# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 #TrackingRef '- KErF4_AP_final.cif' #======================================================================= _audit_creation_method 'Jana2006 Version : 19/04/2012' # 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_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 'Andrzej Grzechnik' _publ_contact_author_address ; ? ; _publ_contact_author_email grzechnik@xtal.rwth-aachen.de _publ_contact_author_fax ? _publ_contact_author_phone ? _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 A.Grzechnik ; ? # footnote ; ; ? # address ; N.Khaidukov '' '' K.Friese '' '' #======================================================================= # 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. (2006). Jana2006. Structure Determination Software Programs. Institute of Physics, Praha, Czech Republic. 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 # 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 _database_code_depnum_ccdc_archive 'CCDC 891236' #TrackingRef '- KErF4_AP_final.cif' #======================================================================= # 5. CHEMICAL DATA _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_iupac ? _chemical_formula_sum 'Er1 F4 K1' _chemical_formula_weight 423.5 _chemical_melting_point ? _chemical_compound_source ? _chemical_absolute_configuration ? #======================================================================= # 6. CRYSTAL DATA _symmetry_cell_setting trigonal _symmetry_space_group_name_H-M 'P 31' _symmetry_space_group_name_Hall 'P 31' _symmetry_Int_Tables_number 144 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 -y,x-y,z+1/3 3 -x+y,-x,z+2/3 _cell_length_a 14.128(2) _cell_length_b 14.128(2) _cell_length_c 10.1580(10) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 120 _cell_volume 1755.9(4) loop_ _jana_cell_twin_matrix_id _jana_cell_twin_volume_fraction _jana_cell_twin_matrix_1_1 _jana_cell_twin_matrix_1_2 _jana_cell_twin_matrix_1_3 _jana_cell_twin_matrix_2_1 _jana_cell_twin_matrix_2_2 _jana_cell_twin_matrix_2_3 _jana_cell_twin_matrix_3_1 _jana_cell_twin_matrix_3_2 _jana_cell_twin_matrix_3_3 1 0.5117(11) 1 0 0 0 1 0 0 0 1 2 0 -1 0 0 0 -1 0 0 0 -1 3 0 1 -1 0 0 -1 0 0 0 -1 4 0.4883(11) -1 1 0 0 1 0 0 0 -1 _cell_formula_units_Z 18 _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _cell_measurement_temperature 293 _cell_special_details ; ? ; _exptl_crystal_density_diffrn 4.8047 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_F_000 2214 _exptl_absorpt_coefficient_mu 4.832 _exptl_crystal_description ? _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.06 _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 ? #======================================================================= # 7. EXPERIMENTAL DATA _exptl_special_details ? _diffrn_ambient_temperature 293 _diffrn_source ? _diffrn_source_power ? _diffrn_source_voltage ? _diffrn_source_current ? _diffrn_radiation_type ? _diffrn_radiation_source ? _diffrn_radiation_wavelength 0.4 _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 113899 _diffrn_reflns_theta_min 0.94 _diffrn_reflns_theta_max 25.81 _diffrn_reflns_theta_full 25.81 _diffrn_measured_fraction_theta_max 0 _diffrn_measured_fraction_theta_full 1 _diffrn_reflns_av_R_equivalents 0.0692 _diffrn_reflns_av_sigmaI/netI 0.0578 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _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 24932 _reflns_number_gt 21805 _reflns_threshold_expression I>3\s(I) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0312 _refine_ls_wR_factor_gt 0.0750 _refine_ls_R_factor_all 0.0386 _refine_ls_wR_factor_ref 0.0780 _refine_ls_goodness_of_fit_ref 1.05 _refine_ls_goodness_of_fit_gt 1.08 _refine_ls_restrained_S_gt ? _refine_ls_restrained_S_all ? _refine_ls_number_reflns 24932 _refine_ls_number_parameters 229 _refine_ls_number_restraints 0 _refine_ls_number_constraints 1 _refine_ls_weighting_scheme sigma _refine_ls_weighting_details w=1/(\s^2^(I)+0.0004I^2^) _refine_ls_hydrogen_treatment ? _refine_ls_shift/su_max 0.0423 _refine_ls_shift/su_mean 0.0043 _refine_diff_density_max 0.97 _refine_diff_density_min -1.22 _refine_ls_extinction_method 'B-C type 1 Gaussian isotropic (Becker & Coppens, 1974)' _refine_ls_extinction_coef 2930(170) _refine_ls_abs_structure_details ; 24265 of Friedel pairs used in the refinement ; _refine_ls_abs_structure_Flack 0 _refine_ls_abs_structure_Rogers ? loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Er -0.6733 1.8684 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' F 0.0032 0.0029 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' K 0.0760 0.0798 '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 ? #======================================================================= # 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_symmetry_multiplicity _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Er1 Er 0.12924(4) 0.88850(5) 0.33061(6) Uani 0.00773(10) 3 1 d . . . Er2 Er 0.28257(4) 0.73204(5) 0.32051(6) Uani 0.00657(9) 3 1 d . . . Er3 Er 0.77948(5) 0.20594(5) 0.33866(5) Uani 0.00651(9) 3 1 d . . . Er4 Er 0.94245(6) 0.05903(6) 0.32607(9) Uani 0.00784(10) 3 1 d . . . Er5 Er 0.45238(7) 0.54450(7) 0.32453(6) Uani 0.00737(9) 3 1 d . . . Er6 Er 0.60496(4) 0.38766(4) 0.34247(4) Uani 0.00627(10) 3 1 d . . . K1 K 0.7818(2) 0.7210(2) 0.3192(2) Uani 0.0168(7) 3 1 d . . . K2 K 0.2670(2) 0.2202(2) 0.3480(3) Uani 0.0188(7) 3 1 d . . . K3 K 0.1042(2) 0.3948(2) 0.3134(3) Uani 0.0168(6) 3 1 d . . . K4 K 0.6111(3) 0.8773(2) 0.3460(3) Uani 0.0213(8) 3 1 d . . . K5 K 0.9493(3) 0.5620(2) 0.3450(3) Uani 0.0223(8) 3 1 d . . . K6 K 0.4543(2) 0.06467(16) 0.3149(2) Uani 0.0161(6) 3 1 d . . . F1 F 0.1313(4) 0.9347(4) 0.1132(5) Uani 0.0153(10) 3 1 d . . . F2 F 0.0689(5) 0.8763(5) 0.5408(5) Uani 0.0184(12) 3 1 d . . . F3 F 0.2094(4) 0.5943(4) 0.4685(5) Uani 0.0234(9) 3 1 d . . . F4 F 0.3359(6) 0.7290(3) 0.6540(8) Uani 0.0341(6) 3 1 d . . . F5 F 0.7363(5) 0.2032(5) 0.5553(6) Uani 0.0184(12) 3 1 d . . . F6 F 0.7880(4) 0.2676(4) 0.1295(5) Uani 0.0153(10) 3 1 d . . . F7 F 0.0004(5) 0.0602(3) 0.6622(7) Uani 0.0341(6) 3 1 d . . . F8 F -0.1241(4) -0.0762(4) 0.4772(5) Uani 0.0234(9) 3 1 d . . . F9 F 0.3907(4) 0.5368(5) 0.5339(5) Uani 0.0184(12) 3 1 d . . . F10 F 0.4571(5) 0.5899(4) 0.1081(5) Uani 0.0153(10) 3 1 d . . . F11 F 0.5466(5) 0.2887(4) 0.5306(5) Uani 0.0234(9) 3 1 d . . . F12 F -0.2666(6) -0.6056(4) 0.6751(7) Uani 0.0341(6) 3 1 d . . . F13 F 0.7678(5) 0.7290(4) 0.0628(6) Uani 0.0183(9) 3 1 d . . . F14 F 0.8088(5) 0.7239(3) 0.5720(6) Uani 0.0165(10) 3 1 d . . . F15 F 0.2484(4) 0.2237(4) 0.6052(5) Uani 0.0171(9) 3 1 d . . . F16 F 0.8082(5) 0.0743(5) 0.4283(6) Uani 0.0154(10) 3 1 d . . . F17 F 0.1319(4) 0.3933(4) 0.5656(6) Uani 0.0165(10) 3 1 d . . . F18 F 0.0922(4) 0.4018(4) 0.0584(5) Uani 0.0183(9) 3 1 d . . . F19 F 0.1535(4) 0.7551(4) 0.4228(5) Uani 0.0154(10) 3 1 d . . . F20 F 0.5883(4) 0.8836(4) 0.6029(5) Uani 0.0171(9) 3 1 d . . . F21 F 0.9365(4) 0.5741(4) 0.5987(5) Uani 0.0171(9) 3 1 d . . . F22 F -0.5311(5) 0.4112(4) 0.4238(5) Uani 0.0154(10) 3 1 d . . . F23 F 0.4842(4) 0.0682(4) 0.5660(5) Uani 0.0165(10) 3 1 d . . . F24 F 0.4519(5) 0.0857(4) 0.0570(6) Uani 0.0183(9) 3 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 Er1 Er 0.00787(11) 0.00947(12) 0.00863(14) 0.00642(10) -0.00118(10) -0.00091(10) Er2 Er 0.00541(11) 0.00537(11) 0.00965(16) 0.00324(8) -0.00133(11) -0.00111(9) Er3 Er 0.00696(11) 0.00674(11) 0.00708(13) 0.00436(9) 0.00149(8) 0.00163(9) Er4 Er 0.00696(12) 0.00709(13) 0.01086(13) 0.00456(11) -0.00212(12) -0.00208(11) Er5 Er 0.00794(10) 0.00881(11) 0.00799(12) 0.00615(9) -0.00090(10) -0.00020(10) Er6 Er 0.00605(12) 0.00683(12) 0.00795(11) 0.00473(13) -0.00041(10) -0.00035(10) K1 K 0.0146(7) 0.0223(11) 0.0099(7) 0.0067(7) 0.0023(6) 0.0074(6) K2 K 0.0323(10) 0.0172(8) 0.0083(6) 0.0134(8) 0.0024(7) 0.0022(6) K3 K 0.0182(8) 0.0184(7) 0.0132(7) 0.0087(7) -0.0038(6) -0.0010(7) K4 K 0.0411(14) 0.0126(7) 0.0148(7) 0.0170(9) -0.0027(9) 0.0024(5) K5 K 0.0382(14) 0.0132(7) 0.0163(7) 0.0136(7) 0.0055(8) 0.0042(6) K6 K 0.0158(8) 0.0096(5) 0.0180(8) 0.0026(5) -0.0018(5) 0.0062(5) F1 F 0.0174(13) 0.0193(12) 0.0120(11) 0.0113(11) -0.0001(9) 0.0044(9) F2 F 0.0203(13) 0.0277(18) 0.0131(12) 0.0165(13) 0.0104(10) 0.0027(11) F3 F 0.0252(8) 0.0208(12) 0.0240(7) 0.0113(12) -0.0035(12) 0.0122(8) F4 F 0.0380(10) 0.0027(4) 0.0506(11) 0.001997 -0.0011(8) 0 F5 F 0.0203(13) 0.0277(18) 0.0131(12) 0.0165(13) 0.0104(10) 0.0027(11) F6 F 0.0174(13) 0.0193(12) 0.0120(11) 0.0113(11) -0.0001(9) 0.0044(9) F7 F 0.0380(10) 0.0027(4) 0.0506(11) 0.001997 -0.0011(8) 0 F8 F 0.0252(8) 0.0208(12) 0.0240(7) 0.0113(12) -0.0035(12) 0.0122(8) F9 F 0.0203(13) 0.0277(18) 0.0131(12) 0.0165(13) 0.0104(10) 0.0027(11) F10 F 0.0174(13) 0.0193(12) 0.0120(11) 0.0113(11) -0.0001(9) 0.0044(9) F11 F 0.0252(8) 0.0208(12) 0.0240(7) 0.0113(12) -0.0035(12) 0.0122(8) F12 F 0.0380(10) 0.0027(4) 0.0506(11) 0.001997 -0.0011(8) 0 F13 F 0.0222(10) 0.0148(11) 0.0218(14) 0.0122(10) -0.0012(11) 0.0040(10) F14 F 0.0208(13) 0.0058(11) 0.0161(15) 0.0015(9) -0.0112(10) -0.0038(9) F15 F 0.0165(11) 0.0197(10) 0.0179(13) 0.0111(10) -0.0032(10) -0.0055(10) F16 F 0.0220(13) 0.0171(12) 0.0144(14) 0.0151(11) 0.0068(10) 0.0092(10) F17 F 0.0208(13) 0.0058(11) 0.0161(15) 0.0015(9) -0.0112(10) -0.0038(9) F18 F 0.0222(10) 0.0148(11) 0.0218(14) 0.0122(10) -0.0012(11) 0.0040(10) F19 F 0.0220(13) 0.0171(12) 0.0144(14) 0.0151(11) 0.0068(10) 0.0092(10) F20 F 0.0165(11) 0.0197(10) 0.0179(13) 0.0111(10) -0.0032(10) -0.0055(10) F21 F 0.0165(11) 0.0197(10) 0.0179(13) 0.0111(10) -0.0032(10) -0.0055(10) F22 F 0.0220(13) 0.0171(12) 0.0144(14) 0.0151(11) 0.0068(10) 0.0092(10) F23 F 0.0208(13) 0.0058(11) 0.0161(15) 0.0015(9) -0.0112(10) -0.0038(9) F24 F 0.0222(10) 0.0148(11) 0.0218(14) 0.0122(10) -0.0012(11) 0.0040(10) 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 Er1 F1 . . 2.299(5) ? Er1 F2 . . 2.274(5) ? Er1 F7 . 3_564 2.229(10) ? Er1 F13 . 2_665 2.170(5) ? Er1 F15 . 3_564 2.149(5) ? Er1 F17 . 3_564 2.260(8) ? Er1 F19 . . 2.279(6) ? Er2 F3 . . 2.259(5) ? Er2 F3 . 3_564 2.264(6) ? Er2 F4 . 3_564 2.205(11) ? Er2 F9 . 3_564 2.207(6) ? Er2 F10 . 2_665 2.228(6) ? Er2 F17 . 3_564 2.272(7) ? Er2 F19 . . 2.259(6) ? Er3 F5 . . 2.279(6) ? Er3 F6 . . 2.277(6) ? Er3 F12 . 3_654 2.230(11) ? Er3 F14 . 3_664 2.268(8) ? Er3 F16 . . 2.281(7) ? Er3 F21 . 3_664 2.143(5) ? Er3 F24 . 2_655 2.172(6) ? Er4 F1 . 2_765 2.217(5) ? Er4 F2 . 3_554 2.215(6) ? Er4 F7 . 3_654 2.201(10) ? Er4 F8 . 1_655 2.257(5) ? Er4 F8 . 3_654 2.263(6) ? Er4 F14 . 3_664 2.269(8) ? Er4 F16 . . 2.266(7) ? Er5 F4 . 3_564 2.230(11) ? Er5 F9 . . 2.280(5) ? Er5 F10 . . 2.281(6) ? Er5 F18 . 2_665 2.171(5) ? Er5 F20 . 3_564 2.144(5) ? Er5 F22 . 1_655 2.248(7) ? Er5 F23 . 3_664 2.290(8) ? Er6 F5 . 3_664 2.226(6) ? Er6 F6 . 2_655 2.208(5) ? Er6 F11 . . 2.266(5) ? Er6 F11 . 3_664 2.234(7) ? Er6 F12 . 3_654 2.215(10) ? Er6 F22 . 1_655 2.265(7) ? Er6 F23 . 3_664 2.268(7) ? K1 F2 . 3_564 3.026(8) ? K1 F6 . 2_655 2.945(8) ? K1 F8 . 1_665 2.957(6) ? K1 F13 . . 2.618(6) ? K1 F14 . . 2.594(7) ? K1 F15 . 3_664 2.590(9) ? K1 F18 . 