data_G7K _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'N7-(carboxymethylguanine)+K' _chemical_melting_point ? _chemical_formula_moiety 'C7 H12 K N5 O6' _chemical_formula_sum 'C7 H12 K N5 O6' _chemical_formula_weight 301.32 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' 'K' 'K' 0.2009 0.2494 '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' 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 16.239(5) _cell_length_b 9.884(4) _cell_length_c 7.574(3) _cell_angle_alpha 90.00 _cell_angle_beta 100.516(5) _cell_angle_gamma 90.00 _cell_volume 1195.3(8) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 2936 _cell_measurement_theta_min 2.4 _cell_measurement_theta_max 28.4 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.674 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 624 _exptl_absorpt_coefficient_mu 0.479 _exptl_absorpt_correction_type PSI-SCAN _exptl_absorpt_correction_T_min 0.9103 _exptl_absorpt_correction_T_max 0.9360 _exptl_absorpt_process_details '(North et al., 1968)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _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 7615 _diffrn_reflns_av_R_equivalents 0.0381 _diffrn_reflns_av_sigmaI/netI 0.0466 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 2.42 _diffrn_reflns_theta_max 28.40 _reflns_number_total 2936 _reflns_number_gt 2294 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART 5.628 (Bruker, 2003)' _computing_cell_refinement 'SMART 5.628 (Bruker, 2003)' _computing_data_reduction 'SAINT+ 6.45 (Bruker, 2003)' _computing_structure_solution Sir92 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'diamond 3.1d' _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^)+(0.0913P)^2^+2.6638P] 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 2936 _refine_ls_number_parameters 196 _refine_ls_number_restraints 9 _refine_ls_R_factor_all 0.0796 _refine_ls_R_factor_gt 0.0539 _refine_ls_wR_factor_ref 0.2098 _refine_ls_wR_factor_gt 0.1347 _refine_ls_goodness_of_fit_ref 1.208 _refine_ls_restrained_S_all 1.206 _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 O6 O 0.15147(15) -0.1220(2) -0.0375(3) 0.0201(5) Uani 1 1 d . . . O2 O 0.33873(16) 0.0888(3) -0.0258(3) 0.0249(6) Uani 1 1 d . . . O1 O 0.38859(15) -0.0587(2) 0.1913(3) 0.0224(5) Uani 1 1 d . . . N3 N 0.02299(17) 0.2368(3) -0.1772(4) 0.0161(6) Uani 1 1 d . . . N1 N 0.03957(17) -0.0024(3) -0.1883(4) 0.0172(6) Uani 1 1 d . . . H1 H 0.0179 -0.0768 -0.2338 0.021 Uiso 1 1 calc R . . N9 N 0.13522(17) 0.3457(3) 0.0262(4) 0.0182(6) Uani 1 1 d . . . N7 N 0.20810(17) 0.1599(3) 