Supplementary Material (ESI) for J. Mater. Chem. This journal is (C) The Royal Society of Chemistry 2003. data_global _journal_name_full J.Mater.Chem. #======================================================================= _audit_creation_method 'Jana2000 Version : 10/10/2002' _journal_coden_Cambridge 1145 loop_ _publ_author_name 'Evgenia Spodine' 'Ana Maria Atria' 'Ricardo F. Baggio' 'E. Le Fur' 'Y. Moreno' 'Octavio Pena' ; J.Y.Pivan ; 'Andres Vega' _publ_contact_author_name 'Dr Evgenia Spodine' _publ_contact_author_address ; Facultad Ciencias Quimicas y Farmaceuticas Universidad de Chile Casilla 233 Santiago CHILE ; _publ_contact_author_email POSGRADO@UCHILE.CL _publ_section_title ; Magnetic Properties of Phosphate-Bridged Copper (II) organic/inorganic hybrid compounds ; _publ_section_references ; Petricek, V. & Dusek, M. (2000). Jana2000. Structure Determination Software Programs. Institute of Physics, Praha, Czech Republic. ; data_compound_triclinic _database_code_CSD 200041 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '[Cu2(phen)2(H2O)2 (H2PO4)2](NO3)2·2 H2O ' _chemical_formula_sum 'C24 H28 Cu2 N6 O18 P2' _chemical_formula_weight 877.54 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' 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 7.1367(6) _cell_length_b 10.6154(9) _cell_length_c 11.0626(9) _cell_angle_alpha 85.5410(10) _cell_angle_beta 83.1500(10) _cell_angle_gamma 70.6520(10) _cell_volume 784.46(11) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4685 _cell_measurement_theta_min 1.75 _cell_measurement_theta_max 28.03 _exptl_crystal_description plate _exptl_crystal_colour blue _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.858 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 446 _exptl_absorpt_coefficient_mu 1.552 _exptl_absorpt_correction_type 'not corrected' _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens SMART CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3889 _diffrn_reflns_av_R_equivalents 0.0362 _diffrn_reflns_av_sigmaI/netI 0.0491 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.86 _diffrn_reflns_theta_max 28.03 _reflns_number_total 3292 _reflns_number_gt 2652 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART (BRUKER 1996)' _computing_data_reduction 'Bruker SAINTPLUS V6.02 (BRUKER 1997)' _computing_structure_solution 'Bruker SHELXTL V6.10(BRUKER 2000)' _computing_structure_refinement 'Bruker SHELXTL V6.10(BRUKER 2000)' _computing_molecular_graphics 'Bruker SHELXTL V6.10(BRUKER 2000)' _computing_publication_material 'Bruker SHELXTL V6.10(BRUKER 2000)' _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^)+(0.0442P)^2^+0.0000P] where P==(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3292 _refine_ls_number_parameters 259 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0426 _refine_ls_R_factor_gt 0.0347 _refine_ls_wR_factor_ref 0.0865 _refine_ls_wR_factor_gt 0.0832 _refine_ls_goodness_of_fit_ref 0.950 _refine_ls_restrained_S_all 0.950 _refine_ls_shift/su_max 0.011 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu Cu 0.66099(5) 0.52508(3) 0.68182(3) 0.02994(12) Uani 1 1 d . . . P P 0.62548(10) 0.30637(6) 0.51213(6) 0.02947(17) Uani 1 1 d . . . O1P O 0.7883(3) 0.1647(2) 0.5114(2) 0.0419(5) Uani 1 1 d . . . H1P H 0.846(5) 0.156(3) 0.455(3) 0.034(10) Uiso 1 1 d . . . O2P O 0.4693(4) 0.2943(3) 0.6188(2) 0.0467(6) Uani 1 1 d . . . H2P H 0.436(5) 0.243(3) 0.615(3) 0.045(12) Uiso 1 1 d . . . O3P O 0.5444(3) 0.33298(17) 0.39047(16) 0.0366(5) Uani 1 1 d . . . O4P O 0.7127(3) 0.40765(17) 0.54707(16) 0.0351(4) Uani 1 1 d . . . N N 0.1816(4) 0.0667(2) 0.2931(2) 0.0424(6) Uani 1 1 d . . . O1N O 0.2923(4) -0.0004(2) 0.2118(2) 0.0617(7) Uani 1 1 d . . . O2N O 0.2542(4) 0.1102(2) 0.3731(2) 0.0542(6) Uani 1 1 d . . . O3N O -0.0026(3) 0.0947(2) 0.2963(2) 0.0532(6) Uani 1 1 d . . . O1W O 0.9194(4) 0.6045(3) 0.6090(2) 0.0504(6) Uani 1 1 d . . . H1WA H 1.015(5) 0.595(3) 0.568(3) 0.037(10) Uiso 1 1 d . . . H1WB H 0.872(7) 0.680(4) 0.595(4) 0.095(19) Uiso 1 1 d . . . O2W O 0.3461(5) 0.0843(3) 0.6253(3) 0.0580(7) Uani 1 1 d . . . H2WA H 0.446(7) 0.017(4) 0.630(4) 0.082(16) Uiso 1 1 d . . . H2WB H 0.296(10) 0.072(6) 0.580(6) 0.17(3) Uiso 1 1 d . . . N1 N 0.8119(3) 0.3796(2) 0.79667(19) 0.0304(5) Uani 1 1 d . . . N2 N 0.6045(3) 0.6327(2) 0.83275(19) 0.0284(5) Uani 1 1 d . . . C1 C 0.9161(4) 0.2529(3) 0.7760(2) 0.0373(7) Uani 1 1 d . . . H1 H 0.9273 0.2225 0.6980 0.045 Uiso 1 1 calc R . . C2 C 1.0096(4) 0.1633(3) 0.8668(3) 0.0392(7) Uani 1 1 d . . . H2 H 1.0826 0.0754 0.8487 0.047 Uiso 1 1 calc R . . C3 C 0.9935(4) 0.2050(3) 0.9821(3) 0.0370(7) Uani 1 1 d . . . H3 H 1.0542 0.1456 1.0432 0.044 Uiso 1 1 calc R . . C4 C 0.8846(4) 0.3385(3) 1.0079(2) 0.0316(6) Uani 1 1 d . . . C5 C 0.8610(4) 0.3944(3) 1.1248(2) 0.0382(7) Uani 1 1 d . . . H5 H 0.9187 0.3401 1.1896 0.046 Uiso 1 1 calc R . . C6 C 0.7566(4) 0.5246(3) 1.1427(2) 0.0369(6) Uani 1 1 d . . . H6 H 0.7438 0.5581 1.2196 0.044 Uiso 1 1 calc R . . C7 C 0.6654(4) 0.6115(3) 1.0456(2) 0.0317(6) Uani 1 1 d . . . C8 C 0.5557(4) 0.7478(3) 1.0570(2) 0.0370(6) Uani 1 1 d . . . H8 H 0.5373 0.7872 1.1316 0.044 Uiso 1 1 calc R . . C9 C 0.4759(4) 0.8220(3) 0.9572(3) 0.0400(7) Uani 1 1 d . . . H9 H 0.4049 0.9125 0.9633 0.048 Uiso 1 1 calc R . . C10 C 0.5020(4) 0.7608(3) 0.8464(3) 0.0356(6) Uani 1 1 d . . . H10 H 0.4454 0.8119 0.7798 0.043 Uiso 1 1 calc R . . C11 C 0.6854(4) 0.5595(3) 0.9305(2) 0.0286(6) Uani 1 1 d . . . C12 C 0.7974(4) 0.4219(3) 0.9113(2) 0.0286(6) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu 0.0343(2) 0.0311(2) 0.02414(18) -0.00495(13) -0.00568(13) -0.00840(14) P 0.0360(4) 0.0272(4) 0.0229(3) -0.0046(3) -0.0040(3) -0.0060(3) O1P 0.0497(14) 0.0352(12) 0.0315(12) -0.0019(9) -0.0047(10) -0.0011(10) O2P 0.0573(15) 0.0476(15) 0.0370(12) -0.0115(10) 0.0091(10) -0.0219(13) O3P 0.0443(12) 0.0326(10) 0.0297(10) -0.0068(8) -0.0127(9) -0.0037(9) O4P 0.0423(11) 0.0337(10) 0.0304(10) -0.0078(8) -0.0079(8) -0.0110(9) N 0.0544(17) 0.0284(13) 0.0405(15) -0.0012(11) -0.0029(12) -0.0091(12) O1N 0.0633(16) 0.0586(15) 0.0536(15) -0.0192(12) 0.0118(12) -0.0093(12) O2N 0.0657(16) 0.0464(13) 0.0535(14) -0.0066(10) -0.0128(12) -0.0190(11) O3N 0.0436(13) 0.0608(15) 0.0484(13) -0.0124(11) -0.0066(10) -0.0050(11) O1W 0.0453(15) 0.0485(16) 0.0595(16) -0.0102(12) 0.0119(12) -0.0219(12) O2W 0.0528(16) 0.0638(18) 0.0592(17) -0.0094(13) 0.0005(13) -0.0221(14) N1 0.0305(12) 0.0335(12) 0.0274(11) -0.0058(9) -0.0044(9) -0.0091(10) N2 0.0295(12) 0.0307(12) 0.0261(11) -0.0047(9) -0.0026(9) -0.0106(9) C1 0.0391(16) 0.0401(17) 0.0308(15) -0.0110(12) -0.0057(12) -0.0075(13) C2 0.0374(16) 0.0331(15) 0.0434(17) -0.0056(12) -0.0091(13) -0.0037(12) C3 0.0356(15) 0.0386(16) 0.0377(16) 0.0023(12) -0.0105(13) -0.0117(12) C4 0.0312(14) 0.0390(15) 0.0278(14) -0.0005(11) -0.0051(11) -0.0152(12) C5 0.0434(17) 0.0505(18) 0.0263(14) 0.0008(12) -0.0084(12) -0.0215(14) C6 0.0413(16) 0.0513(18) 0.0240(13) -0.0068(12) -0.0039(12) -0.0217(14) C7 0.0301(14) 0.0417(16) 0.0290(14) -0.0087(11) 0.0013(11) -0.0189(12) C8 0.0380(16) 0.0456(17) 0.0319(14) -0.0141(12) 0.0010(12) -0.0183(13) C9 0.0411(17) 0.0345(16) 0.0446(17) -0.0129(13) -0.0007(13) -0.0111(13) C10 0.0399(16) 0.0358(16) 0.0332(15) -0.0017(12) -0.0046(12) -0.0148(13) C11 0.0258(13) 0.0364(15) 0.0275(13) -0.0039(11) 0.0001(10) -0.0156(11) C12 0.0273(13) 0.0357(15) 0.0265(13) -0.0036(11) -0.0019(10) -0.0150(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu O3P 1.9202(17) 2_666 Y Cu O4P 1.9405(18) . Y Cu N1 2.019(2) . Y Cu N2 2.021(2) . Y Cu O1W 2.308(2) . Y P O3P 1.4982(17) . ? P O4P 1.5027(19) . ? P O2P 1.552(2) . ? P O1P 1.566(2) . ? O3P Cu 1.9202(17) 2_666 ? N O1N 1.224(3) . ? N O3N 1.245(3) . ? N O2N 1.263(3) . ? N1 C1 1.327(3) . ? N1 C12 1.359(3) . ? N2 C10 1.325(3) . ? N2 C11 1.352(3) . ? C1 C2 1.396(4) . ? C2 C3 1.361(4) . ? C3 C4 1.405(4) . ? C4 C12 1.399(4) . ? C4 C5 1.433(4) . ? C5 C6 1.353(4) . ? C6 C7 1.430(4) . ? C7 C11 1.400(3) . ? C7 C8 1.406(4) . ? C8 C9 1.372(4) . ? C9 C10 1.395(4) . ? C11 C12 1.433(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 O3P Cu O4P 94.76(7) 2_666 . Y O3P Cu N1 163.29(9) 2_666 . Y O4P Cu N1 94.17(8) . . Y O3P Cu N2 88.64(8) 2_666 . Y O4P Cu N2 174.54(8) . . Y N1 Cu N2 81.51(8) . . Y O3P Cu O1W 95.95(10) 2_666 . Y O4P Cu O1W 92.70(9) . . Y N1 Cu O1W 97.71(10) . . Y N2 Cu O1W 91.19(9) . . Y O3P P O4P 115.11(11) . . ? O3P P O2P 113.39(13) . . ? O4P P O2P 106.64(13) . . ? O3P P O1P 107.83(11) . . ? O4P P O1P 109.50(12) . . ? O2P P O1P 103.76(13) . . ? P O3P Cu 135.15(11) . 2_666 ? P O4P Cu 135.17(12) . . ? O1N N O3N 120.4(3) . . ? O1N N O2N 119.9(3) . . ? O3N N O2N 119.6(3) . . ? C1 N1 C12 117.7(2) . . ? C1 N1 Cu 129.54(18) . . ? C12 N1 Cu 112.72(16) . . ? C10 N2 C11 118.2(2) . . ? C10 N2 Cu 128.86(18) . . ? C11 N2 Cu 112.96(17) . . ? N1 C1 C2 122.6(3) . . ? C3 C2 C1 119.8(3) . . ? C2 C3 C4 119.5(2) . . ? C12 C4 C3 117.0(2) . . ? C12 C4 C5 118.5(2) . . ? C3 C4 C5 124.5(2) . . ? C6 C5 C4 121.3(2) . . ? C5 C6 C7 121.1(2) . . ? C11 C7 C8 116.8(2) . . ? C11 C7 C6 118.8(2) . . ? C8 C7 C6 124.4(2) . . ? C9 C8 C7 119.4(3) . . ? C8 C9 C10 119.7(3) . . ? N2 C10 C9 122.4(3) . . ? N2 C11 C7 123.6(2) . . ? N2 C11 C12 116.4(2) . . ? C7 C11 C12 120.0(2) . . ? N1 C12 C4 123.4(2) . . ? N1 C12 C11 116.4(2) . . ? C4 C12 C11 120.2(2) . . ? _diffrn_measured_fraction_theta_max 0.864 _diffrn_reflns_theta_full 28.03 _diffrn_measured_fraction_theta_full 0.864 _refine_diff_density_max 0.453 _refine_diff_density_min -0.340 _refine_diff_density_rms 0.072 data_[Cu2(dpa)2(V2P2O12)]n _database_code_CSD 200042 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety [Cu2(dpa)2(V2P2O12)]n _chemical_formula_sum 'C10 H9 Cu N3 O6 P V' _chemical_formula_weight 412.65 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 7.3914(17) _cell_length_b 9.863(2) _cell_length_c 10.311(2) _cell_angle_alpha 107.030(4) _cell_angle_beta 105.119(4) _cell_angle_gamma 98.158(4) _cell_volume 674.1(3) _cell_formula_units_Z 2 _cell_measurement_temperature 273(2) _cell_measurement_reflns_used 4707 _cell_measurement_theta_min 2.0 _cell_measurement_theta_max 27.99 _exptl_crystal_description needles _exptl_crystal_colour green _exptl_crystal_size_max 0.09 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.033 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 410 _exptl_absorpt_coefficient_mu 2.422 _exptl_absorpt_correction_type 'SADABS (BRUKER, 1996)' _exptl_absorpt_correction_T_min 0.584 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 273(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens SMART CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 'no decay' _diffrn_reflns_number 3408 _diffrn_reflns_av_R_equivalents 0.0700 _diffrn_reflns_av_sigmaI/netI 0.2000 