#------------------------------------------------------------------------------
#$Date: 2024-10-29 04:44:29 +0200 (Tue, 29 Oct 2024) $
#$Revision: 295658 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/31/26/2312667.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_2312667
loop_
_publ_author_name
'Zhang, Qing'
'Wang, Zi Quan'
'Xing, Dian Xiang'
'Wang, Shou Juan'
'Tan, Xue Jie'
_publ_section_title
;
Synthesis, crystal structures and antiproliferative activities of a new
indole-containing dipyridylmethanone hydrazone Schiff base and its
cadmium(II) complex.
;
_journal_coeditor_code OJ3023
_journal_issue 11
_journal_name_full
'Acta crystallographica. Section C, Structural chemistry'
_journal_paper_doi 10.1107/S2053229624010167
_journal_volume 80
_journal_year 2024
_chemical_formula_iupac '[Cd Cl2 (C20 H15 N5)]'
_chemical_formula_moiety 'C20 H15 Cd Cl2 N5'
_chemical_formula_sum 'C20 H15 Cd Cl2 N5'
_chemical_formula_weight 508.67
_chemical_name_systematic
Poly[[2-({[bis(pyridin-2-yl)methylidene]hydrazin-1-ylidene}methyl)-1H-indole]di-\m-chlorido-cadmium(II)]
_space_group_crystal_system trigonal
_space_group_IT_number 167
_space_group_name_Hall '-R 3 2"c'
_space_group_name_H-M_alt 'R -3 c :H'
_atom_sites_solution_hydrogens geom
_audit_creation_method SHELXL-2018/3
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 120
_cell_formula_units_Z 36
_cell_length_a 34.6379(7)
_cell_length_b 34.6379(7)
_cell_length_c 18.4784(3)
_cell_measurement_reflns_used 6284
_cell_measurement_temperature 293(2)
_cell_measurement_theta_max 70.9720
_cell_measurement_theta_min 9.5140
_cell_volume 19199.9(6)
_computing_cell_refinement
;
SMART (Bruker, 2000)
;
_computing_data_collection
;
SMART (Bruker, 2000)
;
_computing_data_reduction
;
SAINT (Bruker, 2000)
;
_computing_molecular_graphics
;
OLEX2 (Dolomanov et al., 2009),
DIAMOND (Brandenburg & Putz, 1999) and
ORTEP-3 for Windows (Farrugia, 2012)
;
_computing_publication_material
;
OLEX2 (Dolomanov et al., 2009)
;
_computing_structure_refinement
;
SHELXL2016 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT2016 (Sheldrick, 2015a)
;
_diffrn_ambient_temperature 293(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type 'Bruker SMART CCD area detector'
_diffrn_measurement_method 'phi and omega scans'
_diffrn_radiation_type CuK\a
_diffrn_radiation_wavelength 1.54184
_diffrn_reflns_av_R_equivalents 0.0200
_diffrn_reflns_av_unetI/netI 0.0188
_diffrn_reflns_limit_h_max 42
_diffrn_reflns_limit_h_min -36
_diffrn_reflns_limit_k_max 41
_diffrn_reflns_limit_k_min -37
_diffrn_reflns_limit_l_max 22
_diffrn_reflns_limit_l_min -20
_diffrn_reflns_number 13934
_diffrn_reflns_theta_full 67.684
_diffrn_reflns_theta_max 70.925
_diffrn_reflns_theta_min 4.422
_diffrn_source 'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu 10.622
_exptl_absorpt_correction_T_max 0.727
_exptl_absorpt_correction_T_min 0.487
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2000)
;
_exptl_crystal_colour 'clear light yellow'
_exptl_crystal_density_diffrn 1.584
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description needle
_exptl_crystal_F_000 9072
_exptl_crystal_size_max 0.210
_exptl_crystal_size_mid 0.060
_exptl_crystal_size_min 0.030
_refine_diff_density_max 0.378
_refine_diff_density_min -0.308
_refine_ls_extinction_coef 0.0000025(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method
;
SHELXL2016 (Sheldrick, 2015b)
;
_refine_ls_goodness_of_fit_ref 1.090
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 254
_refine_ls_number_reflns 4079
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.090