0.1325(4) 0.0182(6) Uani 1 1 d . . . C5 C 0.1385(2) 0.1169(3) 0.0096(4) 0.0163(6) Uani 1 1 d . . . C9 C 0.2741(2) 0.0765(3) 0.2308(4) 0.0184(6) Uani 1 1 d . . . H9A H 0.2490 -0.0027 0.2752 0.022 Uiso 1 1 calc R . . H9B H 0.3024 0.1269 0.3341 0.022 Uiso 1 1 calc R . . C10 C 0.3388(2) 0.0303(3) 0.1210(5) 0.0175(6) Uani 1 1 d . . . N2 N -0.07340(17) 0.1062(3) -0.3635(4) 0.0192(6) Uani 1 1 d . . . H2B H -0.1018 0.1779 -0.3985 0.023 Uiso 1 1 calc R . . H2A H -0.0906 0.0285 -0.4066 0.023 Uiso 1 1 calc R . . C4 C 0.0952(2) 0.2329(3) -0.0530(4) 0.0171(6) Uani 1 1 d . . . C8 C 0.2029(2) 0.2963(3) 0.1372(5) 0.0177(7) Uani 1 1 d . . . H8 H 0.2420 0.3506 0.2097 0.021 Uiso 1 1 calc R . . C6 C 0.11437(19) -0.0104(3) -0.0661(4) 0.0150(6) Uani 1 1 d . . . C2 C -0.0024(2) 0.1154(3) -0.2420(5) 0.0165(6) Uani 1 1 d . . . K1 K 0.38752(5) -0.29145(8) -0.00322(10) 0.0247(3) Uani 1 1 d . . . O3W O 0.25492(17) -0.2923(3) 0.2104(4) 0.0297(6) Uani 1 1 d D . . O1W O 0.5513(2) -0.3114(4) 0.0030(5) 0.0378(7) Uani 1 1 d D . . O2W O 0.43770(18) -0.4771(3) 0.2559(4) 0.0363(7) Uani 1 1 d D . . H1W3 H 0.229(3) -0.324(5) 0.281(6) 0.055(18) Uiso 1 1 d D . . H2W3 H 0.225(3) -0.238(5) 0.150(7) 0.07(2) Uiso 1 1 d D . . H1W1 H 0.580(5) -0.245(5) -0.005(12) 0.13(4) Uiso 1 1 d D . . H2W1 H 0.560(5) -0.364(6) -0.074(7) 0.09(3) Uiso 1 1 d D . . H1W2 H 0.412(3) -0.511(7) 0.327(7) 0.08(2) Uiso 1 1 d D . . H2W2 H 0.4865(13) -0.494(5) 0.292(6) 0.039(14) 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 O6 0.0229(12) 0.0142(11) 0.0218(12) 0.0017(9) 0.0005(10) 0.0023(9) O2 0.0227(12) 0.0302(13) 0.0226(13) 0.0044(11) 0.0063(10) 0.0047(10) O1 0.0221(12) 0.0180(11) 0.0274(13) 0.0044(10) 0.0052(10) 0.0046(9) N3 0.0148(12) 0.0151(12) 0.0184(14) 0.0030(10) 0.0029(10) -0.0016(10) N1 0.0219(14) 0.0119(12) 0.0173(14) -0.0019(10) 0.0018(11) -0.0007(10) N9 0.0194(13) 0.0152(13) 0.0190(13) -0.0012(10) 0.0013(11) 0.0010(10) N7 0.0171(13) 0.0182(13) 0.0190(14) -0.0003(11) 0.0025(11) 0.0026(10) C5 0.0186(15) 0.0146(14) 0.0162(15) -0.0034(11) 0.0048(12) -0.0026(11) C9 0.0178(15) 0.0186(15) 0.0174(15) -0.0004(12) -0.0006(12) 0.0008(12) C10 0.0159(14) 0.0140(14) 0.0206(16) -0.0005(12) -0.0024(12) -0.0022(11) N2 0.0162(13) 0.0139(12) 0.0253(15) -0.0023(11) -0.0022(11) 0.0029(10) C4 0.0197(15) 0.0165(14) 0.0159(15) 0.0006(12) 0.0051(12) -0.0014(12) C8 0.0170(15) 0.0170(15) 0.0195(16) -0.0009(12) 0.0042(13) -0.0018(11) C6 0.0118(13) 0.0164(14) 0.0165(15) 0.0027(11) 0.0014(11) 0.0031(11) C2 0.0174(14) 0.0155(14) 0.0173(15) -0.0008(12) 0.0054(12) 0.0008(11) K1 0.0260(4) 0.0254(4) 0.0217(4) -0.0034(3) 