Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2004 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Jon Zubieta' _publ_contact_author_address ; Department of Chemistry 111 College Place Syracuse University Syracuse, NY 13244 ; _publ_contact_author_email jazubiet@syr.edu _publ_contact_author_phone (315)443-2547 _publ_contact_author_fax (315)443-4070 _publ_section_title ; Solid State Coordination Chemistry: Structural Consequences of Variations in Tether Length in the Oxovanadium-Copper-Bisterpy- {O3P(CH2)nPO3}4- System, n = 1 through 6 (bisterpy = 2,2':4',4'':2'',2'''-quarterpyridyl, 6',6''-di-2 pyridine). ; loop_ _publ_author_name 'Jon Zubieta' 'Eric Burkholder' 'Vladimir Golub' 'Bon-Kweon Koo' C.O'Connor 'Wayne Ouellette' data_Compound_1 _database_code_depnum_ccdc_archive 'CCDC 229550' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H13 Cu N3 O8 P2 V' _chemical_formula_weight 551.71 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' 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' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.7077(6) _cell_length_b 13.1843(8) _cell_length_c 13.3464(8) _cell_angle_alpha 90.00 _cell_angle_beta 98.373(1) _cell_angle_gamma 90.00 _cell_volume 1864.07(19) _cell_formula_units_Z 4 _cell_measurement_temperature 90(2) _cell_measurement_reflns_used 22574 _cell_measurement_theta_min 2.18 _cell_measurement_theta_max 30.51 _exptl_crystal_description plate _exptl_crystal_colour green _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.966 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1104 _exptl_absorpt_coefficient_mu 1.869 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details 'SADABS SHELXL-97 (SHELDRICK, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 90(2) _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_probe x-ray _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'APEX CCD area detector' _diffrn_measurement_method 'Phi and omega scans' _diffrn_detector_area_resol_mean 512 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.001 _diffrn_reflns_number 22574 _diffrn_reflns_av_R_equivalents 0.0627 _diffrn_reflns_av_sigmaI/netI 0.0590 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.18 _diffrn_reflns_theta_max 30.51 _reflns_number_total 5690 _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 and CrystalMaker 5.x' _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^)+(0.0581P)^2^+3.4834P] 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 5690 _refine_ls_number_parameters 289 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0747 _refine_ls_R_factor_gt 0.0508 _refine_ls_wR_factor_ref 0.1300 _refine_ls_wR_factor_gt 0.1197 _refine_ls_goodness_of_fit_ref 1.054 _refine_ls_restrained_S_all 1.054 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.04946(4) 0.04993(3) 0.13652(3) 0.00868(10) Uani 1 1 d . . . V1 V -0.16336(6) -0.10271(5) 0.40620(5) 0.01406(14) Uani 1 1 d . . . P1 P -0.20873(8) 0.05609(7) 0.22001(7) 0.01066(17) Uani 1 1 d . . . P2 P 0.01738(8) 0.08495(7) 0.37013(7) 0.00976(17) Uani 1 1 d . . . O1 O -0.1310(2) 0.05846(19) 0.13341(18) 0.0102(5) Uani 1 1 d . . . O2 O -0.2259(3) -0.0472(2) 0.2643(2) 0.0177(5) Uani 1 1 d . . . O3 O 0.1053(2) 0.09191(19) 0.29205(18) 0.0114(5) Uani 1 1 d . . . O4 O -0.0100(2) -0.02641(19) 0.39389(19) 0.0145(5) Uani 1 1 d . . . O5 O -0.0606(2) -0.14758(19) 0.53410(18) 0.0122(5) Uani 1 1 d . . . O6 O -0.1977(3) -0.2193(2) 0.3702(2) 0.0228(6) Uani 1 1 d . . . O7 O -0.2792(3) -0.0557(2) 0.4555(2) 0.0235(6) Uani 1 1 d . . . O8 O -0.3432(2) 0.1000(2) 0.1835(2) 0.0141(5) Uani 1 1 d . . . H8 H -0.3367 0.1596 0.1627 0.021 Uiso 1 1 calc R . . N1 N 0.0904(3) 0.1978(2) 0.1014(2) 0.0102(5) Uani 1 1 d . . . N2 N 0.2149(3) 0.0336(2) 0.0958(2) 0.0097(5) Uani 1 1 d . . . N3 N 0.0600(3) -0.1040(2) 0.1332(2) 0.0097(5) Uani 1 1 d . . . C1 C 0.0208(3) 0.2791(3) 0.1174(3) 0.0137(7) Uani 1 1 d . . . H1 H -0.0654 0.2700 0.1247 0.016 Uiso 1 1 calc R . . C2 C 0.0711(4) 0.3760(3) 0.1236(3) 0.0195(8) Uani 1 1 d . . . H2 H 0.0199 0.4326 0.1347 0.023 Uiso 1 1 calc R . . C3 C 0.1972(4) 0.3893(3) 0.1135(3) 0.0184(8) Uani 1 1 d . . . H3 H 0.2345 0.4548 0.1202 0.022 Uiso 1 1 calc R . . C4 C 0.2681(3) 0.3057(3) 0.0933(3) 0.0149(7) Uani 1 1 d . . . H4 H 0.3537 0.3133 0.0832 0.018 Uiso 1 1 calc R . . C5 C 0.2124(3) 0.2113(3) 0.0881(3) 0.0111(6) Uani 1 1 d . . . C6 C 0.2785(3) 0.1148(3) 0.0715(3) 0.0107(6) Uani 1 1 d . . . C7 C 0.3919(3) 0.1051(3) 0.0336(3) 0.0112(6) Uani 1 1 d . . . H7 H 0.4360 0.1635 0.0158 0.013 Uiso 1 1 calc R . . C8 C 0.4404(3) 0.0074(3) 0.0220(2) 0.0103(6) Uani 1 1 d . . . C9 C 0.3732(3) -0.0760(3) 0.0505(3) 0.0100(6) Uani 1 1 d . . . H9 H 0.4052 -0.1427 0.0458 0.012 Uiso 1 1 calc R . . C10 C 0.2588(3) -0.0601(3) 0.0860(2) 0.0087(6) Uani 1 1 d . . . C11 C 0.1721(3) -0.1401(3) 0.1118(3) 0.0105(6) Uani 1 1 d . . . C12 C 0.2011(3) -0.2422(3) 0.1143(3) 0.0148(7) Uani 1 1 d . . . H12 H 0.2805 -0.2652 0.0996 0.018 Uiso 1 1 calc R . . C13 C 0.1116(4) -0.3103(3) 0.1389(3) 0.0181(8) Uani 1 1 d . . . H13 H 0.1290 -0.3810 0.1414 0.022 Uiso 1 1 calc R . . C14 C -0.0029(4) -0.2743(3) 0.1597(3) 0.0173(7) Uani 1 1 d . . . H14 H -0.0655 -0.3199 0.1764 0.021 Uiso 1 1 calc R . . C15 C -0.0252(3) -0.1712(3) 0.1560(3) 0.0138(7) Uani 1 1 d . . . H15 H -0.1043 -0.1469 0.1702 0.017 Uiso 1 1 calc R . . C16 C -0.1348(3) 0.1372(3) 0.3192(3) 0.0143(7) Uani 1 1 d . . . H16A H -0.124(4) 0.205(3) 0.299(3) 0.002(9) Uiso 1 1 d . . . H16B H -0.186(5) 0.145(4) 0.368(4) 0.027(13) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.00626(18) 0.00937(19) 0.01111(19) 0.00008(15) 0.00366(14) 0.00126(15) V1 0.0135(3) 0.0142(3) 0.0146(3) -0.0013(2) 0.0023(2) -0.0032(2) P1 0.0069(4) 0.0145(4) 0.0108(4) 0.0004(3) 0.0023(3) 0.0022(3) P2 0.0079(4) 0.0126(4) 0.0088(4) 0.0012(3) 0.0013(3) -0.0026(3) O1 0.0064(10) 0.0149(12) 0.0096(11) -0.0002(9) 0.0022(8) 0.0015(9) O2 0.0175(13) 0.0168(13) 0.0201(13) 0.0035(11) 0.0072(11) 0.0000(11) O3 0.0092(11) 0.0158(12) 0.0094(11) 0.0000(9) 0.0016(9) -0.0017(9) O4 0.0164(12) 0.0133(12) 0.0137(12) 0.0026(10) 0.0013(10) -0.0055(10) O5 0.0126(12) 0.0137(12) 0.0101(11) -0.0005(9) 0.0011(9) -0.0033(9) O6 0.0311(16) 0.0169(14) 0.0179(14) -0.0007(11) -0.0047(12) -0.0122(12) O7 0.0195(14) 0.0322(17) 0.0199(14) -0.0008(12) 0.0066(11) 0.0016(12) O8 0.0076(11) 0.0188(13) 0.0159(12) -0.0027(10) 0.0011(9) 0.0049(10) N1 0.0101(13) 0.0116(13) 0.0097(13) 0.0003(11) 0.0041(10) 0.0028(11) N2 0.0077(12) 0.0118(14) 0.0101(13) -0.0011(10) 0.0030(10) 0.0017(10) N3 0.0102(13) 0.0094(13) 0.0104(13) -0.0006(11) 0.0052(10) 0.0002(10) C1 0.0131(16) 0.0123(16) 0.0162(17) 0.0018(13) 0.0044(13) 0.0026(13) C2 0.0192(19) 0.0113(17) 0.029(2) 0.0022(15) 0.0062(16) 0.0047(14) C3 0.0195(18) 0.0099(16) 0.027(2) 0.0021(14) 0.0063(15) 0.0010(14) C4 0.0119(16) 0.0137(16) 0.0201(18) 0.0027(14) 0.0062(13) 0.0024(13) C5 0.0099(15) 0.0124(16) 0.0117(15) 0.0007(12) 0.0043(12) 0.0005(12) C6 0.0089(14) 0.0111(15) 0.0124(15) -0.0014(12) 0.0025(12) 0.0014(12) C7 0.0082(14) 0.0132(16) 0.0129(15) -0.0021(13) 0.0036(12) -0.0011(12) C8 0.0055(14) 0.0157(16) 0.0098(14) 0.0003(12) 0.0018(11) 0.0008(12) C9 0.0088(14) 0.0090(15) 0.0124(15) 0.0003(12) 0.0028(12) 0.0010(11) C10 0.0075(14) 0.0097(15) 0.0090(14) -0.0020(12) 0.0013(11) -0.0010(11) C11 0.0097(15) 0.0134(16) 0.0091(14) 0.0008(12) 0.0041(12) -0.0014(12) C12 0.0152(16) 0.0098(16) 0.0215(18) -0.0015(13) 0.0103(14) 0.0029(13) C13 0.0221(19) 0.0093(16) 0.026(2) 0.0026(14) 0.0126(16) 0.0011(14) C14 0.0174(18) 0.0145(17) 0.0227(19) 0.0014(14) 0.0118(15) -0.0025(14) C15 0.0114(16) 0.0149(17) 0.0165(17) 0.0015(13) 0.0071(13) -0.0005(13) C16 0.0132(16) 0.0186(18) 0.0107(16) -0.0021(13) 0.0001(13) 0.0016(13) _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 O1 1.930(2) . ? Cu1 N2 1.939(3) . ? Cu1 N3 2.034(3) . ? Cu1 N1 2.067(3) . ? Cu1 O3 2.147(2) . ? V1 O7 1.611(3) . ? V1 O6 1.636(3) . ? V1 O4 1.953(3) . ? V1 O5 1.982(3) . ? V1 O2 2.050(3) . ? P1 O2 1.506(3) . ? P1 O1 1.519(2) . ? P1 O8 1.562(3) . ? P1 C16 1.793(4) . ? P2 O3 1.505(2) . ? P2 O5 1.536(3) 3_556 ? P2 O4 1.539(3) . ? P2 C16 1.809(4) . ? O5 P2 1.536(3) 3_556 ? N1 C1 1.340(4) . ? N1 C5 1.355(4) . ? N2 C10 1.334(4) . ? N2 C6 1.335(4) . ? N3 C15 1.338(4) . ? N3 C11 1.359(4) . ? C1 C2 1.384(5) . ? C2 C3 1.388(5) . ? C3 C4 1.387(5) . ? C4 C5 1.377(5) . ? C5 C6 1.488(5) . ? C6 C7 1.387(5) . ? C7 C8 1.406(5) . ? C8 C9 1.397(5) . ? C8 C8 1.494(6) 3_655 ? C9 C10 1.392(4) . ? C10 C11 1.479(5) . ? C11 C12 1.380(5) . ? C12 C13 1.387(5) . ? C13 C14 1.380(5) . ? C14 C15 1.380(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Cu1 N2 162.40(11) . . ? O1 Cu1 N3 96.69(11) . . ? N2 Cu1 N3 80.03(12) . . ? O1 Cu1 N1 100.66(11) . . ? N2 Cu1 N1 78.97(12) . . ? N3 Cu1 N1 157.22(11) . . ? O1 Cu1 O3 98.20(10) . . ? N2 Cu1 O3 99.33(11) . . ? N3 Cu1 O3 105.65(11) . . ? N1 Cu1 O3 86.44(10) . . ? O7 V1 O6 109.15(16) . . ? O7 V1 O4 122.89(14) . . ? O6 V1 O4 127.96(14) . . ? O7 V1 O5 97.28(13) . . ? O6 V1 O5 92.62(13) . . ? O4 V1 O5 81.85(11) . . ? O7 V1 O2 94.16(13) . . ? O6 V1 O2 91.98(13) . . ? O4 V1 O2 84.49(11) . . ? O5 V1 O2 165.51(11) . . ? O2 P1 O1 115.39(15) . . ? O2 P1 O8 107.30(15) . . ? O1 P1 O8 109.70(14) . . ? O2 P1 C16 108.41(17) . . ? O1 P1 C16 108.51(16) . . ? O8 P1 C16 107.24(16) . . ? O3 P2 O5 113.60(14) . 3_556 ? O3 P2 O4 110.98(15) . . ? O5 P2 O4 112.64(14) 3_556 . ? O3 P2 C16 109.66(16) . . ? O5 P2 C16 104.72(16) 3_556 . ? O4 P2 C16 104.62(17) . . ? P1 O1 Cu1 129.78(15) . . ? P1 O2 V1 130.01(17) . . ? P2 O3 Cu1 122.64(14) . . ? P2 O4 V1 134.16(17) . . ? P2 O5 V1 128.23(16) 3_556 . ? C1 N1 C5 119.0(3) . . ? C1 N1 Cu1 125.2(2) . . ? C5 N1 Cu1 113.2(2) . . ? C10 N2 C6 121.3(3) . . ? C10 N2 Cu1 118.7(2) . . ? C6 N2 Cu1 119.9(2) . . ? C15 N3 C11 117.9(3) . . ? C15 N3 Cu1 127.8(2) . . ? C11 N3 Cu1 114.1(2) . . ? N1 C1 C2 121.8(3) . . ? C1 C2 C3 119.1(3) . . ? C4 C3 C2 119.1(4) . . ? C5 C4 C3 118.8(3) . . ? N1 C5 C4 122.1(3) . . ? N1 C5 C6 113.3(3) . . ? C4 C5 C6 124.6(3) . . ? N2 C6 C7 121.3(3) . . ? N2 C6 C5 112.3(3) . . ? C7 C6 C5 126.4(3) . . ? C6 C7 C8 118.8(3) . . ? C9 C8 C7 118.6(3) . . ? C9 C8 C8 120.5(4) . 3_655 ? C7 C8 C8 120.9(4) . 3_655 ? C10 C9 C8 119.2(3) . . ? N2 C10 C9 120.9(3) . . ? N2 C10 C11 113.3(3) . . ? C9 C10 C11 125.8(3) . . ? N3 C11 C12 122.6(3) . . ? N3 C11 C10 113.7(3) . . ? C12 C11 C10 123.7(3) . . ? C11 C12 C13 118.5(3) . . ? C14 C13 C12 119.3(3) . . ? C15 C14 C13 119.0(3) . . ? N3 C15 C14 122.7(3) . . ? P1 C16 P2 109.1(2) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 P1 O1 Cu1 -77.0(2) . . . . ? O8 P1 O1 Cu1 161.69(18) . . . . ? C16 P1 O1 Cu1 44.8(2) . . . . ? N2 Cu1 O1 P1 165.0(3) . . . . ? N3 Cu1 O1 P1 87.0(2) . . . . ? N1 Cu1 O1 P1 -107.8(2) . . . . ? O3 Cu1 O1 P1 -19.9(2) . . . . ? O1 P1 O2 V1 115.0(2) . . . . ? O8 P1 O2 V1 -122.4(2) . . . . ? C16 P1 O2 V1 -6.8(3) . . . . ? O7 V1 O2 P1 83.3(2) . . . . ? O6 V1 O2 P1 -167.3(2) . . . . ? O4 V1 O2 P1 -39.4(2) . . . . ? O5 V1 O2 P1 -58.8(5) . . . . ? O5 P2 O3 Cu1 -162.31(15) 3_556 . . . ? O4 P2 O3 Cu1 69.6(2) . . . . ? C16 P2 O3 Cu1 -45.5(2) . . . . ? O1 Cu1 O3 P2 19.93(19) . . . . ? N2 Cu1 O3 P2 -161.59(18) . . . . ? N3 Cu1 O3 P2 -79.42(18) . . . . ? N1 Cu1 O3 P2 120.21(18) . . . . ? O3 P2 O4 V1 -133.2(2) . . . . ? O5 P2 O4 V1 98.2(2) 3_556 . . . ? C16 P2 O4 V1 -15.0(3) . . . . ? O7 V1 O4 P2 -37.2(3) . . . . ? O6 V1 O4 P2 142.4(2) . . . . ? O5 V1 O4 P2 -130.6(2) . . . . ? O2 V1 O4 P2 54.2(2) . . . . ? O7 V1 O5 P2 -53.0(2) . . . 3_556 ? O6 V1 O5 P2 -162.7(2) . . . 3_556 ? O4 V1 O5 P2 69.32(19) . . . 3_556 ? O2 V1 O5 P2 88.9(5) . . . 3_556 ? O1 Cu1 N1 C1 24.9(3) . . . . ? N2 Cu1 N1 C1 -173.0(3) . . . . ? N3 Cu1 N1 C1 163.9(3) . . . . ? O3 Cu1 N1 C1 -72.8(3) . . . . ? O1 Cu1 N1 C5 -173.6(2) . . . . ? N2 Cu1 N1 C5 -11.5(2) . . . . ? N3 Cu1 N1 C5 -34.7(4) . . . . ? O3 Cu1 N1 C5 88.7(2) . . . . ? O1 Cu1 N2 C10 -81.4(5) . . . . ? N3 Cu1 N2 C10 -0.8(2) . . . . ? N1 Cu1 N2 C10 -171.9(3) . . . . ? O3 Cu1 N2 C10 103.6(3) . . . . ? O1 Cu1 N2 C6 93.9(4) . . . . ? N3 Cu1 N2 C6 174.5(3) . . . . ? N1 Cu1 N2 C6 3.4(3) . . . . ? O3 Cu1 N2 C6 -81.1(3) . . . . ? O1 Cu1 N3 C15 -18.9(3) . . . . ? N2 Cu1 N3 C15 178.6(3) . . . . ? N1 Cu1 N3 C15 -158.4(3) . . . . ? O3 Cu1 N3 C15 81.6(3) . . . . ? O1 Cu1 N3 C11 166.0(2) . . . . ? N2 Cu1 N3 C11 3.5(2) . . . . ? N1 Cu1 N3 C11 26.5(5) . . . . ? O3 Cu1 N3 C11 -93.5(2) . . . . ? C5 N1 C1 C2 -1.8(5) . . . . ? Cu1 N1 C1 C2 158.6(3) . . . . ? N1 C1 C2 C3 -0.3(6) . . . . ? C1 C2 C3 C4 2.6(6) . . . . ? C2 C3 C4 C5 -2.6(6) . . . . ? C1 N1 C5 C4 1.8(5) . . . . ? Cu1 N1 C5 C4 -160.9(3) . . . . ? C1 N1 C5 C6 179.7(3) . . . . ? Cu1 N1 C5 C6 17.0(4) . . . . ? C3 C4 C5 N1 0.5(6) . . . . ? C3 C4 C5 C6 -177.3(4) . . . . ? C10 N2 C6 C7 0.9(5) . . . . ? Cu1 N2 C6 C7 -174.3(3) . . . . ? C10 N2 C6 C5 179.9(3) . . . . ? Cu1 N2 C6 C5 4.7(4) . . . . ? N1 C5 C6 N2 -14.4(4) . . . . ? C4 C5 C6 N2 163.5(3) . . . . ? N1 C5 C6 C7 164.4(3) . . . . ? C4 C5 C6 C7 -17.7(6) . . . . ? N2 C6 C7 C8 -0.7(5) . . . . ? C5 C6 C7 C8 -179.4(3) . . . . ? C6 C7 C8 C9 -0.9(5) . . . . ? C6 C7 C8 C8 177.7(4) . . . 