Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2001 data_1 _database_code_CSD 156000 _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Trans' loop_ _publ_author_name 'Joaquín Sanchiz' 'Pedro Esparza' 'Sixto Domínguez' 'Alfredo Mederos' 'David Saysell' 'Agustin Sánchez' 'Rafael Ruano' 'Juan Manuel Arrieta' _publ_contact_author_name 'Prof Alfredo Mederos' _publ_contact_author_address ; Prof Alfredo Mederos Department of Inorganic Chemistry University of La Laguna 38204 La Laguna Tenerife SPAIN ; _audit_creation_method 'SHELXL-97' _chemical_name_systematic ; Aquacadmium(II)-(-(3,4-toluenediamine-N,N,N',N'-tetraacetato)-cadmium(II)aqua ; _chemical_name_common ? _chemical_formula_moiety 'C15H14N2O8Cd2, 2H2O' _chemical_formula_sum 'C15 H18 Cd2 N2 O10' _chemical_formula_weight '611.11' 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' 'Cd' 'Cd' -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? monoclinic _symmetry_space_group_name_H-M ? P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 8.597(2) _cell_length_b 24.346(2) _cell_length_c 9.197(2) _cell_angle_alpha 90.00 _cell_angle_beta 106.10(3) _cell_angle_gamma 90.00 _cell_volume 1849.5(6) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 8 _cell_measurement_theta_max 25 _exptl_crystal_description Prismatic _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.6mm _exptl_crystal_size_mid 0.5mm _exptl_crystal_size_min 0.3mm _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.195 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1192 _exptl_absorpt_coefficient_mu 2.359 _exptl_absorpt_correction_type None _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5533 _diffrn_reflns_av_R_equivalents 0.0478 _diffrn_reflns_av_sigmaI/netI 0.0147 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 34 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 1.67 _diffrn_reflns_theta_max 34.05 _reflns_number_total 5267 _reflns_number_gt 5117 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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 w==1/[\s^2^(Fo^2^)+(0.0702P)^2^+8.7079P] 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 5267 _refine_ls_number_parameters 264 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0443 _refine_ls_R_factor_gt 0.0426 _refine_ls_wR_factor_ref 0.1332 _refine_ls_wR_factor_gt 0.1307 _refine_ls_goodness_of_fit_ref 1.271 _refine_ls_restrained_S_all 1.271 _refine_ls_shift/su_max 0.003 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cd1 Cd 0.73729(3) 0.175184(11) 0.84500(3) 0.00848(10) Uani 1 d . . . O1W O 0.6622(4) 0.25882(14) 0.8962(4) 0.0174(6) Uani 1 d . . . Cd2 Cd 0.95775(3) 0.332070(12) 0.70550(3) 0.00911(10) Uani 1 d . . . O2W O 1.2297(4) 0.30884(15) 0.7698(4) 