#------------------------------------------------------------------------------
#$Date: 2021-12-15 05:08:38 +0200 (Wed, 15 Dec 2021) $
#$Revision: 271438 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/24/39/2243949.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_2243949
loop_
_publ_author_name
'G\"um\"u\,s, Mustafa Kemal'
'Kansiz, Sevgi'
'Tulemisova, Gulzhamal Bagitovna'
'Dege, Necmi'
'Saif, Eiad'
_publ_section_title
;
Crystal structure and Hirshfeld surface analysis of
3-(hydroxymethyl)-3-methyl-2,6-diphenylpiperidin-4-one
;
_journal_coeditor_code YK2159
_journal_issue 1
_journal_name_full 'Acta Crystallographica Section E'
_journal_page_first
;
;
_journal_paper_doi 10.1107/S2056989021012640
_journal_volume 78
_journal_year 2022
_chemical_formula_iupac 'C19 H21 N O2'
_chemical_formula_moiety 'C19 H21 N O2'
_chemical_formula_sum 'C19 H21 N O2'
_chemical_formula_weight 295.37
_chemical_name_systematic
;
3-(Hydroxymethyl)-3-methyl-2,6-diphenylpiperidin-4-one
;
_space_group_crystal_system orthorhombic
_space_group_IT_number 33
_space_group_name_Hall 'P 2c -2n'
_space_group_name_H-M_alt 'P n a 21'
_atom_sites_solution_hydrogens mixed
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_audit_creation_method SHELXL-2018/3
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_formula_units_Z 4
_cell_length_a 17.3298(8)
_cell_length_b 14.1856(7)
_cell_length_c 6.5857(3)
_cell_measurement_reflns_used 17006
_cell_measurement_temperature 296(2)
_cell_measurement_theta_max 31.52
_cell_measurement_theta_min 1.86
_cell_volume 1618.99(13)
_computing_cell_refinement
;
X-AREA (Stoe & Cie, 2002)
;
_computing_data_collection
;
X-AREA (Stoe & Cie, 2002)
;
_computing_data_reduction
;
X-RED (Stoe & Cie, 2002)
;
_computing_molecular_graphics
;
PLATON (Spek, 2020)
;
_computing_publication_material
;
WinGX (Farrugia, 2012) and publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL2017/1 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT2017/1 (Sheldrick, 2015a)
;
_diffrn_ambient_temperature 296(2)
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type 'Stoe IPDS 2'
_diffrn_measurement_method 'rotation method'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0416
_diffrn_reflns_av_unetI/netI 0.0369
_diffrn_reflns_limit_h_max 25
_diffrn_reflns_limit_h_min -24
_diffrn_reflns_limit_k_max 20
_diffrn_reflns_limit_k_min -20
_diffrn_reflns_limit_l_max 9
_diffrn_reflns_limit_l_min -7
_diffrn_reflns_number 17314
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 31.195
_diffrn_reflns_theta_min 1.855
_diffrn_source
'sealed X-ray tube, 12 x 0.4 mm long-fine focus'
_exptl_absorpt_coefficient_mu 0.078
_exptl_absorpt_correction_T_max 0.9725
_exptl_absorpt_correction_T_min 0.9578
_exptl_absorpt_correction_type integration
_exptl_absorpt_process_details
;
(X-RED32; Stoe & Cie, 2002)
;
_exptl_crystal_colour colorless
_exptl_crystal_density_diffrn 1.212
_exptl_crystal_description prism
_exptl_crystal_F_000 632
_exptl_crystal_size_max 0.720
_exptl_crystal_size_mid 0.573
_exptl_crystal_size_min 0.330
_refine_diff_density_max 0.156
_refine_diff_density_min -0.192
_refine_ls_abs_structure_details
;
Flack x determined using 1072 quotients
[(I^+^)-(I^-^)]/[(I^+^)+(I^-^)]
(Parsons et al., 2013)
;
_refine_ls_abs_structure_Flack 0.8(5)
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.014
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 204
_refine_ls_number_reflns 4763
_refine_ls_number_restraints 1
_refine_ls_restrained_S_all 1.014
_refine_ls_R_factor_all 0.0617
_refine_ls_R_factor_gt 0.0414
_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^)+(0.0515P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0898
_refine_ls_wR_factor_ref 0.0964
_reflns_number_gt 3441
_reflns_number_total 4763
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file yk2159sup1.cif
_cod_data_source_block I
_cod_database_code 2243949
_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_hkl_file
;
-2 0 0 2356.82 23.13 0
2 0 0 2401.93 23.54 0
-4 0 0 41.60 3.38 0
4 0 0 42.56 3.41 0
-6 0 0 1541.78 11.26 0
6 0 0 1585.49 11.54 0
8 0 0 1049.69 8.24 0
-8 0 0 1018.70 8.11 0
-10 0 0 1483.72 9.14 0
10 0 0 1558.92 9.27 0
12 0 0 1.12 2.01 0
-12 0 0 2.10 2.09 0
14 0 0 29.00 2.44 0
-14 0 0 29.68 2.46 0
-16 0 0 2.37 2.15 0
16 0 0 2.66 2.31 0
