#------------------------------------------------------------------------------
#$Date: 2024-12-25 04:39:53 +0200 (Wed, 25 Dec 2024) $
#$Revision: 296968 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/57/35/1573539.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_1573539
loop_
_publ_author_name
'Slamang, Ferhan'
'Hosten, Eric Cyriel'
'Betz, Richard'
_publ_section_title
;
3-Iodoaniline
;
_journal_coeditor_code BX4032
_journal_issue 12
_journal_name_full IUCrData
_journal_paper_doi 10.1107/S2414314624012264
_journal_volume 9
_journal_year 2024
_chemical_formula_iupac 'C6 H6 I N'
_chemical_formula_moiety 'C6 H6 I N'
_chemical_formula_sum 'C6 H6 I N'
_chemical_formula_weight 219.02
_chemical_name_common 3-Iodoaniline
_chemical_name_systematic 3-Iodoaniline
_space_group_crystal_system orthorhombic
_space_group_IT_number 19
_space_group_name_Hall 'P 2ac 2ab'
_space_group_name_H-M_alt 'P 21 21 21'
_atom_sites_solution_hydrogens mixed
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_audit_creation_method SHELXL-2019/3
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_formula_units_Z 8
_cell_length_a 5.0748(3)
_cell_length_b 12.9872(8)
_cell_length_c 20.6243(12)
_cell_measurement_reflns_used 9179
_cell_measurement_temperature 200(2)
_cell_measurement_theta_max 28.27
_cell_measurement_theta_min 2.52
_cell_volume 1359.29(14)
_computing_cell_refinement
;
SAINT (Bruker, 2014)
;
_computing_data_collection
;
APEX2 (Bruker, 2014)
;
_computing_data_reduction
;
SAINT (Bruker, 2014)
;
_computing_molecular_graphics
;
ORTEP-3 for Windows (Farrugia, 2012), Mercury (Macrae et al,
2020)
;
_computing_publication_material
;
SHELXL2019/3 (Sheldrick, 2015), PLATON (Spek, 2020)
;
_computing_structure_refinement
;
SHELXL2019/3 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick 2008)
;
_diffrn_ambient_temperature 200(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type 'Bruker D8 Quest'
_diffrn_measurement_method '\f and \w scans'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0254
_diffrn_reflns_av_unetI/netI 0.0221
_diffrn_reflns_limit_h_max 6
_diffrn_reflns_limit_h_min -6
_diffrn_reflns_limit_k_max 17
_diffrn_reflns_limit_k_min 0
_diffrn_reflns_limit_l_max 27
_diffrn_reflns_limit_l_min 0
_diffrn_reflns_number 3508
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 28.288
_diffrn_reflns_theta_min 2.522
_exptl_absorpt_coefficient_mu 4.604
_exptl_absorpt_correction_T_max 0.745686
_exptl_absorpt_correction_T_min 0.280050
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
(SADABS; Krause et al., 2015)
;
_exptl_crystal_colour colourless
_exptl_crystal_density_diffrn 2.140
_exptl_crystal_description block
_exptl_crystal_F_000 816
_exptl_crystal_size_max 0.300
_exptl_crystal_size_mid 0.287
_exptl_crystal_size_min 0.220
_refine_diff_density_max 0.958
_refine_diff_density_min -1.039
_refine_ls_abs_structure_details
;
Refined as an inversion twin
;
_refine_ls_abs_structure_Flack 0.44(9)
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.250
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 158
_refine_ls_number_reflns 3379
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.250
_refine_ls_R_factor_all 0.0549
_refine_ls_R_factor_gt 0.0481
_refine_ls_shift/su_max 0.000
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+10.4557P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0772
