# Copyright The Royal Society of Chemistry, 1999 # CCDC Number: 186/1329 data_niv _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C4 H13 N3 Ni O6 V2' _chemical_formula_weight 359.76 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'V' 'V' 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ni' 'Ni' 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.37700(10) _cell_length_b 8.09300(10) _cell_length_c 10.23500(10) _cell_angle_alpha 101.8070(10) _cell_angle_beta 102.8010(10) _cell_angle_gamma 98.8310(10) _cell_volume 570.458(12) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4094 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'trunk' _exptl_crystal_colour 'brown' _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.094 _exptl_crystal_density_method ? _exptl_crystal_F_000 360 _exptl_absorpt_coefficient_mu 3.253 _exptl_absorpt_correction_type 'empirical' _exptl_absorpt_correction_T_min 0.789 _exptl_absorpt_correction_T_max 0.956 _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 'Siemens Smart-CCD diffractometer' _diffrn_measurement_method '\w scans' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5431 _diffrn_reflns_av_R_equivalents 0.0348 _diffrn_reflns_av_sigmaI/netI 0.0400 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.11 _diffrn_reflns_theta_max 27.97 _reflns_number_total 2460 _reflns_number_observed 2104 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'SMART (Siemens, 1994)' _computing_cell_refinement 'SMART (Siemens, 1994)' _computing_data_reduction 'SAINT (Siemens, 1995)' _computing_structure_solution 'SHELXTL (Sheldrick, 1994)' _computing_structure_refinement 'SHELXTL (Sheldrick, 1994)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 1994)' _computing_publication_material 'SHELXTL (Sheldrick, 1994)' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0376P)^2^+0.3103P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0075(16) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 2460 _refine_ls_number_parameters 198 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0380 _refine_ls_R_factor_obs 0.0290 _refine_ls_wR_factor_all 0.0748 _refine_ls_wR_factor_obs 0.0696 _refine_ls_goodness_of_fit_all 1.049 _refine_ls_goodness_of_fit_obs 1.063 _refine_ls_restrained_S_all 1.049 _refine_ls_restrained_S_obs 1.063 _refine_ls_shift/esd_max 0.000 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Ni Ni 0.41875(5) -0.63763(4) 0.35591(3) 0.01584(12) Uani 1 d . . V1 V 0.81682(6) -0.85029(6) 0.38879(5) 0.02016(14) Uani 1 d . . V2 V 0.73513(6) -1.25950(6) 0.37905(5) 0.01742(13) Uani 1 d . . O1 O 0.6774(3) -0.7110(3) 0.3877(2) 0.0274(5) Uani 1 d . . O2 O 0.6849(3) -1.0475(3) 0.4055(3) 0.0350(5) Uani 1 d . . O3 O 0.8792(3) -0.8850(3) 0.2454(3) 