data_wernerbaurite _audit_creation_method SHELXL-2013 _chemical_name_mineral 'wernerbaurite' _chemical_compound_source 'St. Jude mine, Colorado' _chemical_formula_sum 'H40 Ca2 N2 O44 V10' _chemical_formula_weight 1361.90 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'V' 'V' 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ca' 'Ca' 0.2262 0.3064 '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' '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' _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 9.7212(6) _cell_length_b 10.2598(8) _cell_length_c 10.5928(8) _cell_angle_alpha 89.999(6) _cell_angle_beta 77.083(7) _cell_angle_gamma 69.887(8) _cell_volume 963.55(13) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _exptl_crystal_density_diffrn 2.347 _exptl_crystal_F_000 676 _exptl_crystal_size_max 0.220 _exptl_crystal_size_mid 0.220 _exptl_crystal_size_min 0.040 _exptl_absorpt_coefficient_mu 2.706 _shelx_estimated_absorpt_T_min 0.587 _shelx_estimated_absorpt_T_max 0.899 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details Higashi2001 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_reflns_number 18540 _diffrn_reflns_av_unetI/netI 0.0373 _diffrn_reflns_av_R_equivalents 0.0421 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 3.021 _diffrn_reflns_theta_max 27.485 _diffrn_reflns_theta_full 25.242 _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 4389 _reflns_number_gt 3434 _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_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-2013 (Sheldrick, 2013)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; ? ; _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^)+(0.0438P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment refxyz _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 4389 _refine_ls_number_parameters 322 _refine_ls_number_restraints 34 _refine_ls_R_factor_all 0.0456 _refine_ls_R_factor_gt 0.0326 _refine_ls_wR_factor_ref 0.0822 _refine_ls_wR_factor_gt 0.0763 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_restrained_S_all 1.030 _refine_ls_shift/su_max 0.012 _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 V1 V 0.65434(4) 0.03562(4) 0.94781(4) 0.01911(11) Uani 1 1 d . . . . . V2 V 0.34781(5) 0.27087(4) 1.09313(4) 0.02369(12) Uani 1 1 d . . . . . V3 V 0.51792(5) 0.04010(4) 1.24708(4) 0.02204(11) Uani 1 1 d . . . . . V4 V 0.81415(5) -0.19828(4) 1.10353(4) 0.02517(12) Uani 1 1 d . . . . . V5 V 0.47683(5) 0.26108(4) 0.79393(4) 0.02557(12) Uani 1 1 d . . . . . Ca Ca 0.83958(6) 0.26600(5) 1.41295(5) 0.02818(14) Uani 1 1 d . . . . . O1 O 0.42645(18) 0.09865(16) 0.93184(15) 0.0205(4) Uani 1 1 d . . . . . O2 O 0.55958(19) 0.15861(16) 1.10234(16) 0.0220(4) Uani 1 1 d . . . . . O3 O 0.67182(19) -0.10442(16) 0.81795(15) 0.0218(4) Uani 1 1 d . . . . . O4 O 0.67560(19) 0.15783(17) 0.84541(16) 0.0248(4) Uani 1 1 d . . . . . O5 O 0.7192(2) -0.04447(17) 1.23257(16) 0.0256(4) Uani 1 1 d . . . . . O6 O 0.82405(19) -0.04412(17) 0.98197(17) 0.0255(4) Uani 1 1 d . . . . . O7 O 0.4664(2) -0.10252(17) 1.31928(16) 0.0255(4) Uani 1 1 d . . . . . O8 O 0.2763(2) 0.30404(17) 0.79398(17) 0.0280(4) Uani 1 1 d . . . . . O9 O 0.1693(2) 0.29939(17) 1.04787(17) 