#------------------------------------------------------------------------------
#$Date: 2024-10-16 03:59:20 +0200 (Wed, 16 Oct 2024) $
#$Revision: 295503 $
#$URL: svn://www.crystallography.net/cod/cif/2/02/32/2023292.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_2023292
loop_
_publ_author_name
'Vashchenko, Oleksandr V.'
'Khomenko, Dmytro M.'
'Dyakonenko, Viktoriya V.'
'Lampeka, Rostyslav D.'
_publ_section_title
;
Synthesis, structures and Hirshfeld surface analyses of
2-hydroxy-N′-methylacetohydrazide and
2-hydroxy-N-methylacetohydrazide
;
_journal_issue 11
_journal_name_full
'Acta Crystallographica Section E Crystallographic Communications'
_journal_paper_doi 10.1107/S2056989024009526
_journal_volume 80
_journal_year 2024
_chemical_formula_iupac 'C3 H8 N2 O2'
_chemical_formula_moiety 'C3 H8 N2 O2'
_chemical_formula_sum 'C3 H8 N2 O2'
_chemical_formula_weight 104.11
_chemical_name_systematic
;
2-Hydroxy-N-methylacetohydrazide
;
_space_group_crystal_system monoclinic
_space_group_IT_number 15
_space_group_name_Hall '-C 2yc'
_space_group_name_H-M_alt 'C 1 2/c 1'
_atom_sites_solution_hydrogens mixed
_atom_sites_solution_primary dual
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_cell_angle_alpha 90
_cell_angle_beta 105.65(4)
_cell_angle_gamma 90
_cell_formula_units_Z 8
_cell_length_a 11.646(10)
_cell_length_b 9.304(10)
_cell_length_c 10.514(10)
_cell_measurement_reflns_used 1019
_cell_measurement_temperature 296.15
_cell_measurement_theta_max 30.09
_cell_measurement_theta_min 2.84
_cell_volume 1097.0(18)
_computing_cell_refinement
;
SAINT (Bruker, 2008)
;
_computing_data_collection
;
APEX2 (Bruker, 2008)
;
_computing_data_reduction
;
SAINT (Bruker, 2008)
;
_computing_molecular_graphics
;
Olex2 1.5 (Dolomanov et al., 2009)
;
_computing_publication_material
;
Olex2 1.5 (Dolomanov et al., 2009)
;
_computing_structure_refinement
;
SHELXL2019/3 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT2018/2 (Sheldrick, 2015a)
;
_diffrn_ambient_temperature 296.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type 'Bruker APEXII CCD'
_diffrn_measurement_method '\f and \w scans'
_diffrn_radiation_monochromator graphite
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0989
_diffrn_reflns_av_unetI/netI 0.1016
_diffrn_reflns_limit_h_max 15
_diffrn_reflns_limit_h_min -14
_diffrn_reflns_limit_k_max 12
_diffrn_reflns_limit_k_min -12
