#------------------------------------------------------------------------------ #$Date: 2020-03-06 02:55:56 +0200 (Fri, 06 Mar 2020) $ #$Revision: 249096 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/55/74/1557498.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_1557498 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 94.507(17) _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 8.2348(7) _cell_length_b 8.2099(9) _cell_length_c 12.359(8) _cell_measurement_reflns_used 375 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 15.0160 _cell_measurement_theta_min 1.7840 _cell_volume 833.0(6) _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 '2.69 GPa' _diffrn_ambient_temperature 293(2) _diffrn_detector_area_resol_mean 7 _diffrn_measured_fraction_theta_full 0.441 _diffrn_measured_fraction_theta_max 0.403 _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 0.0318 _diffrn_reflns_av_unetI/netI 0.0448 _diffrn_reflns_Laue_measured_fraction_full 0.441 _diffrn_reflns_Laue_measured_fraction_max 0.403 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_l_max 7 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_number 2461 _diffrn_reflns_point_group_measured_fraction_full 0.441 _diffrn_reflns_point_group_measured_fraction_max 0.403 _diffrn_reflns_theta_full 14.282 _diffrn_reflns_theta_max 17.071 _diffrn_reflns_theta_min 1.786 _diffrn_source synchrotron _exptl_absorpt_coefficient_mu 0.231 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.30802 _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 1.808 _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 0.451 _refine_diff_density_min -0.548 _refine_diff_density_rms 0.092 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.883 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 63 _refine_ls_number_reflns 1025 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.883 _refine_ls_R_factor_all 0.1457 _refine_ls_R_factor_gt 0.1047 _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 0.2983 _refine_ls_wR_factor_ref 0.3379 _reflns_Friedel_coverage 0.000 _reflns_number_gt 630 _reflns_number_total 1025 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file jp0c00372_si_002.cif _cod_data_source_block EtaKCrF_c4_p08 _cod_original_cell_volume 832.9(5) _cod_original_sg_symbol_H-M 'P 21/n' _cod_database_code 1557498 _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_p08s2_f3_152_resl0p7_RO in P2(1)/n EtaKCrF_c4_p08s2_f3_152_resl0p7_RO.res created by SHELXL-2016/6 at 17:19:35 on 28-Jan-2019 REM P2(1)/n (#14 in standard setting) CELL 0.41115 8.234767 8.209864 12.358714 