#======================================================================= data_global #======================================================================= _audit_creation_method 'Jana2006 Version : 25/10/2015' # 1. PROCESSING SUMMARY (IUCr Office Use Only) _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_date_printers_first ? _journal_date_printers_final ? _journal_date_proofs_out ? _journal_date_proofs_in ? _journal_coeditor_name ? _journal_coeditor_code ? _journal_coeditor_notes ; ? ; _journal_techeditor_code ? _journal_paper_category ? _journal_techeditor_notes ; ? ; _journal_coden_ASTM ? _journal_name_full 'Acta Crystallographica Section C' _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? #======================================================================= # 2. SUBMISSION DETAILS _publ_contact_author_name ? _publ_contact_author_address ; ? ; _publ_contact_author_email ? _publ_contact_author_fax ? _publ_contact_author_phone ? _publ_requested_journal 'Acta Crystallographica Section C' _publ_requested_category ? _publ_contact_letter ; ? ; #======================================================================= # 3. TITLE AND AUTHOR LIST _publ_section_title ; ? ; _publ_section_title_footnote ; ? ; loop_ _publ_author_name _publ_author_footnote _publ_author_address ; ? # name ; ; ? # footnote ; ; ? # address ; #======================================================================= # 4. TEXT _publ_section_synopsis ; ? ; _publ_section_abstract ; ? ; _publ_section_comment ; ? ; _publ_section_introduction ; ? ; _publ_section_experimental ; ? ; _publ_section_exptl_prep ; ? ; _publ_section_exptl_refinement ; ? ; _publ_section_exptl_solution ; ? ; _publ_section_discussion ; ? ; _publ_section_acknowledgements ; ? ; _publ_section_references ; Petricek, V., Dusek, M. & Palatinus L. (2014). Z. Kristallogr. 229(5), 345-352. Palatinus L. & Chapuis G. (2007). J. Appl. Cryst. 40, 786-790. # enable this reference if Diamond ver. 2 was used for visualization #Brandenburg, K. (1999). DIAMOND. Version. 2.1c. #Crystal Impact GbR, Bonn, Germany. # enable this reference if Diamond ver. 3 was used for visualization #Brandenburg, K. & Putz, H. (2005). DIAMOND Version 3. #Crystal Impact GbR, Postfach 1251, D-53002 Bonn, Germany. # enable this reference if SIR97 was used for solving of the structure #Altomare, A., Burla, M. C., Camalli, M., Cascarano, G., Giacovazzo, C., #Guagliardi, A., Moliterni, A. G. G., Polidori, G., Spagna, R. (1997). #SIR97. A Package for Crystal Structure Solution by Direct Methods #and Refinement, Bari, Rome, Italy. # use this reference if SIR2002 was used for solving of the structure #Burla, M.C., Camalli, M., Carrozzini, B., Cascarano, G., Giacovazzo, C., #Polidori, G., Spagna, R. #SIR2002: the program, J. Appl. Cryst, (2003). 36, 1103 # use this reference if SIR2011 was used for solving of the structure #Burla, M.C., Caliandro, R., Camalli, M., Carrozzini, B., Cascarano, #G.L., Giacovazzo, C., Mallamo. M., Mazzone, A., Polidori, G., Spagna, R. #SIR2011: a new package for crystal structure determination and refinement, #J.Appl.Cryst. (2012) 45, 357-361 # enable this reference if bond valences were calculated #Brown, I. D. (1996). J. Appl. Cryst. 29, 479-480. # enable this reference if Xshape wase used for crystal shape refinement #Stoe & Cie (1998). X-SHAPE. Stoe & Cie, Darmstadt, Germany. # enable this reference if Flack coefficient was refined #Flack, H. D. (1983). Acta Cryst. A39, 876-881. ; _publ_section_figure_captions ; ? ; _publ_section_table_legends ; ? ; #======================================================================= data_I #======================================================================= # 5. CHEMICAL DATA _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_iupac ? _chemical_formula_sum 'Na1 O6 Sc1 Si2' _chemical_formula_weight 220.1 _chemical_melting_point ? _chemical_compound_source ? _chemical_absolute_configuration . #======================================================================= # 6. CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 1 2/c 1' _symmetry_space_group_name_Hall '-C 2yc' _symmetry_Int_Tables_number 15 loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 x,y,z 2 -x,y,-z+1/2 3 -x,-y,-z 4 x,-y,z+1/2 5 x+1/2,y+1/2,z 6 -x+1/2,y+1/2,-z+1/2 7 -x+1/2,-y+1/2,-z 8 x+1/2,-y+1/2,z+1/2 _cell_length_a 9.8478 _cell_length_b 9.0575 _cell_length_c 5.3409 _cell_angle_alpha 90 _cell_angle_beta 106.8709 _cell_angle_gamma 90 _cell_volume 455.886 loop_ _twin_individual_id _twin_individual_mass_fraction_refined _twin_individual_twin_matrix_11 _twin_individual_twin_matrix_12 _twin_individual_twin_matrix_13 _twin_individual_twin_matrix_21 _twin_individual_twin_matrix_22 _twin_individual_twin_matrix_23 _twin_individual_twin_matrix_31 _twin_individual_twin_matrix_32 _twin_individual_twin_matrix_33 ? ? ? ? ? ? ? ? ? ? ? _cell_formula_units_Z 4 _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _cell_measurement_temperature 293 _cell_special_details ; ? ; _exptl_crystal_density_diffrn 3.207 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_F_000 