data_global _journal_name_full CrystEngComm _journal_coden_cambridge 1350 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_email mengjx628@nenu.edu.cn _publ_contact_author_name 'Jingxin Meng' _publ_author_name 'Enbo Wang' data_34b _database_code_depnum_ccdc_archive 'CCDC 795840' #TrackingRef 'compound1.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C56 H61 Mn Mo8 N16 O44 P V6' _chemical_formula_weight 2821.28 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 '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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' V V 0.3005 0.5294 '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' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M 'I 41/a' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y+3/4, x+1/4, z+1/4' '-x+1/2, -y, z+1/2' 'y+3/4, -x+3/4, z+3/4' 'x+1/2, y+1/2, z+1/2' '-y+5/4, x+3/4, z+3/4' '-x+1, -y+1/2, z+1' 'y+5/4, -x+5/4, z+5/4' '-x, -y, -z' 'y-3/4, -x-1/4, -z-1/4' 'x-1/2, y, -z-1/2' '-y-3/4, x-3/4, -z-3/4' '-x+1/2, -y+1/2, -z+1/2' 'y-1/4, -x+1/4, -z+1/4' 'x, y+1/2, -z' '-y-1/4, x-1/4, -z-1/4' _cell_length_a 23.033(10) _cell_length_b 23.033(10) _cell_length_c 15.607(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 8280(5) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 30796 _cell_measurement_theta_min 3.15 _cell_measurement_theta_max 24.99 _exptl_crystal_description block _exptl_crystal_colour black _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.263 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5500 _exptl_absorpt_coefficient_mu 2.080 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.639 _exptl_absorpt_correction_T_max 0.660 _exptl_absorpt_process_details 'ABSCOR by T.Higashi 8 March, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Rotation anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku R-AXIS RAPID IP' _diffrn_measurement_method Oscillation _diffrn_detector_area_resol_mean 0.01 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% none _diffrn_reflns_number 30796 _diffrn_reflns_av_R_equivalents 0.1088 _diffrn_reflns_av_sigmaI/netI 0.0559 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.15 _diffrn_reflns_theta_max 24.99 _reflns_number_total 3646 _reflns_number_gt 2624 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0956P)^2^+76.9581P] 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 3646 _refine_ls_number_parameters 303 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0855 _refine_ls_R_factor_gt 0.0609 _refine_ls_wR_factor_ref 0.1780 _refine_ls_wR_factor_gt 0.1631 _refine_ls_goodness_of_fit_ref 1.070 _refine_ls_restrained_S_all 1.071 _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 -0.06421(4) -0.34464(3) 0.52569(5) 0.0240(3) Uani 1 1 d . . . Mo2 Mo -0.10067(3) -0.19383(4) 0.52721(5) 0.0234(3) Uani 1 1 d . . . V2 V -0.15198(6) -0.28614(6) 0.38010(9) 0.0134(3) Uani 1 1 d . . . Mn1 Mn 0.0000 -0.2500 0.8750 0.0095(5) Uani 1 4 d S . . V1 V 0.0000 -0.2500 0.62975(13) 0.0187(5) Uani 1 2 d S . . P1 P 0.0000 -0.2500 0.3750 0.0190(10) Uani 1 4 d S . . O1 O -0.0782(3) -0.3909(3) 0.6068(4) 0.0275(15) Uani 1 1 d . . . O2 O -0.2187(3) -0.3031(3) 0.3603(4) 0.0300(16) Uani 1 1 d . . . O3 O -0.1362(3) -0.1585(3) 0.6053(4) 0.0312(16) Uani 1 1 d . . . O4 O -0.0530(3) -0.2635(3) 0.4311(4) 0.0237(14) Uani 1 1 d . . . O5 O -0.1340(3) -0.3400(3) 0.4719(4) 0.0220(14) Uani 1 1 d . . . O6 O -0.1592(3) -0.2300(3) 0.4720(4) 0.0251(14) Uani 1 1 d . . . O7 O -0.0849(3) -0.1386(3) 0.4480(4) 0.0245(14) Uani 1 1 d . . . O8 O -0.0793(3) -0.2687(2) 0.5913(4) 0.0187(13) Uani 1 1 d . . . O9 O -0.0254(3) -0.3885(3) 0.4487(4) 0.0244(14) Uani 1 1 d . . . O10 O 0.0000 -0.2500 0.7345(6) 0.027(2) Uani 1 2 d S . . O11 O 0.0165(2) -0.3197(2) 0.5699(4) 0.0172(13) Uani 1 1 d . . . N1 N 0.0468(4) -0.1684(4) 0.8778(5) 0.0307(19) Uani 1 1 d . . . N2 N 0.0896(4) -0.0874(4) 0.8387(6) 0.032(2) Uani 1 1 d . . . N3 N 0.3954(4) -0.0086(4) 0.8390(6) 0.032(2) Uani 1 1 d . . . N4 N 0.4688(5) -0.0644(5) 0.8291(7) 0.057(3) Uani 1 1 d . . . C1 C 0.1147(5) -0.0419(5) 0.7830(7) 0.040(3) Uani 1 1 d . . . H1A H 0.0902 -0.0077 0.7848 0.048 Uiso 1 1 calc R . . H1B H 0.1157 -0.0558 0.7243 0.048 Uiso 1 1 calc R . . C2 C 0.4353(6) -0.0357(6) 0.8845(9) 0.058(4) Uani 1 1 d . . . H2A H 0.4394 -0.0349 0.9438 0.070 Uiso 1 1 calc R . . C3 C 0.4038(5) -0.0216(6) 0.7545(9) 0.051(3) Uani 1 1 d . . . H3A H 0.3817 -0.0078 0.7089 0.061 Uiso 1 1 calc R . . C4 C 0.4494(6) -0.0575(6) 0.7487(10) 0.062(4) Uani 1 1 d . . . H4A H 0.4645 -0.0742 0.6993 0.074 Uiso 1 1 calc R . . C5 C 0.1764(4) -0.0255(4) 0.8112(6) 0.029(2) Uani 1 1 d . . . C6 C 0.2452(5) 0.0491(5) 0.8464(7) 0.035(3) Uani 1 1 d . . . H6A H 0.2532 0.0881 0.8564 0.042 Uiso 1 1 calc R . . C7 C 0.0751(6) -0.0826(6) 0.9239(8) 0.058(4) Uani 1 1 d . . . H7A H 0.0817 -0.0507 0.9592 0.069 Uiso 1 1 calc R . . C8 C 0.2752(5) -0.0481(5) 0.8349(8) 0.040(3) Uani 1 1 d . . . H8A H 0.3042 -0.0761 0.8399 0.048 Uiso 1 1 calc R . . C9 C 0.1888(5) 0.0314(4) 0.8286(7) 0.035(2) Uani 1 1 d . . . H9A H 0.1590 0.0587 0.8284 0.042 Uiso 1 1 calc R . . C10 C 0.2204(4) -0.0649(4) 0.8136(7) 0.035(3) Uani 1 1 d . . . H10A H 0.2129 -0.1036 0.8007 0.042 Uiso 1 1 calc R . . C11 C 0.0712(4) -0.1405(4) 0.8144(6) 0.029(2) Uani 1 1 d . . . H11A H 0.0753 -0.1554 0.7594 0.035 Uiso 1 1 calc R . . C12 C 0.0497(6) -0.1323(5) 0.9461(7) 0.043(3) Uani 1 1 d . . . H12A H 0.0360 -0.1409 1.0006 0.052 Uiso 1 1 calc R . . C13 C 0.2888(5) 0.0091(4) 0.8493(6) 0.031(2) Uani 1 1 d . . . C14 C 0.3492(5) 0.0284(5) 0.8735(8) 0.044(3) Uani 1 1 d . . . H14A H 0.3550 0.0677 0.8531 0.053 Uiso 1 1 calc R . . H14B H 0.3522 0.0290 0.9355 0.053 Uiso 1 1 calc R . . OW1 O -0.1923(9) -0.2939(10) 0.6769(14) 0.081(6) Uani 0.50 1 d PU . . 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 0.0240(5) 0.0228(5) 0.0252(5) 0.0018(3) 0.0014(3) -0.0012(3) Mo2 0.0213(4) 0.0239(5) 0.0248(5) -0.0002(3) 0.0012(3) 0.0036(3) V2 0.0075(7) 0.0138(7) 0.0188(8) 0.0016(6) 0.0006(6) -0.0011(5) Mn1 0.0090(7) 0.0090(7) 0.0106(12) 0.000 0.000 0.000 V1 0.0188(11) 0.0188(11) 0.0185(11) 0.000 0.000 0.0005(8) P1 0.0193(14) 0.0193(14) 0.019(2) 0.000 0.000 0.000 O1 0.026(4) 0.028(4) 0.028(4) 0.006(3) 0.000(3) -0.001(3) O2 0.018(3) 0.034(4) 0.038(4) -0.005(3) 0.001(3) -0.003(3) O3 0.029(4) 0.035(4) 0.029(4) -0.005(3) 0.003(3) 0.011(3) O4 0.021(3) 0.023(3) 0.027(4) 0.003(3) 0.003(3) 0.002(3) O5 0.023(3) 0.016(3) 0.026(3) -0.001(3) -0.001(3) -0.001(2) O6 0.026(3) 0.021(3) 0.029(4) -0.001(3) -0.009(3) 0.001(3) O7 0.018(3) 0.022(3) 0.034(4) 0.007(3) -0.002(3) 0.004(3) O8 0.019(3) 0.019(3) 0.018(3) 0.000(2) -0.002(2) -0.001(2) O9 0.022(3) 0.019(3) 0.032(4) -0.004(3) 0.004(3) -0.001(3) O10 0.025(5) 0.037(6) 0.019(5) 0.000 0.000 -0.002(4) O11 0.015(3) 0.018(3) 0.018(3) 0.000(2) 0.000(2) 0.001(2) N1 0.026(4) 0.036(5) 0.030(5) 0.000(4) 0.000(4) 0.001(4) N2 0.035(5) 0.030(5) 0.031(5) -0.001(4) -0.006(4) -0.011(4) N3 0.028(5) 0.027(5) 0.040(5) 0.008(4) -0.011(4) -0.011(4) N4 0.050(6) 0.065(7) 0.056(7) 0.025(6) -0.006(6) 0.021(6) C1 0.041(7) 0.046(7) 0.032(6) 0.011(5) -0.008(5) -0.008(5) C2 0.062(9) 0.065(9) 0.048(8) 0.013(7) 0.011(7) -0.007(7) C3 0.040(7) 0.052(8) 0.060(8) -0.011(6) -0.005(6) 0.013(6) C4 0.037(7) 0.069(10) 0.079(10) -0.003(8) 0.005(7) 0.011(7) C5 0.037(6) 0.029(5) 0.020(5) 0.004(4) 0.000(4) -0.007(4) C6 0.036(6) 0.029(6) 0.040(6) -0.011(5) 0.011(5) -0.009(5) C7 0.082(10) 0.063(9) 0.028(6) -0.014(6) 0.006(6) -0.032(8) C8 0.034(6) 0.027(6) 0.059(8) 0.006(5) -0.001(6) 0.003(5) C9 0.040(6) 0.023(5) 0.043(6) 0.003(5) 0.000(5) 0.006(4) C10 0.033(6) 0.018(5) 0.054(7) -0.003(5) 0.000(5) -0.003(4) C11 0.028(5) 0.036(6) 0.023(5) -0.002(4) -0.001(4) -0.003(4) C12 0.064(8) 0.041(7) 0.024(6) -0.001(5) 0.004(5) -0.018(6) C13 0.036(6) 0.028(5) 0.029(5) 0.002(4) 0.001(5) -0.005(4) C14 0.043(7) 0.042(7) 0.049(7) -0.013(6) 0.010(6) -0.008(5) OW1 0.074(9) 0.081(10) 0.089(10) -0.013(8) 0.012(8) -0.028(8) _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 1.686(6) . ? Mo1 O9 1.806(6) . ? Mo1 O5 1.817(6) . ? Mo1 O8 2.057(6) . ? Mo1 O11 2.065(6) . ? Mo1 O4 2.395(6) . ? Mo1 V1 3.0946(17) . ? Mo2 O3 1.679(7) . ? Mo2 O6 1.802(6) . ? Mo2 O7 1.811(6) . ? Mo2 O8 2.053(6) . ? Mo2 O11 2.072(6) 7_444 ? Mo2 O4 2.457(6) . ? Mo2 V1 3.1003(17) . ? V2 O2 1.616(6) . ? V2 O7 1.902(6) 16_556 ? V2 O9 1.902(6) 10_656 ? V2 O6 1.939(6) . ? V2 O5 1.940(6) . ? Mn1 N1 2.167(9) . ? Mn1 N1 2.167(9) 7_444 ? Mn1 N1 2.167(9) 16_557 ? Mn1 N1 2.167(9) 10_657 ? Mn1 O10 2.193(9) 10_657 ? Mn1 O10 2.193(9) . ? V1 O10 1.634(9) . ? V1 O11 1.896(6) . ? V1 O11 1.896(6) 7_444 ? V1 O8 1.970(6) . ? V1 O8 1.970(6) 7_444 ? V1 Mo1 3.0946(17) 7_444 ? V1 Mo2 3.1003(17) 7_444 ? P1 O4 1.533(6) 7_444 ? P1 O4 1.533(6) 10_656 ? P1 O4 1.533(6) . ? P1 O4 1.533(6) 16_556 ? O7 V2 1.902(6) 10_656 ? O9 V2 1.902(6) 16_556 ? O11 Mo2 2.072(6) 7_444 ? N1 C11 1.307(13) . ? N1 C12 1.354(14) . ? N2 C11 1.348(13) . ? N2 C7 1.376(14) . ? N2 C1 1.479(13) . ? N3 C2 1.318(16) . ? N3 C3 1.365(16) . ? N3 C14 1.466(14) . ? N4 C2 1.333(17) . ? N4 C4 1.341(18) . ? C1 C5 1.535(14) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 H2A 0.9300 . ? C3 C4 1.342(17) . ? C3 H3A 0.9300 . ? C4 H4A 0.9300 . ? C5 C10 1.362(14) . ? C5 C9 1.368(14) . ? C6 C13 1.363(15) . ? C6 C9 1.389(15) . ? C6 H6A 0.9300 . ? C7 C12 1.331(17) . ? C7 H7A 0.9300 . ? C8 C10 1.363(15) . ? C8 C13 1.372(15) . ? C8 H8A 0.9300 . ? C9 H9A 0.9300 . ? C10 H10A 0.9300 . ? C11 H11A 0.9300 . ? C12 H12A 0.9300 . ? C13 C14 1.509(15) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? 