_refine_ls_R_factor_all 0.0269
_refine_ls_R_factor_gt 0.0219
_refine_ls_shift/su_max 0.003
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0235P)^2^+26.2978P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0527
_refine_ls_wR_factor_ref 0.0569
_reflns_number_gt 3651
_reflns_number_total 4079
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file oj3023sup1.cif
_cod_data_source_block pCd2
_cod_original_cell_volume 19199.9(8)
_cod_database_code 2312667
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_hkl_file
;
0 0 3 29.2359 15.7011 6
0 0 6 999999. 9211.53 3
0 0 6 994971. 9203.69 2
0 0 9 3.15325 21.6000 2
0 0 9-3.95119 21.3429 3
0 0 12 121133. 1423.32 2
0 0 15-16.4755 41.6346 7
0 0 15 16.9743 31.3537 8
0 0 18 11757.3 368.972 7
-1 0 20 56.5347 43.2253 7
0 1 20 50.7832 45.5310 7
-1 0 17 1.41167 29.1667 8
0 1 17-22.0269 47.5174 7
1 -1 17-0.96673 40.1117 7
-1 0 17 28.2938 38.1249 7
1 -1 17-6.38265 26.7562 8
0 1 17 27.7821 29.1612 8
0 1 14 1100.19 97.5424 2
-1 0 14 887.941 88.1541 2
0 1 11-10.5948 31.0015 2
1 -1 11 3.97889 25.7762 3
-1 0 11-6.65878 27.7499 2
1 -1 11 56.1166 33.5421 2
-1 0 8 1024.80 66.4624 3
-1 0 8 960.887 85.5380 6
0 1 8 961.233 65.3522 3
-1 0 8 1009.90 64.8454 2
1 -1 8 954.678 64.6170 3
0 1 8 991.192 64.2475 2
1 -1 8 999.360 64.3773 2
1 -1 5 50.8368 22.6347 6
0 1 5 41.5960 26.8115 6
-1 0 5 41.7633 21.8129 6
-1 1 -2 14910.2 192.882 6
1 -1 2 14940.7 193.146 6
0 1 2 14886.2 210.722 6
-1 0 -4 31898.9 428.348 6
-1 1 4 32530.8 442.877 6
1 0 4 31882.9 427.874 6
0 -1 4 31602.3 421.947 6
1 0 7 31.9764 18.6085 2
0 1 -7 67.3954 24.1827 5
-1 1 7-2.05792 18.2828 3
0 -1 7 4.07074 22.1044 3
1 0 7 32.4479 20.9134 3
0 -1 7 3.65240 16.0405 2
-1 1 7 21.8900 23.2465 6
0 -1 10 3253.61 132.522 2
0 -1 10 3222.15 133.120 3
1 0 10 3213.00 135.271 3
-1 1 10 2986.06 128.622 2
1 0 10 3380.80 133.997 2
1 0 13 25.4330 32.0681 2
0 -1 13-0.07538 34.1335 2
-1 1 13 51.5434 39.0363 2
1 0 16 752.679 84.5434 8
1 0 16 794.589 92.5180 7
-1 1 16 667.996 83.9126 7
-1 1 16 635.010 75.4522 8
0 -1 16 701.053 90.9044 7
0 -1 16 676.290 81.4092 8
0 -1 19 31.1081 47.9698 7
-1 1 19-2.50371 38.6659 7
1 0 19 54.3123 46.7481 7
1 -2 3 7510.15 136.742 6
-2 1 -3 7722.95 148.853 6
1 1 -3 7633.06 146.634 5
-1 2 3 7825.52 161.517 6
2 -1 -6 71009.0 881.482 5
1 -2 6 71155.7 776.502 2
-1 2 6 72733.3 902.111 6
1 -2 6 71760.2 785.184 3
1 1 6 70763.3 784.992 3
1 1 -6 71503.3 862.803 5
2 -1 6 69909.1 777.346 2
-2 1 6 71159.5 898.410 6
-1 -1 6 69019.6 875.238 6
-1 2 6 70681.5 782.291 3
1 -2 6 68965.4 850.234 6
-1 -1 6 70301.8 777.507 3
-1 -1 6 71195.8 776.748 2
-2 1 6 69426.9 777.546 3
1 1 6 69890.3 774.056 2
2 -1 6 70715.0 789.444 3
1 1 9 1268.48 79.9725 3
-1 2 9 1350.34 80.9100 2
-1 -1 9 1338.86 79.8690 3
1 1 9 1265.27 77.7460 2
2 -1 9 1230.36 79.0208 3
1 -2 9 1168.25 74.1817 2
2 -1 9 1482.12 83.2530 2
-2 1 9 1319.17 79.5181 2
1 -2 9 1266.31 78.5948 3
-1 -1 9 1362.48 80.0223 2
-1 -1 12 17326.3 372.600 2
-1 2 12 16785.1 369.562 2
2 -1 12 16824.4 366.595 2
2 -1 12 17211.3 378.853 3
1 1 12 17031.7 369.360 2
-2 1 12 17015.7 372.023 2
1 -2 12 17310.1 370.508 2
-1 2 15 6.28976 25.8800 8
-1 2 15-38.3253 40.8091 2
1 -2 15 45.5344 32.8320 7
-1 2 15 31.4753 32.5035 7
2 -1 15-22.3789 39.5711 7
-2 1 15 15.1118 29.7570 7
-2 1 15 2.86654 33.0929 2
1 -2 15 37.6156 35.8003 8
1 1 15-10.3593 28.6516 8
-1 -1 15 18.9579 25.5100 8
2 -1 15-30.2957 29.8539 8
-2 1 15 4.86411 23.8784 8
1 1 15-2.82370 44.5227 7
-1 -1 15 1.49488 37.1896 7
1 1 18 633.966 77.7649 8
-1 -1 18 676.569 90.8456 7
2 -1 18 651.348 91.7730 7
-1 2 18 513.645 80.8796 7
-1 2 18 465.065 67.6328 8
1 1 18 521.903 84.0343 7
