#------------------------------------------------------------------------------
#$Date: 2025-01-25 05:16:05 +0200 (Sat, 25 Jan 2025) $
#$Revision: 297468 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/31/27/2312743.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2312743
loop_
_publ_author_name
'Movilla, Federico'
'Rey, Juan Manuel'
'López Borda, María Del Rosario'
'Di Salvo, Florencia'
_publ_section_title
;
Conformational versatility among crystalline solids of L-phenylalanine
derivatives.
;
_journal_coeditor_code ZO3057
_journal_issue 2
_journal_name_full
'Acta crystallographica. Section C, Structural chemistry'
_journal_paper_doi 10.1107/S2053229625000269
_journal_volume 81
_journal_year 2025
_chemical_absolute_configuration syn
_chemical_formula_iupac 'C20 H20 N O2 +, Cl -, C2 H4 O2'
_chemical_formula_moiety 'C20 H20 N O2 +, Cl -, C2 H4 O2'
_chemical_formula_sum 'C22 H24 Cl N O4'
_chemical_formula_weight 401.87
_chemical_name_systematic
;
(1-Carboxy-2-phenylethyl)(naphthalen-2-ylmethyl)azanium chloride
acetic acid monosolvate
;
_space_group_crystal_system orthorhombic
_space_group_IT_number 19
_space_group_name_Hall 'P 2ac 2ab'
_space_group_name_H-M_alt 'P 21 21 21'
_atom_sites_solution_hydrogens geom
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_formula_units_Z 4
_cell_length_a 5.058(5)
_cell_length_b 14.786(5)
_cell_length_c 26.482(14)
_cell_measurement_reflns_used 2771
_cell_measurement_temperature 100.0(10)
_cell_measurement_theta_max 31.410
_cell_measurement_theta_min 1.731
_cell_volume 1981(2)
_computing_cell_refinement
;
XDS (Kabsch, 2010)
;
_computing_data_collection
;
MXCuBE (Gabadinho et al., 2010)
;
_computing_data_reduction
;
XDS (Kabsch, 2010)
;
_computing_molecular_graphics
;
OLEX2 (Dolomanov et al., 2009)
;
_computing_publication_material
;
OLEX2 (Dolomanov et al., 2009)
;
_computing_structure_refinement
;
SHELXL2019 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT (Sheldrick, 2015a)
;
_diffrn_ambient_temperature 100.0(10)
_diffrn_detector_area_resol_mean 5.814
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_device_type 'Custom air-bearing with MK3 mini-kappa'
_diffrn_measurement_method 'shuterless \f scans'
_diffrn_radiation_type synchrotron
_diffrn_radiation_wavelength 0.79986
_diffrn_reflns_av_R_equivalents 0.0798
_diffrn_reflns_av_unetI/netI 0.0358
_diffrn_reflns_limit_h_max 6
_diffrn_reflns_limit_h_min -6
_diffrn_reflns_limit_k_max 18
_diffrn_reflns_limit_k_min -18
_diffrn_reflns_limit_l_max 32
_diffrn_reflns_limit_l_min -32
_diffrn_reflns_number 44647
_diffrn_reflns_theta_full 28.680
_diffrn_reflns_theta_max 29.998
_diffrn_reflns_theta_min 1.731
_diffrn_source LNLS-MX2
_exptl_absorpt_coefficient_mu 0.304
_exptl_absorpt_correction_T_max 1.0
_exptl_absorpt_correction_T_min 0.7963
_exptl_absorpt_correction_type empirical
_exptl_absorpt_process_details
;
(XDS; Kabsch, 2010)
;
_exptl_crystal_colour 'clear whiteish white'
_exptl_crystal_density_diffrn 1.348
_exptl_crystal_description prism
_exptl_crystal_F_000 848
_exptl_crystal_size_max 0.1
_exptl_crystal_size_mid 0.1
_exptl_crystal_size_min 0.05
_refine_diff_density_max 0.376
_refine_diff_density_min -0.463
_refine_ls_abs_structure_details
;
Flack x determined using 1159 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons et al., 2013)
;
_refine_ls_abs_structure_Flack 0.02(3)
_refine_ls_extinction_coef 0.026(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method
;
SHELXL2019 (Sheldrick, 2015b)
;
_refine_ls_goodness_of_fit_ref 1.085
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 257
_refine_ls_number_reflns 3952
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.085
_refine_ls_R_factor_all 0.0788
_refine_ls_R_factor_gt 0.0640
_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^)+(0.1152P)^2^+0.6729P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1689
_refine_ls_wR_factor_ref 0.1819
_reflns_number_gt 3267
_reflns_number_total 3952
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file zo3057sup1.cif
_cod_data_source_block pn_hcl
_cod_database_code 2312743
_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 0.970
_shelx_estimated_absorpt_t_max 0.985
_shelx_hkl_file
;
