#------------------------------------------------------------------------------
#$Date: 2018-10-25 05:40:06 +0300 (Thu, 25 Oct 2018) $
#$Revision: 211615 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/02/12/2021284.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_2021284
loop_
_publ_author_name
'Owczarzak, Agata'
'Przyby\/l, Anna K.'
'Kubicki, Maciej'
_publ_section_title
;
Different cationic forms of (--)-cytisine in the crystal structures of
its simple inorganic salts
;
_journal_coeditor_code YF3149
_journal_issue 11
_journal_name_full 'Acta Crystallographica Section C'
_journal_page_first
;
;
_journal_paper_doi 10.1107/S2053229618012585
_journal_volume 74
_journal_year 2018
_chemical_absolute_configuration rmad
_chemical_formula_iupac 'C11 H15 N2 O +, Cl -, H2 O'
_chemical_formula_moiety 'C11 H15 N2 O +, Cl -, H2 O'
_chemical_formula_sum 'C11 H17 Cl N2 O2'
_chemical_formula_weight 244.71
_chemical_name_common
;
Cytisinium chloride monohydrate
;
_chemical_name_systematic
;
6-Oxo-7,11-diazatricyclo[7.3.1.0^2,7^]trideca-2,4-dien-11-ium chloride
monohydrate
;
_space_group_crystal_system monoclinic
_space_group_IT_number 4
_space_group_name_Hall 'P 2yb'
_space_group_name_H-M_alt 'P 1 21 1'
_symmetry_space_group_name_Hall 'P 2yb'
_symmetry_space_group_name_H-M 'P 1 21 1'
_atom_sites_solution_hydrogens difmap
_audit_creation_method SHELXL-2013
_cell_angle_alpha 90
_cell_angle_beta 108.559(3)
_cell_angle_gamma 90
_cell_formula_units_Z 2
_cell_length_a 7.6327(2)
_cell_length_b 10.4510(2)
_cell_length_c 7.6553(2)
_cell_measurement_reflns_used 6830
_cell_measurement_temperature 100.0(10)
_cell_measurement_theta_max 28.7770
_cell_measurement_theta_min 3.2530
_cell_volume 578.90(3)
_computing_cell_refinement
;
(CrysAlis PRO; Agilent, 2014)
;
_computing_data_collection
;
(CrysAlis PRO; Agilent, 2014)
;
_computing_data_reduction
;
(CrysAlis PRO; Agilent, 2014)
;
_computing_molecular_graphics
;
Mercury (Macrae et al., 2008)
;
_computing_publication_material
;
SHELXL2014 (Sheldrick, 2015b)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT (Sheldrick, 2015a)
;
_diffrn_ambient_temperature 100.0(10)
_diffrn_detector 'CCD plate'
_diffrn_detector_area_resol_mean 16.1544
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.935
_diffrn_measurement_device 'four-circle diffractometer'
_diffrn_measurement_device_type 'Agilent Xcalibur Eos'
_diffrn_measurement_method '\w scan'
_diffrn_radiation_monochromator graphite
_diffrn_radiation_probe x-ray
_diffrn_radiation_type 'Mo K\a'
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0343
_diffrn_reflns_av_unetI/netI 0.0297
_diffrn_reflns_limit_h_max 10
_diffrn_reflns_limit_h_min -9
_diffrn_reflns_limit_k_max 13
_diffrn_reflns_limit_k_min -14
_diffrn_reflns_limit_l_max 10
_diffrn_reflns_limit_l_min -10
_diffrn_reflns_number 12838
_diffrn_reflns_theta_full 25.000
_diffrn_reflns_theta_max 29.054
_diffrn_reflns_theta_min 3.283
_diffrn_source 'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu 0.318