0.0022(3) 0.0017(3) O3W 0.0259(14) 0.0313(15) 0.0318(16) 0.0104(12) 0.0049(12) 0.0020(11) O1W 0.0277(15) 0.0383(17) 0.046(2) 0.0038(15) 0.0036(13) -0.0035(13) O2W 0.0206(14) 0.0456(18) 0.0426(18) 0.0187(14) 0.0057(13) 0.0035(12) _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 O6 C6 1.256(4) . ? O2 C10 1.253(4) . ? O1 C10 1.247(4) . ? O1 K1 2.730(3) . ? O1 K1 2.750(3) 4_556 ? N3 C2 1.332(4) . ? N3 C4 1.363(4) . ? N1 C2 1.373(4) . ? N1 C6 1.388(4) . ? N9 C8 1.347(4) . ? N9 C4 1.372(4) . ? N7 C8 1.352(4) . ? N7 C5 1.393(4) . ? N7 C9 1.445(4) . ? C5 C4 1.382(5) . ? C5 C6 1.409(4) . ? C9 C10 1.524(5) . ? N2 C2 1.340(4) . ? K1 O1W 2.659(3) . ? K1 O2W 2.702(3) . ? K1 O1 2.750(3) 4 ? K1 O3W 2.885(3) 4 ? K1 O3W 2.920(3) . ? K1 O2W 3.403(4) 4 ? K1 K1 3.8746(15) 4_556 ? K1 K1 3.8746(15) 4 ? O3W K1 2.885(3) 4_556 ? O2W K1 3.403(4) 4_556 ? 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 C10 O1 K1 115.1(2) . . ? C10 O1 K1 129.5(2) . 4_556 ? K1 O1 K1 89.99(8) . 4_556 ? C2 N3 C4 113.5(3) . . ? C2 N1 C6 124.9(3) . . ? C8 N9 C4 104.3(3) . . ? C8 N7 C5 105.9(3) . . ? C8 N7 C9 126.8(3) . . ? C5 N7 C9 127.2(3) . . ? C4 C5 N7 106.0(3) . . ? C4 C5 C6 121.0(3) . . ? N7 C5 C6 132.5(3) . . ? N7 C9 C10 114.2(3) . . ? O1 C10 O2 126.8(3) . . ? O1 C10 C9 115.9(3) . . ? O2 C10 C9 117.2(3) . . ? N3 C4 N9 123.9(3) . . ? N3 C4 C5 125.4(3) . . ? N9 C4 C5 110.7(3) . . ? N9 C8 N7 113.1(3) . . ? O6 C6 N1 119.9(3) . . ? O6 C6 C5 128.7(3) . . ? N1 C6 C5 111.4(3) . . ? N3 C2 N2 119.0(3) . . ? N3 C2 N1 123.4(3) . . ? N2 C2 N1 117.6(3) . . ? O1W K1 O2W 76.62(10) . . ? O1W K1 O1 98.35(10) . . ? O2W K1 O1 102.05(10) . . ? O1W K1 O1 79.33(10) . 4 ? O2W K1 O1 101.43(10) . 4 ? O1 K1 O1 155.16(8) . 4 ? O1W K1 O3W 129.91(10) . 4 ? O2W K1 O3W 145.68(9) . 4 ? O1 K1 O3W 95.42(8) . 4 ? O1 K1 O3W 68.91(8) 4 4 ? O1W K1 O3W 145.74(10) . . ? O2W K1 O3W 75.56(9) . . ? O1 K1 O3W 68.66(8) . . ? O1 K1 O3W 125.68(8) 4 . ? O3W K1 O3W 83.84(8) 4 . ? O1W K1 O2W 74.38(9) . 4 ? O2W K1 O2W 148.13(11) . 4 ? O1 K1 O2W 69.72(8) . 4 ? O1 K1 O2W 85.99(8) 4 4 ? O3W K1 O2W 65.92(8) 4 4 ? O3W K1 O2W 124.90(8) . 4 ? O1W K1 K1 100.19(8) . 4_556 ? O2W K1 K1 59.16(8) . 4_556 ? O1 K1 K1 45.21(6) . 4_556 ? O1 K1 K1 159.62(6) 4 4_556 ? O3W K1 K1 122.76(6) 4 4_556 ? O3W K1 K1 47.74(6) . 4_556 ? O2W K1 K1 113.68(6) 4 4_556 ? O1W K1 K1 81.63(8) . 4 ? O2W K1 K1 143.12(8) . 4 ? O1 K1 K1 110.37(7) . 4 ? O1 K1 K1 44.80(6) 4 4 ? O3W K1 K1 48.51(6) 4 4 ? O3W K1 K1 132.35(6) . 4 ? O2W K1 K1 42.98(5) 4 4 ? K1 K1 K1 155.58(5) 4_556 4 ? K1 O3W K1 83.75(8) 4_556 . ? K1 O2W K1 77.86(8) . 4_556 ? 