#------------------------------------------------------------------------------
#$Date: 2024-11-01 03:55:10 +0100 (Fri, 01 Nov 2024) $
#$Revision: 295711 $
#$URL: svn://www.crystallography.net/cod/cif/2/02/32/2023298.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_2023298
loop_
_publ_author_name
'Petrosova, Hanna R.'
'Naumova, Dina D.'
'Golenya, Irina A.'
'Buta, Ildiko'
'Gural'skiy, Il'ya A.'
_publ_section_title
;
Crystal structure and Hirshfeld surface analysis of the salt
2-iodoethylammonium iodide -- a possible side product upon synthesis of
hybrid perovskites
;
_journal_coeditor_code WM5738
_journal_issue 11
_journal_name_full
'Acta Crystallographica Section E Crystallographic Communications'
_journal_page_first 1226
_journal_page_last 1229
_journal_paper_doi 10.1107/S205698902401034X
_journal_volume 80
_journal_year 2024
_chemical_formula_iupac 'C2 H7 I N +, I -'
_chemical_formula_moiety 'C2 H7 I N +, I -'
_chemical_formula_sum 'C2 H7 I2 N'
_chemical_formula_weight 298.89
_chemical_name_systematic
;
2-Iodoethylammonium iodide
;
_space_group_crystal_system monoclinic
_space_group_IT_number 14
_space_group_name_Hall '-P 2ybc'
_space_group_name_H-M_alt 'P 1 21/c 1'
_atom_sites_solution_hydrogens geom
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_cell_angle_alpha 90
_cell_angle_beta 102.004(7)
_cell_angle_gamma 90
_cell_formula_units_Z 4
_cell_length_a 8.3073(7)
_cell_length_b 8.8800(6)
_cell_length_c 9.3838(7)
_cell_measurement_reflns_used 3490
_cell_measurement_temperature 100.00(10)
_cell_measurement_theta_max 30.2520
_cell_measurement_theta_min 3.1880
_cell_volume 677.09(9)
_computing_cell_refinement
;
CrysAlisPro (Rigaku OD, 2023)
;
_computing_data_collection
;
CrysAlisPro (Rigaku OD, 2023)
;
_computing_data_reduction
;
CrysAlisPro (Rigaku OD, 2023)
;
_computing_molecular_graphics
;
Olex2 (Dolomanov et al., 2009)
;
_computing_publication_material
;
publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT (Sheldrick, 2015a)
;
_diffrn_ambient_temperature 100.15
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.795
_diffrn_measurement_device 'four-circle diffractometer'
_diffrn_measurement_device_type 'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method '\w scans'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_unetI/netI 0.0184
_diffrn_reflns_limit_h_max 10
_diffrn_reflns_limit_h_min -11
_diffrn_reflns_limit_k_max 11
_diffrn_reflns_limit_k_min -11
_diffrn_reflns_limit_l_max 12
_diffrn_reflns_limit_l_min -10
_diffrn_reflns_number 2744
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 30.381
_diffrn_reflns_theta_min 2.507
_exptl_absorpt_coefficient_mu 9.161
_exptl_absorpt_correction_T_max 0.573
_exptl_absorpt_correction_T_min 0.157
_exptl_absorpt_correction_type analytical
_exptl_absorpt_process_details
;
(CrysAlisPro; Rigaku OD, 2023)
;
_exptl_crystal_colour 'clear intense colourless'
_exptl_crystal_density_diffrn 2.932
_exptl_crystal_description plate
_exptl_crystal_F_000 528
_exptl_crystal_size_max 0.314
