#------------------------------------------------------------------------------ #$Date: 2020-03-06 02:55:56 +0200 (Fri, 06 Mar 2020) $ #$Revision: 249096 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/55/74/1557494.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_1557494 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 87.386(7) _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 8.3142(10) _cell_length_b 8.7604(8) _cell_length_c 12.3106(8) _cell_measurement_reflns_used 366 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 14.2730 _cell_measurement_theta_min 2.7830 _cell_volume 895.72(15) _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 '1.25 GPa' _diffrn_ambient_temperature 293(2) _diffrn_detector_area_resol_mean 7 _diffrn_measured_fraction_theta_full 0.683 _diffrn_measured_fraction_theta_max 0.384 _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 0.0320 _diffrn_reflns_av_unetI/netI 0.0545 _diffrn_reflns_Laue_measured_fraction_full 0.683 _diffrn_reflns_Laue_measured_fraction_max 0.384 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_number 3303 _diffrn_reflns_point_group_measured_fraction_full 0.683 _diffrn_reflns_point_group_measured_fraction_max 0.384 _diffrn_reflns_theta_full 14.282 _diffrn_reflns_theta_max 21.682 _diffrn_reflns_theta_min 1.955 _diffrn_source synchrotron _exptl_absorpt_coefficient_mu 0.214 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.93967 _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 1.681 _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 0.606 _refine_diff_density_min -0.649 _refine_diff_density_rms 0.078 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.072 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 123 _refine_ls_number_reflns 2090 _refine_ls_number_restraints 12 _refine_ls_restrained_S_all 1.070 _refine_ls_R_factor_all 0.1156 _refine_ls_R_factor_gt 0.0680 _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 0.1775 _refine_ls_wR_factor_ref 0.2304 _reflns_Friedel_coverage 0.000 _reflns_number_gt 1002 _reflns_number_total 2090 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file jp0c00372_si_002.cif _cod_data_source_block EtaKCrF_c3_p04 _cod_original_cell_volume 895.71(15) _cod_original_sg_symbol_H-M 'P 21/n' _cod_database_code 1557494 _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_p04_f4_152_R15_RO_s2 in P2(1)/n EtaKCrF_c3_p04_f4_152_R15_RO_s2.res created by SHELXL-2016/6 at 14:09:18 on 08-Nov-2018 REM P2(1)/n (#14 with fixed user cell (not necessary: std = user cell)!) CELL 0.41115 8.314179 8.760355 12.310595 90.0000 87.3858 90.0000 ZERR 2.00 0.000997 0.000764 0.000804 0.0000 0.0066 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 0 2 5 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 7.61095 CR1 6 0.500000 0.500000 0.500000 10.50000 0.04072 0.04559 = 0.04390 0.00431 0.00235 0.00148 K1 5 0.500000 0.500000 1.000000 10.50000 0.04600 0.05171 = 0.05212 -0.00451 0.00419 -0.00163 C1 1 0.774887 0.306009 0.449049 11.00000 0.05865 0.06736 = 0.06351 0.01408 0.01347 0.00935 AFIX 43 H1 2 0.738522 0.254389 0.511453 11.00000 -1.20000 AFIX 0 C2 1 0.327077 0.209119 0.507239 11.00000 0.06211 0.05652 = 0.07783 0.00888 -0.00755 -0.01081 AFIX 43 H2 2 0.267722 0.247562 0.451144 11.00000 -1.20000 AFIX 0 C3 1 0.581194 0.483223 0.726193 11.00000 0.05161 0.06519 = 0.05104 0.00468 0.00198 -0.00082 AFIX 43 H3 2 0.476056 0.448347 0.737151 11.00000 -1.20000 AFIX 0 O1 4 0.690370 0.415593 0.418433 11.00000 0.05809 0.06063 = 0.05377 0.01029 0.00958 0.01189 O2 4 0.901543 0.260656 0.403977 11.00000 0.06705 0.06988 = 0.08374 0.01375 0.02175 0.02029 O3 4 0.433625 0.292952 0.545849 11.00000 0.05518 0.05439 = 0.05703 0.00628 -0.00162 -0.00347 O4 4 0.297804 0.079658 0.539865 11.00000 0.09382 0.06381 = 0.10945 0.02023 -0.02337 -0.02456 O5 4 0.628876 0.514149 0.630106 11.00000 0.05379 0.06724 = 0.04693 0.00631 -0.00065 -0.00068 O6 4 0.662221 0.495426 0.806240 11.00000 0.05698 0.12102 = 0.04347 0.00577 -0.00111 -0.01008 N1 3 1.013363 0.432132 0.224397 11.00000 0.06768 0.08055 = 0.05826 -0.00603 -0.00054 -0.00855 AFIX 137 H1A 2 0.986098 0.374901 0.282067 11.00000 -1.50000 H1B 2 1.119754 0.444122 0.219810 11.00000 -1.50000 H1C 2 0.981462 0.386491 0.164481 11.00000 -1.50000 AFIX 0 C4 1 0.935441 0.582088 0.235669 11.00000 0.07192 0.09794 = 0.10171 0.02630 0.01259 0.00383 AFIX 23 H4A 2 0.962903 0.643374 0.171870 11.00000 -1.20000 H4B 2 0.819489 0.568919 0.240218 11.00000 -1.20000 AFIX 0 C5 1 0.984780 0.659594 0.330238 11.00000 0.13123 0.08326 = 0.16018 -0.03149 0.03588 -0.02065 AFIX 137 H5A 2 1.098590 0.678276 0.323796 11.00000 -1.50000 H5B 2 0.960475 0.597731 0.393230 11.00000 -1.50000 H5C 2 0.928533 0.755019 0.337434 11.00000 -1.50000 AFIX 0 HKLF 4 REM EtaKCrF_c3_p04_f4_152_R15_RO_s2 in P2(1)/n REM R1 = 0.0680 for 1002 Fo > 4sig(Fo) and 0.1156 for all 2090 data REM 123 parameters refined using 12 restraints END WGHT 0.1068 0.1977 REM Highest difference peak 0.606, deepest hole -0.649, 1-sigma level 0.078 Q1 1 0.4201 0.4208 0.4745 11.00000 0.05 0.61 Q2 1 0.4167 0.5867 0.4733 11.00000 0.05 0.42 Q3 1 0.5743 0.4219 1.0228 11.00000 0.05 0.41 Q4 1 0.5827 0.5796 1.0211 11.00000 0.05 0.38 Q5 1 0.4997 0.3447 0.5052 11.00000 0.05 0.34 Q6 1 0.6973 0.4938 0.5004 11.00000 0.05 0.31 Q7 1 0.4782 0.3327 0.5377 11.00000 0.05 0.29 Q8 1 0.5755 0.2899 0.4557 11.00000 0.05 0.28 Q9 1 0.6874 0.5744 0.9138 11.00000 0.05 0.26 Q10 1 0.5367 0.4211 0.5840 11.00000 0.05 0.26 Q11 1 0.1870 0.0010 0.4992 11.00000 0.05 0.25 Q12 1 0.6591 0.4922 0.5447 11.00000 0.05 0.25 Q13 1 0.8771 0.7283 0.2609 11.00000 0.05 0.25 Q14 1 0.8743 0.2008 0.4697 11.00000 0.05 0.25 Q15 1 0.7410 0.4912 0.4421 11.00000 0.05 0.25 Q16 1 0.3736 0.4974 0.8654 11.00000 0.05 0.24 Q17 1 0.6331 0.5183 0.4610 11.00000 0.05 0.23 Q18 1 0.2264 0.1835 0.5772 11.00000 0.05 0.23 Q19 1 0.9395 0.7837 0.2649 11.00000 0.05 0.23 Q20 1 0.5793 0.5666 0.6225 11.00000 0.05 0.23 ; _shelx_res_checksum 35989 _shelx_hkl_file ; 0 -1 6 30509.4 927.192 1 0 -1 7 15030.2 671.392 1 0 -1 8 21136.2 819.188 1 0 -1 9 964.284 176.677 1 0 -1 10 3474.36 337.108 1 0 -1 11-23.7343 38.9018 1 0 -1 12 73.3850 74.8066 1 0 -1 13 2141.41 259.702 1 0 -1 14 19.3517 35.1697 1 0 -1 15 282.330 86.8493 1 0 -2 -4 182176. 1970.53 1 0 -2 -5 300.480 128.800 1 0 -2 9 435.949 143.300 1 0 -2 10 41855.8 1480.89 1 0 -2 11-92.0294 107.443 1 0 -2 12 7052.70 614.109 1 0 -2 13 6.81078 27.7682 1 0 -2 14 10605.6 766.079 1 0 -2 15 234.029 124.355 1 0 -2 16 2562.47 354.744 1 0 -2 17 89.1369 56.0043 1 0 -2 18 153.801 96.3699 1 0 -3 -5 3469.97 347.023 1 0 -3 -6 1078.22 170.998 1 0 -3 -7 43136.7 1111.32 1 0 -3 -8 1218.30 175.402 1 0 -3 -9 21749.6 689.504 1 0 -3 12 97.9117 123.345 1 0 -3 13 3867.95 521.770 1 0 -3 14-1.14661 37.3988 1 0 -3 15 95.0671 59.0694 1 0 -3 16 215.467 124.874 1 0 -3 17 178.894 108.357 1 0 -3 18 64.5815 106.839 1 0 -3 19-16.0128 99.1300 1 0 -4 -7 4124.01 420.937 1 0 -4 -8 44884.3 1381.11 1 0 -4 -9 254.937 112.058 1 0 -4 -10 29501.4 1023.78 1 0 -4 -11 28.9308 33.8739 1 0 -4 18 216.034 131.987 1 0 -5 -8 391.317 114.605 1 0 -5 -9 25.5047 63.0647 1 0 -5 -10 1921.14 324.787 1 0 -5 -11 9035.33 665.117 1 0 -5 -12 91.4379 101.145 1 0 -5 -13 3.62230 52.6272 1 0 -6 -10 7570.70 711.582 1 0 -6 -11 86.3418 125.883 1 0 -6 -12 1893.66 369.348 1 0 -6 -13 10.0411 41.1906 1 0 -6 -14 1953.98 331.681 1 0 -7 -11 41.4625 120.645 1 0 -7 -12-19.1090 60.2083 1 0 -7 -13 656.233 245.126 1 0 -7 -14 54.2392 29.9067 1 0 -7 -15-18.3709 54.2217 1 0 -8 -13-50.1142 154.094 1 0 -8 -14 408.571 227.102 1 0 -8 -15 41.3660 99.1585 1 -1 0 9 11469.6 556.966 1 1 0 -8-2.31171 18.6568 1 -1 0 8 2.11768 15.6156 1 -1 0 7 1307.47 200.276 1 1 0 -7 1536.32 172.941 1 -1 0 6 19.7340 27.2639 1 1 0 -6 5.63981 9.19585 1 -1 0 5 57224.3 1155.03 1 1 0 -5 52669.9 1050.04 1 -1 0 4 5.21709 21.8182 1 1 0 -4-1.30058 21.5030 1 -1 0 3 104734. 1541.74 1 1 0 -3 104155. 1465.79 1 -1 0 2 9.35348 20.1346 1 1 0 -2 3.41793 13.6537 1 1 0 11 23122.1 662.763 1 -1 -1 14 6454.63 486.738 1 -1 -1 13 120.374 43.3740 1 -1 -1 12 4257.00 421.176 1 -1 -1 11-37.9751 74.9264 1 -1 -1 10 90739.5 1909.84 1 -1 -1 9 29.6416 39.7205 1 -1 -1 8 107385. 