Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2004 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? loop_ _publ_author_name W.Ouellette V.Golub C.J.O'Connor J.Zubieta _publ_contact_author_name 'Jon Zubieta' _publ_contact_author_address ; Department of Chemistry Syracuse University 2-012 Center for Science and Techno Syracuse New York 13244 UNITED STATES OF AMERICA ; _publ_contact_author_email jazubiet@syr.edu _publ_requested_journal 'Dalton Transactions' _publ_section_title ; Solid state coordination chemistry of metal oxides: structural consequences of fluoride incorporation into the oxovanadium-copper-bisterpy-{O3P(CH2)nPO3}4- system, n = 1-5 (bisterpy = 2,2':4',4'':2'',2'''-quarterpyridyl-6',6''-di-2-pyridine). ; data_p-1 _database_code_depnum_ccdc_archive 'CCDC 247630' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '[{Cu2(bisterpy)}V2F2O2{HO3PCH2PO3}{O3PCH2PO3}]' _chemical_formula_sum 'C16 H12.50 Cu F N3 O7 P2 V' _chemical_formula_weight 554.21 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 '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' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 6.0565(3) _cell_length_b 9.6934(5) _cell_length_c 15.7351(8) _cell_angle_alpha 87.5440(10) _cell_angle_beta 80.4840(10) _cell_angle_gamma 76.7320(10) _cell_volume 886.74(8) _cell_formula_units_Z 2 _cell_measurement_temperature 90(2) _cell_measurement_reflns_used 11562 _cell_measurement_theta_min 1.31 _cell_measurement_theta_max 31.50 _exptl_crystal_description parallel _exptl_crystal_colour green _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 2.076 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 553 _exptl_absorpt_coefficient_mu 1.969 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5216 _exptl_absorpt_correction_T_max 0.8125 _exptl_absorpt_process_details 'SADABS SHELXL-97 (SHELDRICK, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 90(2) _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_probe x-ray _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'APEX CCD area detector' _diffrn_measurement_method 'Phi and omega scans' _diffrn_detector_area_resol_mean 512 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.001 _diffrn_reflns_number 11562 _diffrn_reflns_av_R_equivalents 0.0276 _diffrn_reflns_av_sigmaI/netI 0.0464 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.31 _diffrn_reflns_theta_max 31.50 _reflns_number_total 5758 _reflns_number_gt 4784 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0465P)^2^+1.0068P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5758 _refine_ls_number_parameters 328 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0513 _refine_ls_R_factor_gt 0.0396 _refine_ls_wR_factor_ref 0.1018 _refine_ls_wR_factor_gt 0.0930 _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_restrained_S_all 1.039 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.21479(5) 0.30694(3) 0.243016(18) 0.00965(8) Uani 1 1 d . . . V1 V 0.42179(7) 0.78192(5) 0.26420(3) 0.01112(9) Uani 1 1 d . . . P1 P -0.01920(11) 0.65466(7) 0.25666(4) 0.01320(13) Uani 1 1 d . . . P2 P 0.29752(11) 0.51883(7) 0.37545(4) 0.01077(12) Uani 1 1 d . . . F1 F 0.4513(3) 0.89638(17) 0.16616(10) 0.0172(3) Uani 1 1 d . . . O1 O 0.3273(3) 0.37525(19) 0.33567(11) 0.0132(3) Uani 1 1 d . . . O2 O 0.0058(3) 0.5158(2) 0.21152(13) 0.0180(4) Uani 1 1 d . . . O3 O 0.3207(3) 0.5066(2) 0.47098(12) 0.0173(4) Uani 1 1 d . . . O4 O 0.4679(3) 0.60101(19) 0.32560(12) 0.0146(4) Uani 1 1 d . . . O5 O 0.1736(3) 0.7292(2) 0.21855(12) 0.0153(4) Uani 1 1 d . . . O6 O 0.7511(3) 0.7581(2) 0.25169(14) 0.0216(4) Uani 1 1 d . . . O7 O 0.3064(3) 0.8922(2) 0.33925(12) 0.0179(4) Uani 1 1 d . . . N1 N -0.0202(4) 0.2151(2) 0.31669(13) 0.0110(4) Uani 1 1 d . . . N2 N 0.1495(3) 0.1901(2) 0.15762(13) 0.0090(4) Uani 1 1 d . . . N3 N 0.4622(3) 0.3287(2) 0.14187(13) 0.0100(4) Uani 1 1 d . . . C1 C -0.0952(5) 0.2321(3) 0.40120(16) 0.0158(5) Uani 1 1 d . . . C2 C -0.2683(5) 0.1715(3) 0.44478(17) 0.0181(5) Uani 1 1 d . . . C3 C -0.3691(5) 0.0925(3) 0.39817(17) 0.0178(5) Uani 1 1 d . . . C4 C -0.2930(5) 0.0737(3) 0.31045(16) 0.0139(5) Uani 1 1 d . . . C5 C -0.1172(4) 0.1346(2) 0.27173(15) 0.0099(4) Uani 1 1 d . . . C6 C -0.0157(4) 0.1187(2) 0.18022(15) 0.0088(4) Uani 1 1 d . . . C7 C -0.0768(4) 0.0401(2) 0.11949(15) 0.0097(4) Uani 1 1 d . . . C8 C 0.0356(4) 0.0379(2) 0.03380(15) 0.0085(4) Uani 1 1 d . . . C9 C 0.2136(4) 0.1096(2) 0.01331(15) 0.0092(4) Uani 1 1 d . . . C10 C 0.2662(4) 0.1852(2) 0.07760(15) 0.0083(4) Uani 1 1 d . . . C11 C 0.4459(4) 0.2676(2) 0.06800(15) 0.0087(4) Uani 1 1 d . . . C12 C 0.5872(4) 0.2837(3) -0.00900(16) 0.0104(4) Uani 1 1 d . . . C13 C 0.7490(4) 0.3647(3) -0.00959(16) 0.0124(4) Uani 1 1 d . . . C14 C 0.7664(4) 0.4255(3) 0.06633(17) 0.0127(4) Uani 1 1 d . . . C15 C 0.6199(4) 0.4052(3) 0.14089(16) 0.0120(4) Uani 1 1 d . . . C16 C 0.0134(4) 0.6222(3) 0.36807(17) 0.0149(5) Uani 1 1 d . . . H1 H -0.027(5) 0.286(3) 0.429(2) 0.012(8) Uiso 1 1 d . . . H2 H -0.321(6) 0.191(4) 0.506(2) 0.030(10) Uiso 1 1 d . . . H3 H -0.486(5) 0.051(3) 0.426(2) 0.013(8) Uiso 1 1 d . . . H4 H -0.348(6) 0.025(4) 0.282(2) 0.020(9) Uiso 1 1 d . . . H7 H -0.181(6) -0.005(3) 0.137(2) 0.014(8) Uiso 1 1 d . . . H9 H 0.295(5) 0.112(3) -0.041(2) 0.010(7) Uiso 1 1 d . . . H12 H 0.575(6) 0.246(3) -0.060(2) 0.016(8) Uiso 1 1 d . . . H13 H 0.849(5) 0.379(3) -0.060(2) 0.014(8) Uiso 1 1 d . . . H14 H 0.862(6) 0.475(3) 0.070(2) 0.018(8) Uiso 1 1 d . . . H15 H 0.632(5) 0.441(3) 0.195(2) 0.013(8) Uiso 1 1 d . . . H16A H -0.089(6) 0.579(4) 0.392(2) 0.023(9) Uiso 1 1 d . . . H16B H -0.008(6) 0.704(4) 0.397(2) 0.020(9) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.01129(14) 0.01092(14) 0.00875(14) -0.00317(10) -0.00138(10) -0.00622(10) V1 0.00967(19) 0.01409(19) 0.01100(19) -0.00054(15) -0.00218(14) -0.00508(15) P1 0.0091(3) 0.0134(3) 0.0189(3) 0.0035(2) -0.0047(2) -0.0053(2) P2 0.0142(3) 0.0100(3) 0.0100(3) -0.0011(2) -0.0033(2) -0.0055(2) F1 0.0163(7) 0.0208(8) 0.0156(7) 0.0019(6) -0.0025(6) -0.0070(6) O1 0.0178(9) 0.0109(8) 0.0139(8) -0.0011(6) -0.0077(7) -0.0056(7) O2 0.0221(10) 0.0138(9) 0.0234(10) 0.0014(7) -0.0137(8) -0.0077(7) O3 0.0239(10) 0.0219(10) 0.0090(8) -0.0001(7) -0.0046(7) -0.0097(8) O4 0.0153(9) 0.0119(8) 0.0189(9) 0.0047(7) -0.0054(7) -0.0069(7) O5 0.0135(8) 0.0229(9) 0.0127(8) 0.0008(7) -0.0031(7) -0.0100(7) O6 0.0109(9) 0.0169(9) 0.0374(12) 0.0050(8) -0.0084(8) -0.0019(7) O7 0.0205(9) 0.0180(9) 0.0159(9) -0.0042(7) -0.0019(7) -0.0057(7) N1 0.0153(10) 0.0114(9) 0.0081(9) -0.0015(7) -0.0028(7) -0.0060(7) N2 0.0101(9) 0.0087(8) 0.0092(9) -0.0019(7) -0.0022(7) -0.0036(7) N3 0.0087(9) 0.0114(9) 0.0110(9) -0.0021(7) -0.0031(7) -0.0033(7) C1 0.0234(13) 0.0182(12) 0.0093(10) -0.0015(9) -0.0026(9) -0.0116(10) C2 0.0272(14) 0.0208(13) 0.0093(11) -0.0021(9) 0.0002(10) -0.0134(11) C3 0.0233(13) 0.0185(12) 0.0131(11) 0.0004(10) 0.0032(10) -0.0121(10) C4 0.0177(12) 0.0133(11) 0.0132(11) -0.0021(9) -0.0012(9) -0.0094(9) C5 0.0127(10) 0.0102(10) 0.0082(10) -0.0020(8) -0.0016(8) -0.0049(8) C6 0.0104(10) 0.0080(9) 0.0084(10) -0.0018(8) -0.0012(8) -0.0030(8) C7 0.0110(10) 0.0097(10) 0.0096(10) -0.0013(8) -0.0014(8) -0.0050(8) C8 0.0086(10) 0.0073(9) 0.0099(10) -0.0012(8) -0.0022(8) -0.0016(8) C9 0.0085(10) 0.0103(10) 0.0099(10) -0.0004(8) -0.0016(8) -0.0043(8) C10 0.0071(9) 0.0087(10) 0.0101(10) -0.0005(8) -0.0028(8) -0.0028(7) C11 0.0076(9) 0.0088(10) 0.0109(10) -0.0011(8) -0.0035(8) -0.0028(8) C12 0.0085(10) 0.0118(10) 0.0115(10) -0.0012(8) -0.0022(8) -0.0029(8) C13 0.0104(10) 0.0136(11) 0.0142(11) 0.0000(9) -0.0022(9) -0.0045(8) C14 0.0111(10) 0.0137(11) 0.0157(11) -0.0011(9) -0.0025(9) -0.0073(9) C15 0.0117(10) 0.0126(11) 0.0133(11) -0.0020(9) -0.0031(9) -0.0048(8) C16 0.0133(11) 0.0151(11) 0.0163(12) 0.0005(9) 0.0004(9) -0.0053(9) _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 1.9097(17) . ? Cu1 N2 1.9380(19) . ? Cu1 N1 2.027(2) . ? Cu1 N3 2.037(2) . ? Cu1 O2 2.2114(19) . ? V1 O7 1.5867(19) . ? V1 F1 1.8697(16) . ? V1 O6 1.9321(19) . ? V1 O5 1.9437(18) . ? V1 O4 1.9509(18) . ? P1 O2 1.514(2) . ? P1 O6 1.528(2) 1_455 ? P1 O5 1.5375(19) . ? P1 C16 1.803(3) . ? P2 O1 1.5110(18) . ? P2 O3 1.5298(19) . ? P2 O4 1.5397(19) . ? P2 C16 1.801(3) . ? O6 P1 1.528(2) 1_655 ? N1 C1 1.337(3) . ? N1 C5 1.360(3) . ? N2 C10 1.335(3) . ? N2 C6 1.336(3) . ? N3 C15 1.335(3) . ? N3 C11 1.355(3) . ? C1 C2 1.388(4) . ? C2 C3 1.381(4) . ? C3 C4 1.387(4) . ? C4 C5 1.377(3) . ? C5 C6 1.469(3) . ? C6 C7 1.393(3) . ? C7 C8 1.405(3) . ? C8 C9 1.400(3) . ? C8 C8 1.491(4) 2 ? C9 C10 1.392(3) . ? C10 C11 1.476(3) . ? C11 C12 1.388(3) . ? C12 C13 1.388(3) . ? C13 C14 1.384(3) . ? C14 C15 1.385(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Cu1 N2 164.79(8) . . ? O1 Cu1 N1 96.83(8) . . ? N2 Cu1 N1 79.75(8) . . ? O1 Cu1 N3 101.10(8) . . ? N2 Cu1 N3 79.28(8) . . ? N1 Cu1 N3 157.22(8) . . ? O1 Cu1 O2 95.02(7) . . ? N2 Cu1 O2 100.20(8) . . ? N1 Cu1 O2 102.67(8) . . ? N3 Cu1 O2 89.72(8) . . ? O7 V1 F1 103.57(9) . . ? O7 V1 O6 108.17(10) . . ? F1 V1 O6 83.75(8) . . ? O7 V1 O5 106.96(9) . . ? F1 V1 O5 86.36(7) . . ? O6 V1 O5 144.83(9) . . ? O7 V1 O4 102.70(9) . . ? F1 V1 O4 153.62(8) . . ? O6 V1 O4 85.90(8) . . ? O5 V1 O4 88.28(8) . . ? O2 P1 O6 113.02(11) . 1_455 ? O2 P1 O5 111.30(11) . . ? O6 P1 O5 107.85(11) 1_455 . ? O2 P1 C16 110.02(12) . . ? O6 P1 C16 109.29(12) 1_455 . ? O5 P1 C16 105.02(11) . . ? O1 P2 O3 111.74(11) . . ? O1 P2 O4 110.97(11) . . ? O3 P2 O4 110.83(11) . . ? O1 P2 C16 109.02(12) . . ? O3 P2 C16 107.35(12) . . ? O4 P2 C16 106.72(11) . . ? P2 O1 Cu1 134.79(11) . . ? P1 O2 Cu1 126.68(11) . . ? P2 O4 V1 132.01(11) . . ? P1 O5 V1 134.08(12) . . ? P1 O6 V1 145.96(13) 1_655 . ? C1 N1 C5 118.5(2) . . ? C1 N1 Cu1 127.19(17) . . ? C5 N1 Cu1 114.15(16) . . ? C10 N2 C6 121.7(2) . . ? C10 N2 Cu1 119.54(16) . . ? C6 N2 Cu1 118.76(16) . . ? C15 N3 C11 119.2(2) . . ? C15 N3 Cu1 126.25(17) . . ? C11 N3 Cu1 114.32(15) . . ? N1 C1 C2 122.7(2) . . ? C3 C2 C1 118.3(2) . . ? C2 C3 C4 119.7(2) . . ? C5 C4 C3 118.9(2) . . ? N1 C5 C4 121.8(2) . . ? N1 C5 C6 113.9(2) . . ? C4 C5 C6 124.3(2) . . ? N2 C6 C7 120.5(2) . . ? N2 C6 C5 113.06(19) . . ? C7 C6 C5 126.4(2) . . ? C6 C7 C8 119.2(2) . . ? C9 C8 C7 118.6(2) . . ? C9 C8 C8 120.9(3) . 2 ? C7 C8 C8 120.5(3) . 2 ? C10 C9 C8 118.9(2) . . ? N2 C10 C9 121.0(2) . . ? N2 C10 C11 112.4(2) . . ? C9 C10 C11 126.6(2) . . ? N3 C11 C12 121.8(2) . . ? N3 C11 C10 114.0(2) . . ? C12 C11 C10 124.2(2) . . ? C11 C12 C13 118.6(2) . . ? C14 C13 C12 119.3(2) . . ? C13 C14 C15 119.1(2) . . ? N3 C15 C14 122.0(2) . . ? P2 C16 P1 110.07(14) . . ? _diffrn_measured_fraction_theta_max 0.977 _diffrn_reflns_theta_full 31.50 _diffrn_measured_fraction_theta_full 0.977 _refine_diff_density_max 1.585 _refine_diff_density_min -0.638 _refine_diff_density_rms 0.125 data_compound_2 _database_code_depnum_ccdc_archive 'CCDC 247631' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ; [{Cu2(bisterpy)}V2F2O2(H2O)2{O3P(CH2)2PO3}2]·2H2O (2·2H2O) ; _chemical_formula_sum 'C17 H19 Cu F N3 O9 P2 V' _chemical_formula_weight 604.77 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' F F 0.0171 0.0103 '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 10.2116(6) _cell_length_b 10.7482(6) _cell_length_c 11.0667(6) _cell_angle_alpha 108.9150(10) _cell_angle_beta 109.9160(10) _cell_angle_gamma 100.4530(10) _cell_volume 1020.51(10) _cell_formula_units_Z 2 _cell_measurement_temperature 90(2) _cell_measurement_reflns_used 6622 _cell_measurement_theta_min 2.12 _cell_measurement_theta_max 31.51 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.968 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 610 _exptl_absorpt_coefficient_mu 1.727 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6254 _exptl_absorpt_correction_T_max 0.7697 _exptl_absorpt_process_details 'SADABS SHELXL-97 (SHELDRICK, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 90(2) _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_probe x-ray _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'APEX CCD area detector' _diffrn_measurement_method 'Phi and omega scans' _diffrn_detector_area_resol_mean 512 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.001 _diffrn_reflns_number 13210 _diffrn_reflns_av_R_equivalents 0.0211 _diffrn_reflns_av_sigmaI/netI 0.0342 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.12 _diffrn_reflns_theta_max 31.51 _reflns_number_total 6622 _reflns_number_gt 5736 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL and CrystalMaker 5.x' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0651P)^2^+2.4469P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6622 _refine_ls_number_parameters 364 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0529 _refine_ls_R_factor_gt 0.0454 _refine_ls_wR_factor_ref 0.1250 _refine_ls_wR_factor_gt 0.1201 _refine_ls_goodness_of_fit_ref 1.058 _refine_ls_restrained_S_all 1.058 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.13930(3) 0.13751(3) 0.25237(3) 0.00854(8) Uani 1 1 d . . . V1 V 0.13388(5) 0.46182(4) 0.70865(4) 0.00976(9) Uani 1 1 d . . . P1 P 0.29373(7) 0.02094(7) 0.49960(7) 0.01093(13) Uani 1 1 d . . . P2 P -0.07744(7) 0.27485(7) 0.36448(7) 0.00922(12) Uani 1 1 d . . . O1 O -0.0328(2) 0.17595(19) 0.26447(19) 0.0111(3) Uani 1 1 d . . . O2 O 0.0555(2) 0.37427(19) 0.50287(19) 0.0122(3) Uani 1 1 d . . . O3 O 0.1627(2) 0.64564(19) 0.7077(2) 0.0123(3) Uani 1 1 d . . . O4 O -0.0054(2) 0.4213(2) 0.7396(2) 0.0152(4) Uani 1 1 d . . . O5 O 0.2339(2) 0.12839(19) 0.4571(2) 0.0121(3) Uani 1 1 d . . . O6 O 0.3041(2) -0.0892(2) 0.3721(2) 0.0148(4) Uani 1 1 d . . . H6 H 0.3645 -0.0506 0.3513 0.022 Uiso 1 1 calc R . . O7 O 0.4406(2) 0.0845(2) 0.6296(2) 0.0140(3) Uani 1 1 d . . . O90 O 0.4460(2) 0.2730(2) 0.8711(2) 0.0203(4) Uani 1 1 d . . . O91 O 0.2251(2) 0.3089(2) 0.6892(2) 0.0152(4) Uani 1 1 d . . . N1 N 0.0320(2) -0.0720(2) 0.1324(2) 0.0096(4) Uani 1 1 d . . . N2 N 0.2708(2) 0.0871(2) 0.1657(2) 0.0093(4) Uani 1 1 d . . . N3 N 0.2767(2) 0.3322(2) 0.3052(2) 0.0111(4) Uani 1 1 d . . . C1 C -0.0957(3) -0.1462(3) 0.1208(3) 0.0120(4) Uani 1 1 d . . . C2 C -0.1523(3) -0.2905(3) 0.0483(3) 0.0127(4) Uani 1 1 d . . . C3 C -0.0738(3) -0.3599(3) -0.0135(3) 0.0132(4) Uani 1 1 d . . . C4 C 0.0585(3) -0.2834(3) -0.0024(3) 0.0114(4) Uani 1 1 d . . . C5 C 0.1077(3) -0.1401(2) 0.0707(2) 0.0095(4) Uani 1 1 d . . . C6 C 0.2434(3) -0.0465(3) 0.0853(3) 0.0093(4) Uani 1 1 d . . . C7 C 0.3320(3) -0.0849(3) 0.0185(3) 0.0095(4) Uani 1 1 d . . . C8 C 0.4511(3) 0.0179(2) 0.0353(2) 0.0087(4) Uani 1 1 d . . . C9 C 0.4749(3) 0.1570(3) 0.1173(3) 0.0106(4) Uani 1 1 d . . . C10 C 0.3811(3) 0.1879(2) 0.1803(3) 0.0100(4) Uani 1 1 d . . . C11 C 0.3834(3) 0.3290(3) 0.2588(3) 0.0111(4) Uani 1 1 d . . . C12 C 0.4788(3) 0.4487(3) 0.2747(3) 0.0186(5) Uani 1 1 d . . . C13 C 0.4656(4) 0.5766(3) 0.3405(4) 0.0226(6) Uani 1 1 d . . . C14 C 0.3568(4) 0.5798(3) 0.3868(4) 0.0234(6) Uani 1 1 d . . . C15 C 0.2646(3) 0.4563(3) 0.3689(3) 0.0165(5) Uani 1 1 d . . . C16 C 0.1550(3) -0.0789(3) 0.5302(3) 0.0124(4) Uani 1 1 d . . . C17 C 0.2084(3) -0.1732(3) 0.6003(3) 0.0141(5) Uani 1 1 d . . . F1 F 0.30002(18) 0.55678(17) 0.88977(17) 0.0156(3) Uani 1 1 d . . . H1 H -0.146(4) -0.103(4) 0.153(4) 0.012(8) Uiso 1 1 d . . . H2 H -0.250(4) -0.342(4) 0.033(4) 0.019(10) Uiso 1 1 d . . . H3 H -0.111(4) -0.463(3) -0.067(3) 0.004(7) Uiso 1 1 d . . . H4 H 0.109(4) -0.321(4) -0.042(4) 0.013(8) Uiso 1 1 d . . . H7 H 0.307(4) -0.172(4) -0.040(4) 0.017(9) Uiso 1 1 d . . . H9 H 0.546(4) 0.223(4) 0.130(4) 0.017(9) Uiso 1 1 d . . . H12 H 0.555(5) 0.448(5) 0.236(5) 0.034(12) Uiso 1 1 d . . . H13 H 0.527(6) 0.657(5) 0.350(5) 0.040(13) Uiso 1 1 d . . . H14 H 0.344(5) 0.659(5) 0.423(5) 0.033(12) Uiso 1 1 d . . . H15 H 0.194(6) 0.447(6) 0.397(6) 0.050(15) Uiso 1 1 d . . . H16A H 0.070(5) -0.138(4) 0.438(4) 0.022(10) Uiso 1 1 d . . . H17A H 0.238(5) -0.245(4) 0.537(4) 0.022(10) Uiso 1 1 d . . . H16B H 0.127(5) -0.018(4) 0.593(4) 0.022(10) Uiso 1 1 d . . . H17B H 0.299(5) -0.117(5) 0.697(5) 0.028(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 0.00854(14) 0.00960(14) 0.00933(14) 0.00299(11) 0.00643(11) 0.00374(10) V1 0.00971(18) 0.01043(19) 0.00876(18) 0.00326(15) 0.00428(15) 0.00324(14) P1 0.0120(3) 0.0098(3) 0.0088(3) 0.0021(2) 0.0037(2) 0.0035(2) P2 0.0090(3) 0.0097(3) 0.0086(3) 0.0027(2) 0.0046(2) 0.0028(2) O1 0.0094(7) 0.0124(8) 0.0100(8) 0.0010(6) 0.0058(6) 0.0040(6) O2 0.0124(8) 0.0126(8) 0.0097(8) 0.0032(7) 0.0043(6) 0.0037(6) O3 0.0123(8) 0.0120(8) 0.0121(8) 0.0052(7) 0.0041(7) 0.0048(6) O4 0.0147(9) 0.0164(9) 0.0160(9) 0.0060(7) 0.0093(7) 0.0045(7) O5 0.0151(8) 0.0118(8) 0.0114(8) 0.0054(7) 0.0066(7) 0.0061(7) O6 0.0144(9) 0.0151(9) 0.0117(8) 0.0018(7) 0.0066(7) 0.0030(7) O7 0.0120(8) 0.0158(9) 0.0099(8) 0.0017(7) 0.0036(7) 0.0041(7) O90 0.0179(9) 0.0281(11) 0.0140(9) 0.0057(8) 0.0061(8) 0.0126(8) O91 0.0180(9) 0.0158(9) 0.0124(8) 0.0049(7) 0.0061(7) 0.0098(7) N1 0.0091(9) 0.0123(9) 0.0091(9) 0.0040(7) 0.0059(7) 0.0045(7) N2 0.0088(8) 0.0101(9) 0.0104(9) 0.0032(7) 0.0064(7) 0.0037(7) N3 0.0130(9) 0.0117(9) 0.0103(9) 0.0031(8) 0.0077(8) 0.0048(8) C1 0.0111(10) 0.0148(11) 0.0122(10) 0.0054(9) 0.0075(9) 0.0042(9) C2 0.0101(10) 0.0134(11) 0.0142(11) 0.0058(9) 0.0059(9) 0.0016(8) C3 0.0130(11) 0.0125(11) 0.0145(11) 0.0055(9) 0.0072(9) 0.0026(9) C4 0.0124(10) 0.0099(10) 0.0111(10) 0.0022(8) 0.0068(9) 0.0028(8) C5 0.0093(9) 0.0103(10) 0.0070(9) 0.0016(8) 0.0039(8) 0.0021(8) C6 0.0090(9) 0.0110(10) 0.0091(10) 0.0033(8) 0.0057(8) 0.0036(8) C7 0.0089(9) 0.0090(10) 0.0093(10) 0.0012(8) 0.0051(8) 0.0024(8) C8 0.0075(9) 0.0102(10) 0.0089(10) 0.0027(8) 0.0050(8) 0.0033(8) C9 0.0091(10) 0.0108(10) 0.0120(10) 0.0027(8) 0.0068(8) 0.0032(8) C10 0.0097(10) 0.0083(9) 0.0106(10) 0.0009(8) 0.0060(8) 0.0024(8) C11 0.0113(10) 0.0114(10) 0.0115(10) 0.0033(8) 0.0072(8) 0.0040(8) C12 0.0200(13) 0.0118(11) 0.0238(14) 0.0020(10) 0.0151(11) 0.0035(10) C13 0.0264(15) 0.0099(11) 0.0308(16) 0.0022(11) 0.0193(13) 0.0025(10) C14 0.0289(15) 0.0106(12) 0.0334(16) 0.0026(11) 0.0224(14) 0.0066(11) C15 0.0208(12) 0.0127(11) 0.0204(13) 0.0040(10) 0.0152(11) 0.0080(10) C16 0.0122(10) 0.0138(11) 0.0138(11) 0.0074(9) 0.0067(9) 0.0046(9) C17 0.0126(11) 0.0166(12) 0.0170(12) 0.0095(10) 0.0079(9) 0.0058(9) F1 0.0156(7) 0.0147(7) 0.0113(7) 0.0032(6) 0.0026(6) 0.0043(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 1.9142(18) . ? Cu1 N2 1.955(2) . ? Cu1 N1 2.051(2) . ? Cu1 N3 2.067(2) . ? Cu1 O5 2.1828(19) . ? V1 O4 1.592(2) . ? V1 F1 1.9147(17) . ? V1 O3 1.9478(19) . ? V1 O2 1.9513(19) . ? V1 O91 2.0197(19) . ? P1 O7 1.519(2) . ? P1 O5 1.5299(19) . ? P1 O6 1.571(2) . ? P1 C16 1.813(3) . ? P2 O1 1.5231(19) . ? P2 O2 1.5252(19) . ? P2 O3 1.5383(19) 2_566 ? P2 C17 1.799(3) 2_556 ? O3 P2 1.5383(19) 2_566 ? N1 C1 1.340(3) . ? N1 C5 1.357(3) . ? N2 C6 1.337(3) . ? N2 C10 1.338(3) . ? N3 C15 1.342(3) . ? N3 C11 1.355(3) . ? C1 C2 1.391(4) . ? C2 C3 1.387(4) . ? C3 C4 1.391(3) . ? C4 C5 1.384(3) . ? C5 C6 1.481(3) . ? C6 C7 1.389(3) . ? C7 C8 1.400(3) . ? C8 C9 1.399(3) . ? C8 C8 1.494(5) 2_655 ? C9 C10 1.390(3) . ? C10 C11 1.474(3) . ? C11 C12 1.384(4) . ? C12 C13 1.387(4) . ? C13 C14 1.374(4) . ? C14 C15 1.391(4) . ? C16 C17 1.532(4) . ? C17 P2 1.799(3) 2_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 O1 Cu1 N2 157.97(9) . . ? O1 Cu1 N1 94.21(8) . . ? N2 Cu1 N1 78.80(8) . . ? O1 Cu1 N3 102.31(8) . . ? N2 Cu1 N3 79.13(8) . . ? N1 Cu1 N3 155.42(8) . . ? O1 Cu1 O5 97.21(8) . . ? N2 Cu1 O5 104.36(8) . . ? N1 Cu1 O5 97.39(8) . . ? N3 Cu1 O5 98.42(8) . . ? O4 V1 F1 105.82(9) . . ? O4 V1 O3 109.01(9) . . ? F1 V1 O3 84.49(8) . . ? O4 V1 O2 104.25(9) . . ? F1 V1 O2 149.46(8) . . ? O3 V1 O2 90.81(8) . . ? O4 V1 O91 109.89(10) . . ? F1 V1 O91 83.58(8) . . ? O3 V1 O91 141.07(9) . . ? O2 V1 O91 81.30(8) . . ? O7 P1 O5 113.81(11) . . ? O7 P1 O6 110.54(11) . . ? O5 P1 O6 110.77(11) . . ? O7 P1 C16 110.29(12) . . ? O5 P1 C16 106.80(12) . . ? O6 P1 C16 104.12(12) . . ? O1 P2 O2 111.57(10) . . ? O1 P2 O3 110.82(11) . 2_566 ? O2 P2 O3 111.45(11) . 2_566 ? O1 P2 C17 108.52(12) . 2_556 ? O2 P2 C17 109.86(12) . 2_556 ? O3 P2 C17 104.34(12) 2_566 2_556 ? P2 O1 Cu1 140.53(12) . . ? P2 O2 V1 145.97(12) . . ? P2 O3 V1 140.09(12) 2_566 . ? P1 O5 Cu1 131.63(11) . . ? C1 N1 C5 118.7(2) . . ? C1 N1 Cu1 126.35(17) . . ? C5 N1 Cu1 114.63(16) . . ? C6 N2 C10 121.0(2) . . ? C6 N2 Cu1 119.58(16) . . ? C10 N2 Cu1 119.25(16) . . ? C15 N3 C11 118.2(2) . . ? C15 N3 Cu1 127.67(18) . . ? C11 N3 Cu1 113.90(17) . . ? N1 C1 C2 122.1(2) . . ? C3 C2 C1 119.0(2) . . ? C2 C3 C4 119.3(2) . . ? C5 C4 C3 118.6(2) . . ? N1 C5 C4 122.4(2) . . ? N1 C5 C6 113.7(2) . . ? C4 C5 C6 123.9(2) . . ? N2 C6 C7 120.9(2) . . ? N2 C6 C5 112.7(2) . . ? C7 C6 C5 126.3(2) . . ? C6 C7 C8 119.4(2) . . ? C9 C8 C7 118.4(2) . . ? C9 C8 C8 120.2(3) . 2_655 ? C7 C8 C8 121.4(3) . 2_655 ? C10 C9 C8 119.1(2) . . ? N2 C10 C9 121.2(2) . . ? N2 C10 C11 113.1(2) . . ? C9 C10 C11 125.5(2) . . ? N3 C11 C12 122.2(2) . . ? N3 C11 C10 114.5(2) . . ? C12 C11 C10 123.1(2) . . ? C11 C12 C13 119.2(3) . . ? C14 C13 C12 118.5(3) . . ? C13 C14 C15 119.8(3) . . ? N3 C15 C14 122.0(3) . . ? C17 C16 P1 113.68(18) . . ? C16 C17 P2 116.40(18) . 2_556 ? _diffrn_measured_fraction_theta_max 0.976 _diffrn_reflns_theta_full 31.51 _diffrn_measured_fraction_theta_full 0.976 _refine_diff_density_max 1.192 _refine_diff_density_min -0.933 _refine_diff_density_rms 0.150 data_p21_n _database_code_depnum_ccdc_archive 'CCDC 247632' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H13 Cu F2 N3 O5 P V' _chemical_formula_weight 510.74 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 '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' H H 0.0000 0.0000 '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 7.2914(4) _cell_length_b 18.1119(10) _cell_length_c 12.9448(7) _cell_angle_alpha 90.00 _cell_angle_beta 98.3650(10) _cell_angle_gamma 90.00 _cell_volume 1691.32(16) _cell_formula_units_Z 4 _cell_measurement_temperature 90(2) _cell_measurement_reflns_used 21868 _cell_measurement_theta_min 1.95 _cell_measurement_theta_max 31.50 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.006 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1020 _exptl_absorpt_coefficient_mu 1.964 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4718 _exptl_absorpt_correction_T_max 0.7984 _exptl_absorpt_process_details 'SADABS SHELXL-97 (SHELDRICK, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 90(2) _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_probe x-ray _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'APEX CCD area detector' _diffrn_measurement_method 'Phi and omega scans' _diffrn_detector_area_resol_mean 512 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.001 _diffrn_reflns_number 21868 _diffrn_reflns_av_R_equivalents 0.0303 _diffrn_reflns_av_sigmaI/netI 0.0282 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.95 _diffrn_reflns_theta_max 31.50 _reflns_number_total 5620 _reflns_number_gt 5083 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL and CrystalMaker 5.x' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0370P)^2^+1.3030P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5620 _refine_ls_number_parameters 263 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0332 _refine_ls_R_factor_gt 0.0291 _refine_ls_wR_factor_ref 0.0754 _refine_ls_wR_factor_gt 0.0730 _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_restrained_S_all 1.041 _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 0.68674(3) 0.234891(10) 0.560358(14) 0.00817(5) Uani 1 1 d . . . V1 V 0.97014(3) 0.130211(14) 0.75232(2) 0.00860(6) Uani 1 1 d . . . P1 P 0.57956(5) 0.07903(2) 0.62952(3) 0.00790(7) Uani 1 1 d . . . O1 O 0.85205(16) 0.20522(6) 0.71191(9) 0.0121(2) Uani 1 1 d . . . O2 O 0.54314(15) 0.14660(6) 0.56048(9) 0.0113(2) Uani 1 1 d . . . O3 O 0.78311(15) 0.06227(6) 0.66496(9) 0.0102(2) Uani 1 1 d . . . O4 O 0.48364(16) 0.08377(7) 0.73013(9) 0.0128(2) Uani 1 1 d . . . H4' H 0.3683 0.0868 0.7129 0.019 Uiso 1 1 calc R . . O5 O 0.91310(16) 0.10563(6) 0.86432(9) 0.0120(2) Uani 1 1 d . . . F1 F 1.13032(13) 0.06872(6) 0.68556(8) 0.0168(2) Uani 1 1 d . . . F2 F 1.19061(14) 0.17794(6) 0.79972(8) 0.0174(2) Uani 1 1 d . . . N1 N 0.50486(18) 0.30241(7) 0.61799(10) 0.0095(2) Uani 1 1 d . . . N2 N 0.79016(18) 0.32944(7) 0.53263(10) 0.0089(2) Uani 1 1 d . . . N3 N 0.89502(18) 0.20179(7) 0.48035(10) 0.0097(2) Uani 1 1 d . . . C1 C 0.3585(2) 0.28127(9) 0.66217(12) 0.0114(3) Uani 1 1 d . . . H1 H 0.3308 0.2301 0.6651 0.014 Uiso 1 1 calc R . . C2 C 0.2452(2) 0.33181(9) 0.70409(13) 0.0124(3) Uani 1 1 d . . . H2 H 0.1424 0.3155 0.7354 0.015 Uiso 1 1 calc R . . C3 C 0.2862(2) 0.40646(9) 0.69904(13) 0.0126(3) Uani 1 1 d . . . H3 H 0.2107 0.4421 0.7264 0.015 Uiso 1 1 calc R . . C4 C 0.4392(2) 0.42869(9) 0.65348(12) 0.0115(3) Uani 1 1 d . . . H4 H 0.4694 0.4795 0.6494 0.014 Uiso 1 1 calc R . . C5 C 0.5462(2) 0.37533(8) 0.61440(12) 0.0089(3) Uani 1 1 d . . . C6 C 0.7148(2) 0.39083(8) 0.56612(12) 0.0094(3) Uani 1 1 d . . . C7 C 0.7941(2) 0.45958(8) 0.55496(12) 0.0106(3) Uani 1 1 d . . . H7 H 0.7418 0.5029 0.5801 0.013 Uiso 1 1 calc R . . C8 C 0.9534(2) 0.46383(8) 0.50562(12) 0.0092(3) Uani 1 1 d . . . C9 C 1.0236(2) 0.39900(8) 0.46762(12) 0.0100(3) Uani 1 1 d . . . H9 H 1.1282 0.4007 0.4317 0.012 Uiso 1 1 calc R . . C10 C 0.9382(2) 0.33215(8) 0.48307(12) 0.0091(3) Uani 1 1 d . . . C11 C 0.9980(2) 0.25856(8) 0.45200(12) 0.0094(3) Uani 1 1 d . . . C12 C 1.1494(2) 0.24711(9) 0.40001(12) 0.0116(3) Uani 1 1 d . . . H12 H 1.2195 0.2876 0.3804 0.014 Uiso 1 1 calc R . . C13 C 1.1961(2) 0.17508(9) 0.37736(13) 0.0122(3) Uani 1 1 d . . . H13 H 1.2988 0.1658 0.3417 0.015 Uiso 1 1 calc R . . C14 C 1.0920(2) 0.11674(9) 0.40705(12) 0.0119(3) Uani 1 1 d . . . H14 H 1.1223 0.0672 0.3924 0.014 Uiso 1 1 calc R . . C15 C 0.9424(2) 0.13266(8) 0.45871(12) 0.0113(3) Uani 1 1 d . . . H15 H 0.8710 0.0929 0.4795 0.014 Uiso 1 1 calc R . . C16 C 0.4714(2) 0.00301(8) 0.55467(12) 