Supplementary Material for Dalton Transactions This journal is © The Royal Society of Chemistry 2005 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 of the Copper(II)-Terpyridine/Oxovanadium Organophosphonate System. Hydrothermal Syntheses and Structural Characterization of the One-Dimensional Materials [{Cu(terpy)}(V2O4)(O3PPh)(HO3PPh)2], [{Cu(terpy)}VO(O3PCH2PO3)], [{Cu(terpy)}2(V4O10)(O3PCH2CH2PO3)] and [{Cu(terpy)}(V2O4){O3P(CH2)3PO3}]*2H2O, the Two-Dimensional [{Cu(terpy)(H2O)}(V3O6){O3P(CH2)4PO3}], and the Three-Dimensional Phase [{Cu(terpy)}(V2O4){O3P(CH2)3PO3}]. ; loop_ _publ_author_name 'Jon Zubieta' 'Vladimir O. Golub' C.O'Connor 'Gundog Yucesan' data_compound_1 _database_code_depnum_ccdc_archive 'CCDC 247950' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C33 H28 Cu N3 O13 P3 V2' _chemical_formula_weight 932.91 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 8.8819(5) _cell_length_b 11.3639(7) _cell_length_c 18.4757(11) _cell_angle_alpha 98.9510(10) _cell_angle_beta 98.0030(10) _cell_angle_gamma 105.1140(10) _cell_volume 1746.49(18) _cell_formula_units_Z 2 _cell_measurement_temperature 89(2) _cell_measurement_reflns_used 11381 _cell_measurement_theta_min 1.89 _cell_measurement_theta_max 31.51 _exptl_crystal_description plate _exptl_crystal_colour green _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.774 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 942 _exptl_absorpt_coefficient_mu 1.338 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5542 _exptl_absorpt_correction_T_max 0.8245 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 89(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'Phi and omega scans' _diffrn_detector_area_resol_mean '512 x 512' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.001 _diffrn_reflns_number 22776 _diffrn_reflns_av_R_equivalents 0.0249 _diffrn_reflns_av_sigmaI/netI 0.0384 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.89 _diffrn_reflns_theta_max 31.51 _reflns_number_total 11381 _reflns_number_gt 10017 _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 6.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^)+(0.0393P)^2^+0.7546P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment refall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11381 _refine_ls_number_parameters 504 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0364 _refine_ls_R_factor_gt 0.0309 _refine_ls_wR_factor_ref 0.0821 _refine_ls_wR_factor_gt 0.0792 _refine_ls_goodness_of_fit_ref 1.051 _refine_ls_restrained_S_all 1.051 _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 O10 O 0.85664(12) 0.81520(10) 0.19569(6) 0.01135(19) Uani 1 1 d . . . Cu1 Cu 0.43799(2) 0.620592(16) 0.062798(10) 0.00834(4) Uani 1 1 d . . . V1 V 0.36578(3) 0.79372(2) 0.222059(13) 0.00763(5) Uani 1 1 d . . . V2 V 0.05764(3) 0.93297(2) 0.199441(13) 0.00785(5) Uani 1 1 d . . . P1 P 0.70241(4) 0.73315(3) 0.20949(2) 0.00759(7) Uani 1 1 d . . . P2 P 0.39668(4) 1.08355(3) 0.29799(2) 0.00898(7) Uani 1 1 d . . . P3 P -0.12188(4) 1.12265(3) 0.27986(2) 0.00855(7) Uani 1 1 d . . . O1 O 0.61318(12) 0.63753(10) 0.13951(6) 0.01026(19) Uani 1 1 d . . . O2 O 0.60091(12) 0.81432(9) 0.23902(6) 0.00965(19) Uani 1 1 d . . . O3 O 0.31674(13) 0.67394(11) 0.26016(7) 0.0158(2) Uani 1 1 d . . . O4 O 0.33380(12) 0.74617(11) 0.13090(6) 0.0131(2) Uani 1 1 d . . . O5 O 0.45031(12) 0.96885(10) 0.27365(6) 0.0122(2) Uani 1 1 d . . . O6 O 0.16302(12) 0.83629(10) 0.22486(6) 0.01117(19) Uani 1 1 d . . . O7 O 0.50954(13) 1.20064(10) 0.28232(6) 0.0126(2) Uani 1 1 d . . . O8 O 0.22889(12) 1.07258(10) 0.25845(6) 0.0127(2) Uani 1 1 d . . . O9 O 0.07196(13) 0.93530(10) 0.11448(6) 0.0138(2) Uani 1 1 d . . . O11 O -0.06073(12) 1.05870(10) 0.21658(6) 0.01113(19) Uani 1 1 d . . . O12 O -0.19637(14) 1.02707(11) 0.32725(6) 0.0126(2) Uani 1 1 d . . . N1 N 0.30973(15) 0.45268(11) 0.07705(7) 0.0106(2) Uani 1 1 d . . . N2 N 0.27697(14) 0.57204(11) -0.02689(7) 0.0095(2) Uani 1 1 d . . . N3 N 0.52627(14) 0.75920(12) 0.00893(7) 0.0103(2) Uani 1 1 d . . . C1 C 0.34024(18) 0.39744(14) 0.13418(8) 0.0130(3) Uani 1 1 d . . . H1 H 0.4349 0.4353 0.1702 0.016 Uiso 1 1 calc R . . C2 C 0.23829(19) 0.28682(14) 0.14249(9) 0.0150(3) Uani 1 1 d . . . H2 H 0.2624 0.2495 0.1835 0.018 Uiso 1 1 calc R . . C3 C 0.10013(19) 0.23197(14) 0.08934(9) 0.0153(3) Uani 1 1 d . . . H3 H 0.0276 0.1569 0.0940 0.018 Uiso 1 1 calc R . . C4 C 0.06875(18) 0.28768(14) 0.02929(9) 0.0134(3) Uani 1 1 d . . . H4 H -0.0246 0.2510 -0.0077 0.016 Uiso 1 1 calc R . . C5 C 0.17637(17) 0.39783(13) 0.02449(8) 0.0107(2) Uani 1 1 d . . . C6 C 0.15991(17) 0.46580(13) -0.03680(8) 0.0101(2) Uani 1 1 d . . . C7 C 0.04087(17) 0.42918(14) -0.10000(8) 0.0120(3) Uani 1 1 d . . . H7 H -0.0438 0.3550 -0.1069 0.014 Uiso 1 1 calc R . . C8 C 0.04914(17) 0.50432(14) -0.15300(8) 0.0126(3) Uani 1 1 d . . . H8 H -0.0312 0.4813 -0.1966 0.015 Uiso 1 1 calc R . . C9 C 0.17405(17) 0.61301(14) -0.14279(8) 0.0125(3) Uani 1 1 d . . . H9 H 0.1815 0.6635 -0.1793 0.015 Uiso 1 1 calc R . . C10 C 0.28755(17) 0.64529(13) -0.07740(8) 0.0102(2) Uani 1 1 d . . . C11 C 0.42777(16) 0.75673(13) -0.05501(8) 0.0100(2) Uani 1 1 d . . . C12 C 0.45825(17) 0.85124(14) -0.09508(8) 0.0122(3) Uani 1 1 d . . . H12 H 0.3863 0.8489 -0.1388 0.015 Uiso 1 1 calc R . . C13 C 0.59677(18) 0.94965(14) -0.06975(9) 0.0140(3) Uani 1 1 d . . . H13 H 0.6210 1.0153 -0.0962 0.017 Uiso 1 1 calc R . . C14 C 0.69832(18) 0.95063(14) -0.00577(9) 0.0143(3) Uani 1 1 d . . . H14 H 0.7943 1.0162 0.0117 0.017 Uiso 1 1 calc R . . C15 C 0.65880(17) 0.85465(14) 0.03299(8) 0.0125(3) Uani 1 1 d . . . H15 H 0.7277 0.8569 0.0777 0.015 Uiso 1 1 calc R . . C16 C 0.75401(17) 0.64997(13) 0.27934(8) 0.0103(2) Uani 1 1 d . . . C17 C 0.63375(18) 0.56679(14) 0.30302(8) 0.0129(3) Uani 1 1 d . . . H17 H 0.5260 0.5631 0.2870 0.015 Uiso 1 1 calc R . . C18 C 0.6706(2) 0.48957(14) 0.34962(9) 0.0161(3) Uani 1 1 d . . . H18 H 0.5882 0.4320 0.3645 0.019 Uiso 1 1 calc R . . C19 C 0.8283(2) 0.49656(16) 0.37443(10) 0.0193(3) Uani 1 1 d . . . H19 H 0.8537 0.4422 0.4052 0.023 Uiso 1 1 calc R . . C20 C 0.9487(2) 0.58294(16) 0.35420(9) 0.0187(3) Uani 1 1 d . . . H20 H 1.0565 0.5901 0.3730 0.022 Uiso 1 1 calc R . . C21 C 0.91233(18) 0.65923(15) 0.30651(9) 0.0145(3) Uani 1 1 d . . . H21 H 0.9952 0.7176 0.2924 0.017 Uiso 1 1 calc R . . C22 C 0.40299(18) 1.10590(14) 0.39635(8) 0.0126(3) Uani 1 1 d . . . C23 C 0.2909(2) 1.02549(16) 0.42564(10) 0.0197(3) Uani 1 1 d . . . H23 H 0.2083 0.9606 0.3930 0.024 Uiso 1 1 calc R . . C24 C 0.2993(2) 1.0397(2) 0.50230(11) 0.0274(4) Uani 1 1 d . . . H24 H 0.2227 0.9845 0.5218 0.033 Uiso 1 1 calc R . . C25 C 0.4190(3) 1.1339(2) 0.55013(10) 0.0288(4) Uani 1 1 d . . . H25 H 0.4238 1.1441 0.6025 0.035 Uiso 1 1 calc R . . C26 C 0.5319(2) 1.21342(18) 0.52198(10) 0.0255(4) Uani 1 1 d . . . H26 H 0.6147 1.2774 0.5551 0.031 Uiso 1 1 calc R . . C27 C 0.5249(2) 1.20022(15) 0.44544(9) 0.0179(3) Uani 1 1 d . . . H27 H 0.6027 1.2552 0.4264 0.021 Uiso 1 1 calc R . . C28 C 0.03717(17) 1.23331(14) 0.34608(8) 0.0113(3) Uani 1 1 d . . . C29 C 0.07118(19) 1.22380(15) 0.42036(9) 0.0154(3) Uani 1 1 d . . . H29 H 0.0124 1.1539 0.4370 0.019 Uiso 1 1 calc R . . C30 C 0.1913(2) 1.31657(16) 0.47052(10) 0.0199(3) Uani 1 1 d . . . H30 H 0.2140 1.3099 0.5213 0.024 Uiso 1 1 calc R . . C31 C 0.27776(19) 1.41864(16) 0.44645(10) 0.0201(3) Uani 1 1 d . . . H31 H 0.3589 1.4821 0.4808 0.024 Uiso 1 1 calc R . . C32 C 0.24595(19) 1.42830(15) 0.37221(10) 0.0192(3) Uani 1 1 d . . . H32 H 0.3062 1.4978 0.3557 0.023 Uiso 1 1 calc R . . C33 C 0.12563(18) 1.33607(15) 0.32200(9) 0.0153(3) Uani 1 1 d . . . H33 H 0.1035 1.3429 0.2713 0.018 Uiso 1 1 calc R . . O14 O -0.23559(12) 1.18944(10) 0.25024(6) 0.0119(2) Uani 1 1 d . . . H102 H 0.597(4) 1.200(3) 0.2746(16) 0.052(9) Uiso 1 1 d . . . H103 H -0.257(3) 0.981(2) 0.3057(15) 0.034(7) 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 O10 0.0057(4) 0.0119(5) 0.0160(5) 0.0032(4) 0.0027(4) 0.0011(4) Cu1 0.00694(8) 0.00831(8) 0.00836(8) 0.00083(6) 0.00048(6) 0.00080(6) V1 0.00548(10) 0.00707(10) 0.00986(11) 0.00076(8) 0.00135(8) 0.00158(8) V2 0.00527(10) 0.00869(11) 0.00890(11) 0.00047(8) 0.00161(8) 0.00144(8) P1 0.00518(14) 0.00747(15) 0.00945(15) 0.00091(12) 0.00081(12) 0.00145(11) P2 0.00607(15) 0.00790(15) 0.01170(16) -0.00077(12) 0.00080(12) 0.00188(12) P3 0.00619(15) 0.00896(16) 0.01007(16) 0.00144(12) 0.00103(12) 0.00197(12) O1 0.0085(4) 0.0107(5) 0.0103(5) 0.0000(4) -0.0001(4) 0.0028(4) O2 0.0060(4) 0.0094(4) 0.0130(5) 0.0001(4) 0.0015(4) 0.0026(3) O3 0.0099(5) 0.0146(5) 0.0251(6) 0.0099(4) 0.0042(4) 0.0035(4) O4 0.0089(5) 0.0178(5) 0.0116(5) -0.0019(4) 0.0005(4) 0.0054(4) O5 0.0071(4) 0.0094(5) 0.0178(5) -0.0026(4) 0.0002(4) 0.0027(4) O6 0.0067(4) 0.0092(5) 0.0166(5) 0.0010(4) 0.0017(4) 0.0017(4) O7 0.0086(5) 0.0106(5) 0.0191(5) 0.0019(4) 0.0050(4) 0.0028(4) O8 0.0082(4) 0.0101(5) 0.0173(5) -0.0022(4) -0.0015(4) 0.0032(4) O9 0.0126(5) 0.0164(5) 0.0114(5) 0.0020(4) 0.0039(4) 0.0021(4) O11 0.0082(4) 0.0117(5) 0.0131(5) 0.0012(4) 0.0015(4) 0.0033(4) O12 0.0113(5) 0.0117(5) 0.0120(5) 0.0026(4) 0.0004(4) -0.0008(4) N1 0.0100(5) 0.0096(5) 0.0113(5) 0.0010(4) 0.0014(4) 0.0021(4) N2 0.0083(5) 0.0098(5) 0.0097(5) 0.0009(4) 0.0016(4) 0.0018(4) N3 0.0086(5) 0.0112(5) 0.0103(5) 0.0016(4) 0.0019(4) 0.0018(4) C1 0.0142(6) 0.0120(6) 0.0120(6) 0.0021(5) 0.0015(5) 0.0029(5) C2 0.0173(7) 0.0131(7) 0.0157(7) 0.0048(5) 0.0049(6) 0.0045(5) C3 0.0163(7) 0.0100(6) 0.0183(7) 0.0025(5) 0.0037(6) 0.0017(5) C4 0.0120(6) 0.0102(6) 0.0158(7) 0.0003(5) 0.0019(5) 0.0010(5) C5 0.0104(6) 0.0094(6) 0.0117(6) 0.0000(5) 0.0026(5) 0.0029(5) C6 0.0090(6) 0.0101(6) 0.0106(6) 0.0000(5) 0.0024(5) 0.0028(5) C7 0.0087(6) 0.0126(6) 0.0125(6) -0.0009(5) 0.0010(5) 0.0018(5) C8 0.0102(6) 0.0145(7) 0.0110(6) -0.0009(5) -0.0009(5) 0.0033(5) C9 0.0122(6) 0.0142(7) 0.0110(6) 0.0026(5) 0.0019(5) 0.0040(5) C10 0.0090(6) 0.0110(6) 0.0107(6) 0.0008(5) 0.0025(5) 0.0035(5) C11 0.0088(6) 0.0112(6) 0.0092(6) 0.0007(5) 0.0021(5) 0.0020(5) C12 0.0117(6) 0.0134(6) 0.0111(6) 0.0026(5) 0.0021(5) 0.0029(5) C13 0.0141(7) 0.0126(7) 0.0156(7) 0.0044(5) 0.0047(5) 0.0026(5) C14 0.0113(6) 0.0130(7) 0.0167(7) 0.0030(5) 0.0031(5) -0.0001(5) C15 0.0087(6) 0.0132(6) 0.0132(6) 0.0019(5) 0.0010(5) 0.0000(5) C16 0.0106(6) 0.0097(6) 0.0105(6) 0.0009(5) 0.0015(5) 0.0037(5) C17 0.0130(6) 0.0115(6) 0.0124(6) 0.0015(5) 0.0009(5) 0.0015(5) C18 0.0214(7) 0.0114(7) 0.0147(7) 0.0033(5) 0.0028(6) 0.0031(6) C19 0.0252(8) 0.0177(7) 0.0180(7) 0.0067(6) 0.0023(6) 0.0104(6) C20 0.0176(7) 0.0233(8) 0.0181(7) 0.0066(6) 0.0010(6) 0.0109(6) C21 0.0125(6) 0.0163(7) 0.0152(7) 0.0035(5) 0.0012(5) 0.0053(5) C22 0.0138(6) 0.0117(6) 0.0133(6) 0.0019(5) 0.0030(5) 0.0057(5) C23 0.0194(8) 0.0196(8) 0.0230(8) 0.0079(6) 0.0082(6) 0.0065(6) C24 0.0326(10) 0.0340(10) 0.0266(9) 0.0171(8) 0.0158(8) 0.0168(8) C25 0.0452(12) 0.0356(11) 0.0149(8) 0.0082(7) 0.0076(8) 0.0247(9) C26 0.0359(10) 0.0247(9) 0.0144(8) -0.0006(6) -0.0041(7) 0.0131(8) C27 0.0218(8) 0.0149(7) 0.0155(7) 0.0010(6) -0.0010(6) 0.0062(6) C28 0.0084(6) 0.0113(6) 0.0137(6) -0.0001(5) 0.0019(5) 0.0038(5) C29 0.0146(7) 0.0146(7) 0.0152(7) 0.0006(5) 0.0003(5) 0.0039(5) C30 0.0195(8) 0.0184(8) 0.0178(8) -0.0032(6) -0.0032(6) 0.0063(6) C31 0.0117(7) 0.0173(7) 0.0247(8) -0.0074(6) -0.0026(6) 0.0026(6) C32 0.0107(7) 0.0143(7) 0.0285(9) -0.0015(6) 0.0048(6) -0.0008(5) C33 0.0121(6) 0.0139(7) 0.0177(7) 0.0010(5) 0.0034(5) 0.0010(5) O14 0.0086(4) 0.0152(5) 0.0141(5) 0.0050(4) 0.0027(4) 0.0057(4) _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 O10 P1 1.5218(11) . ? O10 V2 1.9168(10) 1_655 ? Cu1 O1 1.9005(10) . ? Cu1 N2 1.9339(12) . ? Cu1 N1 2.0284(12) . ? Cu1 N3 2.0365(13) . ? Cu1 O4 2.2205(11) . ? V1 O3 1.6163(11) . ? V1 O4 1.6470(11) . ? V1 O5 1.9658(11) . ? V1 O6 1.9881(10) . ? V1 O2 2.0135(10) . ? V2 O9 1.5961(11) . ? V2 O6 1.6965(11) . ? V2 O10 1.9168(10) 1_455 ? V2 O8 1.9392(11) . ? V2 O11 1.9955(11) . ? P1 O1 1.5194(11) . ? P1 O2 1.5411(10) . ? P1 C16 1.7917(15) . ? P2 O5 1.5262(11) . ? P2 O8 1.5303(11) . ? P2 O7 1.5377(11) . ? P2 C22 1.7862(16) . ? P3 O14 1.5069(11) . ? P3 O11 1.5194(11) . ? P3 O12 1.5706(12) . ? P3 C28 1.7854(15) . ? N1 C1 1.3404(19) . ? N1 C5 1.3568(19) . ? N2 C6 1.3400(18) . ? N2 C10 1.3408(19) . ? N3 C15 1.3410(18) . ? N3 C11 1.3604(19) . ? C1 C2 1.389(2) . ? C2 C3 1.391(2) . ? C3 C4 1.391(2) . ? C4 C5 1.387(2) . ? C5 C6 1.478(2) . ? C6 C7 1.389(2) . ? C7 C8 1.393(2) . ? C8 C9 1.395(2) . ? C9 C10 1.393(2) . ? C10 C11 1.482(2) . ? C11 C12 1.388(2) . ? C12 C13 1.394(2) . ? C13 C14 1.380(2) . ? C14 C15 1.393(2) . ? C16 C21 1.396(2) . ? C16 C17 1.399(2) . ? C17 C18 1.387(2) . ? C18 C19 1.390(2) . ? C19 C20 1.387(2) . ? C20 C21 1.392(2) . ? C22 C23 1.396(2) . ? C22 C27 1.401(2) . ? C23 C24 1.389(3) . ? C24 C25 1.381(3) . ? C25 C26 1.382(3) . ? C26 C27 1.389(2) . ? C28 C29 1.391(2) . ? C28 C33 1.400(2) . ? C29 C30 1.394(2) . ? C30 C31 1.387(3) . ? C31 C32 1.389(3) . ? C32 C33 1.392(2) . ? 