data_tapiaite _audit_creation_method SHELXL-2013 _chemical_name_mineral 'tapiaite' _chemical_compound_source 'Jote mine, Chile' _chemical_formula_sum 'H56 Al4 As8 Ca10 O64' _chemical_formula_weight 2188.52 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'As' 'As' 0.0499 2.0058 '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' 'Al' 'Al' 0.0645 0.0514 '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' _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_H-M_alt 'P 21/n' _space_group_name_Hall '-P 2yn' _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+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 16.0160(12) _cell_length_b 5.7781(3) _cell_length_c 16.3410(12) _cell_angle_alpha 90 _cell_angle_beta 116.704(8) _cell_angle_gamma 90 _cell_volume 1350.93(18) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _exptl_crystal_density_diffrn 2.690 _exptl_crystal_F_000 1084 _exptl_crystal_size_max 0.070 _exptl_crystal_size_mid 0.030 _exptl_crystal_size_min 0.010 _exptl_absorpt_coefficient_mu 6.047 _shelx_estimated_absorpt_T_min 0.677 _shelx_estimated_absorpt_T_max 0.942 _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 10063 _diffrn_reflns_av_unetI/netI 0.0749 _diffrn_reflns_av_R_equivalents 0.0867 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.769 _diffrn_reflns_theta_max 25.018 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 0.987 _diffrn_measured_fraction_theta_full 0.966 _diffrn_reflns_Laue_measured_fraction_max 0.987 _diffrn_reflns_Laue_measured_fraction_full 0.966 _diffrn_reflns_point_group_measured_fraction_max 0.987 _diffrn_reflns_point_group_measured_fraction_full 0.966 _reflns_number_total 2357 _reflns_number_gt 1733 _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^)+(0.0789P)^2^+0.4203P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens . _refine_ls_hydrogen_treatment undef _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 2357 _refine_ls_number_parameters 198 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0784 _refine_ls_R_factor_gt 0.0537 _refine_ls_wR_factor_ref 0.1420 _refine_ls_wR_factor_gt 0.1253 _refine_ls_goodness_of_fit_ref 1.047 _refine_ls_restrained_S_all 1.047 _refine_ls_shift/su_max 0.001 _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 Ca1 Ca 0.5000 0.5000 0.0000 0.0209(6) Uani 1 2 d S . P . . Ca2 Ca 0.47839(11) 0.1855(3) 0.33149(12) 0.0187(5) Uani 1 1 d . . . . . Ca3 Ca 0.32828(11) 0.3149(3) 0.47120(12) 0.0188(5) Uani 1 1 d . . . . . Al Al 0.74473(16) 0.4993(3) 0.75492(16) 0.0131(6) Uani 1 1 d . . . . . As1 As 0.57805(6) 0.24950(12) 0.57888(6) 0.0135(3) Uani 0.967(5) 1 d . . P . . As2 As 0.41220(6) 0.99716(13) 0.09523(6) 0.0149(3) Uani 0.972(5) 1 d . . P . . O1 O 0.4764(4) 0.1762(9) 0.5750(4) 0.0188(13) Uani 1 1 d . . . . . O2 O 0.5762(4) 0.3224(9) 0.4798(4) 0.0199(13) Uani 1 1 d . . . . . O3 O 0.6282(4) 0.4860(8) 0.6444(4) 0.0168(12) Uani 1 1 d . . . . . O4 O 0.6446(4) 0.0114(8) 0.6299(4) 0.0161(12) Uani 1 1 d . . . . . O5 O 0.4156(4) 0.7683(9) 0.0344(4) 0.0261(15) Uani 1 1 d . . . . . O6 O 0.4776(4) 