0.0267(4) Uani 1 1 d . . . . . O10 O 0.4244(2) 0.35648(17) 0.95861(17) 0.0274(4) Uani 1 1 d . . . . . O11 O 0.4654(2) 0.15388(18) 1.36945(17) 0.0315(4) Uani 1 1 d . . . . . O12 O 0.2999(2) 0.38382(19) 1.21502(19) 0.0366(5) Uani 1 1 d . . . . . O13 O 0.9833(2) -0.2523(2) 1.12121(19) 0.0366(5) Uani 1 1 d . . . . . O14 O 0.5287(2) 0.36612(19) 0.69979(19) 0.0380(5) Uani 1 1 d . . . . . OW1 O 0.7548(2) 0.0725(2) 1.46544(18) 0.0310(4) Uani 1 1 d D . . . . H1A H 0.741(3) 0.030(3) 1.406(2) 0.037 Uiso 1 1 d D U . . . H1B H 0.678(3) 0.086(3) 1.523(2) 0.037 Uiso 1 1 d D U . . . OW2 O 0.8884(2) 0.1347(2) 1.2021(2) 0.0388(5) Uani 1 1 d D . . . . H2A H 0.836(3) 0.094(3) 1.183(3) 0.047 Uiso 1 1 d D U . . . H2B H 0.970(2) 0.103(3) 1.153(3) 0.047 Uiso 1 1 d D U . . . OW3 O 1.0954(2) 0.1421(3) 1.3823(2) 0.0496(6) Uani 1 1 d D . . . . H3A H 1.127(4) 0.072(3) 1.418(3) 0.060 Uiso 1 1 d D U . . . H3B H 1.159(3) 0.138(3) 1.318(2) 0.060 Uiso 1 1 d D U . . . OW4 O 0.8367(3) -0.2914(3) 1.4246(2) 0.0693(8) Uani 1 1 d D . . . . H4A H 0.791(4) -0.243(4) 1.496(2) 0.083 Uiso 1 1 d D U . . . H4B H 0.769(4) -0.262(4) 1.381(3) 0.083 Uiso 1 1 d D U . . . OW5 O 0.9031(3) 0.4105(2) 1.2399(2) 0.0419(5) Uani 1 1 d D . . . . H5A H 0.978(3) 0.379(3) 1.179(3) 0.050 Uiso 1 1 d D U . . . H5B H 0.855(3) 0.4946(19) 1.247(3) 0.050 Uiso 1 1 d D U . . . OW6 O 0.5957(2) 0.3614(2) 1.3722(2) 0.0461(6) Uani 1 1 d D . . . . H6A H 0.540(3) 0.313(3) 1.380(3) 0.055 Uiso 1 1 d D U . . . H6B H 0.550(3) 0.4472(17) 1.374(3) 0.055 Uiso 1 1 d D U . . . OW7 O 0.8894(3) 0.2090(3) 1.6287(2) 0.0515(6) Uani 1 1 d D . . . . H7A H 0.960(3) 0.233(4) 1.629(3) 0.062 Uiso 1 1 d D U . . . H7B H 0.830(3) 0.208(4) 1.697(2) 0.062 Uiso 1 1 d D U . . . OW8 O 0.7836(4) 0.4827(3) 1.5249(2) 0.0653(8) Uani 1 1 d D . . . . H8A H 0.763(5) 0.488(4) 1.6041(17) 0.078 Uiso 1 1 d D U . . . H8B H 0.806(5) 0.541(3) 1.482(3) 0.078 Uiso 1 1 d D U . . . N N 0.2873(3) 0.6423(2) 0.9481(3) 0.0343(5) Uani 1 1 d D . . . . HNA H 0.339(3) 0.557(2) 0.957(3) 0.041 Uiso 1 1 d D U . . . HNB H 0.349(3) 0.692(3) 0.941(3) 0.041 Uiso 1 1 d D U . . . HNC H 0.214(3) 0.678(3) 1.021(2) 0.041 Uiso 1 1 d D U . . . HND H 0.249(3) 0.654(3) 0.883(2) 0.041 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 V1 0.0192(2) 0.0180(2) 0.0200(2) 0.00146(16) -0.00139(17) -0.00841(17) V2 0.0266(2) 0.0171(2) 0.0249(2) -0.00078(16) -0.00367(19) -0.00623(18) V3 0.0234(2) 0.0228(2) 0.0198(2) 0.00041(16) -0.00346(18) -0.00900(18) V4 0.0213(2) 0.0249(2) 0.0276(2) 0.00372(18) -0.00495(19) -0.00653(18) V5 0.0274(3) 0.0215(2) 0.0280(2) 0.00769(17) -0.0045(2) -0.01019(19) Ca 0.0267(3) 0.0279(3) 0.0293(3) 0.0016(2) -0.0038(2) -0.0106(2) O1 0.0221(9) 0.0197(8) 0.0194(9) 0.0017(7) -0.0027(7) -0.0083(7) O2 0.0229(9) 0.0198(8) 0.0236(9) -0.0001(7) -0.0024(7) -0.0098(7) O3 0.0209(9) 0.0219(8) 0.0210(9) 0.0006(7) -0.0013(7) -0.0079(7) O4 0.0257(10) 0.0230(9) 0.0269(10) 0.0043(7) -0.0027(8) -0.0123(8) O5 0.0249(10) 0.0293(9) 0.0236(9) 0.0019(7) -0.0055(8) -0.0107(8) O6 0.0215(10) 0.0268(9) 0.0269(9) 0.0020(7) -0.0021(8) -0.0094(8) O7 0.0280(10) 0.0266(9) 0.0208(9) 0.0047(7) -0.0024(8) -0.0104(8) O8 0.0278(10) 0.0241(9) 0.0298(10) 0.0067(7) -0.0063(8) -0.0068(8) O9 0.0232(9) 0.0227(9) 