data_global #=========================================================================== # 1. SUBMISSION DETAILS _journal_coden_Cambridge 222 _publ_contact_author_name 'R. Van Eldik' _publ_contact_author_address ; Institute for Inorganic Chemistry University of Erlangen-Nurnberg Egerlandstr. 1 Erlangen 91058 GERMANY ; _publ_contact_author_phone '049 9131 852-7350' _publ_contact_author_fax '049 9131 852-7387' _publ_contact_author_email VANELDIK@CHEMIE.UNI-ERLANGEN.DE _publ_requested_journal 'Dalton Trans.' _publ_requested_coeditor_name ? _publ_section_title ; Kinetics and mechanism of the reactions of Pd(II) complexes with azoles and diazines. Crystal structure of [Pd(bpma)(H2O)](ClO4)2 * H2O ; loop_ _publ_author_name _publ_author_address 'Bugarcic, Z. D.' ; Department of Chemistry Faculty of Science University of Kragujevac P.O. Box 60 34000 Kragujevac Serbia ; 'Nandibewoor, S. T.' ; Institut fur Anorganische Chemie Universitat Erlangen-Nurnberg Egerlandstr. 1 D-91058 Erlangen Bundesrepublik Deutschland ; 'Hamza, M. S. A.' ; Institut fur Anorganische Chemie Universitat Erlangen-Nurnberg Egerlandstr. 1 D-91058 Erlangen Bundesrepublik Deutschland ; 'Heinemann, F. W.' ; Institut fur Anorganische Chemie Universitat Erlangen-Nurnberg Egerlandstr. 1 D-91058 Erlangen Bundesrepublik Deutschland ; 'van Eldik, R.' ; Institut fur Anorganische Chemie Universitat Erlangen-Nurnberg Egerlandstr. 1 D-91058 Erlangen Bundesrepublik Deutschland ; #=========================================================================== _publ_section_experimental ; source of material: see actual publication ; data_zb0502 _database_code_depnum_ccdc_archive 'CCDC 295150' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C12 H15 N3 O Pd, 2(Cl O4), 2(H2 O)' _chemical_formula_sum 'C12 H19 Cl2 N3 O11 Pd' _chemical_formula_weight 558.60 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c _symmetry_space_group_name_Hall -P2ybc 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 7.7436(5) _cell_length_b 14.722(2) _cell_length_c 16.942(2) _cell_angle_alpha 90.00 _cell_angle_beta 100.370(6) _cell_angle_gamma 90.00 _cell_volume 1899.9(4) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 209 _cell_measurement_theta_min 6.00 _cell_measurement_theta_max 20.00 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.953 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1120 _exptl_absorpt_coefficient_mu 1.323 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.841 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details 'SADABS, Bruker AXS, 2002' _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 