#------------------------------------------------------------------------------
#$Date: 2026-09-25 23:23:22 +0200 (Fri, 25 Sep 2026) $
#$Revision: 306916 $
#$URL: svn://www.crystallography.net/cod/cif/2/02/35/2023573.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_2023573
loop_
_publ_author_name
'Bosch, Eric'
_publ_section_title
;
4-Pyrrolidinopyridine as halogen-bond acceptor in cocrystals
;
_journal_coeditor_code JY2073
_journal_issue 7
_journal_name_full
'Acta Crystallographica Section E Crystallographic Communications'
_journal_page_first 834
_journal_page_last 839
_journal_paper_doi 10.1107/S2056989026006092
_journal_volume 82
_journal_year 2026
_chemical_formula_iupac 'C6 H3 I N2 O4, C9 H12 N2'
_chemical_formula_moiety 'C6 H3 I N2 O4, C9 H12 N2'
_chemical_formula_sum 'C15 H15 I N4 O4'
_chemical_formula_weight 442.21
_chemical_name_common
;
4-Pyrrolidinopyridine--1-iodo-3,5-dinitrobenzene (1/1)
;
_chemical_name_systematic
;
4-(Pyrrolidin-1-yl)pyridine--1-iodo-3,5-dinitrobenzene (1/1)
;
_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 SHELXL-2019/3
_cell_angle_alpha 82.209(2)
_cell_angle_beta 87.800(2)
_cell_angle_gamma 83.219(2)
_cell_formula_units_Z 2
_cell_length_a 7.9441(14)
_cell_length_b 8.4866(15)
_cell_length_c 12.139(2)
_cell_measurement_reflns_used 4152
_cell_measurement_temperature 100(2)
_cell_measurement_theta_max 27.07
_cell_measurement_theta_min 2.44
_cell_volume 805.0(2)
_computing_cell_refinement
;
SAINT (Bruker, 2014)
;
_computing_data_collection
;
SMART (Bruker, 2014)
;
_computing_data_reduction
;
SAINT (Bruker, 2014)
;
_computing_molecular_graphics
;
XSEED-4 (Barbour, 2020)
;
_computing_publication_material
;
XSEED-4 (Barbour, 2020)
;
_computing_structure_refinement
;
SHELXL2019/2 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT2018/2 (Sheldrick, 2015a)
;
_diffrn_ambient_temperature 100(2)
_diffrn_detector_area_resol_mean 8.3660
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type 'Bruker APEXI CCD'
_diffrn_measurement_method '\f and \w scans'
_diffrn_radiation_type 'Mo K\a'
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0245
_diffrn_reflns_av_unetI/netI 0.0322
_diffrn_reflns_limit_h_max 10
_diffrn_reflns_limit_h_min -10
_diffrn_reflns_limit_k_max 10
_diffrn_reflns_limit_k_min -10
_diffrn_reflns_limit_l_max 15
_diffrn_reflns_limit_l_min -15
_diffrn_reflns_number 8115
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 27.101
_diffrn_reflns_theta_min 2.438
_exptl_absorpt_coefficient_mu 2.017
_exptl_absorpt_correction_T_max 0.7455
_exptl_absorpt_correction_T_min 0.5650
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
(SADABS; Krause et al., 2015)
;
_exptl_crystal_colour red
_exptl_crystal_density_diffrn 1.824
_exptl_crystal_description block
_exptl_crystal_F_000 436
_exptl_crystal_size_max 0.18
_exptl_crystal_size_mid 0.05
_exptl_crystal_size_min 0.04
_refine_diff_density_max 0.913
_refine_diff_density_min -0.529
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.042
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 217
_refine_ls_number_reflns 3527
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.042
_refine_ls_R_factor_all 0.0296
_refine_ls_R_factor_gt 0.0242
_refine_ls_shift/su_max 0.002
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0285P)^2^+0.2789P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0542
_refine_ls_wR_factor_ref 0.0565
_reflns_number_gt 3181
_reflns_number_total 3527
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file jy2073.cif
_cod_data_source_block DNIB4PYPY
_cod_database_code 2023573
_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
;
-1 0 0 543.65 7.30
1 0 0 549.85 7.50
-2 0 0 130.09 3.10
2 0 0 128.59 3.40
-3 0 0 39.30 2.20
3 0 0 37.70 2.40
-4 0 0 373.76 7.80
4 0 0 373.36 8.40
-5 0 0 287.67 7.40
5 0 0 282.67 7.90
-6 0 0 114.79 5.30
6 0 0 107.09 6.10
-7 0 0 -4.40 2.30
7 0 0 -3.20 2.30
-8 0 0 108.89 6.60
8 0 0 102.09 7.20
-9 0 0 59.89 6.10
9 0 0 72.59 7.60
-10 0 0 58.69 6.20
10 0 0 63.89 7.20
9 -1 0 90.49 7.10
-9 1 0 83.29 5.90
8 -1 0 31.40 4.80
-8 1 0 34.30 4.40
7 -1 0 -4.90 2.20
-7 1 0 2.90 2.10
6 -1 0 21.10 3.60
-6 1 0 21.30 3.00
5 -1 0 332.37 9.00
-5 1 0 335.07 8.10
4 -1 0 546.05 10.80
-4 1 0 557.54 10.30
3 -1 0 3.80 1.20
-3 1 0 0.90 1.00
2 -1 0 0.20 0.80
-2 1 0 0.40 0.90
1 -1 0 1535.15 19.60
1 -1 0 1570.24 19.50
-1 1 0 1554.84 19.40
0 -1 0 512.35 6.90
0 1 0 482.85 6.50
0 1 0 483.65 6.50
-1 -1 0 240.58 3.90
