#------------------------------------------------------------------------------ #$Date: 2020-03-06 02:55:56 +0200 (Fri, 06 Mar 2020) $ #$Revision: 249096 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/55/74/1557493.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_1557493 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 87.379(11) _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 8.3247(17) _cell_length_b 8.8916(15) _cell_length_c 12.3381(14) _cell_measurement_reflns_used 372 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 17.4570 _cell_measurement_theta_min 2.6790 _cell_volume 912.3(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 '0.91 GPa' _diffrn_ambient_temperature 293(2) _diffrn_detector_area_resol_mean 7 _diffrn_measured_fraction_theta_full 0.680 _diffrn_measured_fraction_theta_max 0.368 _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 0.0425 _diffrn_reflns_av_unetI/netI 0.0682 _diffrn_reflns_Laue_measured_fraction_full 0.680 _diffrn_reflns_Laue_measured_fraction_max 0.368 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_number 3359 _diffrn_reflns_point_group_measured_fraction_full 0.680 _diffrn_reflns_point_group_measured_fraction_max 0.368 _diffrn_reflns_theta_full 14.282 _diffrn_reflns_theta_max 22.012 _diffrn_reflns_theta_min 2.134 _diffrn_source synchrotron _exptl_absorpt_coefficient_mu 0.211 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.88130 _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 1.650 _exptl_crystal_description block _exptl_crystal_F_000 470 _exptl_crystal_size_max 0.040 _exptl_crystal_size_mid 0.030 _exptl_crystal_size_min 0.010 _refine_diff_density_max 0.458 _refine_diff_density_min -0.709 _refine_diff_density_rms 0.081 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.981 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 123 _refine_ls_number_reflns 2134 _refine_ls_number_restraints 12 _refine_ls_restrained_S_all 0.979 _refine_ls_R_factor_all 0.1217 _refine_ls_R_factor_gt 0.0675 _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^)+(0.0899P)^2^+0.3443P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1717 _refine_ls_wR_factor_ref 0.2293 _reflns_Friedel_coverage 0.000 _reflns_number_gt 894 _reflns_number_total 2134 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file jp0c00372_si_002.cif _cod_data_source_block EtaKCrF_c3_p03 _cod_original_sg_symbol_H-M 'P 21/n' _cod_database_code 1557493 _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_c3_p03_f4_152_R15_RO_s2 in P2(1)/n EtaKCrF_c3_p03_f4_152_R15_RO_s2.res created by SHELXL-2016/6 at 13:58:52 on 08-Nov-2018 REM P2(1)/n (#14 with fixed user cell (not necessary: std = user cell)!) CELL 0.41115 8.324659 8.891645 12.338062 90.0000 87.3787 90.0000 ZERR 2.00 0.001733 0.001450 0.001434 0.0000 0.0112 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 1 1 2 OMIT -1 1 2 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 0.089900 0.344300 FVAR 7.54550 CR1 6 0.500000 0.500000 0.500000 10.50000 0.03553 0.05481 = 0.04268 0.00349 0.00111 0.00170 K1 5 0.500000 0.500000 1.000000 10.50000 0.04129 0.05833 = 0.04952 -0.00250 0.00309 0.00036 C1 1 0.772423 0.304353 0.449521 11.00000 0.05551 0.07318 = 0.06529 0.01015 0.01226 0.00899 AFIX 43 H1 2 0.734269 0.252167 0.510748 11.00000 -1.20000 AFIX 0 C2 1 0.325726 0.214136 0.510157 11.00000 0.06610 0.06218 = 0.07459 0.01034 -0.00923 -0.00807 AFIX 43 H2 2 0.267245 0.251244 0.453543 11.00000 -1.20000 AFIX 0 C3 1 0.581730 0.487474 0.725879 11.00000 0.04417 0.07754 = 0.04975 0.00582 -0.00226 -0.00237 AFIX 43 H3 2 0.476610 0.453610 0.737252 11.00000 -1.20000 AFIX 0 O1 4 0.690090 0.415311 0.419671 11.00000 0.05025 0.06900 = 0.05355 0.00841 0.00699 0.00992 O2 4 0.899351 0.259135 0.404371 11.00000 0.06435 0.07329 = 0.08411 0.01149 0.02204 0.01791 O3 4 0.432365 0.297572 0.547747 11.00000 0.05414 0.06052 = 0.05567 0.00324 -0.00453 -0.00497 