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 C8 N7 C5 C4 0.1(3) . . . . ? C9 N7 C5 C4 -178.0(3) . . . . ? C8 N7 C5 C6 172.2(4) . . . . ? C9 N7 C5 C6 -5.9(6) . . . . ? C8 N7 C9 C10 -99.5(4) . . . . ? C5 N7 C9 C10 78.3(4) . . . . ? K1 O1 C10 O2 -61.7(4) . . . . ? K1 O1 C10 O2 -174.4(2) 4_556 . . . ? K1 O1 C10 C9 121.4(2) . . . . ? K1 O1 C10 C9 8.7(4) 4_556 . . . ? N7 C9 C10 O1 -168.9(3) . . . . ? N7 C9 C10 O2 13.9(4) . . . . ? C2 N3 C4 N9 177.0(3) . . . . ? C2 N3 C4 C5 -2.5(5) . . . . ? C8 N9 C4 N3 -179.7(3) . . . . ? C8 N9 C4 C5 -0.1(4) . . . . ? N7 C5 C4 N3 179.6(3) . . . . ? C6 C5 C4 N3 6.3(5) . . . . ? N7 C5 C4 N9 0.0(4) . . . . ? C6 C5 C4 N9 -173.3(3) . . . . ? C4 N9 C8 N7 0.2(4) . . . . ? C5 N7 C8 N9 -0.2(4) . . . . ? C9 N7 C8 N9 178.0(3) . . . . ? C2 N1 C6 O6 -173.9(3) . . . . ? C2 N1 C6 C5 5.5(4) . . . . ? C4 C5 C6 O6 172.1(3) . . . . ? N7 C5 C6 O6 1.0(6) . . . . ? C4 C5 C6 N1 -7.1(4) . . . . ? N7 C5 C6 N1 -178.3(3) . . . . ? C4 N3 C2 N2 179.1(3) . . . . ? C4 N3 C2 N1 0.5(5) . . . . ? C6 N1 C2 N3 -2.3(5) . . . . ? C6 N1 C2 N2 179.0(3) . . . . ? C10 O1 K1 O1W 129.3(2) . . . . ? K1 O1 K1 O1W -96.10(9) 4_556 . . . ? C10 O1 K1 O2W -152.7(2) . . . . ? K1 O1 K1 O2W -18.09(9) 4_556 . . . ? C10 O1 K1 O1 46.7(4) . . . 4 ? K1 O1 K1 O1 -178.74(19) 4_556 . . 4 ? C10 O1 K1 O3W -2.4(2) . . . 4 ? K1 O1 K1 O3W 132.20(8) 4_556 . . 4 ? C10 O1 K1 O3W -83.6(2) . . . . ? K1 O1 K1 O3W 50.99(8) 4_556 . . . ? C10 O1 K1 O2W 59.4(2) . . . 4 ? K1 O1 K1 O2W -165.95(9) 4_556 . . 4 ? C10 O1 K1 K1 -134.6(3) . . . 4_556 ? C10 O1 K1 K1 45.2(2) . . . 4 ? K1 O1 K1 K1 179.78(3) 4_556 . . 4 ? O1W K1 O3W K1 24.58(19) . . . 4_556 ? O2W K1 O3W K1 61.23(9) . . . 4_556 ? O1 K1 O3W K1 -48.17(7) . . . 4_556 ? O1 K1 O3W K1 155.07(8) 4 . . 4_556 ? O3W K1 O3W K1 -146.46(12) 4 . . 4_556 ? O2W K1 O3W K1 -91.60(10) 4 . . 4_556 ? K1 K1 O3W K1 -146.77(7) 4 . . 4_556 ? O1W K1 O2W K1 110.72(10) . . . 4_556 ? O1 K1 O2W K1 14.87(8) . . . 4_556 ? O1 K1 O2W K1 -173.29(6) 4 . . 4_556 ? O3W K1 O2W K1 -104.08(16) 4 . . 4_556 ? O3W K1 O2W K1 -49.08(7) . . . 4_556 ? O2W K1 O2W K1 85.74(19) 4 . . 4_556 ? K1 K1 O2W K1 166.24(6) 4 . . 4_556 ? _diffrn_measured_fraction_theta_max 0.978 _diffrn_reflns_theta_full 28.40 _diffrn_measured_fraction_theta_full 0.978 _refine_diff_density_max 0.660 _refine_diff_density_min -0.798 _refine_diff_density_rms 0.150 data_G9K _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'N9-(carboxymethylguanine)+K' _chemical_melting_point ? _chemical_formula_moiety 'C14 H22 K N10 O11, 4(H2 O)' _chemical_formula_sum 'C14 H30 K N10 O15' _chemical_formula_weight 