1 1 0 235.98 3.90
-2 -1 0 152.38 3.50
2 1 0 143.39 3.50
2 1 0 145.49 3.20
-3 -1 0 100.59 3.30
3 1 0 97.69 2.80
3 1 0 103.39 3.50
-4 -1 0 344.07 7.40
4 1 0 338.77 6.30
4 1 0 348.87 7.80
-5 -1 0 483.85 10.00
5 1 0 492.45 10.80
-6 -1 0 171.78 6.10
6 1 0 175.58 7.00
-7 -1 0 4.10 2.10
7 1 0 -4.80 2.40
-8 -1 0 79.39 5.80
8 1 0 70.29 6.40
-9 -1 0 120.69 7.20
9 1 0 120.59 8.20
-10 -1 0 94.99 7.40
10 1 0 107.79 8.60
9 -2 0 84.19 7.30
-9 2 0 100.69 6.40
8 -2 0 47.40 5.90
-8 2 0 38.20 4.40
7 -2 0 6.70 3.00
-7 2 0 8.60 2.50
6 -2 0 109.49 6.10
-6 2 0 113.29 5.20
5 -2 0 554.44 12.30
-5 2 0 556.24 11.30
4 -2 0 741.03 13.70
-4 2 0 753.72 13.00
3 -2 0 13.50 2.00
3 -2 0 14.60 2.10
-3 2 0 13.00 1.80
2 -2 0 99.19 3.20
2 -2 0 95.49 3.40
-2 2 0 94.29 3.10
1 -2 0 829.12 12.20
-1 2 0 809.92 11.00
-1 2 0 824.52 11.50
0 -2 0 1789.62 23.20
0 2 0 1773.92 22.40
0 2 0 1797.72 22.40
-1 -2 0 732.93 10.40
1 2 0 733.23 10.40
1 2 0 726.73 10.20
-2 -2 0 62.69 2.30
2 2 0 57.39 2.20
-3 -2 0 192.48 4.70
3 2 0 180.88 4.50
3 2 0 188.68 4.80
-4 -2 0 535.85 10.00
4 2 0 529.05 9.30
4 2 0 551.84 10.20
-5 -2 0 253.57 6.80
5 2 0 238.68 5.80
5 2 0 244.98 7.20
-6 -2 0 143.29 5.60
6 2 0 140.49 6.30
6 2 0 136.69 4.70
-7 -2 0 2.80 1.90
7 2 0 -6.50 2.10
-8 -2 0 59.59 5.10
8 2 0 61.29 6.20
-9 -2 0 96.59 6.40
9 2 0 91.59 7.30
-10 -2 0 37.00 5.20
10 2 0 32.30 5.40
9 -3 0 143.99 8.80
-9 3 0 135.09 7.20
8 -3 0 9.20 3.50
-8 3 0 6.50 2.70
7 -3 0 24.10 4.30
-7 3 0 25.40 3.40
6 -3 0 19.70 3.40
-6 3 0 18.60 2.90
5 -3 0 249.28 8.10
-5 3 0 255.77 7.40
4 -3 0 269.57 7.60
4 -3 0 274.37 7.30
-4 3 0 266.27 7.00
3 -3 0 28.00 2.80
-3 3 0 29.80 2.60
2 -3 0 40.80 3.00
-2 3 0 44.90 2.50
1 -3 0 659.53 11.20
-1 3 0 647.24 9.70
-1 3 0 641.94 10.00
0 -3 0 595.74 10.10
0 3 0 596.14 9.10
0 3 0 573.34 9.10
-1 -3 0 280.07 5.80
1 3 0 277.17 5.60
1 3 0 272.87 5.30
-2 -3 0 45.30 2.30
2 3 0 44.10 2.30
-3 -3 0 187.28 4.90
3 3 0 195.78 4.90
-4 -3 0 840.72 14.00
4 3 0 839.12 13.60
-5 -3 0 330.57 8.20
5 3 0 353.16 8.60
5 3 0 350.96 7.90
-6 -3 0 117.09 5.30
6 3 0 130.79 4.80
6 3 0 117.39 5.90
-7 -3 0 14.90 2.90
7 3 0 11.30 3.20
7 3 0 9.80 2.10
-8 -3 0 109.99 6.20
8 3 0 103.89 7.20
8 3 0 105.59 4.90
-9 -3 0 89.39 6.20
9 3 0 95.29 7.20
-10 -3 0 90.79 7.10
10 3 0 88.09 7.60
8 -4 0 1.20 3.10
-8 4 0 7.40 2.60
7 -4 0 0.90 2.60
-7 4 0 1.00 2.20
6 -4 0 184.78 7.50
6 -4 0 188.08 7.90
-6 4 0 171.48 6.80
5 -4 0 334.47 9.40
5 -4 0 322.27 9.60
-5 4 0 314.47 8.70
4 -4 0 261.07 7.90
-4 4 0 261.27 7.30
3 -4 0 15.90 2.50
-3 4 0 16.20 2.30
2 -4 0 316.47 8.00
-2 4 0 299.97 6.80
1 -4 0 423.66 9.10
-1 4 0 416.56 7.80
-1 4 0 399.26 7.40
0 -4 0 1164.78 18.10
0 4 0 1161.28 16.60
0 4 0 1136.89 16.60
-1 -4 0 260.47 6.50
1 4 0 277.77 6.00
1 4 0 253.17 5.60
-2 -4 0 20.30 2.20
2 4 0 19.30 2.00
-3 -4 0 285.27 6.60
3 4 0 288.07 6.70
-4 -4 0 344.57 7.90
4 4 0 336.47 7.80
-5 -4 0 204.88 6.40
5 4 0 203.38 6.20
-6 -4 0 63.99 4.20
6 4 0 64.69 4.00
-7 -4 0 8.30 2.50
7 4 0 9.50 2.30
7 4 0 -0.20 2.70
-8 -4 0 104.29 6.10
8 4 0 119.59 5.50
8 4 0 116.49 7.10
-9 -4 0 107.19 6.70
9 4 0 119.19 7.60
9 4 0 125.79 8.10
8 -5 0 31.90 5.10
-8 5 0 24.90 3.90
7 -5 0 2.10 2.60
-7 5 0 7.10 2.50
6 -5 0 37.50 4.80
-6 5 0 32.10 3.90
5 -5 0 212.28 8.20
-5 5 0 216.98 7.50
4 -5 0 125.69 6.20
-4 5 0 130.99 5.50
3 -5 0 1.90 2.10
-3 5 0 2.30 1.60
2 -5 0 6.60 2.30
-2 5 0 12.80 1.70
-2 5 0 11.50 1.90
1 -5 0 229.28 7.20
-1 5 0 227.28 5.80
-1 5 0 227.78 5.60
0 -5 0 612.14 12.30
0 5 0 597.24 10.60
0 5 0 588.74 10.60
-1 -5 0 66.19 3.90
1 5 0 69.89 3.40
1 5 0 66.49 3.20
-2 -5 0 22.20 2.70
2 5 0 27.00 2.30
2 5 0 21.20 2.50
-3 -5 0 207.18 5.90
3 5 0 188.38 5.80
-4 -5 0 274.97 7.30
4 5 0 289.47 7.60
-5 -5 0 289.07 8.10
5 5 0 304.17 8.10
-6 -5 0 74.99 4.70
6 5 0 73.59 4.40
-7 -5 0 16.40 3.20
7 5 0 15.20 2.80
-8 -5 0 67.69 5.40
8 5 0 76.99 4.90
-9 -5 0 110.59 6.90
9 5 0 117.19 7.30
9 5 0 122.09 6.20
7 -6 0 17.50 4.40
-7 6 0 19.00 3.60
6 -6 0 165.68 8.40
-6 6 0 168.88 7.40
5 -6 0 277.97 10.10
-5 6 0 280.77 9.00
4 -6 0 336.07 10.60
-4 6 0 344.37 9.40
3 -6 0 3.90 2.50
-3 6 0 5.00 1.90
2 -6 0 31.90 4.10
-2 6 0 29.60 3.10
-2 6 0 29.10 2.80
1 -6 0 270.17 8.60
-1 6 0 272.27 6.80
-1 6 0 274.07 7.10
0 -6 0 332.77 9.30
0 6 0 329.47 7.70
0 6 0 328.27 7.80
-1 -6 0 43.00 4.20
1 6 0 43.40 3.20
1 6 0 45.10 3.10
-2 -6 0 64.09 4.30
2 6 0 72.09 4.00
2 6 0 68.59 3.70
-3 -6 0 186.08 6.10
3 6 0 187.68 6.20
-4 -6 0 241.28 7.10
4 6 0 228.28 7.10
-5 -6 0 146.39 5.90
5 6 0 139.59 5.90
-6 -6 0 118.69 6.00
