#------------------------------------------------------------------------------
#$Date: 2022-05-21 03:01:55 +0100 (Sat, 21 May 2022) $
#$Revision: 275591 $
#$URL: svn://www.crystallography.net/cod/cif/2/24/40/2244099.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_2244099
loop_
_publ_author_name
'Lu, Qiang-Qiang'
'Shi, Xin-Wei'
'Zhou, Ya-Fu'
'Cui, Xin-Ai'
'Wang, Hong'
_publ_section_title
;
Crystal structure and Hirshfeld analysis of
(1aS,3aR,4aS,5aR)-15-acetoxylinden-7(11),8-trieno-12,8-lactone
;
_journal_coeditor_code ZN2018
_journal_issue 6
_journal_name_full 'Acta Crystallographica Section E'
_journal_page_first 1
_journal_page_last 0
_journal_paper_doi 10.1107/S2056989022004625
_journal_volume 78
_journal_year 2022
_chemical_absolute_configuration unk
_chemical_formula_iupac 'C17 H20 O4'
_chemical_formula_moiety 'C17 H20 O4'
_chemical_formula_sum 'C17 H20 O4'
_chemical_formula_weight 288.33
_chemical_name_common
(1aS,3aR,4aS,5aR)-15-Acetoxylinden-7(11),8-trieno-12,8-lactone
_chemical_name_systematic
(4aR,5S,5aR,6aS,6bR)-5-(Acetoxymethyl)-4a,5,5a,6,6a,6b-hexahydro-3,6b-dimethylcyclopropa[2,3]indeno[5,6-b]furan-2(4H)-one
_space_group_crystal_system orthorhombic
_space_group_IT_number 19
_space_group_name_Hall 'P 2ac 2ab'
_space_group_name_H-M_alt 'P 21 21 21'
_atom_sites_solution_hydrogens geom
_audit_creation_method SHELXL-2014/7
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_formula_units_Z 4
_cell_length_a 6.7641(3)
_cell_length_b 6.9254(3)
_cell_length_c 31.4538(14)
_cell_measurement_reflns_used 3545
_cell_measurement_temperature 296(2)
_cell_measurement_theta_max 20.68
_cell_measurement_theta_min 2.59
_cell_volume 1473.42(11)
_computing_cell_refinement
;
SMART (Bruker, 2002)
;
_computing_data_collection
;
SMART (Bruker, 2002)
;
_computing_data_reduction
;
SAINT (Bruker, 2002)
;
_computing_molecular_graphics
;
OLEX2 (Dolomanov et al., 2009)
;
_computing_publication_material
;
publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT2014 (Sheldrick, 2015a)
;
_diffrn_ambient_temperature 296(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type 'Bruker SMART CCD'
_diffrn_measurement_method 'phi and omega scans'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0567
_diffrn_reflns_av_unetI/netI 0.0534
_diffrn_reflns_limit_h_max 8
_diffrn_reflns_limit_h_min -7
_diffrn_reflns_limit_k_max 6
_diffrn_reflns_limit_k_min -8
_diffrn_reflns_limit_l_max 37
_diffrn_reflns_limit_l_min -32
_diffrn_reflns_number 12659
_diffrn_reflns_theta_full 25.020
_diffrn_reflns_theta_max 25.020
_diffrn_reflns_theta_min 2.590
_exptl_absorpt_coefficient_mu 0.092
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
(SADABS; Sheldrick, 1996)
;
_exptl_crystal_colour colorless
_exptl_crystal_density_diffrn 1.300
_exptl_crystal_description block
_exptl_crystal_F_000 616
_exptl_crystal_size_max 0.200
_exptl_crystal_size_mid 0.200
_exptl_crystal_size_min 0.200
_refine_diff_density_max 0.299
_refine_diff_density_min -0.209
_refine_ls_abs_structure_details
;
Flack x determined using 574 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons et al., 2013)
;
_refine_ls_abs_structure_Flack 0.10(8)
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.054
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 193
_refine_ls_number_reflns 2576
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.054
_refine_ls_R_factor_all 0.0842
_refine_ls_R_factor_gt 0.0505
_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^)+(0.0466P)^2^+0.3800P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1014
