data_shakhdaraite-(Y) _audit_creation_method SHELXL-2014 _chemical_name_systematic ; ? ; _chemical_name_common shakhdaraite-(Y) _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'Ca0.09 Ho0.25 Mn0.10 Nb1.91 O8 Pb0.01 Sc0.83 Sn0.05 Ta0.10 Th0.04 Ti0.01 U0.06 W0.02 Y0.53' _chemical_formula_weight 493.87 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Sc' 'Sc' 0.2519 0.3716 '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' 'Nb' 'Nb' -2.0727 0.6215 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system monoclinic _space_group_IT_number 13 _space_group_name_H-M_alt 'P 2/c' _space_group_name_Hall '-P 2yc' _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+1/2' '-x, -y, -z' 'x, -y, z-1/2' _cell_length_a 9.930(6) _cell_length_b 5.662(3) _cell_length_c 5.211(3) _cell_angle_alpha 90 _cell_angle_beta 92.383(7) _cell_angle_gamma 90 _cell_volume 292.7(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5159 _cell_measurement_theta_min 3.598 _cell_measurement_theta_max 31.143 _exptl_crystal_description tabular _exptl_crystal_colour 'black to dark-brown' _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_density_diffrn 5.602 _exptl_crystal_F_000 445.6 _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 7.372 _shelx_estimated_absorpt_T_min 0.757 _shelx_estimated_absorpt_T_max 0.867 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.5747 _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 3546 _diffrn_reflns_av_unetI/netI 0.0143 _diffrn_reflns_av_R_equivalents 0.0166 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -7 _diffrn_reflns_limit_l_max 7 _diffrn_reflns_theta_min 3.598 _diffrn_reflns_theta_max 31.199 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measured_fraction_theta_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.998 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.998 _diffrn_reflns_point_group_measured_fraction_full 0.998 _reflns_number_total 948 _reflns_number_gt 878 _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 'SHELXL-2014 (Sheldrick, 2014)' _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^)+(0.0205P)^2^+1.9183P] 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 948 _refine_ls_number_parameters 75 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0316 _refine_ls_R_factor_gt 0.0269 _refine_ls_wR_factor_ref 0.0628 _refine_ls_wR_factor_gt 0.0603 _refine_ls_goodness_of_fit_ref 1.157 _refine_ls_restrained_S_all 1.157 _refine_ls_shift/su_max 0.044 _refine_ls_shift/su_mean 0.011 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 Y1 Y 0.5000 0.7706(9) 0.2500 0.0125(5) Uani 0.99(4) 2 d S T . . . Y2 Y 0.5000 0.820(6) 0.2500 0.026(3) Uani 0.24(4) 2 d S T . . . Nb1 Nb 0.75537(18) 0.3147(4) 0.2262(8) 0.0136(4) Uani 0.90(2) 1 d . . . . . Nb2 Nb 0.746(2) 0.291(4) 0.278(6) 0.026(3) Uani 0.10(2) 1 d . . . . . Sc Sc 0.0000 0.81831(14) 0.2500 0.0178(2) Uani 1.469(13) 2 d S T . . . O1 O 0.6246(4) 1.0980(6) 0.0913(7) 0.0274(8) Uani 1 1 d . . . . . O2 O 0.6381(4) 0.5794(7) 0.0123(9) 0.0394(11) Uani 1 1 d . . . . . O3 O 0.8621(4) 0.3885(6) -0.0824(6) 0.0244(8) Uani 1 1 d . . . . . O4 O 0.8855(3) 0.1145(6) 0.4082(6) 0.0240(8) 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 Y1 0.0128(5) 0.0151(10) 0.0097(6) 0.000 0.0007(3) 0.000 Y2 0.025(3) 0.026(7) 0.029(3) 0.000 0.0045(15) 0.000 Nb1 0.0147(3) 0.0139(4) 0.0118(7) 0.0017(4) -0.0031(3) -0.0001(2) Nb2 0.030(5) 0.035(5) 0.013(5) 0.011(4) -0.002(3) -0.001(3) Sc 0.0168(4) 0.0202(4) 0.0164(4) 0.000 0.0000(3) 0.000 O1 0.0326(19) 0.0228(16) 0.0269(17) -0.0006(13) 0.0025(13) -0.0014(14) O2 0.0269(19) 0.036(2) 0.055(3) 0.0210(19) -0.0025(17) 0.0023(16) O3 0.0279(17) 0.0201(15) 0.0248(16) 0.0025(12) -0.0016(12) 0.0024(13) O4 0.0242(16) 0.0215(15) 0.0262(16) -0.0039(12) -0.0002(12) -0.0006(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Y1 Y2 0.28(3) . ? Y1 O2 2.175(5) . ? Y1 O2 2.175(5) 2_655 ? Y1 O1 2.251(4) 4_576 ? Y1 O1 2.251(4) 3_675 ? Y1 O1 2.395(5) . ? Y1 O1 2.395(5) 2_655 ? Y1 O2 2.742(6) 3_665 ? Y1 O2 2.742(6) 4_566 ? Y1 Y2 3.49(2) 3_676 ? Y1 Y2 3.49(2) 3_675 ? Y1 Nb1 3.507(3) 3_665 ? Y2 O1 2.174(8) 4_576 ? Y2 O1 