# Supplementary Material (ESI) for CrystEngComm # This journal is (c) The Royal Society of Chemistry 2011 data_global _journal_name_full CrystEngComm _journal_coden_cambridge 1350 _publ_contact_author ; 'Prugove\2sigma(I) _computing_data_collection 'CrysAlis CCD (Oxford Diffraction,2003)' _computing_cell_refinement 'CrysAlis RED (Oxford Diffraction,2003)' _computing_data_reduction 'CrysAlis RED (Oxford Diffraction,2003)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON98 (Spek, 1990)' _computing_publication_material 'SHELXL97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0285P)^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 5547 _refine_ls_number_parameters 358 _refine_ls_number_restraints 10 _refine_ls_R_factor_all 0.0225 _refine_ls_R_factor_gt 0.0180 _refine_ls_wR_factor_ref 0.0449 _refine_ls_wR_factor_gt 0.0441 _refine_ls_goodness_of_fit_ref 1.016 _refine_ls_restrained_S_all 1.019 _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 -0.240096(18) 0.015855(16) 0.293849(14) 0.01499(5) Uani 1 1 d . . . Mo2 Mo 0.274138(19) 0.367269(17) 0.039502(17) 0.02204(5) Uani 1 1 d . . . Mo3 Mo 0.433762(19) 0.666756(16) 0.002642(15) 0.01733(5) Uani 1 1 d . . . Mo4 Mo 0.59321(2) 0.555836(18) 0.195719(15) 0.02223(5) Uani 1 1 d . . . O1 O -0.07781(15) 0.01824(13) 0.21437(12) 0.0204(3) Uani 1 1 d . . . O2 O -0.30692(15) 0.09962(14) 0.40205(12) 0.0210(3) Uani 1 1 d . . . O3 O -0.36945(15) -0.01731(13) 0.17204(12) 0.0202(3) Uani 1 1 d . . . O4 O -0.27757(17) -0.12006(14) 0.34945(14) 0.0284(4) Uani 1 1 d . . . O5 O 0.37101(16) 0.25670(13) 0.02379(13) 0.0230(3) Uani 1 1 d . . . O6 O 0.10941(18) 0.26927(16) 0.06558(17) 0.0368(4) Uani 1 1 d . . . O7 O 0.39091(18) 0.43160(15) 0.18782(13) 0.0273(3) Uani 1 1 d . . . O8 O 0.26125(16) 0.52507(14) 0.03367(13) 0.0240(3) Uani 1 1 d . . . O9 O 0.5000 0.5000 0.0000 0.0144(4) Uani 1 2 d S . . O10 O 0.37237(16) 0.59201(14) -0.15388(12) 0.0235(3) Uani 1 1 d . . . O11 O 0.38171(16) 0.78590(14) 0.00405(13) 0.0232(3) Uani 1 1 d . . . O12 O 0.51460(17) 0.67357(14) 0.16143(12) 0.0239(3) Uani 1 1 d . . . O13 O 0.75658(16) 0.65029(14) 0.12833(13) 0.0270(3) Uani 1 1 d . . . O14 O 0.6607(2) 0.59423(17) 0.33732(14) 0.0414(5) Uani 1 1 d . . . N1 N -0.02950(17) 0.12446(15) 0.41680(14) 0.0164(3) Uani 1 1 d . . . N2 N 0.09556(18) 0.13234(16) 0.37634(15) 0.0190(4) Uani 1 1 d . . . N3 N 0.3775(2) 0.02190(17) 0.12007(15) 0.0229(4) Uani 1 1 d . . . H3 H 0.4423 0.0061 0.0918 0.027 Uiso 1 1 calc R . . N4 N -0.1465(2) 0.22586(17) 0.23718(15) 0.0231(4) Uani 1 1 d . . . C1 C 0.0574(2) 0.07315(18) 0.27237(17) 0.0171(4) Uani 1 1 d . . . C2 C 0.1718(2) 0.06206(19) 0.21530(17) 0.0170(4) Uani 1 1 d . . . C3 C 0.1337(2) -0.01437(19) 0.10933(17) 0.0191(4) Uani 1 1 d . . . H3A H 0.0374 -0.0520 0.0705 0.023 Uiso 1 1 calc R . . C4 C 0.2402(2) -0.0331(2) 0.06337(18) 0.0217(4) Uani 1 1 d . . . H4 H 0.2166 -0.0839 -0.0070 0.026 Uiso 1 1 calc R . . C5 C 0.4196(2) 0.1009(2) 0.21934(19) 0.0238(5) Uani 1 1 d . . . H5 H 0.5175 0.1402 0.2544 0.029 Uiso 1 1 calc R . . C6 C 0.3176(2) 0.1231(2) 0.26860(19) 0.0220(4) Uani 1 1 d . . . H6 H 0.3455 0.1784 0.3369 0.026 Uiso 1 1 calc R . . C7 C -0.0087(2) 0.17512(18) 0.52172(17) 0.0175(4) Uani 1 1 d . . . H7 H 0.0857 0.2108 0.5644 0.021 Uiso 1 1 calc R . . C8 C -0.1245(2) 0.17916(18) 0.57622(17) 0.0170(4) Uani 1 1 d . . . C9 C -0.2674(2) 0.14252(19) 0.51608(17) 0.0179(4) Uani 1 1 d . . . C10 C -0.3724(2) 0.1539(2) 0.57339(19) 0.0228(4) Uani 1 1 d . . . H10 H -0.4668 0.1292 0.5336 0.027 Uiso 1 1 calc R . . C11 C -0.3369(2) 0.2015(2) 0.68908(19) 0.0245(5) Uani 1 1 d . . . H11 H -0.4076 0.2091 0.7267 0.029 Uiso 1 1 calc R . . C12 C -0.1962(2) 0.23824(19) 0.74975(18) 0.0234(5) Uani 1 1 d . . . H12 H -0.1730 0.2700 0.8277 0.028 Uiso 1 1 calc R . . C13 C -0.0915(2) 0.22754(19) 0.69413(18) 0.0205(4) Uani 1 1 d . . . H13 H 0.0025 0.2526 0.7350 0.025 Uiso 1 1 calc R . . C14 C -0.0978(2) 0.3250(2) 0.21474(19) 0.0235(5) Uani 1 1 d . . . C15 C -0.0321(3) 0.4535(2) 0.1869(3) 0.0392(6) Uani 1 1 d . . . H15A H -0.0256 0.5120 0.2507 0.059 Uiso 1 1 calc R . . H15B H -0.0914 0.4607 0.1200 0.059 Uiso 1 1 calc R . . H15C H 0.0640 0.4728 0.1715 0.059 Uiso 1 1 calc R . . N5 N 0.0888(5) 0.5189(5) 0.5211(5) 0.0563(10) Uiso 0.50 1 d PD . 1 C16 C 0.1744(6) 0.5066(6) 0.4773(5) 0.0563(10) Uiso 0.50 1 d PD A 1 C17 C 0.2798(7) 0.4891(7) 0.4179(7) 0.0563(10) Uiso 0.50 1 d PD A 1 H17A H 0.2638 0.4020 0.4131 0.084 Uiso 0.50 1 calc PR A 1 H17B H 0.3765 0.5421 0.4595 0.084 Uiso 0.50 1 calc PR A 1 H17C H 0.2694 0.5113 0.3417 0.084 Uiso 0.50 1 calc PR A 1 N5 N 0.4699(8) 0.6486(7) 0.5408(7) 0.0432(17) Uiso 0.262(3) 1 d PD B 2 C16 C 0.3719(9) 0.5658(9) 0.4878(9) 0.0432(17) Uiso 0.262(3) 1 d PD B 2 C17 C 0.2484(10) 0.4620(10) 0.4171(11) 0.0432(17) Uiso 0.262(3) 1 d PD B 2 H17D H 0.1598 0.4644 0.4323 0.065 Uiso 0.262(3) 1 calc PR B 2 H17E H 0.2491 0.3834 0.4343 0.065 Uiso 0.262(3) 1 calc PR B 2 H17F H 0.2539 0.4689 0.3373 0.065 Uiso 0.262(3) 1 calc PR B 2 N5 N 0.3861 0.6574 0.5835 0.051(2) Uiso 0.238(3) 1 d PD C 3 C16 C 0.3211 0.5735 0.5145 0.051(2) Uiso 0.238(3) 1 d PD C 3 C17 C 0.2566 0.4699 0.4198 0.051(2) Uiso 0.238(3) 1 d PD C 3 H17G H 0.1542 0.4239 0.4201 0.076 Uiso 0.238(3) 1 calc PR C 3 H17H H 0.3033 0.4142 0.4285 0.076 Uiso 0.238(3) 1 calc PR C 3 H17I H 0.2697 0.5033 0.3481 0.076 Uiso 0.238(3) 1 calc PR C 3 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 0.01164(9) 0.01680(9) 0.01601(9) -0.00047(6) 0.00209(7) 0.00617(7) Mo2 0.01603(9) 0.01866(10) 0.03229(11) 0.00407(7) 0.00792(8) 0.00717(7) Mo3 0.01885(9) 0.01621(9) 0.01929(9) -0.00075(7) 0.00177(7) 0.01082(7) Mo4 0.02999(11) 0.02501(10) 0.01358(9) -0.00347(7) -0.00267(8) 0.01658(8) O1 0.0151(7) 0.0256(8) 0.0198(7) -0.0060(6) 0.0014(6) 0.0102(6) O2 0.0159(7) 0.0301(8) 0.0177(7) -0.0023(6) 0.0032(6) 0.0113(6) O3 0.0151(7) 0.0250(8) 0.0201(8) -0.0024(6) 0.0018(6) 0.0093(6) O4 0.0262(8) 0.0231(8) 0.0318(9) 0.0056(6) 0.0004(7) 0.0078(7) O5 0.0215(8) 0.0148(7) 0.0328(9) 0.0030(6) 0.0055(7) 0.0079(6) O6 0.0228(9) 0.0271(9) 0.0639(12) 0.0087(8) 0.0191(9) 0.0102(7) O7 0.0355(9) 0.0290(8) 0.0222(8) 0.0056(6) 0.0118(7) 0.0164(7) O8 0.0193(8) 0.0243(8) 0.0329(9) 0.0030(6) 0.0079(7) 0.0130(6) O9 0.0133(9) 0.0148(9) 0.0147(10) -0.0020(7) 0.0000(8) 0.0070(8) O10 0.0280(8) 0.0262(8) 0.0184(8) -0.0014(6) -0.0027(6) 0.0166(7) O11 0.0236(8) 0.0219(8) 0.0265(8) -0.0010(6) 0.0005(7) 0.0140(6) O12 0.0334(9) 0.0233(8) 0.0181(7) -0.0048(6) 0.0009(7) 0.0176(7) O13 0.0192(8) 0.0234(8) 0.0317(9) -0.0050(6) -0.0077(7) 0.0077(6) O14 0.0681(13) 0.0408(10) 0.0197(9) -0.0068(7) -0.0106(8) 0.0351(10) N1 0.0129(8) 0.0203(9) 0.0177(9) 0.0004(7) 0.0036(7) 0.0090(7) N2 0.0127(8) 0.0266(9) 0.0192(9) -0.0002(7) 0.0034(7) 0.0104(7) N3 0.0245(10) 0.0319(10) 0.0246(10) 0.0107(8) 0.0140(8) 0.0201(8) N4 0.0237(10) 0.0230(10) 0.0222(10) 0.0014(7) 0.0025(8) 0.0105(8) C1 0.0142(10) 0.0184(10) 0.0207(10) 0.0019(8) 0.0035(8) 0.0091(8) C2 0.0190(10) 0.0192(10) 0.0181(10) 0.0048(8) 0.0051(8) 0.0125(8) C3 0.0220(11) 0.0216(10) 0.0185(10) 0.0044(8) 0.0044(9) 0.0136(9) C4 0.0292(12) 0.0269(11) 0.0169(10) 0.0063(8) 0.0083(9) 0.0181(10) C5 0.0172(11) 0.0306(12) 0.0276(12) 0.0063(9) 0.0053(9) 0.0136(9) C6 0.0184(10) 0.0267(11) 0.0231(11) 0.0003(9) 0.0025(9) 0.0127(9) C7 0.0142(10) 0.0186(10) 0.0182(10) -0.0008(8) 0.0008(8) 0.0065(8) C8 0.0193(10) 0.0149(9) 0.0176(10) 0.0020(7) 0.0054(8) 0.0075(8) C9 0.0189(10) 0.0172(10) 0.0176(10) 0.0005(8) 0.0055(8) 0.0073(8) C10 0.0198(11) 0.0204(10) 0.0277(12) -0.0004(8) 0.0094(9) 0.0074(9) C11 0.0264(12) 0.0218(11) 0.0264(12) 0.0007(9) 0.0154(10) 0.0085(9) C12 0.0318(12) 0.0185(10) 0.0177(11) 0.0001(8) 0.0096(9) 0.0076(9) C13 0.0213(11) 0.0188(10) 0.0183(10) 0.0008(8) 0.0032(9) 0.0061(8) C14 0.0186(11) 0.0249(12) 0.0267(12) 0.0014(9) 0.0009(9) 0.0104(9) C15 0.0263(13) 0.0249(12) 0.0653(19) 0.0157(12) 0.0038(12) 0.0098(10) _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 1.6803(15) . ? Mo1 O3 1.7192(14) . ? Mo1 O2 1.9227(13) . ? Mo1 O1 2.0094(13) . ? Mo1 N1 2.2343(17) . ? Mo1 N4 2.4226(18) . ? Mo2 O6 1.6848(16) . ? Mo2 O7 1.8902(16) . ? Mo2 O8 1.9140(14) . ? Mo2 O5 1.9458(14) . ? Mo2 O13 1.9503(16) 2_665 ? Mo2 O9 2.3215(2) . ? Mo3 O11 1.6894(14) . ? Mo3 O10 1.8957(14) . ? Mo3 O5 1.9015(15) 2_665 ? Mo3 O12 1.9289(14) . ? Mo3 O8 1.9581(15) . ? Mo3 O9 2.32034(18) . ? Mo4 O14 1.6758(16) . ? Mo4 O13 1.8986(16) . ? Mo4 O12 1.9052(14) . ? Mo4 O10 1.9525(14) 2_665 ? Mo4 O7 1.9594(16) . ? Mo4 O9 2.3173(2) . ? O1 C1 1.319(2) . ? O2 C9 1.351(2) . ? O5 Mo3 1.9015(14) 2_665 ? O9 Mo4 2.3173(2) 2_665 ? O9 Mo3 2.32034(18) 2_665 ? O9 Mo2 2.3215(2) 2_665 ? O10 Mo4 1.9525(14) 2_665 ? O13 Mo2 1.9503(16) 2_665 ? N1 C7 1.289(2) . ? N1 N2 1.397(2) . ? N2 C1 1.293(3) . ? N3 C4 1.331(3) . ? N3 C5 1.343(3) . ? N4 C14 1.125(3) . ? C1 C2 1.475(3) . ? C2 C6 1.390(3) . ? C2 C3 1.396(3) . ? C3 C4 1.370(3) . ? C5 C6 1.367(3) . ? C7 C8 1.441(3) . ? C8 C9 1.408(3) . ? C8 C13 1.409(3) . ? C9 C10 1.392(3) . ? C10 C11 1.381(3) . ? C11 C12 1.391(3) . ? C12 C13 1.376(3) . ? C14 C15 1.456(3) . ? N5 C16 1.1303(18) . ? N5 N5 1.674(10) 2_566 ? C16 C17 1.4391(19) . ? N5 C16 1.1300(19) . ? C16 C17 1.4392(19) . ? N5 C16 1.1293 . ? C16 C17 1.4526 . ? 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 107.25(7) . . ? O4 Mo1 O2 99.50(7) . . ? O3 Mo1 O2 101.55(6) . . ? O4 Mo1 O1 98.47(7) . . ? O3 Mo1 O1 97.28(6) . . ? O2 Mo1 O1 148.70(6) . . ? O4 Mo1 N1 94.32(7) . . ? O3 Mo1 N1 157.35(6) . . ? O2 Mo1 N1 81.06(6) . . ? O1 Mo1 N1 72.21(6) . . ? O4 Mo1 N4 170.06(7) . . ? O3 Mo1 N4 82.50(6) . . ? O2 Mo1 N4 79.96(6) . . ? O1 Mo1 N4 77.97(6) . . ? N1 Mo1 N4 75.77(6) . . ? O6 Mo2 O7 103.90(8) . . ? O6 Mo2 O8 103.35(7) . . ? O7 Mo2 O8 89.03(7) . . ? O6 Mo2 O5 103.19(7) . . ? O7 Mo2 O5 87.29(7) . . ? O8 Mo2 O5 153.32(6) . . ? O6 Mo2 O13 102.95(8) . 2_665 ? O7 Mo2 O13 153.10(7) . 2_665 ? O8 Mo2 O13 86.30(7) . 2_665 ? O5 Mo2 O13 85.15(6) . 2_665 ? O6 Mo2 O9 178.87(7) . . ? O7 Mo2 O9 77.12(5) . . ? O8 Mo2 O9 77.10(4) . . ? O5 Mo2 O9 76.31(4) . . ? O13 Mo2 O9 76.01(4) 2_665 . ? O11 Mo3 O10 102.69(7) . . ? O11 Mo3 O5 104.02(7) . 2_665 ? O10 Mo3 O5 88.84(7) . 2_665 ? O11 Mo3 O12 104.33(7) . . ? O10 Mo3 O12 152.83(6) . . ? O5 Mo3 O12 87.31(6) 2_665 . ? O11 Mo3 O8 102.52(7) . . ? O10 Mo3 O8 86.85(7) . . ? O5 Mo3 O8 153.42(6) 2_665 . ? O12 Mo3 O8 84.69(7) . . ? O11 Mo3 O9 178.76(5) . . ? O10 Mo3 O9 76.87(4) . . ? O5 Mo3 O9 77.15(4) 2_665 . ? O12 Mo3 O9 76.05(4) . . ? O8 Mo3 O9 76.32(4) . . ? O14 Mo4 O13 103.13(9) . . ? O14 Mo4 O12 104.22(7) . . ? O13 Mo4 O12 89.57(7) . . ? O14 Mo4 O10 103.31(7) . 2_665 ? O13 Mo4 O10 86.87(7) . 2_665 ? O12 Mo4 O10 152.34(6) . 