#------------------------------------------------------------------------------
#$Date: 2022-11-08 19:40:59 +0000 (Tue, 08 Nov 2022) $
#$Revision: 279115 $
#$URL: svn://www.crystallography.net/cod/cif/2/24/41/2244173.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_2244173
loop_
_publ_author_name
'Archana, Sreeramapura D.'
'Kiran Kumar, Haruvegowda'
'Yathirajan, Hemmige S.'
'Foro, Sabine'
'Butcher, Ray J.'
_publ_section_title
;
 The structures of eleven (4-phenyl)piperazinium salts containing organic
 anions
;
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              1016
_journal_page_last               1027
_journal_paper_doi               10.1107/S2056989022009057
_journal_volume                  78
_journal_year                    2022
_chemical_absolute_configuration unk
_chemical_formula_iupac          'C10 H15 N2 +, C4 H3 O4 -'
_chemical_formula_moiety         'C10 H15 N2 +, C4 H3 O4 -'
_chemical_formula_sum            'C14 H18 N2 O4'
_chemical_formula_weight         278.30
_chemical_name_common
;
4-Phenylpiperazin-1-ium 4-carboxybut-2-enoate
;
_chemical_name_systematic
;
4-Phenylpiperazin-1-ium fumarate
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_Hall           'P 2c -2ac'
_space_group_name_H-M_alt        'P c a 21'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   26.7020(10)
_cell_length_b                   7.9626(3)
_cell_length_c                   6.7571(3)
_cell_measurement_reflns_used    6248
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.78
_cell_measurement_theta_min      2.65
_cell_volume                     1436.68(10)
_computing_cell_refinement
;
CrysAlis RED (Oxford Diffraction, 2007)
;
_computing_data_collection
;
CrysAlis CCD (Oxford Diffraction, 2007)
;
_computing_data_reduction
;
CrysAlis RED (Oxford Diffraction, 2007)
;
_computing_molecular_graphics
;
SHELXTL (Sheldrick, 2008)
;
_computing_publication_material
;
SHELXTL (Sheldrick, 2008)
;
_computing_structure_refinement
;
<i>SHELXL2014/6</i> (Sheldrick, 2015b)
;
_computing_structure_solution
;
<i>SHELXT2014</i> (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.929
_diffrn_measurement_device_type
;
Oxford Diffraction Xcalibur with Sapphire CCD
;
_diffrn_measurement_method
;
Rotation method data acquisition using omega scans.
;
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0175
_diffrn_reflns_av_unetI/netI     0.0194
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            9534
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.850
_diffrn_reflns_theta_min         2.979
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.095
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.89347
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(CrysalisRED; Oxford Diffraction, 2007)
;
_exptl_crystal_colour            'light brown'
_exptl_crystal_density_diffrn    1.287
_exptl_crystal_description       prism
_exptl_crystal_F_000             592
_exptl_crystal_size_max          0.480
_exptl_crystal_size_mid          0.440
_exptl_crystal_size_min          0.400
_refine_diff_density_max         0.166
_refine_diff_density_min         -0.133
_refine_ls_abs_structure_details
;
Flack <i>x</i> determined using 1130 quotients
[(<i>I</i>^+^)-(<i>I</i>^-^)]/[(<i>I</i>^+^)+(<i>I</i>^-^)]
(Parsons <i>et al.</i>,  2013)
;
_refine_ls_abs_structure_Flack   0.3(3)
_refine_ls_extinction_coef       0.024(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method
;
SHELXL-2018/3 (Sheldrick 2018)
;
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     191
_refine_ls_number_reflns         3127
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0408
_refine_ls_R_factor_gt           0.0337
_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^)+(0.0296P)^2^+0.3161P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0736
_refine_ls_wR_factor_ref         0.0771
_reflns_number_gt                2770
_reflns_number_total             3127
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            hb8034sup1.cif
_cod_data_source_block           12
_cod_depositor_comments
'Adding full bibliography for 2244163--2244173.cif.'