432 _exptl_absorpt_coefficient_mu 2.186 _exptl_crystal_description ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_size_rad ? _exptl_crystal_colour ? _exptl_absorpt_correction_type ? _exptl_absorpt_process_details ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist ? ? ? ? #======================================================================= # 7. EXPERIMENTAL DATA _exptl_special_details ? _diffrn_ambient_temperature 293 _diffrn_source ? _diffrn_source_power ? _diffrn_source_voltage ? _diffrn_source_current ? _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_monochromator ? _diffrn_measurement_device ? _diffrn_measurement_device_type ? _diffrn_detector ? _diffrn_detector_area_resol_mean ? _diffrn_measurement_method ? _diffrn_measurement_specimen_support ? _diffrn_reflns_number 1609 _diffrn_reflns_theta_min 3.12 _diffrn_reflns_theta_max 28.58 _diffrn_reflns_theta_full 27.69 _diffrn_measured_fraction_theta_max 0.93 _diffrn_measured_fraction_theta_full 0.98 _diffrn_reflns_av_R_equivalents 0.0483 _diffrn_reflns_av_unetI/netI 0.0516 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -7 _diffrn_reflns_limit_l_max 6 _diffrn_reflns_reduction_process ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? _diffrn_radiation_probe X-ray #======================================================================= # 8. REFINEMENT DATA _refine_special_details ; ? ; _reflns_number_total 540 _reflns_number_gt 382 _reflns_threshold_expression 'I>3\s(I)' _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.0412 _refine_ls_wR_factor_gt 0.0423 _refine_ls_R_factor_all 0.0627 _refine_ls_wR_factor_ref 0.0458 _refine_ls_goodness_of_fit_ref 1.42 _refine_ls_goodness_of_fit_gt 1.59 _refine_ls_restrained_S_gt ? _refine_ls_restrained_S_all ? _refine_ls_number_reflns 540 _refine_ls_number_parameters 49 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_weighting_scheme sigma _refine_ls_weighting_details 'w=1/(\s^2^(F)+0.0001F^2^)' _refine_ls_hydrogen_treatment ? _refine_ls_shift/su_max 0.0500 _refine_ls_shift/su_mean 0.0065 _refine_diff_density_max 0.56 _refine_diff_density_min -0.71 _refine_ls_extinction_method 'none' _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_abs_structure_Rogers ? loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Na 0.0362 0.0249 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' O 0.0106 0.0060 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' Sc 0.2519 0.3716 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' Si 0.0817 0.0704 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement ? _computing_molecular_graphics ? _computing_publication_material ? loop_ _restr_distance_atom_site_label_1 _restr_distance_site_symmetry_1 _restr_distance_atom_site_label_2 _restr_distance_site_symmetry_2 _restr_distance_target _restr_distance_target_weight_param ? ? ? ? ? ? loop_ _restr_angle_atom_site_label_1 _restr_angle_site_symmetry_1 _restr_angle_atom_site_label_2 _restr_angle_site_symmetry_2 _restr_angle_atom_site_label_3 _restr_angle_site_symmetry_3 _restr_angle_target _restr_angle_target_weight_param ? ? ? ? ? ? ? ? loop_ _restr_torsion_atom_site_label_1 _restr_torsion_site_symmetry_1 _restr_torsion_atom_site_label_2 _restr_torsion_site_symmetry_2 _restr_torsion_atom_site_label_3 _restr_torsion_site_symmetry_3 _restr_torsion_atom_site_label_4 _restr_torsion_site_symmetry_4 _restr_torsion_angle_target _restr_torsion_weight_param ? ? ? ? ? ? ? ? ? ? loop_ _restr_equal_distance_atom_site_label_1 _restr_equal_distance_site_symmetry_1 _restr_equal_distance_atom_site_label_2 _restr_equal_distance_site_symmetry_2 _restr_equal_distance_class_class_id _restr_equal_distance_class_target_weight_param ? ? ? ? ? ? loop_ _restr_equal_angle_atom_site_label_1 _restr_equal_angle_site_symmetry_1 _restr_equal_angle_atom_site_label_2 _restr_equal_angle_site_symmetry_2 _restr_equal_angle_atom_site_label_3 _restr_equal_angle_site_symmetry_3 _restr_equal_angle_class_class_id _restr_equal_angle_class_target_weight_param ? ? ? ? ? ? ? ? loop_ _restr_equal_torsion_atom_site_label_1 _restr_equal_torsion_site_symmetry_1 _restr_equal_torsion_atom_site_label_2 _restr_equal_torsion_site_symmetry_2 _restr_equal_torsion_atom_site_label_3 _restr_equal_torsion_site_symmetry_3 _restr_equal_torsion_atom_site_label_4 _restr_equal_torsion_site_symmetry_4 _restr_equal_torsion_class_class_id _restr_equal_torsion_class_target_weight_param ? ? ? ? ? ? ? ? ? ? #======================================================================= # 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_adp_type _atom_site_U_iso_or_equiv _atom_site_site_symmetry_multiplicity _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Na1 Na 0 0.3040(3) 0.25 Uani 0.0191(10) 4 1.048(8) d . . . Sc1 Sc 0 0.89719(13) 0.25 Uani 0.0094(4) 4 1.017(5) d . . . Si1 Si 0.29094(14) 0.08780(14) 0.2432(2) Uani 0.0104(4) 8 1 d . . . O1 O 0.1181(3) 0.0795(3) 0.1464(5) Uani 0.0107(10) 8 1 d . . . O2 O 0.3600(3) 0.2472(3) 0.3095(6) Uani 0.0141(11) 8 1 d . . . O3 O 0.3495(3) 0.0093(3) 0.0152(6) Uani 0.0130(11) 8 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_type_symbol _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Na1 Na 0.0215(17) 0.0149(15) 0.0141(14) 0 -0.0055(11) 0 Sc1 Sc 0.0078(7) 0.0099(6) 0.0098(6) 0 0.0013(5) 0 Si1 Si 0.0081(7) 0.0115(7) 0.0106(6) 0.0001(6) 0.0014(5) 0.0003(5) O1 O 0.0080(17) 0.0132(16) 0.0103(15) -0.0002(14) 0.0016(13) 0.0010(13) O2 O 0.0127(19) 0.0143(17) 0.0143(16) -0.0016(14) 0.0025(13) -0.0013(13) O3 O 0.0095(17) 0.0173(17) 0.0114(16) -0.0022(14) 0.0018(13) -0.0018(14) loop_ _jana_atom_site_ADP_C_label _jana_atom_site_ADP_C_type_symbol _jana_atom_site_ADP_C_111 _jana_atom_site_ADP_C_112 _jana_atom_site_ADP_C_113 _jana_atom_site_ADP_C_122 _jana_atom_site_ADP_C_123 _jana_atom_site_ADP_C_133 _jana_atom_site_ADP_C_222 _jana_atom_site_ADP_C_223 _jana_atom_site_ADP_C_233 _jana_atom_site_ADP_C_333 ? ? ? ? ? ? ? ? ? ? ? ? loop_ _jana_atom_site_ADP_D_label _jana_atom_site_ADP_D_type_symbol _jana_atom_site_ADP_D_1111 _jana_atom_site_ADP_D_1112 _jana_atom_site_ADP_D_1113 _jana_atom_site_ADP_D_1122 _jana_atom_site_ADP_D_1123 _jana_atom_site_ADP_D_1133 _jana_atom_site_ADP_D_1222 _jana_atom_site_ADP_D_1223 _jana_atom_site_ADP_D_1233 _jana_atom_site_ADP_D_1333 _jana_atom_site_ADP_D_2222 _jana_atom_site_ADP_D_2223 _jana_atom_site_ADP_D_2233 _jana_atom_site_ADP_D_2333 _jana_atom_site_ADP_D_3333 ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? loop_ _jana_atom_site_ADP_E_label _jana_atom_site_ADP_E_type_symbol _jana_atom_site_ADP_E_11111 _jana_atom_site_ADP_E_11112 _jana_atom_site_ADP_E_11113 _jana_atom_site_ADP_E_11122 _jana_atom_site_ADP_E_11123 _jana_atom_site_ADP_E_11133 _jana_atom_site_ADP_E_11222 _jana_atom_site_ADP_E_11223 _jana_atom_site_ADP_E_11233 _jana_atom_site_ADP_E_11333 _jana_atom_site_ADP_E_12222 _jana_atom_site_ADP_E_12223 _jana_atom_site_ADP_E_12233 _jana_atom_site_ADP_E_12333 _jana_atom_site_ADP_E_13333 _jana_atom_site_ADP_E_22222 _jana_atom_site_ADP_E_22223 _jana_atom_site_ADP_E_22233 _jana_atom_site_ADP_E_22333 _jana_atom_site_ADP_E_23333 _jana_atom_site_ADP_E_33333 ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? loop_ _jana_atom_site_ADP_F_label _jana_atom_site_ADP_F_type_symbol _jana_atom_site_ADP_F_111111 _jana_atom_site_ADP_F_111112 _jana_atom_site_ADP_F_111113 _jana_atom_site_ADP_F_111122 _jana_atom_site_ADP_F_111123 _jana_atom_site_ADP_F_111133 _jana_atom_site_ADP_F_111222 _jana_atom_site_ADP_F_111223 _jana_atom_site_ADP_F_111233 _jana_atom_site_ADP_F_111333 _jana_atom_site_ADP_F_112222 _jana_atom_site_ADP_F_112223 _jana_atom_site_ADP_F_112233 _jana_atom_site_ADP_F_112333 _jana_atom_site_ADP_F_113333 _jana_atom_site_ADP_F_122222 _jana_atom_site_ADP_F_122223 _jana_atom_site_ADP_F_122233 _jana_atom_site_ADP_F_122333 _jana_atom_site_ADP_F_123333 _jana_atom_site_ADP_F_133333 _jana_atom_site_ADP_F_222222 _jana_atom_site_ADP_F_222223 _jana_atom_site_ADP_F_222233 _jana_atom_site_ADP_F_222333 _jana_atom_site_ADP_F_223333 _jana_atom_site_ADP_F_233333 _jana_atom_site_ADP_F_333333 ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? #======================================================================= # 10. MOLECULAR GEOMETRY loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Na1 Si1 . 7_556 3.0482(13) ? Na1 Si1 . 8_454 3.0482(13) ? Na1 O1 . . 2.483(4) ? Na1 O1 . 2_555 2.483(4) ? Na1 O2 . 7_556 2.402(3) ? Na1 O2 . 8_454 2.402(3) ? Na1 O3 . 5_455 2.480(3) ? Na1 O3 . 6_555 2.480(3) ? Na1 O3 . 7_555 2.878(4) ? Na1 O3 . 8_455 2.878(4) ? Sc1 O1 . 1_565 2.182(3) ? Sc1 O1 . 2_565 2.182(3) ? Sc1 O1 . 3_565 2.109(3) ? Sc1 O1 . 4_565 2.109(3) ? Sc1 O2 . 5_455 2.025(3) ? Sc1 O2 . 6_555 2.025(3) ? Si1 Si1 . 4_554 3.1082(18) ? Si1 Si1 . 4_555 3.1082(18) ? Si1 O1 . . 1.631(3) ? Si1 O2 . . 1.591(3) ? Si1 O3 . . 1.652(4) ? Si1 O3 . 4_555 1.652(3) ? O1 O1 . 2_555 2.850(5) ? O1 O1 . 3_555 2.796(4) ? O1 O1 . 4_554 3.034(4) ? O1 O1 . 4_555 3.034(4) ? O1 O2 . . 2.745(4) ? O1 O2 . 6_545 3.022(4) ? O1 O2 . 7_555 2.957(4) ? O1 O2 . 8_454 3.083(4) ? O1 O3 . . 2.649(5) ? O1 O3 . 4_555 2.667(4) ? O2 O2 . 2_655 3.005(5) ? O2 O3 . . 2.652(4) ? O2 O3 . 7_555 3.170(4) ? O2 O3 . 4_555 2.585(4) ? O3 O3 . 3_655 3.020(5) ? O3 O3 . 4_554 2.676(4) ? O3 O3 . 4_555 2.676(4) ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag Si1 Na1 Si1 7_556 . 8_454 142.48(9) ? Si1 Na1 O1 7_556 . . 102.82(7) ? Si1 Na1 O1 7_556 . 2_555 107.74(7) ? Si1 Na1 O2 7_556 . 7_556 31.18(8) ? Si1 Na1 O2 7_556 . 8_454 168.44(11) ? Si1 Na1 O3 7_556 . 5_455 111.01(10) ? Si1 Na1 O3 7_556 . 6_555 32.77(7) ? Si1 Na1 O3 7_556 . 7_555 86.35(7) ? Si1 Na1 O3 7_556 . 8_455 71.67(7) ? Si1 Na1 O1 8_454 . . 107.74(7) ? Si1 Na1 O1 8_454 . 2_555 102.82(7) ? Si1 Na1 O2 8_454 . 7_556 168.44(11) ? Si1 Na1 O2 8_454 . 8_454 31.18(8) ? Si1 Na1 O3 8_454 . 5_455 32.77(7) ? Si1 Na1 O3 8_454 . 6_555 111.01(10) ? Si1 Na1 O3 8_454 . 7_555 71.67(7) ? Si1 Na1 O3 8_454 . 8_455 86.35(7) ? O1 Na1 O1 . . 2_555 70.07(13) ? O1 Na1 O2 . . 7_556 83.54(11) ? O1 Na1 O2 . . 8_454 78.26(11) ? O1 Na1 O3 . . 5_455 138.69(10) ? O1 Na1 O3 . . 6_555 118.48(10) ? O1 Na1 O3 . . 7_555 91.73(10) ? O1 Na1 O3 . . 8_455 158.80(11) ? O1 Na1 O2 2_555 . 7_556 78.26(11) ? O1 Na1 O2 2_555 . 