#------------------------------------------------------------------------------
#$Date: 2025-03-08 05:03:09 +0200 (Sat, 08 Mar 2025) $
#$Revision: 298343 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/31/27/2312780.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_2312780
loop_
_publ_author_name
'Shapiro, Nicole M.'
'Govero, Mark D.'
'Bosch, Eric'
'Unruh, Daniel K.'
'Groeneman, Ryan H.'
_publ_section_title
;
Mixed cocrystal approach influences the yield for a [2+2] cycloaddition
reaction within a halogen-bonded organic solid.
;
_journal_coeditor_code JX3092
_journal_issue 4
_journal_name_full
'Acta crystallographica. Section C, Structural chemistry'
_journal_paper_doi 10.1107/S2053229625001913
_journal_volume 81
_journal_year 2025
_chemical_formula_iupac 'C12 H10 N2, 0.75C6 Cl4 I2, 0.25C6 Cl5 I1'
_chemical_formula_moiety 'C12 H10 N2, 0.75(C6 Cl4 I2), 0.25(C6 Cl5 I1)'
_chemical_formula_sum 'C18 H10 Cl4.23 I1.77 N2'
_chemical_formula_weight 628.85
_chemical_name_systematic
;
trans-1,2-Bis(pyridin-4-yl)ethylene
1,4-diiodoperchlorobenzene--iodoperchlorobenzene(0.75/0.25)
;
_space_group_crystal_system triclinic
_space_group_IT_number 2
_space_group_name_Hall '-P 1'
_space_group_name_H-M_alt 'P -1'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary dual
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_cell_angle_alpha 110.8040(10)
_cell_angle_beta 92.660(2)
_cell_angle_gamma 94.651(2)
_cell_formula_units_Z 1
_cell_length_a 4.0677(2)
_cell_length_b 10.9099(6)
_cell_length_c 12.3916(5)
_cell_measurement_reflns_used 5883
_cell_measurement_temperature 290
_cell_measurement_theta_max 28.288
_cell_measurement_theta_min 3.115
_cell_volume 510.70(4)
_computing_cell_refinement
;
SAINT (Bruker, 2016)
;
_computing_data_collection
;
APEX6 (Bruker, 2016)
;
_computing_data_reduction
;
SAINT (Bruker, 2016)
;
_computing_molecular_graphics
;
OLEX2 (Dolomanov et al., 2009)
;
_computing_publication_material
;
OLEX2 (Dolomanov et al., 2009)
;
_computing_structure_refinement
;
SHELXL2019 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT2018 (Sheldrick, 2015a)
;
_diffrn_ambient_temperature 290
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type
'Bruker D8 VENTURE DUO with a Photon III detector'
_diffrn_measurement_method 'phi and omega scans'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0562
_diffrn_reflns_av_unetI/netI 0.0365
_diffrn_reflns_limit_h_max 5
_diffrn_reflns_limit_h_min -5
_diffrn_reflns_limit_k_max 14
_diffrn_reflns_limit_k_min -14
_diffrn_reflns_limit_l_max 15
_diffrn_reflns_limit_l_min -16
_diffrn_reflns_number 18373
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 28.356
_diffrn_reflns_theta_min 2.008
_diffrn_source_current 1.4
_diffrn_source_power 0.07
_diffrn_source_voltage 50.0
_exptl_absorpt_coefficient_mu 3.290
_exptl_absorpt_correction_T_max 0.7457
_exptl_absorpt_correction_T_min 0.6375
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2016)
;
_exptl_crystal_colour 'clear colourless'
_exptl_crystal_density_diffrn 2.045
_exptl_crystal_description irregular
_exptl_crystal_F_000 298
_exptl_crystal_size_max 0.207
_exptl_crystal_size_mid 0.189
_exptl_crystal_size_min 0.07
_refine_diff_density_max 0.396
_refine_diff_density_min -0.608
_refine_ls_extinction_coef 0.0179(16)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method