_cod_database_code               2244173
_cod_database_fobs_code          2244173
_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   0.956
_shelx_estimated_absorpt_t_max   0.963
_shelx_hkl_file
;
  -4   0   0 166590. 1048.47   3
  -5   0   0 62.9586 24.3977   3
   5   0   0 51.9773 17.1083   1
   6   0   0 58664.1 151.466   1
  -6   0   0 60489.7 194.181   3
   7   0   0 201.618 21.7638   1
  -7   0   0 282.254 35.3420   3
  -8   0   0 13790.1 109.487   3
   8   0   0 13588.3 85.6208   1
   9   0   0 141.248 20.6605   1
  -9   0   0 119.928 29.4140   3
  10   0   0 775.484 29.4356   1
 -10   0   0 807.214 42.3983   3
 -11   0   0 76.7092 34.9551   3
  11   0   0 46.8834 21.3622   1
 -12   0   0 62.6727 34.3822   3
  12   0   0 217.121 25.5160   1
 -13   0   0 39.4297 35.2856   3
  13   0   0 278.976 29.0347   1
  14   0   0 16037.9 127.311   1
 -14   0   0 16180.8 160.525   3
  15   0   0 528.285 37.6975   1
 -15   0   0 614.720 59.6271   3
 -16   0   0 8836.11 132.552   3
  16   0   0 8449.30 102.499   1
  17   0   0 309.040 37.7609   1
 -17   0   0 294.629 53.0026   3
  18   0   0 4156.60 80.2944   1
 -18   0   0 4260.37 106.047   3
 -19   0   0 208.797 63.4982   3
  19   0   0 199.609 39.7450   1
  20   0   0 8141.89 116.018   1
 -20   0   0 8423.04 151.463   3
  21   0   0 643.440 54.3598   1
 -21   0   0 466.712 76.6743   3
  22   0   0 21332.4 191.638   1
 -22   0   0 21551.4 244.445   3
  23   0   0 856.971 61.6366   1
 -23   0   0 946.893 90.9583   3
 -24   0   0 911.459 91.2049   3
 -25   0   0 230.383 83.6649   3
 -26   0   0 7286.52 170.601   3
 -27   0   0 322.649 81.7584   3
 -28   0   0 5229.74 154.429   3
 -29   0   0 474.508 101.060   3
 -30   0   0 3754.21 152.300   3
 -31   0   0 187.899 101.403   3
 -32   0   0 420.340 101.127   3
 -33   0   0 34.3188 83.7225   3
  -1   1   0 76514.6 150.124   0
   1  -1   0 77694.5 147.931   0
  -1  -1   0 77020.4 149.422   0
   1   1   0 76182.0 149.633   0
  -2  -1   0 869.085 25.2200   5
  -2  -1   0 890.337 19.7602   0
  -2   1   0 865.890 19.1699   0
   2   1   0 930.984 20.8954   0
   2  -1   0 947.392 21.6308   1
  -2  -1   0 808.235 21.9624   4
  -3  -1   0 43206.8 113.811   0
   3  -1   0 43558.9 127.279   1
   4  -1   0 28839.4 98.7624   6
   4  -1   0 30252.4 115.864   1
  -4  -1   0 28946.4 126.180   2
  -4  -1   0 29992.7 96.9099   0
  -4  -1   0 29340.4 115.823   3
  -5  -1   0 145382. 852.203   0
  -5  -1   0 148739. 313.949   2
  -6  -1   0 51703.5 203.083   2
  -6  -1   0 51357.3 185.358   3
   6  -1   0 52455.1 173.608   1
  -6   1   0 51689.7 179.404   3
  -7   1   0 2085.16 44.4072   3
   7  -1   0 2326.99 44.1608   1
  -7  -1   0 2112.80 46.5908   3
  -8   1   0 28.3276 24.1307   3
  -8  -1   0 44.5243 30.1456   3
   8   1   0 79.0176 14.0839   1
  -9   1   0 49536.5 215.132   3
  -9  -1   0 51123.5 224.077   3
   9  -1   0 50116.2 198.347   1
 -10   1   0 73474.4 275.771   3
 -10  -1   0 71579.0 279.929   3
  10  -1   0 71848.4 248.872   1
  10   1   0 72611.8 187.776   1
  11   1   0 944.139 34.0263   1
  11  -1   0 668.826 44.0734   1
 -11  -1   0 674.979 54.2135   3
  12  -1   0 11919.4 114.163   1
  12   1   0 11512.7 87.0709   1
 -12   1   0 11708.0 124.500   3
 -12  -1   0 12062.7 131.704   3
 -13   1   0 33291.2 215.393   3
  13  -1   0 33852.3 195.341   1
  13   1   0 33411.7 154.317   1
 -13  -1   0 33231.9 221.074   3
 -14  -1   0 43232.3 261.854   3
  14  -1   0 44525.2 230.108   1
  14   1   0 44279.5 185.396   1
 -14   1   0 44173.1 257.474   3
  15  -1   0 771.209 51.3427   1
  15   1   0 1009.41 42.0671   1
 -15  -1   0 1110.78 68.0946   3
 -15   1   0 1141.82 65.8913   3
  16   1   0 4152.89 66.3538   1
  16  -1   0 3965.88 80.5224   1
 -16   1   0 4063.53 94.8260   3
 -16  -1   0 3999.34 94.4833   3
 -17  -1   0 2989.26 90.9294   3
  17   1   0 2993.44 60.1971   1
 -17   1   0 2969.57 87.7571   3
  17  -1   0 2859.64 73.0035   1
  18   1   0 261.446 34.5498   1
 -18  -1   0 265.330 56.2098   3
  18  -1   0 178.026 41.6269   1
 -18   1   0 168.352 54.4078   3
 -19   1   0 3245.53 98.9453   3
  19  -1   0 3349.36 82.5554   1
 -19  -1   0 3323.26 100.768   3
  19   1   0 3206.79 68.1105   1
 -20  -1   0 2532.80 95.1190   3
