#------------------------------------------------------------------------------ #$Date: 2021-05-18 06:08:41 +0300 (Tue, 18 May 2021) $ #$Revision: 265286 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/56/26/1562623.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_1562623 loop_ _publ_author_name 'Chen, Xiao-Xian' 'Zhang, X. Y.' 'Liu, De-Xuan' 'Huang, Rui-Kang' 'Wang, Sha-Sha' 'Xiong, Li-Qun' 'Zhang, Wei-Xiong' 'Chen, Xiao-Ming' _publ_section_title ; Room-temperature ferroelectric and ferroelastic orders coexisting in a new tetrafluoroborate-based perovskite ; _journal_name_full 'Chemical Science' _journal_paper_doi 10.1039/D1SC01345A _journal_year 2021 _chemical_formula_moiety 'B3 F12 K1, 1(C5 H14 N2)' _chemical_formula_sum 'C5 H14 B3 F12 K N2' _chemical_formula_weight 401.71 _space_group_crystal_system cubic _space_group_IT_number 221 _space_group_name_Hall '-P 4 2 3' _space_group_name_H-M_alt 'P m -3 m' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary iterative _audit_creation_date 2020-03-03 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _audit_update_record ; 2020-03-04 deposited with the CCDC. 2021-05-17 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 1 _cell_length_a 7.2964(17) _cell_length_b 7.2964(17) _cell_length_c 7.2964(17) _cell_measurement_reflns_used 45 _cell_measurement_temperature 463.0(2) _cell_measurement_theta_max 17.0240 _cell_measurement_theta_min 6.2220 _cell_volume 388.44(16) _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _computing_structure_solution 'olex2.solve (Bourhis et al., 2015)' _diffrn_ambient_temperature 463.0(2) _diffrn_measured_fraction_theta_full 0.980 _diffrn_measured_fraction_theta_max 0.903 _diffrn_measurement_device_type 'multiwire proportional' _diffrn_measurement_method 'phi and omega scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.1925 _diffrn_reflns_av_unetI/netI 0.0675 _diffrn_reflns_Laue_measured_fraction_full 0.980 _diffrn_reflns_Laue_measured_fraction_max 0.903 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min -5 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_k_min -5 _diffrn_reflns_limit_l_max 7 _diffrn_reflns_limit_l_min -1 _diffrn_reflns_number 415 _diffrn_reflns_point_group_measured_fraction_full 0.980 _diffrn_reflns_point_group_measured_fraction_max 0.903 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 30.095 _diffrn_reflns_theta_min 3.950 _exptl_absorpt_coefficient_mu 0.462 _exptl_absorpt_correction_type none _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.717 _exptl_crystal_description block _exptl_crystal_F_000 200 _exptl_crystal_size_max 0.150 _exptl_crystal_size_mid 0.120 _exptl_crystal_size_min 0.100 _refine_diff_density_max 0.152 _refine_diff_density_min -0.281 _refine_diff_density_rms 0.062 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.928 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 110 _refine_ls_number_reflns 139 _refine_ls_number_restraints 171 _refine_ls_restrained_S_all 0.413 _refine_ls_R_factor_all 0.1483 _refine_ls_R_factor_gt 0.0793 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1678 _refine_ls_wR_factor_ref 0.2237 _reflns_Friedel_coverage 0.000 _reflns_number_gt 33 _reflns_number_total 139 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d1sc01345a3.cif _cod_data_source_block 463K _cod_original_cell_volume 388.4(3) _cod_database_code 1562623 _shelx_shelxl_version_number 2014/7 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H,H) groups, All N(H,H) groups 2. Restrained distances B1-F1 = B1-F2 = B1-F3 = B1-F4 1.36 with sigma of 0.02 C1-C2 = C3-C4 = C4-C5 1.53 with sigma of 0.04 C2-N2 = N2-C3 = C5-N1 = N1-C1 1.5 with sigma of 0.04 C1-N2 = C2-C3 = N2-C4 = C3-C5 = C4-N1 = C5-C1 = N1-C2 2.5 with sigma of 0.04 F1-F2 \\sim F1-F3 \\sim F1-F4 \\sim F2-F3 \\sim F2-F4 \\sim F3-F4 with sigma of 0.04 3. Uiso/Uaniso restraints and constraints F1 \\sim F2 \\sim F3 \\sim F4 \\sim B1: within 2A with sigma of 0.02 and sigma for terminal atoms of 0.04 N1 \\sim N2 \\sim C1 \\sim C2 \\sim C3 \\sim C4 \\sim C5: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 Uanis(B1) \\sim Ueq, Uanis(F1) \\sim Ueq, Uanis(F2) \\sim Ueq, Uanis(F3) \\sim Ueq, Uanis(F4) \\sim Ueq: with sigma of 0.08 and sigma for terminal atoms of 0.16 Uanis(C1) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(C5) \\sim Ueq, Uanis(N1) \\sim Ueq, Uanis(N2) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.04 4. Others Fixed Sof: F1(0.0625) F2(0.0625) F3(0.0625) F4(0.0625) B1(0.0625) N1(0.02083) H1A(0.02083) H1B(0.02083) N2(0.02083) H2A(0.02083) H2B(0.02083) C1(0.02083) H1C(0.02083) H1D(0.02083) C2(0.02083) H2C(0.02083) H2D(0.02083) C3(0.02083) H3A(0.02083) H3B(0.02083) C4(0.02083) H4A(0.02083) H4B(0.02083) C5(0.02083) H5A(0.02083) H5B(0.02083) 5.a Secondary CH2 refined with riding coordinates: N1(H1A,H1B), N2(H2A,H2B), C1(H1C,H1D), C2(H2C,H2D), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B) ; _shelx_res_file ; 463k.res created by SHELXL-2014/7 TITL a in Pm-3m #221 REM reset to Pm-3m #221 CELL 0.71073 7.2964 7.2964 7.2964 90 90 90 ZERR 1 0.0017 0.0017 0.0017 0 0 0 LATT 1 SYMM -Y,+X,+Z SYMM -X,-Y,+Z SYMM +Y,-X,+Z SYMM +X,-Z,+Y SYMM +X,-Y,-Z SYMM +X,+Z,-Y SYMM +Z,+Y,-X SYMM -X,+Y,-Z SYMM -Z,+Y,+X SYMM +Z,+X,+Y SYMM +Y,+Z,+X SYMM -Y,-Z,+X SYMM +Z,-X,-Y SYMM -Y,+Z,-X SYMM -Z,-X,+Y SYMM -Z,+X,-Y SYMM +Y,-Z,-X SYMM +Y,+X,-Z SYMM -Y,-X,-Z SYMM -X,+Z,+Y SYMM -X,-Z,-Y SYMM +Z,-Y,+X SYMM -Z,-Y,-X SFAC C H B F K N UNIT 5 14 3 12 1 2 DFIX 1.36 B1 F1 B1 F2 B1 F3 B1 F4 DFIX 1.53 0.04 C1 C2 C3 C4 C4 C5 DFIX 1.5 0.04 C2 N2 N2 C3 C5 N1 N1 C1 DFIX 2.5 0.04 C1 N2 C2 C3 N2 C4 C3 C5 C4 N1 C5 C1 N1 C2 SADI 0.04 F1 F2 F1 F3 F1 F4 F2 F3 F2 F4 F3 F4 SIMU 0.02 0.04 2 F1 > B1 SIMU 0.01 0.02 2 N1 > C5 ISOR 0.08 0.16 B1 F1 F2 F3 F4 ISOR 0.02 0.04 C1 C2 C3 C4 C5 N1 N2 L.S. 20 PLAN 4 TEMP 0 fmap 2 acta REM REM REM WGHT 0.200000 FVAR 1.31845 K1 5 1.000000 1.000000 0.000000 10.02083 0.16433 0.16433 = 0.16433 0.00000 0.00000 0.00000 PART -1 F1 4 0.965787 0.616126 -0.080122 10.06250 0.16376 0.21939 = 0.24563 -0.00528 -0.10683 0.02897 F2 4 0.956536 0.613575 0.223892 10.06250 0.18778 0.21812 = 0.23913 -0.03514 -0.10081 0.01850 F3 4 1.175057 0.451139 0.078008 10.06250 0.11220 0.25913 = 0.27683 -0.04948 -0.08621 0.02677 F4 4 0.881956 0.356120 0.069201 10.06250 0.19313 0.08832 = 0.27830 0.01473 -0.07949 -0.01976 B1 3 0.994920 0.507722 0.072119 10.06250 0.17228 0.20809 = 0.24925 -0.01862 -0.09605 0.01989 N1 6 0.390893 0.601146 0.344933 10.02083 0.03154 0.04575 = 0.03541 0.00043 -0.00080 -0.00549 AFIX 23 H1A 2 0.328928 0.616553 0.241002 10.02083 -1.20000 H1B 2 0.451552 0.704406 0.368096 10.02083 -1.20000 AFIX 0 N2 6 0.412275 0.355820 0.726741 10.02083 0.03221 0.04783 = 0.04588 -0.00374 0.00358 -0.00073 AFIX 23 H2A 2 0.309805 0.289860 0.732000 10.02083 -1.20000 H2B 2 0.459147 0.358811 0.839314 10.02083 -1.20000 AFIX 0 C1 1 0.257969 0.564555 0.498476 10.02083 0.03116 0.04524 = 0.03963 -0.00075 0.00208 -0.00343 AFIX 23 H1C 2 0.188480 0.454202 0.472648 10.02083 -1.20000 H1D 2 0.172656 0.665925 0.509406 10.02083 -1.20000 AFIX 0 C2 1 0.363112 0.541633 0.675770 10.02083 0.02904 0.04583 = 0.04015 -0.00203 0.00520 -0.00030 AFIX 23 H2C 2 0.474854 0.613141 0.667172 10.02083 -1.20000 H2D 2 0.290306 0.593643 