0.0106(3) Uani 1 1 d . . . H16A H 0.5045 -0.0435 0.5932 0.013 Uiso 1 1 calc R . . H16B H 0.3352 0.0088 0.5475 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 Cu1 0.00859(9) 0.00590(9) 0.01037(9) -0.00040(6) 0.00253(6) -0.00035(6) V1 0.00663(11) 0.00967(12) 0.00954(12) 0.00149(9) 0.00127(8) -0.00063(8) P1 0.00634(16) 0.00702(16) 0.01044(17) -0.00126(13) 0.00154(12) -0.00088(12) O1 0.0143(5) 0.0091(5) 0.0122(5) -0.0002(4) -0.0006(4) -0.0009(4) O2 0.0099(5) 0.0079(5) 0.0153(5) 0.0001(4) -0.0002(4) -0.0012(4) O3 0.0074(5) 0.0092(5) 0.0139(5) -0.0020(4) 0.0010(4) 0.0005(4) O4 0.0082(5) 0.0174(6) 0.0135(5) -0.0024(4) 0.0038(4) -0.0003(4) O5 0.0124(5) 0.0122(5) 0.0116(5) 0.0017(4) 0.0028(4) -0.0006(4) F1 0.0088(4) 0.0208(5) 0.0216(5) -0.0027(4) 0.0048(4) 0.0023(4) F2 0.0127(4) 0.0208(5) 0.0175(5) 0.0019(4) -0.0012(4) -0.0070(4) N1 0.0098(6) 0.0075(6) 0.0115(6) -0.0004(4) 0.0022(4) 0.0001(4) N2 0.0097(5) 0.0070(5) 0.0101(6) 0.0000(4) 0.0023(4) -0.0005(4) N3 0.0114(6) 0.0080(6) 0.0100(6) -0.0001(4) 0.0026(4) -0.0006(4) C1 0.0109(6) 0.0099(6) 0.0135(7) 0.0012(5) 0.0027(5) -0.0008(5) C2 0.0102(6) 0.0137(7) 0.0139(7) 0.0005(5) 0.0031(5) -0.0004(5) C3 0.0118(7) 0.0129(7) 0.0133(7) -0.0014(6) 0.0029(5) 0.0008(5) C4 0.0128(7) 0.0086(6) 0.0135(7) 0.0000(5) 0.0032(5) 0.0006(5) C5 0.0094(6) 0.0084(6) 0.0092(6) 0.0004(5) 0.0022(5) 0.0002(5) C6 0.0101(6) 0.0088(6) 0.0095(6) 0.0002(5) 0.0020(5) 0.0004(5) C7 0.0111(6) 0.0084(6) 0.0128(7) 0.0002(5) 0.0035(5) 0.0001(5) C8 0.0105(6) 0.0079(6) 0.0092(6) 0.0001(5) 0.0011(5) -0.0004(5) C9 0.0106(6) 0.0094(6) 0.0102(6) -0.0003(5) 0.0024(5) -0.0007(5) C10 0.0100(6) 0.0080(6) 0.0092(6) -0.0003(5) 0.0014(5) 0.0002(5) C11 0.0105(6) 0.0082(6) 0.0094(6) -0.0002(5) 0.0014(5) 0.0001(5) C12 0.0116(7) 0.0111(7) 0.0124(7) -0.0003(5) 0.0034(5) -0.0012(5) C13 0.0117(7) 0.0125(7) 0.0132(7) -0.0001(5) 0.0039(5) 0.0024(5) C14 0.0142(7) 0.0086(6) 0.0127(7) -0.0009(5) 0.0019(5) 0.0023(5) C15 0.0136(7) 0.0083(6) 0.0120(7) -0.0001(5) 0.0022(5) -0.0002(5) C16 0.0109(6) 0.0084(6) 0.0123(7) -0.0017(5) 0.0017(5) -0.0021(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 O2 1.9116(11) . ? Cu1 N2 1.9258(13) . ? Cu1 N1 2.0246(13) . ? Cu1 N3 2.0484(13) . ? Cu1 O1 2.2141(12) . ? V1 O5 1.6275(12) . ? V1 O1 1.6522(12) . ? V1 F2 1.8496(10) . ? V1 F1 1.9091(10) . ? V1 O3 2.0504(11) . ? P1 O2 1.5159(12) . ? P1 O3 1.5190(11) . ? P1 O4 1.5677(12) . ? P1 C16 1.7983(15) . ? N1 C1 1.338(2) . ? N1 C5 1.3570(19) . ? N2 C10 1.3346(19) . ? N2 C6 1.3400(19) . ? N3 C15 1.339(2) . ? N3 C11 1.3548(19) . ? C1 C2 1.394(2) . ? C2 C3 1.388(2) . ? C3 C4 1.395(2) . ? C4 C5 1.383(2) . ? C5 C6 1.485(2) . ? C6 C7 1.389(2) . ? C7 C8 1.407(2) . ? C8 C9 1.399(2) . ? C8 C8 1.493(3) 3_766 ? C9 C10 1.389(2) . ? C10 C11 1.476(2) . ? C11 C12 1.389(2) . ? C12 C13 1.390(2) . ? C13 C14 1.387(2) . ? C14 C15 1.390(2) . ? C16 C16 1.536(3) 3_656 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Cu1 N2 166.76(5) . . ? O2 Cu1 N1 96.71(5) . . ? N2 Cu1 N1 80.03(5) . . ? O2 Cu1 N3 101.66(5) . . ? N2 Cu1 N3 80.02(5) . . ? N1 Cu1 N3 159.50(5) . . ? O2 Cu1 O1 91.37(5) . . ? N2 Cu1 O1 101.74(5) . . ? N1 Cu1 O1 96.97(5) . . ? N3 Cu1 O1 91.66(5) . . ? O5 V1 O1 108.54(6) . . ? O5 V1 F2 98.90(5) . . ? O1 V1 F2 96.23(5) . . ? O5 V1 F1 119.75(5) . . ? O1 V1 F1 131.40(5) . . ? F2 V1 F1 82.15(5) . . ? O5 V1 O3 95.25(5) . . ? O1 V1 O3 92.57(5) . . ? F2 V1 O3 160.00(5) . . ? F1 V1 O3 78.57(4) . . ? O2 P1 O3 114.78(6) . . ? O2 P1 O4 112.62(7) . . ? O3 P1 O4 107.12(7) . . ? O2 P1 C16 105.96(7) . . ? O3 P1 C16 110.01(7) . . ? O4 P1 C16 106.01(7) . . ? V1 O1 Cu1 132.18(6) . . ? P1 O2 Cu1 128.82(7) . . ? P1 O3 V1 126.07(7) . . ? C1 N1 C5 119.21(13) . . ? C1 N1 Cu1 126.21(11) . . ? C5 N1 Cu1 114.50(10) . . ? C10 N2 C6 121.57(13) . . ? C10 N2 Cu1 119.23(10) . . ? C6 N2 Cu1 119.17(10) . . ? C15 N3 C11 118.86(13) . . ? C15 N3 Cu1 127.75(11) . . ? C11 N3 Cu1 113.31(10) . . ? N1 C1 C2 122.19(14) . . ? C3 C2 C1 118.51(14) . . ? C2 C3 C4 119.46(15) . . ? C5 C4 C3 118.76(14) . . ? N1 C5 C4 121.86(14) . . ? N1 C5 C6 113.58(13) . . ? C4 C5 C6 124.56(14) . . ? N2 C6 C7 120.91(14) . . ? N2 C6 C5 112.52(13) . . ? C7 C6 C5 126.57(14) . . ? C6 C7 C8 118.68(14) . . ? C9 C8 C7 118.84(14) . . ? C9 C8 C8 120.50(17) . 3_766 ? C7 C8 C8 120.66(17) . 3_766 ? C10 C9 C8 119.13(14) . . ? N2 C10 C9 120.79(14) . . ? N2 C10 C11 112.91(13) . . ? C9 C10 C11 126.28(14) . . ? N3 C11 C12 121.91(14) . . ? N3 C11 C10 114.47(13) . . ? C12 C11 C10 123.60(14) . . ? C11 C12 C13 118.57(15) . . ? C14 C13 C12 119.73(14) . . ? C13 C14 C15 118.31(14) . . ? N3 C15 C14 122.61(14) . . ? C16 C16 P1 113.23(14) 3_656 . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 31.50 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.616 _refine_diff_density_min -0.406 _refine_diff_density_rms 0.093 data_publication_text_compound_4 _database_code_depnum_ccdc_archive 'CCDC 247633' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ; [{Cu2(bisterpy)(H2O)2}V2F2O2{HO3P(CH2)3PO3}2] ; _chemical_formula_sum 'C18 H19 Cu F N3 O8 P2 V' _chemical_formula_weight 600.78 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 '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 20.8359(9) _cell_length_b 13.3393(6) _cell_length_c 15.8184(7) _cell_angle_alpha 90.00 _cell_angle_beta 112.3680(10) _cell_angle_gamma 90.00 _cell_volume 4065.7(3) _cell_formula_units_Z 8 _cell_measurement_temperature 90(2) _cell_measurement_reflns_used 26100 _cell_measurement_theta_min 1.86 _cell_measurement_theta_max 31.51 _exptl_crystal_description parallel _exptl_crystal_colour green _exptl_crystal_size_max 0.48 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.963 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2424 _exptl_absorpt_coefficient_mu 1.729 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4907 _exptl_absorpt_correction_T_max 0.7460 _exptl_absorpt_process_details 'SADABS SHELXL-97 (SHELDRICK, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 90(2) _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_probe x-ray _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'APEX CCD area detector' _diffrn_measurement_method 'Phi and omega scans' _diffrn_detector_area_resol_mean 512 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.001 _diffrn_reflns_number 26100 _diffrn_reflns_av_R_equivalents 0.0306 _diffrn_reflns_av_sigmaI/netI 0.0296 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.86 _diffrn_reflns_theta_max 31.51 _reflns_number_total 6756 _reflns_number_gt 5993 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0656P)^2^+35.3462P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6756 _refine_ls_number_parameters 318 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0562 _refine_ls_R_factor_gt 0.0506 _refine_ls_wR_factor_ref 0.1397 _refine_ls_wR_factor_gt 0.1358 _refine_ls_goodness_of_fit_ref 1.048 _refine_ls_restrained_S_all 1.050 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.273756(16) 0.38820(3) 0.96256(2) 0.00852(9) Uani 1 1 d . . . V1 V 0.57691(2) 0.34132(4) 1.04917(3) 0.00983(10) Uani 1 1 d . . . P1 P 0.55935(5) 0.12916(7) 0.94232(6) 0.02009(17) Uani 1 1 d D . . P2 P 0.43542(3) 0.43432(5) 1.05263(4) 0.00776(13) Uani 1 1 d . . . F1 F 0.64018(10) 0.32426(15) 0.98717(14) 0.0195(4) Uani 1 1 d . . . O1 O 0.48050(11) 0.35107(15) 1.03758(15) 0.0122(4) Uani 1 1 d . . . O2 O 0.42425(10) 0.51745(16) 0.98253(14) 0.0123(4) Uani 1 1 d . . . O3 O 0.36706(10) 0.38931(16) 1.04856(14) 0.0110(4) Uani 1 1 d . . . O4 O 0.5197(2) 0.0329(2) 0.9353(2) 0.0433(9) Uani 1 1 d . A . O5 O 0.55360(10) 0.19760(15) 1.01841(14) 0.0116(4) Uani 1 1 d . A . O6A O 0.6315(2) 0.0850(8) 0.9618(5) 0.020(2) Uani 0.45(2) 1 d PD A 1 O6B O 0.6336(2) 0.1367(8) 0.9449(5) 0.031(2) Uani 0.55(2) 1 d PD A 2 O7 O 0.62102(12) 0.33908(17) 1.15626(15) 0.0158(4) Uani 1 1 d . . . O90 O 0.25249(11) 0.55092(17) 0.93331(15) 0.0150(4) Uani 1 1 d . . . N1 N 0.28018(12) 0.37057(18) 0.83705(16) 0.0105(4) Uani 1 1 d . . . N2 N 0.17735(11) 0.35936(17) 0.88724(15) 0.0086(4) Uani 1 1 d . . . N3 N 0.23316(12) 0.37326(18) 1.06047(16) 0.0096(4) Uani 1 1 d . . . C1 C 0.33725(15) 0.3710(2) 0.8172(2) 0.0141(5) Uani 1 1 d . . . H1 H 0.3813 0.3780 0.8656 0.017 Uiso 1 1 calc R . . C2 C 0.33440(15) 0.3616(2) 0.7284(2) 0.0156(5) Uani 1 1 d . . . H2 H 0.3758 0.3610 0.7167 0.019 Uiso 1 1 calc R . . C3 C 0.27004(15) 0.3532(2) 0.6570(2) 0.0142(5) Uani 1 1 d . . . H3 H 0.2668 0.3469 0.5957 0.017 Uiso 1 1 calc R . . C4 C 0.21074(15) 0.3542(2) 0.67672(19) 0.0122(5) Uani 1 1 d . . . H4 H 0.1662 0.3495 0.6290 0.015 Uiso 1 1 calc R . . C5 C 0.21725(13) 0.3623(2) 0.76701(18) 0.0091(4) Uani 1 1 d . . . C6 C 0.15762(13) 0.35880(19) 0.79601(17) 0.0089(4) Uani 1 1 d . . . C7 C 0.08776(14) 0.3552(2) 0.73942(18) 0.0096(4) Uani 1 1 d . . . H7 H 0.0739 0.3579 0.6749 0.012 Uiso 1 1 calc R . . C8 C 0.03786(13) 0.34740(19) 0.77899(17) 0.0081(4) Uani 1 1 d . . . C9 C 0.06056(13) 0.3432(2) 0.87421(18) 0.0096(4) Uani 1 1 d . . . H9 H 0.0283 0.3342 0.9028 0.012 Uiso 1 1 calc R . . C10 C 0.13122(14) 0.3525(2) 0.92649(18) 0.0101(4) Uani 1 1 d . . . C11 C 0.16348(14) 0.3601(2) 1.02724(18) 0.0104(4) Uani 1 1 d . . . C12 C 0.12637(15) 0.3590(3) 1.0837(2) 0.0174(6) Uani 1 1 d . . . H12 H 0.0777 0.3480 1.0593 0.021 Uiso 1 1 calc R . . C13 C 0.16205(16) 0.3744(3) 1.1769(2) 0.0173(6) Uani 1 1 d . . . H13 H 0.1377 0.3758 1.2168 0.021 Uiso 1 1 calc R . . C14 C 0.23347(15) 0.3876(2) 1.21116(19) 0.0134(5) Uani 1 1 d . . . H14 H 0.2586 0.3980 1.2747 0.016 Uiso 1 1 calc R . . C15 C 0.26735(14) 0.3855(2) 1.15078(18) 0.0116(5) Uani 1 1 d . . . H15 H 0.3164 0.3929 1.1741 0.014 Uiso 1 1 calc R . . C16 C 0.47888(14) 0.4903(2) 1.16405(18) 0.0112(5) Uani 1 1 d . . . H16A H 0.5215 0.5232 1.1641 0.013 Uiso 1 1 calc R . . H16B H 0.4484 0.5439 1.1708 0.013 Uiso 1 1 calc R . . C17 C 0.5000 0.4239(3) 1.2500 0.0118(7) Uani 1 2 d S . . H17A H 0.4606 0.3803 1.2466 0.014 Uiso 0.50 1 calc PR . . H17B H 0.5394 0.3803 1.2534 0.014 Uiso 0.50 1 calc PR . . C18 C 0.5000 0.1275(4) 0.7500 0.0230(9) Uani 1 2 d S . . H18A H 0.4600 0.0840 0.7438 0.028 Uiso 0.50 1 calc PR A . H18B H 0.5400 0.0840 0.7562 0.028 Uiso 0.50 1 calc PR . . C19 C 0.5178(3) 0.1937(3) 0.8352(3) 0.0366(10) Uani 1 1 d . A . H19A H 0.4745 0.2247 0.8346 0.044 Uiso 1 1 calc R . . H19B H 0.5486 0.2485 0.8315 0.044 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 0.00425(14) 0.01292(16) 0.00701(15) -0.00026(10) 0.00060(11) -0.00107(10) V1 0.0079(2) 0.0113(2) 0.0090(2) -0.00007(15) 0.00176(15) -0.00030(15) P1 0.0220(4) 0.0214(4) 0.0180(4) -0.0028(3) 0.0088(3) -0.0038(3) P2 0.0046(3) 0.0095(3) 0.0079(3) 0.0009(2) 0.0008(2) -0.0003(2) F1 0.0172(9) 0.0213(9) 0.0262(10) -0.0091(7) 0.0150(8) -0.0061(7) O1 0.0100(9) 0.0105(9) 0.0172(9) 0.0000(7) 0.0063(7) 0.0008(7) O2 0.0102(8) 0.0122(9) 0.0124(9) 0.0042(7) 0.0020(7) -0.0005(7) O3 0.0046(8) 0.0163(9) 0.0104(8) 0.0027(7) 0.0007(7) -0.0013(7) O4 0.091(3) 0.0205(13) 0.0272(14) -0.0086(11) 0.0329(17) -0.0201(15) O5 0.0115(8) 0.0100(8) 0.0144(9) -0.0026(7) 0.0061(7) -0.0022(7) O6A 0.012(2) 0.019(5) 0.031(3) -0.004(3) 0.009(2) 0.003(2) O6B 0.017(2) 0.030(5) 0.048(3) -0.008(3) 0.016(2) -0.001(2) O7 0.0144(9) 0.0171(10) 0.0115(9) 0.0012(7) 0.0000(7) -0.0004(8) O90 0.0156(9) 0.0137(9) 0.0161(9) 0.0002(7) 0.0063(8) 0.0003(8) N1 0.0067(9) 0.0139(10) 0.0103(10) -0.0025(8) 0.0026(8) -0.0008(8) N2 0.0059(9) 0.0103(9) 0.0085(9) -0.0005(7) 0.0015(7) -0.0010(7) N3 0.0059(9) 0.0137(10) 0.0074(9) 0.0015(7) 0.0003(7) -0.0008(8) C1 0.0086(11) 0.0193(13) 0.0143(12) -0.0041(10) 0.0041(9) -0.0027(10) C2 0.0109(12) 0.0215(14) 0.0161(13) -0.0026(10) 0.0070(10) -0.0028(10) C3 0.0135(12) 0.0189(13) 0.0117(12) -0.0012(10) 0.0064(10) -0.0025(10) C4 0.0108(11) 0.0153(12) 0.0096(11) -0.0011(9) 0.0030(9) -0.0014(9) C5 0.0058(10) 0.0103(11) 0.0105(11) -0.0004(8) 0.0022(8) -0.0001(8) C6 0.0079(10) 0.0099(10) 0.0087(11) -0.0001(8) 0.0029(8) 0.0005(8) C7 0.0078(10) 0.0117(11) 0.0082(10) -0.0006(8) 0.0018(8) -0.0007(8) C8 0.0051(10) 0.0092(10) 0.0079(10) -0.0009(8) 0.0002(8) -0.0008(8) C9 0.0070(10) 0.0133(11) 0.0076(10) 0.0011(8) 0.0017(8) -0.0008(8) C10 0.0073(10) 0.0132(11) 0.0088(10) 0.0016(8) 0.0021(9) -0.0003(9) C11 0.0074(10) 0.0152(12) 0.0068(10) 0.0006(8) 0.0007(8) -0.0008(9) C12 0.0089(11) 0.0327(16) 0.0098(11) 0.0030(11) 0.0027(9) -0.0011(11) C13 0.0139(13) 0.0281(16) 0.0109(12) 0.0017(11) 0.0058(10) 0.0012(11) C14 0.0138(12) 0.0157(12) 0.0081(11) 0.0002(9) 0.0013(9) 0.0007(10) C15 0.0100(11) 0.0141(12) 0.0075(10) 0.0003(9) -0.0001(9) 0.0000(9) C16 0.0108(11) 0.0111(11) 0.0088(10) 0.0004(8) 0.0006(9) -0.0003(9) C17 0.0104(15) 0.0135(16) 0.0097(15) 0.000 0.0018(12) 0.000 C18 0.031(2) 0.023(2) 0.0154(19) 0.000 0.0089(18) 0.000 C19 0.068(3) 0.0208(17) 0.0198(16) -0.0007(13) 0.0156(18) -0.0033(18) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 O3 1.9019(19) . ? Cu1 N2 1.944(2) . ? Cu1 N3 2.037(2) . ? Cu1 N1 2.054(2) . ? Cu1 O90 2.228(2) . ? V1 O7 1.591(2) . ? V1 F1 1.9329(19) . ? V1 O2 1.947(2) 5_667 ? V1 O1 1.951(2) . ? V1 O5 1.992(2) . ? P1 O4 1.508(3) . ? P1 O6A 1.533(3) . ? P1 O5 1.551(2) . ? P1 C19 1.802(4) . ? P2 O2 1.522(2) . ? P2 O3 1.524(2) . ? P2 O1 1.530(2) . ? P2 C16 1.808(3) . ? O2 V1 1.947(2) 5_667 ? N1 C1 1.341(4) . ? N1 C5 1.361(3) . ? N2 C10 1.331(3) . ? N2 C6 1.342(3) . ? N3 C15 1.342(3) . ? N3 C11 1.354(3) . ? C1 C2 1.387(4) . ? C2 C3 1.391(4) . ? C3 C4 1.385(4) . ? C4 C5 1.386(4) . ? C5 C6 1.480(4) . ? C6 C7 1.390(4) . ? C7 C8 1.407(4) . ? C8 C9 1.398(3) . ? C8 C8 1.493(5) 2_556 ? C9 C10 1.393(4) . ? C10 C11 1.479(4) . ? C11 C12 1.386(4) . ? C12 C13 1.391(4) . ? C13 C14 1.388(4) . ? C14 C15 1.387(4) . ? C16 C17 1.540(4) . ? C17 C16 1.540(4) 2_657 ? C18 C19 1.534(5) . ? C18 C19 1.534(5) 2_656 ? 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 O3 Cu1 N2 167.47(9) . . ? O3 Cu1 N3 93.67(9) . . ? N2 Cu1 N3 79.37(9) . . ? O3 Cu1 N1 105.52(9) . . ? N2 Cu1 N1 79.46(9) . . ? N3 Cu1 N1 157.28(10) . . ? O3 Cu1 O90 102.08(9) . . ? N2 Cu1 O90 89.31(9) . . ? N3 Cu1 O90 98.39(9) . . ? N1 Cu1 O90 89.53(9) . . ? O7 V1 F1 107.99(11) . . ? O7 V1 O2 103.77(10) . 5_667 ? F1 V1 O2 85.83(9) . 5_667 ? O7 V1 O1 104.97(11) . . ? F1 V1 O1 146.82(9) . . ? O2 V1 O1 89.99(9) 5_667 . ? O7 V1 O5 103.32(10) . . ? F1 V1 O5 84.99(8) . . ? O2 V1 O5 152.89(9) 5_667 . ? O1 V1 O5 83.95(9) . . ? O4 P1 O6A 99.0(5) . . ? O4 P1 O5 110.88(15) . . ? O6A P1 O5 115.5(3) . . ? O4 P1 C19 106.5(2) . . ? O6A P1 C19 117.1(4) . . ? O5 P1 C19 107.29(17) . . ? O2 P2 O3 112.02(11) . . ? O2 P2 O1 110.37(12) . . ? O3 P2 O1 109.06(12) . . ? O2 P2 C16 106.88(12) . . ? O3 P2 C16 108.49(12) . . ? O1 P2 C16 109.98(12) . . ? P2 O1 V1 134.81(13) . . ? P2 O2 V1 151.15(14) . 5_667 ? P2 O3 Cu1 135.85(13) . . ? P1 O5 V1 132.24(13) . . ? C1 N1 C5 118.4(2) . . ? C1 N1 Cu1 128.04(19) . . ? C5 N1 Cu1 113.52(18) . . ? C10 N2 C6 121.4(2) . . ? C10 N2 Cu1 119.26(18) . . ? C6 N2 Cu1 118.84(18) . . ? C15 N3 C11 119.0(2) . . ? C15 N3 Cu1 126.28(19) . . ? C11 N3 Cu1 114.29(18) . . ? N1 C1 C2 122.4(3) . . ? C1 C2 C3 119.1(3) . . ? C4 C3 C2 118.9(3) . . ? C3 C4 C5 119.1(3) . . ? N1 C5 C4 122.1(2) . . ? N1 C5 C6 114.4(2) . . ? C4 C5 C6 123.5(2) . . ? N2 C6 C7 120.7(2) . . ? N2 C6 C5 112.5(2) . . ? C7 C6 C5 126.8(2) . . ? C6 C7 C8 119.1(2) . . ? C9 C8 C7 118.6(2) . . ? C9 C8 C8 120.5(3) . 2_556 ? C7 C8 C8 120.9(3) . 2_556 ? C10 C9 C8 119.0(2) . . ? N2 C10 C9 121.1(2) . . ? N2 C10 C11 112.7(2) . . ? C9 C10 C11 126.2(2) . . ? N3 C11 C12 122.0(2) . . ? N3 C11 C10 114.1(2) . . ? C12 C11 C10 123.9(2) . . ? C11 C12 C13 118.5(3) . . ? C14 C13 C12 119.6(3) . . ? C15 C14 C13 118.6(3) . . ? N3 C15 C14 122.2(3) . . ? C17 C16 P2 119.5(2) . . ? C16 C17 C16 109.8(3) 2_657 . ? C19 C18 C19 109.7(4) . 2_656 ? C18 C19 P1 114.9(3) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 31.51 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 2.479 _refine_diff_density_min -1.812 _refine_diff_density_rms 0.166 data_publication_text_compound_5 _database_code_depnum_ccdc_archive 'CCDC 247634' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ; [{Cu6(bisterpy)3}V8F6O17(O3P(CH2)3PO3H)4]·0.8H2O ; _chemical_formula_sum 'C51 H44.90 Cu3 F3 N9 O20.90 P4 V4' _chemical_formula_weight 1693.52 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' F F 0.0171 0.0103 '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 11.0177(7) _cell_length_b 15.1098(10) _cell_length_c 17.7349(12) _cell_angle_alpha 88.3430(10) _cell_angle_beta 78.8850(10) _cell_angle_gamma 79.5140(10) _cell_volume 2848.6(3) _cell_formula_units_Z 2 _cell_measurement_temperature 90(2) _cell_measurement_reflns_used 36997 _cell_measurement_theta_min 1.37 _cell_measurement_theta_max 31.51 _exptl_crystal_description block _exptl_crystal_colour dark _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.28 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.974 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1694 _exptl_absorpt_coefficient_mu 1.938 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5111 _exptl_absorpt_correction_T_max 0.6129 _exptl_absorpt_process_details 'SADABS SHELXL-97 (SHELDRICK, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 90(2) _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_probe x-ray _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'APEX CCD area detector' _diffrn_measurement_method 'Phi and omega scans' _diffrn_detector_area_resol_mean 512 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.001 _diffrn_reflns_number 36997 _diffrn_reflns_av_R_equivalents 0.0355 _diffrn_reflns_av_sigmaI/netI 0.0622 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.37 _diffrn_reflns_theta_max 31.51 _reflns_number_total 18538 _reflns_number_gt 14116 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0603P)^2^+9.2394P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 18538 _refine_ls_number_parameters 877 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0780 _refine_ls_R_factor_gt 0.0560 _refine_ls_wR_factor_ref 0.1434 _refine_ls_wR_factor_gt 0.1324 _refine_ls_goodness_of_fit_ref 1.028 _refine_ls_restrained_S_all 1.028 _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 0.60210(4) 0.46480(3) 0.60634(2) 0.00951(8) Uani 1 1 d . . . Cu2 Cu 0.68120(4) 0.09577(3) 1.13495(2) 0.00964(8) Uani 1 1 d . . . Cu3 Cu 0.07305(4) 0.07238(3) 1.28338(2) 0.01088(9) Uani 1 1 d . . . V1 V 0.08137(6) 0.58687(4) 0.50588(3) 0.01307(12) Uani 1 1 d . . . V2 V 0.22783(7) 0.44077(5) 0.97333(4) 0.02295(15) Uani 1 1 d . . . V3 V -0.03532(7) 0.38309(5) 0.91597(4) 0.02260(14) Uani 1 1 d . . . V4 V 0.41353(5) 0.03996(4) 1.26384(3) 0.00923(10) Uani 1 1 d . . . P1 P 0.30724(8) 0.48147(6) 0.57003(5) 0.00918(15) Uani 1 1 d . . . P2 P 0.23448(10) 0.32359(7) 0.82161(5) 0.01768(19) Uani 1 1 d . . . P3 P 0.69912(8) -0.02191(6) 1.28492(5) 0.01020(15) Uani 1 1 d . . . P4 P 0.19635(8) 0.09584(6) 1.42249(5) 0.01099(16) Uani 1 1 d . . . F1 F 0.3888(2) 0.45567(18) 0.96803(16) 0.0289(6) Uani 1 1 d . . . F2 F -0.0851(2) 0.28024(17) 0.95704(14) 0.0258(5) Uani 1 1 d . . . F3 F 0.25634(19) 0.10367(15) 1.24302(11) 0.0142(4) Uani 1 1 d . . . O1 O 0.6307(2) 0.53187(16) 0.51407(13) 0.0117(4) Uani 1 1 d . . . O2 O 0.3888(2) 0.50575(16) 0.62200(13) 0.0115(4) Uani 1 1 d . A . O3 O 0.1845(2) 0.55548(17) 0.57714(15) 0.0153(5) Uani 1 1 d . A . O4 O 0.1641(3) 0.6006(3) 0.42276(19) 0.0405(10) Uani 1 1 d . A . O5A O 0.0079(12) 0.6966(9) 0.5246(5) 0.016(3) Uani 0.49(4) 1 d P A 1 O5B O -0.0309(16) 0.6661(13) 0.5397(8) 0.031(4) Uani 0.51(4) 1 d P A 2 O6 O -0.0277(6) 0.5169(4) 0.5150(4) 0.0233(13) Uani 0.50 1 d P . . O7 O 0.3265(3) 0.2379(2) 0.78814(18) 0.0251(6) Uani 1 1 d . . . H7' H 0.2921 0.2105 0.7601 0.038 Uiso 1 1 calc R . . O8 O 0.2922(3) 0.3664(2) 0.88017(15) 0.0215(6) Uani 1 1 d . . . O9 O 0.1659(3) 0.5539(2) 1.00307(19) 0.0307(7) Uani 1 1 d . . . O10 O 0.2031(4) 0.3767(3) 1.04433(19) 0.0417(9) Uani 1 1 d . . . O11 O 0.0699(3) 0.4493(2) 0.9313(2) 0.0335(7) Uani 1 1 d . . . O12 O 0.1079(3) 0.29928(19) 0.85755(16) 0.0214(6) Uani 1 1 d . . . O13 O -0.0955(3) 0.4234(2) 0.84310(19) 0.0348(8) Uani 1 1 d . . . O14 O 0.7495(2) 0.03042(18) 1.21450(13) 0.0144(5) Uani 1 1 d . . . O15 O 0.7423(3) -0.12291(19) 1.27442(16) 0.0245(6) Uani 1 1 d . . . O16 O 0.4894(2) 0.09997(17) 1.19440(14) 0.0132(5) Uani 1 1 d . . . O17 O 0.5573(2) 0.00471(18) 1.31320(14) 0.0150(5) Uani 1 1 d . . . O18 O 0.3221(2) 0.05836(18) 1.37300(14) 0.0149(5) Uani 1 1 d . . . O19 O 0.4095(3) -0.05538(17) 1.22690(16) 0.0211(6) Uani 1 1 d . . . O20 O 0.2021(3) 0.19289(18) 1.44688(16) 0.0175(5) Uani 1 1 d . . . H20 H 0.1325 0.2265 1.4464 0.026 Uiso 1 1 calc R . . O21 O 0.0815(2) 0.09456(19) 1.38722(14) 0.0162(5) Uani 1 1 d . . . O90 O 0.8442(8) 0.1836(6) 0.4620(7) 0.051(3) Uani 0.40 1 d P . . N1 N 0.5847(3) 0.33727(19) 0.57506(15) 0.0099(5) Uani 1 1 d . . . N2 N 0.6028(3) 0.40179(18) 0.70391(16) 0.0093(5) Uani 1 1 d . . . N3 N 0.6413(3) 0.56099(19) 0.67262(16) 0.0117(5) Uani 1 1 d . . . N4 N 0.6918(3) -0.00578(19) 1.06024(16) 0.0126(5) Uani 1 1 d . . . N5 N 0.6533(3) 0.16504(19) 1.04418(15) 0.0104(5) Uani 1 1 d . . . N6 N 0.6811(3) 0.2210(2) 1.17181(16) 0.0119(5) Uani 1 1 d . . . N7 N 0.0965(3) -0.0650(2) 1.28813(16) 0.0123(5) Uani 1 1 d . . . N8 N 0.0380(3) 0.0466(2) 1.18481(16) 0.0119(5) Uani 1 1 d . . . N9 N 0.0100(3) 0.1998(2) 1.24916(16) 0.0125(5) Uani 1 1 d . . . C1 C 0.5769(3) 0.3090(2) 0.50533(19) 0.0126(6) Uani 1 1 d . . . H1 H 0.5870 0.3487 0.4630 0.015 Uiso 1 1 calc R . . C2 C 0.5545(3) 0.2231(2) 0.4930(2) 0.0150(6) Uani 1 1 d . . . H2 H 0.5501 0.2043 0.4431 0.018 Uiso 1 1 calc R . . C3 C 0.5388(3) 0.1657(2) 0.5552(2) 0.0143(6) Uani 1 1 d . . . H3 H 0.5228 0.1071 0.5483 0.017 Uiso 1 1 calc R . . C4 C 0.5463(3) 0.1940(2) 0.6272(2) 0.0128(6) Uani 1 1 d . . . H4 H 0.5357 0.1553 0.6703 0.015 Uiso 1 1 calc R . . C5 C 0.5698(3) 0.2800(2) 0.63550(18) 0.0104(6) Uani 1 1 d . . . C6 C 0.5834(3) 0.3170(2) 0.70913(18) 0.0093(6) Uani 1 1 d . . . C7 C 0.5837(3) 0.2702(2) 0.77779(18) 0.0106(6) Uani 1 1 d . . . H7 H 0.5682 0.2103 0.7815 0.013 Uiso 1 1 calc R . . C8 C 0.6072(3) 0.3123(2) 0.84140(19) 0.0108(6) Uani 1 1 d . . . C9 C 0.6296(3) 0.4003(2) 0.83389(19) 0.0122(6) Uani 1 1 d . . . H9 H 0.6468 0.4303 0.8759 0.015 Uiso 1 1 calc R . . C10 C 0.6263(3) 0.4434(2) 0.76379(19) 0.0119(6) Uani 1 1 d . . . C11 C 0.6505(3) 0.5359(2) 0.74552(19) 0.0110(6) Uani 1 1 d . . . C12 C 0.6774(4) 0.5924(2) 0.7977(2) 0.0153(6) Uani 1 1 d . . . H12 H 0.6864 0.5724 0.8479 0.018 Uiso 1 1 calc R . . C13 C 0.6908(4) 0.6794(3) 0.7744(2) 0.0181(7) Uani 1 1 d . . . H13 H 0.7071 0.7205 0.8091 0.022 Uiso 1 1 calc R . . C14 C 0.6800(4) 0.7054(3) 0.6999(2) 0.0202(7) Uani 1 1 d . . . H14 H 0.6884 0.7647 0.6831 0.024 Uiso 1 1 calc R . . C15 C 0.6569(4) 0.6441(2) 0.6504(2) 0.0156(7) Uani 1 1 d . . . H15 H 0.6521 0.6616 0.5990 0.019 Uiso 1 1 calc R . . C16 C 0.7093(4) -0.0940(2) 1.0751(2) 0.0183(7) Uani 1 1 d . . . H16 H 0.7269 -0.1138 1.1238 0.022 Uiso 1 1 calc R . . C17 C 0.7028(4) -0.1576(2) 1.0221(2) 0.0184(7) Uani 1 1 d . . . H17 H 0.7156 -0.2198 1.0343 0.022 Uiso 1 1 calc R . . C18 C 0.6773(4) -0.1290(2) 0.9511(2) 0.0166(7) Uani 1 1 d . . . H18 H 0.6721 -0.1715 0.9139 0.020 Uiso 1 1 calc R . . C19 C 0.6591(3) -0.0373(2) 0.93466(19) 0.0142(6) Uani 1 1 d . . . H19 H 0.6418 -0.0163 0.8862 0.017 Uiso 1 1 calc R . . C20 C 0.6670(3) 0.0227(2) 0.99082(18) 0.0114(6) Uani 1 1 d . . . C21 C 0.6495(3) 0.1211(2) 0.98039(18) 0.0102(6) Uani 1 1 d . . . C22 C 0.6318(3) 0.1682(2) 0.91385(19) 0.0114(6) Uani 1 1 d . . . H22 H 0.6297 0.1368 0.8686 0.014 Uiso 1 1 calc R . . C23 C 0.6173(3) 0.2616(2) 0.91367(19) 0.0116(6) Uani 1 1 d . . . C24 C 0.6185(3) 0.3061(2) 0.98251(19) 0.0117(6) Uani 1 1 d . . . H24 H 0.6052 0.3699 0.9850 0.014 Uiso 1 1 calc R . . C25 C 0.6395(3) 0.2546(2) 1.04627(18) 0.0103(6) Uani 1 1 d . . . C26 C 0.6519(3) 0.2876(2) 1.12177(18) 0.0114(6) Uani 1 1 d . . . C27 C 0.6348(3) 0.3778(2) 1.1415(2) 0.0154(6) Uani 1 1 d . . . H27 H 0.6148 0.4236 1.1058 0.018 Uiso 1 1 calc R . . C28 C 0.6478(3) 0.3993(3) 1.2153(2) 0.0168(7) Uani 1 1 d . . . H28 H 0.6356 0.4605 1.2306 0.020 Uiso 1 1 calc R . . C29 C 0.6782(4) 0.3316(3) 1.2659(2) 0.0170(7) Uani 1 1 d . . . H29 H 0.6883 0.3454 1.3160 0.020 Uiso 1 1 calc R . . C30 C 0.6938(3) 0.2430(2) 1.24214(19) 0.0149(6) Uani 1 1 d . . . H30 H 0.7143 0.1962 1.2770 0.018 Uiso 1 1 calc R . . C31 C 0.1190(3) -0.1175(3) 1.3479(2) 0.0165(7) Uani 1 1 d . . . H31 H 0.1356 -0.0909 1.3918 0.020 Uiso 1 1 calc R . . C32 C 0.1189(3) -0.2100(3) 1.3479(2) 0.0171(7) Uani 1 1 d . . . H32 H 0.1337 -0.2456 1.3914 0.020 Uiso 1 1 calc R . . C33 C 0.0970(3) -0.2482(3) 1.2834(2) 0.0177(7) Uani 1 1 d . . . H33 H 0.0973 -0.3110 1.2818 0.021 Uiso 1 1 calc R . . C34 C 0.0744(3) -0.1946(2) 1.2207(2) 0.0161(7) Uani 1 1 d . . . H34 H 0.0588 -0.2202 1.1759 0.019 Uiso 1 1 calc R . . C35 C 0.0752(3) -0.1040(2) 1.22480(19) 0.0127(6) Uani 1 1 d . . . C36 C 0.0476(3) -0.0391(2) 1.16382(19) 0.0117(6) Uani 1 1 d . . . C37 C 0.0321(3) -0.0601(2) 1.09116(19) 0.0129(6) Uani 1 1 d . . . H37 H 0.0382 -0.1210 1.0765 0.015 Uiso 1 1 calc R . . C38 C 0.0070(3) 0.0103(2) 1.03932(19) 0.0128(6) Uani 1 1 d . . . C39 C -0.0064(3) 0.0991(2) 1.06430(19) 0.0131(6) Uani 1 1 d . . . H39 H -0.0264 0.1479 1.0312 0.016 Uiso 1 1 calc R . . C40 C 0.0099(3) 0.1150(2) 1.13847(19) 0.0118(6) Uani 1 1 d . . . C41 C 0.0004(3) 0.2040(2) 1.17388(19) 0.0124(6) Uani 1 1 d . . . C42 C -0.0160(3) 0.2849(2) 1.1354(2) 0.0152(6) Uani 1 1 d . . . H42 H -0.0227 0.2864 1.0828 0.018 Uiso 1 1 calc R . . C43 C -0.0223(4) 0.3641(3) 1.1753(2) 0.0192(7) Uani 1 1 d . . . H43 H -0.0323 0.4205 1.1500 0.023 Uiso 1 1 calc R . . C44 C -0.0139(4) 0.3599(3) 1.2523(2) 0.0193(7) Uani 1 1 d . . . H44 H -0.0190 0.4133 1.2806 0.023 Uiso 1 1 calc R . . C45 C 0.0021(4) 0.2762(3) 1.2878(2) 0.0180(7) Uani 1 1 d . . . H45 H 0.0076 0.2733 1.3406 0.022 Uiso 1 1 calc R . . C46 C 0.2523(3) 0.3769(2) 0.59856(19) 0.0133(6) Uani 1 1 d . A . H46A H 0.2064 0.3616 0.5594 0.016 Uiso 1 1 calc R . . H46B H 0.3270 0.3289 0.5970 0.016 Uiso 1 1 calc R . . C47 C 0.1672(3) 0.3742(3) 0.6774(2) 