Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2002 data_c10m _database_code_CSD 180977 _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Ng, Chew Hee' 'Adams, Farook' 'Chong, Thiam Seong' 'Ng, Seik Weng' 'Teoh, Siang Guan' _publ_contact_author_name 'Dr CHEW HEE NG' _publ_contact_author_address ; Chemistry and Biology Tunku Abdul Rahman College School of Arts and Science, Tunku A Kuala Lumpur 53300 MALAYSIA ; _publ_contact_author_email 'NGCH@MAIL.TARC.EDU.MY' _publ_section_title ; Reactions of a series of bis(á-aminoacidato)copper(II) with formaldehyde and benzamide: aldol-type condensation versus Mannich aminomethylation ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '(C13 H15 N2 O4)2, Cu, 2H2O' _chemical_formula_sum 'C26 H34 Cu N4 O10' _chemical_formula_weight 626.11 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' 'Cu' 'Cu' 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M P212121 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 12.2944(2) _cell_length_b 12.4471(1) _cell_length_c 19.7477(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3021.98(7) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour Blue _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.46 _exptl_crystal_size_min 0.28 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.376 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1308 _exptl_absorpt_coefficient_mu 0.781 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'Siemens CCD area-detector diffractometer' _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 21658 _diffrn_reflns_av_R_equivalents 0.1316 _diffrn_reflns_av_sigmaI/netI 0.1280 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.93 _diffrn_reflns_theta_max 29.17 _reflns_number_total 7437 _reflns_number_gt 5277 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0444P)^2^] 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 0.0371(16) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_abs_structure_details 'Flack & Schwarzenbach (1998)' _refine_ls_abs_structure_Flack -0.02(1) _refine_ls_number_reflns 7437 _refine_ls_number_parameters 371 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0807 _refine_ls_R_factor_gt 0.0534 _refine_ls_wR_factor_ref 0.1309 _refine_ls_wR_factor_gt 0.1233 _refine_ls_goodness_of_fit_ref 0.946 _refine_ls_restrained_S_all 0.946 _refine_ls_shift/su_max <0.001 _refine_ls_shift/su_mean <0.001 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 Cu1 Cu 0.58870(3) 0.22686(3) 0.87708(2) 0.0393(1) Uani 