;
SHELXL2019 (Sheldrick, 2015b)
;
_refine_ls_goodness_of_fit_ref 1.098
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 141
_refine_ls_number_reflns 2555
_refine_ls_number_restraints 44
_refine_ls_restrained_S_all 1.099
_refine_ls_R_factor_all 0.0296
_refine_ls_R_factor_gt 0.0267
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+0.4267P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0473
_refine_ls_wR_factor_ref 0.0484
_reflns_number_gt 2377
_reflns_number_total 2555
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file jx3092sup1.cif
_cod_data_source_block C6I2CL4_C6ICl5_BPE_290and210_290
_cod_database_code 2312780
_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 0.549
_shelx_estimated_absorpt_t_max 0.802
_shelx_hkl_file
;
-1 0 0 93.09 4.90
-1 0 0 89.79 5.60
-1 0 0 88.39 4.90
-1 0 0 87.09 4.70
-1 0 0 102.89 4.90
1 0 0 84.69 4.80
1 0 0 92.59 4.70
1 0 0 79.79 4.70
1 0 0 88.19 4.80
1 0 0 87.99 4.90
-2 0 0 814.12 25.30
-2 0 0 765.12 25.60
-2 0 0 783.32 25.90
-2 0 0 812.22 24.80
-2 0 0 772.72 25.60
2 0 0 836.52 26.30
2 0 0 757.82 24.80
2 0 0 803.32 25.40
2 0 0 794.32 26.00
2 0 0 788.32 25.90
-3 0 0 185.88 11.30
-3 0 0 173.88 11.10
-3 0 0 197.68 12.60
-3 0 0 160.18 11.60
-3 0 0 148.69 11.00
3 0 0 187.68 12.40
3 0 0 154.58 11.00
3 0 0 171.28 11.70
3 0 0 170.38 11.90
3 0 0 144.59 11.20
-4 0 0 73.39 10.70
-4 0 0 64.49 9.50
-4 0 0 62.19 10.10
-4 0 0 59.79 8.90
4 0 0 75.39 10.50
4 0 0 64.39 10.30
4 0 0 55.99 9.70
4 0 0 62.59 9.60
4 0 0 62.49 9.90
-5 0 0 25.40 6.70
-5 0 0 24.60 7.90
-5 0 0 19.90 6.80
5 0 0 25.20 7.20
5 0 0 18.00 7.20
5 0 0 27.30 7.60
5 0 0 21.40 6.50
5 -1 0 23.10 8.10
5 -1 0 31.30 7.30
5 -1 0 28.30 7.90
5 -1 0 19.00 6.50
-5 1 0 52.29 9.80
-5 1 0 26.30 7.20
-5 1 0 47.90 10.50
-5 1 0 32.80 7.50
4 -1 0 218.48 14.80
4 -1 0 210.28 15.70
4 -1 0 229.08 16.00
4 -1 0 254.67 17.10
4 -1 0 238.68 16.20
-4 1 0 190.38 20.70
-4 1 0 216.68 15.70
-4 1 0 204.88 14.30
-4 1 0 220.28 14.70
-4 1 0 225.58 16.40
3 -1 0 448.86 19.80
3 -1 0 436.66 20.50
3 -1 0 459.65 20.80
3 -1 0 483.45 21.50
3 -1 0 479.05 21.10
-3 1 0 481.15 21.30
-3 1 0 491.45 21.50
-3 1 0 470.15 21.40
-3 1 0 465.65 19.80
-3 1 0 458.35 19.20
2 -1 0 67.29 7.30
2 -1 0 59.69 5.50
2 -1 0 67.89 7.30
2 -1 0 60.39 5.40
2 -1 0 56.19 5.10
-2 1 0 70.09 7.50
-2 1 0 67.99 7.20
-2 1 0 56.19 5.00
-2 1 0 64.59 7.00
-2 1 0 59.79 5.20
-1 1 0 604.44 19.90
0 -1 0 111.89 4.30
0 -1 0 114.19 4.40
0 -1 0 110.59 4.80
0 1 0 109.29 4.90
0 1 0 112.69 4.40
0 1 0 132.69 4.50
0 1 0 119.39 4.40
-1 -1 0 1680.23 305.97
-1 -1 0 1509.95 53.69
1 1 0 1483.35 52.89
1 1 0 1759.92 279.47
-2 -1 0 122.49 8.00
-2 -1 0 126.59 7.90
-2 -1 0 133.79 7.70
-2 -1 0 133.69 8.60
-2 -1 0 125.19 7.90
2 1 0 120.29 8.00
2 1 0 134.09 7.90
2 1 0 114.69 7.90
2 1 0 121.29 7.70
2 1 0 134.69 8.30
-3 -1 0 183.68 11.80
-3 -1 0 184.38 12.90
-3 -1 0 197.88 12.40
-3 -1 0 188.48 11.60
3 1 0 192.38 12.60
3 1 0 203.88 12.30
3 1 0 178.08 12.40
3 1 0 198.38 12.90
-4 -1 0 191.68 14.20
-4 -1 0 195.28 15.60
-4 -1 0 184.58 14.40
4 1 0 190.78 14.60
4 1 0 181.18 14.10
4 1 0 178.68 14.60
4 1 0 190.38 14.60
4 1 0 168.28 13.50
-5 -1 0 3.40 4.00
-5 -1 0 -0.50 2.30
5 1 0 9.50 5.70
5 1 0 2.70 4.00
5 1 0 4.60 4.40
5 1 0 5.40 4.40
5 -2 0 14.80 5.10
5 -2 0 33.30 7.80
5 -2 0 19.40 8.20
5 -2 0 36.80 9.50
