# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full CrystEngComm _journal_coden_cambridge 1350 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_email libaolong@suda.edu.cn _publ_contact_author_name 'Bao-Long Li' _publ_author_name 'Bao-Long Li' data_znbtreohbdc _database_code_depnum_ccdc_archive 'CCDC 852884' #TrackingRef 'znbtreohbdc.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C11 H15 N3 O8.50 Zn' _chemical_formula_weight 390.63 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' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c _symmetry_space_group_name_Hall '-C 2yc' _symmetry_Int_Tables_number 15 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' '-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 21.783(6) _cell_length_b 11.251(2) _cell_length_c 15.826(4) _cell_angle_alpha 90.00 _cell_angle_beta 130.550(4) _cell_angle_gamma 90.00 _cell_volume 2947.1(13) _cell_formula_units_Z 8 _cell_measurement_temperature 223(2) _cell_measurement_theta_min 3.2 _cell_measurement_theta_max 27.5 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.761 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1600 _exptl_absorpt_coefficient_mu 1.719 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.6447 _exptl_absorpt_correction_T_max 0.8203 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Saturn CCD' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.63 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 8298 _diffrn_reflns_av_R_equivalents 0.0457 _diffrn_reflns_av_sigmaI/netI 0.0653 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.22 _diffrn_reflns_theta_max 27.50 _reflns_number_total 3351 _reflns_number_gt 2642 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0385P)^2^+1.7690P] 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 none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3351 _refine_ls_number_parameters 235 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0781 _refine_ls_R_factor_gt 0.0533 _refine_ls_wR_factor_ref 0.1032 _refine_ls_wR_factor_gt 0.0944 _refine_ls_goodness_of_fit_ref 1.095 _refine_ls_restrained_S_all 1.095 _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 Zn1 Zn 0.14342(2) 0.59193(3) 0.15934(3) 0.02159(14) Uani 1 1 d . . . O1 O 0.26350(14) 0.5874(2) 0.2395(2) 0.0270(6) Uani 1 1 d . . . O2 O 0.26981(14) 