-18 0 0 10.76 2.97 0
18 0 0 9.88 2.51 0
20 0 0 6.37 2.78 0
-20 0 0 8.14 3.23 0
22 0 0 0.82 3.56 0
24 0 0 1.24 3.99 0
1 -1 0 459.08 12.59 0
1 1 0 473.23 9.77 0
-1 -1 0 459.15 9.51 0
2 1 0 2516.85 18.22 0
2 -1 0 2719.52 27.41 0
-2 -1 0 2444.78 17.94 0
3 -1 0 1514.87 17.45 0
-3 -1 0 1522.93 12.68 0
3 1 0 1539.35 12.84 0
-4 1 0 181.58 5.68 0
4 -1 0 186.90 5.72 0
4 1 0 184.57 4.72 0
-4 -1 0 194.53 4.80 0
5 1 0 809.31 8.08 0
-5 -1 0 796.17 7.87 0
5 -1 0 734.24 9.43 0
-5 1 0 823.87 9.83 0
-6 1 0 44.80 3.06 0
6 -1 0 44.10 3.04 0
6 1 0 43.22 2.30 0
-6 -1 0 44.01 2.74 0
-7 -1 0 49.32 2.65 0
7 -1 0 50.23 3.25 0
7 1 0 52.29 2.66 0
-7 1 0 48.08 2.86 0
8 -1 0 586.98 6.99 0
-8 1 0 561.64 6.68 0
-8 -1 0 578.08 5.93 0
8 1 0 609.43 6.00 0
-9 1 0 349.54 5.36 0
-9 -1 0 324.58 4.52 0
9 1 0 350.63 4.67 0
9 -1 0 337.95 5.07 0
-10 1 0 74.45 3.29 0
10 1 0 73.66 2.69 0
-10 -1 0 77.87 3.17 0
10 -1 0 71.17 2.97 0
11 1 0 1.56 2.03 0
-11 1 0 3.25 1.94 0
11 -1 0 0.38 1.98 0
-11 -1 0 -0.43 1.95 0
12 -1 0 3.87 2.02 0
-12 1 0 2.71 2.04 0
12 1 0 0.58 2.21 0
-12 -1 0 3.04 2.05 0
-13 1 0 29.50 2.90 0
13 1 0 29.27 2.38 0
13 -1 0 29.75 2.42 0
-13 -1 0 26.20 2.40 0
14 -1 0 2.16 2.07 0
14 1 0 0.85 2.25 0
-14 -1 0 2.42 2.23 0
-14 1 0 0.34 2.57 0
-15 -1 0 3.27 2.11 0
15 1 0 4.74 2.67 0
-15 1 0 1.68 2.21 0
15 -1 0 3.44 2.64 0
-16 1 0 4.85 2.20 0
16 1 0 7.89 2.33 0
16 -1 0 7.05 2.38 0
-16 -1 0 8.49 2.28 0
17 -1 0 8.47 2.52 0
-17 -1 0 8.77 2.31 0
-17 1 0 6.24 2.99 0
17 1 0 6.43 2.31 0
18 1 0 67.29 3.54 0
-18 -1 0 64.67 2.96 0
18 -1 0 64.89 3.14 0
-19 -1 0 3.35 2.45 0
19 -1 0 3.01 3.38 0
19 1 0 2.75 2.44 0
20 -1 0 0.55 3.21 0
20 1 0 1.70 2.68 0
-20 -1 0 0.70 2.62 0
21 -1 0 1.02 2.72 0
21 1 0 -1.33 3.45 0
-21 -1 0 0.09 2.81 0
22 -1 0 1.09 3.61 0
22 -1 0 5.38 3.63 0
22 1 0 3.90 3.07 0
-22 -1 0 2.96 3.37 0
23 -1 0 2.68 3.83 0
23 -1 0 -0.04 3.87 0
23 1 0 0.37 3.14 0
-23 -1 0 -1.32 3.10 0
24 -1 0 0.93 4.10 0
24 1 0 -0.22 4.16 0
24 -1 0 1.38 4.09 0
25 -1 0 0.81 4.47 0
25 1 0 1.63 4.35 0
25 -1 0 1.23 5.19 0
0 -2 0 3242.31 20.04 0
0 2 0 3184.06 19.84 0
-1 2 0 313.67 7.09 0
-1 -2 0 319.60 6.43 0
1 -2 0 318.10 7.55 0
1 2 0 311.86 6.05 0
-2 -2 0 1217.37 10.57 0
-2 2 0 1209.44 14.10 0
2 2 0 1223.52 10.62 0
2 -2 0 1235.82 14.30 0
-3 2 0 9999.99 39.80 0
3 -2 0 9895.91 39.48 0
3 2 0 7835.77 24.46 0
-3 -2 0 7990.00 24.88 0
4 2 0 1173.20 9.05 0
4 -2 0 1213.19 13.41 0
-4 -2 0 1184.75 9.02 0
5 -2 0 95.91 4.53 0
5 2 0 105.89 3.34 0
5 -2 0 106.27 4.69 0
-5 -2 0 108.86 3.39 0
-6 -2 0 70.83 2.81 0
6 -2 0 63.84 3.35 0
6 2 0 66.12 2.80 0
7 2 0 36.57 2.43 0
7 -2 0 35.43 3.07 0
-7 -2 0 35.03 2.42 0
-8 -2 0 9.50 2.10 0
8 2 0 10.40 1.67 0
8 -2 0 9.47 2.19 0
-9 -2 0 687.70 6.02 0
9 -2 0 690.42 7.55 0
9 2 0 668.80 5.84 0
10 2 0 383.66 4.54 0
-10 -2 0 378.68 4.53 0
10 -2 0 353.01 5.48 0
-11 -2 0 451.13 4.74 0
11 -2 0 445.81 6.04 0
11 2 0 453.13 4.69 0
-12 -2 0 2.78 1.97 0
12 -2 0 2.36 2.42 0
12 2 0 2.27 2.15 0
-13 -2 0 2.04 2.08 0
13 2 0 2.82 2.10 0
13 -2 0 2.90 2.13 0
14 -2 0 27.87 2.87 0
-14 -2 0 29.74 2.34 0
14 2 0 23.17 2.36 0
15 2 0 11.62 2.25 0
-15 -2 0 17.67 2.23 0
15 -2 0 12.79 2.24 0
16 2 0 34.84 2.53 0
16 -2 0 33.00 3.11 0
-16 -2 0 38.04 2.40 0
17 2 0 2.54 2.84 0
-17 -2 0 3.43 2.30 0
17 -2 0 2.12 3.06 0
-18 -2 0 6.95 2.43 0
18 2 0 8.96 2.53 0
18 -2 0 6.36 2.52 0
-19 -2 0 2.55 2.42 0
19 -2 0 1.72 3.36 0
19 2 0 1.31 2.45 0
19 -2 0 2.65 3.30 0
20 -2 0 1.11 3.27 0
20 2 0 0.20 2.69 0
-20 -2 0 -0.03 2.58 0
20 -2 0 -0.91 3.22 0
-21 -2 0 2.85 2.72 0
21 -2 0 1.70 3.32 0
21 -2 0 1.72 3.43 0
21 2 0 3.23 3.37 0
22 -2 0 0.92 3.60 0
-22 -2 0 1.95 2.89 0
22 2 0 1.24 2.86 0
22 -2 0 2.25 3.63 0
23 2 0 6.82 3.17 0
-23 -2 0 6.57 3.13 0
23 -2 0 5.92 3.75 0
23 -2 0 6.15 3.62 0
24 -2 0 12.31 4.67 0
24 2 0 6.90 3.49 0
24 -2 0 8.36 4.25 0
-24 -2 0 3.01 3.40 0
25 -2 0 1.41 5.06 0
25 2 0 1.19 4.41 0
25 -2 0 0.82 5.13 0
1 3 0 337.35 5.56 0
1 -3 0 349.12 6.23 0
-1 -3 0 343.03 5.58 0
-1 3 0 352.79 6.44 0
-2 -3 0 787.22 7.53 0
2 -3 0 778.04 9.31 0
2 3 0 753.06 7.19 0
-2 3 0 780.89 9.28 0
3 3 0 3611.99 14.79 0
-3 -3 0 3594.61 14.51 0
3 -3 0 3789.15 20.14 0
-3 3 0 3782.90 20.61 0
-4 3 0 127.84 5.00 0
-4 -3 0 122.94 3.04 0
4 3 0 124.39 3.55 0
4 -3 0 122.23 4.47 0
-5 -3 0 -0.48 2.11 0
5 3 0 0.37 2.19 0
5 -3 0 1.02 3.04 0
6 -3 0 98.10 3.83 0
-6 -3 0 98.93 2.96 0
6 3 0 95.99 2.93 0
6 -3 0 86.04 3.56 0
-7 -3 0 31.13 2.31 0
