#------------------------------------------------------------------------------ #$Date: 2020-04-05 21:13:22 +0300 (Sun, 05 Apr 2020) $ #$Revision: 250388 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/55/77/1557746.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_1557746 loop_ _publ_author_name 'Bakalorz, Karolina' 'Przypis, \/Lukasz' 'Tomczyk, Mateusz Micha\/l' 'Ksi\;a\.zek, Maria' 'Grzesik, Ryszard' 'Ku\'znik, Nikodem' _publ_section_title ; Unprecedented Water Effect as a Key Element in Salicyl-Glycine Schiff Base Synthesis. ; _journal_issue 5 _journal_name_full 'Molecules (Basel, Switzerland)' _journal_page_first 1257 _journal_paper_doi 10.3390/molecules25051257 _journal_volume 25 _journal_year 2020 _chemical_formula_moiety 'C9 H9 K N O4' _chemical_formula_sum 'C9 H9 K N O4' _chemical_formula_weight 234.27 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2ybc' _space_group_name_H-M_alt 'P 1 21/c 1' _atom_sites_solution_hydrogens mixed _audit_creation_method SHELXL-2018/3 _cell_angle_alpha 90 _cell_angle_beta 99.765(12) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 18.879(3) _cell_length_b 6.2395(6) _cell_length_c 8.7555(9) _cell_measurement_reflns_used 963 _cell_measurement_temperature 120(1) _cell_measurement_theta_max 68.9840 _cell_measurement_theta_min 4.6950 _cell_volume 1016.4(2) _computing_cell_refinement 'CrysAlisPro 1.171.38.41q (Rigaku OD, 2015)' _computing_data_collection 'CrysAlisPro 1.171.38.41q (Rigaku OD, 2015)' _computing_data_reduction 'CrysAlisPro 1.171.38.41q (Rigaku OD, 2015)' _computing_structure_refinement 'SHELXL-2018/3 (Sheldrick, 2015)' _computing_structure_solution 'SHELXS-2013 (Sheldrick, 2015)' _diffrn_ambient_temperature 120(1) _diffrn_detector_area_resol_mean 10.4498 _diffrn_measured_fraction_theta_full 0.961 _diffrn_measured_fraction_theta_max 0.933 _diffrn_measurement_device_type ; SuperNova diffractometer (Agilent Technologies) with Atlas detector ; _diffrn_measurement_method '\w scans' _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0320 _diffrn_reflns_av_unetI/netI 0.0421 _diffrn_reflns_Laue_measured_fraction_full 0.961 _diffrn_reflns_Laue_measured_fraction_max 0.933 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_k_max 4 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_number 3619 _diffrn_reflns_point_group_measured_fraction_full 0.961 _diffrn_reflns_point_group_measured_fraction_max 0.933 _diffrn_reflns_theta_full 25.000 _diffrn_reflns_theta_max 58.816 _diffrn_reflns_theta_min 4.753 _diffrn_source 'micro-focus sealed X-ray tube' _exptl_absorpt_coefficient_mu 4.567 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.38958 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.38.41q (Rigaku Oxford Diffraction, 2015) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 1.531 _exptl_crystal_description polyhedron _exptl_crystal_F_000 484 _exptl_crystal_size_max 0.070 _exptl_crystal_size_mid 0.070 _exptl_crystal_size_min 0.010 _refine_diff_density_max 0.312 _refine_diff_density_min -0.320 _refine_diff_density_rms 0.070 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.077 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 158 _refine_ls_number_reflns 1350 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.077 _refine_ls_R_factor_all 0.0869 _refine_ls_R_factor_gt 0.0615 _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^)+(0.1067P)^2^+0.3216P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1611 _refine_ls_wR_factor_ref 0.1854 _reflns_Friedel_coverage 0.000 _reflns_number_gt 972 _reflns_number_total 1350 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file Kuznik-1a-1b.cif _cod_data_source_block 1b_psl19_nk1_glysal_3a _cod_original_sg_symbol_H-M 'P 21/c' _cod_database_code 1557746 _shelx_shelxl_version_number 2018/3 _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_estimated_absorpt_t_min 0.740 _shelx_estimated_absorpt_t_max 0.956 _shelx_res_file ; TITL PSl19_NK1_GlySal_3a in P2(1)/c shelx.res created by SHELXL-2018/3 at 12:56:26 on 28-Feb-2020 CELL 1.54184 18.8795 6.2395 8.7555 90 99.765 90 ZERR 4 0.0031 0.0006 0.0009 0 0.012 0 LATT 1 SYMM -X,0.5+Y,0.5-Z SFAC C H N O K UNIT 36 36 4 16 4 EADP O3A O3B rem damp 1000 L.S. 10 PLAN 20 TEMP -153 BOND $H CONF htab HTAB N1 O1 HTAB N1 O2W EQIV $5 x, -y+3/2, z-1/2 HTAB C8 O3A_$5 EQIV $6 x, -y+5/2, z-1/2 HTAB O2W O1_$6 HTAB O2W O1 EQIV $9 x, y+1, z HTAB O2W O2_$9 conn 7 K1A conn 7 k1b fmap 2 acta 50 size 0.01 0.07 0.07 MERG 2 SHEL 999 0.9 OMIT -7 0 2 OMIT -8 0 2 OMIT 1 1 1 OMIT 1 0 2 OMIT 5 0 4 OMIT -2 0 6 OMIT 4 0 4 OMIT 0 1 3 WGHT 0.106700 0.321600 FVAR 5.37801 0.73136 0.57193 0.45532 