0.0395(6) Uani 1 d . . O4 O 0.9765(3) -1.2387(3) 0.4693(3) 0.0376(6) Uani 1 d . . O5 O 0.5805(3) -1.3839(2) 0.4371(2) 0.0179(4) Uani 1 d . . O6 O 0.7062(4) -1.3418(3) 0.2177(2) 0.0401(6) Uani 1 d . . N1 N 0.1761(4) -0.5381(4) 0.3173(3) 0.0234(5) Uani 1 d . . N2 N 0.3979(4) -0.6488(3) 0.1490(3) 0.0255(5) Uani 1 d . . N3 N 0.2973(4) -0.9023(3) 0.2812(3) 0.0262(5) Uani 1 d . . C1 C 0.1837(5) -0.4570(5) 0.2025(4) 0.0352(8) Uani 1 d . . C2 C 0.2308(6) -0.5824(7) 0.0911(4) 0.0456(10) Uani 1 d . . C3 C 0.3978(6) -0.8276(5) 0.0817(4) 0.0386(8) Uani 1 d . . C4 C 0.2668(6) -0.9514(5) 0.1301(4) 0.0452(9) Uani 1 d . . H12 H 0.0630(54) -0.4218(48) 0.1638(39) 0.039(10) Uiso 1 d . . H1B H 0.1729(49) -0.4665(47) 0.3851(38) 0.026(9) Uiso 1 d . . H2A H 0.4921(51) -0.5839(46) 0.1505(36) 0.025(9) Uiso 1 d . . H3B H 0.3727(59) -0.9607(53) 0.3213(43) 0.046(12) Uiso 1 d . . H32 H 0.5284(57) -0.8414(49) 0.1062(40) 0.041(10) Uiso 1 d . . H42 H 0.2799(54) -1.0584(54) 0.0956(41) 0.043(11) Uiso 1 d . . H22 H 0.2497(60) -0.5350(56) 0.0163(47) 0.052(12) Uiso 1 d . . H3A H 0.2003(56) -0.9259(48) 0.3037(39) 0.033(10) Uiso 1 d . . H21 H 0.1170(74) -0.6769(66) 0.0526(52) 0.070(15) Uiso 1 d . . H11 H 0.2977(60) -0.3532(55) 0.2360(44) 0.050(12) Uiso 1 d . . H41 H 0.1280(82) -0.9511(72) 0.0783(59) 0.097(19) Uiso 1 d . . H1A H 0.0596(72) -0.6192(63) 0.2901(51) 0.071(15) Uiso 1 d . . H31 H 0.3562(53) -0.8496(49) -0.0150(41) 0.039(10) Uiso 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 Ni 0.0145(2) 0.0160(2) 0.0154(2) 0.00253(13) 0.00231(12) 0.00254(13) V1 0.0132(2) 0.0170(2) 0.0318(3) 0.0070(2) 0.0075(2) 0.0039(2) V2 0.0148(2) 0.0170(2) 0.0192(2) 0.0049(2) 0.0036(2) 0.0005(2) O1 0.0212(10) 0.0210(10) 0.0392(12) 0.0066(9) 0.0049(9) 0.0076(8) O2 0.0307(12) 0.0213(11) 0.059(2) 0.0165(11) 0.0173(11) 0.0068(9) O3 0.0351(13) 0.0398(14) 0.0426(14) 0.0011(11) 0.0215(11) 0.0010(11) O4 0.0169(10) 0.0399(14) 0.0504(15) 0.0119(11) -0.0011(10) 0.0030(10) O5 0.0186(9) 0.0156(9) 0.0183(9) 0.0037(7) 0.0042(7) 0.0011(7) O6 0.0469(14) 0.0430(14) 0.0230(11) 0.0023(10) 0.0139(10) -0.0112(11) N1 0.0212(13) 0.0274(14) 0.0224(13) 0.0053(11) 0.0067(10) 0.0072(11) N2 0.0238(13) 0.0295(14) 0.0206(13) 0.0021(11) 0.0062(10) 0.0034(11) N3 0.0212(13) 0.0207(12) 0.0331(14) 0.0022(11) 0.0087(11) -0.0026(10) C1 0.036(2) 0.045(2) 0.033(2) 0.021(2) 0.0078(14) 0.021(2) C2 0.044(2) 0.079(3) 0.023(2) 0.020(2) 0.007(2) 0.032(2) C3 0.046(2) 0.042(2) 0.024(2) -0.0030(15) 0.0107(15) 0.010(2) C4 0.057(2) 0.028(2) 0.035(2) -0.012(2) 0.010(2) -0.005(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 Ni O1 2.062(2) . ? Ni N1 2.066(2) . ? Ni N2 2.071(3) . ? Ni O5 2.088(2) 2_636 ? Ni N3 2.101(3) . ? Ni O5 2.108(2) 1_565 ? V1 O3 1.617(2) . ? V1 O1 1.639(2) . ? V1 O4 