7 3 0 29.48 1.83 0
7 -3 0 30.82 2.99 0
7 -3 0 27.60 2.89 0
8 -3 0 362.49 6.00 0
8 -3 0 353.62 5.88 0
8 3 0 342.13 4.27 0
-8 -3 0 357.54 4.33 0
-9 -3 0 201.71 3.49 0
9 -3 0 219.51 4.97 0
9 3 0 222.90 3.61 0
9 -3 0 200.17 4.76 0
-10 -3 0 3.26 2.06 0
10 -3 0 3.78 2.61 0
10 3 0 3.65 2.10 0
10 -3 0 3.47 2.12 0
11 3 0 -1.29 2.10 0
11 -3 0 1.19 2.58 0
-11 -3 0 0.83 1.99 0
11 -3 0 -0.05 2.09 0
12 3 0 25.37 2.29 0
12 -3 0 26.96 2.97 0
12 -3 0 27.78 2.44 0
-12 -3 0 27.49 2.26 0
13 3 0 39.80 2.36 0
-13 -3 0 42.19 2.40 0
13 -3 0 40.90 3.06 0
13 -3 0 42.41 3.11 0
-14 -3 0 1.14 2.16 0
14 -3 0 0.66 2.72 0
14 3 0 1.45 2.23 0
14 -3 0 2.67 2.18 0
15 -3 0 58.12 3.43 0
15 3 0 53.09 2.57 0
-15 -3 0 56.92 2.55 0
15 -3 0 54.43 3.35 0
16 3 0 3.31 2.39 0
-16 -3 0 4.97 2.29 0
16 -3 0 4.54 3.08 0
16 -3 0 4.66 2.77 0
17 -3 0 41.06 3.36 0
17 3 0 39.88 3.08 0
17 -3 0 42.41 3.37 0
-17 -3 0 46.03 2.58 0
18 -3 0 3.88 3.17 0
18 3 0 5.79 2.37 0
18 -3 0 3.10 3.11 0
-18 -3 0 3.02 2.46 0
19 3 0 11.76 2.55 0
19 -3 0 9.51 3.13 0
-19 -3 0 10.19 2.49 0
19 -3 0 10.54 3.28 0
20 -3 0 1.49 3.39 0
-20 -3 0 0.46 2.56 0
20 3 0 0.36 2.59 0
20 -3 0 1.66 3.27 0
21 -3 0 -0.72 3.43 0
21 3 0 -0.41 2.67 0
21 -3 0 0.93 3.44 0
-21 -3 0 -0.42 2.63 0
22 -3 0 1.11 4.28 0
22 3 0 1.26 3.03 0
-22 -3 0 1.50 2.84 0
22 -3 0 -0.27 3.63 0
23 -3 0 7.50 5.09 0
23 3 0 8.46 3.23 0
23 -3 0 9.78 4.65 0
-23 -3 0 12.68 3.17 0
-24 -3 0 2.92 3.26 0
24 -3 0 0.08 5.29 0
24 3 0 1.14 3.31 0
24 -3 0 1.91 5.78 0
0 -4 0 5559.08 18.71 0
0 4 0 5483.26 18.30 0
1 4 0 7853.24 21.01 0
-1 -4 0 7436.62 20.52 0
1 -4 0 8649.43 24.54 0
-1 4 0 8178.53 23.58 0
-2 4 0 1.10 2.79 0
2 4 0 0.58 2.44 0
-2 -4 0 -0.10 2.46 0
2 -4 0 1.32 2.60 0
3 4 0 336.30 4.71 0
3 -4 0 338.09 5.70 0
-3 -4 0 358.89 4.86 0
-3 4 0 345.54 5.88 0
4 -4 0 351.67 5.91 0
-4 -4 0 363.86 4.37 0
-4 4 0 366.88 6.01 0
4 4 0 357.43 4.38 0
5 -4 0 79.87 3.80 0
-5 -4 0 76.27 2.32 0
5 4 0 81.75 2.92 0
-5 4 0 77.12 3.40 0
6 -4 0 118.26 3.81 0
-6 -4 0 126.07 2.99 0
6 4 0 121.81 2.64 0
7 4 0 37.66 2.43 0
7 -4 0 36.75 2.87 0
7 -4 0 39.36 3.07 0
-7 -4 0 41.45 1.86 0
-8 -4 0 18.61 2.17 0
8 -4 0 19.70 2.74 0
8 -4 0 20.33 2.44 0
8 4 0 17.32 2.21 0
9 -4 0 92.30 3.83 0
-9 -4 0 90.54 2.73 0
9 4 0 84.54 2.67 0
9 -4 0 85.00 3.70 0
-10 -4 0 67.61 2.57 0
10 -4 0 63.33 3.39 0
10 -4 0 63.96 3.48 0
10 4 0 62.77 2.53 0
11 4 0 5.80 2.12 0
11 -4 0 5.46 2.65 0
-11 -4 0 7.36 2.01 0
11 -4 0 7.76 2.77 0
12 -4 0 5.91 2.74 0
-12 -4 0 3.15 1.99 0
12 -4 0 6.01 2.59 0
12 4 0 2.74 2.13 0
13 -4 0 10.02 2.62 0
-13 -4 0 6.68 2.04 0
13 4 0 6.99 2.12 0
13 -4 0 9.03 2.73 0
14 -4 0 99.38 3.83 0
14 -4 0 100.82 3.81 0
-14 -4 0 95.71 2.83 0
14 4 0 96.74 2.80 0
-15 -4 0 66.15 2.69 0
15 -4 0 63.00 3.59 0
15 4 0 62.20 2.68 0
15 -4 0 60.59 3.58 0
16 -4 0 0.94 2.79 0
16 -4 0 -0.16 2.85 0
16 4 0 2.97 2.24 0
-16 -4 0 -1.29 2.39 0
17 -4 0 -0.17 2.87 0
17 4 0 1.72 1.67 0
17 -4 0 0.60 3.00 0
-17 -4 0 -0.56 1.66 0
18 -4 0 1.30 3.15 0
18 4 0 1.55 2.46 0
-18 -4 0 3.45 2.32 0
18 -4 0 2.02 3.10 0
19 -4 0 29.93 3.96 0
19 4 0 29.30 2.69 0
19 -4 0 29.82 3.49 0
-19 -4 0 27.03 2.73 0
20 4 0 4.35 2.55 0
20 -4 0 2.18 3.97 0
20 -4 0 3.31 3.49 0
-20 -4 0 2.87 2.51 0
21 4 0 7.13 2.85 0
-21 -4 0 6.16 2.69 0
21 -4 0 3.99 4.07 0
21 -4 0 5.67 4.10 0
22 4 0 4.54 2.88 0
22 -4 0 5.76 4.87 0
-22 -4 0 6.36 2.94 0
22 -4 0 4.01 4.85 0
-23 -4 0 4.43 3.10 0
23 -4 0 4.93 6.15 0
23 4 0 2.97 3.16 0
23 -4 0 3.77 6.13 0
24 4 0 2.17 3.38 0
-24 -4 0 2.77 3.29 0
1 5 0 709.64 6.22 0
-1 -5 0 692.65 6.01 0
-1 5 0 693.21 6.55 0
1 -5 0 720.76 6.53 0
-2 -5 0 540.57 5.19 0
-2 5 0 550.29 6.03 0
2 -5 0 533.27 5.94 0
2 5 0 566.54 5.50 0
3 5 0 1456.91 8.15 0
3 -5 0 1450.18 9.66 0
-3 5 0 1407.43 9.50 0
-3 -5 0 1437.76 8.07 0
-4 -5 0 127.17 3.13 0
-4 5 0 131.12 3.65 0
4 5 0 132.15 2.79 0
4 -5 0 131.12 3.63 0
5 -5 0 81.47 3.46 0
-5 -5 0 78.14 2.25 0
-5 5 0 76.55 3.09 0
5 5 0 79.59 2.32 0
6 5 0 68.20 2.58 0
-6 -5 0 72.89 2.57 0
6 -5 0 65.79 2.98 0
-6 5 0 67.62 2.94 0
-7 -5 0 584.25 4.87 0
7 -5 0 631.13 7.15 0
7 5 0 621.00 5.06 0
8 -5 0 34.08 3.02 0
8 5 0 39.62 2.40 0
-8 -5 0 34.77 2.23 0
9 -5 0 60.20 3.35 0
9 -5 0 57.72 3.20 0
-9 -5 0 61.40 2.40 0
9 5 0 59.69 2.01 0
-10 -5 0 7.07 1.99 0
10 -5 0 5.52 2.30 0
10 5 0 6.50 1.50 0
10 -5 0 9.14 2.83 0
-11 -5 0 42.17 2.30 0
11 -5 0 42.50 3.34 0
11 5 0 44.97 2.34 0
11 -5 0 39.52 3.13 0
