data_ps-dt _audit_creation_method 'SHELXL-2016/6' _shelx_SHELXL_version_number '2016/6' _chemical_name_mineral 'pseudodickthomssenite' _chemical_compound_source 'Pickett Corral mine, Colorado' _chemical_formula_sum 'H16 Mg O14 V2' _chemical_formula_weight 366.32 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' 'Mg' 'Mg' 0.0486 0.0363 '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 7.3566(6) _cell_length_b 9.4672(9) _cell_length_c 9.5529(9) _cell_angle_alpha 104.205(7) _cell_angle_beta 100.786(7) _cell_angle_gamma 100.157(7) _cell_volume 616.08(10) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4126 _cell_measurement_theta_min 3.2 _cell_measurement_theta_max 21.7 _exptl_crystal_description 'needle' _exptl_crystal_colour 'beige' _exptl_crystal_density_diffrn 1.975 _exptl_crystal_F_000 372 _exptl_crystal_size_max 0.260 _exptl_crystal_size_mid 0.020 _exptl_crystal_size_min 0.015 _exptl_absorpt_coefficient_mu 1.633 _shelx_estimated_absorpt_T_min 0.676 _shelx_estimated_absorpt_T_max 0.976 _exptl_absorpt_correction_type 'Multi-scan' _exptl_absorpt_process_details Higashi2001 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.687 _diffrn_ambient_temperature 293(2) _diffrn_measurement_device_type 'Rigaku R-axis RAPID II' _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_reflns_number 5938 _diffrn_reflns_av_unetI/netI 0.0385 _diffrn_reflns_av_R_equivalents 0.0499 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 3.220 _diffrn_reflns_theta_max 21.712 _diffrn_reflns_theta_full 21.712 _diffrn_measured_fraction_theta_max 0.992 _diffrn_measured_fraction_theta_full 0.992 _diffrn_reflns_Laue_measured_fraction_max 0.992 _diffrn_reflns_Laue_measured_fraction_full 0.992 _diffrn_reflns_point_group_measured_fraction_max 0.992 _diffrn_reflns_point_group_measured_fraction_full 0.992 _reflns_number_total 1451 _reflns_number_gt 1124 _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^)+(0.0211P)^2^+0.6932P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment refxyz _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 1451 _refine_ls_number_parameters 205 _refine_ls_number_restraints 24 _refine_ls_R_factor_all 0.0440 _refine_ls_R_factor_gt 0.0307 _refine_ls_wR_factor_ref 0.0707 _refine_ls_wR_factor_gt 0.0660 _refine_ls_goodness_of_fit_ref 1.098 _refine_ls_restrained_S_all 1.095 _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 Mg1 Mg 0.500000 0.000000 