-2 1 18 549.449 85.7012 7
1 -2 18 590.826 84.0002 7
-2 0 19 25.3171 43.1245 7
0 2 19 64.9174 50.9124 7
2 -2 19 29.6903 50.0155 7
2 -2 16 1853.13 140.493 7
0 2 16 1832.20 140.884 7
-2 0 16 1959.93 131.161 8
0 2 16 1851.57 129.824 8
2 -2 16 1951.77 136.053 8
-2 0 16 1687.87 133.475 7
0 2 13 27.1563 37.7657 2
-2 0 13 37.8831 35.6439 2
2 -2 10 22617.8 402.997 3
-2 0 10 22242.4 395.248 2
2 -2 10 22553.1 396.703 2
0 2 10 22933.7 399.557 2
-2 0 7-1.84402 23.1072 3
-2 0 7 61.2790 26.3653 6
0 2 7 19.2265 18.5689 3
2 0 -7 104.577 28.6438 5
2 -2 7 57.6084 22.7239 3
0 2 7-17.5702 23.5078 2
2 0 -4 118541. 1258.81 5
0 2 4 121187. 1276.15 6
-2 0 1 12.9881 8.35945 5
0 2 -2 29602.0 331.180 5
0 -2 5 22.9039 12.3911 3
-2 2 5 104.281 27.4983 6
0 -2 5 46.7291 21.7327 6
0 2 -5 22.5380 15.3123 5
0 -2 5 23.9430 15.5492 2
-2 0 -5 108.082 28.0192 6
0 -2 8 319.347 48.0935 6
0 2 -8 267.719 41.8145 5
2 0 8 232.672 38.7294 3
0 -2 8 328.473 39.2317 2
0 -2 8 276.344 37.1182 3
2 0 8 287.868 37.7113 2
-2 2 11 28.2776 28.4000 2
2 0 11 16.8107 26.1493 2
0 -2 11-27.2450 33.0671 2
2 0 11 37.3789 30.5869 3
-2 2 14 5670.73 222.860 2
0 -2 17 32.4310 40.7880 7
2 0 17-3.05798 31.9464 8
-2 2 17 8.65310 25.4521 8
-2 2 17-51.9429 45.1942 7
2 0 17-1.39187 39.4227 7
-2 2 20 329.581 64.8143 7
1 2 20 1178.48 108.871 7
-2 -1 20 1136.71 105.119 7
-3 1 20 1088.60 103.966 7
-1 3 20 1154.99 107.163 7
1 2 17 6312.63 245.523 8
2 -3 17 6658.18 272.995 7
-1 3 17 6531.89 246.830 8
-2 -1 17 6779.50 272.022 7
1 2 17 6270.91 264.632 7
-1 3 17 6384.31 270.057 7
-3 1 17 6363.26 267.200 7
3 -2 17 6755.07 256.346 8
3 -2 17 6292.11 266.321 7
1 2 14 9332.70 289.707 2
-1 3 14 9508.86 293.130 2
-2 -1 14 9489.70 292.927 2
-3 1 14 9458.87 294.438 2
2 -3 11 23773.8 437.078 3
-3 1 11 23875.5 434.602 2
2 -3 11 24322.0 433.295 2
-2 -1 11 24050.1 435.741 2
-1 3 11 23621.4 431.870 2
3 -2 11 22923.6 437.387 3
3 -2 11 23942.7 431.956 2
1 2 11 24144.0 431.966 2
-2 -1 8 14633.3 354.080 6
3 -2 8 13956.2 274.191 3
3 -2 8 13715.8 263.372 2
-2 3 -8 14696.9 319.860 5
-1 3 8 14085.8 265.024 2
2 1 -8 14733.9 340.865 5
-2 -1 8 14100.9 263.977 3
-2 -1 8 14382.6 266.194 2
2 -3 8 14232.3 270.322 3
1 2 8 14118.7 271.313 3
2 -3 8 14323.7 265.016 2
1 2 8 14185.7 264.890 2
-3 2 -5 101140. 1084.16 6
-1 -2 -5 101312. 1137.03 6
-3 1 5 98372.8 1131.06 6
1 2 5 98227.2 1019.69 2
2 -3 5 101837. 1032.67 3
-2 -1 5 100140. 1019.32 3
2 1 -5 98709.6 1099.52 5
-1 3 5 100243. 1137.71 6
3 -1 -5 97983.3 1118.25 5
2 -3 5 96122.4 1063.48 6
-3 1 2 33757.9 408.847 5
-1 3 2 32773.1 403.813 6
-2 -1 2 32628.8 394.481 5
-3 2 1 127173. 1243.36 5
-2 3 1 125611. 1233.56 6
-2 -1 -4 128871. 1368.35 6
-3 1 -4 130252. 1344.06 6
-3 2 4 129653. 1376.70 6
-1 3 -4 130000. 1299.90 5
1 2 -4 129211. 1328.07 5
-2 3 4 129021. 1377.81 6
1 -3 4 127947. 1309.18 6
-2 3 7 243481. 2511.31 6
-1 -2 7 236131. 2319.35 3
1 -3 7 237021. 2326.20 3
1 -3 7 232687. 2317.27 2
-3 2 7 243273. 2513.73 6
-1 -2 7 233060. 2316.95 2
3 -2 -7 240620. 2486.43 5
2 1 7 230296. 2331.33 3
-1 3 -7 233598. 2403.41 5
1 -3 7 235409. 2418.90 6
-1 -2 7 235143. 2451.99 6
3 -1 7 237274. 2318.97 2
-1 -2 7 236678. 2266.55 1
1 2 -7 239306. 2427.11 5
2 1 7 232211. 2316.44 2
1 -3 7 228225. 2259.29 1
3 -1 7 234816. 2335.96 3
2 1 10 17522.0 349.652 3
1 -3 10 17937.5 343.828 3
2 1 10 17614.4 339.631 2
1 -3 10 17803.5 339.202 2
-2 3 10 17584.9 342.044 2
-3 2 10 17544.0 343.136 2
3 -1 10 17170.7 346.866 3
-1 -2 10 17732.2 340.973 2
3 -1 10 17535.8 338.573 2
2 1 13 49386.6 753.954 2
-1 -2 13 49622.8 755.696 2
-3 2 13 49544.2 763.181 2
-2 3 13 49907.1 761.921 2
-2 3 16 5436.03 233.678 2
-2 3 16 5478.62 221.771 8
