Supplementary Material (ESI) for J. Mater. Chem. This journal is (C) The Royal Society of Chemistry 2003 data_global _journal_coden_Cambridge 1145 loop_ _publ_author_name 'M. Stanley Whittingham' 'Natasha A. Chernova' 'Samuel T. Lutta' 'Peter Y. Zavalij' _publ_contact_author_name 'Prof M. Stanley Whittingham' _publ_contact_author_address ; Department of Chemistry and Materials SUNY at Binghamton Vestal Parkway East Binghamton New York 13902-6016 UNITED STATES OF AMERICA ; _publ_contact_author_email STANWHIT@BINGHAMTON.EDU _publ_requested_journal 'Journal of Materials Chemistry' _publ_section_title ; Solvothermal synthesis and characterization of a layered pyridinium vanadate, (C5H6N)V3O7 ; data_PyV3O7_0266 _database_code_CSD 198811 _chemical_name_systematic 'pyridinium trivanadate heptaoxide' _chemical_formula_moiety '(C5 H5 N H)1+, V3 O7' _chemical_formula_sum 'C5 H6 N O7 V3' _chemical_formula_weight 344.93 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' V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 7.5296(9) _cell_length_b 6.6592(8) _cell_length_c 10.1513(12) _cell_angle_alpha 90.00 _cell_angle_beta 94.460(2) _cell_angle_gamma 90.00 _cell_volume 507.46(10) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 2909 _cell_measurement_theta_min 5.427 _cell_measurement_theta_max 61.867 _exptl_crystal_description plate _exptl_crystal_colour black _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.025 _exptl_crystal_density_diffrn 2.257 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 336 _exptl_absorpt_coefficient_mu 2.723 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7392 _exptl_absorpt_correction_T_max 0.9342 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _diffrn_ambient_temperature 296(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 'Bruker SmartApex CCD area detector' _diffrn_measurement_method '\w scans' _diffrn_standards_decay_% 0.00 _diffrn_reflns_number 5774 _diffrn_reflns_av_R_equivalents 0.0319 _diffrn_reflns_av_sigmaI/netI 0.0568 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.01 _diffrn_reflns_theta_max 30.03 _reflns_number_total 2902 _reflns_number_gt 2577 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 1999)' _computing_cell_refinement 'SAINT (Bruker, 1999)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-3 (Farrugia,1997), ATOMS (Dowty,1999)' _computing_publication_material SHELXL-97 _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 '1/[\s^2^(Fo^2^)+(0.0540P)^2^], 