#------------------------------------------------------------------------------
#$Date: 2024-10-12 04:02:41 +0200 (Sat, 12 Oct 2024) $
#$Revision: 295458 $
#$URL: svn://www.crystallography.net/cod/cif/2/02/32/2023281.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_2023281
loop_
_publ_author_name
'Marmande, Mary Helene'
'Baxter, Bailey N.'
'Zeller, Matthias'
'Forbes, David C.'
_publ_section_title
;
N,N′-Dibenzylethylenediammonium dichloride
;
_journal_coeditor_code YY2013
_journal_issue 11
_journal_name_full
'Acta Crystallographica Section E Crystallographic Communications'
_journal_paper_doi 10.1107/S205698902400954X
_journal_volume 80
_journal_year 2024
_chemical_formula_iupac 'C16 H22 N2 2+, 2Cl -'
_chemical_formula_moiety 'C16 H22 N2 2+, 2(Cl -)'
_chemical_formula_sum 'C16 H22 Cl2 N2'
_chemical_formula_weight 313.25
_chemical_name_common
;
N,N'-Dibenzylethylenediammonium dichloride
;
_chemical_name_systematic
;
Benzyl[2-(benzylazaniumyl)ethyl]azanium dichloride
;
_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 dual
_atom_sites_solution_secondary difmap
_audit_creation_method SHELXL-2019/3
_cell_angle_alpha 90
_cell_angle_beta 91.111(2)
_cell_angle_gamma 90
_cell_formula_units_Z 4
_cell_length_a 7.1738(4)
_cell_length_b 7.2872(4)
_cell_length_c 32.0348(18)
_cell_measurement_reflns_used 9984
_cell_measurement_temperature 150(2)
_cell_measurement_theta_max 79.9810
_cell_measurement_theta_min 5.5242
_cell_volume 1674.37(16)
_computing_cell_refinement
;
SAINT V8.40B (Bruker, 2022)
;
_computing_data_collection
;
APEX4 v2022.10-1 (Bruker, 2022)
;
_computing_data_reduction
;
SAINT V8.40B (Bruker, 2022)
;
_computing_molecular_graphics
;
Mercury (Macrae et al., 2020)
;
_computing_structure_refinement
;
SHELXL2019/2 (Sheldrick, 2015b),
ShelXle Rev1580 (H\"ubschle et al., 2011)
;
_computing_structure_solution
;
SHELXT (Sheldrick, 2015a)
;
_diffrn_ambient_temperature 150(2)
_diffrn_detector_area_resol_mean 7.4074
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device 'four circle diffractometer'
_diffrn_measurement_device_type 'Bruker AXS D8 Quest'
_diffrn_measurement_method 'omega and phi scans'
_diffrn_radiation_monochromator 'HELIOS multilayer Montel optics'
_diffrn_radiation_type CuK\a
_diffrn_radiation_wavelength 1.54178
_diffrn_reflns_av_R_equivalents 0.0591
_diffrn_reflns_av_unetI/netI 0.0420
_diffrn_reflns_limit_h_max 9
_diffrn_reflns_limit_h_min -9
_diffrn_reflns_limit_k_max 9
_diffrn_reflns_limit_k_min -8
_diffrn_reflns_limit_l_max 40
_diffrn_reflns_limit_l_min -40
_diffrn_reflns_number 38723
_diffrn_reflns_theta_full 67.679
_diffrn_reflns_theta_max 80.423
_diffrn_reflns_theta_min 2.759
_diffrn_source 'I-mu-S 3.0 microsource X-ray tube'
_diffrn_source_current '1.1 mA'
_diffrn_source_voltage '50 kV'
_exptl_absorpt_coefficient_mu 3.411
_exptl_absorpt_correction_T_max 0.7543
_exptl_absorpt_correction_T_min 0.5654
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
(SADABS; Krause et al., 2015)
;
_exptl_crystal_colour colourless
_exptl_crystal_density_diffrn 1.243
_exptl_crystal_description block
_exptl_crystal_F_000 664
_exptl_crystal_size_max 0.190
_exptl_crystal_size_mid 0.180
_exptl_crystal_size_min 0.120
_refine_diff_density_max 0.340
_refine_diff_density_min -0.188
_refine_ls_extinction_coef 0.0023(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method
;
SHELXL2019/2 (Sheldrick, 2015b)
;
_refine_ls_goodness_of_fit_ref 1.075
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 194
_refine_ls_number_reflns 3643
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.075
_refine_ls_R_factor_all 0.0348
_refine_ls_R_factor_gt 0.0325
_refine_ls_shift/su_max 0.002
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0421P)^2^+0.4315P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0937
_refine_ls_wR_factor_ref 0.0952
_reflns_number_gt 3295
_reflns_number_total 3643
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file yy2013.cif
_cod_data_source_block I
_cod_original_sg_symbol_H-M 'P 21/n'
_cod_database_code 2023281
_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 0.563
_shelx_estimated_absorpt_t_max 0.685
_shelx_hkl_file
;
1 0 0 -0.0974 0.28445 19
-1 0 0 0.16419 1.12582 1
-1 0 0 0.07277 0.19090 5
1 0 0 -0.0325 0.20232 3
1 0 0 0.06687 0.20938 5
1 0 0 0.04747 0.38092 17
-2 0 0 6525.08 505.992 1
-3 0 0 -0.0141 0.33238 5
3 0 0 0.02671 0.70422 17
3 0 0 0.25151 0.42945 3
3 0 0 -0.0996 0.63482 19
-3 0 0 1.02991 2.72437 1
4 0 0 106.181 8.53951 11
-4 0 0 100.659 8.49632 11
4 0 0 111.037 9.94080 17
-4 0 0 113.402 11.7225 1
-4 0 0 110.497 9.42890 5
4 0 0 112.523 9.58016 19
-4 0 0 116.777 9.23980 17
5 0 0 0.44997 0.49278 13
-5 0 0 0.24121 0.18044 6
5 0 0 0.08897 0.89427 19
5 0 0 0.14221 0.31447 6
5 0 0 0.31704 1.01595 17
-5 0 0 -0.0776 0.11984 11
-5 0 0 0.24641 0.23182 13
-5 0 0 -0.0102 0.45957 17
-5 0 0 -1.4916 5.73687 1
5 0 0 0.22524 0.20744 11
-5 0 0 -0.0297 0.53721 5
6 0 0 274.387 20.1294 13
6 0 0 229.883 20.0204 6
6 0 0 262.276 19.8689 11
-6 0 0 232.240 19.8827 6
-6 0 0 269.952 20.9783 17
-6 0 0 204.650 25.8749 1
6 0 0 272.596 22.5691 17
-6 0 0 270.264 19.9267 13
-7 0 0 0.41338 0.63850 17