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 O9 103.9(3) . . ? O1 Mo1 O5 102.4(3) . . ? O9 Mo1 O5 99.4(3) . . ? O1 Mo1 O8 97.5(3) . . ? O9 Mo1 O8 152.9(3) . . ? O5 Mo1 O8 91.7(3) . . ? O1 Mo1 O11 95.6(3) . . ? O9 Mo1 O11 86.1(3) . . ? O5 Mo1 O11 159.2(2) . . ? O8 Mo1 O11 75.5(2) . . ? O1 Mo1 O4 167.5(3) . . ? O9 Mo1 O4 88.4(3) . . ? O5 Mo1 O4 76.4(2) . . ? O8 Mo1 O4 70.2(2) . . ? O11 Mo1 O4 83.8(2) . . ? O1 Mo1 V1 98.2(2) . . ? O9 Mo1 V1 120.4(2) . . ? O5 Mo1 V1 128.60(19) . . ? O8 Mo1 V1 38.76(16) . . ? O11 Mo1 V1 36.71(16) . . ? O4 Mo1 V1 73.89(16) . . ? O3 Mo2 O6 101.9(3) . . ? O3 Mo2 O7 104.7(3) . . ? O6 Mo2 O7 98.5(3) . . ? O3 Mo2 O8 99.8(3) . . ? O6 Mo2 O8 91.4(3) . . ? O7 Mo2 O8 151.0(3) . . ? O3 Mo2 O11 98.6(3) . 7_444 ? O6 Mo2 O11 157.2(3) . 7_444 ? O7 Mo2 O11 85.8(3) . 7_444 ? O8 Mo2 O11 75.2(2) . 7_444 ? O3 Mo2 O4 168.0(3) . . ? O6 Mo2 O4 75.0(3) . . ? O7 Mo2 O4 87.2(3) . . ? O8 Mo2 O4 69.0(2) . . ? O11 Mo2 O4 82.9(2) 7_444 . ? O3 Mo2 V1 101.1(2) . . ? O6 Mo2 V1 127.8(2) . . ? O7 Mo2 V1 119.70(19) . . ? O8 Mo2 V1 38.62(16) . . ? O11 Mo2 V1 36.63(16) 7_444 . ? O4 Mo2 V1 73.03(15) . . ? O2 V2 O7 101.6(3) . 16_556 ? O2 V2 O9 102.2(3) . 10_656 ? O7 V2 O9 86.9(3) 16_556 10_656 ? O2 V2 O6 102.8(3) . . ? O7 V2 O6 155.4(3) 16_556 . ? O9 V2 O6 89.7(3) 10_656 . ? O2 V2 O5 100.9(3) . . ? O7 V2 O5 89.5(3) 16_556 . ? O9 V2 O5 156.9(3) 10_656 . ? O6 V2 O5 84.2(3) . . ? N1 Mn1 N1 177.7(4) . 7_444 ? N1 Mn1 N1 90.023(10) . 16_557 ? N1 Mn1 N1 90.023(10) 7_444 16_557 ? N1 Mn1 N1 90.023(10) . 10_657 ? N1 Mn1 N1 90.023(10) 7_444 10_657 ? N1 Mn1 N1 177.7(4) 16_557 10_657 ? N1 Mn1 O10 88.9(2) . 10_657 ? N1 Mn1 O10 88.9(2) 7_444 10_657 ? N1 Mn1 O10 91.1(2) 16_557 10_657 ? N1 Mn1 O10 91.1(2) 10_657 10_657 ? N1 Mn1 O10 91.1(2) . . ? N1 Mn1 O10 91.1(2) 7_444 . ? N1 Mn1 O10 88.9(2) 16_557 . ? N1 Mn1 O10 88.9(2) 10_657 . ? O10 Mn1 O10 180.000(1) 10_657 . ? O10 V1 O11 119.52(18) . . ? O10 V1 O11 119.52(18) . 7_444 ? O11 V1 O11 121.0(4) . 7_444 ? O10 V1 O8 107.75(18) . . ? O11 V1 O8 81.5(2) . . ? O11 V1 O8 81.3(2) 7_444 . ? O10 V1 O8 107.75(18) . 7_444 ? O11 V1 O8 81.3(2) . 7_444 ? O11 V1 O8 81.5(2) 7_444 7_444 ? O8 V1 O8 144.5(4) . 7_444 ? O10 V1 Mo1 121.66(4) . . ? O11 V1 Mo1 40.63(17) . . ? O11 V1 Mo1 103.99(18) 7_444 . ? O8 V1 Mo1 40.82(17) . . ? O8 V1 Mo1 115.90(19) 7_444 . ? O10 V1 Mo1 121.66(4) . 7_444 ? O11 V1 Mo1 103.99(18) . 7_444 ? O11 V1 Mo1 40.63(17) 7_444 7_444 ? O8 V1 Mo1 115.90(19) . 7_444 ? O8 V1 Mo1 40.82(17) 7_444 7_444 ? Mo1 V1 Mo1 116.69(8) . 7_444 ? O10 V1 Mo2 121.08(4) . . ? O11 V1 Mo2 104.43(18) . . ? O11 V1 Mo2 40.71(17) 7_444 . ? O8 V1 Mo2 40.57(17) . . ? O8 V1 Mo2 116.42(19) 7_444 . ? Mo1 V1 Mo2 70.47(4) . . ? Mo1 V1 Mo2 78.02(4) 7_444 . ? O10 V1 Mo2 121.08(4) . 7_444 ? O11 V1 Mo2 40.71(17) . 7_444 ? O11 V1 Mo2 104.43(18) 7_444 7_444 ? O8 V1 Mo2 116.42(19) . 7_444 ? O8 V1 Mo2 40.57(17) 7_444 7_444 ? Mo1 V1 Mo2 78.02(4) . 7_444 ? Mo1 V1 Mo2 70.47(4) 7_444 7_444 ? Mo2 V1 Mo2 117.84(8) . 7_444 ? O4 P1 O4 109.0(2) 7_444 10_656 ? O4 P1 O4 110.4(5) 7_444 . ? O4 P1 O4 109.0(2) 10_656 . ? O4 P1 O4 109.0(2) 7_444 16_556 ? O4 P1 O4 110.4(5) 10_656 16_556 ? O4 P1 O4 109.0(2) . 16_556 ? P1 O4 Mo1 126.6(3) . . ? P1 O4 Mo2 124.8(3) . . ? Mo1 O4 Mo2 94.9(2) . . ? Mo1 O5 V2 124.6(3) . . ? Mo2 O6 V2 126.7(4) . . ? Mo2 O7 V2 154.3(4) . 10_656 ? V1 O8 Mo2 100.8(3) . . ? V1 O8 Mo1 100.4(3) . . ? Mo2 O8 Mo1 120.8(3) . . ? Mo1 O9 V2 152.9(4) . 16_556 ? V1 O10 Mn1 180.0 . . ? V1 O11 Mo1 102.7(3) . . ? V1 O11 Mo2 102.7(3) . 7_444 ? Mo1 O11 Mo2 140.9(3) . 7_444 ? C11 N1 C12 105.8(9) . . ? C11 N1 Mn1 128.8(7) . . ? C12 N1 Mn1 125.0(7) . . ? C11 N2 C7 105.6(9) . . ? C11 N2 C1 126.9(9) . . ? C7 N2 C1 127.3(10) . . ? C2 N3 C3 108.6(11) . . ? C2 N3 C14 125.7(11) . . ? C3 N3 C14 125.7(10) . . ? C2 N4 C4 110.8(11) . . ? N2 C1 C5 111.6(8) . . ? N2 C1 H1A 109.3 . . ? C5 C1 H1A 109.3 . . ? N2 C1 H1B 109.3 . . ? C5 C1 H1B 109.3 . . ? H1A C1 H1B 108.0 . . ? N3 C2 N4 106.8(12) . . ? N3 C2 H2A 126.6 . . ? N4 C2 H2A 126.6 . . ? C4 C3 N3 108.1(12) . . ? C4 C3 H3A 126.0 . . ? N3 C3 H3A 126.0 . . ? N4 C4 C3 105.7(13) . . ? N4 C4 H4A 127.1 . . ? C3 C4 H4A 127.1 . . ? C10 C5 C9 118.5(10) . . ? C10 C5 C1 122.1(9) . . ? C9 C5 C1 119.2(10) . . ? C13 C6 C9 119.8(10) . . ? C13 C6 H6A 120.1 . . ? C9 C6 H6A 120.1 . . ? C12 C7 N2 106.8(11) . . ? C12 C7 H7A 126.6 . . ? N2 C7 H7A 126.6 . . ? C10 C8 C13 121.6(10) . . ? C10 C8 H8A 119.2 . . ? C13 C8 H8A 119.2 . . ? C5 C9 C6 121.1(10) . . ? C5 C9 H9A 119.5 . . ? C6 C9 H9A 119.5 . . ? C5 C10 C8 120.5(10) . . ? C5 C10 H10A 119.8 . . ? C8 C10 H10A 119.8 . . ? N1 C11 N2 111.7(9) . . ? N1 C11 H11A 124.2 . . ? N2 C11 H11A 124.2 . . ? C7 C12 N1 110.2(10) . . ? C7 C12 H12A 124.9 . . ? N1 C12 H12A 124.9 . . ? C6 C13 C8 118.5(10) . . ? C6 C13 C14 119.2(10) . . ? C8 C13 C14 122.2(10) . . ? N3 C14 C13 114.0(9) . . ? N3 C14 H14A 108.8 . . ? C13 C14 H14A 108.8 . . ? N3 C14 H14B 108.8 . . ? C13 C14 H14B 108.8 . . ? H14A C14 H14B 107.6 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 2.319 _refine_diff_density_min -1.414 _refine_diff_density_rms 0.192 # Attachment 'compound2.CIF' data_69a _database_code_depnum_ccdc_archive 'CCDC 795841' #TrackingRef 'compound2.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C56 H60 Mo9 N16 O44 P V5 Zn' _chemical_formula_weight 2875.70 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' 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' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 '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' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M 'I 41/a' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-y+3/4, x+1/4, z+1/4' 'y+3/4, -x+3/4, z+3/4' 'x+1/2, y+1/2, z+1/2' '-x+1, -y+1/2, z+1' '-y+5/4, x+3/4, z+3/4' 'y+5/4, -x+5/4, z+5/4' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'y-3/4, -x-1/4, -z-1/4' '-y-3/4, x-3/4, -z-3/4' '-x+1/2, -y+1/2, -z+1/2' 'x, y+1/2, -z' 'y-1/4, -x+1/4, -z+1/4' '-y-1/4, x-1/4, -z-1/4' _cell_length_a 22.921(3) _cell_length_b 22.921(3) _cell_length_c 15.642(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 8218(2) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 30512 _cell_measurement_theta_min 3.15 _cell_measurement_theta_max 25.00 _exptl_crystal_description block _exptl_crystal_colour black _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.324 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5592 _exptl_absorpt_coefficient_mu 2.273 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.613 _exptl_absorpt_correction_T_max 0.649 _exptl_absorpt_process_details 'ABSCOR by T.Higashi 8 March, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Rotation anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku R-AXIS RAPID IP' _diffrn_measurement_method Oscillation _diffrn_detector_area_resol_mean 0.01 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% none _diffrn_reflns_number 30512 _diffrn_reflns_av_R_equivalents 0.0348 _diffrn_reflns_av_sigmaI/netI 0.0198 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.15 _diffrn_reflns_theta_max 25.00 _reflns_number_total 3610 _reflns_number_gt 3137 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0413P)^2^+66.5893P] 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 3610 _refine_ls_number_parameters 303 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0392 _refine_ls_R_factor_gt 0.0332 _refine_ls_wR_factor_ref 0.0861 _refine_ls_wR_factor_gt 0.0839 _refine_ls_goodness_of_fit_ref 1.050 _refine_ls_restrained_S_all 1.050 _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 P1 P 0.5000 0.2500 -0.1250 0.0105(4) Uani 1 4 d S . . Zn1 Zn 0.5000 0.2500 0.3750 0.0147(2) Uani 1 4 d S . . V1 V 0.5000 0.2500 0.12993(7) 0.0168(2) Uani 1 2 d S . . Mo3 Mo 0.34721(3) 0.21389(3) -0.11995(4) 0.01603(15) Uani 0.25 1 d P . 1 V2 V 0.34721(3) 0.21389(3) -0.11995(4) 0.01603(15) Uani 0.75 1 d P . 