# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Ya-Guang Chen' _publ_contact_author_email CHENYG146@NENU.EDU.CN _publ_section_title ; "Tailoring'' microstructures of isopolymolybdates: regularly tuning ligand spacer length and metal coordination preferences ; loop_ _publ_author_name 'Ya-Guang Chen' 'HaiJun Pang' 'Qun Tang' 'Hui-Yuan Wang' ; Chunjing Zhang ; # Attachment 'compound_1.cif' data_compound1 _database_code_depnum_ccdc_archive 'CCDC 757937' #TrackingRef 'compound_1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C6 H8 Cu2 Mo3 N6 O10' _chemical_formula_weight 739.10 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 8.2050(8) _cell_length_b 10.4460(11) _cell_length_c 10.6300(11) _cell_angle_alpha 114.1400(11) _cell_angle_beta 102.6510(12) _cell_angle_gamma 92.7040(13) _cell_volume 801.61(14) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 7.5 _cell_measurement_theta_max 15 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.1121 _exptl_crystal_size_mid 0.1116 _exptl_crystal_size_min 0.1111 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.062 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 700.0 _exptl_absorpt_coefficient_mu 4.959 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.576 _exptl_absorpt_correction_T_max 0.579 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _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 2 _diffrn_standards_interval_count 150 _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 4312 _diffrn_reflns_av_R_equivalents 0.0187 _diffrn_reflns_av_sigmaI/netI 0.0386 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.16 _diffrn_reflns_theta_max 25.75 _reflns_number_total 3045 _reflns_number_gt 2616 _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^)+(0.0617P)^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 refall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3045 _refine_ls_number_parameters 244 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0361 _refine_ls_R_factor_gt 0.0296 _refine_ls_wR_factor_ref 0.0929 _refine_ls_wR_factor_gt 0.0790 _refine_ls_goodness_of_fit_ref 1.010 _refine_ls_restrained_S_all 1.010 _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 0.43220(6) 0.66188(5) 0.05619(5) 0.01343(14) Uani 1 1 d . . . Mo2 Mo 0.81690(6) 0.56822(5) 0.24863(5) 0.01450(14) Uani 1 1 d . . . Mo3 Mo -0.08874(6) 0.57737(5) 0.90818(5) 0.01233(14) Uani 1 1 d . . . Cu2 Cu 0.66289(11) 0.89950(8) 0.40711(8) 0.0277(2) Uani 1 1 d . . . Cu1 Cu 0.10768(10) 0.88805(9) 0.96855(8) 0.0284(2) Uani 1 1 d . . . O1 O 0.6178(5) 0.5515(4) 0.1024(4) 0.0167(8) Uani 1 1 d . . . O2 O -0.0211(5) 0.5065(4) 0.7275(4) 0.0148(8) Uani 1 1 d . . . O3 O 0.8612(5) 0.7492(4) 0.3511(4) 0.0258(10) Uani 1 1 d . . . O4 O 0.7189(5) 0.5060(5) 0.3437(5) 0.0287(10) Uani 1 1 d . . . O5 O -0.0399(5) 0.5992(4) 1.0979(4) 0.0147(8) Uani 1 1 d . . . O6 O 0.4636(5) 0.7789(4) 0.2347(4) 0.0197(9) Uani 1 1 d . . . O7 O 0.2130(5) 0.6508(4) -0.0376(4) 0.0197(9) Uani 1 1 d . . . O8 O -0.2938(5) 0.4921(4) 0.8445(4) 0.0210(9) Uani 1 1 d . . . O9 O -0.1005(5) 0.7521(4) 0.9339(4) 0.0201(9) Uani 1 1 d . . . O10 O 0.5393(5) 0.7501(4) -0.0117(5) 0.0249(9) Uani 1 1 d . . . N1 N 0.2392(6) 0.8236(5) 0.6054(5) 0.0181(10) Uani 1 1 d . . . N2 N 0.7433(6) 1.0319(5) 0.3364(5) 0.0226(11) Uani 1 1 d . . . N3 N 0.6782(6) 0.9171(5) 0.5977(5) 0.0199(10) Uani 1 1 d . . . N4 N 0.2309(6) 1.0048(5) 1.1654(5) 0.0224(11) Uani 1 1 d . . . N5 N 0.1416(6) 0.8861(5) 0.7911(5) 0.0217(11) Uani 1 1 d . . . N6 N 0.6038(6) 0.8281(5) 0.6411(5) 0.0197(10) Uani 1 1 d . . . C1 C 0.8042(8) 0.9986(6) 0.2252(6) 0.0259(14) Uani 1 1 d . . . H1A H 0.8097 0.9058 0.1640 0.031 Uiso 1 1 calc R . . C2 C 0.2232(7) 0.9848(6) 1.2799(6) 0.0217(13) Uani 1 1 d . . . H2A H 0.1546 0.9084 1.2748 0.026 Uiso 1 1 calc R . . C3 C 0.4802(7) 0.7038(6) 0.5388(6) 0.0191(12) Uani 1 1 d . . . H3A H 0.4626 0.6418 0.5836 0.023 Uiso 1 1 calc R . . H3B H 0.5245 0.6517 0.4579 0.023 Uiso 1 1 calc R . . C4 C 0.6587(7) 0.8763(6) 0.7806(6) 0.0212(13) Uani 1 1 d . . . H4A H 0.6251 0.8333 0.8341 0.025 Uiso 1 1 calc R . . C5 C 0.1670(8) 0.7762(6) 0.6821(6) 0.0239(13) Uani 1 1 d . . . H5A H 0.1390 0.6814 0.6621 0.029 Uiso 1 1 calc R . . C6 C 0.3122(7) 0.7442(6) 0.4863(6) 0.0221(13) Uani 1 1 d . . . H6A H 0.3284 0.8019 0.4368 0.026 Uiso 1 1 calc R . . H6B H 0.2341 0.6588 0.4189 0.026 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 0.0114(3) 0.0117(2) 0.0152(3) 0.0043(2) 0.00233(19) 0.00283(18) Mo2 0.0127(3) 0.0179(3) 0.0130(3) 0.0061(2) 0.00398(19) 0.00629(19) Mo3 0.0106(3) 0.0136(2) 0.0148(2) 0.00717(19) 0.00472(18) 0.00400(17) Cu2 0.0390(5) 0.0260(4) 0.0174(4) 0.0101(3) 0.0064(3) -0.0031(3) Cu1 0.0315(5) 0.0324(5) 0.0184(4) 0.0102(3) 0.0042(3) -0.0036(3) O1 0.015(2) 0.0127(19) 0.020(2) 0.0051(16) 0.0026(16) 0.0047(15) O2 0.0135(19) 0.020(2) 0.0140(19) 0.0091(16) 0.0057(15) 0.0046(15) O3 0.027(2) 0.023(2) 0.020(2) 0.0039(18) 0.0037(18) 0.0092(18) O4 0.028(2) 0.039(3) 0.031(2) 0.020(2) 0.017(2) 0.017(2) O5 0.019(2) 0.0120(19) 0.0139(19) 0.0057(16) 0.0049(16) 0.0023(15) O6 0.019(2) 0.019(2) 0.018(2) 0.0036(17) 0.0045(16) 0.0030(16) O7 0.013(2) 0.020(2) 0.027(2) 0.0118(18) 0.0035(17) 0.0041(16) O8 0.017(2) 0.023(2) 0.021(2) 0.0068(18) 0.0070(17) 0.0008(17) O9 0.020(2) 0.015(2) 0.026(2) 0.0102(17) 0.0050(17) 0.0046(16) O10 0.020(2) 0.026(2) 0.033(2) 0.0163(19) 0.0090(19) 0.0045(18) N1 0.018(3) 0.019(2) 0.019(2) 0.008(2) 0.009(2) 0.0028(19) N2 0.026(3) 0.018(3) 0.021(3) 0.005(2) 0.006(2) 0.002(2) N3 0.024(3) 0.018(2) 0.021(3) 0.009(2) 0.008(2) 0.004(2) N4 0.024(3) 0.023(3) 0.019(3) 0.010(2) 0.000(2) 0.006(2) N5 0.028(3) 0.019(3) 0.024(3) 0.010(2) 0.016(2) 0.001(2) N6 0.022(3) 0.016(2) 0.021(3) 0.008(2) 0.004(2) 0.004(2) C1 0.039(4) 0.016(3) 0.020(3) 0.005(2) 0.009(3) 0.005(3) C2 0.022(3) 0.019(3) 0.017(3) 0.006(2) -0.004(2) -0.001(2) C3 0.022(3) 0.012(3) 0.025(3) 0.006(2) 0.014(3) 0.001(2) C4 0.023(3) 0.032(3) 0.018(3) 0.017(3) 0.009(2) 0.007(3) C5 0.026(3) 0.021(3) 0.030(3) 0.013(3) 0.014(3) 0.004(3) C6 0.020(3) 0.025(3) 0.015(3) 0.002(2) 0.006(2) 0.001(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 O10 1.699(4) . ? Mo1 