-5 2 0 22.30 6.40
-5 2 0 21.70 6.90
-5 2 0 21.00 5.70
4 -2 0 120.99 14.30
4 -2 0 146.29 12.80
4 -2 0 154.18 13.30
4 -2 0 122.49 11.00
4 -2 0 144.29 12.90
-4 2 0 125.49 11.20
-4 2 0 109.99 12.80
-4 2 0 131.39 11.10
-4 2 0 129.29 12.20
3 -2 0 24.50 5.70
3 -2 0 37.80 7.00
3 -2 0 21.70 4.80
3 -2 0 27.80 6.10
-3 2 0 23.30 5.50
-3 2 0 33.60 6.00
-3 2 0 15.80 4.60
-3 2 0 18.60 5.60
2 -2 0 510.05 18.60
2 -2 0 505.65 19.10
2 -2 0 513.65 19.50
2 -2 0 503.55 18.10
2 -2 0 523.75 19.10
-2 2 0 509.45 19.60
-2 2 0 487.65 17.80
-2 2 0 461.25 18.50
-2 2 0 541.45 19.40
-2 2 0 505.75 18.10
1 -2 0 26.90 3.70
1 -2 0 24.80 3.10
1 -2 0 24.20 3.30
1 -2 0 27.70 3.20
1 -2 0 33.90 3.70
-1 2 0 27.60 3.80
-1 2 0 29.30 3.30
-1 2 0 24.50 3.30
-1 2 0 27.30 3.20
-1 2 0 23.40 3.20
0 -2 0 1656.93 157.68
0 -2 0 1467.25 44.00
0 2 0 1414.86 41.50
0 2 0 1897.21 222.98
-1 -2 0 1823.52 345.97
-1 -2 0 886.71 47.10
1 2 0 960.30 52.79
1 2 0 1070.49 306.07
-2 -2 0 92.09 6.80
-2 -2 0 84.99 6.30
-2 -2 0 76.89 6.70
-2 -2 0 79.99 6.50
2 2 0 70.39 6.70
2 2 0 86.79 6.50
2 2 0 86.59 6.60
2 2 0 87.39 6.70
2 2 0 87.79 7.00
2 2 0 89.49 6.90
-3 -2 0 471.75 20.60
-3 -2 0 422.86 19.80
-3 -2 0 436.36 21.00
3 2 0 402.16 20.20
3 2 0 464.75 20.30
3 2 0 450.05 20.10
3 2 0 462.25 20.90
3 2 0 462.55 20.60
-4 -2 0 5.80 4.10
-4 -2 0 1.20 3.40
-4 -2 0 6.90 4.70
4 2 0 4.50 3.80
4 2 0 2.70 3.10
4 2 0 7.00 4.70
4 2 0 0.70 3.00
4 2 0 6.10 4.10
4 2 0 -1.00 3.00
-5 -2 0 51.69 10.60
5 2 0 50.39 10.50
5 2 0 57.09 12.10
5 2 0 42.80 10.20
5 2 0 44.20 10.00
5 -3 0 28.80 9.30
5 -3 0 30.90 8.40
5 -3 0 43.10 8.70
5 -3 0 29.20 7.80
-5 3 0 49.30 9.50
-5 3 0 39.10 8.70
-5 3 0 38.10 7.80
4 -3 0 16.30 5.50
4 -3 0 28.90 7.20
4 -3 0 9.70 4.60
4 -3 0 20.30 5.70
4 -3 0 19.80 6.20
-4 3 0 10.00 4.50
-4 3 0 20.50 6.40
-4 3 0 15.10 5.60
3 -3 0 854.51 29.20
3 -3 0 801.82 29.70
3 -3 0 799.32 32.80
3 -3 0 798.62 30.30
3 -3 0 769.32 30.40
-3 3 0 753.62 29.60
-3 3 0 783.52 28.50
-3 3 0 800.82 27.90
-3 3 0 784.82 29.60
2 -3 0 692.63 24.70
2 -3 0 682.33 24.00
2 -3 0 658.63 22.70
2 -3 0 726.13 23.80
-2 3 0 720.63 25.40
-2 3 0 664.73 23.40
-2 3 0 655.73 22.80
-2 3 0 685.93 24.10
-2 3 0 681.83 22.50
1 -3 0 1774.52 397.46
1 -3 0 1469.75 67.29
-1 3 0 1424.76 62.19
-1 3 0 1713.13 414.36
0 -3 0 1947.41 61.29
0 -3 0 2049.89 250.07
0 3 0 2493.95 329.77
0 3 0 1867.71 58.19
-1 -3 0 351.56 13.80
-1 -3 0 351.56 14.10
-1 -3 0 336.57 12.90
-1 -3 0 348.17 13.10
-1 -3 0 330.17 12.40
1 3 0 333.67 12.70
1 3 0 340.47 13.70
1 3 0 348.97 12.80
1 3 0 342.17 13.30
1 3 0 334.17 13.00
-2 -3 0 870.91 29.30
-2 -3 0 945.61 29.70
-2 -3 0 938.51 28.60
-2 -3 0 906.11 30.50
2 3 0 872.01 29.20
2 3 0 939.31 30.60
2 3 0 886.61 28.90
2 3 0 894.51 29.50
2 3 0 938.91 31.00
2 3 0 928.21 29.50
-3 -3 0 68.29 9.20
-3 -3 0 79.69 10.10
-3 -3 0 83.09 9.30
-3 -3 0 76.99 10.40
3 3 0 83.69 10.30
3 3 0 72.69 9.30
3 3 0 67.59 9.60
3 3 0 66.89 9.90
3 3 0 93.39 10.70
3 3 0 87.69 10.20
-4 -3 0 168.08 14.10
-4 -3 0 146.09 12.80
-4 -3 0 179.38 15.20
-4 -3 0 153.78 12.20
4 3 0 134.39 12.70
4 3 0 124.69 15.10
4 3 0 174.38 14.20
4 3 0 159.18 13.50
4 3 0 123.39 14.90
4 3 0 167.18 15.80
-5 -3 0 6.50 4.70
-5 -3 0 0.70 3.30
5 -4 0 5.30 3.60
5 -4 0 2.70 3.70
5 -4 0 3.20 5.00
-5 4 0 13.90 5.60
-5 4 0 10.60 6.00
4 -4 0 192.78 14.90
4 -4 0 170.08 13.10
4 -4 0 167.98 14.40
