#------------------------------------------------------------------------------
#$Date: 2023-08-24 04:44:45 +0300 (Thu, 24 Aug 2023) $
#$Revision: 285856 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/02/28/2022844.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_2022844
loop_
_publ_author_name
'Anil Kumar, Haleyur G.'
'Mohan Kumar, Thaluru M.'
'Divakara, Thayamma R.'
'Geetha, Doreswamy'
'Yathirajan, Hemmige S.'
'Parkin, Sean'
_publ_section_title
;
Crystal structure studies and Hirshfeld surface analysis of
4-(dimethylazaniumyl)-2-hydroxyanilinium dichloride monohydrate at
90 K
;
_journal_coeditor_code VM2289
_journal_issue 9
_journal_name_full
'Acta Crystallographica Section E Crystallographic Communications'
_journal_paper_doi 10.1107/S2056989023007223
_journal_volume 79
_journal_year 2023
_chemical_formula_iupac 'C8 H14 N2 O 2+, 2Cl -, H2 O'
_chemical_formula_moiety 'C8 H14 N2 O 2+, 2(Cl -), H2 O'
_chemical_formula_sum 'C8 H16 Cl2 N2 O2'
_chemical_formula_weight 243.13
_chemical_name_systematic
;
4-(Dimethylazaniumyl)-2-hydroxyanilinium dichloride monohydrate
;
_space_group_crystal_system monoclinic
_space_group_IT_number 14
_space_group_name_Hall '-P 2yn'
_space_group_name_H-M_alt 'P 1 21/n 1'
_atom_sites_solution_hydrogens mixed
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_audit_creation_method 'SHELXL-2019/2 and CIFFIX'
_cell_angle_alpha 90
_cell_angle_beta 117.188(2)
_cell_angle_gamma 90
_cell_formula_units_Z 4
_cell_length_a 9.6493(7)
_cell_length_b 13.0873(8)
_cell_length_c 10.4634(7)
_cell_measurement_reflns_used 9459
_cell_measurement_temperature 90.0(2)
_cell_measurement_theta_max 27.48
_cell_measurement_theta_min 2.38
_cell_volume 1175.36(14)
_computing_cell_refinement
;
APEX3 (Bruker, 2016)
;
_computing_data_collection
;
APEX3 (Bruker, 2016)
;
_computing_data_reduction
;
APEX3 (Bruker, 2016)
;
_computing_molecular_graphics
;
XP in SHELXTL (Sheldrick, 2008)
;
_computing_publication_material
;
SHELX (Sheldrick, 2008) and publCIF (Westrip,
2010)
;
_computing_structure_refinement
;
SHELXL2019/2 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT (Sheldrick, 2015a)
;
_diffrn_ambient_temperature 90.0(2)
_diffrn_detector_area_resol_mean 7.41
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type 'Bruker D8 Venture dual source'
_diffrn_measurement_method '\f and \w scans'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0319
_diffrn_reflns_av_unetI/netI 0.0139
_diffrn_reflns_limit_h_max 12
_diffrn_reflns_limit_h_min -12
_diffrn_reflns_limit_k_max 17
_diffrn_reflns_limit_k_min -16
_diffrn_reflns_limit_l_max 13
_diffrn_reflns_limit_l_min -13
_diffrn_reflns_number 36719
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 27.512
_diffrn_reflns_theta_min 2.382
_diffrn_source microsource
_exptl_absorpt_coefficient_mu 0.532
_exptl_absorpt_correction_T_max 0.971
_exptl_absorpt_correction_T_min 0.888
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
(SADABS; Krause et al., 2015)
;
_exptl_crystal_colour colourless
_exptl_crystal_density_diffrn 1.374
_exptl_crystal_description 'irregular block'
_exptl_crystal_F_000 512
_exptl_crystal_size_max 0.320
_exptl_crystal_size_mid 0.300
_exptl_crystal_size_min 0.220
_refine_diff_density_max 0.340
_refine_diff_density_min -0.218
_refine_ls_extinction_coef 0.008(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method
;
SHELXL-2019/2 (Sheldrick 2015b)
;
_refine_ls_goodness_of_fit_ref 1.126
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 158
_refine_ls_number_reflns 2693
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.126
_refine_ls_R_factor_all 0.0233
_refine_ls_R_factor_gt 0.0210
_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^)+(0.0340P)^2^+0.2669P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0616
_refine_ls_wR_factor_ref 0.0632
_reflns_number_gt 2505
_reflns_number_total 2693
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file vm2289sup1.cif
_cod_data_source_block I
_cod_original_sg_symbol_H-M 'P 21/n'
_cod_database_code 2022844
_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 0.848