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 P1 O10 V2 168.35(7) . 1_655 ? O1 Cu1 N2 166.39(5) . . ? O1 Cu1 N1 95.28(5) . . ? N2 Cu1 N1 79.86(5) . . ? O1 Cu1 N3 102.27(5) . . ? N2 Cu1 N3 80.32(5) . . ? N1 Cu1 N3 158.73(5) . . ? O1 Cu1 O4 94.85(4) . . ? N2 Cu1 O4 98.53(5) . . ? N1 Cu1 O4 100.56(5) . . ? N3 Cu1 O4 89.93(5) . . ? O3 V1 O4 108.86(6) . . ? O3 V1 O5 126.82(6) . . ? O4 V1 O5 124.32(5) . . ? O3 V1 O6 95.07(5) . . ? O4 V1 O6 96.03(5) . . ? O5 V1 O6 80.49(4) . . ? O3 V1 O2 96.79(5) . . ? O4 V1 O2 95.99(5) . . ? O5 V1 O2 78.91(4) . . ? O6 V1 O2 159.39(4) . . ? O9 V2 O6 104.79(6) . . ? O9 V2 O10 105.40(5) . 1_455 ? O6 V2 O10 93.63(5) . 1_455 ? O9 V2 O8 105.80(5) . . ? O6 V2 O8 88.78(5) . . ? O10 V2 O8 146.94(5) 1_455 . ? O9 V2 O11 99.41(5) . . ? O6 V2 O11 155.38(5) . . ? O10 V2 O11 84.13(4) 1_455 . ? O8 V2 O11 80.29(4) . . ? O1 P1 O10 110.92(6) . . ? O1 P1 O2 112.13(6) . . ? O10 P1 O2 110.02(6) . . ? O1 P1 C16 107.47(6) . . ? O10 P1 C16 107.30(6) . . ? O2 P1 C16 108.83(6) . . ? O5 P2 O8 112.97(6) . . ? O5 P2 O7 110.84(6) . . ? O8 P2 O7 107.59(6) . . ? O5 P2 C22 108.49(7) . . ? O8 P2 C22 109.13(7) . . ? O7 P2 C22 107.68(7) . . ? O14 P3 O11 110.62(6) . . ? O14 P3 O12 112.71(6) . . ? O11 P3 O12 110.55(6) . . ? O14 P3 C28 108.37(7) . . ? O11 P3 C28 111.25(6) . . ? O12 P3 C28 103.11(7) . . ? P1 O1 Cu1 136.06(7) . . ? P1 O2 V1 133.27(6) . . ? V1 O4 Cu1 129.77(6) . . ? P2 O5 V1 141.28(7) . . ? V2 O6 V1 144.39(6) . . ? P2 O8 V2 132.71(7) . . ? P3 O11 V2 138.78(7) . . ? C1 N1 C5 119.17(13) . . ? C1 N1 Cu1 126.36(10) . . ? C5 N1 Cu1 114.36(10) . . ? C6 N2 C10 122.33(13) . . ? C6 N2 Cu1 118.92(10) . . ? C10 N2 Cu1 118.74(10) . . ? C15 N3 C11 118.85(13) . . ? C15 N3 Cu1 127.37(10) . . ? C11 N3 Cu1 113.47(9) . . ? N1 C1 C2 122.31(14) . . ? C1 C2 C3 118.44(15) . . ? C2 C3 C4 119.61(14) . . ? C5 C4 C3 118.73(14) . . ? N1 C5 C4 121.72(14) . . ? N1 C5 C6 113.71(12) . . ? C4 C5 C6 124.57(13) . . ? N2 C6 C7 120.42(14) . . ? N2 C6 C5 112.82(12) . . ? C7 C6 C5 126.76(13) . . ? C6 C7 C8 118.16(13) . . ? C7 C8 C9 120.73(14) . . ? C10 C9 C8 118.00(14) . . ? N2 C10 C9 120.33(13) . . ? N2 C10 C11 112.81(12) . . ? C9 C10 C11 126.86(13) . . ? N3 C11 C12 122.09(13) . . ? N3 C11 C10 114.18(13) . . ? C12 C11 C10 123.73(13) . . ? C11 C12 C13 118.53(14) . . ? C14 C13 C12 119.29(14) . . ? C13 C14 C15 119.37(14) . . ? N3 C15 C14 121.84(14) . . ? C21 C16 C17 119.10(14) . . ? C21 C16 P1 121.17(11) . . ? C17 C16 P1 119.55(11) . . ? C18 C17 C16 120.57(14) . . ? C17 C18 C19 119.88(15) . . ? C20 C19 C18 119.97(15) . . ? C19 C20 C21 120.34(15) . . ? C20 C21 C16 120.03(15) . . ? C23 C22 C27 118.97(15) . . ? C23 C22 P2 120.34(12) . . ? C27 C22 P2 120.61(12) . . ? C24 C23 C22 120.43(17) . . ? C25 C24 C23 120.07(18) . . ? C24 C25 C26 120.15(17) . . ? C25 C26 C27 120.36(18) . . ? C26 C27 C22 120.00(17) . . ? C29 C28 C33 119.46(14) . . ? C29 C28 P3 122.70(12) . . ? C33 C28 P3 117.78(12) . . ? C28 C29 C30 120.20(16) . . ? C31 C30 C29 120.07(16) . . ? C30 C31 C32 120.18(15) . . ? C31 C32 C33 119.92(16) . . ? C32 C33 C28 120.17(15) . . ? _diffrn_measured_fraction_theta_max 0.978 _diffrn_reflns_theta_full 31.51 _diffrn_measured_fraction_theta_full 0.978 _refine_diff_density_max 0.638 _refine_diff_density_min -0.387 _refine_diff_density_rms 0.091 data_compound_2 _database_code_depnum_ccdc_archive 'CCDC 247951' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H13 Cu N3 O7 P2 V' _chemical_formula_weight 535.71 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 P21/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 10.5656(6) _cell_length_b 7.7040(4) _cell_length_c 22.4544(13) _cell_angle_alpha 90.00 _cell_angle_beta 99.1410(10) _cell_angle_gamma 90.00 _cell_volume 1804.52(17) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 6345 _cell_measurement_theta_min 1.84 _cell_measurement_theta_max 32.89 _exptl_crystal_description block _exptl_crystal_colour olive _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.972 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1072 _exptl_absorpt_coefficient_mu 1.924 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6247 _exptl_absorpt_correction_T_max 0.9445 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'Phi and omega scans' _diffrn_detector_area_resol_mean '512 x 512' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.001 _diffrn_reflns_number 23299 _diffrn_reflns_av_R_equivalents 0.0266 _diffrn_reflns_av_sigmaI/netI 0.0266 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 1.84 _diffrn_reflns_theta_max 32.89 _reflns_number_total 6345 _reflns_number_gt 5505 _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 6.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^)+(0.0378P)^2^+0.7977P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment refall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6345 _refine_ls_number_parameters 279 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0373 _refine_ls_R_factor_gt 0.0310 _refine_ls_wR_factor_ref 0.0788 _refine_ls_wR_factor_gt 0.0757 _refine_ls_goodness_of_fit_ref 1.058 _refine_ls_restrained_S_all 1.058 _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 O7 O 0.29418(12) 0.54712(15) 0.17863(6) 0.0236(2) Uani 1 1 d . . . Cu1 Cu 0.509433(19) 0.13629(2) 0.098516(9) 0.01769(5) Uani 1 1 d . . . V1 V 0.36185(2) 0.15434(3) 0.303932(11) 0.01432(6) Uani 1 1 d . . . P1 P 0.30343(4) -0.01212(5) 0.170936(17) 0.01500(8) Uani 1 1 d . . . P2 P 0.35872(4) 0.36829(5) 0.182495(19) 0.01653(8) Uani 1 1 d . . . O1 O 0.45604(12) 0.36538(14) 0.14005(6) 0.0222(2) Uani 1 1 d . . . O2 O 0.40633(11) -0.03174(15) 0.13073(5) 0.0215(2) Uani 1 1 d . . . O3 O 0.41541(12) 0.32199(15) 0.24735(5) 0.0221(2) Uani 1 1 d . . . O4 O 0.19515(12) -0.14087(14) 0.15268(5) 0.0202(2) Uani 1 1 d . . . O5 O 0.35886(12) -0.02380(14) 0.23806(5) 0.0201(2) Uani 1 1 d . . . O6 O 0.48093(13) 0.08886(18) 0.35139(6) 0.0298(3) Uani 1 1 d . . . N1 N 0.67389(14) 0.11356(19) 0.15890(7) 0.0215(3) Uani 1 1 d . . . N2 N 0.63118(14) 0.24196(18) 0.05279(6) 0.0204(3) Uani 1 1 d . . . N3 N 0.39633(15) 0.16498(19) 0.01501(6) 0.0227(3) Uani 1 1 d . . . C1 C 0.68473(19) 0.0470(2) 0.21445(8) 0.0279(4) Uani 1 1 d . . . H1 H 0.6140 -0.0063 0.2265 0.033 Uiso 1 1 calc R . . C2 C 0.7987(2) 0.0554(3) 0.25457(9) 0.0329(4) Uani 1 1 d . . . H2 H 0.8057 0.0018 0.2921 0.039 Uiso 1 1 calc R . . C3 C 0.9014(2) 0.1436(3) 0.23851(10) 0.0339(4) Uani 1 1 d . . . H3 H 0.9774 0.1541 0.2655 0.041 Uiso 1 1 calc R . . C4 C 0.88961(18) 0.2168(3) 0.18132(9) 0.0296(4) Uani 1 1 d . . . H4 H 0.9572 0.2786 0.1696 0.035 Uiso 1 1 calc R . . C5 C 0.77597(16) 0.1961(2) 0.14225(8) 0.0218(3) Uani 1 1 d . . . C6 C 0.75280(17) 0.2597(2) 0.07920(8) 0.0230(3) Uani 1 1 d . . . C7 C 0.8441(2) 0.3271(3) 0.04698(10) 0.0340(4) Uani 1 1 d . . . H7 H 0.9287 0.3429 0.0653 0.041 Uiso 1 1 calc R . . C8 C 0.8051(2) 0.3700(3) -0.01312(10) 0.0395(5) Uani 1 1 d . . . H8 H 0.8648 0.4129 -0.0357 0.047 Uiso 1 1 calc R . . C9 C 0.6788(2) 0.3499(3) -0.04010(9) 0.0320(4) Uani 1 1 d . . . H9 H 0.6528 0.3785 -0.0804 0.038 Uiso 1 1 calc R . . C10 C 0.59176(18) 0.2856(2) -0.00498(7) 0.0228(3) Uani 1 1 d . . . C11 C 0.45468(18) 0.2524(2) -0.02536(7) 0.0236(3) Uani 1 1 d . . . C12 C 0.3887(2) 0.3048(3) -0.08076(8) 0.0334(4) Uani 1 1 d . . . H12 H 0.4305 0.3649 -0.1079 0.040 Uiso 1 1 calc R . . C13 C 0.2596(2) 0.2660(3) -0.09492(9) 0.0387(5) Uani 1 1 d . . . H13 H 0.2132 0.3007 -0.1317 0.046 Uiso 1 1 calc R . . C14 C 0.2000(2) 0.1754(3) -0.05401(10) 0.0362(4) Uani 1 1 d . . . H14 H 0.1133 0.1480 -0.0629 0.043 Uiso 1 1 calc R . . C15 C 0.27178(19) 0.1263(2) 0.00046(9) 0.0288(4) Uani 1 1 d . . . H15 H 0.2320 0.0643 0.0279 0.035 Uiso 1 1 calc R . . C16 C 0.23762(16) 0.2047(2) 0.15971(8) 0.0189(3) Uani 1 1 d . . . H16A H 0.196(2) 0.216(3) 0.1188(10) 0.028(6) Uiso 1 1 d . . . H16B H 0.182(2) 0.210(3) 0.1799(10) 0.030(6) 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 O7 0.0292(6) 0.0131(5) 0.0322(6) 0.0025(4) 0.0167(5) 0.0046(4) Cu1 0.01944(10) 0.01871(10) 0.01639(9) 0.00100(7) 0.00740(7) 0.00053(7) V1 0.01618(12) 0.01255(11) 0.01444(11) 0.00050(8) 0.00306(9) 0.00157(8) P1 0.01923(18) 0.01146(16) 0.01568(17) 0.00051(13) 0.00700(13) -0.00025(13) P2 0.02082(19) 0.01106(16) 0.01999(18) 0.00091(13) 0.01025(15) 0.00076(13) O1 0.0275(6) 0.0166(5) 0.0264(6) -0.0005(4) 0.0163(5) 0.0000(4) O2 0.0259(6) 0.0173(5) 0.0245(6) -0.0001(4) 0.0140(5) -0.0006(4) O3 0.0277(6) 0.0194(5) 0.0201(5) 0.0027(4) 0.0064(5) -0.0054(5) O4 0.0252(6) 0.0146(5) 0.0216(5) 0.0011(4) 0.0057(5) -0.0036(4) O5 0.0290(6) 0.0158(5) 0.0158(5) -0.0008(4) 0.0048(4) 0.0031(4) O6 0.0293(7) 0.0291(6) 0.0277(6) -0.0017(5) -0.0058(5) 0.0108(5) N1 0.0218(7) 0.0216(6) 0.0219(7) 0.0017(5) 0.0056(5) 0.0005(5) N2 0.0248(7) 0.0199(6) 0.0182(6) 0.0006(5) 0.0088(5) 0.0006(5) N3 0.0279(7) 0.0221(7) 0.0189(6) 0.0002(5) 0.0062(5) 0.0016(5) C1 0.0299(9) 0.0285(9) 0.0254(8) 0.0071(7) 0.0046(7) -0.0010(7) C2 0.0375(10) 0.0319(10) 0.0268(9) 0.0065(7) -0.0022(8) 0.0025(8) C3 0.0303(10) 0.0292(9) 0.0384(11) 0.0001(8) -0.0058(8) 0.0039(7) C4 0.0213(8) 0.0283(9) 0.0384(10) 0.0014(8) 0.0029(7) -0.0004(7) C5 0.0208(7) 0.0202(7) 0.0254(8) 0.0003(6) 0.0068(6) 0.0008(6) C6 0.0245(8) 0.0211(7) 0.0253(8) -0.0008(6) 0.0098(6) -0.0021(6) C7 0.0295(10) 0.0397(11) 0.0359(10) 0.0005(8) 0.0145(8) -0.0095(8) C8 0.0434(12) 0.0423(12) 0.0381(11) 0.0047(9) 0.0230(10) -0.0128(9) C9 0.0450(11) 0.0313(9) 0.0230(8) 0.0055(7) 0.0157(8) -0.0046(8) C10 0.0321(9) 0.0188(7) 0.0193(7) 0.0010(6) 0.0101(6) 0.0004(6) C11 0.0329(9) 0.0202(7) 0.0186(7) 0.0004(6) 0.0069(6) 0.0043(6) C12 0.0436(11) 0.0355(10) 0.0215(8) 0.0064(7) 0.0070(8) 0.0077(9) C13 0.0419(12) 0.0461(12) 0.0260(9) 0.0040(9) -0.0012(8) 0.0125(10) C14 0.0298(10) 0.0419(11) 0.0354(11) -0.0021(9) 0.0004(8) 0.0060(8) C15 0.0293(9) 0.0290(9) 0.0287(9) -0.0031(7) 0.0067(7) 0.0013(7) C16 0.0191(7) 0.0150(6) 0.0234(8) 0.0017(5) 0.0060(6) 0.0015(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O7 P2 1.5336(12) . ? O7 V1 1.9388(12) 2 ? Cu1 O2 1.9068(11) . ? Cu1 N2 1.9471(14) . ? Cu1 N1 2.0346(15) . ? Cu1 N3 2.0690(15) . ? Cu1 O1 2.1143(11) . ? V1 O6 1.5960(13) . ? V1 O7 1.9387(12) 2_545 ? V1 O3 1.9574(12) . ? V1 O4 1.9969(11) 2 ? V1 O5 2.0143(11) . ? P1 O4 1.5204(12) . ? P1 O2 1.5270(12) . ? P1 O5 1.5305(12) . ? P1 C16 1.8112(16) . ? P2 O1 1.5091(12) . ? P2 O3 1.5262(13) . ? P2 C16 1.8111(17) . ? O4 V1 1.9968(11) 2_545 ? N1 C1 1.337(2) . ? N1 C5 1.355(2) . ? N2 C6 1.334(2) . ? N2 C10 1.341(2) . ? N3 C15 1.338(2) . ? N3 C11 1.354(2) . ? C1 C2 1.386(3) . ? C2 C3 1.376(3) . ? C3 C4 1.390(3) . ? C4 C5 1.379(2) . ? C5 C6 1.481(2) . ? C6 C7 1.395(2) . ? C7 C8 1.387(3) . ? C8 C9 1.384(3) . ? C9 C10 1.394(2) . ? C10 C11 1.470(3) . ? C11 C12 1.386(2) . ? C12 C13 1.384(3) . ? C13 C14 1.382(3) . ? C14 C15 1.386(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 P2 O7 V1 139.12(7) . 2 ? O2 Cu1 N2 161.61(5) . . ? O2 Cu1 N1 99.65(6) . . ? N2 Cu1 N1 79.73(6) . . ? O2 Cu1 N3 97.68(6) . . ? N2 Cu1 N3 79.18(6) . . ? N1 Cu1 N3 157.26(6) . . ? O2 Cu1 O1 101.00(5) . . ? N2 Cu1 O1 97.38(5) . . ? N1 Cu1 O1 92.14(6) . . ? N3 Cu1 O1 98.88(5) . . ? O6 V1 O7 109.63(7) . 