_refine_ls_wR_factor_ref 0.0794
_reflns_number_gt 3094
_reflns_number_total 3379
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file bx4032.cif
_cod_data_source_block I
_cod_database_code 1573539
_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 0.20 0.10
2 0 0 3714.63 24.90
3 0 0 0.90 0.70
4 0 0 189.48 4.60
5 0 0 1.20 3.30
6 0 0 102.39 6.60
1 1 0 201.98 1.50
2 1 0 922.01 5.00
3 1 0 120.39 2.00
4 1 0 553.84 5.00
5 1 0 34.70 1.90
6 1 0 102.49 5.10
0 2 0 1.30 0.30
1 2 0 3.00 0.30
2 2 0 13.00 0.60
3 2 0 21.50 1.40
4 2 0 34.30 1.30
5 2 0 18.30 2.10
6 2 0 40.30 3.30
0 3 0 0.50 0.20
1 3 0 1847.32 11.90
2 3 0 215.28 2.10
3 3 0 178.08 3.10
4 3 0 224.88 3.10
5 3 0 20.10 2.10
6 3 0 53.89 4.20
0 4 0 3898.21 51.09
1 4 0 27.70 0.70
2 4 0 4318.37 22.40
3 4 0 186.28 2.90
4 4 0 54.29 1.80
5 4 0 87.09 2.60
6 4 0 158.98 11.90
0 5 0 3.80 0.60
1 5 0 115.89 1.40
2 5 0 687.43 5.00
3 5 0 1.90 0.60
4 5 0 431.16 4.50
5 5 0 22.40 2.00
6 5 0 194.08 16.90
0 6 0 45.50 2.40
1 6 0 3.90 0.50
2 6 0 11.20 1.00
3 6 0 19.80 1.60
4 6 0 12.70 1.00
5 6 0 23.40 1.90
6 6 0 41.80 12.80
0 7 0 0.10 0.40
1 7 0 1858.91 10.60
2 7 0 2.00 0.60
3 7 0 385.76 4.20
4 7 0 1.20 1.20
5 7 0 20.70 2.50
6 7 0 32.40 9.70
0 8 0 1924.11 14.60
1 8 0 111.09 2.60
2 8 0 520.65 5.60
3 8 0 433.66 4.60
4 8 0 15.20 1.60
5 8 0 192.28 8.10
6 8 0 69.69 10.80
0 9 0 12.60 2.20
1 9 0 0.40 0.70
2 9 0 238.58 3.80
3 9 0 8.90 0.90
4 9 0 274.57 6.00
5 9 0 4.90 6.90
0 10 0 66.49 3.00
1 10 0 8.40 1.40
2 10 0 16.90 1.60
3 10 0 9.40 1.60
4 10 0 23.20 3.20
5 10 0 6.70 3.70
0 11 0 0.00 1.10
1 11 0 873.91 7.60
2 11 0 31.10 1.60
3 11 0 167.38 6.20
4 11 0 14.00 3.60
5 11 0 38.10 10.50
0 12 0 241.48 4.90
1 12 0 151.38 2.90
2 12 0 69.49 3.20
3 12 0 347.57 11.80
4 12 0 0.70 4.00
0 13 0 14.00 3.10
1 13 0 54.69 2.70
2 13 0 82.39 5.90
3 13 0 11.10 5.20
4 13 0 65.19 6.60
0 14 0 49.00 4.00
1 14 0 1.20 3.80
2 14 0 61.89 6.40
3 14 0 4.90 10.00
0 15 0 0.00 4.20
1 15 0 188.58 7.30
2 15 0 42.30 7.40
3 15 0 32.60 6.10
0 16 0 0.60 7.80
1 16 0 36.10 6.10
2 16 0 46.40 9.90
0 17 0 286.67 38.70
1 17 0 25.10 6.60
-6 0 1 160.38 7.80
-5 0 1 0.70 2.90
-4 0 1 554.34 7.20
-3 0 1 5.10 0.80
-2 0 1 843.02 6.90
-1 0 1 1.80 0.20
1 0 1 1.80 0.20
2 0 1 826.52 6.20
3 0 1 4.00 0.90
4 0 1 531.55 6.90
5 0 1 1.20 1.90
6 0 1 162.68 9.10
-6 1 1 65.89 3.60
-5 1 1 70.39 2.30
-4 1 1 456.15 4.90
-3 1 1 570.64 4.50
-2 1 1 969.90 5.40
-1 1 1 208.08 1.50
0 1 1 0.10 0.10
1 1 1 198.48 1.50
2 1 1 955.20 5.20
3 1 1 579.44 5.00
4 1 1 423.06 4.10
5 1 1 82.69 2.70
6 1 1 72.69 4.50
-6 2 1 9.80 3.10
-5 2 1 392.56 5.60
-4 2 1 2.00 0.80
-3 2 1 872.41 5.70
-2 2 1 346.77 2.60
-1 2 1 248.18 1.90
0 2 1 1.30 0.10
1 2 1 249.88 1.80
2 2 1 342.27 2.90
3 2 1 883.21 7.20
4 2 1 3.00 0.90
5 2 1 408.06 5.70
6 2 1 15.90 3.10
-6 3 1 49.50 3.70
-5 3 1 142.19 3.70
-4 3 1 132.99 2.50
-3 3 1 503.25 4.80
-2 3 1 174.78 1.90
-1 3 1 1335.07 7.30
0 3 1 104.99 1.10
1 3 1 1357.16 7.20
2 3 1 183.58 2.50
3 3 1 514.55 5.80
4 3 1 124.79 2.30
5 3 1 160.28 4.00
6 3 1 6.50 4.00
-6 4 1 162.08 8.60
-5 4 1 8.90 1.60
-4 4 1 508.15 4.90
-3 4 1 33.80 1.20
-2 4 1 338.07 3.90
-1 4 1 144.99 1.40
0 4 1 17.10 0.70
1 4 1 142.19 1.50
2 4 1 340.87 3.60
3 4 1 29.50 1.20
4 4 1 551.24 5.60
5 4 1 11.50 1.40
6 4 1 141.69 10.20
-6 5 1 121.89 16.60
-5 5 1 2.20 1.50
-4 5 1 411.56 4.50
-3 5 1 39.70 1.10
-2 5 1 1158.78 7.30
