Supplementary Material (ESI) for Perkin Transactions This journal is © The Royal Society of Chemistry 2001 data_gw1 _database_code_CSD 162336 _journal_coden_Cambridge 207 _publ_requested_journal 'Perkin Transactions 1' loop_ _publ_author_name 'Gdaniec, Maria' 'Gdaniec, Zofia' 'Lamparska-Kupsik, Katarzyna' 'Skalski, Bohdan' 'Taras-Goslinska, Katarzyna' 'Wenska, Grazyna' _publ_contact_author_name 'Dr Bohdan Skalski' _publ_contact_author_address ; Chemistry A.Mickiewicz University Grunwaldzka 6 Poznan Poland 60-780 POLAND ; _publ_contact_author_email 'BSKALSKI@AMU.EDU.PL' _publ_section_title ; Photochemical transformations of 5-halogeno-4-thiouridines ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; 3,8-dimethyl-2,7-dioxo-3H,8H-pyrimido[6',5':4,5]tieno[2,3-d]pyrimidine hydrate ; _chemical_name_common ? _chemical_formula_moiety '(C10 H8 N4 O2 S1)2 . 5.75H2O' _chemical_formula_sum 'C20 H27.50 N8 O9.75 S2' _chemical_formula_weight 600.12 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' 'S' 'S' 0.1246 0.1234 '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 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 28.330(1) _cell_length_b 12.851(1) _cell_length_c 19.354(1) _cell_angle_alpha 90.00 _cell_angle_beta 131.75(1) _cell_angle_gamma 90.00 _cell_volume 5256.9(5) _cell_formula_units_Z 8 _cell_measurement_temperature 130(2) _cell_measurement_reflns_used 'not relevant with the CCD camera' _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description PRISM _exptl_crystal_colour COLORLESS _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.517 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2508 _exptl_absorpt_coefficient_mu 0.272 _exptl_absorpt_correction_type NONE _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; CRYSTAL UNSTABLE- COVERED WITH THE EPOXY RESIN' ; _diffrn_ambient_temperature 130(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 'Kuma KM4CCD \k-geometry diffractometer' _diffrn_measurement_method '\w scans' _diffrn_standards_decay_% <1 _diffrn_reflns_number 13019 _diffrn_reflns_av_R_equivalents 0.0500 _diffrn_reflns_av_sigmaI/netI 0.0582 _diffrn_reflns_limit_h_min -33 _diffrn_reflns_limit_h_max 33 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.47 _diffrn_reflns_theta_max 25.02 _reflns_number_total 4634 _reflns_number_gt 3237 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Kuma KM4CCD software (Kuma Diffraction, 2000)' _computing_cell_refinement 'Kuma KM4CCD software (Kuma Diffraction, 2000)' _computing_data_reduction 'Kuma KM4CCD software (Kuma Diffraction, 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ; 'Stereochemical Workstation (Siemens Analytical X-Ray Instruments, Inc., 