6 6 0 120.69 5.70
-7 -6 0 3.00 2.30
7 6 0 -1.30 1.80
-8 -6 0 90.59 6.10
8 6 0 85.29 5.50
-9 -6 0 56.39 6.00
9 6 0 51.69 5.20
6 -7 0 28.20 4.70
-6 7 0 31.10 4.20
5 -7 0 124.49 7.80
-5 7 0 113.49 6.30
4 -7 0 50.19 5.60
-4 7 0 64.39 4.70
3 -7 0 -1.90 2.90
-3 7 0 2.50 1.80
2 -7 0 174.88 7.90
-2 7 0 179.28 6.30
-2 7 0 179.68 5.90
1 -7 0 137.69 6.90
-1 7 0 148.69 5.50
-1 7 0 156.98 5.60
0 -7 0 210.08 8.00
0 7 0 211.08 6.60
0 7 0 219.18 6.70
-1 -7 0 67.59 5.10
1 7 0 78.09 4.30
1 7 0 76.59 4.10
-2 -7 0 6.80 2.50
2 7 0 11.90 2.30
2 7 0 11.80 2.40
-3 -7 0 61.79 4.30
-3 -7 0 61.69 4.90
3 7 0 68.29 4.40
-4 -7 0 231.68 7.50
4 7 0 242.28 7.70
-5 -7 0 242.38 8.10
5 7 0 240.78 8.10
-6 -7 0 13.60 3.10
6 7 0 9.30 2.50
-7 -7 0 16.00 3.30
-8 -7 0 208.18 8.90
8 7 0 188.88 8.00
5 -8 0 75.59 7.60
-5 8 0 73.09 5.30
4 -8 0 55.99 6.70
-4 8 0 61.79 4.80
3 -8 0 12.40 3.80
-3 8 0 9.40 2.70
-3 8 0 8.80 2.30
2 -8 0 80.79 6.70
-2 8 0 84.09 4.60
-2 8 0 79.49 4.80
1 -8 0 102.89 6.60
-1 8 0 106.19 5.10
-1 8 0 101.09 5.10
0 -8 0 97.59 6.30
0 8 0 98.19 5.10
0 8 0 95.69 5.00
-1 -8 0 17.70 3.40
1 8 0 22.90 3.20
1 8 0 15.30 2.70
-2 -8 0 10.10 2.90
2 8 0 10.10 2.60
2 8 0 10.30 2.40
-3 -8 0 140.99 6.80
-3 -8 0 124.19 6.20
3 8 0 140.19 6.20
-4 -8 0 256.77 8.50
4 8 0 284.37 9.00
-5 -8 0 20.90 3.50
5 8 0 15.60 3.10
-6 -8 0 0.70 2.10
6 8 0 1.80 2.00
-7 -8 0 16.30 3.70
7 8 0 11.20 3.00
4 -9 0 40.60 6.40
-4 9 0 41.00 4.40
3 -9 0 -0.10 3.30
-3 9 0 -1.50 1.90
2 -9 0 18.90 4.30
-2 9 0 19.40 3.40
-2 9 0 25.90 3.40
1 -9 0 149.39 8.20
-1 9 0 147.99 6.40
-1 9 0 161.38 6.50
0 -9 0 105.09 7.00
0 9 0 110.29 5.70
0 9 0 115.09 5.80
-1 -9 0 25.40 4.30
1 9 0 24.10 3.50
1 9 0 23.60 3.60
-2 -9 0 -0.70 2.30
2 9 0 -1.10 1.80
2 9 0 -1.90 1.80
-3 -9 0 101.79 6.80
-3 -9 0 97.49 5.90
3 9 0 105.79 6.00
-4 -9 0 145.79 7.00
4 9 0 142.69 7.10
-5 -9 0 31.40 4.50
5 9 0 29.00 3.90
-6 -9 0 3.60 3.00
6 9 0 6.00 2.80
2 -10 0 50.29 6.20
-2 10 0 47.90 5.00
1 -10 0 102.39 7.60
-1 10 0 86.19 5.40
-1 10 0 92.89 5.80
0 -10 0 51.89 5.90
0 10 0 70.79 4.90
0 10 0 60.09 5.10
-1 -10 0 1.50 2.60
1 10 0 1.00 2.30
1 10 0 5.50 2.40
-2 -10 0 4.70 3.20
-3 -10 0 43.90 5.20
-3 -10 0 49.90 5.90
3 10 0 49.60 5.30
-4 -10 0 94.79 6.30
4 10 0 101.99 6.70
4 10 -1 8.10 3.20
-4 -10 1 12.60 3.60
3 10 -1 86.89 6.20
-3 -10 1 88.79 6.30
-3 -10 1 110.49 7.20
2 10 -1 80.99 5.70
2 10 -1 92.19 6.10
-2 -10 1 92.59 6.60
1 10 -1 38.80 4.50
1 10 -1 46.00 4.70
-1 -10 1 46.20 6.00
0 10 -1 5.60 2.60
0 10 -1 8.30 2.50
0 -10 1 2.90 2.70
-1 10 -1 3.60 2.20
-1 10 -1 4.60 2.40
1 -10 1 1.70 3.00
-2 10 -1 46.80 5.10
2 -10 1 45.90 6.20
6 9 -1 24.90 3.90
-6 -9 1 20.70 4.00
5 9 -1 10.70 2.80
-5 -9 1 6.80 2.90
4 9 -1 0.70 2.30
-4 -9 1 0.50 2.10
3 9 -1 100.99 6.10
-3 -9 1 100.29 6.40
-3 -9 1 95.09 6.00
2 9 -1 110.79 6.00
2 9 -1 104.29 5.80
-2 -9 1 110.69 6.90
1 9 -1 57.09 4.50
1 9 -1 52.59 4.50
-1 -9 1 53.99 5.60
0 9 -1 4.60 2.10
0 9 -1 1.50 2.10
0 -9 1 1.30 2.40
-1 9 -1 34.40 3.90
-1 9 -1 28.90 3.70
1 -9 1 37.30 5.20
-2 9 -1 96.79 5.30
-2 9 -1 95.99 5.40
2 -9 1 92.39 7.10
-3 9 -1 108.79 6.00
3 -9 1 104.79 8.40
-4 9 -1 27.20 4.10
4 -9 1 29.70 5.60
7 8 -1 99.39 6.10
-7 -8 1 103.39 6.60
6 8 -1 66.09 5.00
-6 -8 1 55.89 5.60
5 8 -1 13.80 3.00
-5 -8 1 15.10 3.30
4 8 -1 125.89 6.40
-4 -8 1 136.69 6.40
3 8 -1 85.99 5.30
-3 -8 1 80.99 5.30
-3 -8 1 87.69 5.50
2 8 -1 253.77 8.10
2 8 -1 258.07 8.10
-2 -8 1 238.88 8.70
1 8 -1 46.70 3.90
1 8 -1 47.90 4.20
-1 -8 1 55.79 5.00
0 8 -1 0.90 1.80
0 8 -1 0.30 1.50
0 -8 1 0.20 2.00
-1 8 -1 47.10 3.90
-1 8 -1 42.00 4.20
1 -8 1 43.70 5.40
-2 8 -1 72.89 4.30
-2 8 -1 84.99 4.90
2 -8 1 72.59 6.00
-3 8 -1 69.49 4.90
3 -8 1 59.69 6.40
-4 8 -1 7.60 2.60
4 -8 1 3.80 3.50
-5 8 -1 18.00 3.30
5 -8 1 29.10 5.60
8 7 -1 2.20 2.30
-8 -7 1 2.30 2.90
7 7 -1 46.60 4.90
-7 -7 1 41.80 5.10
6 7 -1 72.79 5.00
-6 -7 1 85.39 5.40
5 7 -1 61.99 4.40
-5 -7 1 64.29 4.70
4 7 -1 15.00 2.70
-4 -7 1 15.20 2.80
3 7 -1 207.68 7.10
-3 -7 1 214.68 7.20
2 7 -1 259.07 7.60
2 7 -1 258.37 7.70
-2 -7 1 274.07 8.60
1 7 -1 160.28 5.80
1 7 -1 153.58 5.90
-1 -7 1 144.79 6.70
0 7 -1 4.20 1.70
0 7 -1 2.90 1.80
0 -7 1 6.80 2.50
-1 7 -1 197.88 6.50
-1 7 -1 207.08 6.30
1 -7 1 208.78 8.30
-2 7 -1 138.19 5.80
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-1 4 -13 40.60 5.30
-2 4 -13 -0.50 3.30
2 -4 13 6.40 2.60
3 3 -13 33.90 4.70
-3 -3 13 30.50 4.40
2 3 -13 0.50 2.40
-2 -3 13 1.10 2.10
1 3 -13 83.99 6.30
-1 -3 13 65.89 5.20
0 3 -13 71.39 5.80
0 -3 13 68.29 5.00
-1 3 -13 80.89 6.70
