#------------------------------------------------------------------------------
#$Date: 2018-10-25 05:40:06 +0300 (Thu, 25 Oct 2018) $
#$Revision: 211615 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/02/12/2021282.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_2021282
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 syn
_chemical_formula_iupac          'C11 H15 N2 O +, Cl O4 -'
_chemical_formula_moiety         'C11 H15 N2 O +, Cl O4 -'
_chemical_formula_sum            'C11 H15 Cl N2 O5'
_chemical_formula_weight         290.70
_chemical_name_common
;
Cytisinium perchlorate
;
_chemical_name_systematic
;
6-Oxo-7,11-diazatricyclo[7.3.1.0^2,7^]trideca-2,4-dien-11-ium perchlorate
;
_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'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   6.8719(3)
_cell_length_b                   18.8925(11)
_cell_length_c                   19.1239(14)
_cell_measurement_reflns_used    1639
_cell_measurement_temperature    100.0(10)
_cell_measurement_theta_max      28.6100
_cell_measurement_theta_min      3.3120
_cell_volume                     2482.8(3)
_computing_cell_refinement
;
(CrysAlis PRO; Agilent, 2013)
;
_computing_data_collection
;
(CrysAlis PRO; Agilent, 2013)
;
_computing_data_reduction
;
(CrysAlis PRO; Agilent, 2013)
;
_computing_molecular_graphics
;
Mercury (Macrae <i>et al.</i>,  2008)
;
_computing_publication_material
;
SHELXL2013 (Sheldrick, 2015b)
;
_computing_structure_refinement
;
SHELXL2013 (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 0.961
_diffrn_measured_fraction_theta_max 0.961
_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  0.0288
_diffrn_reflns_av_unetI/netI     0.0744
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -3
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            4496
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         24.990
_diffrn_reflns_theta_min         3.150
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.327
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.50628
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(CrysAlis PRO; Agilent, 2013)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.555
_exptl_crystal_description       prism
_exptl_crystal_F_000             1216
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.433
_refine_diff_density_min         -0.451
_refine_ls_abs_structure_details
;
Flack <i>x</i> determined using 865 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons & Flack, 2004)
;
_refine_ls_abs_structure_Flack   -0.04(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     343
_refine_ls_number_reflns         3618
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0680
_refine_ls_R_factor_gt           0.0506
_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^)+(0.0600P)^2^] where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1158
_refine_ls_wR_factor_ref         0.1258
_reflns_number_gt                2887
_reflns_number_total             3618
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            yf3149sup1.cif
_cod_data_source_block           3
_cod_database_code               2021282
_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  -8 175601. 1866.30   3
   0   0  -9 21.2405 133.076   3
   0   0 -10 150.596 154.307   3
   0   0 -11 54.6457 149.263   3
   0   0 -12 2944.88 341.508   3
   0   0 -13 63.3758 171.947   3
   0   0 -14 10548.6 647.674   3
   0   0 -15-102.918 235.007   3
   0   0 -16 33995.3 1201.89   3
   0   0 -17 169.593 265.866   3
   0   1  -8 2382.58 290.167   3
   0  -1  -8 813.329 159.378   3
   0  -1  -9 5103.23 325.277   3
   0   1  -9 6236.93 434.007   3
   0  -1 -10 12065.8 525.450   3
   0   1 -10 13290.0 646.958   3
   0  -1 -11 5369.37 373.772   3
   0   1 -11 11613.9 637.971   3
   0   1 -12 724.110 224.441   3
   0  -1 -12 433.425 179.889   3
   0  -1 -13 2163.17 284.918   3
   0   1 -13 2268.60 340.136   3
   0   1 -14 13877.4 773.822   3
   0  -1 -14 13249.0 675.088   3
   0  -1 -15 217.898 247.159   3
   0   1 -15 1473.04 313.943   3
   0  -1 -16 5162.19 477.388   3
   0   1 -16 9404.30 680.510   3
   0   1 -17-61.3331 326.158   3
   0  -2  -7 2091.19 151.852   3
   0  -2  -8 8823.82 320.007   3
   0   2  -8 21012.4 791.494   3
   0   2  -9 1377.71 272.638   3
   0  -2  -9 517.914 117.691   3
   0   2 -10 188.818 178.627   3
   0  -2 -10 67.3295 106.271   3
   0   2 -11 3499.95 388.863   3
   0  -2 -11 2426.71 232.382   3
   0  -2 -12-186.354 173.267   3
   0   2 -12 22.4103 183.424   3
   0  -2 -13 4985.70 355.468   3
   0   2 -13 10977.3 697.814   3
   0   2 -14 1782.57 333.272   3
   0  -2 -14 821.085 252.276   3
   0   2 -15 436.894 264.526   3
   0   2 -16 271.654 263.697   3
   0   2 -17 27067.8 1209.02   3
   0   2 -18-541.910 366.114   3
   0   3   0 219.047 117.994   3
   0   3   1 67078.6 915.666   3
   0   3   2 193926. 1350.12   3
   0   3  -8 40491.5 1170.25   3
   0   3  -9 21832.2 904.282   3
   0   3 -10 1030.81 256.373   3
   0   3 -11 977.251 263.503   3
   0   3 -12 6442.70 561.967   3
   0   3 -13 203.226 215.624   3