3_655 ? C7 C8 C9 C10 2.2(5) . . . . ? C8 C8 C9 C10 -176.4(4) 3_655 . . . ? C6 N2 C10 C9 0.4(5) . . . . ? Cu1 N2 C10 C9 175.7(2) . . . . ? C6 N2 C10 C11 -177.0(3) . . . . ? Cu1 N2 C10 C11 -1.8(4) . . . . ? C8 C9 C10 N2 -2.0(5) . . . . ? C8 C9 C10 C11 175.1(3) . . . . ? C15 N3 C11 C12 -1.1(5) . . . . ? Cu1 N3 C11 C12 174.5(3) . . . . ? C15 N3 C11 C10 179.1(3) . . . . ? Cu1 N3 C11 C10 -5.3(4) . . . . ? N2 C10 C11 N3 4.7(4) . . . . ? C9 C10 C11 N3 -172.6(3) . . . . ? N2 C10 C11 C12 -175.2(3) . . . . ? C9 C10 C11 C12 7.5(6) . . . . ? N3 C11 C12 C13 0.6(6) . . . . ? C10 C11 C12 C13 -179.6(3) . . . . ? C11 C12 C13 C14 0.1(6) . . . . ? C12 C13 C14 C15 -0.3(6) . . . . ? C11 N3 C15 C14 0.9(5) . . . . ? Cu1 N3 C15 C14 -174.0(3) . . . . ? C13 C14 C15 N3 -0.2(6) . . . . ? O2 P1 C16 P2 60.6(2) . . . . ? O1 P1 C16 P2 -65.4(2) . . . . ? O8 P1 C16 P2 176.16(17) . . . . ? O3 P2 C16 P1 68.1(2) . . . . ? O5 P2 C16 P1 -169.62(17) 3_556 . . . ? O4 P2 C16 P1 -50.9(2) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 30.51 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.277 _refine_diff_density_min -1.295 _refine_diff_density_rms 0.149 data_Compound_2 _database_code_depnum_ccdc_archive 'CCDC 229551' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H34 Cu2 N6 O18 P4 V2' _chemical_formula_weight 1167.51 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' 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' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.3815(4) _cell_length_b 12.0768(5) _cell_length_c 18.0377(7) _cell_angle_alpha 73.765(1) _cell_angle_beta 74.301(1) _cell_angle_gamma 74.770(1) _cell_volume 2047.06(14) _cell_formula_units_Z 2 _cell_measurement_temperature 90(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.894 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1176 _exptl_absorpt_coefficient_mu 1.711 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.8475 _exptl_absorpt_correction_T_max 0.9347 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 90(2) _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_probe x-ray _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.001 _diffrn_reflns_number 25329 _diffrn_reflns_av_R_equivalents 0.0395 _diffrn_reflns_av_sigmaI/netI 0.0666 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.79 _diffrn_reflns_theta_max 30.51 _reflns_number_total 12313 _reflns_number_gt 8935 _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^)+(0.0465P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12313 _refine_ls_number_parameters 613 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0709 _refine_ls_R_factor_gt 0.0451 _refine_ls_wR_factor_ref 0.1070 _refine_ls_wR_factor_gt 0.0960 _refine_ls_goodness_of_fit_ref 0.997 _refine_ls_restrained_S_all 0.997 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.28825(3) 0.75503(3) 1.149393(19) 0.00825(8) Uani 1 1 d . . . Cu2 Cu 0.20165(3) 1.25636(3) 0.359814(19) 0.00878(8) Uani 1 1 d . . . V1 V 0.10863(5) 0.68885(4) 0.93119(3) 0.00965(10) Uani 1 1 d . . . V2 V 0.40106(5) 1.30625(4) 0.57734(3) 0.00981(10) Uani 1 1 d . . . P1 P 0.02863(7) 0.81962(6) 1.07587(4) 0.00897(13) Uani 1 1 d . . . P2 P 0.08484(7) 0.88671(6) 0.76379(4) 0.00920(14) Uani 1 1 d . . . P3 P 0.38065(7) 1.10863(6) 0.73666(4) 0.00958(14) Uani 1 1 d . . . P4 P 0.48994(7) 1.18331(6) 0.42674(4) 0.00842(13) Uani 1 1 d . . . O1 O -0.07988(19) 0.75491(17) 1.12914(11) 0.0127(4) Uani 1 1 d . . . O2 O 0.12479(18) 0.84279(17) 1.11740(11) 0.0105(4) Uani 1 1 d . . . O3 O 0.1177(2) 0.75509(18) 1.00993(12) 0.0146(4) Uani 1 1 d . . . O4 O 0.2284(2) 0.57261(18) 0.93037(12) 0.0157(4) Uani 1 1 d . . . O5 O -0.0353(2) 0.64917(19) 0.94989(13) 0.0194(5) Uani 1 1 d . . . O6 O 0.1361(2) 0.79616(18) 0.83460(12) 0.0169(4) Uani 1 1 d . . . O7 O -0.06596(19) 0.91689(17) 0.77181(12) 0.0132(4) Uani 1 1 d . . . O8 O 0.15327(19) 0.83969(18) 0.68761(11) 0.0133(4) Uani 1 1 d . . . H8 H 0.2384 0.8315 0.6797 0.020 Uiso 1 1 calc R . . O9 O 0.3243(2) 1.15952(18) 0.81215(11) 0.0135(4) Uani 1 1 d . . . H9 H 0.2386 1.1771 0.8206 0.020 Uiso 1 1 calc R . . O10 O 0.53202(19) 1.07211(18) 0.72362(12) 0.0131(4) Uani 1 1 d . . . O11 O 0.3276(2) 1.19858(17) 0.66604(11) 0.0139(4) Uani 1 1 d . . . O12 O 0.5040(2) 1.36607(19) 0.59865(12) 0.0189(5) Uani 1 1 d . . . O13 O 0.2765(2) 1.40903(18) 0.55037(12) 0.0165(4) Uani 1 1 d . . . O14 O 0.49757(19) 1.23322(17) 0.49605(11) 0.0124(4) Uani 1 1 d . . . O15 O 0.59005(19) 1.22647(17) 0.35317(11) 0.0117(4) Uani 1 1 d . . . O16 O 0.34445(19) 1.21073(18) 0.41703(11) 0.0133(4) Uani 1 1 d . . . O90 O 0.2789(2) 0.88780(19) 1.21223(13) 0.0157(4) Uani 1 1 d . . . O91 O 0.2259(2) 1.08797(19) 0.32881(13) 0.0150(4) Uani 1 1 d . . . N1 N 0.2058(2) 0.6479(2) 1.25139(13) 0.0102(4) Uani 1 1 d . . . N2 N 0.4528(2) 0.65539(19) 1.17957(13) 0.0085(4) Uani 1 1 d . . . N3 N 0.4314(2) 0.8053(2) 1.05049(13) 0.0110(5) Uani 1 1 d . . . N4 N 0.0503(2) 1.2299(2) 0.45924(13) 0.0112(5) Uani 1 1 d . . . N5 N 0.0404(2) 1.34112(19) 0.31739(13) 0.0084(4) Uani 1 1 d . . . N6 N 0.2900(2) 1.3307(2) 0.24578(13) 0.0107(4) Uani 1 1 d . . . C1 C 0.0731(3) 0.6539(2) 1.28588(16) 0.0123(5) Uani 1 1 d . . . H1 H 0.0061 0.7018 1.2571 0.015 Uiso 1 1 calc R . . C2 C 0.0310(3) 0.5919(3) 1.36244(17) 0.0145(6) Uani 1 1 d . . . H2 H -0.0635 0.5968 1.3856 0.017 Uiso 1 1 calc R . . C3 C 0.1281(3) 0.5230(3) 1.40450(16) 0.0132(5) Uani 1 1 d . . . H3 H 0.1008 0.4804 1.4571 0.016 Uiso 1 1 calc R . . C4 C 0.2648(3) 0.5164(2) 1.36988(16) 0.0124(5) Uani 1 1 d . . . H4 H 0.3329 0.4701 1.3983 0.015 Uiso 1 1 calc R . . C5 C 0.3009(3) 0.5783(2) 1.29317(16) 0.0093(5) Uani 1 1 d . . . C6 C 0.4427(3) 0.5791(2) 1.24950(16) 0.0092(5) Uani 1 1 d . . . C7 C 0.5586(3) 0.5111(2) 1.27537(16) 0.0097(5) Uani 1 1 d . . . H7 H 0.5514 0.4536 1.3238 0.012 Uiso 1 1 calc R . . C8 C 0.6868(3) 0.5283(2) 1.22900(15) 0.0086(5) Uani 1 1 d . . . C9 C 0.8112(3) 0.4644(2) 1.25944(16) 0.0092(5) Uani 1 1 d . . . C10 C 0.6941(3) 0.6074(2) 1.15604(16) 0.0094(5) Uani 1 1 d . . . H10 H 0.7800 0.6189 1.1230 0.011 Uiso 1 1 calc R . . C11 C 0.5740(3) 0.6689(2) 1.13238(16) 0.0096(5) Uani 1 1 d . . . C12 C 0.5623(3) 0.7566(2) 1.05804(15) 0.0092(5) Uani 1 1 d . . . C13 C 0.6729(3) 0.7859(3) 1.00007(16) 0.0142(6) Uani 1 1 d . . . H13 H 0.7633 0.7505 1.0072 0.017 Uiso 1 1 calc R . . C14 C 0.6509(3) 0.8679(3) 0.93099(17) 0.0156(6) Uani 1 1 d . . . H14 H 0.7256 0.8886 0.8898 0.019 Uiso 1 1 calc R . . C15 C 0.5176(3) 0.9186(3) 0.92351(17) 0.0164(6) Uani 1 1 d . . . H15 H 0.4994 0.9761 0.8774 0.020 Uiso 1 1 calc R . . C16 C 0.4119(3) 0.8846(3) 0.98375(17) 0.0146(6) Uani 1 1 d . . . H16 H 0.3208 0.9190 0.9777 0.017 Uiso 1 1 calc R . . C17 C 0.0639(3) 1.1615(3) 0.53079(16) 0.0155(6) Uani 1 1 d . . . H17 H 0.1531 1.1268 0.5401 0.019 Uiso 1 1 calc R . . C18 C -0.0472(3) 1.1400(3) 0.59111(17) 0.0185(6) Uani 1 1 d . . . H18 H -0.0343 1.0890 0.6404 0.022 Uiso 1 1 calc R . . C19 C -0.1775(3) 1.1931(3) 0.57934(17) 0.0172(6) Uani 1 1 d . . . H19 H -0.2551 1.1806 0.6206 0.021 Uiso 1 1 calc R . . C20 C -0.1929(3) 1.2649(3) 0.50641(16) 0.0135(6) Uani 1 1 d . . . H20 H -0.2812 1.3030 0.4969 0.016 Uiso 1 1 calc R . . C21 C -0.0776(3) 1.2803(2) 0.44758(16) 0.0104(5) Uani 1 1 d . . . C22 C -0.0820(3) 1.3477(2) 0.36632(15) 0.0087(5) Uani 1 1 d . . . C23 C -0.1985(3) 1.4115(2) 0.33944(16) 0.0094(5) Uani 1 1 d . . . H23 H -0.2846 1.4192 0.3753 0.011 Uiso 1 1 calc R . . C24 C -0.0589(3) 1.4569(2) 0.20950(16) 0.0100(5) Uani 1 1 d . . . H24 H -0.0486 1.4933 0.1548 0.012 Uiso 1 1 calc R . . C25 C 0.0546(3) 1.3954(2) 0.24103(15) 0.0090(5) Uani 1 1 d . . . C26 C 0.1985(3) 1.3858(2) 0.19869(16) 0.0100(5) Uani 1 1 d . . . C27 C 0.2386(3) 1.4316(3) 0.11848(16) 0.0134(6) Uani 1 1 d . . . H27 H 0.1726 1.4694 0.0869 0.016 Uiso 1 1 calc R . . C28 C 0.3773(3) 1.4211(3) 0.08523(17) 0.0158(6) Uani 1 1 d . . . H28 H 0.4079 1.4511 0.0303 0.019 Uiso 1 1 calc R . . C29 C 0.4703(3) 1.3665(3) 0.13303(17) 0.0158(6) Uani 1 1 d . . . H29 H 0.5655 1.3602 0.1115 0.019 Uiso 1 1 calc R . . C30 C 0.4234(3) 1.3211(2) 0.21270(17) 0.0133(6) Uani 1 1 d . . . H30 H 0.4880 1.2818 0.2449 0.016 Uiso 1 1 calc R . . C31 C -0.0510(3) 0.9619(2) 1.02546(16) 0.0121(5) Uani 1 1 d . . . H31A H -0.1050 0.9506 0.9916 0.015 Uiso 1 1 calc R . . H31B H -0.1149 1.0039 1.0652 0.015 Uiso 1 1 calc R . . C32 C 0.1528(3) 1.0130(2) 0.75415(17) 0.0119(5) Uani 1 1 d . . . H32A H 0.1373 1.0700 0.7044 0.014 Uiso 1 1 calc R . . H32B H 0.1026 1.0515 0.7984 0.014 Uiso 1 1 calc R . . C33 C 0.3052(3) 0.9837(2) 0.75384(16) 0.0111(5) Uani 1 1 d . . . H33A H 0.3540 0.9390 0.7125 0.013 Uiso 1 1 calc R . . H33B H 0.3193 0.9316 0.8054 0.013 Uiso 1 1 calc R . . C34 C 0.5421(3) 1.0262(2) 0.46042(16) 0.0140(6) Uani 1 1 d . . . H34A H 0.5365 0.9873 0.4201 0.017 Uiso 1 1 calc R . . H34B H 0.6389 1.0082 0.4646 0.017 Uiso 1 1 calc R . . H90A H 0.216(4) 0.937(3) 1.214(2) 0.017(10) Uiso 1 1 d . . . H90B H 0.337(4) 0.891(3) 1.235(2) 0.038(12) Uiso 1 1 d . . . H91A H 0.174(3) 1.088(3) 0.302(2) 0.015(9) Uiso 1 1 d . . . H91B H 0.298(3) 1.047(3) 0.3150(19) 0.012(9) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.00580(15) 0.00928(16) 0.00794(15) 0.00067(12) -0.00273(12) -0.00008(12) Cu2 0.00599(15) 0.01035(16) 0.00861(16) 0.00046(12) -0.00336(12) -0.00021(12) V1 0.0083(2) 0.0096(2) 0.0101(2) -0.00141(17) -0.00198(17) -0.00097(17) V2 0.0086(2) 0.0108(2) 0.0096(2) -0.00194(18) -0.00190(17) -0.00171(17) P1 0.0069(3) 0.0099(3) 0.0094(3) -0.0015(3) -0.0029(2) 0.0000(2) P2 0.0080(3) 0.0102(3) 0.0094(3) -0.0015(3) -0.0030(2) -0.0013(3) P3 0.0084(3) 0.0102(3) 0.0105(3) -0.0017(3) -0.0039(2) -0.0013(3) P4 0.0073(3) 0.0086(3) 0.0088(3) -0.0013(3) -0.0032(2) 0.0000(2) O1 0.0123(9) 0.0120(10) 0.0128(10) -0.0014(8) -0.0024(7) -0.0028(8) O2 0.0078(9) 0.0124(10) 0.0102(9) -0.0001(7) -0.0053(7) 0.0006(7) O3 0.0130(10) 0.0162(10) 0.0152(10) -0.0072(8) -0.0036(8) 0.0008(8) O4 0.0148(10) 0.0141(10) 0.0164(10) -0.0049(8) -0.0023(8) 0.0008(8) O5 0.0130(10) 0.0221(12) 0.0240(12) -0.0066(9) -0.0002(9) -0.0073(9) O6 0.0159(10) 0.0183(11) 0.0149(10) 0.0029(8) -0.0057(8) -0.0054(8) O7 0.0091(9) 0.0144(10) 0.0161(10) -0.0037(8) -0.0031(8) -0.0019(8) O8 0.0084(9) 0.0186(11) 0.0150(10) -0.0086(8) -0.0028(8) -0.0008(8) O9 0.0115(9) 0.0170(10) 0.0137(10) -0.0067(8) -0.0043(8) -0.0009(8) O10 0.0083(9) 0.0158(10) 0.0163(10) -0.0049(8) -0.0041(8) -0.0014(8) O11 0.0122(10) 0.0155(10) 0.0121(10) 0.0022(8) -0.0041(8) -0.0038(8) O12 0.0165(11) 0.0252(12) 0.0191(11) -0.0090(9) -0.0017(8) -0.0091(9) O13 0.0117(10) 0.0171(11) 0.0139(10) 0.0018(8) -0.0016(8) 0.0018(8) O14 0.0116(9) 0.0142(10) 0.0136(10) -0.0055(8) -0.0036(8) -0.0028(8) O15 0.0092(9) 0.0125(10) 0.0108(9) -0.0011(8) -0.0010(7) -0.0004(7) O16 0.0083(9) 0.0185(11) 0.0123(10) 0.0001(8) -0.0064(7) -0.0011(8) O90 0.0123(10) 0.0150(11) 0.0222(12) -0.0070(9) -0.0098(9) 0.0023(9) O91 0.0128(10) 0.0143(11) 0.0206(11) -0.0068(9) -0.0078(9) 0.0006(9) N1 0.0079(10) 0.0092(11) 0.0128(11) -0.0019(9) -0.0044(8) 0.0008(8) N2 0.0100(10) 0.0076(11) 0.0076(10) -0.0007(8) -0.0036(8) -0.0006(8) N3 0.0082(10) 0.0120(11) 0.0108(11) -0.0003(9) -0.0034(8) 0.0002(9) N4 0.0092(11) 0.0145(12) 0.0088(11) -0.0012(9) -0.0037(8) -0.0003(9) N5 0.0077(10) 0.0078(11) 0.0090(10) -0.0006(9) -0.0028(8) -0.0007(8) N6 0.0095(11) 0.0102(11) 0.0118(11) -0.0008(9) -0.0039(9) -0.0012(9) C1 0.0100(12) 0.0123(13) 0.0136(13) -0.0006(11) -0.0030(10) -0.0027(10) C2 0.0091(12) 0.0179(15) 0.0165(14) -0.0034(12) -0.0012(10) -0.0048(11) C3 0.0120(13) 0.0158(14) 0.0095(13) -0.0006(11) 0.0004(10) -0.0043(11) C4 0.0116(13) 0.0104(13) 0.0143(13) -0.0002(11) -0.0045(10) -0.0020(10) C5 0.0079(12) 0.0086(12) 0.0110(12) -0.0013(10) -0.0024(10) -0.0019(10) C6 0.0072(12) 0.0091(12) 0.0108(12) -0.0034(10) -0.0008(9) -0.0008(10) C7 0.0112(12) 0.0072(12) 0.0097(12) 0.0002(10) -0.0037(10) -0.0008(10) C8 0.0078(12) 0.0071(12) 0.0107(12) -0.0028(10) -0.0025(10) 0.0005(9) C9 0.0084(12) 0.0072(12) 0.0126(13) 0.0000(10) -0.0056(10) -0.0014(10) C10 0.0082(12) 0.0087(12) 0.0105(12) -0.0019(10) -0.0025(10) 0.0001(10) C11 0.0119(12) 0.0080(12) 0.0095(12) -0.0021(10) -0.0036(10) -0.0016(10) C12 0.0086(12) 0.0084(12) 0.0095(12) -0.0011(10) -0.0033(9) 0.0008(10) C13 0.0099(13) 0.0161(14) 0.0133(13) -0.0013(11) -0.0030(10) 0.0010(11) C14 0.0130(13) 0.0183(15) 0.0109(13) 0.0027(11) 0.0002(10) -0.0046(11) C15 0.0157(14) 0.0174(15) 0.0126(14) 0.0032(11) -0.0057(11) -0.0016(11) C16 0.0110(13) 0.0162(14) 0.0143(14) 0.0011(11) -0.0072(11) 0.0006(11) C17 0.0107(13) 0.0209(15) 0.0110(13) 0.0044(11) -0.0058(10) -0.0014(11) C18 0.0139(14) 0.0250(17) 0.0119(14) 0.0057(12) -0.0049(11) -0.0040(12) C19 0.0123(13) 0.0240(16) 0.0123(14) 0.0020(12) -0.0024(11) -0.0054(12) C20 0.0078(12) 0.0190(15) 0.0121(13) -0.0006(11) -0.0026(10) -0.0023(11) C21 0.0102(12) 0.0122(13) 0.0089(12) -0.0003(10) -0.0038(10) -0.0028(10) C22 0.0101(12) 0.0087(12) 0.0076(12) -0.0014(10) -0.0020(9) -0.0025(10) C23 0.0071(11) 0.0105(13) 0.0100(12) -0.0024(10) -0.0020(9) -0.0009(10) C24 0.0107(12) 0.0110(13) 0.0079(12) 0.0002(10) -0.0048(10) -0.0009(10) C25 0.0086(12) 0.0078(12) 0.0098(12) -0.0017(10) -0.0015(9) -0.0008(10) C26 0.0075(12) 0.0114(13) 0.0091(12) -0.0005(10) -0.0013(9) -0.0011(10) C27 0.0112(13) 0.0176(14) 0.0119(13) 0.0007(11) -0.0061(10) -0.0042(11) C28 0.0141(14) 0.0219(16) 0.0102(13) -0.0008(11) 0.0001(10) -0.0071(12) C29 0.0091(13) 0.0207(15) 0.0162(14) -0.0016(12) -0.0014(11) -0.0045(11) C30 0.0087(12) 0.0147(14) 0.0157(14) -0.0035(11) -0.0030(10) -0.0005(10) C31 0.0095(12) 0.0121(13) 0.0145(13) 0.0000(11) -0.0076(10) 0.0002(10) C32 0.0103(12) 0.0123(13) 0.0138(13) -0.0034(11) -0.0051(10) -0.0004(10) C33 0.0118(12) 0.0102(13) 0.0119(13) -0.0016(10) -0.0047(10) -0.0021(10) C34 0.0149(14) 0.0108(13) 0.0115(13) 0.0004(11) -0.0014(11) 0.0010(11) _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 O2 1.8918(18) . ? Cu1 N2 1.929(2) . ? Cu1 N1 2.047(2) . ? Cu1 N3 2.048(2) . ? Cu1 O90 2.177(2) . ? Cu2 O16 1.9098(18) . ? Cu2 N5 1.947(2) . ? Cu2 N4 2.050(2) . ? Cu2 N6 2.064(2) . ? Cu2 O91 2.191(2) . ? V1 O5 1.609(2) . ? V1 O4 1.613(2) . ? V1 O3 1.848(2) . ? V1 O6 1.860(2) . ? V2 O12 1.611(2) . ? V2 O13 1.615(2) . ? V2 O14 1.843(2) . ? V2 O11 1.879(2) . ? P1 O1 1.503(2) . ? P1 O2 1.5182(19) . ? P1 O3 1.556(2) . ? P1 C31 1.802(3) . ? P2 O7 1.487(2) . ? P2 O6 1.547(2) . ? P2 O8 1.553(2) . ? P2 C32 1.791(3) . ? P3 O10 1.488(2) . ? P3 O11 1.549(2) . ? P3 O9 1.556(2) . ? P3 C33 1.793(3) . ? P4 O15 1.505(2) . ? P4 O16 1.5066(19) . ? P4 O14 1.560(2) . ? P4 C34 1.804(3) . ? N1 C1 1.341(3) . ? N1 C5 1.365(3) . ? N2 C6 1.334(3) . ? N2 C11 1.336(3) . ? N3 C16 1.339(3) . ? N3 C12 1.359(3) . ? N4 C17 1.345(3) . ? N4 C21 1.355(3) . ? N5 C22 1.334(3) . ? N5 C25 1.336(3) . ? N6 C30 1.339(3) . ? N6 C26 1.362(3) . ? C1 C2 1.388(4) . ? C2 C3 1.379(4) . ? C3 C4 1.379(4) . ? C4 C5 1.379(4) . ? C5 C6 1.470(4) . ? C6 C7 1.383(4) . ? C7 C8 1.400(4) . ? C8 C10 1.390(4) . ? C8 C9 1.479(3) . ? C9 C23 1.393(4) 1_646 ? C9 C24 1.401(4) 1_646 ? C10 C11 1.383(3) . ? C11 C12 1.470(4) . ? C12 C13 1.376(4) . ? C13 C14 1.389(4) . ? C14 C15 1.384(4) . ? C15 C16 1.377(4) . ? C17 C18 1.379(4) . ? C18 C19 1.381(4) . ? C19 C20 1.382(4) . ? C20 C21 1.382(4) . ? C21 C22 1.470(4) . ? C22 C23 1.382(3) . ? C23 C9 1.393(4) 1_464 ? C24 C25 1.389(3) . ? C24 C9 1.401(4) 1_464 ? C25 C26 1.473(4) . ? C26 C27 1.386(4) . ? C27 C28 1.389(4) . ? C28 C29 1.382(4) . ? C29 C30 1.387(4) . ? C31 C31 1.524(5) 2_577 ? C32 C33 1.526(4) . ? C34 C34 1.521(5) 2_676 ? 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 Cu1 N2 175.55(9) . . ? O2 Cu1 N1 98.89(9) . . ? N2 Cu1 N1 79.88(9) . . ? O2 Cu1 N3 101.09(9) . . ? N2 Cu1 N3 79.40(9) . . ? N1 Cu1 N3 157.44(9) . . ? O2 Cu1 O90 89.43(8) . . ? N2 Cu1 O90 94.86(9) . . ? N1 Cu1 O90 91.67(9) . . ? N3 Cu1 O90 98.87(9) . . ? O16 Cu2 N5 162.99(9) . . ? O16 Cu2 N4 94.20(9) . . ? N5 Cu2 N4 79.29(9) . . ? O16 Cu2 N6 105.21(9) . . ? N5 Cu2 N6 78.94(9) . . ? N4 Cu2 N6 157.57(9) . . ? O16 Cu2 O91 97.78(8) . . ? N5 Cu2 O91 98.59(9) . . ? N4 Cu2 O91 96.90(9) . . ? N6 Cu2 O91 91.59(9) . . ? O5 V1 O4 108.12(11) . . ? O5 V1 O3 110.72(10) . . ? O4 V1 O3 107.23(10) . . ? O5 V1 O6 111.43(10) . . ? O4 V1 O6 110.07(10) . . ? O3 V1 O6 109.17(9) . . ? O12 V2 O13 108.11(11) . . ? O12 V2 O14 107.62(10) . . ? O13 V2 O14 110.83(10) . . ? O12 V2 O11 110.97(10) . . ? O13 V2 O11 108.04(10) . . ? O14 V2 O11 111.23(9) . . ? O1 P1 O2 115.11(11) . . ? O1 P1 O3 112.14(11) . . ? O2 P1 O3 107.54(11) . . ? O1 P1 C31 109.44(12) . . ? O2 P1 C31 106.12(12) . . ? O3 P1 C31 105.94(12) . . ? O7 P2 O6 115.24(12) . . ? O7 P2 O8 109.46(11) . . ? O6 P2 O8 108.81(12) . . ? O7 P2 C32 111.80(12) . . ? O6 P2 C32 104.36(12) . . ? O8 P2 C32 106.74(12) . . ? O10 P3 O11 114.47(11) . . ? O10 P3 O9 109.71(11) . . ? O11 P3 O9 109.57(11) . . ? O10 P3 C33 110.35(12) . . ? O11 P3 C33 105.72(12) . . ? O9 P3 C33 106.68(12) . . ? O15 P4 O16 114.39(11) . . ? O15 P4 O14 110.07(11) . . ? O16 P4 O14 109.90(11) . . ? O15 P4 C34 109.52(12) . . ? O16 P4 C34 108.84(13) . . ? O14 P4 C34 103.55(12) . . ? P1 O2 Cu1 134.12(12) . . ? P1 O3 V1 143.14(13) . . ? P2 O6 V1 152.36(13) . . ? P3 O11 V2 135.80(12) . . ? P4 O14 V2 146.37(12) . . ? P4 O16 Cu2 155.80(13) . . ? C1 N1 C5 118.6(2) . . ? C1 N1 Cu1 127.33(18) . . ? C5 N1 Cu1 113.04(18) . . ? C6 N2 C11 121.6(2) . . ? C6 N2 Cu1 118.75(18) . . ? C11 N2 Cu1 119.49(18) . . ? C16 N3 C12 117.7(2) . . ? C16 N3 Cu1 128.34(19) . . ? C12 N3 Cu1 113.78(18) . . ? C17 N4 C21 117.9(2) . . ? C17 N4 Cu2 127.46(19) . . ? C21 N4 Cu2 114.33(18) . . ? C22 N5 C25 121.3(2) . . ? C22 N5 Cu2 118.90(18) . . ? C25 N5 Cu2 119.72(18) . . ? C30 N6 C26 118.2(2) . . ? C30 N6 Cu2 127.69(18) . . ? C26 N6 Cu2 113.74(18) . . ? N1 C1 C2 121.7(3) . . ? C3 C2 C1 119.2(3) . . ? C4 C3 C2 119.7(3) . . ? C3 C4 C5 118.7(3) . . ? N1 C5 C4 122.1(2) . . ? N1 C5 C6 113.7(2) . . ? C4 C5 C6 124.2(2) . . ? N2 C6 C7 120.5(2) . . ? N2 C6 C5 113.5(2) . . ? C7 C6 C5 125.9(2) . . ? C6 C7 C8 118.9(2) . . ? C10 C8 C7 119.1(2) . . ? C10 C8 C9 121.4(2) . . ? C7 C8 C9 119.4(2) . . ? C23 C9 C24 118.3(2) 1_646 1_646 ? C23 C9 C8 120.3(2) 1_646 . ? C24 C9 C8 121.4(2) 1_646 . ? C11 C10 C8 118.9(2) . . ? N2 C11 C10 120.8(2) . . ? N2 C11 C12 112.9(2) . . ? C10 C11 C12 126.2(2) . . ? N3 C12 C13 122.4(2) . . ? N3 C12 C11 113.9(2) . . ? C13 C12 C11 123.7(2) . . ? C12 C13 C14 119.2(3) . . ? C15 C14 C13 118.5(3) . . ? C16 C15 C14 119.1(3) . . ? N3 C16 C15 123.0(3) . . ? N4 C17 C18 122.3(3) . . ? C17 C18 C19 119.5(3) . . ? C18 C19 C20 118.8(3) . . ? C19 C20 C21 119.0(3) . . ? N4 C21 C20 122.4(2) . . ? N4 C21 C22 113.8(2) . . ? C20 C21 C22 123.7(2) . . ? N5 C22 C23 120.8(2) . . ? N5 C22 C21 113.5(2) . . ? C23 C22 C21 125.6(2) . . ? C22 C23 C9 119.6(2) . 