#------------------------------------------------------------------------------
#$Date: 2025-01-18 04:35:13 +0200 (Sat, 18 Jan 2025) $
#$Revision: 297375 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/02/33/2023356.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_2023356
loop_
_publ_author_name
'Smirnov, Daniil E.'
'Morozov, Oleg S.'
'Afanasyeva, Ekaterina S.'
'Avdeev, Viktor V.'
_publ_section_title
;
Synthesis and crystal structures of
4,4′-methylenebis(2,6-diethylaniline) and
4,4′-methylenebis(3-chloro-2,6-diethylaniline)
;
_journal_coeditor_code NY2009
_journal_issue 2
_journal_name_full
'Acta Crystallographica Section E Crystallographic Communications'
_journal_paper_doi 10.1107/S2056989025000234
_journal_volume 81
_journal_year 2025
_chemical_formula_iupac 'C21 H30 N2'
_chemical_formula_moiety 'C21 H30 N2'
_chemical_formula_sum 'C21 H30 N2'
_chemical_formula_weight 310.47
_chemical_name_common
;
4,4'-Methylenebis(2,6-diethylaniline)
;
_chemical_name_systematic
;
4,4'-(Methanediyl)bis(2,6-diethylaniline)
;
_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_primary direct
_atom_sites_solution_secondary difmap
_audit_creation_method SHELXL-2019/3
_cell_angle_alpha 90
_cell_angle_beta 102.4188(11)
_cell_angle_gamma 90
_cell_formula_units_Z 4
_cell_length_a 8.9895(3)
_cell_length_b 11.8589(3)
_cell_length_c 17.6765(5)
_cell_measurement_reflns_used 9874
_cell_measurement_temperature 150(2)
_cell_measurement_theta_max 69.56
_cell_measurement_theta_min 4.52
_cell_volume 1840.32(9)
_computing_cell_refinement
;
APEX3 v.2017.3_0 (Bruker, 2016)
;
_computing_data_collection
;
APEX3 v.2017.3_0 (Bruker, 2016)
;
_computing_data_reduction
;
SAINT v.8.38A (Bruker, 2016)
;
_computing_molecular_graphics
;
Olex2 1.3 (Dolomanov et al., 2009)
;
_computing_publication_material
;
Olex2 1.3 (Dolomanov et al., 2009)
;
_computing_structure_refinement
;
SHELXL2019/3 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT2014/5 (Sheldrick, 2015a)
;
_diffrn_ambient_temperature 150(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type 'Bruker D8 Venture'
_diffrn_measurement_method '\f and \w scans'
_diffrn_radiation_type CuK\a
_diffrn_radiation_wavelength 1.54178
_diffrn_reflns_av_R_equivalents 0.0353
_diffrn_reflns_av_unetI/netI 0.0208
_diffrn_reflns_limit_h_max 10
_diffrn_reflns_limit_h_min -10
_diffrn_reflns_limit_k_max 14
_diffrn_reflns_limit_k_min -14
_diffrn_reflns_limit_l_max 21
_diffrn_reflns_limit_l_min -21
_diffrn_reflns_number 22931
_diffrn_reflns_theta_full 67.679
_diffrn_reflns_theta_max 69.564
_diffrn_reflns_theta_min 4.523
_diffrn_source 'microfocus sealed X-ray tube'
_exptl_absorpt_coefficient_mu 0.490
_exptl_absorpt_correction_T_max 0.7532
_exptl_absorpt_correction_T_min 0.6389
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
(SADABS; Krause et al., 2015)
;
_exptl_crystal_colour colourless
_exptl_crystal_density_diffrn 1.121
_exptl_crystal_description prism
_exptl_crystal_F_000 680
_exptl_crystal_size_max 0.320
_exptl_crystal_size_mid 0.210
_exptl_crystal_size_min 0.130
_refine_diff_density_max 0.507
_refine_diff_density_min -0.327
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.026
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 236
_refine_ls_number_reflns 3455
_refine_ls_number_restraints 1
_refine_ls_restrained_S_all 1.035
_refine_ls_R_factor_all 0.0525
_refine_ls_R_factor_gt 0.0495
_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^)+(0.0668P)^2^+0.8039P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1320
_refine_ls_wR_factor_ref 0.1345
_reflns_number_gt 3212
_reflns_number_total 3455
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file ny2009.cif
_cod_data_source_block 1
_cod_original_sg_symbol_H-M 'P 21/n'
_cod_database_code 2023356
_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 0.859
_shelx_estimated_absorpt_t_max 0.939
_shelx_hkl_file
;
1 0 0 0.82937 0.17718 8
1 0 0 0.19283 0.15757 4
1 0 0 0.30662 1.24510 1
-1 0 0 -0.7968 0.75716 1
-2 0 0 13.1256 2.85434 1
2 0 0 13.2614 0.98778 8
2 0 0 19.9608 4.18657 1
-2 0 0 18.5191 1.00098 4
-3 0 0 -0.1422 3.31709 1
3 0 0 0.40483 0.48058 8
-3 0 0 0.43674 0.34353 4
-4 0 0 355.919 19.1640 1
4 0 0 339.941 11.9319 8
-4 0 0 334.525 11.5117 4
-5 0 0 -6.3141 8.34713 1
-5 0 0 0.55835 0.80827 4
5 0 0 0.30116 0.44570 10
-6 0 0 193.277 22.5878 1
-6 0 0 222.353 8.61832 4
6 0 0 221.414 7.59064 10
6 0 0 213.023 9.31761 8
7 0 0 -0.1175 0.44801 2
7 0 0 -0.5750 0.38392 6
7 0 0 0.31659 0.39045 5
7 0 0 -1.7800 2.32885 8
7 0 0 0.31152 0.34298 7
-7 0 0 0.06898 1.58244 4
7 0 0 -0.0796 0.45890 10
8 0 0 17.8047 1.37358 2
8 0 0 19.4254 1.29192 5
8 0 0 20.9276 1.15744 7
8 0 0 18.3125 1.59863 10
8 0 0 18.5213 1.32788 6
9 0 0 0.56930 0.39329 6
9 0 0 0.18158 0.52827 10
9 0 0 0.15448 0.44710 2
9 0 0 0.18552 0.36180 5
9 0 0 -0.1083 0.27142 7
10 0 0 4.12656 0.47932 5
10 0 0 3.62898 0.76119 6
10 0 0 3.82503 0.52702 2
10 0 0 4.15099 0.71651 10
0 -1 0 2.22223 0.89208 1
0 1 0 -0.6359 0.76990 1
0 1 0 0.05177 0.12438 8
-1 -1 0 748.570 23.5237 4
1 -1 0 734.626 23.6298 8
-1 -1 0 805.968 26.3450 1
1 -1 0 785.564 23.5137 4
1 -1 0 750.054 25.3179 1
1 1 0 778.912 26.4205 1
-1 1 0 711.744 25.2679 1