mole 1 PART 1 K1A 5 0.430896 1.160248 0.324177 31.00000 0.10167 0.04016 = 0.04749 0.00561 0.02004 -0.00508 PART 0 PART 2 K1B 5 0.449840 1.130594 0.268273 -31.00000 0.07108 0.02769 = 0.03373 -0.00268 0.00858 0.00079 PART 0 mole 2 O1 4 0.258445 1.181401 0.224727 11.00000 0.07269 0.03613 = 0.03900 -0.00265 0.01453 -0.00857 O2 4 0.422616 0.474197 0.097078 11.00000 0.07362 0.05484 = 0.04266 0.00913 0.01840 0.02863 PART 1 O3A 4 0.399924 0.737675 0.258365 21.00000 0.04955 0.04769 = 0.04707 -0.00397 0.00869 0.00635 PART 0 PART 2 O3B 4 0.415113 0.817669 0.161359 -21.00000 0.04955 0.04769 = 0.04707 -0.00397 0.00869 0.00635 PART 0 N1 3 0.266925 0.802569 0.103782 11.00000 0.05088 0.03472 = 0.02972 -0.00294 0.00662 0.00206 AFIX 43 H1 2 0.283773 0.934123 0.115489 11.00000 -1.20000 AFIX 0 C1 1 0.166762 0.917707 0.218971 11.00000 0.04913 0.03641 = 0.02905 -0.00287 -0.00152 0.00467 C2 1 0.197659 1.122733 0.259330 11.00000 0.05586 0.03403 = 0.02994 0.00061 -0.00038 0.00756 C3 1 0.156950 1.258081 0.347325 11.00000 0.06520 0.03709 = 0.03456 -0.00649 -0.00013 0.00885 AFIX 43 H3 2 0.175184 1.395455 0.380214 11.00000 -1.20000 AFIX 0 C4 1 0.092990 1.192413 0.383946 11.00000 0.06348 0.05321 = 0.03964 -0.00625 0.00171 0.02130 AFIX 43 H4 2 0.067731 1.286125 0.441280 11.00000 -1.20000 AFIX 0 C5 1 0.063485 0.992803 0.340168 11.00000 0.04815 0.06547 = 0.04525 -0.00587 0.00576 0.01186 AFIX 43 H5 2 0.018664 0.951082 0.366398 11.00000 -1.20000 AFIX 0 C6 1 0.100366 0.857672 0.258493 11.00000 0.04472 0.04557 = 0.04133 -0.00708 0.00158 -0.00107 AFIX 43 H6 2 0.080754 0.720961 0.227992 11.00000 -1.20000 AFIX 0 C7 1 0.205026 0.762614 0.142946 11.00000 0.04887 0.03612 = 0.02679 -0.00319 0.00170 0.00196 AFIX 43 H7 2 0.184133 0.625259 0.120468 11.00000 -1.20000 AFIX 0 C8 1 0.310121 0.641474 0.041424 11.00000 0.06089 0.04582 = 0.03070 -0.00102 0.01344 0.01005 AFIX 23 H8A 2 0.313500 0.678805 -0.067004 11.00000 -1.20000 H8B 2 0.285931 0.500607 0.040637 11.00000 -1.20000 AFIX 0 C9 1 0.384681 0.624149 0.134225 11.00000 0.06330 0.04189 = 0.06069 -0.00073 0.00832 0.01170 mole 3 O1W 4 0.500000 0.500000 0.500000 10.50000 0.12923 0.07560 = 0.03779 0.01320 0.00806 -0.02966 mole 4 O2W 4 0.351203 1.108276 -0.063360 10.50000 0.06588 0.04643 = 0.05085 -0.00956 -0.00169 -0.00155 PART 1 AFIX 7 H2WA 2 0.307934 1.118900 -0.116748 10.50000 -1.50000 H2WB 2 0.347057 1.153719 0.028899 10.50000 -1.50000 AFIX 0 HKLF 4 REM PSl19_NK1_GlySal_3a in P2(1)/c REM wR2 = 0.1854, GooF = S = 1.077, Restrained GooF = 1.077 for all data REM R1 = 0.0615 for 972 Fo > 4sig(Fo) and 0.0869 for all 1350 data REM 158 parameters refined using 0 restraints END WGHT 0.1048 0.4373 REM Instructions for potential hydrogen bonds HTAB N1 O1 HTAB N1 O2W HTAB C8 O3A_$5 HTAB O2W O1_$6 HTAB O2W O1 HTAB O2W O2_$9 REM Highest difference peak 0.312, deepest hole -0.320, 1-sigma level 0.070 Q1 1 0.4290 1.3251 0.3056 11.00000 0.05 0.31 Q2 1 0.4184 0.9531 0.3480 11.00000 0.05 0.24 Q3 1 0.4887 0.6226 0.4585 11.00000 0.05 0.24 Q4 1 0.1975 0.9888 0.2680 11.00000 0.05 0.22 Q5 1 0.4480 0.9534 0.2547 11.00000 0.05 0.22 Q6 1 0.4220 0.3042 0.1149 11.00000 0.05 0.22 Q7 1 0.4205 0.5265 0.3694 11.00000 0.05 0.22 Q8 1 0.4084 0.6378 0.0611 11.00000 0.05 0.21 Q9 1 0.1743 1.2359 0.2604 11.00000 0.05 0.21 Q10 1 0.4601 0.4933 0.4979 11.00000 0.05 0.20 Q11 1 0.2106 1.3228 0.3180 11.00000 0.05 0.20 Q12 1 0.4438 0.5783 0.1199 11.00000 0.05 0.19 Q13 1 0.4584 0.5407 0.1363 11.00000 0.05 0.19 Q14 1 0.2628 1.3558 0.2331 11.00000 0.05 0.19 Q15 1 0.4311 0.8257 0.0431 11.00000 0.05 0.19 Q16 1 0.1626 1.0338 0.2129 11.00000 0.05 0.19 Q17 1 0.4517 0.2402 0.0398 11.00000 0.05 0.19 Q18 1 0.0862 0.6482 0.2638 11.00000 0.05 0.19 Q19 1 0.1711 1.1348 0.3746 11.00000 0.05 0.18 Q20 1 0.2430 1.2978 0.1993 11.00000 0.05 0.18 ; _shelx_res_checksum 80753 _shelx_hkl_file ; -2 0 0 3791.77 360.356 1 -2 0 0 3619.35 178.053 3 2 0 0 3833.26 232.407 2 3 0 0 120714. 1510.74 2 -3 0 0 122451. 1135.45 3 -4 0 0 29971.2 649.435 3 5 0 0 38111.1 1066.99 1 -5 0 0 36247.4 815.603 3 6 0 0 275824. 2966.82 1 -6 0 0 278528. 4903.92 2 -6 0 0 268821. 2371.40 3 7 0 0 67355.6 1615.23 1 -7 0 0 66893.9 1319.78 3 -7 0 0 66495.1 2697.69 2 -8 0 0 107387. 3626.44 2 8 0 0 103511. 