   0   3 -14 2656.23 408.329   3
   0   3 -15 17339.9 959.232   3
   0   3 -16 8041.71 683.754   3
   0   3 -17 1968.26 406.560   3
   0   3 -18-599.180 365.157   3
   0   3 -19 4687.26 539.930   3
   0   4   0 272428. 2331.60   3
   0   4   1 24731.3 683.063   3
   0   4   2 205490. 1786.64   3
   0   4   3 1184.48 135.214   3
   0   4  -7 44122.3 1257.80   3
   0   4  -8 127602. 2204.48   3
   0   4  -9 5341.66 512.637   3
   0   4 -10-22.6675 182.045   3
   0   4 -11 2600.42 395.554   3
   0   4 -12 1565.49 338.459   3
   0   4 -13 2226.33 374.290   3
   0   4 -14 21914.2 1086.75   3
   0   4 -15 1777.98 392.867   3
   0   4 -16 10423.9 807.876   3
   0   4 -17 10846.6 824.172   3
   0   4 -18 10959.7 853.950   3
   0   4 -19 64.6719 332.702   3
   0   5   0 337.949 232.817   3
   0   5  -1 1266.41 286.260   3
   0   5   1 1383.20 273.615   3
   0   5  -2 88032.4 1605.43   3
   0   5   2 90991.2 1400.48   3
   0   5   3 248372. 2065.00   3
   0   5   4 525.480 175.438   3
   0   5  -5 12189.2 682.899   3
   0   5  -6 719.449 250.633   3
   0   5  -7 11411.7 703.804   3
   0   5  -8 24071.2 1046.81   3
   0   5  -9 281.410 56.8963   1
   0   5  -9 504.253 258.657   3
   0   5 -10 569.408 79.0966   1
   0   5 -10 815.295 293.662   3
   0   5 -11 57222.6 1725.29   3
   0   5 -12 2317.51 415.089   3
   0   5 -13 7942.11 707.221   3
   0   5 -14 2535.23 441.558   3
   0   5 -15 1472.43 369.433   3
   0   5 -16 1470.52 385.866   3
   0   5 -17 539.547 317.203   3
   0   5 -18 3352.47 527.660   3
   0   5 -19 19749.6 1165.10   3
   0   5 -20-224.904 368.774   3
   0   6   0 126696. 2002.47   3
   0   6   1 16162.4 713.034   3
   0   6  -1 17836.1 786.029   3
   0   6   2 20478.1 775.262   3
   0   6  -2 21283.7 869.616   3
   0   6   3 23377.7 768.796   3
   0   6  -3 23662.0 944.872   3
   0   6  -4 287.414 229.176   3
   0   6   4-185.885 179.455   3
   0  -6   4 306.002 76.6412   1
   0   6  -5 7628.77 590.207   3
   0   6  -6 879.647 292.752   3
   0   6  -7 47577.0 1498.83   3
   0   6  -8 83633.5 2020.56   3
   0   6  -9 8561.41 693.908   3
   0   6 -10 4480.61 526.383   3
   0   6 -11 2298.94 447.265   3
   0   6 -12 2242.46 127.299   1
   0   6 -12 2415.14 139.710   1
   0   6 -13 253.310 295.940   3
   0   6 -13 64.1765 52.7599   1
   0   6 -13 111.454 56.2684   1
   0   6 -14 211.854 75.4367   1
   0   6 -14 298.753 282.367   3
   0   6 -15 6597.22 695.793   3
   0   6 -16 5121.99 642.933   3
   0   6 -17 776.993 345.044   3
   0   6 -18 8264.43 775.408   3
   0   6 -19 604.093 329.248   3
   0   6 -20 698.613 330.366   3
   0   7   0 262.273 228.818   3
   0   7   1 8581.51 579.783   3
   0   7  -1 8240.08 598.393   3
   0   7   2 2144.64 320.170   3
   0   7  -2 1868.77 348.758   3
   0   7   3 1256.91 266.071   3
   0   7  -3 1653.16 363.513   3
   0   7   4 128106. 1791.47   3
   0   7  -4 128013. 2402.00   3
   0   7  -5 7588.61 641.878   3
   0  -7   5 2243.49 103.991   1
   0   7  -6 39932.9 1404.60   3
   0   7  -7 14174.6 893.973   3
   0   7  -8 565.198 322.006   3
   0   7  -9 16622.1 1000.55   3
   0   7 -10 134.222 242.833   3
   0   7 -11 48.8573 264.298   3
   0   7 -12 14717.9 997.092   3
   0   7 -13 66.3853 261.686   3
   0   7 -14 559.370 347.114   3
   0   7 -15 8846.40 843.192   3
   0   7 -16 31162.6 1510.95   3
   0   7 -17 2404.63 479.336   3
   0   7 -18 1908.75 451.421   3
   0   7 -19 2769.50 506.560   3
   0   7 -20-538.514 438.278   3
   0   8   0 37825.3 1310.69   3
   0   8  -1 2446.34 394.779   3
   0   8   1 2727.93 395.938   3
   0   8   2 166.057 222.609   3
   0   8  -2 108.060 239.030   3
   0   8   3 12308.5 693.376   3
   0   8  -3 12037.7 808.348   3
   0   8  -4 81808.1 2046.53   3
   0   8   4 83549.0 1638.47   3
   0   8  -5 4660.69 563.542   3
   0  -8   5 4055.60 229.092   1
   0   8  -6 17892.1 1011.75   3
   0   8  -7 27226.5 1284.51   3
   0   8  -8 25051.2 1228.52   3
   0   8  -9 32315.0 1428.60   3
   0   8 -10 6208.24 683.298   3
   0   8 -11 696.224 333.128   3
   0   8 -12 11019.6 937.042   3
   0   8 -13 9315.56 877.274   3
   0   8 -14 17915.0 1193.77   3
   0   8 -15 21301.9 1298.69   3
   0   8 -16 7802.69 826.263   3
   0   8 -17 918.320 389.482   3
   0   8 -18 5348.48 694.674   3
   0   8 -19-161.322 361.213   3
   0   8 -20-855.758 463.187   3
   0   8 -21-305.877 413.890   3
   0   9   0 340.424 268.557   3
   0   9  -1 19655.3 1016.27   3
   0   9   1 20646.8 1025.51   3
   0   9  -2 52022.7 1647.74   3
   0   9   2 54323.9 1566.69   3
   0   9  -3 1232.13 370.466   3
   0   9   3 1013.96 292.256   3
   0   9  -4 1599.73 397.599   3
   0   9   4 1224.01 249.016   3
   0   9  -5 68054.3 2014.53   3
   0   9   5 66616.8 1484.78   3
   0  -9   5 72698.4 1048.37   1
   0   9  -6 20198.0 1137.81   3
   0  -9   6 17790.7 444.898   1
   0   9  -7 305.210 300.721   3
   0   9  -8 1450.33 419.076   3
   0   9  -9 4427.19 612.873   3
   0   9 -10 2204.53 502.462   3
   0   9 -11 34007.9 1602.37   3
   0   9 -12 460.108 321.302   3
   0   9 -13 10037.9 942.432   3
   0   9 -14 5346.03 744.519   3
   0   9 -15 22872.5 1395.79   3