_diffrn_reflns_limit_l_max 13
_diffrn_reflns_limit_l_min -13
_diffrn_reflns_number 5355
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 27.498
_diffrn_reflns_theta_min 2.845
_diffrn_source_current 35.0
_diffrn_source_power 1.75
_diffrn_source_voltage 50.0
_diffrn_standards_number 0
_exptl_absorpt_coefficient_mu 0.105
_exptl_absorpt_correction_T_max 0.7460
_exptl_absorpt_correction_T_min 0.5541
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
(SADABS; Krause et al., 2015)
;
_exptl_crystal_colour colourless
_exptl_crystal_density_diffrn 1.261
_exptl_crystal_description block
_exptl_crystal_F_000 448
_exptl_crystal_size_max 0.2
_exptl_crystal_size_mid 0.15
_exptl_crystal_size_min 0.09
_refine_diff_density_max 0.138
_refine_diff_density_min -0.159
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 0.813
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 77
_refine_ls_number_reflns 1259
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 0.813
_refine_ls_R_factor_all 0.1624
_refine_ls_R_factor_gt 0.0499
_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^)+(0.0600P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1049
_refine_ls_wR_factor_ref 0.1259
_reflns_number_gt 503
_reflns_number_total 1259
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file yz2059.cif
_cod_data_source_block 2
_cod_database_code 2023292
_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 0.979
_shelx_estimated_absorpt_t_max 0.991
_shelx_hkl_file
;
1 -1 0 2082.69 61.59
1 -1 0 2317.97 39.60
1 -1 0 2343.87 65.09
-1 1 0 2280.47 65.29
-1 1 0 2298.87 39.30
2 -2 0 6646.83 181.88
2 -2 0 7102.29 192.38
2 -2 0 7264.57 123.49
-2 2 0 6999.60 193.98
-2 2 0 7332.57 119.19
3 -3 0 3033.80 100.89
3 -3 0 3060.59 54.39
-3 3 0 3105.89 54.29
-3 3 0 3150.88 104.29
4 -4 0 1963.00 39.90
4 -4 0 2025.80 79.29
-4 4 0 1964.30 82.89
5 -5 0 50.49 20.60
5 -5 0 39.50 7.20
-5 5 0 56.89 27.00
6 -6 0 126.39 28.40
6 -6 0 126.39 12.00
-6 6 0 156.48 42.50
7 -7 0 7.40 7.10
7 -7 0 -7.50 23.50
-7 7 0 27.00 36.10
8 -8 0 -12.50 24.90
-8 8 0 26.20 44.50
9 -9 0 2.60 29.10
-9 9 0 27.50 37.30
-8 10 0 106.39 54.39
8 -10 0 7.30 29.60
-7 9 0 35.10 45.00
7 -9 0 -5.30 25.30
-6 8 0 39.50 41.80
6 -8 0 10.50 24.20
-5 7 0 288.17 48.40
5 -7 0 440.26 65.59
5 -7 0 307.97 15.10
-4 6 0 37.00 27.50
4 -6 0 53.59 23.10
4 -6 0 40.50 6.80
-3 5 0 822.72 20.30
-3 5 0 806.62 55.99
3 -5 0 892.81 61.79
3 -5 0 795.32 20.30