'Bruker-Nonius KappaCCD' _diffrn_measurement_method ; \w-rotations with 2.00 \% and 144 sec per frame ; _diffrn_detector_area_resol_mean 9 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 43598 _diffrn_reflns_av_R_equivalents 0.0410 _diffrn_reflns_av_sigmaI/netI 0.0184 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.43 _diffrn_reflns_theta_max 26.37 _reflns_number_total 3876 _reflns_number_gt 3523 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Bruker-Nonius, 2002)' _computing_cell_refinement 'EVALCCD (Duisenberg, 2003)' _computing_data_reduction 'EVALCCD (Duisenberg, 2003)' _computing_structure_solution 'SHELXTL 6.12 (Bruker AXS, 2002)' _computing_structure_refinement 'SHELXTL 6.12 (Bruker AXS, 2002)' _computing_molecular_graphics 'SHELXTL 6.12 (Bruker AXS, 2002)' _computing_publication_material 'SHELXTL 6.12 (Bruker AXS, 2002)' _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^)+(0.0000P)^2^+17.1169P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens 'geom except O bound H difmap' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3876 _refine_ls_number_parameters 290 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0583 _refine_ls_R_factor_gt 0.0522 _refine_ls_wR_factor_ref 0.1195 _refine_ls_wR_factor_gt 0.1174 _refine_ls_goodness_of_fit_ref 1.329 _refine_ls_restrained_S_all 1.328 _refine_ls_shift/su_max 0.001 _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 Pd1 Pd 0.95758(6) 0.32493(3) 0.70249(3) 0.01845(13) Uani 1 1 d . . . O1 O 0.8273(8) 0.2786(4) 0.5943(3) 0.0484(15) Uani 1 1 d . . . H1A H 0.8916 0.2251 0.5960 0.073 Uiso 1 1 d D . . H1B H 0.8226 0.3047 0.5504 0.073 Uiso 1 1 d D . . N1 N 1.1788(7) 0.3707(3) 0.6698(3) 0.0217(11) Uani 1 1 d . . . N2 N 1.0698(6) 0.3685(4) 0.8086(3) 0.0241(11) Uani 1 1 d . . . H2 H 1.1286 0.3194 0.8355 0.029 Uiso 1 1 calc R . . N3 N 0.7594(6) 0.2932(3) 0.7592(3) 0.0216(11) Uani 1 1 d . . . C1 C 1.2362(9) 0.3545(5) 0.6001(4) 0.0296(14) Uani 1 1 d . . . H1C H 1.1669 0.3176 0.5605 0.036 Uiso 1 1 calc R . . C2 C 1.3904(10) 0.3894(5) 0.5847(4) 0.0368(17) Uani 1 1 d . . . H2C H 1.4256 0.3786 0.5346 0.044 Uiso 1 1 calc R . . C3 C 1.4938(9) 0.4404(5) 0.6429(5) 0.0376(18) Uani 1 1 d . . . H3C H 1.6031 0.4637 0.6339 0.045 Uiso 1 1 calc R . . C4 C 1.4376(8) 0.4574(4) 0.7147(4) 0.0281(15) Uani 1 1 d . . . H4A H 1.5067 0.4939 0.7546 0.034 Uiso 1 1 calc R . . C5 C 1.2802(8) 0.4211(4) 0.7279(4) 0.0218(13) Uani 1 1 d . . . C6 C 1.2046(8) 0.4389(4) 0.8013(4) 0.0247(13) Uani 1 1 d . . . H6A H 1.1502 0.5000 0.7980 0.030 Uiso 1 1 calc R . . H6B H 1.2989 0.4372 0.8493 0.030 Uiso 1 1 