617.58 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' 'K' 'K' 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' 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 17.936(7) _cell_length_b 9.590(3) _cell_length_c 14.730(5) _cell_angle_alpha 90.00 _cell_angle_beta 104.700(11) _cell_angle_gamma 90.00 _cell_volume 2450.8(15) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 2407 _cell_measurement_theta_min 2.3 _cell_measurement_theta_max 26.0 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.674 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1292 _exptl_absorpt_coefficient_mu 0.312 _exptl_absorpt_correction_type PSI-SCAN _exptl_absorpt_correction_T_min 0.9402 _exptl_absorpt_correction_T_max 0.9576 _exptl_absorpt_process_details '(North et al., 1968)' _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 ? _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 6766 _diffrn_reflns_av_R_equivalents 0.0497 _diffrn_reflns_av_sigmaI/netI 0.0551 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.35 _diffrn_reflns_theta_max 26.00 _reflns_number_total 2407 _reflns_number_gt 1854 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART 5.628 (Bruker, 2003)' _computing_cell_refinement 'SMART 5.628 (Bruker, 2003)' _computing_data_reduction 'SAINT+ 6.45 (Bruker, 2003)' _computing_structure_solution Sir92 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'diamond 3.1d' _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^)+(0.0648P)^2^+1.2506P] 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 2407 _refine_ls_number_parameters 218 _refine_ls_number_restraints 13 _refine_ls_R_factor_all 0.0646 _refine_ls_R_factor_gt 0.0476 _refine_ls_wR_factor_ref 0.1306 _refine_ls_wR_factor_gt 0.1155 _refine_ls_goodness_of_fit_ref 1.070 _refine_ls_restrained_S_all 1.104 _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 C2 C 0.19118(15) -0.0043(3) 0.53263(18) 0.0162(6) Uani 1 1 d . . . C4 C 0.24800(15) 0.1741(3) 0.62015(18) 0.0160(6) Uani 1 1 d . . . C5 C 0.31669(14) 0.1626(3) 0.59548(18) 0.0162(6) Uani 1 1 d . . . C6 C 0.32455(15) 0.0542(3) 0.53236(18) 0.0174(6) Uani 1 1 d . . . C8 C 0.32720(15) 0.3431(3) 0.68143(19) 0.0176(6) Uani 1 1 d . . . H8 H 0.3466 0.4225 0.7156 0.021 Uiso 1 1 calc R . . C9 C 0.19814(15) 0.3430(3) 0.72112(19) 0.0176(6) Uani 1 1 d . . . H9A H 0.1481 0.3426 0.6762 0.021 Uiso 1 1 calc R . . H9B H 0.2106 0.4388 0.7402 0.021 Uiso 1 1 calc R . . C10 C 0.19341(15) 0.2573(3) 0.80686(18) 0.0155(6) Uani 1 1 d . . . N1 N 0.25719(12) -0.0237(2) 0.50411(15) 0.0174(5) Uani 1 1 d . . . H1 H 