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 constr _refine_ls_extinction_method none _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.05(4) _refine_ls_number_reflns 2902 _refine_ls_number_parameters 145 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0491 _refine_ls_R_factor_gt 0.0406 _refine_ls_wR_factor_ref 0.0984 _refine_ls_wR_factor_gt 0.0934 _refine_ls_goodness_of_fit_ref 1.018 _refine_ls_restrained_S_all 1.018 _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 V1 V 0.13315(8) 0.36141(10) 0.06143(6) 0.01565(14) Uani 1 1 d . . . V2 V 0.26005(8) -0.14587(9) 0.13344(6) 0.01597(14) Uani 1 1 d . . . V3 V 0.53028(8) 0.13370(9) 0.05984(7) 0.01775(15) Uani 1 1 d . . . O1 O 0.0116(4) 0.3787(6) 0.1823(3) 0.0309(7) Uani 1 1 d . . . O2 O 0.2757(5) -0.1627(6) 0.2904(3) 0.0322(7) Uani 1 1 d . . . O3 O 0.6206(4) 0.2155(5) 0.1972(4) 0.0321(7) Uani 1 1 d . . . O4 O -0.0016(3) 0.3519(5) -0.0830(3) 0.0223(5) Uani 1 1 d . . . O5 O 0.2687(3) 0.1394(5) 0.0800(3) 0.0222(6) Uani 1 1 d . . . O6 O 0.2699(4) 0.5803(4) 0.0580(3) 0.0237(7) Uani 1 1 d . . . O7 O 0.4950(3) -0.1499(4) 0.0674(3) 0.0206(5) Uani 1 1 d . . . N1 N 0.1648(6) 0.3095(8) 0.6888(4) 0.0424(12) Uani 1 1 d . . . H1 H 0.1209 0.3176 0.7644 0.051 Uiso 1 1 calc R . . C1 C 0.1500(8) 0.4640(10) 0.6089(7) 0.0527(16) Uani 1 1 d . . . H1A H 0.0948 0.5808 0.6350 0.063 Uiso 1 1 calc R . . C2 C 0.2161(9) 0.4537(11) 0.4861(7) 0.061(2) Uani 1 1 d . . . H2 H 0.2052 0.5609 0.4273 0.073 Uiso 1 1 calc R . . C3 C 0.2986(9) 0.2786(14) 0.4547(6) 0.067(2) Uani 1 1 d . . . H3 H 0.3470 0.2679 0.3734 0.080 Uiso 1 1 calc R . . C4 C 0.3112(8) 0.1215(12) 0.5384(7) 0.0607(17) Uani 1 1 d . . . H4 H 0.3645 0.0024 0.5144 0.073 Uiso 1 1 calc R . . C5 C 0.2458(8) 0.1396(11) 0.6569(6) 0.0529(14) Uani 1 1 d . . . H5 H 0.2568 0.0339 0.7169 0.063 Uiso 1 1 calc R . . 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 V1 0.0143(3) 0.0074(2) 0.0259(3) -0.0004(3) 0.0058(2) -0.0003(3) V2 0.0172(3) 0.0084(3) 0.0227(3) 0.0002(3) 0.0042(2) -0.0004(3) V3 0.0162(3) 0.0081(3) 0.0292(3) -0.0016(3) 0.0038(2) 0.0000(2) O1 0.0299(16) 0.0282(17) 0.0369(16) -0.0039(15) 0.0169(13) -0.0013(15) O2 0.0417(18) 0.0262(17) 0.0288(15) 0.0001(15) 0.0031(13) -0.0053(15) O3 0.0306(17) 0.0252(16) 0.0400(19) -0.0066(14) -0.0008(14) -0.0046(13) O4 0.0168(12) 0.0189(13) 0.0314(14) -0.0013(15) 0.0036(10) 0.0014(13) O5 0.0152(12) 0.0073(11) 0.0449(17) 0.0045(14) 0.0066(11) 0.0012(12) O6 0.0194(13) 0.0104(13) 0.0430(19) -0.0049(12) 