 -20   1   0 2784.00 98.0172   3
  20  -1   0 2676.90 79.9791   1
 -21  -1   0 245.520 64.2344   3
 -21   1   0 263.461 67.7680   3
  21  -1   0 228.720 50.2287   1
  22  -1   0 2834.14 89.2036   1
 -22   1   0 2706.20 105.407   3
 -22  -1   0 2841.58 110.610   3
  23  -1   0 5733.44 119.698   1
 -23   1   0 5482.64 139.894   3
 -23  -1   0 5109.16 135.971   3
 -24   1   0 1055.87 86.6236   3
 -24  -1   0 1196.01 92.2541   3
  24  -1   0 1049.37 71.2340   1
 -25  -1   0 4313.71 137.370   3
 -25   1   0 4480.28 134.209   3
  25  -1   0 4106.33 107.755   1
 -26   1   0 4659.30 139.646   3
  26  -1   0 4809.74 118.144   1
 -26  -1   0 4455.61 140.268   3
 -27   1   0 457.880 88.0595   3
 -27  -1   0 514.700 85.1422   3
  27  -1   0 536.112 65.4646   1
 -28  -1   0 17.2261 87.3882   3
 -28   1   0 49.7193 81.6507   3
 -29  -1   0 904.737 100.755   3
 -29   1   0 916.088 100.368   3
 -30   1   0 548.871 99.7992   3
 -30  -1   0 473.808 86.8703   3
 -31  -1   0 130.314 85.8147   3
 -31   1   0 156.599 98.9282   3
 -32  -1   0 357.160 102.233   3
 -32   1   0 315.406 100.292   3
 -33  -1   0 1300.83 124.461   3
 -33   1   0 1156.45 114.052   3
   0  -2   0 3846.43 52.9416   6
   0  -2   0 3878.19 50.1696   0
   0  -2   0 3938.01 59.5658   5
   0  -2   0 3715.82 52.6136   4
   0   2   0 3795.46 51.3870   0
   0  -2   0 3794.01 40.3907   1
  -1  -2   0 4181.29 55.4878   6
  -1   2   0 3968.46 52.9119   0
  -1  -2   0 3672.39 54.5619   4
   1  -2   0 3897.22 51.2900   0
  -1  -2   0 4005.24 51.7352   0
  -1  -2   0 3953.92 60.6562   5
   1  -2   0 3924.84 54.3949   6
   1  -2   0 3882.44 44.1358   1
   1  -2   0 3885.31 53.1594   4
   1  -2   0 4116.33 59.1891   5
  -2  -2   0 45559.1 169.178   6
  -2  -2   0 45489.7 181.513   4
  -2  -2   0 45230.7 146.019   2
   2  -2   0 44498.9 151.131   1
  -2  -2   0 46989.8 201.847   5
   2  -2   0 44556.1 168.844   6
   2  -2   0 45045.3 165.566   4
  -2  -2   0 45404.5 161.722   0
   2   2   0 45233.3 165.990   0
  -2   2   0 45446.7 163.199   0
  -3  -2   0 203087. 424.695   5
  -3  -2   0 199405. 339.337   2
   3  -2   0 207088. 1384.44   4
   3  -2   0 204052. 354.974   6
  -3  -2   0 201392. 353.637   6
  -3  -2   0 200460. 1193.62   3
  -3  -2   0 204250. 387.628   4
  -3   2   0 202304. 1371.64   0
   3  -2   0 201352. 1125.85   2
  -3  -2   0 199734. 1355.05   0
  -4  -2   0 919.413 29.9012   0
  -4  -2   0 897.518 40.3237   5
   4  -2   0 873.769 30.4671   6
  -4  -2   0 869.206 27.1373   3
  -4  -2   0 915.341 31.6928   6
   4   2   0 953.418 32.8014   0
  -4   2   0 997.502 30.9094   0
  -4  -2   0 918.604 37.1243   4
  -4  -2   0 1060.78 33.9610   2
   5  -2   0 656.384 30.8424   1
   5  -2   0 502.474 27.4781   6
  -5  -2   0 537.262 30.5251   2
  -5  -2   0 499.742 25.0946   6
  -5  -2   0 532.059 25.7801   3
  -5  -2   0 531.731 26.6953   0
  -5   2   0 519.837 25.3697   0
  -5  -2   0 477.550 37.3972   5
  -6  -2   0 27596.5 129.860   0
  -6  -2   0 28120.8 133.462   6
  -6  -2   0 27409.4 157.400   2
   6  -2   0 27172.5 144.982   1
  -6  -2   0 27175.0 141.169   3
  -6   2   0 27235.0 128.482   0
   6  -2   0 27008.8 134.562   6
  -7  -2   0 2018.40 40.4834   0
  -7   2   0 1884.71 37.9287   0
   7  -2   0 1977.90 47.0356   1
  -7  -2   0 1821.42 49.2798   2
  -7  -2   0 1962.29 39.6337   6
  -7  -2   0 1935.99 45.0992   3
   7  -2   0 1950.71 41.4440   6
  -8  -2   0 44091.0 224.374   2
   8  -2   0 42910.1 171.647   6
  -8  -2   0 43158.3 163.869   0
  -8  -2   0 43284.6 200.944   3
  -8   2   0 42843.9 191.169   3
  -8   2   0 43125.3 162.006   0
   8  -2   0 43379.4 199.098   1
   9  -2   0 5705.21 80.2290   1
  -9  -2   0 5591.67 89.7112   2
  -9  -2   0 5873.43 64.1443   0
  -9  -2   0 5470.45 79.9683   3
  -9   2   0 5435.27 76.4138   3
  -9   2   0 5669.75 62.1094   0
   9  -2   0 5627.90 65.9277   6
 -10  -2   0 70296.4 285.062   3
  10  -2   0 70677.5 222.626   6
 -10  -2   0 70459.4 210.906   0
 -10   2   0 71819.4 271.246   3
  10  -2   0 70728.0 274.814   1
 -10   2   0 69389.6 208.105   0
 -11   2   0 124.181 22.5939   0
 -11  -2   0 156.598 25.8824   0
 -11   2   0 123.256 37.3892   3
 -11  -2   0 67.0019 38.8704   3