2_665 ? O14 Mo4 O7 103.82(9) . . ? O13 Mo4 O7 152.93(6) . . ? O12 Mo4 O7 86.32(7) . . ? O10 Mo4 O7 84.52(6) 2_665 . ? O14 Mo4 O9 179.19(6) . . ? O13 Mo4 O9 77.06(5) . . ? O12 Mo4 O9 76.56(4) . . ? O10 Mo4 O9 75.91(4) 2_665 . ? O7 Mo4 O9 75.96(4) . . ? C1 O1 Mo1 118.72(12) . . ? C9 O2 Mo1 135.19(13) . . ? Mo3 O5 Mo2 116.69(7) 2_665 . ? Mo2 O7 Mo4 116.86(7) . . ? Mo2 O8 Mo3 116.32(7) . . ? Mo4 O9 Mo4 180.0 2_665 . ? Mo4 O9 Mo3 89.875(7) 2_665 2_665 ? Mo4 O9 Mo3 90.125(7) . 2_665 ? Mo4 O9 Mo3 90.125(7) 2_665 . ? Mo4 O9 Mo3 89.875(7) . . ? Mo3 O9 Mo3 180.0 2_665 . ? Mo4 O9 Mo2 90.004(8) 2_665 . ? Mo4 O9 Mo2 89.996(8) . . ? Mo3 O9 Mo2 89.746(7) 2_665 . ? Mo3 O9 Mo2 90.254(7) . . ? Mo4 O9 Mo2 89.996(8) 2_665 2_665 ? Mo4 O9 Mo2 90.004(8) . 2_665 ? Mo3 O9 Mo2 90.254(7) 2_665 2_665 ? Mo3 O9 Mo2 89.746(7) . 2_665 ? Mo2 O9 Mo2 180.000(12) . 2_665 ? Mo3 O10 Mo4 117.09(7) . 2_665 ? Mo4 O12 Mo3 117.38(7) . . ? Mo4 O13 Mo2 116.91(7) . 2_665 ? C7 N1 N2 115.77(16) . . ? C7 N1 Mo1 128.70(13) . . ? N2 N1 Mo1 115.43(11) . . ? C1 N2 N1 108.81(16) . . ? C4 N3 C5 123.01(18) . . ? C14 N4 Mo1 176.90(18) . . ? N2 C1 O1 124.73(17) . . ? N2 C1 C2 118.04(18) . . ? O1 C1 C2 117.20(17) . . ? C6 C2 C3 119.40(18) . . ? C6 C2 C1 120.43(18) . . ? C3 C2 C1 120.12(18) . . ? C4 C3 C2 119.1(2) . . ? N3 C4 C3 119.6(2) . . ? N3 C5 C6 119.6(2) . . ? C5 C6 C2 119.1(2) . . ? N1 C7 C8 123.20(18) . . ? C9 C8 C13 118.46(18) . . ? C9 C8 C7 123.11(18) . . ? C13 C8 C7 118.36(18) . . ? O2 C9 C10 117.72(19) . . ? O2 C9 C8 122.27(17) . . ? C10 C9 C8 119.98(19) . . ? C11 C10 C9 120.3(2) . . ? C10 C11 C12 120.4(2) . . ? C13 C12 C11 119.83(19) . . ? C12 C13 C8 121.0(2) . . ? N4 C14 C15 179.0(3) . . ? C16 N5 N5 133.7(7) . 2_566 ? N5 C16 C17 178.1(8) . . ? N5 C16 C17 178.2(13) . . ? N5 C16 C17 171.960(1) . . ? _diffrn_measured_fraction_theta_max 0.952 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.952 _refine_diff_density_max 0.484 _refine_diff_density_min -0.579 _refine_diff_density_rms 0.073 data_1b _database_code_depnum_ccdc_archive 'CCDC 802259' #TrackingRef '1b.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; bis (acetone cis-dioxo(2-oxobenzaldehyde isonicotinylhydrazonato- O, N, O) molybdenum(VI)) hexamolybdate acetone solvate (1/1) ; _chemical_name_common ; bis (acetone cis-dioxo(2-oxobenzaldehyde isonicotinylhydrazonato-O, N, O) molybdenum(VI)) hexamolybdate acetone solvate (1/1) ; _chemical_melting_point ? _chemical_formula_moiety '2(C16 H16 Mo N3 O5), Mo6 O19, C3 H6 O' _chemical_formula_sum 'C35 H38 Mo8 N6 O30' _chemical_formula_weight 1790.23 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' Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.5322(3) _cell_length_b 11.4529(3) _cell_length_c 11.6939(3) _cell_angle_alpha 92.916(2) _cell_angle_beta 95.266(2) _cell_angle_gamma 114.822(3) _cell_volume 1268.60(6) _cell_formula_units_Z 1 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 15 _cell_measurement_theta_max 25 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.48 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.321 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 855 _exptl_absorpt_coefficient_mu 2.010 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.86584 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'Xcalibur CCD' _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16488 _diffrn_reflns_av_R_equivalents 0.0165 _diffrn_reflns_av_sigmaI/netI 0.0199 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 4.15 _diffrn_reflns_theta_max 27.49 _reflns_number_total 5570 _reflns_number_gt 4859 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD (Oxford Diffraction,2003)' _computing_cell_refinement 'CrysAlis RED (Oxford Diffraction,2003)' _computing_data_reduction 'CrysAlis RED (Oxford Diffraction,2003)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON98 (Spek, 1990)' _computing_publication_material 'SHELXL97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0339P)^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 5570 _refine_ls_number_parameters 378 _refine_ls_number_restraints 20 _refine_ls_R_factor_all 0.0202 _refine_ls_R_factor_gt 0.0158 _refine_ls_wR_factor_ref 0.0401 _refine_ls_wR_factor_gt 0.0394 _refine_ls_goodness_of_fit_ref 0.943 _refine_ls_restrained_S_all 0.942 _refine_ls_shift/su_max 0.002 _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 0.756549(16) 0.480215(15) 0.210072(13) 0.01133(4) Uani 1 1 d . . . Mo2 Mo 0.056154(17) 0.825252(15) 0.504983(14) 0.01276(4) Uani 1 1 d . . . Mo3 Mo -0.165951(17) 0.895785(16) 0.340441(14) 0.01513(4) Uani 1 1 d . . . Mo4 Mo 0.170821(17) 1.094244(16) 0.379077(14) 0.01489(4) Uani 1 1 d . . . O1 O 0.59909(13) 0.49448(13) 0.28668(11) 0.0154(3) Uani 1 1 d . . . O2 O 0.81554(13) 0.37872(13) 0.10884(11) 0.0157(3) Uani 1 1 d . . . O3 O 0.87876(13) 0.51021(13) 0.32766(11) 0.0156(3) Uani 1 1 d . . . O4 O 0.80817(14) 0.61579(13) 0.14192(12) 0.0193(3) Uani 1 1 d . . . O5 O 0.64826(14) 0.28187(13) 0.29720(11) 0.0180(3) Uani 1 1 d . . . O6 O -0.08602(14) 0.77737(13) 0.37362(12) 0.0180(3) Uani 1 1 d . . . O7 O 0.0000 1.0000 0.5000 0.0107(4) Uani 1 2 d S . . O8 O -0.27485(13) 0.84522(13) 0.46047(12) 0.0187(3) Uani 1 1 d . . . O9 O -0.10419(14) 0.77980(13) 0.59526(12) 0.0196(3) Uani 1 1 d . . . O10 O 0.09340(14) 0.69566(13) 0.51126(12) 0.0181(3) Uani 1 1 d . . . O11 O 0.18801(13) 0.93367(13) 0.41544(11) 0.0156(3) Uani 1 1 d . . . O12 O -0.28146(15) 0.82585(14) 0.22119(12) 0.0248(3) Uani 1 1 d . . . O13 O 0.16613(13) 0.93559(13) 0.64059(11) 0.0160(3) Uani 1 1 d . . . O14 O 0.01513(14) 0.99209(14) 0.27506(11) 0.0194(3) Uani 1 1 d . . . O15 O 0.30129(15) 1.16244(15) 0.29743(13) 0.0248(3) Uani 1 1 d . . . N1 N 0.55766(15) 0.37985(15) 0.08843(13) 0.0123(3) Uani 1 1 d . . . N2 N 0.43915(16) 0.38913(15) 0.12428(13) 0.0145(3) Uani 1 1 d . . . N3 N 0.15287(17) 0.50515(16) 0.37711(14) 0.0176(3) Uani 1 1 d . . . H3 H 0.0858 0.5183 0.4072 0.021 Uiso 1 1 calc R . . C1 C 0.47279(19) 0.44937(18) 0.22677(16) 0.0129(4) Uani 1 1 d . . . C2 C 0.36044(19) 0.46843(18) 0.28169(16) 0.0136(4) Uani 1 1 d . . . C3 C 0.3894(2) 0.53797(19) 0.38933(16) 0.0167(4) Uani 1 1 d . . . H31 H 0.4820 0.5734 0.4298 0.020 Uiso 1 1 calc R . . C4 C 0.2820(2) 0.55495(19) 0.43673(17) 0.0176(4) Uani 1 1 d . . . H4 H 0.2995 0.6013 0.5105 0.021 Uiso 1 1 calc R . . C5 C 0.1209(2) 0.43642(19) 0.27404(17) 0.0182(4) Uani 1 1 d . . . H5 H 0.0272 0.4017 0.2357 0.022 Uiso 1 1 calc R . . C6 C 0.2237(2) 0.41630(19) 0.22386(17) 0.0165(4) Uani 1 1 d . . . H6 H 0.2021 0.3676 0.1508 0.020 Uiso 1 1 calc R . . C7 C 0.54112(19) 0.32702(18) -0.01529(16) 0.0140(4) Uani 1 1 d . . . H7 H 0.4519 0.2993 -0.0602 0.017 Uiso 1 1 calc R . . C8 C 0.65131(19) 0.30792(17) -0.06632(16) 0.0132(4) Uani 1 1 d . . . C9 C 0.7841(2) 0.33704(18) -0.00448(16) 0.0141(4) Uani 1 1 d . . . C10 C 0.8863(2) 0.3166(2) -0.06001(17) 0.0193(4) Uani 1 1 d . . . H10 H 0.9764 0.3377 -0.0189 0.023 Uiso 1 1 calc R . . C11 C 0.8567(2) 0.26573(19) -0.17452(17) 0.0204(4) Uani 1 1 d . . . H11 H 0.9262 0.2510 -0.2112 0.024 Uiso 1 1 calc R . . C12 C 0.7251(2) 0.23603(18) -0.23618(17) 0.0179(4) Uani 1 1 d . . . H12 H 0.7050 0.2014 -0.3147 0.021 Uiso 1 1 calc R . . C13 C 0.6250(2) 0.25716(18) -0.18245(16) 0.0151(4) Uani 1 1 d . . . H13 H 0.5358 0.2370 -0.2248 0.018 Uiso 1 1 calc R . . C14 C 0.5974(2) 0.1636(2) 0.28422(18) 0.0192(4) Uani 1 1 d . . . C15 C 0.5443(2) 0.0876(2) 0.38346(19) 0.0239(5) Uani 1 1 d . . . H15A H 0.4435 0.0312 0.3645 0.036 Uiso 1 1 calc R . . H15B H 0.5589 0.1469 0.4519 0.036 Uiso 1 1 calc R . . H15C H 0.5958 0.0348 0.3991 0.036 Uiso 1 1 calc R . . C16 C 0.5857(3) 0.0902(2) 0.1723(2) 0.0374(6) Uani 1 1 d . . . H16A H 0.6284 0.1508 0.1157 0.056 Uiso 1 1 calc R . . H16B H 0.4860 0.0366 0.1444 0.056 Uiso 1 1 calc R . . H16C H 0.6349 0.0347 0.1828 0.056 Uiso 1 1 calc R . . O16 O 0.9768(5) 0.1536(4) 0.0854(4) 0.0848(18) Uani 0.50 1 d PD A -1 C17 C 0.9820(6) 0.0609(6) 0.0398(5) 0.060(2) Uani 0.50 1 d PDU A -1 C18 C 0.8540(10) -0.0576(9) -0.0038(13) 0.085(4) Uani 0.50 1 d PDU A -1 H18A H 0.7701 -0.0447 0.0097 0.128 Uiso 0.50 1 calc PR A -1 H18B H 0.8544 -0.1303 0.0368 0.128 Uiso 0.50 1 calc PR A -1 H18C H 0.8526 -0.0765 -0.0867 0.128 Uiso 0.50 1 calc PR A -1 C19 C 1.1172(9) 0.0544(12) 0.0260(14) 0.092(5) Uani 0.50 1 d PD A -1 H19A H 1.1956 0.1366 0.0576 0.138 Uiso 0.50 1 calc PR A -1 H19B H 1.1226 0.0383 -0.0562 0.138 Uiso 0.50 1 calc PR A -1 H19C H 1.1229 -0.0159 0.0673 0.138 Uiso 0.50 1 calc PR A -1 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 0.00882(8) 0.01367(8) 0.01138(8) -0.00185(6) 0.00100(6) 0.00506(6) Mo2 0.01284(8) 0.01301(8) 0.01496(8) -0.00038(6) 0.00146(6) 0.00822(6) Mo3 0.01364(8) 0.01851(9) 0.01311(8) -0.00519(6) -0.00422(6) 0.00865(7) Mo4 0.01300(8) 0.01869(9) 0.01662(9) 0.00445(7) 0.00611(7) 0.00916(7) O1 0.0114(6) 0.0208(7) 0.0149(7) -0.0024(5) 0.0014(5) 0.0082(6) O2 0.0126(6) 0.0217(7) 0.0137(7) -0.0036(5) 0.0003(5) 0.0091(6) O3 0.0129(6) 0.0167(7) 0.0170(7) -0.0033(5) -0.0003(5) 0.0069(5) O4 0.0178(7) 0.0196(7) 0.0207(7) 0.0023(6) 0.0038(6) 0.0078(6) O5 0.0168(7) 0.0166(7) 0.0189(7) 0.0031(6) 0.0022(6) 0.0055(6) O6 0.0172(7) 0.0166(7) 0.0201(7) -0.0065(6) -0.0029(6) 0.0091(6) O7 0.0101(8) 0.0132(9) 0.0096(8) -0.0015(7) -0.0005(7) 0.0063(7) O8 0.0109(6) 0.0204(7) 0.0223(7) -0.0032(6) -0.0001(6) 0.0055(6) O9 0.0188(7) 0.0185(7) 0.0260(8) 0.0074(6) 0.0093(6) 0.0105(6) O10 0.0183(7) 0.0178(7) 0.0215(7) -0.0011(6) 0.0001(6) 0.0116(6) O11 0.0151(7) 0.0202(7) 0.0154(7) -0.0003(5) 0.0036(5) 0.0112(6) O12 0.0221(8) 0.0326(9) 0.0201(8) -0.0117(6) -0.0094(6) 0.0162(7) O13 0.0148(7) 0.0223(7) 0.0140(7) -0.0010(5) -0.0015(5) 0.0121(6) O14 0.0202(7) 0.0309(8) 0.0119(7) 0.0005(6) 0.0024(6) 0.0158(6) O15 0.0211(8) 0.0317(8) 0.0294(8) 0.0135(7) 0.0128(6) 0.0158(7) N1 0.0090(7) 0.0159(8) 0.0138(8) 0.0011(6) 0.0031(6) 0.0067(6) N2 0.0114(7) 0.0210(9) 0.0142(8) 0.0007(7) 0.0034(6) 0.0096(7) N3 0.0187(8) 0.0192(8) 0.0224(9) 0.0063(7) 0.0107(7) 0.0133(7) C1 0.0116(9) 0.0139(9) 0.0152(9) 0.0032(7) 0.0029(7) 0.0070(7) C2 0.0152(9) 0.0151(9) 0.0145(9) 0.0048(7) 0.0044(7) 0.0095(8) C3 0.0189(10) 0.0218(10) 0.0135(9) 0.0025(8) 0.0021(8) 0.0126(9) C4 0.0242(10) 0.0198(10) 0.0136(9) 0.0039(8) 0.0071(8) 0.0130(9) C5 0.0141(9) 0.0198(10) 0.0227(10) 0.0033(8) 0.0028(8) 0.0088(8) C6 0.0162(9) 0.0191(10) 0.0160(9) 0.0008(8) 0.0025(8) 0.0093(8) C7 0.0125(9) 0.0149(9) 0.0135(9) 0.0007(7) 0.0007(7) 0.0050(8) C8 0.0140(9) 0.0113(9) 0.0140(9) 0.0016(7) 0.0046(7) 0.0043(7) C9 0.0148(9) 0.0130(9) 0.0136(9) -0.0014(7) 0.0036(7) 0.0049(7) C10 0.0137(9) 0.0244(11) 0.0198(10) -0.0032(8) 0.0029(8) 0.0085(8) C11 0.0189(10) 0.0209(10) 0.0219(11) -0.0019(8) 0.0097(8) 0.0082(8) C12 0.0212(10) 0.0149(9) 