O4 4 0.294602 0.088082 0.543369 11.00000 0.09635 0.06753 = 0.10790 0.02187 -0.02374 -0.02776 O5 4 0.628685 0.515328 0.630080 11.00000 0.04824 0.07167 = 0.04636 0.00664 -0.00037 -0.00316 O6 4 0.662747 0.501080 0.806173 11.00000 0.04256 0.13096 = 0.04569 0.00787 -0.00220 -0.00926 N1 3 1.011259 0.428911 0.225267 11.00000 0.05794 0.09054 = 0.05952 -0.00377 -0.00015 -0.01091 AFIX 137 H1A 2 0.982847 0.374038 0.283353 11.00000 -1.50000 H1B 2 1.117766 0.438500 0.220469 11.00000 -1.50000 H1C 2 0.978188 0.383618 0.165946 11.00000 -1.50000 AFIX 0 C4 1 0.936760 0.578778 0.235250 11.00000 0.06963 0.10361 = 0.10622 0.03095 0.01628 0.00636 AFIX 23 H4A 2 0.964989 0.637270 0.170803 11.00000 -1.20000 H4B 2 0.820698 0.568105 0.240338 11.00000 -1.20000 AFIX 0 C5 1 0.988812 0.657144 0.329323 11.00000 0.12542 0.09162 = 0.17114 -0.03803 0.03256 -0.02240 AFIX 137 H5A 2 1.098040 0.689650 0.316713 11.00000 -1.50000 H5B 2 0.982051 0.591064 0.390895 11.00000 -1.50000 H5C 2 0.921107 0.743053 0.343183 11.00000 -1.50000 AFIX 0 HKLF 4 REM EtaKCrF_c3_p03_f4_152_R15_RO_s2 in P2(1)/n REM R1 = 0.0675 for 894 Fo > 4sig(Fo) and 0.1217 for all 2134 data REM 123 parameters refined using 12 restraints END WGHT 0.1107 0.0000 REM Highest difference peak 0.458, deepest hole -0.709, 1-sigma level 0.081 Q1 1 0.4219 0.4133 0.4740 11.00000 0.05 0.46 Q2 1 0.4991 0.3371 0.5006 11.00000 0.05 0.43 Q3 1 0.3597 0.4064 0.5117 11.00000 0.05 0.40 Q4 1 0.4122 0.5910 0.4727 11.00000 0.05 0.39 Q5 1 0.4968 0.3419 0.9996 11.00000 0.05 0.37 Q6 1 0.5307 0.3527 0.4573 11.00000 0.05 0.34 Q7 1 0.5743 0.5888 1.0256 11.00000 0.05 0.34 Q8 1 0.4787 0.6417 1.0394 11.00000 0.05 0.32 Q9 1 0.3214 0.4012 0.5828 11.00000 0.05 0.31 Q10 1 0.5686 0.4209 1.0242 11.00000 0.05 0.30 Q11 1 0.1241 0.0048 0.6251 11.00000 0.05 0.29 Q12 1 0.6767 0.5945 0.9163 11.00000 0.05 0.29 Q13 1 0.8665 0.1984 0.4710 11.00000 0.05 0.27 Q14 1 0.5787 0.2926 0.4548 11.00000 0.05 0.26 Q15 1 0.3395 0.0001 0.5943 11.00000 0.05 0.25 Q16 1 0.8242 0.5006 0.1863 11.00000 0.05 0.25 Q17 1 0.6851 0.5016 0.4919 11.00000 0.05 0.24 Q18 1 0.7349 0.4883 0.4372 11.00000 0.05 0.22 Q19 1 0.4760 0.5838 0.4159 11.00000 0.05 0.21 Q20 1 0.3727 0.4164 1.0128 11.00000 0.05 0.20 ; _shelx_res_checksum 10206 _shelx_hkl_file ; 0 -1 6 30255.1 1085.52 1 0 -1 7 16348.0 834.919 1 0 -1 8 20081.4 924.621 1 0 -1 9 1029.70 213.511 1 0 -1 10 3530.05 397.073 1 0 -1 11 43.3072 71.3789 1 0 -1 12-7.49837 51.5415 1 0 -1 13 2566.74 349.444 1 0 -1 14 10.6909 57.0101 1 0 -1 15 216.651 119.184 1 0 -2 -4 164745. 2182.21 1 0 -2 -5 24412.0 825.041 1 0 -2 9 619.442 228.384 1 0 -2 10 40510.0 1679.24 1 0 -2 11-21.6862 71.0099 1 0 -2 12 8032.96 760.977 1 0 -2 13-57.6233 98.3937 1 0 -2 14 13216.5 971.038 1 0 -2 15 246.105 177.471 1 0 -2 16 3197.94 459.998 1 0 -2 17-177.969 145.986 1 0 -2 18 205.818 130.542 1 0 -3 -5 3611.79 415.914 1 0 -3 -6 1307.47 242.226 1 0 -3 -7 41302.0 1283.43 1 0 -3 -8 1591.45 236.755 1 0 -3 -9 19893.4 767.673 1 0 -3 12 47.4320 57.0795 1 0 -3 13 3810.02 616.992 1 0 -3 14-64.1048 151.220 1 0 -3 15 177.825 148.470 1 0 -3 16 75.2021 111.153 1 0 -3 17 81.5038 86.6823 1 0 -3 18-83.3212 149.675 1 0 -3 19-122.515 152.449 1 0 -4 -6 71530.7 2228.17 1 0 -4 -7 3821.53 489.295 1 0 -4 -8 46728.8 1647.78 1 0 -4 -9-2.95152 33.5407 1 0 -4 -10 32144.8 1253.76 1 0 -4 -11 15.2789 68.5218 1 0 -4 18 465.709 248.728 1 0 -5 -8 774.865 234.467 1 0 -5 -9-26.4634 100.457 1 0 -5 -10 1304.78 328.829 1 0 -5 -11 8689.62 773.909 1 0 -5 -12 11.2880 28.3175 1 0 -5 -13-0.51980 40.6547 1 0 -6 -9 336.369 174.024 1 0 -6 -10 7788.15 880.712 1 0 -6 -11-16.6094 67.9903 1 0 -6 -12 1858.59 428.629 1 0 -6 -13 70.4304 108.080 1 0 -6 -14 1118.13 314.162 1 0 -7 -11 85.3508 135.386 1 0 -7 -12 28.0197 84.7331 1 0 -7 -13 352.907 154.262 1 0 -7 -14 55.5247 154.826 1 0 -7 -15 79.3335 124.156 1 0 -8 -12 2019.18 552.741 1 0 -8 -13 23.1733 157.933 1 0 -8 -14 136.859 123.613 1 0 -8 -15-18.5376 101.312 1 0 -8 -16 158.643 80.0497 1 0 -9 -15-123.405 142.023 1 -1 0 9 10257.3 645.057 1 -1 0 8 37.0554 56.5856 1 1 0 -8-8.24351 42.2490 1 1 0 -7 2847.20 287.519 1 -1 0 7 2269.84 309.020 1 -1 0 6-19.8458 49.4401 1 1 0 -6 8.25284 8.77721 1 1 0 -5 66378.9 1395.22 1 -1 0 5 71913.0 1574.07 1 -1 0 4-3.40711 14.3871 1 1 0 -4-5.54626 9.02148 1 -1 0 3 132300. 