1 1 d . . . O1 O 0.4346(2) 0.2280(2) 0.8532(1) 0.050(1) Uani 1 1 d . . . O2 O 0.2732(2) 0.2990(3) 0.8809(2) 0.072(1) Uani 1 1 d . . . O3 O 0.5146(2) 0.5112(2) 0.9701(1) 0.049(1) Uani 1 1 d . . . O4 O 0.5886(2) 0.0872(2) 0.9528(1) 0.055(1) Uani 1 1 d . . . O5 O 0.7422(2) 0.2636(2) 0.8860(1) 0.052(1) Uani 1 1 d . . . O6 O 0.9076(2) 0.2322(3) 0.8443(1) 0.062(1) Uani 1 1 d . . . O7 O 0.6810(2) 0.1446(2) 0.6843(1) 0.048(1) Uani 1 1 d . . . O8 O 0.4348(3) -0.0496(3) 0.7188(2) 0.088(1) Uani 1 1 d . . . O1w O 0.3169(6) 0.2416(6) 0.7146(3) 0.172(3) Uani 1 1 d . . . O2w O 0.1234(4) 0.3056(6) 0.7711(3) 0.181(3) Uani 1 1 d . . . N1 N 0.5433(2) 0.3271(2) 0.9541(1) 0.036(1) Uani 1 1 d . . . N2 N 0.5164(2) 0.1843(2) 1.0389(1) 0.042(1) Uani 1 1 d . . . N3 N 0.6387(2) 0.1288(2) 0.7990(1) 0.036(1) Uani 1 1 d . . . N4 N 0.4946(3) -0.0028(3) 0.8234(2) 0.050(1) Uani 1 1 d . . . C1 C 0.3712(3) 0.2876(3) 0.8899(2) 0.045(1) Uani 1 1 d . . . C2 C 0.4236(3) 0.3481(3) 0.9489(2) 0.039(1) Uani 1 1 d . . . C3 C 0.4137(3) 0.4721(3) 0.9396(2) 0.046(1) Uani 1 1 d . . . C4 C 0.3174(4) 0.5221(4) 0.9740(3) 0.075(1) Uani 1 1 d . . . C5 C 0.5939(3) 0.4373(3) 0.9462(2) 0.044(1) Uani 1 1 d . . . C6 C 0.5762(3) 0.2805(3) 1.0222(2) 0.041(1) Uani 1 1 d . . . C7 C 0.5305(3) 0.0902(3) 1.0044(2) 0.044(1) Uani 1 1 d . . . C8 C 0.4735(3) -0.0091(3) 1.0285(2) 0.049(1) Uani 1 1 d . . . C9 C 0.3857(3) -0.0082(3) 1.0734(2) 0.057(1) Uani 1 1 d . . . C10 C 0.3342(4) -0.1042(4) 1.0918(3) 0.075(1) Uani 1 1 d . . . C11 C 0.3721(5) -0.2007(4) 1.0664(3) 0.083(2) Uani 1 1 d . . . C12 C 0.4572(5) -0.2031(4) 1.0224(3) 0.078(1) Uani 1 1 d . . . C13 C 0.5104(4) -0.1068(3) 1.0024(2) 0.061(1) Uani 1 1 d . . . C14 C 0.8080(3) 0.2171(3) 0.8452(2) 0.043(1) Uani 1 1 d . . . C15 C 0.7602(3) 0.1370(3) 0.7936(2) 0.039(1) Uani 1 1 d . . . C16 C 0.7818(3) 0.1722(3) 0.7185(2) 0.045(1) Uani 1 1 d . . . C17 C 0.8774(3) 0.1171(5) 0.6843(2) 0.075(1) Uani 1 1 d . . . C18 C 0.5988(3) 0.1712(3) 0.7316(2) 0.043(1) Uani 1 1 d . . . C19 C 0.6071(3) 0.0109(3) 0.8062(2) 0.049(1) Uani 1 1 d . . . C20 C 0.4158(4) -0.0306(3) 0.7792(2) 0.052(1) Uani 1 1 d . . . C21 C 0.3031(3) -0.0421(3) 0.8087(2) 0.055(1) Uani 1 1 d . . . C22 C 0.2842(3) -0.0756(4) 0.8747(2) 0.068(1) Uani 1 1 d . . . C23 C 0.1780(4) -0.0886(5) 0.8991(3) 0.088(2) Uani 1 1 d . . . C24 C 0.0920(5) -0.0674(5) 0.8582(5) 0.112(2) Uani 1 1 d . . . C25 C 0.1077(5) -0.0324(6) 0.7937(5) 0.134(3) Uani 1 1 d . . . C26 C 0.2141(5) -0.0237(5) 0.7665(4) 0.111(3) Uani 1 1 d . . . H1w1 H 