1989)' ; _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; two water molecules are ordered, the remainig are disordered with occupancy factor 0.5. H atoms of the disordered water molecules were not located. ; _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^)+(0.0988P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens REFMAP _refine_ls_hydrogen_treatment REFALL _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4634 _refine_ls_number_parameters 474 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0973 _refine_ls_R_factor_gt 0.0647 _refine_ls_wR_factor_ref 0.1800 _refine_ls_wR_factor_gt 0.1581 _refine_ls_goodness_of_fit_ref 1.079 _refine_ls_restrained_S_all 1.079 _refine_ls_shift/su_max 0.014 _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 S1B S -0.15460(4) -0.14263(7) -0.06985(6) 0.0287(3) Uani 1 1 d . . . O1B O -0.26481(13) -0.12060(19) 0.04847(18) 0.0343(7) Uani 1 1 d . . . O2B O -0.34425(12) -0.12584(19) -0.46747(18) 0.0338(7) Uani 1 1 d . . . N1B N -0.21249(14) -0.1320(2) -0.0033(2) 0.0267(7) Uani 1 1 d . . . C2B C -0.26597(18) -0.1250(3) -0.0156(3) 0.0282(9) Uani 1 1 d . . . N3B N -0.32609(14) -0.1218(2) -0.1080(2) 0.0280(7) Uani 1 1 d . . . C4B C -0.33133(19) -0.1247(3) -0.1808(3) 0.0266(8) Uani 1 1 d . . . H4B H -0.3739(19) -0.122(3) -0.239(3) 0.028(10) Uiso 1 1 d . . . C5B C -0.27834(18) -0.1313(2) -0.1700(3) 0.0265(8) Uani 1 1 d . . . C6B C -0.21996(17) -0.1349(2) -0.0779(3) 0.0256(8) Uani 1 1 d . . . N7B N -0.31771(15) -0.1297(2) -0.3273(2) 0.0266(7) Uani 1 1 d . . . C8B C -0.30285(18) -0.1292(3) -0.3814(3) 0.0269(8) Uani 1 1 d . . . N9B N -0.23880(14) -0.1336(2) -0.3387(2) 0.0273(7) Uani 1 1 d . . . C10B C -0.19116(18) -0.1384(3) -0.2452(3) 0.0259(8) Uani 1 1 d . . . H10B H -0.142(3) -0.147(4) -0.217(4) 0.076(16) Uiso 1 1 d . . . C11B C -0.20580(17) -0.1375(3) -0.1914(3) 0.0258(8) Uani 1 1 d . . . C12B C -0.27078(17) -0.1327(2) -0.2362(3) 0.0249(8) Uani 1 1 d . . . C13B C -0.3822(2) -0.1138(4) -0.1178(3) 0.0389(11) Uani 1 1 d . . . H13E H -0.418(2) -0.106(3) -0.182(3) 0.044(12) Uiso 1 1 d . . . H13F H -0.379(2) -0.045(4) -0.085(3) 0.067(15) Uiso 1 1 d . . . H13D H -0.376(2) -0.166(4) -0.080(4) 0.077(18) Uiso 1 1 d . . . C14B C -0.2248(2) -0.1378(3) -0.3996(3) 0.0317(9) Uani 1 1 d . . . H14E H -0.2434(19) -0.077(3) -0.443(3) 0.042(12) Uiso 1 1 d . . . H14F H -0.178(3) -0.127(3) -0.367(3) 0.066(15) Uiso 1 1 d . . . H14D H -0.2365(15) -0.202(3) -0.431(2) 0.020(9) Uiso 1 1 d . . . S1A S -0.15591(4) -0.11620(7) 0.26178(6) 0.0281(3) Uani 1 1 d . . . O1A O 0.05425(12) -0.1345(2) 0.58193(19) 0.0387(7) Uani 1 1 d . . . O2A O -0.34606(12) -0.1192(2) 0.28843(19) 0.0366(7) Uani 1 1 d . . . N1A