2163.05 1 1 0 -3 124308. 1993.84 1 1 0 -2-15.0544 36.9347 1 -1 0 2 4.95630 38.9737 1 -1 -1 14 5573.40 590.072 1 -1 -1 13 145.581 132.518 1 -1 -1 12 4387.82 534.292 1 -1 -1 11 16.3784 23.3874 1 -1 -1 10 91605.7 2289.12 1 -1 -1 9 31.8967 36.4595 1 -1 -1 8 101449. 2310.66 1 -1 -1 7 14355.7 855.502 1 1 1 -7 13362.3 801.861 1 1 1 -6 55264.2 1613.98 1 -1 -1 6 57429.9 1662.18 1 1 1 -5 129367. 2332.37 1 -1 -1 5 140280. 2536.14 1 1 1 -4 71335.9 1727.18 1 -1 -1 4 71547.0 1784.29 1 1 1 -3 138012. 2330.30 1 -1 -1 3 134534. 2362.86 1 -1 -1 2 214308. 2899.69 1 -1 -1 1 695.112 156.036 1 1 1 -1 529.809 137.507 1 -1 -1 -1 963.473 181.114 1 1 1 1 911.480 167.691 1 -1 -1 -2 320205. 3387.35 1 1 1 3 7479.46 491.023 1 -1 -1 -3 8589.91 540.806 1 -1 -1 -4 60258.7 1458.23 1 1 1 4 58602.7 1337.74 1 1 1 5 3090.54 309.649 1 1 -1 13 25.1786 22.5628 1 1 -1 14 7987.69 613.256 1 1 -1 15 19.0499 368.374 1 1 -1 16 4691.66 413.829 1 -1 -2 17 203.504 152.907 1 -1 -2 16-70.4455 94.7888 1 -1 -2 15 187.129 161.709 1 -1 -2 14 227.277 113.532 1 -1 -2 13 1090.51 304.489 1 -1 -2 12 17.9202 41.2941 1 -1 -2 11 1027.15 296.193 1 -1 -2 10 84.6258 136.696 1 -1 -2 9 24986.1 1364.84 1 -1 -2 8 6703.88 692.138 1 -1 -2 7 562.729 213.972 1 1 2 -6 6931.23 680.764 1 -1 -2 6 7414.89 721.494 1 -1 -2 5 7572.79 710.140 1 1 2 -5 8000.94 706.794 1 1 2 -4 4917.48 542.902 1 -1 -2 4 4960.07 545.746 1 1 2 -3 22658.3 1137.78 1 -1 -2 3 22186.3 1143.47 1 -1 -2 2 173199. 3119.58 1 1 2 -2 176686. 3075.97 1 -1 -2 1 226345. 3484.17 1 1 2 -1 225133. 3396.88 1 -1 -2 0 84042.1 2056.24 1 1 2 0 83616.7 2027.65 1 1 2 1 19331.5 955.837 1 -1 -2 -1 19417.2 976.273 1 -1 -2 -2 40383.7 1372.66 1 1 2 2 40364.0 1327.61 1 -1 -2 -3 72407.1 1805.29 1 1 2 3 72806.0 1724.64 1 -1 -2 -4 9433.02 651.836 1 1 2 4 9606.97 603.835 1 1 2 5 30.7953 47.5371 1 -1 -2 -5 85.1479 72.7182 1 1 2 6 1119.38 178.023 1 -1 -2 -6 1650.98 270.651 1 1 2 7 342.165 98.3634 1 -1 -2 -7 447.992 140.820 1 1 2 8 2475.19 233.986 1 1 -2 16 14.6360 29.2752 1 1 -2 17 22.2355 23.8375 1 1 -2 18 15.0538 30.5927 1 1 -2 19-7.64350 29.7054 1 -1 -3 19-93.7258 137.435 1 -1 -3 18 235.983 218.655 1 -1 -3 17-148.740 179.103 1 -1 -3 16 1724.49 431.540 1 -1 -3 15 109.885 152.860 1 -1 -3 14 6300.45 828.483 1 -1 -3 13 2278.40 493.192 1 -1 -3 12 4325.74 696.720 1 -1 -3 11 574.564 257.011 1 1 -3 -10 54713.5 1134.77 1 -1 -3 10 52837.6 2308.94 1 -1 -3 9 69.1210 51.7269 1 -1 -3 8 78939.3 2717.56 1 -1 -3 7 3277.37 548.072 1 -1 -3 6 82603.1 2720.42 1 1 3 -5 2555.12 463.662 1 -1 -3 5 3066.80 517.243 1 1 3 -4 136864. 3416.09 1 -1 -3 4 142136. 3486.91 1 -1 -3 3 62432.1 2208.97 1 1 3 -3 60336.9 2195.63 1 -1 -3 2 82195.5 2511.67 1 1 3 -2 84751.2 2509.73 1 1 3 -1 849.991 264.921 1 -1 -3 1 903.737 249.576 1 -1 -3 0 439097. 5646.49 1 1 3 0 483083. 5885.92 1 1 3 1 9816.04 816.238 1 -1 -3 -1 11678.1 905.937 1 1 3 2 6979.12 664.776 1 -1 -3 -2 7003.40 688.334 1 1 3 3 72024.4 2109.97 1 -1 -3 -3 80337.6 2250.74 1 1 3 4 18550.0 1034.07 1 -1 -3 -4 20375.4 1117.40 1 1 3 5-7.16201 64.3901 1 -1 -3 -5 29.6532 77.0146 1 -1 -3 -6 146397. 2845.54 1 1 3 6 141298. 