2015.62 1 -1 -1 7 16556.0 777.062 1 1 1 -7 14433.2 706.857 1 1 1 -6 59504.9 1407.86 1 -1 -1 6 62179.0 1460.14 1 1 1 -5 143233. 2136.45 1 -1 -1 5 144465. 2178.60 1 -1 -1 4 77826.3 1547.32 1 1 1 -4 77341.2 1524.90 1 1 1 -3 143107. 1999.30 1 -1 -1 3 142071. 2037.20 1 -1 -1 2 265537. 2701.23 1 1 1 -1 616.453 117.822 1 -1 -1 1 706.738 127.870 1 -1 -1 0 308719. 2781.53 1 -1 -1 -1 886.201 151.736 1 1 1 1 1103.41 151.548 1 -1 -1 -3 8992.69 464.090 1 1 1 3 7721.67 421.406 1 -1 -1 -4 56847.9 1172.90 1 1 1 4 55989.1 1087.68 1 1 -1 13 9.23071 10.8641 1 1 -1 14 6256.79 458.234 1 1 -1 15 74.6441 48.6280 1 1 -1 16 3668.04 311.007 1 -1 -2 17 280.829 121.172 1 -1 -2 16-14.1770 60.9274 1 -1 -2 15 148.582 96.2395 1 -1 -2 14 143.197 89.2856 1 -1 -2 13 957.942 232.037 1 -1 -2 12 137.209 48.6686 1 -1 -2 11 788.359 199.493 1 -1 -2 10 46.0135 60.8646 1 -1 -2 9 23762.4 1119.48 1 -1 -2 8 5984.32 547.574 1 -1 -2 7 543.985 164.124 1 1 2 -6 6382.58 541.105 1 -1 -2 6 6511.60 561.935 1 -1 -2 5 9898.28 693.572 1 1 2 -5 10611.5 704.876 1 -1 -2 4 4668.12 464.556 1 1 2 -4 4306.79 432.613 1 -1 -2 3 31785.4 1170.28 1 1 2 -3 32770.7 1159.44 1 1 2 -2 179602. 2664.54 1 -1 -2 2 188585. 2772.46 1 1 2 -1 247911. 3069.45 1 -1 -2 1 246225. 3078.48 1 1 2 0 94403.8 1836.67 1 -1 -2 0 95863.3 1877.53 1 1 2 1 17819.4 779.015 1 -1 -2 -1 18238.0 796.091 1 1 2 2 40671.7 1143.95 1 -1 -2 -2 44699.3 1211.35 1 -1 -2 -3 66571.4 1471.75 1 1 2 3 69245.2 1443.12 1 -1 -2 -4 11193.1 596.534 1 1 2 4 11074.1 552.127 1 1 2 5 108.938 45.1543 1 -1 -2 -5 38.7371 38.5600 1 -1 -2 -6 804.402 158.360 1 1 2 6 593.812 106.934 1 -1 -2 -7 334.209 99.7498 1 1 2 7 215.887 62.4064 1 1 2 8 1759.18 169.041 1 1 -2 16 217.781 110.344 1 1 -2 17 53.3120 51.3079 1 1 -2 18 118.371 77.9347 1 1 -2 19 35.2347 46.4553 1 -1 -3 19 29.4513 11.4358 1 -1 -3 18 198.276 26.2813 1 -1 -3 17 3.67713 89.8902 1 -1 -3 16 1872.69 374.935 1 -1 -3 15 1.22285 82.4943 1 -1 -3 14 6150.75 695.765 1 -1 -3 13 2451.70 453.475 1 -1 -3 12 4935.91 607.860 1 -1 -3 11 273.267 135.810 1 -1 -3 10 50983.6 1915.59 1 1 -3 -10 50657.6 955.920 1 -1 -3 9 351.322 139.305 1 -1 -3 8 77849.1 2312.17 1 -1 -3 7 3427.94 473.003 1 -1 -3 6 84845.4 2382.53 1 -1 -3 5 2301.10 391.797 1 1 3 -4 161339. 3133.03 1 -1 -3 4 162997. 3163.87 1 1 3 -3 69758.5 2011.95 1 -1 -3 3 70314.6 2018.90 1 1 3 -2 101338. 2357.64 1 -1 -3 2 101731. 2406.56 1 -1 -3 1 543.820 176.639 1 1 3 -1 303.354 118.241 1 -1 -3 0 520409. 5153.50 1 -1 -3 -1 8947.99 669.443 1 1 3 1 9066.06 642.903 1 -1 -3 -2 8900.55 652.748 1 1 3 2 8310.50 619.194 1 -1 -3 -3 90027.3 2026.76 1 1 3 3 88409.5 1963.38 1 1 3 4 16462.5 818.116 1 -1 -3 -4 19019.4 906.458 1 1 3 5 732.706 168.926 1 -1 -3 -5 594.252 170.829 1 1 3 6 133908. 2197.21 1 -1 -3 -6 138485. 2351.94 1 -1 -3 -7 1147.07 209.360 1 -1 -3 -8 55972.4 1458.84 1 -1 -3 -9 150.706 70.3999 1 -1 -4 19-10.4506 85.8900 1 -1 -4 18 214.622 165.735 1 -1 -4 17 398.196 210.484 1 -1 -4 16-66.2439 98.8915 1 -1 -4 15 165.811 53.7806 1 -1 -4 14 38.6428 41.1646 1 -1 -4 13 40.8484 50.6982 1 -1 -4 12-69.3855 218.181 1 1 -4 -12-0.66571 12.2722 1 1 -4 -11 542.997 118.962 1 -1 -4 11 511.653 233.539 1 -1 -4 10 86.7690 149.987 1 -1 -4 9 392.779 172.498 1 -1 -4 8 2112.09 430.414 1 -1 -4 7 9670.21 924.167 1 -1 -4 6 105.898 126.289 1 -1 -4 5 6054.00 723.817 1 -1 -4 4 14668.5 1083.93 1 -1 -4 3 2680.77 467.659 1 1 4 -2 34323.2 1578.37 1 -1 -4 2 35189.8 1603.41 1 -1 -4 1 50363.9 1900.34 1 1 4 -1 52068.5 1913.27 1 -1 -4 0 2971.67 451.481 1 1 4 0 3197.91 464.997 1 -1 -4 -1 6473.92 665.557 1 1 4 1 6496.19 649.765 1 1 4 2 2906.00 430.470 1 -1 -4 -2 2653.76 426.587 1 -1 -4 -3 5098.61 565.042 1 1 4 3 5334.54 560.480 1 1 4 4 22137.2 1122.41 1 -1 -4 -4 23647.1 1196.74 1 -1 -4 -5 10604.0 776.192 1 -1 -4 -6 13749.9 869.436 1 -1 -4 -7 8067.26 652.790 1 -1 -4 -8 3457.05 431.580 1 -1 -4 -9 2348.19 356.036 1 -1 -4 -10 49.7330 39.2038 1 -1 -4 -11 1138.54 227.147 1 -1 -5 18 809.900 296.830 1 -1 -5 17-44.2383 130.647 1 -1 -5 16 1778.69 475.757 1 -1 -5 15-42.3119 64.8109 1 -1 -5 14 5863.47 871.720 1 -1 -5 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568.703 1 3 2 7 628.531 239.113 1 3 2 8 706.118 245.708 1 3 