0.4189(2) 0.1722(2) 0.0286(6) Uani 1 1 d . . . O3 O 0.51743(15) 0.8190(2) 0.5330(2) 0.0289(6) Uani 1 1 d . . . O4 O 0.62830(15) 0.7591(2) 0.5696(2) 0.0297(6) Uani 1 1 d . . . O5 O 0.57211(14) 0.3634(2) 0.3987(2) 0.0294(6) Uani 1 1 d . . . H5 H 0.5450 0.3034 0.3631 0.044 Uiso 1 1 calc R . . O6 O 0.16804(16) 0.6963(2) 0.2893(2) 0.0272(6) Uani 1 1 d . . . O7 O 0.10908(17) 0.4714(2) 0.0306(2) 0.0280(6) Uani 1 1 d . . . O8 O 0.26761(17) 0.5797(3) 0.4886(2) 0.0356(7) Uani 1 1 d . . . O9 O 0.5000 0.1817(3) 0.2500 0.0273(8) Uani 1 2 d S . . N1 N 0.13455(17) 0.4566(2) 0.2403(2) 0.0233(6) Uani 1 1 d . . . N2 N 0.08793(18) 0.4699(3) 0.2701(3) 0.0300(7) Uani 1 1 d . . . N3 N 0.17110(18) 0.3206(2) 0.3622(2) 0.0239(7) Uani 1 1 d . . . C1 C 0.1843(2) 0.3682(3) 0.2971(3) 0.0236(8) Uani 1 1 d . . . H1A H 0.2233 0.3418 0.2932 0.028 Uiso 1 1 calc R . . C2 C 0.1117(2) 0.3874(3) 0.3432(3) 0.0317(9) Uani 1 1 d . . . H2A H 0.0903 0.3758 0.3785 0.038 Uiso 1 1 calc R . . C3 C 0.2174(2) 0.2248(3) 0.4431(3) 0.0311(9) Uani 1 1 d . . . H3A H 0.2419 0.1750 0.4210 0.037 Uiso 1 1 calc R . . H3B H 0.1813 0.1748 0.4445 0.037 Uiso 1 1 calc R . . C4 C 0.3919(2) 0.5275(3) 0.3062(3) 0.0194(7) Uani 1 1 d . . . C5 C 0.4278(2) 0.6285(3) 0.3721(3) 0.0212(7) Uani 1 1 d . . . H5A H 0.3960 0.6875 0.3694 0.025 Uiso 1 1 calc R . . C6 C 0.5112(2) 0.6418(3) 0.4420(3) 0.0206(7) Uani 1 1 d . . . C7 C 0.5583(2) 0.5529(3) 0.4485(3) 0.0213(7) Uani 1 1 d . . . H7A H 0.6147 0.5618 0.4966 0.026 Uiso 1 1 calc R . . C8 C 0.5224(2) 0.4507(3) 0.3841(3) 0.0205(7) Uani 1 1 d . . . C9 C 0.4390(2) 0.4397(3) 0.3106(3) 0.0206(7) Uani 1 1 d . . . H9A H 0.4142 0.3729 0.2639 0.025 Uiso 1 1 calc R . . C10 C 0.3022(2) 0.5091(3) 0.2342(3) 0.0210(7) Uani 1 1 d . . . C11 C 0.5535(2) 0.7474(3) 0.5182(3) 0.0232(8) Uani 1 1 d . . . H1W H 0.191(2) 0.761(4) 0.302(3) 0.028 Uiso 1 1 d . . . H2W H 0.197(2) 0.669(4) 0.350(3) 0.028 Uiso 1 1 d . . . H3W H 0.078(2) 0.430(3) 0.017(3) 0.028 Uiso 1 1 d . . . H4W H 0.152(2) 0.433(3) 0.053(3) 0.028 Uiso 1 1 d . . . H5W H 0.315(2) 0.604(3) 0.517(3) 0.028 Uiso 1 1 d . . . H6W H 0.263(2) 0.585(3) 0.538(3) 0.028 Uiso 1 1 d . . . H7W H 0.534(2) 0.133(3) 0.257(3) 0.028 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 Zn1 0.0213(2) 0.0197(2) 0.0225(2) 0.00478(18) 0.01368(18) 0.00218(17) O1 0.0193(12) 0.0257(13) 