2_545 ? O6 V1 O3 111.31(7) . . ? O7 V1 O3 139.03(6) 2_545 . ? O6 V1 O4 101.00(6) . 2 ? O7 V1 O4 84.60(5) 2_545 2 ? O3 V1 O4 86.34(5) . 2 ? O6 V1 O5 101.17(6) . . ? O7 V1 O5 86.76(5) 2_545 . ? O3 V1 O5 86.87(5) . . ? O4 V1 O5 157.79(5) 2 . ? O4 P1 O2 110.61(7) . . ? O4 P1 O5 112.39(7) . . ? O2 P1 O5 112.30(7) . . ? O4 P1 C16 107.95(7) . . ? O2 P1 C16 107.61(7) . . ? O5 P1 C16 105.65(7) . . ? O1 P2 O3 113.30(7) . . ? O1 P2 O7 108.60(7) . . ? O3 P2 O7 111.57(7) . . ? O1 P2 C16 109.44(7) . . ? O3 P2 C16 105.04(7) . . ? O7 P2 C16 108.75(7) . . ? P2 O1 Cu1 123.18(7) . . ? P1 O2 Cu1 131.33(7) . . ? P2 O3 V1 131.56(7) . . ? P1 O4 V1 131.02(8) . 2_545 ? P1 O5 V1 129.94(7) . . ? C1 N1 C5 118.92(16) . . ? C1 N1 Cu1 126.33(12) . . ? C5 N1 Cu1 114.13(11) . . ? C6 N2 C10 122.25(15) . . ? C6 N2 Cu1 118.61(11) . . ? C10 N2 Cu1 119.04(12) . . ? C15 N3 C11 118.82(16) . . ? C15 N3 Cu1 126.98(13) . . ? C11 N3 Cu1 113.64(12) . . ? N1 C1 C2 121.69(18) . . ? C3 C2 C1 119.50(18) . . ? C2 C3 C4 118.96(18) . . ? C5 C4 C3 118.80(18) . . ? N1 C5 C4 121.98(16) . . ? N1 C5 C6 113.65(15) . . ? C4 C5 C6 124.38(16) . . ? N2 C6 C7 120.29(17) . . ? N2 C6 C5 113.09(14) . . ? C7 C6 C5 126.59(17) . . ? C8 C7 C6 118.06(19) . . ? C9 C8 C7 121.07(18) . . ? C8 C9 C10 117.97(18) . . ? N2 C10 C9 120.33(18) . . ? N2 C10 C11 113.37(14) . . ? C9 C10 C11 126.26(17) . . ? N3 C11 C12 121.90(18) . . ? N3 C11 C10 114.14(15) . . ? C12 C11 C10 123.95(17) . . ? C13 C12 C11 118.69(19) . . ? C14 C13 C12 119.55(19) . . ? C13 C14 C15 118.7(2) . . ? N3 C15 C14 122.28(19) . . ? P2 C16 P1 111.35(9) . . ? _diffrn_measured_fraction_theta_max 0.942 _diffrn_reflns_theta_full 32.89 _diffrn_measured_fraction_theta_full 0.942 _refine_diff_density_max 0.541 _refine_diff_density_min -0.407 _refine_diff_density_rms 0.094 data_compound_3 _database_code_depnum_ccdc_archive 'CCDC 247952' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H26 Cu2 N6 O16 P2 V4' _chemical_formula_weight 1143.37 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 C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 18.7614(13) _cell_length_b 25.3542(17) _cell_length_c 16.1008(11) _cell_angle_alpha 90.00 _cell_angle_beta 99.4410(10) _cell_angle_gamma 90.00 _cell_volume 7555.1(9) _cell_formula_units_Z 8 _cell_measurement_temperature 90(2) _cell_measurement_reflns_used 12544 _cell_measurement_theta_min 1.74 _cell_measurement_theta_max 31.51 _exptl_crystal_description parallelpiped _exptl_crystal_colour blue _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.010 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4544 _exptl_absorpt_coefficient_mu 2.224 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4344 _exptl_absorpt_correction_T_max 0.8082 _exptl_absorpt_process_details 'SADABS SHELXL-97 (Sheldrick, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 90(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'APEX CCD area detector' _diffrn_measurement_method 'Phi and omega scans' _diffrn_detector_area_resol_mean '512 x 512' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.001 _diffrn_reflns_number 48324 _diffrn_reflns_av_R_equivalents 0.0451 _diffrn_reflns_av_sigmaI/netI 0.0409 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -36 _diffrn_reflns_limit_k_max 37 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.74 _diffrn_reflns_theta_max 31.51 _reflns_number_total 12544 _reflns_number_gt 10948 _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 6.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^)+(0.0573P)^2^+21.5737P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment refall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12544 _refine_ls_number_parameters 559 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0385 _refine_ls_R_factor_gt 0.0322 _refine_ls_wR_factor_ref 0.0887 _refine_ls_wR_factor_gt 0.0837 _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_restrained_S_all 1.041 _refine_ls_shift/su_max 0.002 _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 O16 O 0.22572(7) 0.10378(5) 0.63891(8) 0.0145(2) Uani 1 1 d . . . Cu1 Cu 0.413657(11) 0.126851(8) 0.808587(13) 0.00972(5) Uani 1 1 d . . . Cu2 Cu 0.089853(11) 0.128874(8) 0.951462(13) 0.00944(5) Uani 1 1 d . . . V1 V 0.257484(15) 0.080851(11) 0.896839(17) 0.00726(6) Uani 1 1 d . . . V2 V 0.331064(16) 0.122967(12) 1.252934(19) 0.01102(6) Uani 1 1 d . . . V3 V 0.241247(15) 0.055528(11) 1.376788(17) 0.00866(6) Uani 1 1 d . . . V4 V 0.197564(16) 0.136361(12) 1.533971(18) 0.01035(6) Uani 1 1 d . . . P1 P 0.27873(2) 0.069295(17) 0.69918(3) 0.00835(8) Uani 1 1 d . . . P2 P 0.22175(2) 0.087107(17) 1.08727(3) 0.00817(8) Uani 1 1 d . . . O1 O 0.35351(7) 0.09360(5) 0.71621(8) 0.0129(2) Uani 1 1 d . . . O2 O 0.24456(7) 0.05785(5) 0.77711(7) 0.0105(2) Uani 1 1 d . . . O3 O 0.33305(7) 0.11220(5) 0.89112(8) 0.0119(2) Uani 1 1 d . . . O4 O 0.24908(8) 0.00706(5) 0.91837(8) 0.0156(3) Uani 1 1 d . . . O5 O 0.27183(7) 0.08487(5) 1.02177(7) 0.0099(2) Uani 1 1 d . . . O6 O 0.18880(7) 0.12206(5) 0.88553(8) 0.0118(2) Uani 1 1 d . . . O7 O 0.14562(7) 0.10572(5) 1.05453(8) 0.0120(2) Uani 1 1 d . . . O8 O 0.25590(7) 0.12343(5) 1.16053(8) 0.0117(2) Uani 1 1 d . . . O9 O 0.40824(8) 0.11311(8) 1.22291(11) 0.0294(4) Uani 1 1 d . . . O10 O 0.33207(9) 0.17932(6) 1.30080(10) 0.0246(3) Uani 1 1 d . . . O11 O 0.31484(7) 0.06954(5) 1.32435(8) 0.0140(2) Uani 1 1 d . . . O12 O 0.16607(7) 0.06218(6) 1.31231(8) 0.0156(2) Uani 1 1 d . . . O13 O 0.24403(7) 0.10115(5) 1.46018(8) 0.0146(2) Uani 1 1 d . . . O14 O 0.22360(8) 0.19738(5) 1.54118(9) 0.0187(3) Uani 1 1 d . . . O15 O 0.11010(8) 0.13484(6) 1.50581(9) 0.0195(3) Uani 1 1 d . . . N1 N 0.39116(8) 0.20284(6) 0.77420(9) 0.0126(3) Uani 1 1 d . . . N2 N 0.49118(8) 0.16252(6) 0.88192(9) 0.0121(3) Uani 1 1 d . . . N3 N 0.47341(8) 0.06355(6) 0.85573(10) 0.0118(3) Uani 1 1 d . . . N4 N 0.10463(8) 0.20748(6) 0.97045(9) 0.0108(3) Uani 1 1 d . . . N5 N 0.00801(8) 0.15558(6) 0.87438(9) 0.0109(3) Uani 1 1 d . . . N6 N 0.04215(8) 0.05960(6) 0.90860(9) 0.0121(3) Uani 1 1 d . . . C1 C 0.33729(10) 0.21941(8) 0.71476(12) 0.0163(3) Uani 1 1 d . . . H1 H 0.3068 0.1940 0.6833 0.020 Uiso 1 1 calc R . . C2 C 0.32463(11) 0.27276(8) 0.69765(13) 0.0204(4) Uani 1 1 d . . . H2 H 0.2867 0.2837 0.6545 0.024 Uiso 1 1 calc R . . C3 C 0.36843(12) 0.30965(8) 0.74488(14) 0.0214(4) Uani 1 1 d . . . H3 H 0.3602 0.3463 0.7351 0.026 Uiso 1 1 calc R . . C4 C 0.42460(11) 0.29265(7) 0.80674(13) 0.0184(4) Uani 1 1 d . . . H4 H 0.4553 0.3174 0.8393 0.022 Uiso 1 1 calc R . . C5 C 0.43490(10) 0.23886(7) 0.81994(11) 0.0132(3) Uani 1 1 d . . . C6 C 0.49311(10) 0.21537(7) 0.88179(11) 0.0131(3) Uani 1 1 d . . . C7 C 0.54771(10) 0.24204(8) 0.93503(12) 0.0165(3) Uani 1 1 d . . . H7 H 0.5497 0.2795 0.9355 0.020 Uiso 1 1 calc R . . C8 C 0.59909(10) 0.21235(8) 0.98739(13) 0.0183(4) Uani 1 1 d . . . H8 H 0.6365 0.2297 1.0243 0.022 Uiso 1 1 calc R . . C9 C 0.59622(10) 0.15744(8) 0.98627(12) 0.0173(3) Uani 1 1 d . . . H9 H 0.6311 0.1371 1.0221 0.021 Uiso 1 1 calc R . . C10 C 0.54088(10) 0.13324(7) 0.93125(11) 0.0130(3) Uani 1 1 d . . . C11 C 0.53024(9) 0.07586(7) 0.91653(11) 0.0120(3) Uani 1 1 d . . . C12 C 0.57448(10) 0.03709(8) 0.95829(12) 0.0152(3) Uani 1 1 d . . . H12 H 0.6126 0.0462 1.0024 0.018 Uiso 1 1 calc R . . C13 C 0.56224(10) -0.01528(8) 0.93465(13) 0.0168(3) Uani 1 1 d . . . H13 H 0.5930 -0.0423 0.9613 0.020 Uiso 1 1 calc R . . C14 C 0.50473(10) -0.02788(8) 0.87180(12) 0.0166(3) Uani 1 1 d . . . H14 H 0.4957 -0.0634 0.8543 0.020 Uiso 1 1 calc R . . C15 C 0.46068(10) 0.01288(7) 0.83519(12) 0.0144(3) Uani 1 1 d . . . H15 H 0.4200 0.0044 0.7940 0.017 Uiso 1 1 calc R . . C16 C 0.15968(9) 0.23062(7) 1.02076(11) 0.0131(3) Uani 1 1 d . . . H16 H 0.1917 0.2095 1.0588 0.016 Uiso 1 1 calc R . . C17 C 0.17127(10) 0.28469(7) 1.01883(12) 0.0148(3) Uani 1 1 d . . . H17 H 0.2103 0.3004 1.0557 0.018 Uiso 1 1 calc R . . C18 C 0.12517(10) 0.31558(7) 0.96239(12) 0.0155(3) Uani 1 1 d . . . H18 H 0.1330 0.3525 0.9592 0.019 Uiso 1 1 calc R . . C19 C 0.06728(10) 0.29191(7) 0.91047(12) 0.0145(3) Uani 1 1 d . . . H19 H 0.0350 0.3123 0.8715 0.017 Uiso 1 1 calc R . . C20 C 0.05801(9) 0.23777(7) 0.91711(11) 0.0117(3) Uani 1 1 d . . . C21 C -0.00163(9) 0.20790(7) 0.86755(11) 0.0123(3) Uani 1 1 d . . . C22 C -0.06332(10) 0.22880(8) 0.81920(12) 0.0154(3) Uani 1 1 d . . . H22 H -0.0709 0.2658 0.8150 0.018 Uiso 1 1 calc R . . C23 C -0.11378(10) 0.19352(8) 0.77703(11) 0.0161(3) Uani 1 1 d . . . H23 H -0.1564 0.2066 0.7433 0.019 Uiso 1 1 calc R . . C24 C -0.10249(10) 0.13941(8) 0.78378(11) 0.0144(3) Uani 1 1 d . . . H24 H -0.1362 0.1153 0.7540 0.017 Uiso 1 1 calc R . . C25 C -0.04052(9) 0.12150(7) 0.83536(11) 0.0118(3) Uani 1 1 d . . . C26 C -0.02031(9) 0.06601(7) 0.85351(11) 0.0115(3) Uani 1 1 d . . . C27 C -0.06004(10) 0.02314(8) 0.81792(12) 0.0149(3) Uani 1 1 d . . . H27 H -0.1032 0.0283 0.7788 0.018 Uiso 1 1 calc R . . C28 C -0.03572(10) -0.02766(8) 0.84046(12) 0.0161(3) Uani 1 1 d . . . H28 H -0.0626 -0.0575 0.8175 0.019 Uiso 1 1 calc R . . C29 C 0.02801(10) -0.03422(8) 0.89663(12) 0.0165(3) Uani 1 1 d . . . H29 H 0.0456 -0.0685 0.9127 0.020 Uiso 1 1 calc R . . C30 C 0.06561(10) 0.01069(7) 0.92893(12) 0.0143(3) Uani 1 1 d . . . H30 H 0.1097 0.0064 0.9669 0.017 Uiso 1 1 calc R . . C31 C 0.28600(9) 0.00782(7) 0.64592(10) 0.0103(3) Uani 1 1 d . . . H31A H 0.3015 0.0148 0.5910 0.012 Uiso 1 1 calc R . . H31B H 0.3236 -0.0142 0.6799 0.012 Uiso 1 1 calc R . . C32 C 0.21476(9) 0.02249(7) 1.13117(11) 0.0105(3) Uani 1 1 d . . . H32A H 0.1969 0.0260 1.1854 0.013 Uiso 1 1 calc R . . H32B H 0.1787 0.0018 1.0926 0.013 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 O16 0.0183(6) 0.0130(6) 0.0114(6) 0.0030(4) 0.0002(5) 0.0057(5) Cu1 0.00978(10) 0.00850(9) 0.01050(10) -0.00094(7) 0.00051(7) -0.00136(7) Cu2 0.00847(9) 0.00857(9) 0.01027(10) -0.00122(7) -0.00145(7) -0.00014(7) V1 0.00827(12) 0.00629(11) 0.00685(12) -0.00012(9) 0.00014(9) 0.00009(9) V2 0.00949(13) 0.01187(13) 0.01112(13) 0.00101(10) -0.00008(10) -0.00186(10) V3 0.01164(13) 0.00681(12) 0.00717(12) 0.00020(9) 0.00047(9) 0.00018(9) V4 0.01308(13) 0.00901(12) 0.00842(12) 0.00054(9) 0.00015(10) 0.00228(10) P1 0.01027(18) 0.00729(17) 0.00714(17) -0.00027(13) 0.00035(13) 0.00030(14) P2 0.00945(18) 0.00741(17) 0.00705(17) -0.00002(13) -0.00040(13) 0.00007(13) O1 0.0137(6) 0.0132(6) 0.0119(5) -0.0025(4) 0.0021(4) -0.0045(5) O2 0.0129(5) 0.0106(5) 0.0079(5) -0.0014(4) 0.0018(4) -0.0013(4) O3 0.0131(6) 0.0134(6) 0.0092(5) -0.0018(4) 0.0023(4) -0.0034(4) O4 0.0276(7) 0.0073(5) 0.0119(6) -0.0003(4) 0.0036(5) -0.0014(5) O5 0.0108(5) 0.0102(5) 0.0086(5) 0.0007(4) 0.0007(4) -0.0005(4) O6 0.0126(6) 0.0136(6) 0.0088(5) 0.0004(4) 0.0007(4) 0.0040(4) O7 0.0109(5) 0.0142(6) 0.0103(5) 0.0013(4) 0.0001(4) 0.0019(4) O8 0.0149(6) 0.0106(5) 0.0084(5) -0.0013(4) -0.0016(4) -0.0001(4) O9 0.0148(7) 0.0432(10) 0.0317(9) 0.0180(8) 0.0083(6) 0.0069(7) O10 0.0313(8) 0.0157(7) 0.0228(7) -0.0038(6) -0.0079(6) -0.0058(6) O11 0.0145(6) 0.0145(6) 0.0132(6) 0.0026(5) 0.0036(4) -0.0002(5) O12 0.0136(6) 0.0182(6) 0.0138(6) 0.0008(5) -0.0011(5) 0.0006(5) O13 0.0190(6) 0.0118(6) 0.0132(6) -0.0038(4) 0.0030(5) -0.0001(5) O14 0.0295(8) 0.0092(6) 0.0174(6) -0.0003(5) 0.0040(5) 0.0011(5) O15 0.0151(6) 0.0245(7) 0.0173(6) 0.0004(5) -0.0015(5) 0.0034(5) N1 0.0147(7) 0.0109(6) 0.0124(6) -0.0009(5) 0.0023(5) -0.0018(5) N2 0.0118(6) 0.0119(7) 0.0126(6) -0.0022(5) 0.0014(5) -0.0012(5) N3 0.0100(6) 0.0122(6) 0.0128(6) -0.0009(5) 0.0009(5) -0.0006(5) N4 0.0100(6) 0.0096(6) 0.0122(6) -0.0012(5) -0.0002(5) 0.0011(5) N5 0.0077(6) 0.0137(7) 0.0107(6) -0.0004(5) -0.0005(5) -0.0003(5) N6 0.0100(6) 0.0128(7) 0.0128(6) -0.0026(5) -0.0003(5) -0.0014(5) C1 0.0170(8) 0.0146(8) 0.0167(8) 0.0013(6) 0.0009(6) 0.0016(6) C2 0.0225(9) 0.0159(9) 0.0226(9) 0.0040(7) 0.0030(7) 0.0050(7) C3 0.0271(10) 0.0109(8) 0.0278(10) 0.0026(7) 0.0090(8) 0.0037(7) C4 0.0214(9) 0.0102(8) 0.0246(9) -0.0020(7) 0.0072(7) -0.0016(6) C5 0.0151(8) 0.0102(7) 0.0150(8) -0.0012(6) 