# Supplementary Material (ESI) for CrystEngComm # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _publ_contact_author_name 'Ming-Xing Li' _publ_contact_author_email 'MX LI@MAIL.SHU.EDU.CN' _publ_section_title ; Assembly of five organic-inorganic hybrid complexes based on polyoxomolybdates and angular 4-amino-3,5-bis(pyridyl)-1,2,4-triazole ; loop_ _publ_author_name 'Ming-Xing Li' 'Hui-Ling Chen' 'Xiang He' 'Min Shao' 'Zhao-Xi Wang' ; Shou-Rong Zhu ; # Attachment '1.cif' data_090225b_0m _database_code_depnum_ccdc_archive 'CCDC 762849' #TrackingRef '1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H14 Cu Mo4 N6 O15' _chemical_formula_weight 929.59 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' Cu Cu 0.3201 1.2651 '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 9.6892(16) _cell_length_b 9.8474(16) _cell_length_c 13.533(2) _cell_angle_alpha 99.395(2) _cell_angle_beta 109.368(2) _cell_angle_gamma 101.945(2) _cell_volume 1153.6(3) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 3925 _cell_measurement_theta_min 0.00 _cell_measurement_theta_max 0.00 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.676 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 890 _exptl_absorpt_coefficient_mu 3.109 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5104 _exptl_absorpt_correction_T_max 0.5752 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5993 _diffrn_reflns_av_R_equivalents 0.0193 _diffrn_reflns_av_sigmaI/netI 0.0352 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.28 _diffrn_reflns_theta_max 25.05 _reflns_number_total 4012 _reflns_number_gt 3595 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0644P)^2^+2.3258P] 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 4012 _refine_ls_number_parameters 343 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0387 _refine_ls_R_factor_gt 0.0350 _refine_ls_wR_factor_ref 0.1040 _refine_ls_wR_factor_gt 0.0996 _refine_ls_goodness_of_fit_ref 1.061 _refine_ls_restrained_S_all 1.061 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.59089(7) 0.18133(7) 0.02505(6) 0.02699(19) Uani 1 1 d . . . Mo1 Mo 0.54582(5) 0.30702(4) 0.35944(3) 0.01648(14) Uani 1 1 d . . . Mo2 Mo 0.40530(5) 0.30006(4) 0.55554(3) 0.01632(14) Uani 1 1 d . . . Mo3 Mo 0.67600(4) 0.12113(4) 0.53650(3) 0.01290(14) Uani 1 1 d . . . Mo4 Mo 0.48809(5) 0.09143(4) 0.71241(3) 0.01589(14) Uani 1 1 d . . . C1 C 0.6546(6) 0.4516(6) -0.0306(4) 0.0221(11) Uani 1 1 d . . . H1 H 0.6270 0.3932 -0.0994 0.027 Uiso 1 1 calc R . . C2 C 0.6778(6) 0.5977(5) -0.0187(4) 0.0197(11) Uani 1 1 d . . . H2 H 0.6637 0.6360 -0.0786 0.024 Uiso 1 1 calc R . . C3 C 0.7225(5) 0.6864(5) 0.0838(4) 0.0157(10) Uani 1 1 d . . . C4 C 0.7441(6) 0.6249(5) 0.1710(4) 0.0223(11) Uani 1 1 d . . . H4 H 0.7766 0.6815 0.2411 0.027 Uiso 1 1 calc R . . C5 C 0.7162(6) 0.4776(6) 0.1515(4) 0.0225(11) Uani 1 1 d . . . H5 H 0.7303 0.4369 0.2102 0.027 Uiso 1 1 calc R . . C6 C 0.7401(5) 0.8411(5) 0.0963(4) 0.0153(10) Uani 1 1 d . . . C7 C 0.8374(5) 1.0713(5) 0.1545(4) 0.0165(10) Uani 1 1 d . . . C8 C 0.9431(5) 1.2125(5) 0.2197(4) 0.0198(11) Uani 1 1 d . . . C9 C 1.0143(7) 1.3042(6) 0.1717(5) 0.0318(13) Uani 1 1 d . . . H9 H 0.9941 1.2784 0.0980 0.038 Uiso 1 1 calc R . . C10 C 1.1143(7) 1.4327(7) 0.2353(6) 0.0404(16) Uani 1 1 d . . . H10 H 1.1648 1.4943 0.2052 0.048 Uiso 1 1 calc R . . C11 C 1.0707(7) 1.3857(6) 0.3873(5) 0.0312(14) Uani 1 1 d . . . H11 H 1.0897 1.4164 0.4605 0.037 Uiso 1 1 calc R . . C12 C 0.9701(6) 1.2522(6) 0.3278(4) 0.0272(12) Uani 1 1 d . . . H12 H 0.9227 1.1918 0.3603 0.033 Uiso 1 1 calc R . . N1 N 0.6699(5) 0.3900(5) 0.0525(4) 0.0216(9) Uani 1 1 d . . . N2 N 0.6393(5) 0.8990(4) 0.0437(3) 0.0167(9) Uani 1 1 d . . . N3 N 0.7027(5) 1.0473(4) 0.0795(3) 0.0185(9) Uani 1 1 d . . . N4 N 0.8660(5) 0.9450(4) 0.1668(3) 0.0166(9) Uani 1 1 d . . . N5 N 0.9934(5) 0.9190(5) 0.2392(4) 0.0339(12) Uani 1 1 d . . . H5A H 1.0680 0.9897 0.2843 0.041 Uiso 1 1 calc R . . H5B H 0.9971 0.8324 0.2386 0.041 Uiso 1 1 calc R . . N6 N 1.1400(6) 1.4701(5) 0.3401(4) 0.0359(12) Uani 1 1 d . . . O1 O 0.4432(5) 0.2678(4) 0.2243(3) 0.0326(10) Uani 1 1 d . . . O2 O 0.5294(5) 0.5066(4) 0.4018(3) 0.0261(9) Uani 1 1 d . . . O3 O 0.7307(4) 0.3736(4) 0.3748(3) 0.0275(9) Uani 1 1 d . . . O4 O 0.3618(4) 0.2705(4) 0.4121(3) 0.0200(8) Uani 1 1 d . . . O5 O 0.2310(4) 0.2593(5) 0.5605(3) 0.0299(9) Uani 1 1 d . . . O6 O 0.5248(4) 0.2823(4) 0.7028(3) 0.0197(8) Uani 1 1 d . . . O7 O 0.4209(4) 0.0813(3) 0.5362(3) 0.0138(7) Uani 1 1 d . . . O8 O 0.6374(4) 0.3030(4) 0.5396(3) 0.0165(7) Uani 1 1 d . . . O9 O 0.5469(4) 0.1099(4) 0.3678(3) 0.0176(7) Uani 1 1 d . . . O10 O 0.8520(4) 0.1503(4) 0.5330(3) 0.0256(9) Uani 1 1 d . . . O11 O 0.7036(4) 0.1094(4) 0.6688(3) 0.0202(8) Uani 1 1 d . . . O12 O 0.6048(5) 0.1043(4) 0.8435(3) 0.0274(9) Uani 1 1 d . . . O13 O 0.3095(4) 0.0613(4) 0.7123(3) 0.0261(9) Uani 1 1 d . . . O1W O 0.1493(7) 0.0492(7) 0.1047(5) 0.0732(17) Uani 1 1 d . . . O2W O 0.9172(9) 0.3106(9) 0.9057(7) 0.115(3) Uani 1 1 d . . . H1WA H 0.1199 -0.0420 0.0857 0.138 Uiso 1 1 d R . . H1WB H 0.0676 0.0596 0.1113 0.138 Uiso 1 1 d R . . H2WB H 0.8313 0.3234 0.9006 0.138 Uiso 1 1 d R . . H2WA H 0.9289 0.2403 0.8666 0.138 Uiso 1 1 d 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 Cu1 0.0244(4) 0.0081(3) 0.0393(4) 0.0081(3) -0.0001(3) 0.0041(3) Mo1 0.0266(3) 0.0100(2) 0.0169(2) 0.00636(18) 0.0101(2) 0.00833(19) Mo2 0.0236(3) 0.0093(2) 0.0226(3) 0.00818(18) 0.0125(2) 0.00879(18) Mo3 0.0148(2) 0.0072(2) 0.0157(2) 0.00305(17) 0.00455(17) 0.00296(17) Mo4 0.0257(3) 0.0100(2) 0.0146(2) 0.00421(17) 0.00952(18) 0.00646(18) C1 0.027(3) 0.015(3) 0.023(3) 0.004(2) 0.007(2) 0.007(2) C2 0.028(3) 0.013(3) 0.019(3) 0.007(2) 0.009(2) 0.005(2) C3 0.013(2) 0.010(2) 0.024(3) 0.006(2) 0.006(2) 0.0065(19) C4 0.032(3) 0.012(3) 0.024(3) 0.006(2) 0.012(2) 0.006(2) C5 0.029(3) 0.016(3) 0.025(3) 0.009(2) 0.010(2) 0.007(2) C6 0.015(2) 0.008(2) 0.021(2) 0.0018(19) 0.006(2) 0.0019(18) C7 0.017(2) 0.014(3) 0.019(2) 0.004(2) 0.008(2) 0.005(2) C8 0.014(2) 0.014(3) 0.025(3) 0.003(2) 0.000(2) 0.005(2) C9 0.036(3) 0.020(3) 0.035(3) 0.008(2) 0.011(3) 0.001(2) C10 0.036(4) 0.021(3) 0.059(4) 0.015(3) 0.018(3) -0.005(3) C11 0.038(3) 0.018(3) 0.028(3) -0.003(2) 0.002(3) 0.013(3) C12 0.026(3) 0.018(3) 0.030(3) 0.003(2) 0.003(2) 0.005(2) N1 0.022(2) 0.012(2) 0.029(2) 0.0066(19) 0.0066(19) 0.0056(18) N2 0.019(2) 0.008(2) 0.020(2) 0.0044(17) 0.0043(17) 0.0011(16) N3 0.020(2) 0.009(2) 0.024(2) 0.0037(17) 0.0068(18) 0.0012(17) N4 0.017(2) 0.012(2) 0.022(2) 0.0066(17) 0.0079(17) 0.0046(17) N5 0.022(2) 0.014(2) 0.052(3) 0.011(2) -0.007(2) 0.0071(19) N6 0.030(3) 0.018(3) 0.044(3) -0.001(2) 0.000(2) 0.006(2) O1 0.050(3) 0.022(2) 0.025(2) 0.0087(17) 0.0103(19) 0.0113(19) O2 0.044(2) 0.0118(19) 0.032(2) 0.0079(16) 0.0221(18) 0.0117(16) O3 0.034(2) 0.017(2) 0.040(2) 0.0145(17) 0.0201(19) 0.0088(17) O4 0.0247(19) 0.0146(18) 0.0242(19) 0.0090(15) 0.0098(16) 0.0083(15) O5 0.031(2) 0.034(2) 0.039(2) 0.0206(19) 0.0202(19) 0.0184(19) O6 0.033(2) 0.0095(18) 0.0184(18) 0.0041(14) 0.0118(16) 0.0068(15) O7 0.0211(18) 0.0074(16) 0.0138(16) 0.0037(13) 0.0063(14) 0.0055(13) O8 0.0244(19) 0.0069(17) 0.0183(17) 0.0043(14) 0.0086(15) 0.0029(14) O9 0.0257(19) 0.0123(18) 0.0171(17) 0.0064(14) 0.0086(15) 0.0071(15) O10 0.023(2) 0.022(2) 0.036(2) 0.0124(17) 0.0131(17) 0.0085(16) O11 0.0217(19) 0.021(2) 0.0166(17) 0.0046(15) 0.0048(15) 0.0070(15) O12 0.037(2) 0.023(2) 0.0208(19) 0.0069(16) 0.0078(17) 0.0105(17) O13 0.036(2) 0.019(2) 0.031(2) 0.0095(17) 0.0204(18) 0.0085(17) O1W 0.075(4) 0.075(4) 0.091(5) 0.034(4) 0.050(4) 0.024(3) O2W 0.093(6) 0.136(8) 0.112(6) 0.001(5) 0.046(5) 0.036(5) _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 Cu1 N3 1.959(4) 1_545 ? Cu1 N1 1.964(4) . ? Cu1 N2 2.029(4) 2_665 ? Mo1 O1 1.699(4) . ? Mo1 O3 1.704(4) . ? Mo1 O9 1.964(3) . ? Mo1 O2 2.009(4) . ? Mo1 