1_464 ? C25 C24 C9 119.1(2) . 1_464 ? N5 C25 C24 120.8(2) . . ? N5 C25 C26 112.9(2) . . ? C24 C25 C26 126.3(2) . . ? N6 C26 C27 122.4(2) . . ? N6 C26 C25 114.1(2) . . ? C27 C26 C25 123.4(2) . . ? C26 C27 C28 118.5(2) . . ? C29 C28 C27 119.2(3) . . ? C28 C29 C30 119.4(3) . . ? N6 C30 C29 122.2(3) . . ? C31 C31 P1 113.4(2) 2_577 . ? C33 C32 P2 113.40(19) . . ? C32 C33 P3 114.96(19) . . ? C34 C34 P4 114.6(3) 2_676 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 P1 O2 Cu1 85.93(18) . . . . ? O3 P1 O2 Cu1 -39.84(19) . . . . ? C31 P1 O2 Cu1 -152.86(16) . . . . ? N2 Cu1 O2 P1 -6.5(13) . . . . ? N1 Cu1 O2 P1 -80.10(17) . . . . ? N3 Cu1 O2 P1 89.37(17) . . . . ? O90 Cu1 O2 P1 -171.70(17) . . . . ? O1 P1 O3 V1 51.3(2) . . . . ? O2 P1 O3 V1 178.8(2) . . . . ? C31 P1 O3 V1 -68.0(2) . . . . ? O5 V1 O3 P1 -24.5(3) . . . . ? O4 V1 O3 P1 -142.3(2) . . . . ? O6 V1 O3 P1 98.5(2) . . . . ? O7 P2 O6 V1 6.5(4) . . . . ? O8 P2 O6 V1 -116.8(3) . . . . ? C32 P2 O6 V1 129.5(3) . . . . ? O5 V1 O6 P2 17.3(3) . . . . ? O4 V1 O6 P2 137.2(3) . . . . ? O3 V1 O6 P2 -105.4(3) . . . . ? O10 P3 O11 V2 -20.3(2) . . . . ? O9 P3 O11 V2 103.41(19) . . . . ? C33 P3 O11 V2 -141.97(18) . . . . ? O12 V2 O11 P3 -36.8(2) . . . . ? O13 V2 O11 P3 -155.20(18) . . . . ? O14 V2 O11 P3 82.94(19) . . . . ? O15 P4 O14 V2 132.4(2) . . . . ? O16 P4 O14 V2 5.5(3) . . . . ? C34 P4 O14 V2 -110.6(2) . . . . ? O12 V2 O14 P4 -159.1(2) . . . . ? O13 V2 O14 P4 -41.1(3) . . . . ? O11 V2 O14 P4 79.2(2) . . . . ? O15 P4 O16 Cu2 15.6(4) . . . . ? O14 P4 O16 Cu2 140.0(3) . . . . ? C34 P4 O16 Cu2 -107.3(3) . . . . ? N5 Cu2 O16 P4 -117.5(4) . . . . ? N4 Cu2 O16 P4 175.9(3) . . . . ? N6 Cu2 O16 P4 -15.4(4) . . . . ? O91 Cu2 O16 P4 78.4(3) . . . . ? O2 Cu1 N1 C1 -6.8(2) . . . . ? N2 Cu1 N1 C1 177.5(2) . . . . ? N3 Cu1 N1 C1 -158.9(2) . . . . ? O90 Cu1 N1 C1 82.9(2) . . . . ? O2 Cu1 N1 C5 -174.73(18) . . . . ? N2 Cu1 N1 C5 9.60(18) . . . . ? N3 Cu1 N1 C5 33.1(3) . . . . ? O90 Cu1 N1 C5 -85.05(19) . . . . ? O2 Cu1 N2 C6 -81.2(12) . . . . ? N1 Cu1 N2 C6 -6.9(2) . . . . ? N3 Cu1 N2 C6 -177.9(2) . . . . ? O90 Cu1 N2 C6 83.9(2) . . . . ? O2 Cu1 N2 C11 102.6(11) . . . . ? N1 Cu1 N2 C11 176.9(2) . . . . ? N3 Cu1 N2 C11 5.9(2) . . . . ? O90 Cu1 N2 C11 -92.3(2) . . . . ? O2 Cu1 N3 C16 3.5(3) . . . . ? N2 Cu1 N3 C16 179.0(3) . . . . ? N1 Cu1 N3 C16 155.4(2) . . . . ? O90 Cu1 N3 C16 -87.7(3) . . . . ? O2 Cu1 N3 C12 178.20(18) . . . . ? N2 Cu1 N3 C12 -6.30(19) . . . . ? N1 Cu1 N3 C12 -29.9(4) . . . . ? O90 Cu1 N3 C12 87.03(19) . . . . ? O16 Cu2 N4 C17 -21.8(3) . . . . ? N5 Cu2 N4 C17 174.0(3) . . . . ? N6 Cu2 N4 C17 -172.0(2) . . . . ? O91 Cu2 N4 C17 76.5(3) . . . . ? O16 Cu2 N4 C21 164.22(19) . . . . ? N5 Cu2 N4 C21 0.07(19) . . . . ? N6 Cu2 N4 C21 14.1(4) . . . . ? O91 Cu2 N4 C21 -97.4(2) . . . . ? O16 Cu2 N5 C22 -66.4(4) . . . . ? N4 Cu2 N5 C22 2.28(19) . . . . ? N6 Cu2 N5 C22 -172.3(2) . . . . ? O91 Cu2 N5 C22 97.7(2) . . . . ? O16 Cu2 N5 C25 110.9(3) . . . . ? N4 Cu2 N5 C25 179.6(2) . . . . ? N6 Cu2 N5 C25 5.0(2) . . . . ? O91 Cu2 N5 C25 -85.0(2) . . . . ? O16 Cu2 N6 C30 16.6(3) . . . . ? N5 Cu2 N6 C30 179.7(3) . . . . ? N4 Cu2 N6 C30 165.7(2) . . . . ? O91 Cu2 N6 C30 -81.9(2) . . . . ? O16 Cu2 N6 C26 -170.10(19) . . . . ? N5 Cu2 N6 C26 -7.05(19) . . . . ? N4 Cu2 N6 C26 -21.1(4) . . . . ? O91 Cu2 N6 C26 91.40(19) . . . . ? C5 N1 C1 C2 0.3(4) . . . . ? Cu1 N1 C1 C2 -167.0(2) . . . . ? N1 C1 C2 C3 0.5(4) . . . . ? C1 C2 C3 C4 -0.3(4) . . . . ? C2 C3 C4 C5 -0.7(4) . . . . ? C1 N1 C5 C4 -1.4(4) . . . . ? Cu1 N1 C5 C4 167.7(2) . . . . ? C1 N1 C5 C6 -179.8(2) . . . . ? Cu1 N1 C5 C6 -10.7(3) . . . . ? C3 C4 C5 N1 1.6(4) . . . . ? C3 C4 C5 C6 179.8(3) . . . . ? C11 N2 C6 C7 -0.1(4) . . . . ? Cu1 N2 C6 C7 -176.2(2) . . . . ? C11 N2 C6 C5 179.2(2) . . . . ? Cu1 N2 C6 C5 3.1(3) . . . . ? N1 C5 C6 N2 5.4(3) . . . . ? C4 C5 C6 N2 -172.9(3) . . . . ? N1 C5 C6 C7 -175.4(3) . . . . ? C4 C5 C6 C7 6.3(4) . . . . ? N2 C6 C7 C8 3.6(4) . . . . ? C5 C6 C7 C8 -175.5(2) . . . . ? C6 C7 C8 C10 -4.3(4) . . . . ? C6 C7 C8 C9 174.2(2) . . . . ? C10 C8 C9 C23 162.5(3) . . . 1_646 ? C7 C8 C9 C23 -15.9(4) . . . 1_646 ? C10 C8 C9 C24 -16.5(4) . . . 1_646 ? C7 C8 C9 C24 165.0(2) . . . 1_646 ? C7 C8 C10 C11 1.7(4) . . . . ? C9 C8 C10 C11 -176.8(2) . . . . ? C6 N2 C11 C10 -2.7(4) . . . . ? Cu1 N2 C11 C10 173.3(2) . . . . ? C6 N2 C11 C12 179.6(2) . . . . ? Cu1 N2 C11 C12 -4.3(3) . . . . ? C8 C10 C11 N2 1.9(4) . . . . ? C8 C10 C11 C12 179.2(3) . . . . ? C16 N3 C12 C13 -0.1(4) . . . . ? Cu1 N3 C12 C13 -175.4(2) . . . . ? C16 N3 C12 C11 -178.8(2) . . . . ? Cu1 N3 C12 C11 5.9(3) . . . . ? N2 C11 C12 N3 -1.4(3) . . . . ? C10 C11 C12 N3 -178.9(3) . . . . ? N2 C11 C12 C13 179.9(3) . . . . ? C10 C11 C12 C13 2.4(4) . . . . ? N3 C12 C13 C14 -0.3(4) . . . . ? C11 C12 C13 C14 178.4(3) . . . . ? C12 C13 C14 C15 1.0(4) . . . . ? C13 C14 C15 C16 -1.3(5) . . . . ? C12 N3 C16 C15 -0.3(4) . . . . ? Cu1 N3 C16 C15 174.2(2) . . . . ? C14 C15 C16 N3 1.0(5) . . . . ? C21 N4 C17 C18 1.2(4) . . . . ? Cu2 N4 C17 C18 -172.6(2) . . . . ? N4 C17 C18 C19 -2.3(5) . . . . ? C17 C18 C19 C20 1.4(5) . . . . ? C18 C19 C20 C21 0.5(5) . . . . ? C17 N4 C21 C20 0.8(4) . . . . ? Cu2 N4 C21 C20 175.3(2) . . . . ? C17 N4 C21 C22 -176.7(2) . . . . ? Cu2 N4 C21 C22 -2.1(3) . . . . ? C19 C20 C21 N4 -1.6(4) . . . . ? C19 C20 C21 C22 175.6(3) . . . . ? C25 N5 C22 C23 -0.2(4) . . . . ? Cu2 N5 C22 C23 177.0(2) . . . . ? C25 N5 C22 C21 178.7(2) . . . . ? Cu2 N5 C22 C21 -4.0(3) . . . . ? N4 C21 C22 N5 3.9(3) . . . . ? C20 C21 C22 N5 -173.5(3) . . . . ? N4 C21 C22 C23 -177.2(3) . . . . ? C20 C21 C22 C23 5.4(4) . . . . ? N5 C22 C23 C9 3.4(4) . . . 1_464 ? C21 C22 C23 C9 -175.4(3) . . . 1_464 ? C22 N5 C25 C24 -2.5(4) . . . . ? Cu2 N5 C25 C24 -179.7(2) . . . . ? C22 N5 C25 C26 175.1(2) . . . . ? Cu2 N5 C25 C26 -2.1(3) . . . . ? C9 C24 C25 N5 2.0(4) 1_464 . . . ? C9 C24 C25 C26 -175.3(3) 1_464 . . . ? C30 N6 C26 C27 0.0(4) . . . . ? Cu2 N6 C26 C27 -173.9(2) . . . . ? C30 N6 C26 C25 -178.1(2) . . . . ? Cu2 N6 C26 C25 8.0(3) . . . . ? N5 C25 C26 N6 -4.2(3) . . . . ? C24 C25 C26 N6 173.3(3) . . . . ? N5 C25 C26 C27 177.8(3) . . . . ? C24 C25 C26 C27 -4.7(4) . . . . ? N6 C26 C27 C28 -0.2(4) . . . . ? C25 C26 C27 C28 177.7(3) . . . . ? C26 C27 C28 C29 -0.6(4) . . . . ? C27 C28 C29 C30 1.5(4) . . . . ? C26 N6 C30 C29 0.9(4) . . . . ? Cu2 N6 C30 C29 173.9(2) . . . . ? C28 C29 C30 N6 -1.7(5) . . . . ? O1 P1 C31 C31 175.7(3) . . . 2_577 ? O2 P1 C31 C31 50.9(3) . . . 2_577 ? O3 P1 C31 C31 -63.2(3) . . . 2_577 ? O7 P2 C32 C33 174.39(19) . . . . ? O6 P2 C32 C33 49.2(2) . . . . ? O8 P2 C32 C33 -65.9(2) . . . . ? P2 C32 C33 P3 175.40(14) . . . . ? O10 P3 C33 C32 -170.13(19) . . . . ? O11 P3 C33 C32 -45.8(2) . . . . ? O9 P3 C33 C32 70.8(2) . . . . ? O15 P4 C34 C34 173.6(3) . . . 2_676 ? O16 P4 C34 C34 -60.7(3) . . . 2_676 ? O14 P4 C34 C34 56.2(3) . . . 2_676 ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 30.51 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 0.751 _refine_diff_density_min -0.613 _refine_diff_density_rms 0.123 data_Compound_3 _database_code_depnum_ccdc_archive 'CCDC 229552' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H20 Cu N3 O12 P2 V2' _chemical_formula_weight 697.73 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' 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' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.4256(5) _cell_length_b 11.3275(6) _cell_length_c 11.4321(6) _cell_angle_alpha 80.291(1) _cell_angle_beta 82.879(1) _cell_angle_gamma 73.855(1) _cell_volume 1151.82(11) _cell_formula_units_Z 2 _cell_measurement_temperature 90(2) _cell_measurement_reflns_used 15182 _cell_measurement_theta_min 1.89 _cell_measurement_theta_max 31.68 _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.012 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 700 _exptl_absorpt_coefficient_mu 1.922 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details 'SADABS SHELXL-97 (SHELDRICK, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 90(2) _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_probe x-ray _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'APEX CCD area detector' _diffrn_measurement_method 'Phi and omega scans' _diffrn_detector_area_resol_mean 512 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.001 _diffrn_reflns_number 15182 _diffrn_reflns_av_R_equivalents 0.0387 _diffrn_reflns_av_sigmaI/netI 0.0671 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.89 _diffrn_reflns_theta_max 31.68 _reflns_number_total 7583 _reflns_number_gt 5843 _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 and CrystalMaker 5.x' _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^)+(0.0506P)^2^+1.2742P] 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 7583 _refine_ls_number_parameters 343 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0683 _refine_ls_R_factor_gt 0.0486 _refine_ls_wR_factor_ref 0.1193 _refine_ls_wR_factor_gt 0.1104 _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_restrained_S_all 1.034 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.56978(4) 0.30988(3) 0.11295(3) 0.00803(9) Uani 1 1 d . . . V1 V 0.94178(6) -0.08899(5) 0.25524(4) 0.00944(11) Uani 1 1 d . . . V2 V 0.60438(5) 0.16018(5) 0.40453(4) 0.00759(10) Uani 1 1 d . . . P1 P 0.88077(8) 0.16414(7) 0.20721(7) 0.00826(14) Uani 1 1 d . . . P2 P 0.70441(8) -0.13853(7) 0.47460(7) 0.00813(14) Uani 1 1 d . . . O1 O 0.6629(2) -0.00342(19) 0.49695(18) 0.0093(4) Uani 1 1 d . . . O2 O 0.7894(2) -0.1551(2) 0.35232(19) 0.0113(4) Uani 1 1 d . . . O3 O 0.5691(2) -0.18902(19) 0.48071(18) 0.0089(4) Uani 1 1 d . . . O4 O 0.5171(2) 0.1961(2) 0.28165(19) 0.0109(4) Uani 1 1 d . . . O5 O 0.7789(2) 0.2623(2) 0.12695(18) 0.0105(4) Uani 1 1 d . . . O6 O 0.9843(2) 0.0567(2) 0.14601(19) 0.0123(4) Uani 1 1 d . . . O7 O 0.8006(2) 0.08672(19) 0.30593(19) 0.0099(4) Uani 1 1 d . . . O9 O 1.0822(2) -0.1368(2) 0.3340(2) 0.0138(4) Uani 1 1 d . . . O10 O 0.9675(3) -0.1812(2) 0.1550(2) 0.0147(4) Uani 1 1 d . . . O11 O 0.6648(2) 0.2751(2) 0.42444(19) 0.0123(4) Uani 1 1 d . . . O90 O 0.8338(5) 0.4343(4) 0.4900(4) 0.0629(11) Uani 1 1 d . . . O91 O 0.9659(5) 0.5857(4) 0.3325(4) 0.0611(11) Uani 1 1 d . . . N1 N 0.5147(3) 0.4670(2) 0.1903(2) 0.0095(5) Uani 1 1 d . . . N2 N 0.3693(3) 0.3791(2) 0.0687(2) 0.0091(5) Uani 1 1 d . . . N3 N 0.5637(3) 0.1973(2) -0.0054(2) 0.0108(5) Uani 1 1 d . . . C1 C 0.5988(3) 0.5031(3) 0.2566(3) 0.0116(6) Uani 1 1 d . . . H1 H 0.6977 0.4591 0.2610 0.014 Uiso 1 1 calc R . . C2 C 0.5442(4) 0.6027(3) 0.3183(3) 0.0150(6) Uani 1 1 d . . . H2 H 0.6048 0.6245 0.3645 0.018 Uiso 1 1 calc R . . C3 C 0.3980(4) 0.6701(3) 0.3105(3) 0.0177(7) Uani 1 1 d . . . H3 H 0.3595 0.7387 0.3504 0.021 Uiso 1 1 calc R . . C4 C 0.3092(4) 0.6338(3) 0.2423(3) 0.0155(6) Uani 1 1 d . . . H4 H 0.2105 0.6776 0.2359 0.019 Uiso 1 1 calc R . . C5 C 0.3704(3) 0.5319(3) 0.1848(3) 0.0107(5) Uani 1 1 d . . . C6 C 0.2870(3) 0.4826(3) 0.1111(3) 0.0097(5) Uani 1 1 d . . . C7 C 0.1413(3) 0.5341(3) 0.0846(3) 0.0104(5) Uani 1 1 d . . . H7 H 0.0856 0.6066 0.1132 0.012 Uiso 1 1 calc R . . C8 C 0.0790(3) 0.4747(3) 0.0138(3) 0.0090(5) Uani 1 1 d . . . C9 C 0.1685(3) 0.3667(3) -0.0302(3) 0.0103(5) Uani 1 1 d . . . H9 H 0.1300 0.3254 -0.0772 0.012 Uiso 1 1 calc R . . C10 C 0.3150(3) 0.3230(3) -0.0022(3) 0.0103(5) Uani 1 1 d . . . C11 C 0.4288(3) 0.2175(3) -0.0469(3) 0.0103(5) Uani 1 1 d . . . C12 C 0.4050(3) 0.1487(3) -0.1280(3) 0.0135(6) Uani 1 1 d . . . H12 H 0.3114 0.1634 -0.1545 0.016 Uiso 1 1 calc R . . C13 C 0.5234(4) 0.0572(3) -0.1693(3) 0.0149(6) Uani 1 1 d . . . H13 H 0.5102 0.0100 -0.2242 0.018 Uiso 1 1 calc R . . C14 C 0.6609(4) 0.0373(3) -0.1279(3) 0.0145(6) Uani 1 1 d . . . H14 H 0.7412 -0.0237 -0.1545 0.017 Uiso 1 1 calc R . . C15 C 0.6780(3) 0.1089(3) -0.0465(3) 0.0121(6) Uani 1 1 d . . . H15 H 0.7709 0.0957 -0.0194 0.015 Uiso 1 1 calc R . . C16 C 0.8179(3) -0.2272(3) 0.5903(3) 0.0120(6) Uani 1 1 d . . . H16A H 0.7542 -0.2461 0.6603 0.014 Uiso 1 1 calc R . . H16B H 0.8746 -0.3053 0.5645 0.014 Uiso 1 1 calc R . . C17 C 1.0748(3) 0.1616(3) 0.3752(3) 0.0111(5) Uani 1 1 d . . . H17A H 1.1299 0.0816 0.3528 0.013 Uiso 1 1 calc R . . H17B H 1.0059 0.1476 0.4431 0.013 Uiso 1 1 calc R . . C18 C 0.9890(3) 0.2401(3) 0.2712(3) 0.0122(6) Uani 1 1 d . . . H18A H 1.0590 0.2658 0.2094 0.015 Uiso 1 1 calc R . . H18B H 0.9236 0.3145 0.2986 0.015 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 Cu1 0.00598(16) 0.00864(17) 0.00912(16) -0.00268(13) -0.00199(12) 0.00012(13) V1 0.0078(2) 0.0100(2) 0.0097(2) -0.00286(18) -0.00035(17) -0.00031(18) V2 0.0069(2) 0.0076(2) 0.0083(2) -0.00205(17) -0.00052(17) -0.00133(17) P1 0.0060(3) 0.0095(3) 0.0088(3) -0.0017(3) -0.0011(3) -0.0008(3) P2 0.0068(3) 0.0081(3) 0.0094(3) -0.0023(3) -0.0005(3) -0.0012(3) O1 0.0091(9) 0.0085(9) 0.0096(9) -0.0013(8) -0.0004(7) -0.0013(8) O2 0.0105(10) 0.0115(10) 0.0128(10) -0.0056(8) 0.0023(8) -0.0037(8) O3 0.0074(9) 0.0102(10) 0.0101(9) -0.0044(8) 0.0003(7) -0.0024(8) O4 0.0078(9) 0.0128(10) 0.0111(10) -0.0015(8) -0.0002(8) -0.0015(8) O5 0.0074(9) 0.0130(10) 0.0102(10) -0.0002(8) -0.0025(8) -0.0012(8) O6 0.0108(10) 0.0107(10) 0.0127(10) -0.0023(8) 0.0008(8) 0.0010(8) O7 0.0069(9) 0.0090(10) 0.0130(10) -0.0018(8) -0.0003(8) -0.0012(8) O9 0.0100(10) 0.0141(11) 0.0168(11) -0.0037(9) -0.0025(8) -0.0007(8) O10 0.0146(11) 0.0172(11) 0.0139(10) -0.0070(9) 0.0019(8) -0.0054(9) O11 0.0127(10) 0.0114(10) 0.0135(10) -0.0048(8) 0.0015(8) -0.0036(8) O90 0.067(3) 0.068(3) 0.058(2) -0.014(2) -0.002(2) -0.024(2) O91 0.069(3) 0.056(3) 0.055(2) -0.012(2) 0.003(2) -0.011(2) N1 0.0092(11) 0.0103(11) 0.0093(11) -0.0020(9) -0.0016(9) -0.0021(9) N2 0.0074(11) 0.0094(11) 0.0107(11) -0.0005(9) -0.0041(9) -0.0015(9) N3 0.0095(11) 0.0122(12) 0.0108(11) -0.0038(9) -0.0017(9) -0.0011(9) C1 0.0113(13) 0.0094(13) 0.0148(14) -0.0022(11) -0.0035(11) -0.0024(11) C2 0.0153(15) 0.0125(14) 0.0186(15) -0.0056(12) -0.0064(12) -0.0018(12) C3 0.0175(16) 0.0166(15) 0.0198(16) -0.0085(13) -0.0054(13) -0.0006(13) C4 0.0113(14) 0.0152(15) 0.0193(15) -0.0066(12) -0.0044(12) 0.0016(12) C5 0.0117(13) 0.0089(13) 0.0120(13) -0.0030(10) -0.0034(11) -0.0015(11) C6 0.0110(13) 0.0088(13) 0.0092(12) -0.0024(10) -0.0009(10) -0.0018(11) C7 0.0100(13) 0.0113(13) 0.0097(13) -0.0028(10) -0.0024(10) -0.0010(11) C8 0.0077(13) 0.0102(13) 0.0085(12) -0.0015(10) -0.0003(10) -0.0016(10) C9 0.0081(13) 0.0113(13) 0.0123(13) -0.0047(11) -0.0014(10) -0.0021(11) C10 0.0101(13) 0.0105(13) 0.0103(13) -0.0027(10) 0.0008(10) -0.0027(11) C11 0.0078(13) 0.0106(13) 0.0125(13) -0.0041(11) -0.0020(10) -0.0006(10) C12 0.0113(14) 0.0133(14) 0.0167(14) -0.0064(12) -0.0028(11) -0.0011(11) C13 0.0134(14) 0.0125(14) 0.0198(15) -0.0086(12) -0.0005(12) -0.0013(11) C14 0.0140(14) 0.0116(14) 0.0171(15) -0.0062(12) 0.0002(12) -0.0001(11) C15 0.0076(13) 0.0131(14) 0.0149(14) -0.0053(11) 0.0003(11) 0.0000(11) C16 0.0125(14) 0.0099(13) 0.0141(14) -0.0012(11) -0.0044(11) -0.0027(11) C17 0.0115(13) 0.0112(13) 0.0115(13) -0.0011(11) -0.0038(11) -0.0036(11) C18 0.0114(14) 0.0111(13) 0.0137(14) 0.0005(11) -0.0033(11) -0.0029(11) _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 O5 1.913(2) . ? Cu1 N2 1.929(2) . ? Cu1 N3 2.026(3) . ? Cu1 N1 2.030(3) . ? Cu1 O4 2.215(2) . ? V1 O9 1.609(2) . ? V1 O10 1.630(2) . ? V1 O2 1.944(2) . ? V1 O6 1.998(2) . ? V1 O7 2.189(2) . ? V2 O11 1.617(2) . ? V2 O4 1.650(2) . ? V2 O1 1.942(2) . ? V2 O3 1.954(2) 2_656 ? V2 O7 2.081(2) . ? P1 O5 1.510(2) . ? P1 O6 1.543(2) . ? P1 O7 1.561(2) . ? P1 C18 1.789(3) . ? P2 O3 1.526(2) . ? P2 O1 1.528(2) . ? P2 O2 1.536(2) . ? P2 C16 1.791(3) . ? O3 V2 1.954(2) 2_656 ? N1 C1 1.343(4) . ? N1 C5 1.358(4) . ? N2 C10 1.334(4) . ? N2 C6 1.343(4) . ? N3 C15 1.348(4) . ? N3 C11 1.358(4) . ? C1 C2 1.375(4) . ? C2 C3 1.383(5) . ? C3 C4 1.392(4) . ? C4 C5 1.374(4) . ? C5 C6 1.486(4) . ? C6 C7 1.384(4) . ? C7 C8 1.404(4) . ? C8 C9 1.411(4) . ? C8 C8 1.492(6) 2_565 ? C9 C10 1.390(4) . ? C10 C11 1.482(4) . ? C11 C12 1.382(4) . ? C12 C13 1.391(4) . ? C13 C14 1.381(4) . ? C14 C15 1.384(4) . ? C16 C17 1.531(4) 2_756 ? C17 C18 1.530(4) . ? C17 C16 1.531(4) 2_756 ? 