0.0146(9) -0.0019(7) 0.0057(8) 0.0046(8) C13 0.0141(9) 0.0142(9) 0.0146(9) 0.0005(7) 0.0016(7) 0.0038(8) C14 0.0147(10) 0.0209(10) 0.0226(10) 0.0048(8) -0.0012(8) 0.0087(8) C15 0.0186(10) 0.0245(11) 0.0294(12) 0.0098(9) 0.0044(9) 0.0087(9) C16 0.0597(17) 0.0212(12) 0.0259(12) 0.0007(9) -0.0010(12) 0.0136(12) O16 0.115(4) 0.044(3) 0.074(3) 0.012(3) -0.042(3) 0.023(3) C17 0.086(5) 0.037(3) 0.027(3) 0.015(3) -0.011(3) -0.001(3) C18 0.089(7) 0.079(7) 0.018(6) 0.000(4) 0.006(5) -0.031(5) C19 0.121(10) 0.087(8) 0.023(7) 0.013(4) 0.027(5) -0.004(7) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 1.6848(14) . ? Mo1 O3 1.7092(13) . ? Mo1 O2 1.9339(13) . ? Mo1 O1 2.0161(12) . ? Mo1 N1 2.2355(15) . ? Mo1 O5 2.4027(13) . ? Mo2 O10 1.6902(13) . ? Mo2 O11 1.8757(13) . ? Mo2 O13 1.9191(13) . ? Mo2 O6 1.9249(13) . ? Mo2 O9 1.9704(13) . ? Mo2 O7 2.31474(17) . ? Mo3 O12 1.6802(14) . ? Mo3 O8 1.8551(14) . ? Mo3 O6 1.9107(13) . ? Mo3 O13 1.9336(13) 2_576 ? Mo3 O14 2.0064(14) . ? Mo3 O7 2.32040(18) . ? Mo4 O15 1.6809(14) . ? Mo4 O14 1.8481(14) . ? Mo4 O9 1.8730(13) 2_576 ? Mo4 O11 1.9850(13) . ? Mo4 O8 2.0135(14) 2_576 ? Mo4 O7 2.32235(17) . ? O1 C1 1.320(2) . ? O2 C9 1.348(2) . ? O5 C14 1.225(2) . ? O7 Mo2 2.31474(16) 2_576 ? O7 Mo3 2.32040(18) 2_576 ? O7 Mo4 2.32235(17) 2_576 ? O8 Mo4 2.0135(14) 2_576 ? O9 Mo4 1.8730(13) 2_576 ? O13 Mo3 1.9336(13) 2_576 ? N1 C7 1.291(2) . ? N1 N2 1.396(2) . ? N2 C1 1.293(2) . ? N3 C5 1.339(3) . ? N3 C4 1.339(3) . ? C1 C2 1.484(2) . ? C2 C3 1.391(3) . ? C2 C6 1.395(3) . ? C3 C4 1.384(3) . ? C5 C6 1.372(3) . ? C7 C8 1.441(2) . ? C8 C13 1.405(3) . ? C8 C9 1.410(3) . ? C9 C10 1.400(3) . ? C10 C11 1.386(3) . ? C11 C12 1.398(3) . ? C12 C13 1.373(3) . ? C14 C16 1.486(3) . ? C14 C15 1.493(3) . ? O16 C17 1.188(6) . ? C17 C18 1.479(5) . ? C17 C19 1.479(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 O4 Mo1 O3 107.15(6) . . ? O4 Mo1 O2 99.05(6) . . ? O3 Mo1 O2 99.15(6) . . ? O4 Mo1 O1 99.29(6) . . ? O3 Mo1 O1 100.36(6) . . ? O2 Mo1 O1 147.85(5) . . ? O4 Mo1 N1 92.72(6) . . ? O3 Mo1 N1 159.81(6) . . ? O2 Mo1 N1 80.73(5) . . ? O1 Mo1 N1 72.24(5) . . ? O4 Mo1 O5 171.58(6) . . ? O3 Mo1 O5 80.06(5) . . ? O2 Mo1 O5 83.78(5) . . ? O1 Mo1 O5 74.76(5) . . ? N1 Mo1 O5 79.86(5) . . ? O10 Mo2 O11 104.05(6) . . ? O10 Mo2 O13 103.21(6) . . ? O11 Mo2 O13 89.15(6) . . ? O10 Mo2 O6 103.82(6) . . ? O11 Mo2 O6 88.92(6) . . ? O13 Mo2 O6 152.55(6) . . ? O10 Mo2 O9 102.55(6) . . ? O11 Mo2 O9 153.39(6) . . ? O13 Mo2 O9 85.19(6) . . ? O6 Mo2 O9 84.37(6) . . ? O10 Mo2 O7 178.28(5) . . ? O11 Mo2 O7 77.67(4) . . ? O13 Mo2 O7 76.64(4) . . ? O6 Mo2 O7 76.20(4) . . ? O9 Mo2 O7 75.73(4) . . ? O12 Mo3 O8 103.99(7) . . ? O12 Mo3 O6 104.76(6) . . ? O8 Mo3 O6 90.70(6) . . ? O12 Mo3 O13 102.40(6) . 2_576 ? O8 Mo3 O13 89.73(6) . 2_576 ? O6 Mo3 O13 151.88(6) . 2_576 ? O12 Mo3 O14 102.45(7) . . ? O8 Mo3 O14 153.53(6) . . ? O6 Mo3 O14 83.62(6) . . ? O13 Mo3 O14 83.56(6) 2_576 . ? O12 Mo3 O7 177.28(6) . . ? O8 Mo3 O7 78.43(4) . . ? O6 Mo3 O7 76.32(4) . . ? O13 Mo3 O7 76.23(4) 2_576 . ? O14 Mo3 O7 75.11(4) . . ? O15 Mo4 O14 104.77(7) . . ? O15 Mo4 O9 104.11(7) . 2_576 ? O14 Mo4 O9 92.98(6) . 2_576 ? O15 Mo4 O11 102.74(6) . . ? O14 Mo4 O11 87.56(6) . . ? O9 Mo4 O11 152.05(6) 2_576 . ? O15 Mo4 O8 101.68(7) . 2_576 ? O14 Mo4 O8 152.99(6) . 2_576 ? O9 Mo4 O8 85.78(6) 2_576 2_576 ? O11 Mo4 O8 81.35(6) . 2_576 ? O15 Mo4 O7 176.76(5) . . ? O14 Mo4 O7 77.96(4) . . ? O9 Mo4 O7 77.32(4) 2_576 . ? O11 Mo4 O7 75.48(4) . . ? O8 Mo4 O7 75.45(4) 2_576 . ? C1 O1 Mo1 118.21(11) . . ? C9 O2 Mo1 134.08(12) . . ? C14 O5 Mo1 146.76(13) . . ? Mo3 O6 Mo2 117.44(7) . . ? Mo2 O7 Mo2 180.0 . 2_576 ? Mo2 O7 Mo3 89.983(6) . 2_576 ? Mo2 O7 Mo3 90.017(6) 2_576 2_576 ? Mo2 O7 Mo3 90.017(6) . . ? Mo2 O7 Mo3 89.983(6) 2_576 . ? Mo3 O7 Mo3 180.0 2_576 . ? Mo2 O7 Mo4 90.160(6) . . ? Mo2 O7 Mo4 89.840(6) 2_576 . ? Mo3 O7 Mo4 89.967(7) 2_576 . ? Mo3 O7 Mo4 90.033(7) . . ? Mo2 O7 Mo4 89.840(6) . 2_576 ? Mo2 O7 Mo4 90.160(6) 2_576 2_576 ? Mo3 O7 Mo4 90.033(7) 2_576 2_576 ? Mo3 O7 Mo4 89.967(7) . 2_576 ? Mo4 O7 Mo4 180.0 . 2_576 ? Mo3 O8 Mo4 116.01(6) . 2_576 ? Mo4 O9 Mo2 116.82(7) 2_576 . ? Mo2 O11 Mo4 116.50(6) . . ? Mo2 O13 Mo3 116.55(6) . 2_576 ? Mo4 O14 Mo3 116.79(7) . . ? C7 N1 N2 115.57(15) . . ? C7 N1 Mo1 128.58(12) . . ? N2 N1 Mo1 115.37(11) . . ? C1 N2 N1 108.81(15) . . ? C5 N3 C4 123.23(17) . . ? N2 C1 O1 125.06(17) . . ? N2 C1 C2 117.46(16) . . ? O1 C1 C2 117.47(16) . . ? C3 C2 C6 119.57(17) . . ? C3 C2 C1 121.13(17) . . ? C6 C2 C1 119.30(17) . . ? C4 C3 C2 119.26(18) . . ? N3 C4 C3 119.08(18) . . ? N3 C5 C6 119.79(18) . . ? C5 C6 C2 119.05(18) . . ? N1 C7 C8 123.27(17) . . ? C13 C8 C9 118.54(17) . . ? C13 C8 C7 118.63(17) . . ? C9 C8 C7 122.84(17) . . ? O2 C9 C10 117.75(17) . . ? O2 C9 C8 122.55(16) . . ? C10 C9 C8 119.63(17) . . ? C11 C10 C9 120.43(18) . . ? C10 C11 C12 120.24(18) . . ? C13 C12 C11 119.56(18) . . ? C12 C13 C8 121.60(18) . . ? O5 C14 C16 122.64(19) . . ? O5 C14 C15 119.90(19) . . ? C16 C14 C15 117.46(19) . . ? O16 C17 C18 122.4(5) . . ? O16 C17 C19 122.3(5) . . ? C18 C17 C19 115.3(8) . . ? _diffrn_measured_fraction_theta_max 0.955 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.955 _refine_diff_density_max 0.367 _refine_diff_density_min -0.506 _refine_diff_density_rms 0.083 data_2a _database_code_depnum_ccdc_archive 'CCDC 802260' #TrackingRef '2a.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; bis(acetonitrile cis-dioxo(2-oxo-4-methoxybenzaldehyde isonicotinylhydrazonato- O, N,O')molybdenum(VI)) hexamolybdate acetonitrile solvate (1/4) ; _chemical_name_common ; bis(acetonitrile cis-dioxo(2-oxo-4-methoxybenzaldehyde isonicotinylhydrazonato-O, N,O')molybdenum(VI)) hexamolybdate acetonitrile solvate (1/4) ; _chemical_melting_point ? _chemical_formula_moiety '2(C16H15MoN4O5),Mo6O19, 4(C2H3N)' _chemical_formula_sum 'C40 H42 Mo8 N12 O29' _chemical_formula_weight 1922.38 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.0325(3) _cell_length_b 11.0829(4) _cell_length_c 14.1157(5) _cell_angle_alpha 100.866(3) _cell_angle_beta 105.795(3) _cell_angle_gamma 112.231(3) _cell_volume 1452.68(8) _cell_formula_units_Z 1 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 15 _cell_measurement_theta_max 25 _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.66 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.197 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 934 _exptl_absorpt_coefficient_mu 1.767 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.766 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'Xcalibur CCD' _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20320 _diffrn_reflns_av_R_equivalents 0.0191 _diffrn_reflns_av_sigmaI/netI 0.0180 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.70 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5078 _reflns_number_gt 4510 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD (Oxford Diffraction,2003)' _computing_cell_refinement 'CrysAlis RED (Oxford Diffraction,2003)' _computing_data_reduction 'CrysAlis RED (Oxford Diffraction,2003)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON98 (Spek, 1990)' _computing_publication_material 'SHELXL97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0214P)^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 5078 _refine_ls_number_parameters 477 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0201 _refine_ls_R_factor_gt 0.0148 _refine_ls_wR_factor_ref 0.0377 _refine_ls_wR_factor_gt 0.0370 _refine_ls_goodness_of_fit_ref 1.121 _refine_ls_restrained_S_all 1.121 _refine_ls_shift/su_max 0.004 _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 Mo3 Mo 0.341687(19) 0.954066(19) 0.835044(13) 0.01454(5) Uani 1 1 d . . . Mo2 Mo 0.671409(19) 1.178716(18) 0.976756(14) 0.01366(5) Uani 1 1 d . . . Mo1 Mo 0.242342(19) 0.323544(19) 0.551959(14) 0.01432(5) Uani 1 1 d . . . Mo4 Mo 0.425516(19) 1.152684(19) 1.070793(14) 0.01447(5) Uani 1 1 d . . . O11 O 0.78751(15) 1.31167(15) 0.95562(12) 0.0196(3) Uani 1 1 d . . . O10 O 0.36820(16) 1.25873(15) 1.12412(12) 0.0202(3) Uani 1 1 d . . . O2 O 0.36169(15) 0.23363(16) 0.57756(11) 0.0189(3) Uani 1 1 d . . . O4 O 0.35431(15) 0.48150(15) 0.64222(11) 0.0197(3) Uani 1 1 d . . . O6 O 0.5000 1.0000 1.0000 0.0109(4) Uani 1 2 d S . . O3 O 0.11750(16) 0.25274(16) 0.60052(11) 0.0206(3) Uani 1 1 d . . . O5 O 0.73666(17) 0.10711(17) 0.63168(12) 0.0239(4) Uani 1 1 d . . . O9 O 0.50191(15) 1.10451(15) 0.84533(11) 0.0167(3) Uani 1 1 d . . . O15 O 0.23460(14) 0.81008(15) 0.88858(11) 0.0164(3) Uani 1 1 d . . . O13 O 0.43063(15) 0.83678(15) 0.81068(11) 0.0166(3) Uani 1 1 d . . . O12 O 0.69668(15) 1.02526(15) 0.91994(11) 0.0153(3) Uani 1 1 d . . . O8 O 0.56793(15) 1.26479(14) 1.03257(11) 0.0162(3) Uani 1 1 d . . . O7 O 0.30140(15) 1.07403(15) 0.92486(11) 0.0159(3) Uani 1 1 d . . . N1 N 0.32509(18) 0.35276(18) 0.42557(13) 0.0148(4) Uani 1 1 d . . . N4 N 0.09650(19) 0.1139(2) 0.40747(15) 0.0210(4) Uani 1 1 d . . . O1 O 0.12604(15) 0.38855(15) 0.45707(11) 0.0176(3) Uani 1 1 d . . . O14 O 0.22131(16) 0.91238(16) 0.71615(11) 0.0233(4) Uani 1 1 d . . . C6 C 0.1042(2) 0.5080(2) 0.23081(17) 0.0179(5) Uani 1 1 d . . . N2 N 0.25715(18) 0.40000(18) 0.35290(13) 0.0164(4) Uani 1 1 d . . . C5 C 0.0179(2) 0.5450(2) 0.16688(18) 0.0177(5) Uani 1 1 d . . . C15 C 0.0248(2) 0.0171(2) 0.33892(18) 0.0190(5) Uani 1 1 d . . . C10 C 0.5478(2) 0.1742(2) 0.60840(17) 0.0166(5) Uani 1 1 d . . . C8 C 0.4961(2) 0.2663(2) 0.46689(16) 0.0149(5) Uani 1 1 d . . . C2 C 0.0683(2) 0.4612(2) 0.30939(16) 0.0150(5) Uani 1 1 d . . . C14 C 0.7144(3) 0.0709(3) 0.72008(19) 0.0230(5) Uani 1 1 d . . . N3 N -0.1006(2) 0.53606(19) 0.17955(15) 0.0163(4) Uani 1 1 d . . . C9 C 0.4680(2) 0.2267(2) 0.55132(16) 0.0152(5) Uani 1 1 d . . . C11 C 0.6551(2) 0.1596(2) 0.58226(16) 0.0182(5) Uani 1 1 d . . . C7 C 0.4181(2) 0.3199(2) 0.40487(16) 0.0148(5) Uani 1 1 d . . . C13 C 0.6060(2) 0.2493(2) 0.44300(17) 0.0176(5) Uani 1 1 d . . . C3 C -0.0557(2) 0.4540(2) 0.32042(17) 0.0169(5) Uani 1 1 d . . . N5 N 0.3400(2) 0.4118(2) 0.88167(15) 0.0238(4) Uani 1 1 d . . . C16 C -0.0665(3) -0.1077(3) 0.2492(2) 0.0255(6) Uani 1 1 d . . . C12 C 0.6849(2) 0.1979(2) 0.49817(17) 0.0198(5) Uani 1 1 d . . . C19 C 0.0541(3) 0.1522(3) 1.1052(2) 0.0248(5) Uani 1 1 d . . . C17 C 0.5629(3) 0.4307(3) 0.8456(2) 0.0218(5) Uani 1 1 d . . . N6 N 0.0804(2) 0.2947(2) 0.97945(16) 0.0306(5) Uani 1 1 d . . . C4 C -0.1394(2) 0.4912(2) 0.25339(16) 0.0171(5) Uani 1 1 d . . . C1 C 0.1576(2) 0.4158(2) 0.37717(16) 0.0158(5) Uani 1 1 d . . . C18 C 0.4384(2) 0.4205(2) 0.86652(16) 0.0171(5) Uiso 1 1 d . . . C20 C 0.0697(2) 0.2320(2) 1.03448(18) 0.0204(5) Uiso 1 1 d . . . H3 H -0.075(2) 0.424(2) 