#------------------------------------------------------------------------------
#$Date: 2022-11-10 03:47:41 +0100 (Thu, 10 Nov 2022) $
#$Revision: 279171 $
#$URL: svn://www.crystallography.net/cod/cif/2/02/26/2022695.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_2022695
loop_
_publ_author_name
'De Silva, Viraj'
'Magueres, Pierre Le'
'Averkiev, Boris B.'
'Aaker\"oy, Christer B.'
_publ_section_title
;
Competition between chalcogen and halogen bonding assessed through
isostructural species
;
_journal_coeditor_code BS3004
_journal_issue 12
_journal_name_full 'Acta Crystallographica Section C'
_journal_page_first
;
;
_journal_paper_doi 10.1107/S205322962201052X
_journal_volume 78
_journal_year 2022
_chemical_formula_iupac 'C8 H4 I2 N2 S'
_chemical_formula_moiety 'C8 H4 I2 N2 S'
_chemical_formula_sum 'C8 H4 I2 N2 S'
_chemical_formula_weight 413.99
_chemical_name_systematic
;
2-Iodo-5-(4-iodophenyl)-1,3,4-thiadiazole
;
_space_group_crystal_system orthorhombic
_space_group_IT_number 61
_space_group_name_Hall '-P 2ac 2ab'
_space_group_name_H-M_alt 'P b c a'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary dual
_audit_creation_method
;
OLEX2
(compiled 2020.11.27 svn.r5f609507 for Rigaku Oxford Diffraction, GUI svn.r6214)
;
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_formula_units_Z 8
_cell_length_a 11.0392(2)
_cell_length_b 8.1756(2)
_cell_length_c 23.3673(4)
_cell_measurement_reflns_used 5508
_cell_measurement_temperature 293(2)
_cell_measurement_theta_max 68.9500
_cell_measurement_theta_min 3.7600
_cell_volume 2108.95(7)
_computing_cell_refinement
;
CrysAlis PRO (Rigaku OD, 2020)
;
_computing_data_collection
;
CrysAlis PRO (Rigaku OD, 2020)
;
_computing_data_reduction
;
CrysAlis PRO (Rigaku OD, 2020)
;
_computing_molecular_graphics
;
OLEX2 (Dolomanov et al., 2009)
;
_computing_publication_material
;
OLEX2 (Dolomanov et al., 2009)
;
_computing_structure_refinement
;
SHELXL2018 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT2018 (Sheldrick, 2015a)
;
_diffrn_ambient_temperature 293(2)
_diffrn_detector 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device 'four-circle diffractometer'
_diffrn_measurement_device_type
'Rigaku XtaLAB Synergy Custom diffractometer with a HyPix-Arc 150\% detector'
_diffrn_measurement_method '\w scans'
_diffrn_radiation_monochromator mirror
_diffrn_radiation_probe x-ray
_diffrn_radiation_type CuK\a
_diffrn_radiation_wavelength 1.54184
_diffrn_reflns_av_R_equivalents 0.0243
_diffrn_reflns_av_unetI/netI 0.0215
_diffrn_reflns_limit_h_max 13
_diffrn_reflns_limit_h_min -11
_diffrn_reflns_limit_k_max 9
_diffrn_reflns_limit_k_min -8
_diffrn_reflns_limit_l_max 28