0.774096 10.02083 -1.20000 AFIX 0 C3 1 0.545602 0.256593 0.604955 10.02083 0.02986 0.04939 = 0.04026 -0.00310 -0.00240 -0.00530 AFIX 23 H3A 2 0.481225 0.167288 0.530431 10.02083 -1.20000 H3B 2 0.635510 0.192379 0.678893 10.02083 -1.20000 AFIX 0 C4 1 0.641549 0.397561 0.481420 10.02083 0.02713 0.04739 = 0.03779 -0.00121 -0.00231 -0.00547 AFIX 23 H4A 2 0.669256 0.506589 0.552264 10.02083 -1.20000 H4B 2 0.756341 0.346819 0.437583 10.02083 -1.20000 AFIX 0 C5 1 0.524495 0.448526 0.321529 10.02083 0.02991 0.04664 = 0.03745 0.00131 -0.00292 -0.00572 AFIX 23 H5A 2 0.605091 0.480220 0.220666 10.02083 -1.20000 H5B 2 0.456522 0.340325 0.284839 10.02083 -1.20000 AFIX 0 HKLF 4 REM a in Pm-3m #221 REM R1 = 0.0793 for 33 Fo > 4sig(Fo) and 0.1483 for all 139 data REM 110 parameters refined using 171 restraints END WGHT 0.2000 0.0000 REM Highest difference peak 0.152, deepest hole -0.281, 1-sigma level 0.062 Q1 1 0.1984 0.1984 0.8016 10.16667 0.05 0.15 Q2 1 0.5000 0.2574 0.2574 10.25000 0.05 0.08 ; _shelx_res_checksum 86975 _shelx_hkl_file ; -1 1 0 235.64 7.07 1 -1 0 238.31 5.22 -1 -1 1 1829.53 12.71 -2 0 0 1639.07 61.50 -1 2 0 401.85 6.63 -2 0 1 399.86 8.87 1 -2 1 17.28 3.87 2 -1 1 2.78 3.31 2 1 -1 52.63 4.00 -2 1 1 39.79 3.09 2 1 0 440.09 37.27 -2 1 0 482.21 21.59 2 -1 0 458.12 11.15 -2 -1 1 28.18 4.18 2 -2 1 364.90 17.25 2 2 -1 349.69 8.71 -2 2 0 32.17 4.37 2 2 0 2.28 3.24 -2 -1 2 359.87 8.44 -2 -2 2 0.24 0.34 -1 3 0 117.30 4.59 -3 0 1 99.98 9.00 -2 3 0 113.18 6.66 -3 0 2 101.95 4.75 -3 1 2 91.95 5.93 2 3 -1 63.37 3.70 2 -3 1 65.43 3.81 -3 1 1 317.37 12.84 3 1 -1 354.81 10.89 3 -1 1 373.98 37.48 -3 1 0 73.30 14.38 3 1 0 150.29 23.30 -3 -1 1 291.80 26.30 -3 -1 2 42.17 3.75 2 -3 2 38.14 6.55 3 -2 2 19.96 9.53 -3 2 1 36.21 3.14 1 -3 2 34.40 7.39 3 2 -1 70.21 5.01 3 -2 1 83.76 8.98 3 2 0 137.86 26.36 -3 2 0 137.57 17.36 -3 -2 1 6.65 4.77 -1 -3 2 18.71 4.53 -2 -3 2 9.37 5.32 -3 -2 2 43.48 6.23 3 -3 2 8.53 4.46 3 3 -1 47.36 4.25 -3 3 1 24.71 2.69 3 -3 1 50.44 4.32 -3 3 0 11.05 4.27 3 3 0 9.33 7.60 -3 -1 3 60.67 4.90 -3 -2 3 9.10 1.54 -2 -3 3 9.21 1.23 -3 -3 3 2.30 1.78 -4 0 0 4.32 6.48 -1 4 0 5.23 0.96 -4 0 1 5.87 4.35 -2 4 0 8.09 1.93 -4 0 2 12.94 3.01 -4 0 3 3.79 1.22 3 4 0 1.40 3.67 -3 4 0 2.95 2.06 -3 4 1 7.62 1.41 3 4 -1 15.10 2.21 -4 1 2 7.59 1.82 4 -1 2 2.88 4.60 2 4 -1 12.76 1.48 4 1 -1 3.67 1.29 -4 1 1 0.52 0.88 -4 1 0 6.97 5.78 -4 -1 1 0.81 2.65 -4 -1 2 12.25 3.60 -4 -1 3 8.73 