8_454 83.54(11) ? O1 Na1 O3 2_555 . 5_455 118.48(10) ? O1 Na1 O3 2_555 . 6_555 138.69(10) ? O1 Na1 O3 2_555 . 7_555 158.80(11) ? O1 Na1 O3 2_555 . 8_455 91.73(10) ? O2 Na1 O2 7_556 . 8_454 157.75(15) ? O2 Na1 O3 7_556 . 5_455 136.82(13) ? O2 Na1 O3 7_556 . 6_555 63.91(10) ? O2 Na1 O3 7_556 . 7_555 111.35(10) ? O2 Na1 O3 7_556 . 8_455 82.11(10) ? O2 Na1 O3 8_454 . 5_455 63.91(10) ? O2 Na1 O3 8_454 . 6_555 136.82(13) ? O2 Na1 O3 8_454 . 7_555 82.11(10) ? O2 Na1 O3 8_454 . 8_455 111.35(10) ? O3 Na1 O3 5_455 . 6_555 82.83(12) ? O3 Na1 O3 5_455 . 7_555 68.16(11) ? O3 Na1 O3 5_455 . 8_455 59.37(10) ? O3 Na1 O3 6_555 . 7_555 59.37(10) ? O3 Na1 O3 6_555 . 8_455 68.16(11) ? O3 Na1 O3 7_555 . 8_455 108.00(12) ? O1 Sc1 O1 1_565 . 2_565 81.58(13) ? O1 Sc1 O1 1_565 . 3_565 81.31(11) ? O1 Sc1 O1 1_565 . 4_565 89.99(11) ? O1 Sc1 O2 1_565 . 5_455 169.99(11) ? O1 Sc1 O2 1_565 . 6_555 91.76(13) ? O1 Sc1 O1 2_565 . 3_565 89.99(11) ? O1 Sc1 O1 2_565 . 4_565 81.31(11) ? O1 Sc1 O2 2_565 . 5_455 91.76(13) ? O1 Sc1 O2 2_565 . 6_555 169.99(11) ? O1 Sc1 O1 3_565 . 4_565 168.53(13) ? O1 Sc1 O2 3_565 . 5_455 91.28(12) ? O1 Sc1 O2 3_565 . 6_555 96.41(12) ? O1 Sc1 O2 4_565 . 5_455 96.41(12) ? O1 Sc1 O2 4_565 . 6_555 91.28(12) ? O2 Sc1 O2 5_455 . 6_555 95.77(14) ? Na1 Si1 Si1 7_556 . 4_554 139.38(6) ? Na1 Si1 Si1 7_556 . 4_555 64.54(5) ? Na1 Si1 O1 7_556 . . 132.08(13) ? Na1 Si1 O2 7_556 . . 51.38(11) ? Na1 Si1 O3 7_556 . . 120.19(12) ? Na1 Si1 O3 7_556 . 4_555 54.34(11) ? Si1 Si1 Si1 4_554 . 4_555 118.44(5) ? Si1 Si1 O1 4_554 . . 87.96(12) ? Si1 Si1 O2 4_554 . . 123.29(14) ? Si1 Si1 O3 4_554 . . 19.82(11) ? Si1 Si1 O3 4_554 . 4_555 113.33(13) ? Si1 Si1 O1 4_555 . . 89.35(12) ? Si1 Si1 O2 4_555 . . 112.32(12) ? Si1 Si1 O3 4_555 . . 120.00(12) ? Si1 Si1 O3 4_555 . 4_555 19.83(13) ? O1 Si1 O2 . . . 116.82(17) ? O1 Si1 O3 . . . 107.58(16) ? O1 Si1 O3 . . 4_555 108.67(18) ? O2 Si1 O3 . . . 109.68(19) ? O2 Si1 O3 . . 4_555 105.65(15) ? O3 Si1 O3 . . 4_555 108.16(17) ? Na1 O1 Sc1 . . 1_545 104.17(14) ? Na1 O1 Sc1 . . 3_565 89.11(10) ? Na1 O1 Si1 . . . 113.89(15) ? Na1 O1 O1 . . 2_555 54.96(10) ? Na1 O1 O1 . . 3_555 100.33(12) ? Na1 O1 O1 . . 4_554 134.80(11) ? Na1 O1 O1 . . 4_555 94.19(12) ? Na1 O1 O2 . . . 84.01(11) ? Na1 O1 O2 . . 6_545 145.66(16) ? Na1 O1 O2 . . 7_555 84.26(11) ? Na1 O1 O2 . . 8_454 49.71(8) ? Na1 O1 O3 . . . 138.61(15) ? Na1 O1 O3 . . 4_555 115.94(12) ? Sc1 O1 Sc1 1_545 . 3_565 98.69(11) ? Sc1 O1 Si1 1_545 . . 122.57(16) ? Sc1 O1 O1 1_545 . 2_555 49.21(9) ? Sc1 O1 O1 1_545 . 3_555 48.22(8) ? Sc1 O1 O1 1_545 . 4_554 89.99(11) ? Sc1 O1 O1 1_545 . 4_555 44.04(8) ? Sc1 O1 O2 1_545 . . 144.65(13) ? Sc1 O1 O2 1_545 . 6_545 42.06(9) ? Sc1 O1 O2 1_545 . 7_555 141.48(12) ? Sc1 O1 O2 1_545 . 8_454 97.10(12) ? Sc1 O1 O3 1_545 . . 116.61(14) ? Sc1 O1 O3 1_545 . 4_555 89.34(12) ? Sc1 O1 Si1 3_565 . . 122.29(19) ? Sc1 O1 O1 3_565 . 2_555 96.64(12) ? Sc1 O1 O1 3_565 . 3_555 50.47(9) ? Sc1 O1 O1 3_565 . 4_554 45.97(8) ? Sc1 O1 O1 3_565 . 4_555 142.18(15) ? Sc1 O1 O2 3_565 . . 115.97(15) ? Sc1 O1 O2 3_565 . 6_545 100.60(12) ? Sc1 O1 O2 3_565 . 7_555 43.22(8) ? Sc1 O1 O2 3_565 . 8_454 40.76(8) ? Sc1 O1 O3 3_565 . . 91.40(13) ? Sc1 O1 O3 3_565 . 4_555 151.07(18) ? Si1 O1 O1 . . 2_555 140.44(16) ? Si1 O1 O1 . . 3_555 145.39(18) ? Si1 O1 O1 . . 4_554 91.96(15) ? Si1 O1 O1 . . 4_555 90.54(13) ? Si1 O1 O2 . . . 31.15(10) ? Si1 O1 O2 . . 6_545 88.65(14) ? Si1 O1 O2 . . 7_555 85.27(15) ? Si1 O1 O2 . . 8_454 140.31(17) ? Si1 O1 O3 . . . 36.48(10) ? Si1 O1 O3 . . 4_555 35.93(10) ? O1 O1 O1 2_555 . 3_555 65.00(11) ? O1 O1 O1 2_555 . 4_554 123.37(13) ? O1 O1 O1 2_555 . 4_555 56.63(10) ? O1 O1 O2 2_555 . . 127.40(14) ? O1 O1 O2 2_555 . 6_545 91.02(13) ? O1 O1 O2 2_555 . 7_555 125.64(13) ? O1 O1 O2 2_555 . 8_454 66.38(11) ? O1 O1 O3 2_555 . . 164.60(15) ? O1 O1 O3 2_555 . 4_555 109.37(14) ? O1 O1 O1 3_555 . 4_554 58.37(11) ? O1 O1 O1 3_555 . 4_555 92.01(12) ? O1 O1 O2 3_555 . . 165.20(16) ? O1 O1 O2 3_555 . 6_545 63.86(10) ? O1 O1 O2 3_555 . 7_555 93.48(11) ? O1 O1 O2 3_555 . 8_454 61.64(10) ? O1 O1 O3 3_555 . . 111.59(14) ? O1 O1 O3 3_555 . 4_555 130.63(14) ? O1 O1 O1 4_554 . 4_555 123.30(12) ? O1 O1 O2 4_554 . . 108.68(15) ? O1 O1 O2 4_554 . 6_545 65.00(10) ? O1 O1 O2 4_554 . 7_555 60.57(10) ? O1 O1 O2 4_554 . 8_454 86.48(10) ? O1 O1 O3 4_554 . . 55.48(10) ? O1 O1 O3 4_554 . 4_555 106.76(14) ? O1 O1 O2 4_555 . . 101.84(11) ? O1 O1 O2 4_555 . 6_545 58.45(10) ? O1 O1 O2 4_555 . 7_555 174.48(13) ? O1 O1 O2 4_555 . 8_454 123.01(14) ? O1 O1 O3 4_555 . . 109.78(13) ? O1 O1 O3 4_555 . 4_555 54.91(11) ? O2 O1 O2 . . 6_545 119.36(13) ? O2 O1 O2 . . 7_555 72.75(11) ? O2 O1 O2 . . 8_454 113.34(13) ? O2 O1 O3 . . . 58.86(12) ? O2 O1 O3 . . 4_555 57.03(11) ? O2 O1 O2 6_545 . 7_555 124.89(14) ? O2 O1 O2 6_545 . 8_454 125.50(12) ? O2 O1 O3 6_545 . . 74.55(12) ? O2 O1 O3 6_545 . 4_555 67.39(10) ? O2 O1 O2 7_555 . 8_454 59.62(10) ? O2 O1 O3 7_555 . . 68.62(12) ? O2 O1 O3 7_555 . 4_555 121.13(15) ? O2 O1 O3 8_454 . . 126.49(14) ? O2 O1 O3 8_454 . 4_555 165.33(14) ? O3 O1 O3 . . 4_555 60.44(12) ? Na1 O2 Sc1 7_556 . 5_545 93.41(11) ? Na1 O2 Si1 7_556 . . 97.44(15) ? Na1 O2 O1 7_556 . . 