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-5 9 11 5735.90 1422.28 1
-5 -9 -11 3592.39 1206.33 1
-5 -9 -11 5029.80 1204.49 1
5 9 11 5460.79 1336.08 1
5 9 11 4727.18 1094.91 1
5 -9 -11 1370.93 815.680 1
5 -9 -11 2935.35 1272.35 1
-5 9 12 1374.60 1025.68 1
-5 9 12 4635.48 1309.95 1
-5 -9 -12 2705.18 999.08 1
-5 -9 -12 4564.87 1236.13 1
5 9 12 4103.62 1218.71 1
5 9 12 5204.03 1071.98 1
5 -9 -12 89.50 542.870 1
5 -9 -12 2061.44 1231.09 1
-5 9 13 4695.09 1168.27 1
-5 9 13 6254.01 1459.42 1
-5 -9 -13 4240.71 1125.17 1
5 9 13 4837.23 1185.69 1
5 10 0 8839.97 1308.57 1
5 10 0 5373.68 1292.07 1
-5 -10 0 5456.21 1274.64 1
-5 -10 0 3648.78 1246.67 1
5 -10 0 5309.49 1381.02 1
5 -10 0 860.16 1212.29 1
-5 10 0 2052.27 1206.78 1
5 -10 1 1157.72 1342.96 1
5 -10 1 3788.63 1100.87 1
-5 10 1 2874.37 1109.58 1
-5 10 1 7464.46 1479.14 1
5 10 -1 2389.73 1121.96 1
5 10 -1 4924.34 1092.62 1
-5 -10 -1 2725.35 1134.80 1
-5 -10 -1 3399.81 1103.62 1
5 10 1 4055.93 957.358 1
5 10 1 4452.08 1226.04 1
-5 -10 1 2569.46 1171.94 1
-5 -10 1 2071.98 1053.64 1
5 -10 -1 4334.25 1206.78 1
5 -10 -1 3071.07 1277.85 1
-5 10 -1 6254.01 1416.32 1
-5 10 -1 2494.27 1198.07 1
5 -10 2 -550.66 900.962 1
5 -10 2 1406.69 1235.67 1
-5 10 2 965.15 1022.92 1
-5 10 2 912.42 1114.17 1
5 10 -2 -277.99 945.895 1
5 10 -2 95.64 855.570 1
-5 -10 -2 177.21 867.033 1
5 10 2 -417.97 720.770 1
-5 -10 2 108.89 948.647 1
-5 -10 2 973.41 1055.94 1
5 -10 -2 2438.79 1223.75 1
5 -10 -2 1239.34 1048.60 1
-5 10 -2 -405.36 880.788 1
-5 10 -2 -443.37 1046.77 1
5 -10 3 481.89 1364.97 1
5 -10 3 790.92 860.614 1
-5 10 3 543.33 830.352 1
-5 10 3 1535.53 1106.37 1
-5 -10 -3 912.42 977.532 1
-5 -10 -3 328.47 1040.81 1
5 10 3 -36.69 792.755 1
-5 -10 3 280.51 963.319 1
-5 -10 3 -229.44 983.493 1
5 -10 -3 1767.08 939.935 1
5 -10 -3 334.30 845.941 1
-5 10 -3 2102.24 1116.00 1
-5 10 -3 1432.83 1150.39 1
5 -10 4 196.10 1177.44 1
5 -10 4 693.26 985.327 1
-5 10 4 409.54 850.526 1
-5 10 4 555.25 1153.14 1
-5 -10 -4 255.34 904.630 1
5 10 4 2405.32 1059.15 1
-5 -10 4 1172.86 1092.62 1
-5 -10 4 1114.17 968.821 1
5 -10 -4 1122.88 1041.72 1
5 -10 -4 769.37 919.302 1
-5 10 -4 1900.04 1036.68 1
-5 10 -4 543.33 1110.96 1
5 -10 5 1845.02 1137.09 1
-5 10 5 1179.73 1114.17 1
-5 10 5 886.29 890.875 1
-5 -10 -5 -574.05 898.211 1
-5 -10 -5 782.21 935.808 1
5 10 5 53.83 782.668 1
5 10 5 523.15 979.366 1
5 -10 -5 581.38 1032.09 1
5 -10 -5 340.44 790.004 1
-5 10 -5 -71.62 917.468 1
-5 10 6 211.60 890.875 1
-5 10 6 -11.07 1163.23 1
-5 -10 -6 1057.77 885.373 1
-5 -10 -6 -895.00 909.215 1
5 10 6 -519.94 759.742 1
5 10 6 -158.60 937.184 1
5 -10 -6 1814.30 1074.28 1
5 -10 -6 -392.21 742.319 1
-5 10 -6 1563.96 997.248 1
-5 10 7 2049.98 946.812 1
-5 10 7 4125.63 1443.83 1
-5 -10 -7 3790.92 1091.24 1
-5 -10 -7 2340.21 1067.86 1
5 10 7 3987.16 1031.18 1
5 10 7 1441.54 1123.80 1
5 -10 -7 1974.78 1056.40 1
5 -10 -7 3757.45 1114.17 1
-5 10 8 826.23 818.431 1
-5 10 8 501.60 1136.63 1
-5 -10 -8 -351.03 813.388 1
-5 -10 -8 -989.45 922.512 1
5 10 8 1192.57 800.091 1
5 10 8 -835.40 993.580 1
5 -10 -8 600.64 1105.00 1
5 -10 -8 -25.94 793.672 1
-5 10 9 4708.84 1148.10 1
-5 10 9 4928.93 1449.33 1
-5 -10 -9 5758.82 1311.78 1
-5 -10 -9 4029.34 1162.31 1
5 10 9 4434.66 1342.96 1
5 10 9 5369.09 1147.18 1
5 -10 -9 2395.23 1180.65 1
5 -10 -9 145.25 759.284 1
-5 10 10 1036.68 1221.92 1
-5 10 10 3271.43 956.441 1
-5 -10 -10 1513.98 1043.10 1
-5 -10 -10 1022.01 855.570 1
5 10 10 168.18 1046.31 1
5 10 10 1615.77 895.001 1
5 -10 -10 161.62 759.284 1
5 -10 -10 922.97 1046.31 1
-5 10 11 656.58 861.989 1
-5 10 11 1443.37 1003.67 1
-5 -10 -11 1117.83 872.535 1
5 10 11 515.36 788.628 1
5 -10 -11 173.18 720.770 1
5 -10 -11 354.84 1108.21 1
-5 10 12 2705.18 1146.72 1
-5 10 12 976.62 912.883 1
5 -10 -12 828.52 756.991 1
5 11 0 6075.19 1304.90 1
-5 -11 0 3915.63 1315.45 1
-5 11 0 5075.65 1423.20 1
-5 11 1 2342.04 1210.45 1
-5 -11 -1 1683.63 1021.09 1
-5 -11 -1 445.39 891.333 1
5 11 1 1868.41 983.493 1
5 11 1 1659.79 1140.76 1
-5 -11 1 1759.74 1141.68 1
5 -11 -1 35.13 953.690 1
-5 11 2 3273.72 1238.88 1
-5 -11 -2 2413.57 1073.36 1
-5 -11 -2 3207.24 1072.90 1
5 11 2 5653.36 1132.51 1
5 11 2 3215.04 1221.46 1
-5 -11 2 2359.47 1191.20 1
-5 -11 2 2093.99 1162.77 1