1 -3 13 87.89 5.90
-2 3 -13 31.60 5.00
2 -3 13 26.50 4.00
-3 3 -13 17.60 4.20
3 -3 13 14.10 3.20
4 2 -13 76.69 6.90
-4 -2 13 78.99 6.00
3 2 -13 18.70 4.10
-3 -2 13 24.50 4.00
2 2 -13 20.10 3.80
-2 -2 13 7.80 2.70
1 2 -13 33.50 4.50
-1 -2 13 39.70 4.70
0 2 -13 104.19 6.70
0 -2 13 100.59 5.40
-1 2 -13 80.79 6.50
-2 2 -13 -2.30 2.70
2 -2 13 0.70 2.10
-3 2 -13 4.80 3.30
3 -2 13 11.10 3.20
-4 2 -13 40.40 5.60
4 -2 13 41.40 5.20
5 1 -13 90.29 7.80
-5 -1 13 80.59 6.30
4 1 -13 49.40 6.20
-4 -1 13 51.49 5.60
3 1 -13 -1.70 2.50
-3 -1 13 6.00 2.50
2 1 -13 15.10 3.70
-2 -1 13 17.20 3.20
1 1 -13 65.59 5.90
-1 -1 13 59.79 4.80
0 1 -13 121.89 6.70
0 1 -13 120.49 7.20
0 -1 13 120.39 5.80
-1 1 -13 93.39 6.30
-1 1 -13 86.69 6.30
1 -1 13 104.69 5.20
-2 1 -13 -3.70 2.40
2 -1 13 -1.80 1.50
3 -1 13 8.40 2.60
-4 1 -13 72.99 6.70
4 -1 13 79.09 5.90
-5 1 -13 149.79 9.00
5 -1 13 156.78 8.10
5 0 -13 90.19 8.00
-5 0 13 74.69 5.80
4 0 -13 61.49 6.70
-4 0 13 69.29 5.40
3 0 -13 0.60 2.70
-3 0 13 3.00 2.00
2 0 -13 -1.40 2.30
-2 0 13 3.30 2.40
1 0 -13 2.80 2.50
-1 0 13 -0.30 2.10
0 0 -13 50.49 5.50
0 0 13 43.50 4.40
-1 0 -13 113.09 6.90
1 0 13 109.89 5.40
-2 0 -13 4.60 2.70
2 0 13 4.50 2.10
-3 0 -13 42.70 5.40
3 0 13 58.79 5.10
-4 0 -13 108.39 7.70
4 0 13 106.09 6.80
-5 0 -13 129.39 8.40
5 0 13 126.59 7.30
5 -1 -13 75.99 7.90
-5 1 13 84.59 6.70
4 -1 -13 71.39 7.50
-4 1 13 76.29 5.60
3 -1 -13 9.70 3.50
-3 1 13 11.50 3.00
2 -1 -13 5.00 2.90
-2 1 13 6.20 2.30
1 -1 -13 71.99 6.10
-1 1 13 75.39 5.20
0 -1 -13 293.87 10.50
0 1 13 291.67 9.00
-1 -1 -13 55.59 5.60
-1 -1 -13 54.19 5.40
1 1 13 64.99 4.50
-2 -1 -13 11.90 3.30
2 1 13 12.00 2.70
-3 -1 -13 84.29 6.70
3 1 13 96.99 6.00
-4 -1 -13 99.49 7.30
4 1 13 105.89 6.60
-5 -1 -13 62.09 6.60
5 1 13 70.59 5.50
5 -2 -13 36.50 5.30
-5 2 13 37.50 5.30
4 -2 -13 35.40 5.20
-4 2 13 38.30 4.90
3 -2 -13 6.50 2.80
-3 2 13 5.20 2.40
2 -2 -13 47.80 5.50
-2 2 13 63.79 4.90
1 -2 -13 128.29 7.40
-1 2 13 144.59 6.80
0 -2 -13 39.80 5.10
0 -2 -13 38.40 4.60
0 2 13 33.40 4.40
-1 -2 -13 125.09 7.10
-1 -2 -13 136.09 7.10
1 2 13 122.79 6.20
-2 -2 -13 2.80 2.80
2 2 13 1.60 1.80
-3 -2 -13 52.79 5.70
3 2 13 68.69 5.70
-4 -2 -13 88.39 6.80
4 2 13 84.59 6.50
-5 -2 -13 143.19 8.40
5 2 13 162.68 8.50
4 -3 -13 29.70 5.10
-4 3 13 36.20 5.10
3 -3 -13 1.80 2.70
-3 3 13 2.10 2.30
2 -3 -13 27.60 4.50
-2 3 13 35.30 4.50
1 -3 -13 108.29 7.00
-1 3 13 104.89 6.20
0 -3 -13 111.09 6.60
0 -3 -13 100.99 6.60
0 3 13 101.69 6.10
-1 -3 -13 79.49 5.90
-1 -3 -13 84.29 6.20
1 3 13 73.89 5.20
-2 -3 -13 4.00 2.80
2 3 13 1.20 1.80
-3 -3 -13 82.09 6.60
3 3 13 81.99 6.00
3 3 13 74.09 4.70
-4 -3 -13 145.09 8.20
4 3 13 148.09 8.00
-5 -3 -13 40.70 5.20
5 3 13 43.60 5.30
4 -4 -13 37.20 5.40
-4 4 13 27.60 4.90
3 -4 -13 2.10 2.60
-3 4 13 5.80 2.70
2 -4 -13 35.70 5.10
-2 4 13 38.80 4.80
1 -4 -13 76.99 6.00
1 -4 -13 66.49 6.00
-1 4 13 67.39 5.40
0 -4 -13 101.39 6.60
0 -4 -13 104.09 6.70
0 4 13 94.19 5.80
-1 -4 -13 86.19 6.60
-1 -4 -13 69.79 5.70
1 4 13 79.39 5.40
-2 -4 -13 1.50 2.40
2 4 13 -2.10 1.80
-3 -4 -13 52.49 5.90
3 4 13 46.30 5.20
3 4 13 50.59 4.40
-4 -4 -13 88.49 7.10
4 4 13 111.89 7.10
-5 -4 -13 69.99 5.90
5 4 13 77.39 6.40
3 -5 -13 3.40 3.00
-3 5 13 3.10 3.20
2 -5 -13 100.59 7.20
-2 5 13 105.19 6.50
1 -5 -13 69.59 6.20
1 -5 -13 61.59 6.00
-1 5 13 67.69 5.50
0 -5 -13 174.88 8.60
0 -5 -13 178.08 8.60
0 5 13 178.88 7.90
-1 -5 -13 77.99 6.80
-1 -5 -13 69.69 5.90
1 5 13 75.59 5.50
-2 -5 -13 15.60 3.80
2 5 13 16.50 3.40
-3 -5 -13 130.99 8.10
3 5 13 140.19 7.50
3 5 13 141.99 6.60
-4 -5 -13 69.49 7.00
4 5 13 72.29 4.80
4 5 13 71.49 6.10
-5 -5 -13 102.69 6.90
5 5 13 98.79 6.90
2 -6 -13 25.60 4.60
2 -6 -13 23.80 4.00
-2 6 13 20.60 3.70
1 -6 -13 122.19 7.70
1 -6 -13 115.29 7.50
-1 6 13 121.49 7.00
0 -6 -13 82.69 6.60
0 -6 -13 103.09 7.40
0 6 13 102.09 6.50
-1 -6 -13 56.89 6.50
-1 -6 -13 49.80 5.50
1 6 13 61.89 5.30
-2 -6 -13 7.00 3.60
2 6 13 11.20 3.00
-3 -6 -13 60.29 6.60
3 6 13 70.59 5.80
3 6 13 69.69 5.30
-4 -6 -13 80.99 7.30
4 6 13 91.89 5.50
0 -7 -13 68.39 6.30
0 -7 -13 67.79 7.00
0 7 13 73.49 5.80
-1 -7 -13 4.40 3.60
-1 -7 -13 4.20 2.80
1 7 13 8.90 2.80
-2 -7 -13 8.90 4.00
2 7 13 17.20 3.40
2 7 13 22.70 3.80
1 3 -14 1.40 2.80
-1 -3 14 2.40 2.00
-1 3 -14 87.59 7.10
1 -3 14 95.69 6.20
3 2 -14 68.19 6.90
-3 -2 14 74.79 5.80
2 2 -14 31.00 4.80
-2 -2 14 41.20 5.00
1 2 -14 2.10 2.90
-1 -2 14 4.20 2.10
0 2 -14 50.09 5.70
0 -2 14 57.09 4.60
-1 2 -14 116.89 7.50
-2 2 -14 101.49 7.70
