#------------------------------------------------------------------------------
#$Date: 2021-12-15 05:09:00 +0200 (Wed, 15 Dec 2021) $
#$Revision: 271439 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/24/39/2243950.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_2243950
loop_
_publ_author_name
'Schrimpf, Tobias'
'Otte, Felix'
'Strohmann, Carsten'
_publ_section_title
;
Crystal structure of
N,N,N',N'-tetramethylethanediamine
;
_journal_coeditor_code HB8002
_journal_issue 1
_journal_name_full 'Acta Crystallographica Section E'
_journal_page_first
;
;
_journal_paper_doi 10.1107/S2056989021012457
_journal_volume 78
_journal_year 2022
_chemical_formula_iupac 'C6 H16 N2'
_chemical_formula_moiety 'C6 H16 N2'
_chemical_formula_sum 'C6 H16 N2'
_chemical_formula_weight 116.21
_chemical_name_common
;
N,N,N',N'-Tetramethylethanediamine
;
_chemical_name_systematic
;
N,N,N',N'-Tetramethylethane-1,2-diamine
;
_space_group_crystal_system monoclinic
_space_group_IT_number 14
_space_group_name_Hall '-P 2ybc'
_space_group_name_H-M_alt 'P 1 21/c 1'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary dual
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6226)
;
_cell_angle_alpha 90
_cell_angle_beta 106.954(9)
_cell_angle_gamma 90
_cell_formula_units_Z 2
_cell_length_a 5.6987(13)
_cell_length_b 8.311(2)
_cell_length_c 8.453(2)
_cell_measurement_reflns_used 352
_cell_measurement_temperature 100.0
_cell_measurement_theta_max 22.83
_cell_measurement_theta_min 3.52
_cell_volume 382.95(16)
_computing_cell_refinement
;
SAINT (Bruker, 2018)
;
_computing_data_collection
;
APEX2 (Bruker, 2018)
;
_computing_data_reduction
;
SAINT (Bruker, 2018)
;
_computing_molecular_graphics
;
OLEX2 (Dolomanov et al., 2009)
;
_computing_publication_material
;
OLEX2 (Dolomanov et al., 2009)
;
_computing_structure_refinement
;
SHELXL2014/7 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT (Sheldrick, 2015a)
;
_diffrn_ambient_temperature 100.0
_diffrn_detector 'Bruker D8 VENTURE area detector'
_diffrn_detector_area_resol_mean 10.4167
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device 'four-circle diffractometer'
_diffrn_measurement_device_type 'Bruker Venture D8'
_diffrn_measurement_method '\f and \w scans'
_diffrn_radiation_monochromator 'HELIOS mirror optics'
_diffrn_radiation_probe x-ray
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0374
_diffrn_reflns_av_unetI/netI 0.0192
_diffrn_reflns_limit_h_max 9
_diffrn_reflns_limit_h_min -9
_diffrn_reflns_limit_k_max 13