0.0128(13) -0.0021(10) O7 0.0194(12) 0.0077(11) 0.0353(14) -0.0008(14) 0.0065(10) -0.0026(11) N1 0.035(2) 0.064(3) 0.030(2) -0.005(2) 0.0095(17) 0.000(2) C1 0.042(3) 0.041(3) 0.073(5) -0.009(3) -0.003(3) 0.006(3) C2 0.072(5) 0.051(4) 0.058(4) 0.023(3) -0.013(4) -0.014(4) C3 0.052(4) 0.119(7) 0.031(3) -0.009(4) 0.009(3) -0.024(4) C4 0.056(4) 0.057(4) 0.071(4) -0.027(4) 0.015(3) -0.001(3) C5 0.049(3) 0.045(3) 0.063(4) 0.014(3) -0.001(3) -0.005(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. SHELXL: Least-squares planes (x,y,z in crystal coordinates) and deviations from them (* indicates atom used to define plane) 6.3923 (0.0101) x + 2.3623 (0.0155) y + 3.2940 (0.0254) z = 4.0579 (0.0131) * -0.0045 (0.0039) N1 * 0.0027 (0.0041) C1 * -0.0035 (0.0047) C2 * 0.0063 (0.0050) C3 * -0.0079 (0.0046) C4 * 0.0071 (0.0043) C5 Rms deviation of fitted atoms = 0.0057 (0.0044) ; 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 V1 O1 1.591(3) . ? V1 O4 1.718(3) . ? V1 O6 1.787(3) . ? V1 O5 1.798(3) . ? V2 O2 1.593(3) . ? V2 O7 1.940(3) . ? V2 O4 1.973(3) 2_545 ? V2 O5 1.978(3) . ? V2 O6 1.981(3) 1_545 ? V2 V3 2.8984(9) . ? V2 V3 2.9964(9) 2_645 ? V3 O3 1.598(3) . ? V3 O7 1.909(3) . ? V3 O7 1.935(3) 2_655 ? V3 O5 1.996(3) . ? V3 O6 2.025(3) 2_645 ? V3 V2 2.9964(9) 2_655 ? O4 V2 1.973(3) 2 ? O6 V2 1.981(3) 1_565 ? O6 V3 2.025(3) 2_655 ? O7 V3 1.935(3) 2_645 ? N1 C1 1.309(8) . ? N1 C5 1.338(9) . ? N1 H1 0.8600 . ? C1 C2 1.380(10) . ? C1 H1A 0.9300 . ? C2 C3 1.371(10) . ? C2 H2 0.9300 . ? C3 C4 1.346(11) . ? C3 H3 0.9300 . ? C4 C5 1.340(9) . ? C4 H4 0.9300 . ? C5 H5 0.9300 . ? 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 V1 O4 108.88(16) . . ? O1 V1 O6 108.83(16) . . ? O4 V1 O6 108.46(15) . . ? O1 V1 O5 109.56(16) . . ? O4 V1 O5 110.60(15) . . ? O6 V1 O5 110.47(11) . . ? O2 V2 O7 110.27(15) . . ? O2 V2 O4 104.71(15) . 2_545 ? O7 V2 O4 144.81(12) . 2_545 ? O2 V2 O5 109.92(16) . . ? O7 V2 O5 82.41(11) . . ? O4 V2 O5 89.36(12) 2_545 . ? O2 V2 O6 108.65(17) . 1_545 ? O7 V2 O6 77.95(11) . 1_545 ? O4 V2 O6 87.63(13) 2_545 1_545 ? O5 V2 O6 140.78(12) . 1_545 ? O2 V2 V3 107.72(13) . . ? O7 V2 V3 40.75(9) . . ? O4 V2 V3 129.48(9) 2_545 . ? O5 V2 V3 43.42(7) . . ? O6 V2 V3 116.32(8) 1_545 . ? O2 V2 V3 128.23(14) . 2_645 ? O7 V2 V3 39.28(9) . 2_645 ? O4 V2 V3 112.67(9) 2_545 2_645 ? O5 V2 V3 105.10(9) . 2_645 ? O6 V2 V3 42.15(8) 1_545 2_645 ? V3 V2 V3 74.316(17) . 2_645 ? O3 V3 O7 110.68(15) . . ? O3 V3 O7 109.96(15) . 2_655 ? O7 V3 O7 139.18(7) . 