7 0 0 -0.0801 0.29172 11
-7 0 0 -0.1557 0.22137 13
-7 0 0 -0.0235 0.15792 6
7 0 0 0.15875 0.32754 6
-7 0 0 -7.9118 13.5289 1
7 0 0 -0.9849 1.37488 17
7 0 0 -0.2723 0.45254 13
-8 0 0 102.778 7.92498 7
-8 0 0 95.8228 8.03059 13
8 0 0 118.759 8.09794 6
-8 0 0 94.5634 8.10674 15
8 0 0 94.3404 8.05668 13
-9 0 0 0.02643 0.10802 13
0 -1 0 0.32396 0.22276 5
0 1 0 0.07135 0.43060 1
0 1 0 -0.0191 0.10739 8
-1 -1 0 14.6737 1.25556 17
1 -1 0 14.7747 1.35662 17
1 -1 0 13.0176 1.15814 19
-1 -1 0 10.0872 1.36460 5
1 1 0 11.0458 1.44749 5
1 1 0 18.0440 1.61954 19
1 1 0 10.0549 1.11522 8
-1 1 0 6.84705 1.56882 1
-1 1 0 14.5414 1.15092 17
-1 1 0 13.2295 1.04890 8
-2 -1 0 104.888 9.69005 1
2 -1 0 99.3080 8.27056 3
2 -1 0 99.9279 8.32120 19
2 -1 0 103.973 8.63306 17
-2 -1 0 106.379 8.38770 17
-2 -1 0 102.436 8.67164 5
2 -1 0 107.569 8.31097 5
-2 1 0 102.781 8.27650 17
-2 1 0 101.362 8.03623 8
-2 1 0 106.725 8.26972 5
-2 1 0 109.539 9.03948 1
2 1 0 101.740 8.62925 19
2 1 0 98.0276 8.64976 17
-3 -1 0 41.9790 4.42289 5
-3 -1 0 31.3441 6.24417 1
3 -1 0 55.8891 4.34264 19
-3 -1 0 60.0382 5.19132 17
3 -1 0 38.8511 4.00544 3
3 -1 0 41.6882 4.13002 5
3 -1 0 53.2851 4.76853 17
-3 1 0 43.2486 4.04019 5
-3 1 0 37.0948 5.26835 1
-3 1 0 51.0074 4.26483 17
3 1 0 54.0798 4.66961 19
4 -1 0 0.04388 0.79103 17
-4 -1 0 1.15041 0.16394 11
4 -1 0 2.42254 0.74501 3
-4 -1 0 0.13161 5.25715 1
-4 -1 0 2.73684 0.93592 5
-4 -1 0 -0.1427 0.39199 17
4 -1 0 0.82847 0.22552 11
4 -1 0 0.02141 0.71943 19
4 1 0 0.96716 0.23524 11
4 1 0 0.43551 0.91391 17
-4 1 0 7.89818 3.49071 1
-4 1 0 0.52610 0.46234 17
4 1 0 -0.1788 0.89002 19
-4 1 0 2.78582 0.76200 5
5 -1 0 0.46926 0.67205 13
5 -1 0 2.46550 1.29731 19
5 -1 0 0.84357 0.37893 6
-5 -1 0 -7.3224 8.79677 1
5 -1 0 1.09184 0.28243 11
-5 -1 0 0.93141 0.24940 6
-5 -1 0 0.99483 0.17863 11
-5 -1 0 0.62648 0.78734 5
5 -1 0 2.05002 1.55103 17
-5 -1 0 1.36233 0.78884 17
-5 -1 0 1.49870 0.34195 13
5 1 0 1.09187 1.30393 17
5 1 0 0.78269 0.37905 6
-5 1 0 0.78123 0.22780 6
-5 1 0 1.30304 0.28358 13
-5 1 0 2.84158 0.89030 17
5 1 0 1.23153 0.57647 13
-5 1 0 0.90066 4.31211 1
6 -1 0 1.05849 0.30323 11
-6 -1 0 0.71590 0.31047 13
6 -1 0 -0.0321 0.59604 13
-6 -1 0 0.78765 0.16067 11
6 -1 0 0.34141 1.30725 17
-6 -1 0 0.63326 0.23873 6
-6 -1 0 0.44128 14.2967 1
6 -1 0 0.49605 0.36350 6
-6 -1 0 0.36300 0.60516 17
-6 1 0 0.62137 0.65876 17
-6 1 0 2.00001 6.52120 1
6 1 0 1.40692 0.60182 13
-6 1 0 0.83826 0.23468 6
-6 1 0 0.71403 0.28914 13
6 1 0 0.71656 0.39103 6
6 1 0 0.31090 1.28987 17
7 -1 0 4.95539 2.59479 17
7 -1 0 8.71979 1.00593 6
-7 -1 0 7.98100 2.65410 17
7 -1 0 7.38897 0.78533 11
-7 -1 0 7.88127 0.83032 13
7 -1 0 7.17957 1.09236 13
-7 -1 0 7.65415 0.78932 6
-7 1 0 8.05981 0.82725 13
-7 1 0 8.12636 1.58927 17
-7 1 0 8.12412 1.22631 15
7 1 0 8.23497 0.96633 6
-7 1 0 3.35446 9.54161 1
7 1 0 8.16188 1.07793 13
8 -1 0 0.76496 0.49883 6
-8 -1 0 0.61025 0.17342 7
-8 -1 0 0.85844 0.25775 13
8 -1 0 1.32560 0.53699 13
-8 -1 0 0.52580 0.16424 6
-8 1 0 0.68128 0.19889 7
8 1 0 0.59898 0.39741 13
-8 1 0 0.89409 0.26420 13
-8 1 0 1.42672 0.51302 15
8 1 0 0.50153 0.26269 6
-9 -1 0 10.1099 0.87474 13
9 1 0 9.94992 1.47598 21
-9 1 0 11.1502 0.86782 13
0 2 0 9999.99 774.215 1
-1 -2 0 21.3066 1.93520 17
1 -2 0 21.0194 1.90001 3
-1 -2 0 21.4818 2.29776 5
1 -2 0 20.0771 1.91645 17
1 2 0 23.3637 1.84572 8
-1 2 0 23.0259 1.76995 8
1 2 0 22.6460 3.20301 1
1 2 0 20.3045 1.93399 17
-1 2 0 20.2334 2.42141 1
-1 2 0 23.4442 2.25850 1
1 2 0 20.0589 1.97847 17
-2 2 0 2066.33 164.055 1
-2 2 0 2147.92 163.861 1
3 -2 0 18.6169 2.03952 19
3 -2 0 19.7183 2.55412 17
-3 -2 0 16.1932 7.71156 1
-3 -2 0 17.7874 2.45213 5
-3 -2 0 16.8882 1.48971 11
-3 -2 0 19.2024 2.09583 17
3 -2 0 16.9773 1.87374 3
-3 2 0 9.79961 7.86610 1
-3 2 0 15.9196 3.08602 1
3 2 0 21.2789 2.62343 17
-3 2 0 21.4146 1.85217 17
4 -2 0 6.32819 1.78976 17
-4 -2 0 5.04750 0.49142 11
-4 -2 0 4.59548 1.45727 5
-4 -2 0 4.61356 0.58309 6
4 -2 0 5.08867 1.04490 3
-4 -2 0 4.52024 1.14233 17
4 -2 0 5.11502 0.55126 11
-4 -2 0 4.44136 11.9112 1
4 -2 0 5.41573 1.31075 19
-4 2 0 5.49022 2.85231 1
-4 2 0 5.60661 0.96720 17
4 2 0 5.49861 0.81684 13
4 2 0 6.19570 1.81055 17
-4 2 0 6.72600 0.59972 13
-5 -2 0 41.8847 4.41849 17
-5 -2 0 41.7952 3.53518 13
-5 -2 0 49.3132 5.44228 5
-5 -2 0 44.2712 3.42135 11
5 -2 0 41.6446 5.31729 17
5 -2 0 44.1962 3.65435 6
5 -2 0 41.2092 4.56299 19
5 -2 0 45.1253 3.47803 11
-5 -2 0 42.2709 3.50624 6
5 2 0 36.7227 3.48104 9
5 2 0 43.9756 3.69137 13
-5 2 0 44.8544 4.05812 17
5 2 0 42.1903 3.59711 6
-5 2 0 46.7741 3.49976 13
-5 2 0 53.8924 7.61875 1
5 2 0 43.7826 5.26219 17
-6 -2 0 24.5244 2.02924 11
-6 -2 0 28.5247 2.20591 13
-6 -2 0 23.0298 2.12406 6
-6 -2 0 26.3616 3.42870 17
6 -2 0 20.6963 5.97724 17
6 -2 0 23.6155 2.28429 6
6 -2 0 28.2726 2.12912 11
-6 2 0 28.1052 2.14022 13
6 2 0 20.3824 2.10058 9
6 2 0 23.7334 2.23033 6
6 2 0 28.0660 2.39496 13
-6 2 0 20.9291 6.43560 1
-6 2 0 28.4604 2.59251 15
-6 2 0 26.1720 2.66230 17
6 2 0 27.5859 4.40295 17
-7 -2 0 1.18012 0.92861 17
7 -2 0 1.13361 0.42365 6
-7 -2 0 1.13526 0.34116 13
7 -2 0 1.47172 0.32837 11
-7 -2 0 1.26627 0.28460 6