_shelx_estimated_absorpt_t_max 0.892
_shelx_hkl_file
;
-1 0 0 0.19122 0.32081 2
-1 0 0 1.60686 0.47998 3
-1 0 0 0.76368 0.31528 4
-1 0 0 0.31437 0.30852 6
-1 0 0 -0.0827 0.19246 6
-1 0 0 0.66044 0.38344 2
1 0 0 0.46005 0.28559 3
1 0 0 0.34145 0.25179 4
1 0 0 0.73812 0.27751 6
1 0 0 0.63685 0.42541 2
1 0 0 0.35807 0.30790 2
1 0 0 2.10852 0.50554 6
-3 0 0 1.54481 0.90598 6
-3 0 0 0.15647 0.57334 3
-3 0 0 2.99129 1.05361 4
-3 0 0 -0.8195 0.63657 2
-3 0 0 0.49673 0.93323 2
-3 0 0 -0.3543 0.51784 6
3 0 0 0.32065 0.64022 6
3 0 0 -0.0726 0.48166 6
3 0 0 -0.1677 0.85126 2
3 0 0 -0.3992 0.70340 2
3 0 0 1.05531 1.01416 3
-4 0 0 488.291 17.3317 2
-4 0 0 504.886 16.4123 6
-4 0 0 504.622 15.9477 6
-4 0 0 502.410 17.2581 3
-4 0 0 519.647 17.0595 2
-4 0 0 492.736 16.1462 4
4 0 0 512.663 14.8964 6
4 0 0 507.363 17.8653 3
4 0 0 529.960 16.1903 4
4 0 0 499.131 17.3037 2
4 0 0 490.314 15.7922 6
4 0 0 499.923 16.7206 2
-5 0 0 -1.4555 1.24376 2
-5 0 0 0.91303 1.18287 4
-5 0 0 0.41142 1.97485 2
-5 0 0 1.94418 1.54015 3
-5 0 0 -0.4657 1.07697 6
-5 0 0 0.99289 1.43251 6
5 0 0 0.69271 0.86028 6
5 0 0 0.01903 1.10858 4
5 0 0 0.91877 1.61772 2
5 0 0 2.48272 1.60879 2
5 0 0 -2.5651 1.26789 3
-6 0 0 333.693 14.1654 2
-6 0 0 324.330 14.9728 2
-6 0 0 299.607 12.9810 4
-6 0 0 313.849 13.4822 6
-6 0 0 304.536 12.8911 6
-6 0 0 321.705 14.4409 3
6 0 0 322.481 13.7965 2
6 0 0 321.246 11.1945 6
6 0 0 331.421 12.4187 6
6 0 0 289.248 14.2673 2
6 0 0 298.574 14.8986 3
-7 0 0 -0.3317 2.08076 3
-7 0 0 -2.3924 1.98809 4
-7 0 0 -0.7171 3.01050 2
-7 0 0 0.31245 2.25968 2
7 0 0 -0.9554 2.36218 2
7 0 0 1.26469 2.72654 2
7 0 0 -0.2312 1.28263 6
7 0 0 2.76630 2.16829 3
7 0 0 -3.1796 1.74236 6
-8 0 0 545.951 23.9574 2
-8 0 0 521.932 25.1547 3
8 0 0 549.339 18.7253 6
8 0 0 557.361 21.7992 2
-9 0 0 -1.6520 3.32713 2
-9 0 0 4.02120 3.40893 6
-9 0 0 -9.7746 4.96660 2
-9 0 0 0.98041 3.20472 3
9 0 0 0.44355 3.38529 2
9 0 0 -1.2330 2.80059 6
9 0 0 -0.5557 2.38022 6
-10 0 0 1345.38 45.3477 3
-10 0 0 1254.00 47.5493 2
-10 0 0 1311.50 43.9992 2
-10 0 0 1359.77 44.1067 6
10 0 0 1300.97 43.3528 2
-11 0 0 -1.4208 2.59246 3
-11 0 0 2.69280 4.63461 6
-11 0 0 0.16424 4.40965 5
-11 0 0 -3.6173 3.96522 2
11 0 0 -0.8484 5.22935 2
-11 1 0 58.9977 9.53519 2
-11 1 0 37.3827 6.75418 3
-11 1 0 42.4595 8.47001 5
10 -1 0 446.138 20.2925 2
-10 1 0 452.559 21.9310 5
-10 1 0 437.003 20.9271 6
-10 1 0 435.628 21.7905 3
-10 1 0 426.811 24.2041 2
-10 1 0 430.641 20.5049 2
9 -1 0 70.4649 7.73291 2
9 -1 0 59.4341 3.36642 6
-9 1 0 53.1174 8.73627 2
-9 1 0 52.8870 6.94830 6
-9 1 0 61.2411 7.82801 2
-9 1 0 62.4327 7.77257 3
8 -1 0 42.8938 3.34453 6
8 -1 0 47.8422 6.48316 2
-8 1 0 54.4388 6.02243 6
-8 1 0 34.1378 6.41662 2
-8 1 0 44.4095 5.99473 3
-8 1 0 35.1951 5.89683 6
-8 1 0 41.6620 7.03976 2
7 -1 0 1.38148 1.94408 3
7 -1 0 4.05886 1.44076 6
7 -1 0 -1.0199 2.34269 2
7 -1 0 4.46080 2.56118 2
-7 1 0 1.69155 2.29962 4
-7 1 0 0.76888 2.32219 2
-7 1 0 -0.2757 2.01105 6
-7 1 0 1.44415 2.63612 2
-7 1 0 -0.3273 1.61946 3
6 -1 0 488.740 15.8750 6
6 -1 0 525.687 15.0758 6
6 -1 0 514.937 18.2768 2
6 -1 0 475.493 19.2281 2
6 -1 0 504.686 20.5607 3
-6 1 0 481.905 17.8280 4
-6 1 0 518.327 19.6608 3
-6 1 0 499.744 17.5447 6
-6 1 0 488.747 19.6447 2
-6 1 0 529.443 18.7324 2
-6 1 0 520.280 18.3045 6
5 -1 0 47.3751 5.13494 3
5 -1 0 41.1651 3.95674 2
5 -1 0 32.0910 2.97802 6
5 -1 0 39.2919 2.62351 6
5 -1 0 36.7814 4.34332 2
-5 1 0 35.4191 3.61722 4
-5 1 0 38.3323 4.26964 6
-5 1 0 31.6162 3.27739 6
-5 1 0 36.9502 4.41452 2
-5 1 0 45.7264 4.24322 2
-5 1 0 40.6399 4.39270 3
4 -1 0 264.333 9.15994 6
4 -1 0 260.643 11.5082 3
4 -1 0 258.098 8.37450 6
4 -1 0 265.552 10.7974 2
4 -1 0 277.765 10.3054 2
-4 1 0 276.930 11.0126 2
-4 1 0 286.745 11.4278 3
-4 1 0 265.637 10.0533 6
-4 1 0 263.584 9.46372 6
-4 1 0 285.333 10.3587 4
-4 1 0 270.732 10.4075 2
3 -1 0 32.0557 1.86167 6
3 -1 0 35.8785 2.75034 2
3 -1 0 38.8915 3.49274 3
3 -1 0 38.5928 3.00522 2
3 -1 0 34.8948 2.22402 6
-3 1 0 34.0312 2.77216 2
-3 1 0 32.4781 2.58947 4
-3 1 0 33.5168 2.85317 2
-3 1 0 35.9114 2.35113 6
-3 1 0 34.1783 3.02665 3