   0   9 -16 3315.37 603.509   3
   0   9 -17 8421.12 859.982   3
   0   9 -18 1616.60 446.936   3
   0   9 -19 3866.06 607.496   3
   0   9 -20-25.3805 446.863   3
   0   9 -21 55.2691 386.324   3
   0  10   0 4410.44 549.344   3
   0  10   1 29456.6 1266.14   3
   0  10  -1 28406.4 1285.21   3
   0  10   2 131.927 259.121   3
   0  10  -2 348.311 316.285   3
   0  10   3 2569.56 415.250   3
   0  10  -3 2869.89 498.500   3
   0  10  -4 812.908 351.940   3
   0  10   4 218.240 249.053   3
   0 -10   5 2077.76 218.363   1
   0  10  -5 2102.88 463.086   3
   0  10  -6 27532.7 1375.70   3
   0 -10   6 25986.1 615.250   1
   0  10  -7 19542.1 1201.88   3
   0 -10   7 6219.99 197.847   1
   0  10  -8 42319.5 1731.47   3
   0  10  -9 1256.47 412.266   3
   0  10 -10 1498.70 428.261   3
   0  10 -11 5149.40 692.551   3
   0  10 -12 301.320 341.837   3
   0  10 -13 445.658 392.647   3
   0  10 -14 14621.0 1156.98   3
   0  10 -15 8584.54 917.229   3
   0  10 -16-75.5381 299.455   3
   0  10 -17 1569.11 444.431   3
   0  10 -18 83.4376 334.052   3
   0  10 -19-74.9423 381.175   3
   0  10 -20-886.734 496.569   3
   0  10 -21 2096.04 474.391   3
   0  10 -22 8138.95 924.188   3
   0  11   0 118.030 267.269   3
   0  11   1 960.027 364.716   3
   0  11  -1 1533.42 396.688   3
   0  11   2 35243.1 1438.06   3
   0  11  -2 31858.6 1476.50   3
   0  11   3 1869.27 397.832   3
   0  11  -3 2049.98 451.143   3
   0  11  -4 5561.07 676.143   3
   0  11   4 4070.48 474.016   3
   0  11  -5 3529.03 579.104   3
   0 -11   5 3921.95 302.486   1
   0 -11   6 3173.65 256.221   1
   0  11  -6 3069.30 562.232   3
   0 -11   7 18544.8 470.402   1
   0  11  -7 21600.2 1309.66   3
   0  11  -8 1276.28 421.427   3
   0  11  -9 5.86517 309.684   3
   0  11 -10 15157.2 1150.40   3
   0  11 -11 28579.9 1598.00   3
   0  11 -12 4178.20 672.366   3
   0  11 -13 3068.23 602.470   3
   0  11 -14 1574.13 486.934   3
   0  11 -15 6614.49 861.100   3
   0  11 -16 532.003 374.912   3
   0  11 -17 6667.67 836.060   3
   0  11 -18 555.454 334.501   3
   0  11 -19 473.038 346.556   3
   0  11 -20-545.077 476.459   3
   0  11 -21-26.5613 414.898   3
   0  11 -22 589.276 452.236   3
   0  12   0 7530.32 768.591   3
   0  12   1 2369.69 470.723   3
   0  12  -1 2350.48 508.177   3
   0  12  -2-7.72582 286.939   3
   0  12   2 156.896 293.978   3
   0  12   3 1093.05 341.052   3
   0  12  -3 1222.07 441.922   3
   0  12   4 26981.8 1233.43   3
   0  12  -4 27621.8 1487.94   3
   0  12  -5 7819.18 843.048   3
   0 -12   5 8321.91 472.193   1
   0  12  -6 3798.88 633.470   3
   0 -12   6 4067.32 313.989   1
   0 -12   7 2073.18 203.533   1
   0  12  -7 2381.89 562.951   3
   0  12  -8 23189.6 1438.01   3
   0  12  -9 958.008 431.270   3
   0  12 -10 4999.58 735.080   3
   0  12 -11 2177.00 562.847   3
   0  12 -12 864.843 409.943   3
   0  12 -13 920.208 435.173   3
   0  12 -14 529.273 386.890   3
   0  12 -15 1210.73 510.067   3
   0  12 -16 1609.37 542.821   3
   0  12 -17 106.308 354.591   3
   0  12 -18-94.4108 419.360   3
   0  12 -19-538.885 460.466   3
   0  12 -20-191.541 477.708   3
   0  12 -21-84.5868 439.200   3
   0  12 -22 2369.09 598.481   3
   0  13   0 257.929 359.585   3
   0  13   1 33727.6 1565.37   3
   0  13  -1 33147.6 1599.96   3
   0  13   2 501.166 385.452   3
   0  13  -2 85.5556 310.872   3
   0  13  -3 10545.1 971.039   3
   0  13   3 9569.81 831.440   3
   0  13   4 1031.16 329.187   3
   0  13  -4 3313.07 631.618   3
   0  13   5 2646.35 501.632   3
   0 -13   5 3887.81 368.501   1
   0  13  -5 4259.18 704.445   3
   0 -13   6 46506.6 1067.42   1
   0  13  -6 44031.4 1994.21   3
   0 -13   7 55618.5 1024.97   1
   0  13  -7 59196.3 2322.23   3
   0  13  -8 3314.17 689.152   3
   0 -13   8 1614.20 140.304   1
   0  13  -9 2541.41 606.103   3
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   0  13 -11 4227.12 726.912   3
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   4   3 -10 3800.01 500.923   1
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   7 -15   1 1676.03 650.866   1
   7 -15   2 2776.53 759.157   1
   7 -15   3 2026.91 654.400   1
   7 -15   4 2359.56 669.934   1
   7 -15   5 1302.91 621.636   1
   7 -15   6 334.080 462.307   1
   7 -15   7 196.864 419.867   1
   7 -16   5 1797.98 676.356   1
   8   0  -1-116.829 399.869   1
   8   0  -2 782.422 521.561   1
   8   0  -3 597.639 458.608   1
   8   0  -4 2032.69 670.120   1
   8   0  -5 950.152 563.538   1
   8   0  -6 888.360 558.601   1
   8   0  -7 752.979 441.867   1
   8   0  -8 428.267 426.668   1
   8   0  -9 211.920 384.358   1
   8   0 -10 1874.31 659.557   1
   8   0 -11 1253.13 606.320   1
   8   0 -12 1054.72 587.676   1
   8   0 -13 5475.32 944.388   1
   8  -1   0 562.771 484.598   1
   8  -1  -1 247.192 430.001   1
   8   1  -2 1007.58 537.016   1
   8  -1  -2 1442.42 598.043   1
   8   1  -3 1217.34 539.423   1
   8  -1  -3 1215.97 583.427   1
   8   1  -4 274.269 437.683   1
   8  -1  -4 1145.36 550.516   1
   8   1  -5 5464.02 923.799   1
   8  -1  -5 5892.46 956.255   1
   8   1  -6 2865.20 722.803   1