12 -5 0 54.66 3.36 0
12 -5 0 56.13 3.16 0
12 5 0 54.61 2.39 0
-12 -5 0 54.67 2.34 0
-13 -5 0 3.49 1.47 0
13 5 0 1.27 2.09 0
13 -5 0 4.59 2.77 0
13 -5 0 3.14 2.68 0
-14 -5 0 11.75 2.23 0
14 -5 0 8.52 3.06 0
14 5 0 8.93 2.16 0
14 -5 0 8.88 2.89 0
-15 -5 0 1.96 2.31 0
15 -5 0 1.51 2.86 0
15 -5 0 2.52 3.23 0
15 5 0 -0.65 2.35 0
16 -5 0 3.20 3.18 0
16 -5 0 3.09 2.92 0
-16 -5 0 2.52 1.58 0
16 5 0 1.64 2.35 0
17 -5 0 -0.84 3.53 0
17 -5 0 1.13 3.63 0
17 5 0 1.59 2.36 0
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-5 10 8 -1.03 4.16 0
5 10 8 3.18 2.47 0
5 -10 8 1.01 2.35 0
-5 -10 8 2.34 2.28 0
5 -10 8 2.34 3.23 0
-6 10 8 -1.15 4.46 0
-6 10 8 1.53 4.33 0
6 10 8 4.70 3.33 0
6 -10 8 1.44 3.37 0
6 -10 8 1.39 2.37 0
-6 -10 8 2.56 3.33 0
-1 11 8 1.09 3.39 0
1 11 8 0.21 3.39 0
1 -11 8 -3.38 2.43 0
-1 -11 8 -2.12 2.42 0
-2 11 8 -0.89 3.38 0
2 11 8 5.20 3.46 0
2 -11 8 1.88 3.43 0
-2 -11 8 2.32 3.21 0
-2 11 8 1.36 3.55 0
-3 11 8 0.63 4.25 0
3 11 8 -1.38 3.57 0
-3 -11 8 -1.81 3.25 0
3 -11 8 3.40 2.40 0
-3 11 8 1.71 3.51 0
2 0 9 9.40 3.17 0
-2 0 9 3.70 3.19 0
2 0 9 4.63 3.06 0
-2 0 9 1.46 3.07 0
4 0 9 -0.67 2.25 0
-4 0 9 1.12 3.14 0
4 0 9 -0.83 3.18 0
-4 0 9 -0.94 3.14 0
6 0 9 0.11 3.25 0
6 0 9 0.39 3.15 0
-6 0 9 0.00 3.26 0
-6 0 9 4.04 3.22 0
8 0 9 7.12 3.66 0
8 0 9 12.21 3.31 0
-8 0 9 8.75 3.54 0
-8 0 9 11.74 3.47 0
0 1 9 0.27 3.16 0
0 -1 9 5.39 3.17 0
0 1 9 4.03 2.97 0
0 -1 9 1.65 2.10 0
1 1 9 2.18 3.12 0
-1 1 9 0.83 3.16 0
1 -1 9 3.23 3.16 0
-1 -1 9 3.56 3.12 0
1 1 9 -1.62 3.09 0
-1 1 9 0.21 3.13 0
1 -1 9 -1.64 3.06 0
-1 -1 9 -1.82 3.11 0
2 1 9 4.01 3.19 0
2 -1 9 -0.39 3.16 0
-2 1 9 -1.18 3.13 0
-2 -1 9 2.58 3.10 0
2 1 9 5.01 3.13 0
-2 1 9 0.93 3.19 0
2 -1 9 4.05 2.99 0
-2 -1 9 4.95 3.23 0
3 1 9 0.88 3.21 0
3 -1 9 3.22 3.13 0
-3 1 9 2.06 3.19 0
-3 -1 9 0.34 2.27 0
3 1 9 4.50 3.04 0
-3 1 9 7.38 3.06 0
3 -1 9 1.09 3.10 0
-3 -1 9 3.31 3.05 0
4 1 9 1.30 3.38 0
4 -1 9 -1.86 3.17 0
-4 1 9 2.36 2.36 0
4 1 9 0.27 3.29 0
-4 -1 9 2.30 3.12 0
-4 1 9 1.25 3.23 0
4 -1 9 3.07 3.12 0
-4 -1 9 -0.14 2.28 0
5 1 9 1.62 3.34 0
5 -1 9 3.37 3.18 0
5 1 9 2.30 3.21 0
-5 1 9 2.20 3.32 0
-5 -1 9 4.09 3.23 0
-5 1 9 9.42 3.27 0
5 -1 9 9.92 3.25 0
-5 -1 9 2.00 3.22 0
6 1 9 6.32 3.31 0
6 -1 9 7.11 3.42 0
6 1 9 6.02 2.95 0
-6 1 9 4.40 3.30 0
-6 -1 9 3.54 3.22 0
6 -1 9 1.77 3.32 0
-6 1 9 3.05 3.27 0
-6 -1 9 4.14 3.35 0
7 1 9 2.94 3.39 0
7 -1 9 1.34 3.23 0
7 1 9 2.41 3.36 0
-7 1 9 -0.16 3.39 0
-7 -1 9 1.28 3.28 0
7 -1 9 -1.60 3.15 0
-7 1 9 1.25 3.25 0
-7 -1 9 -1.46 3.23 0
8 1 9 4.95 3.44 0
8 -1 9 7.46 3.45 0
8 1 9 8.53 3.39 0
8 -1 9 6.81 2.41 0
-8 1 9 6.56 3.65 0
-8 1 9 4.48 4.37 0
-8 -1 9 4.42 3.51 0
-8 -1 9 6.02 3.44 0
1 2 9 4.22 3.12 0
-1 2 9 -0.16 3.14 0
1 -2 9 0.58 3.10 0
1 2 9 3.09 3.14 0
-1 -2 9 1.94 2.18 0
-1 2 9 1.85 3.10 0
1 -2 9 3.12 3.03 0
-1 -2 9 4.05 3.07 0
-2 -2 9 -3.75 3.21 0
2 2 9 3.61 3.19 0
-2 2 9 3.14 3.19 0
2 -2 9 4.03 3.15 0
2 2 9 4.46 3.16 0
-2 -2 9 0.47 3.13 0
-2 2 9 -3.34 3.10 0
2 -2 9 4.52 2.99 0
-3 -2 9 -1.36 3.26 0
3 2 9 0.27 3.14 0
3 -2 9 5.38 3.21 0
-3 2 9 2.66 2.36 0
3 2 9 4.78 3.12 0
-3 2 9 6.02 3.19 0
-3 -2 9 0.38 3.19 0
3 -2 9 7.29 3.04 0
4 2 9 6.20 2.33 0
-4 -2 9 3.35 3.16 0
4 -2 9 4.61 2.38 0
4 2 9 7.13 3.24 0
-4 2 9 1.70 3.17 0
-4 2 9 7.91 3.22 0
-4 -2 9 1.38 3.30 0
4 -2 9 5.26 3.21 0
5 2 9 -0.42 2.43 0
5 2 9 2.51 3.16 0
5 -2 9 1.65 2.38 0
-5 -2 9 6.75 3.27 0
-5 2 9 2.49 3.28 0
-5 2 9 -1.45 3.38 0
-5 -2 9 5.61 3.28 0
5 -2 9 2.95 2.30 0
6 2 9 4.38 2.40 0
6 2 9 0.41 3.33 0
6 -2 9 3.39 2.29 0
-6 -2 9 1.31 3.24 0
-6 2 9 0.63 3.39 0
-6 2 9 1.98 3.39 0
-6 -2 9 2.36 3.29 0
6 -2 9 6.35 2.32 0
7 2 9 5.15 2.53 0
7 2 9 4.78 3.45 0
7 -2 9 -1.81 2.40 0
-7 -2 9 4.40 3.30 0
-7 2 9 4.93 4.18 0
-7 2 9 7.01 3.39 0
-7 -2 9 6.46 3.41 0
7 -2 9 8.77 3.21 0
8 2 9 2.33 3.37 0
8 -2 9 0.04 3.43 0
-8 -2 9 -0.61 3.32 0
-8 2 9 4.37 4.24 0
-8 2 9 -0.49 3.46 0
8 -2 9 0.85 3.38 0
-8 -2 9 2.21 3.38 0
8 2 9 4.66 3.34 0
0 3 9 3.57 2.22 0
0 3 9 4.34 3.21 0
0 -3 9 4.24 3.11 0
0 -3 9 7.38 3.25 0
1 -3 9 1.87 2.19 0
1 3 9 1.57 2.19 0
1 3 9 2.57 3.23 0
-1 3 9 0.26 3.27 0
-1 3 9 -1.63 3.16 0
-1 -3 9 2.62 3.16 0
1 -3 9 3.36 2.26 0
-1 -3 9 0.46 3.21 0
2 3 9 7.75 3.18 0
2 3 9 6.75 3.19 0
-2 3 9 10.68 3.23 0
-2 3 9 7.94 3.26 0
2 -3 9 5.18 3.20 0
-2 -3 9 7.36 3.26 0
-2 -3 9 7.11 3.22 0
2 -3 9 4.59 2.17 0
3 3 9 2.91 3.17 0
3 3 9 2.51 2.25 0
-3 3 9 1.21 3.17 0