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 O5 Cu1 N2 167.99(10) . . ? O5 Cu1 N3 98.54(10) . . ? N2 Cu1 N3 79.67(10) . . ? O5 Cu1 N1 99.11(10) . . ? N2 Cu1 N1 80.13(10) . . ? N3 Cu1 N1 157.40(10) . . ? O5 Cu1 O4 94.81(8) . . ? N2 Cu1 O4 97.19(9) . . ? N3 Cu1 O4 100.16(9) . . ? N1 Cu1 O4 92.30(9) . . ? O9 V1 O10 107.30(12) . . ? O9 V1 O2 103.85(11) . . ? O10 V1 O2 95.17(10) . . ? O9 V1 O6 103.27(11) . . ? O10 V1 O6 96.95(10) . . ? O2 V1 O6 145.36(9) . . ? O9 V1 O7 109.73(10) . . ? O10 V1 O7 142.37(10) . . ? O2 V1 O7 82.45(9) . . ? O6 V1 O7 68.32(8) . . ? O11 V2 O4 109.86(11) . . ? O11 V2 O1 122.79(10) . . ? O4 V2 O1 126.33(10) . . ? O11 V2 O3 97.30(10) . 2_656 ? O4 V2 O3 98.23(10) . 2_656 ? O1 V2 O3 85.53(9) . 2_656 ? O11 V2 O7 90.93(10) . . ? O4 V2 O7 89.40(9) . . ? O1 V2 O7 80.61(9) . . ? O3 V2 O7 166.11(9) 2_656 . ? O5 P1 O6 115.20(12) . . ? O5 P1 O7 114.74(12) . . ? O6 P1 O7 98.77(12) . . ? O5 P1 C18 107.37(13) . . ? O6 P1 C18 109.64(14) . . ? O7 P1 C18 110.96(13) . . ? O3 P2 O1 112.41(12) . . ? O3 P2 O2 107.69(12) . . ? O1 P2 O2 111.82(12) . . ? O3 P2 C16 108.13(13) . . ? O1 P2 C16 106.68(13) . . ? O2 P2 C16 110.05(14) . . ? P2 O1 V2 137.48(13) . . ? P2 O2 V1 136.16(13) . . ? P2 O3 V2 126.90(12) . 2_656 ? V2 O4 Cu1 128.20(12) . . ? P1 O5 Cu1 134.22(14) . . ? P1 O6 V1 100.40(11) . . ? P1 O7 V2 124.58(12) . . ? P1 O7 V1 92.14(10) . . ? V2 O7 V1 141.81(11) . . ? C1 N1 C5 118.2(3) . . ? C1 N1 Cu1 127.1(2) . . ? C5 N1 Cu1 114.12(19) . . ? C10 N2 C6 121.5(3) . . ? C10 N2 Cu1 119.6(2) . . ? C6 N2 Cu1 119.0(2) . . ? C15 N3 C11 118.8(3) . . ? C15 N3 Cu1 126.8(2) . . ? C11 N3 Cu1 114.4(2) . . ? N1 C1 C2 122.5(3) . . ? C1 C2 C3 119.1(3) . . ? C2 C3 C4 119.1(3) . . ? C5 C4 C3 118.6(3) . . ? N1 C5 C4 122.4(3) . . ? N1 C5 C6 113.7(3) . . ? C4 C5 C6 123.9(3) . . ? N2 C6 C7 121.2(3) . . ? N2 C6 C5 112.6(3) . . ? C7 C6 C5 126.2(3) . . ? C6 C7 C8 118.8(3) . . ? C7 C8 C9 118.8(3) . . ? C7 C8 C8 120.4(3) . 2_565 ? C9 C8 C8 120.9(3) . 2_565 ? C10 C9 C8 118.9(3) . . ? N2 C10 C9 120.9(3) . . ? N2 C10 C11 112.2(3) . . ? C9 C10 C11 126.9(3) . . ? N3 C11 C12 122.0(3) . . ? N3 C11 C10 113.8(3) . . ? C12 C11 C10 124.2(3) . . ? C11 C12 C13 118.8(3) . . ? C14 C13 C12 119.3(3) . . ? C13 C14 C15 119.3(3) . . ? N3 C15 C14 121.9(3) . . ? C17 C16 P2 113.9(2) 2_756 . ? C18 C17 C16 110.5(2) . 2_756 ? C17 C18 P1 115.0(2) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O3 P2 O1 V2 -86.3(2) . . . . ? O2 P2 O1 V2 34.9(2) . . . . ? C16 P2 O1 V2 155.29(19) . . . . ? O11 V2 O1 P2 -139.22(19) . . . . ? O4 V2 O1 P2 28.0(2) . . . . ? O3 V2 O1 P2 125.0(2) 2_656 . . . ? O7 V2 O1 P2 -54.22(19) . . . . ? O3 P2 O2 V1 163.62(18) . . . . ? O1 P2 O2 V1 39.7(2) . . . . ? C16 P2 O2 V1 -78.7(2) . . . . ? O9 V1 O2 P2 63.0(2) . . . . ? O10 V1 O2 P2 172.3(2) . . . . ? O6 V1 O2 P2 -77.6(3) . . . . ? O7 V1 O2 P2 -45.55(19) . . . . ? O1 P2 O3 V2 -41.03(19) . . . 2_656 ? O2 P2 O3 V2 -164.64(14) . . . 2_656 ? C16 P2 O3 V2 76.47(19) . . . 2_656 ? O11 V2 O4 Cu1 35.29(18) . . . . ? O1 V2 O4 Cu1 -133.35(13) . . . . ? O3 V2 O4 Cu1 136.16(14) 2_656 . . . ? O7 V2 O4 Cu1 -55.48(14) . . . . ? O5 Cu1 O4 V2 31.69(16) . . . . ? N2 Cu1 O4 V2 -147.98(15) . . . . ? N3 Cu1 O4 V2 131.28(15) . . . . ? N1 Cu1 O4 V2 -67.65(16) . . . . ? O6 P1 O5 Cu1 110.05(19) . . . . ? O7 P1 O5 Cu1 -3.7(2) . . . . ? C18 P1 O5 Cu1 -127.51(19) . . . . ? N2 Cu1 O5 P1 -170.4(4) . . . . ? N3 Cu1 O5 P1 -89.9(2) . . . . ? N1 Cu1 O5 P1 104.31(19) . . . . ? O4 Cu1 O5 P1 11.19(19) . . . . ? O5 P1 O6 V1 -128.23(12) . . . . ? O7 P1 O6 V1 -5.51(13) . . . . ? C18 P1 O6 V1 110.56(13) . . . . ? O9 V1 O6 P1 -102.06(13) . . . . ? O10 V1 O6 P1 148.28(12) . . . . ? O2 V1 O6 P1 38.6(2) . . . . ? O7 V1 O6 P1 4.17(10) . . . . ? O5 P1 O7 V2 -40.83(19) . . . . ? O6 P1 O7 V2 -163.88(14) . . . . ? C18 P1 O7 V2 81.07(17) . . . . ? O5 P1 O7 V1 128.00(11) . . . . ? O6 P1 O7 V1 4.94(11) . . . . ? C18 P1 O7 V1 -110.10(12) . . . . ? O11 V2 O7 P1 -44.66(16) . . . . ? O4 V2 O7 P1 65.19(16) . . . . ? O1 V2 O7 P1 -167.78(16) . . . . ? O3 V2 O7 P1 -171.2(3) 2_656 . . . ? O11 V2 O7 V1 153.59(18) . . . . ? O4 V2 O7 V1 -96.56(18) . . . . ? O1 V2 O7 V1 30.47(17) . . . . ? O3 V2 O7 V1 27.1(5) 2_656 . . . ? O9 V1 O7 P1 92.82(12) . . . . ? O10 V1 O7 P1 -76.45(18) . . . . ? O2 V1 O7 P1 -165.12(11) . . . . ? O6 V1 O7 P1 -4.06(9) . . . . ? O9 V1 O7 V2 -102.14(18) . . . . ? O10 V1 O7 V2 88.6(2) . . . . ? O2 V1 O7 V2 -0.07(17) . . . . ? O6 V1 O7 V2 161.0(2) . . . . ? O5 Cu1 N1 C1 -14.6(3) . . . . ? N2 Cu1 N1 C1 177.6(3) . . . . ? N3 Cu1 N1 C1 -155.5(3) . . . . ? O4 Cu1 N1 C1 80.7(3) . . . . ? O5 Cu1 N1 C5 174.1(2) . . . . ? N2 Cu1 N1 C5 6.3(2) . . . . ? N3 Cu1 N1 C5 33.2(4) . . . . ? O4 Cu1 N1 C5 -90.6(2) . . . . ? O5 Cu1 N2 C10 88.4(5) . . . . ? N3 Cu1 N2 C10 5.9(2) . . . . ? N1 Cu1 N2 C10 175.8(2) . . . . ? O4 Cu1 N2 C10 -93.1(2) . . . . ? O5 Cu1 N2 C6 -92.1(5) . . . . ? N3 Cu1 N2 C6 -174.6(2) . . . . ? N1 Cu1 N2 C6 -4.8(2) . . . . ? O4 Cu1 N2 C6 86.3(2) . . . . ? O5 Cu1 N3 C15 6.0(3) . . . . ? N2 Cu1 N3 C15 174.0(3) . . . . ? N1 Cu1 N3 C15 147.0(3) . . . . ? O4 Cu1 N3 C15 -90.5(3) . . . . ? O5 Cu1 N3 C11 -172.8(2) . . . . ? N2 Cu1 N3 C11 -4.8(2) . . . . ? N1 Cu1 N3 C11 -31.8(4) . . . . ? O4 Cu1 N3 C11 90.7(2) . . . . ? C5 N1 C1 C2 -0.1(5) . . . . ? Cu1 N1 C1 C2 -171.0(2) . . . . ? N1 C1 C2 C3 -1.2(5) . . . . ? C1 C2 C3 C4 1.2(5) . . . . ? C2 C3 C4 C5 -0.1(5) . . . . ? C1 N1 C5 C4 1.3(5) . . . . ? Cu1 N1 C5 C4 173.4(3) . . . . ? C1 N1 C5 C6 -178.8(3) . . . . ? Cu1 N1 C5 C6 -6.7(3) . . . . ? C3 C4 C5 N1 -1.2(5) . . . . ? C3 C4 C5 C6 178.9(3) . . . . ? C10 N2 C6 C7 1.2(4) . . . . ? Cu1 N2 C6 C7 -178.3(2) . . . . ? C10 N2 C6 C5 -178.1(3) . . . . ? Cu1 N2 C6 C5 2.5(3) . . . . ? N1 C5 C6 N2 3.0(4) . . . . ? C4 C5 C6 N2 -177.1(3) . . . . ? N1 C5 C6 C7 -176.2(3) . . . . ? C4 C5 C6 C7 3.7(5) . . . . ? N2 C6 C7 C8 1.2(4) . . . . ? C5 C6 C7 C8 -179.7(3) . . . . ? C6 C7 C8 C9 -1.6(4) . . . . ? C6 C7 C8 C8 178.2(3) . . . 2_565 ? C7 C8 C9 C10 -0.1(4) . . . . ? C8 C8 C9 C10 -180.0(3) 2_565 . . . ? C6 N2 C10 C9 -3.0(4) . . . . ? Cu1 N2 C10 C9 176.4(2) . . . . ? C6 N2 C10 C11 174.9(3) . . . . ? Cu1 N2 C10 C11 -5.7(3) . . . . ? C8 C9 C10 N2 2.5(4) . . . . ? C8 C9 C10 C11 -175.1(3) . . . . ? C15 N3 C11 C12 1.3(5) . . . . ? Cu1 N3 C11 C12 -179.9(2) . . . . ? C15 N3 C11 C10 -175.6(3) . . . . ? Cu1 N3 C11 C10 3.3(3) . . . . ? N2 C10 C11 N3 1.3(4) . . . . ? C9 C10 C11 N3 179.0(3) . . . . ? N2 C10 C11 C12 -175.5(3) . . . . ? C9 C10 C11 C12 2.2(5) . . . . ? N3 C11 C12 C13 -0.9(5) . . . . ? C10 C11 C12 C13 175.7(3) . . . . ? C11 C12 C13 C14 0.3(5) . . . . ? C12 C13 C14 C15 -0.2(5) . . . . ? C11 N3 C15 C14 -1.1(5) . . . . ? Cu1 N3 C15 C14 -179.9(2) . . . . ? C13 C14 C15 N3 0.6(5) . . . . ? O3 P2 C16 C17 -159.3(2) . . . 2_756 ? O1 P2 C16 C17 -38.2(3) . . . 2_756 ? O2 P2 C16 C17 83.3(2) . . . 2_756 ? C16 C17 C18 P1 170.9(2) 2_756 . . . ? O5 P1 C18 C17 167.4(2) . . . . ? O6 P1 C18 C17 -66.8(3) . . . . ? O7 P1 C18 C17 41.3(3) . . . . ? _diffrn_measured_fraction_theta_max 0.974 _diffrn_reflns_theta_full 31.68 _diffrn_measured_fraction_theta_full 0.974 _refine_diff_density_max 1.148 _refine_diff_density_min -1.076 _refine_diff_density_rms 0.147 data_Compound_4 _database_code_depnum_ccdc_archive 'CCDC 229553' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H37 Cu2 N6 O15 P4 V' _chemical_formula_weight 1095.62 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' 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' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.7056(4) _cell_length_b 15.8466(8) _cell_length_c 15.9357(8) _cell_angle_alpha 115.262(1) _cell_angle_beta 94.060(1) _cell_angle_gamma 90.000(1) _cell_volume 1982.05(17) _cell_formula_units_Z 2 _cell_measurement_temperature 90(2) _cell_measurement_reflns_used 25949 _cell_measurement_theta_min 2.35 _cell_measurement_theta_max 31.50 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.29 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.836 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1112 _exptl_absorpt_coefficient_mu 1.538 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6640 _exptl_absorpt_correction_T_max 0.8490 _exptl_absorpt_process_details 'SADABS SHELXL-97 (SHELDRICK, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 90(2) _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_probe x-ray _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'APEX CCD area detector' _diffrn_measurement_method 'Phi and omega scans' _diffrn_detector_area_resol_mean 512 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.001 _diffrn_reflns_number 25949 _diffrn_reflns_av_R_equivalents 0.0281 _diffrn_reflns_av_sigmaI/netI 0.0472 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.35 _diffrn_reflns_theta_max 31.50 _reflns_number_total 12930 _reflns_number_gt 10802 _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 and CrystalMaker 5.x' _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^)+(0.0458P)^2^+1.3576P] 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 12930 _refine_ls_number_parameters 580 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0499 _refine_ls_R_factor_gt 0.0394 _refine_ls_wR_factor_ref 0.0972 _refine_ls_wR_factor_gt 0.0918 _refine_ls_goodness_of_fit_ref 1.014 _refine_ls_restrained_S_all 1.014 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.38443(3) 0.941374(17) 0.344303(17) 0.00980(6) Uani 1 1 d . . . Cu2 Cu 0.15439(3) 0.409710(17) 0.248677(17) 0.00820(6) Uani 1 1 d . . . V1 V 0.39193(4) 0.60780(2) 0.24871(2) 0.00839(7) Uani 1 1 d . . . P1 P 0.59539(6) 0.76651(3) 0.22866(4) 0.00826(9) Uani 1 1 d . . . P2 P 0.46035(6) 0.38812(4) 0.16500(4) 0.00929(10) Uani 1 1 d . . . P3 P -0.11625(6) 0.23585(4) 0.22800(4) 0.00964(10) Uani 1 1 d . . . P4 P 0.06158(6) 0.08275(4) -0.13880(4) 0.01095(10) Uani 1 1 d . . . O1 O 0.54777(18) 0.85760(10) 0.30413(10) 0.0133(3) Uani 1 1 d . . . O2 O 0.55683(17) 0.68366(10) 0.25349(10) 0.0122(3) Uani 1 1 d . . . O3 O 0.37435(18) 0.61736(11) 0.35253(11) 0.0150(3) Uani 1 1 d . . . O4 O 0.23551(18) 0.64416(11) 0.21390(11) 0.0150(3) Uani 1 1 d . . . O5 O 0.42168(18) 0.48569(10) 0.16631(11) 0.0142(3) Uani 1 1 d . . . O6 O 0.58636(18) 0.39730(11) 0.23807(11) 0.0163(3) Uani 1 1 d . . . O7 O 0.31132(17) 0.33988(10) 0.16930(10) 0.0112(3) Uani 1 1 d . . . O8 O 0.01140(18) 0.30881(11) 0.26432(11) 0.0157(3) Uani 1 1 d . . . O9 O -0.27051(18) 0.27418(11) 0.27491(11) 0.0155(3) Uani 1 1 d . . . H9' H -0.3071 0.3124 0.2558 0.023 Uiso 1 1 calc R . . O10 O -0.07953(18) 0.15103(10) 0.24565(11) 0.0141(3) Uani 1 1 d . . . O11 O 0.1733(2) 0.17025(12) -0.10240(11) 0.0190(3) Uani 1 1 d . . . H11' H 0.1812 0.1879 -0.1447 0.029 Uiso 1 1 calc R . . O12 O -0.00539(18) 0.05539(11) -0.23631(10) 0.0141(3) Uani 1 1 d . . . O13 O 0.15270(19) 0.00528(11) -0.12570(11) 0.0155(3) Uani 1 1 d . . . H13' H 0.1204 -0.0471 -0.1667 0.023 Uiso 1 1 calc R . . O14 O 0.76567(17) 0.76503(10) 0.21594(10) 0.0117(3) Uani 1 1 d . . . O90 O 0.1986(2) 0.83935(13) 0.27118(17) 0.0373(5) Uani 1 1 d . . . N1 N 0.4075(2) 1.01415(12) 0.26477(12) 0.0105(3) Uani 1 1 d . . . N2 N 0.2607(2) 1.04867(12) 0.40865(12) 0.0106(3) Uani 1 1 d . . . N3 N 0.3499(2) 0.92427(12) 0.46183(13) 0.0120(3) Uani 1 1 d . . . N4 N 0.2610(2) 0.43591(12) 0.37566(12) 0.0096(3) Uani 1 1 d . . . N5 N 0.05153(19) 0.52268(12) 0.32617(12) 0.0090(3) Uani 1 1 d . . . N6 N 0.0260(2) 0.43255(12) 0.14930(12) 0.0097(3) Uani 1 1 d . . . C1 C 0.4979(2) 0.99592(14) 0.19492(15) 0.0129(4) Uani 1 1 d . . . H1 H 0.5699 0.9478 0.1824 0.015 Uiso 1 1 calc R . . C2 C 0.4906(3) 1.04449(15) 0.14004(15) 0.0151(4) Uani 1 1 d . . . H2 H 0.5567 1.0299 0.0911 0.018 Uiso 1 1 calc R . . C3 C 0.3856(3) 1.11440(15) 0.15769(15) 0.0152(4) Uani 1 1 d . . . H3 H 0.3761 1.1470 0.1196 0.018 Uiso 1 1 calc R . . C4 C 0.2939(2) 1.13639(15) 0.23207(15) 0.0132(4) Uani 1 1 d . . . H4 H 0.2221 1.1848 0.2462 0.016 Uiso 1 1 calc R . . C5 C 0.3097(2) 1.08620(14) 0.28486(14) 0.0104(4) Uani 1 1 d . . . C6 C 0.2349(2) 1.10989(14) 0.37214(14) 0.0104(4) Uani 1 1 d . . . C7 C 0.2155(2) 1.06394(14) 0.49266(14) 0.0104(4) Uani 1 1 d . . . C8 C 0.2552(2) 0.98718(14) 0.51908(14) 0.0116(4) Uani 1 1 d . . . C9 C 0.1992(2) 0.97818(15) 0.59439(14) 0.0129(4) Uani 1 1 d . . . H9 H 0.1346 1.0238 0.6344 0.015 Uiso 1 1 calc R . . C10 C 0.2401(3) 0.90083(15) 0.60978(15) 0.0145(4) Uani 1 1 d . . . H10 H 0.2023 0.8923 0.6602 0.017 Uiso 1 1 calc R . . C11 C 0.3365(3) 0.83614(15) 0.55092(16) 0.0163(4) Uani 1 1 d . . . H11 H 0.3655 0.7829 0.5604 0.020 Uiso 1 1 calc R . . C12 C 0.3898(3) 0.85062(15) 0.47778(16) 0.0148(4) Uani 1 1 d . . . H12 H 0.4568 0.8068 0.4379 0.018 Uiso 1 1 calc R . . C13 C 0.4868(2) 0.74476(14) 0.12060(14) 0.0113(4) Uani 1 1 d . . . H13A H 0.3804 0.7252 0.1241 0.014 Uiso 1 1 calc R . . H13B H 0.4809 0.8043 0.1145 0.014 Uiso 1 1 calc R . . C14 C 0.5314(2) 0.32243(14) 0.05295(14) 0.0111(4) Uani 1 1 d . . . H14A H 0.6408 0.3416 0.0569 0.013 Uiso 1 1 calc R . . H14B H 0.5290 0.2558 0.0412 0.013 Uiso 1 1 calc R . . C15 C 0.4503(2) 0.32915(14) -0.03195(14) 0.0113(4) Uani 1 1 d . . . H15A H 0.4686 0.3922 -0.0285 0.014 Uiso 1 1 calc R . . H15B H 0.3379 0.3186 -0.0334 0.014 Uiso 1 1 calc R . . C16 C 0.0156(2) 0.37789(14) 0.05757(14) 0.0111(4) Uani 1 1 d . . . H16 H 0.0796 0.3256 0.0341 0.013 Uiso 1 1 calc R . . C17 C -0.0854(2) 0.39498(14) -0.00436(14) 0.0120(4) Uani 1 1 d . . . H17 H -0.0918 0.3544 -0.0689 0.014 Uiso 1 1 calc R . . C18 C -0.1768(2) 0.47242(15) 0.02972(15) 0.0125(4) Uani 1 1 d . . . H18 H -0.2466 0.4856 -0.0114 0.015 Uiso 1 1 calc R . . C19 C -0.1653(2) 0.53061(15) 0.12482(15) 0.0121(4) Uani 1 1 d . . . H19 H -0.2264 0.5842 0.1495 0.015 Uiso 1 1 calc R . . C20 C -0.0627(2) 0.50860(14) 0.18261(14) 0.0098(3) Uani 1 1 d . . . C21 C -0.0378(2) 0.56464(14) 0.28488(14) 0.0096(3) Uani 1 1 d . . . C22 C -0.0940(2) 0.65257(14) 0.33613(14) 0.0109(4) Uani 1 1 d . . . H22 H -0.1570 0.6826 0.3067 0.013 Uiso 1 1 calc R . . C23 C -0.0554(2) 0.69571(14) 0.43250(14) 0.0101(4) Uani 1 1 d . . . C24 C -0.1190(2) 0.78806(14) 0.48978(14) 0.0108(4) Uani 1 1 d . . . C25 C -0.1603(2) 0.80773(14) 0.57909(14) 0.0108(4) Uani 1 1 d . . . H25 H -0.1378 0.7656 0.6061 0.013 Uiso 1 1 calc R . . C26 C -0.1457(2) 0.85361(14) 0.45323(14) 0.0115(4) Uani 1 1 d . . . H26 H -0.1169 0.8419 0.3929 0.014 Uiso 1 1 calc R . . C27 C 0.0381(2) 0.65029(14) 0.47424(14) 0.0102(4) Uani 1 1 d . . . H27 H 0.0642 0.6783 0.5395 0.012 Uiso 1 1 calc R . . C28 C 0.0921(2) 0.56302(14) 0.41785(14) 0.0091(3) Uani 1 1 d . . . C29 C 0.1997(2) 0.50678(13) 0.44748(14) 0.0091(3) Uani 1 1 d . . . C30 C 0.2361(2) 0.52270(14) 0.53886(14) 0.0115(4) Uani 1 1 d . . . H30 H 0.1919 0.5725 0.5881 0.014 Uiso 1 1 calc R . . C31 C 0.3393(2) 0.46425(14) 0.55761(15) 0.0128(4) Uani 1 1 d . . . H31 H 0.3652 0.4732 0.6198 0.015 Uiso 1 1 calc R . . C32 C 0.4031(3) 0.39321(14) 0.48415(15) 0.0135(4) Uani 1 1 d . . . H32 H 0.4745 0.3532 0.4954 0.016 Uiso 1 1 calc R . . C33 C 0.3616(2) 0.38106(14) 0.39376(14) 0.0108(4) Uani 1 1 d . . . H33 H 0.4061 0.3324 0.3435 0.013 Uiso 1 1 calc R . . C34 C -0.1613(2) 0.19788(15) 0.10529(14) 0.0116(4) Uani 1 1 d . . . H34A H -0.2527 0.1548 0.0857 0.014 Uiso 1 1 calc R . . H34B H -0.1898 0.2529 0.0941 0.014 Uiso 1 1 calc R . . C35 C -0.0320(2) 0.14890(14) 0.04377(14) 0.0116(4) Uani 1 1 d . . . H35A H -0.0007 0.0942 0.0547 0.014 Uiso 1 1 calc R . . H35B H 0.0587 0.1922 0.0600 0.014 Uiso 1 1 calc R . . C36 C -0.0869(2) 0.11702(15) -0.05930(14) 0.0135(4) Uani 1 1 d . . . H36A H -0.1429 0.1686 -0.0658 0.016 Uiso 1 1 calc R . . H36B H -0.1612 0.0637 -0.0778 0.016 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 Cu1 0.01330(12) 0.00685(11) 0.00849(11) 0.00227(9) 0.00274(9) 0.00249(9) Cu2 0.01011(11) 0.00735(11) 0.00641(11) 0.00220(8) 0.00096(8) 0.00204(8) V1 0.01006(15) 0.00657(14) 0.00864(15) 0.00337(12) 0.00066(12) 0.00005(11) P1 0.0105(2) 0.0068(2) 0.0076(2) 0.00301(17) 0.00195(17) 0.00162(17) P2 0.0111(2) 0.0079(2) 0.0070(2) 0.00146(17) 0.00055(18) 0.00143(17) P3 0.0119(2) 0.0082(2) 0.0086(2) 0.00327(18) 0.00174(18) -0.00038(18) P4 0.0139(2) 0.0095(2) 0.0091(2) 0.00357(19) 0.00154(19) -0.00055(18) O1 0.0166(7) 0.0107(7) 0.0108(7) 0.0029(6) 0.0022(6) 0.0050(6) O2 0.0131(7) 0.0114(7) 0.0145(7) 0.0078(6) 0.0007(6) -0.0014(5) O3 0.0190(8) 0.0145(7) 0.0126(7) 0.0068(6) 0.0016(6) -0.0009(6) O4 0.0140(7) 0.0127(7) 0.0191(8) 0.0079(6) -0.0013(6) 0.0016(6) O5 0.0199(8) 0.0072(6) 0.0137(7) 0.0025(6) 0.0035(6) 0.0025(6) O6 0.0158(7) 0.0176(8) 0.0102(7) 0.0014(6) -0.0020(6) 0.0024(6) O7 0.0119(7) 0.0103(6) 0.0107(7) 0.0036(5) 0.0031(5) 0.0017(5) O8 0.0173(7) 0.0147(7) 0.0156(7) 0.0073(6) -0.0013(6) -0.0057(6) O9 0.0165(7) 0.0158(7) 0.0145(7) 0.0061(6) 0.0056(6) 0.0038(6) O10 0.0215(8) 0.0102(7) 0.0120(7) 0.0059(6) 0.0013(6) 0.0007(6) O11 0.0281(9) 0.0167(8) 0.0126(7) 0.0068(6) 0.0009(7) -0.0094(7) O12 0.0195(8) 0.0129(7) 0.0094(7) 0.0042(6) 0.0010(6) 0.0009(6) O13 0.0203(8) 0.0103(7) 0.0135(7) 0.0032(6) -0.0010(6) 0.0030(6) O14 0.0106(6) 0.0128(7) 0.0130(7) 0.0065(6) 0.0027(5) 0.0006(5) O90 0.0257(10) 0.0130(8) 0.0611(15) 0.0080(9) -0.0217(10) -0.0009(7) N1 0.0121(8) 0.0073(7) 0.0106(8) 0.0024(6) 0.0014(6) 0.0010(6) N2 0.0132(8) 0.0081(7) 0.0089(7) 0.0023(6) 0.0006(6) 0.0011(6) N3 0.0145(8) 0.0089(7) 0.0126(8) 0.0043(6) 0.0030(7) 0.0018(6) N4 0.0117(8) 0.0075(7) 0.0089(7) 0.0029(6) 0.0007(6) 0.0001(6) N5 0.0105(7) 0.0085(7) 0.0075(7) 0.0028(6) 0.0009(6) 0.0001(6) N6 0.0117(8) 0.0071(7) 0.0092(7) 0.0023(6) 0.0023(6) 0.0012(6) C1 0.0153(9) 0.0086(8) 0.0134(9) 0.0031(7) 0.0033(8) 0.0014(7) C2 0.0171(10) 0.0145(9) 0.0142(10) 0.0058(8) 0.0060(8) 0.0005(8) C3 0.0183(10) 0.0148(10) 0.0152(10) 0.0087(8) 0.0027(8) 0.0004(8) C4 0.0151(9) 0.0117(9) 0.0129(9) 0.0051(8) 0.0026(8) 0.0015(7) C5 0.0114(9) 0.0083(8) 0.0097(9) 0.0019(7) 0.0017(7) 0.0001(7) C6 0.0106(8) 0.0087(8) 0.0103(9) 0.0027(7) 0.0004(7) 0.0012(7) C7 0.0131(9) 0.0084(8) 0.0083(8) 0.0023(7) 0.0019(7) 0.0016(7) C8 0.0134(9) 0.0089(8) 0.0112(9) 0.0029(7) 0.0011(7) 0.0006(7) C9 0.0146(9) 0.0120(9) 0.0099(9) 0.0024(7) 0.0025(7) -0.0007(7) C10 0.0175(10) 0.0135(9) 0.0128(9) 0.0060(8) 0.0013(8) -0.0018(8) C11 0.0219(11) 0.0114(9) 0.0173(10) 0.0076(8) 0.0028(8) 0.0007(8) C12 0.0189(10) 0.0101(9) 0.0157(10) 0.0054(8) 0.0036(8) 0.0013(8) C13 0.0140(9) 0.0107(9) 0.0082(8) 0.0030(7) 0.0012(7) 0.0017(7) C14 0.0133(9) 0.0115(9) 0.0087(8) 0.0044(7) 0.0023(7) 0.0031(7) C15 0.0142(9) 0.0105(8) 0.0092(9) 0.0040(7) 0.0021(7) 0.0034(7) C16 0.0145(9) 0.0083(8) 0.0088(9) 0.0018(7) 0.0029(7) 0.0004(7) C17 0.0149(9) 0.0101(9) 0.0093(9) 0.0028(7) 0.0005(7) -0.0022(7) C18 0.0127(9) 0.0139(9) 0.0114(9) 0.0062(8) -0.0015(7) -0.0009(7) C19 0.0119(9) 0.0124(9) 0.0122(9) 0.0053(7) 0.0009(7) 0.0025(7) C20 0.0101(8) 0.0095(8) 0.0091(8) 0.0033(7) 0.0013(7) 0.0004(7) C21 0.0104(8) 0.0087(8) 0.0091(8) 0.0033(7) 0.0001(7) 0.0005(7) C22 0.0116(9) 0.0092(8) 0.0107(9) 0.0030(7) 0.0012(7) 0.0023(7) C23 0.0113(9) 0.0080(8) 0.0100(9) 0.0024(7) 0.0032(7) 0.0013(7) C24 0.0109(8) 0.0094(8) 0.0096(9) 0.0016(7) 0.0016(7) 0.0011(7) C25 0.0120(9) 0.0088(8) 0.0104(9) 0.0031(7) 0.0001(7) 0.0019(7) C26 0.0132(9) 0.0101(9) 0.0089(9) 0.0016(7) 0.0024(7) 0.0017(7) C27 0.0109(8) 0.0097(8) 0.0086(8) 0.0024(7) 0.0014(7) 0.0003(7) C28 0.0100(8) 0.0080(8) 0.0092(8) 0.0036(7) 0.0012(7) -0.0012(6) C29 0.0107(8) 0.0073(8) 0.0085(8) 0.0027(7) 0.0007(7) 0.0001(7) C30 0.0155(9) 0.0091(8) 0.0087(9) 0.0028(7) 0.0004(7) -0.0009(7) C31 0.0150(9) 0.0119(9) 0.0110(9) 0.0046(7) -0.0011(7) -0.0007(7) C32 0.0158(9) 0.0104(9) 0.0142(9) 0.0055(8) -0.0017(8) 0.0016(7) C33 0.0119(9) 0.0085(8) 0.0117(9) 0.0040(7) 0.0002(7) 0.0011(7) C34 0.0129(9) 0.0127(9) 0.0087(9) 0.0042(7) 0.0009(7) 0.0019(7) C35 0.0127(9) 0.0123(9) 0.0102(9) 0.0053(7) 0.0008(7) 0.0009(7) C36 0.0141(9) 0.0164(10) 0.0103(9) 0.0057(8) 0.0017(7) 0.0012(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 Cu1 O1 1.8967(15) . ? Cu1 N2 1.9418(17) . ? Cu1 N3 2.0456(18) . ? Cu1 N1 2.0640(18) . ? Cu1 O90 2.1709(19) . ? Cu2 O7 1.9342(14) . ? Cu2 N5 1.9497(17) . ? Cu2 N6 2.0313(18) . ? Cu2 N4 2.0360(17) . ? Cu2 O8 2.1336(15) . ? V1 O3 1.6141(16) . ? V1 O4 1.6309(16) . ? V1 O5 1.8480(15) . ? V1 O2 1.8488(15) . ? P1 O14 1.5092(15) . ? P1 O1 1.5135(15) . ? P1 O2 1.5669(15) . ? P1 C13 1.800(2) . ? P2 O6 1.5016(16) . ? P2 O7 1.5263(15) . ? P2 O5 1.5742(16) . ? P2 C14 1.796(2) . ? P3 O8 1.4981(16) . ? P3 O10 1.5159(16) . ? P3 O9 1.5767(16) . ? P3 C34 1.796(2) . ? P4 O12 1.4965(16) . ? P4 O13 1.5411(16) . ? P4 O11 1.5618(16) . ? P4 C36 1.793(2) . ? N1 C1 1.338(3) . ? N1 C5 1.363(3) . ? N2 C6 1.339(3) . ? N2 C7 1.343(3) . ? N3 C12 1.337(3) . ? N3 C8 1.355(3) . ? N4 C33 1.336(3) . ? N4 C29 1.359(2) . ? N5 C21 1.334(3) . ? N5 C28 1.341(3) . ? N6 C16 1.340(3) . ? N6 C20 1.357(3) . ? C1 C2 1.389(3) . ? C2 C3 1.383(3) . ? C3 C4 1.395(3) . ? C4 C5 1.384(3) . ? C5 C6 1.477(3) . ? C6 C25 1.391(3) 2_576 ? C7 C26 1.390(3) 2_576 ? C7 C8 1.481(3) . ? C8 C9 1.388(3) . ? C9 C10 1.390(3) . ? C10 C11 1.388(3) . ? C11 C12 1.390(3) . ? C13 C15 1.538(3) 2_665 ? C14 C15 1.526(3) . ? C15 C13 1.538(3) 2_665 ? C16 C17 1.387(3) . ? C17 C18 1.388(3) . ? C18 C19 1.394(3) . ? C19 C20 1.388(3) . ? C20 C21 1.485(3) . ? C21 C22 1.391(3) . ? C22 C23 1.403(3) . ? C23 C27 1.398(3) . ? C23 C24 1.488(3) . ? C24 C25 1.395(3) . ? C24 C26 1.403(3) . ? C25 C6 1.391(3) 2_576 ? C26 C7 1.390(3) 2_576 ? C27 C28 1.393(3) . ? C28 C29 1.480(3) . ? C29 C30 1.381(3) . ? C30 C31 1.397(3) . ? C31 C32 1.383(3) . ? C32 C33 1.390(3) . ? C34 C35 1.529(3) . ? C35 C36 1.537(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Cu1 N2 164.64(7) . . ? O1 Cu1 N3 97.14(7) . . ? N2 Cu1 N3 79.73(7) . . ? O1 Cu1 N1 100.31(7) . . ? N2 Cu1 N1 79.23(7) . . ? N3 Cu1 N1 156.38(7) . . ? O1 Cu1 O90 96.49(7) . . ? N2 Cu1 O90 98.47(8) . . ? N3 Cu1 O90 88.84(9) . . ? N1 Cu1 O90 104.77(8) . . ? O7 Cu2 N5 154.96(7) . . ? O7 Cu2 N6 96.19(7) . . ? N5 Cu2 N6 79.68(7) . . ? O7 Cu2 N4 100.00(7) . . ? N5 Cu2 N4 79.94(7) . . ? N6 Cu2 N4 158.93(7) . . ? O7 Cu2 O8 105.86(6) . . ? N5 Cu2 O8 99.17(7) . . ? N6 Cu2 O8 100.93(7) . . ? N4 Cu2 O8 87.57(6) . . ? O3 V1 O4 108.60(8) . . ? O3 V1 O5 111.61(8) . . ? O4 V1 O5 109.19(8) . . ? O3 V1 O2 108.21(7) . . ? O4 V1 O2 108.86(7) . . ? O5 V1 O2 110.30(7) . . ? O14 P1 O1 112.86(9) . . ? O14 P1 O2 107.29(8) . . ? O1 P1 O2 109.97(9) . . ? O14 P1 C13 109.89(9) . . ? O1 P1 C13 109.48(9) . . ? O2 P1 C13 107.17(9) . . ? O6 P2 O7 115.24(9) . . ? O6 P2 O5 111.42(9) . . ? O7 P2 O5 108.91(9) . . ? O6 P2 C14 108.07(9) . . ? O7 P2 C14 108.02(9) . . ? O5 P2 C14 104.57(9) . . ? O8 P3 O10 112.74(9) . . ? O8 P3 O9 111.88(9) . . ? O10 P3 O9 106.27(9) . . ? O8 P3 C34 111.36(10) . . ? O10 P3 C34 108.50(9) . . ? O9 P3 C34 105.71(9) . . ? O12 P4 O13 113.90(9) . . ? O12 P4 O11 112.96(9) . . ? O13 P4 O11 106.32(10) . . ? O12 P4 C36 110.64(10) . . ? O13 P4 C36 108.23(10) . . ? O11 P4 C36 104.21(10) . . ? P1 O1 Cu1 144.59(10) . . ? P1 O2 V1 140.30(10) . . ? P2 O5 V1 140.80(10) . . ? P2 O7 Cu2 120.91(9) . . ? P3 O8 Cu2 150.58(10) . . ? C1 N1 C5 118.10(18) . . ? C1 N1 Cu1 128.33(14) . . ? C5 N1 Cu1 113.45(13) . . ? C6 N2 C7 121.67(18) . . ? C6 N2 Cu1 119.11(14) . . ? C7 N2 Cu1 118.93(14) . . ? C12 N3 C8 119.04(19) . . ? C12 N3 Cu1 126.03(15) . . ? C8 N3 Cu1 113.93(14) . . ? C33 N4 C29 119.27(18) . . ? C33 N4 Cu2 125.80(14) . . ? C29 N4 Cu2 113.79(13) . . ? C21 N5 C28 122.04(18) . . ? C21 N5 Cu2 118.78(14) . . ? C28 N5 Cu2 118.34(14) . . ? C16 N6 C20 118.87(18) . . ? C16 N6 Cu2 126.45(14) . . ? C20 N6 Cu2 114.56(13) . . ? N1 C1 C2 122.6(2) . . ? C3 C2 C1 119.0(2) . . ? C2 C3 C4 119.2(2) . . ? C5 C4 C3 118.6(2) . . ? N1 C5 C4 122.38(19) . . ? N1 C5 C6 113.35(18) . . ? C4 C5 C6 124.05(19) . . ? N2 C6 C25 120.61(19) . 2_576 ? N2 C6 C5 113.39(18) . . ? C25 C6 C5 125.53(18) 2_576 . ? N2 C7 C26 120.80(19) . 2_576 ? N2 C7 C8 112.57(17) . . ? C26 C7 C8 126.57(18) 2_576 . ? N3 C8 C9 122.15(19) . . ? N3 C8 C7 114.02(18) . . ? C9 C8 C7 123.82(19) . . ? C8 C9 C10 118.36(19) . . ? C11 C10 C9 119.5(2) . . ? C10 C11 C12 118.8(2) . . ? N3 C12 C11 122.1(2) . . ? C15 C13 P1 116.19(14) 2_665 . ? C15 C14 P2 118.77(14) . . ? C14 C15 C13 109.15(16) . 2_665 ? N6 C16 C17 122.34(19) . . ? C16 C17 C18 118.82(19) . . ? C17 C18 C19 119.37(19) . . ? C20 C19 C18 118.55(19) . . ? N6 C20 C19 122.04(18) . . ? N6 C20 C21 113.67(17) . . ? C19 C20 C21 124.29(18) . . ? N5 C21 C22 120.86(18) . . ? N5 C21 C20 112.67(17) . . ? C22 C21 C20 126.45(18) . . ? C21 C22 C23 118.26(19) . . ? C27 C23 C22 119.85(18) . . ? C27 C23 C24 120.59(18) . . ? C22 C23 C24 119.53(18) . . ? C25 C24 C26 119.58(18) . . ? C25 C24 C23 119.53(18) . . ? C26 C24 C23 120.79(18) . . ? C6 C25 C24 118.81(19) 2_576 . ? C7 C26 C24 118.41(19) 2_576 . ? C28 C27 C23 118.40(18) . . ? N5 C28 C27 120.57(18) . . ? N5 C28 C29 112.80(17) . . ? C27 C28 C29 126.59(18) . . ? N4 C29 C30 121.82(18) . . ? N4 C29 C28 113.73(17) . . ? C30 C29 C28 124.45(18) . . ? C29 C30 C31 118.85(19) . . ? C32 C31 C30 118.95(19) . . ? C31 C32 C33 119.3(2) . . ? N4 C33 C32 121.79(19) . . ? C35 C34 P3 115.25(14) . . ? C34 C35 C36 110.06(17) . . ? C35 C36 P4 115.60(15) . . ? _diffrn_measured_fraction_theta_max 0.979 _diffrn_reflns_theta_full 31.50 _diffrn_measured_fraction_theta_full 0.979 _refine_diff_density_max 0.955 _refine_diff_density_min -0.505 _refine_diff_density_rms 0.107 data_Compound_5 _database_code_depnum_ccdc_archive 'CCDC 229554' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C17 H17 Cu N3 O8 P V' _chemical_formula_weight 536.79 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' 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' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.7232(6) _cell_length_b 10.6767(6) _cell_length_c 10.9724(6) _cell_angle_alpha 87.833(1) _cell_angle_beta 65.826(1) _cell_angle_gamma 81.890(1) _cell_volume 1028.53(10) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 13161 _cell_measurement_theta_min 1.93 _cell_measurement_theta_max 31.51 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.48 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.733 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 542 _exptl_absorpt_coefficient_mu 1.617 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5108 _exptl_absorpt_correction_T_max 0.8296 _exptl_absorpt_process_details 'SADABS SHELXL-97 (SHELDRICK, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 90(2) _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_probe x-ray _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'APEX CCD area detector' _diffrn_measurement_method 'Phi and omega scans' _diffrn_detector_area_resol_mean 512 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.001 _diffrn_reflns_number 13161 _diffrn_reflns_av_R_equivalents 0.0231 _diffrn_reflns_av_sigmaI/netI 0.0374 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.93 _diffrn_reflns_theta_max 31.51 _reflns_number_total 6664 _reflns_number_gt 5740 _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 and CrystalMaker 5.x' _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^)+(0.0593P)^2^+0.5485P] 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 6664 _refine_ls_number_parameters 281 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0437 _refine_ls_R_factor_gt 0.0364 _refine_ls_wR_factor_ref 0.1051 _refine_ls_wR_factor_gt 0.1008 _refine_ls_goodness_of_fit_ref 1.054 _refine_ls_restrained_S_all 1.054 _refine_ls_shift/su_max 0.046 _refine_ls_shift/su_mean 0.001 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 0.32370(2) 0.07040(2) 0.22089(2) 0.01258(7) Uani 1 1 d . . . V1 V 0.44433(4) 0.29094(3) -0.35685(3) 0.01511(8) Uani 1 1 d . . . P1 P 0.45682(5) 0.20004(4) -0.08471(5) 0.01320(9) Uani 1 1 d . . . O1 O 0.33064(16) 0.17493(13) 0.04629(14) 0.0177(3) Uani 1 1 d . . . O2 O 0.58128(17) 0.09156(13) -0.14769(17) 0.0243(3) Uani 1 1 d . . . O3 O 0.37870(16) 0.24553(14) -0.18188(14) 0.0199(3) Uani 1 1 d . . . O4 O 0.47596(17) 0.16032(14) -0.45914(14) 0.0202(3) Uani 1 1 d . . . H4' H 0.4550 0.0977 -0.4132 0.030 Uiso 1 1 calc R . . O5 O 0.30858(18) 0.40239(16) -0.36850(16) 0.0253(3) Uani 1 1 d . . . O6 O 0.60273(16) 0.35015(14) -0.40057(15) 0.0206(3) Uani 1 1 d . . . O90 