-2 4 0 447.96 12.40
-2 4 0 477.25 39.50
2 -4 0 460.55 12.80
2 -4 0 467.05 47.90
-1 3 0 1476.05 57.29
-1 3 0 1527.05 26.50
1 -3 0 1377.86 54.49
1 -3 0 1389.76 61.09
0 2 0 1243.98 42.50
0 2 0 1296.77 22.50
0 -2 0 1200.48 47.30
0 -2 0 1219.78 43.00
1 1 0 2326.27 62.19
1 1 0 2250.27 38.50
1 1 0 2197.38 59.09
-1 -1 0 2187.08 58.09
-1 -1 0 2304.97 38.50
-1 -1 0 2299.47 62.09
2 0 0 20.90 5.40
2 0 0 31.00 3.90
2 0 0 18.00 5.10
2 0 0 9.50 7.10
-2 0 0 29.10 3.90
-2 0 0 22.10 5.80
3 -1 0 2411.86 72.09
3 -1 0 2210.18 70.69
3 -1 0 2289.97 42.40
-3 1 0 2275.07 42.10
-3 1 0 2182.68 72.39
4 -2 0 21.00 4.90
4 -2 0 27.30 15.80
-4 2 0 18.70 13.30
5 -3 0 11.90 5.10
5 -3 0 37.60 20.40
-5 3 0 15.40 16.90
6 -4 0 60.09 9.10
6 -4 0 66.59 24.50
-6 4 0 52.99 27.80
7 -5 0 147.09 12.60
7 -5 0 143.39 27.10
-7 5 0 183.48 44.40
8 -6 0 7.90 6.60
8 -6 0 -14.20 22.10
-8 6 0 -7.20 34.30
9 -7 0 -22.30 24.40
-9 7 0 -30.20 45.60
10 -8 0 -18.10 26.20
-10 8 0 10.80 35.60
11 -9 0 -20.80 29.80
-7 11 0 101.99 58.39
7 -11 0 -1.70 29.40
-6 10 0 7.00 29.80
6 -10 0 -9.10 25.60
-5 9 0 6.50 37.80
5 -9 0 -3.30 23.20
-4 8 0 8.20 28.00
4 -8 0 -0.40 21.50
-3 7 0 31.80 28.70
3 -7 0 25.10 23.20
-2 6 0 58.89 6.00
-2 6 0 83.79 26.90
2 -6 0 57.99 22.10
-1 5 0 939.21 21.30
-1 5 0 899.41 49.50
-1 5 0 904.41 20.50
1 -5 0 971.50 59.59
0 4 0 702.43 37.50
0 4 0 717.93 17.30
0 -4 0 678.83 47.50
1 3 0 1533.75 29.80
1 3 0 1481.35 52.29
-1 -3 0 1482.75 53.19
-1 -3 0 1431.66 28.90
-1 -3 0 1441.86 56.49
2 2 0 7097.19 125.59
2 2 0 7424.56 210.98
-2 -2 0 7453.65 207.58
-2 -2 0 7095.89 191.08
-2 -2 0 7062.69 117.39
3 1 0 2286.57 43.50
3 1 0 2164.58 66.19
-3 -1 0 2248.38 67.09
-3 -1 0 2272.67 67.59
-3 -1 0 2195.28 60.79
4 0 0 972.40 24.70
4 0 0 913.71 37.30
4 0 0 948.91 40.40
-4 0 0 925.11 38.90
5 -1 0 206.38 11.80
-5 1 0 227.98 26.20
6 -2 0 57.79 8.90
6 -2 0 62.49 21.30
-6 2 0 59.99 20.80
7 -3 0 19.10 7.40
7 -3 0 39.10 23.40
-7 3 0 19.00 22.30
8 -4 0 3.00 6.30
8 -4 0 12.30 23.40
-8 4 0 -2.70 28.90
9 -5 0 -16.90 21.40
9 -5 0 13.90 7.30
-9 5 0 23.00 34.70
10 -6 0 13.30 8.00
10 -6 0 -8.20 24.20
-10 6 0 -8.80 42.10
11 -7 0 -24.30 26.70
-11 7 0 39.20 52.49
12 -8 0 -43.80 27.80
-12 8 0 10.70 38.00
-5 11 0 96.79 53.09
5 -11 0 -25.40 24.70
-4 10 0 53.79 44.40
4 -10 0 -1.40 23.90
-3 9 0 16.60 30.30
3 -9 0 -9.70 22.00
-2 8 0 4.20 5.70
-2 8 0 -0.80 28.20
2 -8 0 -3.80 21.70
-1 7 0 193.48 36.90
-1 7 0 187.08 11.70
