# Supplementary Material (ESI) for Perkin Transactions # This journal is © The Royal Society of Chemistry 2001 data_pn2ak _database_code_CSD 164511 _journal_coden_Cambridge 207 _audit_creation_method 'manual editing of SHELXL-97 cif' _journal_name_full 'Perkin Transactions 1' _publ_section_title ; Synthesis and incorporation of a locked tricyclic nucleoside into oligonucleotides ; _publ_contact_author_name 'Asst Poul Nielsen' _publ_contact_author_address ; Department of Chemistry Technical University of Denmark DTU-207 DK-2800 Lyngby Denmark ; _publ_contact_author_email 'PON@CHEM.SDU.DK' loop_ _publ_author_name _publ_author_address 'Ravn, Jacob' ; Department of Chemistry Odense University DK-5230 Odense M Denmark ; 'Thorup, Niels' ; Department of Chemistry Technical University of Denmark DK-2800 Lyngby Denmark ; 'Nielsen, Poul' ; Department of Chemistry Odense University DK-5230 Odense M Denmark ; _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '(C12 H14 N2 O7), 2(H2 O1)' _chemical_formula_sum 'C12 H18 N2 O9' _chemical_formula_weight 334.28 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 1 2 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' _cell_length_a 24.555(3) _cell_length_b 8.5576(11) _cell_length_c 6.7140(8) _cell_angle_alpha 90.00 _cell_angle_beta 98.416(10) _cell_angle_gamma 90.00 _cell_volume 1395.6(3) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 964 _cell_measurement_theta_min 2.52 _cell_measurement_theta_max 29.44 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.43 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.591 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 704 _exptl_absorpt_coefficient_mu 0.138 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9406 _exptl_absorpt_correction_T_max 0.9743 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2000)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(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/Bruker SMART 1K)' _diffrn_measurement_method 'omega scan, frame data integration' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8619 _diffrn_reflns_av_R_equivalents 0.0145 _diffrn_reflns_av_sigmaI/netI 0.0157 _diffrn_reflns_limit_h_min -32 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 1.68 _diffrn_reflns_theta_max 29.79 _reflns_number_total 3464 _reflns_number_gt 3370 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _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. ; _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^)+(0.0510P)^2^+0.1632P] 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 