4 -4 0 170.98 14.60
-4 4 0 158.08 13.40
-4 4 0 177.68 14.50
-4 4 0 153.08 14.30
-4 4 0 185.28 13.40
3 -4 0 15.30 5.30
3 -4 0 13.50 4.40
3 -4 0 7.50 3.80
3 -4 0 6.00 3.50
3 -4 0 10.10 4.10
-3 4 0 10.70 4.50
-3 4 0 7.70 3.80
-3 4 0 9.90 4.00
-3 4 0 9.20 3.60
-3 4 0 5.10 3.60
2 -4 0 726.93 24.20
2 -4 0 718.13 24.90
2 -4 0 744.43 25.00
2 -4 0 719.93 24.90
2 -4 0 705.03 25.50
2 -4 0 718.33 26.20
-2 4 0 734.73 27.00
-2 4 0 671.83 25.10
-2 4 0 730.13 24.60
-2 4 0 688.13 24.70
-2 4 0 760.22 24.20
1 -4 0 655.33 21.00
1 -4 0 626.24 21.30
1 -4 0 654.63 20.90
1 -4 0 642.04 20.40
1 -4 0 649.34 22.00
1 -4 0 656.43 20.90
-1 4 0 672.03 21.10
-1 4 0 628.64 22.10
-1 4 0 636.14 21.20
-1 4 0 619.34 21.20
-1 4 0 642.44 20.60
0 -4 0 2029.20 75.59
0 -4 0 2154.68 419.16
0 4 0 2042.80 71.39
0 4 0 2275.77 460.55
1 4 0 1094.59 32.10
1 4 0 1092.39 33.30
-2 -4 0 224.48 11.40
-2 -4 0 198.48 11.50
-2 -4 0 208.98 12.50
-2 -4 0 206.28 11.80
2 4 0 215.38 12.00
2 4 0 211.98 12.70
2 4 0 224.18 12.80
2 4 0 224.58 12.10
2 4 0 224.48 11.80
2 4 0 233.68 12.30
-3 -4 0 259.37 16.10
-3 -4 0 211.58 13.80
-3 -4 0 220.78 14.50
3 4 0 227.88 14.50
3 4 0 241.58 14.40
3 4 0 212.48 14.10
3 4 0 214.18 15.10
3 4 0 216.48 14.10
3 4 0 223.18 15.30
-4 -4 0 37.40 8.00
-4 -4 0 43.70 9.60
-4 -4 0 41.70 8.90
-4 -4 0 25.60 6.40
4 4 0 43.00 9.50
4 4 0 35.70 7.70
4 4 0 46.20 9.10
4 4 0 49.90 9.50
4 4 0 23.90 6.50
4 4 0 52.39 10.20
5 -5 0 86.09 14.60
5 -5 0 53.79 11.10
-5 5 0 72.59 12.10
4 -5 0 15.40 6.20
4 -5 0 6.70 5.20
4 -5 0 8.00 5.40
4 -5 0 9.60 5.10
4 -5 0 9.80 5.00
4 -5 0 3.30 3.40
-4 5 0 1.80 3.30
-4 5 0 16.60 6.10
-4 5 0 11.20 4.90
-4 5 0 7.50 4.30
3 -5 0 315.67 16.80
3 -5 0 304.67 19.60
3 -5 0 321.77 17.90
3 -5 0 288.17 20.80
3 -5 0 317.47 17.30
-3 5 0 333.57 17.50
-3 5 0 352.76 17.40
-3 5 0 326.57 16.00
-3 5 0 287.47 17.10
-3 5 0 324.27 19.00
2 -5 0 198.38 11.60
2 -5 0 204.18 12.40
2 -5 0 204.68 11.10
2 -5 0 222.38 12.70
2 -5 0 191.98 11.10
2 -5 0 214.48 11.80
-2 5 0 199.28 12.90
-2 5 0 226.48 12.10
-2 5 0 225.98 11.10
-2 5 0 214.58 12.40
-2 5 0 190.18 11.20
1 -5 0 540.45 19.30
1 -5 0 570.84 20.20
1 -5 0 563.64 20.00
1 -5 0 595.04 20.40
1 -5 0 577.44 20.90
1 -5 0 566.84 21.00
-1 5 0 569.54 19.30
-1 5 0 573.54 21.50
-1 5 0 590.44 20.80
-1 5 0 548.25 19.60
-1 5 0 518.35 20.10
-1 5 0 569.94 20.20
0 -5 0 636.54 21.80
0 -5 0 609.44 21.60
0 -5 0 640.34 21.80
0 -5 0 601.34 20.60
0 -5 0 583.54 20.20
0 5 0 653.33 20.90
0 5 0 568.04 20.80
0 5 0 603.44 21.30
0 5 0 595.74 21.30
0 5 0 578.14 21.30
0 5 0 596.84 20.60
-1 -5 0 157.78 10.50
-1 -5 0 155.38 9.50
-1 -5 0 162.78 9.20
-1 -5 0 158.28 10.10
-1 -5 0 164.38 9.70
1 5 0 170.08 9.40
1 5 0 160.58 10.20
1 5 0 147.79 9.30
1 5 0 148.19 9.80
-2 -5 0 139.79 9.20
-2 -5 0 165.28 11.40
-2 -5 0 135.49 9.60
-2 -5 0 134.29 9.90
2 5 0 128.09 9.60
2 5 0 127.79 10.00
2 5 0 135.49 10.70
2 5 0 130.39 9.80
2 5 0 116.39 9.00
-3 -5 0 3.70 4.20
-3 -5 0 0.60 2.60
-3 -5 0 8.00 3.80
-3 -5 0 10.90 5.00
3 5 0 2.70 2.90
3 5 0 8.90 4.00
3 5 0 7.90 4.30
3 5 0 8.10 3.60
-4 -5 0 55.89 10.10
-4 -5 0 46.80 8.70
-4 -5 0 35.60 9.00
-4 -5 0 37.00 7.50
4 5 0 52.29 10.40
4 5 0 46.60 9.40
4 5 0 55.29 10.00
4 5 0 44.90 10.00
4 5 0 54.39 9.70
4 5 0 48.40 9.60
5 -6 0 4.90 3.90
-5 6 0 -0.60 1.80
-5 6 0 3.70 3.60
4 -6 0 40.80 7.70
4 -6 0 41.30 9.10
4 -6 0 60.49 9.90
4 -6 0 42.60 8.30
