data_nacareniobsite-(Y) _audit_creation_method SHELXL-2014 _chemical_name_systematic ; ? ; _chemical_name_common nacareniobsite-(Y) _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'Ca3.06 Ce0.15 Dy0.08 F3 Ho0.02 La0.04 Na2.82 Nb0.64 Nd0.16 O15 Pr0.01 Si4 Sm0.05 Sr0.14 Ti0.38 Y0.36' _chemical_formula_weight 793.65 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' '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' 'Si' 'Si' 0.0817 0.0704 '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' 'Nb' 'Nb' -2.0727 0.6215 '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' 'Sr' 'Sr' -1.5307 3.2498 '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' 'Nd' 'Nd' -0.1943 3.0179 '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' 'Dy' 'Dy' -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Sm' 'Sm' -0.1638 3.4418 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Pr' 'Pr' -0.2180 2.8214 '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' 'Ho' 'Ho' -0.2175 4.6783 '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/c' _space_group_name_Hall '-P 2ybc' _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+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 7.4069(15) _cell_length_b 5.6540(11) _cell_length_c 18.787(4) _cell_angle_alpha 90 _cell_angle_beta 101.36(3) _cell_angle_gamma 90 _cell_volume 771.3(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 9935 _cell_measurement_theta_min 2.805 _cell_measurement_theta_max 31.082 _exptl_crystal_description tabular _exptl_crystal_colour 'pale yellow' _exptl_crystal_density_meas 3.49 _exptl_crystal_density_method 'flotation' _exptl_crystal_density_diffrn 3.417 _exptl_crystal_F_000 760 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.050 _exptl_crystal_size_mid 0.050 _exptl_crystal_size_min 0.020 _exptl_absorpt_coefficient_mu 5.813 _shelx_estimated_absorpt_T_min 0.760 _shelx_estimated_absorpt_T_max 0.893 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.5492 _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 7086 _diffrn_reflns_av_unetI/netI 0.0273 _diffrn_reflns_av_R_equivalents 0.0367 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.805 _diffrn_reflns_theta_max 27.494 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measured_fraction_theta_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.999 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.999 _diffrn_reflns_point_group_measured_fraction_full 0.999 _reflns_number_total 1863 _reflns_number_gt 1788 _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 ; Refined as a 2-component twin. ; _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^)+(0.0514P)^2^+3.2248P] 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 1863 _refine_ls_number_parameters 145 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0363 _refine_ls_R_factor_gt 0.0350 _refine_ls_wR_factor_ref 0.0972 _refine_ls_wR_factor_gt 0.0959 _refine_ls_goodness_of_fit_ref 1.081 _refine_ls_restrained_S_all 1.081 _refine_ls_shift/su_max 0.868 _refine_ls_shift/su_mean 0.106 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 MH Y 0.0947(2) 0.66033(9) 0.19346(3) 0.00961(19) Uani 0.842(4) 1 d . . P . . AP Sr 0.5969(3) 0.66078(11) 0.18988(3) 0.0128(2) Uani 0.722(3) 1 d . . P . . MO1 Nb 0.0000 0.0000 0.0000 0.0282(3) Uani 0.834(5) 2 d S . P . . MO2 Na 0.5000 0.0000 0.0000 0.0203(9) Uani 1.099(14) 2 d S . P . . MO3 Na 0.7435(2) 0.5009(4) -0.00061(10) 0.0198(7) Uani 1.086(11) 1 d . . P . . Si1 Si 0.3506(2) 0.1549(3) 0.14068(7) 0.0087(4) Uani 1 1 d . . . . . Si2 Si 0.78451(19) 0.1541(3) 0.13809(7) 0.0087(4) Uani 1 1 d . . . . . O1 O 0.2156(5) 0.1476(8) 0.06155(19) 0.0136(7) Uani 1 1 d . . . . . O2 O 0.8346(5) 0.1440(8) 0.05793(19) 0.0147(8) Uani 1 1 d . . . . . O3 O 0.3336(11) 0.3952(7) 0.18489(19) 0.0146(8) Uani 1 1 d . . . . . O4 O 0.8466(11) 0.3939(6) 0.18162(19) 0.0159(7) Uani 1 1 d . . . . . O5 O 0.3369(11) 0.9292(6) 0.19115(18) 0.0131(8) Uani 1 1 d . . . . . O6 O 0.8549(11) 0.9310(7) 0.18945(18) 0.0132(8) Uani 1 1 d . . . . . O7 O 0.5573(6) 0.1484(7) 0.12093(18) 0.0183(7) Uani 1 1 d . . . . . XM F 0.0302(11) 0.7095(6) 0.06368(16) 0.0187(6) Uani 0.9439 1 d . . P . . F F 0.5326(12) 0.6614(5) 0.06498(16) 0.0215(6) 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 MH 0.0091(4) 0.0071(3) 0.0123(3) 0.00102(17) 0.0012(6) 0.0008(4) AP 0.0119(4) 0.0117(3) 0.0146(3) 0.0006(2) 0.0021(8) 0.0010(5) MO1 0.0082(4) 0.0490(6) 0.0279(5) -0.0299(4) 0.0046(8) -0.0058(10) MO2 0.0245(16) 0.0185(14) 0.0155(14) -0.0022(10) -0.002(3) -0.004(3) MO3 0.0251(14) 0.0107(9) 0.0237(11) 0.0072(7) 0.005(3) 0.002(2) Si1 0.0102(10) 0.0076(6) 0.0081(5) -0.0001(5) 0.0010(5) 0.0013(9) Si2 0.0120(11) 0.0062(6) 0.0080(6) -0.0007(5) 0.0024(4) 0.0012(9) O1 0.0116(16) 0.0133(17) 0.0132(16) 0.0001(14) -0.0036(12) -0.0030(17) O2 0.0176(18) 0.0163(18) 0.0123(15) 0.0034(15) 0.0081(13) 0.0052(18) O3 0.0139(19) 0.0110(17) 0.0183(16) -0.0053(13) 0.001(3) -0.001(3) O4 0.015(2) 0.0110(17) 0.0199(16) -0.0060(13) 0.000(3) -0.001(3) O5 0.017(2) 0.0086(16) 0.0138(15) 0.0023(11) 0.004(3) -0.001(3) O6 0.016(2) 0.0104(16) 0.0135(15) 0.0023(12) 0.003(3) 0.000(3) O7 0.0113(15) 0.0265(19) 0.0177(16) -0.0040(14) 