data_mikehowardite _audit_creation_method 'SHELXL-2016/6' _shelx_SHELXL_version_number '2016/6' _chemical_name_mineral 'mikehowardite' _chemical_compound_source 'Wilson Springs mine, AR' _chemical_formula_analytical 'K0.11 Ca0.02 Fe3.78 Mn0.03 V3.67 P0.33 O18.87 H6.18' _chemical_formula_sum 'Fe4 H0 K0.28 O18.72 P0.36 V3.64' _chemical_formula_weight 730.44 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source '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' 'P' 'P' 0.1023 0.0942 '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' 'K' 'K' 0.2009 0.2494 '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 6.6546(17) _cell_length_b 6.6689(14) _cell_length_c 9.003(2) _cell_angle_alpha 76.515(5) _cell_angle_beta 84.400(6) _cell_angle_gamma 75.058(5) _cell_volume 375.11(15) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2718 _cell_measurement_theta_min 3.2 _cell_measurement_theta_max 25.0 _exptl_crystal_description 'chunk' _exptl_crystal_colour 'brown' _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 3.234 _exptl_crystal_F_000 348 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.050 _exptl_crystal_size_mid 0.040 _exptl_crystal_size_min 0.020 _exptl_absorpt_coefficient_mu 6.136 _shelx_estimated_absorpt_T_min 0.749 _shelx_estimated_absorpt_T_max 0.887 _exptl_absorpt_correction_type 'Multi-scan' _exptl_absorpt_correction_T_min 0.340 _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 5324 _diffrn_reflns_av_unetI/netI 0.0669 _diffrn_reflns_av_R_equivalents 0.0860 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 3.171 _diffrn_reflns_theta_max 25.009 _diffrn_reflns_theta_full 25.009 _diffrn_measured_fraction_theta_max 0.997 _diffrn_measured_fraction_theta_full 0.997 _diffrn_reflns_Laue_measured_fraction_max 0.997 _diffrn_reflns_Laue_measured_fraction_full 0.997 _diffrn_reflns_point_group_measured_fraction_max 0.997 _diffrn_reflns_point_group_measured_fraction_full 0.997 _reflns_number_total 1316 _reflns_number_gt 1098 _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^)+(0.1146P)^2^+1.0319P] 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 1316 _refine_ls_number_parameters 130 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0778 _refine_ls_R_factor_gt 0.0678 _refine_ls_wR_factor_ref 0.1958 _refine_ls_wR_factor_gt 0.1862 _refine_ls_goodness_of_fit_ref 1.144 _refine_ls_restrained_S_all 1.144 _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 Fe1 Fe 0.2042(2) 0.3275(2) 0.47492(13) 0.0280(5) Uani 1 1 d . . . . . Fe2 