data_bortolanite _audit_creation_method SHELXL-2014 _chemical_name_systematic ; ? ; _chemical_name_common bortolanite _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'Ca4.19 Ce0.06 F2.76 Fe0.06 Gd0.01 Hf0.01 La0.03 Mn0.16 Na2.03 Nb0.06 Nd0.02 O15.24 Si4.07 Ti0.94 Y0.02 Zr0.41' _chemical_formula_weight 745.95 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Ca' 'Ca' 0.2262 0.3064 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Na' 'Na' 0.0362 0.0249 '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' 'Si' 'Si' 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ti' 'Ti' 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Nb' 'Nb' -2.0727 0.6215 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Zr' 'Zr' -2.9673 0.5597 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ce' 'Ce' -0.2486 2.6331 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Mn' 'Mn' 0.3368 0.7283 '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' 'Y' 'Y' -2.7962 3.5667 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Hf' 'Hf' -0.5830 6.1852 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'La' 'La' -0.2871 2.4523 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Nd' 'Nd' -0.1943 3.0179 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Gd' 'Gd' -0.1653 3.9035 '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 9.615(3) _cell_length_b 5.7248(18) _cell_length_c 7.316(2) _cell_angle_alpha 89.906(10) _cell_angle_beta 101.141(11) _cell_angle_gamma 100.905(11) _cell_volume 387.7(2) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4968 _cell_measurement_theta_min 3.233 _cell_measurement_theta_max 31.099 _exptl_crystal_description tabular _exptl_crystal_colour 'pale-yellow to brown' _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_density_diffrn 3.195 _exptl_crystal_F_000 364 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.040 _exptl_crystal_size_mid 0.030 _exptl_crystal_size_min 0.020 _exptl_absorpt_coefficient_mu 3.378 _shelx_estimated_absorpt_T_min 0.877 _shelx_estimated_absorpt_T_max 0.936 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.6666 _exptl_absorpt_correction_T_max 0.7462 _exptl_absorpt_process_details 'SADABS-2008/1 - Bruker AXS area detector scaling and absorption correction' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source 'fine-focus sealed tube' _diffrn_measurement_device_type 'Bruker APEX II ULTRA' _diffrn_measurement_method \\w _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 4988 _diffrn_reflns_av_unetI/netI 0.0218 _diffrn_reflns_av_R_equivalents 0.0145 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 2.200 _diffrn_reflns_theta_max 31.105 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measured_fraction_theta_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.998 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.998 _diffrn_reflns_point_group_measured_fraction_full 1.000 _reflns_number_total 2500 _reflns_number_gt 2194 _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 'SAINT V7.66A' _computing_data_reduction 'SAINT V7.66A' _computing_structure_solution ? _computing_structure_refinement 'SHELXL-2014 (Sheldrick, 2014)' _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^)+(0.0244P)^2^+0.8517P] 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 2500 _refine_ls_number_parameters 147 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0375 _refine_ls_R_factor_gt 0.0319 _refine_ls_wR_factor_ref 0.0735 _refine_ls_wR_factor_gt 0.0711 _refine_ls_goodness_of_fit_ref 1.083 _refine_ls_restrained_S_all 1.083 _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 Zr Zr 0.63264(4) 0.22434(7) 0.90910(5) 0.01592(12) Uani 0.6245(16) 1 d . . P . . Ca Ca 0.63248(5) 0.23075(8) 0.40732(6) 0.01813(14) Uani 1.144(3) 1 d . . P . . Ti Ti -0.0131(3) 0.0233(5) -0.0034(4) 0.0083(4) Uani 0.5164(19) 1 d . . P . . Na1 Na 0.0000 0.0000 0.5000 0.0150(4) Uani 1.123(7) 2 d S . P . . Na2 Na 0.99424(8) 0.49700(11) 0.24233(9) 0.0133(2) Uani 1.329(5) 1 d . . P . . Si1 Si 0.71686(7) 0.75021(11) 0.65134(8) 0.01066(14) Uani 1 1 d . . . . . Si2 Si 0.72274(7) 0.75447(11) 