O4 2.116(4) . ? Mo1 O8 2.312(3) . ? Mo2 O5 1.680(4) . ? Mo2 O4 1.804(4) . ? Mo2 O2 1.805(4) 2_666 ? Mo2 O6 2.003(3) . ? Mo2 O7 2.170(3) . ? Mo2 O8 2.324(3) . ? Mo3 O10 1.687(4) . ? Mo3 O11 1.748(3) . ? Mo3 O8 1.900(3) . ? Mo3 O7 1.948(3) 2_656 ? Mo3 O9 2.181(3) . ? Mo3 O7 2.420(3) . ? Mo4 O13 1.694(4) . ? Mo4 O12 1.726(4) . ? Mo4 O6 1.873(3) . ? Mo4 O9 2.000(3) 2_656 ? Mo4 O7 2.233(3) . ? Mo4 O11 2.332(4) . ? C1 N1 1.343(7) . ? C1 C2 1.383(7) . ? C1 H1 0.9300 . ? C2 C3 1.387(7) . ? C2 H2 0.9300 . ? C3 C4 1.387(7) . ? C3 C6 1.473(7) . ? C4 C5 1.383(7) . ? C4 H4 0.9300 . ? C5 N1 1.344(7) . ? C5 H5 0.9300 . ? C6 N2 1.299(6) . ? C6 N4 1.356(6) . ? C7 N3 1.306(6) . ? C7 N4 1.353(6) . ? C7 C8 1.474(7) . ? C8 C12 1.370(7) . ? C8 C9 1.395(8) . ? C9 C10 1.365(8) . ? C9 H9 0.9300 . ? C10 N6 1.329(8) . ? C10 H10 0.9300 . ? C11 N6 1.333(8) . ? C11 C12 1.389(8) . ? C11 H11 0.9300 . ? C12 H12 0.9300 . ? N2 N3 1.395(6) . ? N2 Cu1 2.029(4) 2_665 ? N3 Cu1 1.959(4) 1_565 ? N4 N5 1.400(6) . ? N5 H5A 0.8600 . ? N5 H5B 0.8600 . ? O2 Mo2 1.806(4) 2_666 ? O7 Mo3 1.948(3) 2_656 ? O9 Mo4 2.000(3) 2_656 ? O1W H1WA 0.8506 . ? O1W H1WB 0.8505 . ? O2W H2WB 0.8500 . ? O2W H2WB 0.8500 . ? O2W H2WA 0.8500 . ? 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 N3 Cu1 N1 127.61(17) 1_545 . ? N3 Cu1 N2 115.57(16) 1_545 2_665 ? N1 Cu1 N2 115.78(17) . 2_665 ? O1 Mo1 O3 105.5(2) . . ? O1 Mo1 O9 96.78(17) . . ? O3 Mo1 O9 99.04(16) . . ? O1 Mo1 O2 99.13(18) . . ? O3 Mo1 O2 90.70(17) . . ? O9 Mo1 O2 158.40(15) . . ? O1 Mo1 O4 98.27(18) . . ? O3 Mo1 O4 155.09(17) . . ? O9 Mo1 O4 85.29(14) . . ? O2 Mo1 O4 78.06(15) . . ? O1 Mo1 O8 164.18(17) . . ? O3 Mo1 O8 87.14(16) . . ? O9 Mo1 O8 71.40(13) . . ? O2 Mo1 O8 90.04(14) . . ? O4 Mo1 O8 70.90(13) . . ? O5 Mo2 O4 102.21(19) . . ? O5 Mo2 O2 104.30(19) . 2_666 ? O4 Mo2 O2 100.97(16) . 2_666 ? O5 Mo2 O6 98.45(17) . . ? O4 Mo2 O6 151.95(15) . . ? O2 Mo2 O6 92.00(16) 2_666 . ? O5 Mo2 O7 94.59(17) . . ? O4 Mo2 O7 86.22(14) . . ? O2 Mo2 O7 157.70(17) 2_666 . ? O6 Mo2 O7 73.32(13) . . ? O5 Mo2 O8 167.59(17) . . ? O4 Mo2 O8 75.96(14) . . ? O2 Mo2 O8 88.07(15) 2_666 . ? O6 Mo2 O8 79.77(14) . . ? O7 Mo2 O8 73.10(12) . . ? O10 Mo3 O11 104.33(18) . . ? O10 Mo3 O8 103.58(17) . . ? O11 Mo3 O8 101.15(16) . . ? O10 Mo3 O7 103.99(17) . 2_656 ? O11 Mo3 O7 98.23(15) . 2_656 ? O8 Mo3 O7 140.93(15) . 2_656 ? O10 Mo3 O9 98.85(16) . . ? O11 Mo3 O9 156.67(15) . . ? O8 Mo3 O9 75.60(13) . . ? O7 Mo3 O9 73.25(13) 2_656 . ? O10 Mo3 O7 178.24(15) . . ? O11 Mo3 O7 77.39(14) . . ? O8 Mo3 O7 75.57(13) . . ? O7 Mo3 O7 76.05(14) 2_656 . ? O9 Mo3 O7 79.45(12) . . ? O13 Mo4 O12 105.45(19) . . ? O13 Mo4 O6 100.14(17) . . ? O12 Mo4 O6 103.25(17) . . ? O13 Mo4 O9 93.92(16) . 2_656 ? O12 Mo4 O9 104.83(16) . 2_656 ? O6 Mo4 O9 143.81(15) . 2_656 ? O13 Mo4 O7 96.08(16) . . ? O12 Mo4 O7 158.39(16) . . ? O6 Mo4 O7 74.26(13) . . ? O9 Mo4 O7 71.19(13) 2_656 . ? O13 Mo4 O11 166.48(16) . . ? O12 Mo4 O11 87.20(16) . . ? O6 Mo4 O11 81.14(14) . . ? O9 Mo4 O11 77.93(13) 2_656 . ? O7 Mo4 O11 71.19(12) . . ? N1 C1 C2 123.1(5) . . ? N1 C1 H1 118.5 . . ? C2 C1 H1 118.5 . . ? C1 C2 C3 119.0(5) . . ? C1 C2 H2 120.5 . . ? C3 C2 H2 120.5 . . ? C2 C3 C4 118.6(5) . . ? C2 C3 C6 119.2(4) . . ? C4 C3 C6 122.2(4) . . ? C5 C4 C3 118.5(5) . . ? C5 C4 H4 120.7 . . ? C3 C4 H4 120.7 . . ? N1 C5 C4 123.7(5) . . ? N1 C5 H5 118.2 . . ? C4 C5 H5 118.2 . . ? N2 C6 N4 109.8(4) . . ? N2 C6 C3 126.1(4) . . ? N4 C6 C3 124.1(4) . . ? N3 C7 N4 109.6(4) . . ? N3 C7 C8 126.5(4) . . ? N4 C7 C8 123.8(4) . . ? C12 C8 C9 120.6(5) . . ? C12 C8 C7 119.2(5) . . ? C9 C8 C7 120.2(5) . . ? C10 C9 C8 118.5(6) . . ? C10 C9 H9 120.7 . . ? C8 C9 H9 120.7 . . ? N6 C10 C9 120.4(6) . . ? N6 C10 H10 119.8 . . ? C9 C10 H10 119.8 . . ? N6 C11 C12 120.4(6) . . ? N6 C11 H11 119.8 . . ? C12 C11 H11 119.8 . . ? C8 C12 C11 117.9(6) . . ? C8 C12 H12 121.1 . . ? C11 C12 H12 121.1 . . ? C1 N1 C5 117.1(4) . . ? C1 N1 Cu1 120.2(4) . . ? C5 N1 Cu1 121.8(4) . . ? C6 N2 N3 107.3(4) . . ? C6 N2 Cu1 129.1(3) . 2_665 ? N3 N2 Cu1 118.9(3) . 2_665 ? C7 N3 N2 107.1(4) . . ? C7 N3 Cu1 130.5(3) . 1_565 ? N2 N3 Cu1 122.3(3) . 1_565 ? C7 N4 C6 106.1(4) . . ? C7 N4 N5 129.4(4) . . ? C6 N4 N5 124.4(4) . . ? N4 N5 H5A 120.0 . . ? N4 N5 H5B 120.0 . . ? H5A N5 H5B 120.0 . . ? C10 N6 C11 122.2(5) . . ? Mo2 O2 Mo1 156.4(2) 2_666 . ? Mo2 O4 Mo1 118.05(18) . . ? Mo4 O6 Mo2 112.15(17) . . ? Mo3 O7 Mo2 148.13(18) 2_656 . ? Mo3 O7 Mo4 104.95(14) 2_656 . ? Mo2 O7 Mo4 93.88(12) . . ? Mo3 O7 Mo3 103.95(14) 2_656 . ? Mo2 O7 Mo3 99.31(13) . . ? Mo4 O7 Mo3 95.89(12) . . ? Mo3 O8 Mo1 103.88(14) . . ? Mo3 O8 Mo2 111.59(15) . . ? Mo1 O8 Mo2 93.04(12) . . ? Mo1 O9 Mo4 147.14(18) . 2_656 ? Mo1 O9 Mo3 106.61(15) . . ? Mo4 O9 Mo3 105.07(15) 2_656 . ? Mo3 O11 Mo4 115.10(17) . . ? H1WA O1W H1WB 95.7 . . ? H2WB O2W H2WB 0.0 . . ? H2WB O2W H2WA 124.3 . . ? H2WB O2W H2WA 124.3 . . ? 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 O2W H2WA N5 0.85 2.36 3.193(9) 168.1 2_766 O2W H2WB O12 0.85 2.54 3.034(9) 118.3 . O1W H1WB N5 0.85 2.57 3.004(7) 112.5 1_445 O1W H1WB N4 0.85 2.45 3.153(7) 140.9 1_445 O1W H1WA O2W 0.85 2.62 3.438(11) 161.2 2_656 _diffrn_measured_fraction_theta_max 0.979 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_full 0.979 _refine_diff_density_max 1.355 _refine_diff_density_min -1.236 _refine_diff_density_rms 0.212 # Attachment '2.cif' data_090226a_0m _database_code_depnum_ccdc_archive 'CCDC 762850' #TrackingRef '2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H24 Mo8 N12 O26' _chemical_formula_weight 1664.07 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 P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.6260(7) _cell_length_b 15.8212(10) _cell_length_c 12.8521(8) _cell_angle_alpha 90.00 _cell_angle_beta 100.7030(10) _cell_angle_gamma 90.00 _cell_volume 2123.1(2) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 7104 _cell_measurement_theta_min 2.29 _cell_measurement_theta_max 27.48 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.603 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1592 _exptl_absorpt_coefficient_mu 2.390 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5341 _exptl_absorpt_correction_T_max 0.5864 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10770 _diffrn_reflns_av_R_equivalents 0.0190 _diffrn_reflns_av_sigmaI/netI 0.0213 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.06 _diffrn_reflns_theta_max 25.04 _reflns_number_total 3753 _reflns_number_gt 3434 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^+3.0553P] 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 3753 _refine_ls_number_parameters 316 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0270 _refine_ls_R_factor_gt 0.0240 _refine_ls_wR_factor_ref 0.0608 _refine_ls_wR_factor_gt 0.0592 _refine_ls_goodness_of_fit_ref 1.079 _refine_ls_restrained_S_all 1.079 _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 0.44916(3) 0.105283(19) 1.02223(2) 0.02181(9) Uani 1 1 d . . . Mo2 Mo 0.23722(3) -0.04151(2) 0.99591(2) 0.02365(9) Uani 1 1 d . . . Mo3 Mo 0.37598(3) -0.00838(2) 0.78077(2) 0.02536(9) Uani 1 1 d . . . Mo4 Mo 0.40802(3) -0.13919(2) 1.19383(3) 0.03021(10) Uani 1 1 d . . . C1 C 0.0948(6) 0.0623(3) 0.3090(4) 0.0546(14) Uani 1 1 d . . . H1 H 0.0389 0.0304 0.2601 0.065 Uiso 1 1 calc R . . C2 C 0.0613(5) 0.0848(3) 0.4018(3) 0.0460(11) Uani 1 1 d . . . H2 H -0.0177 0.0686 0.4163 0.055 Uiso 1 1 calc R . . C3 C 0.1453(4) 0.1323(3) 0.4754(3) 0.0339(9) Uani 1 1 d . . . C4 C 0.2607(4) 0.1569(4) 0.4488(4) 0.0558(14) Uani 1 1 d . . . H4 H 0.3181 0.1895 0.4957 0.067 Uiso 1 1 calc R . . C5 C 0.2898(5) 0.1336(4) 0.3544(4) 0.0696(17) Uani 1 1 d . . . H5 H 0.3666 0.1507 0.3361 0.083 Uiso 1 1 calc R . . C6 C 0.1055(4) 0.1516(3) 0.5762(3) 0.0323(9) Uani 1 1 d . . . C7 C 0.0958(4) 0.1910(2) 0.7361(3) 0.0313(9) Uani 1 1 d . . . C8 C 0.1228(4) 0.2243(3) 0.8443(3) 0.0319(9) Uani 