1 1 0 782.077 23.6806 8
-2 -1 0 5579.96 186.950 1
-2 1 0 5808.77 186.305 1
-2 1 0 6506.43 186.527 1
2 1 0 6016.17 187.694 1
-3 -1 0 661.203 21.5073 4
3 -1 0 661.989 21.6657 8
-3 -1 0 665.688 27.4484 1
3 1 0 680.854 22.2332 8
-3 1 0 712.442 21.4097 4
-3 1 0 650.969 26.2249 1
-4 -1 0 228.670 8.09672 4
4 -1 0 221.717 8.47829 8
-4 -1 0 229.309 15.8634 1
-4 1 0 222.587 15.4659 1
4 1 0 229.637 8.50155 8
-4 1 0 232.332 8.09957 4
5 -1 0 11.7002 1.03846 10
-5 -1 0 8.59381 8.84121 1
-5 -1 0 14.8319 2.57505 4
5 1 0 12.4087 1.02761 10
-5 1 0 15.7247 9.36950 1
5 1 0 12.8703 1.85407 8
-5 1 0 10.1858 1.36785 4
-6 -1 0 101.891 18.6411 1
6 -1 0 117.372 6.29718 8
-6 -1 0 112.950 5.51651 4
6 -1 0 127.347 4.59939 10
6 1 0 114.108 6.11578 8
-6 1 0 116.509 5.53888 4
-6 1 0 173.777 34.8883 1
6 1 0 121.080 4.55384 10
7 -1 0 0.83790 0.49633 2
7 -1 0 0.99869 0.55776 10
7 -1 0 -0.0516 0.45688 5
7 -1 0 0.57724 0.39818 7
7 -1 0 0.57532 0.42863 6
-7 -1 0 1.52515 1.64631 4
7 -1 0 -0.4276 2.12031 8
7 1 0 0.39152 0.39445 5
7 1 0 0.84237 0.63323 3
7 1 0 0.62630 0.46964 6
-7 1 0 0.36465 1.63917 4
7 1 0 0.40171 1.77270 8
7 1 0 0.99075 0.60384 10
7 1 0 0.32023 0.34544 7
7 1 0 0.45088 0.51232 2
8 -1 0 16.6648 1.30460 2
8 -1 0 16.6553 1.03062 7
8 -1 0 15.9007 1.16516 5
8 -1 0 14.8744 1.26110 6
8 -1 0 17.0802 1.53738 10
8 1 0 15.2014 1.25913 6
8 1 0 17.2627 1.21249 5
8 1 0 17.7435 1.53566 10
8 1 0 19.2603 1.35597 2
8 1 0 17.6319 1.06741 7
9 -1 0 0.27527 0.41325 2
9 -1 0 0.36538 0.52199 10
9 -1 0 0.13258 0.29842 7
9 -1 0 0.10600 0.37710 5
9 -1 0 -0.0199 0.35922 6
9 1 0 -0.1378 0.45889 10
9 1 0 -0.2665 0.36179 6
9 1 0 -0.2229 0.27194 7
9 1 0 0.12901 0.35196 5
9 1 0 0.13229 0.39649 2
-10 -1 0 -0.1541 0.46295 7
10 -1 0 -0.1591 0.60317 10
10 -1 0 0.89130 0.34195 6
10 -1 0 0.47215 0.36152 2
10 -1 0 0.92781 0.53760 5
-10 1 0 -0.8467 0.55903 7
10 1 0 -0.2441 0.71551 10
10 1 0 0.41506 0.29970 5
10 1 0 0.77912 0.32819 2
10 1 0 0.28681 0.30393 6
0 -2 0 13.1798 2.38292 1
0 -2 0 13.0607 0.63451 4
0 2 0 16.1409 0.94122 8
0 2 0 10.1465 2.46498 1
1 -2 0 4968.80 151.621 1
-1 -2 0 4981.33 152.764 1
1 2 0 4955.80 153.466 1
-1 2 0 4572.06 151.673 1
-2 -2 0 6728.03 213.672 1
2 -2 0 6723.54 211.972 1
-2 2 0 6979.25 212.559 1
-3 -2 0 4.83014 0.69516 4
-3 -2 0 7.93581 4.66732 1
3 -2 0 7.14668 0.86423 4
3 2 0 5.23473 0.87265 8
-3 2 0 12.3288 4.50836 1
-4 -2 0 764.882 35.2334 1
4 -2 0 831.637 27.0787 8
-4 -2 0 841.531 26.5722 4
-4 2 0 869.199 26.5756 4
4 2 0 832.001 27.0041 8
-4 2 0 814.111 33.9482 1
5 -2 0 7.00536 1.61485 8
5 -2 0 6.34721 0.81963 10
-5 -2 0 6.50068 1.23107 4
-5 -2 0 2.36227 10.1282 1
-5 2 0 5.72794 1.14124 4
-5 2 0 3.79114 9.72821 1
5 2 0 8.26111 0.89398 10
6 -2 0 16.6635 1.17288 6
-6 -2 0 17.5324 16.2746 1
6 -2 0 17.9358 1.33214 10
-6 -2 0 17.8556 2.26747 4
6 -2 0 18.0072 2.76102 8
6 2 0 18.5967 1.37058 10
-6 2 0 12.2061 19.1295 1
6 2 0 17.4480 1.21143 5
-6 2 0 13.6158 1.92998 4
6 2 0 17.7004 2.67349 8
6 2 0 17.7077 1.17361 2
7 -2 0 7.15684 1.06364 10
7 -2 0 5.34612 0.73084 5
-7 -2 0 8.04801 2.09294 4
7 -2 0 5.95389 2.79255 8
7 -2 0 4.75770 0.79603 2
7 -2 0 6.56114 0.87935 6
7 2 0 6.89625 0.95939 10
7 2 0 5.94343 0.85303 2
-7 2 0 5.86215 2.05300 4
7 2 0 5.14398 0.68762 3
7 2 0 5.23014 0.73386 5
7 2 0 5.07216 0.78087 6
7 2 0 4.83515 0.62868 7
7 2 0 1.61461 2.13530 8
8 -2 0 8.58256 1.00881 2
8 -2 0 7.04543 0.90754 6
8 -2 0 7.91526 0.85527 5
8 -2 0 7.21582 0.71083 7
8 -2 0 8.75592 1.21862 10
8 2 0 6.44422 0.75629 7
8 2 0 8.56819 1.23078 10
8 2 0 7.43981 0.88555 5
8 2 0 6.33296 0.88043 2
8 2 0 7.35340 0.79436 3
8 2 0 7.03860 0.89932 6
9 -2 0 88.9842 3.24683 5
9 -2 0 87.5887 3.12543 7
9 -2 0 87.2907 3.45249 2
9 -2 0 91.0785 3.45809 6
9 2 0 86.7646 3.20504 7
9 2 0 85.9504 3.33685 5
9 2 0 88.9700 3.43847 6
9 2 0 87.5134 3.48653 2
9 2 0 91.3850 4.05309 10
10 -2 0 3.26952 0.51784 2
10 -2 0 3.64892 0.73798 10
-10 -2 0 2.91726 0.58084 7
10 -2 0 3.92430 0.54684 6
10 2 0 3.52886 0.49675 2
10 2 0 3.49167 0.50309 6
10 2 0 2.79198 0.62924 10
10 2 0 3.32685 0.44094 5
0 -3 0 0.15175 0.19816 4
0 -3 0 -3.3317 1.81105 1
0 3 0 0.17016 0.39640 8
0 3 0 2.44278 3.92756 1
1 -3 0 3488.95 115.171 1
-1 -3 0 3623.96 116.410 1
-1 3 0 3848.46 115.976 1
-1 3 0 3553.24 111.348 8
-2 -3 0 813.802 31.7017 1
2 -3 0 799.519 25.6466 8
2 -3 0 812.977 25.2424 4
2 -3 0 792.037 30.0478 1
-2 -3 0 794.047 25.2631 4
2 3 0 827.398 25.7084 8
-3 -3 0 61.5468 9.01157 1
3 -3 0 87.3162 3.65680 8
-3 -3 0 70.7992 3.14304 4
3 -3 0 70.7242 3.11750 4
3 3 0 73.7448 3.50481 8
4 -3 0 637.331 21.1671 8
-4 -3 0 588.122 30.4919 1
-4 -3 0 645.252 20.5745 4
4 3 0 624.448 21.0914 8
-4 3 0 653.420 29.7051 1
-4 3 0 631.433 20.5026 4
-5 -3 0 731.309 24.1432 4
5 -3 0 745.340 24.9930 8
-5 -3 0 715.015 37.8777 1
-5 3 0 773.179 24.2014 4
5 3 0 713.478 24.8264 8
-5 3 0 732.177 36.8141 1
6 -3 0 0.31317 1.79698 8
-6 -3 0 1.41461 1.27850 4
6 -3 0 2.74202 0.61910 6
6 -3 0 2.22704 0.67236 2
-6 -3 0 -4.8969 15.5033 1
6 -3 0 1.49286 0.59254 10
6 3 0 2.52119 0.47954 7
6 3 0 2.47625 1.75800 8
6 3 0 1.64533 0.54504 2
6 3 0 1.97070 0.63184 10
6 3 0 2.42965 0.58037 5
-6 3 0 -0.0560 1.35066 4
6 3 0 1.40137 0.48879 6
7 -3 0 6.74130 0.93561 2
7 -3 0 11.1754 3.11292 8
-7 -3 0 6.33243 2.01458 4