-7 2 0 -3.9322 8.85765 1
-7 2 0 1.37676 0.30048 7
-7 2 0 1.46851 0.65439 15
-7 2 0 1.41759 0.29718 13
7 2 0 1.92305 2.74321 17
7 2 0 1.56524 0.39315 6
7 2 0 1.03453 0.49700 13
8 -2 0 41.1607 3.16103 6
8 -2 0 39.0691 3.03460 11
-8 -2 0 31.4890 3.04874 13
-8 -2 0 38.5252 3.03441 6
-8 2 0 38.3418 3.03694 13
-8 2 0 38.9897 3.04161 7
8 2 0 39.0730 3.16160 13
-8 2 0 38.4436 3.27364 15
-8 2 0 37.4964 2.99213 10
0 -3 0 0.00192 0.29744 5
0 3 0 0.30766 0.25310 8
1 -3 0 10.7155 1.31076 5
-1 -3 0 10.5864 1.70700 5
1 -3 0 13.6510 1.31420 17
-1 -3 0 12.3467 1.26534 17
-1 3 0 11.0251 1.09776 8
1 3 0 11.5253 1.18919 8
1 3 0 8.11697 2.50580 1
-2 -3 0 295.370 21.5324 5
2 -3 0 247.652 20.4232 19
2 -3 0 274.693 20.5010 3
2 -3 0 190.851 20.6003 17
-2 -3 0 259.877 20.6294 17
2 3 0 240.176 20.4331 17
-2 3 0 270.201 20.2054 8
-2 3 0 289.610 20.7870 1
2 3 0 276.822 22.6640 1
-3 -3 0 228.306 18.1396 11
3 -3 0 170.395 18.1412 11
-3 -3 0 258.569 18.9654 17
-3 -3 0 235.131 19.7099 5
3 -3 0 244.337 18.7168 19
3 -3 0 226.207 18.5596 3
3 -3 0 258.734 19.4458 17
-3 3 0 249.441 18.2112 8
-3 3 0 223.153 20.2491 1
3 3 0 244.274 19.0179 17
-3 3 0 237.184 19.2007 1
-4 -3 0 0.15288 0.12157 11
4 -3 0 0.33179 0.19631 11
4 -3 0 0.30969 1.11076 17
-4 -3 0 0.38368 0.57635 17
-4 -3 0 0.42427 0.79091 5
4 -3 0 0.19272 0.38554 6
-4 -3 0 0.43941 0.21646 6
-4 3 0 -1.1856 2.70381 1
-4 3 0 0.04361 0.49385 15
4 3 0 0.42376 0.25467 9
4 3 0 -0.1711 1.00021 18
-4 3 0 -0.0017 0.18133 13
4 3 0 0.71019 0.38716 13
-4 3 0 0.21943 0.30321 12
-4 3 0 17.7953 15.6524 1
4 3 0 0.09097 0.84423 17
4 3 0 0.45355 0.65197 4
5 -3 0 34.4000 4.87730 17
-5 -3 0 33.4313 2.82676 6
5 -3 0 34.2552 2.78429 11
5 -3 0 36.4549 3.07949 6
-5 -3 0 35.3576 3.90250 17
5 -3 0 34.0377 4.67244 19
-5 -3 0 34.7371 2.73291 11
5 3 0 34.5357 2.86205 9
5 3 0 32.6241 4.25826 17
-5 3 0 31.7311 5.70903 1
5 3 0 35.8925 3.00983 13
5 3 0 31.0197 2.85199 6
-5 3 0 36.6615 3.26936 15
-5 3 0 34.4005 2.78009 13
6 -3 0 13.4245 1.18103 6
6 -3 0 6.92402 3.03627 17
-6 -3 0 11.4418 0.96148 6
-6 -3 0 6.28932 1.77009 17
6 -3 0 10.3234 0.93277 11
-6 -3 0 9.91322 0.82714 11
-6 3 0 10.8969 0.93494 7
6 3 0 6.79378 2.17219 17
6 3 0 8.40899 1.16706 13
6 3 0 6.88244 1.94168 20
-6 3 0 14.6684 5.48041 1
-6 3 0 8.30789 0.89111 13
-6 3 0 7.92960 1.36789 15
-7 -3 0 28.4680 2.42115 6
7 -3 0 32.0617 2.41452 11
7 -3 0 31.0588 2.56050 6
-7 -3 0 26.4348 2.44866 13
-7 -3 0 27.8372 2.32119 11
-7 3 0 27.2292 2.75037 15
7 3 0 31.6693 2.58193 13
7 3 0 28.7626 3.52574 20
-7 3 0 33.1834 2.42879 7
-7 3 0 29.8299 2.38389 13
7 3 0 26.4655 3.58980 21
8 -3 0 0.77069 0.25460 11
-8 -3 0 1.40034 0.21645 6
8 -3 0 1.44656 0.32560 6
-8 -3 0 0.83132 0.35426 13
-8 3 0 1.37974 0.23428 7
8 3 0 0.86265 0.31577 13
8 3 0 0.88446 0.82396 21
-8 3 0 1.24831 0.44376 15
0 -4 0 381.791 30.4048 5
0 4 0 375.048 29.5811 8
1 -4 0 12.4890 1.45023 5
-1 -4 0 6.74365 1.19952 17
-1 -4 0 10.7976 1.89231 5
1 -4 0 11.1736 1.35245 3
-1 4 0 9.00920 1.05756 8
-2 -4 0 2.91362 0.32304 11
2 -4 0 1.51075 0.58962 3
-2 -4 0 3.89237 0.93138 17
-2 -4 0 2.20532 1.52875 5
2 -4 0 7.47498 0.97906 19
2 4 0 1.52556 0.80497 4
2 4 0 2.40126 1.20161 21
-2 4 0 3.93996 1.41686 20
-2 4 0 5.58881 1.00807 15
-2 4 0 4.35961 1.35116 18
2 4 0 2.86283 1.32020 20
-2 4 0 2.87789 0.52358 8
-3 -4 0 1.84735 0.24622 11
3 -4 0 2.19137 0.84917 19
3 -4 0 2.21436 0.27033 11
-3 -4 0 2.48402 0.95024 17
-3 -4 0 1.76838 1.08115 5
-3 -4 0 1.67054 0.35872 6
-3 4 0 2.21089 0.73890 15
-3 4 0 1.50871 0.49067 9
3 4 0 1.59135 0.84414 4
-3 4 0 1.49573 0.97996 18
-3 4 0 2.11367 0.35025 7
3 4 0 2.05024 1.03107 18
3 4 0 1.70817 0.96070 16
3 4 0 2.76769 1.36221 20
3 4 0 1.79047 0.43787 13
3 4 0 1.96563 0.40364 9
-3 4 0 2.10718 0.38248 12
3 4 0 1.52728 0.35038 10
3 4 0 1.90728 1.03218 21
-3 4 0 1.99027 1.10930 20
-3 4 0 2.33323 0.58508 8
-4 -4 0 229.688 19.0541 11
4 -4 0 242.193 19.0779 11
-4 -4 0 237.984 19.1444 6
-4 -4 0 226.803 20.2192 17
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3 -1 36 12.6647 0.96443 6
3 1 36 12.2374 0.91674 6
-3 1 -36 10.2203 1.07662 13
-3 1 -36 9.01595 1.11025 14
4 -1 36 0.00086 0.10370 6
-4 -1 -36 0.05468 0.15977 13
-4 1 -36 0.27290 0.22589 14
-4 -2 36 11.3944 0.94733 6
-4 2 36 11.4163 0.98412 13
3 -2 -36 0.01837 0.32374 13
3 -2 -36 0.01174 0.31903 16
-3 -2 36 -0.1405 0.17028 6
-3 2 36 -0.0137 0.14012 13
3 2 -36 -0.3069 0.19852 13
3 2 -36 -0.1263 0.34802 16
3 2 -36 0.04370 0.30442 4
-2 -2 36 28.4641 2.20314 6
2 -2 -36 28.9590 2.23077 6
2 -2 -36 21.5140 2.43180 13
2 2 -36 25.6521 2.24618 13
2 2 -36 29.6106 2.64021 4
2 2 -36 23.9841 2.61416 16
-1 -2 36 -0.0142 0.16767 6
1 -2 -36 0.24754 0.19315 6
-1 -2 36 0.08326 0.13551 11
1 -2 -36 0.06449 0.33669 13
-1 2 36 0.16539 0.23486 12
1 2 -36 -0.0424 0.50323 16
1 2 -36 -0.0739 0.34000 4
1 2 -36 0.00205 0.28041 13
0 -2 -36 27.3336 2.18158 6
0 -2 36 26.9681 2.20176 6
0 -2 36 26.2562 2.12539 11
0 -2 -36 24.5070 2.28605 13
0 2 -36 26.0989 2.22319 13
0 2 36 28.5146 2.22802 6
0 2 -36 27.4722 2.58084 4
0 2 36 25.4543 2.18834 12
0 2 -36 25.8865 2.70193 16
1 -2 36 0.72743 0.22808 6
-1 -2 -36 0.82652 0.21912 6
1 -2 36 0.61012 0.17706 11
-1 -2 -36 0.35007 0.31947 13