_diffrn_reflns_limit_k_min -13
_diffrn_reflns_limit_l_max 13
_diffrn_reflns_limit_l_min -12
_diffrn_reflns_number 16732
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 35.306
_diffrn_reflns_theta_min 3.516
_diffrn_source 'microfocus sealed X-ray tube'
_diffrn_source_current 1.0
_diffrn_source_power 0.05
_diffrn_source_voltage 50.0
_diffrn_standards_number 0
_exptl_absorpt_coefficient_mu 0.062
_exptl_absorpt_correction_T_max 0.5670
_exptl_absorpt_correction_T_min 0.3707
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
(SADABS; Krause et al., 2015)
;
_exptl_crystal_colour colourless
_exptl_crystal_density_diffrn 1.008
_exptl_crystal_description block
_exptl_crystal_F_000 132
_exptl_crystal_size_max 0.56
_exptl_crystal_size_mid 0.347
_exptl_crystal_size_min 0.304
_refine_diff_density_max 0.409
_refine_diff_density_min -0.152
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.049
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 39
_refine_ls_number_reflns 1720
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.049
_refine_ls_R_factor_all 0.0482
_refine_ls_R_factor_gt 0.0380
_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^)+(0.0452P)^2^+0.0730P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1030
_refine_ls_wR_factor_ref 0.1097
_reflns_number_gt 1434
_reflns_number_total 1720
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file hb8002sup1.cif
_cod_data_source_block I
_cod_original_cell_volume 382.92(18)
_cod_database_code 2243950
_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 0.966
_shelx_estimated_absorpt_t_max 0.981
_shelx_hkl_file
;
-1 0 0 299.230 11.7747 2
-1 0 0 300.958 12.3309 3
1 0 0 299.104 11.7597 2
1 0 0 313.612 12.4562 3
-1 0 0 304.568 8.48672 13
-1 0 0 300.068 8.51417 14
1 0 0 305.585 8.51902 12
1 0 0 322.848 8.56457 13
1 0 0 297.091 8.52892 14
1 0 0 308.686 8.87512 8
1 0 0 350.503 8.54349 9
1 0 0 321.640 8.93855 10
-1 0 0 290.942 8.93382 6
-1 0 0 348.617 8.81847 7
-1 0 0 304.141 8.89405 8
-1 0 0 310.907 8.53227 9
-1 0 0 302.682 8.88169 10
1 0 0 293.571 8.93542 6
1 0 0 362.953 8.84734 7
-1 0 0 308.530 8.52186 12
2 0 0 10.6603 2.47370 1
-2 0 0 12.9920 0.75852 13
-2 0 0 12.7748 0.73995 14
2 0 0 16.0170 0.65423 11
2 0 0 14.0807 0.90556 12
2 0 0 15.2664 0.88348 14
2 0 0 16.7549 1.18599 7
2 0 0 12.2885 2.93810 2
2 0 0 12.6783 3.26815 3
-2 0 0 15.5248 3.53579 2
2 0 0 12.6689 1.20422 6
-2 0 0 9.13116 2.73403 3
2 0 0 15.4697 1.38289 10
-2 0 0 13.3057 0.82318 9
-2 0 0 14.6609 3.10734 1