2 9 1811.99 164.383 1 3 2 10 458.663 187.914 1 3 2 11 2432.08 343.666 1 3 2 12 384.875 151.506 1 3 2 13 1465.62 255.011 1 3 2 14-27.4091 43.5576 1 3 2 15 160.667 59.9877 1 -3 -3 18 649.270 266.416 1 -3 -3 17 142.520 132.444 1 -3 -3 16 371.961 206.617 1 -3 -3 15 303.060 184.087 1 3 -3 -14 3851.92 319.623 1 -3 -3 14 3497.40 596.637 1 -3 -3 13 27.4289 101.532 1 3 -3 -13 20.6562 48.3268 1 3 3 -12 14005.6 1067.35 1 -3 -3 12 10331.9 1059.49 1 -3 -3 11 1977.81 452.657 1 3 3 -11 3138.13 500.437 1 3 3 -10 26116.0 1498.68 1 -3 -3 10 23250.3 1571.43 1 3 3 -9 304.804 166.719 1 -3 -3 9 446.715 239.638 1 -3 -3 8 24764.5 1543.58 1 3 3 -8 25946.1 1493.02 1 -3 -3 7 2321.89 478.392 1 3 3 -7 2424.89 459.214 1 -3 -3 6 42811.5 1990.03 1 3 3 -6 44913.5 1932.99 1 3 3 -5 20829.1 1313.89 1 -3 -3 5 19020.2 1314.52 1 3 3 -4 72168.7 2458.17 1 -3 -3 4 75737.5 2576.05 1 3 3 -3 2408.78 424.378 1 -3 -3 3 2771.64 490.677 1 -3 -3 2 194698. 3996.52 1 3 3 -2 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716.985 1 -5 -3 1 4498.26 796.239 1 -5 -3 0 61365.2 2944.52 1 5 3 0 63207.8 2717.20 1 5 3 1 4029.48 695.883 1 -5 -3 -1 3413.45 664.872 1 -5 -3 -2 66197.9 2899.70 1 5 3 2 68025.0 2887.98 1 5 3 3 1935.26 524.229 1 -5 -3 -3 1948.96 526.337 1 5 3 4 54410.3 2590.63 1 -5 -3 -4 50710.4 2661.17 1 5 3 5 1609.64 482.761 1 -5 -3 -5 2003.42 567.331 1 -5 -3 -6 6055.01 942.423 1 5 3 6 5608.50 879.887 1 5 3 7 143.834 175.736 1 5 3 8 5903.03 852.233 1 5 3 9 716.831 288.766 1 5 3 10 9420.53 998.576 1 5 3 11-4.28358 92.4952 1 5 3 12 3512.77 590.673 1 5 3 13 202.038 116.830 1 5 3 14 1328.30 329.500 1 5 3 15 214.749 125.007 1 5 3 16 1507.61 305.515 1 5 3 17 17.8556 15.3473 1 -5 -4 18 4.87160 165.384 1 -5 -4 17 198.564 228.979 1 -5 -4 16-573.333 257.171 1 5 4 -16 65.9523 109.585 1 5 4 -15 188.564 196.892 1 -5 -4 15 2.48898 157.790 1 5 4 -14-94.9446 123.267 1 -5 -4 14 233.617 279.504 1 -5 -4 13 2.49957 47.0701 1 5 4 -13 522.864 253.690 1 5 4 -12 347.966 222.298 1 -5 -4 12-180.895 254.922 1 5 4 -11 670.513 304.892 1 -5 -4 11 245.053 189.260 1 5 4 -10 110.753 129.966 1 -5 -4 10 2.40136 95.9277 1 5 4 -9 732.083 318.978 1 -5 -4 9 592.459 299.694 1 5 4 -8 394.659 191.297 1 -5 -4 8 592.271 305.441 1 5 4 -7 895.430 335.479 1 -5 -4 7 635.556 344.784 1 -5 -4 6 10799.8 1251.70 1 5 4 -6 12282.4 1254.58 1 -5 -4 5 1489.09 470.135 1 5 4 -5 996.333 346.009 1 -5 -4 4 469.171 250.695 1 5 4 -4 552.283 259.843 1 -5 -4 3-4.50495 29.9934 1 5 4 -3 190.691 198.387 1 -5 -4 2 7621.00 1015.90 1 5 4 -2 7106.83 920.328 1 5 4 -1 192.097 70.6824 1 -5 -4 1 329.925 233.730 1 5 4 0 41.2444 56.4956 1 -5 -4 0-302.872 236.218 1 5 4 1 4417.37 736.671 1 -5 -4 -1 4901.17 862.834 1 5 4 2 134.553 116.358 1 -5 -4 -2-114.245 122.898 1 5 4 3 10089.8 1125.06 1 -5 -4 -3 9917.19 1208.56 1 5 4 4 955.860 350.389 1 -5 -4 -4 510.997 309.661 1 5 4 5-38.1734 87.2727 1 -5 -4 -5 44.6976 150.862 1 5 4 6 46.3107 107.822 1 -5 -4 -6 171.885 133.171 1 5 4 7 4633.74 754.437 1 -5 -4 -7 3455.48 729.285 1 -5 -4 -8 1067.59 394.428 1 5 4 8 1227.32 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-9 104.409 75.8461 1 7 8 9 118.768 201.664 1 7 8 10 146.052 149.599 1 -7 -8 -10 241.627 55.4504 1 7 8 11-129.127 218.871 1 -7 -8 -11-207.426 396.634 1 7 8 12 106.647 126.473 1 -7 -8 -12-81.4985 138.903 1 7 8 13 409.845 286.713 1 -7 -8 -13 158.374 234.584 1 7 8 14 170.811 157.949 1 7 8 15 15.7816 133.133 1 7 9 2 2250.37 692.946 1 -7 -9 -3 13.0104 57.7475 1 7 9 3 477.527 282.259 1 -7 -9 -4 1537.96 715.805 1 7 9 4 1298.72 568.716 1 7 9 5 611.430 443.588 1 -7 -9 -5 76.1373 192.382 1 7 9 6 1254.59 520.496 1 -7 -9 -6 990.388 527.890 1 7 9 7 892.137 468.720 1 -7 -9 -7 791.428 488.387 1 7 9 8 2074.21 691.915 1 -7 -9 -8 1250.18 545.000 1 7 9 9-194.086 326.450 1 -7 -9 -9-28.1103 326.724 1 7 9 10 967.409 442.038 1 -7 -9 -10 848.216 557.353 1 7 9 11 5.79030 54.5194 1 -7 -9 -11-15.0729 2016.44 1 -7 -9 -12 328.529 296.057 1 7 9 12 381.432 232.510 1 7 9 13 118.460 266.673 1 -7 -9 -13 73.4315 201.577 1 7 9 14 248.582 219.388 1 -7 -9 -14 322.924 315.848 1 7 9 15-34.4652 111.967 1 -7 -10 -13 78.1127 177.636 1 7 10 13 168.142 