2_655 ? O3 V3 O5 105.10(16) . . ? O7 V3 O5 82.71(12) . . ? O7 V3 O5 90.44(12) 2_655 . ? O3 V3 O6 106.85(16) . 2_645 ? O7 V3 O6 87.83(12) . 2_645 ? O7 V3 O6 77.02(12) 2_655 2_645 ? O5 V3 O6 147.99(15) . 2_645 ? O3 V3 V2 104.68(13) . . ? O7 V3 V2 41.55(8) . . ? O7 V3 V2 128.03(8) 2_655 . ? O5 V3 V2 42.93(9) . . ? O6 V3 V2 127.46(9) 2_645 . ? O3 V3 V2 101.20(13) . 2_655 ? O7 V3 V2 126.36(9) . 2_655 ? O7 V3 V2 39.41(8) 2_655 2_655 ? O5 V3 V2 129.20(9) . 2_655 ? O6 V3 V2 41.04(8) 2_645 2_655 ? V2 V3 V2 154.11(3) . 2_655 ? V1 O4 V2 136.58(16) . 2 ? V1 O5 V2 141.98(15) . . ? V1 O5 V3 124.15(16) . . ? V2 O5 V3 93.65(12) . . ? V1 O6 V2 134.79(16) . 1_565 ? V1 O6 V3 127.62(16) . 2_655 ? V2 O6 V3 96.81(12) 1_565 2_655 ? V3 O7 V3 135.80(15) . 2_645 ? V3 O7 V2 97.69(13) . . ? V3 O7 V2 101.31(13) 2_645 . ? C1 N1 C5 122.2(5) . . ? C1 N1 H1 118.9 . . ? C5 N1 H1 118.9 . . ? N1 C1 C2 120.1(6) . . ? N1 C1 H1A 119.9 . . ? C2 C1 H1A 119.9 . . ? C3 C2 C1 117.0(6) . . ? C3 C2 H2 121.5 . . ? C1 C2 H2 121.5 . . ? C4 C3 C2 121.7(6) . . ? C4 C3 H3 119.2 . . ? C2 C3 H3 119.2 . . ? C5 C4 C3 119.0(7) . . ? C5 C4 H4 120.5 . . ? C3 C4 H4 120.5 . . ? N1 C5 C4 120.0(6) . . ? N1 C5 H5 120.0 . . ? C4 C5 H5 120.0 . . ? 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 O2 V2 V3 O3 -4.0(2) . . . . ? O7 V2 V3 O3 -104.76(18) . . . . ? O4 V2 V3 O3 123.47(17) 2_545 . . . ? O5 V2 V3 O3 96.52(19) . . . . ? O6 V2 V3 O3 -126.19(18) 1_545 . . . ? V3 V2 V3 O3 -129.83(13) 2_645 . . . ? O2 V2 V3 O7 100.74(19) . . . . ? O4 V2 V3 O7 -131.77(17) 2_545 . . . ? O5 V2 V3 O7 -158.72(18) . . . . ? O6 V2 V3 O7 -21.43(16) 1_545 . . . ? V3 V2 V3 O7 -25.07(12) 2_645 . . . ? O2 V2 V3 O7 -134.78(18) . . . 2_655 ? O7 V2 V3 O7 124.47(12) . . . 2_655 ? O4 V2 V3 O7 -7.30(16) 2_545 . . 2_655 ? O5 V2 V3 O7 -34.25(17) . . . 2_655 ? O6 V2 V3 O7 103.04(16) 1_545 . . 2_655 ? V3 V2 V3 O7 99.41(11) 2_645 . . 2_655 ? O2 V2 V3 O5 -100.54(19) . . . . ? O7 V2 V3 O5 158.72(18) . . . . ? O4 V2 V3 O5 26.95(17) 2_545 . . . ? O6 V2 V3 O5 137.29(16) 1_545 . . . ? V3 V2 V3 O5 133.65(14) 2_645 . . . ? O2 V2 V3 O6 121.32(19) . . . 2_645 ? O7 V2 V3 O6 20.58(18) . . . 2_645 ? O4 V2 V3 O6 -111.20(17) 2_545 . . 2_645 ? O5 V2 V3 O6 -138.1(2) . . . 2_645 ? O6 V2 V3 O6 -0.9(2) 1_545 . . 2_645 ? V3 V2 V3 O6 -4.49(12) 2_645 . . 2_645 ? O2 V2 V3 V2 174.62(15) . . . 2_655 ? O7 V2 V3 V2 73.88(14) . . . 2_655 ? O4 V2 V3 V2 -57.89(14) 2_545 . . 2_655 ? O5 V2 V3 V2 -84.84(15) . . . 2_655 ? O6 V2 V3 V2 52.45(13) 1_545 . . 2_655 ? V3 V2 V3 V2 48.81(6) 2_645 . . 