calc R . . C7 C 0.9292(8) 0.3955(5) 0.8538(4) 0.0269(14) Uani 1 1 d . . . H7A H 0.8900 0.4583 0.8394 0.032 Uiso 1 1 calc R . . H7B H 0.9752 0.3934 0.9122 0.032 Uiso 1 1 calc R . . C8 C 0.7780(8) 0.3314(4) 0.8332(4) 0.0241(13) Uani 1 1 d . . . C9 C 0.6601(8) 0.3117(5) 0.8834(4) 0.0307(15) Uani 1 1 d . . . H9A H 0.6751 0.3377 0.9355 0.037 Uiso 1 1 calc R . . C10 C 0.5210(8) 0.2544(5) 0.8573(5) 0.0373(18) Uani 1 1 d . . . H10A H 0.4390 0.2406 0.8911 0.045 Uiso 1 1 calc R . . C11 C 0.5022(8) 0.2170(5) 0.7812(5) 0.0333(16) Uani 1 1 d . . . H11A H 0.4058 0.1783 0.7617 0.040 Uiso 1 1 calc R . . C12 C 0.6244(8) 0.2366(4) 0.7342(4) 0.0257(13) Uani 1 1 d . . . H12A H 0.6133 0.2093 0.6827 0.031 Uiso 1 1 calc R . . Cl1 Cl 0.93026(18) 0.60382(10) 0.64324(9) 0.0222(3) Uani 1 1 d . . . O11 O 0.8692(7) 0.6900(3) 0.6086(3) 0.0397(12) Uani 1 1 d . . . O12 O 0.8618(8) 0.5857(5) 0.7141(3) 0.0606(19) Uani 1 1 d . . . O13 O 1.1177(5) 0.6045(3) 0.6627(3) 0.0307(11) Uani 1 1 d . . . O14 O 0.8767(8) 0.5346(4) 0.5856(4) 0.0520(15) Uani 1 1 d . . . Cl2 Cl 0.3379(3) 0.09488(12) 0.55470(10) 0.0447(5) Uani 1 1 d . . . O21 O 0.2628(11) 0.1354(6) 0.6164(4) 0.085(3) Uani 1 1 d . A . O22 O 0.359(3) 0.1542(11) 0.4967(15) 0.073(8) Uani 0.51(2) 1 d P A 1 O23 O 0.192(2) 0.0344(11) 0.5147(8) 0.066(5) Uani 0.51(2) 1 d P A 1 O24 O 0.4568(19) 0.0483(10) 0.6006(8) 0.058(5) Uani 0.51(2) 1 d P A 1 O22' O 0.290(4) 0.139(2) 0.4868(13) 0.107(12) Uani 0.49(2) 1 d P A 2 O23' O 0.322(5) -0.0002(12) 0.5423(17) 0.129(14) Uani 0.49(2) 1 d P A 2 O24' O 0.5456(16) 0.1006(16) 0.5708(8) 0.079(7) Uani 0.49(2) 1 d P A 2 O2 O 0.7366(7) 0.1036(4) 0.9813(3) 0.0380(12) Uani 1 1 d . . . H2A H 0.7657 0.0567 1.0088 0.057 Uiso 1 1 d . . . H2B H 0.7999 0.0928 0.9441 0.057 Uiso 1 1 d . . . O3 O 0.8913(9) 0.1112(4) 0.5815(4) 0.091(3) Uani 1 1 d D . . H3A H 1.0149 0.1082 0.5831 0.136 Uiso 1 1 d D . . H3B H 0.8539 0.0691 0.5394 0.136 Uiso 1 1 d 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 Pd1 0.0208(2) 0.0150(2) 0.0188(2) 0.00016(18) 0.00154(16) -0.00240(18) O1 0.074(4) 0.037(3) 0.028(3) -0.006(2) -0.008(3) -0.007(3) N1 0.023(3) 0.017(2) 0.026(3) 0.006(2) 0.005(2) 0.005(2) N2 0.015(2) 0.027(3) 0.031(3) -0.001(2) 0.005(2) -0.002(2) N3 0.019(2) 0.020(2) 0.024(3) 0.007(2) -0.001(2) -0.002(2) C1 0.033(4) 0.028(3) 0.030(3) 0.008(3) 0.010(3) 0.008(3) C2 0.034(4) 0.046(4) 0.035(4) 0.017(3) 0.019(3) 0.015(3) C3 0.023(3) 0.040(4) 0.054(5) 0.029(4) 0.017(3) 0.010(3) C4 0.018(3) 0.018(3) 0.050(4) 0.009(3) 0.009(3) 0.002(2) C5 0.018(3) 0.014(3) 0.034(3) 0.007(2) 0.005(2) 0.005(2) C6 0.019(3) 0.022(3) 0.032(3) -0.004(3) 