# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Alexander Briceno' _publ_contact_author_email ABRICENO@IVIC.VE # Attachment 'SHELXLE_III_.CIF' #========================================================================== _publ_contact_author_address ; Centro de Qu\'imica Instituto Venezolano de Investigaciones Cient\'ifica (IVIC) Apartado 21827 Caracas 1020-A Venezuela ; _publ_contact_author_phone '(58-212) 504-1320' _publ_contact_author_fax '(58-212) 504-1350' _publ_requested_category ? _publ_requested_coeditor_name ? #========================================================================== # TITLE AND AUTHOR LIST _publ_section_title ; A non photochemical route for the regioselective preparation of rtct-pyridylcyclobutanes via hydrothermal isomerisation promoted by polymolybdates ; loop_ _publ_author_name _publ_author_address 'Alexander Briceno' ; Centro de Qu\'imica Instituto Venezolano de Investigaciones Cient\'ifica (IVIC) Apartado 21827 Caracas 1020-A Venezuela ; 'Aaron Fulgence' ; Centro de Qu\'imica Instituto Venezolano de Investigaciones Cient\'ifica (IVIC) Apartado 21827 Caracas 1020-A Venezuela ; 'Yennifer Hill' ; Centro de Qu\'imica Instituto Venezolano de Investigaciones Cient\'ifica (IVIC) Apartado 21827 Caracas 1020-A Venezuela ; 'Reinaldo Atencio' ; Centro de Qu\'imica Instituto Venezolano de Investigaciones Cient\'ifica (IVIC) Apartado 21827 Caracas 1020-A Venezuela ; #======================================================== data_shelxle3 _database_code_depnum_ccdc_archive 'CCDC 668915' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '(C24 H22 N4), 0.5(Mo8 O26)' _chemical_formula_sum 'C24 H22 Mo4 N4 O13' _chemical_formula_weight 958.22 _chemical_compound_source Synthesis 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' Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall -P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.256(5) _cell_length_b 12.568(5) _cell_length_c 13.128(5) _cell_angle_alpha 106.782(4) _cell_angle_beta 100.890(12) _cell_angle_gamma 109.276(9) _cell_volume 1451.7(11) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3176 _cell_measurement_theta_min 2.14 _cell_measurement_theta_max 28.01 _exptl_crystal_description Prism _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.192 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 932 _exptl_absorpt_coefficient_mu 1.762 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_absorpt_correction_T_min 0.525 _exptl_absorpt_correction_T_max 0.687 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku AFC7S Mercury' _diffrn_measurement_method '\w ' _diffrn_radiation_detector CCD _diffrn_measurement_device ; Mercury (2x2 bin mode) ; _diffrn_detector_area_resol_mean 14.6306 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 16189 _diffrn_reflns_av_R_equivalents 0.0217 _diffrn_reflns_av_sigmaI/netI 0.0294 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.71 _diffrn_reflns_theta_max 28.04 _reflns_number_total 5456 _reflns_number_gt 4976 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_cell_refinement 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_data_reduction 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_structure_solution 'SHELXLTL-NT V5.1 (Bruker AXS, 1998)' _computing_structure_refinement 'SHELXLTL-NT V5.1 (Bruker AXS, 1998)' _computing_molecular_graphics ; SHELXLTL-NT V5.1 (Bruker AXS, 1998) and DIAMOND (Brandenburg, 1998) ; _computing_publication_material ; SHELXLTL-NT V5.1 (Bruker AXS, 1998) and PLATON (Spek, 2003). ; _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^)+(0.0380P)^2^+1.0392P] 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 5456 _refine_ls_number_parameters 406 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0323 _refine_ls_R_factor_gt 0.0283 _refine_ls_wR_factor_ref 0.0718 _refine_ls_wR_factor_gt 0.0691 _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_restrained_S_all 1.052 _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 0.80475(3) 0.76591(2) -0.18550(2) 0.01985(8) Uani 1 1 d . . . Mo2 Mo 0.85511(3) 1.02075(2) 0.03270(2) 0.01825(8) Uani 1 1 d . . . Mo3 Mo 0.98238(3) 0.99968(3) 0.28163(2) 0.02382(9) Uani 1 1 d . . . Mo4 Mo 0.81496(3) 0.74088(2) 0.05826(2) 0.02269(8) Uani 1 1 d . . . O1 O 0.9101(2) 0.6549(2) 0.0230(2) 0.0326(6) Uani 1 1 d . . . O2 O 0.6771(3) 0.6532(2) 0.0911(2) 0.0342(6) Uani 1 1 d . . . O3 O 0.7961(2) 0.91042(19) 0.10268(18) 0.0219(5) Uani 1 1 d . . . O4 O 1.0323(2) 1.1052(2) 0.20433(18) 0.0241(5) Uani 1 1 d . . . O5 O 0.9676(2) 0.88084(19) -0.01756(17) 0.0206(5) Uani 1 1 d . . . O6 O 0.8676(2) 0.6555(2) -0.22304(19) 0.0273(5) Uani 1 1 d . . . O7 O 0.7040(2) 0.7128(2) -0.09086(18) 0.0239(5) Uani 1 1 d . . . O8 O 0.7771(2) 1.1183(2) 0.07697(19) 0.0270(5) Uani 1 1 d . . . O9 O 0.7530(2) 0.9346(2) -0.10816(18) 0.0243(5) Uani 1 1 d . . . O10 O 0.8552(3) 1.0175(2) 0.3426(2) 0.0369(6) Uani 1 1 d . . . O11 O 0.6674(2) 0.7318(2) -0.30094(19) 0.0307(5) Uani 1 1 d . . . O12 O 0.9552(3) 0.8396(2) 0.2123(2) 0.0328(6) Uani 1 1 d . . . O13 O 1.1393(3) 1.0532(2) 0.3878(2) 0.0404(6) Uani 1 1 d . . . N1 N 0.8716(3) 0.3660(2) 0.2376(2) 0.0264(6) Uani 1 1 d . . . H1N H 0.9531 0.3801 0.2946 0.032 Uiso 1 1 d R . . N2 N 0.3874(3) 0.0027(2) 0.3137(2) 0.0283(6) Uani 1 1 d . . . H2N H 0.3977 0.0495 0.3902 0.034 Uiso 1 1 d R . . N3 N 0.4959(3) 0.1646(3) 0.5468(3) 0.0320(7) Uani 1 1 d . . . N4 N 1.0586(3) 0.3698(3) 0.4405(2) 0.0258(6) Uani 1 1 d . . . C1 C 0.7409(3) 0.2411(3) 0.3252(3) 0.0213(7) Uani 1 1 d . . . H1 H 0.7773 0.1793 0.2965 0.026 Uiso 1 1 calc R . . C2 C 0.5992(3) 0.1811(3) 0.3497(3) 0.0231(7) Uani 1 1 d . . . H2 H 0.5452 0.2327 0.3529 0.028 Uiso 1 1 calc R . . C3 C 0.6933(3) 0.2113(3) 0.4709(3) 0.0228(7) Uani 1 1 d . . . H3 H 0.7194 0.1435 0.4733 0.027 Uiso 1 1 calc R . . C4 C 0.8174(3) 0.3086(3) 0.4540(3) 0.0220(7) Uani 1 1 d . . . H4 H 0.8097 0.3870 0.4792 0.026 Uiso 1 1 calc R . . C5 C 0.7425(3) 0.3117(3) 0.2517(3) 0.0212(6) Uani 1 1 d . . . C6 C 0.8881(4) 0.4245(3) 0.1680(3) 0.0305(8) Uani 1 1 d . . . H6 H 0.9788 0.4569 0.1589 0.037 Uiso 1 1 calc R . . C7 C 0.7728(4) 0.4374(3) 0.1098(3) 0.0315(8) Uani 1 1 d . . . H7 H 0.7840 0.4793 0.0620 0.038 Uiso 1 1 calc R . . C8 C 0.6396(4) 0.3867(3) 0.1238(3) 0.0342(8) Uani 1 1 d . . . H8 H 0.5599 0.3956 0.0862 0.041 Uiso 1 1 calc R . . C9 C 0.6237(3) 0.3224(3) 0.1938(3) 0.0297(8) Uani 1 1 d . . . H9 H 0.5330 0.2866 0.2016 0.036 Uiso 1 1 calc R . . C10 C 0.4984(3) 0.0531(3) 0.2781(3) 0.0243(7) Uani 1 1 d . . . C11 C 0.2821(4) -0.1092(3) 0.2553(3) 0.0363(9) Uani 1 1 d . . . H11 H 0.2070 -0.1400 0.2829 0.044 Uiso 1 1 calc R . . C12 C 0.2855(4) -0.1779(3) 0.1548(4) 0.0413(9) Uani 1 1 d . . . H12 H 0.2114 -0.2547 0.1121 0.050 Uiso 1 1 calc R . . C13 C 0.4013(4) -0.1311(4) 0.1180(3) 0.0402(9) Uani 1 1 d . . . H13 H 0.4077 -0.1780 0.0515 0.048 Uiso 1 1 calc R . . C14 C 0.5073(4) -0.0150(3) 0.1794(3) 0.0334(8) Uani 1 1 d . . . H14 H 0.5843 0.0168 0.1539 0.040 Uiso 1 1 calc R . . C15 C 0.6298(3) 0.2469(3) 0.5629(3) 0.0249(7) Uani 1 1 d . . . C16 C 0.4352(4) 0.1904(4) 0.6280(3) 0.0388(9) Uani 1 1 d . . . H16 H 0.3434 0.1346 0.6189 0.047 Uiso 1 1 calc R . . C17 C 0.5011(4) 0.2940(4) 0.7235(3) 0.0414(10) Uani 1 1 d . . . H17 H 0.4556 0.3067 0.7780 0.050 Uiso 1 1 calc R . . C18 C 0.6354(4) 0.3790(4) 0.7375(3) 0.0410(9) Uani 1 1 d . . . H18 H 