#------------------------------------------------------------------------------ #$Date: 2020-03-06 02:55:56 +0200 (Fri, 06 Mar 2020) $ #$Revision: 249096 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/55/74/1557497.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_1557497 loop_ _publ_author_name 'Ptak, Maciej' 'Svane, Katrine L.' 'Collings, Ines E.' 'Paraguassu, Waldeci' _publ_section_title ; Effect of Alkali and Trivalent Metal Ions on the High-Pressure Phase Transition of [C2H5NH3]MI0.5MIII0.5(HCOO)3 (MI = Na, K and MIII = Cr, Al) Heterometallic Perovskites ; _journal_name_full 'The Journal of Physical Chemistry C' _journal_paper_doi 10.1021/acs.jpcc.0c00372 _journal_year 2020 _chemical_formula_moiety 'C6 H6 Cr K O12, 2(C2 H8 N)' _chemical_formula_sum 'C10 H22 Cr K N2 O12' _chemical_formula_weight 453.39 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2yn' _space_group_name_H-M_alt 'P 1 21/n 1' _atom_sites_solution_hydrogens geom _audit_creation_method SHELXL-2016/6 _cell_angle_alpha 90 _cell_angle_beta 87.413(11) _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 8.2602(3) _cell_length_b 8.4583(4) _cell_length_c 12.225(4) _cell_measurement_reflns_used 430 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 16.2260 _cell_measurement_theta_min 1.6840 _cell_volume 853.3(3) _computing_cell_refinement 'CrysAlisPro (Agilent Technologies, 2013)' _computing_data_reduction 'CrysAlisPro (Agilent Technologies, 2013)' _computing_molecular_graphics 'SHELXLE-2011 (Huebschle, 2011)' _computing_structure_refinement 'SHELXL-2016/6 (Sheldrick, 2016)' _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _diffrn_ambient_pressure '2.25 GPa' _diffrn_ambient_temperature 293(2) _diffrn_detector_area_resol_mean 7 _diffrn_measured_fraction_theta_full 0.436 _diffrn_measured_fraction_theta_max 0.260 _diffrn_measurement_device_type 'ID15B beamline, ESRF' _diffrn_measurement_method 'omega scans' _diffrn_radiation_type synchrotron _diffrn_radiation_wavelength 0.41115 _diffrn_reflns_av_R_equivalents 0.0391 _diffrn_reflns_av_unetI/netI 0.0457 _diffrn_reflns_Laue_measured_fraction_full 0.436 _diffrn_reflns_Laue_measured_fraction_max 0.260 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_number 3076 _diffrn_reflns_point_group_measured_fraction_full 0.436 _diffrn_reflns_point_group_measured_fraction_max 0.260 _diffrn_reflns_theta_full 14.282 _diffrn_reflns_theta_max 21.737 _diffrn_reflns_theta_min 1.686 _diffrn_source synchrotron _exptl_absorpt_coefficient_mu 0.225 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.18895 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour 'dark blue' _exptl_crystal_density_diffrn 1.765 _exptl_crystal_description block _exptl_crystal_F_000 470 _exptl_crystal_size_max 0.050 _exptl_crystal_size_mid 0.030 _exptl_crystal_size_min 0.020 _refine_diff_density_max 0.458 _refine_diff_density_min -0.584 _refine_diff_density_rms 0.069 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.315 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 123 _refine_ls_number_reflns 1358 _refine_ls_number_restraints 12 _refine_ls_restrained_S_all 1.310 _refine_ls_R_factor_all 0.1067 _refine_ls_R_factor_gt 0.0738 _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^)+(0.1000P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1969 _refine_ls_wR_factor_ref 0.2448 _reflns_Friedel_coverage 0.000 _reflns_number_gt 758 _reflns_number_total 1358 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file jp0c00372_si_002.cif _cod_data_source_block