_exptl_crystal_size_mid 0.145
_exptl_crystal_size_min 0.074
_refine_diff_density_max 2.069
_refine_diff_density_min -1.678
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.117
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 49
_refine_ls_number_reflns 2744
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.117
_refine_ls_R_factor_all 0.0537
_refine_ls_R_factor_gt 0.0505
_refine_ls_shift/su_max 0.000
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1098P)^2^+4.1089P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1528
_refine_ls_wR_factor_ref 0.1589
_reflns_number_gt 2535
_reflns_number_total 2744
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file wm5738.cif
_cod_data_source_block I
_cod_original_cell_volume 677.10(9)
_cod_database_code 2023298
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_hkl_file
;
0 0 2 663.711 49.9977 1
0 0 4 18870.8 362.315 1
0 0 6 39510.2 456.455 1
-3 0 8 14004.7 599.568 -2
0 0 8 14004.7 599.568 1
0 0 10 1002.35 153.962 1
0 -1 1 490.421 21.2253 1
0 -1 -2 82241.0 380.571 1
0 -1 3 55648.0 292.480 1
0 -1 4 2437.56 61.3517 1
0 -1 5 10694.0 155.649 1
0 -1 6 48683.9 355.316 1
0 -1 7 11.7291 37.0758 1
-3 1 8 33704.0 913.158 -2
0 -1 8 33704.0 913.158 1
0 -1 9 3673.19 244.386 1
0 -1 10 2777.81 231.586 1
-4 1 11 4661.99 400.780 -2
0 -1 11 4661.99 400.780 1
0 2 0 44831.1 85.9334 -2
0 -2 0 44831.1 85.9334 1
0 2 1 31552.1 119.675 1
0 -2 2 109358. 310.470 1
0 2 3 11616.3 114.395 1
0 2 4 13690.8 138.841 1
0 -2 5 43885.2 299.664 1
0 -2 6 915.638 46.2430 1
0 2 7 7293.32 155.852 1
-3 2 8 11216.5 380.072 -2
0 -2 8 11216.5 380.072 1
0 -2 9 13054.3 317.532 1
0 -2 10 2673.64 155.700 1
-4 -2 11 9692.23 406.930 -2
0 2 11 9692.23 406.930 1
0 3 1 16338.5 81.2598 1
0 3 2 9467.30 94.0685 1
0 3 3 46024.0 287.176 1
-1 3 3 52700.5 540.148 -2
0 -3 3 52700.5 540.148 1
0 -3 4 100475. 343.436 1
0 -3 5 183.958 30.3681 1
-2 3 5 24591.1 486.942 -2
0 -3 5 24591.1 486.942 1
0 3 6 5707.11 110.416 1
0 -3 7 27.0676 21.1952 1
-3 -3 8 28027.5 449.161 -2
0 3 8 28027.5 449.161 1
0 3 9 194.320 50.5998 1
0 -3 10 23260.5 437.002 1
-4 3 11 4117.53 266.887 -2
0 -3 11 4117.53 266.887 1
0 4 0 4263.80 43.0375 -2
0 -4 0 4263.80 43.0375 1
0 -4 1 10785.7 53.5148 1
0 -4 2 64547.4 229.960 1
-1 -4 3 24106.2 173.494 -2
0 4 3 24106.2 173.494 1
0 -4 -4 24246.7 135.368 1
0 -4 -5 3363.28 78.7464 1
-2 4 5 6236.51 251.438 -2
0 -4 5 6236.51 251.438 1
0 -4 6 7944.30 132.489 1
0 4 7 31380.3 347.492 1
-3 4 8 14073.8 326.071 -2
0 -4 8 14073.8 326.071 1
0 -4 9 2290.47 107.284 1
0 -4 10 2590.99 151.840 1
-4 -4 11 4310.31 269.091 -2
0 4 11 4310.31 269.091 1
0 5 1 77655.5 605.929 1
0 5 2 53.6572 7.85696 1
-1 5 3 50839.4 243.343 -2
0 -5 3 50839.4 243.343 1
0 -5 4 8982.29 106.048 1
0 -5 5 35593.6 683.288 1
-2 5 5 37712.2 262.073 -2
0 -5 5 37712.2 262.073 1
0 -5 6 6338.77 98.9824 1
-2 5 6 6997.58 140.260 -2
0 -5 6 6997.58 140.260 1
0 -5 7 186.135 27.0832 1
-3 5 8 6543.93 230.192 -2
0 -5 8 6543.93 230.192 1
0 -5 9 8565.74 202.843 1
0 -5 10 3751.29 174.871 1