0.21326(8) 0.01098(14) Uani 1 1 d . . . . . O1 O 0.7555(2) 0.7790(4) 0.4420(3) 0.0315(5) Uani 1 1 d . . . . . O2 O 0.61612(19) 0.9416(3) 0.6679(3) 0.0177(3) Uani 1 1 d . . . . . O3 O 0.6181(2) 0.9369(3) 0.1411(3) 0.0200(4) Uani 1 1 d . . . . . O4 O 0.6419(2) 0.4786(3) 0.6690(3) 0.0272(4) Uani 1 1 d . . . . . O5 O 0.6613(3) 0.4794(4) 0.1558(3) 0.0341(5) Uani 1 1 d . . . . . O6 O 0.87629(19) 0.8138(3) 0.7835(3) 0.0198(4) Uani 1 1 d . . . . . O7 O 0.8842(2) 0.8329(3) 0.1699(3) 0.0193(4) Uani 1 1 d . . . . . F1 F 0.88410(17) 0.2569(3) 0.9671(2) 0.0182(3) Uani 0.9311 1 d . . P . . F2 F 0.88423(17) 0.3044(3) 0.4744(2) 0.0217(3) 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 Zr 0.0173(2) 0.01695(19) 0.01098(17) -0.00012(12) 0.00269(13) -0.00288(13) Ca 0.0147(2) 0.0251(2) 0.01123(19) -0.00279(15) 0.00406(14) -0.00622(16) Ti 0.0075(10) 0.0102(10) 0.0077(3) 0.0002(6) 0.0020(6) 0.0023(4) Na1 0.0084(6) 0.0147(6) 0.0211(7) -0.0018(4) -0.0002(4) 0.0031(4) Na2 0.0270(4) 0.0086(3) 0.0077(3) 0.0013(2) 0.0059(3) 0.0094(3) Si1 0.0105(3) 0.0127(3) 0.0091(3) -0.0001(2) 0.0018(2) 0.0030(2) Si2 0.0117(3) 0.0125(3) 0.0101(3) 0.0014(2) 0.0040(2) 0.0038(2) O1 0.0268(11) 0.0553(14) 0.0113(8) 0.0010(9) 0.0065(8) 0.0025(10) O2 0.0137(8) 0.0177(8) 0.0228(8) -0.0025(7) 0.0022(7) 0.0070(6) O3 0.0180(9) 0.0216(8) 0.0233(9) 0.0058(7) 0.0038(7) 0.0112(7) O4 0.0366(12) 0.0166(8) 0.0244(9) -0.0004(7) 0.0067(8) -0.0061(8) O5 0.0541(15) 0.0165(9) 0.0308(11) -0.0036(8) 0.0173(10) -0.0047(9) O6 0.0148(8) 0.0233(9) 0.0197(8) -0.0067(7) -0.0039(7) 0.0071(7) O7 0.0167(9) 0.0235(9) 0.0214(8) 0.0076(7) 0.0103(7) 0.0063(7) F1 0.0143(7) 0.0211(7) 0.0197(7) 0.0002(6) 0.0031(6) 0.0052(6) F2 0.0176(7) 0.0208(7) 0.0275(8) 0.0018(6) 0.0044(6) 0.0055(6) _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 Zr O5 2.265(2) 1_556 ? Zr O4 2.284(2) . ? Zr F1 2.3439(18) . ? Zr O2 2.3589(18) 1_545 ? Zr O3 2.3672(19) 1_546 ? Zr O3 2.370(2) 2_666 ? Zr Ca 3.6456(12) 1_556 ? Zr Ca 3.6710(12) . ? Zr Ca 3.7245(10) 2_656 ? Zr Na2 3.8926(13) 1_556 ? Ca F2 2.3309(18) . ? Ca O5 2.352(2) . ? Ca O4 2.362(2) . ? Ca O2 2.3645(19) 2_666 ? Ca O2 2.531(2) 1_545 ? Ca O3 2.542(2) 1_545 ? Ca O1 3.032(3) 1_545 ? Ca Si1 3.3257(12) 2_666 ? Ca Si1 3.3517(12) . ? Ca Si2 3.3520(12) . ? Ca Si2 3.4040(11) 1_545 ? Ca Si1 3.4179(11) 1_545 ? Ti Ti 0.397(3) 2 ? Ti F1 1.797(2) 1_454 ? Ti O7 1.961(4) 1_445 ? Ti O6 1.971(4) 1_444 ? Ti O7 1.973(4) 2_665 ? Ti O6 1.978(4) 2_666 ? Ti F1 2.192(2) 2_656 ? Ti Na2 3.238(3) 1_455 ? Ti Na2 3.248(3) 2_665 ? Ti Na2 3.508(3) 2_655 ? Ti Na2 3.511(3) 1_445 ? Ti Na1 3.663(3) 1_554 ? Na1 F2 2.2277(16) 2_656 ? Na1 F2 2.2277(16) 1_455 ? Na1 O1 2.408(2) 2_666 ? Na1 O1 2.408(2) 1_445 ? Na1 O7 2.560(2) 2_666 ? Na1 O7 2.560(2) 1_445 ? Na1 O6 2.705(2) 2_666 ? Na1 O6 2.705(2) 1_445 ? Na1 Si2 3.1487(10) 2_666 ? Na1 Si2 3.1487(10) 1_445 ? Na1 Si1 3.2200(10) 2_666 ? Na1 Si1 3.2200(10) 1_445 ? Na2 F2 2.3376(18) . ? Na2 F2 2.3500(18) 2_766 ? Na2 O7 2.377(2) . ? Na2 O6 2.3836(19) 2_766 ? Na2 F1 2.3875(18) 1_554 ? Na2 F1 2.4008(18) 2_766 ? Na2 Si2 3.2052(12) . ? Na2 Ti 3.238(3) 1_655 ? Na2 Ti 3.248(3) 2_665 ? Na2 Si1 3.3125(12) 2_766 ? Na2 Na1 3.4138(11) 1_655 ? Na2 Na1 3.4302(11) 1_665 ? Si1 O4 1.602(2) . ? Si1 O2 1.6127(18) . ? Si1 O6 1.6230(19) . ? Si1 O1 1.645(2) . ? Si1 Na1 3.2201(10) 1_665 ? Si1 Na2 3.3125(12) 2_766 ? Si1 Ca 3.3257(12) 2_666 ? Si1 Ca 3.4179(11) 1_565 ? Si2 O5 1.600(2) . ? Si2 O3 1.6040(19) . ? Si2 O7 1.6239(19) . ? Si2 O1 1.643(2) . ? Si2 Na1 3.1487(10) 1_665 ? Si2 Ca 3.4041(11) 1_565 ? O1 Na1 2.408(2) 1_665 ? O1 Ca 3.032(3) 1_565 ? O2 Zr 2.3589(18) 1_565 ? O2 Ca 2.3645(19) 2_666 ? O2 Ca 2.531(2) 1_565 ? O3 Zr 2.3671(19) 1_564 ? O3 Zr 2.370(2) 2_666 ? O3 Ca 2.542(2) 1_565 ? O5 Zr 2.265(2) 1_554 ? O6 Ti 1.971(4) 1_666 ? O6 Ti 1.978(4) 2_666 ? O6 Na2 2.3836(19) 2_766 ? O6 Na1 2.705(2) 1_665 ? O7 Ti 1.961(4) 1_665 ? O7 Ti 1.973(4) 2_665 ? O7 Na1 2.560(2) 1_665 ? F1 Ti 1.797(2) 1_656 ? F1 Ti 2.192(2) 2_656 ? F1 Na2 2.3875(18) 1_556 ? F1 Na2 2.4008(18) 2_766 ? F2 Na1 2.2278(16) 1_655 ? F2 Na2 2.3500(18) 2_766 ? 