113.75(14) ? Na1 O2 O1 7_556 . 6_555 96.20(12) ? Na1 O2 O1 7_556 . 7_555 138.64(14) ? Na1 O2 O1 7_556 . 8_555 52.03(9) ? Na1 O2 O2 7_556 . 2_655 84.59(10) ? Na1 O2 O3 7_556 . . 109.65(14) ? Na1 O2 O3 7_556 . 7_555 140.13(14) ? Na1 O2 O3 7_556 . 4_555 59.51(10) ? Sc1 O2 Si1 5_545 . . 147.1(2) ? Sc1 O2 O1 5_545 . . 152.74(14) ? Sc1 O2 O1 5_545 . 6_555 46.18(9) ? Sc1 O2 O1 5_545 . 7_555 45.50(8) ? Sc1 O2 O1 5_545 . 8_555 42.83(8) ? Sc1 O2 O2 5_545 . 2_655 42.12(9) ? Sc1 O2 O3 5_545 . . 111.30(17) ? Sc1 O2 O3 5_545 . 7_555 79.17(11) ? Sc1 O2 O3 5_545 . 4_555 141.48(16) ? Si1 O2 O1 . . . 32.02(10) ? Si1 O2 O1 . . 6_555 159.62(18) ? Si1 O2 O1 . . 7_555 115.28(15) ? Si1 O2 O1 . . 8_555 144.90(16) ? Si1 O2 O2 . . 2_655 108.18(17) ? Si1 O2 O3 . . . 35.92(12) ? Si1 O2 O3 . . 7_555 109.97(14) ? Si1 O2 O3 . . 4_555 37.99(10) ? O1 O2 O1 . . 6_555 127.72(14) ? O1 O2 O1 . . 7_555 107.25(12) ? O1 O2 O1 . . 8_555 163.59(15) ? O1 O2 O2 . . 2_655 134.28(14) ? O1 O2 O3 . . . 58.76(12) ? O1 O2 O3 . . 7_555 81.05(11) ? O1 O2 O3 . . 4_555 59.97(11) ? O1 O2 O1 6_555 . 7_555 60.98(10) ? O1 O2 O1 6_555 . 8_555 54.50(9) ? O1 O2 O2 6_555 . 2_655 88.11(12) ? O1 O2 O3 6_555 . . 147.70(15) ? O1 O2 O3 6_555 . 7_555 50.96(9) ? O1 O2 O3 6_555 . 4_555 150.80(15) ? O1 O2 O1 7_555 . 8_555 88.02(12) ? O1 O2 O2 7_555 . 2_655 62.28(11) ? O1 O2 O3 7_555 . . 86.72(13) ? O1 O2 O3 7_555 . 7_555 51.09(10) ? O1 O2 O3 7_555 . 4_555 148.05(15) ? O1 O2 O2 8_555 . 2_655 58.10(10) ? O1 O2 O3 8_555 . . 130.03(15) ? O1 O2 O3 8_555 . 7_555 105.09(12) ? O1 O2 O3 8_555 . 4_555 109.71(12) ? O2 O2 O3 2_655 . . 75.81(13) ? O2 O2 O3 2_655 . 7_555 112.07(13) ? O2 O2 O3 2_655 . 4_555 104.01(14) ? O3 O2 O3 . . 7_555 109.52(12) ? O3 O2 O3 . . 4_555 61.44(12) ? O3 O2 O3 7_555 . 4_555 139.29(15) ? Na1 O3 Na1 5_545 . 7_555 111.84(13) ? Na1 O3 Si1 5_545 . . 103.61(14) ? Na1 O3 Si1 5_545 . 4_554 92.89(14) ? Na1 O3 O1 5_545 . . 118.70(14) ? Na1 O3 O1 5_545 . 4_554 113.86(13) ? Na1 O3 O2 5_545 . . 113.26(12) ? Na1 O3 O2 5_545 . 7_555 175.50(14) ? Na1 O3 O2 5_545 . 4_554 56.58(9) ? Na1 O3 O3 5_545 . 3_655 62.19(9) ? Na1 O3 O3 5_545 . 4_554 106.54(14) ? Na1 O3 O3 5_545 . 4_555 67.75(10) ? Na1 O3 Si1 7_555 . . 116.71(16) ? Na1 O3 Si1 7_555 . 4_554 88.76(14) ? Na1 O3 O1 7_555 . . 126.47(13) ? Na1 O3 O1 7_555 . 4_554 105.40(12) ? Na1 O3 O2 7_555 . . 82.93(12) ? Na1 O3 O2 7_555 . 7_555 70.62(9) ? Na1 O3 O2 7_555 . 4_554 103.26(14) ? Na1 O3 O3 7_555 . 3_655 49.65(9) ? Na1 O3 O3 7_555 . 4_554 52.88(10) ? Na1 O3 O3 7_555 . 4_555 132.62(13) ? Si1 O3 Si1 . . 4_554 140.4(2) ? Si1 O3 O1 . . . 35.94(10) ? Si1 O3 O1 . . 4_554 105.55(17) ? Si1 O3 O2 . . . 34.40(11) ? Si1 O3 O2 . . 7_555 78.04(13) ? Si1 O3 O2 . . 4_554 140.0(2) ? Si1 O3 O3 . . 3_655 128.42(15) ? Si1 O3 O3 . . 4_554 149.75(17) ? Si1 O3 O3 . . 4_555 35.92(10) ? Si1 O3 O1 4_554 . . 104.65(16) ? Si1 O3 O1 4_554 . 4_554 35.40(11) ? Si1 O3 O2 4_554 . . 153.81(17) ? Si1 O3 O2 4_554 . 7_555 83.32(12) ? Si1 O3 O2 4_554 . 4_554 36.36(10) ? Si1 O3 O3 4_554 . 3_655 91.19(16) ? Si1 O3 O3 4_554 . 4_554 35.92(11) ? Si1 O3 O3 4_554 . 4_555 137.99(19) ? O1 O3 O1 . . 4_554 69.61(12) ? O1 O3 O2 . . . 62.38(12) ? O1 O3 O2 . . 7_555 60.29(11) ? O1 O3 O2 . . 4_554 118.16(16) ? O1 O3 O3 . . 3_655 163.90(14) ? O1 O3 O3 . . 4_554 121.89(13) ? O1 O3 O3 . . 4_555 60.12(12) ? O1 O3 O2 4_554 . . 124.10(15) ? O1 O3 O2 4_554 . 7_555 61.65(10) ? O1 O3 O2 4_554 . 4_554 63.00(11) ? O1 O3 O3 4_554 . 3_655 125.82(15) ? O1 O3 O3 4_554 . 4_554 59.44(12) ? O1 O3 O3 4_554 . 4_555 118.07(16) ? O2 O3 O2 . . 7_555 70.48(11) ? O2 O3 O2 . . 4_554 169.41(15) ? O2 O3 O3 . . 3_655 101.95(13) ? O2 O3 O3 . . 4_554 129.15(15) ? O2 O3 O3 . . 4_555 58.04(11) ? O2 O3 O2 7_555 . 4_554 119.52(12) ? O2 O3 O3 7_555 . 3_655 120.15(14) ? O2 O3 O3 7_555 . 4_554 71.71(11) ? O2 O3 O3 7_555 . 4_555 113.65(15) ? O2 O3 O3 4_554 . 3_655 76.49(13) ? O2 O3 O3 4_554 . 4_554 60.52(12) ? O2 O3 O3 4_554 . 4_555 112.30(15) ? O3 O3 O3 3_655 . 4_554 70.04(12) ? O3 O3 O3 3_655 . 4_555 109.53(12) ? O3 O3 O3 4_554 . 4_555 172.81(16) ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag ? ? ? ? ? ? ? ? ? ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_D _geom_hbond_site_symmetry_H _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag ? ? ? ? ? ? ? ? ? ? ? #======================================================================= # 11. STRUCTURE-FACTOR LIST loop_ _refln_index_h _refln_index_k _refln_index_l _refln_F_squared_calc _refln_F_squared_meas _refln_F_squared_sigma _refln_observed_status 2 0 0 53.79 125.59 17.01 o 4 0 0 250.63 94.82 24.68 o 6 0 0 9908.76 11240.70 319.07 o 8 0 0 4527.19 4505.88 214.06 o 10 0 0 3022.97 3106.99 202.41 o 12 0 0 115.22 49.56 49.10 < 1 1 0 890.29 998.96 22.76 o 3 1 0 12017.50 14796.80 183.82 o 5 1 0 2216.48 2660.54 97.00 o 7 1 0 3491.25 3866.15 131.54 o 9 1 0 294.23 296.97 52.80 o 11 1 0 984.52 861.06 89.53 o 0 2 0 3790.98 3561.18 92.77 o 2 2 0 2214.57 2208.21 46.78 o 4 2 0 53.23 101.37 26.34 o 6 2 0 3.45 -5.96 26.27 < 8 2 0 107.71 187.26 39.64 o 10 2 0 222.84 239.60 45.33 o 12 2 0 95.05 124.86 73.98 < 1 3 0 200.50 219.88 14.95 o 3 3 0 1207.26 1241.14 