0.2168(9) 0.0892(4) 0.0267(14) Uani 1 1 d . . . . . O7 O 0.2998(4) 0.0821(8) 0.0575(4) 0.0218(13) Uani 1 1 d . . . . . O8 O 0.4500(4) 0.9225(8) 0.2067(4) 0.0186(13) Uani 1 1 d . . . . . OH9 O 0.3045(4) 0.2357(8) 0.2162(4) 0.0186(13) Uani 1 1 d . . . . . OH10 O 0.2139(4) 0.2656(8) 0.3027(4) 0.0158(12) Uani 1 1 d . . . . . OW11 O 0.4958(5) 0.4791(9) 0.2378(4) 0.0302(15) Uani 1 1 d . . . . . OW12 O 0.6357(4) 0.1245(10) 0.3388(5) 0.0332(16) Uani 1 1 d . . . . . OW13 O 0.6394(5) 0.5986(11) 0.1367(5) 0.0423(18) Uani 1 1 d . . . . . OW14 O 0.2365(4) 0.0218(9) 0.4928(5) 0.0263(15) Uani 1 1 d . . . . . OW15 O 0.6780(5) 0.6029(10) 0.3769(5) 0.0365(17) Uani 1 1 d . . . . . OW16 O 0.8347(5) 0.5687(12) 0.3282(5) 0.0455(19) 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 Ca1 0.0262(14) 0.0181(12) 0.0232(15) 0.0017(10) 0.0154(12) 0.0017(9) Ca2 0.0196(9) 0.0185(9) 0.0163(10) -0.0012(7) 0.0066(8) -0.0022(6) Ca3 0.0165(9) 0.0199(9) 0.0195(10) 0.0026(7) 0.0076(8) 0.0003(7) Al 0.0156(13) 0.0097(11) 0.0135(14) -0.0007(9) 0.0059(11) 0.0003(8) As1 0.0135(5) 0.0114(5) 0.0134(5) 0.0003(3) 0.0039(4) -0.0006(3) As2 0.0169(5) 0.0130(5) 0.0171(5) -0.0001(3) 0.0098(4) 0.0002(3) O1 0.016(3) 0.017(3) 0.027(4) 0.001(2) 0.012(3) -0.001(2) O2 0.028(3) 0.021(3) 0.013(3) 0.004(2) 0.012(3) 0.006(2) O3 0.017(3) 0.012(3) 0.017(3) 0.006(2) 0.004(3) 0.005(2) O4 0.018(3) 0.013(3) 0.017(3) -0.005(2) 0.009(3) -0.003(2) O5 0.030(4) 0.020(3) 0.034(4) -0.008(2) 0.020(3) 0.003(2) O6 0.030(4) 0.025(3) 0.031(4) 0.002(3) 0.019(3) -0.006(2) O7 0.024(3) 0.013(3) 0.028(4) -0.001(2) 0.012(3) -0.003(2) O8 0.022(3) 0.014(3) 0.018(3) 0.000(2) 0.008(3) -0.001(2) OH9 0.020(3) 0.018(3) 0.018(3) 0.000(2) 0.008(3) 0.002(2) OH10 0.016(3) 0.019(3) 0.011(3) -0.003(2) 0.004(3) -0.002(2) OW11 0.042(4) 0.024(3) 0.030(4) 0.006(3) 0.020(3) 0.004(3) OW12 0.031(4) 0.031(4) 0.033(4) 0.004(3) 0.010(3) 0.006(3) OW13 0.041(4) 0.040(4) 0.036(5) -0.001(3) 0.009(4) -0.004(3) OW14 0.024(3) 0.018(3) 0.038(4) 0.000(3) 0.016(3) -0.007(2) OW15 0.048(4) 0.034(4) 0.033(4) -0.008(3) 0.024(4) -0.011(3) OW16 0.045(5) 0.042(4) 0.040(5) -0.002(3) 0.011(4) -0.006(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 Ca1 O5 2.286(5) . ? Ca1 O5 2.286(5) 3_665 ? Ca1 O6 2.324(5) 3_665 ? Ca1 O6 2.324(5) . ? Ca1 OW13 2.412(7) 3_665 ? Ca1 OW13 2.412(7) . ? Ca2 O2 2.354(6) . ? Ca2 OW11 2.383(6) . ? Ca2 O8 2.417(6) 1_545 ? Ca2 OW12 2.493(6) . ? Ca2 O1 2.497(5) 3_656 ? Ca2 OH9 2.584(6) . ? Ca2 O4 2.586(5) 3_656 ? Ca2 O3 2.698(5) 3_666 ? Ca2 As1 3.2358(18) 3_656 ? Ca2 Al 3.536(3) 4_565 ? Ca2 As1 3.637(2) . ? Ca2 As2 3.6791(19) 1_545 ? Ca3 O1 2.351(6) . ? Ca3 OW14 2.370(6) . ? Ca3 O7 2.439(5) 2 ? Ca3 O2 2.504(6) 3_666 ? Ca3 OH10 2.547(6) . ? Ca3 O3 2.561(5) 3_666 ? Ca3 OW15 2.573(7) 3_666 ? Ca3 O4 2.669(5) 3_656 ? Ca3 As1 3.2185(18) 3_666 ? Ca3 Al 3.506(3) 3_666 ? Ca3 As1 3.5938(19) . ? Ca3 Al 3.651(3) 4_565 ? Al OH9 1.877(5) 3_666 ? Al OH10 1.882(5) 4_666 ? Al O4 1.921(6) 2_656 ? Al OH9 1.925(6) 4_666 ? Al O3 1.929(6) . ? Al OH10 1.932(6) 3_666 ? Al Al 2.9026(5) 2_656 ? Al Al 2.9027(5) 2_646 ? Al Ca3 3.506(3) 3_666 ? Al Ca2 3.536(3) 4_666 ? Al Ca3 3.651(3) 4_666 ? Al Ca2 3.680(3) 3_666 ? As1 O1 1.656(5) . ? As1 O2 1.661(5) . ? As1 O3 1.699(5) . ? As1 O4 1.710(5) . ? As1 Ca3 3.2185(18) 3_666 ? As1 Ca2 3.2359(18) 3_656 ? As2 O5 1.670(5) . ? As2 O6 1.677(5) 1_565 ? As2 O7 1.692(5) 1_565 ? As2 O8 1.697(6) . ? As2 Ca3 3.6556(18) 2 ? As2 Ca2 3.6790(19) 1_565 ? O1 Ca2 2.497(5) 3_656 ? O2 Ca3 2.504(6) 3_666 ? O3 Ca3 2.561(5) 3_666 ? O3 Ca2 2.698(5) 3_666 ? O4 Al 1.921(6) 2_646 ? O4 Ca2 2.586(5) 3_656 ? O4 Ca3 2.669(5) 3_656 ? O6 As2 1.677(5) 1_545 ? O6 OW11 2.765(9) . ? O7 As2 1.692(5) 1_545 ? O7 Ca3 2.439(5) 2_545 ? O7 OH9 2.711(8) . ? O8 Ca2 2.417(6) 1_565 ? O8 OW11 2.651(7) . ? OH9 Al 1.877(5) 3_666 ? OH9 Al 1.925(6) 4_565 ? OH10 Al 1.882(5) 4_565 ? OH10 Al 1.932(6) 3_666 ? OH10 O8 2.715(7) 2_545 ? OW11 OW15 2.869(9) . ? OW12 OW14 2.723(9) 3_656 ? OW12 OW15 2.847(8) . ? OW13 OW16 2.769(9) 2_655 ? OW13 OW16 3.108(9) 2_645 ? OW14 O7 2.653(7) 2_545 ? OW14 O5 2.682(8) 2_545 ? OW15 Ca3 2.573(7) 3_666 ? OW15 OW16 2.960(10) . ? OW16 O6 2.819(9) 2_655 ? OW16 OW12 2.990(10) 2_655 ? 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 O5 Ca1 O5 180.0 . 3_665 ? O5 Ca1 O6 87.2(2) . 3_665 ? O5 Ca1 O6 92.8(2) 3_665 3_665 ? O5 Ca1 O6 92.8(2) . . ? O5 Ca1 O6 87.2(2) 3_665 . ? O6 Ca1 O6 180.0 3_665 . ? O5 Ca1 OW13 89.1(2) . 3_665 ? O5 Ca1 OW13 90.9(2) 3_665 3_665 ? O6 Ca1 OW13 85.7(2) 3_665 3_665 ? O6 Ca1 OW13 94.3(2) . 3_665 ? O5 Ca1 OW13 90.9(2) . . ? O5 Ca1 OW13 89.1(2) 3_665 . ? O6 Ca1 OW13 94.3(2) 3_665 . ? O6 Ca1 OW13 85.7(2) . . ? OW13 Ca1 OW13 180.0 3_665 . ? O2 Ca2 OW11 101.9(2) . . ? O2 Ca2 O8 149.98(19) . 1_545 ? OW11 Ca2 O8 86.4(2) . 1_545 ? O2 Ca2 OW12 78.9(2) . . ? OW11 Ca2 OW12 74.0(2) . . ? O8 Ca2 OW12 75.8(2) 1_545 . ? O2 Ca2 O1 77.02(19) . 3_656 ? OW11 Ca2 O1 154.6(2) . 3_656 ? O8 Ca2 O1 83.27(18) 1_545 3_656 ? OW12 Ca2 O1 80.99(19) . 3_656 ? O2 Ca2 OH9 135.54(19) . . ? OW11 Ca2 OH9 81.4(2) . . ? O8 Ca2 OH9 73.90(18) 1_545 . ? OW12 Ca2 OH9 141.8(2) . . ? O1 Ca2 OH9 117.49(18) 3_656 . ? O2 Ca2 O4 97.14(19) . 3_656 ? OW11 Ca2 O4 142.3(2) . 3_656 ? O8 Ca2 O4 93.08(18) 1_545 3_656 ? OW12 Ca2 O4 142.20(19) . 3_656 ? O1 Ca2 O4 61.69(17) 3_656 3_656 ? OH9 Ca2 O4 62.46(18) . 3_656 ? O2 Ca2 O3 77.59(18) . 3_666 ? OW11 Ca2 O3 81.81(18) . 3_666 ? O8 Ca2 O3 132.39(19) 1_545 3_666 ? OW12 Ca2 O3 141.71(18) . 3_666 ? O1 Ca2 O3 121.87(17) 3_656 3_666 ? OH9 Ca2 O3 58.80(17) . 3_666 ? O4 Ca2 O3 70.88(16) 3_656 3_666 ? O2 Ca2 As1 89.26(14) . 3_656 ? OW11 Ca2 As1 168.68(17) . 3_656 ? O8 Ca2 As1 84.75(13) 1_545 3_656 ? OW12 Ca2 As1 110.51(15) . 3_656 ? O1 Ca2 As1 30.23(12) 3_656 3_656 ? OH9 Ca2 As1 89.33(12) . 3_656 ? O4 Ca2 As1 31.74(12) 3_656 3_656 ? O3 Ca2 As1 98.99(12) 3_666 3_656 ? O2 Ca2 Al 125.08(15) . 4_565 ? OW11 Ca2 Al 113.47(17) . 4_565 ? O8 Ca2 Al 75.14(14) 1_545 4_565 ? OW12 Ca2 Al 149.34(16) . 4_565 ? O1 Ca2 Al 86.20(13) 3_656 4_565 ? OH9 Ca2 Al 32.13(12) . 