0.0046(16) 0.000(2) XM 0.0192(16) 0.0214(15) 0.0144(14) -0.0012(12) 0.001(2) 0.002(3) F 0.0279(17) 0.0175(14) 0.0180(14) 0.0021(11) 0.002(2) 0.001(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 MH O6 2.334(7) 1_455 ? MH O3 2.349(7) . ? MH O4 2.352(7) 1_455 ? MH O5 2.359(7) . ? MH XM 2.406(3) . ? MH O6 2.517(4) 2_645 ? MH O4 2.653(4) 2_655 ? MH Si2 3.1147(16) 2_655 ? MH AP 3.6745(11) 1_455 ? MH AP 3.7336(11) . ? MH MH 3.9556(17) 2 ? MH MH 3.9556(17) 2_545 ? AP F 2.301(3) . ? AP O4 2.415(7) . ? AP O3 2.448(7) . ? AP O6 2.448(7) . ? AP O5 2.456(7) . ? AP O5 2.553(3) 2_645 ? AP O3 2.661(4) 2_655 ? AP O7 3.036(4) 1_565 ? AP Si1 3.1301(15) 2_655 ? AP O7 3.163(4) . ? AP Si2 3.3452(18) 1_565 ? AP Si1 3.3648(18) 1_565 ? MO1 O1 1.964(4) . ? MO1 O1 1.964(4) 3 ? MO1 O2 1.968(4) 3_655 ? MO1 O2 1.968(4) 1_455 ? MO1 XM 2.019(3) 3_565 ? MO1 XM 2.019(3) 1_545 ? MO1 MO3 3.401(2) 1_445 ? MO1 MO3 3.401(2) 3_665 ? MO1 MO3 3.409(2) 1_455 ? MO1 MO3 3.409(2) 3_655 ? MO1 MO2 3.7034(7) . ? MO1 MO2 3.7034(7) 1_455 ? MO2 F 2.258(3) 3_665 ? MO2 F 2.258(3) 1_545 ? MO2 O7 2.380(3) . ? MO2 O7 2.380(3) 3_655 ? MO2 O2 2.632(4) . ? MO2 O2 2.632(4) 3_655 ? MO2 O1 2.726(4) 3_655 ? MO2 O1 2.726(4) . ? MO2 Si2 3.1265(16) 3_655 ? MO2 Si2 3.1265(16) . ? MO2 Si1 3.1826(15) 3_655 ? MO2 Si1 3.1826(15) . ? MO3 O2 2.333(5) . ? MO3 O1 2.343(5) 3_665 ? MO3 F 2.348(7) 3_665 ? MO3 F 2.354(7) . ? MO3 XM 2.519(7) 1_655 ? MO3 XM 2.532(7) 3_665 ? MO3 Si2 3.227(2) . ? MO3 Si1 3.237(2) 3_665 ? MO3 MO2 3.351(2) 1_565 ? MO3 MO1 3.401(2) 1_665 ? MO3 MO1 3.409(2) 1_655 ? Si1 O5 1.605(4) 1_545 ? Si1 O3 1.610(4) . ? Si1 O1 1.621(4) . ? Si1 O7 1.645(4) . ? Si1 AP 3.1301(15) 2_645 ? Si1 MO3 3.237(2) 3_665 ? Si1 AP 3.3648(18) 1_545 ? Si2 O4 1.604(4) . ? Si2 O6 1.611(4) 1_545 ? Si2 O2 1.622(4) . ? Si2 O7 1.651(4) . ? Si2 MH 3.1146(15) 2_645 ? Si2 AP 3.3452(18) 1_545 ? O1 MO3 2.343(5) 3_665 ? O2 MO1 1.968(4) 1_655 ? O3 AP 2.661(4) 2_645 ? O4 MH 2.352(7) 1_655 ? O4 MH 2.653(4) 2_645 ? O5 Si1 1.605(4) 1_565 ? O5 AP 2.553(3) 2_655 ? O6 Si2 1.611(4) 1_565 ? O6 MH 2.334(7) 1_655 ? O6 MH 2.517(4) 2_655 ? O7 AP 3.036(4) 1_545 ? XM MO1 2.019(3) 1_565 ? XM MO3 2.519(7) 1_455 ? XM MO3 2.532(7) 3_665 ? F MO2 2.258(3) 1_565 ? F MO3 2.348(7) 3_665 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O6 MH O3 174.21(14) 1_455 . ? O6 MH O4 80.9(2) 1_455 1_455 ? O3 MH O4 99.78(13) . 1_455 ? O6 MH O5 98.83(12) 1_455 . ? O3 MH O5 79.9(2) . . ? O4 MH O5 173.64(13) 1_455 . ? O6 MH XM 83.90(19) 1_455 . ? O3 MH XM 90.4(2) . . ? O4 MH XM 89.0(2) 1_455 . ? O5 MH XM 84.7(2) . . ? O6 MH O6 110.29(11) 1_455 2_645 ? O3 MH O6 75.4(2) . 2_645 ? O4 MH O6 74.41(19) 1_455 2_645 ? O5 MH O6 111.46(14) . 2_645 ? XM MH O6 155.57(12) . 2_645 ? O6 MH O4 72.13(18) 1_455 2_655 ? O3 MH O4 112.58(14) . 2_655 ? O4 MH O4 113.03(10) 1_455 2_655 ? O5 MH O4 72.71(19) . 2_655 ? XM MH O4 143.51(11) . 2_655 ? O6 MH O4 60.88(11) 2_645 2_655 ? O6 MH Si2 96.00(9) 1_455 2_655 ? O3 MH Si2 89.60(10) . 2_655 ? O4 MH Si2 98.71(10) 1_455 2_655 ? O5 MH Si2 87.64(9) . 2_655 ? XM MH Si2 172.18(17) . 2_655 ? O6 MH Si2 31.00(9) 2_645 2_655 ? O4 MH Si2 30.99(8) 2_655 2_655 ? O6 MH AP 40.94(15) 1_455 1_455 ? O3 MH AP 140.00(15) . 1_455 ? O4 MH AP 40.21(15) 1_455 1_455 ? O5 MH AP 139.77(15) . 1_455 ? XM MH AP 89.0(2) . 1_455 ? O6 MH AP 89.53(18) 2_645 1_455 ? O4 MH AP 90.28(18) 2_655 1_455 ? Si2 MH AP 96.02(5) 2_655 1_455 ? O6 MH AP 138.88(16) 1_455 . ? O3 MH AP 39.87(15) . . ? O4 MH AP 139.57(15) 1_455 . ? O5 MH AP 40.10(15) . . ? XM MH AP 88.9(2) . . ? O6 MH AP 92.26(18) 2_645 . ? O4 MH AP 91.46(18) 2_655 . ? Si2 MH AP 86.02(5) 2_655 . ? AP MH AP 177.96(2) 1_455 . ? O6 MH MH 36.94(10) 1_455 2 ? O3 MH MH 147.63(12) . 2 ? O4 MH MH 98.93(16) 1_455 2 ? O5 MH MH 84.31(13) . 2 ? XM MH MH 116.16(13) . 2 ? O6 MH MH 84.61(11) 2_645 2 ? O4 MH MH 35.20(15) 2_655 2 ? Si2 MH MH 61.56(3) 2_655 2 ? AP MH MH 63.16(5) 1_455 2 ? AP MH MH 117.98(5) . 2 ? O6 MH MH 97.92(16) 1_455 2_545 ? O3 MH MH 86.12(13) . 2_545 ? O4 MH MH 40.54(9) 1_455 2_545 ? O5 MH MH 145.30(11) . 2_545 ? XM MH MH 127.30(16) . 2_545 ? O6 MH MH 33.87(16) 2_645 2_545 ? O4 MH MH 83.94(11) 2_655 2_545 ? Si2 MH MH 60.50(3) 2_655 2_545 ? AP MH MH 63.23(5) 1_455 2_545 ? AP MH MH 118.05(5) . 2_545 ? MH MH MH 91.23(5) 2 2_545 ? F AP O4 86.7(2) . . ? F AP O3 87.6(2) . . ? O4 AP O3 103.22(13) . . ? F AP O6 90.0(2) . . ? O4 AP O6 77.4(2) . . ? O3 AP O6 177.55(14) . . ? F AP O5 90.2(2) . . ? O4 AP O5 176.88(13) . . ? O3 AP O5 76.1(2) . . ? O6 AP O5 103.21(12) . . ? F AP O5 149.23(11) . 2_645 ? O4 AP O5 73.66(19) . 2_645 ? O3 AP O5 74.5(2) . 2_645 ? O6 AP O5 107.91(15) . 2_645 ? O5 AP O5 108.91(12) . 2_645 ? F AP O3 150.02(11) . 2_655 ? O4 AP O3 110.53(14) . 2_655 ? O3 AP O3 110.69(12) . 2_655 ? O6 AP O3 71.14(19) . 2_655 ? O5 AP O3 72.48(19) . 2_655 ? O5 AP O3 60.73(11) 2_645 2_655 ? F AP O7 65.18(10) . 1_565 ? O4 AP O7 123.42(16) . 1_565 ? O3 AP O7 122.09(15) . 1_565 ? O6 AP O7 56.06(15) . 1_565 ? O5 AP O7 55.44(14) . 1_565 ? O5 AP O7 145.59(11) 2_645 1_565 ? O3 AP O7 84.86(10) 2_655 1_565 ? F AP Si1 175.3(3) . 2_655 ? O4 AP Si1 96.63(10) . 2_655 ? O3 AP Si1 88.32(10) . 2_655 ? O6 AP Si1 93.98(9) . 2_655 ? O5 AP Si1 86.40(9) . 