4 -6 0 59.89 10.90
4 -6 0 43.20 8.90
-4 6 0 47.20 8.60
-4 6 0 42.80 8.30
-4 6 0 51.09 8.20
-4 6 0 40.60 11.40
-4 6 0 40.80 8.60
3 -6 0 293.97 18.00
3 -6 0 319.77 18.50
3 -6 0 281.97 15.90
3 -6 0 301.97 17.00
3 -6 0 335.17 17.60
3 -6 0 293.47 17.50
-3 6 0 304.37 18.00
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1 -2 -14 3.50 2.10
0 -2 -14 42.50 9.20
0 -2 -14 39.30 5.10
0 -2 -14 38.10 6.30
0 -2 -14 36.70 5.10
0 -2 -14 40.00 6.90
0 2 14 51.19 10.50
0 10 -15 15.00 2.90
0 10 -15 21.90 5.30
0 10 -15 27.80 5.30
1 9 -15 8.00 2.50
1 9 -15 10.30 3.00
1 9 -15 18.30 6.80
1 9 -15 7.60 3.10
1 9 -15 6.60 2.60
0 9 -15 30.70 5.80
-1 9 -15 19.50 5.70
-1 9 -15 9.60 3.60
-1 9 -15 11.60 3.30
-1 9 -15 10.50 3.30
-1 9 -15 7.20 3.20
1 -9 15 7.70 2.80
1 8 -15 14.60 3.40
1 8 -15 15.80 3.40
1 8 -15 16.10 3.80
1 8 -15 13.10 4.90
1 8 -15 16.90 3.60
0 8 -15 1.80 1.70
0 8 -15 -1.40 1.70
0 8 -15 2.50 2.00
-1 8 -15 11.00 4.30
-1 8 -15 21.00 5.10
-1 8 -15 19.10 4.50
-1 8 -15 16.70 3.30
-1 8 -15 16.30 3.40
2 7 -15 3.60 1.80
2 7 -15 0.50 2.20
2 7 -15 4.30 1.90
1 7 -15 39.50 8.10
1 7 -15 46.50 4.30
1 7 -15 39.70 6.10
1 7 -15 43.10 4.80
0 7 -15 6.30 3.60
0 7 -15 13.40 3.20
0 7 -15 9.30 2.60
-1 7 -15 11.50 2.70
-1 7 -15 6.60 3.00
-1 7 -15 22.40 5.40
-1 7 -15 15.40 3.00
1 -7 15 16.60 2.70
2 6 -15 23.60 3.30
2 6 -15 20.50 6.10
2 6 -15 27.50 3.40
2 6 -15 39.70 9.00
1 6 -15 10.20 4.30
1 6 -15 13.30 2.40
1 6 -15 15.40 4.20
0 6 -15 88.19 10.20
0 6 -15 68.99 5.50
0 6 -15 77.49 6.10
-1 6 -15 0.20 1.00
-1 6 -15 5.20 2.50
-1 6 -15 1.70 2.00
-1 6 -15 5.80 2.70
1 -6 15 4.30 1.70
1 -6 15 3.30 1.40
-2 6 -15 50.59 8.70
-2 6 -15 49.50 8.40
-2 6 -15 54.69 9.20
2 -6 15 44.30 6.80
2 5 -15 45.00 9.00
2 5 -15 45.20 3.10
2 5 -15 41.10 3.40
2 5 -15 52.39 9.10
1 5 -15 82.59 10.10
1 5 -15 99.09 11.80
0 5 -15 3.30 2.50
0 5 -15 4.70 2.10
0 5 -15 4.60 2.20
0 5 -15 3.70 1.80
-1 5 -15 61.09 8.00
-1 5 -15 43.90 6.80
1 -5 15 45.30 2.80
-2 5 -15 4.00 3.10
-2 5 -15 1.80 2.10
-2 5 -15 0.30 2.10
2 -5 15 5.40 2.90
2 -5 15 0.70 1.40
2 4 -15 4.30 3.10
2 4 -15 3.60 3.10
1 4 -15 2.90 2.50
1 4 -15 4.30 3.50
0 4 -15 16.10 3.70
0 4 -15 16.40 4.30
0 4 -15 17.00 3.20
0 4 -15 21.50 3.70
-1 4 -15 2.50 2.40
-1 4 -15 1.30 1.70
-1 4 -15 5.70 2.70
1 -4 15 2.10 0.90
-2 4 -15 18.30 5.20
-2 4 -15 21.50 4.90
-2 4 -15 12.20 4.60
2 -4 15 17.30 4.30
2 3 -15 3.90 3.30
2 3 -15 6.00 3.90
1 3 -15 116.19 10.00
0 3 -15 63.39 5.40
0 3 -15 46.90 7.30
0 3 -15 52.09 4.80
-1 3 -15 23.20 4.70
-1 3 -15 18.70 3.30
-1 3 -15 30.90 5.80
1 -3 15 25.70 2.30
2 2 -15 64.89 10.80
2 2 -15 55.29 9.40
1 2 -15 1.60 1.20
1 2 -15 0.00 2.20
1 2 -15 8.60 3.40
0 2 -15 56.19 5.20
0 2 -15 54.69 6.30
0 2 -15 52.69 9.90
-1 2 -15 23.40 3.50
-1 2 -15 21.20 5.40
-1 2 -15 27.00 5.20
-1 2 -15 18.50 4.70
1 -2 15 23.80 3.10
2 1 -15 1.60 1.10
2 1 -15 2.70 2.40
2 1 -15 2.00 1.40
1 1 -15 35.30 7.90
1 1 -15 27.80 3.80
1 1 -15 31.30 4.00
1 1 -15 38.30 6.00
0 1 -15 16.70 4.00
0 1 -15 18.80 3.90
0 1 -15 21.90 6.30
-1 1 -15 2.90 1.70
-1 1 -15 3.40 2.50
-1 1 -15 8.30 3.80
-1 1 -15 2.20 1.50
-1 1 -15 5.90 3.80
1 0 -15 77.09 6.20
1 0 -15 70.09 11.60
1 0 -15 69.39 6.40
1 0 -15 74.39 6.40
0 0 -15 2.20 1.90
0 0 -15 2.60 2.80
0 0 -15 1.30 2.20
0 8 -16 13.10 3.30
0 8 -16 8.80 3.20
0 8 -16 6.50 3.70
1 7 -16 9.30 2.20
1 7 -16 11.30 4.80
1 7 -16 6.20 2.90
1 7 -16 9.90 2.20