1 -7 0 148.99 27.60
0 6 0 4.20 17.50
0 6 0 3.30 5.10
0 -6 0 5.70 17.20
1 5 0 884.51 45.60
1 5 0 959.60 24.20
-1 -5 0 912.61 50.29
2 4 0 404.56 28.80
-2 -4 0 465.45 34.90
3 3 0 3138.09 59.09
3 3 0 3107.49 93.69
-3 -3 0 3055.89 92.99
-3 -3 0 2996.80 86.69
4 2 0 15.20 5.50
-4 -2 0 18.10 8.70
-4 -2 0 12.70 7.40
-4 -2 0 16.90 8.40
5 1 0 204.28 12.80
-5 -1 0 202.48 19.50
6 0 0 8.20 5.70
6 0 0 4.50 14.70
-6 0 0 9.40 12.50
7 -1 0 172.08 25.30
7 -1 0 264.17 15.60
-7 1 0 257.97 29.90
8 -2 0 39.90 22.80
8 -2 0 14.80 7.80
-8 2 0 33.50 25.60
9 -3 0 160.08 14.30
9 -3 0 182.98 34.10
-9 3 0 197.18 41.90
10 -4 0 5.20 6.80
10 -4 0 -1.90 22.00
-10 4 0 -32.70 34.60
11 -5 0 -18.30 23.70
11 -5 0 -1.70 5.90
-11 5 0 7.30 44.40
12 -6 0 -15.50 26.80
-12 6 0 22.70 51.59
-13 7 0 -4.00 35.10
-4 12 0 120.79 51.79
-3 11 0 53.89 41.00
3 -11 0 -14.60 23.50
-2 10 0 36.60 34.70
2 -10 0 13.60 23.70
-1 9 0 14.10 26.00
1 -9 0 -10.10 20.10
0 8 0 308.67 15.20
0 8 0 362.86 44.40
0 -8 0 329.17 44.30
1 7 0 192.68 35.20
1 7 0 182.58 13.10
-1 -7 0 192.48 37.80
2 6 0 61.69 9.60
2 6 0 55.39 20.00
-2 -6 0 52.99 19.00
3 5 0 754.42 24.40
3 5 0 773.02 42.70
-3 -5 0 864.61 48.40
4 4 0 1924.71 44.70
4 4 0 1976.80 70.49
-4 -4 0 1919.51 62.99
5 3 0 16.50 7.00
-5 -3 0 11.50 10.00
-5 -3 0 9.10 8.40
6 2 0 54.49 9.90
-6 -2 0 37.90 9.00
-6 -2 0 56.09 15.20
7 1 0 241.18 16.30
-7 -1 0 279.07 29.80
8 0 0 11.50 7.50
8 0 0 24.30 18.60
-8 0 0 22.30 20.10
9 -1 0 3.70 21.90
9 -1 0 14.50 8.50
-9 1 0 14.10 26.50
10 -2 0 7.30 7.50
-10 2 0 -12.10 29.80
11 -3 0 8.60 7.50
11 -3 0 -12.50 22.90
-11 3 0 -15.20 38.30
12 -4 0 -33.60 21.80
12 -4 0 8.70 7.30
13 -5 0 5.60 8.40
-13 5 0 -25.30 55.79
-14 6 0 7.50 36.70
-2 12 0 96.49 43.50
2 -12 0 -3.20 25.00
-1 11 0 30.30 31.80
1 -11 0 -12.50 22.30
0 10 0 20.20 28.10
0 -10 0 -3.50 21.00
1 9 0 -2.30 22.20
-1 -9 0 -5.10 19.70
2 8 0 13.60 7.50
2 8 0 0.00 21.20
-2 -8 0 1.90 18.70
3 7 0 21.90 8.30
3 7 0 31.40 19.70
-3 -7 0 23.40 19.50
4 6 0 59.39 10.90
4 6 0 46.60 19.30
-4 -6 0 38.90 16.20
5 5 0 48.10 17.10
5 5 0 36.80 9.50
-5 -5 0 35.20 12.30
6 4 0 40.90 10.00
-6 -4 0 54.19 15.70
-6 -4 0 41.00 11.50
7 3 0 9.20 7.60
-7 -3 0 19.90 9.40
-7 -3 0 18.60 15.60
8 2 0 27.40 9.90
-8 -2 0 32.20 19.90
9 1 0 21.80 9.40
9 1 0 3.30 18.30
-9 -1 0 23.10 23.50
10 0 0 157.28 27.30
10 0 0 196.98 16.90
-10 0 0 263.77 44.00
11 -1 0 111.79 16.40
-11 1 0 102.09 38.40
12 -2 0 28.50 10.30
-12 2 0 5.10 43.10