0.3711(19) 0.019(6) Uiso 1 1 d . . . H5 H 0.034(2) 0.575(2) 0.1210(18) 0.012(6) Uiso 1 1 d . . . H10 H 0.524(2) 0.146(2) 0.6625(19) 0.022(6) Uiso 1 1 d . . . H7 H 0.432(2) 0.329(2) 0.3427(18) 0.018(6) Uiso 1 1 d . . . H4 H -0.220(3) 0.484(2) 0.2552(17) 0.017(6) Uiso 1 1 d . . . H12 H 0.753(2) 0.184(2) 0.4806(18) 0.021(6) Uiso 1 1 d . . . H6 H 0.176(2) 0.516(2) 0.2223(17) 0.014(6) Uiso 1 1 d . . . H14A H 0.622(3) 0.005(2) 0.7014(18) 0.020(6) Uiso 1 1 d . . . H19C H 0.097(3) 0.090(3) 1.0965(18) 0.025(7) Uiso 1 1 d . . . H14B H 0.748(2) 0.156(3) 0.7799(19) 0.025(6) Uiso 1 1 d . . . H14C H 0.776(2) 0.030(2) 0.7378(18) 0.020(6) Uiso 1 1 d . . . H19A H -0.042(3) 0.104(3) 1.092(2) 0.038(8) Uiso 1 1 d . . . H19B H 0.099(3) 0.207(3) 1.169(3) 0.058(10) Uiso 1 1 d . . . H17B H 0.545(3) 0.337(3) 0.816(2) 0.037(8) Uiso 1 1 d . . . H16B H -0.077(3) -0.088(3) 0.193(2) 0.033(8) Uiso 1 1 d . . . H16A H -0.167(3) -0.153(3) 0.250(2) 0.048(8) Uiso 1 1 d . . . H17A H 0.635(3) 0.482(3) 0.904(2) 0.040(8) Uiso 1 1 d . . . H17C H 0.573(3) 0.478(3) 0.797(2) 0.034(7) Uiso 1 1 d . . . H16C H -0.030(3) -0.175(3) 0.257(2) 0.053(9) Uiso 1 1 d . . . H13 H 0.624(2) 0.274(2) 0.3900(18) 0.017(6) Uiso 1 1 d . . . H31 H -0.148(2) 0.556(2) 0.1440(18) 0.013(7) Uiso 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 Mo3 0.01261(10) 0.01703(10) 0.01132(10) 0.00427(8) 0.00218(7) 0.00591(8) Mo2 0.01240(10) 0.01225(10) 0.01568(10) 0.00533(8) 0.00638(7) 0.00385(8) Mo1 0.01489(10) 0.01754(10) 0.01195(10) 0.00518(8) 0.00671(8) 0.00746(8) Mo4 0.01440(10) 0.01289(10) 0.01752(10) 0.00281(8) 0.00726(8) 0.00777(8) O11 0.0194(8) 0.0170(8) 0.0237(8) 0.0079(7) 0.0122(7) 0.0062(7) O10 0.0200(8) 0.0187(8) 0.0243(8) 0.0040(7) 0.0101(7) 0.0114(7) O2 0.0196(8) 0.0260(9) 0.0181(8) 0.0116(7) 0.0110(7) 0.0127(7) O4 0.0196(8) 0.0213(8) 0.0155(8) 0.0054(7) 0.0067(6) 0.0070(7) O6 0.0111(10) 0.0103(10) 0.0102(10) 0.0028(8) 0.0043(8) 0.0037(8) O3 0.0205(8) 0.0234(9) 0.0212(8) 0.0096(7) 0.0114(7) 0.0098(7) O5 0.0295(9) 0.0380(10) 0.0205(9) 0.0160(8) 0.0141(7) 0.0251(8) O9 0.0172(8) 0.0184(8) 0.0153(8) 0.0074(6) 0.0066(6) 0.0076(7) O15 0.0116(7) 0.0151(8) 0.0167(8) 0.0017(6) 0.0033(6) 0.0033(6) O13 0.0173(8) 0.0171(8) 0.0125(7) 0.0010(6) 0.0038(6) 0.0079(7) O12 0.0151(7) 0.0164(8) 0.0160(8) 0.0049(6) 0.0089(6) 0.0068(6) O8 0.0176(8) 0.0118(7) 0.0214(8) 0.0058(6) 0.0090(6) 0.0074(6) O7 0.0142(7) 0.0180(8) 0.0169(8) 0.0055(6) 0.0046(6) 0.0097(6) N1 0.0148(9) 0.0171(9) 0.0117(9) 0.0056(7) 0.0037(7) 0.0068(8) N4 0.0167(10) 0.0197(11) 0.0239(11) 0.0048(9) 0.0069(9) 0.0074(9) O1 0.0190(8) 0.0241(8) 0.0144(8) 0.0080(7) 0.0088(6) 0.0118(7) O14 0.0214(8) 0.0279(9) 0.0165(8) 0.0051(7) 0.0017(7) 0.0118(7) C6 0.0142(12) 0.0189(12) 0.0197(12) 0.0050(10) 0.0088(10) 0.0057(10) N2 0.0162(9) 0.0200(10) 0.0129(9) 0.0059(8) 0.0043(7) 0.0086(8) C5 0.0201(12) 0.0183(12) 0.0159(12) 0.0076(10) 0.0091(10) 0.0075(10) C15 0.0174(11) 0.0203(13) 0.0237(13) 0.0114(11) 0.0091(10) 0.0102(10) C10 0.0209(12) 0.0180(12) 0.0116(11) 0.0049(9) 0.0071(9) 0.0089(10) C8 0.0156(11) 0.0134(11) 0.0125(10) 0.0019(9) 0.0045(9) 0.0051(9) C2 0.0161(11) 0.0126(11) 0.0114(10) -0.0002(9) 0.0022(9) 0.0058(9) C14 0.0264(14) 0.0301(14) 0.0217(13) 0.0132(12) 0.0113(11) 0.0181(13) N3 0.0182(10) 0.0158(10) 0.0134(10) 0.0041(8) 0.0023(8) 0.0092(9) C9 0.0143(11) 0.0136(11) 0.0134(11) -0.0002(9) 0.0044(9) 0.0047(9) C11 0.0200(12) 0.0181(12) 0.0148(11) 0.0030(9) 0.0045(9) 0.0097(10) C7 0.0141(11) 0.0145(11) 0.0119(11) 0.0021(9) 0.0054(9) 0.0033(9) C13 0.0214(12) 0.0181(12) 0.0135(11) 0.0045(10) 0.0082(10) 0.0083(10) C3 0.0199(12) 0.0168(12) 0.0133(11) 0.0042(9) 0.0081(9) 0.0068(10) N5 0.0228(11) 0.0218(11) 0.0219(10) 0.0054(8) 0.0035(8) 0.0096(9) C16 0.0317(15) 0.0177(13) 0.0163(13) 0.0050(10) 0.0001(11) 0.0069(12) C12 0.0206(12) 0.0243(13) 0.0184(12) 0.0058(10) 0.0106(10) 0.0124(11) C19 0.0219(14) 0.0279(14) 0.0219(14) 0.0059(11) 0.0077(11) 0.0101(12) C17 0.0221(13) 0.0206(13) 0.0240(14) 0.0078(12) 0.0076(11) 0.0117(11) N6 0.0243(11) 0.0378(13) 0.0335(12) 0.0118(10) 0.0109(9) 0.0180(10) C4 0.0150(12) 0.0178(12) 0.0164(12) 0.0015(9) 0.0067(9) 0.0067(10) C1 0.0162(11) 0.0133(11) 0.0139(11) 0.0022(9) 0.0047(9) 0.0044(9) _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 Mo3 O14 1.6804(14) . ? Mo3 O9 1.8614(15) . ? Mo3 O7 1.9212(14) . ? Mo3 O13 1.9368(15) . ? Mo3 O15 2.0069(15) . ? Mo3 O6 2.3233(2) . ? Mo2 O11 1.6871(15) . ? Mo2 O15 1.8560(14) 2_677 ? Mo2 O12 1.8920(14) . ? Mo2 O8 1.9658(15) . ? Mo2 O9 1.9969(14) . ? Mo2 O6 2.3142(2) . ? Mo1 O4 1.6970(15) . ? Mo1 O3 1.6975(15) . ? Mo1 O2 1.9305(15) . ? Mo1 O1 2.0216(15) . ? Mo1 N1 2.2365(17) . ? Mo1 N4 2.3967(19) . ? Mo4 O10 1.6840(15) . ? Mo4 O8 1.8816(15) . ? Mo4 O13 1.9163(14) 2_677 ? Mo4 O7 1.9398(14) . ? Mo4 O12 1.9762(15) 2_677 ? Mo4 O6 2.32358(19) . ? O2 C9 1.346(3) . ? O6 Mo2 2.3142(2) 2_677 ? O6 Mo3 2.3234(2) 2_677 ? O6 Mo4 2.3237(2) 2_677 ? O5 C11 1.357(3) . ? O5 C14 1.435(3) . ? O15 Mo2 1.8559(14) 2_677 ? O13 Mo4 1.9163(14) 2_677 ? O12 Mo4 1.9762(14) 2_677 ? N1 C7 1.295(3) . ? N1 N2 1.403(2) . ? N4 C15 1.124(3) . ? O1 C1 1.322(3) . ? C6 C5 1.363(3) . ? C6 C2 1.399(3) . ? N2 C1 1.296(3) . ? C5 N3 1.337(3) . ? C15 C16 1.457(3) . ? C10 C11 1.388(3) . ? C10 C9 1.393(3) . ? C8 C9 1.416(3) . ? C8 C13 1.410(3) . ? C8 C7 1.426(3) . ? C2 C3 1.393(3) . ? C2 C1 1.477(3) . ? N3 C4 1.339(3) . ? C11 C12 1.412(3) . ? C13 C12 1.365(3) . ? C3 C4 1.370(3) . ? N5 C18 1.135(3) . ? C19 C20 1.456(3) . ? C17 C18 1.449(3) . ? N6 C20 1.137(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O14 Mo3 O9 105.10(7) . . ? O14 Mo3 O7 103.89(7) . . ? O9 Mo3 O7 90.33(6) . . ? O14 Mo3 O13 102.86(7) . . ? O9 Mo3 O13 89.40(6) . . ? O7 Mo3 O13 152.35(6) . . ? O14 Mo3 O15 101.56(7) . . ? O9 Mo3 O15 153.32(6) . . ? O7 Mo3 O15 84.37(6) . . ? O13 Mo3 O15 83.56(6) . . ? O14 Mo3 O6 176.79(6) . . ? O9 Mo3 O6 78.03(4) . . ? O7 Mo3 O6 76.62(4) . . ? O13 Mo3 O6 76.29(4) . . ? O15 Mo3 O6 75.30(4) . . ? O11 Mo2 O15 104.68(7) . 2_677 ? O11 Mo2 O12 104.73(7) . . ? O15 Mo2 O12 91.34(6) 2_677 . ? O11 Mo2 O8 101.31(7) . . ? O15 Mo2 O8 88.12(6) 2_677 . ? O12 Mo2 O8 153.20(6) . . ? O11 Mo2 O9 101.10(7) . . ? O15 Mo2 O9 153.89(6) 2_677 . ? O12 Mo2 O9 86.02(6) . . ? O8 Mo2 O9 82.85(6) . . ? O11 Mo2 O6 176.04(5) . . ? O15 Mo2 O6 78.30(5) 2_677 . ? O12 Mo2 O6 77.62(4) . . ? O8 Mo2 O6 76.04(4) . . ? O9 Mo2 O6 75.76(4) . . ? O4 Mo1 O3 104.34(7) . . ? O4 Mo1 O2 99.17(7) . . ? O3 Mo1 O2 104.85(7) . . ? O4 Mo1 O1 95.90(7) . . ? O3 Mo1 O1 94.61(7) . . ? O2 Mo1 O1 151.46(6) . . ? O4 Mo1 N1 98.18(7) . . ? O3 Mo1 N1 154.95(7) . . ? O2 Mo1 N1 81.88(6) . . ? O1 Mo1 N1 72.05(6) . . ? O4 Mo1 N4 171.91(7) . . ? O3 Mo1 N4 83.13(7) . . ? O2 Mo1 N4 81.62(6) . . ? O1 Mo1 N4 80.20(6) . . ? N1 Mo1 N4 73.91(6) . . ? O10 Mo4 O8 104.86(7) . . ? O10 Mo4 O13 102.69(7) . 2_677 ? O8 Mo4 O13 89.08(6) . 2_677 ? O10 Mo4 O7 104.23(7) . . ? O8 Mo4 O7 88.23(6) . . ? O13 Mo4 O7 152.73(6) 2_677 . ? O10 Mo4 O12 101.96(7) . 2_677 ? O8 Mo4 O12 153.17(6) . 2_677 ? O13 Mo4 O12 85.92(6) 2_677 2_677 ? O7 Mo4 O12 84.34(6) . 2_677 ? O10 Mo4 O6 177.72(5) . . ? O8 Mo4 O6 77.35(4) . . ? O13 Mo4 O6 76.66(4) 2_677 . ? O7 Mo4 O6 76.27(4) . . ? O12 Mo4 O6 75.84(4) 2_677 . ? C9 O2 Mo1 137.62(14) . . ? Mo2 O6 Mo2 179.998(8) 2_677 . ? Mo2 O6 Mo3 90.068(7) 2_677 . ? Mo2 O6 Mo3 89.933(8) . . ? Mo2 O6 Mo3 89.932(8) 2_677 2_677 ? Mo2 O6 Mo3 90.068(8) . 2_677 ? Mo3 O6 Mo3 179.999(10) . 2_677 ? Mo2 O6 Mo4 90.201(7) 2_677 . ? Mo2 O6 Mo4 89.801(7) . . ? Mo3 O6 Mo4 90.002(7) . . ? Mo3 O6 Mo4 89.999(7) 2_677 . ? Mo2 O6 Mo4 89.800(7) 2_677 2_677 ? Mo2 O6 Mo4 90.199(8) . 2_677 ? Mo3 O6 Mo4 89.999(8) . 2_677 ? Mo3 O6 Mo4 90.000(7) 2_677 2_677 ? Mo4 O6 Mo4 180.0 . 2_677 ? C11 O5 C14 117.43(18) . . ? Mo3 O9 Mo2 116.26(7) . . ? Mo2 O15 Mo3 116.24(7) 2_677 . ? Mo4 O13 Mo3 117.03(7) 2_677 . ? Mo2 O12 Mo4 116.25(7) . 2_677 ? Mo4 O8 Mo2 116.60(7) . . ? Mo3 O7 Mo4 116.65(7) . . ? C7 N1 N2 115.46(17) . . ? C7 N1 Mo1 128.60(15) . . ? N2 N1 Mo1 115.60(13) . . ? C15 N4 Mo1 177.72(18) . . ? C1 O1 Mo1 118.99(13) . . ? C5 C6 C2 119.8(2) . . ? C1 N2 N1 109.04(17) . . ? N3 C5 C6 119.8(2) . . ? N4 C15 C16 179.0(3) . . ? C11 C10 C9 120.0(2) . . ? C9 C8 C13 117.6(2) . . ? C9 C8 C7 123.4(2) . . ? C13 C8 C7 119.1(2) . . ? C3 C2 C6 118.7(2) . . ? C3 C2 C1 120.6(2) . . ? C6 C2 C1 120.7(2) . . ? C4 N3 C5 122.4(2) . . ? O2 C9 C10 117.47(19) . . ? O2 C9 C8 122.07(19) . . ? C10 C9 C8 120.4(2) . . ? O5 C11 C10 124.4(2) . . ? O5 C11 C12 115.0(2) . . ? C10 C11 C12 120.6(2) . . ? N1 C7 C8 124.4(2) . . ? C12 C13 C8 122.6(2) . . ? C4 C3 C2 119.1(2) . . ? C13 C12 C11 118.8(2) . . ? N3 C4 C3 120.1(2) . . ? N2 C1 O1 124.3(2) . . ? N2 C1 C2 118.75(19) . . ? O1 C1 C2 116.90(19) . . ? N5 C18 C17 179.2(3) . . ? N6 C20 C19 179.0(3) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.416 _refine_diff_density_min -0.428 _refine_diff_density_rms 0.085 data_2b _database_code_depnum_ccdc_archive 'CCDC 802261' #TrackingRef '2b.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; bis(acetone cis-dioxo(2-oxo-4-methoxybenzaldehyde isonicotinylhydrazonato- O, N, O)molybdenum(VI)) hexamolybdate acetone solvate (1/1) ; _chemical_name_common ; bis(acetone cis-dioxo(2-oxo-4-methoxybenzaldehyde isonicotinylhydrazonato-O, N, O)molybdenum(VI)) hexamolybdate acetone solvate (1/1) ; _chemical_melting_point ? _chemical_formula_moiety '2(C17 H18 Mo N3 O6), Mo6 O19, C3 H6 O' _chemical_formula_sum 'C37 H42 Mo8 N6 O32' _chemical_formula_weight 1850.28 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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.5650(3) _cell_length_b 11.5974(3) _cell_length_c 12.5744(3) _cell_angle_alpha 89.039(2) _cell_angle_beta 72.454(2) _cell_angle_gamma 68.084(2) _cell_volume 1354.85(6) _cell_formula_units_Z 1 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.54 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.249 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 889 _exptl_absorpt_coefficient_mu 1.889 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.87012 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'Xcalibur CCD' _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24691 _diffrn_reflns_av_R_equivalents 0.0146 _diffrn_reflns_av_sigmaI/netI 0.0122 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 4.10 _diffrn_reflns_theta_max 27.50 _reflns_number_total 6193 _reflns_number_gt 5950 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD (Oxford Diffraction,2003)' _computing_cell_refinement 'CrysAlis RED (Oxford Diffraction,2003)' _computing_data_reduction 'CrysAlis RED (Oxford Diffraction,2003)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON98 (Spek, 1990)' _computing_publication_material 