EtaKCrF_c4_p07 _cod_original_cell_volume 853.2(3) _cod_original_sg_symbol_H-M 'P 21/n' _cod_database_code 1557497 _shelx_shelxl_version_number 2016/6 _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. ; _shelx_res_file ; TITL EtaKCrF_c4_p07_f3_152_R15_RO_s2 in P2(1)/n EtaKCrF_c4_p07_f3_152_R15_RO_s2.res created by SHELXL-2016/6 at 15:48:57 on 08-Nov-2018 REM P2(1)/n (#14 with fixed user cell (not necessary: std = user cell)!) CELL 0.41115 8.260217 8.458262 12.224823 90.0000 87.4126 90.0000 ZERR 2.00 0.000277 0.000375 0.003917 0.0000 0.0108 0.0000 LATT 1 SYMM -x+1/2, y+1/2,-z+1/2 SFAC C H N O K CR DISP $C -0.00006 0.00048 5.14168!source kissel DISP $H -0.00003 0.00000 0.64129!source kissel DISP $N 0.00062 0.00099 7.19180!source kissel DISP $O 0.00180 0.00183 10.15742!source kissel DISP $K 0.08048 0.08446 216.06612!source kissel DISP $Cr 0.16119 0.22192 542.61250!source kissel UNIT 20.00 44.00 4.00 24.00 2.00 2.00 OMIT 3 6 6 OMIT 1 7 6 L.S. 50 BOND $H ACTA LIST 4 DELU O1 C1 O2 DELU O3 C2 O4 DELU O5 C3 O6 DELU N1 C4 C5 FMAP 2 PLAN 20 WGHT 0.100000 FVAR 8.59737 CR1 6 0.500000 0.500000 0.500000 10.50000 0.03232 0.03556 = 0.06855 0.00394 0.00163 -0.00047 K1 5 0.500000 0.500000 1.000000 10.50000 0.03741 0.04612 = 0.07171 -0.00715 0.00490 -0.00194 C1 1 0.780339 0.310786 0.449627 11.00000 0.04777 0.04937 = 0.10788 0.01364 0.00653 0.00646 AFIX 43 H1 2 0.743370 0.255815 0.511731 11.00000 -1.20000 AFIX 0 C2 1 0.334520 0.196160 0.502794 11.00000 0.04125 0.05176 = 0.06433 0.01383 0.00384 -0.01017 AFIX 43 H2 2 0.275318 0.237089 0.446389 11.00000 -1.20000 AFIX 0 C3 1 0.581633 0.472674 0.724989 11.00000 0.03719 0.05911 = 0.06374 -0.00026 0.00699 -0.00223 AFIX 43 H3 2 0.475021 0.438068 0.734185 11.00000 -1.20000 AFIX 0 O1 4 0.692695 0.420725 0.417270 11.00000 0.03922 0.05013 = 0.09834 0.00999 0.01531 0.00926 O2 4 0.910623 0.269218 0.406643 11.00000 0.05551 0.06029 = 0.15974 0.01334 0.01123 0.02016 O3 4 0.440358 0.283357 0.542848 11.00000 0.04302 0.04088 = 0.07795 0.00128 0.00240 -0.00307 O4 4 0.304746 0.061906 0.533115 11.00000 0.05643 0.04758 = 0.13704 0.01216 -0.00841 -0.01677 O5 4 0.631585 0.511672 0.627321 11.00000 0.03740 0.05717 = 0.06139 0.00665 0.01025 -0.00266 O6 4 0.661204 0.476997 0.806241 11.00000 0.04934 0.10300 = 0.06985 0.00133 0.00104 -0.00908 N1 3 1.016029 0.440991 0.223059 11.00000 0.04764 0.06497 = 0.11616 0.00225 0.00312 -0.00745 AFIX 137 H1A 2 1.000452 0.388660 0.285813 11.00000 -1.50000 H1B 2 1.121336 0.459862 0.211071 11.00000 -1.50000 H1C 2 0.979894 0.383197 0.168427 11.00000 -1.50000 AFIX 0 C4 1 0.927957 0.590950 0.229413 11.00000 0.05201 0.07787 = 0.11846 0.01685 0.01020 -0.00089 AFIX 23 H4A 2 0.951359 0.653003 0.163868 11.00000 -1.20000 H4B 2 0.812152 0.571726 0.235888 11.00000 -1.20000 AFIX 0 C5 1 0.979564 0.673649 0.323613 11.00000 0.08462 0.08474 = 0.17652 -0.02717 0.00028 -0.01729 AFIX 137 H5A 2 1.087750 0.712443 0.309660 11.00000 -1.50000 H5B 2 0.977718 0.603159 0.385204 11.00000 -1.50000 H5C 2 0.907897 0.760911 0.339267 11.00000 -1.50000 AFIX 0 HKLF 4 REM EtaKCrF_c4_p07_f3_152_R15_RO_s2 in P2(1)/n REM R1 = 0.0738 for 758 Fo > 4sig(Fo) and 0.1067 for all 1358 data REM 123 parameters refined using 12 restraints END WGHT 0.1287 0.1052 REM Highest difference peak 0.458, deepest hole -0.584, 1-sigma level 0.069 Q1 1 0.6025 0.5627 0.5038 11.00000 0.05 0.46 Q2 1 0.3986 0.5615 0.4930 11.00000 0.05 0.41 Q3 1 0.4004 0.5536 1.0053 11.00000 0.05 0.34 Q4 1 0.6262 0.5046 0.4311 11.00000 0.05 0.30 Q5 1 0.6040 0.5620 1.0021 11.00000 0.05 0.29 Q6 