5 -11 -2 2864.74 1120.59 1
-5 11 3 4860.15 1450.25 1
-5 -11 -3 5373.68 1221.00 1
-5 -11 -3 4965.61 1200.82 1
5 11 3 3552.95 1013.75 1
5 11 3 4306.28 1313.16 1
5 -11 -3 3426.86 1321.41 1
-5 11 4 3994.95 1303.53 1
-5 -11 -4 1996.79 1127.92 1
-5 -11 -4 2607.98 1066.94 1
5 11 4 3755.61 1231.54 1
5 11 4 3527.28 1044.93 1
5 -11 -4 1183.86 901.420 1
-5 11 5 5804.67 1471.34 1
-5 -11 -5 2609.81 1109.58 1
-5 -11 -5 2138.47 977.532 1
5 11 5 3614.85 1236.59 1
5 11 5 4510.77 1084.82 1
5 -11 -5 1609.35 1028.43 1
-5 11 6 3602.01 1343.42 1
-5 -11 -6 1977.07 1054.10 1
-5 -11 -6 2824.85 954.607 1
5 11 6 3419.07 1031.64 1
5 11 6 3673.08 1321.41 1
-5 11 7 470.88 1128.84 1
-5 -11 -7 1195.32 1004.58 1
-5 -11 -7 473.64 710.682 1
5 11 7 2167.35 1132.51 1
5 11 7 1643.74 921.595 1
-5 11 8 -273.91 1143.51 1
-5 -11 -8 1013.30 818.431 1
5 11 8 1171.94 861.531 1
-5 -12 0 3828.97 1302.61 1
-5 -12 -1 -644.66 1035.76 1
-5 -12 -1 679.50 899.128 1
-5 -12 -2 3309.95 1130.67 1
-5 -12 -2 3023.84 1111.42 1
-5 -12 -3 1568.54 1047.23 1
-5 -12 -3 2907.84 1058.69 1
5 12 3 2309.49 968.362 1
-5 -12 -4 999.08 939.018 1
5 12 4 1958.27 935.808 1
-5 -12 -5 1724.44 1006.88 1
-6 1 -6 -518.11 1320.04 1
-6 1 -7 -564.88 1616.23 1
-6 1 -8 -1328.3 1729.48 1
-6 1 -9 2432.37 2026.13 1
-6 1 -10 -147.32 1518.57 1
-6 1 -11 -330.72 1431.45 1
-6 1 -12 1667.12 1529.57 1
-6 1 -13 -1372.8 1319.12 1
-6 2 -4 2204.03 1465.84 1
-6 2 -5 367.22 1407.15 1
-6 2 -6 610.73 1329.21 1
-6 2 -6 -131.55 1307.66 1
-6 2 -7 1219.62 1760.66 1
-6 2 -7 356.17 1173.31 1
-6 2 -8 1073.82 1617.60 1
-6 2 -8 -1259.1 1207.24 1
-6 2 -9 925.26 1483.26 1
6 -2 10 734.52 1345.71 1
-6 2 -10 661.62 1262.26 1
-6 2 -10 -953.69 1440.62 1
6 -2 11 -246.49 1274.18 1
-6 2 -11 1369.10 1239.80 1
-6 2 -11 -590.10 1340.67 1
-6 2 -12 3468.59 1470.42 1
-6 2 -12 1701.51 1581.84 1
-6 2 -13 2128.84 1309.03 1
-6 3 -3 610.27 1228.79 1
-6 3 -4 -729.48 1228.33 1
-6 3 -4 -284.46 1288.40 1
-6 3 -5 1835.39 1619.44 1
-6 3 -5 2463.09 1350.30 1
-6 3 -6 -289.04 1212.29 1
-6 3 -7 -593.76 1315.45 1
-6 3 -7 1848.23 1320.95 1
-6 3 -8 -102.20 1297.11 1
-6 3 -8 1053.64 1290.69 1
6 -3 9 839.06 1345.71 1
-6 3 -9 1942.68 1435.12 1
-6 3 -9 983.95 1090.32 1
6 -3 10 363.37 1403.48 1
-6 3 -10 696.01 1301.24 1
-6 3 -10 779.46 1156.35 1
6 -3 11 527.74 1454.38 1
-6 3 -11 -0.79 1079.78 1
-6 3 -11 -553.42 1308.57 1
6 -3 12 -561.21 1392.94 1
-6 3 -12 79.92 1191.65 1
-6 3 -13 1174.69 1209.99 1
-6 4 -2 1623.11 1462.63 1
-6 4 -3 4515.81 1642.36 1
-6 4 -3 3020.63 1479.14 1
-6 4 -4 1774.87 1313.16 1
-6 4 -5 1294.82 1264.56 1
-6 4 -5 463.09 1361.30 1
-6 4 -6 -1010.5 1203.12 1
6 -4 7 521.78 1373.22 1
6 -4 7 525.45 1108.66 1
-6 4 -7 -636.40 1199.91 1
-6 4 -7 2762.95 1518.57 1
6 -4 8 -148.14 1023.84 1
6 -4 8 -1033.5 1210.45 1
-6 4 -8 137.60 1135.26 1
-6 4 -8 -2076.6 1048.60 1
6 -4 9 1106.83 1292.53 1
6 -4 9 -1138.5 1266.85 1
-6 4 -9 420.40 1188.44 1
-6 4 -9 4560.29 1367.72 1
6 -4 10 1668.50 1321.41 1
6 -4 10 1052.73 1134.34 1
-6 4 -10 -438.70 1232.00 1
-6 4 -10 241.27 1186.15 1
6 -4 11 3077.94 1473.63 1
6 -4 11 762.95 1258.60 1
-6 4 -11 2911.96 1324.62 1
-6 5 -2 -96.33 1364.05 1
-6 5 -3 1375.97 1219.62 1
-6 5 -3 -1096.7 1071.98 1
-6 5 -4 1396.15 1177.90 1
6 -5 5 -214.21 1140.76 1
-6 5 -5 -300.69 1029.80 1
-6 5 -5 -442.23 1135.72 1
6 -5 6 -1323.7 1085.74 1
6 -5 6 223.02 1026.59 1
-6 5 -6 346.77 1148.10 1
-6 5 -6 275.01 1118.75 1
6 -5 7 1395.69 1347.09 1
6 -5 7 1372.30 1186.61 1
-6 5 -7 109.58 1177.90 1
-6 5 -7 1357.17 1198.53 1
6 -5 8 -292.85 1301.24 1
6 -5 8 312.65 1102.25 1
-6 5 -8 -1759.3 1228.33 1
-6 5 -8 1033.01 1154.52 1
6 -5 9 265.43 1268.68 1
6 -5 9 20.06 1129.76 1
-6 5 -9 445.71 1082.53 1
-6 5 -9 778.54 1102.25 1
-6 5 -10 716.64 1188.44 1
-6 6 -1 964.69 1189.36 1
-6 6 -2 6189.82 1688.21 1
-6 6 -3 2799.17 1246.22 1
-6 6 -3 3045.39 1377.81 1
6 -6 4 2491.52 1451.17 1
-6 6 -4 266.48 1246.67 1
-6 6 -4 3810.18 1346.17 1
6 -6 5 7955.06 1639.15 1
-6 6 -5 9298.48 1748.74 1
-6 6 -5 4901.42 1468.13 1
6 -6 6 822.56 1209.99 1
6 -6 6 1227.42 1119.67 1
-6 6 -6 3116.46 1384.68 1
-6 6 -6 1585.05 1175.61 1
6 -6 7 416.41 1284.73 1
6 -6 7 5185.69 1440.62 1
-6 6 -7 3764.78 1484.64 1
-6 6 -8 -1045.4 1146.26 1
-6 7 -1 502.98 1147.18 1
-6 7 -2 1009.17 1063.73 1
-6 7 -3 1149.01 1085.74 1