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.18 _diffrn_reflns_theta_max 27.99 _reflns_number_total 2816 _reflns_number_gt 1260 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART (BRUKER 1996)' _computing_data_reduction 'Bruker SAINTPLUS V6.02 (BRUKER 1997)' _computing_structure_solution 'Bruker SHELXTL V6.10(BRUKER 2000)' _computing_structure_refinement 'Bruker SHELXTL V6.10(BRUKER 2000)' _computing_molecular_graphics 'Bruker SHELXTL V6.10(BRUKER 2000)' _computing_publication_material 'Bruker SHELXTL V6.10(BRUKER 2000)' _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^)+(0.0229P)^2^+0.0000P] where P==(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2816 _refine_ls_number_parameters 235 _refine_ls_number_restraints 9 _refine_ls_R_factor_all 0.1393 _refine_ls_R_factor_gt 0.0570 _refine_ls_wR_factor_ref 0.1080 _refine_ls_wR_factor_gt 0.0888 _refine_ls_goodness_of_fit_ref 0.765 _refine_ls_restrained_S_all 0.764 _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 Cu Cu 0.38305(14) 0.50920(10) 0.25142(9) 0.0388(3) Uani 1 1 d . . . N1 N 0.2632(8) 0.3929(6) 0.0472(6) 0.0323(16) Uani 1 1 d . . . C1 C 0.2215(12) 0.2466(9) 0.0110(8) 0.046(2) Uani 1 1 d D . . H1 H 0.287(8) 0.205(6) 0.089(4) 0.04(2) Uiso 1 1 d D . . C2 C 0.1167(12) 0.1510(9) -0.1218(8) 0.050(2) Uani 1 1 d D . . H2 H 0.089(10) 0.041(2) -0.128(7) 0.06(3) Uiso 1 1 d D . . C3 C 0.0468(12) 0.2062(10) -0.2264(8) 0.053(2) Uani 1 1 d D . . H3 H -0.061(7) 0.144(7) -0.324(4) 0.08(3) Uiso 1 1 d D . . C4 C 0.0825(12) 0.3528(10) -0.1958(8) 0.046(2) Uani 1 1 d D . . H4 H 0.022(9) 0.412(7) -0.258(6) 0.07(3) Uiso 1 1 d D . . C5 C 0.1962(10) 0.4432(9) -0.0562(8) 0.037(2) Uani 1 1 d . . . N2 N 0.2287(9) 0.5935(8) -0.0286(6) 0.0426(18) Uani 1 1 d D . . H2N H 0.152(7) 0.606(6) -0.112(3) 0.028(19) Uiso 1 1 d D . . C6 C 0.3353(10) 0.7125(8) 0.0893(7) 0.0314(18) Uani 1 1 d . . . C7 C 0.3564(12) 0.8503(9) 0.0765(8) 0.046(2) Uani 1 1 d D . . H7 H 0.267(8) 0.870(7) -0.010(5) 0.07(3) Uiso 1 1 d D . . C8 C 0.4615(12) 0.9696(8) 0.1922(10) 0.050(2) Uani 1 1 d D . . H8 H 0.428(9) 1.055(5) 0.156(6) 0.06(2) Uiso 1 1 d D . . C9 C 0.5490(12) 0.9534(8) 0.3171(8) 0.041(2) Uani 1 1 d D . . H9 H 0.652(6) 1.021(5) 0.415(3) 0.04(2) Uiso 1 1 d D . . C10 C 0.5277(11) 0.8166(9) 0.3250(7) 0.041(2) Uani 1 1 d D . . H10 H 0.588(6) 0.810(5) 0.426(2) 0.005(14) Uiso 1 1 d D . . N3 N 0.4182(8) 0.6942(6) 0.2120(6) 0.0291(15) Uani 1 1 d . . . P P 0.6683(3) 0.3960(2) 0.4330(2) 0.0285(5) Uani 1 1 d . . . O1 O 0.5053(7) 0.3590(5) 0.2991(4) 0.0392(13) Uani 1 1 d . . . O2 O 0.6102(7) 0.3921(5) 0.5589(4) 0.0416(14) Uani 1 1 d . . . O3 O 0.7968(6) 0.5493(5) 0.4608(4) 0.0340(13) Uani 1 1 d . . . O4 O 0.7971(7) 0.2845(5) 0.4087(5) 0.0476(15) Uani 1 1 d . . . V V 0.96535(18) 0.70064(13) 0.61460(13) 0.0337(4) Uani 1 1 d . . . O5 O 0.9044(7) 0.8501(5) 0.6210(5) 0.0573(17) Uani 1 1 d . . . O6 O 0.9723(8) 0.6687(6) 0.7581(5) 0.0649(18) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu 0.0501(7) 0.0304(6) 0.0275(5) 0.0097(4) 0.0016(5) 0.0052(5) N1 0.031(4) 0.034(4) 0.028(3) 0.012(3) 0.002(3) 0.006(3) C1 0.048(6) 0.040(5) 0.035(5) 0.008(4) -0.003(4) 0.007(4) C2 0.062(6) 0.035(6) 0.036(5) 0.001(4) 0.001(5) 0.010(5) C3 0.044(6) 0.045(6) 0.038(5) -0.011(4) 0.004(5) -0.011(4) C4 0.041(6) 0.057(6) 0.031(5) 0.012(4) 0.006(4) 0.005(5) C5 0.028(5) 0.042(5) 0.036(5) 0.008(4) 0.014(4) 0.001(4) N2 0.044(5) 0.060(5) 0.025(4) 0.027(4) 0.001(3) 0.010(4) C6 0.027(5) 0.037(5) 0.030(4) 0.009(4) 0.013(4) 0.007(4) C7 0.047(6) 0.039(5) 0.054(6) 0.033(5) 0.001(5) 0.007(4) C8 0.057(6) 0.025(5) 0.071(6) 0.027(5) 0.012(5) 0.010(4) C9 0.055(6) 0.023(5) 0.034(5) 0.007(4) 0.008(4) -0.002(4) C10 0.047(6) 0.044(5) 0.023(4) 0.010(4) 0.005(4) 0.000(4) N3 0.027(4) 0.028(4) 0.031(3) 0.016(3) 0.003(3) 0.001(3) P 0.0284(12) 0.0214(11) 0.0286(11) 0.0065(8) 0.0021(10) 0.0020(9) O1 0.043(3) 0.027(3) 0.034(3) 0.011(2) -0.004(3) -0.002(2) O2 0.066(4) 0.034(3) 0.023(3) 0.011(2) 0.017(3) -0.001(3) O3 0.041(3) 0.024(3) 0.032(3) 0.008(2) 0.010(2) -0.002(2) O4 0.033(3) 0.024(3) 0.073(4) 0.006(3) 0.012(3) -0.001(2) V 0.0330(9) 0.0286(8) 0.0303(7) 0.0048(6) 0.0020(6) 0.0057(6) O5 0.055(4) 0.025(3) 0.067(4) -0.001(3) -0.002(3) 0.009(3) O6 0.057(4) 0.103(5) 0.036(3) 0.028(3) 0.010(3) 0.024(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu O2 1.896(4) 2_666 Y Cu O1 1.956(5) . Y Cu N1 1.964(5) . Y Cu N3 1.979(5) . Y N3 C6 1.330(8) . ? N3 C10 1.370(8) . ? C10 C9 1.365(9) . ? C9 C8 1.349(10) . ? C8 C7 1.359(10) . ? C7 C6 1.394(9) . ? C6 N2 1.371(8) . ? N2 C5 1.397(9) . ? C5 N1 1.317(8) . ? C5 C4 1.406(9) . ? C4 C3 1.357(11) . ? C3 C2 1.364(11) . ? C2 C1 1.359(9) . ? C1 N1 1.347(9) . ? P O1 1.484(4) . ? P O2 1.479(4) . ? P O3 1.570(5) . ? P O4 1.561(5) . ? O3 V 1.830(4) . ? O2 Cu 1.896(4) 2_666 ? O4 V 1.825(5) 2_766 ? V O4 1.825(5) 2_766 Y V O5 1.589(5) . Y V O6 1.590(5) . Y 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 Cu O1 94.8(2) 2_666 . Y O2 Cu N1 156.4(2) 2_666 . Y O1 Cu N1 94.7(2) . . Y O2 Cu N3 91.7(2) 2_666 . Y O1 Cu N3 146.4(2) . . Y N1 Cu N3 92.3(2) . . Y C6 N3 C10 117.0(6) . . ? C6 N3 Cu 126.2(5) . . ? C10 N3 Cu 116.6(5) . . ? C9 C1 N3 123.0(7) . . ? C8 C9 C10 119.0(7) . . ? C9 C8 C7 119.8(7) . . ? C8 C7 C6 119.6(7) . . ? N3 C6 N2 119.6(7) . . ? N3 C6 C7 121.6(7) . . ? N2 C6 C7 118.8(7) . . ? C6 N2 C5 133.1(6) . . ? N1 C5 N2 120.2(6) . . ? N1 C5 C4 123.3(8) . . ? N2 C5 C4 116.4(7) . . ? C3 C7 C5 118.1(8) . . ? C4 C8 C2 119.8(7) . . ? C1 C9 C3 118.1(8) . . ? N1 C10 C2 124.7(7) . . ? C5 N3 C1 115.9(6) . . ? C5 N3 Cu 126.2(5) . . ? C1 N3 Cu 117.3(5) . . ? O3 P O1 114.6(3) . . ? O3 P O4 107.4(3) . . ? O3 P O4 108.8(3) . . ? O3 P O2 111.6(3) . . ? O1 P O2 107.7(3) . . ? O4 P O2 106.4(3) . . ? P O1 Cu 121.1(3) . . ? P O3 V 137.3(3) . . ? P O2 Cu 148.6(3) . 