0.6818 0.4507 0.8008 0.049 Uiso 1 1 calc R . . C19 C 0.7000(4) 0.3549(3) 0.6547(3) 0.0332(8) Uani 1 1 d . . . H19 H 0.7900 0.4113 0.6611 0.040 Uiso 1 1 calc R . . C20 C 0.9736(3) 0.3273(3) 0.4979(3) 0.0243(7) Uani 1 1 d . . . C21 C 1.2001(3) 0.3930(3) 0.4774(3) 0.0292(8) Uani 1 1 d . . . H21 H 1.2606 0.4234 0.4386 0.035 Uiso 1 1 calc R . . C22 C 1.2597(4) 0.3740(4) 0.5699(3) 0.0391(9) Uani 1 1 d . . . H22 H 1.3585 0.3917 0.5934 0.047 Uiso 1 1 calc R . . C23 C 1.1708(4) 0.3283(4) 0.6269(4) 0.0453(10) Uani 1 1 d . . . H23 H 1.2082 0.3139 0.6894 0.054 Uiso 1 1 calc R . . C24 C 1.0259(4) 0.3042(4) 0.5903(3) 0.0378(9) Uani 1 1 d . . . H24 H 0.9636 0.2727 0.6274 0.045 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mo1 0.01819(14) 0.02139(16) 0.02027(16) 0.00811(12) 0.00692(11) 0.00779(11) Mo2 0.01827(14) 0.02059(16) 0.02000(15) 0.00978(12) 0.00788(11) 0.00999(11) Mo3 0.02646(16) 0.02768(17) 0.02202(16) 0.01355(13) 0.01059(12) 0.01145(12) Mo4 0.02457(15) 0.02153(16) 0.02557(17) 0.01217(13) 0.01013(12) 0.00965(12) O1 0.0337(13) 0.0321(14) 0.0411(15) 0.0189(12) 0.0158(11) 0.0178(11) O2 0.0375(14) 0.0357(15) 0.0367(15) 0.0204(12) 0.0192(12) 0.0136(11) O3 0.0209(11) 0.0232(12) 0.0242(12) 0.0105(10) 0.0096(9) 0.0095(9) O4 0.0214(11) 0.0266(13) 0.0222(12) 0.0127(10) 0.0063(9) 0.0048(9) O5 0.0193(10) 0.0235(12) 0.0197(11) 0.0088(10) 0.0058(9) 0.0092(9) O6 0.0258(11) 0.0285(13) 0.0301(13) 0.0107(11) 0.0111(10) 0.0131(10) O7 0.0196(10) 0.0245(12) 0.0263(12) 0.0095(10) 0.0094(9) 0.0065(9) O8 0.0271(12) 0.0284(13) 0.0295(13) 0.0103(11) 0.0118(10) 0.0152(10) O9 0.0256(11) 0.0248(13) 0.0249(12) 0.0100(10) 0.0070(9) 0.0132(9) O10 0.0422(14) 0.0449(16) 0.0326(14) 0.0180(12) 0.0226(12) 0.0199(12) O11 0.0255(12) 0.0386(15) 0.0272(13) 0.0098(11) 0.0065(10) 0.0156(11) O12 0.0384(13) 0.0313(14) 0.0300(14) 0.0141(11) 0.0043(11) 0.0172(11) O13 0.0396(14) 0.0449(17) 0.0326(15) 0.0164(13) 0.0046(12) 0.0144(12) N1 0.0202(13) 0.0275(16) 0.0338(16) 0.0160(13) 0.0070(12) 0.0096(11) N2 0.0262(14) 0.0255(16) 0.0354(17) 0.0151(13) 0.0115(13) 0.0091(12) N3 0.0274(15) 0.0364(18) 0.0367(18) 0.0182(15) 0.0145(13) 0.0123(13) N4 0.0235(14) 0.0304(16) 0.0276(16) 0.0131(13) 0.0102(12) 0.0128(12) C1 0.0196(15) 0.0220(17) 0.0229(17) 0.0082(14) 0.0061(13) 0.0097(13) C2 0.0267(16) 0.0235(17) 0.0223(17) 0.0112(14) 0.0089(13) 0.0114(13) C3 0.0235(15) 0.0233(17) 0.0235(17) 0.0101(14) 0.0096(13) 0.0094(13) C4 0.0248(16) 0.0234(17) 0.0204(17) 0.0107(14) 0.0079(13) 0.0106(13) C5 0.0224(15) 0.0196(16) 0.0228(17) 0.0082(14) 0.0099(13) 0.0085(13) C6 0.0278(17) 0.0261(19) 0.042(2) 0.0189(17) 0.0147(16) 0.0090(14) C7 0.0377(19) 0.0270(19) 0.036(2) 0.0192(17) 0.0126(16) 0.0131(15) C8 0.0326(19) 0.040(2) 0.036(2) 0.0199(18) 0.0082(16) 0.0188(16) C9 0.0214(16) 0.039(2) 0.037(2) 0.0225(17) 0.0116(15) 0.0148(15) C10 0.0231(16) 0.0286(18) 0.0267(18) 0.0157(15) 0.0076(13) 0.0128(13) C11 0.0218(17) 0.033(2) 0.054(3) 0.0237(19) 0.0059(16) 0.0079(15) C12 0.037(2) 0.025(2) 0.047(2) 0.0107(18) -0.0049(18) 0.0068(16) C13 0.047(2) 0.034(2) 0.031(2) 0.0035(17) 0.0030(17) 0.0196(18) C14 0.0304(18) 0.035(2) 0.032(2) 0.0112(17) 0.0104(15) 0.0111(15) C15 0.0279(17) 0.0296(18) 0.0249(18) 0.0150(15) 0.0111(14) 0.0153(14) C16 0.0329(19) 0.055(3) 0.047(2) 0.032(2) 0.0246(18) 0.0223(18) C17 0.054(2) 0.062(3) 0.037(2) 0.028(2) 0.030(2) 0.040(2) C18 0.056(2) 0.046(2) 0.029(2) 0.0137(18) 0.0179(18) 0.028(2) C19 0.0364(19) 0.033(2) 0.030(2) 0.0118(17) 0.0142(16) 0.0113(16) C20 0.0255(16) 0.0231(17) 0.0229(17) 0.0074(14) 0.0065(13) 0.0100(13) C21 0.0242(17) 0.035(2) 0.0288(19) 0.0112(16) 0.0109(14) 0.0124(15) C22 0.0291(18) 0.053(3) 0.039(2) 0.021(2) 0.0073(16) 0.0212(17) C23 0.041(2) 0.069(3) 0.038(2) 0.032(2) 0.0087(18) 0.028(2) C24 0.0339(19) 0.057(3) 0.031(2) 0.0263(19) 0.0135(16) 0.0186(18) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mo1 O11 1.699(2) . ? Mo1 O6 1.703(2) . ? Mo1 O7 1.888(2) . ? Mo1 O4 2.019(2) 2_775 ? Mo1 O5 2.217(2) . ? Mo1 O9 2.348(2) . ? Mo2 O8 1.701(2) . ? Mo2 O9 1.747(2) . ? Mo2 O3 1.877(2) . ? Mo2 O5 1.915(2) 2_775 ? Mo2 O4 2.303(2) . ? Mo2 O5 2.412(2) . ? Mo3 O10 1.696(2) . ? Mo3 O13 1.697(3) . ? Mo3 O12 1.852(3) . ? Mo3 O4 1.891(2) . ? Mo3 O3 2.407(2) . ? Mo4 O2 1.696(2) . ? Mo4 O1 1.706(2) . ? Mo4 O7 1.936(2) . ? Mo4 O12 1.993(2) . ? Mo4 O3 2.125(2) . ? Mo4 O5 2.514(2) . ? O4 Mo1 2.019(2) 2_775 ? O5 Mo2 1.915(2) 2_775 ? N1 C6 1.330(4) . ? N1 C5 1.351(4) . ? N1 H1N 0.9380 . ? N2 C11 1.340(4) . ? N2 C10 1.346(4) . ? N2 H2N 0.9704 . ? N3 C16 1.347(4) . ? N3 C15 1.351(4) . ? N4 C20 1.336(4) . ? N4 C21 1.341(4) . ? C1 C5 1.486(4) . ? C1 C2 1.541(4) . ? C1 C4 1.557(4) . ? C1 H1 0.9800 . ? C2 C10 1.484(4) . ? C2 C3 1.561(4) . ? C2 H2 0.9800 . ? C3 C15 1.504(4) . ? C3 C4 1.550(4) . ? C3 H3 0.9800 . ? C4 C20 1.509(4) . ? C4 H4 0.9800 . ? C5 C9 1.377(4) . ? C6 C7 1.365(5) . ? C6 H6 0.9300 . ? C7 C8 1.376(5) . ? C7 H7 0.9300 . ? C8 C9 1.386(5) . ? C8 H8 0.9300 . ? C9 H9 0.9300 . ? C10 C14 1.370(5) . ? C11 C12 1.366(6) . ? C11 H11 0.9300 . ? C12 C13 1.382(6) . ? C12 H12 0.9300 . ? C13 C14 1.379(5) . ? C13 H13 0.9300 . ? C14 H14 0.9300 . ? C15 C19 1.377(5) . ? C16 C17 1.371(6) . ? C16 H16 0.9300 . ? C17 C18 1.375(6) . ? C17 H17 0.9300 . ? C18 C19 1.388(5) . ? C18 H18 0.9300 . ? C19 H19 0.9300 . ? C20 C24 1.379(5) . ? C21 C22 1.375(5) . ? C21 H21 0.9300 . ? C22 C23 1.372(5) . ? C22 H22 0.9300 . ? C23 C24 1.371(5) . ? C23 H23 0.9300 . ? C24 H24 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O11 Mo1 O6 104.73(11) . . ? O11 Mo1 O7 102.61(11) . . ? O6 Mo1 O7 99.45(10) . . ? O11 Mo1 O4 99.96(11) . 2_775 ? O6 Mo1 O4 95.20(10) . 2_775 ? O7 Mo1 O4 148.86(9) . 2_775 ? O11 Mo1 O5 155.86(10) . . ? O6 Mo1 O5 98.84(10) . . ? O7 Mo1 O5 78.22(9) . . ? O4 Mo1 O5 72.45(9) 2_775 . ? O11 Mo1 O9 84.48(10) . . ? O6 Mo1 O9 170.56(9) . . ? O7 Mo1 O9 80.14(9) . . ? O4 Mo1 O9 80.98(9) 2_775 . ? O5 Mo1 O9 71.80(8) . . ? O8 Mo2 O9 104.69(11) . . ? O8 Mo2 O3 102.49(10) . . ? O9 Mo2 O3 103.09(10) . . ? O8 Mo2 O5 104.75(10) . 2_775 ? O9 Mo2 O5 100.40(10) . 2_775 ? O3 Mo2 O5 137.82(9) . 2_775 ? O8 Mo2 O4 91.96(10) . . ? O9 Mo2 O4 163.15(9) . . ? O3 Mo2 O4 75.19(9) . . ? O5 Mo2 O4 72.31(9) 2_775 . ? O8 Mo2 O5 175.98(9) . . ? O9 Mo2 O5 78.41(9) . . ? O3 Mo2 O5 74.15(8) . . ? O5 Mo2 O5 76.95(10) 2_775 . ? O4 Mo2 O5 85.07(8) . . ? O10 Mo3 O13 106.29(13) . . ? O10 Mo3 O12 114.83(12) . . ? O13 Mo3 O12 101.06(12) . . ? O10 Mo3 O4 112.35(11) . . ? O13 Mo3 O4 102.20(11) . . ? O12 Mo3 O4 117.78(11) . . ? O10 Mo3 O3 88.05(11) . . ? O13 Mo3 O3 165.63(10) . . ? O12 Mo3 O3 71.12(9) . . ? O4 Mo3 O3 72.41(9) . . ? O2 Mo4 O1 105.11(12) . . ? O2 Mo4 O7 97.61(11) . . ? O1 Mo4 O7 98.92(11) . . ? O2 Mo4 O12 98.73(12) . . ? O1 Mo4 O12 93.54(11) . . ? O7 Mo4 O12 156.08(10) . . ? O2 Mo4 O3 102.93(10) . . ? O1 Mo4 O3 151.09(10) . . ? O7 Mo4 O3 84.10(9) . . ? O12 Mo4 O3 75.30(9) . . ? O2 Mo4 O5 165.16(10) . . ? O1 Mo4 O5 85.65(10) . . ? O7 Mo4 O5 70.22(8) . . ? O12 Mo4 O5 90.61(9) . . ? O3 Mo4 O5 68.21(8) . . ? Mo2 O3 Mo4 123.40(11) . . ? Mo2 O3 Mo3 104.41(9) . . ? Mo4 O3 Mo3 94.03(8) . . ? Mo3 O4 Mo1 145.94(12) . 