13 -3 0 16.10 9.00
-13 3 0 -30.50 42.70
14 -4 0 46.40 12.20
-14 4 0 48.90 61.69
-1 13 0 235.18 33.30
0 12 0 97.79 40.10
0 -12 0 -5.70 22.40
1 11 0 64.19 33.20
-1 -11 0 -8.60 20.60
2 10 0 34.80 27.30
-2 -10 0 34.90 23.60
3 9 0 24.60 24.30
3 9 0 0.40 6.90
-3 -9 0 7.80 19.80
4 8 0 8.00 2.60
4 8 0 14.50 19.30
-4 -8 0 -4.70 15.50
5 7 0 284.77 18.80
5 7 0 309.57 37.20
-5 -7 0 331.97 34.00
6 6 0 136.89 17.10
6 6 0 125.89 26.80
-6 -6 0 88.09 16.80
7 5 0 132.99 14.20
-7 -5 0 165.18 23.90
-7 -5 0 151.58 23.40
8 4 0 -0.20 7.90
-8 -4 0 0.50 17.20
9 3 0 185.98 17.90
-9 -3 0 194.68 31.70
10 2 0 4.30 8.00
-10 -2 0 4.30 24.50
11 1 0 76.59 14.10
-11 -1 0 138.89 38.40
12 0 0 22.60 9.60
-12 0 0 18.30 36.00
13 -1 0 23.30 10.20
-13 1 0 -34.30 41.80
14 -2 0 14.40 10.00
-14 2 0 -65.89 50.19
15 -3 0 15.00 8.70
-15 3 0 -85.99 53.49
1 13 0 435.56 38.70
2 12 0 95.09 34.10
-2 -12 0 -4.20 21.90
3 11 0 59.39 30.20
-3 -11 0 3.90 20.60
4 10 0 43.90 27.00
-4 -10 0 7.00 19.30
5 9 0 31.00 23.80
5 9 0 14.10 6.20
-5 -9 0 31.30 18.50
6 8 0 20.30 9.50
6 8 0 40.50 22.50
-6 -8 0 7.20 12.30
7 7 0 24.00 20.50
7 7 0 7.60 8.50
-8 -6 0 99.49 19.80
9 5 0 8.90 9.00
-9 -5 0 20.70 16.80
10 4 0 -2.80 7.10
-10 -4 0 -16.70 18.60
11 3 0 2.90 8.20
-11 -3 0 -17.20 24.40
12 2 0 39.10 12.10
-12 -2 0 30.50 33.40
13 1 0 28.80 10.60
-13 -1 0 -6.40 36.60
14 0 0 15.00 8.90
15 -1 0 13.30 9.30
-15 1 0 -57.69 50.59
5 11 0 102.59 30.80
6 10 0 72.09 28.80
7 9 0 16.60 9.90
7 9 0 39.20 24.80
-11 -5 0 55.09 24.10
12 4 0 3.00 8.60
-12 -4 0 1.70 28.00
13 3 0 15.20 9.20
-13 -3 0 -10.70 32.60
14 2 0 11.20 9.60
-14 -2 0 -16.00 38.00
15 1 0 15.70 10.30
8 10 0 44.60 13.30
9 9 0 13.00 10.30
10 8 0 30.30 12.60
11 7 0 9.40 9.90
12 6 0 42.20 14.10
13 5 0 11.20 10.60
14 4 0 57.99 14.90
15 3 0 14.80 10.10
11 9 0 25.70 11.50
12 8 0 9.30 10.30
13 7 0 11.80 11.00
14 4 1 16.80 10.60
13 5 1 10.40 10.20
12 6 1 27.10 12.60
11 7 1 7.90 9.70
10 8 1 18.90 11.10
9 9 1 14.90 9.80
8 10 1 209.48 33.70
-15 -1 -1 -24.50 48.90
15 1 1 10.00 10.00
-14 -2 -1 -10.80 41.80
14 2 1 12.50 10.20
-13 -3 -1 -2.50 36.50
13 3 1 4.20 8.50
-12 -4 -1 23.00 30.90
12 4 1 0.80 7.80
-11 -5 -1 83.79 27.70
11 5 1 19.00 10.40
-10 -6 -1 107.69 22.30
7 9 1 18.20 9.60
7 9 1 53.49 29.60
6 10 1 48.00 30.30
5 11 1 111.59 33.70
4 12 1 319.07 34.20
-15 1 -1 -82.79 54.79
15 -1 1 14.50 9.20
-14 0 -1 -66.29 43.60
14 0 1 4.30 9.00
-13 -1 -1 -10.40 40.70
13 1 1 0.30 7.70
