#------------------------------------------------------------------------------
#$Date: 2019-01-16 05:20:17 +0200 (Wed, 16 Jan 2019) $
#$Revision: 213101 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/24/28/2242800.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_2242800
loop_
_publ_author_name
'Hess, David'
'Mayer, Peter'
_publ_section_title
;
The crystal structures of benzylammonium phenylacetate and its hydrate
;
_journal_coeditor_code VM2215
_journal_issue 2
_journal_name_full 'Acta Crystallographica Section E'
_journal_page_first 194
_journal_page_last 201
_journal_paper_doi 10.1107/S2056989019000288
_journal_volume 75
_journal_year 2019
_chemical_formula_iupac 'C7 H10 N +, C8 H7 O2 -'
_chemical_formula_moiety 'C7 H10 N +, C8 H7 O2 -'
_chemical_formula_sum 'C15 H17 N O2'
_chemical_formula_weight 243.29
_chemical_name_systematic
;
Benzylammonium phenylacetate
;
_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'
_symmetry_space_group_name_Hall '-C 2yc'
_symmetry_space_group_name_H-M 'C 1 2/c 1'
_atom_sites_solution_hydrogens mixed
_audit_block_code C7H10N_C8H7O2_vv347_hess-ill
_audit_creation_method SHELXL-2014
_cell_angle_alpha 90
_cell_angle_beta 114.692(3)
_cell_angle_gamma 90
_cell_formula_units_Z 8
_cell_length_a 25.913(2)
_cell_length_b 5.9021(5)
_cell_length_c 19.0842(16)
_cell_measurement_reflns_used 4302
_cell_measurement_temperature 100(2)
_cell_measurement_theta_max 25.3680
_cell_measurement_theta_min 3.4614
_cell_volume 2651.9(4)
_computing_cell_refinement
;
SAINT (Bruker, 2015)
;
_computing_data_collection
;
APEX3 (Bruker, 2016)
;
_computing_data_reduction
;
SAINT (Bruker, 2015)
;
_computing_molecular_graphics
;
ORTEP-3 for Windows (Farrugia, 2012), Mercury (Macrae et al.,
2006),
CrystalExplorer17
(Turner et al., 2017)
;
_computing_publication_material
;
PLATON (Spek, 2009), RPLUTO (CCDC, 2018)
;
_computing_structure_refinement
;
SHELXL2014/7 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT (Sheldrick, 2015a)
;
_diffrn_ambient_temperature 100(2)
_diffrn_detector_area_resol_mean 7.4074
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device 'fixed-chi three-circle diffractometer'
_diffrn_measurement_device_type 'Bruker D8 Venture TXS'
_diffrn_measurement_method 'mix of phi and omega scans'
_diffrn_radiation_monochromator 'focusing mirrors'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0919
_diffrn_reflns_av_unetI/netI 0.0603
_diffrn_reflns_limit_h_max 30
_diffrn_reflns_limit_h_min -30
_diffrn_reflns_limit_k_max 7
_diffrn_reflns_limit_k_min -7
_diffrn_reflns_limit_l_max 22
_diffrn_reflns_limit_l_min -22
_diffrn_reflns_number 14421
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 25.345
_diffrn_reflns_theta_min 3.272
_diffrn_source 'rotating anode (TXS)'
_diffrn_source_current 50
_diffrn_source_power 2.5
_diffrn_source_voltage 50
_exptl_absorpt_coefficient_mu 0.081
_exptl_absorpt_correction_T_max 0.9705
_exptl_absorpt_correction_T_min 0.6513
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2016)
;
_exptl_crystal_colour colourless
_exptl_crystal_density_diffrn 1.219
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description block
_exptl_crystal_F_000 1040
_exptl_crystal_size_max 0.100
_exptl_crystal_size_mid 0.040
_exptl_crystal_size_min 0.020
_refine_diff_density_max 0.168
_refine_diff_density_min -0.225
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.033
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 175
_refine_ls_number_reflns 2398
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.033
