#------------------------------------------------------------------------------
#$Date: 2025-05-14 03:00:02 +0100 (Wed, 14 May 2025) $
#$Revision: 299653 $
#$URL: svn://www.crystallography.net/cod/cif/2/02/35/2023505.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_2023505
loop_
_publ_author_name
'Abubakar Magaji, Mubarak'
'Chen, Beining'
'Robertson, Craig Collumbine'
_publ_section_title
;
Synthesis, crystal structure and Hirshfeld surface analysis of
Fmoc-\b-amino butyric acid and Fmoc carbamate
;
_journal_issue 6
_journal_name_full
'Acta Crystallographica Section E Crystallographic Communications'
_journal_paper_doi 10.1107/S2056989025003810
_journal_volume 81
_journal_year 2025
_chemical_absolute_configuration ad
_chemical_formula_moiety 'C15 H13 N O2'
_chemical_formula_sum 'C15 H13 N O2'
_chemical_formula_weight 239.26
_space_group_crystal_system orthorhombic
_space_group_IT_number 29
_space_group_name_Hall 'P 2c -2ac'
_space_group_name_H-M_alt 'P c a 21'
_atom_sites_solution_hydrogens mixed
_atom_sites_solution_primary dual
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_formula_units_Z 8
_cell_length_a 15.3560(3)
_cell_length_b 5.04000(10)
_cell_length_c 31.0254(7)
_cell_measurement_reflns_used 6701
_cell_measurement_temperature 100.00
_cell_measurement_theta_max 65.907
_cell_measurement_theta_min 3.238
_cell_volume 2401.19(9)
_computing_cell_refinement
;
SAINT V8.40B (Bruker, 2023)
;
_computing_data_collection
;
APEX5 (Bruker, 2023)
;
_computing_data_reduction
;
SAINT V8.40B (Bruker, 2023)
;
_computing_molecular_graphics
;
Olex2 1.5 (Dolomanov et al., 2009)
;
_computing_publication_material
;
Olex2 1.5 (Dolomanov et al., 2009)
;
_computing_structure_refinement
;
SHELXL (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT2018/2 (Sheldrick, 2015a)
;
_diffrn_ambient_temperature 100.00
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type 'Bruker D8 Venture Photon III'
_diffrn_measurement_method '\f and \w scans'
_diffrn_radiation_type CuK\a
_diffrn_radiation_wavelength 1.54178
_diffrn_reflns_av_R_equivalents 0.0508
_diffrn_reflns_av_unetI/netI 0.0356
_diffrn_reflns_limit_h_max 18
_diffrn_reflns_limit_h_min -18
_diffrn_reflns_limit_k_max 5
_diffrn_reflns_limit_k_min -5
_diffrn_reflns_limit_l_max 36
_diffrn_reflns_limit_l_min -36
_diffrn_reflns_number 18874
_diffrn_reflns_theta_full 66.746
_diffrn_reflns_theta_max 66.746
_diffrn_reflns_theta_min 2.848
_diffrn_source_current 1.0
_diffrn_source_power 0.05
_diffrn_source_voltage 50.0
_diffrn_standards_number 0
_exptl_absorpt_coefficient_mu 0.712
_exptl_absorpt_correction_T_max 0.7528
_exptl_absorpt_correction_T_min 0.6829
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
(SADABS; Krause et al., 2015)
;
_exptl_crystal_colour colourless
_exptl_crystal_density_diffrn 1.324
_exptl_crystal_description needle
_exptl_crystal_F_000 1008
_exptl_crystal_size_max 0.25
_exptl_crystal_size_mid 0.026
_exptl_crystal_size_min 0.012
_refine_diff_density_max 0.136
_refine_diff_density_min -0.165
_refine_ls_abs_structure_details
;
Flack x determined using 1617 quotients
[(I^+^)-(I^-^)]/[(I^+^)+(I^-^)]
(Parsons et al., 2013)
;
_refine_ls_abs_structure_Flack -0.26(13)
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.047
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 341
_refine_ls_number_reflns 4069
_refine_ls_number_restraints 1
_refine_ls_restrained_S_all 1.047
_refine_ls_R_factor_all 0.0345
_refine_ls_R_factor_gt 0.0295
_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^)+(0.0291P)^2^+0.3089P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0647
_refine_ls_wR_factor_ref 0.0678
_reflns_number_gt 3754
_reflns_number_total 4069
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file vu2009.cif
_cod_data_source_block 2
_cod_database_code 2023505
_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 0.842
_shelx_estimated_absorpt_t_max 0.992
_shelx_hkl_file
;
0 -1 0 4667.13 124.09
0 -2 0 452.45 16.40
0 -3 0 6.60 3.80
0 -3 0 4.20 2.30
0 -4 0 2.10 2.50
0 -4 0 5.20 2.20
0 -4 0 5.50 2.70
0 -5 0 2.50 2.70
1 0 0 0.50 0.60
-1 0 0 0.00 0.40
-1 0 0 -0.10 0.40
-1 -1 0 609.54 19.10
1 -1 0 632.84 18.50
1 -1 0 629.34 22.80
-1 -2 0 8.50 2.40
1 -2 0 20.80 3.70
-1 -3 0 63.79 4.60
1 -3 0 56.49 4.20
1 -3 0 59.59 4.40
-1 -3 0 52.69 7.60
-1 -4 0 39.70 4.60
-1 -4 0 59.79 5.80
1 -4 0 39.20 3.70
-1 -4 0 46.70 4.20
1 -4 0 44.10 4.00
1 -4 0 36.20 4.00
-1 -5 0 0.70 1.90
1 -5 0 5.20 1.90
1 -5 0 -2.30 2.50
2 0 0 5.40 1.40
-2 0 0 5.00 4.30
-2 0 0 6.20 1.30
-2 -1 0 -0.10 4.20
2 -1 0 2.00 1.40
-2 -1 0 2.20 1.70
2 -1 0 0.20 5.00
-2 -1 0 2.50 1.10
2 -2 0 5.30 1.70
2 -2 0 4.80 4.80
-2 -2 0 3.50 2.30
2 -3 0 8.90 2.80
-2 -3 0 8.60 2.70
-2 -3 0 8.00 2.40
2 -3 0 7.20 2.20
2 -3 0 8.90 2.30
2 -3 0 12.70 2.80
-2 -3 0 6.90 4.10
-2 -4 0 143.29 6.30
-2 -4 0 158.38 8.00
-2 -4 0 164.48 12.50
-2 -4 0 135.19 6.20
2 -4 0 152.38 7.10
2 -4 0 154.78 7.00
3 0 0 -0.90 1.20
-3 0 0 0.30 1.20
-3 0 0 -2.90 6.80
3 -1 0 1123.09 32.50
3 -1 0 1174.18 46.40
-3 1 0 1096.49 31.50
-3 -1 0 1095.39 31.90
-3 -1 0 1109.39 34.40
-3 -1 0 1164.88 41.90
3 -2 0 84.49 5.50
-3 -2 0 87.39 4.90
-3 -2 0 89.79 4.40
-3 -2 0 98.89 7.40
3 -2 0 89.79 11.60
3 -3 0 -1.70 1.70
3 -3 0 -0.10 1.80
-3 -3 0 3.30 3.80
-3 -3 0 2.80 2.50
3 -3 0 2.30 2.20
3 -3 0 3.30 2.50
3 -4 0 60.59 5.30
-3 -4 0 63.19 11.30
-3 -4 0 63.99 4.40
-3 4 0 67.39 7.80
3 -4 0 62.29 4.60