0.0172(7) Uani 1 1 d . . . H47A H 0.1491 0.3126 0.6863 0.021 Uiso 1 1 calc R A . H47B H 0.0863 0.4153 0.6769 0.021 Uiso 1 1 calc R . . C48 C 0.2233(4) 0.4012(3) 0.7452(2) 0.0228(8) Uani 1 1 d . A . H48A H 0.1718 0.4586 0.7671 0.027 Uiso 1 1 calc R . . H48B H 0.3088 0.4130 0.7242 0.027 Uiso 1 1 calc R . . C49 C 0.1772(3) 0.0309(3) 1.5084(2) 0.0160(7) Uani 1 1 d . . . H49A H 0.0880 0.0450 1.5346 0.019 Uiso 1 1 calc R . . H49B H 0.1959 -0.0337 1.4941 0.019 Uiso 1 1 calc R . . C50 C 0.2595(3) 0.0462(2) 1.56494(18) 0.0138(6) Uani 1 1 d . . . H50A H 0.2445 0.1111 1.5781 0.017 Uiso 1 1 calc R . . H50B H 0.3492 0.0280 1.5408 0.017 Uiso 1 1 calc R . . C51 C 0.2303(3) -0.0083(3) 1.63846(19) 0.0150(7) Uani 1 1 d . . . H51A H 0.2605 -0.0730 1.6264 0.018 Uiso 1 1 calc R . . H51B H 0.1380 0.0008 1.6562 0.018 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 0.01344(19) 0.00900(18) 0.00722(17) 0.00182(13) -0.00335(14) -0.00373(14) Cu2 0.01337(19) 0.01146(18) 0.00480(16) 0.00087(13) -0.00232(13) -0.00358(14) Cu3 0.01082(19) 0.0150(2) 0.00747(17) -0.00086(14) -0.00407(14) -0.00135(15) V1 0.0118(3) 0.0154(3) 0.0127(3) -0.0020(2) -0.0043(2) -0.0019(2) V2 0.0223(3) 0.0301(4) 0.0173(3) -0.0065(3) 0.0005(2) -0.0105(3) V3 0.0208(3) 0.0246(3) 0.0224(3) -0.0009(3) -0.0077(3) -0.0001(3) V4 0.0119(3) 0.0095(2) 0.0070(2) -0.00020(18) -0.00385(19) -0.00153(19) P1 0.0101(4) 0.0100(4) 0.0083(3) 0.0005(3) -0.0031(3) -0.0027(3) P2 0.0244(5) 0.0173(4) 0.0128(4) -0.0005(3) -0.0025(3) -0.0085(4) P3 0.0106(4) 0.0135(4) 0.0061(3) 0.0012(3) -0.0022(3) -0.0007(3) P4 0.0107(4) 0.0164(4) 0.0054(3) -0.0005(3) -0.0025(3) -0.0003(3) F1 0.0243(13) 0.0296(14) 0.0361(14) 0.0011(11) -0.0117(11) -0.0075(10) F2 0.0277(13) 0.0296(13) 0.0204(12) 0.0020(10) -0.0006(10) -0.0102(10) F3 0.0098(9) 0.0213(11) 0.0113(9) 0.0034(8) -0.0027(7) -0.0021(8) O1 0.0171(12) 0.0098(11) 0.0088(10) 0.0013(8) -0.0026(9) -0.0038(9) O2 0.0130(11) 0.0132(11) 0.0095(10) 0.0001(8) -0.0038(8) -0.0041(9) O3 0.0148(12) 0.0138(12) 0.0181(12) -0.0019(9) -0.0077(10) 0.0006(9) O4 0.0194(15) 0.066(3) 0.0291(17) 0.0299(17) -0.0031(13) 0.0052(15) O5A 0.022(4) 0.010(4) 0.016(3) -0.002(2) -0.006(3) -0.001(3) O5B 0.030(6) 0.025(6) 0.037(5) -0.012(5) -0.020(5) 0.015(5) O6 0.031(4) 0.020(3) 0.026(4) 0.002(2) -0.013(3) -0.013(3) O7 0.0216(14) 0.0244(15) 0.0290(16) -0.0060(12) -0.0035(12) -0.0036(12) O8 0.0249(14) 0.0256(14) 0.0146(12) -0.0037(11) -0.0026(11) -0.0070(11) O9 0.0256(16) 0.0318(17) 0.0324(17) -0.0076(14) 0.0022(13) -0.0058(13) O10 0.065(3) 0.043(2) 0.0218(16) 0.0037(15) -0.0043(16) -0.0283(19) O11 0.0251(16) 0.0338(18) 0.0401(19) -0.0109(15) -0.0023(14) -0.0040(13) O12 0.0246(14) 0.0208(14) 0.0186(13) 0.0002(11) -0.0014(11) -0.0065(11) O13 0.0353(19) 0.041(2) 0.0253(16) -0.0017(14) -0.0117(14) 0.0060(15) O14 0.0132(12) 0.0231(13) 0.0067(10) 0.0048(9) -0.0027(8) -0.0025(10) O15 0.0350(17) 0.0185(14) 0.0184(13) -0.0029(11) -0.0065(12) 0.0014(12) O16 0.0099(11) 0.0158(12) 0.0147(11) 0.0074(9) -0.0032(9) -0.0043(9) O17 0.0093(11) 0.0265(14) 0.0083(11) 0.0033(9) -0.0020(8) -0.0010(10) O18 0.0112(11) 0.0241(13) 0.0079(10) -0.0024(9) -0.0023(9) 0.0015(10) O19 0.0345(16) 0.0106(12) 0.0222(14) 0.0000(10) -0.0170(12) -0.0024(11) O20 0.0176(13) 0.0149(12) 0.0200(13) -0.0014(10) -0.0075(10) 0.0015(10) O21 0.0119(11) 0.0284(14) 0.0072(11) -0.0018(10) -0.0025(9) 0.0004(10) O90 0.023(4) 0.031(5) 0.088(8) -0.005(5) 0.016(5) -0.002(4) N1 0.0107(12) 0.0107(12) 0.0079(12) 0.0010(9) -0.0006(9) -0.0020(10) N2 0.0101(12) 0.0095(12) 0.0092(12) 0.0020(9) -0.0034(9) -0.0028(9) N3 0.0140(13) 0.0120(13) 0.0098(12) 0.0014(10) -0.0031(10) -0.0039(10) N4 0.0194(14) 0.0117(13) 0.0068(12) 0.0002(10) -0.0022(10) -0.0034(11) N5 0.0121(13) 0.0129(13) 0.0065(11) -0.0015(10) -0.0019(9) -0.0030(10) N6 0.0128(13) 0.0160(14) 0.0073(12) -0.0011(10) -0.0004(10) -0.0051(11) N7 0.0116(13) 0.0156(14) 0.0095(12) -0.0009(10) -0.0028(10) -0.0012(10) N8 0.0104(13) 0.0178(14) 0.0085(12) -0.0002(10) -0.0030(10) -0.0032(10) N9 0.0128(13) 0.0137(13) 0.0114(13) -0.0029(10) -0.0056(10) 0.0005(10) C1 0.0133(15) 0.0141(15) 0.0099(14) -0.0010(11) -0.0019(11) -0.0015(12) C2 0.0192(17) 0.0166(16) 0.0100(14) -0.0012(12) -0.0041(12) -0.0038(13) C3 0.0178(16) 0.0116(15) 0.0151(16) -0.0006(12) -0.0053(13) -0.0046(12) C4 0.0134(15) 0.0110(14) 0.0148(15) 0.0017(12) -0.0039(12) -0.0033(12) C5 0.0105(14) 0.0116(14) 0.0086(13) 0.0006(11) -0.0001(11) -0.0023(11) C6 0.0093(14) 0.0092(14) 0.0096(13) 0.0022(11) -0.0023(11) -0.0023(11) C7 0.0123(15) 0.0099(14) 0.0092(14) 0.0020(11) -0.0010(11) -0.0026(11) C8 0.0101(14) 0.0110(14) 0.0106(14) 0.0015(11) -0.0016(11) -0.0008(11) C9 0.0139(15) 0.0119(15) 0.0112(14) 0.0005(11) -0.0033(12) -0.0023(12) C10 0.0125(15) 0.0111(14) 0.0125(15) -0.0001(11) -0.0031(11) -0.0021(11) C11 0.0113(14) 0.0106(14) 0.0116(14) 0.0013(11) -0.0025(11) -0.0034(11) C12 0.0221(17) 0.0150(16) 0.0106(15) -0.0002(12) -0.0042(13) -0.0074(13) C13 0.0245(19) 0.0157(17) 0.0164(16) 0.0004(13) -0.0044(14) -0.0093(14) C14 0.031(2) 0.0114(16) 0.0200(18) 0.0021(13) -0.0044(15) -0.0088(14) C15 0.0232(18) 0.0109(15) 0.0141(15) 0.0040(12) -0.0053(13) -0.0060(13) C16 0.031(2) 0.0132(16) 0.0117(15) 0.0025(12) -0.0059(14) -0.0050(14) C17 0.033(2) 0.0095(15) 0.0134(16) 0.0016(12) -0.0054(14) -0.0044(14) C18 0.0266(19) 0.0143(16) 0.0106(15) -0.0025(12) -0.0067(13) -0.0040(14) C19 0.0198(17) 0.0167(16) 0.0070(14) -0.0006(12) -0.0035(12) -0.0046(13) C20 0.0158(15) 0.0114(14) 0.0076(13) 0.0009(11) -0.0026(11) -0.0037(12) C21 0.0121(14) 0.0110(14) 0.0076(13) -0.0004(11) -0.0010(11) -0.0031(11) C22 0.0144(15) 0.0111(14) 0.0085(14) 0.0016(11) -0.0014(11) -0.0027(12) C23 0.0122(15) 0.0117(14) 0.0117(14) 0.0034(11) -0.0036(11) -0.0034(11) C24 0.0139(15) 0.0107(14) 0.0112(14) 0.0002(11) -0.0026(11) -0.0038(12) C25 0.0110(14) 0.0123(14) 0.0081(13) -0.0002(11) -0.0010(11) -0.0041(11) C26 0.0118(15) 0.0139(15) 0.0090(14) -0.0011(11) -0.0029(11) -0.0027(12) C27 0.0190(17) 0.0111(15) 0.0168(16) -0.0024(12) -0.0033(13) -0.0042(13) C28 0.0149(16) 0.0191(17) 0.0164(16) -0.0073(13) -0.0010(13) -0.0039(13) C29 0.0208(18) 0.0199(17) 0.0115(15) -0.0048(13) -0.0026(13) -0.0067(14) C30 0.0176(16) 0.0187(17) 0.0100(14) -0.0003(12) -0.0038(12) -0.0061(13) C31 0.0173(17) 0.0199(17) 0.0125(15) 0.0019(13) -0.0062(13) -0.0011(13) C32 0.0159(16) 0.0200(17) 0.0147(16) 0.0056(13) -0.0043(13) -0.0011(13) C33 0.0159(17) 0.0155(16) 0.0218(18) 0.0015(13) -0.0046(13) -0.0025(13) C34 0.0165(16) 0.0179(17) 0.0141(16) -0.0008(13) -0.0044(13) -0.0022(13) C35 0.0104(14) 0.0178(16) 0.0095(14) 0.0002(12) -0.0013(11) -0.0018(12) C36 0.0097(14) 0.0156(15) 0.0101(14) 0.0008(11) -0.0030(11) -0.0016(12) C37 0.0150(15) 0.0140(15) 0.0099(14) 0.0004(11) -0.0039(12) -0.0014(12) C38 0.0112(15) 0.0170(16) 0.0107(15) -0.0003(12) -0.0029(12) -0.0028(12) C39 0.0137(15) 0.0150(15) 0.0112(14) -0.0008(12) -0.0037(12) -0.0027(12) C40 0.0093(14) 0.0150(15) 0.0102(14) -0.0013(12) -0.0019(11) 0.0002(11) C41 0.0106(14) 0.0167(16) 0.0096(14) -0.0033(12) -0.0023(11) -0.0005(12) C42 0.0163(16) 0.0157(16) 0.0130(15) 0.0001(12) -0.0032(12) -0.0011(13) C43 0.0218(18) 0.0151(17) 0.0204(18) -0.0012(13) -0.0050(14) -0.0011(14) C44 0.0212(18) 0.0182(17) 0.0185(17) -0.0056(14) -0.0065(14) 0.0000(14) C45 0.0191(17) 0.0198(17) 0.0156(16) -0.0053(13) -0.0086(13) 0.0013(14) C46 0.0158(16) 0.0134(15) 0.0124(15) 0.0012(12) -0.0034(12) -0.0064(12) C47 0.0150(16) 0.0209(18) 0.0159(16) 0.0016(13) 0.0007(13) -0.0074(13) C48 0.033(2) 0.0233(19) 0.0131(16) 0.0028(14) -0.0014(15) -0.0112(16) C49 0.0163(16) 0.0245(18) 0.0107(15) 0.0032(13) -0.0066(12) -0.0086(14) C50 0.0169(16) 0.0197(17) 0.0066(13) 0.0019(12) -0.0042(11) -0.0062(13) C51 0.0137(16) 0.0239(18) 0.0088(14) 0.0047(13) -0.0034(12) -0.0064(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 O1 1.904(2) . ? Cu1 N2 1.951(3) . ? Cu1 N3 2.050(3) . ? Cu1 N1 2.073(3) . ? Cu1 O2 2.283(2) . ? Cu2 O14 1.895(2) . ? Cu2 N5 1.939(3) . ? Cu2 N6 2.020(3) . ? Cu2 N4 2.029(3) . ? Cu2 O16 2.163(2) . ? Cu3 O21 1.904(2) . ? Cu3 N8 1.926(3) . ? Cu3 N9 2.041(3) . ? Cu3 N7 2.046(3) . ? Cu3 F3 2.141(2) . ? V1 O5B 1.593(7) . ? V1 O4 1.606(3) . ? V1 O5A 1.719(9) . ? V1 O6 1.722(6) . ? V1 O6 1.844(6) 2_566 ? V1 O3 1.853(3) . ? V2 O10 1.578(3) . ? V2 O9 1.776(3) . ? V2 F1 1.812(3) . ? V2 O8 1.965(3) . ? V2 O11 2.003(4) . ? V3 O13 1.618(3) . ? V3 O11 1.727(3) . ? V3 F2 1.827(3) . ? V3 O9 1.955(3) 2_567 ? V3 O12 1.971(3) . ? V4 O19 1.611(3) . ? V4 O16 1.689(2) . ? V4 F3 1.919(2) . ? V4 O17 1.939(2) . ? V4 O18 2.004(2) . ? P1 O2 1.500(2) . ? P1 O1 1.519(2) 2_666 ? P1 O3 1.577(3) . ? P1 C46 1.817(3) . ? P2 O12 1.522(3) . ? P2 O8 1.531(3) . ? P2 O7 1.546(3) . ? P2 C48 1.773(4) . ? P3 O15 1.519(3) . ? P3 O14 1.526(3) . ? P3 O17 1.529(3) . ? P3 C51 1.798(4) 2_658 ? P4 O18 1.511(3) . ? P4 O21 1.519(3) . ? P4 O20 1.556(3) . ? P4 C49 1.787(4) . ? O1 P1 1.519(2) 2_666 ? O6 O6 0.832(11) 2_566 ? O6 V1 1.844(6) 2_566 ? O9 V3 1.955(3) 2_567 ? N1 C1 1.343(4) . ? N1 C5 1.362(4) . ? N2 C6 1.335(4) . ? N2 C10 1.340(4) . ? N3 C15 1.336(4) . ? N3 C11 1.354(4) . ? N4 C16 1.338(5) . ? N4 C20 1.354(4) . ? N5 C25 1.334(4) . ? N5 C21 1.339(4) . ? N6 C30 1.339(4) . ? N6 C26 1.358(4) . ? N7 C31 1.340(4) . ? N7 C35 1.361(4) . ? N8 C40 1.331(4) . ? N8 C36 1.338(5) . ? N9 C45 1.341(5) . ? N9 C41 1.358(4) . ? C1 C2 1.395(5) . ? C2 C3 1.387(5) . ? C3 C4 1.380(5) . ? C4 C5 1.389(5) . ? C5 C6 1.479(5) . ? C6 C7 1.390(4) . ? C7 C8 1.399(5) . ? C8 C9 1.393(5) . ? C8 C23 1.486(5) . ? C9 C10 1.391(5) . ? C10 C11 1.485(5) . ? C11 C12 1.384(5) . ? C12 C13 1.391(5) . ? C13 C14 1.388(5) . ? C14 C15 1.383(5) . ? C16 C17 1.384(5) . ? C17 C18 1.382(5) . ? C18 C19 1.394(5) . ? C19 C20 1.391(5) . ? C20 C21 1.476(5) . ? C21 C22 1.388(4) . ? C22 C23 1.390(5) . ? C23 C24 1.414(5) . ? C24 C25 1.387(4) . ? C25 C26 1.482(4) . ? C26 C27 1.386(5) . ? C27 C28 1.398(5) . ? C28 C29 1.379(5) . ? C29 C30 1.386(5) . ? C31 C32 1.396(5) . ? C32 C33 1.377(5) . ? C33 C34 1.392(5) . ? C34 C35 1.376(5) . ? C35 C36 1.477(5) . ? C36 C37 1.386(5) . ? C37 C38 1.410(5) . ? C38 C39 1.399(5) . ? C38 C38 1.480(7) 2_557 ? C39 C40 1.395(5) . ? C40 C41 1.479(5) . ? C41 C42 1.382(5) . ? C42 C43 1.392(5) . ? C43 C44 1.386(5) . ? C44 C45 1.393(5) . ? C46 C47 1.530(5) . ? C47 C48 1.550(6) . ? C49 C50 1.524(5) . ? C50 C51 1.535(5) . ? C51 P3 1.798(4) 2_658 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Cu1 N2 169.12(11) . . ? O1 Cu1 N3 93.68(11) . . ? N2 Cu1 N3 78.95(11) . . ? O1 Cu1 N1 106.94(10) . . ? N2 Cu1 N1 79.20(11) . . ? N3 Cu1 N1 157.17(11) . . ? O1 Cu1 O2 93.01(10) . . ? N2 Cu1 O2 96.16(10) . . ? N3 Cu1 O2 100.32(10) . . ? N1 Cu1 O2 88.51(10) . . ? O14 Cu2 N5 166.14(12) . . ? O14 Cu2 N6 98.04(12) . . ? N5 Cu2 N6 79.46(12) . . ? O14 Cu2 N4 100.23(12) . . ? N5 Cu2 N4 80.15(12) . . ? N6 Cu2 N4 158.63(11) . . ? O14 Cu2 O16 93.17(10) . . ? N5 Cu2 O16 100.51(11) . . ? N6 Cu2 O16 91.61(11) . . ? N4 Cu2 O16 98.33(11) . . ? O21 Cu3 N8 170.94(12) . . ? O21 Cu3 N9 100.50(12) . . ? N8 Cu3 N9 79.99(12) . . ? O21 Cu3 N7 98.15(12) . . ? N8 Cu3 N7 79.79(12) . . ? N9 Cu3 N7 158.09(12) . . ? O21 Cu3 F3 91.65(10) . . ? N8 Cu3 F3 97.40(10) . . ? N9 Cu3 F3 84.74(10) . . ? N7 Cu3 F3 106.17(10) . . ? O5B V1 O4 118.0(9) . . ? O5B V1 O5A 24.0(5) . . ? O4 V1 O5A 98.7(5) . . ? O5B V1 O6 87.8(10) . . ? O4 V1 O6 119.4(3) . . ? O5A V1 O6 110.5(6) . . ? O5B V1 O6 113.3(9) . 2_566 ? O4 V1 O6 98.4(2) . 2_566 ? O5A V1 O6 134.0(6) . 2_566 ? O6 V1 O6 26.7(4) . 2_566 ? O5B V1 O3 109.7(3) . . ? O4 V1 O3 110.35(15) . . ? O5A V1 O3 107.2(3) . . ? O6 V1 O3 109.7(2) . . ? O6 V1 O3 106.1(2) 2_566 . ? O10 V2 O9 109.05(18) . . ? O10 V2 F1 104.11(18) . . ? O9 V2 F1 92.86(14) . . ? O10 V2 O8 108.65(17) . . ? O9 V2 O8 141.33(15) . . ? F1 V2 O8 86.12(12) . . ? O10 V2 O11 101.81(19) . . ? O9 V2 O11 84.43(15) . . ? F1 V2 O11 153.35(14) . . ? O8 V2 O11 79.82(13) . . ? O13 V3 O11 107.91(19) . . ? O13 V3 F2 115.71(16) . . ? O11 V3 F2 136.27(15) . . ? O13 V3 O9 97.83(16) . 2_567 ? O11 V3 O9 91.54(15) . 2_567 ? F2 V3 O9 85.70(13) . 2_567 ? O13 V3 O12 96.89(15) . . ? O11 V3 O12 88.11(14) . . ? F2 V3 O12 83.97(12) . . ? O9 V3 O12 164.63(14) 2_567 . ? O19 V4 O16 107.63(14) . . ? O19 V4 F3 97.46(12) . . ? O16 V4 F3 89.14(10) . . ? O19 V4 O17 99.62(13) . . ? O16 V4 O17 94.39(11) . . ? F3 V4 O17 160.59(11) . . ? O19 V4 O18 114.45(14) . . ? O16 V4 O18 137.77(12) . . ? F3 V4 O18 82.38(9) . . ? O17 V4 O18 82.21(10) . . ? O2 P1 O1 115.46(14) . 2_666 ? O2 P1 O3 109.35(14) . . ? O1 P1 O3 109.33(14) 2_666 . ? O2 P1 C46 111.81(15) . . ? O1 P1 C46 105.10(15) 2_666 . ? O3 P1 C46 105.25(16) . . ? O12 P2 O8 111.90(16) . . ? O12 P2 O7 109.60(17) . . ? O8 P2 O7 108.74(17) . . ? O12 P2 C48 112.37(19) . . ? O8 P2 C48 106.80(18) . . ? O7 P2 C48 107.25(19) . . ? O15 P3 O14 112.29(16) . . ? O15 P3 O17 112.92(17) . . ? O14 P3 O17 113.59(14) . . ? O15 P3 C51 105.31(17) . 2_658 ? O14 P3 C51 106.38(15) . 2_658 ? O17 P3 C51 105.51(16) . 2_658 ? O18 P4 O21 116.07(14) . . ? O18 P4 O20 107.28(16) . . ? O21 P4 O20 111.25(15) . . ? O18 P4 C49 108.51(16) . . ? O21 P4 C49 106.46(16) . . ? O20 P4 C49 106.90(16) . . ? V4 F3 Cu3 127.53(11) . . ? P1 O1 Cu1 140.32(16) 2_666 . ? P1 O2 Cu1 126.45(14) . . ? P1 O3 V1 128.57(16) . . ? O6 O6 V1 84.8(9) 2_566 . ? O6 O6 V1 68.5(8) 2_566 2_566 ? V1 O6 V1 153.3(4) . 2_566 ? P2 O8 V2 136.00(18) . . ? V2 O9 V3 137.32(19) . 2_567 ? V3 O11 V2 140.3(2) . . ? P2 O12 V3 124.98(17) . . ? P3 O14 Cu2 135.97(16) . . ? V4 O16 Cu2 136.50(14) . . ? P3 O17 V4 134.88(15) . . ? P4 O18 V4 143.33(16) . . ? P4 O21 Cu3 129.05(15) . . ? C1 N1 C5 118.6(3) . . ? C1 N1 Cu1 127.7(2) . . ? C5 N1 Cu1 113.4(2) . . ? C6 N2 C10 121.1(3) . . ? C6 N2 Cu1 119.3(2) . . ? C10 N2 Cu1 119.5(2) . . ? C15 N3 C11 118.7(3) . . ? C15 N3 Cu1 126.1(2) . . ? C11 N3 Cu1 115.2(2) . . ? C16 N4 C20 119.0(3) . . ? C16 N4 Cu2 127.0(2) . . ? C20 N4 Cu2 113.7(2) . . ? C25 N5 C21 121.6(3) . . ? C25 N5 Cu2 119.7(2) . . ? C21 N5 Cu2 118.7(2) . . ? C30 N6 C26 119.1(3) . . ? C30 N6 Cu2 125.8(2) . . ? C26 N6 Cu2 114.7(2) . . ? C31 N7 C35 118.4(3) . . ? C31 N7 Cu3 127.3(2) . . ? C35 N7 Cu3 114.0(2) . . ? C40 N8 C36 122.1(3) . . ? C40 N8 Cu3 118.6(2) . . ? C36 N8 Cu3 119.2(2) . . ? C45 N9 C41 119.2(3) . . ? C45 N9 Cu3 126.5(2) . . ? C41 N9 Cu3 112.9(2) . . ? N1 C1 C2 122.1(3) . . ? C3 C2 C1 118.6(3) . . ? C4 C3 C2 119.9(3) . . ? C3 C4 C5 118.7(3) . . ? N1 C5 C4 122.1(3) . . ? N1 C5 C6 114.2(3) . . ? C4 C5 C6 123.7(3) . . ? N2 C6 C7 120.7(3) . . ? N2 C6 C5 113.3(3) . . ? C7 C6 C5 125.9(3) . . ? C6 C7 C8 119.4(3) . . ? C9 C8 C7 118.7(3) . . ? C9 C8 C23 120.8(3) . . ? C7 C8 C23 120.3(3) . . ? C10 C9 C8 118.9(3) . . ? N2 C10 C9 121.2(3) . . ? N2 C10 C11 113.0(3) . . ? C9 C10 C11 125.8(3) . . ? N3 C11 C12 122.7(3) . . ? N3 C11 C10 113.4(3) . . ? C12 C11 C10 123.9(3) . . ? C11 C12 C13 118.0(3) . . ? C14 C13 C12 119.3(3) . . ? C15 C14 C13 119.2(3) . . ? N3 C15 C14 122.0(3) . . ? N4 C16 C17 122.5(3) . . ? C18 C17 C16 118.9(3) . . ? C17 C18 C19 119.4(3) . . ? C20 C19 C18 118.5(3) . . ? N4 C20 C19 121.8(3) . . ? N4 C20 C21 114.6(3) . . ? C19 C20 C21 123.6(3) . . ? N5 C21 C22 120.4(3) . . ? N5 C21 C20 112.6(3) . . ? C22 C21 C20 127.0(3) . . ? C21 C22 C23 119.7(3) . . ? C22 C23 C24 118.5(3) . . ? C22 C23 C8 120.2(3) . . ? C24 C23 C8 121.2(3) . . ? C25 C24 C23 118.6(3) . . ? N5 C25 C24 121.1(3) . . ? N5 C25 C26 112.0(3) . . ? C24 C25 C26 126.9(3) . . ? N6 C26 C27 121.8(3) . . ? N6 C26 C25 113.8(3) . . ? C27 C26 C25 124.3(3) . . ? C26 C27 C28 118.2(3) . . ? C29 C28 C27 119.9(3) . . ? C28 C29 C30 118.7(3) . . ? N6 C30 C29 122.3(3) . . ? N7 C31 C32 122.4(3) . . ? C33 C32 C31 118.4(3) . . ? C32 C33 C34 119.9(3) . . ? C35 C34 C33 118.6(3) . . ? N7 C35 C34 122.3(3) . . ? N7 C35 C36 113.5(3) . . ? C34 C35 C36 124.2(3) . . ? N8 C36 C37 120.7(3) . . ? N8 C36 C35 113.2(3) . . ? C37 C36 C35 126.1(3) . . ? C36 C37 C38 118.9(3) . . ? C39 C38 C37 118.7(3) . . ? C39 C38 C38 121.2(4) . 2_557 ? C37 C38 C38 120.1(4) . 2_557 ? C40 C39 C38 119.1(3) . . ? N8 C40 C39 120.5(3) . . ? N8 C40 C41 113.2(3) . . ? C39 C40 C41 126.3(3) . . ? N9 C41 C42 122.0(3) . . ? N9 C41 C40 113.6(3) . . ? C42 C41 C40 124.4(3) . . ? C41 C42 C43 118.7(3) . . ? C44 C43 C42 119.3(4) . . ? C43 C44 C45 119.2(4) . . ? N9 C45 C44 121.6(3) . . ? C47 C46 P1 117.7(3) . . ? C46 C47 C48 114.3(3) . . ? C47 C48 P2 117.5(3) . . ? C50 C49 P4 114.8(2) . . ? C49 C50 C51 110.7(3) . . ? C50 C51 P3 113.5(2) . 2_658 ? _diffrn_measured_fraction_theta_max 0.978 _diffrn_reflns_theta_full 31.51 _diffrn_measured_fraction_theta_full 0.978 _refine_diff_density_max 3.477 _refine_diff_density_min -1.168 _refine_diff_density_rms 0.158 data_publication_text_compound_6 _database_code_depnum_ccdc_archive 'CCDC 247635' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ; [{Cu2(bisterpy)}V2O4(HO3P(CH2)3PO3)2]·0.5H2O ; _chemical_formula_sum 'C36 H35 Cu2 N6 O16.50 P4 V2' _chemical_formula_weight 1168.54 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 10.8333(7) _cell_length_b 13.7289(9) _cell_length_c 15.8044(10) _cell_angle_alpha 74.1160(10) _cell_angle_beta 71.5670(10) _cell_angle_gamma 71.0580(10) _cell_volume 2070.5(2) _cell_formula_units_Z 2 _cell_measurement_temperature 90(2) _cell_measurement_reflns_used 3832 _cell_measurement_theta_min 2.25 _cell_measurement_theta_max 28.04 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.874 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1178 _exptl_absorpt_coefficient_mu 1.689 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6312 _exptl_absorpt_correction_T_max 0.8767 _exptl_absorpt_process_details 'SADABS SHELXL-97 (SHELDRICK, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 90(2) _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_probe x-ray _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'APEX CCD area detector' _diffrn_measurement_method 'Phi and omega scans' _diffrn_detector_area_resol_mean 512 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.001 _diffrn_reflns_number 22011 _diffrn_reflns_av_R_equivalents 0.0434 _diffrn_reflns_av_sigmaI/netI 0.0648 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.90 _diffrn_reflns_theta_max 28.28 _reflns_number_total 10197 _reflns_number_gt 8183 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL and CrystalMaker 5.x' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0637P)^2^+5.1009P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10197 _refine_ls_number_parameters 628 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0767 _refine_ls_R_factor_gt 0.0596 _refine_ls_wR_factor_ref 0.1495 _refine_ls_wR_factor_gt 0.1401 _refine_ls_goodness_of_fit_ref 1.073 _refine_ls_restrained_S_all 1.073 _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 0.68038(5) 0.43140(4) 0.51437(3) 0.01171(12) Uani 1 1 d . . . Cu2 Cu 0.83108(5) 0.11018(4) 1.10222(3) 0.01416(12) Uani 1 1 d . . . V1 V 0.88122(7) 0.17433(5) 0.57176(5) 0.01409(16) Uani 1 1 d . . . V2 V 0.70180(8) 0.50932(6) 0.95919(5) 0.01571(16) Uani 1 1 d . . . P1 P 0.57051(12) 0.26866(9) 0.67964(7) 0.0151(2) Uani 1 1 d . . . P2 P 0.57991(12) 0.31193(9) 1.02920(7) 0.0160(2) Uani 1 1 d . . . P3 P 0.83644(15) -0.03921(13) 0.5306(3) 0.0134(8) Uani 0.801(15) 1 d P . 1 P4 P 0.6973(3) -0.0459(3) 1.27772(12) 0.0126(7) Uani 0.801(15) 1 d P . 1 P3B P 0.8305(8) -0.0452(6) 0.5735(14) 0.023(2) Uani 0.199(15) 1 d P . 2 P4B P 0.652(2) -0.0072(13) 1.2722(7) 0.031(3) Uani 0.199(15) 1 d P . 2 O1 O 0.5802(3) 0.3792(2) 0.63292(19) 0.0157(6) Uani 1 1 d . . . O2 O 0.8357(3) 0.2877(2) 0.5054(2) 0.0194(6) Uani 1 1 d . . . O3 O 0.4599(4) 0.2456(3) 0.6529(2) 0.0275(8) Uani 1 1 d . . . H3' H 0.4867 0.1868 0.6407 0.041 Uiso 1 1 calc R . . O4 O 0.7037(4) 0.1871(2) 0.6628(2) 0.0243(7) Uani 1 1 d . . . O5 O 0.9557(4) 0.1908(3) 0.6393(2) 0.0288(8) Uani 1 1 d . . . O6 O 1.0450(3) 0.1341(2) 0.4744(2) 0.0210(7) Uani 1 1 d . . . O7 O 0.8016(4) 0.0131(3) 0.4384(3) 0.0402(10) Uani 1 1 d . . . O8 O 0.8548(4) 0.0391(3) 0.5750(3) 0.0344(9) Uani 1 1 d . . . O9 O 0.8365(3) 0.5191(3) 0.8788(2) 0.0207(7) Uani 1 1 d . . . O10 O 0.7230(4) 0.5269(3) 1.0499(2) 0.0251(7) Uani 1 1 d . . . O11 O 0.6817(3) 0.3764(3) 0.9691(2) 0.0242(7) Uani 1 1 d . . . O12 O 0.4490(3) 0.3914(3) 1.0711(2) 0.0217(7) Uani 1 1 d . . . O13 O 0.6334(3) 0.2275(3) 1.1013(2) 0.0201(7) Uani 1 1 d . . . O14 O 0.7990(3) 0.0066(3) 1.2067(2) 0.0219(7) Uani 1 1 d . . . O15 O 0.6655(4) -0.1233(3) 1.2418(2) 0.0318(8) Uani 1 1 d . . . O16 O 0.7468(5) -0.1017(4) 1.3644(3) 0.0454(11) Uani 1 1 d . . . O90 O 0.3750(7) 0.1433(6) 0.2471(4) 0.0233(14) Uani 0.50 1 d P . . N1 N 0.6107(4) 0.3955(3) 0.4229(2) 0.0138(7) Uani 1 1 d . . . N2 N 0.7515(4) 0.5204(3) 0.4023(2) 0.0121(7) Uani 1 1 d . . . N3 N 0.7664(4) 0.5089(3) 0.5629(2) 0.0158(7) Uani 1 1 d . . . N4 N 0.8188(4) 0.0431(3) 1.0048(2) 0.0144(7) Uani 1 1 d . . . N5 N 0.9307(3) 0.1856(3) 0.9936(2) 0.0130(7) Uani 1 1 d . . . N6 N 0.9057(4) 0.1870(3) 1.1588(2) 0.0165(7) Uani 1 1 d . . . C1 C 0.5371(4) 0.3270(3) 0.4405(3) 0.0151(8) Uani 1 1 d . . . H1 H 0.5045 0.2967 0.5005 0.018 Uiso 1 1 calc R . . C2 C 0.5082(5) 0.3001(4) 0.3720(3) 0.0221(10) Uani 1 1 d . . . H2 H 0.4547 0.2540 0.3862 0.027 Uiso 1 1 calc R . . C3 C 0.5587(5) 0.3418(4) 0.2831(3) 0.0230(10) Uani 1 1 d . . . H3 H 0.5417 0.3231 0.2363 0.028 Uiso 1 1 calc R . . C4 C 0.6354(5) 0.4120(4) 0.2640(3) 0.0185(9) Uani 1 1 d . . . H4 H 0.6700 0.4418 0.2042 0.022 Uiso 1 1 calc R . . C5 C 0.6600(4) 0.4374(3) 0.3347(3) 0.0140(8) Uani 1 1 d . . . C6 C 0.7405(4) 0.5115(3) 0.3230(3) 0.0128(8) Uani 1 1 d . . . C7 C 0.8012(4) 0.5683(3) 0.2421(3) 0.0148(8) Uani 1 1 d . . . H7 H 0.7958 0.5605 0.1868 0.018 Uiso 1 1 calc R . . C8 C 0.8706(4) 0.6375(3) 0.2441(3) 0.0129(8) Uani 1 1 d . . . C9 C 0.8757(4) 0.6469(3) 0.3290(3) 0.0148(8) Uani 1 1 d . . . H9 H 0.9182 0.6938 0.3331 0.018 Uiso 1 1 calc R . . C10 C 0.8171(4) 0.5857(3) 0.4061(3) 0.0150(8) Uani 1 1 d . . . C11 C 0.8232(4) 0.5820(3) 0.4991(3) 0.0162(8) Uani 1 1 d . . . C12 C 0.8822(5) 0.6449(4) 0.5196(3) 0.0233(10) Uani 1 1 d . . . H12 H 0.9187 0.6951 0.4748 0.028 Uiso 1 1 calc R . . C13 C 0.8851(6) 0.6306(4) 0.6100(3) 0.0288(11) Uani 1 1 d . . . H13 H 0.9237 0.6718 0.6264 0.035 Uiso 1 1 calc R . . C14 C 0.8307(5) 0.5554(4) 0.6747(3) 0.0271(11) Uani 1 1 d . . . H14 H 0.8336 0.5445 0.7349 0.033 Uiso 1 1 calc R . . C15 C 0.7713(5) 0.4961(4) 0.6488(3) 0.0217(9) Uani 1 1 d . . . H15 H 0.7338 0.4458 0.6927 0.026 Uiso 1 1 calc R . . C16 C 0.7520(5) -0.0291(3) 1.0186(3) 0.0183(9) Uani 1 1 d . . . H16 H 0.7179 -0.0610 1.0777 0.022 Uiso 1 1 calc R . . C17 C 0.7324(5) -0.0575(4) 0.9462(3) 0.0225(10) Uani 1 1 d . . . H17 H 0.6851 -0.1071 0.9570 0.027 Uiso 1 1 calc R . . C18 C 0.7849(5) -0.0102(4) 0.8581(3) 0.0208(9) Uani 1 1 d . . . H18 H 0.7722 -0.0276 0.8091 0.025 Uiso 1 1 calc R . . C19 C 0.8564(5) 0.0633(3) 0.8434(3) 0.0185(9) Uani 1 1 d . . . H19 H 0.8936 0.0947 0.7848 0.022 Uiso 1 1 calc R . . C20 C 0.8707(4) 0.0883(3) 0.9182(3) 0.0143(8) Uani 1 1 d . . . C21 C 0.9392(4) 0.1685(3) 0.9124(3) 0.0143(8) Uani 1 1 d . . . C22 C 1.0050(4) 0.2243(3) 0.8336(3) 0.0151(8) Uani 1 1 d . . . H22 H 1.0113 0.2120 0.7772 0.018 Uiso 1 1 calc R . . C23 C 1.0619(4) 0.2997(3) 0.8399(3) 0.0142(8) Uani 1 1 d . . . C24 C 1.0517(4) 0.3147(3) 0.9263(3) 0.0145(8) Uani 1 1 d . . . H24 H 1.0888 0.3637 0.9326 0.017 Uiso 1 1 calc R . . C25 C 0.9853(4) 0.2551(3) 1.0022(3) 0.0129(8) Uani 1 1 d . . . C26 C 0.9706(4) 0.2573(3) 1.0982(3) 0.0153(8) Uani 1 1 d . . . C27 C 1.0229(5) 0.3183(4) 1.1252(3) 0.0232(10) Uani 1 1 d . . . H27 H 1.0652 0.3669 1.0827 0.028 Uiso 1 1 calc R . . C28 C 1.0119(5) 0.3064(4) 1.2178(3) 0.0276(11) Uani 1 1 d . . . H28 H 1.0470 0.3471 1.2376 0.033 Uiso 1 1 calc R . . C29 C 0.9484(5) 0.2337(4) 1.2798(3) 0.0242(10) Uani 1 1 d . . . H29 H 0.9410 0.2242 1.3416 0.029 Uiso 1 1 calc R . . C30 C 0.8960(5) 0.1751(4) 1.2476(3) 0.0195(9) Uani 1 1 d . . . H30 H 0.8529 0.1262 1.2888 0.023 Uiso 1 1 calc R . . C31 C 0.5120(5) 0.2587(4) 0.8009(3) 0.0174(9) Uani 1 1 d . . . H31A H 0.4165 0.2937 0.8144 0.021 Uiso 1 1 calc R . . H31B H 0.5206 0.1850 0.8277 0.021 Uiso 1 1 calc R . . C32 C 0.5774(5) 0.3015(3) 0.8504(3) 0.0161(8) Uani 1 1 d . . . H32A H 0.5472 0.3775 0.8396 0.019 Uiso 1 1 calc R . . H32B H 0.6746 0.2813 0.8277 0.019 Uiso 1 1 calc R . . C33 C 0.5382(5) 0.2572(3) 0.9531(3) 0.0167(8) Uani 1 1 d . . . H33A H 0.5806 0.1824 0.9625 0.020 Uiso 1 1 calc R . . H33B H 0.4415 0.2659 0.9712 0.020 Uiso 1 1 calc R . . C34 C 0.6993(6) -0.0909(4) 0.6055(4) 0.0380(13) Uani 1 1 d . . . H34A H 0.6856 -0.1405 0.5780 0.046 Uiso 1 1 calc R . 1 H34B H 0.7235 -0.1289 0.6619 0.046 Uiso 1 1 calc R . 1 C35 C 0.5454(5) 0.0553(4) 1.3033(4) 0.0370(13) Uani 1 1 d . . . H35A H 0.5620 0.1058 1.3280 0.044 Uiso 1 1 calc R . 1 H35B H 0.5168 0.0916 1.2479 0.044 Uiso 1 1 calc R . 