-1 2 -36 0.86994 0.44028 4
1 2 36 0.77888 0.18497 6
-1 2 -36 0.67579 0.27136 13
-1 2 -36 0.60775 0.57773 16
-1 2 -36 0.47114 0.39570 14
-2 -2 -36 19.8455 2.07993 14
2 -2 36 29.4960 2.00258 6
-2 -2 -36 26.4952 2.06216 13
2 -2 36 24.8507 1.92342 11
-2 -2 -36 22.9896 2.17251 16
-2 2 -36 20.6251 2.14446 14
-2 2 -36 23.2607 2.20064 16
-2 2 -36 25.1416 2.01303 13
-3 -2 -36 -0.0681 0.25269 14
3 -2 36 0.04488 0.13549 6
-3 -2 -36 -0.3354 0.18474 13
-3 2 -36 0.05115 0.27886 14
3 2 36 0.08362 0.18063 12
-3 3 36 54.9420 5.16769 13
3 3 -36 78.9619 5.72380 4
-2 -3 36 0.76477 0.17619 6
2 -3 -36 0.65719 0.21051 6
2 3 -36 0.66468 0.46042 16
1 -3 -36 58.7376 4.13609 6
1 -3 -36 36.5580 4.24204 13
-1 -3 36 53.7482 4.08606 11
1 3 -36 64.3960 4.55840 4
-1 3 36 45.1651 4.07872 12
1 3 -36 49.2749 4.50785 16
0 -3 -36 0.32921 0.38532 13
0 -3 -36 0.11140 0.16824 6
0 -3 36 0.20737 0.13616 11
0 3 -36 0.51441 0.54135 16
0 3 36 0.26492 0.20789 12
0 3 -36 0.12988 0.41876 4
1 -3 36 9.80516 0.82847 11
-1 -3 -36 8.38190 1.00764 13
-1 -3 -36 11.1433 0.97233 6
1 -3 36 9.63369 0.85723 6
-1 3 -36 7.85078 1.29261 16
1 3 36 10.3544 0.89343 12
2 -3 36 0.06741 0.13330 6
2 3 36 -0.0064 0.17358 12
-2 3 -36 0.45076 0.34453 14
1 -4 -36 8.53826 0.72855 6
1 4 -36 6.15917 0.98827 16
1 4 -36 9.80579 1.24115 4
0 -4 -36 0.48535 0.16134 6
0 4 36 0.76246 0.20635 12
0 4 -36 0.40809 0.39762 16
-1 -4 -36 -0.0148 0.12862 6
1 4 36 -0.0555 0.14531 12
4 0 -37 -0.1152 0.18722 13
-3 0 37 0.66461 0.14445 6
3 0 -37 1.02517 0.48125 13
3 0 -37 0.89694 0.44645 16
3 0 -37 0.51372 0.33536 4
2 0 -37 0.36009 0.31965 13
2 0 -37 0.22439 0.50387 16
-2 0 37 0.02692 0.13539 6
1 0 -37 0.20218 0.52529 16
1 0 -37 -0.3192 0.28419 13
-1 0 37 0.08047 0.16469 6
-1 0 37 -0.0465 0.22332 12
0 0 -37 0.15482 0.29545 13
0 0 37 -0.0904 0.15378 6
0 0 -37 0.02352 0.51402 16
-1 0 -37 1.66668 0.38243 13
-1 0 -37 1.07920 0.57208 16
1 0 37 1.01202 0.24649 6
-2 0 -37 -0.0842 0.43369 16
2 0 37 0.13654 0.16417 6
-2 0 -37 0.13681 0.33098 14
-2 0 -37 -0.1024 0.22822 13
-3 0 -37 1.82614 0.40649 14
3 0 37 2.69015 0.30695 6
-3 0 -37 2.52812 0.35251 13
3 -1 -37 94.8994 9.41304 16
3 -1 -37 129.072 9.36200 13
-3 -1 37 136.303 9.26875 6
3 -1 -37 115.492 9.45319 4
3 1 -37 119.752 9.38330 13
-3 1 37 106.765 9.25555 13
3 1 -37 148.709 9.60837 4
3 1 -37 99.4983 9.45487 16
2 -1 -37 -0.4205 0.27227 13
2 -1 -37 -0.2045 0.38395 16
-2 -1 37 0.00075 0.13624 6
2 1 -37 -0.2821 0.27577 13
-2 1 37 0.01714 0.11917 6
2 1 -37 0.06243 0.32418 4
2 1 -37 0.05877 0.46639 16
1 -1 -37 12.4526 1.27203 13
-1 -1 37 13.8517 1.16131 6
-1 1 37 11.9342 1.11231 12
-1 1 37 13.5060 1.11799 6
1 1 -37 13.8960 1.26379 13
1 1 -37 13.3892 1.54077 4
1 1 -37 13.1472 1.63702 16
0 -1 37 0.09584 0.17043 6
0 -1 -37 -0.4583 0.25205 13
0 1 -37 -0.1216 0.49332 16
0 1 37 -0.0268 0.14867 6
0 1 -37 0.03224 0.27017 13
-1 -1 -37 17.4316 1.70174 13
-1 -1 -37 17.3235 1.96296 16
1 -1 37 20.6576 1.65049 6
-1 1 -37 21.8297 1.94115 4
-1 1 -37 17.5270 2.01658 16
1 1 37 21.1018 1.62389 6
-1 1 -37 18.6460 1.68159 13
-2 -1 -37 -0.1112 0.33687 14
-2 -1 -37 0.03169 0.41292 16
2 -1 37 0.16257 0.15959 6
-2 -1 -37 0.16562 0.23756 13
-2 1 -37 -0.1029 0.20977 13
-2 1 -37 0.20849 0.46305 16
-2 1 -37 0.05125 0.29229 14
-3 -1 -37 11.8408 1.00799 13
3 -1 37 13.8725 0.97387 6
-3 -1 -37 8.63872 1.08349 14
-3 1 -37 9.81995 1.08362 14
-3 1 -37 11.5850 0.94893 13
-3 -2 37 1.88641 0.23819 6
-3 2 37 2.52957 0.27009 13
3 2 -37 1.36218 0.40189 4
-2 -2 37 2.66531 0.33474 6
2 -2 -37 1.94688 0.43901 13
2 2 -37 2.62329 0.65557 4
2 2 -37 2.83795 0.39050 13
2 2 -37 2.83585 0.70962 16
1 -2 -37 0.57528 0.19826 6
1 -2 -37 0.83455 0.50959 13
-1 -2 37 0.52803 0.19147 6
1 2 -37 0.70840 0.44282 4
-1 2 37 0.51128 0.20519 12
1 2 -37 0.84092 0.28623 13
1 2 -37 0.67196 0.56415 16
0 -2 -37 39.1310 3.45594 13
0 -2 -37 41.1613 3.34507 6
0 -2 37 43.9310 3.39112 6
0 -2 37 38.2024 3.32630 11
0 2 -37 45.3476 3.85838 16
0 2 -37 41.3357 3.38749 13
0 2 -37 46.9893 3.75710 4
0 2 37 41.6459 3.37044 12
1 -2 37 0.14919 0.16369 6
-1 2 -37 0.31443 0.47326 16
-1 2 -37 -0.1061 0.30155 4
1 2 37 0.34164 0.22121 12
2 -2 37 2.67128 0.32837 6
-2 -2 -37 2.67003 0.40988 13
2 2 37 2.22632 0.38442 12
-2 2 -37 1.48199 0.49151 14
3 -2 37 0.02398 0.10671 6
-2 -3 37 1.00691 0.18025 6
2 3 -37 1.37572 0.40795 4
2 3 -37 1.00872 0.46199 16
-1 -3 37 11.3229 0.99186 6
1 -3 -37 11.4419 0.99899 6
1 3 -37 12.4729 1.30726 4
1 3 -37 11.9215 1.37755 16
0 -3 37 0.92981 0.19092 6
0 -3 -37 0.95125 0.19731 6
0 3 -37 0.38761 0.45523 16
0 3 -37 0.95098 0.38367 4
0 3 37 0.73347 0.21599 12
1 -3 37 5.81837 0.50997 6
-1 3 -37 3.81366 0.79195 16
1 3 37 5.67186 0.55137 12
2 3 37 0.12652 0.14943 12
3 0 -38 -0.2059 0.21333 13
3 0 -38 0.05606 0.29133 4
2 0 -38 80.4444 5.92410 4
2 0 -38 56.2823 5.81880 16
2 0 -38 63.8091 5.63301 13
-2 0 38 81.6575 5.65939 6
-1 0 38 0.01503 0.13913 6
1 0 -38 -0.1960 0.43694 16
1 0 -38 -0.0374 0.28023 13
0 0 -38 17.7479 1.75760 13
0 0 -38 17.3255 2.06738 16
0 0 38 24.3865 1.70725 6
-1 0 -38 -0.2011 0.24276 13
1 0 38 0.11803 0.15333 6
-1 0 -38 0.10013 0.42173 16
2 0 38 18.0198 1.49368 6
-2 0 -38 18.1388 1.65667 13
3 0 38 0.00377 0.15481 6