O 0.93860(18) 0.66408(17) 0.92204(18) 0.0309(4) Uani 1 1 d . . . O91 O 0.9916(2) 0.59258(18) 0.1578(2) 0.0364(4) Uani 1 1 d . . . N1 N 0.10794(18) 0.02429(15) 0.28654(16) 0.0152(3) Uani 1 1 d . . . N2 N 0.20854(17) 0.21550(14) 0.33604(15) 0.0132(3) Uani 1 1 d . . . N3 N 0.49709(17) 0.15439(15) 0.22661(16) 0.0143(3) Uani 1 1 d . . . C1 C 0.0683(2) -0.08430(18) 0.2618(2) 0.0190(4) Uani 1 1 d . . . H1 H 0.1435 -0.1457 0.2064 0.023 Uiso 1 1 calc R . . C2 C -0.0824(2) -0.10771(19) 0.3168(2) 0.0216(4) Uani 1 1 d . . . H2 H -0.1072 -0.1838 0.2986 0.026 Uiso 1 1 calc R . . C3 C -0.1948(2) -0.01629(19) 0.3988(2) 0.0203(4) Uani 1 1 d . . . H3 H -0.2961 -0.0300 0.4362 0.024 Uiso 1 1 calc R . . C4 C -0.1541(2) 0.09641(18) 0.4245(2) 0.0176(3) Uani 1 1 d . . . H4 H -0.2276 0.1589 0.4798 0.021 Uiso 1 1 calc R . . C5 C -0.0020(2) 0.11403(17) 0.36616(19) 0.0150(3) Uani 1 1 d . . . C6 C 0.0560(2) 0.22873(17) 0.38773(18) 0.0141(3) Uani 1 1 d . . . C7 C -0.0303(2) 0.34030(18) 0.45327(19) 0.0163(3) Uani 1 1 d . . . H7 H -0.1360 0.3493 0.4884 0.020 Uiso 1 1 calc R . . C8 C 0.0445(2) 0.43937(17) 0.46576(18) 0.0139(3) Uani 1 1 d . . . C9 C 0.2040(2) 0.42094(17) 0.41251(18) 0.0139(3) Uani 1 1 d . . . H9 H 0.2565 0.4846 0.4199 0.017 Uiso 1 1 calc R . . C10 C 0.2829(2) 0.30646(17) 0.34849(18) 0.0132(3) Uani 1 1 d . . . C11 C 0.4507(2) 0.27089(17) 0.28646(18) 0.0138(3) Uani 1 1 d . . . C12 C 0.5532(2) 0.34819(18) 0.28897(19) 0.0165(3) Uani 1 1 d . . . H12 H 0.5188 0.4270 0.3320 0.020 Uiso 1 1 calc R . . C13 C 0.7081(2) 0.30532(19) 0.2259(2) 0.0191(4) Uani 1 1 d . . . H13 H 0.7791 0.3555 0.2254 0.023 Uiso 1 1 calc R . . C14 C 0.7554(2) 0.18647(19) 0.1636(2) 0.0202(4) Uani 1 1 d . . . H14 H 0.8585 0.1560 0.1209 0.024 Uiso 1 1 calc R . . C15 C 0.6465(2) 0.11395(19) 0.1661(2) 0.0188(4) Uani 1 1 d . . . H15 H 0.6784 0.0345 0.1243 0.023 Uiso 1 1 calc R . . C16 C 0.5532(2) 0.32738(17) -0.07017(19) 0.0156(3) Uani 1 1 d . . . H16A H 0.6122 0.2979 -0.0191 0.019 Uiso 1 1 calc R . . H16B H 0.6245 0.3461 -0.1590 0.019 Uiso 1 1 calc R . . C17 C 0.4525(2) 0.45036(17) -0.00497(19) 0.0162(3) Uani 1 1 d . . . H17A H 0.3797 0.4334 0.0838 0.019 Uiso 1 1 calc R . . H17B H 0.3960 0.4834 -0.0572 0.019 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 Cu1 0.01119(11) 0.00896(10) 0.01632(11) -0.00462(8) -0.00390(8) -0.00148(7) V1 0.01398(15) 0.01615(15) 0.01582(14) -0.00176(11) -0.00531(11) -0.00594(11) P1 0.0130(2) 0.00890(19) 0.0168(2) -0.00362(15) -0.00487(16) -0.00140(15) O1 0.0169(6) 0.0169(6) 0.0185(6) -0.0007(5) -0.0058(5) -0.0035(5) O2 0.0170(7) 0.0103(6) 0.0400(9) -0.0108(6) -0.0059(6) 0.0009(5) O3 0.0187(7) 0.0250(7) 0.0180(6) 0.0018(5) -0.0082(5) -0.0074(5) O4 0.0201(7) 0.0198(7) 0.0198(6) -0.0059(5) -0.0039(5) -0.0112(5) O5 0.0257(8) 0.0279(8) 0.0220(7) 0.0026(6) -0.0106(6) -0.0012(6) O6 0.0174(7) 0.0183(6) 0.0246(7) -0.0043(5) -0.0047(5) -0.0080(5) O90 0.0163(7) 0.0323(9) 0.0363(9) -0.0045(7) -0.0039(6) 0.0013(6) O91 0.0304(9) 0.0299(9) 0.0454(11) -0.0077(8) -0.0124(8) -0.0010(7) N1 0.0150(7) 0.0115(7) 0.0181(7) -0.0045(5) -0.0052(6) -0.0024(5) N2 0.0116(6) 0.0108(6) 0.0161(7) -0.0046(5) -0.0039(5) -0.0019(5) N3 0.0129(7) 0.0116(6) 0.0186(7) -0.0038(5) -0.0063(6) -0.0015(5) C1 0.0182(9) 0.0130(8) 0.0241(9) -0.0067(7) -0.0061(7) -0.0033(7) C2 0.0203(9) 0.0143(8) 0.0311(10) -0.0053(7) -0.0095(8) -0.0069(7) C3 0.0161(8) 0.0166(8) 0.0286(10) -0.0031(7) -0.0077(7) -0.0074(7) C4 0.0135(8) 0.0147(8) 0.0230(9) -0.0050(7) -0.0051(7) -0.0030(6) C5 0.0151(8) 0.0111(7) 0.0188(8) -0.0043(6) -0.0059(6) -0.0034(6) C6 0.0127(7) 0.0118(7) 0.0167(8) -0.0041(6) -0.0038(6) -0.0039(6) C7 0.0124(8) 0.0140(8) 0.0204(8) -0.0060(6) -0.0036(6) -0.0033(6) C8 0.0127(7) 0.0127(7) 0.0156(7) -0.0037(6) -0.0043(6) -0.0035(6) C9 0.0128(7) 0.0124(7) 0.0165(8) -0.0034(6) -0.0049(6) -0.0038(6) C10 0.0123(7) 0.0126(7) 0.0148(7) -0.0023(6) -0.0047(6) -0.0030(6) C11 0.0131(8) 0.0120(7) 0.0161(8) -0.0035(6) -0.0054(6) -0.0018(6) C12 0.0140(8) 0.0143(8) 0.0207(8) -0.0033(6) -0.0058(7) -0.0026(6) C13 0.0145(8) 0.0172(8) 0.0264(9) -0.0028(7) -0.0086(7) -0.0036(7) C14 0.0118(8) 0.0189(9) 0.0289(10) -0.0041(7) -0.0073(7) -0.0006(7) C15 0.0145(8) 0.0161(8) 0.0248(9) -0.0055(7) -0.0073(7) 0.0000(7) C16 0.0166(8) 0.0099(7) 0.0199(8) -0.0038(6) -0.0066(7) -0.0026(6) C17 0.0177(8) 0.0097(7) 0.0202(8) -0.0033(6) -0.0063(7) -0.0024(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 Cu1 O2 1.8803(14) 2_655 ? Cu1 N2 1.9365(15) . ? Cu1 N3 2.0416(15) . ? Cu1 N1 2.0467(16) . ? Cu1 O1 2.1620(14) . ? V1 O6 1.6274(14) . ? V1 O5 1.6906(16) . ? V1 O4 1.7360(14) . ? V1 O3 1.8280(15) . ? P1 O1 1.5042(15) . ? P1 O2 1.5045(15) . ? P1 O3 1.5714(15) . ? P1 C16 1.8032(18) . ? O2 Cu1 1.8803(14) 2_655 ? N1 C1 1.343(2) . ? N1 C5 1.354(2) . ? N2 C10 1.332(2) . ? N2 C6 1.341(2) . ? N3 C15 1.339(2) . ? N3 C11 1.357(2) . ? C1 C2 1.393(3) . ? C2 C3 1.384(3) . ? C3 C4 1.391(3) . ? C4 C5 1.388(3) . ? C5 C6 1.483(2) . ? C6 C7 1.389(2) . ? C7 C8 1.406(2) . ? C8 C9 1.402(2) . ? C8 C8 1.488(4) 2_566 ? C9 C10 1.391(2) . ? C10 C11 1.485(2) . ? C11 C12 1.390(2) . ? C12 C13 1.390(3) . ? C13 C14 1.390(3) . ? C14 C15 1.388(3) . ? C16 C17 1.526(3) . ? C17 C17 1.536(4) 2_665 ? 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 Cu1 N2 166.23(7) 2_655 . ? O2 Cu1 N3 103.56(6) 2_655 . ? N2 Cu1 N3 79.83(6) . . ? O2 Cu1 N1 94.29(6) 2_655 . ? N2 Cu1 N1 79.55(6) . . ? N3 Cu1 N1 157.09(6) . . ? O2 Cu1 O1 102.15(7) 2_655 . ? N2 Cu1 O1 91.02(6) . . ? N3 Cu1 O1 91.49(6) . . ? N1 Cu1 O1 98.76(6) . . ? O6 V1 O5 109.63(8) . . ? O6 V1 O4 108.89(7) . . ? O5 V1 O4 111.25(8) . . ? O6 V1 O3 109.27(7) . . ? O5 V1 O3 107.18(7) . . ? O4 V1 O3 110.59(7) . . ? O1 P1 O2 116.48(9) . . ? O1 P1 O3 106.22(8) . . ? O2 P1 O3 110.22(9) . . ? O1 P1 C16 111.91(8) . . ? O2 P1 C16 104.96(8) . . ? O3 P1 C16 106.70(9) . . ? P1 O1 Cu1 133.76(9) . . ? P1 O2 Cu1 159.55(10) . 2_655 ? P1 O3 V1 135.62(9) . . ? C1 N1 C5 118.94(16) . . ? C1 N1 Cu1 126.84(13) . . ? C5 N1 Cu1 114.19(12) . . ? C10 N2 C6 121.73(15) . . ? C10 N2 Cu1 118.70(12) . . ? C6 N2 Cu1 119.07(12) . . ? C15 N3 C11 118.78(16) . . ? C15 N3 Cu1 127.32(13) . . ? C11 N3 Cu1 113.41(12) . . ? N1 C1 C2 121.90(18) . . ? C3 C2 C1 119.18(17) . . ? C2 C3 C4 119.08(18) . . ? C5 C4 C3 118.87(17) . . ? N1 C5 C4 122.02(16) . . ? N1 C5 C6 113.95(15) . . ? C4 C5 C6 124.01(16) . . ? N2 C6 C7 120.76(16) . . ? N2 C6 C5 112.45(15) . . ? C7 C6 C5 126.79(16) . . ? C6 C7 C8 119.02(16) . . ? C9 C8 C7 118.47(16) . . ? C9 C8 C8 121.11(19) . 2_566 ? C7 C8 C8 120.4(2) . 2_566 ? C10 C9 C8 119.27(16) . . ? N2 C10 C9 120.71(16) . . ? N2 C10 C11 112.76(15) . . ? C9 C10 C11 126.53(16) . . ? N3 C11 C12 122.07(17) . . ? N3 C11 C10 114.08(15) . . ? C12 C11 C10 123.84(16) . . ? C11 C12 C13 118.70(17) . . ? C14 C13 C12 119.11(18) . . ? C15 C14 C13 119.02(18) . . ? N3 C15 C14 122.30(18) . . ? C17 C16 P1 116.35(13) . . ? C16 C17 C17 111.26(19) . 2_665 ? _diffrn_measured_fraction_theta_max 0.971 _diffrn_reflns_theta_full 31.51 _diffrn_measured_fraction_theta_full 0.971 _refine_diff_density_max 0.852 _refine_diff_density_min -0.877 _refine_diff_density_rms 0.108 data_Compound_6 _database_code_depnum_ccdc_archive 'CCDC 229555' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C25 H37.30 Cu N3 O17.65 P4 V2' _chemical_formula_weight 951.58 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.5197(5) _cell_length_b 12.5297(6) _cell_length_c 13.9836(6) _cell_angle_alpha 101.338(1) _cell_angle_beta 91.457(1) _cell_angle_gamma 94.363(1) _cell_volume 1800.41(14) _cell_formula_units_Z 2 _cell_measurement_temperature 90(2) _cell_measurement_reflns_used 23632 _cell_measurement_theta_min 1.49 _cell_measurement_theta_max 31.51 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.755 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 969 _exptl_absorpt_coefficient_mu 1.351 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7288 _exptl_absorpt_correction_T_max 0.8767 _exptl_absorpt_process_details 'SADABS SHELXL-97 (SHELDRICK, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 90(2) _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_probe x-ray _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'APEX CCD area detector' _diffrn_measurement_method 'Phi and omega scans' _diffrn_detector_area_resol_mean 512 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.001 _diffrn_reflns_number 23632 _diffrn_reflns_av_R_equivalents 0.0446 _diffrn_reflns_av_sigmaI/netI 0.0796 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.49 _diffrn_reflns_theta_max 31.51 _reflns_number_total 11776 _reflns_number_gt 8294 _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 and CrystalMaker 5.x' _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^)+(0.0711P)^2^+1.1179P] 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 11776 _refine_ls_number_parameters 524 _refine_ls_number_restraints 8 _refine_ls_R_factor_all 0.0917 _refine_ls_R_factor_gt 0.0606 _refine_ls_wR_factor_ref 0.1578 _refine_ls_wR_factor_gt 0.1390 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_restrained_S_all 1.046 _refine_ls_shift/su_max 0.023 _refine_ls_shift/su_mean 0.001 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 0.15783(4) 0.59713(3) -0.00323(3) 0.01454(10) Uani 1 1 d . . . V1 V 0.56347(6) 0.42415(4) 0.14048(4) 0.01273(12) Uani 1 1 d . . . V2 V 0.40325(7) 0.31012(5) 0.45339(5) 0.02328(15) Uani 1 1 d . . . P1 P 0.31981(9) 0.40046(7) -0.02629(6) 0.01355(17) Uani 1 1 d . . . P2 P 0.61742(10) 0.47174(8) 0.37907(7) 0.0201(2) Uani 1 1 d . . . P3 P 0.43716(9) 0.20440(7) 0.21695(6) 0.01327(17) Uani 1 1 d . . . P4 P 0.15895(10) 0.13029(8) 0.40107(8) 0.0216(2) Uani 1 1 d . . . O1 O 0.1948(2) 0.45207(19) 0.00084(18) 0.0167(5) Uani 1 1 d . . . O2 O 0.4186(2) 0.43606(19) 0.05746(17) 0.0170(5) Uani 1 1 d . . . O3 O 0.6307(2) 0.57143(18) 0.12151(17) 0.0156(5) Uani 1 1 d . . . O4 O 0.6181(3) 0.4855(2) 0.27376(18) 0.0229(6) Uani 1 1 d . . . O5 O 0.4523(2) 0.31389(18) 0.18814(17) 0.0166(5) Uani 1 1 d . . . O6 O 0.4864(3) 0.4296(2) 0.40537(19) 0.0252(6) Uani 1 1 d . . . O7 O 0.3054(2) 0.1449(2) 0.17443(18) 0.0195(5) Uani 1 1 d . . . O8 O 0.4432(2) 0.20987(19) 0.32659(17) 0.0174(5) Uani 1 1 d . . . O9 O 0.3324(3) 0.4209(2) 0.5555(2) 0.0334(7) Uani 1 1 d . . . O10 O 0.4902(3) 0.2547(3) 0.5209(2) 0.0373(8) Uani 1 1 d . . . O11 O 0.2302(3) 0.2418(2) 0.4383(2) 0.0315(7) Uani 1 1 d . . . O12 O 0.2267(3) 0.0398(2) 0.4417(2) 0.0250(6) Uani 1 1 d . . . O13 O 0.1463(3) 0.0972(2) 0.2920(2) 0.0232(6) Uani 1 1 d . . . O14 O 0.6672(2) 0.35051(19) 0.08384(18) 0.0172(5) Uani 1 1 d . . . O90 O 0.2660(4) 0.0740(3) 0.6279(2) 0.0464(9) Uani 1 1 d . . . O91 O 0.5169(5) 0.0282(3) 0.4083(3) 0.0748(15) Uani 1 1 d . . . O92 O 0.7434(3) 0.7081(2) 0.3002(2) 0.0358(7) Uani 1 1 d . . . O93 O 0.9678(9) 0.7885(8) 0.2594(7) 0.051(2) Uani 0.40 1 d P . . O94 O 0.9031(12) 0.9983(11) 0.2400(9) 0.037(3) Uani 0.25 1 d P . . N1 N 0.0523(3) 0.5669(2) -0.1299(2) 0.0181(6) Uani 1 1 d . . . N2 N 0.0901(3) 0.7373(2) 0.0030(2) 0.0141(5) Uani 1 1 d . . . N3 N 0.2314(4) 0.6764(3) 0.1279(2) 0.0265(7) Uani 1 1 d . . . C1 C 0.0363(4) 0.4721(3) -0.1945(3) 0.0294(9) Uani 1 1 d . . . H1 H 0.0777 0.4113 -0.1817 0.035 Uiso 1 1 calc R . . C2 C -0.0381(6) 0.4601(4) -0.2789(4) 0.062(2) Uani 1 1 d . . . H2 H -0.0462 0.3926 -0.3244 0.075 Uiso 1 1 calc R . . C3 C -0.1006(7) 0.5473(4) -0.2964(5) 0.073(2) Uani 1 1 d . . . H3 H -0.1549 0.5397 -0.3531 0.087 Uiso 1 1 calc R . . C4 C -0.0841(5) 0.6459(3) -0.2311(4) 0.0394(12) Uani 1 1 d . . . H4 H -0.1254 0.7073 -0.2427 0.047 Uiso 1 1 calc R . . C5 C -0.0062(3) 0.6534(3) -0.1486(3) 0.0190(7) Uani 1 1 d . . . C6 C 0.0214(3) 0.7543(3) -0.0733(2) 0.0135(6) Uani 1 1 d . . . C7 C -0.0143(3) 0.8579(3) -0.0773(3) 0.0160(6) Uani 1 1 d . . . H7 H -0.0608 0.8699 -0.1328 0.019 Uiso 1 1 calc R . . C8 C 0.0189(3) 0.9442(3) 0.0010(3) 0.0160(6) Uani 1 1 d . . . C9 C 0.0878(4) 0.9221(3) 0.0803(3) 0.0256(9) Uani 1 1 d . . . H9 H 0.1096 0.9786 0.1356 0.031 Uiso 1 1 calc R . . C10 C 0.1244(4) 0.8181(3) 0.0784(3) 0.0206(7) Uani 1 1 d . . . C11 C 0.2046(5) 0.7822(3) 0.1539(3) 0.0290(9) Uani 1 1 d . . . C12 C 0.2480(6) 0.8470(4) 0.2409(3) 0.0440(14) Uani 1 1 d . . . H12 H 0.2257 0.9202 0.2581 0.053 Uiso 1 1 calc R . . C13 C 0.3254(6) 0.8038(4) 0.3037(3) 0.0550(17) Uani 1 1 d . . . H13 H 0.3581 0.8476 0.3638 0.066 Uiso 1 1 calc R . . C14 C 0.3539(6) 0.6965(4) 0.2772(3) 0.0501(16) Uani 1 1 d . . . H14 H 0.4069 0.6655 0.3186 0.060 Uiso 1 1 calc R . . C15 C 0.3040(5) 0.6351(4) 0.1896(3) 0.0393(12) Uani 1 1 d . . . H15 H 0.3218 0.5607 0.1722 0.047 Uiso 1 1 calc R . . C16 C 0.2850(3) 0.2554(3) -0.0478(3) 0.0165(6) Uani 1 1 d . . . H16A H 0.2621 0.2342 0.0145 0.020 Uiso 1 1 calc R . . H16B H 0.2099 0.2352 -0.0936 0.020 Uiso 1 1 calc R . . C17 C 0.5573(4) 0.1214(3) 0.1599(3) 0.0194(7) Uani 1 1 d . . . H17A H 0.5703 0.1376 0.0942 0.023 Uiso 1 1 calc R . . H17B H 0.6386 0.1430 0.1985 0.023 Uiso 1 1 calc R . . C18 C 0.5276(4) -0.0017(3) 0.1493(3) 0.0205(7) Uani 1 1 d . . . H18A H 0.4484 -0.0247 0.1083 0.025 Uiso 1 1 calc R . . H18B H 0.5123 -0.0186 0.2146 0.025 Uiso 1 1 calc R . . C19 C 0.6356(4) -0.0672(3) 0.1035(3) 0.0226(8) Uani 1 1 d . . . H19A H 0.6529 -0.0486 0.0392 0.027 Uiso 1 1 calc R . . H19B H 0.7141 -0.0461 0.1456 0.027 Uiso 1 1 calc R . . C20 C 0.6038(4) -0.1901(3) 0.0900(3) 0.0201(7) Uani 1 1 d . . . H20A H 0.5275 -0.2118 0.0455 0.024 Uiso 1 1 calc R . . H20B H 0.5830 -0.2085 0.1538 0.024 Uiso 1 1 calc R . . C22A C -0.0526(8) 0.2405(6) 0.4443(6) 0.0319(19) Uani 0.580(7) 1 d PD . 1 H22A H 0.0085 0.3034 0.4730 0.038 Uiso 0.580(7) 1 calc PR . 1 H22B H -0.0672 0.2422 0.3744 0.038 Uiso 0.580(7) 1 calc PR . 1 C23A C -0.1758(7) 0.2523(6) 0.4944(5) 0.0290(17) Uani 0.580(7) 1 d PD . 1 H23A H -0.1623 0.2490 0.5640 0.035 Uiso 0.580(7) 1 calc PR . 1 H23B H -0.2384 0.1912 0.4643 0.035 Uiso 0.580(7) 1 calc PR . 1 C24A C -0.2282(7) 0.3601(5) 0.4866(5) 0.0242(15) Uani 0.580(7) 1 d PD . 1 H24A H -0.3052 0.3692 0.5257 0.029 Uiso 0.580(7) 1 calc PR . 1 H24B H -0.1638 0.4207 0.5145 0.029 Uiso 0.580(7) 1 calc PR . 1 C25A C -0.2624(10) 0.3673(9) 0.3821(6) 0.0221(19) Uani 0.580(7) 1 d PD . 1 H25A H -0.2986 0.2949 0.3459 0.026 Uiso 0.580(7) 1 calc PR . 1 H25B H -0.1844 0.3882 0.3496 0.026 Uiso 0.580(7) 1 calc PR . 1 C22B C -0.0851(11) 0.1993(8) 0.3999(9) 0.051(4) Uani 0.420(7) 1 d PD . 2 H22C H -0.0696 0.1834 0.3291 0.061 Uiso 0.420(7) 1 calc PR . 2 H22D H -0.1745 0.1732 0.4084 0.061 Uiso 0.420(7) 1 calc PR . 2 C23B C -0.0674(14) 0.3231(8) 0.4377(9) 0.056(4) Uani 0.420(7) 1 d PD . 2 H23C H -0.0808 0.3363 0.5087 0.068 Uiso 0.420(7) 1 calc PR . 2 H23D H 0.0230 0.3465 0.4297 0.068 Uiso 0.420(7) 1 calc PR . 2 C24B C -0.1487(11) 0.3997(12) 0.3946(10) 0.063(4) Uani 0.420(7) 1 d PD . 2 H24C H -0.1211 0.4764 0.4254 0.075 Uiso 0.420(7) 1 calc PR . 2 H24D H -0.1353 0.3905 0.3237 0.075 Uiso 0.420(7) 1 calc PR . 2 C25B C -0.2899(12) 0.3768(16) 0.4107(13) 0.038(4) Uani 0.420(7) 1 d PD . 2 H25C H -0.3010 0.3746 0.4804 0.045 Uiso 0.420(7) 1 calc PR . 2 H25D H -0.3198 0.3039 0.3718 0.045 Uiso 0.420(7) 1 calc PR . 2 C21 C 0.0055(4) 0.1355(4) 0.4528(4) 0.0410(12) Uani 1 1 d D . . H21A H -0.0516 0.0723 0.4186 0.049 Uiso 1 1 calc R . 1 H21B H 0.0137 0.1306 0.5224 0.049 Uiso 1 1 calc R . 