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 Zr O4 101.81(8) 1_556 . ? O5 Zr F1 88.24(8) 1_556 . ? O4 Zr F1 91.22(7) . . ? O5 Zr O2 175.25(8) 1_556 1_545 ? O4 Zr O2 81.69(7) . 1_545 ? F1 Zr O2 88.47(6) . 1_545 ? O5 Zr O3 82.46(8) 1_556 1_546 ? O4 Zr O3 175.69(7) . 1_546 ? F1 Zr O3 89.48(6) . 1_546 ? O2 Zr O3 94.08(7) 1_545 1_546 ? O5 Zr O3 101.88(8) 1_556 2_666 ? O4 Zr O3 101.13(7) . 2_666 ? F1 Zr O3 161.94(6) . 2_666 ? O2 Zr O3 80.43(7) 1_545 2_666 ? O3 Zr O3 77.25(7) 1_546 2_666 ? O5 Zr Ca 38.69(6) 1_556 1_556 ? O4 Zr Ca 140.30(5) . 1_556 ? F1 Zr Ca 91.13(4) . 1_556 ? O2 Zr Ca 138.00(5) 1_545 1_556 ? O3 Zr Ca 43.92(5) 1_546 1_556 ? O3 Zr Ca 87.74(5) 2_666 1_556 ? O5 Zr Ca 140.18(6) 1_556 . ? O4 Zr Ca 38.55(5) . . ? F1 Zr Ca 89.05(4) . . ? O2 Zr Ca 43.15(5) 1_545 . ? O3 Zr Ca 137.23(5) 1_546 . ? O3 Zr Ca 92.44(5) 2_666 . ? Ca Zr Ca 178.840(19) 1_556 . ? O5 Zr Ca 144.26(7) 1_556 2_656 ? O4 Zr Ca 90.20(6) . 2_656 ? F1 Zr Ca 125.43(4) . 2_656 ? O2 Zr Ca 38.01(5) 1_545 2_656 ? O3 Zr Ca 85.93(5) 1_546 2_656 ? O3 Zr Ca 42.45(5) 2_666 2_656 ? Ca Zr Ca 119.732(18) 1_556 2_656 ? Ca Zr Ca 60.990(19) . 2_656 ? O5 Zr Na2 53.34(7) 1_556 1_556 ? O4 Zr Na2 100.01(6) . 1_556 ? F1 Zr Na2 35.01(4) . 1_556 ? O2 Zr Na2 123.15(5) 1_545 1_556 ? O3 Zr Na2 82.96(5) 1_546 1_556 ? O3 Zr Na2 150.41(5) 2_666 1_556 ? Ca Zr Na2 62.85(2) 1_556 1_556 ? Ca Zr Na2 116.90(2) . 1_556 ? Ca Zr Na2 157.227(18) 2_656 1_556 ? F2 Ca O5 84.47(8) . . ? F2 Ca O4 87.93(7) . . ? O5 Ca O4 107.26(8) . . ? F2 Ca O2 165.94(6) . 2_666 ? O5 Ca O2 102.24(8) . 2_666 ? O4 Ca O2 101.59(7) . 2_666 ? F2 Ca O2 92.42(6) . 1_545 ? O5 Ca O2 174.87(7) . 1_545 ? O4 Ca O2 76.64(7) . 1_545 ? O2 Ca O2 79.94(7) 2_666 1_545 ? F2 Ca O3 92.88(6) . 1_545 ? O5 Ca O3 77.11(7) . 1_545 ? O4 Ca O3 175.62(7) . 1_545 ? O2 Ca O3 76.86(6) 2_666 1_545 ? O2 Ca O3 99.01(6) 1_545 1_545 ? F2 Ca O1 67.05(6) . 1_545 ? O5 Ca O1 120.21(7) . 1_545 ? O4 Ca O1 122.04(7) . 1_545 ? O2 Ca O1 98.99(6) 2_666 1_545 ? O2 Ca O1 54.69(5) 1_545 1_545 ? O3 Ca O1 54.63(6) 1_545 1_545 ? F2 Ca Si1 167.17(4) . 2_666 ? O5 Ca Si1 91.91(7) . 2_666 ? O4 Ca Si1 81.38(6) . 2_666 ? O2 Ca Si1 26.70(4) 2_666 2_666 ? O2 Ca Si1 91.99(4) 1_545 2_666 ? O3 Ca Si1 98.32(5) 1_545 2_666 ? O1 Ca Si1 124.90(5) 1_545 2_666 ? F2 Ca Si1 76.99(4) . . ? O5 Ca Si1 82.81(6) . . ? O4 Ca Si1 25.86(5) . . ? O2 Ca Si1 115.84(5) 2_666 . ? O2 Ca Si1 100.49(5) 1_545 . ? O3 Ca Si1 158.33(5) 1_545 . ? O1 Ca Si1 133.54(4) 1_545 . ? Si1 Ca Si1 90.36(2) 2_666 . ? F2 Ca Si2 76.62(4) . . ? O5 Ca Si2 25.69(5) . . ? O4 Ca Si2 82.45(5) . . ? O2 Ca Si2 114.59(5) 2_666 . ? O2 Ca Si2 156.75(4) 1_545 . ? O3 Ca Si2 101.93(5) 1_545 . ? O1 Ca Si2 133.88(4) 1_545 . ? Si1 Ca Si2 94.86(2) 2_666 . ? Si1 Ca Si2 57.35(3) . . ? F2 Ca Si2 75.31(4) . 1_545 ? O5 Ca Si2 95.22(6) . 1_545 ? O4 Ca Si2 150.55(6) . 1_545 ? O2 Ca Si2 91.66(5) 2_666 1_545 ? O2 Ca Si2 80.01(5) 1_545 1_545 ? O3 Ca Si2 26.59(4) 1_545 1_545 ? O1 Ca Si2 28.85(4) 1_545 1_545 ? Si1 Ca Si2 117.35(2) 2_666 1_545 ? Si1 Ca Si2 152.29(2) . 1_545 ? Si2 Ca Si2 115.85(3) . 1_545 ? F2 Ca Si1 75.74(4) . 1_545 ? O5 Ca Si1 148.40(6) . 1_545 ? O4 Ca Si1 96.53(6) . 1_545 ? O2 Ca Si1 92.76(5) 2_666 1_545 ? O2 Ca Si1 26.47(4) 1_545 1_545 ? O3 Ca Si1 79.51(5) 1_545 1_545 ? O1 Ca Si1 28.77(4) 1_545 1_545 ? Si1 Ca Si1 112.38(2) 2_666 1_545 ? Si1 Ca Si1 115.48(3) . 1_545 ? Si2 Ca Si1 152.35(2) . 1_545 ? Si2 Ca Si1 56.26(3) 1_545 1_545 ? Ti Ti F1 174.3(11) 2 1_454 ? Ti Ti O7 86.0(10) 2 1_445 ? F1 Ti O7 98.23(14) 1_454 1_445 ? Ti Ti O6 85.2(9) 2 1_444 ? F1 Ti O6 98.38(14) 1_454 1_444 ? O7 Ti O6 91.48(16) 1_445 1_444 ? Ti Ti O7 82.4(9) 2 2_665 ? F1 Ti O7 93.32(14) 1_454 2_665 ? O7 Ti O7 168.42(7) 1_445 2_665 ? O6 Ti O7 87.58(15) 1_444 2_665 ? Ti Ti O6 83.2(9) 2 2_666 ? F1 Ti O6 93.12(13) 1_454 2_666 ? O7 Ti O6 87.73(15) 1_445 2_666 ? O6 Ti O6 168.46(7) 1_444 2_666 ? O7 Ti O6 90.89(16) 2_665 2_666 ? Ti Ti F1 4.7(9) 2 2_656 ? F1 Ti F1 178.97(19) 1_454 2_656 ? O7 Ti F1 82.54(11) 1_445 2_656 ? O6 Ti F1 82.28(10) 1_444 2_656 ? O7 Ti F1 85.90(11) 2_665 2_656 ? O6 Ti F1 86.21(11) 2_666 2_656 ? Ti Ti Na2 130.3(9) 2 1_455 ? F1 Ti Na2 46.47(8) 1_454 1_455 ? O7 Ti Na2 89.07(11) 1_445 1_455 ? O6 Ti Na2 144.40(9) 1_444 1_455 ? O7 Ti Na2 98.41(12) 2_665 1_455 ? O6 Ti Na2 47.12(7) 2_666 1_455 ? F1 Ti Na2 132.96(13) 2_656 1_455 ? Ti Ti Na2 129.0(10) 2 2_665 ? F1 Ti Na2 46.64(9) 1_454 2_665 ? O7 Ti Na2 144.86(9) 1_445 2_665 ? O6 Ti Na2 94.25(12) 1_444 2_665 ? O7 Ti Na2 46.68(8) 2_665 2_665 ? O6 Ti Na2 93.00(12) 2_666 2_665 ? F1 Ti Na2 132.58(13) 2_656 2_665 ? Na2 Ti Na2 66.77(5) 1_455 2_665 ? Ti Ti Na2 44.8(9) 2 2_655 ? F1 Ti Na2 138.45(15) 1_454 2_655 ? O7 Ti Na2 90.41(10) 1_445 2_655 ? O6 Ti Na2 40.54(6) 1_444 2_655 ? O7 Ti Na2 81.38(10) 2_665 2_655 ? O6 Ti Na2 127.94(8) 2_666 2_655 ? F1 Ti Na2 42.11(6) 2_656 2_655 ? Na2 Ti Na2 175.05(8) 1_455 2_655 ? Na2 Ti Na2 115.81(10) 2_665 2_655 ? Ti Ti Na2 46.0(9) 2 1_445 ? F1 Ti Na2 138.38(15) 1_454 1_445 ? O7 Ti Na2 40.15(7) 1_445 1_445 ? O6 Ti Na2 85.53(10) 1_444 1_445 ? O7 Ti Na2 128.29(8) 2_665 1_445 ? O6 Ti Na2 86.46(10) 2_666 1_445 ? F1 Ti Na2 42.39(7) 2_656 1_445 ? Na2 Ti Na2 115.98(10) 1_455 1_445 ? Na2 Ti Na2 174.96(8) 2_665 1_445 ? Na2 Ti Na2 61.12(4) 2_655 1_445 ? Ti Ti Na1 87.0(9) 2 1_554 ? F1 Ti Na1 92.37(12) 1_454 1_554 ? O7 Ti Na1 137.59(14) 1_445 1_554 ? O6 Ti Na1 46.25(9) 1_444 1_554 ? O7 Ti Na1 41.90(9) 2_665 1_554 ? O6 Ti Na1 132.72(15) 2_666 1_554 ? F1 Ti Na1 87.51(9) 2_656 1_554 ? Na2 Ti Na1 125.91(8) 1_455 1_554 ? Na2 Ti Na1 59.15(5) 2_665 1_554 ? Na2 Ti Na1 56.81(5) 2_655 1_554 ? Na2 Ti Na1 117.93(6) 1_445 1_554 ? F2 Na1 F2 180.0 2_656 1_455 ? F2 Na1 O1 81.17(8) 2_656 2_666 ? F2 Na1 O1 98.83(8) 1_455 2_666 ? F2 Na1 O1 98.83(8) 2_656 1_445 ? F2 Na1 O1 81.17(8) 1_455 1_445 ? O1 Na1 O1 180.0 2_666 1_445 ? F2 Na1 O7 93.77(6) 2_656 2_666 ? F2 Na1 O7 86.23(6) 1_455 2_666 ? O1 Na1 O7 61.10(6) 2_666 2_666 ? O1 Na1 O7 118.90(6) 1_445 2_666 ? F2 Na1 O7 86.23(6) 2_656 1_445 ? F2 Na1 O7 93.77(6) 1_455 1_445 ? O1 Na1 O7 118.90(6) 2_666 1_445 ? O1 Na1 O7 61.10(6) 1_445 1_445 ? O7 Na1 O7 180.0 2_666 1_445 ? F2 Na1 O6 93.28(6) 2_656 2_666 ? F2 Na1 O6 86.72(6) 1_455 2_666 ? O1 Na1 O6 59.09(6) 2_666 2_666 ? O1 Na1 O6 120.91(6) 1_445 2_666 ? O7 Na1 O6 117.63(6) 2_666 2_666 ? O7 Na1 O6 62.37(6) 1_445 2_666 ? F2 Na1 O6 86.72(6) 2_656 1_445 ? F2 Na1 O6 93.28(6) 1_455 1_445 ? O1 Na1 O6 120.91(6) 2_666 1_445 ? O1 Na1 O6 59.09(6) 1_445 1_445 ? O7 Na1 O6 62.37(6) 2_666 1_445 ? O7 Na1 O6 117.63(6) 1_445 1_445 ? O6 Na1 O6 180.0 2_666 1_445 ? F2 Na1 Si2 82.29(5) 2_656 2_666 ? F2 Na1 Si2 97.71(5) 1_455 2_666 ? O1 Na1 Si2 30.89(5) 2_666 2_666 ? O1 Na1 Si2 149.11(5) 1_445 2_666 ? O7 Na1 Si2 30.92(4) 2_666 2_666 ? O7 Na1 Si2 149.08(4) 1_445 2_666 ? O6 Na1 Si2 89.67(4) 2_666 2_666 ? O6 Na1 Si2 90.33(4) 1_445 2_666 ? F2 Na1 Si2 97.71(5) 2_656 1_445 ? F2 Na1 Si2 82.29(5) 1_455 1_445 ? O1 Na1 Si2 149.11(5) 2_666 1_445 ? O1 Na1 Si2 30.89(5) 1_445 1_445 ? O7 Na1 Si2 149.08(4) 2_666 1_445 ? O7 Na1 Si2 30.92(4) 1_445 1_445 ? O6 Na1 Si2 90.33(4) 2_666 1_445 ? O6 Na1 Si2 89.67(4) 1_445 1_445 ? Si2 Na1 Si2 180.0 2_666 1_445 ? F2 Na1 Si1 81.42(5) 2_656 2_666 ? F2 Na1 Si1 98.58(5) 1_455 2_666 ? O1 Na1 Si1 29.78(5) 2_666 2_666 ? O1 Na1 Si1 150.22(5) 1_445 2_666 ? O7 Na1 Si1 90.67(4) 2_666 2_666 ? O7 Na1 Si1 89.33(4) 1_445 2_666 ? O6 Na1 Si1 30.23(4) 2_666 2_666 ? O6 Na1 Si1 149.77(4) 1_445 2_666 ? Si2 Na1 Si1 60.65(3) 2_666 2_666 ? Si2 Na1 Si1 119.35(3) 1_445 2_666 ? F2 Na1 Si1 98.58(5) 2_656 1_445 ? F2 Na1 Si1 81.42(5) 1_455 1_445 ? O1 Na1 Si1 150.22(5) 2_666 1_445 ? O1 Na1 Si1 29.78(5) 1_445 1_445 ? O7 Na1 Si1 89.33(4) 2_666 1_445 ? O7 Na1 Si1 90.67(4) 1_445 1_445 ? O6 Na1 Si1 149.77(4) 2_666 1_445 ? O6 Na1 Si1 30.23(4) 1_445 1_445 ? Si2 Na1 Si1 119.35(3) 2_666 1_445 ? Si2 Na1 Si1 60.65(3) 1_445 1_445 ? Si1 Na1 Si1 180.0 2_666 1_445 ? F2 Na2 F2 73.72(7) . 2_766 ? F2 Na2 O7 105.57(6) . . ? F2 Na2 O7 87.92(6) 2_766 . ? F2 Na2 O6 92.30(7) . 2_766 ? F2 Na2 O6 103.38(6) 2_766 2_766 ? O7 Na2 O6 161.07(7) . 2_766 ? F2 Na2 F1 103.92(7) . 1_554 ? F2 Na2 F1 173.24(6) 2_766 1_554 ? O7 Na2 F1 98.83(7) . 1_554 ? O6 Na2 F1 70.20(6) 2_766 1_554 ? F2 Na2 F1 171.98(6) . 2_766 ? F2 Na2 F1 99.08(6) 2_766 2_766 ? O7 Na2 F1 70.12(6) . 