   8  -1  -6 880.822 487.877   1
   8   1  -7 369.012 439.218   1
   8  -1  -7 118.063 387.004   1
   8   1  -8 729.501 483.300   1
   8  -1  -8 497.569 462.304   1
   8   1  -9 695.418 463.657   1
   8  -1  -9 793.638 514.461   1
   8   1 -10 1345.58 560.072   1
   8  -1 -10 2142.96 702.268   1
   8   1 -11 10874.1 1247.30   1
   8  -1 -11 11693.9 1318.47   1
   8   1 -12 814.531 526.519   1
   8  -1 -12 705.881 561.874   1
   8   1 -13 592.436 487.417   1
   8  -2   0 1196.90 533.352   1
   8  -2   1 194.722 433.125   1
   8  -2  -1 1417.06 607.204   1
   8  -2  -2 253.242 434.298   1
   8  -2  -3 2014.21 653.342   1
   8   2  -4 1162.60 579.828   1
   8  -2  -4 1789.09 615.757   1
   8   2  -5 6209.81 953.268   1
   8  -2  -5 6196.93 1006.56   1
   8   2  -6 1358.40 581.905   1
   8  -2  -6 2617.95 718.726   1
   8   2  -7 797.598 488.542   1
   8  -2  -7 411.442 466.304   1
   8   2  -8 945.176 530.949   1
   8  -2  -8 82.3387 422.674   1
   8   2  -9 453.780 456.825   1
   8  -2  -9 71.0848 421.106   1
   8   2 -10 2435.44 733.495   1
   8  -2 -10 571.470 525.449   1
   8   2 -11 2078.41 630.335   1
   8  -2 -11 1803.40 621.032   1
   8   2 -12 1024.21 516.998   1
   8  -3   0 583.383 494.808   1
   8  -3   1 1881.75 665.282   1
   8  -3  -1 490.801 470.583   1
   8  -3   2 1633.49 593.898   1
   8  -3  -2 2769.39 695.032   1
   8  -3  -3 1353.88 592.546   1
   8  -3  -4 2667.86 753.619   1
   8  -3  -5 4734.14 927.042   1
   8   3  -6 1407.23 675.725   1
   8  -3  -6 1101.14 577.784   1
   8   3  -7 3107.59 728.630   1
   8  -3  -7 4752.21 941.408   1
   8   3  -8 1103.92 515.544   1
   8  -3  -8 1465.61 614.176   1
   8   3  -9 2360.53 662.813   1
   8  -3  -9 1292.95 580.970   1
   8   3 -10 461.716 446.409   1
   8  -3 -10 955.974 525.886   1
   8   3 -11 600.466 444.471   1
   8  -4   0 6621.26 1057.81   1
   8  -4   1 2099.96 727.743   1
   8  -4  -1 1374.67 582.456   1
   8  -4   2 872.904 550.822   1
   8  -4  -2 1368.37 620.116   1
   8  -4   3-11.0036 403.803   1
   8  -4  -3 707.333 514.721   1
   8  -4  -4 2602.07 742.095   1
   8  -4  -5 10289.1 1296.86   1
   8  -4  -6 3354.44 837.177   1
   8  -4  -7 551.800 532.258   1
   8  -4  -8 7504.53 1108.27   1
   8   4  -9 630.127 488.309   1
   8  -4  -9 517.749 479.743   1
   8   4 -10 1054.06 530.198   1
   8   4 -11 1388.03 572.456   1
   8  -5   0 5099.77 925.672   1
   8  -5   1 339.790 501.786   1
   8  -5  -1 515.435 493.147   1
   8  -5   2 229.778 451.077   1
   8  -5  -2 713.587 511.610   1
   8  -5   3 4598.81 902.421   1
   8  -5  -3 5225.62 972.269   1
   8  -5   4 1925.19 761.623   1
   8  -5  -4 2310.41 736.727   1
   8  -5  -5 6004.08 1045.88   1
   8  -5  -6 3074.47 808.789   1
   8  -5  -7 2104.92 667.548   1
   8  -5  -8 3069.32 769.030   1
   8  -6   0 1840.76 650.390   1
   8  -6   1 1826.29 652.811   1
   8  -6  -1 2652.41 751.877   1
   8  -6   2 1086.07 595.572   1
   8  -6  -2 188.057 426.657   1
   8  -6   3 36.0914 410.099   1
   8  -6  -3 561.657 529.942   1
   8  -6   4 860.784 553.814   1
   8  -6  -4 1484.97 640.343   1
   8  -6  -5 1474.23 630.291   1
   8  -6  -6 1969.48 677.240   1
   8  -7   0 1615.39 626.996   1
   8  -7   1 2821.09 740.914   1
   8  -7  -1 3477.28 849.346   1
   8  -7   2 759.576 542.395   1
   8  -7  -2 777.294 578.155   1
   8  -7   3 1351.89 621.606   1
   8  -7  -3 1026.14 585.590   1
   8  -7   4 242.889 466.674   1
   8  -7  -4 639.027 526.421   1
   8  -7   5 2051.11 667.557   1
   8  -7  -5 2056.96 706.901   1
   8  -8   0 578.818 519.750   1
   8  -8   1 634.909 514.040   1
   8  -8  -1 987.228 606.675   1
   8  -8   2 321.035 442.877   1
   8  -8  -2 629.776 578.720   1
   8  -8   3 838.722 540.620   1
   8  -8  -3 897.734 585.921   1
   8  -8   4 314.047 489.683   1
   8  -8   5 5564.79 977.571   1
   8  -8   6 1663.03 634.938   1
   8  -9   0 564.789 534.873   1
   8  -9   1 811.554 604.443   1
   8  -9   2 2942.83 767.918   1
   8  -9   3 891.938 514.137   1
   8  -9   4 1125.17 593.098   1
   8  -9   5 1188.52 611.164   1
   0   0   0    0.00    0.00   0
;
_shelx_hkl_checksum              15808
_shelx_res_file
;
TITL    ap94_hclo4 in P2(1)2(1)2(1)
CELL   0.71073      6.8719  18.8925  19.1239  90.000   90.000   90.000
ZERR         8      0.0003   0.0011   0.0014   0.00     0.00     0.00
LATT -1
SYMM  0.50000-X,-Y, 0.50000+Z
SYMM  0.50000+X, 0.50000-Y,-Z
SYMM -X, 0.50000+Y, 0.50000-Z
SFAC    C   H   N   O   CL
UNIT    88 120  16  40   8
omit 0 50
omit 0 2 7
L.S.    4
FMAP    2
bond $h
acta 50
PLAN   -10
temp -173
conf
HTAB C7A O23
EQIV $1 x+1, y, z
HTAB N12A O22_$1
HTAB N12A O2B
EQIV $2 -x+2, y-1/2, -z+1/2
HTAB C3B O14_$2
EQIV $3 -x+3/2, -y, z-1/2
HTAB C7B O24_$3
HTAB C11B O13
HTAB N12B O2A
EQIV $4 x-1/2, -y+1/2, -z
HTAB N12B O13_$4
HTAB N12B O14_$4
EQIV $5 -x+1/2, -y, z-1/2
HTAB C13B O21_$5
HTAB C13B O23_$5
WGHT    0.060000
FVAR       3.12126
N1A   3    0.471961    0.135429    0.228184    11.00000    0.01696    0.01810 =
         0.02497    0.00055   -0.00159   -0.00208
C2A   1    0.494420    0.090449    0.170854    11.00000    0.01619    0.02370 =