_refine_ls_R_factor_all 0.0661
_refine_ls_R_factor_gt 0.0431
_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^)+(0.0352P)^2^+1.6577P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0937
_refine_ls_wR_factor_ref 0.1031
_reflns_number_gt 1800
_reflns_number_total 2398
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file vm2215sup1.cif
_cod_data_source_block 1
_cod_database_code 2242800
_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 0.992
_shelx_estimated_absorpt_t_max 0.998
_shelx_hkl_file
;
4 0 0 246.08 18.70
-4 0 0 250.57 18.70
-4 0 0 253.27 18.80
4 0 0 236.18 18.70
6 0 0 4576.64 337.77
-8 0 0 207.88 16.80
8 0 0 215.68 16.90
8 0 0 218.48 17.00
10 0 0 794.62 62.59
10 0 0 814.12 62.49
-10 0 0 925.41 62.69
-10 0 0 791.82 62.39
-12 0 0 10.80 3.00
12 0 0 10.10 3.00
-12 0 0 14.90 3.90
12 0 0 16.80 4.30
-14 0 0 312.47 26.10
-14 0 0 382.56 26.80
14 0 0 297.67 26.50
14 0 0 338.67 26.40
16 0 0 34.70 6.60
-16 0 0 60.49 7.10
-16 0 0 46.40 6.30
16 0 0 50.49 6.70
18 0 0 273.47 21.40
-18 0 0 259.97 21.00
18 0 0 226.18 21.40
20 0 0 296.07 23.90
20 0 0 249.78 24.00
-20 0 0 302.57 23.60
-22 0 0 37.60 6.10
22 0 0 25.40 5.80
-22 0 0 55.89 8.10
22 0 0 35.30 8.10
-24 0 0 34.10 7.10
24 0 0 16.20 5.80
26 0 0 19.60 5.80
-26 0 0 46.40 8.40
-26 0 0 25.00 6.00
-28 0 0 19.40 6.20
-28 0 0 22.50 9.50
28 0 0 20.00 6.70
1 -1 0 55.19 5.40
-1 -1 0 64.99 4.90
-1 -1 0 54.09 5.30
-1 1 0 65.89 5.50
1 1 0 74.39 5.00
1 1 0 57.39 5.50
3 -1 0 905.51 63.59
3 -1 0 764.42 64.09
-3 -1 0 875.21 63.99
-3 1 0 816.02 63.59
3 1 0 902.81 63.99
-3 1 0 857.11 64.19
3 1 0 899.91 63.79
5 -1 0 605.54 45.00
-5 -1 0 649.64 45.20
5 -1 0 534.65 45.40
-5 -1 0 601.04 45.20
-5 1 0 579.64 44.90
5 1 0 602.34 45.20
5 1 0 652.33 45.30
-5 1 0 606.44 45.50
-7 -1 0 368.96 27.40
7 -1 0 357.46 27.40
-7 -1 0 383.16 27.40
7 -1 0 327.67 27.70
-7 1 0 348.87 27.10
7 1 0 372.76 27.40
7 1 0 399.76 27.40
-7 1 0 295.07 29.10
9 -1 0 4.20 3.10
-9 -1 0 2.50 2.50
9 -1 0 5.10 2.20
-9 -1 0 5.40 2.30
9 1 0 3.70 2.50
-9 1 0 4.90 3.50
-9 1 0 3.70 1.90
9 1 0 3.90 2.50
11 -1 0 261.37 20.70
-11 -1 0 258.57 20.90
11 -1 0 222.98 21.10
-11 -1 0 267.17 20.90
11 1 0 266.97 21.00
-11 1 0 287.07 21.60
11 1 0 278.47 21.00
-11 1 0 249.58 20.50
13 -1 0 37.10 6.30
-13 -1 0 46.50 5.90
-13 -1 0 42.90 5.80
13 -1 0 39.50 5.70
-13 1 0 47.30 6.50
13 1 0 44.50 6.00
-13 1 0 44.60 5.30
-15 -1 0 154.48 13.80
-15 -1 0 166.08 14.00
15 -1 0 165.18 13.80
15 -1 0 138.39 14.30
15 1 0 157.68 14.00
-15 1 0 171.98 14.60
15 1 0 161.68 14.00
-15 1 0 149.09 13.40
17 -1 0 6.70 3.10
17 -1 0 0.80 4.00
-17 -1 0 2.60 3.20
-17 -1 0 1.30 3.20
17 1 0 1.50 3.60
-17 1 0 0.90 2.30
17 1 0 7.00 3.80
-17 1 0 3.50 4.00
-19 -1 0 0.90 3.30
19 -1 0 3.90 4.70
19 -1 0 -0.20 3.40
-19 1 0 -3.00 2.30
19 1 0 -3.40 3.40
19 1 0 0.20 4.30
-19 1 0 1.60 4.40
21 -1 0 -3.60 4.60
-21 -1 0 2.20 3.60
21 -1 0 0.20 3.40
-21 -1 0 -0.40 3.60
21 1 0 -1.90 4.40
21 1 0 -2.50 3.80
-21 1 0 4.30 4.70
-21 1 0 -3.30 2.80
23 -1 0 47.40 7.60
-23 -1 0 47.40 7.80
-23 -1 0 33.80 6.40
-23 1 0 47.40 8.40
23 1 0 39.20 11.80
-23 1 0 41.80 7.00
23 1 0 27.60 6.30
-25 -1 0 10.00 5.30
25 -1 0 12.80 4.60
-25 -1 0 24.20 6.20
25 1 0 28.90 7.10
-25 1 0 24.60 9.90
-27 -1 0 5.80 4.30
-27 -1 0 -1.90 4.60
27 -1 0 3.10 4.90
-27 1 0 2.60 4.60
27 1 0 4.20 4.90
-27 1 0 2.60 4.80
0 -2 0 72.59 7.20
0 -2 0 82.39 5.90
0 2 0 69.39 6.90
-2 -2 0 140.89 10.00
-2 -2 0 128.59 10.80
2 2 0 123.69 10.60
-2 2 0 125.69 10.80
-2 2 0 112.79 11.00
4 -2 0 550.64 39.30
-4 -2 0 499.45 40.20
-4 -2 0 534.15 39.70
4 2 0 541.35 40.20