0.0045(6) -0.0021(6) C6 0.0131(7) 0.0123(7) 0.0145(8) -0.0026(6) 0.0042(6) -0.0024(6) C7 0.0153(8) 0.0152(8) 0.0195(9) -0.0060(7) 0.0039(6) -0.0048(6) C8 0.0142(8) 0.0214(9) 0.0190(9) -0.0079(7) 0.0015(6) -0.0052(7) C9 0.0116(8) 0.0216(9) 0.0175(8) -0.0042(7) -0.0011(6) -0.0012(7) C10 0.0109(7) 0.0143(8) 0.0136(7) -0.0025(6) 0.0017(6) -0.0014(6) C11 0.0082(7) 0.0145(8) 0.0135(7) -0.0011(6) 0.0022(6) -0.0007(6) C12 0.0102(7) 0.0188(8) 0.0163(8) 0.0004(6) 0.0015(6) 0.0014(6) C13 0.0130(8) 0.0170(8) 0.0209(9) 0.0044(7) 0.0040(6) 0.0041(6) C14 0.0167(8) 0.0130(8) 0.0203(9) 0.0005(7) 0.0039(7) 0.0016(6) C15 0.0136(8) 0.0133(8) 0.0157(8) -0.0007(6) 0.0007(6) -0.0002(6) C16 0.0111(7) 0.0134(8) 0.0142(8) -0.0031(6) -0.0001(6) -0.0006(6) C17 0.0137(8) 0.0134(8) 0.0172(8) -0.0038(6) 0.0018(6) -0.0015(6) C18 0.0178(8) 0.0117(8) 0.0173(8) -0.0011(6) 0.0038(6) -0.0018(6) C19 0.0171(8) 0.0115(7) 0.0147(8) 0.0014(6) 0.0018(6) 0.0006(6) C20 0.0118(7) 0.0108(7) 0.0124(7) -0.0004(6) 0.0015(6) 0.0007(6) C21 0.0109(7) 0.0134(7) 0.0121(7) 0.0004(6) 0.0006(6) 0.0009(6) C22 0.0133(8) 0.0185(8) 0.0134(8) 0.0015(6) -0.0005(6) 0.0023(6) C23 0.0113(7) 0.0234(9) 0.0123(8) 0.0032(6) -0.0015(6) 0.0023(7) C24 0.0109(7) 0.0218(9) 0.0098(7) 0.0003(6) 0.0001(6) -0.0018(6) C25 0.0087(7) 0.0159(8) 0.0105(7) -0.0010(6) 0.0012(5) -0.0020(6) C26 0.0084(7) 0.0161(8) 0.0100(7) -0.0016(6) 0.0012(5) -0.0024(6) C27 0.0120(7) 0.0170(8) 0.0157(8) -0.0024(6) 0.0018(6) -0.0050(6) C28 0.0133(8) 0.0169(8) 0.0185(8) -0.0050(7) 0.0036(6) -0.0041(6) C29 0.0157(8) 0.0127(8) 0.0215(9) -0.0041(6) 0.0040(7) -0.0026(6) C30 0.0128(7) 0.0130(8) 0.0165(8) -0.0020(6) 0.0007(6) 0.0000(6) C31 0.0107(7) 0.0095(7) 0.0106(7) -0.0018(5) 0.0012(5) -0.0009(5) C32 0.0111(7) 0.0086(7) 0.0113(7) 0.0017(5) 0.0007(5) -0.0003(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O16 P1 1.5422(13) . ? O16 V4 1.8770(13) 1_554 ? Cu1 O1 1.9094(13) . ? Cu1 N2 1.9402(15) . ? Cu1 N1 2.0297(16) . ? Cu1 N3 2.0321(15) . ? Cu1 O3 2.2023(13) . ? Cu2 O7 1.9035(12) . ? Cu2 N5 1.9318(15) . ? Cu2 N4 2.0285(15) . ? Cu2 N6 2.0395(15) . ? Cu2 O6 2.2911(13) . ? V1 O3 1.6410(13) . ? V1 O6 1.6457(13) . ? V1 O4 1.9141(13) . ? V1 O5 1.9878(12) . ? V1 O2 1.9903(12) . ? V2 O10 1.6220(16) . ? V2 O9 1.6194(16) . ? V2 O11 1.8343(13) . ? V2 O8 1.8745(13) . ? V3 O12 1.6171(14) . ? V3 O4 1.7192(13) 6_556 ? V3 O13 1.7666(13) . ? V3 O11 1.7686(13) . ? V4 O14 1.6208(14) . ? V4 O15 1.6297(15) . ? V4 O13 1.8188(13) . ? V4 O16 1.8770(13) 1_556 ? P1 O1 1.5157(13) . ? P1 O2 1.5276(13) . ? P1 C31 1.7949(17) . ? P2 O7 1.5145(13) . ? P2 O5 1.5241(13) . ? P2 O8 1.5499(13) . ? P2 C32 1.7977(17) . ? O4 V3 1.7190(13) 6 ? N1 C1 1.340(2) . ? N1 C5 1.361(2) . ? N2 C6 1.340(2) . ? N2 C10 1.345(2) . ? N3 C15 1.338(2) . ? N3 C11 1.360(2) . ? N4 C16 1.339(2) . ? N4 C20 1.359(2) . ? N5 C25 1.335(2) . ? N5 C21 1.341(2) . ? N6 C30 1.338(2) . ? N6 C26 1.358(2) . ? C1 C2 1.393(3) . ? C2 C3 1.387(3) . ? C3 C4 1.394(3) . ? C4 C5 1.389(3) . ? C5 C6 1.477(3) . ? C6 C7 1.398(2) . ? C7 C8 1.393(3) . ? C8 C9 1.393(3) . ? C9 C10 1.392(2) . ? C10 C11 1.482(2) . ? C11 C12 1.387(3) . ? C12 C13 1.390(3) . ? C13 C14 1.390(3) . ? C14 C15 1.392(3) . ? C16 C17 1.389(3) . ? C17 C18 1.389(3) . ? C18 C19 1.393(3) . ? C19 C20 1.390(2) . ? C20 C21 1.473(2) . ? C21 C22 1.390(2) . ? C22 C23 1.395(3) . ? C23 C24 1.390(3) . ? C24 C25 1.389(2) . ? C25 C26 1.474(3) . ? C26 C27 1.388(2) . ? C27 C28 1.394(3) . ? C28 C29 1.386(3) . ? C29 C30 1.394(3) . ? C31 C32 1.526(2) 6 ? C32 C31 1.526(2) 6_556 ? 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 P1 O16 V4 150.82(9) . 1_554 ? O1 Cu1 N2 165.50(6) . . ? O1 Cu1 N1 97.86(6) . . ? N2 Cu1 N1 79.93(6) . . ? O1 Cu1 N3 99.30(6) . . ? N2 Cu1 N3 80.11(6) . . ? N1 Cu1 N3 158.26(6) . . ? O1 Cu1 O3 91.09(5) . . ? N2 Cu1 O3 103.41(6) . . ? N1 Cu1 O3 101.07(6) . . ? N3 Cu1 O3 91.87(6) . . ? O7 Cu2 N5 158.99(6) . . ? O7 Cu2 N4 97.45(6) . . ? N5 Cu2 N4 80.04(6) . . ? O7 Cu2 N6 100.22(6) . . ? N5 Cu2 N6 79.98(6) . . ? N4 Cu2 N6 159.83(6) . . ? O7 Cu2 O6 90.54(5) . . ? N5 Cu2 O6 110.36(5) . . ? N4 Cu2 O6 92.46(5) . . ? N6 Cu2 O6 97.02(5) . . ? O3 V1 O6 110.75(7) . . ? O3 V1 O4 125.53(7) . . ? O6 V1 O4 123.67(7) . . ? O3 V1 O5 93.28(6) . . ? O6 V1 O5 93.04(6) . . ? O4 V1 O5 82.44(5) . . ? O3 V1 O2 93.25(6) . . ? O6 V1 O2 96.32(6) . . ? O4 V1 O2 83.59(5) . . ? O5 V1 O2 165.90(5) . . ? O10 V2 O9 109.66(10) . . ? O10 V2 O11 110.05(7) . . ? O9 V2 O11 108.76(7) . . ? O10 V2 O8 108.68(7) . . ? O9 V2 O8 110.93(8) . . ? O11 V2 O8 108.76(6) . . ? O12 V3 O4 110.86(7) . 6_556 ? O12 V3 O13 109.48(7) . . ? O4 V3 O13 108.57(6) 6_556 . ? O12 V3 O11 109.85(7) . . ? O4 V3 O11 110.35(7) 6_556 . ? O13 V3 O11 107.66(6) . . ? O14 V4 O15 108.69(8) . . ? O14 V4 O13 110.14(7) . . ? O15 V4 O13 112.04(7) . . ? O14 V4 O16 108.58(7) . 1_556 ? O15 V4 O16 111.22(7) . 1_556 ? O13 V4 O16 106.12(6) . 1_556 ? O1 P1 O2 115.42(7) . . ? O1 P1 O16 111.44(8) . . ? O2 P1 O16 108.08(7) . . ? O1 P1 C31 107.39(8) . . ? O2 P1 C31 107.61(7) . . ? O16 P1 C31 106.46(8) . . ? O7 P2 O5 115.08(7) . . ? O7 P2 O8 109.16(7) . . ? O5 P2 O8 108.90(7) . . ? O7 P2 C32 107.18(8) . . ? O5 P2 C32 109.34(8) . . ? O8 P2 C32 106.86(8) . . ? P1 O1 Cu1 137.03(8) . . ? P1 O2 V1 137.65(8) . . ? V1 O3 Cu1 143.19(7) . . ? V3 O4 V1 146.73(8) 6 . ? P2 O5 V1 134.88(8) . . ? V1 O6 Cu2 132.52(7) . . ? P2 O7 Cu2 138.74(8) . . ? P2 O8 V2 139.78(8) . . ? V3 O11 V2 132.10(8) . . ? V3 O13 V4 149.36(9) . . ? C1 N1 C5 119.55(16) . . ? C1 N1 Cu1 126.24(13) . . ? C5 N1 Cu1 114.17(12) . . ? C6 N2 C10 122.44(16) . . ? C6 N2 Cu1 118.87(13) . . ? C10 N2 Cu1 118.69(12) . . ? C15 N3 C11 119.02(16) . . ? C15 N3 Cu1 126.92(12) . . ? C11 N3 Cu1 114.01(12) . . ? C16 N4 C20 119.17(15) . . ? C16 N4 Cu2 126.48(12) . . ? C20 N4 Cu2 113.72(11) . . ? C25 N5 C21 121.96(15) . . ? C25 N5 Cu2 118.97(12) . . ? C21 N5 Cu2 118.80(12) . . ? C30 N6 C26 118.98(16) . . ? C30 N6 Cu2 127.35(12) . . ? C26 N6 Cu2 113.67(12) . . ? N1 C1 C2 121.99(18) . . ? C3 C2 C1 118.68(19) . . ? C4 C3 C2 119.59(18) . . ? C3 C4 C5 118.86(18) . . ? N1 C5 C4 121.32(18) . . ? N1 C5 C6 114.07(15) . . ? C4 C5 C6 124.61(17) . . ? N2 C6 C7 120.00(17) . . ? N2 C6 C5 112.76(16) . . ? C7 C6 C5 127.22(17) . . ? C8 C7 C6 118.33(18) . . ? C9 C8 C7 120.72(17) . . ? C10 C9 C8 118.15(18) . . ? N2 C10 C9 120.34(17) . . ? N2 C10 C11 112.66(15) . . ? C9 C10 C11 126.95(17) . . ? N3 C11 C12 121.50(17) . . ? N3 C11 C10 114.16(16) . . ? C12 C11 C10 124.32(16) . . ? C13 C12 C11 119.04(17) . . ? C12 C13 C14 119.51(17) . . ? C15 C14 C13 118.26(18) . . ? N3 C15 C14 122.58(17) . . ? N4 C16 C17 121.80(17) . . ? C16 C17 C18 119.21(17) . . ? C17 C18 C19 119.36(17) . . ? C18 C19 C20 118.31(17) . . ? N4 C20 C19 122.09(16) . . ? N4 C20 C21 113.88(15) . . ? C19 C20 C21 124.03(16) . . ? N5 C21 C22 120.79(17) . . ? N5 C21 C20 112.59(15) . . ? C22 C21 C20 126.61(17) . . ? C21 C22 C23 117.68(18) . . ? C24 C23 C22 120.82(17) . . ? C25 C24 C23 118.10(17) . . ? N5 C25 C24 120.59(17) . . ? N5 C25 C26 113.02(15) . . ? C24 C25 C26 126.38(16) . . ? N6 C26 C27 121.55(17) . . ? N6 C26 C25 114.21(15) . . ? C27 C26 C25 124.24(16) . . ? C26 C27 C28 119.05(17) . . ? C29 C28 C27 119.41(17) . . ? C28 C29 C30 118.37(18) . . ? N6 C30 C29 122.63(17) . . ? C32 C31 P1 112.24(12) 6 . ? C31 C32 P2 113.68(12) 6_556 . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 31.51 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.912 _refine_diff_density_min -0.764 _refine_diff_density_rms 0.112 data_compound_5 _database_code_depnum_ccdc_archive 'CCDC 247953' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H17 Cu N3 O10 P2 V2' _chemical_formula_weight 662.71 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 P21/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 9.0201(7) _cell_length_b 17.2200(14) _cell_length_c 14.8472(12) _cell_angle_alpha 90.00 _cell_angle_beta 99.985(2) _cell_angle_gamma 90.00 _cell_volume 2271.2(3) _cell_formula_units_Z 4 _cell_measurement_temperature 104(2) _cell_measurement_reflns_used 5636 _cell_measurement_theta_min 1.83 _cell_measurement_theta_max 28.32 _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.938 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1324 _exptl_absorpt_coefficient_mu 1.938 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7126 _exptl_absorpt_correction_T_max 0.9419 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 104(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'Phi and omega scans' _diffrn_detector_area_resol_mean '512 x 512' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.001 _diffrn_reflns_number 23582 _diffrn_reflns_av_R_equivalents 0.0197 _diffrn_reflns_av_sigmaI/netI 0.0172 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.83 _diffrn_reflns_theta_max 28.32 _reflns_number_total 5636 _reflns_number_gt 5331 _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 6.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^)+(0.0319P)^2^+2.0098P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment refall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5636 _refine_ls_number_parameters 320 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0246 _refine_ls_R_factor_gt 0.0231 _refine_ls_wR_factor_ref 0.0629 _refine_ls_wR_factor_gt 0.0621 _refine_ls_goodness_of_fit_ref 1.057 _refine_ls_restrained_S_all 1.057 _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 0.25933(2) 0.065345(11) 0.300824(12) 0.00926(5) Uani 1 1 d . . . V1 V 0.72765(3) -0.056077(15) 0.171503(19) 0.01121(6) Uani 1 1 d . . . V2 V 0.50495(3) -0.264632(15) 0.186440(17) 0.00902(6) Uani 1 1 d . . . P1 P 0.07101(4) -0.09177(2) -0.17549(3) 0.00909(8) Uani 1 1 d . . . P2 P 0.39151(4) -0.08744(2) 0.18638(3) 0.00922(8) Uani 1 1 d . . . O1 O -0.07089(12) -0.05022(7) -0.21780(8) 0.0123(2) Uani 1 1 d . . . O2 O 0.08112(13) -0.17615(6) -0.20935(8) 0.0131(2) Uani 1 1 d . . . O3 O 0.21288(13) -0.04804(7) -0.19367(8) 0.0129(2) Uani 1 1 d . . . O4 O 0.38278(13) -0.03642(7) 0.26640(8) 0.0139(2) Uani 1 1 d . . . O5 O 0.41639(13) -0.17361(6) 0.21727(8) 0.0131(2) Uani 1 1 d . . . O6 O 0.51964(12) -0.06379(7) 0.13367(8) 0.0130(2) Uani 1 1 d . . . O7 O 0.77716(14) -0.10425(7) 0.26520(9) 0.0189(2) Uani 1 1 d . . . O8 O 0.81495(14) -0.09098(7) 0.09387(9) 0.0205(3) Uani 1 1 d . . . O9 O 0.38215(13) -0.31583(7) 0.11941(8) 0.0171(2) Uani 1 1 d . . . O10 O 0.63752(13) -0.24455(7) 0.13002(8) 0.0154(2) Uani 1 1 d . . . N1 N 0.36093(15) 0.13903(8) 0.22320(9) 0.0118(2) Uani 1 1 d . . . N2 N 0.40105(14) 0.11620(8) 0.39561(9) 0.0102(2) Uiso 1 1 d . . . N3 N 0.20941(14) 0.00928(8) 0.41162(9) 0.0108(2) Uani 1 1 d . . . C1 C 0.11322(18) -0.04974(9) 0.41237(11) 0.0139(3) Uani 1 1 d . . . H1 H 0.0516 -0.0650 0.3567 0.017 Uiso 1 1 calc R . . C2 C 0.10083(19) -0.08937(10) 0.49228(12) 0.0167(3) Uani 1 1 d . . . H2 H 0.0307 -0.1306 0.4913 0.020 Uiso 1 1 calc R . . C3 C 0.1921(2) -0.06789(10) 0.57336(12) 0.0167(3) Uani 1 1 d . . . H3 H 0.1865 -0.0949 0.6285 0.020 Uiso 1 1 calc R . . C4 C 0.29217(18) -0.00642(9) 0.57336(11) 0.0139(3) Uani 1 1 d . . . H4 H 0.3555 0.0094 0.6282 0.017 Uiso 1 1 calc R . . C5 C 0.29710(17) 0.03114(9) 0.49129(10) 0.0110(3) Uani 1 1 d . . . C6 C 0.39748(17) 0.09749(9) 0.48258(11) 0.0113(3) Uani 1 1 d . . . C7 C 0.47935(19) 0.14021(10) 0.55382(11) 0.0157(3) Uani 1 1 d . . . H7 H 0.4796 0.1264 0.6158 0.019 Uiso 1 1 calc R . . C8 C 0.56064(19) 0.20366(10) 0.53133(12) 0.0176(3) Uani 1 1 d . . . H8 H 0.6175 0.2337 0.5788 0.021 Uiso 1 1 calc R . . C9 C 0.56031(18) 0.22404(10) 0.44045(11) 0.0154(3) Uani 1 1 d . . . H9 H 0.6144 0.2680 0.4250 0.018 Uiso 1 1 calc R . . C10 C 0.47775(17) 0.17747(9) 0.37308(11) 0.0115(3) Uani 1 1 d . . . C11 C 0.46313(17) 0.18711(9) 0.27269(11) 0.0123(3) Uani 1 1 d . . . C12 C 0.55007(19) 0.23801(10) 0.23176(12) 0.0172(3) Uani 1 1 d . . . H12 H 0.6184 0.2725 0.2676 0.021 Uiso 1 1 calc R . . C13 C 0.5351(2) 0.23746(11) 0.13678(12) 0.0202(4) Uani 1 1 d . . . H13 H 0.5951 0.2710 0.1071 0.024 Uiso 1 1 calc R . . C14 C 0.43256(19) 0.18801(11) 0.08585(12) 0.0194(3) Uani 1 1 d . . . H14 H 