0.0177(6) Uani 1 d . . . C1 C 1.1824(5) -0.04746(19) 0.6631(5) 0.0166(8) Uani 1 d . . . H1A H 1.1727 -0.0442 0.5548 0.010(3) Uiso 1 calc R . . H1B H 1.1734 -0.0862 0.6888 0.010(3) Uiso 1 calc R . . H1C H 1.2877 -0.0331 0.7215 0.010(3) Uiso 1 calc R . . C2 C 1.0492(5) -0.01503(18) 0.7004(4) 0.0142(7) Uani 1 d . . . C3 C 0.9015(6) -0.03953(18) 0.6966(5) 0.0159(8) Uani 1 d . . . H3 H 0.8859 -0.0775 0.6733 0.010(3) Uiso 1 calc R . . C4 C 0.7768(5) -0.00918(16) 0.7265(5) 0.0130(7) Uani 1 d . . . H4 H 0.6773 -0.0266 0.7245 0.010(3) Uiso 1 calc R . . C5 C 0.7978(5) 0.04746(16) 0.7597(4) 0.0095(6) Uani 1 d . . . C6 C 0.9449(5) 0.07251(16) 0.7648(4) 0.0108(7) Uani 1 d . . . C7 C 1.0693(5) 0.04072(17) 0.7358(4) 0.0122(7) Uani 1 d . . . H7 H 1.1701 0.0577 0.7404 0.010(3) Uiso 1 calc R . . N1 N 0.6659(4) 0.07901(14) 0.7909(4) 0.0088(6) Uani 1 d . . . C8 C 0.6212(5) 0.05596(17) 0.9227(4) 0.0116(7) Uani 1 d . . . H8A H 0.7199 0.0422 0.9973 0.010(3) Uiso 1 calc R . . H8B H 0.5474 0.0244 0.8891 0.010(3) Uiso 1 calc R . . C9 C 0.5393(4) 0.09794(16) 0.9984(4) 0.0097(6) Uani 1 d . . . O1 O 0.5474(4) 0.14845(13) 0.9693(4) 0.0144(6) Uani 1 d . . . O2 O 0.4688(4) 0.08104(13) 1.0924(3) 0.0141(6) Uani 1 d . . . C10 C 0.5245(4) 0.08239(17) 0.6573(4) 0.0102(7) Uani 1 d . . . H10A H 0.4272 0.0909 0.6908 0.010(3) Uiso 1 calc R . . H10B H 0.5072 0.0462 0.6064 0.010(3) Uiso 1 calc R . . C11 C 0.5431(5) 0.12615(17) 0.5429(4) 0.0111(7) Uani 1 d . . . O3 O 0.6206(4) 0.16901(13) 0.5900(3) 0.0140(6) Uani 1 d . . . O4 O 0.4734(4) 0.11521(13) 0.4071(3) 0.0152(6) Uani 1 d . . . N2 N 0.9694(4) 0.13072(14) 0.7918(4) 0.0093(6) Uani 1 d . . . C12 C 0.9820(5) 0.15819(16) 0.6521(4) 0.0111(7) Uani 1 d . . . H12A H 0.9080 0.1401 0.5632 0.010(3) Uiso 1 calc R . . H12B H 1.0938 0.1543 0.6437 0.010(3) Uiso 1 calc R . . C13 C 0.9394(4) 0.21881(17) 0.6515(4) 0.0111(7) Uani 1 d . . . O5 O 0.9298(4) 0.24064(12) 0.7734(3) 0.0127(5) Uani 1 d . . . O6 O 0.9210(4) 0.24566(13) 0.5306(4) 0.0149(6) Uani 1 d . . . C14 C 1.1099(5) 0.14329(18) 0.9235(4) 0.0122(7) Uani 1 d . . . H14A H 1.1713 0.1741 0.8958 0.010(3) Uiso 1 calc R . . H14B H 1.1822 0.1109 0.9441 0.010(3) Uiso 1 calc R . . C15 C 1.0667(5) 0.15846(16) 1.0683(4) 0.0096(6) Uani 1 d . . . O7 O 1.1867(4) 0.16664(13) 1.1822(4) 0.0136(6) Uani 1 d . . . O8 O 0.9229(4) 0.16210(13) 1.0726(3) 0.0131(5) Uani 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 Cd1 0.00813(15) 0.00943(15) 0.00857(15) -0.00077(8) 0.00346(10) -0.00017(8) O1W 0.0199(15) 0.0147(15) 0.0234(15) 0.0039(12) 0.0156(12) 0.0043(11) Cd2 0.00890(15) 0.00907(15) 0.00970(15) 0.00035(8) 0.00315(10) -0.00085(8) O2W 0.0108(13) 0.0276(18) 0.0159(14) 0.0062(12) 0.0058(11) 0.0021(12) C1 0.0175(19) 0.017(2) 0.0151(18) -0.0009(15) 