0.0286(10) -0.0004(7) -0.0014(8) -0.0042(7) O10 0.0311(10) 0.0196(8) 0.0314(10) 0.0042(7) -0.0047(8) -0.0106(8) O11 0.0337(11) 0.0330(10) 0.0256(10) -0.0048(8) -0.0040(8) -0.0110(9) O12 0.0412(12) 0.0274(10) 0.0361(11) -0.0070(8) -0.0055(9) -0.0083(9) O13 0.0261(11) 0.0402(11) 0.0378(11) 0.0012(9) -0.0057(9) -0.0057(9) O14 0.0428(12) 0.0338(10) 0.0416(12) 0.0173(9) -0.0108(10) -0.0184(9) OW1 0.0329(11) 0.0356(11) 0.0253(10) 0.0017(8) -0.0006(9) -0.0170(9) OW2 0.0375(12) 0.0389(12) 0.0381(12) -0.0084(9) 0.0064(10) -0.0207(10) OW3 0.0291(12) 0.0656(16) 0.0390(13) 0.0193(11) 0.0029(10) -0.0048(11) OW4 0.098(2) 0.086(2) 0.0473(16) 0.0140(14) -0.0276(15) -0.0554(19) OW5 0.0420(13) 0.0262(10) 0.0449(13) 0.0026(9) 0.0103(10) -0.0094(10) OW6 0.0346(12) 0.0284(11) 0.0784(17) 0.0121(11) -0.0191(12) -0.0115(9) OW7 0.0440(15) 0.0875(18) 0.0334(12) 0.0107(12) -0.0085(11) -0.0364(14) OW8 0.113(2) 0.0469(14) 0.0361(13) -0.0057(11) -0.0029(15) -0.0382(15) N 0.0319(14) 0.0246(12) 0.0459(15) 0.0021(11) -0.0096(12) -0.0093(11) _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 V1 O6 1.6913(18) . ? V1 O4 1.6939(16) . ? V1 O2 1.9096(17) . ? V1 O3 1.9270(16) . ? V1 O1 2.1063(15) 2_657 ? V1 O1 2.1300(17) . ? V1 V4 3.0780(6) . ? V1 V5 3.0818(6) . ? V2 O12 1.6084(18) . ? V2 O10 1.8252(17) . ? V2 O9 1.8304(18) . ? V2 O3 1.9959(16) 2_657 ? V2 O2 2.0082(18) . ? V2 O1 2.2611(16) . ? V2 V3 3.0842(6) . ? V2 V4 3.1058(6) 2_657 ? V3 O11 1.6118(17) . ? V3 O5 1.8176(18) . ? V3 O7 1.8194(16) . ? V3 O3 2.0107(18) 2_657 ? V3 O2 2.0134(16) . ? V3 O1 2.2188(16) 2_657 ? V3 V5 3.1018(6) 2_657 ? V4 O13 1.599(2) . ? V4 O8 1.8326(17) 2_657 ? V4 O9 1.8558(18) 2_657 ? V4 O5 1.9092(17) . ? V4 O6 2.0538(17) . ? V4 O1 2.3245(17) 2_657 ? V4 V5 3.0783(6) 2_657 ? V4 V2 3.1058(6) 2_657 ? V5 O14 1.5998(18) . ? V5 O8 1.8446(19) . ? V5 O7 1.8643(17) 2_657 ? V5 O10 1.8762(18) . ? V5 O4 2.0535(18) . ? V5 O1 2.3221(15) . ? V5 V4 3.0783(6) 2_657 ? V5 V3 3.1018(6) 2_657 ? Ca OW3 2.317(2) . ? Ca OW8 2.350(2) . ? Ca OW6 2.372(2) . ? Ca OW1 2.4182(18) . ? Ca OW5 2.462(2) . ? Ca OW7 2.470(2) . ? Ca OW2 2.473(2) . ? Ca H7A 2.77(3) . ? O1 V1 2.1063(15) 2_657 ? O1 V3 2.2189(16) 2_657 ? O1 V4 2.3245(17) 2_657 ? O3 V2 1.9958(16) 2_657 ? O3 V3 2.0107(17) 2_657 ? O7 V5 1.8642(17) 2_657 ? O8 V4 1.8326(17) 2_657 ? O9 V4 1.8558(18) 2_657 ? OW1 H1A 0.827(16) . ? OW1 H1B 0.819(16) . ? OW2 H2A 0.818(17) . ? OW2 H2B 0.799(17) . ? OW3 H3A 0.809(17) . ? OW3 H3B 0.799(17) . ? OW4 H4A 0.847(18) . ? OW4 H4B 0.859(18) . ? OW5 H5A 0.826(17) . ? OW5 H5B 0.822(17) . ? OW6 H6A 0.842(17) . ? OW6 H6B 0.838(17) . ? OW7 H7A 0.806(17) . ? OW7 H7B 0.820(17) . ? OW8 H8A 0.815(17) . ? OW8 H8B 0.811(17) . ? N HNA 0.866(18) . ? N HNB 0.910(18) . ? N HNC 0.902(18) . ? N HND 0.851(18) . ? 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 O6 V1 O4 106.37(8) . . ? O6 V1 O2 98.11(8) . . ? O4 V1 O2 96.97(8) . . ? O6 V1 O3 97.02(8) . . ? O4 V1 O3 97.18(8) . . ? O2 V1 O3 155.44(7) . . ? O6 V1 O1 87.77(7) . 2_657 ? O4 V1 O1 165.85(8) . 2_657 ? O2 V1 O1 81.17(6) . 2_657 ? O3 V1 O1 80.22(6) . 