-3 3 9 3.25 3.20 0
3 -3 9 2.30 2.32 0
-3 -3 9 1.79 2.34 0
-3 -3 9 1.63 3.27 0
3 -3 9 3.06 2.21 0
4 3 9 -3.09 3.10 0
4 3 9 -1.43 3.23 0
-4 3 9 0.34 2.29 0
4 -3 9 2.37 3.24 0
-4 3 9 1.69 3.24 0
-4 -3 9 5.28 3.32 0
-4 -3 9 2.46 3.17 0
4 -3 9 5.22 3.15 0
5 3 9 -0.13 3.30 0
-5 3 9 3.56 3.34 0
5 -3 9 3.41 3.31 0
-5 3 9 2.30 3.30 0
-5 -3 9 3.43 3.26 0
-5 -3 9 1.38 3.21 0
5 -3 9 2.69 3.28 0
5 3 9 0.40 3.12 0
6 3 9 6.13 3.40 0
-6 3 9 2.20 3.35 0
6 -3 9 3.28 3.30 0
-6 3 9 1.74 3.34 0
-6 -3 9 2.01 3.46 0
-6 -3 9 2.67 3.28 0
6 -3 9 3.39 3.19 0
6 3 9 2.88 3.36 0
7 3 9 0.45 2.41 0
-7 3 9 4.33 4.31 0
7 -3 9 -0.12 3.39 0
-7 3 9 -2.78 3.57 0
-7 -3 9 0.90 3.43 0
-7 -3 9 -1.74 3.37 0
7 -3 9 -1.58 2.35 0
7 3 9 1.43 3.38 0
1 4 9 2.61 3.19 0
-1 4 9 2.36 3.17 0
1 -4 9 -1.33 3.14 0
-1 -4 9 -0.62 2.15 0
1 -4 9 3.12 3.22 0
-1 -4 9 1.67 3.16 0
1 4 9 -0.68 2.25 0
-1 4 9 -0.98 3.17 0
2 4 9 1.81 3.24 0
-2 4 9 1.06 2.30 0
2 -4 9 1.65 3.16 0
2 -4 9 3.17 2.30 0
-2 -4 9 0.98 2.34 0
-2 -4 9 1.34 2.28 0
2 4 9 1.90 3.27 0
-2 4 9 2.92 3.28 0
3 4 9 2.94 3.34 0
3 -4 9 7.02 3.20 0
-3 4 9 2.74 3.31 0
3 -4 9 -3.60 3.05 0
-3 -4 9 1.41 3.29 0
-3 -4 9 2.45 3.14 0
3 4 9 2.43 3.28 0
-3 4 9 2.98 3.26 0
4 4 9 0.85 3.25 0
4 -4 9 1.75 3.29 0
-4 4 9 -1.24 3.29 0
4 -4 9 2.29 3.35 0
-4 -4 9 2.59 3.31 0
-4 -4 9 3.44 3.27 0
4 4 9 6.56 3.39 0
-4 4 9 3.20 3.28 0
5 4 9 3.59 3.39 0
5 -4 9 -1.10 3.29 0
-5 4 9 0.79 3.40 0
-5 -4 9 1.67 2.61 0
-5 -4 9 7.68 3.21 0
5 4 9 0.77 3.29 0
-5 4 9 1.36 3.30 0
5 -4 9 3.17 2.14 0
6 -4 9 3.65 3.47 0
-6 4 9 5.41 3.61 0
-6 -4 9 2.99 3.45 0
6 -4 9 6.73 3.35 0
6 4 9 5.26 3.46 0
-6 -4 9 7.87 3.38 0
-6 4 9 3.11 4.32 0
6 4 9 9.29 3.34 0
-7 4 9 5.41 4.39 0
-7 -4 9 9.86 3.53 0
7 -4 9 8.01 3.41 0
7 4 9 12.37 3.30 0
-7 4 9 7.55 3.49 0
-7 -4 9 7.05 3.49 0
7 4 9 1.91 3.44 0
0 5 9 0.67 3.35 0
0 -5 9 5.70 3.22 0
0 -5 9 5.89 3.38 0
0 5 9 7.82 3.24 0
1 5 9 3.00 3.39 0
-1 5 9 4.09 3.36 0
1 -5 9 2.95 3.07 0
-1 -5 9 3.94 3.20 0
1 -5 9 1.50 2.14 0
-1 -5 9 4.61 3.29 0
1 5 9 4.93 3.44 0
-1 5 9 5.83 3.28 0
2 5 9 2.24 2.37 0
-2 5 9 2.21 3.35 0
2 -5 9 1.06 3.20 0
-2 -5 9 6.55 3.22 0
2 -5 9 5.18 3.28 0
2 5 9 1.60 2.37 0
-2 5 9 3.61 3.14 0
-2 -5 9 6.80 3.44 0
-3 -5 9 3.92 3.28 0
3 5 9 2.23 3.46 0
-3 5 9 0.21 3.40 0
3 -5 9 1.08 3.28 0
3 -5 9 3.58 3.37 0
-3 -5 9 3.60 3.31 0
3 5 9 1.50 3.29 0
-3 5 9 0.66 3.31 0
4 5 9 4.75 3.39 0
-4 -5 9 1.17 2.26 0
-4 5 9 1.36 3.41 0
4 -5 9 -0.02 3.22 0
4 -5 9 1.75 2.33 0
-4 -5 9 0.70 2.43 0
-4 5 9 -0.69 3.44 0
4 5 9 2.89 3.33 0
5 -5 9 1.15 3.29 0
-5 -5 9 2.90 3.23 0
-5 5 9 0.17 3.47 0
5 -5 9 -0.19 2.44 0
-5 -5 9 1.01 3.42 0
5 5 9 0.75 3.25 0
-5 5 9 2.47 4.13 0
5 5 9 5.57 3.54 0
-6 -5 9 2.43 2.39 0
6 -5 9 1.61 2.37 0
-6 5 9 1.53 3.66 0
-6 -5 9 5.28 3.50 0
-6 5 9 3.58 3.56 0
6 5 9 0.74 3.34 0
6 -5 9 -1.14 2.43 0
1 6 9 5.21 3.48 0
-1 6 9 3.01 3.43 0
1 -6 9 0.97 3.29 0
-1 -6 9 7.01 3.36 0
-1 6 9 4.63 2.38 0
1 6 9 3.37 3.32 0
1 -6 9 4.43 2.32 0
-1 -6 9 4.49 2.34 0
2 6 9 1.85 2.42 0
-2 6 9 1.32 3.40 0
-2 -6 9 4.19 2.28 0
2 -6 9 3.57 3.37 0
-2 -6 9 1.55 2.29 0
2 -6 9 0.48 2.18 0
-2 6 9 0.65 3.38 0
2 6 9 3.29 3.41 0
-3 6 9 -1.26 3.43 0
3 -6 9 -0.34 2.43 0
-3 -6 9 2.34 3.39 0
-3 -6 9 2.49 2.43 0
3 -6 9 0.47 3.27 0
-3 6 9 -0.41 3.36 0
3 6 9 1.47 2.42 0
3 6 9 3.80 3.33 0
-4 6 9 1.08 3.40 0
4 -6 9 2.32 3.34 0
4 -6 9 3.17 3.25 0
-4 -6 9 2.18 3.32 0
-4 -6 9 -0.57 3.33 0
-4 6 9 3.84 3.40 0
4 6 9 2.46 3.44 0
4 6 9 3.72 3.38 0
0 7 9 -0.13 3.51 0
0 -7 9 1.10 2.29 0
0 -7 9 4.79 2.41 0
0 7 9 4.27 3.54 0
-1 -7 9 3.60 2.46 0
1 -7 9 3.54 3.29 0
-1 -7 9 -0.07 3.56 0
-1 7 9 1.77 3.46 0
1 7 9 4.30 3.34 0
1 -7 9 3.63 2.31 0
-2 7 9 3.33 3.38 0
;
_shelx_hkl_checksum 62008
_shelx_res_file
;
TITL shelxt_a.res in Pna2(1)
shelx.res
created by SHELXL-2018/3 at 13:34:45 on 04-Nov-2021
CELL 0.71073 17.3298 14.1856 6.5857 90.000 90.000 90.000
ZERR 4.00 0.0008 0.0007 0.0003 0.000 0.000 0.000
LATT -1
SYMM - X, - Y, 1/2 + Z
SYMM 1/2 + X, 1/2 - Y, Z
SYMM 1/2 - X, 1/2 + Y, 1/2 + Z
SFAC C H N O
UNIT 76 84 4 8
MERG 2
MORE -1
MPLA C1 C2 C3 C4 C5 C6
MPLA N1 C7 C8 C9 C10 C13
MPLA C14 C15 C16 C17 C18 C19
MPLA C1 C2 C3 C4 C5 C6
HTAB O2 O1
EQIV $1 -x-1, -y-1, z+1/2
HTAB O2 O1_$1
EQIV $2 x, y, z-1
HTAB C8 O2_$2
HTAB O2 O1_$1
HTAB C8 O2_$2
FMAP 2
PLAN 5
ACTA
BOND
BOND $H
CONF
LIST 6
L.S. 25
WGHT 0.051500
FVAR 0.82626
O1 4 -0.520680 -0.469008 -0.410318 11.00000 0.06539 0.04586 =