  11  -2   0 139.304 35.2746   1
  11  -2   0 194.607 26.2706   6
  11   2   0 204.234 17.4905   1
  12   2   0 857.779 23.9417   1
 -12  -2   0 833.906 30.2568   0
 -12  -2   0 754.506 45.6856   3
  12  -2   0 883.566 32.3543   6
 -12   2   0 803.871 29.6746   0
 -12   2   0 797.070 45.7902   3
  12  -2   0 1048.81 51.8639   1
 -13  -2   0 7768.23 74.3037   0
  13  -2   0 7971.47 107.191   1
 -13  -2   0 7910.50 113.725   3
  13  -2   0 7440.66 76.2705   6
 -13   2   0 7827.17 109.828   3
 -13   2   0 7697.28 73.2406   0
  13   2   0 7857.35 64.5896   1
 -14  -2   0 1303.93 34.6816   0
 -14  -2   0 1390.86 62.1819   3
  14  -2   0 1251.59 36.5784   6
 -14   2   0 1173.07 32.8802   0
  14  -2   0 1284.76 55.1883   1
  14   2   0 1292.16 32.2807   1
 -14   2   0 1471.09 59.0273   3
  15  -2   0 501.439 28.1507   6
  15  -2   0 465.616 47.5128   1
 -15   2   0 419.781 48.1005   3
 -15   2   0 478.110 25.5525   0
 -15  -2   0 548.797 52.9042   3
 -15  -2   0 495.957 27.2370   0
  16  -2   0 3532.50 85.2256   1
 -16  -2   0 3475.74 90.3567   3
 -16   2   0 3431.35 88.0166   3
  17  -2   0 220.823 46.5706   1
 -17   2   0 134.914 49.0323   3
 -17  -2   0 148.065 49.1384   3
  18  -2   0 902.887 58.2474   1
 -18   2   0 933.655 63.1217   3
 -18  -2   0 891.329 65.1987   3
 -19   2   0 1052.74 68.4419   3
  19  -2   0 1258.87 67.8009   1
 -19  -2   0 1162.20 75.2023   3
 -20  -2   0 3635.34 109.216   3
 -20   2   0 3642.15 104.948   3
  20  -2   0 3595.59 96.7453   1
 -21  -2   0 3823.60 114.957   3
 -21   2   0 4140.22 115.424   3
  21  -2   0 4046.98 105.056   1
 -22   2   0 1377.17 90.6893   3
 -22  -2   0 1342.65 91.6601   3
  22  -2   0 1335.21 79.1839   1
 -23   2   0 8065.91 162.056   3
  23  -2   0 8145.53 148.116   1
 -23  -2   0 7781.95 161.945   3
  24  -2   0 6468.25 141.238   1
 -24  -2   0 6592.13 163.939   3
 -24   2   0 6310.75 153.984   3
 -25  -2   0 22502.7 275.712   3
  25  -2   0 23109.2 246.807   1
 -25   2   0 22337.5 268.178   3
 -26   2   0 477.653 92.9004   3
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  14   2  -7 688.754 75.0916   1
  15  -2  -7 375.906 81.7175   1
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   1  -3  -7 123.861 78.2358   1
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   5  -3   7 214.850 93.7309   2
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   6  -3  -7 185.452 75.4286   1
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   8  -1   8 10.2410 66.0215   2
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   8   1  -8-54.3943 70.3613   1
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   9  -1  -8 58.3661 84.8200   1
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  11  -1   8 93.6477 82.8820   2
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;
_shelx_hkl_checksum              14338
_shelx_res_file
;
TITL HP12 IN PCA2(1)
    shelx.res
    created by SHELXL-2018/3 at 18:03:25 on 27-Dec-2021
CELL  0.71073 26.70200  7.96260  6.75710 90.00000 90.00000 90.00000
ZERR 4  0.00100  0.00030  0.00030  0.00000  0.00000  0.00000
LATT -1
SYMM -X, -Y, Z+ 0.50000
SYMM -X+ 0.50000, Y, Z+ 0.50000
SYMM X+ 0.50000, -Y, Z
SFAC C H N O
UNIT 56 72 8 16
rem SHEL 27 0.83
SIZE 0.48 0.44 0.40
L.S. 14
CONF
ACTA
BOND $H
htab
HTAB N2 O4
EQIV $1 -x+1/2, y-1, z+1/2
HTAB N2 O1_$1
EQIV $2 x, y-1, z+1
HTAB C7 O2_$2
EQIV $3 -x+1/2, y, z+1/2
HTAB C8 O3_$3
EQIV $4 x, y-1, z
HTAB C9 O2_$4
EQIV $5 x, y+1, z
HTAB O2 O3_$5
DFIX 0.86 0.02 N2 H21 N2 H22
DFIX 0.82 0.02 O2 H2O
omit    15   1   0   !     36.82          0.13      10.71       0.003       1.74
omit     0   0  -2  !   14049.76      19374.38       8.22       1.000       3.38
omit     2   0   2  !   13183.21      17951.48       7.78       0.963       3.28
omit     0   0   2  !   14431.00      19375.30       7.57       1.000       3.38
omit     1   1   1  !    8010.08      10643.39       6.97       0.741       5.06
omit     5   1   0  !    5692.42       7280.44       6.11       0.613       4.44
omit     1   1  -1  !    8374.25      10643.45       6.10       0.741       5.06
omit     6   0  -1  !    9730.69      11477.72       4.37       0.770       3.72
omit     4   0   0  !    6392.50       7559.20       4.35       0.625       6.68