0.500000 0.0247(5) Uani 1 2 d S . P . . Mg2 Mg 0.000000 0.500000 0.000000 0.0357(6) Uani 1 2 d S . P . . V1 V 0.91768(9) 0.04182(8) 0.13835(8) 0.0202(2) Uani 1 1 d . . . . . V2 V 0.42256(9) 0.05462(8) 0.14131(8) 0.0204(2) Uani 1 1 d . . . . . O1 O 0.9695(4) 0.2190(3) 0.2324(3) 0.0347(8) Uani 1 1 d . . . . . O2 O 0.9338(4) 0.9403(3) 0.2564(3) 0.0289(7) Uani 1 1 d . . . . . O3 O 0.1520(4) 0.0333(3) 0.0807(3) 0.0268(7) Uani 1 1 d . . . . . O4 O 0.6455(4) 0.0068(3) 0.0803(3) 0.0285(7) Uani 1 1 d . . . . . O5 O 0.4968(4) 0.2325(3) 0.2257(3) 0.0317(8) Uani 1 1 d . . . . . O6 O 0.4262(4) 0.9631(3) 0.2693(3) 0.0245(7) Uani 1 1 d . . . . . OW1 O 0.2374(4) 0.0343(5) 0.5093(4) 0.0470(10) Uani 1 1 d D . . . . H1A H 0.159(6) 0.016(6) 0.435(3) 0.056 Uiso 1 1 d D U . . . H1B H 0.196(6) 0.039(6) 0.579(3) 0.056 Uiso 1 1 d D U . . . OW2 O 0.5998(6) 0.2302(4) 0.5318(4) 0.0467(10) Uani 1 1 d D . . . . H2A H 0.545(7) 0.289(5) 0.568(5) 0.056 Uiso 1 1 d D U . . . H2B H 0.619(7) 0.245(5) 0.458(4) 0.056 Uiso 1 1 d D U . . . OW3 O 0.7958(5) 0.4031(4) 0.0874(5) 0.0513(10) Uani 1 1 d D . . . . H3A H 0.804(7) 0.358(5) 0.147(4) 0.062 Uiso 1 1 d D U . . . H3B H 0.695(5) 0.371(6) 0.031(5) 0.062 Uiso 1 1 d D U . . . OW4 O 0.8026(5) 0.6008(4) 0.9077(5) 0.0481(10) Uani 1 1 d D . . . . H4A H 0.823(7) 0.654(5) 0.857(5) 0.058 Uiso 1 1 d D U . . . H4B H 0.731(7) 0.627(5) 0.956(5) 0.058 Uiso 1 1 d D U . . . OW5 O 0.0846(5) 0.6807(4) 0.1921(5) 0.0613(11) Uani 1 1 d D . . . . H5A H 0.036(6) 0.751(5) 0.199(6) 0.074 Uiso 1 1 d D U . . . H5B H 0.190(4) 0.702(6) 0.231(6) 0.074 Uiso 1 1 d D U . . . OW6 O 0.4354(5) 0.3170(4) 0.9112(4) 0.0476(10) Uani 1 1 d D . . . . H6A H 0.415(7) 0.228(3) 0.879(5) 0.057 Uiso 1 1 d D U . . . H6B H 0.416(7) 0.347(5) 0.838(4) 0.057 Uiso 1 1 d D U . . . OW7 O 0.4106(6) 0.4294(4) 0.6674(5) 0.0651(12) Uani 1 1 d D . . . . H7A H 0.456(7) 0.515(3) 0.698(6) 0.078 Uiso 1 1 d D U . . . H7B H 0.303(5) 0.417(6) 0.620(6) 0.078 Uiso 1 1 d D U . . . OW8 O 0.0271(8) 0.3651(5) 0.5301(5) 0.0778(13) Uani 1 1 d D . . . . H8A H 0.009(10) 0.311(5) 0.447(4) 0.093 Uiso 1 1 d D U . . . H8B H 0.012(11) 0.444(4) 0.530(6) 0.093 Uiso 1 1 d D U . . . 