refall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.2(5) _refine_ls_number_reflns 3464 _refine_ls_number_parameters 280 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0270 _refine_ls_R_factor_gt 0.0262 _refine_ls_wR_factor_ref 0.0690 _refine_ls_wR_factor_gt 0.0685 _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_restrained_S_all 1.040 _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 C2 C 1.00838(4) 0.08414(12) 0.25656(15) 0.01397(19) Uani 1 1 d . . . C4 C 1.03424(4) 0.36188(14) 0.29197(16) 0.01547(19) Uani 1 1 d . . . C5 C 0.97714(4) 0.40275(13) 0.23227(16) 0.0157(2) Uani 1 1 d . . . C7 C 0.96051(5) 0.57129(15) 0.2255(2) 0.0227(2) Uani 1 1 d . . . C6 C 0.94056(4) 0.28694(13) 0.18541(16) 0.01505(19) Uani 1 1 d . . . C1' C 0.91495(4) 0.00842(13) 0.12708(15) 0.01438(19) Uani 1 1 d . . . C2' C 0.88536(4) -0.05630(13) 0.29156(15) 0.01502(19) Uani 1 1 d . . . C3' C 0.83210(4) -0.12127(13) 0.16985(16) 0.0156(2) Uani 1 1 d . . . C4' C 0.82039(4) 0.01678(13) 0.02216(16) 0.01563(19) Uani 1 1 d . . . C5' C 0.79193(4) 0.13768(13) 0.14638(16) 0.0166(2) Uani 1 1 d . . . C6' C 0.80659(4) 0.07212(14) 0.35842(16) 0.0163(2) Uani 1 1 d . . . C7' C 0.79286(4) -0.10171(14) 0.32489(17) 0.0169(2) Uani 1 1 d . . . N1 N 0.95524(4) 0.13146(11) 0.19072(14) 0.01399(17) Uani 1 1 d . . . N3 N 1.04507(4) 0.20390(11) 0.30665(14) 0.01522(18) Uani 1 1 d . . . O2 O 1.02193(3) -0.05299(10) 0.26965(13) 0.01951(16) Uani 1 1 d . . . O4 O 1.07215(3) 0.45643(10) 0.33044(13) 0.02108(17) Uani 1 1 d . . . O8 O 0.81841(4) 0.46596(13) 0.47968(15) 0.0280(2) Uani 1 1 d . . . O9 O 0.88677(4) 0.75067(11) 0.75718(14) 0.02360(18) Uani 1 1 d . . . O2' O 0.86625(3) 0.06811(9) 0.41012(11) 0.01534(15) Uani 1 1 d . . . O3' O 0.83476(3) -0.26947(10) 0.08925(13) 0.01974(17) Uani 1 1 d . . . O4' O 0.87341(3) 0.07000(10) -0.02089(11) 0.01642(15) Uani 1 1 d . . . O5' O 0.80938(3) 0.29354(10) 0.13027(13) 0.01934(17) Uani 1 1 d . . . O7' O 0.73767(3) -0.13335(11) 0.24282(12) 0.02100(18) Uani 1 1 d . . . H1 H 0.9346(6) -0.0740(19) 0.072(2) 0.015(3) Uiso 1 1 d . . . H2 H 0.9067(6) -0.1390(17) 0.375(2) 0.015(3) Uiso 1 1 d . . . H3 H 0.8515(10) -0.259(3) -0.009(4) 0.053(6) Uiso 1 1 d . . . H4 H 0.7967(6) -0.010(2) -0.105(2) 0.021(4) Uiso 1 1 d . . . H5 H 1.0751(9) 0.169(3) 0.350(3) 0.045(6) Uiso 1 1 d . . . H6 H 0.9037(7) 0.306(2) 0.146(3) 0.020(4) Uiso 1 1 d . . . H7 H 0.8049(6) -0.1638(18) 0.444(2) 0.013(3) Uiso 1 1 d . . . H8 H 0.7176(9) -0.115(3) 0.328(3) 0.040(5) Uiso 1 1 d . . . H9 H 0.7916(6) 0.1234(18) 0.466(2) 0.014(3) Uiso 1 1 d . . . H10 H 0.7525(5) 0.1289(16) 0.110(2) 