mo3 O1 74.46(17) . 2_766 ? O2 Mo3 O1 73.25(16) . 2_766 ? O12 Mo4 O5 102.5(2) . . ? O12 Mo4 O1 103.8(2) . . ? O5 Mo4 O1 102.0(2) . . ? O12 Mo4 O2 103.6(2) . . ? O5 Mo4 O2 98.8(2) . . ? O1 Mo4 O2 140.82(19) . . ? O12 Mo4 O13 96.8(2) . . ? O5 Mo4 O13 160.54(18) . . ? O1 Mo4 O13 75.47(18) . . ? O2 Mo4 O13 73.96(18) . . ? O12 Mo4 O2 179.3(2) . 2_766 ? O5 Mo4 O2 76.90(18) . 2_766 ? O1 Mo4 O2 76.01(17) . 2_766 ? O2 Mo4 O2 76.89(18) . 2_766 ? O13 Mo4 O2 83.82(16) . 2_766 ? Mo4 O1 Mo3 112.9(2) . 2_766 ? Mo4 O1 Mo1 108.4(2) . . ? Mo3 O1 Mo1 91.30(16) 2_766 . ? Mo4 O2 Mo3 152.6(2) . . ? Mo4 O2 Mo2 103.99(19) . . ? Mo3 O2 Mo2 92.70(16) . . ? Mo4 O2 Mo4 103.11(18) . 2_766 ? Mo3 O2 Mo4 96.38(15) . 2_766 ? Mo2 O2 Mo4 96.04(15) . 2_766 ? Mo1 O10 Mo3 115.9(2) 2_766 . ? Mo2 O7 Mo3 116.0(2) . . ? Mo2 O13 Mo1 144.7(2) . . ? Mo2 O13 Mo4 107.6(2) . . ? Mo1 O13 Mo4 107.06(19) . . ? Mo4 O5 Mo2 117.1(2) . 2_766 ? C1 N1 C2 105.5(6) . . ? C1 N1 Mo1 130.1(5) . . ? C2 N1 Mo1 124.4(5) . . ? C1 N2 C3 108.0(6) . . ? C1 N2 H2A 126.0 . . ? C3 N2 H2A 126.0 . . ? N2 C1 N1 111.3(6) . . ? N2 C1 H1A 124.4 . . ? N1 C1 H1A 124.4 . . ? C3 C2 N1 109.6(7) . . ? C3 C2 H2B 125.2 . . ? N1 C2 H2B 125.2 . . ? C2 C3 N2 105.5(6) . . ? C2 C3 H3A 127.2 . . ? N2 C3 H3A 127.2 . . ? N4 C6 C5 109.4(6) . . ? N4 C6 H6A 125.3 . . ? C5 C6 H6A 125.3 . . ? C7 N5 C8 107.2(7) . . ? C7 N5 H5A 126.4 . . ? C8 N5 H5A 126.4 . . ? N4 C4 N3 108.9(6) . . ? N4 C4 H4A 125.5 . . ? N3 C4 H4A 125.5 . . ? C7 C9 N6 108.1(7) . . ? C7 C9 H9A 126.0 . . ? N6 C9 H9A 126.0 . . ? C5 N3 C4 107.4(6) . . ? C5 N3 H3B 126.3 . . ? C4 N3 H3B 126.3 . . ? N3 C5 C6 106.9(6) . . ? N3 C5 H5B 126.5 . . ? C6 C5 H5B 126.5 . . ? C6 N4 C4 107.4(6) . . ? C6 N4 H4B 126.3 . . ? C4 N4 H4B 126.3 . . ? C9 C7 N5 110.7(8) . . ? C9 C7 H7A 124.6 . . ? N5 C7 H7A 124.6 . . ? N6 C8 N5 106.4(7) . . ? N6 C8 H8A 126.8 . . ? N5 C8 H8A 126.8 . . ? C8 N6 C9 107.6(7) . . ? C8 N6 H6C 126.2 . . ? C9 N6 H6C 126.2 . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 26.99 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 3.141 _refine_diff_density_min -1.077 _refine_diff_density_rms 0.202 # Attachment '6.cif' data_sad6 _database_code_depnum_ccdc_archive 'CCDC 847783' #TrackingRef '6.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C15 H19 Mo3 N10 Na0 O9' _chemical_formula_weight 772.23 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' Na Na 0.0362 0.0249 '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 ? _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.4113(3) _cell_length_b 8.5644(3) _cell_length_c 28.5006(9) _cell_angle_alpha 90.00 _cell_angle_beta 95.693(3) _cell_angle_gamma 90.00 _cell_volume 2528.77(14) _cell_formula_units_Z 4 _cell_measurement_temperature 446(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.028 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1520 _exptl_absorpt_coefficient_mu 1.530 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8620 _exptl_absorpt_correction_T_max 0.9138 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 446(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12174 _diffrn_reflns_av_R_equivalents 0.0536 _diffrn_reflns_av_sigmaI/netI 0.0783 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 2.77 _diffrn_reflns_theta_max 27.25 _reflns_number_total 5481 _reflns_number_gt 4218 _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 ? _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. ; _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^)+(0.0323P)^2^+5.0352P] 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 5481 _refine_ls_number_parameters 337 _refine_ls_number_restraints 370 _refine_ls_R_factor_all 0.0817 _refine_ls_R_factor_gt 0.0577 _refine_ls_wR_factor_ref 0.1245 _refine_ls_wR_factor_gt 0.1168 _refine_ls_goodness_of_fit_ref 1.274 _refine_ls_restrained_S_all 1.256 _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 0.41021(5) -0.67927(7) 0.17163(2) 0.01265(15) Uani 1 1 d . . . Mo2 Mo 0.46767(5) -0.67174(7) 0.054189(19) 0.01287(15) Uani 1 1 d . . . Mo3 Mo 0.24319(5) -0.51193(7) 0.12175(2) 0.01189(14) Uani 1 1 d U . . O1 O 0.4247(4) -0.4749(5) 0.14199(16) 0.0154(10) Uani 1 1 d . . . O2 O 0.3154(4) -0.5767(5) 0.05538(16) 0.0150(10) Uani 1 1 d . . . O3 O 0.3761(5) -0.6421(6) 0.22709(17) 0.0222(11) Uani 1 1 d . . . O4 O 0.2465(4) -0.7333(5) 0.13593(16) 0.0144(10) Uani 1 1 d . . . O5 O 0.4991(4) -0.7674(6) 0.10981(16) 0.0168(11) Uani 1 1 d . . . O6 O 0.4558(5) -0.8134(6) 0.01013(17) 0.0241(12) Uani 1 1 d . . . O7 O 0.1571(5) -0.4291(6) 0.16182(16) 0.0171(11) Uani 1 1 d . . . O8 O 0.5908(5) -0.5408(6) 0.04552(17) 0.0223(12) Uani 1 1 d . . . N1 N 0.2532(6) -0.2826(7) 0.0876(2) 0.0249(5) Uani 1 1 d U . . N2 N 0.6168(6) -0.6500(7) 0.1952(2) 0.0226(5) Uani 1 1 d U . . N3 N 0.4267(6) -0.9292(7) 0.1892(2) 0.0219(5) Uani 1 1 d U . . N4 N 0.0639(6) -0.5628(7) 0.0771(2) 0.0251(5) Uani 1 1 d U . . N5 N 0.3293(6) -0.0863(7) 0.0500(2) 0.0256(5) Uani 1 1 d U . . H5A H 0.3750 -0.0336 0.0321 0.031 Uiso 1 1 calc R . . N6 N -0.1430(6) -0.5729(7) 0.0525(2) 0.0260(5) Uani 1 1 d U . . H6B H -0.2246 -0.5551 0.0505 0.031 Uiso 1 1 calc R . . N7 N 0.7971(6) -0.5507(7) 0.2304(2) 0.0236(6) Uani 1 1 d U . . H7B H 0.8508 -0.4954 0.2483 0.028 Uiso 1 1 calc R . . N8 N 0.4458(6) -1.1827(7) 0.1832(2) 0.0219(6) Uani 1 1 d U . . H8B H 0.4664 -1.2726 0.1728 0.026 Uiso 1 1 calc R . . C1 C 0.6665(7) -0.5419(9) 0.2280(3) 0.0230(6) Uani 1 1 d U . . H1A H 0.6190 -0.4750 0.2453 0.028 Uiso 1 1 calc R . . C2 C 0.8274(7) -0.6606(9) 0.2001(3) 0.0226(6) Uani 1 1 d U . . H2A H 0.9103 -0.6925 0.1949 0.027 Uiso 1 1 calc R . . C3 C 0.7180(7) -0.7158(9) 0.1788(3) 0.0228(6) Uani 1 1 d U . . H3B H 0.7131 -0.7914 0.1552 0.027 Uiso 1 1 calc R . . C5 C 0.4680(7) -1.0444(9) 0.1637(3) 0.0221(6) Uani 1 1 d U . . H5B H 0.5070 -1.0312 0.1360 0.026 Uiso 1 1 calc R . . C7 C 0.0456(7) -0.6600(9) 0.0387(3) 0.0256(5) Uani 1 1 d U . . H7C H 0.1106 -0.7122 0.0249 0.031 Uiso 1 1 calc R . . C8 C 0.3722(7) -0.9994(9) 0.2256(3) 0.0219(6) Uani 1 1 d U . . H8C H 0.3326 -0.9474 0.2489 0.026 Uiso 1 1 calc R . . C9 C 0.3848(7) -1.1554(9) 0.2223(3) 0.0220(6) Uani 1 1 d U . . H9B H 0.3572 -1.2298 0.2428 0.026 Uiso 1 1 calc R . . C11 C -0.0536(7) -0.5123(9) 0.0842(3) 0.0262(5) Uani 1 1 d U . . H11A H -0.0711 -0.4437 0.1080 0.031 Uiso 1 1 calc R . . C12 C 0.3389(7) -0.2378(9) 0.0589(3) 0.0253(5) Uani 1 1 d U . . H12A H 0.3978 -0.3041 0.0466 0.030 Uiso 1 1 calc R . . C13 C -0.0806(7) -0.6675(9) 0.0242(3) 0.0258(5) Uani 1 1 d U . . H13A H -0.1185 -0.7269 -0.0008 0.031 Uiso 1 1 calc R . . C14 C 0.1877(7) -0.1505(9) 0.0969(3) 0.0257(5) Uani 1 1 d U . . H14A H 0.1205 -0.1456 0.1161 0.031 Uiso 1 1 calc R . . C15 C 0.2336(7) -0.0291(9) 0.0745(3) 0.0256(5) Uani 1 1 d U . . H15A H 0.2060 0.0740 0.0755 0.031 Uiso 1 1 calc R . . N9 N -0.1973(6) -0.1883(8) 0.1470(2) 0.0280(5) Uani 1 1 d U . . N10 N -0.2107(6) -0.0607(8) 0.0833(2) 0.0286(5) Uani 1 1 d U . . C4 C -0.1466(8) -0.0638(9) 0.1259(3) 0.0272(5) Uani 1 1 d U . . C6 C -0.2888(8) -0.2611(9) 0.1172(3) 0.0274(5) Uani 1 1 d U . . C10 C -0.2948(7) -0.1820(9) 0.0780(3) 0.0273(5) Uani 1 1 d U . . H4A H -0.3481 -0.2051 0.0507 0.033 Uiso 1 1 calc R . . H6C H -0.3361 -0.3487 0.1245 0.033 Uiso 1 1 d R . . H9A H -0.1708 -0.2170 0.1754 0.033 Uiso 1 1 d R . . O1W O 0.0209(5) -0.8420(7) 0.1731(2) 0.0346(14) Uani 1 1 d D . . H1W2 H 0.090(4) -0.835(11) 0.160(3) 0.041 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 0.0120(3) 0.0122(3) 0.0137(3) -0.0007(2) 0.0013(2) 0.0009(2) Mo2 0.0108(3) 0.0159(3) 0.0122(3) -0.0013(2) 0.0023(2) 0.0002(2) Mo3 0.0099(3) 0.0119(3) 0.0141(3) -0.0014(2) 0.0021(2) 0.0008(2) O1 0.016(3) 0.010(2) 0.020(2) 0.000(2) 0.000(2) -0.0007(19) O2 0.012(2) 0.015(3) 0.019(2) -0.002(2) 0.0041(19) 0.0001(19) O3 0.021(3) 0.022(3) 0.023(3) -0.003(2) 0.005(2) 0.004(2) O4 0.010(2) 0.011(2) 0.022(3) 0.001(2) 0.0039(19) -0.0021(18) O5 0.015(3) 0.019(3) 0.016(2) -0.001(2) 0.0011(19) 0.003(2) O6 0.024(3) 0.028(3) 0.020(3) -0.003(2) 0.000(2) 0.006(2) O7 0.017(3) 0.020(3) 0.014(2) 0.001(2) 0.0054(19) 0.007(2) O8 0.012(3) 0.027(3) 0.028(3) 0.006(2) -0.001(2) -0.002(2) N1 0.0230(10) 0.0227(9) 0.0282(11) 0.0034(8) -0.0018(8) -0.0040(9) N2 0.0202(12) 0.0236(13) 0.0232(12) -0.0008(10) -0.0012(10) 0.0012(10) N3 0.0198(12) 0.0229(13) 0.0224(12) -0.0006(10) -0.0008(10) 0.0010(10) N4 0.0219(10) 0.0243(10) 0.0281(11) 0.0018(9) -0.0030(8) -0.0041(9) N5 0.0238(11) 0.0234(11) 0.0288(12) 0.0032(9) -0.0013(9) -0.0040(10) N6 0.0227(10) 0.0254(10) 0.0289(11) 0.0016(9) -0.0024(8) -0.0037(9) N7 0.0210(13) 0.0247(13) 0.0244(13) -0.0008(11) -0.0015(11) 0.0011(11) N8 0.0200(13) 0.0227(13) 0.0224(13) -0.0006(11) -0.0008(11) 0.0009(11) C1 0.0204(13) 0.0241(13) 0.0236(13) -0.0010(11) -0.0014(11) 0.0013(11) C2 0.0199(13) 0.0238(13) 0.0234(13) -0.0009(11) -0.0013(11) 0.0012(11) C3 0.0203(13) 0.0239(13) 0.0235(12) -0.0009(10) -0.0012(10) 0.0013(10) C5 0.0201(13) 0.0229(13) 0.0226(12) -0.0006(11) -0.0008(10) 0.0010(11) C7 0.0225(11) 0.0249(11) 0.0284(11) 0.0016(9) -0.0026(9) -0.0038(9) C8 0.0200(13) 0.0228(13) 0.0225(13) -0.0005(11) -0.0005(11) 0.0010(11) C9 0.0200(13) 0.0229(13) 0.0226(13) -0.0004(11) -0.0006(11) 0.0009(11) C11 0.0232(10) 0.0254(10) 0.0291(11) 0.0015(8) -0.0021(8) -0.0038(9) C12 0.0235(11) 0.0231(11) 0.0286(12) 0.0030(9) -0.0015(9) -0.0039(10) C13 0.0227(11) 0.0251(11) 0.0287(11) 0.0015(9) -0.0028(9) -0.0038(9) C14 0.0234(10) 0.0239(10) 0.0289(11) 0.0025(9) -0.0016(8) -0.0038(9) C15 0.0237(11) 0.0233(11) 0.0291(12) 0.0030(9) -0.0013(9) -0.0037(10) N9 0.0251(11) 0.0273(11) 0.0307(11) 0.0006(9) -0.0015(9) -0.0035(9) N10 0.0257(11) 0.0278(11) 0.0313(12) 0.0008(10) -0.0013(9) -0.0037(10) C4 0.0244(11) 0.0264(10) 0.0301(11) 0.0010(9) -0.0016(9) -0.0039(9) C6 0.0243(11) 0.0266(10) 0.0303(11) 0.0008(9) -0.0016(9) -0.0037(9) C10 0.0244(11) 0.0267(11) 0.0301(11) 0.0006(9) -0.0017(9) -0.0037(9) O1W 0.021(3) 0.043(4) 0.043(3) -0.009(3) 0.017(3) -0.007(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mo1 O3 1.684(5) . ? Mo1 O4 1.952(4) . ? Mo1 O1 1.956(5) . ? Mo1 N3 2.201(6) . ? Mo1 N2 2.203(6) . ? Mo1 O5 2.203(5) . ? Mo1 Mo3 2.5706(8) . ? Mo2 O8 1.739(5) . ? Mo2 O6 1.741(5) . ? Mo2 O2 1.785(5) . ? Mo2 O5 1.785(5) . ? Mo3 O7 1.677(5) . ? Mo3 O4 1.938(5) . ? Mo3 O1 1.946(4) . ? Mo3 O2 2.176(5) . ? Mo3 N4 2.196(6) . ? Mo3 N1 2.199(6) . ? N1 C12 1.326(10) . ? N1 C14 1.361(10) . ? N2 C3 1.321(9) . ? N2 C1 1.380(9) . ? N3 C5 1.323(9) . ? N3 C8 1.369(10) . ? N4 C11 1.331(10) . ? N4 C7 1.374(10) . ? N5 C12 1.324(10) . ? N5 C15 1.363(10) . ? N6 C11 1.336(9) . ? N6 C13 1.355(10) . ? N7 C2 1.337(9) . ? N7 C1 1.357(9) . ? N8 C5 1.338(9) . ? N8 C9 1.356(9) . ? C2 C3 1.324(10) . ? C7 C13 1.339(10) . ? C8 C9 1.346(10) . ? C14 C15 1.334(10) . ? N9 C4 1.357(10) . ? N9 C6 1.362(9) . ? N10 C4 1.326(9) . ? N10 C10 1.357(10) . ? C6 C10 1.303(11) . ? 