2_775 ? Mo3 O4 Mo2 107.98(10) . . ? Mo1 O4 Mo2 102.88(9) 2_775 . ? Mo2 O5 Mo1 109.79(10) 2_775 . ? Mo2 O5 Mo2 103.05(10) 2_775 . ? Mo1 O5 Mo2 95.63(8) . . ? Mo2 O5 Mo4 155.55(10) 2_775 . ? Mo1 O5 Mo4 87.91(8) . . ? Mo2 O5 Mo4 91.40(7) . . ? Mo1 O7 Mo4 118.73(11) . . ? Mo2 O9 Mo1 113.08(10) . . ? Mo3 O12 Mo4 119.40(12) . . ? C6 N1 C5 123.5(3) . . ? C6 N1 H1N 119.7 . . ? C5 N1 H1N 114.5 . . ? C11 N2 C10 123.2(3) . . ? C11 N2 H2N 122.3 . . ? C10 N2 H2N 113.9 . . ? C16 N3 C15 116.7(3) . . ? C20 N4 C21 117.7(3) . . ? C5 C1 C2 119.6(3) . . ? C5 C1 C4 120.1(3) . . ? C2 C1 C4 88.3(2) . . ? C5 C1 H1 109.1 . . ? C2 C1 H1 109.1 . . ? C4 C1 H1 109.1 . . ? C10 C2 C1 119.8(3) . . ? C10 C2 C3 119.4(3) . . ? C1 C2 C3 88.4(2) . . ? C10 C2 H2 109.2 . . ? C1 C2 H2 109.2 . . ? C3 C2 H2 109.2 . . ? C15 C3 C4 120.7(3) . . ? C15 C3 C2 116.3(3) . . ? C4 C3 C2 87.9(2) . . ? C15 C3 H3 110.0 . . ? C4 C3 H3 110.0 . . ? C2 C3 H3 110.0 . . ? C20 C4 C3 120.7(3) . . ? C20 C4 C1 117.0(3) . . ? C3 C4 C1 88.3(2) . . ? C20 C4 H4 109.7 . . ? C3 C4 H4 109.7 . . ? C1 C4 H4 109.7 . . ? N1 C5 C9 117.5(3) . . ? N1 C5 C1 116.5(3) . . ? C9 C5 C1 126.0(3) . . ? N1 C6 C7 120.4(3) . . ? N1 C6 H6 119.8 . . ? C7 C6 H6 119.8 . . ? C6 C7 C8 118.4(3) . . ? C6 C7 H7 120.8 . . ? C8 C7 H7 120.8 . . ? C7 C8 C9 120.3(3) . . ? C7 C8 H8 119.9 . . ? C9 C8 H8 119.9 . . ? C5 C9 C8 119.9(3) . . ? C5 C9 H9 120.1 . . ? C8 C9 H9 120.1 . . ? N2 C10 C14 118.4(3) . . ? N2 C10 C2 115.9(3) . . ? C14 C10 C2 125.7(3) . . ? N2 C11 C12 119.7(3) . . ? N2 C11 H11 120.1 . . ? C12 C11 H11 120.1 . . ? C11 C12 C13 118.6(4) . . ? C11 C12 H12 120.7 . . ? C13 C12 H12 120.7 . . ? C14 C13 C12 120.3(4) . . ? C14 C13 H13 119.8 . . ? C12 C13 H13 119.8 . . ? C10 C14 C13 119.6(3) . . ? C10 C14 H14 120.2 . . ? C13 C14 H14 120.2 . . ? N3 C15 C19 122.6(3) . . ? N3 C15 C3 114.2(3) . . ? C19 C15 C3 123.2(3) . . ? N3 C16 C17 123.7(3) . . ? N3 C16 H16 118.1 . . ? C17 C16 H16 118.1 . . ? C16 C17 C18 119.1(3) . . ? C16 C17 H17 120.5 . . ? C18 C17 H17 120.5 . . ? C17 C18 C19 118.3(4) . . ? C17 C18 H18 120.8 . . ? C19 C18 H18 120.8 . . ? C15 C19 C18 119.4(3) . . ? C15 C19 H19 120.3 . . ? C18 C19 H19 120.3 . . ? N4 C20 C24 122.3(3) . . ? N4 C20 C4 114.4(3) . . ? C24 C20 C4 123.3(3) . . ? N4 C21 C22 123.0(3) . . ? N4 C21 H21 118.5 . . ? C22 C21 H21 118.5 . . ? C23 C22 C21 118.8(3) . . ? C23 C22 H22 120.6 . . ? C21 C22 H22 120.6 . . ? C24 C23 C22 118.9(4) . . ? C24 C23 H23 120.6 . . ? C22 C23 H23 120.6 . . ? C23 C24 C20 119.4(3) . . ? C23 C24 H24 120.3 . . ? C20 C24 H24 120.3 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N2 H2N N3 0.97 1.97 2.893(4) 158.3 . N1 H1N N4 0.94 2.08 2.952(4) 154.9 . _diffrn_measured_fraction_theta_max 0.774 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.971 _refine_diff_density_max 0.556 _refine_diff_density_min -0.931 _refine_diff_density_rms 0.110 #======================================================== data_shelxle2 _database_code_depnum_ccdc_archive 'CCDC 668916' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H24 N4, Mo8 O26' _chemical_formula_sum 'C24 H24 Mo8 N4 O26' _chemical_formula_weight 1551.99 _chemical_compound_source Synthesis 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 _symmetry_space_group_name_Hall -P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.620(2) _cell_length_b 10.087(2) _cell_length_c 10.578(3) _cell_angle_alpha 100.807(5) _cell_angle_beta 106.923(4) _cell_angle_gamma 97.085(5) _cell_volume 947.2(4) _cell_formula_units_Z 1 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 2490 _cell_measurement_theta_min 2.14 _cell_measurement_theta_max 28.01 _exptl_crystal_description Prism _exptl_crystal_colour 'Pale yellow' _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.721 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 740 _exptl_absorpt_coefficient_mu 2.662 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_absorpt_correction_T_min 0.695 _exptl_absorpt_correction_T_max 0.821 _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku AFC7S Mercury' _diffrn_measurement_method '\w ' _diffrn_radiation_detector CCD _diffrn_measurement_device ; Mercury (2x2 bin mode) ; _diffrn_detector_area_resol_mean 14.6306 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 10969 _diffrn_reflns_av_R_equivalents 0.0678 _diffrn_reflns_av_sigmaI/netI 0.0683 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.07 _diffrn_reflns_theta_max 28.23 _reflns_number_total 3580 _reflns_number_gt 2746 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_cell_refinement 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_data_reduction 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_structure_solution 'SHELXLTL-NT V5.1 (Bruker AXS, 1998)' _computing_structure_refinement 'SHELXLTL-NT V5.1 (Bruker AXS, 1998)' _computing_molecular_graphics ; SHELXLTL-NT V5.1 (Bruker AXS, 1998) and DIAMOND (Brandenburg, 1998) ; _computing_publication_material ; SHELXLTL-NT V5.1 (Bruker AXS, 1998) and PLATON (Spek, 2003). ; _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^)+(0.0564P)^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 3580 _refine_ls_number_parameters 280 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0645 _refine_ls_R_factor_gt 0.0477 _refine_ls_wR_factor_ref 0.1255 _refine_ls_wR_factor_gt 0.1133 _refine_ls_goodness_of_fit_ref 1.091 _refine_ls_restrained_S_all 1.091 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mo1 Mo 0.56380(6) 0.28990(5) 1.13105(5) 0.02086(18) Uani 1 1 d . . . Mo2 Mo 0.68905(5) 0.02856(5) 1.00195(5) 0.01729(17) Uani 1 1 d . . . Mo3 Mo 0.30967(6) 0.24137(5) 0.83736(6) 0.02356(18) Uani 1 1 d . . . Mo4 Mo 0.43164(6) -0.02246(5) 0.71488(5) 0.01965(17) Uani 1 1 d . . . O1 O 0.1460(5) 0.2948(4) 0.7857(5) 0.0382(12) Uani 1 1 d . . . O2 O 0.4881(4) 0.1068(4) 0.9317(4) 0.0208(10) Uani 1 1 d . . . O3 O 0.5872(5) 0.3779(4) 1.2910(5) 0.0334(12) Uani 1 1 d . . . O4 O 0.5807(4) -0.1074(4) 0.8331(4) 0.0198(9) Uani 1 1 d . . . O5 O 0.1990(4) 0.0760(4) 0.9204(4) 0.0246(10) Uani 1 1 d . . . O6 O 0.3555(5) -0.1557(4) 0.5768(4) 0.0314(11) Uani 1 1 d . . . O7 O 0.2763(5) 0.0761(4) 0.6971(4) 0.0246(10) Uani 1 1 d . . . O8 O 0.3789(5) 0.3209(4) 1.0298(4) 0.0251(10) Uani 1 1 d . . . O9 O 0.3110(4) -0.1488(4) 0.8298(4) 0.0188(9) Uani 1 1 d . . . O10 O 0.6811(5) 0.3870(4) 1.0750(5) 0.0312(12) Uani 1 1 d . . . O11 O 0.4316(5) 0.3407(4) 0.7908(5) 0.0336(12) Uani 1 1 d . . . O12 O 0.8000(5) 0.1330(4) 0.9492(4) 0.0269(11) Uani 1 1 d . . . O13 O 0.5580(5) 0.0776(4) 0.6699(4) 0.0257(10) Uani 1 1 d . . . N1 N 0.2021(7) 0.5017(6) 0.1083(6) 0.0456(17) Uani 1 1 d . . . H1B H 0.2478 0.5002 0.0494 0.055 Uiso 1 1 calc R . . N2 N 0.2522(8) 0.1009(6) 0.3967(6) 0.0448(16) Uani 1 1 d . . . H2B H 0.3048 0.0425 0.3760 0.054 Uiso 1 1 calc R . . C1 C -0.0303(7) 0.5038(6) 0.3924(6) 0.0244(14) Uani 1 1 d . . . H1 H -0.1343 0.5023 0.3436 0.029 Uiso 1 1 calc R . . C2 C -0.0207(7) 0.3834(6) 0.4716(6) 0.0222(14) Uani 1 1 d . . . H2 H -0.1201 0.3326 0.4559 0.027 Uiso 1 1 calc R . . C3 C 0.0571(7) 0.5063(6) 0.2963(6) 0.0236(14) Uani 1 1 d . . . C4 C 0.1661(8) 0.6167(6) 0.3060(7) 0.0342(17) Uani 1 1 d . . . H4 H 0.1907 0.6934 0.3780 0.041 Uiso 1 1 calc R . . C5 C 0.2366(8) 0.6129(7) 0.2111(8) 0.0377(19) Uani 1 1 d . . . H5 H 0.3082 0.6872 0.2177 0.045 Uiso 1 1 calc R . . C6 C 0.1011(8) 0.3948(7) 0.0940(7) 0.0415(19) Uani 1 1 d . . . H6 H 0.0799 0.3194 0.0211 0.050 Uiso 1 1 calc R . . C7 C 0.0273(7) 0.3947(6) 0.1862(6) 0.0293(15) Uani 1 1 d . . . H7 H -0.0442 0.3187 0.1754 0.035 Uiso 1 1 calc R . . C8 C 0.0806(7) 0.2854(6) 0.4519(6) 0.0240(14) Uani 1 1 d . . . C9 C 0.2343(8) 0.3266(7) 0.4876(7) 0.0377(18) Uani 1 1 d . . . H9 H 0.2795 0.4176 0.5298 0.045 Uiso 1 1 calc R . . C10 C 0.3182(8) 0.2288(8) 0.4585(7) 0.0388(18) Uani 1 1 d . . . H10 H 0.4204 0.2538 0.4827 0.047 Uiso 1 1 calc R . . C11 C 0.1079(9) 0.0589(7) 0.3655(8) 0.044(2) Uani 1 1 d . . . H11 H 0.0657 -0.0330 0.3251 0.053 Uiso 1 1 calc R . . C12 C 0.0219(8) 0.1489(6) 0.3919(7) 0.0376(18) Uani 1 1 d . . . H12 H -0.0795 0.1181 0.3690 0.045 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mo1 0.0226(3) 0.0132(3) 0.0260(3) 0.0014(2) 0.0096(3) 0.0009(2) Mo2 0.0152(3) 0.0152(3) 0.0206(3) 0.0006(2) 0.0077(2) 0.0004(2) Mo3 0.0249(4) 0.0191(3) 0.0292(3) 0.0068(2) 0.0108(3) 0.0066(2) Mo4 0.0213(3) 0.0184(3) 0.0187(3) 0.0019(2) 0.0079(2) 0.0019(2) O1 0.030(3) 0.041(3) 0.049(3) 0.017(2) 0.012(2) 0.019(2) O2 0.020(2) 0.021(2) 0.022(2) 0.0044(18) 0.0073(19) 0.0032(18) O3 0.045(3) 0.021(2) 0.032(3) -0.001(2) 0.015(2) 0.003(2) O4 0.022(2) 0.0120(19) 0.026(2) -0.0009(17) 0.0131(19) 0.0007(17) O5 0.022(2) 0.021(2) 0.033(3) 0.0062(19) 0.012(2) 0.0052(18) O6 0.040(3) 0.026(2) 0.022(2) -0.0029(19) 0.009(2) 0.001(2) O7 0.021(2) 0.029(2) 0.023(2) 0.0076(19) 0.0053(19) 0.0050(19) O8 0.027(3) 0.017(2) 0.031(3) 0.0012(19) 0.011(2) 0.0066(19) O9 0.015(2) 0.021(2) 0.018(2) 0.0025(17) 0.0045(17) 0.0015(17) O10 0.029(3) 0.028(2) 0.040(3) 0.009(2) 0.018(2) 0.003(2) O11 0.034(3) 0.029(3) 0.044(3) 0.011(2) 0.021(3) 0.007(2) O12 0.026(2) 0.025(2) 0.031(3) 0.006(2) 0.013(2) 0.0012(19) O13 0.026(2) 0.026(2) 0.029(2) 0.008(2) 0.015(2) 0.005(2) N1 0.058(4) 0.034(3) 0.055(4) 0.001(3) 0.041(4) 0.006(3) N2 0.059(4) 0.038(4) 0.046(4) 0.011(3) 0.024(3) 0.023(3) C1 0.030(4) 0.024(3) 0.023(3) 0.002(3) 0.014(3) 0.011(3) C2 0.029(4) 0.025(3) 0.016(3) 0.008(3) 0.008(3) 0.009(3) C3 0.029(4) 0.023(3) 0.019(3) 0.004(3) 0.008(3) 0.010(3) C4 0.047(5) 0.022(3) 0.034(4) -0.002(3) 0.021(4) 0.004(3) C5 0.032(4) 0.031(4) 0.050(5) 0.015(4) 0.015(4) -0.007(3) C6 0.055(5) 0.036(4) 0.030(4) -0.010(3) 0.024(4) -0.003(4) C7 0.027(4) 0.029(3) 0.025(3) 0.002(3) 0.003(3) -0.002(3) C8 0.027(4) 0.022(3) 0.023(3) 0.001(3) 0.011(3) 0.006(3) C9 0.044(5) 0.030(4) 0.039(4) 0.006(3) 0.018(4) 0.003(3) C10 0.023(4) 0.057(5) 0.035(4) 0.005(4) 0.010(3) 0.006(3) C11 0.048(5) 0.028(4) 0.054(5) -0.002(3) 0.020(4) 0.005(4) C12 0.024(4) 0.032(4) 0.050(5) 0.004(4) 0.005(3) 0.009(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mo1 O3 1.693(4) . ? Mo1 O10 1.708(4) . ? Mo1 O8 1.887(4) . ? Mo1 O9 2.001(4) 2_657 ? Mo1 O4 2.325(4) 2_657 ? Mo1 O2 2.388(4) . ? Mo2 O12 1.688(4) . ? Mo2 O5 1.742(4) 2_657 ? Mo2 O4 1.950(4) . ? Mo2 O9 1.957(4) 2_657 ? Mo2 O2 2.162(4) . ? Mo2 O2 2.396(4) 2_657 ? Mo2 Mo4 3.2156(9) . ? Mo3 O11 1.689(4) . ? Mo3 O1 1.699(5) . ? Mo3 O8 1.922(4) . ? Mo3 O7 1.935(4) . ? Mo3 O5 2.311(4) . ? Mo3 O2 2.423(4) . ? Mo4 O6 1.696(4) . ? Mo4 O13 1.713(4) . ? Mo4 O7 1.879(4) . ? Mo4 O4 2.003(4) . ? Mo4 O2 2.288(4) . ? Mo4 O9 2.342(4) . ? O2 Mo2 2.396(4) 2_657 ? O4 Mo1 2.325(4) 2_657 ? O5 Mo2 1.742(4) 2_657 ? O9 Mo2 1.957(4) 2_657 ? O9 Mo1 2.001(4) 2_657 ? N1 C6 1.313(8) . ? N1 C5 1.338(8) . ? N1 H1B 0.8600 . ? N2 C10 1.317(8) . ? N2 C11 1.323(9) . ? N2 H2B 0.8600 . ? C1 C3 1.498(8) . ? C1 C2 1.563(7) 2_566 ? C1 C2 1.596(8) . ? C1 H1 0.9800 . ? C2 C8 1.500(8) . ? C2 C1 1.563(7) 2_566 ? C2 H2 0.9800 . ? C3 C7 1.394(8) . ? C3 C4 1.398(8) . ? C4 C5 1.364(9) . ? C4 H4 0.9300 . ? C5 H5 0.9300 . ? C6 C7 1.363(9) . ? C6 H6 0.9300 . ? C7 H7 0.9300 . ? C8 C12 1.374(8) . ? C8 C9 1.402(9) . ? C9 C10 1.395(10) . ? C9 H9 0.9300 . ? C10 H10 0.9300 . ? C11 C12 1.346(9) . ? C11 H11 0.9300 . ? C12 H12 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 Mo1 O10 105.2(2) . . ? O3 Mo1 O8 103.1(2) . . ? O10 Mo1 O8 101.1(2) . . ? O3 Mo1 O9 100.6(2) . 2_657 ? O10 Mo1 O9 96.55(19) . 2_657 ? O8 Mo1 O9 145.44(16) . 2_657 ? O3 Mo1 O4 88.85(18) . 2_657 ? O10 Mo1 O4 163.68(17) . 2_657 ? O8 Mo1 O4 83.31(16) . 2_657 ? O9 Mo1 O4 72.32(15) 2_657 2_657 ? O3 Mo1 O2 160.30(18) . . ? O10 Mo1 O2 94.02(18) . . ? O8 Mo1 O2 76.73(16) . . ? O9 Mo1 O2 72.55(15) 2_657 . ? O4 Mo1 O2 71.51(14) 2_657 . ? O12 Mo2 O5 105.3(2) . 2_657 ? O12 Mo2 O4 101.35(19) . . ? O5 Mo2 O4 97.27(18) 2_657 . ? O12 Mo2 O9 101.43(18) . 2_657 ? O5 Mo2 O9 96.24(18) 2_657 2_657 ? O4 Mo2 O9 149.34(17) . 2_657 ? O12 Mo2 O2 98.26(19) . . ? O5 Mo2 O2 156.49(18) 2_657 . ? O4 Mo2 O2 77.99(16) . . ? O9 Mo2 O2 78.67(16) 2_657 . ? O12 Mo2 O2 174.09(18) . 2_657 ? O5 Mo2 O2 80.65(16) 2_657 2_657 ? O4 Mo2 O2 77.88(15) . 2_657 ? O9 Mo2 O2 77.34(14) 2_657 2_657 ? O2 Mo2 O2 75.84(17) . 2_657 ? O12 Mo2 Mo4 90.14(15) . . ? O5 Mo2 Mo4 133.38(13) 2_657 . ? O4 Mo2 Mo4 36.13(12) . . ? O9 Mo2 Mo4 123.94(12) 2_657 . ? O2 Mo2 Mo4 45.30(10) . . ? O2 Mo2 Mo4 85.86(10) 2_657 . ? O11 Mo3 O1 106.3(2) . . ? O11 Mo3 O8 99.3(2) . . ? O1 Mo3 O8 102.4(2) . . ? O11 Mo3 O7 97.91(19) . . ? O1 Mo3 O7 101.2(2) . . ? O8 Mo3 O7 145.43(18) . . ? O11 Mo3 O5 163.89(19) . . ? O1 Mo3 O5 89.75(19) . . ? O8 Mo3 O5 77.67(16) . . ? O7 Mo3 O5 77.51(16) . . ? O11 Mo3 O2 93.68(18) . . ? O1 Mo3 O2 159.93(19) . . ? O8 Mo3 O2 75.25(16) . . ? O7 Mo3 O2 73.92(16) . . ? O5 Mo3 O2 70.22(14) . . ? O6 Mo4 O13 103.7(2) . . ? O6 Mo4 O7 100.4(2) . . ? O13 Mo4 O7 102.61(19) . . ? O6 Mo4 O4 100.31(19) . . ? O13 Mo4 O4 95.40(19) . . ? O7 Mo4 O4 148.34(17) . . ? O6 Mo4 O2 159.70(19) . . ? O13 Mo4 O2 96.33(17) . . ? O7 Mo4 O2 78.27(16) . . ? O4 Mo4 O2 74.00(15) . . ? O6 Mo4 O9 87.09(18) . . ? O13 Mo4 O9 164.86(18) . . ? O7 Mo4 O9 85.55(16) . . ? O4 Mo4 O9 71.90(15) . . ? O2 Mo4 O9 72.61(14) . . ? O6 Mo4 Mo2 135.33(16) . . ? O13 Mo4 Mo2 85.43(15) . . ? O7 Mo4 Mo2 120.43(12) . . ? O4 Mo4 Mo2 35.03(10) . . ? O2 Mo4 Mo2 42.19(10) . . ? O9 Mo4 Mo2 79.43(10) . . ? Mo2 O2 Mo4 92.51(14) . . ? Mo2 O2 Mo1 91.58(14) . . ? Mo4 O2 Mo1 164.7(2) . . ? Mo2 O2 Mo2 104.16(17) . 2_657 ? Mo4 O2 Mo2 97.46(13) . 2_657 ? Mo1 O2 Mo2 95.80(14) . 2_657 ? Mo2 O2 Mo3 163.7(2) . . ? Mo4 O2 Mo3 86.87(13) . . ? Mo1 O2 Mo3 85.09(12) . . ? Mo2 O2 Mo3 92.08(14) 2_657 . ? Mo2 O4 Mo4 108.84(18) . . ? Mo2 O4 Mo1 111.98(18) . 2_657 ? Mo4 O4 Mo1 103.37(16) . 2_657 ? Mo2 O5 Mo3 117.0(2) 2_657 . ? Mo4 O7 Mo3 116.3(2) . . ? Mo1 O8 Mo3 117.3(2) . . ? Mo2 O9 Mo1 111.14(19) 2_657 2_657 ? Mo2 O9 Mo4 109.68(15) 2_657 . ? Mo1 O9 Mo4 102.84(16) 2_657 . ? C6 N1 C5 122.5(6) . . ? C6 N1 H1B 118.7 . . ? C5 N1 H1B 118.7 . . ? C10 N2 C11 122.3(7) . . ? C10 N2 H2B 118.8 . . ? C11 N2 H2B 118.8 . . ? C3 C1 C2 119.1(5) . 2_566 ? C3 C1 C2 117.2(5) . . ? C2 C1 C2 91.8(4) 2_566 . ? C3 C1 H1 109.2 . . ? C2 C1 H1 109.2 2_566 . ? C2 C1 H1 109.2 . . ? C8 C2 C1 117.7(5) . 