2111.61 1 -9 0 0 5657.40 1015.09 2 9 0 0 4916.34 527.981 1 -10 0 0 1289.24 592.878 2 10 0 0 1535.88 369.709 1 -11 0 0 19931.9 1952.85 2 11 0 0 20164.1 1133.16 1 -12 0 0 25520.8 2282.69 2 12 0 0 23655.1 1254.55 1 -13 0 0 7980.24 1382.95 2 13 0 0 7118.87 741.436 1 -14 0 0-45.0641 445.655 2 14 0 0 461.170 204.722 9 14 0 0-168.720 196.590 1 15 0 0-315.008 252.495 1 -15 0 0-182.932 490.963 2 15 0 0-370.066 202.713 9 16 0 0-360.058 192.043 9 17 0 0 5050.85 477.371 9 18 0 0 403.990 188.966 9 19 0 0 3606.46 366.687 9 20 0 0 2137.49 249.779 9 0 -1 0 156.623 128.986 3 1 -1 0 1131.98 127.198 3 1 1 0 1503.11 132.728 1 -1 -1 0 887.193 183.035 3 -1 -1 0 1352.51 191.503 2 2 1 0 5880.26 331.423 1 -2 -1 0 6025.03 500.340 2 2 -1 0 6487.84 228.064 1 -2 1 0 6333.28 361.388 2 -2 -1 0 5273.69 364.942 3 3 1 0 20364.8 708.420 1 -3 -1 0 19556.8 1074.25 2 -3 1 0 23051.1 947.456 2 -3 -1 0 20284.1 735.460 3 3 -1 0 23301.1 573.025 1 -4 1 0 52824.6 1787.35 2 -4 -1 0 54441.2 1303.78 3 -4 -1 0 54006.1 1946.53 2 4 -1 0 55807.3 1091.05 1 5 1 0 42510.7 1247.84 1 -5 -1 0 40269.7 1235.01 3 -5 1 0 37855.0 1791.50 2 -5 -1 0 36502.7 1874.66 2 5 -1 0 40114.5 1043.32 1 -6 -1 0 38711.2 1236.30 3 -6 1 0 37611.2 1944.45 2 6 -1 0 37589.1 1109.01 1 -6 -1 0 34604.6 1940.82 2 6 1 0 37616.3 1243.33 1 -7 -1 0 19077.0 898.658 3 7 1 0 17732.4 905.359 1 -7 1 0 20711.1 1555.59 2 7 -1 0 19121.6 845.848 1 8 1 0 9659.59 700.355 1 -8 -1 0 10290.0 709.831 3 -8 1 0 8764.32 1146.40 2 -8 -1 0 8800.28 1168.82 2 8 -1 0 11027.8 684.402 1 -9 -1 0 8655.26 1237.54 2 -9 -1 0 9905.70 722.462 3 9 -1 0 9897.07 695.950 1 9 1 0 9653.25 756.653 1 -9 1 0 9382.77 1200.09 2 -10 1 0 1722.79 610.533 2 10 1 0 2560.25 412.176 1 -10 -1 0 2300.90 448.463 3 -10 -1 0 1530.41 725.675 2 10 -1 0 2232.51 356.775 1 -11 -1 0 48525.9 3052.29 2 11 1 0 51859.6 1839.41 1 -11 1 0 49351.0 2855.61 2 11 -1 0 52165.2 1708.75 1 -12 1 0 15071.1 1699.14 2 12 -1 0 16721.9 1030.38 1 12 1 0 16391.7 1098.22 1 -12 -1 0 16970.4 1998.23 2 -13 -1 0 3464.12 1077.04 2 13 -1 0 4398.38 574.539 1 -13 1 0 3365.44 928.904 2 13 1 0 3807.38 617.484 1 -14 1 0 2236.98 787.398 2 14 1 0 2443.42 507.551 1 14 -1 0 2097.65 343.182 9 -14 -1 0 2975.01 1034.99 2 14 -1 0 2140.63 450.161 1 15 -1 0 63.2897 193.626 1 -15 -1 0 391.693 284.973 7 -15 -1 0-699.976 733.131 2 -15 1 0-537.477 504.371 2 15 -1 0 48.7418 175.442 9 15 1 0-49.4898 216.539 1 16 -1 0 35.7706 204.778 9 -16 -1 0-279.041 243.665 7 -17 -1 0 670.609 281.054 7 17 -1 0 802.649 243.791 9 18 -1 0-94.3459 188.345 9 19 -1 0 92.6462 158.720 9 20 -1 0 356.412 169.630 9 21 -1 0 309.125 147.525 9 22 -1 0 268.250 105.956 9 0 -2 0 82032.9 1390.08 3 1 -2 0 1551.74 232.142 3 -1 -2 0 1251.16 284.728 3 -1 -2 0 1461.47 187.998 2 1 2 0 1273.15 119.203 1 -2 -2 0 68812.6 1522.45 3 -2 -2 0 69244.4 1508.82 2 2 2 0 69235.4 1032.42 1 2 -2 0 67828.7 1028.05 3 -3 -2 0 549.764 286.950 2 3 -2 0 710.098 142.364 3 3 2 0 407.244 132.775 1 -3 -2 0 827.213 323.109 3 4 -2 0 586.976 87.9191 1 4 2 0 834.126 190.669 1 -4 -2 0 1009.69 385.814 2 -4 -2 0 855.863 343.072 3 -4 2 0 632.681 138.638 2 -5 -2 0 2553.10 437.761 3 5 2 0 2454.83 306.096 1 -5 -2 0 2617.37 521.319 2 5 -2 0 2668.91 220.897 1 -5 2 0 2589.75 369.597 2 -6 -2 0 29546.1 1255.59 3 6 -2 0 27288.2 795.127 1 -6 -2 0 29868.7 1778.79 2 6 2 0 26673.8 1004.52 1 -6 2 0 27638.7 1314.20 2 -7 2 0 6436.83 764.656 2 -7 -2 0 7243.24 1046.43 2 -7 -2 0 7755.21 719.363 3 7 2 0 6959.00 579.445 1 7 -2 0 6410.27 438.673 1 8 2 0 5367.12 550.246 1 -8 -2 0 5026.50 921.621 2 -8 -2 0 4814.47 619.149 3 -8 2 0 5405.65 794.946 2 -9 -2 0 1419.82 775.945 2 9 2 0 2183.88 459.729 1 -9 -2 0 2848.35 642.162 3 -10 -2 0 1620.88 483.249 3 10 2 0 1729.18 389.141 1 -10 -2 0 735.855 594.103 2 -11 -2 0 1759.02 514.171 3 -11 -2 0 1728.44 735.608 2 11 2 0 2242.60 422.949 1 12 2 0-229.246 216.281 1 -12 -2 0-108.455 533.996 2 13 -2 0 7.61456 180.252 9 -13 -2 0 25.8702 579.852 2 13 2 0 58.0660 246.299 1 14 2 0 2221.08 476.030 1 14 -2 0 3379.49 429.520 9 -14 -2 0 1881.33 782.615 2 15 -2 0 1727.40 326.947 9 -15 -2 0 2261.72 481.232 7 -16 -2 0 1651.31 388.138 7 16 -2 0 2327.56 360.802 9 17 -2 0 6351.98 551.574 9 -17 -2 0 5784.78 677.014 7 18 -2 0 631.680 255.943 9 -18 -2 0 343.875 231.269 7 -19 -2 0 882.216 270.870 7 19 -2 0 614.232 226.483 9 -20 -2 0 1153.84 243.323 7 20 -2 0 1599.52 267.688 9 21 -2 0-24.5385 129.670 9 22 -2 0 102.014 91.7457 9 0 -3 0 155.048 204.662 3 1 -3 0 1660.38 277.887 3 -1 -3 0 1866.25 377.843 3 2 -3 0 44999.7 1093.65 3 -2 -3 0 45860.6 1512.26 3 -3 -3 0 790.570 354.347 3 -4 -3 0 22540.9 1188.62 3 -5 -3 0 24677.0 1280.14 3 5 3 0 23386.8 1004.73 1 -6 -3 0 2912.36 535.585 2 6 3 0 4056.36 467.726 1 -7 -3 0 102.583 275.734 2 -7 -3 0 164.445 334.107 3 7 3 0 44.4303 229.947 1 -8 -3 0 3299.24 620.008 3 -8 -3 0 3375.25 727.472 2 8 3 0 2605.51 428.399 1 9 3 0 4561.17 602.028 1 -9 -3 0 4108.60 864.476 2 -9 -3 0 4120.59 744.531 3 -10 -3 0 4948.29 778.102 3 10 3 0 4996.19 643.760 1 -10 -3 0 4435.79 997.947 2 -11 -3 0 1484.38 830.727 2 11 -3 0 1154.96 321.449 9 -11 -3 0 2681.75 800.604 3 11 3 0 1232.53 437.240 1 12 -3 0 