# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 1999 # CCDC Number: 186/1636 data_global _publ_requested_journal 'Dalton, Peper ref.9/03997J' _publ_contact_author ; Wanda Sawka Dobrowolska Faculty of Chemistry University of Wroc\/law Joliot-Curie 14 Str. 50-383 Wroc\/law Poland e-mail wanda@wchuwr.chem.uni.wroc.pl ; loop_ _publ_author_name _publ_author_address 'Ewa Matczak-Jon' ; Institute of Inorganic Chemistry Wroc\/law University of Technology 50-370 Wroc\/law Poland e-mail Jon@ichn.ch.pwr.wroc.pl ; 'Barbara Kurzak' ; Institute of Chemistry Pedagogical University 08-110 Siedlce Poland ; 'Anna Kamecka' ; Institute of Chemistry Pedagogical University 08-110 Siedlce Poland ; 'Wanda Sawka-Dobrowolska' ; Faculty of Chemistry University of Wroc\/law 50-383 Wroc\/law Poland ; 'Pawe\/l Kafarski' ; Institute of Organic Chemistry Biochemistry and Technology Wroc\/law University of Technology 50-370 Wroc\/law Poland ; _pub_setion_title ; Interactions of Zinc(II), Magnesium(II) and Calcium(II) with Iminodi(methylenephosphonic) Acids in Aqueous Solutions ; data_bisfos _audit_creation_method SHELXL-93 _chemical_name_systematic ; N-methyliminodi(methylenephosphonate ; _chemical_formula_moiety 'C3 H11 N O6 P2' _chemical_formula_sum 'C3 H11 N O6 P2' _chemical_formula_weight 219.07 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' _symmetry_cell_setting 'monoclinic' _symmetry_space_group_name_H-M 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 7.290(2) _cell_length_b 8.009(4) _cell_length_c 14.473(2) _cell_angle_alpha 90.00 _cell_angle_beta 93.66(3) _cell_angle_gamma 90.00 _cell_volume 843.3(5) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 15 _cell_measurement_theta_min 9.5 _cell_measurement_theta_max 12.5 _exptl_crystal_description 'platy shape' _exptl_crystal_colour 'colourless' _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_diffrn 1.725 _exptl_crystal_F_000 456 _exptl_absorpt_coefficient_mu 0.510 _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Syntex P21 automatic diffractometer' _diffrn_measurement_method 'profile data from theta/2theta scans' _diffrn_standards_number 2 _diffrn_standards_interval_count 50 _diffrn_standards_decay_% 2.1 _diffrn_reflns_number 1552 _diffrn_reflns_av_sigmaI/netI 0.0124 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.80 _diffrn_reflns_theta_max 26.05 _reflns_number_total 1665 _reflns_number_gt 1552 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Syntex P21 software 1976' _computing_cell_refinement 'Syntex P21 software 1976' _computing_data_reduction 'Syntex P21 software 1976' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'ORTEPII (Johnson, 1976)' _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0573P)^2^+0.4269P] 