1 -3 16 5381.76 241.189 7
-3 2 16 5331.40 215.105 8
2 1 16 4935.82 232.978 7
2 1 16 5483.08 228.026 8
-2 3 16 5035.70 236.058 7
3 -1 16 5507.28 245.299 7
-1 -2 16 5250.73 237.307 7
-3 2 16 5329.43 241.769 7
3 -1 16 5338.96 225.753 8
-3 2 16 5501.87 235.740 2
-2 3 19 5699.11 245.657 7
-3 2 19 5716.80 245.584 7
1 -3 19 5757.34 246.790 7
-1 -2 19 5440.78 238.613 7
2 1 19 5520.91 237.879 7
3 -1 19 5406.39 237.514 7
0 3 18 443.864 68.8306 8
-3 0 18 368.052 69.3238 7
0 3 18 378.274 73.0970 7
3 -3 18 371.446 66.6148 7
0 3 15-20.0241 44.1416 7
-3 0 15 7.81132 27.2060 8
0 3 15-3.30338 35.9706 8
-3 0 15-87.9487 51.8840 7
0 3 15-30.1505 40.6084 2
-3 0 15-52.3719 46.5748 2
3 -3 15-37.0729 44.0058 7
3 -3 15 0.44736 28.0420 8
-3 0 12 5625.75 203.225 2
0 3 12 5790.59 203.342 2
3 -3 12 5539.64 202.877 3
3 -3 9 17.0231 21.5553 2
-3 0 9-4.97084 23.5434 2
0 3 9 1.70563 21.7795 2
0 3 9 5.03541 22.1586 3
3 -3 9-5.61309 26.3908 3
3 -3 6 25037.4 312.026 1
3 -3 6 25734.2 364.246 3
0 3 6 26308.5 359.191 3
3 -3 6 26436.8 355.779 2
3 0 -6 25843.8 433.103 5
-3 0 6 25992.1 444.412 6
3 0 -3 5.44721 17.3295 5
-3 0 3 2.93708 18.3511 5
-3 3 0 42493.7 439.033 5
-3 3 3 52.9603 19.2183 6
0 3 -3 32.0539 14.2556 5
-3 3 6 93599.0 1128.02 6
0 -3 6 92638.7 946.624 1
0 -3 6 92386.7 978.423 3
3 0 6 91261.4 990.601 3
-3 0 -6 91535.7 1089.71 6
0 -3 6 91903.6 974.050 2
0 3 -6 90588.0 1037.50 5
3 0 6 92099.3 974.646 2
0 -3 6 91477.6 1056.91 6
3 0 9 38.9341 24.0829 2
0 -3 9-10.2938 21.1373 3
3 0 9 24.5743 27.0777 3
0 -3 9 9.13452 20.1589 2
-3 3 12 6985.41 229.038 2
3 0 12 7110.64 226.770 2
0 -3 12 7490.91 232.096 2
3 0 12 7049.66 233.148 3
0 -3 15 6.64327 28.4361 8
-3 3 15-66.3610 46.4318 2
-3 3 15-6.99538 23.8854 8
-3 3 15-30.1808 41.3093 7
3 0 15-5.80948 33.6044 7
0 -3 15-44.6882 43.3347 7
3 0 15-24.1411 36.1934 8
3 0 18 1967.36 136.261 8
-3 3 18 2161.98 133.608 8
3 0 18 2016.67 149.357 7
-3 3 18 1938.10 146.246 7
0 -3 18 2167.69 152.420 7
-3 3 21-11.2385 38.0562 7
2 -4 0 10742.6 139.980 6
-2 4 3 8173.89 177.134 6
2 -4 3 7873.47 123.677 6
-2 -2 3 7856.53 160.026 5
-2 4 -3 7913.58 121.971 5
4 -2 -6 17208.3 345.730 5
2 -4 6 16621.1 260.574 2
2 2 6 16048.5 266.558 3
-4 2 -6 17369.8 318.638 6
-2 -2 -6 16899.0 347.506 6
-2 -2 6 15729.2 320.818 6
2 -4 6 16533.9 265.712 3
2 2 -6 16853.4 317.119 5
2 -4 6 16789.0 294.377 6
4 -2 6 16644.4 262.130 2
2 2 6 16680.4 258.191 2
2 -4 6 16286.2 236.881 1
-4 2 6 16555.2 350.414 6
4 -2 6 17066.5 273.930 3
-2 4 -6 16792.9 288.277 5
-2 -2 6 16686.1 256.100 3
-2 4 6 16816.8 352.216 6
2 -4 9 1175.77 75.7369 3
2 2 9 1032.19 69.6594 2
4 -2 9 1021.10 73.1520 3
-2 -2 9 1078.05 72.4975 2
4 -2 9 1073.28 71.9864 2
2 2 9 1040.15 73.7687 3
2 -4 9 1086.92 71.5337 2
-4 2 12 351.684 49.8634 2
2 -4 12 527.867 65.3643 3
2 2 12 439.896 58.4800 2
4 -2 12 467.170 63.5764 3
-2 -2 12 544.258 66.9920 2
-2 4 12 317.281 51.4792 2
-2 4 15 703.013 88.1633 7
-4 2 15 680.858 80.2282 2
-2 4 15 710.075 81.2330 8
-4 2 15 562.277 69.4839 8
2 2 15 581.965 77.3828 7
4 -2 15 673.741 79.5846 8
4 -2 15 623.858 82.4698 7
-2 -2 15 483.443 69.6036 7
-4 2 15 626.524 81.6824 7
2 -4 15 705.286 85.9024 7
2 2 15 531.237 70.8576 8
2 -4 15 799.167 87.1764 8
-2 4 15 664.670 81.6621 2
-2 -2 15 613.461 71.5127 8
-4 2 18-9.58448 37.5375 7
2 -4 18 31.5776 39.5824 7
4 -2 18 27.2947 40.0231 7
-2 4 18 41.2976 37.5463 7
2 2 18 1.45711 28.5824 8
-2 4 18 15.5008 26.1179 8
2 2 18 67.2646 48.9913 7
-2 -2 18-4.30330 36.8104 7
-2 4 21 66.0569 40.5997 7
-3 -1 19 3388.90 183.354 7
1 3 19 3295.63 184.207 7
-1 4 19 3125.57 159.132 8
1 3 19 3142.31 167.002 8
-1 4 19 3175.64 182.928 7
-4 1 19 3172.02 180.298 7