-2 0 0 16.5673 1.55046 7
-2 0 0 12.8968 1.17037 8
3 0 0 1468.29 53.4969 3
-3 0 0 1463.31 51.8434 2
-3 0 0 1521.66 42.5699 8
3 0 0 1512.68 42.7303 10
3 0 0 1675.50 42.3291 7
-3 0 0 1558.19 54.7826 3
-3 0 0 1519.78 41.2503 13
3 0 0 1470.83 42.7522 6
3 0 0 1603.11 48.9773 1
3 0 0 1503.43 41.3338 12
3 0 0 1497.82 41.4202 14
-3 0 0 1528.65 49.9337 1
3 0 0 1593.53 41.0161 11
4 0 0 44.3827 1.64047 11
-4 0 0 38.2621 6.29996 4
-4 0 0 43.1396 3.34134 8
4 0 0 55.8456 2.96029 7
4 0 0 51.0769 3.55454 10
-4 0 0 43.8862 6.39268 4
-4 0 0 41.4478 6.26627 4
-4 0 0 53.5714 8.03960 3
-4 0 0 42.3359 1.86402 13
-4 0 0 40.5344 7.33542 1
-4 0 0 39.5571 7.93760 2
4 0 0 38.6974 5.91061 1
4 0 0 49.1002 9.48290 3
4 0 0 42.0333 3.11587 6
-5 0 0 489.431 16.2189 8
-5 0 0 488.434 14.2712 13
5 0 0 513.841 14.6416 12
5 0 0 486.927 13.8339 11
5 0 0 496.183 16.9048 6
5 0 0 524.433 16.0194 7
5 0 0 512.059 17.2174 10
6 0 0 21.3943 3.14500 6
6 0 0 30.7588 4.02685 10
-6 0 0 30.2855 2.72180 5
6 0 0 23.4074 2.58255 7
-6 0 0 19.9854 2.74252 8
-6 0 0 21.0812 1.45022 13
6 0 0 20.3578 1.07813 11
-7 0 0 -0.4190 1.09553 5
-7 0 0 -0.3192 1.29664 8
7 0 0 -0.2148 1.12606 7
7 0 0 1.80751 1.75534 6
7 0 0 1.66037 2.01549 10
8 0 0 288.476 13.8993 6
-8 0 0 279.772 11.8063 8
8 0 0 277.237 13.8805 10
8 0 0 307.968 11.8594 7
0 -1 0 -0.0401 0.14396 9
0 -1 0 0.20605 0.21458 3
0 -1 0 0.33962 0.45920 1
0 -1 0 -0.0204 0.28554 4
0 -1 0 -0.0285 0.09941 12
0 -1 0 0.07841 0.08390 14
0 -1 0 0.29986 0.24284 7
0 1 0 -0.0116 0.05899 9
0 1 0 0.71150 0.18890 14
0 1 0 -0.0448 0.12357 8
1 -1 0 3557.76 99.2030 4
1 -1 0 3588.85 99.9348 4
1 -1 0 3529.75 99.5823 1
1 -1 0 3389.87 99.5321 3
-1 -1 0 3462.05 95.8597 2
-1 -1 0 3545.12 95.0662 1
-1 1 0 3483.74 99.6800 1
-1 1 0 3506.21 99.6848 3
1 1 0 3427.67 96.1829 2
-1 1 0 3411.61 99.7099 4
-2 -1 0 810.252 20.9210 11
-2 -1 0 819.986 24.9793 1
2 -1 0 749.708 21.3228 11
2 -1 0 775.884 30.4352 3
2 -1 0 771.540 22.2752 6
2 -1 0 775.920 21.3508 12
2 -1 0 777.417 22.2364 7
2 -1 0 771.706 21.6344 9
2 -1 0 731.400 28.8774 1
-2 -1 0 794.506 27.1696 2
-2 -1 0 775.190 28.3981 3
-2 -1 0 780.403 21.1058 13
-2 -1 0 789.391 21.4294 7
2 -1 0 769.587 22.1151 10
-2 -1 0 770.140 21.0296 12
2 1 0 775.363 27.2432 2
2 1 0 764.158 20.9948 12
2 1 0 780.517 21.9922 6
2 1 0 785.743 20.9258 11
-2 1 0 794.720 21.2405 13
-2 1 0 783.495 30.4580 3
2 1 0 786.484 21.3924 7
2 1 0 792.036 25.0632 1
-2 1 0 840.476 32.2565 4
2 1 0 776.868 21.5351 14
-2 1 0 770.370 22.1747 8
-2 1 0 786.574 29.6210 2