1 0.5570 0.2937 0.4562 11.00000 0.05 0.27 Q7 1 0.8641 0.7087 0.2598 11.00000 0.05 0.27 Q8 1 0.4756 0.4429 0.4303 11.00000 0.05 0.27 Q9 1 0.5031 0.3607 0.4939 11.00000 0.05 0.25 Q10 1 0.4823 0.5558 0.4269 11.00000 0.05 0.24 Q11 1 0.3686 0.5024 1.0761 11.00000 0.05 0.24 Q12 1 0.5152 0.4393 1.0626 11.00000 0.05 0.22 Q13 1 0.2408 0.2526 0.4846 11.00000 0.05 0.20 Q14 1 0.6998 0.5789 0.3943 11.00000 0.05 0.20 Q15 1 0.8371 0.7227 0.1388 11.00000 0.05 0.19 Q16 1 0.3072 -0.0683 0.5305 11.00000 0.05 0.19 Q17 1 0.5154 0.5598 1.0703 11.00000 0.05 0.19 Q18 1 0.4968 0.3627 0.9981 11.00000 0.05 0.18 Q19 1 0.1337 0.0042 0.6139 11.00000 0.05 0.18 Q20 1 1.0822 0.2799 0.1068 11.00000 0.05 0.17 ; _shelx_res_checksum 67185 _shelx_hkl_file ; 0 5 -3 1085.19 170.256 1 0 7 -4 330.751 77.7778 1 0 8 -5 178.296 74.5548 1 0 9 -6 128.907 46.4684 1 0 10 -7 41.2691 36.0590 1 0 11 -8 17.2093 10.5376 1 -1 0 -1 168161. 2105.85 1 1 0 1 181693. 2198.30 1 1 1 1 1915.91 225.195 1 -1 -1 -1 1964.26 222.637 1 -1 1 -1 1774.29 198.972 1 1 -1 1 1729.53 204.674 1 -1 2 0 146736. 1650.49 1 1 -2 0 149655. 1725.19 1 1 -2 1 12765.4 555.752 1 -1 -2 -1 13188.9 594.493 1 -1 2 -1 11731.8 521.800 1 1 -2 2 69899.1 1482.69 1 -1 2 -2 66869.6 1508.70 1 -1 3 -1 944.676 144.424 1 -1 -3 -1 1066.77 170.628 1 1 -3 1 1082.25 164.604 1 1 -3 2 18775.2 741.464 1 -1 3 -2 16713.3 703.104 1 -1 3 -3 122316. 2253.59 1 1 -4 0 11573.7 519.136 1 -1 4 -1 2065.84 197.775 1 1 -4 1 1567.49 200.931 1 -1 -4 -1 1601.33 211.259 1 1 -4 2 13367.9 628.721 1 -1 4 -2 13331.6 618.257 1 -1 4 -3 18460.9 877.395 1 1 -5 0 202532. 2288.84 1 1 -5 1 11832.3 554.230 1 -1 -5 -1 11843.8 624.042 1 -1 5 -2 45241.3 1041.22 1 -1 5 -3 7260.31 540.760 1 -1 5 -4 137859. 2761.92 1 1 -6 0 19397.7 718.495 1 1 -6 1 6880.85 417.037 1 -1 -6 -1 6417.57 476.968 1 -1 6 -3 1848.89 231.156 1 -1 6 -4 26867.9 1152.38 1 -1 6 -5 1653.66 359.707 1 1 -7 0 75558.9 1440.92 1 -1 -7 -1 792.703 161.359 1 -1 7 -3 3518.98 274.098 1 -1 7 -4 18600.7 792.154 1 -1 7 -5 2008.43 341.055 1 -1 7 -6 50061.3 2673.89 1 1 -8 -1 2330.57 273.388 1 1 -8 0 280.210 85.0235 1 -1 -8 -1 793.112 155.844 1 -1 8 -4 615.282 106.037 1 -1 8 -5 663.405 162.724 1 -1 8 -6-41.6497 99.2400 1 -1 8 -7 900.993 476.438 1 1 -9 -1 1421.16 209.916 1 -1 -9 -2 18123.7 896.281 1 -1 9 -5 527.831 98.7676 1 -1 9 -6 16204.8 814.923 1 -1 9 -7-11.3892 65.2817 1 1 10 -7 312.904 92.3895 1 1 -10 -1 908.632 166.435 1 -1 -10 -2 145.030 54.4680 1 -1 10 -7 1171.04 208.374 1 -1 10 -8-45.4967 65.2414 1 1 -11 -2 3844.16 349.910 1 -1 11 -8 2763.38 299.702 1 -1 11 -9 179.752 73.4020 1 -1 -12 -3-34.3430 36.8270 1 -2 0 1-6.57145 29.4612 1 2 0 -1-0.58436 14.9352 1 2 0 1-0.66867 25.3486 1 -2 0 -1 2.51942 7.19925 1 2 0 2 20055.3 1082.43 1 -2 0 -2 18217.0 999.739 1 -2 0 -3-0.91968 34.8641 1 2 0 3 3.60636 62.2589 1 2 1 0 99384.6 1973.03 1 2 -1 0 96398.8 1932.31 1 -2 1 -1 101095. 2081.77 1 2 -1 1 103615. 2149.12 1 2 1 1 105355. 2167.43 1 -2 -1 -1 103453. 2158.77 1 -2 1 -2 58263.6 1706.03 1 -2 -1 -2 56062.6 1797.35 1 2 1 2 59192.9 1868.53 1 2 -1 2 62535.8 1860.97 1 -2 -1 -3 56993.8 2027.22 1 -2 1 -3 57596.5 1937.71 1 2 -1 3 54260.1 1825.68 1 -2 -2 1 3382.28 320.686 1 2 2 -1 3183.58 331.390 1 -2 2 0 105154. 1983.58 1 -2 -2 0 117284. 2058.18 1 2 2 0 123704. 2204.17 1 2 -2 0 110954. 2144.31 1 2 -2 1 47637.8 1478.89 1 -2 -2 -1 47025.4 1439.77 1 2 2 1 47803.6 1486.37 1 -2 2 -1 47628.9 1410.66 1 2 2 2 145148. 2856.23 1 2 -2 2 144279. 2822.40 1 -2 2 -2 140083. 2673.47 1 -2 -2 -2 144658. 2846.58 1 -2 2 -3 124017. 2771.12 1 2 -2 3 124721. 2779.83 1 -2 2 -4 302136. 