2_766 ? O6 Na2 F1 92.85(7) 2_766 2_766 ? F1 Na2 F1 83.63(6) 1_554 2_766 ? F2 Na2 Si2 79.67(5) . . ? F2 Na2 Si2 93.67(5) 2_766 . ? O7 Na2 Si2 29.31(4) . . ? O6 Na2 Si2 158.38(5) 2_766 . ? F1 Na2 Si2 92.10(5) 1_554 . ? F1 Na2 Si2 97.54(5) 2_766 . ? F2 Na2 Ti 96.78(8) . 1_655 ? F2 Na2 Ti 140.31(6) 2_766 1_655 ? O7 Na2 Ti 131.34(7) . 1_655 ? O6 Na2 Ti 37.45(6) 2_766 1_655 ? F1 Na2 Ti 33.07(6) 1_554 1_655 ? F1 Na2 Ti 91.05(7) 2_766 1_655 ? Si2 Na2 Ti 123.07(5) . 1_655 ? F2 Na2 Ti 142.29(6) . 2_665 ? F2 Na2 Ti 94.56(7) 2_766 2_665 ? O7 Na2 Ti 37.16(6) . 2_665 ? O6 Na2 Ti 125.41(7) 2_766 2_665 ? F1 Na2 Ti 91.05(7) 1_554 2_665 ? F1 Na2 Ti 32.96(6) 2_766 2_665 ? Si2 Na2 Ti 65.16(5) . 2_665 ? Ti Na2 Ti 113.24(5) 1_655 2_665 ? F2 Na2 Si1 93.84(5) . 2_766 ? F2 Na2 Si1 77.59(5) 2_766 2_766 ? O7 Na2 Si1 151.53(5) . 2_766 ? O6 Na2 Si1 27.40(4) 2_766 2_766 ? F1 Na2 Si1 96.39(5) 1_554 2_766 ? F1 Na2 Si1 87.93(5) 2_766 2_766 ? Si2 Na2 Si1 170.37(3) . 2_766 ? Ti Na2 Si1 64.45(5) 1_655 2_766 ? Ti Na2 Si1 119.02(5) 2_665 2_766 ? F2 Na2 Na1 40.39(4) . 1_655 ? F2 Na2 Na1 83.56(5) 2_766 1_655 ? O7 Na2 Na1 145.90(5) . 1_655 ? O6 Na2 Na1 52.01(5) 2_766 1_655 ? F1 Na2 Na1 90.60(5) 1_554 1_655 ? F1 Na2 Na1 143.83(5) 2_766 1_655 ? Si2 Na2 Na1 118.38(3) . 1_655 ? Ti Na2 Na1 66.78(6) 1_655 1_655 ? Ti Na2 Na1 176.03(5) 2_665 1_655 ? Si1 Na2 Na1 57.180(19) 2_766 1_655 ? F2 Na2 Na1 83.36(5) . 1_665 ? F2 Na2 Na1 40.13(4) 2_766 1_665 ? O7 Na2 Na1 48.23(5) . 1_665 ? O6 Na2 Na1 142.98(5) 2_766 1_665 ? F1 Na2 Na1 146.49(5) 1_554 1_665 ? F1 Na2 Na1 88.82(5) 2_766 1_665 ? Si2 Na2 Na1 56.54(2) . 1_665 ? Ti Na2 Na1 179.56(5) 1_655 1_665 ? Ti Na2 Na1 66.47(6) 2_665 1_665 ? Si1 Na2 Na1 115.96(3) 2_766 1_665 ? Na1 Na2 Na1 113.54(3) 1_655 1_665 ? O4 Si1 O2 114.84(11) . . ? O4 Si1 O6 111.47(11) . . ? O2 Si1 O6 114.20(10) . . ? O4 Si1 O1 107.87(12) . . ? O2 Si1 O1 105.50(11) . . ? O6 Si1 O1 101.68(11) . . ? O4 Si1 Na1 133.52(9) . 1_665 ? O2 Si1 Na1 110.03(7) . 1_665 ? O6 Si1 Na1 57.06(7) . 1_665 ? O1 Si1 Na1 46.61(8) . 1_665 ? O4 Si1 Na2 79.57(9) . 2_766 ? O2 Si1 Na2 156.55(7) . 2_766 ? O6 Si1 Na2 42.52(7) . 2_766 ? O1 Si1 Na2 85.89(9) . 2_766 ? Na1 Si1 Na2 62.99(3) 1_665 2_766 ? O4 Si1 Ca 76.46(9) . 2_666 ? O2 Si1 Ca 41.21(7) . 2_666 ? O6 Si1 Ca 147.85(7) . 2_666 ? O1 Si1 Ca 105.26(8) . 2_666 ? Na1 Si1 Ca 139.60(2) 1_665 2_666 ? Na2 Si1 Ca 155.68(3) 2_766 2_666 ? O4 Si1 Ca 40.03(8) . . ? O2 Si1 Ca 128.76(7) . . ? O6 Si1 Ca 116.88(7) . . ? O1 Si1 Ca 67.94(9) . . ? Na1 Si1 Ca 100.50(2) 1_665 . ? Na2 Si1 Ca 74.37(3) 2_766 . ? Ca Si1 Ca 89.64(2) 2_666 . ? O4 Si1 Ca 137.10(9) . 1_565 ? O2 Si1 Ca 44.39(7) . 1_565 ? O6 Si1 Ca 111.42(7) . 1_565 ? O1 Si1 Ca 62.47(9) . 1_565 ? Na1 Si1 Ca 72.77(2) 1_665 1_565 ? Na2 Si1 Ca 135.76(3) 2_766 1_565 ? Ca Si1 Ca 67.62(2) 2_666 1_565 ? Ca Si1 Ca 115.48(3) . 1_565 ? O5 Si2 O3 116.69(13) . . ? O5 Si2 O7 109.96(12) . . ? O3 Si2 O7 113.80(10) . . ? O5 Si2 O1 107.49(12) . . ? O3 Si2 O1 106.06(11) . . ? O7 Si2 O1 101.41(11) . . ? O5 Si2 Na1 130.47(10) . 1_665 ? O3 Si2 Na1 112.09(8) . 1_665 ? O7 Si2 Na1 54.09(7) . 1_665 ? O1 Si2 Na1 48.79(8) . 1_665 ? O5 Si2 Na2 72.52(10) . . ? O3 Si2 Na2 157.98(8) . . ? O7 Si2 Na2 45.77(7) . . ? O1 Si2 Na2 88.60(9) . . ? Na1 Si2 Na2 65.34(3) 1_665 . ? O5 Si2 Ca 39.59(8) . . ? O3 Si2 Ca 126.71(8) . . ? O7 Si2 Ca 119.32(7) . . ? O1 Si2 Ca 67.94(9) . . ? Na1 Si2 Ca 101.99(3) 1_665 . ? Na2 Si2 Ca 73.73(3) . . ? O5 Si2 Ca 141.23(10) . 1_565 ? O3 Si2 Ca 45.17(7) . 1_565 ? O7 Si2 Ca 108.78(7) . 1_565 ? O1 Si2 Ca 62.90(9) . 1_565 ? Na1 Si2 Ca 73.82(2) 1_665 1_565 ? Na2 Si2 Ca 139.16(3) . 1_565 ? Ca Si2 Ca 115.85(3) . 1_565 ? Si2 O1 Si1 155.97(15) . . ? Si2 O1 Na1 100.32(10) . 1_665 ? Si1 O1 Na1 103.61(10) . 1_665 ? Si2 O1 Ca 88.26(10) . 1_565 ? Si1 O1 Ca 88.76(10) . 1_565 ? Na1 O1 Ca 92.13(8) 1_665 1_565 ? Si1 O2 Zr 129.64(10) . 1_565 ? Si1 O2 Ca 112.09(9) . 2_666 ? Zr O2 Ca 104.09(7) 1_565 2_666 ? Si1 O2 Ca 109.14(9) . 1_565 ? Zr O2 Ca 97.25(7) 1_565 1_565 ? Ca O2 Ca 100.06(7) 2_666 1_565 ? Si2 O3 Zr 129.97(10) . 1_564 ? Si2 O3 Zr 115.55(10) . 2_666 ? Zr O3 Zr 102.75(7) 1_564 2_666 ? Si2 O3 Ca 108.24(9) . 