4_565 ? O4 Ca2 Al 32.05(13) 3_656 4_565 ? O3 Ca2 Al 68.00(12) 3_666 4_565 ? As1 Ca2 Al 57.25(5) 3_656 4_565 ? O2 Ca2 As1 20.75(13) . . ? OW11 Ca2 As1 121.46(17) . . ? O8 Ca2 As1 145.48(14) 1_545 . ? OW12 Ca2 As1 91.84(16) . . ? O1 Ca2 As1 62.81(13) 3_656 . ? OH9 Ca2 As1 126.16(14) . . ? O4 Ca2 As1 77.04(13) 3_656 . ? O3 Ca2 As1 75.90(13) 3_666 . ? As1 Ca2 As1 69.40(4) 3_656 . ? Al Ca2 As1 106.86(6) 4_565 . ? O2 Ca2 As2 157.58(15) . 1_545 ? OW11 Ca2 As2 66.32(16) . 1_545 ? O8 Ca2 As2 21.93(12) 1_545 1_545 ? OW12 Ca2 As2 79.43(16) . 1_545 ? O1 Ca2 As2 105.20(14) 3_656 1_545 ? OH9 Ca2 As2 63.90(13) . 1_545 ? O4 Ca2 As2 103.52(13) 3_656 1_545 ? O3 Ca2 As2 117.31(13) 3_666 1_545 ? As1 Ca2 As2 103.76(5) 3_656 1_545 ? Al Ca2 As2 77.25(5) 4_565 1_545 ? As1 Ca2 As2 166.42(5) . 1_545 ? O1 Ca3 OW14 98.1(2) . . ? O1 Ca3 O7 147.5(2) . 2 ? OW14 Ca3 O7 87.51(19) . 2 ? O1 Ca3 O2 77.37(18) . 3_666 ? OW14 Ca3 O2 151.7(2) . 3_666 ? O7 Ca3 O2 82.65(18) 2 3_666 ? O1 Ca3 OH10 138.1(2) . . ? OW14 Ca3 OH10 83.6(2) . . ? O7 Ca3 OH10 74.28(18) 2 . ? O2 Ca3 OH10 118.60(18) 3_666 . ? O1 Ca3 O3 99.48(19) . 3_666 ? OW14 Ca3 O3 145.4(2) . 3_666 ? O7 Ca3 O3 93.34(18) 2 3_666 ? O2 Ca3 O3 62.00(17) 3_666 3_666 ? OH10 Ca3 O3 63.55(18) . 3_666 ? O1 Ca3 OW15 80.3(2) . 3_666 ? OW14 Ca3 OW15 72.1(2) . 3_666 ? O7 Ca3 OW15 71.0(2) 2 3_666 ? O2 Ca3 OW15 79.63(19) 3_666 3_666 ? OH10 Ca3 OW15 138.0(2) . 3_666 ? O3 Ca3 OW15 140.35(19) 3_666 3_666 ? O1 Ca3 O4 79.25(18) . 3_656 ? OW14 Ca3 O4 82.63(19) . 3_656 ? O7 Ca3 O4 133.3(2) 2 3_656 ? O2 Ca3 O4 122.89(17) 3_666 3_656 ? OH10 Ca3 O4 59.30(17) . 3_656 ? O3 Ca3 O4 71.74(16) 3_666 3_656 ? OW15 Ca3 O4 144.65(19) 3_666 3_656 ? O1 Ca3 As1 90.90(13) . 3_666 ? OW14 Ca3 As1 170.98(16) . 3_666 ? O7 Ca3 As1 84.50(13) 2 3_666 ? O2 Ca3 As1 30.62(12) 3_666 3_666 ? OH10 Ca3 As1 90.20(12) . 3_666 ? O3 Ca3 As1 31.66(12) 3_666 3_666 ? OW15 Ca3 As1 109.00(14) 3_666 3_666 ? O4 Ca3 As1 99.83(12) 3_656 3_666 ? O1 Ca3 Al 127.97(15) . 3_666 ? OW14 Ca3 Al 116.12(17) . 3_666 ? O7 Ca3 Al 75.55(15) 2 3_666 ? O2 Ca3 Al 86.98(13) 3_666 3_666 ? OH10 Ca3 Al 32.59(12) . 3_666 ? O3 Ca3 Al 32.60(13) 3_666 3_666 ? OW15 Ca3 Al 145.21(17) 3_666 3_666 ? O4 Ca3 Al 68.50(13) 3_656 3_666 ? As1 Ca3 Al 57.68(5) 3_666 3_666 ? O1 Ca3 As1 21.72(13) . . ? OW14 Ca3 As1 118.69(16) . . ? O7 Ca3 As1 144.67(14) 2 . ? O2 Ca3 As1 62.98(13) 3_666 . ? OH10 Ca3 As1 128.25(14) . . ? O3 Ca3 As1 78.26(13) 3_666 . ? OW15 Ca3 As1 93.69(16) 3_666 . ? O4 Ca3 As1 76.91(12) 3_656 . ? As1 Ca3 As1 70.32(4) 3_666 . ? Al Ca3 As1 108.60(6) 3_666 . ? O1 Ca3 Al 109.93(15) . 4_565 ? OW14 Ca3 Al 78.85(17) . 4_565 ? O7 Ca3 Al 102.60(15) 2 4_565 ? O2 Ca3 Al 129.14(14) 3_666 4_565 ? OH10 Ca3 Al 28.95(12) . 4_565 ? O3 Ca3 Al 67.19(13) 3_666 4_565 ? OW15 Ca3 Al 150.40(15) 3_666 4_565 ? O4 Ca3 Al 30.67(13) 3_656 4_565 ? As1 Ca3 Al 98.78(6) 3_666 4_565 ? Al Ca3 Al 47.80(3) 3_666 4_565 ? As1 Ca3 Al 105.35(6) . 4_565 ? OH9 Al OH10 109.9(3) 3_666 4_666 ? OH9 Al O4 91.8(2) 3_666 2_656 ? OH10 Al O4 85.5(2) 4_666 2_656 ? OH9 Al OH9 170.2(2) 3_666 4_666 ? OH10 Al OH9 79.9(2) 4_666 4_666 ? O4 Al OH9 88.4(2) 2_656 4_666 ? OH9 Al O3 86.0(2) 3_666 . ? OH10 Al O3 91.9(2) 4_666 . ? O4 Al O3 175.7(3) 2_656 . ? OH9 Al O3 94.5(2) 4_666 . ? OH9 Al OH10 79.8(2) 3_666 3_666 ? OH10 Al OH10 170.2(2) 4_666 3_666 ? O4 Al OH10 94.8(2) 2_656 3_666 ? OH9 Al OH10 90.3(2) 4_666 3_666 ? O3 Al OH10 88.3(2) . 