-4 5 11 2427.26 205.061 -2
0 -5 11 2427.26 205.061 1
0 6 0 56846.4 214.505 -2
0 -6 0 56846.4 214.505 1
0 6 1 37406.2 461.888 1
0 6 2 818.820 20.1139 1
-1 -6 3 19213.2 141.839 -2
0 6 3 19213.2 141.839 1
0 6 4 1050.93 41.4794 1
0 -6 5 5434.42 293.097 1
-2 -6 5 12360.9 179.610 -2
0 6 5 12360.9 179.610 1
0 -6 -6 7608.38 136.823 1
-2 6 6 8061.54 198.997 -2
0 -6 6 8061.54 198.997 1
0 -6 7 40214.5 398.814 1
-3 -6 8 3833.13 176.783 -2
0 6 8 3833.13 176.783 1
0 -6 9 4804.41 155.806 1
0 6 10 12.0197 32.3633 1
0 7 -1 27947.2 232.713 1
0 -7 2 15410.6 460.387 1
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0 -7 3 35432.1 179.978 1
0 -7 -4 15894.8 131.980 1
0 -7 5 5156.60 302.579 1
-2 -7 5 14482.1 170.419 -2
0 7 5 14482.1 170.419 1
-2 7 6 11024.8 166.907 -2
0 -7 6 11024.8 166.907 1
0 -7 7 312.294 45.2059 1
-3 7 8 6166.63 226.148 -2
0 -7 8 6166.63 226.148 1
0 7 9 1194.41 83.4454 1
0 7 10 2047.95 179.545 1
0 8 0 5132.93 161.301 -2
0 -8 0 5132.93 161.301 1
0 8 -1 7397.91 111.314 1
0 -8 2 2511.88 142.920 1
-1 8 3 16547.1 335.005 -2
0 -8 3 16547.1 335.005 1
0 8 4 1494.43 41.8812 1
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0 -8 5 28803.6 240.074 1
0 -8 6 4118.47 294.139 1
2 8 -6 5840.19 159.490 -2
0 -8 -6 5840.19 159.490 1
0 8 7 2820.69 136.398 1
-3 -8 8 1840.01 161.432 -2
0 8 8 1840.01 161.432 1
0 -8 9 13042.8 522.292 1
0 -9 1 4127.83 65.8825 1
0 -9 2 1212.72 109.652 1
-1 9 3 48720.2 631.226 -2
0 -9 3 48720.2 631.226 1
0 -9 4 61.3305 28.0480 1
-2 9 5 23014.7 376.430 -2
0 -9 5 23014.7 376.430 1
0 -9 6 2258.92 160.578 1
2 9 -6 2399.44 187.413 -2
0 -9 -6 2399.44 187.413 1
0 -9 7 106.265 63.6334 1
0 10 0 33522.0 1151.25 -2
0 -10 0 33522.0 1151.25 1
0 -10 1 245.188 62.6355 1
0 -10 -2 75.2488 40.0801 1
-1 10 3 3283.82 181.596 -2
0 -10 3 3283.82 181.596 1
0 -10 4 85.7434 41.1004 1
-2 10 5 13328.9 307.013 -2
0 -10 5 13328.9 307.013 1
0 -10 6 6405.74 350.572 1
0 -10 7 2222.50 213.984 1
0 -11 1 8083.74 318.905 1
0 -11 2 6860.94 292.908 1
-1 11 3 9427.16 368.037 -2
0 -11 3 9427.16 368.037 1
0 -11 4 485.150 82.0849 1
-2 11 5 4670.86 226.043 -2
0 -11 5 4670.86 226.043 1
-1 0 10 10819.7 439.743 1
-2 0 8 60961.8 1251.84 -2
-1 0 8 60961.8 1251.84 1
-1 0 6 3368.14 82.9304 1
-1 0 4 250956. 1330.07 1
1 0 -2 3526.19 116.001 1
-1 0 0 14645.2 48.7224 -2
1 0 0 14645.2 48.7224 1
1 0 2 127024. 694.234 1
-1 0 -4 35443.0 294.018 1
1 0 6 6802.79 193.223 1
-4 0 8 8533.33 457.581 -2
1 0 8 8533.33 457.581 1
1 0 10 38482.3 787.252 1
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-1 -1 11 216.231 145.057 1
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-1 -1 8 2424.87 126.900 1
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-1 -1 4 31.6143 17.2507 1
1 -1 -3 96.1715 22.4955 1
1 -1 -2 93099.5 413.464 1
1 -1 -1 42943.3 174.556 1
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1 -1 0 71.7104 5.32994 1
1 -1 1 6942.87 78.8362 1
-1 1 -2 91561.6 352.705 1
1 -1 3 1358.53 49.7042 1
1 -1 4 88913.6 568.566 1
1 -1 5 16274.5 272.420 1
1 -1 6 4582.90 158.875 1