_refine_ls_wR_factor_ref 0.1168
_reflns_number_gt 1857
_reflns_number_total 2576
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file zn2018sup1.cif
_cod_data_source_block I
_cod_database_code 2244099
_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 0.982
_shelx_estimated_absorpt_t_max 0.982
_shelx_hkl_file
;
-1 0 0 2.00 3.40
-1 0 0 2.80 3.40
1 0 0 15.60 4.50
1 0 0 -1.30 2.00
-2 0 0 2998.70 68.29
-2 0 0 2962.50 70.39
2 0 0 3055.09 69.19
2 0 0 3049.89 71.49
-3 0 0 4.60 8.40
-3 0 0 -6.90 5.50
3 0 0 5.60 6.10
3 0 0 -4.70 5.40
-4 0 0 36.70 12.40
-4 0 0 35.80 13.10
4 0 0 52.89 14.70
4 0 0 49.70 15.90
-5 0 0 7.10 12.10
5 0 0 -3.40 5.60
5 0 0 2.10 9.20
6 0 0 -14.20 8.90
7 0 0 -13.70 13.40
7 0 0 -25.30 13.00
8 0 0 20.30 23.20
7 -1 0 37.10 18.20
7 -1 0 -6.60 15.30
7 -1 0 46.20 21.00
6 -1 0 84.09 21.90
6 -1 0 56.79 21.00
6 -1 0 119.39 24.70
6 -1 0 59.29 21.30
5 -1 0 409.96 36.00
5 -1 0 446.86 37.80
5 -1 0 374.06 33.70
5 -1 0 462.35 38.10
4 -1 0 356.36 29.60
4 -1 0 378.16 29.90
4 -1 0 374.66 30.40
3 -1 0 26.30 9.80
3 -1 0 27.90 9.60
3 -1 0 34.70 10.50
3 -1 0 25.10 8.80
2 -1 0 95.89 10.80
2 -1 0 100.89 11.50
2 -1 0 97.79 13.80
0 -1 0 19.00 3.50
0 -1 0 15.50 6.10
0 1 0 22.30 3.60
0 1 0 9.40 3.80
-2 -1 0 87.69 13.80
-2 -1 0 114.19 16.60
2 1 0 109.09 13.70
2 1 0 104.09 15.30
-3 -1 0 7.60 8.70
-3 -1 0 15.90 10.10
3 1 0 16.10 8.80
3 1 0 38.20 11.20
-4 -1 0 371.66 30.90
-4 -1 0 366.46 32.60
4 1 0 319.57 31.10
4 1 0 413.16 32.50
-5 -1 0 481.55 42.60
-5 -1 0 391.96 35.70
5 1 0 394.36 36.10
5 1 0 398.56 38.10
-6 -1 0 45.10 19.90
-6 -1 0 75.59 23.20
6 1 0 59.49 20.60
6 1 0 68.69 23.10
-7 -1 0 56.29 21.10
7 1 0 11.20 16.90
7 -2 0 -1.80 12.40
7 -2 0 16.90 18.30
6 -2 0 19.90 12.70
6 -2 0 7.00 11.40
6 -2 0 10.20 11.30
6 -2 0 43.40 17.20
5 -2 0 110.29 20.80
5 -2 0 109.49 23.90
5 -2 0 90.99 20.30
5 -2 0 88.29 19.20
4 -2 0 179.78 26.50
4 -2 0 153.48 19.20
4 -2 0 171.78 20.90
4 -2 0 138.29 22.50
3 -2 0 762.62 40.30
3 -2 0 756.92 34.00
3 -2 0 825.32 34.80
-3 2 0 701.53 38.50
2 -2 0 951.40 31.20
2 -2 0 968.50 41.70
-2 2 0 1024.90 41.90
1 -2 0 4217.68 92.39
1 -2 0 4102.19 70.09
-1 2 0 4232.08 70.69
-1 2 0 4045.90 90.49
-1 -2 0 3969.00 92.99
-1 -2 0 4068.99 86.79
1 2 0 4146.98 94.69
1 2 0 4250.07 88.59
-2 -2 0 974.40 42.90
-2 -2 0 1019.80 44.40
2 2 0 965.70 43.40
2 2 0 939.31 43.80
-3 -2 0 832.22 44.50
-3 -2 0 774.42 44.50
3 2 0 739.13 43.60
3 2 0 718.43 41.90
-4 -2 0 192.28 28.40
-4 -2 0 142.39 25.50
4 2 0 181.08 27.70
4 2 0 171.08 28.10
-5 -2 0 126.19 26.20
-5 -2 0 131.69 26.60
5 2 0 116.59 26.30
5 2 0 119.29 27.60
-6 -2 0 12.90 16.40
-6 -2 0 -8.80 16.10
6 2 0 32.80 21.40
6 2 0 -9.50 13.00
6 -3 0 8.70 10.80
6 -3 0 -3.10 13.50
6 -3 0 -3.00 13.30
5 -3 0 161.68 23.70
5 -3 0 191.88 33.10
5 -3 0 187.28 31.50
5 -3 0 160.08 24.80
4 -3 0 -11.00 8.40
4 -3 0 17.90 9.40
-4 3 0 29.10 14.60
3 -3 0 298.67 20.40
3 -3 0 293.87 28.80
3 -3 0 321.67 20.90
-3 3 0 315.67 29.30
2 -3 0 65.69 16.60
2 -3 0 43.80 8.40
-2 3 0 63.89 16.50
-2 3 0 61.89 9.10
1 -3 0 3334.27 64.79
1 -3 0 3187.38 90.89
-1 3 0 3310.57 64.69
-1 3 0 3311.47 91.09
0 -3 0 6.40 8.00
0 -3 0 -1.40 3.80
0 3 0 10.00 8.50
0 3 0 5.80 5.10
-1 -3 0 3433.66 82.39
-1 -3 0 3200.28 91.99
1 3 0 3180.28 81.09
1 3 0 3115.19 91.39
-2 -3 0 73.09 15.80
-2 -3 0 63.49 16.60
2 3 0 78.99 16.70
2 3 0 53.69 16.20
-3 -3 0 297.27 31.20
-3 -3 0 325.27 31.00
3 3 0 316.57 30.80
3 3 0 332.07 31.80
-4 -3 0 6.60 11.60
-4 -3 0 0.40 10.60
4 3 0 7.00 12.80
4 3 0 16.70 13.00
-5 -3 0 177.08 33.10
-5 -3 0 225.68 37.50
5 3 0 162.08 31.10
5 3 0 177.48 34.60