         0.02470   -0.00472   -0.00130    0.00329
O2A   4    0.548926    0.117059    0.114772    11.00000    0.02363    0.03049 =
         0.02743    0.00024    0.00060    0.00262
C3A   1    0.448845    0.017900    0.181701    11.00000    0.01797    0.01872 =
         0.03555   -0.00466   -0.00737    0.00103
AFIX  43
H3A   2    0.462179   -0.014746    0.144222    11.00000   -1.20000
AFIX   0
C4A   1    0.386832   -0.005100    0.244674    11.00000    0.01465    0.01688 =
         0.06037    0.01105   -0.00533    0.00071
AFIX  43
H4A   2    0.357387   -0.053814    0.250981    11.00000   -1.20000
AFIX   0
C5A   1    0.365101    0.042051    0.301211    11.00000    0.01828    0.02374 =
         0.03775    0.00724    0.00087   -0.00472
AFIX  43
H5A   2    0.320231    0.025425    0.345234    11.00000   -1.20000
AFIX   0
C6A   1    0.409194    0.111840    0.292051    11.00000    0.01119    0.02236 =
         0.03248   -0.00082   -0.00200   -0.00119
C7A   1    0.391242    0.164194    0.350870    11.00000    0.02304    0.02440 =
         0.02481   -0.00417    0.00607   -0.00506
AFIX  13
H7A   2    0.286100    0.147238    0.382906    11.00000   -1.20000
AFIX   0
C8A   1    0.331918    0.236808    0.323266    11.00000    0.02448    0.02478 =
         0.03504   -0.00358    0.00464    0.00017
AFIX  23
H8A1  2    0.315134    0.270597    0.362373    11.00000   -1.20000
H8A2  2    0.207801    0.233600    0.297176    11.00000   -1.20000
AFIX   0
C9A   1    0.496252    0.261057    0.274904    11.00000    0.02321    0.01538 =
         0.03310    0.00785    0.00024    0.00026
AFIX  13
H9A   2    0.461061    0.309125    0.257029    11.00000   -1.20000
AFIX   0
C10A  1    0.510356    0.211552    0.211694    11.00000    0.02225    0.01372 =
         0.02737    0.00429   -0.00024   -0.00205
AFIX  23
H10A  2    0.415978    0.227375    0.175842    11.00000   -1.20000
H10B  2    0.642256    0.215703    0.191283    11.00000   -1.20000
AFIX   0
C11A  1    0.686503    0.268353    0.315987    11.00000    0.02835    0.02029 =
         0.02561   -0.00695    0.00213   -0.00404
AFIX  23
H11A  2    0.792252    0.282391    0.283682    11.00000   -1.20000
H11B  2    0.672007    0.306146    0.351466    11.00000   -1.20000
AFIX   0
N12A  3    0.741077    0.199908    0.351897    11.00000    0.01901    0.02356 =
         0.02853   -0.00160   -0.00236   -0.00072
AFIX  23
H12A  2    0.782896    0.165129    0.316209    11.00000   -1.20000
H12B  2    0.852712    0.208647    0.383459    11.00000   -1.20000
AFIX   0
C13A  1    0.578126    0.169450    0.392975    11.00000    0.02679    0.02455 =
         0.03138    0.00366    0.00168   -0.00476
AFIX  23
H13A  2    0.554797    0.199348    0.434656    11.00000   -1.20000
H13B  2    0.615328    0.121645    0.409432    11.00000   -1.20000
AFIX   0
N1B   3    0.978635    0.071736    0.145255    11.00000    0.01916    0.01060 =
         0.02667    0.00427   -0.00081    0.00041
C2B   1    0.937757    0.075030    0.215811    11.00000    0.01228    0.02522 =
         0.02639   -0.00249   -0.00092    0.00331
O2B   4    0.933576    0.134978    0.244732    11.00000    0.02281    0.02140 =
         0.02796   -0.00391    0.00131   -0.00101
C3B   1    0.901181    0.010384    0.249732    11.00000    0.01527    0.02564 =
         0.03712    0.00835    0.00195    0.00031
AFIX  43
H3B   2    0.874612    0.010185    0.298482    11.00000   -1.20000
AFIX   0
C4B   1    0.903114   -0.051703    0.214165    11.00000    0.01543    0.02143 =
         0.04898    0.01477   -0.00454   -0.00547
AFIX  43
H4B   2    0.877422   -0.094714    0.238188    11.00000   -1.20000
AFIX   0
C5B   1    0.942210   -0.052977    0.143128    11.00000    0.02158    0.01566 =
         0.03200   -0.00308   -0.00893   -0.00355
AFIX  43
H5B   2    0.940709   -0.096652    0.118515    11.00000   -1.20000
AFIX   0
C6B   1    0.983066    0.008651    0.108263    11.00000    0.01283    0.01734 =
         0.03434    0.00327   -0.00121    0.00097
C7B   1    1.025167    0.009930    0.032793    11.00000    0.02508    0.00996 =
         0.03181   -0.00067   -0.00500    0.00377
AFIX  13
H7B   2    1.089473   -0.035906    0.020546    11.00000   -1.20000
AFIX   0
C8B   1    1.167454    0.069757    0.014356    11.00000    0.01367    0.02905 =
         0.03469   -0.00022    0.00349    0.00278
AFIX  23
H8B1  2    1.290069    0.064543    0.041041    11.00000   -1.20000
H8B2  2    1.198239    0.069044   -0.036211    11.00000   -1.20000
AFIX   0
C9B   1    1.064580    0.138984    0.034083    11.00000    0.02079    0.01168 =
         0.03523    0.00484    0.00224   -0.00338
AFIX  13
H9B   2    1.154894    0.178851    0.022681    11.00000   -1.20000
AFIX   0
C10B  1    1.026447    0.141068    0.111999    11.00000    0.01864    0.01234 =
         0.03021   -0.00074   -0.00402   -0.00502
AFIX  23
H10C  2    1.143048    0.160719    0.135398    11.00000   -1.20000
H10D  2    0.917378    0.174128    0.120787    11.00000   -1.20000
AFIX   0
C11B  1    0.883569    0.147925   -0.010465    11.00000    0.02797    0.00961 =
         0.03089    0.00414    0.00062   -0.00087