7 -3 0 5.34792 0.74980 6
7 -3 0 9.57407 1.04910 5
7 -3 0 4.75738 0.60725 7
7 -3 0 5.82515 1.01294 10
7 3 0 6.36316 0.84011 5
-7 3 0 6.15120 2.38238 4
7 3 0 5.94514 2.83327 8
7 3 0 6.71919 0.84751 6
7 3 0 7.09634 0.76238 7
7 3 0 6.49231 0.87122 2
7 3 0 8.55538 1.13753 10
7 3 0 6.33998 0.71133 3
8 -3 0 18.5813 1.29669 2
8 -3 0 17.1157 1.50551 10
8 -3 0 17.9465 1.26284 6
8 -3 0 17.4269 1.05851 7
8 -3 0 18.7193 1.23003 5
8 3 0 18.2936 1.11418 7
8 3 0 19.9724 1.32712 2
8 3 0 16.2460 1.07483 3
8 3 0 19.4837 1.29430 6
8 3 0 18.5889 1.55754 10
8 3 0 18.4165 1.23537 5
9 -3 0 8.86256 0.88704 6
-9 -3 0 8.07874 0.98987 7
9 -3 0 8.28105 1.10848 10
9 -3 0 7.20012 0.86076 2
9 -3 0 8.07349 0.67545 7
9 3 0 7.61249 0.82752 6
9 3 0 7.92776 0.88742 2
9 3 0 8.35053 1.03726 10
9 3 0 9.33426 0.81418 5
10 -3 0 44.0437 1.93279 2
10 -3 0 41.0494 2.06671 10
10 -3 0 39.9021 1.75879 6
10 3 0 43.8272 1.76812 6
10 3 0 36.1524 1.97949 10
10 3 0 42.9795 1.69015 5
10 3 0 43.1689 1.79399 2
0 -4 0 23.4390 1.14417 4
0 -4 0 23.7382 4.93219 1
0 4 0 20.5517 1.55836 8
-1 -4 0 193.282 12.0088 1
-1 -4 0 194.263 6.44645 4
1 -4 0 192.571 6.43499 4
1 -4 0 200.723 11.3748 1
1 4 0 190.959 7.00156 8
-1 4 0 189.804 6.89930 8
2 -4 0 666.638 20.4581 4
-2 -4 0 616.751 27.7584 1
2 -4 0 619.568 26.2539 1
-2 -4 0 668.119 20.5066 4
2 4 0 644.257 21.0039 8
-2 4 0 641.764 20.9541 8
3 -4 0 326.549 22.6723 1
-3 -4 0 396.700 11.8838 4
3 -4 0 341.778 12.2799 8
-3 -4 0 340.109 20.2943 1
3 -4 0 342.592 11.9853 4
3 4 0 341.141 12.2657 8
-4 -4 0 1140.24 37.4397 4
4 -4 0 1214.18 37.4272 4
-4 -4 0 1190.58 50.2906 1
4 -4 0 1153.86 38.1360 8
4 4 0 1243.49 38.2090 8
-4 4 0 1151.81 47.3818 1
-5 -4 0 34.8528 2.56312 4
5 -4 0 34.8099 3.32013 8
5 -4 0 34.9710 1.90686 10
-5 -4 0 23.5052 12.1859 1
-5 4 0 5.60909 13.3402 1
5 4 0 36.0770 1.89328 10
5 4 0 39.9311 3.31702 8
-6 -4 0 155.855 25.7399 1
6 -4 0 242.335 7.79579 7
-6 -4 0 229.819 9.25963 4
6 -4 0 220.737 7.86445 2
6 -4 0 230.140 11.9187 8
6 -4 0 238.184 8.15663 10
6 4 0 229.940 7.88824 6
6 4 0 225.864 7.69041 7
-6 4 0 249.436 9.36808 4
6 4 0 243.485 7.90891 5
6 4 0 230.807 7.88682 2
6 4 0 241.407 10.3833 8
6 4 0 226.878 8.37302 10
7 -4 0 89.1642 3.38773 7
7 -4 0 89.7807 3.69543 2
7 -4 0 87.7916 7.72300 8
7 -4 0 93.1489 3.89132 10
-7 -4 0 84.4117 6.66065 4
7 -4 0 87.1424 3.54189 5
7 4 0 89.1896 3.42621 3
7 4 0 91.5805 3.84910 10
7 4 0 90.6272 3.62972 5
7 4 0 104.939 4.53038 6
-7 4 0 83.0956 6.20043 4
7 4 0 95.8619 9.43492 8
8 -4 0 2.05181 0.52495 6
8 -4 0 1.84430 0.41665 7
-8 -4 0 2.60223 0.74001 7
8 -4 0 1.54573 0.65738 10
8 -4 0 1.18259 0.58521 2
8 4 0 1.48043 0.50730 5
8 4 0 1.20364 0.69069 10
8 4 0 2.12561 0.54363 6
8 4 0 1.75633 0.56537 2
8 4 0 1.87749 0.47807 3
9 -4 0 10.9161 1.07178 2
-9 -4 0 12.1949 1.07826 7
9 -4 0 10.3592 0.75381 7
9 -4 0 11.5571 0.91973 6
9 -4 0 11.5497 1.29799 10
9 4 0 12.7849 1.33741 10
9 4 0 11.9454 0.96174 2
9 4 0 11.8973 0.93806 6
9 4 0 10.9504 0.87690 5
10 -4 0 39.1112 1.72783 6
10 -4 0 40.9725 2.52697 10
10 4 0 42.3997 1.71069 2
10 4 0 41.3412 1.62386 5
0 -5 0 -0.0876 0.39177 4
0 -5 0 0.31599 4.34373 1
0 5 0 0.70654 0.78551 8
-1 -5 0 21.2711 6.14653 1
-1 -5 0 17.9767 1.35042 4
1 -5 0 17.6241 1.27453 4
1 -5 0 13.9250 4.62524 1
1 5 0 18.9860 1.74804 8
-1 5 0 16.9036 1.87149 8
2 -5 0 110.089 4.25467 4
-2 -5 0 117.005 4.31918 4
-2 -5 0 95.2485 11.3736 1
2 -5 0 93.6478 10.6988 1
2 5 0 116.680 4.90697 8
-2 5 0 110.303 4.86597 8
-3 -5 0 83.0102 3.63400 4
3 -5 0 84.4643 3.68433 4
3 -5 0 78.8778 11.4623 1
-3 -5 0 64.6206 11.3084 1
-3 5 0 83.0224 4.28192 8
3 5 0 86.6981 4.26103 8
-4 -5 0 356.848 25.9425 1
4 -5 0 366.391 12.9738 4
-4 -5 0 389.213 13.1191 4
-4 5 0 394.010 14.0004 8
4 5 0 389.098 13.8487 8
-4 5 0 354.082 25.9253 1
5 -5 0 243.884 10.0028 8
-5 -5 0 225.650 8.16350 7
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-1 3 -19 10.7311 0.63225 9
2 -3 19 1.44226 0.32296 6
2 3 19 1.39621 0.28468 6
6 -4 -19 5.57607 0.45858 9
-6 -4 19 5.85312 0.44541 6
-6 4 19 6.11477 0.64992 2
5 -4 -19 3.90506 0.44129 9
-5 -4 19 3.71312 0.43404 6
5 -4 -19 2.66265 0.37375 5
-5 4 19 4.56573 0.46567 2
-5 4 19 3.57374 0.52758 10
5 4 -19 4.81895 0.44102 9
4 -4 -19 1.49587 0.53829 5
4 -4 -19 1.90530 0.30936 9
-4 -4 19 1.96673 0.33088 6
-4 -4 19 1.72548 0.65101 10
-4 4 19 2.11997 0.49290 10
4 4 -19 1.68332 0.27894 9
-4 4 19 2.44852 0.34132 6
-4 4 19 1.69558 0.33010 2
-3 -4 19 25.3899 1.46384 10
-3 -4 19 26.1275 1.19745 6
-3 4 19 27.7152 1.19519 6
3 4 -19 27.5907 1.24406 9
-3 4 19 25.3449 1.45939 10
-2 -4 19 1.58046 0.59002 10
-2 -4 19 0.66046 0.25439 6
2 4 -19 0.33270 0.23231 9
-2 4 19 0.89860 0.27223 6
1 -4 -19 14.7234 0.82149 9
-1 -4 19 13.5277 1.08543 10
-1 -4 19 13.4930 0.78913 6
-1 4 19 13.2193 0.93614 2
-1 4 19 13.9864 0.78312 6
1 4 -19 17.0559 1.14913 9
-1 4 19 12.0093 1.01959 10
0 -4 19 28.6687 1.23405 6
0 -4 19 29.6873 1.86261 10
0 -4 -19 29.5636 1.23111 9
0 4 19 30.0837 1.22614 6
0 4 -19 28.6445 1.22270 9
0 4 19 24.4238 1.39750 10
0 4 19 30.1309 1.32302 2
1 -4 19 22.2494 1.02095 6
1 4 19 22.7926 1.07187 2
1 4 19 20.2326 0.94988 6
1 4 19 20.4163 1.24519 10
-1 4 -19 22.4575 0.96924 9
5 -5 -19 19.8107 0.92228 9
-5 5 19 20.6826 0.94615 2
5 5 -19 17.7813 0.95074 9