4 2 0 519.85 39.70
6 -2 0 29.00 5.70
6 -2 0 38.20 3.80
-6 -2 0 27.30 4.80
6 2 0 36.10 4.50
-6 2 0 40.90 3.60
-6 2 0 37.10 3.50
-6 2 0 42.10 6.20
6 2 0 38.60 4.80
8 -2 0 68.99 9.30
-8 -2 0 76.89 8.60
-8 -2 0 94.29 8.40
8 -2 0 96.19 7.80
8 2 0 102.79 8.60
-8 2 0 96.79 9.90
-8 2 0 88.19 7.50
8 2 0 99.69 8.70
10 -2 0 160.38 16.00
10 -2 0 185.38 14.90
-10 -2 0 174.38 15.40
-10 -2 0 204.08 15.50
-10 2 0 200.38 16.60
10 2 0 206.68 15.60
-10 2 0 176.48 14.60
10 2 0 183.58 15.40
-12 -2 0 153.78 14.40
12 -2 0 139.69 15.00
12 -2 0 172.68 14.10
-12 -2 0 174.98 14.50
12 2 0 172.18 14.50
-12 2 0 194.58 15.60
12 2 0 201.28 15.80
-12 2 0 165.58 13.80
-14 -2 0 60.19 7.10
14 -2 0 53.29 6.50
14 -2 0 43.30 7.70
-14 -2 0 52.89 6.70
14 2 0 61.89 7.10
-14 2 0 56.49 6.00
-14 2 0 70.49 8.50
14 2 0 64.69 7.20
-16 -2 0 95.29 9.60
16 -2 0 96.99 9.20
-16 -2 0 82.69 9.30
16 -2 0 75.49 10.40
-16 2 0 83.19 8.60
-16 2 0 100.69 10.80
16 2 0 101.69 9.90
16 2 0 91.49 9.70
18 -2 0 32.20 7.60
18 -2 0 28.60 5.20
-18 -2 0 30.50 5.90
-18 -2 0 30.30 5.80
18 2 0 29.40 6.10
-18 2 0 37.50 7.70
-18 2 0 26.50 4.70
18 2 0 35.90 6.70
20 -2 0 129.09 12.90
-20 -2 0 141.09 13.40
-20 -2 0 130.39 13.50
20 -2 0 110.19 14.40
20 2 0 132.79 13.70
-20 2 0 124.19 12.40
-20 2 0 148.39 13.40
20 2 0 140.69 15.20
-20 2 0 162.08 15.00
-22 -2 0 13.00 4.90
22 -2 0 7.60 4.50
-22 -2 0 8.80 4.70
-22 2 0 10.60 3.90
-22 2 0 11.60 6.20
22 2 0 5.60 5.70
22 2 0 12.90 5.40
-22 2 0 12.40 4.00
24 -2 0 -2.40 3.20
-24 -2 0 0.20 4.20
-24 -2 0 0.50 3.00
24 2 0 -1.60 4.00
-24 2 0 1.70 5.90
-24 2 0 6.30 4.10
-26 -2 0 5.40 3.90
-26 -2 0 -11.70 4.20
26 -2 0 3.30 5.30
26 2 0 -2.30 4.40
-26 2 0 1.30 4.80
-26 2 0 4.70 3.90
-1 -3 0 50.39 4.40
1 -3 0 49.99 3.90
1 -3 0 51.69 6.50
-1 -3 0 40.70 6.30
1 -3 0 47.40 3.90
-1 3 0 41.10 5.90
1 3 0 38.30 5.80
-3 -3 0 1.90 3.00
-3 -3 0 1.10 1.60
-3 3 0 -0.90 2.50
-3 3 0 -6.70 3.50
3 3 0 -2.30 2.30
-5 -3 0 368.86 31.80
-5 -3 0 436.06 31.20
5 -3 0 409.66 30.40
5 3 0 447.66 32.00
-5 3 0 376.46 32.10
-5 3 0 411.26 32.60
-7 -3 0 4.00 2.30
-7 -3 0 8.20 3.30
7 -3 0 6.30 1.60
-7 3 0 6.70 4.20
-7 3 0 7.90 3.30
7 3 0 5.40 2.20
7 3 0 7.80 3.10
9 -3 0 65.49 9.20
9 -3 0 85.69 7.30
-9 -3 0 74.69 8.40
9 3 0 94.09 8.10
-9 3 0 90.99 7.00
-9 3 0 79.99 6.80
-9 3 0 96.99 10.00
9 3 0 95.59 9.20
11 -3 0 24.30 5.60
11 -3 0 18.40 3.10
-11 -3 0 19.60 4.90
-11 -3 0 19.30 4.30
11 3 0 23.80 4.60
-11 3 0 31.50 6.60
11 3 0 21.40 3.90
-11 3 0 19.10 2.80
-11 3 0 23.30 3.20
13 -3 0 11.00 5.10
-13 -3 0 10.00 3.30
13 -3 0 9.40 2.70
-13 -3 0 8.90 3.60
13 3 0 8.30 3.10
-13 3 0 11.80 2.60
13 3 0 14.80 4.10
-13 3 0 13.10 5.60
-13 3 0 8.00 2.20
-15 -3 0 58.49 7.50
15 -3 0 49.99 6.60
15 -3 0 61.29 9.80
-15 -3 0 52.09 7.30
-15 3 0 60.29 6.50
-15 3 0 51.39 6.10
15 3 0 65.99 7.90
15 3 0 59.39 7.70
-15 3 0 69.99 9.80
17 -3 0 146.29 15.10
-17 -3 0 176.68 16.10
17 -3 0 152.88 17.30
-17 -3 0 176.18 16.10
-17 3 0 194.08 15.30
-17 3 0 209.58 18.00
17 3 0 190.28 16.40
17 3 0 165.88 16.10
-17 3 0 189.78 15.40
19 -3 0 113.79 11.80
19 -3 0 105.19 13.70
-19 -3 0 123.89 12.60
-19 -3 0 125.19 12.70
-19 3 0 120.19 11.40
-19 3 0 142.99 12.00
19 3 0 119.39 13.10
-19 3 0 140.09 14.60
19 3 0 127.29 12.80
21 -3 0 5.90 3.40
-21 -3 0 -1.90 4.20
-21 -3 0 5.60 3.80
-21 3 0 8.20 5.90
21 3 0 7.60 5.50
21 3 0 14.00 4.60
-21 3 0 6.60 3.20
-23 -3 0 31.70 6.80
-23 -3 0 23.10 5.90
-23 3 0 31.20 10.40
-23 3 0 25.80 5.20
23 3 0 24.50 5.40
-25 -3 0 10.00 4.10
-25 -3 0 -3.80 4.90
25 -3 0 1.00 3.70
-25 3 0 -0.80 5.20
-25 3 0 -1.20 3.10
25 3 0 -0.50 4.10
0 -4 0 41.20 3.70