-6 7 -3 1791.38 1240.71 1
-6 7 -4 -19.35 1110.96 1
-6 7 -4 997.25 1138.47 1
6 -7 5 -185.14 1154.06 1
-6 7 -5 2.99 1209.99 1
-6 7 -6 300.27 1096.29 1
0 0 0 0. 0.00 0
;
_shelx_hkl_checksum 86111
_shelx_res_file
;
TITL PN_HCl_a.res in P2(1)2(1)2(1)
pn_hcl.res
created by SHELXL-2019/3 at 11:05:05 on 12-Jun-2024
REM Old TITL 19_k90_5_proc2_hkl4_SG19_a.res in P2(1)2(1)2(1)
REM SHELXT solution in P2(1)2(1)2(1): R1 0.124, Rweak 0.039, Alpha 0.001
REM 0.000 for 0 systematic absences, Orientation as input
REM Flack x = -0.087 ( 0.032 ) from 1197 Parsons' quotients
REM Formula found by SHELXT: C20 H24 Cl N O2
CELL 0.79986 5.058 14.786 26.482 90 90 90
ZERR 4 0.0049 0.005 0.014 0 0 0
LATT -1
SYMM 0.5-X,-Y,0.5+Z
SYMM -X,0.5+Y,0.5-Z
SYMM 0.5+X,0.5-Y,-Z
SFAC C H Cl N O
DISP C 0.0048 0.0021 14.959
DISP Cl 0.1771 0.202 958.002
DISP H -0 0 0.6287
DISP N 0.0087 0.0042 26.4688
DISP O 0.0151 0.008 44.7392
UNIT 88 96 4 4 16
L.S. 99
PLAN 50
SIZE 0.05 0.1 0.1
TEMP -173.1(10)
CONF
BOND
list 4
MORE -1
BOND $H
HTAB
fmap 2
acta
OMIT -3 60
OMIT -1 4 8
OMIT 0 0 8
OMIT 0 0 10
OMIT 0 1 11
OMIT 0 8 10
OMIT 1 0 2
OMIT 1 0 3
OMIT 1 4 0
OMIT 1 4 8
REM
REM
REM
WGHT 0.115200 0.672900
EXTI 0.026377
FVAR 7.24046
CL1 3 0.198314 0.146824 0.815218 11.00000 0.03480 0.04607 =
0.05660 0.00482 -0.00033 -0.00191
O1 5 0.013125 0.378286 0.736750 11.00000 0.02990 0.05272 =
0.05710 -0.00314 -0.00351 -0.00161
O2 5 0.388995 0.311252 0.762614 11.00000 0.03293 0.04620 =
0.06342 0.01050 -0.00171 -0.00122
AFIX 147
H2 2 0.286258 0.271472 0.773918 11.00000 -1.50000
AFIX 0
N1 4 0.303371 0.520326 0.694859 11.00000 0.02912 0.04242 =
0.04300 -0.00202 -0.00193 -0.00128
AFIX 23
H1A 2 0.418317 0.566518 0.689061 11.00000 -1.20000
H1B 2 0.160038 0.544217 0.710778 11.00000 -1.20000
AFIX 0
C18 1 0.835064 0.381550 0.548696 11.00000 0.03640 0.05099 =
0.03864 -0.00279 -0.00255 0.00029
C5 1 0.213737 0.632023 0.802419 11.00000 0.04014 0.04429 =
0.04563 -0.00345 -0.00169 -0.00459
AFIX 43
H5 2 0.299035 0.668306 0.777698 11.00000 -1.20000
AFIX 0
C8 1 0.249469 0.377809 0.742728 11.00000 0.03548 0.04279 =
0.04079 -0.00388 0.00301 0.00071
C13 1 0.760327 0.473521 0.546108 11.00000 0.03316 0.04740 =
0.03958 -0.00161 -0.00378 -0.00115
C4 1 0.297812 0.542988 0.809845 11.00000 0.03319 0.04644 =
0.03993 -0.00436 -0.00766 -0.00107
C7 1 0.520106 0.503975 0.779004 11.00000 0.03211 0.04847 =
0.03945 -0.00310 -0.00149 -0.00290
AFIX 23
H7A 2 0.618575 0.460251 0.800166 11.00000 -1.20000
H7B 2 0.643416 0.553390 0.769969 11.00000 -1.20000
AFIX 0
C12 1 0.559162 0.505928 0.578397 11.00000 0.03704 0.04151 =
0.04481 -0.00134 -0.00471 0.00060
AFIX 43
H12 2 0.507838 0.567633 0.576439 11.00000 -1.20000
AFIX 0
C19 1 0.708801 0.325187 0.584169 11.00000 0.04045 0.04098 =
0.04750 -0.00475 -0.00232 0.00069
AFIX 43
H19 2 0.758919 0.263389 0.586342 11.00000 -1.20000
AFIX 0
C3 1 0.169676 0.492181 0.846763 11.00000 0.03599 0.04956 =
0.04557 -0.00093 0.00045 -0.00129
AFIX 43
H3 2 0.222006 0.431310 0.852412 11.00000 -1.20000
AFIX 0
C9 1 0.432151 0.455849 0.730090 11.00000 0.02725 0.04429 =
0.04443 -0.00349 -0.00160 0.00323
AFIX 13
H9 2 0.592953 0.430794 0.713150 11.00000 -1.20000
AFIX 0
C20 1 0.517724 0.357043 0.615231 11.00000 0.03857 0.04518 =
0.04184 -0.00150 -0.00110 -0.00067
AFIX 43
H20 2 0.436773 0.317652 0.638982 11.00000 -1.20000
AFIX 0
C17 1 1.038049 0.350334 0.515761 11.00000 0.03774 0.05136 =
0.04202 -0.00627 -0.00045 0.00029
AFIX 43
H17 2 1.090883 0.288723 0.517071 11.00000 -1.20000
AFIX 0
C16 1 1.157452 0.407116 0.482505 11.00000 0.03413 0.06303 =
0.04710 -0.00949 0.00668 -0.00246
AFIX 43
H16 2 1.291029 0.384730 0.460601 11.00000 -1.20000
AFIX 0
C11 1 0.436416 0.450177 0.612510 11.00000 0.03264 0.04749 =
0.04056 -0.00386 -0.00397 0.00147
C6 1 0.007458 0.668503 0.830554 11.00000 0.04357 0.04509 =
0.05044 -0.00446 -0.00636 0.00399
AFIX 43
H6 2 -0.049425 0.728719 0.824351 11.00000 -1.20000
AFIX 0
C10 1 0.213573 0.484280 0.644362 11.00000 0.03295 0.05388 =
0.04048 -0.00767 -0.00503 -0.00028
AFIX 23
H10A 2 0.086127 0.434476 0.649998 11.00000 -1.20000
H10B 2 0.120350 0.532947 0.625865 11.00000 -1.20000
AFIX 0
C14 1 0.890735 0.531449 0.511159 11.00000 0.04832 0.04641 =
0.04641 0.00419 0.00035 -0.00240
AFIX 43