0.005(3) Uiso 1 1 d . . . H11 H 0.7953(8) 0.324(2) 0.023(3) 0.030(5) Uiso 1 1 d . . . H12 H 0.9208(9) 0.582(3) 0.193(3) 0.046(6) Uiso 1 1 d . . . H13 H 0.9711(11) 0.616(4) 0.360(5) 0.074(8) Uiso 1 1 d . . . H14 H 0.9809(9) 0.634(3) 0.148(4) 0.055(6) Uiso 1 1 d . . . H15 H 0.8153(8) 0.424(3) 0.359(3) 0.037(5) Uiso 1 1 d . . . H16 H 0.8546(9) 0.472(2) 0.531(3) 0.039(5) Uiso 1 1 d . . . H17 H 0.9037(10) 0.664(3) 0.727(3) 0.048(6) Uiso 1 1 d . . . H18 H 0.9129(10) 0.835(3) 0.746(3) 0.048(6) 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 C2 0.0113(4) 0.0173(5) 0.0133(4) -0.0011(4) 0.0016(4) -0.0004(4) C4 0.0151(4) 0.0173(5) 0.0141(4) 0.0013(4) 0.0022(4) -0.0003(4) C5 0.0151(5) 0.0159(5) 0.0159(5) 0.0019(4) 0.0018(4) 0.0010(4) C7 0.0209(5) 0.0158(5) 0.0310(6) 0.0028(5) 0.0020(5) 0.0027(4) C6 0.0138(4) 0.0166(5) 0.0148(4) 0.0005(4) 0.0023(4) 0.0017(4) C1' 0.0107(4) 0.0168(5) 0.0150(4) -0.0020(4) -0.0002(4) -0.0003(4) C2' 0.0120(4) 0.0166(5) 0.0160(4) -0.0012(4) 0.0002(3) -0.0002(4) C3' 0.0116(4) 0.0174(5) 0.0173(5) -0.0013(4) 0.0007(3) -0.0014(4) C4' 0.0114(4) 0.0207(5) 0.0145(4) -0.0017(4) 0.0006(4) -0.0002(4) C5' 0.0137(4) 0.0196(5) 0.0160(5) -0.0012(4) 0.0007(4) 0.0026(4) C6' 0.0115(4) 0.0224(5) 0.0148(4) -0.0009(4) 0.0012(4) 0.0008(4) C7' 0.0114(4) 0.0224(5) 0.0165(5) -0.0007(4) 0.0007(4) -0.0022(4) N1 0.0110(4) 0.0150(4) 0.0158(4) -0.0006(3) 0.0015(3) -0.0001(3) N3 0.0107(4) 0.0159(4) 0.0186(4) 0.0003(3) 0.0005(3) 0.0002(3) O2 0.0160(3) 0.0168(4) 0.0252(4) -0.0002(3) 0.0009(3) 0.0011(3) O4 0.0175(4) 0.0177(4) 0.0272(4) 0.0029(3) 0.0005(3) -0.0043(3) O8 0.0227(4) 0.0389(5) 0.0234(4) -0.0052(4) 0.0069(3) -0.0042(4) O9 0.0263(4) 0.0187(4) 0.0270(4) -0.0035(3) 0.0082(3) -0.0026(3) O2' 0.0123(3) 0.0183(4) 0.0150(3) -0.0023(3) 0.0006(3) 0.0003(3) O3' 0.0179(3) 0.0183(4) 0.0235(4) -0.0045(3) 0.0045(3) -0.0024(3) O4' 0.0114(3) 0.0225(4) 0.0147(3) 0.0003(3) -0.0001(3) -0.0011(3) O5' 0.0193(4) 0.0194(4) 0.0181(4) 0.0010(3) -0.0013(3) 0.0029(3) O7' 0.0109(3) 0.0320(5) 0.0200(4) -0.0047(4) 0.0018(3) -0.0042(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. Hydrogen atom positions and isotropic displacement parameters were refined freely. The displacement parameters for hydrogen atoms of the C(7) methyl group are rather high indicating some rotational disorder which probably explains the apparent H(13)-C(7)-H(14) angle of 101.32(3.31) deg. ; 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 O2 1.2194(14) . ? C2 N3 1.3736(14) . ? C2 N1 1.3758(13) . ? C4 O4 1.2319(14) . ? C4 N3 1.3786(15) . ? C4 C5 1.4437(15) . ? C5 C6 1.3435(15) . ? C5 C7 