Fe 0.1406(2) 0.1461(2) 0.19827(13) 0.0311(5) Uani 1 1 d . . . . . V1 V 0.7501(3) 0.2068(3) 0.44738(16) 0.0279(6) Uani 0.927(19) 1 d . . P . . P1 P 0.7501(3) 0.2068(3) 0.44738(16) 0.0279(6) Uani 0.073(19) 1 d . . P . . V2 V 0.0012(3) 0.3050(3) 0.81624(17) 0.0297(6) Uani 0.895(19) 1 d . . P . . P2 P 0.0012(3) 0.3050(3) 0.81624(17) 0.0297(6) Uani 0.105(19) 1 d . . P . . O1 O 0.4973(10) 0.3137(11) 0.4397(7) 0.0339(15) Uani 1 1 d . . . . . O2 O 0.8396(11) 0.1920(10) 0.2697(7) 0.0342(15) Uani 1 1 d . . . . . O3 O 0.8766(9) 0.3666(10) 0.5112(6) 0.0277(14) Uani 1 1 d . . . . . O4 O 0.7874(10) -0.0427(10) 0.5723(7) 0.0316(15) Uani 1 1 d . . . . . O5 O 0.0907(11) 0.2828(11) 0.9860(7) 0.0360(16) Uani 1 1 d . . . . . O6 O -0.1519(11) 0.1345(10) 0.8327(7) 0.0348(16) Uani 1 1 d . . . . . O7 O 0.2152(11) 0.2393(11) 0.6989(7) 0.0355(15) Uani 1 1 d . . . . . O8 O -0.1428(10) 0.5708(9) 0.7514(6) 0.0272(14) Uani 1 1 d . . . . . OW1 O 0.4634(12) 0.0900(13) 0.1412(8) 0.0457(18) Uani 1 1 d . . . . . K K 0.536(3) 0.498(5) 0.051(4) 0.143(16) Uani 0.14(2) 1 d . . P . . OW2 O 0.536(3) 0.498(5) 0.051(4) 0.143(16) Uani 0.36(2) 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 Fe1 0.0292(9) 0.0385(9) 0.0193(8) -0.0107(5) -0.0013(5) -0.0090(6) Fe2 0.0350(9) 0.0411(9) 0.0204(8) -0.0114(6) -0.0018(6) -0.0106(6) V1 0.0284(10) 0.0381(11) 0.0203(9) -0.0096(7) -0.0028(6) -0.0101(7) P1 0.0284(10) 0.0381(11) 0.0203(9) -0.0096(7) -0.0028(6) -0.0101(7) V2 0.0338(11) 0.0390(11) 0.0193(9) -0.0101(7) -0.0018(7) -0.0108(8) P2 0.0338(11) 0.0390(11) 0.0193(9) -0.0101(7) -0.0018(7) -0.0108(8) O1 0.030(4) 0.046(4) 0.029(3) -0.015(3) 0.004(3) -0.012(3) O2 0.034(4) 0.045(4) 0.027(3) -0.010(3) 0.000(3) -0.014(3) O3 0.025(3) 0.036(4) 0.021(3) -0.008(2) 0.002(2) -0.005(3) O4 0.036(4) 0.041(4) 0.020(3) -0.009(3) 0.000(3) -0.011(3) O5 0.047(4) 0.038(4) 0.024(3) -0.012(3) -0.004(3) -0.008(3) O6 0.042(4) 0.033(4) 0.029(3) -0.005(3) 0.001(3) -0.011(3) O7 0.043(4) 0.045(4) 0.023(3) -0.013(3) 0.002(3) -0.014(3) O8 0.040(4) 0.029(3) 0.014(3) -0.007(2) -0.002(2) -0.010(3) OW1 0.035(4) 0.069(5) 0.033(4) -0.009(3) -0.004(3) -0.014(4) K 0.047(15) 0.121(15) 0.22(4) 0.05(2) 0.005(12) -0.023(12) OW2 0.047(15) 0.121(15) 0.22(4) 0.05(2) 0.005(12) -0.023(12) _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 Fe1 O1 1.927(7) . ? Fe1 O7 1.967(6) . ? Fe1 O3 2.001(6) 2_666 ? Fe1 O4 2.027(6) 2_656 ? Fe1 O8 2.038(5) 2_566 ? Fe1 O3 2.129(6) 1_455 ? Fe2 O5 1.936(6) 1_554 ? Fe2 O6 1.937(7) 2_556 ? Fe2 O2 2.011(7) 1_455 ? Fe2 O8 2.045(6) 2_566 ? Fe2 O4 2.081(6) 2_656 ? Fe2 OW1 2.116(8) . ? Fe2 K 3.81(3) 2_665 ? Fe2 K 3.90(3) . ? V1 O1 1.651(7) . ? V1 O2 1.668(6) . ? V1 O3 1.737(6) . ? V1 O4 1.751(7) . ? V1 K 3.85(2) . ? V2 O5 1.655(6) . ? V2 O6 1.686(7) . ? V2 O7 1.714(7) . ? V2 O8 1.776(6) . ? V2 K 3.66(3) 2_566 ? V2 K 3.70(3) 1_456 ? V2 K 4.02(3) 2_666 ? O2 K 2.981(19) . ? O2 OW1 3.143(10) . ? O5 K 3.15(3) 2_666 ? O6 K 3.33(3) 2_566 ? O8 K 3.09(3) 2_566 ? O8 K 3.30(3) 1_456 ? OW1 K 2.80(3) . ? OW1 K 2.89(3) 2_665 ? K K 1.07(6) 2_665 ? 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 Fe1 O7 95.4(3) . . ? O1 Fe1 O3 95.2(3) . 2_666 ? O7 Fe1 O3 90.4(3) . 2_666 ? O1 Fe1 O4 96.9(3) . 2_656 ? O7 Fe1 O4 98.7(3) . 2_656 ? O3 Fe1 O4 164.0(3) 2_666 2_656 ? O1 Fe1 O8 93.6(3) . 2_566 ? O7 Fe1 O8 170.9(3) . 2_566 ? O3 Fe1 O8 87.3(2) 2_666 2_566 ? O4 Fe1 O8 81.6(2) 2_656 2_566 ? O1 Fe1 O3 175.9(3) . 1_455 ? O7 Fe1 O3 85.5(3) . 1_455 ? O3 Fe1 O3 80.8(3) 2_666 1_455 ? O4 Fe1 O3 86.9(3) 2_656 1_455 ? O8 Fe1 O3 85.5(2) 2_566 1_455 ? O5 Fe2 O6 93.8(3) 1_554 2_556 ? O5 Fe2 O2 96.3(3) 1_554 1_455 ? O6 Fe2 O2 92.5(3) 2_556 1_455 ? O5 Fe2 O8 91.0(3) 1_554 2_566 ? O6 Fe2 O8 174.8(3) 2_556 2_566 ? O2 Fe2 O8 88.7(3) 1_455 2_566 ? O5 Fe2 O4 170.5(3) 1_554 2_656 ? O6 Fe2 O4 95.0(3) 2_556 2_656 ? O2 Fe2 O4 87.0(3) 1_455 2_656 ? O8 Fe2 O4 80.1(2) 2_566 2_656 ? O5 Fe2 OW1 88.1(3) 1_554 . ? O6 Fe2 OW1 87.9(3) 2_556 . ? O2 Fe2 OW1 175.6(2) 1_455 . ? O8 Fe2 OW1 90.5(3) 2_566 . ? O4 Fe2 OW1 88.6(3) 2_656 . ? O5 Fe2 K 55.5(4) 1_554 2_665 ? O6 Fe2 K 121.8(6) 2_556 2_665 ? O2 Fe2 K 133.9(4) 1_455 2_665 ? O8 Fe2 K 59.9(6) 2_566 2_665 ? O4 Fe2 K 116.2(4) 2_656 2_665 ? OW1 Fe2 K 48.6(4) . 2_665 ? O5 Fe2 K 71.2(4) 1_554 . ? O6 Fe2 K 128.5(6) 2_556 . ? O2 Fe2 K 136.9(5) 1_455 . ? O8 Fe2 K 51.8(6) 2_566 . ? O4 Fe2 K 100.3(4) 2_656 . ? OW1 Fe2 K 44.2(5) . . ? K Fe2 K 15.9(8) 2_665 . ? O1 V1 O2 107.2(3) . . ? O1 V1 O3 111.0(3) . . ? O2 V1 O3 107.9(3) . . ? O1 V1 O4 107.9(3) . . ? O2 V1 O4 112.7(3) . . ? O3 V1 O4 110.2(3) . . ? O1 V1 K 62.9(5) . . ? O2 V1 K 47.2(6) . . ? O3 V1 K 108.8(5) . . ? O4 V1 K 140.5(6) . . ? O5 V2 O6 108.9(3) . . ? O5 V2 O7 106.2(3) . . ? O6 V2 O7 110.7(3) . . ? O5 V2 O8 108.7(3) . . ? O6 V2 O8 110.5(3) . . ? O7 V2 O8 111.7(3) . . ? O5 V2 K 91.9(5) . 2_566 ? O6 V2 K 65.3(6) . 2_566 ? O7 V2 K 161.5(5) . 2_566 ? O8 V2 K 57.3(5) . 2_566 ? O5 V2 K 75.2(4) . 1_456 ? O6 V2 K 73.1(5) . 1_456 ? O7 V2 K 174.8(5) . 1_456 ? O8 V2 K 63.2(4) . 1_456 ? K V2 K 16.7(9) 2_566 1_456 ? O5 V2 K 47.5(5) . 