0.3580 0.2397 0.7503 0.207 Uiso 1 1 d . . . H1w2 H 0.3616 0.2597 0.6820 0.207 Uiso 1 1 d . . . H2w1 H 0.1404 0.3317 0.8110 0.217 Uiso 1 1 d . . . H2w2 H 0.0537 0.3174 0.7681 0.217 Uiso 1 1 d . . . H2n H 0.4702 0.1864 1.0715 0.051 Uiso 1 1 calc R . . H4n H 0.4761 0.0074 0.8649 0.060 Uiso 1 1 calc R . . H2 H 0.3881 0.3271 0.9913 0.046 Uiso 1 1 calc R . . H3 H 0.4126 0.4897 0.8912 0.055 Uiso 1 1 calc R . . H4a H 0.3172 0.5981 0.9658 0.112 Uiso 1 1 calc R . . H4b H 0.3216 0.5090 1.0219 0.112 Uiso 1 1 calc R . . H4c H 0.2517 0.4910 0.9565 0.112 Uiso 1 1 calc R . . H5a H 0.6601 0.4427 0.9726 0.052 Uiso 1 1 calc R . . H5b H 0.6110 0.4513 0.8990 0.052 Uiso 1 1 calc R . . H6a H 0.6533 0.2641 1.0215 0.050 Uiso 1 1 calc R . . H6b H 0.5640 0.3339 1.0572 0.050 Uiso 1 1 calc R . . H9 H 0.3612 0.0566 1.0912 0.068 Uiso 1 1 calc R . . H10 H 0.2749 -0.1031 1.1210 0.089 Uiso 1 1 calc R . . H11 H 0.3390 -0.2646 1.0794 0.099 Uiso 1 1 calc R . . H12 H 0.4809 -0.2686 1.0053 0.093 Uiso 1 1 calc R . . H13 H 0.5688 -0.1088 0.9724 0.074 Uiso 1 1 calc R . . H15 H 0.7923 0.0659 0.8012 0.047 Uiso 1 1 calc R . . H16 H 0.7922 0.2502 0.7169 0.054 Uiso 1 1 calc R . . H17a H 0.8850 0.1440 0.6390 0.112 Uiso 1 1 calc R . . H17b H 0.8648 0.0410 0.6829 0.112 Uiso 1 1 calc R . . H17c H 0.9427 0.1316 0.7093 0.112 Uiso 1 1 calc R . . H18a H 0.5304 0.1377 0.7192 0.051 Uiso 1 1 calc R . . H18b H 0.5884 0.2484 0.7336 0.051 Uiso 1 1 calc R . . H19a H 0.6218 -0.0259 0.7639 0.058 Uiso 1 1 calc R . . H19b H 0.6517 -0.0219 0.8410 0.058 Uiso 1 1 calc R . . H22 H 0.3428 -0.0896 0.9032 0.081 Uiso 1 1 calc R . . H23 H 0.1665 -0.1116 0.9433 0.106 Uiso 1 1 calc R . . H24 H 0.0216 -0.0770 0.8744 0.134 Uiso 1 1 calc R . . H25 H 0.0480 -0.0139 0.7672 0.161 Uiso 1 1 calc R . . H26 H 0.2243 -0.0060 0.7211 0.134 Uiso 1 1 calc R . . 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 Cu1 0.0345(2) 0.0525(2) 0.0310(2) -0.0117(2) 0.0028(2) -0.0032(2) O1 0.040(1) 0.064(2) 0.046(1) -0.017(1) -0.005(1) -0.004(1) O2 0.039(1) 0.099(2) 0.080(2) -0.031(2) -0.009(1) 0.001(1) O3 0.049(1) 0.045(1) 0.052(2) -0.008(1) -0.001(1) -0.004(1) O4 0.074(2) 0.055(2) 0.035(1) -0.002(1) 0.006(1) 0.021(2) O5 0.036(1) 0.074(2) 0.046(1) -0.027(1) 0.003(1) -0.006(1) O6 0.034(1) 0.104(2) 0.049(2) -0.025(1) 0.000(1) -0.008(2) O7 0.050(1) 0.065(2) 0.030(1) -0.010(1) 0.001(1) -0.006(1) O8 0.097(3) 0.127(3) 0.039(2) -0.011(2) 0.005(2) -0.048(2) O1w 0.180(5) 0.191(6) 0.146(5) -0.049(4) -0.043(4) -0.028(5) O2w 0.131(4) 0.257(8) 0.153(6) -0.023(5) -0.061(4) 