2615.79 1 -1 -3 -7 1036.59 236.726 1 1 3 7 405.160 110.505 1 -1 -3 -8 59511.2 1825.31 1 -1 -3 -9 229.176 120.512 1 -1 -4 19 22.1555 85.6195 1 -1 -4 18-64.2065 169.219 1 -1 -4 17 410.554 258.252 1 -1 -4 16 141.985 173.091 1 -1 -4 15 24.0457 106.402 1 -1 -4 14 21.8186 100.331 1 -1 -4 13-48.8780 151.081 1 -1 -4 12-120.021 461.698 1 1 -4 -12 19.3377 22.1081 1 1 -4 -11 636.908 158.803 1 -1 -4 11 302.654 196.653 1 -1 -4 10 12.4658 31.2722 1 -1 -4 9 679.703 284.662 1 -1 -4 8 2228.57 521.194 1 -1 -4 7 11091.4 1139.75 1 -1 -4 6-4.91603 50.6611 1 -1 -4 5 7283.17 896.628 1 -1 -4 4 13819.1 1204.11 1 -1 -4 3 1891.37 443.381 1 -1 -4 2 39065.1 1957.10 1 1 4 -2 37437.2 1925.56 1 1 4 -1 44095.8 2086.35 1 -1 -4 1 42921.5 2074.69 1 1 4 0 1233.37 328.888 1 -1 -4 0 1312.49 344.691 1 1 4 1 7495.35 826.236 1 -1 -4 -1 8787.74 898.592 1 -1 -4 -2 1795.24 392.203 1 1 4 2 1727.13 392.972 1 -1 -4 -3 2593.01 456.980 1 1 4 3 2740.04 469.429 1 -1 -4 -4 24971.2 1445.63 1 1 4 4 24636.8 1374.45 1 -1 -4 -5 7284.00 764.388 1 -1 -4 -6 13910.5 1027.82 1 -1 -4 -7 7371.65 735.612 1 -1 -4 -8 3773.31 535.236 1 -1 -4 -9 2898.63 458.082 1 -1 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1765.59 1 -7 -7 -2 9568.96 1781.77 1 7 7 3 107.628 206.215 1 -7 -7 -3 304.685 244.583 1 7 7 4 3708.47 941.107 1 -7 -7 -4 2907.95 910.931 1 7 7 5 238.368 242.613 1 -7 -7 -5 179.435 347.511 1 7 7 6 7321.61 1377.87 1 -7 -7 -6 5346.82 1415.60 1 7 7 7-278.429 369.783 1 -7 -7 -7 124.231 306.907 1 7 7 8 4531.89 1030.11 1 -7 -7 -8 3477.25 1074.43 1 7 7 9 303.809 272.892 1 -7 -7 -9 7.37163 260.954 1 7 7 10 3953.14 921.645 1 -7 -7 -10 2614.03 975.911 1 7 7 11 175.502 263.933 1 -7 -7 -11 151.424 304.572 1 7 7 12 581.951 408.231 1 7 7 13 58.7361 206.134 1 7 7 14 495.354 284.922 1 7 7 15 96.8393 114.632 1 7 7 16 259.324 194.028 1 -7 -8 6 4.36631 224.079 1 7 8 -6-40.1908 134.710 1 7 8 -5-152.877 153.747 1 -7 -8 5-302.710 396.599 1 -7 -8 4-149.740 233.296 1 7 8 -4 79.7224 57.8526 1 -7 -8 3 417.201 521.437 1 7 8 -3 96.2851 197.220 1 -7 -8 2 229.365 303.259 1 7 8 -2 56.6964 214.178 1 -7 -8 1 447.414 471.701 1 7 8 -1 371.152 375.589 1 -7 -8 0 88.2171 271.042 1 7 8 0 13.5835 205.254 1 7 8 1 557.001 465.224 1 -7 -8 -1 363.204 325.038 1 7 8 2 75.2769 225.753 1 -7 -8 -2-176.686 363.272 1 7 8 3-22.4531 128.872 1 -7 -8 -3-4.05837 149.629 1 7 8 4 141.391 178.528 1 -7 -8 -4-154.760 325.096 1 7 8 5 33.8358 94.0341 1 -7 -8 -5-3.93415 102.565 1 7 8 6-219.495 218.224 1 -7 -8 -6-131.471 324.709 1 7 8 7 108.604 283.756 1 -7 -8 -7 154.291 411.563 1 7 8 8-28.7148 129.663 1 -7 -8 -8-137.510 149.374 1 -7 -8 -9 317.670 272.378 1 7 8 9 47.4996 89.2146 1 -7 -8 -10 284.812 392.904 1 7 8 10-226.602 237.197 1 -7 -8 -11 3.84013 50.0570 1 7 8 11 49.4286 174.569 1 7 8 12 72.3058 139.792 1 -7 -8 -12 53.1884 257.330 1 7 8 13-46.7079 201.933 1 -7 -8 -13-204.706 362.619 1 7 8 14-29.2397 113.552 1 7 8 15 58.6962 193.238 1 7 9 1 94.7327 235.087 1 -7 -9 -1-48.7012 223.518 1 7 9 2 2972.03 994.879 1 -7 -9 -2 1266.63 735.917 1 -7 -9 -3 393.686 442.900 1 7 9 3 381.387 422.968 1 7 9 4 876.527 531.850 1 -7 -9 -4 634.089 499.993 1 7 9 5 53.5511 287.748 1 -7 -9 -5 426.745 440.646 1 7 9 6 886.998 546.029 1 -7 -9 -6 1402.97 767.545 1 7 9 7 1217.74 576.524 1 -7 -9 -7 194.997 370.765 1 7 9 8 666.526 511.881 1 -7 -9 -8 202.688 261.554 1 7 9 9 169.946 253.355 1 -7 -9 -9 125.778 134.840 1 7 9 10 1730.87 648.016 1 -7 -9 -10 685.756 458.061 1 7 9 11 362.107 415.539 1 -7 -9 -11 115.964 198.376 1 7 9 12 807.647 433.366 1 -7 -9 -12 476.651 537.559 1 -7 -9 -13 59.2709 485.920 1 7 9 13 7.76258 119.250 1 7 9 14 161.275 62.4282 1 -7 -9 -14 721.022 511.690 1 7 9 15-201.670 93.1330 1 7 10 12-35.5568 125.157 1 -7 -10 -12-112.048 63.8866 1 7 10 13-152.254 300.827 1 -7 -10 -13 45.7155 304.050 1 7 10 14-247.366 236.417 1 -7 -10 -14-189.716 237.401 1 8 0 -16 469.032 361.571 1 8 1 -16 108.718 75.4636 1 8 1 -15 406.092 373.928 1 8 1 -14 536.151 352.403 1 8 1 -13 5.38680 212.113 1 8 1 -12-80.5148 252.039 1 8 1 -11 235.418 250.455 1 8 2 -17 93.2131 274.273 1 8 2 -16 1046.19 537.663 1 8 2 -15-74.7178 94.9929 1 8 2 -14 1716.01 672.169 1 8 2 -13-89.8226 96.8065 1 8 2 -12 1053.58 471.859 1 8 2 -11-11.6432 113.829 1 8 2 -10 2060.80 807.064 1 8 2 -9 166.166 280.255 1 8 2 -8 11245.7 1772.86 1 8 2 -7 262.138 203.395 1 8 3 -17 14.9837 32.5527 1 8 3 -16-18.5294 42.2600 1 8 3 -15-89.2510 122.126 1 8 3 -14 108.879 166.767 1 8 3 -13 257.599 300.800 1 