# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2004 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Dr Baoqing Ma Ma' _publ_contact_author_address ; Chemistry Peking University Beijing Beijing 100871 CHINA ; _publ_contact_author_email MABQING@YAHOO.COM _publ_section_title ; Solid state evidence of cyclic water pentamer in a tape-like structure ; loop_ _publ_author_name 'Baoqing Ma Ma' 'Song Gao' 'Hao-Ling Sun' #===================================================================== data_new _database_code_depnum_ccdc_archive 'CCDC 227242' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C10 H16 N4 O6' _chemical_formula_weight 288.27 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' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pca2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y, z' '-x+1/2, y, z+1/2' _cell_length_a 21.52(2) _cell_length_b 9.645(7) _cell_length_c 6.643(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1379(2) _cell_formula_units_Z 4 _cell_measurement_temperature 276(1) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needle _exptl_crystal_colour red _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.388 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 608 _exptl_absorpt_coefficient_mu 0.116 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 276(1) _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 'SMART CCD 1000' _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 3484 _diffrn_reflns_av_R_equivalents 0.1367 _diffrn_reflns_av_sigmaI/netI 0.0898 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -7 _diffrn_reflns_limit_l_max 7 _diffrn_reflns_theta_min 1.89 _diffrn_reflns_theta_max 26.99 _reflns_number_total 2274 _reflns_number_gt 1389 _reflns_threshold_expression >2sigma(I) _computing_data_collection SMART _computing_cell_refinement SMART _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics XP _computing_publication_material XCIF _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^)+(0.1557P)^2^+0.0000P] 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 SHELXL _refine_ls_extinction_coef 0.048(10) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.00 _refine_ls_number_reflns 2274 _refine_ls_number_parameters 246 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.1117 _refine_ls_R_factor_gt 0.0766 _refine_ls_wR_factor_ref 0.2296 _refine_ls_wR_factor_gt 0.1925 _refine_ls_goodness_of_fit_ref 0.964 _refine_ls_restrained_S_all 0.964 _refine_ls_shift/su_max 0.004 _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 N1 N 0.38143(14) 0.0749(4) 0.3290(7) 0.0394(10) Uani 1 1 d . . . N2 N 0.00167(15) 0.4408(4) 0.2415(7) 0.0405(10) Uani 1 1 d . . . N3 N 0.21593(17) 0.2914(4) 0.2760(7) 0.0429(10) Uani 1 1 d . . . N4 N 0.16688(16) 0.2227(4) 0.2890(7) 0.0436(11) Uani 1 1 d . . . O1 O 0.43467(14) 0.0088(4) 0.3467(7) 