'SHELXL97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0320P)^2^+1.4330P] 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 6193 _refine_ls_number_parameters 397 _refine_ls_number_restraints 23 _refine_ls_R_factor_all 0.0168 _refine_ls_R_factor_gt 0.0159 _refine_ls_wR_factor_ref 0.0428 _refine_ls_wR_factor_gt 0.0423 _refine_ls_goodness_of_fit_ref 1.107 _refine_ls_restrained_S_all 1.105 _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 0.804136(14) 0.451559(13) 0.741944(11) 0.01420(4) Uani 1 1 d . . . Mo2 Mo 0.441578(15) 0.830696(13) 0.975103(13) 0.01807(4) Uani 1 1 d . . . Mo3 Mo 0.286266(15) 1.134343(13) 0.976281(12) 0.01682(4) Uani 1 1 d . . . Mo4 Mo 0.613667(15) 0.981915(14) 0.808458(12) 0.01854(4) Uani 1 1 d . . . O1 O 0.94781(12) 0.46183(11) 0.81206(10) 0.0166(2) Uani 1 1 d . . . O2 O 0.75644(12) 0.36689(12) 0.63707(10) 0.0197(2) Uani 1 1 d . . . O3 O 0.66195(12) 0.47073(12) 0.86063(10) 0.0198(2) Uani 1 1 d . . . O4 O 0.76652(13) 0.59112(12) 0.68976(11) 0.0235(3) Uani 1 1 d . . . O5 O 0.89460(13) 0.25012(12) 0.80189(11) 0.0221(3) Uani 1 1 d . . . O6 O 0.68314(15) 0.28870(14) 0.29289(12) 0.0308(3) Uani 1 1 d . . . O7 O 0.23461(13) 1.12246(12) 1.13328(10) 0.0212(3) Uani 1 1 d . . . O8 O 0.28227(13) 0.97248(11) 0.95641(11) 0.0206(2) Uani 1 1 d . . . O9 O 0.13157(14) 1.23252(12) 0.95798(11) 0.0250(3) Uani 1 1 d . . . O10 O 0.62469(13) 0.75415(11) 0.99894(11) 0.0210(3) Uani 1 1 d . . . O11 O 0.39908(15) 0.70797(12) 0.95600(12) 0.0276(3) Uani 1 1 d . . . O12 O 0.5000 1.0000 1.0000 0.0136(3) Uani 1 2 d S . . O13 O 0.54704(13) 0.84900(11) 0.82447(10) 0.0211(3) Uani 1 1 d . . . O14 O 0.42283(13) 1.09575(12) 0.82537(10) 0.0213(3) Uani 1 1 d . . . O15 O 0.70017(15) 0.96603(14) 0.66955(11) 0.0291(3) Uani 1 1 d . . . O16 O 0.35675(14) 0.87888(12) 1.13336(11) 0.0228(3) Uani 1 1 d . . . N1 N 1.02262(14) 0.36189(13) 0.61705(12) 0.0157(3) Uani 1 1 d . . . N2 N 1.13693(14) 0.36156(13) 0.65083(12) 0.0164(3) Uani 1 1 d . . . N3 N 1.37023(15) 0.48916(13) 0.88666(12) 0.0170(3) Uani 1 1 d . . . H3 H 1.4300 0.5070 0.9128 0.020 Uiso 1 1 calc R . . C1 C 1.08564(16) 0.41729(14) 0.75167(14) 0.0142(3) Uani 1 1 d . . . C2 C 1.18635(17) 0.43815(15) 0.80190(13) 0.0139(3) Uani 1 1 d . . . C3 C 1.13338(18) 0.52721(15) 0.89437(14) 0.0165(3) Uani 1 1 d . . . H3A H 1.0326 0.5698 0.9291 0.020 Uiso 1 1 calc R . . C4 C 1.22876(18) 0.55253(16) 0.93462(14) 0.0177(3) Uani 1 1 d . . . H4 H 1.1944 0.6146 0.9961 0.021 Uiso 1 1 calc R . . C5 C 1.42515(17) 0.39922(16) 0.80010(15) 0.0183(3) Uani 1 1 d . . . H5 H 1.5263 0.3543 0.7704 0.022 Uiso 1 1 calc R . . C6 C 1.33484(17) 0.37263(15) 0.75491(14) 0.0166(3) Uani 1 1 d . . . H6 H 1.3726 0.3108 0.6927 0.020 Uiso 1 1 calc R . . C7 C 1.05584(17) 0.32073(15) 0.51332(14) 0.0165(3) Uani 1 1 d . . . H7 H 1.1539 0.2920 0.4680 0.020 Uiso 1 1 calc R . . C8 C 0.95238(17) 0.31630(15) 0.46327(14) 0.0160(3) Uani 1 1 d . . . C9 C 0.80769(18) 0.34074(15) 0.52442(14) 0.0170(3) Uani 1 1 d . . . C10 C 0.71323(18) 0.33272(16) 0.47008(15) 0.0202(3) Uani 1 1 d . . . H10 H 0.6154 0.3501 0.5114 0.024 Uiso 1 1 calc R . . C11 C 0.76416(19) 0.29899(16) 0.35470(15) 0.0214(3) Uani 1 1 d . . . C12 C 0.90879(19) 0.27191(16) 0.29284(15) 0.0208(3) Uani 1 1 d . . . H12 H 0.9429 0.2474 0.2144 0.025 Uiso 1 1 calc R . . C13 C 0.99980(19) 0.28105(15) 0.34649(14) 0.0186(3) Uani 1 1 d . . . H13 H 1.0974 0.2633 0.3043 0.022 Uiso 1 1 calc R . . C14 C 0.5322(2) 0.3238(2) 0.3473(2) 0.0357(5) Uani 1 1 d . . . H14A H 0.4879 0.3092 0.2934 0.054 Uiso 1 1 calc R . . H14B H 0.4883 0.4126 0.3759 0.054 Uiso 1 1 calc R . . H14C H 0.5169 0.2737 0.4098 0.054 Uiso 1 1 calc R . . C15 C 0.94663(18) 0.13693(17) 0.77536(16) 0.0217(4) Uani 1 1 d . . . C16 C 1.0006(2) 0.04977(19) 0.85458(19) 0.0312(4) Uani 1 1 d . . . H16A H 0.9854 0.0979 0.9238 0.047 Uiso 1 1 calc R . . H16B H 1.1036 0.0001 0.8200 0.047 Uiso 1 1 calc R . . H16C H 0.9484 -0.0060 0.8721 0.047 Uiso 1 1 calc R . . C17 C 0.9595(2) 0.08088(19) 0.66465(18) 0.0319(4) Uani 1 1 d . . . H17A H 0.8697 0.1233 0.6474 0.048 Uiso 1 1 calc R . . H17B H 0.9779 -0.0082 0.6677 0.048 Uiso 1 1 calc R . . H17C H 1.0392 0.0908 0.6061 0.048 Uiso 1 1 calc R . . O17 O 0.5088(4) 0.1528(3) 0.5487(3) 0.0417(8) Uani 0.50 1 d PD A -1 C18 C 0.4958(5) 0.0571(4) 0.5297(3) 0.0380(10) Uani 0.50 1 d PDU A -1 C19 C 0.3670(10) 0.0313(11) 0.5962(8) 0.049(2) Uani 0.50 1 d PDU A -1 H19A H 0.3014 0.1024 0.6527 0.073 Uiso 0.50 1 calc PR A -1 H19B H 0.3982 -0.0442 0.6336 0.073 Uiso 0.50 1 calc PR A -1 H19C H 0.3172 0.0187 0.5458 0.073 Uiso 0.50 1 calc PR A -1 C20 C 0.6070(11) -0.0435(10) 0.4400(8) 0.060(3) Uani 0.50 1 d PDU A -1 H20A H 0.6861 -0.0175 0.4019 0.090 Uiso 0.50 1 calc PR A -1 H20B H 0.5637 -0.0582 0.3854 0.090 Uiso 0.50 1 calc PR A -1 H20C H 0.6441 -0.1207 0.4737 0.090 Uiso 0.50 1 calc PR A -1 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 0.01000(6) 0.01934(7) 0.01444(7) -0.00062(5) -0.00451(5) -0.00634(5) Mo2 0.01957(7) 0.01352(7) 0.02421(8) -0.00094(5) -0.00763(6) -0.00909(6) Mo3 0.01379(7) 0.01535(7) 0.02051(8) 0.00098(5) -0.00661(6) -0.00379(5) Mo4 0.01824(7) 0.02241(8) 0.01254(7) -0.00055(5) -0.00197(5) -0.00740(6) O1 0.0121(5) 0.0221(6) 0.0168(6) -0.0026(4) -0.0047(4) -0.0074(4) O2 0.0157(5) 0.0310(7) 0.0161(6) -0.0012(5) -0.0056(5) -0.0125(5) O3 0.0137(5) 0.0284(6) 0.0187(6) -0.0025(5) -0.0050(5) -0.0094(5) O4 0.0183(6) 0.0249(6) 0.0298(7) 0.0057(5) -0.0103(5) -0.0092(5) O5 0.0211(6) 0.0221(6) 0.0266(7) 0.0048(5) -0.0087(5) -0.0113(5) O6 0.0268(7) 0.0390(8) 0.0292(7) -0.0068(6) -0.0193(6) -0.0067(6) O7 0.0146(6) 0.0257(6) 0.0182(6) -0.0030(5) -0.0020(5) -0.0044(5) O8 0.0178(6) 0.0211(6) 0.0264(7) -0.0008(5) -0.0092(5) -0.0095(5) O9 0.0195(6) 0.0210(6) 0.0323(7) -0.0013(5) -0.0121(5) -0.0022(5) O10 0.0229(6) 0.0129(6) 0.0272(7) 0.0008(5) -0.0098(5) -0.0057(5) O11 0.0296(7) 0.0198(6) 0.0388(8) -0.0008(5) -0.0119(6) -0.0145(5) O12 0.0140(7) 0.0133(7) 0.0140(8) 0.0000(6) -0.0041(6) -0.0060(6) O13 0.0248(6) 0.0197(6) 0.0190(6) -0.0046(5) -0.0066(5) -0.0089(5) O14 0.0224(6) 0.0220(6) 0.0175(6) 0.0028(5) -0.0080(5) -0.0051(5) O15 0.0271(7) 0.0392(8) 0.0160(6) 0.0006(5) -0.0020(5) -0.0112(6) O16 0.0255(6) 0.0234(6) 0.0221(6) 0.0039(5) -0.0043(5) -0.0149(5) N1 0.0130(6) 0.0202(7) 0.0169(7) 0.0006(5) -0.0068(5) -0.0081(5) N2 0.0121(6) 0.0211(7) 0.0191(7) 0.0000(5) -0.0079(5) -0.0074(5) N3 0.0195(7) 0.0216(7) 0.0192(7) 0.0049(5) -0.0119(6) -0.0136(6) C1 0.0123(7) 0.0150(7) 0.0176(8) 0.0014(6) -0.0068(6) -0.0062(6) C2 0.0133(7) 0.0157(7) 0.0155(7) 0.0026(6) -0.0062(6) -0.0074(6) C3 0.0157(7) 0.0188(8) 0.0161(8) 0.0011(6) -0.0049(6) -0.0080(6) C4 0.0219(8) 0.0191(8) 0.0158(8) 0.0019(6) -0.0067(6) -0.0113(7) C5 0.0137(7) 0.0209(8) 0.0220(8) 0.0031(6) -0.0071(6) -0.0075(6) C6 0.0143(7) 0.0179(8) 0.0180(8) -0.0009(6) -0.0055(6) -0.0063(6) C7 0.0143(7) 0.0174(7) 0.0176(8) 0.0000(6) -0.0045(6) -0.0062(6) C8 0.0171(7) 0.0165(7) 0.0160(8) -0.0005(6) -0.0079(6) -0.0060(6) C9 0.0188(8) 0.0174(8) 0.0162(8) -0.0005(6) -0.0079(6) -0.0067(6) C10 0.0173(8) 0.0220(8) 0.0230(9) -0.0012(7) -0.0101(7) -0.0065(7) C11 0.0257(9) 0.0173(8) 0.0252(9) 0.0003(7) -0.0175(7) -0.0053(7) C12 0.0261(9) 0.0179(8) 0.0170(8) -0.0014(6) -0.0099(7) -0.0044(7) C13 0.0203(8) 0.0168(8) 0.0176(8) -0.0003(6) -0.0064(7) -0.0055(6) C14 0.0238(10) 0.0409(12) 0.0448(13) -0.0099(10) -0.0219(9) -0.0058(8) C15 0.0164(8) 0.0221(8) 0.0300(10) 0.0054(7) -0.0065(7) -0.0118(7) C16 0.0316(10) 0.0272(10) 0.0427(12) 0.0127(9) -0.0198(9) -0.0139(8) C17 0.0408(11) 0.0232(9) 0.0308(11) 0.0031(8) -0.0084(9) -0.0138(8) O17 0.054(2) 0.0313(16) 0.0323(17) 0.0017(13) -0.0104(15) -0.0106(15) C18 0.043(3) 0.035(2) 0.032(2) 0.0007(18) -0.024(2) -0.001(2) C19 0.053(4) 0.048(4) 0.049(6) -0.001(3) -0.024(3) -0.017(3) C20 0.067(6) 0.048(5) 0.051(6) -0.020(4) -0.033(4) 0.005(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 O4 1.6880(13) . ? Mo1 O3 1.7156(12) . ? Mo1 O2 1.9418(12) . ? Mo1 O1 2.0103(11) . ? Mo1 N1 2.2256(14) . ? Mo1 O5 2.3766(12) . ? Mo2 O11 1.6848(12) . ? Mo2 O16 1.9141(13) . ? Mo2 O10 1.9181(12) . ? Mo2 O8 1.9369(12) . ? Mo2 O13 1.9403(13) . ? Mo2 O12 2.31864(14) . ? Mo3 O9 1.6880(12) . ? Mo3 O7 1.9004(12) . ? Mo3 O8 1.9156(12) . ? Mo3 O10 1.9373(12) 2_677 ? Mo3 O14 1.9438(12) . ? Mo3 O12 2.31939(15) . ? Mo4 O15 1.6860(13) . ? Mo4 O14 1.9019(12) . ? Mo4 O13 1.9043(12) . ? Mo4 O16 1.9477(12) 2_677 ? Mo4 O7 1.9497(13) 2_677 ? Mo4 O12 2.31778(16) . ? O1 C1 1.3224(19) . ? O2 C9 1.350(2) . ? O5 C15 1.226(2) . ? O6 C11 1.353(2) . ? O6 C14 1.429(2) . ? O7 Mo4 1.9497(12) 2_677 ? O10 Mo3 1.9373(12) 2_677 ? O12 Mo4 2.31777(16) 2_677 ? O12 Mo2 2.31863(14) 2_677 ? O12 Mo3 2.31943(15) 2_677 ? O16 Mo4 1.9476(12) 2_677 ? N1 C7 1.293(2) . ? N1 N2 1.3945(18) . ? N2 C1 1.293(2) . ? N3 C4 1.338(2) . ? N3 C5 1.347(2) . ? C1 C2 1.481(2) . ? C2 C3 1.396(2) . ? C2 C6 1.398(2) . ? C3 C4 1.375(2) . ? C5 C6 1.371(2) . ? C7 C8 1.432(2) . ? C8 C9 1.408(2) . ? C8 C13 1.414(2) . ? C9 C10 1.398(2) . ? C10 C11 1.392(2) . ? C11 C12 1.404(3) . ? C12 C13 1.364(2) . ? C15 C16 1.489(3) . ? C15 C17 1.493(3) . ? O17 C18 1.205(6) . ? C18 C20 1.495(6) . ? C18 C19 1.500(6) . ? 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 106.17(6) . . ? O4 Mo1 O2 97.89(6) . . ? O3 Mo1 O2 100.02(5) . . ? O4 Mo1 O1 98.01(6) . . ? O3 Mo1 O1 99.83(5) . . ? O2 Mo1 O1 149.92(5) . . ? O4 Mo1 N1 94.90(6) . . ? O3 Mo1 N1 158.39(6) . . ? O2 Mo1 N1 81.37(5) . . ? O1 Mo1 N1 71.97(5) . . ? O4 Mo1 O5 171.24(5) . . ? O3 Mo1 O5 81.65(5) . . ? O2 Mo1 O5 84.38(5) . . ? O1 Mo1 O5 76.42(5) . . ? N1 Mo1 O5 77.01(5) . . ? O11 Mo2 O16 103.32(6) . . ? O11 Mo2 O10 103.24(6) . . ? O16 Mo2 O10 88.13(6) . . ? O11 Mo2 O8 103.41(6) . . ? O16 Mo2 O8 87.45(6) . . ? O10 Mo2 O8 153.29(5) . . ? O11 Mo2 O13 103.35(6) . . ? O16 Mo2 O13 153.31(5) . . ? O10 Mo2 O13 86.79(5) . . ? O8 Mo2 O13 85.44(5) . . ? O11 Mo2 O12 179.55(5) . . ? O16 Mo2 O12 77.07(4) . . ? O10 Mo2 O12 76.98(4) . . ? O8 Mo2 O12 76.35(4) . . ? O13 Mo2 O12 76.26(4) . . ? O9 Mo3 O7 103.77(6) . . ? O9 Mo3 O8 103.51(6) . . ? O7 Mo3 O8 88.00(6) . . ? O9 Mo3 O10 103.14(6) . 2_677 ? O7 Mo3 O10 87.47(6) . 2_677 ? O8 Mo3 O10 153.28(5) . 2_677 ? O9 Mo3 O14 103.11(6) . . ? O7 Mo3 O14 153.10(5) . . ? O8 Mo3 O14 86.51(5) . . ? O10 Mo3 O14 85.73(5) 2_677 . ? O9 Mo3 O12 179.48(5) . . ? O7 Mo3 O12 76.69(4) . . ? O8 Mo3 O12 76.72(4) . . ? O10 Mo3 O12 76.61(4) 2_677 . ? O14 Mo3 O12 76.42(4) . . ? O15 Mo4 O14 104.21(6) . . ? O15 Mo4 O13 102.92(6) . . ? O14 Mo4 O13 88.87(6) . . ? O15 Mo4 O16 103.61(6) . 2_677 ? O14 Mo4 O16 87.01(6) . 2_677 ? O13 Mo4 O16 153.35(5) . 2_677 ? O15 Mo4 O7 102.72(6) . 2_677 ? O14 Mo4 O7 153.00(5) . 2_677 ? O13 Mo4 O7 86.92(5) . 