-6 -3 0 -24.40 10.20
-6 -3 0 45.70 21.30
6 3 0 -14.30 12.10
-7 -3 0 85.69 31.90
-7 -3 0 132.39 38.30
6 -4 0 46.50 20.90
5 -4 0 -3.90 12.80
4 -4 0 -0.10 7.00
4 -4 0 30.00 16.70
4 -4 0 11.40 8.70
-4 4 0 -15.60 10.40
3 -4 0 136.39 14.10
3 -4 0 164.48 15.40
3 -4 0 134.59 25.30
-3 4 0 131.49 24.80
2 -4 0 3.90 5.20
2 -4 0 5.00 10.10
-2 4 0 0.40 7.70
-2 4 0 0.80 4.30
1 -4 0 1.90 5.00
1 -4 0 23.70 12.90
-1 4 0 0.70 5.50
-1 4 0 -6.70 7.70
0 -4 0 7213.28 169.78
0 -4 0 7370.46 137.29
0 4 0 7431.76 168.88
0 4 0 7064.29 135.79
-1 -4 0 -8.30 5.60
-1 -4 0 1.50 10.00
1 4 0 -1.70 8.00
1 4 0 8.70 10.80
-2 -4 0 0.60 9.80
-2 -4 0 -1.10 7.50
2 4 0 13.00 9.50
2 4 0 3.70 10.70
-3 -4 0 222.88 27.80
-3 -4 0 139.79 28.20
3 4 0 132.59 26.40
3 4 0 117.19 27.10
-4 -4 0 1.50 10.20
-4 -4 0 23.00 16.80
4 4 0 27.30 17.60
4 4 0 -1.10 12.30
-5 -4 0 3.00 16.10
-5 -4 0 8.00 13.40
5 4 0 0.50 16.10
5 4 0 21.80 16.80
-6 -4 0 42.70 22.60
-6 -4 0 21.20 19.70
-7 -4 0 -11.90 17.30
-7 -4 0 0.30 23.50
6 -5 0 19.10 19.90
5 -5 0 363.36 45.40
-5 5 0 407.16 48.20
-4 5 0 252.67 45.10
3 -5 0 27.50 18.50
-3 5 0 47.70 19.50
2 -5 0 8.40 14.60
2 -5 0 13.50 6.20
-2 5 0 15.80 13.00
-2 5 0 16.80 7.10
1 -5 0 1195.58 68.19
1 -5 0 1254.87 42.50
-1 5 0 1313.27 43.50
-1 5 0 1286.27 68.19
0 -5 0 0.20 6.90
0 -5 0 -0.10 12.10
0 5 0 -5.50 7.60
0 5 0 -17.50 11.10
-1 -5 0 1367.96 56.99
-1 -5 0 1333.77 71.19
1 5 0 1321.07 58.39
1 5 0 1321.27 72.29
-2 -5 0 13.00 15.30
-2 -5 0 10.30 11.80
2 5 0 22.80 13.60
2 5 0 10.00 14.80
-3 -5 0 12.50 17.30
-3 -5 0 12.70 14.00
3 5 0 28.00 17.90
3 5 0 4.60 12.50
-4 -5 0 292.87 44.40
-4 -5 0 220.48 37.40
4 5 0 245.08 42.40
4 5 0 234.38 39.00
-5 -5 0 349.77 51.59
-5 -5 0 270.17 44.40
-6 -5 0 18.60 22.80
-6 -5 0 3.70 23.50
5 -6 0 11.90 21.20
4 -6 0 6.60 17.30
3 -6 0 83.39 27.80
-3 6 0 108.19 26.90
2 -6 0 -18.90 14.60
-2 6 0 11.50 14.50
1 -6 0 10.90 17.10
-1 6 0 7.20 14.10
0 -6 0 3150.38 124.59
0 -6 0 3125.09 86.39
0 6 0 2973.80 119.69
0 6 0 2999.70 88.29
-1 -6 0 -23.20 12.60
-1 -6 0 -9.30 9.20
1 6 0 -2.10 11.40
-2 -6 0 12.80 13.00
-2 -6 0 0.20 15.10
2 6 0 -7.90 13.30
2 6 0 0.00 14.00
-3 -6 0 84.09 26.50
-3 -6 0 102.79 31.00
3 6 0 73.19 24.40
-4 -6 0 14.70 16.00
-4 -6 0 -3.70 17.50
-5 -6 0 -14.00 16.80
-5 -6 0 -12.30 17.80
4 -7 0 13.20 20.70
3 -7 0 89.09 29.20
2 -7 0 33.10 24.80
1 -7 0 52.19 22.50
0 -7 0 20.30 16.60
-1 -7 0 -2.10 19.30
-2 -7 0 19.20 22.00
-3 -7 0 94.19 31.70
-3 -7 0 46.10 20.70
-4 -7 0 40.40 21.50
-4 -7 0 0.30 23.50
1 -8 0 1.70 18.10
0 -8 0 166.98 38.60
-1 -8 0 24.90 19.40
-1 -8 1 216.78 45.60
0 -8 1 -13.60 21.70
1 -8 1 188.68 44.40
-4 -7 1 -32.70 21.30
-4 -7 1 25.40 18.70
-3 -7 1 33.90 26.10
-3 -7 1 45.50 19.40
-2 -7 1 93.69 29.70
-2 -7 1 81.59 34.20
-1 -7 1 149.79 35.40
0 -7 1 66.29 28.30
1 -7 1 163.68 39.20
2 -7 1 91.39 31.50
3 -7 1 30.60 23.80
4 -7 1 3.60 22.40
-5 -6 1 18.80 19.70
-5 -6 1 35.00 23.10
-4 -6 1 104.89 34.30
-4 -6 1 96.99 29.20
3 6 -1 -5.90 15.00
-3 -6 1 -26.70 12.80
-3 -6 1 10.30 13.10
2 6 -1 81.59 23.40
2 6 -1 72.19 20.80
-2 -6 1 84.69 21.20
-2 -6 1 72.69 24.60
1 6 -1 526.85 50.89
1 6 -1 551.74 41.60
-1 -6 1 489.45 37.50
-1 -6 1 544.85 52.79
0 6 -1 -26.40 10.50
0 6 -1 -4.40 15.60
0 -6 1 -8.10 15.70
0 -6 1 37.10 14.40
-1 6 -1 488.05 48.40
1 -6 1 490.95 50.09
-2 6 -1 53.89 22.30
2 -6 1 72.29 22.20
-3 6 -1 -39.00 14.60
3 -6 1 1.80 15.60
4 -6 1 106.29 31.00
5 -6 1 46.30 22.60
-6 -5 1 -15.10 23.10
-6 -5 1 -25.30 26.90
-5 -5 1 -25.80 12.70
-5 -5 1 23.30 15.50
4 5 -1 11.90 14.90
4 5 -1 35.80 23.80
-4 -5 1 -3.80 12.00
-4 -5 1 55.99 19.50
3 5 -1 120.89 27.80
3 5 -1 151.08 28.70