2_665 2.518(7) ? K1 F23 . 3_664 2.980(6) ? K2 F1 . 2_665 2.878(8) ? K2 F5 . 3_664 2.873(10) ? K2 F7 . 3_554 3.032(6) ? K2 F13 . 2_655 2.637(10) ? K2 F15 . . 2.629(6) ? K2 F16 . 3_664 2.600(6) ? K2 F20 . 3_564 2.652(7) ? K2 F22 . 1_655 2.884(5) ? K3 F1 . 2_665 2.905(9) ? K3 F3 . . 2.905(6) ? K3 F9 . 3_564 3.009(7) ? K3 F14 . 3_564 2.882(6) ? K3 F17 . . 2.592(7) ? K3 F18 . . 2.601(6) ? K3 F20 . 3_564 2.626(9) ? K3 F24 . 2_555 2.624(8) ? K4 F2 . 3_564 2.854(9) ? K4 F4 . 3_564 3.056(7) ? K4 F10 . 2_665 2.936(8) ? K4 F16 . 1_565 2.907(5) ? K4 F18 . 2_665 2.596(9) ? K4 F19 . 3_564 2.634(6) ? K4 F20 . . 2.636(6) ? K4 F21 . 3_674 2.597(8) ? K5 F6 . 2_655 3.061(8) ? K5 F9 . 3_664 2.910(9) ? K5 F11 . 3_664 2.947(8) ? K5 F15 . 3_664 2.622(7) ? K5 F19 . 1_655 2.919(5) ? K5 F21 . . 2.595(6) ? K5 F22 . 3_554 2.616(6) ? K5 F24 . 2_655 2.597(10) ? K6 F5 . 3_664 2.885(8) ? K6 F10 . 2_655 2.843(9) ? K6 F12 . 3_654 2.900(7) ? K6 F13 . 2_655 2.564(7) ? K6 F17 . 3_554 2.877(5) ? K6 F21 . 3_664 2.646(10) ? K6 F23 . . 2.582(6) ? K6 F24 . . 2.639(6) ? F1 F7 . 2_564 2.993(9) ? F1 F7 . 3_564 2.754(10) ? F1 F14 . 2_664 2.968(7) ? F1 F15 . 3_564 2.905(7) ? F1 F16 . 3_674 3.152(8) ? F1 F17 . 3_564 2.731(11) ? F2 F7 . 3_564 2.812(10) ? F2 F8 . 1_565 3.183(10) ? F2 F8 . 2_565 2.924(8) ? F2 F13 . 2_665 3.004(7) ? F2 F15 . 3_564 3.161(7) ? F2 F16 . 2_555 3.017(8) ? F2 F19 . . 2.802(10) ? F3 F4 . . 2.640(8) ? F3 F4 . 3_564 2.722(10) ? F3 F9 . . 3.122(10) ? F3 F9 . 3_564 2.906(8) ? F3 F17 . . 2.669(7) ? F3 F19 . . 2.791(10) ? F4 F9 . 2_665 2.805(8) ? F4 F10 . 2_665 2.743(9) ? F4 F10 . 3_565 3.018(8) ? F4 F18 . 3_565 2.824(10) ? F4 F20 . . 3.158(8) ? F5 F12 . 1_665 2.981(10) ? F5 F12 . 3_654 2.756(11) ? F5 F16 . . 2.804(11) ? F5 F22 . 2_665 2.914(8) ? F5 F23 . . 3.090(8) ? F5 F24 . 2_655 2.940(7) ? F6 F11 . 2_654 2.885(8) ? F6 F11 . 3_664 3.080(11) ? F6 F12 . 3_654 2.801(10) ? F6 F14 . 3_664 2.749(11) ? F6 F21 . 3_664 2.935(7) ? F6 F23 . 2_654 3.119(7) ? F6 F24 . 2_655 3.108(8) ? F7 F8 . . 2.636(7) ? F7 F8 . 2_555 2.718(11) ? F7 F13 . 3_565 2.832(11) ? F7 F15 . . 3.139(7) ? F8 F14 . 1_445 2.669(7) ? F8 F16 . 1_455 2.778(10) ? F9 F17 . . 3.189(7) ? F9 F18 . 2_665 3.004(7) ? F9 F19 . 2_665 3.023(7) ? F9 F20 . 3_564 3.125(7) ? F9 F22 . 1_655 2.752(10) ? F10 F17 . 2_664 2.993(7) ? F10 F19 . 3_564 3.154(7) ? F10 F20 . 3_564 2.915(7) ? F10 F23 . 3_664 2.790(11) ? F11 F12 . 1_665 2.722(9) ? F11 F12 . 3_654 2.624(11) ? F11 F22 . 1_655 2.699(10) ? F11 F23 . . 2.804(8) ? F12 F21 . 1_445 2.828(7) ? F12 F24 . 3_555 3.162(12) ? F13 F17 . 2_664 2.878(9) ? F14 F16 . 2_655 2.494(9) ? F14 F24 . 3_665 2.918(7) ? F15 F19 . 2_665 2.927(10) ? F16 F21 . 3_664 2.865(11) ? F17 F19 . 2_665 2.487(8) ? F18 F23 . 2_554 2.871(9) ? F20 F22 . 2_675 2.913(10) ? F22 F23 . 3_564 2.489(7) ? 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 ? ? ? ? ? ? ? ? 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 ? ? ? ? ? ? ? ? ? ? ? #======================================================================= data_II _database_code_depnum_ccdc_archive 'CCDC 891237' #TrackingRef '- KHoF4_AP_final.cif' #======================================================================= # 5. CHEMICAL DATA _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_iupac ? _chemical_formula_sum 'F4 Ho1 K1' _chemical_formula_weight 420 _chemical_melting_point ? _chemical_compound_source ? _chemical_absolute_configuration ? #======================================================================= # 6. CRYSTAL DATA _symmetry_cell_setting trigonal _symmetry_space_group_name_H-M 'P 31' _symmetry_space_group_name_Hall 'P 31' _symmetry_Int_Tables_number 144 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 -y,x-y,z+1/3 3 -x+y,-x,z+2/3 _cell_length_a 14.1900(10) _cell_length_b 14.1900(10) _cell_length_c 10.2000(10) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 120 _cell_volume 1778.7(2) loop_ _jana_cell_twin_matrix_id _jana_cell_twin_volume_fraction _jana_cell_twin_matrix_1_1 _jana_cell_twin_matrix_1_2 _jana_cell_twin_matrix_1_3 _jana_cell_twin_matrix_2_1 _jana_cell_twin_matrix_2_2 _jana_cell_twin_matrix_2_3 _jana_cell_twin_matrix_3_1 _jana_cell_twin_matrix_3_2 _jana_cell_twin_matrix_3_3 1 0.4858(9) 1 0 0 0 1 0 0 0 1 2 0 -1 0 0 0 -1 0 0 0 -1 3 0 1 -1 0 0 -1 0 0 0 -1 4 0.5142(9) -1 1 0 0 1 0 0 0 -1 _cell_formula_units_Z 18 _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _cell_measurement_temperature 293 _cell_special_details ; ? ; _exptl_crystal_density_diffrn 4.7041 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_F_000 2196 _exptl_absorpt_coefficient_mu 4.583 _exptl_crystal_description ? _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.04 _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 ? #======================================================================= # 7. EXPERIMENTAL DATA _exptl_special_details ? _diffrn_ambient_temperature 293 _diffrn_source ? _diffrn_source_power ? _diffrn_source_voltage ? _diffrn_source_current ? _diffrn_radiation_type ? _diffrn_radiation_source ? _diffrn_radiation_wavelength 0.4 _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 100915 _diffrn_reflns_theta_min 0.93 _diffrn_reflns_theta_max 25.85 _diffrn_reflns_theta_full 25.84 _diffrn_measured_fraction_theta_max 0 _diffrn_measured_fraction_theta_full 1 _diffrn_reflns_av_R_equivalents 0.0532 _diffrn_reflns_av_sigmaI/netI 0.0461 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _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 25515 _reflns_number_gt 23389 _reflns_threshold_expression I>3\s(I) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.0304 _refine_ls_wR_factor_gt 0.0350 _refine_ls_R_factor_all 0.0344 _refine_ls_wR_factor_ref 0.0358 _refine_ls_goodness_of_fit_ref 1.19 _refine_ls_goodness_of_fit_gt 1.21 _refine_ls_restrained_S_gt ? _refine_ls_restrained_S_all ? _refine_ls_number_reflns 25515 _refine_ls_number_parameters 231 _refine_ls_number_restraints 0 _refine_ls_number_constraints 1 _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 0.0188 _refine_ls_shift/su_mean 0.0028 _refine_diff_density_max 1.59 _refine_diff_density_min -2.19 _refine_ls_extinction_method 'B-C type 1 Gaussian isotropic (Becker & Coppens, 1974)' _refine_ls_extinction_coef 6010(180) _refine_ls_abs_structure_details ; 24839 of Friedel pairs used in the refinement ; _refine_ls_abs_structure_Flack 0 _refine_ls_abs_structure_Rogers ? loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source F 0.0032 0.0029 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' Ho -0.7065 1.7570 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' K 0.0760 0.0798 '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 ? #======================================================================= # 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_symmetry_multiplicity _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ho1 Ho 0.13092(3) 0.89028(4) 0.32997(5) Uani 0.00647(8) 3 1 d . . . Ho2 Ho 0.28333(4) 0.73244(4) 0.31985(6) Uani 0.00601(8) 3 1 d . . . Ho3 Ho 0.77991(5) 0.20619(4) 0.33963(4) Uani 0.00640(8) 3 1 d . . . Ho4 Ho 0.94280(4) 0.05934(5) 0.32538(7) Uani 0.00682(8) 3 1 d . . . Ho5 Ho 0.45263(5) 0.54464(6) 0.32348(4) Uani 0.00677(7) 3 1 d . . . Ho6 Ho 0.60445(4) 0.38679(4) 0.34418(3) Uani 0.00634(8) 3 1 d . . . K1 K 0.7812(2) 0.71865(19) 0.3212(2) Uani 0.0188(7) 3 1 d . . . K2 K 0.26731(18) 0.22010(18) 0.3473(2) Uani 0.0158(6) 3 1 d . . . K3 K 0.10348(19) 0.3955(2) 0.3126(2) Uani 0.0178(5) 3 1 d . . . K4 K 0.6114(2) 0.87697(17) 0.3469(2) Uani 0.0171(6) 3 1 d . . . K5 K 0.9492(2) 0.56257(20) 0.3449(2) Uani 0.0194(6) 3 1 d . . . K6 K 0.45537(17) 0.06479(14) 0.3138(2) Uani 0.0158(5) 3 1 d . . . F1 F 0.1314(4) 0.9341(3) 0.1128(4) Uani 0.0158(9) 3 1 d . . . F2 F 0.0694(4) 0.8779(4) 0.5400(4) Uani 0.0176(10) 3 1 d . . . F3 F 0.2103(4) 0.5940(3) 0.4670(5) Uani 0.0224(7) 3 1 d . . . F4 F 0.3341(4) 0.7293(3) 0.6513(7) Uani 0.0305(8) 3 1 d . . . F5 F 0.7379(4) 0.2035(4) 0.5577(5) Uani 0.0176(10) 3 1 d . . . F6 F 0.7885(3) 0.2679(4) 0.1307(5) Uani 0.0158(9) 3 1 d . . . F7 F -0.0034(4) 0.0602(3) 0.6599(6) Uani 0.0305(8) 3 1 d . . . F8 F -0.1221(4) -0.0774(3) 0.4741(4) Uani 0.0224(7) 3 1 d . . . F9 F 0.3905(4) 0.5374(4) 0.5331(4) Uani 0.0176(10) 3 1 d . . . F10 F 0.4569(4) 0.5886(3) 0.1062(5) Uani 0.0158(9) 3 1 d . . . F11 F 0.5463(4) 0.2904(4) 0.5350(5) Uani 0.0224(7) 3 1 d . . . F12 F 0.7361(4) 0.3949(3) 0.6776(6) Uani 0.0305(8) 3 1 d . . . F13 F 0.7675(4) 0.7281(3) 0.0649(5) Uani 0.0162(7) 3 1 d . . . F14 F 0.8078(4) 0.7233(3) 0.5753(5) Uani 0.0150(7) 3 1 d . . . F15 F 0.2479(3) 0.2233(3) 0.6072(5) Uani 0.0155(7) 3 1 d . . . F16 F 0.8086(4) 0.0749(4) 0.4302(5) Uani 0.0147(8) 3 1 d . . . F17 F 0.1306(3) 0.3946(3) 0.5673(5) Uani 0.0150(7) 3 1 d . . . F18 F 0.0917(3) 0.4027(3) 0.0612(4) Uani 0.0162(7) 3 1 d . . . F19 F 0.1539(3) 0.7554(3) 0.4241(4) Uani 0.0147(8) 3 1 d . . . F20 F 0.5892(3) 0.8837(3) 0.6032(4) Uani 0.0155(7) 3 1 d . . . F21 F 0.9377(3) 0.5758(3) 0.6002(5) Uani 0.0155(7) 3 1 d . . . F22 F -0.5325(4) 0.4106(4) 0.4255(5) Uani 0.0147(8) 3 1 d . . . F23 F 0.4846(3) 0.0702(3) 0.5686(4) Uani 0.0150(7) 3 1 d . . . F24 F 0.4535(4) 0.0868(3) 0.0582(5) Uani 0.0162(7) 3 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 Ho1 Ho 0.00686(9) 0.00825(10) 0.00621(11) 0.00521(8) -0.00007(8) -0.00037(8) Ho2 Ho 0.00518(10) 0.00570(10) 0.00780(13) 0.00321(8) -0.00091(10) -0.00072(8) Ho3 Ho 0.00714(10) 0.00697(10) 0.00646(11) 0.00454(8) 0.00102(8) 0.00048(8) Ho4 Ho 0.00633(10) 0.00635(11) 0.00864(11) 0.00381(8) -0.00062(10) -0.00039(9) Ho5 Ho 0.00713(9) 0.00815(9) 0.00682(10) 0.00515(8) -0.00006(8) -0.00019(8) Ho6 Ho 0.00636(10) 0.00712(9) 0.00746(9) 0.00480(11) -0.00121(9) -0.00085(9) K1 K 0.0159(7) 0.0289(11) 0.0082(6) 0.0086(7) 0.0039(6) 0.0075(6) K2 K 0.0250(8) 0.0163(7) 0.0062(5) 0.0103(6) 0.0049(5) 0.0037(5) K3 K 0.0159(6) 0.0231(7) 0.0138(6) 0.0094(6) -0.0040(5) -0.0005(7) K4 K 0.0321(9) 0.0121(6) 0.0113(6) 0.0142(7) 0.0025(6) 0.0041(4) K5 K 0.0305(11) 0.0133(6) 0.0164(6) 0.0124(6) 0.0042(6) 0.0019(5) K6 K 0.0157(7) 0.0115(5) 0.0166(7) 0.0040(4) -0.0009(5) 0.0020(4) F1 F 0.0201(13) 0.0190(10) 0.0123(10) 0.0128(10) 0.0019(8) 0.0068(8) F2 F 0.0209(11) 0.0282(16) 0.0097(9) 0.0168(11) 0.0074(8) 0.0008(8) F3 F 0.0280(8) 0.0182(9) 0.0188(7) 0.0099(9) -0.0044(10) 0.0094(6) F4 F 0.0313(11) 0.0036(4) 0.0487(11) 0.0027(9) 0.0009(9) 0.0010(12) F5 F 0.0209(11) 0.0282(16) 0.0097(9) 0.0168(11) 0.0074(8) 0.0008(8) F6 F 0.0201(13) 0.0190(10) 0.0123(10) 0.0128(10) 0.0019(8) 0.0068(8) F7 F 0.0313(11) 0.0036(4) 0.0487(11) 0.0027(9) 0.0009(9) 0.0010(12) F8 F 0.0280(8) 0.0182(9) 0.0188(7) 0.0099(9) -0.0044(10) 0.0094(6) F9 F 0.0209(11) 0.0282(16) 0.0097(9) 0.0168(11) 0.0074(8) 0.0008(8) F10 F 0.0201(13) 0.0190(10) 0.0123(10) 0.0128(10) 0.0019(8) 0.0068(8) F11 F 0.0280(8) 0.0182(9) 0.0188(7) 0.0099(9) -0.0044(10) 0.0094(6) F12 F 0.0313(11) 0.0036(4) 0.0487(11) 0.0027(9) 0.0009(9) 0.0010(12) F13 F 0.0203(8) 0.0137(8) 0.0170(10) 0.0103(8) -0.0030(8) 0.0028(8) F14 F 0.0184(9) 0.0078(9) 0.0130(10) 0.0022(7) -0.0077(8) -0.0022(7) F15 F 0.0136(8) 0.0174(8) 0.0179(10) 0.0096(7) -0.0008(8) -0.0020(7) F16 F 0.0213(10) 0.0178(10) 0.0141(10) 0.0166(9) 0.0079(8) 0.0095(8) F17 F 0.0184(9) 0.0078(9) 0.0130(10) 0.0022(7) -0.0077(8) -0.0022(7) F18 F 0.0203(8) 0.0137(8) 0.0170(10) 0.0103(8) -0.0030(8) 0.0028(8) F19 F 0.0213(10) 0.0178(10) 0.0141(10) 0.0166(9) 0.0079(8) 0.0095(8) F20 F 0.0136(8) 0.0174(8) 0.0179(10) 0.0096(7) -0.0008(8) -0.0020(7) F21 F 0.0136(8) 0.0174(8) 0.0179(10) 0.0096(7) -0.0008(8) -0.0020(7) F22 F 0.0213(10) 0.0178(10) 0.0141(10) 0.0166(9) 0.0079(8) 0.0095(8) F23 F 0.0184(9) 0.0078(9) 0.0130(10) 0.0022(7) -0.0077(8) -0.0022(7) F24 F 0.0203(8) 0.0137(8) 0.0170(10) 0.0103(8) -0.0030(8) 0.0028(8) 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 Ho1 F1 . . 