2_655 ? O5 AP Si1 30.71(9) 2_645 2_655 ? O3 AP Si1 30.96(9) 2_655 2_655 ? O7 AP Si1 115.20(7) 1_565 2_655 ? F AP O7 66.41(10) . . ? O4 AP O7 53.99(16) . . ? O3 AP O7 54.11(16) . . ? O6 AP O7 125.43(16) . . ? O5 AP O7 124.08(17) . . ? O5 AP O7 82.84(10) 2_645 . ? O3 AP O7 143.56(10) 2_655 . ? O7 AP O7 131.57(12) 1_565 . ? Si1 AP O7 112.93(7) 2_655 . ? F AP Si2 73.53(14) . 1_565 ? O4 AP Si2 97.75(16) . 1_565 ? O3 AP Si2 150.88(13) . 1_565 ? O6 AP Si2 27.05(12) . 1_565 ? O5 AP Si2 81.89(13) . 1_565 ? O5 AP Si2 131.54(14) 2_645 1_565 ? O3 AP Si2 79.79(11) 2_655 1_565 ? O7 AP Si2 29.47(8) 1_565 1_565 ? Si1 AP Si2 109.22(5) 2_655 1_565 ? O7 AP Si2 130.90(8) . 1_565 ? F AP Si1 74.12(14) . 1_565 ? O4 AP Si1 151.82(14) . 1_565 ? O3 AP Si1 96.55(15) . 1_565 ? O6 AP Si1 82.09(14) . 1_565 ? O5 AP Si1 26.59(12) . 1_565 ? O5 AP Si1 131.79(13) 2_645 1_565 ? O3 AP Si1 80.17(11) 2_655 1_565 ? O7 AP Si1 29.21(8) 1_565 1_565 ? Si1 AP Si1 103.90(5) 2_655 1_565 ? O7 AP Si1 130.26(8) . 1_565 ? Si2 AP Si1 57.43(3) 1_565 1_565 ? O1 MO1 O1 180.0 . 3 ? O1 MO1 O2 88.80(14) . 3_655 ? O1 MO1 O2 91.21(14) 3 3_655 ? O1 MO1 O2 91.20(14) . 1_455 ? O1 MO1 O2 88.79(14) 3 1_455 ? O2 MO1 O2 180.00(18) 3_655 1_455 ? O1 MO1 XM 89.2(2) . 3_565 ? O1 MO1 XM 90.8(2) 3 3_565 ? O2 MO1 XM 91.0(2) 3_655 3_565 ? O2 MO1 XM 89.0(2) 1_455 3_565 ? O1 MO1 XM 90.8(2) . 1_545 ? O1 MO1 XM 89.2(2) 3 1_545 ? O2 MO1 XM 89.0(2) 3_655 1_545 ? O2 MO1 XM 91.0(2) 1_455 1_545 ? XM MO1 XM 180.00(17) 3_565 1_545 ? O1 MO1 MO3 138.03(12) . 1_445 ? O1 MO1 MO3 41.97(12) 3 1_445 ? O2 MO1 MO3 93.60(14) 3_655 1_445 ? O2 MO1 MO3 86.40(14) 1_455 1_445 ? XM MO1 MO3 132.6(2) 3_565 1_445 ? XM MO1 MO3 47.4(2) 1_545 1_445 ? O1 MO1 MO3 41.97(12) . 3_665 ? O1 MO1 MO3 138.03(12) 3 3_665 ? O2 MO1 MO3 86.40(14) 3_655 3_665 ? O2 MO1 MO3 93.60(14) 1_455 3_665 ? XM MO1 MO3 47.4(2) 3_565 3_665 ? XM MO1 MO3 132.6(2) 1_545 3_665 ? MO3 MO1 MO3 180.00(4) 1_445 3_665 ? O1 MO1 MO3 92.11(14) . 1_455 ? O1 MO1 MO3 87.88(14) 3 1_455 ? O2 MO1 MO3 138.51(13) 3_655 1_455 ? O2 MO1 MO3 41.49(13) 1_455 1_455 ? XM MO1 MO3 47.58(19) 3_565 1_455 ? XM MO1 MO3 132.42(19) 1_545 1_455 ? MO3 MO1 MO3 112.27(5) 1_445 1_455 ? MO3 MO1 MO3 67.73(5) 3_665 1_455 ? O1 MO1 MO3 87.89(14) . 3_655 ? O1 MO1 MO3 92.12(14) 3 3_655 ? O2 MO1 MO3 41.49(13) 3_655 3_655 ? O2 MO1 MO3 138.51(13) 1_455 3_655 ? XM MO1 MO3 132.42(19) 3_565 3_655 ? XM MO1 MO3 47.58(19) 1_545 3_655 ? MO3 MO1 MO3 67.73(5) 1_445 3_655 ? MO3 MO1 MO3 112.27(5) 3_665 3_655 ? MO3 MO1 MO3 180.0 1_455 3_655 ? O1 MO1 MO2 45.80(12) . . ? O1 MO1 MO2 134.20(12) 3 . ? O2 MO1 MO2 43.00(12) 3_655 . ? O2 MO1 MO2 137.00(12) 1_455 . ? XM MO1 MO2 89.6(2) 3_565 . ? XM MO1 MO2 90.4(2) 1_545 . ? MO3 MO1 MO2 123.91(3) 1_445 . ? MO3 MO1 MO2 56.09(3) 3_665 . ? MO3 MO1 MO2 123.82(3) 1_455 . ? MO3 MO1 MO2 56.18(3) 3_655 . ? O1 MO1 MO2 134.20(12) . 1_455 ? O1 MO1 MO2 45.80(12) 3 1_455 ? O2 MO1 MO2 137.00(12) 3_655 1_455 ? O2 MO1 MO2 43.00(12) 1_455 1_455 ? XM MO1 MO2 90.4(2) 3_565 1_455 ? XM MO1 MO2 89.6(2) 1_545 1_455 ? MO3 MO1 MO2 56.09(3) 1_445 1_455 ? MO3 MO1 MO2 123.91(3) 3_665 1_455 ? MO3 MO1 MO2 56.18(3) 1_455 1_455 ? MO3 MO1 MO2 123.82(3) 3_655 1_455 ? MO2 MO1 MO2 180.0 . 1_455 ? F MO2 F 180.00(15) 3_665 1_545 ? F MO2 O7 101.37(12) 3_665 . ? F MO2 O7 78.63(12) 1_545 . ? F MO2 O7 78.63(12) 3_665 3_655 ? F MO2 O7 101.37(12) 1_545 3_655 ? O7 MO2 O7 180.00(19) . 3_655 ? F MO2 O2 87.3(2) 3_665 . ? F MO2 O2 92.7(2) 1_545 . ? O7 MO2 O2 61.32(13) . . ? O7 MO2 O2 118.68(13) 3_655 . ? F MO2 O2 92.7(2) 3_665 3_655 ? F MO2 O2 87.3(2) 1_545 3_655 ? O7 MO2 O2 118.68(13) . 3_655 ? O7 MO2 O2 61.32(13) 3_655 3_655 ? O2 MO2 O2 180.0 . 3_655 ? F MO2 O1 92.3(2) 3_665 3_655 ? F MO2 O1 87.7(2) 1_545 3_655 ? O7 MO2 O1 120.37(12) . 3_655 ? O7 MO2 O1 59.63(13) 3_655 3_655 ? O2 MO2 O1 61.75(9) . 3_655 ? O2 MO2 O1 118.25(9) 3_655 3_655 ? F MO2 O1 87.7(2) 3_665 . ? F MO2 O1 92.3(2) 1_545 . ? O7 MO2 O1 59.63(12) . . ? O7 MO2 O1 120.37(13) 3_655 . ? O2 MO2 O1 118.25(9) . . ? O2 MO2 O1 61.75(9) 3_655 . ? O1 MO2 O1 180.00(12) 3_655 . ? F MO2 Si2 78.75(14) 3_665 3_655 ? F MO2 Si2 101.25(14) 1_545 3_655 ? O7 MO2 Si2 148.69(10) . 3_655 ? O7 MO2 Si2 31.31(10) 3_655 3_655 ? O2 MO2 Si2 148.77(8) . 3_655 ? O2 MO2 Si2 31.23(8) 3_655 3_655 ? O1 MO2 Si2 90.78(8) 3_655 3_655 ? O1 MO2 Si2 89.22(8) . 3_655 ? F MO2 Si2 101.25(14) 3_665 . ? F MO2 Si2 78.75(14) 1_545 . ? O7 MO2 Si2 31.31(10) . . ? O7 MO2 Si2 148.69(10) 3_655 . ? O2 MO2 Si2 31.23(8) . . ? O2 MO2 Si2 148.77(8) 3_655 . ? O1 MO2 Si2 89.22(8) 3_655 . ? O1 MO2 Si2 90.78(8) . . ? Si2 MO2 Si2 180.00(5) 3_655 . ? F MO2 Si1 78.57(14) 3_665 3_655 ? F MO2 Si1 101.43(14) 1_545 3_655 ? O7 MO2 Si1 149.76(10) . 3_655 ? O7 MO2 Si1 30.24(10) 3_655 3_655 ? O2 MO2 Si1 88.59(8) . 3_655 ? O2 MO2 Si1 91.41(8) 3_655 3_655 ? O1 MO2 Si1 30.61(8) 3_655 3_655 ? O1 MO2 Si1 149.39(8) . 3_655 ? Si2 MO2 Si1 61.45(3) 3_655 3_655 ? Si2 MO2 Si1 118.55(3) . 3_655 ? F MO2 Si1 101.43(14) 3_665 . ? F MO2 Si1 78.57(14) 1_545 . ? O7 MO2 Si1 30.24(10) . . ? O7 MO2 Si1 149.76(10) 3_655 . ? O2 MO2 Si1 91.41(8) . . ? O2 MO2 Si1 88.59(8) 3_655 . ? O1 MO2 Si1 149.39(8) 3_655 . ? O1 MO2 Si1 30.61(8) . . ? Si2 MO2 Si1 118.55(3) 3_655 . ? Si2 MO2 Si1 61.45(3) . . ? Si1 MO2 Si1 180.0 3_655 . ? O2 MO3 O1 155.61(15) . 