-3 1 0 36.6850 2.75589 6
2 -1 0 1013.92 27.3044 2
2 -1 0 1043.22 28.2551 3
-2 1 0 1050.75 27.2202 2
-2 1 0 1099.20 28.2192 3
-2 1 0 1056.41 27.2401 4
1 -1 0 414.456 11.3588 3
1 -1 0 405.908 10.6802 2
-1 1 0 405.175 11.2584 3
-1 1 0 416.392 10.2732 6
-1 1 0 410.920 11.1931 5
-1 1 0 405.987 10.1784 6
-1 -1 0 432.283 11.9607 2
-1 -1 0 407.780 11.1974 3
-1 -1 0 402.298 11.3781 6
-1 -1 0 410.322 11.3101 6
-1 -1 0 413.856 11.8301 2
-1 -1 0 403.919 11.2359 4
1 1 0 408.021 11.2682 3
1 1 0 397.167 11.8034 2
1 1 0 419.388 11.2706 4
1 1 0 403.833 11.4046 6
1 1 0 412.328 11.3081 6
1 1 0 393.898 11.7523 2
-2 -1 0 1075.09 28.8260 2
-2 -1 0 1037.45 28.0296 3
-2 -1 0 1043.04 27.6930 6
2 1 0 1123.76 28.8018 2
2 1 0 1029.32 28.6407 2
2 1 0 1015.45 28.1664 3
-3 -1 0 38.4612 3.45578 2
-3 -1 0 30.3431 2.57928 4
-3 -1 0 37.0030 3.12326 3
-3 -1 0 36.6614 3.49544 2
-3 -1 0 35.9548 3.07687 6
-3 -1 0 39.9954 3.06055 6
3 1 0 39.8969 3.53504 2
3 1 0 37.4757 2.75521 6
3 1 0 38.8720 3.40773 3
3 1 0 39.6315 3.14447 6
3 1 0 36.4136 3.36904 2
3 1 0 37.3230 2.83185 4
-4 -1 0 280.562 11.5012 2
-4 -1 0 270.531 10.8135 6
-4 -1 0 239.857 11.3422 2
-4 -1 0 268.458 10.4645 6
-4 -1 0 275.762 10.4341 4
-4 -1 0 280.439 11.3154 3
4 1 0 301.144 12.1442 6
4 1 0 255.363 11.4913 2
4 1 0 264.757 9.70730 6
4 1 0 281.762 11.4291 2
4 1 0 274.636 10.2424 4
4 1 0 262.297 11.5215 3
-5 -1 0 39.7269 3.96545 4
-5 -1 0 34.0762 3.93826 6
-5 -1 0 33.5871 3.80965 6
-5 -1 0 41.3495 4.36366 3
-5 -1 0 39.0466 4.43016 2
-5 -1 0 39.4120 4.75247 2
5 1 0 35.8211 4.57900 3
5 1 0 37.4501 3.33921 6
5 1 0 39.4062 3.84465 6
5 1 0 36.8286 4.64993 2
5 1 0 50.6473 4.24795 4
5 1 0 47.3050 4.69718 2
-6 -1 0 489.246 18.2859 6
-6 -1 0 501.659 18.7409 6
-6 -1 0 494.544 20.7461 2
-6 -1 0 525.000 19.6408 3
-6 -1 0 516.915 19.5781 2
-6 -1 0 476.524 18.0195 4
6 1 0 498.143 17.7959 4
6 1 0 467.916 19.9649 3
6 1 0 504.680 20.3054 2
6 1 0 492.409 17.7464 6
6 1 0 541.998 19.6560 2
-7 -1 0 2.50494 1.88055 3
-7 -1 0 -0.1066 2.09712 6
-7 -1 0 1.06795 2.96283 2
-7 -1 0 0.87443 2.69236 6
-7 -1 0 -1.4401 2.28935 2
-7 -1 0 3.19804 2.54200 4
7 1 0 1.63161 1.90132 6
7 1 0 4.82222 3.32672 2
7 1 0 -2.3941 1.72943 4
7 1 0 -0.2149 2.54015 6
7 1 0 3.33572 2.78231 2
7 1 0 1.63211 2.77335 3
-8 -1 0 42.3053 6.69361 3
-8 -1 0 44.6616 7.39776 2
-8 -1 0 38.9464 7.03449 2
8 1 0 60.2182 7.59827 6
8 1 0 55.1935 12.0476 2
8 1 0 30.7381 4.70531 6
-9 -1 0 55.6391 7.62184 2
-9 -1 0 60.1994 7.61452 3
-9 -1 0 52.9965 7.26207 6
-9 -1 0 75.9375 9.88179 2
9 1 0 55.4788 5.44767 6
9 1 0 65.2115 8.04251 2
-10 -1 0 493.939 22.2200 6
-10 -1 0 414.841 24.7928 2
-10 -1 0 466.038 22.5472 3
10 1 0 438.810 17.7068 6
10 1 0 470.949 22.7872 2
-11 -1 0 30.3569 6.15804 3
-11 -1 0 31.8397 7.39663 2
-11 -1 0 40.4345 7.75895 6
11 1 0 42.3014 8.05090 2
-11 2 0 190.843 13.8969 2
-11 2 0 188.553 13.9503 3
10 -2 0 5.14097 5.05253 2
-10 2 0 5.35436 4.26347 3
-10 2 0 3.19160 3.79860 2
-10 2 0 11.8200 4.83003 5
-10 2 0 5.53136 4.11610 6
-10 2 0 9.89095 5.64860 2
9 -2 0 852.382 29.0482 2
-9 2 0 812.165 29.6087 6
-9 2 0 813.955 32.3702 2
-9 2 0 888.328 30.1994 2
-9 2 0 835.993 31.6752 3
8 -2 0 41.2129 5.41608 2
-8 2 0 48.1558 7.58509 2
-8 2 0 44.8553 6.31092 5
-8 2 0 44.9644 5.58956 6
-8 2 0 36.7225 6.04367 2
-8 2 0 39.8969 5.54163 6
-8 2 0 49.8503 6.73692 3
7 -2 0 2049.07 53.7597 2
7 -2 0 1811.21 57.7659 3
7 -2 0 1822.50 55.2374 2
-7 2 0 2032.10 56.5015 3
-7 2 0 2008.56 54.3168 2
-7 2 0 1828.40 52.6709 6
-7 2 0 1882.44 53.8119 4
-7 2 0 1943.52 56.1550 2
6 -2 0 120.023 4.42463 6
6 -2 0 127.474 8.18194 2
6 -2 0 118.300 7.25184 2
6 -2 0 115.959 8.69271 3
6 -2 0 124.124 4.29119 6
-6 2 0 115.944 7.28010 6
-6 2 0 106.598 6.99766 4
-6 2 0 116.976 6.72841 6
-6 2 0 101.605 8.40308 2
-6 2 0 123.564 8.19319 3
-6 2 0 138.350 7.81563 2
5 -2 0 2157.92 54.1843 6
5 -2 0 2165.70 58.8582 2
5 -2 0 2224.21 53.9503 6
5 -2 0 2121.59 60.7671 3
5 -2 0 2263.36 57.8414 2
-5 2 0 2254.55 58.1206 2
-5 2 0 2193.51 57.7358 6
-5 2 0 2149.56 56.7796 6
-5 2 0 2139.90 57.8592 4
-5 2 0 2331.22 60.3124 3
-5 2 0 2242.06 59.3631 2
4 -2 0 24.6923 1.43133 6
4 -2 0 23.2693 3.11651 3