2.174(8) 3_675 ? Y2 O1 2.19(2) . ? Y2 O1 2.19(2) 2_655 ? Y2 O2 2.33(2) . ? Y2 O2 2.33(2) 2_655 ? Y2 Y2 3.31(4) 3_676 ? Y2 Y2 3.31(4) 3_675 ? Y2 Y1 3.49(2) 3_676 ? Y2 Y1 3.49(2) 3_675 ? Y2 Nb1 3.556(8) 3_665 ? Nb1 Nb2 0.32(3) . ? Nb1 O1 1.899(4) 1_545 ? Nb1 O4 1.937(4) . ? Nb1 O3 2.007(5) . ? Nb1 O2 2.021(5) 4_566 ? Nb1 O2 2.176(5) . ? Nb1 O3 2.203(4) 4_566 ? Nb1 Nb2 3.228(17) 4_565 ? Nb1 Nb1 3.346(3) 4_565 ? Nb1 Nb1 3.346(3) 4_566 ? Nb1 Y1 3.507(3) 3_665 ? Nb1 Y2 3.556(8) 3_665 ? Nb2 O4 1.819(18) . ? Nb2 O2 1.81(3) 4_566 ? Nb2 O1 1.869(18) 1_545 ? Nb2 O3 2.25(2) 4_566 ? Nb2 O3 2.31(4) . ? Nb2 O2 2.37(2) . ? Nb2 Nb1 3.228(17) 4_566 ? Nb2 Sc 3.51(2) 3_666 ? Nb2 Y1 3.55(3) 3_666 ? Nb2 Y2 3.59(4) 3_666 ? Nb2 Y1 3.618(19) 3_665 ? Sc O3 2.027(3) 4_466 ? Sc O3 2.027(3) 3_665 ? Sc O4 2.108(3) 3_666 ? Sc O4 2.108(3) 4_465 ? Sc O4 2.205(3) 2_665 ? Sc O4 2.205(3) 1_465 ? Sc Sc 3.3199(17) 3_576 ? Sc Sc 3.3199(17) 3_575 ? Sc Nb2 3.51(2) 4_465 ? Sc Nb2 3.51(2) 3_666 ? O1 Nb2 1.869(18) 1_565 ? O1 Nb1 1.900(4) 1_565 ? O1 Y2 2.174(8) 3_675 ? O1 Y1 2.251(4) 3_675 ? O2 Nb2 1.81(3) 4_565 ? O2 Nb1 2.021(5) 4_565 ? O2 Y1 2.742(6) 3_665 ? O3 Sc 2.027(3) 3_665 ? O3 Nb1 2.203(4) 4_565 ? O3 Nb2 2.25(2) 4_565 ? O4 Sc 2.108(3) 3_666 ? O4 Sc 2.205(3) 1_645 ? 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 Y2 Y1 O2 119.87(15) . . ? Y2 Y1 O2 119.87(17) . 2_655 ? O2 Y1 O2 120.3(3) . 2_655 ? Y2 Y1 O1 70.70(15) . 4_576 ? O2 Y1 O1 106.00(15) . 4_576 ? O2 Y1 O1 93.07(15) 2_655 4_576 ? Y2 Y1 O1 70.70(16) . 3_675 ? O2 Y1 O1 93.07(15) . 3_675 ? O2 Y1 O1 106.00(15) 2_655 3_675 ? O1 Y1 O1 141.4(3) 4_576 3_675 ? Y2 Y1 O1 39.29(11) . . ? O2 Y1 O1 80.89(14) . . ? O2 Y1 O1 158.3(2) 2_655 . ? O1 Y1 O1 75.04(15) 4_576 . ? O1 Y1 O1 75.31(18) 3_675 . ? Y2 Y1 O1 39.29(13) . 2_655 ? O2 Y1 O1 158.3(2) . 2_655 ? O2 Y1 O1 80.89(14) 2_655 2_655 ? O1 Y1 O1 75.31(18) 4_576 2_655 ? O1 Y1 O1 75.04(15) 3_675 2_655 ? O1 Y1 O1 78.6(2) . 2_655 ? Y2 Y1 O2 136.27(12) . 3_665 ? O2 Y1 O2 70.76(19) . 3_665 ? O2 Y1 O2 67.04(14) 2_655 3_665 ? O1 Y1 O2 151.6(2) 4_576 3_665 ? O1 Y1 O2 66.29(13) 3_675 3_665 ? O1 Y1 O2 129.95(12) . 3_665 ? O1 Y1 O2 118.46(13) 2_655 3_665 ? Y2 Y1 O2 136.27(11) . 4_566 ? O2 Y1 O2 67.04(14) . 4_566 ? O2 Y1 O2 70.76(19) 2_655 4_566 ? O1 Y1 O2 66.29(13) 4_576 4_566 ? O1 Y1 O2 151.6(2) 3_675 4_566 ? O1 Y1 O2 118.46(13) . 4_566 ? O1 Y1 O2 129.95(12) 2_655 4_566 ? O2 Y1 O2 87.5(2) 3_665 4_566 ? Y2 Y1 Y2 48.3(4) . 3_676 ? O2 Y1 Y2 140.91(14) . 3_676 ? O2 Y1 Y2 83.4(3) 2_655 3_676 ? O1 Y1 Y2 37.53(17) 4_576 3_676 ? O1 Y1 Y2 110.7(5) 3_675 3_676 ? O1 Y1 Y2 76.1(4) . 3_676 ? O1 Y1 Y2 38.0(3) 2_655 3_676 ? O2 Y1 Y2 146.8(2) 3_665 3_676 ? O2 Y1 Y2 97.1(4) 4_566 3_676 ? Y2 Y1 Y2 48.3(4) . 3_675 ? O2 Y1 Y2 83.4(3) . 3_675 ? O2 Y1 Y2 140.91(14) 2_655 3_675 ? O1 Y1 Y2 110.7(5) 4_576 3_675 ? O1 Y1 Y2 37.53(17) 3_675 3_675 ? O1 Y1 Y2 38.0(3) . 3_675 ? O1 Y1 Y2 76.1(4) 2_655 3_675 ? O2 Y1 Y2 97.1(4) 3_665 3_675 ? O2 Y1 Y2 146.8(2) 4_566 3_675 ? Y2 Y1 Y2 96.7(9) 3_676 3_675 ? Y2 Y1 Nb1 97.91(10) . 3_665 ? O2 Y1 Nb1 89.03(14) . 3_665 ? O2 Y1 Nb1 83.10(14) 2_655 3_665 ? O1 Y1 Nb1 164.24(18) 4_576 3_665 ? O1 Y1 Nb1 29.38(11) 3_675 3_665 ? O1 Y1 Nb1 103.36(13) . 3_665 ? O1 Y1 Nb1 88.97(11) 2_655 3_665 ? O2 Y1 Nb1 38.36(9) 3_665 3_665 ? O2 Y1 Nb1 125.81(18) 4_566 3_665 ? Y2 Y1 Nb1 126.7(2) 3_676 3_665 ? Y2 Y1 Nb1 65.5(2) 3_675 3_665 ? Y1 Y2 O1 102.3(8) . 4_576 ? Y1 Y2 O1 102.3(8) . 3_675 ? O1 Y2 O1 155.4(17) 4_576 3_675 ? Y1 Y2 O1 136.0(6) . . ? O1 Y2 O1 81.0(7) 4_576 . ? O1 Y2 O1 81.3(7) 3_675 . ? Y1 Y2 O1 136.0(6) . 2_655 ? O1 Y2 O1 81.3(7) 4_576 2_655 ? O1 Y2 O1 81.0(7) 3_675 2_655 ? O1 Y2 O1 87.9(12) . 2_655 ? Y1 Y2 O2 54.1(7) . . ? O1 Y2 O2 103.4(4) 4_576 . ? O1 Y2 O2 91.0(4) 3_675 . ? O1 Y2 O2 82.23(15) . . ? O1 Y2 O2 168.2(11) 2_655 . ? Y1 Y2 O2 54.1(7) . 2_655 ? O1 Y2 O2 91.0(4) 4_576 2_655 ? O1 Y2 O2 103.4(4) 3_675 2_655 ? O1 Y2 O2 168.2(11) . 2_655 ? O1 Y2 O2 82.23(15) 2_655 2_655 ? O2 Y2 O2 108.3(13) . 2_655 ? Y1 Y2 Y2 128.0(9) . 3_676 ? O1 Y2 Y2 40.79(19) 4_576 3_676 ? O1 Y2 Y2 119.6(14) 3_675 3_676 ? O1 Y2 Y2 82.7(12) . 3_676 ? O1 Y2 Y2 40.5(5) 2_655 3_676 ? O2 Y2 Y2 143.08(11) . 