2 -2 14 108.69 6.70
-3 2 -14 4.70 3.70
3 -2 14 6.50 3.00
3 1 -14 117.89 8.20
-3 -1 14 130.19 7.00
2 1 -14 56.39 6.30
-2 -1 14 63.49 5.10
1 1 -14 -1.30 2.30
-1 -1 14 -0.60 1.70
0 1 -14 28.40 4.50
0 -1 14 23.00 3.60
-1 1 -14 59.99 6.00
-2 1 -14 79.39 6.80
2 -1 14 77.09 5.70
-3 1 -14 4.90 3.30
3 -1 14 11.40 2.70
-4 0 14 87.69 6.20
3 0 -14 103.49 8.00
-3 0 14 104.59 6.50
2 0 -14 42.40 5.80
-2 0 14 36.10 4.90
1 0 -14 8.20 3.40
-1 0 14 7.50 2.60
0 0 -14 166.98 8.70
0 0 14 168.58 7.20
-1 0 -14 150.78 8.10
-1 0 -14 148.19 8.10
1 0 14 151.48 6.60
-2 0 -14 173.58 8.90
2 0 14 168.78 8.00
-3 0 -14 12.10 3.90
3 0 14 14.20 3.20
-4 0 -14 23.70 4.60
4 0 14 23.70 4.40
4 -1 -14 43.00 6.30
-4 1 14 44.90 5.60
3 -1 -14 42.50 5.90
-3 1 14 39.00 5.30
2 -1 -14 96.39 7.40
-2 1 14 108.29 6.20
1 -1 -14 104.19 7.20
-1 1 14 92.09 5.60
0 -1 -14 74.09 6.00
0 -1 -14 73.49 6.40
0 1 14 72.69 5.40
-1 -1 -14 53.39 5.90
-1 -1 -14 48.60 5.60
1 1 14 47.80 4.90
-2 -1 -14 73.19 6.80
2 1 14 92.79 6.10
-3 -1 -14 18.90 4.20
3 1 14 19.60 3.70
-4 -1 -14 4.40 3.30
4 1 14 0.60 2.30
3 -2 -14 132.89 8.20
-3 2 14 135.59 7.20
2 -2 -14 2.20 2.10
-2 2 14 -2.10 2.10
1 -2 -14 12.00 3.30
-1 2 14 3.80 2.50
0 -2 -14 118.89 7.10
0 2 14 113.79 6.50
-1 -2 -14 102.39 6.60
-1 -2 -14 120.29 7.40
1 2 14 113.69 6.20
-2 -2 -14 172.18 8.60
2 2 14 147.99 6.80
-3 -2 -14 29.40 4.70
3 2 14 29.50 4.50
-4 -2 -14 11.40 3.80
4 2 14 2.50 2.90
3 -3 -14 56.39 6.50
-3 3 14 71.69 5.80
2 -3 -14 40.00 5.20
-2 3 14 34.80 4.60
1 -3 -14 7.60 2.90
-1 3 14 14.20 3.60
0 -3 -14 54.69 5.60
0 -3 -14 62.99 5.70
0 3 14 63.69 5.20
-1 -3 -14 171.58 8.40
-1 -3 -14 172.48 8.50
1 3 14 165.28 7.40
-2 -3 -14 95.89 7.00
2 3 14 94.09 5.70
-3 -3 -14 2.00 3.20
3 3 14 2.60 2.60
-4 -3 -14 31.50 5.10
4 3 14 34.60 5.00
2 -4 -14 -3.60 2.20
-2 4 14 4.40 2.70
1 -4 -14 48.90 5.90
-1 4 14 51.09 5.50
0 -4 -14 116.39 7.40
0 -4 -14 133.59 7.60
0 4 14 136.59 7.10
-1 -4 -14 167.68 8.70
-1 -4 -14 161.88 8.40
1 4 14 149.19 7.20
-2 -4 -14 101.89 7.50
2 4 14 100.59 6.00
-3 -4 -14 0.00 3.00
3 4 14 0.40 2.30
3 4 14 0.20 1.90
-4 -4 -14 40.30 5.70
4 4 14 35.00 5.00
1 -5 -14 14.00 4.00
1 -5 -14 15.00 3.70
-1 5 14 19.30 3.50
0 -5 -14 90.69 7.00
0 -5 -14 94.99 7.30
0 5 14 102.29 6.50
-1 -5 -14 82.39 7.20
-1 -5 -14 75.79 6.30
1 5 14 100.89 6.30
-2 -5 -14 49.99 6.20
2 5 14 62.19 5.90
-3 -5 -14 3.50 3.20
3 5 14 4.50 2.30
3 5 14 0.70 2.40
-1 -6 -14 68.29 7.00
1 6 14 81.29 6.00
-1 -1 15 66.49 5.30
0 1 -15 -0.20 2.80
0 -1 15 1.70 1.90
-1 1 -15 5.90 3.50
2 0 -15 35.00 5.50
-2 0 15 34.70 5.00
1 0 -15 81.49 7.20
-1 0 15 95.19 6.10
0 0 -15 -1.10 2.90
0 0 15 6.60 2.50
-1 0 -15 16.80 4.20
-2 0 -15 53.09 6.30
2 0 15 64.79 5.40
2 -1 -15 122.49 8.60
-2 1 15 119.79 6.90
1 -1 -15 31.00 5.20
-1 1 15 30.50 4.40
0 -1 -15 6.40 3.40
0 1 15 8.80 2.60
-1 -1 -15 45.20 6.00
-1 -1 -15 50.59 6.00
1 1 15 43.00 4.70
-2 -1 -15 64.79 6.70
2 1 15 76.89 5.90
2 -2 -15 35.30 5.40
-2 2 15 39.90 5.30
1 -2 -15 82.59 6.60
-1 2 15 76.39 5.90
0 -2 -15 15.90 3.60
0 -2 -15 17.00 3.80
0 2 15 18.10 3.40
-1 -2 -15 21.00 4.20
-1 -2 -15 25.10 4.20
1 2 15 25.70 3.90
-2 -2 -15 57.19 6.20
2 2 15 56.19 6.20
3 2 15 96.09 7.30
1 -3 -15 42.50 5.50
-1 3 15 49.60 5.80
0 -3 -15 0.50 2.70
0 3 15 -2.00 2.40
-1 -3 -15 36.20 5.00
-1 -3 -15 44.90 5.50
1 3 15 53.49 5.60
-2 -3 -15 111.79 7.80
2 3 15 116.19 6.50
0 -4 -15 1.10 2.50
0 -4 -15 5.00 3.10
0 4 15 6.70 3.10
-1 -4 -15 40.90 5.40
-1 -4 -15 22.60 4.10
1 4 15 27.40 4.10
0 0 0 0.00 0.00
_computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)'
;
_shelx_hkl_checksum 66280
_shelx_res_file
;
TITL eb495_a.res in P-1
H:\CATCHALL\MANUSC~3\A_4567~1\XRD\eb495\eb495_a.res
created by SHELXL-2019/3 at 11:08:07 on 02-Jun-2026
CELL 0.71073 7.9441 8.4866 12.1394 82.209 87.800 83.219
ZERR 2.0000 0.0014 0.0015 0.0022 0.002 0.002 0.002
LATT 1
SFAC C H N O I
UNIT 30 30 8 8 2
BOND
CONF
BOND $H
RTAB XB N1 I1
RTAB XANG C10 I1 N1
EQIV $1 X,Y-1,Z
EQIV $2 -X,-Y,1-Z
EQIV $3 1-X,1-Y,1-Z
EQIV $4 1-X,-Y,1-Z
EQIV $5 X-1,Y,Z-1
HTAB C3 O1_$1
HTAB C7 I1_$2
HTAB C8 O2_$3
HTAB C8 O4_$4
HTAB C9 O4_$5
OMIT 0 0 1
ACTA
FMAP 2 1 53
PLAN 20 0 0
HTAB 2.0
LIST 4 1
TEMP -100
L.S. 16
WGHT 0.028500 0.278900
FVAR 0.33683
I1 5 0.393670 0.489984 0.652397 11.00000 0.02050 0.02056 =
0.01580 -0.00528 -0.00338 -0.00533
O2 4 0.636902 1.046683 0.922357 11.00000 0.03535 0.02296 =
0.03048 -0.01089 -0.00114 -0.01060
O3 4 0.860806 0.517547 1.086183 11.00000 0.02986 0.03412 =
0.02038 -0.00757 -0.00750 -0.00448