2_566 ? C8 C2 C1 118.7(5) . . ? C1 C2 C1 88.2(4) 2_566 . ? C8 C2 H2 110.2 . . ? C1 C2 H2 110.2 2_566 . ? C1 C2 H2 110.2 . . ? C7 C3 C4 116.2(6) . . ? C7 C3 C1 119.4(5) . . ? C4 C3 C1 124.4(5) . . ? C5 C4 C3 120.8(6) . . ? C5 C4 H4 119.6 . . ? C3 C4 H4 119.6 . . ? N1 C5 C4 119.5(6) . . ? N1 C5 H5 120.2 . . ? C4 C5 H5 120.2 . . ? N1 C6 C7 119.8(6) . . ? N1 C6 H6 120.1 . . ? C7 C6 H6 120.1 . . ? C6 C7 C3 121.2(6) . . ? C6 C7 H7 119.4 . . ? C3 C7 H7 119.4 . . ? C12 C8 C9 117.4(6) . . ? C12 C8 C2 119.4(6) . . ? C9 C8 C2 123.1(5) . . ? C10 C9 C8 118.8(6) . . ? C10 C9 H9 120.6 . . ? C8 C9 H9 120.6 . . ? N2 C10 C9 119.9(7) . . ? N2 C10 H10 120.1 . . ? C9 C10 H10 120.1 . . ? N2 C11 C12 120.2(7) . . ? N2 C11 H11 119.9 . . ? C12 C11 H11 119.9 . . ? C11 C12 C8 121.4(7) . . ? C11 C12 H12 119.3 . . ? C8 C12 H12 119.3 . . ? _diffrn_measured_fraction_theta_max 0.765 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.974 _refine_diff_density_max 1.956 _refine_diff_density_min -1.267 _refine_diff_density_rms 0.219 #======================================================== data_shelxle1 _database_code_depnum_ccdc_archive 'CCDC 668917' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H24 N4, Mo8 O26' _chemical_formula_sum 'C24 H24 Mo8 N4 O26' _chemical_formula_weight 1551.99 _chemical_compound_source Synthesis 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' Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall -P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.704(2) _cell_length_b 10.070(2) _cell_length_c 10.482(2) _cell_angle_alpha 98.800(4) _cell_angle_beta 108.104(6) _cell_angle_gamma 99.049(5) _cell_volume 939.0(4) _cell_formula_units_Z 1 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 1850 _cell_measurement_theta_min 2.02 _cell_measurement_theta_max 28.02 _exptl_crystal_description Prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.745 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 740 _exptl_absorpt_coefficient_mu 2.685 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_absorpt_correction_T_min 0.667 _exptl_absorpt_correction_T_max 0.796 _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku AFC7S Mercury' _diffrn_measurement_method '\w ' _diffrn_radiation_detector CCD _diffrn_measurement_device ; Mercury (2x2 bin mode) ; _diffrn_detector_area_resol_mean 14.6306 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 10775 _diffrn_reflns_av_R_equivalents 0.0264 _diffrn_reflns_av_sigmaI/netI 0.0357 _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 -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.09 _diffrn_reflns_theta_max 28.07 _reflns_number_total 3551 _reflns_number_gt 2992 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_cell_refinement 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_data_reduction 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_structure_solution 'SHELXLTL-NT V5.1 (Bruker AXS, 1998)' _computing_structure_refinement 'SHELXLTL-NT V5.1 (Bruker AXS, 1998)' _computing_molecular_graphics ; SHELXLTL-NT V5.1 (Bruker AXS, 1998) and DIAMOND (Brandenburg, 1998) ; _computing_publication_material ; SHELXLTL-NT V5.1 (Bruker AXS, 1998) and PLATON (Spek, 2003). ; _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^)+(0.0376P)^2^+2.1503P] 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 3551 _refine_ls_number_parameters 280 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0454 _refine_ls_R_factor_gt 0.0357 _refine_ls_wR_factor_ref 0.0891 _refine_ls_wR_factor_gt 0.0834 _refine_ls_goodness_of_fit_ref 1.096 _refine_ls_restrained_S_all 1.096 _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 0.70441(5) -0.23558(4) 0.66008(4) 0.02167(13) Uani 1 1 d . . . Mo2 Mo 0.31392(4) -0.03827(4) 0.50380(4) 0.01628(12) Uani 1 1 d . . . Mo3 Mo 0.56395(5) 0.28742(4) 0.63265(4) 0.01888(13) Uani 1 1 d . . . Mo4 Mo 0.58252(4) 0.01386(4) 0.78893(4) 0.01797(13) Uani 1 1 d . . . O1 O 0.4298(3) 0.0967(3) 0.6736(3) 0.0177(7) Uani 1 1 d . . . O2 O 0.4693(4) -0.0986(4) 0.8368(4) 0.0249(8) Uani 1 1 d . . . O3 O 0.1956(4) 0.0638(4) 0.4299(3) 0.0233(8) Uani 1 1 d . . . O4 O 0.3741(4) 0.3136(3) 0.5344(4) 0.0235(8) Uani 1 1 d . . . O5 O 0.5196(3) -0.1087(3) 0.5678(3) 0.0187(7) Uani 1 1 d . . . O6 O 0.7463(4) -0.0713(4) 0.8000(3) 0.0237(8) Uani 1 1 d . . . O7 O 0.6963(3) 0.1530(3) 0.6685(3) 0.0189(7) Uani 1 1 d . . . O8 O 0.6743(4) 0.3923(4) 0.5737(4) 0.0282(9) Uani 1 1 d . . . O9 O 0.2097(4) -0.1490(4) 0.5596(4) 0.0249(8) Uani 1 1 d . . . O10 O 0.6674(4) 0.1453(4) 0.9295(4) 0.0329(9) Uani 1 1 d . . . O11 O 0.5887(4) -0.3401(4) 0.7126(4) 0.0320(9) Uani 1 1 d . . . O12 O 0.5959(4) 0.3704(4) 0.7964(4) 0.0301(9) Uani 1 1 d . . . O13 O 0.8698(4) -0.2848(4) 0.7095(4) 0.0366(10) Uani 1 1 d . . . N1 N 0.0110(5) 0.1589(5) -0.1105(5) 0.0357(12) Uani 1 1 d . . . H1N H -0.0833 0.1328 -0.1300 0.043 Uiso 1 1 calc R . . N2 N -0.2072(5) 0.5052(5) 0.3861(5) 0.0369(12) Uani 1 1 d . . . H2N H -0.2540 0.5109 0.4435 0.044 Uiso 1 1 calc R . . C1 C -0.0268(6) 0.3849(5) -0.0283(5) 0.0266(12) Uani 1 1 d . . . H1 H -0.1272 0.3320 -0.0463 0.032 Uiso 1 1 calc R . . C2 C 0.0298(6) 0.4920(6) 0.1081(5) 0.0282(12) Uani 1 1 d . . . H2 H 0.1328 0.4905 0.1592 0.034 Uiso 1 1 calc R . . C3 C 0.0772(6) 0.2913(6) -0.0467(5) 0.0266(12) Uani 1 1 d . . . C4 C 0.0859(7) 0.0671(6) -0.1443(6) 0.0384(14) Uani 1 1 d . . . H4 H 0.0351 -0.0228 -0.1881 0.046 Uiso 1 1 calc R . . C5 C 0.2347(6) 0.1024(6) -0.1161(6) 0.0343(14) Uani 1 1 d . . . H5 H 0.2859 0.0385 -0.1418 0.041 Uiso 1 1 calc R . . C6 C 0.3080(6) 0.2349(6) -0.0487(6) 0.0340(13) Uani 1 1 d . . . H6 H 0.4102 0.2612 -0.0272 0.041 Uiso 1 1 calc R . . C7 C 0.2293(7) 0.3299(6) -0.0125(6) 0.0308(13) Uani 1 1 d . . . H7 H 0.2791 0.4192 0.0346 0.037 Uiso 1 1 calc R . . C8 C -0.0604(6) 0.4907(6) 0.2033(5) 0.0274(12) Uani 1 1 d . . . C9 C -0.1789(7) 0.3862(6) 0.1896(5) 0.0321(13) Uani 1 1 d . . . H9 H -0.2094 0.3102 0.1168 0.039 Uiso 1 1 calc R . . C10 C -0.2516(6) 0.3943(6) 0.2829(6) 0.0339(13) Uani 1 1 d . . . H10 H -0.3304 0.3239 0.2746 0.041 Uiso 1 1 calc R . . C11 C -0.0931(7) 0.6071(6) 0.4031(6) 0.0345(14) Uani 1 1 d . . . H11 H -0.0644 0.6822 0.4765 0.041 Uiso 1 1 calc R . . C12 C -0.0195(6) 0.6006(5) 0.3134(6) 0.0287(12) Uani 1 1 d . . . H12 H 0.0604 0.6716 0.3259 0.034 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mo1 0.0243(2) 0.0204(2) 0.0244(2) 0.00829(19) 0.01023(19) 0.00935(19) Mo2 0.0156(2) 0.0157(2) 0.0180(2) 0.00266(17) 0.00745(18) 0.00212(17) Mo3 0.0214(2) 0.0132(2) 0.0221(2) 0.00242(18) 0.00882(19) 0.00244(18) Mo4 0.0201(2) 0.0178(2) 0.0163(2) 0.00303(17) 0.00737(18) 0.00294(18) O1 0.0211(17) 0.0144(16) 0.0187(17) 0.0019(14) 0.0098(14) 0.0028(14) O2 0.0260(19) 0.0242(19) 0.0256(19) 0.0048(16) 0.0120(16) 0.0026(16) O3 0.0194(17) 0.029(2) 0.0240(18) 0.0058(16) 0.0096(15) 0.0064(15) O4 0.0251(18) 0.0201(18) 0.0286(19) 0.0036(15) 0.0118(16) 0.0106(15) O5 0.0189(17) 0.0174(17) 0.0214(17) 0.0031(14) 0.0092(15) 0.0043(14) O6 0.0204(17) 0.027(2) 0.0218(18) 0.0062(15) 0.0047(15) 0.0030(15) O7 0.0195(17) 0.0179(17) 0.0166(16) 0.0002(14) 0.0063(14) -0.0005(14) O8 0.030(2) 0.0200(19) 0.037(2) 0.0069(17) 0.0153(17) 0.0037(16) O9 0.0254(19) 0.0219(19) 0.0268(19) 0.0053(15) 0.0107(16) -0.0003(15) O10 0.036(2) 0.029(2) 0.026(2) 0.0009(17) 0.0074(17) -0.0006(18) O11 0.041(2) 0.029(2) 0.033(2) 0.0129(18) 0.0185(19) 0.0091(18) O12 0.039(2) 0.023(2) 0.027(2) 0.0003(16) 0.0141(17) 0.0049(17) O13 0.035(2) 0.041(2) 0.044(2) 0.020(2) 0.0163(19) 0.0233(19) N1 0.028(2) 0.033(3) 0.048(3) 0.006(2) 0.016(2) 0.008(2) N2 0.048(3) 0.037(3) 0.040(3) 0.008(2) 0.035(2) 0.009(2) C1 0.025(3) 0.023(3) 0.029(3) 0.005(2) 0.007(2) 0.002(2) C2 0.027(3) 0.028(3) 0.026(3) 0.006(2) 0.004(2) 0.006(2) C3 0.033(3) 0.030(3) 0.028(3) 0.011(2) 0.020(2) 0.016(2) C4 0.037(3) 0.035(3) 0.042(3) -0.001(3) 0.015(3) 0.011(3) C5 0.032(3) 0.043(4) 0.035(3) 0.004(3) 0.018(3) 0.020(3) C6 0.026(3) 0.046(4) 0.033(3) 0.015(3) 0.009(2) 0.013(3) C7 0.045(3) 0.023(3) 0.028(3) 0.007(2) 0.015(3) 0.008(3) C8 0.039(3) 0.027(3) 0.025(3) 0.010(2) 0.016(2) 0.015(2) C9 0.050(4) 0.021(3) 0.024(3) -0.001(2) 0.017(3) 