-1 5 1 230.68 2.20
0 5 1 826.82 5.10
1 5 1 223.48 2.10
2 5 1 1173.08 8.10
3 5 1 43.50 1.30
4 5 1 414.36 4.70
5 5 1 1.90 1.90
6 5 1 82.89 15.30
-6 6 1 26.00 12.10
-5 6 1 298.57 5.20
-4 6 1 12.40 0.90
-3 6 1 525.55 4.50
-2 6 1 255.47 3.00
-1 6 1 169.88 2.00
0 6 1 1426.56 7.50
1 6 1 168.08 2.10
2 6 1 245.58 2.80
3 6 1 603.94 5.10
4 6 1 14.20 1.40
5 6 1 310.17 5.90
6 6 1 22.50 10.50
-6 7 1 8.50 8.90
-5 7 1 146.29 4.80
-4 7 1 3.00 1.00
-3 7 1 493.95 4.50
-2 7 1 22.00 0.90
-1 7 1 706.93 5.70
0 7 1 0.30 0.50
1 7 1 665.93 4.90
2 7 1 25.60 0.70
3 7 1 518.85 5.10
4 7 1 2.90 1.10
5 7 1 152.38 5.30
6 7 1 60.99 12.90
-5 8 1 12.10 2.70
-4 8 1 190.08 3.10
-3 8 1 92.09 2.30
-2 8 1 240.18 3.00
-1 8 1 483.75 4.90
0 8 1 38.40 1.60
1 8 1 502.25 4.50
2 8 1 216.68 2.60
3 8 1 76.49 1.80
4 8 1 200.18 3.90
5 8 1 16.00 3.50
-5 9 1 11.00 3.20
-4 9 1 312.57 5.70
-3 9 1 3.00 1.30
-2 9 1 423.56 5.80
-1 9 1 2.80 0.50
0 9 1 450.35 4.20
1 9 1 3.50 0.70
2 9 1 426.86 4.80
3 9 1 0.40 0.80
4 9 1 333.77 6.10
5 9 1 2.10 3.60
-5 10 1 80.69 5.10
-4 10 1 36.50 3.30
-3 10 1 191.18 3.90
-2 10 1 285.97 3.80
-1 10 1 44.00 1.90
0 10 1 677.73 5.60
1 10 1 50.89 1.60
2 10 1 277.67 3.90
3 10 1 181.78 4.10
4 10 1 15.00 4.50
5 10 1 83.39 5.90
-5 11 1 80.99 9.30
-4 11 1 16.80 3.20
-3 11 1 276.57 8.40
-2 11 1 16.00 1.30
-1 11 1 333.67 5.80
0 11 1 9.90 1.00
1 11 1 306.47 4.40
2 11 1 17.40 1.30
3 11 1 256.07 8.20
4 11 1 9.10 4.50
5 11 1 118.59 11.20
-4 12 1 44.90 5.30
-3 12 1 79.49 5.80
-2 12 1 28.20 2.50
-1 12 1 377.56 4.60
0 12 1 8.00 1.20
1 12 1 378.56 4.00
2 12 1 15.30 1.80
3 12 1 77.09 6.70
4 12 1 17.40 7.00
-4 13 1 80.69 9.40
-3 13 1 7.80 4.80
-2 13 1 157.18 10.60
-1 13 1 113.99 3.30
0 13 1 74.09 3.40
1 13 1 89.39 2.70
2 13 1 130.19 5.30
3 13 1 6.30 6.40
4 13 1 92.79 7.40
-3 14 1 22.30 5.70
-2 14 1 179.68 9.30
-1 14 1 1.50 3.30
0 14 1 251.37 4.60
1 14 1 3.00 1.90
2 14 1 175.08 9.70
3 14 1 4.90 4.10
-3 15 1 48.80 5.90
-2 15 1 19.80 4.60
-1 15 1 73.29 7.30
0 15 1 142.59 6.70
1 15 1 54.69 4.50
2 15 1 22.60 4.60
3 15 1 30.10 6.10
-1 16 1 161.78 9.60
0 16 1 6.70 5.20
1 16 1 103.19 7.80
2 16 1 72.49 48.50
-1 17 1 114.29 9.40
0 17 1 0.00 10.10
1 17 1 77.39 10.40
-6 0 2 35.50 5.50
-5 0 2 14.80 1.80
-4 0 2 20.30 2.30
-3 0 2 38.60 1.50
-2 0 2 87.59 2.00
-1 0 2 0.30 0.10
0 0 2 0.20 0.10
1 0 2 0.40 0.10
2 0 2 88.79 1.70
3 0 2 37.00 1.60
4 0 2 19.70 3.50
5 0 2 18.20 2.80
6 0 2 66.69 5.90
-6 1 2 65.89 3.80
-5 1 2 166.88 3.30
-4 1 2 35.00 1.70
-3 1 2 725.23 5.50
-2 1 2 620.64 4.20
-1 1 2 43.90 0.60
0 1 2 1339.67 8.50
1 1 2 43.50 0.60
2 1 2 607.24 3.70
3 1 2 729.13 5.30
4 1 2 20.70 1.30
5 1 2 170.68 3.60
6 1 2 80.99 4.90
-6 2 2 15.70 3.10
-5 2 2 25.80 2.20
-4 2 2 62.59 1.70
-3 2 2 968.80 8.00
-2 2 2 8.80 0.50
-1 2 2 9999.00 47.70
0 2 2 4.00 0.20
1 2 2 9821.12 58.99
2 2 2 9.10 0.60
3 2 2 952.30 7.50
4 2 2 66.89 1.80
5 2 2 22.80 2.10
6 2 2 11.20 5.00
-6 3 2 46.40 5.30
-5 3 2 304.47 5.20
-4 3 2 6.90 1.10
-3 3 2 571.44 5.50
-2 3 2 104.39 1.50
-1 3 2 850.01 4.30
0 3 2 290.77 1.90
1 3 2 877.61 5.20
2 3 2 108.99 1.70
3 3 2 557.14 6.00
4 3 2 3.80 1.20
5 3 2 294.97 5.70
6 3 2 63.99 6.10
-6 4 2 21.90 5.40
-5 4 2 19.70 1.80
-4 4 2 22.20 1.60
-3 4 2 15.00 0.80
-2 4 2 56.99 1.40
-1 4 2 84.79 1.00
0 4 2 199.18 1.70
1 4 2 87.49 1.20
2 4 2 68.49 1.80
3 4 2 12.60 1.10
4 4 2 15.10 1.70
5 4 2 28.90 1.90
6 4 2 17.80 8.00
-6 5 2 47.90 13.40
-5 5 2 35.60 2.20