2_666 ? P O4 V 132.7(3) . 2_766 ? O5 V O6 110.4(3) . . Y O5 V O4 108.2(3) . 2_766 Y O6 V O4 110.0(3) . 2_766 Y O5 V O2 110.7(2) . . Y O6 V O2 109.7(3) . . Y O4 V O2 107.7(2) 2_766 . Y _diffrn_measured_fraction_theta_max 0.867 _diffrn_reflns_theta_full 27.99 _diffrn_measured_fraction_theta_full 0.867 _refine_diff_density_max 0.495 _refine_diff_density_min -0.453 _refine_diff_density_rms 0.107 data_[(VO2)2(bipy)2(PO3OH)] _database_code_CSD 200043 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety [(VO2)2(bipy)2(PO3OH)] _chemical_formula_sum 'C10 H8 N2 O5.63 P0.50 V' _chemical_formula_weight 312.61 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'C 2/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 13.9768(16) _cell_length_b 22.157(3) _cell_length_c 9.1984(10) _cell_angle_alpha 90.00 _cell_angle_beta 103.165(2) _cell_angle_gamma 90.00 _cell_volume 2773.7(5) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 8349 _cell_measurement_theta_min 2.0 _cell_measurement_theta_max 25.01 _exptl_crystal_description needles _exptl_crystal_colour yellow _exptl_crystal_size_max 0.6 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.497 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1260 _exptl_absorpt_coefficient_mu 0.792 _exptl_absorpt_correction_type 'SADABS (Bruker, 1996)' _exptl_absorpt_correction_T_min 0.443 _exptl_absorpt_correction_T_max 1 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens SMART CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 'no decay' _diffrn_reflns_number 5701 _diffrn_reflns_av_R_equivalents 0.0289 _diffrn_reflns_av_sigmaI/netI 0.0387 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 1.76 _diffrn_reflns_theta_max 25.01 _reflns_number_total 2438 _reflns_number_gt 1826 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART (BRUKER 1996)' _computing_data_reduction 'Bruker SAINTPLUS V6.02 (BRUKER 1997)' _computing_structure_solution 'Bruker SHELXTL V6.10(BRUKER 2000)' _computing_structure_refinement 'Bruker SHELXTL V6.10(BRUKER 2000)' _computing_molecular_graphics 'Bruker SHELXTL V6.10(BRUKER 2000)' _computing_publication_material 'Bruker SHELXTL V6.10(BRUKER 2000)' _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^)+(0.1488P)^2^+0.2910P] 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 2438 _refine_ls_number_parameters 181 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0863 _refine_ls_R_factor_gt 0.0668 _refine_ls_wR_factor_ref 0.2228 _refine_ls_wR_factor_gt 0.2009 _refine_ls_goodness_of_fit_ref 1.077 _refine_ls_restrained_S_all 1.077 _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 V V 0.11312(6) 0.17165(3) 0.25447(8) 0.0475(4) Uani 1 1 d . . . O1 O 0.0832(3) 0.08792(15) 0.2174(4) 0.0633(10) Uani 1 1 d . . . O2 O 0.0412(4) 0.0101(3) 0.3864(8) 0.154(3) Uani 1 1 d . . . P P 0.0000 0.04910(9) 0.2500 0.0810(8) Uani 1 2 d S . . N1 N 0.1200(3) 0.26511(18) 0.2088(5) 0.0557(10) Uani 1 1 d . . . N2 N 0.1214(3) 0.17866(18) 0.0189(5) 0.0537(10) Uani 1 1 d . . . C1 C 0.1230(5) 0.3056(3) 0.3183(8) 0.0792(18) Uani 1 1 d . . . H1 H 0.1225 0.2922 0.4139 0.095 Uiso 1 1 calc R . . C2 C 0.1269(6) 0.3678(3) 0.2908(12) 0.112(3) Uani 1 1 d . . . H2 H 0.1298 0.3959 0.3668 0.135 Uiso 1 1 calc R . . C3 C 0.1263(6) 0.3856(3) 0.1483(14) 0.118(3) Uani 1 1 d . . . H3 H 0.1281 0.4264 0.1259 0.141 Uiso 1 1 calc R . . C4 C 0.1230(5) 0.3433(3) 0.0381(9) 0.089(2) Uani 1 1 d . . . H4 H 0.1219 0.3557 -0.0589 0.107 Uiso 1 1 calc R . . C5 C 0.1215(4) 0.2838(2) 0.0703(6) 0.0599(13) Uani 1 1 d . . . C6 C 0.1235(3) 0.2349(3) -0.0358(5) 0.0582(13) Uani 1 1 d . . . C7 C 0.1292(4) 0.2435(4) -0.1823(6) 0.0785(18) Uani 1 1 d . . . H7 H 0.1320 0.2822 -0.2200 0.094 Uiso 1 1 calc R . . C8 C 0.1308(5) 0.1939(5) -0.2715(7) 0.103(3) Uani 1 1 d . . . H8 H 0.1351 0.1990 -0.3702 0.124 Uiso 1 1 calc R . . C9 C 0.1261(5) 0.1372(4) -0.2153(7) 0.100(3) Uani 1 1 d . . . H9 H 0.1255 0.1034 -0.2755 0.120 Uiso 1 1 calc R . . C10 C 0.1222(4) 0.1311(3) -0.0688(6) 0.0756(17) Uani 1 1 d . . . H10 H 0.1200 0.0926 -0.0294 0.091 Uiso 1 1 calc R . . O3 O 0.2281(3) 0.16808(17) 0.3326(5) 0.0743(11) Uani 1 1 d . . . O4 O 0.0536(3) 0.18536(16) 0.3858(3) 0.0591(9) Uani 1 1 d . . . O5W O 0.2468(7) 0.0112(4) 0.5259(12) 0.171(4) Uani 0.75 1 d P . . O6W O 0.3232(9) 0.0537(5) 0.2760(16) 0.167(5) Uani 0.60 1 d P . . O7W O 0.511(3) 0.0238(16) 0.352(4) 0.175(13) Uiso 0.22 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 V 0.0558(6) 0.0512(6) 0.0373(5) 0.0029(3) 0.0140(4) -0.0030(3) O1 0.065(2) 0.0467(19) 0.085(2) 0.0003(17) 0.0315(19) 0.0016(15) O2 0.124(5) 0.117(4) 0.249(8) 0.127(5) 0.102(5) 0.056(3) P 0.0751(15) 0.0460(11) 0.136(2) 0.000 0.0538(15) 0.000 N1 0.061(3) 0.050(2) 0.059(2) -0.0038(19) 0.020(2) -0.0060(18) N2 0.053(2) 0.067(3) 0.045(2) -0.0062(18) 0.0182(18) -0.0104(18) C1 0.099(5) 0.059(3) 0.088(4) -0.019(3) 0.037(4) -0.020(3) C2 0.120(6) 0.063(4) 0.167(8) -0.039(5) 0.062(6) -0.030(4) C3 0.111(6) 0.060(4) 0.187(10) 0.031(6) 0.043(6) 0.002(4) C4 0.087(5) 0.075(4) 0.106(5) 0.025(4) 