3_665 ? O2 MO3 F 92.67(15) . 3_665 ? O1 MO3 F 105.25(13) 3_665 3_665 ? O2 MO3 F 104.29(13) . . ? O1 MO3 F 95.26(15) 3_665 . ? F MO3 F 79.61(12) 3_665 . ? O2 MO3 XM 92.34(15) . 1_655 ? O1 MO3 XM 70.08(13) 3_665 1_655 ? F MO3 XM 174.98(14) 3_665 1_655 ? F MO3 XM 98.75(13) . 1_655 ? O2 MO3 XM 69.99(13) . 3_665 ? O1 MO3 XM 90.49(15) 3_665 3_665 ? F MO3 XM 99.51(13) 3_665 3_665 ? F MO3 XM 174.22(13) . 3_665 ? XM MO3 XM 82.60(12) 1_655 3_665 ? O2 MO3 Si2 28.54(9) . . ? O1 MO3 Si2 155.41(13) 3_665 . ? F MO3 Si2 96.45(11) 3_665 . ? F MO3 Si2 77.18(9) . . ? XM MO3 Si2 87.77(9) 1_655 . ? XM MO3 Si2 97.29(10) 3_665 . ? O2 MO3 Si1 154.06(12) . 3_665 ? O1 MO3 Si1 28.42(9) 3_665 3_665 ? F MO3 Si1 77.87(10) 3_665 3_665 ? F MO3 Si1 97.75(10) . 3_665 ? XM MO3 Si1 97.73(10) 1_655 3_665 ? XM MO3 Si1 87.61(9) 3_665 3_665 ? Si2 MO3 Si1 173.08(7) . 3_665 ? O2 MO3 MO2 146.38(11) . 1_565 ? O1 MO3 MO2 53.75(11) 3_665 1_565 ? F MO3 MO2 85.18(13) 3_665 1_565 ? F MO3 MO2 42.28(8) . 1_565 ? XM MO3 MO2 90.43(13) 1_655 1_565 ? XM MO3 MO2 143.48(10) 3_665 1_565 ? Si2 MO3 MO2 118.29(6) . 1_565 ? Si1 MO3 MO2 57.75(4) 3_665 1_565 ? O2 MO3 MO2 51.31(11) . . ? O1 MO3 MO2 146.94(11) 3_665 . ? F MO3 MO2 42.13(8) 3_665 . ? F MO3 MO2 84.89(13) . . ? XM MO3 MO2 142.70(10) 1_655 . ? XM MO3 MO2 90.64(14) 3_665 . ? Si2 MO3 MO2 56.64(4) . . ? Si1 MO3 MO2 118.68(7) 3_665 . ? MO2 MO3 MO2 114.85(5) 1_565 . ? O2 MO3 MO1 127.35(12) . 1_665 ? O1 MO3 MO1 34.08(9) 3_665 1_665 ? F MO3 MO1 139.05(10) 3_665 1_665 ? F MO3 MO1 96.10(14) . 1_665 ? XM MO3 MO1 36.14(8) 1_655 1_665 ? XM MO3 MO1 88.31(14) 3_665 1_665 ? Si2 MO3 MO1 122.54(7) . 1_665 ? Si1 MO3 MO1 62.25(5) 3_665 1_665 ? MO2 MO3 MO1 66.53(4) 1_565 1_665 ? MO2 MO3 MO1 178.57(6) . 1_665 ? O2 MO3 MO1 33.98(9) . 1_655 ? O1 MO3 MO1 125.51(12) 3_665 1_655 ? F MO3 MO1 96.05(14) 3_665 1_655 ? F MO3 MO1 138.20(10) . 1_655 ? XM MO3 MO1 88.33(13) 1_655 1_655 ? XM MO3 MO1 36.05(8) 3_665 1_655 ? Si2 MO3 MO1 61.89(5) . 1_655 ? Si1 MO3 MO1 122.21(6) 3_665 1_655 ? MO2 MO3 MO1 178.74(7) 1_565 1_655 ? MO2 MO3 MO1 66.35(4) . 1_655 ? MO1 MO3 MO1 112.27(5) 1_665 1_655 ? O5 Si1 O3 110.2(2) 1_545 . ? O5 Si1 O1 115.0(3) 1_545 . ? O3 Si1 O1 113.4(3) . . ? O5 Si1 O7 106.6(3) 1_545 . ? O3 Si1 O7 107.8(3) . . ? O1 Si1 O7 103.1(2) . . ? O5 Si1 AP 54.36(13) 1_545 2_645 ? O3 Si1 AP 58.21(14) . 2_645 ? O1 Si1 AP 149.74(16) . 2_645 ? O7 Si1 AP 107.16(14) . 2_645 ? O5 Si1 MO2 110.16(19) 1_545 . ? O3 Si1 MO2 137.4(2) . . ? O1 Si1 MO2 58.93(15) . . ? O7 Si1 MO2 46.79(13) . . ? AP Si1 MO2 148.61(6) 2_645 . ? O5 Si1 MO3 158.4(2) 1_545 3_665 ? O3 Si1 MO3 83.44(15) . 3_665 ? O1 Si1 MO3 43.48(18) . 3_665 ? O7 Si1 MO3 83.74(14) . 3_665 ? AP Si1 MO3 141.64(6) 2_645 3_665 ? MO2 Si1 MO3 62.92(5) . 3_665 ? O5 Si1 AP 43.2(3) 1_545 1_545 ? O3 Si1 AP 130.71(19) . 1_545 ? O1 Si1 AP 115.72(18) . 1_545 ? O7 Si1 AP 64.24(14) . 1_545 ? AP Si1 AP 77.14(4) 2_645 1_545 ? MO2 Si1 AP 75.01(4) . 1_545 ? MO3 Si1 AP 137.81(6) 3_665 1_545 ? O5 Si1 AP 126.70(19) 1_545 . ? O3 Si1 AP 41.1(3) . . ? O1 Si1 AP 117.98(18) . . ? O7 Si1 AP 66.99(14) . . ? AP Si1 AP 76.32(4) 2_645 . ? MO2 Si1 AP 101.56(5) . . ? MO3 Si1 AP 74.62(5) 3_665 . ? AP Si1 AP 112.87(6) 1_545 . ? O4 Si2 O6 109.3(2) . 1_545 ? O4 Si2 O2 114.1(3) . . ? O6 Si2 O2 115.0(3) 1_545 . ? O4 Si2 O7 107.2(3) . . ? O6 Si2 O7 107.4(3) 1_545 . ? O2 Si2 O7 103.25(19) . . ? O4 Si2 MH 58.40(14) . 2_645 ? O6 Si2 MH 53.56(13) 1_545 2_645 ? O2 Si2 MH 150.64(15) . 2_645 ? O7 Si2 MH 106.05(14) . 2_645 ? O4 Si2 MO2 137.5(2) . . ? O6 Si2 MO2 111.38(19) 1_545 . ? O2 Si2 MO2 57.31(14) . . ? O7 Si2 MO2 48.54(12) . . ? MH Si2 MO2 149.08(6) 2_645 . ? O4 Si2 MO3 82.52(15) . . ? O6 Si2 MO3 158.0(2) 1_545 . ? O2 Si2 MO3 43.43(18) . . ? O7 Si2 MO3 85.65(14) . . ? MH Si2 MO3 140.90(6) 2_645 . ? MO2 Si2 MO3 63.81(5) . . ? O4 Si2 AP 130.6(2) . 1_545 ? O6 Si2 AP 43.7(3) 1_545 1_545 ? O2 Si2 AP 115.16(19) . 1_545 ? O7 Si2 AP 64.82(15) . 1_545 ? MH Si2 AP 76.50(4) 2_645 1_545 ? MO2 Si2 AP 76.01(4) . 1_545 ? MO3 Si2 AP 139.74(6) . 1_545 ? O4 Si2 AP 40.2(3) . . ? O6 Si2 AP 126.09(18) 1_545 . ? O2 Si2 AP 118.39(18) . . ? O7 Si2 AP 67.33(14) . . ? MH Si2 AP 75.64(4) 2_645 . ? MO2 Si2 AP 103.01(4) . . ? MO3 Si2 AP 75.00(5) . . ? AP Si2 AP 113.68(6) 1_545 . ? Si1 O1 MO1 146.6(3) . . ? Si1 O1 MO3 108.1(2) . 3_665 ? MO1 O1 MO3 103.95(16) . 3_665 ? Si1 O1 MO2 90.46(17) . . ? MO1 O1 MO2 103.11(16) . . ? MO3 O1 MO2 82.38(12) 3_665 . ? Si2 O2 MO1 144.0(3) . 1_655 ? Si2 O2 MO3 108.0(2) . . ? MO1 O2 MO3 104.53(16) 1_655 . ? Si2 O2 MO2 91.46(17) . . ? MO1 O2 MO2 106.34(17) 1_655 . ? MO3 O2 MO2 84.91(12) . . ? Si1 O3 MH 135.3(4) . . ? Si1 O3 AP 113.2(4) . . ? MH O3 AP 102.19(14) . . ? Si1 O3 AP 90.83(17) . 2_645 ? MH O3 AP 105.9(2) . 2_645 ? AP O3 AP 104.9(2) . 2_645 ? Si2 O4 MH 136.9(4) . 1_655 ? Si2 O4 AP 114.5(4) . . ? MH O4 AP 100.82(13) 1_655 . ? Si2 O4 MH 90.61(17) . 2_645 ? MH O4 MH 104.3(2) 1_655 2_645 ? AP O4 MH 104.4(2) . 2_645 ? Si1 O5 MH 131.3(4) 1_565 . ? Si1 O5 AP 110.2(4) 1_565 . ? MH O5 AP 101.68(14) . . ? Si1 O5 AP 94.93(17) 1_565 2_655 ? MH O5 AP 109.3(2) . 2_655 ? AP O5 AP 108.0(2) . 