-1 4 16 19.4764 43.6659 7
-3 -1 16 31.5221 35.2426 7
-4 1 16 3.97441 34.6911 2
4 -3 16 72.5852 49.8924 7
1 3 16 30.7233 32.6486 8
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0 0 0 0.00 0.00 0
TITL exp_3431 in R-3c
REM R-3c (#167 in standard setting)
CELL 1.54184 34.637914 34.637914 18.478436 90.0000 90.0000 120.0000
ZERR 267.00 0.000697 0.000697 0.000332 0.0000 0.0000 0.0000
LATT 3
SYMM -y, x-y, z
SYMM -x+y,-x, z
SYMM y, x,-z+1/2
SYMM x-y,-y,-z+1/2
SYMM -x,-x+y,-z+1/2
SFAC C H N O Cd
UNIT 267.00 267.00 267.00 267.00 267.00
TREF
HKLF 4
END
;
_shelx_hkl_checksum 76518
_shelx_res_file
;
TITL shelxt_a.res in R-3c
shelx.res
created by SHELXL-2018/3 at 11:27:09 on 07-Sep-2019
CELL 1.54184 34.6379 34.6379 18.4784 90.000 90.000 120.000
ZERR 36.00 0.0007 0.0007 0.0003 0.000 0.000 0.000
LATT 3
SYMM - Y, X - Y, Z
SYMM - X + Y, - X, Z
SYMM Y, X, 1/2 - Z
SYMM X - Y, - Y, 1/2 - Z
SYMM - X, - X + Y, 1/2 - Z
SFAC C H N CD CL
UNIT 720 540 180 36 72
MERG 2
FMAP 2
PLAN 1
HTAB
HTAB C12 N5
EQIV $1 y-1/3,x+1/3,-z+5/6
EQIV $2 x+1/3,x-y+2/3,z+1/6
EQIV $3 x-y+1/3,-y+2/3,-z+7/6
EQIV $4 -y+2/3,-x+1/3,z-1/6
HTAB C9 Cl2_$1
HTAB C20 Cl1_$2
HTAB N1 N5_$3
HTAB C18 Cl2_$4
ACTA
BOND
LIST 6
L.S. 40
WGHT 0.023500 26.297800
EXTI 0.000003
FVAR 0.33149
C1 1 0.093997 0.244721 0.429119 11.00000 0.04425 0.03892 =
0.05669 -0.00447 -0.00978 0.02345
C2 1 0.065044 0.217217 0.377524 11.00000 0.05716 0.04828 =
0.05992 -0.00726 -0.01758 0.03037
AFIX 43
H2 2 0.052534 0.225515 0.340423 11.00000 -1.20000
AFIX 0
C3 1 0.057591 0.173790 0.390910 11.00000 0.04684 0.04517 =
0.05459 -0.00795 -0.00673 0.02373
C4 1 0.031652 0.131848 0.357961 11.00000 0.05473 0.05207 =
0.07422 -0.01607 -0.01298 0.02239
AFIX 43
H4 2 0.014419 0.128848 0.317469 11.00000 -1.20000
AFIX 0
C5 1 0.032102 0.095669 0.386136 11.00000 0.05938 0.04098 =
0.09109 -0.01221 0.00484 0.01701
AFIX 43
H5 2 0.014970 0.067905 0.364584 11.00000 -1.20000
AFIX 0
C6 1 0.057775 0.099644 0.446586 11.00000 0.07104 0.04039 =
0.08858 0.00899 0.01872 0.02930
AFIX 43
H6 2 0.057510 0.074392 0.464353 11.00000 -1.20000
AFIX 0
C7 1 0.083588 0.139889 0.480921 11.00000 0.06258 0.05266 =
0.06060 0.00702 0.00568 0.03357
AFIX 43
H7 2 0.100534 0.142151 0.521426 11.00000 -1.20000
AFIX 0
C8 1 0.083348 0.176998 0.452731 11.00000 0.04482 0.04057 =
0.05091 -0.00313 0.00050 0.02362
C9 1 0.108453 0.291307 0.438338 11.00000 0.04484 0.04084 =
0.05607 -0.00265 -0.00643 0.02463
AFIX 43
H9 2 0.097544 0.304495 0.406742 11.00000 -1.20000
AFIX 0
C10 1 0.179818 0.391546 0.500379 11.00000 0.03059 0.03983 =
0.03609 -0.00219 -0.00415 0.01863
C11 1 0.183373 0.436163 0.503099 11.00000 0.03193 0.03497 =
0.03832 -0.00180 -0.00196 0.01416
C12 1 0.223944 0.475334 0.498848 11.00000 0.03576 0.04035 =
0.07521 0.00194 -0.00196 0.01352
AFIX 43
H12 2 0.250248 0.474485 0.494282 11.00000 -1.20000
AFIX 0
C13 1 0.224995 0.515650 0.501448 11.00000 0.04947 0.03561 =
0.08724 -0.00057 -0.00724 0.00984
AFIX 43
H13 2 0.252062 0.542222 0.499212 11.00000 -1.20000
AFIX 0
C14 1 0.185948 0.516262 0.507339 11.00000 0.06643 0.03607 =
0.07224 -0.00830 -0.00943 0.02578
AFIX 43
H14 2 0.185895 0.543066 0.509179 11.00000 -1.20000
AFIX 0
C15 1 0.146601 0.475962 0.510477 11.00000 0.04801 0.04248 =
0.06121 -0.01068 -0.00457 0.02673
AFIX 43
H15 2 0.119955 0.476184 0.514635 11.00000 -1.20000
AFIX 0
C16 1 0.221035 0.388486 0.509497 11.00000 0.03052 0.04120 =
0.04133 -0.00138 -0.00267 0.01991
C17 1 0.232953 0.365545 0.461754 11.00000 0.04215 0.05822 =
0.04659 -0.01207 -0.00479 0.02726
AFIX 43
H17 2 0.215069 0.350835 0.422090 11.00000 -1.20000
AFIX 0
C18 1 0.271984 0.364874 0.474074 11.00000 0.05437 0.07564 =