N -0.04132(15) -0.1244(2) 0.4339(2) 0.0314(8) Uani 1 1 d . . . C2A C -0.00415(19) -0.1297(3) 0.5271(3) 0.0301(9) Uani 1 1 d . . . N3A N -0.03300(15) -0.1297(2) 0.5653(2) 0.0312(8) Uani 1 1 d . . . C4A C -0.09575(18) -0.1268(3) 0.5115(3) 0.0290(9) Uani 1 1 d . . . H4A H -0.1110(17) -0.132(3) 0.541(3) 0.025(10) Uiso 1 1 d . . . C5A C -0.13376(17) -0.1225(3) 0.4177(2) 0.0247(8) Uani 1 1 d . . . C6A C -0.10297(18) -0.1217(3) 0.3830(3) 0.0274(8) Uani 1 1 d . . . N7A N -0.24154(14) -0.1203(2) 0.3588(2) 0.0268(7) Uani 1 1 d . . . C8A C -0.30505(18) -0.1171(3) 0.2826(3) 0.0283(9) Uani 1 1 d . . . N9A N -0.32454(14) -0.1112(2) 0.1949(2) 0.0250(7) Uani 1 1 d . . . C10A C -0.28297(17) -0.1105(3) 0.1817(3) 0.0238(8) Uani 1 1 d . . . H10A H -0.3013(18) -0.104(3) 0.114(3) 0.036(11) Uiso 1 1 d . . . C11A C -0.22004(18) -0.1153(3) 0.2571(3) 0.0251(8) Uani 1 1 d . . . C12A C -0.20172(17) -0.1200(2) 0.3452(2) 0.0226(8) Uani 1 1 d . . . C13A C 0.0095(2) -0.1363(5) 0.6659(3) 0.0562(15) Uani 1 1 d . . . H13C H -0.017(3) -0.141(4) 0.675(4) 0.078(18) Uiso 1 1 d . . . H13B H 0.037(2) -0.205(4) 0.684(3) 0.065(15) Uiso 1 1 d . . . H13A H 0.044(3) -0.064(4) 0.695(4) 0.090(18) Uiso 1 1 d . . . C14A C -0.39293(19) -0.1055(3) 0.1145(3) 0.0328(9) Uani 1 1 d . . . H14B H -0.400(2) -0.102(3) 0.056(3) 0.050(13) Uiso 1 1 d . . . H14B' H -0.409(2) -0.042(4) 0.129(4) 0.090(18) Uiso 1 1 d . . . H14A H -0.417(3) -0.171(4) 0.106(4) 0.098(19) Uiso 1 1 d . . . O1W O -0.11094(14) -0.7065(2) 0.1334(2) 0.0407(7) Uani 1 1 d . . . H2W1 H -0.139(3) -0.685(4) 0.062(4) 0.085(17) Uiso 1 1 d . . . H1W1 H -0.132(2) -0.679(4) 0.148(3) 0.066(16) Uiso 1 1 d . . . O2W O 0.0000 -0.5966(4) 0.2500 0.0558(12) Uani 1 2 d S . . H2W H -0.043(3) -0.657(5) 0.207(4) 0.11(2) Uiso 1 1 d . . . O3W O -0.0280(3) -0.5495(5) 0.0860(4) 0.0528(17) Uani 0.50 1 d P . . O4W O -0.0085(3) -0.5259(5) -0.1347(4) 0.0476(15) Uani 0.50 1 d P . . O5W O 0.0286(3) -0.3648(4) 0.1269(4) 0.0405(14) Uani 0.50 1 d P . . O6W O 0.0378(2) -0.3605(4) -0.0098(4) 0.0375(14) Uani 0.50 1 d P . . O7W O 0.0039(4) -0.7360(6) -0.1324(5) 0.073(2) Uani 0.50 1 d P . . O8W O 0.0057(3) -0.1664(5) 0.1657(4) 0.0450(15) Uani 0.50 1 d P . . O9W O 0.0000 -0.8555(7) -0.2500 0.053(2) Uani 0.50 2 d SP . . O10W O -0.0851(3) -0.0733(6) 0.1582(4) 0.0432(16) Uani 0.50 1 d P . . O11W O 0.1022(3) -0.9906(5) -0.1454(4) 0.0394(15) Uani 0.50 1 d P . . 