2.300(4) ? Ho1 F2 . . 2.287(4) ? Ho1 F7 . 3_564 2.242(8) ? Ho1 F13 . 2_665 2.176(4) ? Ho1 F15 . 3_564 2.171(4) ? Ho1 F17 . 3_564 2.274(7) ? Ho1 F19 . . 2.306(5) ? Ho2 F3 . . 2.270(4) ? Ho2 F3 . 3_564 2.266(5) ? Ho2 F4 . 3_564 2.216(9) ? Ho2 F9 . 3_564 2.218(5) ? Ho2 F10 . 2_665 2.237(5) ? Ho2 F17 . 3_564 2.270(6) ? Ho2 F19 . . 2.282(5) ? Ho3 F5 . . 2.298(5) ? Ho3 F6 . . 2.284(5) ? Ho3 F12 . 3_664 2.243(8) ? Ho3 F14 . 3_664 2.262(7) ? Ho3 F16 . . 2.291(6) ? Ho3 F21 . 3_664 2.158(4) ? Ho3 F24 . 2_655 2.176(5) ? Ho4 F1 . 2_765 2.232(5) ? Ho4 F2 . 3_554 2.225(5) ? Ho4 F7 . 3_654 2.220(8) ? Ho4 F8 . 1_655 2.264(4) ? Ho4 F8 . 3_654 2.268(5) ? Ho4 F14 . 3_664 2.271(6) ? Ho4 F16 . . 2.289(6) ? Ho5 F4 . 3_564 2.243(8) ? Ho5 F9 . . 2.295(5) ? Ho5 F10 . . 2.295(5) ? Ho5 F18 . 2_665 2.175(4) ? Ho5 F20 . 3_564 2.163(4) ? Ho5 F22 . 1_655 2.269(6) ? Ho5 F23 . 3_664 2.307(7) ? Ho6 F5 . 3_664 2.241(5) ? Ho6 F6 . 2_655 2.224(5) ? Ho6 F11 . . 2.283(5) ? Ho6 F11 . 3_664 2.249(6) ? Ho6 F12 . 3_664 2.232(8) ? Ho6 F22 . 1_655 2.288(6) ? Ho6 F23 . 3_664 2.264(6) ? K1 F2 . 3_564 3.065(6) ? K1 F6 . 2_655 2.923(7) ? K1 F8 . 1_665 2.953(5) ? K1 F13 . . 2.629(5) ? K1 F14 . . 2.616(5) ? K1 F15 . 3_664 2.597(7) ? K1 F18 . 2_665 2.540(6) ? K1 F23 . 3_664 2.964(5) ? K2 F1 . 2_665 2.892(6) ? K2 F5 . 3_664 2.857(8) ? K2 F7 . 3_554 2.995(5) ? K2 F13 . 2_655 2.649(8) ? K2 F15 . . 2.668(5) ? K2 F16 . 3_664 2.585(5) ? K2 F20 . 3_564 2.655(5) ? K2 F22 . 1_655 2.887(4) ? K3 F1 . 2_665 2.923(7) ? K3 F3 . . 2.906(5) ? K3 F9 . 3_564 3.009(6) ? K3 F14 . 3_564 2.873(5) ? K3 F17 . . 2.627(5) ? K3 F18 . . 2.575(5) ? K3 F20 . 3_564 2.645(7) ? K3 F24 . 2_555 2.646(6) ? K4 F2 . 3_564 2.885(7) ? K4 F4 . 3_564 3.047(5) ? K4 F10 . 2_665 2.934(7) ? K4 F16 . 1_565 2.929(4) ? K4 F18 . 2_665 2.618(7) ? K4 F19 . 3_564 2.641(5) ? K4 F20 . . 2.641(5) ? K4 F21 . 3_674 2.594(6) ? K5 F6 . 2_655 3.080(6) ? K5 F9 . 3_664 2.938(7) ? K5 F11 . 3_664 2.915(6) ? K5 F15 . 3_664 2.626(6) ? K5 F19 . 1_655 2.937(4) ? K5 F21 . . 2.622(5) ? K5 F22 . 3_554 2.607(5) ? K5 F24 . 2_655 2.606(7) ? K6 F5 . 3_664 2.879(7) ? K6 F10 . 2_655 2.841(7) ? K6 F12 . 3_664 2.874(5) ? K6 F13 . 2_655 2.590(6) ? K6 F17 . 3_554 2.863(4) ? K6 F21 . 3_664 2.655(8) ? K6 F23 . . 2.627(5) ? K6 F24 . . 2.628(5) ? F1 F7 . 2_564 2.994(8) ? F1 F7 . 3_564 2.756(9) ? F1 F14 . 2_664 2.956(6) ? F1 F15 . 3_564 2.924(5) ? F1 F16 . 3_674 3.168(6) ? F1 F17 . 3_564 2.764(9) ? F2 F7 . 3_564 2.839(8) ? F2 F8 . 1_565 3.156(8) ? F2 F8 . 2_565 2.921(7) ? F2 F13 . 2_665 3.003(6) ? F2 F15 . 3_564 3.155(6) ? F2 F16 . 2_555 3.064(6) ? F2 F19 . . 2.819(8) ? F3 F4 . . 2.633(7) ? F3 F4 . 3_564 2.749(8) ? F3 F9 . . 3.113(9) ? F3 F9 . 3_564 2.914(7) ? F3 F17 . . 2.670(6) ? F3 F19 . . 2.813(8) ? F4 F9 . 2_665 2.833(7) ? F4 F10 . 2_665 2.756(8) ? F4 F10 . 3_565 3.030(7) ? F4 F18 . 3_565 2.829(8) ? F4 F20 . . 3.196(6) ? F5 F12 . . 2.992(8) ? F5 F12 . 3_664 2.774(9) ? F5 F16 . . 2.802(9) ? F5 F22 . 2_665 2.931(6) ? F5 F23 . . 3.116(6) ? F5 F24 . 2_655 2.943(6) ? F6 F11 . 2_654 2.873(7) ? F6 F11 . 3_664 3.088(9) ? F6 F12 . 3_664 2.834(9) ? F6 F14 . 3_664 2.761(9) ? F6 F21 . 3_664 2.961(6) ? F6 F23 . 2_654 3.102(6) ? F6 F24 . 2_655 3.114(6) ? F7 F8 . . 2.637(6) ? F7 F8 . 2_555 2.738(9) ? F7 F13 . 3_565 2.833(9) ? F7 F15 . . 3.179(6) ? F8 F14 . 1_445 2.691(6) ? F8 F16 . 1_455 2.822(9) ? F9 F18 . 2_665 2.987(5) ? F9 F19 . 2_665 3.054(6) ? F9 F20 . 3_564 3.137(6) ? F9 F22 . 1_655 2.757(9) ? F10 F17 . 2_664 2.968(6) ? F10 F19 . 3_564 3.177(6) ? F10 F20 . 3_564 2.941(6) ? F10 F23 . 3_664 2.836(9) ? F11 F12 . . 2.752(7) ? F11 F12 . 3_664 2.660(9) ? F11 F22 . 1_655 2.704(9) ? F11 F23 . . 2.813(7) ? F12 F21 . . 2.838(6) ? F12 F24 . 3_665 3.181(10) ? F13 F17 . 2_664 2.893(8) ? F14 F16 . 2_655 2.497(8) ? F14 F24 . 3_665 2.922(6) ? F15 F19 . 2_665 2.940(8) ? F16 F21 . 3_664 2.868(9) ? F17 F19 . 2_665 2.508(7) ? F18 F23 . 2_554 2.886(7) ? F20 F22 . 2_675 2.925(8) ? F22 F23 . 3_564 2.508(6) ? 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 ? ? ? ? ? ? ? ? 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 ? ? ? ? ? ? ? ? ? ? ? #======================================================================= data_III _database_code_depnum_ccdc_archive 'CCDC 891238' #TrackingRef '- KTmF4_AP_final.cif' #======================================================================= # 5. CHEMICAL DATA _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_iupac ? _chemical_formula_sum 'F4 K1 Tm1' _chemical_formula_weight 426 _chemical_melting_point ? _chemical_compound_source ? _chemical_absolute_configuration ? #======================================================================= # 6. CRYSTAL DATA _symmetry_cell_setting trigonal _symmetry_space_group_name_H-M 'P 32' _symmetry_space_group_name_Hall 'P 32' _symmetry_Int_Tables_number 145 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 -y,x-y,z+2/3 3 -x+y,-x,z+1/3 _cell_length_a 14.087(2) _cell_length_b 14.087(2) _cell_length_c 10.1460(10) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 120 _cell_volume 1743.7(4) loop_ _jana_cell_twin_matrix_id _jana_cell_twin_volume_fraction _jana_cell_twin_matrix_1_1 _jana_cell_twin_matrix_1_2 _jana_cell_twin_matrix_1_3 _jana_cell_twin_matrix_2_1 _jana_cell_twin_matrix_2_2 _jana_cell_twin_matrix_2_3 _jana_cell_twin_matrix_3_1 _jana_cell_twin_matrix_3_2 _jana_cell_twin_matrix_3_3 1 0.4953(10) 1 0 0 0 1 0 0 0 1 2 0 -1 0 0 0 -1 0 0 0 -1 3 0 1 -1 0 0 -1 0 0 0 -1 4 0.5047(10) -1 1 0 0 1 0 0 0 -1 _cell_formula_units_Z 18 _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _cell_measurement_temperature 293 _cell_special_details ; ? ; _exptl_crystal_density_diffrn 4.8671 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_F_000 2232 _exptl_absorpt_coefficient_mu 5.241 _exptl_crystal_description ? _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.05 _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 ? #======================================================================= # 7. EXPERIMENTAL DATA _exptl_special_details ? _diffrn_ambient_temperature 293 _diffrn_source ? _diffrn_source_power ? _diffrn_source_voltage ? _diffrn_source_current ? _diffrn_radiation_type ? _diffrn_radiation_source ? _diffrn_radiation_wavelength 0.4 _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 100309 _diffrn_reflns_theta_min 0.94 _diffrn_reflns_theta_max 25.85 _diffrn_reflns_theta_full 25.84 _diffrn_measured_fraction_theta_max 0 _diffrn_measured_fraction_theta_full 0.99 _diffrn_reflns_av_R_equivalents 0.0413 _diffrn_reflns_av_sigmaI/netI 0.0321 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _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 24992 _reflns_number_gt 24255 _reflns_threshold_expression I>3\s(I) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.0301 _refine_ls_wR_factor_gt 0.0385 _refine_ls_R_factor_all 0.0310 _refine_ls_wR_factor_ref 0.0386 _refine_ls_goodness_of_fit_ref 1.71 _refine_ls_goodness_of_fit_gt 1.73 _refine_ls_restrained_S_gt ? _refine_ls_restrained_S_all ? _refine_ls_number_reflns 24992 _refine_ls_number_parameters 231 _refine_ls_number_restraints 0 _refine_ls_number_constraints 1 _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 0.0427 _refine_ls_shift/su_mean 0.0086 _refine_diff_density_max 3.49 _refine_diff_density_min -3.37 _refine_ls_extinction_method 'B-C type 1 Gaussian isotropic (Becker & Coppens, 1974)' _refine_ls_extinction_coef 5200(400) _refine_ls_abs_structure_details ; 24331 of Friedel pairs used in the refinement ; _refine_ls_abs_structure_Flack 0 _refine_ls_abs_structure_Rogers ? loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source F 0.0032 0.0029 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' K 0.0760 0.0798 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' Tm -0.6440 1.9847 '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 ? #======================================================================= # 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_symmetry_multiplicity _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Tm1 Tm 0.12764(4) 0.88686(4) 0.66930(5) Uani 0.00854(8) 3 1 d . . . Tm2 Tm 0.28098(4) 0.73088(4) 0.67972(5) Uani 0.00683(8) 3 1 d . . . Tm3 Tm 0.77849(4) 0.20520(4) 0.66356(4) Uani 0.00623(6) 3 1 d . . . Tm4 Tm 0.94085(6) 0.05764(6) 0.67311(8) Uani 0.00832(8) 3 1 d . . . Tm5 Tm 0.45217(6) 0.54475(6) 0.67551(4) Uani 0.00666(6) 3 1 d . . . Tm6 Tm 0.60485(4) 0.38809(4) 0.66008(4) Uani 0.00624(8) 3 1 d . . . K7 K 0.26504(19) 0.22064(19) 0.6510(2) Uani 0.0169(5) 3 1 d . . . K8 K 0.7811(2) 0.7188(2) 0.6814(2) Uani 0.0214(6) 3 1 d . . . K9 K 0.6068(2) 0.87666(16) 0.65505(17) Uani 0.0152(5) 3 1 d . . . K10 K 0.1039(2) 0.3920(2) 0.6833(2) Uani 0.0182(6) 3 1 d . . . K11 K 0.45351(19) 0.06488(19) 0.68443(18) Uani 0.0183(5) 3 1 d . . . K12 K 0.9447(2) 0.55911(19) 0.6549(2) Uani 0.0185(6) 3 1 d . . . F1 F 0.1340(4) 0.9396(4) 0.8845(4) Uani 0.0190(11) 3 1 d . . . F2 F 0.0712(3) 0.8783(3) 0.4580(4) Uani 0.0149(9) 3 1 d . . . F3 F 0.2087(4) 0.5951(3) 0.5294(4) Uani 0.0217(7) 3 1 d . . . F4 F 0.3375(5) 0.7291(3) 0.3462(6) Uani 0.0315(7) 3 1 d . . . F5 F 0.7366(3) 0.2044(4) 0.4468(4) Uani 0.0149(9) 3 1 d . . . F6 F 0.7911(4) 0.2707(4) 0.8717(4) Uani 0.0190(11) 3 1 d . . . F7 F 0.0083(4) 0.0603(3) 0.3377(5) Uani 0.0315(7) 3 1 d . . . F8 F -0.1255(3) -0.0729(3) 1.5168(4) Uani 0.0217(7) 3 1 d . . . F9 F 0.3947(3) 0.5392(3) 0.4648(4) Uani 0.0149(9) 3 1 d . . . F10 F 0.4609(5) 0.5942(4) 0.8912(4) Uani 0.0190(11) 3 1 d . . . F11 F 0.5450(4) 0.2867(3) 0.4740(4) Uani 0.0217(7) 3 1 d . . . F12 F -0.2698(5) -0.6070(3) 1.3294(6) Uani 0.0315(7) 3 1 d . . . F13 F 0.7687(4) 0.7317(3) 0.9380(4) Uani 0.0170(7) 3 1 d . . . F14 F 0.8109(4) 0.7241(3) 0.4293(5) Uani 0.0174(9) 3 1 d . . . F15 F 0.2503(3) 0.2258(3) 0.3962(4) Uani 0.0161(7) 3 1 d . . . F16 F 0.8065(4) 0.0739(4) 1.5735(4) Uani 0.0143(8) 3 1 d . . . F17 F 0.1331(4) 0.3930(3) 0.4342(4) Uani 0.0174(9) 3 1 d . . . F18 F 0.0930(3) 0.4030(3) 0.9398(4) Uani 0.0170(7) 3 1 d . . . F19 F 0.1512(3) 0.7534(3) 0.5782(4) Uani 0.0143(8) 3 1 d . . . F20 F 0.5879(3) 0.8837(3) 0.3982(4) Uani 0.0161(7) 3 1 d . . . F21 F 0.9366(3) 0.5724(3) 0.4017(4) Uani 0.0161(7) 3 1 d . . . F22 F -0.5311(3) 0.4113(4) 1.5780(4) Uani 0.0143(8) 3 1 d . . . F23 F 0.4834(4) 0.0667(3) 1.4339(4) Uani 0.0174(9) 3 1 d . . . F24 F 0.4513(3) 0.0869(3) 0.9442(4) Uani 0.0170(7) 3 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 Tm1 Tm 0.00950(9) 0.01101(9) 0.00864(10) 0.00777(8) -0.00017(9) 0.00028(9) Tm2 