O6 1.738(4) . ? Mo1 O7 1.828(4) . ? Mo1 O1 2.047(4) . ? Mo1 O1 2.125(4) 2_665 ? Mo2 O4 1.713(4) . ? Mo2 O3 1.723(4) . ? Mo2 O2 1.892(4) 2_666 ? Mo2 O1 1.938(4) . ? Mo2 O5 2.295(4) 1_654 ? Mo2 O7 2.416(4) 2_665 ? Mo2 Mo3 3.1530(7) 2_666 ? Mo3 O8 1.717(4) . ? Mo3 O9 1.742(4) . ? Mo3 O5 1.882(4) . ? Mo3 O2 1.972(4) . ? Mo3 O5 2.153(4) 2_567 ? Mo3 O7 2.426(4) 1_556 ? Mo3 Mo2 3.1530(7) 2_666 ? Mo3 Mo3 3.1783(9) 2_567 ? Cu2 N3 1.933(5) . ? Cu2 N2 1.973(5) . ? Cu2 O6 2.055(4) . ? Cu2 O3 2.317(4) . ? Cu1 N4 1.938(5) . ? Cu1 N5 1.959(5) . ? Cu1 O9 2.034(4) . ? Cu1 Cu1 2.9442(17) 2_577 ? O1 Mo1 2.125(4) 2_665 ? O2 Mo2 1.892(4) 2_666 ? O5 Mo3 2.153(4) 2_567 ? O5 Mo2 2.295(4) 1_456 ? O7 Mo2 2.416(4) 2_665 ? O7 Mo3 2.426(4) 1_554 ? N1 C5 1.331(7) . ? N1 N2 1.364(7) 2_676 ? N1 C6 1.473(7) . ? N2 C1 1.306(7) . ? N2 N1 1.364(6) 2_676 ? N3 C2 1.329(7) 2_677 ? N3 N6 1.368(6) . ? N4 C2 1.331(7) . ? N4 C4 1.333(7) 2_677 ? N5 C5 1.321(8) . ? N5 C1 1.354(7) 2_676 ? N6 C4 1.316(7) . ? N6 C3 1.461(7) . ? C1 N5 1.354(7) 2_676 ? C2 N3 1.329(7) 2_677 ? C3 C6 1.517(8) . ? C4 N4 1.333(7) 2_677 ? 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 O10 Mo1 O6 104.85(19) . . ? O10 Mo1 O7 101.82(18) . . ? O6 Mo1 O7 108.33(18) . . ? O10 Mo1 O1 97.89(18) . . ? O6 Mo1 O1 92.74(17) . . ? O7 Mo1 O1 146.06(16) . . ? O10 Mo1 O1 103.63(18) . 2_665 ? O6 Mo1 O1 148.24(16) . 2_665 ? O7 Mo1 O1 78.98(16) . 2_665 ? O1 Mo1 O1 69.62(16) . 2_665 ? O4 Mo2 O3 104.1(2) . . ? O4 Mo2 O2 98.85(18) . 2_666 ? O3 Mo2 O2 107.75(18) . 2_666 ? O4 Mo2 O1 97.84(19) . . ? O3 Mo2 O1 101.69(18) . . ? O2 Mo2 O1 141.23(16) 2_666 . ? O4 Mo2 O5 166.86(17) . 1_654 ? O3 Mo2 O5 88.21(17) . 1_654 ? O2 Mo2 O5 72.49(14) 2_666 1_654 ? O1 Mo2 O5 83.98(15) . 1_654 ? O4 Mo2 O7 99.31(18) . 2_665 ? O3 Mo2 O7 156.11(17) . 2_665 ? O2 Mo2 O7 73.01(14) 2_666 2_665 ? O1 Mo2 O7 69.90(14) . 2_665 ? O5 Mo2 O7 68.99(13) 1_654 2_665 ? O4 Mo2 Mo3 124.78(15) . 2_666 ? O3 Mo2 Mo3 117.23(14) . 2_666 ? O2 Mo2 Mo3 36.15(11) 2_666 2_666 ? O1 Mo2 Mo3 107.22(11) . 2_666 ? O5 Mo2 Mo3 43.06(9) 1_654 2_666 ? O7 Mo2 Mo3 49.50(9) 2_665 2_666 ? O8 Mo3 O9 105.84(19) . . ? O8 Mo3 O5 100.82(17) . . ? O9 Mo3 O5 100.84(17) . . ? O8 Mo3 O2 99.18(17) . . ? O9 Mo3 O2 99.04(17) . . ? O5 Mo3 O2 146.61(16) . . ? O8 Mo3 O5 99.22(17) . 2_567 ? O9 Mo3 O5 154.83(16) . 2_567 ? O5 Mo3 O5 76.25(16) . 2_567 ? O2 Mo3 O5 74.36(14) . 2_567 ? O8 Mo3 O7 167.85(17) . 1_556 ? O9 Mo3 O7 83.80(16) . 1_556 ? O5 Mo3 O7 84.23(15) . 1_556 ? O2 Mo3 O7 71.55(14) . 1_556 ? O5 Mo3 O7 71.05(13) 2_567 1_556 ? O8 Mo3 Mo2 118.80(13) . 2_666 ? O9 Mo3 Mo2 115.91(13) . 2_666 ? O5 Mo3 Mo2 112.16(11) . 2_666 ? O2 Mo3 Mo2 34.47(11) . 2_666 ? O5 Mo3 Mo2 46.70(9) 2_567 2_666 ? O7 Mo3 Mo2 49.22(9) 1_556 2_666 ? O8 Mo3 Mo3 102.69(14) . 2_567 ? O9 Mo3 Mo3 136.42(13) . 2_567 ? O5 Mo3 Mo3 41.14(11) . 2_567 ? O2 Mo3 Mo3 108.16(11) . 2_567 ? O5 Mo3 Mo3 35.11(9) 2_567 2_567 ? O7 Mo3 Mo3 73.77(9) 1_556 2_567 ? Mo2 Mo3 Mo3 76.042(19) 2_666 2_567 ? N3 Cu2 N2 132.2(2) . . ? N3 Cu2 O6 123.12(18) . . ? N2 Cu2 O6 99.27(18) . . ? N3 Cu2 O3 98.40(17) . . ? N2 Cu2 O3 96.29(18) . . ? O6 Cu2 O3 97.97(15) . . ? N4 Cu1 N5 130.3(2) . . ? N4 Cu1 O9 117.16(19) . . ? N5 Cu1 O9 112.39(18) . . ? N4 Cu1 Cu1 82.13(15) . 2_577 ? N5 Cu1 Cu1 97.89(15) . 2_577 ? O9 Cu1 Cu1 86.48(11) . 2_577 ? Mo2 O1 Mo1 142.1(2) . . ? Mo2 O1 Mo1 107.30(17) . 2_665 ? Mo1 O1 Mo1 110.38(16) . 2_665 ? Mo2 O2 Mo3 109.38(17) 2_666 . ? Mo2 O3 Cu2 125.6(2) . . ? Mo3 O5 Mo3 103.75(16) . 2_567 ? Mo3 O5 Mo2 137.85(19) . 1_456 ? Mo3 O5 Mo2 90.24(13) 2_567 1_456 ? Mo1 O6 Cu2 137.9(2) . . ? Mo1 O7 Mo2 100.05(16) . 2_665 ? Mo1 O7 Mo3 152.4(2) . 1_554 ? Mo2 O7 Mo3 81.28(12) 2_665 1_554 ? Mo3 O9 Cu1 121.7(2) . . ? C5 N1 N2 109.5(5) . 2_676 ? C5 N1 C6 129.1(5) . . ? N2 N1 C6 121.0(4) 2_676 . ? C1 N2 N1 104.0(5) . 2_676 ? C1 N2 Cu2 126.4(4) . . ? N1 N2 Cu2 129.5(4) 2_676 . ? C2 N3 N6 102.3(5) 2_677 . ? C2 N3 Cu2 127.7(4) 2_677 . ? N6 N3 Cu2 129.8(4) . . ? C2 N4 C4 103.3(5) . 2_677 ? C2 N4 Cu1 127.6(4) . . ? C4 N4 Cu1 129.1(4) 2_677 . ? C5 N5 C1 105.1(5) . 2_676 ? C5 N5 Cu1 126.6(4) . . ? C1 N5 Cu1 125.3(4) 2_676 . ? C4 N6 N3 109.4(5) . . ? C4 N6 C3 129.5(5) . . ? N3 N6 C3 121.1(5) . . ? N2 C1 N5 112.6(5) . 2_676 ? N3 C2 N4 114.5(5) 2_677 . ? N6 C3 C6 112.1(5) . . ? N6 C4 N4 110.5(5) . 2_677 ? N5 C5 N1 108.8(5) . . ? N1 C6 C3 111.4(5) . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 25.75 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 0.706 _refine_diff_density_min -0.857 _refine_diff_density_rms 0.204 # Attachment 'compound_2.cif' data_compound2 _database_code_depnum_ccdc_archive 'CCDC 757938' #TrackingRef 'compound_2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C7 H12 Cu2 Mo3 N6 O11' _chemical_formula_weight 771.15 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' 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' Mn Mn 0.3368 0.7283 '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 7.5960(2) _cell_length_b 11.2990(5) _cell_length_c 11.3000(7) _cell_angle_alpha 68.561(5) _cell_angle_beta 73.317(4) _cell_angle_gamma 76.600(3) _cell_volume 855.95(8) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 7.5 _cell_measurement_theta_max 15 _exptl_crystal_description cuboid _exptl_crystal_colour red _exptl_crystal_size_max 0.1121 _exptl_crystal_size_mid 0.1116 _exptl_crystal_size_min 0.1111 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.992 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 736.0 _exptl_absorpt_coefficient_mu 4.655 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.596 _exptl_absorpt_correction_T_max 0.599 _exptl_absorpt_process_details ; CrysAlis (Oxford Diffraction, 2006) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Gemini R Ultra' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean 10.0 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6469 _diffrn_reflns_av_R_equivalents 0.0269 _diffrn_reflns_av_sigmaI/netI 0.0649 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 4.17 _diffrn_reflns_theta_max 29.23 _reflns_number_total 4664 _reflns_number_gt 2781 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis (Oxford