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 'refall' _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.052(5) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 1552 _refine_ls_number_parameters 154 _refine_ls_number_restraints 0 _refine_ls_R_factor_gt 0.0295 _refine_ls_wR_factor_gt 0.0811 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 # # Table1. Fractional atomic coordination and equivalent isotopic # displacement parameters (\%A^2^) # 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 P1 P 0.22616(5) 0.20140(5) 0.06588(3) 0.01869(17) Uani 1 d . . . P2 P 0.26646(5) -0.08472(5) 0.31264(3) 0.02022(18) Uani 1 d . . . O1 O 0.24354(19) 0.29092(16) 0.16122(9) 0.0271(3) Uani 1 d . . . O2 O 0.34233(18) 0.28282(17) -0.00439(9) 0.0334(3) Uani 1 d . . . O3 O 0.02411(16) 0.18201(15) 0.03833(8) 0.0238(3) Uani 1 d . . . O4 O 0.45900(16) -0.06721(16) 0.28556(8) 0.0270(3) Uani 1 d . . . O5 O 0.1887(2) 0.0526(2) 0.37110(10) 0.0388(4) Uani 1 d . . . O6 O 0.24492(19) -0.25872(18) 0.35982(9) 0.0311(3) Uani 1 d . . . N1 N 0.18758(19) -0.13014(16) 0.11986(9) 0.0177(3) Uani 1 d . . . C1 C 0.3216(2) -0.0077(2) 0.08349(11) 0.0203(3) Uani 1 d . . . C2 C 0.1075(2) -0.0824(2) 0.20928(11) 0.0193(3) Uani 1 d . . . C3 C 0.2663(3) -0.3037(2) 0.12307(14) 0.0279(4) Uani 1 d . . . H1 H 0.335(4) 0.325(4) 0.171(2) 0.053(9) Uiso 1 d . . . H2 H 0.101(3) -0.133(3) 0.0780(14) 0.018(4) Uiso 1 d . . . H6 H 0.166(5) -0.253(4) 0.392(2) 0.071(10) Uiso 1 d . . . H5 H 0.238(6) 0.091(6) 0.423(3) 0.139(19) Uiso 1 d . . . H11 H 0.424(3) -0.003(3) 0.1244(13) 0.020(5) Uiso 1 d . . . H12 H 0.350(3) -0.045(3) 0.0285(16) 0.029(5) Uiso 1 d . . . H21 H 0.017(3) -0.161(3) 0.2167(14) 0.026(5) Uiso 1 d . . . H22 H 0.056(3) 0.025(3) 0.2040(13) 0.020(5) Uiso 1 d . . . H31 H 0.361(3) -0.300(3) 0.1650(18) 0.034(6) Uiso 1 d . . . H32 H 0.163(3) -0.374(3) 0.1347(16) 0.036(6) Uiso 1 d . . . H33 H 0.305(3) -0.341(3) 0.0609(19) 0.046(7) 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 P1 0.0191(3) 0.0188(2) 0.0180(3) 0.00271(14) 0.00009(16) 0.00044(14) P2 0.0205(3) 0.0240(3) 0.0159(2) -0.00140(15) -0.00111(16) -0.00024(15) O1 0.0274(7) 0.0265(7) 0.0271(7) -0.0058(5) -0.0001(5) -0.0037(5) O2 0.0299(7) 0.0392(8) 0.0316(7) 0.0176(6) 0.0060(6) 0.0012(5) O3 0.0210(6) 0.0275(6) 0.0223(6) -0.0031(5) -0.0030(5) 0.0021(5) O4 0.0194(6) 0.0339(7) 0.0272(6) 0.0058(5) -0.0024(5) -0.0025(5) O5 0.0377(8) 0.0443(8) 0.0340(8) -0.0199(6) -0.0020(6) 0.0055(6) O6 0.0315(7) 0.0362(7) 0.0258(7) 0.0111(5) 0.0032(5) 0.0017(6) N1 0.0190(7) 0.0173(6) 0.0163(6) 0.0001(5) -0.0019(5) 0.0008(5) C1 0.0191(8) 0.0229(8) 0.0193(7) 0.0028(6) 0.0042(6) 0.0023(6) C2 0.0168(7) 0.0228(8) 0.0182(8) 0.0015(6) 0.0009(6) 0.0002(6) C3 