0.003(3) C10 0.035(3) 0.025(3) 0.043(3) 0.006(3) 0.018(3) 0.001(2) C11 0.044(3) 0.031(3) 0.030(3) 0.001(2) 0.019(3) 0.003(3) C12 0.021(3) 0.023(3) 0.037(3) 0.006(2) 0.006(2) 0.000(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mo1 O11 1.691(4) . ? Mo1 O13 1.704(4) . ? Mo1 O4 1.926(3) 2_656 ? Mo1 O6 1.931(4) . ? Mo1 O3 2.316(4) 2_656 ? Mo1 O5 2.409(3) . ? Mo2 O9 1.680(3) . ? Mo2 O3 1.743(3) . ? Mo2 O1 1.953(3) . ? Mo2 O7 1.954(3) 2_656 ? Mo2 O5 2.167(3) . ? Mo2 O5 2.388(3) 2_656 ? Mo2 Mo4 3.2015(8) . ? Mo3 O12 1.700(4) . ? Mo3 O8 1.702(4) . ? Mo3 O4 1.892(3) . ? Mo3 O7 2.006(3) . ? Mo3 O1 2.319(3) . ? Mo3 O5 2.374(3) 2_656 ? Mo4 O2 1.693(4) . ? Mo4 O10 1.705(4) . ? Mo4 O6 1.902(4) . ? Mo4 O1 1.984(3) . ? Mo4 O5 2.297(3) . ? Mo4 O7 2.387(3) . ? O3 Mo1 2.316(4) 2_656 ? O4 Mo1 1.926(3) 2_656 ? O5 Mo3 2.374(3) 2_656 ? O5 Mo2 2.388(3) 2_656 ? O7 Mo2 1.954(3) 2_656 ? N1 C4 1.334(7) . ? N1 C3 1.352(7) . ? N1 H1N 0.8600 . ? N2 C11 1.332(7) . ? N2 C10 1.339(7) . ? N2 H2N 0.8600 . ? C1 C3 1.520(7) . ? C1 C2 1.538(7) . ? C1 C2 1.597(7) 2_565 ? C1 H1 0.9800 . ? C2 C8 1.518(8) . ? C2 C1 1.597(7) 2_565 ? C2 H2 0.9800 . ? C3 C7 1.380(8) . ? C4 C5 1.357(8) . ? C4 H4 0.9300 . ? C5 C6 1.373(8) . ? C5 H5 0.9300 . ? C6 C7 1.393(8) . ? C6 H6 0.9300 . ? C7 H7 0.9300 . ? C8 C12 1.378(7) . ? C8 C9 1.386(8) . ? C9 C10 1.372(8) . ? C9 H9 0.9300 . ? C10 H10 0.9300 . ? C11 C12 1.345(8) . ? C11 H11 0.9300 . ? C12 H12 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O11 Mo1 O13 105.84(19) . . ? O11 Mo1 O4 99.68(17) . 2_656 ? O13 Mo1 O4 102.38(17) . 2_656 ? O11 Mo1 O6 98.66(17) . . ? O13 Mo1 O6 100.71(18) . . ? O4 Mo1 O6 145.17(15) 2_656 . ? O11 Mo1 O3 163.48(16) . 2_656 ? O13 Mo1 O3 90.64(16) . 2_656 ? O4 Mo1 O3 77.45(14) 2_656 2_656 ? O6 Mo1 O3 76.58(14) . 2_656 ? O11 Mo1 O5 93.21(15) . . ? O13 Mo1 O5 160.90(16) . . ? O4 Mo1 O5 75.21(13) 2_656 . ? O6 Mo1 O5 74.43(13) . . ? O3 Mo1 O5 70.30(12) 2_656 . ? O9 Mo2 O3 104.51(17) . . ? O9 Mo2 O1 101.62(15) . . ? O3 Mo2 O1 97.13(15) . . ? O9 Mo2 O7 100.94(16) . 2_656 ? O3 Mo2 O7 96.56(15) . 2_656 ? O1 Mo2 O7 149.66(14) . 2_656 ? O9 Mo2 O5 99.06(16) . . ? O3 Mo2 O5 156.42(15) . . ? O1 Mo2 O5 77.89(13) . . ? O7 Mo2 O5 78.76(13) 2_656 . ? O9 Mo2 O5 174.72(15) . 2_656 ? O3 Mo2 O5 80.76(14) . 2_656 ? O1 Mo2 O5 77.52(12) . 2_656 ? O7 Mo2 O5 78.14(12) 2_656 2_656 ? O5 Mo2 O5 75.66(14) . 2_656 ? O9 Mo2 Mo4 90.05(12) . . ? O3 Mo2 Mo4 133.05(11) . . ? O1 Mo2 Mo4 35.92(10) . . ? O7 Mo2 Mo4 124.59(10) 2_656 . ? O5 Mo2 Mo4 45.84(8) . . ? O5 Mo2 Mo4 86.28(8) 2_656 . ? O12 Mo3 O8 105.00(18) . . ? O12 Mo3 O4 103.40(17) . . ? O8 Mo3 O4 101.03(17) . . ? O12 Mo3 O7 100.22(16) . . ? O8 Mo3 O7 95.67(16) . . ? O4 Mo3 O7 146.27(14) . . ? O12 Mo3 O1 88.58(15) . . ? O8 Mo3 O1 163.75(15) . . ? O4 Mo3 O1 84.03(14) . . ? O7 Mo3 O1 72.77(12) . . ? O12 Mo3 O5 159.94(15) . 2_656 ? O8 Mo3 O5 94.55(15) . 2_656 ? O4 Mo3 O5 76.67(13) . 2_656 ? O7 Mo3 O5 72.94(12) . 2_656 ? O1 Mo3 O5 71.41(11) . 2_656 ? O2 Mo4 O10 105.30(18) . . ? O2 Mo4 O6 102.64(16) . . ? O10 Mo4 O6 98.21(17) . . ? O2 Mo4 O1 98.51(16) . . ? O10 Mo4 O1 101.09(16) . . ? O6 Mo4 O1 146.34(14) . . ? O2 Mo4 O5 96.18(15) . . ? O10 Mo4 O5 158.49(16) . . ? O6 Mo4 O5 77.70(13) . . ? O1 Mo4 O5 74.22(12) . . ? O2 Mo4 O7 166.16(14) . . ? O10 Mo4 O7 86.47(15) . . ? O6 Mo4 O7 82.41(14) . . ? O1 Mo4 O7 71.61(12) . . ? O5 Mo4 O7 72.09(11) . . ? O2 Mo4 Mo2 86.68(12) . . ? O10 Mo4 Mo2 136.37(13) . . ? O6 Mo4 Mo2 120.29(10) . . ? O1 Mo4 Mo2 35.29(9) . . ? O5 Mo4 Mo2 42.58(8) . . ? O7 Mo4 Mo2 79.69(8) . . ? Mo2 O1 Mo4 108.79(15) . . ? Mo2 O1 Mo3 111.88(14) . . ? Mo4 O1 Mo3 104.74(13) . . ? Mo2 O3 Mo1 116.48(16) . 2_656 ? Mo3 O4 Mo1 116.90(17) . 2_656 ? Mo2 O5 Mo4 91.58(12) . . ? Mo2 O5 Mo3 91.70(11) . 2_656 ? Mo4 O5 Mo3 163.86(16) . 2_656 ? Mo2 O5 Mo2 104.34(14) . 2_656 ? Mo4 O5 Mo2 98.23(12) . 2_656 ? Mo3 O5 Mo2 96.25(12) 2_656 2_656 ? Mo2 O5 Mo1 163.19(17) . . ? Mo4 O5 Mo1 86.58(11) . . ? Mo3 O5 Mo1 85.72(11) 2_656 . ? Mo2 O5 Mo1 92.45(11) 2_656 . ? Mo4 O6 Mo1 114.74(16) . . ? Mo2 O7 Mo3 110.85(15) 2_656 . ? Mo2 O7 Mo4 108.99(14) 2_656 . ? Mo3 O7 Mo4 101.64(14) . . ? C4 N1 C3 122.7(5) . . ? C4 N1 H1N 118.6 . . ? C3 N1 H1N 118.6 . . ? C11 N2 C10 122.4(5) . . ? C11 N2 H2N 118.8 . . ? C10 N2 H2N 118.8 . . ? C3 C1 C2 115.5(4) . . ? C3 C1 C2 115.9(4) . 2_565 ? C2 C1 C2 89.0(4) . 2_565 ? C3 C1 H1 111.6 . . ? C2 C1 H1 111.6 . . ? C2 C1 H1 111.6 2_565 . ? C8 C2 C1 119.2(4) . . ? C8 C2 C1 116.1(4) . 2_565 ? C1 C2 C1 91.0(4) . 2_565 ? C8 C2 H2 109.7 . . ? C1 C2 H2 109.7 . . ? C1 C2 H2 109.7 2_565 . ? N1 C3 C7 117.6(5) . . ? N1 C3 C1 115.6(5) . . ? C7 C3 C1 126.6(5) . . ? N1 C4 C5 121.2(6) . . ? N1 C4 H4 119.4 . . ? C5 C4 H4 119.4 . . ? C4 C5 C6 118.4(5) . . ? C4 C5 H5 120.8 . . ? C6 C5 H5 120.8 . . ? C5 C6 C7 120.0(5) . . ? C5 C6 H6 120.0 . . ? C7 C6 H6 120.0 . . ? C3 C7 C6 119.9(5) . . ? C3 C7 H7 120.1 . . ? C6 C7 H7 120.1 . . ? C12 C8 C9 117.4(5) . . ? C12 C8 C2 117.5(5) . . ? C9 C8 C2 125.0(5) . . ? C10 C9 C8 120.3(5) . . ? C10 C9 H9 119.8 . . ? C8 C9 H9 119.8 . . ? N2 C10 C9 119.0(5) . . ? N2 C10 H10 120.5 . . ? C9 C10 H10 120.5 . . ? N2 C11 C12 119.6(5) . . ? N2 C11 H11 120.2 . . ? C12 C11 H11 120.2 . . ? C11 C12 C8 121.3(5) . . ? C11 C12 H12 119.3 . . ? C8 C12 H12 119.3 . . ? _diffrn_measured_fraction_theta_max 0.778 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.970 _refine_diff_density_max 1.189 _refine_diff_density_min -0.856 _refine_diff_density_rms 0.152 #======================================================== data_p21n _database_code_depnum_ccdc_archive 'CCDC 668918' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '(C48 H44 N8 Mo8 O26), 12(H2O)' _chemical_formula_sum 'C48 H68 Mo8 N8 O38' _chemical_formula_weight 2132.62 _chemical_compound_source Synthesis 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' Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/n _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 13.0150(4) _cell_length_b 20.6053(4) _cell_length_c 12.9391(3) _cell_angle_alpha 90.00 _cell_angle_beta 102.3160(10) _cell_angle_gamma 90.00 _cell_volume 3390.12(15) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5215 _cell_measurement_theta_min 1.88 _cell_measurement_theta_max 28.04 _exptl_crystal_description needle _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.089 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2104 _exptl_absorpt_coefficient_mu 1.533 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_absorpt_correction_T_min 0.738 _exptl_absorpt_correction_T_max 0.842 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku AFC7S Mercury' _diffrn_measurement_method '\w ' _diffrn_radiation_detector CCD _diffrn_measurement_device ; Mercury (2x2 bin mode) ; _diffrn_detector_area_resol_mean 14.6306 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 38836 _diffrn_reflns_av_R_equivalents 0.0972 _diffrn_reflns_av_sigmaI/netI 0.0950 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.88 _diffrn_reflns_theta_max 28.06 _reflns_number_total 6620 _reflns_number_gt 4128 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_cell_refinement 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_data_reduction 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_structure_solution 'SHELXLTL-NT V5.1 (Bruker AXS, 1998)' _computing_structure_refinement 'SHELXLTL-NT V5.1 (Bruker AXS, 