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 Mg1 0.0210(12) 0.0365(13) 0.0198(12) 0.0106(10) 0.0066(9) 0.0093(9) Mg2 0.0283(13) 0.0305(13) 0.0498(16) 0.0157(12) 0.0058(11) 0.0088(10) V1 0.0160(5) 0.0301(5) 0.0169(5) 0.0082(4) 0.0043(3) 0.0093(3) V2 0.0153(4) 0.0327(5) 0.0162(5) 0.0091(4) 0.0047(3) 0.0093(3) O1 0.0358(19) 0.0315(18) 0.034(2) 0.0038(16) 0.0069(16) 0.0109(15) O2 0.0270(18) 0.0411(19) 0.0244(18) 0.0164(15) 0.0064(14) 0.0125(14) O3 0.0155(16) 0.051(2) 0.0164(17) 0.0111(15) 0.0055(13) 0.0109(14) O4 0.0167(16) 0.053(2) 0.0168(17) 0.0074(15) 0.0057(13) 0.0141(14) O5 0.036(2) 0.0300(17) 0.0279(19) 0.0062(15) 0.0063(15) 0.0086(15) O6 0.0227(17) 0.0356(18) 0.0177(17) 0.0101(14) 0.0051(13) 0.0099(13) OW1 0.025(2) 0.099(3) 0.021(2) 0.019(2) 0.0062(15) 0.022(2) OW2 0.059(3) 0.042(2) 0.042(3) 0.014(2) 0.020(2) 0.0094(18) OW3 0.037(2) 0.059(3) 0.069(3) 0.040(2) 0.010(2) 0.013(2) OW4 0.034(2) 0.052(2) 0.071(3) 0.037(2) 0.0116(18) 0.0152(17) OW5 0.047(3) 0.048(2) 0.072(3) -0.001(2) -0.008(2) 0.019(2) OW6 0.043(2) 0.038(2) 0.060(3) 0.018(2) 0.005(2) 0.0069(19) OW7 0.082(3) 0.046(2) 0.057(3) 0.004(2) 0.005(2) 0.017(2) OW8 0.107(4) 0.076(3) 0.052(3) 0.011(3) 0.023(3) 0.035(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 Mg1 OW1 2.029(3) . ? Mg1 OW1 2.029(3) 2_656 ? Mg1 O6 2.093(3) 1_545 ? Mg1 O6 2.093(3) 2_666 ? Mg1 OW2 2.099(3) . ? Mg1 OW2 2.099(3) 2_656 ? Mg2 OW3 2.038(3) 2_665 ? Mg2 OW3 2.038(3) 1_455 ? Mg2 OW4 2.054(3) 2_666 ? Mg2 OW4 2.054(3) 1_454 ? Mg2 OW5 2.083(4) 2_565 ? Mg2 OW5 2.083(4) . ? V1 O1 1.635(3) . ? V1 O2 1.652(3) 1_545 ? V1 O3 1.914(3) 1_655 ? V1 O4 1.920(3) . ? V1 O3 1.971(3) 2_655 ? V1 V1 3.0968(14) 2_755 ? V1 V2 3.1192(10) 2_655 ? V2 O5 1.622(3) . ? V2 O6 1.662(3) 1_545 ? V2 O3 1.926(3) . ? V2 O4 1.930(3) . ? V2 O4 1.992(3) 2_655 ? OW1 H1A 0.79(3) . ? OW1 H1B 0.77(3) . ? OW2 H2A 0.80(3) . ? OW2 H2B 0.78(3) . ? OW3 H3A 0.79(3) . ? OW3 H3B 0.79(3) . ? OW4 H4A 0.80(3) . ? OW4 H4B 0.79(3) . ? OW5 H5A 0.81(3) . ? OW5 H5B 0.76(3) . ? OW6 H6A 0.80(3) . ? OW6 H6B 0.81(3) . ? OW7 H7A 0.78(3) . ? OW7 H7B 0.80(3) . ? OW8 H8A 0.81(3) . ? OW8 H8B 0.77(3) . ? 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 OW1 Mg1 OW1 180.0 . 2_656 ? OW1 Mg1 O6 89.35(12) . 1_545 ? OW1 Mg1 O6 90.65(12) 2_656 1_545 ? OW1 Mg1 O6 90.65(12) . 2_666 ? OW1 Mg1 O6 89.35(12) 2_656 2_666 ? O6 Mg1 O6 180.00(15) 1_545 2_666 ? OW1 Mg1 OW2 89.43(16) . . ? OW1 Mg1 OW2 90.57(16) 2_656 . ? O6 Mg1 OW2 90.48(12) 1_545 . ? O6 Mg1 OW2 89.52(12) 2_666 . ? OW1 Mg1 OW2 90.57(16) . 2_656 ? OW1 Mg1 OW2 89.43(16) 2_656 2_656 ? O6 Mg1 OW2 89.52(12) 1_545 2_656 ? O6 Mg1 OW2 90.48(12) 2_666 2_656 ? OW2 Mg1 OW2 180.0 . 