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 O3 Mo1 O4 106.2(2) . . ? O3 Mo1 O1 105.6(2) . . ? O4 Mo1 O1 95.04(18) . . ? O3 Mo1 N3 89.4(2) . . ? O4 Mo1 N3 86.1(2) . . ? O1 Mo1 N3 163.9(2) . . ? O3 Mo1 N2 89.0(2) . . ? O4 Mo1 N2 164.0(2) . . ? O1 Mo1 N2 85.1(2) . . ? N3 Mo1 N2 89.4(2) . . ? O3 Mo1 O5 163.7(2) . . ? O4 Mo1 O5 85.20(18) . . ? O1 Mo1 O5 84.52(19) . . ? N3 Mo1 O5 79.6(2) . . ? N2 Mo1 O5 78.9(2) . . ? O3 Mo1 Mo3 102.68(16) . . ? O4 Mo1 Mo3 48.41(13) . . ? O1 Mo1 Mo3 48.64(13) . . ? N3 Mo1 Mo3 134.53(15) . . ? N2 Mo1 Mo3 133.75(16) . . ? O5 Mo1 Mo3 93.64(12) . . ? O8 Mo2 O6 110.3(3) . . ? O8 Mo2 O2 112.2(2) . . ? O6 Mo2 O2 109.4(2) . . ? O8 Mo2 O5 110.4(2) . . ? O6 Mo2 O5 108.3(2) . . ? O2 Mo2 O5 106.1(2) . . ? O7 Mo3 O4 105.7(2) . . ? O7 Mo3 O1 107.3(2) . . ? O4 Mo3 O1 95.80(19) . . ? O7 Mo3 O2 162.53(19) . . ? O4 Mo3 O2 86.06(19) . . ? O1 Mo3 O2 83.68(18) . . ? O7 Mo3 N4 89.9(2) . . ? O4 Mo3 N4 85.6(2) . . ? O1 Mo3 N4 161.6(2) . . ? O2 Mo3 N4 78.1(2) . . ? O7 Mo3 N1 88.6(2) . . ? O4 Mo3 N1 164.9(2) . . ? O1 Mo3 N1 84.2(2) . . ? O2 Mo3 N1 78.9(2) . . ? N4 Mo3 N1 89.8(2) . . ? O7 Mo3 Mo1 103.71(15) . . ? O4 Mo3 Mo1 48.88(13) . . ? O1 Mo3 Mo1 48.95(13) . . ? O2 Mo3 Mo1 93.75(12) . . ? N4 Mo3 Mo1 134.38(17) . . ? N1 Mo3 Mo1 133.11(16) . . ? Mo3 O1 Mo1 82.41(18) . . ? Mo2 O2 Mo3 121.1(2) . . ? Mo3 O4 Mo1 82.71(17) . . ? Mo2 O5 Mo1 119.9(2) . . ? C12 N1 C14 105.2(7) . . ? C12 N1 Mo3 126.6(6) . . ? C14 N1 Mo3 127.6(5) . . ? C3 N2 C1 105.5(6) . . ? C3 N2 Mo1 129.3(5) . . ? C1 N2 Mo1 124.9(5) . . ? C5 N3 C8 105.7(6) . . ? C5 N3 Mo1 128.5(5) . . ? C8 N3 Mo1 124.8(5) . . ? C11 N4 C7 105.1(6) . . ? C11 N4 Mo3 126.1(5) . . ? C7 N4 Mo3 128.7(5) . . ? C12 N5 C15 107.5(7) . . ? C11 N6 C13 107.0(7) . . ? C2 N7 C1 107.8(6) . . ? C5 N8 C9 107.7(6) . . ? N7 C1 N2 107.7(7) . . ? C3 C2 N7 107.5(7) . . ? N2 C3 C2 111.4(7) . . ? N3 C5 N8 110.7(7) . . ? C13 C7 N4 109.2(7) . . ? C9 C8 N3 109.5(7) . . ? C8 C9 N8 106.5(7) . . ? N4 C11 N6 111.1(7) . . ? N5 C12 N1 111.0(8) . . ? C7 C13 N6 107.5(7) . . ? C15 C14 N1 110.1(8) . . ? C14 C15 N5 106.3(7) . . ? C4 N9 C6 111.2(6) . . ? C4 N10 C10 110.3(7) . . ? N10 C4 N9 103.8(6) . . ? C10 C6 N9 105.5(7) . . ? C6 C10 N10 109.1(7) . . ? _diffrn_measured_fraction_theta_max 0.969 _diffrn_reflns_theta_full 27.25 _diffrn_measured_fraction_theta_full 0.969 _refine_diff_density_max 1.549 _refine_diff_density_min -3.065 _refine_diff_density_rms 0.195 data_sad1 _database_code_depnum_ccdc_archive 'CCDC 890809' #TrackingRef '1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C14 H30 Mo4 N4 Na2 O34' _chemical_formula_weight 1228.16 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' Na Na 0.0362 0.0249 '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 ? _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.6765(2) _cell_length_b 9.5675(3) _cell_length_c 11.8913(4) _cell_angle_alpha 100.703(3) _cell_angle_beta 100.708(2) _cell_angle_gamma 102.734(3) _cell_volume 919.24(5) _cell_formula_units_Z 1 _cell_measurement_temperature 446(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.219 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 604 _exptl_absorpt_coefficient_mu 1.479 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6653 _exptl_absorpt_correction_T_max 0.9297 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 446(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7001 _diffrn_reflns_av_R_equivalents 0.0323 _diffrn_reflns_av_sigmaI/netI 0.0555 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.69 _diffrn_reflns_theta_max 27.00 _reflns_number_total 3919 _reflns_number_gt 3304 _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 ? _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. ; _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^)+(0.0268P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3919 _refine_ls_number_parameters 292 _refine_ls_number_restraints 13 _refine_ls_R_factor_all 0.0450 _refine_ls_R_factor_gt 0.0340 _refine_ls_wR_factor_ref 0.0721 _refine_ls_wR_factor_gt 0.0677 _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_restrained_S_all 1.028 _refine_ls_shift/su_max 0.003 _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 0.63292(4) 2.05469(3) -0.26143(3) 0.00947(9) Uani 1 1 d . . . Mo2 Mo 0.35440(4) 2.04696(3) -0.21688(3) 0.00938(9) Uani 1 1 d . . . Na1 Na -0.17343(18) 1.56890(17) -0.53003(13) 0.0184(4) Uani 1 1 d . . . O1 O 0.4210(3) 2.0131(3) -0.3652(2) 0.0127(6) Uani 1 1 d . . . O2 O 0.5907(3) 1.8124(3) -0.3014(2) 0.0129(6) Uani 1 1 d . . . O3 O 0.1103(3) 1.9944(3) -0.3180(2) 0.0125(6) Uani 1 1 d . . . O4 O 0.5524(3) 2.0293(3) -0.1228(2) 0.0126(6) Uani 1 1 d . . . O5 O 0.8455(3) 2.0119(3) -0.1725(2) 0.0130(6) Uani 1 1 d . . . O6 O 0.9617(3) 1.8424(3) -0.1158(2) 0.0157(6) Uani 1 1 d . . . O7 O 0.6739(3) 1.6325(3) -0.2332(2) 0.0225(7) Uani 1 1 d . . . O8 O 0.2645(3) 1.8072(3) -0.2592(2) 0.0141(6) Uani 1 1 d . . . O9 O -0.1128(3) 1.8154(3) -0.4139(2) 0.0143(6) Uani 1 1 d . . . O10 O 0.0628(3) 1.6143(3) -0.3695(2) 0.0156(6) Uani 1 1 d . . . O11 O 0.7184(3) 2.2367(3) -0.2338(2) 0.0154(6) Uani 1 1 d . . . O12 O 0.3606(3) 2.2276(3) -0.1893(2) 0.0140(6) Uani 1 1 d . . . O1W O 0.7270(3) 2.0148(3) -0.4155(2) 0.0121(6) Uani 1 1 d D . . H1W1 H 0.788(4) 1.957(3) -0.422(3) 0.015 Uiso 1 1 d D . . H1W2 H 0.663(4) 2.005(4) -0.4808(17) 0.015 Uiso 1 1 d D . . O2W O 0.2607(3) 2.0179(3) -0.0670(2) 0.0147(6) Uani 1 1 d D . . H2W1 H 0.324(3) 1.997(4) -0.013(2) 0.018 Uiso 1 1 d D . . H2W2 H 0.1648(17) 1.965(3) -0.078(3) 0.018 Uiso 1 1 d D . . C1 C 0.0302(4) 1.8599(4) -0.3583(3) 0.0120(8) Uani 1 1 d . . . C2 C 0.1243(4) 1.7471(4) -0.3278(3) 0.0117(8) Uani 1 1 d . . . C3 C 0.8474(4) 1.8795(4) -0.1674(3) 0.0124(8) Uani 1 1 d . . . C4 C 0.6898(4) 1.7610(4) -0.2397(3) 0.0138(8) Uani 1 1 d . . . C5 C 0.2342(5) 1.5524(5) -0.1101(4) 0.0261(10) Uani 1 1 d . . . H5A H 0.2729 1.6228 -0.1497 0.031 Uiso 1 1 calc R . . C6 C 0.2926(5) 1.5509(5) 0.0020(4) 0.0253(10) Uani 1 1 d . . . H6A H 0.3803 1.6207 0.0552 0.030 Uiso 1 1 calc R . . C7 C 0.0887(5) 1.3552(5) -0.0725(4) 0.0259(10) Uani 1 1 d . . . H7A H 0.0116 1.2668 -0.0814 0.031 Uiso 1 1 calc R . . N1 N 0.2004(4) 1.4285(4) 0.0239(3) 0.0220(8) Uani 1 1 d . . . H1A H 0.2131 1.4032 0.0901 0.026 Uiso 1 1 calc R . . N2 N 0.1061(4) 1.4297(4) -0.1545(3) 0.0238(8) Uani 1 1 d . . . H2A H 0.0460 1.4048 -0.2250 0.029 Uiso 1 1 calc R . . O3W O -0.3415(3) 1.3550(3) -0.4898(2) 0.0237(7) Uani 1 1 d D . . O4W O 0.0437(3) 1.7028(3) -0.6117(3) 0.0222(7) Uani 1 1 d D . . O5W O -0.4123(4) 1.5953(3) -0.6416(2) 0.0245(7) Uani 1 1 d . . . H3W1 H -0.403(4) 1.364(5) -0.442(2) 0.029 Uiso 1 1 d D . . H3W2 H -0.399(4) 1.306(4) -0.5569(16) 0.029 Uiso 1 1 d D . . H4W1 H 0.069(4) 1.7941(15) -0.608(4) 0.029 Uiso 1 1 d D . . H4W2 H 0.128(3) 1.674(4) -0.594(4) 0.029 Uiso 1 1 d D . . H5W1 H -0.399(5) 1.647(4) -0.684(4) 0.029 Uiso 1 1 d D . . H5W2 H -0.496(5) 1.509(4) -0.687(4) 0.029 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 0.00798(16) 0.01007(18) 0.00913(16) 0.00178(13) 0.00080(13) 0.00132(13) Mo2 0.00767(16) 0.00945(18) 0.00963(16) 0.00187(13) 0.00036(13) 0.00116(13) Na1 0.0137(8) 0.0160(9) 0.0207(8) -0.0003(7) -0.0004(7) 0.0018(6) O1 0.0094(13) 0.0149(14) 0.0138(13) 0.0049(11) 0.0024(11) 0.0019(11) O2 0.0114(13) 0.0114(14) 0.0134(13) 0.0021(11) -0.0013(11) 0.0022(11) O3 0.0094(13) 0.0103(14) 0.0160(13) 0.0022(11) -0.0008(11) 0.0029(11) O4 0.0116(13) 0.0187(15) 0.0080(12) 0.0043(11) 0.0024(10) 0.0036(11) O5 0.0104(13) 0.0107(14) 0.0158(13) 0.0023(11) 0.0011(11) 0.0007(11) O6 0.0098(13) 0.0190(15) 0.0171(14) 0.0063(12) -0.0010(11) 0.0032(11) O7 0.0213(15) 0.0136(15) 0.0255(15) 0.0066(13) -0.0074(13) -0.0005(12) O8 0.0114(13) 0.0118(14) 0.0169(13) 0.0029(11) -0.0002(11) 0.0021(11) O9 0.0097(13) 0.0145(15) 0.0154(13) -0.0002(11) -0.0012(11) 0.0031(11) O10 0.0142(13) 0.0116(14) 0.0176(14) 0.0013(11) -0.0008(12) 0.0018(11) O11 0.0129(13) 0.0145(15) 0.0157(13) 0.0006(11) 0.0028(11) 0.0001(11) O12 0.0145(13) 0.0089(14) 0.0167(13) 0.0015(11) 0.0013(11) 0.0023(11) O1W 0.0137(14) 0.0148(14) 0.0087(12) 0.0033(11) 0.0008(11) 0.0065(11) O2W 0.0095(13) 0.0195(16) 0.0135(13) 0.0059(12) -0.0003(11) 0.0015(12) C1 0.0116(19) 0.017(2) 0.0083(17) 0.0004(15) 0.0044(15) 0.0067(16) C2 0.0082(18) 0.014(2) 0.0123(18) 0.0009(15) 0.0028(15) 0.0034(15) C3 0.0109(18) 0.017(2) 0.0082(17) 0.0011(15) 0.0031(15) 0.0031(16) C4 0.0135(19) 0.015(2) 0.0131(18) 0.0040(16) 0.0058(16) 0.0025(16) C5 0.035(3) 0.019(2) 0.026(2) 0.0111(19) 0.006(2) 0.006(2) C6 0.029(2) 0.017(2) 0.024(2) 0.0036(19) -0.001(2) 0.0017(19) C7 0.022(2) 0.024(2) 0.026(2) 0.004(2) 0.0011(19) 0.0016(19) N1 0.029(2) 0.019(2) 0.0177(17) 0.0081(15) 0.0010(16) 0.0048(16) N2 0.0241(19) 0.028(2) 0.0160(17) 0.0034(16) -0.0018(15) 0.0077(17) O3W 0.0207(15) 0.0275(18) 0.0170(14) 0.0014(13) 0.0035(13) -0.0014(13) O4W 0.0251(16) 0.0159(16) 0.0225(15) 0.0038(13) 0.0050(13) 0.0000(13) O5W 0.0227(16) 0.0207(17) 0.0245(17) 0.0092(13) -0.0030(14) -0.0016(14) _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 O11 1.679(3) . ? Mo1 O1 1.927(2) . ? Mo1 O4 1.941(3) . ? Mo1 O5 2.111(2) . ? Mo1 O1W 2.145(3) . ? Mo1 O2 2.210(2) . ? Mo1 Mo2 2.5568(4) . ? Mo2 O12 1.685(2) . ? Mo2 O4 1.928(2) . ? Mo2 O1 1.948(3) . ? Mo2 O2W 2.130(3) . ? Mo2 O3 2.132(2) . ? Mo2 O8 2.182(3) . ? Na1 O5W 2.336(3) . ? Na1 O9 2.391(3) . ? Na1 O10 2.411(3) 2_584 ? Na1 O3W 2.419(3) . ? Na1 O10 2.425(3) . ? Na1 O4W 2.492(3) . ? Na1 C1 3.070(4) . ? Na1 C2 3.097(4) . ? Na1 Na1 3.550(3) 2_584 ? O2 C4 1.268(4) . ? O3 C1 1.274(4) . ? O5 C3 1.283(4) . ? O6 C3 1.223(4) . ? O7 C4 1.225(4) . ? O8 C2 1.275(4) . ? O9 C1 1.232(4) . ? O10 C2 1.230(4) . ? O10 Na1 2.411(3) 2_584 ? C1 C2 1.545(5) . ? C3 C4 1.553(5) . ? C5 C6 1.339(6) . ? C5 N2 1.367(5) . ? C6 N1 1.363(5) . ? C7 N1 1.317(5) . ? C7 N2 1.321(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O11 Mo1 O1 107.76(11) . . ? O11 Mo1 O4 104.11(12) . . ? O1 Mo1 O4 95.25(10) . . ? O11 Mo1 O5 93.45(11) . . ? O1 Mo1 O5 157.88(10) . . ? O4 Mo1 O5 85.31(10) . . ? O11 Mo1 O1W 91.49(12) . . ? O1 Mo1 O1W 87.70(10) . . ? O4 Mo1 O1W 162.31(10) . . ? O5 Mo1 O1W 85.48(10) . . ? O11 Mo1 O2 163.73(11) . . ? O1 Mo1 O2 84.61(10) . . ? O4 Mo1 O2 84.70(10) . . ? O5 Mo1 O2 73.40(9) . . ? O1W Mo1 O2 78.21(10) . . ? O11 Mo1 Mo2 102.11(9) . . ? O1 Mo1 Mo2 49.08(8) . . ? O4 Mo1 Mo2 48.40(7) . . ? O5 Mo1 Mo2 133.37(7) . . ? O1W Mo1 Mo2 136.76(7) . . ? O2 Mo1 Mo2 93.97(7) . . ? O12 Mo2 O4 106.99(11) . . ? O12 Mo2 O1 103.30(12) . . ? O4 Mo2 O1 94.98(10) . . ? O12 Mo2 O2W 92.40(12) . . ? O4 Mo2 O2W 83.96(10) . . ? O1 Mo2 O2W 163.82(11) . . ? O12 Mo2 O3 90.11(10) . . ? O4 Mo2 O3 161.51(10) . . ? O1 Mo2 O3 87.65(10) . . ? O2W Mo2 O3 88.45(10) . . ? O12 Mo2 O8 161.87(11) . . ? O4 Mo2 O8 88.54(10) . . ? O1 Mo2 O8 84.12(10) . . ? O2W Mo2 O8 79.72(10) . . ? O3 Mo2 O8 73.50(9) . . ? O12 Mo2 Mo1 100.87(9) . . ? O4 Mo2 Mo1 48.84(8) . . ? O1 Mo2 Mo1 48.36(7) . . ? O2W Mo2 Mo1 132.80(7) . . ? O3 Mo2 Mo1 135.96(7) . . ? O8 Mo2 Mo1 96.40(7) . . ? O5W Na1 O9 91.03(11) . . ? O5W Na1 O10 114.12(11) . 2_584 ? O9 Na1 O10 145.15(11) . 2_584 ? O5W Na1 O3W 86.80(11) . . ? O9 Na1 O3W 124.72(12) . . ? O10 Na1 O3W 82.35(11) 2_584 . ? O5W Na1 O10 160.24(12) . . ? O9 Na1 O10 70.22(9) . . ? O10 Na1 O10 85.51(10) 2_584 . ? O3W Na1 O10 98.62(11) . . ? O5W Na1 O4W 103.52(12) . . ? O9 Na1 O4W 77.87(10) . . ? O10 Na1 O4W 73.17(10) 2_584 . ? O3W Na1 O4W 155.51(12) . . ? O10 Na1 O4W 79.22(10) . . ? O5W Na1 C1 111.98(12) . . ? O9 Na1 C1 21.87(8) . . ? O10 Na1 C1 124.77(10) 2_584 . ? O3W Na1 C1 129.07(12) . . ? O10 Na1 C1 50.38(9) . . ? O4W Na1 C1 67.91(10) . . ? O5W Na1 C2 140.86(12) . . ? O9 Na1 C2 49.90(9) . . ? O10 Na1 C2 101.11(10) 2_584 . ? O3W Na1 C2 115.35(11) . . ? O10 Na1 C2 21.67(9) . . ? O4W Na1 C2 70.02(10) . . ? C1 Na1 C2 29.01(9) . . ? O5W Na1 Na1 156.95(11) . 2_584 ? O9 Na1 Na1 109.03(9) . 2_584 ? O10 Na1 Na1 42.91(6) 2_584 2_584 ? O3W Na1 Na1 90.68(9) . 2_584 ? O10 Na1 Na1 42.60(7) . 2_584 ? O4W Na1 Na1 71.07(9) . 2_584 ? C1 Na1 Na1 87.23(8) . 2_584 ? C2 Na1 Na1 59.75(8) . 