1 1 d . . . C9 C 0.2070(4) 0.2892(3) 0.8797(3) 0.0369(9) Uani 1 1 d . . . H9 H 0.2541 0.3146 0.8340 0.044 Uiso 1 1 calc R . . C10 C 0.2203(4) 0.3156(3) 0.9820(4) 0.0475(12) Uani 1 1 d . . . H10 H 0.2767 0.3593 1.0063 0.057 Uiso 1 1 calc R . . C11 C 0.0722(5) 0.2168(4) 1.0176(4) 0.0581(14) Uani 1 1 d . . . H11 H 0.0274 0.1925 1.0656 0.070 Uiso 1 1 calc R . . C12 C 0.0552(5) 0.1883(3) 0.9169(4) 0.0485(11) Uani 1 1 d . . . H12 H -0.0019 0.1443 0.8956 0.058 Uiso 1 1 calc R . . N1 N 0.2072(4) 0.0858(3) 0.2875(3) 0.0548(11) Uani 1 1 d . . . H1A H 0.2277 0.0698 0.2290 0.066 Uiso 1 1 calc R . . N2 N 0.1671(3) 0.19864(19) 0.6581(2) 0.0270(7) Uani 1 1 d . . . N3 N -0.0050(3) 0.1433(2) 0.7020(3) 0.0428(9) Uani 1 1 d . . . N4 N 0.0009(3) 0.1192(2) 0.6006(3) 0.0420(9) Uani 1 1 d . . . N5 N 0.2791(3) 0.2455(2) 0.6573(3) 0.0331(7) Uani 1 1 d . . . H5A H 0.2648 0.3038 0.6557 0.040 Uiso 1 1 d R . . H5B H 0.3374 0.2322 0.7151 0.040 Uiso 1 1 d R . . N6 N 0.1531(4) 0.2794(3) 1.0473(3) 0.0529(11) Uani 1 1 d . . . H6 H 0.1626 0.2974 1.1115 0.063 Uiso 1 1 calc R . . O1 O 0.3707(2) 0.15445(17) 1.1085(2) 0.0330(6) Uani 1 1 d . . . O2 O 0.6216(2) 0.09612(15) 1.10696(19) 0.0243(5) Uani 1 1 d . . . O3 O 0.4836(2) 0.18411(16) 0.9378(2) 0.0305(6) Uani 1 1 d . . . O4 O 0.3065(2) 0.05448(15) 0.92454(18) 0.0232(5) Uani 1 1 d . . . O5 O 0.4185(2) 0.10389(16) 0.7523(2) 0.0315(6) Uani 1 1 d . . . O6 O 0.4646(3) -0.06359(19) 0.7069(2) 0.0392(7) Uani 1 1 d . . . O7 O 0.2227(3) -0.01694(19) 0.7148(2) 0.0384(7) Uani 1 1 d . . . O8 O 0.1164(2) -0.07503(18) 0.9001(2) 0.0365(6) Uani 1 1 d . . . O9 O 0.1677(3) 0.01611(19) 1.0820(2) 0.0370(7) Uani 1 1 d . . . O10 O 0.2745(2) -0.14412(16) 1.0728(2) 0.0314(6) Uani 1 1 d . . . O11 O 0.4444(2) -0.02143(15) 1.08620(19) 0.0229(5) Uani 1 1 d . . . O12 O 0.3330(3) -0.0839(2) 1.2775(2) 0.0424(7) Uani 1 1 d . . . O13 O 0.4150(3) -0.23921(18) 1.2438(2) 0.0437(7) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mo1 0.01947(16) 0.01595(16) 0.02974(17) -0.00175(12) 0.00389(12) 0.00250(12) Mo2 0.01797(16) 0.02453(18) 0.02885(18) -0.00076(13) 0.00538(12) -0.00032(12) Mo3 0.02418(17) 0.02481(18) 0.02638(17) 0.00026(13) 0.00283(13) -0.00008(13) Mo4 0.03085(19) 0.0280(2) 0.03199(19) 0.00794(14) 0.00635(14) -0.00266(14) C1 0.086(4) 0.034(3) 0.036(3) -0.001(2) -0.009(2) -0.006(3) C2 0.058(3) 0.041(3) 0.036(2) 0.001(2) -0.002(2) -0.011(2) C3 0.036(2) 0.028(2) 0.035(2) -0.0010(17) -0.0029(17) 0.0097(17) C4 0.037(3) 0.074(4) 0.057(3) -0.029(3) 0.008(2) 0.003(2) C5 0.047(3) 0.101(5) 0.064(3) -0.033(3) 0.018(3) 0.014(3) C6 0.031(2) 0.029(2) 0.034(2) 0.0012(17) -0.0028(16) 0.0019(17) C7 0.031(2) 0.028(2) 0.035(2) 0.0023(17) 0.0061(16) 0.0010(17) C8 0.032(2) 0.033(2) 0.031(2) 0.0068(17) 0.0060(16) 0.0111(17) C9 0.039(2) 0.039(2) 0.032(2) 0.0031(18) 0.0033(17) -0.0006(19) C10 0.038(2) 0.053(3) 0.048(3) -0.010(2) -0.002(2) 0.005(2) C11 0.060(3) 0.077(4) 0.044(3) 0.008(3) 0.025(2) 0.005(3) C12 0.052(3) 0.050(3) 0.048(3) 0.000(2) 0.023(2) -0.006(2) N1 0.073(3) 0.049(3) 0.041(2) -0.0150(19) 0.007(2) 0.022(2) N2 0.0244(16) 0.0241(17) 0.0317(17) 0.0018(14) 0.0031(13) -0.0002(13) N3 0.037(2) 0.045(2) 0.047(2) -0.0029(18) 0.0095(16) -0.0100(17) N4 0.036(2) 0.045(2) 0.043(2) -0.0021(17) 0.0039(16) -0.0089(17) N5 0.0282(17) 0.0284(18) 0.0404(19) 0.0047(15) 0.0004(14) -0.0020(14) N6 0.047(2) 0.081(3) 0.0313(19) -0.004(2) 0.0094(17) 0.018(2) O1 0.0308(14) 0.0292(15) 0.0395(15) -0.0075(12) 0.0077(11) 0.0068(12) O2 0.0218(12) 0.0201(13) 0.0308(13) -0.0019(10) 0.0046(10) -0.0011(10) O3 0.0312(14) 0.0209(14) 0.0390(15) 0.0025(11) 0.0056(11) 0.0022(11) O4 0.0194(12) 0.0209(13) 0.0282(13) 0.0009(10) 0.0017(10) 0.0033(10) O5 0.0305(14) 0.0288(15) 0.0332(14) 0.0068(12) 0.0004(11) 0.0003(11) O6 0.0373(16) 0.0415(17) 0.0410(16) -0.0057(14) 0.0130(13) 0.0026(13) O7 0.0294(15) 0.0451(18) 0.0380(16) -0.0008(13) -0.0006(12) -0.0024(13) O8 0.0248(14) 0.0424(17) 0.0402(15) -0.0010(13) 0.0007(11) -0.0057(12) O9 0.0305(15) 0.0439(18) 0.0393(15) -0.0054(13) 0.0137(12) 0.0039(13) O10 0.0281(14) 0.0283(15) 0.0380(15) 0.0049(12) 0.0068(11) -0.0064(11) O11 0.0213(12) 0.0197(13) 0.0281(13) 0.0000(10) 0.0053(10) 0.0006(10) O12 0.0409(16) 0.0485(19) 0.0402(16) 0.0037(14) 0.0139(13) -0.0005(14) O13 0.0548(19) 0.0320(16) 0.0424(16) 0.0105(14) 0.0041(14) -0.0067(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mo1 O1 1.695(3) . ? Mo1 O3 1.736(3) . ? Mo1 O4 1.953(2) . ? Mo1 O2 1.956(2) . ? Mo1 O11 2.171(2) . ? Mo1 O11 2.359(2) 3_657 ? Mo2 O8 1.691(3) . ? Mo2 O9 1.705(3) . ? Mo2 O10 1.904(3) . ? Mo2 O4 1.985(2) . ? Mo2 O11 2.312(2) . ? Mo2 O2 2.341(2) 3_657 ? Mo3 O7 1.696(3) . ? Mo3 O6 1.698(3) . ? Mo3 O5 1.885(3) . ? Mo3 O2 1.999(2) 3_657 ? Mo3 O4 2.336(2) . ? Mo3 O11 2.361(2) 3_657 ? Mo4 O12 1.696(3) . ? Mo4 O13 1.704(3) . ? Mo4 O10 1.902(3) . ? Mo4 O5 1.927(3) 3_657 ? Mo4 O3 2.327(3) 3_657 ? Mo4 O11 2.394(2) . ? C1 N1 1.327(7) . ? C1 C2 1.354(7) . ? C1 H1 0.9300 . ? C2 C3 1.394(6) . ? C2 H2 0.9300 . ? C3 C4 1.389(6) . ? C3 C6 1.468(6) . ? C4 C5 1.358(7) . ? C4 H4 0.9300 . ? C5 N1 1.342(7) . ? C5 H5 0.9300 . ? C6 N4 1.314(5) . ? C6 N2 1.354(5) . ? C7 N3 1.318(5) . ? C7 N2 1.369(5) . ? C7 C8 1.465(5) . ? C8 C9 1.382(6) . ? C8 C12 1.400(6) . ? C9 C10 1.362(6) . ? C9 H9 0.9300 . ? C10 N6 1.329(6) . ? C10 H10 0.9300 . ? C11 N6 1.320(7) . ? C11 C12 1.351(7) . ? C11 H11 0.9300 . ? C12 H12 0.9300 . ? N1 H1A 0.8600 . ? N2 N5 1.404(4) . ? N3 N4 1.370(5) . ? N5 H5A 0.9348 . ? N5 H5B 0.8994 . ? N6 H6 0.8600 . ? O2 Mo3 1.999(2) 3_657 ? O2 Mo2 2.341(2) 3_657 ? O3 Mo4 2.327(3) 3_657 ? O5 Mo4 1.927(3) 3_657 ? O11 Mo1 2.359(2) 3_657 ? O11 Mo3 2.361(2) 3_657 ? 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 O1 Mo1 O3 105.40(13) . . ? O1 Mo1 O4 101.07(11) . . ? O3 Mo1 O4 97.02(11) . . ? O1 Mo1 O2 101.16(11) . . ? O3 Mo1 O2 96.72(11) . . ? O4 Mo1 O2 149.64(10) . . ? O1 Mo1 O11 97.31(12) . . ? O3 Mo1 O11 157.29(11) . . ? O4 Mo1 O11 78.08(9) . . ? O2 Mo1 O11 78.81(9) . . ? O1 Mo1 O11 172.93(11) . 3_657 ? O3 Mo1 O11 81.66(10) . 3_657 ? O4 Mo1 O11 77.82(9) . 3_657 ? O2 Mo1 O11 77.57(9) . 3_657 ? O11 Mo1 O11 75.63(10) . 3_657 ? O8 Mo2 O9 106.17(13) . . ? O8 Mo2 O10 99.64(13) . . ? O9 Mo2 O10 101.10(13) . . ? O8 Mo2 O4 101.53(12) . . ? O9 Mo2 O4 97.67(12) . . ? O10 Mo2 O4 146.42(10) . . ? O8 Mo2 O11 158.76(11) . . ? O9 Mo2 O11 95.05(11) . . ? O10 Mo2 O11 76.67(10) . . ? O4 Mo2 O11 74.14(9) . . ? O8 Mo2 O2 87.27(11) . 3_657 ? O9 Mo2 O2 164.69(11) . 3_657 ? O10 Mo2 O2 83.40(10) . 3_657 ? O4 Mo2 O2 71.94(9) . 3_657 ? O11 Mo2 O2 71.57(8) . 3_657 ? O7 Mo3 O6 105.06(14) . . ? O7 Mo3 O5 102.76(13) . . ? O6 Mo3 O5 101.44(13) . . ? O7 Mo3 O2 100.83(12) . 3_657 ? O6 Mo3 O2 96.46(12) . 3_657 ? O5 Mo3 O2 145.36(11) . 3_657 ? O7 Mo3 O4 90.82(11) . . ? O6 Mo3 O4 162.01(11) . . ? O5 Mo3 O4 82.80(10) . . ? O2 Mo3 O4 71.83(9) 3_657 . ? O7 Mo3 O11 161.78(12) . 3_657 ? O6 Mo3 O11 92.88(11) . 3_657 ? O5 Mo3 O11 76.20(10) . 3_657 ? O2 Mo3 O11 73.49(9) 3_657 3_657 ? O4 Mo3 O11 70.97(8) . 3_657 ? O12 Mo4 O13 103.42(15) . . ? O12 Mo4 O10 99.95(13) . . ? O13 Mo4 O10 104.10(13) . . ? O12 Mo4 O5 98.84(13) . 3_657 ? O13 Mo4 O5 99.32(13) . 3_657 ? O10 Mo4 O5 145.47(11) . 3_657 ? O12 Mo4 O3 166.65(12) . 3_657 ? O13 Mo4 O3 89.86(12) . 3_657 ? O10 Mo4 O3 77.76(10) . 