-4 -5 19 -0.0420 0.26609 6
4 -5 -19 0.04193 0.21065 9
4 -5 -19 0.15090 0.28904 5
-4 5 19 0.11068 0.51175 10
-4 5 19 -1.0525 0.53363 6
4 5 -19 0.18507 0.18753 9
-4 5 19 -0.0776 0.21754 2
3 -5 -19 0.17006 0.21554 9
-3 5 19 0.74450 0.27016 2
-3 5 19 -0.1650 0.48055 10
-3 5 19 -0.3084 0.32546 6
3 5 -19 0.06628 0.18494 9
2 -5 -19 13.0715 0.77186 9
-2 -5 19 12.7866 0.77614 6
-2 5 19 13.8738 0.80381 5
-2 5 19 14.8327 0.83528 2
2 5 -19 13.9461 0.75188 9
1 -5 -19 8.98198 0.62141 9
-1 5 19 9.83947 0.68630 2
1 5 -19 9.33413 0.58591 9
-1 5 19 6.99888 0.62230 6
-1 5 19 6.38827 0.80036 10
0 -5 19 40.8623 1.55565 6
0 5 -19 42.2609 1.59906 9
0 5 19 43.0944 1.70126 2
1 -5 19 45.5178 1.78986 6
1 5 19 50.3885 1.80845 2
-1 5 -19 44.3389 1.67045 9
4 -6 -19 0.66674 0.22227 9
4 -6 -19 1.40455 0.29108 5
4 6 -19 1.64314 0.23848 9
-4 6 19 1.02161 0.26127 2
3 -6 -19 2.07791 0.35254 9
-3 6 19 2.85757 0.37135 5
3 6 -19 1.72686 0.26832 9
-3 6 19 2.34557 0.33874 2
2 -6 -19 1.01076 0.26367 9
-2 6 19 1.37036 0.30731 2
2 6 -19 1.25698 0.26338 9
-2 6 19 0.64854 0.32142 5
1 -6 -19 34.9769 1.45780 9
-1 6 19 39.3163 1.55185 2
1 6 -19 40.5026 1.47693 9
0 6 19 2.18308 0.36177 2
-6 0 20 11.3297 0.64411 6
-6 0 20 12.0392 0.84447 10
6 0 -20 9.59561 0.63806 9
-5 0 20 -0.0566 0.18739 6
-5 0 20 -0.1212 0.34168 10
-5 0 20 0.15606 0.32455 2
5 0 -20 -0.2059 0.19766 9
-4 0 20 46.9628 1.86937 6
-4 0 20 46.3203 2.23793 10
4 0 -20 50.5780 1.85644 9
-3 0 20 0.14657 0.22852 6
3 0 -20 0.35157 0.25414 9
-3 0 20 -0.1954 0.36474 10
-3 0 20 0.26999 0.34926 2
-2 0 20 1.58400 0.52291 10
-2 0 20 0.57955 0.36917 2
-1 0 20 0.43117 0.51541 2
-1 0 20 0.28604 0.38039 10
1 0 -20 0.23663 0.19742 9
0 0 20 1.01798 0.41939 10
0 0 20 1.21365 0.26461 6
0 0 -20 1.13392 0.28382 9
1 0 20 0.18311 0.37838 10
1 0 20 0.33630 0.21670 6
-1 0 -20 -0.0831 0.25289 9
-6 -1 20 22.2664 1.17265 10
-6 1 20 23.8451 1.19145 10
-6 1 20 22.2652 0.98612 2
-6 1 20 24.4962 1.25355 6
-5 -1 20 98.0997 3.48438 10
-5 -1 20 94.0773 3.28637 6
5 -1 -20 92.9920 3.24564 9
5 1 -20 95.6641 3.22885 9
-5 1 20 96.3448 3.48862 10
-5 1 20 98.4685 3.29792 6
-4 -1 20 0.28652 0.20692 6
-4 -1 20 0.39354 0.37319 10
4 -1 -20 -0.0764 0.19501 9
-4 1 20 0.12687 0.26395 2
-4 1 20 0.08484 0.19439 6
-4 1 20 -0.1654 0.34341 10
4 1 -20 0.04487 0.20226 9
3 -1 -20 0.54674 0.23181 9
-3 -1 20 0.43596 0.25261 6
-3 -1 20 0.10517 0.45994 10
-3 1 20 0.89638 0.32243 2
-3 1 20 0.49095 0.23914 6
-3 1 20 0.54621 0.39176 10
3 1 -20 0.98728 0.25615 9
-2 -1 20 7.27370 0.82973 6
-2 -1 20 5.89130 0.72101 10
2 -1 -20 5.90036 0.53225 9
-2 1 20 6.09820 0.74012 10
-2 1 20 4.56617 0.57695 2
-2 1 20 5.43234 0.52781 6
2 1 -20 6.75783 0.64219 9
1 -1 -20 4.13305 0.46337 9
-1 -1 20 3.12488 0.40685 6
-1 1 20 2.98298 0.43957 2
-1 1 20 4.09646 0.44673 6
1 1 -20 2.93897 0.36856 9
-1 1 20 3.67537 0.59698 10
0 -1 20 2.16526 0.34595 6
0 -1 20 2.64082 0.52190 10
0 -1 -20 2.47822 0.33177 9
0 1 -20 2.98177 0.35110 9
0 1 20 2.78633 0.48855 10
0 1 20 2.42847 0.33566 6
1 -1 20 1.99170 0.49442 10
-1 -1 -20 1.17836 0.37674 9
1 -1 20 1.95950 0.31829 6
1 1 20 2.25970 0.33963 6
1 1 20 1.71340 0.42674 10
-1 1 -20 1.00520 0.26752 9
-5 -2 20 1.53931 0.51529 10
5 -2 -20 2.51072 0.34862 9
-5 -2 20 2.51917 0.32214 6
-5 2 20 1.80496 0.32602 2
5 2 -20 2.42959 0.35379 9
-5 2 20 1.33639 0.39681 10
-5 2 20 2.40814 0.32265 6
-4 -2 20 4.85878 0.60761 10
4 -2 -20 6.03549 0.49367 9
-4 -2 20 5.34723 0.47368 6
4 2 -20 5.91537 0.46985 9
-4 2 20 5.91074 0.49926 6
-4 2 20 5.86420 0.55410 2
-4 2 20 5.88740 0.69148 10
-3 -2 20 108.815 3.76081 6
3 -2 -20 110.770 3.75927 9
-3 -2 20 105.041 3.92739 10
-3 2 20 107.326 3.74202 6
3 2 -20 106.695 3.71811 9
-3 2 20 124.935 4.66566 10
-3 2 20 106.818 3.75151 2
2 -2 -20 12.5066 0.75182 9
-2 -2 20 12.6900 0.76306 6
-2 -2 20 14.8015 1.02763 10
2 2 -20 13.6806 0.75537 9
-2 2 20 12.8871 0.77515 6
-2 2 20 13.5202 0.80853 2
-1 -2 20 0.62725 0.22870 6
1 -2 -20 0.70271 0.22419 9
-1 -2 20 0.82331 0.43099 10
-1 2 20 1.17833 0.32921 2
-1 2 20 1.06284 0.41489 10
-1 2 20 1.03970 0.25486 6
1 2 -20 1.11122 0.23458 9
0 -2 -20 3.11323 0.35699 9
0 -2 20 2.50842 0.33209 6
0 -2 20 2.96397 0.56075 10
0 2 20 3.33035 0.42787 2
0 2 20 2.94968 0.37638 6
0 2 -20 2.51302 0.32709 9
0 2 20 2.71500 0.49941 10
1 -2 20 1.77153 0.30104 6
1 -2 20 1.53665 0.48564 10
-1 2 -20 0.95403 0.24308 9
1 2 20 1.63140 0.33916 2
1 2 20 1.20805 0.42827 10
1 2 20 1.42099 0.35419 6
5 -3 -20 32.5457 1.39971 9
-5 -3 20 32.7515 1.35560 6
-5 3 20 33.7056 1.59301 10
-5 3 20 33.5518 1.27887 6
5 3 -20 30.5657 1.21534 9
-4 -3 20 17.7567 0.85939 6
4 -3 -20 17.7966 0.88192 9
-4 -3 20 17.6849 1.49473 10
4 3 -20 17.3934 0.82739 9
-4 3 20 17.6949 0.89529 2
-4 3 20 17.5294 0.86423 6
-4 3 20 16.1493 1.03814 10
-3 -3 20 11.5025 0.94506 10
3 -3 -20 10.7371 0.66008 9
-3 -3 20 9.97360 0.65513 6
3 3 -20 11.1251 0.63195 9
-3 3 20 10.5186 0.67030 6
-3 3 20 10.4092 0.70740 2
-3 3 20 10.6039 0.89935 10
-2 -3 20 0.02920 0.19386 6
-2 -3 20 0.52917 0.46745 10
2 -3 -20 0.03241 0.18993 9
-2 3 20 0.06567 0.40020 10
2 3 -20 0.13039 0.18234 9
-2 3 20 0.25559 0.24505 6
-2 3 20 0.13949 0.23854 2
-1 -3 20 2.78629 0.37260 6
-1 -3 20 2.71223 0.53652 10
1 -3 -20 3.75731 0.42438 9