1998)' _computing_molecular_graphics ; SHELXLTL-NT V5.1 (Bruker AXS, 1998) and DIAMOND (Brandenburg, 1998) ; _computing_publication_material ; SHELXLTL-NT V5.1 (Bruker AXS, 1998) and PLATON (Spek, 2003). ; _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^)+(0.0555P)^2^+21.7959P] 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 6620 _refine_ls_number_parameters 452 _refine_ls_number_restraints 36 _refine_ls_R_factor_all 0.1265 _refine_ls_R_factor_gt 0.0675 _refine_ls_wR_factor_ref 0.1687 _refine_ls_wR_factor_gt 0.1385 _refine_ls_goodness_of_fit_ref 1.068 _refine_ls_restrained_S_all 1.071 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mo1 Mo 1.22861(6) -0.05841(4) 0.34061(7) 0.0369(2) Uani 1 1 d . . . Mo2 Mo 1.41891(6) 0.05401(4) 0.41788(7) 0.0320(2) Uani 1 1 d . . . Mo3 Mo 1.33950(6) 0.00251(4) 0.62756(7) 0.0351(2) Uani 1 1 d . . . Mo4 Mo 1.55139(7) 0.08458(5) 0.73109(7) 0.0416(3) Uani 1 1 d . . . O1 O 1.4741(4) 0.0457(3) 0.5690(5) 0.0310(14) Uani 1 1 d . . . O2 O 1.5329(5) 0.0789(3) 0.3782(5) 0.0363(15) Uani 1 1 d . . . O3 O 1.3442(5) 0.1220(3) 0.4056(6) 0.0446(17) Uani 1 1 d . . . O4 O 1.3122(5) -0.0101(3) 0.4769(5) 0.0324(15) Uani 1 1 d . . . O5 O 1.3529(5) 0.0046(3) 0.2981(5) 0.0356(15) Uani 1 1 d . . . O6 O 1.6223(6) 0.0864(4) 0.8587(6) 0.058(2) Uani 1 1 d . . . O7 O 1.4472(5) 0.0211(3) 0.7530(5) 0.0418(17) Uani 1 1 d . . . O9 O 1.3395(5) -0.1175(3) 0.3416(5) 0.0416(17) Uani 1 1 d . . . O10 O 1.2617(5) 0.0685(3) 0.6304(6) 0.0480(19) Uani 1 1 d . . . O11 O 1.1649(5) -0.0613(4) 0.2102(6) 0.0508(19) Uani 1 1 d . . . O12 O 1.2742(5) -0.0598(3) 0.6736(6) 0.0524(19) Uani 1 1 d . . . O13 O 1.1493(5) -0.1000(3) 0.4054(6) 0.0483(18) Uani 1 1 d . . . O14 O 1.4795(5) 0.1539(4) 0.7175(6) 0.059(2) Uani 1 1 d . . . C1 C 0.9471(7) 0.2052(5) 0.3473(8) 0.036(2) Uani 1 1 d . . . H1A H 0.9824 0.2418 0.3211 0.044 Uiso 1 1 calc R . . C2 C 0.9029(7) 0.2284(5) 0.4450(8) 0.041(2) Uani 1 1 d . . . H2 H 0.8788 0.1904 0.4788 0.049 Uiso 1 1 calc R . . C3 C 0.8077(7) 0.2574(5) 0.3626(8) 0.041(2) Uani 1 1 d . . . H3 H 0.8288 0.2993 0.3380 0.049 Uiso 1 1 calc R . . C4 C 0.8302(7) 0.2032(5) 0.2862(8) 0.038(2) Uani 1 1 d . . . H4 H 0.7980 0.1625 0.3026 0.046 Uiso 1 1 calc R . . C5 C 1.0139(7) 0.1452(4) 0.3489(8) 0.036(2) Uani 1 1 d . . . C6 C 1.0610(8) 0.1331(5) 0.2660(8) 0.044(3) Uani 1 1 d . . . H6 H 1.0547 0.1623 0.2102 0.052 Uiso 1 1 calc R . . C7 C 1.1179(8) 0.0768(5) 0.2669(8) 0.045(3) Uani 1 1 d . . . H7 H 1.1481 0.0684 0.2094 0.054 Uiso 1 1 calc R . . C8 C 1.0865(7) 0.0470(5) 0.4270(8) 0.045(3) Uani 1 1 d . . . H8 H 1.0980 0.0187 0.4843 0.054 Uiso 1 1 calc R . . C9 C 1.0249(8) 0.0992(5) 0.4305(8) 0.045(3) Uani 1 1 d . . . H9 H 0.9904 0.1046 0.4859 0.054 Uiso 1 1 calc R . . C10 C 0.9613(8) 0.2718(6) 0.5278(8) 0.047(3) Uani 1 1 d . . . C11 C 1.0167(9) 0.3253(6) 0.5092(9) 0.055(3) Uani 1 1 d . . . H11 H 1.0261 0.3330 0.4410 0.065 Uiso 1 1 calc R . . C12 C 1.0572(10) 0.3665(7) 0.5857(12) 0.077(4) Uani 1 1 d . . . H12 H 1.0951 0.4023 0.5708 0.092 Uiso 1 1 calc R . . N2 N 1.0439(10) 0.3567(9) 0.6845(13) 0.118(6) Uani 1 1 d . . . H2N H 1.0669 0.3850 0.7328 0.142 Uiso 1 1 calc R . . C14 C 0.9523(12) 0.2595(8) 0.6316(11) 0.087(5) Uani 1 1 d . . . H14 H 0.9180 0.2224 0.6476 0.105 Uiso 1 1 calc R . . C15 C 0.7044(9) 0.2654(6) 0.3928(13) 0.075(3) Uani 1 1 d U . . C16 C 0.6619(9) 0.2183(6) 0.4496(12) 0.075(3) Uani 1 1 d U . . H16 H 0.6957 0.1786 0.4646 0.090 Uiso 1 1 calc R . . C17 C 0.5695(10) 0.2306(7) 0.4837(15) 0.094(3) Uani 1 1 d U . . H17 H 0.5450 0.1992 0.5241 0.113 Uiso 1 1 calc R . . N3 N 0.5148(10) 0.2848(7) 0.4617(14) 0.114(3) Uani 1 1 d U . . C18 C 0.5528(13) 0.3297(8) 0.4022(17) 0.118(4) Uani 1 1 d U . . H18 H 0.5133 0.3669 0.3816 0.142 Uiso 1 1 calc R . . C19 C 0.6495(10) 0.3224(7) 0.3703(15) 0.097(3) Uani 1 1 d U . . H19 H 0.6755 0.3557 0.3347 0.116 Uiso 1 1 calc R . . C20 C 0.8054(7) 0.2134(5) 0.1698(9) 0.040(2) Uani 1 1 d . . . C21 C 0.7715(8) 0.2722(6) 0.1199(10) 0.054(3) Uani 1 1 d . . . H21 H 0.7642 0.3084 0.1606 0.064 Uiso 1 1 calc R . . C22 C 0.7497(10) 0.2768(8) 0.0152(12) 0.071(4) Uani 1 1 d . . . H22 H 0.7225 0.3155 -0.0162 0.086 Uiso 1 1 calc R . . C23 C 0.7992(9) 0.1702(7) -0.0036(11) 0.063(4) Uani 1 1 d . . . H23 H 0.8094 0.1360 -0.0473 0.076 Uiso 1 1 calc R . . C24 C 0.8183(8) 0.1614(6) 0.1039(10) 0.057(3) Uani 1 1 d . . . H24 H 0.8398 0.1211 0.1329 0.069 Uiso 1 1 calc R . . N1 N 1.1323(6) 0.0334(4) 0.3455(7) 0.0367(19) Uani 1 1 d . . . C13 C 0.9944(15) 0.3025(10) 0.7093(13) 0.114(6) Uani 1 1 d . . . H13 H 0.9893 0.2948 0.7789 0.137 Uiso 1 1 calc R . . N4 N 0.7656(7) 0.2279(7) -0.0458(9) 0.071(3) Uani 1 1 d . . . H4N H 0.7544 0.2332 -0.1132 0.085 Uiso 1 1 calc R . . O1W O 1.2639(8) -0.2398(5) 0.2587(7) 0.094(3) Uani 1 1 d . . . O2W O 1.297(3) 0.0551(17) 1.082(3) 0.194(10) Uiso 0.60 1 d P . . O2WA O 1.230(4) 0.019(2) 1.042(4) 0.194(10) Uiso 0.40 1 d P . . O3W O 1.039(3) -0.014(3) 0.979(4) 0.260(16) Uiso 0.56 1 d P . . O3WA O 1.125(5) -0.009(3) 0.952(5) 0.260(16) Uiso 0.44 1 d P . . O4W O 1.079(3) 0.0519(17) 0.725(3) 0.190(10) Uiso 0.54 1 d P . . O4WA O 1.133(3) 0.003(2) 0.821(3) 0.190(10) Uiso 0.46 1 d P . . O5W O 1.147(2) -0.4648(15) 0.572(2) 0.141(7) Uiso 0.50 1 d P . . O5WA O 1.070(2) -0.4825(15) 0.540(2) 0.141(7) Uiso 0.50 1 d P . . O6W O 0.2923(18) 0.1315(12) 0.1450(18) 0.151(7) Uiso 0.65 1 d P . . O6WA O 0.199(3) 0.161(2) 0.095(3) 0.151(7) Uiso 0.35 1 d P . . 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 0.0322(5) 0.0348(5) 0.0437(6) -0.0032(4) 0.0078(4) 0.0007(4) Mo2 0.0354(5) 0.0253(5) 0.0360(5) 0.0017(4) 0.0087(4) 0.0030(3) Mo3 0.0357(5) 0.0325(5) 0.0395(5) 0.0015(4) 0.0133(4) 0.0018(4) Mo4 0.0386(5) 0.0434(6) 0.0433(6) -0.0129(4) 0.0095(4) 0.0033(4) O1 0.035(3) 0.025(4) 0.033(4) 0.000(3) 0.007(3) -0.001(3) O2 0.043(4) 0.024(4) 0.043(4) 0.002(3) 0.014(3) 0.003(3) O3 0.051(4) 0.030(4) 0.052(5) -0.001(3) 0.010(3) 0.009(3) O4 0.035(3) 0.030(4) 0.033(4) 0.003(3) 0.009(3) 0.002(3) O5 0.037(4) 0.034(4) 0.035(4) -0.005(3) 0.006(3) 0.007(3) O6 0.051(4) 0.072(6) 0.049(5) -0.012(4) 0.004(4) 0.004(4) O7 0.032(4) 0.059(5) 0.036(4) -0.002(3) 0.012(3) 0.002(3) O9 0.043(4) 0.029(4) 0.054(5) -0.002(3) 0.014(3) 0.003(3) O10 0.048(4) 0.043(5) 0.054(5) -0.011(4) 0.014(3) 0.004(3) O11 0.042(4) 0.060(5) 0.047(5) -0.011(4) 0.003(3) 0.005(3) O12 0.057(5) 0.045(5) 0.064(5) 0.006(4) 0.031(4) -0.005(3) O13 0.044(4) 0.040(4) 0.063(5) -0.003(4) 0.017(3) -0.010(3) O14 0.050(4) 0.052(5) 0.077(6) -0.026(4) 0.020(4) 0.007(4) C1 0.032(5) 0.035(6) 0.041(6) 0.010(5) 0.005(4) 0.004(4) C2 0.040(6) 0.042(6) 0.044(7) -0.009(5) 0.014(5) 0.001(5) C3 0.038(6) 0.028(6) 0.056(7) -0.010(5) 0.008(5) 0.005(4) C4 0.043(6) 0.026(5) 0.045(7) 0.006(5) 0.006(5) 0.001(4) C5 0.042(6) 0.026(5) 0.038(6) -0.002(5) 0.006(4) 0.000(4) C6 0.054(6) 0.041(6) 0.045(7) 0.006(5) 0.029(5) 0.003(5) C7 0.045(6) 0.053(7) 0.039(7) -0.002(6) 0.018(5) 0.010(5) C8 0.038(6) 0.060(8) 0.038(6) -0.001(5) 0.014(5) 0.000(5) C9 0.046(6) 0.049(7) 0.044(7) 0.006(5) 0.022(5) 0.014(5) C10 0.050(6) 0.056(7) 0.036(7) -0.010(5) 0.013(5) -0.009(5) C11 0.064(7) 0.057(8) 0.040(7) -0.015(6) 0.005(5) -0.012(6) C12 0.077(9) 0.079(11) 0.067(10) -0.021(9) 0.001(8) -0.005(7) N2 0.087(10) 0.148(15) 0.115(13) -0.088(12) 0.011(9) -0.034(9) C14 0.103(11) 0.104(13) 0.059(10) -0.009(9) 0.027(8) -0.027(9) C15 0.045(5) 0.040(6) 