0 -4 0 41.00 3.70
0 -4 0 37.40 6.30
0 4 0 40.80 6.10
-2 -4 0 99.69 10.00
-2 -4 0 100.09 7.90
-2 -4 0 95.59 7.90
-2 4 0 92.09 9.70
2 4 0 91.19 9.70
-2 4 0 89.99 10.60
-4 -4 0 96.29 9.90
-4 -4 0 102.89 8.80
-4 4 0 85.39 10.60
4 4 0 102.09 9.80
-4 4 0 86.39 9.70
-6 -4 0 93.49 8.50
-6 -4 0 83.39 9.60
6 4 0 103.89 9.70
-6 4 0 97.89 10.90
-6 4 0 89.69 10.00
-8 -4 0 16.70 4.50
-8 -4 0 11.10 3.10
8 -4 0 16.10 2.20
-8 4 0 20.60 5.30
8 4 0 23.80 5.00
-8 4 0 21.60 6.10
-10 -4 0 21.10 4.20
-10 -4 0 22.70 5.40
-10 4 0 24.80 6.50
10 4 0 21.80 4.20
-10 4 0 25.40 7.00
10 4 0 26.60 5.30
-12 -4 0 6.80 3.20
12 -4 0 5.30 2.20
-12 -4 0 1.50 3.20
12 4 0 5.50 3.80
12 4 0 5.10 3.20
-12 4 0 5.10 5.50
14 -4 0 5.50 4.90
-14 -4 0 3.50 3.70
14 -4 0 3.50 2.40
-14 4 0 3.00 1.60
-14 4 0 9.20 5.90
14 4 0 5.30 3.60
-14 4 0 3.30 1.60
14 4 0 8.50 4.30
-16 -4 0 28.50 6.20
-16 -4 0 26.40 5.30
16 -4 0 33.30 8.40
16 -4 0 24.80 4.40
16 4 0 28.60 8.40
-16 4 0 24.70 3.60
-16 4 0 20.10 3.30
-16 4 0 28.30 8.20
16 4 0 20.70 4.70
18 -4 0 0.20 2.70
-18 -4 0 -0.70 3.10
-18 -4 0 2.40 3.40
18 4 0 1.50 4.50
-18 4 0 -1.00 2.00
18 4 0 -1.90 3.00
-18 4 0 -4.80 5.40
-20 -4 0 18.40 5.20
-20 -4 0 4.90 4.20
20 4 0 6.10 3.80
-20 4 0 11.80 3.20
-20 4 0 5.40 6.90
-22 -4 0 20.70 6.30
22 -4 0 8.60 3.80
22 4 0 18.90 5.80
-22 4 0 16.40 7.70
-22 4 0 18.40 3.90
-1 -5 0 72.29 6.40
-1 -5 0 76.29 6.40
-1 -5 0 70.89 9.40
1 5 0 82.09 9.50
-1 5 0 77.59 9.60
-1 5 0 76.99 10.90
-3 -5 0 51.49 8.20
-3 -5 0 52.99 5.30
-3 -5 0 47.00 5.20
-3 5 0 53.79 8.30
3 5 0 57.69 8.30
-3 5 0 57.09 9.90
-5 -5 0 49.10 7.70
-5 -5 0 41.90 5.20
-5 -5 0 47.10 5.50
-5 5 0 51.99 8.50
-5 5 0 47.40 10.60
5 5 0 47.50 7.60
-7 -5 0 4.10 2.60
-7 -5 0 5.80 2.60
-7 -5 0 2.90 4.20
-7 5 0 5.60 5.40
-7 5 0 6.30 5.00
7 5 0 7.80 4.10
-9 -5 0 44.50 8.00
-9 -5 0 44.60 6.00
-9 5 0 41.90 9.20
-9 5 0 68.99 11.40
9 5 0 54.19 7.70
-11 -5 0 8.00 4.20
-11 -5 0 9.80 3.30
-11 -5 0 6.70 3.00
11 5 0 14.80 4.70
-11 5 0 15.60 6.60
-11 5 0 2.20 6.00
-13 -5 0 8.90 3.60
-13 -5 0 11.30 4.60
-13 -5 0 12.40 4.10
-13 5 0 23.00 7.60
13 5 0 13.90 4.70
-13 5 0 9.50 6.70
-15 -5 0 4.50 3.50
-15 -5 0 8.40 4.10
-15 -5 0 5.20 3.20
-15 5 0 -0.10 6.70
15 5 0 8.60 4.40
-17 -5 0 -3.30 2.30
17 -5 0 5.10 2.90
-17 -5 0 6.30 3.70
-17 5 0 3.50 7.00
-19 -5 0 -6.20 3.80
-19 -5 0 2.80 3.40
-19 -5 0 10.70 4.40
19 -5 0 1.40 2.80
-19 5 0 -13.10 5.90
0 6 0 11.50 6.30
-2 -6 0 14.70 2.30
-2 -6 0 10.60 5.50
-2 6 0 22.80 8.10
-2 6 0 18.80 7.20
-4 -6 0 2.90 1.90
-4 -6 0 3.10 4.30
-4 -6 0 1.00 2.00
4 6 0 17.50 9.50
-4 6 0 9.80 5.00
-4 6 0 1.50 5.30
-6 -6 0 2.10 4.60
-6 -6 0 -1.90 2.20
-6 -6 0 0.80 2.00
-6 6 0 1.80 5.40
6 6 0 7.70 4.10
-6 6 0 9.00 5.00
-8 -6 0 1.30 2.30
-8 -6 0 -2.30 2.20
-8 -6 0 0.20 3.60
-8 6 0 -1.70 5.60
-8 6 0 7.90 5.50
-10 -6 0 6.50 4.20
-10 -6 0 6.20 3.30
-10 -6 0 7.70 2.90
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7 -1 -9 1457.95 99.99
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1 -1 -9 5.40 1.90
1 -1 -9 3.60 2.60
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-8 -2 -9 -0.70 2.20
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10 -2 9 1.90 3.20
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-12 -2 -9 61.99 8.80
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-12 2 -9 56.59 8.20
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-12 2 -9 73.49 11.50
14 -2 9 -0.70 3.40
14 -2 9 6.50 5.70
-14 -2 -9 2.10 3.30
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-16 -2 -9 -3.40 3.40
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21 -3 -9 16.50 5.60