2_657 ? O6 V1 O1 166.07(7) . . ? O4 V1 O1 87.51(7) . . ? O2 V1 O1 80.98(7) . . ? O3 V1 O1 79.69(7) . . ? O1 V1 O1 78.34(7) 2_657 . ? O6 V1 V4 38.78(6) . . ? O4 V1 V4 145.14(6) . . ? O2 V1 V4 90.94(5) . . ? O3 V1 V4 88.84(5) . . ? O1 V1 V4 49.00(5) 2_657 . ? O1 V1 V4 127.32(4) . . ? O6 V1 V5 145.04(6) . . ? O4 V1 V5 38.68(6) . . ? O2 V1 V5 89.39(5) . . ? O3 V1 V5 89.21(5) . . ? O1 V1 V5 127.17(5) 2_657 . ? O1 V1 V5 48.83(4) . . ? V4 V1 V5 176.000(17) . . ? O12 V2 O10 102.79(9) . . ? O12 V2 O9 102.97(9) . . ? O10 V2 O9 95.63(8) . . ? O12 V2 O3 101.31(9) . 2_657 ? O10 V2 O3 153.54(8) . 2_657 ? O9 V2 O3 89.45(7) . 2_657 ? O12 V2 O2 100.33(9) . . ? O10 V2 O2 88.92(8) . . ? O9 V2 O2 154.60(7) . . ? O3 V2 O2 76.12(7) 2_657 . ? O12 V2 O1 175.12(9) . . ? O10 V2 O1 80.20(7) . . ? O9 V2 O1 80.44(7) . . ? O3 V2 O1 75.07(6) 2_657 . ? O2 V2 O1 75.73(6) . . ? O12 V2 V3 90.73(7) . . ? O10 V2 V3 128.89(6) . . ? O9 V2 V3 129.29(6) . . ? O3 V2 V3 39.84(5) 2_657 . ? O2 V2 V3 39.99(5) . . ? O1 V2 V3 84.39(4) . . ? O12 V2 V4 135.53(8) . 2_657 ? O10 V2 V4 83.60(6) . 2_657 ? O9 V2 V4 32.84(5) . 2_657 ? O3 V2 V4 86.85(5) 2_657 2_657 ? O2 V2 V4 123.95(5) . 2_657 ? O1 V2 V4 48.23(4) . 2_657 ? V3 V2 V4 119.542(17) . 2_657 ? O11 V3 O5 103.61(9) . . ? O11 V3 O7 102.56(8) . . ? O5 V3 O7 95.41(8) . . ? O11 V3 O3 98.74(8) . 2_657 ? O5 V3 O3 155.28(7) . 2_657 ? O7 V3 O3 89.88(7) . 2_657 ? O11 V3 O2 99.46(8) . . ? O5 V3 O2 90.22(7) . . ? O7 V3 O2 155.26(7) . . ? O3 V3 O2 75.67(7) 2_657 . ? O11 V3 O1 173.68(8) . 2_657 ? O5 V3 O1 81.19(7) . 2_657 ? O7 V3 O1 80.87(7) . 2_657 ? O3 V3 O1 75.83(6) 2_657 2_657 ? O2 V3 O1 76.21(6) . 2_657 ? O11 V3 V2 88.59(7) . . ? O5 V3 V2 130.08(6) . . ? O7 V3 V2 129.36(6) . . ? O3 V3 V2 39.49(5) 2_657 . ? O2 V3 V2 39.86(5) . . ? O1 V3 V2 85.15(4) 2_657 . ? O11 V3 V5 135.55(7) . 2_657 ? O5 V3 V5 84.28(6) . 2_657 ? O7 V3 V5 33.09(5) . 2_657 ? O3 V3 V5 87.16(5) 2_657 2_657 ? O2 V3 V5 124.48(5) . 2_657 ? O1 V3 V5 48.32(4) 2_657 2_657 ? V2 V3 V5 119.779(18) . 2_657 ? O13 V4 O8 104.32(9) . 2_657 ? O13 V4 O9 102.86(9) . 2_657 ? O8 V4 O9 92.51(8) 2_657 2_657 ? O13 V4 O5 101.41(9) . . ? O8 V4 O5 90.69(8) 2_657 . ? O9 V4 O5 153.89(8) 2_657 . ? O13 V4 O6 99.69(9) . . ? O8 V4 O6 155.92(8) 2_657 . ? O9 V4 O6 83.79(7) 2_657 . ? O5 V4 O6 82.79(7) . . ? O13 V4 O1 173.70(8) . 2_657 ? O8 V4 O1 81.76(7) 2_657 2_657 ? O9 V4 O1 78.23(7) 2_657 2_657 ? O5 V4 O1 76.60(7) . 2_657 ? O6 V4 O1 74.19(6) . 2_657 ? O13 V4 V1 130.73(7) . . ? O8 V4 V1 124.90(6) 2_657 . ? O9 V4 V1 79.00(6) 2_657 . ? O5 V4 V1 77.95(5) . . ? O6 V4 V1 31.05(5) . . ? O1 V4 V1 43.14(4) 2_657 . ? O13 V4 V5 137.61(7) . 2_657 ? O8 V4 V5 33.29(6) 2_657 2_657 ? O9 V4 V5 85.01(6) 2_657 2_657 ? O5 V4 V5 83.56(5) . 2_657 ? O6 V4 V5 122.66(5) . 2_657 ? O1 V4 V5 48.48(4) 2_657 2_657 ? V1 V4 V5 91.618(17) . 2_657 ? O13 V4 V2 135.12(7) . 2_657 ? O8 V4 V2 82.22(6) 2_657 2_657 ? O9 V4 V2 32.34(6) 2_657 2_657 ? O5 V4 V2 123.11(6) . 2_657 ? O6 V4 V2 82.07(5) . 2_657 ? O1 V4 V2 46.51(4) 2_657 2_657 ? V1 V4 V2 61.936(14) . 2_657 ? V5 V4 V2 60.700(15) 2_657 2_657 ? O14 V5 O8 104.13(9) . . ? O14 V5 O7 101.89(9) . 2_657 ? O8 V5 O7 91.62(8) . 2_657 ? O14 V5 O10 102.52(9) . . ? O8 V5 O10 91.11(8) . . ? O7 V5 O10 153.96(7) 2_657 . ? O14 V5 O4 99.59(9) . . ? O8 V5 O4 156.27(7) . . ? O7 V5 O4 83.95(7) 2_657 . ? O10 V5 O4 83.19(8) . . ? O14 V5 O1 174.27(9) . . ? O8 V5 O1 81.58(7) . . ? O7 V5 O1 77.22(6) 2_657 . ? O10 V5 O1 77.58(6) . . ? O4 V5 O1 74.70(6) . . ? O14 V5 V4 137.17(8) . 