1.95 3 -4 2 4.53 1.22 -4 2 2 14.59 2.18 2 -4 2 15.47 1.57 4 -2 2 16.54 10.02 -4 2 1 9.09 2.80 4 2 -1 15.83 3.00 4 -2 1 15.42 3.98 4 2 0 17.02 7.49 4 -2 0 16.79 3.23 -4 2 0 10.96 6.60 -4 -2 2 10.43 7.74 -4 -2 3 3.07 1.93 4 -3 3 1.22 3.68 4 -3 2 5.25 2.41 2 -4 3 2.92 2.04 1 -4 3 4.06 2.38 4 3 -1 14.17 2.88 4 -3 1 17.59 3.01 -4 3 1 10.67 3.12 4 3 0 10.78 6.47 -4 3 0 2.47 3.76 -1 -4 3 0.62 0.78 -3 -2 4 4.82 1.55 -2 -4 3 -0.53 1.15 -4 -3 2 0.00 1.34 -3 -3 4 2.20 0.91 -4 -3 3 1.19 3.46 4 -4 4 4.07 3.15 4 -3 4 4.79 4.76 4 -4 3 1.11 1.54 4 -4 2 5.74 1.73 -4 4 1 1.75 1.55 4 4 -1 5.24 1.58 4 4 0 6.93 6.20 -4 4 0 5.32 5.81 -4 -2 4 3.94 1.47 -2 -4 4 5.87 1.44 -3 -4 4 0.96 1.37 -4 -3 4 0.06 1.17 -4 -4 4 0.00 2.40 5 0 0 46.84 9.07 5 0 1 31.13 11.13 -1 5 0 11.88 1.24 5 0 -1 59.43 8.16 -2 5 0 2.94 1.20 5 0 2 0.36 6.52 -3 5 0 1.52 1.80 3 5 0 1.64 3.44 4 5 0 -5.01 3.99 -4 5 0 0.89 3.98 4 5 -1 1.74 0.77 3 5 -1 0.00 0.23 -3 5 1 0.19 0.41 5 -1 3 9.54 8.78 -2 5 1 9.91 1.83 2 5 -1 6.54 0.83 5 -1 2 7.88 6.00 5 1 -1 4.03 1.50 5 -1 1 6.76 3.73 5 1 0 41.49 8.62 5 -1 0 31.14 5.15 5 1 1 -0.70 4.18 4 5 1 1.72 4.77 5 -2 3 5.39 8.39 5 -2 2 1.36 2.15 5 -2 1 10.22 3.22 5 2 -1 14.41 3.49 5 -2 0 5.86 2.28 5 2 0 9.19 5.01 5 2 1 9.94 8.10 5 2 2 4.31 6.12 -5 -2 2 -0.19 2.94 -2 -4 5 0.12 0.29 4 -5 3 0.00 0.20 3 -4 5 3.00 2.62 5 -3 4 0.00 0.21 3 -5 3 0.00 0.06 5 -3 3 0.89 2.74 2 -5 3 1.16 0.57 5 -3 2 3.35 2.14 5 -3 1 0.39 0.29 5 3 -1 -0.15 0.44 5 3 0 4.67 3.94 5 3 1 7.67 7.32 -3 -3 5 0.01 0.26 -3 -4 5 0.00 0.18 5 -4 4 1.15 1.24 4 -4 5 -1.03 1.70 4 -5 4 0.00 0.38 5 -4 3 0.00 0.77 5 -4 2 1.03 0.87 2 -5 4 3.08 1.20 1 -5 4 0.40 0.32 5 4 -1 1.33 0.97 5 4 0 0.81 2.29 5 4 1 4.22 4.91 5 -5 5 0.00 0.80 5 -4 5 0.00 0.80 5 -5 4 0.00 0.25 4 -5 5 0.35 0.58 3 -5 5 0.00 0.65 5 -5 3 0.00 0.33 5 -3 5 0.00 3.76 2 -5 5 0.42 0.93 5 5 -1 0.62 0.56 5 5 0 -1.73 1.72 5 5 1 0.00 2.73 6 0 0 12.46 4.26 -1 6 0 1.24 0.54 6 0 -1 5.93 3.49 6 0 1 5.57 4.41 6 0 2 -4.49 7.02 -2 6 0 1.29 1.43 -3 6 0 0.12 1.81 6 0 3 -2.95 4.65 3 6 0 0.05 0.35 4 6 0 0.00 1.76 6 0 4 5.15 7.58 5 6 0 0.00 0.87 6 -1 5 0.01 5.88 5 6 -1 0.00 0.19 4 6 -1 1.73 0.63 6 -1 4 1.26 5.40 -3 6 1 0.99 0.73 3 6 -1 0.54 0.37 6 -1 3 2.79 7.19 6 -1 2 0.47 2.18 -2 6 1 0.44 0.48 6 1 -1 5.10 2.29 6 -1 1 0.97 1.20 6 1 0 8.77 4.79 6 -1 0 5.11 1.97 6 1 1 6.07 4.75 6 1 2 8.81 7.68 5 6 1 -6.74 5.58 6 -2 5 0.00 3.70 6 -2 4 0.00 3.30 6 -2 3 -1.21 1.86 6 -2 2 3.50 2.63 6 2 -1 2.24 1.52 6 -2 