2_584 ? Mo1 O1 Mo2 82.56(9) . . ? C4 O2 Mo1 117.0(2) . . ? C1 O3 Mo2 119.6(2) . . ? Mo2 O4 Mo1 82.75(9) . . ? C3 O5 Mo1 120.1(2) . . ? C2 O8 Mo2 118.6(2) . . ? C1 O9 Na1 111.8(2) . . ? C2 O10 Na1 129.8(2) . 2_584 ? C2 O10 Na1 111.6(2) . . ? Na1 O10 Na1 94.49(10) 2_584 . ? O9 C1 O3 125.8(3) . . ? O9 C1 C2 119.3(3) . . ? O3 C1 C2 114.8(3) . . ? O9 C1 Na1 46.33(18) . . ? O3 C1 Na1 161.4(3) . . ? C2 C1 Na1 76.47(19) . . ? O10 C2 O8 126.7(3) . . ? O10 C2 C1 120.1(3) . . ? O8 C2 C1 113.1(3) . . ? O10 C2 Na1 46.71(17) . . ? O8 C2 Na1 167.2(3) . . ? C1 C2 Na1 74.52(19) . . ? O6 C3 O5 125.7(3) . . ? O6 C3 C4 120.1(3) . . ? O5 C3 C4 114.1(3) . . ? O7 C4 O2 127.3(3) . . ? O7 C4 C3 119.3(3) . . ? O2 C4 C3 113.4(3) . . ? C6 C5 N2 106.1(4) . . ? C5 C6 N1 107.6(4) . . ? N1 C7 N2 107.7(4) . . ? C7 N1 C6 109.0(4) . . ? C7 N2 C5 109.6(3) . . ? _diffrn_measured_fraction_theta_max 0.975 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.975 _refine_diff_density_max 0.829 _refine_diff_density_min -0.743 _refine_diff_density_rms 0.127 # Attachment '2.cif' data_sad2 _database_code_depnum_ccdc_archive 'CCDC 890810' #TrackingRef '2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C10 H14 K0 Mo2 N4 O14' _chemical_formula_weight 606.13 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' K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.8559(4) _cell_length_b 9.3464(5) _cell_length_c 11.5089(5) _cell_angle_alpha 95.999(4) _cell_angle_beta 96.930(4) _cell_angle_gamma 103.116(5) _cell_volume 912.36(8) _cell_formula_units_Z 2 _cell_measurement_temperature 446(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.206 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 596 _exptl_absorpt_coefficient_mu 1.459 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8678 _exptl_absorpt_correction_T_max 0.8678 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 446(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8976 _diffrn_reflns_av_R_equivalents 0.0388 _diffrn_reflns_av_sigmaI/netI 0.0561 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.77 _diffrn_reflns_theta_max 26.99 _reflns_number_total 3916 _reflns_number_gt 3187 _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 ? _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. ; _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^)+(0.0854P)^2^+0.6106P] 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 3916 _refine_ls_number_parameters 283 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0546 _refine_ls_R_factor_gt 0.0386 _refine_ls_wR_factor_ref 0.1436 _refine_ls_wR_factor_gt 0.1053 _refine_ls_goodness_of_fit_ref 1.097 _refine_ls_restrained_S_all 1.097 _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 0.38274(5) 0.08302(5) 0.78725(4) 0.00858(16) Uani 1 1 d . . . Mo2 Mo 0.65440(5) 0.08536(5) 0.73269(4) 0.00863(16) Uani 1 1 d . . . N1 N 0.3992(6) -0.3953(6) 0.5796(5) 0.0190(11) Uani 1 1 d . . . H1A H 0.4692 -0.3130 0.5985 0.023 Uiso 1 1 calc R . . N2 N 0.2067(6) -0.5661(5) 0.4850(4) 0.0150(10) Uani 1 1 d . . . H2A H 0.1302 -0.6124 0.4312 0.018 Uiso 1 1 calc R . . N3 N 0.0889(8) -0.6032(9) 0.8932(8) 0.057(2) Uani 1 1 d . . . H3A H 0.0102 -0.6708 0.8561 0.068 Uiso 1 1 calc R . . N4 N 0.2797(10) -0.4835(9) 1.0247(6) 0.051(2) Uani 1 1 d . . . H4A H 0.3466 -0.4595 1.0884 0.061 Uiso 1 1 calc R . . O1 O 0.4542(5) 0.0545(5) 0.6345(3) 0.0121(8) Uani 1 1 d . . . O2 O 0.5673(5) 0.0497(5) 0.8768(3) 0.0116(8) Uani 1 1 d . . . O4 O 0.8620(5) 0.0447(4) 0.8234(3) 0.0120(8) Uani 1 1 d . . . O5 O 0.1559(5) 0.0499(5) 0.6870(4) 0.0127(8) Uani 1 1 d . . . O7 O 0.6278(5) -0.1535(5) 0.7026(3) 0.0131(8) Uani 1 1 d . . . O8 O 0.3950(5) 0.2648(5) 0.8138(4) 0.0162(9) Uani 1 1 d . . . O9 O -0.0559(5) -0.1156(5) 0.5913(3) 0.0138(9) Uani 1 1 d . . . O10 O 0.0761(5) -0.3373(5) 0.6668(4) 0.0183(9) Uani 1 1 d . . . O11 O 0.2837(5) -0.1602(5) 0.7528(4) 0.0143(9) Uani 1 1 d . . . O12 O 0.7388(5) 0.2677(5) 0.7503(3) 0.0129(8) Uani 1 1 d . . . O3 O 0.9776(5) -0.1266(5) 0.8899(3) 0.0142(9) Uani 1 1 d . . . O6 O 0.7178(5) -0.3380(5) 0.7729(4) 0.0208(10) Uani 1 1 d . . . C1 C 0.3837(8) -0.5156(7) 0.6414(6) 0.0222(14) Uani 1 1 d . . . H1B H 0.4451 -0.5218 0.7114 0.027 Uiso 1 1 calc R . . C2 C 0.2628(8) -0.6221(7) 0.5812(6) 0.0218(14) Uani 1 1 d . . . H2B H 0.2249 -0.7160 0.6013 0.026 Uiso 1 1 calc R . . C3 C 0.2901(8) -0.4276(7) 0.4880(5) 0.0197(13) Uani 1 1 d . . . H3C H 0.2731 -0.3641 0.4334 0.024 Uiso 1 1 calc R . . C4 C 0.1485(7) -0.2067(7) 0.6918(5) 0.0116(11) Uani 1 1 d . . . C5 C 0.0734(7) -0.0839(6) 0.6510(5) 0.0100(11) Uani 1 1 d . . . C6 C 0.7259(7) -0.2083(6) 0.7655(5) 0.0113(11) Uani 1 1 d . . . C7 C 0.8693(7) -0.0865(7) 0.8329(5) 0.0124(12) Uani 1 1 d . . . C8 C 0.2753(10) -0.4048(9) 0.9333(7) 0.0367(18) Uani 1 1 d . . . H8B H 0.3425 -0.3146 0.9270 0.044 Uiso 1 1 calc R . . C9 C 0.1548(7) -0.4828(7) 0.8537(5) 0.0149(12) Uani 1 1 d U . . H9A H 0.1229 -0.4551 0.7812 0.018 Uiso 1 1 calc R . . C10 C 0.1623(7) -0.6052(7) 0.9994(5) 0.0140(12) Uani 1 1 d . . . H10A H 0.1370 -0.6780 1.0479 0.017 Uiso 1 1 calc R . . O1W O 0.2753(5) 0.0416(5) 0.9424(4) 0.0152(9) Uani 1 1 d D . . O2W O 0.7443(5) 0.0572(5) 0.5676(4) 0.0155(9) Uani 1 1 d D . . H2W2 H 0.676(5) 0.031(7) 0.506(3) 0.019 Uiso 1 1 d D . . H2W1 H 0.812(6) 0.006(6) 0.565(5) 0.023 Uiso 1 1 d D . . H1W1 H 0.183(3) -0.008(7) 0.948(5) 0.019 Uiso 1 1 d D . . H1W2 H 0.338(5) 0.026(7) 1.000(4) 0.023 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 0.0066(3) 0.0106(3) 0.0081(3) 0.00174(19) -0.00047(18) 0.00168(19) Mo2 0.0073(3) 0.0101(3) 0.0078(3) 0.00198(19) -0.00018(18) 0.00099(19) N1 0.020(3) 0.013(3) 0.018(3) 0.000(2) -0.005(2) -0.001(2) N2 0.021(3) 0.012(3) 0.008(2) -0.0002(19) -0.001(2) -0.002(2) N3 0.027(4) 0.046(5) 0.086(6) -0.015(4) -0.008(4) 0.007(3) N4 0.073(6) 0.047(5) 0.030(4) 0.006(3) -0.007(4) 0.014(4) O1 0.011(2) 0.015(2) 0.0103(19) 0.0059(16) 0.0006(15) 0.0014(16) O2 0.013(2) 0.014(2) 0.0085(19) 0.0055(16) 0.0002(15) 0.0026(16) O4 0.012(2) 0.013(2) 0.0101(19) 0.0031(16) -0.0001(16) 0.0020(16) O5 0.009(2) 0.013(2) 0.015(2) 0.0058(17) -0.0015(16) 0.0008(16) O7 0.009(2) 0.014(2) 0.014(2) -0.0004(17) -0.0017(16) 0.0013(16) O8 0.016(2) 0.015(2) 0.017(2) 0.0032(17) 0.0015(17) 0.0030(17) O9 0.009(2) 0.020(2) 0.0106(19) -0.0007(17) -0.0024(16) 0.0017(17) O10 0.015(2) 0.012(2) 0.025(2) 0.0037(18) -0.0049(18) -0.0005(17) O11 0.008(2) 0.018(2) 0.016(2) -0.0009(17) 0.0000(16) 0.0027(17) O12 0.017(2) 0.015(2) 0.0062(18) 0.0023(16) 0.0023(16) 0.0016(17) O3 0.012(2) 0.016(2) 0.014(2) 0.0059(17) -0.0005(16) 0.0036(17) O6 0.024(2) 0.015(2) 0.018(2) 0.0004(18) -0.0085(19) 0.0019(19) C1 0.025(4) 0.015(3) 0.021(3) 0.006(3) -0.006(3) -0.002(3) C2 0.023(3) 0.019(3) 0.019(3) 0.001(3) 0.000(3) -0.001(3) C3 0.022(3) 0.022(3) 0.015(3) 0.007(3) 0.005(3) 0.003(3) C4 0.009(3) 0.018(3) 0.008(3) 0.000(2) 0.005(2) 0.003(2) C5 0.013(3) 0.013(3) 0.005(2) 0.002(2) 0.003(2) 0.003(2) C6 0.010(3) 0.016(3) 0.009(3) 0.005(2) 0.003(2) 0.002(2) C7 0.010(3) 0.019(3) 0.009(3) 0.002(2) 0.003(2) 0.003(2) C8 0.045(5) 0.021(4) 0.041(5) 0.006(3) 0.005(4) 0.001(3) C9 0.0159(15) 0.0153(14) 0.0139(14) 0.0039(9) 0.0014(9) 0.0045(10) C10 0.019(3) 0.018(3) 0.011(3) 0.011(2) 0.005(2) 0.010(2) O1W 0.008(2) 0.023(2) 0.014(2) 0.0027(18) 0.0019(16) 0.0036(18) O2W 0.014(2) 0.020(2) 0.013(2) 0.0010(17) 0.0005(17) 0.0066(18) _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 1.671(4) . ? Mo1 O2 1.929(4) . ? Mo1 O1 1.951(4) . ? Mo1 O5 2.132(4) . ? Mo1 O1W 2.152(4) . ? Mo1 O11 2.218(4) . ? Mo1 Mo2 2.5547(6) . ? Mo2 O12 1.678(4) . ? Mo2 O1 1.928(4) . ? Mo2 O2 1.940(4) . ? Mo2 O4 2.133(4) . ? Mo2 O2W 2.160(4) . ? Mo2 O7 2.177(4) . ? N1 C3 1.300(8) . ? N1 C1 1.382(8) . ? N2 C3 1.332(8) . ? N2 C2 1.361(8) . ? N3 C9 1.299(10) . ? N3 C10 1.317(10) . ? N4 C10 1.334(10) . ? N4 C8 1.347(10) . ? O4 C7 1.258(7) . ? O5 C5 1.293(7) . ? O7 C6 1.292(7) . ? O9 C5 1.219(7) . ? O10 C4 1.229(7) . ? O11 C4 1.270(7) . ? O3 C7 1.246(7) . ? O6 C6 1.210(7) . ? C1 C2 1.345(9) . ? C4 C5 1.537(8) . ? C6 C7 1.560(8) . ? C8 C9 1.335(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 O8 Mo1 O2 106.34(19) . . ? O8 Mo1 O1 104.90(19) . . ? O2 Mo1 O1 94.73(16) . . ? O8 Mo1 O5 90.17(18) . . ? O2 Mo1 O5 162.81(17) . . ? O1 Mo1 O5 85.40(16) . . ? O8 Mo1 O1W 92.09(19) . . ? O2 Mo1 O1W 85.19(16) . . ? O1 Mo1 O1W 162.25(18) . . ? O5 Mo1 O1W 89.50(16) . . ? O8 Mo1 O11 161.04(18) . . ? O2 Mo1 O11 89.10(16) . . ? O1 Mo1 O11 84.23(16) . . ? O5 Mo1 O11 73.79(15) . . ? O1W Mo1 O11 78.02(16) . . ? O8 Mo1 Mo2 100.70(15) . . ? O2 Mo1 Mo2 48.87(12) . . ? O1 Mo1 Mo2 48.43(12) . . ? O5 Mo1 Mo2 133.83(11) . . ? O1W Mo1 Mo2 134.05(11) . . ? O11 Mo1 Mo2 97.76(10) . . ? O12 Mo2 O1 107.21(18) . . ? O12 Mo2 O2 105.55(18) . . ? O1 Mo2 O2 95.12(16) . . ? O12 Mo2 O4 90.40(17) . . ? O1 Mo2 O4 161.51(17) . . ? O2 Mo2 O4 85.25(15) . . ? O12 Mo2 O2W 90.09(17) . . ? O1 Mo2 O2W 84.90(16) . . ? O2 Mo2 O2W 163.53(17) . . ? O4 Mo2 O2W 89.58(15) . . ? O12 Mo2 O7 160.08(18) . . ? O1 Mo2 O7 87.83(16) . . ? O2 Mo2 O7 85.48(16) . . ? O4 Mo2 O7 73.75(15) . . ? O2W Mo2 O7 78.06(16) . . ? O12 Mo2 Mo1 101.88(14) . . ? O1 Mo2 Mo1 49.20(12) . . ? O2 Mo2 Mo1 48.49(12) . . ? O4 Mo2 Mo1 133.73(11) . . ? O2W Mo2 Mo1 134.10(11) . . ? O7 Mo2 Mo1 97.83(11) . . ? C3 N1 C1 108.5(5) . . ? C3 N2 C2 108.6(5) . . ? C9 N3 C10 109.0(7) . . ? C10 N4 C8 108.3(7) . . ? Mo2 O1 Mo1 82.37(15) . . ? Mo1 O2 Mo2 82.64(15) . . ? C7 O4 Mo2 119.5(4) . . ? C5 O5 Mo1 119.2(3) . . ? C6 O7 Mo2 117.7(4) . . ? C4 O11 Mo1 117.4(4) . . ? C2 C1 N1 106.9(6) . . ? C1 C2 N2 106.9(6) . . ? N1 C3 N2 109.0(6) . . ? O10 C4 O11 125.5(5) . . ? O10 C4 C5 119.9(5) . . ? O11 C4 C5 114.6(5) . . ? O9 C5 O5 124.7(5) . . ? O9 C5 C4 120.3(5) . . ? O5 C5 C4 115.0(5) . . ? O6 C6 O7 127.2(5) . . ? O6 C6 C7 120.4(5) . . ? O7 C6 C7 112.4(5) . . ? O3 C7 O4 126.7(6) . . ? O3 C7 C6 118.3(5) . . ? O4 C7 C6 115.0(5) . . ? C9 C8 N4 105.8(7) . . ? N3 C9 C8 109.5(6) . . ? N3 C10 N4 107.4(6) . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 26.99 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 1.248 _refine_diff_density_min -1.204 _refine_diff_density_rms 0.229 # Attachment '3.cif' data_sad3 _database_code_depnum_ccdc_archive 'CCDC 891643' #TrackingRef '3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'Sodium oxalato imidazole molybdate(V)' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C20 H34 Mo4 N8 Na4 O33' _chemical_formula_weight 1390.27 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' Na Na 0.0362 0.0249 '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 ? _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 27.7825(15) _cell_length_b 10.1376(4) _cell_length_c 18.3598(10) _cell_angle_alpha 90.00 _cell_angle_beta 121.619(7) _cell_angle_gamma 90.00 _cell_volume 4403.4(4) _cell_formula_units_Z 4 _cell_measurement_temperature 446(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.097 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2744 _exptl_absorpt_coefficient_mu 1.267 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7424 _exptl_absorpt_correction_T_max 0.8327 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 446(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11203 _diffrn_reflns_av_R_equivalents 0.0392 _diffrn_reflns_av_sigmaI/netI 0.0555 _diffrn_reflns_limit_h_min -34 _diffrn_reflns_limit_h_max 35 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.98 _diffrn_reflns_theta_max 27.00 _reflns_number_total 4713 _reflns_number_gt 3980 _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 ? _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. ; _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^)+(0.0292P)^2^+9.9158P] 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 4713 _refine_ls_number_parameters 345 _refine_ls_number_restraints 15 _refine_ls_R_factor_all 0.0469 _refine_ls_R_factor_gt 0.0359 _refine_ls_wR_factor_ref 0.0795 _refine_ls_wR_factor_gt 0.0745 _refine_ls_goodness_of_fit_ref 1.018 _refine_ls_restrained_S_all 1.318 _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 0.136100(17) 0.07693(4) 0.23059(2) 0.01247(12) Uani 1 1 d . . . Mo2 Mo 0.139580(17) 0.30753(4) 0.28997(2) 0.01324(12) Uani 1 1 d . . . Na1 Na -0.02460(9) -0.3734(2) 0.03924(12) 0.0190(4) Uani 1 1 d . . . Na2 Na 0.0000 -0.3615(3) 0.2500 0.0189(6) Uani 1 2 d S . . Na3 Na 0.0000 0.0000 0.0000 0.0231(7) Uani 1 2 d S . . O1 O 0.19633(14) 0.1723(3) 0.3249(2) 0.0159(7) Uani 1 1 d . . . O2 O 0.07661(14) 0.1862(3) 0.2258(2) 0.0150(7) Uani 1 1 d . . . O3 O 0.08837(16) -0.2310(4) 0.3337(2) 0.0246(8) Uani 1 1 d . . . O4 O 0.13517(14) 0.2384(3) 0.4013(2) 0.0172(7) Uani 1 1 d . . . O5 O 0.08262(15) 0.4339(3) 0.3004(2) 0.0182(8) Uani 1 1 d . . . O6 O 0.13784(15) 0.1136(3) 0.1429(2) 0.0184(8) Uani 1 1 d . . . O7 O 0.07174(14) -0.0655(3) 0.1558(2) 0.0157(7) Uani 1 1 d . . . O8 O 0.02311(15) -0.2385(4) 0.1586(2) 0.0213(8) Uani 1 1 d . . . O9 O 0.12581(14) -0.0435(3) 0.3216(2) 0.0156(7) Uani 1 1 d . . . O10 O 0.04219(15) 0.4912(3) 0.3732(2) 0.0214(8) Uani 1 1 d . . . O11 O 0.14107(15) 0.4040(3) 0.2164(2) 0.0207(8) Uani 1 1 d . . . O12 O 0.10135(16) 0.2799(3) 0.4847(2) 0.0225(8) Uani 1 1 d . . . N1 N 0.20711(18) 0.4231(4) 0.3935(3) 0.0189(9) Uani 1 1 d . . . N2 N 0.28945(19) 0.4727(5) 0.5034(3) 0.0271(11) Uani 1 1 d . . . H2A H 0.3243 0.4654 0.5435 0.033 Uiso 1 1 calc R . . N3 N 0.19981(18) -0.0774(4) 0.2670(3) 0.0191(9) Uani 1 1 d . . . N4 N 0.2767(2) -0.1916(5) 0.3485(3) 0.0297(11) Uani 1 1 d . . . H4A H 0.3102 -0.2116 0.3894 0.036 Uiso 1 1 calc R . . C1 C 0.0738(2) 0.4207(5) 0.3619(3) 0.0174(11) Uani 1 1 d . . . C2 C 0.1056(2) 0.3043(5) 0.4224(3) 0.0162(10) Uani 1 1 d . . . C3 C 0.2592(2) 0.3813(6) 0.4474(3) 0.0278(13) Uani 1 1 d . . . H3A H 0.2726 0.2980 0.4457 0.033 Uiso 1 1 calc R . . C4 C 0.2058(3) 0.5500(6) 0.4191(4) 0.0327(14) Uani 1 1 d . . . H4B H 0.1747 0.6062 0.3936 0.039 Uiso 1 1 calc R . . C5 C 0.2571(3) 0.5789(6) 0.4876(4) 0.0386(15) Uani 1 1 d . . . H5A H 0.2678 0.6578 0.5180 0.046 Uiso 1 1 calc R . . C6 C 0.0589(2) -0.1538(5) 0.1938(3) 0.0151(10) Uani 1 1 d . . . C7 C 0.0939(2) -0.1435(5) 0.2926(3) 0.0162(10) Uani 1 1 d . . . C9 C 0.2512(2) -0.0751(6) 0.3367(4) 0.0257(12) Uani 1 1 d . . . H9A H 0.2672 -0.0024 0.3725 0.031 Uiso 1 1 calc R . . C10 C 0.2402(3) -0.2728(7) 0.2845(4) 0.0411(16) Uani 1 1 d . . . H10A H 0.2465 -0.3605 0.2770 0.049 Uiso 1 1 calc R . . C11 C 0.1930(3) -0.2013(6) 0.2335(4) 0.0369(15) Uani 1 1 d . . . H11B H 0.1610 -0.2316 0.1838 0.044 Uiso 1 1 calc R . . O1W O -0.06828(17) -0.0011(4) 0.0448(3) 0.0294(9) Uani 1 1 d D . . O2W O -0.11494(16) -0.2668(4) -0.0004(2) 0.0243(8) Uani 1 1 d D . . O3W O -0.06519(15) -0.5421(4) -0.0659(2) 0.0192(8) Uani 1 1 d D . . O4W O -0.01046(16) -0.2269(4) -0.0485(2) 0.0203(8) Uani 1 1 d D . . O5W O 0.0000 0.0505(7) 0.2500 0.097(4) Uani 1 2 d SD . . H1W1 H -0.083(3) 0.075(4) 0.035(6) 0.116 Uiso 1 1 d D . . H1W2 H -0.092(3) -0.057(6) 0.010(5) 0.116 Uiso 1 1 d D . . H2W1 H -0.131(3) -0.291(9) 0.026(4) 0.116 Uiso 1 1 d D . . H3W1 H -0.084(3) -0.592(8) -0.053(5) 0.116 Uiso 1 1 d D . . H3W2 H -0.087(3) -0.512(9) -0.116(3) 0.116 Uiso 1 1 d D . . H4W1 H 0.0217(17) -0.251(10) -0.038(5) 0.116 Uiso 1 1 d D . . H4W2 H -0.033(3) -0.220(10) -0.1021(13) 0.116 Uiso 1 1 d D . . H5W1 H -0.025(7) 0.107(18) 0.220(12) 0.116 Uiso 0.50 1 d PD . . H5W2 H 0.032(4) 0.078(18) 0.259(13) 0.116 Uiso 0.50 1 d PD . . H2W2 H -0.103(3) -0.246(7) 0.0517(17) 0.05(2) 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 0.0117(2) 0.0144(2) 0.0102(2) 0.00010(17) 0.00494(17) -0.00054(17) Mo2 0.0127(2) 0.0137(2) 0.0114(2) 0.00079(17) 0.00501(17) 0.00063(17) Na1 0.0234(11) 0.0181(11) 0.0166(10) -0.0029(8) 0.0113(9) -0.0056(9) Na2 0.0241(16) 0.0171(15) 0.0153(13) 0.000 0.0101(12) 0.000 Na3 0.0260(16) 0.0221(17) 0.0218(15) -0.0004(13) 0.0129(13) 0.0002(13) O1 0.0130(17) 0.0153(18) 0.0171(16) -0.0012(15) 0.0063(14) 0.0013(15) O2 0.0124(17) 0.0159(18) 0.0152(16) 0.0000(14) 0.0062(14) 0.0002(15) O3 0.031(2) 0.023(2) 0.0150(17) 0.0035(16) 0.0091(16) -0.0055(18) O4 0.0192(19) 0.0151(18) 0.0169(17) 0.0033(15) 0.0091(15) 0.0053(15) O5 0.0207(19) 0.0171(19) 0.0167(17) 0.0026(15) 0.0097(15) 0.0048(16) O6 0.0192(19) 0.021(2) 0.0145(17) 0.0008(15) 0.0084(15) -0.0018(16) O7 0.0167(18) 0.0179(19) 0.0115(16) -0.0007(14) 0.0067(14) -0.0031(15) O8 0.025(2) 0.020(2) 0.0175(17) -0.0052(16) 0.0104(16) -0.0102(17) O9 0.0154(17) 0.0181(19) 0.0109(15) -0.0025(14) 0.0052(14) -0.0048(15) O10 0.027(2) 0.017(2) 0.0234(19) 0.0007(16) 0.0153(17) 0.0093(17) O11 0.023(2) 0.023(2) 0.0160(18) 0.0041(15) 0.0096(16) 0.0010(16) O12 0.032(2) 0.021(2) 0.0202(18) 0.0042(16) 0.0170(17) 0.0072(17) N1 0.017(2) 0.019(2) 0.017(2) -0.0006(18) 0.0062(18) 0.0003(19) N2 0.019(2) 0.029(3) 0.020(2) -0.001(2) 0.0015(19) 0.000(2) N3 0.017(2) 0.020(2) 0.020(2) -0.0016(19) 0.0091(18) 0.0028(19) N4 0.022(3) 0.035(3) 0.032(3) 0.006(2) 0.015(2) 0.007(2) C1 0.019(3) 0.015(3) 0.014(2) -0.002(2) 0.006(2) -0.002(2) C2 0.017(3) 0.014(3) 0.017(2) -0.004(2) 0.009(2) 0.000(2) C3 0.019(3) 0.024(3) 0.027(3) -0.008(2) 0.003(2) 0.000(2) C4 0.024(3) 0.021(3) 0.036(3) -0.002(3) 0.005(3) 0.005(3) C5 0.039(4) 0.020(3) 0.039(4) -0.006(3) 0.009(3) 0.003(3) C6 0.015(2) 0.016(3) 0.015(2) -0.003(2) 0.008(2) 0.000(2) C7 0.012(2) 0.021(3) 0.013(2) 0.001(2) 0.005(2) 0.001(2) C9 0.025(3) 0.024(3) 0.027(3) 0.001(2) 0.013(2) 0.006(3) C10 0.036(4) 0.030(4) 0.059(4) -0.011(3) 0.026(3) 0.008(3) C11 0.022(3) 0.034(4) 0.044(4) -0.022(3) 0.010(3) 0.001(3) O1W 0.033(2) 0.020(2) 0.039(2) -0.0041(19) 0.022(2) -0.0059(19) O2W 0.023(2) 0.033(2) 0.0165(18) -0.0006(17) 0.0101(16) -0.0051(18) O3W 0.022(2) 0.0161(19) 0.0160(17) 0.0018(15) 0.0080(15) -0.0001(16) O4W 0.0202(19) 0.022(2) 0.0168(17) 0.0024(16) 0.0086(15) 0.0003(17) O5W 0.082(7) 0.018(4) 0.257(14) 0.000 0.135(9) 0.000 _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 O6 1.678(3) . ? Mo1 O1 1.922(3) . ? Mo1 O2 1.953(3) . ? Mo1 O7 2.143(3) . ? Mo1 N3 2.188(4) . ? Mo1 O9 2.207(3) . ? Mo1 Mo2 2.5598(6) . ? Mo2 O11 1.685(3) . ? Mo2 O1 1.928(3) . ? Mo2 O2 1.950(3) . ? Mo2 O5 2.121(3) . ? Mo2 N1 2.183(4) . ? Mo2 O4 2.225(3) . ? Na1 O8 2.321(4) . ? Na1 O10 2.352(4) 2_545 ? Na1 O4W 2.371(4) . ? Na1 O3W 2.375(4) . ? Na1 O3W 2.432(4) 5_545 ? Na1 O2W 2.466(4) . ? Na1 Na1 3.550(4) 5_545 ? Na1 Na2 3.5611(18) . ? Na1 Na3 3.979(2) . ? Na2 O8 2.431(4) 2 ? Na2 O8 2.431(4) . ? Na2 O10 2.437(4) 1_545 ? Na2 O10 2.437(4) 2_545 ? Na2 O3 2.487(4) . ? Na2 O3 2.487(4) 2 ? Na2 O5 2.864(4) 2_545 ? Na2 O5 2.864(4) 1_545 ? Na2 C1 2.980(5) 2_545 ? Na2 C1 2.980(5) 1_545 ? Na2 Na1 3.5611(18) 2 ? Na3 O4W 2.428(4) 5 ? Na3 O4W 2.428(4) . ? Na3 O1W 2.431(4) . ? Na3 O1W 2.431(4) 5 ? Na3 O7 2.573(3) . ? Na3 O7 2.573(3) 5 ? Na3 Na1 3.979(2) 5 ? O3 C7 1.226(6) . ? O4 C2 1.267(5) . ? O5 C1 1.282(5) . ? O5 Na2 2.864(4) 1_565 ? O7 C6 1.294(6) . ? O8 C6 1.213(6) . ? O9 C7 1.265(6) . ? O10 C1 1.231(6) . ? O10 Na1 2.352(4) 2_565 ? O10 Na2 2.437(4) 1_565 ? O12 C2 1.234(5) . ? N1 C3 1.324(7) . ? N1 C4 1.377(7) . ? N2 C3 1.309(7) . ? N2 C5 1.334(7) . ? N3 C9 1.326(7) . ? N3 C11 1.367(7) . ? N4 C9 1.336(7) . ? N4 C10 1.355(8) . ? C1 C2 1.542(7) . ? C1 Na2 2.980(5) 1_565 ? C4 C5 1.349(9) . ? C6 C7 1.548(6) . ? C10 C11 1.355(9) . ? O3W Na1 2.432(4) 5_545 ? 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 O6 Mo1 O1 107.69(15) . . ? O6 Mo1 O2 106.29(15) . . ? O1 Mo1 O2 94.12(14) . . ? O6 Mo1 O7 88.19(14) . . ? O1 Mo1 O7 162.91(13) . . ? O2 Mo1 O7 87.19(13) . . ? O6 Mo1 N3 91.47(16) . . ? O1 Mo1 N3 84.37(15) . . ? O2 Mo1 N3 161.70(14) . . ? O7 Mo1 N3 89.05(15) . . ? O6 Mo1 O9 158.43(15) . . ? O1 Mo1 O9 89.62(13) . . ? O2 Mo1 O9 84.58(13) . . ? O7 Mo1 O9 73.53(12) . . ? N3 Mo1 O9 77.18(14) . . ? O6 Mo1 Mo2 101.13(12) . . ? O1 Mo1 Mo2 48.41(10) . . ? O2 Mo1 Mo2 48.95(10) . . ? O7 Mo1 Mo2 136.11(9) . . ? N3 Mo1 Mo2 132.78(11) . . ? O9 Mo1 Mo2 100.01(9) . . ? O11 Mo2 O1 108.66(15) . . ? O11 Mo2 O2 105.84(15) . . ? O1 Mo2 O2 94.06(14) . . ? O11 Mo2 O5 93.14(15) . . ? O1 Mo2 O5 156.65(13) . . ? O2 Mo2 O5 87.71(13) . . ? O11 Mo2 N1 90.88(16) . . ? O1 Mo2 N1 84.97(15) . . ? O2 Mo2 N1 162.58(14) . . ? O5 Mo2 N1 86.48(14) . . ? O11 Mo2 O4 162.83(15) . . ? O1 Mo2 O4 84.25(12) . . ? O2 Mo2 O4 83.84(13) . . ? O5 Mo2 O4 72.78(12) . . ? N1 Mo2 O4 78.75(14) . . ? O11 Mo2 Mo1 101.55(12) . . ? O1 Mo2 Mo1 48.24(10) . . ? O2 Mo2 Mo1 49.06(9) . . ? O5 Mo2 Mo1 136.60(10) . . ? N1 Mo2 Mo1 133.18(11) . . ? O4 Mo2 Mo1 95.50(9) . . ? O8 Na1 O10 85.35(13) . 2_545 ? O8 Na1 O4W 93.25(14) . . ? O10 Na1 O4W 176.48(16) 2_545 . ? O8 Na1 O3W 169.98(16) . . ? O10 Na1 O3W 87.41(13) 2_545 . ? O4W Na1 O3W 94.36(13) . . ? O8 Na1 O3W 89.98(14) . 5_545 ? O10 Na1 O3W 102.44(14) 2_545 5_545 ? O4W Na1 O3W 80.77(13) . 5_545 ? O3W Na1 O3W 84.82(14) . 5_545 ? O8 Na1 O2W 90.54(14) . . ? O10 Na1 O2W 85.03(14) 2_545 . ? O4W Na1 O2W 91.76(14) . . ? O3W Na1 O2W 95.73(14) . . ? O3W Na1 O2W 172.53(14) 5_545 . ? O8 Na1 Na1 131.21(14) . 5_545 ? O10 Na1 Na1 96.74(12) 2_545 5_545 ? O4W Na1 Na1 86.62(11) . 5_545 ? O3W Na1 Na1 43.03(10) . 5_545 ? O3W Na1 Na1 41.79(9) 5_545 5_545 ? O2W Na1 Na1 138.26(14) . 5_545 ? O8 Na1 Na2 42.65(9) . . ? O10 Na1 Na2 42.89(10) 2_545 . ? O4W Na1 Na2 135.36(12) . . ? O3W Na1 Na2 130.27(11) . . ? O3W Na1 Na2 101.58(10) 5_545 . ? O2W Na1 Na2 83.77(9) . . ? Na1 Na1 Na2 124.76(10) 5_545 . ? O8 Na1 Na3 62.82(9) . . ? O10 Na1 Na3 142.77(11) 2_545 . ? O4W Na1 Na3 34.46(9) . . ? O3W Na1 Na3 126.25(10) . . ? O3W Na1 Na3 96.67(10) 5_545 . ? O2W Na1 Na3 76.98(10) . . ? Na1 Na1 Na3 118.38(7) 5_545 . ? Na2 Na1 Na3 102.20(6) . . ? O8 Na2 O8 118.3(2) 2 . ? O8 Na2 O10 81.16(11) 2 1_545 ? O8 Na2 O10 141.46(12) . 1_545 ? O8 Na2 O10 141.46(12) 2 2_545 ? O8 Na2 O10 81.16(11) . 2_545 ? O10 Na2 O10 104.44(19) 1_545 2_545 ? O8 Na2 O3 80.39(13) 2 . ? O8 Na2 O3 67.73(12) . . ? O10 Na2 O3 85.06(12) 1_545 . ? O10 Na2 O3 137.56(11) 2_545 . ? O8 Na2 O3 67.73(12) 2 2 ? O8 Na2 O3 80.39(13) . 2 ? O10 Na2 O3 137.56(11) 1_545 2 ? O10 Na2 O3 85.06(12) 2_545 2 ? O3 Na2 O3 115.7(2) . 2 ? O8 Na2 O5 97.91(11) 2 2_545 ? O8 Na2 O5 127.26(11) . 2_545 ? O10 Na2 O5 76.71(13) 1_545 2_545 ? O10 Na2 O5 48.88(10) 2_545 2_545 ? O3 Na2 O5 161.72(13) . 2_545 ? O3 Na2 O5 79.70(11) 2 2_545 ? O8 Na2 O5 127.26(11) 2 1_545 ? O8 Na2 O5 97.91(11) . 1_545 ? O10 Na2 O5 48.88(10) 1_545 1_545 ? O10 Na2 O5 76.71(13) 2_545 1_545 ? O3 Na2 O5 79.70(11) . 1_545 ? O3 Na2 O5 161.72(13) 2 1_545 ? O5 Na2 O5 87.17(16) 2_545 1_545 ? O8 Na2 C1 121.37(13) 2 2_545 ? O8 Na2 C1 103.86(12) . 2_545 ? O10 Na2 C1 90.47(15) 1_545 2_545 ? O10 Na2 C1 23.66(12) 2_545 2_545 ? O3 Na2 C1 156.87(14) . 2_545 ? O3 Na2 C1 82.46(13) 2 2_545 ? O5 Na2 C1 25.24(11) 2_545 2_545 ? O5 Na2 C1 80.29(14) 1_545 2_545 ? O8 Na2 C1 103.86(12) 2 1_545 ? O8 Na2 C1 121.37(13) . 1_545 ? O10 Na2 C1 23.66(12) 1_545 1_545 ? O10 Na2 C1 90.47(15) 2_545 1_545 ? O3 Na2 C1 82.46(13) . 1_545 ? O3 Na2 C1 156.87(14) 2 1_545 ? O5 Na2 C1 80.29(14) 2_545 1_545 ? O5 Na2 C1 25.24(11) 1_545 1_545 ? C1 Na2 C1 84.4(2) 2_545 1_545 ? O8 Na2 Na1 40.30(9) 2 2 ? O8 Na2 Na1 142.88(12) . 