2_655 ? Si2 O6 MH 133.4(4) 1_565 1_655 ? Si2 O6 AP 109.3(4) 1_565 . ? MH O6 AP 100.39(14) 1_655 . ? Si2 O6 MH 95.44(18) 1_565 2_655 ? MH O6 MH 109.2(2) 1_655 2_655 ? AP O6 MH 107.5(2) . 2_655 ? Si1 O7 Si2 156.1(2) . . ? Si1 O7 MO2 102.97(18) . . ? Si2 O7 MO2 100.16(18) . . ? Si1 O7 AP 86.56(16) . 1_545 ? Si2 O7 AP 85.71(16) . 1_545 ? MO2 O7 AP 94.08(12) . 1_545 ? Si1 O7 AP 84.41(15) . . ? Si2 O7 AP 83.88(16) . . ? MO2 O7 AP 134.30(15) . . ? AP O7 AP 131.57(12) 1_545 . ? MO1 XM MH 132.16(15) 1_565 . ? MO1 XM MO3 96.5(2) 1_565 1_455 ? MH XM MO3 114.3(3) . 1_455 ? MO1 XM MO3 96.4(2) 1_565 3_665 ? MH XM MO3 113.7(2) . 3_665 ? MO3 XM MO3 97.40(12) 1_455 3_665 ? MO2 F AP 122.10(13) 1_565 . ? MO2 F MO3 93.6(2) 1_565 3_665 ? AP F MO3 120.6(3) . 3_665 ? MO2 F MO3 93.2(2) 1_565 . ? AP F MO3 120.5(3) . . ? MO3 F MO3 100.39(12) 3_665 . ? _refine_diff_density_max 1.442 _refine_diff_density_min -2.430 _refine_diff_density_rms 0.195 _shelxl_version_number 2014-3 _shelx_res_file ; TITL nac in P2(1)/c CELL 0.71073 7.40686 5.65397 18.78703 90.0000 101.3650 90.0000 ZERR 2.00 0.00148 0.00113 0.00376 0.0000 0.0300 0.0000 LATT 1 SYMM -X, 0.5+Y, 0.5-Z SFAC O F NA SI CA NB Y Sr Ti Nd Ce Dy Sm Pr La Ho UNIT 30 6 5.64 8 6.12 1.28 .72 .28 .76 .32 .3 .16 .1 .02 .08 .04 ACTA SIZE 0.05 0.05 0.02 TWIN -1 0 0 0 -1 0 1 0 1 2 L.S. 6 OMIT -1 3 4 omit -3 55.0 BOND FMAP 2 PLAN 20 WGHT 0.051400 3.224800 BASF 0.45461 FVAR 0.25311 0.84201 0.72248 0.83392 1.09897 1.08575 MH 7 0.094697 0.660329 0.193463 21.00000 0.00914 0.00705 = 0.01226 0.00102 0.00119 0.00077 AP 8 0.596896 0.660776 0.189881 31.00000 0.01191 0.01166 = 0.01465 0.00063 0.00212 0.00104 MO1 6 0.000000 0.000000 0.000000 40.50000 0.00819 0.04901 = 0.02791 -0.02990 0.00461 -0.00578 MO2 3 0.500000 0.000000 0.000000 50.50000 0.02447 0.01853 = 0.01550 -0.00217 -0.00175 -0.00437 MO3 3 0.743543 0.500863 -0.000608 61.00000 0.02507 0.01072 = 0.02371 0.00718 0.00485 0.00242 SI1 4 0.350616 0.154884 0.140681 11.00000 0.01018 0.00758 = 0.00811 -0.00015 0.00102 0.00126 SI2 4 0.784506 0.154090 0.138086 11.00000 0.01196 0.00615 = 0.00803 -0.00073 0.00245 0.00119 O1 1 0.215581 0.147580 0.061551 11.00000 0.01163 0.01332 = 0.01321 0.00008 -0.00364 -0.00300 O2 1 0.834632 0.144023 0.057925 11.00000 0.01762 0.01631 = 0.01234 0.00341 0.00813 0.00520 O3 1 0.333580 0.395213 0.184895 11.00000 0.01393 0.01098 = 0.01833 -0.00533 0.00149 -0.00133 O4 1 0.846597 0.393946 0.181622 11.00000 0.01530 0.01099 = 0.01991 -0.00597 -0.00024 -0.00142 O5 1 0.336929 0.929233 0.191145 11.00000 0.01745 0.00858 = 0.01376 0.00231 0.00397 -0.00101 O6 1 0.854919 0.930965 0.189454 11.00000 0.01588 0.01036 = 0.01353 0.00227 0.00319 -0.00002 O7 1 0.557258 0.148426 0.120925 11.00000 0.01131 0.02650 = 0.01767 -0.00403 0.00461 0.00022 XM 2 0.030156 0.709455 0.063684 10.94390 0.01925 0.02141 = 0.01444 -0.00116 0.00084 0.00197 F 2 0.532568 0.661401 0.064982 11.00000 0.02786 0.01752 = 0.01805 0.00212 0.00173 0.00145 HKLF 4 REM nac in P2(1)/c REM R1 = 0.0350 for 1788 Fo > 4sig(Fo) and 0.0363 for all 1863 data REM 145 parameters refined using 0 restraints END WGHT 0.0513 3.2442 REM Highest difference peak 1.442, deepest hole -2.430, 1-sigma level 0.195 Q1 1 0.0796 0.6609 0.1521 11.00000 0.05 1.44 Q2 1 0.0086 -0.0163 0.0311 11.00000 0.05 1.29 Q3 1 0.5701 0.6638 0.1418 11.00000 0.05 1.29 Q4 1 0.6105 0.6606 0.2319 11.00000 0.05 1.19 Q5 1 0.1125 0.6606 0.2367 11.00000 0.05 1.17 Q6 1 1.0964 1.1029 0.1932 11.00000 0.05 0.95 Q7 1 -0.0227 0.6617 0.1807 11.00000 0.05 0.86 Q8 1 0.4989 0.6597 0.1866 11.00000 0.05 0.85 Q9 1 0.6038 0.1068 0.1897 11.00000 0.05 0.85 Q10 1 0.7059 0.6657 0.1934 11.00000 0.05 0.79 Q11 1 0.0061 0.7453 0.0140 11.00000 0.05 0.76 Q12 1 0.3124 0.1581 0.0982 11.00000 0.05 0.75 Q13 1 0.6527 0.1589 0.1289 11.00000 0.05 0.72 Q14 1 0.7101 0.1432 0.0546 11.00000 0.05 0.69 Q15 1 0.2563 0.1520 0.1417 11.00000 0.05 0.66 Q16 1 0.2025 0.6742 0.2028 11.00000 0.05 0.65 Q17 1 0.7868 0.1558 0.0971 11.00000 0.05 0.64 Q18 1 0.5044 -0.0064 0.0393 11.00000 0.05 0.63 Q19 1 0.0903 -0.0519 0.0084 11.00000 0.05 0.57 Q20 1 0.8836 0.1583 0.1377 11.00000 0.05 0.55 ; _shelx_res_checksum 13021 _shelx_hkl_file ; -1 0 0 19.88 1.16 1 0 0 19.22 0.58 -2 0 0 155.74 6.14 2 0 0 155.72 4.53 -3 0 0 1.99 0.28 3 0 0 1.94 0.21 -4 0 0 187.39 7.41 4 0 0 184.45 5.47 -5 0 0 75.82 3.26 5 0 0 75.50 2.69 -6 0 0 31.17 1.44 6 0 0 30.93 1.58 -7 0 0 8.28 0.94 7 0 0 8.69 1.10 -8 0 0 121.85 5.42 8 0 0 124.12 5.95 -9 0 0 95.93 4.48 9 0 0 93.41 6.11 -10 0 0 203.75 10.82 10 0 0 193.62 16.69 0 -1 0 1.58 0.15 0 1 0 1.35 0.17 -1 -1 0 32.39 1.67 1 -1 0 35.70 2.34 -1 1 0 33.14 2.24 1 1 0 27.45 1.06 -2 -1 0 3162.58 122.35 2 -1 0 3026.77 96.06 -2 1 0 3018.44 119.03 2 1 0 3061.11 70.89 -3 -1 0 14.93 0.95 3 -1 0 12.64 0.63 -3 1 0 11.72 0.78 3 1 0 14.97 0.58 -4 -1 0 150.90 6.39 4 -1 0 175.44 5.99 -4 1 0 163.52 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3.28 0.44 3 4 -7 2.19 0.64 -3 -4 7 1.81 0.62 -3 4 7 3.15 0.63 2 -4 -7 539.33 15.91 2 4 -7 528.41 21.25 -2 -4 7 513.58 19.78 -2 4 7 532.24 18.49 1 -4 -7 42.99 1.72 1 4 -7 38.97 1.71 -1 -4 7 33.70 1.60 -1 4 7 39.66 1.72 0 -4 -7 789.18 27.03 0 4 -7 706.00 28.27 0 -4 7 693.63 25.98 0 4 7 685.77 24.97 -1 -4 -7 28.33 1.59 -1 4 -7 23.50 1.45 1 -4 7 