2 Mo1 Mo 0.399400(16) 0.306615(16) 0.02752(2) 0.01636(12) Uani 1 1 d . . . Mo2 Mo 0.564107(17) 0.344720(16) 0.02599(3) 0.01759(12) Uani 1 1 d . . . C1 C 0.39102(19) 0.32040(19) 0.4363(3) 0.0185(9) Uani 1 1 d . . . H1A H 0.4055 0.3241 0.4916 0.022 Uiso 1 1 calc R . . C2 C 0.2416(2) 0.5389(2) 0.3996(3) 0.0198(10) Uani 1 1 d . . . C3 C 0.2220(2) 0.6001(2) 0.3750(3) 0.0289(11) Uani 1 1 d . . . H3A H 0.2220 0.6036 0.3132 0.035 Uiso 1 1 calc R . . H3B H 0.1823 0.6060 0.3947 0.035 Uiso 1 1 calc R . . C4 C 0.2865(3) 0.6872(2) 0.3690(4) 0.0389(14) Uani 1 1 d . . . H4A H 0.2854 0.6924 0.3100 0.047 Uiso 1 1 calc R . . C5 C 0.2750(2) 0.4256(2) 0.4392(3) 0.0194(9) Uani 1 1 d . . . C6 C 0.2923(2) 0.3641(2) 0.4655(3) 0.0242(10) Uani 1 1 d . . . H6A H 0.3059 0.3649 0.5242 0.029 Uiso 1 1 calc R . . H6B H 0.2582 0.3392 0.4632 0.029 Uiso 1 1 calc R . . C7 C 0.2177(2) 0.4386(2) 0.4204(3) 0.0219(10) Uani 1 1 d . . . H7A H 0.1900 0.4090 0.4200 0.026 Uiso 1 1 calc R . . C8 C 0.2009(2) 0.4950(2) 0.4024(3) 0.0217(10) Uani 1 1 d . . . H8A H 0.1619 0.5033 0.3920 0.026 Uiso 1 1 calc R . . C9 C 0.3835(2) 0.2998(2) 0.3035(3) 0.0307(12) Uani 1 1 d . . . H9A H 0.3923 0.2863 0.2489 0.037 Uiso 1 1 calc R . . C10 C 0.2993(2) 0.5260(2) 0.4169(3) 0.0245(11) Uani 1 1 d . . . H10A H 0.3272 0.5555 0.4147 0.029 Uiso 1 1 calc R . . C11 C 0.3326(2) 0.3258(3) 0.3265(3) 0.0359(13) Uani 1 1 d . . . H11A H 0.3006 0.3331 0.2915 0.043 Uiso 1 1 calc R . . C12 C 0.3158(2) 0.4699(2) 0.4374(3) 0.0251(11) Uani 1 1 d . . . H12A H 0.3546 0.4618 0.4501 0.030 Uiso 1 1 calc R . . C13 C 0.3070(3) 0.6988(2) 0.5040(4) 0.0389(14) Uani 1 1 d . . . H13A H 0.3230 0.7134 0.5543 0.047 Uiso 1 1 calc R . . C14 C 0.2714(2) 0.6530(2) 0.4966(4) 0.0332(12) Uani 1 1 d . . . H14A H 0.2572 0.6302 0.5412 0.040 Uiso 1 1 calc R . . O11 O 0.63405(13) 0.34003(13) -0.0275(2) 0.0187(7) Uani 1 1 d . . . O10 O 0.48349(12) 0.31952(13) 0.0687(2) 0.0163(6) Uani 1 1 d . . . O9 O 0.55307(12) 0.26346(12) -0.06880(19) 0.0161(6) Uani 1 1 d U . . O8 O 0.36401(14) 0.34204(14) 0.1058(2) 0.0216(7) Uani 1 1 d . . . O7 O 0.41469(13) 0.36225(13) -0.0517(2) 0.0184(7) Uani 1 1 d . . . O6 O 0.34017(13) 0.27024(13) -0.0283(2) 0.0186(7) Uani 1 1 d . . . O5 O 0.57826(13) 0.39075(13) 0.10746(19) 0.0181(7) Uani 1 1 d . . . O4 O 0.52634(13) 0.38889(13) -0.0516(2) 0.0192(7) Uani 1 1 d . . . O3 O 0.41981(13) 0.23148(12) 0.0912(2) 0.0169(6) Uani 1 1 d . . . O2 O 0.28000(13) 0.19689(14) -0.1397(2) 0.0221(7) Uani 1 1 d . . . O1 O 0.5000 0.2500 0.2338(3) 0.0190(9) Uani 1 2 d S . . O1W O 0.3078(4) 0.2044(4) 0.1777(7) 0.067(3) Uani 0.50 1 d P . . N1 N 0.41972(16) 0.29623(16) 0.3725(2) 0.0181(8) Uani 1 1 d . . . N2 N 0.25959(17) 0.64579(16) 0.4115(3) 0.0228(9) Uani 1 1 d . . . N3 N 0.33790(17) 0.33915(16) 0.4114(3) 0.0210(8) Uani 1 1 d . . . N4 N 0.3154(2) 0.7200(2) 0.4236(3) 0.0425(12) 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 P1 0.0100(6) 0.0100(6) 0.0116(10) 0.000 0.000 0.000 Zn1 0.0154(3) 0.0154(3) 0.0135(5) 0.000 0.000 0.000 V1 0.0170(5) 0.0167(5) 0.0167(6) 0.000 0.000 0.0018(4) Mo3 0.0116(3) 0.0177(3) 0.0189(3) 0.0011(2) -0.0003(2) -0.0005(2) V2 0.0116(3) 0.0177(3) 0.0189(3) 0.0011(2) -0.0003(2) -0.0005(2) Mo1 0.0158(2) 0.0161(2) 0.0172(2) -0.00018(15) 0.00227(15) 0.00308(14) Mo2 0.0184(2) 0.0165(2) 0.0179(2) -0.00314(15) -0.00181(15) -0.00140(15) C1 0.020(2) 0.020(2) 0.016(2) 0.0026(18) -0.0011(18) -0.0006(18) C2 0.022(2) 0.020(2) 0.017(2) -0.0010(18) -0.0003(19) 0.0038(19) C3 0.028(3) 0.026(3) 0.032(3) 0.001(2) -0.006(2) 0.006(2) C4 0.047(3) 0.029(3) 0.041(3) 0.004(3) 0.016(3) 0.002(3) C5 0.020(2) 0.023(2) 0.014(2) 0.0019(18) 0.0053(18) 0.0040(18) C6 0.030(3) 0.025(3) 0.018(2) 0.003(2) 0.006(2) 0.006(2) C7 0.017(2) 0.027(3) 0.022(2) -0.001(2) 0.0010(19) -0.0026(19) C8 0.015(2) 0.030(3) 0.021(2) -0.004(2) -0.0033(18) 0.0040(19) C9 0.031(3) 0.047(3) 0.015(2) -0.003(2) -0.004(2) 0.014(2) C10 0.015(2) 0.026(3) 0.032(3) 0.004(2) 0.002(2) -0.0023(19) C11 0.035(3) 0.057(4) 0.016(2) -0.003(2) -0.004(2) 0.019(3) C12 0.016(2) 0.028(3) 0.031(3) 0.001(2) -0.001(2) 0.0023(19) C13 0.045(3) 0.026(3) 0.046(3) -0.003(3) -0.004(3) -0.005(2) C14 0.035(3) 0.031(3) 0.034(3) 0.005(2) 0.001(2) -0.005(2) O11 0.0207(16) 0.0146(15) 0.0208(16) -0.0006(13) 0.0026(13) 0.0001(12) O10 0.0124(14) 0.0147(15) 0.0219(16) 0.0047(12) -0.0021(12) 0.0002(11) O9 0.0144(15) 0.0161(15) 0.0178(16) 0.0000(12) 0.0000(12) 0.0004(12) O8 0.0221(17) 0.0255(17) 0.0172(16) -0.0018(13) 0.0023(13) 0.0086(14) O7 0.0143(15) 0.0186(16) 0.0223(16) 0.0055(13) -0.0029(13) -0.0009(12) O6 0.0193(15) 0.0145(15) 0.0218(16) -0.0008(13) -0.0030(13) 0.0037(12) O5 0.0196(16) 0.0178(15) 0.0170(16) -0.0035(13) -0.0011(13) -0.0021(12) O4 0.0159(15) 0.0207(16) 0.0209(16) 0.0051(13) -0.0025(13) -0.0042(12) O3 0.0167(15) 0.0141(15) 0.0198(16) 0.0000(12) -0.0025(13) 0.0014(12) O2 0.0153(16) 0.0224(17) 0.0287(18) -0.0008(14) 0.0013(14) -0.0032(13) O1 0.015(2) 0.021(2) 0.021(2) 0.000 0.000 0.0025(18) O1W 0.042(5) 0.064(6) 0.094(8) -0.047(6) 0.037(5) -0.043(5) N1 0.0176(19) 0.0183(19) 0.018(2) 0.0023(16) 0.0011(16) 0.0019(15) N2 0.022(2) 0.0172(19) 0.030(2) 0.0060(17) 0.0078(17) 0.0028(16) N3 0.023(2) 0.020(2) 0.020(2) 0.0018(16) 0.0032(17) 0.0044(16) N4 0.046(3) 0.030(3) 0.052(3) 0.001(2) 0.010(3) -0.010(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 P1 O9 1.532(3) 11_665 ? P1 O9 1.532(3) . ? P1 O9 1.532(3) 6_554 ? P1 O9 1.532(3) 16_655 ? Zn1 N1 2.124(4) 16_656 ? Zn1 N1 2.124(4) 6_554 ? Zn1 N1 2.124(4) . ? Zn1 N1 2.124(4) 11_666 ? Zn1 O1 2.209(4) . ? Zn1 O1 2.209(4) 11_666 ? V1 O1 1.624(4) . ? V1 O10 1.897(3) 6_554 ? V1 O10 1.897(3) . ? V1 O3 1.981(3) . ? V1 O3 1.981(3) 6_554 ? V1 Mo2 3.0848(8) 6_554 ? V1 Mo2 3.0848(8) . ? V1 Mo1 3.0930(8) 6_554 ? V1 Mo1 3.0930(8) . ? Mo3 O2 1.619(3) . ? Mo3 O7 1.907(3) 16_655 ? Mo3 O4 1.913(3) 16_655 ? Mo3 O6 1.937(3) . ? Mo3 O11 1.950(3) 6_554 ? Mo3 O9 2.477(3) 6_554 ? Mo1 O8 1.678(3) . ? Mo1 O7 1.813(3) . ? Mo1 O6 1.816(3) . ? Mo1 O3 2.043(3) . ? Mo1 O10 2.054(3) . ? Mo1 O9 2.457(3) 6_554 ? Mo2 O5 1.686(3) . ? Mo2 O4 1.802(3) . ? Mo2 O11 1.812(3) . ? Mo2 O10 2.048(3) . ? Mo2 O3 2.056(3) 6_554 ? Mo2 O9 2.394(3) . ? C1 N1 1.318(6) . ? C1 N3 1.349(6) . ? C1 H1A 0.9300 . ? C2 C8 1.372(7) . ? C2 C10 1.382(7) . ? C2 C3 1.523(7) . ? C3 N2 1.473(6) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 N2 1.313(7) . ? C4 N4 1.317(8) . ? C4 H4A 0.9300 . ? C5 C7 1.378(6) . ? C5 C12 1.381(7) . ? C5 C6 1.520(6) . ? C6 N3 1.462(6) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 C8 1.376(7) . ? C7 H7A 0.9300 . ? C8 H8A 0.9300 . ? C9 C11 1.360(7) . ? C9 N1 1.364(6) . ? C9 H9A 0.9300 . ? C10 C12 1.380(7) . ? C10 H10A 0.9300 . ? C11 N3 1.369(6) . ? C11 H11A 0.9300 . ? C12 H12A 0.9300 . ? C13 C14 1.335(8) . ? C13 N4 1.363(8) . ? C13 H13A 0.9300 . ? C14 N2 1.369(7) . ? C14 H14A 0.9300 . ? O11 V2 1.950(3) 6_554 ? O11 Mo3 1.950(3) 6_554 ? O9 Mo1 2.457(3) 6_554 ? O9 Mo3 2.477(3) 6_554 ? O7 V2 1.907(3) 11_665 ? O7 Mo3 1.907(3) 11_665 ? O4 V2 1.913(3) 11_665 ? O4 Mo3 1.913(3) 11_665 ? O3 Mo2 2.056(3) 6_554 ? 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 O9 P1 O9 109.22(11) 11_665 . ? O9 P1 O9 109.22(11) 11_665 6_554 ? O9 P1 O9 110.0(2) . 6_554 ? O9 P1 O9 110.0(2) 11_665 16_655 ? O9 P1 O9 109.22(11) . 16_655 ? O9 P1 O9 109.22(11) 6_554 16_655 ? N1 Zn1 N1 90.020(4) 16_656 6_554 ? N1 Zn1 N1 90.020(4) 16_656 . ? N1 Zn1 N1 177.9(2) 6_554 . ? N1 Zn1 N1 177.9(2) 16_656 11_666 ? N1 Zn1 N1 90.020(4) 6_554 11_666 ? N1 Zn1 N1 90.020(4) . 11_666 ? N1 Zn1 O1 91.07(10) 16_656 . ? N1 Zn1 O1 88.93(10) 6_554 . ? N1 Zn1 O1 88.93(10) . . ? N1 Zn1 O1 91.07(10) 11_666 . ? N1 Zn1 O1 88.93(10) 16_656 11_666 ? N1 Zn1 O1 91.07(10) 6_554 11_666 ? N1 Zn1 O1 91.07(10) . 11_666 ? N1 Zn1 O1 88.93(10) 11_666 11_666 ? O1 Zn1 O1 180.0 . 11_666 ? O1 V1 O10 120.31(10) . 6_554 ? O1 V1 O10 120.31(10) . . ? O10 V1 O10 119.37(19) 6_554 . ? O1 V1 O3 107.81(10) . . ? O10 V1 O3 81.41(12) 6_554 . ? O10 V1 O3 80.82(12) . . ? O1 V1 O3 107.81(10) . 6_554 ? O10 V1 O3 80.82(12) 6_554 6_554 ? O10 V1 O3 81.41(12) . 6_554 ? O3 V1 O3 144.38(19) . 6_554 ? O1 V1 Mo2 121.804(19) . 6_554 ? O10 V1 Mo2 40.35(9) 6_554 6_554 ? O10 V1 Mo2 103.31(10) . 6_554 ? O3 V1 Mo2 41.07(9) . 6_554 ? O3 V1 Mo2 115.56(9) 6_554 6_554 ? O1 V1 Mo2 121.804(19) . . ? O10 V1 Mo2 103.31(10) 6_554 . ? O10 V1 Mo2 40.35(9) . . ? O3 V1 Mo2 115.56(9) . . ? O3 V1 Mo2 41.07(9) 6_554 . ? Mo2 V1 Mo2 116.39(4) 6_554 . ? O1 V1 Mo1 121.188(19) . 6_554 ? O10 V1 Mo1 40.32(9) 6_554 6_554 ? O10 V1 Mo1 103.87(10) . 6_554 ? O3 V1 Mo1 116.32(9) . 6_554 ? O3 V1 Mo1 40.52(8) 6_554 6_554 ? Mo2 V1 Mo1 77.70(2) 6_554 6_554 ? Mo2 V1 Mo1 70.564(18) . 