-4 5 2 38.70 1.70
-3 5 2 36.90 1.20
-2 5 2 1129.89 7.50
-1 5 2 180.98 1.70
0 5 2 2446.06 10.20
1 5 2 178.38 1.90
2 5 2 1130.89 7.50
3 5 2 37.50 1.50
4 5 2 31.20 1.60
5 5 2 36.00 2.10
6 5 2 36.40 12.20
-6 6 2 109.79 14.90
-5 6 2 33.60 2.60
-4 6 2 267.87 3.50
-3 6 2 465.75 4.50
-2 6 2 360.86 3.40
-1 6 2 3024.20 14.50
0 6 2 4.40 0.40
1 6 2 3004.40 14.50
2 6 2 342.17 3.70
3 6 2 491.35 5.50
4 6 2 275.37 4.00
5 6 2 36.10 2.70
6 6 2 62.19 12.00
-6 7 2 45.60 9.30
-5 7 2 200.98 7.60
-4 7 2 16.80 1.10
-3 7 2 486.85 4.80
-2 7 2 0.30 0.50
-1 7 2 108.39 1.90
0 7 2 5.30 0.50
1 7 2 105.69 1.80
2 7 2 1.10 0.60
3 7 2 523.25 5.10
4 7 2 16.20 1.40
5 7 2 210.48 7.70
6 7 2 7.40 7.10
-5 8 2 29.80 3.30
-4 8 2 18.20 1.40
-3 8 2 2.50 0.90
-2 8 2 31.60 1.20
-1 8 2 45.90 1.40
0 8 2 1.90 0.80
1 8 2 38.60 1.30
2 8 2 28.90 1.40
3 8 2 0.60 0.90
4 8 2 12.80 2.30
5 8 2 24.80 4.80
-5 9 2 12.60 3.50
-4 9 2 42.30 2.30
-3 9 2 2.90 1.00
-2 9 2 676.33 6.60
-1 9 2 6.30 0.60
0 9 2 1791.02 11.10
1 9 2 2.30 0.90
2 9 2 636.74 5.50
3 9 2 3.20 0.90
4 9 2 37.50 2.40
5 9 2 7.80 3.90
-5 10 2 7.10 3.70
-4 10 2 351.46 7.90
-3 10 2 67.49 2.10
-2 10 2 356.66 4.10
-1 10 2 627.34 5.20
0 10 2 7.30 1.30
1 10 2 619.84 5.80
2 10 2 344.17 4.20
3 10 2 59.29 2.20
4 10 2 351.86 7.30
5 10 2 0.00 6.40
-5 11 2 91.99 10.20
-4 11 2 17.70 3.40
-3 11 2 206.18 6.30
-2 11 2 38.20 1.40
-1 11 2 73.29 2.50
0 11 2 23.20 1.00
1 11 2 72.49 2.30
2 11 2 25.90 1.50
3 11 2 207.38 5.30
4 11 2 12.70 3.40
5 11 2 86.89 9.10
-4 12 2 21.10 8.00
-3 12 2 9.90 3.20
-2 12 2 2.90 1.60
-1 12 2 57.89 2.30
0 12 2 12.80 1.30
1 12 2 47.10 2.20
2 12 2 1.90 1.40
3 12 2 19.30 3.50
4 12 2 1.70 4.30
-4 13 2 0.00 6.50
-3 13 2 39.70 6.10
-2 13 2 355.16 16.70
-1 13 2 26.50 1.90
0 13 2 432.46 6.70
1 13 2 17.70 2.00
2 13 2 292.37 7.60
3 13 2 57.09 3.90
4 13 2 14.10 6.10
-3 14 2 25.70 4.80
-2 14 2 199.48 9.80
-1 14 2 56.59 3.00
0 14 2 10.60 3.30
1 14 2 41.10 4.70
2 14 2 155.08 10.80
3 14 2 18.20 3.10
-3 15 2 47.80 5.80
-2 15 2 38.80 4.90
-1 15 2 28.50 5.90
0 15 2 84.49 7.20
1 15 2 31.30 3.90
2 15 2 14.70 4.00
3 15 2 37.20 4.90
-2 16 2 16.10 8.20
-1 16 2 39.70 7.00
0 16 2 7.30 4.60
1 16 2 62.99 10.30
2 16 2 14.70 6.30
-1 17 2 55.49 7.80
0 17 2 124.79 14.40
1 17 2 7.90 5.50
-6 0 3 211.48 9.60
-5 0 3 0.20 1.40
-4 0 3 1022.10 11.60
-3 0 3 0.40 0.50
-2 0 3 1123.49 7.30
-1 0 3 0.60 0.10
0 0 3 1.20 0.20
1 0 3 0.30 0.20
2 0 3 1122.79 7.50
3 0 3 0.70 0.50
4 0 3 1033.90 9.60
5 0 3 2.70 4.80
6 0 3 280.27 14.60
-6 1 3 37.80 4.50
-5 1 3 86.39 2.50
-4 1 3 181.38 2.80
-3 1 3 596.84 4.80
-2 1 3 690.43 3.80
-1 1 3 257.97 1.60
0 1 3 789.82 3.80
1 1 3 263.87 1.80
2 1 3 684.93 3.60
3 1 3 590.84 4.20
4 1 3 186.08 2.90
5 1 3 86.49 2.90
6 1 3 46.50 5.80
-6 2 3 13.40 3.90
-5 2 3 263.87 4.10
-4 2 3 3.80 0.90
-3 2 3 687.83 6.00
-2 2 3 53.39 0.90
-1 2 3 83.89 0.80
0 2 3 234.78 1.90
1 2 3 87.59 1.00
2 2 3 54.69 1.00
3 2 3 663.53 4.80
4 2 3 0.90 0.70
5 2 3 286.17 5.20
6 2 3 24.90 5.60
-6 3 3 36.80 5.20
-5 3 3 272.97 5.00
-4 3 3 72.49 1.80
-3 3 3 746.83 6.30
-2 3 3 413.86 3.10
-1 3 3 1469.55 6.20
0 3 3 392.46 2.60
1 3 3 1487.85 7.30
2 3 3 416.66 3.20
3 3 3 718.03 6.90
4 3 3 78.29 2.20
5 3 3 286.37 5.70
6 3 3 36.50 10.60
-6 4 3 215.38 9.60
-5 4 3 5.50 1.70
-4 4 3 747.63 6.90
-3 4 3 155.08 2.50
-2 4 3 896.31 5.40
-1 4 3 667.33 3.80
0 4 3 8.50 0.30
1 4 3 666.73 3.80
2 4 3 900.01 6.20