0.021(4) -0.011(3) C5 0.047(3) 0.067(3) 0.065(3) 0.023(3) 0.011(2) -0.004(2) C6 0.038(3) 0.092(4) 0.042(2) 0.012(2) 0.006(2) -0.011(2) C7 0.058(4) 0.130(5) 0.044(3) 0.019(3) 0.006(2) -0.021(3) C8 0.062(4) 0.204(9) 0.043(3) -0.001(5) 0.013(3) -0.035(5) C9 0.071(4) 0.176(9) 0.058(4) -0.045(5) 0.026(3) -0.032(5) C10 0.065(4) 0.103(5) 0.065(3) -0.024(3) 0.028(3) -0.008(3) O3 0.057(2) 0.085(3) 0.076(3) 0.0142(19) 0.007(2) -0.0071(18) O4 0.075(2) 0.073(2) 0.0331(17) -0.0002(14) 0.0184(16) -0.0077(17) O5W 0.163(9) 0.132(7) 0.203(11) -0.034(6) 0.010(8) -0.048(6) O6W 0.164(11) 0.125(8) 0.219(12) 0.032(8) 0.057(9) 0.085(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 V O3 1.606(4) . Y V O4 1.643(3) . Y V O1 1.915(3) . Y V N1 2.120(4) . Y V N2 2.201(4) . Y V O4 2.412(4) 2 Y O1 P 1.530(3) . Y O2 P 1.524(5) . Y P O2 1.524(5) 2 ? P O1 1.530(3) 2 ? N1 C1 1.342(7) . ? N1 C5 1.344(7) . ? N2 C10 1.328(6) . ? N2 C6 1.347(6) . ? C1 C2 1.405(9) . ? C2 C3 1.366(12) . ? C3 C4 1.372(12) . ? C4 C5 1.353(8) . ? C5 C6 1.463(8) . ? C6 C7 1.381(7) . ? C7 C8 1.374(12) . ? C8 C9 1.367(12) . ? C9 C10 1.368(9) . ? O4 V 2.412(4) 2 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 V O4 107.61(19) . . Y O3 V O1 100.80(18) . . Y O4 V O1 100.58(16) . . Y O3 V N1 92.91(18) . . Y O4 V N1 91.06(17) . . Y O1 V N1 158.29(18) . . Y O3 V N2 99.92(19) . . Y O4 V N2 149.24(18) . . Y O1 V N2 87.22(15) . . Y N1 V N2 73.80(16) . . Y O3 V O4 172.73(16) . 2 ? O4 V O4 77.33(15) . 2 ? O1 V O4 83.22(14) . 2 ? N1 V O4 81.54(14) . 2 ? N2 V O4 74.09(13) . 2 ? P O1 V 130.9(2) . . ? O2 P O2 110.9(6) 2 . ? O2 P O1 108.6(3) 2 . ? O2 P O1 108.6(3) . . ? O2 P O1 108.6(3) 2 2 ? O2 P O1 108.6(3) . 2 ? O1 P O1 111.6(3) . 2 ? C1 N1 C5 120.0(5) . . ? C1 N1 V 120.0(4) . . ? C5 N1 V 120.0(4) . . ? C10 N2 C6 120.2(5) . . ? C10 N2 V 123.5(4) . . ? C6 N2 V 116.3(3) . . ? N1 C1 C2 121.1(6) . . ? C3 C2 C1 117.6(7) . . ? C2 C3 C4 120.3(7) . . ? C5 C4 C3 120.2(7) . . ? N1 C5 C4 120.8(6) . . ? N1 C5 C6 114.2(4) . . ? C4 C5 C6 124.9(6) . . ? N2 C6 C7 120.2(6) . . ? N2 C6 C5 115.5(4) . . ? C7 C6 C5 124.3(6) . . ? C8 C7 C6 119.0(7) . . ? C9 C8 C7 120.1(6) . . ? C8 C9 C10 118.6(7) . . ? N2 C10 C9 121.9(7) . . ? V O4 V 99.95(14) . 2 ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.672 _refine_diff_density_min -0.241 _refine_diff_density_rms 0.120 #======================================================================= data_(I) _database_code_CSD 208664 #======================================================================= # 5. CHEMICAL DATA _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_iupac ? _chemical_formula_sum 'C40 H32 Cu4 N8 O29 P5 V4' _chemical_formula_weight 1701.55 _chemical_melting_point ? _chemical_compound_source ? #======================================================================= # 6. CRYSTAL DATA _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 -x,-y,-z _cell_length_a 7.4130(10) _cell_length_b 12.9922(5) _cell_length_c 14.9682(5) _cell_angle_alpha 87.80(10) _cell_angle_beta 78.85(10) _cell_angle_gamma 78.09(10) _cell_volume 1383.9(7) _cell_formula_units_Z 1 _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _cell_measurement_temperature ? _cell_special_details ; ? ; _exptl_crystal_density_diffrn 2.0420(11) _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_F_000 843 _exptl_absorpt_coefficient_mu 2.395 _exptl_crystal_description ? _exptl_crystal_size_max 0.7 _exptl_crystal_size_mid 0.6 _exptl_crystal_size_min 0.2 _exptl_crystal_size_rad ? _exptl_crystal_colour Blue _exptl_absorpt_correction_type None _exptl_absorpt_process_details ? _exptl_absorpt_correction_T_min 0.800 _exptl_absorpt_correction_T_max 1.000 #======================================================================= # 7. EXPERIMENTAL DATA _exptl_special_details ; ? ; _diffrn_ambient_temperature ? _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_source ? _diffrn_radiation_monochromator ? _diffrn_measurement_device_type ? _diffrn_detector_area_resol_mean ? _diffrn_measurement_method ? _diffrn_reflns_number 5851 _diffrn_reflns_theta_min 1.60 _diffrn_reflns_theta_max 27.50 _diffrn_reflns_theta_full ? _diffrn_measured_fraction_theta_max ? _diffrn_measured_fraction_theta_full ? _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.2500 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_reduction_process ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? #======================================================================= # 8. REFINEMENT DATA _refine_special_details ; ? ; _reflns_number_total 5852 _reflns_number_gt 1808 _reflns_threshold_expression I>2\s(I) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0682 _refine_ls_wR_factor_gt 0.0887 _refine_ls_R_factor_all 0.0682 _refine_ls_wR_factor_ref 0.0887 _refine_ls_goodness_of_fit_ref 0.95 _refine_ls_goodness_of_fit_gt 0.95 _refine_ls_restrained_S_gt ? _refine_ls_restrained_S_all ? _refine_ls_number_reflns 1808 _refine_ls_number_parameters 247 _refine_ls_number_restraints ? _refine_ls_number_constraints ? _refine_ls_weighting_scheme sigma _refine_ls_weighting_details w=1/\s^2^(I) _refine_ls_hydrogen_treatment ? _refine_ls_shift/su_max 0.0003 _refine_ls_shift/su_mean 0.0000 _refine_diff_density_max 1.25 _refine_diff_density_min -0.71 _refine_ls_extinction_method none _refine_ls_extinction_coef ? loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c C 0.003 