-3 -5 1 92.99 22.00
2 5 -1 164.58 31.10
2 5 -1 147.49 25.30
-2 -5 1 94.39 24.90
-2 -5 1 194.68 28.90
1 5 -1 189.58 31.40
1 5 -1 267.97 28.40
-1 -5 1 216.68 35.20
-1 -5 1 238.88 24.60
0 5 -1 1157.38 65.89
0 5 -1 1104.19 47.20
0 -5 1 1092.39 65.09
-1 5 -1 234.78 35.70
-1 5 -1 284.37 21.90
1 -5 1 249.58 37.90
1 -5 1 205.38 19.30
-2 5 -1 211.68 33.10
-2 5 -1 142.19 14.60
2 -5 1 146.29 31.40
2 -5 1 168.78 15.30
-3 5 -1 124.09 29.00
3 -5 1 111.29 27.80
-4 5 -1 17.10 17.20
4 -5 1 53.69 22.40
-5 5 -1 24.10 20.40
5 -5 1 38.60 21.90
6 -5 1 12.50 18.70
-7 -4 1 -7.10 21.30
-7 -4 1 64.89 29.30
-6 -4 1 249.48 43.80
-6 -4 1 165.88 34.80
5 4 -1 85.69 27.60
5 4 -1 60.59 21.90
-5 -4 1 83.29 25.80
-5 -4 1 86.99 26.40
4 4 -1 356.96 40.70
4 4 -1 337.87 39.10
-4 -4 1 344.67 38.90
-4 -4 1 307.47 37.70
3 4 -1 15.20 11.80
3 4 -1 -4.40 7.10
-3 -4 1 10.30 12.80
-3 -4 1 -9.80 9.90
2 4 -1 122.59 25.90
2 4 -1 169.48 25.00
-2 -4 1 173.98 28.80
-2 -4 1 166.08 24.30
1 4 -1 2004.70 79.89
1 4 -1 1963.50 67.09
-1 -4 1 1950.40 65.49
-1 -4 1 2144.59 82.59
0 4 -1 66.69 14.20
0 4 -1 83.39 20.60
0 -4 1 81.39 20.80
0 -4 1 82.59 14.20
-1 4 -1 1991.60 53.19
-1 4 -1 1880.01 75.39
1 -4 1 2024.80 53.49
1 -4 1 1977.60 78.89
-2 4 -1 149.29 13.60
-2 4 -1 161.68 26.70
2 -4 1 143.09 13.90
2 -4 1 122.89 23.20
-3 4 -1 -6.20 10.40
3 -4 1 5.60 7.10
3 -4 1 -3.30 10.30
-4 4 -1 380.76 38.90
4 -4 1 338.87 37.40
4 -4 1 299.47 24.30
4 -4 1 360.36 26.20
5 -4 1 39.10 20.30
6 -4 1 271.77 61.69
6 -4 1 223.98 38.60
-7 -3 1 43.20 28.70
-7 -3 1 95.49 30.70
6 3 -1 22.20 17.90
-6 -3 1 14.90 16.30
-6 -3 1 1.10 13.60
5 3 -1 31.50 19.20
5 3 -1 36.50 20.10
-5 -3 1 69.29 22.70
-5 -3 1 91.89 22.80
4 3 -1 79.79 21.50
4 3 -1 123.99 26.60
-4 -3 1 137.99 25.00
-4 -3 1 148.59 27.20
3 3 -1 859.81 50.79
3 3 -1 865.11 50.49
-3 -3 1 917.61 51.69
-3 -3 1 882.91 51.19
2 3 -1 5571.64 130.19
2 3 -1 5612.54 136.59
-2 -3 1 5522.45 128.59
-2 -3 1 5538.65 133.89
1 3 -1 190.98 22.60
1 3 -1 155.18 17.30
-1 -3 1 177.18 19.00
-1 -3 1 181.78 22.60
0 3 -1 14.30 9.20
0 3 -1 19.50 7.20
0 -3 1 10.90 6.10
0 -3 1 10.10 8.70
-1 3 -1 226.28 22.30
-1 3 -1 176.68 13.80
1 -3 1 180.68 14.40
1 -3 1 184.38 22.10
-2 3 -1 5533.55 130.29
-2 3 -1 5553.14 101.19
2 -3 1 5619.74 132.99
2 -3 1 5412.56 100.79
-3 3 -1 903.91 49.00
3 -3 1 912.61 50.09
3 -3 1 903.91 36.30
3 -3 1 896.61 36.70
-4 3 -1 126.09 24.60
4 -3 1 108.89 23.50
4 -3 1 111.69 18.20
4 -3 1 150.28 18.80
5 -3 1 51.39 16.80
5 -3 1 71.19 21.90
5 -3 1 46.70 15.10
5 -3 1 53.59 19.80
6 -3 1 22.40 19.20
6 -3 1 -3.00 12.20
7 -3 1 46.30 24.90
-7 -2 1 -15.20 14.40
-7 -2 1 30.90 20.80
6 2 -1 221.88 36.10
6 2 -1 134.89 29.70
-6 -2 1 237.38 41.20
-6 -2 1 220.98 37.90
5 2 -1 49.30 18.10
5 2 -1 49.90 19.10
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_computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)'
;
_shelx_hkl_checksum 47606
_shelx_res_file
;
1_a.res created by SHELXL-2014/7
TITL 1_a.res in P2(1)2(1)2(1)
CELL 0.71073 6.7641 6.9254 31.4538 90 90 90
ZERR 4 0.0003 0.0003 0.0014 0 0 0
LATT -1
SYMM 0.5-X,-Y,0.5+Z
SYMM -X,0.5+Y,0.5-Z
SYMM 0.5+X,0.5-Y,-Z
SFAC C H O
UNIT 68 80 16
EQIV $1 0.5+X,0.5-Y,1-Z
EQIV $2 -1+X,+Y,+Z
EQIV $3 0.5+X,1.5-Y,1-Z
EQIV $4 +X,1+Y,+Z
EQIV $5 2-X,-0.5+Y,0.5-Z
L.S. 24
PLAN 1
SIZE 0.2 0.2 0.2
TEMP 23
CONF
HTAB C8 O1_$1
HTAB C11 O3_$2
HTAB C13 O1_$3
HTAB C13 O4_$4
HTAB C14 O2_$1
HTAB C17 O3_$5
BOND $H
LIST 4
fmap 2
acta
MORE -1
OMIT 0 0 2
REM
REM
REM
WGHT 0.046600 0.380000
FVAR 1.46913
O1 3 0.165757 0.514443 0.547927 11.00000 0.10619 0.07374 =
0.04368 -0.00193 0.02832 0.01694