Diffraction, 2006)' _computing_cell_refinement CrysAlis _computing_data_reduction CrysAlis _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The highest residual peak, 1.86 eA3, is close to the Mo2 position, which is featureless. ; _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^)+(0.0524P)^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 refall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4664 _refine_ls_number_parameters 262 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0583 _refine_ls_R_factor_gt 0.0384 _refine_ls_wR_factor_ref 0.0919 _refine_ls_wR_factor_gt 0.0880 _refine_ls_goodness_of_fit_ref 0.922 _refine_ls_restrained_S_all 0.922 _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 -0.05214(6) 0.41429(5) 0.16931(5) 0.00938(12) Uani 1 1 d . . . Mo2 Mo -0.45457(6) 0.59532(5) -0.16753(5) 0.01173(13) Uani 1 1 d . . . Mo3 Mo -0.17174(7) 0.34001(5) -0.05412(5) 0.01444(13) Uani 1 1 d . . . Cu2 Cu 0.26153(13) 0.11790(9) 0.21277(9) 0.0341(2) Uani 1 1 d . . . Cu1 Cu 0.73047(15) 0.04528(10) -0.77115(9) 0.0384(3) Uani 1 1 d . . . O10 O 0.8317(6) 0.1868(4) -0.9414(5) 0.0288(11) Uani 1 1 d . . . O9 O -0.4501(6) 0.7585(4) -0.2127(5) 0.0283(11) Uani 1 1 d . . . O8 O -0.1623(6) 0.4578(5) 0.3048(5) 0.0306(12) Uani 1 1 d . . . O7 O -0.4234(6) 0.5694(5) -0.3122(5) 0.0303(11) Uani 1 1 d . . . O6 O 0.0231(6) 0.2530(4) 0.2314(5) 0.0277(11) Uani 1 1 d . . . O5 O -0.1010(7) 0.3133(5) -0.2010(5) 0.0337(12) Uani 1 1 d . . . O4 O -0.4354(5) 0.3987(4) -0.0422(4) 0.0211(10) Uani 1 1 d . . . O3 O -0.0385(6) 0.6047(4) 0.0361(4) 0.0217(10) Uani 1 1 d . . . O2 O -0.2018(6) 0.5497(4) -0.1445(5) 0.0234(10) Uani 1 1 d . . . O1 O -0.2766(6) 0.4070(4) 0.1259(5) 0.0215(10) Uani 1 1 d . . . N2 N 0.7537(8) -0.0117(5) -0.3956(6) 0.0297(14) Uani 1 1 d . . . N5 N 0.7274(8) 0.0483(6) -0.6021(5) 0.0261(13) Uani 1 1 d . . . N4 N 0.3450(8) 0.1770(5) -0.1739(6) 0.0268(13) Uani 1 1 d . . . C5 C 0.7208(10) 0.1994(8) -0.3682(8) 0.0366(18) Uani 1 1 d . . . H5A H 0.8338 0.2385 -0.4038 0.044 Uiso 1 1 calc R . . H5B H 0.7215 0.1457 -0.2789 0.044 Uiso 1 1 calc R . . C4 C 0.5546(11) 0.3039(7) -0.3694(8) 0.0366(19) Uani 1 1 d . . . H4A H 0.5660 0.3561 -0.3210 0.044 Uiso 1 1 calc R . . H4B H 0.5579 0.3588 -0.4588 0.044 Uiso 1 1 calc R . . N3 N 0.3018(8) 0.1134(5) 0.0377(5) 0.0257(13) Uani 1 1 d . . . N1 N 0.7180(8) 0.1196(5) -0.4442(5) 0.0250(13) Uani 1 1 d . . . C3 C 0.3560(9) 0.2054(7) -0.0716(7) 0.0266(15) Uani 1 1 d . . . H3A H 0.3959 0.2793 -0.0766 0.032 Uiso 1 1 calc R . . C1 C 0.7028(10) 0.1512(7) -0.5654(7) 0.0275(16) Uani 1 1 d . . . H1A H 0.6778 0.2352 -0.6188 0.033 Uiso 1 1 calc R . . C2 C 0.3679(10) 0.2566(7) -0.3124(7) 0.0336(18) Uani 1 1 d . . . H2A H 0.2707 0.3300 -0.3207 0.040 Uiso 1 1 calc R . . H2B H 0.3536 0.2067 -0.3621 0.040 Uiso 1 1 calc R . . C6 C 0.7574(11) -0.0489(7) -0.4941(7) 0.0315(17) Uani 1 1 d . . . H6A H 0.7789 -0.1348 -0.4893 0.038 Uiso 1 1 calc R . . O1W O -0.0788(15) 0.6434(12) -0.5055(11) 0.137(4) Uani 1 1 d . . . H1WA H -0.1931 0.6364 -0.4732 0.164 Uiso 1 1 d R . . H1WB H -0.0228 0.6122 -0.4431 0.164 Uiso 1 1 d R . . N6 N 0.2798(8) 0.0614(5) -0.1299(6) 0.0272(13) Uani 1 1 d . . . C7 C 0.2558(10) 0.0283(7) -0.0029(7) 0.0292(16) Uani 1 1 d . . . H7A H 0.2109 -0.0471 0.0543 0.035 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 0.0062(2) 0.0100(2) 0.0126(2) -0.00193(19) -0.00445(18) -0.00233(18) Mo2 0.0080(2) 0.0114(2) 0.0156(3) -0.0016(2) -0.00557(19) -0.00176(19) Mo3 0.0127(2) 0.0121(2) 0.0207(3) -0.0061(2) -0.0062(2) -0.0016(2) Cu2 0.0466(5) 0.0336(5) 0.0236(5) -0.0112(4) -0.0122(4) 0.0003(4) Cu1 0.0578(6) 0.0399(6) 0.0241(5) -0.0146(4) -0.0095(5) -0.0118(5) O10 0.032(2) 0.022(2) 0.033(3) -0.007(2) -0.010(2) -0.006(2) O9 0.030(2) 0.019(2) 0.036(3) -0.002(2) -0.016(2) -0.004(2) O8 0.027(2) 0.037(3) 0.030(3) -0.014(2) -0.003(2) -0.005(2) O7 0.028(2) 0.040(3) 0.029(3) -0.015(2) -0.010(2) -0.005(2) O6 0.019(2) 0.024(2) 0.035(3) -0.003(2) -0.007(2) -0.004(2) O5 0.034(3) 0.040(3) 0.033(3) -0.019(2) -0.008(2) -0.004(2) O4 0.017(2) 0.020(2) 0.027(2) -0.004(2) -0.0086(19) -0.0046(18) O3 0.017(2) 0.022(2) 0.025(2) -0.0013(19) -0.0079(19) -0.0055(18) O2 0.017(2) 0.024(2) 0.030(3) -0.007(2) -0.0080(19) -0.0025(19) O1 0.017(2) 0.017(2) 0.033(3) -0.010(2) -0.0094(19) -0.0014(18) N2 0.043(3) 0.024(3) 0.023(3) -0.006(3) -0.014(3) -0.001(3) N5 0.033(3) 0.028(3) 0.018(3) -0.007(2) -0.006(2) -0.003(3) N4 0.035(3) 0.019(3) 0.025(3) -0.009(2) -0.004(3) -0.002(3) C5 0.037(4) 0.040(4) 0.041(5) -0.022(4) -0.005(4) -0.011(4) C4 0.058(5) 0.023(4) 0.027(4) -0.012(3) 0.001(4) -0.011(4) N3 0.032(3) 0.026(3) 0.023(3) -0.013(3) -0.006(3) -0.003(3) N1 0.032(3) 0.022(3) 0.024(3) -0.010(2) -0.010(3) 0.001(2) C3 0.032(4) 0.022(3) 0.028(4) -0.011(3) -0.007(3) -0.004(3) C1 0.039(4) 0.019(3) 0.023(4) -0.004(3) -0.011(3) -0.002(3) C2 0.041(4) 0.033(4) 0.024(4) -0.012(3) -0.009(3) 0.004(3) C6 0.053(5) 0.017(3) 0.028(4) -0.006(3) -0.018(4) -0.003(3) O1W 0.121(8) 0.172(11) 0.132(9) -0.045(8) -0.043(7) -0.037(8) N6 0.038(3) 0.021(3) 0.025(3) -0.008(2) -0.010(3) -0.005(3) C7 0.038(4) 0.028(4) 0.022(4) -0.008(3) -0.004(3) -0.008(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 O8 1.706(5) . ? Mo1 O6 1.718(4) . ? Mo1 O1 1.931(4) . ? Mo1 O2 1.983(4) 2_565 ? Mo1 O3 2.134(4) . ? Mo1 O3 2.299(5) 2_565 ? Mo2 O7 1.706(5) . ? Mo2 O9 1.730(5) . ? Mo2 O2 1.936(4) . ? Mo2 O1 1.964(4) 2_465 ? Mo2 O4 2.152(4) . ? Mo2 O4 2.296(5) 2_465 ? Mo3 O5 1.707(5) . ? Mo3 O10 1.734(4) 1_456 ? Mo3 O3 1.930(4) 2_565 ? Mo3 O4 1.940(4) . ? Mo3 O2 2.196(4) . ? Mo3 O1 2.293(5) . ? Cu2 N3 1.931(6) . ? Cu2 N2 1.959(6) 2_655 ? Cu2 O6 2.095(5) . ? Cu2 O9 2.220(5) 2_565 ? Cu1 N5 1.916(6) . ? Cu1 N6 1.946(6) 2_654 ? Cu1 O10 2.079(5) . ? O10 Mo3 1.734(4) 1_654 ? O9 Cu2 2.220(5) 2_565 ? O4 Mo2 2.296(5) 2_465 ? O3 Mo3 1.930(4) 2_565 ? O3 Mo1 2.299(5) 2_565 ? O2 Mo1 1.983(4) 2_565 ? O1 Mo2 1.964(4) 2_465 ? N2 C6 1.317(9) . ? N2 N1 1.371(8) . ? N2 Cu2 1.959(6) 2_655 ? N5 C1 1.329(9) . ? N5 C6 1.346(8) . ? N4 C3 1.336(9) . ? N4 N6 1.372(8) . ? N4 C2 1.475(9) . ? C5 N1 1.462(10) . ? C5 C4 1.515(11) . ? C4 C2 1.512(11) . ? N3 C3 1.321(8) . ? N3 C7 1.352(9) . ? N1 C1 1.316(9) . ? N6 C7 1.312(9) . ? N6 Cu1 1.946(6) 2_654 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O8 Mo1 O6 103.7(2) . . ? O8 Mo1 O1 95.4(2) . . ? O6 Mo1 O1 100.0(2) . . ? O8 Mo1 O2 100.4(2) . 