0.046(5) N1 0.032(1) 0.045(2) 0.031(1) -0.004(1) -0.003(1) 0.002(1) N2 0.051(2) 0.046(2) 0.030(1) -0.004(1) 0.002(1) 0.004(1) N3 0.038(1) 0.039(2) 0.030(1) -0.006(1) 0.003(1) -0.001(1) N4 0.055(2) 0.059(2) 0.036(2) -0.010(1) 0.005(1) -0.019(2) C1 0.036(2) 0.055(2) 0.044(2) -0.005(2) -0.002(1) -0.004(2) C2 0.036(2) 0.047(2) 0.033(2) 0.002(1) 0.001(1) 0.001(2) C3 0.043(2) 0.047(2) 0.047(2) 0.003(2) -0.001(2) 0.004(2) C4 0.063(3) 0.056(3) 0.106(4) -0.013(3) 0.010(3) 0.016(2) C5 0.040(2) 0.049(2) 0.041(2) -0.003(2) 0.000(2) -0.007(2) C6 0.044(2) 0.052(2) 0.028(1) -0.007(1) -0.005(1) 0.004(2) C7 0.052(2) 0.052(2) 0.029(2) -0.002(2) -0.009(2) 0.018(2) C8 0.064(2) 0.045(2) 0.038(2) 0.001(2) -0.019(2) 0.012(2) C9 0.066(3) 0.050(2) 0.056(2) -0.003(2) 0.001(2) 0.003(2) C10 0.093(3) 0.061(3) 0.069(3) 0.002(2) 0.006(3) -0.010(3) C11 0.102(4) 0.049(3) 0.097(4) 0.003(3) -0.013(3) -0.003(3) C12 0.100(4) 0.040(2) 0.093(4) -0.011(2) -0.020(3) 0.012(2) C13 0.074(3) 0.057(3) 0.053(3) -0.006(2) -0.013(2) 0.016(2) C14 0.043(2) 0.057(2) 0.030(2) -0.006(2) -0.002(1) -0.001(2) C15 0.036(2) 0.047(2) 0.034(2) -0.009(1) 0.000(1) 0.001(2) C16 0.046(2) 0.058(2) 0.032(2) -0.009(2) 0.005(1) -0.007(2) C17 0.056(2) 0.115(4) 0.052(3) -0.022(3) 0.016(2) 0.010(3) C18 0.042(2) 0.051(2) 0.036(2) -0.006(1) -0.006(2) -0.001(2) C19 0.052(2) 0.047(2) 0.047(2) -0.004(2) 0.005(2) -0.007(2) C20 0.066(2) 0.049(2) 0.042(2) -0.003(2) 0.002(2) -0.021(2) C21 0.053(2) 0.050(2) 0.060(3) -0.005(2) -0.003(2) -0.013(2) C22 0.062(2) 0.092(3) 0.049(2) -0.017(2) 0.001(2) -0.027(2) C23 0.077(3) 0.116(5) 0.073(4) -0.038(3) 0.028(3) -0.032(3) C24 0.064(3) 0.085(4) 0.187(8) -0.018(5) 0.032(5) -0.007(3) C25 0.060(4) 0.115(5) 0.23(1) 0.073(6) -0.035(5) -0.008(3) C26 0.085(4) 0.113(5) 0.136(6) 0.070(4) -0.043(4) -0.029(4) 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 Cu1 O1 1.953(2) . ? Cu1 N1 2.046(3) . ? Cu1 N3 2.060(3) . ? Cu1 O4 2.293(3) . ? Cu1 O5 1.950(2) . ? Cu1 O8 3.379(4) 3_656 ? O1 C1 1.297(4) . ? O2 C1 1.226(4) . ? O3 C5 1.421(4) . ? O3 C3 1.463(5) . ? O4 C7 1.246(4) . ? O5 C14 1.280(4) . ? O6 C14 1.240(4) . ? O7 C18 1.416(4) . ? O7 C16 1.453(4) . ? O8 C20 1.238(5) . ? N1 C2 1.499(4) . ? N1 C5 1.514(4) . ? N1 C6 1.519(4) . ? N2 C7 1.366(4) . ? N2 C6 1.443(4) . ? N3 C15 1.502(4) . ? N3 C18 1.513(4) . ? N3 C19 1.524(5) . ? N4 C20 1.348(5) . ? N4 C19 1.434(5) . ? C1 C2 1.529(5) . ? C2 C3 1.558(5) . ? C3 C4 1.501(6) . ? C7 C8 1.498(6) . ? C8 C13 1.397(6) . ? C8 C9 1.397(6) . ? C9 C10 1.400(6) . ? C10 C11 1.382(7) . ? C11 C12 1.359(8) . ? C12 C13 1.422(7) . ? C14 C15 1.542(5) . ? C15 C16 1.568(5) . ? C16 C17 1.519(5) . ? C20 C21 1.510(6) . ? C21 C26 1.395(7) . ? C21 C22 1.389(7) . ? C22 C23 1.400(6) . ? C23 C24 1.356(9) . ? C24 C25 1.36(1) . ? C25 C26 1.42(1) . ? 