Electronic Supplementary Material for Dalton Transactions This journal is © The Royal Society of Chemistry 2005 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_23mar _database_code_depnum_ccdc_archive 'CCDC 282762' _audit_creation_method SHELXL-97 _chemical_name_systematic ; bis [mu-oxo ((E)-N'-(1-(pyridin-2-yl)ethylidene)nicotinohydrazonium) oxovanadium(V))] sesquihydrate ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C26 H22 N8 O6 V2 ,1.5(H2 O)' _chemical_formula_sum 'C26 H25 N8 O7.50 V2' _chemical_formula_weight 671.42 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' _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 23.9504(7) _cell_length_b 15.1397(4) _cell_length_c 7.7450(2) _cell_angle_alpha 90.00 _cell_angle_beta 102.4840(10) _cell_angle_gamma 90.00 _cell_volume 2741.95(13) _cell_formula_units_Z 4 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 100 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.72 _exptl_crystal_size_mid 0.36 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas 'not determined' _exptl_crystal_density_diffrn 1.626 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1372 _exptl_absorpt_coefficient_mu 0.746 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6156 _exptl_absorpt_correction_T_max 0.8412 _exptl_absorpt_process_details 'program SADABS (Bruker axs systems)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19955 _diffrn_reflns_av_R_equivalents 0.0343 _diffrn_reflns_av_sigmaI/netI 0.0326 _diffrn_reflns_limit_h_min -36 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.69 _diffrn_reflns_theta_max 32.54 _reflns_number_total 4906 _reflns_number_gt 4069 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _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. The structure contains two disordered molecules of water. O4 sits on two sites with an occupancy of 0.5 each, O5 on two sites with an occupancy of 0.25 each. The hydrogens belonging to O5 were not found, leading to a discrepancy between given cell content and atom list. ; _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^)+(0.0725P)^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 4906 _refine_ls_number_parameters 209 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0484 _refine_ls_R_factor_gt 0.0406 _refine_ls_wR_factor_ref 0.1199 _refine_ls_wR_factor_gt 0.1165 _refine_ls_goodness_of_fit_ref 1.072 _refine_ls_restrained_S_all 1.072 _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 V1 V 0.287861(9) 0.224287(14) 0.18337(3) 0.02032(8) Uani 1 1 d . . . O1 O 0.31036(4) 0.23954(7) 0.39340(13) 0.0280(2) Uani 1 1 d . . . O2 O 0.25447(4) 0.18997(6) -0.11042(12) 0.02322(19) Uani 1 1 d . . . O3 O 0.36001(4) 0.24699(7) 0.10814(14) 0.0263(2) Uani 1 1 d . . . N1 N 0.22558(4) 0.13023(8) 0.21175(14) 0.0228(2) Uani 1 1 d . . . N2 N 0.32292(4) 0.09807(8) 0.15092(14) 0.0226(2) Uani 1 1 d . . . N3 N 0.37619(5) 0.09622(9) 0.11056(16) 0.0271(2) Uani 1 1 d . . . N4 N 0.51798(7) 0.29678(15) -0.0064(2) 0.0603(5) Uani 1 1 d . . . C1 C 0.55019(8) 0.2271(2) -0.0304(3) 0.0651(8) Uani 1 1 d . . . H1 H 0.5868 0.2385 -0.0545 0.078 Uiso 1 1 calc R . . C2 C 0.53393(8) 0.14100(19) -0.0225(3) 0.0611(6) Uani 1 1 d . . . H2 H 0.5581 0.0942 -0.0430 0.073 Uiso 1 1 calc R . . C3 C 0.48158(7) 0.12424(15) 0.0159(3) 0.0495(5) Uani 1 1 d . . . H3 H 0.4691 0.0651 0.0233 0.059 Uiso 1 1 calc R . . C4 C 0.44687(6) 0.19383(12) 0.0439(2) 0.0329(3) Uani 1 1 d . . . C5 C 0.46673(7) 0.27880(13) 0.0317(3) 0.0426(4) Uani 1 1 d . . . H5 H 0.4433 0.3268 0.0511 0.051 Uiso 1 1 calc R . . C6 C 0.39099(5) 0.17824(10) 0.09097(17) 0.0258(3) Uani 1 1 d . . . C7 C 0.29499(6) 0.02614(9) 0.16030(16) 0.0233(3) Uani 1 1 d . . . C8 C 0.23754(5) 0.04340(9) 0.19330(17) 0.0229(2) Uani 1 1 d . . . C9 C 0.19788(6) -0.02195(10) 0.20269(19) 0.0298(3) Uani 1 1 d . . . H9 H 0.2066 -0.0822 0.1865 0.036 Uiso 1 1 calc R . . C10 C 0.14534(6) 0.00160(12) 0.2359(2) 0.0375(4) Uani 1 1 d . . . H10 H 0.1175 -0.0423 0.2420 0.045 Uiso 1 1 calc R . . C11 C 0.13395(6) 0.08949(12) 0.2602(2) 0.0358(3) Uani 1 1 d . . . H11 H 0.0986 0.1068 0.2863 0.043 Uiso 1 1 calc R . . C12 C 0.17486(6) 0.15222(11) 0.24578(18) 0.0280(3) Uani 1 1 d . . . H12 H 0.1667 0.2128 0.2605 0.034 Uiso 1 1 calc R . . C13 C 0.31697(7) -0.06429(10) 0.1413(2) 0.0314(3) Uani 1 1 d . . . H13A H 0.3484 -0.0613 0.0788 0.047 Uiso 1 1 calc R . . H13B H 0.2861 -0.1010 0.0739 0.047 Uiso 1 1 calc R . . H13C H 0.3309 -0.0902 0.2587 0.047 Uiso 1 1 calc R . . O4 O 0.5180(3) 0.4854(4) -0.0610(9) 0.127(2) Uani 0.50 1 d PD . . H4B H 0.503(2) 0.505(3) -0.162(3) 0.048(9) Uiso 0.50 1 d PD . . H4A H 0.523(2) 0.4312(8) -0.076(6) 0.048(9) Uiso 0.50 1 d PD . . O5 O 0.5070(4) 0.4646(7) -0.1858(9) 0.076(2) Uiso 0.25 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 V1 0.01897(12) 0.01904(13) 0.02301(13) -0.00225(7) 0.00468(8) 0.00201(7) O1 0.0276(5) 0.0299(5) 0.0255(5) -0.0020(4) 0.0032(4) -0.0004(4) O2 0.0235(4) 0.0206(5) 0.0255(5) -0.0034(4) 0.0054(3) 0.0034(4) O3 0.0194(4) 0.0269(5) 0.0327(5) 0.0000(4) 0.0057(4) 0.0004(4) N1 0.0224(5) 0.0236(5) 0.0227(5) -0.0006(4) 0.0055(4) 0.0024(4) N2 0.0194(5) 0.0244(5) 0.0242(5) 0.0003(4) 0.0052(4) 0.0048(4) N3 0.0211(5) 0.0330(6) 0.0283(6) 0.0009(5) 0.0079(4) 0.0073(5) N4 0.0274(7) 0.0933(14) 0.0583(11) 0.0288(10) 0.0049(7) -0.0121(9) C1 0.0192(7) 0.131(2) 0.0461(11) 0.0293(12) 0.0091(7) 0.0035(10) C2 0.0342(9) 0.0962(18) 0.0604(13) 0.0180(12) 0.0266(9) 0.0213(11) C3 0.0320(8) 0.0604(12) 0.0621(12) 0.0054(9) 0.0230(8) 0.0110(8) C4 0.0202(6) 0.0495(9) 0.0295(7) 0.0060(6) 0.0064(5) 0.0031(6) C5 0.0239(7) 0.0571(11) 0.0449(10) 0.0143(8) 0.0032(7) -0.0050(7) C6 0.0200(6) 0.0331(7) 0.0239(6) 0.0012(5) 0.0042(4) 0.0032(5) C7 0.0288(6) 0.0216(6) 0.0193(6) 0.0012(4) 0.0050(4) 0.0058(5) C8 0.0243(6) 0.0234(6) 0.0203(6) 0.0027(5) 0.0033(4) 0.0017(5) C9 0.0316(7) 0.0250(7) 0.0312(7) 0.0068(5) 0.0032(5) -0.0015(5) C10 0.0303(7) 0.0417(9) 0.0401(9) 0.0119(7) 0.0066(6) -0.0067(7) C11 0.0262(7) 0.0443(9) 0.0386(8) 0.0086(7) 0.0108(6) 0.0022(6) C12 0.0237(6) 