0 7 -16 28.70 5.90
0 7 -16 39.50 5.60
0 7 -16 32.80 4.80
1 6 -16 48.30 8.60
1 6 -16 42.60 6.90
0 6 -16 19.70 3.70
0 6 -16 18.10 3.50
0 6 -16 13.80 3.90
-1 6 -16 30.90 4.50
-1 6 -16 40.20 5.10
-1 6 -16 34.60 6.20
-1 6 -16 22.10 4.70
1 5 -16 59.29 8.50
1 5 -16 55.99 8.70
0 5 -16 33.20 5.10
0 5 -16 34.70 4.80
0 5 -16 44.80 5.30
0 5 -16 39.10 6.00
-1 5 -16 -0.90 1.30
-1 5 -16 3.80 2.50
1 4 -16 0.80 2.00
0 4 -16 3.30 1.80
0 4 -16 -0.10 1.40
0 4 -16 7.10 2.20
0 4 -16 2.90 1.70
0 4 -16 3.90 2.70
-1 4 -16 3.80 2.30
-1 4 -16 3.90 2.30
1 3 -16 1.20 2.00
1 3 -16 1.40 1.90
0 3 -16 94.89 13.20
0 3 -16 95.19 6.50
0 3 -16 93.69 7.00
1 2 -16 85.79 7.70
1 2 -16 56.59 9.80
1 2 -16 75.69 4.80
1 2 -16 69.69 4.40
0 2 -16 -0.60 1.30
0 2 -16 0.60 1.30
0 0 0 0.00 0.00
_computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)'
;
_shelx_hkl_checksum 12871
_shelx_res_file
;
TITL gro24_05_290_a.res in P-1
gro24_05_290.res
created by SHELXL-2019/3 at 14:34:27 on 06-Mar-2025
REM Old TITL gro24_05_290 in P1
REM SHELXT solution in P-1: R1 0.110, Rweak 0.014, Alpha 0.043
REM 0.000 for 0 systematic absences, Orientation as input
REM Formula found by SHELXT: C10 Cl2 I
CELL 0.71073 4.0677 10.9099 12.3916 110.804 92.66 94.651
ZERR 1 0.0002 0.0006 0.0005 0.001 0.002 0.002
LATT 1
SFAC C H Cl I N
UNIT 18 10 4.23 1.77 2
EQIV $1 2-X,-Y,-Z
RIGU 0.001 0.001 I1 Cl3 C3
SIMU 0.005 0.01 2 I1 Cl3 C3
RIGU 0.001 0.001 C6 C9A C9B
SIMU 0.005 0.01 2 C6 C9A C9B
DFIX 41 C6 C9A C6 C9B
DFIX 51 C9A C9A_$1 C9B C9B_$1
L.S. 10
PLAN 2
SIZE 0.07 0.189 0.207
TEMP 16.85
CONF
BIND N1 I1
BIND N1 Cl3
BOND
list 4
MORE -1
BOND $H
fmap 2 53
acta
REM
REM
REM
WGHT 0.000000 0.407800
EXTI 0.017899
FVAR 0.59906 0.88404 0.90480 1.51794 1.30242
PART 1
I1 4 0.710363 0.711167 0.287770 21.00000 0.04078 0.03521 =
0.03498 0.00056 0.00314 0.00703
PART 0
CL1 3 0.233558 0.987401 0.727407 11.00000 0.06214 0.05773 =
0.03422 0.01691 0.01370 0.00281
CL2 3 0.413358 0.734149 0.541107 11.00000 0.07958 0.04143 =
0.04825 0.02040 0.00557 0.00508
PART 2
CL3 3 0.715065 0.743206 0.302609 -21.00000 0.03488 0.03556 =
0.03994 -0.01023 -0.00360 0.00464
PART 0
C3 1 0.585698 0.883541 0.414189 11.00000 0.03006 0.03198 =
0.02972 0.00411 -0.00067 0.00379
C1 1 0.380577 0.995624 0.601519 11.00000 0.03462 0.04226 =
0.02443 0.00972 0.00116 0.00193
C2 1 0.463978 0.880936 0.516714 11.00000 0.03583 0.03405 =
0.03283 0.01073 -0.00243 0.00138
N1 5 0.884854 0.455052 0.143132 11.00000 0.06731 0.03044 =
0.05281 0.00953 0.01068 0.00923
PART 1
C9A 1 1.074164 0.050204 0.043685 31.00000 0.04202 0.03669 =
0.03600 0.01560 0.00733 0.00964
AFIX 43
H9A 2 1.236143 0.032888 0.090237 31.00000 -1.20000
AFIX 0
PART 2
C9B 1 0.930452 0.044631 -0.012979 -31.00000 0.04261 0.03336 =
0.04048 0.01595 0.01063 0.00936
AFIX 43
H9B 2 0.793030 0.023461 -0.080536 -31.00000 -1.20000
AFIX 0
PART 0
C7 1 0.840167 0.237725 -0.001154 11.00000 0.05941 0.03868 =
0.03881 0.00575 0.00677 0.00535
AFIX 43
H7 2 0.766554 0.182317 -0.076174 11.00000 -1.20000
AFIX 0
C4 1 1.041614 0.406819 0.213797 11.00000 0.07323 0.03704 =
0.04402 0.00624 0.00092 -0.00088
AFIX 43
H4 2 1.110742 0.464124 0.288607 11.00000 -1.20000
AFIX 0
C8 1 0.788720 0.370573 0.037597 11.00000 0.06283 0.04148 =
0.05053 0.01765 0.00547 0.01143
AFIX 43
H8 2 0.680493 0.401725 -0.013688 11.00000 -1.20000
AFIX 0