_exptl_absorpt_correction_T_max 1.00000
_exptl_absorpt_correction_T_min 0.94783
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
(CrysAlis PRO; Agilent, 2014)
;
_exptl_crystal_colour colourless
_exptl_crystal_density_diffrn 1.404
_exptl_crystal_description prism
_exptl_crystal_F_000 260
_exptl_crystal_size_max 0.3
_exptl_crystal_size_mid 0.2
_exptl_crystal_size_min 0.15
_refine_diff_density_max 0.304
_refine_diff_density_min -0.180
_refine_ls_abs_structure_details
;
Flack x determined using 1146 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons et al., 2013)
;
_refine_ls_abs_structure_Flack -0.05(2)
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.036
_refine_ls_hydrogen_treatment refall
_refine_ls_matrix_type full
_refine_ls_number_parameters 213
_refine_ls_number_reflns 2796
_refine_ls_number_restraints 1
_refine_ls_restrained_S_all 1.035
_refine_ls_R_factor_all 0.0312
_refine_ls_R_factor_gt 0.0286
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0399P)^2^+0.0651P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0668
_refine_ls_wR_factor_ref 0.0682
_reflns_number_gt 2653
_reflns_number_total 2796
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file yf3149sup1.cif
_cod_data_source_block 5
_cod_database_code 2021284
_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_hkl_file
;
0 0 2 2426.54 364.176 16
0 0 -2 2670.46 349.958 2
0 0 -2 2060.96 339.547 8
0 0 -2 1856.52 361.256 1
0 0 2 2121.94 373.596 1
0 0 -2 2778.63 294.798 9
0 0 2 2569.67 412.199 8
0 0 2 2179.12 312.184 2
0 0 -2 2022.15 408.878 16
0 0 -3 223604. 5753.76 8
0 0 3 227728. 5759.00 8
0 0 -3 223811. 5798.10 16
0 0 -3 224881. 5526.14 9
0 0 3 234014. 5668.86 2
0 0 3 228792. 5796.37 16
0 0 -3 225331. 5669.42 2
0 0 3 220309. 5775.18 1
0 0 -3 235344. 5800.78 1
0 0 -4 60924.2 1869.16 9
0 0 4 56919.4 2115.92 1
0 0 4 61200.9 2122.72 8
0 0 -4 59637.8 2161.01 16
0 0 -4 59724.3 2032.83 2
0 0 5-569.589 487.933 1
0 0 -5 141.491 400.318 2
0 0 5-110.039 362.055 10
0 0 -5-260.088 366.008 9
0 0 -5-16.0842 216.041 11
0 0 5-728.011 566.545 8
0 0 -5-250.947 517.502 16
0 0 6 16476.6 1222.87 8
0 0 -6 15377.2 1223.65 16
0 0 -6 13071.5 1029.38 2
0 0 6 13167.9 1153.37 1
0 0 -6 14553.4 914.171 9
0 0 6 16220.4 1005.20 10
0 0 7 1604.37 497.553 10
0 0 -7 972.607 533.250 2
0 0 -7 2867.41 805.109 16
0 0 7 1356.15 661.121 8
0 0 7 443.283 543.688 1
0 0 7 2451.73 576.139 6
0 0 8-277.972 707.188 8
0 0 -8 271.581 564.805 2
0 0 8 867.110 1108.32 1
0 0 -8 485.000 669.503 16
0 0 8 513.094 750.565 13
0 0 9 607.767 706.868 1
0 0 -9 132.322 758.862 16
0 0 9 362.095 760.993 8
0 0 9 66.2406 982.169 13
0 -1 1 27043.6 2438.45 16
0 1 1 26876.3 2613.73 13
0 -1 -1 2854.83 2554.57 14
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0 1 1 8999.60 2558.66 14
0 -1 1 32719.7 2432.91 1
0 -1 -1 14654.4 2421.02 8
0 1 -1 12238.8 2591.66 2
0 -1 -1 3755.73 2506.28 10
0 1 1 21786.3 2582.28 1
0 -1 -1 37744.2 2646.33 16
0 -1 -1 2741.97 2631.39 9
0 1 -1 59.8764 2409.78 16