0.002 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 2.31 20.843901 1.02 10.2075 1.5886 0.5687 0.865 51.651199 0.2156 H 0.000 0.000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 0.493002 10.5109 0.322912 26.1257 0.140191 3.14236 0.04081 57.799702 0.003038 N 0.006 0.003 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 12.2126 0.0057 3.1322 9.8933 2.0125 28.997499 1.1663 0.5826 -11.529 O 0.011 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.867 32.908901 0.2508 P 0.102 0.094 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 6.4345 1.9067 4.1791 27.157 1.78 0.526 1.4908 68.164497 1.1149 V 0.301 0.529 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 10.2971 6.8657 7.3511 0.4385 2.0703 26.893801 2.0571 102.477997 1.2199 Cu 0.320 1.265 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 13.338 3.5828 7.1676 0.247 5.6158 11.3966 1.6735 64.812599 1.191 _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement '(Jana2000; Petricek and Dusek, 2000)' _computing_molecular_graphics ? _computing_publication_material '(Jana2000; Petricek and Dusek, 2000)' #======================================================================= # 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_adp_type _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_symmetry_multiplicity _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu Uani 0.1733(2) 0.82761(11) 0.61353(11) 0.0345(7) 2 1 d . . . Cu2 Cu Uani 0.1950(2) 0.59122(13) 0.83923(11) 0.0425(7) 2 1 d . . . V1 V Uani 0.5730(3) 0.70325(15) 0.70646(14) 0.0256(9) 2 1 d . . . V2 V Uani 0.7652(3) 0.51538(16) 0.55945(14) 0.0278(9) 2 1 d . . . P1 P Uani 0.3007(4) 0.5787(2) 0.6253(2) 0.0194(12) 2 1 d . . . P2 P Uani 0.8868(4) 0.7912(2) 0.7890(2) 0.0220(12) 2 1 d . . . P3 P Uani 0.6894(7) 0.9850(4) 0.9126(4) 0.0275 2 0.5 d . . . O1 O Uani 0.4959(10) 0.6041(5) 0.6191(5) 0.020(3) 2 1 d . . . O2 O Uani 0.4558(13) 0.6572(6) 0.7929(6) 0.053(4) 2 1 d . . . O3 O Uani 0.4442(13) 0.8070(6) 0.6728(6) 0.050(4) 2 1 d . . . O4 O Uani 0.8030(10) 0.6309(5) 0.6253(5) 0.033(3) 2 1 d . . . O5 O Uani 0.7616(12) 0.4146(6) 0.6215(5) 0.046(4) 2 1 d . . . O6 O Uani 0 0.5 0.5 0.0313 1 1 d . . . O7 O Uani 0.1709(10) 0.6775(6) 0.6009(5) 0.0313 2 1 d . . . O8 O Uani 0.3233(10) 0.4945(6) 0.5526(5) 0.0313 2 1 d . . . O9 O Uani 0.2388(10) 0.5323(6) 0.7167(5) 0.0313 2 1 d . . . O10 O Uani 0.7790(9) 0.8667(5) 0.8706(5) 0.066(3) 2 1 d . . . O11 O Uani 0.7685(12) 0.7093(6) 0.7770(4) 0.066(3) 2 0.5 d . . . O11' O Uani 1.0535(14) 0.8369(7) 0.7357(6) 0.066(3) 2 0.5 d . . . O12 O Uani 1.0769(12) 0.7338(6) 0.8104(5) 0.066(3) 2 0.5 d . . . O12' O Uani 0.9619(15) 0.6812(7) 0.8266(5) 0.066(3) 2 0.5 d . . . O13 O Uani 0.9208(10) 0.8546(7) 0.6992(6) 0.066(3) 2 0.5 d . . . O13' O Uani 0.7511(12) 0.7813(8) 0.7247(6) 0.066(3) 2 0.5 d . . . O14 O Uani 0.679(2) 1.0651(7) 0.8342(7) 0.0845 2 0.5 d . . . O15 O Uani 0.4887(16) 0.9875(8) 0.9685(9) 0.0845 2 0.5 d . . . O16 O Uani 0.8147(16) 1.0136(8) 0.9752(9) 0.0845 2 0.5 d . . . O17 O Uani 0.243(3) 0.9644(15) 0.8399(15) 0.0845 2 0.5 d . . . N1 N Uani 0.1227(14) 0.9855(7) 0.6027(6) 0.031(3) 2 1 d . . . N2 N Uani 0.3436(14) 0.8383(7) 0.4931(6) 0.031(3) 2 1 d . . . C1 C Uani 0.0210(17) 1.0563(10) 0.6595(9) 0.0359(18) 2 1 d . . . H1 H Uiso -0.0361 1.0298 0.7144 0.05 2 1 d . . . C2 C Uani -0.0109(17) 1.1598(9) 0.6442(8) 0.0359(18) 2 1 d . . . H2 H Uiso -0.0915 1.2076 0.6843 0.05 2 1 d . . . C3 C Uani 0.0670(17) 1.1978(9) 0.5617(9) 0.0359(18) 2 1 d . . . H3 H Uiso 0.0464 1.2684 0.5478 0.05 2 1 d . . . C4 C Uani 0.1808(18) 1.1259(9) 0.4995(9) 0.0359(18) 2 1 d . . . H4 H Uiso 0.2465 1.1493 0.447 0.05 2 1 d . . . C5 C Uani 0.2166(17) 1.0200(9) 0.5167(8) 0.0359(18) 2 1 d . . . C6 C Uani 0.3317(17) 0.9362(9) 0.4581(9) 0.0359(18) 2 1 d . . . C7 C Uani 0.4341(17) 0.9535(9) 0.3733(9) 0.0359(18) 2 1 d . . . H7 H Uiso 0.4295 1.0211 0.3517 0.05 2 1 d . . . C8 C Uani 0.5560(17) 0.8701(9) 0.3219(9) 0.0359(18) 2 1 d . . . H8 H Uiso 0.6152 0.8823 0.2666 0.05 2 1 d . . . C9 C Uani 0.5584(17) 0.7736(9) 0.3593(9) 0.0359(18) 2 1 d . . . H9 H Uiso 0.632 0.7143 0.3257 0.05 2 1 d . . . C10 C Uani 0.4437(18) 0.7580(9) 0.4423(9) 0.0359(18) 2 1 d . . . H10 H Uiso 0.4433 0.6914 0.4614 0.05 2 1 d . . . N3 N Uani 0.3472(14) 0.4602(8) 0.8846(7) 0.040(3) 2 1 d . . . N4 N Uani 0.1338(14) 0.6169(8) 0.9753(7) 0.040(3) 2 1 d . . . C11 C Uani 0.453(2) 0.3868(11) 0.8322(9) 0.047(2) 2 1 d . . . H11 H Uiso 0.4828 0.3922 0.767 0.05 2 1 d . . . C12 C Uani 0.5417(18) 0.2959(10) 0.8670(9) 0.047(2) 2 1 d . . . H12 H Uiso 0.6136 0.2394 0.8235 0.05 2 1 d . . . C13 C Uani 0.5147(19) 0.2749(11) 0.9556(9) 0.047(2) 2 1 d . . . H13 H Uiso 0.5631 0.2121 0.9833 0.05 2 1 d . . . C14 C Uani 0.4001(19) 0.3558(11) 0.0101(9) 0.047(2) 2 1 d . . . H14 H Uiso 0.3745 0.346 1.0735 0.05 2 1 d . . . C15 C Uani 0.3164(19) 0.4497(11) 0.9749(9) 0.047(2) 2 1 d . . . C16 C Uani 0.1998(19) 0.5349(11) 0.0272(9) 0.047(2) 2 1 d . . . C17 C Uani 0.1528(19) 0.5358(11) 0.1204(9) 0.047(2) 2 1 d . . . H17 H Uiso 0.1956 0.4834 1.1569 0.05 2 1 d . . . C18 C Uani 0.0344(18) 0.6319(10) 0.1628(9) 0.047(2) 2 1 d . . . H18 H Uiso -0.0011 0.6334 1.2255 0.05 2 1 d . . . C19 C Uani -0.0248(18) 0.7133(10) 0.1125(9) 0.047(2) 2 1 d . . . H19 H Uiso -0.0973 0.7738 1.1387 0.05 2 1 d . . . C20 C Uani 0.0313(19) 0.7060(11) 0.0165(9) 0.047(2) 2 1 d . . . H20 H Uiso -0.0056 0.7648 0.9828 0.05 2 