data_donowensite _audit_creation_method 'SHELXL-2016/6' _shelx_SHELXL_version_number '2016/6' _chemical_name_mineral 'donowensite' _chemical_compound_source 'Wilson Springs mine, AR' _chemical_formula_analytical 'Ca0.93 Fe1.92 Mn0.01 V4.06 P0.01 O17 H6' _chemical_formula_sum 'Ca Fe2 H6 O17 V4' _chemical_formula_weight 633.59 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Ca' 'Ca' 0.2262 0.3064 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Fe' 'Fe' 0.3463 0.8444 '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' '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' _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 1' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.3452(4) _cell_length_b 9.9291(4) _cell_length_c 10.0151(7) _cell_angle_alpha 94.455(7) _cell_angle_beta 98.476(7) _cell_angle_gamma 100.779(7) _cell_volume 705.52(7) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 11799 _cell_measurement_theta_min 3.1 _cell_measurement_theta_max 27.5 _exptl_crystal_description 'needle' _exptl_crystal_colour 'orange' _exptl_crystal_density_diffrn 2.982 _exptl_crystal_F_000 612 _exptl_crystal_size_max 0.430 _exptl_crystal_size_mid 0.020 _exptl_crystal_size_min 0.020 _exptl_absorpt_coefficient_mu 4.997 _shelx_estimated_absorpt_T_min 0.223 _shelx_estimated_absorpt_T_max 0.907 _exptl_absorpt_correction_type 'Multi-scan' _exptl_absorpt_correction_T_min 0.634 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details Higashi2001 _diffrn_measurement_device_type 'Rigaku R-axis RAPID II' _diffrn_ambient_temperature 293(2) _diffrn_radiation_probe 'x-ray' _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_reflns_number 16955 _diffrn_reflns_av_unetI/netI 0.0392 _diffrn_reflns_av_R_equivalents 0.0579 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 3.104 _diffrn_reflns_theta_max 27.470 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 0.996 _diffrn_measured_fraction_theta_full 0.996 _diffrn_reflns_Laue_measured_fraction_max 0.996 _diffrn_reflns_Laue_measured_fraction_full 0.996 _diffrn_reflns_point_group_measured_fraction_max 0.996 _diffrn_reflns_point_group_measured_fraction_full 0.996 _reflns_number_total 3213 _reflns_number_gt 2615 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _computing_structure_refinement 'SHELXL-2016/6 (Sheldrick, 2016)' _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0921P)^2^+5.1060P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_hydrogens . _refine_ls_hydrogen_treatment undef _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 