2 ? O10 Na2 Na1 41.05(8) 1_545 2 ? O10 Na2 Na1 135.46(12) 2_545 2 ? O3 Na2 Na1 77.39(8) . 2 ? O3 Na2 Na1 104.73(9) 2 2 ? O5 Na2 Na1 89.51(8) 2_545 2 ? O5 Na2 Na1 87.69(8) 1_545 2 ? C1 Na2 Na1 113.25(11) 2_545 2 ? C1 Na2 Na1 63.59(10) 1_545 2 ? O8 Na2 Na1 142.88(12) 2 . ? O8 Na2 Na1 40.30(9) . . ? O10 Na2 Na1 135.46(12) 1_545 . ? O10 Na2 Na1 41.05(8) 2_545 . ? O3 Na2 Na1 104.73(9) . . ? O3 Na2 Na1 77.39(8) 2 . ? O5 Na2 Na1 87.69(8) 2_545 . ? O5 Na2 Na1 89.51(8) 1_545 . ? C1 Na2 Na1 63.59(10) 2_545 . ? C1 Na2 Na1 113.25(11) 1_545 . ? Na1 Na2 Na1 176.13(11) 2 . ? O4W Na3 O4W 180.00(18) 5 . ? O4W Na3 O1W 81.08(12) 5 . ? O4W Na3 O1W 98.92(12) . . ? O4W Na3 O1W 98.92(12) 5 5 ? O4W Na3 O1W 81.08(12) . 5 ? O1W Na3 O1W 180.00(13) . 5 ? O4W Na3 O7 87.86(11) 5 . ? O4W Na3 O7 92.14(11) . . ? O1W Na3 O7 84.83(12) . . ? O1W Na3 O7 95.17(12) 5 . ? O4W Na3 O7 92.14(11) 5 5 ? O4W Na3 O7 87.86(11) . 5 ? O1W Na3 O7 95.17(12) . 5 ? O1W Na3 O7 84.83(12) 5 5 ? O7 Na3 O7 180.00(18) . 5 ? O4W Na3 Na1 146.47(8) 5 . ? O4W Na3 Na1 33.53(8) . . ? O1W Na3 Na1 72.29(9) . . ? O1W Na3 Na1 107.71(9) 5 . ? O7 Na3 Na1 70.10(8) . . ? O7 Na3 Na1 109.90(8) 5 . ? O4W Na3 Na1 33.53(8) 5 5 ? O4W Na3 Na1 146.47(8) . 5 ? O1W Na3 Na1 107.71(9) . 5 ? O1W Na3 Na1 72.29(9) 5 5 ? O7 Na3 Na1 109.90(8) . 5 ? O7 Na3 Na1 70.10(8) 5 5 ? Na1 Na3 Na1 180.00(7) . 5 ? Mo1 O1 Mo2 83.34(13) . . ? Mo2 O2 Mo1 81.99(12) . . ? C7 O3 Na2 114.0(3) . . ? C2 O4 Mo2 118.1(3) . . ? C1 O5 Mo2 120.9(3) . . ? C1 O5 Na2 82.5(3) . 1_565 ? Mo2 O5 Na2 156.59(14) . 1_565 ? C6 O7 Mo1 119.5(3) . . ? C6 O7 Na3 120.4(3) . . ? Mo1 O7 Na3 115.99(13) . . ? C6 O8 Na1 145.4(3) . . ? C6 O8 Na2 115.8(3) . . ? Na1 O8 Na2 97.05(14) . . ? C7 O9 Mo1 117.7(3) . . ? C1 O10 Na1 151.2(3) . 2_565 ? C1 O10 Na2 103.7(3) . 1_565 ? Na1 O10 Na2 96.05(13) 2_565 1_565 ? C3 N1 C4 105.0(5) . . ? C3 N1 Mo2 125.6(4) . . ? C4 N1 Mo2 129.3(4) . . ? C3 N2 C5 108.6(5) . . ? C9 N3 C11 106.0(5) . . ? C9 N3 Mo1 124.8(4) . . ? C11 N3 Mo1 128.3(4) . . ? C9 N4 C10 107.7(5) . . ? O10 C1 O5 124.8(5) . . ? O10 C1 C2 120.8(4) . . ? O5 C1 C2 114.3(4) . . ? O10 C1 Na2 52.6(3) . 1_565 ? O5 C1 Na2 72.3(3) . 1_565 ? C2 C1 Na2 172.2(3) . 1_565 ? O12 C2 O4 124.7(5) . . ? O12 C2 C1 121.6(4) . . ? O4 C2 C1 113.7(4) . . ? N2 C3 N1 111.1(5) . . ? C5 C4 N1 108.5(5) . . ? N2 C5 C4 106.8(5) . . ? O8 C6 O7 125.7(4) . . ? O8 C6 C7 120.5(4) . . ? O7 C6 C7 113.8(4) . . ? O3 C7 O9 127.4(4) . . ? O3 C7 C6 117.9(4) . . ? O9 C7 C6 114.7(4) . . ? N3 C9 N4 110.6(5) . . ? N4 C10 C11 106.7(5) . . ? C10 C11 N3 108.9(5) . . ? Na1 O3W Na1 95.18(14) . 5_545 ? Na1 O4W Na3 112.01(14) . . ? _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 0.697 _refine_diff_density_min -0.761 _refine_diff_density_rms 0.123 # Attachment '4.cif' data_sad4 _database_code_depnum_ccdc_archive 'CCDC 891644' #TrackingRef '4.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'Potassium oxalato imidazole molybdate(V)' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C10 H14 K2 Mo2 N4 O15' _chemical_formula_weight 700.33 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' K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 8.6355(2) _cell_length_b 29.6451(9) _cell_length_c 8.8144(3) _cell_angle_alpha 90.00 _cell_angle_beta 107.402(3) _cell_angle_gamma 90.00 _cell_volume 2153.21(11) _cell_formula_units_Z 4 _cell_measurement_temperature 446(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.160 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1376 _exptl_absorpt_coefficient_mu 1.633 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8537 _exptl_absorpt_correction_T_max 0.8537 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 446(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10909 _diffrn_reflns_av_R_equivalents 0.0395 _diffrn_reflns_av_sigmaI/netI 0.0553 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 37 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.75 _diffrn_reflns_theta_max 26.99 _reflns_number_total 4622 _reflns_number_gt 3908 _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 ? _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. ; _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^)+(0.0241P)^2^+1.1688P] 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 4622 _refine_ls_number_parameters 316 _refine_ls_number_restraints 9 _refine_ls_R_factor_all 0.0500 _refine_ls_R_factor_gt 0.0381 _refine_ls_wR_factor_ref 0.0745 _refine_ls_wR_factor_gt 0.0706 _refine_ls_goodness_of_fit_ref 1.067 _refine_ls_restrained_S_all 1.067 _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 1.44298(4) 0.151377(11) 0.63468(4) 0.01239(9) Uani 1 1 d . . . Mo2 Mo 1.21632(4) 0.167584(11) 0.37931(4) 0.01391(9) Uani 1 1 d . . . N1 N 1.7075(4) 0.14894(11) 0.6936(4) 0.0178(7) Uani 1 1 d . . . N2 N 1.9499(4) 0.14486(12) 0.6677(4) 0.0245(8) Uani 1 1 d . . . H2A H 2.0280 0.1466 0.6261 0.029 Uiso 1 1 calc R . . N3 N 1.2015(4) 0.19403(11) 0.1439(4) 0.0216(8) Uani 1 1 d . . . N4 N 1.2603(6) 0.21853(13) -0.0640(4) 0.0368(10) Uani 1 1 d . . . H4A H 1.3122 0.2226 -0.1323 0.044 Uiso 1 1 calc R . . C1 C 1.7948(5) 0.15507(14) 0.5956(5) 0.0218(9) Uani 1 1 d . . . H1A H 1.7542 0.1651 0.4912 0.026 Uiso 1 1 calc R . . C2 C 1.9628(6) 0.13129(17) 0.8176(5) 0.0319(11) Uani 1 1 d . . . H2B H 2.0567 0.1219 0.8944 0.038 Uiso 1 1 calc R . . C3 C 1.8137(5) 0.13407(17) 0.8336(5) 0.0302(11) Uani 1 1 d . . . H3A H 1.7864 0.1270 0.9252 0.036 Uiso 1 1 calc R . . C4 C 1.0794(6) 0.22219(15) 0.0589(5) 0.0306(11) Uani 1 1 d . . . H4B H 0.9866 0.2295 0.0864 0.037 Uiso 1 1 calc R . . C5 C 1.3094(6) 0.19253(16) 0.0651(5) 0.0292(11) Uani 1 1 d . . . H5A H 1.4050 0.1759 0.0950 0.035 Uiso 1 1 calc R . . C6 C 1.1158(7) 0.23738(16) -0.0702(5) 0.0379(13) Uani 1 1 d . . . H6A H 1.0543 0.2568 -0.1478 0.045 Uiso 1 1 calc R . . C7 C 0.9419(5) 0.10531(14) 0.2371(4) 0.0166(9) Uani 1 1 d . . . C8 C 1.0881(5) 0.08124(13) 0.2016(4) 0.0151(8) Uani 1 1 d . . . C9 C 1.5249(5) 0.05421(13) 0.7213(4) 0.0140(8) Uani 1 1 d . . . C10 C 1.4877(5) 0.07613(13) 0.8667(4) 0.0145(8) Uani 1 1 d . . . O1 O 1.2189(3) 0.13109(9) 0.5640(3) 0.0157(6) Uani 1 1 d . . . O2 O 1.4484(3) 0.16421(8) 0.4206(3) 0.0150(6) Uani 1 1 d . . . O3 O 1.4468(3) 0.20103(9) 0.7279(3) 0.0195(6) Uani 1 1 d . . . O4 O 1.1640(3) 0.21944(9) 0.4240(3) 0.0207(6) Uani 1 1 d . . . O5 O 1.4591(3) 0.11818(9) 0.8516(3) 0.0170(6) Uani 1 1 d . . . O6 O 1.4943(3) 0.07955(9) 0.5997(3) 0.0143(6) Uani 1 1 d . . . O7 O 1.5818(4) 0.01568(9) 0.7319(3) 0.0208(6) Uani 1 1 d . . . O8 O 1.4901(3) 0.05330(9) 0.9836(3) 0.0188(6) Uani 1 1 d . . . O9 O 0.9717(3) 0.14569(9) 0.2917(3) 0.0183(6) Uani 1 1 d . . . O10 O 1.2205(3) 0.10309(9) 0.2524(3) 0.0176(6) Uani 1 1 d . . . O11 O 0.8107(3) 0.08635(10) 0.2084(3) 0.0252(7) Uani 1 1 d . . . O12 O 1.0660(4) 0.04591(10) 0.1283(3) 0.0268(7) Uani 1 1 d . . . K1 K 1.53689(11) 0.07273(3) 1.30177(10) 0.0189(2) Uani 1 1 d . . . K2 K 0.77640(11) 0.00031(3) 0.05163(11) 0.0228(2) Uani 1 1 d . . . O1W O 0.8666(4) -0.04356(10) 0.3511(3) 0.0249(7) Uani 1 1 d D . . O2W O 1.7906(4) 0.02519(11) 1.5275(3) 0.0272(7) Uani 1 1 d D . . O3W O 0.6939(5) 0.20611(15) 0.1626(5) 0.0571(11) Uani 1 1 d D . . H3W1 H 0.701(7) 0.2209(16) 0.081(4) 0.068 Uiso 1 1 d D . . H1W1 H 0.830(7) -0.0690(7) 0.364(6) 0.068 Uiso 1 1 d D . . H1W2 H 0.836(7) -0.0235(11) 0.403(6) 0.068 Uiso 1 1 d D . . H2W1 H 1.887(3) 0.0334(19) 1.575(5) 0.068 Uiso 1 1 d D . . H2W2 H 1.741(5) 0.0186(19) 1.595(4) 0.068 Uiso 1 1 d D . . H3W2 H 0.770(5) 0.1862(15) 0.186(6) 0.068 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 0.01275(17) 0.01229(18) 0.01419(17) -0.00034(13) 0.00718(13) -0.00026(13) Mo2 0.01406(18) 0.01323(19) 0.01571(18) 0.00064(13) 0.00639(13) 0.00110(14) N1 0.0151(18) 0.023(2) 0.0160(17) -0.0040(14) 0.0056(14) -0.0035(15) N2 0.0163(19) 0.030(2) 0.031(2) -0.0023(16) 0.0130(16) 0.0002(16) N3 0.027(2) 0.020(2) 0.0189(18) -0.0001(14) 0.0085(15) 0.0025(16) N4 0.058(3) 0.032(2) 0.029(2) 0.0028(18) 0.026(2) -0.005(2) C1 0.018(2) 0.024(2) 0.026(2) -0.0019(18) 0.0105(18) -0.0014(18) C2 0.023(3) 0.045(3) 0.025(2) 0.002(2) 0.0037(19) 0.000(2) C3 0.019(2) 0.048(3) 0.023(2) 0.002(2) 0.0049(19) -0.004(2) C4 0.040(3) 0.030(3) 0.024(2) 0.007(2) 0.014(2) 0.018(2) C5 0.029(3) 0.033(3) 0.031(3) 0.001(2) 0.018(2) -0.001(2) C6 0.062(4) 0.024(3) 0.028(3) 0.007(2) 0.015(2) 0.015(3) C7 0.013(2) 0.024(2) 0.0101(19) 0.0017(16) 0.0003(15) 0.0021(17) C8 0.017(2) 0.016(2) 0.0133(19) 0.0024(16) 0.0057(15) 0.0008(17) C9 0.0114(19) 0.018(2) 0.0111(18) -0.0040(16) 0.0014(14) -0.0044(16) C10 0.0095(19) 0.018(2) 0.0151(19) -0.0012(16) 0.0021(15) -0.0021(16) O1 0.0120(14) 0.0166(15) 0.0210(14) 0.0029(12) 0.0085(11) 0.0005(11) O2 0.0149(14) 0.0165(15) 0.0149(13) 0.0018(11) 0.0063(11) 0.0001(11) O3 0.0213(16) 0.0181(16) 0.0231(15) -0.0047(12) 0.0126(12) -0.0024(12) O4 0.0246(16) 0.0168(16) 0.0211(15) 0.0003(12) 0.0076(12) 0.0053(13) O5 0.0187(15) 0.0175(16) 0.0173(14) 0.0000(11) 0.0091(12) 0.0020(12) O6 0.0181(15) 0.0139(14) 0.0122(13) 0.0007(11) 0.0068(11) 0.0027(11) O7 0.0304(17) 0.0139(15) 0.0187(15) 0.0002(12) 0.0084(12) 0.0052(13) O8 0.0174(15) 0.0254(16) 0.0156(14) 0.0037(12) 0.0083(11) -0.0021(12) O9 0.0161(15) 0.0152(15) 0.0229(15) -0.0016(12) 0.0048(12) 0.0027(12) O10 0.0138(15) 0.0168(15) 0.0228(15) -0.0037(12) 0.0064(11) 0.0002(12) O11 0.0157(16) 0.0303(18) 0.0300(16) -0.0032(13) 0.0076(13) -0.0039(13) O12 0.0222(17) 0.0248(18) 0.0344(17) -0.0131(14) 0.0100(13) -0.0049(13) K1 0.0171(4) 0.0246(5) 0.0165(4) -0.0031(4) 0.0074(3) 0.0019(4) K2 0.0201(5) 0.0233(5) 0.0247(5) -0.0014(4) 0.0063(4) -0.0017(4) O1W 0.0302(18) 0.0208(17) 0.0253(16) -0.0025(13) 0.0106(13) -0.0039(14) O2W 0.0208(17) 0.036(2) 0.0255(16) -0.0011(14) 0.0082(13) 0.0012(15) O3W 0.053(3) 0.064(3) 0.064(3) 0.017(2) 0.032(2) 0.019(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 O3 1.681(3) . ? Mo1 O2 1.939(2) . ? Mo1 O1 1.943(3) . ? Mo1 O5 2.118(3) . ? Mo1 N1 2.187(3) . ? Mo1 O6 2.215(3) . ? Mo1 Mo2 2.5482(5) . ? Mo1 K1 4.0159(9) 1_554 ? Mo2 O4 1.682(3) . ? Mo2 O2 1.929(3) . ? Mo2 O1 1.949(3) . ? Mo2 O9 2.123(3) . ? Mo2 N3 2.186(3) . ? Mo2 O10 2.221(3) . ? N1 C1 1.318(5) . ? N1 C3 1.372(5) . ? N2 C1 1.334(5) . ? N2 C2 1.354(5) . ? N3 C5 1.318(5) . ? N3 C4 1.378(5) . ? N4 C5 1.334(6) . ? N4 C6 1.353(6) . ? C2 C3 1.340(6) . ? C4 C6 1.346(6) . ? C7 O11 1.222(5) . ? C7 O9 1.287(5) . ? C7 C8 1.561(5) . ? C8 O12 1.215(5) . ? C8 O10 1.273(5) . ? C9 O7 1.236(5) . ? C9 O6 1.270(4) . ? C9 C10 1.554(5) . ? C9 K2 3.459(4) 1_656 ? C10 O8 1.228(4) . ? C10 O5 1.270(4) . ? C10 K2 3.390(4) 1_656 ? C10 K2 3.440(4) 3_756 ? O2 K1 3.085(3) 1_554 ? O6 K1 2.766(2) 1_554 ? O7 K1 2.798(3) 3_857 ? O7 K2 2.853(3) 1_656 ? O8 K2 2.737(3) 3_756 ? O8 K1 2.772(3) . ? O8 K2 2.838(3) 1_656 ? O10 K1 2.785(3) 1_554 ? O11 K1 2.756(3) 1_454 ? O11 K2 2.874(3) . ? O12 K2 2.744(3) . ? O12 K2 2.745(3) 3_755 ? K1 O11 2.756(3) 1_656 ? K1 O6 2.766(2) 1_556 ? K1 O10 2.785(3) 1_556 ? K1 O7 2.798(3) 3_857 ? K1 O2W 2.853(3) . ? K1 O2 3.085(3) 1_556 ? K1 Mo1 4.0159(9) 1_556 ? K1 K2 4.0591(12) 1_656 ? K1 K2 4.0830(12) 3_756 ? K2 O8 2.737(3) 3_756 ? K2 O12 2.745(3) 3_755 ? K2 O1W 2.835(3) . ? K2 O8 2.838(3) 1_454 ? K2 O7 2.853(3) 1_454 ? K2 C10 3.390(4) 1_454 ? K2 C10 3.440(4) 3_756 ? K2 C9 3.459(4) 1_454 ? K2 K1 4.0591(12) 1_454 ? K2 K1 4.0830(12) 3_756 ? 