0 -1 -1 44793.9 2668.76 1
0 -1 -1-0.10083 2483.36 6
0 1 -1 7796.60 2561.72 15
0 1 1 15278.6 2498.56 10
0 1 1 13264.0 2592.83 16
0 1 -2 90368.9 2425.02 1
0 -1 -2 91620.3 2414.19 11
0 1 2 91485.3 2226.05 4
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0 1 2 89625.9 2402.53 6
0 1 2 89483.4 2605.73 13
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0 1 2 93117.3 2413.82 8
0 -1 2 91797.6 2529.66 2
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0 1 2 93906.4 2576.08 16
0 1 -2 93484.5 2543.09 2
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0 -1 2 91504.3 2581.88 8
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0 1 2 88576.9 2549.95 1
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0 1 2 95658.8 2582.64 14
0 -1 2 89700.0 2410.68 1
0 1 2 94843.0 2320.19 2
0 -1 -3 210777. 5648.63 16
0 -1 3 225222. 5574.03 2
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0 -1 4 83115.8 2618.07 1
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0 -1 4 82413.2 2727.23 8
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0 -1 5 21519.4 1350.91 8
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0 -1 5 20671.6 1224.63 1
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0 3 2 440.751 371.585 1
0 -3 2 1232.42 406.360 2
0 -3 -2 590.465 344.638 1
0 -3 2 188.389 441.497 8
0 -3 -2 623.445 462.641 9
0 3 2 675.505 177.245 3
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0 -3 -2 1137.83 426.686 16
0 3 -2 568.094 461.689 2
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-8 8 1 1902.37 750.960 7
-8 8 0 7380.17 1177.95 7
-8 8 0 8377.06 1339.27 12
8 9 -3 15149.3 1599.29 10
-9 0 6 2583.44 784.041 8
9 0 -5 1497.36 740.754 2
-9 0 5 2958.11 993.202 7
9 0 -4 4739.50 1040.19 2
-9 0 4 6094.83 1204.51 7
9 0 -3 4140.18 836.478 10
9 0 -3 4484.84 983.685 2
-9 0 3 3505.74 1026.43 7
9 0 -2 5491.58 975.582 10
9 0 -2 6497.00 956.180 6
9 0 -2 6129.95 1134.89 2
-9 0 2 6801.19 1150.59 7
9 0 -1 36855.7 2301.24 3
-9 0 1 36287.5 2455.08 7
9 0 -1 32145.0 2168.44 6
9 0 -1 34636.4 2259.87 10
9 0 0 93500.0 3850.71 3
-9 0 0 92974.0 4211.47 7
9 0 0 84473.8 3899.01 6
9 0 0 86594.1 3992.30 10
-9 -1 7 12472.1 1442.45 8
-9 -1 6 53719.3 2869.53 8
-9 1 6 51274.6 2786.01 11
9 1 -5 10701.3 1428.43 2
9 -1 -5 12502.4 1510.91 2
-9 -1 5 10672.3 1357.02 7
-9 1 5 14674.3 1589.15 7
-9 -1 4 19248.6 1740.77 7
-9 1 4 17225.2 1699.85 7
9 1 -4 20249.0 1813.67 2
9 -1 -4 18232.6 1770.64 2
-9 -1 3 21843.8 1895.99 7
-9 1 3 25459.3 2035.07 7
9 1 -3 27313.6 2059.21 2
9 -1 -3 25066.0 1976.88 2
9 -1 -3 25354.7 1727.29 10
9 1 -3 22347.7 1624.42 10
9 -1 -2 10810.4 1250.52 10
9 1 -2 10045.2 1221.30 10
9 -1 -2 7678.38 1057.30 6
9 1 -2 7715.25 1052.38 6
9 -1 -2 10268.4 1337.02 3
9 1 -2 11151.9 1380.46 2
-9 -1 2 9327.26 1319.48 7
-9 1 2 9951.90 1399.40 7
9 1 -1 14055.8 1458.99 6
9 -1 -1 17513.4 1647.87 3
9 1 -1 14282.7 1499.36 2
-9 -1 1 13363.0 1563.72 7
-9 1 1 14842.5 1608.14 7
9 -1 -1 15323.3 1520.59 6
9 -1 -1 14634.0 1535.53 10
9 1 -1 15864.7 1574.19 10