3213 _refine_ls_number_parameters 217 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0668 _refine_ls_R_factor_gt 0.0561 _refine_ls_wR_factor_ref 0.1714 _refine_ls_wR_factor_gt 0.1617 _refine_ls_goodness_of_fit_ref 1.079 _refine_ls_restrained_S_all 1.079 _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_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Ca Ca 0.67710(18) 0.65850(13) 0.43307(12) 0.0194(3) Uani 1 1 d . . . . . Fe1 Fe 0.52282(11) 0.63729(8) 0.08924(8) 0.0097(2) Uani 1 1 d . . . . . Fe2 Fe 0.52312(11) 0.13442(8) 0.10125(8) 0.0102(2) Uani 1 1 d . . . . . V1 V 0.25217(13) 0.86735(10) 0.17089(10) 0.0111(2) Uani 1 1 d . . . . . V2 V 0.82419(13) 0.91550(9) 0.17197(10) 0.0109(2) Uani 1 1 d . . . . . V3 V 0.82446(13) 0.42083(9) 0.17435(9) 0.0102(2) Uani 1 1 d . . . . . V4 V 0.26681(13) 0.37812(10) 0.18110(9) 0.0103(2) Uani 1 1 d . . . . . O1 O 0.2373(7) 0.7854(5) 0.3038(5) 0.0241(10) Uani 1 1 d . . . . . O2 O 0.8986(7) 0.0216(5) 0.3069(5) 0.0289(11) Uani 1 1 d . . . . . O3 O 0.8784(6) 0.5330(5) 0.3071(4) 0.0207(9) Uani 1 1 d . . . . . O4 O 0.2586(6) 0.3050(4) 0.3193(4) 0.0190(9) Uani 1 1 d . . . . . O5 O 0.0210(6) 0.8833(5) 0.0993(4) 0.0188(9) Uani 1 1 d . . . . . O6 O 0.0364(6) 0.3967(5) 0.1153(4) 0.0177(9) Uani 1 1 d . . . . . O7 O 0.3963(6) 0.0274(4) 0.2262(4) 0.0155(8) Uani 1 1 d . . . . . O8 O 0.3551(5) 0.7724(4) 0.0557(4) 0.0119(8) Uani 1 1 d . . . . . O9 O 0.7029(6) 0.7661(4) 0.2247(4) 0.0136(8) Uani 1 1 d . . . . . O10 O 0.6701(5) 0.9903(4) 0.0600(4) 0.0109(8) Uani 1 1 d . . . . . O11 O 0.7016(6) 0.2751(4) 0.2280(4) 0.0153(8) Uani 1 1 d . . . . . O12 O 0.6739(5) 0.4924(4) 0.0541(4) 0.0111(8) Uani 1 1 d . . . . . O13 O 0.4220(6) 0.5354(4) 0.2315(4) 0.0144(8) Uani 1 1 d . . . . . O14 O 0.3573(5) 0.2728(4) 0.0662(4) 0.0118(8) Uani 1 1 d . . . . . OW1 O 0.3579(7) 0.5935(5) 0.5091(5) 0.0260(10) Uani 1 1 d . . . . . OW2 O 0.9998(6) 0.7577(5) 0.4987(5) 0.0330(13) Uani 1 1 d . . . . . OW3 O 0.6254(9) 0.8842(6) 0.4992(6) 0.0385(13) Uani 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 Ca 0.0221(6) 0.0196(6) 0.0155(6) 0.0014(5) 0.0047(5) 0.0005(5) Fe1 0.0093(4) 0.0080(4) 0.0118(4) 0.0001(3) 0.0017(3) 0.0019(3) Fe2 0.0096(4) 0.0083(4) 0.0131(4) 0.0012(3) 0.0024(3) 0.0027(3) V1 0.0087(5) 0.0108(5) 0.0146(5) 0.0011(3) 0.0044(3) 0.0022(3) V2 0.0079(5) 0.0095(5) 0.0146(5) 0.0013(3) 0.0004(3) 0.0009(3) V3 0.0079(5) 0.0101(5) 0.0126(5) 0.0009(3) 0.0012(3) 0.0022(3) V4 0.0087(5) 0.0111(5) 0.0117(5) 0.0011(3) 0.0032(3) 0.0024(3) O1 0.029(3) 0.020(2) 0.026(2) 0.0097(19) 