3_657 ? O5 Mo4 O3 77.29(10) 3_657 3_657 ? O12 Mo4 O11 96.37(12) . . ? O13 Mo4 O11 160.03(12) . . ? O10 Mo4 O11 74.66(9) . . ? O5 Mo4 O11 74.67(9) 3_657 . ? O3 Mo4 O11 70.30(9) 3_657 . ? N1 C1 C2 120.2(4) . . ? N1 C1 H1 119.9 . . ? C2 C1 H1 119.9 . . ? C1 C2 C3 120.0(5) . . ? C1 C2 H2 120.0 . . ? C3 C2 H2 120.0 . . ? C4 C3 C2 117.9(4) . . ? C4 C3 C6 124.8(4) . . ? C2 C3 C6 117.3(4) . . ? C5 C4 C3 120.1(5) . . ? C5 C4 H4 119.9 . . ? C3 C4 H4 119.9 . . ? N1 C5 C4 119.6(5) . . ? N1 C5 H5 120.2 . . ? C4 C5 H5 120.2 . . ? N4 C6 N2 109.7(4) . . ? N4 C6 C3 121.6(4) . . ? N2 C6 C3 128.6(4) . . ? N3 C7 N2 109.4(3) . . ? N3 C7 C8 121.7(4) . . ? N2 C7 C8 128.8(4) . . ? C9 C8 C12 117.7(4) . . ? C9 C8 C7 125.4(4) . . ? C12 C8 C7 116.9(4) . . ? C10 C9 C8 119.3(4) . . ? C10 C9 H9 120.3 . . ? C8 C9 H9 120.3 . . ? N6 C10 C9 120.4(5) . . ? N6 C10 H10 119.8 . . ? C9 C10 H10 119.8 . . ? N6 C11 C12 119.5(5) . . ? N6 C11 H11 120.3 . . ? C12 C11 H11 120.3 . . ? C11 C12 C8 120.6(5) . . ? C11 C12 H12 119.7 . . ? C8 C12 H12 119.7 . . ? C1 N1 C5 122.1(4) . . ? C1 N1 H1A 118.9 . . ? C5 N1 H1A 118.9 . . ? C6 N2 C7 105.5(3) . . ? C6 N2 N5 124.9(3) . . ? C7 N2 N5 129.5(3) . . ? C7 N3 N4 107.3(3) . . ? C6 N4 N3 107.9(3) . . ? N2 N5 H5A 112.7 . . ? N2 N5 H5B 109.0 . . ? H5A N5 H5B 109.4 . . ? C11 N6 C10 122.6(4) . . ? C11 N6 H6 118.7 . . ? C10 N6 H6 118.7 . . ? Mo1 O2 Mo3 109.78(11) . 3_657 ? Mo1 O2 Mo2 110.20(11) . 3_657 ? Mo3 O2 Mo2 103.17(10) 3_657 3_657 ? Mo1 O3 Mo4 115.15(12) . 3_657 ? Mo1 O4 Mo2 109.15(11) . . ? Mo1 O4 Mo3 111.22(10) . . ? Mo2 O4 Mo3 103.81(10) . . ? Mo3 O5 Mo4 116.83(13) . 3_657 ? Mo4 O10 Mo2 116.19(13) . . ? Mo1 O11 Mo2 91.36(8) . . ? Mo1 O11 Mo1 104.37(10) . 3_657 ? Mo2 O11 Mo1 98.19(9) . 3_657 ? Mo1 O11 Mo3 90.99(8) . 3_657 ? Mo2 O11 Mo3 163.15(12) . 3_657 ? Mo1 O11 Mo3 97.38(8) 3_657 3_657 ? Mo1 O11 Mo4 162.74(12) . . ? Mo2 O11 Mo4 86.68(8) . . ? Mo1 O11 Mo4 92.88(8) 3_657 . ? Mo3 O11 Mo4 86.14(8) 3_657 . ? 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 N5 H5B O13 0.90 2.59 3.264(4) 132.6 3_657 N5 H5B O5 0.90 2.22 2.834(4) 124.8 . N5 H5A O8 0.93 2.47 3.185(4) 133.0 2_556 N5 H5A O2 0.93 2.20 3.016(4) 144.7 4_565 N6 H6 O12 0.86 2.35 3.105(5) 146.2 2_557 N6 H6 O13 0.86 2.25 2.922(5) 135.4 2_557 N1 H1A O9 0.86 2.06 2.821(5) 146.9 1_554 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.04 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.951 _refine_diff_density_min -0.573 _refine_diff_density_rms 0.114 # Attachment '3.cif' data_090615d_0m _database_code_depnum_ccdc_archive 'CCDC 762851' #TrackingRef '3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H12 Cu Mo4 N6 O14' _chemical_formula_weight 911.58 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' Cu Cu 0.3201 1.2651 '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 P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 7.6630(4) _cell_length_b 29.4740(17) _cell_length_c 9.7421(6) _cell_angle_alpha 90.00 _cell_angle_beta 101.8230(10) _cell_angle_gamma 90.00 _cell_volume 2153.7(2) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 8085 _cell_measurement_theta_min 2.24 _cell_measurement_theta_max 27.53 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.811 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1740 _exptl_absorpt_coefficient_mu 3.324 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4354 _exptl_absorpt_correction_T_max 0.4904 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11121 _diffrn_reflns_av_R_equivalents 0.0177 _diffrn_reflns_av_sigmaI/netI 0.0198 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -35 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 2.24 _diffrn_reflns_theta_max 25.05 _reflns_number_total 3804 _reflns_number_gt 3584 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0193P)^2^+3.8697P] 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 3804 _refine_ls_number_parameters 335 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0231 _refine_ls_R_factor_gt 0.0210 _refine_ls_wR_factor_ref 0.0490 _refine_ls_wR_factor_gt 0.0482 _refine_ls_goodness_of_fit_ref 1.099 _refine_ls_restrained_S_all 1.099 _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 0.27613(3) 0.480966(9) 0.97780(3) 0.01271(7) Uani 1 1 d . . . Mo2 Mo 0.52750(4) 0.529501(9) 1.28412(3) 0.01423(8) Uani 1 1 d . . . Mo3 Mo 0.34984(4) 0.588772(9) 0.99102(3) 0.01386(8) Uani 1 1 d . . . Mo4 Mo 0.45414(4) 0.420210(10) 1.27169(3) 0.01494(8) Uani 1 1 d . . . Cu1 Cu 0.02924(6) 0.605421(14) 0.67129(4) 0.01940(10) Uani 1 1 d . . . C1 C -0.0414(5) 0.68531(13) 0.8270(4) 0.0306(9) Uani 1 1 d . . . H1 H -0.1373 0.6685 0.8441 0.037 Uiso 1 1 calc R . . C2 C -0.0030(6) 0.72617(14) 0.8928(5) 0.0383(10) Uani 1 1 d . . . H2 H -0.0731 0.7372 0.9529 0.046 Uiso 1 1 calc R . . C3 C 0.1409(6) 0.75085(14) 0.8690(5) 0.0372(10) Uani 1 1 d . . . H3 H 0.1684 0.7786 0.9135 0.045 Uiso 1 1 calc R . . C4 C 0.2441(5) 0.73440(12) 0.7793(4) 0.0256(8) Uani 1 1 d . . . C5 C 0.1943(5) 0.69243(12) 0.7158(4) 0.0250(8) Uani 1 1 d . . . H5 H 0.2616 0.6805 0.6549 0.030 Uiso 1 1 calc R . . C6 C 0.4036(5) 0.75573(13) 0.7484(4) 0.0280(9) Uani 1 1 d . . . C7 C 0.6332(5) 0.79909(12) 0.7501(4) 0.0240(8) Uani 1 1 d . . . C8 C 0.7705(5) 0.83432(12) 0.7889(4) 0.0207(7) Uani 1 1 d . . . C9 C 0.8322(4) 0.84551(11) 0.9285(4) 0.0193(7) Uani 1 1 d . . . H9 H 0.7841 0.8307 0.9965 0.023 Uiso 1 1 calc R . . C10 C 1.0306(5) 0.89731(12) 0.8713(4) 0.0228(8) Uani 1 1 d . . . H10 H 1.1180 0.9192 0.8992 0.027 Uiso 1 1 calc R . . C11 C 0.9797(5) 0.88708(13) 0.7303(4) 0.0250(8) Uani 1 1 d . . . H11 H 1.0345 0.9012 0.6649 0.030 Uiso 1 1 calc R . . C12 C 0.8461(5) 0.85558(13) 0.6884(4) 0.0260(8) Uani 1 1 d . . . H12 H 0.8074 0.8487 0.5939 0.031 Uiso 1 1 calc R . . N1 N 0.0559(4) 0.66902(10) 0.7385(3) 0.0236(7) Uani 1 1 d . . . N2 N 0.4938(5) 0.73907(12) 0.6580(4) 0.0372(9) Uani 1 1 d . . . N3 N 0.6397(5) 0.76658(12) 0.6586(4) 0.0350(8) Uani 1 1 d . . . N4 N 0.4882(4) 0.79378(10) 0.8089(3) 0.0216(6) Uani 1 1 d . . . N5 N 0.4212(4) 0.82362(10) 0.8985(3) 0.0256(7) Uani 1 1 d . . . H5A H 0.4741 0.8490 0.9224 0.031 Uiso 1 1 calc R . . H5B H 0.3274 0.8165 0.9293 0.031 Uiso 1 1 calc R . . N6 N 0.9587(4) 0.87681(9) 0.9690(3) 0.0193(6) Uani 1 1 d . . . O1 O 0.0848(3) 0.48882(8) 0.8579(2) 0.0190(5) Uani 1 1 d . . . O2 O 0.3981(3) 0.43786(7) 0.8748(2) 0.0143(5) Uani 1 1 d . . . O3 O 0.4419(3) 0.52517(7) 0.8789(2) 0.0140(5) Uani 1 1 d . . . O4 O 0.1522(3) 0.59022(8) 0.8651(2) 0.0196(5) Uani 1 1 d . . . O5 O 0.5070(3) 0.61445(7) 0.8890(2) 0.0167(5) Uani 1 1 d . . . O6 O 0.3327(3) 0.63074(8) 1.1052(3) 0.0241(6) Uani 1 1 d . . . O7 O 0.2841(3) 0.53480(7) 1.0922(2) 0.0144(5) Uani 1 1 d . . . O8 O 0.4354(3) 0.57359(8) 1.3551(2) 0.0246(6) Uani 1 1 d . . . O9 O 0.7344(3) 0.52323(8) 1.3857(3) 0.0245(6) Uani 1 1 d . . . O10 O 0.4052(3) 0.47856(8) 1.3384(2) 0.0186(5) Uani 1 1 d . . . O11 O 0.6606(3) 0.40890(8) 1.3700(3) 0.0243(6) Uani 1 1 d . . . O12 O 0.3102(3) 0.38583(8) 1.3360(3) 0.0244(6) Uani 1 1 d . . . O13 O 0.2242(3) 0.44163(8) 1.0966(2) 0.0187(5) Uani 1 1 d . . . O14 O -0.0224(3) 0.54267(8) 0.6255(3) 0.0234(5) Uani 1 1 d . . . H14A H -0.1138 0.5409 0.5649 0.035 Uiso 1 1 calc R . . H14B H 0.0100 0.5208 0.6948 0.035 Uiso 1 1 d 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 0.01068(13) 0.01422(15) 0.01275(15) -0.00044(11) 0.00129(11) -0.00076(10) Mo2 0.01676(15) 0.01508(15) 0.01041(15) -0.00143(11) 0.00174(11) -0.00071(11) Mo3 0.01461(14) 0.01382(15) 0.01273(15) -0.00025(11) 0.00181(11) 0.00119(11) Mo4 0.01575(15) 0.01594(15) 0.01307(15) 0.00143(11) 0.00276(11) -0.00115(11) Cu1 0.0243(2) 0.0140(2) 0.0167(2) 0.00084(16) -0.00314(17) -0.00221(17) C1 0.029(2) 0.027(2) 0.035(2) -0.0035(17) 0.0053(18) -0.0046(16) C2 0.037(2) 0.034(2) 0.046(3) -0.018(2) 0.013(2) -0.0041(19) C3 0.040(2) 0.024(2) 0.047(3) -0.0149(19) 0.009(2) -0.0074(18) C4 0.029(2) 0.0195(18) 0.025(2) -0.0029(15) -0.0031(16) -0.0026(15) C5 0.031(2) 0.0187(18) 0.024(2) 0.0002(15) 0.0015(16) 0.0007(15) C6 0.033(2) 0.024(2) 0.025(2) -0.0054(16) 0.0006(17) -0.0046(16) C7 0.031(2) 0.0229(19) 0.0178(18) -0.0036(15) 0.0032(15) -0.0052(16) C8 0.0221(18) 0.0187(18) 0.0206(19) -0.0020(14) 0.0026(15) 0.0023(14) C9 0.0221(18) 0.0163(17) 0.0201(18) -0.0025(14) 0.0053(15) 0.0018(14) C10 0.0194(17) 0.0205(18) 0.027(2) 0.0006(15) 0.0013(15) -0.0003(14) C11 0.0223(18) 0.028(2) 0.027(2) 0.0052(16) 0.0108(16) 0.0028(15) C12 0.031(2) 0.030(2) 0.0168(18) -0.0033(16) 0.0041(16) 0.0033(16) N1 0.0289(16) 0.0166(15) 0.0220(16) 