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19 -3 -9 -2.90 3.90
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17 -3 -9 0.90 2.50
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3 -3 -9 26.50 4.10
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3 3 -9 14.90 3.20
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1 -3 -9 219.78 17.10
1 3 -9 182.58 19.30
1 3 -9 202.18 16.90
1 3 -9 207.28 18.50
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1 -3 9 9.30 3.10
-1 3 -9 13.90 3.20
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3 3 9 93.79 8.20
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5 3 9 35.90 5.10
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-7 -3 -9 8.30 2.70
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-9 -3 -9 257.37 21.20
-9 -3 -9 226.98 19.80
9 -3 9 266.07 20.80
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-9 3 -9 237.28 22.80
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11 -3 9 37.80 6.10
-11 -3 -9 38.90 5.30
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-13 -3 -9 1.30 3.80
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-15 -3 -9 33.40 5.20
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24 -4 -9 10.70 6.00
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18 -4 -9 2.40 3.90
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16 -4 -9 18.40 3.60
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14 -4 -9 2.90 2.20
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12 -4 -9 36.50 5.10
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-6 -4 -9 38.10 4.90
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-13 -5 9 124.69 12.80
13 -5 -9 139.39 11.40
-13 -5 9 124.59 12.50
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-13 5 9 132.29 12.70
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-11 -5 9 88.89 12.50
-11 -5 9 103.49 10.50
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10 0 -22 5.80 5.20
-10 0 22 8.70 4.70
10 0 -22 10.10 4.80
8 0 -22 6.50 5.10
6 0 -22 4.70 4.60
-6 0 22 18.30 7.20
-19 -1 22 0.10 3.90
19 -1 -22 -4.30 5.00
-19 -1 22 3.70 3.30
-19 1 22 3.40 2.70
19 1 -22 13.40 3.70
19 1 -22 -5.80 4.40
-19 1 22 1.20 3.40
17 -1 -22 1.60 2.50
17 -1 -22 7.10 4.80
-17 -1 22 4.10 3.90
-17 -1 22 0.30 3.90
-17 1 22 -3.60 3.40
17 1 -22 7.30 5.50
15 -1 -22 15.10 5.40
-15 -1 22 4.90 4.80
-15 -1 22 17.00 5.20
15 1 -22 15.80 6.20
-15 1 22 10.40 5.30
-13 -1 22 28.70 7.40
13 -1 -22 49.40 8.30
13 1 -22 47.20 8.80
13 1 -22 37.20 7.60
-13 1 22 54.09 8.80
11 -1 -22 4.80 4.10
-11 -1 22 0.60 4.50
11 1 -22 5.40 5.00
11 1 -22 9.70 5.30
-11 1 22 6.70 4.70
-9 -1 22 23.70 6.20
9 -1 -22 23.20 6.10
9 1 -22 16.70 6.50
-9 1 22 39.30 7.30
9 1 -22 20.20 6.30
7 -1 -22 13.60 5.70
-7 -1 22 0.80 4.00
7 1 -22 0.50 5.10
-7 1 22 9.60 5.60
14 -2 -22 -7.80 4.00
-14 -2 22 -0.50 3.90
-14 2 22 -0.10 3.10
12 -2 -22 -1.90 3.30
-12 -2 22 1.40 3.90
12 2 -22 9.30 5.50
-12 2 22 -7.10 2.80
0 0 0 0.00 0.00
_computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)'
;
_shelx_hkl_checksum 52916
_shelx_res_file
;
TITL vv347_0m_a.res in C2/c
REM Old TITL vv347_0m in C2/c
REM SHELXT solution in C2/c
REM R1 0.139, Rweak 0.007, Alpha 0.024, Orientation as input
REM Formula found by SHELXT: C15 O3
CELL 0.71073 25.9130 5.9021 19.0842 90.000 114.692 90.000
ZERR 8.000 0.0024 0.0005 0.0016 0.000 0.003 0.000
LATT 7
SYMM -X, Y, 1/2-Z
SFAC C H N O
UNIT 120 136 8 16
TEMP -173.150
SIZE 0.02 0.04 0.10
L.S. 10
BOND $H
LIST 4
CONF
ACTA
SHEL 9.0 0.83
HTAB
REM h k l Fo^2 Fc^2 Error/esd Fc/Fc(max) Resolution(A)