4 -2 0 23.3121 2.71598 2
4 -2 0 24.9199 1.38520 6
4 -2 0 23.7937 2.71460 2
-4 2 0 28.3074 3.29606 3
-4 2 0 24.9933 2.97879 2
-4 2 0 21.2302 2.33611 6
-4 2 0 22.1372 2.58281 4
-4 2 0 20.2070 2.03567 6
-4 2 0 25.3446 2.78368 2
3 -2 0 3504.04 90.1641 1
-3 2 0 3410.48 88.8157 1
2 -2 0 25.1711 2.19822 3
2 -2 0 20.9987 1.62016 2
-2 2 0 20.8097 2.01547 3
-2 2 0 21.8804 1.24908 6
-2 2 0 22.7385 2.12018 5
-2 2 0 24.1409 1.74189 2
-2 2 0 23.2402 1.68781 2
-2 2 0 22.6876 1.38680 6
1 -2 0 2290.35 56.3946 1
-1 2 0 2260.66 56.5113 1
0 -2 0 75.4901 2.65475 5
0 -2 0 74.5998 2.47170 6
0 -2 0 70.1539 2.30063 6
0 -2 0 71.9783 3.62811 2
0 -2 0 76.9828 3.15954 2
0 -2 0 77.5819 3.30234 4
0 2 0 69.4454 2.48382 6
0 2 0 73.4184 3.24736 4
0 2 0 72.3349 3.11321 2
0 2 0 71.6602 2.64389 5
0 2 0 71.4687 3.09199 2
0 2 0 71.2734 2.63052 6
-1 -2 0 2184.99 60.5842 1
1 2 0 2345.11 61.2842 1
-2 -2 0 22.7267 2.55164 2
-2 -2 0 25.3718 2.55352 2
-2 -2 0 20.0183 2.14668 6
-2 -2 0 23.5015 2.09201 3
-2 -2 0 19.0551 1.99042 4
-2 -2 0 24.3770 2.30380 6
-2 -2 0 23.5263 2.12202 5
2 2 0 23.1209 2.06075 6
2 2 0 23.3077 2.55251 2
2 2 0 24.1389 2.21661 3
2 2 0 23.1625 2.59598 2
2 2 0 21.9448 2.26635 6
2 2 0 25.0261 2.17522 4
-3 -2 0 3561.45 97.4079 1
3 2 0 3542.30 98.4994 1
-4 -2 0 20.1341 2.92444 6
-4 -2 0 25.2976 3.09213 3
-4 -2 0 22.8440 2.93666 6
-4 -2 0 24.1062 2.83784 4
-4 -2 0 20.4154 3.32787 2
-4 -2 0 25.1331 3.48126 2
4 2 0 20.0398 2.63648 4
4 2 0 22.9116 3.48305 2
4 2 0 27.7899 3.26402 3
4 2 0 19.6663 3.20471 2
4 2 0 19.6070 2.93492 6
4 2 0 22.9249 2.75794 6
-5 -2 0 2133.41 61.7363 2
-5 -2 0 2240.19 59.5644 6
-5 -2 0 2131.49 58.5827 4
-5 -2 0 2169.37 59.5400 3
-5 -2 0 2274.82 60.8218 2
-5 -2 0 2147.19 58.9695 6
5 2 0 2420.47 60.1825 6
5 2 0 2082.68 61.0682 2
5 2 0 2140.91 58.9495 6
5 2 0 2140.06 60.5995 3
5 2 0 2262.36 58.3406 4
5 2 0 2213.76 60.4756 2
-6 -2 0 117.509 9.14089 2
-6 -2 0 131.927 8.38357 3
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-8 4 12 437.025 20.2839 5
7 -4 -12 31.1858 7.51255 2
7 -4 -12 41.1673 8.06240 6
-7 4 12 36.9877 8.36143 2
-7 4 12 35.7003 7.01024 5
-7 4 12 39.6598 7.23229 6
6 -4 -12 39.8609 9.25326 2
6 -4 -12 42.9847 8.03598 6
-6 4 12 33.3832 5.54837 4
-6 4 12 43.8562 6.14744 4
-6 4 12 44.0314 7.69759 5
-6 4 12 44.6863 7.74242 6
5 -4 -12 89.7945 10.5615 6
5 -4 -12 75.2969 11.0934 2
-5 4 12 73.5864 6.49233 4
-5 4 12 79.5540 6.44554 4
-5 4 12 75.6857 9.81809 6
-5 4 12 68.6397 9.04517 5
4 -4 -12 70.0992 11.1334 2
4 -4 -12 64.2990 9.39127 6
-4 4 12 62.9636 11.4670 2
-4 4 12 58.6078 5.00228 4
-4 4 12 70.3160 8.39801 6
-4 4 12 70.4825 9.12240 5
-4 4 12 56.3681 4.71390 4
3 -4 -12 -4.2332 3.90917 6
3 -4 -12 -1.3077 5.09893 2
-3 4 12 1.43532 4.47510 5
-3 4 12 6.08615 7.24974 2
-2 4 12 333.365 20.0397 5
-2 4 12 365.082 17.9185 6
-2 4 12 397.316 24.5756 2
1 -4 -12 37.4272 8.40706 6
1 -4 -12 41.6979 10.8345 2
-1 4 12 35.0847 9.61666 2
9 -5 -12 11.6301 5.45202 6
9 -5 -12 15.6640 6.94313 2
-9 5 12 16.1372 5.84424 6
-9 5 12 12.4945 4.40622 5
-9 5 12 20.1164 6.99315 2
8 -5 -12 303.630 20.7707 2
-8 5 12 262.618 16.8908 6
-8 5 12 278.457 16.5139 5
-8 5 12 298.261 20.3362 2
7 -5 -12 632.436 31.9232 2
7 -5 -12 677.856 29.7651 6
-7 5 12 663.721 26.9715 5
-7 5 12 625.986 27.6221 6
6 -5 -12 307.447 18.8380 6
6 -5 -12 268.915 20.0836 2
-6 5 12 275.775 20.0195 2
-6 5 12 277.660 14.5321 4
-6 5 12 283.337 17.0599 6
-6 5 12 266.815 14.9210 4
-6 5 12 291.510 16.6937 5
5 -5 -12 540.235 29.1169 2
5 -5 -12 502.341 25.4811 6
-5 5 12 540.182 28.8243 2
-5 5 12 533.924 20.2040 4
-5 5 12 497.042 23.6905 6
-5 5 12 537.183 24.1408 5
4 -5 -12 35.7922 6.98235 6
4 -5 -12 39.1403 9.94746 2
-4 5 12 28.2018 4.31124 4
-4 5 12 43.5819 7.80967 6
-4 5 12 21.8955 7.69590 2
-4 5 12 27.8394 4.79358 4
-4 5 12 34.1089 7.04194 5
3 -5 -12 1.46177 5.12662 2
-3 5 12 -0.6063 4.26943 5
-3 5 12 -0.1276 4.87789 6
-3 5 12 -1.8996 1.86722 4
2 -5 -12 17.6138 8.29050 2
2 -5 -12 9.12507 6.12096 6
-2 5 12 0.25712 6.83378 2
-2 5 12 19.0180 6.89073 5
-2 5 12 9.18671 4.68508 6
1 -5 -12 43.7138 10.5099 2
1 -5 -12 29.9129 8.69340 6
8 -6 -12 -3.3467 5.37261 2
