Supplementary Material (ESI) for PCCP This journal is © The Owner Societies 2007 data_global _journal_name_full Phys.Chem.Chem.Phys.(PCCP) _journal_coden_Cambridge 1326 _publ_contact_author_name 'Jon Are Beukes' _publ_contact_author_address ;The Norwegian University of Science and Technology Department of Physics N-7491 Trondheim Norway ; _publ_contact_author_email beukes@ntnu.no _publ_contact_author_phone +4773593273 loop_ _publ_author_name _publ_author_address J.A.Beukes ;The Norwegian University of Science and Technology Department of Physics N-7491 Trondheim Norway ; F.Mo ;The Norwegian University of Science and Technology Department of Physics N-7491 Trondheim Norway ; 'Wouter van Beek' ; ? ; _publ_section_title ; X-ray induced radiation damage in taurine - A combined X-ray diffraction and Raman study ; data_tau1_2cif120k _database_code_depnum_ccdc_archive 'CCDC 638411' _audit_creation_date ; 'Thu May 18 12:00:32 2006' ; _audit_creation_method ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.29.8 (release 17-03-2006 CrysAlis171 .NET) (compiled Mar 17 2006,10:57:34) and SHELXL-97 and manual editing ; _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.29.8 (release 17-03-2006 CrysAlis171 .NET) (compiled Mar 17 2006,10:57:34) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.29.8 (release 17-03-2006 CrysAlis171 .NET) (compiled Mar 17 2006,10:57:34) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.29.8 (release 17-03-2006 CrysAlis171 .NET) (compiled Mar 17 2006,10:57:34) ; _chemical_name_systematic '2-aminoethane sulfonic acid' _chemical_name_common '2-aminoethane sulfonic acid' _chemical_melting_point 328 _chemical_formula_moiety 'C2 H7 N O3 S' _chemical_formula_sum 'C2 H7 N O3 S' _chemical_formula_weight 125.15 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0031 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 0.0109 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1248 0.1237 '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' _symmetry_int_tables_number 14 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 5.2737(10) _cell_length_b 11.658(2) _cell_length_c 7.7995(15) _cell_angle_alpha 90.00 _cell_angle_beta 94.070(15) _cell_angle_gamma 90.00 _cell_volume 478.29(15) _cell_formula_units_Z 4 _cell_measurement_temperature 120.0(2) _cell_measurement_reflns_used 4239 _cell_measurement_theta_min 4.2515 _cell_measurement_theta_max 41.3872 _exptl_crystal_description Prism _exptl_crystal_colour Transparent _exptl_crystal_size_max 0.125 _exptl_crystal_size_mid 0.100 _exptl_crystal_size_min 0.075 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.738 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 264 _exptl_absorpt_coefficient_mu 0.500 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0 _exptl_absorpt_correction_T_max 0 _exptl_absorpt_process_details none _exptl_special_details ; ? ; _diffrn_ambient_temperature 120.0(2) _diffrn_radiation_probe x-ray _diffrn_radiation_type Synchrotron _diffrn_radiation_wavelength 0.7100 _diffrn_source Synchrotron _diffrn_source_type ESRF _diffrn_radiation_monochromator 'Si 111' _diffrn_measurement_device_type 'Oxford diffraction, KM 6, Onyx' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 8.2896 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 5066 _diffrn_reflns_av_R_equivalents 0.0413 _diffrn_reflns_av_sigmaI/netI 0.0325 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 