Tm 0.00708(11) 0.00668(9) 0.00787(13) 0.00429(7) 0.00132(8) 0.00083(7) Tm3 Tm 0.00648(8) 0.00655(8) 0.00648(8) 0.00386(6) -0.00119(6) -0.00057(6) Tm4 Tm 0.00857(10) 0.00844(9) 0.00994(12) 0.00575(8) 0.00279(8) 0.00250(8) Tm5 Tm 0.00683(7) 0.00752(7) 0.00735(8) 0.00487(6) 0.00017(8) 0.00030(8) Tm6 Tm 0.00600(9) 0.00676(9) 0.00726(10) 0.00417(9) -0.00020(7) -0.00017(7) K7 K 0.0265(7) 0.0152(6) 0.0111(5) 0.0120(5) -0.0039(5) -0.0038(4) K8 K 0.0144(6) 0.0314(10) 0.0156(7) 0.0094(6) -0.0040(5) -0.0086(6) K9 K 0.0266(8) 0.0106(6) 0.0093(4) 0.0099(6) 0.0007(5) -0.0024(3) K10 K 0.0169(6) 0.0235(8) 0.0110(5) 0.0077(6) 0.0006(5) 0.0002(6) K11 K 0.0171(7) 0.0199(7) 0.0163(5) 0.0080(5) 0.0023(5) -0.0083(5) K12 K 0.0331(9) 0.0151(6) 0.0118(5) 0.0153(6) -0.0025(6) -0.0027(4) F1 F 0.0298(17) 0.0242(13) 0.0108(9) 0.0195(13) -0.0020(8) -0.0081(8) F2 F 0.0170(10) 0.0168(12) 0.0132(9) 0.0102(9) -0.0063(7) -0.0013(7) F3 F 0.0237(7) 0.0204(10) 0.0210(6) 0.0110(9) 0.0027(8) -0.0107(6) F4 F 0.0367(11) 0.0047(4) 0.0401(8) 0.0007(8) 0.0008(8) -0.0008(10) F5 F 0.0170(10) 0.0168(12) 0.0132(9) 0.0102(9) -0.0063(7) -0.0013(7) F6 F 0.0298(17) 0.0242(13) 0.0108(9) 0.0195(13) -0.0020(8) -0.0081(8) F7 F 0.0367(11) 0.0047(4) 0.0401(8) 0.0007(8) 0.0008(8) -0.0008(10) F8 F 0.0237(7) 0.0204(10) 0.0210(6) 0.0110(9) 0.0027(8) -0.0107(6) F9 F 0.0170(10) 0.0168(12) 0.0132(9) 0.0102(9) -0.0063(7) -0.0013(7) F10 F 0.0298(17) 0.0242(13) 0.0108(9) 0.0195(13) -0.0020(8) -0.0081(8) F11 F 0.0237(7) 0.0204(10) 0.0210(6) 0.0110(9) 0.0027(8) -0.0107(6) F12 F 0.0367(11) 0.0047(4) 0.0401(8) 0.0007(8) 0.0008(8) -0.0008(10) F13 F 0.0200(8) 0.0148(9) 0.0184(9) 0.0103(8) 0.0045(8) -0.0023(8) F14 F 0.0254(13) 0.0074(9) 0.0144(10) 0.0045(8) 0.0088(10) -0.0028(7) F15 F 0.0156(9) 0.0177(8) 0.0187(9) 0.0110(7) 0.0014(8) 0.0016(8) F16 F 0.0174(10) 0.0178(10) 0.0147(10) 0.0139(9) -0.0078(8) -0.0049(8) F17 F 0.0254(13) 0.0074(9) 0.0144(10) 0.0045(8) 0.0088(10) -0.0028(7) F18 F 0.0200(8) 0.0148(9) 0.0184(9) 0.0103(8) 0.0045(8) -0.0023(8) F19 F 0.0174(10) 0.0178(10) 0.0147(10) 0.0139(9) -0.0078(8) -0.0049(8) F20 F 0.0156(9) 0.0177(8) 0.0187(9) 0.0110(7) 0.0014(8) 0.0016(8) F21 F 0.0156(9) 0.0177(8) 0.0187(9) 0.0110(7) 0.0014(8) 0.0016(8) F22 F 0.0174(10) 0.0178(10) 0.0147(10) 0.0139(9) -0.0078(8) -0.0049(8) F23 F 0.0254(13) 0.0074(9) 0.0144(10) 0.0045(8) 0.0088(10) -0.0028(7) F24 F 0.0200(8) 0.0148(9) 0.0184(9) 0.0103(8) 0.0045(8) -0.0023(8) 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 Tm1 F1 . . 2.294(4) ? Tm1 F2 . . 2.269(4) ? Tm1 F7 . 3_565 2.212(8) ? Tm1 F13 . 2_664 2.153(4) ? Tm1 F15 . 3_565 2.136(4) ? Tm1 F17 . 3_565 2.251(7) ? Tm1 F19 . . 2.264(5) ? Tm2 F3 . . 2.252(4) ? Tm2 F3 . 3_565 2.261(5) ? Tm2 F4 . 3_565 2.204(9) ? Tm2 F9 . 3_565 2.206(4) ? Tm2 F10 . 2_664 2.217(5) ? Tm2 F17 . 3_565 2.263(7) ? Tm2 F19 . . 2.255(5) ? Tm3 F5 . . 2.276(4) ? Tm3 F6 . . 2.276(4) ? Tm3 F12 . 3_654 2.228(9) ? Tm3 F14 . 3_665 2.256(7) ? Tm3 F16 . 1_554 2.268(6) ? Tm3 F21 . 3_665 2.131(4) ? Tm3 F24 . 2_654 2.159(5) ? Tm4 F1 . 2_764 2.199(5) ? Tm4 F2 . 3_555 2.205(4) ? Tm4 F7 . 3_655 2.183(8) ? Tm4 F8 . 1_654 2.247(4) ? Tm4 F8 . 3_654 2.261(4) ? Tm4 F14 . 3_665 2.265(7) ? Tm4 F16 . 1_554 2.256(6) ? Tm5 F4 . 3_565 2.213(9) ? Tm5 F9 . . 2.273(4) ? Tm5 F10 . . 2.281(4) ? Tm5 F18 . 2_664 2.160(4) ? Tm5 F20 . 3_565 2.133(4) ? Tm5 F22 . 1_654 2.238(6) ? Tm5 F23 . 3_664 2.273(7) ? Tm6 F5 . 3_665 2.215(5) ? Tm6 F6 . 2_654 2.192(5) ? Tm6 F11 . . 2.260(4) ? Tm6 F11 . 3_665 2.240(5) ? Tm6 F12 . 3_654 2.192(8) ? Tm6 F22 . 1_654 2.257(6) ? Tm6 F23 . 3_664 2.258(6) ? K7 F1 . 2_664 2.899(7) ? K7 F5 . 3_665 2.918(7) ? K7 F7 . 3_555 3.126(5) ? K7 F13 . 2_654 2.653(8) ? K7 F15 . . 2.598(5) ? K7 F16 . 3_664 2.626(5) ? K7 F20 . 3_565 2.638(6) ? K7 F22 . 1_654 2.880(4) ? K8 F2 . 3_565 3.007(6) ? K8 F6 . 2_654 2.900(7) ? K8 F8 . 1_664 3.044(5) ? K8 F13 . . 2.622(5) ? K8 F14 . . 2.587(5) ? K8 F15 . 3_665 2.594(7) ? K8 F18 . 2_664 2.533(6) ? K8 F23 . 3_664 2.950(5) ? K9 F2 . 3_565 2.887(7) ? K9 F4 . 3_565 3.034(6) ? K9 F10 . 2_664 2.935(7) ? K9 F16 . 1_564 2.916(4) ? K9 F18 . 2_664 2.610(7) ? K9 F19 . 3_565 2.628(5) ? K9 F20 . . 2.626(5) ? K9 F21 . 3_675 2.583(6) ? K10 F1 . 2_664 2.866(8) ? K10 F3 . . 2.930(5) ? K10 F9 . 3_565 2.999(6) ? K10 F14 . 3_565 2.891(5) ? K10 F17 . . 2.560(5) ? K10 F18 . . 2.616(4) ? K10 F20 . 3_565 2.620(7) ? K10 F24 . 2_554 2.622(6) ? K11 F5 . 3_665 2.870(6) ? K11 F10 . 2_654 2.832(8) ? K11 F12 . 3_654 2.927(6) ? K11 F13 . 2_654 2.567(6) ? K11 F17 . 3_555 2.885(5) ? K11 F21 . 3_665 2.629(8) ? K11 F23 . 1_554 2.574(5) ? K11 F24 . . 2.656(5) ? K12 F6 . 2_654 3.041(7) ? K12 F9 . 3_665 2.937(7) ? K12 F11 . 3_665 2.921(6) ? K12 F15 . 3_665 2.608(6) ? K12 F19 . 1_655 2.931(4) ? K12 F21 . . 2.583(5) ? K12 F22 . 3_554 2.629(5) ? K12 F24 . 2_654 2.588(7) ? F1 F7 . 2_565 3.051(8) ? F1 F7 . 3_565 2.723(8) ? F1 F8 . 2_564 3.170(6) ? F1 F14 . 2_665 2.959(6) ? F1 F15 . 3_565 2.940(6) ? F1 F16 . 3_674 3.107(6) ? F1 F17 . 3_565 2.724(10) ? F2 F7 . 3_565 2.781(8) ? F2 F8 . 2_563 2.946(6) ? F2 F13 . 2_664 2.951(5) ? F2 F16 . 2_553 3.014(6) ? F2 F19 . . 2.799(8) ? F3 F4 . . 2.623(6) ? F3 F4 . 3_565 2.723(9) ? F3 F9 . . 3.158(8) ? F3 F9 . 3_565 2.899(6) ? F3 F17 . . 2.673(6) ? F3 F19 . . 2.771(8) ? F4 F9 . 2_664 2.800(7) ? F4 F10 . 2_664 2.725(8) ? F4 F10 . 3_564 3.043(7) ? F4 F18 . 3_564 2.820(8) ? F4 F20 . . 3.128(7) ? F5 F12 . 1_664 2.955(8) ? F5 F12 . 3_654 2.773(9) ? F5 F16 . 1_554 2.795(8) ? F5 F22 . 2_663 2.918(6) ? F5 F23 . 1_554 3.096(6) ? F5 F24 . 2_654 2.904(6) ? F6 F11 . 2_655 2.913(6) ? F6 F11 . 3_665 3.075(9) ? F6 F12 . 3_654 2.782(9) ? F6 F14 . 3_665 2.735(10) ? F6 F21 . 3_665 2.975(6) ? F6 F23 . 2_654 3.085(6) ? F6 F24 . 2_654 3.071(6) ? F7 F8 . 1_554 2.615(6) ? F7 F8 . 2_553 2.692(8) ? F7 F13 . 3_564 2.864(9) ? F7 F15 . . 3.076(6) ? F8 F14 . 1_446 2.685(6) ? F8 F16 . 1_455 2.740(8) ? F9 F18 . 2_664 2.941(5) ? F9 F19 . 2_664 3.024(6) ? F9 F20 . 3_565 3.159(6) ? F9 F22 . 1_654 2.747(8) ? F10 F17 . 2_665 2.959(6) ? F10 F19 . 3_565 3.119(6) ? F10 F20 . 3_565 2.940(6) ? F10 F23 . 3_664 2.764(10) ? F11 F12 . 1_664 2.700(7) ? F11 F12 . 3_654 2.621(9) ? F11 F22 . 1_654 2.688(8) ? F11 F23 . 1_554 2.799(7) ? F12 F21 . 1_446 2.834(6) ? F12 F24 . 3_555 3.127(9) ? F13 F17 . 2_665 2.864(8) ? F14 F16 . 2_653 2.477(7) ? F14 F24 . 3_664 2.911(6) ? F15 F19 . 2_664 2.891(8) ? F16 F21 . 3_666 2.853(8) ? F17 F19 . 2_664 2.478(7) ? F18 F23 . 2_554 2.863(7) ? F20 F22 . 2_673 2.898(8) ? F22 F23 . 3_565 2.468(6) ? 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 ? ? ? ? ? ? ? ? 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 ? ? ? ? ? ? ? ? ? ? ? #======================================================================= data_IV _database_code_depnum_ccdc_archive 'CCDC 891239' #TrackingRef '- KYF4_2.04_GPa.cif' #======================================================================= # 5. CHEMICAL DATA _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_iupac ? _chemical_formula_sum 'F4 K1 Y1' _chemical_formula_weight 306 _chemical_melting_point ? _chemical_compound_source ? _chemical_absolute_configuration ? #======================================================================= # 6. CRYSTAL DATA _symmetry_cell_setting trigonal _symmetry_space_group_name_H-M 'P 32' _symmetry_space_group_name_Hall 'P 32' _symmetry_Int_Tables_number 145 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 -y,x-y,z+2/3 3 -x+y,-x,z+1/3 _cell_length_a 14.006(2) _cell_length_b 14.006(2) _cell_length_c 10.0620(10) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 120 _cell_volume 1709.4(4) loop_ _jana_cell_twin_matrix_id _jana_cell_twin_volume_fraction _jana_cell_twin_matrix_1_1 _jana_cell_twin_matrix_1_2 _jana_cell_twin_matrix_1_3 _jana_cell_twin_matrix_2_1 _jana_cell_twin_matrix_2_2 _jana_cell_twin_matrix_2_3 _jana_cell_twin_matrix_3_1 _jana_cell_twin_matrix_3_2 _jana_cell_twin_matrix_3_3 1 0.505(3) 1 0 0 0 1 0 0 0 1 2 0 -1 0 0 0 -1 0 0 0 -1 3 0 1 -1 0 0 -1 0 0 0 -1 4 0.495(3) -1 1 0 0 1 0 0 0 -1 _cell_formula_units_Z 18 _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _cell_measurement_temperature 293 _cell_special_details ; ? ; _exptl_crystal_density_diffrn 3.5658 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_F_000 1692 _exptl_absorpt_coefficient_mu 3.624 _exptl_crystal_description ? _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.04 _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 ? #======================================================================= # 7. EXPERIMENTAL DATA _exptl_special_details ? _diffrn_ambient_temperature 293 _diffrn_source ? _diffrn_source_power ? _diffrn_source_voltage ? _diffrn_source_current ? _diffrn_radiation_type ? _diffrn_radiation_source ? _diffrn_radiation_wavelength 0.4 _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 17909 _diffrn_reflns_theta_min 1.48 _diffrn_reflns_theta_max 22.38 _diffrn_reflns_theta_full 12.9 _diffrn_measured_fraction_theta_max 0 _diffrn_measured_fraction_theta_full 0.78 _diffrn_reflns_av_R_equivalents 0.0967 _diffrn_reflns_av_sigmaI/netI 0.0385 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 17 _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 8382 _reflns_number_gt 8379 _reflns_threshold_expression I>3\s(I) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.0730 _refine_ls_wR_factor_gt 0.0724 _refine_ls_R_factor_all 0.0730 _refine_ls_wR_factor_ref 0.0724 _refine_ls_goodness_of_fit_ref 2.67 _refine_ls_goodness_of_fit_gt 2.67 _refine_ls_restrained_S_gt ? _refine_ls_restrained_S_all ? _refine_ls_number_reflns 8382 _refine_ls_number_parameters 142 _refine_ls_number_restraints 0 _refine_ls_number_constraints 65 _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 0.0394 _refine_ls_shift/su_mean 0.0074 _refine_diff_density_max 2.56 _refine_diff_density_min -3.10 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ; 8697 of Friedel pairs used in the refinement ; _refine_ls_abs_structure_Flack 0 _refine_ls_abs_structure_Rogers ? loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source F 0.0032 0.0029 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' K 0.0760 0.0798 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' Y 0.2211 1.3572 '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 ? #======================================================================= # 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_symmetry_multiplicity _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Y1 Y 0.13331(13) 0.89179(15) 0.6661(2) Uani 0.0120(3) 3 1 d . . . Y2 Y 0.28454(14) 0.73332(16) 0.6762(3) Uani 0.0125(2) 3 1 d . . . Y3 Y 0.77952(15) 0.20568(16) 0.6537(2) Uani 0.0120(3) 3 1 d . . . Y4 Y 0.94207(16) 0.0588(2) 0.6712(3) Uani 0.0125(2) 3 1 d . . . Y5 Y 0.45206(17) 0.5437(2) 0.6736(2) Uani 0.0120(3) 3 1 d . . . Y6 Y 0.60309(12) 0.38517(17) 0.6496(2) Uani 0.0125(2) 3 1 d . . . K1 K 0.2681(4) 0.2190(4) 0.6451(7) Uani 0.0174(8) 3 1 d . . . K2 K 0.7806(5) 0.7114(5) 0.6783(7) Uani 0.0255(12) 3 1 d . . . K3 K 0.6117(5) 0.8763(4) 0.6499(5) Uani 0.0174(8) 3 1 d . . . K4 K 0.1026(4) 0.3965(5) 0.6832(6) Uani 0.0255(12) 3 1 d . . . K5 K 0.4585(4) 0.0652(4) 0.6831(7) Uani 