0.011(2) 0.0053(19) O2 0.035(3) 0.022(2) 0.023(2) -0.0053(19) -0.003(2) -0.003(2) O3 0.023(2) 0.018(2) 0.019(2) -0.0056(17) 0.0014(17) 0.0023(17) O4 0.020(2) 0.020(2) 0.018(2) 0.0086(17) 0.0058(17) 0.0009(17) O5 0.014(2) 0.027(2) 0.020(2) 0.0042(18) 0.0042(17) 0.0145(18) O6 0.012(2) 0.026(2) 0.018(2) -0.0019(17) 0.0009(16) 0.0119(17) O7 0.018(2) 0.0114(19) 0.016(2) -0.0005(15) 0.0046(16) 0.0007(16) O8 0.0101(18) 0.0102(18) 0.017(2) -0.0002(15) 0.0057(15) 0.0027(14) O9 0.016(2) 0.0132(19) 0.0101(18) 0.0013(15) 0.0020(15) -0.0004(16) O10 0.0083(18) 0.0109(18) 0.0144(19) 0.0036(14) 0.0014(14) 0.0035(14) O11 0.018(2) 0.013(2) 0.013(2) 0.0026(15) -0.0003(15) 0.0011(16) O12 0.0079(18) 0.0100(18) 0.0150(19) 0.0021(14) 0.0003(14) 0.0021(14) O13 0.018(2) 0.0132(19) 0.0130(19) 0.0028(15) 0.0039(15) 0.0029(16) O14 0.0119(19) 0.0100(18) 0.0150(19) 0.0006(15) 0.0048(15) 0.0043(15) OW1 0.029(3) 0.027(2) 0.025(2) 0.0072(19) 0.011(2) 0.006(2) OW2 0.032(3) 0.034(3) 0.028(3) -0.013(2) 0.011(2) -0.006(2) OW3 0.056(4) 0.033(3) 0.028(3) 0.000(2) 0.004(2) 0.017(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 Ca OW2 2.364(5) . ? Ca OW3 2.402(6) . ? Ca O9 2.433(4) . ? Ca O4 2.441(4) 2_666 ? Ca O3 2.515(5) . ? Ca OW1 2.555(5) . ? Ca OW1 2.587(5) 2_666 ? Ca O13 2.594(4) . ? Ca Fe1 3.4400(15) . ? Ca V3 3.7797(16) . ? Ca Ca 4.134(2) 2_666 ? Fe1 O9 1.948(4) . ? Fe1 O13 1.963(4) . ? Fe1 O8 1.999(4) . ? Fe1 O12 2.015(4) . ? Fe1 O12 2.052(4) 2_665 ? Fe1 O14 2.079(4) 2_665 ? Fe2 O7 1.935(4) . ? Fe2 O11 1.957(4) . ? Fe2 O10 2.000(4) 1_545 ? Fe2 O14 2.018(4) . ? Fe2 O8 2.112(4) 2_665 ? Fe2 O10 2.125(4) 2_665 ? V1 O1 1.619(4) . ? V1 O7 1.736(4) 1_565 ? V1 O8 1.773(4) . ? V1 O5 1.784(4) . ? V2 O2 1.606(5) 1_565 ? V2 O9 1.743(4) . ? V2 O10 1.777(4) . ? V2 O5 1.780(4) 1_655 ? V3 O3 1.617(4) . ? V3 O11 1.724(4) . ? V3 O12 1.793(4) . ? V3 O6 1.794(4) 1_655 ? V4 O4 1.615(4) . ? V4 O13 1.742(4) . ? V4 O6 1.772(4) . ? V4 O14 1.777(4) . ? 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 OW2 Ca OW3 85.4(2) . . ? OW2 Ca O9 85.63(16) . . ? OW3 Ca O9 79.04(17) . . ? OW2 Ca O4 72.47(15) . 2_666 ? OW3 Ca O4 72.69(17) . 2_666 ? O9 Ca O4 145.22(15) . 2_666 ? OW2 Ca O3 68.43(15) . . ? OW3 Ca O3 143.10(19) . . ? O9 Ca O3 73.67(15) . . ? O4 Ca O3 119.77(16) 2_666 . ? OW2 Ca OW1 146.55(16) . . ? OW3 Ca OW1 80.07(19) . . ? O9 Ca OW1 120.34(16) . . ? O4 Ca OW1 74.48(16) 2_666 . ? O3 Ca OW1 135.47(16) . . ? OW2 Ca OW1 105.48(18) . 2_666 ? OW3 Ca OW1 145.4(2) . 2_666 ? O9 Ca OW1 133.61(15) . 2_666 ? O4 Ca OW1 79.34(16) 2_666 2_666 ? O3 Ca OW1 69.52(15) . 