0.06861 0.00796 0.01281 0.01989
O2 4 -0.600740 -0.409449 -0.022768 11.00000 0.08108 0.06184 =
0.04001 0.00148 -0.00500 0.02709
AFIX 147
H2 2 -0.565229 -0.447609 -0.026638 11.00000 -1.50000
AFIX 0
N1 3 -0.585266 -0.200753 -0.482569 11.00000 0.04894 0.03681 =
0.04800 0.00044 0.00311 0.00236
C14 1 -0.694887 -0.212600 -0.249227 11.00000 0.04544 0.03694 =
0.04391 -0.00206 -0.00199 0.00369
C9 1 -0.547650 -0.393512 -0.458685 11.00000 0.04684 0.03830 =
0.03993 -0.00518 -0.00388 0.00443
C13 1 -0.618358 -0.254561 -0.313138 11.00000 0.04280 0.03764 =
0.03833 0.00054 -0.00311 0.00379
AFIX 13
H13 2 -0.582802 -0.250220 -0.197803 11.00000 -1.20000
AFIX 0
C6 1 -0.471254 -0.163389 -0.687224 11.00000 0.04836 0.04279 =
0.05369 -0.00276 0.00379 -0.00334
C10 1 -0.625081 -0.360749 -0.375559 11.00000 0.04240 0.03695 =
0.03719 0.00018 -0.00396 0.00297
C11 1 -0.647898 -0.421485 -0.192918 11.00000 0.05241 0.04254 =
0.04954 0.00495 0.00474 0.00465
AFIX 23
H11A 2 -0.700646 -0.406616 -0.155468 11.00000 -1.20000
H11B 2 -0.646451 -0.487258 -0.233009 11.00000 -1.20000
AFIX 0
C7 1 -0.505974 -0.227900 -0.529197 11.00000 0.04480 0.04685 =
0.04411 -0.00060 -0.00126 -0.00112
AFIX 13
H7 2 -0.474939 -0.224784 -0.404983 11.00000 -1.20000
AFIX 0
C19 1 -0.742088 -0.164747 -0.386073 11.00000 0.05494 0.04753 =
0.05213 0.00336 -0.00427 0.00921
AFIX 43
H19 2 -0.725854 -0.156467 -0.519485 11.00000 -1.20000
AFIX 0
C8 1 -0.507694 -0.329680 -0.605978 11.00000 0.04783 0.04650 =
0.05090 -0.00077 0.00608 0.00443
AFIX 23
H8A 2 -0.534221 -0.331932 -0.735585 11.00000 -1.20000
H8B 2 -0.455272 -0.351604 -0.626845 11.00000 -1.20000
AFIX 0
C12 1 -0.685098 -0.375612 -0.543331 11.00000 0.05357 0.04819 =
0.05068 -0.00643 -0.01168 0.00168
AFIX 137
H12A 2 -0.674874 -0.333097 -0.653506 11.00000 -1.50000
H12B 2 -0.735741 -0.363652 -0.490172 11.00000 -1.50000
H12C 2 -0.682287 -0.439401 -0.591446 11.00000 -1.50000
AFIX 0
C15 1 -0.720361 -0.221772 -0.052048 11.00000 0.05936 0.06000 =
0.04713 0.00215 0.00231 0.01205
AFIX 43
H15 2 -0.688985 -0.251458 0.043011 11.00000 -1.20000
AFIX 0
C18 1 -0.812596 -0.129561 -0.325690 11.00000 0.05835 0.05270 =
0.08034 0.00337 -0.01103 0.01748
AFIX 43
H18 2 -0.843205 -0.097262 -0.418500 11.00000 -1.20000
AFIX 0
C1 1 -0.512070 -0.137488 -0.859548 11.00000 0.07352 0.06114 =
0.05440 0.00332 -0.00751 -0.02077
AFIX 43
H1A 2 -0.562927 -0.157131 -0.875089 11.00000 -1.20000
AFIX 0
C17 1 -0.838308 -0.141743 -0.128794 11.00000 0.05177 0.06041 =
0.09541 -0.01212 0.01012 0.01405
AFIX 43
H17 2 -0.886403 -0.119157 -0.089324 11.00000 -1.20000
AFIX 0
C3 1 -0.403164 -0.052952 -0.986537 11.00000 0.08056 0.05331 =
0.08507 0.01537 0.02717 0.00093
AFIX 43
H3 2 -0.379964 -0.017017 -1.087645 11.00000 -1.20000
AFIX 0
C16 1 -0.791742 -0.187684 0.007461 11.00000 0.06823 0.07482 =
0.06317 -0.00501 0.01758 0.01047
AFIX 43
H16 2 -0.808210 -0.195995 0.140665 11.00000 -1.20000
AFIX 0
C2 1 -0.478086 -0.082861 -1.008386 11.00000 0.09796 0.06307 =
0.05396 0.00605 -0.00300 -0.01504
AFIX 43
H2A 2 -0.505992 -0.066302 -1.123614 11.00000 -1.20000
AFIX 0
C5 1 -0.396766 -0.130626 -0.667309 11.00000 0.04588 0.07461 =
0.09397 0.02830 -0.00487 -0.00346
AFIX 43
H5 2 -0.368693 -0.145511 -0.551306 11.00000 -1.20000
AFIX 0
C4 1 -0.363174 -0.076164 -0.816436 11.00000 0.05331 0.08240 =
0.11852 0.03654 0.00551 -0.00987
AFIX 43
H4 2 -0.312707 -0.055149 -0.800405 11.00000 -1.20000
AFIX 0
H1 2 -0.590208 -0.139578 -0.450440 11.00000 -1.20000
HKLF 4
REM shelxt_a.res in Pna2(1)
REM wR2 = 0.0964, GooF = S = 1.014, Restrained GooF = 1.014 for all data
REM R1 = 0.0414 for 3441 Fo > 4sig(Fo) and 0.0617 for all 4763 data
REM 204 parameters refined using 1 restraints
END
WGHT 0.0510 0.0000
REM Highest difference peak 0.156, deepest hole -0.192, 1-sigma level 0.035
Q1 1 -0.7064 -0.3193 -0.0599 11.00000 0.05 0.11
Q2 1 -0.7185 -0.3154 -0.5670 11.00000 0.05 0.11
Q3 1 -0.7866 -0.2835 -0.5394 11.00000 0.05 0.10
Q4 1 -0.9012 -0.0996 -0.1515 11.00000 0.05 0.10
Q5 1 -0.7133 -0.3215 -0.8257 11.00000 0.05 0.09
;
_shelx_res_checksum 920
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'
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 -0.52068(8) -0.46901(9) -0.4103(2) 0.0600(4) Uani d 1 . .
O O2 -0.60074(9) -0.40945(10) -0.0228(2) 0.0610(4) Uani d 1 . .
H H2 -0.565229 -0.447609 -0.026638 0.091 Uiso calc 1 . .