3_666 ? OH9 Al Al 40.84(17) 3_666 2_656 ? OH10 Al Al 149.9(2) 4_666 2_656 ? O4 Al Al 88.11(18) 2_656 2_656 ? OH9 Al Al 129.4(2) 4_666 2_656 ? O3 Al Al 92.50(18) . 2_656 ? OH10 Al Al 39.81(16) 3_666 2_656 ? OH9 Al Al 150.2(2) 3_666 2_646 ? OH10 Al Al 41.08(17) 4_666 2_646 ? O4 Al Al 92.25(18) 2_656 2_646 ? OH9 Al Al 39.62(16) 4_666 2_646 ? O3 Al Al 87.96(18) . 2_646 ? OH10 Al Al 129.2(2) 3_666 2_646 ? Al Al Al 168.90(18) 2_656 2_646 ? OH9 Al Ca3 92.10(19) 3_666 3_666 ? OH10 Al Ca3 131.37(19) 4_666 3_666 ? O4 Al Ca3 138.17(18) 2_656 3_666 ? OH9 Al Ca3 81.31(18) 4_666 3_666 ? O3 Al Ca3 45.65(16) . 3_666 ? OH10 Al Ca3 45.24(16) 3_666 3_666 ? Al Al Ca3 68.72(9) 2_656 3_666 ? Al Al Ca3 104.27(11) 2_646 3_666 ? OH9 Al Ca2 130.89(19) 3_666 4_666 ? OH10 Al Ca2 92.33(18) 4_666 4_666 ? O4 Al Ca2 45.59(16) 2_656 4_666 ? OH9 Al Ca2 45.56(17) 4_666 4_666 ? O3 Al Ca2 138.05(18) . 4_666 ? OH10 Al Ca2 81.07(17) 3_666 4_666 ? Al Al Ca2 103.98(11) 2_656 4_666 ? Al Al Ca2 68.92(9) 2_646 4_666 ? Ca3 Al Ca2 105.32(7) 3_666 4_666 ? OH9 Al Ca3 100.06(19) 3_666 4_666 ? OH10 Al Ca3 40.91(17) 4_666 4_666 ? O4 Al Ca3 45.12(16) 2_656 4_666 ? OH9 Al Ca3 86.99(18) 4_666 4_666 ? O3 Al Ca3 131.79(18) . 4_666 ? OH10 Al Ca3 139.90(19) 3_666 4_666 ? Al Al Ca3 122.92(12) 2_656 4_666 ? Al Al Ca3 63.48(8) 2_646 4_666 ? Ca3 Al Ca3 167.48(8) 3_666 4_666 ? Ca2 Al Ca3 68.78(6) 4_666 4_666 ? OH9 Al Ca2 41.23(18) 3_666 3_666 ? OH10 Al Ca2 99.86(18) 4_666 3_666 ? O4 Al Ca2 131.87(18) 2_656 3_666 ? OH9 Al Ca2 139.76(19) 4_666 3_666 ? O3 Al Ca2 45.31(16) . 3_666 ? OH10 Al Ca2 87.22(17) 3_666 3_666 ? Al Al Ca2 63.70(8) 2_656 3_666 ? Al Al Ca2 122.81(11) 2_646 3_666 ? Ca3 Al Ca2 68.76(6) 3_666 3_666 ? Ca2 Al Ca2 167.42(8) 4_666 3_666 ? Ca3 Al Ca2 119.20(7) 4_666 3_666 ? O1 As1 O2 116.2(3) . . ? O1 As1 O3 114.1(3) . . ? O2 As1 O3 101.9(3) . . ? O1 As1 O4 101.5(3) . . ? O2 As1 O4 114.5(3) . . ? O3 As1 O4 109.0(3) . . ? O1 As1 Ca3 138.85(19) . 3_666 ? O2 As1 Ca3 50.19(19) . 3_666 ? O3 As1 Ca3 52.29(18) . 3_666 ? O4 As1 Ca3 119.59(18) . 3_666 ? O1 As1 Ca2 49.36(19) . 3_656 ? O2 As1 Ca2 138.79(19) . 3_656 ? O3 As1 Ca2 119.29(18) . 3_656 ? O4 As1 Ca2 52.68(18) . 3_656 ? Ca3 As1 Ca2 168.38(5) 3_666 3_656 ? O1 As1 Ca3 31.69(19) . . ? O2 As1 Ca3 88.1(2) . . ? O3 As1 Ca3 109.35(18) . . ? O4 As1 Ca3 129.47(17) . . ? Ca3 As1 Ca3 109.68(4) 3_666 . ? Ca2 As1 Ca3 80.06(4) 3_656 . ? O1 As1 Ca2 89.9(2) . . ? O2 As1 Ca2 30.1(2) . . ? O3 As1 Ca2 128.98(18) . . ? O4 As1 Ca2 109.05(18) . . ? Ca3 As1 Ca2 79.56(4) 3_666 . ? Ca2 As1 Ca2 110.60(4) 3_656 . ? Ca3 As1 Ca2 68.32(4) . . ? O5 As2 O6 112.1(3) . 1_565 ? O5 As2 O7 109.1(3) . 1_565 ? O6 As2 O7 110.5(3) 1_565 1_565 ? O5 As2 O8 110.3(3) . . ? O6 As2 O8 109.0(3) 1_565 . ? O7 As2 O8 105.9(3) 1_565 . ? O5 As2 Ca3 84.7(2) . 2 ? O6 As2 Ca3 143.5(2) 1_565 2 ? O7 As2 Ca3 33.81(17) 1_565 2 ? O8 As2 Ca3 93.75(18) . 2 ? O5 As2 Ca2 142.0(2) . 