0.05976 -0.01452 -0.00046 0.04481
AFIX 43
H18 2 0.280967 0.349941 0.442539 11.00000 -1.20000
AFIX 0
C19 1 0.297157 0.386518 0.533360 11.00000 0.04682 0.08269 =
0.06519 -0.01369 -0.01126 0.04643
AFIX 43
H19 2 0.323451 0.386395 0.542971 11.00000 -1.20000
AFIX 0
C20 1 0.282943 0.408520 0.578649 11.00000 0.04448 0.07372 =
0.05401 -0.01612 -0.01588 0.03701
AFIX 43
H20 2 0.300185 0.422940 0.619039 11.00000 -1.20000
AFIX 0
N1 3 0.105451 0.220627 0.474583 11.00000 0.04758 0.04196 =
0.05114 -0.00791 -0.01149 0.02609
AFIX 43
H1 2 0.123466 0.231180 0.510672 11.00000 -1.20000
AFIX 0
N2 3 0.135721 0.315480 0.488196 11.00000 0.03548 0.03469 =
0.05586 -0.00108 -0.00417 0.01988
N3 3 0.140774 0.358226 0.489019 11.00000 0.03640 0.03293 =
0.04699 -0.00189 -0.00487 0.02075
N4 3 0.145067 0.436966 0.507834 11.00000 0.03510 0.03501 =
0.04475 -0.00538 -0.00308 0.01681
N5 3 0.245748 0.410239 0.567640 11.00000 0.03576 0.05441 =
0.04525 -0.00950 -0.00627 0.02701
CD1 4 0.076778 0.370145 0.499860 11.00000 0.02975 0.03423 =
0.03777 0.00158 -0.00226 0.01637
CL1 5 0.026121 0.288401 0.524847 11.00000 0.04475 0.03661 =
0.03739 -0.00202 -0.00406 0.00638
CL2 5 0.031035 0.408989 0.477147 11.00000 0.05010 0.06586 =
0.03680 0.00432 0.00167 0.04211
HKLF 4
REM shelxt_a.res in R-3c
REM wR2 = 0.0569, GooF = S = 1.090, Restrained GooF = 1.090 for all data
REM R1 = 0.0219 for 3651 Fo > 4sig(Fo) and 0.0269 for all 4079 data
REM 254 parameters refined using 0 restraints
END
WGHT 0.0235 26.2395
REM Instructions for potential hydrogen bonds
HTAB C9 Cl2_$1
HTAB C12 N5
HTAB C15 Cl2
HTAB C19 Cl1_$2
HTAB C20 Cl1_$2
HTAB N1 N5_$3
REM Highest difference peak 0.378, deepest hole -0.308, 1-sigma level 0.051
Q1 1 0.0515 0.3297 0.5086 11.00000 0.05 0.38
;
_shelx_res_checksum 7224
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'y, x, -z+1/2'
'x-y, -y, -z+1/2'
'-x, -x+y, -z+1/2'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'y+2/3, x+1/3, -z+5/6'
'x-y+2/3, -y+1/3, -z+5/6'
'-x+2/3, -x+y+1/3, -z+5/6'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'y+1/3, x+2/3, -z+7/6'
'x-y+1/3, -y+2/3, -z+7/6'
'-x+1/3, -x+y+2/3, -z+7/6'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-y, -x, z-1/2'
'-x+y, y, z-1/2'
'x, x-y, z-1/2'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-y+2/3, -x+1/3, z-1/6'
'-x+y+2/3, y+1/3, z-1/6'
'x+2/3, x-y+1/3, z-1/6'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
'-y+1/3, -x+2/3, z+1/6'
'-x+y+1/3, y+2/3, z+1/6'
'x+1/3, x-y+2/3, z+1/6'
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
C C1 0.09400(9) 0.24472(8) 0.42912(14) 0.0454(6) Uani d 1 . .
C C2 0.06504(10) 0.21722(9) 0.37752(15) 0.0533(7) Uani d 1 . .
H H2 0.052534 0.225515 0.340423 0.064 Uiso calc 1 . .
C C3 0.05759(9) 0.17379(9) 0.39091(15) 0.0485(6) Uani d 1 . .
C C4 0.03165(10) 0.13185(10) 0.35796(18) 0.0623(8) Uani d 1 . .
H H4 0.014419 0.128848 0.317469 0.075 Uiso calc 1 . .
C C5 0.03210(11) 0.09567(10) 0.38614(19) 0.0674(9) Uani d 1 . .
H H5 0.014970 0.067905 0.364584 0.081 Uiso calc 1 . .
C C6 0.05778(11) 0.09964(10) 0.44659(19) 0.0660(8) Uani d 1 . .
H H6 0.057510 0.074392 0.464353 0.079 Uiso calc 1 . .
C C7 0.08359(10) 0.13989(10) 0.48092(16) 0.0565(7) Uani d 1 . .
H H7 0.100534 0.142151 0.521426 0.068 Uiso calc 1 . .
C C8 0.08335(9) 0.17700(8) 0.45273(14) 0.0444(6) Uani d 1 . .
C C9 0.10845(9) 0.29131(8) 0.43834(14) 0.0458(6) Uani d 1 . .
H H9 0.097544 0.304495 0.406742 0.055 Uiso calc 1 . .
C C10 0.17982(7) 0.39155(8) 0.50038(12) 0.0350(5) Uani d 1 . .
C C11 0.18337(7) 0.43616(8) 0.50310(12) 0.0362(5) Uani d 1 . .
C C12 0.22394(9) 0.47533(9) 0.49885(16) 0.0529(7) Uani d 1 . .