O2 3 0.132854 0.530310 0.476831 11.00000 0.05923 0.05913 =
0.04268 -0.00212 0.01821 0.00348
O3 3 0.915065 0.152013 0.316677 11.00000 0.07552 0.04217 =
0.05202 -0.00384 0.02674 0.00309
O4 3 0.931451 -0.160042 0.328440 11.00000 0.13685 0.05797 =
0.18360 0.01399 0.10079 0.01310
C1 1 0.244562 0.514001 0.513659 11.00000 0.08018 0.04038 =
0.04029 -0.00126 0.01367 0.01289
C2 1 0.453895 0.495964 0.502137 11.00000 0.06852 0.03638 =
0.03908 -0.00258 0.00373 0.00197
C3 1 0.464786 0.499073 0.459523 11.00000 0.05445 0.03441 =
0.03658 -0.00071 0.00369 -0.00023
C4 1 0.265027 0.521464 0.442819 11.00000 0.04942 0.04289 =
0.04031 -0.00298 0.01132 0.00039
C5 1 0.214340 0.538620 0.402499 11.00000 0.03756 0.05240 =
0.04416 -0.00346 0.00272 -0.00308
AFIX 43
H5 2 0.082887 0.549525 0.394173 11.00000 -1.20000
AFIX 0
C6 1 0.381009 0.539612 0.370593 11.00000 0.03947 0.04486 =
0.03242 -0.00235 0.00049 -0.00527
C7 1 0.546502 0.405666 0.387456 11.00000 0.04161 0.04045 =
0.03398 -0.00332 0.00457 -0.00541
AFIX 13
H7 2 0.480207 0.283896 0.394432 11.00000 -1.20000
AFIX 0
C8 1 0.634521 0.476532 0.429370 11.00000 0.04443 0.04662 =
0.03663 -0.00449 -0.00072 -0.00275
AFIX 23
H8A 2 0.728976 0.383584 0.440307 11.00000 -1.20000
H8B 2 0.701411 0.599055 0.425323 11.00000 -1.20000
AFIX 0
C9 1 0.674870 0.360289 0.348361 11.00000 0.04456 0.04063 =
0.03901 -0.00397 0.00515 -0.00549
AFIX 13
H9 2 0.758580 0.471344 0.341375 11.00000 -1.20000
AFIX 0
C10 1 0.516911 0.332231 0.314092 11.00000 0.05366 0.05846 =
0.03866 -0.01198 0.00489 -0.00519
AFIX 13
H10 2 0.498834 0.202536 0.302251 11.00000 -1.20000
AFIX 0
C11 1 0.334041 0.443518 0.327840 11.00000 0.04354 0.06779 =
0.04041 -0.00665 0.00195 -0.01150
AFIX 13
H11 2 0.204706 0.381768 0.324329 11.00000 -1.20000
AFIX 0
C12 1 0.446140 0.500297 0.288644 11.00000 0.06118 0.09054 =
0.03216 0.00170 -0.00024 -0.00201
AFIX 23
H12A 2 0.385323 0.473868 0.261328 11.00000 -1.20000
H12B 2 0.523524 0.618114 0.289736 11.00000 -1.20000
AFIX 0
C13 1 0.447687 0.749637 0.365590 11.00000 0.05711 0.04789 =
0.05182 0.00534 0.00047 -0.00588
AFIX 137
H13A 2 0.346892 0.821677 0.351096 11.00000 -1.50000
H13B 2 0.567883 0.753908 0.349388 11.00000 -1.50000
H13C 2 0.470098 0.805026 0.393151 11.00000 -1.50000
AFIX 0
C14 1 0.612706 0.476415 0.534501 11.00000 0.09326 0.05782 =
0.04399 -0.00274 -0.00626 0.00437
AFIX 137
H14A 2 0.604703 0.351249 0.547504 11.00000 -1.50000
H14B 2 0.596754 0.574292 0.555839 11.00000 -1.50000
H14C 2 0.739252 0.491075 0.521065 11.00000 -1.50000
AFIX 0
C15 1 0.800327 0.183155 0.355113 11.00000 0.06190 0.04569 =
0.03884 -0.00287 0.01528 -0.00078
AFIX 23
H15A 2 0.887714 0.201853 0.379215 11.00000 -1.20000
H15B 2 0.717061 0.072037 0.360755 11.00000 -1.20000
AFIX 0
C16 1 0.974538 -0.022987 0.307231 11.00000 0.04712 0.04786 =
0.07012 -0.00691 0.01339 -0.00583
C17 1 1.101652 -0.030542 0.268934 11.00000 0.06275 0.07123 =
0.06396 -0.01698 0.01369 0.00605
AFIX 137
H17A 2 1.217920 0.046152 0.273540 11.00000 -1.50000
H17B 2 1.030060 0.019179 0.244962 11.00000 -1.50000
H17C 2 1.139378 -0.161853 0.263473 11.00000 -1.50000
AFIX 0
HKLF 4
REM 1_a.res in P2(1)2(1)2(1)
REM R1 = 0.0505 for 1857 Fo > 4sig(Fo) and 0.0842 for all 2576 data
REM 193 parameters refined using 0 restraints
END
WGHT 0.0468 0.3794
REM Highest difference peak 0.299, deepest hole -0.209, 1-sigma level 0.036
Q1 1 0.8232 -0.1160 0.3010 11.00000 0.05 0.30
;
_shelx_res_checksum 53481
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
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 0.1658(5) 0.5144(4) 0.54793(8) 0.0745(9) Uani d 1 . .