1 C36 C 0.4316(6) 0.0076(4) 1.3734(4) 0.0386(13) Uani 1 1 d . . . H36A H 0.4173 -0.0445 1.3491 0.046 Uiso 1 1 calc R . . H36B H 0.4598 -0.0273 1.4290 0.046 Uiso 1 1 calc R . . H7' H 0.715(5) -0.020(4) 0.420(3) 0.017(12) 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 0.0175(3) 0.0122(2) 0.0080(2) 0.00053(17) -0.00406(18) -0.0084(2) Cu2 0.0190(3) 0.0170(3) 0.0093(2) 0.00039(18) -0.00299(19) -0.0112(2) V1 0.0212(4) 0.0125(3) 0.0106(3) -0.0012(2) -0.0043(3) -0.0077(3) V2 0.0186(4) 0.0186(4) 0.0111(3) -0.0012(3) -0.0044(3) -0.0072(3) P1 0.0223(6) 0.0182(5) 0.0087(5) 0.0007(4) -0.0032(4) -0.0138(5) P2 0.0197(5) 0.0177(5) 0.0126(5) -0.0027(4) -0.0055(4) -0.0064(4) P3 0.0108(7) 0.0152(7) 0.0162(19) -0.0055(7) 0.0010(7) -0.0083(5) P4 0.0139(11) 0.0127(15) 0.0111(7) 0.0009(7) -0.0009(6) -0.0083(10) P3B 0.034(4) 0.025(3) 0.010(7) -0.006(3) -0.007(3) -0.007(3) P4B 0.034(7) 0.007(5) 0.038(5) 0.007(3) -0.001(4) -0.005(5) O1 0.0196(15) 0.0175(15) 0.0106(13) -0.0004(11) -0.0013(11) -0.0099(12) O2 0.0235(16) 0.0177(15) 0.0134(14) 0.0009(12) -0.0015(12) -0.0067(13) O3 0.039(2) 0.039(2) 0.0161(16) 0.0038(15) -0.0089(15) -0.0307(17) O4 0.0352(19) 0.0158(16) 0.0152(15) 0.0010(12) 0.0021(14) -0.0093(14) O5 0.040(2) 0.039(2) 0.0167(16) -0.0053(14) -0.0085(15) -0.0205(17) O6 0.0238(17) 0.0178(16) 0.0187(15) -0.0020(12) -0.0019(13) -0.0064(13) O7 0.039(2) 0.039(2) 0.046(2) -0.0007(19) -0.0176(19) -0.0133(19) O8 0.038(2) 0.0248(19) 0.041(2) -0.0183(16) 0.0089(17) -0.0174(16) O9 0.0238(17) 0.0264(17) 0.0150(15) -0.0016(12) -0.0049(13) -0.0124(14) O10 0.0332(19) 0.0296(18) 0.0155(15) -0.0054(13) -0.0082(14) -0.0090(15) O11 0.0297(18) 0.0218(17) 0.0247(17) -0.0024(13) -0.0070(14) -0.0129(14) O12 0.0244(17) 0.0225(16) 0.0197(16) -0.0054(13) -0.0094(13) -0.0034(14) O13 0.0211(16) 0.0251(17) 0.0152(15) -0.0040(12) -0.0060(12) -0.0057(13) O14 0.0247(17) 0.0273(17) 0.0154(15) 0.0047(13) -0.0015(13) -0.0197(14) O15 0.039(2) 0.039(2) 0.0242(18) -0.0025(15) -0.0014(16) -0.0288(18) O16 0.053(3) 0.051(3) 0.036(2) 0.0116(19) -0.017(2) -0.029(2) O90 0.032(4) 0.040(4) 0.008(3) -0.006(3) -0.002(3) -0.025(3) N1 0.0193(18) 0.0158(17) 0.0096(15) -0.0018(13) -0.0035(13) -0.0096(14) N2 0.0178(17) 0.0111(16) 0.0091(15) -0.0011(12) -0.0050(13) -0.0051(13) N3 0.0208(18) 0.0191(18) 0.0113(16) -0.0014(13) -0.0052(14) -0.0104(15) N4 0.0179(18) 0.0132(17) 0.0133(16) 0.0002(13) -0.0037(14) -0.0081(14) N5 0.0154(17) 0.0157(17) 0.0094(15) 0.0012(13) -0.0039(13) -0.0083(14) N6 0.0198(18) 0.0206(18) 0.0123(17) 0.0013(14) -0.0047(14) -0.0125(15) C1 0.021(2) 0.016(2) 0.0108(18) -0.0006(15) -0.0022(16) -0.0113(17) C2 0.032(3) 0.024(2) 0.018(2) -0.0054(18) -0.0022(19) -0.020(2) C3 0.033(3) 0.027(2) 0.016(2) -0.0088(18) -0.0024(19) -0.017(2) C4 0.030(2) 0.022(2) 0.0090(18) -0.0022(16) -0.0050(17) -0.0135(19) C5 0.019(2) 0.0140(19) 0.0093(18) -0.0004(14) -0.0021(15) -0.0083(16) C6 0.018(2) 0.0118(18) 0.0095(18) -0.0002(14) -0.0041(15) -0.0059(16) C7 0.025(2) 0.0135(19) 0.0083(18) 0.0008(14) -0.0044(16) -0.0092(17) C8 0.0146(19) 0.0154(19) 0.0107(18) -0.0029(15) -0.0047(15) -0.0046(16) C9 0.020(2) 0.0135(19) 0.0118(19) -0.0009(15) -0.0041(16) -0.0068(16) C10 0.020(2) 0.016(2) 0.0106(18) 0.0011(15) -0.0042(16) -0.0097(17) C11 0.023(2) 0.018(2) 0.0118(19) -0.0002(15) -0.0077(16) -0.0097(17) C12 0.036(3) 0.029(2) 0.013(2) 0.0025(18) -0.0079(19) -0.023(2) C13 0.043(3) 0.041(3) 0.015(2) 0.000(2) -0.011(2) -0.029(3) C14 0.040(3) 0.037(3) 0.013(2) 0.0005(19) -0.010(2) -0.022(2) C15 0.026(2) 0.031(3) 0.012(2) 0.0022(17) -0.0058(17) -0.016(2) C16 0.024(2) 0.017(2) 0.017(2) 0.0005(16) -0.0041(17) -0.0132(18) C17 0.029(3) 0.018(2) 0.026(2) -0.0029(18) -0.007(2) -0.0148(19) C18 0.028(2) 0.023(2) 0.018(2) -0.0059(17) -0.0069(18) -0.0121(19) C19 0.026(2) 0.016(2) 0.015(2) -0.0022(16) -0.0039(17) -0.0091(18) C20 0.017(2) 0.015(2) 0.0110(18) -0.0017(15) -0.0013(15) -0.0075(16) C21 0.018(2) 0.0136(19) 0.0131(19) -0.0001(15) -0.0053(16) -0.0077(16) C22 0.020(2) 0.016(2) 0.0114(18) -0.0018(15) -0.0026(16) -0.0088(17) C23 0.018(2) 0.0131(19) 0.0104(18) 0.0008(14) -0.0033(15) -0.0047(16) C24 0.016(2) 0.0138(19) 0.0153(19) -0.0003(15) -0.0042(16) -0.0084(16) C25 0.017(2) 0.0131(19) 0.0093(18) -0.0011(14) -0.0042(15) -0.0041(16) C26 0.019(2) 0.016(2) 0.0130(19) 0.0005(15) -0.0050(16) -0.0088(17) C27 0.034(3) 0.030(3) 0.013(2) 0.0003(18) -0.0061(19) -0.021(2) C28 0.043(3) 0.038(3) 0.016(2) -0.0007(19) -0.010(2) -0.029(2) C29 0.034(3) 0.037(3) 0.0089(19) -0.0010(18) -0.0067(18) -0.020(2) C30 0.025(2) 0.027(2) 0.0101(19) 0.0007(16) -0.0029(17) -0.0161(19) C31 0.022(2) 0.021(2) 0.0125(19) -0.0016(16) -0.0055(16) -0.0096(18) C32 0.023(2) 0.019(2) 0.0097(18) -0.0033(15) -0.0055(16) -0.0070(17) C33 0.023(2) 0.015(2) 0.0124(19) -0.0011(15) -0.0051(16) -0.0061(17) C34 0.032(3) 0.031(3) 0.049(3) -0.009(3) 0.000(3) -0.013(2) C35 0.022(3) 0.035(3) 0.052(4) -0.016(3) 0.006(2) -0.015(2) C36 0.030(3) 0.032(3) 0.051(4) -0.006(3) -0.002(3) -0.012(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 O1 1.920(3) . ? Cu1 N2 1.946(3) . ? Cu1 N3 2.032(4) . ? Cu1 N1 2.055(3) . ? Cu1 O2 2.142(3) . ? Cu2 O14 1.882(3) . ? Cu2 N5 1.940(3) . ? Cu2 N6 2.024(4) . ? Cu2 N4 2.054(3) . ? Cu2 O13 2.224(3) . ? V1 O5 1.624(3) . ? V1 O2 1.643(3) . ? V1 O8 1.953(3) . ? V1 O6 1.981(3) . ? V1 O4 1.992(3) . ? V2 O10 1.612(3) . ? V2 O9 1.619(3) . ? V2 O12 1.857(3) 2_667 ? V2 O11 1.867(3) . ? P1 O4 1.510(4) . ? P1 O1 1.517(3) . ? P1 O3 1.533(3) . ? P1 C31 1.800(4) . ? P2 O13 1.496(3) . ? P2 O11 1.553(3) . ? P2 O12 1.561(3) . ? P2 C33 1.810(4) . ? P3 O6 1.502(3) 2_756 ? P3 O8 1.525(5) . ? P3 O7 1.544(6) . ? P3 C34 1.796(6) . ? P4 O15 1.503(4) . ? P4 O14 1.512(3) . ? P4 O16 1.542(5) . ? P4 C35 1.789(7) . ? P3B C34 1.619(10) . ? P3B O6 1.635(12) 2_756 ? P4B O14 1.641(15) . ? O3 H3' 0.8200 . ? O6 P3 1.502(3) 2_756 ? O6 P3B 1.635(12) 2_756 ? O7 H7' 1.29(5) . ? O12 V2 1.857(3) 2_667 ? N1 C1 1.342(5) . ? N1 C5 1.360(5) . ? N2 C10 1.336(5) . ? N2 C6 1.337(5) . ? N3 C15 1.336(5) . ? N3 C11 1.363(5) . ? N4 C16 1.342(5) . ? N4 C20 1.360(5) . ? N5 C25 1.329(5) . ? N5 C21 1.337(5) . ? N6 C30 1.341(5) . ? N6 C26 1.360(5) . ? C1 C2 1.384(6) . ? C1 H1 0.9300 . ? C2 C3 1.370(6) . ? C2 H2 0.9300 . ? C3 C4 1.384(6) . ? C3 H3 0.9300 . ? C4 C5 1.380(6) . ? C4 H4 0.9300 . ? C5 C6 1.483(6) . ? C6 C7 1.390(5) . ? C7 C8 1.400(6) . ? C7 H7 0.9300 . ? C8 C9 1.403(5) . ? C8 C23 1.486(6) 2_766 ? C9 C10 1.375(5) . ? C9 H9 0.9300 . ? C10 C11 1.478(5) . ? C11 C12 1.379(6) . ? C12 C13 1.398(6) . ? C12 H12 0.9300 . ? C13 C14 1.376(7) . ? C13 H13 0.9300 . ? C14 C15 1.391(6) . ? C14 H14 0.9300 . ? C15 H15 0.9300 . ? C16 C17 1.398(6) . ? C16 H16 0.9300 . ? C17 C18 1.389(6) . ? C17 H17 0.9300 . ? C18 C19 1.391(6) . ? C18 H18 0.9300 . ? C19 C20 1.383(6) . ? C19 H19 0.9300 . ? C20 C21 1.486(6) . ? C21 C22 1.383(6) . ? C22 C23 1.405(6) . ? C22 H22 0.9300 . ? C23 C24 1.400(6) . ? C23 C8 1.486(6) 2_766 ? C24 C25 1.387(5) . ? C24 H24 0.9300 . ? C25 C26 1.481(5) . ? C26 C27 1.364(6) . ? C27 C28 1.398(6) . ? C27 H27 0.9300 . ? C28 C29 1.383(6) . ? C28 H28 0.9300 . ? C29 C30 1.390(6) . ? C29 H29 0.9300 . ? C30 H30 0.9300 . ? C31 C32 1.527(6) . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C32 C33 1.541(5) . ? C32 H32A 0.9700 . ? C32 H32B 0.9700 . ? C33 H33A 0.9700 . ? C33 H33B 0.9700 . ? C34 C36 1.512(8) 2_657 ? C34 H34A 0.9700 . ? C34 H34B 0.9700 . ? C35 C36 1.562(7) . ? C35 H35A 0.9700 . ? C35 H35B 0.9700 . ? C36 C34 1.512(8) 2_657 ? C36 H36A 0.9700 . ? C36 H36B 0.9700 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Cu1 N2 164.57(14) . . ? O1 Cu1 N3 93.57(13) . . ? N2 Cu1 N3 79.81(14) . . ? O1 Cu1 N1 106.31(13) . . ? N2 Cu1 N1 78.74(14) . . ? N3 Cu1 N1 158.25(14) . . ? O1 Cu1 O2 94.38(12) . . ? N2 Cu1 O2 100.46(13) . . ? N3 Cu1 O2 99.84(14) . . ? N1 Cu1 O2 87.60(13) . . ? O14 Cu2 N5 158.97(15) . . ? O14 Cu2 N6 95.18(14) . . ? N5 Cu2 N6 79.77(14) . . ? O14 Cu2 N4 101.00(14) . . ? N5 Cu2 N4 79.61(14) . . ? N6 Cu2 N4 157.64(14) . . ? O14 Cu2 O13 105.88(13) . . ? N5 Cu2 O13 95.04(13) . . ? N6 Cu2 O13 97.35(13) . . ? N4 Cu2 O13 92.97(13) . . ? O5 V1 O2 108.28(18) . . ? O5 V1 O8 122.99(18) . . ? O2 V1 O8 128.73(17) . . ? O5 V1 O6 97.16(16) . . ? O2 V1 O6 89.69(14) . . ? O8 V1 O6 84.60(14) . . ? O5 V1 O4 93.78(16) . . ? O2 V1 O4 95.46(14) . . ? O8 V1 O4 81.86(14) . . ? O6 V1 O4 165.80(14) . . ? O10 V2 O9 107.67(17) . . ? O10 V2 O12 110.12(16) . 2_667 ? O9 V2 O12 110.93(16) . 2_667 ? O10 V2 O11 113.75(16) . . ? O9 V2 O11 106.04(16) . . ? O12 V2 O11 108.28(15) 2_667 . ? O4 P1 O1 113.39(18) . . ? O4 P1 O3 113.3(2) . . ? O1 P1 O3 108.58(19) . . ? O4 P1 C31 106.1(2) . . ? O1 P1 C31 110.81(19) . . ? O3 P1 C31 104.3(2) . . ? O13 P2 O11 113.28(19) . . ? O13 P2 O12 111.41(18) . . ? O11 P2 O12 107.08(19) . . ? O13 P2 C33 110.97(19) . . ? O11 P2 C33 106.49(19) . . ? O12 P2 C33 107.27(19) . . ? O6 P3 O8 111.2(3) 2_756 . ? O6 P3 O7 113.5(3) 2_756 . ? O8 P3 O7 111.9(3) . . ? O6 P3 C34 103.6(3) 2_756 . ? O8 P3 C34 107.8(3) . . ? O7 P3 C34 108.4(3) . . ? O15 P4 O14 111.4(2) . . ? O15 P4 O16 109.5(3) . . ? O14 P4 O16 111.5(3) . . ? O15 P4 C35 107.5(3) . . ? O14 P4 C35 106.7(3) . . ? O16 P4 C35 110.2(3) . . ? C34 P3B O6 106.0(5) . 2_756 ? P1 O1 Cu1 130.83(19) . . ? V1 O2 Cu1 137.98(17) . . ? P1 O3 H3' 109.5 . . ? P1 O4 V1 137.27(19) . . ? P3 O6 P3B 23.2(5) 2_756 2_756 ? P3 O6 V1 133.0(3) 2_756 . ? P3B O6 V1 151.1(5) 2_756 . ? P3 O7 H7' 116(2) . . ? P3 O8 V1 152.3(3) . . ? P2 O11 V2 136.0(2) . . ? P2 O12 V2 141.2(2) . 2_667 ? P2 O13 Cu2 133.30(19) . . ? P4 O14 P4B 21.5(5) . . ? P4 O14 Cu2 147.1(3) . . ? P4B O14 Cu2 126.9(7) . . ? C1 N1 C5 118.3(3) . . ? C1 N1 Cu1 126.9(3) . . ? C5 N1 Cu1 114.3(3) . . ? C10 N2 C6 121.2(4) . . ? C10 N2 Cu1 118.6(3) . . ? C6 N2 Cu1 120.1(3) . . ? C15 N3 C11 118.2(4) . . ? C15 N3 Cu1 127.2(3) . . ? C11 N3 Cu1 114.6(3) . . ? C16 N4 C20 119.0(4) . . ? C16 N4 Cu2 126.5(3) . . ? C20 N4 Cu2 113.9(3) . . ? C25 N5 C21 121.9(4) . . ? C25 N5 Cu2 118.8(3) . . ? C21 N5 Cu2 119.2(3) . . ? C30 N6 C26 119.2(4) . . ? C30 N6 Cu2 126.4(3) . . ? C26 N6 Cu2 114.4(3) . . ? N1 C1 C2 122.0(4) . . ? N1 C1 H1 119.0 . . ? C2 C1 H1 119.0 . . ? C3 C2 C1 119.7(4) . . ? C3 C2 H2 120.2 . . ? C1 C2 H2 120.2 . . ? C2 C3 C4 118.9(4) . . ? C2 C3 H3 120.5 . . ? C4 C3 H3 120.5 . . ? C5 C4 C3 119.2(4) . . ? C5 C4 H4 120.4 . . ? C3 C4 H4 120.4 . . ? N1 C5 C4 121.9(4) . . ? N1 C5 C6 113.8(3) . . ? C4 C5 C6 124.3(4) . . ? N2 C6 C7 120.3(4) . . ? N2 C6 C5 112.3(3) . . ? C7 C6 C5 127.5(4) . . ? C6 C7 C8 119.7(4) . . ? C6 C7 H7 120.2 . . ? C8 C7 H7 120.2 . . ? C7 C8 C9 118.1(4) . . ? C7 C8 C23 122.4(4) . 2_766 ? C9 C8 C23 119.5(4) . 2_766 ? C10 C9 C8 119.1(4) . . ? C10 C9 H9 120.5 . . ? C8 C9 H9 120.5 . . ? N2 C10 C9 121.6(4) . . ? N2 C10 C11 113.6(4) . . ? C9 C10 C11 124.8(4) . . ? N3 C11 C12 123.0(4) . . ? N3 C11 C10 113.4(4) . . ? C12 C11 C10 123.6(4) . . ? C11 C12 C13 117.6(4) . . ? C11 C12 H12 121.2 . . ? C13 C12 H12 121.2 . . ? C14 C13 C12 119.9(4) . . ? C14 C13 H13 120.1 . . ? C12 C13 H13 120.1 . . ? C13 C14 C15 119.0(4) . . ? C13 C14 H14 120.5 . . ? C15 C14 H14 120.5 . . ? N3 C15 C14 122.2(4) . . ? N3 C15 H15 118.9 . . ? C14 C15 H15 118.9 . . ? N4 C16 C17 121.7(4) . . ? N4 C16 H16 119.2 . . ? C17 C16 H16 119.2 . . ? C18 C17 C16 118.8(4) . . ? C18 C17 H17 120.6 . . ? C16 C17 H17 120.6 . . ? C17 C18 C19 119.8(4) . . ? C17 C18 H18 120.1 . . ? C19 C18 H18 120.1 . . ? C20 C19 C18 118.3(4) . . ? C20 C19 H19 120.9 . . ? C18 C19 H19 120.9 . . ? N4 C20 C19 122.5(4) . . ? N4 C20 C21 113.7(3) . . ? C19 C20 C21 123.8(4) . . ? N5 C21 C22 120.5(4) . . ? N5 C21 C20 113.1(3) . . ? C22 C21 C20 126.4(4) . . ? C21 C22 C23 119.2(4) . . ? C21 C22 H22 120.4 . . ? C23 C22 H22 120.4 . . ? C24 C23 C22 118.5(4) . . ? C24 C23 C8 121.6(4) . 2_766 ? C22 C23 C8 119.9(4) . 2_766 ? C25 C24 C23 119.0(4) . . ? C25 C24 H24 120.5 . . ? C23 C24 H24 120.5 . . ? N5 C25 C24 120.8(4) . . ? N5 C25 C26 113.0(3) . . ? C24 C25 C26 126.1(4) . . ? N6 C26 C27 121.9(4) . . ? N6 C26 C25 113.4(4) . . ? C27 C26 C25 124.5(4) . . ? C26 C27 C28 118.9(4) . . ? C26 C27 H27 120.6 . . ? C28 C27 H27 120.6 . . ? C29 C28 C27 119.6(4) . . ? C29 C28 H28 120.2 . . ? C27 C28 H28 120.2 . . ? C28 C29 C30 118.4(4) . . ? C28 C29 H29 120.8 . . ? C30 C29 H29 120.8 . . ? N6 C30 C29 122.0(4) . . ? N6 C30 H30 119.0 . . ? C29 C30 H30 119.0 . . ? C32 C31 P1 119.9(3) . . ? C32 C31 H31A 107.3 . . ? P1 C31 H31A 107.3 . . ? C32 C31 H31B 107.3 . . ? P1 C31 H31B 107.3 . . ? H31A C31 H31B 106.9 . . ? C31 C32 C33 109.4(3) . . ? C31 C32 H32A 109.8 . . ? C33 C32 H32A 109.8 . . ? C31 C32 H32B 109.8 . . ? C33 C32 H32B 109.8 . . ? H32A C32 H32B 108.3 . . ? C32 C33 P2 118.1(3) . . ? C32 C33 H33A 107.8 . . ? P2 C33 H33A 107.8 . . ? C32 C33 H33B 107.8 . . ? P2 C33 H33B 107.8 . . ? H33A C33 H33B 107.1 . . ? C36 C34 P3B 112.9(5) 2_657 . ? C36 C34 P3 113.5(4) 2_657 . ? P3B C34 P3 21.0(6) . . ? C36 C34 H34A 108.9 2_657 . ? P3B C34 H34A 125.6 . . ? P3 C34 H34A 108.9 . . ? C36 C34 H34B 108.9 2_657 . ? P3B C34 H34B 90.3 . . ? P3 C34 H34B 108.9 . . ? H34A C34 H34B 107.7 . . ? C36 C35 P4 110.4(4) . . ? C36 C35 H35A 109.6 . . ? P4 C35 H35A 109.6 . . ? C36 C35 H35B 109.6 . . ? P4 C35 H35B 109.6 . . ? H35A C35 H35B 108.1 . . ? C34 C36 C35 111.7(5) 2_657 . ? C34 C36 H36A 109.3 2_657 . ? C35 C36 H36A 109.3 . . ? C34 C36 H36B 109.3 2_657 . ? C35 C36 H36B 109.3 . . ? H36A C36 H36B 107.9 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O4 P1 O1 Cu1 40.4(3) . . . . ? O3 P1 O1 Cu1 -86.4(3) . . . . ? C31 P1 O1 Cu1 159.6(2) . . . . ? N2 Cu1 O1 P1 168.3(4) . . . . ? N3 Cu1 O1 P1 -127.8(3) . . . . ? N1 Cu1 O1 P1 61.1(3) . . . . ? O2 Cu1 O1 P1 -27.7(3) . . . . ? O5 V1 O2 Cu1 -77.0(3) . . . . ? O8 V1 O2 Cu1 102.7(3) . . . . ? O6 V1 O2 Cu1 -174.4(3) . . . . ? O4 V1 O2 Cu1 18.8(3) . . . . ? O1 Cu1 O2 V1 -8.0(3) . . . . ? N2 Cu1 O2 V1 167.7(3) . . . . ? N3 Cu1 O2 V1 86.4(3) . . . . ? N1 Cu1 O2 V1 -114.2(3) . . . . ? O1 P1 O4 V1 -20.6(4) . . . . ? O3 P1 O4 V1 103.7(3) . . . . ? C31 P1 O4 V1 -142.5(3) . . . . ? O5 V1 O4 P1 103.8(3) . . . . ? O2 V1 O4 P1 -5.0(3) . . . . ? O8 V1 O4 P1 -133.4(3) . . . . ? O6 V1 O4 P1 -115.8(5) . . . . ? O5 V1 O6 P3 68.6(3) . . . 2_756 ? O2 V1 O6 P3 177.0(3) . . . 2_756 ? O8 V1 O6 P3 -54.0(3) . . . 2_756 ? O4 V1 O6 P3 -71.5(7) . . . 2_756 ? O5 V1 O6 P3B 93.1(12) . . . 2_756 ? O2 V1 O6 P3B -158.5(12) . . . 2_756 ? O8 V1 O6 P3B -29.5(12) . . . 2_756 ? O4 V1 O6 P3B -47.0(14) . . . 2_756 ? O6 P3 O8 V1 113.3(6) 2_756 . . . ? O7 P3 O8 V1 -14.8(6) . . . . ? C34 P3 O8 V1 -133.8(5) . . . . ? O5 V1 O8 P3 -152.7(5) . . . . ? O2 V1 O8 P3 27.5(6) . . . . ? O6 V1 O8 P3 -57.7(5) . . . . ? O4 V1 O8 P3 118.0(6) . . . . ? O13 P2 O11 V2 -104.5(3) . . . . ? O12 P2 O11 V2 18.8(3) . . . . ? C33 P2 O11 V2 133.3(3) . . . . ? O10 V2 O11 P2 61.7(3) . . . . ? O9 V2 O11 P2 179.8(3) . . . . ? O12 V2 O11 P2 -61.1(3) 2_667 . . . ? O13 P2 O12 V2 -158.7(3) . . . 2_667 ? O11 P2 O12 V2 76.9(4) . . . 2_667 ? C33 P2 O12 V2 -37.1(4) . . . 2_667 ? O11 P2 O13 Cu2 -43.2(3) . . . . ? O12 P2 O13 Cu2 -164.0(2) . . . . ? C33 P2 O13 Cu2 76.5(3) . . . . ? O14 Cu2 O13 P2 -162.1(3) . . . . ? N5 Cu2 O13 P2 20.1(3) . . . . ? N6 Cu2 O13 P2 100.4(3) . . . . ? N4 Cu2 O13 P2 -59.8(3) . . . . ? O15 P4 O14 P4B 103.9(11) . . . . ? O16 P4 O14 P4B -133.4(13) . . . . ? C35 P4 O14 P4B -13.1(11) . . . . ? O15 P4 O14 Cu2 79.0(6) . . . . ? O16 P4 O14 Cu2 -158.3(4) . . . . ? C35 P4 O14 Cu2 -38.0(5) . . . . ? N5 Cu2 O14 P4 -163.8(4) . . . . ? N6 Cu2 O14 P4 121.3(5) . . . . ? N4 Cu2 O14 P4 -74.2(5) . . . . ? O13 Cu2 O14 P4 22.2(5) . . . . ? N5 Cu2 O14 P4B -175.0(5) . . . . ? N6 Cu2 O14 P4B 110.2(5) . . . . ? N4 Cu2 O14 P4B -85.3(5) . . . . ? O13 Cu2 O14 P4B 11.0(5) . . . . ? O1 Cu1 N1 C1 -15.6(4) . . . . ? N2 Cu1 N1 C1 179.4(4) . . . . ? N3 Cu1 N1 C1 -170.9(4) . . . . ? O2 Cu1 N1 C1 78.3(4) . . . . ? O1 Cu1 N1 C5 172.9(3) . . . . ? N2 Cu1 N1 C5 7.9(3) . . . . ? N3 Cu1 N1 C5 17.6(6) . . . . ? O2 Cu1 N1 C5 -93.3(3) . . . . ? O1 Cu1 N2 C10 65.3(6) . . . . ? N3 Cu1 N2 C10 -0.2(3) . . . . ? N1 Cu1 N2 C10 176.1(3) . . . . ? O2 Cu1 N2 C10 -98.5(3) . . . . ? O1 Cu1 N2 C6 -118.2(5) . . . . ? N3 Cu1 N2 C6 176.2(3) . . . . ? N1 Cu1 N2 C6 -7.4(3) . . . . ? O2 Cu1 N2 C6 78.0(3) . . . . ? O1 Cu1 N3 C15 15.4(4) . . . . ? N2 Cu1 N3 C15 -178.6(4) . . . . ? N1 Cu1 N3 C15 171.7(4) . . . . ? O2 Cu1 N3 C15 -79.6(4) . . . . ? O1 Cu1 N3 C11 -164.0(3) . . . . ? N2 Cu1 N3 C11 2.0(3) . . . . ? N1 Cu1 N3 C11 -7.7(6) . . . . ? O2 Cu1 N3 C11 100.9(3) . . . . ? O14 Cu2 N4 C16 24.2(4) . . . . ? N5 Cu2 N4 C16 -177.2(4) . . . . ? N6 Cu2 N4 C16 159.8(4) . . . . ? O13 Cu2 N4 C16 -82.6(4) . . . . ? O14 Cu2 N4 C20 -164.4(3) . . . . ? N5 Cu2 N4 C20 -5.8(3) . . . . ? N6 Cu2 N4 C20 -28.8(6) . . . . ? O13 Cu2 N4 C20 88.8(3) . . . . ? O14 Cu2 N5 C25 -84.2(5) . . . . ? N6 Cu2 N5 C25 -6.6(3) . . . . ? N4 Cu2 N5 C25 -177.9(3) . . . . ? O13 Cu2 N5 C25 90.0(3) . . . . ? O14 Cu2 N5 C21 97.7(5) . . . . ? N6 Cu2 N5 C21 175.3(3) . . . . ? N4 Cu2 N5 C21 4.0(3) . . . . ? O13 Cu2 N5 C21 -88.1(3) . . . . ? O14 Cu2 N6 C30 -14.3(4) . . . . ? N5 Cu2 N6 C30 -173.7(4) . . . . ? N4 Cu2 N6 C30 -150.7(4) . . . . ? O13 Cu2 N6 C30 92.5(4) . . . . ? O14 Cu2 N6 C26 166.1(3) . . . . ? N5 Cu2 N6 C26 6.7(3) . . . . ? N4 Cu2 N6 C26 29.7(6) . . . . ? O13 Cu2 N6 C26 -87.1(3) . . . . ? C5 N1 C1 C2 -1.4(6) . . . . ? Cu1 N1 C1 C2 -172.6(3) . . . . ? N1 C1 C2 C3 1.9(7) . . . . ? C1 C2 C3 C4 -1.4(7) . . . . ? C2 C3 C4 C5 0.6(7) . . . . ? C1 N1 C5 C4 0.6(6) . . . . ? Cu1 N1 C5 C4 172.9(3) . . . . ? C1 N1 C5 C6 -179.6(4) . . . . ? Cu1 N1 C5 C6 -7.3(5) . . . . ? C3 C4 C5 N1 -0.2(7) . . . . ? C3 C4 C5 C6 -180.0(4) . . . . ? C10 N2 C6 C7 1.9(6) . . . . ? Cu1 N2 C6 C7 -174.5(3) . . . . ? C10 N2 C6 C5 -178.1(4) . . . . ? Cu1 N2 C6 C5 5.5(5) . . . . ? N1 C5 C6 N2 1.6(5) . . . . ? C4 C5 C6 N2 -178.6(4) . . . . ? N1 C5 C6 C7 -178.4(4) . . . . ? C4 C5 C6 C7 1.3(7) . . . . ? N2 C6 C7 C8 -1.9(6) . . . . ? C5 C6 C7 C8 178.1(4) . . . . ? C6 C7 C8 C9 -0.2(6) . . . . ? C6 C7 C8 C23 179.8(4) . . . 2_766 ? C7 C8 C9 C10 2.3(6) . . . . ? C23 C8 C9 C10 -177.7(4) 2_766 . . . ? C6 N2 C10 C9 0.3(6) . . . . ? Cu1 N2 C10 C9 176.7(3) . . . . ? C6 N2 C10 C11 -177.8(4) . . . . ? Cu1 N2 C10 C11 -1.4(5) . . . . ? C8 C9 C10 N2 -2.4(6) . . . . ? C8 C9 C10 C11 175.5(4) . . . . ? C15 N3 C11 C12 -1.8(7) . . . . ? Cu1 N3 C11 C12 177.7(4) . . . . ? C15 N3 C11 C10 177.3(4) . . . . ? Cu1 N3 C11 C10 -3.2(5) . . . . ? N2 C10 C11 N3 3.0(6) . . . . ? C9 C10 C11 N3 -175.0(4) . . . . ? N2 C10 C11 C12 -177.9(4) . . . . ? C9 C10 C11 C12 4.1(7) . . . . ? N3 C11 C12 C13 1.2(7) . . . . ? C10 C11 C12 C13 -177.8(5) . . . . ? C11 C12 C13 C14 0.3(8) . . . . ? C12 C13 C14 C15 -1.2(8) . . . . ? C11 N3 C15 C14 0.8(7) . . . . ? Cu1 N3 C15 C14 -178.6(4) . . . . ? C13 C14 C15 N3 0.6(8) . . . . ? C20 N4 C16 C17 -1.2(7) . . . . ? Cu2 N4 C16 C17 169.8(3) . . . . ? N4 C16 C17 C18 0.7(7) . . . . ? C16 C17 C18 C19 0.5(7) . . . . ? C17 C18 C19 C20 -1.2(7) . . . . ? C16 N4 C20 C19 0.6(6) . . . . ? Cu2 N4 C20 C19 -171.5(3) . . . . ? C16 N4 C20 C21 178.6(4) . . . . ? Cu2 N4 C20 C21 6.5(5) . . . . ? C18 C19 C20 N4 0.6(7) . . . . ? C18 C19 C20 C21 -177.2(4) . . . . ? C25 N5 C21 C22 -0.7(6) . . . . ? Cu2 N5 C21 C22 177.4(3) . . . . ? C25 N5 C21 C20 -179.6(4) . . . . ? Cu2 N5 C21 C20 -1.6(5) . . . . ? N4 C20 C21 N5 -3.4(5) . . . . ? C19 C20 C21 N5 174.6(4) . . . . ? N4 C20 C21 C22 177.6(4) . . . . ? C19 C20 C21 C22 -4.3(7) . . . . ? N5 C21 C22 C23 -0.4(6) . . . . ? C20 C21 C22 C23 178.4(4) . . . . ? C21 C22 C23 C24 0.9(6) . . . . ? C21 C22 C23 C8 -178.2(4) . . . 2_766 ? C22 C23 C24 C25 -0.4(6) . . . . ? C8 C23 C24 C25 178.8(4) 2_766 . . . ? C21 N5 C25 C24 1.2(6) . . . . ? Cu2 N5 C25 C24 -176.8(3) . . . . ? C21 N5 C25 C26 -176.8(4) . . . . ? Cu2 N5 C25 C26 5.2(5) . . . . ? C23 C24 C25 N5 -0.7(6) . . . . ? C23 C24 C25 C26 177.0(4) . . . . ? C30 N6 C26 C27 -1.9(7) . . . . ? Cu2 N6 C26 C27 177.7(4) . . . . ? C30 N6 C26 C25 174.5(4) . . . . ? Cu2 N6 C26 C25 -5.9(5) . . . . ? N5 C25 C26 N6 0.7(5) . . . . ? C24 C25 C26 N6 -177.2(4) . . . . ? N5 C25 C26 C27 177.0(4) . . . . ? C24 C25 C26 C27 -0.9(7) . . . . ? N6 C26 C27 C28 1.4(7) . . . . ? C25 C26 C27 C28 -174.5(5) . . . . ? C26 C27 C28 C29 -0.1(8) . . . . ? C27 C28 C29 C30 -0.7(8) . . . . ? C26 N6 C30 C29 1.0(7) . . . . ? Cu2 N6 C30 C29 -178.5(4) . . . . ? C28 C29 C30 N6 0.2(8) . . . . ? O4 P1 C31 C32 74.7(4) . . . . ? O1 P1 C31 C32 -48.9(4) . . . . ? O3 P1 C31 C32 -165.5(3) . . . . ? P1 C31 C32 C33 -164.5(3) . . . . ? C31 C32 C33 P2 -170.2(3) . . . . ? O13 P2 C33 C32 -137.8(3) . . . . ? O11 P2 C33 C32 -14.1(4) . . . . ? O12 P2 C33 C32 100.3(3) . . . . ? O6 P3B C34 C36 -163.6(7) 2_756 . . 2_657 ? O6 P3B C34 P3 -67.3(11) 2_756 . . . ? O6 P3 C34 C36 176.0(5) 2_756 . . 2_657 ? O8 P3 C34 C36 58.1(6) . . . 2_657 ? O7 P3 C34 C36 -63.2(5) . . . 2_657 ? O6 P3 C34 P3B 83.2(8) 2_756 . . . ? O8 P3 C34 P3B -34.7(8) . . . . ? O7 P3 C34 P3B -156.0(8) . . . . ? O15 P4 C35 C36 57.9(5) . . . . ? O14 P4 C35 C36 177.5(4) . . . . ? O16 P4 C35 C36 -61.3(5) . . . . ? P4 C35 C36 C34 -178.5(4) . . . 2_657 ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 28.28 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 1.420 _refine_diff_density_min -0.697 _refine_diff_density_rms 0.141 data_publication_text_compound_7 _database_code_depnum_ccdc_archive 'CCDC 247636' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ; [{Cu6(bisterpy)3}V4O8(OH)2{O3P(CH2)3PO3}2{HO3P(CH2)3PO3}]·5H2O ; _chemical_formula_sum 'C51 H49 Cu3 N9 O19.50 P4 V2' _chemical_formula_weight 1516.37 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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.3517(8) _cell_length_b 14.1008(9) _cell_length_c 15.2997(10) _cell_angle_alpha 77.7850(10) _cell_angle_beta 77.1100(10) _cell_angle_gamma 81.1780(10) _cell_volume 2727.2(3) _cell_formula_units_Z 2 _cell_measurement_temperature 90(2) _cell_measurement_reflns_used 8174 _cell_measurement_theta_min 2.28 _cell_measurement_theta_max 32.90 _exptl_crystal_description block _exptl_crystal_colour black _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.847 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1534 _exptl_absorpt_coefficient_mu 1.687 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4859 _exptl_absorpt_correction_T_max 0.7981 _exptl_absorpt_process_details 'SADABS SHELXL-97 (SHELDRICK, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 90(2) _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_probe x-ray _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'APEX CCD area detector' _diffrn_measurement_method 'Phi and omega scans' _diffrn_detector_area_resol_mean 512 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.001 _diffrn_reflns_number 35777 _diffrn_reflns_av_R_equivalents 0.0343 _diffrn_reflns_av_sigmaI/netI 0.0544 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.84 _diffrn_reflns_theta_max 31.51 _reflns_number_total 17815 _reflns_number_gt 14401 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL and CrystalMaker 5.x' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0477P)^2^+2.5141P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 17815 _refine_ls_number_parameters 804 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0566 _refine_ls_R_factor_gt 0.0427 _refine_ls_wR_factor_ref 0.1086 _refine_ls_wR_factor_gt 0.1014 _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_restrained_S_all 1.024 _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 0.35954(2) 0.328067(19) 0.783276(18) 0.00942(6) Uani 1 1 d . . . Cu2 Cu 0.12324(2) 0.30649(2) 0.614972(18) 0.00987(6) Uani 1 1 d . . . Cu3 Cu -0.04579(2) 0.08983(2) 0.681084(18) 0.00963(6) Uani 1 1 d . . . V1 V 0.26324(4) 0.62371(3) 0.92619(3) 0.02440(11) Uani 1 1 d . . . V2 V -0.17965(3) -0.10553(3) 0.67405(3) 0.00886(7) Uani 1 1 d . . . P1 P 0.43378(5) 0.54150(5) 0.76994(4) 0.01374(12) Uani 1 1 d . . . P2 P 0.25202(4) 0.47210(4) 0.62427(4) 0.00958(11) Uani 1 1 d . . . P3 P 0.03623(4) 0.22538(4) 0.48113(4) 0.00842(10) Uani 1 1 d . . . P4 P -0.37694(4) -0.13001(4) 0.74680(4) 0.01005(11) Uani 1 1 d . . . O1 O 0.1394(2) 0.6518(2) 0.93266(18) 0.0577(9) Uani 1 1 d . . . O2 O 0.3090(3) 0.7227(2) 0.9297(2) 0.0716(11) Uani 1 1 d . . . O3 O 0.32369(15) 0.58470(15) 0.81797(14) 0.0227(4) Uani 1 1 d . . . O4 O 0.44470(15) 0.57625(14) 0.66783(12) 0.0216(4) Uani 1 1 d . . . O5 O 0.44644(15) 0.43249(13) 0.80167(13) 0.0193(4) Uani 1 1 d . . . O6 O 0.26475(13) 0.40417(12) 0.71331(11) 0.0144(3) Uani 1 1 d . . . O7 O 0.35653(13) 0.51015(12) 0.57070(11) 0.0133(3) Uani 1 1 d . . . H7' H 0.3858 0.5283 0.6066 0.020 Uiso 1 1 calc R . . O8 O 0.20878(13) 0.42645(12) 0.56183(11) 0.0127(3) Uani 1 1 d . . . O9 O 0.08249(13) 0.30967(12) 0.49929(11) 0.0130(3) Uani 1 1 d . . . O10 O -0.03054(14) 0.17417(13) 0.56678(12) 0.0165(3) Uani 1 1 d . . . O11 O 0.12014(13) 0.15204(12) 0.43828(11) 0.0125(3) Uani 1 1 d . . . O12 O -0.15298(13) 0.00858(12) 0.64796(11) 0.0134(3) Uani 1 1 d . . . O13 O -0.10244(13) -0.16936(12) 0.73822(11) 0.0139(3) Uani 1 1 d . . . O14 O -0.29603(12) -0.08911(11) 0.78467(11) 0.0104(3) Uani 1 1 d . . . O15 O -0.31239(13) -0.13725(13) 0.65050(11) 0.0145(3) Uani 1 1 d . . . O16 O -0.47988(13) -0.06989(13) 0.75160(12) 0.0161(3) Uani 1 1 d . . . O17 O 0.28382(17) 0.53287(17) 1.01949(14) 0.0326(5) Uani 1 1 d . . . H17' H 0.3387 0.4969 1.0046 0.049 Uiso 1 1 calc R . . O90 O 0.34961(15) 0.91330(14) 0.88711(13) 0.0236(4) Uani 1 1 d . . . O91 O 0.32854(16) 0.44909(18) 0.38199(14) 0.0323(5) Uani 1 1 d . . . O92 O 0.4535(3) 0.3720(3) 0.9791(2) 0.0200(7) Uani 0.50 1 d P . . N1 N 0.25021(15) 0.32965(14) 0.90147(13) 0.0115(4) Uani 1 1 d . . . N2 N 0.40950(15) 0.21061(13) 0.86038(13) 0.0097(3) Uani 1 1 d . . . N3 N 0.47942(15) 0.27108(13) 0.69052(13) 0.0106(3) Uani 1 1 d . . . N4 N -0.00226(15) 0.38624(14) 0.68053(13) 0.0116(4) Uani 1 1 d . . . N5 N 0.11744(15) 0.24070(14) 0.74284(13) 0.0109(3) Uani 1 1 d . . . N6 N 0.24592(15) 0.20478(14) 0.60155(13) 0.0115(4) Uani 1 1 d . . . N7 N -0.15746(15) 0.18356(14) 0.74564(13) 0.0114(4) Uani 1 1 d . . . N8 N -0.05865(15) 0.02376(14) 0.80808(13) 0.0109(3) Uani 1 1 d . . . N9 N 0.08392(15) -0.01011(14) 0.67223(13) 0.0113(4) Uani 1 1 d . . . C1 C 0.1677(2) 0.39513(18) 0.91531(18) 0.0187(5) Uani 1 1 d . . . H1 H 0.1556 0.4473 0.8669 0.022 Uiso 1 1 calc R . . C2 C 0.0989(2) 0.38918(19) 0.99845(19) 0.0240(6) Uani 1 1 d . . . H2 H 0.0388 0.4348 1.0057 0.029 Uiso 1 1 calc R . . C3 C 0.1184(2) 0.31653(18) 1.07049(17) 0.0177(5) Uani 1 1 d . . . H3 H 0.0728 0.3126 1.1282 0.021 Uiso 1 1 calc R . . C4 C 0.20557(18) 0.24897(17) 1.05768(16) 0.0124(4) Uani 1 1 d . . . H4 H 0.2214 0.1986 1.1063 0.015 Uiso 1 1 calc R . . C5 C 0.26845(17) 0.25757(16) 0.97179(15) 0.0104(4) Uani 1 1 d . . . C6 C 0.35986(17) 0.18777(16) 0.94743(15) 0.0100(4) Uani 1 1 d . . . C7 C 0.39371(18) 0.10495(16) 1.00439(15) 0.0108(4) Uani 1 1 d . . . H7 H 0.3581 0.0890 1.0658 0.013 Uiso 1 1 calc R . . C8 C 0.48117(18) 0.04489(15) 0.97038(15) 0.0099(4) Uani 1 1 d . . . C9 C 0.53121(18) 0.07052(16) 0.87991(15) 0.0105(4) Uani 1 1 d . . . H9 H 0.5911 0.0314 0.8554 0.013 Uiso 1 1 calc R . . C10 C 0.49216(17) 0.15411(15) 0.82614(15) 0.0097(4) Uani 1 1 d . . . C11 C 0.53501(18) 0.19057(15) 0.72911(15) 0.0099(4) Uani 1 1 d . . . C12 C 0.62546(18) 0.14762(16) 0.68219(15) 0.0113(4) Uani 1 1 d . . . H12 H 0.6615 0.0901 0.7106 0.014 Uiso 1 1 calc R . . C13 C 