90.0000 94.5070 90.0000 ZERR 2.00 0.000661 0.000861 0.007777 0.0000 0.0169 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 L.S. 50 BOND $H OMIT -1 10 2 OMIT 0 8 1 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 9.76439 CR1 6 0.500000 0.500000 0.500000 10.50000 0.03684 0.04673 = 0.09942 0.00342 0.00299 0.00162 K1 5 0.500000 0.500000 1.000000 10.50000 0.04379 0.05848 = 0.10909 -0.00805 0.01481 -0.00390 C1 1 0.799214 0.326424 0.468312 11.00000 0.05908 AFIX 43 H1 2 0.765245 0.259387 0.522839 11.00000 -1.20000 AFIX 0 C2 1 0.339829 0.188631 0.513221 11.00000 0.06095 AFIX 43 H2 2 0.268467 0.227423 0.457029 11.00000 -1.20000 AFIX 0 C3 1 0.582653 0.484628 0.728513 11.00000 0.06490 AFIX 43 H3 2 0.489283 0.420530 0.725354 11.00000 -1.20000 AFIX 0 O1 4 0.702010 0.439710 0.432719 11.00000 0.05989 O2 4 0.930930 0.300402 0.436475 11.00000 0.06522 O3 4 0.462407 0.274435 0.544115 11.00000 0.05410 O4 4 0.310388 0.054847 0.554527 11.00000 0.07115 O5 4 0.626131 0.532580 0.641425 11.00000 0.05894 O6 4 0.652007 0.513045 0.824749 11.00000 0.07419 N1 3 0.974145 0.553499 0.752796 11.00000 0.06293 AFIX 137 H1A 2 0.997364 0.597094 0.689907 11.00000 -1.50000 H1B 2 1.043922 0.590672 0.805724 11.00000 -1.50000 H1C 2 0.873153 0.580661 0.766486 11.00000 -1.50000 AFIX 0 C4 1 0.987635 0.371375 0.746506 11.00000 0.06735 AFIX 23 H4A 2 0.955794 0.325475 0.813999 11.00000 -1.20000 H4B 2 0.910560 0.332820 0.688776 11.00000 -1.20000 AFIX 0 C5 1 1.139427 0.312847 0.728250 11.00000 0.07798 AFIX 137 H5A 2 1.145816 0.295786 0.651855 11.00000 -1.50000 H5B 2 1.157755 0.211536 0.766037 11.00000 -1.50000 H5C 2 1.220747 0.390334 0.754105 11.00000 -1.50000 AFIX 0 HKLF 4 REM EtaKCrF_c4_p08s2_f3_152_resl0p7_RO in P2(1)/n REM R1 = 0.1047 for 630 Fo > 4sig(Fo) and 0.1457 for all 1025 data REM 63 parameters refined using 0 restraints END WGHT 0.1795 1.5803 REM Highest difference peak 0.451, deepest hole -0.548, 1-sigma level 0.092 Q1 1 0.5907 0.5701 0.5292 11.00000 0.05 0.44 Q2 1 0.9031 0.2485 0.4020 11.00000 0.05 0.39 Q3 1 0.9956 0.4960 0.7426 11.00000 0.05 0.38 Q4 1 0.6271 0.5048 0.6092 11.00000 0.05 0.37 Q5 1 0.9535 0.3346 0.4750 11.00000 0.05 0.36 Q6 1 0.6991 0.4266 0.5442 11.00000 0.05 0.33 Q7 1 0.5752 0.5715 1.0386 11.00000 0.05 0.32 Q8 1 0.4853 0.5514 0.6002 11.00000 0.05 0.30 Q9 1 0.6192 0.4437 0.8345 11.00000 0.05 0.30 Q10 1 0.7151 0.4846 0.4944 11.00000 0.05 0.30 Q11 1 0.5654 0.4938 0.7538 11.00000 0.05 0.29 Q12 1 0.2739 0.1076 0.5854 11.00000 0.05 0.29 Q13 1 0.5132 0.5594 0.4094 11.00000 0.05 0.29 Q14 1 0.6871 0.4036 0.4077 11.00000 0.05 0.28 Q15 1 0.4637 0.2671 0.6371 11.00000 0.05 