REM -12 0 12 576.69 150.55 7.91 0.030 1.50
REM -9 3 6 322.95 7.88 7.70 0.007 1.55
REM -18 0 12 1981.06 486.34 7.50 0.054 1.27
REM 16 0 0 747.47 245.28 6.45 0.038 1.47
REM 0 0 2 -2.90 117.92 6.12 0.027 8.67
REM -21 3 9 195.87 20.77 6.06 0.011 1.03
REM -6 0 12 905.26 451.54 6.00 0.052 1.59
REM -12 0 8 179.60 16.24 5.49 0.010 1.90
REM 9 3 3 106.06 19.70 4.80 0.011 1.43
OMIT -12 0 12
OMIT -9 3 6
OMIT -18 0 12
OMIT 16 0 0
OMIT 0 0 2
OMIT -21 3 9
OMIT -6 0 12
OMIT -12 0 8
OMIT 9 3 3
EQIV $1 -x+1/2, y+3/2, -z+1/2
HTAB N1 O1_$1
EQIV $2 -x+1/2, y+1/2, -z+1/2
HTAB N1 O2_$2
EQIV $3 x, y+1, z
HTAB N1 O2_$3
EQIV $4 -x+1/2, -y-1/2, -z+1
HTAB C2 O1_$4
HTAB C8 O1_$3
FMAP 2
PLAN -20
WGHT 0.035200 1.657700
FVAR 0.25751
O1 4 0.282786 -0.354589 0.417058 11.00000 0.02661 0.01677 =
0.01769 0.00001 0.00888 0.00020
O2 4 0.247718 -0.070608 0.333623 11.00000 0.03046 0.02022 =
0.01341 0.00063 0.00914 0.00234
N1 3 0.273879 0.874816 0.206673 11.00000 0.02789 0.01815 =
0.01501 0.00134 0.00889 0.00003
H11 2 0.249606 0.977093 0.166680 11.00000 0.03969
H12 2 0.266642 0.714492 0.186690 11.00000 0.03496
H13 2 0.266059 0.882616 0.251124 11.00000 0.04842
C1 1 0.270131 -0.150618 0.401686 11.00000 0.01611 0.02025 =
0.01684 -0.00169 0.00926 -0.00239
C2 1 0.281132 0.011797 0.468553 11.00000 0.02335 0.01789 =
0.01772 0.00064 0.01044 0.00145
AFIX 23
H2A 2 0.268731 0.165592 0.447565 11.00000 -1.20000
H2B 2 0.257727 -0.035301 0.495837 11.00000 -1.20000
AFIX 0
C3 1 0.342593 0.022043 0.525908 11.00000 0.02463 0.01995 =
0.01521 -0.00300 0.01216 0.00000
C4 1 0.368660 -0.159515 0.574846 11.00000 0.02817 0.02246 =
0.01848 -0.00194 0.01190 -0.00230
AFIX 43
H4 2 0.347605 -0.293715 0.571890 11.00000 -1.20000
AFIX 0
C5 1 0.424925 -0.145992 0.627684 11.00000 0.03007 0.02715 =
0.02192 0.00008 0.01020 0.00598
AFIX 43
H5 2 0.442096 -0.270539 0.660782 11.00000 -1.20000
AFIX 0
C6 1 0.456234 0.048048 0.632484 11.00000 0.02202 0.03710 =
0.02867 -0.00808 0.00639 -0.00073
AFIX 43
H6 2 0.494782 0.057276 0.668782 11.00000 -1.20000
AFIX 0
C7 1 0.430977 0.227872 0.584110 11.00000 0.02902 0.02753 =
0.03932 -0.00618 0.01399 -0.00807
AFIX 43
H7 2 0.452323 0.361099 0.586899 11.00000 -1.20000
AFIX 0
C8 1 0.374572 0.215344 0.531392 11.00000 0.03014 0.01968 =
0.02827 -0.00048 0.01383 -0.00144
AFIX 43
H8 2 0.357614 0.340739 0.498613 11.00000 -1.20000
AFIX 0
C9 1 0.334540 0.937949 0.228880 11.00000 0.02832 0.02739 =
0.02632 0.00458 0.01162 -0.00264
AFIX 23
H9A 2 0.341116 1.094838 0.249072 11.00000 -1.20000
H9B 2 0.342833 0.932604 0.182755 11.00000 -1.20000
AFIX 0
C10 1 0.373709 0.779410 0.289177 11.00000 0.01996 0.02448 =
0.02318 0.00192 0.01054 -0.00376
C11 1 0.388605 0.817934 0.366837 11.00000 0.02327 0.03771 =
0.02600 -0.00168 0.01279 -0.00181
AFIX 43
H11A 2 0.376314 0.952521 0.382572 11.00000 -1.20000
AFIX 0
C12 1 0.421239 0.662181 0.421768 11.00000 0.02532 0.05912 =
0.02159 0.00728 0.00972 -0.00107
AFIX 43
H12A 2 0.430995 0.689784 0.474843 11.00000 -1.20000
AFIX 0
C13 1 0.439566 0.467241 0.399501 11.00000 0.02193 0.04220 =
0.04022 0.01762 0.00507 0.00057
AFIX 43
H13A 2 0.461430 0.359239 0.437098 11.00000 -1.20000
AFIX 0
C14 1 0.426091 0.429189 0.322444 11.00000 0.02218 0.02923 =
0.04815 -0.00291 0.00732 0.00014
AFIX 43
H14 2 0.439361 0.296248 0.307176 11.00000 -1.20000
AFIX 0
C15 1 0.393296 0.584130 0.267318 11.00000 0.02456 0.03180 =
0.02989 -0.00367 0.00896 -0.00286
AFIX 43
H15 2 0.384135 0.557000 0.214373 11.00000 -1.20000
REM #####
AFIX 0
HKLF 4
REM vv347_0m_a.res in C2/c
REM R1 = 0.0431 for 1800 Fo > 4sig(Fo) and 0.0661 for all 2398 data