O4 4 0.782849 0.309915 1.023830 11.00000 0.04069 0.02134 =
0.02570 -0.00032 -0.01064 0.00044
O1 4 0.470925 1.074763 0.783208 11.00000 0.04487 0.02033 =
0.03828 -0.00153 -0.01357 -0.00111
N1 3 0.241626 0.315027 0.503661 11.00000 0.02668 0.02365 =
0.02040 -0.00888 -0.00141 -0.00607
N2 3 0.092453 0.000813 0.297197 11.00000 0.02173 0.01830 =
0.01832 -0.00435 -0.00705 -0.00146
N3 3 0.562613 0.992434 0.852294 11.00000 0.02639 0.01652 =
0.02582 -0.00561 0.00020 -0.00419
N4 3 0.785026 0.454444 1.021062 11.00000 0.02029 0.02490 =
0.01754 -0.00381 -0.00195 -0.00076
C5 1 0.138479 0.101584 0.364961 11.00000 0.01559 0.01747 =
0.01557 -0.00447 0.00038 -0.00274
C10 1 0.515946 0.590577 0.772390 11.00000 0.01525 0.02067 =
0.01460 -0.00657 0.00057 -0.00463
C15 1 0.608493 0.490602 0.854891 11.00000 0.01696 0.01649 =
0.01568 -0.00446 0.00182 -0.00377
AFIX 43
H15 2 0.617536 0.377528 0.857578 11.00000 -1.20000
AFIX 0
C3 1 0.295459 0.157277 0.518723 11.00000 0.02217 0.02782 =
0.01823 -0.00555 -0.00573 -0.00309
AFIX 43
H3 2 0.370755 0.118433 0.577767 11.00000 -1.20000
AFIX 0
C1 1 0.082264 0.266412 0.349284 11.00000 0.01985 0.01902 =
0.01754 -0.00302 -0.00200 -0.00042
AFIX 43
H1 2 0.007726 0.310176 0.290738 11.00000 -1.20000
AFIX 0
C4 1 0.248872 0.047929 0.454328 11.00000 0.01992 0.02213 =
0.01952 -0.00216 -0.00525 0.00084
AFIX 43
H4 2 0.290598 -0.062168 0.469952 11.00000 -1.20000
AFIX 0
C6 1 0.126067 -0.173748 0.319459 11.00000 0.03055 0.01755 =
0.02164 -0.00464 -0.00508 -0.00527
AFIX 23
H6A 2 0.103579 -0.212086 0.398760 11.00000 -1.20000
H6B 2 0.245087 -0.210446 0.299989 11.00000 -1.20000
AFIX 0
C11 1 0.503199 0.756133 0.770064 11.00000 0.01737 0.02189 =
0.01301 -0.00116 0.00057 -0.00390
AFIX 43
H11 2 0.441806 0.825365 0.713548 11.00000 -1.20000
AFIX 0
C12 1 0.581880 0.817394 0.851827 11.00000 0.01967 0.01332 =
0.02043 -0.00607 0.00350 -0.00399
C14 1 0.687410 0.560702 0.933322 11.00000 0.01698 0.02077 =
0.01446 -0.00391 -0.00074 -0.00140
C2 1 0.136346 0.364000 0.419703 11.00000 0.02436 0.01691 =
0.02271 -0.00351 0.00274 -0.00268
AFIX 43
H2 2 0.095426 0.474592 0.407427 11.00000 -1.20000
AFIX 0
C13 1 0.676049 0.723036 0.934952 11.00000 0.01931 0.02193 =
0.01806 -0.00661 -0.00087 -0.00611
AFIX 43
H13 2 0.729706 0.768028 0.989943 11.00000 -1.20000
AFIX 0
C7 1 0.003506 -0.233155 0.244983 11.00000 0.03236 0.03037 =
0.02652 -0.01229 0.00017 -0.01255
AFIX 23
H7A 2 0.056018 -0.330624 0.214921 11.00000 -1.20000
H7B 2 -0.101840 -0.257661 0.286700 11.00000 -1.20000
AFIX 0
C8 1 -0.033383 -0.095746 0.152049 11.00000 0.02467 0.03730 =
0.02633 -0.01041 -0.00581 -0.00602
AFIX 23
H8A 2 0.053908 -0.100886 0.091809 11.00000 -1.20000
H8B 2 -0.146104 -0.097701 0.120528 11.00000 -1.20000
AFIX 0
C9 1 -0.028989 0.053122 0.208056 11.00000 0.02519 0.02872 =
0.02407 -0.00764 -0.00984 -0.00022
AFIX 23
H9A 2 0.010003 0.141619 0.155250 11.00000 -1.20000
H9B 2 -0.142273 0.088875 0.238628 11.00000 -1.20000
AFIX 0
HKLF 4
REM eb495_a.res in P-1
REM wR2 = 0.0565, GooF = S = 1.042, Restrained GooF = 1.042 for all data
REM R1 = 0.0242 for 3181 Fo > 4sig(Fo) and 0.0296 for all 3527 data
REM 217 parameters refined using 0 restraints
END
WGHT 0.0285 0.2789
REM Instructions for potential hydrogen bonds
HTAB C3 O1_$1
HTAB C7 I1_$2
HTAB C8 O2_$3
HTAB C8 O4_$4
HTAB C9 O4_$5
REM Highest difference peak 0.913, deepest hole -0.529, 1-sigma level 0.091
Q1 1 0.5018 0.4888 0.6159 11.00000 0.05 0.91
Q2 1 0.3054 0.4611 0.6812 11.00000 0.05 0.89
Q3 1 0.4208 0.3935 0.6175 11.00000 0.05 0.79
Q4 1 0.3567 0.5806 0.6799 11.00000 0.05 0.74
Q5 1 0.1032 0.3037 0.3936 11.00000 0.05 0.41
Q6 1 0.3484 0.5674 0.6017 11.00000 0.05 0.39
Q7 1 0.8341 0.3971 1.0000 11.00000 0.05 0.38
Q8 1 -0.0245 -0.0200 0.1776 11.00000 0.05 0.38
Q9 1 0.6009 0.8922 0.8440 11.00000 0.05 0.37
Q10 1 0.1467 0.0455 0.3238 11.00000 0.05 0.37
Q11 1 0.1273 0.1871 0.3477 11.00000 0.05 0.36
Q12 1 -0.2620 -0.3619 0.2815 11.00000 0.05 0.35
Q13 1 0.7238 0.5161 0.9816 11.00000 0.05 0.35
Q14 1 0.2581 -0.2146 0.3426 11.00000 0.05 0.34
Q15 1 -0.1035 0.4927 0.2440 11.00000 0.05 0.34
Q16 1 0.0581 -0.2327 0.2966 11.00000 0.05 0.34
Q17 1 0.2771 0.3823 0.5325 11.00000 0.05 0.34
Q18 1 0.7162 0.6335 0.9160 11.00000 0.05 0.33
Q19 1 0.6003 0.5218 0.7989 11.00000 0.05 0.33
Q20 1 0.2147 0.5339 0.7344 11.00000 0.05 0.33
;
_shelx_res_checksum 74782
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 0.39367(2) 0.48998(2) 0.65240(2) 0.01837(6) Uani d 1 . .