O O2 0.1329(4) 0.5303(4) 0.47683(7) 0.0537(7) Uani d 1 . .
O O3 0.9151(4) 0.1520(4) 0.31668(8) 0.0566(8) Uani d 1 . .
O O4 0.9315(6) -0.1600(5) 0.32844(14) 0.1261(18) Uani d 1 . .
C C1 0.2446(6) 0.5140(6) 0.51366(12) 0.0536(10) Uani d 1 . .
C C2 0.4539(6) 0.4960(5) 0.50214(10) 0.0480(9) Uani d 1 . .
C C3 0.4648(5) 0.4991(5) 0.45952(10) 0.0418(8) Uani d 1 . .
C C4 0.2650(5) 0.5215(5) 0.44282(11) 0.0442(9) Uani d 1 . .
C C5 0.2143(5) 0.5386(5) 0.40250(11) 0.0447(10) Uani d 1 . .
H H5 0.0829 0.5495 0.3942 0.054 Uiso calc 1 . .
C C6 0.3810(5) 0.5396(5) 0.37059(10) 0.0389(9) Uani d 1 . .
C C7 0.5465(5) 0.4057(5) 0.38746(10) 0.0387(9) Uani d 1 . .
H H7 0.4802 0.2839 0.3944 0.046 Uiso calc 1 . .
C C8 0.6345(5) 0.4765(6) 0.42937(10) 0.0426(9) Uani d 1 . .
H H8A 0.7290 0.3836 0.4403 0.051 Uiso calc 1 . .
H H8B 0.7014 0.5991 0.4253 0.051 Uiso calc 1 . .
C C9 0.6749(5) 0.3603(5) 0.34836(10) 0.0414(9) Uani d 1 . .
H H9 0.7586 0.4713 0.3414 0.050 Uiso calc 1 . .
C C10 0.5169(6) 0.3322(6) 0.31409(11) 0.0503(10) Uani d 1 . .
H H10 0.4988 0.2025 0.3023 0.060 Uiso calc 1 . .
C C11 0.3340(6) 0.4435(6) 0.32784(11) 0.0506(11) Uani d 1 . .
H H11 0.2047 0.3818 0.3243 0.061 Uiso calc 1 . .
C C12 0.4461(6) 0.5003(7) 0.28864(10) 0.0613(11) Uani d 1 . .
H H12A 0.3853 0.4739 0.2613 0.074 Uiso calc 1 . .
H H12B 0.5235 0.6181 0.2897 0.074 Uiso calc 1 . .
C C13 0.4477(6) 0.7496(5) 0.36559(12) 0.0523(11) Uani d 1 . .
H H13A 0.3469 0.8217 0.3511 0.078 Uiso calc 1 . .
H H13B 0.5679 0.7539 0.3494 0.078 Uiso calc 1 . .
H H13C 0.4701 0.8050 0.3932 0.078 Uiso calc 1 . .
C C14 0.6127(7) 0.4764(6) 0.53450(12) 0.0650(12) Uani d 1 . .
H H14A 0.6047 0.3512 0.5475 0.098 Uiso calc 1 . .
H H14B 0.5968 0.5743 0.5558 0.098 Uiso calc 1 . .
H H14C 0.7393 0.4911 0.5211 0.098 Uiso calc 1 . .
C C15 0.8003(6) 0.1832(5) 0.35511(11) 0.0488(10) Uani d 1 . .
H H15A 0.8877 0.2019 0.3792 0.059 Uiso calc 1 . .
H H15B 0.7171 0.0720 0.3608 0.059 Uiso calc 1 . .
C C16 0.9745(5) -0.0230(6) 0.30723(13) 0.0550(10) Uani d 1 . .
C C17 1.1017(6) -0.0305(7) 0.26893(12) 0.0660(12) Uani d 1 . .
H H17A 1.2179 0.0462 0.2735 0.099 Uiso calc 1 . .
H H17B 1.0301 0.0192 0.2450 0.099 Uiso calc 1 . .