47.18 o 5 3 0 33.20 63.32 32.82 < 7 3 0 417.71 548.88 61.60 o 9 3 0 140.82 215.78 42.41 o 11 3 0 4.71 35.60 42.28 < 0 4 0 543.28 372.67 37.85 o 2 4 0 583.09 633.38 34.41 o 4 4 0 8358.26 8079.03 156.36 o 6 4 0 7.78 32.09 37.05 < 8 4 0 8.63 45.19 29.97 < 10 4 0 3925.37 5229.25 267.33 o 1 5 0 10165.80 9985.58 169.06 o 3 5 0 4635.72 4061.22 102.83 o 5 5 0 20.42 63.19 42.94 < 7 5 0 12414.40 12518.40 305.04 o 9 5 0 224.03 318.08 65.04 o 0 6 0 11574.80 11676.90 266.27 o 2 6 0 477.58 515.00 46.52 o 4 6 0 480.81 487.80 47.24 o 6 6 0 76.16 31.96 42.15 < 8 6 0 287.82 361.29 69.08 o 10 6 0 2225.53 2126.69 174.29 o 1 7 0 58.05 70.07 16.74 o 3 7 0 26.46 -37.45 27.20 < 5 7 0 2294.28 2094.79 105.54 o 7 7 0 1711.95 1765.54 140.61 o 9 7 0 218.41 249.52 66.24 o 0 8 0 45.04 16.48 24.75 < 2 8 0 11.53 40.83 17.87 < 4 8 0 373.56 371.21 47.18 o 6 8 0 412.50 373.73 71.26 o 8 8 0 120.59 72.12 42.35 < 1 9 0 152.33 190.90 28.25 o 3 9 0 2029.16 1943.53 111.69 o 5 9 0 307.65 278.77 63.85 o 7 9 0 300.59 305.57 67.10 o 0 10 0 4061.22 4653.24 340.64 o 2 10 0 209.04 226.63 43.14 o 4 10 0 2071.77 2306.74 131.61 o 6 10 0 896.76 700.14 96.87 o 1 11 0 37.08 56.11 40.03 < 3 11 0 1012.41 1152.08 120.89 o 5 11 0 413.39 481.91 80.46 o 0 12 0 2084.65 2255.79 268.58 o -11 1 1 2.78 -18.33 30.17 < -9 1 1 211.47 237.68 49.03 o -7 1 1 67.71 3.51 31.17 < -5 1 1 2180.31 2449.86 101.90 o -3 1 1 2373.22 2626.33 47.05 o -1 1 1 1363.52 1424.37 27.79 o 1 1 1 1170.57 1138.98 28.39 o 3 1 1 2285.84 2287.68 51.88 o 5 1 1 1087.12 1143.81 60.41 o 7 1 1 5.64 30.04 26.93 < 9 1 1 398.27 381.00 48.70 o 11 1 1 100.79 97.34 50.82 < -12 2 1 4457.44 4263.57 212.07 o -10 2 1 47.22 23.09 37.45 < -8 2 1 2326.95 2634.94 133.33 o -6 2 1 2371.80 2567.64 144.65 o -4 2 1 5746.55 6067.22 112.49 o -2 2 1 27162.70 26012.60 209.29 o 0 2 1 580.62 568.46 21.44 o 2 2 1 14466.50 13860.00 150.67 o 4 2 1 2728.37 2893.20 96.34 o 6 2 1 4896.38 4790.48 153.98 o 8 2 1 2660.75 2569.69 130.15 o 10 2 1 20.81 5.23 49.56 < -11 3 1 1322.63 1317.57 110.70 o -9 3 1 4379.93 5202.78 204.13 o -7 3 1 1876.43 1923.15 96.01 o -5 3 1 14472.00 13960.60 287.84 o -3 3 1 8946.18 9193.00 126.12 o -1 3 1 6862.94 6393.30 91.38 o 1 3 1 21.88 20.64 12.70 < 3 3 1 1616.33 1733.71 57.04 o 5 3 1 23060.50 22589.30 286.25 o 7 3 1 383.98 368.37 46.72 o 9 3 1 1874.75 2127.95 160.00 o 11 3 1 547.64 550.99 124.73 o -10 4 1 295.11 448.56 68.09 o -8 4 1 25.35 51.55 31.03 < -6 4 1 6.08 44.66 26.47 < -4 4 1 26.18 25.94 13.37 < -2 4 1 3018.96 2776.01 68.22 o 0 4 1 6567.84 6461.65 99.98 o 2 4 1 1129.98 1062.62 39.04 o 4 4 1 207.35 205.19 25.14 o 6 4 1 279.50 281.82 40.43 o 8 4 1 226.64 346.86 68.35 o 10 4 1 729.91 903.61 114.01 o -11 5 1 95.90 78.48 48.77 < -9 5 1 3.19 -6.35 31.23 < -7 5 1 79.08 93.17 31.96 < -5 5 1 324.50 251.11 37.05 o -3 5 1 714.09 628.54 40.83 o -1 5 1 383.57 407.41 31.70 o 1 5 1 26.61 35.60 13.43 < 3 5 1 1101.67 951.25 41.22 o 5 5 1 495.85 488.20 48.44 o 7 5 1 15.07 -18.53 32.89 < 9 5 1 6.22 2.25 36.19 < -10 6 1 9.14 34.54 35.67 < -8 6 1 431.80 352.88 66.96 o -6 6 1 86.86 74.97 26.47 < -4 6 1 19.81 12.31 13.96 < -2 6 1 430.17 432.22 29.58 o 0 6 1 22.56 16.48 16.01 < 2 6 1 142.82 114.08 21.97 o 4 6 1 14.71 35.86 34.61 < 6 6 1 95.19 175.68 52.01 o 8 6 1 96.94 143.46 53.99 < -9 7 1 1290.71 1255.90 130.02 o -7 7 1 290.18 315.23 48.70 o -5 7 1 6427.19 5723.53 181.11 o -3 7 1 124.82 132.27 23.49 o -1 7 1 3453.31 3563.49 90.26 o 1 7 1 5358.17 5519.13 160.86 o 3 7 1 271.96 178.59 44.80 o 5 7 1 3236.56 2849.92 170.19 o 7 7 1 566.37 421.30 76.62 o -8 8 1 1346.49 1387.64 132.67 o -6 8 1 470.12 528.56 60.61 o -4 8 1 467.05 415.08 42.94 o -2 8 1 7422.65 7660.18 181.44 o 0 8 1 337.05 346.00 33.28 o 2 8 1 3211.25 3315.75 178.46 o 4 8 1 570.79 601.75 80.46 o 6 8 1 1677.00 1786.71 145.37 o -7 9 1 2283.25 2343.72 138.96 o -5 9 1 1941.56 1866.64 114.74 o -3 9 1 2.13 18.00 18.00 < -1 9 1 0.90 7.87 18.92 < 1 9 1 146.16 191.76 41.36 o 3 9 1 171.67 232.19 56.38 o 5 9 1 2028.22 1760.84 147.03 o -6 10 1 52.65 81.65 34.41 < -4 10 1 74.61 115.86 34.41 o -2 10 1 817.20 962.63 71.93 o 0 10 1 1077.45 1187.68 95.35 o 2 10 1 39.31 7.87 35.53 < 4 10 1 30.31 60.68 40.76 < -5 11 1 9.69 -19.78 28.45 < -3 11 1 326.21 398.41 105.61 o -1 11 1 119.51 83.04 31.63 < 1 11 1 10.49 47.71 32.42 < 3 11 1 321.88 286.85 83.11 o -12 0 2 168.54 146.37 83.97 < -10 0 2 4248.73 4744.62 345.21 o -8 0 2 1263.11 1318.96 164.10 o -6 0 2 9098.84 9449.80 264.61 o -4 0 2 11274.10 10729.80 205.79 o -2 0 2 589.46 668.58 31.10 o 0 0 2 29439.30 27986.40 302.13 o 2 0 2 7017.61 7090.00 154.64 o 4 0 2 10602.70 10147.10 266.80 o 6 0 2 149.94 189.97 48.90 o 8 0 2 1100.39 1000.48 101.44 o 10 0 2 6728.54 5621.37 408.33 o -11 1 2 91.76 74.57 41.49 < -9 1 2 335.40 315.63 52.27 o -7 1 2 12284.90 12669.00 246.08 o -5 1 2 43.61 30.04 15.22 < -3 1 2 104.14 63.26 10.72 o -1 1 2 285.94 293.53 16.94 o 1 1 2 6934.61 7466.50 84.30 o 3 1 2 2908.31 2772.70 68.88 o 5 1 2 1379.57 1376.52 66.77 o 7 1 2 4309.60 4015.63 135.51 o 9 1 2 30.21 12.57 30.24 < -12 2 2 644.03 566.94 92.11 o -10 2 2 1424.63 1615.86 119.04 o -8 2 2 101.18 62.46 25.48 < -6 2 2 1415.93 1401.80 58.69 o -4 2 2 1302.75 1329.61 