1 -1 7 18522.2 467.480 1
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1 -1 8 46234.2 1064.62 1
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1 -1 10 529.409 104.312 1
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1 -2 -2 74503.4 198.241 1
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1 -2 2 1410.69 30.8528 1
-1 2 -3 22136.2 137.754 1
1 2 4 583.485 34.0962 1
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3 2 -5 38228.6 582.695 -2
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1 -2 6 7941.05 145.939 1
1 2 7 10399.6 248.175 1
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1 -2 8 17028.3 455.345 1
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0 3 3 29967.9 219.248 -2
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1 -3 3 1144.88 56.3679 1
1 -3 4 8609.14 104.077 1
1 -3 5 1022.16 56.0405 1
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0 -4 3 22492.7 169.059 -2
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1 -4 5 8027.64 295.972 1
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1 -4 5 35670.2 223.482 1
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1 4 7 5849.38 118.152 1
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1 4 8 20653.1 352.780 1
1 4 9 4540.47 134.642 1
1 -4 10 48.1129 35.1693 1
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1 -5 0 20972.2 79.0823 1
1 -5 1 57359.9 202.115 1
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1 5 4 2366.36 62.6851 1
1 -5 5 26047.5 577.799 1
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1 -5 5 26976.6 187.958 1
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1 5 7 356.106 24.8972 1
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1 -5 8 3015.11 191.849 1
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1 -7 0 25700.3 102.649 1
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1 -7 6 10523.4 435.126 1
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1 7 7 6193.24 127.985 1
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1 -7 8 8496.42 264.259 1
1 -7 9 5782.78 197.308 1
1 7 10 194.661 79.7445 1
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-2 -8 8 1627.77 160.777 -2
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-6 -4 10 34.8710 42.1660 2
-6 -4 9 280.792 58.5261 2
-6 -4 7 1585.02 85.9188 2
-6 4 6 16272.6 259.768 2
-6 4 4 3851.81 127.704 2
6 4 -2 2021.16 78.6155 2
6 4 -1 6417.83 150.982 2
-6 -4 -1 1494.97 84.7683 2
-6 -4 -2 11093.9 134.964 2
-6 -4 -4-52.7847 35.1763 2
-6 -4 -7 215.083 77.7061 2
-6 -5 10 14.4524 32.0767 2
-6 -5 9 14630.9 325.091 2
-6 -5 7 16.6878 27.8386 2
-6 5 6 3667.41 130.918 2
-6 5 4 2009.45 64.8744 2
6 5 -2 1878.01 84.8633 2
6 5 -1 11833.2 203.746 2
-6 -5 -1 192.076 38.8877 2
-6 -5 -2 2079.49 100.526 2
-6 -5 -4-42.3322 32.7385 2
-6 5 -7 103.796 69.4320 2
-6 -6 10 1615.84 118.335 2
-6 -6 9 292.276 59.6673 2
-6 -6 7 3342.06 145.180 2
-6 -6 6 461.078 100.425 2
-6 -6 4 5366.48 283.020 2
-6 -6 2 755.134 78.9846 2
-6 -6 1 7762.81 244.745 2