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 O3 Mo1 O2 107.53(12) . . ? O3 Mo1 O1 107.45(12) . . ? O2 Mo1 O1 93.44(11) . . ? O3 Mo1 O5 88.80(11) . . ? O2 Mo1 O5 162.86(10) . . ? O1 Mo1 O5 86.34(11) . . ? O3 Mo1 N1 92.67(13) . . ? O2 Mo1 N1 84.84(11) . . ? O1 Mo1 N1 159.31(12) . . ? O5 Mo1 N1 89.34(11) . . ? O3 Mo1 O6 159.07(12) . . ? O2 Mo1 O6 89.39(10) . . ? O1 Mo1 O6 83.07(10) . . ? O5 Mo1 O6 73.56(9) . . ? N1 Mo1 O6 76.30(11) . . ? O3 Mo1 Mo2 99.46(10) . . ? O2 Mo1 Mo2 48.63(8) . . ? O1 Mo1 Mo2 49.20(7) . . ? O5 Mo1 Mo2 135.31(8) . . ? N1 Mo1 Mo2 133.45(8) . . ? O6 Mo1 Mo2 101.02(7) . . ? O3 Mo1 K1 152.47(9) . 1_554 ? O2 Mo1 K1 48.24(8) . 1_554 ? O1 Mo1 K1 89.16(8) . 1_554 ? O5 Mo1 K1 114.64(7) . 1_554 ? N1 Mo1 K1 74.30(8) . 1_554 ? O6 Mo1 K1 41.22(6) . 1_554 ? Mo2 Mo1 K1 74.552(16) . 1_554 ? O4 Mo2 O2 109.85(12) . . ? O4 Mo2 O1 104.39(12) . . ? O2 Mo2 O1 93.55(11) . . ? O4 Mo2 O9 93.26(12) . . ? O2 Mo2 O9 156.57(10) . . ? O1 Mo2 O9 84.00(11) . . ? O4 Mo2 N3 87.20(13) . . ? O2 Mo2 N3 87.72(12) . . ? O1 Mo2 N3 167.08(12) . . ? O9 Mo2 N3 89.72(12) . . ? O4 Mo2 O10 161.94(12) . . ? O2 Mo2 O10 83.01(10) . . ? O1 Mo2 O10 86.85(10) . . ? O9 Mo2 O10 73.61(10) . . ? N3 Mo2 O10 80.54(11) . . ? O4 Mo2 Mo1 98.89(9) . . ? O2 Mo2 Mo1 48.95(7) . . ? O1 Mo2 Mo1 48.99(8) . . ? O9 Mo2 Mo1 132.98(7) . . ? N3 Mo2 Mo1 135.85(10) . . ? O10 Mo2 Mo1 99.14(7) . . ? C1 N1 C3 105.9(4) . . ? C1 N1 Mo1 127.0(3) . . ? C3 N1 Mo1 126.4(3) . . ? C1 N2 C2 108.1(4) . . ? C5 N3 C4 106.3(4) . . ? C5 N3 Mo2 129.6(3) . . ? C4 N3 Mo2 123.5(3) . . ? C5 N4 C6 109.1(4) . . ? N1 C1 N2 110.3(4) . . ? C3 C2 N2 106.4(4) . . ? C2 C3 N1 109.3(4) . . ? C6 C4 N3 109.2(4) . . ? N3 C5 N4 109.6(4) . . ? C4 C6 N4 105.9(4) . . ? O11 C7 O9 125.0(4) . . ? O11 C7 C8 120.3(4) . . ? O9 C7 C8 114.7(3) . . ? O12 C8 O10 127.4(4) . . ? O12 C8 C7 119.5(4) . . ? O10 C8 C7 113.1(3) . . ? O7 C9 O6 126.1(3) . . ? O7 C9 C10 120.0(3) . . ? O6 C9 C10 114.0(3) . . ? O7 C9 K2 51.23(19) . 1_656 ? O6 C9 K2 154.6(3) . 1_656 ? C10 C9 K2 74.4(2) . 1_656 ? O8 C10 O5 125.6(3) . . ? O8 C10 C9 120.4(4) . . ? O5 C10 C9 114.0(3) . . ? O8 C10 K2 53.5(2) . 1_656 ? O5 C10 K2 142.4(3) . 1_656 ? C9 C10 K2 79.4(2) . 1_656 ? O8 C10 K2 46.17(19) . 3_756 ? O5 C10 K2 123.2(2) . 3_756 ? C9 C10 K2 102.2(2) . 3_756 ? K2 C10 K2 84.31(9) 1_656 3_756 ? Mo1 O1 Mo2 81.81(10) . . ? Mo2 O2 Mo1 82.42(10) . . ? Mo2 O2 K1 109.29(10) . 1_554 ? Mo1 O2 K1 103.80(10) . 1_554 ? C10 O5 Mo1 120.6(2) . . ? C9 O6 Mo1 116.8(2) . . ? C9 O6 K1 134.8(2) . 1_554 ? Mo1 O6 K1 106.93(9) . 1_554 ? C9 O7 K1 137.1(3) . 3_857 ? C9 O7 K2 109.0(2) . 1_656 ? K1 O7 K2 92.52(8) 3_857 1_656 ? C10 O8 K2 115.0(2) . 3_756 ? C10 O8 K1 134.1(3) . . ? K2 O8 K1 95.65(8) 3_756 . ? C10 O8 K2 106.1(2) . 1_656 ? K2 O8 K2 110.63(10) 3_756 1_656 ? K1 O8 K2 92.70(8) . 1_656 ? C7 O9 Mo2 119.1(2) . . ? C8 O10 Mo2 117.8(2) . . ? C8 O10 K1 128.8(2) . 1_554 ? Mo2 O10 K1 111.24(10) . 1_554 ? C7 O11 K1 146.2(3) . 1_454 ? C7 O11 K2 117.6(3) . . ? K1 O11 K2 92.25(9) 1_454 . ? C8 O12 K2 122.8(3) . . ? C8 O12 K2 135.3(3) . 3_755 ? K2 O12 K2 100.63(9) . 3_755 ? O11 K1 O6 129.98(9) 1_656 1_556 ? O11 K1 O8 66.83(8) 1_656 . ? O6 K1 O8 162.81(9) 1_556 . ? O11 K1 O10 142.69(9) 1_656 1_556 ? O6 K1 O10 73.86(8) 1_556 1_556 ? O8 K1 O10 94.00(8) . 1_556 ? O11 K1 O7 115.18(9) 1_656 3_857 ? O6 K1 O7 91.18(8) 1_556 3_857 ? O8 K1 O7 76.12(8) . 3_857 ? O10 K1 O7 88.56(8) 1_556 3_857 ? O11 K1 O2W 74.47(9) 1_656 . ? O6 K1 O2W 70.51(8) 1_556 . ? O8 K1 O2W 116.88(9) . . ? O10 K1 O2W 141.42(9) 1_556 . ? O7 K1 O2W 77.99(9) 3_857 . ? O11 K1 O2 107.13(8) 1_656 1_556 ? O6 K1 O2 59.77(7) 1_556 1_556 ? O8 K1 O2 123.40(8) . 1_556 ? O10 K1 O2 55.79(7) 1_556 1_556 ? O7 K1 O2 137.69(8) 3_857 1_556 ? O2W K1 O2 114.46(8) . 1_556 ? O11 K1 Mo1 120.79(7) 1_656 1_556 ? O6 K1 Mo1 31.85(5) 1_556 1_556 ? O8 K1 Mo1 149.30(7) . 1_556 ? O10 K1 Mo1 61.54(5) 1_556 1_556 ? O7 K1 Mo1 118.28(6) 3_857 1_556 ? O2W K1 Mo1 93.32(6) . 1_556 ? O2 K1 Mo1 27.96(5) 1_556 1_556 ? O11 K1 K2 45.03(6) 1_656 1_656 ? O6 K1 K2 142.04(6) 1_556 1_656 ? O8 K1 K2 44.29(6) . 1_656 ? O10 K1 K2 136.18(6) 1_556 1_656 ? O7 K1 K2 71.15(6) 3_857 1_656 ? O2W K1 K2 73.01(6) . 1_656 ? O2 K1 K2 150.20(6) 1_556 1_656 ? Mo1 K1 K2 161.99(3) 1_556 1_656 ? O11 K1 K2 106.37(6) 1_656 3_756 ? O6 K1 K2 121.14(6) 1_556 3_756 ? O8 K1 K2 41.85(6) . 3_756 ? O10 K1 K2 69.93(6) 1_556 3_756 ? O7 K1 K2 44.27(6) 3_857 3_756 ? O2W K1 K2 117.75(7) . 3_756 ? O2 K1 K2 123.39(6) 1_556 3_756 ? Mo1 K1 K2 129.26(3) 1_556 3_756 ? K2 K1 K2 68.54(3) 1_656 3_756 ? O8 K2 O12 170.96(9) 3_756 . ? O8 K2 O12 100.95(9) 3_756 3_755 ? O12 K2 O12 79.37(9) . 3_755 ? O8 K2 O1W 80.02(9) 3_756 . ? O12 K2 O1W 91.16(9) . . ? O12 K2 O1W 105.28(9) 3_755 . ? O8 K2 O8 69.37(10) 3_756 1_454 ? O12 K2 O8 116.85(9) . 1_454 ? O12 K2 O8 134.85(9) 3_755 1_454 ? O1W K2 O8 115.48(9) . 1_454 ? O8 K2 O7 75.76(8) 3_756 1_454 ? O12 K2 O7 112.88(9) . 1_454 ? O12 K2 O7 75.89(9) 3_755 1_454 ? O1W K2 O7 155.46(9) . 1_454 ? O8 K2 O7 58.96(8) 1_454 1_454 ? O8 K2 O11 122.15(9) 3_756 . ? O12 K2 O11 59.27(8) . . ? O12 K2 O11 136.32(9) 3_755 . ? O1W K2 O11 89.96(9) . . ? O8 K2 O11 64.42(8) 1_454 . ? O7 K2 O11 106.18(8) 1_454 . ? O8 K2 C10 81.83(9) 3_756 1_454 ? O12 K2 C10 106.08(9) . 1_454 ? O12 K2 C10 118.25(9) 3_755 1_454 ? O1W K2 C10 135.20(9) . 1_454 ? O8 K2 C10 20.36(8) 1_454 1_454 ? O7 K2 C10 44.60(8) 1_454 1_454 ? O11 K2 C10 66.30(9) . 1_454 ? O8 K2 C10 18.88(8) 3_756 3_756 ? O12 K2 C10 152.29(9) . 3_756 ? O12 K2 C10 105.45(9) 3_755 3_756 ? O1W K2 C10 61.16(9) . 3_756 ? O8 K2 C10 79.56(9) 1_454 3_756 ? O7 K2 C10 94.62(9) 1_454 3_756 ? O11 K2 C10 117.61(9) . 3_756 ? C10 K2 C10 95.69(9) 1_454 3_756 ? O8 K2 C9 82.98(9) 3_756 1_454 ? O12 K2 C9 106.05(9) . 1_454 ? O12 K2 C9 92.23(9) 3_755 1_454 ? O1W K2 C9 157.55(9) . 1_454 ? O8 K2 C9 43.82(8) 1_454 1_454 ? O7 K2 C9 19.74(8) 1_454 1_454 ? O11 K2 C9 86.74(9) . 1_454 ? C10 K2 C9 26.20(9) 1_454 1_454 ? C10 K2 C9 101.06(9) 3_756 1_454 ? O8 K2 K1 79.69(6) 3_756 1_454 ? O12 K2 K1 100.40(6) . 1_454 ? O12 K2 K1 177.44(7) 3_755 1_454 ? O1W K2 K1 77.26(6) . 1_454 ? O8 K2 K1 43.01(5) 1_454 1_454 ? O7 K2 K1 101.93(6) 1_454 1_454 ? O11 K2 K1 42.72(6) . 1_454 ? C10 K2 K1 59.31(6) 1_454 1_454 ? C10 K2 K1 75.96(7) 3_756 1_454 ? C9 K2 K1 85.37(7) 1_454 1_454 ? O8 K2 K1 42.50(6) 3_756 3_756 ? O12 K2 K1 142.80(7) . 3_756 ? O12 K2 K1 67.93(6) 3_755 3_756 ? O1W K2 K1 113.70(7) . 3_756 ? O8 K2 K1 78.21(6) 1_454 3_756 ? O7 K2 K1 43.20(6) 1_454 3_756 ? O11 K2 K1 141.91(7) . 3_756 ? C10 K2 K1 76.14(7) 1_454 3_756 ? C10 K2 K1 58.73(6) 3_756 3_756 ? C9 K2 K1 59.79(6) 1_454 3_756 ? K1 K2 K1 111.46(3) 1_454 3_756 ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 26.99 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.491 _refine_diff_density_min -0.722 _refine_diff_density_rms 0.122 # Attachment '5.cif' data_sad5 _database_code_depnum_ccdc_archive 'CCDC 891645' #TrackingRef '5.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'Potassium imidazolium oxalato imidazole molybdate(IV)' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H17 K Mo3 N8 O19' _chemical_formula_weight 976.32 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' K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.5495(4) _cell_length_b 11.8097(5) _cell_length_c 15.7370(8) _cell_angle_alpha 76.902(4) _cell_angle_beta 73.425(4) _cell_angle_gamma 66.739(4) _cell_volume 1549.61(12) _cell_formula_units_Z 2 _cell_measurement_temperature 396(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.092 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 880 _exptl_absorpt_coefficient_mu 1.403 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8725 _exptl_absorpt_correction_T_max 0.8725 _exptl_absorpt_process_details Sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 396(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15258 _diffrn_reflns_av_R_equivalents 0.0678 _diffrn_reflns_av_sigmaI/netI 0.1161 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.72 _diffrn_reflns_theta_max 27.00 _reflns_number_total 6635 _reflns_number_gt 4808 _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 ? _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. ; _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^)+(0.0291P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6635 _refine_ls_number_parameters 446 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0921 _refine_ls_R_factor_gt 0.0601 _refine_ls_wR_factor_ref 0.1191 _refine_ls_wR_factor_gt 0.1045 _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_restrained_S_all 1.053 _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 0.15795(7) 0.66444(5) 1.31150(4) 0.01577(15) Uani 1 1 d . . . Mo2 Mo -0.08949(7) 0.78317(5) 1.25883(4) 0.01631(15) Uani 1 1 d . . . Mo3 Mo 0.15972(7) 0.80844(5) 1.16833(4) 0.01672(15) Uani 1 1 d . . . C1 C -0.3866(9) 1.0302(7) 1.2984(5) 0.034(2) Uani 1 1 d . . . H1A H -0.3454 1.0796 1.2512 0.040 Uiso 1 1 calc R . . C2 C -0.4211(9) 0.8749(7) 1.3915(5) 0.033(2) Uani 1 1 d . . . H2B H -0.4052 0.7944 1.4206 0.040 Uiso 1 1 calc R . . C3 C -0.5467(9) 0.9734(7) 1.4143(5) 0.037(2) Uani 1 1 d . . . H3A H -0.6330 0.9753 1.4608 0.045 Uiso 1 1 calc R . . C4 C 0.2053(8) 0.5846(6) 1.5117(4) 0.0228(17) Uani 1 1 d . . . H4B H 0.1391 0.5395 1.5262 0.027 Uiso 1 1 calc R . . C5 C 0.3391(9) 0.6994(7) 1.4394(5) 0.033(2) Uani 1 1 d . . . H5A H 0.3833 0.7484 1.3935 0.039 Uiso 1 1 calc R . . C6 C 0.3633(9) 0.6695(7) 1.5226(5) 0.036(2) Uani 1 1 d . . . H6B H 0.4253 0.6942 1.5451 0.043 Uiso 1 1 calc R . . C7 C 0.2185(9) 1.0477(7) 1.0464(5) 0.0305(19) Uani 1 1 d . . . H7A H 0.1543 1.0537 1.0096 0.037 Uiso 1 1 calc R . . C8 C 0.3514(8) 0.9838(6) 1.1498(5) 0.0257(18) Uani 1 1 d . . . H8A H 0.3943 0.9365 1.1982 0.031 Uiso 1 1 calc R . . C9 C 0.3822(9) 1.0858(7) 1.1012(4) 0.0275(18) Uani 1 1 d . . . H9A H 0.4475 1.1213 1.1099 0.033 Uiso 1 1 calc R . . C10 C -0.2364(8) 0.6983(6) 1.1572(4) 0.0200(16) Uani 1 1 d . . . C11 C -0.2327(8) 0.6093(6) 1.2475(4) 0.0166(15) Uani 1 1 d . . . C12 C 0.3888(8) 0.4095(6) 1.3049(4) 0.0211(16) Uani 1 1 d . . . C13 C 0.2348(8) 0.3947(6) 1.3658(5) 0.0238(17) Uani 1 1 d . . . C14 C 0.2255(9) 0.7771(6) 0.9790(4) 0.0269(18) Uani 1 1 d . . . C15 C 0.3814(8) 0.6979(6) 1.0102(4) 0.0211(16) Uani 1 1 d . . . C16 C 0.0457(12) 0.8315(9) 0.7735(7) 0.054(3) Uani 1 1 d . . . H21A H 0.0908 0.8629 0.8033 0.065 Uiso 1 1 calc R . . C17 C -0.0586(12) 0.7144(11) 0.7429(8) 0.068(3) Uani 1 1 d . . . H22A H -0.0961 0.6510 0.7476 0.082 Uiso 1 1 calc R . . C18 C 0.0154(13) 0.8734(11) 0.6922(10) 0.079(4) Uani 1 1 d . . . H23A H 0.0364 0.9403 0.6542 0.095 Uiso 1 1 calc R . . N1 N -0.3177(7) 0.9082(5) 1.3188(4) 0.0221(14) Uani 1 1 d . . . N2 N -0.5225(7) 1.0709(6) 1.3554(4) 0.0344(17) Uani 1 1 d . . . H2A H -0.5852 1.1469 1.3551 0.041 Uiso 1 1 calc R . . N3 N 0.2390(6) 0.6464(5) 1.4325(3) 0.0187(13) Uani 1 1 d . . . N4 N 0.2786(7) 0.5953(5) 1.5680(4) 0.0246(15) Uani 1 1 d . . . H4A H 0.2737 0.5618 1.6229 0.030 Uiso 1 1 calc R . . N5 N 0.2484(7) 0.9611(5) 1.1171(3) 0.0194(13) Uani 1 1 d . . . N6 N 0.2966(8) 1.1246(5) 1.0372(4) 0.0301(16) Uani 1 1 d . . . H6A H 0.2930 1.1882 0.9972 0.036 Uiso 1 1 calc R . . N7 N -0.0023(11) 0.7354(11) 0.8028(8) 0.102(4) Uani 1 1 d . . . H7B H 0.0028 0.6922 0.8545 0.122 Uiso 1 1 calc R . . N8 N -0.0505(12) 0.8024(13) 0.6748(8) 0.104(4) Uani 1 1 d . . . H8B H -0.0825 0.8125 0.6268 0.124 Uiso 1 1 calc R . . O1 O 0.1034(5) 0.6520(4) 1.1994(3) 0.0163(10) Uani 1 1 d . . . O2 O -0.0429(5) 0.7616(4) 1.3734(3) 0.0171(10) Uani 1 1 d . . . O3 O 0.2480(5) 0.7898(4) 1.2680(3) 0.0177(10) Uani 1 1 d . . . O4 O -0.1862(5) 0.6416(4) 