2_656 ? OW3 Mg2 OW3 180.0 2_665 1_455 ? OW3 Mg2 OW4 87.63(14) 2_665 2_666 ? OW3 Mg2 OW4 92.37(14) 1_455 2_666 ? OW3 Mg2 OW4 92.37(14) 2_665 1_454 ? OW3 Mg2 OW4 87.63(14) 1_455 1_454 ? OW4 Mg2 OW4 180.0 2_666 1_454 ? OW3 Mg2 OW5 89.16(17) 2_665 2_565 ? OW3 Mg2 OW5 90.84(17) 1_455 2_565 ? OW4 Mg2 OW5 90.18(16) 2_666 2_565 ? OW4 Mg2 OW5 89.82(16) 1_454 2_565 ? OW3 Mg2 OW5 90.84(17) 2_665 . ? OW3 Mg2 OW5 89.16(17) 1_455 . ? OW4 Mg2 OW5 89.82(16) 2_666 . ? OW4 Mg2 OW5 90.18(16) 1_454 . ? OW5 Mg2 OW5 180.0 2_565 . ? O1 V1 O2 108.95(14) . 1_545 ? O1 V1 O3 98.87(13) . 1_655 ? O2 V1 O3 99.19(13) 1_545 1_655 ? O1 V1 O4 99.65(14) . . ? O2 V1 O4 98.69(13) 1_545 . ? O3 V1 O4 148.41(12) 1_655 . ? O1 V1 O3 124.28(13) . 2_655 ? O2 V1 O3 126.78(14) 1_545 2_655 ? O3 V1 O3 74.32(13) 1_655 2_655 ? O4 V1 O3 74.11(11) . 2_655 ? O1 V1 V1 116.99(11) . 2_755 ? O2 V1 V1 118.68(11) 1_545 2_755 ? O3 V1 V1 37.80(8) 1_655 2_755 ? O4 V1 V1 110.62(9) . 2_755 ? O3 V1 V1 36.52(8) 2_655 2_755 ? O1 V1 V2 115.20(11) . 2_655 ? O2 V1 V2 120.64(10) 1_545 2_655 ? O3 V1 V2 110.59(8) 1_655 2_655 ? O4 V1 V2 37.93(8) . 2_655 ? O3 V1 V2 36.33(8) 2_655 2_655 ? V1 V1 V2 72.81(3) 2_755 2_655 ? O5 V2 O6 108.30(14) . 1_545 ? O5 V2 O3 101.89(14) . . ? O6 V2 O3 98.88(12) 1_545 . ? O5 V2 O4 101.78(13) . . ? O6 V2 O4 96.86(13) 1_545 . ? O3 V2 O4 145.68(12) . . ? O5 V2 O4 117.13(13) . 2_655 ? O6 V2 O4 134.56(13) 1_545 2_655 ? O3 V2 O4 73.53(11) . 2_655 ? O4 V2 O4 73.68(13) . 2_655 ? O5 V2 V1 116.95(10) . 2_655 ? O6 V2 V1 120.46(10) 1_545 2_655 ? O3 V2 V1 37.34(8) . 2_655 ? O4 V2 V1 108.92(8) . 2_655 ? O4 V2 V1 36.34(8) 2_655 2_655 ? V1 O3 V2 147.83(15) 1_455 . ? V1 O3 V1 105.69(13) 1_455 2_655 ? V2 O3 V1 106.34(13) . 2_655 ? V1 O4 V2 144.91(16) . . ? V1 O4 V2 105.73(13) . 2_655 ? V2 O4 V2 106.32(13) . 2_655 ? V2 O6 Mg1 141.32(16) 1_565 1_565 ? Mg1 OW1 H1A 119(3) . . ? Mg1 OW1 H1B 124(4) . . ? H1A OW1 H1B 113(4) . . ? Mg1 OW2 H2A 121(4) . . ? Mg1 OW2 H2B 111(4) . . ? H2A OW2 H2B 109(4) . . ? Mg2 OW3 H3A 130(4) 1_655 . ? Mg2 OW3 H3B 114(4) 1_655 . ? H3A OW3 H3B 109(4) . . ? Mg2 OW4 H4A 124(4) 1_656 . ? Mg2 OW4 H4B 117(4) 1_656 . ? H4A OW4 H4B 111(4) . . ? Mg2 OW5 H5A 121(4) . . ? Mg2 OW5 H5B 116(4) . . ? H5A OW5 H5B 113(4) . . ? H6A OW6 H6B 105(4) . . ? H7A OW7 H7B 109(4) . . ? H8A OW8 H8B 112(5) . . ? 