3_676 ? O2 Y2 Y2 85.5(2) 2_655 3_676 ? Y1 Y2 Y2 128.0(9) . 3_675 ? O1 Y2 Y2 119.6(14) 4_576 3_675 ? O1 Y2 Y2 40.79(19) 3_675 3_675 ? O1 Y2 Y2 40.5(5) . 3_675 ? O1 Y2 Y2 82.7(12) 2_655 3_675 ? O2 Y2 Y2 85.5(2) . 3_675 ? O2 Y2 Y2 143.08(11) 2_655 3_675 ? Y2 Y2 Y2 104.0(18) 3_676 3_675 ? Y1 Y2 Y1 131.7(4) . 3_676 ? O1 Y2 Y1 42.7(4) 4_576 3_676 ? O1 Y2 Y1 116.9(11) 3_675 3_676 ? O1 Y2 Y1 79.7(8) . 3_676 ? O1 Y2 Y1 38.8(3) 2_655 3_676 ? O2 Y2 Y1 143.7(2) . 3_676 ? O2 Y2 Y1 88.5(2) 2_655 3_676 ? Y2 Y2 Y1 3.6(5) 3_676 3_676 ? Y2 Y2 Y1 100.3(13) 3_675 3_676 ? Y1 Y2 Y1 131.7(4) . 3_675 ? O1 Y2 Y1 116.9(11) 4_576 3_675 ? O1 Y2 Y1 42.7(4) 3_675 3_675 ? O1 Y2 Y1 38.8(3) . 3_675 ? O1 Y2 Y1 79.7(8) 2_655 3_675 ? O2 Y2 Y1 88.5(2) . 3_675 ? O2 Y2 Y1 143.7(2) 2_655 3_675 ? Y2 Y2 Y1 100.3(13) 3_676 3_675 ? Y2 Y2 Y1 3.6(5) 3_675 3_675 ? Y1 Y2 Y1 96.7(9) 3_676 3_675 ? Y1 Y2 Nb1 77.6(5) . 3_665 ? O1 Y2 Nb1 169.03(11) 4_576 3_665 ? O1 Y2 Nb1 27.1(3) 3_675 3_665 ? O1 Y2 Nb1 106.8(4) . 3_665 ? O1 Y2 Nb1 91.1(2) 2_655 3_665 ? O2 Y2 Nb1 85.5(5) . 3_665 ? O2 Y2 Nb1 80.0(4) 2_655 3_665 ? Y2 Y2 Nb1 131.2(6) 3_676 3_665 ? Y2 Y2 Nb1 66.79(18) 3_675 3_665 ? Y1 Y2 Nb1 129.9(5) 3_676 3_665 ? Y1 Y2 Nb1 69.11(15) 3_675 3_665 ? Nb2 Nb1 O1 80(3) . 1_545 ? Nb2 Nb1 O4 64(4) . . ? O1 Nb1 O4 103.6(2) 1_545 . ? Nb2 Nb1 O3 162(4) . . ? O1 Nb1 O3 102.3(2) 1_545 . ? O4 Nb1 O3 98.65(17) . . ? Nb2 Nb1 O2 45(3) . 4_566 ? O1 Nb1 O2 93.4(2) 1_545 4_566 ? O4 Nb1 O2 101.9(3) . 4_566 ? O3 Nb1 O2 150.4(2) . 4_566 ? Nb2 Nb1 O2 123(3) . . ? O1 Nb1 O2 84.98(18) 1_545 . ? O4 Nb1 O2 170.2(2) . . ? O3 Nb1 O2 74.6(2) . . ? O2 Nb1 O2 82.00(13) 4_566 . ? Nb2 Nb1 O3 95(3) . 4_566 ? O1 Nb1 O3 165.60(18) 1_545 4_566 ? O4 Nb1 O3 85.76(15) . 4_566 ? O3 Nb1 O3 86.76(16) . 4_566 ? O2 Nb1 O3 73.78(16) 4_566 4_566 ? O2 Nb1 O3 86.77(18) . 4_566 ? Nb2 Nb1 Nb2 154(4) . 4_565 ? O1 Nb1 Nb2 100.3(4) 1_545 4_565 ? O4 Nb1 Nb2 139.3(4) . 4_565 ? O3 Nb1 Nb2 43.7(5) . 4_565 ? O2 Nb1 Nb2 109.1(7) 4_566 4_565 ? O2 Nb1 Nb2 32.3(6) . 4_565 ? O3 Nb1 Nb2 78.4(5) 4_566 4_565 ? Nb2 Nb1 Nb1 158(3) . 4_565 ? O1 Nb1 Nb1 98.00(14) 1_545 4_565 ? O4 Nb1 Nb1 136.61(14) . 4_565 ? O3 Nb1 Nb1 39.47(10) . 4_565 ? O2 Nb1 Nb1 114.0(2) 4_566 4_565 ? O2 Nb1 Nb1 35.56(16) . 4_565 ? O3 Nb1 Nb1 81.86(18) 4_566 4_565 ? Nb2 Nb1 Nb1 5.2(6) 4_565 4_565 ? Nb2 Nb1 Nb1 66(3) . 4_566 ? O1 Nb1 Nb1 132.16(15) 1_545 4_566 ? O4 Nb1 Nb1 90.43(14) . 4_566 ? O3 Nb1 Nb1 120.69(13) . 4_566 ? O2 Nb1 Nb1 38.78(11) 4_566 4_566 ? O2 Nb1 Nb1 87.10(14) . 4_566 ? O3 Nb1 Nb1 35.37(12) 4_566 4_566 ? Nb2 Nb1 Nb1 97.4(6) 4_565 4_566 ? Nb1 Nb1 Nb1 102.29(13) 4_565 4_566 ? Nb2 Nb1 Y1 108(4) . 3_665 ? O1 Nb1 Y1 35.54(15) 1_545 3_665 ? O4 Nb1 Y1 135.56(14) . 3_665 ? O3 Nb1 Y1 81.50(15) . 3_665 ? O2 Nb1 Y1 98.11(14) 4_566 3_665 ? O2 Nb1 Y1 51.44(15) . 3_665 ? O3 Nb1 Y1 138.20(17) 4_566 3_665 ? Nb2 Nb1 Y1 65.5(3) 4_565 3_665 ? Nb1 Nb1 Y1 63.82(8) 4_565 3_665 ? Nb1 Nb1 Y1 127.88(7) 4_566 3_665 ? Nb2 Nb1 Y2 106(3) . 3_665 ? O1 Nb1 Y2 31.4(5) 1_545 3_665 ? O4 Nb1 Y2 131.1(5) . 3_665 ? O3 Nb1 Y2 82.57(19) . 3_665 ? O2 Nb1 Y2 99.35(19) 4_566 3_665 ? O2 Nb1 Y2 55.9(5) . 3_665 ? O3 Nb1 Y2 142.7(5) 4_566 3_665 ? Nb2 Nb1 Y2 69.2(5) 4_565 3_665 ? Nb1 Nb1 Y2 67.3(4) 4_565 3_665 ? Nb1 Nb1 Y2 130.9(3) 4_566 3_665 ? Y1 Nb1 Y2 4.5(5) 3_665 3_665 ? Nb1 Nb2 O4 107(4) . . ? Nb1 Nb2 O2 128(4) . 4_566 ? O4 Nb2 O2 115.7(16) . 4_566 ? Nb1 Nb2 O1 91(3) . 1_545 ? O4 Nb2 O1 109.6(10) . 1_545 ? O2 Nb2 O1 101.7(13) 4_566 1_545 ? Nb1 Nb2 O3 77(4) . 4_566 ? O4 Nb2 O3 87.1(7) . 4_566 ? O2 Nb2 O3 76.5(6) 4_566 4_566 ? O1 Nb2 O3 161.6(14) 1_545 4_566 ? Nb1 Nb2 O3 15(3) . . ? O4 Nb2 O3 92.0(11) . . ? O2 Nb2 O3 141.3(13) 4_566 . ? O1 Nb2 O3 92.8(11) 1_545 . ? O3 Nb2 O3 78.7(10) 4_566 . ? Nb1 Nb2 O2 50(3) . . ? O4 Nb2 O2 156.4(19) . . ? O2 Nb2 O2 81.4(7) 4_566 . ? O1 Nb2 O2 80.4(7) 1_545 . ? O3 Nb2 O2 81.2(8) 4_566 . ? O3 Nb2 O2 65.7(9) . . ? Nb1 Nb2 Nb1 109(4) . 4_566 ? O4 Nb2 Nb1 96.4(8) . 4_566 ? O2 Nb2 Nb1 39.9(4) 4_566 4_566 ? O1 Nb2 Nb1 141.3(12) 1_545 4_566 ? O3 Nb2 Nb1 37.9(4) 4_566 4_566 ? O3 Nb2 Nb1 115.0(9) . 4_566 ? O2 Nb2 Nb1 86.9(5) . 4_566 ? Nb1 Nb2 Sc 116(4) . 3_666 ? O4 Nb2 Sc 29.0(4) . 