8 3 -12 363.639 287.550 1 8 3 -11 36.4304 92.8077 1 8 3 -10 126.515 421.078 1 8 3 -9 270.843 295.525 1 8 3 -8 607.228 405.860 1 -8 -3 8 599.671 413.005 1 8 3 -7 863.283 412.746 1 -8 -3 7 1213.09 641.336 1 8 3 -6-102.070 133.721 1 -8 -3 6 178.078 234.486 1 8 3 -5-47.3473 207.775 1 -8 -3 5-50.8547 66.9634 1 8 3 -4 144.217 164.471 1 -8 -3 4 261.177 435.945 1 8 3 -3 618.289 428.924 1 -8 -3 3 662.445 523.324 1 8 3 -2 2177.40 799.080 1 8 4 -17 68.6969 180.879 1 8 4 -16 590.690 474.782 1 8 4 -15 46.8669 26.9992 1 -8 -4 14 920.995 624.023 1 8 4 -14 399.103 409.957 1 8 4 -13 63.6400 142.430 1 -8 -4 13-15.4213 319.823 1 8 4 -12 1157.99 535.890 1 -8 -4 12 358.332 344.326 1 8 4 -11 231.548 338.808 1 -8 -4 11 179.826 312.544 1 -8 -4 10 2276.37 975.950 1 8 4 -10 3060.73 922.713 1 -8 -4 9 60.1574 227.874 1 8 4 -9 196.353 269.797 1 8 4 -8 12701.1 1910.73 1 -8 -4 8 8690.01 1754.25 1 -8 -4 7 23.8706 89.8241 1 8 4 -7-263.213 259.623 1 8 4 -6 1266.81 544.955 1 -8 -4 6 683.247 534.372 1 8 4 -5 903.214 507.271 1 -8 -4 5 257.521 344.508 1 8 4 -4 5824.83 1371.41 1 -8 -4 4 6261.16 1505.59 1 8 4 -3 5390.53 1220.72 1 -8 -4 3 3895.41 1134.80 1 8 4 -2 7722.15 1452.71 1 -8 -4 2 6326.03 1474.69 1 8 4 -1 330.217 398.067 1 -8 -4 1 70.6754 95.7523 1 -8 -4 0 11893.3 2155.85 1 8 4 0 15416.4 2060.04 1 8 4 1 3582.86 1093.88 1 -8 -4 -1 3271.55 1098.69 1 -8 -4 -2 19107.2 2685.10 1 8 4 2 18059.9 2381.77 1 8 4 3 922.827 553.881 1 -8 -4 -3 766.052 573.555 1 8 4 4 918.766 548.107 1 8 4 5-12.1757 104.979 1 8 4 6 6556.27 1421.95 1 8 4 7 358.265 383.749 1 8 5 -16 33.7484 135.622 1 8 5 -15 261.407 307.924 1 -8 -5 15 104.364 272.081 1 8 5 -14-54.2954 121.379 1 -8 -5 14 797.597 551.473 1 -8 -5 13-257.353 347.815 1 8 5 -13 253.049 326.204 1 -8 -5 12-88.7507 216.889 1 8 5 -12 61.9579 216.745 1 8 5 -11 472.523 397.115 1 -8 -5 11 63.4108 304.328 1 8 5 -10 247.460 261.616 1 -8 -5 10-99.8238 369.717 1 8 5 -9 110.417 256.184 1 -8 -5 9-28.9279 258.347 1 8 5 -8 127.310 75.6413 1 -8 -5 8 162.266 83.6099 1 -8 -5 7 3.96548 236.878 1 8 5 -7-73.0903 310.785 1 -8 -5 6 3.95246 233.273 1 8 5 -6 157.955 181.818 1 -8 -5 5-74.7641 223.581 1 8 5 -5-212.631 278.250 1 -8 -5 4-19.5689 80.6653 1 8 5 -4 76.6625 181.758 1 8 5 -3 165.900 273.543 1 -8 -5 3 87.3697 325.354 1 8 5 -2 9.86805 142.209 1 -8 -5 2-449.632 427.067 1 8 5 -1 1619.55 698.708 1 -8 -5 1 235.215 431.675 1 8 5 0-3.26772 112.697 1 -8 -5 0 4.01876 82.8288 1 8 5 1 248.306 404.459 1 -8 -5 -1-762.199 593.583 1 8 5 2 126.563 172.538 1 -8 -5 -2 226.065 427.501 1 8 5 3 78.8278 275.718 1 -8 -5 -3 76.8494 268.840 1 8 5 4 328.890 327.330 1 -8 -5 -4 742.485 636.661 1 8 5 5 3.05070 93.2611 1 -8 -5 -5 290.414 266.955 1 8 5 6-332.631 323.299 1 -8 -5 -6-162.071 295.451 1 8 5 7 182.293 246.901 1 8 5 8 241.978 239.057 1 8 5 9 220.883 172.606 1 8 5 10 60.0328 216.365 1 8 5 11 61.0231 156.590 1 8 5 12-35.4618 123.543 1 8 5 13-110.853 50.7722 1 8 5 14-30.3550 206.436 1 8 5 15 415.613 375.639 1 8 5 16 60.7038 237.872 1 8 6 -10 854.059 546.581 1 -8 -6 10-297.239 376.689 1 8 6 -9-92.8359 286.916 1 -8 -6 9 21.7333 226.640 1 8 6 -8 2710.51 916.332 1 -8 -6 8 2157.04 974.667 1 8 6 -7 169.572 287.585 1 -8 -6 7 207.237 355.938 1 8 6 -6 688.617 566.684 1 -8 -6 6 399.625 466.962 1 8 6 -5-17.6757 156.270 1 -8 -6 5-307.662 219.294 1 8 6 -4 5357.43 1288.18 1 -8 -6 4 3924.14 1205.86 1 -8 -6 3 248.356 357.714 1 8 6 -3 279.184 320.856 1 -8 -6 2 8834.60 1815.23 1 8 6 -2 10494.3 1800.85 1 -8 -6 1 1458.08 754.005 1 8 6 -1 1908.35 760.322 1 8 6 0 13351.3 2028.85 1 -8 -6 0 9680.38 1851.49 1 -8 -6 -1 309.585 318.793 1 8 6 1 3.34621 332.190 1 8 6 2 11626.9 1820.57 1 -8 -6 -2 9232.32 1898.73 1 -8 -6 -3 263.626 402.633 1 8 6 3 149.081 295.720 1 -8 -6 -4 1032.65 610.420 1 8 6 4 2247.16 818.534 1 -8 -6 -5-150.682 306.220 1 8 6 5 144.156 304.327 1 -8 -6 -6 5614.11 1638.04 1 8 6 6 8369.70 1505.83 1 -8 -6 -7 20.7998 411.189 1 8 6 7-12.0165 83.0702 1 -8 -6 -8 1083.90 725.891 1 