1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0236(2) 0.00957(18) 0.01123(19) 0.00129(14) 0.00164(16) 0.00805(15) V1 0.0215(3) 0.0074(2) 0.0101(2) 0.00201(19) 0.0028(2) 0.0046(2) V2 0.0359(4) 0.0175(3) 0.0140(3) 0.0006(2) 0.0026(3) -0.0075(3) P1 0.0219(4) 0.0067(3) 0.0129(4) 0.0024(3) 0.0027(3) 0.0051(3) P2 0.0313(5) 0.0162(4) 0.0115(4) 0.0019(3) -0.0002(4) -0.0040(4) P3 0.0208(4) 0.0075(3) 0.0120(4) 0.0022(3) 0.0014(3) 0.0033(3) P4 0.0230(5) 0.0142(4) 0.0255(5) -0.0003(4) 0.0071(4) -0.0016(3) O1 0.0251(13) 0.0110(11) 0.0159(11) 0.0041(9) 0.0045(10) 0.0077(9) O2 0.0263(13) 0.0115(11) 0.0145(11) 0.0041(9) 0.0008(10) 0.0061(9) O3 0.0256(13) 0.0091(10) 0.0129(11) 0.0031(9) 0.0034(9) 0.0036(9) O4 0.0338(15) 0.0217(13) 0.0120(12) 0.0035(10) 0.0000(10) -0.0055(11) O5 0.0274(13) 0.0091(10) 0.0142(11) 0.0038(9) 0.0028(10) 0.0019(9) O6 0.0398(16) 0.0157(12) 0.0174(13) -0.0006(10) 0.0082(11) -0.0075(11) O7 0.0250(13) 0.0140(12) 0.0183(12) 0.0008(9) -0.0042(10) 0.0022(10) O8 0.0271(13) 0.0138(11) 0.0107(11) 0.0020(9) 0.0008(9) -0.0007(10) O9 0.0525(19) 0.0232(14) 0.0183(14) -0.0050(11) 0.0104(13) -0.0148(13) O10 0.056(2) 0.0345(17) 0.0216(15) 0.0090(13) -0.0056(14) -0.0004(15) O11 0.0424(18) 0.0191(13) 0.0280(15) -0.0048(11) 0.0158(13) -0.0092(12) O12 0.0267(14) 0.0236(14) 0.0238(14) 0.0027(11) 0.0009(11) 0.0029(11) O13 0.0235(13) 0.0193(13) 0.0259(14) 0.0039(11) -0.0013(11) -0.0014(10) O14 0.0230(13) 0.0108(11) 0.0189(12) 0.0036(9) 0.0057(10) 0.0049(9) O90 0.091(3) 0.0233(16) 0.0229(16) 0.0019(13) 0.0077(17) -0.0017(17) O91 0.116(4) 0.037(2) 0.071(3) 0.009(2) -0.043(3) 0.026(2) O92 0.063(2) 0.0205(14) 0.0230(15) 0.0023(12) 0.0088(14) -0.0030(14) O93 0.044(5) 0.045(5) 0.059(6) 0.003(5) 0.014(5) -0.004(4) O94 0.042(7) 0.049(8) 0.019(6) 0.007(5) 0.005(5) -0.006(6) N1 0.0240(15) 0.0099(13) 0.0192(15) -0.0009(11) -0.0023(12) 0.0052(11) N2 0.0190(14) 0.0112(12) 0.0126(13) 0.0016(10) 0.0010(10) 0.0054(10) N3 0.048(2) 0.0181(15) 0.0128(14) -0.0033(12) -0.0040(14) 0.0176(14) C1 0.039(2) 0.0122(16) 0.034(2) -0.0018(15) -0.0130(18) 0.0072(15) C2 0.095(5) 0.016(2) 0.063(4) -0.020(2) -0.053(3) 0.019(2) C3 0.109(5) 0.018(2) 0.077(4) -0.019(2) -0.075(4) 0.021(3) C4 0.050(3) 0.0143(18) 0.048(3) -0.0063(18) -0.032(2) 0.0110(18) C5 0.0224(17) 0.0114(15) 0.0213(17) -0.0012(13) -0.0040(14) 0.0024(13) C6 0.0138(15) 0.0088(13) 0.0161(15) -0.0024(11) -0.0006(12) 0.0027(11) C7 0.0188(16) 0.0113(14) 0.0174(16) 0.0009(12) -0.0055(13) 0.0045(12) C8 0.0213(16) 0.0095(14) 0.0173(16) 0.0011(12) -0.0011(13) 0.0061(12) C9 0.046(2) 0.0125(16) 0.0165(17) -0.0032(13) -0.0098(16) 0.0119(16) C10 0.035(2) 0.0160(16) 0.0112(15) -0.0009(12) -0.0048(14) 0.0130(14) C11 0.055(3) 0.0172(18) 0.0151(17) -0.0017(14) -0.0096(17) 0.0202(18) C12 0.085(4) 0.024(2) 0.020(2) -0.0093(16) -0.022(2) 0.028(2) C13 0.103(5) 0.035(3) 0.023(2) -0.0104(19) -0.029(3) 0.040(3) C14 0.087(4) 0.041(3) 0.022(2) -0.0065(19) -0.025(2) 0.040(3) C15 0.071(3) 0.029(2) 0.0187(19) -0.0018(16) -0.013(2) 0.033(2) C16 0.0232(17) 0.0080(14) 0.0190(16) 0.0021(12) 0.0059(13) 0.0056(12) C17 0.0243(18) 0.0108(15) 0.0248(18) 0.0047(13) 0.0105(14) 0.0063(13) C18 0.0282(19) 0.0104(15) 0.0235(18) 0.0029(13) 0.0038(15) 0.0051(13) C19 0.031(2) 0.0118(15) 0.0269(19) 0.0060(14) 0.0084(16) 0.0076(14) C20 0.0268(18) 0.0107(15) 0.0239(18) 0.0034(13) 0.0063(14) 0.0070(13) C22A 0.046(5) 0.018(4) 0.030(4) 0.000(3) 0.011(4) 0.004(3) C23A 0.036(4) 0.030(4) 0.021(3) 0.006(3) 0.003(3) 0.003(3) C24A 0.029(4) 0.022(3) 0.022(3) 0.003(3) -0.005(3) 0.006(3) C25A 0.021(5) 0.020(4) 0.022(4) -0.002(3) 0.005(3) -0.002(3) C22B 0.049(9) 0.035(8) 0.076(11) 0.016(7) 0.032(8) 0.024(6) C23B 0.088(11) 0.041(7) 0.044(7) 0.003(6) 0.005(7) 0.040(7) C24B 0.064(10) 0.073(11) 0.048(9) 0.002(8) -0.006(7) 0.013(8) C25B 0.030(8) 0.046(9) 0.045(10) 0.024(8) 0.007(6) 0.015(6) C21 0.034(2) 0.029(2) 0.067(4) 0.021(2) 0.027(2) 0.0100(18) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 O1 1.899(2) . ? Cu1 N2 1.932(3) . ? Cu1 N3 2.011(3) . ? Cu1 N1 2.021(3) . ? Cu1 O14 2.302(2) 2_665 ? V1 O14 1.606(2) . ? V1 O2 1.925(3) . ? V1 O4 1.926(3) . ? V1 O5 1.969(2) . ? V1 O3 1.995(2) . ? V2 O10 1.587(3) . ? V2 O6 1.919(3) . ? V2 O11 1.941(3) . ? V2 O9 1.988(3) . ? V2 O8 2.035(2) . ? P1 O2 1.521(3) . ? P1 O1 1.533(3) . ? P1 O3 1.536(2) 2_665 ? P1 C16 1.790(3) . ? P2 O4 1.516(3) . ? P2 O6 1.518(3) . ? P2 O9 1.519(3) 2_666 ? P2 C25B 1.709(17) 1_655 ? P2 C25A 1.893(12) 1_655 ? P3 O5 1.502(2) . ? P3 O8 1.521(2) . ? P3 O7 1.568(3) . ? P3 C17 1.800(3) . ? P4 O13 1.500(3) . ? P4 O11 1.523(3) . ? P4 O12 1.572(3) . ? P4 C21 1.786(4) . ? O3 P1 1.536(2) 2_665 ? O9 P2 1.519(3) 2_666 ? O14 Cu1 2.302(2) 2_665 ? N1 C1 1.339(5) . ? N1 C5 1.352(4) . ? N2 C10 1.331(4) . ? N2 C6 1.334(4) . ? N3 C15 1.340(5) . ? N3 C11 1.357(5) . ? C1 C2 1.377(6) . ? C2 C3 1.376(7) . ? C3 C4 1.381(6) . ? C4 C5 1.382(5) . ? C5 C6 1.482(4) . ? C6 C7 1.390(4) . ? C7 C8 1.395(4) . ? C8 C9 1.393(5) . ? C8 C8 1.487(6) 2_575 ? C9 C10 1.382(5) . ? C10 C11 1.493(5) . ? C11 C12 1.368(5) . ? C12 C13 1.395(6) . ? C13 C14 1.380(6) . ? C14 C15 1.380(6) . ? C16 C20 1.541(5) 2_655 ? C17 C18 1.528(5) . ? C18 C19 1.532(5) . ? C19 C20 1.525(5) . ? C20 C16 1.541(5) 2_655 ? C22A C23A 1.493(10) . ? C22A C21 1.516(9) . ? C23A C24A 1.519(9) . ? C24A C25A 1.518(11) . ? C25A P2 1.893(12) 1_455 ? C22B C23B 1.533(5) . ? C22B C21 1.551(5) . ? C23B C24B 1.531(5) . ? C24B C25B 1.523(5) . ? C25B P2 1.709(17) 1_455 ? 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 Cu1 N2 169.16(12) . . ? O1 Cu1 N3 100.54(12) . . ? N2 Cu1 N3 79.83(12) . . ? O1 Cu1 N1 98.92(11) . . ? N2 Cu1 N1 79.87(12) . . ? N3 Cu1 N1 159.55(12) . . ? O1 Cu1 O14 99.31(10) . 2_665 ? N2 Cu1 O14 91.46(10) . 2_665 ? N3 Cu1 O14 93.08(13) . 2_665 ? N1 Cu1 O14 89.91(11) . 2_665 ? O14 V1 O2 112.57(12) . . ? O14 V1 O4 112.09(13) . . ? O2 V1 O4 135.25(12) . . ? O14 V1 O5 101.55(11) . . ? O2 V1 O5 85.29(10) . . ? O4 V1 O5 88.65(11) . . ? O14 V1 O3 100.13(11) . . ? O2 V1 O3 87.73(10) . . ? O4 V1 O3 81.90(10) . . ? O5 V1 O3 158.27(10) . . ? O10 V2 O6 115.38(15) . . ? O10 V2 O11 111.46(16) . . ? O6 V2 O11 133.15(14) . . ? O10 V2 O9 99.36(15) . . ? O6 V2 O9 87.31(12) . . ? O11 V2 O9 84.49(12) . . ? O10 V2 O8 95.06(14) . . ? O6 V2 O8 88.29(11) . . ? O11 V2 O8 88.44(11) . . ? O9 V2 O8 165.44(13) . . ? O2 P1 O1 109.91(14) . . ? O2 P1 O3 111.36(14) . 2_665 ? O1 P1 O3 111.41(14) . 2_665 ? O2 P1 C16 109.82(15) . . ? O1 P1 C16 107.05(15) . . ? O3 P1 C16 107.16(15) 2_665 . ? O4 P2 O6 111.43(16) . . ? O4 P2 O9 108.83(16) . 2_666 ? O6 P2 O9 113.35(16) . 2_666 ? O4 P2 C25B 117.2(6) . 1_655 ? O6 P2 C25B 101.1(5) . 1_655 ? O9 P2 C25B 104.8(7) 2_666 1_655 ? O4 P2 C25A 102.6(3) . 1_655 ? O6 P2 C25A 111.1(3) . 1_655 ? O9 P2 C25A 109.0(3) 2_666 1_655 ? C25B P2 C25A 14.9(5) 1_655 1_655 ? O5 P3 O8 114.15(14) . . ? O5 P3 O7 108.85(14) . . ? O8 P3 O7 108.39(14) . . ? O5 P3 C17 108.86(15) . . ? O8 P3 C17 110.07(16) . . ? O7 P3 C17 106.22(16) . . ? O13 P4 O11 114.41(16) . . ? O13 P4 O12 108.45(15) . . ? O11 P4 O12 110.14(17) . . ? O13 P4 C21 110.7(2) . . ? O11 P4 C21 106.5(2) . . ? O12 P4 C21 106.40(19) . . ? P1 O1 Cu1 126.71(15) . . ? P1 O2 V1 156.95(16) . . ? P1 O3 V1 126.16(14) 2_665 . ? P2 O4 V1 146.55(17) . . ? P3 O5 V1 148.27(17) . . ? P2 O6 V2 140.91(19) . . ? P3 O8 V2 140.43(16) . . ? P2 O9 V2 136.0(2) 2_666 . ? P4 O11 V2 139.7(2) . . ? V1 O14 Cu1 129.20(13) . 2_665 ? C1 N1 C5 118.8(3) . . ? C1 N1 Cu1 126.7(3) . . ? C5 N1 Cu1 114.5(2) . . ? C10 N2 C6 121.3(3) . . ? C10 N2 Cu1 119.3(2) . . ? C6 N2 Cu1 119.0(2) . . ? C15 N3 C11 118.4(3) . . ? C15 N3 Cu1 126.3(3) . . ? C11 N3 Cu1 115.3(3) . . ? N1 C1 C2 122.1(4) . . ? C3 C2 C1 119.0(4) . . ? C2 C3 C4 119.7(4) . . ? C3 C4 C5 118.5(4) . . ? N1 C5 C4 121.8(3) . . ? N1 C5 C6 113.8(3) . . ? C4 C5 C6 124.3(3) . . ? N2 C6 C7 120.7(3) . . ? N2 C6 C5 112.4(3) . . ? C7 C6 C5 126.9(3) . . ? C6 C7 C8 119.4(3) . . ? C9 C8 C7 117.9(3) . . ? C9 C8 C8 121.6(4) . 2_575 ? C7 C8 C8 120.5(4) . 2_575 ? C10 C9 C8 120.0(3) . . ? N2 C10 C9 120.6(3) . . ? N2 C10 C11 112.5(3) . . ? C9 C10 C11 126.9(3) . . ? N3 C11 C12 122.2(4) . . ? N3 C11 C10 112.9(3) . . ? C12 C11 C10 124.9(3) . . ? C11 C12 C13 118.9(4) . . ? C14 C13 C12 119.1(4) . . ? C15 C14 C13 118.8(4) . . ? N3 C15 C14 122.5(4) . . ? C20 C16 P1 113.9(2) 2_655 . ? C18 C17 P3 115.4(3) . . ? C17 C18 C19 112.6(3) . . ? C20 C19 C18 112.4(3) . . ? C19 C20 C16 112.2(3) . 2_655 ? C23A C22A C21 112.6(6) . . ? C22A C23A C24A 110.7(6) . . ? C25A C24A C23A 112.7(6) . . ? C24A C25A P2 110.5(5) . 1_455 ? C23B C22B C21 113.1(8) . . ? C24B C23B C22B 120.7(10) . . ? C25B C24B C23B 111.5(12) . . ? C24B C25B P2 113.3(11) . 1_455 ? C22A C21 C22B 29.4(5) . . ? C22A C21 P4 111.0(4) . . ? C22B C21 P4 112.1(6) . . ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 31.51 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 1.415 _refine_diff_density_min -1.232 _refine_diff_density_rms 0.146 data_Compound_7 _database_code_depnum_ccdc_archive 'CCDC 229556' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H48 Cu2 N6 O18 P4 V2' _chemical_formula_weight 1277.70 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' 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' 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' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.0548(5) _cell_length_b 15.4425(8) _cell_length_c 17.3746(9) _cell_angle_alpha 96.1160(1) _cell_angle_beta 98.6860(1) _cell_angle_gamma 95.3960(1) _cell_volume 2372.9(2) _cell_formula_units_Z 2 _cell_measurement_temperature 95(2) _cell_measurement_reflns_used 15517 _cell_measurement_theta_min 1.33 _cell_measurement_theta_max 31.51 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.788 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1300 _exptl_absorpt_coefficient_mu 1.485 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6813 _exptl_absorpt_correction_T_max 0.8657 _exptl_absorpt_process_details 'SADABS SHELXL-97 (SHELDRICK, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 90(2) _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_probe x-ray _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'APEX CCD area detector' _diffrn_measurement_method 'Phi and omega scans' _diffrn_detector_area_resol_mean 512 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.001 _diffrn_reflns_number 31203 _diffrn_reflns_av_R_equivalents 0.0420 _diffrn_reflns_av_sigmaI/netI 0.0723 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.33 _diffrn_reflns_theta_max 31.51 _reflns_number_total 15517 _reflns_number_gt 11769 _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 and CrystalMaker 5.x' _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^)+(0.0553P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 15517 _refine_ls_number_parameters 669 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0727 _refine_ls_R_factor_gt 0.0497 _refine_ls_wR_factor_ref 0.1237 _refine_ls_wR_factor_gt 0.1102 _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_restrained_S_all 1.049 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.09406(4) 0.63743(2) 0.463401(18) 0.00839(7) Uani 1 1 d . . . Cu2 Cu 0.41692(4) 0.35005(2) 0.997704(19) 0.00948(7) Uani 1 1 d . . . V1 V 0.42749(5) 0.78575(3) 0.43077(3) 0.01075(10) Uani 1 1 d . . . V2 V 0.11908(5) 0.27159(3) 1.11666(3) 0.01013(9) Uani 1 1 d . . . P1 P 0.09773(8) 0.73581(5) 0.31847(4) 0.00914(13) Uani 1 1 d . . . P2 P 0.35567(8) 0.79365(5) 0.57668(4) 0.01052(13) Uani 1 1 d . . . P3 P 0.48185(8) 0.29284(4) 1.16232(4) 0.00892(13) Uani 1 1 d . . . P4 P 0.08465(8) 0.21913(5) 0.96292(4) 0.01040(13) Uani 1 1 d . . . O1 O 0.0131(2) 0.68123(12) 0.36915(11) 0.0109(4) Uani 1 1 d . . . O2 O 0.0606(2) 0.68986(13) 0.23267(11) 0.0153(4) Uani 1 1 d . . . H2' H 0.0176 0.7233 0.2037 0.023 Uiso 1 1 calc R . . O3 O 0.2675(2) 0.74155(13) 0.34248(11) 0.0132(4) Uani 1 1 d . . . O4 O 0.5494(2) 0.71848(15) 0.41357(12) 0.0187(4) Uani 1 1 d . . . O5 O 0.4757(3) 0.87759(14) 0.39828(13) 0.0220(5) Uani 1 1 d . . . O6 O 0.4973(2) 0.83063(13) 0.54587(11) 0.0144(4) Uani 1 1 d . . . O7 O 0.3792(2) 0.73195(13) 0.63660(12) 0.0157(4) Uani 1 1 d . . . O8 O 0.2640(2) 0.75042(12) 0.49568(11) 0.0102(4) Uani 1 1 d . . . O9 O 0.5377(2) 0.32989(13) 1.09279(11) 0.0117(4) Uani 1 1 d . . . O10 O 0.5945(2) 0.33706(13) 1.23636(11) 0.0135(4) Uani 1 1 d . . . H10' H 0.5982 0.3035 1.2714 0.020 Uiso 1 1 calc R . . O11 O 0.3240(2) 0.31352(12) 1.17217(11) 0.0114(4) Uani 1 1 d . . . O12 O 0.0369(2) 0.35101(13) 1.15632(11) 0.0143(4) Uani 1 1 d . . . O13 O 0.0886(2) 0.18513(13) 1.15953(12) 0.0162(4) Uani 1 1 d . . . O14 O -0.0307(2) 0.24112(13) 1.01725(11) 0.0144(4) Uani 1 1 d . . . O15 O 0.0688(2) 0.25632(14) 0.88627(11) 0.0164(4) Uani 1 1 d . . . O16 O 0.2322(2) 0.25727(12) 1.02025(11) 0.0105(4) Uani 1 1 d . . . O90 O 0.3463(3) 0.02475(16) 0.35261(15) 0.0321(6) Uani 1 1 d . . . O91 O 0.1974(3) 0.01471(17) 0.19550(16) 0.0349(6) Uani 1 1 d . . . N1 N 0.2127(3) 0.54199(15) 0.42116(13) 0.0110(4) Uani 1 1 d . . . N2 N 0.1360(3) 0.57690(14) 0.55479(13) 0.0095(4) Uani 1 1 d . . . N3 N -0.0321(3) 0.69831(15) 0.53491(13) 0.0090(4) Uani 1 1 d . . . N4 N 0.5037(3) 0.26768(15) 0.92114(13) 0.0110(4) Uani 1 1 d . . . N5 N 0.3414(3) 0.39137(15) 0.89964(13) 0.0096(4) Uani 1 1 d . . . N6 N 0.3339(3) 0.46295(15) 1.03813(13) 0.0104(4) Uani 1 1 d . . . C1 C 0.2396(3) 0.52475(19) 0.34744(16) 0.0145(5) Uani 1 1 d . . . H1 H 0.2010 0.5599 0.3091 0.017 Uiso 1 1 calc R . . C2 C 0.3212(4) 0.45798(19) 0.32536(17) 0.0172(6) Uani 1 1 d . . . H2 H 0.3364 0.4467 0.2725 0.021 Uiso 1 1 calc R . . C3 C 0.3806(3) 0.40770(19) 0.38096(17) 0.0157(6) Uani 1 1 d . . . H3 H 0.4393 0.3624 0.3671 0.019 Uiso 1 1 calc R . . C4 C 0.3535(3) 0.42414(18) 0.45765(16) 0.0127(5) Uani 1 1 d . . . H4 H 0.3933 0.3905 0.4970 0.015 Uiso 1 1 calc R . . C5 C 0.2670(3) 0.49071(17) 0.47529(15) 0.0098(5) Uani 1 1 d . . . C6 C 0.2223(3) 0.51149(17) 0.55318(15) 0.0092(5) Uani 1 1 d . . . C7 C 0.2596(3) 0.46911(17) 0.61872(15) 0.0100(5) Uani 1 1 d . . . H7 H 0.3210 0.4225 0.6169 0.012 Uiso 1 1 calc R . . C8 C 0.2051(3) 0.49624(17) 0.68764(15) 0.0092(5) Uani 1 1 d . . . C9 C 0.1133(3) 0.56456(18) 0.68758(15) 0.0106(5) Uani 1 1 d . . . H9 H 0.0721 0.5829 0.7330 0.013 Uiso 1 1 calc R . . C10 C 0.0836(3) 0.60487(17) 0.61997(15) 0.0096(5) Uani 1 1 d . . . C11 C -0.0066(3) 0.67870(18) 0.61007(16) 0.0107(5) Uani 1 1 d . . . C12 C -0.0582(3) 0.72702(19) 0.67005(17) 0.0148(5) Uani 1 1 d . . . H12 H -0.0383 0.7132 0.7223 0.018 Uiso 1 1 calc R . . C13 C -0.1399(3) 0.7964(2) 0.65253(17) 0.0165(6) Uani 1 1 d . . . H13 H -0.1769 0.8305 0.6927 0.020 Uiso 1 1 calc R . . C14 C -0.1666(3) 0.81530(19) 0.57563(17) 0.0151(6) Uani 1 1 d . . . H14 H -0.2221 0.8624 0.5624 0.018 Uiso 1 1 calc R . . C15 C -0.1110(3) 0.76417(18) 0.51855(16) 0.0128(5) Uani 1 1 d . . . H15 H -0.1300 0.7767 0.4658 0.015 Uiso 1 1 calc R . . C16 C 0.5943(3) 0.20705(19) 0.93918(16) 0.0140(5) Uani 1 1 d . . . H16 H 0.6276 0.2022 0.9929 0.017 Uiso 1 1 calc R . . C17 C 0.6421(3) 0.15068(19) 0.88241(17) 0.0153(6) Uani 1 1 d . . . H17 H 0.7051 0.1073 0.8970 0.018 Uiso 1 1 calc R . . C18 C 0.5958(3) 0.15921(19) 0.80406(17) 0.0147(5) Uani 1 1 d . . . H18 H 0.6269 