# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_coden_Cambridge 222 _journal_volume ? _journal_page_first ? _journal_year ? loop_ _publ_author_name 'Ewa Matczak-Jon' 'Pawel Kafarski' 'Teresa Kowalik-Jankowska' 'Anna Rajewska' 'Katarzyna Slepokura' _publ_contact_author_name 'Ewa Matczak-Jon' _publ_contact_author_email EWA.MATCZAK-JON@PWR.WROC.PL _publ_section_title ; pecificity of the zinc(II), magnesium(II) and calcium(II) complexation by (pyridin-2-yl)aminomethane-1,1-diphosphonic acids and related 1,3-(thiazol-2-yl) and 1,3-(benzothiazol-2-yl) derivatives ; # Attachment '5_Mj11abs.cif' data_mj11abs _database_code_depnum_ccdc_archive 'CCDC 741089' _audit_creation_method SHELXL-97 _chemical_name_systematic ; hydrogen phosphono(1,3-thiazol-3-ium-2-ylamino)methylphosphonate ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C4 H8 N2 O6 P2 S' _chemical_formula_weight 274.12 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' S S 0.1246 0.1234 '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' _symmetry_space_group_name_Hall '-P 2ybc' 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 7.354(2) _cell_length_b 9.510(3) _cell_length_c 13.547(4) _cell_angle_alpha 90.00 _cell_angle_beta 91.64(2) _cell_angle_gamma 90.00 _cell_volume 947.0(5) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 14801 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 36.5 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.923 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 560 _exptl_absorpt_coefficient_mu 0.691 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.838 _exptl_absorpt_correction_T_max 0.934 _exptl_absorpt_process_details 'CrysAlis RED; Oxford-Diffraction Poland, 2003' _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 'KUMA KM4CCD kappa-geometry diffractometer' _diffrn_measurement_method omega _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10239 _diffrn_reflns_av_R_equivalents 0.0460 _diffrn_reflns_av_sigmaI/netI 0.0261 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.01 _diffrn_reflns_theta_max 27.00 _reflns_number_total 2068 _reflns_number_gt 1808 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD; Oxford-Diffraction Poland, 2003' _computing_cell_refinement 'CrysAlis RED; Oxford-Diffraction Poland, 2003' _computing_data_reduction 'CrysAlis RED; Oxford-Diffraction Poland, 2003' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0593P)^2^+0.6250P] 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 none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2068 _refine_ls_number_parameters 168 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0428 _refine_ls_R_factor_gt 0.0372 _refine_ls_wR_factor_ref 0.0970 _refine_ls_wR_factor_gt 0.0944 _refine_ls_goodness_of_fit_ref 1.090 _refine_ls_restrained_S_all 1.090 _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 S1 S 0.79749(7) 0.63175(6) 0.56434(4) 0.01531(16) Uani 1 1 d . . . P1 P 0.49466(7) 0.57130(6) 0.85095(4) 0.01158(16) Uani 1 1 d . . . P2 P 0.91610(7) 0.52652(6) 0.85509(4) 0.01384(17) Uani 1 1 d . . . O1 O 0.3549(2) 0.63767(17) 0.78163(11) 0.0157(3) Uani 1 1 d . . . O2 O 0.5316(2) 0.65227(16) 0.94493(11) 0.0141(3) Uani 1 1 d . . . O3 O 0.4408(2) 0.41492(18) 0.87096(13) 0.0162(4) Uani 1 1 d . . . H3 H 0.441(4) 0.399(3) 0.920(2) 0.022(9) Uiso 1 1 d . . . O4 O 0.9640(2) 0.64469(17) 0.92368(12) 0.0164(3) Uani 1 1 d . . . O5 O 0.8774(2) 0.38505(18) 0.90750(14) 0.0212(4) Uani 1 1 d . . . H5 H 0.926(6) 0.373(4) 0.956(3) 0.058(13) Uiso 1 1 d . . . O6 O 1.0561(2) 0.5023(2) 0.77356(13) 0.0229(4) Uani 1 1 d . . . H6 H 1.143(6) 0.551(5) 0.777(3) 0.065(14) Uiso 1 1 d . . . N1 N 0.6822(2) 0.4519(2) 0.70525(14) 0.0132(4) Uani 1 1 d . . . H1N H 0.657(4) 0.374(3) 0.720(2) 0.014(7) Uiso 1 1 d . . . N2 N 0.6836(3) 0.3828(2) 0.53905(14) 0.0151(4) Uani 1 1 d . . . H2N H 0.628(4) 0.315(3) 0.548(2) 0.023(8) Uiso 1 1 d . . . C1 C 0.7061(3) 0.5583(2) 0.78297(16) 0.0135(4) Uani 1 1 d . . . H1 H 0.716(4) 0.644(3) 0.750(2) 0.019(7) Uiso 1 1 d . . . C2 C 0.7154(3) 0.4769(2) 0.61093(16) 0.0123(4) Uani 1 1 d . . . C3 C 0.7847(3) 0.5627(2) 0.44523(17) 0.0165(5) Uani 1 1 d . . . H13 H 0.825(4) 0.610(3) 0.394(2) 0.013(6) Uiso 1 1 d . . . C4 C 0.7230(3) 0.4314(3) 0.44541(16) 0.0155(4) Uani 1 1 d . . . H14 H 0.714(4) 0.370(3) 0.399(2) 0.019(7) Uiso 1 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 S1 0.0161(3) 0.0136(3) 0.0163(3) 0.0002(2) 0.0009(2) -0.0016(2) P1 0.0091(3) 0.0137(3) 0.0118(3) 0.0000(2) -0.0004(2) 0.0001(2) P2 0.0093(3) 0.0177(3) 0.0144(3) -0.0024(2) -0.0025(2) 0.0007(2) O1 0.0096(7) 0.0219(8) 0.0156(8) 0.0012(6) -0.0012(6) 0.0022(6) O2 0.0139(7) 0.0143(8) 0.0139(7) -0.0012(6) 0.0000(6) 0.0002(6) O3 0.0181(8) 0.0166(9) 0.0139(8) 0.0004(7) 0.0025(7) -0.0041(6) O4 0.0149(8) 0.0157(8) 0.0182(8) -0.0012(6) -0.0042(6) -0.0010(6) O5 0.0237(9) 0.0162(9) 0.0231(9) 0.0014(7) -0.0101(7) -0.0002(7) O6 0.0094(7) 0.0374(11) 0.0221(9) -0.0102(8) 0.0011(7) -0.0032(7) N1 0.0133(9) 0.0129(10) 0.0133(9) 0.0018(7) -0.0002(7) -0.0026(7) N2 0.0129(9) 0.0151(10) 0.0173(10) -0.0003(8) -0.0002(7) -0.0023(8) C1 0.0121(10) 0.0146(11) 0.0138(10) -0.0014(8) 0.0000(8) -0.0008(8) C2 0.0078(9) 0.0147(10) 0.0144(10) 0.0001(8) -0.0014(7) 0.0026(8) C3 0.0155(10) 0.0200(12) 0.0142(10) 0.0014(9) 0.0018(8) 0.0031(9) C4 0.0171(11) 