H14 2 0.842135 0.593425 0.509341 11.00000 -1.20000
AFIX 0
C1 1 -0.114317 0.617816 0.867266 11.00000 0.03598 0.06125 =
0.04696 -0.00862 -0.00366 0.00437
AFIX 43
H1 2 -0.252836 0.643135 0.886941 11.00000 -1.20000
AFIX 0
C15 1 1.084354 0.499170 0.480277 11.00000 0.05097 0.06321 =
0.04522 0.00158 0.00492 -0.01367
AFIX 43
H15 2 1.170277 0.538649 0.457219 11.00000 -1.20000
AFIX 0
C2 1 -0.033154 0.529026 0.875423 11.00000 0.03669 0.06670 =
0.03819 -0.00091 -0.00008 -0.00741
AFIX 43
H2A 2 -0.116926 0.493555 0.900694 11.00000 -1.20000
AFIX 0
O4 5 1.042233 0.305228 0.940647 11.00000 0.09095 0.09611 =
0.15185 0.01635 -0.01203 -0.01421
AFIX 147
H4 2 1.104045 0.283152 0.967383 11.00000 -1.50000
AFIX 0
O3 5 0.687622 0.222659 0.963908 11.00000 0.12697 0.08333 =
0.13621 0.01865 0.02263 -0.02168
C22 1 0.703285 0.287814 0.880353 11.00000 0.08841 0.08343 =
0.10216 -0.00825 -0.02056 0.00807
AFIX 137
H22A 2 0.748851 0.349831 0.870621 11.00000 -1.50000
H22B 2 0.510622 0.280794 0.880406 11.00000 -1.50000
H22C 2 0.781282 0.245325 0.856172 11.00000 -1.50000
AFIX 0
C21 1 0.807291 0.268986 0.931319 11.00000 0.08264 0.06566 =
0.13037 -0.00549 -0.00281 -0.00367
HKLF 4
REM PN_HCl_a.res in P2(1)2(1)2(1)
REM wR2 = 0.1819, GooF = S = 1.085, Restrained GooF = 1.085 for all data
REM R1 = 0.0640 for 3267 Fo > 4sig(Fo) and 0.0788 for all 3952 data
REM 257 parameters refined using 0 restraints
END
WGHT 0.1152 0.6729
REM Instructions for potential hydrogen bonds
HTAB O2 Cl1
EQIV $1 -x+1, y+1/2, -z+3/2
HTAB N1 Cl1_$1
EQIV $2 -x, y+1/2, -z+3/2
HTAB N1 Cl1_$2
HTAB C7 Cl1_$1
EQIV $3 x+1, y, z
HTAB C9 O1_$3
HTAB C10 O1
HTAB C10 Cl1_$2
EQIV $4 x+1/2, -y+1/2, -z+2
HTAB O4 O3_$4
HTAB C22 Cl1_$3
REM Highest difference peak 0.376, deepest hole -0.463, 1-sigma level 0.079
Q1 1 0.9601 0.2820 0.8985 11.00000 0.05 0.38
Q2 1 0.4589 0.2834 0.9045 11.00000 0.05 0.33
Q3 1 0.8056 0.2438 1.0041 11.00000 0.05 0.30
Q4 1 0.0280 0.5209 0.6685 11.00000 0.05 0.29
Q5 1 1.2267 0.2763 0.9904 11.00000 0.05 0.29
Q6 1 1.3724 0.2961 0.9421 11.00000 0.05 0.28
Q7 1 0.1426 0.1945 0.8184 11.00000 0.05 0.27
Q8 1 0.9734 0.2542 1.0026 11.00000 0.05 0.25
Q9 1 0.8148 0.4960 0.5288 11.00000 0.05 0.25
Q10 1 1.3054 0.2422 0.9675 11.00000 0.05 0.25
Q11 1 0.4594 0.1496 0.8187 11.00000 0.05 0.25
Q12 1 0.1225 0.5374 0.6417 11.00000 0.05 0.25
Q13 1 0.6757 0.4713 0.5552 11.00000 0.05 0.24
Q14 1 0.5209 0.6303 0.8054 11.00000 0.05 0.23
Q15 1 0.2018 0.5892 0.8112 11.00000 0.05 0.23
Q16 1 -0.0665 0.1120 0.8359 11.00000 0.05 0.23
Q17 1 0.7064 0.5742 0.8041 11.00000 0.05 0.23
Q18 1 0.2421 0.2588 0.8058 11.00000 0.05 0.22
Q19 1 0.5411 0.3811 0.5547 11.00000 0.05 0.22
Q20 1 0.3147 0.4055 0.7327 11.00000 0.05 0.22
Q21 1 0.0828 0.3109 0.7733 11.00000 0.05 0.22
Q22 1 0.5696 0.2594 0.9247 11.00000 0.05 0.21
Q23 1 -0.2822 0.5582 0.8455 11.00000 0.05 0.21
Q24 1 0.2334 0.2283 0.7772 11.00000 0.05 0.21
Q25 1 0.7225 0.4144 0.7515 11.00000 0.05 0.20
Q26 1 0.5417 0.7028 0.8246 11.00000 0.05 0.20
Q27 1 0.2256 0.5189 0.8318 11.00000 0.05 0.20
Q28 1 0.5353 0.4130 0.6085 11.00000 0.05 0.20
Q29 1 0.1033 0.0613 0.8069 11.00000 0.05 0.20
Q30 1 0.1663 0.6097 0.8685 11.00000 0.05 0.20
Q31 1 -0.3152 0.6409 0.8181 11.00000 0.05 0.20
Q32 1 0.2968 0.0858 0.7892 11.00000 0.05 0.19
Q33 1 1.0549 0.4565 0.4830 11.00000 0.05 0.19
Q34 1 0.3160 0.2452 0.8081 11.00000 0.05 0.19
Q35 1 0.5931 0.4235 0.5392 11.00000 0.05 0.19
Q36 1 0.3811 0.6626 0.8208 11.00000 0.05 0.19
Q37 1 -0.2985 0.6853 0.8348 11.00000 0.05 0.19
Q38 1 0.4459 0.3599 0.6188 11.00000 0.05 0.19
Q39 1 0.7209 0.4515 0.6002 11.00000 0.05 0.19
Q40 1 0.5969 0.4238 0.5661 11.00000 0.05 0.19
Q41 1 0.3594 0.0990 0.8472 11.00000 0.05 0.19
Q42 1 0.3971 0.4541 0.5948 11.00000 0.05 0.19
Q43 1 0.5595 0.4982 0.7564 11.00000 0.05 0.18
Q44 1 0.5100 0.4810 0.5913 11.00000 0.05 0.18
Q45 1 0.0737 0.5186 0.8597 11.00000 0.05 0.18
Q46 1 0.3015 0.3677 0.7492 11.00000 0.05 0.18
Q47 1 0.9303 0.2217 0.9051 11.00000 0.05 0.18
Q48 1 0.0242 0.3616 0.7876 11.00000 0.05 0.18
Q49 1 -0.0483 0.6435 0.8494 11.00000 0.05 0.18
Q50 1 1.0481 0.6619 0.5105 11.00000 0.05 0.18
;
_shelx_res_checksum 33516
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cl Cl1 0.1983(3) 0.14682(8) 0.81522(5) 0.0458(4) Uani d 1 . .