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1 2 23 20.60 2.20
2 2 23 3.20 1.40
3 2 23 34.30 3.70
-3 3 23 40.60 4.00
-2 3 23 43.70 3.20
-1 3 23 28.10 2.90
0 3 23 31.00 2.80
1 3 23 33.50 2.30
2 3 23 39.50 2.90
3 3 23 56.49 4.10
-3 4 23 15.40 3.70
-2 4 23 86.49 4.20
-1 4 23 31.80 2.50
0 4 23 1.70 1.20
1 4 23 28.90 1.90
2 4 23 86.49 3.20
3 4 23 16.20 2.70
-3 5 23 5.70 2.60
-2 5 23 66.59 4.20
-1 5 23 1.00 1.70
0 5 23 119.19 3.50
1 5 23 1.90 1.20
2 5 23 50.29 3.80
3 5 23 3.00 2.00
-2 6 23 9.20 2.30
-1 6 23 7.50 2.00
0 6 23 17.50 1.90
1 6 23 8.80 1.60
2 6 23 6.60 1.50
-2 7 23 5.60 1.90
-1 7 23 28.00 3.20
0 7 23 19.30 2.10
1 7 23 31.60 2.80
2 7 23 7.60 1.60
-2 8 23 37.40 10.10
-1 8 23 104.09 4.50
0 8 23 2.50 1.70
1 8 23 86.09 4.70
2 8 23 29.30 6.90
-1 9 23 7.00 2.50
0 9 23 52.59 3.70
1 9 23 4.90 3.30
-3 0 24 5.10 2.70
-2 0 24 13.20 2.60
-1 0 24 1.00 2.70
0 0 24 24.70 3.80
1 0 24 7.60 1.80
2 0 24 15.00 3.40
3 0 24 28.30 9.40
-3 1 24 26.00 3.50
-2 1 24 33.40 3.10
-1 1 24 4.20 1.30
0 1 24 83.99 3.90
1 1 24 8.10 2.00
2 1 24 33.70 3.60
3 1 24 27.80 5.30
-3 2 24 42.50 3.70
-2 2 24 2.50 1.60
-1 2 24 280.97 6.70
0 2 24 7.00 1.70
1 2 24 291.17 6.30
2 2 24 2.70 1.60
3 2 24 40.00 3.90
-3 3 24 48.80 3.90
-2 3 24 16.60 2.80
-1 3 24 17.40 2.10
0 3 24 14.20 2.10
1 3 24 10.80 2.00
2 3 24 13.20 2.10
3 3 24 39.80 3.40
-2 4 24 27.50 3.60
-1 4 24 2.90 1.50
0 4 24 7.60 1.50
1 4 24 3.00 1.70
2 4 24 13.80 2.00
-2 5 24 67.39 4.90
-1 5 24 5.60 1.90
0 5 24 182.68 4.70
1 5 24 5.30 1.60
2 5 24 57.79 4.40
-2 6 24 33.60 3.40
-1 6 24 96.09 5.20
0 6 24 13.60 1.70
1 6 24 107.89 4.60
2 6 24 35.10 2.60
-1 7 24 14.30 2.50
0 7 24 10.90 2.60
1 7 24 19.30 2.80
-1 8 24 3.70 2.10
0 8 24 4.00 3.00
1 8 24 2.60 1.90
-2 0 25 64.49 5.40
-1 0 25 19.90 4.40
0 0 25 8.80 2.20
1 0 25 1.80 2.10
2 0 25 46.10 7.30
-2 1 25 20.20 3.40
-1 1 25 33.90 3.10
0 1 25 18.00 1.60
1 1 25 20.00 2.80
2 1 25 23.50 4.10
-2 2 25 9.50 3.20
-1 2 25 14.10 1.80
0 2 25 7.10 1.60
1 2 25 19.20 2.90
2 2 25 8.60 2.70
-2 3 25 1.70 3.30
-1 3 25 73.79 3.80
0 3 25 5.80 2.30
1 3 25 71.09 3.20
2 3 25 18.70 2.60
-2 4 25 8.70 2.60
-1 4 25 12.80 2.20
0 4 25 5.70 1.90
1 4 25 13.90 2.50
2 4 25 16.20 2.20
-2 5 25 32.60 4.90
-1 5 25 8.30 2.80
0 5 25 19.50 2.70
1 5 25 20.20 2.60
2 5 25 26.60 3.30
-1 6 25 8.90 3.00
0 6 25 31.60 3.30
1 6 25 9.50 2.30
0 7 25 4.70 2.50
-2 0 26 100.39 8.30
-1 0 26 5.10 3.40
0 0 26 309.87 13.00
1 0 26 4.60 4.20
2 0 26 84.39 14.70
-2 1 26 27.70 3.70
-1 1 26 14.90 3.20
0 1 26 1.00 2.50
1 1 26 22.10 3.60
2 1 26 22.80 4.80
-2 2 26 8.70 2.00
-1 2 26 4.10 3.80
0 2 26 5.80 3.90
1 2 26 10.30 4.50
2 2 26 2.10 3.60
-1 3 26 99.29 4.70
0 3 26 14.60 5.40
1 3 26 71.29 5.40
-1 4 26 11.90 2.60
0 4 26 162.98 8.80
1 4 26 8.60 2.10
-1 5 26 8.90 3.00
0 5 26 2.50 2.10
1 5 26 6.50 3.20
-1 0 27 19.50 4.20
0 0 27 6.60 3.40
1 0 27 14.50 6.80
-1 1 27 13.70 2.40
0 1 27 26.60 3.50
1 1 27 13.60 3.50
-1 2 27 20.70 4.00
0 2 27 12.90 3.60
1 2 27 21.40 4.90
0 3 27 17.20 4.90
0 0 0 0.00 0.00
_computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)'
;
_shelx_hkl_checksum 825
_shelx_res_file
;
TITL bq203_Pbca_a.res in P2(1)2(1)2(1)
bq203.res
created by SHELXL-2019/3 at 16:37:00 on 09-Nov-2024
CELL 0.71073 5.0748 12.9872 20.6243 90.000 90.000 90.000
ZERR 8.000 0.0003 0.0008 0.0012 0.000 0.000 0.000
LATT -1
SYMM 1/2-X, -Y, 1/2+Z
SYMM -X, 1/2+Y, 1/2-Z
SYMM 1/2+X, 1/2-Y, -Z
SFAC C H I N