0.0013(12) -0.0024(13) -0.0029(13) N2 0.040(2) 0.0329(19) 0.040(2) -0.0193(16) 0.0092(17) -0.0152(16) N3 0.037(2) 0.037(2) 0.0311(19) -0.0158(15) 0.0080(16) -0.0135(15) N4 0.0270(16) 0.0178(15) 0.0187(15) -0.0033(12) 0.0017(13) -0.0031(12) N5 0.0309(17) 0.0171(15) 0.0312(18) -0.0074(13) 0.0119(14) -0.0056(13) N6 0.0202(15) 0.0160(14) 0.0211(15) -0.0016(12) 0.0028(12) 0.0002(12) O1 0.0143(11) 0.0220(13) 0.0193(13) 0.0003(10) 0.0001(10) 0.0001(10) O2 0.0150(11) 0.0152(11) 0.0123(11) -0.0015(9) 0.0020(9) -0.0015(9) O3 0.0143(11) 0.0163(12) 0.0109(11) -0.0013(9) 0.0011(9) 0.0007(9) O4 0.0184(12) 0.0211(13) 0.0180(12) 0.0032(10) 0.0008(10) 0.0005(10) O5 0.0184(11) 0.0153(12) 0.0162(12) 0.0009(9) 0.0031(9) -0.0015(9) O6 0.0293(14) 0.0210(13) 0.0219(13) -0.0047(10) 0.0048(11) 0.0002(11) O7 0.0138(11) 0.0173(12) 0.0124(11) 0.0001(9) 0.0032(9) 0.0004(9) O8 0.0332(14) 0.0211(13) 0.0203(13) -0.0026(10) 0.0074(11) 0.0045(11) O9 0.0242(13) 0.0286(14) 0.0180(13) 0.0001(10) -0.0020(11) -0.0020(11) O10 0.0212(12) 0.0209(12) 0.0149(12) -0.0009(10) 0.0068(10) -0.0007(10) O11 0.0222(13) 0.0311(14) 0.0175(13) -0.0005(11) -0.0009(10) 0.0022(11) O12 0.0278(13) 0.0229(13) 0.0240(14) 0.0027(11) 0.0088(11) -0.0049(11) O13 0.0176(12) 0.0194(12) 0.0193(12) 0.0021(10) 0.0045(10) -0.0012(10) O14 0.0250(13) 0.0172(12) 0.0219(13) 0.0024(10) -0.0094(10) 0.0005(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 O1 1.693(2) . ? Mo1 O13 1.741(2) . ? Mo1 O7 1.932(2) . ? Mo1 O2 1.969(2) . ? Mo1 O3 2.177(2) . ? Mo1 O3 2.327(2) 3_667 ? Mo2 O8 1.693(2) . ? Mo2 O9 1.698(2) . ? Mo2 O10 1.901(2) . ? Mo2 O2 2.002(2) 3_667 ? Mo2 O3 2.308(2) 3_667 ? Mo2 O7 2.360(2) . ? Mo3 O6 1.687(2) . ? Mo3 O4 1.743(2) . ? Mo3 O5 1.871(2) . ? Mo3 O7 1.990(2) . ? Mo3 O2 2.241(2) 3_667 ? Mo3 O3 2.350(2) . ? Mo4 O11 1.706(2) . ? Mo4 O12 1.708(2) . ? Mo4 O10 1.903(2) . ? Mo4 O5 1.943(2) 3_667 ? Mo4 O13 2.277(2) . ? Mo4 O3 2.420(2) 3_667 ? Cu1 O14 1.924(2) . ? Cu1 O4 1.981(2) . ? Cu1 N1 1.982(3) . ? Cu1 N6 2.004(3) 4_475 ? C1 N1 1.339(5) . ? C1 C2 1.367(5) . ? C1 H1 0.9300 . ? C2 C3 1.380(6) . ? C2 H2 0.9300 . ? C3 C4 1.381(6) . ? C3 H3 0.9300 . ? C4 C5 1.401(5) . ? C4 C6 1.460(5) . ? C5 N1 1.322(5) . ? C5 H5 0.9300 . ? C6 N2 1.320(5) . ? C6 N4 1.367(5) . ? C7 N3 1.317(5) . ? C7 N4 1.359(5) . ? C7 C8 1.471(5) . ? C8 C12 1.385(5) . ? C8 C9 1.386(5) . ? C9 N6 1.338(4) . ? C9 H9 0.9300 . ? C10 N6 1.338(5) . ? C10 C11 1.381(5) . ? C10 H10 0.9300 . ? C11 C12 1.380(5) . ? C11 H11 0.9300 . ? C12 H12 0.9300 . ? N2 N3 1.380(5) . ? N4 N5 1.408(4) . ? N5 H5A 0.8600 . ? N5 H5B 0.8600 . ? N6 Cu1 2.004(3) 4_676 ? O2 Mo2 2.002(2) 3_667 ? O2 Mo3 2.241(2) 3_667 ? O3 Mo2 2.308(2) 3_667 ? O3 Mo1 2.327(2) 3_667 ? O3 Mo4 2.420(2) 3_667 ? O5 Mo4 1.943(2) 3_667 ? O14 H14A 0.8200 . ? O14 H14B 0.9304 . ? 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 O1 Mo1 O13 105.43(11) . . ? O1 Mo1 O7 101.89(10) . . ? O13 Mo1 O7 98.51(10) . . ? O1 Mo1 O2 99.85(10) . . ? O13 Mo1 O2 96.10(10) . . ? O7 Mo1 O2 149.44(9) . . ? O1 Mo1 O3 96.55(10) . . ? O13 Mo1 O3 157.86(9) . . ? O7 Mo1 O3 79.13(9) . . ? O2 Mo1 O3 77.28(9) . . ? O1 Mo1 O3 172.35(10) . 3_667 ? O13 Mo1 O3 81.96(9) . 3_667 ? O7 Mo1 O3 78.59(8) . 3_667 ? O2 Mo1 O3 77.06(8) . 3_667 ? O3 Mo1 O3 75.98(9) . 3_667 ? O8 Mo2 O9 105.25(12) . . ? O8 Mo2 O10 102.83(11) . . ? O9 Mo2 O10 101.92(11) . . ? O8 Mo2 O2 98.96(11) . 3_667 ? O9 Mo2 O2 97.07(11) . 3_667 ? O10 Mo2 O2 146.00(9) . 3_667 ? O8 Mo2 O3 157.96(10) . 3_667 ? O9 Mo2 O3 96.35(10) . 3_667 ? O10 Mo2 O3 76.43(9) . 3_667 ? O2 Mo2 O3 73.63(8) 3_667 3_667 ? O8 Mo2 O7 86.85(10) . . ? O9 Mo2 O7 163.88(10) . . ? O10 Mo2 O7 85.30(9) . . ? O2 Mo2 O7 70.10(8) 3_667 . ? O3 Mo2 O7 71.11(7) 3_667 . ? O6 Mo3 O4 105.80(11) . . ? O6 Mo3 O5 101.49(11) . . ? O4 Mo3 O5 100.19(10) . . ? O6 Mo3 O7 101.43(11) . . ? O4 Mo3 O7 95.53(10) . . ? O5 Mo3 O7 147.38(9) . . ? O6 Mo3 O2 92.67(10) . 3_667 ? O4 Mo3 O2 160.02(9) . 3_667 ? O5 Mo3 O2 83.11(9) . 3_667 ? O7 Mo3 O2 72.94(8) . 3_667 ? O6 Mo3 O3 164.40(10) . . ? O4 Mo3 O3 89.58(9) . . ? O5 Mo3 O3 77.79(9) . . ? O7 Mo3 O3 73.91(8) . . ? O2 Mo3 O3 71.74(8) 3_667 . ? O11 Mo4 O12 105.80(12) . . ? O11 Mo4 O10 102.11(11) . . ? O12 Mo4 O10 102.93(11) . . ? O11 Mo4 O5 94.12(11) . 3_667 ? O12 Mo4 O5 101.57(11) . 3_667 ? O10 Mo4 O5 145.49(9) . 3_667 ? O11 Mo4 O13 164.03(11) . . ? O12 Mo4 O13 88.87(10) . . ? O10 Mo4 O13 80.14(9) . . ? O5 Mo4 O13 76.42(9) 3_667 . ? O11 Mo4 O3 95.04(10) . 3_667 ? O12 Mo4 O3 159.09(10) . 3_667 ? O10 Mo4 O3 73.63(9) . 3_667 ? O5 Mo4 O3 74.78(8) 3_667 3_667 ? O13 Mo4 O3 70.23(8) . 3_667 ? O14 Cu1 O4 92.21(10) . . ? O14 Cu1 N1 171.00(12) . . ? O4 Cu1 N1 84.39(11) . . ? O14 Cu1 N6 91.25(11) . 4_475 ? O4 Cu1 N6 167.52(11) . 4_475 ? N1 Cu1 N6 93.83(12) . 4_475 ? N1 C1 C2 121.5(4) . . ? N1 C1 H1 119.2 . . ? C2 C1 H1 119.2 . . ? C1 C2 C3 119.2(4) . . ? C1 C2 H2 120.4 . . ? C3 C2 H2 120.4 . . ? C2 C3 C4 120.2(4) . . ? C2 C3 H3 119.9 . . ? C4 C3 H3 119.9 . . ? C3 C4 C5 116.8(4) . . ? C3 C4 C6 126.3(3) . . ? C5 C4 C6 116.9(3) . . ? N1 C5 C4 122.8(4) . . ? N1 C5 H5 118.6 . . ? C4 C5 H5 118.6 . . ? N2 C6 N4 109.1(3) . . ? N2 C6 C4 123.5(3) . . ? N4 C6 C4 127.4(3) . . ? N3 C7 N4 110.4(3) . . ? N3 C7 C8 124.3(3) . . ? N4 C7 C8 125.2(3) . . ? C12 C8 C9 118.5(3) . . ? C12 C8 C7 121.3(3) . . ? C9 C8 C7 120.1(3) . . ? N6 C9 C8 122.3(3) . . ? N6 C9 H9 118.9 . . ? C8 C9 H9 118.9 . . ? N6 C10 C11 122.4(3) . . ? N6 C10 H10 118.8 . . ? C11 C10 H10 118.8 . . ? C12 C11 C10 118.8(3) . . ? C12 C11 H11 120.6 . . ? C10 C11 H11 120.6 . . ? C11 C12 C8 119.2(3) . . ? C11 C12 H12 120.4 . . ? C8 C12 H12 120.4 . . ? C5 N1 C1 119.5(3) . . ? C5 N1 Cu1 118.0(3) . . ? C1 N1 Cu1 121.2(3) . . ? C6 N2 N3 108.2(3) . . ? C7 N3 N2 106.7(3) . . ? C7 N4 C6 105.6(3) . . ? C7 N4 N5 128.5(3) . . ? C6 N4 N5 125.4(3) . . ? N4 N5 H5A 120.0 . . ? N4 N5 H5B 120.0 . . ? H5A N5 H5B 120.0 . . ? C10 N6 C9 118.8(3) . . ? C10 N6 Cu1 121.0(2) . 4_676 ? C9 N6 Cu1 120.2(2) . 4_676 ? Mo1 O2 Mo2 108.91(10) . 3_667 ? Mo1 O2 Mo3 111.79(10) . 3_667 ? Mo2 O2 Mo3 105.75(9) 3_667 3_667 ? Mo1 O3 Mo2 92.14(8) . 3_667 ? Mo1 O3 Mo1 104.02(9) . 3_667 ? Mo2 O3 Mo1 98.38(8) 3_667 3_667 ? Mo1 O3 Mo3 90.79(8) . . ? Mo2 O3 Mo3 163.64(10) 3_667 . ? Mo1 O3 Mo3 96.52(8) 3_667 . ? Mo1 O3 Mo4 163.86(10) . 3_667 ? Mo2 O3 Mo4 87.41(7) 3_667 3_667 ? Mo1 O3 Mo4 92.00(7) 3_667 3_667 ? Mo3 O3 Mo4 85.34(7) . 3_667 ? Mo3 O4 Cu1 148.35(14) . . ? Mo3 O5 Mo4 115.91(11) . 3_667 ? Mo1 O7 Mo3 110.63(10) . . ? Mo1 O7 Mo2 109.21(9) . . ? Mo3 O7 Mo2 101.89(9) . . ? Mo2 O10 Mo4 118.43(12) . . ? Mo1 O13 Mo4 115.81(11) . . ? Cu1 O14 H14A 109.5 . . ? Cu1 O14 H14B 119.1 . . ? H14A O14 H14B 122.6 . . ? 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 O14 H14B O1 0.93 1.83 2.749(3) 166.9 . N5 H5A O8 0.86 2.38 3.064(4) 137.4 4_575 O14 H14A O9 0.82 1.96 2.734(3) 157.2 1_454 _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.681 _refine_diff_density_min -0.739 _refine_diff_density_rms 0.103 # Attachment '4.cif' data_08102103 _database_code_depnum_ccdc_archive 'CCDC 762852' #TrackingRef '4.