_diffrn_reflns_limit_l_min -24
_diffrn_reflns_number 8336
_diffrn_reflns_theta_full 67.684
_diffrn_reflns_theta_max 69.060
_diffrn_reflns_theta_min 3.783
_diffrn_source 'Rotating-anode X-ray tube'
_exptl_absorpt_coefficient_mu 48.342
_exptl_absorpt_correction_T_max 0.522
_exptl_absorpt_correction_T_min 0.209
_exptl_absorpt_correction_type gaussian
_exptl_absorpt_process_details
;
(CrysAlis PRO; Rigaku OD, 2020)
;
_exptl_crystal_colour colourless
_exptl_crystal_density_diffrn 2.608
_exptl_crystal_description block
_exptl_crystal_F_000 1504
_exptl_crystal_size_max 0.065
_exptl_crystal_size_mid 0.054
_exptl_crystal_size_min 0.027
_refine_diff_density_max 1.328
_refine_diff_density_min -1.221
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.088
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 118
_refine_ls_number_reflns 1942
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.088
_refine_ls_R_factor_all 0.0293
_refine_ls_R_factor_gt 0.0262
_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^)+(0.0388P)^2^+4.6153P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0691
_refine_ls_wR_factor_ref 0.0709
_reflns_number_gt 1753
_reflns_number_total 1942
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file bs3004sup1.cif
_cod_data_source_block T1
_cod_database_code 2022695
_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 2 172.31 5.49
0 0 2 174.60 5.48
0 0 -2 176.79 5.48
0 0 2 172.36 5.53
0 0 3 -0.03 0.38
0 0 3 0.01 0.31
0 0 3 0.04 0.31
0 0 -3 0.14 0.36
0 0 -3 0.31 0.35
0 0 3 0.14 0.35
0 0 4 87.28 3.04
0 0 -4 88.52 2.95
0 0 4 92.57 2.99
0 0 -4 84.31 2.93
0 0 -5 0.19 0.45
0 0 5 -0.06 0.52
0 0 5 0.36 0.47
0 0 6 1090.84 32.98
0 0 6 1060.34 32.88
0 0 -6 1032.62 32.82
0 0 7 0.03 0.54
0 0 7 0.30 0.57
0 0 -7 0.32 0.54
0 0 7 0.15 0.58
0 0 -8 5611.65 182.72
0 0 8 5875.50 182.80
0 0 8 5946.90 182.82
0 0 -9 0.34 0.49
0 0 9 0.42 0.50
0 0 9 0.31 0.59
0 0 10 25.38 1.49
0 0 10 32.98 1.50
0 0 11 0.71 0.54
0 0 11 -0.28 0.56
0 0 11 0.34 0.59
0 0 12 52.66 2.32
0 0 12 46.68 2.26
0 0 13 0.19 0.62
0 0 13 0.38 0.53
0 0 13 0.40 0.73
0 0 13 0.22 0.61
0 0 14 2131.25 67.11
0 0 14 2181.22 66.95
0 0 14 2129.25 67.05
0 0 14 2167.36 67.12
0 0 15 0.19 0.53
0 0 15 0.42 0.61
0 0 15 0.52 0.72
0 0 15 0.99 0.59
0 0 16 1275.64 40.69
0 0 16 1308.03 40.50
0 0 16 1287.22 40.63
0 0 17 -0.07 0.58
0 0 17 -0.21 0.73
0 0 17 -0.25 0.68
0 0 18 29.45 1.75
0 0 18 26.87 1.84
0 0 19 0.24 0.66
0 0 19 -0.18 0.75
0 0 19 0.08 0.59
0 0 19 0.34 0.66
0 0 20 74.49 3.29
0 0 20 76.37 3.47
0 0 20 74.28 3.31
0 0 21 -0.31 0.65
0 0 21 -0.08 0.68
0 0 21 0.28 0.76
0 0 -22 516.53 17.37
0 0 23 -0.14 0.58
0 0 23 0.42 0.65
0 0 24 145.84 5.60
0 0 24 151.88 5.47
