# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'T Kiss' 'Attila Csaba Benyei' 'Annalisa Dean' 'Valerio Di Marco' 'Tamas Jakusch' 'Tamas Oncsik' _publ_contact_author_name 'Tamas Kiss' _publ_contact_author_email TKISS@CHEM.U-SZEGED.HU _publ_section_title ; Vanadate complexes in serum: a speciation modeling study ; # Attachment 'jakuschetal3.cif' #\#CIF_1.1 # CIF produced by WinGX routine CIF_UPDATE # Created on 2009-05-22 at 10:10:42 # Using CIFtbx version 2.6.2 16 Jun 1998 # Dictionary name : cif_core.dic # Dictionary vers : 2.3 # Request file : c:\wingx\files\cifdoc.dat # CIF files read : 0917b dreduc psi_scan stdanal struct #------------------ SECTION 1. GLOBAL INFORMATION ---------------------------# data_VO2L2.NH4.3H2O _database_code_depnum_ccdc_archive 'CCDC 741282' _audit_creation_date 2009-07-16T11:15:06-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #============================================================================== # CHEMICAL DATA _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C10 H18 N3 O9 V1' _chemical_formula_sum 'C10 H18 N3 O9 V' _chemical_formula_weight 375.21 #============================================================================== # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 1 2/c 1' _symmetry_space_group_name_Hall '-C 2yc' 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 16.1650(19) _cell_length_b 9.6283(9) _cell_length_c 11.8184(17) _cell_angle_alpha 90 _cell_angle_beta 121.333(9) _cell_angle_gamma 90 _cell_volume 1571.2(3) _cell_formula_units_Z 4 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 9.1 _cell_measurement_theta_max 15.5 _cell_measurement_temperature 293(2) _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.25 _exptl_crystal_density_diffrn 1.586 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 776 _exptl_absorpt_coefficient_mu 0.682 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details ; North A.C.T., Phillips D.C. & Mathews F.S. (1968) Acta. Cryst. A24, 351 Number of psi-scan sets used was 5 Theta correction was applied. Averaged transmission function was used. Fourier smoothing - Window value 5 ; _exptl_absorpt_correction_T_min 0.7855 _exptl_absorpt_correction_T_max 0.8423 #============================================================================== # EXPERIMENTAL DATA _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Enraf Nonius MACH3' _diffrn_measurement_method 'profiled omega/2theta scans' _diffrn_reflns_number 4140 _diffrn_reflns_av_R_equivalents 0.0358 _diffrn_reflns_av_unetI/netI 0.022 _diffrn_reflns_theta_min 3.55 _diffrn_reflns_theta_max 26.47 _diffrn_reflns_theta_full 26.47 _diffrn_measured_fraction_theta_max 0.988 _diffrn_measured_fraction_theta_full 0.988 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 10 _diffrn_standards_number 3 _diffrn_standards_interval_count 99 _diffrn_standards_interval_time 8 _diffrn_standards_decay_% 2 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 0 -11 2 2 6 -6 2 4 -6 #============================================================================== # STRUCTURE SOLUTION _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #============================================================================== # REFINEMENT DATA _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. ; _reflns_number_total 1607 _reflns_number_gt 1582 _reflns_threshold_expression >2sigma(I) _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_R_factor_all 0.042 _refine_ls_R_factor_gt 0.0412 _refine_ls_wR_factor_ref 0.1167 _refine_ls_goodness_of_fit_ref 1.196 _refine_ls_restrained_S_all 1.195 _refine_ls_number_reflns 1607 _refine_ls_number_parameters 141 _refine_ls_number_restraints 8 _refine_ls_hydrogen_treatment mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0438P)^2^+4.0866P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_shift/su_max 0.009 _refine_ls_shift/su_mean 0.001 _refine_diff_density_max 0.452 _refine_diff_density_min -0.367 _refine_diff_density_rms 0.065 _refine_ls_extinction_method none 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 0 '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 0.006 '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' _computing_data_collection 'MACH3/PC (Enraf Nonius, 1996)' _computing_cell_refinement 'MACH3/PC (Enraf Nonius, 1996)' _computing_data_reduction 'PROFIT (Streltsov & Zavodnik, 1989)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #============================================================================== # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_refinement_flags _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_type_symbol C2 0.37150(17) 0.0135(3) 0.7816(2) 0.0274(5) Uani d . 1 . . C C3 0.3238(2) -0.0644(3) 0.8303(3) 0.0409(7) Uani d . 1 . . C H3 0.3594 -0.1156 0.9078 0.049 Uiso calc . 1 . . H C4 0.2247(2) -0.0652(3) 0.7640(3) 0.0432(7) Uani d . 1 . . C H4 0.1933 -0.117 0.7972 0.052 Uiso calc . 1 . . H C5 0.17008(19) 0.0106(3) 0.6472(3) 0.0385(6) Uani d . 1 . . C H5 0.1028 0.0092 0.6024 0.046 Uiso calc . 1 . . H C6 0.21662(18) 0.0863(3) 0.5999(3) 0.0307(5) Uani d . 1 . . C H6 0.1814 0.1375 0.5223 0.037 Uiso calc . 1 . . H N1 0.31476(14) 0.0867(2) 0.6668(2) 0.0252(4) Uani d . 1 . . N N2 0.5515(14) -0.212(2) 0.965(2) 0.093(6) Uani d PD 0.5 . . N O1 0.49436(14) 0.3049(2) 0.8555(2) 0.0360(5) Uani d . 1 . . O O2 0.36162(12) 0.16278(19) 0.62129(16) 0.0274(4) Uani d . 1 . . O O1W 0.5 -0.4072(4) 0.75 0.105(2) Uani d SD 1 . . O O3 0.46346(13) 0.0261(2) 0.83392(18) 0.0338(4) Uani d . 1 . . O O2W 0.2684(5) -0.2811(9) 0.5549(8) 0.081(2) Uani d PD 0.5 . . O O3W 0.5640(5) -0.2263(7) 0.9561(7) 0.0239(10) Uani d P 0.5 . . O V1 0.5 0.20040(6) 0.75 0.0227(2) Uani d S 1 . . V H11 0.5 -0.499(2) 0.75 0.027 Uiso d SD 1 . . H H12 0.544(3) -0.343(5) 0.773(6) 0.027 Uiso d PD 0.5 . . H H13 0.310(4) -0.353(4) 0.593(6) 0.027 Uiso d PD 0.5 . . H H14 0.225(5) -0.226(7) 0.489(6) 0.027 Uiso d PD 0.5 . . H H21 0.532(5) -0.137(5) 0.918(6) 0.027 Uiso d PD 0.5 . . H H22 0.552(5) -0.239(7) 1.035(4) 0.027 Uiso d PD 0.5 . . H H23 0.547(3) -0.275(3) 0.916(3) 0.027 Uiso d D 1 . . H H24 0.6040(19) -0.219(4) 0.969(4) 0.027 Uiso d D 1 . . H loop_ _atom_site_aniso_label _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 C2 0.0246(11) 0.0306(12) 0.0246(12) -0.0020(9) 0.0111(10) 0.0036(9) C3 0.0381(15) 0.0456(16) 0.0383(15) -0.0049(13) 0.0195(13) 0.0123(13) C4 0.0369(15) 0.0482(17) 0.0520(17) -0.0096(13) 0.0283(14) 0.0063(14) C5 0.0252(13) 0.0423(15) 0.0484(16) -0.0053(11) 0.0195(12) -0.0008(13) C6 0.0214(11) 0.0340(13) 0.0308(13) -0.0006(10) 0.0094(10) 0.0008(10) N1 0.0213(9) 0.0291(10) 0.0247(10) -0.0028(8) 0.0116(8) 0.0010(8) N2 0.100(10) 0.107(11) 0.102(10) 0.038(7) 0.074(8) -0.005(7) O1 0.0294(9) 