2_666 ? OW1 Ca OW1 72.96(18) . 2_666 ? OW2 Ca O13 144.34(15) . . ? OW3 Ca O13 110.49(18) . . ? O9 Ca O13 67.44(13) . . ? O4 Ca O13 141.93(15) 2_666 . ? O3 Ca O13 81.39(14) . . ? OW1 Ca O13 69.07(15) . . ? OW1 Ca O13 79.88(15) 2_666 . ? OW2 Ca Fe1 113.68(12) . . ? OW3 Ca Fe1 99.29(14) . . ? O9 Ca Fe1 33.50(10) . . ? O4 Ca Fe1 169.88(12) 2_666 . ? O3 Ca Fe1 70.35(11) . . ? OW1 Ca Fe1 98.37(12) . . ? OW1 Ca Fe1 105.72(12) 2_666 . ? O13 Ca Fe1 34.50(9) . . ? OW2 Ca V3 86.77(11) . . ? OW3 Ca V3 148.21(15) . . ? O9 Ca V3 69.67(10) . . ? O4 Ca V3 133.26(12) 2_666 . ? O3 Ca V3 18.81(10) . . ? OW1 Ca V3 120.47(12) . . ? OW1 Ca V3 66.30(11) 2_666 . ? O13 Ca V3 62.69(10) . . ? Fe1 Ca V3 56.49(3) . . ? OW2 Ca Ca 133.05(14) . 2_666 ? OW3 Ca Ca 114.09(16) . 2_666 ? O9 Ca Ca 138.05(11) . 2_666 ? O4 Ca Ca 73.67(11) 2_666 2_666 ? O3 Ca Ca 102.80(11) . 2_666 ? OW1 Ca Ca 36.74(11) . 2_666 ? OW1 Ca Ca 36.22(11) 2_666 2_666 ? O13 Ca Ca 70.69(10) . 2_666 ? Fe1 Ca Ca 105.04(5) . 2_666 ? V3 Ca Ca 93.55(4) . 2_666 ? O9 Fe1 O13 91.16(17) . . ? O9 Fe1 O8 92.97(17) . . ? O13 Fe1 O8 103.58(17) . . ? O9 Fe1 O12 100.68(17) . . ? O13 Fe1 O12 89.97(17) . . ? O8 Fe1 O12 160.59(17) . . ? O9 Fe1 O12 177.60(16) . 2_665 ? O13 Fe1 O12 89.25(17) . 2_665 ? O8 Fe1 O12 84.63(16) . 2_665 ? O12 Fe1 O12 81.68(16) . 2_665 ? O9 Fe1 O14 90.71(16) . 2_665 ? O13 Fe1 O14 173.83(16) . 2_665 ? O8 Fe1 O14 82.19(16) . 2_665 ? O12 Fe1 O14 83.91(15) . 2_665 ? O12 Fe1 O14 89.13(16) 2_665 2_665 ? O9 Fe1 Ca 43.57(12) . . ? O13 Fe1 Ca 48.43(12) . . ? O8 Fe1 Ca 108.45(12) . . ? O12 Fe1 Ca 90.92(12) . . ? O12 Fe1 Ca 137.20(11) 2_665 . ? O14 Fe1 Ca 132.15(12) 2_665 . ? O7 Fe2 O11 100.83(17) . . ? O7 Fe2 O10 92.76(17) . 1_545 ? O11 Fe2 O10 104.42(17) . 1_545 ? O7 Fe2 O14 101.14(17) . . ? O11 Fe2 O14 89.18(17) . . ? O10 Fe2 O14 158.44(17) 1_545 . ? O7 Fe2 O8 171.98(16) . 2_665 ? O11 Fe2 O8 86.90(17) . 2_665 ? O10 Fe2 O8 83.15(15) 1_545 2_665 ? O14 Fe2 O8 80.94(16) . 2_665 ? O7 Fe2 O10 87.96(16) . 2_665 ? O11 Fe2 O10 169.77(16) . 2_665 ? O10 Fe2 O10 80.13(16) 1_545 2_665 ? O14 Fe2 O10 83.95(15) . 2_665 ? O8 Fe2 O10 84.56(15) 2_665 2_665 ? O1 V1 O7 106.7(2) . 1_565 ? O1 V1 O8 108.2(2) . . ? O7 V1 O8 110.40(19) 1_565 . ? O1 V1 O5 108.0(2) . . ? O7 V1 O5 111.6(2) 1_565 . ? O8 V1 O5 111.79(19) . . ? O2 V2 O9 105.8(2) 1_565 . ? O2 V2 O10 107.8(2) 1_565 . ? O9 V2 O10 110.69(19) . . ? O2 V2 O5 108.8(2) 1_565 1_655 ? O9 V2 O5 111.3(2) . 1_655 ? O10 V2 O5 112.18(19) . 1_655 ? O3 V3 O11 104.8(2) . . ? O3 V3 O12 105.1(2) . . ? O11 V3 O12 110.74(19) . . ? O3 V3 O6 108.9(2) . 