0.4210 0.1869 0.0210 0.023 Uiso 1 1 calc R . . C15 C 0.34665(18) 0.13989(10) 0.13200(11) 0.0151(3) Uani 1 1 d . . . H15 H 0.2750 0.1063 0.0973 0.018 Uiso 1 1 calc R . . C16 C 0.22100(17) -0.08369(10) 0.10414(10) 0.0130(3) Uani 1 1 d . . . H16A H 0.1432 -0.1134 0.1290 0.016 Uiso 1 1 calc R . . H16B H 0.1872 -0.0289 0.0985 0.016 Uiso 1 1 calc R . . C17 C 0.22593(17) -0.11430(10) 0.00802(10) 0.0136(3) Uani 1 1 d . . . H17A H 0.2393 -0.1714 0.0097 0.016 Uiso 1 1 calc R . . H17B H 0.3117 -0.0908 -0.0157 0.016 Uiso 1 1 calc R . . C18 C 0.07769(17) -0.09309(10) -0.05433(10) 0.0124(3) Uani 1 1 d . . . H18A H 0.0476 -0.0409 -0.0360 0.015 Uiso 1 1 calc R . . H18B H 0.0000 -0.1301 -0.0414 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 0.01017(9) 0.00990(9) 0.00721(9) 0.00032(6) 0.00013(7) -0.00129(6) V1 0.00987(12) 0.01044(13) 0.01331(13) -0.00196(9) 0.00202(9) -0.00080(9) V2 0.01009(12) 0.00798(12) 0.00886(12) 0.00047(9) 0.00129(9) 0.00013(9) P1 0.00962(17) 0.00941(18) 0.00778(17) -0.00140(13) 0.00021(13) -0.00028(13) P2 0.00963(17) 0.00934(17) 0.00818(17) -0.00054(13) 0.00013(13) 0.00139(13) O1 0.0115(5) 0.0133(5) 0.0109(5) -0.0011(4) -0.0015(4) 0.0011(4) O2 0.0164(5) 0.0100(5) 0.0120(5) -0.0021(4) 0.0004(4) -0.0008(4) O3 0.0118(5) 0.0120(5) 0.0153(5) -0.0020(4) 0.0031(4) -0.0024(4) O4 0.0167(5) 0.0135(5) 0.0104(5) -0.0026(4) -0.0010(4) 0.0041(4) O5 0.0170(5) 0.0098(5) 0.0131(5) 0.0009(4) 0.0042(4) 0.0026(4) O6 0.0106(5) 0.0156(5) 0.0124(5) 0.0016(4) 0.0011(4) -0.0018(4) O7 0.0198(6) 0.0162(6) 0.0189(6) 0.0013(5) -0.0020(5) 0.0017(5) O8 0.0186(6) 0.0188(6) 0.0266(7) -0.0077(5) 0.0108(5) -0.0039(5) O9 0.0164(6) 0.0163(6) 0.0176(6) -0.0019(5) -0.0001(4) -0.0039(5) O10 0.0145(5) 0.0172(6) 0.0153(5) 0.0024(4) 0.0046(4) 0.0001(4) N1 0.0120(6) 0.0123(6) 0.0111(6) 0.0010(5) 0.0014(5) 0.0005(5) N3 0.0118(6) 0.0105(6) 0.0098(6) 0.0004(5) 0.0016(5) 0.0010(5) C1 0.0142(7) 0.0132(7) 0.0142(7) -0.0019(6) 0.0022(6) -0.0014(6) C2 0.0193(8) 0.0129(7) 0.0190(8) 0.0005(6) 0.0060(6) -0.0031(6) C3 0.0232(8) 0.0148(8) 0.0136(7) 0.0022(6) 0.0076(6) 0.0006(6) C4 0.0177(7) 0.0145(7) 0.0096(7) -0.0001(6) 0.0023(6) 0.0023(6) C5 0.0113(7) 0.0105(7) 0.0110(7) -0.0008(5) 0.0018(5) 0.0018(5) C6 0.0108(7) 0.0116(7) 0.0112(7) 0.0005(5) 0.0012(5) 0.0018(5) C7 0.0177(8) 0.0178(8) 0.0105(7) -0.0010(6) -0.0005(6) -0.0012(6) C8 0.0171(8) 0.0186(8) 0.0157(8) -0.0053(6) -0.0010(6) -0.0041(6) C9 0.0135(7) 0.0141(7) 0.0181(8) -0.0019(6) 0.0017(6) -0.0034(6) C10 0.0103(7) 0.0115(7) 0.0124(7) 0.0006(5) 0.0017(5) 0.0012(5) C11 0.0109(7) 0.0125(7) 0.0129(7) 0.0013(6) 0.0008(5) 0.0018(5) C12 0.0141(7) 0.0165(8) 0.0199(8) 0.0050(6) 0.0002(6) -0.0026(6) C13 0.0161(8) 0.0245(9) 0.0204(8) 0.0110(7) 0.0043(6) -0.0010(7) C14 0.0181(8) 0.0268(9) 0.0138(8) 0.0067(7) 0.0041(6) 0.0025(7) C15 0.0150(7) 0.0180(8) 0.0120(7) 0.0017(6) 0.0012(6) 0.0007(6) C16 0.0104(7) 0.0181(8) 0.0094(7) -0.0028(6) -0.0009(5) 0.0018(6) C17 0.0129(7) 0.0174(8) 0.0096(7) -0.0018(6) -0.0003(5) 0.0038(6) C18 0.0113(7) 0.0172(7) 0.0083(7) -0.0009(5) 0.0007(5) 0.0016(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 O1 1.9365(11) 3 ? Cu1 N2 1.9385(13) . ? Cu1 N3 2.0243(13) . ? Cu1 N1 2.0358(13) . ? Cu1 O4 2.1839(11) . ? V1 O7 1.6147(13) . ? V1 O8 1.6201(12) . ? V1 O6 1.8676(12) . ? V1 O3 1.8839(12) 3_655 ? V2 O10 1.6121(12) . ? V2 O9 1.6162(12) . ? V2 O5 1.8524(11) . ? V2 O2 1.8808(11) 4_656 ? P1 O1 1.5053(11) . ? P1 O2 1.5454(12) . ? P1 O3 1.5483(12) . ? P1 C18 1.7895(15) . ? P2 O4 1.4907(12) . ? P2 O5 1.5578(12) . ? P2 O6 1.5581(12) . ? P2 C16 1.7914(16) . ? O1 Cu1 1.9366(11) 3 ? O2 V2 1.8808(11) 4 ? O3 V1 1.8839(12) 3_655 ? N1 C15 1.338(2) . ? N1 C11 1.356(2) . ? N2 C10 1.336(2) . ? N2 C6 1.337(2) . ? N3 C1 1.338(2) . ? N3 C5 1.357(2) . ? C1 C2 1.390(2) . ? C2 C3 1.386(2) . ? C3 C4 1.391(2) . ? C4 C5 1.387(2) . ? C5 C6 1.477(2) . ? C6 C7 1.391(2) . ? C7 C8 1.388(2) . ? C8 C9 1.394(2) . ? C9 C10 1.393(2) . ? C10 C11 1.483(2) . ? C11 C12 1.385(2) . ? C12 C13 1.393(2) . ? C13 C14 1.382(3) . ? C14 C15 1.393(2) . ? C16 C17 1.529(2) . ? C17 C18 1.533(2) . ? 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 156.70(5) 3 . ? O1 Cu1 N3 99.14(5) 3 . ? N2 Cu1 N3 80.63(5) . . ? O1 Cu1 N1 98.92(5) 3 . ? N2 Cu1 N1 79.89(5) . . ? N3 Cu1 N1 160.51(5) . . ? O1 Cu1 O4 99.79(5) 3 . ? N2 Cu1 O4 103.51(5) . . ? N3 Cu1 O4 90.10(5) . . ? N1 Cu1 O4 94.00(5) . . ? O7 V1 O8 109.05(7) . . ? O7 V1 O6 109.63(6) . . ? O8 V1 O6 110.28(6) . . ? O7 V1 O3 108.09(6) . 3_655 ? O8 V1 O3 108.58(6) . 3_655 ? O6 V1 O3 111.16(5) . 3_655 ? O10 V2 O9 106.74(6) . . ? O10 V2 O5 109.72(6) . . ? O9 V2 O5 109.56(6) . . ? O10 V2 O2 110.23(6) . 4_656 ? O9 V2 O2 108.93(6) . 4_656 ? O5 V2 O2 111.54(5) . 4_656 ? O1 P1 O2 113.89(6) . . ? O1 P1 O3 111.39(7) . . ? O2 P1 O3 107.66(6) . . ? O1 P1 C18 107.67(7) . . ? O2 P1 C18 108.75(7) . . ? O3 P1 C18 107.26(7) . . ? O4 P2 O5 110.58(7) . . ? O4 P2 O6 113.11(7) . . ? O5 P2 O6 108.38(6) . . ? O4 P2 C16 111.36(7) . . ? O5 P2 C16 107.33(7) . . ? O6 P2 C16 105.79(7) . . ? P1 O1 Cu1 142.25(7) . 3 ? P1 O2 V2 138.04(7) . 4 ? P1 O3 V1 130.64(7) . 3_655 ? P2 O4 Cu1 139.37(7) . . ? P2 O5 V2 141.22(7) . . ? P2 O6 V1 131.42(7) . . ? C15 N1 C11 118.60(14) . . ? C15 N1 Cu1 127.30(11) . . ? C11 N1 Cu1 113.83(10) . . ? C10 N2 C6 122.19(14) . . ? C10 N2 Cu1 118.69(11) . . ? C6 N2 Cu1 117.97(11) . . ? C1 N3 C5 118.97(14) . . ? C1 N3 Cu1 127.24(11) . . ? C5 N3 Cu1 113.44(10) . . ? N3 C1 C2 121.91(15) . . ? C3 C2 C1 119.12(15) . . ? C2 C3 C4 119.40(15) . . ? C5 C4 C3 118.34(15) . . ? N3 C5 C4 122.25(15) . . ? N3 C5 C6 114.31(13) . . ? C4 C5 C6 123.44(14) . . ? N2 C6 C7 120.57(15) . . ? N2 C6 C5 112.88(13) . . ? C7 C6 C5 126.52(14) . . ? C8 C7 C6 117.79(15) . . ? C7 C8 C9 121.23(15) . . ? C10 C9 C8 117.48(15) . . ? N2 C10 C9 120.70(15) . . ? N2 C10 C11 112.37(13) . . ? C9 C10 C11 126.93(14) . . ? N1 C11 C12 122.13(15) . . ? N1 C11 C10 114.20(13) . . ? C12 C11 C10 123.61(15) . . ? C11 C12 C13 118.48(16) . . ? C14 C13 C12 119.76(16) . . ? C13 C14 C15 118.29(16) . . ? N1 C15 C14 122.70(16) . . ? C17 C16 P2 117.59(11) . . ? C16 C17 C18 108.54(12) . . ? C17 C18 P1 118.94(11) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 28.32 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.546 _refine_diff_density_min -0.254 _refine_diff_density_rms 0.072 data_compound_6 _database_code_depnum_ccdc_archive 'CCDC 247954' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C19 H21 Cu N3 O13 P2 V3' _chemical_formula_weight 777.69 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 10.051(3) _cell_length_b 10.220(3) _cell_length_c 14.287(5) _cell_angle_alpha 88.698(6) _cell_angle_beta 76.678(6) _cell_angle_gamma 69.082(6) _cell_volume 1331.1(7) _cell_formula_units_Z 2 _cell_measurement_temperature 96(2) _cell_measurement_reflns_used 9037 _cell_measurement_theta_min 1.47 _cell_measurement_theta_max 32.81 _exptl_crystal_description needle _exptl_crystal_colour green _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.940 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 776 _exptl_absorpt_coefficient_mu 2.000 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7953 _exptl_absorpt_correction_T_max 0.9611 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 96(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'Phi and omega scans' _diffrn_detector_area_resol_mean '512 x 512' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.001 _diffrn_reflns_number 17857 _diffrn_reflns_av_R_equivalents 0.0335 _diffrn_reflns_av_sigmaI/netI 0.0578 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.47 _diffrn_reflns_theta_max 32.81 _reflns_number_total 9037 _reflns_number_gt 7117 _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 6.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^)+(0.0471P)^2^+0.6497P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment refall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9037 _refine_ls_number_parameters 394 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0609 _refine_ls_R_factor_gt 0.0436 _refine_ls_wR_factor_ref 0.1030 _refine_ls_wR_factor_gt 0.0940 _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 0.38404(3) 0.72243(3) 0.45302(2) 0.00987(7) Uani 1 1 d . . . V1 V 0.53902(6) 0.22934(6) 0.02166(4) 0.00774(15) Uani 0.7100(15) 1 d P . 1 V2 V 0.16469(5) 0.69941(4) 0.30575(3) 0.00945(8) Uani 1 1 d . . . V3 V -0.05620(5) 0.94105(4) -0.27591(3) 0.01018(9) Uani 1 1 d . . . V1A V 0.47421(15) 0.26249(14) -0.02363(10) 0.0075(4) Uani 0.2900(15) 1 d P . 2 P1 P 0.31334(7) 0.56526(6) 0.09744(4) 0.00834(11) Uani 1 1 d . . . P2 P -0.28872(7) 0.91441(7) -0.08755(5) 0.00924(12) Uani 1 1 d . . . O1 O 0.3097(2) 0.6725(2) 0.35228(14) 0.0155(4) Uani 1 1 d . . . O2 O 0.21328(19) 0.57432(18) 0.20022(12) 0.0104(3) Uani 1 1 d . . . O3 O -0.2034(2) 0.8962(2) -0.19467(13) 0.0149(4) Uani 1 1 d . . . O4 O 0.1967(2) 0.9180(2) 0.49833(14) 0.0145(4) Uani 1 1 d . . . H99 H 0.1269 0.9007 0.5343 0.022 Uiso 1 1 calc R . . O5 O 0.0957(2) 0.8736(2) 0.27097(15) 0.0222(4) Uani 1 1 d . . . O6 O 0.0387(2) 0.6707(2) 0.38608(14) 0.0170(4) Uani 1 1 d . . . O7 O 0.4359(2) 0.42318(18) 0.07905(14) 0.0143(4) Uani 1 1 d . . . O8 O -0.40038(19) 1.06237(18) -0.06638(13) 0.0120(3) Uani 1 1 d . . . O9 O 0.0995(2) 0.8632(2) -0.24909(15) 0.0189(4) Uani 1 1 d . . . O10 O -0.0449(2) 0.8872(2) -0.38657(13) 0.0153(4) Uani 1 1 d . . . O11 O 0.3667(2) 0.68847(18) 0.09081(13) 0.0126(3) Uani 1 1 d . . . O12 O 0.6453(3) 0.1716(3) 0.09248(18) 0.0130(5) Uani 0.7100(15) 1 d P . 1 O13 O -0.3543(2) 0.80032(19) -0.07162(15) 0.0192(4) Uani 1 1 d . . . O12A O 0.3642(7) 0.3123(7) -0.0934(5) 0.0163(13) Uani 0.2900(15) 1 d P . 2 N1 N 0.3100(2) 0.6214(2) 0.56519(16) 0.0124(4) Uani 1 1 d . . . N2 N 0.5111(2) 0.7247(2) 0.53575(15) 0.0108(4) Uani 1 1 d . . . N3 N 0.5102(2) 0.8142(2) 0.36738(16) 0.0122(4) Uani 1 1 d . . . C1 C 0.1990(3) 0.5736(3) 0.57464(19) 0.0141(5) Uani 1 1 d . . . H1 H 0.1506 0.5833 0.5237 0.017 Uiso 1 1 calc R . . C2 C 0.1536(3) 0.5106(3) 0.6571(2) 0.0184(5) Uani 1 1 d . . . H2 H 0.0748 0.4779 0.6626 0.022 Uiso 1 1 calc R . . C3 C 0.2246(3) 0.4964(3) 0.7307(2) 0.0193(5) Uani 1 1 d . . . H3 H 0.1958 0.4526 0.7871 0.023 Uiso 1 1 calc R . . C4 C 0.3384(3) 0.5460(3) 0.72235(19) 0.0169(5) Uani 1 1 d . . . H4 H 0.3882 0.5366 0.7725 0.020 Uiso 1 1 calc R . . C5 C 0.3775(3) 0.6094(2) 0.63919(18) 0.0119(4) Uani 1 1 d . . . C6 C 0.4937(3) 0.6700(3) 0.62201(18) 0.0119(4) Uani 1 1 d . . . C7 C 0.5818(3) 0.6726(3) 0.68349(19) 0.0156(5) Uani 1 1 d . . . H7 H 0.5679 0.6373 0.7457 0.019 Uiso 1 1 calc R . . C8 C 0.6907(3) 0.7283(3) 0.6515(2) 0.0179(5) Uani 1 1 d . . . H8 H 0.7531 0.7300 0.6920 0.021 Uiso 1 1 calc R . . C9 C 0.7095(3) 0.7819(3) 0.5606(2) 0.0155(5) Uani 1 1 d . . . H9 H 0.7853 0.8179 0.5379 0.019 Uiso 1 1 calc R . . C10 C 0.6142(3) 0.7809(3) 0.50460(18) 0.0119(4) Uani 1 1 d . . . C11 C 0.6114(3) 0.8360(3) 0.40783(18) 0.0114(4) Uani 1 1 d . . . C12 C 0.7005(3) 0.9061(3) 0.36134(19) 0.0158(5) Uani 1 1 d . . . H12 H 0.7717 0.9192 0.3899 0.019 Uiso 1 1 calc R . . C13 C 0.6836(3) 0.9570(3) 0.2716(2) 0.0188(5) Uani 1 1 d . . . H13 H 0.7426 1.0063 0.2385 0.023 Uiso 1 1 calc R . . C14 C 0.5800(3) 0.9350(3) 0.2315(2) 0.0191(5) Uani 1 1 d . . . H14 H 0.5667 0.9693 0.1706 0.023 Uiso 1 1 calc R . . C15 C 0.4959(3) 0.8625(3) 0.28103(19) 0.0162(5) Uani 1 1 d . . . H15 H 0.4257 0.8465 0.2529 0.019 Uiso 1 1 calc R . . C16 C 0.1968(3) 0.5854(3) 0.01644(19) 0.0148(5) Uani 1 1 d . . . H16A H 0.2554 0.5781 -0.0505 0.018 Uiso 1 1 calc R . . H16B H 0.1589 0.5077 0.0230 0.018 Uiso 1 1 calc R . . C17 C 0.0669(3) 0.7255(3) 0.0344(2) 0.0196(5) Uani 1 1 d . . . H17A H 0.0092 0.7333 0.1016 0.024 Uiso 1 1 calc R . . H17B H 0.1048 0.8032 0.0268 0.024 Uiso 1 1 calc R . . C18 C -0.0336(3) 0.7420(3) -0.0335(2) 0.0168(5) Uani 1 1 d . . . H18A H -0.0763 0.6677 -0.0237 0.020 Uiso 1 1 calc R . . H18B H 0.0242 0.7304 -0.1010 0.020 Uiso 1 1 calc R . . C19 C -0.1574(3) 0.8864(3) -0.0159(2) 0.0165(5) Uani 1 1 d . . . H19A H -0.1132 0.9593 -0.0286 0.020 Uiso 1 1 calc R . . H19B H -0.2097 