1_565 ? Zr O3 Ca 95.84(7) 1_564 1_565 ? Zr O3 Ca 98.57(7) 2_666 1_565 ? Si1 O4 Zr 134.67(12) . . ? Si1 O4 Ca 114.10(11) . . ? Zr O4 Ca 104.40(8) . . ? Si2 O5 Zr 139.46(13) . 1_554 ? Si2 O5 Ca 114.72(12) . . ? Zr O5 Ca 104.30(8) 1_554 . ? Si1 O6 Ti 141.29(12) . 1_666 ? Si1 O6 Ti 151.86(12) . 2_666 ? Ti O6 Ti 11.53(7) 1_666 2_666 ? Si1 O6 Na2 110.08(9) . 2_766 ? Ti O6 Na2 106.95(9) 1_666 2_766 ? Ti O6 Na2 95.43(8) 2_666 2_766 ? Si1 O6 Na1 92.71(8) . 1_665 ? Ti O6 Na1 102.00(12) 1_666 1_665 ? Ti O6 Na1 101.82(12) 2_666 1_665 ? Na2 O6 Na1 84.01(6) 2_766 1_665 ? Si2 O7 Ti 140.60(13) . 1_665 ? Si2 O7 Ti 149.94(13) . 2_665 ? Ti O7 Ti 11.57(7) 1_665 2_665 ? Si2 O7 Na2 104.92(9) . . ? Ti O7 Na2 107.71(9) 1_665 . ? Ti O7 Na2 96.16(8) 2_665 . ? Si2 O7 Na1 95.00(8) . 1_665 ? Ti O7 Na1 107.55(12) 1_665 1_665 ? Ti O7 Na1 107.12(12) 2_665 1_665 ? Na2 O7 Na1 87.95(6) . 1_665 ? Ti F1 Ti 1.03(19) 1_656 2_656 ? Ti F1 Zr 128.59(13) 1_656 . ? Ti F1 Zr 129.62(11) 2_656 . ? Ti F1 Na2 100.46(12) 1_656 1_556 ? Ti F1 Na2 99.90(10) 2_656 1_556 ? Zr F1 Na2 110.71(7) . 1_556 ? Ti F1 Na2 100.40(13) 1_656 2_766 ? Ti F1 Na2 99.62(11) 2_656 2_766 ? Zr F1 Na2 114.96(7) . 2_766 ? Na2 F1 Na2 96.37(6) 1_556 2_766 ? Na1 F2 Ca 119.62(7) 1_655 . ? Na1 F2 Na2 96.76(6) 1_655 . ? Ca F2 Na2 114.92(7) . . ? Na1 F2 Na2 97.03(6) 1_655 2_766 ? Ca F2 Na2 118.73(7) . 2_766 ? Na2 F2 Na2 106.28(7) . 2_766 ? _refine_diff_density_max 0.948 _refine_diff_density_min -0.573 _refine_diff_density_rms 0.114 _shelxl_version_number 2014-3 _shelx_res_file ; TITL "hainite" from Brazil CELL 0.71073 9.6151 5.7248 7.3162 89.906 101.141 100.905 ZERR 1 0.0028 0.0018 0.0022 0.010 0.011 0.011 LATT 1 SFAC CA F NA O SI TI NB ZR CE MN FE Y HF LA ND GD UNIT 4.19 2.76 2.03 15.24 4.07 .94 .06 .41 .06 .16 .06 .02 .01 .03 .02 .01 MERG 2 ACTA LIST 4 PLAN 20 SIZE 0.02 0.03 0.04 L.S. 10 WGHT 0.024400 0.851700 FVAR 0.56417 0.62450 1.14440 0.51641 1.32908 1.12317 ZR 8 0.632644 0.224345 0.909101 21.00000 0.01731 0.01695 = 0.01098 -0.00012 0.00269 -0.00288 CA 1 0.632478 0.230755 0.407316 31.00000 0.01468 0.02511 = 0.01123 -0.00279 0.00406 -0.00622 TI 6 -0.013094 0.023290 -0.003388 41.00000 0.00753 0.01017 = 0.00775 0.00022 0.00196 0.00231 NA1 3 0.000000 0.000000 0.500000 60.50000 0.00839 0.01465 = 0.02113 -0.00179 -0.00020 0.00305 NA2 3 0.994244 0.497003 0.242329 51.00000 0.02699 0.00860 = 0.00767 0.00133 0.00592 0.00936 SI1 5 0.716865 0.750214 0.651337 11.00000 0.01047 0.01268 = 0.00910 -0.00012 0.00180 0.00303 SI2 5 0.722736 0.754471 0.213257 11.00000 0.01172 0.01248 = 0.01011 0.00138 0.00401 0.00385 O1 4 0.755527 0.779046 0.441990 11.00000 0.02681 0.05528 = 0.01133 0.00096 0.00653 0.00247 O2 4 0.616118 0.941603 0.667852 11.00000 0.01372 0.01771 = 0.02280 -0.00252 0.00218 0.00701 O3 4 0.618065 0.936899 0.141076 11.00000 0.01802 0.02157 = 0.02326 0.00582 0.00381 0.01122 O4 4 0.641918 0.478563 0.668967 11.00000 0.03658 0.01659 = 0.02435 -0.00037 0.00672 -0.00614 O5 4 0.661321 0.479415 0.155753 11.00000 0.05405 0.01654 = 0.03080 -0.00361 0.01733 -0.00470 O6 4 0.876289 0.813823 0.783478 11.00000 0.01480 0.02327 = 0.01969 -0.00668 -0.00388 0.00713 O7 4 0.884156 0.832895 0.169905 11.00000 0.01671 0.02352 = 0.02143 0.00762 0.01029 0.00631 F1 2 0.884103 0.256852 0.967110 10.93111 0.01431 0.02108 = 0.01973 0.00023 0.00305 0.00524 F2 2 0.884226 0.304382 0.474404 11.00000 0.01763 0.02075 = 0.02753 0.00184 0.00436 0.00550 HKLF 4 REM "hainite" from Brazil REM R1 = 0.0319 for 2194 Fo > 4sig(Fo) and 0.0375 for all 2500 data REM 147 parameters refined using 0 restraints END WGHT 0.0244 0.8506 REM Highest difference peak 0.948, deepest hole -0.573, 1-sigma level 0.114 Q1 1 0.7161 0.6617 0.4296 11.00000 0.05 0.95 Q2 1 0.6297 0.1330 0.9735 11.00000 0.05 0.80 Q3 1 0.5956 0.2984 0.3983 11.00000 0.05 0.77 Q4 1 0.6167 0.1299 0.8462 11.00000 0.05 0.62 Q5 1 0.6632 0.2013 0.8280 11.00000 0.05 0.58 Q6 1 0.7181 0.8384 0.4236 11.00000 0.05 0.55 Q7 1 1.0474 0.5932 0.2978 11.00000 0.05 0.52 Q8 1 0.6345 0.1741 0.4757 11.00000 0.05 0.50 Q9 1 0.5851 0.2840 0.8964 11.00000 0.05 0.48 Q10 1 0.7017 0.2869 0.9623 11.00000 0.05 0.47 Q11 1 0.6018 0.5469 0.1094 11.00000 0.05 0.45 Q12 1 0.5474 0.8459 0.1326 11.00000 