20.85 1.28 1 4 7 24.15 1.56 -2 -4 -7 63.89 3.24 -2 4 -7 63.40 2.99 2 -4 7 68.92 3.28 2 4 7 64.66 3.20 -3 -4 -7 16.78 1.47 -3 4 -7 21.27 1.22 3 -4 7 19.66 1.06 3 4 7 15.26 1.41 -4 -4 -7 250.78 11.37 -4 4 -7 253.51 12.78 4 -4 7 273.78 14.30 4 4 7 259.21 11.02 -5 -4 -7 18.06 2.12 -5 4 -7 23.10 1.75 5 -4 7 17.40 2.13 5 4 7 23.74 1.85 -6 -4 -7 29.11 2.89 -6 4 -7 28.88 2.09 6 -4 7 23.15 2.76 6 4 7 34.18 2.39 -7 -4 -7 26.04 2.83 -7 4 -7 27.64 2.10 7 -4 7 28.30 3.01 7 4 7 24.25 2.18 -8 -4 -7 100.26 6.90 -8 4 -7 107.52 5.16 8 -4 7 102.32 6.98 8 4 7 111.26 5.50 8 -5 -7 28.01 2.41 8 5 -7 29.70 4.15 -8 -5 7 26.20 2.76 -8 5 7 30.37 2.23 7 -5 -7 3.45 1.14 7 5 -7 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5.51 4 -1 21 90.33 6.05 4 1 21 85.44 4.70 7 -2 -21 13.82 1.56 7 2 -21 20.97 2.22 -7 -2 21 17.24 2.13 -7 2 21 13.41 1.93 6 -2 -21 67.26 3.66 6 2 -21 69.57 4.47 -6 -2 21 73.79 2.97 -6 2 21 70.62 3.62 5 -2 -21 4.32 1.24 5 2 -21 6.05 1.07 -5 -2 21 6.07 0.85 -5 2 21 7.30 1.11 4 -2 -21 200.84 10.82 4 2 -21 206.48 8.73 -4 -2 21 198.88 7.32 -4 2 21 220.37 11.15 3 -2 -21 66.61 4.45 3 2 -21 72.90 3.65 -3 -2 21 73.54 3.02 -3 2 21 77.57 4.72 2 -2 -21 144.26 8.26 2 2 -21 152.02 5.80 -2 -2 21 151.70 5.56 -2 2 21 154.97 6.96 1 -2 -21 8.83 1.51 1 2 -21 4.37 0.88 -1 -2 21 6.35 0.92 -1 2 21 7.35 1.44 0 -2 -21 19.37 1.74 0 2 -21 13.61 1.48 0 -2 21 12.66 1.25 0 2 21 16.75 2.09 -1 -2 -21 11.56 1.48 -1 2 -21 10.26 1.66 1 -2 21 11.25 1.43 1 2 21 9.50 1.74 -2 -2 -21 120.13 5.58 -2 2 -21 109.13 6.59 2 -2 21 104.72 7.04 2 2 21 114.89 6.90 -3 -2 -21 6.13 1.36 -3 2 -21 4.60 1.44 3 -2 21 5.10 1.67 3 2 21 7.73 1.40 -4 -2 -21 43.29 4.08 -4 2 -21 42.58 3.77 4 -2 21 49.94 4.32 4 2 21 41.57 3.21 7 -3 -21 10.59 1.44 7 3 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-21 1.24 1.39 3 4 -21 3.44 0.92 -3 -4 21 2.48 0.76 -3 4 21 3.50 1.35 2 -4 -21 3.64 1.50 2 4 -21 4.47 1.14 -2 -4 21 5.23 0.97 -2 4 21 3.44 1.41 1 -4 -21 11.84 2.13 1 4 -21 17.82 2.12 -1 -4 21 19.91 1.56 -1 4 21 13.28 2.93 0 -4 -21 25.42 2.30 0 4 -21 28.16 2.63 0 -4 21 22.78 1.74 0 4 21 19.76 2.48 -1 -4 -21 24.90 2.86 -1 4 -21 23.95 2.48 1 -4 21 24.94 2.78 1 4 21 21.46 2.65 -2 -4 -21 115.86 7.28 -2 4 -21 116.21 6.59 2 -4 21 119.80 7.37 2 4 21 101.63 6.96 3 -5 -21 -1.17 1.26 3 5 -21 0.68 1.06 -3 -5 21 0.33 0.76 -3 5 21 1.58 1.36 2 -5 -21 10.38 2.05 2 5 -21 8.90 1.74 -2 -5 21 7.51 1.16 -2 5 21 8.98 1.87 1 -5 -21 8.48 1.97 1 5 -21 6.77 2.43 -1 -5 21 6.74 1.10 -1 5 21 4.00 2.18 0 -5 -21 6.30 1.55 0 5 -21 7.44 1.64 0 -5 21 4.23 1.20 0 5 21 7.92 2.57 7 0 -22 1.16 0.85 -7 0 22 1.18 0.70 6 0 -22 1.60 0.84 -6 0 22 2.15 0.79 5 0 -22 40.98 2.54 -5 0 22 44.46 2.36 4 0 -22 246.10 10.82 -4 0 22 268.92 9.17 3 0 -22 48.61 2.72 -3 0 22 48.41 2.22 2 0 -22 41.46 2.66 -2 0 22 40.42 2.02 1 0 -22 0.67 1.03 -1 0 22 1.27 1.02 0 0 -22 322.88 16.70 0 0 22 326.05 17.15 -1 0 -22 15.03 2.01 1 0 22 12.34 1.98 -2 0 -22 175.22 9.71 2 0 22 178.05 9.98 -3 0 -22 -0.42 1.13 3 0 22 1.73 1.15 -4 0 -22 192.24 10.74 4 0 22 199.16 11.71 7 -1 -22 1.35 0.75 7 1 -22 0.40 1.05 -7 -1 22 2.11 1.27 -7 1 22 2.15 0.74 6 -1 -22 104.95 5.22 6 1 -22 119.16 5.36 -6 -1 22 115.37 4.95 -6 1 22 115.81 4.32 5 -1 -22 23.87 1.93 5 1 -22 26.48 2.02 -5 -1 22 26.24 1.54 -5 1 22 25.31 1.54 4 -1 -22 25.54 1.90 4 1 -22 22.80 1.62 -4 -1 22 22.96 1.49 -4 1 22 26.16 2.51 3 -1 -22 36.27 3.33 3 1 -22 46.07 2.30 -3 -1 22 46.43 2.15 -3 1 22 47.84 2.77 2 -1 -22 17.85 2.07 2 1 -22 18.34 1.41 -2 -1 22 15.51 1.35 -2 1 22 14.43 1.57 1 -1 -22 8.43 1.59 1 1 -22 7.10 1.15 -1 -1 22 7.99 1.00 -1 1 22 6.85 1.49 0 -1 -22 180.99 10.13 0 1 -22 189.90 10.15 0 -1 22 195.18 10.45 0 1 22 186.39 10.45 -1 -1 -22 7.42 1.57 -1 1 -22 8.17 1.62 1 -1 22 6.64 1.53 1 1 22 4.60 1.43 -2 -1 -22 275.73 14.46 -2 1 -22 263.91 14.36 2 -1 22 282.98 14.84 2 1 22 277.34 14.85 -3 -1 -22 21.25 2.56 -3 1 -22 24.67 2.69 3 -1 22 32.50 3.25 3 1 22 23.41 2.75 -4 -1 -22 108.81 6.68 -4 1 -22 104.80 6.68 4 -1 22 111.21 7.35 4 1 22 117.61 7.38 7 -2 -22 34.10 2.42 7 2 -22 27.82 2.84 -7 -2 22 33.39 3.06 -7 2 22 30.86 2.86 6 -2 -22 40.57 3.35 6 2 -22 43.76 3.59 -6 -2 22 47.15 2.23 -6 2 22 46.75 2.76 5 -2 -22 7.26 1.48 5 2 -22 8.60 1.23 -5 -2 22 8.47 0.95 -5 2 22 7.26 1.56 4 -2 -22 7.53 1.45 4 2 -22 4.30 1.06 -4 -2 22 4.98 0.85 -4 2 22 11.19 1.72 3 -2 -22 17.28 2.08 3 2 -22 21.40 1.77 -3 -2 22 19.60 1.36 -3 2 22 18.49 2.20 2 -2 -22 7.96 1.54 2 2 -22 8.84 1.06 -2 -2 22 8.79 1.04 -2 2 22 8.03 1.28 1 -2 -22 9.85 1.69 1 2 -22 12.44 1.39 -1 -2 22 11.03 1.17 -1 2 22 6.28 1.52 0 -2 -22 29.26 2.86 0 2 -22 34.20 2.35 0 -2 22 32.68 2.02 0 2 22 31.29 3.06 -1 -2 -22 13.16 1.87 -1 2 -22 12.73 1.86 1 -2 22 15.44 2.04 1 2 22 7.69 1.71 -2 -2 -22 124.20 5.95 -2 2 -22 114.58 7.02 2 -2 22 120.22 7.61 2 2 22 124.07 7.40 -3 -2 -22 9.65 1.59 -3 2 -22 7.11 1.62 3 -2 22 5.64 1.87 3 2 22 5.76 1.73 6 -3 -22 0.66 0.88 6 3 -22 0.44 0.92 -6 -3 22 1.31 0.75 -6 3 22 0.52 1.89 5 -3 -22 2.81 0.99 5 3 -22 2.63 1.01 -5 -3 22 1.31 0.73 -5 3 22 1.77 1.22 4 -3 -22 0.70 0.98 4 3 -22 0.23 0.88 -4 -3 22 0.51 0.67 -4 3 22 2.40 1.27 3 -3 -22 5.24 1.35 3 3 -22 4.68 1.08 -3 -3 22 4.08 0.83 -3 3 22 6.50 1.51 2 -3 -22 0.55 0.97 2 3 -22 0.54 0.87 -2 -3 22 -0.23 0.70 -2 3 22 0.44 1.15 1 -3 -22 5.30 