3945.99 467.305 9 -12 -3 0 5237.46 1197.70 2 12 3 0 3628.38 613.315 1 13 -3 0 3930.09 459.557 9 -14 -3 0 9170.89 903.302 7 14 -3 0 9918.53 695.658 9 -15 -3 0 426.451 289.033 7 15 -3 0 265.466 221.772 9 16 -3 0 5571.94 532.354 9 -16 -3 0 5147.27 650.909 7 17 -3 0 356.497 207.439 9 -17 -3 0-97.0254 209.456 7 18 -3 0 825.786 222.743 9 -18 -3 0 760.972 261.988 7 -19 -3 0 889.973 275.732 7 19 -3 0 1572.71 249.582 9 20 -3 0-6.25161 114.518 9 -20 -3 0 187.210 166.004 7 21 -3 0 3.81845 75.2257 9 21 -3 0-67.3284 69.4677 8 0 -4 0 11224.2 765.085 3 -1 -4 0 10296.5 800.300 3 -2 -4 0 34.4171 249.424 3 -3 -4 0 136.502 310.122 3 -4 -4 0 905.460 420.652 3 -5 -4 0 286.403 352.431 3 -6 -4 0 834.766 490.953 3 7 -4 0 1579.87 329.254 4 7 -4 0 1222.87 268.555 8 -7 -4 0 1350.97 551.257 3 7 -4 0 1772.23 323.239 5 -8 -4 0 4438.64 804.658 3 8 -4 0 4188.09 489.145 5 8 -4 0 5170.81 514.998 4 9 -4 0 13598.9 805.511 4 9 -4 0 13910.1 848.083 5 -9 -4 0 12132.5 1251.53 3 10 -4 0 933.452 265.305 5 -10 -4 0 327.913 225.118 7 10 -4 0 1172.02 284.610 4 11 -4 0 11306.2 755.351 5 -11 -4 0 11345.5 947.175 7 11 -4 0 12169.7 736.672 9 -12 -4 0 2283.30 463.542 7 12 -4 0 2740.86 374.651 5 12 -4 0 2851.07 411.809 9 13 -4 0 191.017 172.606 9 -13 -4 0-34.4973 224.586 7 -14 -4 0 1985.26 463.862 7 14 -4 0 1781.37 337.345 9 -15 -4 0 1780.70 428.857 7 15 -4 0 1724.38 305.027 9 -16 -4 0 325.782 247.037 7 16 -4 0 495.733 198.946 9 -17 -4 0 549.545 242.686 7 17 -4 0 107.094 110.706 8 17 -4 0 664.670 180.509 9 18 -4 0-38.5057 123.459 9 18 -4 0 22.7659 84.5483 8 -18 -4 0 98.4100 154.895 7 -19 -4 0 288.592 169.709 7 19 -4 0 127.555 76.0062 8 19 -4 0 376.228 113.362 9 0 -5 0 101.204 127.533 8 0 -5 0 43.5868 155.869 5 1 -5 0 3296.66 446.258 5 -1 -5 0 2771.05 422.116 5 1 -5 0 3185.23 370.693 8 1 -5 0 3592.67 474.616 4 -1 -5 0 3213.52 395.849 8 2 -5 0 3625.78 497.512 4 -2 -5 0 2459.50 371.348 5 2 -5 0 3031.16 358.637 8 2 -5 0 3119.71 424.200 5 3 -5 0 1261.26 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903.038 214.785 11 12 -2 7 744.796 166.521 6 12 -2 7 578.424 167.524 12 12 2 7 563.204 154.286 11 13 -2 7 514.246 121.722 6 13 -2 7 256.108 108.543 12 13 2 7 515.812 131.142 11 17 -3 -7 68.3135 73.5760 9 17 -3 -7 122.875 84.6619 5 16 -3 -7 166.071 109.157 5 15 -3 -7 196.608 123.934 5 14 -3 -7-25.1730 120.715 5 13 -3 -7-504.308 342.159 10 13 -3 -7 101.257 153.457 5 12 -3 -7 2468.16 480.899 10 -12 -3 7 2854.13 398.438 11 12 -3 -7 2067.27 361.102 5 11 -3 -7 167.911 266.947 10 -11 -3 7 274.039 253.770 11 10 -3 -7 1979.63 473.823 10 -10 -3 7 1785.14 356.301 11 9 -3 -7 1319.94 433.623 10 -9 -3 7 1187.65 313.622 11 8 -3 -7 1909.99 483.352 10 -8 -3 7 1213.41 351.277 11 -7 -3 7 303.965 228.699 11 6 -3 -7 2184.35 399.154 5 -6 -3 7 2974.78 412.941 11 -5 -3 7 755.560 251.229 11 -4 -3 7 5767.42 522.169 11 -3 -3 7 105.868 205.335 11 -2 -3 7 500.875 253.420 6 -2 -3 7 608.934 229.466 11 -1 -3 7 2862.12 407.314 6 -1 3 7 3053.84 377.799 11 0 -3 7 237.253 234.346 6 0 3 7 469.480 251.902 11 1 -3 7 10640.1 706.525 6 1 3 7 11417.6 727.606 11 2 -3 7 4145.86 456.313 6 2 3 7 4089.16 479.073 11 3 -3 7 1124.19 288.498 6 3 3 7 1187.85 330.422 11 4 -3 7 915.927 243.683 6 4 3 7 776.743 290.494 11 5 -3 7 1096.24 250.961 6 5 3 7 1164.17 326.203 11 6 -3 7 286.722 164.812 6 6 3 7 306.643 243.371 11 7 -3 7-86.6418 151.479 6 7 -3 7-54.3734 177.248 12 7 3 7-113.013 211.267 11 8 -3 7 6142.03 489.126 6 8 -3 7 5340.25 536.838 12 8 3 7 6437.46 538.841 11 9 -3 7 283.265 147.548 6 9 -3 7 70.7205 148.972 12 9 3 7 288.686 208.060 11 10 -3 7 936.089 184.771 6 10 3 7 920.741 210.670 11 11 -3 7-32.9759 85.4471 6 11 3 7 345.738 151.200 11 12 -3 7 175.264 81.0846 6 12 3 7-42.7287 91.3178 11 15 -4 -7-19.9972 73.7916 5 14 -4 -7 269.994 121.834 5 14 -4 -7 30.1322 77.1368 4 13 -4 -7 395.162 165.785 5 12 -4 -7-63.1937 158.804 5 11 -4 -7 407.223 214.838 5 10 -4 -7 341.231 197.623 5 9 -4 -7 145.827 178.281 10 9 -4 -7 242.984 244.529 5 -9 -4 7 433.739 185.321 11 8 -4 -7 284.123 207.713 10 8 -4 -7-119.414 201.574 5 -8 -4 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4.74414 85.4953 6 10 0 8 9.71476 98.3692 11 11 0 8 1089.42 137.990 6 -15 -1 8 1134.52 238.386 11 14 -1 -8 685.664 354.198 10 -14 -1 8 1456.65 282.916 11 13 -1 -8-372.501 407.236 10 -13 -1 8-32.4377 182.701 11 12 -1 -8-294.786 389.785 10 -12 -1 8 179.576 192.872 11 11 1 -8 2302.72 463.573 10 11 -1 -8 3205.30 650.436 10 -11 -1 8 3827.39 467.160 11 10 1 -8 128.302 267.333 10 10 -1 -8 555.784 442.372 10 -10 -1 8-136.977 292.264 11 -10 1 8 15.3955 176.993 11 9 1 -8 123.820 283.835 10 9 -1 -8 339.138 437.631 10 -9 -1 8 103.880 232.899 11 -9 1 8 384.331 231.162 11 -8 -1 8 