0.0184(12) 0.0109(10) -0.0011(9) 0.0001(8) 0.0020(9) _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 S1 C2 1.718(2) . ? S1 C3 1.742(2) . ? P1 O2 1.5058(16) . ? P1 O1 1.5106(16) . ? P1 O3 1.5647(18) . ? P1 C1 1.834(2) . ? P2 O4 1.4939(17) . ? P2 O6 1.5486(18) . ? P2 O5 1.5513(19) . ? P2 C1 1.829(2) . ? O3 H3 0.68(3) . ? O5 H5 0.75(4) . ? O6 H6 0.79(5) . ? N1 C2 1.329(3) . ? N1 C1 1.467(3) . ? N1 H1N 0.79(3) . ? N2 C2 1.338(3) . ? N2 C4 1.388(3) . ? N2 H2N 0.78(3) . ? C1 H1 0.94(3) . ? C3 C4 1.328(3) . ? C3 H13 0.89(3) . ? C4 H14 0.85(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 C2 S1 C3 90.40(11) . . ? O2 P1 O1 114.51(9) . . ? O2 P1 O3 112.34(10) . . ? O1 P1 O3 109.49(10) . . ? O2 P1 C1 108.91(10) . . ? O1 P1 C1 106.72(10) . . ? O3 P1 C1 104.21(10) . . ? O4 P2 O6 113.93(10) . . ? O4 P2 O5 114.25(10) . . ? O6 P2 O5 109.38(11) . . ? O4 P2 C1 112.85(10) . . ? O6 P2 C1 102.24(10) . . ? O5 P2 C1 103.00(10) . . ? P1 O3 H3 113(3) . . ? P2 O5 H5 116(3) . . ? P2 O6 H6 115(3) . . ? C2 N1 C1 123.0(2) . . ? C2 N1 H1N 117(2) . . ? C1 N1 H1N 120(2) . . ? C2 N2 C4 113.9(2) . . ? C2 N2 H2N 122(2) . . ? C4 N2 H2N 123(2) . . ? N1 C1 P2 110.56(15) . . ? N1 C1 P1 108.72(14) . . ? P2 C1 P1 117.26(12) . . ? N1 C1 H1 105.4(17) . . ? P2 C1 H1 108.9(18) . . ? P1 C1 H1 105.2(18) . . ? N1 C2 N2 123.1(2) . . ? N1 C2 S1 125.63(17) . . ? N2 C2 S1 111.21(16) . . ? C4 C3 S1 111.22(18) . . ? C4 C3 H13 127.0(17) . . ? S1 C3 H13 121.6(17) . . ? C3 C4 N2 113.3(2) . . ? C3 C4 H14 131.2(19) . . ? N2 C4 H14 115.2(19) . . ? 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 P2 -103.0(2) . . . . ? C2 N1 C1 P1 126.94(19) . . . . ? O4 P2 C1 N1 170.13(14) . . . . ? O6 P2 C1 N1 47.31(17) . . . . ? O5 P2 C1 N1 -66.18(17) . . . . ? O4 P2 C1 P1 -64.50(15) . . . . ? O6 P2 C1 P1 172.68(13) . . . . ? O5 P2 C1 P1 59.19(15) . . . . ? O2 P1 C1 N1 166.25(14) . . . . ? O1 P1 C1 N1 -69.64(16) . . . . ? O3 P1 C1 N1 46.18(17) . . . . ? O2 P1 C1 P2 39.97(15) . . . . ? O1 P1 C1 P2 164.08(12) . . . . ? O3 P1 C1 P2 -80.10(14) . . . . ? C1 N1 C2 N2 -175.95(19) . . . . ? C1 N1 C2 S1 2.4(3) . . . . ? C4 N2 C2 N1 178.3(2) . . . . ? C4 N2 C2 S1 -0.2(2) . . . . ? C3 S1 C2 N1 -178.2(2) . . . . ? C3 S1 C2 N2 0.34(16) . . . . ? C2 S1 C3 C4 -0.36(18) . . . . ? S1 C3 C4 N2 0.3(3) . . . . ? C2 N2 C4 C3 0.0(3) . . . . ? 