0.0331(7) 0.0283(7) 0.0012(5) 0.0084(5) 0.0051(5) C13 0.0410(8) 0.0228(7) 0.0326(7) 0.0031(5) 0.0129(6) 0.0087(6) O4 0.101(4) 0.104(4) 0.168(6) -0.012(4) 0.012(4) -0.040(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 V1 O1 1.6158(10) . ? V1 O2 1.6687(9) 7 ? V1 O3 1.9695(10) . ? V1 N1 2.1078(11) . ? V1 N2 2.1239(11) . ? V1 O2 2.3022(9) . ? O2 V1 1.6687(9) 7 ? O3 C6 1.3018(17) . ? N1 C12 1.3397(16) . ? N1 C8 1.3595(18) . ? N2 C7 1.2882(18) . ? N2 N3 1.3780(15) . ? N3 C6 1.3092(19) . ? N4 C1 1.343(3) . ? N4 C5 1.351(2) . ? C1 C2 1.366(4) . ? C1 H1 0.9500 . ? C2 C3 1.373(2) . ? C2 H2 0.9500 . ? C3 C4 1.388(3) . ? C3 H3 0.9500 . ? C4 C5 1.382(3) . ? C4 C6 1.4801(19) . ? C5 H5 0.9500 . ? C7 C8 1.4760(18) . ? C7 C13 1.4855(19) . ? C8 C9 1.3843(19) . ? C9 C10 1.384(2) . ? C9 H9 0.9500 . ? C10 C11 1.379(3) . ? C10 H10 0.9500 . ? C11 C12 1.386(2) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? O4 O5 0.997(9) . ? O4 O4 1.480(13) 5_665 ? O4 H4B 0.8399(10) . ? O4 H4A 0.8400(10) . ? O5 O5 0.978(14) 2_654 ? O5 H4B 0.65(4) . ? O5 H4A 0.99(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 V1 O2 106.00(5) . 7 ? O1 V1 O3 98.63(5) . . ? O2 V1 O3 105.77(5) 7 . ? O1 V1 N1 94.65(5) . . ? O2 V1 N1 99.73(4) 7 . ? O3 V1 N1 146.58(4) . . ? O1 V1 N2 101.15(5) . . ? O2 V1 N2 152.45(4) 7 . ? O3 V1 N2 74.18(4) . . ? N1 V1 N2 73.22(4) . . ? O1 V1 O2 175.04(5) . . ? O2 V1 O2 77.59(4) 7 . ? O3 V1 O2 83.49(4) . . ? N1 V1 O2 81.27(4) . . ? N2 V1 O2 75.03(4) . . ? V1 O2 V1 102.41(4) 7 . ? C6 O3 V1 116.53(9) . . ? C12 N1 C8 118.79(12) . . ? C12 N1 V1 123.01(10) . . ? C8 N1 V1 118.19(9) . . ? C7 N2 N3 120.87(11) . . ? C7 N2 V1 122.04(9) . . ? N3 N2 V1 117.02(9) . . ? C6 N3 N2 107.11(11) . . ? C1 N4 C5 116.6(2) . . ? N4 C1 C2 124.44(18) . . ? N4 C1 H1 117.8 . . ? C2 C1 H1 117.8 . . ? C1 C2 C3 117.9(2) . . ? C1 C2 H2 121.0 . . ? C3 C2 H2 121.0 . . ? C2 C3 C4 120.0(2) . . ? C2 C3 H3 120.0 . . ? C4 C3 H3 120.0 . . ? C5 C4 C3 117.99(16) . . ? C5 C4 C6 120.55(16) . . ? C3 C4 C6 121.43(16) . . ? N4 C5 C4 123.02(19) . . ? N4 C5 H5 118.5 . . ? C4 C5 H5 118.5 . . ? O3 C6 N3 124.89(12) . . ? O3 C6 C4 117.61(14) . . ? N3 C6 C4 117.50(13) . . ? N2 C7 C8 112.02(11) . . ? N2 C7 C13 125.03(12) . . ? C8 C7 C13 122.94(13) . . ? N1 C8 C9 121.53(12) . . ? N1 C8 C7 114.51(12) . . ? C9 C8 C7 123.96(13) . . ? C8 C9 C10 119.17(14) . . ? C8 C9 H9 120.4 . . ? C10 C9 H9 120.4 . . ? C11 C10 C9 119.22(14) . . ? C11 C10 H10 120.4 . . ? C9 C10 H10 120.4 . . ? C10 C11 C12 119.08(14) . . ? C10 C11 H11 120.5 . . ? C12 C11 H11 120.5 . . ? N1 C12 C11 122.16(14) . . ? N1 C12 H12 118.9 . . ? C11 C12 H12 118.9 . . ? C7 C13 H13A 109.5 . . ? C7 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C7 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? O4 O4 H4B 108(4) 5_665 . ? O4 O4 H4A 120(4) 5_665 . ? H4B O4 H4A 104.48(17) . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 32.54 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 0.639 _refine_diff_density_min -0.345 _refine_diff_density_rms 0.083