-2 1 0 793.163 32.3905 1
-2 1 0 763.639 29.8992 4
2 1 0 789.642 21.9512 10
-3 -1 0 36.2076 2.18298 8
3 -1 0 37.2884 3.24294 10
3 -1 0 36.8014 1.88062 12
3 -1 0 35.5283 2.69560 6
3 -1 0 31.1652 2.60998 7
3 -1 0 32.5761 1.61542 11
-3 -1 0 33.2047 4.38805 1
-3 -1 0 35.3298 5.01301 2
3 -1 0 35.4366 7.36817 3
3 -1 0 40.7146 6.00347 1
-3 -1 0 31.1948 5.32035 3
-3 -1 0 34.8591 1.46488 13
3 -1 0 33.8790 1.91037 9
-3 1 0 45.0733 6.83117 1
-3 1 0 29.8643 6.20677 2
3 1 0 34.3706 5.33229 3
-3 1 0 34.6610 5.92366 4
3 1 0 34.5171 1.49536 12
3 1 0 34.1925 2.41920 10
-3 1 0 27.1238 6.23802 3
3 1 0 35.8905 4.02358 1
3 1 0 34.4878 6.06989 2
3 1 0 38.5104 1.89175 7
-3 1 0 36.1069 1.57982 13
-3 1 0 28.7665 5.62363 4
3 1 0 37.8319 2.04058 14
-3 1 0 34.1155 1.15896 14
3 1 0 36.4457 1.21947 11
4 -1 0 2.70336 3.21930 3
-4 -1 0 -0.9270 2.41189 2
-4 -1 0 0.12638 2.40137 1
4 -1 0 0.07383 0.38807 11
-4 -1 0 -0.0913 2.38834 3
4 -1 0 0.35046 1.05485 10
4 -1 0 -0.6317 0.73356 7
4 -1 0 -0.2659 0.70818 12
4 -1 0 -0.9170 1.84636 1
4 -1 0 0.93990 0.88181 6
4 1 0 0.49582 0.85981 14
-4 1 0 -3.5105 3.17047 4
4 1 0 1.06585 1.00597 10
4 1 0 1.49795 0.88573 6
-4 1 0 -2.7079 2.90248 1
4 1 0 1.21317 0.59424 12
4 1 0 1.06519 0.61407 7
-4 1 0 -0.6240 2.51874 2
-4 1 0 -0.1798 2.55818 4
-4 1 0 0.28939 0.37079 13
4 1 0 1.17460 3.28823 3
4 1 0 -1.7177 1.44703 1
-4 1 0 -0.1457 2.20273 3
-4 1 0 -0.1549 0.74156 8
5 -1 0 16.3482 2.85313 10
-5 -1 0 23.3251 2.32488 8
5 -1 0 18.6496 1.20514 11
5 -1 0 20.3586 2.00722 12
5 -1 0 19.1515 2.61105 6
5 -1 0 19.3005 2.46844 7
5 1 0 23.0425 2.02509 7
5 1 0 28.9923 2.65130 14
5 1 0 17.8272 3.02676 10
5 1 0 21.3316 1.61672 12
-5 1 0 21.1432 2.58668 8
5 1 0 19.4284 2.55607 6
-6 -1 0 85.4049 4.82077 8
6 -1 0 75.3045 5.81991 10
-6 -1 0 90.1672 4.26818 5
6 -1 0 80.6153 3.81104 12
6 -1 0 81.5951 3.36622 11
6 -1 0 71.9124 4.88853 7
6 -1 0 74.7200 5.47710 6
6 1 0 89.2939 4.31560 7
6 1 0 75.3763 5.86763 10
6 1 0 90.2663 3.36867 12
-6 1 0 71.7520 5.41126 8
6 1 0 87.5621 5.60383 6
-6 1 0 76.1473 3.20542 13
7 -1 0 60.3517 3.27129 12
-7 -1 0 57.1365 4.26225 8
7 -1 0 61.2359 5.39919 6
7 -1 0 56.1805 4.43308 7
7 -1 0 57.0939 5.68310 10
-7 1 0 55.6043 4.71339 8
7 1 0 61.6520 2.82893 12
-7 1 0 51.8162 2.63935 13
7 1 0 63.2985 3.85980 7
7 1 0 54.5853 5.37324 10
7 1 0 57.9464 5.42899 6
-7 1 0 49.1984 4.05272 5
8 -1 0 3.09752 1.30014 12
0 -2 0 608.371 16.1887 12
0 -2 0 595.598 16.1238 10
0 -2 0 628.730 16.8063 7
0 -2 0 612.512 23.0573 1
0 -2 0 555.540 16.6368 8
0 -2 0 603.413 16.6391 9