2_565 ? O6 Mo1 O2 89.4(2) . 2_565 ? O1 Mo1 O2 159.2(2) . 2_565 ? O8 Mo1 O3 96.3(2) . . ? O6 Mo1 O3 155.96(19) . . ? O1 Mo1 O3 91.18(17) . . ? O2 Mo1 O3 73.78(17) 2_565 . ? O8 Mo1 O3 165.2(2) . 2_565 ? O6 Mo1 O3 88.7(2) . 2_565 ? O1 Mo1 O3 74.29(17) . 2_565 ? O2 Mo1 O3 87.54(17) 2_565 2_565 ? O3 Mo1 O3 73.8(2) . 2_565 ? O7 Mo2 O9 103.6(2) . . ? O7 Mo2 O2 100.1(2) . . ? O9 Mo2 O2 93.6(2) . . ? O7 Mo2 O1 92.6(2) . 2_465 ? O9 Mo2 O1 100.25(19) . 2_465 ? O2 Mo2 O1 158.45(19) . 2_465 ? O7 Mo2 O4 98.8(2) . . ? O9 Mo2 O4 156.2(2) . . ? O2 Mo2 O4 74.69(17) . . ? O1 Mo2 O4 86.31(16) 2_465 . ? O7 Mo2 O4 164.36(19) . 2_465 ? O9 Mo2 O4 86.2(2) . 2_465 ? O2 Mo2 O4 91.17(18) . 2_465 ? O1 Mo2 O4 73.49(17) 2_465 2_465 ? O4 Mo2 O4 73.68(19) . 2_465 ? O5 Mo3 O10 103.7(2) . 1_456 ? O5 Mo3 O3 104.7(2) . 2_565 ? O10 Mo3 O3 101.5(2) 1_456 2_565 ? O5 Mo3 O4 102.6(2) . . ? O10 Mo3 O4 102.5(2) 1_456 . ? O3 Mo3 O4 137.9(2) 2_565 . ? O5 Mo3 O2 93.1(2) . . ? O10 Mo3 O2 163.2(2) 1_456 . ? O3 Mo3 O2 73.38(17) 2_565 . ? O4 Mo3 O2 73.59(16) . . ? O5 Mo3 O1 171.6(2) . . ? O10 Mo3 O1 84.6(2) 1_456 . ? O3 Mo3 O1 74.44(17) 2_565 . ? O4 Mo3 O1 73.97(17) . . ? O2 Mo3 O1 78.56(16) . . ? N3 Cu2 N2 144.2(3) . 2_655 ? N3 Cu2 O6 104.0(2) . . ? N2 Cu2 O6 100.5(2) 2_655 . ? N3 Cu2 O9 108.7(2) . 2_565 ? N2 Cu2 O9 95.0(2) 2_655 2_565 ? O6 Cu2 O9 94.30(19) . 2_565 ? N5 Cu1 N6 145.1(2) . 2_654 ? N5 Cu1 O10 122.1(2) . . ? N6 Cu1 O10 91.2(2) 2_654 . ? Mo3 O10 Cu1 155.1(3) 1_654 . ? Mo2 O9 Cu2 136.3(2) . 2_565 ? Mo1 O6 Cu2 140.6(2) . . ? Mo3 O4 Mo2 105.22(17) . . ? Mo3 O4 Mo2 103.80(19) . 2_465 ? Mo2 O4 Mo2 106.32(19) . 2_465 ? Mo3 O3 Mo1 106.2(2) 2_565 . ? Mo3 O3 Mo1 103.79(18) 2_565 2_565 ? Mo1 O3 Mo1 106.2(2) . 2_565 ? Mo2 O2 Mo1 154.0(3) . 2_565 ? Mo2 O2 Mo3 103.67(19) . . ? Mo1 O2 Mo3 102.00(18) 2_565 . ? Mo1 O1 Mo2 152.0(3) . 2_465 ? Mo1 O1 Mo3 103.94(18) . . ? Mo2 O1 Mo3 103.1(2) 2_465 . ? C6 N2 N1 103.5(5) . . ? C6 N2 Cu2 127.5(5) . 2_655 ? N1 N2 Cu2 127.4(5) . 2_655 ? C1 N5 C6 102.6(6) . . ? C1 N5 Cu1 127.2(5) . . ? C6 N5 Cu1 130.2(5) . . ? C3 N4 N6 108.9(5) . . ? C3 N4 C2 129.7(6) . . ? N6 N4 C2 120.9(6) . . ? N1 C5 C4 111.8(7) . . ? C2 C4 C5 115.1(6) . . ? C3 N3 C7 103.7(6) . . ? C3 N3 Cu2 126.4(5) . . ? C7 N3 Cu2 129.1(5) . . ? C1 N1 N2 108.2(6) . . ? C1 N1 C5 130.8(6) . . ? N2 N1 C5 120.8(6) . . ? N3 C3 N4 110.2(6) . . ? N1 C1 N5 111.7(6) . . ? N4 C2 C4 112.9(6) . . ? N2 C6 N5 114.1(6) . . ? C7 N6 N4 103.1(6) . . ? C7 N6 Cu1 127.0(5) . 2_654 ? N4 N6 Cu1 129.0(4) . 2_654 ? N6 C7 N3 114.2(6) . . ? _diffrn_measured_fraction_theta_max 0.835 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 1.856 _refine_diff_density_min -1.468 _refine_diff_density_rms 0.201 # Attachment 'compound_3.cif' data_compound3 _database_code_depnum_ccdc_archive 'CCDC 757939' #TrackingRef 'compound_3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C9 H14 Cu Mo4 N9 O14' _chemical_formula_weight 919.56 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 8.2120(14) _cell_length_b 10.6380(18) _cell_length_c 13.506(2) _cell_angle_alpha 97.538(2) _cell_angle_beta 90.294(2) _cell_angle_gamma 108.6110(19) _cell_volume 1107.1(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 7.5 _cell_measurement_theta_max 15 _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max 0.1124 _exptl_crystal_size_mid 0.1116 _exptl_crystal_size_min 0.1101 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.753 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 876.0 _exptl_absorpt_coefficient_mu 3.238 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.700 _exptl_absorpt_correction_T_max 0.702 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _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 2 _diffrn_standards_interval_count 150 _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 5946 _diffrn_reflns_av_R_equivalents 0.0221 _diffrn_reflns_av_sigmaI/netI 0.0474 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.52 _diffrn_reflns_theta_max 25.75 _reflns_number_total 4225 _reflns_number_gt 3309 _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^)+(0.0472P)^2^+2.7018P] 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 refall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4225 _refine_ls_number_parameters 337 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0489 _refine_ls_R_factor_gt 0.0356 _refine_ls_wR_factor_ref 0.0993 _refine_ls_wR_factor_gt 0.0826 _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_restrained_S_all 1.053 _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 0.55046(7) 0.37446(5) 0.05634(4) 0.00995(14) Uani 1 1 d . . . Mo2 Mo 0.96238(7) 0.59448(5) 0.21890(4) 0.01113(14) Uani 1 1 d . . . Mo3 Mo 0.16428(7) 0.38725(5) 0.05243(4) 0.00987(14) Uani 1 1 d . . . Mo4 Mo 0.56800(7) 0.61142(6) 0.22335(4) 0.01401(15) Uani 1 1 d . . . Cu2 Cu 1.0000 0.5000 0.5000 0.0168(3) Uani 1 2 d S . . Cu1 Cu 0.5000 0.0000 0.0000 0.0162(3) Uani 1 2 d S . . N9 N 1.4684(8) 0.7839(6) 0.5895(5) 0.0295(15) Uani 1 1 d . . . C9 C 1.5317(10) 0.9473(7) 0.4722(6) 0.0258(17) Uani 1 1 d . . . H9A H 1.5164 0.9458 0.4007 0.031 Uiso 1 1 calc R . . H9B H 1.6533 0.9673 0.4885 0.031 Uiso 1 1 calc R . . N8 N 0.6758(7) 0.0278(5) 0.1064(4) 0.0191(13) Uani 1 1 d . . . N7 N 1.1565(7) 0.1948(5) 0.3541(4) 0.0162(12) Uani 1 1 d . . . N6 N 0.8786(7) 0.0131(6) 0.2015(4) 0.0202(13) Uani 1 1 d . . . C8 C 1.1834(9) 0.1066(7) 0.2676(5) 0.0217(15) Uani 1 1 d . . . H8A H 1.2812 0.0787 0.2826 0.026 Uiso 1 1 calc R . . H8B H 1.2102 0.1560 0.2111 0.026 Uiso 1 1 calc R . . O1W O 0.6777(7) 0.1104(5) -0.0910(4) 0.0262(12) Uani 1 1 d . . . O1 O 0.8123(6) 0.7012(4) 0.2381(3) 0.0162(10) Uani 1 1 d . . . O2 O 0.4764(6) 0.2075(4) 0.0686(3) 0.0172(10) Uani 1 1 d . . . O3 O 1.0432(6) 0.4530(4) 0.1492(3) 0.0176(10) Uani 1 1 d . . . O4 O 0.3736(5) 0.3873(4) -0.0368(3) 0.0131(9) Uani 1 1 d . . . O5 O 1.1478(6) 0.7266(5) 0.2352(4) 0.0203(11) Uani 1 1 d . . . O6 O 0.3879(5) 