0.0306(14) -0.0037(12) 0.0138(11) 0.0018(11) O2 0.0189(12) 0.0236(13) 0.0311(14) -0.0101(12) 0.0109(11) -0.0038(11) O3 0.0294(14) 0.0234(13) 0.0325(14) -0.0067(12) 0.0196(13) 0.0001(11) O4 0.0229(13) 0.0265(14) 0.0347(15) -0.0116(12) 0.0165(12) -0.0076(11) O5 0.0195(13) 0.0258(14) 0.0382(16) -0.0083(12) 0.0166(12) -0.0015(11) O6 0.0316(15) 0.0194(14) 0.0264(14) 0.0009(12) 0.0170(13) 0.0004(12) O7 0.0236(14) 0.0308(15) 0.0293(14) -0.0034(13) 0.0171(13) -0.0043(12) O8 0.0262(14) 0.0461(18) 0.0287(15) -0.0002(14) 0.0153(13) -0.0056(13) O9 0.026(2) 0.0182(19) 0.041(2) 0.000 0.0230(19) 0.000 N1 0.0249(15) 0.0213(15) 0.0229(15) 0.0012(14) 0.0151(13) -0.0020(13) N2 0.0299(17) 0.0330(18) 0.0346(18) 0.0107(16) 0.0242(15) 0.0066(15) N3 0.0285(16) 0.0192(15) 0.0201(15) 0.0028(13) 0.0142(14) -0.0004(13) C1 0.0259(19) 0.0201(18) 0.0237(18) 0.0014(16) 0.0156(17) -0.0003(15) C2 0.032(2) 0.033(2) 0.034(2) 0.0086(18) 0.0231(19) 0.0038(18) C3 0.041(2) 0.0188(19) 0.0248(19) 0.0073(16) 0.0174(18) 0.0027(17) C4 0.0204(17) 0.0225(18) 0.0146(16) 0.0008(15) 0.0110(14) -0.0014(14) C5 0.0233(17) 0.0172(17) 0.0197(17) 0.0008(15) 0.0125(15) 0.0004(15) C6 0.0225(17) 0.0180(17) 0.0180(17) -0.0007(15) 0.0118(15) -0.0021(15) C7 0.0168(16) 0.0233(18) 0.0226(17) 0.0002(15) 0.0123(15) -0.0016(14) C8 0.0197(17) 0.0201(17) 0.0196(17) -0.0004(15) 0.0118(15) 0.0022(15) C9 0.0217(17) 0.0191(17) 0.0226(17) -0.0026(15) 0.0150(15) -0.0017(14) C10 0.0205(17) 0.0219(18) 0.0164(16) 0.0043(15) 0.0101(15) 0.0005(15) C11 0.0281(19) 0.0202(18) 0.0210(18) -0.0014(15) 0.0159(16) -0.0030(15) _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 Zn1 O1 2.035(2) . ? Zn1 N1 2.078(3) . ? Zn1 O4 2.079(2) 8_465 ? Zn1 O6 2.113(3) . ? Zn1 O7 2.138(3) . ? Zn1 O3 2.324(2) 8_465 ? Zn1 C11 2.530(3) 8_465 ? O1 C10 1.260(4) . ? O2 C10 1.261(4) . ? O3 C11 1.250(4) . ? O3 Zn1 2.324(2) 8_566 ? O4 C11 1.268(4) . ? O4 Zn1 2.079(2) 8_566 ? O5 C8 1.365(4) . ? O5 H5 0.8300 . ? O6 H1W 0.83(4) . ? O6 H2W 0.79(4) . ? O7 H3W 0.74(4) . ? O7 H4W 0.87(4) . ? O8 H5W 0.85(4) . ? O8 H6W 0.85(4) . ? O9 H7W 0.87(3) . ? N1 C1 1.306(4) . ? N1 N2 1.378(4) . ? N2 C2 1.300(5) . ? N3 C1 1.348(4) . ? N3 C2 1.350(5) . ? N3 C3 1.462(4) . ? C1 H1A 0.9400 . ? C2 H2A 0.9400 . ? C3 C3 1.502(7) 7_556 ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C4 C5 1.390(5) . ? C4 C9 1.392(5) . ? C4 C10 1.504(5) . ? C5 C6 1.389(5) . ? C5 H5A 0.9400 . ? C6 C7 1.389(5) . ? C6 C11 1.507(5) . ? C7 C8 1.392(5) . ? C7 H7A 0.9400 . ? C8 C9 1.387(5) . ? C9 H9A 0.9400 . ? C11 Zn1 2.530(3) 8_566 ? 