1.44 1 3 -22 4.68 1.37 -1 -3 22 4.73 0.92 -1 3 22 6.12 1.54 0 -3 -22 20.03 2.56 0 3 -22 23.52 2.34 0 -3 22 21.05 1.63 0 3 22 18.70 2.37 -1 -3 -22 3.53 1.62 -1 3 -22 4.15 1.33 1 -3 22 6.11 2.37 1 3 22 2.43 1.37 -2 -3 -22 30.01 3.32 -2 3 -22 29.10 4.05 2 -3 22 31.51 3.31 2 3 22 31.67 3.34 -3 -3 -22 -0.32 1.55 -3 3 -22 0.11 1.58 3 -3 22 0.28 1.50 3 3 22 0.52 1.36 5 -4 -22 10.23 2.77 5 4 -22 17.95 2.18 -5 -4 22 12.38 1.25 -5 4 22 13.80 3.12 4 -4 -22 1.87 1.89 4 4 -22 0.75 0.95 -4 -4 22 0.80 0.74 -4 4 22 1.16 1.28 3 -4 -22 4.12 2.23 3 4 -22 6.80 1.27 -3 -4 22 4.10 0.86 -3 4 22 7.25 1.67 2 -4 -22 2.22 1.45 2 4 -22 2.43 1.04 -2 -4 22 2.13 0.87 -2 4 22 2.15 1.37 1 -4 -22 25.21 2.80 1 4 -22 20.31 2.34 -1 -4 22 22.23 1.74 -1 4 22 15.43 3.34 0 -4 -22 8.67 1.60 0 4 -22 16.07 1.99 0 -4 22 15.16 3.04 0 4 22 9.48 1.90 -1 -4 -22 13.49 2.30 -1 4 -22 13.28 1.95 1 -4 22 11.35 2.98 1 4 22 10.78 2.02 7 0 -23 4.24 1.12 -7 0 23 4.26 0.85 6 0 -23 0.58 0.84 -6 0 23 0.49 0.74 5 0 -23 2.92 0.96 -5 0 23 4.47 0.90 4 0 -23 0.35 0.79 -4 0 23 0.64 0.64 3 0 -23 33.72 2.40 -3 0 23 36.60 1.91 2 0 -23 -0.20 1.03 -2 0 23 0.66 1.05 1 0 -23 14.38 1.99 -1 0 23 14.50 2.01 0 0 -23 1.59 1.15 0 0 23 2.48 1.23 -1 0 -23 4.31 1.40 1 0 23 2.36 1.29 -2 0 -23 -0.28 1.16 2 0 23 1.23 1.22 -3 0 -23 16.84 2.29 3 0 23 12.41 2.13 7 -1 -23 14.78 1.64 7 1 -23 15.86 2.06 -7 -1 23 17.00 1.49 -7 1 23 17.85 1.35 6 -1 -23 0.54 0.83 6 1 -23 0.10 0.83 -6 -1 23 0.77 0.78 -6 1 23 1.66 0.71 5 -1 -23 5.45 1.08 5 1 -23 6.45 1.14 -5 -1 23 6.92 0.92 -5 1 23 8.63 1.25 4 -1 -23 3.05 1.23 4 1 -23 3.77 0.86 -4 -1 23 3.98 0.80 -4 1 23 3.92 1.32 3 -1 -23 35.47 3.12 3 1 -23 32.55 2.06 -3 -1 23 33.63 1.89 -3 1 23 38.37 2.55 2 -1 -23 10.15 1.64 2 1 -23 8.21 1.07 -2 -1 23 4.52 0.92 -2 1 23 5.92 1.48 1 -1 -23 6.79 1.52 1 1 -23 4.06 1.36 -1 -1 23 5.34 0.95 -1 1 23 4.96 1.49 0 -1 -23 91.84 5.72 0 1 -23 90.62 5.68 0 -1 23 94.98 5.87 0 1 23 93.53 5.91 -1 -1 -23 7.78 1.73 -1 1 -23 12.20 1.93 1 -1 23 11.61 1.86 1 1 23 7.66 1.79 -2 -1 -23 277.89 14.84 -2 1 -23 271.99 14.81 2 -1 23 290.87 15.30 2 1 23 291.36 15.35 -3 -1 -23 6.23 1.69 -3 1 -23 4.77 1.51 3 -1 23 3.76 1.85 3 1 23 7.39 1.79 6 -2 -23 106.48 6.64 6 2 -23 113.68 6.65 -6 -2 23 122.10 4.53 -6 2 23 114.03 5.44 5 -2 -23 31.68 3.02 5 2 -23 36.03 2.52 -5 -2 23 36.11 1.98 -5 2 23 41.91 3.42 4 -2 -23 4.17 1.33 4 2 -23 3.12 1.01 -4 -2 23 4.71 0.83 -4 2 23 4.46 1.47 3 -2 -23 1.75 1.12 3 2 -23 1.03 0.88 -3 -2 23 0.22 0.64 -3 2 23 0.32 1.13 2 -2 -23 120.27 6.75 2 2 -23 110.37 5.32 -2 -2 23 112.16 5.03 -2 2 23 121.69 6.92 1 -2 -23 7.70 1.66 1 2 -23 11.64 1.44 -1 -2 23 10.70 1.21 -1 2 23 11.93 1.86 0 -2 -23 118.18 7.24 0 2 -23 126.83 7.27 0 -2 23 133.29 5.52 0 2 23 124.33 7.56 -1 -2 -23 35.56 3.07 -1 2 -23 23.85 2.73 1 -2 23 28.61 2.88 1 2 23 30.67 3.06 -2 -2 -23 305.46 14.99 -2 2 -23 264.71 14.80 2 -2 23 261.92 22.16 2 2 23 293.74 15.47 -3 -2 -23 0.79 2.29 -3 2 -23 2.03 1.36 3 -2 23 0.71 1.59 3 2 23 1.14 1.43 5 -3 -23 26.68 2.26 5 3 -23 32.87 2.42 -5 -3 23 31.11 1.83 -5 3 23 32.98 3.08 4 -3 -23 159.05 9.25 4 3 -23 173.79 7.58 -4 -3 23 171.28 6.32 -4 3 23 175.83 9.60 3 -3 -23 14.82 2.00 3 3 -23 15.07 1.64 -3 -3 23 16.48 1.34 -3 3 23 17.67 2.30 2 -3 -23 131.67 7.57 2 3 -23 133.64 6.13 -2 -3 23 133.31 5.76 -2 3 23 135.20 11.06 1 -3 -23 5.27 2.33 1 3 -23 0.84 1.13 -1 -3 23 3.89 0.94 -1 3 23 1.50 1.28 0 -3 -23 198.18 15.88 0 3 -23 199.02 10.47 0 -3 23 199.29 9.54 0 3 23 197.39 11.15 -1 -3 -23 1.73 1.58 -1 3 -23 0.87 1.69 1 -3 23 0.09 1.91 1 3 23 1.51 1.37 -2 -3 -23 156.12 9.06 -2 3 -23 130.99 11.48 2 -3 23 140.96 12.67 2 3 23 150.78 8.90 4 -4 -23 9.77 2.88 4 4 -23 19.98 2.04 -4 -4 23 16.90 1.39 -4 4 23 15.56 2.29 3 -4 -23 15.12 3.23 3 4 -23 17.85 1.82 -3 -4 23 17.43 1.58 -3 4 23 13.43 2.18 2 -4 -23 101.38 9.57 2 4 -23 116.40 5.41 -2 -4 23 111.52 5.01 -2 4 23 100.25 9.47 1 -4 -23 16.88 2.52 1 4 -23 16.02 2.13 -1 -4 23 15.38 1.50 -1 4 23 16.84 3.34 0 -4 -23 241.20 11.10 0 4 -23 233.97 12.11 0 -4 23 222.61 18.47 0 4 23 218.48 12.77 6 0 -24 83.62 4.34 -6 0 24 91.45 4.08 5 0 -24 8.49 1.26 -5 0 24 9.56 1.17 4 0 -24 186.61 8.41 -4 0 24 199.04 7.10 3 0 -24 -0.02 1.09 -3 0 24 -0.14 0.66 2 0 -24 167.83 9.54 -2 0 24 179.30 9.84 1 0 -24 2.99 1.34 -1 0 24 2.71 1.34 0 0 -24 389.82 20.17 0 0 24 398.21 20.77 -1 0 -24 26.33 2.86 1 0 24 31.68 3.18 -2 0 -24 244.08 13.09 2 0 24 242.95 13.44 -3 0 -24 1.93 1.44 3 0 24 -1.66 1.83 6 -1 -24 4.67 1.09 6 1 -24 2.20 1.26 -6 -1 24 5.26 1.02 -6 1 24 3.43 1.12 5 -1 -24 4.00 1.05 5 1 -24 3.95 1.08 -5 -1 24 5.43 0.90 -5 1 24 5.75 1.17 4 -1 -24 185.27 10.69 4 1 -24 206.14 8.71 -4 -1 24 201.67 7.28 -4 1 24 197.81 10.97 3 -1 -24 19.38 2.29 3 1 -24 17.26 1.48 -3 -1 24 15.68 1.32 -3 1 24 17.88 1.85 2 -1 -24 263.72 14.28 2 1 -24 274.90 14.30 -2 -1 24 272.44 10.96 -2 1 24 280.31 14.74 1 -1 -24 15.28 2.11 1 1 -24 13.71 2.01 -1 -1 24 11.45 1.30 -1 1 24 13.70 2.10 0 -1 -24 212.41 11.57 0 1 -24 215.18 11.57 0 -1 24 207.57 11.84 0 1 24 221.41 11.97 -1 -1 -24 3.50 1.49 -1 1 -24 2.37 1.34 1 -1 24 1.37 1.33 1 1 24 2.88 1.50 -2 -1 -24 125.58 7.41 -2 1 -24 120.24 7.37 2 -1 24 123.10 7.58 2 1 24 129.30 7.72 6 -2 -24 6.00 1.53 6 2 -24 12.48 1.93 -6 -2 24 13.39 1.41 -6 2 24 10.17 1.93 5 -2 -24 18.49 2.36 