-8 6 12 13.2650 4.63254 5
-8 6 12 7.11623 5.66550 6
7 -6 -12 -1.7355 5.24109 2
-7 6 12 2.88872 3.37737 4
-7 6 12 1.48772 4.26926 6
-7 6 12 -1.7565 3.43268 5
-6 6 12 95.2229 8.60652 4
-6 6 12 100.345 10.7245 6
-6 6 12 76.4117 10.2788 5
-6 6 12 96.2901 12.9880 2
5 -6 -12 12.7543 6.12974 2
-5 6 12 3.21523 4.79387 6
-5 6 12 13.4485 6.36170 2
-5 6 12 8.55996 4.38609 4
-5 6 12 6.69494 4.97063 4
-5 6 12 7.56163 4.39707 5
4 -6 -12 33.8004 9.47005 2
-4 6 12 22.2538 7.82420 2
-4 6 12 30.4617 6.83443 6
3 -6 -12 7.68673 5.44682 6
-3 6 12 30.7838 6.93691 5
-3 6 12 26.8792 8.67096 2
-3 6 12 11.9336 5.32398 6
2 -6 -12 107.419 13.1226 6
2 -6 -12 110.265 14.6452 2
-2 6 12 110.650 15.3857 2
-2 6 12 93.1144 12.8190 5
-2 6 12 109.968 12.0915 6
7 -7 -12 6.12244 6.11185 6
7 -7 -12 -4.7653 5.47861 2
-7 7 12 1.05021 6.41699 2
-7 7 12 9.17951 6.24732 6
-7 7 12 14.9460 5.73437 4
-7 7 12 -2.1513 3.97114 5
6 -7 -12 259.813 20.8481 2
6 -7 -12 257.326 21.3558 6
-6 7 12 260.715 17.2125 6
-6 7 12 277.124 17.2400 5
-6 7 12 286.637 21.4619 2
5 -7 -12 23.9691 8.56532 2
5 -7 -12 15.0981 6.08190 6
-5 7 12 28.6243 5.86212 4
-5 7 12 21.9769 7.63934 2
-5 7 12 28.5768 7.22049 6
-5 7 12 23.5217 6.40657 5
4 -7 -12 23.1089 7.16599 6
4 -7 -12 7.30850 7.33125 2
-4 7 12 8.96056 6.56316 2
-4 7 12 13.3795 5.92636 5
-4 7 12 11.3401 4.02358 4
-4 7 12 13.1658 5.62645 6
3 -7 -12 125.817 14.0167 6
3 -7 -12 74.8390 15.5978 2
-3 7 12 98.0319 8.12332 4
-3 7 12 154.339 16.4449 2
-3 7 12 123.578 12.3779 6
7 4 -13 12.4230 5.64488 6
7 4 -13 2.89431 5.64784 2
-7 -4 13 3.84072 6.53327 2
6 4 -13 46.1282 7.97876 2
5 4 -13 60.7866 9.45532 2
5 4 -13 86.2157 8.86782 6
4 4 -13 132.451 12.2243 2
4 4 -13 129.780 10.9741 6
8 3 -13 45.4164 8.22880 2
8 3 -13 30.2170 6.39998 6
-8 -3 13 25.7191 7.23290 2
-8 -3 13 20.3086 5.53548 6
7 3 -13 338.341 20.5419 6
-7 -3 13 334.003 19.8072 2
6 3 -13 91.1579 10.5039 2
6 3 -13 108.480 11.4153 6
-6 -3 13 84.2914 11.0110 2
5 3 -13 83.9337 9.42437 6
5 3 -13 80.3506 10.2179 2
-5 -3 13 77.2888 11.8240 2
4 3 -13 56.0312 10.1232 2
4 3 -13 72.0735 8.46815 6
3 3 -13 57.3845 8.81954 6
3 3 -13 68.5601 10.5616 2
8 2 -13 294.526 19.1287 2
-8 -2 13 340.944 20.1870 2
-8 -2 13 328.878 16.0406 6
7 2 -13 30.6133 7.29670 2
7 2 -13 68.1100 10.1906 6
-7 -2 13 48.1451 7.10974 6
-7 -2 13 50.2823 9.34143 2
-7 -2 13 52.4572 6.33295 5
6 2 -13 862.085 39.9323 2
6 2 -13 714.287 32.6954 6
-6 -2 13 808.334 33.8398 2
5 2 -13 5.76216 5.91385 2
5 2 -13 13.0338 4.72980 6
-5 -2 13 7.76050 6.13473 2
4 2 -13 78.9475 10.4967 2
4 2 -13 68.7243 8.67957 6
-4 -2 13 53.2438 10.1943 2
3 2 -13 9.46341 4.61600 6
3 2 -13 13.7617 5.70705 2
8 1 -13 16.6343 6.23610 2
8 1 -13 52.7680 8.37316 6
-8 -1 13 32.4198 5.50067 5
-8 -1 13 23.1942 6.95949 2
7 1 -13 648.806 30.6928 6
7 1 -13 544.830 27.6993 2
-7 -1 13 575.385 28.0607 2
-7 -1 13 607.952 22.2561 5
-7 -1 13 575.576 22.6737 6
6 1 -13 18.0706 7.14067 2
-6 -1 13 15.7067 4.55854 5
-6 -1 13 16.4568 4.34778 6
5 1 -13 82.7972 9.31039 6
5 1 -13 54.7038 6.86023 5
-5 -1 13 86.2268 11.4420 2
4 1 -13 93.5100 12.5314 2
4 1 -13 120.136 11.3263 6
-4 -1 13 62.3215 12.3253 2
3 1 -13 6.44308 5.07603 6
3 1 -13 5.78072 5.10173 2
-3 -1 13 -5.5103 6.97703 2
8 0 -13 -7.2197 4.16315 2
8 0 -13 -0.1627 3.57872 6
-8 0 13 -0.2527 3.81538 6
-8 0 13 6.11251 6.04101 2
-8 0 13 -1.3034 3.72064 5
7 0 -13 81.1506 12.6434 2
7 0 -13 73.7904 9.03864 6
-7 0 13 67.3473 11.2692 2
-7 0 13 54.7196 7.43424 5
-7 0 13 50.8118 9.63454 6
-6 0 13 2.49161 4.28092 6
-6 0 13 0.27387 3.80207 5
5 0 -13 209.948 14.8079 6
-5 0 13 195.690 10.8419 6
-5 0 13 215.593 13.1899 5
-5 0 13 199.644 16.7244 2
4 0 -13 -0.8792 4.02524 6
4 0 -13 3.73106 4.85626 2
-4 0 13 3.57720 5.76955 2
-3 0 13 550.970 28.9498 2
8 -1 -13 23.2178 7.16868 2
8 -1 -13 31.3038 6.63897 6
-8 1 13 31.5362 8.18051 2
-8 1 13 21.0315 4.94243 5
-8 1 13 36.2544 6.82190 6
7 -1 -13 590.400 34.0672 2
7 -1 -13 622.772 27.2219 6
-7 1 13 507.417 31.1747 2
-7 1 13 596.272 24.6697 6
-6 1 13 11.1237 4.53923 6
5 -1 -13 88.8514 14.0887 2
5 -1 -13 75.4124 11.7867 2
-5 1 13 92.5763 12.8549 2
-5 1 13 100.600 9.81207 5