0.2571 -0.0903 0.4650 0.021 Uiso 1 1 calc R . . N2 N 0.13251(13) -0.0896(2) 0.49513(16) 0.0200(5) Uani 1 1 d . . . H2A H 0.0897 -0.0821 0.5110 0.024 Uiso 1 1 calc R . . H2B H 0.1376 -0.1519 0.4551 0.024 Uiso 1 1 calc R . . N3 N 0.18400(12) 0.0929(2) 0.59474(15) 0.0171(5) Uani 1 1 d . . . N7 N 0.36612(13) 0.2702(2) 0.63343(15) 0.0180(5) Uani 1 1 d . . . N9 N 0.25525(12) 0.2903(2) 0.67615(15) 0.0165(5) Uani 1 1 d . . . O2 O 0.25109(10) 0.1876(2) 0.84722(13) 0.0234(5) Uani 1 1 d . . . O1 O 0.13149(10) 0.26564(19) 0.83117(13) 0.0188(4) Uani 1 1 d . . . O1W O 0.49551(12) 0.3358(2) 0.57235(14) 0.0218(5) Uani 1 1 d D . . O2W O 0.0000 0.5102(3) 0.7500 0.0258(7) Uani 1 2 d SD . . O3W O 0.05294(12) 0.0703(2) 0.67849(14) 0.0218(5) Uani 1 1 d D . . O4W O 0.00317(12) 0.3383(2) 0.59507(14) 0.0218(5) Uani 1 1 d D . . O6 O 0.38180(10) 0.0284(2) 0.50281(13) 0.0202(5) Uani 1 1 d . . . O5W O 0.40140(12) 0.1315(2) 0.85124(15) 0.0220(5) Uani 1 1 d D . . K1 K 0.0000 0.26180(8) 0.7500 0.0126(2) Uani 1 2 d S . . H1W1 H 0.452(2) 0.315(4) 0.594(3) 0.052(11) Uiso 1 1 d D . . H2W1 H 0.527(2) 0.274(4) 0.596(3) 0.049(12) Uiso 1 1 d . . . H1W2 H 0.032(2) 0.567(4) 0.732(3) 0.070(14) Uiso 1 1 d D . . H2W3 H 0.093(2) 0.082(3) 0.651(2) 0.040(10) Uiso 1 1 d D . . H1W3 H 0.029(2) -0.006(4) 0.644(3) 0.059(12) Uiso 1 1 d D . . H2W4 H -0.032(2) 0.406(4) 0.566(3) 0.054(12) Uiso 1 1 d D . . H1W4 H 0.012(2) 0.289(4) 0.552(3) 0.050(12) Uiso 1 1 d D . . H1W5 H 0.399(2) 0.067(4) 0.893(3) 0.047(11) Uiso 1 1 d D . . H2W5 H 0.351(2) 0.162(4) 0.839(3) 0.056(12) 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 C2 0.0162(13) 0.0175(14) 0.0154(13) 0.0031(11) 0.0048(11) 0.0012(11) C4 0.0181(13) 0.0153(14) 0.0146(13) 0.0023(11) 0.0041(11) 0.0018(11) C5 0.0158(13) 0.0177(15) 0.0146(13) 0.0014(10) 0.0028(10) -0.0018(11) C6 0.0178(14) 0.0178(15) 0.0156(14) 0.0019(11) 0.0024(11) -0.0004(11) C8 0.0160(13) 0.0172(15) 0.0191(14) 0.0012(11) 0.0033(11) -0.0013(11) C9 0.0157(13) 0.0166(15) 0.0211(14) -0.0021(11) 0.0055(11) 0.0006(11) C10 0.0142(13) 0.0184(15) 0.0133(13) -0.0021(10) 0.0025(10) -0.0019(11) N1 0.0166(12) 0.0189(13) 0.0172(12) -0.0018(9) 0.0051(9) -0.0004(9) N2 0.0160(12) 0.0226(13) 0.0232(13) -0.0043(10) 0.0083(10) -0.0036(10) N3 0.0171(12) 0.0187(12) 0.0160(12) 0.0002(9) 0.0050(9) -0.0002(9) N7 0.0182(12) 0.0204(13) 0.0159(12) 0.0005(9) 0.0052(9) -0.0001(9) N9 0.0159(11) 0.0180(12) 0.0156(11) 0.0002(9) 0.0041(9) -0.0005(9) O2 0.0187(10) 0.0293(12) 0.0238(11) 0.0089(9) 0.0085(9) 0.0068(9) O1 0.0149(10) 0.0245(11) 0.0178(10) 0.0007(8) 0.0054(8) 0.0003(8) O1W 0.0185(11) 