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 Zn1 N1 101.22(11) . . ? O1 Zn1 O4 90.83(10) . 8_465 ? N1 Zn1 O4 167.01(11) . 8_465 ? O1 Zn1 O6 89.85(10) . . ? N1 Zn1 O6 82.73(11) . . ? O4 Zn1 O6 92.55(11) 8_465 . ? O1 Zn1 O7 95.14(10) . . ? N1 Zn1 O7 90.43(11) . . ? O4 Zn1 O7 93.34(11) 8_465 . ? O6 Zn1 O7 172.22(11) . . ? O1 Zn1 O3 150.20(9) . 8_465 ? N1 Zn1 O3 108.37(10) . 8_465 ? O4 Zn1 O3 59.39(9) 8_465 8_465 ? O6 Zn1 O3 90.46(10) . 8_465 ? O7 Zn1 O3 88.17(10) . 8_465 ? O1 Zn1 C11 120.76(11) . 8_465 ? N1 Zn1 C11 137.63(12) . 8_465 ? O4 Zn1 C11 29.95(10) 8_465 8_465 ? O6 Zn1 C11 91.33(11) . 8_465 ? O7 Zn1 C11 91.23(11) . 8_465 ? O3 Zn1 C11 29.45(10) 8_465 8_465 ? C10 O1 Zn1 128.4(2) . . ? C11 O3 Zn1 84.5(2) . 8_566 ? C11 O4 Zn1 95.1(2) . 8_566 ? C8 O5 H5 109.5 . . ? Zn1 O6 H1W 117(3) . . ? Zn1 O6 H2W 117(3) . . ? H1W O6 H2W 100(4) . . ? Zn1 O7 H3W 111(3) . . ? Zn1 O7 H4W 108(2) . . ? H3W O7 H4W 111(4) . . ? H5W O8 H6W 108(4) . . ? C1 N1 N2 108.2(3) . . ? C1 N1 Zn1 128.0(2) . . ? N2 N1 Zn1 121.1(2) . . ? C2 N2 N1 105.8(3) . . ? C1 N3 C2 104.9(3) . . ? C1 N3 C3 126.4(3) . . ? C2 N3 C3 128.5(3) . . ? N1 C1 N3 109.6(3) . . ? N1 C1 H1A 125.2 . . ? N3 C1 H1A 125.2 . . ? N2 C2 N3 111.5(3) . . ? N2 C2 H2A 124.3 . . ? N3 C2 H2A 124.3 . . ? N3 C3 C3 110.3(4) . 7_556 ? N3 C3 H3A 109.6 . . ? C3 C3 H3A 109.6 7_556 . ? N3 C3 H3B 109.6 . . ? C3 C3 H3B 109.6 7_556 . ? H3A C3 H3B 108.1 . . ? C5 C4 C9 120.3(3) . . ? C5 C4 C10 120.1(3) . . ? C9 C4 C10 119.5(3) . . ? C6 C5 C4 119.5(3) . . ? C6 C5 H5A 120.2 . . ? C4 C5 H5A 120.2 . . ? C7 C6 C5 120.1(3) . . ? C7 C6 C11 118.0(3) . . ? C5 C6 C11 121.7(3) . . ? C6 C7 C8 120.3(3) . . ? C6 C7 H7A 119.8 . . ? C8 C7 H7A 119.8 . . ? O5 C8 C9 122.7(3) . . ? O5 C8 C7 117.7(3) . . ? C9 C8 C7 119.6(3) . . ? C8 C9 C4 120.0(3) . . ? C8 C9 H9A 120.0 . . ? C4 C9 H9A 120.0 . . ? O1 C10 O2 123.6(3) . . ? O1 C10 C4 116.7(3) . . ? O2 C10 C4 119.7(3) . . ? O3 C11 O4 121.0(3) . . ? O3 C11 C6 121.7(3) . . ? O4 C11 C6 117.3(3) . . ? O3 C11 Zn1 66.07(19) . 8_566 ? O4 C11 Zn1 54.94(17) . 8_566 ? C6 C11 Zn1 171.7(3) . 8_566 ? 