0.28 Q16 1 0.6452 0.5415 0.7131 11.00000 0.05 0.25 Q17 1 0.8274 0.3747 0.4801 11.00000 0.05 0.24 Q18 1 0.6451 0.5822 0.8389 11.00000 0.05 0.24 Q19 1 0.4252 0.5696 0.9665 11.00000 0.05 0.24 Q20 1 1.1319 0.3036 0.6767 11.00000 0.05 0.24 ; _shelx_res_checksum 59189 _shelx_hkl_file ; 0 5 -3 7525.19 593.996 1 0 6 -4 65908.6 2187.89 1 0 7 -5 2587.83 511.807 1 0 -8 -1 106.076 42.4067 1 0 8 -5 36.6501 64.1210 1 0 8 -6 13178.0 1324.29 1 0 9 -6 69.0802 95.7698 1 0 9 -7 251.706 256.537 1 0 10 -7-41.2004 68.5156 1 0 10 -8 499.322 248.807 1 1 0 1 183275. 2845.06 1 -1 0 -1 180322. 2759.85 1 -1 -1 -1 708.025 192.736 1 -1 1 -1 700.209 167.577 1 1 -1 1 762.666 164.080 1 1 1 1 717.311 176.031 1 1 -2 0 162482. 2150.53 1 -1 2 0 158232. 2073.23 1 1 -2 1 60988.3 1596.53 1 -1 2 -1 58488.9 1498.80 1 -1 2 -2 254386. 3927.18 1 -1 3 -1 90.4663 51.7812 1 1 -3 1-1.15067 52.2698 1 -1 3 -2 60457.1 1861.66 1 1 -3 2 59771.2 1880.03 1 -1 3 -3 94225.5 2834.11 1 1 -4 0 318.033 109.282 1 1 -4 1 2021.84 335.929 1 -1 4 -1 2584.47 274.363 1 -1 4 -2 30070.5 1170.00 1 1 -4 2 30033.9 1299.75 1 -1 4 -3 26953.4 1419.06 1 1 -5 0 175157. 2606.67 1 1 -5 1 3559.36 412.722 1 -1 5 -2 54846.1 1428.64 1 -1 5 -3 21412.7 1188.88 1 -1 5 -4 79479.3 2861.67 1 1 -6 0 2634.14 339.262 1 1 -6 1 7191.96 680.126 1 -1 6 -2 20064.4 768.395 1 -1 6 -3 433.755 174.718 1 -1 6 -4 12198.9 1057.38 1 -1 6 -5 2235.18 591.813 1 1 -7 -1 248.497 120.313 1 1 -7 0 29348.5 1172.58 1 1 -7 1 312.135 132.409 1 -1 -7 -1-188.253 120.544 1 -1 7 -3 355.103 110.799 1 -1 7 -4 14497.0 939.776 1 -1 7 -5 2754.36 578.315 1 -1 7 -6 15460.9 1580.77 1 1 -8 -1 4147.00 416.262 1 1 -8 0-0.30941 100.823 1 -1 -8 -1 0.33624 119.012 1 -1 8 -4 46.6567 109.068 1 -1 8 -5 405.757 189.198 1 -1 8 -6 178.439 152.263 1 -1 8 -7 284.709 270.374 1 1 -9 -1 0.31066 62.1736 1 -1 9 -5-105.939 75.8744 1 -1 9 -6 2230.70 419.112 1 -1 9 -7-368.469 393.958 1 -1 9 -8 3738.12 935.788 1 1 -10 -2 0.32286 46.0807 1 1 -10 -1 53.7372 124.277 1 -1 -10 -2 0.53929 155.083 1 -1 10 -6 0.22934 82.7941 1 -1 10 -7 730.816 292.230 1 -1 10 -8-323.156 178.166 1 1 -11 -2-178.333 110.478 1 -2 0 1 37.3448 23.1163 1 2 0 -1-21.7673 51.9304 1 2 0 1 41.5452 70.1236 1 -2 0 -1-71.9795 117.213 1 -2 0 -2 1491.18 346.273 1 2 0 2 1326.75 382.173 1 -2 -1 1 439703. 4356.11 1 2 -1 -1 460941. 4816.55 1 -2 1 1 445328. 4572.04 1 2 1 -1 458982. 4828.66 1 -2 1 0 171175. 2959.35 1 -2 -1 0 176696. 3023.38 1 2 1 0 178409. 3140.05 1 2 -1 0 175345. 3099.56 1 -2 -1 -1 138122. 3061.38 1 2 -1 1 133307. 3021.72 1 2 1 1 138537. 3139.84 1 -2 1 -1 133063. 2964.13 1 2 -1 2 217374. 4343.46 1 2 1 2 216992. 4523.52 1 -2 1 -2 220734. 