0.002(3) -0.002(2) C7 0.020(3) 0.033(4) 0.028(3) -0.006(3) 0.004(3) 0.001(3) C8 0.020(3) 0.025(3) 0.027(3) 0.006(3) 0.003(2) 0.002(3) C9 0.021(3) 0.043(4) 0.030(3) 0.012(3) 0.007(3) 0.008(3) C10 0.016(3) 0.044(4) 0.053(5) 0.026(4) 0.010(3) 0.004(3) C11 0.015(3) 0.028(3) 0.055(5) 0.018(3) -0.001(3) -0.001(3) C12 0.021(3) 0.020(3) 0.033(3) 0.007(3) -0.004(3) 0.001(2) Cl1 0.0181(7) 0.0209(7) 0.0266(7) -0.0017(6) 0.0010(6) 0.0029(6) O11 0.038(3) 0.026(3) 0.049(3) -0.002(2) -0.008(2) 0.012(2) O12 0.045(3) 0.101(5) 0.042(3) 0.026(3) 0.025(3) 0.026(3) O13 0.016(2) 0.035(3) 0.040(3) 0.008(2) 0.0018(19) 0.0031(19) O14 0.055(4) 0.039(3) 0.055(4) -0.016(3) -0.009(3) -0.010(3) Cl2 0.0875(15) 0.0229(8) 0.0209(8) 0.0003(6) 0.0019(9) -0.0160(9) O21 0.119(7) 0.100(6) 0.045(4) -0.035(4) 0.039(4) -0.046(5) O22 0.103(17) 0.032(7) 0.105(18) 0.044(8) 0.077(15) 0.021(8) O23 0.084(11) 0.049(9) 0.050(8) -0.017(6) -0.027(7) -0.012(8) O24 0.046(9) 0.070(10) 0.051(8) 0.018(7) -0.009(6) 0.026(7) O22' 0.10(2) 0.19(3) 0.022(8) 0.037(12) -0.001(11) 0.037(17) O23' 0.23(3) 0.032(9) 0.16(2) -0.020(11) 0.14(3) -0.056(14) O24' 0.021(6) 0.17(2) 0.044(8) -0.029(10) 0.000(6) 0.000(9) O2 0.044(3) 0.036(3) 0.036(3) 0.006(2) 0.013(2) 0.006(2) O3 0.163(9) 0.041(4) 0.064(5) 0.002(3) 0.012(5) 0.019(5) _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 Pd1 N2 1.958(5) . ? Pd1 N3 2.007(5) . ? Pd1 N1 2.009(5) . ? Pd1 O1 2.043(5) . ? O1 H1A 0.9291 . ? O1 H1B 0.8323 . ? N1 C1 1.357(8) . ? N1 C5 1.362(8) . ? N2 C6 1.491(8) . ? N2 C7 1.494(8) . ? N2 H2 0.9300 . ? N3 C12 1.345(8) . ? N3 C8 1.358(8) . ? C1 C2 1.367(10) . ? C1 H1C 0.9500 . ? C2 C3 1.375(11) . ? C2 H2C 0.9500 . ? C3 C4 1.387(10) . ? C3 H3C 0.9500 . ? C4 C5 1.385(8) . ? C4 H4A 0.9500 . ? C5 C6 1.491(9) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.495(9) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C9 1.386(9) . ? C9 C10 1.378(10) . ? C9 H9A 0.9500 . ? C10 C11 1.386(11) . ? C10 H10A 0.9500 . ? C11 C12 1.372(9) . ? C11 H11A 0.9500 . ? C12 H12A 0.9500 . ? Cl1 O14 1.421(5) . ? Cl1 O12 1.422(5) . ? Cl1 O13 1.429(4) . ? Cl1 O11 1.442(5) . ? Cl2 O24 1.290(10) . ? Cl2 O22' 1.32(2) . ? Cl2 O22 1.346(17) . ? Cl2 O21 1.416(7) . ? Cl2 O23' 1.418(16) . ? Cl2 O23 1.501(13) . ? Cl2 O24' 1.584(13) . ? O2 H2A 0.8411 . ? O2 H2B 0.8800 . ? O3 H3A 0.9531 . ? O3 H3B 0.9500 . ? 