0.8992 0.0530 0.020 Uiso 1 1 calc R . . H100 H 0.170(4) 0.965(4) 0.462(3) 0.029(11) 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 0.01026(14) 0.01151(14) 0.01037(14) 0.00135(10) -0.00405(11) -0.00598(11) V1 0.0087(3) 0.0055(2) 0.0094(3) 0.00120(19) -0.0022(2) -0.0031(2) V2 0.01060(19) 0.00890(18) 0.00982(18) -0.00070(14) -0.00218(15) -0.00475(15) V3 0.00973(18) 0.00854(18) 0.01106(19) 0.00028(14) -0.00155(15) -0.00244(15) V1A 0.0091(7) 0.0040(6) 0.0096(7) 0.0006(4) -0.0019(5) -0.0029(5) P1 0.0101(3) 0.0058(3) 0.0095(3) 0.0005(2) -0.0023(2) -0.0033(2) P2 0.0086(3) 0.0087(3) 0.0109(3) 0.0003(2) -0.0010(2) -0.0046(2) O1 0.0153(9) 0.0198(9) 0.0151(9) -0.0023(7) -0.0048(7) -0.0097(8) O2 0.0139(8) 0.0093(8) 0.0094(8) -0.0002(6) -0.0025(6) -0.0061(7) O3 0.0127(8) 0.0199(9) 0.0117(8) -0.0005(7) 0.0004(7) -0.0073(7) O4 0.0132(9) 0.0141(9) 0.0149(9) 0.0024(7) -0.0027(7) -0.0040(7) O5 0.0325(12) 0.0114(9) 0.0200(10) 0.0012(7) -0.0050(9) -0.0054(8) O6 0.0167(9) 0.0214(10) 0.0144(9) 0.0004(7) -0.0013(7) -0.0100(8) O7 0.0131(8) 0.0063(8) 0.0207(9) 0.0015(7) -0.0008(7) -0.0024(7) O8 0.0122(8) 0.0073(8) 0.0168(9) 0.0004(6) -0.0027(7) -0.0043(7) O9 0.0142(9) 0.0167(9) 0.0275(11) 0.0033(8) -0.0093(8) -0.0049(8) O10 0.0165(9) 0.0170(9) 0.0126(9) 0.0001(7) -0.0014(7) -0.0076(8) O11 0.0175(9) 0.0075(8) 0.0144(9) 0.0004(6) -0.0031(7) -0.0068(7) O12 0.0149(12) 0.0091(11) 0.0144(12) 0.0005(9) -0.0050(10) -0.0027(10) O13 0.0111(8) 0.0105(8) 0.0331(11) -0.0050(8) 0.0054(8) -0.0068(7) O12A 0.019(3) 0.013(3) 0.015(3) -0.001(2) -0.005(3) -0.003(3) N1 0.0124(10) 0.0100(9) 0.0142(10) -0.0007(7) -0.0022(8) -0.0038(8) N2 0.0114(9) 0.0107(9) 0.0110(9) 0.0016(7) -0.0039(8) -0.0040(8) N3 0.0104(9) 0.0146(10) 0.0132(10) 0.0024(8) -0.0045(8) -0.0056(8) C1 0.0149(11) 0.0115(11) 0.0179(12) 0.0008(9) -0.0039(10) -0.0070(9) C2 0.0179(13) 0.0152(12) 0.0228(14) 0.0039(10) -0.0024(11) -0.0083(10) C3 0.0219(14) 0.0186(13) 0.0172(13) 0.0052(10) -0.0017(11) -0.0090(11) C4 0.0197(13) 0.0163(12) 0.0139(12) 0.0047(9) -0.0045(10) -0.0056(10) C5 0.0120(11) 0.0077(10) 0.0145(11) 0.0013(8) -0.0027(9) -0.0020(9) C6 0.0140(11) 0.0098(11) 0.0108(11) 0.0006(8) -0.0041(9) -0.0022(9) C7 0.0217(13) 0.0130(11) 0.0134(12) 0.0036(9) -0.0080(10) -0.0055(10) C8 0.0223(13) 0.0164(12) 0.0206(13) 0.0016(10) -0.0143(11) -0.0079(11) C9 0.0171(12) 0.0139(12) 0.0196(13) 0.0011(9) -0.0093(10) -0.0073(10) C10 0.0118(11) 0.0101(10) 0.0155(12) 0.0004(9) -0.0059(9) -0.0042(9) C11 0.0112(11) 0.0107(11) 0.0133(11) 0.0014(8) -0.0042(9) -0.0045(9) C12 0.0159(12) 0.0195(13) 0.0168(12) 0.0012(10) -0.0042(10) -0.0120(11) C13 0.0174(13) 0.0241(14) 0.0200(13) 0.0061(11) -0.0056(10) -0.0130(11) C14 0.0188(13) 0.0279(15) 0.0166(13) 0.0096(11) -0.0072(10) -0.0139(12) C15 0.0145(12) 0.0228(13) 0.0154(12) 0.0055(10) -0.0079(10) -0.0092(10) C16 0.0181(12) 0.0158(12) 0.0139(12) 0.0017(9) -0.0072(10) -0.0079(10) C17 0.0172(13) 0.0222(14) 0.0199(13) 0.0010(11) -0.0113(11) -0.0036(11) C18 0.0177(12) 0.0156(12) 0.0202(13) 0.0033(10) -0.0101(10) -0.0065(10) C19 0.0166(12) 0.0152(12) 0.0168(12) -0.0016(9) -0.0075(10) -0.0025(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 O1 1.9213(19) . ? Cu1 N2 1.936(2) . ? Cu1 N3 2.016(2) . ? Cu1 N1 2.028(2) . ? Cu1 O4 2.184(2) . ? V1 O12 1.592(3) . ? V1 O13 1.956(2) 2_565 ? V1 O8 1.9666(19) 1_645 ? V1 O7 1.9715(19) . ? V1 O11 1.9978(19) 2_665 ? V2 O6 1.6086(19) . ? V2 O1 1.6717(19) . ? V2 O5 1.770(2) . ? V2 O2 1.8570(18) . ? V3 O9 1.613(2) . ? V3 O10 1.651(2) . ? V3 O5 1.791(2) 2_575 ? V3 O3 1.8482(19) . ? V1A O12A 1.600(7) . ? V1A O13 1.863(2) 2_565 ? V1A O11 1.890(2) 2_665 ? V1A O8 2.002(2) 1_645 ? V1A O7 2.096(2) . ? P1 O7 1.5120(19) . ? P1 O11 1.5281(18) . ? P1 O2 1.5606(19) . ? P1 C16 1.788(3) . ? P2 O8 1.5133(19) . ? P2 O13 1.5213(19) . ? P2 O3 1.551(2) . ? P2 C19 1.792(3) . ? O5 V3 1.791(2) 2_575 ? O8 V1 1.9666(19) 1_465 ? O8 V1A 2.002(2) 1_465 ? O11 V1A 1.890(2) 2_665 ? O11 V1 1.9979(19) 2_665 ? O13 V1A 1.863(2) 2_565 ? O13 V1 1.956(2) 2_565 ? N1 C1 1.348(3) . ? N1 C5 1.363(3) . ? N2 C6 1.342(3) . ? N2 C10 1.342(3) . ? N3 C15 1.338(3) . ? N3 C11 1.363(3) . ? C1 C2 1.393(4) . ? C2 C3 1.379(4) . ? C3 C4 1.388(4) . ? C4 C5 1.385(4) . ? C5 C6 1.478(4) . ? C6 C7 1.390(4) . ? C7 C8 1.391(4) . ? C8 C9 1.396(4) . ? C9 C10 1.385(3) . ? C10 C11 1.484(3) . ? C11 C12 1.385(3) . ? C12 C13 1.396(4) . ? C13 C14 1.383(4) . ? C14 C15 1.383(4) . ? C16 C17 1.533(4) . ? C17 C18 1.520(4) . ? C18 C19 1.533(4) . ? 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 162.53(9) . . ? O1 Cu1 N3 95.52(9) . . ? N2 Cu1 N3 80.52(9) . . ? O1 Cu1 N1 102.24(9) . . ? N2 Cu1 N1 79.96(9) . . ? N3 Cu1 N1 160.25(9) . . ? O1 Cu1 O4 94.03(8) . . ? N2 Cu1 O4 103.22(8) . . ? N3 Cu1 O4 94.60(8) . . ? N1 Cu1 O4 92.73(8) . . ? O12 V1 O13 110.29(12) . 2_565 ? O12 V1 O8 100.75(11) . 1_645 ? O13 V1 O8 87.42(8) 2_565 1_645 ? O12 V1 O7 98.76(11) . . ? O13 V1 O7 86.84(8) 2_565 . ? O8 V1 O7 160.46(8) 1_645 . ? O12 V1 O11 110.65(11) . 2_665 ? O13 V1 O11 139.06(9) 2_565 2_665 ? O8 V1 O11 85.50(8) 1_645 2_665 ? O7 V1 O11 86.65(8) . 2_665 ? O6 V2 O1 108.46(10) . . ? O6 V2 O5 109.16(10) . . ? O1 V2 O5 111.41(10) . . ? O6 V2 O2 107.55(9) . . ? O1 V2 O2 110.62(9) . . ? O5 V2 O2 109.54(9) . . ? O9 V3 O10 108.98(10) . . ? O9 V3 O5 108.67(10) . 2_575 ? O10 V3 O5 109.07(10) . 2_575 ? O9 V3 O3 111.21(10) . . ? O10 V3 O3 107.29(9) . . ? O5 V3 O3 111.56(9) 2_575 . ? O12A V1A O13 96.9(3) . 2_565 ? O12A V1A O11 101.6(3) . 2_665 ? O13 V1A O11 161.43(12) 2_565 2_665 ? O12A V1A O8 106.0(2) . 1_645 ? O13 V1A O8 89.01(9) 2_565 1_645 ? O11 V1A O8 87.44(9) 2_665 1_645 ? O12A V1A O7 111.4(2) . . ? O13 V1A O7 85.76(10) 2_565 . ? O11 V1A O7 86.02(9) 2_665 . ? O8 V1A O7 142.53(10) 1_645 . ? O7 P1 O11 113.75(11) . . ? O7 P1 O2 109.01(10) . . ? O11 P1 O2 108.35(10) . . ? O7 P1 C16 110.83(12) . . ? O11 P1 C16 109.19(11) . . ? O2 P1 C16 105.35(12) . . ? O8 P2 O13 114.31(11) . . ? O8 P2 O3 109.09(11) . . ? O13 P2 O3 107.07(11) . . ? O8 P2 C19 109.77(12) . . ? O13 P2 C19 109.29(13) . . ? O3 P2 C19 107.04(12) . . ? V2 O1 Cu1 147.01(12) . . ? P1 O2 V2 130.44(11) . . ? P2 O3 V3 141.36(12) . . ? V2 O5 V3 156.45(14) . 2_575 ? P1 O7 V1 155.07(13) . . ? P1 O7 V1A 127.74(12) . . ? V1 O7 V1A 28.02(5) . . ? P2 O8 V1 141.19(12) . 1_465 ? P2 O8 V1A 169.82(13) . 1_465 ? V1 O8 V1A 28.94(5) 1_465 1_465 ? P1 O11 V1A 139.98(12) . 2_665 ? P1 O11 V1 131.88(11) . 2_665 ? V1A O11 V1 29.40(5) 2_665 2_665 ? P2 O13 V1A 140.78(14) . 2_565 ? P2 O13 V1 142.40(12) . 2_565 ? V1A O13 V1 29.98(5) 2_565 2_565 ? C1 N1 C5 118.9(2) . . ? C1 N1 Cu1 126.74(18) . . ? C5 N1 Cu1 114.30(17) . . ? C6 N2 C10 122.2(2) . . ? C6 N2 Cu1 119.11(17) . . ? C10 N2 Cu1 118.69(17) . . ? C15 N3 C11 119.2(2) . . ? C15 N3 Cu1 126.52(18) . . ? C11 N3 Cu1 114.10(17) . . ? N1 C1 C2 121.7(3) . . ? C3 C2 C1 118.9(3) . . ? C2 C3 C4 120.0(3) . . ? C5 C4 C3 118.5(3) . . ? N1 C5 C4 122.0(2) . . ? N1 C5 C6 113.9(2) . . ? C4 C5 C6 124.1(2) . . ? N2 C6 C7 120.2(2) . . ? N2 C6 C5 112.6(2) . . ? C7 C6 C5 127.1(2) . . ? C6 C7 C8 118.2(2) . . ? C7 C8 C9 120.8(2) . . ? C10 C9 C8 118.0(2) . . ? N2 C10 C9 120.6(2) . . ? N2 C10 C11 112.5(2) . . ? C9 C10 C11 126.9(2) . . ? N3 C11 C12 121.6(2) . . ? N3 C11 C10 114.1(2) . . ? C12 C11 C10 124.3(2) . . ? C11 C12 C13 118.6(2) . . ? C14 C13 C12 119.3(2) . . ? C15 C14 C13 119.2(3) . . ? N3 C15 C14 122.1(2) . . ? C17 C16 P1 113.11(18) . . ? C18 C17 C16 113.2(2) . . ? C17 C18 C19 111.2(2) . . ? C18 C19 P2 115.20(19) . . ? _diffrn_measured_fraction_theta_max 0.913 _diffrn_reflns_theta_full 32.81 _diffrn_measured_fraction_theta_full 0.913 _refine_diff_density_max 0.784 _refine_diff_density_min -0.493 _refine_diff_density_rms 0.126 data_compound_7 _database_code_depnum_ccdc_archive 'CCDC 247955' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H22 Cu2 N6 O17 V6' _chemical_formula_weight 1171.26 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' 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 8.8569(6) _cell_length_b 10.7058(7) _cell_length_c 20.4918(14) _cell_angle_alpha 99.3440(10) _cell_angle_beta 98.7790(10) _cell_angle_gamma 94.0670(10) _cell_volume 1885.6(2) _cell_formula_units_Z 2 _cell_measurement_temperature 92(2) _cell_measurement_reflns_used 12232 _cell_measurement_theta_min 1.94 _cell_measurement_theta_max 31.51 _exptl_crystal_description parallepiped _exptl_crystal_colour green _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.063 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1152 _exptl_absorpt_coefficient_mu 2.608 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4218 _exptl_absorpt_correction_T_max 0.7805 _exptl_absorpt_process_details 'SADABS SHELXL-97 (Sheldrick, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 92(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'APEX CCD area detector' _diffrn_measurement_method 'Phi and omega scans' _diffrn_detector_area_resol_mean '512 x 512' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.001 _diffrn_reflns_number 24446 _diffrn_reflns_av_R_equivalents 0.0257 _diffrn_reflns_av_sigmaI/netI 0.0420 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 1.94 _diffrn_reflns_theta_max 31.51 _reflns_number_total 12232 _reflns_number_gt 9714 _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 6.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^)+(0.0504P)^2^+0.3365P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment refall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12232 _refine_ls_number_parameters 550 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0527 _refine_ls_R_factor_gt 0.0388 _refine_ls_wR_factor_ref 0.0993 _refine_ls_wR_factor_gt 0.0932 _refine_ls_goodness_of_fit_ref 1.027 _refine_ls_restrained_S_all 1.027 _refine_ls_shift/su_max 0.002 _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 0.85867(3) 0.78224(2) 1.075179(12) 0.00959(6) Uani 1 1 d . . . Cu2 Cu 0.84267(3) 0.27856(2) 0.567659(12) 0.01018(6) Uani 1 1 d . . . V1 V 0.65937(4) 1.17167(3) 1.273692(17) 0.01027(7) Uani 1 1 d . . . V2 V 0.77492(4) 1.09236(3) 1.126301(18) 0.01088(7) Uani 1 1 d . . . V3 V 0.91090(4) 0.76407(3) 0.926020(17) 0.01005(7) Uani 1 1 d . . . V4 V 0.67312(4) 0.69824(4) 0.776386(17) 0.01176(8) Uani 1 1 d . . . V5 V 0.78093(4) 0.59224(3) 0.634966(17) 0.01131(7) Uani 1 1 d . . . V6 V 0.90460(4) 0.26629(3) 0.419900(17) 0.01103(7) Uani 1 1 d . . . O1 O 0.6515(2) 1.02541(15) 1.28335(8) 0.0189(3) Uani 1 1 d . . . O2 O 0.75908(19) 1.26823(16) 1.34637(8) 0.0198(3) Uani 1 1 d . . . O3 O 0.7491(2) 1.18841(16) 1.20638(9) 0.0253(4) Uani 1 1 d . . . O4 O 0.90578(18) 1.18452(17) 1.08976(8) 0.0191(3) Uani 1 1 d . . . O5 O 0.6111(2) 1.06494(19) 1.07735(9) 0.0279(4) Uani 1 1 d . . . O6 O 0.8350(2) 0.95612(15) 1.14081(8) 0.0191(3) Uani 1 1 d . . . O7 O 0.86883(18) 0.85302(15) 0.99517(7) 0.0136(3) Uani 1 1 d . . . O8 O 0.9108(2) 0.61858(16) 0.93661(9) 0.0254(4) Uani 1 1 d . . . O9 O 0.7662(2) 0.77761(18) 0.85481(8) 0.0224(4) Uani 1 1 d . . . O10 O 0.5962(2) 0.56239(18) 0.78241(9) 0.0261(4) Uani 1 1 d . . . O11 O 0.5350(2) 0.79397(18) 0.74336(9) 0.0242(4) Uani 1 1 d . . . O12 O 0.80622(19) 0.67793(15) 0.72266(8) 0.0167(3) Uani 1 1 d . . . O13 O 0.6087(2) 0.60178(19) 0.59891(9) 0.0251(4) Uani 1 1 d . . . O14 O 0.8054(2) 0.44237(16) 0.63783(8) 0.0231(4) Uani 1 1 d . . . O15 O 0.84964(18) 0.34933(15) 0.48769(7) 0.0141(3) Uani 1 1 d . . . O16 O 0.9208(2) 0.12261(17) 0.43154(9) 0.0246(4) Uani 1 1 d . . . O17 O 1.0832(2) 0.33396(19) 0.40726(8) 0.0242(4) Uani 1 1 d . . . N1 N 0.6381(2) 0.70872(17) 1.05542(9) 0.0112(3) Uani 1 1 d . . . N2 N 0.8684(2) 0.65630(16) 1.13326(8) 0.0106(3) Uani 1 1 d . . . N3 N 1.0860(2) 0.80490(17) 1.11140(9) 0.0125(3) Uani 1 1 d . . . N4 N 0.6226(2) 0.20361(17) 0.54852(9) 0.0119(3) Uani 1 1 d . . . N5 N 0.8529(2) 0.15832(17) 0.62878(9) 0.0114(3) Uani 1 1 d . . . N6 N 1.0692(2) 0.30621(17) 0.60486(9) 0.0134(3) Uani 1 1 d . . . C1 C 0.5253(2) 0.7466(2) 1.01391(10) 0.0135(4) Uani 1 1 d . . . H1 H 0.5486 0.8132 0.9904 0.016 Uiso 1 1 calc R . . C2 C 0.3746(2) 0.6908(2) 1.00429(11) 0.0143(4) Uani 1 1 