O O1 0.0131(7) 0.3783(3) 0.73675(14) 0.0466(9) Uani d 1 . .
O O2 0.3890(7) 0.3113(2) 0.76261(15) 0.0475(9) Uani d 1 . .
H H2 0.286258 0.271472 0.773918 0.071 Uiso calc 1 . .
N N1 0.3034(8) 0.5203(3) 0.69486(14) 0.0382(9) Uani d 1 . .
H H1A 0.418317 0.566518 0.689061 0.046 Uiso calc 1 . .
H H1B 0.160038 0.544217 0.710778 0.046 Uiso calc 1 . .
C C18 0.8351(11) 0.3816(4) 0.54870(18) 0.0420(11) Uani d 1 . .
C C5 0.2137(11) 0.6320(3) 0.80242(18) 0.0434(11) Uani d 1 . .
H H5 0.299035 0.668306 0.777698 0.052 Uiso calc 1 . .
C C8 0.2495(9) 0.3778(3) 0.74273(18) 0.0397(11) Uani d 1 . .
C C13 0.7603(9) 0.4735(3) 0.54611(18) 0.0400(11) Uani d 1 . .
C C4 0.2978(10) 0.5430(3) 0.80985(17) 0.0399(10) Uani d 1 . .
C C7 0.5201(10) 0.5040(3) 0.77900(18) 0.0400(11) Uani d 1 . .
H H7A 0.618575 0.460251 0.800166 0.048 Uiso calc 1 . .
H H7B 0.643416 0.553390 0.769969 0.048 Uiso calc 1 . .
C C12 0.5592(10) 0.5059(3) 0.57840(19) 0.0411(11) Uani d 1 . .
H H12 0.507838 0.567633 0.576439 0.049 Uiso calc 1 . .
C C19 0.7088(11) 0.3252(3) 0.58417(19) 0.0430(11) Uani d 1 . .
H H19 0.758919 0.263389 0.586342 0.052 Uiso calc 1 . .
C C3 0.1697(11) 0.4922(3) 0.84676(19) 0.0437(11) Uani d 1 . .
H H3 0.222006 0.431310 0.852412 0.052 Uiso calc 1 . .
C C9 0.4322(10) 0.4558(3) 0.73009(18) 0.0387(10) Uani d 1 . .
H H9 0.592953 0.430794 0.713150 0.046 Uiso calc 1 . .
C C20 0.5177(10) 0.3570(3) 0.61523(18) 0.0419(11) Uani d 1 . .
H H20 0.436773 0.317652 0.638982 0.050 Uiso calc 1 . .
C C17 1.0380(10) 0.3503(4) 0.51576(18) 0.0437(11) Uani d 1 . .
H H17 1.090883 0.288723 0.517071 0.052 Uiso calc 1 . .
C C16 1.1575(11) 0.4071(4) 0.4825(2) 0.0481(13) Uani d 1 . .
H H16 1.291029 0.384730 0.460601 0.058 Uiso calc 1 . .
C C11 0.4364(10) 0.4502(3) 0.61251(18) 0.0402(11) Uani d 1 . .
C C6 0.0075(11) 0.6685(3) 0.8306(2) 0.0464(12) Uani d 1 . .
H H6 -0.049425 0.728719 0.824351 0.056 Uiso calc 1 . .
C C10 0.2136(11) 0.4843(3) 0.64436(18) 0.0424(11) Uani d 1 . .
H H10A 0.086127 0.434476 0.649998 0.051 Uiso calc 1 . .
H H10B 0.120350 0.532947 0.625865 0.051 Uiso calc 1 . .
C C14 0.8907(11) 0.5314(4) 0.51116(19) 0.0470(12) Uani d 1 . .
H H14 0.842135 0.593425 0.509341 0.056 Uiso calc 1 . .
C C1 -0.1143(11) 0.6178(4) 0.8673(2) 0.0481(13) Uani d 1 . .
H H1 -0.252836 0.643135 0.886941 0.058 Uiso calc 1 . .
C C15 1.0844(12) 0.4992(4) 0.4803(2) 0.0531(14) Uani d 1 . .
H H15 1.170277 0.538649 0.457219 0.064 Uiso calc 1 . .
C C2 -0.0332(11) 0.5290(4) 0.87542(19) 0.0472(12) Uani d 1 . .
H H2A -0.116926 0.493555 0.900694 0.057 Uiso calc 1 . .
O O4 1.0422(15) 0.3052(5) 0.9406(3) 0.113(2) Uani d 1 . .
H H4 1.104045 0.283152 0.967383 0.169 Uiso calc 1 . .