omit     4   0  -2  !    7340.61       8564.76       4.07       0.665       3.01
omit     4   0   2  !    7354.66       8566.15       4.00       0.665       3.0
omit     6   0   1  !    9828.57      11478.30       4.11       0.770       3.72
omit     3   2   0  !    7761.49       8876.52       3.55       0.677       3.63
omit     8   0  -1  !    1546.18       1737.96       2.90       0.299       2.99
omit     1   1   0  !    2949.42       3287.87       2.80       0.412       7.63
omit     8   0   1  !    1551.96       1740.53       2.96       0.559       2.99
omit     3   1   0  !    1631.11       1825.59       2.93       0.573       5.93
omit     2   1   1  !    3721.51       4111.30       2.66       0.859       4.81
omit     4   2  -1  !    3339.70       3678.44       2.61       0.813       3.05
omit     4   2   1  !    3331.25       3678.98       2.76       0.813       3.05
omit     6   0   0  !    2227.95       2478.74       2.71       0.667       4.45
omit     2   1  -1  !    3746.21       4113.26       2.62       0.860       4.81
WGHT    0.029600    0.316100
EXTI    0.024368
FVAR       5.21257
N1    3    0.071387    0.097412    0.455976    11.00000    0.03159    0.04256 =
         0.04467    0.00661    0.00625    0.00085
N2    3    0.152886    0.188921    0.201804    11.00000    0.02579    0.03169 =
         0.05036    0.00707    0.00698    0.00146
H21   2    0.163947    0.257639    0.111171    11.00000   -1.20000
H22   2    0.175761    0.111961    0.231276    11.00000   -1.20000
C1    1    0.026752    0.191990    0.449529    11.00000    0.02923    0.03432 =
         0.03887    0.00468    0.00632   -0.00445
C2    1   -0.011178    0.156461    0.315522    11.00000    0.03845    0.04950 =
         0.05015   -0.00906    0.00014   -0.00295
AFIX  43
H2    2   -0.006524    0.072842    0.221209    11.00000   -1.20000
AFIX   0
C3    1   -0.055814    0.244246    0.320975    11.00000    0.03547    0.06363 =
         0.06704    0.00383   -0.00951   -0.00421
AFIX  43
H3    2   -0.080837    0.217775    0.230469    11.00000   -1.20000
AFIX   0
C4    1   -0.064068    0.368461    0.455466    11.00000    0.03643    0.04661 =
         0.09120    0.00658    0.00814    0.00852
AFIX  43
H4    2   -0.094144    0.427343    0.457231    11.00000   -1.20000
AFIX   0
C5    1   -0.026809    0.404147    0.588006    11.00000    0.05382    0.04738 =
         0.08043   -0.01654    0.00954    0.00571
AFIX  43
H5    2   -0.031873    0.488166    0.681492    11.00000   -1.20000
AFIX   0
C6    1    0.017939    0.318717    0.586226    11.00000    0.04231    0.04889 =
         0.05672   -0.01382   -0.00299   -0.00273
AFIX  43
H6    2    0.042619    0.346194    0.677785    11.00000   -1.20000
AFIX   0
C7    1    0.116624    0.176251    0.533537    11.00000    0.03391    0.08173 =
         0.03910    0.00267   -0.00574    0.00616
AFIX  23
H7A   2    0.140074    0.089729    0.573846    11.00000   -1.20000
H7B   2    0.108145    0.242129    0.649545    11.00000   -1.20000
AFIX   0
C8    1    0.141156    0.288081    0.382487    11.00000    0.02787    0.04769 =
         0.06036   -0.01365   -0.00097   -0.00489
AFIX  23
H8A   2    0.118887    0.380029    0.348976    11.00000   -1.20000
H8B   2    0.171722    0.335098    0.436782    11.00000   -1.20000
AFIX   0
C9    1    0.108458    0.098236    0.124102    11.00000    0.03382    0.04594 =
         0.04191   -0.00752    0.00341   -0.00036
AFIX  23
H9A   2    0.118462    0.025512    0.015935    11.00000   -1.20000
H9B   2    0.084244    0.178364    0.073747    11.00000   -1.20000
AFIX   0
C10   1    0.085025   -0.004834    0.285936    11.00000    0.03681    0.02955 =
         0.07092   -0.00280    0.01302   -0.00331
AFIX  23
H10A  2    0.055321   -0.060037    0.234969    11.00000   -1.20000
H10B  2    0.108400   -0.091175    0.327448    11.00000   -1.20000
AFIX   0
O1    4    0.282788    0.927666   -0.201948    11.00000    0.03088    0.02588 =
         0.08023    0.00256    0.00866   -0.00349
O2    4    0.206150    1.034688   -0.169949    11.00000    0.03670    0.01878 =
         0.06544    0.00383    0.00512    0.00110
H2O   2    0.221735    1.136445   -0.190038    11.00000   -1.20000