219.872 1 -7 -10 -14 239.368 368.323 1 7 10 14 445.275 334.235 1 8 0 -16 422.936 246.317 1 8 1 -16 2.27736 74.2800 1 8 1 -15 128.282 152.311 1 8 1 -14 159.127 266.164 1 8 1 -13-7.80094 215.307 1 8 1 -12-234.240 314.111 1 8 1 -11 183.774 193.168 1 8 2 -17 25.8186 47.7412 1 8 2 -16 276.065 169.610 1 8 2 -15-5.07143 139.216 1 8 2 -14 952.691 420.041 1 8 2 -13-153.858 115.691 1 8 2 -12 426.102 216.458 1 8 2 -11-73.8080 139.742 1 8 2 -10 1500.97 566.493 1 8 2 -9 59.5459 48.7441 1 8 2 -8 9745.65 1374.45 1 8 2 -7-70.7124 113.354 1 8 3 -17 148.274 140.655 1 8 3 -16-279.475 255.587 1 8 3 -15-196.477 190.767 1 8 3 -14 212.061 328.840 1 8 3 -13-177.718 236.574 1 8 3 -12-17.5410 154.083 1 8 3 -11 6.00549 130.586 1 8 3 -10-122.706 172.523 1 -8 -3 9 82.2547 226.721 1 8 3 -9 66.6822 164.769 1 8 3 -8 522.605 354.253 1 -8 -3 8 245.328 168.498 1 8 3 -7 835.772 365.441 1 -8 -3 7 1003.26 523.963 1 8 3 -6-44.9688 112.909 1 -8 -3 6 7.05716 105.063 1 8 3 -5 76.3116 23.4669 1 -8 -3 5-151.559 127.095 1 8 3 -4-132.620 285.171 1 -8 -3 4-137.215 290.061 1 8 3 -3 643.806 315.345 1 -8 -3 3 601.419 363.881 1 8 3 -2 801.192 358.700 1 -8 -3 2 1674.14 636.760 1 8 3 -1 3140.30 846.298 1 -8 -3 1 2068.82 675.385 1 8 4 -17 275.248 202.046 1 8 4 -16 111.386 58.0924 1 8 4 -15-44.0345 133.518 1 -8 -4 14 520.701 380.975 1 8 4 -14 831.116 417.667 1 -8 -4 13-59.9059 299.134 1 8 4 -13 69.4228 61.3942 1 8 4 -12 685.795 354.649 1 -8 -4 12 1075.43 522.605 1 8 4 -11-133.094 243.831 1 -8 -4 11 65.3965 211.200 1 8 4 -10 2067.63 673.283 1 -8 -4 10 1149.02 521.909 1 -8 -4 9 233.206 341.493 1 8 4 -9 3.22097 107.936 1 -8 -4 8 10009.2 1462.84 1 8 4 -8 9916.58 1404.09 1 -8 -4 7-217.700 229.326 1 8 4 -7-176.352 177.907 1 8 4 -6 2107.04 667.269 1 -8 -4 6 1364.46 545.817 1 8 4 -5 277.579 164.596 1 -8 -4 5 1140.16 579.960 1 8 4 -4 4276.14 904.596 1 -8 -4 4 5176.95 1050.14 1 8 4 -3 3987.34 896.188 1 -8 -4 3 3930.06 973.414 1 8 4 -2 6164.64 1109.03 1 -8 -4 2 5492.40 1191.40 1 8 4 -1 474.835 263.959 1 -8 -4 1 243.962 177.871 1 -8 -4 0 13764.0 1816.23 1 8 4 0 11797.2 1557.01 1 8 4 1 4798.13 1009.26 1 -8 -4 -1 3894.30 986.946 1 -8 -4 -2 13487.4 1827.47 1 8 4 2 16173.0 1855.06 1 8 4 3 688.508 412.538 1 -8 -4 -3 1213.50 456.560 1 8 4 4 704.681 421.043 1 -8 -4 -4 1170.93 579.259 1 8 4 5-3.10427 23.8651 1 8 4 6 6003.41 1178.90 1 8 4 7 343.839 313.280 1 8 4 8 2056.58 664.078 1 8 4 9 83.5762 93.3561 1 8 4 10 1016.52 467.067 1 8 5 -15-111.579 224.625 1 -8 -5 15 337.850 479.715 1 8 5 -14 408.091 307.990 1 -8 -5 14-552.387 378.789 1 -8 -5 13-221.624 260.184 1 8 5 -13 442.319 312.865 1 -8 -5 12-127.402 317.527 1 8 5 -12-52.8010 198.149 1 8 5 -11 354.659 227.917 1 -8 -5 11 441.121 395.947 1 8 5 -10-26.9866 172.024 1 -8 -5 10-16.2431 116.809 1 8 5 -9 144.699 270.094 1 -8 -5 9 661.075 314.507 1 8 5 -8 565.520 356.209 1 -8 -5 8 158.470 30.4573 1 8 5 -7 221.837 217.946 1 -8 -5 7 715.144 403.103 1 -8 -5 6 11.6191 201.945 1 8 5 -6 147.476 172.898 1 -8 -5 5 139.998 193.753 1 8 5 -5 102.114 252.354 1 -8 -5 4 299.233 263.794 1 8 5 -4 39.4033 128.719 1 8 5 -3-6.56427 35.6842 1 -8 -5 3 137.308 258.968 1 8 5 -2 218.413 230.381 1 -8 -5 2 7.70681 306.437 1 8 5 -1 948.997 401.936 1 -8 -5 1 264.414 196.026 1 8 5 0 16.4491 56.5539 1 -8 -5 0-349.932 263.994 1 8 5 1 174.163 123.976 1 -8 -5 -1-688.209 475.316 1 8 5 2 34.8909 42.2362 1 -8 -5 -2-46.8321 103.934 1 8 5 3 215.498 197.994 1 -8 -5 -3 65.7733 107.245 1 8 5 4 381.575 302.960 1 -8 -5 -4 323.198 358.635 1 8 5 5-9.08843 154.489 1 -8 -5 -5 202.338 314.743 1 8 5 6-101.312 174.462 1 -8 -5 -6 416.406 362.674 1 8 5 7-70.3736 149.530 1 8 5 8 256.212 323.758 1 8 5 9 679.558 406.661 1 8 5 10-116.749 228.171 1 8 5 11 183.322 210.343 1 8 5 12 41.2970 156.242 1 8 5 13 159.521 173.947 1 8 5 14-24.5156 116.182 1 8 5 15 377.939 221.207 1 8 5 16 29.9588 111.578 1 8 6 -10 762.839 464.255 1 8 6 -9 145.255 169.815 1 -8 -6 9-332.672 435.607 1 8 6 -8 3653.80 893.932 1 -8 -6 8 1217.44 459.454 1 8 6 -7 498.435 352.688 1 -8 -6 7 107.141 73.6724 1 8 6 -6 1153.44 476.074 1 -8 -6 6 67.8132 223.382 1 8 6 -5-269.100 216.060 1 -8 -6 5-139.057 235.843 1 8 6 -4 