9 -1 0 34027.6 2234.83 3
-9 -1 0 30993.1 2264.17 7
-9 1 0 31136.9 2374.83 7
9 -1 0 33249.1 2294.75 6
9 1 0 31727.0 2215.74 6
9 -1 0 28789.5 2173.58 10
9 1 0 30596.2 2243.90 10
-9 -2 7-507.269 829.485 8
-9 -2 6 8580.88 1268.87 8
-9 2 6 8232.59 1206.10 11
9 2 -5 3903.93 1009.83 2
9 -2 -5 5125.32 1074.31 2
-9 -2 5 5079.13 1072.90 7
-9 2 5 6238.75 1234.76 7
9 2 -4 1456.15 791.159 2
9 -2 -4 2942.72 990.063 2
-9 -2 4 3633.70 933.221 7
-9 2 4 1984.34 880.480 7
9 -2 -3 1016.63 631.392 10
9 2 -3 1080.93 632.397 10
9 2 -3 610.735 533.848 6
9 2 -3 1353.58 740.745 2
9 -2 -3 1676.81 949.217 2
-9 -2 3 2928.18 897.415 7
-9 2 3-26.0391 832.780 7
9 -2 -2 10619.0 1240.04 10
9 -2 -2 9054.76 1111.37 6
9 2 -2 7642.53 1122.45 10
9 2 -2 9262.68 1125.92 6
9 2 -2 8665.55 1284.15 2
-9 -2 2 8840.58 1282.44 7
-9 2 2 9348.42 1336.38 7
9 -2 -2 10966.5 1334.79 3
9 -2 -1 1724.62 855.675 10
9 -2 -1 1012.19 749.433 6
9 2 -1 1162.22 748.169 10
9 2 -1 1818.90 715.739 6
9 2 -1 1637.59 749.478 2
-9 -2 1 1608.28 933.207 7
-9 2 1 2996.14 890.220 7
9 -2 -1 1490.27 782.794 3
9 -2 0 1223.19 854.730 10
9 -2 0 1638.42 858.007 6
9 2 0 2109.49 915.519 10
9 2 0 3389.70 1041.67 6
9 2 0 1782.34 761.172 2
-9 -2 0 640.172 692.034 7
9 -2 0 2587.88 912.369 3
9 -2 1 20506.5 1814.13 3
-9 -3 6 26981.8 2134.61 8
-9 3 6 23749.4 1937.48 11
9 3 -5 2546.69 935.841 2
9 -3 -5 2324.68 983.925 2
-9 -3 5 866.336 719.426 7
-9 3 5-443.777 807.965 7
-9 3 5 379.297 753.422 11
-9 -3 4 34355.0 2346.46 7
-9 3 4 36890.8 2437.35 7
9 3 -4 33852.5 2355.00 2
9 -3 -4 31679.5 2325.26 2
9 3 -3 5806.86 933.764 10
9 3 -3 6202.24 942.384 6
9 3 -3 7049.54 1147.59 2
-9 -3 3 4925.19 1103.63 7
-9 3 3 5575.65 1099.40 7
9 -3 -3 4714.93 1110.70 3
9 -3 -2 13079.0 1319.30 6
9 -3 -2 16354.7 1632.10 3
9 3 -2 16358.4 1612.85 2
-9 -3 2 13945.7 1513.44 7
-9 3 2 13589.6 1537.21 7
9 3 -2 15832.9 1446.69 6
9 3 -2 15284.7 1486.75 10
9 -3 -1 349.579 708.039 6
9 3 -1 97.2014 757.733 10
9 3 -1 1647.55 732.862 6
9 3 -1 362.314 647.095 2
-9 -3 1 63.8335 724.246 7
-9 3 1 1282.80 892.102 7
9 -3 -1 1655.08 813.735 3
9 -3 0 9297.93 1328.89 6
9 3 0 9625.77 1405.94 10
9 3 0 8866.16 1365.62 6
9 3 0 9159.72 1241.01 2
9 -3 0 12429.5 1370.69 15
-9 -3 0 8524.01 1360.95 7
9 -3 0 13315.9 1474.13 3
9 -3 1 7303.04 1177.54 15
9 -3 1 8047.45 1270.75 3
-9 4 6 6781.15 1208.93 11
-9 -4 5 15609.7 1675.58 8
-9 -4 5 13366.0 1518.37 7
-9 4 5 14209.7 1651.20 7
-9 4 5 13121.0 1599.21 11
9 4 -4 4283.83 1009.66 2
9 -4 -4 3352.47 946.588 2
-9 -4 4 5359.44 1070.00 7
-9 4 4 5453.84 1109.50 7
-9 4 4 6327.51 1293.98 11
9 4 -3 7519.42 1037.47 10
9 4 -3 8236.64 1089.11 6
9 4 -3 7381.24 1153.47 2
-9 -4 3 7577.94 1214.46 7
-9 4 3 9483.27 1318.77 7
9 -4 -3 7801.38 1276.04 3
9 4 -2 1992.04 773.937 10
9 4 -2 2840.80 855.807 6
9 4 -2 1188.53 804.891 2
-9 -4 2 2100.39 890.543 7
-9 4 2 3073.19 969.801 7
9 -4 -2 3734.11 1024.44 3
9 4 -1 3529.84 908.330 10
9 4 -1 777.857 721.407 6
9 4 -1 2844.45 849.900 2
-9 -4 1 1101.73 803.714 7
-9 4 1 1912.10 795.409 7
9 -4 -1 3730.99 1029.91 3