AFIX  23
H11C  2    0.816619    0.192341    0.002794    11.00000   -1.20000
H11D  2    0.921605    0.151644   -0.060260    11.00000   -1.20000
AFIX   0
N12B  3    0.746718    0.086817   -0.001394    11.00000    0.01935    0.01848 =
         0.01797   -0.00284   -0.00179    0.00361
AFIX  23
H12C  2    0.692304    0.088028    0.046524    11.00000   -1.20000
H12D  2    0.637281    0.091981   -0.034673    11.00000   -1.20000
AFIX   0
C13B  1    0.842588    0.016999   -0.013100    11.00000    0.02133    0.01724 =
         0.03528   -0.00256   -0.00373   -0.00104
AFIX  23
H13C  2    0.879307    0.012430   -0.062954    11.00000   -1.20000
H13D  2    0.750217   -0.021538   -0.001748    11.00000   -1.20000
AFIX   0
CL1   5    0.935014    0.339233    0.132144    11.00000    0.02591    0.01526 =
         0.02781    0.00083    0.00239   -0.00235
O11   4    0.736471    0.346774    0.153731    11.00000    0.02531    0.03624 =
         0.05680    0.00930    0.01153   -0.00124
O12   4    1.043318    0.301658    0.184151    11.00000    0.04153    0.02074 =
         0.03516    0.00455   -0.00791    0.00379
O13   4    0.944482    0.303010    0.066035    11.00000    0.04160    0.02028 =
         0.02156   -0.00509   -0.00389   -0.00415
O14   4    1.016479    0.409270    0.122666    11.00000    0.03515    0.01313 =
         0.03339    0.00001    0.00321   -0.00910
CL2   5    0.047958    0.140184    0.500959    11.00000    0.02367    0.01984 =
         0.02876   -0.00203    0.00281   -0.00224
O21   4   -0.074621    0.122760    0.558027    11.00000    0.05433    0.04191 =
         0.04217   -0.00885    0.02473   -0.02114
O22   4   -0.010707    0.206917    0.471289    11.00000    0.05228    0.02904 =
         0.04653    0.00294   -0.02028    0.01306
O23   4    0.034348    0.086257    0.448203    11.00000    0.05103    0.03429 =
         0.04655   -0.01898    0.01562   -0.02060
O24   4    0.245232    0.147530    0.524488    11.00000    0.02529    0.03225 =
         0.06030    0.00000   -0.00592    0.00293
HKLF 4
REM     ap94_hclo4 in P2(1)2(1)2(1)
REM R1 =  0.0506 for    2887 Fo > 4sig(Fo)  and  0.0680 for all    3618 data
REM    343 parameters refined using      0 restraints
END
WGHT      0.0608      0.0000
REM Highest difference peak  0.433,  deepest hole -0.451,  1-sigma level  0.075
Q1    1  -0.1371  0.1375  0.5034  11.00000  0.05    0.43
Q2    1   0.5362  0.2159  0.1625  11.00000  0.05    0.34
Q3    1   0.1601  0.1826  0.5315  11.00000  0.05    0.32
Q4    1   1.1497  0.3362  0.2011  11.00000  0.05    0.30
Q5    1   0.0940  0.1390  0.4423  11.00000  0.05    0.29
Q6    1   0.9921  0.4184  0.1814  11.00000  0.05    0.28
Q7    1   0.9847  0.3157  0.0177  11.00000  0.05    0.26
Q8    1   0.2223  0.1414  0.5023  11.00000  0.05    0.26
Q9    1  -0.0554  0.1348  0.4398  11.00000  0.05    0.25
Q10   1  -0.0123  0.3047  0.4407  11.00000  0.05    0.25
;
_shelx_res_checksum              61765
_shelxl_version_number           20.13
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z'
'-x, y+1/2, -z+1/2'
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 N1A 0.4720(7) 0.1354(3) 0.2282(2) 0.0200(11) Uani d 1
C C2A 0.4944(8) 0.0904(3) 0.1709(3) 0.0215(15) Uani d 1
O O2A 0.5489(7) 0.1171(2) 0.1148(2) 0.0272(10) Uani d 1
C C3A 0.4488(9) 0.0179(3) 0.1817(4) 0.0241(14) Uani d 1
H H3A 0.4622 -0.0147 0.1442 0.029 Uiso calc 1
C C4A 0.3868(9) -0.0051(3) 0.2447(4) 0.0306(18) Uani d 1
H H4A 0.3574 -0.0538 0.2510 0.037 Uiso calc 1
C C5A 0.3651(9) 0.0421(3) 0.3012(4) 0.0266(16) Uani d 1
H H5A 0.3202 0.0254 0.3452 0.032 Uiso calc 1
C C6A 0.4092(8) 0.1118(3) 0.2921(3) 0.0220(15) Uani d 1
C C7A 0.3912(9) 0.1642(3) 0.3509(3) 0.0241(15) Uani d 1
H H7A 0.2861 0.1472 0.3829 0.029 Uiso calc 1
C C8A 0.3319(10) 0.2368(3) 0.3233(4) 0.0281(16) Uani d 1
H H8A1 0.3151 0.2706 0.3624 0.034 Uiso calc 1
H H8A2 0.2078 0.2336 0.2972 0.034 Uiso calc 1
C C9A 0.4963(8) 0.2611(3) 0.2749(3) 0.0239(15) Uani d 1
H H9A 0.4611 0.3091 0.2570 0.029 Uiso calc 1
C C10A 0.5104(9) 0.2116(3) 0.2117(3) 0.0211(14) Uani d 1
H H10A 0.4160 0.2274 0.1758 0.025 Uiso calc 1
H H10B 0.6423 0.2157 0.1913 0.025 Uiso calc 1
C C11A 0.6865(9) 0.2684(3) 0.3160(3) 0.0247(15) Uani d 1
H H11A 0.7923 0.2824 0.2837 0.030 Uiso calc 1
H H11B 0.6720 0.3061 0.3515 0.030 Uiso calc 1
N N12A 0.7411(7) 0.1999(3) 0.3519(3) 0.0237(13) Uani d 1
H H12A 0.7829 0.1651 0.3162 0.028 Uiso calc 1
H H12B 0.8527 0.2086 0.3835 0.028 Uiso calc 1
C C13A 0.5781(9) 0.1695(3) 0.3930(3) 0.0276(15) Uani d 1
H H13A 0.5548 0.1993 0.4347 0.033 Uiso calc 1
H H13B 0.6153 0.1216 0.4094 0.033 Uiso calc 1
N N1B 0.9786(7) 0.0717(2) 0.1453(3) 0.0188(12) Uani d 1
C C2B 0.9378(9) 0.0750(3) 0.2158(3) 0.0213(14) Uani d 1
O O2B 0.9336(6) 0.1350(2) 0.2447(2) 0.0241(10) Uani d 1
C C3B 0.9012(9) 0.0104(3) 0.2497(4) 0.0260(16) Uani d 1
H H3B 0.8746 0.0102 0.2985 0.031 Uiso calc 1
C C4B 0.9031(8) -0.0517(3) 0.2142(4) 0.0286(16) Uani d 1
H H4B 0.8774 -0.0947 0.2382 0.034 Uiso calc 1
C C5B 0.9422(9) -0.0530(3) 0.1431(3) 0.0231(14) Uani d 1
H H5B 0.9407 -0.0967 0.1185 0.028 Uiso calc 1
C C6B 0.9831(8) 0.0087(3) 0.1083(3) 0.0215(14) Uani d 1