-6 -6 -1 291.075 41.7848 2
-6 -6 -2 1307.01 78.0298 2
-6 -6 -4 2958.76 148.505 2
-6 -6 -7 1177.32 137.450 2
-6 -7 9 3585.03 232.543 2
-6 -7 7 6055.09 173.431 2
-6 -7 6 2203.80 204.860 2
-6 -7 4 42.7751 60.4099 2
-6 -7 2 5995.68 203.231 2
-6 -7 1 299.190 56.2938 2
-6 -7 -1 1656.20 85.7855 2
-6 -7 -2 179.179 32.6494 2
-6 -7 -4 2350.18 127.020 2
-6 -8 7 102.360 62.1133 2
-6 -8 4 1416.48 154.266 2
-6 -8 2 252.769 75.6340 2
-6 -8 1 5400.45 201.721 2
-6 -8 -1 9927.60 225.561 2
-6 -8 -2 1918.07 103.927 2
-6 -8 -4 90.1487 59.9283 2
-6 -9 4 432.178 92.0276 2
-6 -9 2 824.999 131.119 2
-6 -9 1 4364.10 303.143 2
-6 -9 -1 7777.13 341.795 2
-6 -10 4 4243.89 264.327 2
-6 -10 2 296.832 93.7456 2
-6 -10 1 2489.70 225.199 2
-7 0 10 362.364 67.5063 2
-7 0 6 218.422 46.8254 2
-7 0 4 12778.0 195.460 2
-7 0 2 5496.68 367.086 2
-7 0 -2 20728.7 739.606 2
-7 0 -4-61.9607 97.8669 2
-7 1 10 806.452 80.4261 2
-7 1 9-25.3680 31.6504 2
-7 1 7 1534.91 65.4901 2
-7 1 6 27826.8 359.169 2
-7 1 4 1792.76 61.9807 2
-7 1 2 10128.2 314.582 2
-7 1 1 4842.09 215.334 2
-7 1 -1 2878.48 95.1184 2
-7 1 -2 2375.77 86.4650 2
-7 1 -4-127.761 63.8126 2
-7 -2 10 4103.38 137.888 2
-7 -2 9 10066.2 205.106 2
-7 -2 7 382.787 43.1589 2
-7 2 6 27.8888 25.1692 2
-7 2 4 180.279 22.5447 2
-7 2 2 17675.7 429.869 2
-7 2 1 9930.23 435.324 2
-7 -2 -1 1316.55 94.3582 2
-7 -2 -2 6078.52 114.994 2
-7 -2 -4 4921.65 283.530 2
-7 -3 9 1334.68 80.2771 2
-7 3 7 136.796 30.8956 2
-7 3 6 48.9113 24.8082 2
-7 3 4 27109.2 320.709 2
-7 3 2 4347.05 263.324 2
-7 3 1 6871.56 266.467 2
-7 -3 -1 168.176 38.9227 2
-7 -3 -2 7095.91 183.949 2
-7 -3 -4 2539.57 206.783 2
-7 -4 9-25.9559 32.3070 2
-7 4 7 9935.43 200.771 2
-7 -4 6 916.220 75.8276 2
-7 4 4 856.653 114.942 2
-7 4 2 21124.6 441.498 2
-7 -4 1 9050.70 463.263 2
-7 -4 -1 32.9706 25.5817 2
-7 -4 -2 2019.59 103.295 2
-7 -4 -4 7054.10 236.511 2
-7 5 9 1928.57 129.311 2
-7 -5 7 4892.65 196.607 2
-7 -5 6 700.965 77.7810 2
-7 5 4 3576.56 167.957 2
-7 -5 2 2298.09 228.726 2
-7 -5 1 1760.59 219.263 2
-7 -5 -1 27025.2 352.338 2
-7 -5 -2 89.1518 33.8052 2
-7 -5 -4 53.6912 45.4638 2
-7 -6 9 189.181 50.2836 2
-7 -6 7 9247.32 221.978 2
-7 -6 6 48.4976 53.5308 2
-7 -6 4 1690.31 178.544 2
-7 -6 2 1367.50 181.873 2
-7 -6 1 19189.0 666.914 2
-7 -6 -1 48.9918 29.1031 2
-7 -6 -2 618.145 59.7730 2
-7 -6 -4 72.6785 42.4434 2
-7 -7 9 1301.13 156.944 2
-7 -7 7 156.068 58.2257 2
-7 -7 4 2862.02 225.296 2
-7 -7 2 225.738 91.6266 2
-7 -7 1 5132.13 350.136 2
-7 -7 -1 5238.10 159.908 2
-7 -7 -2 4292.51 144.688 2
-7 -7 -4 371.508 75.7075 2
-7 -8 4 358.365 90.5010 2
-7 -8 2 1783.45 211.463 2
-7 -8 1 211.316 55.9833 2
-7 -8 -1 985.516 81.0016 2
-7 -8 -2 10.8868 39.2890 2
-7 -9 4 85.3342 63.6828 2
-7 -9 2 464.159 119.027 2
-7 -9 1 7973.58 417.052 2
-7 -9 -1 147.659 65.8278 2
-7 -10 2 555.865 124.788 2
-8 0 10 37.5315 59.1993 2
-8 0 6 1320.27 114.783 2
-8 0 4 28617.4 860.758 2
-8 0 2 33836.0 886.064 2
-8 0 -2 31397.5 913.851 2
-8 0 -4 34.1139 90.1259 2
-8 1 10 10939.6 453.593 2
-8 1 9 2511.96 126.613 2