N N1 -0.58527(9) -0.20075(10) -0.4826(2) 0.0446(3) Uani d 1 . .
C C14 -0.69489(10) -0.21260(11) -0.2492(3) 0.0421(4) Uani d 1 . .
C C9 -0.54765(10) -0.39351(11) -0.4587(3) 0.0417(4) Uani d 1 . .
C C13 -0.61836(10) -0.25456(10) -0.3131(3) 0.0396(3) Uani d 1 . .
H H13 -0.582802 -0.250220 -0.197803 0.048 Uiso calc 1 . .
C C6 -0.47125(11) -0.16339(12) -0.6872(3) 0.0483(4) Uani d 1 . .
C C10 -0.62508(9) -0.36075(11) -0.3756(3) 0.0388(3) Uani d 1 . .
C C11 -0.64790(12) -0.42148(12) -0.1929(3) 0.0482(4) Uani d 1 . .
H H11A -0.700646 -0.406616 -0.155468 0.058 Uiso calc 1 . .
H H11B -0.646451 -0.487258 -0.233009 0.058 Uiso calc 1 . .
C C7 -0.50597(10) -0.22790(12) -0.5292(3) 0.0453(4) Uani d 1 . .
H H7 -0.474939 -0.224784 -0.404983 0.054 Uiso calc 1 . .
C C19 -0.74209(11) -0.16475(13) -0.3861(3) 0.0515(4) Uani d 1 . .
H H19 -0.725854 -0.156467 -0.519485 0.062 Uiso calc 1 . .
C C8 -0.50769(11) -0.32968(13) -0.6060(3) 0.0484(4) Uani d 1 . .
H H8A -0.534221 -0.331932 -0.735585 0.058 Uiso calc 1 . .
H H8B -0.455272 -0.351604 -0.626845 0.058 Uiso calc 1 . .
C C12 -0.68510(11) -0.37561(13) -0.5433(3) 0.0508(4) Uani d 1 . .
H H12A -0.674874 -0.333097 -0.653506 0.076 Uiso calc 1 . .
H H12B -0.735741 -0.363652 -0.490172 0.076 Uiso calc 1 . .
H H12C -0.682287 -0.439401 -0.591446 0.076 Uiso calc 1 . .
C C15 -0.72036(12) -0.22177(14) -0.0520(3) 0.0555(5) Uani d 1 . .
H H15 -0.688985 -0.251458 0.043011 0.067 Uiso calc 1 . .
C C18 -0.81260(13) -0.12956(14) -0.3257(4) 0.0638(6) Uani d 1 . .
H H18 -0.843205 -0.097262 -0.418500 0.077 Uiso calc 1 . .
C C1 -0.51207(14) -0.13749(15) -0.8595(4) 0.0630(5) Uani d 1 . .
H H1A -0.562927 -0.157131 -0.875089 0.076 Uiso calc 1 . .
C C17 -0.83831(13) -0.14174(16) -0.1288(4) 0.0692(6) Uani d 1 . .
H H17 -0.886403 -0.119157 -0.089324 0.083 Uiso calc 1 . .
C C3 -0.40316(15) -0.05295(15) -0.9865(4) 0.0730(7) Uani d 1 . .
H H3 -0.379964 -0.017017 -1.087645 0.088 Uiso calc 1 . .
C C16 -0.79174(14) -0.18768(16) 0.0075(4) 0.0687(6) Uani d 1 . .
H H16 -0.808210 -0.195995 0.140665 0.082 Uiso calc 1 . .
C C2 -0.47809(16) -0.08286(16) -1.0084(4) 0.0717(6) Uani d 1 . .
H H2A -0.505992 -0.066302 -1.123614 0.086 Uiso calc 1 . .
C C5 -0.39677(12) -0.13063(17) -0.6673(5) 0.0715(7) Uani d 1 . .
H H5 -0.368693 -0.145511 -0.551306 0.086 Uiso calc 1 . .
C C4 -0.36317(14) -0.07616(19) -0.8164(5) 0.0847(9) Uani d 1 . .
H H4 -0.312707 -0.055149 -0.800405 0.102 Uiso calc 1 . .
H H1 -0.5902(17) -0.140(2) -0.450(5) 0.102 Uiso d 1 . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
O1 0.0654(9) 0.0459(7) 0.0686(9) 0.0199(6) 0.0128(8) 0.0080(6)
O2 0.0811(10) 0.0618(7) 0.0400(7) 0.0271(7) -0.0050(7) 0.0015(6)
N1 0.0489(8) 0.0368(6) 0.0480(9) 0.0024(6) 0.0031(7) 0.0004(6)
C14 0.0454(9) 0.0369(7) 0.0439(9) 0.0037(7) -0.0020(8) -0.0021(6)
C9 0.0468(9) 0.0383(7) 0.0399(8) 0.0044(7) -0.0039(7) -0.0052(6)
C13 0.0428(9) 0.0376(7) 0.0383(8) 0.0038(6) -0.0031(7) 0.0005(7)
C6 0.0484(10) 0.0428(8) 0.0537(11) -0.0033(7) 0.0038(9) -0.0028(8)
C10 0.0424(8) 0.0370(7) 0.0372(8) 0.0030(6) -0.0040(7) 0.0002(6)
C11 0.0524(10) 0.0425(8) 0.0495(10) 0.0046(7) 0.0047(9) 0.0050(7)
C7 0.0448(9) 0.0468(8) 0.0441(9) -0.0011(7) -0.0013(8) -0.0006(8)
C19 0.0549(11) 0.0475(9) 0.0521(10) 0.0092(8) -0.0043(9) 0.0034(8)
C8 0.0478(10) 0.0465(9) 0.0509(10) 0.0044(8) 0.0061(8) -0.0008(8)
C12 0.0536(11) 0.0482(9) 0.0507(10) 0.0017(8) -0.0117(9) -0.0064(8)
C15 0.0594(11) 0.0600(10) 0.0471(11) 0.0121(9) 0.0023(9) 0.0022(9)
C18 0.0584(12) 0.0527(10) 0.0803(16) 0.0175(9) -0.0110(11) 0.0034(11)
C1 0.0735(14) 0.0611(11) 0.0544(12) -0.0208(10) -0.0075(11) 0.0033(10)
C17 0.0518(12) 0.0604(11) 0.0954(19) 0.0141(10) 0.0101(13) -0.0121(12)
C3 0.0806(16) 0.0533(10) 0.0851(18) 0.0009(10) 0.0272(14) 0.0154(12)
C16 0.0682(13) 0.0748(13) 0.0632(14) 0.0105(11) 0.0176(12) -0.0050(11)
C2 0.0980(17) 0.0631(12) 0.0540(13) -0.0150(12) -0.0030(12) 0.0060(11)
C5 0.0459(12) 0.0746(14) 0.0940(19) -0.0035(10) -0.0049(12) 0.0283(14)
C4 0.0533(13) 0.0824(16) 0.119(3) -0.0099(11) 0.0055(15) 0.0365(17)
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
C11 O2 H2 . . 109.5 ?
C7 N1 C13 . . 112.98(14) ?
C7 N1 H1 . . 113.2(19) ?
C13 N1 H1 . . 107(2) ?
C15 C14 C19 . . 117.87(17) ?
C15 C14 C13 . . 120.38(16) ?
C19 C14 C13 . . 121.74(17) ?
O1 C9 C8 . . 121.79(16) ?
O1 C9 C10 . . 121.04(16) ?
C8 C9 C10 . . 117.15(14) ?
N1 C13 C14 . . 110.43(13) ?
N1 C13 C10 . . 109.24(13) ?
C14 C13 C10 . . 112.72(13) ?
N1 C13 H13 . . 108.1 ?
C14 C13 H13 . . 108.1 ?
C10 C13 H13 . . 108.1 ?
C5 C6 C1 . . 117.8(2) ?
C5 C6 C7 . . 120.78(19) ?
C1 C6 C7 . . 121.40(17) ?
C9 C10 C12 . . 107.29(14) ?
C9 C10 C11 . . 109.78(14) ?