0.0224(12) 0.0264(11) 0.0017(9) 0.0091(9) 0.0013(9) O2W 0.0290(17) 0.0196(16) 0.0331(17) 0.000 0.0156(14) 0.000 O3W 0.0218(11) 0.0201(11) 0.0259(11) -0.0030(9) 0.0105(9) -0.0013(9) O4W 0.0215(11) 0.0263(12) 0.0185(11) 0.0006(9) 0.0070(9) 0.0044(9) O6 0.0151(10) 0.0263(11) 0.0209(10) 0.0005(8) 0.0076(8) 0.0010(8) O5W 0.0185(11) 0.0221(12) 0.0267(12) 0.0031(9) 0.0079(9) 0.0012(9) K1 0.0107(4) 0.0141(4) 0.0136(4) 0.000 0.0044(3) 0.000 _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 C2 N3 1.335(3) . ? C2 N2 1.337(3) . ? C2 N1 1.366(3) . ? C4 N3 1.359(3) . ? C4 N9 1.373(3) . ? C4 C5 1.374(4) . ? C5 N7 1.383(3) . ? C5 C6 1.425(4) . ? C6 O6 1.238(3) . ? C6 N1 1.391(3) . ? C8 N7 1.314(3) . ? C8 N9 1.370(3) . ? C9 N9 1.445(3) . ? C9 C10 1.527(4) . ? C10 O2 1.248(3) . ? C10 O1 1.253(3) . ? O1 K1 2.358(2) . ? O2W K1 2.382(3) . ? O3W K1 2.427(2) . ? O4W K1 2.412(2) . ? K1 O1 2.358(2) 2_556 ? K1 O4W 2.412(2) 2_556 ? K1 O3W 2.427(2) 2_556 ? K1 C10 3.356(3) 2_556 ? 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 N3 C2 N2 120.5(2) . . ? N3 C2 N1 123.2(2) . . ? N2 C2 N1 116.3(2) . . ? N3 C4 N9 125.1(2) . . ? N3 C4 C5 129.2(2) . . ? N9 C4 C5 105.6(2) . . ? C4 C5 N7 111.0(2) . . ? C4 C5 C6 118.3(2) . . ? N7 C5 C6 130.4(2) . . ? O6 C6 N1 121.5(2) . . ? O6 C6 C5 127.1(2) . . ? N1 C6 C5 111.4(2) . . ? N7 C8 N9 113.2(2) . . ? N9 C9 C10 112.7(2) . . ? O2 C10 O1 125.8(2) . . ? O2 C10 C9 117.9(2) . . ? O1 C10 C9 116.2(2) . . ? C2 N1 C6 126.1(2) . . ? C2 N3 C4 111.5(2) . . ? C8 N7 C5 103.9(2) . . ? C8 N9 C4 106.1(2) . . ? C8 N9 C9 127.8(2) . . ? C4 N9 C9 126.1(2) . . ? C10 O1 K1 134.35(17) . . ? O1 K1 O1 178.21(9) . 2_556 ? O1 K1 O2W 89.11(5) . . ? O1 K1 O2W 89.11(5) 2_556 . ? O1 K1 O4W 77.06(7) . 2_556 ? O1 K1 O4W 102.38(7) 2_556 2_556 ? O2W K1 O4W 72.28(6) . 2_556 ? O1 K1 O4W 102.38(7) . . ? O1 K1 O4W 77.06(7) 2_556 . ? O2W K1 O4W 72.28(6) . . ? O4W K1 O4W 144.56(11) 2_556 . ? O1 K1 O3W 104.05(7) . 2_556 ? O1 K1 O3W 77.34(7) 2_556 2_556 ? O2W K1 O3W 139.17(5) . 2_556 ? O4W K1 O3W 73.37(7) 2_556 2_556 ? O4W K1 O3W 138.31(7) . 2_556 ? O1 K1 O3W 77.34(7) . . ? O1 K1 O3W 104.05(7) 2_556 . ? O2W K1 O3W 139.17(5) . . ? O4W K1 O3W 138.31(7) 2_556 . ? O4W K1 O3W 73.37(7) . . ? O3W K1 O3W 81.66(10) 2_556 . ? O1 K1 C10 164.60(6) . 2_556 ? O1 K1 C10 15.48(6) 2_556 2_556 ? O2W K1 C10 90.73(4) . 2_556 ? O4W K1 C10 88.22(7) 2_556 2_556 ? O4W K1 C10 92.22(7) . 2_556 ? O3W K1 C10 66.75(7) 2_556 2_556 ? O3W K1 C10 112.05(7) . 2_556 ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.780 _refine_diff_density_min -0.386 _refine_diff_density_rms 0.086