1495.39 324.146 11 -8 1 8 1025.36 246.122 11 -7 -1 8 4599.39 480.433 11 -7 1 8 4705.66 469.277 11 -6 -1 8 1443.20 324.773 11 -6 1 8 2142.95 334.140 11 -5 -1 8 536.227 258.927 11 -5 1 8 1076.75 275.771 11 -4 -1 8-56.1226 216.204 11 -4 1 8-222.197 228.075 11 -3 -1 8 820.477 250.092 6 -3 -1 8 1027.60 287.552 11 -3 1 8 1243.02 285.986 11 -2 -1 8 375.369 209.044 6 -2 -1 8 300.420 205.250 11 -2 1 8 403.009 212.247 11 -1 -1 8 1277.60 295.275 6 -1 -1 8 1386.58 304.014 11 -1 1 8 1310.41 315.182 11 0 -1 8 2833.63 400.588 6 0 -1 8 2455.55 363.739 11 0 1 8 2898.13 386.939 11 1 -1 8 218.193 178.470 6 1 -1 8-382.877 260.796 11 1 1 8 159.487 208.994 11 2 -1 8 3770.05 429.442 6 2 -1 8 3857.51 440.267 11 2 1 8 2942.85 396.491 11 3 -1 8 981.755 259.040 6 3 1 8 643.672 216.704 11 4 -1 8 1386.08 281.224 6 4 -1 8 1555.07 293.062 11 4 1 8 1332.24 301.525 11 5 -1 8 801.657 215.415 6 5 -1 8 1332.64 266.787 11 5 1 8 986.450 285.233 11 6 -1 8 206.914 159.024 6 6 -1 8 199.855 149.441 11 6 1 8 407.127 208.985 11 7 -1 8 712.213 199.028 6 7 -1 8 666.834 174.669 11 7 1 8 980.764 260.805 11 8 -1 8 311.105 141.299 6 8 1 8 305.564 161.698 11 9 -1 8 238.981 118.939 6 9 1 8 144.403 135.285 11 10 -1 8 988.464 168.022 6 10 1 8 1075.40 187.930 11 11 -1 8 1383.08 176.725 6 11 1 8 1565.83 183.661 11 17 -2 -8-112.476 63.5608 5 16 -2 -8 399.216 118.485 5 -14 -2 8 615.150 204.422 11 13 -2 -8 183.854 364.778 10 -13 -2 8 202.162 191.482 11 12 -2 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53.3535 211.933 11 6 -2 8 2967.04 368.136 6 6 2 8 3423.24 401.834 11 7 -2 8 496.088 174.482 6 7 2 8 439.743 180.422 11 8 -2 8 373.131 147.804 6 8 2 8 586.965 190.583 11 9 -2 8 2003.25 247.094 6 9 2 8 2106.13 257.431 11 10 -2 8 163.681 91.7203 6 10 2 8-140.118 111.156 11 11 -2 8 4.50172 70.2181 6 11 2 8-17.9425 80.0537 11 15 -3 -8 38.2935 82.7995 5 14 -3 -8 39.3891 98.9648 5 13 -3 -8 79.9026 125.230 5 12 -3 -8 137.057 247.348 10 -12 -3 8 195.796 181.022 11 12 -3 -8 100.344 135.930 5 11 -3 -8-71.4346 272.281 10 -11 -3 8 31.1895 161.139 11 11 -3 -8-62.2380 159.233 5 10 -3 -8 1510.52 371.667 10 -10 -3 8 956.990 242.422 11 10 -3 -8 975.439 278.195 5 9 -3 -8 875.497 357.981 10 9 -3 -8 13.4523 186.547 5 -9 -3 8 690.201 232.950 11 8 -3 -8 2229.62 480.707 10 8 -3 -8 1431.08 298.126 5 -8 -3 8 1921.31 321.005 11 -7 -3 8 187.586 173.267 11 -6 -3 8 216.591 160.964 11 -5 -3 8 620.107 216.603 11 -4 -3 8 1232.01 257.183 11 -3 -3 8 1638.69 284.405 11 -2 -3 8-81.9551 169.694 11 -1 3 8 14.6782 147.447 11 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319.402 10 -10 0 9-14.7745 175.126 11 9 0 -9-226.249 284.676 10 -9 0 9 183.033 195.622 11 8 0 -9 75.5637 297.176 10 -8 0 9 152.408 204.497 11 7 0 -9-34.7048 282.726 10 -7 0 9 224.284 224.405 11 6 0 -9 603.461 365.954 10 -6 0 9 26.1240 221.369 11 -5 0 9-88.9153 218.554 11 -4 0 9 67.4237 192.555 11 -3 0 9 289.618 215.325 11 -2 0 9 211.212 220.628 11 -1 0 9-182.577 212.817 11 0 0 9 195.341 185.956 11 1 0 9 67.1256 184.121 11 2 0 9 158.863 180.305 11 3 0 9-127.670 172.943 11 4 0 9-117.010 167.571 11 5 0 9 229.028 181.475 11 6 0 9 7.97124 139.203 11 7 0 9 153.189 115.093 11 8 0 9-124.810 89.1071 11 -14 -1 9 207.138 147.362 11 13 -1 -9 1.53685 262.831 10 -13 -1 9-44.2413 154.249 11 12 -1 -9 2118.44 465.642 10 -12 -1 9 2401.49 327.068 11 11 -1 -9 436.509 354.362 10 -11 -1 9 405.891 196.320 11 10 -1 -9 451.249 394.241 10 -10 -1 9 130.793 186.185 11 -10 1 9 390.405 169.047 11 -9 -1 9 4941.67 482.479 11 -9 1 9 4780.27 408.627 11 8 -1 -9 467.145 350.108 10 -8 -1 9 312.675 194.041 11 -8 1 9 252.181 180.124 11 7 -1 -9-56.3478 357.150 10 -7 -1 9 152.360 192.310 11 -7 1 9-223.382 181.291 11 -6 -1 9 178.668 191.553 11 -6 1 9 235.481 169.295 11 -5 -1 9 231.569 209.275 11 -5 1 9-162.098 217.621 11 -4 -1 9 234.962 196.238 11 -4 1 9 325.322 220.451 11 -3 -1 9 771.297 237.592 11 -3 1 9 310.543 201.731 11 -2 -1 9-287.018 228.840 11 -2 1 9 158.237 183.709 11 -1 -1 9 750.779 225.944 11 -1 1 9 1117.08 272.361 11 0 -1 9 343.615 175.838 6 0 -1 9 216.653 180.184 11 0 1 9 642.861 240.727 11 1 -1 9 258.939 167.360 6 1 -1 9 138.013 205.340 11 1 1 9 133.116 183.165 11 2 -1 9 1447.40 257.821 6 2 -1 9 1397.68 257.736 11 2 1 9 1190.95 267.080 11 3 -1 9 555.403 155.697 6 3 -1 9 353.279 161.844 11 4 -1 9 1053.83 203.002 6 4 -1 9 1145.47 206.331 11 4 1 9 1063.78 230.986 11 5 -1 9 1147.49 193.865 6 5 -1 9 1555.31 219.108 11 5 1 9 1170.24 220.963 11 6 -1 9 10.3801 94.4449 6 6 1 9-74.5914 141.919 11 7 -1 9 140.131 88.1342 6 7 1 9 4.31983 116.271 11 8 -1 9 535.121 110.025 6 8 1 9 560.804 132.289 11 14 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170.721 11 4 -2 9 500.659 162.937 