4634.55 1 2 3 -2 5693.54 446.984 1 2 3 -1 50985.9 1339.57 1 -2 -3 1 51162.6 1252.51 1 2 3 0 176315. 2608.64 1 -2 -3 0 173891. 2506.01 1 -2 3 0 174971. 2529.29 1 2 3 1 46292.4 1475.70 1 -2 -3 -1 43220.2 1387.56 1 -2 3 -1 43431.1 1351.25 1 2 -3 1 43183.6 1442.17 1 -2 -3 -2 5231.57 557.418 1 2 -3 2 4909.00 527.797 1 -2 3 -2 3885.07 435.027 1 2 -3 3 6204.29 615.786 1 -2 3 -3 5734.78 594.011 1 -2 3 -4 3514.89 519.850 1 2 4 -2 346252. 3408.97 1 2 4 -1 50532.1 1318.24 1 -2 -4 1 49301.0 1193.87 1 2 -4 0 168110. 2761.01 1 2 4 0 168874. 2549.26 1 -2 -4 0 165151. 2409.40 1 2 4 1 6896.30 578.990 1 -2 4 -1 5821.19 462.918 1 -2 -4 -1 6843.07 554.910 1 2 -4 1 6699.29 566.390 1 -2 -4 -2 80606.5 2155.55 1 2 -4 2 83573.0 2123.93 1 2 -4 3 42812.3 1566.67 1 -2 4 -3 41658.5 1563.17 1 -2 4 -4 64694.5 2162.62 1 -2 4 -5 10456.0 951.981 1 2 5 -2 23950.8 873.618 1 2 5 -1 81305.9 1623.92 1 2 5 0 1859.08 270.291 1 2 -5 0 1723.16 285.747 1 -2 -5 0 1539.07 224.295 1 2 -5 1 719.379 177.679 1 -2 -5 -1 608.866 182.080 1 -2 5 -1 916.307 190.399 1 -2 -5 -2 11780.9 827.531 1 -2 5 -2 13198.5 746.281 1 2 -5 2 11731.7 812.483 1 -2 5 -3 2178.91 340.522 1 2 -5 3 1780.81 320.605 1 -2 5 -4 991.998 263.028 1 -2 5 -5 19099.1 1312.67 1 2 6 -3 169.390 62.8150 1 2 6 -2 123276. 1942.00 1 2 6 -1 834.075 164.873 1 2 -6 0 64702.6 1751.39 1 -2 -6 0 65347.0 1414.45 1 -2 -6 -1 2274.22 324.928 1 2 -6 1 2354.92 356.727 1 -2 6 -2 42530.5 1289.42 1 2 -6 2 43520.2 1595.97 1 -2 -6 -2 43941.4 1646.19 1 2 -6 3 12999.1 893.847 1 -2 6 -3 14236.3 797.021 1 -2 6 -4 15559.2 986.130 1 -2 6 -5 9621.09 876.386 1 -2 6 -6 32708.8 1982.92 1 2 7 -4 502.451 111.843 1 2 7 -3 40.5486 45.1996 1 2 -7 -1 1650.64 295.061 1 -2 -7 0 104.168 64.1085 1 2 -7 0 197.192 104.418 1 2 -7 1 1419.87 297.460 1 -2 -7 -1 1650.17 264.675 1 -2 -7 -2 710.802 212.587 1 2 -7 2 807.353 232.510 1 -2 7 -3 2817.01 330.270 1 -2 7 -4 1485.84 289.168 1 -2 7 -5 1117.08 278.611 1 -2 7 -6 554.899 229.800 1 -2 7 -7-67.0167 72.1658 1 2 8 -5 3568.90 345.461 1 2 8 -4 25628.7 757.831 1 2 -8 -1 449.723 152.581 1 2 -8 0 36772.3 1367.59 1 -2 -8 -1-2.49603 46.8790 1 2 -8 1 47.8056 65.7548 1 -2 -8 -2 32343.1 1397.05 1 2 -8 2 30596.1 1257.53 1 -2 -8 -3 137.546 154.826 1 -2 8 -4 11814.5 638.185 1 -2 8 -5 1083.02 240.227 1 -2 8 -6 16646.6 1118.86 1 -2 8 -7 4320.51 812.939 1 2 9 -5-34.7838 35.9189 1 2 -9 -1 3448.37 435.901 1 2 -9 0 13.0213 25.2360 1 2 -9 1 964.336 223.389 1 -2 -9 -1 1256.31 161.422 1 -2 -9 -2 38.2873 29.2351 1 -2 -9 -3 1209.85 293.887 1 -2 9 -5 2257.63 282.158 1 -2 9 -6 247.212 91.3394 1 -2 9 -7 1176.51 310.910 1 -2 9 -8 84.0334 105.582 1 2 -10 -1 1273.01 231.195 1 2 -10 0 5731.40 488.455 1 -2 -10 -2 7640.67 527.358 1 -2 -10 -3 723.673 181.001 1 -2 10 -6 6249.92 454.041 1 -2 10 -7 90.4885 32.2822 1 -2 10 -8 1347.06 288.374 1 -2 10 -9 171.153 125.210 1 2 -11 -2 256.049 95.5180 1 2 -11 -1 23.7832 62.8404 1 2 -11 0 27.5994 20.2786 1 -2 -11 -2 30.5809 19.4899 1 -2 -11 -3 0.58344 54.1771 1 -2 11 -8 81.0522 39.8746 1 -2 11 -9 15.3952 60.3872 1 2 -12 -2 1861.76 291.147 1 2 -12 -1-9.59914 28.6453 1 -2 -12 -3 94.2917 51.3521 1 -2 -12 -4 852.558 173.117 1 -3 0 1 31427.3 1264.49 1 3 0 -1 30462.9 1297.67 1 -3 0 0-18.5133 43.5495 1 3 0 0-1.78288 50.9456 1 -3 0 -1 79524.2 2185.68 1 3 0 1 83682.5 2385.28 1 3 0 2 23.1400 42.5052 1 -3 0 -2-18.3852 71.4919 1 -3 0 -3 1021.71 314.686 1 3 0 3 867.943 320.456 1 -3 0 -4-1.33119 10.7590 1 3 0 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-10 1 -4 303.091 309.979 1 10 -1 5 1018.14 562.513 1 -10 -1 -5 1720.07 683.878 1 -10 1 -5 2143.94 718.114 1 10 1 5 257.225 288.101 1 -10 -1 -6 164.360 272.838 1 -10 1 -6 308.584 294.467 1 10 1 6 478.345 571.192 1 10 -1 6 35.0859 121.531 1 -10 -2 2 27756.5 2330.59 1 10 2 -2 21468.5 2373.77 1 10 -2 -1-117.026 172.243 1 -10 -2 1-11.6258 87.8935 1 -10 2 1 120.625 217.998 1 10 2 -1-52.9929 143.493 1 -10 -2 0 19164.8 1911.08 1 -10 2 0 20542.8 1926.07 1 10 2 0 13521.9 1931.01 1 10 -2 0 16462.5 2078.93 1 -10 2 -1 1461.87 590.744 1 10 2 1 588.206 556.415 1 10 -2 1 455.060 381.106 1 -10 -2 -1 438.393 259.601 1 -10 -2 -2 11021.6 1538.40 1 -10 2 -2 11652.6 1520.00 1 10 2 2 8524.88 1566.61 1 10 -2 2 9794.04 1840.25 1 -10 -2 -3 1436.80 566.480 1 10 2 3 282.484 183.505 1 10 -2 3 952.132 658.768 1 -10 2 -3 805.229 482.645 1 -10 2 -4 18741.2 2156.00 1 10 2 4 11427.4 2098.51 1 10 -2 4 13607.7 2266.35 1 -10 -2 -4 17108.8 2083.47 1 10 -2 5 4.74418 271.130 1 -10 -2 -5 98.6799 241.787 1 -10 2 -5 467.449 402.692 1 10 2 5 312.313 425.401 1 -10 -2 -6 6333.11 1316.45 1 -10 2 -6 7337.03 1491.04 1 10 2 6 4960.81 1421.52 1 10 -2 6 4771.34 1449.53 1 10 3 -3-74.1825 257.880 1 10 3 -2 11.5258 158.331 1 -10 -3 2 72.0661 171.206 1 10 -3 -1-127.602 348.888 1 -10 -3 1 45.9027 176.589 1 -10 3 1-107.014 89.0996 1 10 3 -1-49.4505 168.391 1 -10 -3 0 2013.65 646.284 1 -10 3 0 752.520 430.401 1 10 3 0 714.729 510.402 1 10 -3 0 804.585 494.824 1 10 3 1 789.040 501.128 1 -10 3 -1 574.036 267.612 1 10 -3 1 44.3206 298.458 1 -10 -3 -1 577.727 300.987 1 10 3 2-210.250 373.904 1 -10 -3 -2 212.970 255.620 1 10 -3 2 33.8989 184.427 1 -10 3 -2-27.9840 71.0794 1 -10 -3 -3 6.61169 177.231 1 10 3 3 212.334 308.904 1 10 -3 3-72.1658 211.497 1 -10 3 -3-53.1309 118.479 1 10 -3 4 75.2479 237.303 1 -10 3 -4-3.37213 60.9426 1 -10 -3 -4-3.43004 123.978 1 10 3 4-173.682 264.495 1 10 -3 5 373.729 542.074 1 -10 -3 -5 1140.48 599.204 1 10 3 5 1041.73 657.308 1 -10 3 -5 2057.27 699.492 1 -10 -3 -6 285.481 85.8696 1 -10 3 -6 912.580 527.844 1 10 3 6 228.153 365.948 1 10 -3 6 572.117 480.824 1 10 4 -3 326.365 376.899 1 10 4 -2 8037.47 1433.19 1 10 -4 -1-55.1750 68.6057 1 -10 -4 1 138.742 286.743 1 10 4 -1 157.229 238.237 1 -10 4 0 7753.61 1210.37 1 -10 -4 0 7041.50 1214.00 1 10 4 0 4792.28 1186.23 1 10 -4 0 4964.05 1273.32 1 10 4 1 200.561 285.273 1 10 -4 1 12.2595 136.178 1 -10 -4 -1 130.046 145.303 1 -10 4 -1 530.648 301.291 1 10 4 2 3229.18 1027.53 1 -10 4 -2 5988.13 1138.28 1 -10 -4 -2 4385.12 982.889 1 10 -4 2 3892.01 1101.70 1 10 4 3 214.319 331.043 1 -10 -4 -3 259.254 305.110 1 10 -4 3 378.668 461.356 1 -10 4 -3 6.20400 114.890 1 10 -4 4 4337.14 1294.12 1 -10 4 -4 6549.51 1225.96 1 -10 -4 -4 4167.68 1037.69 1 10 4 4 1652.83 752.446 1 10 -4 5-126.934 131.624 1 -10 4 -5 17.1786 100.120 1 -10 -4 -5-28.8480 96.6613 1 10 4 5-226.465 319.036 1 -10 -4 -6 3116.30 886.729 1 10 4 6 2188.31 972.694 1 -10 4 -6 3729.32 1077.12 1 10 5 -3 432.358 344.617 1 10 5 -2 772.342 374.175 1 10 -5 -1 274.612 229.057 1 10 5 -1 420.029 351.085 1 -10 -5 1 371.711 314.677 1 10 5 0-306.732 337.790 1 -10 -5 0-59.3815 167.977 1 -10 5 0-313.484 278.281 1 10 -5 0 74.7301 217.460 1 10 5 1 237.952 234.927 1 -10 5 -1 17.9696 113.535 1 10 -5 1 61.6878 124.366 1 -10 -5 -1-53.2323 281.800 1 10 5 2-134.308 236.199 1 -10 -5 -2 15.3237 242.695 1 -10 5 -2 6.33167 57.2143 1 10 -5 2 272.134 398.057 1 -10 5 -3 122.151 136.321 1 -10 -5 -3 170.669 164.520 1 10 -5 3 59.3790 171.398 1 10 5 3 61.1558 197.710 1 10 -5 4 149.553 112.421 1 -10 5 -4 148.225 217.779 1 -10 -5 -4 83.8826 193.660 1 10 5 4 321.522 335.826 1 10 -5 5 813.892 439.967 1 -10 5 -5 574.627 401.070 1 -10 -5 -5 881.368 516.204 1 10 5 5 216.762 307.541 1 10 6 -3 97.6695 261.176 1 10 6 -2 3281.48 908.634 1 -10 -6 1-37.6818 108.769 1 10 6 -1 129.756 233.727 1 10 6 0 317.956 350.099 1 -10 -6 0 1375.21 490.798 1 10 -6 0 1014.47 548.886 1 -10 -6 -1 330.546 183.219 1 10 6 1 370.531 411.356 1 -10 6 -1 299.087 192.101 1 10 -6 1 316.384 409.427 1 10 6 2 787.016 470.594 1 -10 6 -2 3494.38 816.500 1 10 -6 2 1765.31 788.092 1 -10 -6 -2 2781.22 738.268 1 -10 -6 -3-16.6789 203.547 1 10 -6 3 234.837 419.232 1 -10 6 -3 143.412 299.198 1 10 6 3 393.523 447.354 1 10 -6 4 3353.42 1090.87 1 -10 -6 -4 4243.90 986.028 1 -10 6 -4 5577.57 1072.40 1 10 -6 5-9.08091 190.683 1 -10 6 -5 839.154 443.460 1 -10 -6 -5 770.968 452.714 1 10 6 5 275.191 325.487 1 10 7 -4 22.2053 171.827 1 10 7 -3 270.615 312.002 1 10 7 -2-268.867 332.678 1 10 7 -1 100.689 146.089 1 -10 -7 1 432.130 281.531 1 -10 -7 0 16.2420 53.5912 1 10 7 0 259.137 276.075 1 10 -7 0-45.8503 168.442 1 10 7 1-3.39855 38.8454 1 -10 -7 -1 47.9535 125.867 1 10 -7 1-350.409 388.254 1 10 -7 2 325.597 305.298 1 -10 -7 -2 306.790 264.806 1 10 7 2 267.308 274.453 1 -10 7 -2 874.977 432.574 1 10 -7 3 354.814 126.210 1 -10 -7 -3 713.409 426.163 1 -10 7 -3 1034.11 476.927 1 10 7 3 7.91159 207.200 1 10 -7 4 279.345 371.594 1 -10 7 -4 66.4963 156.689 1 10 7 4 338.700 444.943 1 -10 -7 -4 539.504 344.606 1 -10 -7 -5 1366.51 658.496 1 10 7 5 294.167 493.348 1 10 8 -4 1027.11 490.128 1 10 8 -3-3.19754 171.424 1 10 8 -2 815.284 458.191 1 10 8 -1 138.478 260.859 1 10 8 0 368.225 358.458 1 -10 -8 0 1003.48 408.563 1 -10 -8 -1 2.81305 64.3064 1 10 8 1 351.013 288.689 1 10 -8 2 1005.62 576.239 1 10 8 2 915.022 523.760 1 -10 -8 -3 240.284 289.825 1 -10 8 -3 152.795 265.666 1 10 8 3-316.259 241.527 1 -10 -8 -4 1826.18 681.549 1 10 8 4 885.843 521.126 1 10 8 5-155.599 242.022 1 -10 -8 -5-74.9648 308.050 1 10 9 -4-253.772 305.319 1 10 9 -3 529.517 330.859 1 10 9 -2-39.2626 268.192 1 10 9 -1 362.229 266.112 1 -10 -9 0 170.753 244.586 1 10 9 0 44.1845 258.876 1 -10 -9 -1 120.767 145.219 1 10 9 1-320.360 261.421 1 -10 -9 -2 119.946 169.629 1 10 9 2 254.680 245.664 1 -10 -9 -3 128.618 207.481 1 10 9 3-130.268 173.088 1 -10 -9 -4 24.1589 133.684 1 10 9 4 3.84778 332.042 1 -10 -9 -5 171.596 192.193 1 10 10 -4 732.114 463.705 1 10 10 -3-281.107 312.985 1 10 10 -2 5.82220 148.805 1 10 10 -1-297.266 141.508 1 10 10 0-142.305 134.645 1 -10 -10 -1-93.0009 239.033 1 10 10 1-27.2525 73.4203 1 -10 -10 -2 196.694 214.728 1 10 10 2 3.02482 97.7891 1 10 10 3-38.2435 109.281 1 -10 -10 -3-24.4706 48.4453 1 -10 -10 -4 310.622 230.988 1 10 11 -1-89.4869 108.467 1 10 11 0-24.0604 187.532 1 10 11 1 100.678 80.6100 1 10 11 2-248.259 231.952 1 -10 -11 -2 200.222 136.935 1 -10 -11 -3 6.84606 122.342 1 -10 -11 -4-252.757 179.078 1 0 0 0 0.00 0.00 0 TITL EtaKCrF_c4_p07_f3_152_R15_RO_s2 in P2(1)/n REM P2(1)/n (#14 with fixed user cell (not necessary: std = user cell)!) CELL 0.41115 8.260217 8.458262 12.224823 90.0000 87.4126 90.0000 ZERR 2.00 0.000277 0.000375 0.003917 0.0000 0.0108 0.0000 LATT 1 SYMM -x+1/2, y+1/2,-z+1/2 SFAC C H N O K Cr UNIT 20.00 44.00 4.00 24.00 2.00 2.00 TREF HKLF 4 END ; _shelx_hkl_checksum 86635 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' 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 Cr1 Cr 0.500000 0.500000 0.500000 0.0456(10) Uani 1 2 d S . P . . K1 K 0.500000 0.500000 1.000000 0.0520(15) Uani 1 2 d S . P . . C1 C 0.7803(6) 0.3108(5) 0.4496(11) 0.069(5) Uani 1 1 d . U . . . H1 H 0.743370 0.255815 0.511731 