6_554 ? O1 V1 Mo1 121.188(19) . . ? O10 V1 Mo1 103.87(10) 6_554 . ? O10 V1 Mo1 40.32(9) . . ? O3 V1 Mo1 40.52(8) . . ? O3 V1 Mo1 116.32(9) 6_554 . ? Mo2 V1 Mo1 70.564(18) 6_554 . ? Mo2 V1 Mo1 77.70(2) . . ? Mo1 V1 Mo1 117.62(4) 6_554 . ? O2 Mo3 O7 101.49(15) . 16_655 ? O2 Mo3 O4 102.50(15) . 16_655 ? O7 Mo3 O4 87.08(13) 16_655 16_655 ? O2 Mo3 O6 102.85(15) . . ? O7 Mo3 O6 155.59(13) 16_655 . ? O4 Mo3 O6 89.43(13) 16_655 . ? O2 Mo3 O11 101.44(15) . 6_554 ? O7 Mo3 O11 89.66(13) 16_655 6_554 ? O4 Mo3 O11 156.00(13) 16_655 6_554 ? O6 Mo3 O11 83.79(13) . 6_554 ? O2 Mo3 O9 172.02(14) . 6_554 ? O7 Mo3 O9 83.20(12) 16_655 6_554 ? O4 Mo3 O9 84.07(12) 16_655 6_554 ? O6 Mo3 O9 72.41(11) . 6_554 ? O11 Mo3 O9 71.94(11) 6_554 6_554 ? O8 Mo1 O7 104.60(15) . . ? O8 Mo1 O6 102.20(15) . . ? O7 Mo1 O6 97.98(14) . . ? O8 Mo1 O3 99.38(14) . . ? O7 Mo1 O3 151.86(13) . . ? O6 Mo1 O3 91.04(13) . . ? O8 Mo1 O10 98.92(14) . . ? O7 Mo1 O10 86.09(12) . . ? O6 Mo1 O10 156.67(13) . . ? O3 Mo1 O10 75.74(11) . . ? O8 Mo1 O9 167.96(13) . 6_554 ? O7 Mo1 O9 87.41(12) . 6_554 ? O6 Mo1 O9 74.74(12) . 6_554 ? O3 Mo1 O9 69.29(11) . 6_554 ? O10 Mo1 O9 82.55(11) . 6_554 ? O8 Mo1 V1 100.69(11) . . ? O7 Mo1 V1 120.34(9) . . ? O6 Mo1 V1 127.83(9) . . ? O3 Mo1 V1 39.05(8) . . ? O10 Mo1 V1 36.71(8) . . ? O9 Mo1 V1 73.30(7) 6_554 . ? O5 Mo2 O4 104.46(15) . . ? O5 Mo2 O11 102.47(14) . . ? O4 Mo2 O11 98.48(14) . . ? O5 Mo2 O10 95.94(14) . . ? O4 Mo2 O10 86.83(12) . . ? O11 Mo2 O10 158.81(13) . . ? O5 Mo2 O3 97.03(14) . 6_554 ? O4 Mo2 O3 153.84(13) . 6_554 ? O11 Mo2 O3 91.14(13) . 6_554 ? O10 Mo2 O3 76.14(11) . 6_554 ? O5 Mo2 O9 167.25(13) . . ? O4 Mo2 O9 88.24(12) . . ? O11 Mo2 O9 76.19(12) . . ? O10 Mo2 O9 83.53(11) . . ? O3 Mo2 O9 70.44(11) 6_554 . ? O5 Mo2 V1 97.68(11) . . ? O4 Mo2 V1 121.43(9) . . ? O11 Mo2 V1 128.55(9) . . ? O10 Mo2 V1 36.85(8) . . ? O3 Mo2 V1 39.29(8) 6_554 . ? O9 Mo2 V1 74.25(7) . . ? N1 C1 N3 111.4(4) . . ? N1 C1 H1A 124.3 . . ? N3 C1 H1A 124.3 . . ? C8 C2 C10 119.2(4) . . ? C8 C2 C3 118.9(4) . . ? C10 C2 C3 121.9(4) . . ? N2 C3 C2 112.7(4) . . ? N2 C3 H3A 109.1 . . ? C2 C3 H3A 109.1 . . ? N2 C3 H3B 109.1 . . ? C2 C3 H3B 109.1 . . ? H3A C3 H3B 107.8 . . ? N2 C4 N4 108.7(5) . . ? N2 C4 H4A 125.7 . . ? N4 C4 H4A 125.7 . . ? C7 C5 C12 118.8(4) . . ? C7 C5 C6 120.6(4) . . ? C12 C5 C6 120.6(4) . . ? N3 C6 C5 113.1(4) . . ? N3 C6 H6A 109.0 . . ? C5 C6 H6A 109.0 . . ? N3 C6 H6B 109.0 . . ? C5 C6 H6B 109.0 . . ? H6A C6 H6B 107.8 . . ? C8 C7 C5 120.9(4) . . ? C8 C7 H7A 119.5 . . ? C5 C7 H7A 119.5 . . ? C2 C8 C7 120.3(4) . . ? C2 C8 H8A 119.8 . . ? C7 C8 H8A 119.8 . . ? C11 C9 N1 109.8(4) . . ? C11 C9 H9A 125.1 . . ? N1 C9 H9A 125.1 . . ? C12 C10 C2 120.4(4) . . ? C12 C10 H10A 119.8 . . ? C2 C10 H10A 119.8 . . ? C9 C11 N3 106.2(4) . . ? C9 C11 H11A 126.9 . . ? N3 C11 H11A 126.9 . . ? C10 C12 C5 120.4(4) . . ? C10 C12 H12A 119.8 . . ? C5 C12 H12A 119.8 . . ? C14 C13 N4 106.7(5) . . ? C14 C13 H13A 126.7 . . ? N4 C13 H13A 126.7 . . ? C13 C14 N2 107.5(5) . . ? C13 C14 H14A 126.3 . . ? N2 C14 H14A 126.3 . . ? Mo2 O11 V2 125.10(16) . 6_554 ? Mo2 O11 Mo3 125.10(16) . 6_554 ? V2 O11 Mo3 0.00(4) 6_554 6_554 ? V1 O10 Mo2 102.80(13) . . ? V1 O10 Mo1 102.98(13) . . ? Mo2 O10 Mo1 141.73(16) . . ? P1 O9 Mo2 126.58(16) . . ? P1 O9 Mo1 124.90(16) . 6_554 ? Mo2 O9 Mo1 94.70(10) . 6_554 ? P1 O9 Mo3 126.13(16) . 6_554 ? Mo2 O9 Mo3 86.53(9) . 6_554 ? Mo1 O9 Mo3 85.75(9) 6_554 6_554 ? Mo1 O7 V2 153.71(18) . 11_665 ? Mo1 O7 Mo3 153.71(18) . 11_665 ? V2 O7 Mo3 0.00(5) 11_665 11_665 ? Mo1 O6 Mo3 126.84(16) . . ? Mo2 O4 V2 152.31(18) . 11_665 ? Mo2 O4 Mo3 152.31(18) . 11_665 ? V2 O4 Mo3 0.00(4) 11_665 11_665 ? V1 O3 Mo1 100.42(13) . . ? V1 O3 Mo2 99.63(13) . 6_554 ? Mo1 O3 Mo2 121.03(15) . 6_554 ? V1 O1 Zn1 180.0 . . ? C1 N1 C9 105.7(4) . . ? C1 N1 Zn1 128.9(3) . . ? C9 N1 Zn1 124.9(3) . . ? C4 N2 C14 108.2(5) . . ? C4 N2 C3 126.4(5) . . ? C14 N2 C3 125.4(4) . . ? C1 N3 C11 106.9(4) . . ? C1 N3 C6 127.1(4) . . ? C11 N3 C6 125.9(4) . . ? C4 N4 C13 108.9(5) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.820 _refine_diff_density_min -0.603 _refine_diff_density_rms 0.117 # Attachment 'compound3.CIF' data_1 _database_code_depnum_ccdc_archive 'CCDC 795842' #TrackingRef 'compound3.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C56 H64 Cu Mo9 N16 O46 P V5' _chemical_formula_weight 2909.90 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' 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' 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' V V 0.3005 0.5294 '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' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M 'I 41/a' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y+3/4, x+1/4, z+1/4' '-x+1/2, -y, z+1/2' 'y+3/4, -x+3/4, z+3/4' 'x+1/2, y+1/2, z+1/2' '-y+5/4, x+3/4, z+3/4' '-x+1, -y+1/2, z+1' 'y+5/4, -x+5/4, z+5/4' '-x, -y, -z' 'y-3/4, -x-1/4, -z-1/4' 'x-1/2, y, -z-1/2' '-y-3/4, x-3/4, -z-3/4' '-x+1/2, -y+1/2, -z+1/2' 'y-1/4, -x+1/4, -z+1/4' 'x, y+1/2, -z' '-y-1/4, x-1/4, -z-1/4' _cell_length_a 22.878(9) _cell_length_b 22.878(9) _cell_length_c 15.853(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 8298(5) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 30123 _cell_measurement_theta_min 3.13 _cell_measurement_theta_max 25.00 _exptl_crystal_description block _exptl_crystal_colour black _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.329 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5668 _exptl_absorpt_coefficient_mu 2.222 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.677 _exptl_absorpt_correction_T_max 0.717 _exptl_absorpt_process_details 'ABSCOR by T.Higashi 8 March, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Rotation anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku R-AXIS RAPID IP' _diffrn_measurement_method Oscillation _diffrn_detector_area_resol_mean 0.01 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% none _diffrn_reflns_number 30123 _diffrn_reflns_av_R_equivalents 0.1079 _diffrn_reflns_av_sigmaI/netI 0.0637 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.13 _diffrn_reflns_theta_max 25.00 _reflns_number_total 3615 _reflns_number_gt 2577 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0568P)^2^+99.3228P] 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 3615 _refine_ls_number_parameters 312 _refine_ls_number_restraints 24 _refine_ls_R_factor_all 0.0818 _refine_ls_R_factor_gt 0.0534 _refine_ls_wR_factor_ref 0.1369 _refine_ls_wR_factor_gt 0.1234 _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_restrained_S_all 1.049 _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 0.0000 0.2500 0.1250 0.0129(4) Uani 1 4 d S . . Mo1 Mo 0.06323(3) 0.34571(3) 0.47619(5) 0.0194(2) Uani 1 1 d . . . Mo2 Mo 0.10101(3) 0.19349(3) 0.47473(5) 0.0174(2) Uani 1 1 d . . . Mo3 Mo 0.15300(4) 0.28722(5) 0.62037(8) 0.0190(3) Uani 0.25 1 d P . . V2 V 0.15300(4) 0.28722(5) 0.62037(8) 0.0190(3) Uani 0.75 1 d P . . V1 V 0.0000 0.2500 0.37426(13) 0.0188(4) Uani 1 2 d S . . P1 P 0.0000 0.2500 0.6250 0.0147(8) Uani 1 4 d S . . O1 O 0.0000 0.2500 0.2734(5) 0.0202(17) Uani 1 2 d S . . O2 O 0.0864(2) 0.1373(2) 0.5517(4) 0.0239(14) Uani 1 1 d . . . O3 O 0.0534(2) 0.2638(2) 0.5695(4) 0.0210(13) Uani 1 1 d . . . O4 O 0.0254(2) 0.3902(2) 0.5517(4) 0.0240(14) Uani 1 1 d . . . O5 O 0.1594(2) 0.2302(2) 0.5301(4) 0.0257(14) Uani 1 1 d . . . O6 O 0.1334(2) 0.3414(2) 0.5291(4) 0.0250(14) Uani 1 1 d . . . O7 O 0.1368(2) 0.1590(3) 0.3967(4) 0.0275(15) Uani 1 1 d . . . O8 O 0.0782(2) 0.3913(2) 0.3947(4) 0.0208(13) Uani 1 1 d . . . O9 O 0.0801(2) 0.2692(2) 0.4124(4) 0.0216(13) Uani 1 1 d . . . O10 O -0.0171(2) 0.3201(2) 0.4337(4) 0.0206(13) Uani 1 1 d . . . O11 O 0.2200(2) 0.3047(2) 0.6377(4) 0.0268(14) Uani 1 1 d . . . N1 N 0.0769(3) 0.2052(3) 0.1272(5) 0.0196(15) Uani 1 1 d . . . N3 N 0.2414(3) -0.1440(3) 0.0923(5) 0.0264(18) Uani 1 1 d . . . N5 N 0.1588(3) 0.1616(3) 0.0877(5) 0.0221(16) Uani 1 1 d U . . N7 N 0.1860(4) -0.2187(4) 0.0820(7) 0.048(2) Uani 1 1 d . . . C1 C 0.2580(4) -0.0364(4) 0.1024(6) 0.023(2) Uani 1 1 d . . . C2 C 0.2782(4) -0.0978(4) 0.1277(7) 0.031(2) Uani 1 1 d . . . H2A H 0.3181 -0.1035 0.1087 0.038 Uiso 1 1 calc R . . H2B H 0.2779 -0.1009 0.1887 0.038 Uiso 1 1 calc R . . C3 C 0.2148(4) -0.1863(4) 0.1353(8) 0.044(3) Uani 1 1 d . . . H3A H 0.2166 -0.1918 0.1933 0.053 Uiso 1 1 calc R . . C6 C 0.1129(4) 0.1988(5) 0.1965(7) 0.036(2) Uani 1 1 d U . . H6A H 0.1045 0.2110 0.2512 0.043 Uiso 1 1 calc R . . C8 C 0.1068(3) 0.1823(3) 0.0633(6) 0.022(2) Uani 1 1 d . . . H8A H 0.0932 0.1809 0.0081 0.027 Uiso 1 1 calc R . . C10 C 0.1951(5) -0.1986(5) 0.0024(8) 0.049(3) Uani 1 1 d . . . H10A H 0.1800 -0.2145 -0.0470 0.059 Uiso 1 1 calc R . . C12 C 0.1997(4) -0.0250(4) 0.0865(7) 0.028(2) Uani 1 1 d U . . H12A H 0.1721 -0.0547 0.0909 0.034 Uiso 1 1 calc R . . C14 C 0.2979(4) 0.0081(4) 0.0985(6) 0.025(2) Uani 1 1 d . . . H14A H 0.3371 0.0004 0.1096 0.030 Uiso 1 1 calc R . . C15 C 0.1632(4) 0.1715(5) 0.1710(7) 0.041(3) Uani 1 1 d . . . H15A H 0.1947 0.1617 0.2052 0.049 Uiso 1 1 calc R . . C17 C 0.2808(3) 0.0637(4) 0.0784(6) 0.026(2) Uani 1 1 d . . . H17A H 0.3083 0.0936 0.0763 0.032 Uiso 1 1 calc R . . C18 C 0.2295(5) -0.1521(4) 0.0083(8) 0.041(3) Uani 1 1 d . . . H18A H 0.2430 -0.1292 -0.0361 0.049 Uiso 1 1 calc R . . C23 C 0.1826(4) 0.0311(4) 0.0640(6) 0.028(2) Uani 1 1 d . . . H23A H 0.1436 0.0384 0.0508 0.034 Uiso 1 1 calc R . . C25 C 0.2222(3) 0.0759(3) 0.0609(5) 0.0199(18) Uani 1 1 d . . . C26 C 0.2038(4) 0.1369(4) 0.0338(6) 0.026(2) Uani 1 1 d . . . H26A H 0.2377 0.1624 0.0345 0.031 Uiso 1 1 calc R . . H26B H 0.1894 0.1353 -0.0237 0.031 Uiso 1 1 calc R . . O1W O 0.3096(5) 0.2038(5) 0.1761(9) 0.077(4) Uani 0.75 1 d PU . . O2W O 0.2390(19) 0.2834(15) 0.176(3) 0.082(12) Uani 0.25 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0124(6) 0.0124(6) 0.0138(11) 0.000 0.000 0.000 Mo1 0.0215(4) 0.0177(4) 0.0191(5) 0.0027(3) 0.0025(3) -0.0019(3) Mo2 0.0175(4) 0.0165(4) 0.0183(5) -0.0006(3) 0.0023(3) 0.0033(3) Mo3 0.0134(5) 0.0192(6) 0.0245(7) 0.0011(5) -0.0002(5) -0.0016(4) V2 0.0134(5) 0.0192(6) 0.0245(7) 0.0011(5) -0.0002(5) -0.0016(4) V1 0.0202(10) 0.0212(10) 0.0149(12) 0.000 0.000 0.0008(8) P1 0.0136(12) 0.0136(12) 0.017(2) 0.000 0.000 0.000 O1 0.020(4) 0.020(4) 0.020(5) 0.000 0.000 0.000(3) O2 0.016(3) 0.029(3) 0.027(4) 0.012(3) -0.002(2) -0.001(2) O3 0.018(3) 0.015(3) 0.030(4) 0.003(2) -0.002(3) -0.001(2) O4 0.018(3) 0.024(3) 0.030(4) -0.010(3) 0.003(3) -0.004(2) O5 0.026(3) 0.019(3) 0.032(4) 0.001(3) -0.012(3) 0.007(2) O6 0.034(3) 0.018(3) 0.023(4) 0.005(3) -0.008(3) 0.002(3) O7 0.023(3) 0.031(3) 0.028(4) -0.002(3) 0.000(3) 0.016(3) O8 0.023(3) 0.023(3) 0.017(4) 0.006(2) -0.001(2) -0.003(2) O9 0.025(3) 0.018(3) 0.022(4) -0.001(2) -0.007(3) 0.006(2) O10 0.014(3) 0.019(3) 0.029(4) -0.009(3) 0.006(2) -0.003(2) O11 0.020(3) 0.026(3) 0.034(4) -0.003(3) 0.000(3) -0.003(3) N1 0.022(3) 0.017(3) 0.020(4) -0.005(3) 0.003(3) -0.002(3) N3 0.021(4) 0.023(4) 0.036(5) 0.009(3) 0.009(3) 0.007(3) N5 0.022(3) 0.022(3) 0.022(4) -0.001(3) 0.006(3) 0.005(3) N7 0.043(5) 0.041(5) 0.060(8) -0.001(5) 0.017(5) -0.007(4) C1 0.023(4) 0.024(4) 0.021(6) 0.002(4) -0.001(4) 0.004(4) C2 0.038(5) 0.025(5) 0.031(6) -0.002(4) -0.014(5) 0.009(4) C3 0.044(6) 0.036(6) 0.053(8) 0.004(5) 0.027(6) 0.003(5) C6 0.033(5) 0.055(5) 0.019(5) -0.007(4) -0.010(4) 0.021(4) C8 0.023(4) 0.016(4) 0.028(6) 0.005(4) -0.004(4) 0.007(3) C10 0.053(7) 0.035(6) 0.058(9) -0.010(6) -0.005(6) 0.001(5) C12 0.021(4) 0.022(4) 0.042(6) 0.002(4) 0.003(4) -0.006(3) C14 0.017(4) 0.035(5) 0.022(6) -0.001(4) -0.003(3) 0.009(4) C15 0.036(6) 0.062(7) 0.025(7) 0.002(5) -0.010(5) 0.025(5) C17 0.015(4) 0.032(5) 0.032(6) -0.002(4) 0.002(4) -0.001(4) C18 0.043(6) 0.039(6) 0.042(8) -0.004(5) -0.003(5) -0.005(5) C23 0.015(4) 0.031(5) 0.038(7) 0.006(4) -0.001(4) 0.000(4) C25 0.023(4) 0.021(4) 0.016(5) -0.002(3) 0.006(3) 0.002(3) C26 0.027(4) 0.025(4) 0.026(6) 0.009(4) 0.006(4) 0.011(4) O1W 0.064(6) 0.082(7) 0.085(8) -0.022(6) 0.026(6) -0.039(6) O2W 0.11(3) 0.05(2) 0.08(3) 0.00(2) 0.00(3) -0.03(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 N1 2.038(7) 7_454 ? Cu1 N1 2.038(7) 12_666 ? Cu1 N1 2.038(7) . ? Cu1 N1 2.038(7) 14 ? Cu1 O1 2.353(8) 14 ? Cu1 O1 2.353(8) . ? Mo1 O8 1.695(6) . ? Mo1 O4 1.793(6) . ? Mo1 O6 1.813(6) . ? Mo1 O10 2.042(5) . ? Mo1 O9 2.057(6) . ? Mo1 O3 2.398(6) . ? Mo1 V1 3.0819(16) . ? Mo2 O7 1.680(6) . ? Mo2 O2 1.803(6) . ? Mo2 O5 1.805(6) . ? Mo2 O9 2.051(6) . ? Mo2 O10 2.051(5) 7_454 ? Mo2 O3 2.454(6) . ? Mo2 V1 3.0900(16) . ? Mo3 O11 1.607(6) . ? Mo3 O2 1.909(6) 12_667 ? Mo3 O4 1.915(6) 14_556 ? Mo3 O5 1.943(6) . ? Mo3 O6 1.957(6) . ? Mo3 O3 2.475(5) . ? V1 O1 1.599(8) . ? V1 O10 1.902(5) . ? V1 O10 1.902(5) 7_454 ? V1 O9 1.979(5) . ? V1 O9 1.979(5) 7_454 ? V1 Mo1 3.0819(16) 7_454 ? V1 Mo2 3.0900(16) 7_454 ? P1 O3 1.539(6) 12_667 ? P1 O3 1.539(6) 7_454 ? P1 O3 1.539(6) . ? P1 O3 1.539(6) 14_556 ? O2 V2 1.909(6) 14_556 ? O2 Mo3 1.909(6) 14_556 ? O4 V2 1.915(6) 12_667 ? O4 Mo3 1.915(6) 12_667 ? O10 Mo2 2.051(5) 7_454 ? N1 C8 1.329(11) . ? N1 C6 1.381(11) . ? N3 C3 1.331(12) . ? N3 C18 1.371(14) . ? N3 C2 1.464(11) . ? N5 C8 1.336(10) . ? N5 C15 1.344(13) . ? N5 C26 1.453(11) . ? N7 C3 1.302(15) . ? N7 C10 1.359(15) . ? C1 C14 1.369(12) . ? C1 C12 1.382(12) . ? C1 C2 1.530(12) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 H3A 0.9300 . ? C6 C15 1.369(13) . ? C6 H6A 0.9300 . ? C8 H8A 0.9300 . ? C10 C18 1.327(14) . ? C10 H10A 0.9300 . ? C12 C23 1.390(12) . ? C12 H12A 0.9300 . ? C14 C17 1.370(12) . ? C14 H14A 0.9300 . ? C15 H15A 0.9300 . ? C17 C25 1.396(11) . ? C17 H17A 0.9300 . ? C18 H18A 0.9300 . ? C23 C25 1.370(11) . ? C23 H23A 0.9300 . ? C25 C26 1.520(11) . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? 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 N1 Cu1 N1 90.017(8) 7_454 12_666 ? N1 Cu1 N1 178.0(4) 7_454 . ? N1 Cu1 N1 90.017(8) 12_666 . ? N1 Cu1 N1 90.017(8) 7_454 14 ? N1 Cu1 N1 178.0(4) 12_666 14 ? N1 Cu1 N1 90.017(8) . 14 ? N1 Cu1 O1 91.0(2) 7_454 14 ? N1 Cu1 O1 89.0(2) 12_666 14 ? N1 Cu1 O1 91.0(2) . 14 ? N1 Cu1 O1 89.0(2) 14 14 ? N1 Cu1 O1 89.0(2) 7_454 . ? N1 Cu1 O1 91.0(2) 12_666 . ? N1 Cu1 O1 89.0(2) . . ? N1 Cu1 O1 91.0(2) 14 . ? O1 Cu1 O1 180.0 14 . ? O8 Mo1 O4 104.9(3) . . ? O8 Mo1 O6 102.0(3) . . ? O4 Mo1 O6 98.6(3) . . ? O8 Mo1 O10 96.1(3) . . ? O4 Mo1 O10 87.1(2) . . ? O6 Mo1 O10 158.9(2) . . ? O8 Mo1 O9 96.4(3) . . ? O4 Mo1 O9 154.3(2) . . ? O6 Mo1 O9 90.8(2) . . ? O10 Mo1 O9 76.3(2) . . ? O8 Mo1 O3 165.8(2) . . ? O4 Mo1 O3 89.2(2) . . ? O6 Mo1 O3 75.8(2) . . ? O10 Mo1 O3 84.0(2) . . ? O9 Mo1 O3 69.8(2) . . ? O8 Mo1 V1 97.6(2) . . ? O4 Mo1 V1 121.78(17) . . ? O6 Mo1 V1 128.22(18) . . ? O10 Mo1 V1 37.00(15) . . ? O9 Mo1 V1 39.29(15) . . ? O3 Mo1 V1 73.98(14) . . ? O7 Mo2 O2 104.7(3) . . ? O7 Mo2 O5 102.4(3) . . ? O2 Mo2 O5 98.0(3) . . ? O7 Mo2 O9 99.0(3) . . ? O2 Mo2 O9 152.2(2) . . ? O5 Mo2 O9 90.8(2) . . ? O7 Mo2 O10 98.7(3) . 7_454 ? O2 Mo2 O10 86.2(2) . 7_454 ? O5 Mo2 O10 156.6(2) . 7_454 ? O9 Mo2 O10 76.0(2) . 7_454 ? O7 Mo2 O3 166.9(2) . . ? O2 Mo2 O3 88.3(2) . . ? O5 Mo2 O3 74.1(2) . . ? O9 Mo2 O3 68.8(2) . . ? O10 Mo2 O3 83.0(2) 7_454 . ? O7 Mo2 V1 100.5(2) . . ? O2 Mo2 V1 120.58(17) . . ? O5 Mo2 V1 127.55(17) . . ? O9 Mo2 V1 39.09(15) . . ? O10 Mo2 V1 36.89(15) 7_454 . ? O3 Mo2 V1 73.13(14) . . ? O11 Mo3 O2 101.8(3) . 12_667 ? O11 Mo3 O4 102.9(3) . 14_556 ? O2 Mo3 O4 87.1(2) 12_667 14_556 ? O11 Mo3 O5 102.8(3) . . ? O2 Mo3 O5 155.4(2) 12_667 . ? O4 Mo3 O5 89.1(3) 14_556 . ? O11 Mo3 O6 100.8(3) . . ? O2 Mo3 O6 89.7(3) 12_667 . ? O4 Mo3 O6 156.3(2) 14_556 . ? O5 Mo3 O6 84.1(3) . . ? O11 Mo3 O3 170.7(3) . . ? O2 Mo3 O3 83.9(2) 12_667 . ? O4 Mo3 O3 84.7(2) 14_556 . ? O5 Mo3 O3 71.5(2) . . ? O6 Mo3 O3 71.6(2) . . ? O1 V1 O10 119.71(19) . . ? O1 V1 O10 119.71(19) . 7_454 ? O10 V1 O10 120.6(4) . 7_454 ? O1 V1 O9 107.81(19) . . ? O10 V1 O9 81.4(2) . . ? O10 V1 O9 81.1(2) 7_454 . ? O1 V1 O9 107.81(19) . 7_454 ? O10 V1 O9 81.1(2) . 7_454 ? O10 V1 O9 81.4(2) 7_454 7_454 ? O9 V1 O9 144.4(4) . 7_454 ? O1 V1 Mo1 121.62(4) . . ? O10 V1 Mo1 40.26(16) . . ? O10 V1 Mo1 104.09(18) 7_454 . ? O9 V1 Mo1 41.17(16) . . ? O9 V1 Mo1 115.60(18) 7_454 . ? O1 V1 Mo1 121.62(4) . 7_454 ? O10 V1 Mo1 104.09(18) . 7_454 ? O10 V1 Mo1 40.26(16) 7_454 7_454 ? O9 V1 Mo1 115.60(18) . 7_454 ? O9 V1 Mo1 41.17(16) 7_454 7_454 ? Mo1 V1 Mo1 116.76(7) . 7_454 ? O1 V1 Mo2 121.03(4) . . ? O10 V1 Mo2 104.55(19) . . ? O10 V1 Mo2 40.35(15) 7_454 . ? O9 V1 Mo2 40.80(16) . . ? O9 V1 Mo2 116.21(18) 7_454 . ? Mo1 V1 Mo2 71.10(3) . . ? Mo1 V1 Mo2 77.50(4) 7_454 . ? O1 V1 Mo2 121.03(4) . 7_454 ? O10 V1 Mo2 40.35(15) . 7_454 ? O10 V1 Mo2 104.55(19) 7_454 7_454 ? O9 V1 Mo2 116.21(18) . 7_454 ? O9 V1 Mo2 40.80(16) 7_454 7_454 ? Mo1 V1 Mo2 77.50(4) . 7_454 ? Mo1 V1 Mo2 71.10(3) 7_454 7_454 ? Mo2 V1 Mo2 117.95(7) . 7_454 ? O3 P1 O3 109.1(2) 12_667 7_454 ? O3 P1 O3 109.1(2) 12_667 . ? O3 P1 O3 110.2(4) 7_454 . ? O3 P1 O3 110.2(4) 12_667 14_556 ? O3 P1 O3 109.1(2) 7_454 14_556 ? O3 P1 O3 109.1(2) . 14_556 ? V1 O1 Cu1 180.0 . . ? Mo2 O2 V2 153.0(3) . 14_556 ? Mo2 O2 Mo3 153.0(3) . 14_556 ? V2 O2 Mo3 0.00(7) 14_556 14_556 ? P1 O3 Mo1 125.9(3) . . ? P1 O3 Mo2 124.6(3) . . ? Mo1 O3 Mo2 95.4(2) . . ? P1 O3 Mo3 126.1(3) . . ? Mo1 O3 Mo3 86.88(17) . . ? Mo2 O3 Mo3 86.19(17) . . ? Mo1 O4 V2 151.5(3) . 12_667 ? Mo1 O4 Mo3 151.5(3) . 12_667 ? V2 O4 Mo3 0.00(4) 12_667 12_667 ? Mo2 O5 Mo3 128.0(3) . . ? Mo1 O6 Mo3 125.4(3) . . ? V1 O9 Mo2 100.1(2) . . ? V1 O9 Mo1 99.5(2) . . ? Mo2 O9 Mo1 121.7(3) . . ? V1 O10 Mo1 102.7(2) . . ? V1 O10 Mo2 102.8(2) . 