O O2 0.6369(3) 1.0467(2) 0.92236(17) 0.0283(5) Uani d 1 . .
O O3 0.8608(3) 0.5175(2) 1.08618(16) 0.0275(4) Uani d 1 . .
O O4 0.7828(3) 0.3099(2) 1.02383(17) 0.0296(5) Uani d 1 . .
O O1 0.4709(3) 1.0748(2) 0.78321(19) 0.0346(5) Uani d 1 . .
N N1 0.2416(3) 0.3150(3) 0.50366(19) 0.0227(5) Uani d 1 . .
N N2 0.0925(3) 0.0008(3) 0.29720(19) 0.0192(5) Uani d 1 . .
N N3 0.5626(3) 0.9924(3) 0.85229(19) 0.0225(5) Uani d 1 . .
N N4 0.7850(3) 0.4544(3) 1.02106(19) 0.0209(5) Uani d 1 . .
C C5 0.1385(3) 0.1016(3) 0.3650(2) 0.0159(5) Uani d 1 . .
C C10 0.5159(3) 0.5906(3) 0.7724(2) 0.0163(5) Uani d 1 . .
C C15 0.6085(3) 0.4906(3) 0.8549(2) 0.0161(5) Uani d 1 . .
H H15 0.617536 0.377528 0.857578 0.019 Uiso calc 1 . .
C C3 0.2955(4) 0.1573(3) 0.5187(2) 0.0223(6) Uani d 1 . .
H H3 0.370755 0.118433 0.577767 0.027 Uiso calc 1 . .
C C1 0.0823(3) 0.2664(3) 0.3493(2) 0.0189(5) Uani d 1 . .
H H1 0.007726 0.310176 0.290738 0.023 Uiso calc 1 . .
C C4 0.2489(3) 0.0479(3) 0.4543(2) 0.0207(5) Uani d 1 . .
H H4 0.290598 -0.062168 0.469952 0.025 Uiso calc 1 . .
C C6 0.1261(4) -0.1737(3) 0.3195(2) 0.0227(6) Uani d 1 . .
H H6A 0.103579 -0.212086 0.398760 0.027 Uiso calc 1 . .
H H6B 0.245087 -0.210446 0.299989 0.027 Uiso calc 1 . .
C C11 0.5032(3) 0.7561(3) 0.7701(2) 0.0174(5) Uani d 1 . .
H H11 0.441806 0.825365 0.713548 0.021 Uiso calc 1 . .
C C12 0.5819(3) 0.8174(3) 0.8518(2) 0.0174(5) Uani d 1 . .
C C14 0.6874(3) 0.5607(3) 0.9333(2) 0.0173(5) Uani d 1 . .
C C2 0.1363(3) 0.3640(3) 0.4197(2) 0.0213(6) Uani d 1 . .
H H2 0.095426 0.474592 0.407427 0.026 Uiso calc 1 . .
C C13 0.6760(3) 0.7230(3) 0.9350(2) 0.0191(5) Uani d 1 . .
H H13 0.729706 0.768028 0.989943 0.023 Uiso calc 1 . .
C C7 0.0035(4) -0.2332(4) 0.2450(2) 0.0283(6) Uani d 1 . .
H H7A 0.056018 -0.330624 0.214921 0.034 Uiso calc 1 . .
H H7B -0.101840 -0.257661 0.286700 0.034 Uiso calc 1 . .
C C8 -0.0334(4) -0.0957(4) 0.1520(2) 0.0285(6) Uani d 1 . .
H H8A 0.053908 -0.100886 0.091809 0.034 Uiso calc 1 . .
H H8B -0.146104 -0.097701 0.120528 0.034 Uiso calc 1 . .
C C9 -0.0290(4) 0.0531(4) 0.2081(2) 0.0256(6) Uani d 1 . .
H H9A 0.010003 0.141619 0.155250 0.031 Uiso calc 1 . .
H H9B -0.142273 0.088875 0.238628 0.031 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 0.02050(9) 0.02056(9) 0.01580(9) -0.00533(6) -0.00338(6) -0.00528(6)
O2 0.0354(12) 0.0230(10) 0.0305(11) -0.0106(9) -0.0011(9) -0.0109(9)
O3 0.0299(11) 0.0341(11) 0.0204(10) -0.0045(9) -0.0075(8) -0.0076(9)
O4 0.0407(12) 0.0213(10) 0.0257(11) 0.0004(9) -0.0106(9) -0.0003(8)
O1 0.0449(14) 0.0203(10) 0.0383(13) -0.0011(10) -0.0136(11) -0.0015(9)
N1 0.0267(13) 0.0237(12) 0.0204(12) -0.0061(10) -0.0014(9) -0.0089(10)
N2 0.0217(11) 0.0183(11) 0.0183(11) -0.0015(9) -0.0070(9) -0.0044(9)
N3 0.0264(12) 0.0165(11) 0.0258(13) -0.0042(9) 0.0002(10) -0.0056(10)
N4 0.0203(11) 0.0249(12) 0.0175(11) -0.0008(9) -0.0019(9) -0.0038(9)
C5 0.0156(12) 0.0175(12) 0.0156(12) -0.0027(10) 0.0004(10) -0.0045(10)
C10 0.0152(12) 0.0207(12) 0.0146(12) -0.0046(10) 0.0006(9) -0.0066(10)
C15 0.0170(12) 0.0165(12) 0.0157(12) -0.0038(10) 0.0018(9) -0.0045(10)
C3 0.0222(14) 0.0278(14) 0.0182(13) -0.0031(11) -0.0057(11) -0.0055(11)
C1 0.0199(13) 0.0190(13) 0.0175(13) -0.0004(10) -0.0020(10) -0.0030(10)
C4 0.0199(13) 0.0221(13) 0.0195(13) 0.0008(11) -0.0052(10) -0.0022(11)
C6 0.0305(15) 0.0175(13) 0.0216(14) -0.0053(11) -0.0051(11) -0.0046(11)
C11 0.0174(13) 0.0219(13) 0.0130(12) -0.0039(10) 0.0006(10) -0.0012(10)
C12 0.0197(13) 0.0133(12) 0.0204(13) -0.0040(10) 0.0035(10) -0.0061(10)
C14 0.0170(12) 0.0208(13) 0.0145(12) -0.0014(10) -0.0007(10) -0.0039(10)
C2 0.0244(14) 0.0169(13) 0.0227(14) -0.0027(11) 0.0027(11) -0.0035(11)
C13 0.0193(13) 0.0219(13) 0.0181(13) -0.0061(10) -0.0009(10) -0.0066(10)
C7 0.0324(16) 0.0304(15) 0.0265(15) -0.0126(13) 0.0002(12) -0.0123(13)
C8 0.0247(15) 0.0373(17) 0.0263(16) -0.0060(13) -0.0058(12) -0.0104(13)
C9 0.0252(15) 0.0287(15) 0.0241(15) -0.0002(12) -0.0098(12) -0.0076(12)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 '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 N1 C3 . . 115.5(2) ?
C5 N2 C6 . . 123.9(2) ?