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 S1B 0.0254(5) 0.0279(5) 0.0284(5) -0.0010(4) 0.0161(5) -0.0002(4) O1B 0.0339(16) 0.0401(16) 0.0295(15) -0.0013(12) 0.0214(14) -0.0032(12) O2B 0.0267(15) 0.0401(16) 0.0288(15) 0.0005(12) 0.0161(13) 0.0008(11) N1B 0.0259(17) 0.0237(17) 0.0270(17) -0.0012(13) 0.0162(15) -0.0016(12) C2B 0.031(2) 0.021(2) 0.030(2) -0.0001(15) 0.0186(19) -0.0025(15) N3B 0.0279(18) 0.0297(18) 0.0304(18) -0.0038(13) 0.0211(16) -0.0033(13) C4B 0.026(2) 0.021(2) 0.028(2) -0.0020(15) 0.016(2) -0.0053(15) C5B 0.030(2) 0.0148(18) 0.031(2) -0.0040(15) 0.0184(18) -0.0031(14) C6B 0.026(2) 0.0144(18) 0.028(2) 0.0008(14) 0.0145(18) -0.0027(14) N7B 0.0292(18) 0.0213(16) 0.0315(18) -0.0017(13) 0.0211(16) -0.0019(12) C8B 0.028(2) 0.0199(19) 0.027(2) -0.0012(15) 0.0164(19) -0.0006(15) N9B 0.0293(18) 0.0215(16) 0.0322(18) -0.0012(13) 0.0209(16) 0.0013(12) C10B 0.025(2) 0.0176(18) 0.030(2) -0.0016(15) 0.0163(18) 0.0004(14) C11B 0.027(2) 0.0156(18) 0.030(2) -0.0001(14) 0.0163(18) 0.0023(14) C12B 0.026(2) 0.0165(18) 0.032(2) -0.0029(15) 0.0191(19) -0.0026(14) C13B 0.028(2) 0.057(3) 0.030(2) 0.001(2) 0.019(2) 0.005(2) C14B 0.031(2) 0.034(2) 0.036(2) 0.0024(19) 0.025(2) 0.0051(18) S1A 0.0257(5) 0.0320(5) 0.0282(5) -0.0017(4) 0.0187(5) -0.0011(4) O1A 0.0216(15) 0.0524(19) 0.0347(16) -0.0036(13) 0.0157(14) 0.0000(12) O2A 0.0282(15) 0.0471(17) 0.0435(17) 0.0028(13) 0.0276(14) -0.0002(12) N1A 0.0256(18) 0.039(2) 0.0294(18) -0.0020(14) 0.0183(16) 0.0018(14) C2A 0.030(2) 0.028(2) 0.035(2) -0.0012(16) 0.022(2) 0.0004(16) N3A 0.0274(18) 0.0377(19) 0.0277(17) -0.0019(14) 0.0181(16) 0.0007(13) C4A 0.028(2) 0.031(2) 0.036(2) -0.0028(17) 0.024(2) -0.0018(16) C5A 0.026(2) 0.0233(19) 0.027(2) -0.0018(15) 0.0191(18) -0.0008(15) C6A 0.030(2) 0.0220(19) 0.033(2) -0.0009(15) 0.0222(19) 0.0010(15) N7A 0.0256(17) 0.0271(17) 0.0278(17) -0.0005(13) 0.0178(15) -0.0005(13) C8A 0.032(2) 0.0200(19) 0.037(2) -0.0007(16) 0.025(2) -0.0017(15) N9A 0.0231(16) 0.0220(16) 0.0286(17) -0.0020(12) 0.0167(15) -0.0036(12) C10A 0.025(2) 0.0177(18) 0.028(2) -0.0032(15) 0.0176(18) -0.0025(14) C11A 0.029(2) 0.0179(18) 0.031(2) -0.0021(15) 0.0212(18) -0.0030(15) C12A 0.026(2) 0.0131(17) 0.032(2) 0.0010(14) 0.0211(18) 0.0013(14) C13A 0.031(3) 0.115(5) 0.025(2) 0.002(3) 0.020(2) 0.004(3) C14A 0.025(2) 0.036(2) 0.031(2) -0.0029(18) 0.0156(19) -0.0047(17) O1W 0.0382(17) 0.0513(19) 0.0367(18) 0.0053(14) 0.0266(16) 0.0094(14) O2W 0.038(3) 0.084(4) 0.042(3) 0.000 0.026(2) 0.000 O3W 0.040(4) 0.062(4) 0.051(4) 0.004(3) 0.029(3) -0.009(3) O4W 0.044(4) 0.051(4) 0.046(4) -0.003(3) 0.029(3) 0.002(3) O5W 0.028(3) 0.051(4) 0.031(3) 0.005(3) 0.015(3) 0.003(2) O6W 0.026(3) 0.034(3) 0.044(3) 0.009(2) 0.020(3) 0.005(2) O7W 0.118(6) 0.064(5) 0.090(6) -0.005(4) 0.091(6) -0.021(4) O8W 0.037(3) 0.059(4) 0.045(4) -0.006(3) 0.030(3) 0.002(3) O9W 0.047(6) 0.052(6) 0.052(6) 0.000 0.030(5) 0.000 O10W 0.033(4) 0.054(4) 0.036(4) -0.002(3) 0.020(3) 0.002(3) O11W 0.034(4) 0.045(4) 0.035(4) 0.003(3) 