7_454 ? Mo1 O10 Mo2 141.4(3) . 7_454 ? C8 N1 C6 105.0(7) . . ? C8 N1 Cu1 129.0(6) . . ? C6 N1 Cu1 125.6(6) . . ? C3 N3 C18 108.0(9) . . ? C3 N3 C2 126.3(10) . . ? C18 N3 C2 125.7(8) . . ? C8 N5 C15 107.0(8) . . ? C8 N5 C26 126.7(8) . . ? C15 N5 C26 126.2(8) . . ? C3 N7 C10 109.4(9) . . ? C14 C1 C12 119.7(8) . . ? C14 C1 C2 119.5(7) . . ? C12 C1 C2 120.8(8) . . ? N3 C2 C1 112.8(7) . . ? N3 C2 H2A 109.0 . . ? C1 C2 H2A 109.0 . . ? N3 C2 H2B 109.0 . . ? C1 C2 H2B 109.0 . . ? H2A C2 H2B 107.8 . . ? N7 C3 N3 108.2(11) . . ? N7 C3 H3A 125.9 . . ? N3 C3 H3A 125.9 . . ? C15 C6 N1 108.3(9) . . ? C15 C6 H6A 125.9 . . ? N1 C6 H6A 125.9 . . ? N1 C8 N5 112.1(8) . . ? N1 C8 H8A 123.9 . . ? N5 C8 H8A 123.9 . . ? C18 C10 N7 107.2(11) . . ? C18 C10 H10A 126.4 . . ? N7 C10 H10A 126.4 . . ? C1 C12 C23 119.6(8) . . ? C1 C12 H12A 120.2 . . ? C23 C12 H12A 120.2 . . ? C1 C14 C17 120.7(8) . . ? C1 C14 H14A 119.7 . . ? C17 C14 H14A 119.7 . . ? N5 C15 C6 107.7(8) . . ? N5 C15 H15A 126.2 . . ? C6 C15 H15A 126.2 . . ? C14 C17 C25 120.5(8) . . ? C14 C17 H17A 119.7 . . ? C25 C17 H17A 119.7 . . ? C10 C18 N3 107.1(10) . . ? C10 C18 H18A 126.4 . . ? N3 C18 H18A 126.4 . . ? C25 C23 C12 120.9(8) . . ? C25 C23 H23A 119.5 . . ? C12 C23 H23A 119.5 . . ? C23 C25 C17 118.6(8) . . ? C23 C25 C26 120.9(8) . . ? C17 C25 C26 120.4(7) . . ? N5 C26 C25 112.8(7) . . ? N5 C26 H26A 109.0 . . ? C25 C26 H26A 109.0 . . ? N5 C26 H26B 109.0 . . ? C25 C26 H26B 109.0 . . ? H26A C26 H26B 107.8 . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 1.314 _refine_diff_density_min -0.838 _refine_diff_density_rms 0.170 # Attachment 'compound4.CIF' data_mmm _database_code_depnum_ccdc_archive 'CCDC 795843' #TrackingRef 'compound4.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C56 H64 Cu3 Mo12 N16 O44 P' _chemical_formula_weight 3038.10 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' 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' 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' P P 0.1023 0.0942 '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' _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 13.280(3) _cell_length_b 13.476(3) _cell_length_c 14.623(3) _cell_angle_alpha 109.29(3) _cell_angle_beta 116.85(3) _cell_angle_gamma 97.96(3) _cell_volume 2071.2(8) _cell_formula_units_Z 1 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 15429 _cell_measurement_theta_min 3.06 _cell_measurement_theta_max 25.00 _exptl_crystal_description block _exptl_crystal_colour black _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.436 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1470 _exptl_absorpt_coefficient_mu 2.625 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.497 _exptl_absorpt_correction_T_max 0.533 _exptl_absorpt_process_details 'ABSCOR by T.Higashi 8 March, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX area-detector diffractometer' _diffrn_measurement_method '\f and \w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 15429 _diffrn_reflns_av_R_equivalents 0.0273 _diffrn_reflns_av_sigmaI/netI 0.0375 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.06 _diffrn_reflns_theta_max 25.00 _reflns_number_total 7242 _reflns_number_gt 6706 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Rapid Auto' _computing_cell_refinement 'Rapid Auto' _computing_data_reduction 'Rapid Auto' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0388P)^2^+73.2589P] 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 7242 _refine_ls_number_parameters 616 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0717 _refine_ls_R_factor_gt 0.0657 _refine_ls_wR_factor_ref 0.1665 _refine_ls_wR_factor_gt 0.1639 _refine_ls_goodness_of_fit_ref 1.074 _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 0.39668(9) 0.15122(8) 0.16808(8) 0.0200(2) Uani 1 1 d . . . Mo2 Mo 0.70628(9) 0.22874(8) 0.26916(8) 0.0211(2) Uani 1 1 d . . . Mo3 Mo 0.43956(9) 0.02269(9) -0.25249(8) 0.0252(2) Uani 1 1 d . . . Mo4 Mo 0.18840(8) -0.06024(8) -0.11290(8) 0.0220(2) Uani 1 1 d . . . Mo5 Mo 0.36330(9) 0.19323(9) -0.06954(9) 0.0279(3) Uani 1 1 d . . . Mo6 Mo 0.66867(9) 0.24174(8) 0.01808(9) 0.0252(2) Uani 1 1 d . . . Cu1 Cu 0.5000 0.5000 0.0000 0.0266(5) Uani 1 2 d S . . Cu2 Cu 0.39604(14) 0.07013(12) 0.40820(13) 0.0328(4) Uani 1 1 d . . . P1 P 0.5000 0.0000 0.0000 0.0136(7) Uani 1 2 d S . . O22 O 0.5187(9) 0.2720(10) -0.0083(9) 0.067(4) Uani 1 1 d U . . O21 O 0.4009(11) 0.0476(11) -0.0009(11) 0.012(3) Uani 0.50 1 d P . . O20 O 0.4950(11) 0.0829(11) -0.0559(11) 0.009(3) Uani 0.50 1 d P . . O19 O 0.3571(8) 0.1057(10) -0.2080(9) 0.074(5) Uani 1 1 d . . . O18 O 0.5849(9) 0.1526(10) -0.1376(10) 0.066(3) Uani 1 1 d U . . O17 O 0.6779(8) 0.1109(9) 0.3105(10) 0.049(3) Uani 1 1 d . . . O16 O 0.8146(11) 0.1600(9) 0.2385(9) 0.052(3) Uani 1 1 d . . . O15 O 0.4476(7) 0.0591(8) 0.2369(9) 0.043(3) Uani 1 1 d . . . O14 O 0.2215(10) 0.0596(7) -0.1359(7) 0.052(3) Uani 1 1 d . . . O13 O 0.3784(9) 0.2238(7) 0.0708(7) 0.050(3) Uani 1 1 d . . . O12 O 0.8041(8) 0.3355(7) 0.3958(8) 0.042(2) Uani 1 1 d . . . O11 O 0.7044(12) 0.2930(9) 0.1751(10) 0.056(3) Uani 1 1 d . . . O10 O 0.3497(9) 0.2222(7) 0.2463(9) 0.044(3) Uani 1 1 d . . . O9 O 0.2568(10) 0.0362(8) 0.0467(7) 0.055(3) Uani 1 1 d . . . O8 O 0.2208(11) -0.1715(10) -0.0514(9) 0.055(3) Uani 1 1 d . . . O7 O 0.7440(8) 0.3586(6) 0.0292(7) 0.0272(18) Uani 1 1 d . . . O6 O 0.5631(7) 0.2438(9) 0.2505(10) 0.048(3) Uani 1 1 d . . . O5 O 0.4134(7) 0.0343(7) -0.3694(7) 0.0303(19) Uani 1 1 d . . . O4 O 0.0439(7) -0.0915(9) -0.1606(7) 0.039(2) Uani 1 1 d . . . O3 O 0.2924(8) 0.2777(7) -0.1069(7) 0.0312(19) Uani 1 1 d . . . O2 O 0.5305(11) 0.0672(10) 0.1223(11) 0.011(3) Uani 0.50 1 d P . . O1 O 0.6220(12) 0.0939(11) 0.0746(11) 0.014(3) Uani 0.50 1 d P . . OW1 O -0.0050(9) 0.6326(8) 0.6825(8) 0.043(2) Uani 1 1 d . . . OW2 O -0.1795(10) -0.2523(9) -0.3217(10) 0.061(3) Uani 1 1 d . . . N6 N 0.0630(8) -0.1239(8) 0.1373(8) 0.023(2) Uani 1 1 d . . . N5 N 0.2399(9) -0.0334(8) 0.2986(8) 0.030(2) Uani 1 1 d . . . N4 N 0.5459(8) 0.1807(8) 0.5246(8) 0.025(2) Uani 1 1 d . . . N3 N 0.7133(9) 0.2873(8) 0.6909(8) 0.025(2) Uani 1 1 d . . . N2 N 0.6134(8) 0.5548(8) 0.3230(7) 0.021(2) Uani 1 1 d . . . N1 N 0.5410(8) 0.5461(8) 0.1517(8) 0.023(2) Uani 1 1 d . . . C21 C 0.7241(11) 0.3084(11) 0.6086(11) 0.034(3) Uani 1 1 d . . . H21A H 0.7891 0.3593 0.6207 0.041 Uiso 1 1 calc R . . C20 C 0.7823(10) 0.5239(10) 0.8988(10) 0.030(3) Uani 1 1 d . . . H20A H 0.7128 0.4846 0.8902 0.036 Uiso 1 1 calc R . . C19 C 0.9497(11) 0.5267(10) 0.8797(10) 0.032(3) Uani 1 1 d . . . H19A H 0.9949 0.4890 0.8585 0.038 Uiso 1 1 calc R . . C18 C 0.8030(11) 0.3403(10) 0.8143(10) 0.032(3) Uani 1 1 d . . . H18A H 0.8713 0.3154 0.8275 0.038 Uiso 1 1 calc R . . H18B H 0.7685 0.3167 0.8529 0.038 Uiso 1 1 calc R . . C17 C 0.1558(11) -0.0715(11) 0.3219(11) 0.035(3) Uani 1 1 d . . . H17A H 0.1718 -0.0593 0.3943 0.041 Uiso 1 1 calc R . . C16 C 0.9879(10) 0.6417(10) 0.9257(10) 0.028(3) Uani 1 1 d . . . H16A H 1.0570 0.6804 0.9331 0.034 Uiso 1 1 calc R . . C15 C 0.0479(12) -0.1287(11) 0.2244(11) 0.036(3) Uani 1 1 d . . . H15A H -0.0228 -0.1643 0.2165 0.044 Uiso 1 1 calc R . . C14 C 0.1791(11) -0.0671(9) 0.1855(10) 0.030(3) Uani 1 1 d . . . H14A H 0.2130 -0.0530 0.1457 0.035 Uiso 1 1 calc R . . C13 C 0.6216(12) 0.2405(11) 0.5076(12) 0.038(3) Uani 1 1 d . . . H13A H 0.6051 0.2353 0.4369 0.046 Uiso 1 1 calc R . . C12 C 0.8454(9) 0.4660(9) 0.8644(9) 0.024(2) Uani 1 1 d . . . C11 C 0.8194(12) 0.6405(11) 0.9464(11) 0.034(3) Uani 1 1 d . . . H11A H 0.7750 0.6788 0.9685 0.041 Uiso 1 1 calc R . . C10 C 0.6037(10) 0.2108(9) 0.6361(10) 0.026(3) Uani 1 1 d . . . H10A H 0.5726 0.1827 0.6717 0.031 Uiso 1 1 calc R . . C7 C 0.5927(10) 0.6528(10) 0.3294(10) 0.026(3) Uani 1 1 d . . . H7A H 0.6060 0.7115 0.3939 0.032 Uiso 1 1 calc R . . C6 C 0.5775(10) 0.4914(10) 0.2136(10) 0.026(3) Uani 1 1 d . . . H6A H 0.5782 0.4189 0.1855 0.032 Uiso 1 1 calc R . . C5 C 0.5495(11) 0.6482(10) 0.2250(11) 0.029(3) Uani 1 1 d . . . H5A H 0.5286 0.7043 0.2049 0.035 Uiso 1 1 calc R . . C4 C 0.4541(12) 0.4876(12) 0.3899(10) 0.035(3) Uani 1 1 d . . . H4A H 0.4218 0.4777 0.3149 0.042 Uiso 1 1 calc R . . C3 C 0.6593(12) 0.5226(11) 0.4169(11) 0.032(3) Uani 1 1 d . . . H3A H 0.7364 0.5785 0.4802 0.038 Uiso 1 1 calc R . . H3B H 0.6718 0.4519 0.3912 0.038 Uiso 1 1 calc R . . C2 C 0.6198(12) 0.5218(11) 0.5691(10) 0.032(3) Uani 1 1 d . . . H2A H 0.7012 0.5352 0.6158 0.039 Uiso 1 1 calc R . . C1 C 0.5746(11) 0.5115(9) 0.4582(9) 0.024(2) Uani 1 1 d . . . N8 N 0.0939(9) 0.3005(8) -0.4216(8) 0.029(2) Uani 1 1 d . . . C28 C 0.0827(10) 