0.0564(11) Uani 1 1 d . . . O1W O 0.1556(2) 0.8299(5) 0.3921(9) 0.0756(15) Uani 1 1 d . . . H1 H 0.118(3) 0.849(5) 0.353(11) 0.046(14) Uiso 1 1 d D . . H2 H 0.150(6) 0.758(12) 0.51(2) 0.22(7) Uiso 1 1 d D . . O2 O -0.05083(14) 0.5073(3) 0.2305(7) 0.0569(11) Uani 1 1 d . . . O2W O 0.2135(2) 0.6928(6) 0.0833(10) 0.0765(15) Uani 1 1 d . . . H4 H 0.258(4) 0.680(7) 0.077(14) 0.08(2) Uiso 1 1 d . . . H3 H 0.201(4) 0.726(9) 0.183(17) 0.10(4) Uiso 1 1 d . . . O3W O 0.1580(2) 0.6447(4) 0.7241(9) 0.0640(12) Uani 1 1 d . . . H6 H 0.123(3) 0.602(6) 0.750(10) 0.055(16) Uiso 1 1 d . . . H5 H 0.183(4) 0.641(10) 0.813(18) 0.11(4) Uiso 1 1 d . . . O4W O 0.04207(17) 0.8691(4) 0.2061(9) 0.0609(12) Uani 1 1 d . . . H8 H 0.053(2) 0.915(6) 0.075(11) 0.056(16) Uiso 1 1 d . . . H7 H 0.005(2) 0.909(4) 0.248(8) 0.033(11) Uiso 1 1 d . . . C1 C 0.3802(2) 0.2110(5) 0.2914(8) 0.0416(12) Uani 1 1 d . . . C2 C 0.3257(2) 0.2798(5) 0.2724(8) 0.0418(12) Uani 1 1 d . . . H2A H 0.323(2) 0.386(6) 0.240(10) 0.057(15) Uiso 1 1 d . . . C3 C 0.27011(18) 0.2088(5) 0.2950(8) 0.0381(11) Uani 1 1 d . . . C4 C 0.27182(19) 0.0680(5) 0.3357(9) 0.0412(12) Uani 1 1 d . . . H4A H 0.234(2) 0.025(5) 0.366(10) 0.042(13) Uiso 1 1 d . . . C5 C 0.3276(2) 0.0040(5) 0.3555(10) 0.0437(13) Uani 1 1 d . . . H5A H 0.328(2) -0.085(6) 0.411(9) 0.048(15) Uiso 1 1 d . . . C6 C 0.1126(2) 0.3034(5) 0.2732(9) 0.0411(12) Uani 1 1 d . . . C7 C 0.1110(2) 0.4473(5) 0.2481(9) 0.0447(12) Uani 1 1 d . . . H7A H 0.147(2) 0.499(5) 0.237(9) 0.043(13) Uiso 1 1 d . . . C8 C 0.0552(2) 0.5124(5) 0.2321(10) 0.0451(13) Uani 1 1 d . . . H8A H 0.052(2) 0.598(6) 0.210(10) 0.052(16) Uiso 1 1 d . . . C9 C 0.0028(2) 0.3017(5) 0.2668(10) 0.0498(14) Uani 1 1 d . . . H9A H -0.039(3) 0.265(5) 0.258(9) 0.050(14) Uiso 1 1 d . . . C10 C 0.0576(2) 0.2330(5) 0.2803(10) 0.0499(14) Uani 1 1 d . . . H10A H 0.0548(19) 0.129(5) 0.314(9) 0.037(12) Uiso 1 1 d . . . H1A H 0.419(2) 0.249(5) 0.283(9) 0.042(13) 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 N1 0.0367(16) 0.036(2) 0.045(3) -0.002(2) -0.0003(17) 0.0001(14) N2 0.0370(16) 0.035(2) 0.050(3) 0.003(2) -0.0018(17) 0.0047(14) N3 0.0444(19) 0.037(2) 0.047(3) 0.002(2) -0.0012(17) -0.0017(15) N4 0.0435(19) 0.036(2) 0.051(3) -0.003(2) 0.0050(17) -0.0004(15) O1 0.0388(15) 0.054(2) 0.076(3) 0.011(2) 0.0002(18) 0.0096(13) O1W 0.051(2) 0.082(3) 0.093(4) 0.015(3) -0.007(2) -0.002(2) O2 0.0380(15) 0.0444(19) 0.088(3) 0.005(2) 0.0036(18) 0.0078(12) O2W 0.058(3) 0.099(4) 0.073(4) 0.011(3) -0.009(2) -0.004(2) O3W 0.050(2) 0.062(2) 0.080(4) 0.009(2) 0.001(2) -0.0056(17) O4W 0.0457(19) 0.054(2) 0.083(3) 0.007(2) 0.002(2) 0.0017(15) C1 0.039(2) 0.041(3) 0.045(4) 0.002(2) 0.0051(19) -0.0081(17) C2 0.046(2) 0.033(2) 0.046(4) 0.006(3) -0.004(2) -0.0034(16) C3 0.043(2) 0.036(2) 0.035(3) -0.002(2) 0.0041(18) 0.0015(17) C4 0.038(2) 0.043(3) 0.043(3) -0.002(2) 