0 -2 0 630.265 22.3574 3
0 -2 0 601.799 23.6029 4
0 2 0 617.655 22.0396 3
0 2 0 594.879 16.5203 14
0 2 0 553.698 16.8250 8
-1 -2 0 465.350 13.1018 8
1 -2 0 465.991 13.6644 9
1 -2 0 507.909 21.8223 1
-1 -2 0 489.422 13.1143 7
1 -2 0 450.747 13.9465 7
1 -2 0 487.583 13.6540 6
1 -2 0 482.138 13.4850 10
-1 -2 0 480.284 13.0622 11
-1 -2 0 476.605 16.4044 2
1 -2 0 496.716 21.0309 3
-1 -2 0 474.761 13.0525 10
1 -2 0 461.380 12.9659 14
-1 -2 0 471.537 13.1458 9
1 -2 0 507.476 23.5468 4
1 -2 0 466.671 13.1450 12
1 -2 0 472.422 21.6158 4
-1 -2 0 481.914 13.1241 6
-1 2 0 466.537 13.7261 8
1 2 0 461.484 13.2704 9
1 2 0 467.367 13.2268 6
1 2 0 473.704 13.0795 10
-1 2 0 467.287 20.1839 3
1 2 0 483.527 16.7824 2
-1 2 0 465.301 13.1097 13
-1 2 0 471.370 12.9796 14
-1 2 0 481.976 22.7663 4
-1 2 0 464.063 22.4089 4
-1 2 0 525.925 25.3130 1
1 2 0 469.885 13.4861 14
2 -2 0 3.88113 1.38284 7
2 -2 0 3.92118 2.15380 4
-2 -2 0 5.02201 0.50694 9
2 -2 0 4.92012 0.78519 12
-2 -2 0 4.54516 0.43913 5
-2 -2 0 5.44788 1.55730 1
2 -2 0 4.18176 0.90112 6
2 -2 0 4.34674 3.20971 1
2 -2 0 4.97617 1.02091 10
-2 -2 0 4.69038 0.35553 11
-2 -2 0 3.85120 1.92888 3
-2 -2 0 5.15420 0.55111 7
-2 -2 0 5.14717 0.49475 13
-2 -2 0 2.24853 1.28541 2
2 -2 0 7.32887 3.72887 4
-2 2 0 10.0841 4.10246 4
-2 2 0 2.93847 0.83806 8
2 2 0 4.68025 0.53923 7
2 2 0 3.89141 0.83695 14
2 2 0 3.84001 0.81564 6
2 2 0 4.14069 1.85072 2
-2 2 0 10.5958 3.74690 1
-2 2 0 3.98431 0.60213 13
-2 2 0 6.25652 3.60816 4
-2 2 0 0.58981 1.52298 3
-3 -2 0 39.5011 4.11476 1
3 -2 0 37.4019 2.63024 6
-3 -2 0 39.1539 2.14348 8
3 -2 0 41.8316 4.48949 4
3 -2 0 39.7089 3.01786 7
-3 -2 0 37.8234 5.65657 3
3 -2 0 35.3679 2.36858 9
-3 -2 0 40.5357 2.00650 7
3 -2 0 34.3331 7.69825 3
-3 -2 0 37.4741 1.56091 13
3 -2 0 42.5143 8.01224 1
-3 -2 0 43.2230 5.23945 2
-3 -2 0 37.9066 1.26678 11
3 -2 0 38.6501 2.34788 12
3 -2 0 39.7985 2.72906 10
3 -2 0 40.2809 2.09158 11
-3 2 0 37.6361 7.70214 1
-3 2 0 38.2300 7.56976 4
3 2 0 36.8587 2.38817 6
-3 2 0 40.5523 8.81371 3
-3 2 0 36.6955 7.58388 2
3 2 0 39.3322 4.25954 1
3 2 0 37.4480 1.31756 12
3 2 0 40.4001 2.38036 14
3 2 0 40.5594 5.03314 2
-3 2 0 36.4205 1.74339 13
3 2 0 38.3659 1.82351 7
3 2 0 35.9777 2.96321 10
4 -2 0 136.984 6.46545 10
4 -2 0 147.757 6.56027 6
4 -2 0 142.203 5.05542 11
4 -2 0 151.628 6.70670 7
4 -2 0 134.954 14.0005 1
-4 -2 0 154.720 12.9891 3
4 -2 0 143.847 5.22473 12
4 -2 0 144.209 5.64152 9
-4 -2 0 155.353 11.6625 2
-4 -2 0 152.167 5.74027 8
4 -2 0 125.300 13.7550 3