2_666 ? O6 V2 K 153.2(4) . 2_666 ? O7 V2 K 72.3(6) . 2_666 ? O8 V2 K 91.6(4) . 2_666 ? K V2 K 120.0(10) 2_566 2_666 ? K V2 K 105.9(4) 1_456 2_666 ? V1 O1 Fe1 157.5(4) . . ? V1 O2 Fe2 125.2(4) . 1_655 ? V1 O2 K 108.6(8) . . ? Fe2 O2 K 116.0(6) 1_655 . ? V1 O2 OW1 100.9(3) . . ? Fe2 O2 OW1 130.5(3) 1_655 . ? K O2 OW1 54.4(6) . . ? V1 O3 Fe1 133.0(3) . 2_666 ? V1 O3 Fe1 120.7(3) . 1_655 ? Fe1 O3 Fe1 99.2(3) 2_666 1_655 ? V1 O4 Fe1 128.6(3) . 2_656 ? V1 O4 Fe2 132.5(3) . 2_656 ? Fe1 O4 Fe2 98.7(3) 2_656 2_656 ? V2 O5 Fe2 153.6(4) . 1_556 ? V2 O5 K 109.8(6) . 2_666 ? Fe2 O5 K 94.1(5) 1_556 2_666 ? V2 O6 Fe2 140.4(4) . 2_556 ? V2 O6 K 87.3(5) . 2_566 ? Fe2 O6 K 132.2(5) 2_556 2_566 ? V2 O7 Fe1 121.9(4) . . ? V2 O8 Fe1 118.2(3) . 2_566 ? V2 O8 Fe2 133.4(3) . 2_566 ? Fe1 O8 Fe2 99.6(3) 2_566 2_566 ? V2 O8 K 93.7(5) . 2_566 ? Fe1 O8 K 111.7(5) 2_566 2_566 ? Fe2 O8 K 96.8(7) 2_566 2_566 ? V2 O8 K 88.1(5) . 1_456 ? Fe1 O8 K 129.8(4) 2_566 1_456 ? Fe2 O8 K 87.7(6) 2_566 1_456 ? K O8 K 18.9(9) 2_566 1_456 ? Fe2 OW1 K 104.1(6) . . ? Fe2 OW1 O7 126.3(3) . 2_656 ? K OW1 O7 117.1(4) . 2_656 ? Fe2 OW1 K 98.1(5) . 2_665 ? K OW1 K 21.6(12) . 2_665 ? O7 OW1 K 132.3(5) 2_656 2_665 ? Fe2 OW1 O2 133.7(3) . . ? K OW1 O2 59.9(4) . . ? O7 OW1 O2 58.4(2) 2_656 . ? K OW1 O2 79.2(5) 2_665 . ? K K OW1 84(3) 2_665 . ? K K OW1 74(3) 2_665 2_665 ? OW1 K OW1 158.4(12) . 2_665 ? K K O2 139(4) 2_665 . ? OW1 K O2 65.8(5) . . ? OW1 K O2 132.5(8) 2_665 . ? K K O8 92(3) 2_665 2_566 ? OW1 K O8 60.0(5) . 2_566 ? OW1 K O8 119.9(9) 2_665 2_566 ? O2 K O8 95.9(8) . 2_566 ? K K O5 116(3) 2_665 2_666 ? OW1 K O5 139.1(8) . 2_666 ? OW1 K O5 55.4(5) 2_665 2_666 ? O2 K O5 77.2(5) . 2_666 ? O8 K O5 144.2(14) 2_566 2_666 ? K K O8 69(3) 2_665 1_654 ? OW1 K O8 115.6(13) . 1_654 ? OW1 K O8 56.5(5) 2_665 1_654 ? O2 K O8 98.5(7) . 1_654 ? O8 K O8 161.1(9) 2_566 1_654 ? O5 K O8 52.2(4) 2_666 1_654 ? K K O6 96(3) 2_665 2_566 ? OW1 K O6 112.5(9) . 2_566 ? OW1 K O6 70.4(7) 2_665 2_566 ? O2 K O6 121.3(12) . 2_566 ? O8 K O6 52.5(5) 2_566 2_566 ? O5 K O6 101.0(10) 2_666 2_566 ? O8 K O6 126.8(8) 1_654 2_566 ? K K V2 84(3) 2_665 2_566 ? OW1 K V2 86.7(6) . 2_566 ? OW1 K V2 90.9(7) 2_665 2_566 ? O2 K V2 119.8(10) . 2_566 ? O8 K V2 29.0(3) 2_566 2_566 ? O5 K V2 128.3(11) 2_666 2_566 ? O8 K V2 141.4(6) 1_654 2_566 ? O6 K V2 27.4(3) 2_566 2_566 ? K K V2 80(3) 2_665 1_654 ? OW1 K V2 91.5(10) . 1_654 ? OW1 K V2 84.7(7) 2_665 1_654 ? O2 K V2 74.1(6) . 