0.021(3) -0.006(3) _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 S1B C6B 1.755(4) . ? S1B C11B 1.759(4) . ? O1B C2B 1.220(4) . ? O2B C8B 1.246(4) . ? N1B C6B 1.313(5) . ? N1B C2B 1.371(5) . ? C2B N3B 1.429(5) . ? N3B C4B 1.316(5) . ? N3B C13B 1.475(5) . ? C4B C5B 1.373(5) . ? C5B C6B 1.411(5) . ? C5B C12B 1.433(5) . ? N7B C12B 1.325(5) . ? N7B C8B 1.364(5) . ? C8B N9B 1.408(5) . ? N9B C10B 1.359(5) . ? N9B C14B 1.474(5) . ? C10B C11B 1.355(5) . ? C11B C12B 1.421(5) . ? S1A C6A 1.752(4) . ? S1A C11A 1.758(4) . ? O1A C2A 1.237(5) . ? O2A C8A 1.240(4) . ? N1A C6A 1.316(5) . ? N1A C2A 1.356(5) . ? C2A N3A 1.422(5) . ? N3A C4A 1.334(5) . ? N3A C13A 1.458(5) . ? C4A C5A 1.361(5) . ? C5A C6A 1.412(5) . ? C5A C12A 1.442(5) . ? N7A C12A 1.317(5) . ? N7A C8A 1.371(5) . ? C8A N9A 1.395(5) . ? N9A C10A 1.360(5) . ? N9A C14A 1.471(5) . ? C10A C11A 1.359(5) . ? C11A C12A 1.415(5) . ? 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 C6B S1B C11B 89.86(17) . . ? C6B N1B C2B 117.4(3) . . ? O1B C2B N1B 123.2(3) . . ? O1B C2B N3B 118.3(3) . . ? N1B C2B N3B 118.6(3) . . ? C4B N3B C2B 122.0(3) . . ? C4B N3B C13B 121.4(3) . . ? C2B N3B C13B 116.6(3) . . ? N3B C4B C5B 120.4(4) . . ? C4B C5B C6B 115.9(3) . . ? C4B C5B C12B 131.6(4) . . ? C6B C5B C12B 112.5(3) . . ? N1B C6B C5B 125.7(4) . . ? N1B C6B S1B 121.1(3) . . ? C5B C6B S1B 113.2(3) . . ? C12B N7B C8B 118.2(3) . . ? O2B C8B N7B 122.0(3) . . ? O2B C8B N9B 118.9(3) . . ? N7B C8B N9B 119.1(3) . . ? C10B N9B C8B 122.1(3) . . ? C10B N9B C14B 120.4(3) . . ? C8B N9B C14B 117.4(3) . . ? C11B C10B N9B 118.9(3) . . ? C10B C11B C12B 117.8(3) . . ? C10B C11B S1B 128.8(3) . . ? C12B C11B S1B 113.4(3) . . ? N7B C12B C11B 123.9(3) . . ? N7B C12B C5B 125.1(3) . . ? C11B C12B C5B 111.0(3) . . ? C6A S1A C11A 90.18(18) . . ? C6A N1A C2A 117.7(3) . . ? O1A C2A N1A 123.7(4) . . ? O1A C2A N3A 117.2(3) . . ? N1A C2A N3A 119.1(3) . . ? C4A N3A C2A 121.5(3) . . ? C4A N3A C13A 122.0(3) . . ? C2A N3A C13A 116.5(3) . . ? N3A C4A C5A 120.2(4) . . ? C4A C5A C6A 116.3(3) . . ? C4A C5A C12A 131.0(3) . . ? C6A C5A C12A 112.6(3) . . ? N1A C6A C5A 125.2(3) . . ? N1A C6A S1A 122.0(3) . . ? C5A C6A S1A 112.8(3) . . ? C12A N7A C8A 118.1(3) . . ? O2A C8A N7A 122.7(4) . . ? O2A C8A N9A 118.4(3) . . ? N7A C8A N9A 118.8(3) . . ? C10A N9A C8A 122.5(3) . . ? C10A N9A C14A 119.8(3) . . ? C8A N9A C14A 117.7(3) . . ? C11A C10A N9A 118.6(3) . . ? C10A C11A C12A 117.5(3) . . ? C10A C11A S1A 128.9(3) . . ? C12A C11A S1A 113.6(3) . . ? N7A C12A C11A 124.4(3) . . ? N7A C12A C5A 124.9(3) . . ? C11A C12A C5A 110.7(3) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.653 _refine_diff_density_min -0.361 _refine_diff_density_rms 0.098