-4 -2 0 146.190 4.63165 13
-4 -2 0 154.959 9.80582 1
-4 2 0 149.217 6.49134 8
-4 2 0 135.780 13.2809 1
-4 2 0 151.308 4.88488 13
4 2 0 155.531 6.36507 6
-4 2 0 132.818 13.7777 2
4 2 0 140.829 11.7524 2
4 2 0 147.108 4.33576 12
-4 2 0 129.616 14.8979 4
-4 2 0 141.616 14.4106 3
4 2 0 135.353 9.65128 1
4 2 0 146.318 5.10589 7
4 2 0 148.881 6.37098 10
-4 2 0 124.084 14.5864 4
-5 -2 0 0.97719 0.48962 13
5 -2 0 1.93547 1.28526 7
5 -2 0 0.43318 1.18653 6
5 -2 0 0.06233 1.56418 10
5 -2 0 -0.3024 0.53900 11
5 -2 0 2.16431 1.08624 12
-5 -2 0 0.65654 0.85634 8
-5 -2 0 -0.3495 0.64828 5
5 2 0 0.86445 0.42896 12
5 2 0 0.99428 0.60364 7
5 2 0 -1.5409 1.04805 10
5 2 0 3.52698 1.58018 14
5 2 0 -1.1338 0.88176 6
6 -2 0 10.2568 2.24443 7
-6 -2 0 8.89919 1.42840 5
6 -2 0 11.1270 1.77116 12
6 -2 0 9.72789 2.79476 10
6 -2 0 10.5728 2.67337 6
-6 -2 0 12.5129 2.09059 8
6 -2 0 12.5105 1.17289 11
6 2 0 11.4791 1.01861 12
6 2 0 11.1731 1.47225 7
6 2 0 8.36947 2.17784 6
6 2 0 11.3494 2.63352 10
-6 2 0 10.7910 1.36725 13
-6 2 0 8.94951 2.33311 8
7 -2 0 2.27731 1.12997 12
-7 -2 0 0.33743 1.20141 8
-7 -2 0 1.04178 0.77534 5
7 -2 0 3.37881 2.74442 6
7 -2 0 2.20690 1.42941 7
7 -2 0 4.44343 3.55172 10
7 2 0 1.19567 2.17957 10
7 2 0 2.06517 1.82986 6
-7 2 0 -0.3050 1.25591 5
7 2 0 2.48895 1.20268 7
-7 2 0 2.62228 0.96873 13
-7 2 0 -0.4416 1.72882 8
8 -2 0 5.23400 1.83538 12
0 -3 0 -2.0085 1.28835 4
0 -3 0 0.31800 0.34814 12
0 -3 0 -0.2528 0.54084 9
0 -3 0 1.06727 0.75791 7
0 -3 0 -0.0671 1.35461 3
0 -3 0 0.19151 0.27128 10
0 -3 0 -0.6807 1.45372 1
0 -3 0 0.79242 1.92217 4
0 3 0 0.57263 0.56989 14
0 3 0 -0.2664 0.27267 6
0 3 0 0.02098 0.39257 8
0 3 0 -0.3311 1.22809 3
1 -3 0 29.0876 1.50744 12
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-2 -2 13 3.30225 2.32177 14
-2 2 13 2.10465 1.53510 11
-2 2 13 4.27372 2.04699 14
-2 2 13 2.69655 1.47840 13
-1 -2 13 0.59935 1.31421 11
-1 -2 13 -0.6625 1.72211 14
-1 2 13 1.50593 1.60536 14
-1 2 13 0.74215 1.22446 11
0 -2 13 0.68921 1.61969 14
0 -2 13 0.27783 1.16260 11
0 2 13 0.86317 1.72154 14
0 2 13 0.91370 1.49367 11
-4 -3 13 -0.5554 0.88143 11
-4 -3 13 1.33143 1.33489 14
-4 3 13 -1.4166 0.96634 13
-4 3 13 0.04197 1.47937 11
-3 -3 13 0.79576 0.99141 11
-3 -3 13 3.07893 1.35894 13
-3 -3 13 2.58703 1.79905 14
-3 3 13 2.02451 1.97183 11
-3 3 13 2.49429 1.34010 13
-2 -3 13 40.6984 3.40626 13
-2 -3 13 30.5112 3.97263 14
-2 -3 13 39.9215 3.74609 11
-2 3 13 38.3445 4.20963 14
-2 3 13 30.9687 5.12627 11
-2 3 13 41.0849 3.42763 13