1_565 ? O6 As2 Ca2 86.8(2) 1_565 1_565 ? O7 As2 Ca2 93.1(2) 1_565 1_565 ? O8 As2 Ca2 32.13(17) . 1_565 ? Ca3 As2 Ca2 99.51(4) 2 1_565 ? As1 O1 Ca3 126.6(3) . . ? As1 O1 Ca2 100.4(2) . 3_656 ? Ca3 O1 Ca2 130.4(2) . 3_656 ? As1 O2 Ca2 129.1(3) . . ? As1 O2 Ca3 99.2(2) . 3_666 ? Ca2 O2 Ca3 129.7(2) . 3_666 ? As1 O3 Al 127.3(3) . . ? As1 O3 Ca3 96.0(2) . 3_666 ? Al O3 Ca3 101.8(2) . 3_666 ? As1 O3 Ca2 120.4(3) . 3_666 ? Al O3 Ca2 104.1(2) . 3_666 ? Ca3 O3 Ca2 101.05(16) 3_666 3_666 ? As1 O4 Al 127.3(3) . 2_646 ? As1 O4 Ca2 95.6(2) . 3_656 ? Al O4 Ca2 102.4(2) 2_646 3_656 ? As1 O4 Ca3 120.4(3) . 3_656 ? Al O4 Ca3 104.2(2) 2_646 3_656 ? Ca2 O4 Ca3 101.19(17) 3_656 3_656 ? As2 O5 Ca1 149.8(3) . . ? As2 O6 Ca1 147.8(4) 1_545 . ? As2 O6 OW11 100.7(3) 1_545 . ? Ca1 O6 OW11 100.4(2) . . ? As2 O7 Ca3 123.5(3) 1_545 2_545 ? As2 O7 OH9 100.3(3) 1_545 . ? Ca3 O7 OH9 92.9(2) 2_545 . ? As2 O8 Ca2 125.9(3) . 1_565 ? As2 O8 OW11 112.7(3) . . ? Ca2 O8 OW11 121.0(3) 1_565 . ? Al OH9 Al 99.5(3) 3_666 4_565 ? Al OH9 Ca2 110.2(2) 3_666 . ? Al OH9 Ca2 102.3(2) 4_565 . ? Al OH9 O7 132.4(3) 3_666 . ? Al OH9 O7 106.2(2) 4_565 . ? Ca2 OH9 O7 102.6(2) . . ? Al OH10 Al 99.1(2) 4_565 3_666 ? Al OH10 Ca3 110.1(2) 4_565 . ? Al OH10 Ca3 102.2(2) 3_666 . ? Al OH10 O8 132.5(3) 4_565 2_545 ? Al OH10 O8 105.8(2) 3_666 2_545 ? Ca3 OH10 O8 103.4(2) . 2_545 ? Ca2 OW11 O8 135.2(3) . . ? Ca2 OW11 O6 100.2(2) . . ? O8 OW11 O6 116.8(3) . . ? Ca2 OW11 OW15 92.3(2) . . ? O8 OW11 OW15 90.3(2) . . ? O6 OW11 OW15 120.0(3) . . ? Ca2 OW12 OW14 112.1(3) . 3_656 ? Ca2 OW12 OW15 90.5(2) . . ? OW14 OW12 OW15 94.8(3) 3_656 . ? Ca1 OW13 OW16 114.4(3) . 2_655 ? Ca1 OW13 OW16 86.0(2) . 2_645 ? OW16 OW13 OW16 158.9(4) 2_655 2_645 ? Ca3 OW14 O7 134.6(3) . 2_545 ? Ca3 OW14 O5 100.0(2) . 2_545 ? O7 OW14 O5 113.6(3) 2_545 2_545 ? Ca3 OW15 OW12 106.4(3) 3_666 . ? Ca3 OW15 OW11 110.1(3) 3_666 . ? OW12 OW15 OW11 61.8(2) . . ? Ca3 OW15 OW16 132.6(3) 3_666 . ? OW12 OW15 OW16 91.3(3) . . ? OW11 OW15 OW16 117.0(3) . . ? O6 OW16 OW15 134.6(3) 2_655 . ? O6 OW16 OW12 80.3(3) 2_655 2_655 ? OW15 OW16 OW12 137.7(3) . 2_655 ? _refine_diff_density_max 2.048 _refine_diff_density_min -0.844 _refine_diff_density_rms 0.217 _shelxl_version_number 2013-4 _shelx_res_file ; TITL tapiaite CELL 0.71075 16.0160 5.7781 16.3410 90.000 116.704 90.000 ZERR 1 0.0012 0.0003 0.0012 0.000 0.008 0.000 LATT 1 SYMM .50-X, .50+Y, .50-Z SFAC AS CA AL O H UNIT 8 10 4 64 56 L.S. 5 OMIT -10 3 17 OMIT -3 5 11 OMIT -8 3 16 OMIT -8 1 17 OMIT -2 5 12 OMIT -2 0 6 OMIT 1 0 3 OMIT -9 1 18 OMIT -5 1 4 OMIT -16 3 8 OMIT -6 3 17 OMIT 1 5 9 OMIT -12 3 7 EQIV $1 -x+1/2, y-1/2, -z+1/2 EQIV $2 -x+1, -y, -z+1 EQIV $3 -x+3/2, y-1/2, -z+1/2 EQIV $4 -x+3/2, y+1/2, -z+1/2 BOND BIND OH9 O7 BIND OH10 O8_$1 BIND OW11 O6 BIND OW11 O8 BIND OW12 OW14_$2 BIND OW12 OW15 BIND OW13 OW16_$4 BIND OW13 OW16_$3 BIND OW14 O5_$1 BIND OW14 O7_$1 BIND OW15 OW11 BIND OW15 OW16 BIND OW16 O6_$4 BIND OW16 OW12_$4 FMAP 2 PLAN 20 ACTA SIZE 0.070 0.030 0.010 WGHT 0.078900 0.420300 FVAR 0.58021 0.96712 0.97158 CA1 2 0.500000 0.500000 0.000000 