O3    4    0.242478    0.314422   -0.228055    11.00000    0.03744    0.02080 =
         0.06037   -0.00154    0.01030    0.00160
O4    4    0.174091    0.419631   -0.087397    11.00000    0.03046    0.02579 =
         0.06712    0.00876    0.01069    0.00080
C11   1    0.237664    0.912723   -0.176362    11.00000    0.03320    0.02238 =
         0.03377    0.00041    0.00111   -0.00085
C12   1    0.214436    0.744566   -0.152203    11.00000    0.02966    0.02309 =
         0.04431    0.00185    0.00447   -0.00368
AFIX  43
H12   2    0.181218    0.738436   -0.111463    11.00000   -1.20000
AFIX   0
C13   1    0.238625    0.604899   -0.185676    11.00000    0.02965    0.02242 =
         0.03691    0.00292    0.00239   -0.00279
AFIX  43
H13   2    0.271921    0.611739   -0.225248    11.00000   -1.20000
AFIX   0
C14   1    0.215782    0.435147   -0.163920    11.00000    0.02829    0.02010 =
         0.03654    0.00331   -0.00244    0.00032
HKLF 4
REM  HP12 IN PCA2(1)
REM wR2 = 0.0771, GooF = S = 1.057, Restrained GooF = 1.060 for all data
REM R1 = 0.0337 for 2770 Fo > 4sig(Fo) and 0.0408 for all 3127 data
REM 191 parameters refined using 4 restraints
END
WGHT      0.0292      0.3190
REM Instructions for potential hydrogen bonds
HTAB N2 O4
HTAB N2 O1_$1
HTAB C7 O2_$2
HTAB C8 O3_$3
HTAB C9 O2_$4
HTAB O2 O3_$5
REM Highest difference peak  0.166,  deepest hole -0.133,  1-sigma level  0.027
Q1    1   0.2223  0.8261 -0.1877  11.00000  0.05    0.17
Q2    1   0.2269  0.5263 -0.1746  11.00000  0.05    0.16
Q3    1   0.2383  1.2210 -0.1765  11.00000  0.05    0.12
Q4    1   0.2301  0.2246 -0.2365  11.00000  0.05    0.12
Q5    1   0.2224  1.0052 -0.0760  11.00000  0.05    0.11
Q6    1   0.1742  0.3222 -0.0070  11.00000  0.05    0.11
Q7    1   0.1897  0.7429 -0.1936  11.00000  0.05    0.11
Q8    1   0.1425  0.2546  0.2848  11.00000  0.05    0.11
Q9    1   0.1886  0.4448 -0.1977  11.00000  0.05    0.11
Q10   1   0.2215  0.6747 -0.2459  11.00000  0.05    0.11
Q11   1   0.0180  0.2119  0.5469  11.00000  0.05    0.11
Q12   1   0.0808  0.0930  0.2125  11.00000  0.05    0.10
Q13   1   0.0515  0.1707  0.4322  11.00000  0.05    0.10
Q14   1   0.1195 -0.0802  0.4320  11.00000  0.05    0.10
Q15   1   0.0058  0.1587  0.3972  11.00000  0.05    0.09
Q16   1   0.2511  0.3590 -0.1127  11.00000  0.05    0.09
Q17   1   0.0032  0.3954  0.5055  11.00000  0.05    0.09
Q18   1   0.0267  0.2964  0.4629  11.00000  0.05    0.09
Q19   1   0.1378  0.2065  0.4480  11.00000  0.05    0.09
Q20   1   0.1715  0.3830  0.3289  11.00000  0.05    0.09
;
_shelx_res_checksum              85336
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z+1/2'
'-x+1/2, y, z+1/2'
'x+1/2, -y, 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
N N1 0.07139(6) 0.0974(2) 0.4560(3) 0.0396(4) Uani d 1 . .
N N2 0.15289(7) 0.1889(2) 0.2018(3) 0.0359(4) Uani d 1 . .
H H21 0.1639(9) 0.258(3) 0.111(3) 0.043 Uiso d 1 . .
H H22 0.1758(8) 0.112(3) 0.231(4) 0.043 Uiso d 1 . .
C C1 0.02675(7) 0.1920(3) 0.4495(3) 0.0341(5) Uani d 1 . .
C C2 -0.01118(8) 0.1565(3) 0.3155(4) 0.0460(5) Uani d 1 . .
H H2 -0.006524 0.072842 0.221209 0.055 Uiso calc 1 . .
C C3 -0.05581(9) 0.2442(3) 0.3210(5) 0.0554(6) Uani d 1 . .
H H3 -0.080837 0.217775 0.230469 0.066 Uiso calc 1 . .
C C4 -0.06407(10) 0.3685(3) 0.4555(5) 0.0581(8) Uani d 1 . .
H H4 -0.094144 0.427343 0.457231 0.070 Uiso calc 1 . .
C C5 -0.02681(11) 0.4041(4) 0.5880(5) 0.0605(8) Uani d 1 . .
H H5 -0.031873 0.488166 0.681492 0.073 Uiso calc 1 . .
C C6 0.01794(9) 0.3187(3) 0.5862(4) 0.0493(6) Uani d 1 . .
H H6 0.042619 0.346194 0.677785 0.059 Uiso calc 1 . .
C C7 0.11662(9) 0.1763(4) 0.5335(4) 0.0516(7) Uani d 1 . .
H H7A 0.140074 0.089729 0.573846 0.062 Uiso calc 1 . .
H H7B 0.108145 0.242129 0.649545 0.062 Uiso calc 1 . .
C C8 0.14116(9) 0.2881(3) 0.3825(4) 0.0453(6) Uani d 1 . .
H H8A 0.118887 0.380029 0.348976 0.054 Uiso calc 1 . .
H H8B 0.171722 0.335098 0.436782 0.054 Uiso calc 1 . .
C C9 0.10846(8) 0.0982(3) 0.1241(3) 0.0406(5) Uani d 1 . .
H H9A 0.118462 0.025512 0.015935 0.049 Uiso calc 1 . .
H H9B 0.084244 0.178364 0.073747 0.049 Uiso calc 1 . .
C C10 0.08503(8) -0.0048(3) 0.2859(4) 0.0458(6) Uani d 1 . .