UNIT 48 48 8 8
ACTA
BOND $H
CONF
HTAB
TEMP -73.150
OMIT 0 1 1
OMIT 0 0 2
OMIT 0 4 0
OMIT -6 4 6
OMIT -6 3 1
EQIV $1 x+1, y, z
HTAB N1 N2
HTAB N2 N1_$1
TWIN
MPLA C11 C12 C13 C14 C15 C16
MPLA C21 C22 C23 C24 C25 C26
L.S. 50
FMAP 2
PLAN -5
WGHT 0.000000 10.455700
BASF 0.44448
FVAR 0.23835
I1 3 -0.299540 0.231850 0.366942 11.00000 0.02826 0.02771 =
0.03565 0.00217 0.00435 0.00174
I2 3 0.190291 1.012079 0.364769 11.00000 0.02728 0.02533 =
0.03774 0.00207 0.00219 0.00139
N1 4 0.311194 0.551655 0.285908 11.00000 0.02946 0.03605 =
0.04890 0.00420 0.00445 -0.01094
H711 2 0.445646 0.581008 0.283037 11.00000 -1.50000
H712 2 0.285202 0.522742 0.245649 11.00000 -1.50000
N2 4 0.811007 0.696139 0.282380 11.00000 0.04262 0.02596 =
0.03744 -0.00417 0.00438 0.00190
H721 2 0.790604 0.718093 0.244273 11.00000 -1.50000
H722 2 0.945821 0.660128 0.287755 11.00000 -1.50000
C11 1 0.245671 0.485574 0.336687 11.00000 0.02743 0.02612 =
0.04920 -0.00472 -0.00464 0.00405
C12 1 0.054759 0.409821 0.328585 11.00000 0.02891 0.03229 =
0.02111 -0.00127 -0.00293 0.00250
AFIX 43
H12 2 -0.025586 0.399800 0.287462 11.00000 -1.20000
AFIX 0
C13 1 -0.017102 0.349405 0.380570 11.00000 0.02486 0.02815 =
0.03221 -0.00091 -0.00199 0.00107
C14 1 0.095918 0.360389 0.441487 11.00000 0.03761 0.04578 =
0.02693 0.00211 0.00207 0.00729
AFIX 43
H14 2 0.044405 0.317533 0.476599 11.00000 -1.20000
AFIX 0
C15 1 0.284799 0.435276 0.449383 11.00000 0.04143 0.04776 =
0.03072 -0.01042 -0.01242 0.00745
AFIX 43
H15 2 0.365993 0.444220 0.490503 11.00000 -1.20000
AFIX 0
C16 1 0.358900 0.498606 0.397383 11.00000 0.03036 0.03205 =
0.04294 -0.01475 0.00602 -0.01377
AFIX 43
H16 2 0.487506 0.550785 0.403765 11.00000 -1.20000
AFIX 0
C21 1 0.740230 0.758826 0.335057 11.00000 0.01516 0.03551 =
0.03591 0.00579 -0.00199 -0.01263
C22 1 0.547513 0.835596 0.324913 11.00000 0.02528 0.02797 =
0.02686 0.00569 -0.00990 -0.00221
AFIX 43
H22 2 0.474817 0.847272 0.283107 11.00000 -1.20000
AFIX 0
C23 1 0.467704 0.893459 0.378003 11.00000 0.01216 0.02343 =
0.03293 0.00160 0.00484 -0.00388
C24 1 0.567832 0.877921 0.439500 11.00000 0.03847 0.03216 =
0.02416 -0.00078 0.00457 -0.00001
AFIX 43
H24 2 0.507738 0.917882 0.475135 11.00000 -1.20000
AFIX 0
C25 1 0.756514 0.803227 0.447848 11.00000 0.04020 0.03771 =
0.02758 0.00394 -0.00025 -0.00167
AFIX 43
H25 2 0.827830 0.792069 0.489853 11.00000 -1.20000
AFIX 0
C26 1 0.845600 0.743624 0.396415 11.00000 0.02293 0.03622 =
0.03743 0.01304 -0.00460 -0.00329
AFIX 43
H26 2 0.977570 0.692867 0.403175 11.00000 -1.20000
AFIX 0
HKLF 4
REM bq203_Pbca_a.res in P2(1)2(1)2(1)
REM wR2 = 0.0794, GooF = S = 1.250, Restrained GooF = 1.250 for all data
REM R1 = 0.0481 for 3094 Fo > 4sig(Fo) and 0.0549 for all 3379 data
REM 158 parameters refined using 0 restraints
END
WGHT 0.0000 10.4559
REM Instructions for potential hydrogen bonds
HTAB N1 N2
EQIV $2 -x, y-1/2, -z+1/2
HTAB N1 I2_$2
HTAB N2 N1_$1
REM Highest difference peak 0.958, deepest hole -1.039, 1-sigma level 0.153
Q1 1 -0.1831 0.2753 0.3818 11.00000 0.05 0.96
Q2 1 0.3386 1.0324 0.3636 11.00000 0.05 0.89
Q3 1 0.2870 0.9950 0.3280 11.00000 0.05 0.89
Q4 1 0.5188 1.0342 0.3766 11.00000 0.05 0.85
Q5 1 0.3337 1.0065 0.3873 11.00000 0.05 0.85
;
_shelx_res_checksum 99256
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
I I1 -0.29954(15) 0.23185(5) 0.36694(4) 0.03054(16) Uani d 1 . .