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 Cu1 O4 99.3(1) . . ? O1 Cu1 O5 163.6(1) . . ? O1 Cu1 N1 84.9(1) . . ? O1 Cu1 N3 96.5(1) . . ? O4 Cu1 O5 96.8(1) . . ? O4 Cu1 N1 88.7(1) . . ? O4 Cu1 N3 92.3(1) . . ? O5 Cu1 N1 93.1(1) . . ? O5 Cu1 N3 85.3(1) . . ? N1 Cu1 N3 178.2(1) . . ? C1 O1 Cu1 116.9(2) . . ? C5 O3 C3 103.2(3) . . ? C7 O4 Cu1 120.8(2) . . ? C14 O5 Cu1 116.6(2) . . ? C18 O7 C16 104.3(2) . . ? C2 N1 C5 103.8(3) . . ? C2 N1 C6 112.9(2) . . ? C5 N1 C6 109.2(2) . . ? C2 N1 Cu1 108.8(2) . . ? C5 N1 Cu1 111.3(2) . . ? C6 N1 Cu1 110.7(2) . . ? C7 N2 C6 122.3(3) . . ? C15 N3 C18 103.7(2) . . ? C15 N3 C19 109.0(3) . . ? C18 N3 C19 109.6(3) . . ? C15 N3 Cu1 108.1(2) . . ? C18 N3 Cu1 110.8(2) . . ? C19 N3 Cu1 115.1(2) . . ? C20 N4 C19 124.8(3) . . ? O2 C1 O1 125.1(3) . . ? O2 C1 C2 117.9(3) . . ? O1 C1 C2 117.0(3) . . ? N1 C2 C1 112.4(3) . . ? N1 C2 C3 104.9(3) . . ? C1 C2 C3 111.4(3) . . ? O3 C3 C4 110.1(3) . . ? O3 C3 C2 102.4(3) . . ? C4 C3 C2 114.7(3) . . ? O3 C5 N1 105.7(3) . . ? N2 C6 N1 112.5(2) . . ? O4 C7 N2 120.4(3) . . ? O4 C7 C8 120.3(3) . . ? N2 C7 C8 119.4(3) . . ? C13 C8 C9 119.5(4) . . ? C13 C8 C7 116.7(4) . . ? C9 C8 C7 123.8(4) . . ? C8 C9 C10 120.5(4) . . ? C11 C10 C9 119.7(5) . . ? C12 C11 C10 120.7(5) . . ? C11 C12 C13 120.9(4) . . ? C8 C13 C12 118.8(5) . . ? O6 C14 O5 124.3(3) . . ? O6 C14 C15 117.7(3) . . ? O5 C14 C15 117.9(3) . . ? N3 C15 C14 112.0(3) . . ? N3 C15 C16 104.7(3) . . ? C14 C15 C16 112.3(3) . . ? O7 C16 C17 110.2(3) . . ? O7 C16 C15 103.3(3) . . ? C17 C16 C15 115.2(4) . . ? O7 C18 N3 105.5(3) . . ? N4 C19 N3 112.5(3) . . ? O8 C20 N4 122.4(4) . . ? O8 C20 C21 121.7(4) . . ? N4 C20 C21 115.8(3) . . ? C26 C21 C22 118.6(5) . . ? C26 C21 C20 118.3(5) . . ? C22 C21 C20 122.9(4) . . ? C21 C22 C23 120.9(5) . . ? C24 C23 C22 120.0(6) . . ? C23 C24 C25 120.6(6) . . ? C24 C25 C26 120.7(6) . . ? C21 C26 C25 119.0(7) . . ? 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 N2 H2N O6 0.86 2.09 2.862(4) 148.6 4_457 N4 H4N O4 0.86 2.43 3.020(4) 126.2 . _diffrn_measured_fraction_theta_max 0.943 _diffrn_reflns_theta_full 29.17 _diffrn_measured_fraction_theta_full 0.943 _refine_diff_density_max 0.536 _refine_diff_density_min -0.759 _refine_diff_density_rms 0.162