0.0255(12) 3 1 d . . . K6 K 0.9484(4) 0.5663(4) 0.6507(6) Uani 0.0174(8) 3 1 d . . . F1 F 0.1287(10) 0.9292(10) 0.8867(17) Uiso 0.0197(15) 3 1 d . . . F2 F 0.0714(9) 0.8765(10) 0.4500(15) Uiso 0.0188(14) 3 1 d . . . F3 F 0.2065(8) 0.5927(9) 0.5287(14) Uiso 0.0237(9) 3 1 d . . . F4 F 0.3331(10) 0.7304(9) 0.3428(16) Uiso 0.0255(10) 3 1 d . . . F5 F 0.7385(10) 0.1997(10) 0.4338(17) Uiso 0.0188(14) 3 1 d . . . F6 F 0.7870(9) 0.2688(9) 0.8594(15) Uiso 0.0197(15) 3 1 d . . . F7 F -0.0066(10) 0.0604(9) 0.3281(15) Uiso 0.0255(10) 3 1 d . . . F8 F 0.0789(9) -0.0449(9) 1.1897(14) Uiso 0.0237(9) 3 1 d . . . F9 F 0.3901(9) 0.5338(9) 0.4573(15) Uiso 0.0188(14) 3 1 d . . . F10 F 0.4515(10) 0.5848(10) 0.8936(16) Uiso 0.0197(15) 3 1 d . . . F11 F 0.5506(9) 0.2963(9) 0.4539(15) Uiso 0.0237(9) 3 1 d . . . F12 F -0.2600(9) -0.6058(10) 1.3053(14) Uiso 0.0255(10) 3 1 d . . . F13 F 0.7708(8) 0.7285(8) 0.9359(15) Uiso 0.0155(12) 3 1 d . . . F14 F 0.8088(8) 0.7257(8) 0.4185(14) Uiso 0.0124(9) 3 1 d . . . F15 F 0.2460(9) 0.2233(8) 0.3949(14) Uiso 0.0174(12) 3 1 d . . . F16 F 0.8171(8) 0.0827(9) 1.5560(13) Uiso 0.0164(11) 3 1 d . . . F17 F 0.1252(8) 0.3952(9) 0.4301(13) Uiso 0.0124(9) 3 1 d . . . F18 F 0.0958(7) 0.4045(8) 0.9397(12) Uiso 0.0155(12) 3 1 d . . . F19 F 0.1623(7) 0.7643(7) 0.5642(11) Uiso 0.0164(11) 3 1 d . . . F20 F 0.5913(8) 0.8848(8) 0.4024(14) Uiso 0.0174(12) 3 1 d . . . F21 F 0.9440(8) 0.5822(8) 0.3982(14) Uiso 0.0174(12) 3 1 d . . . F22 F -0.4084(10) -0.9443(9) 1.2391(14) Uiso 0.0164(11) 3 1 d . . . F23 F 0.4766(7) 0.0706(7) 1.4222(12) Uiso 0.0124(9) 3 1 d . . . F24 F 0.4599(8) 0.0894(8) 0.9446(12) Uiso 0.0155(12) 3 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 Y1 Y 0.0078(3) 0.0140(4) 0.0165(3) 0.00713(18) -0.0020(2) 0.0010(3) Y2 Y 0.0040(3) 0.0148(4) 0.0198(3) 0.00555(16) -0.0023(2) 0.0041(3) Y3 Y 0.0078(3) 0.0140(4) 0.0165(3) 0.00713(18) -0.0020(2) 0.0010(3) Y4 Y 0.0040(3) 0.0148(4) 0.0198(3) 0.00555(16) -0.0023(2) 0.0041(3) Y5 Y 0.0078(3) 0.0140(4) 0.0165(3) 0.00713(18) -0.0020(2) 0.0010(3) Y6 Y 0.0040(3) 0.0148(4) 0.0198(3) 0.00555(16) -0.0023(2) 0.0041(3) K1 K 0.0188(10) 0.0119(8) 0.0168(15) 0.0042(8) 0.0036(9) 0.0018(8) K2 K 0.0206(11) 0.0336(15) 0.029(2) 0.0189(12) -0.0083(10) -0.0129(12) K3 K 0.0188(10) 0.0119(8) 0.0168(15) 0.0042(8) 0.0036(9) 0.0018(8) K4 K 0.0206(11) 0.0336(15) 0.029(2) 0.0189(12) -0.0083(10) -0.0129(12) K5 K 0.0206(11) 0.0336(15) 0.029(2) 0.0189(12) -0.0083(10) -0.0129(12) K6 K 0.0188(10) 0.0119(8) 0.0168(15) 0.0042(8) 0.0036(9) 0.0018(8) 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 Y1 F1 . . 2.289(17) ? Y1 F2 . . 2.311(15) ? Y1 F7 . 3_565 2.223(19) ? Y1 F13 . 2_664 2.125(11) ? Y1 F15 . 3_565 2.163(11) ? Y1 F17 . 3_565 2.266(17) ? Y1 F19 . . 2.265(12) ? Y2 F3 . . 2.264(12) ? Y2 F3 . 3_565 2.243(14) ? Y2 F4 . 3_565 2.20(2) ? Y2 F9 . 3_565 2.190(13) ? Y2 F10 . 2_664 2.187(13) ? Y2 F17 . 3_565 2.268(15) ? Y2 F19 . . 2.265(12) ? Y3 F5 . . 2.277(17) ? Y3 F6 . . 2.233(15) ? Y3 F12 . 3_654 2.24(2) ? Y3 F14 . 3_665 2.259(17) ? Y3 F16 . 1_554 2.262(14) ? Y3 F21 . 3_665 2.185(11) ? Y3 F24 . 2_654 2.155(11) ? Y4 F1 . 2_764 2.233(14) ? Y4 F2 . 3_555 2.187(13) ? Y4 F7 . 3_655 2.21(2) ? Y4 F8 . 2_654 2.249(13) ? Y4 F8 . 3_654 2.240(13) ? Y4 F14 . 3_665 2.208(16) ? Y4 F16 . 1_554 2.260(14) ? Y5 F4 . 3_565 2.21(2) ? Y5 F9 . . 2.322(15) ? Y5 F10 . . 2.288(16) ? Y5 F18 . 2_664 2.148(10) ? Y5 F20 . 3_565 2.168(11) ? Y5 F22 . 3_654 2.230(17) ? Y5 F23 . 3_664 2.297(15) ? Y6 F5 . 3_665 2.215(14) ? Y6 F6 . 2_654 2.212(13) ? Y6 F11 . . 2.247(14) ? Y6 F11 . 3_665 2.218(16) ? Y6 F12 . 3_654 2.203(19) ? Y6 F22 . 3_654 2.266(19) ? Y6 F23 . 3_664 2.268(13) ? K1 F1 . 2_664 2.794(17) ? K1 F5 . 3_665 2.75(2) ? K1 F7 . 3_555 2.903(12) ? K1 F13 . 2_654 2.535(18) ? K1 F15 . . 2.541(15) ? K1 F16 . 3_664 2.505(15) ? K1 F20 . 3_565 2.659(14) ? K1 F22 . 3_654 2.797(12) ? K2 F2 . 3_565 3.073(17) ? K2 F6 . 2_654 2.877(18) ? K2 F8 . 3_664 2.987(14) ? K2 F13 . . 2.613(16) ? K2 F14 . . 2.637(15) ? K2 F15 . 3_665 2.560(17) ? K2 F18 . 2_664 2.568(14) ? K2 F23 . 3_664 2.737(10) ? K3 F2 . 3_565 2.773(19) ? K3 F4 . 3_565 2.980(13) ? K3 F10 . 2_664 2.835(18) ? K3 F16 . 1_564 3.034(10) ? K3 F18 . 2_664 2.524(17) ? K3 F19 . 3_565 2.539(12) ? K3 F20 . . 2.516(15) ? K3 F21 . 3_675 2.492(14) ? K4 F1 . 2_664 2.88(2) ? K4 F3 . . 2.843(13) ? K4 F9 . 3_565 2.952(16) ? K4 F14 . 3_565 2.835(11) ? K4 F17 . . 2.567(14) ? K4 F18 . . 2.587(13) ? K4 F20 . 3_565 2.645(18) ? K4 F24 . 2_554 2.629(14) ? K5 F5 . 3_665 2.858(18) ? K5 F10 . 2_654 2.82(2) ? K5 F12 . 3_654 2.770(13) ? K5 F13 . 2_654 2.604(15) ? K5 F17 . 3_555 2.774(11) ? K5 F21 . 3_665 2.630(19) ? K5 F23 . 1_554 2.635(14) ? K5 F24 . . 2.652(14) ? K6 F6 . 2_654 3.038(15) ? K6 F9 . 3_665 2.858(18) ? K6 F11 . 3_665 2.825(15) ? K6 F15 . 3_665 2.572(14) ? K6 F19 . 1_655 3.019(9) ? K6 F21 . . 2.554(15) ? K6 F22 . 2_554 2.597(16) ? K6 F24 . 2_654 2.551(17) ? F1 F7 . 2_565 2.89(2) ? F1 F7 . 3_565 2.83(2) ? F1 F8 . 1_565 3.19(2) ? F1 F14 . 2_665 2.898(18) ? F1 F15 . 3_565 2.803(17) ? F1 F16 . 3_674 3.081(15) ? F1 F17 . 3_565 2.75(2) ? F2 F7 . 3_565 2.82(2) ? F2 F8 . 1_564 2.82(2) ? F2 F8 . 3_564 3.18(2) ? F2 F13 . 2_664 3.015(16) ? F2 F16 . 2_553 3.092(18) ? F2 F19 . . 2.72(2) ? F3 F4 . . 2.635(18) ? F3 F4 . 3_565 2.77(2) ? F3 F9 . . 3.15(2) ? F3 F9 . 3_565 2.83(2) ? F3 F10 . 3_564 3.17(2) ? F3 F17 . . 2.604(17) ? F3 F19 . . 2.789(18) ? F4 F9 . 2_664 2.854(19) ? F4 F10 . 2_664 2.75(2) ? F4 F10 . 3_564 2.924(17) ? F4 F18 . 3_564 2.71(2) ? F5 F12 . 1_664 3.01(2) ? F5 F12 . 3_654 2.71(2) ? F5 F16 . 1_554 2.69(2) ? F5 F22 . 1_664 2.826(18) ? F5 F23 . 1_554 3.179(15) ? F5 F24 . 2_654 2.992(16) ? F6 F11 . 2_655 2.84(2) ? F6 F11 . 3_665 2.95(2) ? F6 F12 . 3_654 2.86(2) ? F6 F14 . 3_665 2.76(2) ? F6 F21 . 3_665 2.944(15) ? F6 F23 . 2_654 3.028(17) ? F6 F24 . 2_654 2.965(18) ? F7 F8 . 1_554 2.71(2) ? F7 F8 . 3_554 2.674(18) ? F7 F13 . 3_564 2.71(2) ? F7 F15 . . 3.179(14) ? F8 F14 . 2_655 2.628(15) ? F8 F16 . 2_544 2.792(16) ? F9 F18 . 2_664 3.007(15) ? F9 F19 . 2_664 3.062(16) ? F9 F22 . 3_654 2.71(2) ? F10 F17 . 2_665 2.926(18) ? F10 F19 . 3_565 3.086(14) ? F10 F20 . 3_565 2.837(16) ? F10 F23 . 3_664 2.89(2) ? F11 F12 . 1_664 2.741(17) ? F11 F12 . 3_654 2.56(2) ? F11 F22 . 3_654 2.69(2) ? F11 F23 . 1_554 2.810(16) ? F12 F21 . 1_446 2.906(14) ? F12 F24 . 3_555 3.13(2) ? F13 F17 . 2_665 2.84(2) ? F14 F16 . 2_653 2.453(19) ? F14 F24 . 3_664 2.922(14) ? F15 F19 . 2_664 3.015(19) ? F16 F21 . 3_666 2.93(2) ? F17 F19 . 2_664 2.522(17) ? F18 F23 . 2_554 2.782(17) ? F20 F22 . 1_674 2.901(19) ? F22 F23 . 1_445 2.523(19) ? 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 ? ? ? ? ? ? ? ? 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 ? ? ? ? ? ? ? ? ? ? ? #======================================================================= data_V _database_code_depnum_ccdc_archive 'CCDC 891240' #TrackingRef '- KYF4_AP_final.cif' #======================================================================= # 5. CHEMICAL DATA _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_iupac ? _chemical_formula_sum 'F4 K1 Y1' _chemical_formula_weight 306 _chemical_melting_point ? _chemical_compound_source ? _chemical_absolute_configuration ? #======================================================================= # 6. CRYSTAL DATA _symmetry_cell_setting trigonal _symmetry_space_group_name_H-M 'P 32' _symmetry_space_group_name_Hall 'P 32' _symmetry_Int_Tables_number 145 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 -y,x-y,z+2/3 3 -x+y,-x,z+1/3 _cell_length_a 14.1630(10) _cell_length_b 14.1630(10) _cell_length_c 10.1900(10) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 120 _cell_volume 1770.2(2) loop_ _jana_cell_twin_matrix_id _jana_cell_twin_volume_fraction _jana_cell_twin_matrix_1_1 _jana_cell_twin_matrix_1_2 _jana_cell_twin_matrix_1_3 _jana_cell_twin_matrix_2_1 _jana_cell_twin_matrix_2_2 _jana_cell_twin_matrix_2_3 _jana_cell_twin_matrix_3_1 _jana_cell_twin_matrix_3_2 _jana_cell_twin_matrix_3_3 1 0.4999(10) 1 0 0 0 1 0 0 0 1 2 0 -1 0 0 0 -1 0 0 0 -1 3 0 1 -1 0 0 -1 0 0 0 -1 4 0.5001(10) -1 1 0 0 1 0 0 0 -1 _cell_formula_units_Z 18 _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _cell_measurement_temperature 293 _cell_special_details ; ? ; _exptl_crystal_density_diffrn 3.4434 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_F_000 1692 _exptl_absorpt_coefficient_mu 3.5 _exptl_crystal_description ? _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.04 _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 ? #======================================================================= # 7. EXPERIMENTAL DATA _exptl_special_details ? _diffrn_ambient_temperature 293 _diffrn_source ? _diffrn_source_power ? _diffrn_source_voltage ? _diffrn_source_current ? _diffrn_radiation_type ? _diffrn_radiation_source ? _diffrn_radiation_wavelength 0.4 _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 138252 _diffrn_reflns_theta_min 0.94 _diffrn_reflns_theta_max 26.15 _diffrn_reflns_theta_full 26.14 _diffrn_measured_fraction_theta_max 0 _diffrn_measured_fraction_theta_full 0.99 _diffrn_reflns_av_R_equivalents 0.049 _diffrn_reflns_av_sigmaI/netI 0.0551 _diffrn_reflns_limit_h_min -31 _diffrn_reflns_limit_h_max 31 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 21 _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 25527 _reflns_number_gt 23445 _reflns_threshold_expression I>3\s(I) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.0306 _refine_ls_wR_factor_gt 0.0400 _refine_ls_R_factor_all 0.0361 _refine_ls_wR_factor_ref 0.0409 _refine_ls_goodness_of_fit_ref 1.19 _refine_ls_goodness_of_fit_gt 1.21 _refine_ls_restrained_S_gt ? _refine_ls_restrained_S_all ? _refine_ls_number_reflns 25527 _refine_ls_number_parameters 231 _refine_ls_number_restraints 0 _refine_ls_number_constraints 97 _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 0.0349 _refine_ls_shift/su_mean 0.0058 _refine_diff_density_max 0.55 _refine_diff_density_min -0.59 _refine_ls_extinction_method 'B-C type 1 Gaussian isotropic (Becker & Coppens, 1974)' _refine_ls_extinction_coef 11400(700) _refine_ls_abs_structure_details ; 24869 of Friedel pairs used in the refinement ; _refine_ls_abs_structure_Flack 0 _refine_ls_abs_structure_Rogers ? loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source F 0.0032 0.0029 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' K 0.0760 0.0798 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' Y 0.2211 1.3572 '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 ? #======================================================================= # 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_symmetry_multiplicity _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Y1 Y 0.13055(3) 0.89040(3) 0.66619(4) Uani 0.00575(7) 3 1 d . . . Y2 Y 0.28078(4) 0.73037(4) 0.67411(5) Uani 0.00745(10) 3 1 d . . . Y3 Y 0.78105(4) 0.20748(4) 0.65710(4) Uani 0.00633(8) 3 1 d . . . Y4 Y 0.94103(4) 0.05768(4) 0.66979(6) Uani 0.00663(8) 3 1 d . . . Y5 Y 0.45274(4) 0.54494(5) 0.67143(4) Uani 0.00674(8) 3 1 d . . . Y6 Y 0.60289(3) 0.38552(4) 0.65198(3) Uani 0.00522(7) 3 1 d . . . K1 K 