0.4553(4) 0.1479(3) 0.0138(9) Uani 1 1 d . . . O7 O 0.5011(6) 0.7454(5) 0.2093(4) 0.0248(11) Uani 1 1 d . . . O8 O 0.1109(6) 0.2251(4) 0.0734(3) 0.0184(10) Uani 1 1 d . . . O9 O 0.9515(6) 0.5370(4) 0.3326(3) 0.0160(10) Uani 1 1 d . . . O10 O 0.7121(5) 0.3916(4) -0.0280(3) 0.0141(10) Uani 1 1 d . . . O11 O 0.6917(5) 0.4585(4) 0.1714(3) 0.0120(9) Uani 1 1 d . . . O12 O 0.5219(7) 0.5804(5) 0.3408(4) 0.0269(12) Uani 1 1 d . . . O13 O 0.9521(5) 0.6282(5) 0.0598(3) 0.0175(10) Uani 1 1 d . . . C7 C 0.8032(9) -0.0224(7) 0.1120(6) 0.0244(16) Uani 1 1 d . . . H7A H 0.8345 -0.0751 0.0600 0.029 Uiso 1 1 calc R . . N5 N 1.4355(8) 0.8179(6) 0.5000(4) 0.0224(13) Uani 1 1 d . . . C6 C 1.1287(9) 0.3099(7) 0.3569(5) 0.0211(15) Uani 1 1 d . . . H6A H 1.1334 0.3567 0.3029 0.025 Uiso 1 1 calc R . . N4 N 1.2346(7) 0.6324(6) 0.5115(4) 0.0215(13) Uani 1 1 d . . . N3 N 1.0917(8) 0.3497(6) 0.4519(4) 0.0199(13) Uani 1 1 d . . . C5 C 1.0273(9) -0.0165(7) 0.2394(6) 0.0259(17) Uani 1 1 d . . . H5A H 1.0578 -0.0775 0.1888 0.031 Uiso 1 1 calc R . . H5B H 0.9955 -0.0616 0.2977 0.031 Uiso 1 1 calc R . . C4 C 1.1021(10) 0.2474(7) 0.5001(6) 0.0271(17) Uani 1 1 d U . . H4A H 1.0848 0.2460 0.5680 0.033 Uiso 1 1 calc R . . N2 N 0.8014(9) 0.0891(7) 0.2624(5) 0.0368(17) Uani 1 1 d . . . C3 C 1.3440(9) 0.6724(8) 0.5934(6) 0.0287(18) Uani 1 1 d . . . H3A H 1.3315 0.6247 0.6474 0.034 Uiso 1 1 calc R . . C2 C 1.2989(9) 0.7260(7) 0.4541(5) 0.0229(16) Uani 1 1 d . . . H2A H 1.2544 0.7268 0.3908 0.028 Uiso 1 1 calc R . . C1 C 0.6816(11) 0.0950(8) 0.1983(6) 0.036(2) Uani 1 1 d . . . H1A H 0.6066 0.1428 0.2160 0.043 Uiso 1 1 calc R . . N1 N 1.1392(9) 0.1495(6) 0.4419(5) 0.0300(15) 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 0.0094(3) 0.0107(3) 0.0107(3) 0.0017(2) 0.0005(2) 0.0045(2) Mo2 0.0111(3) 0.0148(3) 0.0082(3) 0.0010(2) 0.0005(2) 0.0053(2) Mo3 0.0095(3) 0.0127(3) 0.0082(3) 0.0018(2) 0.0012(2) 0.0045(2) Mo4 0.0117(3) 0.0162(3) 0.0140(3) -0.0022(2) 0.0004(2) 0.0060(2) Cu2 0.0165(6) 0.0136(6) 0.0183(6) -0.0009(5) 0.0006(5) 0.0034(5) Cu1 0.0166(6) 0.0185(6) 0.0131(6) 0.0017(5) -0.0011(5) 0.0053(5) N9 0.023(3) 0.033(4) 0.027(4) 0.012(3) -0.007(3) -0.001(3) C9 0.028(4) 0.022(4) 0.021(4) 0.008(3) 0.008(3) -0.002(3) N8 0.022(3) 0.018(3) 0.016(3) 0.000(2) -0.005(2) 0.005(2) N7 0.020(3) 0.018(3) 0.012(3) -0.001(2) 0.003(2) 0.009(2) N6 0.023(3) 0.022(3) 0.016(3) -0.005(2) -0.004(2) 0.011(3) C8 0.021(4) 0.026(4) 0.020(4) -0.001(3) 0.001(3) 0.012(3) O1W 0.033(3) 0.020(3) 0.023(3) 0.002(2) 0.012(2) 0.007(2) O1 0.013(2) 0.017(2) 0.018(3) -0.0043(19) 0.0009(18) 0.0059(19) O2 0.019(2) 0.016(2) 0.018(3) 0.0032(19) 0.003(2) 0.007(2) O3 0.014(2) 0.021(3) 0.020(3) 0.008(2) 0.0022(19) 0.007(2) O4 0.012(2) 0.017(2) 0.012(2) 0.0007(18) -0.0010(18) 0.0079(19) O5 0.011(2) 0.022(3) 0.028(3) 0.007(2) -0.003(2) 0.004(2) O6 0.014(2) 0.011(2) 0.016(2) 0.0033(18) -0.0009(18) 0.0030(18) O7 0.022(3) 0.024(3) 0.030(3) -0.005(2) -0.002(2) 0.013(2) O8 0.019(3) 0.020(3) 0.017(3) 0.004(2) 0.0040(19) 0.006(2) O9 0.016(2) 0.020(2) 0.010(2) -0.0006(18) 0.0044(18) 0.0038(19) O10 0.015(2) 0.012(2) 0.017(3) 0.0024(18) 0.0000(18) 0.0063(19) O11 0.013(2) 0.017(2) 0.007(2) 0.0006(17) 0.0002(17) 0.0064(18) O12 0.031(3) 0.037(3) 0.012(3) -0.003(2) 0.007(2) 0.012(2) O13 0.012(2) 0.024(3) 0.017(3) 0.007(2) -0.0025(19) 0.005(2) C7 0.022(4) 0.020(4) 0.026(4) -0.008(3) -0.002(3) 0.005(3) N5 0.026(3) 0.019(3) 0.020(3) 0.004(2) 0.001(3) 0.003(3) C6 0.027(4) 0.019(4) 0.019(4) 0.005(3) 0.004(3) 0.009(3) N4 0.022(3) 0.018(3) 0.021(3) 0.001(2) -0.001(2) 0.002(3) N3 0.027(3) 0.021(3) 0.013(3) -0.004(2) 0.005(2) 0.012(3) C5 0.023(4) 0.017(4) 0.037(5) -0.002(3) -0.009(3) 0.008(3) C4 0.0281(19) 0.0273(19) 0.0266(19) 0.0032(10) 0.0026(10) 0.0099(11) N2 0.032(4) 0.051(5) 0.032(4) -0.005(3) -0.011(3) 0.025(4) C3 0.018(4) 0.031(4) 0.033(5) 0.012(3) -0.005(3) -0.001(3) C2 0.023(4) 0.023(4) 0.020(4) 0.005(3) -0.005(3) 0.003(3) C1 0.037(5) 0.044(5) 0.033(5) -0.009(4) -0.013(4) 0.027(4) N1 0.042(4) 0.034(4) 0.021(4) 0.006(3) 0.004(3) 0.022(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 O2 1.715(4) . ? Mo1 O10 1.734(4) . ? Mo1 O11 1.875(4) . ? Mo1 O4 1.966(4) . ? Mo1 O6 2.126(4) . ? Mo1 O4 2.460(4) 2_665 ? Mo1 Mo4 3.1201(9) . ? Mo1 Mo3 3.2178(9) . ? Mo2 O5 1.701(5) . ? Mo2 O9 1.719(4) . ? Mo2 O1 1.922(4) . ? Mo2 O3 1.966(4) . ? Mo2 O13 2.229(4) . ? Mo2 O11 2.266(4) . ? Mo3 O8 1.701(4) . ? Mo3 O13 1.749(4) 2_665 ? Mo3 O3 1.844(4) 1_455 ? Mo3 O4 2.104(4) . ? Mo3 O6 2.107(4) . ? Mo3 O10 2.314(4) 2_665 ? Mo4 O12 1.683(5) . ? Mo4 O7 1.714(5) . ? Mo4 O1 1.923(4) . ? Mo4 O6 1.989(4) . ? Mo4 O11 2.221(4) . ? Cu2 N4 1.982(6) . ? Cu2 N4 1.982(6) 2_766 ? Cu2 N3 2.011(5) . ? Cu2 N3 2.011(5) 2_766 ? Cu2 O9 2.398(4) 2_766 ? Cu2 O9 2.398(4) . ? Cu1 N8 1.958(6) . ? Cu1 N8 1.958(6) 2_655 ? Cu1 O1W 2.079(5) 2_655 ? Cu1 O1W 2.079(5) . ? Cu1 O2 2.347(4) 2_655 ? Cu1 O2 2.347(4) . ? N9 C3 1.303(9) . ? N9 N5 1.356(8) . ? C9 N5 1.451(8) . ? C9 C9 1.499(14) 2_876 ? N8 C7 1.323(9) . ? N8 C1 1.341(10) . ? N7 C6 1.311(8) . ? N7 N1 1.330(8) . ? N7 C8 1.463(8) . ? N6 C7 1.308(9) . ? N6 N2 1.375(8) . ? N6 C5 1.461(8) . ? C8 C5 1.515(10) . ? O3 Mo3 1.844(4) 1_655 ? O4 Mo1 2.460(4) 2_665 ? O10 Mo3 2.314(4) 2_665 ? O13 Mo3 1.749(4) 2_665 ? N5 C2 1.316(9) . ? C6 N3 1.364(9) . ? N4 C2 1.320(9) . ? N4 C3 1.353(9) . ? N3 C4 1.364(9) . ? C4 N1 1.336(9) . ? N2 C1 1.329(10) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Mo1 O10 105.7(2) . . ? O2 Mo1 O11 105.5(2) . . ? O10 Mo1 O11 97.46(19) . . ? O2 Mo1 O4 101.3(2) . . ? O10 Mo1 O4 96.60(19) . . ? O11 Mo1 O4 144.90(18) . . ? O2 Mo1 O6 103.11(19) . . ? O10 Mo1 O6 151.07(17) . . ? O11 Mo1 O6 77.14(17) . . ? O4 Mo1 O6 75.05(17) . . ? O2 Mo1 O4 174.28(18) . 2_665 ? O10 Mo1 O4 78.21(17) . 2_665 ? O11 Mo1 O4 77.79(16) . 2_665 ? O4 Mo1 O4 73.86(18) . 2_665 ? O6 Mo1 O4 72.86(15) . 