1 3.25 1.78 6 -2 0 11.53 3.86 6 2 0 8.40 4.29 6 2 1 1.98 3.72 6 2 2 -1.77 3.46 6 2 3 2.09 7.42 5 6 2 0.00 4.58 3 -5 6 0.00 1.19 6 -3 5 0.00 1.78 6 -3 4 0.00 2.47 6 -3 3 0.00 1.17 6 -3 2 0.76 1.12 6 3 -1 1.25 1.06 6 -3 1 1.35 0.87 6 3 0 1.38 2.05 6 3 1 -1.25 3.49 6 3 2 -4.42 5.45 4 -5 6 0.00 2.09 6 -4 5 0.00 1.17 6 -4 4 0.00 0.70 6 -4 3 0.00 0.62 6 -4 2 0.00 0.12 6 4 -1 0.33 0.91 6 4 0 0.00 1.60 6 4 1 0.00 7.01 6 4 2 0.00 3.70 6 -5 5 0.00 0.88 6 -5 4 0.00 0.17 5 -4 6 0.00 2.51 6 -5 3 0.25 0.37 5 -3 6 3.40 3.48 6 5 -1 0.00 0.44 6 5 0 0.00 1.36 6 5 1 -2.76 3.77 6 5 2 0.00 3.52 6 -4 6 0.00 1.72 6 -3 6 0.00 2.12 6 6 -1 0.00 0.75 6 6 0 0.00 0.70 6 6 1 0.00 1.87 6 6 2 0.00 5.78 6 6 3 0.00 4.24 0 7 0 0.56 0.35 7 0 0 7.55 3.29 -1 7 0 0.08 1.33 7 0 1 0.72 1.20 7 0 2 3.35 3.33 2 7 0 2.06 2.55 7 0 3 -1.08 2.62 3 7 0 2.12 1.43 4 7 0 1.09 0.88 7 0 4 0.00 1.36 7 0 6 0.00 5.43 7 -1 5 0.00 4.32 7 -1 4 -5.35 5.46 7 -1 3 12.86 6.72 -2 7 1 0.00 0.06 7 -1 2 1.91 2.00 7 1 -1 -2.19 1.86 7 -1 1 0.13 0.95 7 -1 0 -1.81 1.37 7 1 0 0.30 0.58 7 1 1 1.05 3.10 7 1 2 3.41 3.79 7 1 3 0.00 4.53 7 1 4 22.83 12.13 4 7 1 0.00 2.32 5 7 1 0.00 4.84 7 1 5 0.00 3.18 7 -2 6 0.00 1.33 7 -2 5 0.00 3.28 7 -2 4 -3.50 3.27 7 -2 3 0.00 0.75 7 -2 2 1.92 1.81 7 2 -1 -0.54 0.73 7 -2 1 -0.77 0.89 7 2 0 -0.75 1.00 7 -2 0 0.58 0.81 7 2 1 1.59 2.21 7 2 2 0.00 1.15 7 2 3 22.25 12.64 6 7 2 16.15 9.20 7 -3 6 0.00 1.11 7 -3 5 0.00 2.14 7 -3 4 0.00 0.99 7 -3 3 0.00 0.38 7 -3 2 -0.91 0.91 7 3 -1 0.00 1.11 7 -3 1 -2.15 1.69 7 3 0 -2.21 1.67 7 3 1 0.00 1.61 7 3 2 0.00 4.55 7 3 3 0.00 1.72 7 3 4 5.80 6.29 7 -4 6 0.00 1.93 7 -4 5 0.00 0.97 7 -4 4 0.00 0.87 7 -4 3 0.00 0.35 7 -4 2 0.00 0.17 7 4 -1 0.00 0.09 7 4 0 -2.62 1.74 7 4 1 0.00 2.10 7 4 2 0.00 8.58 7 4 3 0.00 7.31 7 4 4 0.00 7.51 7 -5 5 0.00 0.61 7 -5 4 0.00 0.28 5 -4 7 0.00 2.46 7 -5 3 0.00 0.63 7 5 -1 0.00 0.27 7 5 0 0.00 0.33 7 5 1 0.00 2.56 7 5 2 0.00 8.15 7 5 3 0.00 6.69 7 5 4 0.00 1.37 6 -4 7 0.00 4.81 6 -3 7 0.00 2.49 7 6 0 0.00 0.65 7 6 1 0.00 1.06 7 6 2 0.00 6.20 7 6 3 0.00 3.90 8 0 0 2.18 1.64 8 0 1 1.25 1.24 8 0 2 5.05 3.32 8 0 3 0.00 2.42 8 0 4 0.00 2.93 8 0 5 8.97 7.68 8 -1 5 0.00 3.45 8 -1 4 5.28 4.41 8 -1 3 0.00 2.13 8 -1 2 2.09 2.09 8 -1 1 3.24 2.03 8 1 0 -1.22 1.16 8 -1 0 0.43 0.88 8 1 1 2.55 2.46 8 1 2 0.00 0.56 8 1 3 0.00 0.98 8 1 4 0.00 5.16 8 1 5 0.00 1.94 8 -2 5 2.64 2.67 8 -2 4 0.00 0.62 8 -2 3 0.00 0.38 8 -2 2 -1.65 1.30 8 2 -1 0.00 1.50 8 -2 1 -0.13 