5150.02 1071.18 1 -8 -6 4 3562.43 960.099 1 8 6 -3 413.313 389.315 1 -8 -6 3 211.938 283.960 1 -8 -6 2 8985.60 1518.18 1 8 6 -2 9745.90 1444.64 1 -8 -6 1 984.729 479.337 1 8 6 -1 1170.23 533.538 1 8 6 0 12283.1 1601.78 1 -8 -6 0 13080.5 1774.48 1 -8 -6 -1-195.249 103.717 1 8 6 1-82.0480 180.181 1 -8 -6 -2 10003.0 1607.15 1 8 6 2 9627.91 1389.08 1 -8 -6 -3-75.4756 257.328 1 8 6 3-199.247 148.559 1 -8 -6 -4 1859.87 717.634 1 8 6 4 1487.32 594.760 1 -8 -6 -5 8.06370 43.8353 1 8 6 5 164.135 215.683 1 -8 -6 -6 5588.41 1323.26 1 8 6 6 6363.37 1153.84 1 -8 -6 -7 27.7325 74.6055 1 8 6 7-224.746 250.388 1 -8 -6 -8 1446.31 658.831 1 8 6 8 1952.52 628.983 1 -8 -6 -9 390.933 281.392 1 8 6 9 620.764 360.316 1 8 6 10 720.102 375.145 1 8 6 11-8.32827 120.729 1 8 6 12-174.931 225.700 1 8 6 13-32.9435 106.707 1 8 6 14 108.095 116.426 1 8 6 15 16.5206 161.267 1 8 6 16-190.687 186.731 1 8 7 -5 345.408 273.617 1 8 7 -4 199.793 83.5461 1 -8 -7 4 304.304 408.519 1 8 7 -3-109.919 156.920 1 -8 -7 3-474.670 394.788 1 8 7 -2-18.7302 40.7279 1 -8 -7 2-370.514 301.400 1 8 7 -1 1535.57 597.199 1 -8 -7 1 886.386 492.210 1 8 7 0 21.7050 157.321 1 -8 -7 0 154.534 182.793 1 8 7 1 458.075 375.303 1 -8 -7 -1 709.352 415.024 1 8 7 2 3.49166 92.9879 1 -8 -7 -2 283.821 280.524 1 8 7 3 99.2644 78.9444 1 -8 -7 -3-21.3936 197.365 1 8 7 4 36.9713 189.877 1 -8 -7 -4 183.207 283.666 1 8 7 5 62.6528 212.100 1 -8 -7 -5-133.239 119.771 1 8 7 6-58.3105 1481.75 1 -8 -7 -6-201.174 374.791 1 8 7 7 240.906 206.778 1 -8 -7 -7 128.839 191.708 1 8 7 8-108.660 41.3397 1 -8 -7 -8 37.1518 126.941 1 8 7 9 328.289 276.504 1 -8 -7 -9-61.2013 54.3293 1 8 7 10 17.8237 55.9407 1 -8 -7 -10-137.401 134.971 1 8 7 11-43.2457 164.375 1 -8 -7 -11 489.288 406.110 1 8 7 12-375.507 247.544 1 8 7 13-292.979 298.137 1 8 7 14-17.8986 83.3991 1 8 7 15 14.8382 19.0122 1 8 8 3-40.7331 227.745 1 -8 -8 -3 242.778 346.836 1 8 8 4 805.971 457.770 1 -8 -8 -4 539.551 418.889 1 8 8 5 206.270 290.637 1 -8 -8 -5 129.617 90.9115 1 8 8 6 1846.38 645.234 1 -8 -8 -6 1037.70 637.773 1 8 8 7 641.325 365.215 1 -8 -8 -7-152.075 211.263 1 8 8 8 529.083 359.058 1 -8 -8 -8 460.304 410.559 1 -8 -8 -9-198.661 328.680 1 8 8 9 112.874 257.657 1 -8 -8 -10 635.617 449.040 1 8 8 10 350.738 281.793 1 -8 -8 -11-91.4369 223.667 1 8 8 11 359.146 191.527 1 -8 -8 -12 244.008 117.182 1 8 8 12 53.3489 120.569 1 8 8 13 287.845 117.989 1 8 8 14 582.691 401.861 1 8 8 15-276.806 230.654 1 8 9 14-45.9480 162.236 1 9 2 -16 301.260 338.109 1 9 2 -15 45.8115 38.1258 1 9 2 -14-39.7628 124.428 1 9 2 -13 172.952 263.912 1 9 2 -12-223.391 297.461 1 9 2 -11 119.277 220.278 1 9 3 -16 676.438 489.189 1 9 3 -15 148.513 187.294 1 9 3 -14 443.470 403.155 1 9 3 -13-45.8655 135.632 1 9 3 -12 780.966 447.168 1 9 3 -11 39.5841 113.412 1 9 3 -10-157.055 239.131 1 9 3 -9-125.497 271.991 1 9 3 -8 4650.62 1063.70 1 9 3 -7 3.43858 199.582 1 9 3 -6 964.106 468.833 1 9 3 -5 232.044 282.562 1 9 4 -12 17.3222 157.570 1 9 4 -11 100.133 162.651 1 -9 -4 11 372.526 299.712 1 -9 -4 10 811.996 475.420 1 9 4 -10 47.2670 160.574 1 -9 -4 9 154.748 253.836 1 9 4 -9-136.458 383.528 1 -9 -4 8-73.5917 305.017 1 9 4 -8-218.416 326.865 1 -9 -4 7 913.921 521.211 1 9 4 -7 62.3785 84.6275 1 9 4 -6-172.368 270.431 1 -9 -4 6 246.900 327.971 1 9 4 -5 14.5231 207.008 1 -9 -4 5 315.787 304.801 1 9 4 -4-168.631 275.831 1 -9 -4 4 284.909 193.511 1 9 4 -3 3.57601 1552.42 1 -9 -4 3-12.9081 144.186 1 9 4 -2 156.711 238.703 1 -9 -4 2 132.930 259.574 1 9 4 -1-122.441 78.3064 1 -9 -4 1 123.200 263.314 1 9 4 0 597.276 351.936 1 -9 -4 0 867.488 571.843 1 9 4 1 95.6729 256.169 1 -9 -5 7 845.274 560.813 1 9 5 -7 885.251 534.463 1 -9 -5 6 2619.59 888.665 1 9 5 -6 1927.15 681.751 1 -9 -5 5 162.681 208.359 1 9 5 -5-198.774 180.061 1 -9 -5 4 3126.03 867.004 1 9 5 -4 3172.52 846.583 1 9 5 -3 418.028 285.856 1 -9 -5 3-101.441 269.966 1 9 5 -2 7736.27 1407.27 1 -9 -5 2 7396.02 1517.54 1 9 5 -1 33.8457 129.295 1 -9 -5 1 68.4357 49.6033 1 9 5 0 3358.34 890.207 1 -9 -5 0 4050.44 1104.33 1 9 5 1 128.271 203.173 1 -9 -5 -1 291.232 494.742 1 9 5 2 4358.01 1012.15 1 -9 -5 -2 4615.43 