-3 -4 0 57.69 5.30
-3 -5 0 -0.70 1.70
-3 -5 0 -0.80 3.20
3 -5 0 1.20 2.30
-4 0 0 998.30 42.90
-4 0 0 914.31 27.10
4 0 0 912.41 28.10
-4 -1 0 61.19 12.00
-4 1 0 52.19 14.50
-4 -1 0 59.39 4.90
4 -1 0 57.19 4.80
-4 1 0 59.79 3.70
4 -2 0 60.59 13.40
-4 -2 0 56.29 4.40
4 -2 0 55.39 5.00
-4 -2 0 43.10 5.50
-4 -2 0 66.89 4.20
-4 2 0 58.59 4.50
-4 -3 0 3.60 2.10
-4 -3 0 5.80 2.80
4 -3 0 4.60 2.10
-4 -3 0 4.10 2.40
4 -3 0 4.80 2.80
4 -3 0 4.00 2.40
-4 3 0 10.00 3.10
-4 -3 0 8.10 4.60
4 -4 0 52.99 5.10
-4 -4 0 35.10 5.60
-4 -4 0 46.00 8.50
4 -4 0 52.19 6.10
-4 -4 0 48.80 4.10
4 -4 0 54.39 4.30
-4 -5 0 15.80 3.60
-4 -5 0 11.40 2.10
5 0 0 2.00 2.00
-5 0 0 -0.20 8.80
-5 0 0 -2.00 1.40
-5 -1 0 310.47 23.70
-5 1 0 286.47 12.20
-5 -1 0 309.57 12.80
-5 1 0 288.77 10.70
5 -1 0 320.87 12.90
-5 1 0 314.27 27.20
5 -2 0 957.10 30.90
-5 -2 0 945.11 27.90
5 -2 0 965.60 50.59
-5 -2 0 898.11 30.00
-5 -2 0 982.40 41.30
-5 2 0 953.80 28.70
-5 -2 0 937.01 32.50
-5 -3 0 49.60 4.00
5 -3 0 53.69 4.30
5 -3 0 51.79 4.90
5 -3 0 45.20 6.10
-5 -3 0 51.99 4.90
-5 -3 0 47.50 4.00
-5 -4 0 59.49 5.90
5 -4 0 53.69 5.10
5 -4 0 68.99 7.80
-5 -4 0 62.19 10.70
-5 -4 0 54.39 4.10
5 -4 0 66.19 4.70
5 -5 0 1.30 2.30
-5 -5 0 -1.20 1.50
-5 -5 0 3.10 3.10
5 -5 0 -1.50 1.80
-6 0 0 6.60 8.20
-6 0 0 1.00 1.70
6 0 0 0.50 2.30
-6 -1 0 0.10 1.90
-6 1 0 1.30 3.80
-6 1 0 -1.60 7.80
6 -1 0 -0.80 2.20
-6 1 0 -1.10 1.50
-6 -1 0 2.20 8.30
-6 -2 0 25.40 9.40
-6 -2 0 37.80 3.80
6 -2 0 34.90 3.40
-6 -2 0 35.40 3.40
6 -2 0 37.00 5.50
-6 2 0 41.80 4.40
-6 -3 0 -2.20 3.50
-6 -3 0 1.30 2.30
-6 -3 0 5.90 2.10
6 -3 0 3.00 4.00
-6 3 0 4.10 3.00
6 -3 0 1.80 1.50
6 -3 0 3.40 2.70
-6 -3 0 3.00 1.80
-6 -4 0 -3.60 2.70
-6 -4 0 1.90 1.90
6 -4 0 -2.10 1.70
6 -4 0 0.90 2.30
6 -4 0 0.00 3.30
-6 -4 0 -1.60 5.20
-6 -4 0 0.20 2.70
6 -5 0 2.20 1.70
-6 -5 0 3.40 1.60
-6 -5 0 7.00 3.10
-7 0 0 1.80 2.00
7 0 0 -2.50 2.00
-7 0 0 0.20 1.20
-7 0 0 -1.20 8.20
-7 -1 0 472.95 15.10
-7 -1 0 504.25 35.90
-7 1 0 456.95 16.50
7 -1 0 490.35 19.60
-7 1 0 458.55 14.20
-7 1 0 454.55 39.00
-7 -1 0 474.95 19.00
-7 1 0 466.05 19.30
7 -2 0 188.68 7.70
-7 2 0 168.98 6.70
7 -2 0 189.88 11.60
-7 -2 0 169.88 8.10
-7 2 0 178.88 8.80
7 -2 0 182.28 7.50
7 -3 0 14.30 4.60
-7 -3 0 14.30 2.90
7 -3 0 13.50 2.50
-7 -3 0 11.60 4.80
-7 3 0 15.70 3.20
-7 -3 0 15.20 2.40
-7 -3 0 14.90 2.70
-7 3 0 16.20 4.00
7 -4 0 22.70 3.60
7 -4 0 35.20 6.90
7 -4 0 28.10 3.50
-7 -4 0 28.00 3.10
-7 -4 0 26.30 4.10
-7 -4 0 17.10 6.90
-7 -4 0 27.90 5.20
-7 -5 0 58.19 5.60
7 -5 0 80.19 4.40
7 -5 0 76.89 4.70
-7 -5 0 87.69 4.30
8 0 0 321.57 15.60
-8 0 0 315.87 10.90
-8 0 0 322.57 14.10
-8 0 0 316.17 31.60
-8 1 0 72.29 5.90
8 -1 0 77.19 4.60
-8 1 0 102.59 26.50
-8 -1 0 84.39 20.00
-8 -1 0 75.99 4.80
-8 1 0 72.99 4.10
-8 -1 0 76.09 7.30
-8 1 0 83.99 9.40
8 -1 0 86.39 7.90
8 -2 0 41.70 3.90
8 -2 0 41.90 4.10
-8 -2 0 42.20 3.50
-8 -2 0 41.20 4.70
-8 2 0 44.80 5.40
-8 2 0 47.00 3.50
8 -2 0 38.90 6.50
-8 -2 0 44.70 13.70
-8 -3 0 109.29 14.00
-8 -3 0 115.49 7.40
8 -3 0 106.59 6.00
-8 -3 0 102.59 5.40
8 -3 0 111.69 6.70
8 -3 0 119.19 10.60
-8 -4 0 157.98 10.90
8 -4 0 159.58 7.60
8 -4 0 176.08 12.90
-8 -4 0 165.88 9.40
-8 -4 0 163.98 15.50
-8 -4 0 181.48 7.30
8 -4 0 175.78 8.20
-8 -5 0 96.79 4.50
8 -5 0 88.59 4.70
-8 -5 0 88.89 7.80
-9 0 0 -9.10 10.10
9 0 0 3.90 3.80
-9 0 0 -0.70 2.40
-9 0 0 -0.20 1.40
9 0 0 0.40 1.60
-9 1 0 27.70 20.60
9 -1 0 36.10 6.10
-9 1 0 34.10 3.30
9 -1 0 39.20 3.70
9 -1 0 29.30 3.10
-9 -1 0 35.80 3.50
-9 -1 0 43.10 4.80
-9 -1 0 50.49 8.20
-9 -1 0 48.40 17.40
-9 1 0 43.10 5.80
9 -2 0 158.88 12.20
-9 2 0 137.19 9.10
-9 -2 0 147.69 12.00
-9 -2 0 137.99 7.70
-9 2 0 140.29 6.40
9 -2 0 135.49 6.90
9 -2 0 144.59 6.80
-9 -2 0 135.39 6.10
-9 -3 0 88.59 5.20
-9 -3 0 74.39 10.30
-9 -3 0 102.79 7.00
9 -3 0 91.39 11.90
9 -3 0 89.69 6.10
9 -3 0 91.29 5.80
9 -4 0 27.00 7.50
9 -4 0 31.30 3.70
-9 -4 0 36.00 3.50
-9 -4 0 24.80 4.10
-9 -4 0 32.50 8.70
-9 -4 0 39.70 6.90
9 -4 0 28.50 3.70
-9 -5 0 1.40 1.40
9 -5 0 3.30 1.60
9 -5 0 5.10 2.00
-9 -5 0 -1.60 2.90
10 0 0 7.70 2.10
-10 0 0 12.80 12.60
-10 0 0 10.10 2.40
10 0 0 -1.10 5.30
-10 0 0 14.50 4.20
10 -1 0 2.00 2.00
10 -1 0 5.40 2.10
-10 -1 0 3.70 2.90
10 -1 0 8.50 5.00
-10 -1 0 4.80 2.10
-10 1 0 3.70 3.00
-10 1 0 4.00 1.90
-10 -1 0 4.00 2.00
-10 -2 0 19.90 6.80
-10 -2 0 19.80 3.90
10 -2 0 18.70 3.10
-10 -2 0 18.70 2.80
10 -2 0 18.50 3.20
10 -2 0 17.80 6.20
-10 2 0 23.40 3.20
-10 2 0 20.00 5.20
-10 -3 0 4.50 5.30
-10 -3 0 0.00 2.60
-10 -3 0 2.30 2.00
10 -3 0 -1.70 2.20
10 -3 0 1.00 1.70
10 -3 0 0.30 5.00
-10 -4 0 -1.10 7.20
10 -4 0 3.90 6.50
10 -4 0 2.10 1.90
-10 -4 0 2.80 1.70
-10 -4 0 6.50 5.60
-10 -4 0 1.00 3.60
10 -5 0 1.80 1.90
10 -5 0 4.40 1.40
-10 -5 0 0.40 4.00
-10 -5 0 2.20 1.20
-11 0 0 -1.50 2.90
-11 0 0 -1.30 5.00
-11 0 0 -0.70 1.90
-11 0 0 -2.90 3.10
11 0 0 0.20 1.80
-11 -1 0 169.48 6.70
-11 1 0 166.88 11.50
-11 -1 0 155.78 12.50
-11 1 0 163.08 7.70
11 -1 0 166.18 7.60
11 -1 0 157.68 7.20
-11 -1 0 165.68 8.40
11 -1 0 158.28 16.30
-11 -2 0 11.10 2.40
-11 2 0 8.60 5.20
-11 -2 0 8.80 2.90
11 -2 0 8.80 2.40
11 -2 0 10.90 5.70
-11 2 0 14.70 3.30
11 -2 0 13.60 2.60
-11 -2 0 11.80 5.80
-11 -3 0 238.18 18.10
11 -3 0 241.58 11.20
11 -3 0 253.57 11.20
-11 -3 0 220.58 15.80
-11 -3 0 193.98 15.30
-11 -3 0 242.08 9.70
11 -3 0 220.78 17.60
-11 -4 0 2.60 2.60
11 -4 0 3.40 1.90
-11 -4 0 5.00 1.80
11 -4 0 0.90 2.30
-11 -4 0 -6.80 8.20
-12 0 0 21.60 3.80