9 -4 -1 2567.27 855.513 6
9 -4 0 11970.1 1388.11 15
-9 -4 0 8578.45 1305.70 14
-9 -4 0 9048.28 1316.43 7
9 -4 0 8956.80 1314.03 6
-9 -4 -1 412.082 902.676 14
-9 -5 5 33728.5 2417.88 7
9 5 -4 3039.59 936.177 2
-9 -5 4 5329.10 1081.10 7
-9 5 4 3884.51 1011.66 7
9 5 -3 2724.76 796.146 6
9 5 -3 3242.80 851.138 2
-9 -5 3 3118.03 932.684 7
-9 5 3 2475.74 795.411 7
9 5 -2 14542.0 1537.13 10
-9 5 2 18360.2 1757.57 7
-9 -5 2 16042.6 1537.95 14
9 5 -2 20171.0 1684.49 2
-9 -5 2 14302.7 1558.70 7
9 5 -2 18288.1 1659.81 6
9 5 -1 966.798 785.459 10
9 5 -1 3357.59 957.463 6
-9 -5 1 1189.96 865.703 14
-9 -5 1 2761.47 888.580 7
-9 -5 0 2099.05 1005.62 14
9 6 -4 678.818 670.468 2
-9 -6 4-670.766 800.972 7
-9 6 4-554.188 856.391 7
9 6 -3 1156.82 743.281 6
9 6 -3 3688.80 972.377 2
-9 -6 3 2742.87 936.819 14
-9 -6 3 1895.13 758.123 7
-9 6 3 2414.38 944.381 7
9 6 -2 3901.62 977.131 10
9 6 -2 3701.76 998.722 6
-9 -6 2 5449.29 1103.90 14
-9 -6 2 6168.41 1124.20 7
-9 6 2 4374.41 1085.97 7
-9 -6 1 7097.05 1284.20 14
-9 -6 1 8069.45 1227.20 7
-9 -7 3 6696.46 1185.49 14
10 0 -2 64.2269 730.323 10
10 0 -1-1035.61 896.139 6
10 -1 -2 6932.27 1193.44 10
10 1 -2 5402.37 1096.34 10
10 -1 -1 3736.64 969.797 6
10 -1 -1 5549.65 1108.94 3
10 -2 -2-286.941 864.502 10
10 2 -2-812.101 771.575 10
10 2 -2-1012.74 824.689 6
10 -2 -1-126.767 723.528 6
10 -3 -2 22040.7 1880.19 10
10 3 -2 21373.2 1858.80 6
10 3 -2 22968.1 1935.55 10
0 0 0 0.00 0.00 0
;
_shelx_hkl_checksum 41884
_shelx_res_file
;
shelx.res created by SHELXL-2014/7
TITL ap8 in P2(1)
CELL 0.71073 7.6327 10.4510 7.6553 90.000 108.559 90.000
ZERR 2.00 0.0002 0.0002 0.0002 0.000 0.003 0.000
LATT -1
SYMM - X, 1/2 + Y, - Z
SFAC C H N O CL
UNIT 22 34 4 4 2
MERG 2
OMIT 0 1 1
OMIT 1 -1 0
OMIT 1 1 0
OMIT 0 -1 1
OMIT 6 -6 5
mpla n1 c2 c3 c4 c5 c6
FMAP 2
PLAN 20
ACTA 50.00
HTAB C5 Cl1
EQIV $1 -x+1, y-1/2, -z+1
HTAB C11 O1W_$1
HTAB C11 Cl1_$1
EQIV $2 x-1, y, z
HTAB N12 O2_$2
EQIV $3 -x+1, y-1/2, -z
HTAB N12 Cl1_$3
HTAB C13 Cl1
EQIV $4 x, y, z+1
HTAB O1W Cl1_$4
HTAB O1W Cl1_$1
BOND $H
CONF
L.S. 4
WGHT 0.039900 0.065100
FVAR 13.75626
N1 3 0.952839 0.401644 0.341096 11.00000 0.01053 0.01077 =
0.01132 0.00050 0.00380 -0.00024
C2 1 1.070423 0.376431 0.238753 11.00000 0.01015 0.01361 =
0.01300 -0.00279 0.00338 -0.00319
O2 4 1.175339 0.280523 0.281566 11.00000 0.01199 0.01525 =
0.01937 0.00030 0.00652 0.00066
C3 1 1.063872 0.462999 0.094078 11.00000 0.01364 0.01945 =
0.01307 -0.00250 0.00581 -0.00373
REM AFIX 43
H3 2 1.138646 0.447373 0.020007 11.00000 0.02112
REM AFIX 0
C4 1 0.950949 0.566876 0.061292 11.00000 0.01962 0.01611 =
0.01038 0.00246 0.00302 -0.00500
REM AFIX 43
H4 2 0.945330 0.622527 -0.035027 11.00000 0.01725
REM AFIX 0
C5 1 0.835227 0.589005 0.169108 11.00000 0.01434 0.01193 =
0.01326 -0.00025 0.00124 -0.00167
REM AFIX 43
H5 2 0.753871 0.660522 0.147567 11.00000 0.02158
REM AFIX 0
C6 1 0.838886 0.506796 0.308324 11.00000 0.01026 0.01193 =
0.01217 -0.00306 0.00183 -0.00175
C7 1 0.718427 0.528627 0.428944 11.00000 0.01405 0.00898 =