0.37 8 2 0 0.00 1.40 8 2 1 0.00 0.94 8 2 2 0.00 1.69 8 2 3 0.00 5.19 8 2 4 0.00 1.64 8 -3 5 0.00 2.12 8 -3 4 0.00 1.32 8 -3 3 0.00 0.07 8 -3 2 0.00 0.92 8 -3 1 0.00 0.83 8 3 -1 0.00 1.60 8 3 0 0.00 0.91 8 3 1 0.00 0.93 8 3 2 6.37 4.96 8 3 3 0.00 6.87 8 3 4 0.00 4.60 8 -4 5 0.00 0.99 8 -4 4 0.00 0.74 8 -4 3 0.00 0.22 8 -4 2 0.00 0.83 8 4 -1 0.00 0.83 8 4 0 0.00 1.24 8 4 1 0.00 2.01 8 4 2 16.57 7.88 8 4 3 0.00 10.19 8 4 4 10.69 9.21 8 5 0 0.00 0.54 8 5 1 0.00 0.31 8 5 2 0.00 2.38 8 5 3 0.00 6.32 8 6 1 0.00 0.92 8 6 2 0.00 2.21 9 0 0 0.49 1.01 9 0 1 0.00 1.33 9 0 2 0.00 1.31 9 0 3 0.00 1.17 9 -1 3 0.00 2.45 9 -1 2 1.29 1.26 9 -1 1 0.00 0.89 9 1 0 -1.90 1.62 9 1 1 0.00 1.06 9 1 2 0.00 1.81 9 1 3 0.00 3.57 9 -2 2 0.00 0.86 9 -2 1 0.00 0.37 9 2 0 0.00 1.52 9 2 1 0.00 1.06 9 2 2 0.00 2.50 9 -3 2 0.00 1.40 9 3 0 0.00 0.68 9 3 1 0.00 0.17 9 3 2 0.00 0.37 9 4 0 0.08 1.40 9 4 1 0.00 0.20 9 5 0 0.00 0.37 0 0 0 0.00 0.00 ; _shelx_hkl_checksum 78861 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-y, x, z' '-x, -y, z' 'y, -x, z' 'x, -z, y' 'x, -y, -z' 'x, z, -y' 'z, y, -x' '-x, y, -z' '-z, y, x' 'z, x, y' 'y, z, x' '-y, -z, x' 'z, -x, -y' '-y, z, -x' '-z, -x, y' '-z, x, -y' 'y, -z, -x' 'y, x, -z' '-y, -x, -z' '-x, z, y' '-x, -z, -y' 'z, -y, x' '-z, -y, -x' '-x, -y, -z' 'y, -x, -z' 'x, y, -z' '-y, x, -z' '-x, z, -y' '-x, y, z' '-x, -z, y' '-z, -y, x' 'x, -y, z' 'z, -y, -x' '-z, -x, -y' '-y, -z, -x' 'y, z, -x' '-z, x, y' 'y, -z, x' 'z, x, -y' 'z, -x, y' '-y, z, x' '-y, -x, z' 'y, x, z' 'x, -z, -y' 'x, z, y' '-z, y, -x' 'z, y, x' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group K1 K 1.0000 1.0000 0.0000 0.164(6) Uani 1 48 d S T P . . F1 F 0.966(14) 0.616(13) -0.080(17) 0.21(4) Uani 0.0625 1 d D U . A -1 F2 F 0.957(10) 0.614(17) 0.224(16) 0.22(4) Uani 0.0625 1 d D U . A -1 F3 F 1.175(10) 0.451(17) 0.078(9) 0.22(5) Uani 0.0625 1 d D U . A -1 F4 F 0.882(15) 0.356(8) 0.069(16) 0.19(4) Uani 0.0625 1 d D U . A -1 B1 B 0.995(10) 0.508(11) 0.072(11) 0.21(4) Uani 0.0625 1 d D U . A -1 N1 N 0.39(3) 0.60(2) 0.345(9) 0.038(18) Uani 0.0208 1 d D U . B -1 H1A H 0.3289 0.6166 0.2410 0.045 Uiso 0.0208 1 calc R . . B -1 H1B H 0.4516 0.7044 0.3681 0.045 Uiso 0.0208 1 calc R . . B -1 N2 N 0.412(17) 0.356(14) 0.727(11) 0.04(2) Uani 0.0208 1 d D U . B -1 H2A H 0.3098 0.2899 0.7320 0.050 Uiso 0.0208 1 calc R . . B -1 H2B H 0.4591 0.3588 0.8393 0.050 Uiso 0.0208 1 calc R . . B -1 C1 C 