0.66243(18) 0.19057(17) 0.59250(16) 0.0133(4) Uani 1 1 d . . . H13 H 0.7260 0.1646 0.5594 0.016 Uiso 1 1 calc R . . C14 C 0.6053(2) 0.27171(17) 0.55199(16) 0.0158(5) Uani 1 1 d . . . H14 H 0.6280 0.3008 0.4901 0.019 Uiso 1 1 calc R . . C15 C 0.51416(19) 0.31007(17) 0.60309(16) 0.0146(4) Uani 1 1 d . . . H15 H 0.4753 0.3658 0.5751 0.018 Uiso 1 1 calc R . . C16 C -0.05577(18) 0.46637(17) 0.64238(16) 0.0141(4) Uani 1 1 d . . . H16 H -0.0438 0.4832 0.5777 0.017 Uiso 1 1 calc R . . C17 C -0.12808(19) 0.52624(18) 0.69278(17) 0.0152(4) Uani 1 1 d . . . H17 H -0.1644 0.5829 0.6634 0.018 Uiso 1 1 calc R . . C18 C -0.14562(19) 0.50095(18) 0.78706(17) 0.0163(5) Uani 1 1 d . . . H18 H -0.1945 0.5403 0.8235 0.020 Uiso 1 1 calc R . . C19 C -0.09108(19) 0.41726(17) 0.82800(16) 0.0150(4) Uani 1 1 d . . . H19 H -0.1020 0.3989 0.8925 0.018 Uiso 1 1 calc R . . C20 C -0.02083(18) 0.36151(17) 0.77309(15) 0.0119(4) Uani 1 1 d . . . C21 C 0.04251(17) 0.27131(16) 0.80790(15) 0.0109(4) Uani 1 1 d . . . C22 C 0.03022(19) 0.22069(17) 0.89735(16) 0.0133(4) Uani 1 1 d . . . H22 H -0.0236 0.2427 0.9432 0.016 Uiso 1 1 calc R . . C23 C 0.09825(18) 0.13645(17) 0.91947(15) 0.0119(4) Uani 1 1 d . . . C24 C 0.17810(18) 0.10814(16) 0.84993(15) 0.0123(4) Uani 1 1 d . . . H24 H 0.2264 0.0527 0.8628 0.015 Uiso 1 1 calc R . . C25 C 0.18559(18) 0.16246(16) 0.76162(15) 0.0108(4) Uani 1 1 d . . . C26 C 0.26464(17) 0.14548(16) 0.68013(15) 0.0101(4) Uani 1 1 d . . . C27 C 0.35169(18) 0.07851(17) 0.68211(16) 0.0132(4) Uani 1 1 d . . . H27 H 0.3628 0.0369 0.7375 0.016 Uiso 1 1 calc R . . C28 C 0.42298(19) 0.07356(18) 0.60061(16) 0.0150(4) Uani 1 1 d . . . H28 H 0.4844 0.0294 0.6000 0.018 Uiso 1 1 calc R . . C29 C 0.40343(19) 0.13346(18) 0.52095(16) 0.0149(4) Uani 1 1 d . . . H29 H 0.4510 0.1306 0.4649 0.018 Uiso 1 1 calc R . . C30 C 0.31327(19) 0.19806(17) 0.52359(16) 0.0138(4) Uani 1 1 d . . . H30 H 0.2993 0.2384 0.4685 0.017 Uiso 1 1 calc R . . C31 C -0.20048(19) 0.26919(17) 0.70654(16) 0.0141(4) Uani 1 1 d . . . H31 H -0.1748 0.2932 0.6439 0.017 Uiso 1 1 calc R . . C32 C -0.2815(2) 0.32471(17) 0.75393(17) 0.0162(5) Uani 1 1 d . . . H32 H -0.3104 0.3857 0.7245 0.019 Uiso 1 1 calc R . . C33 C -0.3190(2) 0.28864(18) 0.84517(18) 0.0181(5) Uani 1 1 d . . . H33 H -0.3740 0.3249 0.8794 0.022 Uiso 1 1 calc R . . C34 C -0.27523(19) 0.19871(18) 0.88630(17) 0.0160(5) Uani 1 1 d . . . H34 H -0.3009 0.1723 0.9484 0.019 Uiso 1 1 calc R . . C35 C -0.19390(18) 0.14861(16) 0.83518(15) 0.0112(4) Uani 1 1 d . . . C36 C -0.13574(18) 0.05533(16) 0.87163(15) 0.0114(4) Uani 1 1 d . . . C37 C -0.15196(18) 0.00447(17) 0.96136(15) 0.0125(4) Uani 1 1 d . . . H37 H -0.2076 0.0264 1.0058 0.015 Uiso 1 1 calc R . . C38 C -0.08492(18) -0.07977(16) 0.98523(15) 0.0112(4) Uani 1 1 d . . . C39 C -0.00422(18) -0.10892(17) 0.91726(15) 0.0128(4) Uani 1 1 d . . . H39 H 0.0429 -0.1649 0.9315 0.015 Uiso 1 1 calc R . . C40 C 0.00678(18) -0.05550(16) 0.82871(15) 0.0115(4) Uani 1 1 d . . . C41 C 0.09040(18) -0.07426(17) 0.75111(16) 0.0127(4) Uani 1 1 d . . . C42 C 0.1712(2) -0.14801(19) 0.75810(17) 0.0178(5) Uani 1 1 d . . . H42 H 0.1726 -0.1933 0.8136 0.021 Uiso 1 1 calc R . . C43 C 0.2504(2) -0.1547(2) 0.68246(17) 0.0191(5) Uani 1 1 d . . . H43 H 0.3072 -0.2041 0.6856 0.023 Uiso 1 1 calc R . . C44 C 0.24490(19) -0.08830(18) 0.60263(17) 0.0162(5) Uani 1 1 d . . . H44 H 0.2990 -0.0905 0.5506 0.019 Uiso 1 1 calc R . . C45 C 0.15970(19) -0.01821(17) 0.59889(16) 0.0143(4) Uani 1 1 d . . . H45 H 0.1549 0.0252 0.5429 0.017 Uiso 1 1 calc R . . C46 C 0.5331(2) 0.70184(17) 0.76767(17) 0.0156(4) Uani 1 1 d . . . H46A H 0.5574 0.7089 0.7008 0.019 Uiso 1 1 calc R . . H46B H 0.4630 0.7378 0.7790 0.019 Uiso 1 1 calc R . . C47 C 0.5267(2) 0.59348(18) 0.80911(17) 0.0165(5) Uani 1 1 d . . . H47A H 0.5081 0.5860 0.8764 0.020 Uiso 1 1 calc R . . H47B H 0.5957 0.5568 0.7934 0.020 Uiso 1 1 calc R . . C48 C -0.04417(18) 0.27663(16) 0.39901(16) 0.0121(4) Uani 1 1 d . . . H48A H 0.0003 0.3027 0.3405 0.014 Uiso 1 1 calc R . . H48B H -0.0788 0.2240 0.3885 0.014 Uiso 1 1 calc R . . C49 C -0.12652(18) 0.35816(16) 0.42782(15) 0.0122(4) Uani 1 1 d . . . H49A H -0.0971 0.3984 0.4595 0.015 Uiso 1 1 calc R . . H49B H -0.1854 0.3290 0.4713 0.015 Uiso 1 1 calc R . . C50 C -0.16563(18) 0.42359(16) 0.34607(15) 0.0126(4) Uani 1 1 d . . . H50A H -0.2018 0.3846 0.3187 0.015 Uiso 1 1 calc R . . H50B H -0.1056 0.4463 0.2995 0.015 Uiso 1 1 calc R . . C51 C -0.39428(19) -0.25269(17) 0.80702(17) 0.0150(4) Uani 1 1 d . . . H51A H -0.3264 -0.2930 0.8025 0.018 Uiso 1 1 calc R . . H51B H -0.4232 -0.2517 0.8723 0.018 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 0.00955(12) 0.00808(12) 0.00915(12) 0.00055(9) -0.00128(10) -0.00022(9) Cu2 0.00972(12) 0.01061(12) 0.00836(12) -0.00097(9) -0.00102(10) -0.00051(10) Cu3 0.00913(12) 0.00957(12) 0.00867(12) 0.00029(9) -0.00030(10) -0.00130(10) V1 0.0272(3) 0.0172(2) 0.0218(2) -0.00319(17) 0.00900(19) -0.00225(18) V2 0.00830(16) 0.00919(16) 0.00859(16) -0.00130(12) -0.00064(13) -0.00138(13) P1 0.0121(3) 0.0147(3) 0.0155(3) -0.0054(2) 0.0004(2) -0.0056(2) P2 0.0086(2) 0.0091(2) 0.0100(2) 0.00024(19) -0.0017(2) -0.00071(19) P3 0.0079(2) 0.0084(2) 0.0077(2) -0.00017(18) -0.00038(19) -0.00069(19) P4 0.0085(2) 0.0113(2) 0.0103(2) -0.00169(19) -0.0013(2) -0.0021(2) O1 0.0347(14) 0.0685(19) 0.0396(15) 0.0124(13) 0.0132(11) 0.0261(13) O2 0.123(3) 0.0490(17) 0.0421(16) -0.0279(13) 0.0317(18) -0.0510(19) O3 0.0141(9) 0.0295(10) 0.0270(10) -0.0139(8) -0.0017(8) -0.0009(8) O4 0.0219(10) 0.0283(10) 0.0166(9) -0.0037(7) 0.0001(7) -0.0156(8) O5 0.0187(9) 0.0146(8) 0.0270(10) -0.0055(7) -0.0049(8) -0.0061(7) O6 0.0118(8) 0.0150(8) 0.0139(8) 0.0028(6) -0.0035(6) 0.0001(6) O7 0.0103(7) 0.0154(8) 0.0142(8) -0.0005(6) -0.0023(6) -0.0044(6) O8 0.0134(8) 0.0111(7) 0.0131(8) -0.0011(6) -0.0012(6) -0.0034(6) O9 0.0164(8) 0.0128(7) 0.0111(7) -0.0010(6) -0.0056(6) -0.0032(6) O10 0.0143(8) 0.0152(8) 0.0134(8) 0.0052(6) 0.0027(6) 0.0000(6) O11 0.0122(8) 0.0138(8) 0.0098(7) -0.0023(6) -0.0014(6) 0.0032(6) O12 0.0124(8) 0.0113(7) 0.0152(8) -0.0017(6) 0.0010(6) -0.0037(6) O13 0.0121(8) 0.0165(8) 0.0115(7) -0.0018(6) -0.0017(6) 0.0012(6) O14 0.0099(7) 0.0119(7) 0.0093(7) -0.0036(6) 0.0005(6) -0.0023(6) O15 0.0119(8) 0.0228(9) 0.0109(7) -0.0059(6) -0.0013(6) -0.0056(7) O16 0.0117(8) 0.0156(8) 0.0199(9) -0.0007(6) -0.0036(7) -0.0005(6) O17 0.0256(11) 0.0350(12) 0.0251(11) 0.0048(9) 0.0014(9) 0.0101(9) O90 0.0202(9) 0.0253(10) 0.0214(9) -0.0046(8) 0.0018(8) 0.0018(8) O91 0.0211(10) 0.0572(15) 0.0188(10) -0.0089(10) -0.0024(8) -0.0042(10) O92 0.0248(19) 0.0220(18) 0.0120(16) 0.0019(13) -0.0073(14) -0.0008(15) N1 0.0123(9) 0.0086(8) 0.0115(9) 0.0008(7) -0.0018(7) 0.0006(7) N2 0.0094(8) 0.0097(8) 0.0086(8) 0.0001(6) 0.0000(7) -0.0011(7) N3 0.0113(9) 0.0088(8) 0.0103(8) 0.0001(6) -0.0010(7) -0.0013(7) N4 0.0101(8) 0.0128(9) 0.0107(8) 0.0002(7) -0.0003(7) -0.0031(7) N5 0.0103(9) 0.0110(8) 0.0107(8) -0.0012(7) -0.0019(7) -0.0009(7) N6 0.0122(9) 0.0122(9) 0.0100(8) -0.0009(7) -0.0027(7) -0.0015(7) N7 0.0108(9) 0.0122(9) 0.0115(9) -0.0013(7) -0.0025(7) -0.0025(7) N8 0.0095(8) 0.0110(8) 0.0109(8) -0.0007(7) -0.0009(7) -0.0009(7) N9 0.0111(9) 0.0123(9) 0.0094(8) -0.0012(7) -0.0005(7) -0.0014(7) C1 0.0186(12) 0.0133(11) 0.0187(12) 0.0015(9) -0.0009(9) 0.0051(9) C2 0.0222(13) 0.0170(12) 0.0230(13) 0.0012(10) 0.0030(10) 0.0100(10) C3 0.0180(12) 0.0142(11) 0.0162(11) -0.0015(9) 0.0020(9) 0.0030(9) C4 0.0137(10) 0.0116(10) 0.0114(10) -0.0017(8) -0.0023(8) -0.0009(8) C5 0.0103(9) 0.0092(9) 0.0110(9) -0.0010(7) -0.0020(8) -0.0007(8) C6 0.0108(10) 0.0091(9) 0.0092(9) -0.0009(7) -0.0009(8) -0.0010(8) C7 0.0112(10) 0.0100(9) 0.0093(9) -0.0010(7) -0.0006(8) 0.0011(8) C8 0.0126(10) 0.0078(9) 0.0090(9) -0.0003(7) -0.0031(8) -0.0003(8) C9 0.0107(10) 0.0098(9) 0.0100(9) -0.0011(7) -0.0016(8) 0.0003(8) C10 0.0109(10) 0.0084(9) 0.0095(9) -0.0011(7) -0.0014(8) -0.0016(7) C11 0.0113(10) 0.0088(9) 0.0092(9) -0.0009(7) -0.0015(8) -0.0016(8) C12 0.0119(10) 0.0097(9) 0.0112(10) -0.0012(7) -0.0013(8) -0.0004(8) C13 0.0109(10) 0.0131(10) 0.0141(10) -0.0026(8) 0.0014(8) -0.0014(8) C14 0.0168(11) 0.0150(11) 0.0117(10) 0.0009(8) 0.0027(9) -0.0021(9) C15 0.0152(11) 0.0122(10) 0.0125(10) 0.0016(8) -0.0001(8) 0.0009(8) C16 0.0122(10) 0.0150(10) 0.0140(10) 0.0015(8) -0.0026(8) -0.0036(8) C17 0.0130(11) 0.0146(11) 0.0165(11) 0.0002(8) -0.0032(9) -0.0006(8) C18 0.0127(11) 0.0159(11) 0.0181(11) -0.0018(9) -0.0014(9) 0.0011(9) C19 0.0142(11) 0.0170(11) 0.0106(10) -0.0012(8) 0.0005(8) 0.0017(9) C20 0.0104(10) 0.0136(10) 0.0099(9) -0.0003(8) -0.0001(8) -0.0014(8) C21 0.0103(10) 0.0113(10) 0.0105(10) -0.0014(7) -0.0018(8) -0.0008(8) C22 0.0134(10) 0.0132(10) 0.0111(10) 0.0000(8) -0.0004(8) -0.0005(8) C23 0.0118(10) 0.0131(10) 0.0102(10) -0.0005(8) -0.0011(8) -0.0036(8) C24 0.0133(10) 0.0119(10) 0.0111(10) -0.0008(8) -0.0024(8) -0.0015(8) C25 0.0113(10) 0.0092(9) 0.0111(10) -0.0006(7) -0.0012(8) -0.0022(8) C26 0.0098(9) 0.0108(9) 0.0095(9) -0.0019(7) -0.0004(8) -0.0023(8) C27 0.0120(10) 0.0150(10) 0.0119(10) -0.0007(8) -0.0026(8) -0.0020(8) C28 0.0131(10) 0.0164(11) 0.0146(11) -0.0039(8) -0.0020(9) 0.0014(9) C29 0.0119(10) 0.0191(11) 0.0125(10) -0.0044(8) 0.0008(8) -0.0007(9) C30 0.0135(10) 0.0168(11) 0.0109(10) -0.0030(8) -0.0023(8) -0.0003(8) C31 0.0152(11) 0.0126(10) 0.0150(10) 0.0000(8) -0.0054(9) -0.0032(8) C32 0.0180(11) 0.0124(10) 0.0192(11) -0.0038(9) -0.0052(9) -0.0013(9) C33 0.0149(11) 0.0165(11) 0.0220(12) -0.0062(9) -0.0007(9) 0.0004(9) C34 0.0138(11) 0.0173(11) 0.0150(11) -0.0031(9) 0.0011(9) -0.0019(9) C35 0.0116(10) 0.0108(10) 0.0112(10) -0.0030(8) -0.0012(8) -0.0016(8) C36 0.0112(10) 0.0123(10) 0.0104(9) -0.0013(8) -0.0008(8) -0.0029(8) C37 0.0114(10) 0.0151(10) 0.0101(10) -0.0016(8) -0.0005(8) -0.0021(8) C38 0.0112(10) 0.0133(10) 0.0092(9) -0.0015(8) -0.0009(8) -0.0040(8) C39 0.0122(10) 0.0144(10) 0.0106(10) -0.0004(8) -0.0016(8) -0.0008(8) C40 0.0103(10) 0.0120(10) 0.0118(10) -0.0017(8) -0.0016(8) -0.0018(8) C41 0.0119(10) 0.0139(10) 0.0120(10) -0.0013(8) -0.0021(8) -0.0027(8) C42 0.0168(11) 0.0198(12) 0.0140(11) -0.0007(9) -0.0029(9) 0.0028(9) C43 0.0137(11) 0.0233(12) 0.0176(12) -0.0037(9) -0.0023(9) 0.0050(9) C44 0.0127(11) 0.0213(12) 0.0137(11) -0.0044(9) 0.0006(9) -0.0018(9) C45 0.0146(11) 0.0143(10) 0.0126(10) -0.0016(8) 0.0001(8) -0.0026(9) C46 0.0161(11) 0.0141(10) 0.0182(11) -0.0018(8) -0.0043(9) -0.0069(9) C47 0.0156(11) 0.0164(11) 0.0185(11) -0.0026(9) -0.0032(9) -0.0062(9) C48 0.0128(10) 0.0113(10) 0.0126(10) -0.0021(8) -0.0037(8) -0.0010(8) C49 0.0113(10) 0.0117(10) 0.0121(10) -0.0001(8) -0.0034(8) 0.0017(8) C50 0.0144(10) 0.0111(10) 0.0118(10) -0.0021(8) -0.0037(8) 0.0018(8) C51 0.0164(11) 0.0110(10) 0.0187(11) -0.0003(8) -0.0059(9) -0.0047(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 O6 1.8977(17) . ? Cu1 N2 1.9403(19) . ? Cu1 N1 2.057(2) . ? Cu1 N3 2.0727(19) . ? Cu1 O5 2.1067(18) . ? Cu2 O9 1.9543(16) . ? Cu2 N5 1.9699(19) . ? Cu2 N6 2.009(2) . ? Cu2 N4 2.056(2) . ? Cu2 O8 2.1031(16) . ? Cu3 O10 1.8840(17) . ? Cu3 N8 1.9511(19) . ? Cu3 N9 2.057(2) . ? Cu3 N7 2.058(2) . ? Cu3 O12 2.1656(17) . ? V1 O2 1.622(3) . ? V1 O1 1.626(3) . ? V1 O17 1.746(2) . ? V1 O3 1.830(2) . ? V2 O13 1.6216(17) . ? V2 O12 1.6479(16) . ? V2 O11 1.9294(16) 2_556 ? V2 O15 2.0167(17) . ? V2 O14 2.0529(16) . ? P1 O5 1.5061(19) . ? P1 O4 1.516(2) . ? P1 O3 1.583(2) . ? P1 C47 1.798(3) . ? P2 O8 1.5103(18) . ? P2 O6 1.5176(17) . ? P2 O7 1.5620(17) . ? P2 C50 1.797(2) 2_566 ? P3 O10 1.5195(17) . ? P3 O9 1.5208(17) . ? P3 O11 1.5357(17) . ? P3 C48 1.798(2) . ? P4 O16 1.4956(18) . ? P4 O15 1.5473(17) . ? P4 O14 1.5643(17) . ? P4 C51 1.802(2) . ? O11 V2 1.9294(16) 2_556 ? N1 C1 1.334(3) . ? N1 C5 1.352(3) . ? N2 C10 1.333(3) . ? N2 C6 1.344(3) . ? N3 C15 1.341(3) . ? N3 C11 1.357(3) . ? N4 C16 1.337(3) . ? N4 C20 1.360(3) . ? N5 C21 1.335(3) . ? N5 C25 1.342(3) . ? N6 C30 1.335(3) . ? N6 C26 1.361(3) . ? N7 C31 1.334(3) . ? N7 C35 1.359(3) . ? N8 C40 1.336(3) . ? N8 C36 1.341(3) . ? N9 C45 1.345(3) . ? N9 C41 1.357(3) . ? C1 C2 1.388(4) . ? C2 C3 1.379(4) . ? C3 C4 1.392(3) . ? C4 C5 1.385(3) . ? C5 C6 1.477(3) . ? C6 C7 1.382(3) . ? C7 C8 1.401(3) . ? C8 C9 1.394(3) . ? C8 C8 1.483(4) 2_657 ? C9 C10 1.389(3) . ? C10 C11 1.478(3) . ? C11 C12 1.383(3) . ? C12 C13 1.390(3) . ? C13 C14 1.385(3) . ? C14 C15 1.392(3) . ? C16 C17 1.390(3) . ? C17 C18 1.386(3) . ? C18 C19 1.394(3) . ? C19 C20 1.380(3) . ? C20 C21 1.484(3) . ? C21 C22 1.390(3) . ? C22 C23 1.409(3) . ? C23 C24 1.404(3) . ? C23 C38 1.494(3) 2_557 ? C24 C25 1.396(3) . ? C25 C26 1.479(3) . ? C26 C27 1.382(3) . ? C27 C28 1.397(3) . ? C28 C29 1.381(3) . ? C29 C30 1.392(3) . ? C31 C32 1.393(3) . ? C32 C33 1.387(4) . ? C33 C34 1.394(3) . ? C34 C35 1.382(3) . ? C35 C36 1.488(3) . ? C36 C37 1.394(3) . ? C37 C38 1.408(3) . ? C38 C39 1.399(3) . ? C38 C23 1.494(3) 2_557 ? C39 C40 1.392(3) . ? C40 C41 1.475(3) . ? C41 C42 1.385(3) . ? C42 C43 1.391(3) . ? C43 C44 1.382(3) . ? C44 C45 1.391(3) . ? C46 C51 1.526(3) 1_665 ? C46 C47 1.533(3) . ? C48 C49 1.528(3) . ? C49 C50 1.531(3) . ? C50 P2 1.797(2) 2_566 ? C51 C46 1.526(3) 1_445 ? 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 O6 Cu1 N2 153.75(8) . . ? O6 Cu1 N1 90.96(8) . . ? N2 Cu1 N1 79.13(8) . . ? O6 Cu1 N3 105.80(8) . . ? N2 Cu1 N3 79.36(8) . . ? N1 Cu1 N3 157.60(7) . . ? O6 Cu1 O5 103.17(8) . . ? N2 Cu1 O5 102.16(8) . . ? N1 Cu1 O5 97.11(8) . . ? N3 Cu1 O5 93.47(8) . . ? O9 Cu2 N5 146.93(8) . . ? O9 Cu2 N6 98.02(8) . . ? N5 Cu2 N6 79.06(8) . . ? O9 Cu2 N4 101.34(8) . . ? N5 Cu2 N4 78.70(8) . . ? N6 Cu2 N4 157.71(8) . . ? O9 Cu2 O8 93.25(7) . . ? N5 Cu2 O8 119.80(7) . . ? N6 Cu2 O8 95.30(7) . . ? N4 Cu2 O8 94.51(7) . . ? O10 Cu3 N8 169.33(8) . . ? O10 Cu3 N9 105.09(8) . . ? N8 Cu3 N9 79.30(8) . . ? O10 Cu3 N7 94.49(8) . . ? N8 Cu3 N7 78.71(8) . . ? N9 Cu3 N7 154.18(8) . . ? O10 Cu3 O12 93.27(7) . . ? N8 Cu3 O12 95.56(7) . . ? N9 Cu3 O12 99.81(7) . . ? N7 Cu3 O12 95.63(7) . . ? O2 V1 O1 106.33(19) . . ? O2 V1 O17 110.67(16) . . ? O1 V1 O17 108.63(12) . . ? O2 V1 O3 108.73(12) . . ? O1 V1 O3 110.65(13) . . ? O17 V1 O3 111.69(10) . . ? O13 V2 O12 109.03(9) . . ? O13 V2 O11 99.59(8) . 2_556 ? O12 V2 O11 102.03(8) . 2_556 ? O13 V2 O15 129.94(8) . . ? O12 V2 O15 119.26(8) . . ? O11 V2 O15 83.27(7) 2_556 . ? O13 V2 O14 92.12(8) . . ? O12 V2 O14 96.75(7) . . ? O11 V2 O14 153.14(7) 2_556 . ? O15 V2 O14 70.79(7) . . ? O5 P1 O4 115.78(11) . . ? O5 P1 O3 108.94(11) . . ? O4 P1 O3 108.20(11) . . ? O5 P1 C47 108.56(11) . . ? O4 P1 C47 108.83(11) . . ? O3 P1 C47 106.09(11) . . ? O8 P2 O6 113.62(10) . . ? O8 P2 O7 108.32(10) . . ? O6 P2 O7 111.55(10) . . ? O8 P2 C50 109.43(10) . 2_566 ? O6 P2 C50 106.63(10) . 2_566 ? O7 P2 C50 107.07(10) . 2_566 ? O10 P3 O9 111.94(10) . . ? O10 P3 O11 110.64(10) . . ? O9 P3 O11 111.60(10) . . ? O10 P3 C48 108.41(11) . . ? O9 P3 C48 106.87(10) . . ? O11 P3 C48 107.15(10) . . ? O16 P4 O15 116.87(10) . . ? O16 P4 O14 114.81(10) . . ? O15 P4 O14 98.50(9) . . ? O16 P4 C51 109.37(11) . . ? O15 P4 C51 107.37(11) . . ? O14 P4 C51 109.22(10) . . ? P1 O3 V1 138.30(13) . . ? P1 O5 Cu1 128.38(12) . . ? P2 O6 Cu1 145.95(11) . . ? P2 O8 Cu2 120.33(10) . . ? P3 O9 Cu2 122.33(10) . . ? P3 O10 Cu3 151.37(12) . . ? P3 O11 V2 143.37(11) . 2_556 ? V2 O12 Cu3 135.72(10) . . ? P4 O14 V2 93.96(8) . . ? P4 O15 V2 95.92(8) . . ? C1 N1 C5 118.5(2) . . ? C1 N1 Cu1 126.79(16) . . ? C5 N1 Cu1 114.65(15) . . ? C10 N2 C6 121.26(19) . . ? C10 N2 Cu1 119.49(15) . . ? C6 N2 Cu1 119.25(15) . . ? C15 N3 C11 118.1(2) . . ? C15 N3 Cu1 128.11(16) . . ? C11 N3 Cu1 113.21(15) . . ? C16 N4 C20 118.2(2) . . ? C16 N4 Cu2 126.32(16) . . ? C20 N4 Cu2 114.71(15) . . ? C21 N5 C25 121.6(2) . . ? C21 N5 Cu2 119.39(15) . . ? C25 N5 Cu2 118.89(15) . . ? C30 N6 C26 119.2(2) . . ? C30 N6 Cu2 124.54(16) . . ? C26 N6 Cu2 115.95(15) . . ? C31 N7 C35 119.0(2) . . ? C31 N7 Cu3 126.31(16) . . ? C35 N7 Cu3 114.46(15) . . ? C40 N8 C36 121.5(2) . . ? C40 N8 Cu3 118.74(15) . . ? C36 N8 Cu3 119.65(15) . . ? C45 N9 C41 118.4(2) . . ? C45 N9 Cu3 127.66(16) . . ? C41 N9 Cu3 113.91(15) . . ? N1 C1 C2 121.9(2) . . ? C3 C2 C1 119.5(2) . . ? C2 C3 C4 119.2(2) . . ? C5 C4 C3 117.8(2) . . ? N1 C5 C4 123.0(2) . . ? N1 C5 C6 113.56(19) . . ? C4 C5 C6 123.5(2) . . ? N2 C6 C7 120.8(2) . . ? N2 C6 C5 113.22(19) . . ? C7 C6 C5 126.0(2) . . ? C6 C7 C8 119.1(2) . . ? C9 C8 C7 118.9(2) . . ? C9 C8 C8 120.8(3) . 2_657 ? C7 C8 C8 120.4(2) . 2_657 ? C10 C9 C8 119.0(2) . . ? N2 C10 C9 121.0(2) . . ? N2 C10 C11 113.25(19) . . ? C9 C10 C11 125.7(2) . . ? N3 C11 C12 122.8(2) . . ? N3 C11 C10 114.33(19) . . ? C12 C11 C10 122.8(2) . . ? C11 C12 C13 118.5(2) . . ? C14 C13 C12 119.1(2) . . ? C13 C14 C15 119.2(2) . . ? N3 C15 C14 122.2(2) . . ? N4 C16 C17 123.2(2) . . ? C18 C17 C16 118.1(2) . . ? C17 C18 C19 119.5(2) . . ? C20 C19 C18 118.8(2) . . ? N4 C20 C19 122.2(2) . . ? N4 C20 C21 113.6(2) . . ? C19 C20 C21 124.2(2) . . ? N5 C21 C22 120.8(2) . . ? N5 C21 C20 112.69(19) . . ? C22 C21 C20 126.5(2) . . ? C21 C22 C23 119.4(2) . . ? C24 C23 C22 118.2(2) . . ? C24 C23 C38 121.5(2) . 2_557 ? C22 C23 C38 120.2(2) . 2_557 ? C25 C24 C23 119.1(2) . . ? N5 C25 C24 120.8(2) . . ? N5 C25 C26 112.05(19) . . ? C24 C25 C26 127.2(2) . . ? N6 C26 C27 122.1(2) . . ? N6 C26 C25 113.62(19) . . ? C27 C26 C25 124.3(2) . . ? C26 C27 C28 118.3(2) . . ? C29 C28 C27 119.4(2) . . ? C28 C29 C30 119.3(2) . . ? N6 C30 C29 121.7(2) . . ? N7 C31 C32 122.6(2) . . ? C33 C32 C31 118.3(2) . . ? C32 C33 C34 119.5(2) . . ? C35 C34 C33 118.9(2) . . ? N7 C35 C34 121.7(2) . . ? N7 C35 C36 113.66(19) . . ? C34 C35 C36 124.6(2) . . ? N8 C36 C37 120.8(2) . . ? N8 C36 C35 112.37(19) . . ? C37 C36 C35 126.8(2) . . ? C36 C37 C38 119.2(2) . . ? C39 C38 C37 118.2(2) . . ? C39 C38 C23 120.5(2) . 2_557 ? C37 C38 C23 121.3(2) . 2_557 ? C40 C39 C38 119.7(2) . . ? N8 C40 C39 120.7(2) . . ? N8 C40 C41 113.3(2) . . ? C39 C40 C41 126.0(2) . . ? N9 C41 C42 122.4(2) . . ? N9 C41 C40 114.1(2) . . ? C42 C41 C40 123.5(2) . . ? C41 C42 C43 118.9(2) . . ? C44 C43 C42 118.8(2) . . ? C43 C44 C45 119.6(2) . . ? N9 C45 C44 121.9(2) . . ? C51 C46 C47 112.6(2) 1_665 . ? C46 C47 P1 112.98(18) . . ? C49 C48 P3 113.85(16) . . ? C48 C49 C50 111.92(19) . . ? C49 C50 P2 113.10(16) . 2_566 ? C46 C51 P4 111.00(17) 1_445 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O5 P1 O3 V1 83.8(2) . . . . ? O4 P1 O3 V1 -149.55(18) . . . . ? C47 P1 O3 V1 -32.9(2) . . . . ? O2 V1 O3 P1 69.2(3) . . . . ? O1 V1 O3 P1 -174.4(2) . . . . ? O17 V1 O3 P1 -53.3(2) . . . . ? O4 P1 O5 Cu1 -59.49(17) . . . . ? O3 P1 O5 Cu1 62.69(16) . . . . ? C47 P1 O5 Cu1 177.80(13) . . . . ? O6 Cu1 O5 P1 2.01(16) . . . . ? N2 Cu1 O5 P1 -171.01(14) . . . . ? N1 Cu1 O5 P1 -90.65(15) . . . . ? N3 Cu1 O5 P1 109.13(15) . . . . ? O8 P2 O6 Cu1 109.0(2) . . . . ? O7 P2 O6 Cu1 -13.8(2) . . . . ? C50 P2 O6 Cu1 -130.4(2) 2_566 . . . ? N2 Cu1 O6 P2 -134.19(19) . . . . ? N1 Cu1 O6 P2 158.9(2) . . . . ? N3 Cu1 O6 P2 -36.1(2) . . . . ? O5 Cu1 O6 P2 61.4(2) . . . . ? O6 P2 O8 Cu2 22.33(14) . . . . ? O7 P2 O8 Cu2 146.89(10) . . . . ? C50 P2 O8 Cu2 -96.71(12) 2_566 . . . ? O9 Cu2 O8 P2 171.79(11) . . . . ? N5 Cu2 O8 P2 -9.42(15) . . . . ? N6 Cu2 O8 P2 -89.84(12) . . . . ? N4 Cu2 O8 P2 70.13(12) . . . . ? O10 P3 O9 Cu2 33.98(15) . . . . ? O11 P3 O9 Cu2 -90.64(13) . . . . ? C48 P3 O9 Cu2 152.53(12) . . . . ? N5 Cu2 O9 P3 -12.3(2) . . . . ? N6 Cu2 O9 P3 69.92(13) . . . . ? N4 Cu2 O9 P3 -98.99(12) . . . . ? O8 Cu2 O9 P3 165.74(12) . . . . ? O9 P3 O10 Cu3 -74.8(3) . . . . ? O11 P3 O10 Cu3 50.4(3) . . . . ? C48 P3 O10 Cu3 167.6(2) . . . . ? N8 Cu3 O10 P3 83.2(5) . . . . ? N9 Cu3 O10 P3 -29.9(3) . . . . ? N7 Cu3 O10 P3 133.1(3) . . . . ? O12 Cu3 O10 P3 -130.9(3) . . . . ? O10 P3 O11 V2 127.69(18) . . . 2_556 ? O9 P3 O11 V2 -106.96(18) . . . 2_556 ? C48 P3 O11 V2 9.7(2) . . . 2_556 ? O13 V2 O12 Cu3 -1.82(16) . . . . ? O11 V2 O12 Cu3 -106.53(13) 2_556 . . . ? O15 V2 O12 Cu3 164.51(11) . . . . ? O14 V2 O12 Cu3 92.77(13) . . . . ? O10 Cu3 O12 V2 147.23(14) . . . . ? N8 Cu3 O12 V2 -38.77(14) . . . . ? N9 Cu3 O12 V2 41.30(14) . . . . ? N7 Cu3 O12 V2 -117.92(14) . . . . ? O16 P4 O14 V2 -132.52(9) . . . . ? O15 P4 O14 V2 -7.60(9) . . . . ? C51 P4 O14 V2 104.24(10) . . . . ? O13 V2 O14 P4 -125.77(9) . . . . ? O12 V2 O14 P4 124.78(9) . . . . ? O11 V2 O14 P4 -9.53(19) 2_556 . . . ? O15 V2 O14 P4 6.10(7) . . . . ? O16 P4 O15 V2 131.21(9) . . . . ? O14 P4 O15 V2 7.76(9) . . . . ? C51 P4 O15 V2 -105.55(10) . . . . ? O13 V2 O15 P4 69.89(13) . . . . ? O12 V2 O15 P4 -93.17(10) . . . . ? O11 V2 O15 P4 166.78(9) 2_556 . . . ? O14 V2 O15 P4 -6.18(8) . . . . ? O6 Cu1 N1 C1 -22.9(2) . . . . ? N2 Cu1 N1 C1 -178.5(2) . . . . ? N3 Cu1 N1 C1 -162.0(2) . . . . ? O5 Cu1 N1 C1 80.5(2) . . . . ? O6 Cu1 N1 C5 159.42(16) . . . . ? N2 Cu1 N1 C5 3.89(16) . . . . ? N3 Cu1 N1 C5 20.4(3) . . . . ? O5 Cu1 N1 C5 -97.19(16) . . . . ? O6 Cu1 N2 C10 107.5(2) . . . . ? N1 Cu1 N2 C10 176.94(18) . . . . ? N3 Cu1 N2 C10 3.25(17) . . . . ? O5 Cu1 N2 C10 -88.04(18) . . . . ? O6 Cu1 N2 C6 -72.5(3) . . . . ? N1 Cu1 N2 C6 -3.01(17) . . . . ? N3 Cu1 N2 C6 -176.70(18) . . . . ? O5 Cu1 N2 C6 92.01(18) . . . . ? O6 Cu1 N3 C15 29.8(2) . . . . ? N2 Cu1 N3 C15 -176.6(2) . . . . ? N1 Cu1 N3 C15 166.9(2) . . . . ? O5 Cu1 N3 C15 -74.9(2) . . . . ? O6 Cu1 N3 C11 -158.81(15) . . . . ? N2 Cu1 N3 C11 -5.28(16) . . . . ? N1 Cu1 N3 C11 -21.7(3) . . . . ? O5 Cu1 N3 C11 96.45(16) . . . . ? O9 Cu2 N4 C16 -39.1(2) . . . . ? N5 Cu2 N4 C16 174.6(2) . . . . ? N6 Cu2 N4 C16 171.0(2) . . . . ? O8 Cu2 N4 C16 55.1(2) . . . . ? O9 Cu2 N4 C20 151.04(16) . . . . ? N5 Cu2 N4 C20 4.79(16) . . . . ? N6 Cu2 N4 C20 1.2(3) . . . . ? O8 Cu2 N4 C20 -114.72(16) . . . . ? O9 Cu2 N5 C21 -92.1(2) . . . . ? N6 Cu2 N5 C21 179.98(19) . . . . ? N4 Cu2 N5 C21 1.37(17) . . . . ? O8 Cu2 N5 C21 90.10(18) . . . . ? O9 Cu2 N5 C25 84.1(2) . . . . ? N6 Cu2 N5 C25 -3.84(17) . . . . ? N4 Cu2 N5 C25 177.55(18) . . . . ? O8 Cu2 N5 C25 -93.71(18) . . . . ? O9 Cu2 N6 C30 39.1(2) . . . . ? N5 Cu2 N6 C30 -174.3(2) . . . . ? N4 Cu2 N6 C30 -170.73(19) . . . . ? O8 Cu2 N6 C30 -55.0(2) . . . . ? O9 Cu2 N6 C26 -147.08(16) . . . . ? N5 Cu2 N6 C26 -0.49(16) . . . . ? N4 Cu2 N6 C26 3.1(3) . . . . ? O8 Cu2 N6 C26 118.87(16) . . . . ? O10 Cu3 N7 C31 4.2(2) . . . . ? N8 Cu3 N7 C31 175.9(2) . . . . ? N9 Cu3 N7 C31 143.8(2) . . . . ? O12 Cu3 N7 C31 -89.6(2) . . . . ? O10 Cu3 N7 C35 179.05(16) . . . . ? N8 Cu3 N7 C35 -9.25(16) . . . . ? N9 Cu3 N7 C35 -41.3(3) . . . . ? O12 Cu3 N7 C35 85.31(16) . . . . ? O10 Cu3 N8 C40 -123.0(4) . . . . ? N9 Cu3 N8 C40 -7.62(17) . . . . ? N7 Cu3 N8 C40 -174.00(19) . . . . ? O12 Cu3 N8 C40 91.35(18) . . . . ? O10 Cu3 N8 C36 60.6(5) . . . . ? N9 Cu3 N8 C36 175.94(18) . . . . ? N7 Cu3 N8 C36 9.56(17) . . . . ? O12 Cu3 N8 C36 -85.09(18) . . . . ? O10 Cu3 N9 C45 -4.4(2) . . . . ? N8 Cu3 N9 C45 -174.4(2) . . . . ? N7 Cu3 N9 C45 -142.4(2) . . . . ? O12 Cu3 N9 C45 91.8(2) . . . . ? O10 Cu3 N9 C41 175.98(16) . . . . ? N8 Cu3 N9 C41 5.95(16) . . . . ? N7 Cu3 N9 C41 38.0(3) . . . . ? O12 Cu3 N9 C41 -87.91(16) . . . . ? C5 N1 C1 C2 -2.2(4) . . . . ? Cu1 N1 C1 C2 -179.7(2) . . . . ? N1 C1 C2 C3 3.2(5) . . . . ? C1 C2 C3 C4 -1.6(4) . . . . ? C2 C3 C4 C5 -0.8(4) . . . . ? C1 N1 C5 C4 -0.3(3) . . . . ? Cu1 N1 C5 C4 177.50(18) . . . . ? C1 N1 C5 C6 178.1(2) . . . . ? Cu1 N1 C5 C6 -4.1(2) . . . . ? C3 C4 C5 N1 1.8(4) . . . . ? C3 C4 C5 C6 -176.4(2) . . . . ? C10 N2 C6 C7 0.4(3) . . . . ? Cu1 N2 C6 C7 -179.63(17) . . . . ? C10 N2 C6 C5 -178.3(2) . . . . ? Cu1 N2 C6 C5 1.7(3) . . . . ? N1 C5 C6 N2 1.7(3) . . . . ? C4 C5 C6 N2 -179.9(2) . . . . ? N1 C5 C6 C7 -176.9(2) . . . . ? C4 C5 C6 C7 1.5(4) . . . . ? N2 C6 C7 C8 0.3(3) . . . . ? C5 C6 C7 C8 178.8(2) . . . . ? C6 C7 C8 C9 -0.2(3) . . . . ? C6 C7 C8 C8 -179.5(3) . . . 2_657 ? C7 C8 C9 C10 -0.7(3) . . . . ? C8 C8 C9 C10 178.6(3) 2_657 . . . ? C6 N2 C10 C9 -1.3(3) . . . . ? Cu1 N2 C10 C9 178.73(17) . . . . ? C6 N2 C10 C11 179.2(2) . . . . ? Cu1 N2 C10 C11 -0.7(3) . . . . ? C8 C9 C10 N2 1.4(3) . . . . ? C8 C9 C10 C11 -179.1(2) . . . . ? C15 N3 C11 C12 0.1(3) . . . . ? Cu1 N3 C11 C12 -172.18(18) . . . . ? C15 N3 C11 C10 178.7(2) . . . . ? Cu1 N3 C11 C10 6.4(2) . . . . ? N2 C10 C11 N3 -3.9(3) . . . . ? C9 C10 C11 N3 176.6(2) . . . . ? N2 C10 C11 C12 174.6(2) . . . . ? C9 C10 C11 C12 -4.8(4) . . . . ? N3 C11 C12 C13 1.9(3) . . . . ? C10 C11 C12 C13 -176.5(2) . . . . ? C11 C12 C13 C14 -3.0(3) . . . . ? C12 C13 C14 C15 2.1(4) . . . . ? C11 N3 C15 C14 -1.1(4) . . . . ? Cu1 N3 C15 C14 169.91(18) . . . . ? C13 C14 C15 N3 -0.1(4) . . . . ? C20 N4 C16 C17 1.0(3) . . . . ? Cu2 N4 C16 C17 -168.49(18) . . . . ? N4 C16 C17 C18 -0.4(4) . . . . ? C16 C17 C18 C19 -0.1(4) . . . . ? C17 C18 C19 C20 -0.1(4) . . . . ? C16 N4 C20 C19 -1.3(3) . . . . ? Cu2 N4 C20 C19 169.46(19) . . . . ? C16 N4 C20 C21 179.8(2) . . . . ? Cu2 N4 C20 C21 -9.5(2) . . . . ? C18 C19 C20 N4 0.8(4) . . . . ? C18 C19 C20 C21 179.6(2) . . . . ? C25 N5 C21 C22 -2.4(3) . . . . ? Cu2 N5 C21 C22 173.72(17) . . . . ? C25 N5 C21 C20 177.3(2) . . . . ? Cu2 N5 C21 C20 -6.7(3) . . . . ? N4 C20 C21 N5 10.4(3) . . . . ? C19 C20 C21 N5 -168.5(2) . . . . ? N4 C20 C21 C22 -170.0(2) . . . . ? C19 C20 C21 C22 11.1(4) . . . . ? N5 C21 C22 C23 0.4(3) . . . . ? C20 C21 C22 C23 -179.1(2) . . . . ? C21 C22 C23 C24 1.5(3) . . . . ? C21 C22 C23 C38 -178.7(2) . . . 