0.05 0.43 Q13 1 0.6711 0.2342 0.3593 11.00000 0.05 0.43 Q14 1 0.7938 0.7972 0.4537 11.00000 0.05 0.43 Q15 1 0.6213 0.3694 0.7013 11.00000 0.05 0.42 Q16 1 0.7239 0.7114 0.3460 11.00000 0.05 0.39 Q17 1 0.8039 0.8181 0.7410 11.00000 0.05 0.39 Q18 1 0.6218 0.4544 0.7646 11.00000 0.05 0.39 Q19 1 0.6997 0.5013 0.1780 11.00000 0.05 0.39 Q20 1 0.9565 0.4126 0.2962 11.00000 0.05 0.38 ; _shelx_res_checksum 89200 _shelx_hkl_file ; -1 0 0 0.1579 0.1441 1 0 0 0.0532 0.1140 -2 0 0 26.921 0.974 2 0 0 26.590 0.779 -3 0 0 5828.37 70.94 3 0 0 5797.54 58.31 -4 0 0 1275.13 16.97 4 0 0 1299.45 14.79 -5 0 0 182.92 5.04 5 0 0 201.51 3.37 -6 0 0 179.88 3.65 6 0 0 178.88 3.35 -7 0 0 45.980 2.932 7 0 0 44.477 2.409 -8 0 0 2386.91 40.13 8 0 0 2393.43 33.03 -9 0 0 12.562 2.062 9 0 0 11.758 1.590 -10 0 0 50.871 4.069 10 0 0 42.435 3.939 -11 0 0 688.74 16.06 11 0 0 670.11 16.61 -12 0 0 216.76 8.35 12 0 0 227.56 8.85 -13 0 0 2.1240 2.1554 13 0 0 0.1479 2.0694 13 -1 0 49.096 5.102 -13 1 0 58.721 5.275 12 -1 0 21.363 3.309 -12 1 0 25.517 3.324 11 -1 0 12.803 2.452 -11 1 0 17.910 2.693 10 -1 0 27.546 2.507 -10 1 0 33.602 3.408 9 -1 0 351.79 7.77 -9 1 0 361.88 7.55 8 -1 0 1015.86 15.95 -8 1 0 1018.39 15.60 7 -1 0 22.155 1.477 -7 1 0 21.045 1.703 6 -1 0 1628.55 19.07 -6 1 0 1598.62 22.03 5 -1 0 2461.46 27.86 -5 1 0 2503.06 32.19 4 -1 0 22.388 1.147 -4 1 0 24.836 1.064 3 -1 0 2435.07 26.64 -3 1 0 2404.75 30.80 2 -1 0 1128.47 9.72 -2 1 0 1141.16 14.72 1 -1 0 0.7291 0.1879 -1 1 0 1.0212 0.2334 0 -1 0 190.15 3.63 0 1 0 188.95 2.47 -1 -1 0 4.8769 0.4522 1 1 0 5.5245 0.3905 -2 -1 0 419.42 6.12 2 1 0 424.63 4.14 -3 -1 0 2153.31 27.36 3 1 0 2166.89 20.79 -4 -1 0 75.923 1.755 4 1 0 76.962 1.451 -5 -1 0 791.03 9.95 5 1 0 807.71 8.83 -6 -1 0 1056.41 13.43 6 1 0 1079.16 11.75 -7 -1 0 4.7433 0.8780 7 1 0 4.6932 0.8481 -8 -1 0 155.22 4.58 8 1 0 148.22 4.23 -9 -1 0 195.79 5.53 9 1 0 193.65 7.06 -10 -1 0 1.4234 1.5383 10 1 0 2.2123 1.6830 -11 -1 0 20.068 3.027 11 1 0 11.247 2.526 -12 -1 0 1.5814 1.9082 12 1 0 2.9599 2.3330 -13 -1 0 -0.3721 2.1048 13 1 0 0.7623 2.4282 13 -2 0 161.91 7.73 -13 2 0 168.15 6.06 12 -2 0 327.64 8.41 -12 2 0 311.55 8.14 11 -2 0 39.083 3.157 -11 2 0 39.970 3.094 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59.128 5.036 11 -4 0 335.75 10.78 -11 4 0 339.50 8.27 10 -4 0 59.687 4.823 -10 4 0 64.568 3.543 9 -4 0 4.3181 1.4160 -9 4 0 8.6728 1.6040 8 -4 0 492.05 9.74 -8 4 0 488.16 9.37 7 -4 0 87.747 4.335 -7 4 0 85.817 2.709 6 -4 0 1074.87 12.66 -6 4 0 1111.14 12.59 5 -4 0 10.872 0.792 -5 4 0 12.151 1.091 4 -4 0 31.655 1.186 -4 4 0 34.272 2.439 3 -4 0 2358.54 22.33 -3 4 0 2336.12 28.40 2 -4 0 1191.28 11.89 -2 4 0 1171.82 12.94 1 -4 0 56.016 4.153 0 -4 0 3707.86 37.99 0 4 0 3773.19 42.62 -1 -4 0 66.361 1.476 1 4 0 67.680 2.232 -2 -4 0 665.45 12.98 2 4 0 657.23 9.41 -3 -4 0 998.60 19.72 3 4 0 1000.45 11.31 -4 -4 0 -0.0332 0.7932 4 4 0 0.0008 0.5223 -5 -4 0 383.26 10.32 5 4 0 378.86 5.92 -6 -4 0 49.638 4.158 6 4 0 57.013 1.931 -7 -4 0 18.492 2.507 7 4 0 23.140 2.251 -8 -4 0 535.59 14.49 8 4 0 524.98 10.71 -9 -4 0 84.788 6.440 9 4 0 88.600 4.959 -10 -4 0 131.36 5.89 10 4 0 139.89 6.27 12 -5 0 36.503 4.474 -12 5 0 34.535 4.057 11 -5 0 26.254 3.821 -11 5 0 35.204 3.940 10 -5 0 153.93 6.80 -10 5 0 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-9 37.288 3.528 -6 3 9 38.128 4.388 5 -3 -9 45.580 2.765 -5 3 9 51.888 4.874 4 -3 -9 -0.3171 1.0019 -4 3 9 1.2116 1.8315 3 -3 -9 107.15 3.64 -3 3 9 105.98 6.25 2 -3 -9 10.902 2.165 -2 3 9 15.382 3.040 1 -3 -9 68.637 4.838 -1 3 9 74.474 6.003 0 -3 -9 19.127 2.839 0 3 9 15.853 3.139 -1 -3 -9 14.039 2.617 1 3 9 20.037 1.822 -2 -3 -9 5.7830 2.2274 2 3 9 3.4471 2.3393 6 -4 -9 19.829 3.001 -6 4 9 15.696 2.228 5 -4 -9 2.4243 1.9514 -5 4 9 1.8115 1.4155 4 -4 -9 81.720 3.392 -4 4 9 71.116 3.809 3 -4 -9 37.418 2.505 -3 4 9 32.353 2.711 2 -4 -9 13.173 2.596 -2 4 9 12.696 1.776 1 -4 -9 12.169 2.573 -1 4 9 13.972 1.951 5 2 -10 166.66 8.77 -5 -2 10 156.14 11.91 4 2 -10 146.38 4.96 -4 -2 10 154.75 11.61 3 2 -10 46.074 3.043 -3 -2 10 38.416 6.982 2 2 -10 180.11 5.60 -2 -2 10 180.45 8.21 1 2 -10 317.44 7.71 -1 -2 10 315.08 