4426.92 1 -2 -1 -2 216150. 4463.56 1 2 -1 3 677.432 306.435 1 -2 1 -3 442.390 329.749 1 2 2 -2 390.589 170.905 1 2 2 -1 6969.33 566.045 1 2 -2 -1 6557.04 578.262 1 -2 -2 1 6299.29 490.255 1 -2 -2 0 178108. 2988.53 1 2 -2 0 175180. 3162.08 1 -2 2 0 169191. 2995.83 1 2 2 0 181207. 3328.57 1 -2 2 -1 24858.4 1255.71 1 -2 -2 -1 25066.6 1381.85 1 2 -2 1 24365.5 1335.85 1 2 2 1 24584.0 1400.55 1 -2 2 -2 64592.3 2363.79 1 -2 -2 -2 65732.5 2580.73 1 2 -2 2 65050.5 2442.17 1 -2 2 -3 29192.9 1907.61 1 2 -2 3 29715.2 1849.69 1 2 3 -2 21798.7 956.803 1 2 -3 -1 38171.0 1453.87 1 -2 -3 1 38707.8 1193.47 1 2 3 -1 40181.0 1381.62 1 -2 3 0 6848.90 584.088 1 2 -3 0 8463.76 725.345 1 -2 -3 0 7875.29 688.546 1 2 3 0 7042.93 793.207 1 -2 3 -1 43113.8 1598.46 1 -2 -3 -1 43752.1 1945.36 1 2 3 1 42658.8 1957.39 1 2 -3 1 44317.6 1823.44 1 -2 -3 -2 13903.0 1286.90 1 2 -3 2 15447.1 1245.52 1 -2 3 -2 14798.4 1125.60 1 2 -3 3 1173.61 383.972 1 -2 3 -3 1073.60 369.176 1 -2 3 -4 2163.51 569.857 1 2 4 -2 282585. 3488.74 1 2 -4 -1 26104.3 1183.63 1 -2 -4 1 25453.9 909.512 1 -2 4 0 208672. 3134.15 1 2 -4 0 213589. 3569.75 1 -2 -4 0 209017. 3259.98 1 2 4 0 209076. 4005.29 1 2 -4 1 24813.8 1360.56 1 -2 4 -1 27793.9 1247.80 1 -2 -4 -1 24623.5 1481.17 1 -2 4 -2 201645. 3843.44 1 -2 -4 -2 202889. 4632.11 1 2 -4 2 200682. 4307.77 1 2 -4 3 78648.6 2869.29 1 -2 4 -3 78773.8 2756.97 1 -2 4 -4 115882. 3885.37 1 2 5 -3 7628.07 563.649 1 2 5 -2 1611.88 275.704 1 2 5 -1 154835. 3144.23 1 -2 -5 1 155947. 2049.58 1 2 -5 -1 157079. 3028.58 1 -2 -5 0 4202.71 466.468 1 2 -5 0 4266.87 534.588 1 -2 -5 -1 427.365 134.466 1 -2 5 -1 748.888 196.409 1 2 -5 1 382.403 172.351 1 -2 -5 -2 1578.08 465.661 1 2 -5 2 847.962 301.865 1 -2 5 -2 1421.89 302.856 1 -2 5 -3 8840.24 912.513 1 2 -5 3 8706.23 974.144 1 -2 5 -4 18978.2 1584.48 1 -2 5 -5 734.520 344.697 1 2 6 -4 41842.4 1297.56 1 2 6 -3 4328.09 411.909 1 2 -6 -1 618.005 184.913 1 2 -6 0 48584.9 1875.32 1 -2 -6 0 47898.9 1439.41 1 2 -6 1 618.965 227.119 1 -2 -6 -1 912.890 324.463 1 2 -6 2 22134.7 1539.44 1 -2 -6 -2 24664.7 1706.72 1 -2 6 -2 25657.1 1155.64 1 -2 6 -3 19657.9 1232.14 1 -2 6 -4 10601.2 1075.85 1 -2 6 -5 4132.77 781.208 1 -2 6 -6 4644.82 960.155 1 2 7 -4 1347.62 146.591 1 2 -7 -1 717.482 227.495 1 -2 -7 0 2282.35 278.529 1 2 -7 0 3952.64 541.023 1 2 -7 1 1854.86 420.253 1 -2 -7 -1 581.427 158.813 1 -2 7 -2 7944.29 600.005 1 -2 -7 -2 6769.66 877.848 1 2 -7 2 7237.64 880.186 1 -2 7 -3 321.379 188.254 1 -2 7 -4-233.797 213.025 1 -2 7 -5 862.961 413.459 1 -2 7 -6 4538.25 905.200 1 -2 7 -7 854.868 560.938 1 2 8 -5 201.176 77.4350 1 2 -8 -1-30.0365 61.3583 1 2 -8 0 32569.1 1566.56 1 2 -8 1-6.72084 171.336 1 -2 -8 -1 0.37857 112.956 1 -2 -8 -2 22577.9 1616.68 1 2 -8 2 27118.4 1683.87 1 -2 8 -3-162.651 100.078 1 -2 8 -4 10953.3 882.312 1 -2 8 -5-644.958 313.752 1 -2 8 -6 6127.78 1002.59 1 -2 8 -7 1599.95 610.789 1 2 -9 -2-1810.66 396.431 1 2 -9 -1 2555.52 403.822 1 2 -9 0-116.835 122.818 1 -2 -9 -1 802.371 176.629 1 2 -9 1 1947.73 492.249 1 -2 -9 -2 1377.90 515.159 1 -2 9 -4 375.254 131.422 1 -2 9 -5 989.365 287.668 1 -2 9 -6 64.2518 223.760 1 -2 9 -7 112.982 259.665 1 -2 9 -8 626.114 591.468 1 2 -10 -2 4893.89 585.123 1 2 -10 -1 682.761 264.360 1 2 -10 0 2178.69 388.938 1 -2 -10 -2 1889.14 410.831 1 -2 10 -6 838.394 340.442 1 -2 10 -7 111.271 221.232 1 -2 10 -8 288.920 381.211 1 2 -11 -2 407.084 243.547 1 2 -11 -1-203.650 158.419 1 -2 -11 -3-124.462 222.781 1 -3 0 2-42.5982 43.7277 1 3 0 -2 101.133 89.4543 1 -3 0 1 37706.8 1647.05 1 3 0 -1 41471.3 1820.99 1 3 0 0 4.76372 41.5939 1 -3 0 0-21.1883 107.965 1 -3 0 -1 219722. 4420.27 1 3 0 1 220459. 4724.47 1 -3 0 -2 174.713 194.239 1 3 0 2 65.5200 112.902 1 3 0 3 7718.68 1080.39 1 -3 0 -3 6776.75 1026.44 1 3 1 -2 968945. 8581.58 1 -3 -1 2 999999. 7861.51 1 3 1 -1 71998.3 2403.54 1 -3 1 1 70516.6 2222.62 1 3 -1 -1 72797.4 2409.47 1 -3 -1 1 70141.5 2153.40 1 3 1 0 37753.2 1774.96 1 -3 1 0 35026.7 1590.79 1 -3 -1 0 36367.7 1613.93 1 3 -1 0 37583.0 1795.95 1 -3 1 -1 9037.57 874.243 1 -3 -1 -1 10762.1 979.141 1 3 -1 1 9441.23 965.740 1 3 1 1 10437.7 1022.50 1 3 -1 2 593952. 8347.57 1 -3 1 -2 587830. 8097.31 1 3 1 2 587813. 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-10 2 -4 4057.35 1220.35 1 10 3 -5 122.336 310.534 1 10 3 -4 595.758 628.517 1 10 3 -3 406.378 398.335 1 -10 3 3 50.3539 339.941 1 10 -3 -3-372.618 549.915 1 -10 -3 3-172.331 353.268 1 -10 3 2 789.719 390.024 1 10 -3 -2 458.714 592.271 1 10 3 -2 184.897 372.062 1 -10 -3 2 317.784 173.194 1 10 -3 -1 105.022 608.696 1 -10 3 1 138.984 255.817 1 -10 -3 1-232.620 200.713 1 10 3 -1-53.3093 450.428 1 -10 3 0 184.601 161.962 1 10 3 0-318.060 698.616 1 10 -3 0-63.6972 474.021 1 -10 -3 0 447.368 675.864 1 -10 -3 -1 851.507 539.757 1 10 3 1-239.224 671.858 1 10 -3 1 911.591 932.725 1 -10 3 -1 481.002 445.318 1 -10 -3 -2 614.827 609.682 1 10 3 2 322.753 341.720 1 10 -3 2 186.025 327.011 1 -10 3 -2 748.786 466.854 1 10 3 3-262.926 544.621 1 -10 3 -3 273.007 309.381 1 10 -3 3 1095.58 1055.47 1 -10 -3 -3 420.970 371.716 1 10 3 4-787.374 890.486 1 -10 -3 -4 72.0702 259.515 1 10 4 -5 648.337 702.526 1 10 4 -4 2471.82 969.155 1 -10 -4 3 2031.69 732.973 1 10 -4 -3 2190.14 1089.92 1 10 4 -3 2198.19 912.123 1 -10 -4 2 7297.31 1332.53 1 -10 4 2 7131.63 1319.53 1 10 -4 -2 6027.88 1566.96 1 10 4 -2 5948.98 1486.85 1 10 -4 -1 1449.49 715.844 1 -10 -4 1 794.327 481.782 1 -10 4 1 478.807 416.755 1 10 4 -1 32.3927 447.776 1 10 4 0 2585.13 920.682 1 -10 4 0 3262.09 1009.68 1 10 -4 0 2157.04 999.581 1 -10 -4 0 3495.16 1008.15 1 -10 4 -1-148.267 358.682 1 10 4 1-42.5259 259.669 1 -10 -4 -1 677.466 565.893 1 10 -4 1-74.6614 241.897 1 -10 -4 -2 5411.30 1410.88 1 10 4 2 3997.23 1423.53 1 10 -4 2 2663.80 1230.37 1 -10 4 -2 3447.59 1166.93 1 10 4 3 572.963 866.526 1 10 -4 3-403.648 439.799 1 -10 4 -3-121.530 190.457 1 -10 -4 -3 217.793 280.214 1 10 4 4 2681.32 1160.85 1 -10 -4 -4 4298.06 1429.52 1 10 5 -5 169.646 231.946 1 10 5 -4 827.589 556.110 1 -10 -5 3 143.461 250.814 1 10 5 -3 135.576 725.105 1 -10 -5 2-318.938 522.399 1 10 5 -2 82.8437 386.415 1 -10 5 2-225.132 419.085 1 10 -5 -1 2073.66 1132.16 1 -10 -5 1 509.214 435.975 1 10 5 -1 1206.88 997.259 1 -10 5 1 434.432 550.830 1 -10 5 0 632.350 544.603 1 10 5 0-530.944 834.585 1 10 -5 0-612.412 569.169 1 -10 -5 0 16.3324 183.413 1 10 5 1 891.988 724.287 1 -10 5 -1 106.699 278.197 1 -10 -5 -1 455.248 457.679 1 10 -5 1 690.867 764.238 1 -10 5 -2 641.604 640.033 1 -10 -5 -2 273.397 243.758 1 10 5 2 606.507 688.078 1 10 -5 2 156.245 531.946 1 10 5 3 775.854 1205.07 1 -10 -5 -3 1383.46 948.499 1 10 5 4 679.750 920.674 1 -10 -5 -4-278.336 544.655 1 -10 -6 3-16.8662 160.263 1 10 6 -3 468.735 902.888 1 -10 -6 2 5259.95 997.117 1 10 6 -2 4259.51 1429.03 1 10 6 -1-368.084 280.956 1 -10 -6 1 236.933 278.795 1 -10 -6 0 3026.31 964.359 1 10 6 0 1743.35 912.581 1 -10 6 0 2084.15 736.878 1 0 0 0 0.00 0.00 0 TITL EtaKCrF_c4_p08s2_f3_152_resl0p7_RO in P2(1)/n REM P2(1)/n (#14 in standard setting) CELL 0.41115 8.234767 8.209864 12.358714 90.0000 94.5070 90.0000 ZERR 2.00 0.000661 0.000861 0.007777 0.0000 0.0169 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 81402 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 0.061(2) Uani 1 2 d S . P . . K1 K 0.500000 0.500000 1.000000 0.070(3) Uani 1 2 d S . P . . C1 C 0.7992(10) 0.3264(10) 0.4683(17) 0.059(2) Uiso 1 1 d . . . . . H1 H 0.765245 0.259387 0.522839 0.071 Uiso 1 1 calc R U . . . C2 C 0.3398(11) 0.1886(11) 0.5132(16) 0.061(2) Uiso 1 1 d . . . . . H2 H 0.268467 0.227423 0.457029 0.073 Uiso 1 1 calc R U . . . C3 C 0.5827(12) 0.4846(11) 0.729(2) 0.065(3) Uiso 1 1 d . . . . . H3 H 0.489283 0.420530 0.725354 0.078 Uiso 1 1 calc R U . . . O1 O 0.7020(6) 0.4397(7) 0.4327(10) 0.0599(17) Uiso 1 1 d . . . . . O2 O 0.9309(7) 0.3004(7) 0.4365(11) 0.0652(18) Uiso 