H H12 0.250248 0.474485 0.494282 0.063 Uiso calc 1 . .
C C13 0.22500(10) 0.51565(9) 0.50145(17) 0.0625(8) Uani d 1 . .
H H13 0.252062 0.542222 0.499212 0.075 Uiso calc 1 . .
C C14 0.18595(10) 0.51626(9) 0.50734(16) 0.0582(7) Uani d 1 . .
H H14 0.185895 0.543066 0.509179 0.070 Uiso calc 1 . .
C C15 0.14660(9) 0.47596(9) 0.51048(15) 0.0487(6) Uani d 1 . .
H H15 0.119955 0.476184 0.514635 0.058 Uiso calc 1 . .
C C16 0.22104(7) 0.38849(8) 0.50950(12) 0.0368(5) Uani d 1 . .
C C17 0.23295(9) 0.36554(9) 0.46175(14) 0.0480(6) Uani d 1 . .
H H17 0.215069 0.350835 0.422090 0.058 Uiso calc 1 . .
C C18 0.27198(10) 0.36487(11) 0.47407(16) 0.0578(7) Uani d 1 . .
H H18 0.280967 0.349941 0.442539 0.069 Uiso calc 1 . .
C C19 0.29716(9) 0.38652(11) 0.53336(16) 0.0587(8) Uani d 1 . .
H H19 0.323451 0.386395 0.542971 0.070 Uiso calc 1 . .
C C20 0.28294(9) 0.40852(10) 0.57865(15) 0.0541(7) Uani d 1 . .
H H20 0.300185 0.422940 0.619039 0.065 Uiso calc 1 . .
N N1 0.10545(7) 0.22063(7) 0.47458(11) 0.0452(5) Uani d 1 . .
H H1 0.123466 0.231180 0.510672 0.054 Uiso calc 1 . .
N N2 0.13572(6) 0.31548(6) 0.48820(11) 0.0410(5) Uani d 1 . .
N N3 0.14077(6) 0.35823(6) 0.48902(10) 0.0373(4) Uani d 1 . .
N N4 0.14507(6) 0.43697(6) 0.50783(10) 0.0386(4) Uani d 1 . .
N N5 0.24575(7) 0.41024(7) 0.56764(11) 0.0432(5) Uani d 1 . .
Cd Cd1 0.07678(2) 0.37014(2) 0.49986(2) 0.03375(6) Uani d 1 . .
Cl Cl1 0.02612(2) 0.28840(2) 0.52485(3) 0.04579(15) Uani d 1 . .
Cl Cl2 0.03104(2) 0.40899(2) 0.47715(3) 0.04509(14) 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
C1 0.0442(14) 0.0389(13) 0.0567(15) 0.0234(12) -0.0098(12) -0.0045(11)
C2 0.0572(17) 0.0483(15) 0.0599(16) 0.0304(14) -0.0176(13) -0.0073(13)
C3 0.0468(15) 0.0452(14) 0.0546(15) 0.0237(12) -0.0067(12) -0.0079(12)
C4 0.0547(18) 0.0521(17) 0.0742(19) 0.0224(14) -0.0130(15) -0.0161(15)
C5 0.0594(19) 0.0410(16) 0.091(2) 0.0170(14) 0.0048(17) -0.0122(15)
C6 0.071(2) 0.0404(15) 0.089(2) 0.0293(15) 0.0187(18) 0.0090(15)
C7 0.0626(18) 0.0527(17) 0.0606(17) 0.0336(15) 0.0057(14) 0.0070(13)
C8 0.0448(14) 0.0406(13) 0.0509(14) 0.0236(12) 0.0005(11) -0.0031(11)
C9 0.0448(14) 0.0408(13) 0.0561(15) 0.0246(12) -0.0064(12) -0.0026(11)
C10 0.0306(11) 0.0398(12) 0.0361(11) 0.0186(10) -0.0042(9) -0.0022(9)
C11 0.0319(11) 0.0350(12) 0.0383(12) 0.0142(10) -0.0020(9) -0.0018(9)
C12 0.0358(13) 0.0404(14) 0.0752(18) 0.0135(11) -0.0020(12) 0.0019(13)
C13 0.0495(17) 0.0356(14) 0.087(2) 0.0098(13) -0.0072(15) -0.0006(14)
C14 0.0664(19) 0.0361(14) 0.0722(18) 0.0258(14) -0.0094(15) -0.0083(13)
C15 0.0480(15) 0.0425(14) 0.0612(16) 0.0267(12) -0.0046(12) -0.0107(12)
C16 0.0305(11) 0.0412(13) 0.0413(12) 0.0199(10) -0.0027(9) -0.0014(10)
C17 0.0422(14) 0.0582(16) 0.0466(14) 0.0273(13) -0.0048(11) -0.0121(12)
C18 0.0544(17) 0.076(2) 0.0598(17) 0.0448(16) -0.0005(14) -0.0145(15)
C19 0.0468(16) 0.083(2) 0.0652(18) 0.0464(16) -0.0113(13) -0.0137(16)
C20 0.0445(15) 0.0737(19) 0.0540(15) 0.0370(15) -0.0159(12) -0.0161(14)
N1 0.0476(12) 0.0420(11) 0.0511(12) 0.0261(10) -0.0115(10) -0.0079(9)
N2 0.0355(10) 0.0347(10) 0.0559(12) 0.0199(9) -0.0042(9) -0.0011(9)
N3 0.0364(10) 0.0329(10) 0.0470(11) 0.0207(9) -0.0049(8) -0.0019(8)
N4 0.0351(10) 0.0350(10) 0.0447(11) 0.0168(9) -0.0031(8) -0.0054(8)
N5 0.0358(11) 0.0544(13) 0.0453(11) 0.0270(10) -0.0063(9) -0.0095(9)
Cd1 0.02975(9) 0.03423(10) 0.03777(10) 0.01637(7) -0.00226(6) 0.00158(6)
Cl1 0.0447(3) 0.0366(3) 0.0374(3) 0.0064(2) -0.0041(2) -0.0020(2)
Cl2 0.0501(3) 0.0659(4) 0.0368(3) 0.0421(3) 0.0017(2) 0.0043(3)
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'
Cd Cd 0.1185 4.6533 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 '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
C2 C1 N1 . . 109.7(2) ?