0.0035(19) -0.0096(18) C5 0.046(2) 0.030(3) 0.055(4) 0.008(3) -0.003(2) -0.0057(17) C6 0.045(2) 0.036(2) 0.043(3) -0.002(3) 0.0029(19) 0.0040(17) C7 0.040(2) 0.043(3) 0.051(4) 0.007(3) 0.003(2) -0.0041(18) C8 0.048(2) 0.027(2) 0.061(4) 0.004(3) -0.001(2) -0.0008(16) C9 0.040(2) 0.040(3) 0.069(4) -0.002(3) 0.007(2) -0.0067(18) C10 0.050(2) 0.031(2) 0.069(4) 0.000(3) 0.003(2) 0.0022(17) _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 N1 O1 1.317(5) . ? N1 C1 1.336(6) . ? N1 C5 1.357(6) . ? N2 O2 1.302(4) . ? N2 C8 1.345(6) . ? N2 C9 1.352(6) . ? N3 N4 1.249(5) . ? N3 C3 1.418(6) . ? N4 C6 1.407(6) . ? C1 C2 1.353(6) . ? C2 C3 1.387(6) . ? C3 C4 1.385(7) . ? C4 C5 1.357(6) . ? C6 C10 1.365(7) . ? C6 C7 1.399(7) . ? C7 C8 1.358(7) . ? C9 C10 1.357(7) . ? 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 O1 N1 C1 120.6(3) . . ? O1 N1 C5 119.2(4) . . ? C1 N1 C5 120.2(4) . . ? O2 N2 C8 119.2(4) . . ? O2 N2 C9 120.8(4) . . ? C8 N2 C9 120.0(4) . . ? N4 N3 C3 113.0(4) . . ? N3 N4 C6 113.8(4) . . ? N1 C1 C2 121.1(4) . . ? C1 C2 C3 119.7(5) . . ? C4 C3 C2 118.8(4) . . ? C4 C3 N3 126.2(4) . . ? C2 C3 N3 115.0(4) . . ? C5 C4 C3 119.3(4) . . ? C4 C5 N1 120.9(4) . . ? C10 C6 C7 118.5(4) . . ? C10 C6 N4 116.2(4) . . ? C7 C6 N4 125.3(4) . . ? C8 C7 C6 119.3(4) . . ? N2 C8 C7 121.1(5) . . ? N2 C9 C10 120.6(4) . . ? C9 C10 C6 120.5(5) . . ? 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 H1 O4W 0.87(6) 1.91(6) 2.763(7) 165(6) . O1W H2 O3W 1.04(10) 1.81(9) 2.839(7) 167(11) . O2W H3 O1W 0.78(11) 1.98(10) 2.741(9) 166(11) . O2W H4 O3W 0.97(9) 2.08(9) 2.956(7) 150(8) 4_554 O3W H6 O2 0.87(6) 1.88(6) 2.734(6) 164(6) 2_565 O3W H5 O2W 0.79(11) 1.98(12) 2.708(8) 153(10) 1_556 O4W H8 O1 1.01(7) 1.78(7) 2.787(7) 173(5) 4_564 O4W H7 O1 0.93(5) 1.82(5) 2.757(6) 176(5) 3_465 _diffrn_measured_fraction_theta_max 0.870 _diffrn_reflns_theta_full 26.99 _diffrn_measured_fraction_theta_full 0.870 _refine_diff_density_max 0.272 _refine_diff_density_min -0.278 _refine_diff_density_rms 0.074 data_p _database_code_depnum_ccdc_archive 'CCDC 227243' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C10 H16 N4 O6' _chemical_formula_weight 288.27 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' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pca2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y, z' '-x+1/2, y, z+1/2' _cell_length_a 21.519(3) _cell_length_b 9.5841(9) _cell_length_c 6.5759(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1356.2(2) _cell_formula_units_Z 4 _cell_measurement_temperature 90(1) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needle _exptl_crystal_colour red _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.412 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 608 _exptl_absorpt_coefficient_mu 0.117 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 