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H12 Cu Mo N6 O5' _chemical_formula_weight 479.76 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' Cu Cu 0.3201 1.2651 '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 P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.9052(6) _cell_length_b 17.6030(10) _cell_length_c 7.8921(4) _cell_angle_alpha 90.00 _cell_angle_beta 92.640(2) _cell_angle_gamma 90.00 _cell_volume 1513.39(14) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 1138 _cell_measurement_theta_min 2.31 _cell_measurement_theta_max 21.77 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.106 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 948 _exptl_absorpt_coefficient_mu 2.275 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6590 _exptl_absorpt_correction_T_max 0.8045 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8029 _diffrn_reflns_av_R_equivalents 0.0640 _diffrn_reflns_av_sigmaI/netI 0.0740 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 2.20 _diffrn_reflns_theta_max 25.05 _reflns_number_total 2670 _reflns_number_gt 1917 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0418P)^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 2670 _refine_ls_number_parameters 234 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0713 _refine_ls_R_factor_gt 0.0448 _refine_ls_wR_factor_ref 0.1045 _refine_ls_wR_factor_gt 0.0912 _refine_ls_goodness_of_fit_ref 1.054 _refine_ls_restrained_S_all 1.054 _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 Cu1 Cu 0.71301(7) 0.37561(4) 0.96547(9) 0.0233(2) Uani 1 1 d . . . Mo1 Mo 0.80160(5) 0.17520(3) 1.06520(6) 0.02375(18) Uani 1 1 d . . . C1 C -0.1471(6) 0.0106(3) 0.6689(8) 0.0283(15) Uani 1 1 d . . . H1 H -0.2205 -0.0163 0.6595 0.034 Uiso 1 1 calc R . . C2 C -0.0474(6) -0.0215(3) 0.7585(8) 0.0334(16) Uani 1 1 d . . . H2 H -0.0537 -0.0691 0.8089 0.040 Uiso 1 1 calc R . . C3 C 0.0618(6) 0.0188(3) 0.7712(8) 0.0326(16) Uani 1 1 d . . . H3 H 0.1295 -0.0008 0.8323 0.039 Uiso 1 1 calc R . . C4 C 0.0688(6) 0.0887(3) 0.6917(7) 0.0259(15) Uani 1 1 d . . . C5 C -0.0341(6) 0.1176(3) 0.6049(7) 0.0263(15) Uani 1 1 d . . . H5 H -0.0292 0.1646 0.5519 0.032 Uiso 1 1 calc R . . C6 C 0.1855(6) 0.1285(3) 0.6930(7) 0.0273(15) Uani 1 1 d . . . C7 C 0.3259(6) 0.2176(4) 0.7000(7) 0.0278(15) Uani 1 1 d . . . C8 C 0.3852(5) 0.2918(3) 0.7101(7) 0.0233(14) Uani 1 1 d . . . C9 C 0.3395(6) 0.3558(4) 0.6276(8) 0.0306(16) Uani 1 1 d . . . H9 H 0.2649 0.3534 0.5659 0.037 Uiso 1 1 calc R . . C10 C 0.4032(6) 0.4224(3) 0.6362(8) 0.0303(16) Uani 1 1 d . . . H10 H 0.3744 0.4650 0.5771 0.036 Uiso 1 1 calc R . . C11 C 0.5113(6) 0.4256(4) 0.7343(8) 0.0315(16) Uani 1 1 d . . . H11 H 0.5530 0.4716 0.7441 0.038 Uiso 1 1 calc R . . C12 C 0.4970(6) 0.2988(3) 0.8019(7) 0.0249(14) Uani 1 1 d . . . H12 H 0.5304 0.2561 0.8557 0.030 Uiso 1 1 calc R . . N1 N -0.1407(4) 0.0794(3) 0.5953(6) 0.0227(12) Uani 1 1 d . . . N2 N 0.2920(5) 0.0951(3) 0.6748(7) 0.0341(14) Uani 1 1 d . . . N3 N 0.2027(5) 0.2054(3) 0.7102(6) 0.0246(12) Uani 1 1 d . . . N5 N 0.3805(5) 0.1516(3) 0.6769(7) 0.0334(14) Uani 1 1 d . . . N6 N 0.5582(5) 0.3647(3) 0.8158(6) 0.0277(13) Uani 1 1 d . . . O2 O 0.7185(4) 0.2595(2) 1.0549(6) 0.0391(12) Uani 1 1 d . . . O3 O 0.7237(4) 0.1056(3) 0.9450(5) 0.0451(13) Uani 1 1 d . . . O4 O 0.8166(4) 0.1429(2) 1.2796(5) 0.0320(11) Uani 1 1 d . . . O5 O 0.9501(4) 0.1898(3) 0.9924(6) 0.0420(12) Uani 1 1 d . . . O1 O 0.6096(5) 0.4104(3) 1.1474(6) 0.0287(11) Uani 1 1 d . . . N4 N 0.1174(5) 0.2605(3) 0.7621(7) 0.0363(14) Uani 1 1 d . . . H4A H 0.1421 0.3054 0.7901 0.044 Uiso 1 1 calc R . . H4B H 0.0409 0.2491 0.7657 0.044 Uiso 1 1 calc R . . H1W H 0.559(6) 0.385(3) 1.180(8) 0.02(2) Uiso 1 1 d . . . H2W H 0.644(7) 0.403(4) 1.250(9) 0.05(3) 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 Cu1 0.0203(4) 0.0256(4) 0.0241(4) -0.0018(3) 0.0013(3) -0.0018(3) Mo1 0.0258(3) 0.0237(3) 0.0219(3) 0.0023(2) 0.0035(2) 0.0002(2) C1 0.024(4) 0.029(4) 0.032(4) -0.004(3) 0.004(3) -0.005(3) C2 0.033(4) 0.018(3) 0.049(4) 0.003(3) 0.003(4) -0.001(3) C3 0.034(4) 0.025(4) 0.038(4) 0.002(3) -0.005(3) 0.009(3) C4 0.021(4) 0.031(4) 0.026(3) -0.005(3) 0.004(3) 0.003(3) C5 0.030(4) 0.022(3) 0.026(3) -0.003(3) 0.002(3) -0.004(3) C6 0.030(4) 0.028(4) 0.024(3) -0.008(3) 0.000(3) 0.000(3) C7 0.020(4) 0.043(4) 0.020(3) 0.001(3) 0.001(3) -0.007(3) C8 0.019(3) 0.029(3) 0.022(3) -0.003(3) 0.002(3) -0.003(3) C9 0.023(4) 0.042(4) 0.026(4) -0.002(3) -0.005(3) 0.009(3) C10 0.036(4) 0.023(3) 0.031(4) 0.010(3) -0.002(3) 0.001(3) C11 0.041(4) 0.020(3) 0.034(4) 0.001(3) 0.004(3) -0.002(3) C12 0.026(4) 0.025(3) 0.024(3) 0.001(3) 0.002(3) -0.003(3) N1 0.019(3) 0.025(3) 0.025(3) 0.001(2) 0.005(2) -0.001(2) N2 0.027(3) 0.031(3) 0.045(4) -0.003(3) 0.001(3) -0.004(3) N3 0.025(3) 0.026(3) 0.023(3) -0.003(2) 0.001(2) 0.002(2) N5 0.017(3) 0.033(3) 0.050(4) -0.005(3) -0.003(3) 0.000(2) N6 0.027(3) 0.027(3) 0.029(3) -0.003(2) 0.001(3) -0.002(2) O2 0.037(3) 0.027(2) 0.053(3) 0.010(2) 0.003(2) 0.005(2) O3 0.054(4) 0.046(3) 0.035(3) -0.008(2) 0.000(3) -0.010(3) O4 0.030(3) 0.046(3) 0.020(2) 0.007(2) 0.005(2) 0.007(2) O5 0.036(3) 0.051(3) 0.040(3) 0.001(2) 0.012(2) -0.005(2) O1 0.024(3) 0.035(3) 0.028(3) 0.001(2) 0.005(2) -0.002(2) N4 0.020(3) 0.026(3) 0.064(4) -0.014(3) 0.010(3) -0.003(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 Cu1 O4 1.920(4) 4_565 ? Cu1 O1 1.964(5) . ? Cu1 N1 2.017(5) 4_666 ? Cu1 N6 2.024(5) . ? Cu1 O2 2.163(4) . ? Mo1 O2 1.738(4) . ? Mo1 O3 1.746(4) . ? Mo1 O5 1.761(5) . ? Mo1 O4 1.785(4) . ? C1 N1 1.347(7) . ? C1 C2 1.390(8) . ? C1 H1 0.9300 . ? C2 C3 1.386(8) . ? C2 H2 0.9300 . ? C3 C4 1.385(8) . ? C3 H3 0.9300 . ? C4 C5 1.383(8) . ? C4 C6 1.452(8) . ? C5 N1 1.342(7) . ? C5 H5 0.9300 . ? C6 N2 1.315(8) . ? C6 N3 1.374(7) . ? C7 N5 1.321(8) . ? C7 N3 1.367(7) . ? C7 C8 1.459(8) . ? C8 C9 1.382(8) . ? C8 C12 1.395(8) . ? C9 C10 1.364(8) . ? C9 H9 0.9300 . ? C10 C11 1.381(8) . ? C10 H10 0.9300 . ? C11 N6 1.339(7) . ? C11 H11 0.9300 . ? C12 N6 1.340(7) . ? C12 H12 0.9300 . ? N1 Cu1 2.017(5) 4_465 ? N2 N5 1.387(7) . ? N3 N4 1.417(7) . ? O4 Cu1 1.920(4) 4_566 ? O1 H1W 0.77(6) . ? O1 H2W 0.88(7) . ? N4 H4A 0.8600 . ? N4 H4B 0.8600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O4 Cu1 O1 171.63(19) 4_565 . ? O4 Cu1 N1 88.60(18) 4_565 4_666 ? O1 Cu1 N1 88.5(2) . 4_666 ? O4 Cu1 N6 92.41(19) 4_565 . ? O1 Cu1 N6 88.0(2) . . ? N1 Cu1 N6 162.2(2) 4_666 . ? O4 Cu1 O2 94.58(18) 4_565 . ? O1 Cu1 O2 93.69(19) . . ? N1 Cu1 O2 101.31(19) 4_666 . ? N6 Cu1 O2 96.35(19) . . ? O2 Mo1 O3 109.5(2) . . ? O2 Mo1 O5 110.2(2) . . ? O3 Mo1 O5 110.9(2) . . ? O2 Mo1 O4 109.9(2) . . ? O3 Mo1 O4 108.2(2) . . ? O5 Mo1 O4 108.1(2) . . ? N1 C1 C2 122.0(6) . . ? N1 C1 H1 119.0 . . ? C2 C1 H1 119.0 . . ? C3 C2 C1 118.5(6) . . ? C3 C2 H2 120.7 . . ? C1 C2 H2 120.7 . . ? C4 C3 C2 119.2(6) . . ? C4 C3 H3 120.4 . . ? C2 C3 H3 120.4 . . ? C5 C4 C3 119.3(6) . . ? C5 C4 C6 121.2(6) . . ? C3 C4 C6 119.4(6) . . ? N1 C5 C4 121.7(6) . . ? N1 C5 H5 119.2 . . ? C4 C5 H5 119.2 . . ? N2 C6 N3 109.6(5) . . ? N2 C6 C4 124.2(6) . . ? N3 C6 C4 126.2(6) . . ? N5 C7 N3 108.7(5) . . ? N5 C7 C8 126.4(6) . . ? N3 C7 C8 124.9(6) . . ? C9 C8 C12 117.4(6) . . ? C9 C8 C7 123.7(6) . . ? C12 C8 C7 118.8(6) . . ? C10 C9 C8 120.4(6) . . ? C10 C9 H9 119.8 . . ? C8 C9 H9 119.8 . . ? C9 C10 C11 118.8(6) . . ? C9 C10 H10 120.6 . . ? C11 C10 H10 120.6 . . ? N6 C11 C10 122.3(6) . . ? N6 C11 H11 118.9 . . ? C10 C11 H11 118.9 . . ? N6 C12 C8 122.6(6) . . ? N6 C12 H12 118.7 . . ? C8 C12 H12 118.7 . . ? C5 N1 C1 119.2(5) . . ? C5 N1 Cu1 119.7(4) . 4_465 ? C1 N1 Cu1 121.1(4) . 4_465 ? C6 N2 N5 107.2(5) . . ? C7 N3 C6 106.2(5) . . ? C7 N3 N4 124.8(5) . . ? C6 N3 N4 127.9(5) . . ? C7 N5 N2 108.4(5) . . ? C11 N6 C12 118.4(6) . . ? C11 N6 Cu1 119.6(4) . . ? C12 N6 Cu1 121.9(4) . . ? Mo1 O2 Cu1 146.0(3) . . ? Mo1 O4 Cu1 138.3(2) . 4_566 ? Cu1 O1 H1W 121(5) . . ? Cu1 O1 H2W 113(5) . . ? H1W O1 H2W 84(6) . . ? N3 N4 H4A 120.0 . . ? N3 N4 H4B 120.0 . . ? H4A N4 H4B 120.0 . . ? 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 O1 H1W N5 0.77(6) 2.05(6) 2.746(7) 152(6) 4_566 O1 H2W O3 0.88(7) 1.74(7) 2.622(6) 174(7) 4_566 N4 H4B O5 0.86 2.57 2.876(7) 102.2 4_465 N4 H4B O5 0.86 2.33 2.914(7) 125.2 1_455 _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.668 _refine_diff_density_min -0.771 _refine_diff_density_rms 0.144 # Attachment '5.cif' data_081205b_0m _database_code_depnum_ccdc_archive 'CCDC 762853' #TrackingRef '5.