H H10A 0.055321 -0.060037 0.234969 0.055 Uiso calc 1 . .
H H10B 0.108400 -0.091175 0.327448 0.055 Uiso calc 1 . .
O O1 0.28279(5) 0.92767(16) -0.2019(3) 0.0457(4) Uani d 1 . .
O O2 0.20615(5) 1.03469(16) -0.1699(3) 0.0403(4) Uani d 1 . .
H H2O 0.2217(8) 1.136(3) -0.190(4) 0.048 Uiso d 1 . .
O O3 0.24248(5) 0.31442(15) -0.2281(3) 0.0395(4) Uani d 1 . .
O O4 0.17409(5) 0.41963(17) -0.0874(3) 0.0411(4) Uani d 1 . .
C C11 0.23766(7) 0.9127(2) -0.1764(3) 0.0298(4) Uani d 1 . .
C C12 0.21444(7) 0.7446(2) -0.1522(4) 0.0324(5) Uani d 1 . .
H H12 0.181218 0.738436 -0.111463 0.039 Uiso calc 1 . .
C C13 0.23863(7) 0.6049(2) -0.1857(3) 0.0297(4) Uani d 1 . .
H H13 0.271921 0.611739 -0.225248 0.036 Uiso calc 1 . .
C C14 0.21578(7) 0.4351(2) -0.1639(3) 0.0283(4) 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
N1 0.0316(9) 0.0426(10) 0.0447(11) 0.0009(8) 0.0062(8) 0.0066(9)
N2 0.0258(9) 0.0317(9) 0.0504(12) 0.0015(7) 0.0070(8) 0.0071(9)
C1 0.0292(10) 0.0343(10) 0.0389(11) -0.0044(8) 0.0063(9) 0.0047(10)
C2 0.0385(11) 0.0495(12) 0.0502(14) -0.0029(10) 0.0001(12) -0.0091(13)
C3 0.0355(11) 0.0636(15) 0.0670(17) -0.0042(11) -0.0095(14) 0.0038(16)
C4 0.0364(13) 0.0466(14) 0.091(2) 0.0085(11) 0.0081(15) 0.0066(16)
C5 0.0538(16) 0.0474(15) 0.080(2) 0.0057(12) 0.0095(15) -0.0165(15)
C6 0.0423(13) 0.0489(14) 0.0567(16) -0.0027(11) -0.0030(12) -0.0138(13)
C7 0.0339(13) 0.0817(19) 0.0391(13) 0.0062(13) -0.0057(10) 0.0027(14)
C8 0.0279(10) 0.0477(13) 0.0604(16) -0.0049(10) -0.0010(10) -0.0136(12)
C9 0.0338(12) 0.0459(13) 0.0419(13) -0.0004(10) 0.0034(10) -0.0075(11)
C10 0.0368(11) 0.0295(10) 0.0709(17) -0.0033(9) 0.0130(12) -0.0028(12)
O1 0.0309(7) 0.0259(7) 0.0802(13) -0.0035(6) 0.0087(9) 0.0026(9)
O2 0.0367(7) 0.0188(6) 0.0654(11) 0.0011(6) 0.0051(8) 0.0038(8)
O3 0.0374(8) 0.0208(6) 0.0604(11) 0.0016(6) 0.0103(7) -0.0015(7)
O4 0.0305(8) 0.0258(7) 0.0671(11) 0.0008(6) 0.0107(7) 0.0088(7)
C11 0.0332(10) 0.0224(9) 0.0338(11) -0.0009(7) 0.0011(9) 0.0004(9)
C12 0.0297(9) 0.0231(8) 0.0443(12) -0.0037(8) 0.0045(9) 0.0019(9)
C13 0.0297(9) 0.0224(8) 0.0369(11) -0.0028(7) 0.0024(9) 0.0029(9)
C14 0.0283(9) 0.0201(8) 0.0365(10) 0.0003(7) -0.0024(9) 0.0033(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'
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
C1 N1 C10 . . 119.1(2) ?
C1 N1 C7 . . 118.8(2) ?
C10 N1 C7 . . 108.50(18) ?
C9 N2 C8 . . 112.35(16) ?
C9 N2 H21 . . 109.1(17) ?
C8 N2 H21 . . 108.3(17) ?
C9 N2 H22 . . 107.1(16) ?
C8 N2 H22 . . 109.1(17) ?
H21 N2 H22 . . 111(2) ?
C2 C1 C6 . . 117.3(2) ?
C2 C1 N1 . . 121.9(2) ?
C6 C1 N1 . . 120.7(2) ?
C3 C2 C1 . . 120.6(2) ?
C3 C2 H2 . . 119.7 ?
C1 C2 H2 . . 119.7 ?
C4 C3 C2 . . 121.7(3) ?
C4 C3 H3 . . 119.2 ?
C2 C3 H3 . . 119.2 ?
C3 C4 C5 . . 118.0(2) ?
C3 C4 H4 . . 121.0 ?
C5 C4 H4 . . 121.0 ?
C4 C5 C6 . . 121.6(3) ?
C4 C5 H5 . . 119.2 ?
C6 C5 H5 . . 119.2 ?
C5 C6 C1 . . 120.8(2) ?
C5 C6 H6 . . 119.6 ?
C1 C6 H6 . . 119.6 ?
N1 C7 C8 . . 111.8(2) ?
N1 C7 H7A . . 109.3 ?
C8 C7 H7A . . 109.3 ?
N1 C7 H7B . . 109.3 ?