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 N1 Zn1 O1 C10 70.3(3) . . . . ? O4 Zn1 O1 C10 -114.6(3) 8_465 . . . ? O6 Zn1 O1 C10 152.9(3) . . . . ? O7 Zn1 O1 C10 -21.1(3) . . . . ? O3 Zn1 O1 C10 -116.4(3) 8_465 . . . ? C11 Zn1 O1 C10 -115.6(3) 8_465 . . . ? O1 Zn1 N1 C1 -20.9(3) . . . . ? O4 Zn1 N1 C1 -178.6(4) 8_465 . . . ? O6 Zn1 N1 C1 -109.3(3) . . . . ? O7 Zn1 N1 C1 74.4(3) . . . . ? O3 Zn1 N1 C1 162.6(3) 8_465 . . . ? C11 Zn1 N1 C1 166.7(3) 8_465 . . . ? O1 Zn1 N1 N2 137.9(2) . . . . ? O4 Zn1 N1 N2 -19.7(6) 8_465 . . . ? O6 Zn1 N1 N2 49.6(2) . . . . ? O7 Zn1 N1 N2 -126.7(2) . . . . ? O3 Zn1 N1 N2 -38.5(3) 8_465 . . . ? C11 Zn1 N1 N2 -34.4(3) 8_465 . . . ? C1 N1 N2 C2 -0.5(4) . . . . ? Zn1 N1 N2 C2 -163.1(2) . . . . ? N2 N1 C1 N3 1.2(4) . . . . ? Zn1 N1 C1 N3 162.2(2) . . . . ? C2 N3 C1 N1 -1.4(4) . . . . ? C3 N3 C1 N1 -176.1(3) . . . . ? N1 N2 C2 N3 -0.4(4) . . . . ? C1 N3 C2 N2 1.1(4) . . . . ? C3 N3 C2 N2 175.6(3) . . . . ? C1 N3 C3 C3 94.3(5) . . . 7_556 ? C2 N3 C3 C3 -79.1(6) . . . 7_556 ? C9 C4 C5 C6 0.5(5) . . . . ? C10 C4 C5 C6 177.0(3) . . . . ? C4 C5 C6 C7 -2.0(5) . . . . ? C4 C5 C6 C11 -177.8(3) . . . . ? C5 C6 C7 C8 0.8(5) . . . . ? C11 C6 C7 C8 176.7(3) . . . . ? C6 C7 C8 O5 -176.2(3) . . . . ? C6 C7 C8 C9 2.0(5) . . . . ? O5 C8 C9 C4 174.6(3) . . . . ? C7 C8 C9 C4 -3.6(5) . . . . ? C5 C4 C9 C8 2.4(5) . . . . ? C10 C4 C9 C8 -174.2(3) . . . . ? Zn1 O1 C10 O2 2.5(5) . . . . ? Zn1 O1 C10 C4 -178.1(2) . . . . ? C5 C4 C10 O1 -1.5(5) . . . . ? C9 C4 C10 O1 175.1(3) . . . . ? C5 C4 C10 O2 177.9(3) . . . . ? C9 C4 C10 O2 -5.5(5) . . . . ? Zn1 O3 C11 O4 -1.3(3) 8_566 . . . ? Zn1 O3 C11 C6 176.7(3) 8_566 . . . ? Zn1 O4 C11 O3 1.4(4) 8_566 . . . ? Zn1 O4 C11 C6 -176.6(3) 8_566 . . . ? C7 C6 C11 O3 -166.0(3) . . . . ? C5 C6 C11 O3 9.8(5) . . . . ? C7 C6 C11 O4 12.0(5) . . . . ? C5 C6 C11 O4 -172.2(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 O5 H5 O9 0.83 1.94 2.716(4) 155.6 . O6 H1W O2 0.83(4) 1.90(4) 2.721(4) 171(4) 4 O6 H2W O8 0.79(4) 1.95(4) 2.734(4) 171(4) . O7 H3W O3 0.74(4) 2.08(4) 2.818(4) 175(5) 4_545 O7 H4W O2 0.87(4) 1.96(4) 2.725(4) 145(3) . O8 H5W O5 0.85(4) 1.93(4) 2.772(4) 170(4) 5_666 O8 H6W O2 0.85(4) 2.04(4) 2.876(4) 171(4) 6_566 O9 H7W N2 0.87(3) 2.12(4) 2.942(4) 159(3) 3_545 _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.365 _refine_diff_density_min -0.384 _refine_diff_density_rms 0.089