8 6 8 1647.24 726.720 1 8 6 9-2.88296 79.7194 1 8 6 10 1122.65 571.732 1 8 6 11-152.549 234.310 1 8 6 12 197.439 277.642 1 8 6 13-17.4172 119.170 1 8 6 14 434.901 300.386 1 8 6 15-224.257 248.045 1 8 6 16 151.220 202.120 1 8 7 -5 154.347 261.974 1 -8 -7 5-4.54491 138.940 1 8 7 -4 452.901 423.247 1 -8 -7 4 153.265 431.799 1 8 7 -3-238.958 314.241 1 -8 -7 3 187.607 417.853 1 8 7 -2 142.258 240.105 1 -8 -7 2-278.628 323.563 1 8 7 -1 1078.45 597.920 1 -8 -7 1 1000.41 660.427 1 8 7 0-68.1447 140.255 1 -8 -7 0 244.690 504.641 1 8 7 1 42.3344 112.644 1 -8 -7 -1 157.591 258.360 1 8 7 2-13.9015 64.0671 1 -8 -7 -2-486.517 243.549 1 8 7 3 64.8555 220.240 1 -8 -7 -3 149.980 315.981 1 8 7 4 103.841 250.833 1 -8 -7 -4 104.812 228.618 1 8 7 5-321.840 314.580 1 -8 -7 -5-32.7479 113.193 1 8 7 6 106.141 78.4375 1 -8 -7 -6-299.141 215.746 1 8 7 7-232.339 238.644 1 -8 -7 -7 82.1426 132.165 1 8 7 8 395.639 383.463 1 -8 -7 -8 12.9561 199.034 1 8 7 9-92.6899 347.515 1 -8 -7 -9 34.3954 262.870 1 8 7 10 92.5128 159.885 1 -8 -7 -10 66.2789 293.283 1 8 7 11 287.479 239.957 1 8 7 12 126.045 188.255 1 8 7 13 387.130 351.235 1 8 7 14 26.8985 59.6334 1 8 7 15 147.871 236.995 1 8 7 16-118.161 213.558 1 8 8 1-105.251 162.512 1 8 8 2 7385.02 1571.07 1 -8 -8 -2 4762.53 1384.13 1 8 8 3 105.369 160.615 1 -8 -8 -3-534.081 504.088 1 8 8 4 637.454 510.632 1 -8 -8 -4 484.440 539.462 1 8 8 5 24.4076 160.694 1 -8 -8 -5 311.608 480.053 1 8 8 6 1892.53 705.620 1 -8 -8 -6 713.770 547.878 1 8 8 7-63.0626 273.633 1 -8 -8 -7 552.319 553.909 1 8 8 8 772.674 499.524 1 -8 -8 -8 75.6592 278.225 1 8 8 9-22.0301 287.169 1 -8 -8 -9 130.701 366.887 1 8 8 10 586.095 363.074 1 -8 -8 -10 161.009 276.541 1 -8 -8 -11 105.998 135.017 1 8 8 11-459.778 327.274 1 -8 -8 -12-4.14401 451.949 1 8 8 12 470.991 404.194 1 8 8 13 147.805 217.029 1 8 8 14-119.127 71.6108 1 8 8 15-2.41308 260.337 1 8 9 13-137.208 220.521 1 -8 -9 -13-648.809 670.079 1 8 9 14 145.779 313.595 1 8 9 15 73.3752 200.641 1 9 2 -16 126.612 245.966 1 9 2 -15 195.590 302.560 1 9 2 -14 112.479 221.669 1 9 2 -13 137.642 88.5134 1 9 2 -12-52.4707 241.820 1 9 2 -11 183.326 435.576 1 9 3 -16 477.970 385.359 1 9 3 -15 298.229 200.471 1 9 3 -14 164.944 234.730 1 9 3 -13-254.256 399.162 1 9 3 -12 501.729 377.372 1 9 3 -11-195.990 202.935 1 9 3 -10 290.004 198.528 1 9 3 -9-281.914 421.226 1 9 3 -8 5489.45 1353.37 1 9 3 -7-251.475 401.477 1 9 3 -6 1025.00 556.627 1 9 4 -13-86.1846 155.668 1 9 4 -12-14.1726 219.079 1 9 4 -11 171.112 143.226 1 -9 -4 10-596.590 595.623 1 9 4 -10 287.473 320.975 1 -9 -4 9 386.572 277.776 1 9 4 -9 98.7438 82.5708 1 -9 -4 8-409.521 423.015 1 9 4 -8 151.086 299.980 1 -9 -4 7-108.168 287.815 1 9 4 -7 96.9717 238.176 1 9 4 -6 209.218 294.223 1 -9 -4 6 576.971 577.202 1 9 4 -5 41.1734 103.502 1 -9 -4 5 4.50293 166.020 1 9 4 -4-133.226 156.315 1 -9 -4 4 44.9383 82.8422 1 9 4 -3-448.365 374.159 1 -9 -4 3 112.027 330.428 1 9 4 -2 132.965 198.508 1 -9 -4 2-4.42259 313.118 1 9 4 -1 3.73503 220.440 1 -9 -4 1 87.4010 161.121 1 9 4 0 837.520 605.280 1 -9 -5 8 4739.75 1409.83 1 9 5 -8 7471.70 1569.61 1 -9 -5 7 330.157 173.325 1 9 5 -7 353.416 311.361 1 -9 -5 6 985.618 663.529 1 9 5 -6 2393.64 863.775 1 -9 -5 5-1016.59 646.600 1 9 5 -5 15.5382 62.0162 1 9 5 -4 2828.22 961.386 1 -9 -5 4 2301.79 991.502 1 9 5 -3 150.613 371.634 1 -9 -5 3 119.822 481.921 1 9 5 -2 8562.01 1737.64 1 -9 -5 2 6019.09 1652.04 1 9 5 -1 104.641 128.889 1 -9 -5 1 57.3822 271.702 1 9 5 0 4381.13 1202.82 1 -9 -5 0 3138.39 1185.19 1 9 5 1-22.5674 84.9202 1 -9 -5 -1-4.74051 214.060 1 9 5 2 4925.62 1295.97 1 -9 -5 -2 3780.44 1268.26 1 9 5 3-806.110 594.297 1 -9 -5 -3 408.358 573.673 1 9 5 4 1778.67 783.123 1 -9 -5 -4 1250.36 674.978 1 9 5 5 250.957 166.937 1 9 5 6 3058.93 1015.76 1 9 5 7 174.858 392.054 1 9 5 8 1093.41 587.850 1 9 5 9 445.692 404.136 1 -9 -6 3-720.421 615.267 1 9 6 -3 24.2027 64.3989 1 -9 -6 2-195.972 263.316 1 9 6 -2-435.393 