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 O3 H3 O2 0.68(3) 1.90(3) 2.577(2) 173(4) 3_667 O5 H5 O4 0.75(4) 1.80(4) 2.553(2) 176(5) 3_767 O6 H6 O1 0.79(5) 1.76(5) 2.546(2) 172(5) 1_655 N1 H1N O1 0.79(3) 2.25(3) 3.007(3) 161(3) 2_646 N2 H2N O2 0.78(3) 1.95(3) 2.716(3) 172(3) 2_646 C1 H1 S1 0.94(3) 2.60(3) 3.135(2) 117(2) . C3 H13 O4 0.89(3) 2.57(3) 3.097(3) 119(2) 4_575 C3 H13 O6 0.89(3) 2.68(3) 3.277(3) 126(2) 3_766 C4 H14 O1 0.85(3) 2.49(3) 3.181(3) 139(2) 3_666 C4 H14 O5 0.85(3) 2.71(3) 3.263(3) 124(2) 4_565 _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.62 _refine_diff_density_min -0.43 _refine_diff_density_rms 0.10 # Attachment '6_Emjsabs.cif' data_emjsabs _database_code_depnum_ccdc_archive 'CCDC 741090' _audit_creation_method SHELXL-97 _chemical_name_systematic ; oxonium chloride compound with hydrogen (1,3-benzothiazol-3-ium-2-ylamino)(phosphono)methylphosphonate (1:1) 1.3 hydrate ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C8 H15.60 Cl N2 O8.30 P2 S' _chemical_formula_weight 402.07 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P n a 21' _symmetry_space_group_name_Hall 'P 2c -2n' 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' _cell_length_a 7.231(2) _cell_length_b 16.087(3) _cell_length_c 13.728(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1596.9(6) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 11372 _cell_measurement_theta_min 4.7 _cell_measurement_theta_max 35.1 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.668 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 824 _exptl_absorpt_coefficient_mu 0.611 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.903 _exptl_absorpt_correction_T_max 0.989 _exptl_absorpt_process_details 'CrysAlis RED; Oxford-Diffraction Poland, 2003' _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 'Xcalibur PX kappa-geometry diffractometer with Onyx CCD camera' _diffrn_measurement_method 'omega and phi' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 26569 _diffrn_reflns_av_R_equivalents 0.0756 _diffrn_reflns_av_sigmaI/netI 0.0769 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 4.73 _diffrn_reflns_theta_max 28.98 _reflns_number_total 4217 _reflns_number_gt 3813 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD; Oxford-Diffraction Poland, 2003' _computing_cell_refinement 'CrysAlis RED; Oxford-Diffraction Poland, 2003' _computing_data_reduction 'CrysAlis RED; Oxford-Diffraction Poland, 2003' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0379P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens mixed _refine_ls_hydrogen_treatment constr _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 -0.02(9) _refine_ls_number_reflns 4217 _refine_ls_number_parameters 224 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0839 _refine_ls_R_factor_gt 0.0697 _refine_ls_wR_factor_ref 0.1023 _refine_ls_wR_factor_gt 0.0979 _refine_ls_goodness_of_fit_ref 1.155 _refine_ls_restrained_S_all 1.155 _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 Cl1 Cl 0.38612(14) 0.41942(6) 0.56499(8) 0.0257(2) Uani 1 1 d . . . S1 S 0.55478(14) 0.38648(6) 0.16335(7) 0.0190(2) Uani 1 1 d . . . P1 P 0.70446(14) 0.62350(6) 0.40052(7) 0.0147(2) Uani 1 1 d . . . P2 P 0.27773(13) 0.62198(6) 0.36066(8) 0.0153(2) Uani 1 1 d . . . O1 O 0.8416(4) 0.55686(17) 0.4313(2) 0.0224(7) Uani 1 1 d . . . O2 O 0.6615(4) 0.69010(17) 0.4720(2) 0.0215(7) Uani 1 1 d . . . O3 O 0.7725(4) 0.65752(18) 0.30024(18) 0.0197(7) Uani 1 1 d . . . H3 H 0.7659 0.7097 0.3002 0.030 Uiso 1 1 calc R . . O4 O 0.2903(4) 0.68408(17) 0.27962(19) 0.0196(7) Uani 1 1 d . . . O5 O 0.1423(4) 0.55059(17) 0.3376(2) 0.0253(7) Uani 1 1 d . . . H5 H 0.0512 0.5532 0.3755 0.038 Uiso 1 1 calc R . . O6 O 0.2315(4) 0.65918(17) 0.46040(19) 0.0184(6) Uani 1 1 d . . . H6 H 0.2136 0.7105 0.4546 0.028 Uiso 1 1 calc R . . N1 N 0.5252(4) 0.51799(19) 0.2829(2) 0.0140(7) Uani 1 1 d . . . H1N H 0.5547 0.5464 0.2304 0.017 Uiso 1 1 calc R . . N2 N 0.4766(4) 0.38262(18) 0.3463(2) 0.0162(7) Uani 1 1 d . . . H2N H 0.4499 0.3986 0.4060 0.019 Uiso 1 1 calc R . . C1 C 0.4931(5) 0.5652(2) 0.3715(3) 0.0126(7) Uani 1 1 d . . . H1 H 0.4755 0.5238 0.4250 0.015 Uiso 1 1 calc R . . C2 C 0.5142(5) 0.4361(2) 0.2738(3) 0.0125(8) Uani 1 1 d . . . C3 C 0.5275(5) 0.2893(2) 0.2200(3) 0.0154(8) Uani 1 1 d . . . C4 C 0.4838(5) 0.2996(2) 0.3180(3) 0.0169(9) Uani 1 1 d . . . C5 C 0.4553(5) 0.2313(2) 0.3786(3) 0.0227(10) Uani 1 1 d . . . H15 H 0.4228 0.2382 0.4451 0.027 Uiso 1 1 calc R . . C6 C 0.4758(5) 0.1537(3) 0.3385(3) 0.0253(10) Uani 1 1 d . . . H16 H 0.4575 0.1060 0.3780 0.030 Uiso 1 1 calc R . . C7 C 0.5229(6) 0.1437(2) 0.2414(4) 0.0255(10) Uani 1 1 d . . . H17 H 0.5380 0.0891 0.2162 0.031 Uiso 1 1 calc R . . C8 C 0.5485(5) 0.2111(3) 0.1798(3) 0.0228(9) Uani 1 1 d . . . H18 H 0.5791 0.2039 0.1130 0.027 Uiso 1 1 calc R . . O1W O 0.9684(6) 0.4768(3) 0.5830(3) 0.0281(12) Uani 0.709(6) 1 d PD A 1 H1W H 1.0853(18) 0.475(4) 0.572(5) 0.031(18) Uiso 0.709(6) 1 d PD A 1 H2W H 0.917(9) 0.506(3) 0.538(3) 0.04(2) Uiso 0.709(6) 1 d PD A 1 O2W O 0.8101(9) 0.3454(3) 0.6044(4) 0.065(2) Uani 0.709(6) 1 d P A 1 O10W O 0.7890(13) 0.4708(6) 0.5847(8) 0.027(3) Uiso 0.291(6) 1 d P A 2 O20W O 1.0144(13) 0.3628(6) 0.6264(7) 0.025(3) Uiso 0.291(6) 1 d P A 2 O3W O 1.1535(12) 0.2542(6) 0.5952(7) 0.034(4) Uiso 0.326(11) 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 Cl1 0.0329(6) 0.0293(6) 0.0148(5) -0.0004(5) 0.0013(5) -0.0042(5) S1 0.0240(5) 0.0185(5) 0.0144(5) -0.0031(4) 0.0016(5) 0.0009(4) P1 0.0156(5) 0.0151(5) 0.0133(5) 0.0016(5) 0.0009(4) -0.0029(4) P2 0.0148(5) 0.0142(5) 0.0168(5) 0.0003(5) -0.0004(4) 