0 0 25 0.45 0.55
0 0 25 -0.35 0.61
0 0 26 122.85 4.59
0 0 27 0.20 0.50
0 1 0 0.31 0.33
0 -1 0 0.11 0.31
0 1 0 0.46 0.42
0 -1 -1 0.12 0.23
0 1 1 0.13 0.20
0 1 -1 -0.28 0.47
0 -1 1 0.56 0.43
0 1 -1 0.23 0.16
0 -1 -1 0.24 0.15
0 1 -1 0.48 0.45
0 1 2 0.88 0.25
0 1 -2 0.13 0.52
0 1 2 0.37 0.25
0 1 2 0.16 0.28
0 1 -2 0.05 0.56
0 -1 2 0.20 0.56
0 1 2 0.34 0.26
0 -1 -2 0.41 0.26
0 -1 2 0.28 0.50
0 1 3 0.08 0.41
0 1 3 0.14 0.31
0 -1 -3 0.20 0.30
0 1 -3 0.59 0.62
0 -1 3 0.14 0.63
0 1 3 -0.01 0.31
0 1 3 0.67 0.16
0 1 3 0.91 0.34
0 -1 -3 0.47 0.19
0 -1 3 -0.43 0.66
0 1 3 0.27 0.33
0 -1 4 0.27 0.71
0 -1 4 -0.22 0.65
0 1 4 0.26 0.40
0 1 4 0.13 0.37
0 1 4 0.14 0.25
0 1 4 0.54 0.17
0 1 4 0.71 0.47
0 1 4 0.41 0.40
0 -1 -4 0.38 0.21
0 1 4 0.15 0.41
0 1 -4 1.22 0.72
0 1 -5 -0.08 0.76
0 -1 -5 0.28 0.27
0 1 5 0.07 0.46
0 -1 5 -0.26 0.71
0 -1 5 0.45 0.80
0 1 5 0.09 0.43
0 1 5 0.76 0.54
0 1 5 0.12 0.48
0 1 5 0.59 0.35
0 1 5 0.16 0.22
0 1 5 0.16 0.35
0 -1 5 0.26 0.31
0 1 6 0.36 0.48
0 1 -6 0.17 0.81
0 -1 6 1.08 0.74
0 1 6 -0.22 0.60
0 1 6 0.56 0.39
0 -1 6 0.24 0.39
0 1 6 0.32 0.53
0 -1 6 0.81 0.76
0 1 6 0.15 0.41
0 1 7 -0.05 0.42
0 1 7 2.75 0.65
0 1 -7 0.18 0.73
0 -1 7 0.72 0.82
0 1 7 -0.08 0.43
0 1 7 0.12 0.30
0 1 7 0.41 0.49
0 1 7 0.10 0.57
0 -1 7 0.16 0.71
0 1 8 0.18 0.46
0 1 -8 0.09 0.72
0 1 8 0.79 0.43
0 1 8 0.40 0.50
0 -1 8 -0.16 0.68
0 1 8 0.24 0.32
0 -1 8 0.41 0.72
0 1 8 0.95 0.62
0 1 8 1.45 0.66
0 1 -9 0.37 0.66
0 1 9 0.41 0.33
0 1 9 0.28 0.50
0 1 9 -0.03 0.41
0 1 9 0.23 0.48
0 -1 9 -0.12 0.68
0 -1 9 -0.03 0.58
0 1 9 0.71 0.67
0 1 -10 0.34 0.61
0 -1 10 -0.44 0.66
0 1 10 -0.10 0.43
0 1 10 1.73 0.70
0 -1 10 -0.11 0.58
0 1 10 0.66 0.54
0 1 11 0.68 0.53
0 1 11 -0.62 0.82
0 -1 11 0.46 0.59
0 1 11 0.38 0.63
0 1 11 -0.04 0.41
0 1 11 -0.10 0.51
0 1 -11 1.04 0.58
0 1 12 0.08 0.40
0 1 -12 0.30 0.55
0 1 12 0.29 0.63
0 1 12 0.32 0.53
0 1 12 0.10 0.67
0 1 12 0.26 0.80
0 1 12 1.39 0.59
0 -1 12 0.08 0.60
0 1 13 0.20 0.76
0 1 13 1.10 0.54
0 1 13 0.73 0.70
0 1 13 0.29 0.69
0 1 13 -0.06 0.66
0 1 13 0.12 0.54
0 1 14 0.62 0.56
0 -1 14 0.19 0.53
0 1 14 0.27 0.59
0 1 14 0.07 0.80
0 1 14 1.06 0.65
0 1 14 0.70 0.70
0 1 14 1.44 0.54
0 1 15 0.20 0.63
0 1 15 -0.23 0.75
0 1 15 0.33 0.58
0 1 15 1.22 0.68
0 -1 15 -0.07 0.68
0 1 15 0.44 0.65
0 1 16 0.07 0.63
0 1 16 0.24 0.84
0 1 16 0.19 0.67
0 1 16 -0.47 0.68
0 1 17 -0.25 0.77
0 1 17 0.17 0.71
0 -1 17 -0.07 0.58
0 1 17 0.74 0.65
0 -1 17 0.56 0.72
0 1 17 0.92 0.65
0 1 18 -0.08 0.66
0 1 18 0.09 0.67
0 1 18 0.94 0.81
0 -1 18 0.14 0.54
0 -1 18 0.16 0.70
0 1 18 -0.47 0.62
0 -1 19 -0.07 0.56
0 1 19 0.64 0.73
0 1 19 0.24 0.61
0 1 19 0.17 0.77
0 -1 19 -0.16 0.74
0 1 19 0.54 0.74
0 -1 20 1.56 0.81
0 1 20 0.56 0.69