0.0426(11) 0.0372(10) 0.0027(8) 0.0182(8) -0.0085(8) O2 0.0215(8) 0.0369(10) 0.0240(8) -0.0016(7) 0.0119(7) 0.0078(7) O1W 0.204(7) 0.033(2) 0.089(3) 0 0.084(4) 0 O3 0.0231(9) 0.0421(11) 0.0312(9) 0.0001(8) 0.0106(7) 0.0114(8) O2W 0.066(4) 0.099(6) 0.096(5) 0.007(3) 0.057(4) 0.006(4) O3W 0.029(2) 0.026(2) 0.023(2) 0.016(2) 0.017(2) 0.0018(17) V1 0.0188(3) 0.0256(3) 0.0250(3) 0 0.0122(2) 0 #============================================================================== # MOLECULAR GEOMETRY _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_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag C2 O3 . 1.285(3) ? C2 N1 . 1.373(3) ? C2 C3 . 1.397(4) ? C3 C4 . 1.370(4) ? C3 H3 . 0.93 ? C4 C5 . 1.397(4) ? C4 H4 . 0.93 ? C5 C6 . 1.359(4) ? C5 H5 . 0.93 ? C6 N1 . 1.356(3) ? C6 H6 . 0.93 ? N1 O2 . 1.350(3) ? N2 H21 . 0.86(2) ? N2 H22 . 0.86(2) ? N2 H23 . 0.816(19) ? N2 H24 . 0.833(19) ? O1 V1 . 1.6412(19) ? O2 V1 . 1.9773(17) ? O1W H11 . 0.881(19) ? O1W H12 . 0.87(2) ? O3 V1 . 2.1817(19) ? O2W O2W 7_546 1.262(16) ? O2W H13 . 0.91(2) ? O2W H14 . 0.90(2) ? O3W H21 . 0.98(4) ? O3W H22 . 1.06(4) ? O3W H23 . 0.62(3) ? O3W H24 . 0.59(2) ? V1 O1 2_656 1.6411(19) ? V1 O2 2_656 1.9773(17) ? V1 O3 2_656 2.1817(19) ? 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 C2 N1 116.0(2) . . ? O3 C2 C3 126.9(2) . . ? N1 C2 C3 117.1(2) . . ? C4 C3 C2 120.0(3) . . ? C4 C3 H3 120 . . ? C2 C3 H3 120 . . ? C3 C4 C5 120.8(3) . . ? C3 C4 H4 119.6 . . ? C5 C4 H4 119.6 . . ? C6 C5 C4 119.1(2) . . ? C6 C5 H5 120.4 . . ? C4 C5 H5 120.4 . . ? N1 C6 C5 119.5(2) . . ? N1 C6 H6 120.3 . . ? C5 C6 H6 120.3 . . ? O2 N1 C6 119.9(2) . . ? O2 N1 C2 116.56(19) . . ? C6 N1 C2 123.5(2) . . ? H21 N2 H22 134(7) . . ? H21 N2 H23 107(6) . . ? H22 N2 H23 114(7) . . ? H21 N2 H24 97(6) . . ? H22 N2 H24 115(6) . . ? H23 N2 H24 72(4) . . ? N1 O2 V1 115.95(13) . . ? H11 O1W H12 135(4) . . ? C2 O3 V1 111.86(15) . . ? O2W O2W H13 135(4) 7_546 . ? O2W O2W H14 25(5) 7_546 . ? H13 O2W H14 158(7) . . ? H21 O3W H22 102(5) . . ? H21 O3W H23 113(5) . . ? H22 O3W H23 112(5) . . ? H21 O3W H24 106(5) . . ? H22 O3W H24 118(5) . . ? H23 O3W H24 106(5) . . ? O1 V1 O1 104.42(15) 2_656 . ? O1 V1 O2 102.08(9) 2_656 2_656 ? O1 V1 O2 90.88(8) . 2_656 ? O1 V1 O2 90.88(8) 2_656 . ? O1 V1 O2 102.08(9) . . ? O2 V1 O2 158.89(11) 2_656 . ? O1 V1 O3 162.20(9) 2_656 . ? O1 V1 O3 89.48(9) . . ? O2 V1 O3 88.55(7) 2_656 . ? O2 V1 O3 75.13(7) . . ? O1 V1 O3 89.48(9) 2_656 2_656 ? O1 V1 O3 162.20(9) . 2_656 ? O2 V1 O3 75.13(7) 2_656 2_656 ? O2 V1 O3 88.55(7) . 2_656 ? O3 V1 O3 79.40(11) . 2_656 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1W H11 O1 0.881(19) 2.293(17) 3.061(4) 145.6(3) 2_646 O1W H11 O1 0.881(19) 2.293(17) 3.061(4) 145.6(3) 1_545 O1W H12 N2 0.87(2) 2.54(6) 2.917(19) 107(5) . O1W H12 O3W 0.87(2) 2.30(6) 2.723(8) 110(5) . N2 H21 O3 0.86(2) 1.88(4) 2.72(2) 163(7) . N2 H22 O1 0.86(2) 1.91(4) 2.73(2) 160(6) 5_657 N2 H23 O1W 0.816(19) 2.12(2) 2.917(19) 164(4) . N2 H24 O2W 0.833(19) 2.30(3) 3.09(2) 159(4) 8_546 N2 H24 O2W 0.833(19) 2.30(2) 3.115(17) 167(4) 2_656 O2W H13 N2 0.91(2) 3.00(6) 3.115(17) 89(4) 2_656 O2W H14 N2 0.90(2) 2.74(8) 3.09(2) 105(6) 8_445 O2W H14 O3W 0.90(2) 2.47(8) 2.877(10) 108(6) 8_445 O2W H13 O3W 0.91(2) 2.69(6) 2.829(11) 89(4) 2_656 O3W H23 O1W 0.62(3) 2.12(2) 2.723(8) 164(4) . O3W H24 O2W 0.59(2) 2.30(2) 2.829(11) 151(5) 2_656 # END of CIF