C C7B 1.0252(9) 0.0099(3) 0.0328(3) 0.0223(15) Uani d 1
H H7B 1.0895 -0.0359 0.0205 0.027 Uiso calc 1
C C8B 1.1675(8) 0.0698(3) 0.0144(4) 0.0258(16) Uani d 1
H H8B1 1.2901 0.0645 0.0410 0.031 Uiso calc 1
H H8B2 1.1982 0.0690 -0.0362 0.031 Uiso calc 1
C C9B 1.0646(9) 0.1390(3) 0.0341(3) 0.0226(14) Uani d 1
H H9B 1.1549 0.1789 0.0227 0.027 Uiso calc 1
C C10B 1.0264(8) 0.1411(3) 0.1120(3) 0.0204(14) Uani d 1
H H10C 1.1430 0.1607 0.1354 0.024 Uiso calc 1
H H10D 0.9174 0.1741 0.1208 0.024 Uiso calc 1
C C11B 0.8836(8) 0.1479(3) -0.0105(3) 0.0228(14) Uani d 1
H H11C 0.8166 0.1923 0.0028 0.027 Uiso calc 1
H H11D 0.9216 0.1516 -0.0603 0.027 Uiso calc 1
N N12B 0.7467(7) 0.0868(2) -0.0014(3) 0.0186(11) Uani d 1
H H12C 0.6923 0.0880 0.0465 0.022 Uiso calc 1
H H12D 0.6373 0.0920 -0.0347 0.022 Uiso calc 1
C C13B 0.8426(9) 0.0170(3) -0.0131(4) 0.0246(15) Uani d 1
H H13C 0.8793 0.0124 -0.0630 0.030 Uiso calc 1
H H13D 0.7502 -0.0215 -0.0017 0.030 Uiso calc 1
Cl Cl1 0.9350(2) 0.33923(7) 0.13214(8) 0.0230(4) Uani d 1
O O11 0.7365(6) 0.3468(2) 0.1537(2) 0.0394(12) Uani d 1
O O12 1.0433(7) 0.3017(2) 0.1842(2) 0.0325(11) Uani d 1
O O13 0.9445(7) 0.3030(2) 0.0660(2) 0.0278(11) Uani d 1
O O14 1.0165(6) 0.4093(2) 0.1227(2) 0.0272(11) Uani d 1
Cl Cl2 0.0480(2) 0.14018(7) 0.50096(8) 0.0241(4) Uani d 1
O O21 -0.0746(8) 0.1228(3) 0.5580(3) 0.0461(14) Uani d 1
O O22 -0.0107(7) 0.2069(2) 0.4713(3) 0.0426(14) Uani d 1
O O23 0.0343(8) 0.0863(2) 0.4482(3) 0.0440(14) Uani d 1
O O24 0.2452(6) 0.1475(2) 0.5245(3) 0.0393(13) 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
N1A 0.017(3) 0.018(3) 0.025(3) -0.002(2) -0.002(2) 0.001(2)
C2A 0.016(4) 0.024(3) 0.025(4) 0.003(3) -0.001(3) -0.005(3)
O2A 0.024(2) 0.030(2) 0.027(3) 0.003(2) 0.001(2) 0.000(2)
C3A 0.018(3) 0.019(3) 0.036(4) 0.001(3) -0.007(3) -0.005(3)
C4A 0.015(4) 0.017(3) 0.060(5) 0.001(3) -0.005(3) 0.011(4)
C5A 0.018(3) 0.024(3) 0.038(4) -0.005(3) 0.001(3) 0.007(3)
C6A 0.011(3) 0.022(3) 0.032(4) -0.001(3) -0.002(3) -0.001(3)
C7A 0.023(4) 0.024(3) 0.025(4) -0.005(3) 0.006(3) -0.004(3)
C8A 0.024(4) 0.025(3) 0.035(4) 0.000(3) 0.005(3) -0.004(3)
C9A 0.023(4) 0.015(3) 0.033(4) 0.000(3) 0.000(3) 0.008(3)
C10A 0.022(4) 0.014(3) 0.027(3) -0.002(3) 0.000(3) 0.004(3)
C11A 0.028(4) 0.020(3) 0.026(4) -0.004(3) 0.002(3) -0.007(3)
N12A 0.019(3) 0.024(3) 0.029(3) -0.001(2) -0.002(2) -0.002(2)
C13A 0.027(4) 0.025(3) 0.031(4) -0.005(3) 0.002(3) 0.004(3)
N1B 0.019(3) 0.011(2) 0.027(3) 0.000(2) -0.001(2) 0.004(2)
C2B 0.012(3) 0.025(3) 0.026(4) 0.003(3) -0.001(3) -0.002(3)
O2B 0.023(2) 0.021(2) 0.028(2) -0.001(2) 0.0013(19) -0.004(2)
C3B 0.015(4) 0.026(3) 0.037(4) 0.000(3) 0.002(3) 0.008(3)
C4B 0.015(3) 0.021(3) 0.049(5) -0.005(3) -0.005(3) 0.015(3)
C5B 0.022(3) 0.016(3) 0.032(4) -0.004(3) -0.009(3) -0.003(3)
C6B 0.013(3) 0.017(3) 0.034(4) 0.001(3) -0.001(3) 0.003(3)
C7B 0.025(4) 0.010(3) 0.032(4) 0.004(3) -0.005(3) -0.001(3)
C8B 0.014(3) 0.029(3) 0.035(4) 0.003(3) 0.003(3) 0.000(3)
C9B 0.021(3) 0.012(3) 0.035(4) -0.003(3) 0.002(3) 0.005(3)
C10B 0.019(3) 0.012(3) 0.030(3) -0.005(3) -0.004(3) -0.001(3)
C11B 0.028(3) 0.010(3) 0.031(4) -0.001(3) 0.001(3) 0.004(3)
N12B 0.019(3) 0.018(2) 0.018(3) 0.004(2) -0.002(2) -0.003(2)
C13B 0.021(3) 0.017(3) 0.035(4) -0.001(3) -0.004(3) -0.003(3)
Cl1 0.0259(8) 0.0153(7) 0.0278(8) -0.0024(7) 0.0024(7) 0.0008(7)
O11 0.025(3) 0.036(3) 0.057(3) -0.001(2) 0.012(2) 0.009(3)
O12 0.042(3) 0.021(2) 0.035(3) 0.004(2) -0.008(2) 0.005(2)
O13 0.042(3) 0.020(2) 0.022(2) -0.004(2) -0.004(2) -0.0051(19)
O14 0.035(3) 0.013(2) 0.033(3) -0.0091(19) 0.003(2) 0.0000(19)
Cl2 0.0237(8) 0.0198(7) 0.0288(8) -0.0022(7) 0.0028(7) -0.0020(7)
O21 0.054(4) 0.042(3) 0.042(3) -0.021(3) 0.025(3) -0.009(2)
O22 0.052(4) 0.029(3) 0.047(3) 0.013(2) -0.020(3) 0.003(2)
O23 0.051(3) 0.034(3) 0.047(3) -0.021(3) 0.016(3) -0.019(2)
O24 0.025(3) 0.032(3) 0.060(4) 0.003(2) -0.006(2) 0.000(3)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 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
C6A N1A C2A 122.5(5)
C6A N1A C10A 123.8(5)
C2A N1A C10A 113.6(5)
O2A C2A N1A 117.7(5)
O2A C2A C3A 125.6(6)
N1A C2A C3A 116.6(6)
C4A C3A C2A 120.7(6)
C4A C3A H3A 119.7
C2A C3A H3A 119.7
C3A C4A C5A 121.0(6)
C3A C4A H4A 119.5
C5A C4A H4A 119.5
C6A C5A C4A 119.3(6)
C6A C5A H5A 120.4
C4A C5A H5A 120.4
C5A C6A N1A 119.9(6)
C5A C6A C7A 121.4(6)
N1A C6A C7A 118.6(5)
C6A C7A C13A 111.7(5)
C6A C7A C8A 110.8(5)
C13A C7A C8A 110.5(5)
C6A C7A H7A 107.9
C13A C7A H7A 107.9
C8A C7A H7A 107.9
C7A C8A C9A 106.3(5)
C7A C8A H8A1 110.5
C9A C8A H8A1 110.5
C7A C8A H8A2 110.5
C9A C8A H8A2 110.5
H8A1 C8A H8A2 108.7
C8A C9A C10A 109.9(5)
C8A C9A C11A 110.3(5)
C10A C9A C11A 113.9(5)
C8A C9A H9A 107.5
C10A C9A H9A 107.5
C11A C9A H9A 107.5
N1A C10A C9A 114.2(5)
N1A C10A H10A 108.7
C9A C10A H10A 108.7
N1A C10A H10B 108.7
C9A C10A H10B 108.7
H10A C10A H10B 107.6
N12A C11A C9A 111.6(5)
N12A C11A H11A 109.3
C9A C11A H11A 109.3
N12A C11A H11B 109.3
C9A C11A H11B 109.3
H11A C11A H11B 108.0
C13A N12A C11A 112.6(5)
C13A N12A H12A 109.1
C11A N12A H12A 109.1
C13A N12A H12B 109.1
C11A N12A H12B 109.1
H12A N12A H12B 107.8