-1 3 20 2.49092 0.51572 10
-1 3 20 2.41806 0.37504 2
-1 3 20 3.75429 0.43067 6
1 3 -20 2.38795 0.32349 9
0 -3 20 7.66066 0.84264 10
0 -3 -20 4.07044 0.44976 9
0 -3 20 5.06478 0.45639 6
0 3 -20 4.09350 0.40742 9
0 3 20 3.92679 0.53589 10
0 3 20 5.93153 0.55142 2
0 3 20 4.46777 0.54995 6
1 -3 20 13.7307 0.67514 6
1 3 20 11.5846 0.64167 6
1 3 20 13.3326 0.71480 2
-4 -4 20 1.39681 0.27176 6
4 -4 -20 1.76079 0.30420 9
4 4 -20 1.47993 0.35393 9
-4 4 20 1.66222 0.30546 2
-4 4 20 1.34397 0.53342 10
3 -4 -20 5.97783 0.49446 9
-3 4 20 6.27368 0.53517 2
-3 4 20 4.64525 0.49418 6
3 4 -20 7.88441 0.49640 9
2 -4 -20 0.97174 0.25357 9
-2 -4 20 1.86620 0.43426 6
-2 4 20 1.12135 0.45956 10
2 4 -20 1.23045 0.25941 9
-2 4 20 1.28967 0.29296 6
-2 4 20 0.74801 0.27187 2
-1 -4 20 10.7523 0.70502 6
1 -4 -20 10.0716 0.77437 9
1 4 -20 9.96906 0.60229 9
-1 4 20 9.98851 0.66661 2
-1 4 20 8.61431 1.07161 10
0 -4 20 6.00204 0.46214 6
0 4 -20 5.90321 0.63485 9
3 -5 -20 -0.0957 0.21508 9
-3 5 20 0.39304 0.25555 2
3 5 -20 0.16120 0.16654 9
2 -5 -20 11.6021 0.76282 9
-2 5 20 13.3350 0.72570 2
2 5 -20 12.0515 0.64722 9
-4 0 21 -0.2423 0.44655 10
4 0 -21 0.12781 0.18950 9
-4 0 21 -0.0324 0.17424 6
-3 0 21 0.43315 0.38347 10
-3 0 21 -0.1190 0.19504 6
3 0 -21 0.06612 0.17465 9
-2 0 21 -0.1627 0.17817 6
-2 0 21 -0.4672 0.37132 10
2 0 -21 0.31131 0.20404 9
-1 0 21 208.164 6.80149 10
-1 0 21 207.867 6.61815 6
1 0 -21 200.821 6.57204 9
4 -1 -21 30.8234 1.26219 9
-4 -1 21 31.3036 1.27759 6
-4 -1 21 30.9405 1.44589 10
-4 1 21 31.9280 1.62225 10
-4 1 21 31.6193 1.27559 6
4 1 -21 34.7922 1.61896 9
-3 -1 21 13.2536 0.71259 6
3 -1 -21 13.0850 0.70077 9
-3 -1 21 11.9988 0.91417 10
-3 1 21 12.4076 0.72354 2
-3 1 21 12.6764 0.89698 10
-3 1 21 12.7623 0.69678 6
3 1 -21 12.8959 0.69581 9
-2 -1 21 59.1945 2.13071 6
-2 -1 21 57.6221 2.30122 10
2 -1 -21 59.3998 2.11554 9
2 1 -21 60.4789 2.11490 9
-2 1 21 57.8688 2.11496 6
-2 1 21 57.0088 2.17338 2
-2 1 21 56.8954 2.31503 10
-1 -1 21 46.0295 2.26052 10
-1 -1 21 44.7467 1.70644 6
-1 1 21 43.8587 1.69052 6
-1 1 21 46.8138 1.90148 10
1 1 -21 44.8701 1.67736 9
-4 2 21 0.25419 0.25010 2
3 -2 -21 27.6556 1.13762 9
-3 -2 21 25.8826 1.32093 10
-3 -2 21 26.0614 1.11043 6
-3 2 21 27.6859 1.11761 2
-3 2 21 24.8862 1.34406 10
3 2 -21 27.5884 1.11246 9
-2 -2 21 23.6039 1.04461 6
2 -2 -21 25.2345 1.05305 9
-2 -2 21 23.2793 1.21708 10
-2 2 21 24.4758 1.23008 6
2 2 -21 25.3557 1.04210 9
-2 2 21 23.2709 1.21148 10
-2 2 21 24.1066 1.04712 2
1 -2 -21 2.65817 0.31709 9
-1 2 21 2.30413 0.58816 10
-1 2 21 2.13379 0.35379 2
-1 2 21 2.18492 0.29435 6
-2 3 21 1.47817 0.30828 2
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 0.7532
_exptl_absorpt_correction_T_min 0.6389
_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 1.54187 8.987 11.860 17.677 90.010 102.393 90.008
)
;
_shelx_hkl_checksum 32923
_shelx_res_file
;
TITL 1_a.res in P2(1)/n
24danza02v2.res
created by SHELXL-2019/3 at 03:50:15 on 15-Dec-2024
REM Old TITL 1 in P2(1)/n
REM SHELXT solution in P2(1)/n
REM R1 0.187, Rweak 0.006, Alpha 0.040, Orientation as input
REM Formula found by SHELXT: C8' N
CELL 1.54178 8.9895 11.8589 17.6765 90 102.4188 90
ZERR 4 0.0003 0.0003 0.0005 0 0.0011 0
LATT 1
SYMM 0.5-X,0.5+Y,0.5-Z
SFAC C H N
UNIT 84 120 8
EQIV $1 +X,1+Y,+Z
SADI C7 C2 C7' C2
L.S. 12
PLAN 6
SIZE 0.32 0.21 0.13
TEMP -123
CONF
HTAB N2 N1_$1
BOND $H
LIST 4
MORE 3
fmap 2
acta
WGHT 0.066800 0.803900
FVAR 0.74669 0.73633
N1 3 0.508013 0.228870 0.443196 11.00000 0.05890 0.03563 =
0.04890 0.00291 0.00018 -0.00717
AFIX 7 0.8800
H1A 2 0.444518 0.203843 0.401577 11.00000 0.07340
H1B 2 0.454778 0.243338 0.478419 11.00000 0.04227
AFIX 0
N2 3 0.763303 1.022203 0.528305 11.00000 0.04799 0.04080 =
0.04108 -0.00374 0.00865 -0.00515
AFIX 7 0.8800
H2A 2 0.702084 1.069094 0.497865 11.00000 -1.20000
H2B 2 0.841893 1.056893 0.557216 11.00000 -1.20000
AFIX 0
C1 1 0.593655 0.323153 0.429820 11.00000 0.04444 0.02762 =
0.03531 0.00408 -0.00003 0.00534
C2 1 0.628142 0.342451 0.356740 11.00000 0.06859 0.03227 =
0.02963 -0.00047 0.00053 0.00497
C3 1 0.717598 0.433841 0.347427 11.00000 0.06590 0.03587 =
0.02569 0.00351 0.01206 0.01202
AFIX 43
H3 2 0.738899 0.447362 0.297852 11.00000 -1.20000
AFIX 0
C4 1 0.777153 0.506168 0.407222 11.00000 0.03477 0.03172 =
0.03094 0.00559 0.00884 0.01175
C5 1 0.743476 0.485299 0.479424 11.00000 0.02840 0.03070 =
0.02636 0.00055 0.00370 0.00865
AFIX 43
H5 2 0.782842 0.534865 0.521151 11.00000 -1.20000
AFIX 0
C6 1 0.654723 0.394911 0.492373 11.00000 0.02927 0.03004 =
0.02769 0.00363 0.00441 0.01005
PART 1
C7 1 0.577986 0.267309 0.286712 21.00000 0.04061 0.03733 =
0.03286 -0.00551 0.00690 0.00573
AFIX 23
H7A 2 0.572874 0.188130 0.303718 21.00000 -1.20000
H7B 2 0.653349 0.271536 0.253388 21.00000 -1.20000
AFIX 0
PART 2
C7' 1 0.493330 0.276875 0.292109 -21.00000 0.08879 0.03907 =
0.03664 -0.00258 0.00324 -0.01847
AFIX 23
H7'A 2 0.522766 0.196888 0.288739 -21.00000 -1.20000
H7'B 2 0.396857 0.278633 0.310534 -21.00000 -1.20000
AFIX 0
PART 1
C8 1 0.421616 0.304076 0.240457 21.00000 0.05608 0.04752 =
0.04456 -0.01272 -0.01120 0.00096
AFIX 137
H8A 2 0.391557 0.255842 0.194700 21.00000 -1.50000