0.1216 0.7641 0.018 Uiso 1 1 calc R . . C19 C 0.5035(3) 0.22325(18) 0.78448(16) 0.0118(5) Uani 1 1 d . . . H19 H 0.4710 0.2302 0.7311 0.014 Uiso 1 1 calc R . . C20 C 0.4595(3) 0.27685(18) 0.84441(15) 0.0110(5) Uani 1 1 d . . . C21 C 0.3682(3) 0.35011(17) 0.83191(15) 0.0095(5) Uani 1 1 d . . . C22 C 0.3214(3) 0.38065(17) 0.76102(15) 0.0106(5) Uani 1 1 d . . . H22 H 0.3392 0.3505 0.7133 0.013 Uiso 1 1 calc R . . C23 C 0.2476(3) 0.45659(17) 0.76047(15) 0.0097(5) Uani 1 1 d . . . C24 C 0.2220(3) 0.49830(18) 0.83255(15) 0.0116(5) Uani 1 1 d . . . H24 H 0.1728 0.5500 0.8344 0.014 Uiso 1 1 calc R . . C25 C 0.2695(3) 0.46296(17) 0.90038(15) 0.0097(5) Uani 1 1 d . . . C26 C 0.2567(3) 0.50143(18) 0.98057(15) 0.0110(5) Uani 1 1 d . . . C27 C 0.1784(3) 0.57219(18) 0.99674(16) 0.0138(5) Uani 1 1 d . . . H27 H 0.1261 0.5987 0.9555 0.017 Uiso 1 1 calc R . . C28 C 0.1779(3) 0.60347(19) 1.07432(17) 0.0157(6) Uani 1 1 d . . . H28 H 0.1220 0.6506 1.0870 0.019 Uiso 1 1 calc R . . C29 C 0.2591(3) 0.56582(19) 1.13310(16) 0.0146(5) Uani 1 1 d . . . H29 H 0.2622 0.5877 1.1866 0.018 Uiso 1 1 calc R . . C30 C 0.3358(3) 0.49591(18) 1.11299(16) 0.0131(5) Uani 1 1 d . . . H30 H 0.3918 0.4702 1.1536 0.016 Uiso 1 1 calc R . . C31 C 0.0384(3) 0.84364(18) 0.32285(16) 0.0129(5) Uani 1 1 d . . . H31A H 0.0773 0.8753 0.3757 0.015 Uiso 1 1 calc R . . H31B H 0.0843 0.8757 0.2844 0.015 Uiso 1 1 calc R . . C32 C -0.1322(3) 0.84557(18) 0.30622(17) 0.0142(5) Uani 1 1 d . . . H32A H -0.1794 0.8054 0.3386 0.017 Uiso 1 1 calc R . . H32B H -0.1687 0.8227 0.2505 0.017 Uiso 1 1 calc R . . C33 C -0.1856(3) 0.93638(19) 0.32249(17) 0.0149(5) Uani 1 1 d . . . H33A H -0.1471 0.9753 0.2865 0.018 Uiso 1 1 calc R . . H33B H -0.2968 0.9305 0.3110 0.018 Uiso 1 1 calc R . . C34 C -0.1339(4) 0.97911(19) 0.40723(17) 0.0177(6) Uani 1 1 d . . . H34A H -0.1292 0.9324 0.4421 0.021 Uiso 1 1 calc R . . H34B H -0.0309 1.0090 0.4116 0.021 Uiso 1 1 calc R . . C35 C 0.2623(3) 0.88236(19) 0.61558(16) 0.0140(5) Uani 1 1 d . . . H35A H 0.1643 0.8575 0.6270 0.017 Uiso 1 1 calc R . . H35B H 0.3232 0.9094 0.6661 0.017 Uiso 1 1 calc R . . C36 C 0.2341(3) 0.95462(18) 0.56345(17) 0.0144(5) Uani 1 1 d . . . H36A H 0.1870 0.9272 0.5102 0.017 Uiso 1 1 calc R . . H36B H 0.3321 0.9863 0.5590 0.017 Uiso 1 1 calc R . . C37 C 0.4888(3) 0.17767(18) 1.15615(17) 0.0135(5) Uani 1 1 d . . . H37A H 0.4513 0.1561 1.2021 0.016 Uiso 1 1 calc R . . H37B H 0.4202 0.1493 1.1085 0.016 Uiso 1 1 calc R . . C38 C 0.6463(3) 0.14953(18) 1.15328(17) 0.0137(5) Uani 1 1 d . . . H38A H 0.6949 0.1824 1.1162 0.016 Uiso 1 1 calc R . . H38B H 0.7086 0.1642 1.2059 0.016 Uiso 1 1 calc R . . C39 C 0.6396(3) 0.05177(19) 1.12772(18) 0.0179(6) Uani 1 1 d . . . H39A H 0.6101 0.0194 1.1703 0.021 Uiso 1 1 calc R . . H39B H 0.5606 0.0354 1.0811 0.021 Uiso 1 1 calc R . . C40 C 0.7868(3) 0.02331(18) 1.10805(18) 0.0156(6) Uani 1 1 d . . . H40A H 0.8149 0.0539 1.0642 0.019 Uiso 1 1 calc R . . H40B H 0.8667 0.0410 1.1541 0.019 Uiso 1 1 calc R . . C41 C 0.0832(3) 0.10253(18) 0.94600(17) 0.0142(5) Uani 1 1 d . . . H41A H 0.0764 0.0778 0.9958 0.017 Uiso 1 1 calc R . . H41B H -0.0074 0.0778 0.9079 0.017 Uiso 1 1 calc R . . C42 C 0.2224(3) 0.07448(18) 0.91474(18) 0.0155(6) Uani 1 1 d . . . H42A H 0.2357 0.1046 0.8683 0.019 Uiso 1 1 calc R . . H42B H 0.3119 0.0934 0.9554 0.019 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 Cu1 0.01037(16) 0.00887(15) 0.00682(15) 0.00141(11) 0.00245(12) 0.00352(12) Cu2 0.01325(17) 0.00992(16) 0.00640(15) 0.00122(11) 0.00251(12) 0.00540(12) V1 0.0098(2) 0.0130(2) 0.0101(2) 0.00206(16) 0.00273(17) 0.00215(17) V2 0.0111(2) 0.0118(2) 0.0084(2) 0.00105(16) 0.00260(16) 0.00460(17) P1 0.0110(3) 0.0106(3) 0.0062(3) 0.0010(2) 0.0013(2) 0.0036(2) P2 0.0121(3) 0.0104(3) 0.0088(3) 0.0002(2) 0.0008(3) 0.0029(3) P3 0.0105(3) 0.0091(3) 0.0071(3) 0.0005(2) 0.0005(2) 0.0031(2) P4 0.0115(3) 0.0118(3) 0.0080(3) -0.0005(2) 0.0008(2) 0.0051(3) O1 0.0105(9) 0.0126(9) 0.0097(9) 0.0029(7) 0.0005(7) 0.0024(7) O2 0.0222(11) 0.0158(10) 0.0078(9) -0.0009(7) -0.0004(8) 0.0086(8) O3 0.0131(10) 0.0186(10) 0.0088(9) 0.0018(7) 0.0033(7) 0.0041(8) O4 0.0151(11) 0.0251(12) 0.0173(10) 0.0005(9) 0.0037(8) 0.0095(9) O5 0.0291(13) 0.0169(11) 0.0196(11) 0.0039(9) 0.0056(9) -0.0043(9) O6 0.0114(10) 0.0176(10) 0.0132(10) -0.0018(8) 0.0017(8) 0.0013(8) O7 0.0226(11) 0.0155(10) 0.0110(9) 0.0037(8) 0.0038(8) 0.0077(8) O8 0.0116(9) 0.0112(9) 0.0081(8) 0.0000(7) 0.0039(7) 0.0007(7) O9 0.0127(10) 0.0145(10) 0.0086(9) 0.0022(7) 0.0017(7) 0.0051(8) O10 0.0171(10) 0.0132(10) 0.0086(9) 0.0013(7) -0.0019(8) 0.0004(8) O11 0.0122(9) 0.0124(9) 0.0097(9) -0.0010(7) 0.0023(7) 0.0044(7) O12 0.0155(10) 0.0162(10) 0.0122(9) -0.0009(8) 0.0029(8) 0.0078(8) O13 0.0195(11) 0.0154(10) 0.0138(10) 0.0029(8) 0.0025(8) 0.0017(8) O14 0.0136(10) 0.0189(10) 0.0118(9) -0.0003(8) 0.0042(8) 0.0071(8) O15 0.0200(11) 0.0209(11) 0.0092(9) 0.0025(8) 0.0003(8) 0.0097(9) O16 0.0123(9) 0.0115(9) 0.0082(9) 0.0002(7) 0.0027(7) 0.0031(7) O90 0.0308(14) 0.0245(13) 0.0352(14) -0.0059(11) -0.0081(11) 0.0055(11) O91 0.0385(16) 0.0246(13) 0.0385(15) -0.0042(11) -0.0014(12) 0.0099(12) N1 0.0135(11) 0.0115(11) 0.0092(10) 0.0016(8) 0.0042(8) 0.0035(9) N2 0.0104(11) 0.0093(10) 0.0092(10) 0.0010(8) 0.0021(8) 0.0025(8) N3 0.0082(10) 0.0110(10) 0.0082(10) 0.0015(8) 0.0013(8) 0.0022(8) N4 0.0131(11) 0.0113(11) 0.0095(10) 0.0017(8) 0.0031(8) 0.0037(9) N5 0.0109(11) 0.0102(10) 0.0082(10) 0.0009(8) 0.0021(8) 0.0030(8) N6 0.0138(11) 0.0110(11) 0.0070(10) 0.0004(8) 0.0031(8) 0.0036(9) C1 0.0220(15) 0.0144(13) 0.0091(12) 0.0029(10) 0.0054(11) 0.0068(11) C2 0.0291(17) 0.0151(14) 0.0112(13) 0.0024(10) 0.0104(12) 0.0099(12) C3 0.0197(15) 0.0146(13) 0.0156(14) 0.0021(11) 0.0084(11) 0.0072(11) C4 0.0124(13) 0.0136(13) 0.0135(13) 0.0026(10) 0.0046(10) 0.0040(10) C5 0.0106(12) 0.0098(12) 0.0093(12) 0.0014(9) 0.0027(9) 0.0014(9) C6 0.0084(12) 0.0090(12) 0.0099(12) 0.0000(9) 0.0005(9) 0.0012(9) C7 0.0128(13) 0.0086(12) 0.0090(12) 0.0007(9) 0.0008(9) 0.0045(10) C8 0.0112(12) 0.0098(12) 0.0064(11) 0.0018(9) 0.0007(9) 0.0004(9) C9 0.0131(13) 0.0119(12) 0.0070(11) -0.0003(9) 0.0024(9) 0.0031(10) C10 0.0091(12) 0.0111(12) 0.0086(11) 0.0000(9) 0.0019(9) 0.0022(9) C11 0.0091(12) 0.0132(12) 0.0105(12) 0.0026(9) 0.0012(9) 0.0040(10) C12 0.0182(14) 0.0169(14) 0.0109(12) 0.0029(10) 0.0044(10) 0.0058(11) C13 0.0182(15) 0.0181(14) 0.0164(14) 0.0019(11) 0.0084(11) 0.0099(12) C14 0.0138(14) 0.0161(14) 0.0173(14) 0.0040(11) 0.0040(11) 0.0073(11) C15 0.0122(13) 0.0151(13) 0.0125(13) 0.0045(10) 0.0028(10) 0.0042(10) C16 0.0164(14) 0.0163(13) 0.0104(12) 0.0031(10) 0.0015(10) 0.0073(11) C17 0.0158(14) 0.0165(14) 0.0156(13) 0.0026(11) 0.0045(11) 0.0086(11) C18 0.0157(14) 0.0147(13) 0.0146(13) -0.0014(10) 0.0048(11) 0.0056(11) C19 0.0149(13) 0.0130(13) 0.0080(12) 0.0002(9) 0.0025(10) 0.0040(10) C20 0.0121(13) 0.0133(13) 0.0082(11) 0.0026(9) 0.0021(9) 0.0033(10) C21 0.0121(13) 0.0105(12) 0.0069(11) 0.0018(9) 0.0032(9) 0.0031(10) C22 0.0134(13) 0.0111(12) 0.0079(11) 0.0012(9) 0.0021(9) 0.0031(10) C23 0.0126(13) 0.0088(12) 0.0080(11) 0.0024(9) 0.0017(9) 0.0012(10) C24 0.0136(13) 0.0127(13) 0.0092(12) 0.0024(9) 0.0017(10) 0.0050(10) C25 0.0111(12) 0.0087(12) 0.0100(12) 0.0012(9) 0.0029(9) 0.0026(9) C26 0.0140(13) 0.0112(12) 0.0085(12) 0.0023(9) 0.0027(10) 0.0025(10) C27 0.0189(14) 0.0144(13) 0.0101(12) 0.0026(10) 0.0039(10) 0.0083(11) C28 0.0227(15) 0.0139(13) 0.0144(13) 0.0029(10) 0.0091(11) 0.0115(11) C29 0.0195(15) 0.0158(14) 0.0103(12) 0.0015(10) 0.0060(11) 0.0063(11) C30 0.0184(14) 0.0130(13) 0.0091(12) 0.0017(10) 0.0033(10) 0.0055(11) C31 0.0166(14) 0.0097(12) 0.0127(13) -0.0001(9) 0.0039(10) 0.0024(10) C32 0.0152(14) 0.0128(13) 0.0143(13) 0.0004(10) 0.0004(10) 0.0057(11) C33 0.0162(14) 0.0135(13) 0.0143(13) -0.0013(10) -0.0010(11) 0.0073(11) C34 0.0219(16) 0.0147(14) 0.0165(14) 0.0016(11) -0.0004(11) 0.0078(12) C35 0.0144(13) 0.0162(14) 0.0118(13) 0.0006(10) 0.0022(10) 0.0045(11) C36 0.0184(14) 0.0115(13) 0.0139(13) -0.0003(10) 0.0041(11) 0.0040(11) C37 0.0132(13) 0.0119(13) 0.0156(13) 0.0015(10) 0.0018(10) 0.0045(10) C38 0.0146(14) 0.0120(13) 0.0148(13) 0.0016(10) 0.0015(10) 0.0045(10) C39 0.0173(15) 0.0152(14) 0.0212(15) -0.0006(11) 0.0032(12) 0.0050(11) C40 0.0189(15) 0.0104(13) 0.0184(14) 0.0002(10) 0.0037(11) 0.0063(11) C41 0.0147(14) 0.0113(13) 0.0167(13) -0.0005(10) 0.0031(11) 0.0035(10) C42 0.0168(14) 0.0117(13) 0.0192(14) 0.0001(10) 0.0057(11) 0.0047(11) _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 O1 1.9089(19) . ? Cu1 N2 1.934(2) . ? Cu1 N3 2.028(2) . ? Cu1 N1 2.042(2) . ? Cu1 O8 2.1801(19) . ? Cu2 O9 1.9105(19) . ? Cu2 N5 1.934(2) . ? Cu2 N4 2.037(2) . ? Cu2 N6 2.060(2) . ? Cu2 O16 2.207(2) . ? V1 O4 1.623(2) . ? V1 O5 1.628(2) . ? V1 O3 1.959(2) . ? V1 O6 2.030(2) . ? V1 O8 2.0601(19) . ? V1 P2 2.7040(8) . ? V2 O13 1.618(2) . ? V2 O12 1.637(2) . ? V2 O11 1.973(2) . ? V2 O14 2.010(2) . ? V2 O16 2.0945(19) . ? V2 P4 2.6698(8) . ? P1 O1 1.521(2) . ? P1 O3 1.522(2) . ? P1 O2 1.555(2) . ? P1 C31 1.795(3) . ? P2 O7 1.490(2) . ? P2 O6 1.547(2) . ? P2 O8 1.568(2) . ? P2 C35 1.800(3) . ? P3 O9 1.523(2) . ? P3 O11 1.523(2) . ? P3 O10 1.564(2) . ? P3 C37 1.778(3) . ? P4 O15 1.498(2) . ? P4 O14 1.547(2) . ? P4 O16 1.565(2) . ? P4 C41 1.792(3) . ? N1 C1 1.343(3) . ? N1 C5 1.358(3) . ? N2 C6 1.334(3) . ? N2 C10 1.339(3) . ? N3 C15 1.328(3) . ? N3 C11 1.363(3) . ? N4 C16 1.333(3) . ? N4 C20 1.359(3) . ? N5 C25 1.335(3) . ? N5 C21 1.344(3) . ? N6 C30 1.342(3) . ? N6 C26 1.355(3) . ? C1 C2 1.378(4) . ? C2 C3 1.381(4) . ? C3 C4 1.392(4) . ? C4 C5 1.386(4) . ? C5 C6 1.481(4) . ? C6 C7 1.387(4) . ? C7 C8 1.401(4) . ? C8 C9 1.403(4) . ? C8 C23 1.479(4) . ? C9 C10 1.390(4) . ? C10 C11 1.473(4) . ? C11 C12 1.381(4) . ? C12 C13 1.392(4) . ? C13 C14 1.388(4) . ? C14 C15 1.386(4) . ? C16 C17 1.391(4) . ? C17 C18 1.386(4) . ? C18 C19 1.391(4) . ? C19 C20 1.389(4) . ? C20 C21 1.478(4) . ? C21 C22 1.387(4) . ? C22 C23 1.404(4) . ? C23 C24 1.407(4) . ? C24 C25 1.378(4) . ? C25 C26 1.481(4) . ? C26 C27 1.384(4) . ? C27 C28 1.383(4) . ? C28 C29 1.379(4) . ? C29 C30 1.380(4) . ? C31 C32 1.532(4) . ? C32 C33 1.538(4) . ? C33 C34 1.533(4) . ? C34 C36 1.527(4) 2_576 ? C35 C36 1.526(4) . ? C36 C34 1.527(4) 2_576 ? C37 C38 1.536(4) . ? C38 C39 1.521(4) . ? C39 C40 1.517(4) . ? C40 C42 1.511(4) 2_657 ? C41 C42 1.527(4) . ? C42 C40 1.511(4) 2_657 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Cu1 N2 167.74(9) . . ? O1 Cu1 N3 97.33(9) . . ? N2 Cu1 N3 79.82(9) . . ? O1 Cu1 N1 101.43(9) . . ? N2 Cu1 N1 79.37(9) . . ? N3 Cu1 N1 157.88(9) . . ? O1 Cu1 O8 91.90(8) . . ? N2 Cu1 O8 99.88(8) . . ? N3 Cu1 O8 88.04(8) . . ? N1 Cu1 O8 102.83(8) . . ? O9 Cu2 N5 164.72(9) . . ? O9 Cu2 N4 98.65(9) . . ? N5 Cu2 N4 79.58(9) . . ? O9 Cu2 N6 99.03(9) . . ? N5 Cu2 N6 79.36(9) . . ? N4 Cu2 N6 156.71(9) . . ? O9 Cu2 O16 90.26(8) . . ? N5 Cu2 O16 105.02(9) . . ? N4 Cu2 O16 98.18(8) . . ? N6 Cu2 O16 96.79(8) . . ? O4 V1 O5 108.33(12) . . ? O4 V1 O3 99.11(10) . . ? O5 V1 O3 96.21(10) . . ? O4 V1 O6 102.11(10) . . ? O5 V1 O6 95.58(10) . . ? O3 V1 O6 151.04(8) . . ? O4 V1 O8 119.34(10) . . ? O5 V1 O8 131.93(10) . . ? O3 V1 O8 82.68(8) . . ? O6 V1 O8 69.81(8) . . ? O4 V1 P2 114.86(8) . . ? O5 V1 P2 117.88(8) . . ? O3 V1 P2 117.51(6) . . ? O6 V1 P2 34.56(6) . . ? O8 V1 P2 35.25(6) . . ? O13 V2 O12 109.12(11) . . ? O13 V2 O11 98.83(10) . . ? O12 V2 O11 96.21(9) . . ? O13 V2 O14 100.53(10) . . ? O12 V2 O14 97.47(9) . . ? O11 V2 O14 151.09(8) . . ? O13 V2 O16 116.60(9) . . ? O12 V2 O16 134.00(9) . . ? O11 V2 O16 81.96(8) . . ? O14 V2 O16 70.23(8) . . ? O13 V2 P4 107.15(8) . . ? O12 V2 P4 124.61(7) . . ? O11 V2 P4 117.80(6) . . ? O14 V2 P4 35.15(6) . . ? O16 V2 P4 35.85(6) . . ? O1 P1 O3 112.46(11) . . ? O1 P1 O2 107.97(12) . . ? O3 P1 O2 106.77(12) . . ? O1 P1 C31 109.60(12) . . ? O3 P1 C31 110.16(13) . . ? O2 P1 C31 109.79(12) . . ? O7 P2 O6 116.47(12) . . ? O7 P2 O8 114.26(12) . . ? O6 P2 O8 97.44(11) . . ? O7 P2 C35 108.64(12) . . ? O6 P2 C35 109.85(13) . . ? O8 P2 C35 109.71(12) . . ? O7 P2 V1 129.98(9) . . ? O6 P2 V1 48.12(8) . . ? O8 P2 V1 49.33(7) . . ? C35 P2 V1 121.38(9) . . ? O9 P3 O11 113.57(11) . . ? O9 P3 O10 105.51(11) . . ? O11 P3 O10 108.69(11) . . ? O9 P3 C37 111.16(12) . . ? O11 P3 C37 109.55(13) . . ? O10 P3 C37 108.13(12) . . ? O15 P4 O14 116.95(11) . . ? O15 P4 O16 113.41(12) . . ? O14 P4 O16 98.76(11) . . ? O15 P4 C41 109.83(13) . . ? O14 P4 C41 109.04(13) . . ? O16 P4 C41 108.15(12) . . ? O15 P4 V2 140.14(9) . . ? O14 P4 V2 48.45(8) . . ? O16 P4 V2 51.60(7) . . ? C41 P4 V2 110.01(10) . . ? P1 O1 Cu1 127.35(12) . . ? P1 O3 V1 141.21(12) . . ? P2 O6 V1 97.32(10) . . ? P2 O8 V1 95.42(10) . . ? P2 O8 Cu1 132.29(11) . . ? V1 O8 Cu1 125.21(9) . . ? P3 O9 Cu2 126.54(12) . . ? P3 O11 V2 135.21(12) . . ? P4 O14 V2 96.40(10) . . ? P4 O16 V2 92.55(9) . . ? P4 O16 Cu2 127.78(11) . . ? V2 O16 Cu2 125.44(9) . . ? C1 N1 C5 118.3(2) . . ? C1 N1 Cu1 127.45(19) . . ? C5 N1 Cu1 114.28(17) . . ? C6 N2 C10 121.3(2) . . ? C6 N2 Cu1 119.84(18) . . ? C10 N2 Cu1 118.75(18) . . ? C15 N3 C11 119.3(2) . . ? C15 N3 Cu1 125.68(19) . . ? C11 N3 Cu1 113.76(17) . . ? C16 N4 C20 119.0(2) . . ? C16 N4 Cu2 126.72(19) . . ? C20 N4 Cu2 114.26(18) . . ? C25 N5 C21 120.8(2) . . ? C25 N5 Cu2 119.55(18) . . ? C21 N5 Cu2 119.55(18) . . ? C30 N6 C26 118.4(2) . . ? C30 N6 Cu2 127.62(19) . . ? C26 N6 Cu2 113.61(17) . . ? N1 C1 C2 122.5(3) . . ? C1 C2 C3 119.3(3) . . ? C2 C3 C4 119.2(3) . . ? C5 C4 C3 118.4(3) . . ? N1 C5 C4 122.3(2) . . ? N1 C5 C6 113.9(2) . . ? C4 C5 C6 123.9(2) . . ? N2 C6 C7 121.3(2) . . ? N2 C6 C5 112.4(2) . . ? C7 C6 C5 126.3(2) . . ? C6 C7 C8 118.8(2) . . ? C7 C8 C9 118.8(2) . . ? C7 C8 C23 121.1(2) . . ? C9 C8 C23 120.0(2) . . ? C10 C9 C8 118.9(2) . . ? N2 C10 C9 120.9(2) . . ? N2 C10 C11 112.9(2) . . ? C9 C10 C11 126.2(2) . . ? N3 C11 C12 121.5(2) . . ? N3 C11 C10 113.6(2) . . ? C12 C11 C10 124.9(2) . . ? C11 C12 C13 118.8(3) . . ? C14 C13 C12 119.3(3) . . ? C15 C14 C13 118.7(3) . . ? N3 C15 C14 122.3(3) . . ? N4 C16 C17 122.6(3) . . ? C18 C17 C16 118.5(3) . . ? C17 C18 C19 119.4(3) . . ? C20 C19 C18 118.8(3) . . ? N4 C20 C19 121.6(2) . . ? N4 C20 C21 114.0(2) . . ? C19 C20 C21 124.3(2) . . ? N5 C21 C22 120.8(2) . . ? N5 C21 C20 112.3(2) . . ? C22 C21 C20 126.7(2) . . ? C21 C22 C23 119.3(2) . . ? C22 C23 C24 118.2(2) . . ? C22 C23 C8 122.0(2) . . ? C24 C23 C8 119.7(2) . . ? C25 C24 C23 118.9(2) . . ? N5 C25 C24 121.8(2) . . ? N5 C25 C26 112.9(2) . . ? C24 C25 C26 125.1(2) . . ? N6 C26 C27 122.1(2) . . ? N6 C26 C25 113.8(2) . . ? C27 C26 C25 124.1(2) . . ? C28 C27 C26 118.5(3) . . ? C29 C28 C27 119.6(3) . . ? C28 C29 C30 119.0(3) . . ? N6 C30 C29 122.3(3) . . ? C32 C31 P1 114.7(2) . . ? C31 C32 C33 115.1(2) . . ? C34 C33 C32 113.3(2) . . ? C36 C34 C33 114.8(2) 2_576 . ? C36 C35 P2 116.27(19) . . ? C35 C36 C34 114.5(2) . 2_576 ? C38 C37 P3 114.2(2) . . ? C39 C38 C37 111.6(2) . . ? C40 C39 C38 113.8(3) . . ? C42 C40 C39 112.5(3) 2_657 . ? C42 C41 P4 113.1(2) . . ? C40 C42 C41 113.0(2) 2_657 . ? _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 31.51 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 1.037 _refine_diff_density_min -0.938 _refine_diff_density_rms 0.163