O O3 0.6876(17) 0.2227(4) 0.9639(3) 0.116(2) Uani d 1 . .
C C22 0.703(2) 0.2878(6) 0.8804(3) 0.091(2) Uani d 1 . .
H H22A 0.748851 0.349831 0.870621 0.137 Uiso calc 1 . .
H H22B 0.510622 0.280794 0.880406 0.137 Uiso calc 1 . .
H H22C 0.781282 0.245325 0.856172 0.137 Uiso calc 1 . .
C C21 0.807(2) 0.2690(5) 0.9313(4) 0.093(3) Uani d 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_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
Cl1 0.0348(6) 0.0461(6) 0.0566(7) -0.0019(5) -0.0003(5) 0.0048(5)
O1 0.0299(19) 0.053(2) 0.057(2) -0.0016(15) -0.0035(16) -0.0031(16)
O2 0.0329(18) 0.0462(19) 0.063(2) -0.0012(15) -0.0017(17) 0.0105(17)
N1 0.0291(18) 0.0424(19) 0.043(2) -0.0013(18) -0.0019(18) -0.0020(16)
C18 0.036(3) 0.051(3) 0.039(2) 0.000(2) -0.003(2) -0.0028(19)
C5 0.040(3) 0.044(2) 0.046(2) -0.005(2) -0.002(2) -0.0035(19)
C8 0.035(3) 0.043(2) 0.041(2) 0.0007(19) 0.0030(19) -0.0039(19)
C13 0.033(3) 0.047(3) 0.040(2) -0.001(2) -0.0038(19) -0.002(2)
C4 0.033(2) 0.046(2) 0.040(2) -0.001(2) -0.008(2) -0.0044(19)
C7 0.032(2) 0.048(3) 0.039(2) -0.003(2) -0.001(2) -0.003(2)
C12 0.037(3) 0.042(2) 0.045(3) 0.001(2) -0.005(2) -0.001(2)
C19 0.040(3) 0.041(2) 0.047(3) 0.001(2) -0.002(2) -0.0048(19)
C3 0.036(3) 0.050(3) 0.046(3) -0.001(2) 0.000(2) -0.001(2)
C9 0.027(2) 0.044(3) 0.044(2) 0.003(2) -0.002(2) -0.003(2)
C20 0.039(3) 0.045(3) 0.042(2) -0.001(2) -0.001(2) -0.001(2)
C17 0.038(3) 0.051(3) 0.042(2) 0.000(2) 0.000(2) -0.006(2)
C16 0.034(3) 0.063(3) 0.047(3) -0.002(2) 0.007(2) -0.009(2)
C11 0.033(2) 0.047(3) 0.041(2) 0.001(2) -0.004(2) -0.004(2)
C6 0.044(3) 0.045(3) 0.050(3) 0.004(2) -0.006(2) -0.004(2)
C10 0.033(2) 0.054(3) 0.040(2) 0.000(2) -0.005(2) -0.008(2)
C14 0.048(3) 0.046(3) 0.046(3) -0.002(2) 0.000(2) 0.004(2)
C1 0.036(3) 0.061(3) 0.047(3) 0.004(2) -0.004(2) -0.009(2)
C15 0.051(3) 0.063(3) 0.045(3) -0.014(3) 0.005(3) 0.002(2)
C2 0.037(3) 0.067(3) 0.038(2) -0.007(3) 0.000(2) -0.001(2)
O4 0.091(5) 0.096(4) 0.152(7) -0.014(4) -0.012(5) 0.016(4)
O3 0.127(5) 0.083(4) 0.136(5) -0.022(4) 0.023(5) 0.019(4)
C22 0.088(6) 0.083(5) 0.102(6) 0.008(5) -0.021(5) -0.008(4)
C21 0.083(5) 0.066(4) 0.130(8) -0.004(5) -0.003(6) -0.005(5)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0048 0.0021 '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'
Cl Cl 0.1771 0.2020 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0087 0.0042 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0151 0.0080 '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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
C8 O2 H2 . . 109.5 ?
H1A N1 H1B . . 107.2 ?
C9 N1 H1A . . 107.9 ?
C9 N1 H1B . . 107.9 ?
C9 N1 C10 . . 117.5(4) ?
C10 N1 H1A . . 107.9 ?
C10 N1 H1B . . 107.9 ?
C13 C18 C17 . . 118.4(5) ?
C19 C18 C13 . . 118.7(5) ?
C19 C18 C17 . . 122.9(5) ?
C4 C5 H5 . . 119.4 ?
C6 C5 H5 . . 119.4 ?
C6 C5 C4 . . 121.2(5) ?
O1 C8 O2 . . 125.9(5) ?
O1 C8 C9 . . 124.8(5) ?
O2 C8 C9 . . 109.2(4) ?
C18 C13 C14 . . 119.1(4) ?
C12 C13 C18 . . 119.3(4) ?
C12 C13 C14 . . 121.6(5) ?
C5 C4 C7 . . 120.8(5) ?
C3 C4 C5 . . 117.7(5) ?
C3 C4 C7 . . 121.5(4) ?
C4 C7 H7A . . 108.6 ?
C4 C7 H7B . . 108.6 ?
C4 C7 C9 . . 114.6(4) ?
H7A C7 H7B . . 107.6 ?
C9 C7 H7A . . 108.6 ?
C9 C7 H7B . . 108.6 ?
C13 C12 H12 . . 119.3 ?
C11 C12 C13 . . 121.4(5) ?
C11 C12 H12 . . 119.3 ?
C18 C19 H19 . . 119.2 ?
C20 C19 C18 . . 121.5(5) ?
C20 C19 H19 . . 119.2 ?
C4 C3 H3 . . 119.5 ?
C2 C3 C4 . . 121.1(5) ?
C2 C3 H3 . . 119.5 ?
N1 C9 C8 . . 111.1(4) ?
N1 C9 C7 . . 111.0(4) ?
N1 C9 H9 . . 108.2 ?
C8 C9 C7 . . 110.0(4) ?
C8 C9 H9 . . 108.2 ?
C7 C9 H9 . . 108.2 ?
C19 C20 H20 . . 119.8 ?
C19 C20 C11 . . 120.4(5) ?
C11 C20 H20 . . 119.8 ?
C18 C17 H17 . . 119.4 ?
C16 C17 C18 . . 121.2(5) ?
C16 C17 H17 . . 119.4 ?
C17 C16 H16 . . 119.8 ?
C17 C16 C15 . . 120.4(5) ?
C15 C16 H16 . . 119.8 ?