-12 0 0 13.20 5.30
-12 0 0 27.50 10.10
12 0 0 22.00 3.20
12 -1 0 2.60 2.10
-12 -1 0 1.50 2.40
12 -1 0 2.40 8.30
12 -1 0 1.20 1.80
12 1 0 5.80 1.90
-12 1 0 5.10 2.50
-12 -1 0 4.70 1.90
-12 -1 0 5.00 4.50
-12 1 0 2.80 4.50
-12 -2 0 278.27 19.00
12 -2 0 267.87 20.80
-12 2 0 265.47 16.80
-12 -2 0 281.67 10.00
-12 2 0 263.47 11.20
-12 -2 0 308.97 13.10
12 -2 0 279.27 11.20
12 -2 0 279.27 10.70
-12 -3 0 43.50 5.90
-12 -3 0 30.80 8.50
12 -3 0 47.00 10.90
-12 -3 0 33.00 3.30
12 -3 0 42.80 4.20
12 -3 0 50.19 4.80
-12 -3 0 39.90 8.40
-12 -4 0 6.00 1.70
12 -4 0 5.40 2.00
12 -4 0 11.80 2.80
-12 -4 0 6.20 2.70
-13 0 0 -0.40 3.30
13 0 0 -0.90 1.80
-13 0 0 0.60 2.00
13 1 0 -0.40 1.90
-13 -1 0 -2.20 2.30
13 -1 0 -1.30 2.30
-13 -1 0 -2.20 7.60
13 -1 0 0.00 2.20
-13 -1 0 0.10 2.00
-13 1 0 -1.70 4.50
-13 -1 0 0.20 3.60
-13 1 0 1.40 2.50
-13 -2 0 92.29 7.20
-13 2 0 99.59 7.40
13 -2 0 86.79 5.60
-13 -2 0 84.19 6.20
13 -2 0 83.09 14.80
-13 -2 0 94.49 13.80
13 2 0 90.89 5.90
-13 -2 0 103.39 14.40
13 3 0 24.50 4.00
13 -3 0 21.70 2.90
-13 -3 0 27.90 7.60
-13 -3 0 21.20 4.00
13 -4 0 1.30 1.40
-13 -4 0 -0.20 1.20
-13 -4 0 -1.60 2.10
13 -4 0 1.40 2.10
-14 0 0 3.80 5.10
14 0 0 0.10 2.20
-14 0 0 2.30 2.40
-14 -1 0 9.50 3.30
-14 -1 0 -2.20 11.60
-14 1 0 17.00 4.00
14 -1 0 9.80 3.00
-14 1 0 23.90 7.60
-14 -1 0 13.10 2.40
-14 -1 0 10.90 5.70
14 2 0 1.10 2.50
-14 -2 0 11.70 14.10
-14 -2 0 2.30 3.00
14 -2 0 5.60 2.20
-14 -2 0 1.90 5.80
-14 -2 0 0.50 1.50
14 -2 0 3.70 2.30
-14 -3 0 8.00 7.60
-14 -3 0 5.60 1.70
14 -3 0 8.30 2.50
-14 -3 0 4.80 2.40
14 -3 0 5.30 1.90
-15 0 0 1.20 2.90
15 0 0 2.20 2.10
-15 0 0 -0.50 5.90
-15 -1 0 100.09 7.00
-15 -1 0 105.89 14.50
15 -1 0 83.69 5.80
15 1 0 85.69 5.40
-15 1 0 73.79 11.70
-15 1 0 86.19 7.00
-15 -2 0 4.90 1.80
15 2 0 6.10 2.60
15 -2 0 4.40 2.20
-15 -2 0 3.50 3.00
-15 -2 0 10.60 7.60
-15 -3 0 12.00 1.80
15 -3 0 13.60 1.90
-15 -3 0 15.90 3.30
15 -3 0 14.90 2.80
16 0 0 19.10 2.90
-16 0 0 18.10 3.60
-16 -1 0 60.79 5.80
-16 1 0 57.79 5.70
16 1 0 58.89 4.80
-16 -1 0 50.89 11.10
16 -1 0 60.19 4.90
16 -2 0 110.69 6.10
-16 -2 0 119.19 6.90
16 2 0 111.59 5.80
17 0 0 -1.30 2.60
17 -1 0 -1.80 1.90
17 1 0 1.10 1.90
-17 -1 0 0.70 2.30
-17 -2 0 39.70 4.40
17 -2 0 40.20 3.60
18 0 0 35.00 3.50
18 -1 0 1.00 1.70
18 1 0 5.70 2.30
-18 -1 0 2.40 3.20
0 0 -1 1.10 1.50
0 0 1 0.10 0.30
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14 -3 -8 58.99 3.50
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1 -5 -9 75.39 4.70
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-7 2 -29 4.40 2.60
7 -2 -29 3.60 2.30
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-7 -2 -29 2.90 1.80
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-8 0 -29 5.10 3.20
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8 -1 -29 4.10 2.00
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-8 1 -29 3.00 2.50
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-8 -1 -29 -4.90 2.80
-8 2 -29 -2.00 2.40
8 -2 -29 -0.70 1.80
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-8 -2 -29 0.70 2.00
8 -2 29 2.10 2.10
8 2 -29 0.30 1.80
9 0 29 0.80 1.90
-9 0 -29 4.90 4.10
9 0 -29 1.30 2.00
9 1 29 4.60 2.60
9 -1 -29 2.30 2.00
-9 1 -29 5.60 2.50
9 1 -29 5.50 2.60
9 -2 -29 4.40 2.50
-9 2 -29 0.00 2.50
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0 -2 -30 17.50 3.40
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0 -3 -30 74.29 4.90
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-1 -1 -30 0.20 2.40
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1 -2 -30 -0.80 2.80
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-1 -2 -30 3.40 2.00
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1 -3 -30 121.39 5.00
-1 -3 -30 123.69 5.90
-1 -3 -30 121.89 4.80
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2 0 -30 35.60 4.10
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2 1 -30 125.59 6.40
2 -1 30 123.19 6.40
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-2 2 -30 66.79 11.00
2 -2 -30 95.39 5.50
2 2 -30 103.39 5.70
-2 -2 -30 96.49 5.70
2 -3 -30 39.00 3.40
2 -3 -30 42.20 3.40
-2 -3 -30 43.80 3.10
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-3 1 -30 9.20 4.00
3 -1 -30 9.50 2.90
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-3 -1 -30 7.20 2.50
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3 -2 -30 58.39 4.70
-3 -2 -30 54.09 4.70
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-3 -2 -30 48.10 4.30
-3 3 -30 5.40 2.50
3 -3 -30 0.60 1.90
3 -3 -30 1.20 2.00
-3 -3 -30 3.40 1.90
-3 -3 -30 4.10 1.70
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4 0 -30 59.69 4.90
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-4 1 -30 2.30 2.40
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4 -2 -30 8.30 2.30
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-4 -3 -30 28.40 2.90
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-5 -2 -30 3.50 2.20
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6 -1 -30 24.10 3.20
-6 -1 -30 27.00 3.50
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-6 2 -30 21.50 3.20
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7 -2 -30 18.90 2.70
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7 -2 30 20.60 2.70
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-7 -2 -30 20.80 2.90
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-8 0 -30 33.10 4.40
8 0 -30 28.20 3.00