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 OW1 H1A O2 0.79(3) 2.02(3) 2.800(4) 170(5) 1_445 OW1 H1B O2 0.77(3) 1.98(3) 2.748(4) 173(5) 2_666 OW2 H2A OW7 0.80(3) 1.96(3) 2.752(6) 177(5) . OW2 H2B O5 0.78(3) 2.20(4) 2.886(5) 147(5) . OW3 H3A O1 0.79(3) 2.14(4) 2.810(4) 142(5) . OW3 H3B OW6 0.79(3) 1.94(3) 2.724(5) 171(6) 1_554 OW4 H4A O1 0.80(3) 2.20(3) 2.909(4) 148(5) 2_766 OW4 H4B OW6 0.79(3) 1.97(3) 2.760(5) 174(5) 2_667 OW5 H5A O2 0.81(3) 2.05(3) 2.850(5) 170(6) 1_455 OW5 H5B O6 0.76(3) 2.66(5) 3.158(4) 125(5) . OW5 H5B OW2 0.76(3) 2.36(5) 2.998(6) 142(6) 2_666 OW6 H6A O4 0.80(3) 2.33(3) 3.042(4) 149(4) 2_656 OW6 H6A O6 0.80(3) 2.60(4) 3.226(5) 137(5) 2_666 OW6 H6B OW7 0.81(3) 1.97(3) 2.778(6) 171(5) . OW7 H7A O5 0.78(3) 2.26(3) 3.019(5) 165(5) 2_666 OW7 H7B OW8 0.80(3) 1.98(3) 2.769(7) 169(6) . OW8 H8A O1 0.81(3) 1.96(3) 2.756(5) 167(6) 1_455 OW8 H8B OW8 0.77(3) 2.08(3) 2.830(9) 164(6) 2_566 _refine_diff_density_max 0.261 _refine_diff_density_min -0.281 _refine_diff_density_rms 0.066 _shelx_res_file ; TITL pseudodickthomssenite ps-dt.res created by SHELXL-2016/6 at 20:13:46 on 16-Feb-2021 CELL 0.71075 7.35657 9.46717 9.55291 104.20500 100.78600 100.15700 ZERR 2 0.00061 0.00094 0.00091 0.00730 0.00710 0.00710 LATT 1 SFAC H MG O V UNIT 32 2 28 4 L.S. 20 omit 6 0 0 FMAP 2 PLAN 20 HTAB EQIV $13 x-1, y-1, z HTAB OW1 O2_$13 EQIV $8 -x+1, -y+1, -z+1 HTAB OW1 O2_$8 HTAB OW2 OW7 HTAB OW2 O5 HTAB OW3 O1 EQIV $14 x, y, z-1 HTAB OW3 OW6_$14 EQIV $15 -x+2, -y+1, -z+1 HTAB OW4 O1_$15 EQIV $16 -x+1, -y+1, -z+2 HTAB OW4 OW6_$16 EQIV $4 x-1, y, z HTAB OW5 O2_$4 HTAB OW5 O6 HTAB OW5 OW2_$8 EQIV $9 -x+1, -y, -z+1 HTAB OW6 O4_$9 HTAB OW6 O6_$8 HTAB OW6 OW7 HTAB OW7 O5_$8 HTAB OW7 OW8 HTAB OW8 O1_$4 EQIV $17 -x, -y+1, -z+1 HTAB OW8 OW8_$17 BOND $H DFIX 0.82 0.03 OW1 H1a OW1 H1b OW2 H2a OW2 H2b OW3 H3a OW3 H3b DFIX 0.82 0.03 OW4 H4a OW4 H4b OW5 H5a OW5 H5b OW6 H6a OW6 H6b DFIX 0.82 0.03 OW7 H7a OW7 H7b OW8 H8a OW8 H8b DFIX 1.30 0.03 H1a H1b H2a H2b H3a H3b H4a H4b H5a H5b DFIX 1.30 0.03 H6a H6b H7a H7b H8a H8b ACTA SIZE 0.260 0.020 0.015 WGHT 0.021100 0.693200 FVAR 0.83728 MG1 2 0.500000 0.000000 0.500000 10.50000 0.02099 0.03653 = 0.01977 0.01064 0.00665 0.00933 MG2 2 0.000000 0.500000 0.000000 10.50000 0.02826 0.03048 = 0.04976 0.01566 0.00575 0.00879 V1 4 0.917681 0.041821 0.138350 11.00000 0.01598 0.03006 = 0.01693 0.00815 0.00434 0.00934 V2 4 0.422555 0.054623 0.141306 11.00000 0.01527 0.03268 = 0.01623 0.00911 0.00470 0.00935 O1 3 0.969510 0.219010 0.232353 11.00000 0.03578 0.03146 = 0.03437 0.00380 0.00689 