6 4 2 9 393.737 163.085 11 5 -2 9 351.055 126.274 6 5 2 9 458.912 159.102 11 6 -2 9 1228.70 189.154 6 6 2 9 718.479 168.037 11 7 -2 9 1786.05 198.264 6 7 2 9 1537.31 204.188 11 8 2 9 208.634 93.3663 11 11 -3 -9-8.45371 190.859 10 10 -3 -9 645.957 245.655 10 -10 -3 9 637.026 161.509 11 9 -3 -9 190.598 252.037 10 -9 -3 9-11.4548 126.527 11 8 -3 -9 1283.14 339.844 10 -8 -3 9 1010.46 208.315 11 7 -3 -9 7500.01 661.687 10 -7 -3 9 5093.44 402.552 11 6 -3 -9 1518.14 408.600 10 -6 -3 9 958.770 193.748 11 -5 -3 9 77.3300 129.443 11 -4 -3 9-126.914 157.678 11 -3 -3 9 689.171 159.526 11 -1 3 9 812.718 155.569 11 0 3 9 146.464 114.328 11 1 3 9 967.619 190.136 11 2 3 9 4896.48 357.057 11 3 3 9 813.281 165.657 11 4 3 9 961.740 189.549 11 5 3 9-8.54704 94.0352 11 -11 0 10 987.639 164.349 11 10 0 -10 242.007 179.639 10 -10 0 10 248.503 144.541 11 9 0 -10-33.6810 222.382 10 -9 0 10 563.561 177.137 11 8 0 -10 9216.12 657.117 10 -8 0 10 8291.21 503.487 11 7 0 -10 642.652 249.316 10 -7 0 10 569.250 175.546 11 6 0 -10 374.445 249.410 10 -6 0 10 4.52605 144.209 11 5 0 -10 1079.86 299.086 10 -5 0 10 753.306 187.910 11 4 0 -10 1686.47 304.547 10 -4 0 10 1486.27 242.164 11 3 0 -10 854.358 294.747 10 -3 0 10 569.803 179.375 11 -2 0 10 23.3416 137.964 11 -1 0 10 332.368 159.179 11 0 0 10 2404.52 281.406 11 1 0 10 1798.23 235.359 11 2 0 10 376.564 137.047 11 3 0 10 1596.67 204.502 11 4 0 10 170.633 95.6905 11 11 -1 -10 3551.15 400.399 10 -11 -1 10 3170.28 276.287 11 10 -1 -10 1713.83 329.730 10 -10 -1 10 1731.49 245.941 11 9 -1 -10 2404.94 396.676 10 -9 -1 10 1158.34 218.189 11 8 -1 -10 2061.88 404.406 10 -8 -1 10 2001.12 266.048 11 -8 1 10 1444.50 212.062 11 7 -1 -10 3056.93 464.151 10 -7 -1 10 2653.68 297.948 11 -7 1 10 1978.34 230.598 11 -6 -1 10 4288.99 375.362 11 -6 1 10 3886.63 326.582 11 5 -1 -10 313.798 334.969 10 -5 -1 10 340.282 183.115 11 -5 1 10 353.755 144.483 11 -4 -1 10 681.595 193.549 11 -4 1 10 702.321 183.443 11 -3 -1 10 139.332 138.072 11 -3 1 10 248.269 129.408 11 -2 -1 10 305.385 150.372 11 -2 1 10 121.517 141.636 11 -1 -1 10 120.121 134.697 11 -1 1 10 289.295 144.217 11 0 -1 10 285.887 126.472 11 0 1 10 49.1555 124.686 11 1 -1 10 117.145 107.582 11 1 1 10 129.883 132.524 11 2 -1 10 286.229 122.413 11 2 1 10 204.993 122.256 11 3 -1 10 1630.81 177.772 11 3 1 10 1459.77 190.217 11 4 1 10-60.4941 90.0269 11 10 -2 -10 60.7305 168.125 10 -10 -2 10-342.497 139.277 11 9 -2 -10 479.069 216.236 10 -9 -2 10-142.996 126.884 11 8 -2 -10 836.076 289.583 10 -8 -2 10 817.510 173.954 11 7 -2 -10 934.664 328.640 10 -7 -2 10 700.151 190.422 11 6 -2 -10 703.860 285.787 10 -6 -2 10 431.669 152.278 11 5 -2 -10 534.779 286.873 10 -5 -2 10 441.372 154.453 11 4 -2 -10-219.325 240.556 10 -4 -2 10-9.95076 118.107 11 -4 2 10 211.381 110.744 11 -3 -2 10 164.593 127.891 11 -3 2 10 303.726 132.501 11 -2 -2 10 809.485 171.654 11 -2 2 10 590.832 137.386 11 -1 -2 10 934.449 153.523 11 -1 2 10 1272.82 181.994 11 0 2 10 1495.38 191.511 11 1 2 10 48.1003 102.808 11 2 2 10 220.625 103.282 11 0 0 0 0.00 0.00 0 TITL PSl19_NK1_GlySal_3a in P2(1)/c REM P2(1)/c (#14 in standard setting) CELL 1.54184 18.879473 6.239468 8.755548 90.0000 99.7652 90.0000 ZERR 4.00 0.003058 0.000604 0.000854 0.0000 0.0122 0.0000 LATT 1 SYMM -x, y+1/2,-z+1/2 SFAC C H N O UNIT 44.00 40.00 4.00 4.00 TREF HKLF 4 END ; _shelx_hkl_checksum 88333 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -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 K1A K 0.4309(5) 1.1602(11) 0.3242(14) 0.0622(17) Uani 0.57(3) 1 d . . P A 1 K1B K 0.4498(5) 1.1306(7) 0.2683(15) 0.044(2) Uani 0.43(3) 1 d . . P A 2 O1 O 0.25844(19) 1.1814(5) 0.2247(3) 0.0487(9) Uani 1 1 d . . . . . O2 O 0.42262(19) 0.4742(6) 0.0971(3) 0.0560(10) Uani 1 1 d . . . . . O3A O 0.3999(2) 0.7377(7) 0.2584(5) 0.0480(12) Uani 0.731(6) 1 d . . P A 1 O3B O 0.4151(6) 0.818(2) 0.1614(14) 0.0480(12) Uani 0.269(6) 1 d . . P A 2 N1 N 0.2669(2) 0.8026(6) 0.1038(3) 0.0385(9) Uani 1 1 d . . . . . H1 H 0.283773 0.934123 0.115489 0.046 Uiso 1 1 calc R U . . . C1 C 0.1668(2) 0.9177(7) 0.2190(4) 0.0391(11) Uani 1 1 d . . . . . C2 C 0.1977(3) 1.1227(7) 0.2593(5) 0.0408(11) Uani 1 1 d . . . . . C3 C 0.1569(3) 1.2581(8) 0.3473(5) 0.0466(12) Uani 1 1 d . . . . . H3 H 0.175184 1.395455 0.380214 0.056 Uiso 1 1 calc R U . . . C4 C 0.0930(3) 1.1924(8) 0.3839(5) 0.0529(14) Uani 1 1 d . . . . . H4 H 0.067731 1.286125 0.441280 0.064 Uiso 1 1 calc R U . . . C5 C 0.0635(3) 0.9928(9) 0.3402(5) 0.0532(13) Uani 1 1 d . . . . . H5 H 0.018664 0.951082 0.366398 0.064 Uiso 1 1 calc R U . . . C6 C 0.1004(2) 0.8577(8) 0.2585(5) 0.0445(11) Uani 1 1 d . . . . . H6 H 0.080754 