-12 -2 -1 107.89 43.90
12 2 1 81.19 15.90
-11 -3 -1 -5.40 29.20
11 3 1 12.20 9.30
-10 -4 -1 5.30 23.50
10 4 1 0.70 8.10
-9 -5 -1 108.19 26.70
9 5 1 50.09 12.90
-8 -6 -1 47.80 16.60
8 6 1 21.00 9.70
7 7 1 22.80 9.80
7 7 1 50.59 26.20
6 8 1 57.99 27.70
6 8 1 28.20 9.70
-5 -9 -1 13.80 15.10
5 9 1 13.00 7.20
5 9 1 40.80 27.70
-4 -10 -1 10.00 17.30
4 10 1 29.40 25.50
-3 -11 -1 10.90 20.10
3 11 1 91.69 36.20
2 12 1 145.59 38.70
1 13 1 403.06 39.20
-14 2 -1 -88.99 51.59
14 -2 1 7.80 8.90
-13 1 -1 -46.90 42.20
13 -1 1 10.20 9.00
-12 0 -1 -34.10 35.80
12 0 1 2.50 7.60
-11 -1 -1 147.39 43.60
11 1 1 124.09 18.50
-10 -2 -1 23.10 29.00
10 2 1 20.60 9.80
-9 -3 -1 344.77 38.80
9 3 1 309.97 22.00
-8 -4 -1 63.69 23.70
8 4 1 34.00 11.10
-7 -5 -1 184.98 26.90
7 5 1 179.88 17.10
-6 -6 -1 28.80 11.50
6 6 1 21.90 9.40
6 6 1 35.20 21.90
-5 -7 -1 46.20 15.50
5 7 1 32.70 9.70
5 7 1 47.60 23.70
-4 -8 -1 18.60 16.90
4 8 1 61.29 27.50
4 8 1 27.70 8.70
-3 -9 -1 38.50 21.60
3 9 1 48.90 9.60
3 9 1 98.39 33.60
-2 -10 -1 -4.80 19.90
2 10 1 26.60 29.70
-1 -11 -1 -16.10 21.50
1 11 1 46.90 31.00
0 -12 -1 -22.90 22.30
0 12 1 47.20 26.80
-1 13 1 320.47 42.00
-14 4 -1 -51.89 57.19
14 -4 1 9.30 9.10
-13 3 -1 -43.90 46.40
13 -3 1 14.80 9.00
-12 2 -1 102.79 48.90
12 -2 1 93.59 16.10
-11 1 -1 138.99 46.50
11 -1 1 92.99 15.30
-10 0 -1 -15.50 23.20
10 0 1 0.00 6.60
-9 -1 -1 20.40 24.50
9 1 1 3.60 7.90
-8 -2 -1 552.54 44.40
8 2 1 525.55 25.90
-7 -3 -1 43.80 19.80
7 3 1 38.50 9.90
-6 -4 -1 164.88 25.30
6 4 1 204.78 16.50
-5 -5 -1 2.20 8.90
5 5 1 -6.40 5.70
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-4 0 14 19.10 22.10
-5 1 14 4.90 21.10
6 -2 -14 4.30 34.10
-3 -3 14 27.40 22.20
-4 -2 14 42.40 23.50
-5 -1 14 32.10 24.90
6 0 -14 -12.40 10.20
-6 0 14 9.90 22.30
7 -1 -14 -12.30 10.50
-7 1 14 11.70 22.30
5 3 -14 -11.00 11.50
6 2 -14 -5.30 12.00
-6 -2 14 34.20 23.20
7 1 -14 -7.00 11.90
-7 -1 14 10.10 23.70
8 0 -14 -0.90 11.60
-8 0 14 30.90 26.30
7 3 -14 -6.30 12.30
8 2 -14 -2.30 12.40
-8 -2 14 19.00 24.20
0 0 0 0.00 0.00
_computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)'
;
_shelx_hkl_checksum 14497
_shelx_res_file
;
TITL lamp8a_a.res in C2/c
lamp8a.res
created by SHELXL-2019/3 at 19:00:00 on 19-Sep-2024
REM Old TITL lamp8a in C2/c
REM SHELXT solution in C2/c: R1 0.203, Rweak 0.073, Alpha 0.033
REM 0.239 for 71 systematic absences, Orientation as input
REM Formula found by SHELXT: C1 N1 O1