0.01091 O2 3 0.933791 0.940345 0.256381 11.00000 0.02700 0.04109 = 0.02439 0.01640 0.00644 0.01246 O3 3 0.151987 0.033349 0.080684 11.00000 0.01549 0.05122 = 0.01639 0.01111 0.00552 0.01094 O4 3 0.645488 0.006762 0.080342 11.00000 0.01672 0.05347 = 0.01678 0.00739 0.00570 0.01407 O5 3 0.496762 0.232543 0.225746 11.00000 0.03584 0.02996 = 0.02792 0.00620 0.00627 0.00863 O6 3 0.426180 0.963069 0.269314 11.00000 0.02265 0.03561 = 0.01775 0.01006 0.00505 0.00987 OW1 3 0.237398 0.034317 0.509258 11.00000 0.02491 0.09900 = 0.02113 0.01901 0.00618 0.02165 H1A 1 0.158945 0.016298 0.435034 11.00000 -1.20000 H1B 1 0.196080 0.039322 0.578637 11.00000 -1.20000 OW2 3 0.599824 0.230175 0.531750 11.00000 0.05910 0.04191 = 0.04232 0.01383 0.01994 0.00938 H2A 1 0.545154 0.289116 0.568497 11.00000 -1.20000 H2B 1 0.618587 0.245166 0.458087 11.00000 -1.20000 OW3 3 0.795798 0.403084 0.087378 11.00000 0.03708 0.05923 = 0.06878 0.03968 0.01007 0.01291 H3A 1 0.804251 0.358086 0.147231 11.00000 -1.20000 H3B 1 0.695477 0.370876 0.030928 11.00000 -1.20000 OW4 3 0.802631 0.600765 0.907706 11.00000 0.03362 0.05186 = 0.07109 0.03722 0.01157 0.01524 H4A 1 0.822969 0.653687 0.856618 11.00000 -1.20000 H4B 1 0.731073 0.627243 0.955578 11.00000 -1.20000 OW5 3 0.084560 0.680727 0.192075 11.00000 0.04705 0.04818 = 0.07230 -0.00067 -0.00818 0.01883 H5A 1 0.036433 0.751499 0.199142 11.00000 -1.20000 H5B 1 0.190038 0.701945 0.230584 11.00000 -1.20000 OW6 3 0.435352 0.317018 0.911220 11.00000 0.04343 0.03777 = 0.05971 0.01820 0.00468 0.00693 H6A 1 0.415226 0.228084 0.879258 11.00000 -1.20000 H6B 1 0.415955 0.347302 0.838439 11.00000 -1.20000 OW7 3 0.410616 0.429399 0.667361 11.00000 0.08185 0.04604 = 0.05718 0.00400 0.00457 0.01728 H7A 1 0.455727 0.515293 0.698310 11.00000 -1.20000 H7B 1 0.303423 0.416952 0.620183 11.00000 -1.20000 OW8 3 0.027056 0.365086 0.530134 11.00000 0.10728 0.07641 = 0.05241 0.01122 0.02303 0.03492 H8A 1 0.009289 0.310578 0.447091 11.00000 -1.20000 H8B 1 0.012275 0.443713 0.530167 11.00000 -1.20000 HKLF 4 REM pseudodickthomssenite REM R1 = 0.0307 for 1124 Fo > 4sig(Fo) and 0.0440 for all 1451 data REM 205 parameters refined using 24 restraints END WGHT 0.0210 0.7014 REM Instructions for potential hydrogen bonds HTAB OW1 O2_$13 HTAB OW1 O2_$8 HTAB OW2 OW7 HTAB OW2 O5 HTAB OW3 O1 HTAB OW3 OW6_$14 HTAB OW4 O1_$15 HTAB OW4 OW6_$16 HTAB OW5 O2_$4 HTAB OW5 O6 HTAB OW5 OW2_$8 HTAB OW6 