4 -1 -13 96.1348 11.9262 2
-4 1 13 106.080 9.90048 6
-4 1 13 86.5060 13.8324 2
3 -1 -13 7.90686 6.05330 2
-3 1 13 6.98554 6.29753 2
8 -2 -13 311.848 21.6227 2
8 -2 -13 338.976 19.5155 6
-8 2 13 361.064 19.4901 6
-8 2 13 372.989 18.1809 5
-8 2 13 361.220 22.5924 2
7 -2 -13 39.9788 7.98067 6
-7 2 13 48.2415 8.23053 5
-7 2 13 32.1599 6.41283 6
-7 2 13 40.6663 9.05665 2
6 -2 -13 868.348 35.2134 6
-6 2 13 826.810 37.3860 2
-6 2 13 866.123 31.9069 5
5 -2 -13 4.99112 6.11923 2
5 -2 -13 9.86545 5.79972 6
-5 2 13 9.34758 4.63442 5
-5 2 13 13.3356 7.24648 2
-5 2 13 6.88018 5.07391 6
-5 2 13 1.74347 1.91896 4
4 -2 -13 89.0205 12.0936 2
4 -2 -13 56.7216 9.36173 6
-4 2 13 67.0263 8.55505 5
-4 2 13 72.4238 11.7447 2
3 -2 -13 20.0005 7.56467 2
3 -2 -13 14.0248 5.70855 6
-3 2 13 9.39090 7.29840 2
-3 2 13 9.50387 4.60425 6
8 -3 -13 41.3595 7.34368 6
8 -3 -13 30.6975 8.00352 2
-8 3 13 26.7242 6.40073 6
-8 3 13 23.5819 5.76390 5
-8 3 13 57.4911 11.1927 2
7 -3 -13 368.727 21.5844 6
-7 3 13 396.394 19.7091 5
-7 3 13 364.604 19.4066 6
6 -3 -13 124.906 12.4988 6
-6 3 13 91.2629 10.9330 6
-6 3 13 119.172 14.0590 2
-6 3 13 100.200 10.5850 5
-6 3 13 98.0804 7.82961 4
5 -3 -13 114.442 13.4871 2
5 -3 -13 91.8867 11.3694 6
-5 3 13 106.274 15.3079 2
-5 3 13 96.5927 10.7852 5
-5 3 13 103.524 11.0634 6
4 -3 -13 71.1380 10.1598 6
4 -3 -13 79.2799 13.5438 2
-4 3 13 67.2095 12.5028 2
-4 3 13 46.1890 8.97902 6
-4 3 13 60.4469 8.62383 5
3 -3 -13 57.4183 10.1220 6
3 -3 -13 46.1757 9.90056 2
-3 3 13 39.8872 9.94174 2
-3 3 13 48.9702 8.64519 6
7 -4 -13 4.10203 6.67386 2
7 -4 -13 17.5221 6.08165 6
-7 4 13 11.3400 5.05398 5
-7 4 13 14.8680 4.41808 4
-7 4 13 20.2673 6.71543 6
6 -4 -13 27.0803 7.37475 6
6 -4 -13 29.3215 10.0506 2
-6 4 13 28.6631 6.81490 5
-6 4 13 24.7818 8.14037 2
-6 4 13 35.6045 7.10620 6
5 -4 -13 67.6089 10.2488 6
5 -4 -13 72.7415 12.1007 2
-5 4 13 66.7432 12.0997 2
-5 4 13 54.6793 8.41688 5
-5 4 13 57.1938 8.76201 6
4 -4 -13 149.233 14.0052 6
4 -4 -13 143.424 16.1160 2
-4 4 13 126.152 12.3455 6
-4 4 13 105.730 17.0040 2
-4 4 13 131.189 11.7889 5
0 0 0 0.00 0.00 0
;
_shelx_hkl_checksum 33026
_shelx_res_file
;
TITL m22298 : space group P21/n
m22298.res
created by SHELXL-2019/2 at 12:42:52 on 04-Aug-2023
CELL 0.71073 9.6493 13.0873 10.4634 90.000 117.188 90.000
ZERR 4 0.0007 0.0008 0.0007 0.000 0.002 0.000
LATT 1
SYMM 1/2-X, 1/2+Y, 1/2-Z
SFAC C H CL N O
UNIT 32 64 8 8 8
TEMP -183
SIZE 0.32 0.30 0.22
REM FORM irregular block
REM COLR colourless
L.S. 10
BOND $H
LIST 4
ACTA
CONF
REM Instructions for potential hydrogen bonds:
EQIV $1 -x+1, -y+1, -z+1
HTAB N1 Cl2_$1
EQIV $2 x+1/2, -y+3/2, z+1/2
HTAB N1 Cl1_$2
HTAB N1 O1W
HTAB O1 Cl1
HTAB N2 Cl2
EQIV $3 x+1, y, z
HTAB C5 Cl1_$3
EQIV $4 x+1/2, -y+3/2, z-1/2
HTAB C7 Cl1_$4
HTAB C7 Cl1_$3
EQIV $5 -x+1, -y+1, -z
HTAB C8 Cl2_$5
HTAB C8 O1_$1
HTAB C8 Cl1_$3
EQIV $6 x+1, y, z+1
HTAB O1W Cl2_$6
HTAB O1W Cl1_$6
HTAB
REM Planarity of ring and three attached atoms:
MPLA 9 C1 C2 C3 C4 C5 C6 N1 N2 O1 C7 C8 O1W CL1 CL2
REM Twist of dimethylamino group:
RTAB tors C3 C4 N2 C7
RTAB tors C3 C4 N2 C8
RTAB tors C3 C4 N2 H2N
REM Twist of phenolic OH:
RTAB tors C1 C2 O1 H1O
REM Twist of ammonium group:
RTAB tors C2 C1 N1 H3N1
REM
FMAP 2
PLAN 5
WGHT 0.034000 0.266900
EXTI 0.007802
FVAR 0.86737
N1 4 0.759304 0.613979 0.877042 11.00000 0.01328 0.01544 =
0.01046 0.00046 0.00459 0.00004
H1N1 2 0.719430 0.671184 0.893776 11.00000 0.02201
H2N1 2 0.715061 0.559756 0.890679 11.00000 0.02305
H3N1 2 0.857924 0.613382 0.945885 11.00000 0.02771
C1 1 0.746432 0.615904 0.732836 11.00000 0.01421 0.01148 =
0.01067 -0.00003 0.00561 -0.00035
O1 5 0.478175 0.622009 0.653464 11.00000 0.01035 0.02881 =
0.01273 0.00131 0.00570 0.00186
H1O 2 0.392081 0.632080 0.580490 11.00000 0.03673
CL1 3 0.157129 0.667382 0.423668 11.00000 0.01198 0.01708 =
0.01299 0.00011 0.00449 -0.00068
C2 1 0.596930 0.620720 0.618896 11.00000 0.01208 0.01316 =
0.01364 0.00003 0.00635 0.00016
N2 4 0.687645 0.622365 0.309585 11.00000 0.01189 0.01729 =
0.01117 -0.00086 0.00500 -0.00114
H2N 2 0.584897 0.615421 0.250135 11.00000 0.02072