-1 -3 13 3.23991 1.39374 11
-1 -3 13 4.01173 2.16684 14
-1 3 13 4.04923 1.79233 11
-1 3 13 1.72310 1.65974 14
-3 -4 13 10.0910 2.17963 13
-3 -4 13 12.7183 2.29575 11
-3 -4 13 10.4169 2.79464 14
-3 4 13 10.0732 2.44144 14
-3 4 13 8.96958 2.47825 11
-3 4 13 5.17471 1.75651 13
-2 -4 13 0.28091 1.22462 13
-2 -4 13 2.41577 1.82256 14
-2 -4 13 -0.7833 0.97446 11
-2 4 13 2.51913 1.51825 14
-2 4 13 0.79257 1.38482 11
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 0.5670
_exptl_absorpt_correction_T_min 0.3707
_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 0.71072 5.698 8.312 8.453 89.999 106.949 90.003
)
;
_shelx_hkl_checksum 27554
_shelx_res_file
;
b1696_0m.res created by SHELXL-2014/7
TITL b1696_0m_a.res in P2(1)/c
REM Old TITL b1696_0m_a.res in P2(1)/c
REM SHELXT solution in P2(1)/c
REM R1 0.168, Rweak 0.033, Alpha 0.018, Orientation as input
REM Formula found by SHELXT: C3 N
CELL 0.71073 5.6987 8.3105 8.4528 90 106.954 90
ZERR 2 0.0013 0.0023 0.0024 0 0.009 0
LATT 1
SYMM -X,0.5+Y,0.5-Z
SFAC C H N
UNIT 12 32 4
L.S. 4 0 0
PLAN 2
SIZE 0.304 0.347 0.56
TEMP -173.15
CONF
BOND $H
list 4
MORE -1
fmap 2 53
acta
REM
REM
REM
WGHT 0.045200 0.073000
FVAR 1.70973
N1 3 0.252695 0.345281 0.536357 11.00000 0.01667 0.01545 =
0.01966 0.00150 0.00420 0.00035
C1 1 0.493381 0.338070 0.659767 11.00000 0.01696 0.02605 =
0.02651 0.00427 0.00275 0.00253
AFIX 137
H1A 2 0.579369 0.440365 0.660798 11.00000 -1.50000
H1B 2 0.589563 0.250480 0.632000 11.00000 -1.50000
H1C 2 0.472504 0.318534 0.769203 11.00000 -1.50000
AFIX 0
C2 1 0.125261 0.193032 0.535630 11.00000 0.02440 0.01571 =
0.02973 0.00150 0.00626 -0.00141
AFIX 137
H2A 2 0.097636 0.176428 0.643591 11.00000 -1.50000
H2B 2 0.225303 0.104791 0.513430 11.00000 -1.50000
H2C 2 -0.032813 0.195541 0.449380 11.00000 -1.50000
AFIX 0
C3 1 0.113666 0.481437 0.571608 11.00000 0.01760 0.01632 =
0.01741 -0.00102 0.00177 0.00014
AFIX 23
H3A 2 0.220712 0.577636 0.595233 11.00000 -1.20000
H3B 2 0.063129 0.457342 0.671646 11.00000 -1.20000
AFIX 0
HKLF 4
REM b1696_0m_a.res in P2(1)/c
REM R1 = 0.0380 for 1434 Fo > 4sig(Fo) and 0.0482 for all 1720 data
REM 39 parameters refined using 0 restraints
END
WGHT 0.0452 0.0730
REM Highest difference peak 0.409, deepest hole -0.152, 1-sigma level 0.042
Q1 1 0.0000 0.5000 0.5000 10.50000 0.05 0.41
Q2 1 0.1804 0.4132 0.5488 11.00000 0.05 0.28
;
_shelx_res_checksum 34297
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
N N1 0.25269(10) 0.34528(6) 0.53636(6) 0.01749(12) Uani d 1 . .