C5 N2 C9 . . 122.4(2) ?
C6 N2 C9 . . 112.3(2) ?
O1 N3 O2 . . 123.7(2) ?
O1 N3 C12 . . 117.8(2) ?
O2 N3 C12 . . 118.5(2) ?
O4 N4 O3 . . 124.9(2) ?
O4 N4 C14 . . 117.5(2) ?
O3 N4 C14 . . 117.6(2) ?
N2 C5 C1 . . 122.0(2) ?
N2 C5 C4 . . 121.9(2) ?
C1 C5 C4 . . 116.1(2) ?
C11 C10 C15 . . 120.1(2) ?
C11 C10 I1 . . 120.25(19) ?
C15 C10 I1 . . 119.66(18) ?
C14 C15 C10 . . 118.3(2) ?
C14 C15 H15 . . 120.8 ?
C10 C15 H15 . . 120.8 ?
N1 C3 C4 . . 124.6(2) ?
N1 C3 H3 . . 117.7 ?
C4 C3 H3 . . 117.7 ?
C2 C1 C5 . . 119.4(2) ?
C2 C1 H1 . . 120.3 ?
C5 C1 H1 . . 120.3 ?
C3 C4 C5 . . 119.3(2) ?
C3 C4 H4 . . 120.3 ?
C5 C4 H4 . . 120.3 ?
N2 C6 C7 . . 104.0(2) ?
N2 C6 H6A . . 111.0 ?
C7 C6 H6A . . 111.0 ?
N2 C6 H6B . . 111.0 ?
C7 C6 H6B . . 111.0 ?
H6A C6 H6B . . 109.0 ?
C12 C11 C10 . . 118.5(2) ?
C12 C11 H11 . . 120.7 ?
C10 C11 H11 . . 120.7 ?
C11 C12 C13 . . 123.5(2) ?
C11 C12 N3 . . 118.6(2) ?
C13 C12 N3 . . 117.9(2) ?
C13 C14 C15 . . 123.4(2) ?
C13 C14 N4 . . 118.3(2) ?
C15 C14 N4 . . 118.2(2) ?
N1 C2 C1 . . 125.1(2) ?
N1 C2 H2 . . 117.5 ?
C1 C2 H2 . . 117.5 ?
C14 C13 C12 . . 116.1(2) ?
C14 C13 H13 . . 121.9 ?
C12 C13 H13 . . 121.9 ?
C8 C7 C6 . . 104.7(2) ?
C8 C7 H7A . . 110.8 ?
C6 C7 H7A . . 110.8 ?
C8 C7 H7B . . 110.8 ?
C6 C7 H7B . . 110.8 ?
H7A C7 H7B . . 108.9 ?
C9 C8 C7 . . 104.1(2) ?
C9 C8 H8A . . 110.9 ?
C7 C8 H8A . . 110.9 ?
C9 C8 H8B . . 110.9 ?
C7 C8 H8B . . 110.9 ?
H8A C8 H8B . . 109.0 ?
N2 C9 C8 . . 103.6(2) ?
N2 C9 H9A . . 111.0 ?
C8 C9 H9A . . 111.0 ?
N2 C9 H9B . . 111.0 ?
C8 C9 H9B . . 111.0 ?
H9A C9 H9B . . 109.0 ?
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 C10 . 2.106(2) ?
O2 N3 . 1.222(3) ?
O3 N4 . 1.225(3) ?
O4 N4 . 1.225(3) ?
O1 N3 . 1.221(3) ?
N1 C2 . 1.334(4) ?
N1 C3 . 1.346(4) ?
N2 C5 . 1.353(3) ?
N2 C6 . 1.464(3) ?
N2 C9 . 1.465(3) ?
N3 C12 . 1.476(3) ?
N4 C14 . 1.479(3) ?
C5 C1 . 1.407(4) ?
C5 C4 . 1.414(4) ?
C10 C11 . 1.393(4) ?
C10 C15 . 1.394(3) ?
C15 C14 . 1.393(3) ?
C15 H15 . 0.9500 ?
C3 C4 . 1.382(4) ?
C3 H3 . 0.9500 ?
C1 C2 . 1.380(4) ?
C1 H1 . 0.9500 ?
C4 H4 . 0.9500 ?
C6 C7 . 1.525(4) ?
C6 H6A . 0.9900 ?
C6 H6B . 0.9900 ?
C11 C12 . 1.382(3) ?
C11 H11 . 0.9500 ?
C12 C13 . 1.384(4) ?
C14 C13 . 1.373(4) ?
C2 H2 . 0.9500 ?
C13 H13 . 0.9500 ?
C7 C8 . 1.519(4) ?
C7 H7A . 0.9900 ?
C7 H7B . 0.9900 ?
C8 C9 . 1.518(4) ?
C8 H8A . 0.9900 ?
C8 H8B . 0.9900 ?
C9 H9A . 0.9900 ?
C9 H9B . 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
C3 H3 O1 1_545 0.95 2.61 3.499(3) 155.6 yes
C7 H7B I1 2_556 0.99 3.22 4.104(3) 149.7 yes
C8 H8A O2 2_666 0.99 2.55 3.301(4) 132.9 yes
C8 H8A O4 2_656 0.99 2.61 3.420(4) 139.5 yes
C9 H9A O4 1_454 0.99 2.61 3.186(3) 116.8 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
C6 N2 C5 C1 . . . . -170.4(3) ?
C9 N2 C5 C1 . . . . -4.8(4) ?
C6 N2 C5 C4 . . . . 11.0(4) ?
C9 N2 C5 C4 . . . . 176.6(2) ?
C11 C10 C15 C14 . . . . -0.4(4) ?
I1 C10 C15 C14 . . . . -179.76(18) ?
C2 N1 C3 C4 . . . . -0.1(4) ?
N2 C5 C1 C2 . . . . -178.6(2) ?
C4 C5 C1 C2 . . . . 0.1(4) ?
N1 C3 C4 C5 . . . . 0.7(4) ?
N2 C5 C4 C3 . . . . 178.1(3) ?
C1 C5 C4 C3 . . . . -0.6(4) ?
C5 N2 C6 C7 . . . . 161.7(3) ?
C9 N2 C6 C7 . . . . -5.2(3) ?
C15 C10 C11 C12 . . . . -0.9(4) ?
I1 C10 C11 C12 . . . . 178.47(19) ?
C10 C11 C12 C13 . . . . 1.4(4) ?
C10 C11 C12 N3 . . . . -177.5(2) ?
O1 N3 C12 C11 . . . . 3.4(4) ?
O2 N3 C12 C11 . . . . -177.6(2) ?
O1 N3 C12 C13 . . . . -175.5(3) ?
O2 N3 C12 C13 . . . . 3.5(4) ?
C10 C15 C14 C13 . . . . 1.3(4) ?
C10 C15 C14 N4 . . . . 179.8(2) ?
O4 N4 C14 C13 . . . . 174.3(2) ?
O3 N4 C14 C13 . . . . -5.0(4) ?
O4 N4 C14 C15 . . . . -4.2(4) ?
O3 N4 C14 C15 . . . . 176.4(2) ?
C3 N1 C2 C1 . . . . -0.5(4) ?
C5 C1 C2 N1 . . . . 0.5(4) ?
C15 C14 C13 C12 . . . . -0.9(4) ?
N4 C14 C13 C12 . . . . -179.3(2) ?
C11 C12 C13 C14 . . . . -0.5(4) ?
N3 C12 C13 C14 . . . . 178.4(2) ?
N2 C6 C7 C8 . . . . 24.1(3) ?
C6 C7 C8 C9 . . . . -33.9(3) ?
C5 N2 C9 C8 . . . . 177.2(2) ?
C6 N2 C9 C8 . . . . -15.7(3) ?
C7 C8 C9 N2 . . . . 30.1(3) ?