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-9 1 -30 19.10 3.10
9 -1 -30 12.60 2.20
9 1 -30 14.30 2.30
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10 0 -30 90.99 4.90
-10 0 -30 83.29 7.80
-10 1 -30 4.40 3.40
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10 -1 -30 7.10 1.90
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0 -3 -31 0.00 2.20
-1 0 -31 1.00 1.90
-1 0 31 -1.60 2.20
1 0 -31 -0.80 2.20
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-1 1 -31 16.00 3.40
-1 1 -31 1.40 3.90
1 -1 -31 12.00 2.70
1 1 -31 8.90 2.80
-1 -1 -31 12.10 2.80
1 -1 31 2.40 2.60
-1 2 -31 -3.90 2.20
1 -2 -31 -1.10 1.90
-1 -2 -31 -3.80 2.70
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-1 -2 -31 -0.70 2.10
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1 -3 -31 66.09 4.40
-1 -3 -31 64.09 4.30
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2 -1 -31 28.70 3.60
-2 1 -31 39.10 4.20
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2 -1 31 32.00 3.30
-2 2 -31 1.20 2.50
2 -2 -31 0.70 1.80
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-2 -2 -31 1.90 2.10
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-3 0 -31 2.80 2.60
-3 1 -31 -3.60 2.90
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-3 -1 -31 15.30 2.80
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3 -3 -31 3.50 1.90
-3 -3 -31 2.80 1.60
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5 -1 -31 6.40 2.30
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-5 -1 -31 7.50 2.70
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-6 -2 -31 8.20 2.10
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5 -2 -32 20.20 2.60
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-5 -2 -32 21.90 2.80
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6 -1 32 9.40 2.50
-6 -1 -32 17.30 2.70
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6 -2 -32 4.20 1.90
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-6 2 -32 1.20 2.80
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7 0 32 -2.20 1.70
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7 -1 -32 18.90 2.50
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7 1 -32 17.60 2.60
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8 -1 -32 47.50 3.70
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9 0 -32 -0.40 1.60
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0 -1 -33 0.00 1.90
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2 -2 -33 88.79 4.80
2 2 -33 92.09 6.00
-2 -2 -33 98.69 5.20
-3 0 -33 2.10 2.60
3 0 33 -0.40 1.90
3 0 -33 -0.70 1.90
3 1 33 2.60 1.80
3 -1 -33 1.30 2.10
3 -1 33 4.00 2.30
-3 -1 -33 4.30 3.60
3 -2 -33 23.40 2.80
-3 2 -33 25.80 4.50
3 2 -33 30.70 3.30
-3 -2 -33 24.00 2.90
4 0 33 5.20 2.10
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4 0 -33 -0.30 1.90
4 1 33 -2.00 2.10
4 -1 -33 1.40 2.10
-4 -1 -33 -0.30 2.20
4 -1 33 0.40 2.20
4 1 -33 2.70 2.30
4 -2 -33 15.10 2.60
4 2 33 14.20 2.00
-4 -2 -33 13.80 2.20
5 0 33 1.90 2.30
5 0 -33 0.40 1.90
5 -1 -33 58.39 4.20
5 1 33 59.59 3.80
-5 -1 -33 60.79 4.40
5 -1 33 56.39 4.30
5 1 -33 61.59 4.30
5 2 33 22.50 2.20
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5 -2 -33 20.90 2.40
5 2 -33 27.10 4.20
-5 -2 -33 21.90 2.30
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6 -1 -33 2.70 1.90
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6 -1 33 4.30 2.00
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0 -1 -34 8.00 3.70
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1 1 -34 9.10 2.60
-1 -1 -34 11.00 2.40
1 -2 -34 3.50 2.10
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3 -1 -35 8.70 2.30
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-1 -1 -36 16.30 2.30
1 1 -36 9.20 2.90
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-2 0 -36 24.10 2.90
2 1 36 13.20 3.70
2 -1 -36 11.00 2.10
-2 -1 -36 17.90 2.40
2 1 -36 11.10 2.40
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0 0 0 0.00 0.00
_computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)'
;
_shelx_hkl_checksum 89469
_shelx_res_file
;
TITL obc126v_a.res in Pca2(1)
obc126v.res
created by SHELXL-2019/1 at 12:01:47 on 07-Nov-2023
REM Old TITL OBC126v in Pca2(1)
REM SHELXT solution in Pca2(1): R1 0.091, Rweak 0.004, Alpha 0.002
REM 0.296 for 363 systematic absences, Orientation as input
REM Flack x = -0.051 ( 0.207 ) from 1688 Parsons' quotients
REM Formula found by SHELXT: C30 N O5
CELL 1.54178 15.356 5.04 31.0254 90 90 90
ZERR 8 0.0003 0.0001 0.0007 0 0 0
LATT -1
SYMM -X,-Y,0.5+Z
SYMM 0.5+X,-Y,+Z
SYMM 0.5-X,+Y,0.5+Z
SFAC C H N O
UNIT 120 104 8 16
EQIV $1 +X,-1+Y,+Z
EQIV $2 +X,1+Y,+Z
L.S. 12
PLAN 5
SIZE 0.012 0.026 0.25
TEMP -173.15
CONF
HTAB N1 O1_$1
HTAB N2 O3_$2
list 4
MORE -1
BOND $H
fmap 2
ACTA
OMIT 0 5 0
OMIT 1 5 -2
REM
REM
REM
WGHT 0.029100 0.308900
FVAR 0.43219
O1 4 0.530865 0.715130 0.474511 11.00000 0.02272 0.01468 =
0.03257 -0.00150 -0.00872 -0.00112
O2 4 0.424765 0.438438 0.451150 11.00000 0.02150 0.01674 =
0.02106 0.00428 -0.00750 -0.00408
N1 3 0.536091 0.274124 0.487867 11.00000 0.02220 0.01502 =
0.03182 0.00046 -0.00847 -0.00292
H1A 2 0.514076 0.122631 0.481597 11.00000 0.01870
H1B 2 0.588762 0.295297 0.500698 11.00000 0.03075
C1 1 0.326357 0.563329 0.394492 11.00000 0.01604 0.01918 =
0.01764 0.00231 -0.00100 -0.00192
AFIX 13
H1 2 0.293372 0.398198 0.401756 11.00000 -1.20000
AFIX 0