-8 1 7 1385.49 94.0817 2
-8 1 6 2771.22 132.010 2
-8 1 4 8740.05 309.563 2
-8 1 2 6630.04 270.593 2
-8 1 1 11541.2 342.374 2
-8 1 -1 161.141 35.3014 2
-8 1 -2 799.187 45.3946 2
-8 1 -4 14166.5 751.248 2
-8 2 10 16.4729 49.2831 2
-8 -2 9 144.409 40.0056 2
-8 2 7 7912.35 185.227 2
-8 2 6 5272.61 180.847 2
-8 2 4 3336.31 134.935 2
-8 2 2 14038.2 394.088 2
-8 2 1 5568.33 357.627 2
-8 -2 -1 13769.8 236.633 2
-8 -2 -2 1010.31 72.5081 2
-8 -2 -4 366.844 58.4131 2
-8 3 9 67.2169 50.0834 2
-8 3 7 936.721 69.3715 2
-8 -3 6 2868.54 130.902 2
-8 3 4 2075.69 143.636 2
-8 3 2 10382.1 434.024 2
-8 3 1 12477.0 375.246 2
-8 -3 -1 3085.46 123.955 2
-8 -3 -2 7387.08 193.405 2
-8 -3 -4-36.5299 30.8533 2
-8 4 7 427.563 55.1607 2
-8 -4 6 10208.3 304.876 2
-8 4 4 254.723 77.3969 2
-8 4 2 1350.15 129.575 2
-8 -4 1 2364.12 253.971 2
-8 -4 -1 52.0745 28.4384 2
-8 -4 -2 846.387 73.9028 2
-8 -4 -4 301.991 64.6074 2
-8 -4 -5 1920.26 197.931 2
8 4 6 602.462 128.721 2
-8 -5 7-29.5357 46.6020 2
-8 5 4-25.5242 29.4971 2
-8 -5 2 25.4443 62.2413 2
-8 -5 1 386.262 120.539 2
-8 -5 -1 3271.79 131.214 2
-8 -5 -2 1172.38 87.5506 2
-8 -5 -4 105.337 53.1563 2
-8 -6 7-16.4284 73.2840 2
-8 -6 4 3071.77 271.991 2
-8 -6 2 1240.25 195.737 2
-8 -6 1 5850.20 388.957 2
-8 -6 -1 248.147 45.9852 2
-8 -6 -2 3056.24 132.491 2
-8 -6 -4-0.62152 37.1328 2
-8 -7 4 2408.78 241.656 2
-8 -7 2 6432.00 419.694 2
-8 -7 1 7044.28 235.163 2
-8 -7 -1 1998.83 106.552 2
-8 -7 -2 488.625 56.5637 2
-8 -7 -4 1825.29 227.766 2
-8 -8 2 47.5453 74.9827 2
-8 -8 1 272.414 62.3418 2
-8 -8 -1 8430.88 400.847 2
-8 -8 -2 590.676 118.338 2
-9 0 6 10691.2 345.522 2
-9 0 4 154.003 92.4260 2
-9 0 2 30097.9 878.352 2
-9 0 -2 7016.66 446.037 2
-9 1 9 836.398 144.607 2
-9 1 7 1102.57 92.2496 2
-9 1 6 2572.96 178.438 2
-9 1 4 1011.02 121.304 2
-9 1 2 1666.32 147.287 2
-9 1 1 3810.10 207.079 2
-9 1 -1 5332.38 397.348 2
-9 1 -2 870.526 70.7226 2
-9 2 9 362.057 109.866 2
-9 -2 7 83.4512 31.5736 2
-9 -2 6 3890.70 299.682 2
-9 2 4 10128.5 345.614 2
-9 2 2 1171.66 120.214 2
-9 2 1 292.181 114.450 2
-9 -2 -1-13.2172 28.2654 2
-9 -2 -2 72.7685 27.8862 2
9 2 4 1370.03 123.510 2
-9 3 7 238.585 43.5274 2
-9 -3 6 2820.38 190.424 2
-9 3 4 2970.05 182.066 2
-9 3 2 11928.9 496.208 2
-9 3 1 323.762 77.1172 2
-9 -3 -1 1372.47 83.9157 2
-9 -3 -2 10941.2 234.996 2
9 3 4 1347.35 136.066 2
9 3 5 866.992 123.047 2
-9 -4 7 35.5267 41.4184 2
-9 -4 6 391.157 116.241 2
-9 4 4 16918.7 530.388 2
-9 4 2 751.671 101.272 2
-9 -4 1 7631.78 433.284 2
-9 -4 -1 3012.59 126.939 2
-9 -4 -2 1477.24 94.6995 2
9 4 4 3302.64 225.542 2
-9 5 7 11074.1 485.905 2
-9 5 4 206.626 62.6465 2
-9 -5 2 2627.00 281.622 2
-9 -5 1 12915.6 553.119 2
-9 -5 -1 3469.68 138.141 2
-9 -5 -2 1274.19 91.4155 2
9 5 4 792.078 125.215 2
-9 -6 2 4886.39 376.951 2
-9 -6 1 8701.78 460.898 2
-9 -6 -1 9837.38 287.823 2
-9 -6 -2 1070.02 96.5432 2
-9 -7 1 1331.87 178.813 2
-9 -7 -1 40.9743 61.2614 2
-10 0 4 1778.49 228.862 2
-10 0 2 9728.94 498.974 2
-10 1 7 410.434 120.425 2
-10 1 6 488.178 95.4906 2