C12 C10 C11 . . 108.28(15) ?
C9 C10 C13 . . 108.82(13) ?
C12 C10 C13 . . 111.86(13) ?
C11 C10 C13 . . 110.75(14) ?
O2 C11 C10 . . 114.21(15) ?
O2 C11 H11A . . 108.7 ?
C10 C11 H11A . . 108.7 ?
O2 C11 H11B . . 108.7 ?
C10 C11 H11B . . 108.7 ?
H11A C11 H11B . . 107.6 ?
N1 C7 C6 . . 111.10(15) ?
N1 C7 C8 . . 107.46(14) ?
C6 C7 C8 . . 110.59(16) ?
N1 C7 H7 . . 109.2 ?
C6 C7 H7 . . 109.2 ?
C8 C7 H7 . . 109.2 ?
C18 C19 C14 . . 120.7(2) ?
C18 C19 H19 . . 119.7 ?
C14 C19 H19 . . 119.7 ?
C9 C8 C7 . . 111.45(15) ?
C9 C8 H8A . . 109.3 ?
C7 C8 H8A . . 109.3 ?
C9 C8 H8B . . 109.3 ?
C7 C8 H8B . . 109.3 ?
H8A C8 H8B . . 108.0 ?
C10 C12 H12A . . 109.5 ?
C10 C12 H12B . . 109.5 ?
H12A C12 H12B . . 109.5 ?
C10 C12 H12C . . 109.5 ?
H12A C12 H12C . . 109.5 ?
H12B C12 H12C . . 109.5 ?
C14 C15 C16 . . 121.3(2) ?
C14 C15 H15 . . 119.3 ?
C16 C15 H15 . . 119.3 ?
C19 C18 C17 . . 120.7(2) ?
C19 C18 H18 . . 119.6 ?
C17 C18 H18 . . 119.6 ?
C2 C1 C6 . . 120.8(2) ?
C2 C1 H1A . . 119.6 ?
C6 C1 H1A . . 119.6 ?
C16 C17 C18 . . 118.9(2) ?
C16 C17 H17 . . 120.5 ?
C18 C17 H17 . . 120.5 ?
C4 C3 C2 . . 119.6(2) ?
C4 C3 H3 . . 120.2 ?
C2 C3 H3 . . 120.2 ?
C17 C16 C15 . . 120.4(2) ?
C17 C16 H16 . . 119.8 ?
C15 C16 H16 . . 119.8 ?
C3 C2 C1 . . 120.1(3) ?
C3 C2 H2A . . 119.9 ?
C1 C2 H2A . . 119.9 ?
C4 C5 C6 . . 121.1(2) ?
C4 C5 H5 . . 119.4 ?
C6 C5 H5 . . 119.4 ?
C3 C4 C5 . . 120.5(2) ?
C3 C4 H4 . . 119.7 ?
C5 C4 H4 . . 119.7 ?
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 C9 . 1.211(2) ?
O2 C11 . 1.397(2) ?
O2 H2 . 0.8200 ?
N1 C7 . 1.460(2) ?
N1 C13 . 1.469(2) ?
N1 H1 . 0.90(3) ?
C14 C15 . 1.378(3) ?
C14 C19 . 1.394(3) ?
C14 C13 . 1.513(2) ?
C9 C8 . 1.497(3) ?
C9 C10 . 1.522(2) ?
C13 C10 . 1.566(2) ?
C13 H13 . 0.9800 ?
C6 C5 . 1.378(3) ?
C6 C1 . 1.387(3) ?
C6 C7 . 1.511(3) ?
C10 C12 . 1.532(3) ?
C10 C11 . 1.531(2) ?
C11 H11A . 0.9700 ?
C11 H11B . 0.9700 ?
C7 C8 . 1.530(3) ?
C7 H7 . 0.9800 ?
C19 C18 . 1.379(3) ?
C19 H19 . 0.9300 ?
C8 H8A . 0.9700 ?
C8 H8B . 0.9700 ?
C12 H12A . 0.9600 ?
C12 H12B . 0.9600 ?
C12 H12C . 0.9600 ?
C15 C16 . 1.385(3) ?
C15 H15 . 0.9300 ?
C18 C17 . 1.382(4) ?
C18 H18 . 0.9300 ?
C1 C2 . 1.381(3) ?
C1 H1A . 0.9300 ?
C17 C16 . 1.372(4) ?
C17 H17 . 0.9300 ?
C3 C4 . 1.358(4) ?
C3 C2 . 1.374(4) ?
C3 H3 . 0.9300 ?
C16 H16 . 0.9300 ?
C2 H2A . 0.9300 ?
C5 C4 . 1.379(4) ?
C5 H5 . 0.9300 ?
C4 H4 . 0.9300 ?
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
O2 H2 O1 2_445 0.82 2.05 2.8194(18) 156.1 yes
C8 H8A O2 1_554 0.97 2.47 3.379(3) 155.3 yes
N1 H1 C3 2_455 0.90(3) 2.75(3) 3.605(2) 161(3) 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
C7 N1 C13 C14 . . . . 170.51(14) ?
C7 N1 C13 C10 . . . . -64.98(17) ?
C15 C14 C13 N1 . . . . -152.01(17) ?
C19 C14 C13 N1 . . . . 28.7(2) ?
C15 C14 C13 C10 . . . . 85.5(2) ?
C19 C14 C13 C10 . . . . -93.80(19) ?
O1 C9 C10 C12 . . . . -102.5(2) ?
C8 C9 C10 C12 . . . . 75.99(19) ?
O1 C9 C10 C11 . . . . 15.0(2) ?
C8 C9 C10 C11 . . . . -166.55(15) ?
O1 C9 C10 C13 . . . . 136.33(17) ?
C8 C9 C10 C13 . . . . -45.2(2) ?
N1 C13 C10 C9 . . . . 50.76(17) ?
C14 C13 C10 C9 . . . . 173.93(15) ?
N1 C13 C10 C12 . . . . -67.59(18) ?
C14 C13 C10 C12 . . . . 55.57(19) ?
N1 C13 C10 C11 . . . . 171.52(14) ?
C14 C13 C10 C11 . . . . -65.32(18) ?
C9 C10 C11 O2 . . . . 67.49(18) ?
C12 C10 C11 O2 . . . . -175.68(14) ?
C13 C10 C11 O2 . . . . -52.70(19) ?
C13 N1 C7 C6 . . . . -173.39(15) ?
C13 N1 C7 C8 . . . . 65.51(18) ?
C5 C6 C7 N1 . . . . 137.2(2) ?
C1 C6 C7 N1 . . . . -44.8(2) ?
C5 C6 C7 C8 . . . . -103.5(2) ?
C1 C6 C7 C8 . . . . 74.5(2) ?
C15 C14 C19 C18 . . . . -1.2(3) ?
C13 C14 C19 C18 . . . . 178.07(17) ?
O1 C9 C8 C7 . . . . -133.78(19) ?
C10 C9 C8 C7 . . . . 47.8(2) ?
N1 C7 C8 C9 . . . . -54.0(2) ?
C6 C7 C8 C9 . . . . -175.41(15) ?
C19 C14 C15 C16 . . . . 2.3(3) ?
C13 C14 C15 C16 . . . . -177.03(19) ?
C14 C19 C18 C17 . . . . -0.6(3) ?
C5 C6 C1 C2 . . . . 1.8(3) ?
C7 C6 C1 C2 . . . . -176.3(2) ?
C19 C18 C17 C16 . . . . 1.4(4) ?
C18 C17 C16 C15 . . . . -0.4(4) ?
C14 C15 C16 C17 . . . . -1.5(3) ?
C4 C3 C2 C1 . . . . -1.0(4) ?
C6 C1 C2 C3 . . . . -0.4(4) ?
C1 C6 C5 C4 . . . . -1.8(4) ?
C7 C6 C5 C4 . . . . 176.2(2) ?
C2 C3 C4 C5 . . . . 1.0(4) ?
C6 C5 C4 C3 . . . . 0.5(4) ?
_cod_database_fobs_code 2243949