90(1) _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 'SMART CCD 1000' _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 8324 _diffrn_reflns_av_R_equivalents 0.0740 _diffrn_reflns_av_sigmaI/netI 0.0723 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 1.89 _diffrn_reflns_theta_max 30.73 _reflns_number_total 3635 _reflns_number_gt 2651 _reflns_threshold_expression >2sigma(I) _computing_data_collection SMART _computing_cell_refinement SMART _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics XP _computing_publication_material XCIF _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^)+(0.0737P)^2^+0.0000P] 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 SHELXL _refine_ls_extinction_coef 0.017(2) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.00 _refine_ls_number_reflns 3635 _refine_ls_number_parameters 246 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0771 _refine_ls_R_factor_gt 0.0550 _refine_ls_wR_factor_ref 0.1353 _refine_ls_wR_factor_gt 0.1230 _refine_ls_goodness_of_fit_ref 0.960 _refine_ls_restrained_S_all 0.960 _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 N1 N 0.38125(8) 0.0704(2) 0.3317(3) 0.0150(4) Uani 1 1 d . . . N2 N -0.00007(8) 0.44320(19) 0.2375(3) 0.0163(4) Uani 1 1 d . . . N3 N 0.21501(8) 0.28996(19) 0.2707(3) 0.0168(4) Uani 1 1 d . . . N4 N 0.16580(8) 0.2206(2) 0.2861(3) 0.0168(4) Uani 1 1 d . . . O1 O 0.43465(7) 0.00336(17) 0.3513(3) 0.0204(4) Uani 1 1 d . . . O1W O 0.15572(9) 0.8337(2) 0.4029(3) 0.0257(4) Uani 1 1 d . . . H1 H 0.1168(18) 0.840(4) 0.356(7) 0.057(11) Uiso 1 1 d . . . H2 H 0.1481(17) 0.786(4) 0.512(8) 0.058(12) Uiso 1 1 d . . . O2 O -0.05285(7) 0.51117(16) 0.2241(3) 0.0202(4) Uani 1 1 d . . . O2W O 0.21304(9) 0.6921(2) 0.0931(3) 0.0283(5) Uani 1 1 d . . . H4 H 0.2445(16) 0.662(3) 0.117(5) 0.019(7) Uiso 1 1 d . . . H3 H 0.1988(13) 0.741(3) 0.182(5) 0.022(8) Uiso 1 1 d . . . O3W O 0.15961(9) 0.64277(19) 0.7277(3) 0.0224(4) Uani 1 1 d . . . H6 H 0.1355(18) 0.607(4) 0.733(7) 0.042(12) Uiso 1 1 d . . . H5 H 0.1757(13) 0.647(3) 0.857(5) 0.023(7) Uiso 1 1 d . . . O4W O 0.04152(8) 0.86651(18) 0.2152(3) 0.0209(4) Uani 1 1 d . . . H8 H 0.0510(14) 0.909(3) 0.106(6) 0.035(9) Uiso 1 1 d . . . H7 H 0.0114(18) 0.904(4) 0.256(6) 0.049(11) Uiso 1 1 d . . . C1 C 0.38089(10) 0.2070(2) 0.2860(4) 0.0155(5) Uani 1 1 d . . . C2 C 0.32541(10) 0.2782(2) 0.2658(4) 0.0150(5) Uani 1 1 d . . . H2A H 0.3239(10) 0.382(2) 0.227(4) 0.005(5) Uiso 1 1 d . . . C3 C 0.26951(10) 0.2072(2) 0.2930(3) 0.0153(5) Uani 1 1 d . . . C4 C 0.27045(10) 0.0649(2) 0.3396(4) 0.0164(5) Uani 1 1 d . . . H4A H 0.2321(13) 0.018(3) 0.355(5) 0.020(7) Uiso 1 1 d . . . C5 C 0.32685(10) -0.0006(2) 0.3601(4) 0.0152(4) Uani 1 1 d . . . H5A H 0.3309(9) -0.094(2) 0.384(4) 0.001(5) Uiso 1 1 d . . . C6 C 0.11117(10) 0.3026(2) 0.2681(4) 0.0162(5) Uani 1 1 d . . . C7 C 0.11027(10) 0.4482(2) 