CL2 3 0.356537 0.597625 0.069801 11.00000 0.01496 0.01780 =
0.01421 0.00050 0.00409 -0.00158
C3 1 0.578441 0.622438 0.478825 11.00000 0.01125 0.01459 =
0.01214 -0.00055 0.00382 0.00023
AFIX 43
H3 2 0.477593 0.625003 0.399057 11.00000 -1.20000
AFIX 0
C4 1 0.710731 0.620315 0.458702 11.00000 0.01489 0.01162 =
0.01080 -0.00026 0.00612 -0.00038
C5 1 0.859950 0.617106 0.571309 11.00000 0.01133 0.01574 =
0.01451 0.00029 0.00620 -0.00018
AFIX 43
H5 2 0.948406 0.616984 0.554007 11.00000 -1.20000
AFIX 0
C6 1 0.876883 0.614063 0.710577 11.00000 0.01079 0.01473 =
0.01277 0.00025 0.00308 -0.00022
AFIX 43
H6 2 0.977827 0.610731 0.790114 11.00000 -1.20000
AFIX 0
C7 1 0.734699 0.722779 0.272117 11.00000 0.01904 0.01739 =
0.01567 0.00438 0.00836 0.00151
AFIX 137
H7A 2 0.699595 0.725867 0.168286 11.00000 -1.50000
H7B 2 0.848358 0.729470 0.323059 11.00000 -1.50000
H7C 2 0.686888 0.778611 0.300525 11.00000 -1.50000
AFIX 0
C8 1 0.765581 0.535613 0.274427 11.00000 0.02269 0.01795 =
0.01917 -0.00387 0.01353 -0.00042
AFIX 137
H8A 2 0.725765 0.531196 0.170044 11.00000 -1.50000
H8B 2 0.743641 0.471597 0.310319 11.00000 -1.50000
H8C 2 0.878337 0.547275 0.319913 11.00000 -1.50000
AFIX 0
O1W 5 1.051179 0.614319 1.098616 11.00000 0.01597 0.04153 =
0.01386 -0.00560 0.00391 -0.00056
H1W1 2 1.074647 0.629549 1.180223 11.00000 0.04137
H2W1 2 1.137449 0.618748 1.094193 11.00000 0.03528
HKLF 4
REM m22298 : space group P21/n
REM wR2 = 0.0632, GooF = S = 1.126, Restrained GooF = 1.126 for all data
REM R1 = 0.0210 for 2505 Fo > 4sig(Fo) and 0.0233 for all 2693 data
REM 158 parameters refined using 0 restraints
END
WGHT 0.0340 0.2669
REM Instructions for potential hydrogen bonds
HTAB N1 Cl1_$2
HTAB N1 Cl2_$1
HTAB N1 O1W
HTAB O1 Cl1
HTAB N2 Cl2
HTAB C5 Cl1_$3
HTAB C7 Cl1_$4
HTAB C7 Cl1_$3
HTAB C8 Cl2_$5
HTAB C8 O1_$1
HTAB C8 Cl1_$3
HTAB O1W Cl1_$6
HTAB O1W Cl2_$6
REM Highest difference peak 0.340, deepest hole -0.218, 1-sigma level 0.042
Q1 1 0.8051 0.6124 0.7153 11.00000 0.05 0.34
Q2 1 0.6511 0.6270 0.4771 11.00000 0.05 0.31
Q3 1 0.8619 0.6172 0.6371 11.00000 0.05 0.30
Q4 1 0.7815 0.6189 0.5180 11.00000 0.05 0.30
Q5 1 0.6738 0.6211 0.6800 11.00000 0.05 0.29
;
_shelx_res_checksum 65537
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -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
_atom_site_disorder_assembly
_atom_site_disorder_group
N N1 0.75930(11) 0.61398(6) 0.87704(9) 0.01338(18) Uani d 1 . .
H H1N1 0.7194(15) 0.6712(11) 0.8938(14) 0.022(3) Uiso d 1 . .
H H2N1 0.7151(15) 0.5598(11) 0.8907(13) 0.023(3) Uiso d 1 . .
H H3N1 0.858(2) 0.6134(10) 0.9459(17) 0.028(4) Uiso d 1 . .
C C1 0.74643(11) 0.61590(6) 0.73284(10) 0.01215(19) Uani d 1 . .
O O1 0.47817(9) 0.62201(5) 0.65346(8) 0.01714(17) Uani d 1 . .
H H1O 0.392(2) 0.6321(11) 0.5805(18) 0.037(4) Uiso d 1 . .
Cl Cl1 0.15713(2) 0.66738(2) 0.42367(2) 0.01449(9) Uani d 1 . .
C C2 0.59693(11) 0.62072(7) 0.61890(11) 0.0128(2) Uani d 1 . .
N N2 0.68764(10) 0.62236(6) 0.30958(9) 0.01355(18) Uani d 1 . .
H H2N 0.5849(17) 0.6154(9) 0.2501(15) 0.021(3) Uiso d 1 . .
Cl Cl2 0.35654(3) 0.59763(2) 0.06980(2) 0.01665(9) Uani d 1 . .
C C3 0.57844(11) 0.62244(7) 0.47882(11) 0.0132(2) Uani d 1 . .
H H3 0.477593 0.625003 0.399057 0.016 Uiso calc 1 . .
C C4 0.71073(12) 0.62031(7) 0.45870(11) 0.0123(2) Uani d 1 . .
C C5 0.85995(11) 0.61711(7) 0.57131(11) 0.0137(2) Uani d 1 . .
H H5 0.948406 0.616984 0.554007 0.016 Uiso calc 1 . .
C C6 0.87688(11) 0.61406(7) 0.71058(11) 0.0136(2) Uani d 1 . .
H H6 0.977827 0.610731 0.790114 0.016 Uiso calc 1 . .
C C7 0.73470(12) 0.72278(8) 0.27212(11) 0.0172(2) Uani d 1 . .
H H7A 0.699595 0.725867 0.168286 0.026 Uiso calc 1 . .
H H7B 0.848358 0.729470 0.323059 0.026 Uiso calc 1 . .
H H7C 0.686888 0.778611 0.300525 0.026 Uiso calc 1 . .
C C8 0.76558(12) 0.53561(8) 0.27443(11) 0.0184(2) Uani d 1 . .
H H8A 0.725765 0.531196 0.170044 0.028 Uiso calc 1 . .
H H8B 0.743641 0.471597 0.310319 0.028 Uiso calc 1 . .
H H8C 0.878337 0.547275 0.319913 0.028 Uiso calc 1 . .
O O1W 1.05118(10) 0.61432(6) 1.09862(9) 0.0249(2) Uani d 1 . .
H H1W1 1.075(2) 0.6295(12) 1.180(2) 0.041(5) Uiso d 1 . .