0.4557(10) -0.3311(12) 0.034(3) Uani 1 1 d . . . H28A H 0.0645 0.5212 -0.3157 0.041 Uiso 1 1 calc R . . N7 N 0.1422(14) 0.4187(12) -0.2526(14) 0.067(4) Uani 1 1 d . . . C27 C 0.0554(11) 0.3842(11) -0.4312(12) 0.038(3) Uani 1 1 d . . . H27A H 0.0152 0.3909 -0.4988 0.046 Uiso 1 1 calc R . . C26 C 0.1492(11) 0.3207(10) -0.3099(10) 0.032(3) Uani 1 1 d . . . H26A H 0.1850 0.2758 -0.2788 0.038 Uiso 1 1 calc R . . C25 C 0.0796(12) 0.2014(10) -0.5158(10) 0.032(3) Uani 1 1 d . . . H25A H 0.1555 0.2093 -0.5117 0.038 Uiso 1 1 calc R . . H25B H 0.0209 0.1967 -0.5888 0.038 Uiso 1 1 calc R . . C24 C 0.1204(11) 0.0566(10) -0.4441(11) 0.032(3) Uani 1 1 d . . . H24A H 0.2022 0.0940 -0.4074 0.038 Uiso 1 1 calc R . . C23 C -0.0834(11) 0.0370(10) -0.5671(10) 0.029(3) Uani 1 1 d . . . H23A H -0.1395 0.0605 -0.6133 0.034 Uiso 1 1 calc R . . C22 C 0.0396(10) 0.0963(9) -0.5081(9) 0.024(2) Uani 1 1 d . . . C9 C 0.9681(11) 0.8256(10) 1.0145(11) 0.030(3) Uani 1 1 d . . . H9A H 0.9988 0.8518 0.9746 0.036 Uiso 1 1 calc R . . H9B H 0.9004 0.8501 1.0061 0.036 Uiso 1 1 calc R . . C8 C 0.9256(10) 0.6987(10) 0.9600(9) 0.025(2) 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 0.0251(5) 0.0205(5) 0.0206(5) 0.0094(4) 0.0159(4) 0.0105(4) Mo2 0.0224(5) 0.0185(5) 0.0148(4) 0.0051(4) 0.0070(4) 0.0034(4) Mo3 0.0200(5) 0.0396(6) 0.0151(5) 0.0122(4) 0.0094(4) 0.0073(4) Mo4 0.0132(4) 0.0279(5) 0.0249(5) 0.0141(4) 0.0088(4) 0.0063(4) Mo5 0.0237(5) 0.0239(5) 0.0273(5) 0.0084(4) 0.0072(4) 0.0147(4) Mo6 0.0267(5) 0.0163(5) 0.0364(6) 0.0087(4) 0.0228(5) 0.0028(4) Cu1 0.0293(11) 0.0322(11) 0.0196(10) 0.0128(9) 0.0139(9) 0.0076(9) Cu2 0.0286(8) 0.0222(7) 0.0261(8) -0.0007(6) 0.0090(7) -0.0002(6) P1 0.0148(18) 0.0125(17) 0.0137(17) 0.0062(15) 0.0073(15) 0.0050(15) O22 0.031(5) 0.076(7) 0.050(6) -0.023(4) 0.026(4) 0.011(4) O21 0.004(6) 0.020(7) 0.016(7) 0.013(6) 0.005(5) 0.003(5) O20 0.006(6) 0.013(7) 0.011(6) 0.007(5) 0.006(5) 0.000(5) O19 0.016(4) 0.083(8) 0.045(6) -0.044(6) 0.016(5) -0.006(5) O18 0.028(5) 0.070(6) 0.057(6) -0.019(5) 0.025(4) 0.012(4) O17 0.025(5) 0.059(6) 0.099(9) 0.068(7) 0.034(5) 0.024(5) O16 0.104(9) 0.065(7) 0.070(7) 0.059(6) 0.075(7) 0.074(7) O15 0.013(4) 0.038(5) 0.086(8) 0.051(5) 0.016(5) 0.010(4) O14 0.081(7) 0.027(5) 0.009(4) 0.009(4) 0.004(4) -0.021(5) O13 0.061(6) 0.026(5) 0.020(4) 0.015(4) -0.003(4) -0.023(4) O12 0.025(5) 0.029(5) 0.032(5) -0.006(4) -0.001(4) 0.010(4) O11 0.120(10) 0.066(7) 0.079(8) 0.065(7) 0.087(8) 0.081(7) O10 0.055(6) 0.024(5) 0.065(7) 0.004(4) 0.055(6) 0.005(4) O9 0.073(7) 0.029(5) 0.013(4) 0.012(4) -0.006(4) -0.022(5) O8 0.110(9) 0.077(8) 0.066(7) 0.062(6) 0.079(7) 0.078(7) O7 0.042(5) 0.015(4) 0.037(5) 0.010(4) 0.032(4) 0.007(3) O6 0.014(4) 0.063(7) 0.093(8) 0.068(7) 0.024(5) 0.016(4) O5 0.028(4) 0.042(5) 0.035(5) 0.028(4) 0.019(4) 0.014(4) O4 0.014(4) 0.070(7) 0.026(5) 0.018(5) 0.010(4) 0.011(4) O3 0.039(5) 0.032(5) 0.025(4) 0.018(4) 0.014(4) 0.016(4) O2 0.011(6) 0.009(6) 0.012(7) 0.005(5) 0.006(6) 0.002(5) O1 0.015(7) 0.015(7) 0.015(7) 0.012(6) 0.007(6) 0.001(6) OW1 0.048(6) 0.035(5) 0.047(6) 0.016(5) 0.025(5) 0.018(5) OW2 0.051(7) 0.046(6) 0.067(7) -0.005(6) 0.043(6) -0.003(5) N6 0.021(5) 0.020(5) 0.020(5) 0.007(4) 0.007(4) 0.003(4) N5 0.026(5) 0.023(5) 0.024(5) 0.003(4) 0.009(4) -0.004(4) N4 0.026(5) 0.020(5) 0.026(5) 0.006(4) 0.015(4) 0.008(4) N3 0.025(5) 0.017(5) 0.022(5) 0.005(4) 0.009(4) -0.003(4) N2 0.029(5) 0.020(5) 0.015(4) 0.006(4) 0.013(4) 0.008(4) N1 0.020(5) 0.020(5) 0.022(5) 0.004(4) 0.011(4) 0.005(4) C21 0.029(7) 0.030(7) 0.034(7) 0.013(6) 0.013(6) -0.002(5) C20 0.018(6) 0.024(6) 0.035(7) 0.004(5) 0.014(5) -0.003(5) C19 0.030(6) 0.031(7) 0.029(6) 0.005(5) 0.016(6) 0.013(5) C18 0.031(7) 0.028(7) 0.022(6) 0.005(5) 0.008(5) 0.009(5) C17 0.033(7) 0.037(7) 0.024(6) 0.005(6) 0.018(6) 0.001(6) C16 0.019(6) 0.035(7) 0.035(7) 0.016(6) 0.019(5) 0.005(5) C15 0.036(7) 0.037(7) 0.026(7) 0.006(6) 0.017(6) 0.004(6) C14 0.037(7) 0.017(6) 0.021(6) 0.003(5) 0.012(5) -0.002(5) C13 0.036(7) 0.040(8) 0.038(8) 0.018(6) 0.021(6) 0.009(6) C12 0.013(5) 0.019(6) 0.016(5) 0.003(4) -0.003(4) -0.005(4) C11 0.035(7) 0.031(7) 0.041(7) 0.006(6) 0.032(6) 0.008(6) C10 0.026(6) 0.020(6) 0.027(6) 0.005(5) 0.016(5) 0.000(5) C7 0.030(6) 0.022(6) 0.023(6) 0.003(5) 0.016(5) 0.007(5) C6 0.029(6) 0.027(6) 0.022(6) 0.012(5) 0.011(5) 0.012(5) C5 0.034(7) 0.024(6) 0.035(7) 0.014(5) 0.022(6) 0.009(5) C4 0.036(7) 0.052(8) 0.012(5) 0.013(6) 0.012(5) 0.013(6) C3 0.043(7) 0.037(7) 0.029(6) 0.019(6) 0.023(6) 0.023(6) C2 0.033(7) 0.039(7) 0.021(6) 0.019(6) 0.007(5) 0.013(6) C1 0.037(7) 0.017(5) 0.016(5) 0.007(4) 0.014(5) 0.008(5) N8 0.030(5) 0.023(5) 0.027(5) 0.014(4) 0.008(4) 0.012(4) C28 0.021(6) 0.014(6) 0.054(9) 0.008(6) 0.015(6) 0.005(5) N7 0.066(10) 0.039(8) 0.071(10) 0.001(7) 0.038(9) 0.001(7) C27 0.025(6) 0.035(7) 0.043(8) 0.022(7) 0.007(6) 0.007(6) C26 0.033(7) 0.027(6) 0.026(6) 0.012(5) 0.010(6) 0.008(5) C25 0.041(7) 0.027(6) 0.025(6) 0.014(5) 0.015(6) 0.009(6) C24 0.027(6) 0.030(7) 0.030(6) 0.009(5) 0.011(5) 0.010(5) C23 0.028(6) 0.025(6) 0.031(6) 0.015(5) 0.013(5) 0.008(5) C22 0.022(6) 0.023(6) 0.021(6) 0.007(5) 0.010(5) 0.007(5) C9 0.029(6) 0.023(6) 0.033(7) 0.016(5) 0.011(6) 0.007(5) C8 0.023(6) 0.031(6) 0.014(5) 0.007(5) 0.010(5) 0.002(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 Mo1 O10 1.643(8) . ? Mo1 O9 1.847(9) . ? Mo1 O15 1.858(8) . ? Mo1 O13 1.926(8) . ? Mo1 O6 1.931(8) . ? Mo1 O21 2.435(13) . ? Mo1 O2 2.454(13) . ? Mo2 O12 1.654(8) . ? Mo2 O6 1.845(8) . ? Mo2 O11 1.846(9) . ? Mo2 O17 1.925(8) . ? Mo2 O16 1.951(9) . ? Mo2 O2 2.403(13) . ? Mo2 O1 2.407(14) . ? Mo3 O5 1.650(8) . ? Mo3 O19 1.837(9) . ? Mo3 O17 1.847(9) 2_655 ? Mo3 O18 1.951(10) . ? Mo3 O15 1.957(9) 2_655 ? Mo3 O20 2.417(12) . ? Mo3 O2 2.495(13) 2_655 ? Mo4 O4 1.649(8) . ? Mo4 O14 1.791(8) . ? Mo4 O16 1.862(9) 2_655 ? Mo4 O9 1.928(9) . ? Mo4 O8 1.990(9) . ? Mo4 O21 2.424(12) . ? Mo4 O1 2.464(14) 2_655 ? Mo5 O3 1.651(8) . ? Mo5 O22 1.811(10) . ? Mo5 O13 1.863(9) . ? Mo5 O19 1.935(9) . ? Mo5 O14 1.997(9) . ? Mo5 O20 2.431(13) . ? Mo5 O21 2.496(13) . ? Mo6 O7 1.659(7) . ? Mo6 O8 1.825(9) 2_655 ? Mo6 O18 1.843(11) . ? Mo6 O11 1.962(10) . ? Mo6 O22 1.980(10) . ? Mo6 O20 2.433(12) . ? Mo6 O1 2.500(13) . ? Cu1 N1 1.873(9) 2_665 ? Cu1 N1 1.873(9) . ? Cu2 N4 1.876(10) . ? Cu2 N5 1.879(10) . ? P1 O1 1.529(13) . ? P1 O1 1.529(13) 2_655 ? P1 O2 1.535(13) . ? P1 O2 1.535(13) 2_655 ? P1 O21 1.538(13) 2_655 ? P1 O21 1.538(13) . ? P1 O20 1.581(12) . ? P1 O20 1.581(12) 2_655 ? O21 O2 1.742(17) . ? O21 O1 1.753(19) 2_655 ? O17 Mo3 1.847(9) 2_655 ? O16 Mo4 1.862(9) 2_655 ? O15 Mo3 1.957(9) 2_655 ? O8 Mo6 1.825(9) 2_655 ? O2 O1 1.702(18) . ? O2 Mo3 2.495(13) 2_655 ? O1 O21 1.753(19) 2_655 ? O1 Mo4 2.464(14) 2_655 ? N6 C14 1.340(15) . ? N6 C15 1.396(16) . ? N6 C9 1.479(15) 1_444 ? N5 C14 1.337(15) . ? N5 C17 1.390(16) . ? N4 C10 1.327(15) . ? N4 C13 1.362(16) . ? N3 C10 1.345(14) . ? N3 C21 1.386(16) . ? N3 C18 1.468(15) . ? N2 C6 1.345(14) . ? N2 C7 1.367(15) . ? N2 C3 1.469(15) . ? N1 C6 1.319(15) . ? N1 C5 1.389(15) . ? C21 C13 1.348(19) . ? C21 H21A 0.9300 . ? C20 C12 1.366(17) . ? C20 C11 1.396(17) . ? C20 H20A 0.9300 . ? C19 C16 1.377(17) . ? C19 C12 1.388(17) . ? C19 H19A 0.9300 . ? C18 C12 1.506(16) . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C17 C15 1.342(18) . ? C17 H17A 0.9300 . ? C16 C8 1.350(17) . ? C16 H16A 0.9300 . ? C15 H15A 0.9300 . ? C14 H14A 0.9300 . ? C13 H13A 0.9300 . ? C11 C8 1.406(16) . ? C11 H11A 0.9300 . ? C10 H10A 0.9300 . ? C7 C5 1.342(17) . ? C7 H7A 0.9300 . ? C6 H6A 0.9300 . ? C5 H5A 0.9300 . ? C4 C1 1.365(17) . ? C4 C2 1.373(18) 2_666 ? C4 H4A 0.9300 . ? C3 C1 1.510(17) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C2 C4 1.373(18) 2_666 ? C2 C1 1.400(15) . ? C2 H2A 0.9300 . ? N8 C27 1.325(16) . ? N8 C26 1.360(15) . ? N8 C25 1.482(16) . ? C28 C27 1.302(19) . ? C28 N7 1.36(2) . ? C28 H28A 0.9300 . ? N7 C26 1.352(19) . ? C27 H27A 0.9300 . ? C26 H26A 0.9300 . ? C25 C22 1.501(16) . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C24 C23 1.377(18) 2_554 ? C24 C22 1.378(17) . ? C24 H24A 0.9300 . ? C23 C24 1.377(18) 2_554 ? C23 C22 1.401(16) . ? C23 H23A 0.9300 . ? C9 N6 1.479(15) 1_666 ? C9 C8 1.519(16) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? 