REM 175 parameters refined using 0 restraints
END
WGHT 0.0352 1.6577
REM Instructions for potential hydrogen bonds
HTAB N1 O1_$1
HTAB N1 O2_$2
HTAB N1 O2_$3
HTAB C2 O1_$4
REM Highest difference peak 0.168, deepest hole -0.225, 1-sigma level 0.047
Q1 1 0.1730 -0.2480 0.2290 11.00000 0.05 0.17
Q2 1 0.3461 0.0455 0.4188 11.00000 0.05 0.15
Q3 1 0.4383 0.7885 0.4779 11.00000 0.05 0.15
Q4 1 0.2871 -0.5138 0.3896 11.00000 0.05 0.14
Q5 1 0.2479 -0.2645 0.3328 11.00000 0.05 0.14
Q6 1 0.2125 -0.2198 0.2733 11.00000 0.05 0.14
Q7 1 0.3467 -0.4346 0.5795 11.00000 0.05 0.14
Q8 1 0.2811 0.1140 0.3612 11.00000 0.05 0.14
Q9 1 0.3311 0.8826 0.1394 11.00000 0.05 0.14
Q10 1 0.3128 0.0112 0.4985 11.00000 0.05 0.14
Q11 1 0.1612 -0.2421 0.2792 11.00000 0.05 0.14
Q12 1 0.4505 -0.4316 0.7202 11.00000 0.05 0.14
Q13 1 0.3706 0.6326 0.2788 11.00000 0.05 0.13
Q14 1 0.4485 0.9215 0.4320 11.00000 0.05 0.13
Q15 1 0.2929 0.3092 0.3775 11.00000 0.05 0.13
Q16 1 0.3230 -0.5002 0.4680 11.00000 0.05 0.13
Q17 1 0.3477 -0.3984 0.5288 11.00000 0.05 0.13
Q18 1 0.4655 0.6039 0.3214 11.00000 0.05 0.13
Q19 1 0.4372 0.8881 0.5203 11.00000 0.05 0.13
Q20 1 0.1197 -0.2152 0.2627 11.00000 0.05 0.13
;
_shelx_res_checksum 97221
_shelxl_version_number 2.014
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
O O1 0.28279(5) -0.35459(19) 0.41706(7) 0.0205(3) Uani d 1
O O2 0.24772(5) -0.07061(19) 0.33362(7) 0.0214(3) Uani d 1
N N1 0.27388(7) 0.8748(3) 0.20667(9) 0.0204(4) Uani d 1
H H11 0.2496(9) 0.977(4) 0.1667(13) 0.040(6) Uiso d 1
H H12 0.2666(8) 0.714(4) 0.1867(12) 0.035(6) Uiso d 1
H H13 0.2661(10) 0.883(4) 0.2511(14) 0.048(7) Uiso d 1
C C1 0.27013(7) -0.1506(3) 0.40169(10) 0.0169(4) Uani d 1
C C2 0.28113(7) 0.0118(3) 0.46855(10) 0.0190(4) Uani d 1
H H2A 0.2687 0.1656 0.4476 0.023 Uiso calc 1
H H2B 0.2577 -0.0353 0.4958 0.023 Uiso calc 1
C C3 0.34259(7) 0.0220(3) 0.52591(10) 0.0186(4) Uani d 1
C C4 0.36866(8) -0.1595(3) 0.57485(10) 0.0223(4) Uani d 1
H H4 0.3476 -0.2937 0.5719 0.027 Uiso calc 1
C C5 0.42493(8) -0.1460(3) 0.62768(11) 0.0266(4) Uani d 1
H H5 0.4421 -0.2705 0.6608 0.032 Uiso calc 1
C C6 0.45623(8) 0.0480(3) 0.63248(11) 0.0307(5) Uani d 1
H H6 0.4948 0.0573 0.6688 0.037 Uiso calc 1
C C7 0.43098(8) 0.2279(3) 0.58411(12) 0.0321(5) Uani d 1
H H7 0.4523 0.3611 0.5869 0.038 Uiso calc 1
C C8 0.37457(8) 0.2153(3) 0.53139(11) 0.0255(4) Uani d 1
H H8 0.3576 0.3407 0.4986 0.031 Uiso calc 1
C C9 0.33454(8) 0.9379(3) 0.22888(11) 0.0273(5) Uani d 1
H H9A 0.3411 1.0948 0.2491 0.033 Uiso calc 1
H H9B 0.3428 0.9326 0.1828 0.033 Uiso calc 1
C C10 0.37371(7) 0.7794(3) 0.28918(10) 0.0220(4) Uani d 1
C C11 0.38860(8) 0.8179(3) 0.36684(11) 0.0281(5) Uani d 1
H H11A 0.3763 0.9525 0.3826 0.034 Uiso calc 1
C C12 0.42124(8) 0.6622(4) 0.42177(11) 0.0354(5) Uani d 1
H H12A 0.4310 0.6898 0.4748 0.042 Uiso calc 1
C C13 0.43957(9) 0.4672(4) 0.39950(13) 0.0375(5) Uani d 1
H H13A 0.4614 0.3592 0.4371 0.045 Uiso calc 1
C C14 0.42609(8) 0.4292(3) 0.32244(13) 0.0357(5) Uani d 1
H H14 0.4394 0.2962 0.3072 0.043 Uiso calc 1
C C15 0.39330(8) 0.5841(3) 0.26732(12) 0.0296(5) Uani d 1
H H15 0.3841 0.5570 0.2144 0.035 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 0.0266(7) 0.0168(7) 0.0177(6) 0.0002(5) 0.0089(5) 0.0000(5)
O2 0.0305(7) 0.0202(7) 0.0134(6) 0.0023(5) 0.0091(5) 0.0006(5)
N1 0.0279(9) 0.0181(9) 0.0150(8) 0.0000(7) 0.0089(7) 0.0013(7)
C1 0.0161(9) 0.0203(10) 0.0168(9) -0.0024(7) 0.0093(7) -0.0017(7)
C2 0.0233(10) 0.0179(9) 0.0177(9) 0.0015(7) 0.0104(8) 0.0006(7)