2_665 ? O2 Mo1 Mo4 125.99(15) . . ? O10 Mo1 Mo4 119.77(14) . . ? O11 Mo1 Mo4 44.68(12) . . ? O4 Mo1 Mo4 100.78(12) . . ? O6 Mo1 Mo4 39.09(12) . . ? O4 Mo1 Mo4 53.22(10) 2_665 . ? O2 Mo1 Mo3 91.10(15) . . ? O10 Mo1 Mo3 135.68(14) . . ? O11 Mo1 Mo3 117.44(13) . . ? O4 Mo1 Mo3 39.29(12) . . ? O6 Mo1 Mo3 40.31(12) . . ? O4 Mo1 Mo3 83.21(10) 2_665 . ? Mo4 Mo1 Mo3 76.606(18) . . ? O5 Mo2 O9 101.8(2) . . ? O5 Mo2 O1 95.3(2) . . ? O9 Mo2 O1 100.3(2) . . ? O5 Mo2 O3 101.3(2) . . ? O9 Mo2 O3 94.68(19) . . ? O1 Mo2 O3 154.79(19) . . ? O5 Mo2 O13 87.4(2) . . ? O9 Mo2 O13 169.08(19) . . ? O1 Mo2 O13 84.37(18) . . ? O3 Mo2 O13 77.64(17) . . ? O5 Mo2 O11 163.31(19) . . ? O9 Mo2 O11 91.76(18) . . ? O1 Mo2 O11 72.48(17) . . ? O3 Mo2 O11 87.04(17) . . ? O13 Mo2 O11 80.19(16) . . ? O8 Mo3 O13 101.9(2) . 2_665 ? O8 Mo3 O3 100.6(2) . 1_455 ? O13 Mo3 O3 104.7(2) 2_665 1_455 ? O8 Mo3 O4 96.86(19) . . ? O13 Mo3 O4 86.01(18) 2_665 . ? O3 Mo3 O4 157.05(18) 1_455 . ? O8 Mo3 O6 94.99(19) . . ? O13 Mo3 O6 154.24(19) 2_665 . ? O3 Mo3 O6 90.93(18) 1_455 . ? O4 Mo3 O6 72.68(17) . . ? O8 Mo3 O10 169.59(19) . 2_665 ? O13 Mo3 O10 84.60(18) 2_665 2_665 ? O3 Mo3 O10 85.39(17) 1_455 2_665 ? O4 Mo3 O10 75.32(16) . 2_665 ? O6 Mo3 O10 76.25(15) . 2_665 ? O8 Mo3 Mo1 83.74(15) . . ? O13 Mo3 Mo1 121.80(15) 2_665 . ? O3 Mo3 Mo1 131.49(14) 1_455 . ? O4 Mo3 Mo1 36.27(11) . . ? O6 Mo3 Mo1 40.74(12) . . ? O10 Mo3 Mo1 85.92(10) 2_665 . ? O12 Mo4 O7 105.0(2) . . ? O12 Mo4 O1 101.4(2) . . ? O7 Mo4 O1 99.3(2) . . ? O12 Mo4 O6 99.5(2) . . ? O7 Mo4 O6 104.2(2) . . ? O1 Mo4 O6 143.08(18) . . ? O12 Mo4 O11 101.6(2) . . ? O7 Mo4 O11 153.3(2) . . ? O1 Mo4 O11 73.51(17) . . ? O6 Mo4 O11 72.68(16) . . ? O12 Mo4 Mo1 119.54(18) . . ? O7 Mo4 Mo1 125.55(17) . . ? O1 Mo4 Mo1 100.72(13) . . ? O6 Mo4 Mo1 42.36(12) . . ? O11 Mo4 Mo1 36.41(11) . . ? N4 Cu2 N4 180.0 . 2_766 ? N4 Cu2 N3 91.4(2) . . ? N4 Cu2 N3 88.6(2) 2_766 . ? N4 Cu2 N3 88.6(2) . 2_766 ? N4 Cu2 N3 91.4(2) 2_766 2_766 ? N3 Cu2 N3 180.000(2) . 2_766 ? N4 Cu2 O9 87.6(2) . 2_766 ? N4 Cu2 O9 92.4(2) 2_766 2_766 ? N3 Cu2 O9 87.73(19) . 2_766 ? N3 Cu2 O9 92.27(19) 2_766 2_766 ? N4 Cu2 O9 92.4(2) . . ? N4 Cu2 O9 87.6(2) 2_766 . ? N3 Cu2 O9 92.27(19) . . ? N3 Cu2 O9 87.73(19) 2_766 . ? O9 Cu2 O9 180.000(1) 2_766 . ? N8 Cu1 N8 180.0(3) . 2_655 ? N8 Cu1 O1W 87.7(2) . 2_655 ? N8 Cu1 O1W 92.3(2) 2_655 2_655 ? N8 Cu1 O1W 92.3(2) . . ? N8 Cu1 O1W 87.7(2) 2_655 . ? O1W Cu1 O1W 180.0(2) 2_655 . ? N8 Cu1 O2 93.09(19) . 2_655 ? N8 Cu1 O2 86.91(19) 2_655 2_655 ? O1W Cu1 O2 85.04(17) 2_655 2_655 ? O1W Cu1 O2 94.96(17) . 2_655 ? N8 Cu1 O2 86.91(19) . . ? N8 Cu1 O2 93.09(19) 2_655 . ? O1W Cu1 O2 94.96(17) 2_655 . ? O1W Cu1 O2 85.04(17) . . ? O2 Cu1 O2 180.0(2) 2_655 . ? C3 N9 N5 103.0(6) . . ? N5 C9 C9 109.1(7) . 2_876 ? C7 N8 C1 102.9(6) . . ? C7 N8 Cu1 131.0(5) . . ? C1 N8 Cu1 125.8(5) . . ? C6 N7 N1 112.9(5) . . ? C6 N7 C8 129.0(6) . . ? N1 N7 C8 117.7(5) . . ? C7 N6 N2 111.4(6) . . ? C7 N6 C5 128.4(6) . . ? N2 N6 C5 120.2(6) . . ? N7 C8 C5 112.4(6) . . ? Mo2 O1 Mo4 118.3(2) . . ? Mo1 O2 Cu1 141.8(2) . . ? Mo3 O3 Mo2 153.1(3) 1_655 . ? Mo1 O4 Mo3 104.44(19) . . ? Mo1 O4 Mo1 106.14(18) . 2_665 ? Mo3 O4 Mo1 94.52(15) . 2_665 ? Mo4 O6 Mo3 147.1(2) . . ? Mo4 O6 Mo1 98.55(18) . . ? Mo3 O6 Mo1 98.95(18) . . ? Mo2 O9 Cu2 166.2(2) . . ? Mo1 O10 Mo3 111.4(2) . 2_665 ? Mo1 O11 Mo4 98.91(18) . . ? Mo1 O11 Mo2 141.1(2) . . ? Mo4 O11 Mo2 94.73(16) . . ? Mo3 O13 Mo2 150.6(2) 2_665 . ? N6 C7 N8 110.0(6) . . ? C2 N5 N9 110.0(6) . . ? C2 N5 C9 128.8(6) . . ? N9 N5 C9 120.7(6) . . ? N7 C6 N3 108.9(6) . . ? C2 N4 C3 103.5(6) . . ? C2 N4 Cu2 127.1(5) . . ? C3 N4 Cu2 126.9(5) . . ? C4 N3 C6 101.7(6) . . ? C4 N3 Cu2 129.0(5) . . ? C6 N3 Cu2 128.2(5) . . ? N6 C5 C8 113.7(6) . . ? N1 C4 N3 114.6(7) . . ? C1 N2 N6 99.9(6) . . ? N9 C3 N4 113.8(7) . . ? N5 C2 N4 109.7(6) . . ? N2 C1 N8 115.8(7) . . ? N7 N1 C4 101.8(6) . . ? _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 25.75 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 0.733 _refine_diff_density_min -1.018 _refine_diff_density_rms 0.190 # Attachment 'compound_4.cif' data_compound4 _database_code_depnum_ccdc_archive 'CCDC 757940' #TrackingRef 'compound_4.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C14 H26 Cu Mo4 N12 O16' _chemical_formula_weight 1065.78 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 11.6710(12) _cell_length_b 11.7000(12) _cell_length_c 11.9010(12) _cell_angle_alpha 71.1380(12) _cell_angle_beta 77.1160(12) _cell_angle_gamma 85.8450(14) _cell_volume 1499.1(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 7.5 _cell_measurement_theta_max 15 _exptl_crystal_description rhombus _exptl_crystal_colour blue _exptl_crystal_size_max 0.1121 _exptl_crystal_size_mid 0.1116 _exptl_crystal_size_min 0.1111 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.361 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1038.0 _exptl_absorpt_coefficient_mu 2.416 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.765 _exptl_absorpt_correction_T_max 0.770 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _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 2 _diffrn_standards_interval_count 150 _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 8055 _diffrn_reflns_av_R_equivalents 0.0180 _diffrn_reflns_av_sigmaI/netI 0.0410 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.84 _diffrn_reflns_theta_max 25.75 _reflns_number_total 5737 _reflns_number_gt 4298 _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^)+(0.0357P)^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 refall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5737 _refine_ls_number_parameters 425 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0501 _refine_ls_R_factor_gt 0.0325 _refine_ls_wR_factor_ref 0.0760 _refine_ls_wR_factor_gt 0.0704 _refine_ls_goodness_of_fit_ref 1.004 _refine_ls_restrained_S_all 1.004 _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 0.46078(3) 0.50438(3) 0.36226(3) 0.02701(10) Uani 1 1 d . . . Mo2 Mo 0.70225(3) 0.69181(4) 0.25069(4) 0.03293(11) Uani 1 1 d . . . Mo3 Mo 0.25957(3) 0.57487(4) 0.56420(3) 0.03014(11) Uani 1 1 d . . . Mo4 Mo 0.49935(3) 0.76043(4) 0.45353(4) 0.03198(11) Uani 1 1 d . . . Cu1 Cu 0.75421(4) 0.79283(5) -0.11821(5) 0.03153(14) Uani 1 1 d . . . O1 O 0.3579(3) 0.4487(3) 0.3153(3) 0.0440(8) Uani 1 1 d . . . O2 O 0.5503(3) 0.5948(3) 0.2291(3) 0.0340(7) Uani 1 1 d . . . O2W O 0.0583(6) 0.2907(5) 0.5043(5) 