1.791(2) 2_736 ? V1 O2 1.798(2) . ? V2 O6 1.602(2) . ? V2 O5 1.692(2) . ? V2 O4 1.780(2) . ? V2 O2 1.790(2) . ? O4 V1 1.791(2) 2_736 ? O5 Ni 2.088(2) 2_636 ? O5 Ni 2.108(2) 1_545 ? N1 C1 1.466(4) . ? N2 C3 1.469(4) . ? N2 C2 1.473(4) . ? N3 C4 1.472(5) . ? C1 C2 1.503(5) . ? C3 C4 1.517(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Ni N1 172.86(10) . . ? O1 Ni N2 93.49(9) . . ? N1 Ni N2 82.99(10) . . ? O1 Ni O5 91.39(8) . 2_636 ? N1 Ni O5 92.06(9) . 2_636 ? N2 Ni O5 175.04(8) . 2_636 ? O1 Ni N3 86.08(10) . . ? N1 Ni N3 99.63(11) . . ? N2 Ni N3 83.42(11) . . ? O5 Ni N3 97.78(9) 2_636 . ? O1 Ni O5 85.23(8) . 1_565 ? N1 Ni O5 89.07(9) . 1_565 ? N2 Ni O5 97.52(9) . 1_565 ? O5 Ni O5 82.02(8) 2_636 1_565 ? N3 Ni O5 171.29(9) . 1_565 ? O3 V1 O1 109.69(12) . . ? O3 V1 O4 109.57(12) . 2_736 ? O1 V1 O4 108.31(11) . 2_736 ? O3 V1 O2 109.76(12) . . ? O1 V1 O2 107.61(10) . . ? O4 V1 O2 111.86(11) 2_736 . ? O6 V2 O5 108.64(11) . . ? O6 V2 O4 109.50(13) . . ? O5 V2 O4 113.06(10) . . ? O6 V2 O2 110.38(13) . . ? O5 V2 O2 107.99(10) . . ? O4 V2 O2 107.25(11) . . ? V1 O1 Ni 154.79(13) . . ? V2 O2 V1 129.92(13) . . ? V2 O4 V1 154.2(2) . 2_736 ? V2 O5 Ni 125.65(10) . 2_636 ? V2 O5 Ni 132.65(10) . 1_545 ? Ni O5 Ni 97.98(8) 2_636 1_545 ? C1 N1 Ni 106.3(2) . . ? C3 N2 C2 115.5(3) . . ? C3 N2 Ni 107.0(2) . . ? C2 N2 Ni 109.4(2) . . ? C4 N3 Ni 109.3(2) . . ? N1 C1 C2 108.0(3) . . ? N2 C2 C1 110.7(3) . . ? N2 C3 C4 109.8(3) . . ? N3 C4 C3 111.7(3) . . ? _refine_diff_density_max 0.410 _refine_diff_density_min -0.395 _refine_diff_density_rms 0.095 #=END data_cuv _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C4 H15 Cu N3 O7 V2' _chemical_formula_weight 382.61 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'V' 'V' 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cu' 'Cu' 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 8.0144(3) _cell_length_b 9.7028(4) _cell_length_c 16.2300(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1262.08(9) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3674 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'needle' _exptl_crystal_colour 'black' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.014 _exptl_crystal_density_method ? _exptl_crystal_F_000 764 _exptl_absorpt_coefficient_mu 3.145 _exptl_absorpt_correction_type 'empirical' _exptl_absorpt_correction_T_min 0.585 _exptl_absorpt_correction_T_max 0.879 _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 'Siemens Smart-CCD diffractometer' _diffrn_measurement_method '\w scan' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7919 _diffrn_reflns_av_R_equivalents 0.0475 _diffrn_reflns_av_sigmaI/netI 0.0678 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.45 _diffrn_reflns_theta_max 28.84 _reflns_number_total 3042 _reflns_number_observed 2340 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'SMART (Siemens, 1994)' _computing_cell_refinement 'SMART (Siemens, 1994)' _computing_data_reduction 'SAINT (Siemens, 1995)' _computing_structure_solution 'SHELXTL (Sheldrick, 1994)' _computing_structure_refinement 'SHELXTL (Sheldrick, 1994)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 1994)' _computing_publication_material 'SHELXTL (Sheldrick, 1994)' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0277P)^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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.03(2) _refine_ls_number_reflns 3042 _refine_ls_number_parameters 214 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0626 _refine_ls_R_factor_obs 0.0369 _refine_ls_wR_factor_all 0.0737 _refine_ls_wR_factor_obs 0.0649 _refine_ls_goodness_of_fit_all 0.987 _refine_ls_goodness_of_fit_obs 1.002 _refine_ls_restrained_S_all 0.987 _refine_ls_restrained_S_obs 1.002 _refine_ls_shift/esd_max 0.000 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Cu Cu 0.91373(7) 0.01461(5) 0.31751(3) 0.02412(14) Uani 1 d . . V1 V 0.88772(9) -0.31690(7) 0.36286(4) 0.0201(2) Uani 1 d . . V2 V 0.59983(10) -0.15972(8) 0.45197(4) 0.0243(2) Uani 1 d . . O1 O 0.9169(4) -0.1845(3) 0.2975(2) 0.0248(6) Uani 1 d . . O2 O 0.9202(4) 0.5428(3) 0.3108(2) 0.0354(8) Uani 1 d . . O3 O 0.6783(4) -0.3179(3) 0.4031(2) 0.0332(8) Uani 1 d . . O4 O 0.5306(4) 0.8028(4) 0.5543(2) 0.0418(9) Uani 1 d . . O5 O 0.7532(4) -0.0480(3) 0.4534(2) 0.0330(8) Uani 1 d . . O6 O 0.4527(4) -0.0979(4) 0.3938(2) 0.0421(9) Uani 1 d . . N1 N 1.1132(5) 0.0143(4) 0.3913(3) 0.0322(10) Uani 1 d . . N2 N 0.9033(5) 0.2156(4) 0.3438(2) 0.0281(9) Uani 1 d . . N3 N 0.6876(5) 0.0438(5) 0.2672(3) 0.0314(10) Uani 1 d . . C1 C 1.1616(7) 0.1575(6) 0.4107(4) 0.0436(14) Uani 1 d . . C2 C 1.0022(7) 0.2403(6) 0.4187(4) 0.0371(13) Uani 1 d . . C3 C 0.7246(6) 0.2540(6) 0.3463(4) 0.0382(13) Uani 1 d . . C4 C 0.6462(7) 0.1927(6) 0.2703(4) 0.0443(14) Uani 1 d . . OW O 0.5755(6) 0.9728(4) 0.0978(3) 0.0465(10) Uani 1 d . . H1 H 1.1780(62) -0.0274(55) 0.3807(32) 0.035(18) Uiso 1 d . . H2 H 1.0498(122) -0.0425(108) 0.4485(54) 0.173(41) Uiso 1 d . . H3 H 1.2233(70) 0.1651(57) 0.4723(33) 0.063(18) Uiso 1 d . . H4 H 1.2350(52) 0.2036(49) 0.3651(28) 0.033(13) Uiso 1 d . . H5 H 1.0291(57) 0.3264(62) 0.4285(29) 0.038(15) Uiso 1 d . . H6 H 0.9330(67) 0.2236(55) 0.4658(31) 0.051(17) Uiso 1 d . . H7 H 0.9542(58) 0.2430(55) 0.3080(31) 0.035(17) Uiso 1 d . . H8 H 0.6972(61) 0.3565(55) 0.3478(28) 0.041(14) Uiso 1 d . . H9 H 0.6759(51) 0.2098(50) 0.3986(28) 0.028(13) Uiso 1 d . . H10 H 0.6869(63) 0.2347(54) 0.2301(31) 0.039(16) Uiso 1 d . . H11 H 0.5183(66) 