1.4979(16) . ? C7 H12 0.97(2) . ? C7 H13 0.98(3) . ? C7 H14 0.94(2) . ? C6 N1 1.3777(14) . ? C6 H6 0.919(17) . ? C1' O4' 1.4173(13) . ? C1' N1 1.4651(14) . ? C1' C2' 1.5130(14) . ? C1' H1 0.959(15) . ? C2' O2' 1.4480(12) . ? C2' C3' 1.5409(14) . ? C2' H2 1.003(16) . ? C3' O3' 1.3841(14) . ? C3' C7' 1.5275(14) . ? C3' C4' 1.5422(16) . ? C4' O4' 1.4478(12) . ? C4' C5' 1.5571(15) . ? C4' H4 0.991(16) . ? C5' O5' 1.4100(14) . ? C5' C6' 1.5235(15) . ? C5' H10 0.966(13) . ? C6' O2' 1.4555(13) . ? C6' C7' 1.5346(17) . ? C6' H9 0.961(15) . ? C7' O7' 1.4126(12) . ? C7' H7 0.967(15) . ? N3 H5 0.81(2) . ? O8 H15 0.88(2) . ? O8 H16 0.91(2) . ? O9 H17 0.89(2) . ? O9 H18 0.97(2) . ? O3' H3 0.83(2) . ? O5' H11 0.80(2) . ? O7' H8 0.82(2) . ? 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 C2 N3 122.55(10) . . ? O2 C2 N1 122.85(10) . . ? N3 C2 N1 114.60(10) . . ? O4 C4 N3 119.81(10) . . ? O4 C4 C5 124.92(11) . . ? N3 C4 C5 115.27(10) . . ? C6 C5 C4 118.36(10) . . ? C6 C5 C7 122.22(10) . . ? C4 C5 C7 119.42(10) . . ? C5 C7 H12 110.9(13) . . ? C5 C7 H13 108.2(18) . . ? H12 C7 H13 107(2) . . ? C5 C7 H14 113.7(15) . . ? H12 C7 H14 115(2) . . ? H13 C7 H14 101(2) . . ? C5 C6 N1 122.88(10) . . ? C5 C6 H6 122.2(11) . . ? N1 C6 H6 114.9(11) . . ? O4' C1' N1 108.86(9) . . ? O4' C1' C2' 105.93(8) . . ? N1 C1' C2' 115.23(9) . . ? O4' C1' H1 110.8(9) . . ? N1 C1' H1 106.5(9) . . ? C2' C1' H1 109.6(9) . . ? O2' C2' C1' 111.16(9) . . ? O2' C2' C3' 103.80(8) . . ? C1' C2' C3' 101.89(8) . . ? O2' C2' H2 113.3(8) . . ? C1' C2' H2 113.6(8) . . ? C3' C2' H2 112.1(9) . . ? O3' C3' C7' 115.94(9) . . ? O3' C3' C2' 116.94(9) . . ? C7' C3' C2' 99.79(8) . . ? O3' C3' C4' 117.75(9) . . ? C7' C3' C4' 106.10(9) . . ? C2' C3' C4' 97.38(8) . . ? O4' C4' C3' 106.31(8) . . ? O4' C4' C5' 112.65(9) . . ? C3' C4' C5' 102.75(8) . . ? O4' C4' H4 109.5(9) . . ? C3' C4' H4 114.0(10) . . ? C5' C4' H4 111.5(9) . . ? O5' C5' C6' 112.77(10) . . ? O5' C5' C4' 114.97(9) . . ? C6' C5' C4' 101.11(9) . . ? O5' C5' H10 111.0(8) . . ? C6' C5' H10 107.5(8) . . ? C4' C5' H10 108.9(8) . . ? O2' C6' C5' 108.87(8) . . ? O2' C6' C7' 101.77(8) . . ? C5' C6' C7' 101.71(9) . . ? O2' C6' H9 108.3(9) . . ? C5' C6' H9 117.9(9) . . ? C7' C6' H9 116.9(9) . . ? O7' C7' C3' 112.21(9) . . ? O7' C7' C6' 114.88(9) . . ? C3' C7' C6' 93.40(8) . . ? O7' C7' H7 112.1(9) . . ? C3' C7' H7 110.8(9) . . ? C6' C7' H7 112.2(9) . . ? C2 N1 C6 121.66(9) . . ? C2 N1 C1' 116.77(9) . . ? C6 N1 C1' 121.58(9) . . ? C2 N3 C4 126.97(10) . . ? C2 N3 H5 110.0(16) . . ? C4 N3 H5 123.0(16) . . ? H15 O8 H16 108.7(18) . . ? H17 O9 H18 105.3(19) . . ? C2' O2' C6' 106.39(8) . . ? C3' O3' H3 105.8(18) . . ? C1' O4' C4' 108.61(8) . . ? C5' O5' H11 106.6(13) . . ? C7' O7' H8 109.3(15) . . ? 