0.2416(4) 0.0174(5) Uani 1 1 d . . . H7A H 0.1437(12) 0.504(3) 0.239(4) 0.015(6) Uiso 1 1 d . . . C8 C 0.05439(10) 0.5159(2) 0.2270(4) 0.0155(4) Uani 1 1 d . . . H8A H 0.0494(10) 0.611(3) 0.205(4) 0.009(6) Uiso 1 1 d . . . C9 C 0.00000(11) 0.3024(2) 0.2617(4) 0.0190(5) Uani 1 1 d . . . H9A H -0.0388(13) 0.256(3) 0.257(5) 0.025(7) Uiso 1 1 d . . . C10 C 0.05541(10) 0.2313(3) 0.2783(4) 0.0189(5) Uani 1 1 d . . . H10A H 0.0567(11) 0.135(3) 0.304(4) 0.019(7) Uiso 1 1 d . . . H1A H 0.4197(14) 0.254(3) 0.267(5) 0.031(8) 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 N1 0.0109(8) 0.0170(9) 0.0173(10) -0.0001(8) -0.0006(7) 0.0005(7) N2 0.0121(8) 0.0206(9) 0.0164(9) -0.0014(9) 0.0006(8) 0.0031(7) N3 0.0148(9) 0.0174(9) 0.0181(10) 0.0012(8) -0.0001(8) 0.0014(7) N4 0.0160(9) 0.0190(9) 0.0153(10) -0.0002(8) 0.0001(7) 0.0015(7) O1 0.0108(7) 0.0231(8) 0.0274(10) 0.0043(8) -0.0002(7) 0.0059(6) O1W 0.0168(9) 0.0310(10) 0.0292(11) 0.0066(9) -0.0027(7) -0.0008(7) O2 0.0120(7) 0.0170(8) 0.0315(10) 0.0016(8) 0.0003(7) 0.0050(5) O2W 0.0167(9) 0.0382(12) 0.0299(11) -0.0004(10) -0.0044(8) 0.0027(8) O3W 0.0170(8) 0.0208(8) 0.0294(11) 0.0029(8) -0.0010(8) -0.0039(7) O4W 0.0157(8) 0.0202(8) 0.0269(10) 0.0029(8) 0.0017(8) 0.0006(6) C1 0.0130(10) 0.0181(11) 0.0155(11) 0.0005(9) -0.0003(8) -0.0028(8) C2 0.0158(10) 0.0142(10) 0.0150(11) 0.0001(9) 0.0008(9) -0.0004(7) C3 0.0133(10) 0.0196(11) 0.0130(11) -0.0010(9) 0.0006(8) 0.0016(8) C4 0.0134(10) 0.0208(11) 0.0151(11) -0.0007(9) 0.0007(9) -0.0015(8) C5 0.0155(10) 0.0110(10) 0.0191(12) 0.0009(9) 0.0014(9) -0.0002(8) C6 0.0139(10) 0.0205(11) 0.0143(11) -0.0034(10) 0.0004(8) 0.0024(8) C7 0.0141(10) 0.0223(11) 0.0158(11) 0.0018(10) 0.0010(9) -0.0021(8) C8 0.0176(10) 0.0115(10) 0.0175(11) 0.0008(10) 0.0014(9) -0.0004(7) C9 0.0147(10) 0.0170(10) 0.0254(13) -0.0009(10) 0.0013(9) -0.0025(8) C10 0.0187(11) 0.0162(11) 0.0216(12) -0.0006(9) 0.0015(9) 0.0000(8) _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 N1 O1 1.323(2) . ? N1 C1 1.343(3) . ? N1 C5 1.367(3) . ? N2 O2 1.312(2) . ? N2 C9 1.359(3) . ? N2 C8 1.365(3) . ? N3 N4 1.254(3) . ? N3 C3 1.424(3) . ? N4 C6 1.419(3) . ? C1 C2 1.382(3) . ? C2 C3 1.394(3) . ? C3 C4 1.398(3) . ? C4 C5 1.373(3) . ? C6 C10 1.382(3) . ? C6 C7 1.406(3) . ? C7 C8 1.370(3) . ? C9 C10 1.378(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 O1 N1 C1 120.01(18) . . ? O1 N1 C5 119.28(18) . . ? C1 N1 C5 120.71(18) . . ? O2 N2 C9 120.13(18) . . ? O2 N2 C8 119.09(17) . . ? C9 N2 C8 120.77(18) . . ? N4 N3 C3 113.07(18) . . ? N3 N4 C6 113.55(18) . . ? N1 C1 C2 120.5(2) . . ? C1 C2 C3 119.46(19) . . ? C2 C3 C4 119.5(2) . . ? C2 C3 N3 115.17(19) . . ? C4 C3 N3 125.32(19) . . ? C5 C4 C3 118.7(2) . . ? N1 C5 C4 121.1(2) . . ? C10 C6 C7 119.0(2) . . ? C10 C6 N4 116.19(19) . . ? C7 C6 N4 124.8(2) . . ? C8 C7 C6 119.4(2) . . ? N2 C8 C7 120.56(19) . . ? N2 