0.142(2) Uani 1 1 d . . . H2WA H 0.0940 0.2777 0.5610 0.170 Uiso 1 1 d R . . H2WB H 0.0159 0.2247 0.5222 0.170 Uiso 1 1 d R . . O3 O 0.5725(3) 0.7932(3) 0.2871(3) 0.0361(7) Uani 1 1 d . . . O1W O 0.7766(4) 0.8643(4) -0.3533(3) 0.0764(13) Uani 1 1 d . . . H1WA H 0.8156 0.9303 -0.3905 0.092 Uiso 1 1 d R . . H1WB H 0.7327 0.8591 -0.4010 0.092 Uiso 1 1 d R . . O4 O 0.5983(2) 0.5764(3) 0.4450(2) 0.0278(7) Uani 1 1 d . . . O5 O 0.3751(2) 0.6382(3) 0.4094(2) 0.0294(7) Uani 1 1 d . . . O6 O 0.7436(3) 0.7493(3) 0.0959(3) 0.0449(9) Uani 1 1 d . . . O7 O 0.4303(2) 0.6318(3) 0.6055(2) 0.0298(7) Uani 1 1 d . . . O8 O 0.8027(3) 0.7448(3) 0.3048(3) 0.0457(9) Uani 1 1 d . . . O9 O 0.7624(2) 0.5296(3) 0.2744(3) 0.0332(7) Uani 1 1 d . . . O11 O 0.3942(3) 0.8684(3) 0.4460(3) 0.0515(9) Uani 1 1 d . . . O12 O 0.1608(3) 0.5191(3) 0.5097(3) 0.0463(9) Uani 1 1 d . . . O13 O 0.1962(3) 0.7040(3) 0.5854(3) 0.0445(8) Uani 1 1 d . . . O14 O 0.6030(3) 0.8078(3) 0.5081(3) 0.0480(9) Uani 1 1 d . . . N1 N 0.6535(4) 1.1043(4) -0.0281(4) 0.0477(11) Uani 1 1 d . . . N2 N 0.7174(3) 1.1500(3) -0.1433(4) 0.0345(9) Uani 1 1 d . . . N3 N 0.6986(3) 0.9595(3) -0.1162(3) 0.0340(9) Uani 1 1 d . . . C13 C -0.0388(4) 0.9120(5) -0.0835(4) 0.0389(12) Uani 1 1 d . . . H13B H -0.0819 0.9222 -0.0116 0.047 Uiso 1 1 calc R . . N5 N 0.8133(3) 0.6263(3) -0.1076(4) 0.0335(9) Uani 1 1 d . . . N6 N 0.8864(4) 0.4400(4) -0.0403(4) 0.0472(11) Uani 1 1 d . . . N7 N 0.0945(3) 0.9197(3) -0.2352(3) 0.0308(8) Uani 1 1 d . . . N8 N 0.5935(3) 0.7484(3) -0.1142(3) 0.0327(9) Uani 1 1 d . . . N9 N 0.4220(3) 0.7523(3) -0.1585(3) 0.0282(8) Uani 1 1 d . . . N10 N 0.8912(3) 0.4738(3) -0.1611(4) 0.0350(9) Uani 1 1 d . . . N11 N -0.0801(3) 0.8499(3) -0.1455(3) 0.0307(8) Uani 1 1 d . . . N12 N 0.4276(3) 0.6440(3) -0.0703(4) 0.0410(10) Uani 1 1 d . . . C1 C 0.5327(4) 0.6470(4) -0.0489(5) 0.0390(12) Uani 1 1 d . . . H1A H 0.5627 0.5836 0.0073 0.047 Uiso 1 1 calc R . . C2 C 0.6432(4) 0.9899(4) -0.0161(5) 0.0438(12) Uani 1 1 d . . . H2A H 0.6020 0.9346 0.0541 0.053 Uiso 1 1 calc R . . C3 C 0.7640(4) 0.2731(4) -0.1904(4) 0.0386(12) Uani 1 1 d . . . H3A H 0.7184 0.3221 -0.1443 0.046 Uiso 1 1 calc R . . H3B H 0.7581 0.3088 -0.2747 0.046 Uiso 1 1 calc R . . C4 C 0.5200(4) 0.8130(4) -0.1823(4) 0.0343(11) Uani 1 1 d . . . H4A H 0.5358 0.8897 -0.2383 0.041 Uiso 1 1 calc R . . C5 C 0.9449(4) 0.3955(4) -0.2329(5) 0.0464(13) Uani 1 1 d . . . H5A H 1.0285 0.3886 -0.2343 0.056 Uiso 1 1 calc R . . H5B H 0.9350 0.4316 -0.3159 0.056 Uiso 1 1 calc R . . C6 C 0.2043(4) 0.9577(4) -0.3245(4) 0.0360(11) Uani 1 1 d . . . H6A H 0.2037 1.0449 -0.3603 0.043 Uiso 1 1 calc R . . H6B H 0.2087 0.9228 -0.3890 0.043 Uiso 1 1 calc R . . C7 C 0.8376(4) 0.5344(4) -0.0115(5) 0.0423(12) Uani 1 1 d . . . H7A H 0.8211 0.5380 0.0674 0.051 Uiso 1 1 calc R . . C8 C 0.8902(4) 0.2710(4) -0.1807(4) 0.0371(11) Uani 1 1 d . . . H8A H 0.9344 0.2186 -0.2235 0.045 Uiso 1 1 calc R . . H8B H 0.8950 0.2377 -0.0959 0.045 Uiso 1 1 calc R . . C9 C 0.8476(4) 0.5828(4) -0.2000(4) 0.0371(11) Uani 1 1 d . . . H9A H 0.8417 0.6232 -0.2798 0.045 Uiso 1 1 calc R . . C10 C 0.7427(4) 1.0639(4) -0.1936(5) 0.0395(12) Uani 1 1 d . . . H10A H 0.7855 1.0747 -0.2722 0.047 Uiso 1 1 calc R . . C11 C 0.3123(3) 0.9210(4) -0.2707(4) 0.0327(11) Uani 1 1 d . . . H11A H 0.3820 0.9429 -0.3352 0.039 Uiso 1 1 calc R . . H11B H 0.3140 0.9650 -0.2146 0.039 Uiso 1 1 calc R . . C12 C 0.3149(4) 0.7870(4) -0.2045(4) 0.0333(10) Uani 1 1 d . . . H12A H 0.2474 0.7656 -0.1373 0.040 Uiso 1 1 calc R . . H12B H 0.3096 0.7427 -0.2594 0.040 Uiso 1 1 calc R . . N4 N 0.0666(3) 0.9556(4) -0.1344(4) 0.0409(10) Uani 1 1 d . . . C14 C 0.0078(4) 0.8571(4) -0.2392(4) 0.0333(11) Uani 1 1 d . . . H14A H 0.0081 0.8226 -0.2995 0.040 Uiso 1 1 calc R . . O3W O 0.9332(6) 1.0860(7) -0.4474(5) 0.157(3) Uani 1 1 d . . . H3WA H 0.9873 1.1368 -0.4518 0.189 Uiso 1 1 d R . . H3WB H 0.8835 1.1309 -0.4858 0.189 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 0.0273(2) 0.0301(2) 0.0245(2) -0.00949(17) -0.00579(16) -0.00072(17) Mo2 0.0312(2) 0.0298(2) 0.0306(2) -0.00572(18) 0.00333(17) -0.00352(18) Mo3 0.0248(2) 0.0331(2) 0.0294(2) -0.00747(18) -0.00292(17) -0.00036(17) Mo4 0.0348(2) 0.0257(2) 0.0324(2) -0.00956(18) 0.00099(18) -0.00374(18) Cu1 0.0229(3) 0.0259(3) 0.0473(4) -0.0135(3) -0.0072(2) -0.0009(2) O1 0.0387(19) 0.054(2) 0.048(2) -0.0232(18) -0.0160(16) -0.0021(17) O2 0.0356(17) 0.0372(18) 0.0266(16) -0.0079(14) -0.0041(14) -0.0015(15) O2W 0.230(7) 0.121(5) 0.096(4) -0.039(4) -0.059(5) -0.031(5) O3 0.0343(17) 0.0307(17) 0.0353(18) -0.0054(14) 0.0017(14) -0.0015(14) O1W 0.069(3) 0.105(4) 0.055(3) -0.018(3) -0.016(2) -0.022(3) O4 0.0272(16) 0.0296(17) 0.0257(16) -0.0087(13) -0.0033(13) -0.0015(13) O5 0.0287(16) 0.0292(17) 0.0276(16) -0.0064(13) -0.0047(13) 0.0013(13) O6 0.045(2) 0.040(2) 0.0355(19) -0.0055(16) 0.0104(16) -0.0029(17) O7 0.0307(16) 0.0309(17) 0.0286(16) -0.0130(14) -0.0030(13) 0.0007(14) O8 0.0384(19) 0.041(2) 0.056(2) -0.0162(18) -0.0016(17) -0.0097(16) O9 0.0305(16) 0.0346(18) 0.0309(17) -0.0108(14) 0.0016(13) -0.0005(14) O11 0.056(2) 0.037(2) 0.054(2) -0.0147(18) 0.0013(18) 0.0082(18) O12 0.0348(18) 0.062(2) 0.043(2) -0.0166(18) -0.0073(16) -0.0065(18) O13 0.0394(19) 0.040(2) 0.048(2) -0.0121(17) -0.0039(16) 0.0070(16) O14 0.054(2) 0.043(2) 0.048(2) -0.0156(17) -0.0078(18) -0.0147(18) N1 0.048(3) 0.038(2) 0.051(3) -0.016(2) 0.006(2) -0.002(2) N2 0.037(2) 0.024(2) 0.045(2) -0.0118(18) -0.0118(19) 0.0002(17) N3 0.030(2) 0.026(2) 0.047(2) -0.0130(19) -0.0088(18) -0.0020(17) C13 0.028(2) 0.052(3) 0.044(3) -0.025(3) -0.005(2) -0.002(2) N5 0.029(2) 0.030(2) 0.048(2) -0.0174(19) -0.0137(18) 0.0050(17) N6 0.054(3) 0.039(3) 0.049(3) -0.013(2) -0.016(2) 0.006(2) N7 0.0230(18) 0.035(2) 0.032(2) -0.0073(18) -0.0054(16) -0.0021(17) N8 0.0247(19) 0.022(2) 0.051(2) -0.0109(18) -0.0084(18) -0.0017(16) N9 0.0243(19) 0.026(2) 0.034(2) -0.0081(17) -0.0069(16) -0.0016(16) N10 0.032(2) 0.027(2) 0.047(2) -0.0148(19) -0.0039(18) -0.0045(17) N11 0.0233(18) 0.035(2) 0.034(2) -0.0110(17) -0.0061(16) -0.0015(16) N12 0.037(2) 0.029(2) 0.052(3) 0.0001(19) -0.019(2) -0.0063(18) C1 