4.25 _diffrn_reflns_theta_max 32.17 _reflns_number_total 1626 _reflns_number_gt 1483 _reflns_threshold_expression >2sigma(I) _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega -124.00 92.00 1.0000 10.0000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - -15.0000 0.0000 0.0000 0.0000 0.0000 216 #__ type_ start__ end____ width___ exp.time_ 2 omega -64.00 152.00 1.0000 20.0000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - 45.0000 0.0000 0.0000 0.0000 0.0000 216 ; _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _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. The parameters for all atoms including the hydrogen atoms were refined until convergence and the hydrogen distances were then normalized to C-H = 1.10 and N-H = 1.045. . With the H atomic parameters fixed the coordinates and the ADPs of the non-H atoms were refined on data with sin(theta)/lambda > 0.60 A-1. With the coordinates of all atoms fixed, the ADPs of the non-H atoms were refined on the full data set. ; _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^)+(0.0541P)^2^+0.1738P] 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 0 _refine_ls_number_reflns 1626 _refine_ls_number_parameters 92 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0353 _refine_ls_R_factor_gt 0.0326 _refine_ls_wR_factor_ref 0.0921 _refine_ls_wR_factor_gt 0.0905 _refine_ls_goodness_of_fit_ref 1.101 _refine_ls_restrained_S_all 1.101 _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 S1 S 0.79810(6) 0.65011(3) 0.14980(5) 0.0108(2) Uani 1 1 d . . . O1 O 1.0673(2) 0.66154(11) 0.2094(2) 0.0158(3) Uani 1 1 d . . . O2 O 0.6584(2) 0.75798(11) 0.1466(2) 0.0169(3) Uani 1 1 d . . . O3 O 0.7697(2) 0.58738(10) -0.0139(2) 0.0140(3) Uani 1 1 d . . . C1 C 0.7908(3) 0.44319(12) 0.3205(2) 0.0137(4) Uani 1 1 d . . . C2 C 0.6612(3) 0.56018(13) 0.3032(2) 0.0127(4) Uani 1 1 d . . . N1 N 0.7330(2) 0.36971(12) 0.1670(2) 0.0126(4) Uani 1 1 d . . . H1A H 0.726(3) 0.398(2) 0.434(2) 0.018(4) Uiso 1 1 d . . . H1B H 0.998(4) 0.455(2) 0.334(3) 0.022(5) Uiso 1 1 d . . . H2A H 0.683(3) 0.609(2) 0.424(2) 0.018(4) Uiso 1 1 d . . . H2B H 0.461(4) 0.552(2) 0.255(3) 0.025(5) Uiso 1 1 d . . . H1 H 0.828(4) 0.396(2) 0.061(3) 0.022(5) Uiso 1 1 d . . . H2 H 0.806(4) 0.288(2) 0.195(3) 0.024(5) Uiso 1 1 d . . . H3 H 0.538(4) 0.364(2) 0.134(3) 0.023(5) 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 S1 0.0085(3) 0.0098(3) 0.0142(3) -0.00009(16) 0.00137(18) 0.00036(15) O1 0.0090(7) 0.0146(7) 0.0234(8) -0.0007(6) -0.0015(5) -0.0026(5) O2 0.0173(7) 0.0130(7) 0.0208(8) 0.0021(6) 0.0046(6) 0.0052(5) O3 0.0132(6) 0.0151(7) 0.0137(7) -0.0010(5) 0.0013(5) 0.0001(5) C1 0.0140(9) 0.0134(10) 0.0135(10) 0.0007(7) -0.0009(7) -0.0005(7) C2 0.0111(8) 0.0142(10) 0.0131(10) 0.0005(7) 0.0029(7) -0.0006(7) N1 0.0106(7) 0.0118(8) 0.0155(9) 0.0000(7) 0.0013(6) 0.0003(6) _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 S1 O2 1.4568(13) . ? S1 O1 1.4680(13) . ? S1 O3 1.4697(14) . ? S1 C2 1.7816(16) . ? C1 N1 1.4861(21) . ? C1 C2 1.5273(20) . ? 