2_657 ? O8 V5 V4 33.04(5) . 2_657 ? O7 V5 V4 84.64(5) 2_657 2_657 ? O10 V5 V4 83.63(6) . 2_657 ? O4 V5 V4 123.23(5) . 2_657 ? O1 V5 V4 48.54(4) . 2_657 ? O14 V5 V1 130.63(8) . . ? O8 V5 V1 125.24(5) . . ? O7 V5 V1 79.01(5) 2_657 . ? O10 V5 V1 78.30(6) . . ? O4 V5 V1 31.04(4) . . ? O1 V5 V1 43.67(4) . . ? V4 V5 V1 92.201(16) 2_657 . ? O14 V5 V3 134.02(8) . 2_657 ? O8 V5 V3 81.90(5) . 2_657 ? O7 V5 V3 32.20(5) 2_657 2_657 ? O10 V5 V3 123.12(5) . 2_657 ? O4 V5 V3 82.04(5) . 2_657 ? O1 V5 V3 45.54(4) . 2_657 ? V4 V5 V3 60.815(16) 2_657 2_657 ? V1 V5 V3 61.887(14) . 2_657 ? OW3 Ca OW8 108.48(11) . . ? OW3 Ca OW6 160.89(9) . . ? OW8 Ca OW6 86.07(10) . . ? OW3 Ca OW1 96.93(8) . . ? OW8 Ca OW1 132.62(8) . . ? OW6 Ca OW1 81.00(7) . . ? OW3 Ca OW5 88.18(8) . . ? OW8 Ca OW5 76.33(8) . . ? OW6 Ca OW5 83.24(8) . . ? OW1 Ca OW5 145.35(7) . . ? OW3 Ca OW7 72.43(8) . . ? OW8 Ca OW7 75.26(9) . . ? OW6 Ca OW7 124.57(9) . . ? OW1 Ca OW7 75.38(7) . . ? OW5 Ca OW7 137.97(8) . . ? OW3 Ca OW2 80.14(9) . . ? OW8 Ca OW2 147.27(8) . . ? OW6 Ca OW2 81.01(8) . . ? OW1 Ca OW2 74.79(7) . . ? OW5 Ca OW2 72.39(7) . . ? OW7 Ca OW2 136.18(9) . . ? OW3 Ca H7A 62.3(6) . . ? OW8 Ca H7A 69.1(7) . . ? OW6 Ca H7A 136.3(6) . . ? OW1 Ca H7A 90.0(6) . . ? OW5 Ca H7A 122.1(5) . . ? OW7 Ca H7A 16.4(4) . . ? OW2 Ca H7A 137.5(7) . . ? V1 O1 V1 101.66(7) 2_657 . ? V1 O1 V3 93.24(6) 2_657 2_657 ? V1 O1 V3 93.94(6) . 2_657 ? V1 O1 V2 93.47(6) 2_657 . ? V1 O1 V2 92.55(6) . . ? V3 O1 V2 169.54(8) 2_657 . ? V1 O1 V5 170.84(8) 2_657 . ? V1 O1 V5 87.50(6) . . ? V3 O1 V5 86.14(5) 2_657 . ? V2 O1 V5 85.96(5) . . ? V1 O1 V4 87.86(6) 2_657 2_657 ? V1 O1 V4 170.35(8) . 2_657 ? V3 O1 V4 86.99(6) 2_657 2_657 ? V2 O1 V4 85.25(6) . 2_657 ? V5 O1 V4 82.98(5) . 2_657 ? V1 O2 V2 108.22(8) . . ? V1 O2 V3 106.53(7) . . ? V2 O2 V3 100.15(7) . . ? V1 O3 V2 108.41(8) . 2_657 ? V1 O3 V3 107.68(8) . 2_657 ? V2 O3 V3 100.67(7) 2_657 2_657 ? V1 O4 V5 110.28(8) . . ? V3 O5 V4 114.12(9) . . ? V1 O6 V4 110.17(8) . . ? V3 O7 V5 114.71(9) . 2_657 ? V4 O8 V5 113.67(9) 2_657 . ? V2 O9 V4 114.82(9) . 2_657 ? V2 O10 V5 115.17(9) . . ? Ca OW1 H1A 118(2) . . ? Ca OW1 H1B 119(2) . . ? H1A OW1 H1B 103(2) . . ? Ca OW2 H2A 126(2) . . ? Ca OW2 H2B 124(2) . . ? H2A OW2 H2B 107(2) . . ? Ca OW3 H3A 122(2) . . ? Ca OW3 H3B 126(2) . . ? H3A OW3 H3B 107(2) . . ? H4A OW4 H4B 101(3) . . ? Ca OW5 H5A 122(2) . . ? Ca OW5 H5B 119(2) . . ? H5A OW5 H5B 119(3) . . ? Ca OW6 H6A 120(2) . . ? Ca OW6 H6B 123(2) . . ? H6A OW6 H6B 114(3) . . ? Ca OW7 H7A 103(2) . . ? Ca OW7 H7B 129(2) . . ? H7A OW7 H7B 120(3) . . ? Ca OW8 H8A 118(3) . . ? Ca OW8 H8B 117(3) . . ? H8A OW8 H8B 123(3) . . ? HNA N HNB 108(2) . . ? HNA N HNC 109(2) . . ? HNB N HNC 107(2) . . ? HNA N HND 115(2) . . ? HNB N HND 108(2) . . ? HNC N HND 109(2) . . ? 