d . . . H2 H 0.2963 0.7185 0.9744 0.017 Uiso 1 1 calc R . . C3 C 0.3409(2) 0.5943(2) 1.03899(11) 0.0139(4) Uani 1 1 d . . . H3 H 0.2391 0.5546 1.0329 0.017 Uiso 1 1 calc R . . C4 C 0.4574(2) 0.5562(2) 1.08287(10) 0.0133(4) Uani 1 1 d . . . H4 H 0.4362 0.4913 1.1077 0.016 Uiso 1 1 calc R . . C5 C 0.6053(2) 0.61467(19) 1.08960(10) 0.0109(4) Uani 1 1 d . . . C6 C 0.7409(2) 0.58210(19) 1.13357(10) 0.0107(4) Uani 1 1 d . . . C7 C 0.7460(3) 0.4862(2) 1.17211(11) 0.0151(4) Uani 1 1 d . . . H7 H 0.6565 0.4319 1.1723 0.018 Uiso 1 1 calc R . . C8 C 0.8857(3) 0.4720(2) 1.21029(11) 0.0173(4) Uani 1 1 d . . . H8 H 0.8915 0.4078 1.2374 0.021 Uiso 1 1 calc R . . C9 C 1.0174(3) 0.5506(2) 1.20933(11) 0.0152(4) Uani 1 1 d . . . H9 H 1.1128 0.5418 1.2356 0.018 Uiso 1 1 calc R . . C10 C 1.0043(2) 0.6428(2) 1.16845(10) 0.0114(4) Uani 1 1 d . . . C11 C 1.1290(2) 0.7336(2) 1.15858(11) 0.0129(4) Uani 1 1 d . . . C12 C 1.2772(3) 0.7477(2) 1.19415(12) 0.0180(4) Uani 1 1 d . . . H12 H 1.3063 0.6955 1.2263 0.022 Uiso 1 1 calc R . . C13 C 1.3823(3) 0.8402(2) 1.18164(13) 0.0217(5) Uani 1 1 d . . . H13 H 1.4842 0.8525 1.2058 0.026 Uiso 1 1 calc R . . C14 C 1.3381(3) 0.9139(2) 1.13403(12) 0.0200(5) Uani 1 1 d . . . H14 H 1.4085 0.9775 1.1250 0.024 Uiso 1 1 calc R . . C15 C 1.1878(3) 0.8929(2) 1.09949(11) 0.0154(4) Uani 1 1 d . . . H15 H 1.1568 0.9428 1.0664 0.019 Uiso 1 1 calc R . . C16 C 0.5095(2) 0.2391(2) 0.50615(11) 0.0142(4) Uani 1 1 d . . . H16 H 0.5332 0.3023 0.4807 0.017 Uiso 1 1 calc R . . C17 C 0.3582(3) 0.1861(2) 0.49840(11) 0.0151(4) Uani 1 1 d . . . H17 H 0.2797 0.2124 0.4680 0.018 Uiso 1 1 calc R . . C18 C 0.3245(3) 0.0940(2) 0.53589(11) 0.0154(4) Uani 1 1 d . . . H18 H 0.2224 0.0558 0.5312 0.019 Uiso 1 1 calc R . . C19 C 0.4417(2) 0.0583(2) 0.58049(11) 0.0146(4) Uani 1 1 d . . . H19 H 0.4205 -0.0038 0.6070 0.018 Uiso 1 1 calc R . . C20 C 0.5891(2) 0.1145(2) 0.58556(10) 0.0123(4) Uani 1 1 d . . . C21 C 0.7251(2) 0.0858(2) 0.63109(10) 0.0124(4) Uani 1 1 d . . . C22 C 0.7298(3) -0.0035(2) 0.67325(11) 0.0166(4) Uani 1 1 d . . . H22 H 0.6406 -0.0569 0.6748 0.020 Uiso 1 1 calc R . . C23 C 0.8693(3) -0.0124(2) 0.71324(11) 0.0184(4) Uani 1 1 d . . . H23 H 0.8749 -0.0723 0.7428 0.022 Uiso 1 1 calc R . . C24 C 1.0004(3) 0.0649(2) 0.71069(11) 0.0159(4) Uani 1 1 d . . . H24 H 1.0952 0.0596 0.7385 0.019 Uiso 1 1 calc R . . C25 C 0.9884(2) 0.1501(2) 0.66618(10) 0.0125(4) Uani 1 1 d . . . C26 C 1.1118(2) 0.2399(2) 0.65458(11) 0.0135(4) Uani 1 1 d . . . C27 C 1.2593(3) 0.2595(2) 0.69159(12) 0.0176(4) Uani 1 1 d . . . H27 H 1.2882 0.2116 0.7259 0.021 Uiso 1 1 calc R . . C28 C 1.3634(3) 0.3505(2) 0.67735(13) 0.0219(5) Uani 1 1 d . . . H28 H 1.4647 0.3656 0.7021 0.026 Uiso 1 1 calc R . . C29 C 1.3197(3) 0.4189(2) 0.62718(12) 0.0195(5) Uani 1 1 d . . . H29 H 1.3895 0.4820 0.6173 0.023 Uiso 1 1 calc R . . C30 C 1.1705(3) 0.3933(2) 0.59136(11) 0.0163(4) Uani 1 1 d . . . H30 H 1.1399 0.4390 0.5563 0.020 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 0.01083(12) 0.00872(12) 0.01002(12) 0.00265(9) 0.00308(9) 0.00119(9) Cu2 0.01215(12) 0.00887(12) 0.01041(12) 0.00302(9) 0.00328(9) 0.00099(9) V1 0.01190(16) 0.01026(16) 0.00894(15) 0.00096(12) 0.00279(12) 0.00257(12) V2 0.01101(16) 0.01074(16) 0.01209(16) 0.00295(13) 0.00423(12) 0.00194(12) V3 0.01140(16) 0.00983(16) 0.00935(15) 0.00141(12) 0.00400(12) -0.00041(12) V4 0.01146(16) 0.01480(17) 0.00875(15) 0.00069(13) 0.00169(12) 0.00253(13) V5 0.01145(16) 0.01221(17) 0.01108(16) 0.00280(13) 0.00365(12) 0.00118(13) V6 0.01275(17) 0.01034(16) 0.01027(15) 0.00190(12) 0.00329(12) -0.00032(13) O1 0.0238(9) 0.0155(8) 0.0179(8) 0.0050(6) 0.0039(6) -0.0004(7) O2 0.0218(8) 0.0176(8) 0.0164(8) -0.0029(6) -0.0021(6) 0.0024(7) O3 0.0444(11) 0.0117(8) 0.0252(9) 0.0010(7) 0.0253(8) 0.0013(7) O4 0.0158(8) 0.0248(9) 0.0183(8) 0.0044(7) 0.0091(6) -0.0020(7) O5 0.0156(8) 0.0361(11) 0.0346(10) 0.0217(9) -0.0023(7) -0.0024(7) O6 0.0318(9) 0.0142(8) 0.0128(7) 0.0020(6) 0.0044(7) 0.0115(7) O7 0.0170(7) 0.0144(7) 0.0102(7) 0.0028(6) 0.0047(6) 0.0013(6) O8 0.0391(11) 0.0126(8) 0.0283(9) 0.0052(7) 0.0160(8) 0.0031(7) O9 0.0196(8) 0.0297(10) 0.0144(8) -0.0041(7) -0.0013(6) 0.0066(7) O10 0.0315(10) 0.0252(9) 0.0217(9) 0.0063(7) 0.0080(7) -0.0090(8) O11 0.0212(9) 0.0288(9) 0.0218(8) 0.0017(7) -0.0004(7) 0.0113(7) O12 0.0219(8) 0.0133(7) 0.0159(7) 0.0005(6) 0.0086(6) 0.0012(6) O13 0.0158(8) 0.0350(10) 0.0275(9) 0.0176(8) 0.0005(7) 0.0006(7) O14 0.0412(11) 0.0140(8) 0.0143(8) -0.0005(6) 0.0047(7) 0.0098(7) O15 0.0176(8) 0.0136(7) 0.0121(7) 0.0027(6) 0.0052(6) 0.0024(6) O16 0.0369(11) 0.0152(8) 0.0247(9) 0.0060(7) 0.0092(8) 0.0074(7) O17 0.0190(8) 0.0379(11) 0.0157(8) 0.0044(7) 0.0074(6) -0.0076(8) N1 0.0117(8) 0.0116(8) 0.0114(8) 0.0039(6) 0.0032(6) 0.0016(6) N2 0.0115(8) 0.0102(8) 0.0107(8) 0.0026(6) 0.0022(6) 0.0017(6) N3 0.0130(8) 0.0109(8) 0.0136(8) 0.0004(6) 0.0039(6) 0.0014(6) N4 0.0135(8) 0.0119(8) 0.0116(8) 0.0040(6) 0.0036(6) 0.0013(6) N5 0.0134(8) 0.0095(8) 0.0114(8) 0.0010(6) 0.0032(6) 0.0017(6) N6 0.0154(9) 0.0099(8) 0.0151(8) 0.0017(7) 0.0040(7) 0.0014(7) C1 0.0159(10) 0.0128(9) 0.0132(9) 0.0049(8) 0.0030(8) 0.0035(8) C2 0.0148(10) 0.0156(10) 0.0132(9) 0.0035(8) 0.0026(8) 0.0029(8) C3 0.0132(10) 0.0141(10) 0.0144(9) 0.0013(8) 0.0038(8) 0.0010(8) C4 0.0148(10) 0.0132(10) 0.0134(9) 0.0032(8) 0.0061(8) 0.0018(8) C5 0.0116(9) 0.0100(9) 0.0118(9) 0.0021(7) 0.0037(7) 0.0015(7) C6 0.0132(9) 0.0093(9) 0.0101(8) 0.0017(7) 0.0032(7) 0.0011(7) C7 0.0176(10) 0.0135(10) 0.0156(10) 0.0055(8) 0.0044(8) 0.0020(8) C8 0.0243(12) 0.0130(10) 0.0162(10) 0.0067(8) 0.0038(8) 0.0035(8) C9 0.0178(10) 0.0133(10) 0.0149(10) 0.0038(8) 0.0009(8) 0.0046(8) C10 0.0123(9) 0.0111(9) 0.0111(9) 0.0012(7) 0.0030(7) 0.0027(7) C11 0.0137(10) 0.0097(9) 0.0152(9) 0.0004(7) 0.0028(8) 0.0029(7) C12 0.0176(11) 0.0159(10) 0.0184(10) 0.0009(8) -0.0013(8) 0.0024(8) C13 0.0140(11) 0.0205(11) 0.0267(12) -0.0040(9) 0.0006(9) 0.0007(9) C14 0.0165(11) 0.0152(11) 0.0264(12) -0.0019(9) 0.0051(9) -0.0027(8) C15 0.0163(10) 0.0119(10) 0.0185(10) 0.0007(8) 0.0062(8) 0.0010(8) C16 0.0154(10) 0.0128(9) 0.0162(10) 0.0055(8) 0.0042(8) 0.0034(8) C17 0.0147(10) 0.0157(10) 0.0156(10) 0.0031(8) 0.0036(8) 0.0032(8) C18 0.0146(10) 0.0141(10) 0.0177(10) 0.0010(8) 0.0049(8) 0.0011(8) C19 0.0157(10) 0.0139(10) 0.0146(10) 0.0010(8) 0.0059(8) -0.0007(8) C20 0.0155(10) 0.0113(9) 0.0109(9) 0.0020(7) 0.0041(7) 0.0020(7) C21 0.0164(10) 0.0112(9) 0.0099(9) 0.0017(7) 0.0035(7) 0.0018(7) C22 0.0198(11) 0.0151(10) 0.0165(10) 0.0063(8) 0.0051(8) 0.0009(8) C23 0.0239(12) 0.0195(11) 0.0148(10) 0.0103(9) 0.0044(9) 0.0032(9) C24 0.0191(11) 0.0149(10) 0.0139(10) 0.0031(8) 0.0016(8) 0.0055(8) C25 0.0154(10) 0.0110(9) 0.0110(9) 0.0003(7) 0.0025(7) 0.0031(7) C26 0.0142(10) 0.0112(9) 0.0150(9) 0.0009(8) 0.0036(8) 0.0028(7) C27 0.0178(11) 0.0131(10) 0.0196(11) -0.0004(8) -0.0008(8) 0.0025(8) C28 0.0183(11) 0.0167(11) 0.0273(12) -0.0015(9) -0.0007(9) 0.0015(9) C29 0.0168(11) 0.0129(10) 0.0280(12) 0.0001(9) 0.0058(9) -0.0011(8) C30 0.0197(11) 0.0105(9) 0.0186(10) 0.0017(8) 0.0052(8) -0.0007(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 O7 1.9259(15) . ? Cu1 N2 1.9359(17) . ? Cu1 N1 2.0091(18) . ? Cu1 N3 2.0200(18) . ? Cu1 O6 2.1556(16) . ? Cu2 O15 1.9211(15) . ? Cu2 N5 1.9337(18) . ? Cu2 N4 2.0100(18) . ? Cu2 N6 2.0171(19) . ? Cu2 O14 2.1589(17) . ? V1 O1 1.6078(17) . ? V1 O3 1.7207(17) . ? V1 O2 1.7424(16) . ? V1 O11 1.7801(17) 2_677 ? V2 O5 1.6113(18) . ? V2 O6 1.6436(16) . ? V2 O4 1.7945(16) . ? V2 O3 1.8445(17) . ? V3 O8 1.6071(18) . ? V3 O7 1.6813(15) . ? V3 O4 1.7705(16) 2_777 ? V3 O9 1.8212(17) . ? V4 O10 1.5930(18) . ? V4 O12 1.7332(16) . ? V4 O9 1.7427(17) . ? V4 O11 1.7762(17) . ? V5 O13 1.6078(17) . ? V5 O14 1.6434(17) . ? V5 O17 1.7963(17) 2_766 ? V5 O12 1.8529(16) . ? V6 O16 1.6073(18) . ? V6 O15 1.6804(16) . ? V6 O17 1.7653(17) . ? V6 O2 1.8311(16) 1_544 ? O2 V6 1.8313(16) 1_566 ? O4 V3 1.7705(16) 2_777 ? O11 V1 1.7801(17) 2_677 ? O17 V5 1.7963(17) 2_766 ? N1 C1 1.340(3) . ? N1 C5 1.356(3) . ? N2 C10 1.336(3) . ? N2 C6 1.335(3) . ? N3 C15 1.334(3) . ? N3 C11 1.353(3) . ? N4 C16 1.340(3) . ? N4 C20 1.356(3) . ? N5 C25 1.338(3) . ? N5 C21 1.338(3) . ? N6 C30 1.338(3) . ? N6 C26 1.356(3) . ? C1 C2 1.395(3) . ? C2 C3 1.386(3) . ? C3 C4 1.392(3) . ? C4 C5 1.388(3) . ? C5 C6 1.486(3) . ? C6 C7 1.393(3) . ? C7 C8 1.391(3) . ? C8 C9 1.394(3) . ? C9 C10 1.394(3) . ? C10 C11 1.478(3) . ? C11 C12 1.386(3) . ? C12 C13 1.392(3) . ? C13 C14 1.380(4) . ? C14 C15 1.393(3) . ? C16 C17 1.393(3) . ? C17 C18 1.387(3) . ? C18 C19 1.393(3) . ? C19 C20 1.380(3) . ? C20 C21 1.490(3) . ? C21 C22 1.387(3) . ? C22 C23 1.393(3) . ? C23 C24 1.390(3) . ? C24 C25 1.389(3) . ? C25 C26 1.476(3) . ? C26 C27 1.390(3) . ? C27 C28 1.390(3) . ? C28 C29 1.381(3) . ? C29 C30 1.396(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 O7 Cu1 N2 158.18(7) . . ? O7 Cu1 N1 99.54(7) . . ? N2 Cu1 N1 80.33(7) . . ? O7 Cu1 N3 97.31(7) . . ? N2 Cu1 N3 80.28(7) . . ? N1 Cu1 N3 160.37(7) . . ? O7 Cu1 O6 97.68(6) . . ? N2 Cu1 O6 103.91(7) . . ? N1 Cu1 O6 98.92(7) . . ? N3 Cu1 O6 88.71(7) . . ? O15 Cu2 N5 160.74(7) . . ? O15 Cu2 N4 99.34(7) . . ? N5 Cu2 N4 80.36(7) . . ? O15 Cu2 N6 97.87(7) . . ? N5 Cu2 N6 80.52(7) . . ? N4 Cu2 N6 160.71(7) . . ? O15 Cu2 O14 101.75(7) . . ? N5 Cu2 O14 97.45(7) . . ? N4 Cu2 O14 95.24(7) . . ? N6 Cu2 O14 89.71(7) . . ? O1 V1 O3 109.31(8) . . ? O1 V1 O2 109.77(8) . . ? O3 V1 O2 110.37(9) . . ? O1 V1 O11 105.55(9) . 2_677 ? O3 V1 O11 109.97(9) . 2_677 ? O2 V1 O11 111.74(8) . 2_677 ? O5 V2 O6 108.87(10) . . ? O5 V2 O4 109.34(8) . . ? O6 V2 O4 113.57(9) . . ? O5 V2 O3 108.46(10) . . ? O6 V2 O3 108.86(8) . . ? O4 V2 O3 107.63(8) . . ? O8 V3 O7 108.98(8) . . ? O8 V3 O4 108.55(9) . 2_777 ? O7 V3 O4 111.27(8) . 2_777 ? O8 V3 O9 110.28(10) . . ? O7 V3 O9 108.58(8) . . ? O4 V3 O9 109.18(8) 2_777 . ? O10 V4 O12 109.10(9) . . ? O10 V4 O9 110.21(9) . . ? O12 V4 O9 108.98(8) . . ? O10 V4 O11 111.68(10) . . ? O12 V4 O11 107.95(8) . . ? O9 V4 O11 108.86(8) . . ? O13 V5 O14 109.17(10) . . ? O13 V5 O17 110.17(9) . 2_766 ? O14 V5 O17 112.89(10) . 2_766 ? O13 V5 O12 108.68(9) . . ? O14 V5 O12 107.36(8) . . ? O17 V5 O12 108.45(8) 2_766 . ? O16 V6 O15 108.75(8) . . ? O16 V6 O17 109.10(10) . . ? O15 V6 O17 110.54(8) . . ? O16 V6 O2 110.16(9) . 1_544 ? O15 V6 O2 108.79(8) . 1_544 ? O17 V6 O2 109.49(8) . 1_544 ? V1 O2 V6 142.28(10) . 1_566 ? V1 O3 V2 138.60(10) . . ? V3 O4 V2 154.58(11) 2_777 . ? V2 O6 Cu1 132.42(9) . . ? V3 O7 Cu1 120.73(9) . . ? V4 O9 V3 143.41(11) . . ? V4 O11 V1 149.77(13) . 2_677 ? V4 O12 V5 129.56(10) . . ? V5 O14 Cu2 136.00(10) . . ? V6 O15 Cu2 121.36(9) . . ? V6 O17 V5 158.05(11) . 