1 1 d . . . . . O3 O 0.4624(6) 0.2744(7) 0.5441(9) 0.0541(15) Uiso 1 1 d . . . . . O4 O 0.3104(7) 0.0548(9) 0.5545(12) 0.0712(19) Uiso 1 1 d . . . . . O5 O 0.6261(7) 0.5326(7) 0.6414(12) 0.0589(16) Uiso 1 1 d . . . . . O6 O 0.6520(9) 0.5130(8) 0.8247(14) 0.074(2) Uiso 1 1 d . . . . . N1 N 0.9741(9) 0.5535(10) 0.7528(14) 0.063(2) Uiso 1 1 d . . . . . H1A H 0.997364 0.597094 0.689907 0.094 Uiso 1 1 calc R U . . . H1B H 1.043922 0.590672 0.805724 0.094 Uiso 1 1 calc R U . . . H1C H 0.873153 0.580661 0.766486 0.094 Uiso 1 1 calc R U . . . C4 C 0.9876(10) 0.3714(12) 0.7465(16) 0.067(3) Uiso 1 1 d . . . . . H4A H 0.955794 0.325475 0.813999 0.081 Uiso 1 1 calc R U . . . H4B H 0.910560 0.332820 0.688776 0.081 Uiso 1 1 calc R U . . . C5 C 1.1394(11) 0.3128(14) 0.7282(19) 0.078(3) Uiso 1 1 d . . . . . H5A H 1.145816 0.295786 0.651855 0.117 Uiso 1 1 calc R U . . . H5B H 1.157755 0.211536 0.766037 0.117 Uiso 1 1 calc R U . . . H5C H 1.220747 0.390334 0.754105 0.117 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 0.0368(10) 0.0467(10) 0.099(6) 0.0034(11) 0.0030(13) 0.0016(5) K1 0.0438(13) 0.0585(16) 0.109(10) -0.0080(17) 0.0148(19) -0.0039(8) 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 O3 Cr1 O3 180.00(10) . 3_666 ? O3 Cr1 O5 92.0(3) . 3_666 ? O3 Cr1 O5 88.0(3) 3_666 3_666 ? O3 Cr1 O5 88.0(3) . . ? O3 Cr1 O5 92.0(3) 3_666 . ? O5 Cr1 O5 180.0 3_666 . ? O3 Cr1 O1 92.1(3) . . ? O3 Cr1 O1 87.9(3) 3_666 . ? O5 Cr1 O1 89.7(4) 3_666 . ? O5 Cr1 O1 90.3(4) . . ? O3 Cr1 O1 87.9(3) . 3_666 ? O3 Cr1 O1 92.1(3) 3_666 3_666 ? O5 Cr1 O1 90.3(4) 3_666 3_666 ? O5 Cr1 O1 89.7(4) . 3_666 ? O1 Cr1 O1 180.0 . 3_666 ? O6 K1 O6 180.0 3_667 . ? O6 K1 O4 107.6(4) 3_667 4_666 ? O6 K1 O4 72.4(4) . 4_666 ? O6 K1 O4 72.4(4) 3_667 2_556 ? O6 K1 O4 107.6(4) . 2_556 ? O4 K1 O4 180.0 4_666 2_556 ? O6 K1 O2 95.9(3) 3_667 4_566 ? O6 K1 O2 84.1(3) . 4_566 ? O4 K1 O2 95.7(2) 4_666 4_566 ? O4 K1 O2 84.3(2) 2_556 4_566 ? O6 K1 O2 84.1(3) 3_667 2_656 ? O6 K1 O2 95.9(3) . 2_656 ? O4 K1 O2 84.3(2) 4_666 2_656 ? O4 K1 O2 95.7(2) 2_556 2_656 ? O2 K1 O2 180.0 4_566 2_656 ? O6 K1 C1 102.4(4) 3_667 2_656 ? O6 K1 C1 77.6(4) . 2_656 ? O4 K1 C1 68.0(2) 4_666 2_656 ? O4 K1 C1 112.0(2) 2_556 2_656 ? O2 K1 C1 158.4(4) 4_566 2_656 ? O2 K1 C1 21.6(3) 2_656 2_656 ? O6 K1 C1 77.6(4) 3_667 4_566 ? O6 K1 C1 102.4(4) . 4_566 ? O4 K1 C1 112.0(2) 4_666 4_566 ? O4 K1 C1 68.0(2) 2_556 4_566 ? O2 K1 C1 21.6(4) 4_566 4_566 ? O2 K1 C1 158.4(4) 2_656 4_566 ? C1 K1 C1 180.0 2_656 4_566 ? O6 K1 C2 114.6(4) 3_667 4_666 ? O6 K1 C2 65.4(4) . 