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 O5 0.827(16) 2.072(17) 2.883(3) 167(3) . OW1 H1B O7 0.819(16) 1.893(17) 2.696(3) 167(3) 2_658 OW2 H2A O5 0.818(17) 2.10(2) 2.833(3) 149(3) . OW2 H2A O6 0.818(17) 2.60(2) 3.261(3) 139(2) . OW3 H3A OW1 0.809(17) 2.12(2) 2.901(3) 162(4) 2_758 OW3 H3B O3 0.799(17) 1.859(19) 2.650(3) 170(3) 2_757 OW4 H4A O11 0.847(18) 2.43(3) 3.108(3) 137(3) 2_658 OW4 H4A OW3 0.847(18) 2.32(3) 2.875(4) 124(3) 2_758 OW4 H4B O8 0.859(18) 2.07(2) 2.796(3) 141(3) 2_657 OW5 H5A O9 0.826(17) 1.961(17) 2.784(3) 174(3) 1_655 OW5 H5B O8 0.822(17) 2.13(2) 2.918(3) 161(3) 2_667 OW6 H6A O11 0.842(17) 2.016(17) 2.830(3) 162(3) . OW6 H6B O14 0.838(17) 2.03(2) 2.819(3) 157(3) 2_667 OW7 H7B O4 0.820(17) 2.113(18) 2.912(3) 165(3) 1_556 OW8 H8A O12 0.815(17) 2.17(3) 2.891(3) 148(3) 2_668 OW8 H8B OW4 0.811(17) 1.92(2) 2.711(4) 165(4) 1_565 N HNA O10 0.866(18) 1.934(19) 2.787(3) 168(3) . N HNB O2 0.910(18) 2.020(19) 2.900(3) 162(2) 2_667 N HNC O13 0.902(18) 2.12(2) 2.940(3) 151(2) 1_465 N HND OW2 0.851(18) 2.41(2) 3.035(3) 131(2) 2_667 N HND OW5 0.851(18) 2.41(2) 3.167(4) 148(2) 2_667 _refine_diff_density_max 0.626 _refine_diff_density_min -0.404 _refine_diff_density_rms 0.107 _shelxl_version_number 2013-4 _shelx_res_file ; TITL wernerbaurite CELL 0.71075 9.72115 10.25980 10.59280 89.999 77.083 69.887 ZERR 1 0.00064 0.00076 0.00075 0.006 0.007 0.008 LATT 1 SFAC V CA O H N UNIT 10 2 44 40 2 L.S. 8 omit 2 -1 1 omit 1 -1 5 omit -1 4 0 OMIT 4 4 1 OMIT 2 0 5 omit -2 0 3 omit 4 4 2 omit -3 -1 2 omit 2 -1 4 omit 0 0 2 omit -3 0 3 omit -3 -1 3 omit -3 0 2 omit 0 4 0 omit 1 4 0 omit 3 4 2 omit -2 1 0 HTAB OW1 O5 EQIV $1 -x+1, -y, -z+3 HTAB OW1 O7_$1 HTAB OW2 O5 HTAB OW2 O6 EQIV $2 -x+2, -y, -z+2 EQIV $3 -x+2, -y, -z+3 HTAB OW3 OW1_$3 HTAB OW3 O3_$2 HTAB OW4 O11_$1 HTAB OW4 OW3_$3 EQIV $4 -x+1, -y, -z+2 HTAB OW4 O8_$4 EQIV $5 x+1, y, z HTAB OW5 O9_$5 EQIV $6 -x+1, -y+1, -z+2 HTAB OW5 O8_$6 HTAB OW6 O11 HTAB OW6 O14_$6 EQIV $7 x, y, z+1 HTAB OW7 O4_$7 EQIV $8 -x+1, -y+1, -z+3 HTAB OW8 O12_$8 EQIV $9 x, y+1, z HTAB OW8 OW4_$9 HTAB N O10 HTAB N O2_$6 EQIV $10 x-1, y+1, z HTAB N O13_$10 HTAB N OW2_$6 HTAB N OW5_$6 FMAP 2 PLAN 30 HTAB BOND $H ACTA DFIX 0.82 0.02 OW1 H1A OW1 H1B DFIX 0.82 0.02 OW2 H2A OW2 H2B DFIX 0.82 0.02 OW3 H3A OW3 H3B DFIX 0.82 0.02 OW4 H4A OW4 H4B DFIX 0.82 0.02 OW5 H5A OW5 H5B DFIX 0.82 0.02 OW6 H6A OW6 H6B DFIX 0.82 0.02 OW7 H7A OW7 H7B DFIX 0.82 0.02 OW8 H8A OW8 H8B DFIX 1.3 0.02 H1A H1B H2A H2B H3A H3B H4A H4B DFIX 1.45 0.02 H5A H5B H6A H6B H7A H7B H8A H8B DFIX 0.9 0.03 N HNa N HNb N HNc N HNd DFIX 1.45 0.03 HNa HNb HNa HNc HNa HNd HNb HNc HNb HNd HNc HNd SIZE 0.220 0.220 0.040 WGHT 0.043800 FVAR 0.63752 V1 1 0.654339 0.035619 0.947812 11.00000 0.01917 0.01799 = 0.02000 0.00146 -0.00139 -0.00841 V2 1 0.347814 0.270868 1.093133 11.00000 0.02659 0.01710 = 0.02495 -0.00078 -0.00367 -0.00623 V3 1 0.517920 0.040103 1.247078 11.00000 0.02336 0.02284 = 0.01976 0.00041 -0.00346 -0.00900 V4 1 0.814149 -0.198277 1.103527 11.00000 0.02125 0.02494 = 0.02759 0.00372 -0.00495 -0.00653 V5 1 0.476825 0.261077 0.793930 11.00000 0.02739 0.02154 = 0.02797 0.00769 -0.00449 -0.01019 CA 2 0.839580 0.266002 1.412954 11.00000 0.02671 0.02785 = 0.02930 0.00157 -0.00382 -0.01056 O1 3 0.426454 0.098654 0.931836 11.00000 0.02213 0.01970 = 0.01937 0.00167 -0.00272 -0.00831 O2 3 0.559578 0.158607 1.102342 11.00000 0.02289 0.01982 = 0.02356 -0.00012 -0.00238 -0.00975 O3 3 0.671816 -0.104422 0.817948 11.00000 0.02092 0.02187 = 0.02105 0.00060 -0.00130 -0.00792 O4 3 0.675601 0.157830 0.845411 11.00000 0.02573 0.02303 = 0.02690 