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H28 Co Mo6 N12 O23' _chemical_formula_weight 1487.15 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' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.5193(8) _cell_length_b 10.9534(9) _cell_length_c 11.4935(9) _cell_angle_alpha 91.7860(10) _cell_angle_beta 113.8000(10) _cell_angle_gamma 105.4690(10) _cell_volume 1043.60(15) _cell_formula_units_Z 1 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 4935 _cell_measurement_theta_min 2.40 _cell_measurement_theta_max 27.57 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.366 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 719 _exptl_absorpt_coefficient_mu 2.231 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6054 _exptl_absorpt_correction_T_max 0.6639 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5378 _diffrn_reflns_av_R_equivalents 0.0147 _diffrn_reflns_av_sigmaI/netI 0.0255 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 1.95 _diffrn_reflns_theta_max 25.05 _reflns_number_total 3617 _reflns_number_gt 3468 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0316P)^2^+3.1780P] 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 3617 _refine_ls_number_parameters 302 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0277 _refine_ls_R_factor_gt 0.0264 _refine_ls_wR_factor_ref 0.0710 _refine_ls_wR_factor_gt 0.0702 _refine_ls_goodness_of_fit_ref 1.103 _refine_ls_restrained_S_all 1.103 _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 Co1 Co 1.0000 0.5000 0.5000 0.01196(16) Uani 1 2 d S . . Mo1 Mo 0.58111(4) 0.37889(3) 0.25017(3) 0.01088(10) Uani 1 1 d . . . Mo2 Mo 0.48849(4) 0.35266(3) -0.06347(3) 0.01239(10) Uani 1 1 d . . . Mo3 Mo 0.47606(4) 0.07135(3) 0.13998(3) 0.01545(10) Uani 1 1 d . . . C1 C 0.0885(5) 0.2847(4) -0.0570(4) 0.0162(8) Uani 1 1 d . . . C2 C -0.0201(5) 0.2668(4) -0.1944(4) 0.0174(8) Uani 1 1 d . . . C3 C 0.0199(5) 0.3583(4) -0.2648(4) 0.0154(8) Uani 1 1 d . . . H3 H 0.1102 0.4294 -0.2220 0.018 Uiso 1 1 calc R . . C4 C -0.1923(6) 0.2458(4) -0.4520(4) 0.0289(11) Uani 1 1 d . . . H4 H -0.2506 0.2368 -0.5407 0.035 Uiso 1 1 calc R . . C5 C -0.2409(7) 0.1507(5) -0.3871(5) 0.0491(16) Uani 1 1 d . . . H5 H -0.3314 0.0804 -0.4321 0.059 Uiso 1 1 calc R . . C6 C -0.1556(6) 0.1601(5) -0.2568(5) 0.0409(14) Uani 1 1 d . . . H6 H -0.1871 0.0977 -0.2117 0.049 Uiso 1 1 calc R . . C7 C 0.1764(5) 0.2992(4) 0.1523(4) 0.0139(8) Uani 1 1 d . . . C8 C 0.1823(5) 0.2982(4) 0.2826(4) 0.0144(8) Uani 1 1 d . . . C9 C 0.1074(5) 0.3717(4) 0.3229(4) 0.0167(8) Uani 1 1 d . . . H9 H 0.0503 0.4176 0.2650 0.020 Uiso 1 1 calc R . . C10 C 0.1958(5) 0.3135(4) 0.5224(4) 0.0181(8) Uani 1 1 d . . . H10 H 0.2014 0.3188 0.6052 0.022 Uiso 1 1 calc R . . C11 C 0.2735(6) 0.2372(4) 0.4902(4) 0.0246(10) Uani 1 1 d . . . H11 H 0.3289 0.1919 0.5499 0.030 Uiso 1 1 calc R . . C12 C 0.2676(5) 0.2294(4) 0.3684(4) 0.0213(9) Uani 1 1 d . . . H12 H 0.3194 0.1794 0.3443 0.026 Uiso 1 1 calc R . . N1 N 0.2456(4) 0.3179(3) -0.0070(3) 0.0137(7) Uani 1 1 d . . . N2 N 0.3005(4) 0.3260(3) 0.1245(3) 0.0132(7) Uani 1 1 d . . . N3 N 0.0402(4) 0.2725(3) 0.0414(3) 0.0153(7) Uani 1 1 d . . . N4 N -0.1168(4) 0.2374(4) 0.0345(4) 0.0253(8) Uani 1 1 d . . . H4A H -0.1306 0.2318 0.1038 0.030 Uiso 1 1 calc R . . H4B H -0.1987 0.2215 -0.0390 0.030 Uiso 1 1 calc R . . N5 N -0.0652(4) 0.3497(3) -0.3920(3) 0.0177(7) Uani 1 1 d . . . N6 N 0.1135(4) 0.3795(3) 0.4411(3) 0.0150(7) Uani 1 1 d . . . O1 O 0.5347(4) 0.4590(3) 0.3507(3) 0.0211(6) Uani 1 1 d . . . O2 O 0.5702(3) 0.4897(2) 0.1145(2) 0.0133(5) Uani 1 1 d . . . O3 O 0.5236(3) 0.2103(2) 0.2791(2) 0.0144(6) Uani 1 1 d . . . O4 O 0.7919(3) 0.4200(3) 0.3306(2) 0.0145(6) Uani 1 1 d . . . O5 O 0.3474(4) 0.2458(3) -0.1970(3) 0.0240(7) Uani 1 1 d . . . O6 O 0.6635(4) 0.3860(3) -0.0818(3) 0.0239(7) Uani 1 1 d . . . O7 O 0.5332(3) 0.2559(2) 0.0717(2) 0.0139(6) Uani 1 1 d . . . O8 O 0.2706(4) 0.0403(3) 0.0702(3) 0.0285(7) Uani 1 1 d . . . O9 O 0.5000 0.0000 0.0000 0.0285(10) Uani 1 2 d S . . O10 O 0.7560(4) 0.1428(3) 0.2274(3) 0.0271(7) Uani 1 1 d . . . H10A H 0.7849 0.1917 0.1832 0.041 Uiso 1 1 calc R . . H10B H 0.8041 0.0894 0.2626 0.041 Uiso 1 1 d R . . O11 O 0.5029(4) -0.0397(3) 0.2396(3) 0.0319(8) Uani 1 1 d . . . O1W O 0.0898(6) 0.0224(5) 0.6516(6) 0.0806(17) Uani 1 1 d . . . H1WB H 0.1274 0.1020 0.6819 0.097 Uiso 1 1 d R . . H1WA H 0.0497 0.0037 0.5701 0.097 Uiso 1 1 d 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 Co1 0.0127(4) 0.0158(4) 0.0085(3) 0.0028(3) 0.0053(3) 0.0048(3) Mo1 0.01117(17) 0.01243(17) 0.00847(17) 0.00237(12) 0.00408(13) 0.00280(13) Mo2 0.01739(18) 0.01339(18) 0.00996(17) 0.00411(13) 0.00773(14) 0.00699(13) Mo3 0.01878(19) 0.01178(18) 0.01631(18) 0.00221(13) 0.00944(15) 0.00240(14) C1 0.019(2) 0.018(2) 0.0125(19) 0.0057(15) 0.0082(17) 0.0041(16) C2 0.013(2) 0.024(2) 0.012(2) 0.0053(16) 0.0047(16) 0.0025(17) C3 0.0134(19) 0.019(2) 0.0114(19) 0.0026(15) 0.0048(16) 0.0016(16) C4 0.027(2) 0.032(3) 0.013(2) 0.0055(18) 0.0009(19) 0.000(2) C5 0.039(3) 0.044(3) 0.024(3) 0.011(2) -0.005(2) -0.020(3) C6 0.038(3) 0.042(3) 0.022(2) 0.015(2) 0.007(2) -0.012(2) C7 0.017(2) 0.0136(19) 0.0142(19) 0.0034(15) 0.0080(16) 0.0067(16) C8 0.0130(19) 0.020(2) 0.0122(19) 0.0037(15) 0.0081(16) 0.0035(16) C9 0.017(2) 0.021(2) 0.0131(19) 0.0046(16) 0.0063(16) 0.0087(17) C10 0.019(2) 0.024(2) 0.0124(19) 0.0040(16) 0.0080(17) 0.0058(17) C11 0.030(2) 0.032(2) 0.021(2) 0.0138(19) 0.013(2) 0.018(2) C12 0.026(2) 0.026(2) 0.022(2) 0.0077(18) 0.0163(19) 0.0141(19) N1 0.0152(17) 0.0188(17) 0.0084(15) 0.0044(13) 0.0060(13) 0.0054(14) N2 0.0140(16) 0.0173(16) 0.0086(15) 0.0033(12) 0.0056(13) 0.0039(13) N3 0.0140(17) 0.0208(17) 0.0124(16) 0.0048(13) 0.0081(14) 0.0034(14) N4 0.0129(18) 0.047(2) 0.0180(18) 0.0085(17) 0.0094(15) 0.0069(17) N5 0.0178(17) 0.0212(18) 0.0150(17) 0.0050(14) 0.0084(14) 0.0050(14) N6 0.0148(17) 0.0187(17) 0.0125(16) 0.0021(13) 0.0067(14) 0.0054(14) O1 0.0225(16) 0.0219(15) 0.0176(15) -0.0031(12) 0.0092(13) 0.0043(12) O2 0.0161(14) 0.0143(13) 0.0107(13) 0.0034(10) 0.0061(11) 0.0056(11) O3 0.0156(14) 0.0146(13) 0.0118(13) 0.0036(10) 0.0060(11) 0.0022(11) O4 0.0112(13) 0.0180(14) 0.0112(13) 0.0042(11) 0.0033(11) 0.0021(11) O5 0.0330(18) 0.0208(15) 0.0141(14) 0.0004(12) 0.0067(13) 0.0078(13) O6 0.0277(17) 0.0292(17) 0.0290(17) 0.0135(13) 0.0217(14) 0.0145(14) O7 0.0162(14) 0.0145(13) 0.0116(13) 0.0028(10) 0.0067(11) 0.0044(11) O8 0.0215(16) 0.0244(16) 0.0313(18) -0.0007(13) 0.0081(14) -0.0003(13) O9 0.044(3) 0.018(2) 0.029(2) 0.0000(18) 0.021(2) 0.009(2) O10 0.0237(16) 0.0317(18) 0.0305(18) 0.0121(14) 0.0134(14) 0.0121(14) O11 0.046(2) 0.0238(17) 0.0365(19) 0.0153(14) 0.0248(17) 0.0139(15) O1W 0.061(3) 0.047(3) 0.099(4) 0.019(3) 0.003(3) 0.013(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 Co1 O4 2.083(3) 2_766 ? Co1 O4 2.083(3) . ? Co1 N6 2.159(3) 1_655 ? Co1 N6 2.159(3) 2_666 ? Co1 N5 2.200(3) 2_665 ? Co1 N5 2.200(3) 1_656 ? Mo1 O1 1.690(3) . ? Mo1 O4 1.754(3) . ? Mo1 O3 1.862(3) . ? Mo1 O2 1.993(3) . ? Mo1 O7 2.230(3) . ? Mo1 N2 2.359(3) . ? Mo2 O5 1.708(3) . ? Mo2 O6 1.708(3) . ? Mo2 O7 1.879(3) . ? Mo2 O2 1.987(3) 2_665 ? Mo2 O2 2.224(3) . ? Mo3 O11 1.695(3) . ? Mo3 O8 1.717(3) . ? Mo3 O9 1.8878(4) . ? Mo3 O3 1.993(3) . ? Mo3 O7 2.203(3) . ? Mo3 O10 2.324(3) . ? C1 N1 1.305(5) . ? C1 N3 1.380(5) . ? C1 C2 1.469(5) . ? C2 C3 1.378(5) . ? C2 C6 1.393(6) . ? C3 N5 1.341(5) . ? C3 H3 0.9300 . ? C4 N5 1.333(6) . ? C4 C5 1.388(7) . ? C4 H4 0.9300 . ? C5 C6 1.370(7) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? C7 N2 1.308(5) . ? C7 N3 1.354(5) . ? C7 C8 1.476(5) . ? C8 C9 1.386(6) . ? C8 C12 1.387(6) . ? C9 N6 1.335(5) . ? C9 H9 0.9300 . ? C10 N6 1.328(5) . ? C10 C11 1.384(6) . ? C10 H10 0.9300 . ? C11 C12 1.378(6) . ? C11 H11 0.9300 . ? C12 H12 0.9300 . ? N1 N2 1.377(4) . ? N3 N4 1.408(5) . ? N4 H4A 0.8600 . ? N4 H4B 0.8600 . ? N5 Co1 2.200(3) 1_454 ? N6 Co1 2.159(3) 1_455 ? O2 Mo2 1.987(3) 2_665 ? O9 Mo3 1.8877(4) 2_655 ? O10 H10A 0.8200 . ? O10 H10B 0.8502 . ? O1W H1WB 0.8500 . ? O1W H1WA 0.8500 . ? 