2_557 ? C22 C23 C24 C25 -1.6(3) . . . . ? C38 C23 C24 C25 178.6(2) 2_557 . . . ? C21 N5 C25 C24 2.2(3) . . . . ? Cu2 N5 C25 C24 -173.86(17) . . . . ? C21 N5 C25 C26 -176.9(2) . . . . ? Cu2 N5 C25 C26 7.0(3) . . . . ? C23 C24 C25 N5 -0.2(3) . . . . ? C23 C24 C25 C26 178.9(2) . . . . ? C30 N6 C26 C27 0.3(3) . . . . ? Cu2 N6 C26 C27 -173.85(18) . . . . ? C30 N6 C26 C25 178.4(2) . . . . ? Cu2 N6 C26 C25 4.2(2) . . . . ? N5 C25 C26 N6 -7.0(3) . . . . ? C24 C25 C26 N6 173.8(2) . . . . ? N5 C25 C26 C27 170.9(2) . . . . ? C24 C25 C26 C27 -8.2(4) . . . . ? N6 C26 C27 C28 1.2(3) . . . . ? C25 C26 C27 C28 -176.7(2) . . . . ? C26 C27 C28 C29 -1.5(4) . . . . ? C27 C28 C29 C30 0.4(4) . . . . ? C26 N6 C30 C29 -1.5(3) . . . . ? Cu2 N6 C30 C29 172.14(18) . . . . ? C28 C29 C30 N6 1.1(4) . . . . ? C35 N7 C31 C32 0.1(3) . . . . ? Cu3 N7 C31 C32 174.80(18) . . . . ? N7 C31 C32 C33 -0.5(4) . . . . ? C31 C32 C33 C34 -0.2(4) . . . . ? C32 C33 C34 C35 1.3(4) . . . . ? C31 N7 C35 C34 1.0(3) . . . . ? Cu3 N7 C35 C34 -174.30(18) . . . . ? C31 N7 C35 C36 -176.9(2) . . . . ? Cu3 N7 C35 C36 7.8(2) . . . . ? C33 C34 C35 N7 -1.7(4) . . . . ? C33 C34 C35 C36 176.0(2) . . . . ? C40 N8 C36 C37 -1.9(3) . . . . ? Cu3 N8 C36 C37 174.48(17) . . . . ? C40 N8 C36 C35 175.7(2) . . . . ? Cu3 N8 C36 C35 -8.0(3) . . . . ? N7 C35 C36 N8 -0.4(3) . . . . ? C34 C35 C36 N8 -178.2(2) . . . . ? N7 C35 C36 C37 177.0(2) . . . . ? C34 C35 C36 C37 -0.9(4) . . . . ? N8 C36 C37 C38 1.3(3) . . . . ? C35 C36 C37 C38 -175.9(2) . . . . ? C36 C37 C38 C39 0.0(3) . . . . ? C36 C37 C38 C23 179.4(2) . . . 2_557 ? C37 C38 C39 C40 -0.9(3) . . . . ? C23 C38 C39 C40 179.7(2) 2_557 . . . ? C36 N8 C40 C39 1.0(3) . . . . ? Cu3 N8 C40 C39 -175.38(17) . . . . ? C36 N8 C40 C41 -175.9(2) . . . . ? Cu3 N8 C40 C41 7.7(3) . . . . ? C38 C39 C40 N8 0.4(3) . . . . ? C38 C39 C40 C41 176.9(2) . . . . ? C45 N9 C41 C42 -0.9(3) . . . . ? Cu3 N9 C41 C42 178.84(19) . . . . ? C45 N9 C41 C40 176.6(2) . . . . ? Cu3 N9 C41 C40 -3.7(2) . . . . ? N8 C40 C41 N9 -2.2(3) . . . . ? C39 C40 C41 N9 -178.9(2) . . . . ? N8 C40 C41 C42 175.2(2) . . . . ? C39 C40 C41 C42 -1.5(4) . . . . ? N9 C41 C42 C43 2.2(4) . . . . ? C40 C41 C42 C43 -175.0(2) . . . . ? C41 C42 C43 C44 -0.8(4) . . . . ? C42 C43 C44 C45 -1.6(4) . . . . ? C41 N9 C45 C44 -1.7(3) . . . . ? Cu3 N9 C45 C44 178.61(18) . . . . ? C43 C44 C45 N9 3.0(4) . . . . ? C51 C46 C47 P1 175.41(17) 1_665 . . . ? O5 P1 C47 C46 170.52(17) . . . . ? O4 P1 C47 C46 43.7(2) . . . . ? O3 P1 C47 C46 -72.5(2) . . . . ? O10 P3 C48 C49 65.65(19) . . . . ? O9 P3 C48 C49 -55.17(19) . . . . ? O11 P3 C48 C49 -174.91(16) . . . . ? P3 C48 C49 C50 159.18(16) . . . . ? C48 C49 C50 P2 -173.61(16) . . . 2_566 ? O16 P4 C51 C46 57.6(2) . . . 1_445 ? O15 P4 C51 C46 -70.12(19) . . . 1_445 ? O14 P4 C51 C46 -175.97(16) . . . 1_445 ? _diffrn_measured_fraction_theta_max 0.979 _diffrn_reflns_theta_full 31.51 _diffrn_measured_fraction_theta_full 0.979 _refine_diff_density_max 1.000 _refine_diff_density_min -1.110 _refine_diff_density_rms 0.116 data_publication_text_compound_8 _database_code_depnum_ccdc_archive 'CCDC 247637' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '[{Cu2(bisterpy)}V4F2O6{O3P(CH2)4PO3}2]' _chemical_formula_sum 'C19 H18 Cu F N3 O9 P2 V2' _chemical_formula_weight 678.72 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' F F 0.0171 0.0103 '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 23.4642(12) _cell_length_b 14.3545(7) _cell_length_c 17.1194(9) _cell_angle_alpha 90.00 _cell_angle_beta 127.5000(10) _cell_angle_gamma 90.00 _cell_volume 4574.6(4) _cell_formula_units_Z 8 _cell_measurement_temperature 90(2) _cell_measurement_reflns_used 29506 _cell_measurement_theta_min 1.79 _cell_measurement_theta_max 31.50 _exptl_crystal_description black _exptl_crystal_colour plate _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.971 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2712 _exptl_absorpt_coefficient_mu 1.929 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6989 _exptl_absorpt_correction_T_max 0.8930 _exptl_absorpt_process_details 'SADABS SHELXL-97 (SHELDRICK, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 90(2) _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_probe x-ray _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'APEX CCD area detector' _diffrn_measurement_method 'Phi and omega scans' _diffrn_detector_area_resol_mean 512 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.001 _diffrn_reflns_number 29506 _diffrn_reflns_av_R_equivalents 0.0614 _diffrn_reflns_av_sigmaI/netI 0.0601 _diffrn_reflns_limit_h_min -34 _diffrn_reflns_limit_h_max 34 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.79 _diffrn_reflns_theta_max 31.50 _reflns_number_total 7623 _reflns_number_gt 5276 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL and CrystalMaker 5.x' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0490P)^2^+0.6793P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7623 _refine_ls_number_parameters 334 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0913 _refine_ls_R_factor_gt 0.0540 _refine_ls_wR_factor_ref 0.1162 _refine_ls_wR_factor_gt 0.1028 _refine_ls_goodness_of_fit_ref 1.019 _refine_ls_restrained_S_all 1.019 _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 0.29694(2) 0.37070(3) 0.35324(3) 0.01360(10) Uani 1 1 d . . . V1 V 0.27865(3) 0.61890(4) 0.30749(4) 0.01245(12) Uani 1 1 d . . . V2 V 0.02581(3) 0.40838(4) 0.06687(4) 0.01173(12) Uani 1 1 d . . . P1 P 0.32509(4) 0.82159(6) 0.38582(6) 0.01183(17) Uani 1 1 d . . . P2 P 0.10665(4) 0.60184(6) 0.16298(6) 0.01321(17) Uani 1 1 d . . . F1 F -0.03903(9) 0.51265(12) 0.02819(13) 0.0142(4) Uani 1 1 d . . . O1 O 0.23252(12) 0.36176(18) 0.21457(17) 0.0212(5) Uani 1 1 d . . . O2 O 0.29225(12) 0.52515(16) 0.36982(17) 0.0191(5) Uani 1 1 d . . . O3 O 0.30566(12) 0.71791(16) 0.39101(16) 0.0146(5) Uani 1 1 d . . . O4 O 0.32861(13) 0.61556(18) 0.27158(18) 0.0230(6) Uani 1 1 d . . . O5 O 0.18421(12) 0.63285(16) 0.20087(17) 0.0188(5) Uani 1 1 d . . . O6 O 0.10402(11) 0.49666(16) 0.16574(16) 0.0155(5) Uani 1 1 d . . . O7 O 0.09948(11) 0.32204(16) 0.08317(16) 0.0153(5) Uani 1 1 d . . . O8 O 0.01247(12) 0.35228(16) 0.13540(17) 0.0163(5) Uani 1 1 d . . . O9 O -0.05377(11) 0.35079(16) -0.06445(16) 0.0151(5) Uani 1 1 d . . . N1 N 0.23409(13) 0.35572(19) 0.39492(19) 0.0134(5) Uani 1 1 d . . . N2 N 0.36962(13) 0.36238(18) 0.49470(19) 0.0126(5) Uani 1 1 d . . . N3 N 0.38723(14) 0.3794(2) 0.3637(2) 0.0165(6) Uani 1 1 d . . . C1 C 0.16259(16) 0.3510(2) 0.3354(2) 0.0146(6) Uani 1 1 d . . . H1 H 0.1386 0.3434 0.2681 0.018 Uiso 1 1 calc R . . C2 C 0.12258(17) 0.3570(2) 0.3709(2) 0.0160(7) Uani 1 1 d . . . H2 H 0.0727 0.3549 0.3278 0.019 Uiso 1 1 calc R . . C3 C 0.15843(17) 0.3663(2) 0.4714(2) 0.0167(7) Uani 1 1 d . . . H3 H 0.1330 0.3698 0.4968 0.020 Uiso 1 1 calc R . . C4 C 0.23368(16) 0.3702(2) 0.5340(2) 0.0154(6) Uani 1 1 d . . . H4 H 0.2590 0.3764 0.6017 0.018 Uiso 1 1 calc R . . C5 C 0.26928(16) 0.3650(2) 0.4941(2) 0.0130(6) Uani 1 1 d . . . C6 C 0.34862(17) 0.3662(2) 0.5517(2) 0.0153(6) Uani 1 1 d . . . C7 C 0.39897(17) 0.3692(2) 0.6529(2) 0.0152(6) Uani 1 1 d . . . H7 H 0.3844 0.3745 0.6926 0.018 Uiso 1 1 calc R . . C8 C 0.47257(16) 0.3639(2) 0.6956(2) 0.0133(6) Uani 1 1 d . . . C9 C 0.49189(17) 0.3589(2) 0.6331(2) 0.0166(7) Uani 1 1 d . . . H9 H 0.5400 0.3541 0.6590 0.020 Uiso 1 1 calc R . . C10 C 0.43896(16) 0.3612(2) 0.5322(2) 0.0146(6) Uani 1 1 d . . . C11 C 0.44950(16) 0.3693(2) 0.4562(2) 0.0155(7) Uani 1 1 d . . . C12 C 0.51533(18) 0.3728(3) 0.4747(3) 0.0228(8) Uani 1 1 d . . . H12 H 0.5573 0.3631 0.5380 0.027 Uiso 1 1 calc R . . C13 C 0.51820(19) 0.3907(3) 0.3976(3) 0.0285(9) Uani 1 1 d . . . H13 H 0.5621 0.3933 0.4085 0.034 Uiso 1 1 calc R . . C14 C 0.4546(2) 0.4049(3) 0.3040(3) 0.0302(9) Uani 1 1 d . . . H14 H 0.4554 0.4192 0.2516 0.036 Uiso 1 1 calc R . . C15 C 0.39014(19) 0.3975(3) 0.2895(3) 0.0239(8) Uani 1 1 d . . . H15 H 0.3475 0.4053 0.2264 0.029 Uiso 1 1 calc R . . C16 C 0.32075(18) 0.8810(2) 0.4737(2) 0.0177(7) Uani 1 1 d . . . H16A H 0.3336 0.9457 0.4761 0.021 Uiso 1 1 calc R . . H16B H 0.2715 0.8795 0.4510 0.021 Uiso 1 1 calc R . . C17 C 0.3691(2) 0.8414(3) 0.5779(3) 0.0227(8) Uani 1 1 d . . . H17A H 0.3600 0.7751 0.5752 0.027 Uiso 1 1 calc R . . H17B H 0.4189 0.8492 0.6040 0.027 Uiso 1 1 calc R . . C18 C 0.0943(2) 0.6496(3) 0.2486(3) 0.0267(9) Uani 1 1 d . . . H18A H 0.1013 0.7165 0.2511 0.032 Uiso 1 1 calc R . . H18B H 0.0448 0.6391 0.2225 0.032 Uiso 1 1 calc R . . C19 C 0.1421(2) 0.6128(3) 0.3526(3) 0.0215(7) Uani 1 1 d . . . H19A H 0.1918 0.6213 0.3786 0.026 Uiso 1 1 calc R . . H19B H 0.1338 0.5464 0.3510 0.026 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.00615(17) 0.0176(2) 0.00951(18) -0.00165(15) 0.00086(14) 0.00116(14) V1 0.0061(2) 0.0163(3) 0.0090(2) -0.0026(2) 0.00155(19) -0.00048(19) V2 0.0049(2) 0.0137(3) 0.0091(2) -0.0025(2) 0.00040(19) 0.00179(19) P1 0.0066(3) 0.0139(4) 0.0092(4) -0.0003(3) 0.0018(3) -0.0023(3) P2 0.0057(3) 0.0162(4) 0.0096(4) -0.0041(3) 0.0005(3) 0.0011(3) F1 0.0078(8) 0.0160(9) 0.0137(9) -0.0022(7) 0.0040(7) 0.0041(7) O1 0.0078(10) 0.0353(15) 0.0094(11) -0.0066(10) -0.0005(9) 0.0020(10) O2 0.0146(11) 0.0166(12) 0.0185(13) -0.0004(9) 0.0062(10) 0.0020(9) O3 0.0159(11) 0.0161(12) 0.0130(11) -0.0044(9) 0.0094(9) -0.0054(9) O4 0.0141(12) 0.0401(16) 0.0146(12) -0.0036(11) 0.0087(10) 0.0024(10) O5 0.0082(10) 0.0212(13) 0.0150(12) 0.0001(10) 0.0008(9) -0.0012(9) O6 0.0070(10) 0.0170(12) 0.0095(11) -0.0023(9) -0.0016(9) -0.0003(8) O7 0.0082(10) 0.0178(12) 0.0149(11) -0.0007(9) 0.0045(9) 0.0031(8) O8 0.0103(10) 0.0181(12) 0.0148(11) -0.0018(9) 0.0047(9) 0.0007(9) O9 0.0082(10) 0.0160(11) 0.0102(11) -0.0018(9) 0.0000(9) 0.0032(8) N1 0.0064(11) 0.0150(13) 0.0086(12) 0.0007(10) -0.0008(10) 0.0008(10) N2 0.0058(11) 0.0121(13) 0.0114(12) -0.0009(10) 0.0009(10) 0.0007(9) N3 0.0097(12) 0.0221(15) 0.0109(13) -0.0051(11) 0.0028(10) 0.0021(11) C1 0.0080(13) 0.0157(15) 0.0125(15) -0.0014(12) 0.0022(12) 0.0005(11) C2 0.0093(14) 0.0175(16) 0.0145(16) 0.0030(12) 0.0039(12) 0.0015(12) C3 0.0104(14) 0.0178(16) 0.0174(16) 0.0014(13) 0.0062(13) 0.0008(12) C4 0.0102(14) 0.0175(16) 0.0093(14) 0.0011(12) 0.0012(12) -0.0018(12) C5 0.0068(13) 0.0135(15) 0.0098(14) 0.0006(11) 0.0005(11) -0.0007(11) C6 0.0116(14) 0.0130(15) 0.0140(15) 0.0007(12) 0.0040(12) 0.0031(12) C7 0.0108(14) 0.0151(15) 0.0115(15) -0.0016(12) 0.0026(12) -0.0007(12) C8 0.0064(13) 0.0112(14) 0.0117(14) 0.0009(11) 0.0000(11) 0.0009(11) C9 0.0077(13) 0.0168(16) 0.0131(15) -0.0029(12) 0.0000(12) 0.0020(12) C10 0.0085(13) 0.0119(15) 0.0143(15) -0.0013(12) 0.0022(12) 0.0026(11) C11 0.0073(13) 0.0170(16) 0.0124(15) -0.0041(12) 0.0009(11) 0.0034(12) C12 0.0116(15) 0.029(2) 0.0172(17) -0.0052(15) 0.0035(13) 0.0013(14) C13 0.0109(16) 0.048(3) 0.022(2) -0.0086(17) 0.0075(15) 0.0000(15) C14 0.0173(18) 0.053(3) 0.0199(19) -0.0072(18) 0.0111(16) -0.0016(17) C15 0.0118(16) 0.037(2) 0.0127(16) -0.0034(15) 0.0024(13) 0.0045(14) C16 0.0136(15) 0.0154(16) 0.0138(16) -0.0022(12) 0.0029(13) 0.0019(12) C17 0.0226(18) 0.0265(19) 0.0129(16) -0.0009(14) 0.0076(14) 0.0074(15) C18 0.0254(19) 0.033(2) 0.0156(17) -0.0018(15) 0.0092(15) 0.0134(16) C19 0.0219(18) 0.0213(18) 0.0208(18) -0.0003(14) 0.0128(15) 0.0061(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 O1 1.889(2) . ? Cu1 N2 1.939(3) . ? Cu1 N1 2.003(3) . ? Cu1 N3 2.018(3) . ? Cu1 O2 2.246(2) . ? V1 O4 1.623(3) . ? V1 O2 1.624(2) . ? V1 O5 1.832(2) . ? V1 O3 1.834(2) . ? V2 O8 1.603(2) . ? V2 F1 1.9407(18) . ? V2 O7 2.004(2) . ? V2 O6 2.014(2) . ? V2 O9 2.028(2) . ? V2 F1 2.155(2) 5_565 ? P1 O7 1.507(2) 4 ? P1 O1 1.512(2) 4 ? P1 O3 1.575(2) . ? P1 C16 1.785(4) . ? P2 O6 1.513(2) . ? P2 O9 1.516(2) 5_565 ? P2 O5 1.579(2) . ? P2 C18 1.793(4) . ? F1 V2 2.155(2) 5_565 ? O1 P1 1.512(2) 4_545 ? O7 P1 1.507(2) 4_545 ? O9 P2 1.516(2) 5_565 ? N1 C1 1.333(4) . ? N1 C5 1.370(4) . ? N2 C6 1.336(4) . ? N2 C10 1.337(4) . ? N3 C15 1.339(5) . ? N3 C11 1.359(4) . ? C1 C2 1.398(5) . ? C2 C3 1.387(5) . ? C3 C4 1.402(4) . ? C4 C5 1.365(5) . ? C5 C6 1.484(4) . ? C6 C7 1.381(4) . ? C7 C8 1.409(4) . ? C8 C9 1.395(5) . ? C8 C8 1.486(6) 2_656 ? C9 C10 1.384(4) . ? C10 C11 1.468(5) . ? C11 C12 1.376(5) . ? C12 C13 1.386(5) . ? C13 C14 1.387(5) . ? C14 C15 1.380(5) . ? C16 C17 1.526(5) . ? C17 C19 1.515(5) 7_566 ? C18 C19 1.509(5) . ? C19 C17 1.515(5) 7_566 ? 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 171.14(11) . . ? O1 Cu1 N1 103.94(11) . . ? N2 Cu1 N1 80.03(11) . . ? O1 Cu1 N3 96.29(11) . . ? N2 Cu1 N3 79.36(11) . . ? N1 Cu1 N3 159.35(11) . . ? O1 Cu1 O2 99.36(10) . . ? N2 Cu1 O2 88.65(10) . . ? N1 Cu1 O2 87.57(10) . . ? N3 Cu1 O2 93.29(10) . . ? O4 V1 O2 109.04(13) . . ? O4 V1 O5 109.90(12) . . ? O2 V1 O5 112.33(11) . . ? O4 V1 O3 109.38(12) . . ? O2 V1 O3 107.07(12) . . ? O5 V1 O3 109.05(11) . . ? O8 V2 F1 100.10(10) . . ? O8 V2 O7 97.10(11) . . ? F1 V2 O7 162.78(9) . . ? O8 V2 O6 100.66(11) . . ? F1 V2 O6 85.73(8) . . ? O7 V2 O6 90.27(9) . . ? O8 V2 O9 98.53(11) . . ? F1 V2 O9 86.25(8) . . ? O7 V2 O9 92.08(9) . . ? O6 V2 O9 160.22(10) . . ? O8 V2 F1 177.27(10) . 5_565 ? F1 V2 F1 77.29(8) . 5_565 ? O7 V2 F1 85.52(8) . 5_565 ? O6 V2 F1 80.06(9) . 5_565 ? O9 V2 F1 80.56(8) . 5_565 ? O7 P1 O1 116.40(14) 4 4 ? O7 P1 O3 107.60(13) 4 . ? O1 P1 O3 109.60(13) 4 . ? O7 P1 C16 111.00(15) 4 . ? O1 P1 C16 107.80(15) 4 . ? O3 P1 C16 103.69(15) . . ? O6 P2 O9 117.45(13) . 5_565 ? O6 P2 O5 109.09(13) . . ? O9 P2 O5 106.77(14) 5_565 . ? O6 P2 C18 109.05(18) . . ? O9 P2 C18 107.91(15) 5_565 . ? O5 P2 C18 105.97(17) . . ? V2 F1 V2 102.71(8) . 5_565 ? P1 O1 Cu1 158.81(19) 4_545 . ? V1 O2 Cu1 137.74(14) . . ? P1 O3 V1 131.53(15) . . ? P2 O5 V1 140.42(16) . . ? P2 O6 V2 129.43(13) . . ? P1 O7 V2 141.30(15) 4_545 . ? P2 O9 V2 128.91(14) 5_565 . ? C1 N1 C5 118.8(3) . . ? C1 N1 Cu1 126.2(2) . . ? C5 N1 Cu1 114.4(2) . . ? C6 N2 C10 122.2(3) . . ? C6 N2 Cu1 118.4(2) . . ? C10 N2 Cu1 119.2(2) . . ? C15 N3 C11 119.1(3) . . ? C15 N3 Cu1 125.8(2) . . ? C11 N3 Cu1 115.0(2) . . ? N1 C1 C2 122.0(3) . . ? C3 C2 C1 119.0(3) . . ? C2 C3 C4 118.9(3) . . ? C5 C4 C3 119.0(3) . . ? C4 C5 N1 122.3(3) . . ? C4 C5 C6 124.7(3) . . ? N1 C5 C6 113.0(3) . . ? N2 C6 C7 120.2(3) . . ? N2 C6 C5 112.7(3) . . ? C7 C6 C5 127.1(3) . . ? C6 C7 C8 119.4(3) . . ? C9 C8 C7 118.2(3) . . ? C9 C8 C8 121.6(4) . 2_656 ? C7 C8 C8 120.2(4) . 2_656 ? C10 C9 C8 119.5(3) . . ? N2 C10 C9 120.3(3) . . ? N2 C10 C11 112.7(3) . . ? C9 C10 C11 126.9(3) . . ? N3 C11 C12 121.6(3) . . ? N3 C11 C10 113.5(3) . . ? C12 C11 C10 124.8(3) . . ? C11 C12 C13 119.1(3) . . ? C12 C13 C14 119.1(4) . . ? C15 C14 C13 119.1(4) . . ? N3 C15 C14 121.9(3) . . ? C17 C16 P1 115.1(2) . . ? C19 C17 C16 113.3(3) 7_566 . ? C19 C18 P2 117.2(3) . . ? C18 C19 C17 114.6(3) . 7_566 ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 31.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.925 _refine_diff_density_min -0.725 _refine_diff_density_rms 0.154 data_publication_text_compound_9 _database_code_depnum_ccdc_archive 'CCDC 247638' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ; [{Cu2(bisterpy)}V4F4O4(OH)(H2O){HO3P(CH2)5PO3}{O3P(CH2)5PO3}]·H2O ; _chemical_formula_sum 'C40 H46 Cu2 F4 N6 O19 P4 V4' _chemical_formula_weight 1445.55 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 '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' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.9835(7) _cell_length_b 11.0327(7) _cell_length_c 21.7243(14) _cell_angle_alpha 90.9850(10) _cell_angle_beta 96.6920(10) _cell_angle_gamma 102.6760(10) _cell_volume 2548.4(3) _cell_formula_units_Z 2 _cell_measurement_temperature 90(2) _cell_measurement_reflns_used 32850 _cell_measurement_theta_min 1.89 _cell_measurement_theta_max 31.51 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.884 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1452 _exptl_absorpt_coefficient_mu 1.745 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7442 _exptl_absorpt_correction_T_max 0.7923 _exptl_absorpt_process_details 'SADABS SHELXL-97 (SHELDRICK, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 90(2) _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_probe x-ray _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'APEX CCD area detector' _diffrn_measurement_method 'Phi and omega scans' _diffrn_detector_area_resol_mean 512 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.001 _diffrn_reflns_number 32850 _diffrn_reflns_av_R_equivalents 0.0493 _diffrn_reflns_av_sigmaI/netI 0.0678 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 1.89 _diffrn_reflns_theta_max 31.51 _reflns_number_total 16522 _reflns_number_gt 11557 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0542P)^2^+0.3427P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 16522 _refine_ls_number_parameters 712 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0917 _refine_ls_R_factor_gt 0.0564 _refine_ls_wR_factor_ref 0.1281 _refine_ls_wR_factor_gt 0.1153 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_restrained_S_all 1.031 _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 0.92806(4) 0.41375(4) 0.425288(19) 0.00928(9) Uani 1 1 d . . . Cu2 Cu 0.57380(4) -0.38705(4) 0.066542(19) 0.00829(9) Uani 1 1 d . . . V1 V 1.06801(5) 0.26070(5) 0.21868(3) 0.00921(11) Uani 1 1 d . . . V2 V 0.86487(5) 0.13378(5) 0.33632(3) 0.00814(11) Uani 1 1 d . . . V3 V 0.61341(5) -0.07258(5) 0.11656(3) 0.00833(11) Uani 1 1 d . . . V4 V 0.38017(6) -0.27629(6) 0.27137(3) 0.01055(12) Uani 1 1 d . . . P1 P 1.12692(8) 0.31219(8) 0.36628(4) 0.00912(16) Uani 1 1 d . . . P2 P 0.87281(8) 0.11474(8) 0.10017(4) 0.01030(17) Uani 1 1 d . . . P3 P 0.58859(8) -0.02412(8) 0.26366(4) 0.00860(16) Uani 1 1 d . . . P4 P 0.37208(8) -0.27557(8) 0.11436(4) 0.00808(16) Uani 1 1 d . . . F1 F 1.1201(2) 0.4169(2) 0.18163(10) 0.0178(5) Uani 1 1 d . . . F2 F 0.8475(2) 0.0225(2) 0.39990(10) 0.0163(4) Uani 1 1 d . . . F3 F 0.6093(2) -0.0040(2) 0.03432(10) 0.0188(5) Uani 1 1 d . . . F4 F 0.4288(2) -0.3346(2) 0.34935(10) 0.0177(5) Uani 1 1 d . . . O1 O 0.8127(2) 0.2525(2) 0.35666(11) 0.0110(5) Uani 1 1 d . . . O2 O 1.0923(2) 0.4071(2) 0.40945(11) 0.0118(5) Uani 1 1 d . . . O3 O 1.1224(2) 0.3574(2) 0.29945(11) 0.0122(5) Uani 1 1 d . . . O4 O 1.0435(2) 0.1818(2) 0.36913(11) 0.0104(5) Uani 1 1 d . . . O5 O 1.1696(2) 0.1782(2) 0.21772(12) 0.0154(5) Uani 1 1 d . . . O6 O 0.9190(2) 0.1699(2) 0.25321(11) 0.0138(5) Uani 1 1 d . . . O7 O 0.7284(2) 0.0167(2) 0.28688(12) 0.0129(5) Uani 1 1 d . . . O8 O 0.9688(2) 0.2224(2) 0.13505(11) 0.0119(5) Uani 1 1 d . . . O9 O 0.7670(2) 0.0632(2) 0.13956(11) 0.0109(5) Uani 1 1 d . . . O10 O 0.8182(2) 0.1596(2) 0.03802(11) 0.0155(5) Uani 1 1 d . . . O11 O 0.5635(2) -0.0228(2) 0.19314(11) 0.0104(5) Uani 1 1 d . . . O12 O 0.5377(2) -0.1517(2) 0.28838(11) 0.0129(5) Uani 1 1 d . . . O13 O 0.6709(2) -0.1951(2) 0.11766(11) 0.0113(5) Uani 1 1 d . . . O14 O 0.4364(2) -0.1501(2) 0.09042(11) 0.0109(5) Uani 1 1 d . . . O15 O 0.4042(2) -0.2849(2) 0.18393(11) 0.0106(5) Uani 1 1 d . . . O16 O 0.2692(3) -0.2072(3) 0.27844(13) 0.0212(6) Uani 1 1 d . . . O17 O 0.2977(3) -0.4600(3) 0.25537(12) 0.0206(6) Uani 1 1 d . . . O18 O 0.4064(2) -0.3836(2) 0.07945(11) 0.0090(5) Uani 1 1 d . . . O91 O 0.6373(3) 0.8538(3) 0.43285(16) 0.0366(8) Uani 1 1 d . . . N1 N 0.9093(3) 0.2971(3) 0.49579(13) 0.0121(6) Uani 1 1 d . . . N2 N 0.7782(3) 0.4472(3) 0.45263(13) 0.0085(5) Uani 1 1 d . . . N3 N 0.9013(3) 0.5521(3) 0.36873(14) 0.0117(6) Uani 1 1 d . . . N4 N 0.6216(3) -0.4828(3) 0.14018(13) 0.0091(5) Uani 1 1 d . . . N5 N 0.7287(3) -0.4222(3) 0.04422(13) 0.0085(5) Uani 1 1 d . . . N6 N 0.5738(3) -0.3180(3) -0.01882(13) 0.0097(5) Uani 1 1 d . . . C1 C 0.9811(3) 0.2177(3) 0.51399(16) 0.0148(7) Uani 1 1 d . . . H1 H 1.0543 0.2185 0.4945 0.018 Uiso 1 1 calc R . . C2 C 0.9533(4) 0.1342(4) 0.56014(18) 0.0201(8) Uani 1 1 d . . . H2 H 1.0050 0.0774 0.5711 0.024 Uiso 1 1 calc R . . C3 C 0.8484(4) 0.1355(4) 0.58987(19) 0.0208(8) Uani 1 1 d . . . H3 H 0.8288 0.0814 0.6226 0.025 Uiso 1 1 calc R . . C4 C 0.7724(4) 0.2166(4) 0.57114(17) 0.0181(8) Uani 1 1 d . . . H4 H 0.6995 0.2183 0.5905 0.022 Uiso 1 1 calc R . . C5 C 0.8043(3) 0.2944(3) 0.52414(16) 0.0126(7) Uani 1 1 d . . . C6 C 0.7294(3) 0.3831(3) 0.49897(15) 0.0102(6) Uani 1 1 d . . . C7 C 0.6192(3) 0.4013(3) 0.51863(16) 0.0105(6) Uani 1 1 d . . . H7 H 0.5845 0.3551 0.5514 0.013 Uiso 1 1 calc R . . C8 C 0.5594(3) 0.4887(3) 0.48964(16) 0.0108(6) Uani 1 1 d . . . C9 C 0.6123(3) 0.5540(3) 0.44090(16) 0.0110(6) Uani 1 1 d . . . H9 H 0.5730 0.6129 0.4200 0.013 Uiso 1 1 calc R . . C10 C 0.7232(3) 0.5311(3) 0.42377(16) 0.0103(6) Uani 1 1 d . . . C11 C 0.7941(3) 0.5932(3) 0.37426(17) 0.0134(7) Uani 1 1 d . . . C12 C 0.7587(4) 0.6833(3) 0.33769(17) 0.0163(7) Uani 1 1 d . . . H12 H 0.6824 0.7083 0.3417 0.020 Uiso 1 1 calc R . . C13 C 0.8370(4) 0.7373(4) 0.29460(18) 0.0189(8) Uani 1 1 d . . . H13 H 0.8155 0.8005 0.2692 0.023 Uiso 1 1 calc R . . C14 C 0.9468(4) 0.6972(4) 0.28951(18) 0.0201(8) Uani 1 1 d . . . H14 H 1.0019 0.7331 0.2608 0.024 Uiso 1 1 calc R . . C15 C 0.9748(3) 0.6040(3) 0.32685(17) 0.0149(7) Uani 1 1 d . . . H15 H 1.0492 0.5757 0.3226 0.018 Uiso 1 1 calc R . . C16 C 0.5581(3) -0.5074(3) 0.18915(16) 0.0128(7) Uani 1 1 d . . . H16 H 0.4813 -0.4814 0.1897 0.015 Uiso 1 1 calc R . . C17 C 0.6016(4) -0.5701(3) 0.23932(17) 0.0163(7) Uani 1 1 d . . . H17A H 0.5556 -0.5858 0.2738 0.020 Uiso 1 1 calc R . . C18 C 0.7131(4) -0.6093(4) 0.23814(17) 0.0169(7) Uani 1 1 d . . . H18 H 0.7442 -0.6528 0.2716 0.020 Uiso 1 1 calc R . . C19 C 0.7788(3) -0.5837(3) 0.18701(17) 0.0142(7) Uani 1 1 d . . . H19 H 0.8557 -0.6090 0.1853 0.017 Uiso 1 1 calc R . . C20 C 0.7308(3) -0.5210(3) 0.13892(16) 0.0104(6) Uani 1 1 d . . . C21 C 0.7915(3) -0.4884(3) 0.08199(15) 0.0091(6) Uani 1 1 d . . . C22 C 0.8988(3) -0.5213(3) 0.06625(16) 0.0102(6) Uani 1 1 d . . . H22 H 0.9421 -0.5692 0.0931 0.012 Uiso 1 1 calc R . . C23 C 0.9432(3) -0.4825(3) 0.00962(15) 0.0083(6) Uani 1 1 d . . . C24 C 0.8759(3) -0.4114(3) -0.02857(15) 0.0094(6) Uani 1 1 d . . . H24 H 0.9033 -0.3832 -0.0668 0.011 Uiso 1 1 calc R . . C25 C 0.7683(3) -0.3832(3) -0.00924(15) 0.0084(6) Uani 1 1 d . . . C26 C 0.6815(3) -0.3164(3) -0.04498(16) 0.0098(6) Uani 1 1 d . . . C27 C 0.7053(3) -0.2570(4) -0.09873(17) 0.0161(7) Uani 1 1 d . . . H27 H 0.7826 -0.2539 -0.1150 0.019 Uiso 1 1 calc R . . C28 C 0.6146(4) -0.2014(3) -0.12902(17) 0.0155(7) Uani 1 1 d . . . H28 H 0.6290 -0.1600 -0.1663 0.019 Uiso 1 1 calc R . . C29 C 0.5029(3) -0.2071(3) -0.10420(16) 0.0126(7) Uani 1 1 d . . . H29 H 0.4383 -0.1725 -0.1250 0.015 Uiso 1 1 calc R . . C30 C 0.4873(3) -0.2643(3) -0.04837(16) 0.0116(6) Uani 1 1 d . . . H30 H 0.4122 -0.2652 -0.0305 0.014 Uiso 1 1 calc R . . C31 C 0.5070(3) 0.0837(3) 0.29297(16) 0.0139(7) Uani 1 1 d . . . H31A H 0.5460 0.1683 0.2810 0.017 Uiso 1 1 calc R . . H31B H 0.4188 0.0631 0.2731 0.017 Uiso 1 1 calc R . . C32 C 0.5075(3) 0.0846(4) 0.36351(17) 0.0154(7) Uani 1 1 d . . . H32A H 0.4516 0.0069 0.3746 0.018 Uiso 1 1 calc R . . H32B H 0.5937 0.0857 0.3833 0.018 Uiso 1 1 calc R . . C33 C 0.4646(3) 0.1957(4) 0.38953(18) 0.0174(8) Uani 1 1 d . . . H33A H 0.5257 0.2731 0.3825 0.021 Uiso 1 1 calc R . . H33B H 0.4640 0.1887 0.4349 0.021 Uiso 1 1 calc R . . C34 C 0.3337(3) 0.2045(4) 0.35992(18) 0.0169(7) Uani 1 1 d . . . H34A H 0.2747 0.1229 0.3612 0.020 Uiso 1 1 calc R . . H34B H 0.3370 0.2253 0.3159 0.020 Uiso 1 1 calc R . . C35 C 1.2851(3) 0.3044(3) 0.39406(17) 0.0137(7) Uani 1 1 d . . . H35A H 1.3412 0.3865 0.3898 0.016 Uiso 1 1 calc R . . H35B H 1.2899 0.2873 0.4388 0.016 Uiso 1 1 calc R . . C36 C 0.2064(3) -0.2877(3) 0.09778(17) 0.0114(6) Uani 1 1 d . . . H36A H 0.1821 -0.2993 0.0524 0.014 Uiso 1 1 calc R . . H36B H 0.1616 -0.3621 0.1173 0.014 Uiso 1 1 calc R . . C37 C 0.1648(3) -0.1727(3) 0.12125(17) 0.0130(7) Uani 1 1 d . . . H37A H 0.2087 -0.1465 0.1634 0.016 Uiso 1 1 calc R . . H37B H 0.1888 -0.1034 0.0936 0.016 Uiso 1 1 calc R . . C38 C 0.0238(3) -0.1996(3) 0.12316(18) 0.0159(7) Uani 1 1 d . . . H38A H 0.0016 -0.2643 0.1535 0.019 Uiso 1 1 calc R . . H38B H -0.0192 -0.2337 0.0819 0.019 Uiso 1 1 calc R . . C39 C -0.0253(3) -0.0857(3) 0.14076(17) 0.0136(7) Uani 1 1 d . . . H39A H 0.0377 -0.0323 0.1718 0.016 Uiso 1 1 calc R . . H39B H -0.1035 -0.1134 0.1600 0.016 Uiso 1 1 calc R . . C40 C 0.9480(3) -0.0093(3) 0.08445(16) 0.0143(7) Uani 1 1 d . . . H40A H 0.8940 -0.0658 0.0514 0.017 Uiso 1 1 calc R . . H40B H 1.0285 0.0262 0.0684 0.017 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 0.00898(19) 0.0127(2) 0.00820(19) 0.00046(15) 0.00316(15) 0.00561(16) Cu2 0.00813(19) 0.0107(2) 0.00781(19) 0.00085(15) 0.00260(15) 0.00510(15) V1 0.0085(3) 0.0109(3) 0.0083(3) -0.0003(2) 0.0024(2) 0.0018(2) V2 0.0077(3) 0.0091(3) 0.0081(3) -0.0002(2) 0.0019(2) 0.0025(2) V3 0.0084(3) 0.0088(3) 0.0083(3) -0.0007(2) 0.0017(2) 0.0028(2) V4 0.0105(3) 0.0130(3) 0.0086(3) 0.0005(2) 0.0022(2) 0.0030(2) P1 0.0069(4) 0.0115(4) 0.0094(4) -0.0021(3) 0.0018(3) 0.0027(3) P2 0.0090(4) 0.0120(4) 0.0097(4) -0.0017(3) 0.0026(3) 0.0014(3) P3 0.0085(4) 0.0094(4) 0.0080(4) -0.0014(3) 0.0018(3) 0.0021(3) P4 0.0073(4) 0.0097(4) 0.0078(4) -0.0005(3) 0.0016(3) 0.0026(3) F1 0.0214(12) 0.0133(10) 0.0144(11) 0.0007(8) -0.0004(9) -0.0036(9) F2 0.0138(10) 0.0168(11) 0.0183(11) 0.0070(9) 0.0000(8) 0.0040(9) F3 0.0159(11) 0.0214(12) 0.0180(11) 0.0012(9) 0.0016(9) 0.0019(9) F4 0.0169(11) 0.0235(12) 0.0117(10) 0.0047(9) 0.0023(8) 0.0019(9) O1 0.0115(12) 0.0114(11) 0.0107(11) -0.0008(9) 0.0001(9) 0.0047(9) O2 0.0093(11) 0.0155(12) 0.0121(12) -0.0029(9) 0.0032(9) 0.0055(10) O3 0.0123(12) 0.0135(12) 0.0101(12) -0.0022(9) 0.0024(9) 0.0011(10) O4 0.0071(11) 0.0111(11) 0.0129(12) -0.0006(9) 0.0014(9) 0.0015(9) O5 0.0136(12) 0.0216(14) 0.0119(12) -0.0028(10) 0.0019(10) 0.0059(11) O6 0.0119(12) 0.0174(13) 0.0108(12) -0.0006(10) 0.0034(9) -0.0007(10) O7 0.0102(12) 0.0135(12) 0.0145(12) -0.0018(10) 0.0028(9) 0.0012(10) O8 0.0103(12) 0.0124(12) 0.0117(12) 0.0001(9) 0.0013(9) 0.0000(9) O9 0.0107(12) 0.0104(11) 0.0120(12) -0.0011(9) 0.0020(9) 0.0027(9) O10 0.0184(13) 0.0176(13) 0.0090(12) 0.0027(10) -0.0002(10) 0.0016(11) O11 0.0113(12) 0.0120(12) 0.0087(11) -0.0006(9) 0.0028(9) 0.0032(9) O12 0.0125(12) 0.0125(12) 0.0134(12) 0.0015(9) 0.0005(10) 0.0028(10) O13 0.0094(11) 0.0101(11) 0.0142(12) -0.0023(9) -0.0013(9) 0.0034(9) O14 0.0105(12) 0.0116(12) 0.0108(11) 0.0027(9) 0.0018(9) 0.0024(9) O15 0.0115(12) 0.0127(12) 0.0079(11) 0.0011(9) 0.0020(9) 0.0029(9) O16 0.0172(14) 0.0327(16) 0.0188(14) 0.0028(12) 0.0061(11) 0.0145(12) O17 0.0206(14) 0.0204(14) 0.0159(13) 0.0004(11) 0.0019(11) -0.0055(11) O18 0.0092(11) 0.0087(11) 0.0104(11) -0.0019(9) 