0.26672(10) 0.21929(11) 0.64643(12) Uani 0.0158(3) 3 1 d . . . K2 K 0.78083(12) 0.71936(12) 0.67589(13) Uani 0.0202(4) 3 1 d . . . K3 K 0.61130(12) 0.87785(10) 0.65016(11) Uani 0.0180(3) 3 1 d . . . K4 K 0.10466(11) 0.39538(12) 0.67984(12) Uani 0.0167(3) 3 1 d . . . K5 K 0.45608(9) 0.06437(9) 0.68040(11) Uani 0.0151(3) 3 1 d . . . K6 K 0.94765(11) 0.56221(12) 0.65014(11) Uani 0.0182(3) 3 1 d . . . F1 F 0.1309(2) 0.9354(2) 0.8839(2) Uani 0.0152(5) 3 1 d . . . F2 F 0.0702(2) 0.8784(2) 0.4569(2) Uani 0.0176(6) 3 1 d . . . F3 F 0.20735(19) 0.59552(19) 0.5238(3) Uani 0.0199(3) 3 1 d . . . F4 F 0.3388(3) 0.72858(17) 0.3409(3) Uani 0.0296(4) 3 1 d . . . F5 F 0.7377(2) 0.2036(2) 0.4403(3) Uani 0.0176(6) 3 1 d . . . F6 F 0.78924(19) 0.2701(2) 0.8667(3) Uani 0.0152(5) 3 1 d . . . F7 F -0.0014(3) 0.05974(17) 0.3346(3) Uani 0.0296(4) 3 1 d . . . F8 F 0.0761(2) -0.04768(18) 1.1866(3) Uani 0.0199(3) 3 1 d . . . F9 F 0.3917(2) 0.5369(2) 0.4623(2) Uani 0.0176(6) 3 1 d . . . F10 F 0.4571(2) 0.5913(2) 0.8881(2) Uani 0.0152(5) 3 1 d . . . F11 F 0.54783(19) 0.29041(19) 0.4623(3) Uani 0.0199(3) 3 1 d . . . F12 F -0.2663(2) -0.60517(18) 1.3190(4) Uani 0.0296(4) 3 1 d . . . F13 F 0.7667(2) 0.72828(18) 0.9313(3) Uani 0.0159(4) 3 1 d . . . F14 F 0.8094(2) 0.72448(15) 0.4231(3) Uani 0.0156(4) 3 1 d . . . F15 F 0.24799(17) 0.22319(18) 0.3903(3) Uani 0.0152(4) 3 1 d . . . F16 F 0.8089(2) 0.0749(2) 1.5653(3) Uani 0.0144(4) 3 1 d . . . F17 F 0.13261(19) 0.39378(16) 0.4279(2) Uani 0.0156(4) 3 1 d . . . F18 F 0.09371(19) 0.40422(19) 0.9355(2) Uani 0.0159(4) 3 1 d . . . F19 F 0.15200(18) 0.75538(18) 0.5735(2) Uani 0.0144(4) 3 1 d . . . F20 F 0.59000(17) 0.88469(18) 0.3935(2) Uani 0.0152(4) 3 1 d . . . F21 F 0.93653(19) 0.5753(2) 0.3960(3) Uani 0.0152(4) 3 1 d . . . F22 F -0.4102(2) -0.94313(19) 1.2380(2) Uani 0.0144(4) 3 1 d . . . F23 F 0.4854(2) 0.06895(16) 1.4277(2) Uani 0.0156(4) 3 1 d . . . F24 F 0.4524(2) 0.08634(19) 0.9383(3) Uani 0.0159(4) 3 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 Y1 Y 0.00519(8) 0.00669(9) 0.00674(10) 0.00399(8) -0.00005(8) -0.00017(8) Y2 Y 0.00810(12) 0.00733(11) 0.00923(16) 0.00559(9) 0.00291(9) 0.00259(8) Y3 Y 0.00652(10) 0.00749(10) 0.00654(11) 0.00468(9) -0.00015(8) -0.00014(9) Y4 Y 0.00633(9) 0.00652(10) 0.00799(13) 0.00393(7) 0.00168(8) 0.00142(8) Y5 Y 0.00703(10) 0.00929(11) 0.00657(10) 0.00609(9) -0.00016(8) -0.00031(8) Y6 Y 0.00477(8) 0.00508(8) 0.00640(8) 0.00289(8) -0.00084(7) -0.00120(7) K1 K 0.0237(4) 0.0133(3) 0.0110(3) 0.0096(3) -0.0039(3) -0.0022(3) K2 K 0.0163(4) 0.0313(7) 0.0142(4) 0.0128(5) -0.0024(4) -0.0062(4) K3 K 0.0325(5) 0.0120(4) 0.0100(3) 0.0115(4) -0.0021(4) -0.0019(2) K4 K 0.0168(4) 0.0217(4) 0.0124(3) 0.0102(4) -0.0010(3) -0.0006(3) K5 K 0.0140(4) 0.0149(3) 0.0155(3) 0.0065(2) 0.0002(2) -0.0050(3) K6 K 0.0284(5) 0.0133(4) 0.0118(3) 0.0095(3) -0.0020(3) -0.0006(3) F1 F 0.0182(7) 0.0170(6) 0.0110(5) 0.0092(5) -0.0005(4) -0.0055(4) F2 F 0.0222(7) 0.0275(9) 0.0118(6) 0.0189(7) -0.0078(5) -0.0014(5) F3 F 0.0216(4) 0.0188(4) 0.0189(4) 0.0096(4) 0.0042(4) -0.0047(4) F4 F 0.0333(7) 0.0041(2) 0.0429(6) 0.0029(5) 0.0004(5) -0.0006(7) F5 F 0.0222(7) 0.0275(9) 0.0118(6) 0.0189(7) -0.0078(5) -0.0014(5) F6 F 0.0182(7) 0.0170(6) 0.0110(5) 0.0092(5) -0.0005(4) -0.0055(4) F7 F 0.0333(7) 0.0041(2) 0.0429(6) 0.0029(5) 0.0004(5) -0.0006(7) F8 F 0.0216(4) 0.0188(4) 0.0189(4) 0.0096(4) 0.0042(4) -0.0047(4) F9 F 0.0222(7) 0.0275(9) 0.0118(6) 0.0189(7) -0.0078(5) -0.0014(5) F10 F 0.0182(7) 0.0170(6) 0.0110(5) 0.0092(5) -0.0005(4) -0.0055(4) F11 F 0.0216(4) 0.0188(4) 0.0189(4) 0.0096(4) 0.0042(4) -0.0047(4) F12 F 0.0333(7) 0.0041(2) 0.0429(6) 0.0029(5) 0.0004(5) -0.0006(7) F13 F 0.0186(5) 0.0132(5) 0.0165(6) 0.0084(4) 0.0025(4) -0.0001(4) F14 F 0.0227(6) 0.0018(3) 0.0164(6) 0.0016(3) 0.0120(4) -0.0016(3) F15 F 0.0128(5) 0.0177(5) 0.0186(6) 0.0101(4) -0.0010(4) 0.0025(4) F16 F 0.0184(5) 0.0163(5) 0.0114(5) 0.0108(4) -0.0038(3) -0.0030(3) F17 F 0.0227(6) 0.0018(3) 0.0164(6) 0.0016(3) 0.0120(4) -0.0016(3) F18 F 0.0186(5) 0.0132(5) 0.0165(6) 0.0084(4) 0.0025(4) -0.0001(4) F19 F 0.0184(5) 0.0163(5) 0.0114(5) 0.0108(4) -0.0038(3) -0.0030(3) F20 F 0.0128(5) 0.0177(5) 0.0186(6) 0.0101(4) -0.0010(4) 0.0025(4) F21 F 0.0128(5) 0.0177(5) 0.0186(6) 0.0101(4) -0.0010(4) 0.0025(4) F22 F 0.0184(5) 0.0163(5) 0.0114(5) 0.0108(4) -0.0038(3) -0.0030(3) F23 F 0.0227(6) 0.0018(3) 0.0164(6) 0.0016(3) 0.0120(4) -0.0016(3) F24 F 0.0186(5) 0.0132(5) 0.0165(6) 0.0084(4) 0.0025(4) -0.0001(4) 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 Y1 F1 . . 2.307(2) ? Y1 F2 . . 2.273(3) ? Y1 F7 . 3_565 2.232(5) ? Y1 F13 . 2_664 2.164(2) ? Y1 F15 . 3_565 2.171(2) ? Y1 F17 . 3_565 2.252(4) ? Y1 F19 . . 2.285(3) ? Y2 F3 . . 2.256(3) ? Y2 F3 . 3_565 2.286(3) ? Y2 F4 . 3_565 2.203(5) ? Y2 F9 . 3_565 2.212(3) ? Y2 F10 . 2_664 2.228(3) ? Y2 F17 . 3_565 2.274(3) ? Y2 F19 . . 2.269(3) ? Y3 F5 . . 2.286(3) ? Y3 F6 . . 2.293(3) ? Y3 F12 . 3_654 2.235(5) ? Y3 F14 . 3_665 2.267(4) ? Y3 F16 . 1_554 2.302(3) ? Y3 F21 . 3_665 2.157(2) ? Y3 F24 . 2_654 2.153(3) ? Y4 F1 . 2_764 2.221(3) ? Y4 F2 . 3_555 2.217(3) ? Y4 F7 . 3_655 2.210(5) ? Y4 F8 . 2_654 2.289(2) ? Y4 F8 . 3_654 2.242(3) ? Y4 F14 . 3_665 2.270(4) ? Y4 F16 . 1_554 2.270(3) ? Y5 F4 . 3_565 2.231(5) ? Y5 F9 . . 2.281(3) ? Y5 F10 . . 2.295(3) ? Y5 F18 . 2_664 2.155(2) ? Y5 F20 . 3_565 2.169(2) ? Y5 F22 . 3_654 2.260(4) ? Y5 F23 . 3_664 2.291(4) ? Y6 F5 . 3_665 2.227(3) ? Y6 F6 . 2_654 2.207(3) ? Y6 F11 . . 2.260(3) ? Y6 F11 . 3_665 2.254(3) ? Y6 F12 . 3_654 2.219(4) ? Y6 F22 . 3_654 2.274(4) ? Y6 F23 . 3_664 2.270(3) ? K1 F1 . 2_664 2.880(4) ? K1 F5 . 3_665 2.879(5) ? K1 F7 . 3_555 3.011(3) ? K1 F13 . 2_654 2.645(4) ? K1 F15 . . 2.627(3) ? K1 F16 . 3_664 2.600(3) ? K1 F20 . 3_565 2.656(3) ? K1 F22 . 3_654 2.877(3) ? K2 F2 . 3_565 3.039(4) ? K2 F6 . 2_654 2.937(4) ? K2 F8 . 3_664 2.971(3) ? K2 F13 . . 2.618(3) ? K2 F14 . . 2.603(3) ? K2 F15 . 3_665 2.599(4) ? K2 F18 . 2_664 2.550(3) ? K2 F23 . 3_664 2.978(3) ? K3 F2 . 3_565 2.882(4) ? K3 F4 . 3_565 3.113(3) ? K3 F10 . 2_664 2.953(4) ? K3 F16 . 1_564 2.925(3) ? K3 F18 . 2_664 2.611(4) ? K3 F19 . 3_565 2.643(3) ? K3 F20 . . 2.640(3) ? K3 F21 . 3_675 2.587(3) ? K4 F1 . 2_664 2.910(4) ? K4 F3 . . 2.925(3) ? K4 F9 . 3_565 3.013(4) ? K4 F14 . 3_565 2.905(3) ? K4 F17 . . 2.599(3) ? K4 F18 . . 2.617(3) ? K4 F20 . 3_565 2.638(4) ? K4 F24 . 2_554 2.636(3) ? K5 F5 . 3_665 2.896(4) ? K5 F10 . 2_654 2.849(4) ? K5 F12 . 3_654 2.896(3) ? K5 F13 . 2_654 2.588(3) ? K5 F17 . 3_555 2.895(2) ? K5 F21 . 3_665 2.642(4) ? K5 F23 . 1_554 2.604(3) ? K5 F24 . . 2.650(3) ? K6 F6 . 2_654 3.069(3) ? K6 F9 . 3_665 2.937(4) ? K6 F11 . 3_665 2.922(3) ? K6 F15 . 3_665 2.625(3) ? K6 F19 . 1_655 2.924(2) ? K6 F21 . . 2.606(3) ? K6 F22 . 2_554 2.622(3) ? K6 F24 . 2_654 2.612(4) ? F1 F7 . 2_565 2.975(5) ? F1 F7 . 3_565 2.760(5) ? F1 F14 . 2_665 2.957(3) ? F1 F15 . 3_565 2.924(3) ? F1 F16 . 3_674 3.142(4) ? F1 F17 . 3_565 2.770(5) ? F2 F7 . 3_565 2.810(5) ? F2 F8 . 1_564 2.933(4) ? F2 F8 . 3_564 3.185(6) ? F2 F13 . 2_664 2.981(3) ? F2 F15 . 3_565 3.161(4) ? F2 F16 . 2_553 3.074(4) ? F2 F19 . . 2.795(5) ? F3 F4 . . 2.642(4) ? F3 F4 . 3_565 2.736(5) ? F3 F9 . . 3.173(5) ? F3 F9 . 3_565 2.939(4) ? F3 F17 . . 2.686(3) ? F3 F19 . . 2.788(4) ? F4 F9 . 2_664 2.795(4) ? F4 F10 . 2_664 2.753(4) ? F4 F10 . 3_564 3.028(4) ? F4 F18 . 3_564 2.836(5) ? F4 F20 . . 3.157(4) ? F5 F12 . 1_664 3.003(5) ? F5 F12 . 3_654 2.756(5) ? F5 F16 . 1_554 2.793(5) ? F5 F22 . 1_664 2.933(3) ? F5 F23 . 1_554 3.100(4) ? F5 F24 . 2_654 2.930(3) ? F6 F11 . 2_655 2.871(4) ? F6 F11 . 3_665 3.051(5) ? F6 F12 . 3_654 2.823(5) ? F6 F14 . 3_665 2.778(5) ? F6 F21 . 3_665 2.971(3) ? F6 F23 . 2_654 3.090(3) ? F6 F24 . 2_654 3.109(4) ? F7 F8 . 1_554 2.731(5) ? F7 F8 . 3_554 2.634(4) ? F7 F13 . 3_564 2.849(5) ? F7 F15 . . 3.159(3) ? F8 F14 . 2_655 2.678(3) ? F8 F16 . 2_544 2.781(4) ? F9 F18 . 2_664 2.968(3) ? F9 F19 . 2_664 3.045(3) ? F9 F20 . 3_565 3.149(3) ? F9 F22 . 3_654 2.740(6) ? F10 F17 . 2_665 2.974(3) ? F10 F19 . 3_565 3.164(3) ? F10 F20 . 3_565 2.946(3) ? F10 F23 . 3_664 2.831(5) ? F11 F12 . 1_664 2.712(4) ? F11 F12 . 3_654 2.644(5) ? F11 F22 . 3_654 2.713(5) ? F11 F23 . 1_554 2.823(4) ? F12 F21 . 1_446 2.839(3) ? F12 F24 . 3_555 3.157(5) ? F13 F17 . 2_665 2.880(4) ? F14 F16 . 2_653 2.506(4) ? F14 F24 . 3_664 2.934(3) ? F15 F19 . 2_664 2.914(4) ? F16 F21 . 3_666 2.870(5) ? F17 F19 . 2_664 2.473(4) ? F18 F23 . 2_554 2.891(4) ? F20 F22 . 1_674 2.909(4) ? F22 F23 . 1_445 2.491(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 ? ? ? ? ? ? ? ? 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 ? ? ? ? ? ? ? ? ? ? ? #======================================================================= data_VI _database_code_depnum_ccdc_archive 'CCDC 891241' #TrackingRef '- KYbF4_3.98_GPa.cif' #======================================================================= # 5. CHEMICAL DATA _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_iupac ? _chemical_formula_sum 'F4 K1 Yb1' _chemical_formula_weight 432.2 _chemical_melting_point ? _chemical_compound_source ? _chemical_absolute_configuration ? #======================================================================= # 6. CRYSTAL DATA _symmetry_cell_setting trigonal _symmetry_space_group_name_H-M 'P 32' _symmetry_space_group_name_Hall 'P 32' _symmetry_Int_Tables_number 145 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 -y,x-y,z+2/3 3 -x+y,-x,z+1/3 _cell_length_a 13.754(3) _cell_length_b 13.754(3) _cell_length_c 9.891(2) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 120 _cell_volume 1620.4(6) loop_ _jana_cell_twin_matrix_id _jana_cell_twin_volume_fraction _jana_cell_twin_matrix_1_1 _jana_cell_twin_matrix_1_2 _jana_cell_twin_matrix_1_3 _jana_cell_twin_matrix_2_1 _jana_cell_twin_matrix_2_2 _jana_cell_twin_matrix_2_3 _jana_cell_twin_matrix_3_1 _jana_cell_twin_matrix_3_2 _jana_cell_twin_matrix_3_3 1 0.498(3) 1 0 0 0 1 0 0 0 1 2 0 -1 0 0 0 -1 0 0 0 -1 3 0 1 -1 0 0 -1 0 0 0 -1 4 0.502(3) -1 1 0 0 1 0 0 0 -1 _cell_formula_units_Z 18 _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _cell_measurement_temperature 293 _cell_special_details ; ? ; _exptl_crystal_density_diffrn 5.313 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_F_000 2250 _exptl_absorpt_coefficient_mu 5.956 _exptl_crystal_description ? _exptl_crystal_size_max 0.09 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.04 _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 ? #======================================================================= # 7. EXPERIMENTAL DATA _exptl_special_details ? _diffrn_ambient_temperature 293 _diffrn_source ? _diffrn_source_power ? _diffrn_source_voltage ? _diffrn_source_current ? _diffrn_radiation_type ? _diffrn_radiation_source ? _diffrn_radiation_wavelength 0.4 _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 25800 _diffrn_reflns_theta_min 1.51 _diffrn_reflns_theta_max 22.39 _diffrn_reflns_theta_full 16.65 _diffrn_measured_fraction_theta_max 0 _diffrn_measured_fraction_theta_full 0.85 _diffrn_reflns_av_R_equivalents 0.0917 _diffrn_reflns_av_sigmaI/netI 0.0319 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 11 _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 9785 _reflns_number_gt 9785 _reflns_threshold_expression I>3\s(I) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.0828 _refine_ls_wR_factor_gt 0.0862 _refine_ls_R_factor_all 0.0828 _refine_ls_wR_factor_ref 0.0862 _refine_ls_goodness_of_fit_ref 3.81 _refine_ls_goodness_of_fit_gt 3.81 _refine_ls_restrained_S_gt ? _refine_ls_restrained_S_all ? _refine_ls_number_reflns 9785 _refine_ls_number_parameters 143 _refine_ls_number_restraints 0 _refine_ls_number_constraints 1 _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 0.0478 _refine_ls_shift/su_mean 0.0065 _refine_diff_density_max 11.57 _refine_diff_density_min -7.34 _refine_ls_extinction_method 'B-C type 1 Gaussian isotropic (Becker & Coppens, 1974)' _refine_ls_extinction_coef 1400(300) _refine_ls_abs_structure_details ; 9686 of Friedel pairs used in the refinement ; _refine_ls_abs_structure_Flack 0 _refine_ls_abs_structure_Rogers ? loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source F 0.0032 0.0029 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' K 0.0760 0.0798 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' Yb -0.6177 2.1062 '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 ? #======================================================================= # 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_symmetry_multiplicity _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Yb1 Yb 0.13433(12) 0.89287(13) 0.6710(2) Uani 0.0121(2) 3 1 d . . . Yb2 Yb 0.28475(16) 0.73326(14) 0.6809(2) Uani 0.0125(2) 3 1 d . . . Yb3 Yb 0.77966(18) 0.20538(15) 0.65941(18) Uani 0.0121(2) 3 1 d . . . Yb4 Yb 0.94283(17) 0.05946(19) 0.6763(3) Uani 0.0125(2) 3 1 d . . . Yb5 Yb 0.45111(19) 0.5417(2) 0.67879(18) Uani 0.0121(2) 3 1 d . . . Yb6 Yb 0.60383(13) 0.38564(16) 0.65423(16) Uani 0.0125(2) 3 1 d . . . K1 K 0.2653(8) 0.2183(7) 0.6523(13) Uani 0.027(2) 3 1 d . . . K2 K 0.7829(7) 0.7152(7) 0.6807(9) Uani 0.0181(14) 3 1 d . . . K3 K 0.6122(10) 0.8752(7) 0.6507(11) Uani 0.027(2) 3 1 d . . . K4 K 0.1056(6) 0.3982(7) 0.6909(9) Uani 0.0181(14) 3 1 d . . . K5 K 0.4586(7) 0.0656(6) 0.6892(9) Uani 0.0181(14) 3 1 d . . . K6 K 0.9516(9) 0.5702(6) 0.6555(10) Uani 0.027(2) 3 1 d . . . F1 F 0.1361(13) 0.9343(12) 0.8961(17) Uiso 0.0118(16) 3 1 d . . . F2 F 0.068(2) 0.877(2) 0.466(3) Uiso 0.032(3) 3 1 d . . . F3 F 0.2038(14) 0.5934(14) 0.537(2) Uiso 0.0231(17) 3 1 d . . . F4 F 0.3352(18) 0.7318(17) 0.347(3) Uiso 0.0290(17) 3 1 d . . . F5 F 0.750(2) 0.211(2) 0.443(3) Uiso 0.032(3) 3 1 d . . . F6 F 0.7839(12) 0.2650(13) 0.873(2) Uiso 0.0118(16) 3 1 d . . . F7 F -0.0105(18) 0.0584(16) 0.341(3) Uiso 0.0290(17) 3 1 d . . . F8 F -0.1237(14) -0.0765(14) 1.526(2) Uiso 0.0231(17) 3 1 d . . . F9 F 0.3881(18) 0.5320(18) 0.470(3) Uiso 0.032(3) 3 1 d . . . F10 F 0.4597(15) 0.5890(13) 0.8981(19) Uiso 0.0118(16) 3 1 d . . . F11 F 0.5482(14) 0.2997(14) 0.452(2) Uiso 0.0231(17) 3 1 d . . . F12 F -0.2601(17) -0.6055(19) 1.314(3) Uiso 0.0290(17) 3 1 d . . . F13 F 0.7702(16) 0.7268(13) 0.943(2) Uiso 0.0185(19) 3 1 d . . . F14 F 0.7999(14) 0.7213(14) 0.416(2) Uiso 0.0172(17) 3 1 d . . . F15 F 0.2463(13) 0.2225(12) 0.398(2) Uiso 0.0161(18) 3 1 d . . . F16 F 0.8053(14) 0.0696(15) 1.572(2) Uiso 0.0139(16) 3 1 d . . . F17 F 0.1232(13) 0.3959(17) 0.425(2) Uiso 0.0172(17) 3 1 d . . . F18 F 0.0901(13) 0.4034(15) 0.9489(18) Uiso 0.0185(19) 3 1 d . . . F19 F 0.1534(13) 0.7531(14) 0.5748(19) Uiso 0.0139(16) 3 1 d . . . F20 F 0.5921(13) 0.8853(13) 0.3986(19) Uiso 0.0161(18) 3 1 d . . . F21 F 0.9430(14) 0.5837(15) 0.406(2) Uiso 0.0161(18) 3 1 d . . . F22 F -0.5286(13) 0.4121(13) 1.5645(18) Uiso 0.0139(16) 3 1 d . . . F23 F 0.4913(15) 0.0706(15) 1.436(2) Uiso 0.0172(17) 3 1 d . . . F24 F 0.4612(14) 0.0895(14) 0.947(2) Uiso 0.0185(19) 3 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 Yb1 Yb 0.0105(3) 0.0101(3) 0.0171(2) 0.00627(15) -0.0004(2) 0.0009(2) Yb2 Yb 0.0065(3) 0.0126(3) 0.0199(2) 0.00588(14) 0.0030(2) -0.0010(2) Yb3 Yb 0.0105(3) 0.0101(3) 0.0171(2) 0.00627(15) -0.0004(2) 0.0009(2) Yb4 Yb 0.0065(3) 0.0126(3) 0.0199(2) 0.00588(14) 0.0030(2) -0.0010(2) Yb5 Yb 0.0105(3) 0.0101(3) 0.0171(2) 0.00627(15) -0.0004(2) 0.0009(2) Yb6 Yb 0.0065(3) 0.0126(3) 0.0199(2) 0.00588(14) 0.0030(2) -0.0010(2) K1 K 0.039(3) 0.0114(14) 0.027(3) 0.0108(19) -0.007(2) -0.0032(15) K2 K 0.0154(16) 0.0170(17) 0.020(2) 0.0068(14) -0.0026(12) -0.0035(14) K3 K 0.039(3) 0.0114(14) 0.027(3) 0.0108(19) -0.007(2) -0.0032(15) K4 K 0.0154(16) 0.0170(17) 0.020(2) 0.0068(14) -0.0026(12) -0.0035(14) K5 K 0.0154(16) 0.0170(17) 0.020(2) 0.0068(14) -0.0026(12) -0.0035(14) K6 K 0.039(3) 0.0114(14) 0.027(3) 0.0108(19) -0.007(2) -0.0032(15) 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 Yb1 F1 . . 2.296(17) ? Yb1 F2 . . 2.19(3) ? Yb1 F7 . 3_565 2.21(3) ? Yb1 F13 . 2_664 2.086(18) ? Yb1 F15 . 3_565 2.141(17) ? Yb1 F17 . 3_565 2.20(3) ? Yb1 F19 . . 2.27(2) ? Yb2 F3 . . 2.193(18) ? Yb2 F3 . 3_565 2.26(2) ? Yb2 F4 . 3_565 2.17(4) ? Yb2 F9 . 3_565 2.19(2) ? Yb2 F10 . 2_664 2.150(17) ? Yb2 F17 . 3_565 2.20(2) ? Yb2 F19 . . 2.22(2) ? Yb3 F5 . . 2.19(3) ? Yb3 F6 . . 2.25(2) ? Yb3 F12 . 3_654 2.20(4) ? Yb3 F14 . 3_665 2.18(3) ? Yb3 F16 . 1_554 2.24(2) ? Yb3 F21 . 3_665 2.132(17) ? Yb3 F24 . 2_654 2.14(2) ? Yb4 F1 . 2_764 2.155(16) ? Yb4 F2 . 3_555 2.17(3) ? Yb4 F7 . 3_655 2.15(4) ? Yb4 F8 . 1_654 2.202(18) ? Yb4 F8 . 3_654 2.20(2) ? Yb4 F14 . 3_665 2.22(3) ? Yb4 F16 . 1_554 2.22(2) ? Yb5 F4 . 3_565 2.17(3) ? Yb5 F9 . . 2.21(3) ? Yb5 F10 . . 2.251(19) ? Yb5 F18 . 2_664 2.092(17) ? Yb5 F20 . 3_565 2.094(18) ? Yb5 F22 . 1_654 2.24(2) ? Yb5 F23 . 3_664 2.22(3) ? Yb6 F5 . 3_665 2.27(3) ? Yb6 F6 . 2_654 2.145(17) ? Yb6 F11 . . 2.258(19) ? Yb6 F11 . 3_665 2.19(2) ? Yb6 F12 . 3_654 2.16(3) ? Yb6 F22 . 1_654 2.21(2) ? Yb6 F23 . 3_664 2.20(3) ? K1 F1 . 2_664 2.78(2) ? K1 F5 . 3_665 2.79(4) ? K1 F7 . 3_555 2.79(2) ? K1 F13 . 2_654 2.50(3) ? K1 F15 . . 2.54(2) ? K1 F16 . 3_664 2.52(2) ? K1 F20 . 3_565 2.56(2) ? K1 F22 . 1_654 2.888(16) ? K2 F2 . 3_565 3.06(3) ? K2 F6 . 2_654 2.81(3) ? K2 F8 . 1_664 2.92(2) ? K2 F13 . . 2.61(2) ? K2 F14 . . 2.62(2) ? K2 F15 . 3_665 2.49(3) ? K2 F18 . 2_664 2.48(2) ? K2 F23 . 3_664 2.955(19) ? K3 F2 . 3_565 2.83(4) ? K3 F4 . 3_565 2.94(2) ? K3 F10 . 2_664 2.87(3) ? K3 F16 . 1_564 2.776(17) ? K3 F18 . 2_664 2.52(3) ? K3 F19 . 3_565 2.57(2) ? K3 F20 . . 2.52(2) ? K3 F21 . 3_675 2.49(2) ? K4 F1 . 2_664 2.78(2) ? K4 F3 . . 2.78(2) ? K4 F9 . 3_565 2.93(3) ? K4 F14 . 3_565 2.698(18) ? K4 F17 . . 2.65(2) ? K4 F18 . . 2.57(2) ? K4 F20 . 3_565 2.55(3) ? K4 F24 . 2_554 2.64(2) ? K5 F5 . 3_665 2.66(3) ? K5 F10 . 2_654 2.72(3) ? K5 F12 . 3_654 2.72(2) ? K5 F13 . 2_654 2.54(2) ? K5 F17 . 3_555 2.666(19) ? K5 F21 . 3_665 2.61(3) ? K5 F23 . 1_554 2.54(2) ? K5 F24 . . 2.56(2) ? K6 F6 . 2_654 2.93(2) ? K6 F9 . 3_665 2.82(4) ? K6 F11 . 3_665 2.72(2) ? K6 F15 . 3_665 2.49(2) ? K6 F19 . 1_655 2.773(16) ? K6 F21 . . 2.48(2) ? K6 F22 . 3_554 2.45(2) ? K6 F24 . 2_654 2.53(3) ? F1 F7 . 2_565 2.88(3) ? F1 F7 . 3_565 2.78(3) ? F1 F8 . 2_564 3.09(3) ? F1 F14 . 2_665 2.70(2) ? F1 F15 . 3_565 2.87(2) ? F1 F16 . 3_674 3.10(2) ? F1 F17 . 3_565 2.74(3) ? F2 F7 . 3_565 2.76(4) ? F2 F8 . 1_564 3.06(4) ? F2 F8 . 2_563 2.88(4) ? F2 F13 . 2_664 2.96(3) ? F2 F15 . 3_565 3.03(3) ? F2 F16 . 2_553 2.96(3) ? F2 F19 . . 2.73(4) ? F3 F4 . . 2.65(3) ? F3 F4 . 3_565 2.72(4) ? F3 F9 . . 3.12(4) ? F3 F9 . 3_565 2.81(4) ? F3 F10 . 3_564 3.16(3) ? F3 F17 . . 2.62(3) ? F3 F19 . . 2.64(3) ? F4 F9 . 2_664 2.73(3) ? F4 F10 . 2_664 2.72(3) ? F4 F10 . 3_564 2.97(3) ? F4 F18 . 3_564 2.69(4) ? F4 F20 . . 3.12(3) ? F5 F12 . 1_664 2.89(4) ? F5 F12 . 3_654 2.68(4) ? F5 F13 . 3_664 3.18(4) ? F5 F16 . 1_554 2.74(4) ? F5 F22 . 2_663 3.01(3) ? F5 F23 . 1_554 3.09(3) ? F5 F24 . 2_654 2.77(3) ? F6 F11 . 2_655 2.65(3) ? F6 F11 . 3_665 2.95(3) ? F6 F12 . 3_654 2.83(4) ? F6 F14 . 3_665 2.75(4) ? F6 F21 . 3_665 2.86(2) ? F6 F22 . 3_554 3.17(2) ? F6 F23 . 2_654 3.08(3) ? F6 F24 . 2_654 3.04(3) ? F7 F8 . 1_554 2.51(3) ? F7 F8 . 2_553 2.73(4) ? F7 F13 . 3_564 2.69(4) ? F7 F15 . . 3.15(2) ? F8 F14 . 1_446 2.66(3) ? F8 F16 . 1_455 2.68(3) ? F9 F17 . . 3.19(3) ? F9 F18 . 2_664 2.95(3) ? F9 F19 . 2_664 2.94(3) ? F9 F20 . 3_565 3.01(3) ? F9 F22 . 1_654 2.61(4) ? F10 F17 . 2_665 2.73(3) ? F10 F19 . 3_565 3.07(2) ? F10 F20 . 3_565 2.91(2) ? F10 F23 . 3_664 2.71(4) ? F11 F12 . 1_664 2.66(3) ? F11 F12 . 3_654 2.65(4) ? F11 F22 . 1_654 2.53(3) ? F11 F23 . 1_554 2.85(3) ? F12 F21 . 1_446 2.85(2) ? F12 F24 . 3_555 3.07(4) ? F13 F17 . 2_665 2.72(3) ? F14 F16 . 2_653 2.45(3) ? F14 F24 . 3_664 2.79(2) ? F15 F19 . 2_664 2.89(3) ? F16 F21 . 3_666 2.74(3) ? F17 F19 . 2_664 2.47(3) ? F18 F23 . 2_554 2.79(3) ? F19 F21 . 1_455 3.14(2) ? F20 F22 . 2_673 2.93(3) ? F22 F23 . 3_565 2.47(3) ? 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 ? ? ? ? ? ? ? ? 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 ? ? ? ? ? ? ? ? ? ? ? #======================================================================= data_VII _database_code_depnum_ccdc_archive 'CCDC 891242' #TrackingRef '- KYbF4_AP_final.cif' #======================================================================= # 5. CHEMICAL DATA _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_iupac ? _chemical_formula_sum 'F4 K1 Yb1' _chemical_formula_weight 432.2 _chemical_melting_point ? _chemical_compound_source ? _chemical_absolute_configuration ? #======================================================================= # 6. CRYSTAL DATA _symmetry_cell_setting trigonal _symmetry_space_group_name_H-M 'P 32' _symmetry_space_group_name_Hall 'P 32' _symmetry_Int_Tables_number 145 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 -y,x-y,z+2/3 3 -x+y,-x,z+1/3 _cell_length_a 14.026(2) _cell_length_b 14.026(2) _cell_length_c 10.1190(10) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 120 _cell_volume 1724.0(4) loop_ _jana_cell_twin_matrix_id _jana_cell_twin_volume_fraction _jana_cell_twin_matrix_1_1 _jana_cell_twin_matrix_1_2 _jana_cell_twin_matrix_1_3 _jana_cell_twin_matrix_2_1 _jana_cell_twin_matrix_2_2 _jana_cell_twin_matrix_2_3 _jana_cell_twin_matrix_3_1 _jana_cell_twin_matrix_3_2 _jana_cell_twin_matrix_3_3 1 0.5008(10) 1 0 0 0 1 0 0 0 1 2 0 -1 0 0 0 -1 0 0 0 -1 3 0 1 -1 0 0 -1 0 0 0 -1 4 0.4992(10) -1 1 0 0 1 0 0 0 -1 _cell_formula_units_Z 18 _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _cell_measurement_temperature 293 _cell_special_details ; ? ; _exptl_crystal_density_diffrn 4.9938 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_F_000 2250 _exptl_absorpt_coefficient_mu 5.598 _exptl_crystal_description ? _exptl_crystal_size_max 0.09 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.04 _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 ? #======================================================================= # 7. EXPERIMENTAL DATA _exptl_special_details ? _diffrn_ambient_temperature 293 _diffrn_source ? _diffrn_source_power ? _diffrn_source_voltage ? _diffrn_source_current ? _diffrn_radiation_type ? _diffrn_radiation_source ? _diffrn_radiation_wavelength 0.4 _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 100600 _diffrn_reflns_theta_min 0.94 _diffrn_reflns_theta_max 26.01 _diffrn_reflns_theta_full 26.01 _diffrn_measured_fraction_theta_max 0 _diffrn_measured_fraction_theta_full 0.99 _diffrn_reflns_av_R_equivalents 0.0739 _diffrn_reflns_av_sigmaI/netI 0.0602 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 22 _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 24602 _reflns_number_gt 17621 _reflns_threshold_expression I>3\s(I) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.0381 _refine_ls_wR_factor_gt 0.0353 _refine_ls_R_factor_all 0.0587 _refine_ls_wR_factor_ref 0.0384 _refine_ls_goodness_of_fit_ref 1.09 _refine_ls_goodness_of_fit_gt 1.18 _refine_ls_restrained_S_gt ? _refine_ls_restrained_S_all ? _refine_ls_number_reflns 24602 _refine_ls_number_parameters 231 _refine_ls_number_restraints 0 _refine_ls_number_constraints 1 _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 0.0241 _refine_ls_shift/su_mean 0.0053 _refine_diff_density_max 3.32 _refine_diff_density_min -4.05 _refine_ls_extinction_method 'B-C type 1 Gaussian isotropic (Becker & Coppens, 1974)' _refine_ls_extinction_coef 520(60) _refine_ls_abs_structure_details ; 24125 of Friedel pairs used in the refinement ; _refine_ls_abs_structure_Flack 0 _refine_ls_abs_structure_Rogers ? loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source F 0.0032 0.0029 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' K 0.0760 0.0798 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' Yb -0.6177 2.1062 '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 ? #======================================================================= # 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_symmetry_multiplicity _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Yb1 Yb 0.13032(3) 0.88970(4) 0.67154(8) Uani 0.00581(10) 3 1 d . . . Yb2 Yb 0.27742(5) 0.72800(5) 0.67585(10) Uani 0.00714(17) 3 1 d . . . Yb3 Yb 0.78381(7) 0.21038(6) 0.66442(6) Uani 0.00503(14) 3 1 d . . . Yb4 Yb 0.93987(8) 0.05710(8) 0.67429(12) Uani 0.00646(15) 3 1 d . . . Yb5 Yb 0.45319(9) 0.54605(10) 0.67458(8) Uani 0.00765(18) 3 1 d . . . Yb6 Yb 0.60253(5) 0.38535(5) 0.65929(5) Uani 0.00495(11) 3 1 d . . . K7 K 0.2668(3) 0.2173(3) 0.6549(4) Uani 0.0154(9) 3 1 d . . . K8 K 0.7787(3) 0.7165(3) 0.6877(4) Uani 0.0223(12) 3 1 d . . . K9 K 0.6052(3) 0.8798(3) 0.6585(4) Uani 0.0179(10) 3 1 d . . . K10 K 0.1049(3) 0.3975(3) 0.6896(3) Uani 0.0160(8) 3 1 d . . . K11 K 0.4542(3) 0.0614(3) 0.6859(4) Uani 0.0195(11) 3 1 d . . . K12 K 0.9458(3) 0.5596(3) 0.6625(3) Uani 0.0095(7) 3 1 d . . . F1 F 0.1328(6) 0.9374(6) 0.8843(9) Uani 0.0176(16) 3 1 d . . . F2 F 0.0690(6) 0.8783(6) 0.4594(6) Uani 0.0135(13) 3 1 d . . . F3 F 0.2067(5) 0.5985(5) 0.5200(7) Uani 0.0199(10) 3 1 d . . . F4 F 0.3440(7) 0.7280(4) 0.3414(9) Uani 0.0316(11) 3 1 d . . . F5 F 0.7372(6) 0.2048(6) 0.4470(8) Uani 0.0135(13) 3 1 d . . . F6 F 0.7919(6) 0.2713(6) 0.8699(7) Uani 0.0176(16) 3 1 d . . . F7 F 0.0015(7) 0.0602(4) 0.3368(10) Uani 0.0316(11) 3 1 d . . . F8 F -0.1236(5) -0.0746(5) 1.5235(7) Uani 0.0199(10) 3 1 d . . . F9 F 0.3948(6) 0.5382(6) 0.4599(7) Uani 0.0135(13) 3 1 d . . . F10 F 0.4593(7) 0.5949(7) 0.8885(8) Uani 0.0176(16) 3 1 d . . . F11 F 0.5449(6) 0.2842(5) 0.4762(8) Uani 0.0199(10) 3 1 d . . . F12 F -0.2745(7) -0.6061(5) 1.3272(11) Uani 0.0316(11) 3 1 d . . . F13 F 0.7665(6) 0.7312(5) 0.9371(8) Uani 0.0157(13) 3 1 d . . . F14 F 0.8053(6) 0.7234(5) 0.4265(8) Uani 0.0119(11) 3 1 d . . . F15 F 0.2483(5) 0.2220(5) 0.3936(8) Uani 0.0167(14) 3 1 d . . . F16 F 0.8101(6) 0.0775(6) 1.5701(8) Uani 0.0164(15) 3 1 d . . . F17 F 0.1328(5) 0.3939(5) 0.4313(8) Uani 0.0119(11) 3 1 d . . . F18 F 0.0961(6) 0.4070(5) 0.9390(8) Uani 0.0157(13) 3 1 d . . . F19 F 0.1509(5) 0.7547(6) 0.5748(7) Uani 0.0164(15) 3 1 d . . . F20 F 0.5896(5) 0.8865(6) 0.3969(8) Uani 0.0167(14) 3 1 d . . . F21 F 0.9339(6) 0.5726(7) 0.3975(10) Uani 0.0167(14) 3 1 d . . . F22 F -0.5272(7) 0.4133(7) 1.5734(9) Uani 0.0164(15) 3 1 d . . . F23 F 0.4844(5) 0.0678(5) 1.4283(8) Uani 0.0119(11) 3 1 d . . . F24 F 0.4492(6) 0.0844(6) 0.9417(8) Uani 0.0157(13) 3 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 Yb1 Yb 0.00222(10) 0.00549(13) 0.00895(16) 0.00135(11) -0.00006(13) 0.00063(13) Yb2 Yb 0.00807(17) 0.00616(17) 0.0094(3) 0.00522(15) 0.00393(15) 0.00372(14) Yb3 Yb 0.00632(18) 0.00628(17) 0.00371(15) 0.00405(16) -0.00312(14) -0.00208(14) Yb4 Yb 0.00802(16) 0.00673(16) 0.0072(3) 0.00558(12) 0.00143(14) 0.00278(13) Yb5 Yb 0.0083(2) 0.0094(2) 0.0081(2) 0.0066(2) 0.00163(15) 0.00224(16) Yb6 Yb 0.00572(14) 0.00403(13) 0.00566(13) 0.00285(11) -0.00145(13) -0.00117(13) K7 K 0.0190(11) 0.0128(11) 0.0206(14) 0.0127(10) -0.0035(9) -0.0015(8) K8 K 0.0208(12) 0.042(2) 0.0062(9) 0.0175(13) -0.0080(9) -0.0050(10) K9 K 0.0170(12) 0.0159(11) 0.0240(17) 0.0107(11) 0.0013(10) 0.0011(11) K10 K 0.0117(8) 0.0312(13) 0.0047(7) 0.0106(9) -0.0009(6) -0.0083(9) K11 K 0.0175(13) 0.0336(17) 0.0046(8) 0.0106(12) 0.0031(9) -0.0022(8) K12 K 0.0154(10) 0.0104(7) 0.0065(9) 0.0092(7) 0.0034(6) 0.0030(6) F1 F 0.022(2) 0.0203(18) 0.017(2) 0.0158(17) -0.0008(16) -0.0084(16) F2 F 0.0178(16) 0.0195(17) 0.0056(14) 0.0111(15) -0.0055(12) -0.0021(12) F3 F 0.0205(8) 0.0153(13) 0.0203(10) 0.0062(13) 0.0039(16) -0.0086(9) F4 F 0.0417(18) 0.0025(5) 0.0374(13) 0.0012(15) 0.0016(13) -0.0020(19) F5 F 0.0178(16) 0.0195(17) 0.0056(14) 0.0111(15) -0.0055(12) -0.0021(12) F6 F 0.022(2) 0.0203(18) 0.017(2) 0.0158(17) -0.0008(16) -0.0084(16) F7 F 0.0417(18) 0.0025(5) 0.0374(13) 0.0012(15) 0.0016(13) -0.0020(19) F8 F 0.0205(8) 0.0153(13) 0.0203(10) 0.0062(13) 0.0039(16) -0.0086(9) F9 F 0.0178(16) 0.0195(17) 0.0056(14) 0.0111(15) -0.0055(12) -0.0021(12) F10 F 0.022(2) 0.0203(18) 0.017(2) 0.0158(17) -0.0008(16) -0.0084(16) F11 F 0.0205(8) 0.0153(13) 0.0203(10) 0.0062(13) 0.0039(16) -0.0086(9) F12 F 0.0417(18) 0.0025(5) 0.0374(13) 0.0012(15) 0.0016(13) -0.0020(19) F13 F 0.0190(16) 0.0156(15) 0.0157(19) 0.0110(15) 0.0006(16) -0.0022(14) F14 F 0.0132(13) 0.0103(13) 0.0107(15) 0.0048(10) 0.0014(12) -0.0004(10) F15 F 0.0132(14) 0.0204(17) 0.020(2) 0.0111(14) 0.0010(14) 0.0047(17) F16 F 0.0231(17) 0.0235(18) 0.0161(19) 0.0219(17) -0.0144(15) -0.0144(16) F17 F 0.0132(13) 0.0103(13) 0.0107(15) 0.0048(10) 0.0014(12) -0.0004(10) F18 F 0.0190(16) 0.0156(15) 0.0157(19) 0.0110(15) 0.0006(16) -0.0022(14) F19 F 0.0231(17) 0.0235(18) 0.0161(19) 0.0219(17) -0.0144(15) -0.0144(16) F20 F 0.0132(14) 0.0204(17) 0.020(2) 0.0111(14) 0.0010(14) 0.0047(17) F21 F 0.0132(14) 0.0204(17) 0.020(2) 0.0111(14) 0.0010(14) 0.0047(17) F22 F 0.0231(17) 0.0235(18) 0.0161(19) 0.0219(17) -0.0144(15) -0.0144(16) F23 F 0.0132(13) 0.0103(13) 0.0107(15) 0.0048(10) 0.0014(12) -0.0004(10) F24 F 0.0190(16) 0.0156(15) 0.0157(19) 0.0110(15) 0.0006(16) -0.0022(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 Yb1 F1 . . 2.250(9) ? Yb1 F2 . . 2.288(7) ? Yb1 F7 . 3_565 2.207(13) ? Yb1 F13 . 2_664 2.108(7) ? Yb1 F15 . 3_565 2.153(7) ? Yb1 F17 . 3_565 2.221(11) ? Yb1 F19 . . 2.274(9) ? Yb2 F3 . . 2.229(7) ? Yb2 F3 . 3_565 2.274(8) ? Yb2 F4 . 3_565 2.183(13) ? Yb2 F9 . 3_565 2.162(7) ? Yb2 F10 . 2_664 2.220(8) ? Yb2 F17 . 3_565 2.262(9) ? Yb2 F19 . . 2.236(9) ? Yb3 F5 . . 2.286(8) ? Yb3 F6 . . 2.229(8) ? Yb3 F12 . 3_654 2.210(14) ? Yb3 F14 . 3_665 2.224(11) ? Yb3 F16 . 1_554 2.282(10) ? Yb3 F21 . 3_665 2.138(8) ? Yb3 F24 . 2_654 2.103(8) ? Yb4 F1 . 2_764 2.223(9) ? Yb4 F2 . 3_555 2.163(7) ? Yb4 F7 . 3_655 2.197(14) ? Yb4 F8 . 1_654 2.211(7) ? Yb4 F8 . 3_654 2.279(8) ? Yb4 F14 . 3_665 2.271(10) ? Yb4 F16 . 1_554 2.242(10) ? Yb5 F4 . 3_565 2.194(13) ? Yb5 F9 . . 2.304(7) ? Yb5 F10 . . 2.259(9) ? Yb5 F18 . 2_664 2.103(7) ? Yb5 F20 . 3_565 2.137(7) ? Yb5 F22 . 1_654 2.259(11) ? Yb5 F23 . 3_664 2.252(11) ? Yb6 F5 . 3_665 2.186(8) ? Yb6 F6 . 2_654 2.217(7) ? Yb6 F11 . . 2.225(8) ? Yb6 F11 . 3_665 2.252(9) ? Yb6 F12 . 3_654 2.170(14) ? Yb6 F22 . 1_654 2.221(11) ? Yb6 F23 . 3_664 2.230(9) ? K7 F1 . 2_664 2.920(11) ? K7 F5 . 3_665 2.855(12) ? K7 F7 . 3_555 3.001(8) ? K7 F13 . 2_654 2.617(13) ? K7 F15 . . 2.661(9) ? K7 F16 . 3_664 2.544(9) ? K7 F20 . 3_565 2.637(9) ? K7 F22 . 1_654 2.940(8) ? K8 F2 . 3_565 3.012(10) ? K8 F6 . 2_654 2.907(11) ? K8 F8 . 1_664 3.034(8) ? K8 F13 . . 2.546(9) ? K8 F14 . . 2.664(9) ? K8 F15 . 3_665 2.556(12) ? K8 F18 . 2_664 2.572(10) ? K8 F23 . 3_664 2.878(7) ? K9 F2 . 3_565 2.915(11) ? K9 F4 . 3_565 3.125(8) ? K9 F10 . 2_664 2.901(12) ? K9 F16 . 1_564 2.962(7) ? K9 F18 . 2_664 2.648(12) ? K9 F19 . 3_565 2.561(9) ? K9 F20 . . 2.662(9) ? K9 F21 . 3_675 2.521(10) ? K10 F1 . 2_664 2.945(13) ? K10 F3 . . 2.985(7) ? K10 F9 . 3_565 2.882(10) ? K10 F14 . 3_565 2.829(7) ? K10 F17 . . 2.646(8) ? K10 F18 . . 2.534(9) ? K10 F20 . 3_565 2.640(12) ? K10 F24 . 2_554 2.592(10) ? K11 F5 . 3_665 2.898(11) ? K11 F10 . 2_654 2.822(13) ? K11 F12 . 3_654 3.007(9) ? K11 F13 . 2_654 2.577(9) ? K11 F17 . 3_555 2.831(7) ? K11 F21 . 3_665 2.595(14) ? K11 F23 . 1_554 2.635(9) ? K11 F24 . . 2.614(9) ? K12 F6 . 2_654 3.087(9) ? K12 F9 . 3_665 2.841(11) ? K12 F11 . 3_665 2.916(9) ? K12 F15 . 3_665 2.605(9) ? K12 F19 . 1_655 2.947(6) ? K12 F21 . . 2.699(10) ? K12 F22 . 3_554 2.507(9) ? K12 F24 . 2_654 2.605(12) ? F1 F7 . 2_565 2.988(13) ? F1 F7 . 3_565 2.720(15) ? F1 F14 . 2_665 2.924(11) ? F1 F15 . 3_565 2.914(10) ? F1 F16 . 3_674 3.075(10) ? F1 F17 . 3_565 2.730(15) ? F2 F7 . 3_565 2.767(13) ? F2 F8 . 1_564 3.152(12) ? F2 F8 . 2_563 2.896(10) ? F2 F13 . 2_664 2.944(9) ? F2 F15 . 3_565 3.146(10) ? F2 F16 . 2_553 3.045(10) ? F2 F19 . . 2.771(13) ? F3 F4 . . 2.603(10) ? F3 F4 . 3_565 2.700(13) ? F3 F9 . 3_565 2.920(11) ? F3 F10 . 3_564 3.154(11) ? F3 F17 . . 2.672(9) ? F3 F19 . . 2.726(12) ? F4 F9 . 2_664 2.780(11) ? F4 F10 . 2_664 2.725(13) ? F4 F10 . 3_564 3.038(11) ? F4 F18 . 3_564 2.817(13) ? F4 F20 . . 3.077(10) ? F5 F12 . 1_664 2.994(13) ? F5 F12 . 3_654 2.738(15) ? F5 F16 . 1_554 2.760(14) ? F5 F22 . 2_663 2.948(11) ? F5 F23 . 1_554 3.080(10) ? F5 F24 . 2_654 2.889(10) ? F6 F11 . 2_655 2.938(11) ? F6 F11 . 3_665 3.077(14) ? F6 F12 . 3_654 2.752(15) ? F6 F14 . 3_665 2.726(15) ? F6 F21 . 3_665 2.950(10) ? F6 F22 . 3_554 3.144(11) ? F6 F23 . 2_654 3.033(10) ? F6 F24 . 2_654 3.075(11) ? F7 F8 . 1_554 2.628(10) ? F7 F8 . 2_553 2.678(14) ? F7 F13 . 3_564 2.806(14) ? F7 F15 . . 3.100(10) ? F8 F14 . 1_446 2.675(9) ? F8 F16 . 1_455 2.761(13) ? F9 F18 . 2_664 2.916(9) ? F9 F19 . 2_664 3.013(10) ? F9 F20 . 3_565 3.180(10) ? F9 F22 . 1_654 2.739(15) ? F10 F17 . 2_665 2.942(10) ? F10 F19 . 3_565 3.103(10) ? F10 F20 . 3_565 2.925(10) ? F10 F23 . 3_664 2.802(15) ? F11 F12 . 1_664 2.676(11) ? F11 F12 . 3_654 2.595(15) ? F11 F22 . 1_654 2.664(15) ? F11 F23 . 1_554 2.756(10) ? F12 F21 . 1_446 2.829(10) ? F12 F24 . 3_555 3.084(16) ? F13 F17 . 2_665 2.823(13) ? F14 F16 . 2_653 2.490(12) ? F14 F24 . 3_664 2.850(10) ? F15 F19 . 2_664 2.906(14) ? F16 F21 . 3_666 2.840(15) ? F17 F19 . 2_664 2.476(12) ? F18 F23 . 2_554 2.846(12) ? F20 F22 . 2_673 2.916(16) ? F22 F23 . 3_565 2.422(11) ? 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 ? ? ? ? ? ? ? ? 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 ? ? ? ? ? ? ? ? ? ? ? #=======================================================================