0.0022(4) O1 0.0184(15) 0.0245(16) 0.0242(16) 0.0075(13) -0.0045(12) 0.0002(12) O2 0.0296(16) 0.0205(16) 0.0144(14) 0.0009(12) 0.0036(12) -0.0079(13) O3 0.0265(16) 0.0178(16) 0.0149(16) -0.0015(13) 0.0046(12) -0.0009(14) O4 0.0302(17) 0.0128(14) 0.0159(15) -0.0013(12) -0.0042(13) 0.0064(12) O5 0.0156(15) 0.0224(16) 0.038(2) -0.0069(14) 0.0010(13) 0.0010(12) O6 0.0251(16) 0.0134(15) 0.0167(15) 0.0024(13) 0.0030(12) 0.0039(13) N1 0.0198(17) 0.0136(16) 0.0086(15) 0.0006(13) 0.0011(14) -0.0017(14) N2 0.0172(16) 0.0146(16) 0.0168(18) -0.0078(14) 0.0018(14) 0.0014(14) C1 0.0163(17) 0.0084(16) 0.0132(19) -0.0014(17) 0.0019(15) -0.0009(16) C2 0.0069(18) 0.019(2) 0.012(2) -0.0016(16) -0.0001(15) 0.0019(15) C3 0.0102(19) 0.017(2) 0.019(2) -0.0019(16) -0.0003(16) -0.0003(15) C4 0.014(2) 0.021(2) 0.016(2) -0.0025(17) -0.0026(16) -0.0006(17) C5 0.022(2) 0.024(2) 0.022(2) 0.0000(19) 0.0035(19) -0.0025(17) C6 0.019(2) 0.019(2) 0.038(3) 0.002(2) 0.003(2) -0.0001(17) C7 0.024(2) 0.011(2) 0.041(3) -0.009(2) -0.003(2) -0.0009(17) C8 0.019(2) 0.025(2) 0.024(2) -0.0110(19) 0.0010(19) 0.0010(17) O1W 0.027(3) 0.033(3) 0.024(3) 0.002(2) 0.000(2) 0.012(2) O2W 0.105(5) 0.064(4) 0.027(3) -0.010(3) 0.020(3) -0.049(3) _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 S1 C2 1.738(4) . ? S1 C3 1.758(4) . ? P1 O2 1.486(3) . ? P1 O1 1.520(3) . ? P1 O3 1.561(3) . ? P1 C1 1.837(4) . ? P2 O4 1.498(3) . ? P2 O6 1.531(3) . ? P2 O5 1.542(3) . ? P2 C1 1.812(4) . ? O3 H3 0.84 . ? O5 H5 0.84 . ? O6 H6 0.84 . ? N1 C2 1.326(5) . ? N1 C1 1.452(5) . ? N1 H1N 0.88 . ? N2 C2 1.343(5) . ? N2 C4 1.392(5) . ? N2 H2N 0.88 . ? C1 H1 1.00 . ? C3 C8 1.381(5) . ? C3 C4 1.391(5) . ? C4 C5 1.393(6) . ? C5 C6 1.372(5) . ? C5 H15 0.95 . ? C6 C7 1.385(7) . ? C6 H16 0.95 . ? C7 C8 1.387(6) . ? C7 H17 0.95 . ? C8 H18 0.95 . ? O1W H1W 0.86 . ? O1W H2W 0.86 . ? 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 C2 S1 C3 90.19(18) . . ? O2 P1 O1 117.50(17) . . ? O2 P1 O3 113.31(16) . . ? O1 P1 O3 106.65(17) . . ? O2 P1 C1 109.72(17) . . ? O1 P1 C1 104.06(16) . . ? O3 P1 C1 104.45(17) . . ? O4 P2 O6 114.62(15) . . ? O4 P2 O5 112.52(17) . . ? O6 P2 O5 109.61(17) . . ? O4 P2 C1 110.17(17) . . ? O6 P2 C1 108.15(17) . . ? O5 P2 C1 100.81(15) . . ? P1 O3 H3 109.5 . . ? P2 O5 H5 109.5 . . ? P2 O6 H6 109.5 . . ? C2 N1 C1 126.1(3) . . ? C2 N1 H1N 116.9 . . ? C1 N1 H1N 116.9 . . ? C2 N2 C4 113.5(3) . . ? C2 N2 H2N 123.2 . . ? C4 N2 H2N 123.2 . . ? N1 C1 P2 109.4(3) . . ? N1 C1 P1 108.4(3) . . ? P2 C1 P1 118.40(18) . . ? N1 C1 H1 106.7 . . ? P2 C1 H1 106.7 . . ? P1 C1 H1 106.7 . . ? N1 C2 N2 125.3(3) . . ? N1 C2 S1 121.9(3) . . ? N2 C2 S1 112.8(3) . . ? C8 