3_666 ? O2 Nb2 Sc 91.5(9) 4_566 3_666 ? O1 Nb2 Sc 133.7(11) 1_545 3_666 ? O3 Nb2 Sc 64.6(4) 4_566 3_666 ? O3 Nb2 Sc 104.0(7) . 3_666 ? O2 Nb2 Sc 145.8(8) . 3_666 ? Nb1 Nb2 Sc 67.4(4) 4_566 3_666 ? Nb1 Nb2 Y1 150(4) . 3_666 ? O4 Nb2 Y1 102.9(14) . 3_666 ? O2 Nb2 Y1 29.7(7) 4_566 3_666 ? O1 Nb2 Y1 81.8(11) 1_545 3_666 ? O3 Nb2 Y1 102.3(9) 4_566 3_666 ? O3 Nb2 Y1 165.1(8) . 3_666 ? O2 Nb2 Y1 99.6(7) . 3_666 ? Nb1 Nb2 Y1 64.4(5) 4_566 3_666 ? Sc Nb2 Y1 89.6(7) 3_666 3_666 ? Nb1 Nb2 Y2 153(4) . 3_666 ? O4 Nb2 Y2 100.2(14) . 3_666 ? O2 Nb2 Y2 34.1(9) 4_566 3_666 ? O1 Nb2 Y2 79.2(11) 1_545 3_666 ? O3 Nb2 Y2 105.9(10) 4_566 3_666 ? O3 Nb2 Y2 167.1(8) . 3_666 ? O2 Nb2 Y2 102.6(8) . 3_666 ? Nb1 Nb2 Y2 68.1(7) 4_566 3_666 ? Sc Nb2 Y2 88.8(7) 3_666 3_666 ? Y1 Nb2 Y2 4.5(5) 3_666 3_666 ? Nb1 Nb2 Y1 67(3) . 3_665 ? O4 Nb2 Y1 135.2(8) . 3_665 ? O2 Nb2 Y1 98.8(7) 4_566 3_665 ? O1 Nb2 Y1 31.6(5) 1_545 3_665 ? O3 Nb2 Y1 130.1(10) 4_566 3_665 ? O3 Nb2 Y1 75.5(7) . 3_665 ? O2 Nb2 Y1 49.3(4) . 3_665 ? Nb1 Nb2 Y1 128.0(5) 4_566 3_665 ? Sc Nb2 Y1 163.7(6) 3_666 3_665 ? Y1 Nb2 Y1 93.2(5) 3_666 3_665 ? Y2 Nb2 Y1 92.7(6) 3_666 3_665 ? O3 Sc O3 109.4(2) 4_466 3_665 ? O3 Sc O4 95.19(14) 4_466 3_666 ? O3 Sc O4 96.79(14) 3_665 3_666 ? O3 Sc O4 96.79(14) 4_466 4_465 ? O3 Sc O4 95.19(14) 3_665 4_465 ? O4 Sc O4 159.19(19) 3_666 4_465 ? O3 Sc O4 165.58(13) 4_466 2_665 ? O3 Sc O4 84.86(13) 3_665 2_665 ? O4 Sc O4 84.85(11) 3_666 2_665 ? O4 Sc O4 79.35(14) 4_465 2_665 ? O3 Sc O4 84.86(13) 4_466 1_465 ? O3 Sc O4 165.58(14) 3_665 1_465 ? O4 Sc O4 79.35(14) 3_666 1_465 ? O4 Sc O4 84.85(11) 4_465 1_465 ? O4 Sc O4 80.97(18) 2_665 1_465 ? O3 Sc Sc 89.89(10) 4_466 3_576 ? O3 Sc Sc 135.91(10) 3_665 3_576 ? O4 Sc Sc 40.75(9) 3_666 3_576 ? O4 Sc Sc 122.26(10) 4_465 3_576 ? O4 Sc Sc 80.72(10) 2_665 3_576 ? O4 Sc Sc 38.60(9) 1_465 3_576 ? O3 Sc Sc 135.91(10) 4_466 3_575 ? O3 Sc Sc 89.89(10) 3_665 3_575 ? O4 Sc Sc 122.26(10) 3_666 3_575 ? O4 Sc Sc 40.75(9) 4_465 3_575 ? O4 Sc Sc 38.60(9) 2_665 3_575 ? O4 Sc Sc 80.72(10) 1_465 3_575 ? Sc Sc Sc 103.40(6) 3_576 3_575 ? O3 Sc Nb2 73.8(4) 4_466 4_465 ? O3 Sc Nb2 94.3(6) 3_665 4_465 ? O4 Sc Nb2 166.5(6) 3_666 4_465 ? O4 Sc Nb2 24.7(3) 4_465 4_465 ? O4 Sc Nb2 103.9(3) 2_665 4_465 ? O4 Sc Nb2 91.7(5) 1_465 4_465 ? Sc Sc Nb2 129.5(6) 3_576 4_465 ? Sc Sc Nb2 65.3(3) 3_575 4_465 ? O3 Sc Nb2 94.3(6) 4_466 3_666 ? O3 Sc Nb2 73.8(4) 3_665 3_666 ? O4 Sc Nb2 24.7(3) 3_666 3_666 ? O4 Sc Nb2 166.5(6) 4_465 3_666 ? O4 Sc Nb2 91.7(5) 2_665 3_666 ? O4 Sc Nb2 103.9(3) 1_465 3_666 ? Sc Sc Nb2 65.3(3) 3_576 3_666 ? Sc Sc Nb2 129.5(6) 3_575 3_666 ? Nb2 Sc Nb2 159.6(7) 4_465 3_666 ? Nb2 O1 Nb1 9.7(10) 1_565 1_565 ? Nb2 O1 Y2 129.3(12) 1_565 3_675 ? Nb1 O1 Y2 121.5(8) 1_565 3_675 ? Nb2 O1 Y2 125.9(11) 1_565 . ? Nb1 O1 Y2 135.6(3) 1_565 . ? Y2 O1 Y2 98.7(7) 3_675 . ? Nb2 O1 Y1 122.6(9) 1_565 3_675 ? Nb1 O1 Y1 115.1(2) 1_565 3_675 ? Y2 O1 Y1 7.0(8) 3_675 3_675 ? Y2 O1 Y1 103.6(3) . 3_675 ? Nb2 O1 Y1 127.1(11) 1_565 . ? Nb1 O1 Y1 136.6(2) 1_565 . ? Y2 O1 Y1 99.4(7) 3_675 . ? Y2 O1 Y1 4.7(6) . . ? Y1 O1 Y1 104.69(19) 3_675 . ? Nb2 O2 Nb1 7.2(9) 4_565 4_565 ? Nb2 O2 Nb1 107.8(7) 4_565 . ? Nb1 O2 Nb1 105.7(2) 4_565 . ? Nb2 O2 Y1 125.9(9) 4_565 . ? Nb1 O2 Y1 132.0(2) 4_565 . ? Nb1 O2 Y1 112.8(2) . . ? Nb2 O2 Y2 120.0(11) 4_565 . ? Nb1 O2 Y2 126.1(7) 4_565 . ? Nb1 O2 Y2 116.5(4) . . ? Y1 O2 Y2 6.0(6) . . ? Nb2 O2 Nb2 114.1(13) 4_565 . ? Nb1 O2 Nb2 112.1(8) 4_565 . ? Nb1 O2 Nb2 6.5(7) . . ? Y1 O2 Nb2 106.9(7) . . ? Y2 O2 Nb2 110.7(8) . . ? Nb2 O2 Y1 104.7(9) 4_565 3_665 ? Nb1 O2 Y1 98.0(2) 4_565 3_665 ? Nb1 O2 Y1 90.19(17) . 3_665 ? Y1 O2 Y1 109.24(19) . 3_665 ? Y2 O2 Y1 113.3(5) . 3_665 ? Nb2 O2 Y1 89.9(5) . 3_665 ? Nb1 O3 Sc 127.85(18) . 3_665 ? Nb1 O3 Nb1 105.16(17) . 4_565 ? Sc O3 Nb1 124.51(19) 3_665 4_565 ? Nb1 O3 Nb2 98.4(8) . 4_565 ? Sc O3 Nb2 132.2(9) 3_665 4_565 ? Nb1 O3 Nb2 8.1(8) 4_565 4_565 ? Nb1 O3 Nb2 2.4(5) . . ? Sc O3 Nb2 125.6(5) 3_665 . ? Nb1 O3 Nb2 107.6(4) 4_565 . ? Nb2 O3 Nb2 100.8(9) 4_565 . ? Nb2 O4 Nb1 9.1(10) . . ? Nb2 O4 Sc 126.3(6) . 3_666 ? Nb1 O4 Sc 129.31(18) . 3_666 ? Nb2 O4 Sc 132.6(7) . 1_645 ? Nb1 O4 Sc 127.29(19) . 