-10 1 4 20990.0 525.499 2
-10 1 2 3248.26 208.137 2
-10 1 1 489.931 90.2081 2
-10 2 7 7365.51 426.478 2
-10 2 6 1159.33 168.036 2
-10 2 4 280.279 74.4437 2
-10 2 2-8.25674 62.0187 2
-10 2 1 15194.6 639.116 2
-10 3 7 1488.45 183.659 2
-10 3 4 121.598 71.4674 2
-10 3 2 11115.7 507.551 2
-10 -3 1 357.625 101.110 2
-10 4 4 104.878 76.0040 2
0 0 0 0.00000 0.00000 0
TITL shS_496_IlGu_twin1_hklf4 in P2(1)/c
REM P2(1)/c (#14 in standard setting)
CELL 0.71073 8.307344 8.879975 9.383787 90.0000 102.0042 90.0000
ZERR 8.00 0.000724 0.000608 0.000670 0.0000 0.0074 0.0000
LATT 1
SYMM -x, y+1/2,-z+1/2
SFAC C H N I
UNIT 16.00 56.00 8.00 16.00
REM CrysAlisPro recorded range (K): Min=100.0; max=100.0; aver:100.0
TEMP -173
TREF
HKLF 5
BASF 0.39701
END
;
_shelx_hkl_checksum 42906
_shelx_res_file
;
TITL shS_496_IlGu_twin1_hklf4 in P21/c #14
shs_496_ilgu_twin1_hklf4.res
created by SHELXL-2018/3 at 11:38:51 on 13-Sep-2024
CELL 0.71073 8.307344 8.879975 9.383787 90 102.0042 90
ZERR 4 0.000724 0.000608 0.00067 0 0.0074 0
LATT 1
SYMM -X,0.5+Y,0.5-Z
SFAC C H I N
UNIT 8 28 8 4
EQIV $1 1-X,-0.5+Y,0.5-Z
EQIV $2 1-X,1-Y,1-Z
EQIV $3 +X,1.5-Y,-0.5+Z
L.S. 4 0 0
PLAN 6
TEMP -173
HTAB N1 I2
CONF
HTAB N1 I2_$1
HTAB N1 I2_$2
HTAB N1 I2_$3
BOND
MORE -1
BOND $H
fmap 2 53
acta
OMIT 4 6 3
REM
REM
REM
WGHT 0.109800 4.108900
BASF 0.38325
FVAR 2.10207
I2 3 0.633814 0.783342 0.533129 11.00000 0.02141 0.01347 =
0.01504 0.00083 0.00506 -0.00033
I1 3 0.195456 0.893074 0.178324 11.00000 0.01885 0.01918 =
0.03007 0.00373 0.00682 0.00346
N1 4 0.381875 0.545888 0.261811 11.00000 0.02215 0.01262 =
0.01854 0.00120 0.00568 -0.00154
AFIX 138
H1A 2 0.412091 0.470595 0.314425 11.00000 -1.50000
H1B 2 0.417064 0.624402 0.307358 11.00000 -1.50000
H1C 2 0.419497 0.540061 0.185772 11.00000 -1.50000
AFIX 0
C2 1 0.195800 0.550595 0.221854 11.00000 0.01957 0.01963 =
0.02047 0.00300 0.00325 -0.00091
AFIX 23
H2A 2 0.153639 0.449803 0.187631 11.00000 -1.20000
H2B 2 0.152455 0.575673 0.309573 11.00000 -1.20000
AFIX 0
C1 1 0.134874 0.664267 0.105308 11.00000 0.02404 0.02859 =
0.01665 -0.00481 0.00065 0.00384
AFIX 23
H1D 2 0.013934 0.654792 0.073950 11.00000 -1.20000
H1E 2 0.183992 0.642845 0.019956 11.00000 -1.20000
AFIX 0
HKLF 5
REM shS_496_IlGu_twin1_hklf4 in P21/c #14
REM wR2 = 0.1589, GooF = S = 1.117, Restrained GooF = 1.117 for all data
REM R1 = 0.0505 for 2535 Fo > 4sig(Fo) and 0.0537 for all 2744 data
REM 49 parameters refined using 0 restraints
END
WGHT 0.1098 4.1089
REM Highest difference peak 2.069, deepest hole -1.678, 1-sigma level 0.355
Q1 1 0.1767 0.6140 0.3637 11.00000 0.05 1.84
Q2 1 0.6041 0.7172 0.4335 11.00000 0.05 1.77
Q3 1 0.5212 0.8128 0.4628 11.00000 0.05 1.58
Q4 1 0.0749 0.8961 0.2746 11.00000 0.05 1.49
Q5 1 0.0915 0.9313 0.1051 11.00000 0.05 1.36
Q6 1 0.7408 0.7771 0.4951 11.00000 0.05 1.35
;
_shelx_res_checksum 11766
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
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 I2 0.63381(7) 0.78334(6) 0.53313(6) 0.0165(2) Uani d 1 . .