1165.33 1 9 5 3 67.4547 220.049 1 -9 -5 -3-361.758 287.789 1 9 5 4 1236.37 585.609 1 -9 -5 -4 1247.79 610.518 1 9 5 5 113.934 269.378 1 9 5 6 3135.06 927.169 1 9 5 7-10.0366 92.7347 1 9 5 8 1186.53 521.753 1 9 5 9 90.9830 264.372 1 9 5 10 133.565 255.248 1 9 5 11-131.221 181.341 1 -9 -6 2-186.822 294.618 1 9 6 -2 56.2477 115.570 1 -9 -6 1-694.693 516.966 1 9 6 -1 35.2163 210.574 1 -9 -6 0 402.243 404.954 1 9 6 0 347.448 363.076 1 -9 -6 -1 726.103 390.389 1 9 6 1 479.553 364.281 1 -9 -6 -2 71.4653 103.598 1 9 6 2-123.841 239.650 1 -9 -6 -3-320.933 166.272 1 9 6 3 63.5189 245.426 1 -9 -6 -4-422.062 529.865 1 9 6 4 132.436 229.763 1 -9 -6 -5 456.410 383.957 1 9 6 5 390.831 331.523 1 -9 -6 -6 45.2558 273.952 1 9 6 6 67.5670 1568.79 1 -9 -6 -7 482.073 471.763 1 9 6 7-132.645 175.974 1 9 6 8 88.0639 122.135 1 9 6 9-23.0175 43.7850 1 9 6 10 175.411 61.1706 1 9 6 11 270.125 234.537 1 9 6 12 50.3841 147.258 1 9 6 13-63.0296 180.216 1 9 6 14-20.2719 66.7917 1 9 6 15 38.0525 207.911 1 9 7 7-77.4247 194.318 1 9 7 8-46.8358 221.579 1 -9 -7 -8 295.489 241.886 1 9 7 9-279.604 327.179 1 -9 -7 -9 9.13207 313.970 1 9 7 10 149.918 286.353 1 9 7 11-19.5615 50.1285 1 9 7 12-101.594 327.459 1 9 7 13 384.451 202.021 1 9 7 14 655.026 390.261 1 9 7 15 110.128 65.1265 1 0 0 0 0.00 0.00 0 TITL EtaKCrF_c3_p04_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 8.314179 8.760355 12.310595 90.0000 87.3858 90.0000 ZERR 2.00 0.000997 0.000764 0.000804 0.0000 0.0066 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 85883 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 0.0435(3) Uani 1 2 d S . P . . K1 K 0.500000 0.500000 1.000000 0.0501(4) Uani 1 2 d S . P . . C1 C 0.7749(7) 0.3060(6) 0.4490(4) 0.0637(13) Uani 1 1 d . U . . . H1 H 0.738522 0.254389 0.511453 0.076 Uiso 1 1 calc R U . . . C2 C 0.3271(7) 0.2091(6) 0.5072(4) 0.0654(13) Uani 1 1 d . U . . . H2 H 0.267722 0.247562 0.451144 0.078 Uiso 1 1 calc R U . . . C3 C 0.5812(7) 0.4832(5) 0.7262(4) 0.0561(11) Uani 1 1 d . U . . . H3 H 0.476056 0.448347 0.737151 0.067 Uiso 1 1 calc R U . . . O1 O 0.6904(4) 0.4156(4) 0.4184(2) 0.0579(9) Uani 1 1 d . U . . . O2 O 0.9015(5) 0.2607(4) 0.4040(3) 0.0743(12) Uani 1 1 d . U . . . O3 O 0.4336(4) 0.2930(4) 0.5458(2) 0.0556(8) Uani 1 1 d . U . . . O4 O 0.2978(6) 0.0797(5) 0.5399(4) 0.0885(13) Uani 1 1 d . U . . . O5 O 0.6289(5) 0.5141(3) 0.6301(2) 0.0560(8) Uani 1 1 d . U . . . O6 O 0.6622(5) 0.4954(4) 0.8062(3) 0.0739(12) Uani 1 1 d . U . . . N1 N 1.0134(6) 0.4321(6) 0.2244(4) 0.0689(12) Uani 1 1 d . U . . . H1A H 0.986098 0.374901 0.282067 0.103 Uiso 1 1 calc R U . . . H1B H 1.119754 0.444122 0.219810 0.103 Uiso 1 1 calc R U . . . H1C H 0.981462 0.386491 0.164481 0.103 Uiso 1 1 calc R U . . . C4 C 0.9354(9) 0.5821(8) 0.2357(6) 0.0910(19) Uani 1 1 d . U . . . H4A H 0.962903 0.643374 0.171870 0.109 Uiso 1 1 calc R U . . . H4B H 0.819489 0.568919 0.240218 0.109 Uiso 1 1 calc R U . . . C5 C 0.9848(12) 0.6596(9) 0.3302(8) 0.126(3) Uani 1 1 d . U . . . H5A H 1.098590 0.678276 0.323796 0.189 Uiso 1 1 calc R U . . . H5B H 0.960475 0.597731 0.393230 0.189 Uiso 1 1 calc R U . . . H5C H 0.928533 0.755019 0.337434 0.189 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 0.0407(8) 0.0456(7) 0.0439(5) 0.0043(3) 0.0024(4) 0.0015(3) K1 0.0460(11) 0.0517(10) 0.0521(6) -0.0045(5) 0.0042(6) -0.0016(5) C1 0.059(4) 0.067(4) 0.064(2) 0.014(2) 0.013(2) 0.009(2) C2 0.062(4) 0.057(4) 0.078(3) 0.009(2) -0.008(2) -0.011(2) C3 0.052(4) 0.065(3) 0.051(2) 0.0047(17) 0.0020(19) -0.0008(17) O1 0.058(2) 0.061(2) 0.0538(15) 0.0103(13) 0.0096(14) 0.0119(13) O2 0.067(3) 0.070(3) 0.084(2) 0.0137(18) 0.022(2) 0.0203(16) O3 0.055(3) 0.054(2) 0.0570(15) 0.0063(12) -0.0016(14) -0.0035(12) O4 0.094(4) 0.064(3) 0.109(3) 0.020(2) -0.023(2) -0.0246(19) O5 0.054(2) 0.067(2) 0.0469(14) 0.0063(12) -0.0006(13) -0.0007(12) O6 0.057(3) 0.121(4) 0.0435(15) 0.0058(15) -0.0011(16) -0.0101(17) N1 0.068(4) 0.081(4) 0.0583(19) -0.006(2) -0.0005(19) -0.009(2) C4 0.072(5) 0.098(5) 0.102(4) 0.026(3) 0.013(3) 0.004(3) C5 0.131(8) 0.083(6) 0.160(7) -0.031(5) 0.036(6) -0.021(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 . 