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 O2 S1 O1 113.81(7) . . ? O2 S1 O3 113.23(7) . . ? O1 S1 O3 110.90(8) . . ? O2 S1 C2 106.91(7) . . ? O1 S1 C2 105.65(7) . . ? O3 S1 C2 105.63(7) . . ? N1 C1 C2 112.24(12) . . ? C1 C2 S1 112.62(10) . . ? _diffrn_measured_fraction_theta_max 0.966 _diffrn_reflns_theta_full 32.17 _diffrn_measured_fraction_theta_full 0.966 _refine_diff_density_max 0.446 _refine_diff_density_min -0.599 _refine_diff_density_rms 0.088 # Attachment 'Taurine_296K_Depot.cif' data_fulltau2_3 _database_code_depnum_ccdc_archive 'CCDC 638412' _audit_creation_date ; 'Thu May 18 11:12:32 2006' ; _audit_creation_method ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.29.8 (release 17-03-2006 CrysAlis171 .NET) (compiled Mar 17 2006,10:57:34) and SHELXL-97 and manual editing ; _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.29.8 (release 17-03-2006 CrysAlis171 .NET) (compiled Mar 17 2006,10:57:34) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.29.8 (release 17-03-2006 CrysAlis171 .NET) (compiled Mar 17 2006,10:57:34) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.29.8 (release 17-03-2006 CrysAlis171 .NET) (compiled Mar 17 2006,10:57:34) ; _chemical_name_systematic '2-aminoethane sulfonic acid' _chemical_name_common '2-aminoethane sulfonic acid' _chemical_melting_point 328 _chemical_formula_moiety 'C2 H7 N O3 S' _chemical_formula_sum 'C2 H7 N O3 S' _chemical_formula_weight 125.15 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 0.0017 '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 0.0065 0.0034 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0114 0.0063 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1293 0.1292 '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' _symmetry_int_tables_number 14 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 5.2815(11) _cell_length_b 11.644(2) _cell_length_c 7.9276(16) _cell_angle_alpha 90.00 _cell_angle_beta 94.09(3) _cell_angle_gamma 90.00 _cell_volume 486.29(17) _cell_formula_units_Z 4 _cell_measurement_temperature 296(1) _cell_measurement_reflns_used 2110 _cell_measurement_theta_min 4.3343 _cell_measurement_theta_max 24.6007 _exptl_crystal_description Prism _exptl_crystal_colour Transparent _exptl_crystal_size_max 0.125 _exptl_crystal_size_mid 0.100 _exptl_crystal_size_min 0.075 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.709 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 264 _exptl_absorpt_coefficient_mu 0.525 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.0 _exptl_absorpt_correction_T_max 0.0 _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(1) _diffrn_radiation_probe x-ray _diffrn_radiation_type Synchrotron _diffrn_radiation_wavelength 0.7256(1) _diffrn_source Synchrotron _diffrn_source_type ESRF _diffrn_radiation_monochromator 'Si 111' _diffrn_measurement_device_type 'Oxford diffraction, KM 6, Onyx' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 8.2896 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 7608 _diffrn_reflns_av_R_equivalents 0.0241 _diffrn_reflns_av_sigmaI/netI 0.0235 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 3.57 _diffrn_reflns_theta_max 43.17 _reflns_number_total 3044 _reflns_number_gt 2366 _reflns_threshold_expression >2sigma(I) _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega -124.00 92.00 1.0000 10.0000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - -15.0000 0.0000 0.0000 0.0000 0.0000 216 #__ type_ start__ end____ width___ exp.time_ 2 omega -64.00 152.00 1.0000 20.0000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - 45.0000 0.0000 0.0000 0.0000 0.0000 216 ; _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _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. The parameters for all atoms including