2_677 ? O16 Mo4 O7 84.94(6) 2_677 2_677 ? O15 Mo4 O12 178.55(5) . . ? O14 Mo4 O12 77.24(4) . . ? O13 Mo4 O12 76.94(4) . . ? O16 Mo4 O12 76.47(4) 2_677 . ? O7 Mo4 O12 75.83(4) 2_677 . ? C1 O1 Mo1 118.82(10) . . ? C9 O2 Mo1 132.83(10) . . ? C15 O5 Mo1 146.12(13) . . ? C11 O6 C14 118.28(15) . . ? Mo3 O7 Mo4 117.21(6) . 2_677 ? Mo3 O8 Mo2 116.81(6) . . ? Mo2 O10 Mo3 116.46(6) . 2_677 ? Mo4 O12 Mo4 179.999(2) 2_677 . ? Mo4 O12 Mo2 89.916(6) 2_677 2_677 ? Mo4 O12 Mo2 90.085(6) . 2_677 ? Mo4 O12 Mo2 90.085(6) 2_677 . ? Mo4 O12 Mo2 89.914(6) . . ? Mo2 O12 Mo2 180.0 2_677 . ? Mo4 O12 Mo3 90.263(6) 2_677 . ? Mo4 O12 Mo3 89.737(6) . . ? Mo2 O12 Mo3 89.937(6) 2_677 . ? Mo2 O12 Mo3 90.062(6) . . ? Mo4 O12 Mo3 89.738(6) 2_677 2_677 ? Mo4 O12 Mo3 90.263(6) . 2_677 ? Mo2 O12 Mo3 90.063(5) 2_677 2_677 ? Mo2 O12 Mo3 89.938(6) . 2_677 ? Mo3 O12 Mo3 179.999(1) . 2_677 ? Mo4 O13 Mo2 116.88(6) . . ? Mo4 O14 Mo3 116.57(6) . . ? Mo2 O16 Mo4 116.33(6) . 2_677 ? C7 N1 N2 115.54(13) . . ? C7 N1 Mo1 127.93(11) . . ? N2 N1 Mo1 116.17(10) . . ? C1 N2 N1 108.45(13) . . ? C4 N3 C5 122.84(14) . . ? N2 C1 O1 124.52(14) . . ? N2 C1 C2 118.19(14) . . ? O1 C1 C2 117.24(14) . . ? C3 C2 C6 119.53(15) . . ? C3 C2 C1 119.91(14) . . ? C6 C2 C1 120.51(14) . . ? C4 C3 C2 119.23(15) . . ? N3 C4 C3 119.58(15) . . ? N3 C5 C6 119.89(15) . . ? C5 C6 C2 118.86(15) . . ? N1 C7 C8 123.39(15) . . ? C9 C8 C13 118.31(15) . . ? C9 C8 C7 123.70(15) . . ? C13 C8 C7 117.95(15) . . ? O2 C9 C10 117.47(15) . . ? O2 C9 C8 121.92(14) . . ? C10 C9 C8 120.54(15) . . ? C11 C10 C9 119.22(16) . . ? O6 C11 C10 124.64(17) . . ? O6 C11 C12 114.40(16) . . ? C10 C11 C12 120.95(15) . . ? C13 C12 C11 119.36(16) . . ? C12 C13 C8 121.59(16) . . ? O5 C15 C16 120.01(18) . . ? O5 C15 C17 122.47(17) . . ? C16 C15 C17 117.53(17) . . ? O17 C18 C20 122.3(6) . . ? O17 C18 C19 121.7(5) . . ? C20 C18 C19 116.0(9) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.393 _refine_diff_density_min -0.558 _refine_diff_density_rms 0.082 data_shelxl _database_code_depnum_ccdc_archive 'CCDC 802262' #TrackingRef '3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; bis(cis-dioxo(2-oxo-4-diethylaminobenzaldehyde isonicotinylhydrazonato- O, N,O)molybdenum(VI)) hexamolybdate aqua (1/4) ; _chemical_name_common ; bis(cis-dioxo(2-oxo-4-diethylaminobenzaldehyde isonicotinylhydrazonato-O, N,O)molybdenum(VI)) hexamolybdate aqua (1/4) ; _chemical_melting_point ? _chemical_formula_moiety '2(C17 H19 Mo N4 O4), Mo6 O19, 2(H2 O), 2(HO)' _chemical_formula_sum 'C34 H44 Mo8 N8 O31' _chemical_formula_weight 1828.29 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 monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.2754(8) _cell_length_b 7.9268(5) _cell_length_c 29.789(2) _cell_angle_alpha 90.00 _cell_angle_beta 94.231(6) _cell_angle_gamma 90.00 _cell_volume 2655.2(3) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 15 _cell_measurement_theta_max 25 _exptl_crystal_description plate _exptl_crystal_colour black _exptl_crystal_size_max 0.56 _exptl_crystal_size_mid 0.31 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.279 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1764 _exptl_absorpt_coefficient_mu 1.927 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.81092 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'Xcalibur CCD' _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23290 _diffrn_reflns_av_R_equivalents 0.0344 _diffrn_reflns_av_sigmaI/netI 0.0350 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -38 _diffrn_reflns_limit_l_max 38 _diffrn_reflns_theta_min 4.26 _diffrn_reflns_theta_max 27.00 _reflns_number_total 5762 _reflns_number_gt 4641 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD (Oxford Diffraction,2003)' _computing_cell_refinement 'CrysAlis RED (Oxford Diffraction,2003)' _computing_data_reduction 'CrysAlis RED (Oxford Diffraction,2003)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON98 (Spek, 1990)' _computing_publication_material 'SHELXL97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0177P)^2^+6.4984P] 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 costr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5762 _refine_ls_number_parameters 394 _refine_ls_number_restraints 29 _refine_ls_R_factor_all 0.0630 _refine_ls_R_factor_gt 0.0444 _refine_ls_wR_factor_ref 0.0796 _refine_ls_wR_factor_gt 0.0758 _refine_ls_goodness_of_fit_ref 1.173 _refine_ls_restrained_S_all 1.175 _refine_ls_shift/su_max 0.002 _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 0.91978(4) 0.24965(6) 0.137899(13) 0.02978(11) Uani 1 1 d . . . Mo2 Mo 0.66687(4) 0.60979(6) 0.969707(14) 0.02817(11) Uani 1 1 d . . . Mo3 Mo 0.61838(4) 0.39699(6) 1.060958(13) 0.02537(11) Uani 1 1 d . . . Mo4 Mo 0.52441(4) 0.24825(6) 0.961758(14) 0.02748(10) Uani 1 1 d . . . O1 O 0.9365(3) 0.2747(4) 0.07218(11) 0.0294(8) Uani 1 1 d . . . O2 O 0.8304(3) 0.1706(5) 0.18598(11) 0.0370(9) Uani 1 1 d . . . O4 O 1.0557(3) 0.1713(6) 0.15400(13) 0.0496(11) Uani 1 1 d . . . O3 O 0.9253(3) 0.4611(5) 0.14870(12) 0.0414(9) Uani 1 1 d . . . O5 O 0.6192(3) 0.2188(4) 1.01922(11) 0.0278(8) Uani 1 1 d . . . O6 O 0.7096(3) 0.3324(5) 1.10595(11) 0.0326(8) Uani 1 1 d . . . O7 O 0.7330(3) 0.5112(5) 1.02369(11) 0.0297(8) Uani 1 1 d . . . O8 O 0.7849(3) 0.6886(5) 0.94500(12) 0.0381(9) Uani 1 1 d . . . O9 O 0.6540(3) 0.3856(4) 0.94434(11) 0.0300(8) Uani 1 1 d . . . O10 O 0.5000 0.5000 1.0000 0.0211(10) Uani 1 2 d S . . O11 O 0.5800(3) 0.6261(4) 1.07890(10) 0.0276(7) Uani 1 1 d . . . O12 O 0.5349(3) 0.6636(4) 0.92438(10) 0.0276(8) Uani 1 1 d . . . O13 O 0.6122(3) 0.7936(4) 1.00365(11) 0.0288(8) Uani 1 1 d . . . O14 O 0.5443(4) 0.0687(4) 0.93356(12) 0.0407(9) Uani 1 1 d . . . N1 N 0.8356(3) 0.0290(5) 0.10422(13) 0.0260(9) Uani 1 1 d . . . N2 N 0.8422(3) 0.0207(5) 0.05772(12) 0.0261(9) Uani 1 1 d . . . N3 N 0.9305(4) 0.2142(6) -0.09336(15) 0.0410(12) Uani 1 1 d . . . H3 H 0.9365 0.2273 -0.1218 0.049 Uiso 1 1 calc R . . C1 C 0.8958(4) 0.1534(6) 0.04447(15) 0.0234(10) Uani 1 1 d . . . C2 C 0.9086(4) 0.1755(6) -0.00430(15) 0.0248(10) Uani 1 1 d . . . C3 C 0.9873(4) 0.2935(6) -0.01941(16) 0.0301(11) Uani 1 1 d . . . H31 H 1.0331 0.3599 0.0009 0.036 Uiso 1 1 calc R . . C4 C 0.9966(5) 0.3109(7) -0.06475(18) 0.0387(13) Uani 1 1 d . . . H4 H 1.0486 0.3896 -0.0755 0.046 Uiso 1 1 calc R . . C5 C 0.8555(5) 0.0982(8) -0.07977(17) 0.0390(13) Uani 1 1 d . . . H5 H 0.8122 0.0318 -0.1009 0.047 Uiso 1 1 calc R . . C6 C 0.8422(4) 0.0766(7) -0.03516(16) 0.0318(12) Uani 1 1 d . . . H6 H 0.7893 -0.0033 -0.0255 0.038 Uiso 1 1 calc R . . C7 C 0.7747(4) -0.0930(6) 0.12151(16) 0.0286(11) Uani 1 1 d . . . H7 H 0.7455 -0.1783 0.1023 0.034 Uiso 1 1 calc R . . C8 C 0.7802(5) 0.0254(7) 0.19834(17) 0.0317(11) Uani 1 1 d . . . C9 C 0.7563(5) 0.0084(8) 0.24250(18) 0.0402(14) Uani 1 1 d . . . H9 H 0.7790 0.0939 0.2627 0.048 Uiso 1 1 calc R . . C10 C 0.6984(7) -0.1349(9) 0.2582(2) 0.060(2) Uani 1 1 d . A . C11 C 0.6650(8) -0.2621(10) 0.2259(2) 0.076(2) Uani 1 1 d . . . H11 H 0.6241 -0.3571 0.2346 0.091 Uiso 1 1 calc R . . C12 C 0.6925(6) -0.2456(9) 0.1823(2) 0.0550(17) Uani 1 1 d . . . H12 H 0.6718 -0.3321 0.1621 0.066 Uiso 1 1 calc R . . C13 C 0.7508(5) -0.1036(7) 0.16678(16) 0.0343(12) Uani 1 1 d . . . N4 N 0.6737(7) -0.1478(7) 0.30154(19) 0.092(3) Uani 1 1 d D . . C14 C 0.7161(7) -0.0191(9) 0.3358(2) 0.064(2) Uani 1 1 d D A . H14A H 0.7203 -0.0692 0.3656 0.077 Uiso 1 1 calc R . . H14B H 0.7952 0.0187 0.3298 0.077 Uiso 1 1 calc R . . C15 C 0.6346(7) 0.1245(12) 0.3342(3) 0.092(3) Uani 1 1 d D . . H15A H 0.6619 0.2060 0.3565 0.138 Uiso 1 1 calc R A . H15B H 0.5565 0.0866 0.3402 0.138 Uiso 1 1 calc R . . H15C H 0.6320 0.1752 0.3049 0.138 Uiso 1 1 calc R . . C16A C 0.6407(11) -0.3161(15) 0.3226(4) 0.065(5) Uani 0.60(2) 1 d PDU A 1 H16A H 0.6769 -0.4095 0.3075 0.078 Uiso 0.60(2) 1 calc PR A 1 H16B H 0.6670 -0.3191 0.3543 0.078 Uiso 0.60(2) 1 calc PR A 1 C17A C 0.5099(11) -0.325(2) 0.3163(5) 0.099(8) Uani 0.60(2) 1 d PDU A 1 H17A H 0.4832 -0.4294 0.3286 0.149 Uiso 0.60(2) 1 calc PR A 1 H17B H 0.4856 -0.3207 0.2847 0.149 Uiso 0.60(2) 1 calc PR A 1 H17C H 0.4758 -0.2322 0.3314 0.149 Uiso 0.60(2) 1 calc PR A 1 C16B C 0.5591(12) -0.240(2) 0.3121(5) 0.058(7) Uani 0.40(2) 1 d PDU A 2 H16C H 0.5175 -0.1782 0.3341 0.070 Uiso 0.40(2) 1 calc PR A 2 H16D H 0.5066 -0.2537 0.2850 0.070 Uiso 0.40(2) 1 calc PR A 2 C17B C 0.597(2) -0.406(2) 0.3301(8) 0.092(10) Uani 0.40(2) 1 d PDU A 2 H17D H 0.5291 -0.4692 0.3378 0.138 Uiso 0.40(2) 1 calc PR A 2 H17E H 0.6505 -0.3908 0.3565 0.138 Uiso 0.40(2) 1 calc PR A 2 H17F H 0.6376 -0.4666 0.3078 0.138 Uiso 0.40(2) 1 calc PR A 2 O1W O 0.9458(5) 0.2795(7) 0.31454(15) 0.0720(15) Uani 1 1 d U . . O2W O 0.9233(7) 0.5482(12) 0.2491(3) 0.153(3) Uiso 1 1 d . . . H11W H 0.9114 0.3730 0.3038 0.229 Uiso 1 1 d . . . H21W H 0.9301 0.5116 0.2227 0.229 Uiso 1 1 d . . . H12W H 0.9673 0.2215 0.2911 0.229 Uiso 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 0.0365(2) 0.0286(2) 0.0239(2) -0.0010(2) -0.00009(17) -0.0071(2) Mo2 0.0248(2) 0.0325(3) 0.0277(2) 0.0022(2) 0.00495(16) -0.0060(2) Mo3 0.0267(2) 0.0265(2) 0.0223(2) 0.00201(19) -0.00195(16) 0.00389(19) Mo4 0.0340(2) 0.0210(2) 0.0272(2) -0.00344(19) 0.00055(17) 0.0026(2) O1 0.0305(18) 0.031(2) 0.0272(17) -0.0028(15) 0.0043(14) -0.0046(15) O2 0.057(2) 0.031(2) 0.0235(18) -0.0002(16) 0.0063(16) -0.0104(18) O4 0.042(2) 0.059(3) 0.046(2) 0.002(2) -0.0096(18) 0.002(2) O3 0.061(3) 0.031(2) 0.033(2) -0.0030(17) 0.0049(18) -0.0102(19) O5 0.0357(19) 0.0178(18) 0.0297(17) 0.0017(14) 0.0010(14) 0.0077(14) O6 0.0322(19) 0.038(2) 0.0269(18) 0.0056(16) -0.0033(14) 0.0030(16) O7 0.0231(17) 0.037(2) 0.0286(18) 0.0056(16) 0.0001(14) 0.0013(15) O8 0.0304(19) 0.049(2) 0.035(2) 0.0065(18) 0.0067(15) -0.0108(18) O9 0.0295(18) 0.0291(19) 0.0321(18) -0.0006(16) 0.0074(14) 0.0056(16) O10 0.020(2) 0.023(2) 0.021(2) 0.0014(19) 0.0012(17) -0.0006(18) O11 0.0320(18) 0.0253(19) 0.0249(16) -0.0030(15) -0.0019(13) 0.0000(15) O12 0.0288(18) 0.0290(19) 0.0249(17) 0.0051(15) 0.0024(14) -0.0021(15) O13 0.0348(19) 0.0224(19) 0.0290(18) 0.0011(14) 0.0006(14) -0.0066(14) O14 0.062(3) 0.021(2) 0.039(2) -0.0075(16) 0.0024(18) 0.0072(18) N1 0.029(2) 0.027(2) 0.0215(19) -0.0011(18) 0.0029(16) 0.0021(18) N2 0.027(2) 0.030(2) 0.0208(19) -0.0028(17) 0.0031(16) 0.0013(18) N3 0.053(3) 0.045(3) 0.025(2) 0.004(2) 0.004(2) 0.015(2) C1 0.019(2) 0.026(3) 0.026(2) -0.002(2) 0.0020(18) 0.0050(19) C2 0.023(2) 0.026(2) 0.026(2) 0.000(2) 0.0025(19) 0.010(2) C3 0.030(3) 0.028(3) 0.032(3) 0.000(2) 0.003(2) 0.003(2) C4 0.042(3) 0.036(3) 0.039(3) 0.006(3) 0.008(2) 0.005(3) C5 0.041(3) 0.043(3) 0.032(3) -0.006(3) -0.004(2) 0.005(3) C6 0.033(3) 0.032(3) 