0.00433 -0.00274 -0.01229 O5 3 0.719219 -0.044468 1.232571 11.00000 0.02490 0.02926 = 0.02362 0.00187 -0.00553 -0.01074 O6 3 0.824047 -0.044123 0.981965 11.00000 0.02146 0.02682 = 0.02693 0.00204 -0.00205 -0.00935 O7 3 0.466375 -0.102524 1.319278 11.00000 0.02805 0.02660 = 0.02075 0.00469 -0.00242 -0.01035 O8 3 0.276303 0.304038 0.793983 11.00000 0.02785 0.02411 = 0.02983 0.00675 -0.00630 -0.00682 O9 3 0.169279 0.299393 1.047874 11.00000 0.02321 0.02275 = 0.02862 -0.00036 -0.00139 -0.00418 O10 3 0.424370 0.356481 0.958610 11.00000 0.03108 0.01964 = 0.03136 0.00416 -0.00467 -0.01059 O11 3 0.465373 0.153885 1.369451 11.00000 0.03367 0.03302 = 0.02556 -0.00483 -0.00400 -0.01104 O12 3 0.299874 0.383823 1.215022 11.00000 0.04123 0.02738 = 0.03613 -0.00705 -0.00555 -0.00828 O13 3 0.983330 -0.252297 1.121210 11.00000 0.02608 0.04024 = 0.03778 0.00119 -0.00574 -0.00571 O14 3 0.528725 0.366120 0.699786 11.00000 0.04277 0.03381 = 0.04163 0.01728 -0.01083 -0.01841 OW1 3 0.754806 0.072546 1.465445 11.00000 0.03290 0.03557 = 0.02531 0.00167 -0.00064 -0.01701 H1A 4 0.741033 0.029582 1.406265 11.00000 -1.20000 H1B 4 0.678432 0.085569 1.523011 11.00000 -1.20000 OW2 3 0.888392 0.134683 1.202055 11.00000 0.03748 0.03889 = 0.03814 -0.00835 0.00643 -0.02068 H2A 4 0.836087 0.093737 1.182861 11.00000 -1.20000 H2B 4 0.969690 0.102505 1.153357 11.00000 -1.20000 OW3 3 1.095400 0.142135 1.382292 11.00000 0.02911 0.06561 = 0.03899 0.01930 0.00286 -0.00485 H3A 4 1.126973 0.072205 1.418242 11.00000 -1.20000 H3B 4 1.158661 0.138125 1.318038 11.00000 -1.20000 OW4 3 0.836710 -0.291362 1.424579 11.00000 0.09830 0.08596 = 0.04727 0.01404 -0.02755 -0.05538 H4A 4 0.790906 -0.242974 1.496265 11.00000 -1.20000 H4B 4 0.769296 -0.262004 1.380553 11.00000 -1.20000 OW5 3 0.903131 0.410535 1.239922 11.00000 0.04204 0.02620 = 0.04495 0.00263 0.01035 -0.00939 H5A 4 0.978301 0.378676 1.179024 11.00000 -1.20000 H5B 4 0.855092 0.494619 1.247332 11.00000 -1.20000 OW6 3 0.595712 0.361358 1.372213 11.00000 0.03458 0.02841 = 0.07841 0.01206 -0.01909 -0.01152 H6A 4 0.539794 0.313366 1.380302 11.00000 -1.20000 H6B 4 0.549534 0.447177 1.373710 11.00000 -1.20000 OW7 3 0.889366 0.208992 1.628744 11.00000 0.04399 0.08753 = 0.03341 0.01073 -0.00853 -0.03638 H7A 4 0.959857 0.233073 1.629481 11.00000 -1.20000 H7B 4 0.829924 0.207957 1.696868 11.00000 -1.20000 OW8 3 0.783575 0.482662 1.524914 11.00000 0.11348 0.04695 = 0.03606 -0.00574 -0.00291 -0.03821 H8A 4 0.763480 0.488102 1.604125 11.00000 -1.20000 H8B 4 0.805619 0.541474 1.482449 11.00000 -1.20000 N 5 0.287338 0.642278 0.948089 11.00000 0.03190 0.02461 = 0.04595 0.00209 -0.00964 -0.00933 HNA 4 0.338850 0.556710 0.957270 11.00000 -1.20000 HNB 4 0.349497 0.692316 0.941167 11.00000 -1.20000 HNC 4 0.213623 0.677617 1.020853 11.00000 -1.20000 HND 4 0.248548 0.654156 0.882616 11.00000 -1.20000 HKLF 4 REM wernerbaurite REM R1 = 0.0326 for 3434 Fo > 4sig(Fo) and 0.0456 for all 4389 data REM 322 parameters refined using 34 restraints END WGHT 0.0439 0.0000 REM Instructions for potential hydrogen bonds HTAB OW1 O5 HTAB OW1 O7_$1 HTAB OW2 O5 HTAB OW2 O6 HTAB OW2 O6_$2 HTAB OW3 OW1_$3 HTAB OW3 O3_$2 HTAB OW4 O11_$1 HTAB OW4 OW3_$3 HTAB OW4 O8_$4 HTAB OW5 O9_$5 HTAB