C C1 0.49338(12) 0.33807(9) 0.65977(9) 0.02394(15) Uani d 1 . .
H H1A 0.5794 0.4404 0.6608 0.036 Uiso calc 1 . .
H H1B 0.5896 0.2505 0.6320 0.036 Uiso calc 1 . .
H H1C 0.4725 0.3185 0.7692 0.036 Uiso calc 1 . .
C C2 0.12526(13) 0.19303(8) 0.53563(9) 0.02363(14) Uani d 1 . .
H H2A 0.0976 0.1764 0.6436 0.035 Uiso calc 1 . .
H H2B 0.2253 0.1048 0.5134 0.035 Uiso calc 1 . .
H H2C -0.0328 0.1955 0.4494 0.035 Uiso calc 1 . .
C C3 0.11367(10) 0.48144(7) 0.57161(7) 0.01782(13) Uani d 1 . .
H H3A 0.2207 0.5776 0.5952 0.021 Uiso calc 1 . .
H H3B 0.0631 0.4573 0.6716 0.021 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 0.0167(2) 0.0154(2) 0.0197(2) 0.00035(16) 0.00420(16) 0.00150(16)
C1 0.0170(3) 0.0261(3) 0.0265(3) 0.0025(2) 0.0028(2) 0.0043(2)
C2 0.0244(3) 0.0157(3) 0.0297(3) -0.0014(2) 0.0063(2) 0.0015(2)
C3 0.0176(2) 0.0163(2) 0.0174(2) 0.00014(19) 0.00177(17) -0.00102(18)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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
C2 N1 C1 . . 109.26(5) ?
C2 N1 C3 . . 111.96(5) ?
C3 N1 C1 . . 109.75(5) ?
N1 C1 H1A . . 109.5 ?
N1 C1 H1B . . 109.5 ?
N1 C1 H1C . . 109.5 ?
H1A C1 H1B . . 109.5 ?
H1A C1 H1C . . 109.5 ?
H1B C1 H1C . . 109.5 ?
N1 C2 H2A . . 109.5 ?
N1 C2 H2B . . 109.5 ?
N1 C2 H2C . . 109.5 ?
H2A C2 H2B . . 109.5 ?
H2A C2 H2C . . 109.5 ?
H2B C2 H2C . . 109.5 ?
N1 C3 C3 . 3_566 112.37(6) ?
N1 C3 H3A . . 109.1 ?
N1 C3 H3B . . 109.1 ?
C3 C3 H3A 3_566 . 109.1 ?
C3 C3 H3B 3_566 . 109.1 ?
H3A C3 H3B . . 107.9 ?
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 . 1.4624(9) ?
N1 C2 . 1.4580(9) ?
N1 C3 . 1.4610(8) ?
C1 H1A . 0.9800 ?
C1 H1B . 0.9800 ?
C1 H1C . 0.9800 ?
C2 H2A . 0.9800 ?
C2 H2B . 0.9800 ?
C2 H2C . 0.9800 ?
C3 C3 3_566 1.5246(12) ?
C3 H3A . 0.9900 ?
C3 H3B . 0.9900 ?
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
C1 N1 C3 C3 . . . 3_566 167.33(6) ?
C2 N1 C3 C3 . . . 3_566 -71.17(8) ?
N1 C3 C3 N1 . . 3_566 3_566 180.0 ?
_cod_database_fobs_code 2243950