0.2036(69) 0.2689(37) 0.069(19) Uiso 1 d . . H12 H 0.6244(66) -0.0044(57) 0.2953(34) 0.055(18) Uiso 1 d . . H13 H 0.6746(54) 0.0044(49) 0.2187(29) 0.024(13) Uiso 1 d . . H1W H 0.5134(60) 1.0246(56) 0.1054(32) 0.026(17) Uiso 1 d . . H2W H 0.6532(78) 1.0035(69) 0.0633(36) 0.072(22) Uiso 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 0.0269(3) 0.0186(3) 0.0268(3) -0.0009(2) -0.0019(3) 0.0023(2) V1 0.0224(4) 0.0193(4) 0.0187(3) 0.0010(3) 0.0005(3) 0.0017(3) V2 0.0201(4) 0.0285(4) 0.0243(4) 0.0009(3) 0.0036(4) -0.0006(4) O1 0.035(2) 0.0201(15) 0.0195(14) 0.0016(12) 0.0011(14) -0.001(2) O2 0.051(2) 0.019(2) 0.036(2) -0.0040(14) 0.010(2) 0.000(2) O3 0.027(2) 0.030(2) 0.042(2) -0.005(2) 0.007(2) -0.002(2) O4 0.038(2) 0.052(3) 0.035(2) 0.006(2) 0.014(2) -0.001(2) O5 0.031(2) 0.035(2) 0.033(2) -0.001(2) 0.003(2) -0.011(2) O6 0.027(2) 0.053(2) 0.046(2) 0.001(2) -0.006(2) 0.008(2) N1 0.025(2) 0.029(2) 0.042(3) -0.005(2) -0.004(2) 0.005(2) N2 0.030(2) 0.027(2) 0.027(2) 0.002(2) 0.011(2) 0.000(2) N3 0.035(2) 0.036(3) 0.023(2) 0.005(2) -0.005(2) -0.002(2) C1 0.036(3) 0.041(3) 0.054(4) -0.013(3) -0.009(3) -0.007(3) C2 0.049(3) 0.027(3) 0.036(3) -0.010(2) 0.001(3) -0.003(2) C3 0.037(3) 0.026(3) 0.052(4) 0.002(2) 0.008(3) 0.007(2) C4 0.038(3) 0.037(3) 0.058(4) 0.020(3) -0.001(3) 0.014(3) OW 0.044(2) 0.046(2) 0.049(2) 0.004(2) 0.010(2) 0.009(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 Cu O1 1.959(3) . ? Cu N1 1.997(4) . ? Cu N2 1.998(4) . ? Cu N3 2.008(4) . ? V1 O2 1.623(3) 1_545 ? V1 O1 1.682(3) . ? V1 O4 1.771(3) 4_556 ? V1 O3 1.802(3) . ? V2 O6 1.626(3) . ? V2 O5 1.639(3) . ? V2 O4 1.789(3) 1_545 ? V2 O3 1.838(3) . ? O2 V1 1.623(3) 1_565 ? O4 V1 1.771(3) 4_456 ? O4 V2 1.789(3) 1_565 ? N1 C1 1.476(7) . ? N2 C2 1.471(6) . ? N2 C3 1.481(6) . ? N3 C4 1.483(7) . ? C1 C2 1.515(8) . ? C3 C4 1.507(8) . ? 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 Cu N1 95.01(15) . . ? O1 Cu N2 176.74(15) . . ? N1 Cu N2 84.7(2) . . ? O1 Cu N3 94.8(2) . . ? N1 Cu N3 165.1(2) . . ? N2 Cu N3 84.9(2) . . ? O2 V1 O1 106.88(14) 1_545 . ? O2 V1 O4 110.8(2) 1_545 4_556 ? O1 V1 O4 109.3(2) . 4_556 ? O2 V1 O3 109.5(2) 1_545 . ? O1 V1 O3 111.2(2) . . ? O4 V1 O3 109.1(2) 4_556 . ? O6 V2 O5 107.9(2) . . ? O6 V2 O4 112.9(2) . 1_545 ? O5 V2 O4 110.7(2) . 1_545 ? O6 V2 O3 107.8(2) . . ? O5 V2 O3 107.57(15) . . ? O4 V2 O3 109.7(2) 1_545 . ? V1 O1 Cu 130.3(2) . . ? V1 O3 V2 118.1(2) . . ? V1 O4 V2 152.9(2) 4_456 1_565 ? C1 N1 Cu 109.7(3) . . ? C2 N2 C3 117.2(4) . . ? C2 N2 Cu 108.2(3) . . ? C3 N2 Cu 107.0(3) . . ? C4 N3 Cu 109.0(3) . . ? N1 C1 C2 107.2(4) . . ? N2 C2 C1 107.3(4) . . ? N2 C3 C4 106.3(4) . . ? N3 C4 C3 108.6(4) . . ? _refine_diff_density_max 0.402 _refine_diff_density_min -0.439 _refine_diff_density_rms 0.100