0.720961 0.227992 0.053 Uiso 1 1 calc R U . . . C7 C 0.2050(3) 0.7626(7) 0.1429(4) 0.0378(11) Uani 1 1 d . . . . . H7 H 0.184133 0.625259 0.120468 0.045 Uiso 1 1 calc R U . . . C8 C 0.3101(3) 0.6415(8) 0.0414(5) 0.0451(12) Uani 1 1 d . . . . . H8A H 0.313500 0.678805 -0.067004 0.054 Uiso 1 1 calc R U . . . H8B H 0.285931 0.500607 0.040637 0.054 Uiso 1 1 calc R U . . . C9 C 0.3847(3) 0.6241(8) 0.1342(6) 0.0555(13) Uani 1 1 d . . . . . O1W O 0.500000 0.500000 0.500000 0.0816(19) Uani 1 2 d S . P . . O2W O 0.3512(4) 1.1083(10) -0.0634(8) 0.0557(17) Uani 0.5 1 d . . P . . H2WA H 0.307934 1.118900 -0.116748 0.084 Uiso 0.5 1 d R U P A 1 H2WB H 0.347057 1.153719 0.028899 0.084 Uiso 0.5 1 d R U P A 1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 K1A 0.102(3) 0.0402(17) 0.047(3) 0.0056(19) 0.020(3) -0.0051(16) K1B 0.071(3) 0.0277(16) 0.034(4) -0.0027(16) 0.009(2) 0.0008(14) O1 0.073(2) 0.0361(18) 0.0390(16) -0.0026(14) 0.0145(15) -0.0086(16) O2 0.074(2) 0.055(2) 0.0427(16) 0.0091(16) 0.0184(16) 0.0286(19) O3A 0.050(3) 0.048(3) 0.047(2) -0.004(2) 0.009(2) 0.006(2) O3B 0.050(3) 0.048(3) 0.047(2) -0.004(2) 0.009(2) 0.006(2) N1 0.051(2) 0.035(2) 0.0297(17) -0.0029(15) 0.0066(16) 0.0021(16) C1 0.049(3) 0.036(2) 0.0290(19) -0.0029(19) -0.0015(18) 0.005(2) C2 0.056(3) 0.034(2) 0.030(2) 0.0006(18) 0.000(2) 0.008(2) C3 0.065(3) 0.037(3) 0.035(2) -0.006(2) 0.000(2) 0.009(2) C4 0.063(4) 0.053(3) 0.040(2) -0.006(2) 0.002(2) 0.021(3) C5 0.048(3) 0.065(3) 0.045(2) -0.006(3) 0.006(2) 0.012(3) C6 0.045(3) 0.046(3) 0.041(2) -0.007(2) 0.002(2) -0.001(2) C7 0.049(3) 0.036(2) 0.0268(19) -0.0032(18) 0.0017(18) 0.002(2) C8 0.061(3) 0.046(3) 0.031(2) -0.001(2) 0.013(2) 0.010(2) C9 0.063(3) 0.042(3) 0.061(3) -0.001(3) 0.008(2) 0.012(3) O1W 0.129(5) 0.076(4) 0.038(2) 0.013(3) 0.008(3) -0.030(4) O2W 0.066(4) 0.046(4) 0.051(3) -0.010(3) -0.002(3) -0.002(3) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' K K 0.3868 1.0657 '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 O2W K1A O2 71.0(5) 4_586 4_576 ? O2W K1A O3A 122.4(4) 4_586 . ? O2 K1A O3A 80.59(16) 4_576 . ? O2W K1A O2 84.6(3) 4_586 1_565 ? O2 K1A O2 153.4(6) 4_576 1_565 ? O3A K1A O2 123.0(4) . 1_565 ? O2W K1A O1W 65.7(3) 4_586 1_565 ? O2 K1A O1W 80.3(3) 4_576 1_565 ? O3A K1A O1W 154.73(16) . 1_565 ? O2 K1A O1W 79.89(12) 1_565 1_565 ? O2W K1A O2 139.4(4) 4_586 2_655 ? O2 K1A O2 81.79(14) 4_576 2_655 ? O3A K1A O2 80.2(3) . 2_655 ? O2 K1A O2 112.3(4) 1_565 2_655 ? O1W K1A O2 80.80(12) 1_565 2_655 ? O2W K1A O1 54.2(3) 4_586 . ? O2 K1A O1 92.7(4) 4_576 . ? O3A K1A O1 79.23(15) . . ? O2 K1A O1 81.16(14) 1_565 . ? O1W K1A O1 118.1(5) 1_565 . ? O2 K1A O1 159.3(2) 2_655 . ? O2W K1A H2WB 95.3 4_586 . ? O2 K1A H2WB 138.1 4_576 . ? O3A K1A H2WB 74.0 . . ? O2 K1A H2WB 52.6 1_565 . ? O1W K1A H2WB 131.0 1_565 . ? O2 K1A H2WB 124.6 2_655 . ? O1 K1A H2WB 50.5 . . ? O2 K1B O2 128.7(4) 1_565 2_655 ? O2 K1B O3B 82.3(3) 1_565 2_655 ? O2 K1B O3B 48.1(3) 2_655 2_655 ? O2 K1B O1W 79.6(4) 1_565 2_655 ? O2 K1B O1W 81.7(4) 2_655 2_655 ? O3B K1B O2W 121.1(6) . 4_586 ? O2 K1B O2W 76.2(3) 1_565 4_586 ? O2 K1B O2W 124.1(5) 2_655 4_586 ? O3B K1B O2W 106.4(4) 2_655 4_586 ? O1W K1B O2W 152.4(2) 2_655 4_586 ? O2 K1B O2 131.4(5) 1_565 4_576 ? O2 K1B O2 78.0(2) 2_655 4_576 ? O1W K1B O2 149.0(2) 2_655 4_576 ? O2W K1B O2 56.4(3) 4_586 4_576 ? C2 O1 K1A 145.4(3) . . ? C9 O2 K1A 127.9(3) . 4_575 ? C9 O2 K1B 121.9(5) . 1_545 ? K1A O2 K1B 103.2(2) 4_575 1_545 ? C9 O2 K1B 97.1(4) . 2_645 ? K1A O2 K1B 109.71(19) 4_575 2_645 ? C9 O2 K1A 107.8(5) . 1_545 ? K1A O2 K1A 115.59(16) 4_575 1_545 ? C9 O2 K1A 101.4(3) . 2_645 ? K1A O2 K1A 98.21(14) 4_575 2_645 ? K1A O2 K1A 99.9(3) 1_545 2_645 ? C9 O2 K1B 126.4(3) . 4_575 ? K1A O2 K1B 121.4(3) 1_545 4_575 ? K1A O2 K1B 90.20(14) 2_645 4_575 ? C9 O3A K1A 135.7(4) . . ? C9 O3A K1A 80.1(3) . 2_645 ? K1A O3A K1A 90.4(2) . 2_645 ? C9 O3B K1B 162.8(10) . . ? C9 O3B K1B 90.6(6) . 2_645 ? C7 N1 C8 123.6(4) . . ? C7 N1 H1 118.2 . . ? C8 N1 H1 118.2 . . ? C6 C1 C2 121.5(4) . . ? C6 C1 C7 118.3(4) . . ? C2 C1 C7 120.2(4) . . ? O1 C2 C1 122.7(4) . . ? O1 C2 C3 122.2(4) . . ? C1 C2 C3 115.0(4) . . ? C4 C3 C2 121.4(4) . . ? C4 C3 H3 119.3 . . ? C2 C3 H3 119.3 . . ? C3 C4 C5 122.2(5) . . ? C3 C4 H4 118.9 . . ? C5 C4 H4 118.9 . . ? C6 C5 C4 118.7(5) . . ? C6 C5 H5 120.7 . . ? C4 C5 H5 120.7 . . ? C5 C6 C1 121.2(5) . . ? C5 C6 H6 119.4 . . ? C1 C6 H6 119.4 . . ? N1 C7 C1 122.7(4) . . ? N1 C7 H7 118.7 . . ? C1 C7 H7 118.7 . . ? N1 C8 C9 112.3(4) . . ? N1 C8 H8A 109.2 . . ? C9 C8 H8A 109.2 . . ? N1 C8 H8B 109.2 . . ? C9 C8 H8B 109.2 . . ? H8A C8 H8B 107.9 . . ? O2 C9 O3A 125.0(5) . . ? O2 C9 O3B 118.1(7) . . ? O2 C9 C8 115.9(4) . . ? O3A C9 C8 118.1(4) . . ? O3B C9 C8 111.4(6) . . ? O2 C9 K1B 59.2(3) . 