3_666 ? O5 Cr1 O3 91.11(13) . 3_666 ? O5 Cr1 O3 88.89(13) 3_666 3_666 ? O5 Cr1 O3 88.89(13) . . ? O5 Cr1 O3 91.11(13) 3_666 . ? O3 Cr1 O3 180.0 3_666 . ? O5 Cr1 O1 89.08(14) . . ? O5 Cr1 O1 90.92(14) 3_666 . ? O3 Cr1 O1 89.51(14) 3_666 . ? O3 Cr1 O1 90.48(14) . . ? O5 Cr1 O1 90.92(14) . 3_666 ? O5 Cr1 O1 89.08(14) 3_666 3_666 ? O3 Cr1 O1 90.48(14) 3_666 3_666 ? O3 Cr1 O1 89.52(14) . 3_666 ? O1 Cr1 O1 180.0 . 3_666 ? O4 K1 O4 180.0 4_666 2_556 ? O4 K1 O6 73.98(14) 4_666 . ? O4 K1 O6 106.02(14) 2_556 . ? O4 K1 O6 106.02(14) 4_666 3_667 ? O4 K1 O6 73.98(14) 2_556 3_667 ? O6 K1 O6 180.0 . 3_667 ? O4 K1 O2 99.36(13) 4_666 4_566 ? O4 K1 O2 80.64(13) 2_556 4_566 ? O6 K1 O2 75.52(10) . 4_566 ? O6 K1 O2 104.48(10) 3_667 4_566 ? O4 K1 O2 80.64(13) 4_666 2_656 ? O4 K1 O2 99.36(13) 2_556 2_656 ? O6 K1 O2 104.48(10) . 2_656 ? O6 K1 O2 75.52(10) 3_667 2_656 ? O2 K1 O2 180.00(9) 4_566 2_656 ? O4 K1 C2 159.63(13) 4_666 2_556 ? O4 K1 C2 20.37(13) 2_556 2_556 ? O6 K1 C2 111.54(13) . 2_556 ? O6 K1 C2 68.46(13) 3_667 2_556 ? O2 K1 C2 101.01(14) 4_566 2_556 ? O2 K1 C2 78.99(14) 2_656 2_556 ? O4 K1 C2 20.37(13) 4_666 4_666 ? O4 K1 C2 159.63(13) 2_556 4_666 ? O6 K1 C2 68.46(13) . 4_666 ? O6 K1 C2 111.54(13) 3_667 4_666 ? O2 K1 C2 78.99(14) 4_566 4_666 ? O2 K1 C2 101.01(14) 2_656 4_666 ? C2 K1 C2 180.0 2_556 4_666 ? O4 K1 C1 111.13(14) 4_666 4_566 ? O4 K1 C1 68.87(14) 2_556 4_566 ? O6 K1 C1 94.82(11) . 4_566 ? O6 K1 C1 85.18(11) 3_667 4_566 ? O2 K1 C1 20.26(10) 4_566 4_566 ? O2 K1 C1 159.74(10) 2_656 4_566 ? C2 K1 C1 88.33(15) 2_556 4_566 ? C2 K1 C1 91.67(15) 4_666 4_566 ? O4 K1 C1 68.87(14) 4_666 2_656 ? O4 K1 C1 111.13(14) 2_556 2_656 ? O6 K1 C1 85.18(11) . 2_656 ? O6 K1 C1 94.82(11) 3_667 2_656 ? O2 K1 C1 159.74(10) 4_566 2_656 ? O2 K1 C1 20.26(10) 2_656 2_656 ? C2 K1 C1 91.67(15) 2_556 2_656 ? C2 K1 C1 88.33(15) 4_666 2_656 ? C1 K1 C1 180.00(16) 4_566 2_656 ? O4 K1 C3 91.56(14) 4_666 . ? O4 K1 C3 88.44(14) 2_556 . ? O6 K1 C3 18.75(13) . . ? O6 K1 C3 161.25(13) 3_667 . ? O2 K1 C3 65.38(11) 4_566 . ? O2 K1 C3 114.62(11) 2_656 . ? C2 K1 C3 97.13(13) 2_556 . ? C2 K1 C3 82.87(13) 4_666 . ? C1 K1 C3 82.38(12) 4_566 . ? C1 K1 C3 97.62(12) 2_656 . ? O4 K1 C3 88.44(14) 4_666 3_667 ? O4 K1 C3 91.56(14) 2_556 3_667 ? O6 K1 C3 161.25(13) . 3_667 ? O6 K1 C3 18.75(13) 3_667 3_667 ? O2 K1 C3 114.62(11) 4_566 3_667 ? O2 K1 C3 65.38(11) 2_656 3_667 ? C2 K1 C3 82.87(13) 2_556 3_667 ? C2 K1 C3 97.13(13) 4_666 3_667 ? C1 K1 C3 97.62(12) 4_566 3_667 ? C1 K1 C3 82.38(12) 2_656 3_667 ? C3 K1 C3 180.00(15) . 3_667 ? O2 C1 O1 126.0(4) . . ? O2 C1 K1 49.7(2) . 2_646 ? O1 C1 K1 173.2(4) . 2_646 ? O2 C1 H1 117.0 . . ? O1 C1 H1 117.0 . . ? K1 C1 H1 67.6 2_646 . ? O4 C2 O3 123.3(5) . . ? O4 C2 K1 48.6(3) . 2_546 ? O3 C2 K1 158.8(4) . 2_546 ? O4 C2 H2 118.4 . . ? O3 C2 H2 118.4 . . ? K1 C2 H2 73.4 2_546 . ? O6 C3 O5 125.2(5) . . ? O6 C3 K1 44.9(2) . . ? O5 C3 K1 163.4(3) . . ? O6 C3 H3 117.4 . . ? O5 C3 H3 117.4 . . ? K1 C3 H3 74.2 . . ? C1 O1 Cr1 125.3(3) . . ? C1 O2 K1 110.1(3) . 2_646 ? C2 O3 Cr1 128.4(4) . . ? C2 O4 K1 111.0(4) . 2_546 ? C3 O5 Cr1 126.2(4) . . ? C3 O6 K1 116.4(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 111.2(7) . . ? C5 C4 H4A 109.4 . . ? N1 C4 H4A 109.4 . . ? C5 C4 H4B 109.4 . . ? N1 C4 H4B 109.4 . . ? 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 O5 1.971(3) . ? Cr1 O5 1.971(3) 3_666 ? Cr1 O3 1.971(3) 3_666 ? Cr1 O3 1.971(3) . ? Cr1 O1 1.979(3) . ? Cr1 O1 1.979(3) 3_666 ? K1 O4 2.640(4) 4_666 ? K1 O4 2.640(4) 2_556 ? K1 O6 2.686(3) . ? K1 O6 2.686(3) 3_667 ? K1 O2 2.715(3) 4_566 ? K1 O2 2.715(3) 2_656 ? K1 C2 3.283(5) 2_556 ? K1 C2 3.283(5) 4_666 ? K1 C1 3.345(5) 4_566 ? K1 C1 3.345(5) 2_656 ? K1 C3 3.411(4) . ? K1 C3 3.411(4) 3_667 ? C1 O2 1.233(6) . ? C1 O1 1.258(6) . ? C1 H1 0.9300 . ? C2 O4 1.224(6) . ? C2 O3 1.260(6) . ? C2 H2 0.9300 . ? C3 O6 1.223(6) . ? C3 O5 1.260(5) . ? C3 H3 0.9300 . ? N1 C4 1.469(9) . ? N1 H1A 0.8900 . ? N1 H1B 0.8900 . ? N1 H1C 0.8900 . ? C4 C5 1.424(11) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C5 H5C 0.9600 . ?