0.038(3) 0.028(3) 0.053(3) -0.010(2) -0.018(2) 0.002(2) C2 0.035(3) 0.034(3) 0.055(3) -0.013(3) 0.001(2) 0.001(2) C3 0.045(3) 0.024(2) 0.046(3) -0.005(2) -0.018(2) 0.001(2) C4 0.025(2) 0.028(2) 0.047(3) -0.008(2) -0.008(2) 0.000(2) C5 0.037(3) 0.039(3) 0.066(4) -0.031(3) 0.004(3) -0.003(2) C6 0.034(3) 0.038(3) 0.030(3) -0.002(2) -0.007(2) -0.002(2) C7 0.052(3) 0.034(3) 0.044(3) -0.013(2) -0.017(3) 0.004(2) C8 0.037(3) 0.028(2) 0.048(3) -0.017(2) -0.006(2) 0.003(2) C9 0.039(3) 0.031(3) 0.043(3) -0.013(2) -0.009(2) -0.006(2) C10 0.040(3) 0.034(3) 0.041(3) -0.011(2) -0.006(2) 0.000(2) C11 0.018(2) 0.038(3) 0.036(3) -0.004(2) -0.0035(19) -0.006(2) C12 0.028(2) 0.033(3) 0.041(3) -0.013(2) -0.009(2) 0.000(2) N4 0.033(2) 0.052(3) 0.041(2) -0.020(2) -0.0036(19) -0.007(2) C14 0.032(2) 0.036(3) 0.038(3) -0.016(2) -0.011(2) -0.001(2) O3W 0.156(6) 0.219(8) 0.074(4) 0.005(4) -0.036(4) -0.047(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 O1 1.681(3) . ? Mo1 O2 1.749(3) . ? Mo1 O7 1.957(3) 2_666 ? Mo1 O5 1.964(3) . ? Mo1 O4 2.148(3) 2_666 ? Mo1 O4 2.387(3) . ? Mo2 O8 1.695(3) . ? Mo2 O6 1.712(3) . ? Mo2 O3 1.915(3) . ? Mo2 O9 1.929(3) . ? Mo2 O2 2.276(3) . ? Mo2 O4 2.369(3) . ? Mo3 O12 1.701(3) . ? Mo3 O13 1.701(3) . ? Mo3 O9 1.886(3) 2_666 ? Mo3 O5 1.978(3) . ? Mo3 O7 2.345(3) . ? Mo3 O4 2.348(3) 2_666 ? Mo4 O11 1.692(3) . ? Mo4 O14 1.695(3) . ? Mo4 O3 1.897(3) . ? Mo4 O7 1.988(3) . ? Mo4 O5 2.356(3) . ? Mo4 O4 2.390(3) . ? Cu1 N8 1.969(3) . ? Cu1 N5 1.993(4) . ? Cu1 N11 2.014(3) 1_655 ? Cu1 N3 2.016(4) . ? Cu1 O6 2.407(3) . ? O4 Mo1 2.148(3) 2_666 ? O4 Mo3 2.348(3) 2_666 ? O7 Mo1 1.957(3) 2_666 ? O9 Mo3 1.886(3) 2_666 ? N1 C2 1.311(6) . ? N1 N2 1.359(5) . ? N2 C10 1.315(5) . ? N2 C3 1.463(5) 1_565 ? N3 C10 1.326(6) . ? N3 C2 1.364(6) . ? C13 N4 1.304(6) . ? C13 N11 1.364(5) . ? N5 C9 1.328(5) . ? N5 C7 1.360(6) . ? N6 C7 1.315(6) . ? N6 N10 1.352(5) . ? N7 C14 1.308(5) . ? N7 N4 1.362(5) . ? N7 C6 1.462(5) . ? N8 C4 1.335(5) . ? N8 C1 1.340(6) . ? N9 C4 1.318(5) . ? N9 N12 1.367(5) . ? N9 C12 1.454(5) . ? N10 C9 1.315(6) . ? N10 C5 1.464(5) . ? N11 C14 1.321(5) . ? N11 Cu1 2.014(3) 1_455 ? N12 C1 1.313(6) . ? C3 N2 1.463(5) 1_545 ? C3 C8 1.500(6) . ? C5 C8 1.513(6) . ? C6 C11 1.512(6) . ? C11 C12 1.512(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Mo1 O2 105.05(15) . . ? O1 Mo1 O7 101.87(14) . 2_666 ? O2 Mo1 O7 96.72(13) . 2_666 ? O1 Mo1 O5 101.34(14) . . ? O2 Mo1 O5 96.05(13) . . ? O7 Mo1 O5 149.51(11) 2_666 . ? O1 Mo1 O4 98.96(14) . 2_666 ? O2 Mo1 O4 155.96(12) . 2_666 ? O7 Mo1 O4 79.13(11) 2_666 2_666 ? O5 Mo1 O4 77.96(11) . 2_666 ? O1 Mo1 O4 175.44(13) . . ? O2 Mo1 O4 79.47(11) . . ? O7 Mo1 O4 77.88(11) 2_666 . ? O5 Mo1 O4 77.42(10) . . ? O4 Mo1 O4 76.50(11) 2_666 . ? O8 Mo2 O6 105.30(16) . . ? O8 Mo2 O3 98.83(15) . . ? O6 Mo2 O3 102.48(14) . . ? O8 Mo2 O9 98.16(14) . . ? O6 Mo2 O9 99.70(14) . . ? O3 Mo2 O9 147.28(13) . . ? O8 Mo2 O2 165.35(13) . . ? O6 Mo2 O2 89.30(14) . . ? O3 Mo2 O2 78.66(12) . . ? O9 Mo2 O2 77.85(12) . . ? O8 Mo2 O4 94.66(13) . . ? O6 Mo2 O4 159.91(13) . . ? O3 Mo2 O4 76.21(11) . . ? O9 Mo2 O4 74.71(11) . . ? O2 Mo2 O4 70.71(10) . . ? O12 Mo3 O13 104.34(16) . . ? O12 Mo3 O9 101.57(15) . 2_666 ? O13 Mo3 O9 101.28(14) . 2_666 ? O12 Mo3 O5 97.82(14) . . ? O13 Mo3 O5 101.90(14) . . ? O9 Mo3 O5 144.87(12) 2_666 . ? O12 Mo3 O7 165.45(13) . . ? O13 Mo3 O7 87.60(13) . . ? O9 Mo3 O7 83.84(11) 2_666 . ? O5 Mo3 O7 71.17(11) . . ? O12 Mo3 O4 96.25(13) . 2_666 ? O13 Mo3 O4 159.33(13) . 2_666 ? O9 Mo3 O4 75.96(11) 2_666 2_666 ? O5 Mo3 O4 73.02(10) . 2_666 ? O7 Mo3 O4 71.76(10) . 2_666 ? O11 Mo4 O14 104.85(17) . . ? O11 Mo4 O3 101.45(15) . . ? O14 Mo4 O3 101.78(15) . . ? O11 Mo4 O7 102.19(14) . . ? O14 Mo4 O7 97.15(14) . . ? O3 Mo4 O7 144.62(12) . . ? O11 Mo4 O5 89.78(14) . . ? O14 Mo4 O5 162.96(14) . . ? O3 Mo4 O5 83.39(12) . . ? O7 Mo4 O5 70.79(11) . . ? O11 Mo4 O4 160.32(14) . . ? O14 Mo4 O4 94.73(13) . . ? O3 Mo4 O4 76.01(11) . . ? O7 Mo4 O4 72.86(10) . . ? O5 Mo4 O4 70.56(9) . . ? N8 Cu1 N5 91.92(14) . . ? N8 Cu1 N11 172.51(15) . 1_655 ? N5 Cu1 N11 90.16(15) . 1_655 ? N8 Cu1 N3 90.39(14) . . ? N5 Cu1 N3 175.36(15) . . ? N11 Cu1 N3 88.05(15) 1_655 . ? N8 Cu1 O6 99.87(14) . . ? N5 Cu1 O6 90.21(13) . . ? N11 Cu1 O6 87.30(13) 1_655 . ? N3 Cu1 O6 85.43(13) . . ? Mo1 O2 Mo2 117.03(14) . . ? Mo4 O3 Mo2 116.48(15) . . ? Mo1 O4 Mo3 91.85(10) 2_666 2_666 ? Mo1 O4 Mo2 163.67(14) 2_666 . ? Mo3 O4 Mo2 87.19(9) 2_666 . ? Mo1 O4 Mo1 103.50(11) 2_666 . ? Mo3 O4 Mo1 97.07(10) 2_666 . ? Mo2 O4 Mo1 92.79(9) . . ? Mo1 O4 Mo4 90.84(9) 2_666 . ? Mo3 O4 Mo4 164.23(13) 2_666 . ? Mo2 O4 Mo4 85.88(9) . . ? Mo1 O4 Mo4 97.40(10) . . ? Mo1 O5 Mo3 110.20(14) . . ? Mo1 O5 Mo4 112.02(12) . . ? Mo3 O5 Mo4 103.69(12) . . ? Mo2 O6 Cu1 162.87(19) . . ? Mo1 O7 Mo4 110.25(13) 2_666 . ? Mo1 O7 Mo3 110.79(13) 2_666 . ? Mo4 O7 Mo3 103.76(12) . . ? Mo3 O9 Mo2 116.97(14) 2_666 . ? C2 N1 N2 102.9(4) . . ? C10 N2 N1 110.0(4) . . ? C10 N2 C3 127.4(4) . 1_565 ? N1 N2 C3 121.8(4) . 1_565 ? C10 N3 C2 103.0(4) . . ? C10 N3 Cu1 126.9(3) . . ? C2 N3 Cu1 125.9(3) . . ? N4 C13 N11 113.7(4) . . ? C9 N5 C7 103.2(4) . . ? C9 N5 Cu1 126.2(3) . . ? C7 N5 Cu1 130.5(3) . . ? C7 N6 N10 102.4(4) . . ? C14 N7 N4 109.8(4) . . ? C14 N7 C6 128.9(4) . . ? N4 N7 C6 121.1(4) . . ? C4 N8 C1 103.1(4) . . ? C4 N8 Cu1 127.0(3) . . ? C1 N8 Cu1 129.8(3) . . ? C4 N9 N12 109.6(4) . . ? C4 N9 C12 130.3(4) . . ? N12 N9 C12 120.0(3) . . ? C9 N10 N6 111.0(4) . . ? C9 N10 C5 127.9(4) . . ? N6 N10 C5 121.0(4) . . ? C14 N11 C13 102.9(4) . . ? C14 N11 Cu1 128.6(3) . 1_455 ? C13 N11 Cu1 127.4(3) . 1_455 ? C1 N12 N9 102.6(4) . . ? N12 C1 N8 114.7(4) . . ? N1 C2 N3 113.8(5) . . ? N2 C3 C8 109.8(4) 1_545 . ? N9 C4 N8 110.1(4) . . ? N10 C5 C8 111.3(4) . . ? N7 C6 C11 113.1(3) . . ? N6 C7 N5 113.9(4) . . ? C3 C8 C5 112.2(4) . . ? N10 C9 N5 109.5(4) . . ? N2 C10 N3 110.3(4) . . ? C12 C11 C6 112.2(4) . . ? N9 C12 C11 111.5(4) . . ? C13 N4 N7 103.0(4) . . ? N7 C14 N11 110.5(4) . . ? _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 25.75 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 0.847 _refine_diff_density_min -0.546 _refine_diff_density_rms 0.100