2_645 ? O3A C9 K1B 71.9(4) . 2_645 ? C8 C9 K1B 162.8(5) . 2_645 ? O2 C9 K1A 51.5(4) . 1_545 ? O3A C9 K1A 93.1(4) . 1_545 ? C8 C9 K1A 117.8(3) . 1_545 ? O2 C9 K1A 57.7(3) . 2_645 ? O3A C9 K1A 78.3(3) . 2_645 ? C8 C9 K1A 152.6(4) . 2_645 ? K1A C9 K1A 80.3(4) 1_545 2_645 ? O3A C9 K1B 100.8(4) . 1_545 ? C8 C9 K1B 119.7(3) . 1_545 ? K1A C9 K1B 74.1(3) 2_645 1_545 ? O3A C9 K1A 152.8(4) . 4_575 ? C8 C9 K1A 87.2(3) . 4_575 ? K1A C9 K1A 82.47(15) 1_545 4_575 ? K1A C9 K1A 74.51(14) 2_645 4_575 ? O2 C9 K1B 125.0(4) . . ? C8 C9 K1B 110.9(3) . . ? K1B C9 K1B 67.5(2) 2_645 . ? K1B C9 K1B 127.2(2) 1_545 . ? K1A O1W K1A 180.0 1_545 3_676 ? K1A O1W K1B 168.19(9) 3_676 1_545 ? K1A O1W K1B 168.19(9) 1_545 3_676 ? K1B O2W K1B 96.2(2) 4_585 . ? K1A O2W H2WA 109.1 4_585 . ? K1A O2W H2WB 110.1 4_585 . ? H2WA O2W H2WB 104.4 . . ? 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 K1A O2W 2.413(17) 4_586 ? K1A O2 2.562(12) 4_576 ? K1A O3A 2.741(9) . ? K1A O2 2.777(6) 1_565 ? K1A O1W 2.808(8) 1_565 ? K1A O2 2.971(10) 2_655 ? K1A O1 3.227(9) . ? K1A H2WB 2.7933 . ? K1B O3B 2.216(14) . ? K1B O2 2.616(6) 1_565 ? K1B O2 2.679(7) 2_655 ? K1B O3B 2.777(13) 2_655 ? K1B O1W 2.799(17) 2_655 ? K1B O2W 3.038(17) 4_586 ? K1B O2 3.079(16) 4_576 ? O1 C2 1.289(6) . ? O2 C9 1.254(6) . ? O3A C9 1.288(7) . ? O3B C9 1.341(13) . ? N1 C7 1.297(6) . ? N1 C8 1.458(5) . ? N1 H1 0.8800 . ? C1 C6 1.407(6) . ? C1 C2 1.425(6) . ? C1 C7 1.437(6) . ? C2 C3 1.449(6) . ? C3 C4 1.364(7) . ? C3 H3 0.9500 . ? C4 C5 1.391(7) . ? C4 H4 0.9500 . ? C5 C6 1.370(7) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 H7 0.9500 . ? C8 C9 1.505(7) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? O2W H2WA 0.8722 . ? O2W H2WB 0.8720 . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A _geom_hbond_publ_flag N1 H1 O1 0.88 1.92 2.606(5) 133.8 . yes N1 H1 O2W 0.88 2.44 3.017(8) 124.0 . yes C8 H8A O3A^a 0.99 2.47 3.318(6) 143.0 4_575 yes O2W H2WA^a O1 0.87 1.98 2.670(7) 135.4 4_585 yes O2W H2WB^a O1 0.87 2.60 3.337(7) 143.4 . yes O2W H2WB^a O2 0.87 2.47 2.892(7) 110.4 1_565 yes loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag K1A O1 C2 C1 -82.5(7) . . . . ? K1A O1 C2 C3 95.2(7) . . . . ? C6 C1 C2 O1 179.9(4) . . . . ? C7 C1 C2 O1 3.0(6) . . . . ? C6 C1 C2 C3 2.0(5) . . . . ? C7 C1 C2 C3 -174.8(3) . . . . ? O1 C2 C3 C4 -179.4(4) . . . . ? C1 C2 C3 C4 -1.6(6) . . . . ? C2 C3 C4 C5 0.4(7) . . . . ? C3 C4 C5 C6 0.5(7) . . . . ? C4 C5 C6 C1 0.0(7) . . . . ? C2 C1 C6 C5 -1.3(6) . . . . ? C7 C1 C6 C5 175.6(4) . . . . ? C8 N1 C7 C1 173.4(3) . . . . ? C6 C1 C7 N1 -179.2(4) . . . . ? C2 C1 C7 N1 -2.2(6) . . . . ? C7 N1 C8 C9 -124.5(4) . . . . ? K1A O2 C9 O3A -152.7(6) 4_575 . . . ? K1A O2 C9 O3A 61.8(6) 1_545 . . . ? K1A O2 C9 O3A -42.7(7) 2_645 . . . ? K1B O2 C9 O3B 117.9(7) 1_545 . . . ? K1B O2 C9 O3B 25.4(8) 2_645 . . . ? K1B O2 C9 O3B -85.3(8) 4_575 . . . ? K1A O2 C9 C8 39.4(7) 4_575 . . . ? K1B O2 C9 C8 -106.1(4) 1_545 . . . ? K1B O2 C9 C8 161.3(5) 2_645 . . . ? K1A O2 C9 C8 -106.1(4) 1_545 . . . ? K1A O2 C9 C8 149.4(5) 2_645 . . . ? K1B O2 C9 C8 50.6(6) 4_575 . . . ? K1B O2 C9 K1B 92.5(4) 1_545 . . 2_645 ? K1B O2 C9 K1B -110.7(4) 4_575 . . 2_645 ? K1A O2 C9 K1A 145.5(6) 4_575 . . 1_545 ? K1A O2 C9 K1A -104.5(3) 2_645 . . 1_545 ? K1A O2 C9 K1A -110.0(4) 4_575 . . 2_645 ? K1A O2 C9 K1A 104.5(3) 1_545 . . 2_645 ? K1B O2 C9 K1B -92.5(4) 2_645 . . 1_545 ? K1B O2 C9 K1B 156.7(6) 4_575 . . 1_545 ? K1A O2 C9 K1A -145.5(6) 1_545 . . 4_575 ? K1A O2 C9 K1A 110.0(4) 2_645 . . 4_575 ? K1B O2 C9 K1B 108.3(4) 1_545 . . . ? K1B O2 C9 K1B 15.7(7) 2_645 . . . ? K1B O2 C9 K1B -95.0(6) 4_575 . . . ? K1A O3A C9 O2 116.0(6) . . . . ? K1A O3A C9 O2 35.8(6) 2_645 . . . ? K1A O3A C9 C8 -76.3(7) . . . . ? K1A O3A C9 C8 -156.6(5) 2_645 . . . ? K1A O3A C9 K1A 159.7(7) . . . 1_545 ? K1A O3A C9 K1A 79.5(4) 2_645 . . 1_545 ? K1A O3A C9 K1A 80.2(4) . . . 2_645 ? K1A O3A C9 K1A 80.2(12) . . . 4_575 ? K1A O3A C9 K1A 0.0(10) 2_645 . . 4_575 ? K1B O3B C9 O2 -132(3) . . . . ? K1B O3B C9 O2 -24.2(8) 2_645 . . . ? K1B O3B C9 C8 90(3) . . . . ? K1B O3B C9 C8 -162.0(5) 2_645 . . . ? K1B O3B C9 K1B -108(3) . . . 2_645 ? K1B O3B C9 K1B -85(3) . . . 1_545 ? K1B O3B C9 K1B 22.7(10) 2_645 . . 1_545 ? K1B O3B C9 K1B 108(3) 2_645 . . . ? N1 C8 C9 O2 173.1(4) . . . . ? N1 C8 C9 O3A 4.3(7) . . . . ? N1 C8 C9 O3B -48.1(8) . . . . ? N1 C8 C9 K1B -118.0(11) . . . 2_645 ? N1 C8 C9 K1A 114.8(5) . . . 1_545 ? N1 C8 C9 K1A -117.8(6) . . . 2_645 ? N1 C8 C9 K1B 127.6(5) . . . 1_545 ? N1 C8 C9 K1A -165.2(4) . . . 4_575 ? N1 C8 C9 K1B -36.7(5) . . . . ?