H8B 2 0.426673 0.382675 0.224074 21.00000 -1.50000
H8C 2 0.346445 0.297264 0.272966 21.00000 -1.50000
AFIX 0
PART 2
C8' 1 0.467052 0.327384 0.214038 -21.00000 0.04983 0.04901 =
0.04072 -0.00668 0.00740 -0.00301
AFIX 137
H8'A 2 0.403094 0.276881 0.176766 -21.00000 -1.50000
H8'B 2 0.564933 0.338586 0.199170 -21.00000 -1.50000
H8'C 2 0.415683 0.400219 0.214345 -21.00000 -1.50000
AFIX 0
PART 0
C9 1 0.622891 0.369426 0.571379 11.00000 0.03445 0.04034 =
0.03278 0.00744 0.00988 0.00755
AFIX 23
H9A 2 0.659524 0.292198 0.586402 11.00000 -1.20000
H9B 2 0.511194 0.369814 0.566853 11.00000 -1.20000
AFIX 0
C10 1 0.693983 0.449299 0.636014 11.00000 0.05330 0.05749 =
0.02913 -0.00047 0.01629 0.00857
AFIX 137
H10A 2 0.659453 0.526391 0.622011 11.00000 -1.50000
H10B 2 0.805186 0.445821 0.643944 11.00000 -1.50000
H10C 2 0.663280 0.427331 0.683880 11.00000 -1.50000
AFIX 0
C11 1 0.882893 0.600615 0.395498 11.00000 0.03804 0.04190 =
0.04027 0.00859 0.01515 0.00896
AFIX 23
H11A 2 0.988886 0.577452 0.418229 11.00000 -1.20000
H11B 2 0.874584 0.611130 0.339183 11.00000 -1.20000
AFIX 0
C12 1 0.853179 0.712513 0.430326 11.00000 0.03085 0.03607 =
0.03665 0.00914 0.01143 -0.00005
C13 1 0.731122 0.780015 0.394797 11.00000 0.02954 0.03555 =
0.02917 0.00475 0.00649 -0.00258
AFIX 43
H13 2 0.666330 0.754365 0.348255 11.00000 -1.20000
AFIX 0
C14 1 0.701015 0.883404 0.425086 11.00000 0.03018 0.03393 =
0.03157 0.00665 0.00814 -0.00238
C15 1 0.795795 0.920466 0.495059 11.00000 0.03679 0.03509 =
0.03246 0.00358 0.01120 -0.00641
C16 1 0.918794 0.853066 0.531974 11.00000 0.03341 0.04548 =
0.03225 0.00883 0.00532 -0.00708
C17 1 0.945541 0.750955 0.498556 11.00000 0.03041 0.04342 =
0.03733 0.01276 0.00502 0.00039
AFIX 43
H17 2 1.029684 0.706187 0.523247 11.00000 -1.20000
AFIX 0
C18 1 0.572003 0.958384 0.385049 11.00000 0.03728 0.03649 =
0.04107 0.00516 0.00728 0.00425
AFIX 23
H18A 2 0.615497 1.031988 0.374583 11.00000 -1.20000
H18B 2 0.504104 0.972245 0.421362 11.00000 -1.20000
AFIX 0
C19 1 0.475640 0.914397 0.309542 11.00000 0.04155 0.04979 =
0.04339 0.00775 -0.00095 0.00820
AFIX 137
H19A 2 0.539667 0.904872 0.271582 11.00000 -1.50000
H19B 2 0.394034 0.968336 0.289597 11.00000 -1.50000
H19C 2 0.431041 0.841598 0.318726 11.00000 -1.50000
AFIX 0
C20 1 1.020157 0.886638 0.608610 11.00000 0.04449 0.05866 =
0.03635 0.00619 0.00089 -0.00914
AFIX 23
H20A 2 1.119249 0.847402 0.614784 11.00000 -1.20000
H20B 2 1.039622 0.968796 0.608464 11.00000 -1.20000
AFIX 0
C21 1 0.949238 0.857841 0.676409 11.00000 0.07331 0.07260 =
0.03711 0.00611 0.00908 -0.00958
AFIX 137
H21A 2 0.852117 0.897807 0.671087 11.00000 -1.50000
H21B 2 1.018192 0.880692 0.724765 11.00000 -1.50000
H21C 2 0.931458 0.776368 0.677302 11.00000 -1.50000
AFIX 0
HKLF 4
REM 1_a.res in P2(1)/n
REM wR2 = 0.1345, GooF = S = 1.026, Restrained GooF = 1.035 for all data
REM R1 = 0.0495 for 3212 Fo > 4sig(Fo) and 0.0525 for all 3455 data
REM 236 parameters refined using 1 restraints
END
WGHT 0.0668 0.8039
REM Highest difference peak 0.507, deepest hole -0.327, 1-sigma level 0.039
Q1 1 0.5403 0.3561 0.3610 11.00000 0.05 0.51
Q2 1 1.0864 0.8358 0.6672 11.00000 0.05 0.44
Q3 1 0.6257 0.4323 0.3407 11.00000 0.05 0.33
Q4 1 0.9388 0.9272 0.6239 11.00000 0.05 0.27
Q5 1 0.8930 0.7845 0.5260 11.00000 0.05 0.22
Q6 1 0.8432 0.8754 0.5339 11.00000 0.05 0.21
;
_shelx_res_checksum 2514
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 0.50801(18) 0.22887(12) 0.44320(9) 0.0495(4) Uani d 1 . .
H H1A 0.444518 0.203843 0.401577 0.073(7) Uiso d 1 . .
H H1B 0.454778 0.243338 0.478419 0.042(5) Uiso d 1 . .
N N2 0.76330(16) 1.02220(12) 0.52830(8) 0.0434(3) Uani d 1 . .
H H2A 0.702084 1.069094 0.497865 0.052 Uiso d 1 . .
H H2B 0.841893 1.056893 0.557216 0.052 Uiso d 1 . .
C C1 0.59366(18) 0.32315(12) 0.42982(9) 0.0371(3) Uani d 1 . .
C C2 0.6281(2) 0.34245(13) 0.35674(9) 0.0450(4) Uani d 1 . .
C C3 0.7176(2) 0.43384(13) 0.34743(8) 0.0422(4) Uani d 1 . .
H H3 0.738899 0.447362 0.297852 0.051 Uiso calc 1 . .
C C4 0.77715(16) 0.50617(12) 0.40722(8) 0.0322(3) Uani d 1 . .
C C5 0.74348(15) 0.48530(12) 0.47942(8) 0.0288(3) Uani d 1 . .
H H5 0.782842 0.534865 0.521151 0.035 Uiso calc 1 . .
C C6 0.65472(15) 0.39491(11) 0.49237(8) 0.0293(3) Uani d 1 . .
C C7 0.5780(5) 0.2673(2) 0.28671(14) 0.0371(8) Uani d 0.736(11) A 1
H H7A 0.572874 0.188130 0.303718 0.045 Uiso calc 0.736(11) A 1
H H7B 0.653349 0.271536 0.253388 0.045 Uiso calc 0.736(11) A 1
C C7' 0.493(2) 0.2769(8) 0.2921(5) 0.056(4) Uani d 0.264(11) A 2
H H7'A 0.522766 0.196888 0.288739 0.068 Uiso calc 0.264(11) A 2
H H7'B 0.396857 0.278633 0.310534 0.068 Uiso calc 0.264(11) A 2
C C8 0.4216(5) 0.3041(3) 0.2405(3) 0.0527(11) Uani d 0.736(11) A 1
H H8A 0.391557 0.255842 0.194700 0.079 Uiso calc 0.736(11) A 1
H H8B 0.426673 0.382675 0.224074 0.079 Uiso calc 0.736(11) A 1
H H8C 0.346445 0.297264 0.272966 0.079 Uiso calc 0.736(11) A 1
C C8' 0.4671(12) 0.3274(9) 0.2140(6) 0.047(2) Uani d 0.264(11) A 2
H H8'A 0.403094 0.276881 0.176766 0.070 Uiso calc 0.264(11) A 2
H H8'B 0.564933 0.338586 0.199170 0.070 Uiso calc 0.264(11) A 2
H H8'C 0.415683 0.400219 0.214345 0.070 Uiso calc 0.264(11) A 2
C C9 0.62289(17) 0.36943(13) 0.57138(8) 0.0355(3) Uani d 1 . .