4_666 ? O4 K1 C2 22.1(3) 4_666 4_666 ? O4 K1 C2 157.9(3) 2_556 4_666 ? O2 K1 C2 74.3(2) 4_566 4_666 ? O2 K1 C2 105.7(2) 2_656 4_666 ? C1 K1 C2 87.5(2) 2_656 4_666 ? C1 K1 C2 92.5(2) 4_566 4_666 ? O6 K1 C2 65.4(4) 3_667 2_556 ? O6 K1 C2 114.6(4) . 2_556 ? O4 K1 C2 157.9(3) 4_666 2_556 ? O4 K1 C2 22.1(3) 2_556 2_556 ? O2 K1 C2 105.7(2) 4_566 2_556 ? O2 K1 C2 74.3(2) 2_656 2_556 ? C1 K1 C2 92.5(2) 2_656 2_556 ? C1 K1 C2 87.5(2) 4_566 2_556 ? C2 K1 C2 180.0 4_666 2_556 ? O6 K1 C3 161.8(2) 3_667 . ? O6 K1 C3 18.2(2) . . ? O4 K1 C3 88.9(4) 4_666 . ? O4 K1 C3 91.1(4) 2_556 . ? O2 K1 C3 74.5(3) 4_566 . ? O2 K1 C3 105.5(3) 2_656 . ? C1 K1 C3 90.6(4) 2_656 . ? C1 K1 C3 89.4(4) 4_566 . ? C2 K1 C3 78.1(4) 4_666 . ? C2 K1 C3 101.9(4) 2_556 . ? O6 K1 C3 18.2(2) 3_667 3_667 ? O6 K1 C3 161.8(2) . 3_667 ? O4 K1 C3 91.1(4) 4_666 3_667 ? O4 K1 C3 88.9(4) 2_556 3_667 ? O2 K1 C3 105.5(3) 4_566 3_667 ? O2 K1 C3 74.5(3) 2_656 3_667 ? C1 K1 C3 89.4(4) 2_656 3_667 ? C1 K1 C3 90.6(4) 4_566 3_667 ? C2 K1 C3 101.9(4) 4_666 3_667 ? C2 K1 C3 78.1(4) 2_556 3_667 ? C3 K1 C3 180.0 . 3_667 ? O2 C1 O1 124.9(15) . . ? O2 C1 K1 54.0(5) . 2_646 ? O1 C1 K1 164.8(10) . 2_646 ? O2 C1 H1 117.6 . . ? O1 C1 H1 117.6 . . ? K1 C1 H1 65.9 2_646 . ? O4 C2 O3 123.0(12) . . ? O4 C2 K1 52.7(4) . 2_546 ? O3 C2 K1 164.0(13) . 2_546 ? O4 C2 H2 118.5 . . ? O3 C2 H2 118.5 . . ? K1 C2 H2 68.2 2_546 . ? O5 C3 O6 127.5(11) . . ? O5 C3 K1 158.2(10) . . ? O6 C3 K1 38.3(9) . . ? O5 C3 H3 116.3 . . ? O6 C3 H3 116.3 . . ? K1 C3 H3 80.6 . . ? C1 O1 Cr1 124.0(11) . . ? C1 O2 K1 104.4(7) . 2_646 ? C2 O3 Cr1 125.5(7) . . ? C2 O4 K1 105.2(5) . 2_546 ? C3 O5 Cr1 124.2(8) . . ? C3 O6 K1 123.5(9) . . ? 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 115.4(9) . . ? C5 C4 H4A 108.4 . . ? N1 C4 H4A 108.4 . . ? C5 C4 H4B 108.4 . . ? N1 C4 H4B 108.4 . . ? H4A C4 H4B 107.5 . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? 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 O3 1.962(6) . ? Cr1 O3 1.962(6) 3_666 ? Cr1 O5 1.980(12) 3_666 ? Cr1 O5 1.980(12) . ? Cr1 O1 1.980(9) . ? Cr1 O1 1.980(9) 3_666 ? K1 O6 2.588(17) 3_667 ? K1 O6 2.588(17) . ? K1 O4 2.630(6) 4_666 ? K1 O4 2.630(6) 2_556 ? K1 O2 2.637(7) 4_566 ? K1 O2 2.637(7) 2_656 ? K1 C1 3.157(8) 2_656 ? K1 C1 3.157(8) 4_566 ? K1 C2 3.191(9) 4_666 ? K1 C2 3.191(9) 2_556 ? K1 C3 3.48(3) . ? K1 C3 3.48(3) 3_667 ? C1 O2 1.202(16) . ? C1 O1 1.282(11) . ? C1 H1 0.9300 . ? C2 O4 1.243(14) . ? C2 O3 1.265(10) . ? C2 H2 0.9300 . ? C3 O5 1.23(3) . ? C3 O6 1.30(3) . ? C3 H3 0.9300 . ? N1 C4 1.502(11) . ? N1 H1A 0.8900 . ? N1 H1B 0.8900 . ? N1 H1C 0.8900 . ? C4 C5 1.374(16) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C5 H5C 0.9600 . ?