455.676 1 -9 -6 1-563.469 502.907 1 9 6 -1 7.82027 108.123 1 -9 -6 0 29.3833 259.305 1 9 6 0-35.2852 213.790 1 -9 -6 -1 592.743 462.071 1 9 6 1 134.211 360.447 1 -9 -6 -2 24.6373 157.332 1 9 6 2 86.8516 344.562 1 -9 -6 -3 172.042 450.805 1 9 6 3 238.697 464.106 1 -9 -6 -4 367.343 508.765 1 9 6 4 173.298 349.022 1 -9 -6 -5 311.394 563.720 1 9 6 5 395.992 346.427 1 -9 -6 -6-518.682 506.854 1 9 6 6-577.651 522.138 1 9 6 7 327.413 397.640 1 9 6 8 300.594 338.171 1 9 6 9 89.7865 308.044 1 9 6 10 329.381 429.175 1 9 6 11-214.081 359.469 1 9 6 12-3.03253 209.172 1 9 6 13 8.92614 281.023 1 9 6 14-157.031 160.600 1 9 6 15 78.9428 168.041 1 9 7 6 1074.53 582.607 1 -9 -7 -7 573.780 486.566 1 9 7 7 120.071 318.163 1 9 7 9-159.669 187.880 1 9 7 10-197.866 254.315 1 9 7 11-252.513 244.729 1 9 7 12 130.096 273.849 1 9 7 13-201.082 239.174 1 9 7 14 379.765 452.831 1 9 7 15 172.799 177.726 1 0 0 0 0.00 0.00 0 TITL EtaKCrF_c3_p03_f4_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 8.324659 8.891645 12.338062 90.0000 87.3787 90.0000 ZERR 2.00 0.001733 0.001450 0.001434 0.0000 0.0112 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 12467 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 0.0444(3) Uani 1 2 d S . P . . K1 K 0.500000 0.500000 1.000000 0.0499(4) Uani 1 2 d S . P . . C1 C 0.7724(7) 0.3044(6) 0.4495(4) 0.0651(14) Uani 1 1 d . U . . . H1 H 0.734269 0.252167 0.510748 0.078 Uiso 1 1 calc R U . . . C2 C 0.3257(7) 0.2141(6) 0.5102(4) 0.0674(14) Uani 1 1 d . U . . . H2 H 0.267245 0.251244 0.453543 0.081 Uiso 1 1 calc R U . . . C3 C 0.5817(7) 0.4875(5) 0.7259(4) 0.0572(12) Uani 1 1 d . U . . . H3 H 0.476610 0.453610 0.737252 0.069 Uiso 1 1 calc R U . . . O1 O 0.6901(4) 0.4153(4) 0.4197(2) 0.0579(9) Uani 1 1 d . U . . . O2 O 0.8994(5) 0.2591(4) 0.4044(3) 0.0747(12) Uani 1 1 d . U . . . O3 O 0.4324(4) 0.2976(4) 0.5477(2) 0.0567(9) Uani 1 1 d . U . . . O4 O 0.2946(6) 0.0881(5) 0.5434(4) 0.0900(14) Uani 1 1 d . U . . . O5 O 0.6287(5) 0.5153(3) 0.6301(2) 0.0555(9) Uani 1 1 d . U . . . O6 O 0.6627(5) 0.5011(4) 0.8062(3) 0.0731(12) Uani 1 1 d . U . . . N1 N 1.0113(6) 0.4289(6) 0.2253(4) 0.0694(13) Uani 1 1 d . U . . . H1A H 0.982847 0.374038 0.283353 0.104 Uiso 1 1 calc R U . . . H1B H 1.117766 0.438500 0.220469 0.104 Uiso 1 1 calc R U . . . H1C H 0.978188 0.383618 0.165946 0.104 Uiso 1 1 calc R U . . . C4 C 0.9368(10) 0.5788(8) 0.2353(6) 0.094(2) Uani 1 1 d . U . . . H4A H 0.964989 0.637270 0.170803 0.113 Uiso 1 1 calc R U . . . H4B H 0.820698 0.568105 0.240338 0.113 Uiso 1 1 calc R U . . . C5 C 0.9888(12) 0.6571(9) 0.3293(8) 0.131(3) Uani 1 1 d . U . . . H5A H 1.098040 0.689650 0.316713 0.196 Uiso 1 1 calc R U . . . H5B H 0.982051 0.591064 0.390895 0.196 Uiso 1 1 calc R U . . . H5C H 0.921107 0.743053 0.343183 0.196 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 0.0355(8) 0.0548(8) 0.0427(5) 0.0035(3) 0.0011(4) 0.0017(3) K1 0.0413(11) 0.0583(11) 0.0495(6) -0.0025(5) 0.0031(6) 0.0004(5) C1 0.056(4) 0.073(4) 0.065(3) 0.010(2) 0.012(2) 0.009(2) C2 0.066(5) 0.062(4) 0.075(3) 0.010(2) -0.009(3) -0.008(2) C3 0.044(4) 0.078(4) 0.050(2) 0.0058(18) -0.002(2) -0.0024(19) O1 0.050(3) 0.069(3) 0.0536(15) 0.0084(14) 0.0070(15) 0.0099(14) O2 0.064(3) 0.073(3) 0.084(2) 0.0115(19) 0.022(2) 0.0179(17) O3 0.054(3) 0.061(2) 0.0557(16) 0.0032(13) -0.0045(15) -0.0050(14) O4 0.096(4) 0.068(3) 0.108(3) 0.022(2) -0.024(3) -0.028(2) O5 0.048(3) 0.072(3) 0.0464(14) 0.0066(12) -0.0004(14) -0.0032(13) O6 0.043(3) 0.131(4) 0.0457(16) 0.0079(15) -0.0022(16) -0.0093(16) N1 0.058(4) 0.091(4) 0.060(2) -0.004(2) 0.000(2) -0.011(2) C4 0.070(6) 0.104(6) 0.106(4) 0.031(4) 0.016(4) 0.006(3) C5 0.125(8) 0.092(6) 0.171(8) -0.038(6) 0.033(6) -0.022(5) 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 180.0 . 3_666 ? O3 Cr1 O5 88.75(13) . . ? O3 Cr1 O5 91.25(13) 3_666 . ? O3 Cr1 O5 91.25(13) . 3_666 ? O3 Cr1 O5 88.75(13) 3_666 3_666 ? O5 Cr1 O5 180.0 . 