0.0032(9) 0.0037(9) O91 0.039(2) 0.0314(19) 0.039(2) 0.0001(15) 0.0135(16) 0.0046(15) N1 0.0131(14) 0.0165(15) 0.0095(13) 0.0009(11) 0.0038(11) 0.0081(12) N2 0.0085(13) 0.0095(13) 0.0089(13) -0.0017(10) 0.0027(10) 0.0045(10) N3 0.0111(14) 0.0147(14) 0.0113(14) 0.0003(11) 0.0030(11) 0.0061(11) N4 0.0086(13) 0.0089(13) 0.0108(13) -0.0012(10) 0.0025(10) 0.0033(10) N5 0.0094(13) 0.0103(13) 0.0070(12) 0.0008(10) 0.0030(10) 0.0034(11) N6 0.0096(13) 0.0109(13) 0.0107(13) 0.0008(11) 0.0040(11) 0.0054(11) C1 0.0162(18) 0.0196(18) 0.0121(16) 0.0005(14) 0.0046(13) 0.0103(14) C2 0.024(2) 0.023(2) 0.0187(19) 0.0041(15) 0.0039(15) 0.0154(17) C3 0.023(2) 0.024(2) 0.021(2) 0.0086(16) 0.0087(16) 0.0141(17) C4 0.023(2) 0.0206(19) 0.0157(18) 0.0073(15) 0.0084(15) 0.0126(16) C5 0.0152(17) 0.0133(16) 0.0110(16) 0.0000(13) 0.0018(13) 0.0069(13) C6 0.0104(16) 0.0137(16) 0.0078(15) -0.0010(12) 0.0012(12) 0.0058(13) C7 0.0101(16) 0.0128(16) 0.0103(15) -0.0005(12) 0.0032(12) 0.0051(13) C8 0.0095(15) 0.0129(16) 0.0103(15) -0.0033(12) 0.0003(12) 0.0037(13) C9 0.0106(16) 0.0130(16) 0.0112(15) 0.0005(12) 0.0032(12) 0.0057(13) C10 0.0086(15) 0.0121(15) 0.0106(15) -0.0008(12) 0.0019(12) 0.0030(12) C11 0.0137(17) 0.0125(16) 0.0146(17) -0.0008(13) 0.0037(13) 0.0034(13) C12 0.0153(18) 0.0187(18) 0.0185(18) 0.0034(15) 0.0052(14) 0.0097(14) C13 0.023(2) 0.0193(19) 0.0194(19) 0.0081(15) 0.0091(15) 0.0114(16) C14 0.0196(19) 0.024(2) 0.021(2) 0.0094(16) 0.0109(16) 0.0094(16) C15 0.0141(17) 0.0159(17) 0.0168(18) 0.0019(14) 0.0070(14) 0.0055(14) C16 0.0130(17) 0.0141(16) 0.0136(16) 0.0002(13) 0.0051(13) 0.0061(13) C17 0.0204(19) 0.0185(18) 0.0129(17) 0.0034(14) 0.0078(14) 0.0075(15) C18 0.0210(19) 0.0200(19) 0.0128(17) 0.0061(14) 0.0025(14) 0.0104(15) C19 0.0143(17) 0.0178(18) 0.0137(17) 0.0037(14) 0.0040(13) 0.0092(14) C20 0.0106(16) 0.0120(15) 0.0105(15) -0.0004(12) 0.0027(12) 0.0055(13) C21 0.0084(15) 0.0097(15) 0.0095(15) -0.0011(12) 0.0019(12) 0.0022(12) C22 0.0084(15) 0.0100(15) 0.0129(16) -0.0009(12) 0.0023(12) 0.0031(12) C23 0.0063(14) 0.0089(14) 0.0104(15) -0.0006(12) 0.0008(12) 0.0032(12) C24 0.0091(15) 0.0116(15) 0.0084(15) -0.0005(12) 0.0018(12) 0.0040(12) C25 0.0111(15) 0.0074(14) 0.0076(14) -0.0008(11) 0.0013(12) 0.0042(12) C26 0.0096(15) 0.0099(15) 0.0115(15) -0.0021(12) 0.0011(12) 0.0061(12) C27 0.0137(17) 0.0230(19) 0.0144(17) 0.0048(14) 0.0051(14) 0.0078(15) C28 0.0198(19) 0.0180(18) 0.0117(16) 0.0060(14) 0.0037(14) 0.0090(15) C29 0.0161(17) 0.0115(16) 0.0121(16) 0.0007(13) -0.0001(13) 0.0079(13) C30 0.0134(16) 0.0117(16) 0.0109(15) -0.0024(12) 0.0023(13) 0.0053(13) C31 0.0151(17) 0.0151(17) 0.0119(16) -0.0034(13) 0.0029(13) 0.0042(14) C32 0.0129(17) 0.0218(19) 0.0135(17) -0.0022(14) 0.0033(13) 0.0075(14) C33 0.0094(16) 0.0231(19) 0.0209(19) -0.0068(15) 0.0004(14) 0.0074(14) C34 0.0087(16) 0.0198(19) 0.0237(19) -0.0079(15) 0.0019(14) 0.0068(14) C35 0.0112(16) 0.0166(17) 0.0140(17) -0.0053(13) -0.0003(13) 0.0058(13) C36 0.0106(16) 0.0094(15) 0.0150(16) -0.0020(13) 0.0019(13) 0.0039(12) C37 0.0138(17) 0.0106(16) 0.0149(17) -0.0033(13) 0.0002(13) 0.0046(13) C38 0.0108(17) 0.0171(18) 0.0205(19) -0.0017(14) 0.0021(14) 0.0050(14) C39 0.0098(16) 0.0181(18) 0.0147(17) -0.0015(14) 0.0030(13) 0.0062(13) C40 0.0140(17) 0.0173(17) 0.0120(16) -0.0015(13) 0.0021(13) 0.0045(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 O2 1.892(2) . ? Cu1 N2 1.919(3) . ? Cu1 N1 2.017(3) . ? Cu1 N3 2.026(3) . ? Cu1 O1 2.339(2) . ? Cu2 O18 1.900(2) . ? Cu2 N5 1.938(3) . ? Cu2 N4 2.014(3) . ? Cu2 N6 2.017(3) . ? Cu2 O13 2.347(2) . ? V1 O5 1.588(3) . ? V1 F1 1.915(2) . ? V1 O6 1.959(2) . ? V1 O8 1.994(2) . ? V1 O3 1.996(2) . ? V2 O1 1.615(2) . ? V2 F2 1.862(2) . ? V2 O7 1.949(3) . ? V2 O4 1.961(2) . ? V2 O6 1.986(2) . ? V3 O13 1.612(2) . ? V3 O11 1.919(2) . ? V3 F3 1.952(2) . ? V3 O14 1.957(2) . ? V3 O9 2.002(2) . ? V4 O16 1.593(3) . ? V4 F4 1.883(2) . ? V4 O15 1.952(2) . ? V4 O12 1.952(3) . ? V4 O17 2.036(3) . ? P1 O2 1.532(2) . ? P1 O4 1.533(3) . ? P1 O3 1.542(3) . ? P1 C35 1.792(4) . ? P2 O8 1.526(3) . ? P2 O9 1.538(2) . ? P2 O10 1.547(3) . ? P2 C40 1.794(4) . ? P3 O7 1.524(3) . ? P3 O11 1.526(2) . ? P3 O12 1.527(3) . ? P3 C31 1.788(4) . ? P4 O15 1.522(2) . ? P4 O14 1.539(2) . ? P4 O18 1.540(2) . ? P4 C36 1.788(3) . ? N1 C1 1.338(4) . ? N1 C5 1.364(4) . ? N2 C6 1.336(4) . ? N2 C10 1.339(4) . ? N3 C15 1.339(4) . ? N3 C11 1.367(4) . ? N4 C16 1.338(4) . ? N4 C20 1.358(4) . ? N5 C25 1.333(4) . ? N5 C21 1.338(4) . ? N6 C30 1.336(4) . ? N6 C26 1.368(4) . ? C1 C2 1.388(5) . ? C2 C3 1.388(5) . ? C3 C4 1.388(5) . ? C4 C5 1.373(5) . ? C5 C6 1.483(5) . ? C6 C7 1.383(4) . ? C7 C8 1.400(5) . ? C8 C9 1.402(5) . ? C8 C8 1.497(7) 2_666 ? C9 C10 1.387(4) . ? C10 C11 1.489(5) . ? C11 C12 1.377(5) . ? C12 C13 1.398(5) . ? C13 C14 1.387(5) . ? C14 C15 1.385(5) . ? C16 C17 1.395(5) . ? C17 C18 1.388(5) . ? C18 C19 1.394(5) . ? C19 C20 1.380(5) . ? C20 C21 1.485(5) . ? C21 C22 1.385(4) . ? C22 C23 1.414(5) . ? C23 C24 1.409(5) . ? C23 C23 1.486(6) 2_745 ? C24 C25 1.393(4) . ? C25 C26 1.487(5) . ? C26 C27 1.372(5) . ? C27 C28 1.390(5) . ? C28 C29 1.386(5) . ? C29 C30 1.388(5) . ? C31 C32 1.532(5) . ? C32 C33 1.528(5) . ? C33 C34 1.530(5) . ? C34 C35 1.540(5) 1_455 ? C35 C34 1.540(5) 1_655 ? C36 C37 1.538(5) . ? C37 C38 1.517(5) . ? C38 C39 1.532(5) . ? C39 C40 1.534(5) 1_455 ? C40 C39 1.534(5) 1_655 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Cu1 N2 168.64(11) . . ? O2 Cu1 N1 99.58(11) . . ? N2 Cu1 N1 80.52(12) . . ? O2 Cu1 N3 98.62(11) . . ? N2 Cu1 N3 80.07(12) . . ? N1 Cu1 N3 160.15(12) . . ? O2 Cu1 O1 99.23(9) . . ? N2 Cu1 O1 92.13(10) . . ? N1 Cu1 O1 89.60(11) . . ? N3 Cu1 O1 95.24(11) . . ? O18 Cu2 N5 168.35(11) . . ? O18 Cu2 N4 99.89(11) . . ? N5 Cu2 N4 79.96(11) . . ? O18 Cu2 N6 98.75(11) . . ? N5 Cu2 N6 79.97(11) . . ? N4 Cu2 N6 159.32(11) . . ? O18 Cu2 O13 96.86(9) . . ? N5 Cu2 O13 94.78(10) . . ? N4 Cu2 O13 92.47(10) . . ? N6 Cu2 O13 94.13(10) . . ? O5 V1 F1 111.76(12) . . ? O5 V1 O6 110.74(13) . . ? F1 V1 O6 137.37(11) . . ? O5 V1 O8 102.81(12) . . ? F1 V1 O8 80.31(10) . . ? O6 V1 O8 87.42(10) . . ? O5 V1 O3 102.41(12) . . ? F1 V1 O3 85.35(10) . . ? O6 V1 O3 88.78(10) . . ? O8 V1 O3 154.18(11) . . ? O1 V2 F2 107.56(11) . . ? O1 V2 O7 108.51(12) . . ? F2 V2 O7 87.54(10) . . ? O1 V2 O4 102.53(11) . . ? F2 V2 O4 86.66(10) . . ? O7 V2 O4 148.74(10) . . ? O1 V2 O6 105.37(12) . . ? F2 V2 O6 147.06(11) . . ? O7 V2 O6 81.70(10) . . ? O4 V2 O6 86.69(10) . . ? O13 V3 O11 116.30(12) . . ? O13 V3 F3 110.89(11) . . ? O11 V3 F3 132.81(10) . . ? O13 V3 O14 99.31(11) . . ? O11 V3 O14 87.66(10) . . ? F3 V3 O14 84.85(10) . . ? O13 V3 O9 102.26(11) . . ? O11 V3 O9 84.56(10) . . ? F3 V3 O9 85.70(10) . . ? O14 V3 O9 158.34(10) . . ? O16 V4 F4 108.09(12) . . ? O16 V4 O15 108.86(12) . . ? F4 V4 O15 142.61(10) . . ? O16 V4 O12 107.07(13) . . ? F4 V4 O12 84.56(10) . . ? O15 V4 O12 90.02(10) . . ? O16 V4 O17 106.29(14) . . ? F4 V4 O17 81.04(11) . . ? O15 V4 O17 83.44(11) . . ? O12 V4 O17 146.34(11) . . ? O2 P1 O4 112.15(14) . . ? O2 P1 O3 110.01(14) . . ? O4 P1 O3 111.55(14) . . ? O2 P1 C35 106.16(15) . . ? O4 P1 C35 107.63(16) . . ? O3 P1 C35 109.13(16) . . ? O8 P2 O9 110.71(14) . . ? O8 P2 O10 109.44(14) . . ? O9 P2 O10 110.45(14) . . ? O8 P2 C40 109.61(16) . . ? O9 P2 C40 107.56(15) . . ? O10 P2 C40 109.03(16) . . ? O7 P3 O11 111.85(14) . . ? O7 P3 O12 108.70(14) . . ? O11 P3 O12 112.53(14) . . ? O7 P3 C31 109.45(16) . . ? O11 P3 C31 105.82(15) . . ? O12 P3 C31 108.37(16) . . ? O15 P4 O14 112.86(14) . . ? O15 P4 O18 109.85(14) . . ? O14 P4 O18 110.43(13) . . ? O15 P4 C36 108.55(15) . . ? O14 P4 C36 106.51(15) . . ? O18 P4 C36 108.48(15) . . ? V2 O1 Cu1 123.93(13) . . ? P1 O2 Cu1 126.19(15) . . ? P1 O3 V1 129.93(15) . . ? P1 O4 V2 124.69(14) . . ? V1 O6 V2 137.88(14) . . ? P3 O7 V2 148.88(16) . . ? P2 O8 V1 138.62(15) . . ? P2 O9 V3 128.34(15) . . ? P3 O11 V3 144.53(16) . . ? P3 O12 V4 134.45(16) . . ? V3 O13 Cu2 125.54(13) . . ? P4 O14 V3 122.17(14) . . ? P4 O15 V4 156.50(16) . . ? P4 O18 Cu2 123.23(14) . . ? C1 N1 C5 117.8(3) . . ? C1 N1 Cu1 127.8(2) . . ? C5 N1 Cu1 114.2(2) . . ? C6 N2 C10 121.7(3) . . ? C6 N2 Cu1 118.9(2) . . ? C10 N2 Cu1 119.5(2) . . ? C15 N3 C11 118.1(3) . . ? C15 N3 Cu1 127.2(2) . . ? C11 N3 Cu1 114.6(2) . . ? C16 N4 C20 119.3(3) . . ? C16 N4 Cu2 125.9(2) . . ? C20 N4 Cu2 114.8(2) . . ? C25 N5 C21 121.5(3) . . ? C25 N5 Cu2 119.3(2) . . ? C21 N5 Cu2 119.2(2) . . ? C30 N6 C26 118.3(3) . . ? C30 N6 Cu2 127.0(2) . . ? C26 N6 Cu2 114.2(2) . . ? N1 C1 C2 122.8(3) . . ? C3 C2 C1 118.6(3) . . ? C2 C3 C4 119.2(4) . . ? C5 C4 C3 118.8(4) . . ? N1 C5 C4 122.7(3) . . ? N1 C5 C6 113.3(3) . . ? C4 C5 C6 124.0(3) . . ? N2 C6 C7 120.7(3) . . ? N2 C6 C5 113.0(3) . . ? C7 C6 C5 126.3(3) . . ? C6 C7 C8 119.2(3) . . ? C7 C8 C9 118.9(3) . . ? C7 C8 C8 120.4(4) . 2_666 ? C9 C8 C8 120.8(4) . 2_666 ? C10 C9 C8 118.8(3) . . ? N2 C10 C9 120.8(3) . . ? N2 C10 C11 112.9(3) . . ? C9 C10 C11 126.3(3) . . ? N3 C11 C12 122.4(3) . . ? N3 C11 C10 112.8(3) . . ? C12 C11 C10 124.8(3) . . ? C11 C12 C13 118.7(3) . . ? C14 C13 C12 119.0(3) . . ? C15 C14 C13 119.0(3) . . ? N3 C15 C14 122.7(3) . . ? N4 C16 C17 121.8(3) . . ? C18 C17 C16 119.1(3) . . ? C17 C18 C19 118.9(3) . . ? C20 C19 C18 119.1(3) . . ? N4 C20 C19 121.8(3) . . ? N4 C20 C21 113.8(3) . . ? C19 C20 C21 124.3(3) . . ? N5 C21 C22 121.1(3) . . ? N5 C21 C20 112.2(3) . . ? C22 C21 C20 126.7(3) . . ? C21 C22 C23 119.1(3) . . ? C24 C23 C22 118.3(3) . . ? C24 C23 C23 120.8(4) . 2_745 ? C22 C23 C23 120.9(4) . 2_745 ? C25 C24 C23 118.7(3) . . ? N5 C25 C24 121.3(3) . . ? N5 C25 C26 112.4(3) . . ? C24 C25 C26 126.2(3) . . ? N6 C26 C27 122.1(3) . . ? N6 C26 C25 113.5(3) . . ? C27 C26 C25 124.4(3) . . ? C26 C27 C28 118.9(3) . . ? C29 C28 C27 119.3(3) . . ? C28 C29 C30 118.7(3) . . ? N6 C30 C29 122.5(3) . . ? C32 C31 P3 113.9(3) . . ? C33 C32 C31 113.3(3) . . ? C32 C33 C34 112.7(3) . . ? C33 C34 C35 111.2(3) . 1_455 ? C34 C35 P1 114.1(3) 1_655 . ? C37 C36 P4 112.9(2) . . ? C38 C37 C36 111.4(3) . . ? C37 C38 C39 113.9(3) . . ? C38 C39 C40 112.2(3) . 1_455 ? C39 C40 P2 114.4(2) 1_655 . ? _diffrn_measured_fraction_theta_max 0.974 _diffrn_reflns_theta_full 31.51 _diffrn_measured_fraction_theta_full 0.974 _refine_diff_density_max 1.179 _refine_diff_density_min -0.951 _refine_diff_density_rms 0.153 data_publication_text_compound_10 _database_code_depnum_ccdc_archive 'CCDC 247639' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ; [{Cu4(bisterpy)2(H2O)2}V8F4O12{O3P(CH2)5PO3}5]·4.8·H2O ; _chemical_formula_sum 'C42.50 H55.80 Cu2 F2 N6 O24.40 P5 V4' _chemical_formula_weight 1564.82 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 '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' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.7766(9) _cell_length_b 14.1439(11) _cell_length_c 20.1563(16) _cell_angle_alpha 73.173(2) _cell_angle_beta 88.644(2) _cell_angle_gamma 73.019(2) _cell_volume 2806.3(4) _cell_formula_units_Z 2 _cell_measurement_temperature 90(2) _cell_measurement_reflns_used 18310 _cell_measurement_theta_min 1.98 _cell_measurement_theta_max 31.51 _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.852 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1582 _exptl_absorpt_coefficient_mu 1.621 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7590 _exptl_absorpt_correction_T_max 0.8547 _exptl_absorpt_process_details 'SADABS SHELXL-97 (SHELDRICK, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 90(2) _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_probe x-ray _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'APEX CCD area detector' _diffrn_measurement_method 'Phi and omega scans' _diffrn_detector_area_resol_mean 512 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.001 _diffrn_reflns_number 36815 _diffrn_reflns_av_R_equivalents 0.0389 _diffrn_reflns_av_sigmaI/netI 0.0677 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.98 _diffrn_reflns_theta_max 31.51 _reflns_number_total 18310 _reflns_number_gt 13325 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0654P)^2^+3.2366P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 18310 _refine_ls_number_parameters 839 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0816 _refine_ls_R_factor_gt 0.0549 _refine_ls_wR_factor_ref 0.1411 _refine_ls_wR_factor_gt 0.1275 _refine_ls_goodness_of_fit_ref 1.010 _refine_ls_restrained_S_all 1.010 _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 0.56142(4) 0.39395(3) 0.076785(19) 0.01492(8) Uani 1 1 d . . . Cu2 Cu 0.42960(3) 0.12262(3) 0.426909(19) 0.01145(8) Uani 1 1 d . . . V1 V 0.62783(5) 0.16445(4) 0.21177(3) 0.01230(10) Uani 1 1 d . . . V3 V 1.11612(5) 0.76444(4) 0.30569(3) 0.01768(11) Uani 1 1 d . . . V4 V 0.86357(5) 0.77271(4) 0.18864(3) 0.01528(11) Uani 1 1 d . . . V2A V 0.4299(2) 0.06336(15) 0.11086(12) 0.0154(4) Uani 0.486(5) 1 d P . 1 P5A P 0.7032(4) 0.9166(4) 0.0394(3) 0.0247(8) Uani 0.486(5) 1 d P . 1 O6A O 0.3327(5) 0.0131(4) 0.1575(3) 0.0260(13) Uani 0.486(5) 1 d P . 1 O20A O 0.5618(5) -0.0604(4) 0.1007(2) 0.0207(12) Uani 0.486(5) 1 d P . 1 C41A C 0.8323(8) 0.9412(9) -0.0096(5) 0.035(2) Uani 0.486(5) 1 d P . 1 H41A H 0.8732 0.8816 -0.0255 0.042 Uiso 0.486(5) 1 calc PR . 1 H41B H 0.7968 0.9994 -0.0504 0.042 Uiso 0.486(5) 1 calc PR . 1 C42A C 0.9356(12) 0.9641(10) 0.0259(6) 0.056(3) Uani 0.486(5) 1 d P . 1 H42A H 0.9621 0.9107 0.0701 0.067 Uiso 0.486(5) 1 calc PR . 1 H42B H 0.8967 1.0291 0.0361 0.067 Uiso 0.486(5) 1 calc PR . 1 V2B V 0.4658(2) 0.07369(13) 0.09575(10) 0.0121(3) Uani 0.514(5) 1 d P . 2 P5B P 0.6711(4) 0.9123(3) 0.0523(2) 0.0189(6) Uani 0.514(5) 1 d P . 2 O6B O 0.4006(5) -0.0129(4) 0.1364(3) 0.0224(11) Uani 0.514(5) 1 d P . 2 O20B O 0.6294(4) 0.0110(4) 0.0601(2) 0.0201(11) Uani 0.514(5) 1 d P . 2 C41B C 0.7280(9) 1.0218(6) 0.0191(4) 0.038(2) Uani 0.514(5) 1 d P . 2 H41C H 0.6580 1.0776 -0.0100 0.045 Uiso 0.514(5) 1 calc PR . 2 H41D H 0.7475 1.0439 0.0579 0.045 Uiso 0.514(5) 1 calc PR . 2 C42B C 0.8440(8) 1.0065(7) -0.0216(4) 0.0317(18) Uani 0.514(5) 1 d P . 2 H42C H 0.8735 0.9358 -0.0238 0.038 Uiso 0.514(5) 1 calc PR . 2 H42D H 0.8237 1.0528 -0.0686 0.038 Uiso 0.514(5) 1 calc PR . 2 P1 P 0.35390(7) 0.28905(6) 0.13805(4) 0.01163(14) Uani 1 1 d . . . P2 P 0.68791(7) 0.17149(6) 0.37042(4) 0.01264(14) Uani 1 1 d . . . P3 P 1.18492(8) 0.51867(6) 0.32435(4) 0.01600(16) Uani 1 1 d . . . P4 P 0.89144(7) 0.96921(6) 0.23292(4) 0.01192(14) Uani 1 1 d . . . F1 F 1.12870(19) 0.76585(15) 0.39910(10) 0.0219(4) Uani 1 1 d . . . F2 F 0.96009(18) 0.65278(15) 0.16204(10) 0.0193(4) Uani 1 1 d . . . O1 O 0.3907(2) 0.38311(17) 0.09320(11) 0.0154(4) Uani 1 1 d . . . O2 O 0.6862(2) 0.24013(18) 0.15307(12) 0.0212(5) Uani 1 1 d . . . O3 O 0.4428(2) 0.23772(17) 0.20588(11) 0.0132(4) Uani 1 1 d . . . O4 O 0.5812(2) 0.07168(19) 0.16918(12) 0.0225(5) Uani 1 1 d . . . O5 O 0.3584(2) 0.21223(17) 0.09806(11) 0.0152(4) Uani 1 1 d . . . O7 O 0.6259(2) 0.20572(17) 0.29743(11) 0.0144(4) Uani 1 1 d . . . O8 O 0.6022(2) 0.13565(18) 0.42677(11) 0.0163(4) Uani 1 1 d . . . O9 O 0.8180(2) 0.08115(18) 0.37491(12) 0.0183(5) Uani 1 1 d . . . O10 O 1.3065(2) 0.43393(17) 0.35328(12) 0.0180(4) Uani 1 1 d . . . O11 O 1.1746(2) 0.53836(17) 0.24290(12) 0.0175(4) Uani 1 1 d . . . O12 O 1.1843(3) 0.61762(19) 0.34201(14) 0.0297(6) Uani 1 1 d . . . O13 O 1.2326(3) 0.8019(2) 0.26720(15) 0.0359(7) Uani 1 1 d . . . O14 O 0.9748(2) 0.89249(17) 0.29705(11) 0.0164(4) Uani 1 1 d . . . O15 O 1.0337(3) 0.75071(19) 0.23082(15) 0.0321(7) Uani 1 1 d . . . O16 O 0.7771(3) 0.7298(2) 0.24664(16) 0.0399(8) Uani 1 1 d . . . O17 O 0.8338(2) 0.91865(17) 0.18881(11) 0.0154(4) Uani 1 1 d . . . O18 O 0.7804(2) 1.04500(16) 0.25847(11) 0.0144(4) Uani 1 1 d . . . O19 O 0.7735(3) 0.8217(2) 0.09860(15) 0.0340(7) Uani 1 1 d . . . O21 O 0.6202(3) 0.8840(2) -0.00549(14) 0.0339(7) Uani 1 1 d . . . O90 O 0.3445(2) 0.24890(17) 0.33464(11) 0.0147(4) Uani 1 1 d . . . O91 O 0.3574(3) 0.6367(2) 0.47078(14) 0.0275(6) Uani 1 1 d . . . O92 O 0.8595(8) 0.7053(6) 0.0035(4) 0.043(2) Uani 0.40 1 d P . . O93 O 0.4994(2) 0.49464(19) 0.40792(13) 0.0228(5) Uani 1 1 d . . . N1 N 0.5729(3) 0.4707(2) 0.14587(14) 0.0213(6) Uani 1 1 d . . . N2 N 0.7172(3) 0.4317(2) 0.04952(14) 0.0212(6) Uani 1 1 d . . . N3 N 0.5999(3) 0.3395(2) -0.00696(14) 0.0180(5) Uani 1 1 d . . . N4 N 0.4623(2) 0.0019(2) 0.38674(14) 0.0147(5) Uani 1 1 d . . . N5 N 0.2715(2) 0.08419(19) 0.44939(13) 0.0122(5) Uani 1 1 d . . . N6 N 0.3517(2) 0.2115(2) 0.48991(13) 0.0143(5) Uani 1 1 d . . . C1 C 0.4916(3) 0.4863(3) 0.19540(17) 0.0239(7) Uani 1 1 d . . . H1 H 0.4191 0.4626 0.1988 0.029 Uiso 1 1 calc R . . C2 C 0.5117(4) 0.5368(4) 0.24188(19) 0.0329(9) Uani 1 1 d . . . H2 H 0.4535 0.5470 0.2758 0.039 Uiso 1 1 calc R . . C3 C 0.6198(5) 0.5717(4) 0.2369(2) 0.0420(12) Uani 1 1 d . . . H3 H 0.6354 0.6055 0.2677 0.050 Uiso 1 1 calc R . . C4 C 0.7049(4) 0.5558(4) 0.1856(2) 0.0410(12) Uani 1 1 d . . . H4 H 0.7779 0.5790 0.1813 0.049 Uiso 1 1 calc R . . C5 C 0.6792(4) 0.5051(4) 0.14130(18) 0.0302(9) Uani 1 1 d . . . C6 C 0.7611(4) 0.4833(4) 0.08424(18) 0.0315(9) Uani 1 1 d . . . C7 C 0.8734(4) 0.5116(5) 0.0657(2) 0.0467(14) Uani 1 1 d . . . H7 H 0.9034 0.5486 0.0897 0.056 Uiso 1 1 calc R . . C8 C 0.9406(4) 0.4838(4) 0.01067(18) 0.0369(11) Uani 1 1 d . . . C9 C 0.8936(3) 0.4280(3) -0.02336(18) 0.0291(9) Uani 1 1 d . . . H9 H 0.9375 0.4071 -0.0593 0.035 Uiso 1 1 calc R . . C10 C 0.7798(3) 0.4038(3) -0.00306(17) 0.0224(7) Uani 1 1 d . . . C11 C 0.7141(3) 0.3475(3) -0.03501(18) 0.0221(7) Uani 1 1 d . . . C12 C 0.7605(4) 0.3070(3) -0.0881(2) 0.0329(9) Uani 1 1 d . . . H12 H 0.8391 0.3126 -0.1063 0.039 Uiso 1 1 calc R . . C13 C 0.6883(5) 0.2577(4) -0.1142(3) 0.0467(13) Uani 1 1 d . . . H13 H 0.7178 0.2304 -0.1504 0.056 Uiso 1 1 calc R . . C14 C 0.5730(5) 0.2492(4) -0.0863(2) 0.0454(13) Uani 1 1 d . . . H14 H 0.5239 0.2159 -0.1032 0.054 Uiso 1 1 calc R . . C15 C 0.5311(4) 0.2914(3) -0.0325(2) 0.0278(8) Uani 1 1 d . . . H15 H 0.4529 0.2860 -0.0137 0.033 Uiso 1 1 calc R . . C16 C 0.5659(3) -0.0361(2) 0.35344(17) 0.0182(6) Uani 1 1 d . . . H16 H 0.6385 -0.0134 0.3542 0.022 Uiso 1 1 calc R . . C17 C 0.5696(3) -0.1070(3) 0.31830(19) 0.0235(7) Uani 1 1 d . . . H17 H 0.6424 -0.1308 0.2952 0.028 Uiso 1 1 calc R . . C18 C 0.4628(4) -0.1420(3) 0.3180(2) 0.0304(9) Uani 1 1 d . . . H18 H 0.4620 -0.1887 0.2939 0.036 Uiso 1 1 calc R . . C19 C 0.3564(3) -0.1067(3) 0.35426(19) 0.0247(7) Uani 1 1 d . . . H19 H 0.2848 -0.1312 0.3560 0.030 Uiso 1 1 calc R . . C20 C 0.3592(3) -0.0345(2) 0.38756(16) 0.0157(6) Uani 1 1 d . . . C21 C 0.2521(3) 0.0092(2) 0.42737(15) 0.0132(5) Uani 1 1 d . . . C22 C 0.1434(3) -0.0242(2) 0.44492(16) 0.0142(5) Uani 1 1 d . . . H22 H 0.1291 -0.0755 0.4286 0.017 Uiso 1 1 calc R . . C23 C 0.0557(3) 0.0204(2) 0.48750(15) 0.0123(5) Uani 1 1 d . . . C24 C 0.0767(3) 0.1014(2) 0.50779(15) 0.0137(5) Uani 1 1 d . . . H24 H 0.0176 0.1349 0.5341 0.016 Uiso 1 1 calc R . . C25 C 0.1872(3) 0.1308(2) 0.48805(15) 0.0120(5) Uani 1 1 d . . . C26 C 0.2304(3) 0.2092(2) 0.50870(16) 0.0147(6) Uani 1 1 d . . . C27 C 0.1578(3) 0.2738(3) 0.54451(18) 0.0209(7) Uani 1 1 d . . . H27 H 0.0745 0.2720 0.5566 0.025 Uiso 1 1 calc R . . C28 C 0.2125(4) 0.3417(3) 0.5621(2) 0.0285(8) Uani 1 1 d . . . H28 H 0.1658 0.3856 0.5865 0.034 Uiso 1 1 calc R . . C29 C 0.3354(4) 0.3442(3) 0.5435(2) 0.0254(7) Uani 1 1 d . . . H29 H 0.3724 0.3895 0.5550 0.030 Uiso 1 1 calc R . . C30 C 0.4031(3) 0.2773(3) 0.50703(16) 0.0176(6) Uani 1 1 d . . . H30 H 0.4863 0.2784 0.4943 0.021 Uiso 1 1 calc R . . C31 C 0.1926(3) 0.3332(2) 0.16386(16) 0.0146(6) Uani 1 1 d . . . H31A H 0.1908 0.3825 0.1890 0.018 Uiso 1 1 calc R . . H31B H 0.1346 0.3695 0.1224 0.018 Uiso 1 1 calc R . . C32 C 0.1400(3) 0.2473(3) 0.20967(17) 0.0195(6) Uani 1 1 d . . . H32A H 0.2093 0.1984 0.2431 0.023 Uiso 1 1 calc R . . H32B H 0.0709 0.2782 0.2355 0.023 Uiso 1 1 calc R . . C33 C 0.0883(4) 0.1885(3) 0.17064(19) 0.0256(8) Uani 1 1 d . . . H33A H 0.1577 0.1548 0.1461 0.031 Uiso 1 1 calc R . . H33B H 0.0201 0.2369 0.1364 0.031 Uiso 1 1 calc R . . C34 C 0.0344(3) 0.1076(3) 0.21882(18) 0.0206(6) Uani 1 1 d . . . H34A H -0.0362 0.1418 0.2425 0.025 Uiso 1 1 calc R . . H34B H 0.1021 0.0606 0.2538 0.025 Uiso 1 1 calc R . . C35 C 0.7368(3) 0.2713(3) 0.38869(16) 0.0168(6) Uani 1 1 d . . . H35A H 0.6627 0.3331 0.3786 0.020 Uiso 1 1 calc R . . H35B H 0.7610 0.2506 0.4380 0.020 Uiso 1 1 calc R . . C36 C 0.8501(3) 0.2987(3) 0.34870(18) 0.0221(7) Uani 1 1 d . . . H36A H 0.9235 0.2367 0.3565 0.027 Uiso 1 1 calc R . . H36B H 0.8247 0.3245 0.2994 0.027 Uiso 1 1 calc R . . C37 C 0.8906(4) 0.3792(3) 0.37069(19) 0.0252(7) Uani 1 1 d . . . H37A H 0.9084 0.3554 0.4207 0.030 Uiso 1 1 calc R . . H37B H 0.8187 0.4426 0.3596 0.030 Uiso 1 1 calc R . . C38 C 1.0108(4) 0.4033(3) 0.3363(2) 0.0263(7) Uani 1 1 d . . . H38A H 1.0850 0.3417 0.3506 0.032 Uiso 1 1 calc R . . H38B H 0.9961 0.4220 0.2863 0.032 Uiso 1 1 calc R . . C39 C 1.0409(3) 0.4903(3) 0.35534(19) 0.0238(7) Uani 1 1 d . . . H39A H 1.0466 0.4734 0.4056 0.029 Uiso 1 1 calc R . . H39B H 0.9683 0.5524 0.3379 0.029 Uiso 1 1 calc R . . C40 C 0.9846(3) 1.0451(3) 0.18090(16) 0.0164(6) Uani 1 1 d . . . H40A H 1.0583 0.9997 0.1658 0.020 Uiso 1 1 calc R . . H40B H 0.9313 1.0924 0.1398 0.020 Uiso 1 1 calc R . . C43 C 0.9425(10) 1.0282(9) 0.0123(5) 0.048(2) Uani 0.50 1 d P . . H43A H 0.9417 1.0032 0.0624 0.057 Uiso 0.50 1 calc PR . 2 H43B H 0.9332 1.1017 -0.0015 0.057 Uiso 0.50 1 calc PR . 2 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 0.00958(16) 0.02014(19) 0.01331(17) 0.00123(14) 0.00187(13) -0.00802(14) Cu2 0.00988(16) 0.01241(17) 0.01315(17) -0.00325(13) 0.00370(12) -0.00571(13) V1 0.0113(2) 0.0133(2) 0.0101(2) -0.00091(18) 0.00156(17) -0.00307(18) V3 0.0161(3) 0.0158(3) 0.0198(3) -0.0070(2) -0.0010(2) -0.0007(2) V4 0.0171(3) 0.0141(2) 0.0159(2) -0.00431(19) 0.00103(19) -0.00666(19) V2A 0.0113(8) 0.0202(7) 0.0170(9) -0.0098(6) -0.0003(6) -0.0037(6) P5A 0.0103(16) 0.0432(17) 0.0229(19) -0.0197(15) -0.0027(10) -0.0015(12) O6A 0.017(3) 0.025(3) 0.037(3) -0.011(2) 0.006(2) -0.008(2) O20A 0.017(2) 0.025(3) 0.021(2) -0.013(2) -0.0022(18) -0.0001(19) C41A 0.021(4) 0.050(6) 0.030(4) -0.015(4) 0.000(3) -0.004(4) C42A 0.081(9) 0.054(7) 0.044(6) -0.001(5) -0.013(5) -0.050(7) V2B 0.0102(7) 0.0168(6) 0.0114(7) -0.0050(5) 0.0004(5) -0.0063(5) P5B 0.0175(17) 0.0185(10) 0.0191(16) -0.0073(10) -0.0072(11) -0.0005(12) O6B 0.024(3) 0.022(2) 0.027(3) -0.008(2) 0.002(2) -0.014(2) O20B 0.020(2) 0.025(2) 0.017(2) -0.0092(19) -0.0009(17) -0.0062(19) C41B 0.048(5) 0.030(4) 0.026(4) -0.002(3) 0.014(4) -0.005(4) C42B 0.028(4) 0.034(4) 0.020(4) -0.004(3) 0.002(3) 0.007(3) P1 0.0092(3) 0.0151(3) 0.0118(3) -0.0036(3) 0.0021(3) -0.0058(3) P2 0.0098(3) 0.0170(4) 0.0119(3) -0.0034(3) 0.0010(3) -0.0060(3) P3 0.0161(4) 0.0133(4) 0.0169(4) -0.0052(3) -0.0005(3) -0.0011(3) P4 0.0111(3) 0.0111(3) 0.0128(3) -0.0023(3) 0.0006(3) -0.0033(3) F1 0.0218(10) 0.0214(10) 0.0171(9) -0.0060(8) 0.0016(7) 0.0020(8) F2 0.0167(9) 0.0214(10) 0.0224(10) -0.0094(8) 0.0001(7) -0.0067(7) O1 0.0110(10) 0.0177(11) 0.0165(10) 0.0001(8) 0.0013(8) -0.0080(8) O2 0.0135(10) 0.0234(12) 0.0157(11) 0.0074(9) 0.0035(8) -0.0022(9) O3 0.0098(9) 0.0185(10) 0.0122(10) -0.0047(8) 0.0001(7) -0.0053(8) O4 0.0231(12) 0.0219(12) 0.0201(12) -0.0108(10) -0.0060(9) 0.0020(10) O5 0.0146(10) 0.0212(11) 0.0119(10) -0.0062(8) 0.0002(8) -0.0068(9) O7 0.0114(10) 0.0165(10) 0.0142(10) -0.0035(8) -0.0020(8) -0.0033(8) O8 0.0137(10) 0.0226(11) 0.0142(10) -0.0035(9) 0.0034(8) -0.0099(9) O9 0.0122(10) 0.0211(11) 0.0182(11) -0.0051(9) -0.0003(8) -0.0006(9) O10 0.0130(10) 0.0157(11) 0.0229(12) -0.0043(9) -0.0021(9) -0.0021(8) O11 0.0178(11) 0.0177(11) 0.0171(11) -0.0072(9) 0.0022(9) -0.0034(9) O12 0.0404(16) 0.0157(12) 0.0299(14) -0.0071(10) -0.0074(12) -0.0029(11) O13 0.0371(16) 0.0440(17) 0.0337(16) -0.0189(14) 0.0176(13) -0.0164(14) O14 0.0160(10) 0.0148(10) 0.0169(11) -0.0048(8) -0.0046(8) -0.0020(8) O15 0.0295(14) 0.0189(12) 0.0457(16) -0.0203(12) -0.0250(12) 0.0091(10) O16 0.0545(19) 0.0254(14) 0.0467(18) -0.0162(13) 0.0354(15) -0.0193(13) O17 0.0136(10) 0.0139(10) 0.0184(11) -0.0044(8) -0.0015(8) -0.0040(8) O18 0.0138(10) 0.0138(10) 0.0135(10) -0.0021(8) 0.0014(8) -0.0027(8) O19 0.0388(16) 0.0250(14) 0.0356(15) -0.0128(12) -0.0205(12) -0.0001(12) O21 0.0238(13) 0.0472(18) 0.0309(14) -0.0257(13) -0.0116(11) 0.0043(12) O90 0.0143(10) 0.0150(10) 0.0132(10) -0.0028(8) 0.0020(8) -0.0032(8) O91 0.0250(13) 0.0299(14) 0.0273(13) -0.0119(11) -0.0064(10) -0.0037(11) O92 0.047(5) 0.038(4) 0.035(4) -0.021(3) -0.015(3) 0.012(4) O93 0.0233(12) 0.0240(12) 0.0223(12) -0.0081(10) -0.0015(10) -0.0071(10) N1 0.0170(13) 0.0358(17) 0.0141(12) -0.0019(12) 0.0011(10) -0.0178(12) N2 0.0121(12) 0.0345(16) 0.0139(12) 0.0035(11) 0.0009(10) -0.0129(12) N3 0.0165(13) 0.0199(13) 0.0180(13) -0.0026(11) 0.0069(10) -0.0095(10) N4 0.0128(12) 0.0148(12) 0.0173(12) -0.0045(10) 0.0058(9) -0.0059(9) N5 0.0119(11) 0.0118(11) 0.0138(11) -0.0025(9) 0.0042(9) -0.0065(9) N6 0.0144(12) 0.0169(12) 0.0129(12) -0.0033(10) 0.0025(9) -0.0077(10) C1 0.0229(17) 0.038(2) 0.0187(16) -0.0065(14) 0.0062(13) -0.0234(15) C2 0.032(2) 0.062(3) 0.0201(17) -0.0153(18) 0.0107(15) -0.034(2) C3 0.046(3) 0.078(3) 0.026(2) -0.021(2) 0.0097(18) -0.049(3) C4 0.042(2) 0.084(4) 0.0199(18) -0.017(2) 0.0116(17) -0.052(3) C5 0.0261(18) 0.060(3) 0.0146(15) -0.0056(16) 0.0048(13) -0.0325(19) C6 0.0216(17) 0.067(3) 0.0121(15) -0.0051(16) 0.0015(13) -0.0282(19) C7 0.036(2) 0.108(4) 0.0163(17) -0.017(2) 0.0074(16) -0.054(3) C8 0.0203(18) 0.085(3) 0.0101(15) -0.0017(18) 0.0028(13) -0.035(2) C9 0.0137(15) 0.053(2) 0.0149(15) 0.0045(15) 0.0014(12) -0.0153(16) C10 0.0132(14) 0.0325(18) 0.0130(14) 0.0074(13) 0.0007(11) -0.0082(13) C11 0.0161(15) 0.0241(17) 0.0203(16) 0.0014(13) 0.0067(12) -0.0057(13) C12 0.031(2) 0.034(2) 0.033(2) -0.0061(17) 0.0205(17) -0.0139(17) C13 0.061(3) 0.051(3) 0.052(3) -0.035(2) 0.043(3) -0.034(2) C14 0.061(3) 0.056(3) 0.049(3) -0.033(2) 0.038(2) -0.046(3) C15 0.035(2) 