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 N2 Pd1 N3 83.6(2) . . ? N2 Pd1 N1 83.3(2) . . ? N3 Pd1 N1 166.8(2) . . ? N2 Pd1 O1 176.7(2) . . ? N3 Pd1 O1 93.1(2) . . ? N1 Pd1 O1 100.0(2) . . ? Pd1 O1 H1A 94.6 . . ? Pd1 O1 H1B 125.6 . . ? H1A O1 H1B 110.8 . . ? C1 N1 C5 119.2(6) . . ? C1 N1 Pd1 127.6(5) . . ? C5 N1 Pd1 113.1(4) . . ? C6 N2 C7 116.3(5) . . ? C6 N2 Pd1 110.7(4) . . ? C7 N2 Pd1 108.3(4) . . ? C6 N2 H2 107.0 . . ? C7 N2 H2 107.0 . . ? Pd1 N2 H2 107.0 . . ? C12 N3 C8 119.7(5) . . ? C12 N3 Pd1 127.7(5) . . ? C8 N3 Pd1 112.5(4) . . ? N1 C1 C2 122.3(7) . . ? N1 C1 H1C 118.9 . . ? C2 C1 H1C 118.9 . . ? C1 C2 C3 119.0(7) . . ? C1 C2 H2C 120.5 . . ? C3 C2 H2C 120.5 . . ? C2 C3 C4 119.6(6) . . ? C2 C3 H3C 120.2 . . ? C4 C3 H3C 120.2 . . ? C5 C4 C3 119.7(7) . . ? C5 C4 H4A 120.1 . . ? C3 C4 H4A 120.1 . . ? N1 C5 C4 120.2(6) . . ? N1 C5 C6 115.9(5) . . ? C4 C5 C6 123.8(6) . . ? C5 C6 N2 109.4(5) . . ? C5 C6 H6A 109.8 . . ? N2 C6 H6A 109.8 . . ? C5 C6 H6B 109.8 . . ? N2 C6 H6B 109.8 . . ? H6A C6 H6B 108.2 . . ? N2 C7 C8 109.0(5) . . ? N2 C7 H7A 109.9 . . ? C8 C7 H7A 109.9 . . ? N2 C7 H7B 109.9 . . ? C8 C7 H7B 109.9 . . ? H7A C7 H7B 108.3 . . ? N3 C8 C9 120.6(6) . . ? N3 C8 C7 115.2(5) . . ? C9 C8 C7 124.3(6) . . ? C10 C9 C8 119.7(7) . . ? C10 C9 H9A 120.2 . . ? C8 C9 H9A 120.2 . . ? C9 C10 C11 119.1(6) . . ? C9 C10 H10A 120.5 . . ? C11 C10 H10A 120.5 . . ? C12 C11 C10 119.3(6) . . ? C12 C11 H11A 120.3 . . ? C10 C11 H11A 120.3 . . ? N3 C12 C11 121.7(6) . . ? N3 C12 H12A 119.2 . . ? C11 C12 H12A 119.2 . . ? O14 Cl1 O12 109.8(4) . . ? O14 Cl1 O13 108.8(3) . . ? O12 Cl1 O13 108.9(3) . . ? O14 Cl1 O11 108.5(3) . . ? O12 Cl1 O11 111.4(4) . . ? O13 Cl1 O11 109.4(3) . . ? O24 Cl2 O22' 148.0(14) . . ? O24 Cl2 O22 128.2(12) . . ? O24 Cl2 O21 97.0(8) . . ? O22' Cl2 O21 110.4(14) . . ? O22 Cl2 O21 112.6(10) . . ? O24 Cl2 O23' 66.4(16) . . ? O22' Cl2 O23' 110.7(19) . . ? O22 Cl2 O23' 123.5(13) . . ? O21 Cl2 O23' 119.2(8) . . ? O24 Cl2 O23 110.7(9) . . ? O22' Cl2 O23 80.1(15) . . ? O22 Cl2 O23 103.6(13) . . ? O21 Cl2 O23 102.0(8) . . ? O23' Cl2 O23 46.2(13) . . ? O24 Cl2 O24' 48.1(9) . . ? O22' Cl2 O24' 104.0(14) . . ? O22 Cl2 O24' 80.8(12) . . ? O21 Cl2 O24' 112.9(6) . . ? O23' Cl2 O24' 97.9(15) . . ? O23 Cl2 O24' 140.1(9) . . ? H2A O2 H2B 96.9 . . ? H3A O3 H3B 99.2 . . ? 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 H1A O3 0.93 1.69 2.530(8) 147.9 . O1 H1B O2 0.83 1.83 2.586(8) 149.8 4_565 N2 H2 O11 0.93 2.13 2.977(7) 151.6 2_746 O2 H2A O14 0.84 1.96 2.784(7) 166.8 4_566 O2 H2B O13 0.88 2.03 2.866(7) 158.0 2_746 O3 H3A O21 0.95 1.94 2.853(11) 158.9 1_655 O3 H3B O23 0.95 1.78 2.700(15) 162.0 3_656 O3 H3A O23 0.95 2.23 2.99(2) 135.7 1_655 O3 H3B O23' 0.95 2.03 2.92(3) 156.2 3_656 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.939 _refine_diff_density_min -0.888 _refine_diff_density_rms 0.133 #===END OF ALL DATA