C2 C1 C9 . . 125.9(2) ?
N1 C1 C9 . . 124.3(2) ?
C1 C2 C3 . . 107.4(2) ?
C4 C3 C2 . . 134.8(3) ?
C4 C3 C8 . . 118.7(3) ?
C2 C3 C8 . . 106.5(2) ?
C5 C4 C3 . . 119.2(3) ?
C4 C5 C6 . . 121.1(3) ?
C7 C6 C5 . . 121.9(3) ?
C6 C7 C8 . . 117.5(3) ?
N1 C8 C7 . . 130.6(3) ?
N1 C8 C3 . . 107.8(2) ?
C7 C8 C3 . . 121.5(3) ?
N2 C9 C1 . . 123.0(2) ?
N3 C10 C11 . . 116.3(2) ?
N3 C10 C16 . . 124.8(2) ?
C11 C10 C16 . . 119.0(2) ?
N4 C11 C12 . . 120.8(2) ?
N4 C11 C10 . . 117.0(2) ?
C12 C11 C10 . . 122.2(2) ?
C13 C12 C11 . . 119.4(3) ?
C14 C13 C12 . . 119.5(3) ?
C13 C14 C15 . . 118.1(3) ?
N4 C15 C14 . . 123.0(3) ?
N5 C16 C17 . . 122.9(2) ?
N5 C16 C10 . . 114.4(2) ?
C17 C16 C10 . . 122.7(2) ?
C16 C17 C18 . . 118.7(2) ?
C19 C18 C17 . . 118.9(2) ?
C18 C19 C20 . . 118.9(2) ?
N5 C20 C19 . . 123.5(2) ?
C8 N1 C1 . . 108.5(2) ?
C9 N2 N3 . . 111.0(2) ?
C10 N3 N2 . . 118.11(19) ?
C10 N3 Cd1 . . 118.00(15) ?
N2 N3 Cd1 . . 122.12(14) ?
C15 N4 C11 . . 119.1(2) ?
C15 N4 Cd1 . . 120.98(17) ?
C11 N4 Cd1 . . 119.64(15) ?
C20 N5 C16 . . 117.1(2) ?
N4 Cd1 N3 . . 67.76(6) ?
N4 Cd1 Cl1 . . 152.90(5) ?
N3 Cd1 Cl1 . . 90.34(5) ?
N4 Cd1 Cl2 . . 94.30(5) ?
N3 Cd1 Cl2 . . 156.49(5) ?
Cl1 Cd1 Cl2 . . 110.65(2) ?
N4 Cd1 Cl1 . 17 85.72(5) ?
N3 Cd1 Cl1 . 17 102.69(5) ?
Cl1 Cd1 Cl1 . 17 83.75(2) ?
Cl2 Cd1 Cl1 . 17 90.436(19) ?
N4 Cd1 Cl2 . 10_455 96.11(5) ?
N3 Cd1 Cl2 . 10_455 83.49(5) ?
Cl1 Cd1 Cl2 . 10_455 97.04(2) ?
Cl2 Cd1 Cl2 . 10_455 83.511(19) ?
Cl1 Cd1 Cl2 17 10_455 173.78(2) ?
Cd1 Cl1 Cd1 . 17 94.281(19) ?
Cd1 Cl2 Cd1 . 10_455 96.248(19) ?
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
C1 C2 . 1.366(4) ?
C1 N1 . 1.375(3) ?
C1 C9 . 1.441(3) ?
C2 C3 . 1.415(4) ?
C3 C4 . 1.408(4) ?
C3 C8 . 1.419(4) ?
C4 C5 . 1.364(4) ?
C5 C6 . 1.391(5) ?
C6 C7 . 1.378(4) ?
C7 C8 . 1.391(4) ?
C8 N1 . 1.370(3) ?
C9 N2 . 1.285(3) ?
C10 N3 . 1.282(3) ?
C10 C11 . 1.489(3) ?
C10 C16 . 1.493(3) ?
C11 N4 . 1.344(3) ?
C11 C12 . 1.384(3) ?
C12 C13 . 1.379(4) ?
C13 C14 . 1.368(4) ?
C14 C15 . 1.381(4) ?
C15 N4 . 1.326(3) ?
C16 N5 . 1.345(3) ?
C16 C17 . 1.381(3) ?
C17 C18 . 1.383(4) ?
C18 C19 . 1.367(4) ?
C19 C20 . 1.378(4) ?
C20 N5 . 1.335(3) ?
N2 N3 . 1.401(3) ?
N3 Cd1 . 2.4575(19) ?
N4 Cd1 . 2.3450(19) ?
Cd1 Cl1 . 2.5181(6) ?
Cd1 Cl2 . 2.5746(6) ?
Cd1 Cl1 17 2.6561(6) ?
Cd1 Cl2 10_455 2.6612(6) ?
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 H1 N5 17 0.86 2.13 2.987(3) 178.6 yes
C9 H9 Cl2 10_455 0.93 2.71 3.588(3) 158.7 yes
C12 H12 N5 . 0.93 2.54 2.995(4) 110.3 yes
C18 H18 Cl2 28 0.93 2.83 3.607(3) 142.0 yes
C20 H20 Cl1 36 0.93 2.78 3.431(3) 127.7 yes
_cod_database_fobs_code 2312667