C6 1 1.002846 0.188995 0.073663 11.00000 0.04592 0.03375 =
0.04583 0.01463 0.01559 0.00621
C5 1 1.107348 0.277652 0.182912 11.00000 0.06421 0.04231 =
0.04965 0.02006 0.00254 0.00360
AFIX 43
H5 2 1.221883 0.250248 0.235555 11.00000 -1.20000
AFIX 0
HKLF 4
REM gro24_05_290_a.res in P-1
REM wR2 = 0.0482, GooF = S = 1.108, Restrained GooF = 1.108 for all data
REM R1 = 0.0267 for 2377 Fo > 4sig(Fo) and 0.0296 for all 2555 data
REM 141 parameters refined using 44 restraints
END
WGHT 0.0000 0.4077
REM Highest difference peak 0.396, deepest hole -0.609, 1-sigma level 0.090
Q1 1 0.1928 1.1597 0.7838 11.00000 0.05 0.40
Q2 1 0.6617 0.8207 0.2016 11.00000 0.05 0.36
;
_shelx_res_checksum 78069
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -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
I I1 0.71036(16) 0.71117(4) 0.28777(4) 0.04012(11) Uani d 0.884(3) A 1
Cl Cl1 0.23356(19) 0.98740(7) 0.72741(6) 0.0511(2) Uani d 1 . .
Cl Cl2 0.4134(2) 0.73415(7) 0.54111(6) 0.0553(2) Uani d 1 . .
Cl Cl3 0.715(5) 0.7432(13) 0.3026(16) 0.043(2) Uani d 0.116(3) A 2
C C3 0.5857(6) 0.8835(2) 0.41419(19) 0.0326(5) Uani d 1 . .
C C1 0.3806(6) 0.9956(2) 0.60152(19) 0.0346(5) Uani d 1 . .
C C2 0.4640(6) 0.8809(2) 0.5167(2) 0.0349(5) Uani d 1 . .
N N1 0.8849(7) 0.4551(2) 0.1431(2) 0.0512(6) Uani d 1 . .
C C9A 1.0742(7) 0.0502(3) 0.0437(2) 0.0371(7) Uani d 0.905(6) B 1
H H9A 1.236143 0.032888 0.090237 0.045 Uiso calc 0.905(6) B 1
C C9B 0.930(6) 0.0446(17) -0.013(2) 0.038(2) Uani d 0.095(6) B 2
H H9B 0.793030 0.023461 -0.080536 0.045 Uiso calc 0.095(6) B 2
C C7 0.8402(7) 0.2377(3) -0.0012(2) 0.0478(7) Uani d 1 . .
H H7 0.766554 0.182317 -0.076174 0.057 Uiso calc 1 . .
C C4 1.0416(8) 0.4068(3) 0.2138(3) 0.0542(8) Uani d 1 . .
H H4 1.110742 0.464124 0.288607 0.065 Uiso calc 1 . .
C C8 0.7887(8) 0.3706(3) 0.0376(3) 0.0509(7) Uani d 1 . .
H H8 0.680493 0.401725 -0.013688 0.061 Uiso calc 1 . .
C C6 1.0028(7) 0.1890(2) 0.0737(2) 0.0412(6) Uani d 1 . .
C C5 1.1073(8) 0.2777(3) 0.1829(3) 0.0513(7) Uani d 1 . .
H H5 1.221883 0.250248 0.235555 0.062 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
I1 0.04078(14) 0.0352(2) 0.0350(2) 0.00703(17) 0.00314(12) 0.00056(15)
Cl1 0.0621(5) 0.0577(4) 0.0342(3) 0.0028(3) 0.0137(3) 0.0169(3)
Cl2 0.0796(5) 0.0414(4) 0.0482(4) 0.0051(3) 0.0056(3) 0.0204(3)
Cl3 0.035(3) 0.036(3) 0.040(3) 0.005(3) -0.004(2) -0.010(3)
C3 0.0301(11) 0.0320(12) 0.0297(11) 0.0038(9) -0.0007(9) 0.0041(9)
C1 0.0346(12) 0.0423(13) 0.0244(11) 0.0019(10) 0.0012(9) 0.0097(9)
C2 0.0358(12) 0.0341(12) 0.0328(12) 0.0014(10) -0.0024(9) 0.0107(10)
N1 0.0673(16) 0.0304(11) 0.0528(14) 0.0092(11) 0.0107(12) 0.0095(10)
C9A 0.0420(15) 0.0367(13) 0.0360(14) 0.0096(11) 0.0073(11) 0.0156(10)
C9B 0.043(4) 0.033(3) 0.040(3) 0.009(3) 0.011(3) 0.016(3)
C7 0.0594(17) 0.0387(14) 0.0388(14) 0.0054(13) 0.0068(12) 0.0057(11)
C4 0.073(2) 0.0370(15) 0.0440(15) -0.0009(14) 0.0009(14) 0.0062(12)
C8 0.0628(18) 0.0415(15) 0.0505(16) 0.0114(13) 0.0055(13) 0.0176(13)
C6 0.0459(14) 0.0337(12) 0.0458(13) 0.0062(10) 0.0156(11) 0.0146(10)
C5 0.0642(19) 0.0423(15) 0.0496(16) 0.0036(13) 0.0025(14) 0.0201(13)
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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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
C3 I1 N1 . . 170.53(9) ?