C9 C10 120.1(2) . . ? C9 C10 C6 120.2(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 O1W H1 O4W 0.89(4) 1.88(4) 2.768(3) 170(4) . O1W H2 O3W 0.87(5) 1.99(5) 2.814(3) 159(4) . O2W H3 O1W 0.81(3) 1.94(3) 2.741(3) 171(3) . O2W H4 O3W 0.75(3) 2.20(3) 2.918(3) 161(3) 4_554 O3W H6 O2 0.62(4) 2.11(4) 2.730(2) 175(5) 2_565 O3W H5 O2W 0.92(3) 1.80(3) 2.706(3) 167(3) 1_556 O4W H8 O1 0.85(4) 1.93(4) 2.776(3) 175(3) 4_564 O4W H7 O1 0.79(4) 1.98(4) 2.765(2) 179(4) 3_465 _diffrn_measured_fraction_theta_max 0.904 _diffrn_reflns_theta_full 30.73 _diffrn_measured_fraction_theta_full 0.904 _refine_diff_density_max 0.367 _refine_diff_density_min -0.306 _refine_diff_density_rms 0.064 #====================================================================== data_new_b _database_code_depnum_ccdc_archive 'CCDC 227244' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C10 H8 D8 N4 O6' _chemical_formula_weight 296.32 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' D D 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pca2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y, z' '-x+1/2, y, z+1/2' _cell_length_a 21.483(3) _cell_length_b 9.5933(14) _cell_length_c 6.5701(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1354.1(3) _cell_formula_units_Z 4 _cell_measurement_temperature 90(1) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needle _exptl_crystal_colour red _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.454 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 608 _exptl_absorpt_coefficient_mu 0.118 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 90(1) _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 'SMART CCD 1000' _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 12764 _diffrn_reflns_av_R_equivalents 0.1086 _diffrn_reflns_av_sigmaI/netI 0.0635 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 1.90 _diffrn_reflns_theta_max 26.98 _reflns_number_total 2950 _reflns_number_gt 2367 _reflns_threshold_expression >2sigma(I) _computing_data_collection SMART _computing_cell_refinement SMART _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics XP _computing_publication_material XCIF _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^)+(0.1051P)^2^+0.0000P] 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 SHELXL _refine_ls_extinction_coef 0.025(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.00 _refine_ls_number_reflns 2950 _refine_ls_number_parameters 246 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0728 _refine_ls_R_factor_gt 0.0589 _refine_ls_wR_factor_ref 0.1554 _refine_ls_wR_factor_gt 0.1442 _refine_ls_goodness_of_fit_ref 1.010 _refine_ls_restrained_S_all 1.010 _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 N1 N 0.38134(9) 0.0708(2) 0.3320(4) 0.0158(5) Uani 1 1 d . . . N2 N -0.00027(9) 0.4432(2) 0.2366(4) 0.0165(5) Uani 