3_666 ? O3 Cr1 O1 90.76(14) . . ? O3 Cr1 O1 89.25(14) 3_666 . ? O5 Cr1 O1 88.98(14) . . ? O5 Cr1 O1 91.02(14) 3_666 . ? O3 Cr1 O1 89.24(14) . 3_666 ? O3 Cr1 O1 90.76(14) 3_666 3_666 ? O5 Cr1 O1 91.02(14) . 3_666 ? O5 Cr1 O1 88.98(14) 3_666 3_666 ? O1 Cr1 O1 180.0 . 3_666 ? O4 K1 O4 180.0 4_666 2_556 ? O4 K1 O6 104.60(14) 4_666 3_667 ? O4 K1 O6 75.40(14) 2_556 3_667 ? O4 K1 O6 75.41(14) 4_666 . ? O4 K1 O6 104.59(14) 2_556 . ? O6 K1 O6 180.0 3_667 . ? O4 K1 O2 98.19(13) 4_666 4_566 ? O4 K1 O2 81.81(13) 2_556 4_566 ? O6 K1 O2 103.19(10) 3_667 4_566 ? O6 K1 O2 76.81(10) . 4_566 ? O4 K1 O2 81.81(13) 4_666 2_656 ? O4 K1 O2 98.19(13) 2_556 2_656 ? O6 K1 O2 76.81(10) 3_667 2_656 ? O6 K1 O2 103.19(10) . 2_656 ? O2 K1 O2 180.00(9) 4_566 2_656 ? O4 K1 C2 160.26(13) 4_666 2_556 ? O4 K1 C2 19.74(13) 2_556 2_556 ? O6 K1 C2 69.95(13) 3_667 2_556 ? O6 K1 C2 110.05(13) . 2_556 ? O2 K1 C2 101.53(14) 4_566 2_556 ? O2 K1 C2 78.47(14) 2_656 2_556 ? O4 K1 C2 19.74(13) 4_666 4_666 ? O4 K1 C2 160.26(13) 2_556 4_666 ? O6 K1 C2 110.05(13) 3_667 4_666 ? O6 K1 C2 69.95(13) . 4_666 ? O2 K1 C2 78.47(14) 4_566 4_666 ? O2 K1 C2 101.53(14) 2_656 4_666 ? C2 K1 C2 180.0 2_556 4_666 ? O4 K1 C1 70.60(15) 4_666 2_656 ? O4 K1 C1 109.40(15) 2_556 2_656 ? O6 K1 C1 95.90(12) 3_667 2_656 ? O6 K1 C1 84.10(12) . 2_656 ? O2 K1 C1 159.91(10) 4_566 2_656 ? O2 K1 C1 20.09(10) 2_656 2_656 ? C2 K1 C1 90.77(15) 2_556 2_656 ? C2 K1 C1 89.23(15) 4_666 2_656 ? O4 K1 C1 109.40(15) 4_666 4_566 ? O4 K1 C1 70.60(15) 2_556 4_566 ? O6 K1 C1 84.10(12) 3_667 4_566 ? O6 K1 C1 95.90(12) . 4_566 ? O2 K1 C1 20.09(10) 4_566 4_566 ? O2 K1 C1 159.91(10) 2_656 4_566 ? C2 K1 C1 89.23(15) 2_556 4_566 ? C2 K1 C1 90.77(15) 4_666 4_566 ? C1 K1 C1 180.0 2_656 4_566 ? O4 K1 C3 92.63(14) 4_666 . ? O4 K1 C3 87.37(14) 2_556 . ? O6 K1 C3 161.20(13) 3_667 . ? O6 K1 C3 18.80(13) . . ? O2 K1 C3 66.26(11) 4_566 . ? O2 K1 C3 113.74(11) 2_656 . ? C2 K1 C3 96.15(13) 2_556 . ? C2 K1 C3 83.85(13) 4_666 . ? C1 K1 C3 96.92(12) 2_656 . ? C1 K1 C3 83.08(12) 4_566 . ? O4 K1 C3 87.37(14) 4_666 3_667 ? O4 K1 C3 92.63(14) 2_556 3_667 ? O6 K1 C3 18.80(13) 3_667 3_667 ? O6 K1 C3 161.20(13) . 3_667 ? O2 K1 C3 113.74(11) 4_566 3_667 ? O2 K1 C3 66.26(11) 2_656 3_667 ? C2 K1 C3 83.85(13) 2_556 3_667 ? C2 K1 C3 96.15(13) 4_666 3_667 ? C1 K1 C3 83.08(12) 2_656 3_667 ? C1 K1 C3 96.92(12) 4_566 3_667 ? C3 K1 C3 180.0 . 3_667 ? O2 C1 O1 125.8(5) . . ? O2 C1 K1 49.4(3) . 2_646 ? O1 C1 K1 173.7(3) . 2_646 ? O2 C1 H1 117.1 . . ? O1 C1 H1 117.1 . . ? K1 C1 H1 67.9 2_646 . ? O4 C2 O3 124.1(6) . . ? O4 C2 K1 47.4(3) . 2_546 ? O3 C2 K1 160.2(4) . 2_546 ? O4 C2 H2 118.0 . . ? O3 C2 H2 118.0 . . ? K1 C2 H2 73.7 2_546 . ? O6 C3 O5 125.6(5) . . ? O6 C3 K1 44.9(2) . . ? O5 C3 K1 165.0(4) . . ? O6 C3 H3 117.2 . . ? O5 C3 H3 117.2 . . ? K1 C3 H3 73.6 . . ? C1 O1 Cr1 125.6(3) . . ? C1 O2 K1 110.5(3) . 2_646 ? C2 O3 Cr1 128.6(4) . . ? C2 O4 K1 112.9(4) . 2_546 ? C3 O5 Cr1 126.6(4) . . ? C3 O6 K1 116.3(3) . . ? 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 111.4(7) . . ? C5 C4 H4A 109.3 . . ? N1 C4 H4A 109.3 . . ? C5 C4 H4B 109.3 . . ? N1 C4 H4B 109.3 . . ? H4A C4 H4B 108.0 . . ? 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 1.968(3) . ? Cr1 O3 1.968(3) 3_666 ? Cr1 O5 1.975(3) . ? Cr1 O5 1.975(3) 3_666 ? Cr1 O1 1.977(3) . ? Cr1 O1 1.977(3) 3_666 ? K1 O4 2.652(5) 4_666 ? K1 O4 2.652(5) 2_556 ? K1 O6 2.694(3) 3_667 ? K1 O6 2.694(3) . ? K1 O2 2.737(4) 4_566 ? K1 O2 2.737(4) 2_656 ? K1 C2 3.320(6) 2_556 ? K1 C2 3.320(6) 4_666 ? K1 C1 3.378(5) 2_656 ? K1 C1 3.378(5) 4_566 ? K1 C3 3.421(5) . ? K1 C3 3.421(5) 3_667 ? C1 O2 1.239(6) . ? C1 O1 1.266(6) . ? C1 H1 0.9300 . ? C2 O4 1.217(6) . ? C2 O3 1.261(7) . ? C2 H2 0.9300 . ? C3 O6 1.230(6) . ? C3 O5 1.253(5) . ? C3 H3 0.9300 . ? N1 C4 1.473(9) . ? N1 H1A 0.8900 . ? N1 H1B 0.8900 . ? N1 H1C 0.8900 . ? C4 C5 1.438(12) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C5 H5C 0.9600 . ?