C3 Cl3 N1 . . 166.0(10) ?
C1 C3 I1 2_676 . 121.32(17) ?
C1 C3 Cl3 2_676 . 117.6(7) ?
C2 C3 I1 . . 120.83(18) ?
C2 C3 Cl3 . . 124.6(7) ?
C2 C3 C1 . 2_676 117.8(2) ?
C3 C1 Cl1 2_676 . 119.63(18) ?
C3 C1 C2 2_676 . 121.0(2) ?
C2 C1 Cl1 . . 119.36(19) ?
C3 C2 Cl2 . . 120.16(18) ?
C3 C2 C1 . . 121.1(2) ?
C1 C2 Cl2 . . 118.70(19) ?
C4 N1 I1 . . 106.31(18) ?
C4 N1 Cl3 . . 106.2(4) ?
C8 N1 I1 . . 135.4(2) ?
C8 N1 Cl3 . . 136.1(4) ?
C8 N1 C4 . . 116.3(2) ?
C9A C9A H9A 2_755 . 117.5 ?
C9A C9A C6 2_755 . 124.9(4) ?
C6 C9A H9A . . 117.5 ?
C9B C9B H9B 2_755 . 121.5 ?
C9B C9B C6 2_755 . 117(3) ?
C6 C9B H9B . . 121.5 ?
C8 C7 H7 . . 120.4 ?
C6 C7 H7 . . 120.4 ?
C6 C7 C8 . . 119.2(3) ?
N1 C4 H4 . . 118.0 ?
N1 C4 C5 . . 124.1(3) ?
C5 C4 H4 . . 118.0 ?
N1 C8 C7 . . 123.8(3) ?
N1 C8 H8 . . 118.1 ?
C7 C8 H8 . . 118.1 ?
C7 C6 C9A . . 124.8(2) ?
C7 C6 C9B . . 92.1(7) ?
C5 C6 C9A . . 118.4(3) ?
C5 C6 C9B . . 150.2(7) ?
C5 C6 C7 . . 116.9(2) ?
C4 C5 C6 . . 119.7(3) ?
C4 C5 H5 . . 120.1 ?
C6 C5 H5 . . 120.1 ?
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
I1 C3 . 2.094(2) ?
I1 N1 . 2.899(2) ?
Cl1 C1 . 1.725(2) ?
Cl2 C2 . 1.730(3) ?
Cl3 C3 . 1.796(14) ?
Cl3 N1 . 3.214(13) ?
C3 C1 2_676 1.396(3) ?
C3 C2 . 1.393(3) ?
C1 C2 . 1.397(3) ?
N1 C4 . 1.334(4) ?
N1 C8 . 1.323(4) ?
C9A C9A 2_755 1.314(6) ?
C9A H9A . 0.9300 ?
C9A C6 . 1.482(4) ?
C9B C9B 2_755 1.29(3) ?
C9B H9B . 0.9300 ?
C9B C6 . 1.55(2) ?
C7 H7 . 0.9300 ?
C7 C8 . 1.393(4) ?
C7 C6 . 1.389(4) ?
C4 H4 . 0.9300 ?
C4 C5 . 1.375(4) ?
C8 H8 . 0.9300 ?
C6 C5 . 1.378(4) ?
C5 H5 . 0.9300 ?
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
I1 C3 C2 Cl2 . . . . -0.1(3) ?
I1 C3 C2 C1 . . . . 179.94(17) ?
I1 N1 C4 C5 . . . . 166.8(3) ?
I1 N1 C8 C7 . . . . -160.8(2) ?
Cl1 C1 C2 Cl2 . . . . 0.5(3) ?
Cl1 C1 C2 C3 . . . . -179.55(18) ?
Cl3 C3 C2 Cl2 . . . . -2.6(8) ?
Cl3 C3 C2 C1 . . . . 177.4(7) ?
Cl3 N1 C4 C5 . . . . 168.7(5) ?
Cl3 N1 C8 C7 . . . . -163.3(6) ?
C3 C1 C2 Cl2 2_676 . . . -179.51(18) ?
C3 C1 C2 C3 2_676 . . . 0.5(4) ?
C1 C3 C2 Cl2 2_676 . . . 179.53(18) ?
C1 C3 C2 C1 2_676 . . . -0.5(4) ?
N1 Cl3 C3 C1 . . . 2_676 -179(4) ?
N1 Cl3 C3 C2 . . . . 4(4) ?
N1 C4 C5 C6 . . . . -1.4(5) ?
C9A C9A C6 C7 2_755 . . . -18.2(5) ?
C9A C9A C6 C5 2_755 . . . 162.6(4) ?
C9A C6 C5 C4 . . . . -179.3(3) ?
C9B C9B C6 C7 2_755 . . . 173(3) ?
C9B C9B C6 C5 2_755 . . . -19(5) ?
C9B C6 C5 C4 . . . . -165(2) ?
C7 C6 C5 C4 . . . . 1.5(4) ?
C4 N1 C8 C7 . . . . 0.5(5) ?
C8 N1 C4 C5 . . . . 0.3(5) ?
C8 C7 C6 C9A . . . . -179.9(3) ?
C8 C7 C6 C9B . . . . 172.5(10) ?
C8 C7 C6 C5 . . . . -0.7(4) ?
C6 C7 C8 N1 . . . . -0.3(5) ?
_cod_database_fobs_code 2312780