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 Co1 O4 180.0 2_766 . ? O4 Co1 N6 91.26(11) 2_766 1_655 ? O4 Co1 N6 88.74(11) . 1_655 ? O4 Co1 N6 88.74(11) 2_766 2_666 ? O4 Co1 N6 91.26(11) . 2_666 ? N6 Co1 N6 180.00(19) 1_655 2_666 ? O4 Co1 N5 94.02(11) 2_766 2_665 ? O4 Co1 N5 85.98(11) . 2_665 ? N6 Co1 N5 92.69(13) 1_655 2_665 ? N6 Co1 N5 87.31(13) 2_666 2_665 ? O4 Co1 N5 85.98(11) 2_766 1_656 ? O4 Co1 N5 94.02(11) . 1_656 ? N6 Co1 N5 87.32(12) 1_655 1_656 ? N6 Co1 N5 92.68(13) 2_666 1_656 ? N5 Co1 N5 179.997(1) 2_665 1_656 ? O1 Mo1 O4 102.72(13) . . ? O1 Mo1 O3 103.06(13) . . ? O4 Mo1 O3 100.32(12) . . ? O1 Mo1 O2 102.95(13) . . ? O4 Mo1 O2 97.42(11) . . ? O3 Mo1 O2 144.23(11) . . ? O1 Mo1 O7 156.27(12) . . ? O4 Mo1 O7 100.95(11) . . ? O3 Mo1 O7 74.08(10) . . ? O2 Mo1 O7 72.19(10) . . ? O1 Mo1 N2 81.22(13) . . ? O4 Mo1 N2 174.76(11) . . ? O3 Mo1 N2 81.97(11) . . ? O2 Mo1 N2 78.21(11) . . ? O7 Mo1 N2 75.05(10) . . ? O5 Mo2 O6 105.17(15) . . ? O5 Mo2 O7 105.38(13) . . ? O6 Mo2 O7 100.96(13) . . ? O5 Mo2 O2 98.97(13) . 2_665 ? O6 Mo2 O2 98.88(12) . 2_665 ? O7 Mo2 O2 143.08(11) . 2_665 ? O5 Mo2 O2 154.41(13) . . ? O6 Mo2 O2 99.87(13) . . ? O7 Mo2 O2 74.40(10) . . ? O2 Mo2 O2 71.72(11) 2_665 . ? O11 Mo3 O8 102.84(16) . . ? O11 Mo3 O9 102.23(11) . . ? O8 Mo3 O9 99.05(11) . . ? O11 Mo3 O3 93.90(14) . . ? O8 Mo3 O3 96.48(13) . . ? O9 Mo3 O3 154.44(8) . . ? O11 Mo3 O7 157.60(14) . . ? O8 Mo3 O7 96.37(13) . . ? O9 Mo3 O7 85.81(7) . . ? O3 Mo3 O7 72.35(10) . . ? O11 Mo3 O10 84.68(14) . . ? O8 Mo3 O10 171.81(13) . . ? O9 Mo3 O10 82.29(8) . . ? O3 Mo3 O10 79.59(11) . . ? O7 Mo3 O10 75.63(10) . . ? N1 C1 N3 108.6(3) . . ? N1 C1 C2 126.2(4) . . ? N3 C1 C2 125.2(4) . . ? C3 C2 C6 119.2(4) . . ? C3 C2 C1 117.4(3) . . ? C6 C2 C1 123.3(4) . . ? N5 C3 C2 123.1(4) . . ? N5 C3 H3 118.5 . . ? C2 C3 H3 118.5 . . ? N5 C4 C5 122.5(4) . . ? N5 C4 H4 118.8 . . ? C5 C4 H4 118.8 . . ? C6 C5 C4 120.1(5) . . ? C6 C5 H5 119.9 . . ? C4 C5 H5 119.9 . . ? C5 C6 C2 117.5(4) . . ? C5 C6 H6 121.2 . . ? C2 C6 H6 121.2 . . ? N2 C7 N3 108.7(3) . . ? N2 C7 C8 126.1(4) . . ? N3 C7 C8 125.2(3) . . ? C9 C8 C12 118.9(4) . . ? C9 C8 C7 119.7(3) . . ? C12 C8 C7 121.4(4) . . ? N6 C9 C8 122.9(4) . . ? N6 C9 H9 118.5 . . ? C8 C9 H9 118.5 . . ? N6 C10 C11 123.3(4) . . ? N6 C10 H10 118.4 . . ? C11 C10 H10 118.4 . . ? C12 C11 C10 119.1(4) . . ? C12 C11 H11 120.5 . . ? C10 C11 H11 120.5 . . ? C11 C12 C8 118.2(4) . . ? C11 C12 H12 120.9 . . ? C8 C12 H12 120.9 . . ? C1 N1 N2 107.7(3) . . ? C7 N2 N1 108.6(3) . . ? C7 N2 Mo1 133.4(3) . . ? N1 N2 Mo1 118.0(2) . . ? C7 N3 C1 106.5(3) . . ? C7 N3 N4 124.3(3) . . ? C1 N3 N4 129.2(3) . . ? N3 N4 H4A 120.0 . . ? N3 N4 H4B 120.0 . . ? H4A N4 H4B 120.0 . . ? C4 N5 C3 117.5(4) . . ? C4 N5 Co1 120.6(3) . 1_454 ? C3 N5 Co1 121.9(3) . 1_454 ? C10 N6 C9 117.6(3) . . ? C10 N6 Co1 121.1(3) . 1_455 ? C9 N6 Co1 121.2(3) . 1_455 ? Mo2 O2 Mo1 139.85(14) 2_665 . ? Mo2 O2 Mo2 108.28(11) 2_665 . ? Mo1 O2 Mo2 104.20(11) . . ? Mo1 O3 Mo3 117.47(13) . . ? Mo1 O4 Co1 147.85(15) . . ? Mo2 O7 Mo3 148.70(14) . . ? Mo2 O7 Mo1 107.98(12) . . ? Mo3 O7 Mo1 96.07(10) . . ? Mo3 O9 Mo3 180.0 2_655 . ? Mo3 O10 H10A 109.5 . . ? Mo3 O10 H10B 116.3 . . ? H10A O10 H10B 123.3 . . ? H1WB O1W H1WA 115.9 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C1 C2 C3 -44.8(6) . . . . ? N3 C1 C2 C3 133.2(4) . . . . ? N1 C1 C2 C6 132.3(5) . . . . ? N3 C1 C2 C6 -49.7(7) . . . . ? C6 C2 C3 N5 -0.5(7) . . . . ? C1 C2 C3 N5 176.8(4) . . . . ? N5 C4 C5 C6 -1.2(10) . . . . ? C4 C5 C6 C2 -0.6(10) . . . . ? C3 C2 C6 C5 1.4(8) . . . . ? C1 C2 C6 C5 -175.7(5) . . . . ? N2 C7 C8 C9 125.2(4) . . . . ? N3 C7 C8 C9 -54.7(6) . . . . ? N2 C7 C8 C12 -52.0(6) . . . . ? N3 C7 C8 C12 128.2(4) . . . . ? C12 C8 C9 N6 0.0(6) . . . . ? C7 C8 C9 N6 -177.2(4) . . . . ? N6 C10 C11 C12 0.7(7) . . . . ? C10 C11 C12 C8 -0.5(7) . . . . ? C9 C8 C12 C11 0.2(6) . . . . ? C7 C8 C12 C11 177.3(4) . . . . ? N3 C1 N1 N2 0.8(4) . . . . ? C2 C1 N1 N2 179.0(4) . . . . ? N3 C7 N2 N1 0.5(4) . . . . ? C8 C7 N2 N1 -179.4(3) . . . . ? N3 C7 N2 Mo1 -178.5(2) . . . . ? C8 C7 N2 Mo1 1.6(6) . . . . ? C1 N1 N2 C7 -0.8(4) . . . . ? C1 N1 N2 Mo1 178.4(2) . . . . ? O1 Mo1 N2 C7 -37.8(4) . . . . ? O4 Mo1 N2 C7 -176.8(11) . . . . ? O3 Mo1 N2 C7 66.9(4) . . . . ? O2 Mo1 N2 C7 -143.1(4) . . . . ? O7 Mo1 N2 C7 142.5(4) . . . . ? O1 Mo1 N2 N1 143.3(3) . . . . ? O4 Mo1 N2 N1 4.2(14) . . . . ? O3 Mo1 N2 N1 -112.0(3) . . . . ? O2 Mo1 N2 N1 38.0(2) . . . . ? O7 Mo1 N2 N1 -36.5(2) . . . . ? N2 C7 N3 C1 0.0(4) . . . . ? C8 C7 N3 C1 179.8(4) . . . . ? N2 C7 N3 N4 178.9(3) . . . . ? C8 C7 N3 N4 -1.2(6) . . . . ? N1 C1 N3 C7 -0.5(4) . . . . ? C2 C1 N3 C7 -178.7(4) . . . . ? N1 C1 N3 N4 -179.4(4) . . . . ? C2 C1 N3 N4 2.4(7) . . . . ? C5 C4 N5 C3 2.2(7) . . . . ? C5 C4 N5 Co1 -177.9(5) . . . 1_454 ? C2 C3 N5 C4 -1.3(6) . . . . ? C2 C3 N5 Co1 178.7(3) . . . 1_454 ? C11 C10 N6 C9 -0.5(6) . . . . ? C11 C10 N6 Co1 -178.6(3) . . . 1_455 ? C8 C9 N6 C10 0.1(6) . . . . ? C8 C9 N6 Co1 178.2(3) . . . 1_455 ? O1 Mo1 O2 Mo2 -4.9(2) . . . 2_665 ? O4 Mo1 O2 Mo2 -109.8(2) . . . 2_665 ? O3 Mo1 O2 Mo2 130.8(2) . . . 2_665 ? O7 Mo1 O2 Mo2 151.0(2) . . . 2_665 ? N2 Mo1 O2 Mo2 73.1(2) . . . 2_665 ? O1 Mo1 O2 Mo2 -148.19(13) . . . . ? O4 Mo1 O2 Mo2 106.87(12) . . . . ? O3 Mo1 O2 Mo2 -12.5(2) . . . . ? O7 Mo1 O2 Mo2 7.70(10) . . . . ? N2 Mo1 O2 Mo2 -70.19(12) . . . . ? O5 Mo2 O2 Mo2 -72.0(3) . . . 2_665 ? O6 Mo2 O2 Mo2 96.17(14) . . . 2_665 ? O7 Mo2 O2 Mo2 -165.10(15) . . . 2_665 ? O2 Mo2 O2 Mo2 0.0 2_665 . . 2_665 ? O5 Mo2 O2 Mo1 84.1(3) . . . . ? O6 Mo2 O2 Mo1 -107.77(14) . . . . ? O7 Mo2 O2 Mo1 -9.04(11) . . . . ? O2 Mo2 O2 Mo1 156.06(19) 2_665 . . . ? O1 Mo1 O3 Mo3 157.00(15) . . . . ? O4 Mo1 O3 Mo3 -97.21(16) . . . . ? O2 Mo1 O3 Mo3 21.3(3) . . . . ? O7 Mo1 O3 Mo3 1.35(13) . . . . ? N2 Mo1 O3 Mo3 78.01(15) . . . . ? O11 Mo3 O3 Mo1 160.56(18) . . . . ? O8 Mo3 O3 Mo1 -96.03(17) . . . . ? O9 Mo3 O3 Mo1 31.2(3) . . . . ? O7 Mo3 O3 Mo1 -1.38(13) . . . . ? O10 Mo3 O3 Mo1 76.71(15) . . . . ? O1 Mo1 O4 Co1 13.4(3) . . . . ? O3 Mo1 O4 Co1 -92.7(3) . . . . ? O2 Mo1 O4 Co1 118.5(3) . . . . ? O7 Mo1 O4 Co1 -168.3(3) . . . . ? N2 Mo1 O4 Co1 151.8(11) . . . . ? O4 Co1 O4 Mo1 -18(10) 2_766 . . . ? N6 Co1 O4 Mo1 152.5(3) 1_655 . . . ? N6 Co1 O4 Mo1 -27.5(3) 2_666 . . . ? N5 Co1 O4 Mo1 -114.7(3) 2_665 . . . ? N5 Co1 O4 Mo1 65.3(3) 1_656 . . . ? O5 Mo2 O7 Mo3 -6.8(3) . . . . ? O6 Mo2 O7 Mo3 -116.1(3) . . . . ? O2 Mo2 O7 Mo3 122.6(3) 2_665 . . . ? O2 Mo2 O7 Mo3 146.6(3) . . . . ? O5 Mo2 O7 Mo1 -145.20(14) . . . . ? O6 Mo2 O7 Mo1 105.54(14) . . . . ? O2 Mo2 O7 Mo1 -15.8(2) 2_665 . . . ? O2 Mo2 O7 Mo1 8.23(10) . . . . ? O11 Mo3 O7 Mo2 166.2(3) . . . . ? O8 Mo3 O7 Mo2 -44.7(3) . . . . ? O9 Mo3 O7 Mo2 53.9(3) . . . . ? O3 Mo3 O7 Mo2 -139.5(3) . . . . ? O10 Mo3 O7 Mo2 137.0(3) . . . . ? O11 Mo3 O7 Mo1 -53.2(4) . . . . ? O8 Mo3 O7 Mo1 95.83(13) . . . . ? O9 Mo3 O7 Mo1 -165.51(8) . . . . ? O3 Mo3 O7 Mo1 1.03(10) . . . . ? O10 Mo3 O7 Mo1 -82.41(11) . . . . ? O1 Mo1 O7 Mo2 72.3(3) . . . . ? O4 Mo1 O7 Mo2 -103.65(14) . . . . ? O3 Mo1 O7 Mo2 158.61(15) . . . . ? O2 Mo1 O7 Mo2 -9.30(12) . . . . ? N2 Mo1 O7 Mo2 72.87(13) . . . . ? O1 Mo1 O7 Mo3 -87.4(3) . . . . ? O4 Mo1 O7 Mo3 96.65(11) . . . . ? O3 Mo1 O7 Mo3 -1.09(10) . . . . ? O2 Mo1 O7 Mo3 -169.00(13) . . . . ? N2 Mo1 O7 Mo3 -86.83(11) . . . . ? O11 Mo3 O9 Mo3 154(4) . . . 2_655 ? O8 Mo3 O9 Mo3 49(4) . . . 2_655 ? O3 Mo3 O9 Mo3 -78(4) . . . 2_655 ? O7 Mo3 O9 Mo3 -47(4) . . . 2_655 ? O10 Mo3 O9 Mo3 -123(4) . . . 2_655 ? 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 O1W H1WA O1W 0.85 2.32 3.153(11) 168.9 2_556 O1W H1WB O5 0.85 2.13 2.849(6) 141.5 1_556 O10 H10B O1W 0.85 1.85 2.700(6) 176.7 2_656 O10 H10A N4 0.82 2.27 3.016(5) 152.0 1_655 N4 H4B O6 0.86 2.45 2.917(5) 114.8 1_455 N4 H4A O10 0.86 2.21 3.016(5) 155.5 1_455 _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 1.971 _refine_diff_density_min -0.733 _refine_diff_density_rms 0.119