1.3033(3) 0.0179(10) Uani 1 1 d . . . O5 O -0.0429(5) 0.9292(4) 1.2058(3) 0.0170(10) Uani 1 1 d . . . O6 O 0.3727(5) 0.5243(4) 1.2727(3) 0.0202(11) Uani 1 1 d . . . O7 O -0.1901(5) 0.7871(4) 1.1547(3) 0.0199(11) Uani 1 1 d . . . O8 O 0.1194(5) 0.4970(4) 1.3715(3) 0.0210(11) Uani 1 1 d . . . O9 O 0.1175(5) 0.8338(4) 1.0396(3) 0.0204(11) Uani 1 1 d . . . O10 O -0.2746(6) 0.5213(4) 1.2593(3) 0.0266(12) Uani 1 1 d . . . O11 O 0.3716(5) 0.7012(4) 1.0925(3) 0.0189(11) Uani 1 1 d . . . O12 O 0.5088(6) 0.3210(4) 1.2921(3) 0.0324(14) Uani 1 1 d . . . O13 O -0.2848(6) 0.6801(5) 1.0996(3) 0.0324(13) Uani 1 1 d . . . O14 O 0.4962(6) 0.6401(5) 0.9576(3) 0.0313(13) Uani 1 1 d . . . O15 O 0.2333(7) 0.2931(4) 1.3999(4) 0.0484(19) Uani 1 1 d . . . O16 O 0.2179(7) 0.7791(5) 0.9028(3) 0.0475(17) Uani 1 1 d . . . K1 K -0.37602(18) 0.47633(13) 1.13088(9) 0.0212(3) Uani 1 1 d . . . O1W O -0.1922(10) 0.4923(8) 0.9334(5) 0.101(3) Uiso 1 1 d . . . O2W O -0.0599(19) 0.9437(13) 1.4592(8) 0.079(5) Uani 0.60 1 d P . . O2W' O -0.067(2) 0.8931(16) 1.5064(11) 0.056(6) Uani 0.40 1 d P . . O3W O -0.0367(17) 0.4196(13) 1.0529(11) 0.288(11) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mo1 0.0206(3) 0.0130(3) 0.0126(3) 0.0024(2) -0.0053(2) -0.0058(2) Mo2 0.0196(3) 0.0118(3) 0.0177(3) 0.0011(2) -0.0058(2) -0.0061(2) Mo3 0.0227(3) 0.0147(3) 0.0124(3) 0.0025(2) -0.0049(2) -0.0078(3) C1 0.035(5) 0.027(4) 0.040(5) -0.005(4) -0.009(4) -0.011(4) C2 0.027(5) 0.021(4) 0.044(5) 0.000(4) 0.003(4) -0.011(4) C3 0.029(5) 0.028(4) 0.046(5) 0.003(4) 0.002(4) -0.012(4) C4 0.025(4) 0.019(4) 0.017(4) 0.005(3) -0.005(3) -0.005(3) C5 0.046(5) 0.040(5) 0.018(4) 0.017(4) -0.014(4) -0.028(4) C6 0.044(5) 0.047(5) 0.029(4) 0.012(4) -0.018(4) -0.031(4) C7 0.050(5) 0.024(4) 0.017(4) 0.006(3) -0.011(4) -0.014(4) C8 0.026(4) 0.023(4) 0.021(4) 0.008(3) -0.007(3) -0.006(3) C9 0.040(5) 0.029(4) 0.020(4) 0.003(3) -0.012(3) -0.019(4) C10 0.026(4) 0.018(4) 0.017(4) 0.004(3) -0.004(3) -0.012(3) C11 0.018(4) 0.015(3) 0.010(3) 0.004(3) -0.005(3) -0.001(3) C12 0.021(4) 0.018(4) 0.018(4) -0.002(3) -0.006(3) 0.001(3) C13 0.022(4) 0.013(4) 0.026(4) 0.001(3) 0.000(3) -0.001(3) C14 0.047(5) 0.018(4) 0.017(4) 0.003(3) -0.015(3) -0.010(4) C15 0.027(4) 0.017(4) 0.020(4) 0.004(3) -0.005(3) -0.012(3) C16 0.072(8) 0.034(5) 0.080(8) -0.008(5) -0.053(6) -0.016(5) C17 0.045(7) 0.086(9) 0.078(8) -0.012(7) -0.029(6) -0.017(6) C18 0.049(7) 0.067(8) 0.124(12) -0.036(8) 0.003(7) -0.026(6) N1 0.021(3) 0.015(3) 0.029(3) -0.002(3) -0.007(3) -0.004(3) N2 0.027(4) 0.024(3) 0.050(4) -0.010(3) -0.008(3) -0.003(3) N3 0.020(3) 0.023(3) 0.013(3) 0.006(2) -0.002(2) -0.013(3) N4 0.034(4) 0.032(3) 0.013(3) 0.012(3) -0.013(3) -0.021(3) N5 0.027(3) 0.014(3) 0.016(3) 0.003(2) -0.007(3) -0.009(3) N6 0.057(5) 0.025(3) 0.013(3) 0.013(3) -0.009(3) -0.026(3) N7 0.059(7) 0.106(9) 0.148(11) -0.063(8) -0.048(7) 0.006(6) N8 0.054(7) 0.149(12) 0.103(9) -0.052(9) -0.025(6) -0.006(7) O1 0.027(3) 0.008(2) 0.015(2) 0.0035(19) -0.008(2) -0.009(2) O2 0.018(3) 0.012(2) 0.017(2) 0.0010(19) -0.0012(19) -0.0032(19) O3 0.025(3) 0.018(2) 0.012(2) 0.003(2) -0.0088(19) -0.009(2) O4 0.023(3) 0.016(2) 0.016(2) 0.003(2) -0.006(2) -0.010(2) O5 0.022(3) 0.013(2) 0.016(2) 0.002(2) -0.0076(19) -0.006(2) O6 0.022(3) 0.017(2) 0.016(2) 0.005(2) -0.003(2) -0.006(2) O7 0.028(3) 0.019(2) 0.018(2) 0.011(2) -0.012(2) -0.017(2) O8 0.022(3) 0.017(2) 0.021(3) 0.003(2) -0.004(2) -0.007(2) O9 0.024(3) 0.019(2) 0.015(2) 0.001(2) -0.004(2) -0.007(2) O10 0.049(4) 0.023(3) 0.023(3) 0.010(2) -0.020(2) -0.027(3) O11 0.022(3) 0.018(2) 0.015(2) 0.002(2) -0.008(2) -0.005(2) O12 0.029(3) 0.016(3) 0.036(3) 0.003(2) 0.000(2) 0.000(2) O13 0.053(4) 0.037(3) 0.023(3) 0.018(3) -0.023(3) -0.034(3) O14 0.025(3) 0.032(3) 0.028(3) -0.010(2) 0.001(2) -0.003(2) O15 0.043(4) 0.012(3) 0.062(4) 0.009(3) 0.012(3) -0.004(3) O16 0.068(5) 0.040(3) 0.022(3) -0.009(3) -0.022(3) 0.005(3) K1 0.0261(9) 0.0212(8) 0.0167(7) -0.0021(6) -0.0055(6) -0.0084(7) O2W 0.119(13) 0.071(11) 0.057(9) -0.030(8) -0.001(9) -0.046(10) O2W' 0.068(13) 0.046(12) 0.037(11) -0.004(9) 0.013(10) -0.021(10) O3W 0.188(15) 0.198(15) 0.35(2) -0.046(14) 0.126(15) -0.059(12) _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 O3 1.900(4) . ? Mo1 O2 1.909(4) . ? Mo1 O1 2.026(4) . ? Mo1 O6 2.093(4) . ? Mo1 O8 2.113(4) . ? Mo1 N3 2.190(6) . ? Mo1 Mo2 2.4921(8) . ? Mo1 Mo3 2.4966(7) . ? Mo2 O5 1.900(4) . ? Mo2 O2 1.916(4) . ? Mo2 O1 2.022(4) . ? Mo2 O7 2.107(5) . ? Mo2 O4 2.112(4) . ? Mo2 N1 2.177(6) . ? Mo2 Mo3 2.4931(8) . ? Mo3 O3 1.915(4) . ? Mo3 O5 1.918(4) . ? Mo3 O1 2.041(4) . ? Mo3 O11 2.099(4) . ? Mo3 O9 2.110(4) . ? Mo3 N5 2.185(5) . ? C1 N2 1.326(9) . ? C1 N1 1.332(9) . ? C2 C3 1.328(10) . ? C2 N1 1.377(8) . ? C3 N2 1.357(8) . ? C4 N3 1.316(7) . ? C4 N4 1.329(9) . ? C5 C6 1.338(9) . ? C5 N3 1.371(9) . ? C6 N4 1.372(9) . ? C7 N5 1.342(8) . ? C7 N6 1.347(10) . ? C8 C9 1.362(9) . ? C8 N5 1.365(9) . ? C9 N6 1.363(9) . ? C10 O13 1.221(8) . ? C10 O7 1.278(8) . ? C10 C11 1.565(8) . ? C10 K1 3.520(7) . ? C11 O10 1.214(8) . ? C11 O4 1.274(8) . ? C11 K1 3.485(8) . ? C12 O12 1.210(7) . ? C12 O6 1.299(7) . ? C12 C13 1.559(9) . ? C12 K1 3.175(7) 1_655 ? C13 O15 1.202(8) . ? C13 O8 1.274(7) . ? C14 O16 1.215(8) . ? C14 O9 1.267(8) . ? C14 C15 1.562(10) . ? C14 K1 3.397(8) 2_567 ? C15 O14 1.226(8) . ? C15 O11 1.279(8) . ? C15 K1 3.360(7) 1_655 ? C15 K1 3.375(8) 2_567 ? C16 N7 1.327(14) . ? C16 C18 1.333(15) . ? C17 N7 1.319(14) . ? C17 N8 1.322(13) . ? C18 N8 1.339(15) . ? O6 K1 2.739(4) 1_655 ? O10 K1 2.705(5) . ? O11 K1 2.876(4) 1_655 ? O12 K1 2.984(5) 1_655 ? O13 K1 2.768(5) . ? O14 K1 2.858(6) 2_567 ? O14 K1 3.211(5) 1_655 ? O16 K1 2.887(6) 2_567 ? K1 O6 2.739(4) 1_455 ? K1 O14 2.858(6) 2_567 ? K1 O11 2.876(4) 1_455 ? K1 O16 2.887(6) 2_567 ? K1 O12 2.984(5) 1_455 ? K1 O3W 2.974(14) . ? K1 O1W 3.108(8) . ? K1 C12 3.175(7) 1_455 ? K1 O14 3.211(5) 1_455 ? K1 C15 3.360(7) 1_455 ? O2W O2W' 0.846(15) . ? 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 O3 Mo1 O2 99.33(18) . . ? O3 Mo1 O1 100.64(17) . . ? O2 Mo1 O1 100.15(19) . . ? O3 Mo1 O6 91.87(18) . . ? O2 Mo1 O6 165.23(16) . . ? O1 Mo1 O6 87.08(18) . . ? O3 Mo1 O8 163.47(18) . . ? O2 Mo1 O8 91.72(17) . . ? O1 Mo1 O8 89.36(17) . . ? O6 Mo1 O8 75.38(17) . . ? O3 Mo1 N3 84.31(19) . . ? O2 Mo1 N3 86.5(2) . . ? O1 Mo1 N3 170.89(18) . . ? O6 Mo1 N3 85.10(19) . . ? O8 Mo1 N3 84.16(19) . . ? O3 Mo1 Mo2 96.44(13) . . ? O2 Mo1 Mo2 49.47(13) . . ? O1 Mo1 Mo2 51.92(12) . . ? O6 Mo1 Mo2 138.98(13) . . ? O8 Mo1 Mo2 100.09(13) . . ? N3 Mo1 Mo2 135.60(15) . . ? O3 Mo1 Mo3 49.39(13) . . ? O2 Mo1 Mo3 96.37(12) . . ? O1 Mo1 Mo3 52.41(11) . . ? O6 Mo1 Mo3 98.23(11) . . ? O8 Mo1 Mo3 141.72(13) . . ? N3 Mo1 Mo3 133.55(14) . . ? Mo2 Mo1 Mo3 59.97(2) . . ? O5 Mo2 O2 99.67(19) . . ? O5 Mo2 O1 100.80(17) . . ? O2 Mo2 O1 100.07(17) . . ? O5 Mo2 O7 93.65(17) . . ? O2 Mo2 O7 163.79(17) . . ? O1 Mo2 O7 86.34(18) . . ? O5 Mo2 O4 166.59(18) . . ? O2 Mo2 O4 90.47(17) . . ? O1 Mo2 O4 85.89(17) . . ? O7 Mo2 O4 75.05(16) . . ? O5 Mo2 N1 85.94(19) . . ? O2 Mo2 N1 84.7(2) . . ? O1 Mo2 N1 170.8(2) . . ? O7 Mo2 N1 87.0(2) . . ? O4 Mo2 N1 86.27(19) . . ? O5 Mo2 Mo1 96.84(14) . . ? O2 Mo2 Mo1 49.23(13) . . ? O1 Mo2 Mo1 52.08(13) . . ? O7 Mo2 Mo1 138.31(13) . . ? O4 Mo2 Mo1 96.43(12) . . ? N1 Mo2 Mo1 133.80(16) . . ? O5 Mo2 Mo3 49.54(13) . . ? O2 Mo2 Mo3 96.30(13) . . ? O1 Mo2 Mo3 52.50(12) . . ? O7 Mo2 Mo3 99.37(12) . . ? O4 Mo2 Mo3 138.39(12) . . ? N1 Mo2 Mo3 135.15(15) . . ? Mo1 Mo2 Mo3 60.11(2) . . ? O3 Mo3 O5 99.77(18) . . ? O3 Mo3 O1 99.58(17) . . ? O5 Mo3 O1 99.51(18) . . ? O3 Mo3 O11 93.66(18) . . ? O5 Mo3 O11 164.27(17) . . ? O1 Mo3 O11 86.17(17) . . ? O3 Mo3 O9 165.22(18) . . ? O5 Mo3 O9 90.12(18) . . ? O1 Mo3 O9 89.49(17) . . ? O11 Mo3 O9 75.19(17) . . ? O3 Mo3 N5 83.9(2) . . ? O5 Mo3 N5 88.29(19) . . ? O1 Mo3 N5 170.71(19) . . ? O11 Mo3 N5 85.02(19) . . ? O9 Mo3 N5 85.44(19) . . ? O3 Mo3 Mo2 96.00(13) . . ? O5 Mo3 Mo2 48.93(12) . . ? O1 Mo3 Mo2 51.79(12) . . ? O11 Mo3 Mo2 137.86(13) . . ? O9 Mo3 Mo2 98.79(13) . . ? N5 Mo3 Mo2 136.74(15) . . ? O3 Mo3 Mo1 48.86(13) . . ? O5 Mo3 Mo1 96.22(12) . . ? O1 Mo3 Mo1 51.86(12) . . ? O11 Mo3 Mo1 98.78(11) . . ? O9 Mo3 Mo1 141.35(13) . . ? N5 Mo3 Mo1 132.69(15) . . ? Mo2 Mo3 Mo1 59.93(2) . . ? N2 C1 N1 110.0(7) . . ? C3 C2 N1 110.7(6) . . ? C2 C3 N2 105.5(7) . . ? N3 C4 N4 111.0(7) . . ? C6 C5 N3 109.3(6) . . ? C5 C6 N4 106.4(7) . . ? N5 C7 N6 109.0(7) . . ? C9 C8 N5 110.1(6) . . ? N6 C9 C8 105.2(7) . . ? O13 C10 O7 127.3(6) . . ? O13 C10 C11 119.5(6) . . ? O7 C10 C11 113.2(6) . . ? O13 C10 K1 43.7(3) . . ? O7 C10 K1 171.0(5) . . ? C11 C10 K1 75.8(4) . . ? O10 C11 O4 126.5(6) . . ? O10 C11 C10 120.2(6) . . ? O4 C11 C10 113.2(6) . . ? O10 C11 K1 41.9(3) . . ? O4 C11 K1 168.3(4) . . ? C10 C11 K1 78.4(4) . . ? O12 C12 O6 125.5(6) . . ? O12 C12 C13 121.6(6) . . ? O6 C12 C13 112.9(5) . . ? O12 C12 K1 69.9(4) . 1_655 ? O6 C12 K1 58.9(3) . 1_655 ? C13 C12 K1 159.4(5) . 1_655 ? O15 C13 O8 126.7(7) . . ? O15 C13 C12 119.8(6) . . ? O8 C13 C12 113.4(6) . . ? O16 C14 O9 126.9(7) . . ? O16 C14 C15 119.7(7) . . ? O9 C14 C15 113.4(6) . . ? O16 C14 K1 55.4(4) . 2_567 ? O9 C14 K1 145.5(5) . 2_567 ? C15 C14 K1 75.9(4) . 2_567 ? O14 C15 O11 126.8(7) . . ? O14 C15 C14 120.0(6) . . ? O11 C15 C14 113.1(6) . . ? O14 C15 K1 72.5(4) . 1_655 ? O11 C15 K1 57.2(3) . 1_655 ? C14 C15 K1 158.1(4) . 1_655 ? O14 C15 K1 55.2(4) . 2_567 ? O11 C15 K1 143.2(4) . 2_567 ? C14 C15 K1 77.5(4) . 2_567 ? K1 C15 K1 99.36(18) 1_655 2_567 ? N7 C16 C18 105.4(11) . . ? N7 C17 N8 105.4(13) . . ? C16 C18 N8 108.1(12) . . ? C1 N1 C2 104.7(6) . . ? C1 N1 Mo2 129.8(5) . . ? C2 N1 Mo2 125.4(4) . . ? C1 N2 C3 109.1(6) . . ? C4 N3 C5 105.9(6) . . ? C4 N3 Mo1 128.9(5) . . ? C5 N3 Mo1 125.2(4) . . ? C4 N4 C6 107.3(6) . . ? C7 N5 C8 106.3(6) . . ? C7 N5 Mo3 127.7(5) . . ? C8 N5 Mo3 125.9(4) . . ? C7 N6 C9 109.4(6) . . ? C17 N7 C16 111.7(12) . . ? C17 N8 C18 109.3(12) . . ? Mo2 O1 Mo1 76.00(15) . . ? Mo2 O1 Mo3 75.70(14) . . ? Mo1 O1 Mo3 75.73(16) . . ? Mo1 O2 Mo2 81.31(16) . . ? Mo1 O3 Mo3 81.75(19) . . ? C11 O4 Mo2 118.4(4) . . ? Mo2 O5 Mo3 81.53(16) . . ? C12 O6 Mo1 119.0(4) . . ? C12 O6 K1 97.2(4) . 1_655 ? Mo1 O6 K1 139.92(18) . 1_655 ? C10 O7 Mo2 118.5(4) . . ? C13 O8 Mo1 118.9(4) . . ? C14 O9 Mo3 119.1(4) . . ? C11 O10 K1 120.7(4) . . ? C15 O11 Mo3 119.1(4) . . ? C15 O11 K1 100.8(4) . 1_655 ? Mo3 O11 K1 134.94(18) . 1_655 ? C12 O12 K1 87.7(4) . 1_655 ? C10 O13 K1 118.6(4) . . ? C15 O14 K1 104.2(5) . 2_567 ? C15 O14 K1 86.2(4) . 1_655 ? K1 O14 K1 115.44(16) 2_567 1_655 ? C14 O16 K1 104.3(4) . 2_567 ? O10 K1 O6 74.66(15) . 1_455 ? O10 K1 O13 60.95(14) . . ? O6 K1 O13 104.26(15) 1_455 . ? O10 K1 O14 160.02(14) . 2_567 ? O6 K1 O14 95.40(15) 1_455 2_567 ? O13 K1 O14 139.02(14) . 2_567 ? O10 K1 O11 105.28(15) . 1_455 ? O6 K1 O11 67.39(12) 1_455 1_455 ? O13 K1 O11 69.62(15) . 1_455 ? O14 K1 O11 86.04(14) 2_567 1_455 ? O10 K1 O16 110.78(16) . 2_567 ? O6 K1 O16 116.99(16) 1_455 2_567 ? O13 K1 O16 134.30(18) . 2_567 ? O14 K1 O16 57.84(16) 2_567 2_567 ? O11 K1 O16 143.51(17) 1_455 2_567 ? O10 K1 O12 77.93(15) . 1_455 ? O6 K1 O12 45.63(13) 1_455 1_455 ? O13 K1 O12 135.84(16) . 1_455 ? O14 K1 O12 82.75(15) 2_567 1_455 ? O11 K1 O12 110.00(14) 1_455 1_455 ? O16 K1 O12 73.21(15) 2_567 1_455 ? O10 K1 O3W 77.1(4) . . ? O6 K1 O3W 151.1(4) 1_455 . ? O13 K1 O3W 66.3(3) . . ? O14 K1 O3W 109.5(4) 2_567 . ? O11 K1 O3W 127.2(3) 1_455 . ? O16 K1 O3W 68.1(3) 2_567 . ? O12 K1 O3W 121.6(3) 1_455 . ? O10 K1 O1W 119.8(2) . . ? O6 K1 O1W 157.87(19) 1_455 . ? O13 K1 O1W 73.0(2) . . ? O14 K1 O1W 75.4(2) 2_567 . ? O11 K1 O1W 91.62(18) 1_455 . ? O16 K1 O1W 75.48(19) 2_567 . ? O12 K1 O1W 148.06(19) 1_455 . ? O3W K1 O1W 48.8(4) . . ? O10 K1 C12 79.28(17) . 