N12A C13A C7A 112.5(5)
N12A C13A H13A 109.1
C7A C13A H13A 109.1
N12A C13A H13B 109.1
C7A C13A H13B 109.1
H13A C13A H13B 107.8
C2B N1B C6B 122.8(5)
C2B N1B C10B 115.0(5)
C6B N1B C10B 122.2(5)
O2B C2B N1B 118.3(5)
O2B C2B C3B 125.0(6)
N1B C2B C3B 116.7(5)
C4B C3B C2B 121.2(6)
C4B C3B H3B 119.4
C2B C3B H3B 119.4
C3B C4B C5B 120.6(6)
C3B C4B H4B 119.7
C5B C4B H4B 119.7
C6B C5B C4B 120.1(6)
C6B C5B H5B 119.9
C4B C5B H5B 119.9
C5B C6B N1B 118.5(6)
C5B C6B C7B 122.1(5)
N1B C6B C7B 119.4(5)
C6B C7B C8B 111.2(5)
C6B C7B C13B 113.6(5)
C8B C7B C13B 108.9(5)
C6B C7B H7B 107.6
C8B C7B H7B 107.6
C13B C7B H7B 107.6
C9B C8B C7B 106.1(5)
C9B C8B H8B1 110.5
C7B C8B H8B1 110.5
C9B C8B H8B2 110.5
C7B C8B H8B2 110.5
H8B1 C8B H8B2 108.7
C10B C9B C11B 114.1(5)
C10B C9B C8B 110.1(5)
C11B C9B C8B 109.6(5)
C10B C9B H9B 107.6
C11B C9B H9B 107.6
C8B C9B H9B 107.6
N1B C10B C9B 115.8(5)
N1B C10B H10C 108.3
C9B C10B H10C 108.3
N1B C10B H10D 108.3
C9B C10B H10D 108.3
H10C C10B H10D 107.4
N12B C11B C9B 111.3(5)
N12B C11B H11C 109.4
C9B C11B H11C 109.4
N12B C11B H11D 109.4
C9B C11B H11D 109.4
H11C C11B H11D 108.0
C13B N12B C11B 112.7(4)
C13B N12B H12C 109.0
C11B N12B H12C 109.0
C13B N12B H12D 109.0
C11B N12B H12D 109.0
H12C N12B H12D 107.8
N12B C13B C7B 110.6(5)
N12B C13B H13C 109.5
C7B C13B H13C 109.5
N12B C13B H13D 109.5
C7B C13B H13D 109.5
H13C C13B H13D 108.1
O12 Cl1 O11 110.1(3)
O12 Cl1 O13 110.6(3)
O11 Cl1 O13 110.1(3)
O12 Cl1 O14 109.8(3)
O11 Cl1 O14 108.3(3)
O13 Cl1 O14 107.9(3)
O21 Cl2 O24 110.0(3)
O21 Cl2 O23 109.7(3)
O24 Cl2 O23 110.5(3)
O21 Cl2 O22 109.9(3)
O24 Cl2 O22 107.7(3)
O23 Cl2 O22 109.0(3)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
N1A C6A 1.370(8)
N1A C2A 1.396(8)
N1A C10A 1.496(7)
C2A O2A 1.242(7)
C2A C3A 1.421(8)
C3A C4A 1.349(9)
C3A H3A 0.9500
C4A C5A 1.409(10)
C4A H4A 0.9500
C5A C6A 1.364(8)
C5A H5A 0.9500
C6A C7A 1.503(8)
C7A C13A 1.519(9)
C7A C8A 1.525(8)
C7A H7A 1.0000
C8A C9A 1.530(9)
C8A H8A1 0.9900
C8A H8A2 0.9900
C9A C10A 1.531(9)
C9A C11A 1.532(8)
C9A H9A 1.0000
C10A H10A 0.9900
C10A H10B 0.9900
C11A N12A 1.511(8)
C11A H11A 0.9900
C11A H11B 0.9900
N12A C13A 1.484(8)
N12A H12A 0.9900
N12A H12B 0.9900
C13A H13A 0.9900
C13A H13B 0.9900
N1B C2B 1.380(7)
N1B C6B 1.386(7)
N1B C10B 1.493(7)
C2B O2B 1.261(7)
C2B C3B 1.406(8)
C3B C4B 1.356(9)
C3B H3B 0.9500
C4B C5B 1.385(9)
C4B H4B 0.9500
C5B C6B 1.371(8)
C5B H5B 0.9500
C6B C7B 1.472(9)
C7B C8B 1.536(8)
C7B C13B 1.537(8)
C7B H7B 1.0000
C8B C9B 1.534(8)
C8B H8B1 0.9900
C8B H8B2 0.9900
C9B C10B 1.513(8)
C9B C11B 1.517(8)
C9B H9B 1.0000
C10B H10C 0.9900
C10B H10D 0.9900
C11B N12B 1.499(7)
C11B H11C 0.9900
C11B H11D 0.9900
N12B C13B 1.491(7)
N12B H12C 0.9900
N12B H12D 0.9900
C13B H13C 0.9900
C13B H13D 0.9900
Cl1 O12 1.431(4)
Cl1 O11 1.433(4)
Cl1 O13 1.439(4)
Cl1 O14 1.448(4)
Cl2 O21 1.417(5)
Cl2 O24 1.435(4)
Cl2 O23 1.437(5)
Cl2 O22 1.440(5)
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
C7A H7A O23 . 1.00 2.42 3.413(8) 169.5
N12A H12B O22 1_655 0.99 1.92 2.853(7) 155.1
N12A H12A O2B . 0.99 1.81 2.730(6) 153.8
C3B H3B O14 4_745 0.95 2.54 3.150(8) 121.9
C7B H7B O24 2_654 1.00 2.40 3.371(7) 164.6
C11B H11C O13 . 0.99 2.57 3.302(7) 130.6
N12B H12C O2A . 0.99 1.72 2.666(7) 157.4
N12B H12D O13 3_455 0.99 2.46 3.190(6) 130.2
N12B H12D O14 3_455 0.99 1.88 2.808(6) 155.7
C13B H13D O21 2_554 0.99 2.53 3.495(8) 163.6
C13B H13D O23 2_554 0.99 2.50 3.326(7) 141.1
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
C6A N1A C2A O2A 178.8(5)
C10A N1A C2A O2A 2.5(8)
C6A N1A C2A C3A -0.1(8)
C10A N1A C2A C3A -176.3(5)
O2A C2A C3A C4A -178.6(6)
N1A C2A C3A C4A 0.1(9)
C2A C3A C4A C5A 0.2(10)
C3A C4A C5A C6A -0.6(10)
C4A C5A C6A N1A 0.6(9)
C4A C5A C6A C7A -179.2(6)
C2A N1A C6A C5A -0.3(9)
C10A N1A C6A C5A 175.6(5)
C2A N1A C6A C7A 179.5(5)
C10A N1A C6A C7A -4.6(8)
C5A C6A C7A C13A 89.3(7)
N1A C6A C7A C13A -90.5(7)
C5A C6A C7A C8A -147.0(6)
N1A C6A C7A C8A 33.2(7)
C6A C7A C8A C9A -62.4(6)
C13A C7A C8A C9A 62.0(7)
C7A C8A C9A C10A 64.5(7)
C7A C8A C9A C11A -62.0(7)
C6A N1A C10A C9A 6.7(8)
C2A N1A C10A C9A -177.1(5)
C8A C9A C10A N1A -37.0(7)
C11A C9A C10A N1A 87.4(6)
C8A C9A C11A N12A 57.0(7)
C10A C9A C11A N12A -67.2(7)
C9A C11A N12A C13A -50.2(7)
C11A N12A C13A C7A 50.5(7)
C6A C7A C13A N12A 66.3(7)
C8A C7A C13A N12A -57.5(7)
C6B N1B C2B O2B -178.7(5)
C10B N1B C2B O2B 3.8(8)
C6B N1B C2B C3B 0.4(9)
C10B N1B C2B C3B -177.0(5)
O2B C2B C3B C4B 178.0(6)
N1B C2B C3B C4B -1.1(9)
C2B C3B C4B C5B 0.3(10)
C3B C4B C5B C6B 1.2(9)
C4B C5B C6B N1B -1.8(9)
C4B C5B C6B C7B -179.9(6)
C2B N1B C6B C5B 1.0(9)
C10B N1B C6B C5B 178.3(5)
C2B N1B C6B C7B 179.1(5)
C10B N1B C6B C7B -3.6(8)
C5B C6B C7B C8B -148.7(6)
N1B C6B C7B C8B 33.2(7)
C5B C6B C7B C13B 87.9(7)
N1B C6B C7B C13B -90.2(6)
C6B C7B C8B C9B -62.1(6)
C13B C7B C8B C9B 63.9(6)
C7B C8B C9B C10B 62.8(6)
C7B C8B C9B C11B -63.5(6)
C2B N1B C10B C9B -177.9(5)
C6B N1B C10B C9B 4.6(8)
C11B C9B C10B N1B 88.5(6)
C8B C9B C10B N1B -35.1(7)
C10B C9B C11B N12B -65.6(6)
C8B C9B C11B N12B 58.3(6)
C9B C11B N12B C13B -53.0(7)
C11B N12B C13B C7B 53.4(7)
C6B C7B C13B N12B 65.1(6)
C8B C7B C13B N12B -59.5(7)

_cod_database_fobs_code 2021282