10.50000 0.02618 0.01807 = 0.02317 0.00170 0.01536 0.00171 CA2 2 0.478386 0.185541 0.331492 11.00000 0.01956 0.01855 = 0.01628 -0.00120 0.00665 -0.00222 CA3 2 0.328280 0.314904 0.471205 11.00000 0.01649 0.01992 = 0.01945 0.00259 0.00762 0.00032 AL 3 0.744726 0.499322 0.754919 11.00000 0.01557 0.00968 = 0.01347 -0.00072 0.00587 0.00025 AS1 1 0.578052 0.249505 0.578880 21.00000 0.01349 0.01137 = 0.01337 0.00028 0.00390 -0.00056 AS2 1 0.412197 0.997162 0.095233 31.00000 0.01691 0.01298 = 0.01709 -0.00005 0.00976 0.00016 O1 4 0.476357 0.176170 0.574988 11.00000 0.01552 0.01669 = 0.02659 0.00061 0.01154 -0.00117 O2 4 0.576186 0.322439 0.479777 11.00000 0.02808 0.02068 = 0.01343 0.00362 0.01167 0.00576 O3 4 0.628237 0.486033 0.644363 11.00000 0.01747 0.01196 = 0.01683 0.00648 0.00415 0.00496 O4 4 0.644567 0.011397 0.629926 11.00000 0.01832 0.01340 = 0.01716 -0.00473 0.00853 -0.00261 O5 4 0.415633 0.768259 0.034375 11.00000 0.02959 0.02015 = 0.03446 -0.00835 0.01956 0.00306 O6 4 0.477622 0.216798 0.089191 11.00000 0.03032 0.02470 = 0.03072 0.00204 0.01875 -0.00553 O7 4 0.299816 0.082068 0.057452 11.00000 0.02442 0.01322 = 0.02825 -0.00105 0.01233 -0.00257 O8 4 0.449979 0.922516 0.206698 11.00000 0.02206 0.01378 = 0.01828 0.00018 0.00755 -0.00076 OH9 4 0.304466 0.235691 0.216171 11.00000 0.01981 0.01806 = 0.01774 -0.00027 0.00821 0.00182 OH10 4 0.213920 0.265590 0.302704 11.00000 0.01597 0.01853 = 0.01107 -0.00321 0.00439 -0.00212 OW11 4 0.495764 0.479070 0.237842 11.00000 0.04150 0.02448 = 0.02950 0.00641 0.02025 0.00445 OW12 4 0.635701 0.124549 0.338762 11.00000 0.03069 0.03116 = 0.03334 0.00437 0.01046 0.00551 OW13 4 0.639373 0.598557 0.136745 11.00000 0.04119 0.04034 = 0.03619 -0.00126 0.00912 -0.00366 OW14 4 0.236544 0.021816 0.492794 11.00000 0.02436 0.01827 = 0.03844 -0.00039 0.01600 -0.00687 OW15 4 0.677958 0.602920 0.376880 11.00000 0.04833 0.03442 = 0.03312 -0.00774 0.02384 -0.01060 OW16 4 0.834666 0.568733 0.328243 11.00000 0.04527 0.04194 = 0.03991 -0.00214 0.01074 -0.00640 HKLF 4 REM tapiaite REM R1 = 0.0537 for 1733 Fo > 4sig(Fo) and 0.0784 for all 2357 data REM 198 parameters refined using 0 restraints END WGHT 0.0789 0.4203 REM Highest difference peak 2.048, deepest hole -0.844, 1-sigma level 0.217 Q1 1 0.3550 1.0063 0.0397 11.00000 0.05 2.05 Q2 1 0.6453 0.2602 0.6439 11.00000 0.05 1.78 Q3 1 0.5185 0.2506 0.5157 11.00000 0.05 1.75 Q4 1 0.4754 1.0141 0.1666 11.00000 0.05 1.54 Q5 1 0.5275 0.2414 0.6167 11.00000 0.05 1.20 Q6 1 0.5408 0.1990 0.3971 11.00000 0.05 1.13 Q7 1 0.5593 0.5421 0.0653 11.00000 0.05 1.11 Q8 1 0.6987 0.0362 0.6877 11.00000 0.05 0.99 Q9 1 0.3713 1.0031 0.1296 11.00000 0.05 0.98 Q10 1 0.4009 0.2999 0.5447 11.00000 0.05 0.96 Q11 1 0.4126 0.1849 0.2751 11.00000 0.05 0.95 Q12 1 0.4439 0.3256 0.5840 11.00000 0.05 0.83 Q13 1 0.6773 0.4863 0.6925 11.00000 0.05 0.82 Q14 1 0.6622 0.8018 0.1596 11.00000 0.05 0.82 Q15 1 0.5182 0.5154 0.1766 11.00000 0.05 0.81 Q16 1 0.2671 0.3337 0.4083 11.00000 0.05 0.76 Q17 1 0.6266 0.2508 0.5298 11.00000 0.05 0.76 Q18 1 0.1752 0.0570 0.4795 