H H2W1 1.137(2) 0.6187(10) 1.0942(18) 0.035(4) 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 0.0133(4) 0.0154(4) 0.0105(4) 0.0000(3) 0.0046(4) 0.0005(3)
C1 0.0142(5) 0.0115(4) 0.0107(4) -0.0004(3) 0.0056(4) 0.0000(3)
O1 0.0104(4) 0.0288(4) 0.0127(4) 0.0019(3) 0.0057(3) 0.0013(3)
Cl1 0.01198(13) 0.01708(14) 0.01299(13) -0.00068(8) 0.00449(10) 0.00011(8)
C2 0.0121(5) 0.0132(4) 0.0136(5) 0.0002(3) 0.0063(4) 0.0000(3)
N2 0.0119(4) 0.0173(4) 0.0112(4) -0.0011(3) 0.0050(3) -0.0009(3)
Cl2 0.01496(14) 0.01780(14) 0.01421(14) -0.00158(8) 0.00409(10) 0.00050(8)
C3 0.0113(4) 0.0146(5) 0.0121(5) 0.0002(3) 0.0038(4) -0.0006(3)
C4 0.0149(5) 0.0116(4) 0.0108(4) -0.0004(3) 0.0061(4) -0.0003(3)
C5 0.0113(5) 0.0157(5) 0.0145(5) -0.0002(3) 0.0062(4) 0.0003(3)
C6 0.0108(5) 0.0147(5) 0.0128(5) -0.0002(3) 0.0031(4) 0.0002(3)
C7 0.0190(5) 0.0174(5) 0.0157(5) 0.0015(4) 0.0084(4) 0.0044(4)
C8 0.0227(5) 0.0180(5) 0.0192(5) -0.0004(4) 0.0135(4) -0.0039(4)
O1W 0.0160(4) 0.0415(5) 0.0139(4) -0.0006(3) 0.0039(3) -0.0056(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'
Cl Cl 0.1484 0.1585 '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 H1N1 . . 110.3(8) ?
C1 N1 H2N1 . . 111.5(8) ?
H1N1 N1 H2N1 . . 111.2(13) ?
C1 N1 H3N1 . . 113.0(10) ?
H1N1 N1 H3N1 . . 104.1(12) ?
H2N1 N1 H3N1 . . 106.3(12) ?
C6 C1 C2 . . 121.64(9) ?
C6 C1 N1 . . 121.44(9) ?
C2 C1 N1 . . 116.93(9) ?
C2 O1 H1O . . 111.4(11) ?
O1 C2 C1 . . 116.47(9) ?
O1 C2 C3 . . 124.41(9) ?
C1 C2 C3 . . 119.11(9) ?
C4 N2 C8 . . 113.37(8) ?
C4 N2 C7 . . 112.07(7) ?
C8 N2 C7 . . 110.74(8) ?
C4 N2 H2N . . 108.4(9) ?
C8 N2 H2N . . 105.7(8) ?
C7 N2 H2N . . 106.1(8) ?
C4 C3 C2 . . 118.39(9) ?
C4 C3 H3 . . 120.8 ?
C2 C3 H3 . . 120.8 ?
C5 C4 C3 . . 122.95(9) ?
C5 C4 N2 . . 119.86(9) ?
C3 C4 N2 . . 117.19(9) ?
C4 C5 C6 . . 118.14(9) ?
C4 C5 H5 . . 120.9 ?
C6 C5 H5 . . 120.9 ?
C1 C6 C5 . . 119.76(9) ?
C1 C6 H6 . . 120.1 ?
C5 C6 H6 . . 120.1 ?
N2 C7 H7A . . 109.5 ?
N2 C7 H7B . . 109.5 ?
H7A C7 H7B . . 109.5 ?
N2 C7 H7C . . 109.5 ?
H7A C7 H7C . . 109.5 ?
H7B C7 H7C . . 109.5 ?
N2 C8 H8A . . 109.5 ?
N2 C8 H8B . . 109.5 ?
H8A C8 H8B . . 109.5 ?
N2 C8 H8C . . 109.5 ?
H8A C8 H8C . . 109.5 ?
H8B C8 H8C . . 109.5 ?
H1W1 O1W H2W1 . . 103.4(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 . 1.4565(12) ?
N1 H1N1 . 0.895(14) ?
N1 H2N1 . 0.873(14) ?
N1 H3N1 . 0.893(17) ?
C1 C6 . 1.3810(14) ?
C1 C2 . 1.3909(14) ?
O1 C2 . 1.3502(12) ?
O1 H1O . 0.843(18) ?
C2 C3 . 1.3934(14) ?
N2 C4 . 1.4721(12) ?
N2 C8 . 1.4976(12) ?
N2 C7 . 1.4998(12) ?
N2 H2N . 0.903(15) ?
C3 C4 . 1.3857(14) ?
C3 H3 . 0.9500 ?
C4 C5 . 1.3831(14) ?
C5 C6 . 1.3908(14) ?
C5 H5 . 0.9500 ?
C6 H6 . 0.9500 ?
C7 H7A . 0.9800 ?
C7 H7B . 0.9800 ?
C7 H7C . 0.9800 ?
C8 H8A . 0.9800 ?
C8 H8B . 0.9800 ?
C8 H8C . 0.9800 ?
O1W H1W1 . 0.802(19) ?
O1W H2W1 . 0.857(18) ?
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
N1 H2N1 Cl2 3_666 0.873(14) 2.270(14) 3.1299(9) 168.5(12) yes
N1 H1N1 Cl1 4_676 0.895(14) 2.257(14) 3.1364(9) 167.4(12) yes
N1 H3N1 O1W . 0.893(17) 1.819(17) 2.7093(12) 174.4(14) yes
O1 H1O Cl1 . 0.843(18) 2.156(18) 2.9873(8) 168.9(15) yes
N2 H2N Cl2 . 0.903(15) 2.161(15) 3.0467(9) 166.7(12) yes
C5 H5 Cl1 1_655 0.95 2.98 3.8846(10) 160 yes
C7 H7A Cl1 4_675 0.98 2.78 3.6641(10) 151 yes
C7 H7B Cl1 1_655 0.98 2.79 3.7079(11) 156 yes
C8 H8A Cl2 3_665 0.98 2.82 3.6774(10) 147 yes
C8 H8B O1 3_666 0.98 2.64 3.4610(13) 142 yes
C8 H8C Cl1 1_655 0.98 2.87 3.7809(11) 156 yes
O1W H2W1 Cl2 1_656 0.857(18) 2.259(18) 3.1036(9) 168.7(13) yes
O1W H1W1 Cl1 1_656 0.802(19) 2.348(19) 3.1493(9) 176.4(16) 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
C6 C1 C2 O1 . . . . 179.93(8) ?
N1 C1 C2 O1 . . . . -0.70(12) ?
C6 C1 C2 C3 . . . . 0.81(13) ?
N1 C1 C2 C3 . . . . -179.82(8) ?
O1 C2 C3 C4 . . . . -179.70(8) ?
C1 C2 C3 C4 . . . . -0.65(13) ?
C2 C3 C4 C5 . . . . -0.34(13) ?
C2 C3 C4 N2 . . . . -179.91(8) ?
C8 N2 C4 C5 . . . . 55.10(11) ?
C7 N2 C4 C5 . . . . -71.16(11) ?
C8 N2 C4 C3 . . . . -125.32(9) ?
C7 N2 C4 C3 . . . . 108.41(9) ?
C3 C4 C5 C6 . . . . 1.17(13) ?
N2 C4 C5 C6 . . . . -179.27(8) ?
C2 C1 C6 C5 . . . . 0.03(13) ?
N1 C1 C6 C5 . . . . -179.31(8) ?
C4 C5 C6 C1 . . . . -0.99(13) ?
_cod_database_fobs_code 2022844