0.0292(19) 0.0295(19) -0.0124(16) 0.0170(16) -0.0221(16) C16 0.0160(14) 0.0153(14) 0.0240(16) -0.0053(12) 0.0083(12) -0.0070(11) C17 0.0229(17) 0.0241(17) 0.0266(18) -0.0119(14) 0.0141(14) -0.0084(13) C18 0.0285(19) 0.036(2) 0.041(2) -0.0266(18) 0.0195(17) -0.0176(16) C19 0.0218(17) 0.0323(19) 0.0324(19) -0.0191(16) 0.0155(14) -0.0182(15) C20 0.0151(14) 0.0172(14) 0.0180(14) -0.0075(12) 0.0066(11) -0.0075(11) C21 0.0124(13) 0.0166(14) 0.0125(13) -0.0054(11) 0.0054(10) -0.0065(11) C22 0.0116(13) 0.0178(14) 0.0160(14) -0.0061(11) 0.0027(10) -0.0078(11) C23 0.0116(13) 0.0134(13) 0.0112(12) -0.0010(10) 0.0012(10) -0.0054(10) C24 0.0132(13) 0.0161(14) 0.0136(13) -0.0050(11) 0.0046(10) -0.0069(11) C25 0.0119(13) 0.0122(13) 0.0118(13) -0.0021(10) 0.0025(10) -0.0049(10) C26 0.0133(13) 0.0162(14) 0.0143(13) -0.0036(11) 0.0026(11) -0.0048(11) C27 0.0197(15) 0.0245(17) 0.0264(17) -0.0154(14) 0.0110(13) -0.0116(13) C28 0.0289(19) 0.032(2) 0.040(2) -0.0271(18) 0.0164(16) -0.0166(16) C29 0.0285(18) 0.0280(18) 0.0320(19) -0.0191(16) 0.0105(15) -0.0174(15) C30 0.0195(15) 0.0209(15) 0.0177(15) -0.0073(12) 0.0057(12) -0.0129(12) C31 0.0107(13) 0.0169(14) 0.0182(14) -0.0050(11) 0.0034(11) -0.0073(11) C32 0.0176(15) 0.0280(17) 0.0195(15) -0.0089(13) 0.0071(12) -0.0154(13) C33 0.0311(19) 0.035(2) 0.0223(17) -0.0123(15) 0.0092(14) -0.0249(16) C34 0.0204(16) 0.0244(17) 0.0219(16) -0.0070(13) 0.0041(12) -0.0138(13) C35 0.0175(14) 0.0215(15) 0.0163(14) -0.0071(12) 0.0047(11) -0.0117(12) C36 0.0229(17) 0.0305(18) 0.0190(16) -0.0069(14) 0.0033(13) -0.0173(14) C37 0.0236(17) 0.035(2) 0.0250(17) -0.0120(15) 0.0081(14) -0.0179(15) C38 0.0214(17) 0.0313(19) 0.0289(19) -0.0107(16) 0.0040(14) -0.0102(15) C39 0.0204(16) 0.0293(18) 0.0233(17) -0.0105(14) 0.0059(13) -0.0072(14) C40 0.0139(14) 0.0206(15) 0.0181(14) -0.0071(12) 0.0029(11) -0.0091(12) C43 0.065(7) 0.060(7) 0.023(4) -0.011(4) -0.002(4) -0.027(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 1.904(2) . ? Cu1 N2 1.927(3) . ? Cu1 N1 2.023(3) . ? Cu1 N3 2.037(3) . ? Cu1 O2 2.315(2) . ? Cu2 O8 1.922(2) . ? Cu2 N5 1.940(2) . ? Cu2 N4 2.032(3) . ? Cu2 N6 2.038(3) . ? Cu2 O90 2.166(2) . ? V1 O2 1.602(2) . ? V1 O4 1.941(2) . ? V1 O3 1.949(2) . ? V1 O7 1.974(2) . ? V1 O18 1.993(2) 1_545 ? V3 O13 1.601(3) . ? V3 O15 1.854(2) . ? V3 F1 1.897(2) . ? V3 O12 1.908(3) . ? V3 O14 1.962(2) . ? V4 O16 1.572(3) . ? V4 O19 1.918(3) . ? V4 F2 1.928(2) . ? V4 O15 1.941(3) . ? V4 O17 1.995(2) . ? V2A O6A 1.576(6) . ? V2A O5 1.960(3) . ? V2A O20A 1.966(5) . ? V2A O21 2.064(3) 2_665 ? V2A O4 2.083(3) . ? P5A O19 1.524(6) . ? P5A O21 1.535(6) . ? P5A C41A 1.746(10) . ? P5A O20A 1.952(6) 1_565 ? O20A P5A 1.952(6) 1_545 ? C41A C42A 1.497(13) . ? C41A H41A 0.9700 . ? C41A H41B 0.9700 . ? C42A C43 1.523(14) 2_775 ? C42A H42A 0.9700 . ? C42A H42B 0.9700 . ? V2B O6B 1.600(5) . ? V2B O21 1.911(3) 2_665 ? V2B O4 1.944(3) . ? V2B O20B 1.952(5) . ? V2B O5 1.977(3) . ? P5B O20B 1.390(6) 1_565 ? P5B O21 1.499(5) . ? P5B O19 1.503(5) . ? P5B C41B 1.777(9) . ? O20B P5B 1.390(6) 1_545 ? C41B C42B 1.477(11) . ? C41B H41C 0.9700 . ? C41B H41D 0.9700 . ? C42B C43 1.426(13) . ? C42B H42C 0.9700 . ? C42B H42D 0.9700 . ? P1 O5 1.519(2) . ? P1 O1 1.530(2) . ? P1 O3 1.548(2) . ? P1 C31 1.787(3) . ? P2 O7 1.513(2) . ? P2 O8 1.514(2) . ? P2 O9 1.581(2) . ? P2 C35 1.775(3) . ? P3 O10 1.485(2) . ? P3 O12 1.539(3) . ? P3 O11 1.585(2) . ? P3 C39 1.770(4) . ? P4 O14 1.526(2) . ? P4 O17 1.530(2) . ? P4 O18 1.545(2) . ? P4 C40 1.786(3) . ? O18 V1 1.993(2) 1_565 ? O21 V2B 1.911(3) 2_665 ? O21 V2A 2.064(3) 2_665 ? N1 C1 1.337(4) . ? N1 C5 1.361(4) . ? N2 C6 1.328(5) . ? N2 C10 1.337(4) . ? N3 C15 1.339(4) . ? N3 C11 1.363(4) . ? N4 C16 1.345(4) . ? N4 C20 1.352(4) . ? N5 C21 1.331(4) . ? N5 C25 1.335(4) . ? N6 C30 1.337(4) . ? N6 C26 1.359(4) . ? C1 C2 1.386(5) . ? C1 H1 0.9300 . ? C2 C3 1.383(5) . ? C2 H2 0.9300 . ? C3 C4 1.390(6) . ? C3 H3 0.9300 . ? C4 C5 1.373(5) . ? C4 H4 0.9300 . ? C5 C6 1.482(5) . ? C6 C7 1.392(5) . ? C7 C8 1.399(6) . ? C7 H7 0.9300 . ? C8 C9 1.383(6) . ? C8 C8 1.495(7) 2_765 ? C9 C10 1.389(4) . ? C9 H9 0.9300 . ? C10 C11 1.482(5) . ? C11 C12 1.374(5) . ? C12 C13 1.384(6) . ? C12 H12 0.9300 . ? C13 C14 1.374(6) . ? C13 H13 0.9300 . ? C14 C15 1.389(5) . ? C14 H14 0.9300 . ? C15 H15 0.9300 . ? C16 C17 1.376(5) . ? C16 H16 0.9300 . ? C17 C18 1.380(5) . ? C17 H17 0.9300 . ? C18 C19 1.390(5) . ? C18 H18 0.9300 . ? C19 C20 1.382(5) . ? C19 H19 0.9300 . ? C20 C21 1.478(4) . ? C21 C22 1.389(4) . ? C22 C23 1.398(4) . ? C22 H22 0.9300 . ? C23 C24 1.400(4) . ? C23 C23 1.494(5) 2_556 ? C24 C25 1.385(4) . ? C24 H24 0.9300 . ? C25 C26 1.482(4) . ? C26 C27 1.381(4) . ? C27 C28 1.389(5) . ? C27 H27 0.9300 . ? C28 C29 1.375(5) . ? C28 H28 0.9300 . ? C29 C30 1.393(5) . ? C29 H29 0.9300 . ? C30 H30 0.9300 . ? C31 C32 1.542(4) . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C32 C33 1.514(5) . ? C32 H32A 0.9700 . ? C32 H32B 0.9700 . ? C33 C34 1.518(5) . ? C33 H33A 0.9700 . ? C33 H33B 0.9700 . ? C34 C40 1.530(4) 1_445 ? C34 H34A 0.9700 . ? C34 H34B 0.9700 . ? C35 C36 1.529(4) . ? C35 H35A 0.9700 . ? C35 H35B 0.9700 . ? C36 C37 1.509(5) . ? C36 H36A 0.9700 . ? C36 H36B 0.9700 . ? C37 C38 1.533(5) . ? C37 H37A 0.9700 . ? C37 H37B 0.9700 . ? C38 C39 1.510(5) . ? C38 H38A 0.9700 . ? C38 H38B 0.9700 . ? C39 H39A 0.9700 . ? C39 H39B 0.9700 . ? C40 C34 1.530(4) 1_665 ? C40 H40A 0.9700 . ? C40 H40B 0.9700 . ? C43 C43 1.43(2) 2_775 ? C43 C42A 1.523(14) 2_775 ? C43 H43A 0.9700 . ? C43 H43B 0.9700 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Cu1 N2 168.97(11) . . ? O1 Cu1 N1 98.06(10) . . ? N2 Cu1 N1 80.11(12) . . ? O1 Cu1 N3 100.84(10) . . ? N2 Cu1 N3 79.90(12) . . ? N1 Cu1 N3 159.66(11) . . ? O1 Cu1 O2 101.19(9) . . ? N2 Cu1 O2 89.74(10) . . ? N1 Cu1 O2 90.62(11) . . ? N3 Cu1 O2 93.00(10) . . ? O8 Cu2 N5 165.64(10) . . ? O8 Cu2 N4 99.48(10) . . ? N5 Cu2 N4 79.86(10) . . ? O8 Cu2 N6 98.41(10) . . ? N5 Cu2 N6 79.29(10) . . ? N4 Cu2 N6 157.16(10) . . ? O8 Cu2 O90 98.75(9) . . ? N5 Cu2 O90 95.49(9) . . ? N4 Cu2 O90 99.45(10) . . ? N6 Cu2 O90 91.72(9) . . ? O2 V1 O4 107.17(12) . . ? O2 V1 O3 104.37(10) . . ? O4 V1 O3 87.19(10) . . ? O2 V1 O7 107.85(12) . . ? O4 V1 O7 144.92(10) . . ? O3 V1 O7 82.35(9) . . ? O2 V1 O18 105.38(10) . 1_545 ? O4 V1 O18 86.77(10) . 1_545 ? O3 V1 O18 150.11(9) . 1_545 ? O7 V1 O18 85.96(9) . 1_545 ? O13 V3 O15 99.15(15) . . ? O13 V3 F1 107.51(13) . . ? O15 V3 F1 153.12(12) . . ? O13 V3 O12 105.31(15) . . ? O15 V3 O12 90.53(11) . . ? F1 V3 O12 85.79(10) . . ? O13 V3 O14 104.76(13) . . ? O15 V3 O14 87.52(10) . . ? F1 V3 O14 82.56(9) . . ? O12 V3 O14 149.79(12) . . ? O16 V4 O19 111.13(17) . . ? O16 V4 F2 103.93(12) . . ? O19 V4 F2 86.42(10) . . ? O16 V4 O15 108.90(17) . . ? O19 V4 O15 139.80(14) . . ? F2 V4 O15 80.70(9) . . ? O16 V4 O17 104.12(12) . . ? O19 V4 O17 89.79(10) . . ? F2 V4 O17 151.14(9) . . ? O15 V4 O17 83.94(10) . . ? O6A V2A O5 105.0(2) . . ? O6A V2A O20A 101.0(3) . . ? O5 V2A O20A 153.8(2) . . ? O6A V2A O21 115.4(3) . 2_665 ? O5 V2A O21 79.68(12) . 2_665 ? O20A V2A O21 91.26(18) . 2_665 ? O6A V2A O4 112.6(2) . . ? O5 V2A O4 85.21(12) . . ? O20A V2A O4 82.75(17) . . ? O21 V2A O4 131.86(18) 2_665 . ? O19 P5A O21 108.4(4) . . ? O19 P5A C41A 101.6(4) . . ? O21 P5A C41A 106.4(4) . . ? O19 P5A O20A 86.8(3) . 1_565 ? O21 P5A O20A 90.5(3) . 1_565 ? C41A P5A O20A 157.2(5) . 1_565 ? P5A O20A V2A 134.1(3) 1_545 . ? C42A C41A P5A 116.7(7) . . ? C42A C41A H41A 108.1 . . ? P5A C41A H41A 108.1 . . ? C42A C41A H41B 108.1 . . ? P5A C41A H41B 108.1 . . ? H41A C41A H41B 107.3 . . ? C41A C42A C43 117.6(9) . 2_775 ? C41A C42A H42A 107.9 . . ? C43 C42A H42A 107.9 2_775 . ? C41A C42A H42B 107.9 . . ? C43 C42A H42B 107.9 2_775 . ? H42A C42A H42B 107.2 . . ? O6B V2B O21 100.6(2) . 2_665 ? O6B V2B O4 101.1(2) . . ? O21 V2B O4 158.27(17) 2_665 . ? O6B V2B O20B 110.6(3) . . ? O21 V2B O20B 90.42(18) 2_665 . ? O4 V2B O20B 82.66(17) . . ? O6B V2B O5 110.6(2) . . ? O21 V2B O5 83.10(12) 2_665 . ? O4 V2B O5 88.59(11) . . ? O20B V2B O5 138.78(19) . . ? O20B P5B O21 123.3(4) 1_565 . ? O20B P5B O19 125.3(4) 1_565 . ? O21 P5B O19 111.4(3) . . ? O20B P5B C41B 48.4(3) 1_565 . ? O21 P5B C41B 110.8(4) . . ? O19 P5B C41B 112.0(4) . . ? P5B O20B V2B 126.8(3) 1_545 . ? C42B C41B P5B 116.0(7) . . ? C42B C41B H41C 108.3 . . ? P5B C41B H41C 108.3 . . ? C42B C41B H41D 108.3 . . ? P5B C41B H41D 108.3 . . ? H41C C41B H41D 107.4 . . ? C43 C42B C41B 107.3(8) . . ? C43 C42B H42C 110.3 . . ? C41B C42B H42C 110.3 . . ? C43 C42B H42D 110.3 . . ? C41B C42B H42D 110.3 . . ? H42C C42B H42D 108.5 . . ? O5 P1 O1 111.18(13) . . ? O5 P1 O3 111.42(12) . . ? O1 P1 O3 110.39(12) . . ? O5 P1 C31 109.30(13) . . ? O1 P1 C31 108.19(13) . . ? O3 P1 C31 106.17(13) . . ? O7 P2 O8 114.26(13) . . ? O7 P2 O9 107.87(12) . . ? O8 P2 O9 109.67(13) . . ? O7 P2 C35 111.52(14) . . ? O8 P2 C35 107.93(14) . . ? O9 P2 C35 105.19(14) . . ? O10 P3 O12 110.95(14) . . ? O10 P3 O11 108.00(13) . . ? O12 P3 O11 111.08(14) . . ? O10 P3 C39 114.35(16) . . ? O12 P3 C39 106.29(17) . . ? O11 P3 C39 106.08(15) . . ? O14 P4 O17 113.95(13) . . ? O14 P4 O18 107.22(13) . . ? O17 P4 O18 109.54(12) . . ? O14 P4 C40 109.65(14) . . ? O17 P4 C40 109.86(14) . . ? O18 P4 C40 106.30(14) . . ? P1 O1 Cu1 127.08(13) . . ? V1 O2 Cu1 124.04(12) . . ? P1 O3 V1 125.33(13) . . ? V1 O4 V2B 140.88(14) . . ? V1 O4 V2A 141.12(13) . . ? V2B O4 V2A 14.17(5) . . ? P1 O5 V2A 138.77(15) . . ? P1 O5 V2B 139.33(14) . . ? V2A O5 V2B 15.04(4) . . ? P2 O7 V1 143.25(14) . . ? P2 O8 Cu2 134.23(14) . . ? P3 O12 V3 140.24(17) . . ? P4 O14 V3 129.85(14) . . ? V3 O15 V4 142.87(17) . . ? P4 O17 V4 133.79(14) . . ? P4 O18 V1 134.40(13) . 1_565 ? P5B O19 P5A 16.58(16) . . ? P5B O19 V4 142.0(2) . . ? P5A O19 V4 145.6(3) . . ? P5B O21 P5A 16.51(17) . . ? P5B O21 V2B 149.1(3) . 2_665 ? P5A O21 V2B 142.1(3) . 2_665 ? P5B O21 V2A 142.5(3) . 2_665 ? P5A O21 V2A 131.2(3) . 2_665 ? V2B O21 V2A 14.24(5) 2_665 2_665 ? C1 N1 C5 118.7(3) . . ? C1 N1 Cu1 127.0(2) . . ? C5 N1 Cu1 114.2(2) . . ? C6 N2 C10 121.4(3) . . ? C6 N2 Cu1 119.1(2) . . ? C10 N2 Cu1 119.4(2) . . ? C15 N3 C11 118.7(3) . . ? C15 N3 Cu1 127.1(2) . . ? C11 N3 Cu1 114.0(2) . . ? C16 N4 C20 117.9(3) . . ? C16 N4 Cu2 127.8(2) . . ? C20 N4 Cu2 113.8(2) . . ? C21 N5 C25 121.6(2) . . ? C21 N5 Cu2 118.7(2) . . ? C25 N5 Cu2 119.7(2) . . ? C30 N6 C26 119.4(3) . . ? C30 N6 Cu2 125.8(2) . . ? C26 N6 Cu2 114.4(2) . . ? N1 C1 C2 122.2(3) . . ? N1 C1 H1 118.9 . . ? C2 C1 H1 118.9 . . ? C3 C2 C1 118.8(4) . . ? C3 C2 H2 120.6 . . ? C1 C2 H2 120.6 . . ? C2 C3 C4 119.4(4) . . ? C2 C3 H3 120.3 . . ? C4 C3 H3 120.3 . . ? C5 C4 C3 118.7(3) . . ? C5 C4 H4 120.6 . . ? C3 C4 H4 120.6 . . ? N1 C5 C4 122.1(3) . . ? N1 C5 C6 113.4(3) . . ? C4 C5 C6 124.4(3) . . ? N2 C6 C7 120.4(4) . . ? N2 C6 C5 113.1(3) . . ? C7 C6 C5 126.6(4) . . ? C6 C7 C8 119.4(4) . . ? C6 C7 H7 120.3 . . ? C8 C7 H7 120.3 . . ? C9 C8 C7 118.6(3) . . ? C9 C8 C8 121.7(5) . 2_765 ? C7 C8 C8 119.7(5) . 2_765 ? C8 C9 C10 119.1(4) . . ? C8 C9 H9 120.4 . . ? C10 C9 H9 120.4 . . ? N2 C10 C9 121.0(4) . . ? N2 C10 C11 112.8(3) . . ? C9 C10 C11 126.2(3) . . ? N3 C11 C12 121.9(3) . . ? N3 C11 C10 113.6(3) . . ? C12 C11 C10 124.6(3) . . ? C11 C12 C13 118.8(3) . . ? C11 C12 H12 120.6 . . ? C13 C12 H12 120.6 . . ? C14 C13 C12 119.9(4) . . ? C14 C13 H13 120.1 . . ? C12 C13 H13 120.1 . . ? C13 C14 C15 118.8(4) . . ? C13 C14 H14 120.6 . . ? C15 C14 H14 120.6 . . ? N3 C15 C14 122.0(3) . . ? N3 C15 H15 119.0 . . ? C14 C15 H15 119.0 . . ? N4 C16 C17 123.1(3) . . ? N4 C16 H16 118.4 . . ? C17 C16 H16 118.4 . . ? C16 C17 C18 118.6(3) . . ? C16 C17 H17 120.7 . . ? C18 C17 H17 120.7 . . ? C17 C18 C19 119.4(3) . . ? C17 C18 H18 120.3 . . ? C19 C18 H18 120.3 . . ? C20 C19 C18 118.7(3) . . ? C20 C19 H19 120.7 . . ? C18 C19 H19 120.7 . . ? N4 C20 C19 122.3(3) . . ? N4 C20 C21 113.9(3) . . ? C19 C20 C21 123.8(3) . . ? N5 C21 C22 120.7(3) . . ? N5 C21 C20 113.0(3) . . ? C22 C21 C20 126.2(3) . . ? C21 C22 C23 119.1(3) . . ? C21 C22 H22 120.5 . . ? C23 C22 H22 120.5 . . ? C22 C23 C24 118.7(3) . . ? C22 C23 C23 120.3(3) . 2_556 ? C24 C23 C23 121.0(3) . 2_556 ? C25 C24 C23 118.9(3) . . ? C25 C24 H24 120.6 . . ? C23 C24 H24 120.6 . . ? N5 C25 C24 120.9(3) . . ? N5 C25 C26 112.5(2) . . ? C24 C25 C26 126.5(3) . . ? N6 C26 C27 121.8(3) . . ? N6 C26 C25 113.6(3) . . ? C27 C26 C25 124.6(3) . . ? C26 C27 C28 118.2(3) . . ? C26 C27 H27 120.9 . . ? C28 C27 H27 120.9 . . ? C29 C28 C27 120.3(3) . . ? C29 C28 H28 119.9 . . ? C27 C28 H28 119.9 . . ? C28 C29 C30 118.6(3) . . ? C28 C29 H29 120.7 . . ? C30 C29 H29 120.7 . . ? N6 C30 C29 121.7(3) . . ? N6 C30 H30 119.1 . . ? C29 C30 H30 119.1 . . ? C32 C31 P1 114.9(2) . . ? C32 C31 H31A 108.6 . . ? P1 C31 H31A 108.6 . . ? C32 C31 H31B 108.6 . . ? P1 C31 H31B 108.6 . . ? H31A C31 H31B 107.5 . . ? C33 C32 C31 115.0(3) . . ? C33 C32 H32A 108.5 . . ? C31 C32 H32A 108.5 . . ? C33 C32 H32B 108.5 . . ? C31 C32 H32B 108.5 . . ? H32A C32 H32B 107.5 . . ? C32 C33 C34 112.0(3) . . ? C32 C33 H33A 109.2 . . ? C34 C33 H33A 109.2 . . ? C32 C33 H33B 109.2 . . ? C34 C33 H33B 109.2 . . ? H33A C33 H33B 107.9 . . ? C33 C34 C40 113.1(3) . 1_445 ? C33 C34 H34A 109.0 . . ? C40 C34 H34A 109.0 1_445 . ? C33 C34 H34B 109.0 . . ? C40 C34 H34B 109.0 1_445 . ? H34A C34 H34B 107.8 . . ? C36 C35 P2 115.5(2) . . ? C36 C35 H35A 108.4 . . ? P2 C35 H35A 108.4 . . ? C36 C35 H35B 108.4 . . ? P2 C35 H35B 108.4 . . ? H35A C35 H35B 107.5 . . ? C37 C36 C35 111.9(3) . . ? C37 C36 H36A 109.2 . . ? C35 C36 H36A 109.2 . . ? C37 C36 H36B 109.2 . . ? C35 C36 H36B 109.2 . . ? H36A C36 H36B 107.9 . . ? C36 C37 C38 114.0(3) . . ? C36 C37 H37A 108.7 . . ? C38 C37 H37A 108.7 . . ? C36 C37 H37B 108.7 . . ? C38 C37 H37B 108.7 . . ? H37A C37 H37B 107.6 . . ? C39 C38 C37 112.0(3) . . ? C39 C38 H38A 109.2 . . ? C37 C38 H38A 109.2 . . ? C39 C38 H38B 109.2 . . ? C37 C38 H38B 109.2 . . ? H38A C38 H38B 107.9 . . ? C38 C39 P3 116.3(2) . . ? C38 C39 H39A 108.2 . . ? P3 C39 H39A 108.2 . . ? C38 C39 H39B 108.2 . . ? P3 C39 H39B 108.2 . . ? H39A C39 H39B 107.4 . . ? C34 C40 P4 113.5(2) 1_665 . ? C34 C40 H40A 108.9 1_665 . ? P4 C40 H40A 108.9 . . ? C34 C40 H40B 108.9 1_665 . ? P4 C40 H40B 108.9 . . ? H40A C40 H40B 107.7 . . ? C42B C43 C43 101.3(10) . 2_775 ? C42B C43 C42A 117.6(7) . 2_775 ? C43 C43 C42A 35.0(6) 2_775 2_775 ? C42B C43 H43A 111.5 . . ? C43 C43 H43A 111.5 2_775 . ? C42A C43 H43A 123.8 2_775 . ? C42B C43 H43B 111.5 . . ? C43 C43 H43B 111.5 2_775 . ? C42A C43 H43B 76.6 2_775 . ? H43A C43 H43B 109.3 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O6A V2A O20A P5A 165.8(4) . . . 1_545 ? O5 V2A O20A P5A -19.3(7) . . . 1_545 ? O21 V2A O20A P5A 49.6(4) 2_665 . . 1_545 ? O4 V2A O20A P5A -82.5(4) . . . 1_545 ? O19 P5A C41A C42A -60.6(9) . . . . ? O21 P5A C41A C42A -173.9(8) . . . . ? O20A P5A C41A C42A 49.5(17) 1_565 . . . ? P5A C41A C42A C43 172.1(9) . . . 2_775 ? O6B V2B O20B P5B 16.7(5) . . . 1_545 ? O21 V2B O20B P5B -84.8(4) 2_665 . . 1_545 ? O4 V2B O20B P5B 115.8(4) . . . 1_545 ? O5 V2B O20B P5B -164.8(3) . . . 1_545 ? O20B P5B C41B C42B 176.7(9) 1_565 . . . ? O21 P5B C41B C42B -66.6(7) . . . . ? O19 P5B C41B C42B 58.4(8) . . . . ? P5B C41B C42B C43 -120.8(8) . . . . ? O5 P1 O1 Cu1 -82.78(18) . . . . ? O3 P1 O1 Cu1 41.4(2) . . . . ? C31 P1 O1 Cu1 157.19(17) . . . . ? N2 Cu1 O1 P1 -179(29) . . . . ? N1 Cu1 O1 P1 -99.64(18) . . . . ? N3 Cu1 O1 P1 87.90(18) . . . . ? O2 Cu1 O1 P1 -7.40(19) . . . . ? O4 V1 O2 Cu1 87.30(17) . . . . ? O3 V1 O2 Cu1 -4.21(18) . . . . ? O7 V1 O2 Cu1 -90.67(16) . . . . ? O18 V1 O2 Cu1 178.65(13) 1_545 . . . ? O1 Cu1 O2 V1 -10.74(19) . . . . ? N2 Cu1 O2 V1 167.71(18) . . . . ? N1 Cu1 O2 V1 87.60(18) . . . . ? N3 Cu1 O2 V1 -112.42(17) . . . . ? O5 P1 O3 V1 55.57(18) . . . . ? O1 P1 O3 V1 -68.48(18) . . . . ? C31 P1 O3 V1 174.48(15) . . . . ? O2 V1 O3 P1 47.77(19) . . . . ? O4 V1 O3 P1 -59.23(16) . . . . ? O7 V1 O3 P1 154.33(17) . . . . ? O18 V1 O3 P1 -137.77(17) 1_545 . . . ? O2 V1 O4 V2B -62.3(3) . . . . ? O3 V1 O4 V2B 41.9(2) . . . . ? O7 V1 O4 V2B 114.3(3) . . . . ? O18 V1 O4 V2B -167.4(2) 1_545 . . . ? O2 V1 O4 V2A -84.9(3) . . . . ? O3 V1 O4 V2A 19.3(2) . . . . ? O7 V1 O4 V2A 91.7(3) . . . . ? O18 V1 O4 V2A 170.0(2) 1_545 . . . ? O6B V2B O4 V1 -130.1(3) . . . . ? O21 V2B O4 V1 47.8(6) 2_665 . . . ? O20B V2B O4 V1 120.2(3) . . . . ? O5 V2B O4 V1 -19.5(3) . . . . ? O6B V2B O4 V2A -30.4(4) . . . . ? O21 V2B O4 V2A 147.6(7) 2_665 . . . ? O20B V2B O4 V2A -140.1(4) . . . . ? O5 V2B O4 V2A 80.3(4) . . . . ? O6A V2A O4 V1 -92.3(3) . . . . ? O5 V2A O4 V1 12.0(3) . . . . ? O20A V2A O4 V1 168.8(3) . . . . ? O21 V2A O4 V1 83.6(3) 2_665 . . . ? O6A V2A O4 V2B 169.9(5) . . . . ? O5 V2A O4 V2B -85.8(4) . . . . ? O20A V2A O4 V2B 70.9(4) . . . . ? O21 V2A O4 V2B -14.3(3) 2_665 . . . ? O1 P1 O5 V2A 131.6(2) . . . . ? O3 P1 O5 V2A 8.0(3) . . . . ? C31 P1 O5 V2A -109.1(2) . . . . ? O1 P1 O5 V2B 108.6(2) . . . . ? O3 P1 O5 V2B -15.0(3) . . . . ? C31 P1 O5 V2B -132.1(2) . . . . ? O6A V2A O5 P1 79.1(3) . . . . ? O20A V2A O5 P1 -95.9(5) . . . . ? O21 V2A O5 P1 -167.2(2) 2_665 . . . ? O4 V2A O5 P1 -33.1(3) . . . . ? O6A V2A O5 V2B 179.9(5) . . . . ? O20A V2A O5 V2B 5.0(4) . . . . ? O21 V2A O5 V2B -66.4(4) 2_665 . . . ? O4 V2A O5 V2B 67.7(4) . . . . ? O6B V2B O5 P1 99.2(3) . . . . ? O21 V2B O5 P1 -162.0(2) 2_665 . . . ? O4 V2B O5 P1 -2.1(3) . . . . ? O20B V2B O5 P1 -79.3(3) . . . . ? O6B V2B O5 V2A 2.5(3) . . . . ? O21 V2B O5 V2A 101.4(4) 2_665 . . . ? O4 V2B O5 V2A -98.8(4) . . . . ? O20B V2B O5 V2A -175.9(5) . . . . ? O8 P2 O7 V1 -105.9(2) . . . . ? O9 P2 O7 V1 16.3(3) . . . . ? C35 P2 O7 V1 131.4(2) . . . . ? O2 V1 O7 P2 -111.2(2) . . . . ? O4 V1 O7 P2 72.2(3) . . . . ? O3 V1 O7 P2 146.1(2) . . . . ? O18 V1 O7 P2 -6.3(2) 1_545 . . . ? O7 P2 O8 Cu2 0.4(3) . . . . ? O9 P2 O8 Cu2 -120.81(19) . . . . ? C35 P2 O8 Cu2 125.1(2) . . . . ? N5 Cu2 O8 P2 156.2(3) . . . . ? N4 Cu2 O8 P2 70.1(2) . . . . ? N6 Cu2 O8 P2 -124.1(2) . . . . ? O90 Cu2 O8 P2 -31.1(2) . . . . ? O10 P3 O12 V3 150.6(3) . . . . ? O11 P3 O12 V3 30.5(3) . . . . ? C39 P3 O12 V3 -84.5(3) . . . . ? O13 V3 O12 P3 -98.3(3) . . . . ? O15 V3 O12 P3 1.3(3) . . . . ? F1 V3 O12 P3 154.7(3) . . . . ? O14 V3 O12 P3 87.3(3) . . . . ? O17 P4 O14 V3 49.0(2) . . . . ? O18 P4 O14 V3 170.41(16) . . . . ? C40 P4 O14 V3 -74.6(2) . . . . ? O13 V3 O14 P4 69.2(2) . . . . ? O15 V3 O14 P4 -29.6(2) . . . . ? F1 V3 O14 P4 175.42(19) . . . . ? O12 V3 O14 P4 -116.4(2) . . . . ? O13 V3 O15 V4 -141.3(3) . . . . ? F1 V3 O15 V4 31.4(4) . . . . ? O12 V3 O15 V4 113.1(3) . . . . ? O14 V3 O15 V4 -36.7(3) . . . . ? O16 V4 O15 V3 -46.1(3) . . . . ? O19 V4 O15 V3 139.2(3) . . . . ? F2 V4 O15 V3 -147.8(3) . . . . ? O17 V4 O15 V3 56.7(3) . . . . ? O14 P4 O17 V4 -10.6(2) . . . . ? O18 P4 O17 V4 -130.69(17) . . . . ? C40 P4 O17 V4 112.9(2) . . . . ? O16 V4 O17 P4 82.8(2) . . . . ? O19 V4 O17 P4 -165.5(2) . . . . ? F2 V4 O17 P4 -83.3(3) . . . . ? O15 V4 O17 P4 -25.3(2) . . . . ? O14 P4 O18 V1 -178.07(17) . . . 1_565 ? O17 P4 O18 V1 -53.9(2) . . . 1_565 ? C40 P4 O18 V1 64.7(2) . . . 1_565 ? O20B P5B O19 P5A -94.7(14) 1_565 . . . ? O21 P5B O19 P5A 83.8(13) . . . . ? C41B P5B O19 P5A -40.9(12) . . . . ? O20B P5B O19 V4 18.6(7) 1_565 . . . ? O21 P5B O19 V4 -162.9(3) . . . . ? C41B P5B O19 V4 72.4(5) . . . . ? O21 P5A O19 P5B -72.4(12) . . . . ? C41A P5A O19 P5B 175.8(16) . . . . ? O20A P5A O19 P5B 17.1(12) 1_565 . . . ? O21 P5A O19 V4 -161.5(3) . . . . ? C41A P5A O19 V4 86.6(6) . . . . ? O20A P5A O19 V4 -72.0(5) 1_565 . . . ? O16 V4 O19 P5B 78.7(4) . . . . ? F2 V4 O19 P5B -177.8(4) . . . . ? O15 V4 O19 P5B -106.7(4) . . . . ? O17 V4 O19 P5B -26.4(4) . . . . ? O16 V4 O19 P5A 106.3(4) . . . . ? F2 V4 O19 P5A -150.2(4) . . . . ? O15 V4 O19 P5A -79.1(5) . . . . ? O17 V4 O19 P5A 1.2(4) . . . . ? O20B P5B O21 P5A 96.1(13) 1_565 . . . ? O19 P5B O21 P5A -82.5(12) . . . . ? C41B P5B O21 P5A 42.9(11) . . . . ? O20B P5B O21 V2B 19.8(7) 1_565 . . 2_665 ? O19 P5B O21 V2B -158.8(4) . . . 2_665 ? C41B P5B O21 V2B -33.4(7) . . . 2_665 ? O20B P5B O21 V2A 42.4(6) 1_565 . . 2_665 ? O19 P5B O21 V2A -136.2(3) . . . 2_665 ? C41B P5B O21 V2A -10.8(6) . . . 2_665 ? O19 P5A O21 P5B 73.7(12) . . . . ? C41A P5A O21 P5B -177.7(15) . . . . ? O20A P5A O21 P5B -13.1(11) 1_565 . . . ? O19 P5A O21 V2B -160.4(3) . . . 2_665 ? C41A P5A O21 V2B -51.9(6) . . . 2_665 ? O20A P5A O21 V2B 112.7(4) 1_565 . . 2_665 ? O19 P5A O21 V2A -147.0(2) . . . 2_665 ? C41A P5A O21 V2A -38.4(6) . . . 2_665 ? O20A P5A O21 V2A 126.2(3) 1_565 . . 2_665 ? O1 Cu1 N1 C1 11.6(3) . . . . ? N2 Cu1 N1 C1 -179.4(3) . . . . ? N3 Cu1 N1 C1 169.8(3) . . . . ? O2 Cu1 N1 C1 -89.8(3) . . . . ? O1 Cu1 N1 C5 -171.2(3) . . . . ? N2 Cu1 N1 C5 -2.2(3) . . . . ? N3 Cu1 N1 C5 -12.9(5) . . . . ? O2 Cu1 N1 C5 87.4(3) . . . . ? O1 Cu1 N2 C6 82.6(7) . . . . ? N1 Cu1 N2 C6 1.2(3) . . . . ? N3 Cu1 N2 C6 177.5(3) . . . . ? O2 Cu1 N2 C6 -89.5(3) . . . . ? O1 Cu1 N2 C10 -98.6(7) . . . . ? N1 Cu1 N2 C10 -179.9(3) . . . . ? N3 Cu1 N2 C10 -3.7(3) . . . . ? O2 Cu1 N2 C10 89.4(3) . . . . ? O1 Cu1 N3 C15 -11.3(3) . . . . ? N2 Cu1 N3 C15 179.9(3) . . . . ? N1 Cu1 N3 C15 -169.4(3) . . . . ? O2 Cu1 N3 C15 90.7(3) . . . . ? O1 Cu1 N3 C11 174.0(2) . . . . ? N2 Cu1 N3 C11 5.2(2) . . . . ? N1 Cu1 N3 C11 16.0(5) . . . . ? O2 Cu1 N3 C11 -84.0(2) . . . . ? O8 Cu2 N4 C16 -15.4(3) . . . . ? N5 Cu2 N4 C16 179.1(3) . . . . ? N6 Cu2 N4 C16 -156.6(3) . . . . ? O90 Cu2 N4 C16 85.2(3) . . . . ? O8 Cu2 N4 C20 172.7(2) . . . . ? N5 Cu2 N4 C20 7.3(2) . . . . ? N6 Cu2 N4 C20 31.6(4) . . . . ? O90 Cu2 N4 C20 -86.6(2) . . . . ? O8 Cu2 N5 C21 -92.5(5) . . . . ? N4 Cu2 N5 C21 -3.9(2) . . . . ? N6 Cu2 N5 C21 -174.5(2) . . . . ? O90 Cu2 N5 C21 94.8(2) . . . . ? O8 Cu2 N5 C25 85.5(5) . . . . ? N4 Cu2 N5 C25 174.1(2) . . . . ? N6 Cu2 N5 C25 3.4(2) . . . . ? O90 Cu2 N5 C25 -87.3(2) . . . . ? O8 Cu2 N6 C30 15.2(3) . . . . ? N5 Cu2 N6 C30 -179.2(3) . . . . ? N4 Cu2 N6 C30 156.4(3) . . . . ? O90 Cu2 N6 C30 -83.9(3) . . . . ? O8 Cu2 N6 C26 -172.2(2) . . . . ? N5 Cu2 N6 C26 -6.6(2) . . . . ? N4 Cu2 N6 C26 -31.0(4) . . . . ? O90 Cu2 N6 C26 88.7(2) . . . . ? C5 N1 C1 C2 0.3(6) . . . . ? Cu1 N1 C1 C2 177.4(3) . . . . ? N1 C1 C2 C3 -0.2(7) . . . . ? C1 C2 C3 C4 0.2(7) . . . . ? C2 C3 C4 C5 -0.3(8) . . . . ? C1 N1 C5 C4 -0.3(6) . . . . ? Cu1 N1 C5 C4 -177.8(4) . . . . ? C1 N1 C5 C6 -179.8(3) . . . . ? Cu1 N1 C5 C6 2.7(4) . . . . ? C3 C4 C5 N1 0.4(7) . . . . ? C3 C4 C5 C6 179.7(5) . . . . ? C10 N2 C6 C7 1.2(6) . . . . ? Cu1 N2 C6 C7 180.0(3) . . . . ? C10 N2 C6 C5 -178.9(3) . . . . ? Cu1 N2 C6 C5 -0.1(5) . . . . ? N1 C5 C6 N2 -1.8(5) . . . . ? C4 C5 C6 N2 178.8(4) . . . . ? N1 C5 C6 C7 178.1(4) . . . . ? C4 C5 C6 C7 -1.3(8) . . . . ? N2 C6 C7 C8 -0.8(7) . . . . ? C5 C6 C7 C8 179.3(4) . . . . ? C6 C7 C8 C9 -0.6(7) . . . . ? C6 C7 C8 C8 178.5(5) . . . 2_765 ? C7 C8 C9 C10 1.6(6) . . . . ? C8 C8 C9 C10 -177.4(5) 2_765 . . . ? C6 N2 C10 C9 0.0(5) . . . . ? Cu1 N2 C10 C9 -178.9(3) . . . . ? C6 N2 C10 C11 -179.6(3) . . . . ? Cu1 N2 C10 C11 1.6(4) . . . . ? C8 C9 C10 N2 -1.4(5) . . . . ? C8 C9 C10 C11 178.1(4) . . . . ? C15 N3 C11 C12 -0.5(5) . . . . ? Cu1 N3 C11 C12 174.6(3) . . . . ? C15 N3 C11 C10 179.0(3) . . . . ? Cu1 N3 C11 C10 -5.8(4) . . . . ? N2 C10 C11 N3 3.0(4) . . . . ? C9 C10 C11 N3 -176.6(3) . . . . ? N2 C10 C11 C12 -177.5(3) . . . . ? C9 C10 C11 C12 3.0(6) . . . . ? N3 C11 C12 C13 0.7(6) . . . . ? C10 C11 C12 C13 -178.8(4) . . . . ? C11 C12 C13 C14 -0.6(7) . . . . ? C12 C13 C14 C15 0.4(8) . . . . ? C11 N3 C15 C14 0.3(6) . . . . ? Cu1 N3 C15 C14 -174.1(3) . . . . ? C13 C14 C15 N3 -0.3(7) . . . . ? C20 N4 C16 C17 2.5(5) . . . . ? Cu2 N4 C16 C17 -169.0(3) . . . . ? N4 C16 C17 C18 -1.0(6) . . . . ? C16 C17 C18 C19 -1.4(6) . . . . ? C17 C18 C19 C20 2.2(6) . . . . ? C16 N4 C20 C19 -1.6(5) . . . . ? Cu2 N4 C20 C19 171.1(3) . . . . ? C16 N4 C20 C21 178.0(3) . . . . ? Cu2 N4 C20 C21 -9.3(3) . . . . ? C18 C19 C20 N4 -0.8(6) . . . . ? C18 C19 C20 C21 179.7(3) . . . . ? C25 N5 C21 C22 -0.9(5) . . . . ? Cu2 N5 C21 C22 177.0(2) . . . . ? C25 N5 C21 C20 -177.9(3) . . . . ? Cu2 N5 C21 C20 0.0(3) . . . . ? N4 C20 C21 N5 6.3(4) . . . . ? C19 C20 C21 N5 -174.1(3) . . . . ? N4 C20 C21 C22 -170.5(3) . . . . ? C19 C20 C21 C22 9.0(5) . . . . ? N5 C21 C22 C23 -1.5(5) . . . . ? C20 C21 C22 C23 175.1(3) . . . . ? C21 C22 C23 C24 3.6(4) . . . . ? C21 C22 C23 C23 -174.5(3) . . . 2_556 ? C22 C23 C24 C25 -3.4(4) . . . . ? C23 C23 C24 C25 174.7(3) 2_556 . . . ? C21 N5 C25 C24 1.1(4) . . . . ? Cu2 N5 C25 C24 -176.8(2) . . . . ? C21 N5 C25 C26 178.0(3) . . . . ? Cu2 N5 C25 C26 0.1(3) . . . . ? C23 C24 C25 N5 1.1(4) . . . . ? C23 C24 C25 C26 -175.3(3) . . . . ? C30 N6 C26 C27 0.7(5) . . . . ? Cu2 N6 C26 C27 -172.4(3) . . . . ? C30 N6 C26 C25 -178.4(3) . . . . ? Cu2 N6 C26 C25 8.4(3) . . . . ? N5 C25 C26 N6 -5.7(4) . . . . ? C24 C25 C26 N6 171.0(3) . . . . ? N5 C25 C26 C27 175.2(3) . . . . ? C24 C25 C26 C27 -8.1(5) . . . . ? N6 C26 C27 C28 -0.8(5) . . . . ? C25 C26 C27 C28 178.2(3) . . . . ? C26 C27 C28 C29 0.5(6) . . . . ? C27 C28 C29 C30 -0.2(6) . . . . ? C26 N6 C30 C29 -0.3(5) . . . . ? Cu2 N6 C30 C29 172.0(3) . . . . ? C28 C29 C30 N6 0.0(6) . . . . ? O5 P1 C31 C32 58.7(3) . . . . ? O1 P1 C31 C32 179.9(2) . . . . ? O3 P1 C31 C32 -61.6(3) . . . . ? P1 C31 C32 C33 -80.6(3) . . . . ? C31 C32 C33 C34 -178.2(3) . . . . ? C32 C33 C34 C40 -178.5(3) . . . 1_445 ? O7 P2 C35 C36 -68.5(3) . . . . ? O8 P2 C35 C36 165.2(2) . . . . ? O9 P2 C35 C36 48.2(3) . . . . ? P2 C35 C36 C37 -176.4(3) . . . . ? C35 C36 C37 C38 175.4(3) . . . . ? C36 C37 C38 C39 175.3(3) . . . . ? C37 C38 C39 P3 175.2(3) . . . . ? O10 P3 C39 C38 -64.5(3) . . . . ? O12 P3 C39 C38 172.7(3) . . . . ? O11 P3 C39 C38 54.4(3) . . . . ? O14 P4 C40 C34 -60.0(3) . . . 1_665 ? O17 P4 C40 C34 174.0(2) . . . 1_665 ? O18 P4 C40 C34 55.6(3) . . . 1_665 ? C41B C42B C43 C43 157.0(10) . . . 2_775 ? C41B C42B C43 C42A -169.9(10) . . . 2_775 ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 31.51 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 1.900 _refine_diff_density_min -0.703 _refine_diff_density_rms 0.137