O4_$9 HTAB OW6 O6_$8 HTAB OW6 OW7 HTAB OW7 O5_$8 HTAB OW7 OW8 HTAB OW8 O1_$4 HTAB OW8 OW8_$17 REM Highest difference peak 0.261, deepest hole -0.281, 1-sigma level 0.066 Q1 1 0.1002 0.5657 0.1833 11.00000 0.05 0.26 Q2 1 0.4651 0.9614 0.2068 11.00000 0.05 0.24 Q3 1 0.4614 1.0157 0.3256 11.00000 0.05 0.22 Q4 1 0.4573 0.5074 0.5998 11.00000 0.05 0.22 Q5 1 0.5967 0.0680 0.1221 11.00000 0.05 0.22 Q6 1 0.8819 1.0173 0.2548 11.00000 0.05 0.22 Q7 1 0.5315 -0.0374 0.0918 11.00000 0.05 0.21 Q8 1 0.9663 1.0177 0.3203 11.00000 0.05 0.21 Q9 1 0.7156 0.3939 0.5845 11.00000 0.05 0.20 Q10 1 0.8260 0.3355 0.0721 11.00000 0.05 0.20 Q11 1 0.1085 0.1092 0.1328 11.00000 0.05 0.20 Q12 1 0.8970 0.8560 0.2334 11.00000 0.05 0.20 Q13 1 0.1404 0.2237 0.5172 11.00000 0.05 0.20 Q14 1 0.4944 0.2158 0.7819 11.00000 0.05 0.20 Q15 1 0.5398 0.3257 0.2757 11.00000 0.05 0.20 Q16 1 0.0841 0.0594 0.1317 11.00000 0.05 0.20 Q17 1 0.0404 0.4373 0.7181 11.00000 0.05 0.20 Q18 1 1.0364 0.1632 0.2492 11.00000 0.05 0.20 Q19 1 0.8856 0.1566 0.2025 11.00000 0.05 0.19 Q20 1 1.0281 0.9374 0.3266 11.00000 0.05 0.19 ; _shelx_res_checksum 47446 _shelx_hkl_file ; -1 0 1 197.46 4.89 1 0 -1 200.68 4.62 -1 0 1 184.90 3.76 1 0 -1 180.56 10.82 -1 1 0 417.89 7.73 -1 1 0 456.23 11.83 1 -1 0 427.89 10.58 1 -1 0 421.46 11.58 1 -1 0 438.60 11.55 0 -1 -1 46.34 5.46 0 1 1 46.39 5.29 0 1 1 49.56 5.42 1 -1 -1 142.25 10.74 -1 1 1 125.52 6.44 -1 1 1 117.06 5.02 1 -1 -1 115.73 5.35 -1 -1 1 0.51 3.74 -1 -1 1 3.87 2.74 1 1 -1 -0.37 2.06 1 1 -1 3.24 2.54 1 1 -1 0.90 2.24 1 -1 1 23.24 4.38 -1 1 -1 22.75 4.11 1 -1 1 22.68 3.64 -1 1 -1 13.57 3.52 1 1 0 340.69 8.89 1 1 0 378.22 10.50 -1 -1 0 373.73 9.22 -1 -1 0 360.60 10.70 1 1 0 369.74 6.68 1 0 1 542.53 12.36 1 0 1 525.17 15.19 -1 0 -1 542.80 9.72 0 1 -2 309.74 16.53 0 -1 2 303.51 11.91 0 -1 2 298.56 11.38 0 1 -2 303.14 11.84 0 -1 2 307.39 7.52 0 -2 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12.69 22.46 -1 -6 -5 14.36 11.79 1 6 5 18.87 19.59 1 6 5 19.84 21.00 -1 -6 -5 7.00 12.14 2 1 8 848.90 61.63 2 1 8 657.58 41.42 -2 -1 -8 561.49 44.54 2 1 8 911.86 90.77 3 5 -9 4.52 13.61 -3 -5 9 -1.41 14.58 4 -8 -3 54.21 22.50 4 -8 -3 60.04 22.14 -4 8 3 0.46 24.50 -4 8 3 55.07 19.87 -3 5 7 -2.06 28.06 -3 5 7 -29.95 18.85 3 -5 -7 -7.87 20.63 4 -9 3 281.89 37.23 -4 9 -3 271.48 34.44 5 -2 -8 11.20 15.26 -5 2 8 21.75 14.02 -7 4 4 9.81 4.60 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 96965