0.01564 -0.00151 0.00501 -0.00007
REM AFIX 13
H7 2 0.707181 0.616888 0.436832 11.00000 0.01863
REM AFIX 0
C8 1 0.806097 0.470969 0.619342 11.00000 0.01582 0.01756 =
0.01257 -0.00332 0.00481 -0.00171
REM AFIX 23
H8A 2 0.914636 0.514335 0.673731 11.00000 0.01579
H8B 2 0.736727 0.486903 0.704242 11.00000 0.02230
REM AFIX 0
C9 1 0.826617 0.328834 0.591682 11.00000 0.01390 0.01686 =
0.01218 0.00340 0.00580 0.00172
REM AFIX 13
H9 2 0.875956 0.286306 0.709995 11.00000 0.01638
REM AFIX 0
C10 1 0.967064 0.308245 0.491155 11.00000 0.01389 0.01511 =
0.01565 0.00505 0.00599 0.00282
REM AFIX 23
H10A 2 1.096040 0.319783 0.581354 11.00000 0.02376
H10B 2 0.963855 0.220305 0.440418 11.00000 0.00566
REM AFIX 0
C11 1 0.639474 0.266419 0.498006 11.00000 0.01564 0.01521 =
0.01614 0.00215 0.00830 0.00129
REM AFIX 23
H11A 2 0.652898 0.176311 0.467975 11.00000 0.02312
H11B 2 0.565624 0.271372 0.581255 11.00000 0.01084
REM AFIX 0
N12 3 0.532546 0.331560 0.322412 11.00000 0.01179 0.01373 =
0.01388 -0.00184 0.00555 -0.00167
REM AFIX 23
H12A 2 0.419289 0.308043 0.292651 11.00000 0.01276
H12B 2 0.574447 0.308842 0.226892 11.00000 0.01168
REM AFIX 0
C13 1 0.525334 0.473583 0.341483 11.00000 0.01357 0.01172 =
0.01758 -0.00058 0.00632 0.00110
REM AFIX 23
H13A 2 0.455335 0.481846 0.419586 11.00000 0.01105
H13B 2 0.471003 0.507971 0.220122 11.00000 0.02245
REM AFIX 0
CL1 5 0.375660 0.749893 0.026059 11.00000 0.02556 0.02575 =
0.02047 0.01003 0.01306 0.00912
O1W 4 0.358552 0.491574 0.770805 11.00000 0.04592 0.03692 =
0.03279 0.00020 0.00670 0.00064
H1W2 2 0.354831 0.565239 0.849775 11.00000 0.07200
H1W1 2 0.425132 0.431845 0.832772 11.00000 0.05011
HKLF 4
REM ap8 in P2(1)
REM R1 = 0.0286 for 2653 Fo > 4sig(Fo) and 0.0312 for all 2796 data
REM 213 parameters refined using 1 restraints
END
WGHT 0.0396 0.0672
REM Highest difference peak 0.304, deepest hole -0.180, 1-sigma level 0.047
Q1 1 0.3155 0.6913 -0.0386 11.00000 0.05 0.30
Q2 1 0.7898 0.5237 0.3763 11.00000 0.05 0.25
Q3 1 0.7565 0.5044 0.5342 11.00000 0.05 0.22
Q4 1 0.2543 0.5643 0.7578 11.00000 0.05 0.22
Q5 1 1.0491 0.4268 0.1735 11.00000 0.05 0.21
Q6 1 0.5283 0.4047 0.3306 11.00000 0.05 0.21
Q7 1 0.4117 0.7024 -0.0587 11.00000 0.05 0.21
Q8 1 1.0165 0.4041 0.3040 11.00000 0.05 0.20
Q9 1 0.8711 0.4187 0.2997 11.00000 0.05 0.19
Q10 1 0.8681 0.5596 0.2580 11.00000 0.05 0.19
Q11 1 0.3861 0.7804 -0.0721 11.00000 0.05 0.19
Q12 1 0.9555 0.3634 0.4084 11.00000 0.05 0.19
Q13 1 0.7123 0.3152 0.5186 11.00000 0.05 0.18
Q14 1 1.2821 0.4991 0.0532 11.00000 0.05 0.18
Q15 1 0.8104 0.3927 0.5910 11.00000 0.05 0.18
Q16 1 0.4721 0.8224 0.0821 11.00000 0.05 0.17
Q17 1 0.8750 0.3217 0.5219 11.00000 0.05 0.16
Q18 1 0.7846 0.5542 0.2430 11.00000 0.05 0.16
Q19 1 0.9272 0.5922 0.1376 11.00000 0.05 0.16
Q20 1 1.0319 0.5277 0.1158 11.00000 0.05 0.15
;
_shelx_res_checksum 43437
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, 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