the hydrogen atoms were refined until convergence on the full data set, the hydrogen distances were then normalized to C-H = 1.10 and N-H = 1.045. With the H atomic parameters fixed the coordinates and the ADPs of the non-H atoms were refined on data with sin(theta)/lambda > 0.75 A-1. At convergence the coordinates of the non-H atoms were fixed, and the non-H ADPs and the H atomic positions and isotropic ADPs were refined again on the full data set, wherupon the H atomic coordinates were renormalized and fixed. The non-H positions and ADPs were subsequently refined once more with data at sin(theta)/lambda > 0.75 A-1. With the coordinates of all atoms fixed, the ADPs of the non-H atoms were refined on the full data set. ; _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^)+(0.0587P)^2^+0.0538P] 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 none _refine_ls_number_reflns 3044 _refine_ls_number_parameters 92 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0445 _refine_ls_R_factor_gt 0.0324 _refine_ls_wR_factor_ref 0.1017 _refine_ls_wR_factor_gt 0.0897 _refine_ls_goodness_of_fit_ref 1.042 _refine_ls_restrained_S_all 1.042 _refine_ls_shift/su_max 0.002 _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 S1 S 0.79683(4) 0.65139(2) 0.14913(4) 0.0243(2) Uani 1 1 d . . . O1 O 1.06502(19) 0.66229(11) 0.20633(25) 0.0379(4) Uani 1 1 d . . . O2 O 0.65798(29) 0.75877(11) 0.14561(24) 0.0393(4) Uani 1 1 d . . . O3 O 0.76827(22) 0.58899(10) -0.01141(17) 0.0314(3) Uani 1 1 d . . . C1 C 0.78951(23) 0.44513(11) 0.31835(18) 0.0299(4) Uani 1 1 d . . . C2 C 0.66001(21) 0.56129(11) 0.29990(18) 0.0276(4) Uani 1 1 d . . . N1 N 0.73622(19) 0.37063(9) 0.16862(17) 0.0274(4) Uani 1 1 d . . . H2A H 0.684(3) 0.6077(14) 0.4213(18) 0.038(4) Uiso 1 1 d . . . H2B H 0.459(3) 0.5584(15) 0.2547(20) 0.042(4) Uiso 1 1 d . . . H1A H 0.725(3) 0.4034(14) 0.4319(18) 0.037(4) Uiso 1 1 d . . . H1B H 0.997(3) 0.4528(15) 0.3393(22) 0.044(4) Uiso 1 1 d . . . H1 H 0.831(4) 0.4058(17) 0.0695(22) 0.051(5) Uiso 1 1 d . . . H3 H 0.541(4) 0.3752(16) 0.1347(22) 0.049(5) Uiso 1 1 d . . . H2 H 0.798(3) 0.2865(16) 0.1926(24) 0.050(5) 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 S1 0.0207(3) 0.0183(3) 0.0339(3) -0.00075(15) 0.00265(19) 0.00096(14) O1 0.0225(8) 0.0295(8) 0.0608(10) -0.0037(7) -0.0031(7) -0.0059(5) O2 0.0421(8) 0.0258(7) 0.0510(9) 0.0045(6) 0.0109(7) 0.0129(6) O3 0.0331(7) 0.0303(7) 0.0310(7) -0.0022(6) 0.0039(5) 0.0002(6) C1 0.0309(10) 0.0255(10) 0.0326(10) 0.0035(7) -0.0033(8) -0.0013(7) C2 0.0268(9) 0.0263(9) 0.0302(9) -0.0007(7) 0.0047(7) -0.0006(7) N1 0.0254(8) 0.0228(8) 0.0341(9) 0.0018(6) 0.0036(6) 0.0015(6) _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 S1 O1 1.4616(11) . ? S1 O2 1.4488(14) . ? S1 O3 1.4639(14) . ? S1 C2 1.7818(14) . ? C1 N1 1.4809(19) . ? C1 C2 1.5180(18) . ? 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 S1 O2 114.14(8) . . ? O1 S1 O3 110.50(8) . . ? O2 S1 O3 113.02(8) . . ? O1 S1 C2 105.87(6) . . ? O2 S1 C2 106.98(7) . . ? O3 S1 C2 105.63(7) . . ? N1 C1 C2 112.72(11) . . ? C1 C2 S1 112.82(9) . . ? _diffrn_measured_fraction_theta_max 0.895 _diffrn_reflns_theta_full 43.17 _diffrn_measured_fraction_theta_full 0.895 _refine_diff_density_max 0.344 _refine_diff_density_min -0.563 _refine_diff_density_rms 0.070 _chemical_compound_source Commercial _exptl_crystal_recrystallization_method Water _diffrn_ambient_pressure 100