44.86 o -2 2 2 14.60 -5.82 9.59 < 0 2 2 1511.15 1792.80 37.32 o 2 2 2 926.11 908.31 40.56 o 4 2 2 2926.66 2901.07 86.62 o 6 2 2 730.31 645.22 57.17 o 8 2 2 878.41 766.77 91.25 o 10 2 2 957.39 677.58 98.53 o -11 3 2 99.81 60.21 36.13 < -9 3 2 134.98 100.97 36.79 < -7 3 2 249.76 237.48 31.56 o -5 3 2 187.50 145.18 25.94 o -3 3 2 1316.48 1416.95 36.99 o -1 3 2 425.17 453.20 25.14 o 1 3 2 1180.98 1170.08 50.29 o 3 3 2 420.35 411.38 40.76 o 5 3 2 1.96 11.05 18.06 < 7 3 2 141.56 187.92 52.80 o 9 3 2 8.17 21.84 30.37 < -12 4 2 0.49 -39.37 38.84 < -10 4 2 1322.92 1347.74 107.66 o -8 4 2 236.76 239.14 43.01 o -6 4 2 1389.95 1298.38 69.81 o -4 4 2 1403.07 1360.38 52.74 o -2 4 2 12.41 29.84 12.31 < 0 4 2 6820.54 6853.38 161.32 o 2 4 2 24.00 -1.79 18.59 < 4 4 2 2168.93 2121.26 131.94 o 6 4 2 805.70 703.78 83.44 o 8 4 2 32.69 96.08 44.73 < 10 4 2 833.19 857.03 160.46 o -11 5 2 944.11 1067.78 102.30 o -9 5 2 427.51 408.60 71.00 o -7 5 2 7523.27 7333.44 188.78 o -5 5 2 104.00 120.36 21.04 o -3 5 2 11007.80 10121.90 157.42 o -1 5 2 850.24 833.67 37.52 o 1 5 2 3381.45 3608.09 117.98 o 3 5 2 13401.00 12008.40 345.87 o 5 5 2 1.58 21.64 30.04 < 7 5 2 3069.74 2915.83 186.40 o 9 5 2 439.12 347.32 73.51 o -10 6 2 207.07 279.23 52.80 o -8 6 2 40.60 5.43 24.09 < -6 6 2 4154.09 4037.33 131.28 o -4 6 2 150.38 187.26 23.95 o -2 6 2 4776.44 4534.27 119.83 o 0 6 2 12510.70 12763.70 274.34 o 2 6 2 3.21 -43.74 35.93 < 4 6 2 166.52 175.75 50.02 o 6 6 2 15.14 -25.87 40.69 < 8 6 2 269.57 304.91 67.69 o -9 7 2 102.64 130.55 42.08 o -7 7 2 688.62 696.37 59.75 o -5 7 2 1126.39 1088.49 55.05 o -3 7 2 566.84 604.66 44.80 o -1 7 2 999.14 1012.66 50.82 o 1 7 2 111.24 104.68 42.94 < 3 7 2 1379.62 1170.80 109.38 o 5 7 2 1257.15 1113.50 112.75 o 7 7 2 16.31 47.44 44.53 < -8 8 2 19.87 25.28 25.01 < -6 8 2 9.87 6.29 22.10 < -4 8 2 8.62 9.79 17.80 < -2 8 2 228.82 266.13 33.61 o 0 8 2 256.72 340.31 47.44 o 2 8 2 116.17 140.15 42.88 o 4 8 2 36.02 96.21 42.94 < 6 8 2 7.94 81.79 43.54 < -7 9 2 986.77 798.47 78.34 o -5 9 2 201.26 208.70 33.61 o -3 9 2 596.33 596.25 51.48 o -1 9 2 726.16 805.02 75.83 o 1 9 2 632.61 719.46 73.25 o 3 9 2 325.54 280.10 63.85 o 5 9 2 219.49 224.98 61.27 o -6 10 2 288.70 342.30 69.81 o -4 10 2 2527.80 2622.10 133.73 o -2 10 2 603.53 727.73 94.36 o 0 10 2 1800.12 1973.18 154.97 o 2 10 2 127.71 74.11 38.91 < 4 10 2 3346.70 2926.74 269.31 o -5 11 2 104.50 124.53 70.60 < -3 11 2 270.14 387.75 99.39 o -1 11 2 1.89 34.94 55.71 < 1 11 2 357.58 351.76 99.45 o -11 1 3 86.52 53.53 27.26 < -9 1 3 215.35 278.04 39.30 o -7 1 3 172.56 181.83 28.85 o -5 1 3 2141.41 2087.78 71.33 o -3 1 3 1300.76 1236.71 51.94 o -1 1 3 263.86 260.18 21.57 o 1 1 3 967.27 955.82 32.95 o 3 1 3 508.59 458.89 29.05 o 5 1 3 110.77 163.04 35.40 o 7 1 3 17.74 16.61 25.74 < 9 1 3 840.84 520.03 89.33 o -12 2 3 2848.95 3237.54 224.45 o -10 2 3 161.83 204.93 51.55 o -8 2 3 4276.23 4315.77 135.78 o -6 2 3 537.55 559.60 54.72 o -4 2 3 807.17 725.88 38.97 o -2 2 3 17644.60 16737.50 225.44 o 0 2 3 281.59 318.67 26.27 o 2 2 3 6229.92 6229.73 105.94 o 4 2 3 146.18 147.62 25.74 o 6 2 3 3245.57 3373.79 143.39 o 8 2 3 2343.79 2083.41 159.93 o -11 3 3 1142.23 1178.15 109.44 o -9 3 3 6384.92 6417.12 216.18 o -7 3 3 812.97 738.98 56.18 o -5 3 3 4662.19 4337.54 103.22 o -3 3 3 1751.19 1684.08 78.54 o -1 3 3 11505.10 11577.70 171.31 o 1 3 3 867.82 846.24 43.80 o 3 3 3 20.45 80.26 23.95 o 5 3 3 9012.83 8706.45 235.37 o 7 3 3 27.42 99.85 49.89 < -12 4 3 878.97 603.80 139.22 o -10 4 3 80.34 57.10 31.70 < -8 4 3 845.57 821.69 64.65 o -6 4 3 277.08 270.04 35.47 o -4 4 3 501.66 476.02 27.00 o -2 4 3 3704.13 3600.88 112.95 o 0 4 3 1084.09 1048.39 63.72 o 2 4 3 337.96 376.17 59.82 o 4 4 3 809.68 745.60 88.47 o 6 4 3 358.90 368.89 66.77 o 8 4 3 319.55 266.86 67.43 o -11 5 3 6.73 -65.18 46.85 < -9 5 3 0.00 22.96 25.67 < -7 5 3 279.89 254.42 35.93 o -5 5 3 604.51 585.34 39.77 o -3 5 3 686.70 654.09 39.44 o -1 5 3 15.54 13.23 13.70 < 1 5 3 379.67 467.02 68.09 o 3 5 3 318.70 229.87 50.22 o 5 5 3 9.80 13.96 37.19 < 7 5 3 3.71 -66.43 44.60 < -10 6 3 22.57 76.29 48.97 < -8 6 3 84.17 66.63 29.71 < -6 6 3 210.28 193.61 26.73 o -4 6 3 130.38 138.62 21.64 o -2 6 3 32.91 15.81 22.17 < 0 6 3 3.57 -5.16 19.52 < 2 6 3 533.14 505.67 74.90 o 4 6 3 4.03 73.71 41.82 < 6 6 3 12.46 21.17 48.44 < -9 7 3 1310.08 1185.43 100.64 o -7 7 3 274.61 208.17 42.94 o -5 7 3 3959.41 3775.57 125.79 o -3 7 3 91.32 134.39 31.63 o -1 7 3 3071.01 3289.02 188.52 o 1 7 3 2637.08 2694.56 170.19 o 3 7 3 239.60 122.88 45.59 < 5 7 3 2253.60 2345.45 176.28 o -8 8 3 1286.93 1166.17 96.14 o -6 8 3 204.15 217.70 41.42 o -4 8 3 305.14 274.27 35.00 o -2 8 3 4398.69 4941.87 247.94 o 0 8 3 12.16 -44.07 40.96 < 2 8 3 3068.46 3122.08 194.27 o 4 8 3 3.11 -8.87 33.55 < -7 9 3 924.65 825.07 98.53 o -5 9 3 140.96 145.64 33.28 o -3 9 3 65.96 82.31 41.49 < -1 9 3 1139.42 1244.52 127.04 o 1 9 3 162.87 180.11 55.91 o 3 9 3 822.33 870.39 105.94 o -6 10 3 104.30 40.36 43.67 < -4 10 3 67.48 108.98 42.35 < -2 10 3 312.89 480.06 86.02 o 0 10 3 356.59 498.85 86.81 o -3 11 3 311.82 286.91 87.28 o -10 0 4 1313.16 1330.74 123.67 o -8 0 4 33.08 34.74 30.11 < -6 0 4 