0.0354(10) 0.0182(8) 0.0298(9) -0.0006(7) -0.0001(8) 0.0058(7) # # Table 2. Selected interatomic distances (\%A) and bond angles (\%) # with e.s.d. in parentheses # 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 P1 O1 1.5531(13) . yes P1 O2 1.5122(13) . yes P1 O3 1.5092(13) . yes P1 C1 1.8248(18) . yes P2 O4 1.4878(13) . yes P2 O5 1.5190(15) . yes P2 O6 1.5642(16) . yes P2 C2 1.8330(17) . yes N1 C2 1.503(2) . yes N1 C1 1.503(2) . yes N1 C3 1.503(2) . yes O1 H1 0.73(3) . ? N1 H2 0.85(2) . ? O5 H5 0.87(5) . ? O6 H6 0.76(3) . ? C1 H11 0.93(2) . ? C1 H12 0.89(2) . ? C2 H21 0.92(2) . ? C2 H22 0.94(2) . ? C3 H31 0.89(3) . ? C3 H32 0.97(2) . ? C3 H33 1.01(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 O3 P1 O2 116.47(8) . . yes O3 P1 O1 107.77(8) . . yes O2 P1 O1 112.40(8) . . yes O3 P1 C1 107.42(7) . . yes O2 P1 C1 105.35(8) . . yes O1 P1 C1 106.90(8) . . yes O4 P2 O5 118.05(8) . . yes O4 P2 O6 108.77(8) . . yes O5 P2 O6 110.50(9) . . yes O4 P2 C2 110.00(7) . . yes O5 P2 C2 102.04(8) . . yes O6 P2 C2 106.82(7) . . yes C2 N1 C1 115.64(13) . . yes C2 N1 C3 112.14(13) . . yes C1 N1 C3 111.03(13) . . yes N1 C1 P1 113.41(11) . . yes C2 N1 H2 108.1(13) . . ? C1 N1 H2 103.6(13) . . ? C3 N1 H2 105.4(14) . . ? N1 C1 H11 108.6(12) . . ? P1 C1 H11 109.9(13) . . ? N1 C1 H12 106.8(14) . . ? P1 C1 H12 107.2(14) . . ? H11 C1 H12 110.9(18) . . ? N1 C2 P2 116.12(11) . . ? N1 C2 H21 104.4(13) . . ? P2 C2 H21 108.5(13) . . ? N1 C2 H22 109.7(11) . . ? P2 C2 H22 107.5(12) . . ? H21 C2 H22 110.6(17) . . ? N1 C3 H31 105.4(15) . . ? N1 C3 H32 104.1(14) . . ? H31 C3 H32 119(2) . . ? N1 C3 H33 112.1(15) . . ? H31 C3 H33 112(2) . . ? H32 C3 H33 105(2) . . ? P1 O1 H1 112(2) . . ? P2 O5 H5 126(3) . . ? P2 O6 H6 108(3) . . ? # # Table 3. Selected torsion angles (\%) # loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C2 N1 C1 P1 -57.02(16) . . . . yes C3 N1 C1 P1 173.75(12) . . . . yes O3 P1 C1 N1 -32.47(13) . . . . yes O2 P1 C1 N1 -157.26(11) . . . . yes O1 P1 C1 N1 82.97(13) . . . . yes C1 N1 C2 P2 -69.06(16) . . . . yes C3 N1 C2 P2 59.63(16) . . . . yes O4 P2 C2 N1 22.70(14) . . . . yes O5 P2 C2 N1 148.81(12) . . . . yes O6 P2 C2 N1 -95.18(12) . . . . yes # # Table 4. Hydrogen bonds and angles (\%A,\%) # 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 O1 H1 O4 0.73(3) 1.81(3) 2.5245(19) 168(3) 2_655 N1 H2 O3 0.85(2) 1.90(2) 2.7101(19) 158.7(19) 3 O6 H6 O3 0.76(3) 1.84(3) 2.5717(19) 160(4) 2_545 O5 H5 O2 0.87(5) 1.61(5) 2.4457(19) 160(5) 4_566 C3 H31 O4 0.89(3) 2.59(2) 3.142(2) 121.0(18) 2_645 C3 H32 O5 0.97(2) 2.62(2) 3.517(3) 153.9(19) 2_545 C3 H33 O2 1.01(3) 2.78(2) 3.427(3) 122.1(18) 3_655 _refine_diff_density_max 0.375 _refine_diff_density_min -0.289 _refine_diff_density_rms 0.065