-3 0 -38 0.01407 0.21774 13
-3 -1 38 15.5240 1.13922 6
3 1 -38 13.0675 1.32604 4
3 1 -38 12.5609 1.17591 13
2 -1 -38 0.36831 0.30068 13
-2 -1 38 0.68137 0.21353 6
2 -1 -38 0.55559 0.49527 16
2 1 -38 0.96134 0.60632 4
2 1 -38 1.04107 0.31955 13
2 1 -38 0.39434 0.52531 16
1 -1 -38 37.6853 3.49699 13
1 -1 -38 38.6360 3.74641 16
-1 -1 38 46.8556 3.43281 6
1 1 -38 47.9940 3.79019 4
1 1 -38 42.4162 3.48854 13
-1 1 38 45.6017 3.39038 6
1 1 -38 38.8690 3.78562 16
0 -1 38 1.88749 0.28478 6
0 -1 -38 1.26652 0.38314 13
0 -1 -38 1.21078 0.57493 16
0 1 -38 0.69360 0.56608 16
0 1 38 1.06849 0.25345 12
0 1 -38 2.19911 0.57121 4
0 1 -38 1.47261 0.35611 13
0 1 38 1.91249 0.35189 6
-1 -1 -38 20.8644 1.95042 13
1 -1 38 23.3418 1.89556 6
-1 -1 -38 20.8807 2.30795 16
-1 1 -38 22.7371 1.93026 13
-1 1 -38 24.8992 2.12340 4
1 1 38 24.2014 1.87333 6
-2 -1 -38 4.52489 0.58681 13
2 -1 38 5.87408 0.52092 6
-2 1 -38 4.52787 0.54330 13
3 -1 38 0.08121 0.10420 6
-3 -1 -38 0.08009 0.17066 13
3 1 38 0.14887 0.13857 12
2 -2 -38 8.03101 0.96231 16
2 -2 -38 6.92063 0.81474 13
2 2 -38 8.26111 1.01998 16
1 -2 -38 0.37208 0.31505 13
-1 -2 38 1.15705 0.26108 6
1 2 -38 2.11055 0.90298 4
1 2 -38 0.39902 0.49498 16
0 -2 -38 1.02704 0.35144 13
0 2 38 1.44355 0.25425 12
0 2 -38 0.79843 0.56748 16
0 2 -38 1.90526 0.50484 4
-1 -2 -38 0.27334 0.26325 13
1 -2 38 0.51330 0.16381 6
-1 -2 -38 0.46689 0.38020 16
1 2 38 0.25878 0.18901 12
-1 2 -38 0.19253 0.40779 16
-2 -2 -38 5.70830 0.86961 13
2 -2 38 8.93863 0.72387 6
2 2 38 8.60474 0.73948 12
-1 -3 38 116.201 9.10868 6
1 3 -38 102.311 9.30965 16
1 3 -38 131.574 9.54343 4
0 -3 38 0.02808 0.10212 6
0 3 -38 0.21097 0.38491 16
1 3 38 43.6624 3.44823 12
2 0 -39 -0.0100 0.24589 13
2 0 -39 0.46061 0.42216 16
-2 0 39 -0.0489 0.11336 6
2 0 -39 0.15144 0.26886 4
-1 0 39 0.33314 0.13982 6
1 0 -39 0.33238 0.43899 16
1 0 -39 0.81528 0.43405 13
0 0 -39 0.12298 0.25623 13
0 0 -39 0.01473 0.45610 16
-1 0 -39 0.31871 0.39594 16
1 0 39 0.50187 0.16331 6
-1 0 -39 0.15766 0.43305 4
-2 0 -39 -0.1302 0.16678 13
2 0 39 0.16235 0.12072 6
2 -1 -39 -0.2015 0.22862 13
2 -1 -39 0.02276 0.31798 16
-2 -1 39 -0.0111 0.09662 6
2 -1 -39 0.02335 0.23064 4
2 1 -39 0.00863 0.26174 4
2 1 -39 0.05801 0.36288 16
2 1 -39 0.05612 0.19218 13
1 -1 -39 5.06061 0.66326 13
-1 -1 39 5.72689 0.51179 6
1 -1 -39 4.73757 0.90445 16
1 1 -39 5.72083 0.80980 4
1 1 -39 5.24458 0.60064 13
1 1 -39 4.41624 0.88056 16
0 -1 -39 0.12536 0.48578 16
0 -1 39 0.20751 0.22791 6
0 -1 -39 0.18007 0.25334 13
0 1 39 -0.1327 0.27355 12
0 1 -39 -0.0040 0.27818 4
0 1 -39 -0.0908 0.46862 16
0 1 -39 0.07714 0.30883 13
1 -1 39 65.7708 4.36919 6
-1 -1 -39 48.2281 4.53132 16
-1 -1 -39 55.2293 4.40583 13
-1 1 -39 54.7574 4.36249 13
1 1 39 55.7342 4.34779 12
-1 1 -39 50.9119 4.56873 16
-2 -1 -39 0.41782 0.20888 13
2 -1 39 0.51528 0.13385 6
2 1 39 0.00469 0.14423 12
-2 -2 39 14.3499 1.18438 6
2 2 -39 15.1051 1.39694 4
1 -2 -39 0.72446 0.39734 16
-1 -2 39 0.92195 0.16351 6
1 -2 -39 0.31614 0.45686 13
1 2 -39 0.52613 0.42234 16
1 2 -39 0.86423 0.33621 4
0 -2 39 28.1275 1.97811 6
0 -2 -39 20.8516 2.17415 16
0 -2 -39 20.2497 2.17869 13
0 2 -39 21.3410 2.21558 16
0 2 -39 28.5637 2.19957 4
-1 -2 -39 0.00528 0.24186 13
1 -2 39 0.15070 0.11947 6
1 2 39 0.09711 0.24526 12
2 0 -40 101.511 7.93735 13
1 0 -40 0.01371 0.22151 4
-1 0 40 -0.0684 0.10967 6
1 0 -40 -0.0310 0.34437 16
1 0 -40 -0.1562 0.20223 13
0 0 -40 203.200 15.1262 4
0 0 -40 190.230 14.9739 13
0 0 -40 183.528 15.1651 16
0 0 40 190.977 14.9161 6
-1 0 -40 0.47890 0.20397 13
1 0 40 -0.0309 0.11561 6
1 -1 -40 6.38690 0.68760 13
1 -1 -40 4.70097 0.74798 16
-1 -1 40 5.25026 0.48360 6
1 1 -40 5.08802 0.79265 16
1 1 -40 6.16698 0.78667 4
1 1 -40 4.92284 0.62989 13
0 -1 40 1.59641 0.22589 6
0 -1 -40 1.54024 0.45402 16
0 -1 -40 1.92994 0.32913 13
0 1 -40 1.35396 0.44556 4
0 1 -40 1.48909 0.48915 16
-1 -1 -40 1.06748 0.37026 13
0 0 0 0.00 0.00 0
_exptl_absorpt_process_details
)
SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
J. Appl. Cryst. 48 (2015) 3-10
)
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_correction_T_max 0.7543
_exptl_absorpt_correction_T_min 0.5654
_exptl_special_details
)
The following wavelength and cell were deduced by SADABS from the
direction cosines etc. They are given here for emergency use only:
CELL 1.54184 7.173 7.291 32.018 90.014 91.091 90.007
)
;
_shelx_hkl_checksum 83494
_shelx_res_file
;
TITL DCF_04_12_24_0m_a.res in P2(1)/n
DCF_04_12_24_0m.res
created by SHELXL-2019/3 at 09:19:32 on 27-Aug-2024
REM Old TITL DCF_04_12_24_0m in P2(1)/n
REM SHELXT solution in P2(1)/n: R1 0.111, Rweak 0.001, Alpha 0.021
REM 0.649 for 282 systematic absences, Orientation as input
REM Formula found by SHELXT: C16 N2 Cl2
CELL 1.54178 7.1738 7.2872 32.0348 90.000 91.111 90.000
ZERR 4.000 0.0004 0.0004 0.0018 0.000 0.002 0.000
LATT 1
SYMM 1/2-X, 1/2+Y, 1/2-Z
SFAC C H N CL
UNIT 64 88 8 8
TEMP -123.150
SIZE 0.19 0.18 0.12
L.S. 10
BOND $H
CONF
ACTA
LIST 4
FMAP 2
PLAN 20
HTAB
HTAB N1 Cl1
HTAB N1 Cl2
EQIV $1 -x, -y+1, -z+1
HTAB N2 Cl2_$1
EQIV $2 -x+1, -y+2, -z+1
HTAB N2 Cl1_$2
HTAB C1 Cl1_$2
HTAB C1 Cl2_$1
HTAB C2 Cl1