11.00000 0.05 0.72 Q19 1 0.2758 0.2205 0.3752 11.00000 0.05 0.70 Q20 1 0.6762 0.0255 0.3911 11.00000 0.05 0.69 ; _shelx_res_checksum 60615 _shelx_hkl_file ; 0 -1 0 -16.95 17.54 -1 0 -2 -36.74 18.67 1 0 2 6.30 17.40 2 0 1 2.35 21.16 -2 0 -1 -34.14 35.63 1 0 -3 907.47 50.97 -1 0 3 822.98 79.16 0 -1 1 2402.77 86.87 0 -1 1 2501.08 70.78 0 -1 -1 2524.80 52.33 0 1 -1 2528.03 81.08 0 1 -1 2423.77 65.18 1 1 0 2650.19 55.38 -1 -1 0 2706.36 61.24 -1 1 0 2726.87 110.08 1 -1 0 2703.00 103.41 -1 1 0 2604.77 67.22 -1 -1 1 9.55 12.45 -1 -1 1 -6.56 15.99 1 -1 -1 15.09 25.35 1 -1 -1 4.68 13.62 1 1 -1 22.81 16.09 -1 1 1 1.59 7.86 -3 0 1 653.50 47.72 -3 0 1 631.52 67.15 3 0 -1 675.58 66.22 3 0 -1 766.40 73.91 -2 0 3 42.22 25.40 2 0 -3 20.58 23.81 3 0 -2 32.20 38.66 -3 0 2 3.41 22.94 3 0 -2 16.64 16.90 -3 0 2 29.25 27.63 0 0 -3 -17.31 22.20 0 0 3 5.23 37.99 1 -1 1 78.23 22.37 -1 1 -1 -5.28 14.46 -1 -1 -1 21.60 7.97 -1 1 -1 54.96 22.94 -3 0 0 -57.44 38.29 3 0 0 -37.23 40.78 3 0 0 -31.59 23.82 -3 0 0 12.29 24.22 1 -1 -2 2336.43 95.46 -1 -1 2 2252.95 77.56 1 1 -2 2478.40 74.74 -1 1 2 2438.63 67.93 1 1 -2 2390.22 110.70 -1 -1 2 2473.03 70.64 -2 1 1 2215.56 75.07 -2 1 1 2303.01 111.60 2 -1 -1 2160.34 74.59 2 1 -1 2199.40 91.41 -2 -1 1 2147.75 98.32 2 -1 -1 2135.13 107.74 -3 0 3 9351.63 403.75 3 0 -3 9297.57 398.22 3 0 -3 9495.35 338.56 0 -1 2 890.21 58.03 0 1 2 685.70 26.96 0 -1 -2 727.63 26.78 0 -1 2 693.31 42.63 0 1 -2 783.50 39.67 -2 1 0 1087.04 51.28 2 1 0 1146.30 53.86 -2 -1 0 1164.29 40.94 2 -1 0 1274.52 113.15 -2 1 2 44.87 27.33 2 -1 -2 -2.98 26.72 2 1 -2 36.65 30.32 -2 -1 2 -2.68 18.28 2 -1 -2 14.61 30.45 -2 -1 2 7.72 7.87 -2 0 -2 1358.67 87.50 -1 0 -3 2647.49 114.68 1 0 3 2534.06 108.82 -2 0 4 4178.56 245.05 2 0 -4 4025.65 238.45 -3 0 -1 3851.05 159.52 -3 0 -1 4962.10 275.72 3 0 1 4948.86 262.94 -1 1 -2 623.93 46.26 -1 1 -2 955.59 54.88 -1 -1 -2 722.54 35.13 1 -1 2 958.25 84.25 4 0 -2 3829.53 236.16 4 0 -2 3863.22 194.42 -4 0 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6979.77 341.46 0 -4 6 6087.52 318.92 0 4 -6 5317.90 450.93 -12 1 9 175.01 93.05 -12 -1 9 209.70 135.62 12 1 -9 240.90 132.44 12 -1 -9 237.43 112.17 12 1 -9 260.65 45.65 -12 -1 2 664.09 97.77 -12 -1 2 963.60 176.95 -12 1 2 893.45 123.82 -12 1 2 743.39 123.59 12 1 -2 824.25 113.02 12 -1 -2 802.10 124.72 0 3 9 641.43 67.42 0 3 -9 1088.98 134.49 0 -3 9 700.64 102.60 0 3 -9 797.20 148.59 0 -3 -9 886.72 107.60 -3 -4 -4 19.56 12.24 -3 -4 -4 -7.03 12.91 3 -4 4 -45.66 68.87 -3 4 -4 54.05 32.53 -3 4 -4 -9.08 49.50 -1 -1 -11 139.97 54.91 1 -1 11 63.25 60.07 -1 1 -11 -14.74 94.12 1 1 11 69.68 55.43 -1 1 -11 20.22 91.58 -4 4 -3 82.06 58.15 -4 4 -3 50.64 62.08 -4 4 -3 38.72 60.89 4 -4 3 6.01 56.34 -4 -4 -3 80.88 17.04 -4 -4 -3 86.12 18.47 -8 3 9 7680.10 577.93 8 -3 -9 7969.67 794.71 8 3 -9 7701.92 502.52 -8 -3 9 7528.55 485.27 8 -3 -9 7482.04 574.11 3 -3 -10 -7.41 53.03 3 3 -10 -5.14 41.62 -3 -3 10 67.74 45.40 -3 3 10 -64.24 50.46 -6 -4 0 6048.06 282.68 -6 4 0 6894.41 440.18 -6 4 0 6255.02 489.25 6 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