CELL 0.71073 11.6461 9.3036 10.5138 90 105.649 90
ZERR 8 0.0097 0.0097 0.0098 0 0.043 0
LATT 7
SYMM -X,+Y,0.5-Z
SFAC C H N O
UNIT 24 64 16 16
EQIV $1 1-X,+Y,0.5-Z
EQIV $2 +X,1-Y,0.5+Z
EQIV $3 0.5+X,0.5-Y,0.5+Z
L.S. 4
PLAN 1
SIZE 0.09 0.15 0.2
TEMP 23
CONF
HTAB O1 O2_$1
HTAB N2 O2_$2
HTAB N2 O1_$3
BOND
list 4
MORE -1
BOND $H
fmap 2
acta
OMIT 0 55
REM
REM
REM
WGHT 0.060000
FVAR 0.77189
O1 4 0.426462 0.213546 0.388743 11.00000 0.06483 0.10602 =
0.06561 -0.00351 0.00644 -0.02912
H1 2 0.445541 0.251012 0.331356 11.00000 0.10581
O2 4 0.612504 0.370662 0.377119 11.00000 0.07731 0.07987 =
0.04695 0.00085 0.01176 -0.01698
N1 3 0.683100 0.404304 0.599361 11.00000 0.04758 0.05571 =
0.04633 0.00047 0.00948 -0.00161
N2 3 0.667871 0.368297 0.726403 11.00000 0.06498 0.08122 =
0.04579 -0.00197 0.01280 0.00895
H2A 2 0.649817 0.461085 0.764961 11.00000 0.11202
H2B 2 0.741764 0.336020 0.773348 11.00000 0.08215
C1 1 0.504261 0.256034 0.513176 11.00000 0.05327 0.06603 =
0.06107 -0.00465 0.01458 -0.00671
AFIX 23
H1A 2 0.536650 0.171285 0.564015 11.00000 -1.20000
H1B 2 0.459633 0.310151 0.562713 11.00000 -1.20000
AFIX 0
C2 1 0.605734 0.348056 0.492143 11.00000 0.04862 0.04611 =
0.04643 0.00019 0.00785 0.00581
C3 1 0.782585 0.498270 0.591344 11.00000 0.06048 0.06523 =
0.07490 -0.00134 0.01017 -0.00954
AFIX 137
H3A 2 0.768514 0.593786 0.618254 11.00000 -1.50000
H3B 2 0.788558 0.500277 0.502060 11.00000 -1.50000
H3C 2 0.855570 0.462034 0.648489 11.00000 -1.50000
AFIX 0
HKLF 4
REM lamp8a_a.res in C2/c
REM wR2 = 0.1259, GooF = S = 0.813, Restrained GooF = 0.813 for all data
REM R1 = 0.0499 for 503 Fo > 4sig(Fo) and 0.1624 for all 1259 data
REM 77 parameters refined using 0 restraints
END
WGHT 0.0600 0.0000
REM Highest difference peak 0.138, deepest hole -0.159, 1-sigma level 0.041
Q1 1 0.6161 0.2695 0.7098 11.00000 0.05 0.14
;
_shelx_res_checksum 68501
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -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
O O1 0.42646(16) 0.2135(2) 0.3887(2) 0.0810(7) Uani d 1 . .
H H1 0.446(3) 0.251(4) 0.331(3) 0.106(14) Uiso d 1 . .
O O2 0.61250(14) 0.37066(17) 0.37712(16) 0.0690(6) Uani d 1 . .
N N1 0.68310(16) 0.40430(19) 0.59936(19) 0.0505(6) Uani d 1 . .
N N2 0.6679(2) 0.3683(3) 0.7264(2) 0.0644(7) Uani d 1 . .
H H2A 0.650(2) 0.461(4) 0.765(3) 0.112(11) Uiso d 1 . .
H H2B 0.742(2) 0.336(3) 0.773(3) 0.082(9) Uiso d 1 . .