1_655 ? O11 V3 O6 113.9(2) . 1_655 ? O12 V3 O6 112.80(19) . 1_655 ? O3 V3 Ca 30.09(17) . . ? O11 V3 Ca 92.78(15) . . ? O12 V3 Ca 84.13(13) . . ? O6 V3 Ca 138.13(15) 1_655 . ? O4 V4 O13 104.4(2) . . ? O4 V4 O6 108.1(2) . . ? O13 V4 O6 113.1(2) . . ? O4 V4 O14 108.1(2) . . ? O13 V4 O14 110.87(19) . . ? O6 V4 O14 111.88(19) . . ? V3 O3 Ca 131.1(2) . . ? V4 O4 Ca 145.2(3) . 2_666 ? V2 O5 V1 133.0(3) 1_455 . ? V4 O6 V3 139.6(3) . 1_455 ? V1 O7 Fe2 120.9(2) 1_545 . ? V1 O8 Fe1 130.3(2) . . ? V1 O8 Fe2 121.2(2) . 2_665 ? Fe1 O8 Fe2 98.19(16) . 2_665 ? V2 O9 Fe1 118.1(2) . . ? V2 O9 Ca 139.0(2) . . ? Fe1 O9 Ca 102.93(17) . . ? V2 O10 Fe2 129.6(2) . 1_565 ? V2 O10 Fe2 120.4(2) . 2_665 ? Fe2 O10 Fe2 99.87(16) 1_565 2_665 ? V3 O11 Fe2 121.9(2) . . ? V3 O12 Fe1 128.4(2) . . ? V3 O12 Fe1 119.4(2) . 2_665 ? Fe1 O12 Fe1 98.32(16) . 2_665 ? V4 O13 Fe1 117.7(2) . . ? V4 O13 Ca 140.4(2) . . ? Fe1 O13 Ca 97.07(16) . . ? V4 O14 Fe2 130.5(2) . . ? V4 O14 Fe1 118.5(2) . 2_665 ? Fe2 O14 Fe1 98.68(16) . 2_665 ? Ca OW1 Ca 107.04(18) . 2_666 ? _refine_diff_density_max 2.436 _refine_diff_density_min -0.820 _refine_diff_density_rms 0.271 _shelx_res_file ; TITL JS-9-2019-02 js-9-2019-02.res created by SHELXL-2016/6 at 21:58:52 on 06-Jul-2020 CELL 0.71075 7.34519 9.92915 10.01510 94.45470 98.47550 100.77900 ZERR 1 0.00037 0.00044 0.00071 0.00670 0.00690 0.00710 LATT 1 SFAC CA FE H O V UNIT 2 4 12 34 8 L.S. 10 omit -4 4 2 omit -3 -2 2 omit 3 -6 7 omit -5 -4 3 omit -3 -3 2 omit -4 12 3 FMAP 2 PLAN 20 ACTA SIZE 0.430 0.020 0.020 WGHT 0.092100 5.106000 FVAR 0.36542 CA 1 0.677101 0.658495 0.433072 11.00000 0.02207 0.01959 = 0.01549 0.00138 0.00469 0.00051 FE1 2 0.522823 0.637294 0.089244 11.00000 0.00930 0.00799 = 0.01182 0.00011 0.00171 0.00191 FE2 2 0.523123 0.134423 0.101254 11.00000 0.00964 0.00832 = 0.01311 0.00117 0.00244 0.00265 V1 5 0.252166 0.867351 0.170894 11.00000 0.00868 0.01079 = 0.01460 0.00109 0.00441 0.00219 V2 5 0.824192 0.915499 0.171972 11.00000 0.00790 0.00953 = 0.01460 0.00135 0.00045 0.00089 V3 5 0.824462 0.420828 0.174354 11.00000 0.00786 0.01008 = 0.01257 0.00092 0.00124 0.00217 V4 5 0.266811 0.378123 0.181100 11.00000 0.00867 0.01106 = 0.01166 0.00105 0.00325 0.00243 O1 4 0.237333 0.785390 0.303759 11.00000 0.02884 0.02050 = 0.02629 0.00973 0.01139 0.00527 O2 4 0.898553 0.021580 0.306872 11.00000 0.03452 0.02175 = 0.02322 -0.00534 -0.00301 -0.00316 O3 4 0.878374 0.532960 0.307142 11.00000 0.02251 0.01802 = 0.01912 -0.00559 0.00143 0.00230 O4 4 0.258565 0.305037 0.319283 11.00000 