I I1 0.19546(8) 0.89307(7) 0.17832(7) 0.0224(2) Uani d 1 . .
N N1 0.3819(10) 0.5459(8) 0.2618(8) 0.0176(15) Uani d 1 . .
H H1A 0.412(3) 0.471(7) 0.314(7) 0.026 Uiso calc 1 . .
H H1B 0.417(3) 0.624(7) 0.307(8) 0.026 Uiso calc 1 . .
H H1C 0.419(3) 0.540(8) 0.186(6) 0.026 Uiso calc 1 . .
C C2 0.1958(12) 0.5506(11) 0.2219(10) 0.0200(18) Uani d 1 . .
H H2A 0.153639 0.449803 0.187631 0.024 Uiso calc 1 . .
H H2B 0.152455 0.575673 0.309573 0.024 Uiso calc 1 . .
C C1 0.1349(13) 0.6643(12) 0.1053(10) 0.024(2) Uani d 1 . .
H H1D 0.013934 0.654792 0.073950 0.028 Uiso calc 1 . .
H H1E 0.183992 0.642845 0.019956 0.028 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
I2 0.0214(4) 0.0135(4) 0.0150(4) -0.00033(17) 0.0051(3) 0.00083(17)
I1 0.0189(4) 0.0192(4) 0.0301(4) 0.0035(2) 0.0068(3) 0.0037(2)
N1 0.022(4) 0.013(3) 0.019(4) -0.002(3) 0.006(3) 0.001(3)
C2 0.020(4) 0.020(5) 0.020(5) -0.001(3) 0.003(4) 0.003(3)
C1 0.024(5) 0.029(5) 0.017(4) 0.004(4) 0.001(4) -0.005(4)
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_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-11 0 -1 0.0319
1 10 -8 0.1130
-8 -8 6 0.0762
1 12 0 0.0663
4 5 -12 0.1238
-1 -12 0 0.0777
-4 -2 13 0.1318
-1 -12 3 0.0867
-3 -7 11 0.1172
9 8 -1 0.0484
-5 5 -9 0.1028
-8 0 -8 0.0911
-9 -8 1 0.0451
-11 3 2 0.0531
-8 8 -3 0.0654
-7 10 0 0.0542
6 -11 0 0.0743
11 1 0 0.0412
11 4 -2 0.0496
11 -2 2 0.0527
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
H1A N1 H1B . . 109.5 ?
H1A N1 H1C . . 109.5 ?
H1B N1 H1C . . 109.5 ?
C2 N1 H1A . . 109.5 ?
C2 N1 H1B . . 109.5 ?
C2 N1 H1C . . 109.5 ?
N1 C2 H2A . . 109.2 ?
N1 C2 H2B . . 109.2 ?
H2A C2 H2B . . 107.9 ?
C1 C2 N1 . . 111.9(8) ?
C1 C2 H2A . . 109.2 ?
C1 C2 H2B . . 109.2 ?
I1 C1 H1D . . 109.1 ?
I1 C1 H1E . . 109.1 ?
C2 C1 I1 . . 112.3(6) ?
C2 C1 H1D . . 109.1 ?
C2 C1 H1E . . 109.1 ?
H1D C1 H1E . . 107.9 ?
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 C1 . 2.170(10) ?
N1 H1A . 0.84(6) ?
N1 H1B . 0.84(6) ?
N1 H1C . 0.84(6) ?
N1 C2 . 1.514(12) ?
C2 H2A . 0.9900 ?
C2 H2B . 0.9900 ?
C2 C1 . 1.497(14) ?
C1 H1D . 0.9900 ?
C1 H1E . 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
N1 H1A I2 3_666 0.84 2.74 3.517(7) 155.1 yes
N1 H1B I2 . 0.84 2.85 3.618(8) 152.9 yes
N1 H1C I2 4_575 0.84 2.96 3.627(8) 138.5 yes
N1 H1C I2 2_645 0.84 3.04 3.600(8) 126.5 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
N1 C2 C1 I1 . . . . -65.8(9) ?
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.617(2)
2 0.383(2)