0.0049(15) 0.0063(15) C2 0.0172(18) 0.017(2) 0.0090(16) 0.0011(13) 0.0051(14) 0.0064(14) C3 0.024(2) 0.0098(18) 0.0150(18) -0.0034(14) 0.0078(15) 0.0014(15) C4 0.0186(18) 0.0070(17) 0.0155(17) 0.0003(13) 0.0079(14) -0.0008(13) C5 0.0114(15) 0.0103(17) 0.0079(15) 0.0010(12) 0.0044(12) 0.0017(13) C6 0.0127(16) 0.0106(17) 0.0087(15) -0.0011(12) 0.0025(13) 0.0001(13) C7 0.0124(16) 0.0129(18) 0.0119(16) 0.0021(13) 0.0044(13) 0.0023(13) N1 0.0095(13) 0.0107(15) 0.0070(13) 0.0016(10) 0.0035(11) 0.0004(11) C8 0.0139(17) 0.0134(18) 0.0094(15) -0.0001(13) 0.0065(13) 0.0012(13) C9 0.0069(15) 0.0128(17) 0.0092(15) -0.0011(13) 0.0018(12) 0.0015(12) O1 0.0153(13) 0.0126(14) 0.0190(14) -0.0017(11) 0.0106(11) -0.0003(10) O2 0.0171(14) 0.0163(15) 0.0121(13) 0.0013(10) 0.0094(11) 0.0021(11) C10 0.0094(15) 0.0140(18) 0.0069(15) 0.0007(12) 0.0015(12) -0.0027(12) C11 0.0108(16) 0.0123(17) 0.0108(16) 0.0013(13) 0.0041(13) 0.0007(13) O3 0.0151(14) 0.0144(15) 0.0115(13) 0.0012(10) 0.0022(11) -0.0035(10) O4 0.0215(15) 0.0142(14) 0.0084(12) 0.0019(10) 0.0016(11) -0.0036(11) N2 0.0124(14) 0.0085(15) 0.0082(13) 0.0000(11) 0.0050(11) 0.0000(11) C12 0.0142(17) 0.0070(16) 0.0133(17) 0.0000(13) 0.0057(13) 0.0013(13) C13 0.0086(15) 0.0130(18) 0.0141(17) -0.0033(13) 0.0073(13) -0.0025(13) O5 0.0153(13) 0.0094(13) 0.0165(13) -0.0036(10) 0.0093(11) -0.0017(10) O6 0.0175(14) 0.0142(14) 0.0163(14) 0.0024(11) 0.0102(11) -0.0001(11) C14 0.0103(16) 0.0169(19) 0.0102(16) -0.0028(13) 0.0044(13) -0.0006(13) C15 0.0105(16) 0.0094(17) 0.0093(15) -0.0022(12) 0.0035(13) 0.0004(12) O7 0.0100(13) 0.0181(15) 0.0116(13) -0.0034(10) 0.0010(10) 0.0005(10) O8 0.0096(13) 0.0193(15) 0.0113(13) -0.0017(11) 0.0045(10) 0.0010(10) _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 Cd1 O1W 2.226(3) . ? Cd1 O8 2.275(3) . ? Cd1 O3 2.286(3) . ? Cd1 O1 2.330(3) . ? Cd1 N2 2.436(3) . ? Cd1 N1 2.437(3) . ? Cd1 O5 2.513(3) . ? Cd2 O4 2.228(3) 4_666 ? Cd2 O7 2.280(3) 4_565 ? Cd2 O2W 2.317(3) . ? Cd2 O5 2.342(3) . ? Cd2 O2 2.371(3) 4_665 ? Cd2 O1 2.543(3) 4_665 ? Cd2 O6 2.614(3) . ? C1 C2 1.506(6) . ? C2 C3 1.395(6) . ? C2 C7 1.395(6) . ? C3 C4 1.391(6) . ? C4 C5 1.413(5) . ? C5 C6 1.392(5) . ? C5 N1 1.463(5) . ? C6 C7 1.405(5) . ? C6 N2 1.444(5) . ? N1 C10 1.472(5) . ? N1 C8 1.480(5) . ? C8 C9 1.515(5) . ? C9 O2 1.254(5) . ? C9 O1 1.265(5) . ? O1 Cd2 2.543(3) 4_566 ? O2 Cd2 2.371(3) 4_566 ? C10 C11 1.536(5) . ? C11 O3 1.249(5) . ? C11 O4 1.255(5) . ? O4 Cd2 2.228(3) 4_565 ? N2 C12 1.479(5) . ? N2 C14 1.486(5) . ? C12 C13 1.520(6) . ? C13 O6 1.261(5) . ? C13 O5 1.264(5) . ? C14 C15 1.524(5) . ? C15 O8 1.251(5) . ? C15 O7 1.265(5) . ? O7 Cd2 2.280(3) 4_666 ? 