10658.00 9647.98 436.65 o -4 0 4 7384.10 6765.50 207.31 o -2 0 4 1011.17 1024.04 59.29 o 0 0 4 12597.70 12902.80 256.21 o 2 0 4 1218.65 1223.67 71.13 o 4 0 4 4575.98 4492.65 160.59 o 6 0 4 676.91 515.00 73.58 o 8 0 4 690.78 658.72 131.54 o -11 1 4 456.18 511.16 70.80 o -9 1 4 0.84 -40.83 25.41 < -7 1 4 2032.92 2023.33 109.05 o -5 1 4 64.85 84.37 23.82 o -3 1 4 7307.04 6904.59 123.34 o -1 1 4 328.78 284.53 23.09 o 1 1 4 9.62 -17.20 15.02 < 3 1 4 4821.25 4717.56 119.83 o 5 1 4 0.87 26.47 26.47 < 7 1 4 584.33 552.65 68.15 o -12 2 4 66.68 64.91 53.20 < -10 2 4 47.18 49.49 26.80 < -8 2 4 72.08 108.65 35.73 o -6 2 4 126.37 110.57 39.04 < -4 2 4 5.40 10.98 14.89 < -2 2 4 472.76 459.35 39.44 o 0 2 4 641.86 619.41 36.46 o 2 2 4 1240.85 1244.12 64.58 o 4 2 4 77.03 50.62 25.14 < 6 2 4 82.27 12.90 30.90 < 8 2 4 115.87 70.60 45.79 < -11 3 4 5.19 50.22 35.14 < -9 3 4 63.56 124.07 38.84 o -7 3 4 270.96 272.29 44.14 o -5 3 4 1.37 0.26 26.80 < -3 3 4 289.86 247.01 29.97 o -1 3 4 9.54 19.85 16.54 < 1 3 4 146.16 83.90 34.14 < 3 3 4 169.82 197.52 37.32 o 5 3 4 68.49 58.63 32.69 < 7 3 4 212.22 207.64 58.76 o -10 4 4 2378.62 2277.16 140.61 o -8 4 4 185.54 190.30 40.63 o -6 4 4 21.61 3.84 22.37 < -4 4 4 1968.16 1892.91 96.28 o -2 4 4 796.76 829.30 56.05 o 0 4 4 828.83 1062.55 97.86 o 2 4 4 168.80 255.35 53.07 o 4 4 4 3491.88 3516.78 204.40 o 6 4 4 267.38 283.21 69.21 o -9 5 4 44.54 51.55 34.47 < -7 5 4 6222.88 6067.75 207.77 o -5 5 4 515.52 462.59 51.55 o -3 5 4 4032.90 4247.36 150.07 o -1 5 4 366.87 396.36 66.17 o 1 5 4 2576.99 2736.44 169.26 o 3 5 4 3868.18 4177.94 223.26 o 5 5 4 58.73 -6.22 46.58 < -10 6 4 1109.41 1047.27 168.20 o -8 6 4 298.99 304.31 51.08 o -6 6 4 892.29 846.77 62.07 o -4 6 4 2687.66 2590.74 121.09 o -2 6 4 797.78 918.76 81.59 o 0 6 4 967.71 1120.65 114.41 o 2 6 4 7.03 -42.35 39.04 < 4 6 4 2657.69 2696.67 188.38 o -9 7 4 758.73 638.60 130.35 o -7 7 4 832.33 721.18 72.85 o -5 7 4 162.87 153.98 33.48 o -3 7 4 120.64 133.13 38.58 o -1 7 4 501.29 473.58 79.67 o 1 7 4 0.03 0.53 41.82 < 3 7 4 157.65 170.59 51.28 o -8 8 4 56.95 16.01 42.41 < -6 8 4 217.85 152.72 42.94 o -4 8 4 60.21 23.62 34.87 < -2 8 4 10.08 21.70 39.44 < 0 8 4 77.39 51.35 43.27 < 2 8 4 320.15 359.37 72.32 o -5 9 4 35.13 57.04 57.96 < -3 9 4 1142.20 1348.53 114.87 o -1 9 4 350.00 377.03 80.99 o -9 1 5 207.64 204.46 50.42 o -7 1 5 55.69 54.39 29.31 < -5 1 5 1359.17 1354.56 110.17 o -3 1 5 442.04 464.44 41.49 o -1 1 5 58.91 77.15 20.25 o 1 1 5 347.33 306.30 37.72 o 3 1 5 0.64 -19.19 21.51 < 5 1 5 46.34 64.58 35.47 < -10 2 5 18.66 -4.57 36.99 < -8 2 5 3493.19 3422.29 204.13 o -6 2 5 642.64 699.54 86.35 o -4 2 5 162.29 192.62 27.46 o -2 2 5 4218.60 4281.23 130.42 o 0 2 5 199.72 172.30 32.03 o 2 2 5 4947.83 5332.01 166.28 o 4 2 5 1.12 -1.06 31.03 < -9 3 5 4065.01 4096.56 231.59 o -7 3 5 61.88 61.14 30.77 < -5 3 5 1960.12 2038.55 111.63 o -3 3 5 56.10 46.85 18.59 < -1 3 5 6022.74 6499.44 207.38 o 1 3 5 1396.44 1395.71 96.28 o 3 3 5 13.64 85.29 36.53 < 5 3 5 2816.68 2760.79 194.93 o -10 4 5 100.36 147.89 67.23 < -8 4 5 924.40 911.88 104.35 o -6 4 5 0.45 51.55 29.64 < -4 4 5 213.04 234.84 37.65 o -2 4 5 534.98 569.79 63.26 o 0 4 5 246.68 301.67 49.23 o 2 4 5 1244.29 1365.21 124.80 o 4 4 5 592.46 536.17 87.15 o -9 5 5 7.06 -52.01 50.69 < -7 5 5 55.86 8.07 30.37 < -5 5 5 207.83 208.70 51.35 o -3 5 5 436.02 426.46 59.82 o -1 5 5 6.74 -15.75 29.05 < 1 5 5 94.41 13.56 27.86 < 3 5 5 22.07 9.59 44.07 < -8 6 5 189.85 147.96 60.55 < -6 6 5 77.99 76.82 36.59 < -4 6 5 40.47 52.47 32.22 < -2 6 5 231.05 195.40 42.35 o 0 6 5 2.54 -36.66 35.20 < 2 6 5 81.37 96.21 50.35 < -5 7 5 3246.40 3370.68 198.91 o -3 7 5 71.66 94.42 36.06 < -1 7 5 789.81 831.55 86.81 o 1 7 5 1592.08 1758.06 230.93 o -4 8 5 5.35 1.72 38.64 < -2 8 5 2199.22 2789.05 208.10 o -8 0 6 64.73 70.07 48.90 < -6 0 6 653.06 614.58 119.11 o -4 0 6 4728.67 4516.47 305.31 o -2 0 6 442.54 645.02 87.67 o 0 0 6 1751.17 2193.78 223.26 o 2 0 6 3.25 -42.02 40.03 < -9 1 6 91.97 72.19 48.24 < -7 1 6 1405.73 1520.18 114.08 o -5 1 6 4.75 16.94 38.18 < -3 1 6 1728.60 1889.93 114.67 o -1 1 6 9.78 18.13 35.73 < 1 1 6 269.97 270.43 45.33 o 3 1 6 372.67 371.54 96.81 o -8 2 6 0.03 25.54 39.11 < -6 2 6 172.72 178.46 38.44 o -4 2 6 19.93 127.71 52.01 < -2 2 6 87.83 141.21 46.12 o 0 2 6 33.07 73.05 34.54 < 2 2 6 857.20 951.39 90.52 o -9 3 6 134.35 75.70 57.57 < -7 3 6 0.17 22.89 31.63 < -5 3 6 47.72 145.04 48.04 o -3 3 6 181.21 239.34 56.05 o -1 3 6 0.31 16.87 40.43 < 1 3 6 69.18 49.36 46.78 < 3 3 6 57.65 65.84 49.83 < -6 4 6 710.90 593.01 124.80 o -4 4 6 239.15 328.20 65.38 o -2 4 6 40.54 62.66 36.19 < 0 4 6 2099.89 2122.72 166.95 o -5 5 6 0.58 4.76 35.00 < -3 5 6 5056.16 5130.59 257.99 o -1 5 6 245.82 320.59 94.89 o -6 6 6 638.53 599.23 131.15 o -4 6 6 1106.81 1092.53 164.50 o -5 1 7 874.84 666.59 127.71 o -3 1 7 26.25 113.28 65.84 < -4 2 7 205.65 120.43 56.31 < -2 2 7 1091.96 977.12 152.26 o loop_ _twin_refln_datum_id _twin_refln_individual_id _twin_refln_index_h _twin_refln_index_k _twin_refln_index_l _twin_refln_F_squared_calc _twin_refln_F_squared_meas _twin_refln_F_squared_sigma _twin_refln_include_status ? ? ? ? ? ? ? ? ?