H H9A 0.659524 0.292198 0.586402 0.043 Uiso calc 1 . .
H H9B 0.511194 0.369814 0.566853 0.043 Uiso calc 1 . .
C C10 0.6940(2) 0.44930(16) 0.63601(9) 0.0455(4) Uani d 1 . .
H H10A 0.659453 0.526391 0.622011 0.068 Uiso calc 1 . .
H H10B 0.805186 0.445821 0.643944 0.068 Uiso calc 1 . .
H H10C 0.663280 0.427331 0.683880 0.068 Uiso calc 1 . .
C C11 0.88289(18) 0.60062(13) 0.39550(9) 0.0391(4) Uani d 1 . .
H H11A 0.988886 0.577452 0.418229 0.047 Uiso calc 1 . .
H H11B 0.874584 0.611130 0.339183 0.047 Uiso calc 1 . .
C C12 0.85318(16) 0.71251(12) 0.43033(8) 0.0339(3) Uani d 1 . .
C C13 0.73112(15) 0.78002(12) 0.39480(8) 0.0314(3) Uani d 1 . .
H H13 0.666330 0.754365 0.348255 0.038 Uiso calc 1 . .
C C14 0.70101(16) 0.88340(12) 0.42509(8) 0.0317(3) Uani d 1 . .
C C15 0.79580(17) 0.92047(13) 0.49506(8) 0.0342(3) Uani d 1 . .
C C16 0.91879(17) 0.85307(14) 0.53197(8) 0.0373(3) Uani d 1 . .
C C17 0.94554(16) 0.75095(14) 0.49856(9) 0.0374(3) Uani d 1 . .
H H17 1.029684 0.706187 0.523247 0.045 Uiso calc 1 . .
C C18 0.57200(17) 0.95838(13) 0.38505(9) 0.0385(3) Uani d 1 . .
H H18A 0.615497 1.031988 0.374583 0.046 Uiso calc 1 . .
H H18B 0.504104 0.972245 0.421362 0.046 Uiso calc 1 . .
C C19 0.47564(19) 0.91440(15) 0.30954(10) 0.0464(4) Uani d 1 . .
H H19A 0.539667 0.904872 0.271582 0.070 Uiso calc 1 . .
H H19B 0.394034 0.968336 0.289597 0.070 Uiso calc 1 . .
H H19C 0.431041 0.841598 0.318726 0.070 Uiso calc 1 . .
C C20 1.0202(2) 0.88664(17) 0.60861(9) 0.0477(4) Uani d 1 . .
H H20A 1.119249 0.847402 0.614784 0.057 Uiso calc 1 . .
H H20B 1.039622 0.968796 0.608464 0.057 Uiso calc 1 . .
C C21 0.9492(3) 0.8578(2) 0.67641(11) 0.0614(5) Uani d 1 . .
H H21A 0.852117 0.897807 0.671087 0.092 Uiso calc 1 . .
H H21B 1.018192 0.880692 0.724765 0.092 Uiso calc 1 . .
H H21C 0.931458 0.776368 0.677302 0.092 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
N1 0.0589(9) 0.0356(7) 0.0489(8) -0.0072(6) 0.0002(7) 0.0029(6)
N2 0.0480(8) 0.0408(7) 0.0411(7) -0.0051(6) 0.0087(6) -0.0037(6)
C1 0.0444(8) 0.0276(7) 0.0353(8) 0.0053(6) 0.0000(6) 0.0041(6)
C2 0.0686(11) 0.0323(8) 0.0296(8) 0.0050(7) 0.0005(7) -0.0005(6)
C3 0.0659(10) 0.0359(8) 0.0257(7) 0.0120(7) 0.0121(7) 0.0035(6)
C4 0.0348(7) 0.0317(7) 0.0309(7) 0.0117(6) 0.0088(6) 0.0056(5)
C5 0.0284(6) 0.0307(7) 0.0264(6) 0.0086(5) 0.0037(5) 0.0006(5)
C6 0.0293(7) 0.0300(7) 0.0277(7) 0.0101(5) 0.0044(5) 0.0036(5)
C7 0.0406(18) 0.0373(12) 0.0329(12) 0.0057(11) 0.0069(10) -0.0055(8)
C7' 0.089(10) 0.039(4) 0.037(4) -0.018(5) 0.003(5) -0.003(3)
C8 0.056(2) 0.0475(17) 0.045(2) 0.0010(14) -0.0112(16) -0.0127(15)
C8' 0.050(5) 0.049(4) 0.041(5) -0.003(4) 0.007(3) -0.007(4)
C9 0.0344(7) 0.0403(8) 0.0328(7) 0.0075(6) 0.0099(6) 0.0074(6)
C10 0.0533(9) 0.0575(10) 0.0291(7) 0.0086(8) 0.0163(7) -0.0005(7)
C11 0.0380(8) 0.0419(8) 0.0403(8) 0.0090(6) 0.0151(6) 0.0086(6)
C12 0.0308(7) 0.0361(8) 0.0367(7) 0.0000(6) 0.0114(6) 0.0091(6)
C13 0.0295(7) 0.0355(7) 0.0292(7) -0.0026(5) 0.0065(5) 0.0048(5)
C14 0.0302(7) 0.0339(7) 0.0316(7) -0.0024(6) 0.0081(5) 0.0067(6)
C15 0.0368(7) 0.0351(7) 0.0325(7) -0.0064(6) 0.0112(6) 0.0036(6)
C16 0.0334(7) 0.0455(9) 0.0322(7) -0.0071(6) 0.0053(6) 0.0088(6)
C17 0.0304(7) 0.0434(8) 0.0373(8) 0.0004(6) 0.0050(6) 0.0128(6)
C18 0.0373(8) 0.0365(8) 0.0411(8) 0.0042(6) 0.0073(6) 0.0052(6)
C19 0.0415(8) 0.0498(9) 0.0434(9) 0.0082(7) -0.0010(7) 0.0077(7)
C20 0.0445(9) 0.0587(10) 0.0363(8) -0.0091(8) 0.0009(7) 0.0062(7)
C21 0.0733(13) 0.0726(13) 0.0371(9) -0.0096(11) 0.0091(9) 0.0061(9)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 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'
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 H1A . . 114.1 ?
C1 N1 H1B . . 111.4 ?
H1A N1 H1B . . 107.7 ?
C15 N2 H2A . . 116.6 ?
C15 N2 H2B . . 115.6 ?
H2A N2 H2B . . 112.2 ?
N1 C1 C6 . . 118.89(14) ?
N1 C1 C2 . . 121.28(14) ?
C6 C1 C2 . . 119.68(14) ?
C3 C2 C1 . . 119.02(14) ?
C3 C2 C7 . . 116.33(19) ?
C1 C2 C7 . . 124.6(2) ?
C3 C2 C7' . . 129.8(3) ?
C1 C2 C7' . . 106.3(5) ?
C4 C3 C2 . . 122.54(14) ?
C4 C3 H3 . . 118.7 ?
C2 C3 H3 . . 118.7 ?
C3 C4 C5 . . 117.81(14) ?
C3 C4 C11 . . 120.56(13) ?
C5 C4 C11 . . 121.54(13) ?
C6 C5 C4 . . 122.31(13) ?
C6 C5 H5 . . 118.8 ?
C4 C5 H5 . . 118.8 ?
C5 C6 C1 . . 118.61(13) ?
C5 C6 C9 . . 122.46(13) ?
C1 C6 C9 . . 118.93(13) ?
C2 C7 C8 . . 110.3(3) ?
C2 C7 H7A . . 109.6 ?
C8 C7 H7A . . 109.6 ?
C2 C7 H7B . . 109.6 ?
C8 C7 H7B . . 109.6 ?
H7A C7 H7B . . 108.1 ?
C8' C7' C2 . . 113.4(8) ?
C8' C7' H7'A . . 108.9 ?
C2 C7' H7'A . . 108.9 ?
C8' C7' H7'B . . 108.9 ?
C2 C7' H7'B . . 108.9 ?
H7'A C7' H7'B . . 107.7 ?
C7 C8 H8A . . 109.5 ?
C7 C8 H8B . . 109.5 ?
H8A C8 H8B . . 109.5 ?
C7 C8 H8C . . 109.5 ?
H8A C8 H8C . . 109.5 ?
H8B C8 H8C . . 109.5 ?
C7' C8' H8'A . . 109.5 ?
C7' C8' H8'B . . 109.5 ?
H8'A C8' H8'B . . 109.5 ?
C7' C8' H8'C . . 109.5 ?
H8'A C8' H8'C . . 109.5 ?
H8'B C8' H8'C . . 109.5 ?
C6 C9 C10 . . 115.95(13) ?