C2 1 0.264749 0.776764 0.378503 11.00000 0.01448 0.01632 =
0.02197 -0.00272 -0.00552 -0.00355
C3 1 0.194973 0.895534 0.399554 11.00000 0.01771 0.02707 =
0.02313 -0.00392 -0.00050 -0.00141
AFIX 43
H3 2 0.179526 0.844026 0.427999 11.00000 -1.20000
AFIX 0
C4 1 0.148318 1.091325 0.378051 11.00000 0.01462 0.02563 =
0.03877 -0.01031 -0.00223 0.00207
AFIX 43
H4 2 0.100259 1.173510 0.391963 11.00000 -1.20000
AFIX 0
C5 1 0.170854 1.168886 0.336490 11.00000 0.01945 0.02159 =
0.03337 -0.00078 -0.01076 0.00176
AFIX 43
H5 2 0.138392 1.303942 0.322415 11.00000 -1.20000
AFIX 0
C6 1 0.240625 1.049927 0.315410 11.00000 0.02356 0.02163 =
0.02125 0.00122 -0.00474 -0.00059
AFIX 43
H6 2 0.256156 1.102689 0.287037 11.00000 -1.20000
AFIX 0
C7 1 0.287184 0.852796 0.336531 11.00000 0.01354 0.01688 =
0.02250 -0.00202 -0.00370 -0.00267
C8 1 0.361783 0.691562 0.322541 11.00000 0.01451 0.01591 =
0.02079 0.00037 -0.00242 -0.00411
C9 1 0.406253 0.688425 0.283451 11.00000 0.02094 0.02143 =
0.02126 0.00373 0.00017 -0.00131
AFIX 43
H9 2 0.391122 0.808222 0.261028 11.00000 -1.20000
AFIX 0
C10 1 0.473308 0.506136 0.277932 11.00000 0.01971 0.03078 =
0.02479 -0.00126 0.00628 -0.00062
AFIX 43
H10 2 0.503783 0.499597 0.251306 11.00000 -1.20000
AFIX 0
C11 1 0.496164 0.333738 0.310898 11.00000 0.01796 0.02260 =
0.03043 -0.00138 0.00006 0.00194
AFIX 43
H11 2 0.542294 0.210925 0.306624 11.00000 -1.20000
AFIX 0
C12 1 0.452285 0.338490 0.350215 11.00000 0.01918 0.01865 =
0.02355 0.00183 -0.00379 -0.00114
AFIX 43
H12 2 0.468555 0.221720 0.372863 11.00000 -1.20000
AFIX 0
C13 1 0.384453 0.516839 0.355642 11.00000 0.01568 0.01601 =
0.01936 -0.00135 -0.00468 -0.00345
C14 1 0.376771 0.661890 0.433724 11.00000 0.02002 0.01829 =
0.01990 0.00326 -0.00441 0.00070
AFIX 23
H14A 2 0.417409 0.805151 0.425237 11.00000 -1.20000
H14B 2 0.336087 0.732822 0.455632 11.00000 -1.20000
AFIX 0
C15 1 0.500034 0.489874 0.471371 11.00000 0.01604 0.01876 =
0.01485 -0.00197 0.00051 0.00019
O3 4 0.717898 0.328867 0.517742 11.00000 0.02105 0.01417 =
0.03515 -0.00017 -0.00830 -0.00076
O4 4 0.817019 0.605210 0.547878 11.00000 0.02256 0.01438 =
0.02388 0.00200 -0.00790 -0.00169
N2 3 0.711378 0.771991 0.507305 11.00000 0.01949 0.01448 =
0.02633 0.00119 -0.00795 -0.00044
H2A 2 0.662874 0.759439 0.494605 11.00000 0.01897
H2B 2 0.730125 0.928336 0.514662 11.00000 0.03299
C16 1 0.917757 0.465420 0.602160 11.00000 0.01626 0.01846 =
0.01984 0.00198 -0.00304 -0.00119
AFIX 13
H16 2 0.948852 0.635510 0.595949 11.00000 -1.20000
AFIX 0
C17 1 0.982315 0.250261 0.615062 11.00000 0.01495 0.01904 =
0.02225 -0.00019 -0.00428 -0.00315
C18 1 1.050750 0.143402 0.591565 11.00000 0.01625 0.02775 =
0.02478 -0.00318 -0.00194 -0.00301
AFIX 43
H18 2 1.062974 0.204782 0.563253 11.00000 -1.20000
AFIX 0
C19 1 1.101035 -0.054837 0.610178 11.00000 0.01626 0.03109 =
0.03724 -0.00715 -0.00356 0.00084
AFIX 43
H19 2 1.148311 -0.128562 0.594474 11.00000 -1.20000
AFIX 0
C20 1 1.083244 -0.146438 0.651263 11.00000 0.02558 0.02127 =
0.04317 -0.00148 -0.01559 0.00544
AFIX 43
H20 2 1.118190 -0.283160 0.663310 11.00000 -1.20000
AFIX 0
C21 1 1.014683 -0.040804 0.675256 11.00000 0.02392 0.02508 =
0.02552 0.00278 -0.01167 -0.00276
AFIX 43
H21 2 1.002632 -0.103184 0.703529 11.00000 -1.20000
AFIX 0
C22 1 0.964308 0.158838 0.656625 11.00000 0.01833 0.01721 =
0.02045 -0.00079 -0.00563 -0.00325
C23 1 0.889948 0.307634 0.673748 11.00000 0.01827 0.01899 =
0.01765 -0.00003 -0.00437 -0.00531
C24 1 0.848078 0.291578 0.713401 11.00000 0.02604 0.02682 =
0.01672 -0.00144 -0.00296 -0.00932
AFIX 43
H24 2 0.865756 0.164739 0.734293 11.00000 -1.20000
AFIX 0
C25 1 0.779777 0.465153 0.721821 11.00000 0.02580 0.03270 =
0.02361 -0.01041 0.00538 -0.01128
AFIX 43
H25 2 0.751130 0.458980 0.748942 11.00000 -1.20000
AFIX 0
C26 1 0.753066 0.647171 0.691021 11.00000 0.02077 0.02505 =
0.03402 -0.01243 0.00414 -0.00207
AFIX 43
H26 2 0.706041 0.763484 0.697254 11.00000 -1.20000
AFIX 0
C27 1 0.794138 0.661903 0.651128 11.00000 0.01974 0.02022 =
0.02755 -0.00334 -0.00198 -0.00093
AFIX 43
H27 2 0.775450 0.786606 0.630113 11.00000 -1.20000
AFIX 0
C28 1 0.862686 0.491695 0.642610 11.00000 0.01469 0.01862 =
0.02009 -0.00220 -0.00154 -0.00425
C29 1 0.865634 0.376794 0.563140 11.00000 0.02019 0.01663 =
0.01891 0.00285 -0.00246 0.00295
AFIX 23
H29A 2 0.905150 0.311282 0.540284 11.00000 -1.20000
H29B 2 0.825305 0.231754 0.571180 11.00000 -1.20000
AFIX 0
C30 1 0.746317 0.554061 0.523799 11.00000 0.01528 0.01965 =
0.01423 -0.00040 -0.00029 -0.00059
HKLF 4
REM obc126v_a.res in Pca2(1)
REM wR2 = 0.0678, GooF = S = 1.047, Restrained GooF = 1.047 for all data
REM R1 = 0.0295 for 3754 Fo > 4sig(Fo) and 0.0345 for all 4069 data
REM 341 parameters refined using 1 restraints
END
WGHT 0.0291 0.3089
REM Highest difference peak 0.136, deepest hole -0.165, 1-sigma level 0.033
Q1 1 0.7413 0.2601 0.4777 11.00000 0.05 0.14
Q2 1 0.8561 0.3399 0.6512 11.00000 0.05 0.13
Q3 1 0.2210 0.7941 0.3869 11.00000 0.05 0.12
Q4 1 0.3004 0.6864 0.3884 11.00000 0.05 0.11
Q5 1 0.7129 1.0443 0.6992 11.00000 0.05 0.11
;
_shelx_res_checksum 86673
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z+1/2'
'x+1/2, -y, z'
'-x+1/2, y, 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 0.53087(12) 0.7151(3) 0.47451(7) 0.0233(4) Uani d 1 . .
O O2 0.42477(11) 0.4384(3) 0.45115(6) 0.0198(4) Uani d 1 . .
N N1 0.53609(17) 0.2741(4) 0.48787(8) 0.0230(5) Uani d 1 . .