HTAB C2 Cl2
EQIV $3 x-1, y, z
HTAB C3 Cl1_$3
EQIV $4 x, y+1, z
HTAB C3 Cl2_$4
EQIV $5 -x+1, -y+1, -z+1
HTAB C10 Cl1_$5
HTAB C10 Cl2_$5
MPLA C3 > C9
MPLA N1 N2 C1 > C3 C10 C11
MPLA C10 > C16
MPLA N1 N2 C1 > C3 C10 C11
WGHT 0.042100 0.431500
EXTI 0.002293
FVAR 0.47066
CL1 4 0.678340 0.831782 0.559822 11.00000 0.02593 0.02588 =
0.04219 0.00266 -0.00181 -0.00401
CL2 4 0.172994 0.327431 0.559046 11.00000 0.02475 0.02573 =
0.04041 0.00231 0.00017 -0.00358
N1 3 0.260339 0.742821 0.558692 11.00000 0.02366 0.02378 =
0.02416 0.00145 -0.00038 -0.00180
REM AFIX 23
H1C 2 0.383183 0.758373 0.562188 11.00000 -1.20000
H1D 2 0.230686 0.622236 0.561138 11.00000 -1.20000
REM AFIX 0
N2 3 0.247973 0.750552 0.440892 11.00000 0.02178 0.02314 =
0.02327 0.00167 -0.00072 -0.00133
REM AFIX 23
H2C 2 0.128968 0.732015 0.438187 11.00000 -1.20000
H2D 2 0.273295 0.868312 0.438502 11.00000 -1.20000
REM AFIX 0
C1 1 0.203641 0.802134 0.515804 11.00000 0.02854 0.02774 =
0.02346 0.00333 -0.00201 0.00096
AFIX 23
H1A 2 0.231807 0.934128 0.512218 11.00000 -1.20000
H1B 2 0.067652 0.784755 0.511695 11.00000 -1.20000
AFIX 0
C2 1 0.307618 0.690634 0.483556 11.00000 0.02740 0.02753 =
0.02364 0.00354 -0.00230 0.00120
AFIX 23
H2A 2 0.443622 0.708939 0.487384 11.00000 -1.20000
H2B 2 0.280311 0.558490 0.487189 11.00000 -1.20000
AFIX 0
C3 1 0.166240 0.853183 0.591613 11.00000 0.03125 0.02974 =
0.02823 0.00051 0.00176 0.00437
AFIX 23
H3A 2 0.029932 0.851445 0.586173 11.00000 -1.20000
H3B 2 0.208683 0.982172 0.589849 11.00000 -1.20000
AFIX 0
C4 1 0.205887 0.782136 0.635014 11.00000 0.02986 0.02688 =
0.02569 -0.00176 0.00291 0.00269
C5 1 0.089505 0.651889 0.652556 11.00000 0.03640 0.04193 =
0.03391 -0.00206 0.00404 -0.00820
AFIX 43
H5 2 -0.012124 0.603728 0.636570 11.00000 -1.20000
AFIX 0
C6 1 0.120310 0.591472 0.693213 11.00000 0.05289 0.04293 =
0.03628 0.00532 0.01381 -0.00396
AFIX 43
H6 2 0.040482 0.501694 0.704820 11.00000 -1.20000
AFIX 0
C7 1 0.266547 0.661575 0.716751 11.00000 0.05712 0.05003 =
0.02451 0.00096 0.00420 0.01461
AFIX 43
H7 2 0.286901 0.621077 0.744657 11.00000 -1.20000
AFIX 0
C8 1 0.382941 0.790297 0.699747 11.00000 0.04602 0.04919 =
0.03482 -0.00735 -0.00920 0.00141
AFIX 43
H8 2 0.483795 0.838448 0.715983 11.00000 -1.20000
AFIX 0
C9 1 0.353931 0.850416 0.658935 11.00000 0.03684 0.03440 =
0.03588 -0.00163 -0.00062 -0.00525
AFIX 43
H9 2 0.435684 0.938554 0.647356 11.00000 -1.20000
AFIX 0
C10 1 0.340864 0.643650 0.407694 11.00000 0.02869 0.02937 =
0.02626 0.00013 -0.00007 0.00463
AFIX 23
H10A 2 0.298227 0.514629 0.409097 11.00000 -1.20000
H10B 2 0.477090 0.644637 0.413258 11.00000 -1.20000
AFIX 0
C11 1 0.303327 0.715445 0.364267 11.00000 0.02848 0.02404 =
0.02522 -0.00092 0.00075 -0.00345
C12 1 0.153974 0.827263 0.353361 11.00000 0.03832 0.04923 =
0.02590 -0.00030 0.00079 0.01246
AFIX 43
H12 2 0.067446 0.862173 0.373986 11.00000 -1.20000
AFIX 0
C13 1 0.129325 0.889050 0.312477 11.00000 0.04855 0.05142 =
0.02980 0.00258 -0.00550 0.01199
AFIX 43
H13 2 0.028142 0.968187 0.305545 11.00000 -1.20000
AFIX 0
C14 1 0.251418 0.835665 0.282015 11.00000 0.05387 0.04286 =
0.02499 0.00303 -0.00032 -0.00641
AFIX 43
H14 2 0.234239 0.877038 0.254083 11.00000 -1.20000
AFIX 0
C15 1 0.398629 0.721723 0.292456 11.00000 0.05257 0.04764 =
0.03259 -0.00049 0.01530 0.00103
AFIX 43
H15 2 0.481997 0.683011 0.271523 11.00000 -1.20000
AFIX 0
C16 1 0.425585 0.663462 0.333256 11.00000 0.03807 0.03886 =
0.03568 0.00189 0.00939 0.00555
AFIX 43
H16 2 0.528917 0.586997 0.340157 11.00000 -1.20000
AFIX 0
HKLF 4
REM DCF_04_12_24_0m_a.res in P2(1)/n
REM wR2 = 0.0952, GooF = S = 1.075, Restrained GooF = 1.075 for all data
REM R1 = 0.0325 for 3295 Fo > 4sig(Fo) and 0.0348 for all 3643 data
REM 194 parameters refined using 0 restraints
END
WGHT 0.0421 0.4329
REM Instructions for potential hydrogen bonds
HTAB N1 Cl1
HTAB N1 Cl2
HTAB N2 Cl2_$1
HTAB N2 Cl1_$2
HTAB C1 Cl1_$2
HTAB C1 Cl2_$1
HTAB C2 Cl1
HTAB C2 Cl2
HTAB C3 Cl1_$3
HTAB C3 Cl2_$4
HTAB C10 Cl1_$5
HTAB C10 Cl2_$5
REM Highest difference peak 0.340, deepest hole -0.188, 1-sigma level 0.048
Q1 1 0.2523 0.7460 0.4998 11.00000 0.05 0.34
Q2 1 0.3046 0.7755 0.6439 11.00000 0.05 0.31
Q3 1 0.2052 0.7349 0.3557 11.00000 0.05 0.30
Q4 1 0.1697 0.8234 0.2977 11.00000 0.05 0.29
Q5 1 0.2881 0.6974 0.4261 11.00000 0.05 0.29
Q6 1 0.3403 0.6800 0.3494 11.00000 0.05 0.29
Q7 1 0.3149 0.6832 0.3859 11.00000 0.05 0.27
Q8 1 0.3241 0.7059 0.7025 11.00000 0.05 0.27
Q9 1 0.1598 0.3656 0.5834 11.00000 0.05 0.26
Q10 1 0.1683 0.6576 0.7055 11.00000 0.05 0.25
Q11 1 0.6033 0.8368 0.5847 11.00000 0.05 0.25
Q12 1 0.2810 0.7190 0.4613 11.00000 0.05 0.23
Q13 1 0.2194 0.7948 0.5729 11.00000 0.05 0.23
Q14 1 0.2457 0.8386 0.6512 11.00000 0.05 0.23
Q15 1 0.3592 0.8209 0.2929 11.00000 0.05 0.23
Q16 1 0.1953 0.8126 0.6143 11.00000 0.05 0.21
Q17 1 0.2796 0.3333 0.5692 11.00000 0.05 0.21
Q18 1 0.2602 0.3164 0.5383 11.00000 0.05 0.19
Q19 1 0.2195 0.7750 0.5379 11.00000 0.05 0.19
Q20 1 0.1558 0.7171 0.6442 11.00000 0.05 0.19
;
_shelx_res_checksum 58859
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
Cl Cl1 0.67834(4) 0.83178(4) 0.55982(2) 0.03137(12) Uani d 1 . .