C C1 0.50426(19) 0.2560(3) 0.5132(2) 0.0603(7) Uani d 1 . .
H H1A 0.536650 0.171285 0.564015 0.072 Uiso calc 1 . .
H H1B 0.459633 0.310151 0.562713 0.072 Uiso calc 1 . .
C C2 0.60573(19) 0.3481(2) 0.4921(2) 0.0480(6) Uani d 1 . .
C C3 0.7826(2) 0.4983(3) 0.5913(2) 0.0684(8) Uani d 1 . .
H H3A 0.768514 0.593786 0.618254 0.103 Uiso calc 1 . .
H H3B 0.788558 0.500277 0.502060 0.103 Uiso calc 1 . .
H H3C 0.855570 0.462034 0.648489 0.103 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
O1 0.0648(12) 0.1060(18) 0.0656(14) -0.0291(11) 0.0064(11) -0.0035(12)
O2 0.0773(13) 0.0799(13) 0.0469(11) -0.0170(9) 0.0118(9) 0.0008(9)
N1 0.0476(11) 0.0557(12) 0.0463(12) -0.0016(10) 0.0095(9) 0.0005(10)
N2 0.0650(16) 0.0812(18) 0.0458(14) 0.0090(12) 0.0128(12) -0.0020(12)
C1 0.0533(14) 0.0660(17) 0.0611(17) -0.0067(13) 0.0146(12) -0.0046(14)
C2 0.0486(14) 0.0461(15) 0.0464(15) 0.0058(11) 0.0079(12) 0.0002(12)
C3 0.0605(16) 0.0652(18) 0.0749(19) -0.0095(13) 0.0102(13) -0.0013(14)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
C1 O1 H1 . . 110(2) ?
N2 N1 C3 . . 119.29(19) ?
C2 N1 N2 . . 117.8(2) ?
C2 N1 C3 . . 122.9(2) ?
N1 N2 H2A . . 105.6(16) ?
N1 N2 H2B . . 104.1(16) ?
H2A N2 H2B . . 109(2) ?
O1 C1 H1A . . 109.6 ?
O1 C1 H1B . . 109.6 ?
O1 C1 C2 . . 110.3(2) ?
H1A C1 H1B . . 108.1 ?
C2 C1 H1A . . 109.6 ?
C2 C1 H1B . . 109.6 ?
O2 C2 N1 . . 122.8(2) ?
O2 C2 C1 . . 119.3(2) ?
N1 C2 C1 . . 117.9(2) ?
N1 C3 H3A . . 109.5 ?
N1 C3 H3B . . 109.5 ?
N1 C3 H3C . . 109.5 ?
H3A C3 H3B . . 109.5 ?
H3A C3 H3C . . 109.5 ?
H3B C3 H3C . . 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
O1 H1 . 0.78(4) ?
O1 C1 . 1.432(3) ?
O2 C2 . 1.251(3) ?
N1 N2 . 1.434(3) ?
N1 C2 . 1.345(3) ?
N1 C3 . 1.472(3) ?
N2 H2A . 1.00(3) ?
N2 H2B . 0.92(3) ?
C1 H1A . 0.9700 ?
C1 H1B . 0.9700 ?
C1 C2 . 1.523(3) ?
C3 H3A . 0.9600 ?
C3 H3B . 0.9600 ?
C3 H3C . 0.9600 ?
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
O1 H1 O2 2_655 0.78(4) 2.39(4) 3.078(4) 148(3) yes
N2 H2A O2 6_566 1.00(3) 2.08(3) 3.062(4) 169(2) yes
N2 H2B O1 8_556 0.92(3) 2.21(3) 3.129(4) 173(2) yes
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
O1 C1 C2 O2 . . . . -2.5(3) ?
O1 C1 C2 N1 . . . . 176.05(19) ?
N2 N1 C2 O2 . . . . -178.7(2) ?
N2 N1 C2 C1 . . . . 2.8(3) ?
C3 N1 C2 O2 . . . . 0.3(3) ?
C3 N1 C2 C1 . . . . -178.2(2) ?