0.082 Uiso 1 1 calc R U . . . C2 C 0.3345(6) 0.1962(5) 0.5028(9) 0.053(4) Uani 1 1 d . U . . . H2 H 0.275318 0.237089 0.446389 0.063 Uiso 1 1 calc R U . . . C3 C 0.5816(7) 0.4727(7) 0.7250(13) 0.054(4) Uani 1 1 d . U . . . H3 H 0.475021 0.438068 0.734185 0.064 Uiso 1 1 calc R U . . . O1 O 0.6927(4) 0.4207(4) 0.4173(7) 0.063(3) Uani 1 1 d . U . . . O2 O 0.9106(4) 0.2692(5) 0.4066(9) 0.092(5) Uani 1 1 d . U . . . O3 O 0.4404(4) 0.2834(3) 0.5428(6) 0.054(3) Uani 1 1 d . U . . . O4 O 0.3047(4) 0.0619(4) 0.5331(7) 0.080(4) Uani 1 1 d . U . . . O5 O 0.6316(5) 0.5117(4) 0.6273(9) 0.052(4) Uani 1 1 d . U . . . O6 O 0.6612(6) 0.4770(6) 0.8062(9) 0.074(4) Uani 1 1 d . U . . . N1 N 1.0160(6) 0.4410(7) 0.2231(11) 0.076(5) Uani 1 1 d . U . . . H1A H 1.000452 0.388660 0.285813 0.115 Uiso 1 1 calc R U . . . H1B H 1.121336 0.459862 0.211071 0.115 Uiso 1 1 calc R U . . . H1C H 0.979894 0.383197 0.168427 0.115 Uiso 1 1 calc R U . . . C4 C 0.9280(7) 0.5909(8) 0.2294(13) 0.083(6) Uani 1 1 d . U . . . H4A H 0.951359 0.653003 0.163868 0.100 Uiso 1 1 calc R U . . . H4B H 0.812152 0.571726 0.235888 0.100 Uiso 1 1 calc R U . . . C5 C 0.9796(11) 0.6736(10) 0.3236(19) 0.115(7) Uani 1 1 d . U . . . H5A H 1.087750 0.712443 0.309660 0.173 Uiso 1 1 calc R U . . . H5B H 0.977718 0.603159 0.385204 0.173 Uiso 1 1 calc R U . . . H5C H 0.907897 0.760911 0.339267 0.173 Uiso 1 1 calc R U . . . 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 Cr1 0.0323(6) 0.0356(5) 0.069(3) 0.0039(5) 0.0016(10) -0.0005(2) K1 0.0374(8) 0.0461(7) 0.072(5) -0.0071(8) 0.0049(14) -0.0019(4) C1 0.048(2) 0.049(2) 0.108(15) 0.014(4) 0.007(4) 0.0065(16) C2 0.041(2) 0.052(2) 0.064(14) 0.014(3) 0.004(4) -0.0102(14) C3 0.037(3) 0.059(3) 0.064(13) 0.000(4) 0.007(5) -0.0022(18) O1 0.0392(15) 0.0501(16) 0.098(11) 0.010(3) 0.015(3) 0.0093(11) O2 0.056(2) 0.060(2) 0.160(15) 0.013(3) 0.011(4) 0.0202(15) O3 0.0430(15) 0.0409(13) 0.078(9) 0.001(2) 0.002(3) -0.0031(10) O4 0.0564(19) 0.0476(17) 0.137(13) 0.012(3) -0.008(4) -0.0168(13) O5 0.0374(18) 0.0572(19) 0.061(12) 0.007(3) 0.010(4) -0.0027(12) O6 0.049(2) 0.103(3) 0.070(13) 0.001(4) 0.001(5) -0.0091(19) N1 0.048(2) 0.065(3) 0.116(17) 0.002(4) 0.003(5) -0.0075(16) C4 0.052(3) 0.078(3) 0.118(19) 0.017(6) 0.010(6) -0.001(2) C5 0.085(5) 0.085(5) 0.18(2) -0.027(8) 0.000(9) -0.017(4) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C -0.0001 0.0005 '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' N N 0.0006 0.0010 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0018 0.0018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' K K 0.0805 0.0845 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cr Cr 0.1612 0.2219 '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 O5 Cr1 O5 180.0(4) 3_666 . ? O5 Cr1 O3 91.4(2) 3_666 . ? O5 Cr1 O3 88.6(2) . . ? O5 Cr1 O3 88.6(2) 3_666 3_666 ? O5 Cr1 O3 91.4(2) . 3_666 ? O3 Cr1 O3 180.0 . 3_666 ? O5 Cr1 O1 92.3(3) 3_666 . ? O5 Cr1 O1 87.7(3) . . ? O3 Cr1 O1 90.37(19) . . ? O3 Cr1 O1 89.63(19) 3_666 . ? O5 Cr1 O1 87.7(3) 3_666 3_666 ? O5 Cr1 O1 92.3(3) . 3_666 ? O3 Cr1 O1 89.63(19) . 3_666 ? O3 Cr1 O1 90.37(19) 3_666 3_666 ? O1 Cr1 O1 180.0 . 3_666 ? O4 K1 O4 180.0 4_666 2_556 ? O4 K1 O2 100.48(13) 4_666 4_566 ? O4 K1 O2 79.52(13) 2_556 4_566 ? O4 K1 O2 79.52(13) 4_666 2_656 ? O4 K1 O2 100.48(13) 2_556 2_656 ? O2 K1 O2 180.00(9) 4_566 2_656 ? O4 K1 O6 108.7(2) 4_666 3_667 ? O4 K1 O6 71.3(2) 2_556 3_667 ? O2 K1 O6 107.8(2) 4_566 3_667 ? O2 K1 O6 72.2(2) 2_656 3_667 ? O4 K1 O6 71.3(2) 4_666 . ? O4 K1 O6 108.7(2) 2_556 . ? O2 K1 O6 72.2(2) 4_566 . ? O2 K1 O6 107.8(2) 2_656 . ? O6 K1 O6 180.0 3_667 . ? O4 K1 C2 159.08(13) 4_666 2_556 ? O4 K1 C2 20.92(13) 2_556 2_556 ? O2 K1 C2 100.42(13) 4_566 2_556 ? O2 K1 C2 79.58(13) 2_656 2_556 ? O6 K1 C2 65.1(2) 3_667 2_556 ? O6 K1 C2 114.9(2) . 