I I2 0.19029(13) 1.01208(5) 0.36477(4) 0.03011(16) Uani d 1 . .
N N1 0.311(2) 0.5517(8) 0.2859(5) 0.038(2) Uani d 1 . .
H H711 0.45(3) 0.581(12) 0.283(7) 0.057 Uiso d 1 . .
H H712 0.29(3) 0.523(10) 0.246(6) 0.057 Uiso d 1 . .
N N2 0.811(2) 0.6961(7) 0.2824(5) 0.035(2) Uani d 1 . .
H H721 0.79(3) 0.718(10) 0.244(6) 0.053 Uiso d 1 . .
H H722 0.95(3) 0.660(12) 0.288(7) 0.053 Uiso d 1 . .
C C11 0.246(2) 0.4856(8) 0.3367(5) 0.034(3) Uani d 1 . .
C C12 0.055(2) 0.4098(8) 0.3286(5) 0.027(2) Uani d 1 . .
H H12 -0.025586 0.399800 0.287462 0.033 Uiso calc 1 . .
C C13 -0.017(2) 0.3494(8) 0.3806(5) 0.028(2) Uani d 1 . .
C C14 0.096(2) 0.3604(10) 0.4415(5) 0.037(3) Uani d 1 . .
H H14 0.044405 0.317533 0.476599 0.044 Uiso calc 1 . .
C C15 0.285(3) 0.4353(9) 0.4494(5) 0.040(3) Uani d 1 . .
H H15 0.365993 0.444220 0.490503 0.048 Uiso calc 1 . .
C C16 0.359(2) 0.4986(9) 0.3974(5) 0.035(3) Uani d 1 . .
H H16 0.487506 0.550785 0.403765 0.042 Uiso calc 1 . .
C C21 0.7402(19) 0.7588(8) 0.3351(5) 0.029(2) Uani d 1 . .
C C22 0.548(2) 0.8356(8) 0.3249(5) 0.027(2) Uani d 1 . .
H H22 0.474817 0.847272 0.283107 0.032 Uiso calc 1 . .
C C23 0.4677(17) 0.8935(7) 0.3780(5) 0.023(2) Uani d 1 . .
C C24 0.568(2) 0.8779(8) 0.4395(5) 0.032(2) Uani d 1 . .
H H24 0.507738 0.917882 0.475135 0.038 Uiso calc 1 . .
C C25 0.757(2) 0.8032(8) 0.4478(5) 0.035(3) Uani d 1 . .
H H25 0.827830 0.792069 0.489853 0.042 Uiso calc 1 . .
C C26 0.846(2) 0.7436(9) 0.3964(5) 0.032(3) Uani d 1 . .
H H26 0.977570 0.692867 0.403175 0.039 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 0.0283(3) 0.0277(3) 0.0356(3) 0.0017(3) 0.0044(4) 0.0022(3)
I2 0.0273(3) 0.0253(3) 0.0377(3) 0.0014(3) 0.0022(4) 0.0021(3)
N1 0.029(5) 0.036(5) 0.049(6) -0.011(5) 0.004(5) 0.004(4)
N2 0.043(6) 0.026(5) 0.037(5) 0.002(5) 0.004(5) -0.004(4)
C11 0.027(7) 0.026(5) 0.049(6) 0.004(5) -0.005(5) -0.005(5)
C12 0.029(6) 0.032(6) 0.021(5) 0.003(5) -0.003(4) -0.001(4)
C13 0.025(5) 0.028(5) 0.032(6) 0.001(4) -0.002(4) -0.001(4)
C14 0.038(7) 0.046(7) 0.027(5) 0.007(6) 0.002(5) 0.002(5)
C15 0.041(7) 0.048(7) 0.031(5) 0.007(6) -0.012(5) -0.010(5)
C16 0.030(6) 0.032(6) 0.043(6) -0.014(5) 0.006(5) -0.015(5)
C21 0.015(6) 0.036(6) 0.036(5) -0.013(5) -0.002(4) 0.006(4)
C22 0.025(6) 0.028(5) 0.027(5) -0.002(5) -0.010(4) 0.006(4)
C23 0.012(4) 0.023(5) 0.033(5) -0.004(4) 0.005(4) 0.002(4)
C24 0.038(6) 0.032(6) 0.024(5) 0.000(5) 0.005(5) -0.001(4)
C25 0.040(8) 0.038(6) 0.028(5) -0.002(5) 0.000(5) 0.004(4)
C26 0.023(6) 0.036(6) 0.037(5) -0.003(5) -0.005(5) 0.013(5)
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'
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
C11 N1 H711 . . 124(10) ?