1_654 ? O8 K V2 151.2(11) 2_566 1_654 ? O5 K V2 61.0(5) 2_666 1_654 ? O8 K V2 28.7(3) 1_654 1_654 ? O6 K V2 155.0(8) 2_566 1_654 ? V2 K V2 163.3(9) 2_566 1_654 ? K K Fe2 87(3) 2_665 2_665 ? OW1 K Fe2 147.0(13) . 2_665 ? OW1 K Fe2 33.3(3) 2_665 2_665 ? O2 K Fe2 103.6(6) . 2_665 ? O8 K Fe2 152.0(10) 2_566 2_665 ? O5 K Fe2 30.4(3) 2_666 2_665 ? O8 K Fe2 32.4(3) 1_654 2_665 ? O6 K Fe2 99.8(8) 2_566 2_665 ? V2 K Fe2 123.5(8) 2_566 2_665 ? V2 K Fe2 55.7(4) 1_654 2_665 ? _refine_diff_density_max 1.328 _refine_diff_density_min -1.508 _refine_diff_density_rms 0.264 _shelx_res_file ; TITL JS-9-2019-01 js-9-2019-01.res created by SHELXL-2016/6 at 16:03:28 on 27-Aug-2020 CELL 0.71075 6.65460 6.66887 9.00340 76.51500 84.40000 75.05830 ZERR 1 0.00166 0.00140 0.00220 0.00540 0.00590 0.00530 LATT 1 SFAC H O V P FE K UNIT 0 18.72 3.64 0.36 4 0.28 L.S. 20 omit 2 -2 1 EXYZ V1 P1 EADP V1 P1 EXYZ V2 P2 EADP V2 P2 EXYZ K OW2 EADP K OW2 FMAP 2 PLAN 20 EQIV $1 -x+1, -y, -z+1 BIND OW1 O2 BIND OW1 O7_$1 ACTA SIZE 0.050 0.040 0.020 WGHT 0.114600 1.031900 FVAR 0.68793 0.92666 0.89479 0.27673 FE1 5 0.204152 0.327517 0.474917 11.00000 0.02920 0.03848 = 0.01927 -0.01074 -0.00135 -0.00904 FE2 5 0.140571 0.146144 0.198267 11.00000 0.03504 0.04111 = 0.02037 -0.01145 -0.00184 -0.01060 V1 3 0.750150 0.206835 0.447378 21.00000 0.02841 0.03814 = 0.02030 -0.00959 -0.00278 -0.01009 P1 4 0.750150 0.206835 0.447378 -21.00000 0.02841 0.03814 = 0.02030 -0.00959 -0.00278 -0.01009 V2 3 0.001201 0.304960 0.816242 31.00000 0.03381 0.03899 = 0.01933 -0.01012 -0.00176 -0.01077 P2 4 0.001201 0.304960 0.816242 -31.00000 0.03381 0.03899 = 0.01933 -0.01012 -0.00176 -0.01077 O1 2 0.497299 0.313667 0.439663 11.00000 0.03034 0.04586 = 0.02916 -0.01465 0.00362 -0.01166 O2 2 0.839572 0.192003 0.269655 11.00000 0.03367 0.04509 = 0.02721 -0.01010 0.00000 -0.01407 O3 2 0.876629 0.366636 0.511191 11.00000 0.02524 0.03566 = 0.02134 -0.00849 0.00231 -0.00493 O4 2 0.787412 -0.042723 0.572293 11.00000 0.03603 0.04105 = 0.02013 -0.00940 -0.00007 -0.01145 O5 2 0.090739 0.282757 0.986009 11.00000 0.04719 0.03832 = 0.02433 -0.01238 -0.00381 -0.00771 O6 2 -0.151882 0.134493 0.832696 11.00000 0.04186 0.03333 = 0.02901 -0.00515 0.00125 -0.01110 O7 2 0.215172 0.239298 0.698854 11.00000 0.04268 0.04455 = 0.02310 -0.01250 0.00236 -0.01387 O8 2 -0.142797 0.570843 0.751366 11.00000 0.03970 0.02920 = 0.01449 -0.00688 -0.00186 -0.00954 OW1 2 0.463407 0.090025 0.141186 11.00000 0.03500 0.06906 = 0.03307 -0.00873 -0.00377 -0.01372 K 6 0.535523 0.497641 0.051483 40.50000 0.04664 0.12136 = 0.21635 0.04865 0.00501 -0.02340 OW2 2 0.535523 0.497641 0.051483 -40.50000 0.04664 0.12136 = 0.21635 0.04865 0.00501 -0.02340 HKLF 4 REM JS-9-2019-01 REM R1 = 0.0678 for 1098 Fo > 4sig(Fo) and 0.0778 for all 1316 data REM 130 parameters refined using 0 restraints END WGHT 0.1146 1.0323 REM Highest difference peak 1.328, deepest hole -1.508, 1-sigma level 0.264 Q1 1 0.0489 0.3503 0.4819 11.00000 0.05 1.29 Q2 1 0.3586 0.3171 0.4588 11.00000 0.05 1.17 Q3 1 0.2845 0.1357 0.1974 11.00000 0.05 1.13 Q4 1 0.5773 0.2201 0.4379 11.00000 0.05 1.07 Q5 1 0.1630 0.2969 0.8263 11.00000 0.05 1.02 Q6 1 -0.0202 0.1543 0.2024 11.00000 0.05 0.95 Q7 1 0.7196 0.0021 0.5102 11.00000 0.05 0.91 Q8 1 0.8531 -0.0588 0.5492 11.00000 0.05 0.88 Q9 1 0.9191 0.3185 0.5546 11.00000 0.05 0.86 Q10 1 -0.2166 0.6716 0.8760 11.00000 0.05 0.84 Q11 1 0.0001 0.0326 0.7464 11.00000 0.05 0.81 Q12 1 0.4948 0.1617 0.0818 11.00000 0.05 0.81 Q13 1 0.8758 -0.1437 0.4642 11.00000 0.05 0.80 Q14 1 0.2891 0.5071 0.4014 11.00000 0.05 0.79 Q15 1 0.7875 0.3663 0.5336 11.00000 0.05 0.79 Q16 1 0.7126 -0.1371 0.5614 11.00000 0.05 0.77 Q17 1 -0.1204 -0.0168 0.8541 11.00000 0.05 0.72 Q18 1 0.5889 0.3970 0.0810 11.00000 0.05 0.71 Q19 1 0.5997 -0.1718 0.1372 11.00000 0.05 0.71 Q20 1 -0.1633 0.2887 0.7988 11.00000 0.05 0.70 ; _shelx_res_checksum 54825 _shelx_hkl_file ; 1 0 0 5336.75 407.90 1 0 0 5266.40 390.32 -1 0 0 5219.60 365.31 -1 0 0 5588.12 412.87 0 -1 -1 47.06 3.57 0 -1 -1 51.56 6.64 0 1 1 45.90 5.86 0 1 1 41.69 3.45 0 -1 -1 52.27 3.69 0 1 1 48.80 3.42 -1 0 -1 329.40 17.31 1 0 1 330.88 17.72 1 1 0 849.00 35.14 1 1 0 781.21 31.37 -1 -1 0 769.02 30.48 -1 -1 0 921.78 39.92 1 0 -1 688.40 29.73 1 0 -1 726.52 38.42 -1 0 1 745.63 28.07 -1 -1 -1 0.49 3.87 1 1 1 1.56 2.26 -1 -1 -1 1.41 2.28 1 1 1 -1.64 2.22 0 1 -1 873.97 30.15 0 1 -1 868.04 29.71 0 -1 1 882.51 31.44 0 -1 1 877.57 29.52 0 0 2 123.82 7.14 0 0 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300.49 57.67 5 -2 -7 418.02 67.14 -5 2 7 428.58 73.34 -5 2 7 419.25 64.69 7 -1 3 511.13 76.39 7 -1 3 455.87 83.42 7 -1 3 344.84 82.64 -7 1 -3 364.02 80.65 6 -2 -5 -17.41 10.15 -6 2 5 -10.28 18.16 -6 2 5 10.73 15.63 6 -2 -5 -0.16 16.38 -7 -1 4 13.91 22.38 -7 -1 4 18.21 23.12 7 1 -4 43.36 24.09 7 1 -4 33.97 16.37 7 5 4 33.01 28.73 -7 -5 -4 113.84 21.37 -7 -5 -4 75.29 17.10 7 5 4 123.97 33.38 0 1 -10 -3.41 14.69 0 -1 10 1.51 13.80 1 -7 1 30.76 16.22 1 -7 1 41.09 16.40 5 6 7 15.93 19.69 -5 -6 -7 22.79 15.16 -5 -6 -7 52.23 22.81 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 70848