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 O4 C4 C5 C6 176.78(10) . . . . ? N3 C4 C5 C6 -3.80(14) . . . . ? O4 C4 C5 C7 -3.54(16) . . . . ? N3 C4 C5 C7 175.88(10) . . . . ? C4 C5 C6 N1 -0.41(15) . . . . ? C7 C5 C6 N1 179.92(10) . . . . ? O4' C1' C2' O2' -74.14(10) . . . . ? N1 C1' C2' O2' 46.26(11) . . . . ? O4' C1' C2' C3' 35.92(10) . . . . ? N1 C1' C2' C3' 156.32(9) . . . . ? O2' C2' C3' O3' -160.91(9) . . . . ? C1' C2' C3' O3' 83.52(11) . . . . ? O2' C2' C3' C7' -35.06(10) . . . . ? C1' C2' C3' C7' -150.64(9) . . . . ? O2' C2' C3' C4' 72.76(9) . . . . ? C1' C2' C3' C4' -42.81(9) . . . . ? O3' C3' C4' O4' -88.93(11) . . . . ? C7' C3' C4' O4' 139.29(8) . . . . ? C2' C3' C4' O4' 36.82(10) . . . . ? O3' C3' C4' C5' 152.54(9) . . . . ? C7' C3' C4' C5' 20.76(10) . . . . ? C2' C3' C4' C5' -81.71(9) . . . . ? O4' C4' C5' O5' 23.41(13) . . . . ? C3' C4' C5' O5' 137.39(9) . . . . ? O4' C4' C5' C6' -98.37(10) . . . . ? C3' C4' C5' C6' 15.61(10) . . . . ? O5' C5' C6' O2' -63.36(11) . . . . ? C4' C5' C6' O2' 59.94(11) . . . . ? O5' C5' C6' C7' -170.28(8) . . . . ? C4' C5' C6' C7' -46.98(9) . . . . ? O3' C3' C7' O7' -61.59(13) . . . . ? C2' C3' C7' O7' 171.88(9) . . . . ? C4' C3' C7' O7' 71.19(11) . . . . ? O3' C3' C7' C6' 179.75(9) . . . . ? C2' C3' C7' C6' 53.23(9) . . . . ? C4' C3' C7' C6' -47.46(9) . . . . ? O2' C6' C7' O7' -171.08(8) . . . . ? C5' C6' C7' O7' -58.71(11) . . . . ? O2' C6' C7' C3' -54.66(9) . . . . ? C5' C6' C7' C3' 57.71(9) . . . . ? O2 C2 N1 C6 177.22(10) . . . . ? N3 C2 N1 C6 -2.76(14) . . . . ? O2 C2 N1 C1' -2.59(15) . . . . ? N3 C2 N1 C1' 177.43(8) . . . . ? C5 C6 N1 C2 3.95(16) . . . . ? C5 C6 N1 C1' -176.25(9) . . . . ? O4' C1' N1 C2 -151.22(9) . . . . ? C2' C1' N1 C2 90.00(11) . . . . ? O4' C1' N1 C6 28.97(13) . . . . ? C2' C1' N1 C6 -89.81(12) . . . . ? O2 C2 N3 C4 178.06(11) . . . . ? N1 C2 N3 C4 -1.96(15) . . . . ? O4 C4 N3 C2 -175.34(10) . . . . ? C5 C4 N3 C2 5.20(15) . . . . ? C1' C2' O2' C6' 108.88(9) . . . . ? C3' C2' O2' C6' 0.06(10) . . . . ? C5' C6' O2' C2' -71.84(10) . . . . ? C7' C6' O2' C2' 35.04(10) . . . . ? N1 C1' O4' C4' -136.76(8) . . . . ? C2' C1' O4' C4' -12.30(11) . . . . ? C3' C4' O4' C1' -16.40(11) . . . . ? C5' C4' O4' C1' 95.39(10) . . . . ? _diffrn_measured_fraction_theta_max 0.921 _diffrn_reflns_theta_full 29.79 _diffrn_measured_fraction_theta_full 0.921 _refine_diff_density_max 0.232 _refine_diff_density_min -0.225 _refine_diff_density_rms 0.047