1_455 ? O6 K1 C12 23.95(14) 1_455 1_455 ? O13 K1 C12 124.94(17) . 1_455 ? O14 K1 C12 84.83(17) 2_567 1_455 ? O11 K1 C12 88.00(15) 1_455 1_455 ? O16 K1 C12 93.23(17) 2_567 1_455 ? O12 K1 C12 22.38(14) 1_455 1_455 ? O3W K1 C12 141.7(3) . 1_455 ? O1W K1 C12 160.2(2) . 1_455 ? O10 K1 O14 134.47(14) . 1_455 ? O6 K1 O14 106.17(13) 1_455 1_455 ? O13 K1 O14 75.46(14) . 1_455 ? O14 K1 O14 64.56(16) 2_567 1_455 ? O11 K1 O14 42.74(12) 1_455 1_455 ? O16 K1 O14 108.75(14) 2_567 1_455 ? O12 K1 O14 135.73(15) 1_455 1_455 ? O3W K1 O14 98.0(3) . 1_455 ? O1W K1 O14 51.70(19) . 1_455 ? C12 K1 O14 120.06(16) 1_455 1_455 ? O10 K1 C15 123.90(17) . 1_455 ? O6 K1 C15 85.56(15) 1_455 1_455 ? O13 K1 C15 74.79(16) . 1_455 ? O14 K1 C15 71.27(16) 2_567 1_455 ? O11 K1 C15 21.96(14) 1_455 1_455 ? O16 K1 C15 124.89(17) 2_567 1_455 ? O12 K1 C15 122.00(16) 1_455 1_455 ? O3W K1 C15 115.8(3) . 1_455 ? O1W K1 C15 72.5(2) . 1_455 ? C12 K1 C15 102.40(17) 1_455 1_455 ? O14 K1 C15 21.34(13) 1_455 1_455 ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 1.594 _refine_diff_density_min -1.275 _refine_diff_density_rms 0.185 # Attachment '8.cif' data_sad8 _database_code_depnum_ccdc_archive 'CCDC 891646' #TrackingRef '8.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'Oxomolybdenum(VI/V) imidazole hydrate' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H18 Mo3 N8 O9' _chemical_formula_weight 706.16 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' Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M P2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 8.2312(2) _cell_length_b 15.6958(4) _cell_length_c 8.7803(2) _cell_angle_alpha 90.00 _cell_angle_beta 99.098(2) _cell_angle_gamma 90.00 _cell_volume 1120.10(5) _cell_formula_units_Z 2 _cell_measurement_temperature 446(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.094 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 688 _exptl_absorpt_coefficient_mu 1.714 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7256 _exptl_absorpt_correction_T_max 0.9192 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 446(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6232 _diffrn_reflns_av_R_equivalents 0.0437 _diffrn_reflns_av_sigmaI/netI 0.0609 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 5 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.82 _diffrn_reflns_theta_max 27.00 _reflns_number_total 4075 _reflns_number_gt 3876 _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 ? _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. ; _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^)+(0.0620P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.03(4) _refine_ls_number_reflns 4075 _refine_ls_number_parameters 295 _refine_ls_number_restraints 28 _refine_ls_R_factor_all 0.0312 _refine_ls_R_factor_gt 0.0271 _refine_ls_wR_factor_ref 0.0700 _refine_ls_wR_factor_gt 0.0680 _refine_ls_goodness_of_fit_ref 0.741 _refine_ls_restrained_S_all 0.741 _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 0.12582(5) 0.23385(2) 0.42228(5) 0.01020(10) Uani 1 1 d . . . Mo2 Mo 0.30341(5) 0.04209(3) 0.53683(5) 0.01103(10) Uani 1 1 d . . . Mo3 Mo 0.22677(5) 0.15540(2) 0.19748(4) 0.00944(9) Uani 1 1 d . . . O1 O 0.3376(4) 0.2358(3) 0.3491(4) 0.0139(7) Uani 1 1 d . . . O2 O 0.3482(4) 0.0545(2) 0.3451(4) 0.0148(8) Uani 1 1 d . . . O3 O 0.0165(5) 0.3131(2) 0.3279(4) 0.0191(8) Uani 1 1 d . . . O4 O 0.0473(4) 0.1302(2) 0.3108(4) 0.0135(7) Uani 1 1 d . . . O5 O 0.2358(4) 0.1424(2) 0.6001(4) 0.0146(7) Uani 1 1 d . . . O6 O 0.4838(4) 0.0130(2) 0.6596(4) 0.0182(8) Uani 1 1 d . . . O7 O 0.1441(4) 0.2139(2) 0.0438(4) 0.0176(8) Uani 1 1 d . . . O8 O 0.1525(5) -0.0335(2) 0.5453(4) 0.0227(8) Uani 1 1 d . . . N1 N 0.4683(5) 0.1460(3) 0.1226(5) 0.0164(9) Uani 1 1 d . . . N2 N 0.2368(5) 0.3184(3) 0.6062(5) 0.0162(9) Uani 1 1 d . . . N3 N -0.0821(5) 0.2099(3) 0.5494(5) 0.0143(9) Uani 1 1 d . . . N4 N 0.1451(5) 0.0400(3) 0.0609(5) 0.0160(9) Uani 1 1 d . . . N5 N 0.7352(5) 0.1332(3) 0.1560(6) 0.0252(11) Uani 1 1 d . . . H5A H 0.8366 0.1368 0.1983 0.030 Uiso 1 1 calc R . . N7 N 0.3291(6) 0.3691(3) 0.8351(6) 0.0291(12) Uani 1 1 d . . . H7B H 0.3457 0.3750 0.9337 0.035 Uiso 1 1 calc R . . N8 N -0.2800(5) 0.1400(3) 0.6336(6) 0.0230(11) Uani 1 1 d . . . H8B H -0.3371 0.0986 0.6614 0.028 Uiso 1 1 calc R . . C13 C 0.0646(9) -0.0898(4) -0.0047(8) 0.0369(16) Uani 1 1 d U . . H13A H 0.0315 -0.1462 0.0001 0.044 Uiso 1 1 calc R . . N6 N 0.0791(6) -0.0452(3) -0.1361(6) 0.0269(11) Uani 1 1 d U . . H6B H 0.0613 -0.0641 -0.2291 0.032 Uiso 1 1 calc R . . C1 C 0.2381(7) 0.3080(4) 0.7555(7) 0.0228(12) Uani 1 1 d U . . H1A H 0.1837 0.2647 0.7993 0.027 Uiso 1 1 calc R . . C2 C 0.3903(7) 0.4196(4) 0.7332(8) 0.0301(15) Uani 1 1 d . . . H2A H 0.4591 0.4664 0.7564 0.036 Uiso 1 1 calc R . . C3 C 0.3328(8) 0.3893(4) 0.5919(7) 0.0273(13) Uani 1 1 d U . . H3B H 0.3542 0.4122 0.4994 0.033 Uiso 1 1 calc R . . C5 C -0.1397(6) 0.1329(4) 0.5767(6) 0.0185(11) Uani 1 1 d . . . H5B H -0.0893 0.0817 0.5587 0.022 Uiso 1 1 calc R . . C7 C 0.1062(8) -0.0383(4) 0.1136(7) 0.0309(14) Uani 1 1 d . . . H7C H 0.1087 -0.0528 0.2166 0.037 Uiso 1 1 calc R . . C8 C -0.1944(7) 0.2684(4) 0.5867(7) 0.0247(12) Uani 1 1 d . . . H8C H -0.1877 0.3273 0.5770 0.030 Uiso 1 1 calc R . . C9 C -0.3171(7) 0.2248(4) 0.6402(7) 0.0280(13) Uani 1 1 d . . . H9A H -0.4086 0.2482 0.6746 0.034 Uiso 1 1 calc R . . C11 C 0.1261(6) 0.0331(4) -0.0912(6) 0.0198(11) Uani 1 1 d . . . H11A H 0.1432 0.0772 -0.1576 0.024 Uiso 1 1 calc R . . C12 C 0.6065(6) 0.1600(4) 0.2169(6) 0.0220(11) Uani 1 1 d . . . H12A H 0.6132 0.1854 0.3134 0.026 Uiso 1 1 calc R . . C14 C 0.5137(7) 0.1087(5) -0.0063(7) 0.0323(15) Uani 1 1 d . . . H14A H 0.4420 0.0926 -0.0943 0.039 Uiso 1 1 calc R . . C15 C 0.6791(7) 0.0992(5) 0.0153(8) 0.0391(18) Uani 1 1 d . . . H15A H 0.7415 0.0744 -0.0524 0.047 Uiso 1 1 calc R . . O1W O 0.3933(9) 0.3795(4) 1.1534(6) 0.067(2) Uani 1 1 d D . . H1W1 H 0.464(9) 0.416(4) 1.194(10) 0.081 Uiso 1 1 d D . . H1W2 H 0.391(11) 0.338(4) 1.214(8) 0.081 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 0.01315(19) 0.00897(18) 0.00872(19) 0.00033(17) 0.00251(14) 0.00103(15) Mo2 0.0150(2) 0.00922(18) 0.00932(19) 0.00088(17) 0.00315(14) 0.00076(16) Mo3 0.01073(18) 0.01041(18) 0.00718(18) -0.00027(17) 0.00145(13) -0.00020(15) O1 0.0189(17) 0.0135(16) 0.0096(16) -0.0031(17) 0.0032(13) -0.0037(15) O2 0.0163(17) 0.0185(19) 0.0102(17) -0.0006(16) 0.0038(13) 0.0041(14) O3 0.0267(19) 0.0182(18) 0.0135(19) 0.0022(16) 0.0065(15) 0.0063(15) O4 0.0120(16) 0.0157(18) 0.0129(17) -0.0013(15) 0.0021(13) -0.0005(13) O5 0.0193(17) 0.0130(19) 0.0122(17) 0.0004(15) 0.0044(13) -0.0004(14) O6 0.0254(19) 0.0153(17) 0.0139(18) 0.0020(16) 0.0034(15) 0.0082(14) O7 0.0187(17) 0.021(2) 0.0126(17) 0.0047(16) 0.0019(13) 0.0028(14) O8 0.031(2) 0.0179(18) 0.021(2) -0.0029(18) 0.0083(16) -0.0080(17) N1 0.0122(19) 0.025(2) 0.011(2) 0.001(2) 0.0016(15) -0.0032(18) N2 0.024(2) 0.013(2) 0.013(2) 0.0001(18) 0.0079(17) -0.0052(18) N3 0.0132(19) 0.018(2) 0.013(2) -0.0027(18) 0.0043(16) 0.0013(16) N4 0.021(2) 0.017(2) 0.010(2) -0.003(2) 0.0039(16) -0.0088(19) N5 0.013(2) 0.043(3) 0.019(2) 0.001(2) 0.0008(17) -0.0011(19) N7 0.040(3) 0.029(3) 0.020(3) -0.006(2) 0.008(2) -0.010(2) N8 0.018(2) 0.031(3) 0.022(2) 0.008(2) 0.0078(18) 0.0001(19) C13 0.057(4) 0.021(3) 0.032(3) -0.004(3) 0.005(3) -0.020(3) N6 0.039(3) 0.023(2) 0.019(2) -0.014(2) 0.004(2) -0.012(2) C1 0.037(3) 0.017(3) 0.014(3) -0.007(2) 0.004(2) -0.010(2) C2 0.039(3) 0.025(3) 0.031(3) -0.010(3) 0.017(3) -0.020(3) C3 0.048(3) 0.018(3) 0.020(3) -0.003(2) 0.016(2) -0.015(3) C5 0.013(2) 0.024(3) 0.020(3) 0.005(2) 0.005(2) 0.0019(19) C7 0.055(4) 0.021(3) 0.017(3) -0.001(3) 0.007(3) -0.019(3) C8 0.023(3) 0.023(3) 0.029(3) -0.001(3) 0.008(2) 0.007(2) C9 0.023(3) 0.036(3) 0.028(3) -0.002(3) 0.013(2) 0.006(3) C11 0.025(3) 0.021(3) 0.014(2) 0.000(2) 0.007(2) -0.005(2) C12 0.019(2) 0.036(3) 0.012(2) -0.008(3) 0.0040(19) -0.002(2) C14 0.017(3) 0.067(5) 0.013(3) -0.011(3) 0.002(2) -0.002(3) C15 0.018(3) 0.071(5) 0.029(3) -0.013(4) 0.009(2) 0.004(3) O1W 0.144(6) 0.039(3) 0.018(3) -0.004(3) 0.009(3) -0.053(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 O3 1.676(4) . ? Mo1 O1 1.951(3) . ? Mo1 O4 1.955(3) . ? Mo1 N2 2.176(4) . ? Mo1 O5 2.207(3) . ? Mo1 N3 2.218(4) . ? Mo1 Mo3 2.5732(6) . ? Mo2 O8 1.728(4) . ? Mo2 O6 1.752(4) . ? Mo2 O5 1.788(3) . ? Mo2 O2 1.790(4) . ? Mo3 O7 1.684(4) . ? Mo3 O4 1.948(3) . ? Mo3 O1 1.953(4) . ? Mo3 O2 2.186(4) . ? Mo3 N1 2.195(4) . ? Mo3 N4 2.218(5) . ? N1 C12 1.315(7) . ? N1 C14 1.377(7) . ? N2 C1 1.320(7) . ? N2 C3 1.382(7) . ? N3 C5 1.333(7) . ? N3 C8 1.379(7) . ? N4 C11 1.324(6) . ? N4 C7 1.368(7) . ? N5 C12 1.328(7) . ? N5 C15 1.358(8) . ? N7 C1 1.343(7) . ? N7 C2 1.351(8) . ? N8 C5 1.334(6) . ? N8 C9 1.369(8) . ? C13 C7 1.318(9) . ? C13 N6 1.370(9) . ? N6 C11 1.330(7) . ? C2 C3 1.343(9) . ? C8 C9 1.364(8) . ? C14 C15 1.352(8) . ? 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 O3 Mo1 O1 105.26(17) . . ? O3 Mo1 O4 105.13(16) . . ? O1 Mo1 O4 95.16(15) . . ? O3 Mo1 N2 92.51(18) . . ? O1 Mo1 N2 86.72(16) . . ? O4 Mo1 N2 161.01(16) . . ? O3 Mo1 O5 163.91(15) . . ? O1 Mo1 O5 87.43(14) . . ? O4 Mo1 O5 83.06(13) . . ? N2 Mo1 O5 78.14(14) . . ? O3 Mo1 N3 88.74(17) . . ? O1 Mo1 N3 165.70(15) . . ? O4 Mo1 N3 83.72(15) . . ? N2 Mo1 N3 89.82(16) . . ? O5 Mo1 N3 78.28(14) . . ? O3 Mo1 Mo3 100.90(13) . . ? O1 Mo1 Mo3 48.79(10) . . ? O4 Mo1 Mo3 48.63(10) . . ? N2 Mo1 Mo3 135.43(12) . . ? O5 Mo1 Mo3 94.90(9) . . ? N3 Mo1 Mo3 132.32(11) . . ? O8 Mo2 O6 109.85(18) . . ? O8 Mo2 O5 109.30(17) . . ? O6 Mo2 O5 108.29(16) . . ? O8 Mo2 O2 111.81(17) . . ? O6 Mo2 O2 109.04(16) . . ? O5 Mo2 O2 108.48(17) . . ? O7 Mo3 O4 106.09(16) . . ? O7 Mo3 O1 106.26(17) . . ? O4 Mo3 O1 95.37(14) . . ? O7 Mo3 O2 163.53(16) . . ? O4 Mo3 O2 82.09(13) . . ? O1 Mo3 O2 86.77(15) . . ? O7 Mo3 N1 93.84(17) . . ? O4 Mo3 N1 159.25(16) . . ? O1 Mo3 N1 84.27(15) . . ? O2 Mo3 N1 77.17(15) . . ? O7 Mo3 N4 87.85(17) . . ? O4 Mo3 N4 85.45(15) . . ? O1 Mo3 N4 164.94(16) . . ? O2 Mo3 N4 78.44(15) . . ? N1 Mo3 N4 89.67(15) . . ? O7 Mo3 Mo1 102.43(13) . . ? O4 Mo3 Mo1 48.89(10) . . ? O1 Mo3 Mo1 48.74(10) . . ? O2 Mo3 Mo1 93.72(9) . . ? N1 Mo3 Mo1 132.81(11) . . ? N4 Mo3 Mo1 134.33(10) . . ? Mo1 O1 Mo3 82.47(13) . . ? Mo2 O2 Mo3 119.56(17) . . ? Mo3 O4 Mo1 82.49(13) . . ? Mo2 O5 Mo1 117.78(18) . . ? C12 N1 C14 105.5(4) . . ? C12 N1 Mo3 122.3(4) . . ? C14 N1 Mo3 130.6(4) . . ? C1 N2 C3 106.0(5) . . ? C1 N2 Mo1 126.7(4) . . ? C3 N2 Mo1 127.1(4) . . ? C5 N3 C8 106.9(4) . . ? C5 N3 Mo1 124.6(3) . . ? C8 N3 Mo1 127.3(4) . . ? C11 N4 C7 105.8(5) . . ? C11 N4 Mo3 126.1(4) . . ? C7 N4 Mo3 128.2(4) . . ? C12 N5 C15 108.2(4) . . ? C1 N7 C2 108.1(5) . . ? C5 N8 C9 108.0(5) . . ? C7 C13 N6 107.7(5) . . ? C11 N6 C13 106.4(5) . . ? N2 C1 N7 110.2(5) . . ? C3 C2 N7 106.8(5) . . ? C2 C3 N2 109.0(5) . . ? N3 C5 N8 110.2(5) . . ? C13 C7 N4 109.2(5) . . ? C9 C8 N3 108.0(5) . . ? C8 C9 N8 106.9(5) . . ? N4 C11 N6 110.9(5) . . ? N1 C12 N5 111.1(5) . . ? C15 C14 N1 109.3(5) . . ? C14 C15 N5 105.9(5) . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 0.460 _refine_diff_density_min -0.483 _refine_diff_density_rms 0.105