2_766 ? C1 N1 C5 119.44(19) . . ? C1 N1 Cu1 125.93(15) . . ? C5 N1 Cu1 114.61(14) . . ? C10 N2 C6 122.83(18) . . ? C10 N2 Cu1 118.42(14) . . ? C6 N2 Cu1 118.64(14) . . ? C15 N3 C11 119.38(19) . . ? C15 N3 Cu1 125.92(15) . . ? C11 N3 Cu1 114.06(14) . . ? C16 N4 C20 119.28(19) . . ? C16 N4 Cu2 125.80(15) . . ? C20 N4 Cu2 114.81(14) . . ? C25 N5 C21 122.94(18) . . ? C25 N5 Cu2 118.38(15) . . ? C21 N5 Cu2 118.67(14) . . ? C30 N6 C26 119.49(19) . . ? C30 N6 Cu2 126.14(15) . . ? C26 N6 Cu2 113.72(14) . . ? N1 C1 C2 121.7(2) . . ? C3 C2 C1 119.0(2) . . ? C2 C3 C4 119.4(2) . . ? C5 C4 C3 118.7(2) . . ? N1 C5 C4 121.75(19) . . ? N1 C5 C6 113.73(18) . . ? C4 C5 C6 124.52(19) . . ? N2 C6 C7 120.00(19) . . ? N2 C6 C5 112.61(17) . . ? C7 C6 C5 127.39(19) . . ? C8 C7 C6 118.2(2) . . ? C7 C8 C9 120.9(2) . . ? C8 C9 C10 117.7(2) . . ? N2 C10 C9 120.3(2) . . ? N2 C10 C11 112.88(18) . . ? C9 C10 C11 126.79(19) . . ? N3 C11 C12 121.7(2) . . ? N3 C11 C10 114.00(18) . . ? C12 C11 C10 124.3(2) . . ? C11 C12 C13 118.5(2) . . ? C14 C13 C12 119.8(2) . . ? C13 C14 C15 118.5(2) . . ? N3 C15 C14 122.1(2) . . ? N4 C16 C17 121.9(2) . . ? C18 C17 C16 118.7(2) . . ? C17 C18 C19 119.3(2) . . ? C20 C19 C18 118.9(2) . . ? N4 C20 C19 121.8(2) . . ? N4 C20 C21 113.45(18) . . ? C19 C20 C21 124.75(19) . . ? N5 C21 C22 120.0(2) . . ? N5 C21 C20 112.65(18) . . ? C22 C21 C20 127.4(2) . . ? C21 C22 C23 118.0(2) . . ? C24 C23 C22 121.2(2) . . ? C25 C24 C23 117.8(2) . . ? N5 C25 C24 120.1(2) . . ? N5 C25 C26 112.69(18) . . ? C24 C25 C26 127.2(2) . . ? N6 C26 C27 121.5(2) . . ? N6 C26 C25 114.33(18) . . ? C27 C26 C25 124.2(2) . . ? C26 C27 C28 118.6(2) . . ? C29 C28 C27 120.0(2) . . ? C28 C29 C30 118.4(2) . . ? N6 C30 C29 122.0(2) . . ? _diffrn_measured_fraction_theta_max 0.975 _diffrn_reflns_theta_full 31.51 _diffrn_measured_fraction_theta_full 0.975 _refine_diff_density_max 1.026 _refine_diff_density_min -0.659 _refine_diff_density_rms 0.127 data_compound_4 _database_code_depnum_ccdc_archive 'CCDC 262941' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H22 Cu N3 O12.50 P2 V2' _chemical_formula_weight 702.71 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source O O 0.0106 0.0060 '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' 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' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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 10.361(3) _cell_length_b 10.443(4) _cell_length_c 12.259(4) _cell_angle_alpha 83.080(6) _cell_angle_beta 86.584(6) _cell_angle_gamma 82.832(6) _cell_volume 1305.2(7) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 6421 _cell_measurement_theta_min 1.68 _cell_measurement_theta_max 28.37 _exptl_crystal_description block _exptl_crystal_colour dark _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.788 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 702 _exptl_absorpt_coefficient_mu 1.698 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6678 _exptl_absorpt_correction_T_max 0.8439 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'Phi and omega scans' _diffrn_detector_area_resol_mean '512 x 512' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.001 _diffrn_reflns_number 13821 _diffrn_reflns_av_R_equivalents 0.0209 _diffrn_reflns_av_sigmaI/netI 0.0297 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.68 _diffrn_reflns_theta_max 28.37 _reflns_number_total 6421 _reflns_number_gt 6041 _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 6.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^)+(0.0456P)^2^+2.2343P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment refall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6421 _refine_ls_number_parameters 352 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0563 _refine_ls_R_factor_gt 0.0528 _refine_ls_wR_factor_ref 0.1244 _refine_ls_wR_factor_gt 0.1225 _refine_ls_goodness_of_fit_ref 1.207 _refine_ls_restrained_S_all 1.207 _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 O7 O 0.0458(2) -0.0307(2) 0.84769(19) 0.0272(5) Uani 1 1 d . . . P2 P 0.17342(7) -0.01889(8) 0.89755(6) 0.02218(17) Uani 1 1 d . . . C18 C 0.2551(3) 0.1041(4) 0.8164(3) 0.0334(8) Uani 1 1 d . . . H18A H 0.2697 0.0811 0.7419 0.040 Uiso 1 1 calc R . . H18B H 0.1986 0.1858 0.8132 0.040 Uiso 1 1 calc R . . C17 C 0.3854(3) 0.1234(4) 0.8603(3) 0.0313(7) Uani 1 1 d . . . H17A H 0.3726 0.1409 0.9364 0.038 Uiso 1 1 calc R . . H17B H 0.4451 0.0443 0.8580 0.038 Uiso 1 1 calc R . . O6 O 0.1578(2) 0.0185(2) 1.01386(18) 0.0266(5) Uani 1 1 d . . . O5 O 0.5748(3) 0.3260(3) 0.9450(2) 0.0471(7) Uani 1 1 d . . . Cu1 Cu 0.83240(4) 0.37900(4) 0.70277(3) 0.02680(11) Uani 1 1 d . . . V1 V 0.87043(5) 0.06787(5) 0.83696(4) 0.02101(12) Uani 1 1 d . . . V2 V 0.39814(6) -0.27454(6) 0.90864(5) 0.03204(15) Uani 1 1 d . . . P1 P 0.59984(8) 0.26310(8) 0.83631(7) 0.02464(18) Uani 1 1 d . . . O1 O 0.9192(2) 0.2120(2) 0.8155(2) 0.0326(5) Uani 1 1 d . . . O2 O 0.6559(2) 0.3592(2) 0.7482(2) 0.0322(5) Uani 1 1 d . . . O3 O 0.6821(2) 0.1332(2) 0.8567(2) 0.0345(6) Uani 1 1 d . . . O4 O 0.8484(3) 0.0162(3) 0.7210(2) 0.0397(6) Uani 1 1 d . . . O8 O 0.2574(3) -0.1507(3) 0.8924(2) 0.0392(6) Uani 1 1 d . . . O9 O 0.5254(4) -0.2202(5) 0.8481(4) 0.0862(14) Uani 1 1 d . . . O10 O 0.3702(4) -0.3978(4) 0.8521(3) 0.0779(13) Uani 1 1 d . . . O12 O 0.3512(6) 0.1101(7) 0.3474(4) 0.121(2) Uani 1 1 d . . . N1 N 0.8677(3) 0.5113(3) 0.8008(3) 0.0332(6) Uani 1 1 d . . . N2 N 1.0051(3) 0.4106(3) 0.6464(2) 0.0293(6) Uani 1 1 d . . . N3 N 0.8457(3) 0.2829(3) 0.5685(2) 0.0318(6) Uani 1 1 d . . . C1 C 0.7868(4) 0.5600(4) 0.8788(4) 0.0441(9) Uani 1 1 d . . . H1 H 0.7025 0.5372 0.8876 0.053 Uiso 1 1 calc R . . C2 C 0.8255(5) 0.6438(5) 0.9471(4) 0.0559(12) Uani 1 1 d . . . H2 H 0.7682 0.6760 1.0013 0.067 Uiso 1 1 calc R . . C3 C 0.9493(5) 0.6783(4) 0.9337(4) 0.0534(12) Uani 1 1 d . . . H3 H 0.9765 0.7349 0.9783 0.064 Uiso 1 1 calc R . . C4 C 1.0330(5) 0.6286(4) 0.8535(4) 0.0460(10) Uani 1 1 d . . . H4 H 1.1173 0.6512 0.8434 0.055 Uiso 1 1 calc R . . C5 C 0.9906(4) 0.5448(3) 0.7884(3) 0.0331(7) Uani 1 1 d . . . C6 C 1.0708(3) 0.4847(3) 0.6997(3) 0.0315(7) Uani 1 1 d . . . C7 C 1.2005(4) 0.4973(4) 0.6684(3) 0.0398(9) Uani 1 1 d . . . H7 H 1.2475 0.5487 0.7041 0.048 Uiso 1 1 calc R . . C8 C 1.2579(4) 0.4315(5) 0.5830(4) 0.0452(10) Uani 1 1 d . . . H8 H 1.3442 0.4393 0.5609 0.054 Uiso 1 1 calc R . . C9 C 1.1885(4) 0.3546(4) 0.5305(3) 0.0421(9) Uani 1 1 d . . . H9 H 1.2273 0.3099 0.4735 0.050 Uiso 1 1 calc R . . C10 C 1.0599(4) 0.3454(3) 0.5644(3) 0.0314(7) Uani 1 1 d . . . C11 C 0.9673(4) 0.2701(4) 0.5195(3) 0.0348(8) Uani 1 1 d . . . C12 C 0.9977(5) 0.1957(5) 0.4337(3) 0.0479(10) Uani 1 1 d . . . H12 H 1.0818 0.1867 0.4022 0.058 Uiso 1 1 calc R . . C13 C 0.9015(5) 0.1349(5) 0.3954(4) 0.0563(12) Uani 1 1 d . . . H13 H 0.9198 0.0848 0.3374 0.068 Uiso 1 1 calc R . . C14 C 0.7789(5) 0.1494(5) 0.4437(4) 0.0551(12) Uani 1 1 d . . . H14 H 0.7127 0.1100 0.4181 0.066 Uiso 1 1 calc R . . C15 C 0.7540(4) 0.2229(4) 0.5310(3) 0.0429(9) Uani 1 1 d . . . H15 H 0.6709 0.2307 0.5645 0.052 Uiso 1 1 calc R . . C16 C 0.4447(3) 0.2356(4) 0.7928(3) 0.0350(8) Uani 1 1 d . . . H16A H 0.3848 0.3143 0.7965 0.042 Uiso 1 1 calc R . . H16B H 0.4541 0.2186 0.7165 0.042 Uiso 1 1 calc R . . O13 O 0.5468(11) 0.9122(13) 0.4447(9) 0.116(4) Uani 0.50 1 d P . . O11 O 0.4737(5) 0.4081(5) 0.3721(4) 0.1052(17) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O7 0.0177(10) 0.0316(12) 0.0321(12) -0.0036(10) -0.0019(9) -0.0021(9) P2 0.0146(3) 0.0290(4) 0.0217(4) -0.0013(3) 0.0005(3) 0.0000(3) C18 0.0241(16) 0.049(2) 0.0270(16) 0.0057(15) -0.0021(13) -0.0129(15) C17 0.0201(15) 0.0405(19) 0.0325(17) 0.0025(15) -0.0021(13) -0.0064(13) O6 0.0271(11) 0.0285(12) 0.0234(11) -0.0014(9) 0.0018(9) -0.0027(9) O5 0.0591(19) 0.0487(17) 0.0320(14) -0.0101(12) -0.0063(13) 0.0065(14) Cu1 0.0268(2) 0.0261(2) 0.0282(2) -0.00285(16) 0.00226(16) -0.00795(16) V1 0.0168(2) 0.0247(3) 0.0217(2) -0.00205(19) -0.00267(18) -0.00313(19) V2 0.0245(3) 0.0378(3) 0.0325(3) -0.0088(3) -0.0015(2) 0.0064(2) P1 0.0167(4) 0.0302(4) 0.0264(4) -0.0008(3) -0.0022(3) -0.0023(3) O1 0.0239(12) 0.0294(12) 0.0431(14) 0.0048(11) -0.0029(10) -0.0055(9) O2 0.0218(11) 0.0338(13) 0.0400(14) 0.0033(11) -0.0014(10) -0.0063(10) O3 0.0180(11) 0.0331(13) 0.0500(16) 0.0028(11) 0.0001(10) -0.0018(9) O4 0.0347(14) 0.0562(17) 0.0308(13) -0.0148(12) -0.0108(11) -0.0022(12) O8 0.0308(13) 0.0447(15) 0.0395(14) -0.0128(12) -0.0058(11) 0.0154(11) O9 0.0403(19) 0.102(3) 0.097(3) 0.034(3) 0.0223(19) 0.010(2) O10 0.087(3) 0.063(2) 0.090(3) -0.046(2) -0.045(2) 0.025(2) O12 0.127(4) 0.189(6) 0.069(3) -0.016(3) -0.002(3) -0.106(4) N1 0.0335(16) 0.0258(14) 0.0411(17) -0.0069(12) -0.0008(13) -0.0047(12) N2 0.0285(14) 0.0294(14) 0.0289(14) 0.0031(11) 0.0010(11) -0.0067(11) N3 0.0366(16) 0.0332(15) 0.0260(14) -0.0020(12) 0.0000(12) -0.0078(13) C1 0.037(2) 0.037(2) 0.060(3) -0.0169(19) 0.0038(18) -0.0043(16) C2 0.061(3) 0.044(2) 0.067(3) -0.031(2) 0.006(2) -0.002(2) C3 0.063(3) 0.040(2) 0.064(3) -0.024(2) -0.008(2) -0.012(2) C4 0.049(2) 0.039(2) 0.055(3) -0.0099(19) -0.006(2) -0.0184(18) C5 0.0360(19) 0.0251(16) 0.0385(19) 0.0005(14) -0.0041(15) -0.0074(14) C6 0.0314(17) 0.0263(16) 0.0351(18) 0.0058(14) -0.0036(14) -0.0044(13) C7 0.0309(19) 0.044(2) 0.044(2) 0.0071(17) -0.0055(16) -0.0122(16) C8 0.0277(18) 0.059(3) 0.045(2) 0.0070(19) 0.0022(16) -0.0048(18) C9 0.037(2) 0.052(2) 0.0332(19) 0.0026(17) 0.0052(16) -0.0002(18) C10 0.0324(17) 0.0315(17) 0.0273(16) 0.0031(13) 0.0011(13) 0.0002(14) C11 0.042(2) 0.0336(18) 0.0269(17) 0.0025(14) 0.0009(15) -0.0046(15) C12 0.054(3) 0.052(3) 0.036(2) -0.0110(18) 0.0059(19) -0.001(2) C13 0.071(3) 0.063(3) 0.039(2) -0.024(2) 0.000(2) -0.008(2) C14 0.065(3) 0.061(3) 0.045(2) -0.020(2) -0.005(2) -0.020(2) C15 0.048(2) 0.049(2) 0.034(2) -0.0087(17) 0.0008(17) -0.0149(19) C16 0.0201(16) 0.049(2) 0.0349(18) 0.0083(16) -0.0078(13) -0.0086(15) O13 0.098(8) 0.153(11) 0.106(8) -0.052(8) -0.016(6) -0.012(7) O11 0.109(4) 0.112(4) 0.085(3) -0.004(3) 0.016(3) 0.008(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O7 P2 1.514(2) . ? O7 V1 1.977(2) 1_455 ? P2 O6 1.517(2) . ? P2 O8 1.539(3) . ? P2 C18 1.794(4) . ? C18 C17 1.529(5) . ? C17 C16 1.524(5) . ? O6 V1 1.962(2) 2_657 ? O5 P1 1.550(3) . ? O5 V2 1.838(3) 2_657 ? Cu1 O2 1.908(2) . ? Cu1 N2 1.932(3) . ? Cu1 N1 2.016(3) . ? Cu1 N3 2.018(3) . ? Cu1 O1 2.221(2) . ? V1 O4 1.618(3) . ? V1 O1 1.634(2) . ? V1 O6 1.962(2) 2_657 ? V1 O7 1.977(2) 1_655 ? V1 O3 1.996(2) . ? V2 O10 1.598(4) . ? V2 O9 1.607(4) . ? V2 O8 1.828(3) . ? V2 O5 1.838(3) 2_657 ? P1 O3 1.511(3) . ? P1 O2 1.524(3) . ? P1 C16 1.790(3) . ? N1 C1 1.338(5) . ? N1 C5 1.357(5) . ? N2 C6 1.340(5) . ? N2 C10 1.340(5) . ? N3 C15 1.333(5) . ? N3 C11 1.361(5) . ? C1 C2 1.390(6) . ? C2 C3 1.370(7) . ? C3 C4 1.377(7) . ? C4 C5 1.379(5) . ? C5 C6 1.481(5) . ? C6 C7 1.393(5) . ? C7 C8 1.385(6) . ? C8 C9 1.379(6) . ? C9 C10 1.384(5) . ? C10 C11 1.483(5) . ? C11 C12 1.380(6) . ? C12 C13 1.379(7) . ? C13 C14 1.369(7) . ? C14 C15 1.385(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P2 O7 V1 137.77(15) . 1_455 ? O7 P2 O6 113.73(13) . . ? O7 P2 O8 106.25(15) . . ? O6 P2 O8 111.65(14) . . ? O7 P2 C18 109.95(15) . . ? O6 P2 C18 106.72(16) . . ? O8 P2 C18 108.47(18) . . ? C17 C18 P2 113.9(2) . . ? C16 C17 C18 111.2(3) . . ? P2 O6 V1 137.52(15) . 2_657 ? P1 O5 V2 136.18(19) . 2_657 ? O2 Cu1 N2 174.85(11) . . ? O2 Cu1 N1 99.97(12) . . ? N2 Cu1 N1 80.40(13) . . ? O2 Cu1 N3 98.64(12) . . ? N2 Cu1 N3 80.08(13) . . ? N1 Cu1 N3 158.34(13) . . ? O2 Cu1 O1 95.59(10) . . ? N2 Cu1 O1 89.51(11) . . ? N1 Cu1 O1 93.50(12) . . ? N3 Cu1 O1 95.63(11) . . ? O4 V1 O1 110.13(15) . . ? O4 V1 O6 128.25(13) . 2_657 ? O1 V1 O6 121.60(12) . 2_657 ? O4 V1 O7 92.28(12) . 1_655 ? O1 V1 O7 96.37(11) . 1_655 ? O6 V1 O7 83.71(10) 2_657 1_655 ? O4 V1 O3 92.23(13) . . ? O1 V1 O3 95.03(12) . . ? O6 V1 O3 82.65(10) 2_657 . ? O7 V1 O3 165.47(10) 1_655 . ? O10 V2 O9 108.3(3) . . ? O10 V2 O8 108.60(16) . . ? O9 V2 O8 110.17(18) . . ? O10 V2 O5 108.54(19) . 2_657 ? O9 V2 O5 110.6(2) . 2_657 ? O8 V2 O5 110.65(13) . 2_657 ? O3 P1 O2 114.84(15) . . ? O3 P1 O5 109.97(16) . . ? O2 P1 O5 109.21(17) . . ? O3 P1 C16 108.20(17) . . ? O2 P1 C16 107.27(15) . . ? O5 P1 C16 107.02(19) . . ? V1 O1 Cu1 126.17(14) . . ? P1 O2 Cu1 130.40(15) . . ? P1 O3 V1 135.77(15) . . ? P2 O8 V2 159.0(2) . . ? C1 N1 C5 119.0(3) . . ? C1 N1 Cu1 126.8(3) . . ? C5 N1 Cu1 114.0(2) . . ? C6 N2 C10 122.6(3) . . ? C6 N2 Cu1 118.2(3) . . ? C10 N2 Cu1 118.7(2) . . ? C15 N3 C11 118.6(3) . . ? C15 N3 Cu1 127.3(3) . . ? C11 N3 Cu1 113.8(2) . . ? N1 C1 C2 121.7(4) . . ? C3 C2 C1 119.2(4) . . ? C2 C3 C4 119.4(4) . . ? C3 C4 C5 119.3(4) . . ? N1 C5 C4 121.5(4) . . ? N1 C5 C6 113.9(3) . . ? C4 C5 C6 124.6(4) . . ? N2 C6 C7 119.4(4) . . ? N2 C6 C5 112.7(3) . . ? C7 C6 C5 127.8(4) . . ? C8 C7 C6 118.6(4) . . ? C9 C8 C7 120.8(4) . . ? C8 C9 C10 118.5(4) . . ? N2 C10 C9 120.2(4) . . ? N2 C10 C11 112.2(3) . . ? C9 C10 C11 127.7(4) . . ? N3 C11 C12 121.8(4) . . ? N3 C11 C10 114.0(3) . . ? C12 C11 C10 124.2(4) . . ? C13 C12 C11 119.0(4) . . ? C14 C13 C12 119.2(4) . . ? C13 C14 C15 119.6(4) . . ? N3 C15 C14 121.9(4) . . ? C17 C16 P1 114.4(2) . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 28.37 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 0.600 _refine_diff_density_min -0.536 _refine_diff_density_rms 0.093