C12 C11 C20 . . 118.6(5) ?
C12 C11 C10 . . 120.7(5) ?
C20 C11 C10 . . 120.7(5) ?
C5 C6 H6 . . 119.9 ?
C1 C6 C5 . . 120.3(5) ?
C1 C6 H6 . . 119.9 ?
N1 C10 H10A . . 109.0 ?
N1 C10 H10B . . 109.0 ?
C11 C10 N1 . . 113.1(4) ?
C11 C10 H10A . . 109.0 ?
C11 C10 H10B . . 109.0 ?
H10A C10 H10B . . 107.8 ?
C13 C14 H14 . . 119.6 ?
C15 C14 C13 . . 120.8(5) ?
C15 C14 H14 . . 119.6 ?
C6 C1 H1 . . 120.3 ?
C6 C1 C2 . . 119.5(5) ?
C2 C1 H1 . . 120.3 ?
C16 C15 H15 . . 120.0 ?
C14 C15 C16 . . 120.1(5) ?
C14 C15 H15 . . 120.0 ?
C3 C2 C1 . . 120.2(5) ?
C3 C2 H2A . . 119.9 ?
C1 C2 H2A . . 119.9 ?
C21 O4 H4 . . 109.5 ?
H22A C22 H22B . . 109.5 ?
H22A C22 H22C . . 109.5 ?
H22B C22 H22C . . 109.5 ?
C21 C22 H22A . . 109.5 ?
C21 C22 H22B . . 109.5 ?
C21 C22 H22C . . 109.5 ?
O4 C21 C22 . . 114.4(9) ?
O3 C21 O4 . . 121.6(10) ?
O3 C21 C22 . . 124.0(9) ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
O1 C8 . 1.206(7) ?
O2 H2 . 0.8400 ?
O2 C8 . 1.321(6) ?
N1 H1A . 0.9100 ?
N1 H1B . 0.9100 ?
N1 C9 . 1.484(6) ?
N1 C10 . 1.510(6) ?
C18 C13 . 1.413(7) ?
C18 C19 . 1.409(7) ?
C18 C17 . 1.424(7) ?
C5 H5 . 0.9500 ?
C5 C4 . 1.397(7) ?
C5 C6 . 1.391(8) ?
C8 C9 . 1.516(7) ?
C13 C12 . 1.413(7) ?
C13 C14 . 1.423(7) ?
C4 C7 . 1.505(7) ?
C4 C3 . 1.393(7) ?
C7 H7A . 0.9900 ?
C7 H7B . 0.9900 ?
C7 C9 . 1.543(7) ?
C12 H12 . 0.9500 ?
C12 C11 . 1.372(7) ?
C19 H19 . 0.9500 ?
C19 C20 . 1.354(7) ?
C3 H3 . 0.9500 ?
C3 C2 . 1.388(8) ?
C9 H9 . 1.0000 ?
C20 H20 . 0.9500 ?
C20 C11 . 1.439(7) ?
C17 H17 . 0.9500 ?
C17 C16 . 1.358(7) ?
C16 H16 . 0.9500 ?
C16 C15 . 1.412(8) ?
C11 C10 . 1.495(7) ?
C6 H6 . 0.9500 ?
C6 C1 . 1.373(8) ?
C10 H10A . 0.9900 ?
C10 H10B . 0.9900 ?
C14 H14 . 0.9500 ?
C14 C15 . 1.362(8) ?
C1 H1 . 0.9500 ?
C1 C2 . 1.392(8) ?
C15 H15 . 0.9500 ?
C2 H2A . 0.9500 ?
O4 H4 . 0.8400 ?
O4 C21 . 1.327(12) ?
O3 C21 . 1.257(11) ?
C22 H22A . 0.9800 ?
C22 H22B . 0.9800 ?
C22 H22C . 0.9800 ?
C22 C21 . 1.475(13) ?
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_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
O1 C8 C9 N1 . . . . -18.4(7) ?
O1 C8 C9 C7 . . . . 104.9(6) ?
O2 C8 C9 N1 . . . . 163.6(4) ?
O2 C8 C9 C7 . . . . -73.1(5) ?
C18 C13 C12 C11 . . . . 0.6(7) ?
C18 C13 C14 C15 . . . . 0.3(7) ?
C18 C19 C20 C11 . . . . 0.5(8) ?
C18 C17 C16 C15 . . . . 0.7(8) ?
C5 C4 C7 C9 . . . . -91.1(6) ?
C5 C4 C3 C2 . . . . -0.5(7) ?
C5 C6 C1 C2 . . . . -1.3(8) ?
C13 C18 C19 C20 . . . . 0.5(7) ?
C13 C18 C17 C16 . . . . -0.1(7) ?
C13 C12 C11 C20 . . . . 0.4(7) ?
C13 C12 C11 C10 . . . . -176.5(4) ?
C13 C14 C15 C16 . . . . 0.3(8) ?
C4 C5 C6 C1 . . . . 1.5(8) ?
C4 C7 C9 N1 . . . . 63.2(6) ?
C4 C7 C9 C8 . . . . -60.1(5) ?
C4 C3 C2 C1 . . . . 0.7(8) ?
C7 C4 C3 C2 . . . . 179.3(5) ?
C12 C13 C14 C15 . . . . 180.0(5) ?
C12 C11 C10 N1 . . . . -92.5(6) ?
C19 C18 C13 C12 . . . . -1.0(7) ?
C19 C18 C13 C14 . . . . 178.6(5) ?
C19 C18 C17 C16 . . . . -179.1(5) ?
C19 C20 C11 C12 . . . . -0.9(7) ?
C19 C20 C11 C10 . . . . 176.0(5) ?
C3 C4 C7 C9 . . . . 89.2(6) ?
C9 N1 C10 C11 . . . . -62.7(6) ?
C20 C11 C10 N1 . . . . 90.6(5) ?
C17 C18 C13 C12 . . . . 179.9(4) ?
C17 C18 C13 C14 . . . . -0.4(7) ?
C17 C18 C19 C20 . . . . 179.5(5) ?
C17 C16 C15 C14 . . . . -0.8(8) ?
C6 C5 C4 C7 . . . . 179.6(5) ?
C6 C5 C4 C3 . . . . -0.6(7) ?
C6 C1 C2 C3 . . . . 0.2(8) ?
C10 N1 C9 C8 . . . . -59.2(5) ?
C10 N1 C9 C7 . . . . 178.1(4) ?
C14 C13 C12 C11 . . . . -179.1(5) ?
_cod_database_fobs_code 2312743