H H1A 0.5141(19) 0.123(6) 0.4816(10) 0.019(7) Uiso d 1 . .
H H1B 0.589(2) 0.295(6) 0.5007(11) 0.031(8) Uiso d 1 . .
C C1 0.32636(17) 0.5633(5) 0.39449(9) 0.0176(6) Uani d 1 . .
H H1 0.293372 0.398198 0.401756 0.021 Uiso calc 1 . .
C C2 0.26475(15) 0.7768(5) 0.37850(9) 0.0176(5) Uani d 1 . .
C C3 0.19497(17) 0.8955(5) 0.39955(9) 0.0226(6) Uani d 1 . .
H H3 0.179526 0.844026 0.427999 0.027 Uiso calc 1 . .
C C4 0.14832(17) 1.0913(6) 0.37805(11) 0.0263(6) Uani d 1 . .
H H4 0.100259 1.173510 0.391963 0.032 Uiso calc 1 . .
C C5 0.17085(18) 1.1689(5) 0.33649(9) 0.0248(6) Uani d 1 . .
H H5 0.138392 1.303942 0.322415 0.030 Uiso calc 1 . .
C C6 0.24063(19) 1.0499(5) 0.31541(10) 0.0221(6) Uani d 1 . .
H H6 0.256156 1.102689 0.287037 0.027 Uiso calc 1 . .
C C7 0.28718(16) 0.8528(5) 0.33653(9) 0.0176(5) Uani d 1 . .
C C8 0.36178(15) 0.6916(5) 0.32254(8) 0.0171(5) Uani d 1 . .
C C9 0.40625(17) 0.6884(5) 0.28345(9) 0.0212(6) Uani d 1 . .
H H9 0.391122 0.808222 0.261028 0.025 Uiso calc 1 . .
C C10 0.4733(2) 0.5061(5) 0.27793(11) 0.0251(7) Uani d 1 . .
H H10 0.503783 0.499597 0.251306 0.030 Uiso calc 1 . .
C C11 0.49616(17) 0.3337(5) 0.31090(10) 0.0237(6) Uani d 1 . .
H H11 0.542294 0.210925 0.306624 0.028 Uiso calc 1 . .
C C12 0.45228(17) 0.3385(5) 0.35021(9) 0.0205(6) Uani d 1 . .
H H12 0.468555 0.221720 0.372863 0.025 Uiso calc 1 . .
C C13 0.38445(19) 0.5168(5) 0.35564(10) 0.0170(6) Uani d 1 . .
C C14 0.37677(17) 0.6619(5) 0.43372(9) 0.0194(5) Uani d 1 . .
H H14A 0.417409 0.805151 0.425237 0.023 Uiso calc 1 . .
H H14B 0.336087 0.732822 0.455632 0.023 Uiso calc 1 . .
C C15 0.50003(18) 0.4899(5) 0.47137(9) 0.0165(6) Uani d 1 . .
O O3 0.71790(12) 0.3289(3) 0.51774(6) 0.0235(4) Uani d 1 . .
O O4 0.81702(12) 0.6052(3) 0.54788(6) 0.0203(4) Uani d 1 . .
N N2 0.71138(16) 0.7720(4) 0.50730(8) 0.0201(5) Uani d 1 . .
H H2A 0.663(2) 0.759(5) 0.4946(10) 0.019(7) Uiso d 1 . .
H H2B 0.730(2) 0.928(7) 0.5147(11) 0.033(9) Uiso d 1 . .
C C16 0.91776(18) 0.4654(5) 0.60216(9) 0.0182(6) Uani d 1 . .
H H16 0.948852 0.635510 0.595949 0.022 Uiso calc 1 . .
C C17 0.98232(16) 0.2503(5) 0.61506(9) 0.0187(5) Uani d 1 . .
C C18 1.05075(16) 0.1434(5) 0.59156(9) 0.0229(6) Uani d 1 . .
H H18 1.062974 0.204782 0.563253 0.028 Uiso calc 1 . .
C C19 1.10103(18) -0.0548(6) 0.61018(11) 0.0282(7) Uani d 1 . .
H H19 1.148311 -0.128562 0.594474 0.034 Uiso calc 1 . .
C C20 1.08324(19) -0.1464(5) 0.65126(11) 0.0300(7) Uani d 1 . .
H H20 1.118190 -0.283160 0.663310 0.036 Uiso calc 1 . .
C C21 1.0147(2) -0.0408(5) 0.67526(10) 0.0248(7) Uani d 1 . .
H H21 1.002632 -0.103184 0.703529 0.030 Uiso calc 1 . .
C C22 0.96431(16) 0.1588(5) 0.65662(9) 0.0187(5) Uani d 1 . .
C C23 0.88995(16) 0.3076(5) 0.67375(8) 0.0183(5) Uani d 1 . .
C C24 0.84808(18) 0.2916(6) 0.71340(9) 0.0232(6) Uani d 1 . .
H H24 0.865756 0.164739 0.734293 0.028 Uiso calc 1 . .
C C25 0.7798(2) 0.4652(6) 0.72182(11) 0.0274(7) Uani d 1 . .
H H25 0.751130 0.458980 0.748942 0.033 Uiso calc 1 . .
C C26 0.75307(19) 0.6472(5) 0.69102(10) 0.0266(6) Uani d 1 . .
H H26 0.706041 0.763484 0.697254 0.032 Uiso calc 1 . .
C C27 0.79414(17) 0.6619(5) 0.65113(9) 0.0225(6) Uani d 1 . .
H H27 0.775450 0.786606 0.630113 0.027 Uiso calc 1 . .
C C28 0.86269(19) 0.4917(5) 0.64261(10) 0.0178(6) Uani d 1 . .
C C29 0.86563(17) 0.3768(5) 0.56314(9) 0.0186(5) Uani d 1 . .
H H29A 0.905150 0.311282 0.540284 0.022 Uiso calc 1 . .
H H29B 0.825305 0.231754 0.571180 0.022 Uiso calc 1 . .