1 1 d . . . N3 N 0.21501(10) 0.2903(2) 0.2706(4) 0.0183(5) Uani 1 1 d . . . N4 N 0.16569(10) 0.2207(2) 0.2861(4) 0.0177(5) Uani 1 1 d . . . O1 O 0.43467(8) 0.00358(19) 0.3519(4) 0.0211(5) Uani 1 1 d . . . O1W O 0.15593(10) 0.8339(2) 0.4032(4) 0.0257(5) Uani 1 1 d . . . D1 D 0.118(2) 0.845(4) 0.351(8) 0.040(11) Uiso 1 1 d . . . D2 D 0.1501(17) 0.776(4) 0.514(7) 0.030(10) Uiso 1 1 d . . . O2 O -0.05307(8) 0.51149(19) 0.2237(4) 0.0211(5) Uani 1 1 d . . . O2W O 0.21271(10) 0.6922(3) 0.0929(4) 0.0289(5) Uani 1 1 d . . . D4 D 0.248(2) 0.667(4) 0.126(7) 0.032(10) Uiso 1 1 d . . . D3 D 0.1992(16) 0.740(4) 0.190(7) 0.023(9) Uiso 1 1 d . . . O3W O 0.16002(10) 0.6435(2) 0.7269(4) 0.0230(5) Uani 1 1 d . . . D6 D 0.1368(15) 0.601(3) 0.725(5) 0.003(7) Uiso 1 1 d . . . D5 D 0.1731(17) 0.644(4) 0.862(7) 0.028(10) Uiso 1 1 d . . . O4W O 0.04151(9) 0.8665(2) 0.2158(4) 0.0223(5) Uani 1 1 d . . . D8 D 0.0523(17) 0.912(4) 0.104(7) 0.035(11) Uiso 1 1 d . . . D7 D 0.009(2) 0.901(4) 0.260(7) 0.047(12) Uiso 1 1 d . . . C1 C 0.38101(12) 0.2076(3) 0.2859(4) 0.0170(6) Uani 1 1 d . . . C2 C 0.32530(12) 0.2780(3) 0.2661(4) 0.0171(6) Uani 1 1 d . . . H2A H 0.3219(13) 0.384(3) 0.225(5) 0.011(7) Uiso 1 1 d . . . C3 C 0.26946(12) 0.2074(3) 0.2926(4) 0.0163(6) Uani 1 1 d . . . C4 C 0.27048(12) 0.0655(3) 0.3401(4) 0.0167(6) Uani 1 1 d . . . H4A H 0.2302(13) 0.015(3) 0.356(5) 0.007(7) Uiso 1 1 d . . . C5 C 0.32720(12) -0.0004(3) 0.3606(5) 0.0167(6) Uani 1 1 d . . . H5A H 0.3307(13) -0.090(3) 0.391(5) 0.014(7) Uiso 1 1 d . . . C6 C 0.11120(12) 0.3029(3) 0.2682(4) 0.0179(6) Uani 1 1 d . . . C7 C 0.11020(12) 0.4479(3) 0.2410(5) 0.0179(5) Uani 1 1 d . . . H7A H 0.1443(17) 0.502(3) 0.244(6) 0.027(9) Uiso 1 1 d . . . C8 C 0.05420(12) 0.5155(3) 0.2264(5) 0.0172(5) Uani 1 1 d . . . H8A H 0.0490(12) 0.610(3) 0.198(5) 0.005(6) Uiso 1 1 d . . . C9 C -0.00010(12) 0.3030(3) 0.2624(5) 0.0197(6) Uani 1 1 d . . . H9A H -0.0383(16) 0.254(3) 0.258(6) 0.024(8) Uiso 1 1 d . . . C10 C 0.05523(12) 0.2310(3) 0.2785(5) 0.0196(6) Uani 1 1 d . . . H10A H 0.0581(12) 0.120(3) 0.320(5) 0.008(7) Uiso 1 1 d . . . H1A H 0.4198(15) 0.249(3) 0.272(5) 0.016(8) 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 N1 0.0106(9) 0.0204(11) 0.0164(12) 0.0002(9) 0.0003(9) 0.0014(8) N2 0.0107(9) 0.0208(10) 0.0181(10) -0.0014(11) -0.0005(9) 0.0036(8) N3 0.0146(11) 0.0214(11) 0.0187(13) 0.0014(10) 0.0005(10) 0.0015(8) N4 0.0140(11) 0.0214(11) 0.0177(12) -0.0012(9) 0.0003(9) 0.0008(8) O1 0.0098(8) 0.0243(10) 0.0290(12) 0.0043(9) -0.0006(9) 0.0049(7) O1W 0.0147(9) 0.0322(11) 0.0304(12) 0.0077(10) -0.0020(9) 0.0004(8) O2 0.0105(8) 0.0224(9) 0.0303(12) 0.0010(9) 0.0006(9) 0.0053(6) O2W 0.0160(10) 0.0386(13) 0.0320(13) -0.0006(12) -0.0036(10) 0.0017(9) O3W 0.0154(10) 0.0248(10) 0.0289(13) 0.0025(10) 0.0002(10) -0.0049(9) O4W 0.0144(9) 0.0236(10) 0.0288(12) 0.0033(10) 