2_655 ? O1 V1 O4 V2 -0.8(3) . . . 2 ? O6 V1 O4 V2 -119.1(2) . . . 2 ? O5 V1 O4 V2 119.6(2) . . . 2 ? O1 V1 O5 V2 40.8(3) . . . . ? O4 V1 O5 V2 -79.2(3) . . . . ? O6 V1 O5 V2 160.7(3) . . . . ? O1 V1 O5 V3 -132.2(2) . . . . ? O4 V1 O5 V3 107.8(2) . . . . ? O6 V1 O5 V3 -12.3(2) . . . . ? O2 V2 O5 V1 -79.2(3) . . . . ? O7 V2 O5 V1 171.9(3) . . . . ? O4 V2 O5 V1 26.2(3) 2_545 . . . ? O6 V2 O5 V1 111.7(3) 1_545 . . . ? V3 V2 O5 V1 -174.2(4) . . . . ? V3 V2 O5 V1 139.6(3) 2_645 . . . ? O2 V2 O5 V3 95.04(17) . . . . ? O7 V2 O5 V3 -13.83(12) . . . . ? O4 V2 O5 V3 -159.52(13) 2_545 . . . ? O6 V2 O5 V3 -74.07(18) 1_545 . . . ? V3 V2 O5 V3 -46.18(12) 2_645 . . . ? O3 V3 O5 V1 80.2(2) . . . . ? O7 V3 O5 V1 -170.2(2) . . . . ? O7 V3 O5 V1 -30.6(2) 2_655 . . . ? O6 V3 O5 V1 -96.3(3) 2_645 . . . ? V2 V3 O5 V1 175.7(3) . . . . ? V2 V3 O5 V1 -38.4(3) 2_655 . . . ? O3 V3 O5 V2 -95.48(17) . . . . ? O7 V3 O5 V2 14.05(12) . . . . ? O7 V3 O5 V2 153.69(13) 2_655 . . . ? O6 V3 O5 V2 88.0(3) 2_645 . . . ? V2 V3 O5 V2 145.87(6) 2_655 . . . ? O1 V1 O6 V2 -19.5(3) . . . 1_565 ? O4 V1 O6 V2 98.8(3) . . . 1_565 ? O5 V1 O6 V2 -139.8(3) . . . 1_565 ? O1 V1 O6 V3 173.1(2) . . . 2_655 ? O4 V1 O6 V3 -68.6(2) . . . 2_655 ? O5 V1 O6 V3 52.8(2) . . . 2_655 ? O3 V3 O7 V3 -156.0(2) . . . 2_645 ? O7 V3 O7 V3 18.41(18) 2_655 . . 2_645 ? O5 V3 O7 V3 100.6(2) . . . 2_645 ? O6 V3 O7 V3 -48.8(2) 2_645 . . 2_645 ? V2 V3 O7 V3 115.0(2) . . . 2_645 ? V2 V3 O7 V3 -33.6(2) 2_655 . . 2_645 ? O3 V3 O7 V2 89.00(17) . . . . ? O7 V3 O7 V2 -96.59(11) 2_655 . . . ? O5 V3 O7 V2 -14.43(12) . . . . ? O6 V3 O7 V2 -163.79(14) 2_645 . . . ? V2 V3 O7 V2 -148.61(6) 2_655 . . . ? O2 V2 O7 V3 -93.92(18) . . . . ? O4 V2 O7 V3 92.5(2) 2_545 . . . ? O5 V2 O7 V3 14.58(12) . . . . ? O6 V2 O7 V3 160.43(15) 1_545 . . . ? V3 V2 O7 V3 139.89(18) 2_645 . . . ? O2 V2 O7 V3 126.19(17) . . . 2_645 ? O4 V2 O7 V3 -47.4(3) 2_545 . . 2_645 ? O5 V2 O7 V3 -125.31(15) . . . 2_645 ? O6 V2 O7 V3 20.55(13) 1_545 . . 2_645 ? V3 V2 O7 V3 -139.89(18) . . . 2_645 ? C5 N1 C1 C2 1.3(9) . . . . ? N1 C1 C2 C3 -1.1(10) . . . . ? C1 C2 C3 C4 1.5(11) . . . . ? C2 C3 C4 C5 -1.9(11) . . . . ? C1 N1 C5 C4 -1.7(9) . . . . ? C3 C4 C5 N1 2.0(10) . . . . ? 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 N1 H1 O4 0.86 1.878 2.732(5) 172.25 1_556 _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 30.03 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.849 _refine_diff_density_min -0.460 _refine_diff_density_rms 0.122