5 2 -24 28.22 2.15 -5 -2 24 24.62 1.63 -5 2 24 23.09 2.67 4 -2 -24 20.02 2.46 4 2 -24 23.48 2.05 -4 -2 24 25.86 1.64 -4 2 24 24.36 2.71 3 -2 -24 3.08 1.31 3 2 -24 5.39 1.17 -3 -2 24 5.77 1.01 -3 2 24 3.73 1.54 2 -2 -24 109.29 6.96 2 2 -24 129.69 6.92 -2 -2 24 123.50 5.32 -2 2 24 117.24 7.18 1 -2 -24 26.61 2.74 1 2 -24 26.60 2.62 -1 -2 24 25.25 1.90 -1 2 24 29.18 2.94 0 -2 -24 147.26 8.50 0 2 -24 152.47 8.49 0 -2 24 149.58 8.77 0 2 24 151.30 8.86 -1 -2 -24 2.19 1.44 -1 2 -24 6.09 1.59 1 -2 24 4.80 1.55 1 2 24 3.09 1.48 -2 -2 -24 1.87 1.47 -2 2 -24 4.68 1.54 2 -2 24 3.38 2.37 2 2 24 3.40 1.62 5 -3 -24 18.95 2.32 5 3 -24 20.54 1.99 -5 -3 24 22.54 1.59 -5 3 24 19.39 2.50 4 -3 -24 19.51 2.39 4 3 -24 25.02 2.13 -4 -3 24 24.55 1.68 -4 3 24 23.03 2.70 3 -3 -24 18.41 2.29 3 3 -24 23.88 2.03 -3 -3 24 22.34 1.77 -3 3 24 24.74 2.75 2 -3 -24 27.91 2.84 2 3 -24 31.65 2.41 -2 -3 24 31.32 2.06 -2 3 24 25.04 4.16 1 -3 -24 -0.92 1.73 1 3 -24 2.97 1.34 -1 -3 24 1.30 0.89 -1 3 24 1.52 1.40 0 -3 -24 0.66 2.14 0 3 -24 0.22 1.16 0 -3 24 0.55 1.26 0 3 24 2.23 1.45 -1 -3 -24 24.11 4.14 -1 3 -24 26.70 3.92 1 -3 24 25.95 4.18 1 3 24 18.51 2.64 6 0 -25 0.13 0.90 -6 0 25 0.18 0.82 5 0 -25 21.57 1.89 -5 0 25 19.25 1.64 4 0 -25 1.11 1.21 -4 0 25 -0.05 0.71 3 0 -25 -0.13 1.17 -3 0 25 -1.23 1.09 2 0 -25 1.09 1.25 -2 0 25 0.00 1.08 1 0 -25 23.12 2.62 -1 0 25 20.65 2.62 0 0 -25 2.98 1.39 0 0 25 0.75 1.32 -1 0 -25 3.39 1.54 1 0 25 3.46 1.60 -2 0 -25 -0.71 1.25 2 0 25 1.68 1.45 5 -1 -25 3.93 1.40 5 1 -25 5.40 1.21 -5 -1 25 3.08 0.96 -5 1 25 4.90 1.53 4 -1 -25 80.53 7.58 4 1 -25 72.56 4.06 -4 -1 25 81.04 3.39 -4 1 25 86.66 5.34 3 -1 -25 21.95 2.53 3 1 -25 23.38 1.74 -3 -1 25 18.62 1.65 -3 1 25 25.28 2.71 2 -1 -25 280.84 14.95 2 1 -25 278.79 14.93 -2 -1 25 291.87 11.47 -2 1 25 282.64 15.36 1 -1 -25 0.61 1.31 1 1 -25 1.52 1.29 -1 -1 25 4.49 1.53 -1 1 25 1.97 1.44 0 -1 -25 15.39 2.14 0 1 -25 7.76 1.80 0 -1 25 6.48 1.75 0 1 25 10.07 2.00 -1 -1 -25 6.44 1.68 -1 1 -25 6.76 1.78 1 -1 25 5.05 1.66 1 1 25 9.33 1.99 -2 -1 -25 1.03 1.37 -2 1 -25 -0.27 1.29 2 -1 25 -1.44 2.00 2 1 25 -0.54 1.38 5 -2 -25 21.95 2.58 5 2 -25 23.78 2.54 -5 -2 25 21.27 1.55 -5 2 25 21.17 2.63 4 -2 -25 36.90 3.59 4 2 -25 47.70 3.06 -4 -2 25 50.24 2.38 -4 2 25 46.96 3.83 3 -2 -25 6.86 1.64 3 2 -25 7.58 1.35 -3 -2 25 6.79 1.13 -3 2 25 6.00 2.36 2 -2 -25 274.75 14.49 2 2 -25 287.69 14.15 -2 -2 25 269.04 11.07 -2 2 25 271.19 14.82 1 -2 -25 6.09 1.65 1 2 -25 6.31 2.23 -1 -2 25 5.13 1.06 -1 2 25 8.41 1.83 0 -2 -25 143.51 8.09 0 2 -25 145.84 11.27 0 -2 25 131.56 8.23 0 2 25 140.02 8.40 -1 -2 -25 0.85 1.43 -1 2 -25 1.59 1.38 1 -2 25 0.40 1.32 1 2 25 0.66 1.40 3 -3 -25 0.80 1.18 3 3 -25 -0.15 0.98 -3 -3 25 1.07 0.86 -3 3 25 1.50 2.10 2 -3 -25 149.71 12.64 2 3 -25 149.39 8.35 -2 -3 25 147.86 6.48 -2 3 25 154.99 12.49 1 -3 -25 22.11 4.22 1 3 -25 27.99 2.81 -1 -3 25 28.13 2.03 -1 3 25 24.72 2.94 5 0 -26 1.02 1.02 -5 0 26 2.86 0.99 4 0 -26 182.69 10.34 -4 0 26 190.37 7.84 3 0 -26 17.20 2.32 -3 0 26 16.49 2.35 2 0 -26 233.83 12.72 -2 0 26 238.75 13.05 1 0 -26 6.90 1.78 -1 0 26 5.74 1.70 0 0 -26 183.46 10.37 0 0 26 188.11 10.77 -1 0 -26 0.65 1.45 1 0 26 0.68 1.47 4 -1 -26 111.22 9.77 4 1 -26 109.48 5.33 -4 -1 26 108.99 4.97 -4 1 26 110.66 6.78 3 -1 -26 4.24 1.58 3 1 -26 4.24 1.51 -3 -1 26 3.95 1.00 -3 1 26 5.46 1.67 2 -1 -26 134.49 7.63 2 1 -26 120.38 7.46 -2 -1 26 130.67 5.67 -2 1 26 124.03 7.74 1 -1 -26 6.22 1.77 1 1 -26 10.48 1.96 -1 -1 26 6.17 1.75 -1 1 26 7.81 1.87 0 -1 -26 12.45 2.08 0 1 -26 12.59 2.16 0 -1 26 10.51 2.10 0 1 26 8.68 2.00 3 -2 -26 0.65 1.23 3 2 -26 1.14 1.09 -3 -2 26 0.05 0.87 -3 2 26 -3.19 1.62 2 -2 -26 4.53 1.59 2 2 -26 -2.43 1.43 -2 -2 26 4.58 1.08 -2 2 26 2.96 1.50 1 -2 -26 1.56 1.42 1 2 -26 1.94 1.79 -1 -2 26 0.75 0.93 -1 2 26 1.86 1.53 3 0 -27 1.09 1.39 -3 0 27 1.44 1.35 2 0 -27 -0.67 1.29 -2 0 27 0.67 1.40 1 0 -27 -0.40 1.33 -1 0 27 0.54 1.46 2 -1 -27 0.56 1.38 2 1 -27 2.18 1.42 -2 -1 27 0.95 1.41 -2 1 27 2.42 1.52 0 0 0 0.00 0.00 ; _shelx_hkl_checksum 14734 # start Validation Reply Form _vrf_ABSMU01_nacareniobsite-Y ; PROBLEM: The ratio of given/expected absorption coefficient lies RESPONSE: The chemical formula of nacareniobsite-(Y) 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_SHFSU01_nacareniobsite-Y ; PROBLEM: The absolute value of parameter shift to su ratio > 0.20 RESPONSE: The absolute value of parameter shift for U13 is due to the occurrence of both Na and Ca at the large [8]-coordinated MO2 site. ; _vrf_PLAT051_nacareniobsite-Y ; PROBLEM: Mu(calc) and Mu(CIF) Ratio Differs from 1.0 by . 112.72 % RESPONSE: Mu(calc) is based on ideal formula and Mu(CIF) on the data from electron-microprobe analysis, with heavier scatters. ; _vrf_PLAT075_nacareniobsite-Y ; PROBLEM: Occupancy 1.099 Greater Than 1.0 for ...... MO2 RESPONSE: Besides Na, this particular site is occupied by a heavier cation such as Ca. That is why occupancy of the site is greater than 1. ; _vrf_PLAT080_nacareniobsite-Y ; PROBLEM: Maximum Shift/Error ............................ 0.87 Why ? RESPONSE: Maximum Shift/Error for U13 is due the occurrence of both Na and Ca at the large [8]-coordinated MO2 site. ; # end Validation Reply Form PLATON