0.148(9) -0.003(6) 0.036(6) 0.005(4) C16 0.049(5) 0.045(6) 0.141(8) -0.011(6) 0.043(6) 0.004(5) C17 0.065(6) 0.061(7) 0.166(9) -0.002(7) 0.046(6) 0.006(5) N3 0.079(6) 0.076(7) 0.197(9) 0.009(7) 0.053(6) 0.008(5) C18 0.087(7) 0.071(7) 0.208(10) 0.016(7) 0.053(7) 0.017(6) C19 0.064(6) 0.052(6) 0.185(9) 0.011(7) 0.049(6) 0.008(5) C20 0.031(5) 0.038(6) 0.049(7) 0.001(5) 0.004(5) -0.007(4) C21 0.050(7) 0.049(7) 0.052(8) 0.014(6) -0.012(5) -0.012(5) C22 0.061(8) 0.077(11) 0.072(11) 0.028(9) 0.005(7) -0.012(7) C23 0.046(7) 0.092(11) 0.052(9) -0.016(8) 0.011(6) -0.019(7) C24 0.036(6) 0.068(9) 0.066(9) 0.006(7) 0.006(5) 0.000(5) N1 0.032(4) 0.035(5) 0.041(5) 0.007(4) 0.005(4) 0.008(3) C13 0.131(15) 0.149(18) 0.065(12) -0.061(12) 0.028(10) -0.029(14) N4 0.052(6) 0.114(11) 0.042(7) 0.026(7) 0.001(5) -0.021(6) O1W 0.135(9) 0.086(7) 0.064(6) -0.023(6) 0.031(6) -0.014(6) _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 O13 1.695(7) . ? Mo1 O11 1.715(7) . ? Mo1 O9 1.886(6) . ? Mo1 O4 2.114(6) . ? Mo1 O5 2.233(6) . ? Mo1 N1 2.277(8) . ? Mo2 O3 1.693(6) . ? Mo2 O2 1.747(6) . ? Mo2 O5 1.900(6) . ? Mo2 O1 1.942(6) . ? Mo2 O4 2.170(6) . ? Mo2 O1 2.467(6) 3_856 ? Mo3 O10 1.701(7) . ? Mo3 O12 1.715(7) . ? Mo3 O4 1.923(6) . ? Mo3 O7 1.943(6) . ? Mo3 O1 2.236(6) . ? Mo3 O2 2.373(6) 3_856 ? Mo4 O14 1.696(7) . ? Mo4 O6 1.712(7) . ? Mo4 O7 1.948(7) . ? Mo4 O9 1.983(6) 3_856 ? Mo4 O1 2.270(6) . ? Mo4 O5 2.296(6) 3_856 ? O1 Mo2 2.467(6) 3_856 ? O2 Mo3 2.373(6) 3_856 ? O5 Mo4 2.296(6) 3_856 ? O9 Mo4 1.983(6) 3_856 ? C1 C5 1.510(13) . ? C1 C4 1.559(13) . ? C1 C2 1.570(13) . ? C1 H1A 0.9800 . ? C2 C10 1.476(14) . ? C2 C3 1.570(13) . ? C2 H2 0.9800 . ? C3 C15 1.487(15) . ? C3 C4 1.560(13) . ? C3 H3 0.9800 . ? C4 C20 1.486(14) . ? C4 H4 0.9800 . ? C5 C6 1.367(13) . ? C5 C9 1.404(13) . ? C6 C7 1.375(14) . ? C6 H6 0.9300 . ? C7 N1 1.337(12) . ? C7 H7 0.9300 . ? C8 C9 1.347(14) . ? C8 N1 1.347(12) . ? C8 H8 0.9300 . ? C9 H9 0.9300 . ? C10 C11 1.366(15) . ? C10 C14 1.396(16) . ? C11 C12 1.325(16) . ? C11 H11 0.9300 . ? C12 N2 1.342(19) . ? C12 H12 0.9300 . ? N2 C13 1.36(2) . ? N2 H2N 0.8600 . ? C14 C13 1.36(2) . ? C14 H14 0.9300 . ? C15 C19 1.374(17) . ? C15 C16 1.400(17) . ? C16 C17 1.390(17) . ? C16 H16 0.9300 . ? C17 N3 1.321(17) . ? C17 H17 0.9300 . ? N3 C18 1.36(2) . ? C18 C19 1.413(19) . ? C18 H18 0.9300 . ? C19 H19 0.9300 . ? C20 C21 1.399(14) . ? C20 C24 1.402(15) . ? C21 C22 1.327(17) . ? C21 H21 0.9300 . ? C22 N4 1.323(17) . ? C22 H22 0.9300 . ? C23 N4 1.343(16) . ? C23 C24 1.371(16) . ? C23 H23 0.9300 . ? C24 H24 0.9300 . ? C13 H13 0.9300 . ? N4 H4N 0.8600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O13 Mo1 O11 104.6(3) . . ? O13 Mo1 O9 102.5(3) . . ? O11 Mo1 O9 101.1(3) . . ? O13 Mo1 O4 94.9(3) . . ? O11 Mo1 O4 153.2(3) . . ? O9 Mo1 O4 92.4(3) . . ? O13 Mo1 O5 165.0(3) . . ? O11 Mo1 O5 90.1(3) . . ? O9 Mo1 O5 77.5(2) . . ? O4 Mo1 O5 70.2(2) . . ? O13 Mo1 N1 90.5(3) . . ? O11 Mo1 N1 84.4(3) . . ? O9 Mo1 N1 163.9(3) . . ? O4 Mo1 N1 76.9(3) . . ? O5 Mo1 N1 87.5(2) . . ? O3 Mo2 O2 103.7(3) . . ? O3 Mo2 O5 102.4(3) . . ? O2 Mo2 O5 100.5(3) . . ? O3 Mo2 O1 104.5(3) . . ? O2 Mo2 O1 99.6(3) . . ? O5 Mo2 O1 141.3(3) . . ? O3 Mo2 O4 98.0(3) . . ? O2 Mo2 O4 158.3(3) . . ? O5 Mo2 O4 75.5(3) . . ? O1 Mo2 O4 73.7(2) . . ? O3 Mo2 O1 178.5(3) . 3_856 ? O2 Mo2 O1 76.2(2) . 3_856 ? O5 Mo2 O1 76.1(2) . 3_856 ? O1 Mo2 O1 77.0(2) . 3_856 ? O4 Mo2 O1 82.1(2) . 3_856 ? O10 Mo3 O12 104.5(3) . . ? O10 Mo3 O4 98.5(3) . . ? O12 Mo3 O4 104.6(3) . . ? O10 Mo3 O7 98.7(3) . . ? O12 Mo3 O7 100.4(3) . . ? O4 Mo3 O7 144.9(3) . . ? O10 Mo3 O1 101.6(3) . . ? O12 Mo3 O1 153.8(3) . . ? O4 Mo3 O1 72.5(2) . . ? O7 Mo3 O1 74.2(2) . . ? O10 Mo3 O2 171.8(3) . 3_856 ? O12 Mo3 O2 83.3(3) . 3_856 ? O4 Mo3 O2 81.5(2) . 3_856 ? O7 Mo3 O2 77.3(3) . 3_856 ? O1 Mo3 O2 70.5(2) . 3_856 ? O14 Mo4 O6 104.7(4) . . ? O14 Mo4 O7 101.3(3) . . ? O6 Mo4 O7 97.1(3) . . ? O14 Mo4 O9 95.6(3) . 3_856 ? O6 Mo4 O9 99.0(3) . 3_856 ? O7 Mo4 O9 152.9(3) . 3_856 ? O14 Mo4 O1 94.3(3) . . ? O6 Mo4 O1 160.1(3) . . ? O7 Mo4 O1 73.3(2) . . ? O9 Mo4 O1 84.5(2) 3_856 . ? O14 Mo4 O5 164.5(3) . 3_856 ? O6 Mo4 O5 88.6(3) . 3_856 ? O7 Mo4 O5 84.6(2) . 3_856 ? O9 Mo4 O5 74.2(2) 3_856 3_856 ? O1 Mo4 O5 73.4(2) . 3_856 ? Mo2 O1 Mo3 103.2(2) . . ? Mo2 O1 Mo4 153.5(3) . . ? Mo3 O1 Mo4 93.0(2) . . ? Mo2 O1 Mo2 103.0(2) . 3_856 ? Mo3 O1 Mo2 96.7(2) . 3_856 ? Mo4 O1 Mo2 95.6(2) . 3_856 ? Mo2 O2 Mo3 116.5(3) . 3_856 ? Mo3 O4 Mo1 149.3(3) . . ? Mo3 O4 Mo2 106.3(3) . . ? Mo1 O4 Mo2 104.3(3) . . ? Mo2 O5 Mo1 109.6(3) . . ? Mo2 O5 Mo4 113.3(3) . 3_856 ? Mo1 O5 Mo4 91.3(2) . 3_856 ? Mo3 O7 Mo4 114.3(3) . . ? Mo1 O9 Mo4 113.6(3) . 3_856 ? C5 C1 C4 118.8(8) . . ? C5 C1 C2 123.1(8) . . ? C4 C1 C2 86.0(7) . . ? C5 C1 H1A 108.9 . . ? C4 C1 H1A 108.9 . . ? C2 C1 H1A 108.9 . . ? C10 C2 C1 123.3(8) . . ? C10 C2 C3 118.1(9) . . ? C1 C2 C3 86.6(7) . . ? C10 C2 H2 108.9 . . ? C1 C2 H2 108.9 . . ? C3 C2 H2 108.9 . . ? C15 C3 C4 123.2(9) . . ? C15 C3 C2 119.4(10) . . ? C4 C3 C2 86.0(7) . . ? C15 C3 H3 108.7 . . ? C4 C3 H3 108.7 . . ? C2 C3 H3 108.7 . . ? C20 C4 C1 119.2(8) . . ? C20 C4 C3 120.7(8) . . ? C1 C4 C3 87.3(7) . . ? C20 C4 H4 109.2 . . ? C1 C4 H4 109.2 . . ? C3 C4 H4 109.2 . . ? C6 C5 C9 118.4(9) . . ? C6 C5 C1 119.5(9) . . ? C9 C5 C1 122.0(9) . . ? C5 C6 C7 118.5(10) . . ? C5 C6 H6 120.7 . . ? C7 C6 H6 120.7 . . ? N1 C7 C6 124.0(9) . . ? N1 C7 H7 118.0 . . ? C6 C7 H7 118.0 . . ? C9 C8 N1 123.9(10) . . ? C9 C8 H8 118.0 . . ? N1 C8 H8 118.0 . . ? C8 C9 C5 118.7(9) . . ? C8 C9 H9 120.7 . . ? C5 C9 H9 120.7 . . ? C11 C10 C14 118.2(11) . . ? C11 C10 C2 124.8(10) . . ? C14 C10 C2 116.9(11) . . ? C12 C11 C10 121.8(13) . . ? C12 C11 H11 119.1 . . ? C10 C11 H11 119.1 . . ? C11 C12 N2 120.3(15) . . ? C11 C12 H12 119.9 . . ? N2 C12 H12 119.9 . . ? C12 N2 C13 120.8(13) . . ? C12 N2 H2N 119.6 . . ? C13 N2 H2N 119.6 . . ? C13 C14 C10 119.2(15) . . ? C13 C14 H14 120.4 . . ? C10 C14 H14 120.4 . . ? C19 C15 C16 117.2(12) . . ? C19 C15 C3 119.9(12) . . ? C16 C15 C3 122.8(11) . . ? C17 C16 C15 120.4(12) . . ? C17 C16 H16 119.8 . . ? C15 C16 H16 119.8 . . ? N3 C17 C16 123.3(15) . . ? N3 C17 H17 118.3 . . ? C16 C17 H17 118.3 . . ? C17 N3 C18 116.8(14) . . ? N3 C18 C19 123.1(15) . . ? N3 C18 H18 118.4 . . ? C19 C18 H18 118.4 . . ? C15 C19 C18 119.0(14) . . ? C15 C19 H19 120.5 . . ? C18 C19 H19 120.5 . . ? C21 C20 C24 116.6(11) . . ? C21 C20 C4 124.7(10) . . ? C24 C20 C4 118.7(10) . . ? C22 C21 C20 120.7(13) . . ? C22 C21 H21 119.6 . . ? C20 C21 H21 119.6 . . ? N4 C22 C21 121.9(13) . . ? N4 C22 H22 119.1 . . ? C21 C22 H22 119.1 . . ? N4 C23 C24 120.2(13) . . ? N4 C23 H23 119.9 . . ? C24 C23 H23 119.9 . . ? C23 C24 C20 119.8(12) . . ? C23 C24 H24 120.1 . . ? C20 C24 H24 120.1 . . ? C7 N1 C8 116.2(8) . . ? C7 N1 Mo1 121.6(6) . . ? C8 N1 Mo1 122.2(7) . . ? N2 C13 C14 119.7(16) . . ? N2 C13 H13 120.2 . . ? C14 C13 H13 120.2 . . ? C22 N4 C23 120.7(12) . . ? C22 N4 H4N 119.7 . . ? C23 N4 H4N 119.7 . . ? _diffrn_measured_fraction_theta_max 0.803 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.979 _refine_diff_density_max 1.092 _refine_diff_density_min -0.961 _refine_diff_density_rms 0.173 _vrf_PLAT306_p21n ; PROBLEM: Isolated Oxygen Atom (H-atoms Missing) O1W RESPONSE: The hydrogen atoms of this water molecule were not found from the Fourier map. Likewise, for the rest of water molecules. ;