0.0024(9) 0.0013(7) C1 0.0126(12) 0.0206(12) 0.0177(14) -0.0004(11) -0.0005(11) -0.0030(9) C2 0.0158(12) 0.0179(13) 0.0175(14) -0.0008(11) 0.0002(11) -0.0003(9) C3 0.0131(11) 0.0228(12) 0.0129(13) -0.0011(10) 0.0004(10) 0.0023(10) C4 0.0131(11) 0.0227(13) 0.0144(13) -0.0006(11) 0.0007(11) -0.0017(10) C5 0.0154(12) 0.0163(12) 0.0185(14) 0.0019(11) 0.0006(11) -0.0010(9) C6 0.0149(12) 0.0236(13) 0.0151(14) -0.0005(12) -0.0001(11) 0.0029(10) C7 0.0130(11) 0.0236(13) 0.0172(13) 0.0009(12) 0.0020(12) -0.0015(10) C8 0.0164(12) 0.0171(12) 0.0182(13) 0.0018(12) 0.0005(12) -0.0002(9) C9 0.0140(12) 0.0209(12) 0.0243(15) -0.0020(12) 0.0011(11) -0.0023(10) C10 0.0182(12) 0.0202(13) 0.0204(15) -0.0010(11) 0.0016(11) 0.0021(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 N1 O1 1.322(3) . ? N1 C1 1.346(3) . ? N1 C5 1.362(3) . ? N2 O2 1.313(3) . ? N2 C9 1.356(3) . ? N2 C8 1.362(3) . ? N3 N4 1.257(3) . ? N3 C3 1.422(3) . ? N4 C6 1.417(3) . ? C1 H1A 0.93(3) . ? C1 C2 1.380(4) . ? C2 H2A 1.05(3) . ? C2 C3 1.388(4) . ? C3 C4 1.397(4) . ? C4 H4A 1.00(3) . ? C4 C5 1.379(4) . ? C5 H5A 0.89(3) . ? C6 C10 1.388(4) . ? C6 C7 1.403(4) . ? C7 H7A 0.90(4) . ? C7 C8 1.370(4) . ? C8 H8A 0.93(3) . ? C9 H9A 0.95(3) . ? C9 C10 1.379(4) . ? C10 H10A 1.10(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 O1 N1 C1 120.2(2) . . ? O1 N1 C5 118.8(2) . . ? C1 N1 C5 121.0(2) . . ? O2 N2 C9 120.4(2) . . ? O2 N2 C8 119.0(2) . . ? C9 N2 C8 120.6(2) . . ? N4 N3 C3 112.8(2) . . ? N3 N4 C6 113.2(2) . . ? H1A C1 N1 116.0(18) . . ? H1A C1 C2 123.9(18) . . ? N1 C1 C2 120.2(2) . . ? H2A C2 C1 123.7(15) . . ? H2A C2 C3 116.3(15) . . ? C1 C2 C3 119.9(2) . . ? C2 C3 C4 119.3(2) . . ? C2 C3 N3 115.2(2) . . ? C4 C3 N3 125.5(2) . . ? H4A C4 C5 122.1(15) . . ? H4A C4 C3 119.1(15) . . ? C5 C4 C3 118.8(2) . . ? H5A C5 N1 116.5(18) . . ? H5A C5 C4 122.7(18) . . ? N1 C5 C4 120.7(2) . . ? C10 C6 C7 119.1(2) . . ? C10 C6 N4 115.8(2) . . ? C7 C6 N4 125.1(2) . . ? H7A C7 C8 117(2) . . ? H7A C7 C6 124(2) . . ? C8 C7 C6 119.4(2) . . ? H8A C8 N2 113.7(16) . . ? H8A C8 C7 125.4(16) . . ? N2 C8 C7 120.7(2) . . ? H9A C9 N2 119(2) . . ? H9A C9 C10 120(2) . . ? N2 C9 C10 120.6(2) . . ? H10A C10 C9 123.5(14) . . ? H10A C10 C6 116.4(14) . . ? C9 C10 C6 119.6(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 O1W D1 O4W 0.88(5) 1.89(5) 2.767(3) 175(5) . O1W D2 O3W 0.92(4) 1.90(4) 2.805(3) 165(3) . O2W D3 O1W 0.84(4) 1.91(4) 2.737(4) 171(3) . O2W D4 O3W 0.82(5) 2.10(5) 2.910(3) 169(3) 4_554 O3W D6 O2 0.64(3) 2.10(3) 2.737(3) 172(3) 2_565 O3W D5 O2W 0.93(5) 1.80(5) 2.698(4) 161(3) 1_556 O4W D8 O1 0.88(5) 1.90(5) 2.776(3) 173(4) 4_564 O4W D7 O1 0.83(5) 1.94(5) 2.761(3) 175(4) 3_465 _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 26.98 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.318 _refine_diff_density_min -0.258 _refine_diff_density_rms 0.071