1_645 ? Sc O4 Sc 100.65(14) 3_666 1_645 ? _refine_diff_density_max 1.138 _refine_diff_density_min -0.980 _refine_diff_density_rms 0.197 _shelxl_version_number 2014-3 _shelx_res_file ; TITL scox in P2/c CELL 0.71073 9.92989 5.66246 5.21080 90.0000 92.3828 90.0000 ZERR 2.00 0.00609 0.00314 0.00301 0.0000 0.0068 0.0000 LATT 1 SYMM -X, Y, 0.5-Z SFAC O SC Y NB UNIT 8 1 1 2 SIZE 0.02 0.03 0.04 L.S. 6 BOND acta OMIT 0 0 1 BIND NB1 NB2 BIND Y1 Y2 FMAP 2 PLAN 20 WGHT 0.020500 1.918300 FVAR 0.44231 Y1 3 0.500000 0.770608 0.250000 0.49456 0.01283 0.01511 = 0.00973 0.00000 0.00071 0.00000 Y2 3 0.500000 0.820134 0.250000 0.12184 0.02464 0.02567 = 0.02931 0.00000 0.00451 0.00000 NB1 4 0.755367 0.314660 0.226166 0.89623 0.01472 0.01388 = 0.01175 0.00174 -0.00311 -0.00009 NB2 4 0.745735 0.291320 0.278061 0.10357 0.03014 0.03492 = 0.01318 0.01127 -0.00224 -0.00138 SC 2 0.000000 0.818308 0.250000 0.73473 0.01677 0.02015 = 0.01640 0.00000 -0.00005 0.00000 O1 1 0.624646 1.098009 0.091285 11.00000 0.03260 0.02283 = 0.02688 -0.00059 0.00250 -0.00145 O2 1 0.638108 0.579360 0.012276 11.00000 0.02693 0.03607 = 0.05479 0.02100 -0.00246 0.00227 O3 1 0.862122 0.388532 -0.082421 11.00000 0.02795 0.02013 = 0.02479 0.00248 -0.00160 0.00241 O4 1 0.885510 0.114486 0.408157 11.00000 0.02420 0.02151 = 0.02617 -0.00394 -0.00023 -0.00056 HKLF 4 REM scox in P2/c REM R1 = 0.0269 for 878 Fo > 4sig(Fo) and 0.0316 for all 948 data REM 75 parameters refined using 0 restraints END WGHT 0.0216 1.7232 REM Highest difference peak 1.138, deepest hole -0.980, 1-sigma level 0.197 Q1 1 0.0000 0.6980 0.2500 10.50000 0.05 1.14 Q2 1 0.5851 0.6348 0.1077 11.00000 0.05 0.97 Q3 1 0.7627 0.1969 0.2289 11.00000 0.05 0.80 Q4 1 0.8703 0.4913 -0.0287 11.00000 0.05 0.67 Q5 1 1.0000 0.5183 -0.2500 10.50000 0.05 0.66 Q6 1 0.8034 0.3999 0.0012 11.00000 0.05 0.60 Q7 1 0.5000 0.6614 0.2500 10.50000 0.05 0.59 Q8 1 0.7440 0.9101 0.2171 11.00000 0.05 0.56 Q9 1 0.5582 1.1319 -0.0020 11.00000 0.05 0.54 Q10 1 0.7227 1.1381 0.0332 11.00000 0.05 0.53 Q11 1 0.8047 0.1033 0.0569 11.00000 0.05 0.53 Q12 1 0.8566 0.0236 0.4932 11.00000 0.05 0.51 Q13 1 0.7396 0.5177 0.2500 11.00000 0.05 0.51 Q14 1 0.9170 0.0978 0.5494 11.00000 0.05 0.50 Q15 1 0.7647 -0.0465 0.2454 11.00000 0.05 0.49 Q16 1 0.8838 -0.0128 0.4980 11.00000 0.05 0.49 Q17 1 0.6427 0.4012 0.1293 11.00000 0.05 0.49 Q18 1 0.5841 0.8043 0.0536 11.00000 0.05 0.49 Q19 1 0.9127 0.3819 0.0284 11.00000 0.05 0.48 Q20 1 0.7500 0.3228 -0.0458 11.00000 0.05 0.48 ; _shelx_res_checksum 63230 _shelx_hkl_file ; -2 0 0 38.19 0.95 2 0 0 33.91 0.87 -3 0 0 194.63 2.90 3 0 0 195.03 3.12 -4 0 0 3902.41 48.67 4 0 0 3924.53 50.64 -5 0 0 30.57 1.41 5 0 0 27.95 1.29 -6 0 0 5.58 1.11 6 0 0 3.83 0.94 -7 0 0 277.58 4.08 7 0 0 276.93 4.52 -8 0 0 5369.56 61.04 8 0 0 5505.96 81.54 -9 0 0 5.22 1.35 9 0 0 4.60 1.97 -10 0 0 7.97 2.17 10 0 0 9.98 2.43 -11 0 0 132.90 4.58 11 0 0 139.75 5.42 -12 0 0 932.27 15.99 12 0 0 940.82 18.72 -13 0 0 5.62 4.18 13 0 0 1.54 4.00 -14 0 0 -0.15 4.49 14 0 0 -1.69 4.33 0 -1 0 60.77 1.32 0 1 0 65.89 1.21 -1 -1 0 9.22 0.56 1 -1 0 9.58 0.59 -1 1 0 10.74 0.48 1 1 0 10.39 0.63 -2 -1 0 1619.09 22.68 2 -1 0 1570.10 23.04 -2 1 0 1629.97 18.05 2 1 0 1655.26 21.54 -3 -1 0 27.31 1.27 3 -1 0 18.96 0.82 -3 1 0 21.00 0.77 3 1 0 21.79 1.23 -4 -1 0 36.04 1.79 4 -1 0 34.51 1.21 -4 1 0 35.98 1.01 4 1 0 35.76 1.59 -5 -1 0 4.49 1.31 5 -1 0 3.60 0.87 -5 1 0 3.31 0.70 5 1 0 3.73 1.13 -6 -1 0 333.25 5.17 6 -1 0 329.25 5.04 -6 1 0 329.81 4.03 6 1 0 336.08 6.03 -7 -1 0 15.00 1.61 7 -1 0 12.84 1.25 -7 1 0 13.41 1.08 7 1 0 10.70 1.65 -8 -1 0 10.10 1.73 8 -1 0 14.43 1.47 -8 1 0 15.23 1.20 8 1 0 16.41 1.98 -9 -1 0 0.74 1.64 9 -1 0 -0.41 1.72 -9 1 0 0.13 1.20 9 1 0 2.62 2.08 -10 -1 0 344.64 9.09 10 -1 0 348.20 8.23 -10 1 0 337.30 6.91 10 1 0 336.42 7.17 -11 -1 0 19.56 2.79 11 -1 0 20.86 3.51 -11 1 0 16.17 3.49 11 1 0 21.33 3.07 -12 -1 0 5.78 2.70 12 -1 0 9.86 3.66 -12 1 0 0.21 3.66 12 1 0 7.41 3.17 -13 -1 0 4.17 2.90 13 -1 0 11.82 4.07 -13 1 0 6.83 4.02 13 1 0 1.12 4.07 -14 -1 0 31.61 5.39 14 -1 0 21.09 7.44 -14 1 0 31.96 8.14 14 1 0 23.31 6.74 0 -2 0 4194.00 50.09 0 2 0 4091.63 52.79 -1 -2 0 100.02 1.98 1 -2 0 94.62 2.02 -1 2 0 98.51 1.96 1 2 0 96.77 1.94 -2 -2 0 19.66 1.01 2 -2 0 17.89 0.89 -2 2 0 17.65 0.80 2 2 0 18.34 1.00 -3 -2 0 355.14 5.83 3 -2 0 346.79 5.47 -3 2 0 352.19 4.42 3 2 0 356.80 5.21 -4 -2 0 5066.14 69.65 4 -2 0 5018.93 71.02 -4 2 0 5036.08 55.54 4 2 0 5108.20 81.19 -5 -2 0 78.54 2.77 5 -2 0 75.84 2.14 -5 2 0 77.26 1.78 5 2 0 77.77 2.39 -6 -2 0 5.48 1.67 6 -2 0 5.84 1.28 -6 2 0 5.20 1.02 6 2 0 3.80 1.41 -7 -2 0 147.73 4.08 7 -2 0 146.74 3.44 -7 2 0 149.60 2.78 7 2 0 150.63 3.80 -8 -2 0 1481.24 19.72 8 -2 0 1465.06 22.07 -8 2 0 1480.80 18.79 8 2 0 1517.27 23.56 -9 -2 0 10.41 2.10 9 -2 0 10.01 1.99 -9 2 0 13.55 1.68 9 2 0 11.85 2.41 -10 -2 0 8.72 2.98 10 -2 0 6.18 2.19 -10 2 0 8.93 3.13 10 2 0 7.01 2.58 -11 -2 0 150.69 6.84 11 -2 0 152.60 8.54 -11 2 0 156.78 5.97 11 2 0 139.31 6.33 -12 -2 0 681.28 15.77 12 -2 0 683.76 20.99 -12 2 0 682.80 15.07 12 2 0 663.95 20.77 -13 -2 0 4.45 4.58 13 -2 0 3.90 6.48 -13 2 0 0.61 3.96 13 2 0 0.87 4.42 -14 -2 0 1.10 3.45 0 -3 0 109.41 1.94 0 3 0 109.87 2.21 -1 -3 0 0.87 0.91 1 -3 0 0.32 0.85 -1 3 0 1.26 0.96 1 3 0 0.75 1.00 -2 -3 0 4182.74 57.42 2 -3 0 4114.06 57.34 -2 3 0 4147.64 55.80 2 3 0 4069.12 55.57 -3 -3 0 54.38 1.79 3 -3 0 50.99 1.84 -3 3 0 53.29 1.87 3 3 0 57.12 1.97 -4 -3 0 173.65 3.94 4 -3 0 173.41 3.46 -4 3 0 181.68 2.86 4 3 0 184.16 4.13 -5 -3 0 13.56 1.85 5 -3 0 11.63 1.76 -5 3 0 12.05 1.13 5 3 0 12.37 1.77 -6 -3 0 2056.12 29.87 6 -3 0 2079.36 37.50 -6 3 0 2047.47 23.51 6 3 0 2116.63 40.79 -7 -3 0 32.97 2.60 7 -3 0 27.98 2.69 -7 3 0 33.27 1.75 7 3 0 35.79 3.32 -8 -3 0 52.01 3.34 8 -3 0 43.25 3.41 -8 3 0 50.52 2.30 8 3 0 53.45 4.13 -9 -3 0 20.97 3.88 9 -3 0 21.17 3.10 -9 3 0 17.82 1.85 9 3 0 24.84 3.96 -10 -3 0 992.98 17.77 10 -3 0 1026.05 20.17 -10 3 0 1041.89 16.48 10 3 0 1016.16 28.03 -11 -3 0 76.82 6.10 11 -3 0 60.59 4.66 -11 3 0 68.29 5.15 11 3 0 50.14 5.12 -12 -3 0 22.29 4.95 12 -3 0 29.56 6.61 -12 3 0 25.52 4.24 12 3 0 17.30 4.81 -13 -3 0 14.27 5.14 13 -3 0 15.64 7.14 -13 3 0 23.56 7.45 13 3 0 25.53 5.26 0 -4 0 29.47 1.61 0 4 0 32.65 2.20 -1 -4 0 315.09 5.41 1 -4 0 304.91 4.53 -1 4 0 320.48 5.30 1 4 0 314.19 5.15 -2 -4 0 155.74 3.39 2 -4 0 150.54 3.19 -2 4 0 155.28 3.79 2 4 0 155.81 3.25 -3 -4 0 142.20 3.31 3 -4 0 147.99 3.21 -3 4 0 145.70 3.75 3 4 0 146.96 3.30 -4 -4 0 479.29 8.21 4 -4 0 472.29 7.64 -4 4 0 473.23 7.17 4 4 0 473.78 8.90 -5 -4 0 132.61 3.97 5 -4 0 135.37 3.37 -5 4 0 133.57 3.24 5 4 0 137.35 4.10 -6 -4 0 87.90 3.67 6 -4 0 88.43 2.93 -6 4 0 86.19 2.90 6 4 0 93.17 4.42 -7 -4 0 145.78 4.54 7 -4 0 145.66 3.72 -7 4 0 141.52 4.16 7 4 0 141.85 5.55 -8 -4 0 15.53 2.76 8 -4 0 9.54 2.11 -8 4 0 15.45 2.45 8 4 0 9.68 1.35 -9 -4 0 117.22 6.29 9 -4 0 121.58 3.84 -9 4 0 116.58 4.27 9 4 0 121.29 5.96 -10 -4 0 58.24 5.71 10 -4 0 59.61 4.78 -10 4 0 66.30 3.98 10 4 0 58.06 2.26 -11 -4 0 51.51 4.64 11 -4 0 38.18 4.32 -11 4 0 63.57 4.38 11 4 0 41.76 5.18 -12 -4 0 56.20 6.37 12 -4 0 41.85 7.80 -12 4 0 55.33 8.48 12 4 0 49.23 7.19 0 -5 0 74.01 2.77 0 5 0 79.22 3.51 -1 -5 0 9.03 1.71 1 -5 0 7.77 1.67 -1 5 0 3.95 2.83 1 5 0 7.66 2.35 -2 -5 0 1730.83 25.22 2 -5 0 1730.86 25.18 -2 5 0 1779.53 27.27 2 5 0 1746.48 29.63 -3 -5 0 5.86 2.26 3 -5 0 1.85 2.02 -3 5 0 2.80 1.96 3 5 0 2.02 2.41 -4 -5 0 42.94 2.94 4 -5 0 46.84 2.52 -4 5 0 47.08 2.95 4 5 0 40.95 2.51 -5 -5 0 40.33 3.09 5 -5 0 29.83 2.25 -5 5 0 36.36 2.89 5 5 0 32.20 3.00 -6 -5 0 1383.76 21.34 6 -5 0 1421.96 20.75 -6 5 0 1403.11 19.19 -7 -5 0 7.04 2.69 7 -5 0 10.64 2.23 -7 5 0 9.92 2.42 7 5 0 6.29 3.58 -8 -5 0 43.50 4.00 8 -5 0 30.23 2.76 -8 5 0 43.41 3.23 8 5 0 37.65 4.57 -9 -5 0 29.90 4.76 9 -5 0 38.61 3.05 -9 5 0 45.27 3.51 9 5 0 37.45 4.83 -10 -5 0 425.68 16.44 10 -5 0 469.56 11.38 -10 5 0 458.63 9.11 10 5 0 439.09 15.61 -11 -5 0 -0.37 4.65 11 -5 0 2.85 4.35 -11 5 0 5.51 4.20 11 5 0 4.13 6.04 0 -6 0 115.33 3.59 0 6 0 112.20 5.53 -1 -6 0 179.73 4.46 1 -6 0 182.02 4.42 -1 6 0 187.66 6.74 1 6 0 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5.75 -3 6 5 80.11 7.82 2 -6 -5 11.49 3.58 2 6 -5 11.65 6.15 -2 -6 5 18.07 4.34 -2 6 5 8.32 4.99 1 6 -5 6.26 5.95 -1 -6 5 8.32 4.23 0 6 -5 232.79 13.61 0 -6 5 244.72 8.10 -1 6 -5 