N N1 0.9528(2) 0.40164(16) 0.3411(2) 0.0108(3) Uani d 1
C C2 1.0704(3) 0.37643(19) 0.2388(3) 0.0123(4) Uani d 1
O O2 1.1753(2) 0.28052(13) 0.2816(2) 0.0152(3) Uani d 1
C C3 1.0639(3) 0.4630(2) 0.0941(3) 0.0150(4) Uani d 1
H H3 1.139(4) 0.447(3) 0.020(4) 0.021(7) Uiso d 1
C C4 0.9509(3) 0.5669(2) 0.0613(3) 0.0158(4) Uani d 1
H H4 0.945(4) 0.623(3) -0.035(4) 0.017(6) Uiso d 1
C C5 0.8352(3) 0.5890(2) 0.1691(3) 0.0139(4) Uani d 1
H H5 0.754(4) 0.661(3) 0.148(4) 0.022(7) Uiso d 1
C C6 0.8389(3) 0.50680(18) 0.3083(3) 0.0119(4) Uani d 1
C C7 0.7184(3) 0.52863(19) 0.4289(3) 0.0128(4) Uani d 1
H H7 0.707(4) 0.617(3) 0.437(4) 0.019(7) Uiso d 1
C C8 0.8061(3) 0.4710(2) 0.6193(3) 0.0152(4) Uani d 1
H H8A 0.915(4) 0.514(2) 0.674(4) 0.016(6) Uiso d 1
H H8B 0.737(4) 0.487(3) 0.704(4) 0.022(7) Uiso d 1
C C9 0.8266(3) 0.3288(2) 0.5917(3) 0.0139(4) Uani d 1
H H9 0.876(4) 0.286(2) 0.710(4) 0.016(6) Uiso d 1
C C10 0.9671(3) 0.3082(2) 0.4912(3) 0.0146(4) Uani d 1
H H10A 1.096(4) 0.320(3) 0.581(4) 0.024(7) Uiso d 1
H H10B 0.964(3) 0.220(2) 0.440(3) 0.006(5) Uiso d 1
C C11 0.6395(3) 0.2664(2) 0.4980(3) 0.0149(4) Uani d 1
H H11A 0.653(4) 0.176(3) 0.468(4) 0.023(8) Uiso d 1
H H11B 0.566(3) 0.271(2) 0.581(3) 0.011(6) Uiso d 1
N N12 0.5325(3) 0.33156(17) 0.3224(2) 0.0128(4) Uani d 1
H H12A 0.419(4) 0.308(2) 0.293(3) 0.013(6) Uiso d 1
H H12B 0.574(4) 0.309(2) 0.227(3) 0.012(6) Uiso d 1
C C13 0.5253(3) 0.4736(2) 0.3415(3) 0.0140(4) Uani d 1
H H13A 0.455(4) 0.482(2) 0.420(3) 0.011(6) Uiso d 1
H H13B 0.471(4) 0.508(3) 0.220(4) 0.022(7) Uiso d 1
Cl Cl1 0.37566(8) 0.74989(5) 0.02606(7) 0.02257(15) Uani d 1
O O1W 0.3586(3) 0.4916(2) 0.7708(3) 0.0399(5) Uani d 1
H H1W2 0.355(6) 0.565(4) 0.850(6) 0.072(13) Uiso d 1
H H1W1 0.425(5) 0.432(4) 0.833(5) 0.050(11) Uiso 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
N1 0.0105(8) 0.0108(8) 0.0113(8) -0.0002(6) 0.0038(6) 0.0005(6)
C2 0.0101(9) 0.0136(9) 0.0130(9) -0.0032(7) 0.0034(7) -0.0028(7)
O2 0.0120(7) 0.0152(8) 0.0194(7) 0.0007(5) 0.0065(6) 0.0003(5)
C3 0.0136(10) 0.0194(10) 0.0131(10) -0.0037(8) 0.0058(8) -0.0025(8)
C4 0.0196(11) 0.0161(10) 0.0104(9) -0.0050(8) 0.0030(8) 0.0025(8)
C5 0.0143(10) 0.0119(9) 0.0133(10) -0.0017(8) 0.0012(8) -0.0002(8)
C6 0.0103(9) 0.0119(9) 0.0122(9) -0.0018(7) 0.0018(8) -0.0031(7)
C7 0.0140(10) 0.0090(9) 0.0156(10) -0.0001(8) 0.0050(8) -0.0015(7)
C8 0.0158(10) 0.0176(10) 0.0126(10) -0.0017(9) 0.0048(8) -0.0033(8)
C9 0.0139(10) 0.0169(10) 0.0122(9) 0.0017(8) 0.0058(8) 0.0034(8)
C10 0.0139(11) 0.0151(10) 0.0157(10) 0.0028(8) 0.0060(8) 0.0051(8)
C11 0.0156(10) 0.0152(12) 0.0161(9) 0.0013(8) 0.0083(8) 0.0021(8)
N12 0.0118(9) 0.0137(8) 0.0139(9) -0.0017(7) 0.0055(7) -0.0018(7)
C13 0.0136(10) 0.0117(10) 0.0176(10) 0.0011(8) 0.0063(8) -0.0006(8)
Cl1 0.0256(3) 0.0258(3) 0.0205(3) 0.0091(2) 0.0131(2) 0.0100(2)
O1W 0.0459(13) 0.0369(12) 0.0328(11) 0.0006(10) 0.0067(10) 0.0002(9)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 '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 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 '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