0.258(10) 0.565(12) 0.50(2) 0.039(19) Uani 0.0208 1 d D U . B -1 H1C H 0.1885 0.4542 0.4726 0.046 Uiso 0.0208 1 calc R . . B -1 H1D H 0.1727 0.6659 0.5094 0.046 Uiso 0.0208 1 calc R . . B -1 C2 C 0.36(2) 0.542(14) 0.676(13) 0.04(2) Uani 0.0208 1 d D U . B -1 H2C H 0.4749 0.6131 0.6672 0.046 Uiso 0.0208 1 calc R . . B -1 H2D H 0.2903 0.5936 0.7741 0.046 Uiso 0.0208 1 calc R . . B -1 C3 C 0.55(2) 0.257(12) 0.605(12) 0.04(2) Uani 0.0208 1 d D U . B -1 H3A H 0.4812 0.1673 0.5304 0.048 Uiso 0.0208 1 calc R . . B -1 H3B H 0.6355 0.1924 0.6789 0.048 Uiso 0.0208 1 calc R . . B -1 C4 C 0.642(11) 0.398(15) 0.481(18) 0.037(19) Uani 0.0208 1 d D U . B -1 H4A H 0.6693 0.5066 0.5523 0.045 Uiso 0.0208 1 calc R . . B -1 H4B H 0.7563 0.3468 0.4376 0.045 Uiso 0.0208 1 calc R . . B -1 C5 C 0.52(3) 0.449(17) 0.322(9) 0.038(19) Uani 0.0208 1 d D U . B -1 H5A H 0.6051 0.4802 0.2207 0.046 Uiso 0.0208 1 calc R . . B -1 H5B H 0.4565 0.3403 0.2848 0.046 Uiso 0.0208 1 calc R . . B -1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 K1 0.164(6) 0.164(6) 0.164(6) 0.000 0.000 0.000 F1 0.16(6) 0.22(5) 0.25(8) -0.01(5) -0.11(5) 0.03(5) F2 0.19(6) 0.22(5) 0.24(8) -0.04(5) -0.10(5) 0.02(4) F3 0.11(4) 0.26(9) 0.28(9) -0.05(7) -0.09(6) 0.03(5) F4 0.19(7) 0.088(19) 0.28(10) 0.01(5) -0.08(7) -0.02(4) B1 0.17(5) 0.21(5) 0.25(7) -0.02(5) -0.10(5) 0.02(4) N1 0.03(2) 0.05(3) 0.04(2) 0.00(2) 0.00(2) -0.01(2) N2 0.03(2) 0.05(3) 0.05(3) -0.004(19) 0.004(19) -0.001(19) C1 0.03(2) 0.05(3) 0.04(2) 0.00(2) 0.00(2) -0.003(18) C2 0.03(2) 0.05(3) 0.04(3) 0.00(2) 0.01(2) 0.000(19) C3 0.03(2) 0.05(3) 0.04(3) 0.00(2) 0.00(2) -0.005(19) C4 0.03(2) 0.05(3) 0.04(2) 0.00(2) 0.00(2) -0.01(2) C5 0.03(2) 0.05(3) 0.04(2) 0.001(19) 0.00(2) -0.01(2) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag F1 K1 F2 41.7(18) . . ? B1 F1 K1 112(7) . . ? B1 F2 K1 94(5) . . ? F2 B1 F1 107(4) . . ? F2 B1 F4 110(4) . . ? F3 B1 F1 110(5) . . ? F3 B1 F2 110(4) . . ? F3 B1 F4 109(4) . . ? F4 B1 F1 111(5) . . ? C5 N1 C1 112(8) . . ? C2 N2 C3 117(5) . . ? N1 C1 C2 109(6) . . ? N2 C2 C1 117(8) . . ? N2 C3 C4 109(6) . . ? C5 C4 C3 111(7) . . ? N1 C5 C4 118(8) . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag K1 F1 2.87(10) . ? K1 F2 3.27(15) . ? F1 B1 1.38(4) . ? F2 B1 1.38(4) . ? F3 B1 1.38(4) . ? F4 B1 1.38(4) . ? N1 C1 1.51(8) . ? N1 C5 1.49(7) . ? N2 C2 1.45(7) . ? N2 C3 1.50(6) . ? C1 C2 1.51(8) . ? C3 C4 1.54(8) . ? C4 C5 1.49(8) . ?