H H17C 1.1394 -0.1619 0.2635 0.099 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 0.106(2) 0.074(2) 0.0437(16) 0.017(2) 0.0283(16) -0.0019(15)
O2 0.0592(16) 0.0591(17) 0.0427(15) 0.0035(15) 0.0182(13) -0.0021(13)
O3 0.076(2) 0.0422(16) 0.0520(16) 0.0031(15) 0.0267(16) -0.0038(13)
O4 0.137(4) 0.058(2) 0.184(4) 0.013(2) 0.101(3) 0.014(3)
C1 0.080(3) 0.040(2) 0.040(2) 0.013(2) 0.014(2) -0.001(2)
C2 0.069(3) 0.036(2) 0.039(2) 0.002(2) 0.0037(19) -0.0026(18)
C3 0.054(2) 0.0344(19) 0.0366(19) 0.000(2) 0.0037(17) -0.0007(17)
C4 0.049(2) 0.043(2) 0.040(2) 0.000(2) 0.0113(18) -0.0030(19)
C5 0.038(2) 0.052(2) 0.044(2) -0.003(2) 0.0027(17) -0.0035(19)
C6 0.0395(19) 0.045(2) 0.0324(18) -0.0053(18) 0.0005(16) -0.0023(16)
C7 0.042(2) 0.040(2) 0.0340(19) -0.0054(18) 0.0046(17) -0.0033(15)
C8 0.044(2) 0.047(2) 0.0366(18) -0.003(2) -0.0007(16) -0.0045(17)
C9 0.045(2) 0.041(2) 0.039(2) -0.0055(18) 0.0052(18) -0.0040(16)
C10 0.054(2) 0.058(3) 0.039(2) -0.005(2) 0.005(2) -0.0120(19)
C11 0.044(2) 0.068(3) 0.040(2) -0.011(2) 0.0019(18) -0.0067(18)
C12 0.061(2) 0.091(3) 0.0322(19) -0.002(3) -0.0002(18) 0.002(2)
C13 0.057(3) 0.048(2) 0.052(2) -0.006(2) 0.000(2) 0.0053(18)
C14 0.093(3) 0.058(3) 0.044(2) 0.004(3) -0.006(2) -0.003(2)
C15 0.062(2) 0.046(2) 0.039(2) -0.001(2) 0.015(2) -0.0029(18)
C16 0.047(2) 0.048(3) 0.070(3) -0.006(2) 0.013(2) -0.007(2)
C17 0.063(3) 0.071(3) 0.064(3) 0.006(3) 0.014(2) -0.017(2)
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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
C1 O2 C4 . . 106.7(3) ?
C16 O3 C15 . . 119.3(3) ?
O1 C1 O2 . . 120.4(4) ?
O1 C1 C2 . . 130.5(4) ?
O2 C1 C2 . . 109.0(3) ?
C3 C2 C1 . . 107.4(3) ?
C3 C2 C14 . . 130.2(4) ?
C1 C2 C14 . . 122.4(3) ?
C2 C3 C4 . . 108.1(3) ?
C2 C3 C8 . . 132.3(3) ?
C4 C3 C8 . . 119.6(3) ?
C5 C4 O2 . . 124.5(3) ?
C5 C4 C3 . . 126.6(3) ?
O2 C4 C3 . . 108.8(3) ?
C4 C5 C6 . . 116.5(3) ?
C4 C5 H5 . . 121.8 ?
C6 C5 H5 . . 121.8 ?
C5 C6 C13 . . 107.0(3) ?
C5 C6 C11 . . 115.2(3) ?
C13 C6 C11 . . 112.5(3) ?
C5 C6 C7 . . 108.0(3) ?
C13 C6 C7 . . 113.1(3) ?
C11 C6 C7 . . 101.0(3) ?
C8 C7 C9 . . 122.4(3) ?
C8 C7 C6 . . 112.7(3) ?
C9 C7 C6 . . 104.9(3) ?
C8 C7 H7 . . 105.2 ?
C9 C7 H7 . . 105.2 ?
C6 C7 H7 . . 105.2 ?
C3 C8 C7 . . 106.3(3) ?
C3 C8 H8A . . 110.5 ?
C7 C8 H8A . . 110.5 ?
C3 C8 H8B . . 110.5 ?
C7 C8 H8B . . 110.5 ?
H8A C8 H8B . . 108.7 ?
C15 C9 C10 . . 112.9(3) ?
C15 C9 C7 . . 111.8(3) ?
C10 C9 C7 . . 101.2(3) ?
C15 C9 H9 . . 110.2 ?
C10 C9 H9 . . 110.2 ?
C7 C9 H9 . . 110.2 ?
C12 C10 C11 . . 59.7(3) ?
C12 C10 C9 . . 120.2(4) ?
C11 C10 C9 . . 107.7(3) ?
C12 C10 H10 . . 118.1 ?
C11 C10 H10 . . 118.1 ?
C9 C10 H10 . . 118.1 ?
C12 C11 C10 . . 59.2(3) ?
C12 C11 C6 . . 120.1(3) ?
C10 C11 C6 . . 107.5(3) ?
C12 C11 H11 . . 118.2 ?
C10 C11 H11 . . 118.2 ?
C6 C11 H11 . . 118.2 ?
C10 C12 C11 . . 61.1(3) ?
C10 C12 H12A . . 117.7 ?
C11 C12 H12A . . 117.7 ?
C10 C12 H12B . . 117.7 ?
C11 C12 H12B . . 117.7 ?
H12A C12 H12B . . 114.8 ?
C6 C13 H13A . . 109.5 ?
C6 C13 H13B . . 109.5 ?
H13A C13 H13B . . 109.5 ?
C6 C13 H13C . . 109.5 ?
H13A C13 H13C . . 109.5 ?
H13B C13 H13C . . 109.5 ?
C2 C14 H14A . . 109.5 ?
C2 C14 H14B . . 109.5 ?
H14A C14 H14B . . 109.5 ?
C2 C14 H14C . . 109.5 ?
H14A C14 H14C . . 109.5 ?
H14B C14 H14C . . 109.5 ?
O3 C15 C9 . . 107.7(3) ?
O3 C15 H15A . . 110.2 ?
C9 C15 H15A . . 110.2 ?
O3 C15 H15B . . 110.2 ?
C9 C15 H15B . . 110.2 ?
H15A C15 H15B . . 108.5 ?
O4 C16 O3 . . 122.2(4) ?
O4 C16 C17 . . 124.5(4) ?
O3 C16 C17 . . 113.3(4) ?
C16 C17 H17A . . 109.5 ?
C16 C17 H17B . . 109.5 ?
H17A C17 H17B . . 109.5 ?
C16 C17 H17C . . 109.5 ?
H17A C17 H17C . . 109.5 ?
H17B C17 H17C . . 109.5 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
O1 C1 . 1.202(4) ?
O2 C1 . 1.388(4) ?