11.13 0 2 -10 19.535 2.268 0 -2 10 24.180 3.887 -1 2 -10 1.9672 1.3030 1 -2 10 0.0646 1.7577 6 1 -10 411.89 13.75 -6 -1 10 413.04 19.29 5 1 -10 33.246 2.766 -5 -1 10 30.451 6.209 4 1 -10 -1.380 1.199 -4 -1 10 -0.3022 2.7028 3 1 -10 292.52 7.28 -3 -1 10 292.71 10.49 2 1 -10 0.3133 1.1454 -2 -1 10 0.1448 2.0276 1 1 -10 125.40 4.05 -1 -1 10 118.28 6.69 0 1 -10 110.88 4.04 0 -1 10 106.75 5.92 -1 1 -10 34.900 2.555 1 -1 10 33.838 3.585 -2 1 -10 286.78 6.54 2 -1 10 270.53 8.49 7 0 -10 53.549 8.373 -7 0 10 49.359 5.143 6 0 -10 6.5285 4.1621 -6 0 10 6.8435 3.6987 5 0 -10 53.686 3.165 -5 0 10 54.011 7.727 4 0 -10 116.01 4.37 -4 0 10 114.70 11.04 3 0 -10 103.43 3.90 -3 0 10 103.17 6.99 2 0 -10 141.53 4.30 -2 0 10 134.50 6.96 1 0 -10 82.732 3.424 -1 0 10 82.769 6.387 0 0 -10 53.373 2.781 0 0 10 43.919 4.756 -1 0 -10 0.8168 1.1172 1 0 10 0.1888 1.7750 -2 0 -10 29.328 3.448 2 0 10 23.387 3.195 7 -1 -10 267.21 15.73 -7 1 10 271.35 10.32 6 -1 -10 29.414 6.517 -6 1 10 41.663 4.679 5 -1 -10 93.770 4.552 -5 1 10 98.552 10.096 4 -1 -10 112.22 4.32 -4 1 10 115.90 6.71 3 -1 -10 1.6427 1.2121 -3 1 10 1.0017 1.8557 2 -1 -10 364.59 8.24 -2 1 10 364.21 11.99 1 -1 -10 1.1925 1.1102 -1 1 10 1.1128 2.0946 0 -1 -10 25.797 2.357 0 1 10 25.684 4.006 -1 -1 -10 395.91 13.43 1 1 10 401.89 12.89 6 -2 -10 -2.153 2.215 -6 2 10 0.6556 2.2843 5 -2 -10 36.871 2.582 -5 2 10 37.861 4.527 4 -2 -10 376.87 7.63 -4 2 10 374.23 12.30 3 -2 -10 112.77 3.93 -3 2 10 110.89 6.89 2 -2 -10 40.017 2.497 -2 2 10 43.603 4.835 1 -2 -10 157.34 6.59 -1 2 10 157.90 7.73 0 -2 -10 126.56 7.89 0 2 10 134.20 8.17 0 0 0 0.00 0.00 0 ; _shelx_hkl_checksum 58123 Validation response form Please find below a validation response form (VRF) that can be filled in and pasted into your CIF. # start Validation Reply Form _vrf_ABSMU01_bortolanite ; PROBLEM: The ratio of given/expected absorption coefficient lies RESPONSE: The chemical formula of bortolanite was determined by electron-microprobe analysis and is given in the CIF (Z = 1). Calculated value of Mu is based on formal s.o.f. values which do not take into account heavier scatters at several sites ; _vrf_CHEMW01_bortolanite ; PROBLEM: The ratio of given/expected molecular weight as calculated RESPONSE: The chemical formula of bortolanite was determined by electron-microprobe analysis and is given in the CIF (Z = 1). Calculated value of formula weight is based on formal s.o.f. values which do not take into account heavier scatters at several sites. ; _vrf_PLAT051_bortolanite ; PROBLEM: Mu(calc) and Mu(CIF) Ratio Differs from 1.0 by . 21.43 % RESPONSE: The chemical formula of bortolanite was determined by electron-microprobe analysis and is given in the CIF (Z = 1). Calculated value of Mu is based on formal s.o.f. values which do not take into account heavier scatters at several sites ; _vrf_PLAT075_bortolanite ; PROBLEM: Occupancy 1.144 Greater Than 1.0 for ...... CA RESPONSE: Many sites are occupied by several cations, and the site occupancies cannot be determined solely from s.o.f. values. They must be assigned on crystal-chemical grounds (e.g., mean bondlengths, known solid-solution behaviour, etc.) using the chemical formula and the refined s.o.f. values as constraints. We handle this by (1) determining the dominant cation at a site, (2) refining its s.o.f. with that scattering species, and (3) assigning additional species to that site on the basis of the total refined scattering at that site, the known chemical composition of the crystal, and ionic-radii - mean-bondlength considerations. For example, Ca is dominantly occupied by Ca, but the somewhat higher refined s.o.f. 1.144 versus a maximum of 1.0 for complete occupancy by Ca indicates small occupancy by 0.06REE: Ca0.94REE0.06, where 0.06REE = 1/2(La0.03Ce0.06Nd0.02Gd0.01). We use the "excess" scattering to determine on average how much Ca is present at this site. Many years of experience have shown that this is the best way that minerals with complex chemical compositions are handled. This is the origin of the "occupancy greater than 1.0" message. ; # end Validation Reply Form