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 O1W Cd1 O8 95.98(12) . . ? O1W Cd1 O3 101.93(12) . . ? O8 Cd1 O3 158.59(11) . . ? O1W Cd1 O1 82.41(11) . . ? O8 Cd1 O1 85.27(11) . . ? O3 Cd1 O1 108.49(11) . . ? O1W Cd1 N2 138.67(12) . . ? O8 Cd1 N2 73.62(11) . . ? O3 Cd1 N2 85.15(12) . . ? O1 Cd1 N2 134.33(11) . . ? O1W Cd1 N1 148.30(11) . . ? O8 Cd1 N1 97.24(11) . . ? O3 Cd1 N1 73.34(11) . . ? O1 Cd1 N1 70.17(11) . . ? N2 Cd1 N1 72.90(11) . . ? O1W Cd1 O5 74.10(10) . . ? O8 Cd1 O5 89.14(11) . . ? O3 Cd1 O5 84.63(11) . . ? O1 Cd1 O5 155.14(10) . . ? N2 Cd1 O5 66.02(10) . . ? N1 Cd1 O5 134.65(10) . . ? O4 Cd2 O7 83.96(12) 4_666 4_565 ? O4 Cd2 O2W 95.99(12) 4_666 . ? O7 Cd2 O2W 163.71(11) 4_565 . ? O4 Cd2 O5 108.21(11) 4_666 . ? O7 Cd2 O5 81.98(11) 4_565 . ? O2W Cd2 O5 82.58(12) . . ? O4 Cd2 O2 81.42(11) 4_666 4_665 ? O7 Cd2 O2 96.36(11) 4_565 4_665 ? O2W Cd2 O2 99.75(11) . 4_665 ? O5 Cd2 O2 169.90(10) . 4_665 ? O4 Cd2 O1 129.85(11) 4_666 4_665 ? O7 Cd2 O1 117.45(11) 4_565 4_665 ? O2W Cd2 O1 74.94(11) . 4_665 ? O5 Cd2 O1 118.87(10) . 4_665 ? O2 Cd2 O1 53.14(10) 4_665 4_665 ? O4 Cd2 O6 160.89(11) 4_666 . ? O7 Cd2 O6 90.41(11) 4_565 . ? O2W Cd2 O6 84.37(12) . . ? O5 Cd2 O6 52.80(10) . . ? O2 Cd2 O6 117.43(10) 4_665 . ? O1 Cd2 O6 68.76(10) 4_665 . ? C3 C2 C7 118.3(4) . . ? C3 C2 C1 121.0(4) . . ? C7 C2 C1 120.7(4) . . ? C4 C3 C2 121.0(4) . . ? C3 C4 C5 120.1(4) . . ? C6 C5 C4 119.7(4) . . ? C6 C5 N1 120.6(3) . . ? C4 C5 N1 119.7(3) . . ? C5 C6 C7 119.0(4) . . ? C5 C6 N2 121.6(3) . . ? C7 C6 N2 119.4(4) . . ? C2 C7 C6 121.9(4) . . ? C5 N1 C10 111.8(3) . . ? C5 N1 C8 110.7(3) . . ? C10 N1 C8 111.3(3) . . ? C5 N1 Cd1 112.3(2) . . ? C10 N1 Cd1 102.7(2) . . ? C8 N1 Cd1 107.8(2) . . ? N1 C8 C9 112.3(3) . . ? O2 C9 O1 122.0(4) . . ? O2 C9 C8 118.0(4) . . ? O1 C9 C8 119.9(3) . . ? C9 O1 Cd1 117.6(2) . . ? C9 O1 Cd2 87.3(2) . 4_566 ? Cd1 O1 Cd2 141.86(14) . 4_566 ? C9 O2 Cd2 95.5(2) . 4_566 ? N1 C10 C11 113.1(3) . . ? O3 C11 O4 125.7(4) . . ? O3 C11 C10 119.3(3) . . ? O4 C11 C10 115.0(3) . . ? C11 O3 Cd1 116.8(3) . . ? C11 O4 Cd2 127.4(3) . 4_565 ? C6 N2 C12 109.7(3) . . ? C6 N2 C14 112.9(3) . . ? C12 N2 C14 112.1(3) . . ? C6 N2 Cd1 112.4(2) . . ? C12 N2 Cd1 103.6(2) . . ? C14 N2 Cd1 105.7(2) . . ? N2 C12 C13 111.5(3) . . ? O6 C13 O5 122.7(4) . . ? O6 C13 C12 118.6(3) . . ? O5 C13 C12 118.6(4) . . ? C13 O5 Cd2 97.2(2) . . ? C13 O5 Cd1 100.1(2) . . ? Cd2 O5 Cd1 142.77(13) . . ? C13 O6 Cd2 84.9(2) . . ? N2 C14 C15 115.0(3) . . ? O8 C15 O7 123.2(4) . . ? O8 C15 C14 121.8(3) . . ? O7 C15 C14 114.9(3) . . ? C15 O7 Cd2 131.1(3) . 4_666 ? C15 O8 Cd1 115.3(3) . . ? _diffrn_measured_fraction_theta_max 0.682 _diffrn_reflns_theta_full 34.05 _diffrn_measured_fraction_theta_full 0.682 _refine_diff_density_max 2.217 _refine_diff_density_min -2.694 _refine_diff_density_rms 0.328 #======END