OW5 O8_$6 HTAB OW6 O11 HTAB OW6 O14_$6 HTAB OW7 O4_$7 HTAB OW8 O12_$8 HTAB OW8 OW4_$9 HTAB N O10 HTAB N O2_$6 HTAB N O4_$6 HTAB N O10_$6 HTAB N O13_$10 HTAB N OW2_$6 HTAB N OW5_$6 REM Highest difference peak 0.626, deepest hole -0.404, 1-sigma level 0.107 Q1 1 0.6188 0.0043 1.2377 11.00000 0.05 0.63 Q2 1 0.1743 0.4983 0.9426 11.00000 0.05 0.62 Q3 1 0.6735 -0.1910 1.3959 11.00000 0.05 0.53 Q4 1 0.5391 -0.0590 1.2861 11.00000 0.05 0.45 Q5 1 0.9135 -0.2209 1.1013 11.00000 0.05 0.43 Q6 1 0.7424 -0.0227 0.9582 11.00000 0.05 0.43 Q7 1 0.5282 0.1027 1.2895 11.00000 0.05 0.43 Q8 1 0.2697 0.3379 0.8206 11.00000 0.05 0.42 Q9 1 0.3890 0.3215 1.1689 11.00000 0.05 0.40 Q10 1 0.6448 0.0100 0.9379 11.00000 0.05 0.40 Q11 1 0.8635 0.3167 1.4126 11.00000 0.05 0.40 Q12 1 0.4817 -0.0344 1.2610 11.00000 0.05 0.39 Q13 1 0.8380 -0.2617 1.0320 11.00000 0.05 0.39 Q14 1 0.4480 0.2193 1.0966 11.00000 0.05 0.38 Q15 1 0.8684 0.2311 1.3617 11.00000 0.05 0.38 Q16 1 0.5097 -0.0242 1.1673 11.00000 0.05 0.38 Q17 1 0.7616 0.1276 1.4996 11.00000 0.05 0.37 Q18 1 0.4403 0.1697 1.3986 11.00000 0.05 0.37 Q19 1 0.9926 0.1729 1.3860 11.00000 0.05 0.37 Q20 1 0.7758 0.2789 1.4220 11.00000 0.05 0.36 Q21 1 0.9553 0.1901 1.6655 11.00000 0.05 0.35 Q22 1 0.9710 0.5770 1.2526 11.00000 0.05 0.35 Q23 1 0.9580 0.3712 1.2952 11.00000 0.05 0.34 Q24 1 1.0026 -0.2348 1.1281 11.00000 0.05 0.34 Q25 1 1.0046 0.0414 1.5647 11.00000 0.05 0.33 Q26 1 0.2471 0.3001 1.0852 11.00000 0.05 0.33 Q27 1 0.9344 -0.2938 1.0828 11.00000 0.05 0.33 Q28 1 0.5455 0.0836 0.9489 11.00000 0.05 0.33 Q29 1 0.4663 0.2071 0.8524 11.00000 0.05 0.33 Q30 1 0.5750 0.1840 1.0977 11.00000 0.05 0.33 ; _shelx_res_checksum 97132 _shelx_hkl_file ; 0 1 1 2614.92 48.38 0 1 1 2446.05 44.62 0 -1 -1 2402.75 49.27 0 -1 -1 2468.35 43.02 0 1 1 2371.36 45.36 0 -1 -1 2578.89 47.39 -1 0 1 5215.53 139.81 1 0 -1 5205.20 140.08 1 0 -1 5601.52 136.44 1 0 -1 5773.58 116.28 1 1 -1 2998.09 66.92 -1 -1 1 3038.78 61.86 -1 -1 1 2915.46 60.75 -1 -1 1 2882.13 55.79 1 1 -1 2961.20 60.41 1 1 -1 3035.41 62.00 1 -1 0 39.51 3.90 1 -1 0 43.23 2.36 -1 1 0 39.23 2.28 -1 1 0 38.16 1.97 1 -1 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435.92 40.68 -4 7 -4 443.69 23.79 -2 3 -10 26.23 7.04 -2 3 -10 34.16 14.07 2 -3 10 15.00 3.58 7 -2 -3 41.97 15.11 7 -2 -3 37.40 9.66 7 -2 -3 31.51 16.53 7 -2 -3 41.36 10.18 -3 7 3 55.67 9.44 3 -7 -3 61.94 16.11 3 -7 -3 49.43 17.16 3 -7 -3 54.16 8.43 -3 8 -1 15.45 6.36 -3 8 -1 5.77 6.39 -3 8 -1 -6.71 4.94 3 -8 1 -0.05 6.00 3 -8 1 0.55 4.30 3 -8 1 -2.85 4.49 5 1 10 172.43 9.14 -5 -1 -10 166.82 11.24 -5 -1 -10 167.50 10.10 5 1 10 164.31 8.50 -6 -8 -6 383.54 44.77 6 8 6 381.46 31.64 -6 -8 -6 387.09 23.12 -6 -8 -6 453.54 31.59 6 8 6 422.50 21.40 6 8 6 374.64 34.25 5 10 0 54.71 17.99 5 10 0 38.49 20.07 -5 -10 0 45.61 17.78 -5 -10 0 45.61 11.70 5 10 0 37.29 17.28 -5 -10 0 68.44 12.80 -4 -3 -10 15.36 10.10 -4 -3 -10 13.19 14.08 -4 -3 -10 14.27 5.04 -5 -5 -9 1078.69 38.97 -5 -5 -9 1052.23 40.66 5 5 9 1059.00 43.18 -5 -5 -9 1138.02 57.28 5 10 1 81.84 19.04 5 10 1 54.15 14.58 -5 -10 -1 63.57 13.95 -5 -10 -1 50.31 12.83 5 10 1 72.71 18.96 -5 -10 -1 76.96 18.92 -1 9 -3 45.37 9.03 1 -9 3 57.57 18.92 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