C3 C4 121.3(4) . . ? C8 C3 S1 128.3(3) . . ? C4 C3 S1 110.3(3) . . ? C3 C4 N2 113.1(3) . . ? C3 C4 C5 121.1(4) . . ? N2 C4 C5 125.8(4) . . ? C6 C5 C4 117.5(4) . . ? C6 C5 H15 121.3 . . ? C4 C5 H15 121.3 . . ? C5 C6 C7 121.2(4) . . ? C5 C6 H16 119.4 . . ? C7 C6 H16 119.4 . . ? C6 C7 C8 121.9(4) . . ? C6 C7 H17 119.1 . . ? C8 C7 H17 119.1 . . ? C3 C8 C7 117.0(4) . . ? C3 C8 H18 121.5 . . ? C7 C8 H18 121.5 . . ? H1W O1W H2W 108(7) . . ? 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 P2 -108.8(3) . . . . ? C2 N1 C1 P1 120.7(3) . . . . ? O4 P2 C1 N1 -63.3(3) . . . . ? O6 P2 C1 N1 170.7(2) . . . . ? O5 P2 C1 N1 55.7(3) . . . . ? O4 P2 C1 P1 61.5(3) . . . . ? O6 P2 C1 P1 -64.5(3) . . . . ? O5 P2 C1 P1 -179.4(2) . . . . ? O2 P1 C1 N1 163.6(2) . . . . ? O1 P1 C1 N1 -69.8(3) . . . . ? O3 P1 C1 N1 41.9(3) . . . . ? O2 P1 C1 P2 38.3(3) . . . . ? O1 P1 C1 P2 164.8(2) . . . . ? O3 P1 C1 P2 -83.5(3) . . . . ? C1 N1 C2 N2 -2.1(6) . . . . ? C1 N1 C2 S1 179.7(2) . . . . ? C4 N2 C2 N1 -176.5(3) . . . . ? C4 N2 C2 S1 1.8(4) . . . . ? C3 S1 C2 N1 176.3(3) . . . . ? C3 S1 C2 N2 -2.1(3) . . . . ? C2 S1 C3 C8 -176.5(4) . . . . ? C2 S1 C3 C4 1.8(3) . . . . ? C8 C3 C4 N2 177.3(3) . . . . ? S1 C3 C4 N2 -1.2(4) . . . . ? C8 C3 C4 C5 -1.5(6) . . . . ? S1 C3 C4 C5 180.0(3) . . . . ? C2 N2 C4 C3 -0.3(5) . . . . ? C2 N2 C4 C5 178.4(3) . . . . ? C3 C4 C5 C6 1.4(6) . . . . ? N2 C4 C5 C6 -177.3(4) . . . . ? C4 C5 C6 C7 -0.1(6) . . . . ? C5 C6 C7 C8 -1.0(6) . . . . ? C4 C3 C8 C7 0.4(6) . . . . ? S1 C3 C8 C7 178.6(3) . . . . ? C6 C7 C8 C3 0.9(6) . . . . ? 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 O3 H3 O4 0.84 1.74 2.567(4) 167 3_565 O5 H5 O1 0.84 1.70 2.527(4) 168 1_455 O6 H6 O2 0.84 1.66 2.482(4) 166 3_465 N1 H1N Cl1 0.88 2.38 3.221(3) 161 2_664 N2 H2N Cl1 0.88 2.26 3.129(3) 172 . O1W H1W Cl1 0.86 2.35 3.168(4) 158 1_655 O1W H2W O1 0.86 1.76 2.615(5) 170 . C1 H1 Cl1 1.00 2.63 3.627(4) 173 . C5 H15 O2W 0.95 2.69 3.499(6) 143 3_455 C5 H15 O3W 0.95 2.65 3.31(1) 127 3_455 C7 H17 O1W 0.95 2.57 3.455(6) 155 4_644 C8 H18 O2 0.95 2.70 3.557(5) 150 4_644 _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 28.98 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.71 _refine_diff_density_min -0.36 _refine_diff_density_rms 0.09 # start Validation Reply Form _vrf_PLAT430_emjsabs ; PROBLEM: Short Inter D...A Contact O10W .. O20W .. 2.45 Ang. RESPONSE: Pair of oxygen atoms: O1W - O2W and O10W - O20W are involved in formation of disordered Zundel cation [H5O2]+, in which the O...O distance of 2.45 A is correct. Most of the hydrogen atoms in the disordered Zundel cation have not been found. ; # end Validation Reply Form