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_type_symbol _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Cu1 Cu 0.0311(11) 0.0218(8) 0.0455(12) -0.0084(7) 0.0087(9) 0.0012(8) Cu2 Cu 0.0301(11) 0.0703(12) 0.0217(10) 0.0018(9) -0.0061(9) 0.0096(9) V1 V 0.0200(14) 0.0339(13) 0.0234(14) -0.0054(10) -0.0059(11) 0.0010(11) V2 V 0.0278(15) 0.0346(13) 0.0229(14) -0.0079(10) -0.0068(12) -0.0050(11) P1 P 0.016(2) 0.0260(18) 0.018(2) -0.0067(14) -0.0046(16) 0.0079(15) P2 P 0.015(2) 0.0308(19) 0.021(2) -0.0085(15) -0.0011(17) -0.0043(16) P3 P 0.026978 0.030355 0.023174 -0.007363 0.003028 -0.004952 O1 O 0.023(5) 0.025(4) 0.015(4) -0.007(3) -0.007(4) -0.001(3) O2 O 0.070(8) 0.038(5) 0.053(7) -0.009(5) -0.021(6) 0.004(5) O3 O 0.068(7) 0.046(6) 0.039(6) -0.020(5) -0.004(6) -0.008(5) O4 O 0.025(5) 0.034(5) 0.037(5) -0.009(4) 0.006(5) -0.013(4) O5 O 0.059(7) 0.051(6) 0.032(6) -0.003(5) -0.025(5) -0.001(5) O6 O 0.024606 0.039897 0.031501 -0.009119 -0.006584 -0.004841 O7 O 0.024606 0.039897 0.031501 -0.009119 -0.006584 -0.004841 O8 O 0.024606 0.039897 0.031501 -0.009119 -0.006584 -0.004841 O9 O 0.024606 0.039897 0.031501 -0.009119 -0.006584 -0.004841 O10 O 0.056(5) 0.062(4) 0.080(5) -0.021(3) -0.004(4) -0.010(4) O11 O 0.056(5) 0.062(4) 0.080(5) -0.021(3) -0.004(4) -0.010(4) O11' O 0.056(5) 0.062(4) 0.080(5) -0.021(3) -0.004(4) -0.010(4) O12 O 0.056(5) 0.062(4) 0.080(5) -0.021(3) -0.004(4) -0.010(4) O12' O 0.056(5) 0.062(4) 0.080(5) -0.021(3) -0.004(4) -0.010(4) O13 O 0.056(5) 0.062(4) 0.080(5) -0.021(3) -0.004(4) -0.010(4) O13' O 0.056(5) 0.062(4) 0.080(5) -0.021(3) -0.004(4) -0.010(4) O14 O 0.070429 0.071101 0.105338 -0.010004 -0.00133 -0.020339 O15 O 0.070429 0.071101 0.105338 -0.010004 -0.00133 -0.020339 O16 O 0.070429 0.071101 0.105338 -0.010004 -0.00133 -0.020339 O17 O 0.070429 0.071101 0.105338 -0.010004 -0.00133 -0.020339 N1 N 0.049(5) 0.012(4) 0.031(5) -0.002(3) -0.009(4) 0.005(3) N2 N 0.049(5) 0.012(4) 0.031(5) -0.002(3) -0.009(4) 0.005(3) C1 C 0.032(3) 0.037(2) 0.041(3) -0.012(2) -0.008(2) 0.004(2) C2 C 0.032(3) 0.037(2) 0.041(3) -0.012(2) -0.008(2) 0.004(2) C3 C 0.032(3) 0.037(2) 0.041(3) -0.012(2) -0.008(2) 0.004(2) C4 C 0.032(3) 0.037(2) 0.041(3) -0.012(2) -0.008(2) 0.004(2) C5 C 0.032(3) 0.037(2) 0.041(3) -0.012(2) -0.008(2) 0.004(2) C6 C 0.032(3) 0.037(2) 0.041(3) -0.012(2) -0.008(2) 0.004(2) C7 C 0.032(3) 0.037(2) 0.041(3) -0.012(2) -0.008(2) 0.004(2) C8 C 0.032(3) 0.037(2) 0.041(3) -0.012(2) -0.008(2) 0.004(2) C9 C 0.032(3) 0.037(2) 0.041(3) -0.012(2) -0.008(2) 0.004(2) C10 C 0.032(3) 0.037(2) 0.041(3) -0.012(2) -0.008(2) 0.004(2) N3 N 0.038(6) 0.057(5) 0.026(5) -0.012(4) -0.005(4) 0.006(4) N4 N 0.038(6) 0.057(5) 0.026(5) -0.012(4) -0.005(4) 0.006(4) C11 C 0.047(3) 0.062(3) 0.043(3) -0.026(2) -0.023(3) 0.013(3) C12 C 0.047(3) 0.062(3) 0.043(3) -0.026(2) -0.023(3) 0.013(3) C13 C 0.047(3) 0.062(3) 0.043(3) -0.026(2) -0.023(3) 0.013(3) C14 C 0.047(3) 0.062(3) 0.043(3) -0.026(2) -0.023(3) 0.013(3) C15 C 0.047(3) 0.062(3) 0.043(3) -0.026(2) -0.023(3) 0.013(3) C16 C 0.047(3) 0.062(3) 0.043(3) -0.026(2) -0.023(3) 0.013(3) C17 C 0.047(3) 0.062(3) 0.043(3) -0.026(2) -0.023(3) 0.013(3) C18 C 0.047(3) 0.062(3) 0.043(3) -0.026(2) -0.023(3) 0.013(3) C19 C 0.047(3) 0.062(3) 0.043(3) -0.026(2) -0.023(3) 0.013(3) C20 C 0.047(3) 0.062(3) 0.043(3) -0.026(2) -0.023(3) 0.013(3) #======================================================================= # 10. MOLECULAR GEOMETRY loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Cu1 O3 . . 2.311(10) yes Cu1 O7 . . 1.971(8) yes Cu1 O11' . 1_455 1.868(9) yes Cu1 O13 . 1_455 2.026(7) yes Cu1 N1 . . 2.014(8) yes Cu1 N2 . . 2.009(9) yes Cu2 O2 . . 2.252(10) yes Cu2 O9 . . 1.957(8) yes Cu2 O12 . 1_455 1.949(8) yes Cu2 O12' . 1_455 1.914(10) yes Cu2 N3 . . 2.011(10) yes Cu2 N4 . . 2.024(10) yes V1 O1 . . 2.102(8) yes V1 O2 . . 1.584(8) yes V1 O3 . . 1.608(8) yes V1 O4 . . 1.972(7) yes V1 O11 . . 1.966(9) yes V1 O13' . . 1.887(11) yes V2 O1 . . 2.133(6) yes V2 O4 . . 1.923(8) yes V2 O5 . . 1.577(8) yes V2 O6 . 1_655 1.770(2) yes V2 O8 . 2_666 1.934(9) yes P1 O1 . . 1.535(8) yes P1 O7 . . 1.516(8) yes P1 O8 . . 1.534(8) yes P1 O9 . . 1.501(8) yes P2 O10 . . 1.576(7) yes P2 O11 . . 1.547(10) yes P2 O11' . . 1.550(11) yes P2 O12 . . 1.538(9) yes P2 O12' . . 1.549(9) yes P2 O13 . . 1.556(9) yes P2 O13' . . 1.547(11) yes P3 O10 . . 1.640(8) yes P3 O14 . . 1.541(11) yes P3 O15 . . 1.554(12) yes P3 O15 . 2_677 1.996(13) yes P3 O16 . . 1.544(15) yes N1 C1 . . 1.290(14) yes N1 C5 . . 1.442(15) yes N2 C6 . . 1.349(15) yes N2 C10 . . 1.319(14) yes C1 H1 . . 0.937(12) yes C1 C2 . . 1.334(17) yes C2 H2 . . 0.917(11) yes C2 C3 . . 1.377(17) yes C3 H3 . . 0.920(12) yes C3 C4 . . 1.375(16) yes C4 H4 . . 0.918(12) yes C4 C5 . . 1.371(17) yes C5 C6 . . 1.443(16) yes C6 C7 . . 1.384(17) yes C7 H7 . . 0.921(12) yes C7 C8 . . 1.405(15) yes C8 H8 . . 0.883(12) yes C8 C9 . . 1.351(17) yes C9 H9 . . 0.946(11) yes C9 C10 . . 1.398(17) yes C10 H10 . . 0.902(12) yes N3 C11 . . 1.284(16) yes N3 C15 . . 1.332(17) yes N4 C16 . 1_556 1.360(17) yes N4 C20 . 1_556 1.344(16) yes C11 H11 . . 0.962(14) yes C11 C12 . . 1.366(19) yes C12 H12 . . 0.993(12) yes C12 C13 . . 1.328(19) yes C13 H13 . . 0.937(14) yes C13 C14 . 1_556 1.386(18) yes C14 H14 . 1_554 0.941(13) yes C14 C15 . 1_554 1.384(19) yes C15 C16 . 1_556 1.413(18) yes C16 C17 . . 1.370(19) yes C16 C20 . . 2.331(18) yes C17 H17 . 