2_556 ? O4 K1 C2 20.92(13) 4_666 4_666 ? O4 K1 C2 159.08(13) 2_556 4_666 ? O2 K1 C2 79.58(13) 4_566 4_666 ? O2 K1 C2 100.42(13) 2_656 4_666 ? O6 K1 C2 114.9(2) 3_667 4_666 ? O6 K1 C2 65.1(2) . 4_666 ? C2 K1 C2 180.0 2_556 4_666 ? O4 K1 C1 114.44(12) 4_666 4_566 ? O4 K1 C1 65.56(12) 2_556 4_566 ? O2 K1 C1 20.9(2) 4_566 4_566 ? O2 K1 C1 159.1(2) 2_656 4_566 ? O6 K1 C1 88.1(3) 3_667 4_566 ? O6 K1 C1 91.9(3) . 4_566 ? C2 K1 C1 85.90(12) 2_556 4_566 ? C2 K1 C1 94.10(12) 4_666 4_566 ? O4 K1 C1 65.56(12) 4_666 2_656 ? O4 K1 C1 114.44(12) 2_556 2_656 ? O2 K1 C1 159.1(2) 4_566 2_656 ? O2 K1 C1 20.9(2) 2_656 2_656 ? O6 K1 C1 91.9(3) 3_667 2_656 ? O6 K1 C1 88.1(3) . 2_656 ? C2 K1 C1 94.10(12) 2_556 2_656 ? C2 K1 C1 85.90(12) 4_666 2_656 ? C1 K1 C1 180.0 4_566 2_656 ? O4 K1 C3 90.6(2) 4_666 3_667 ? O4 K1 C3 89.4(2) 2_556 3_667 ? O2 K1 C3 115.7(2) 4_566 3_667 ? O2 K1 C3 64.3(2) 2_656 3_667 ? O6 K1 C3 18.48(14) 3_667 3_667 ? O6 K1 C3 161.52(14) . 3_667 ? C2 K1 C3 81.0(2) 2_556 3_667 ? C2 K1 C3 99.0(2) 4_666 3_667 ? C1 K1 C3 98.8(3) 4_566 3_667 ? C1 K1 C3 81.2(3) 2_656 3_667 ? O4 K1 C3 89.4(2) 4_666 . ? O4 K1 C3 90.6(2) 2_556 . ? O2 K1 C3 64.3(2) 4_566 . ? O2 K1 C3 115.7(2) 2_656 . ? O6 K1 C3 161.52(14) 3_667 . ? O6 K1 C3 18.48(14) . . ? C2 K1 C3 99.0(2) 2_556 . ? C2 K1 C3 81.0(2) 4_666 . ? C1 K1 C3 81.2(3) 4_566 . ? C1 K1 C3 98.8(3) 2_656 . ? C3 K1 C3 180.0 3_667 . ? O2 C1 O1 125.8(10) . . ? O2 C1 K1 50.7(4) . 2_646 ? O1 C1 K1 171.7(8) . 2_646 ? O2 C1 H1 117.1 . . ? O1 C1 H1 117.1 . . ? K1 C1 H1 67.0 2_646 . ? O4 C2 O3 124.2(7) . . ? O4 C2 K1 50.3(2) . 2_546 ? O3 C2 K1 156.3(8) . 2_546 ? O4 C2 H2 117.9 . . ? O3 C2 H2 117.9 . . ? K1 C2 H2 72.8 2_546 . ? O6 C3 O5 125.9(6) . . ? O6 C3 K1 44.1(7) . . ? O5 C3 K1 159.7(6) . . ? O6 C3 H3 117.0 . . ? O5 C3 H3 117.0 . . ? K1 C3 H3 76.0 . . ? C1 O1 Cr1 123.8(8) . . ? C1 O2 K1 108.4(6) . 2_646 ? C2 O3 Cr1 127.8(5) . . ? C2 O4 K1 108.8(3) . 2_546 ? C3 O5 Cr1 124.2(4) . . ? C3 O6 K1 117.4(6) . . ? C4 N1 H1A 109.5 . . ? C4 N1 H1B 109.5 . . ? H1A N1 H1B 109.5 . . ? C4 N1 H1C 109.5 . . ? H1A N1 H1C 109.5 . . ? H1B N1 H1C 109.5 . . ? C5 C4 N1 107.6(8) . . ? C5 C4 H4A 110.2 . . ? N1 C4 H4A 110.2 . . ? C5 C4 H4B 110.2 . . ? N1 C4 H4B 110.2 . . ? H4A C4 H4B 108.5 . . ? C4 C5 K1 154.7(7) . 2_656 ? C4 C5 H5A 109.5 . . ? K1 C5 H5A 76.7 2_656 . ? C4 C5 H5B 109.5 . . ? K1 C5 H5B 90.3 2_656 . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? K1 C5 H5C 47.1 2_656 . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? 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 Cr1 O5 1.941(8) 3_666 ? Cr1 O5 1.941(8) . ? Cr1 O3 1.963(3) . ? Cr1 O3 1.963(3) 3_666 ? Cr1 O1 1.965(5) . ? Cr1 O1 1.965(5) 3_666 ? K1 O4 2.620(3) 4_666 ? K1 O4 2.620(3) 2_556 ? K1 O2 2.666(5) 4_566 ? K1 O2 2.666(5) 2_656 ? K1 O6 2.671(11) 3_667 ? K1 O6 2.671(11) . ? K1 C2 3.225(4) 2_556 ? K1 C2 3.225(4) 4_666 ? K1 C1 3.268(4) 4_566 ? K1 C1 3.268(4) 2_656 ? K1 C3 3.407(16) 3_667 ? K1 C3 3.407(16) . ? C1 O2 1.228(10) . ? C1 O1 1.253(6) . ? C1 H1 0.9300 . ? C2 O4 1.216(6) . ? C2 O3 1.260(6) . ? C2 H2 0.9300 . ? C3 O6 1.216(15) . ? C3 O5 1.288(18) . ? C3 H3 0.9300 . ? N1 C4 1.463(9) . ? N1 H1A 0.8900 . ? N1 H1B 0.8900 . ? N1 H1C 0.8900 . ? C4 C5 1.43(2) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C5 H5C 0.9600 . ?