C11 N1 H712 . . 113(8) ?
H711 N1 H712 . . 105(10) ?
C21 N2 H721 . . 120(9) ?
C21 N2 H722 . . 116(10) ?
H721 N2 H722 . . 114(10) ?
C16 C11 C12 . . 118.9(10) ?
C16 C11 N1 . . 120.2(10) ?
C12 C11 N1 . . 120.7(10) ?
C13 C12 C11 . . 119.6(10) ?
C13 C12 H12 . . 120.2 ?
C11 C12 H12 . . 120.2 ?
C12 C13 C14 . . 122.4(11) ?
C12 C13 I1 . . 119.2(8) ?
C14 C13 I1 . . 118.3(8) ?
C15 C14 C13 . . 117.9(11) ?
C15 C14 H14 . . 121.1 ?
C13 C14 H14 . . 121.1 ?
C14 C15 C16 . . 120.7(10) ?
C14 C15 H15 . . 119.6 ?
C16 C15 H15 . . 119.6 ?
C11 C16 C15 . . 120.5(10) ?
C11 C16 H16 . . 119.8 ?
C15 C16 H16 . . 119.8 ?
C26 C21 N2 . . 121.6(10) ?
C26 C21 C22 . . 120.2(10) ?
N2 C21 C22 . . 118.2(10) ?
C23 C22 C21 . . 117.9(9) ?
C23 C22 H22 . . 121.1 ?
C21 C22 H22 . . 121.1 ?
C24 C23 C22 . . 122.5(10) ?
C24 C23 I2 . . 118.2(8) ?
C22 C23 I2 . . 119.3(7) ?
C25 C24 C23 . . 118.3(10) ?
C25 C24 H24 . . 120.8 ?
C23 C24 H24 . . 120.8 ?
C24 C25 C26 . . 121.6(10) ?
C24 C25 H25 . . 119.2 ?
C26 C25 H25 . . 119.2 ?
C21 C26 C25 . . 119.5(10) ?
C21 C26 H26 . . 120.3 ?
C25 C26 H26 . . 120.3 ?
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 C13 . 2.113(11) ?
I2 C23 . 2.105(10) ?
N1 C11 . 1.394(14) ?
N1 H711 . 0.78(15) ?
N1 H712 . 0.92(13) ?
N2 C21 . 1.404(14) ?
N2 H721 . 0.84(13) ?
N2 H722 . 0.84(15) ?
C11 C16 . 1.388(14) ?
C11 C12 . 1.391(15) ?
C12 C13 . 1.378(14) ?
C12 H12 . 0.9500 ?
C13 C14 . 1.388(15) ?
C14 C15 . 1.375(17) ?
C14 H14 . 0.9500 ?
C15 C16 . 1.403(16) ?
C15 H15 . 0.9500 ?
C16 H16 . 0.9500 ?
C21 C26 . 1.388(13) ?
C21 C22 . 1.412(15) ?
C22 C23 . 1.388(14) ?
C22 H22 . 0.9500 ?
C23 C24 . 1.381(14) ?
C24 C25 . 1.374(16) ?
C24 H24 . 0.9500 ?
C25 C26 . 1.389(15) ?
C25 H25 . 0.9500 ?
C26 H26 . 0.9500 ?
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 H711 N2 . 0.78(15) 2.38(16) 3.156(17) 170(15) yes
N2 H722 N1 1_655 0.84(15) 2.33(15) 3.157(18) 171(13) yes
C13 I1 I2 1_455 2.113(11) 3.8538(10) 8.677(10) 172.9(3) yes
C23 I2 I1 1_565 2.105(10) 3.7852(10) 9.437(9) 171.8(3) yes
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
C16 C11 C12 C13 . . . . -0.2(16) ?
N1 C11 C12 C13 . . . . -176.3(10) ?
C11 C12 C13 C14 . . . . -0.6(17) ?
C11 C12 C13 I1 . . . . -178.3(8) ?
C12 C13 C14 C15 . . . . 0.5(17) ?
I1 C13 C14 C15 . . . . 178.2(8) ?
C13 C14 C15 C16 . . . . 0.3(17) ?
C12 C11 C16 C15 . . . . 1.0(17) ?
N1 C11 C16 C15 . . . . 177.1(11) ?
C14 C15 C16 C11 . . . . -1.1(18) ?
C26 C21 C22 C23 . . . . -0.6(15) ?
N2 C21 C22 C23 . . . . 176.5(10) ?
C21 C22 C23 C24 . . . . -0.5(15) ?
C21 C22 C23 I2 . . . . 178.0(7) ?
C22 C23 C24 C25 . . . . 1.0(16) ?
I2 C23 C24 C25 . . . . -177.5(8) ?
C23 C24 C25 C26 . . . . -0.4(17) ?
N2 C21 C26 C25 . . . . -175.8(10) ?
C22 C21 C26 C25 . . . . 1.1(16) ?
C24 C25 C26 C21 . . . . -0.7(17) ?