Cl Cl2 0.17299(4) 0.32743(4) 0.55905(2) 0.03030(11) Uani d 1 . .
N N1 0.26034(13) 0.74282(13) 0.55869(3) 0.0239(2) Uani d 1 . .
H H1C 0.383(2) 0.758(2) 0.5622(4) 0.029 Uiso d 1 . .
H H1D 0.231(2) 0.622(2) 0.5611(4) 0.029 Uiso d 1 . .
N N2 0.24797(13) 0.75055(13) 0.44089(3) 0.0227(2) Uani d 1 . .
H H2C 0.129(2) 0.732(2) 0.4382(4) 0.027 Uiso d 1 . .
H H2D 0.273(2) 0.868(2) 0.4385(4) 0.027 Uiso d 1 . .
C C1 0.20364(17) 0.80213(16) 0.51580(3) 0.0266(2) Uani d 1 . .
H H1A 0.231807 0.934128 0.512218 0.032 Uiso calc 1 . .
H H1B 0.067652 0.784755 0.511695 0.032 Uiso calc 1 . .
C C2 0.30762(16) 0.69063(16) 0.48356(3) 0.0262(2) Uani d 1 . .
H H2A 0.443622 0.708939 0.487384 0.031 Uiso calc 1 . .
H H2B 0.280311 0.558490 0.487189 0.031 Uiso calc 1 . .
C C3 0.16624(18) 0.85318(17) 0.59161(4) 0.0297(3) Uani d 1 . .
H H3A 0.029932 0.851445 0.586173 0.036 Uiso calc 1 . .
H H3B 0.208683 0.982172 0.589849 0.036 Uiso calc 1 . .
C C4 0.20589(16) 0.78214(17) 0.63501(4) 0.0274(2) Uani d 1 . .
C C5 0.08951(19) 0.65189(19) 0.65256(4) 0.0374(3) Uani d 1 . .
H H5 -0.012124 0.603728 0.636570 0.045 Uiso calc 1 . .
C C6 0.1203(2) 0.5915(2) 0.69321(4) 0.0439(3) Uani d 1 . .
H H6 0.040482 0.501694 0.704820 0.053 Uiso calc 1 . .
C C7 0.2665(2) 0.6616(2) 0.71675(4) 0.0438(4) Uani d 1 . .
H H7 0.286901 0.621077 0.744657 0.053 Uiso calc 1 . .
C C8 0.3829(2) 0.7903(2) 0.69975(4) 0.0435(3) Uani d 1 . .
H H8 0.483795 0.838448 0.715983 0.052 Uiso calc 1 . .
C C9 0.35393(18) 0.85042(18) 0.65893(4) 0.0357(3) Uani d 1 . .
H H9 0.435684 0.938554 0.647356 0.043 Uiso calc 1 . .
C C10 0.34086(17) 0.64365(17) 0.40769(4) 0.0281(3) Uani d 1 . .
H H10A 0.298227 0.514629 0.409097 0.034 Uiso calc 1 . .
H H10B 0.477090 0.644637 0.413258 0.034 Uiso calc 1 . .
C C11 0.30333(16) 0.71545(16) 0.36427(3) 0.0259(2) Uani d 1 . .
C C12 0.15397(19) 0.82726(19) 0.35336(4) 0.0378(3) Uani d 1 . .
H H12 0.067446 0.862173 0.373986 0.045 Uiso calc 1 . .
C C13 0.1293(2) 0.8890(2) 0.31248(4) 0.0433(3) Uani d 1 . .
H H13 0.028142 0.968187 0.305545 0.052 Uiso calc 1 . .
C C14 0.2514(2) 0.83566(19) 0.28202(4) 0.0406(3) Uani d 1 . .
H H14 0.234239 0.877038 0.254083 0.049 Uiso calc 1 . .
C C15 0.3986(2) 0.7217(2) 0.29246(4) 0.0441(3) Uani d 1 . .
H H15 0.481997 0.683011 0.271523 0.053 Uiso calc 1 . .
C C16 0.42558(19) 0.66346(18) 0.33326(4) 0.0374(3) Uani d 1 . .
H H16 0.528917 0.586997 0.340157 0.045 Uiso calc 1 . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
Cl1 0.02593(17) 0.02588(17) 0.04219(19) -0.00401(9) -0.00181(12) 0.00266(10)
Cl2 0.02475(17) 0.02573(17) 0.04041(19) -0.00358(9) 0.00017(12) 0.00231(10)
N1 0.0237(5) 0.0238(5) 0.0242(5) -0.0018(4) -0.0004(3) 0.0014(4)
N2 0.0218(5) 0.0231(5) 0.0233(4) -0.0013(3) -0.0007(3) 0.0017(3)
C1 0.0285(6) 0.0277(5) 0.0235(5) 0.0010(4) -0.0020(4) 0.0033(4)
C2 0.0274(6) 0.0275(6) 0.0236(5) 0.0012(4) -0.0023(4) 0.0035(4)
C3 0.0312(6) 0.0297(6) 0.0282(6) 0.0044(5) 0.0018(5) 0.0005(4)
C4 0.0299(6) 0.0269(5) 0.0257(5) 0.0027(4) 0.0029(4) -0.0018(4)
C5 0.0364(7) 0.0419(7) 0.0339(6) -0.0082(5) 0.0040(5) -0.0021(5)
C6 0.0529(8) 0.0429(8) 0.0363(7) -0.0040(6) 0.0138(6) 0.0053(6)
C7 0.0571(9) 0.0500(9) 0.0245(6) 0.0146(6) 0.0042(6) 0.0010(5)
C8 0.0460(8) 0.0492(8) 0.0348(7) 0.0014(6) -0.0092(6) -0.0074(6)
C9 0.0368(7) 0.0344(6) 0.0359(6) -0.0052(5) -0.0006(5) -0.0016(5)
C10 0.0287(6) 0.0294(6) 0.0263(6) 0.0046(4) -0.0001(4) 0.0001(4)
C11 0.0285(5) 0.0240(5) 0.0252(5) -0.0034(4) 0.0008(4) -0.0009(4)
C12 0.0383(7) 0.0492(8) 0.0259(6) 0.0125(5) 0.0008(5) -0.0003(5)
C13 0.0485(8) 0.0514(8) 0.0298(6) 0.0120(6) -0.0055(5) 0.0026(6)
C14 0.0539(8) 0.0429(8) 0.0250(6) -0.0064(6) -0.0003(5) 0.0030(5)
C15 0.0526(8) 0.0476(8) 0.0326(7) 0.0010(6) 0.0153(6) -0.0005(6)
C16 0.0381(7) 0.0389(7) 0.0357(7) 0.0055(5) 0.0094(5) 0.0019(5)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 '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 C3 . . 112.03(9) ?