1_554 0.901(13) yes C17 C18 . . 1.458(17) yes C18 H18 . 1_554 0.925(13) yes C18 C19 . . 1.323(18) yes C19 H19 . 1_554 0.911(12) yes C19 C20 . . 1.417(19) yes C20 H20 . 1_554 0.923(14) yes loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag O3 Cu1 O7 . . . 98.0(3) yes O3 Cu1 O11' . . 1_455 84.0(4) yes O3 Cu1 O13 . . 1_455 119.3(3) yes O3 Cu1 N1 . . . 97.8(4) yes O3 Cu1 N2 . . . 84.7(4) yes O7 Cu1 O11' . . 1_455 95.0(4) yes O7 Cu1 O13 . . 1_455 92.5(3) yes O7 Cu1 N1 . . . 163.7(4) yes O7 Cu1 N2 . . . 95.3(3) yes O11' Cu1 O13 1_455 . 1_455 35.4(4) yes O11' Cu1 N1 1_455 . . 90.9(4) yes O11' Cu1 N2 1_455 . . 165.7(5) yes O13 Cu1 N1 1_455 . . 83.5(4) yes O13 Cu1 N2 1_455 . . 153.4(4) yes N1 Cu1 N2 . . . 81.8(3) yes O2 Cu2 O9 . . . 87.1(3) yes O2 Cu2 O12 . . 1_455 81.2(3) yes O2 Cu2 O12' . . 1_455 116.5(4) yes O2 Cu2 N3 . . . 90.7(4) yes O2 Cu2 N4 . . . 103.6(4) yes O9 Cu2 O12 . . 1_455 97.3(3) yes O9 Cu2 O12' . . 1_455 93.5(3) yes O9 Cu2 N3 . . . 91.8(4) yes O9 Cu2 N4 . . . 165.7(4) yes O12 Cu2 O12' 1_455 . 1_455 35.7(4) yes O12 Cu2 N3 1_455 . . 167.5(5) yes O12 Cu2 N4 1_455 . . 93.8(4) yes O12' Cu2 N3 1_455 . . 152.4(4) yes O12' Cu2 N4 1_455 . . 90.2(4) yes N3 Cu2 N4 . . . 78.7(4) yes O1 V1 O2 . . . 91.4(4) yes O1 V1 O3 . . . 93.1(4) yes O1 V1 O4 . . . 71.8(3) yes O1 V1 O11 . . . 141.7(3) yes O1 V1 O13' . . . 146.8(3) yes O2 V1 O3 . . . 109.0(4) yes O2 V1 O4 . . . 127.9(4) yes O2 V1 O11 . . . 89.4(4) yes O2 V1 O13' . . . 118.3(5) yes O3 V1 O4 . . . 120.5(4) yes O3 V1 O11 . . . 122.6(4) yes O3 V1 O13' . . . 90.9(5) yes O4 V1 O11 . . . 77.7(3) yes O4 V1 O13' . . . 77.7(4) yes O11 V1 O13' . . . 36.2(4) yes O1 V2 O4 . . . 72.1(3) yes O1 V2 O5 . . . 97.9(3) yes O1 V2 O6 . . 1_655 154.4(2) yes O1 V2 O8 . . 2_666 89.8(3) yes O4 V2 O5 . . . 111.1(4) yes O4 V2 O6 . . 1_655 89.0(2) yes O4 V2 O8 . . 2_666 133.5(3) yes O5 V2 O6 . . 1_655 105.1(3) yes O5 V2 O8 . . 2_666 113.7(4) yes O6 V2 O8 1_655 . 2_666 91.3(2) yes O1 P1 O7 . . . 107.8(4) yes O1 P1 O8 . . . 106.0(4) yes O1 P1 O9 . . . 110.1(5) yes O7 P1 O8 . . . 108.9(5) yes O7 P1 O9 . . . 115.5(4) yes O8 P1 O9 . . . 108.1(5) yes O10 P2 O11 . . . 109.2(4) yes O10 P2 O11' . . . 109.4(5) yes O10 P2 O12 . . . 109.2(4) yes O10 P2 O12' . . . 109.5(4) yes O10 P2 O13 . . . 110.6(4) yes O10 P2 O13' . . . 109.5(4) yes O11 P2 O11' . . . 139.7(5) yes O11 P2 O12 . . . 109.2(5) yes O11 P2 O12' . . . 66.9(5) yes O11 P2 O13 . . . 109.2(5) yes O11 P2 O13' . . . 45.6(5) yes O11' P2 O12 . . . 67.4(5) yes O11' P2 O12' . . . 109.5(5) yes O11' P2 O13 . . . 45.2(5) yes O11' P2 O13' . . . 109.5(5) yes O12 P2 O12' . . . 45.1(6) yes O12 P2 O13 . . . 109.3(4) yes O12 P2 O13' . . . 139.5(5) yes O12' P2 O13 . . . 138.3(4) yes O12' P2 O13' . . . 109.5(6) yes O13 P2 O13' . . . 66.8(5) yes O10 P3 O14 . . . 109.5(5) yes O10 P3 O15 . . . 109.5(6) yes O10 P3 O15 . . 2_677 123.4(5) yes O10 P3 O16 . . . 109.5(5) yes O14 P3 O15 . . . 109.5(7) yes O14 P3 O15 . . 2_677 120.9(6) yes O14 P3 O16 . . . 109.5(7) yes O15 P3 O15 . . 2_677 31.9(6) yes O15 P3 O16 . . . 109.5(7) yes O15 P3 O15 2_677 . . 31.9(6) yes O15 P3 O16 2_677 . . 77.7(6) yes Cu1 N1 C1 . . . 129.9(8) yes C1 N1 C5 . . . 118.0(9) yes Cu1 N2 C6 . . . 115.1(7) yes C6 N2 C10 . . . 118.8(10) yes N1 C1 H1 . . . 114.6(12) yes N1 C1 C2 . . . 125.3(11) yes H1 C1 C2 . . . 120.0(11) yes N1 C2 C1 . . . 26.8(6) yes C1 C2 H2 . . . 123.1(12) yes C1 C2 C3 . . . 119.7(11) yes H2 C2 C3 . . . 117.0(11) yes C2 C3 C4 . . . 117.4(11) yes H3 C3 C4 . . . 120.0(12) yes C3 C4 H4 . . . 119.4(12) yes C3 C4 C5 . . . 122.5(11) yes H4 C4 C5 . . . 117.7(11) yes N1 C5 C4 . . . 116.9(10) yes N1 C5 C6 . . . 114.6(10) yes C4 C5 C6 . . . 128.4(11) yes N2 C6 C5 . . . 115.9(10) yes N2 C6 C7 . . . 120.8(10) yes C5 C6 C7 . . . 123.2(11) yes C6 C7 H7 . . . 119.9(11) yes C6 C7 C8 . . . 121.1(11) yes H7 C7 C8 . . . 118.9(12) yes C7 C8 C9 . . . 115.4(11) yes H8 C8 C9 . . . 124.6(12) yes C8 C9 H9 . . . 118.8(12) yes C8 C9 C10 . . . 122.1(10) yes N2 C10 C9 . . . 121.1(11) yes N2 C10 H10 . . . 120.7(12) yes C9 C10 H10 . . . 118.1(11) yes Cu2 N3 C11 . . . 123.7(9) yes Cu2 N3 C15 . . . 114.6(8) yes C11 N3 C15 . . . 121.4(11) yes Cu2 N4 C16 . . 1_556 115.6(8) yes Cu2 N4 C20 . . 1_556 125.3(9) yes C16 N4 C20 1_556 . 1_556 119.1(11) yes N3 C11 H11 . . . 124.1(13) yes N3 C11 C12 . . . 121.2(13) yes H11 C11 C12 . . . 114.6(12) yes C11 C12 H12 . . . 117.9(13) yes C11 C12 C13 . . . 122.5(12) yes H12 C12 C13 . . . 118.9(13) yes C12 C13 H13 . . . 126.7(13) yes C12 C13 C14 . . 1_556 114.6(12) yes H13 C13 H14 . . . 94.6(9) yes C13 C14 H14 1_554 . 1_554 119.0(13) yes C13 C14 C15 1_554 . 1_554 122.7(12) yes H14 C14 C15 1_554 . 1_554 118.3(12) yes N3 C15 C14 . . 1_556 117.4(11) yes N3 C15 C16 . . 1_556 117.5(12) yes C14 C15 C16 1_556 . 1_556 125.0(12) yes N4 C16 C15 1_554 . 1_554 112.9(12) yes N4 C16 C17 1_554 . . 122.5(11) yes C15 C16 C17 1_554 . . 124.6(12) yes C16 C17 H17 . . 1_554 124.9(13) yes C16 C17 C18 . . . 116.8(12) yes H17 C17 C18 1_554 . . 118.1(13) yes C17 C18 H18 . . 1_554 118.0(13) yes C17 C18 C19 . . . 120.8(12) yes H18 C18 C19 1_554 . . 121.2(12) yes C18 C19 H19 . . 1_554 121.0(13) yes C18 C19 C20 . . . 118.8(11) yes H19 C19 C20 1_554 . . 120.1(13) yes N4 C20 C19 1_554 . . 121.8(12) yes N4 C20 H20 1_554 . 1_554 120.7(13) yes C19 C20 H20 . . 1_554 117.5(12) yes #=======================================================================