C6 N1 C2 122.20(17)
C6 N1 C10 123.58(16)
C2 N1 C10 114.18(15)
O2 C2 N1 118.35(17)
O2 C2 C3 124.90(19)
N1 C2 C3 116.75(18)
C4 C3 C2 121.1(2)
C4 C3 H3 120.0(18)
C2 C3 H3 118.9(18)
C3 C4 C5 120.18(19)
C3 C4 H4 120.9(18)
C5 C4 H4 118.9(17)
C6 C5 C4 119.7(2)
C6 C5 H5 118.7(17)
C4 C5 H5 121.6(17)
C5 C6 N1 120.09(19)
C5 C6 C7 121.14(18)
N1 C6 C7 118.77(17)
C6 C7 C8 110.94(17)
C6 C7 C13 111.43(17)
C8 C7 C13 109.90(18)
C6 C7 H7 106.0(17)
C8 C7 H7 110.6(17)
C13 C7 H7 107.8(17)
C9 C8 C7 106.73(17)
C9 C8 H8A 115.3(16)
C7 C8 H8A 107.3(16)
C9 C8 H8B 111.3(16)
C7 C8 H8B 113.9(17)
H8A C8 H8B 102(2)
C8 C9 C10 109.28(18)
C8 C9 C11 111.21(18)
C10 C9 C11 114.01(18)
C8 C9 H9 110.2(15)
C10 C9 H9 106.3(16)
C11 C9 H9 105.7(15)
N1 C10 C9 114.12(17)
N1 C10 H10A 105.4(16)
C9 C10 H10A 109.1(15)
N1 C10 H10B 108.6(13)
C9 C10 H10B 113.2(14)
H10A C10 H10B 106(2)
N12 C11 C9 112.90(17)
N12 C11 H11A 107.1(16)
C9 C11 H11A 111.6(18)
N12 C11 H11B 107.4(14)
C9 C11 H11B 108.6(14)
H11A C11 H11B 109(2)
C13 N12 C11 113.00(17)
C13 N12 H12A 104.2(17)
C11 N12 H12A 108.9(17)
C13 N12 H12B 111.6(15)
C11 N12 H12B 111.7(16)
H12A N12 H12B 107(2)
N12 C13 C7 110.93(18)
N12 C13 H13A 101.7(16)
C7 C13 H13A 111.0(15)
N12 C13 H13B 107.2(17)
C7 C13 H13B 110.1(18)
H13A C13 H13B 116(2)
H1W2 O1W H1W1 111(3)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
N1 C6 1.374(3)
N1 C2 1.392(3)
N1 C10 1.485(3)
C2 O2 1.259(3)
C2 C3 1.419(3)
C3 C4 1.359(3)
C3 H3 0.94(3)
C4 C5 1.407(3)
C4 H4 0.93(3)
C5 C6 1.362(3)
C5 H5 0.95(3)
C6 C7 1.513(3)
C7 C8 1.521(3)
C7 C13 1.524(3)
C7 H7 0.93(3)
C8 C9 1.516(3)
C8 H8A 0.92(3)
C8 H8B 0.97(3)
C9 C10 1.521(3)
C9 C11 1.526(3)
C9 H9 0.97(3)
C10 H10A 1.01(3)
C10 H10B 1.00(2)
C11 N12 1.496(3)
C11 H11A 0.98(3)
C11 H11B 0.98(2)
N12 C13 1.494(3)
N12 H12A 0.86(3)
N12 H12B 0.92(3)
C13 H13A 0.92(2)
C13 H13B 0.96(3)
O1W H1W2 0.98(4)
O1W H1W1 0.85(4)
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
N12 H12A O2 1_455 0.86(3) 1.86(3) 2.697(2) 165(2)
N12 H12B Cl1 2_645 0.92(3) 2.18(3) 3.0863(19) 170(2)
O1W H1W2 Cl1 1_556 0.98(4) 2.33(5) 3.311(2) 173(4)
O1W H1W1 Cl1 2_646 0.85(4) 2.46(4) 3.302(2) 172(3)
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
C6 N1 C2 O2 177.52(18)
C10 N1 C2 O2 -0.4(3)
C6 N1 C2 C3 -1.7(3)
C10 N1 C2 C3 -179.60(18)
O2 C2 C3 C4 -177.6(2)
N1 C2 C3 C4 1.6(3)
C2 C3 C4 C5 -1.2(3)
C3 C4 C5 C6 1.0(3)
C4 C5 C6 N1 -1.1(3)
C4 C5 C6 C7 179.09(18)
C2 N1 C6 C5 1.5(3)
C10 N1 C6 C5 179.21(19)
C2 N1 C6 C7 -178.64(17)
C10 N1 C6 C7 -1.0(3)
C5 C6 C7 C8 -152.29(19)
N1 C6 C7 C8 27.9(2)
C5 C6 C7 C13 84.9(2)
N1 C6 C7 C13 -94.9(2)
C6 C7 C8 C9 -60.1(2)
C13 C7 C8 C9 63.6(2)
C7 C8 C9 C10 66.7(2)
C7 C8 C9 C11 -60.1(2)
C6 N1 C10 C9 7.4(3)
C2 N1 C10 C9 -174.76(18)
C8 C9 C10 N1 -40.3(2)
C11 C9 C10 N1 84.8(2)
C8 C9 C11 N12 53.4(2)
C10 C9 C11 N12 -70.7(2)
C9 C11 N12 C13 -48.3(2)
C11 N12 C13 C7 51.3(2)
C6 C7 C13 N12 63.5(2)
C8 C7 C13 N12 -59.9(2)
_cod_database_fobs_code 2021284