C8 C7 H7B . . 109.3 ?
H7A C7 H7B . . 107.9 ?
N2 C8 C7 . . 109.53(19) ?
N2 C8 H8A . . 109.8 ?
C7 C8 H8A . . 109.8 ?
N2 C8 H8B . . 109.8 ?
C7 C8 H8B . . 109.8 ?
H8A C8 H8B . . 108.2 ?
N2 C9 C10 . . 109.9(2) ?
N2 C9 H9A . . 109.7 ?
C10 C9 H9A . . 109.7 ?
N2 C9 H9B . . 109.7 ?
C10 C9 H9B . . 109.7 ?
H9A C9 H9B . . 108.2 ?
N1 C10 C9 . . 111.91(17) ?
N1 C10 H10A . . 109.2 ?
C9 C10 H10A . . 109.2 ?
N1 C10 H10B . . 109.2 ?
C9 C10 H10B . . 109.2 ?
H10A C10 H10B . . 107.9 ?
C11 O2 H2O . . 111.3(14) ?
O1 C11 O2 . . 125.17(17) ?
O1 C11 C12 . . 120.99(17) ?
O2 C11 C12 . . 113.83(16) ?
C13 C12 C11 . . 122.85(17) ?
C13 C12 H12 . . 118.6 ?
C11 C12 H12 . . 118.6 ?
C12 C13 C14 . . 123.57(17) ?
C12 C13 H13 . . 118.2 ?
C14 C13 H13 . . 118.2 ?
O4 C14 O3 . . 124.92(16) ?
O4 C14 C13 . . 120.10(17) ?
O3 C14 C13 . . 114.97(16) ?
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
N1 C1 . 1.411(3) ?
N1 C10 . 1.455(3) ?
N1 C7 . 1.459(3) ?
N2 C9 . 1.485(3) ?
N2 C8 . 1.487(3) ?
N2 H21 . 0.87(2) ?
N2 H22 . 0.89(2) ?
C1 C2 . 1.388(3) ?
C1 C6 . 1.388(3) ?
C2 C3 . 1.382(3) ?
C2 H2 . 0.9300 ?
C3 C4 . 1.361(4) ?
C3 H3 . 0.9300 ?
C4 C5 . 1.368(4) ?
C4 H4 . 0.9300 ?
C5 C6 . 1.375(4) ?
C5 H5 . 0.9300 ?
C6 H6 . 0.9300 ?
C7 C8 . 1.505(4) ?
C7 H7A . 0.9700 ?
C7 H7B . 0.9700 ?
C8 H8A . 0.9700 ?
C8 H8B . 0.9700 ?
C9 C10 . 1.504(3) ?
C9 H9A . 0.9700 ?
C9 H9B . 0.9700 ?
C10 H10A . 0.9700 ?
C10 H10B . 0.9700 ?
O1 C11 . 1.223(2) ?
O2 C11 . 1.286(2) ?
O2 H2O . 0.921(19) ?
O3 C14 . 1.273(2) ?
O4 C14 . 1.234(2) ?
C11 C12 . 1.485(2) ?
C12 C13 . 1.306(3) ?
C12 H12 . 0.9300 ?
C13 C14 . 1.490(2) ?
C13 H13 . 0.9300 ?
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
_geom_hbond_publ_flag
N2 H21 O4 . 0.87(2) 1.88(2) 2.741(2) 168(2) yes
N2 H22 O1 3_545 0.89(2) 1.89(2) 2.775(2) 172(2) yes
C7 H7A O2 1_546 0.97 2.51 3.317(3) 140.5 yes
C8 H8B O3 3 0.97 2.55 3.203(3) 124.4 yes
C9 H9A O2 1_545 0.97 2.66 3.318(3) 125.6 yes
O2 H2O O3 1_565 0.921(19) 1.543(19) 2.4610(18) 174(2) yes
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
C10 N1 C1 C2 . . . . 18.6(3) ?
C7 N1 C1 C2 . . . . 154.6(2) ?
C10 N1 C1 C6 . . . . -165.3(2) ?
C7 N1 C1 C6 . . . . -29.3(3) ?
C6 C1 C2 C3 . . . . -0.4(4) ?
N1 C1 C2 C3 . . . . 175.8(2) ?
C1 C2 C3 C4 . . . . 0.5(4) ?
C2 C3 C4 C5 . . . . -0.5(4) ?
C3 C4 C5 C6 . . . . 0.4(5) ?
C4 C5 C6 C1 . . . . -0.3(5) ?
C2 C1 C6 C5 . . . . 0.3(4) ?
N1 C1 C6 C5 . . . . -176.0(3) ?
C1 N1 C7 C8 . . . . -79.5(3) ?
C10 N1 C7 C8 . . . . 60.7(3) ?
C9 N2 C8 C7 . . . . 53.1(3) ?
N1 C7 C8 N2 . . . . -57.3(3) ?
C8 N2 C9 C10 . . . . -52.9(2) ?
C1 N1 C10 C9 . . . . 79.8(2) ?
C7 N1 C10 C9 . . . . -60.2(3) ?
N2 C9 C10 N1 . . . . 56.7(2) ?
O1 C11 C12 C13 . . . . -10.5(4) ?
O2 C11 C12 C13 . . . . 168.7(2) ?
C11 C12 C13 C14 . . . . -179.4(2) ?
C12 C13 C14 O4 . . . . -9.5(3) ?
C12 C13 C14 O3 . . . . 170.9(2) ?