C3 0.0246(10) 0.0200(9) 0.0152(9) 0.0000(7) 0.0122(8) -0.0030(7)
C4 0.0282(10) 0.0225(10) 0.0185(9) -0.0023(8) 0.0119(8) -0.0019(7)
C5 0.0301(11) 0.0271(10) 0.0219(10) 0.0060(8) 0.0102(8) 0.0001(8)
C6 0.0220(10) 0.0371(12) 0.0287(11) -0.0007(9) 0.0064(9) -0.0081(9)
C7 0.0290(11) 0.0275(11) 0.0393(12) -0.0081(9) 0.0140(10) -0.0062(9)
C8 0.0301(11) 0.0197(10) 0.0283(11) -0.0014(8) 0.0138(9) -0.0005(8)
C9 0.0283(11) 0.0274(11) 0.0263(10) -0.0026(8) 0.0116(9) 0.0046(8)
C10 0.0200(10) 0.0245(10) 0.0232(10) -0.0038(7) 0.0105(8) 0.0019(8)
C11 0.0233(10) 0.0377(12) 0.0260(11) -0.0018(8) 0.0128(9) -0.0017(9)
C12 0.0253(11) 0.0591(15) 0.0216(10) -0.0011(10) 0.0097(9) 0.0073(10)
C13 0.0219(11) 0.0422(13) 0.0402(13) 0.0006(9) 0.0051(10) 0.0176(10)
C14 0.0222(11) 0.0292(11) 0.0481(14) 0.0001(8) 0.0073(10) -0.0029(10)
C15 0.0246(11) 0.0318(11) 0.0299(11) -0.0029(8) 0.0090(9) -0.0037(9)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 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
C9 N1 H11 109.1(13)
C9 N1 H12 110.4(11)
H11 N1 H12 109.2(17)
C9 N1 H13 109.0(14)
H11 N1 H13 111.2(19)
H12 N1 H13 107.9(17)
O1 C1 O2 124.09(15)
O1 C1 C2 118.04(15)
O2 C1 C2 117.86(15)
C3 C2 C1 113.80(14)
C3 C2 H2A 108.8
C1 C2 H2A 108.8
C3 C2 H2B 108.8
C1 C2 H2B 108.8
H2A C2 H2B 107.7
C8 C3 C4 118.27(17)
C8 C3 C2 120.20(16)
C4 C3 C2 121.53(16)
C5 C4 C3 120.69(17)
C5 C4 H4 119.7
C3 C4 H4 119.7
C6 C5 C4 120.34(18)
C6 C5 H5 119.8
C4 C5 H5 119.8
C7 C6 C5 119.42(18)
C7 C6 H6 120.3
C5 C6 H6 120.3
C6 C7 C8 120.39(18)
C6 C7 H7 119.8
C8 C7 H7 119.8
C7 C8 C3 120.88(18)
C7 C8 H8 119.6
C3 C8 H8 119.6
N1 C9 C10 110.87(15)
N1 C9 H9A 109.5
C10 C9 H9A 109.5
N1 C9 H9B 109.5
C10 C9 H9B 109.5
H9A C9 H9B 108.1
C11 C10 C15 118.89(17)
C11 C10 C9 120.98(17)
C15 C10 C9 120.05(17)
C12 C11 C10 120.66(19)
C12 C11 H11A 119.7
C10 C11 H11A 119.7
C13 C12 C11 120.06(19)
C13 C12 H12A 120.0
C11 C12 H12A 120.0
C12 C13 C14 119.87(19)
C12 C13 H13A 120.1
C14 C13 H13A 120.1
C13 C14 C15 120.2(2)
C13 C14 H14 119.9
C15 C14 H14 119.9
C14 C15 C10 120.26(19)
C14 C15 H15 119.9
C10 C15 H15 119.9
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
O1 C1 1.250(2)
O2 C1 1.272(2)
N1 C9 1.494(2)
N1 H11 0.97(2)
N1 H12 1.01(2)
N1 H13 0.95(3)
C1 C2 1.525(2)
C2 C3 1.511(2)
C2 H2A 0.9900
C2 H2B 0.9900
C3 C8 1.388(3)
C3 C4 1.396(2)
C4 C5 1.386(3)
C4 H4 0.9500
C5 C6 1.384(3)
C5 H5 0.9500
C6 C7 1.379(3)
C6 H6 0.9500
C7 C8 1.388(3)
C7 H7 0.9500
C8 H8 0.9500
C9 C10 1.501(3)
C9 H9A 0.9900
C9 H9B 0.9900
C10 C11 1.385(3)
C10 C15 1.392(3)
C11 C12 1.385(3)
C11 H11A 0.9500
C12 C13 1.378(3)
C12 H12A 0.9500
C13 C14 1.381(3)
C13 H13A 0.9500
C14 C15 1.385(3)
C14 H14 0.9500
C15 H15 0.9500
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
N1 H11 O1 4_565 0.97(2) 1.77(2) 2.7177(19) 165(2)
N1 H12 O2 4 1.01(2) 1.73(2) 2.7306(19) 170.1(18)
N1 H13 O2 1_565 0.95(3) 1.85(3) 2.7938(19) 174(2)
C2 H2B O1 7_546 0.99 2.40 3.375(2) 169.4
C8 H8 O1 1_565 0.95 2.63 3.539(2) 161.4
C9 H9 Cg1 6_565 0.95 2.92 3.877(2) 163
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
O1 C1 C2 C3 59.1(2)
O2 C1 C2 C3 -122.12(17)
C1 C2 C3 C8 110.26(18)
C1 C2 C3 C4 -70.2(2)
C8 C3 C4 C5 0.3(2)
C2 C3 C4 C5 -179.29(16)
C3 C4 C5 C6 -0.3(3)
C4 C5 C6 C7 -0.1(3)
C5 C6 C7 C8 0.4(3)
C6 C7 C8 C3 -0.4(3)
C4 C3 C8 C7 0.0(3)
C2 C3 C8 C7 179.60(17)
N1 C9 C10 C11 -86.5(2)
N1 C9 C10 C15 90.2(2)
C15 C10 C11 C12 -1.6(3)
C9 C10 C11 C12 175.07(17)
C10 C11 C12 C13 0.4(3)
C11 C12 C13 C14 1.0(3)
C12 C13 C14 C15 -1.3(3)
C13 C14 C15 C10 0.0(3)
C11 C10 C15 C14 1.4(3)
C9 C10 C15 C14 -175.34(18)
_cod_database_fobs_code 2242800