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 O9 102.1(5) . . ? O10 Mo1 O15 100.7(5) . . ? O9 Mo1 O15 92.0(4) . . ? O10 Mo1 O13 101.3(5) . . ? O9 Mo1 O13 88.1(4) . . ? O15 Mo1 O13 157.5(5) . . ? O10 Mo1 O6 101.8(5) . . ? O9 Mo1 O6 155.7(5) . . ? O15 Mo1 O6 87.9(3) . . ? O13 Mo1 O6 82.9(4) . . ? O10 Mo1 O21 159.3(5) . . ? O9 Mo1 O21 63.8(5) . . ? O15 Mo1 O21 95.0(5) . . ? O13 Mo1 O21 64.9(5) . . ? O6 Mo1 O21 92.0(5) . . ? O10 Mo1 O2 158.8(5) . . ? O9 Mo1 O2 95.2(5) . . ? O15 Mo1 O2 66.2(4) . . ? O13 Mo1 O2 91.4(5) . . ? O6 Mo1 O2 62.7(5) . . ? O21 Mo1 O2 41.8(4) . . ? O12 Mo2 O6 101.0(5) . . ? O12 Mo2 O11 100.0(6) . . ? O6 Mo2 O11 93.2(4) . . ? O12 Mo2 O17 101.8(5) . . ? O6 Mo2 O17 88.2(4) . . ? O11 Mo2 O17 157.5(5) . . ? O12 Mo2 O16 100.3(5) . . ? O6 Mo2 O16 158.3(5) . . ? O11 Mo2 O16 86.8(4) . . ? O17 Mo2 O16 83.8(4) . . ? O12 Mo2 O2 159.4(5) . . ? O6 Mo2 O2 64.8(5) . . ? O11 Mo2 O2 95.8(5) . . ? O17 Mo2 O2 64.5(4) . . ? O16 Mo2 O2 93.7(5) . . ? O12 Mo2 O1 159.1(5) . . ? O6 Mo2 O1 96.0(5) . . ? O11 Mo2 O1 66.7(5) . . ? O17 Mo2 O1 90.8(5) . . ? O16 Mo2 O1 64.1(5) . . ? O2 Mo2 O1 41.5(4) . . ? O5 Mo3 O19 101.9(6) . . ? O5 Mo3 O17 102.4(5) . 2_655 ? O19 Mo3 O17 92.5(5) . 2_655 ? O5 Mo3 O18 100.2(5) . . ? O19 Mo3 O18 87.2(4) . . ? O17 Mo3 O18 157.0(5) 2_655 . ? O5 Mo3 O15 100.9(4) . 2_655 ? O19 Mo3 O15 156.7(5) . 2_655 ? O17 Mo3 O15 87.6(4) 2_655 2_655 ? O18 Mo3 O15 83.7(4) . 2_655 ? O5 Mo3 O20 157.7(4) . . ? O19 Mo3 O20 64.0(5) . . ? O17 Mo3 O20 95.7(5) 2_655 . ? O18 Mo3 O20 63.6(5) . . ? O15 Mo3 O20 92.8(4) 2_655 . ? O5 Mo3 O2 158.3(4) . 2_655 ? O19 Mo3 O2 95.2(6) . 2_655 ? O17 Mo3 O2 63.3(4) 2_655 2_655 ? O18 Mo3 O2 93.7(5) . 2_655 ? O15 Mo3 O2 64.1(4) 2_655 2_655 ? O20 Mo3 O2 43.8(4) . 2_655 ? O4 Mo4 O14 103.0(5) . . ? O4 Mo4 O16 101.4(5) . 2_655 ? O14 Mo4 O16 95.0(4) . 2_655 ? O4 Mo4 O9 100.6(5) . . ? O14 Mo4 O9 89.9(4) . . ? O16 Mo4 O9 155.7(5) 2_655 . ? O4 Mo4 O8 98.8(5) . . ? O14 Mo4 O8 157.7(5) . . ? O16 Mo4 O8 85.6(4) 2_655 . ? O9 Mo4 O8 81.0(4) . . ? O4 Mo4 O21 159.7(5) . . ? O14 Mo4 O21 66.8(5) . . ? O16 Mo4 O21 97.1(5) 2_655 . ? O9 Mo4 O21 63.1(5) . . ? O8 Mo4 O21 90.9(5) . . ? O4 Mo4 O1 157.5(5) . 2_655 ? O14 Mo4 O1 95.5(5) . 2_655 ? O16 Mo4 O1 63.9(5) 2_655 2_655 ? O9 Mo4 O1 92.0(5) . 2_655 ? O8 Mo4 O1 64.7(4) . 2_655 ? O21 Mo4 O1 42.0(4) . 2_655 ? O3 Mo5 O22 102.8(5) . . ? O3 Mo5 O13 101.2(5) . . ? O22 Mo5 O13 95.0(5) . . ? O3 Mo5 O19 101.4(5) . . ? O22 Mo5 O19 88.5(4) . . ? O13 Mo5 O19 155.8(6) . . ? O3 Mo5 O14 99.2(5) . . ? O22 Mo5 O14 157.2(5) . . ? O13 Mo5 O14 86.4(4) . . ? O19 Mo5 O14 81.4(4) . . ? O3 Mo5 O20 158.9(4) . . ? O22 Mo5 O20 65.1(5) . . ? O13 Mo5 O20 97.2(5) . . ? O19 Mo5 O20 62.6(5) . . ? O14 Mo5 O20 92.2(5) . . ? O3 Mo5 O21 156.2(4) . . ? O22 Mo5 O21 97.3(5) . . ? O13 Mo5 O21 64.3(4) . . ? O19 Mo5 O21 91.5(6) . . ? O14 Mo5 O21 62.8(4) . . ? O20 Mo5 O21 44.2(4) . . ? O7 Mo6 O8 102.7(5) . 2_655 ? O7 Mo6 O18 101.4(5) . . ? O8 Mo6 O18 94.6(5) 2_655 . ? O7 Mo6 O11 100.0(4) . . ? O8 Mo6 O11 89.0(4) 2_655 . ? O18 Mo6 O11 156.9(5) . . ? O7 Mo6 O22 99.4(5) . . ? O8 Mo6 O22 157.3(6) 2_655 . ? O18 Mo6 O22 86.1(4) . . ? O11 Mo6 O22 82.0(5) . . ? O7 Mo6 O20 157.0(4) . . ? O8 Mo6 O20 96.7(5) 2_655 . ? O18 Mo6 O20 64.5(5) . . ? O11 Mo6 O20 92.4(5) . . ? O22 Mo6 O20 63.1(5) . . ? O7 Mo6 O1 158.6(4) . . ? O8 Mo6 O1 65.8(5) 2_655 . ? O18 Mo6 O1 97.5(5) . . ? O11 Mo6 O1 63.3(4) . . ? O22 Mo6 O1 91.6(5) . . ? O20 Mo6 O1 43.5(4) . . ? N1 Cu1 N1 180.0(2) 2_665 . ? N4 Cu2 N5 174.8(4) . . ? O1 P1 O1 180.0(16) . 2_655 ? O1 P1 O2 67.5(7) . . ? O1 P1 O2 112.5(7) 2_655 . ? O1 P1 O2 112.5(7) . 2_655 ? O1 P1 O2 67.5(7) 2_655 2_655 ? O2 P1 O2 180.0(9) . 2_655 ? O1 P1 O21 69.7(7) . 2_655 ? O1 P1 O21 110.3(7) 2_655 2_655 ? O2 P1 O21 110.9(7) . 2_655 ? O2 P1 O21 69.1(7) 2_655 2_655 ? O1 P1 O21 110.3(7) . . ? O1 P1 O21 69.7(7) 2_655 . ? O2 P1 O21 69.1(7) . . ? O2 P1 O21 110.9(7) 2_655 . ? O21 P1 O21 180.0(17) 2_655 . ? O1 P1 O20 72.1(6) . . ? O1 P1 O20 107.9(6) 2_655 . ? O2 P1 O20 107.9(7) . . ? O2 P1 O20 72.1(7) 2_655 . ? O21 P1 O20 107.1(6) 2_655 . ? O21 P1 O20 72.9(6) . . ? O1 P1 O20 107.9(6) . 2_655 ? O1 P1 O20 72.1(6) 2_655 2_655 ? O2 P1 O20 72.1(7) . 2_655 ? O2 P1 O20 107.9(7) 2_655 2_655 ? O21 P1 O20 72.9(6) 2_655 2_655 ? O21 P1 O20 107.1(6) . 2_655 ? O20 P1 O20 180.0(7) . 2_655 ? Mo5 O22 Mo6 138.0(7) . . ? P1 O21 O2 55.4(6) . . ? P1 O21 O1 54.9(6) . 2_655 ? O2 O21 O1 93.6(9) . 2_655 ? P1 O21 Mo4 125.0(7) . . ? O2 O21 Mo4 138.5(8) . . ? O1 O21 Mo4 70.2(6) 2_655 . ? P1 O21 Mo1 125.0(7) . . ? O2 O21 Mo1 69.7(6) . . ? O1 O21 Mo1 132.8(8) 2_655 . ? Mo4 O21 Mo1 93.2(4) . . ? P1 O21 Mo5 120.6(6) . . ? O2 O21 Mo5 125.0(8) . . ? O1 O21 Mo5 131.0(8) 2_655 . ? Mo4 O21 Mo5 91.9(4) . . ? Mo1 O21 Mo5 91.9(5) . . ? P1 O20 Mo3 123.0(7) . . ? P1 O20 Mo5 122.2(6) . . ? Mo3 O20 Mo5 93.6(4) . . ? P1 O20 Mo6 122.7(6) . . ? Mo3 O20 Mo6 93.8(4) . . ? Mo5 O20 Mo6 93.4(4) . . ? Mo3 O19 Mo5 139.1(7) . . ? Mo6 O18 Mo3 138.0(7) . . ? Mo3 O17 Mo2 139.2(6) 2_655 . ? Mo4 O16 Mo2 138.0(7) 2_655 . ? Mo1 O15 Mo3 137.5(6) . 2_655 ? Mo4 O14 Mo5 138.0(6) . . ? Mo5 O13 Mo1 138.7(6) . . ? Mo2 O11 Mo6 137.0(6) . . ? Mo1 O9 Mo4 138.6(7) . . ? Mo6 O8 Mo4 137.6(6) 2_655 . ? Mo2 O6 Mo1 138.6(7) . . ? P1 O2 O1 56.1(6) . . ? P1 O2 O21 55.5(6) . . ? O1 O2 O21 93.9(9) . . ? P1 O2 Mo2 125.4(7) . . ? O1 O2 Mo2 69.4(6) . . ? O21 O2 Mo2 132.1(8) . . ? P1 O2 Mo1 124.0(7) . . ? O1 O2 Mo1 137.2(8) . . ? O21 O2 Mo1 68.5(6) . . ? Mo2 O2 Mo1 93.3(4) . . ? P1 O2 Mo3 120.8(7) . 2_655 ? O1 O2 Mo3 126.4(8) . 2_655 ? O21 O2 Mo3 130.4(8) . 2_655 ? Mo2 O2 Mo3 92.4(4) . 2_655 ? Mo1 O2 Mo3 91.9(4) . 2_655 ? P1 O1 O2 56.4(6) . . ? P1 O1 O21 55.4(6) . 2_655 ? O2 O1 O21 94.2(9) . 2_655 ? P1 O1 Mo2 125.5(7) . . ? O2 O1 Mo2 69.2(6) . . ? O21 O1 Mo2 137.8(8) 2_655 . ? P1 O1 Mo4 123.1(8) . 2_655 ? O2 O1 Mo4 131.4(8) . 2_655 ? O21 O1 Mo4 67.8(6) 2_655 2_655 ? Mo2 O1 Mo4 93.9(5) . 2_655 ? P1 O1 Mo6 121.4(7) . . ? O2 O1 Mo6 132.7(8) . . ? O21 O1 Mo6 124.3(8) 2_655 . ? Mo2 O1 Mo6 92.4(5) . . ? Mo4 O1 Mo6 91.6(4) 2_655 . ? C14 N6 C15 107.3(10) . . ? C14 N6 C9 126.8(10) . 1_444 ? C15 N6 C9 125.9(10) . 1_444 ? C14 N5 C17 105.4(10) . . ? C14 N5 Cu2 127.7(9) . . ? C17 N5 Cu2 125.6(8) . . ? C10 N4 C13 106.2(10) . . ? C10 N4 Cu2 128.5(8) . . ? C13 N4 Cu2 125.1(9) . . ? C10 N3 C21 106.7(10) . . ? C10 N3 C18 126.8(10) . . ? C21 N3 C18 126.5(10) . . ? C6 N2 C7 107.3(9) . . ? C6 N2 C3 126.6(10) . . ? C7 N2 C3 126.0(9) . . ? C6 N1 C5 105.9(10) . . ? C6 N1 Cu1 126.7(8) . . ? C5 N1 Cu1 127.3(8) . . ? C13 C21 N3 106.3(11) . . ? C13 C21 H21A 126.8 . . ? N3 C21 H21A 126.8 . . ? C12 C20 C11 121.8(11) . . ? C12 C20 H20A 119.1 . . ? C11 C20 H20A 119.1 . . ? C16 C19 C12 121.5(11) . . ? C16 C19 H19A 119.3 . . ? C12 C19 H19A 119.3 . . ? N3 C18 C12 112.1(10) . . ? N3 C18 H18A 109.2 . . ? C12 C18 H18A 109.2 . . ? N3 C18 H18B 109.2 . . ? C12 C18 H18B 109.2 . . ? H18A C18 H18B 107.9 . . ? C15 C17 N5 109.9(11) . . ? C15 C17 H17A 125.0 . . ? N5 C17 H17A 125.0 . . ? C8 C16 C19 120.4(11) . . ? C8 C16 H16A 119.8 . . ? C19 C16 H16A 119.8 . . ? C17 C15 N6 106.2(11) . . ? C17 C15 H15A 126.9 . . ? N6 C15 H15A 126.9 . . ? N5 C14 N6 111.1(11) . . ? N5 C14 H14A 124.4 . . ? N6 C14 H14A 124.4 . . ? C21 C13 N4 109.8(12) . . ? C21 C13 H13A 125.1 . . ? N4 C13 H13A 125.1 . . ? C20 C12 C19 117.9(11) . . ? C20 C12 C18 120.2(11) . . ? C19 C12 C18 121.8(11) . . ? C20 C11 C8 118.4(11) . . ? C20 C11 H11A 120.8 . . ? C8 C11 H11A 120.8 . . ? N4 C10 N3 111.0(10) . . ? N4 C10 H10A 124.5 . . ? N3 C10 H10A 124.5 . . ? C5 C7 N2 107.1(10) . . ? C5 C7 H7A 126.5 . . ? N2 C7 H7A 126.5 . . ? N1 C6 N2 110.8(10) . . ? N1 C6 H6A 124.6 . . ? N2 C6 H6A 124.6 . . ? C7 C5 N1 108.9(11) . . ? C7 C5 H5A 125.6 . . ? N1 C5 H5A 125.6 . . ? C1 C4 C2 120.6(11) . 2_666 ? C1 C4 H4A 119.7 . . ? C2 C4 H4A 119.7 2_666 . ? N2 C3 C1 112.3(10) . . ? N2 C3 H3A 109.2 . . ? C1 C3 H3A 109.2 . . ? N2 C3 H3B 109.2 . . ? C1 C3 H3B 109.2 . . ? H3A C3 H3B 107.9 . . ? C4 C2 C1 121.0(12) 2_666 . ? C4 C2 H2A 119.5 2_666 . ? C1 C2 H2A 119.5 . . ? C4 C1 C2 118.3(11) . . ? C4 C1 C3 122.5(10) . . ? C2 C1 C3 119.1(11) . . ? C27 N8 C26 108.3(11) . . ? C27 N8 C25 126.2(11) . . ? C26 N8 C25 125.5(10) . . ? C27 C28 N7 108.8(12) . . ? C27 C28 H28A 125.6 . . ? N7 C28 H28A 125.6 . . ? C26 N7 C28 106.8(13) . . ? C28 C27 N8 109.2(12) . . ? C28 C27 H27A 125.4 . . ? N8 C27 H27A 125.4 . . ? N7 C26 N8 106.8(12) . . ? N7 C26 H26A 126.6 . . ? N8 C26 H26A 126.6 . . ? N8 C25 C22 110.6(10) . . ? N8 C25 H25A 109.5 . . ? C22 C25 H25A 109.5 . . ? N8 C25 H25B 109.5 . . ? C22 C25 H25B 109.5 . . ? H25A C25 H25B 108.1 . . ? C23 C24 C22 121.8(12) 2_554 . ? C23 C24 H24A 119.1 2_554 . ? C22 C24 H24A 119.1 . . ? C24 C23 C22 119.3(11) 2_554 . ? C24 C23 H23A 120.3 2_554 . ? C22 C23 H23A 120.3 . . ? C24 C22 C23 118.9(11) . . ? C24 C22 C25 121.9(11) . . ? C23 C22 C25 119.3(11) . . ? N6 C9 C8 112.2(9) 1_666 . ? N6 C9 H9A 109.2 1_666 . ? C8 C9 H9A 109.2 . . ? N6 C9 H9B 109.2 1_666 . ? C8 C9 H9B 109.2 . . ? H9A C9 H9B 107.9 . . ? C16 C8 C11 120.1(11) . . ? C16 C8 C9 121.3(11) . . ? C11 C8 C9 118.6(11) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 1.389 _refine_diff_density_min -0.905 _refine_diff_density_rms 0.190