C6 C9 H9A . . 108.3 ?
C10 C9 H9A . . 108.3 ?
C6 C9 H9B . . 108.3 ?
C10 C9 H9B . . 108.3 ?
H9A C9 H9B . . 107.4 ?
C9 C10 H10A . . 109.5 ?
C9 C10 H10B . . 109.5 ?
H10A C10 H10B . . 109.5 ?
C9 C10 H10C . . 109.5 ?
H10A C10 H10C . . 109.5 ?
H10B C10 H10C . . 109.5 ?
C12 C11 C4 . . 115.05(12) ?
C12 C11 H11A . . 108.5 ?
C4 C11 H11A . . 108.5 ?
C12 C11 H11B . . 108.5 ?
C4 C11 H11B . . 108.5 ?
H11A C11 H11B . . 107.5 ?
C17 C12 C13 . . 117.99(14) ?
C17 C12 C11 . . 121.21(13) ?
C13 C12 C11 . . 120.79(13) ?
C14 C13 C12 . . 122.25(13) ?
C14 C13 H13 . . 118.9 ?
C12 C13 H13 . . 118.9 ?
C13 C14 C15 . . 118.80(13) ?
C13 C14 C18 . . 122.21(13) ?
C15 C14 C18 . . 118.99(13) ?
N2 C15 C16 . . 120.62(14) ?
N2 C15 C14 . . 119.65(14) ?
C16 C15 C14 . . 119.70(14) ?
C17 C16 C15 . . 119.23(14) ?
C17 C16 C20 . . 118.89(15) ?
C15 C16 C20 . . 121.84(15) ?
C12 C17 C16 . . 122.01(14) ?
C12 C17 H17 . . 119.0 ?
C16 C17 H17 . . 119.0 ?
C14 C18 C19 . . 116.41(13) ?
C14 C18 H18A . . 108.2 ?
C19 C18 H18A . . 108.2 ?
C14 C18 H18B . . 108.2 ?
C19 C18 H18B . . 108.2 ?
H18A C18 H18B . . 107.3 ?
C18 C19 H19A . . 109.5 ?
C18 C19 H19B . . 109.5 ?
H19A C19 H19B . . 109.5 ?
C18 C19 H19C . . 109.5 ?
H19A C19 H19C . . 109.5 ?
H19B C19 H19C . . 109.5 ?
C21 C20 C16 . . 111.99(15) ?
C21 C20 H20A . . 109.2 ?
C16 C20 H20A . . 109.2 ?
C21 C20 H20B . . 109.2 ?
C16 C20 H20B . . 109.2 ?
H20A C20 H20B . . 107.9 ?
C20 C21 H21A . . 109.5 ?
C20 C21 H21B . . 109.5 ?
H21A C21 H21B . . 109.5 ?
C20 C21 H21C . . 109.5 ?
H21A C21 H21C . . 109.5 ?
H21B C21 H21C . . 109.5 ?
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 . 1.406(2) ?
N1 H1A . 0.8801 ?
N1 H1B . 0.8799 ?
N2 C15 . 1.400(2) ?
N2 H2A . 0.8799 ?
N2 H2B . 0.8799 ?
C1 C6 . 1.410(2) ?
C1 C2 . 1.410(2) ?
C2 C3 . 1.380(2) ?
C2 C7 . 1.513(3) ?
C2 C7' . 1.668(9) ?
C3 C4 . 1.377(2) ?
C3 H3 . 0.9500 ?
C4 C5 . 1.3957(19) ?
C4 C11 . 1.512(2) ?
C5 C6 . 1.384(2) ?
C5 H5 . 0.9500 ?
C6 C9 . 1.5151(19) ?
C7 C8 . 1.530(5) ?
C7 H7A . 0.9900 ?
C7 H7B . 0.9900 ?
C7' C8' . 1.476(15) ?
C7' H7'A . 0.9900 ?
C7' H7'B . 0.9900 ?
C8 H8A . 0.9800 ?
C8 H8B . 0.9800 ?
C8 H8C . 0.9800 ?
C8' H8'A . 0.9800 ?
C8' H8'B . 0.9800 ?
C8' H8'C . 0.9800 ?
C9 C10 . 1.516(2) ?
C9 H9A . 0.9900 ?
C9 H9B . 0.9900 ?
C10 H10A . 0.9800 ?
C10 H10B . 0.9800 ?
C10 H10C . 0.9800 ?
C11 C12 . 1.511(2) ?
C11 H11A . 0.9900 ?
C11 H11B . 0.9900 ?
C12 C17 . 1.386(2) ?
C12 C13 . 1.394(2) ?
C13 C14 . 1.388(2) ?
C13 H13 . 0.9500 ?
C14 C15 . 1.413(2) ?
C14 C18 . 1.511(2) ?
C15 C16 . 1.406(2) ?
C16 C17 . 1.391(2) ?
C16 C20 . 1.514(2) ?
C17 H17 . 0.9500 ?
C18 C19 . 1.519(2) ?
C18 H18A . 0.9900 ?
C18 H18B . 0.9900 ?
C19 H19A . 0.9800 ?
C19 H19B . 0.9800 ?
C19 H19C . 0.9800 ?
C20 C21 . 1.513(2) ?
C20 H20A . 0.9900 ?
C20 H20B . 0.9900 ?
C21 H21A . 0.9800 ?
C21 H21B . 0.9800 ?
C21 H21C . 0.9800 ?
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 H2A N1 1_565 0.88 2.62 3.472(2) 164.5 yes
C17 H17 Cg1 3_766 0.95 2.92 3.8568(17) 171 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
N1 C1 C2 C3 . . . . -177.50(15) ?
C6 C1 C2 C3 . . . . -2.0(2) ?
N1 C1 C2 C7 . . . . 0.4(3) ?
C6 C1 C2 C7 . . . . 175.9(2) ?
N1 C1 C2 C7' . . . . 24.7(6) ?
C6 C1 C2 C7' . . . . -159.8(6) ?
C1 C2 C3 C4 . . . . 1.2(3) ?
C7 C2 C3 C4 . . . . -176.90(19) ?
C7' C2 C3 C4 . . . . 153.0(9) ?
C2 C3 C4 C5 . . . . -0.5(2) ?
C2 C3 C4 C11 . . . . 175.98(15) ?
C3 C4 C5 C6 . . . . 0.6(2) ?
C11 C4 C5 C6 . . . . -175.81(12) ?
C4 C5 C6 C1 . . . . -1.5(2) ?
C4 C5 C6 C9 . . . . 177.61(12) ?
N1 C1 C6 C5 . . . . 177.72(13) ?
C2 C1 C6 C5 . . . . 2.1(2) ?
N1 C1 C6 C9 . . . . -1.4(2) ?
C2 C1 C6 C9 . . . . -176.97(13) ?
C3 C2 C7 C8 . . . . -93.4(5) ?
C1 C2 C7 C8 . . . . 88.6(4) ?
C3 C2 C7' C8' . . . . -1.0(18) ?
C1 C2 C7' C8' . . . . 153.5(12) ?
C5 C6 C9 C10 . . . . 0.1(2) ?
C1 C6 C9 C10 . . . . 179.21(13) ?
C3 C4 C11 C12 . . . . 137.06(15) ?
C5 C4 C11 C12 . . . . -46.59(19) ?
C4 C11 C12 C17 . . . . 103.56(16) ?
C4 C11 C12 C13 . . . . -76.11(17) ?
C17 C12 C13 C14 . . . . 0.6(2) ?
C11 C12 C13 C14 . . . . -179.74(12) ?
C12 C13 C14 C15 . . . . -1.2(2) ?
C12 C13 C14 C18 . . . . 177.80(13) ?
C13 C14 C15 N2 . . . . -177.22(12) ?
C18 C14 C15 N2 . . . . 3.8(2) ?
C13 C14 C15 C16 . . . . 0.7(2) ?
C18 C14 C15 C16 . . . . -178.32(13) ?
N2 C15 C16 C17 . . . . 178.22(13) ?
C14 C15 C16 C17 . . . . 0.4(2) ?
N2 C15 C16 C20 . . . . 0.3(2) ?
C14 C15 C16 C20 . . . . -177.59(13) ?
C13 C12 C17 C16 . . . . 0.5(2) ?
C11 C12 C17 C16 . . . . -179.18(13) ?
C15 C16 C17 C12 . . . . -1.0(2) ?
C20 C16 C17 C12 . . . . 177.05(14) ?
C13 C14 C18 C19 . . . . 0.3(2) ?
C15 C14 C18 C19 . . . . 179.22(13) ?
C17 C16 C20 C21 . . . . -97.07(19) ?
C15 C16 C20 C21 . . . . 80.9(2) ?