O2 C4 . 1.396(4) ?
O3 C16 . 1.311(5) ?
O3 C15 . 1.453(4) ?
O4 C16 . 1.196(5) ?
C1 C2 . 1.467(6) ?
C2 C3 . 1.343(4) ?
C2 C14 . 1.486(5) ?
C3 C4 . 1.458(5) ?
C3 C8 . 1.497(5) ?
C4 C5 . 1.319(5) ?
C5 C6 . 1.509(5) ?
C5 H5 . 0.9300 ?
C6 C13 . 1.531(5) ?
C6 C11 . 1.534(5) ?
C6 C7 . 1.548(5) ?
C7 C8 . 1.528(4) ?
C7 C9 . 1.538(5) ?
C7 H7 . 0.9800 ?
C8 H8A . 0.9700 ?
C8 H8B . 0.9700 ?
C9 C15 . 1.507(5) ?
C9 C10 . 1.530(5) ?
C9 H9 . 0.9800 ?
C10 C12 . 1.492(6) ?
C10 C11 . 1.520(5) ?
C10 H10 . 0.9800 ?
C11 C12 . 1.500(5) ?
C11 H11 . 0.9800 ?
C12 H12A . 0.9700 ?
C12 H12B . 0.9700 ?
C13 H13A . 0.9600 ?
C13 H13B . 0.9600 ?
C13 H13C . 0.9600 ?
C14 H14A . 0.9600 ?
C14 H14B . 0.9600 ?
C14 H14C . 0.9600 ?
C15 H15A . 0.9700 ?
C15 H15B . 0.9700 ?
C16 C17 . 1.481(5) ?
C17 H17A . 0.9600 ?
C17 H17B . 0.9600 ?
C17 H17C . 0.9600 ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
C8 H8A O1 4_556 0.97 2.81 3.481(5) 126.6
C11 H11 O3 1_455 0.98 2.54 3.497(5) 167.0
C13 H13C O1 4_566 0.96 2.60 3.499(5) 156.5
C13 H13B O4 1_565 0.96 2.61 3.530(6) 159.6
C14 H14A O2 4_556 0.96 2.76 3.530(5) 138.0
C17 H17C O3 3_745 0.96 2.86 3.478(5) 123.5
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
C4 O2 C1 O1 . . . . -178.9(4) ?
C4 O2 C1 C2 . . . . 0.5(4) ?
O1 C1 C2 C3 . . . . 178.5(4) ?
O2 C1 C2 C3 . . . . -0.8(5) ?
O1 C1 C2 C14 . . . . -0.9(7) ?
O2 C1 C2 C14 . . . . 179.8(3) ?
C1 C2 C3 C4 . . . . 0.7(5) ?
C14 C2 C3 C4 . . . . -179.9(4) ?
C1 C2 C3 C8 . . . . -176.5(4) ?
C14 C2 C3 C8 . . . . 2.9(7) ?
C1 O2 C4 C5 . . . . -177.6(4) ?
C1 O2 C4 C3 . . . . 0.0(4) ?
C2 C3 C4 C5 . . . . 177.1(4) ?
C8 C3 C4 C5 . . . . -5.3(6) ?
C2 C3 C4 O2 . . . . -0.4(4) ?
C8 C3 C4 O2 . . . . 177.2(3) ?
O2 C4 C5 C6 . . . . 175.6(3) ?
C3 C4 C5 C6 . . . . -1.5(6) ?
C4 C5 C6 C13 . . . . -88.5(4) ?
C4 C5 C6 C11 . . . . 145.6(4) ?
C4 C5 C6 C7 . . . . 33.5(4) ?
C5 C6 C7 C8 . . . . -62.8(4) ?
C13 C6 C7 C8 . . . . 55.4(4) ?
C11 C6 C7 C8 . . . . 175.8(3) ?
C5 C6 C7 C9 . . . . 161.8(3) ?
C13 C6 C7 C9 . . . . -80.0(3) ?
C11 C6 C7 C9 . . . . 40.5(3) ?
C2 C3 C8 C7 . . . . 155.5(4) ?
C4 C3 C8 C7 . . . . -21.5(5) ?
C9 C7 C8 C3 . . . . -178.6(3) ?
C6 C7 C8 C3 . . . . 55.0(4) ?
C8 C7 C9 C15 . . . . 69.2(4) ?
C6 C7 C9 C15 . . . . -161.0(3) ?
C8 C7 C9 C10 . . . . -170.4(3) ?
C6 C7 C9 C10 . . . . -40.5(3) ?
C15 C9 C10 C12 . . . . -151.0(3) ?
C7 C9 C10 C12 . . . . 89.3(4) ?
C15 C9 C10 C11 . . . . 144.3(3) ?
C7 C9 C10 C11 . . . . 24.6(4) ?
C9 C10 C11 C12 . . . . 115.2(4) ?
C12 C10 C11 C6 . . . . -115.2(4) ?
C9 C10 C11 C6 . . . . 0.0(4) ?
C5 C6 C11 C12 . . . . 155.4(4) ?
C13 C6 C11 C12 . . . . 32.3(5) ?
C7 C6 C11 C12 . . . . -88.5(4) ?
C5 C6 C11 C10 . . . . -140.6(3) ?
C13 C6 C11 C10 . . . . 96.4(4) ?
C7 C6 C11 C10 . . . . -24.5(4) ?
C9 C10 C12 C11 . . . . -93.8(4) ?
C6 C11 C12 C10 . . . . 93.4(4) ?
C16 O3 C15 C9 . . . . -153.7(3) ?
C10 C9 C15 O3 . . . . 66.5(4) ?
C7 C9 C15 O3 . . . . 179.9(3) ?
C15 O3 C16 O4 . . . . 2.8(6) ?
C15 O3 C16 C17 . . . . -175.9(3) ?
_cod_database_fobs_code 2244099