C1 N1 H1C . . 109.3(9) ?
C3 N1 H1C . . 107.5(10) ?
C1 N1 H1D . . 107.5(9) ?
C3 N1 H1D . . 110.5(9) ?
H1C N1 H1D . . 110.1(14) ?
C10 N2 C2 . . 112.21(9) ?
C10 N2 H2C . . 107.5(10) ?
C2 N2 H2C . . 108.1(10) ?
C10 N2 H2D . . 110.6(9) ?
C2 N2 H2D . . 108.0(9) ?
H2C N2 H2D . . 110.3(14) ?
N1 C1 C2 . . 110.04(10) ?
N1 C1 H1A . . 109.7 ?
C2 C1 H1A . . 109.7 ?
N1 C1 H1B . . 109.7 ?
C2 C1 H1B . . 109.7 ?
H1A C1 H1B . . 108.2 ?
N2 C2 C1 . . 109.31(10) ?
N2 C2 H2A . . 109.8 ?
C1 C2 H2A . . 109.8 ?
N2 C2 H2B . . 109.8 ?
C1 C2 H2B . . 109.8 ?
H2A C2 H2B . . 108.3 ?
N1 C3 C4 . . 112.71(9) ?
N1 C3 H3A . . 109.1 ?
C4 C3 H3A . . 109.1 ?
N1 C3 H3B . . 109.1 ?
C4 C3 H3B . . 109.1 ?
H3A C3 H3B . . 107.8 ?
C9 C4 C5 . . 118.70(11) ?
C9 C4 C3 . . 120.98(11) ?
C5 C4 C3 . . 120.26(11) ?
C6 C5 C4 . . 120.65(12) ?
C6 C5 H5 . . 119.7 ?
C4 C5 H5 . . 119.7 ?
C7 C6 C5 . . 120.09(13) ?
C7 C6 H6 . . 120.0 ?
C5 C6 H6 . . 120.0 ?
C8 C7 C6 . . 119.84(13) ?
C8 C7 H7 . . 120.1 ?
C6 C7 H7 . . 120.1 ?
C7 C8 C9 . . 120.42(13) ?
C7 C8 H8 . . 119.8 ?
C9 C8 H8 . . 119.8 ?
C4 C9 C8 . . 120.29(12) ?
C4 C9 H9 . . 119.9 ?
C8 C9 H9 . . 119.9 ?
N2 C10 C11 . . 113.85(9) ?
N2 C10 H10A . . 108.8 ?
C11 C10 H10A . . 108.8 ?
N2 C10 H10B . . 108.8 ?
C11 C10 H10B . . 108.8 ?
H10A C10 H10B . . 107.7 ?
C12 C11 C16 . . 118.39(11) ?
C12 C11 C10 . . 124.12(10) ?
C16 C11 C10 . . 117.48(11) ?
C11 C12 C13 . . 120.71(12) ?
C11 C12 H12 . . 119.6 ?
C13 C12 H12 . . 119.6 ?
C14 C13 C12 . . 120.20(13) ?
C14 C13 H13 . . 119.9 ?
C12 C13 H13 . . 119.9 ?
C15 C14 C13 . . 119.45(13) ?
C15 C14 H14 . . 120.3 ?
C13 C14 H14 . . 120.3 ?
C14 C15 C16 . . 120.39(12) ?
C14 C15 H15 . . 119.8 ?
C16 C15 H15 . . 119.8 ?
C15 C16 C11 . . 120.83(12) ?
C15 C16 H16 . . 119.6 ?
C11 C16 H16 . . 119.6 ?
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 . 1.4894(14) ?
N1 C3 . 1.4974(15) ?
N1 H1C . 0.893(16) ?
N1 H1D . 0.908(17) ?
N2 C10 . 1.4864(15) ?
N2 C2 . 1.4897(14) ?
N2 H2C . 0.867(16) ?
N2 H2D . 0.881(17) ?
C1 C2 . 1.5211(18) ?
C1 H1A . 0.9900 ?
C1 H1B . 0.9900 ?
C2 H2A . 0.9900 ?
C2 H2B . 0.9900 ?
C3 C4 . 1.5056(16) ?
C3 H3A . 0.9900 ?
C3 H3B . 0.9900 ?
C4 C9 . 1.3897(17) ?
C4 C5 . 1.3899(17) ?
C5 C6 . 1.3885(19) ?
C5 H5 . 0.9500 ?
C6 C7 . 1.378(2) ?
C6 H6 . 0.9500 ?
C7 C8 . 1.375(2) ?
C7 H7 . 0.9500 ?
C8 C9 . 1.3907(19) ?
C8 H8 . 0.9500 ?
C9 H9 . 0.9500 ?
C10 C11 . 1.5057(16) ?
C10 H10A . 0.9900 ?
C10 H10B . 0.9900 ?
C11 C12 . 1.3854(17) ?
C11 C16 . 1.3905(17) ?
C12 C13 . 1.3930(18) ?
C12 H12 . 0.9500 ?
C13 C14 . 1.380(2) ?
C13 H13 . 0.9500 ?
C14 C15 . 1.379(2) ?
C14 H14 . 0.9500 ?
C15 C16 . 1.3843(19) ?
C15 H15 . 0.9500 ?
C16 H16 . 0.9500 ?
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 H1C Cl1 . 0.893(16) 2.187(16) 3.0675(10) 168.6(13) yes
N1 H1D Cl2 . 0.908(17) 2.189(17) 3.0913(10) 172.7(13) yes
N2 H2C Cl2 3_566 0.867(16) 2.213(16) 3.0730(10) 171.7(13) yes
N2 H2D Cl1 3_676 0.881(17) 2.213(17) 3.0893(10) 172.9(13) yes
C1 H1A Cl1 3_676 0.99 2.95 3.7125(12) 134.5 yes
C1 H1B Cl2 3_566 0.99 2.94 3.7000(12) 134.5 yes
C2 H2A Cl1 . 0.99 2.98 3.7213(12) 132.7 yes
C2 H2B Cl2 . 0.99 2.97 3.7251(12) 134.3 yes
C3 H3A Cl1 1_455 0.99 2.65 3.6296(13) 171.2 yes
C3 H3B Cl2 1_565 0.99 2.71 3.6106(13) 151.0 yes
C10 H10A Cl1 3_666 0.99 2.72 3.6209(13) 151.9 yes
C10 H10B Cl2 3_666 0.99 2.65 3.6329(13) 170.0 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
C3 N1 C1 C2 . . . . 178.09(11) ?
C10 N2 C2 C1 . . . . -178.55(11) ?
N1 C1 C2 N2 . . . . 179.49(8) ?
C1 N1 C3 C4 . . . . 173.85(10) ?
N1 C3 C4 C9 . . . . 92.30(14) ?
N1 C3 C4 C5 . . . . -90.43(14) ?
C9 C4 C5 C6 . . . . 0.14(19) ?
C3 C4 C5 C6 . . . . -177.19(12) ?
C4 C5 C6 C7 . . . . 0.5(2) ?
C5 C6 C7 C8 . . . . -0.6(2) ?
C6 C7 C8 C9 . . . . 0.1(2) ?
C5 C4 C9 C8 . . . . -0.66(19) ?
C3 C4 C9 C8 . . . . 176.65(12) ?
C7 C8 C9 C4 . . . . 0.6(2) ?
C2 N2 C10 C11 . . . . -172.64(10) ?
N2 C10 C11 C12 . . . . -20.36(17) ?
N2 C10 C11 C16 . . . . 160.55(11) ?
C16 C11 C12 C13 . . . . -1.3(2) ?
C10 C11 C12 C13 . . . . 179.62(13) ?
C11 C12 C13 C14 . . . . 1.6(2) ?
C12 C13 C14 C15 . . . . -0.4(2) ?
C13 C14 C15 C16 . . . . -1.0(2) ?
C14 C15 C16 C11 . . . . 1.3(2) ?
C12 C11 C16 C15 . . . . -0.1(2) ?
C10 C11 C16 C15 . . . . 179.03(12) ?