0.02001 0.01975 = 0.01799 0.00858 0.00582 0.00088 O5 4 0.021000 0.883272 0.099282 11.00000 0.01413 0.02687 = 0.02029 0.00423 0.00424 0.01451 O6 4 0.036395 0.396698 0.115350 11.00000 0.01154 0.02580 = 0.01794 -0.00187 0.00089 0.01191 O7 4 0.396323 0.027361 0.226194 11.00000 0.01805 0.01139 = 0.01629 -0.00051 0.00455 0.00066 O8 4 0.355066 0.772413 0.055743 11.00000 0.01012 0.01015 = 0.01660 -0.00017 0.00569 0.00272 O9 4 0.702869 0.766122 0.224745 11.00000 0.01601 0.01322 = 0.01009 0.00132 0.00196 -0.00044 O10 4 0.670128 0.990319 0.060025 11.00000 0.00832 0.01094 = 0.01439 0.00365 0.00143 0.00350 O11 4 0.701584 0.275100 0.228033 11.00000 0.01806 0.01301 = 0.01318 0.00262 -0.00035 0.00108 O12 4 0.673871 0.492391 0.054062 11.00000 0.00795 0.01004 = 0.01499 0.00211 0.00032 0.00213 O13 4 0.421980 0.535450 0.231455 11.00000 0.01768 0.01320 = 0.01300 0.00278 0.00388 0.00286 O14 4 0.357263 0.272845 0.066212 11.00000 0.01194 0.01002 = 0.01502 0.00064 0.00481 0.00434 OW1 4 0.357902 0.593507 0.509053 11.00000 0.02876 0.02706 = 0.02493 0.00715 0.01120 0.00585 OW2 4 0.999767 0.757728 0.498656 11.00000 0.03190 0.03367 = 0.02772 -0.01262 0.01076 -0.00599 OW3 4 0.625357 0.884223 0.499189 11.00000 0.05606 0.03319 = 0.02788 0.00026 0.00403 0.01667 HKLF 4 REM JS-9-2019-02 REM R1 = 0.0561 for 2615 Fo > 4sig(Fo) and 0.0668 for all 3213 data REM 217 parameters refined using 0 restraints END WGHT 0.0921 5.1059 REM Highest difference peak 2.436, deepest hole -0.820, 1-sigma level 0.271 Q1 1 0.3645 0.1996 0.1794 11.00000 0.05 2.44 Q2 1 0.8025 0.6564 0.1708 11.00000 0.05 2.38 Q3 1 0.8015 0.1588 0.1741 11.00000 0.05 2.37 Q4 1 0.3576 0.6928 0.1776 11.00000 0.05 2.25 Q5 1 0.0613 0.4112 0.0899 11.00000 0.05 2.07 Q6 1 0.0667 0.9149 0.0947 11.00000 0.05 2.01 Q7 1 -0.0205 0.3510 0.0962 11.00000 0.05 1.95 Q8 1 0.7242 0.5947 0.1749 11.00000 0.05 1.84 Q9 1 0.5254 0.6882 0.4346 11.00000 0.05 1.81 Q10 1 0.7022 1.0828 0.1674 11.00000 0.05 1.67 Q11 1 0.4720 0.8092 0.5670 11.00000 0.05 1.61 Q12 1 0.2722 0.1385 0.1780 11.00000 0.05 1.57 Q13 1 1.0676 0.4608 0.4330 11.00000 0.05 1.38 Q14 1 1.0630 -0.0290 0.4340 11.00000 0.05 1.37 Q15 1 0.3540 -0.0579 0.1759 11.00000 0.05 1.34 Q16 1 0.3503 0.4450 0.1724 11.00000 0.05 1.12 Q17 1 0.5965 0.6940 0.0963 11.00000 0.05 1.10 Q18 1 0.9158 0.4836 0.1670 11.00000 0.05 1.07 Q19 1 0.2080 0.7651 0.0600 11.00000 0.05 0.98 Q20 1 1.1140 0.7382 0.4929 11.00000 0.05 0.96 ; _shelx_res_checksum 3440 _shelx_hkl_file ; 0 1 1 123.39 4.57 0 1 1 115.80 3.42 0 1 1 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