0.031(3) -0.001(2) 0.000(2) 0.005(2) C7 0.030(3) 0.026(3) 0.029(2) -0.005(2) 0.003(2) -0.007(2) C8 0.035(3) 0.030(3) 0.029(3) 0.002(2) 0.002(2) -0.004(2) C9 0.048(3) 0.044(4) 0.028(3) -0.007(3) 0.005(2) -0.011(3) C10 0.088(5) 0.063(5) 0.033(3) -0.004(3) 0.021(3) -0.034(4) C11 0.117(7) 0.067(5) 0.047(4) -0.008(4) 0.029(4) -0.055(5) C12 0.078(5) 0.050(4) 0.038(3) -0.008(3) 0.017(3) -0.033(4) C13 0.040(3) 0.036(3) 0.028(3) 0.003(2) 0.007(2) -0.006(3) N4 0.160(7) 0.082(5) 0.039(3) -0.012(3) 0.044(4) -0.072(5) C14 0.090(6) 0.069(5) 0.033(3) 0.000(3) 0.016(3) -0.016(4) C15 0.080(6) 0.144(9) 0.054(5) 0.006(6) 0.018(4) -0.003(6) C16A 0.073(9) 0.080(12) 0.043(7) 0.001(7) 0.010(6) -0.013(8) C17A 0.063(9) 0.17(2) 0.063(10) -0.027(12) 0.025(8) -0.055(11) C16B 0.064(17) 0.083(15) 0.028(8) -0.001(9) 0.014(9) -0.027(11) C17B 0.14(3) 0.067(16) 0.073(15) 0.018(13) 0.021(16) -0.037(16) O1W 0.094(4) 0.080(4) 0.042(3) -0.014(3) 0.008(2) -0.012(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 1.690(4) . ? Mo1 O3 1.707(4) . ? Mo1 O2 1.917(3) . ? Mo1 O1 1.990(3) . ? Mo1 N1 2.197(4) . ? Mo2 O8 1.688(3) . ? Mo2 O7 1.891(3) . ? Mo2 O13 1.902(3) . ? Mo2 O9 1.932(4) . ? Mo2 O12 1.981(3) . ? Mo2 O10 2.3157(4) . ? Mo3 O6 1.707(3) . ? Mo3 O12 1.876(3) 3_667 ? Mo3 O5 1.882(3) . ? Mo3 O11 1.951(3) . ? Mo3 O7 1.983(3) . ? Mo3 O10 2.3213(4) . ? Mo4 O14 1.676(3) . ? Mo4 O11 1.906(3) 3_667 ? Mo4 O9 1.923(3) . ? Mo4 O13 1.944(3) 3_667 ? Mo4 O5 1.964(3) . ? Mo4 O10 2.3243(4) . ? O1 C1 1.327(5) . ? O2 C8 1.346(6) . ? O10 Mo2 2.3157(4) 3_667 ? O10 Mo3 2.3212(4) 3_667 ? O10 Mo4 2.3242(4) 3_667 ? O11 Mo4 1.906(3) 3_667 ? O12 Mo3 1.876(3) 3_667 ? O13 Mo4 1.944(3) 3_667 ? N1 C7 1.313(6) . ? N1 N2 1.394(5) . ? N2 C1 1.289(6) . ? N3 C4 1.332(7) . ? N3 C5 1.333(7) . ? C1 C2 1.481(6) . ? C2 C6 1.385(7) . ? C2 C3 1.387(7) . ? C3 C4 1.369(7) . ? C5 C6 1.359(7) . ? C7 C13 1.397(7) . ? C8 C9 1.369(7) . ? C8 C13 1.412(7) . ? C9 C10 1.407(8) . ? C10 N4 1.346(7) . ? C10 C11 1.425(9) . ? C11 C12 1.362(8) . ? C12 C13 1.399(8) . ? N4 C14 1.497(7) . ? N4 C16A 1.531(9) . ? N4 C16B 1.538(10) . ? C14 C15 1.462(9) . ? C16A C17A 1.475(10) . ? C16B C17B 1.471(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 O4 Mo1 O3 106.7(2) . . ? O4 Mo1 O2 100.59(19) . . ? O3 Mo1 O2 101.18(17) . . ? O4 Mo1 O1 99.56(17) . . ? O3 Mo1 O1 94.75(16) . . ? O2 Mo1 O1 149.40(14) . . ? O4 Mo1 N1 100.91(18) . . ? O3 Mo1 N1 151.20(17) . . ? O2 Mo1 N1 81.24(15) . . ? O1 Mo1 N1 72.49(14) . . ? O8 Mo2 O7 104.46(16) . . ? O8 Mo2 O13 104.19(17) . . ? O7 Mo2 O13 89.28(14) . . ? O8 Mo2 O9 102.07(17) . . ? O7 Mo2 O9 88.05(15) . . ? O13 Mo2 O9 153.44(14) . . ? O8 Mo2 O12 101.54(15) . . ? O7 Mo2 O12 153.90(14) . . ? O13 Mo2 O12 86.60(14) . . ? O9 Mo2 O12 84.28(14) . . ? O8 Mo2 O10 177.08(12) . . ? O7 Mo2 O10 78.11(10) . . ? O13 Mo2 O10 77.07(10) . . ? O9 Mo2 O10 76.51(10) . . ? O12 Mo2 O10 75.84(9) . . ? O6 Mo3 O12 104.64(15) . 3_667 ? O6 Mo3 O5 105.17(16) . . ? O12 Mo3 O5 90.62(15) 3_667 . ? O6 Mo3 O11 101.37(15) . . ? O12 Mo3 O11 86.99(14) 3_667 . ? O5 Mo3 O11 153.07(13) . . ? O6 Mo3 O7 101.33(15) . . ? O12 Mo3 O7 153.72(13) 3_667 . ? O5 Mo3 O7 86.43(15) . . ? O11 Mo3 O7 84.01(14) . . ? O6 Mo3 O10 176.63(13) . . ? O12 Mo3 O10 77.63(10) 3_667 . ? O5 Mo3 O10 77.15(9) . . ? O11 Mo3 O10 76.14(9) . . ? O7 Mo3 O10 76.26(9) . . ? O14 Mo4 O11 102.97(16) . 3_667 ? O14 Mo4 O9 102.29(17) . . ? O11 Mo4 O9 88.76(14) 3_667 . ? O14 Mo4 O13 105.16(17) . 3_667 ? O11 Mo4 O13 87.13(14) 3_667 3_667 ? O9 Mo4 O13 152.48(14) . 3_667 ? O14 Mo4 O5 104.58(16) . . ? O11 Mo4 O5 152.45(14) 3_667 . ? O9 Mo4 O5 85.83(14) . . ? O13 Mo4 O5 85.36(14) 3_667 . ? O14 Mo4 O10 178.74(14) . . ? O11 Mo4 O10 76.87(10) 3_667 . ? O9 Mo4 O10 76.47(10) . . ? O13 Mo4 O10 76.10(10) 3_667 . ? O5 Mo4 O10 75.60(9) . . ? C1 O1 Mo1 119.1(3) . . ? C8 O2 Mo1 137.6(3) . . ? Mo3 O5 Mo4 117.25(15) . . ? Mo2 O7 Mo3 115.61(15) . . ? Mo4 O9 Mo2 116.86(16) . . ? Mo2 O10 Mo2 179.998(1) . 3_667 ? Mo2 O10 Mo3 89.989(16) . 3_667 ? Mo2 O10 Mo3 90.013(16) 3_667 3_667 ? Mo2 O10 Mo3 90.011(16) . . ? Mo2 O10 Mo3 89.987(16) 3_667 . ? Mo3 O10 Mo3 180.0 3_667 . ? Mo2 O10 Mo4 89.845(17) . 3_667 ? Mo2 O10 Mo4 90.153(17) 3_667 3_667 ? Mo3 O10 Mo4 89.960(15) 3_667 3_667 ? Mo3 O10 Mo4 90.038(16) . 3_667 ? Mo2 O10 Mo4 90.154(17) . . ? Mo2 O10 Mo4 89.848(17) 3_667 . ? Mo3 O10 Mo4 90.039(16) 3_667 . ? Mo3 O10 Mo4 89.963(16) . . ? Mo4 O10 Mo4 180.0 3_667 . ? Mo4 O11 Mo3 116.84(15) 3_667 . ? Mo3 O12 Mo2 116.41(16) 3_667 . ? Mo2 O13 Mo4 116.84(16) . 3_667 ? C7 N1 N2 115.0(4) . . ? C7 N1 Mo1 128.9(3) . . ? N2 N1 Mo1 116.0(3) . . ? C1 N2 N1 109.0(4) . . ? C4 N3 C5 122.7(5) . . ? N2 C1 O1 123.3(4) . . ? N2 C1 C2 118.6(4) . . ? O1 C1 C2 118.1(4) . . ? C6 C2 C3 119.6(5) . . ? C6 C2 C1 119.8(5) . . ? C3 C2 C1 120.6(4) . . ? C4 C3 C2 119.0(5) . . ? N3 C4 C3 119.6(5) . . ? N3 C5 C6 120.1(5) . . ? C5 C6 C2 119.0(5) . . ? N1 C7 C13 124.5(5) . . ? O2 C8 C9 117.6(5) . . ? O2 C8 C13 121.3(4) . . ? C9 C8 C13 121.0(5) . . ? C8 C9 C10 121.9(5) . . ? N4 C10 C9 120.9(6) . . ? N4 C10 C11 122.1(6) . . ? C9 C10 C11 116.9(5) . . ? C12 C11 C10 120.5(6) . . ? C11 C12 C13 122.5(6) . . ? C7 C13 C12 119.8(5) . . ? C7 C13 C8 123.1(5) . . ? C12 C13 C8 117.1(5) . . ? C10 N4 C14 121.7(5) . . ? C10 N4 C16A 122.2(7) . . ? C14 N4 C16A 112.9(7) . . ? C10 N4 C16B 118.0(8) . . ? C14 N4 C16B 114.6(8) . . ? C16A N4 C16B 42.9(8) . . ? C15 C14 N4 109.9(6) . . ? C17A C16A N4 105.2(7) . . ? C17B C16B N4 105.8(8) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.783 _refine_diff_density_min -0.712 _refine_diff_density_rms 0.106 # Attachment '3b.cif' data_3b _database_code_depnum_ccdc_archive 'CCDC 802263' #TrackingRef '3b.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; bis(aqua cis-dioxo(2-oxo-4-diethylaminobenzaldehyde isonicotinylhydrazonato- O, N, O)molybdenum(VI)) hexamolybdate acetone solvate (1/4) ; _chemical_name_common ; bis(aqua cis-dioxo(2-oxo-4-diethylaminobenzaldehyde isonicotinylhydrazonato-O, N, O)molybdenum(VI)) hexamolybdate acetone solvate (1/4) ; _chemical_melting_point ? _chemical_formula_moiety '2(C17 H21 Mo N4 O5), Mo6 O19, 4(C3 H6 O)' _chemical_formula_sum 'C46 H66 Mo8 N8 O33' _chemical_formula_weight 2026.59 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 triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.2570(2) _cell_length_b 10.4104(2) _cell_length_c 15.5335(3) _cell_angle_alpha 91.9350(10) _cell_angle_beta 97.170(2) _cell_angle_gamma 95.1900(10) _cell_volume 1637.24(5) _cell_formula_units_Z 1 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 15 _cell_measurement_theta_max 25 _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.7 _exptl_crystal_size_mid 0.5 _exptl_crystal_size_min 0.3 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.055 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 998 _exptl_absorpt_coefficient_mu 1.576 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.77749 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'Xcalibur CCD' _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19653 _diffrn_reflns_av_R_equivalents 0.0105 _diffrn_reflns_av_sigmaI/netI 0.0085 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 4.19 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5749 _reflns_number_gt 5510 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD (Oxford Diffraction,2003)' _computing_cell_refinement 'CrysAlis RED (Oxford Diffraction,2003)' _computing_data_reduction 'CrysAlis RED (Oxford Diffraction,2003)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON98 (Spek, 1990)' _computing_publication_material 'SHELXL97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0241P)^2^+2.8737P] 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 SHELXL _refine_ls_extinction_coef 0.0044(2) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 5749 _refine_ls_number_parameters 439 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0209 _refine_ls_R_factor_gt 0.0197 _refine_ls_wR_factor_ref 0.0507 _refine_ls_wR_factor_gt 0.0501 _refine_ls_goodness_of_fit_ref 1.055 _refine_ls_restrained_S_all 1.055 _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 N1 N 0.6434(2) 0.13316(19) 0.01689(13) 0.0166(4) Uani 1 1 d . . . N2 N 0.6454(2) 0.02048(19) 0.06232(13) 0.0185(4) Uani 1 1 d . . . O10 O 0.0000 0.0000 0.5000 0.0137(5) Uani 1 2 d S . . O7 O 0.5378(2) 0.50749(18) 0.39042(13) 0.0286(4) Uani 1 1 d . . . O14 O 0.35864(18) -0.00862(19) 0.42399(13) 0.0263(4) Uani 1 1 d . . . O8 O 0.10617(17) 0.07216(18) 0.36017(11) 0.0215(4) Uani 1 1 d . . . O17 O -0.12962(18) 0.15126(18) 0.27488(12) 0.0258(4) Uani 1 1 d . . . O9 O -0.11322(18) -0.09299(17) 0.34470(11) 0.0216(4) Uani 1 1 d . . . O13 O -0.1060(2) -0.35350(18) 0.39164(13) 0.0289(4) Uani 1 1 d . . . O12 O -0.21754(17) -0.16216(16) 0.48494(12) 0.0203(4) Uani 1 1 d . . . O16 O -0.01445(17) 0.23781(16) 0.44729(12) 0.0206(4) Uani 1 1 d . . . O15 O -0.22831(16) 0.07787(16) 0.43244(11) 0.0188(4) Uani 1 1 d . . . O11 O 0.11619(17) -0.16674(17) 0.41022(11) 0.0211(4) Uani 1 1 d . . . O5 O 0.8033(2) 0.3136(2) 0.13327(15) 0.0255(4) Uani 1 1 d . . . O3 O 0.57529(18) 0.41745(16) 0.16253(11) 0.0207(4) Uani 1 1 d . . . O4 O 0.40805(18) 0.27048(17) 0.04284(11) 0.0220(4) Uani 1 1 d . . . O2 O 0.63683(18) 0.38787(16) -0.01048(11) 0.0199(4) Uani 1 1 d . . . O1 O 0.57570(17) 0.15361(15) 0.16602(11) 0.0179(4) Uani 1 1 d . . . N3 N 0.5827(2) -0.2719(2) 0.30107(14) 0.0202(4) Uani 1 1 d . . . H30 H 0.5772 -0.3361 0.3343 0.024 Uiso 1 1 calc R . . C2 C 0.6010(2) -0.0680(2) 0.19615(16) 0.0159(5) Uani 1 1 d . . . C9 C 0.6817(2) 0.3613(2) -0.08633(15) 0.0154(5) Uani 1 1 d . . . C4 C 0.5554(2) -0.1565(2) 0.33012(17) 0.0199(5) Uani 1 1 d . . . H4 H 0.5307 -0.1468 0.3854 0.024 Uiso 1 1 calc R . . C3 C 0.5638(2) -0.0517(2) 0.27863(16) 0.0181(5) Uani 1 1 d . . . H3 H 0.5447 0.0288 0.2987 0.022 Uiso 1 1 calc R . . C13 C 0.7607(3) 0.2183(2) -0.18943(16) 0.0208(5) Uani 1 1 d . . . H13 H 0.7762 0.1358 -0.2079 0.025 Uiso 1 1 calc R . . C8 C 0.7062(2) 0.2337(2) -0.11081(16) 0.0176(5) Uani 1 1 d . . . C11 C 0.7650(2) 0.4466(2) -0.21452(16) 0.0192(5) Uani 1 1 d . . . C7 C 0.6884(2) 0.1278(2) -0.05802(16) 0.0181(5) Uani 1 1 d . . . H7 H 0.7104 0.0483 -0.0780 0.022 Uiso 1 1 calc R . . C10 C 0.7070(2) 0.4633(2) -0.13758(15) 0.0176(5) Uani 1 1 d . . . H10 H 0.6856 0.5448 -0.1213 0.021 Uiso 1 1 calc R . . C1 C 0.6084(2) 0.0410(2) 0.13769(16) 0.0165(5) Uani 1 1 d . . . C6 C 0.6285(3) -0.1904(2) 0.16798(17) 0.0207(5) Uani 1 1 d . . . H6 H 0.6535 -0.2033 0.1131 0.025 Uiso 1 1 calc R . . C5 C 0.6183(3) -0.2912(2) 0.22185(17) 0.0220(5) Uani 1 1 d . . . H5 H 0.6360 -0.3730 0.2035 0.026 Uiso 1 1 calc R . . C12 C 0.7913(3) 0.3191(2) -0.23915(16) 