C C30 0.74632(18) 0.5541(5) 0.52380(9) 0.0164(5) Uani 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 0.0227(10) 0.0147(9) 0.0326(11) -0.0011(7) -0.0087(8) -0.0015(8)
O2 0.0215(10) 0.0167(9) 0.0211(10) -0.0041(7) -0.0075(8) 0.0043(7)
N1 0.0222(13) 0.0150(12) 0.0318(14) -0.0029(9) -0.0085(11) 0.0005(10)
C1 0.0160(14) 0.0192(13) 0.0176(14) -0.0019(11) -0.0010(11) 0.0023(10)
C2 0.0145(11) 0.0163(12) 0.0220(14) -0.0035(9) -0.0055(10) -0.0027(11)
C3 0.0177(13) 0.0271(14) 0.0231(15) -0.0014(11) -0.0005(11) -0.0039(11)
C4 0.0146(13) 0.0256(14) 0.0388(18) 0.0021(11) -0.0022(12) -0.0103(14)
C5 0.0194(13) 0.0216(13) 0.0334(16) 0.0018(10) -0.0108(11) -0.0008(11)
C6 0.0236(15) 0.0216(13) 0.0212(15) -0.0006(11) -0.0047(12) 0.0012(11)
C7 0.0135(12) 0.0169(13) 0.0225(14) -0.0027(9) -0.0037(10) -0.0020(10)
C8 0.0145(12) 0.0159(13) 0.0208(14) -0.0041(10) -0.0024(10) 0.0004(10)
C9 0.0209(13) 0.0214(13) 0.0213(14) -0.0013(11) 0.0002(11) 0.0037(10)
C10 0.0197(16) 0.0308(16) 0.0248(18) -0.0006(10) 0.0063(13) -0.0013(12)
C11 0.0180(13) 0.0226(14) 0.0304(16) 0.0019(11) 0.0001(11) -0.0014(11)
C12 0.0192(13) 0.0186(13) 0.0235(15) -0.0011(10) -0.0038(11) 0.0018(11)
C13 0.0157(15) 0.0160(13) 0.0194(15) -0.0034(9) -0.0047(12) -0.0014(10)
C14 0.0200(13) 0.0183(13) 0.0199(14) 0.0007(9) -0.0044(11) 0.0033(11)
C15 0.0160(13) 0.0188(13) 0.0149(14) 0.0002(9) 0.0005(11) -0.0020(10)
O3 0.0211(10) 0.0142(9) 0.0351(12) -0.0008(7) -0.0083(8) -0.0002(8)
O4 0.0226(10) 0.0144(9) 0.0239(10) -0.0017(7) -0.0079(8) 0.0020(8)
N2 0.0195(12) 0.0145(11) 0.0263(13) -0.0004(9) -0.0079(10) 0.0012(9)
C16 0.0163(12) 0.0185(13) 0.0198(15) -0.0012(9) -0.0030(11) 0.0020(11)
C17 0.0150(11) 0.0190(12) 0.0223(14) -0.0031(9) -0.0043(10) -0.0002(10)
C18 0.0163(12) 0.0278(14) 0.0248(15) -0.0030(10) -0.0019(11) -0.0032(11)
C19 0.0163(14) 0.0311(15) 0.0372(18) 0.0008(11) -0.0036(12) -0.0071(13)
C20 0.0256(14) 0.0213(14) 0.0432(19) 0.0054(11) -0.0156(14) -0.0015(12)
C21 0.0239(16) 0.0251(14) 0.0255(16) -0.0028(11) -0.0117(13) 0.0028(12)
C22 0.0183(13) 0.0172(12) 0.0205(14) -0.0033(9) -0.0056(11) -0.0008(10)
C23 0.0183(12) 0.0190(13) 0.0176(14) -0.0053(10) -0.0044(10) 0.0000(10)
C24 0.0260(14) 0.0268(15) 0.0167(13) -0.0093(11) -0.0030(10) -0.0014(11)
C25 0.0258(17) 0.0327(16) 0.0236(18) -0.0113(12) 0.0054(14) -0.0104(12)
C26 0.0208(13) 0.0251(15) 0.0340(17) -0.0021(11) 0.0041(12) -0.0124(12)
C27 0.0197(13) 0.0202(13) 0.0275(15) -0.0009(10) -0.0020(12) -0.0033(11)
C28 0.0147(14) 0.0186(14) 0.0201(16) -0.0043(9) -0.0015(12) -0.0022(10)
C29 0.0202(13) 0.0166(13) 0.0189(13) 0.0030(10) -0.0025(10) 0.0028(10)
C30 0.0153(13) 0.0197(13) 0.0142(14) -0.0006(10) -0.0003(11) -0.0004(11)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 '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
C15 O2 C14 . . 117.54(19) ?
H1A N1 H1B . . 124(3) ?
C15 N1 H1A . . 119(2) ?
C15 N1 H1B . . 116(2) ?
C2 C1 H1 . . 110.4 ?
C2 C1 C13 . . 102.5(2) ?
C2 C1 C14 . . 110.3(2) ?
C13 C1 H1 . . 110.4 ?
C13 C1 C14 . . 112.7(2) ?
C14 C1 H1 . . 110.4 ?
C3 C2 C1 . . 129.3(3) ?
C3 C2 C7 . . 120.6(2) ?
C7 C2 C1 . . 110.2(2) ?
C2 C3 H3 . . 120.7 ?
C4 C3 C2 . . 118.5(3) ?
C4 C3 H3 . . 120.7 ?
C3 C4 H4 . . 119.5 ?
C3 C4 C5 . . 121.1(3) ?
C5 C4 H4 . . 119.5 ?
C4 C5 H5 . . 119.8 ?
C4 C5 C6 . . 120.4(3) ?
C6 C5 H5 . . 119.8 ?
C5 C6 H6 . . 120.6 ?
C7 C6 C5 . . 118.9(3) ?
C7 C6 H6 . . 120.6 ?
C2 C7 C8 . . 108.4(2) ?
C6 C7 C2 . . 120.5(2) ?
C6 C7 C8 . . 131.1(3) ?
C9 C8 C7 . . 130.2(2) ?
C9 C8 C13 . . 120.7(2) ?
C13 C8 C7 . . 109.0(2) ?
C8 C9 H9 . . 120.7 ?
C10 C9 C8 . . 118.6(3) ?
C10 C9 H9 . . 120.7 ?
C9 C10 H10 . . 119.7 ?
C11 C10 C9 . . 120.7(3) ?
C11 C10 H10 . . 119.7 ?
C10 C11 H11 . . 119.6 ?
C10 C11 C12 . . 120.8(2) ?
C12 C11 H11 . . 119.6 ?
C11 C12 H12 . . 120.6 ?
C13 C12 C11 . . 118.7(3) ?
C13 C12 H12 . . 120.6 ?
C8 C13 C1 . . 109.9(2) ?
C12 C13 C1 . . 129.7(3) ?
C12 C13 C8 . . 120.4(3) ?
O2 C14 C1 . . 107.6(2) ?
O2 C14 H14A . . 110.2 ?
O2 C14 H14B . . 110.2 ?
C1 C14 H14A . . 110.2 ?
C1 C14 H14B . . 110.2 ?
H14A C14 H14B . . 108.5 ?
O1 C15 O2 . . 123.1(2) ?
O1 C15 N1 . . 124.4(3) ?
N1 C15 O2 . . 112.5(2) ?
C30 O4 C29 . . 116.43(19) ?
H2A N2 H2B . . 119(3) ?
C30 N2 H2A . . 118.4(19) ?
C30 N2 H2B . . 121(2) ?
C17 C16 H16 . . 110.5 ?
C28 C16 H16 . . 110.5 ?
C28 C16 C17 . . 102.0(2) ?
C29 C16 H16 . . 110.5 ?
C29 C16 C17 . . 110.1(2) ?
C29 C16 C28 . . 113.0(2) ?
C18 C17 C16 . . 129.1(2) ?
C18 C17 C22 . . 120.4(2) ?
C22 C17 C16 . . 110.4(2) ?
C17 C18 H18 . . 120.6 ?
C17 C18 C19 . . 118.8(3) ?
C19 C18 H18 . . 120.6 ?
C18 C19 H19 . . 119.5 ?
C20 C19 C18 . . 120.9(3) ?
C20 C19 H19 . . 119.5 ?
C19 C20 H20 . . 119.6 ?
C19 C20 C21 . . 120.9(3) ?
C21 C20 H20 . . 119.6 ?
C20 C21 H21 . . 120.9 ?
C22 C21 C20 . . 118.2(3) ?
C22 C21 H21 . . 120.9 ?
C17 C22 C23 . . 108.7(2) ?
C21 C22 C17 . . 120.7(3) ?
C21 C22 C23 . . 130.6(3) ?
C24 C23 C22 . . 130.6(2) ?
C24 C23 C28 . . 120.6(2) ?
C28 C23 C22 . . 108.7(2) ?
C23 C24 H24 . . 120.7 ?
C23 C24 C25 . . 118.6(3) ?
C25 C24 H24 . . 120.7 ?
C24 C25 H25 . . 119.7 ?
C26 C25 C24 . . 120.7(3) ?
C26 C25 H25 . . 119.7 ?
C25 C26 H26 . . 119.5 ?
C25 C26 C27 . . 121.0(3) ?
C27 C26 H26 . . 119.5 ?
C26 C27 H27 . . 120.6 ?
C28 C27 C26 . . 118.8(3) ?
C28 C27 H27 . . 120.6 ?
C23 C28 C16 . . 110.2(2) ?
C27 C28 C16 . . 129.5(3) ?
C27 C28 C23 . . 120.4(3) ?
O4 C29 C16 . . 107.33(19) ?
O4 C29 H29A . . 110.2 ?
O4 C29 H29B . . 110.2 ?
C16 C29 H29A . . 110.2 ?
C16 C29 H29B . . 110.2 ?
H29A C29 H29B . . 108.5 ?
O3 C30 O4 . . 123.3(2) ?
O3 C30 N2 . . 124.2(3) ?
N2 C30 O4 . . 112.5(2) ?
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 C15 . 1.234(3) ?
O2 C14 . 1.450(3) ?