86.52 10.59 1 -6 5 104.42 9.64 9 0 -6 34.69 3.62 -9 0 6 17.79 6.34 8 0 -6 471.00 9.94 -8 0 6 470.03 12.57 7 0 -6 228.29 6.15 -7 0 6 224.78 7.41 6 0 -6 63.43 3.79 -6 0 6 72.55 5.16 5 0 -6 62.02 3.65 -5 0 6 50.16 3.61 4 0 -6 608.13 11.98 -4 0 6 624.96 11.15 3 0 -6 469.24 9.97 -3 0 6 472.65 7.84 2 0 -6 71.96 5.56 -2 0 6 76.40 3.33 1 0 -6 111.58 6.14 -1 0 6 116.72 4.71 0 0 -6 1410.11 29.74 0 0 6 1392.29 22.90 -1 0 -6 304.50 7.66 1 0 6 302.68 7.25 -2 0 -6 9.10 3.19 2 0 6 7.03 2.93 -3 0 -6 36.23 3.87 3 0 6 38.65 4.56 -4 0 -6 823.46 15.88 4 0 6 854.59 18.01 -5 0 -6 287.53 7.85 5 0 6 296.34 8.77 -6 0 -6 8.83 3.73 6 0 6 11.33 4.38 -7 0 -6 54.45 4.40 7 0 6 65.18 5.80 -8 0 -6 881.43 17.48 8 0 6 879.88 18.85 9 -1 -6 7.50 3.15 9 1 -6 9.94 4.52 -9 -1 6 -3.95 5.75 -9 1 6 1.46 4.11 8 -1 -6 4.48 2.86 8 1 -6 4.31 2.75 -8 -1 6 2.31 3.80 -8 1 6 7.27 4.12 7 -1 -6 8.81 4.21 7 1 -6 11.35 2.72 -7 -1 6 1.89 2.99 -7 1 6 8.02 3.93 6 -1 -6 51.79 6.55 6 1 -6 42.18 3.66 -6 -1 6 33.63 3.51 -6 1 6 30.15 4.14 5 -1 -6 20.99 3.56 5 1 -6 14.14 2.62 -5 -1 6 10.47 2.81 -5 1 6 12.88 3.57 4 -1 -6 3.31 3.19 4 1 -6 2.05 2.39 -4 -1 6 -0.16 2.54 -4 1 6 -1.05 3.20 3 -1 -6 72.12 4.41 3 1 -6 80.62 4.60 -3 -1 6 76.43 3.51 -3 1 6 70.99 3.57 2 -1 -6 105.34 4.79 2 1 -6 109.37 6.13 -2 -1 6 110.90 3.81 -2 1 6 107.62 3.51 1 -1 -6 42.34 4.81 1 1 -6 34.99 4.70 -1 -1 6 39.44 3.45 -1 1 6 37.61 2.99 0 -1 -6 6.97 3.78 0 1 -6 4.66 3.08 0 -1 6 2.16 2.71 0 1 6 3.34 2.27 -1 -1 -6 24.42 4.41 -1 1 -6 20.60 2.54 1 -1 6 21.46 3.29 1 1 6 20.52 2.69 -2 -1 -6 100.00 4.73 -2 1 -6 99.23 3.87 2 -1 6 94.54 4.99 2 1 6 99.79 4.43 -3 -1 -6 4.36 3.18 -3 1 -6 5.34 2.43 3 -1 6 7.39 4.06 3 1 6 4.75 2.62 -4 -1 -6 14.31 3.57 -4 1 -6 13.55 2.64 4 -1 6 13.86 4.36 4 1 6 16.79 4.09 -5 -1 -6 31.71 4.11 -5 1 -6 27.36 3.00 5 -1 6 33.81 4.87 5 1 6 36.03 4.73 -6 -1 -6 89.87 6.81 -6 1 -6 95.68 4.27 6 -1 6 89.64 5.96 6 1 6 95.99 5.98 -7 -1 -6 25.27 5.97 -7 1 -6 19.45 3.20 7 -1 6 30.38 5.02 7 1 6 26.03 4.94 -8 -1 -6 2.43 5.80 -8 1 -6 -2.75 3.22 8 -1 6 6.14 6.46 8 1 6 -1.10 4.23 8 -2 -6 204.86 8.33 8 2 -6 203.15 6.70 -8 -2 6 206.30 6.37 -8 2 6 198.06 7.31 7 -2 -6 194.80 7.59 7 2 -6 188.27 6.25 -7 -2 6 193.39 6.09 -7 2 6 189.41 6.98 6 -2 -6 79.32 5.81 6 2 -6 77.14 3.95 -6 -2 6 77.94 4.65 -6 2 6 63.31 4.85 5 -2 -6 4.62 3.93 5 2 -6 5.00 2.58 -5 -2 6 4.75 2.73 -5 2 6 7.58 3.55 4 -2 -6 407.38 10.50 4 2 -6 409.78 7.69 -4 -2 6 403.08 8.48 -4 2 6 396.84 9.65 3 -2 -6 215.85 6.36 3 2 -6 214.65 5.34 -3 -2 6 216.99 5.06 -3 2 6 217.11 6.62 2 -2 -6 53.22 4.27 2 2 -6 52.55 5.35 -2 -2 6 52.61 3.17 -2 2 6 49.97 3.51 1 -2 -6 8.86 3.20 1 2 -6 10.02 4.22 -1 -2 6 8.69 3.00 -1 2 6 8.07 3.88 0 -2 -6 552.67 14.07 0 2 -6 555.99 11.62 0 -2 6 557.36 11.11 0 2 6 566.48 13.08 -1 -2 -6 262.40 8.74 -1 2 -6 260.58 7.26 1 -2 6 272.90 7.32 1 2 6 275.30 8.37 -2 -2 -6 29.84 3.76 -2 2 -6 31.69 3.93 2 -2 6 27.95 3.67 2 2 6 28.70 4.30 -3 -2 -6 7.72 3.40 -3 2 -6 8.01 3.55 3 -2 6 3.77 4.29 3 2 6 8.35 3.96 -4 -2 -6 528.50 11.55 -4 2 -6 545.89 11.66 4 -2 6 555.68 13.34 4 2 6 531.43 12.69 -5 -2 -6 150.79 7.94 -5 2 -6 154.46 5.08 5 -2 6 157.15 7.43 5 2 6 144.98 6.74 -6 -2 -6 5.45 5.52 -6 2 -6 6.21 2.98 6 -2 6 5.48 4.39 6 2 6 7.83 4.35 -7 -2 -6 -5.09 5.48 -7 2 -6 2.95 3.86 7 -2 6 3.58 6.95 7 2 6 0.76 4.16 7 -3 -6 105.28 6.70 7 3 -6 102.50 5.28 -7 -3 6 101.28 6.04 -7 3 6 103.52 5.71 6 -3 -6 185.72 6.04 6 3 -6 175.77 6.17 -6 -3 6 178.20 6.83 -6 3 6 182.40 6.67 5 -3 -6 106.75 6.28 5 3 -6 102.69 4.86 -5 -3 6 109.97 4.90 -5 3 6 107.37 5.37 4 -3 -6 2.48 4.00 4 3 -6 3.50 3.03 -4 -3 6 4.17 2.86 -4 3 6 1.66 3.30 3 -3 -6 147.24 6.56 3 3 -6 157.98 5.69 -3 -3 6 157.50 5.42 -3 3 6 162.17 5.80 2 -3 -6 407.85 10.62 2 3 -6 414.13 9.31 -2 -3 6 421.21 8.78 -2 3 6 428.02 15.56 1 -3 -6 115.99 5.09 1 3 -6 111.29 4.31 -1 -3 6 122.40 5.34 -1 3 6 112.12 6.35 0 -3 -6 3.84 3.16 0 3 -6 -0.30 3.49 0 -3 6 -3.73 2.88 0 3 6 -2.72 3.79 -1 -3 -6 145.25 6.90 -1 3 -6 142.21 5.92 1 -3 6 158.39 6.20 1 3 6 163.14 6.71 -2 -3 -6 452.99 12.57 -2 3 -6 463.13 10.60 2 -3 6 482.02 10.32 2 3 6 466.21 16.70 -3 -3 -6 88.10 5.05 -3 3 -6 78.76 6.86 3 -3 6 85.22 6.34 3 3 6 93.62 5.78 -4 -3 -6 9.73 3.85 -4 3 -6 13.62 5.63 4 -3 6 8.63 4.70 4 3 6 4.90 3.91 -5 -3 -6 89.53 7.33 -5 3 -6 84.55 7.32 5 -3 6 91.68 6.78 5 3 6 85.51 5.80 -6 -3 -6 386.07 13.08 -6 3 -6 374.05 13.12 6 -3 6 412.23 11.41 6 3 6 404.45 10.85 5 -4 -6 41.63 5.11 5 4 -6 43.86 4.16 -5 -4 6 44.33 5.25 -5 4 6 38.18 5.43 4 -4 -6 71.96 6.53 4 4 -6 78.52 4.71 -4 -4 6 79.60 5.54 -4 4 6 70.78 4.73 3 -4 -6 39.06 4.84 3 4 -6 37.86 3.86 -3 -4 6 39.90 4.72 -3 4 6 35.10 3.87 2 -4 -6 35.58 4.61 2 4 -6 38.69 4.71 -2 -4 6 36.54 4.51 -2 4 6 41.76 6.40 1 -4 -6 90.28 4.53 1 4 -6 92.92 5.10 -1 -4 6 101.94 9.55 -1 4 6 104.14 8.51 0 -4 -6 3.68 3.84 0 4 -6 11.27 3.58 0 -4 6 12.64 6.07 -1 -4 -6 68.71 4.86 -1 4 -6 71.07 4.95 1 -4 6 80.54 9.03 1 4 6 69.31 8.45 -2 -4 -6 53.42 4.53 -2 4 -6 49.75 4.43 2 -4 6 45.08 8.30 2 4 6 60.38 8.08 -3 -4 -6 40.28 5.43 -3 4 -6 43.74 6.64 3 -4 6 42.46 8.12 -4 -4 -6 77.11 5.36 -4 4 -6 74.93 7.55 4 -4 6 96.30 9.61 4 4 6 77.08 7.97 1 5 -6 88.44 7.47 -1 -5 6 100.65 10.13 0 5 -6 2.84 5.87 6 0 -7 2.47 3.46 -6 0 7 -4.02 4.71 5 0 -7 -0.33 3.78 -5 0 7 -5.00 2.86 4 0 -7 2.41 3.74 -4 0 7 -1.12 3.53 3 0 -7 -1.09 3.81 -3 0 7 -3.29 3.28 2 0 -7 2.94 3.71 -2 0 7 0.02 2.88 1 0 -7 3.83 4.75 -1 0 7 -1.90 2.91 0 0 -7 -0.08 4.45 0 0 7 3.44 2.89 -1 0 -7 -7.11 4.25 1 0 7 -2.48 2.84 -2 0 -7 6.44 4.71 2 0 7 -2.07 2.99 -3 0 -7 0.71 3.91 3 0 7 -0.46 3.26 -4 0 -7 2.13 4.01 4 0 7 -0.36 4.22 -5 0 -7 -6.76 7.82 5 -1 -7 184.62 7.62 5 1 -7 193.13 5.67 -5 -1 7 188.57 6.10 -5 1 7 185.27 7.11 4 -1 -7 95.30 5.41 4 1 -7 90.74 4.50 -4 -1 7 87.43 4.60 -4 1 7 88.69 9.37 3 -1 -7 32.98 4.54 3 1 -7 31.22 4.72 -3 -1 7 32.92 3.95 -3 1 7 32.49 7.44 2 -1 -7 439.59 10.13 2 1 -7 454.37 10.25 -2 -1 7 445.02 9.73 -2 1 7 461.54 12.02 1 -1 -7 277.39 7.86 1 1 -7 258.35 9.94 -1 -1 7 293.12 7.56 -1 1 7 307.58 9.47 0 -1 -7 32.38 5.53 0 1 -7 29.35 5.58 0 -1 7 36.37 3.96 0 1 7 36.25 5.28 -1 -1 -7 62.78 6.28 -1 1 -7 53.67 6.01 1 -1 7 59.89 4.49 1 1 7 63.65 5.86 -2 -1 -7 483.08 13.79 -2 1 -7 482.25 13.80 2 -1 7 506.61 10.78 2 1 7 509.08 12.83 -3 -1 -7 214.70 8.93 -3 1 -7 217.37 6.10 3 -1 7 237.84 7.42 3 1 7 233.75 12.48 -4 -1 -7 16.55 4.27 -4 1 -7 21.44 3.43 4 -1 7 25.24 4.43 4 1 7 17.55 7.94 4 -2 -7 156.38 7.31 4 2 -7 158.41 5.30 -4 -2 7 160.09 5.70 -4 2 7 168.25 11.14 3 -2 -7 33.46 5.11 3 2 -7 47.39 3.82 -3 -2 7 35.46 4.14 -3 2 7 31.22 7.47 2 -2 -7 11.41 3.82 2 2 -7 21.22 4.28 -2 -2 7 9.12 3.42 -2 2 7 6.94 6.72 1 -2 -7 104.53 5.46 1 2 -7 102.14 7.14 -1 -2 7 106.70 5.37 -1 2 7 105.19 6.54 0 -2 -7 98.14 6.89 0 2 -7 108.00 7.10 0 -2 7 109.45 5.63 0 2 7 108.21 6.93 -1 -2 -7 86.91 6.76 -1 2 -7 76.33 6.56 1 -2 7 92.32 5.79 1 2 7 79.83 6.22 -2 -2 -7 5.64 4.87 -2 2 -7 4.91 4.08 2 -2 7 8.28 3.67 2 2 7 14.35 7.46 -3 -2 -7 74.91 6.84 -3 2 -7 71.99 5.57 3 -2 7 80.18 5.32 3 2 7 86.28 9.69 2 -3 -7 91.52 6.30 2 3 -7 104.67 9.06 -2 -3 7 99.91 9.87 -2 3 7 100.05 9.77 1 -3 -7 76.71 5.92 1 3 -7 70.57 8.38 -1 -3 7 82.68 9.38 -1 3 7 69.06 8.27 0 -3 -7 55.04 4.91 0 3 -7 46.33 6.17 0 -3 7 40.06 7.54 0 3 7 48.75 5.62 -1 -3 -7 15.69 4.25 -1 3 -7 12.25 6.72 1 -3 7 9.48 4.32 1 3 7 10.20 7.46 0 0 0 0.00 0.00 ; _shelx_hkl_checksum 6763 # start Validation Reply Form _vrf_ABSMU01_shakhdaraite-Y ; PROBLEM: The ratio of given/expected absorption coefficient lies RESPONSE: The chemical formula of shakhdaraite was determined by electron-microprobe analysis and is given in the CIF (Z = 2). 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_shakhdaraite-Y ; PROBLEM: The ratio of given/expected molecular weight as calculated RESPONSE: The chemical formula of shakhdaraite was determined by electron-microprobe analysis and is given in the CIF (Z = 2). 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_shakhdaraite-Y ; PROBLEM: Mu(calc) and Mu(CIF) Ratio Differs from 1.0 by . 137.29 % RESPONSE: Mu(calc) is based on ideal formula and Mu(CIF) on the data from electron-microprobe analysis, with heavier scatters. ; _vrf_PLAT075_shakhdaraite-Y ; PROBLEM: Occupancy 1.469 Greater Than 1.0 for ...... SC RESPONSE: Besides Sc, this particular site is occupied by heavier cations such as Ta,Mn,U,W and Pb. That is why occupancy of the site is greater than 1. ; # end Validation Reply Form