0.0210(5) Uani 1 1 d . . . H12 H 0.8297 0.3049 -0.2894 0.025 Uiso 1 1 calc R . . C16 C 0.8847(3) 0.5394(3) -0.32924(17) 0.0255(6) Uani 1 1 d . . . H16A H 0.9471 0.4775 -0.3121 0.031 Uiso 1 1 calc R . . H16B H 0.9343 0.6228 -0.3316 0.031 Uiso 1 1 calc R . . N4 N 0.7948(2) 0.5480(2) -0.26302(15) 0.0262(5) Uani 1 1 d . . . C14 C 0.7360(3) 0.6716(3) -0.25371(18) 0.0292(6) Uani 1 1 d . . . H14A H 0.6495 0.6545 -0.2352 0.035 Uiso 1 1 calc R . . H14B H 0.7244 0.7099 -0.3099 0.035 Uiso 1 1 calc R . . C15 C 0.8192(3) 0.7666(3) -0.1894(2) 0.0385(7) Uani 1 1 d . . . H15A H 0.7767 0.8448 -0.1859 0.058 Uiso 1 1 calc R . . H15B H 0.9044 0.7855 -0.2079 0.058 Uiso 1 1 calc R . . H15C H 0.8294 0.7301 -0.1333 0.058 Uiso 1 1 calc R . . C17 C 0.8144(3) 0.4996(3) -0.41873(18) 0.0319(7) Uani 1 1 d . . . H17A H 0.8779 0.4960 -0.4590 0.048 Uiso 1 1 calc R . . H17B H 0.7537 0.5615 -0.4368 0.048 Uiso 1 1 calc R . . H17C H 0.7669 0.4161 -0.4173 0.048 Uiso 1 1 calc R . . C23 C 0.7039(3) 0.3776(3) 0.35366(18) 0.0257(6) Uani 1 1 d . . . H23A H 0.7334 0.4521 0.3240 0.039 Uiso 1 1 calc R . . H23B H 0.6811 0.3055 0.3127 0.039 Uiso 1 1 calc R . . H23C H 0.7733 0.3576 0.3971 0.039 Uiso 1 1 calc R . . C21 C 0.5860(3) 0.4048(2) 0.39577(17) 0.0222(5) Uani 1 1 d . . . C22 C 0.5265(3) 0.2978(3) 0.4452(2) 0.0323(7) Uani 1 1 d . . . H22A H 0.4516 0.3258 0.4694 0.049 Uiso 1 1 calc R . . H22B H 0.5910 0.2756 0.4912 0.049 Uiso 1 1 calc R . . H22C H 0.4990 0.2236 0.4067 0.049 Uiso 1 1 calc R . . Mo3 Mo -0.07377(2) 0.08345(2) 0.368217(13) 0.01709(7) Uani 1 1 d . . . Mo2 Mo -0.06006(2) -0.20707(2) 0.440576(14) 0.01751(7) Uani 1 1 d . . . Mo1 Mo 0.56989(2) 0.299086(18) 0.083135(13) 0.01390(7) Uani 1 1 d . . . Mo4 Mo 0.20847(2) -0.00661(2) 0.457129(14) 0.01721(7) Uani 1 1 d . . . O6 O 0.9681(3) 0.2564(9) 0.0113(2) 0.230(4) Uani 1 1 d . . . C18 C 1.0351(4) 0.2534(9) -0.0454(3) 0.103(3) Uani 1 1 d . . . C19 C 1.1019(5) 0.3693(5) -0.0800(4) 0.0853(18) Uani 1 1 d . . . H19A H 1.0852 0.4451 -0.0477 0.128 Uiso 1 1 calc R . . H19B H 1.0686 0.3755 -0.1401 0.128 Uiso 1 1 calc R . . H19C H 1.1953 0.3624 -0.0744 0.128 Uiso 1 1 calc R . . C20 C 1.0567(5) 0.1266(6) -0.0889(5) 0.117(3) Uani 1 1 d . . . H20A H 1.0116 0.0570 -0.0620 0.175 Uiso 1 1 calc R . . H20B H 1.1494 0.1165 -0.0829 0.175 Uiso 1 1 calc R . . H20C H 1.0228 0.1257 -0.1494 0.175 Uiso 1 1 calc R . . HW1 H 0.824(4) 0.271(4) 0.172(3) 0.045(11) Uiso 1 1 d . . . HW2 H 0.844(3) 0.297(3) 0.099(2) 0.027(10) Uiso 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 N1 0.0216(11) 0.0115(10) 0.0178(10) 0.0024(8) 0.0058(8) 0.0032(8) N2 0.0256(11) 0.0118(10) 0.0196(11) 0.0033(8) 0.0068(9) 0.0041(8) O10 0.0146(11) 0.0123(11) 0.0147(11) 0.0008(9) 0.0037(9) 0.0019(9) O7 0.0384(11) 0.0178(9) 0.0323(11) 0.0078(8) 0.0096(9) 0.0079(8) O14 0.0189(9) 0.0311(10) 0.0315(10) 0.0041(8) 0.0104(8) 0.0054(8) O8 0.0217(9) 0.0279(10) 0.0171(9) 0.0077(7) 0.0081(7) 0.0041(7) O17 0.0274(10) 0.0306(10) 0.0206(9) 0.0100(8) 0.0030(8) 0.0070(8) O9 0.0245(9) 0.0228(9) 0.0167(9) -0.0004(7) -0.0003(7) 0.0032(7) O13 0.0319(11) 0.0184(9) 0.0353(11) -0.0054(8) 0.0033(9) 0.0005(8) O12 0.0164(9) 0.0178(9) 0.0270(9) 0.0027(7) 0.0045(7) 0.0001(7) O16 0.0232(9) 0.0144(8) 0.0250(9) 0.0062(7) 0.0034(7) 0.0035(7) O15 0.0165(8) 0.0202(9) 0.0206(9) 0.0042(7) 0.0025(7) 0.0053(7) O11 0.0221(9) 0.0189(9) 0.0236(9) -0.0037(7) 0.0076(7) 0.0054(7) O5 0.0229(10) 0.0303(11) 0.0245(11) 0.0101(9) 0.0040(9) 0.0048(8) O3 0.0322(10) 0.0137(8) 0.0171(9) 0.0001(7) 0.0050(7) 0.0052(7) O4 0.0245(9) 0.0215(9) 0.0206(9) -0.0002(7) 0.0040(7) 0.0049(7) O2 0.0314(10) 0.0149(8) 0.0166(8) 0.0037(7) 0.0111(7) 0.0075(7) O1 0.0266(9) 0.0119(8) 0.0173(8) 0.0023(7) 0.0079(7) 0.0046(7) N3 0.0217(11) 0.0140(10) 0.0251(11) 0.0085(9) 0.0027(9) 0.0008(8) C2 0.0151(11) 0.0137(11) 0.0184(12) 0.0014(9) 0.0004(9) 0.0003(9) C9 0.0151(11) 0.0177(12) 0.0143(11) 0.0005(9) 0.0036(9) 0.0038(9) C4 0.0189(12) 0.0212(13) 0.0206(12) 0.0043(10) 0.0048(10) 0.0032(10) C3 0.0185(12) 0.0140(12) 0.0225(13) 0.0012(10) 0.0041(10) 0.0029(9) C13 0.0252(13) 0.0193(13) 0.0191(12) -0.0023(10) 0.0057(10) 0.0067(10) C8 0.0190(12) 0.0170(12) 0.0176(12) 0.0005(9) 0.0042(10) 0.0037(9) C11 0.0209(13) 0.0213(13) 0.0168(12) 0.0036(10) 0.0049(10) 0.0043(10) C7 0.0217(13) 0.0140(12) 0.0199(12) -0.0015(9) 0.0055(10) 0.0046(10) C10 0.0221(13) 0.0162(12) 0.0163(12) 0.0025(9) 0.0058(10) 0.0061(10) C1 0.0169(12) 0.0121(11) 0.0205(12) 0.0009(9) 0.0028(9) 0.0011(9) C6 0.0261(13) 0.0172(12) 0.0191(12) 0.0000(10) 0.0039(10) 0.0031(10) C5 0.0277(14) 0.0132(12) 0.0244(13) -0.0012(10) 0.0009(11) 0.0026(10) C12 0.0251(13) 0.0241(13) 0.0161(12) 0.0015(10) 0.0092(10) 0.0055(10) C16 0.0309(15) 0.0254(14) 0.0228(13) 0.0046(11) 0.0140(11) 0.0016(11) N4 0.0380(14) 0.0230(12) 0.0217(11) 0.0063(9) 0.0159(10) 0.0063(10) C14 0.0373(16) 0.0284(15) 0.0240(14) 0.0070(11) 0.0098(12) 0.0034(12) C15 0.0471(19) 0.0372(17) 0.0320(16) 0.0014(13) 0.0125(14) -0.0025(14) C17 0.0427(18) 0.0322(16) 0.0231(14) 0.0047(12) 0.0096(13) 0.0069(13) C23 0.0286(14) 0.0228(14) 0.0255(14) 0.0021(11) 0.0011(11) 0.0039(11) C21 0.0288(14) 0.0168(13) 0.0197(13) 0.0013(10) -0.0022(11) 0.0018(11) C22 0.0355(16) 0.0221(14) 0.0415(17) 0.0115(12) 0.0090(13) 0.0046(12) Mo3 0.01944(12) 0.01827(12) 0.01436(11) 0.00554(8) 0.00232(8) 0.00414(8) Mo2 0.02075(12) 0.01235(11) 0.01953(12) -0.00087(8) 0.00342(8) 0.00148(8) Mo1 0.01987(12) 0.01064(11) 0.01273(11) 0.00130(7) 0.00567(8) 0.00459(8) Mo4 0.01424(11) 0.01927(12) 0.01991(12) 0.00280(8) 0.00717(8) 0.00375(8) O6 0.0341(19) 0.626(14) 0.0368(19) 0.011(4) 0.0062(15) 0.074(4) C18 0.0182(19) 0.265(9) 0.033(2) 0.017(3) 0.0036(16) 0.043(3) C19 0.049(3) 0.089(4) 0.112(4) -0.048(3) -0.014(3) 0.028(3) C20 0.035(2) 0.108(5) 0.220(8) 0.096(5) 0.034(4) 0.023(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 N1 C7 1.306(3) . ? N1 N2 1.390(3) . ? N1 Mo1 2.218(2) . ? N2 C1 1.292(3) . ? O10 Mo2 2.3156(2) . ? O10 Mo2 2.3156(2) 2_556 ? O10 Mo3 2.3173(2) 2_556 ? O10 Mo3 2.3173(2) . ? O10 Mo4 2.3236(2) 2_556 ? O10 Mo4 2.3237(2) . ? O7 C21 1.219(3) . ? O14 Mo4 1.6855(18) . ? O8 Mo3 1.8793(17) . ? O8 Mo4 1.9714(17) . ? O17 Mo3 1.6922(17) . ? O9 Mo3 1.8586(18) . ? O9 Mo2 1.9898(18) . ? O13 Mo2 1.6810(18) . ? O12 Mo2 1.9222(17) . ? O12 Mo4 1.9360(18) 2_556 ? O16 Mo2 1.8629(18) 2_556 ? O16 Mo3 1.9911(18) . ? O15 Mo4 1.8869(17) 2_556 ? O15 Mo3 1.9731(17) . ? O11 Mo4 1.9148(17) . ? O11 Mo2 1.9379(17) . ? O5 Mo1 2.413(2) . ? O3 Mo1 1.7060(17) . ? O4 Mo1 1.6955(18) . ? O2 C9 1.346(3) . ? O2 Mo1 1.9146(16) . ? O1 C1 1.324(3) . ? O1 Mo1 2.0208(16) . ? N3 C4 1.335(3) . ? N3 C5 1.340(3) . ? C2 C3 1.391(3) . ? C2 C6 1.397(3) . ? C2 C1 1.480(3) . ? C9 C10 1.374(3) . ? C9 C8 1.422(3) . ? C4 C3 1.377(4) . ? C13 C12 1.361(4) . ? C13 C8 1.415(3) . ? C8 C7 1.408(3) . ? C11 N4 1.352(3) . ? C11 C10 1.412(3) . ? C11 C12 1.427(4) . ? C6 C5 1.369(4) . ? C16 N4 1.470(3) . ? C16 C17 1.510(4) . ? N4 C14 1.480(4) . ? C14 C15 1.508(4) . ? C23 C21 1.489(4) . ? C21 C22 1.502(4) . ? Mo2 O16 1.8628(18) 2_556 ? Mo4 O15 1.8869(17) 2_556 ? Mo4 O12 1.9360(18) 2_556 ? O6 C18 1.184(5) . ? C18 C19 1.483(9) . ? C18 C20 1.509(9) . ? 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 C7 N1 N2 115.4(2) . . ? C7 N1 Mo1 128.85(16) . . ? N2 N1 Mo1 115.68(14) . . ? C1 N2 N1 109.48(19) . . ? Mo2 O10 Mo2 180.0 . 2_556 ? Mo2 O10 Mo3 90.187(8) . 2_556 ? Mo2 O10 Mo3 89.814(8) 2_556 2_556 ? Mo2 O10 Mo3 89.814(8) . . ? Mo2 O10 Mo3 90.186(8) 2_556 . ? Mo3 O10 Mo3 180.0 2_556 . ? Mo2 O10 Mo4 90.036(8) . 2_556 ? Mo2 O10 Mo4 89.965(8) 2_556 2_556 ? Mo3 O10 Mo4 89.885(8) 2_556 2_556 ? Mo3 O10 Mo4 90.115(8) . 2_556 ? Mo2 O10 Mo4 89.963(8) . . ? Mo2 O10 Mo4 90.036(8) 2_556 . ? Mo3 O10 Mo4 90.115(8) 2_556 . ? Mo3 O10 Mo4 89.884(7) . . ? Mo4 O10 Mo4 180.0 2_556 . ? Mo3 O8 Mo4 116.70(8) . . ? Mo3 O9 Mo2 116.35(9) . . ? Mo2 O12 Mo4 116.53(8) . 2_556 ? Mo2 O16 Mo3 116.69(8) 2_556 . ? Mo4 O15 Mo3 116.63(8) 2_556 . ? Mo4 O11 Mo2 116.68(8) . . ? C9 O2 Mo1 139.50(15) . . ? C1 O1 Mo1 118.07(15) . . ? C4 N3 C5 122.2(2) . . ? C3 C2 C6 118.9(2) . . ? C3 C2 C1 121.0(2) . . ? C6 C2 C1 120.0(2) . . ? O2 C9 C10 117.2(2) . . ? O2 C9 C8 121.3(2) . . ? C10 C9 C8 121.5(2) . . ? N3 C4 C3 120.3(2) . . ? C4 C3 C2 119.1(2) . . ? C12 C13 C8 122.8(2) . . ? C7 C8 C13 120.1(2) . . ? C7 C8 C9 123.3(2) . . ? C13 C8 C9 116.5(2) . . ? N4 C11 C10 121.1(2) . . ? N4 C11 C12 121.2(2) . . ? C10 C11 C12 117.7(2) . . ? N1 C7 C8 124.7(2) . . ? C9 C10 C11 121.1(2) . . ? N2 C1 O1 124.1(2) . . ? N2 C1 C2 118.2(2) . . ? O1 C1 C2 117.6(2) . . ? C5 C6 C2 119.5(2) . . ? N3 C5 C6 120.0(2) . . ? C13 C12 C11 120.3(2) . . ? N4 C16 C17 113.3(2) . . ? C11 N4 C16 121.4(2) . . ? C11 N4 C14 121.8(2) . . ? C16 N4 C14 116.8(2) . . ? N4 C14 C15 112.9(3) . . ? O7 C21 C23 122.7(2) . . ? O7 C21 C22 120.7(3) . . ? C23 C21 C22 116.6(2) . . ? O17 Mo3 O9 104.46(9) . . ? O17 Mo3 O8 103.84(8) . . ? O9 Mo3 O8 91.88(8) . . ? O17 Mo3 O15 102.51(8) . . ? O9 Mo3 O15 87.54(8) . . ? O8 Mo3 O15 152.92(7) . . ? O17 Mo3 O16 102.04(8) . . ? O9 Mo3 O16 153.13(7) . . ? O8 Mo3 O16 86.06(8) . . ? O15 Mo3 O16 82.44(7) . . ? O17 Mo3 O10 177.00(7) . . ? O9 Mo3 O10 78.08(5) . . ? O8 Mo3 O10 77.53(5) . . ? O15 Mo3 O10 75.87(5) . . ? O16 Mo3 O10 75.31(5) . . ? O13 Mo2 O16 105.71(9) . 2_556 ? O13 Mo2 O12 103.31(9) . . ? O16 Mo2 O12 89.96(8) 2_556 . ? O13 Mo2 O11 103.04(9) . . ? O16 Mo2 O11 88.87(8) 2_556 . ? O12 Mo2 O11 152.92(7) . . ? O13 Mo2 O9 100.89(9) . . ? O16 Mo2 O9 153.39(7) 2_556 . ? O12 Mo2 O9 84.77(7) . . ? O11 Mo2 O9 84.26(8) . . ? O13 Mo2 O10 176.56(7) . . ? O16 Mo2 O10 77.70(5) 2_556 . ? O12 Mo2 O10 76.94(5) . . ? O11 Mo2 O10 76.38(5) . . ? O9 Mo2 O10 75.70(5) . . ? O4 Mo1 O3 104.95(9) . . ? O4 Mo1 O2 100.48(8) . . ? O3 Mo1 O2 103.66(8) . . ? O4 Mo1 O1 97.16(8) . . ? O3 Mo1 O1 94.70(7) . . ? O2 Mo1 O1 150.16(7) . . ? O4 Mo1 N1 98.15(8) . . ? O3 Mo1 N1 154.85(8) . . ? O2 Mo1 N1 81.41(7) . . ? O1 Mo1 N1 72.37(7) . . ? O4 Mo1 O5 172.95(8) . . ? O3 Mo1 O5 81.62(8) . . ? O2 Mo1 O5 80.12(8) . . ? O1 Mo1 O5 79.53(7) . . ? N1 Mo1 O5 74.95(8) . . ? O14 Mo4 O15 104.17(8) . 2_556 ? O14 Mo4 O11 103.76(8) . . ? O15 Mo4 O11 89.04(8) 2_556 . ? O14 Mo4 O12 103.06(8) . 2_556 ? O15 Mo4 O12 88.26(7) 2_556 2_556 ? O11 Mo4 O12 152.88(7) . 2_556 ? O14 Mo4 O8 102.85(8) . . ? O15 Mo4 O8 152.96(7) 2_556 . ? O11 Mo4 O8 85.48(8) . . ? O12 Mo4 O8 84.78(8) 2_556 . ? O14 Mo4 O10 178.48(7) . . ? O15 Mo4 O10 77.29(5) 2_556 . ? O11 Mo4 O10 76.60(5) . . ? O12 Mo4 O10 76.48(5) 2_556 . ? O8 Mo4 O10 75.69(5) . . ? O6 C18 C19 124.3(9) . . ? O6 C18 C20 120.8(8) . . ? C19 C18 C20 115.0(4) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.215 _refine_diff_density_min -1.070 _refine_diff_density_rms 0.072