O2 C15 . 1.340(3) ?
N1 H1A . 0.86(3) ?
N1 H1B . 0.91(3) ?
N1 C15 . 1.323(4) ?
C1 H1 . 1.0000 ?
C1 C2 . 1.516(4) ?
C1 C13 . 1.518(4) ?
C1 C14 . 1.526(4) ?
C2 C3 . 1.390(4) ?
C2 C7 . 1.400(4) ?
C3 H3 . 0.9500 ?
C3 C4 . 1.390(4) ?
C4 H4 . 0.9500 ?
C4 C5 . 1.391(4) ?
C5 H5 . 0.9500 ?
C5 C6 . 1.391(4) ?
C6 H6 . 0.9500 ?
C6 C7 . 1.388(4) ?
C7 C8 . 1.470(4) ?
C8 C9 . 1.392(4) ?
C8 C13 . 1.397(4) ?
C9 H9 . 0.9500 ?
C9 C10 . 1.391(4) ?
C10 H10 . 0.9500 ?
C10 C11 . 1.387(4) ?
C11 H11 . 0.9500 ?
C11 C12 . 1.394(4) ?
C12 H12 . 0.9500 ?
C12 C13 . 1.386(4) ?
C14 H14A . 0.9900 ?
C14 H14B . 0.9900 ?
O3 C30 . 1.230(3) ?
O4 C29 . 1.451(3) ?
O4 C30 . 1.343(3) ?
N2 H2A . 0.85(3) ?
N2 H2B . 0.87(4) ?
N2 C30 . 1.325(3) ?
C16 H16 . 1.0000 ?
C16 C17 . 1.523(4) ?
C16 C28 . 1.519(4) ?
C16 C29 . 1.518(4) ?
C17 C18 . 1.388(4) ?
C17 C22 . 1.397(4) ?
C18 H18 . 0.9500 ?
C18 C19 . 1.389(4) ?
C19 H19 . 0.9500 ?
C19 C20 . 1.383(5) ?
C20 H20 . 0.9500 ?
C20 C21 . 1.395(4) ?
C21 H21 . 0.9500 ?
C21 C22 . 1.395(4) ?
C22 C23 . 1.466(4) ?
C23 C24 . 1.390(4) ?
C23 C28 . 1.403(4) ?
C24 H24 . 0.9500 ?
C24 C25 . 1.391(4) ?
C25 H25 . 0.9500 ?
C25 C26 . 1.387(5) ?
C26 H26 . 0.9500 ?
C26 C27 . 1.391(4) ?
C27 H27 . 0.9500 ?
C27 C28 . 1.383(4) ?
C29 H29A . 0.9900 ?
C29 H29B . 0.9900 ?
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
N1 H1B O3 1_555 0.91(3) 2.06(3) 2.955(3) 169(3) yes
N1 H1A O1 1_545 0.86(3) 2.08(3) 2.849(3) 149(3) yes
N2 H2A O1 1_555 0.85(3) 2.13(3) 2.967(3) 169(3) yes
N2 H2B O3 1_565 0.87(4) 2.03(4) 2.827(3) 152(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
C1 C2 C3 C4 . . . . 179.2(3) ?
C1 C2 C7 C6 . . . . -178.9(2) ?
C1 C2 C7 C8 . . . . 1.5(3) ?
C2 C1 C13 C8 . . . . 2.8(3) ?
C2 C1 C13 C12 . . . . -178.2(3) ?
C2 C1 C14 O2 . . . . 171.9(2) ?
C2 C3 C4 C5 . . . . -0.4(4) ?
C2 C7 C8 C9 . . . . 178.4(2) ?
C2 C7 C8 C13 . . . . 0.4(3) ?
C3 C2 C7 C6 . . . . 0.6(4) ?
C3 C2 C7 C8 . . . . -179.0(2) ?
C3 C4 C5 C6 . . . . 0.4(4) ?
C4 C5 C6 C7 . . . . 0.1(4) ?
C5 C6 C7 C2 . . . . -0.6(4) ?
C5 C6 C7 C8 . . . . 179.0(3) ?
C6 C7 C8 C9 . . . . -1.2(5) ?
C6 C7 C8 C13 . . . . -179.2(3) ?
C7 C2 C3 C4 . . . . -0.2(4) ?
C7 C8 C9 C10 . . . . -177.3(3) ?
C7 C8 C13 C1 . . . . -2.1(3) ?
C7 C8 C13 C12 . . . . 178.8(2) ?
C8 C9 C10 C11 . . . . -0.9(4) ?
C9 C8 C13 C1 . . . . 179.7(2) ?
C9 C8 C13 C12 . . . . 0.5(4) ?
C9 C10 C11 C12 . . . . 0.3(4) ?
C10 C11 C12 C13 . . . . 0.8(4) ?
C11 C12 C13 C1 . . . . 179.9(3) ?
C11 C12 C13 C8 . . . . -1.2(4) ?
C13 C1 C2 C3 . . . . 178.0(2) ?
C13 C1 C2 C7 . . . . -2.6(3) ?
C13 C1 C14 O2 . . . . -74.2(3) ?
C13 C8 C9 C10 . . . . 0.5(4) ?
C14 O2 C15 O1 . . . . -2.3(4) ?
C14 O2 C15 N1 . . . . 176.8(2) ?
C14 C1 C2 C3 . . . . -61.8(3) ?
C14 C1 C2 C7 . . . . 117.6(2) ?
C14 C1 C13 C8 . . . . -115.7(2) ?
C14 C1 C13 C12 . . . . 63.3(4) ?
C15 O2 C14 C1 . . . . 150.3(2) ?
C16 C17 C18 C19 . . . . -179.5(3) ?
C16 C17 C22 C21 . . . . 179.5(2) ?
C16 C17 C22 C23 . . . . -1.2(3) ?
C17 C16 C28 C23 . . . . -2.3(3) ?
C17 C16 C28 C27 . . . . 178.2(3) ?
C17 C16 C29 O4 . . . . -170.1(2) ?
C17 C18 C19 C20 . . . . 0.4(4) ?
C17 C22 C23 C24 . . . . -179.6(2) ?
C17 C22 C23 C28 . . . . -0.3(3) ?
C18 C17 C22 C21 . . . . 0.1(4) ?
C18 C17 C22 C23 . . . . 179.4(2) ?
C18 C19 C20 C21 . . . . -0.5(4) ?
C19 C20 C21 C22 . . . . 0.3(4) ?
C20 C21 C22 C17 . . . . -0.1(4) ?
C20 C21 C22 C23 . . . . -179.2(3) ?
C21 C22 C23 C24 . . . . -0.3(5) ?
C21 C22 C23 C28 . . . . 178.9(3) ?
C22 C17 C18 C19 . . . . -0.2(4) ?
C22 C23 C24 C25 . . . . 178.0(3) ?
C22 C23 C28 C16 . . . . 1.7(3) ?
C22 C23 C28 C27 . . . . -178.7(2) ?
C23 C24 C25 C26 . . . . 1.1(4) ?
C24 C23 C28 C16 . . . . -179.0(2) ?
C24 C23 C28 C27 . . . . 0.6(4) ?
C24 C25 C26 C27 . . . . -0.4(4) ?
C25 C26 C27 C28 . . . . -0.2(4) ?
C26 C27 C28 C16 . . . . 179.6(3) ?
C26 C27 C28 C23 . . . . 0.1(4) ?
C28 C16 C17 C18 . . . . -178.6(3) ?
C28 C16 C17 C22 . . . . 2.1(3) ?
C28 C16 C29 O4 . . . . 76.7(3) ?
C28 C23 C24 C25 . . . . -1.2(4) ?
C29 O4 C30 O3 . . . . 6.6(4) ?
C29 O4 C30 N2 . . . . -173.0(2) ?
C29 C16 C17 C18 . . . . 61.2(3) ?
C29 C16 C17 C22 . . . . -118.1(2) ?
C29 C16 C28 C23 . . . . 115.9(2) ?
C29 C16 C28 C27 . . . . -63.7(4) ?
C30 O4 C29 C16 . . . . -158.2(2) ?