0 -1 20 -0.07 0.59
0 1 20 0.50 0.78
0 -1 20 0.56 0.73
0 1 20 0.45 0.74
0 -1 21 0.60 0.60
0 -1 21 0.08 0.73
0 -1 21 -0.19 0.76
0 1 21 -0.09 0.73
0 1 21 0.65 0.72
0 -1 22 0.22 0.57
0 -1 23 0.69 0.68
0 1 23 -0.17 0.62
0 -1 23 -0.43 0.63
0 1 23 -0.22 0.61
0 -1 24 -0.39 0.60
0 1 24 -0.39 0.63
0 1 -24 -0.09 0.72
0 -1 24 0.23 0.64
0 1 25 0.48 0.56
0 -1 25 0.41 0.59
0 -1 25 0.22 0.53
0 -1 26 0.18 0.55
0 -1 27 0.39 0.47
0 -1 28 -0.27 0.39
0 2 0 42.30 1.62
0 2 0 41.25 1.88
0 -2 0 41.31 1.66
0 -2 1 9.46 0.85
0 -2 -1 8.22 0.52
0 2 1 8.24 0.84
0 2 1 7.73 0.80
0 2 -1 8.94 0.54
0 2 1 9.61 0.60
0 2 2 472.64 14.70
0 -2 -2 465.84 14.70
0 -2 2 498.34 15.07
0 2 2 472.40 14.82
0 2 -2 488.35 15.09
0 2 2 477.31 14.69
0 2 2 462.26 14.50
0 -2 -2 454.85 14.55
0 2 2 496.29 14.92
0 -2 3 369.61 11.19
0 2 3 351.40 10.95
0 2 3 345.11 10.66
0 -2 -3 340.75 10.68
0 -2 -3 324.42 10.45
0 2 3 340.64 10.67
0 2 3 335.66 10.70
0 2 -3 353.23 11.11
0 2 4 9921.72 304.16
0 -2 4 9473.19 304.36
0 2 4 9986.27 303.85
0 -2 -4 9999.00 303.91
0 2 4 9844.26 303.84
0 -2 -4 9856.25 303.62
0 2 4 9930.70 303.89
0 -2 -4 9864.00 303.68
0 2 -4 9806.31 304.31
0 -2 -5 123.70 4.57
0 -2 5 143.09 5.17
0 2 5 146.73 4.59
0 2 5 135.85 4.57
0 2 5 132.03 4.43
0 2 -5 129.62 4.97
0 2 5 145.28 4.60
0 2 5 137.41 4.92
0 2 6 223.10 6.94
0 2 6 199.94 7.25
0 2 6 225.39 6.93
0 2 6 216.38 6.92
0 -2 -6 204.06 6.65
0 -2 -6 207.47 6.67
0 2 -6 203.33 7.30
0 -2 6 212.04 7.50
0 2 7 81.92 2.86
0 -2 -7 75.02 2.58
0 2 -7 72.73 3.18
0 -2 -7 72.99 2.53
0 -2 7 75.03 3.29
0 2 7 76.40 2.80
0 -2 -8 95.57 2.64
0 2 8 85.30 2.86
0 2 -8 90.59 3.24
0 -2 8 93.68 3.37
0 2 9 71.15 2.91
0 2 9 73.36 2.90
0 2 9 71.63 3.19
0 2 9 77.92 2.97
0 2 -9 79.30 3.18
0 -2 -9 72.46 2.70
0 2 -10 1818.31 56.16
0 2 10 1835.66 56.00
0 2 10 1800.51 55.97
0 -2 -10 1785.36 55.75
0 2 10 1822.08 56.26
0 2 10 1735.31 55.96
0 2 -11 98.84 3.92
0 2 11 98.34 3.79
0 2 11 91.94 3.72
0 2 11 100.46 3.80
0 2 11 98.35 4.02
0 -2 -11 97.42 3.57
0 2 12 2485.73 76.43
0 2 12 2476.52 76.42
0 2 12 2394.51 76.39
0 2 -12 2490.00 76.52
0 2 12 2532.81 76.66
0 -2 -12 2404.05 76.18
0 2 13 5.33 0.84
0 2 -13 3.40 0.80
0 2 13 4.06 0.78
0 2 13 2.78 0.75
0 -2 -13 4.30 0.70
0 2 13 3.05 0.88
0 2 14 0.87 0.72
0 2 -14 2.54 0.72
0 2 14 1.20 0.74
0 2 14 1.34 0.80
0 2 15 5.03 1.00
0 2 15 4.02 0.83
0 2 15 4.33 0.85
0 2 16 45.80 2.54
0 -2 16 48.62 2.56
0 2 16 47.13 2.41
0 2 16 47.76 2.46
0 2 17 1.61 0.92
0 -2 17 1.00 0.80
0 2 17 2.38 0.80
0 2 17 0.56 0.72
0 2 18 916.14 30.50
0 2 18 986.10 30.78
0 -2 18 945.66 30.41
0 2 18 954.59 30.63
0 -2 18 988.51 30.73
0 -2 19 0.93 0.75
0 2 19 0.29 0.84
0 2 19 0.73 0.72
0 -2 19 0.23 0.60
0 2 19 0.34 0.69
0 2 20 518.29 17.56
0 -2 20 544.07 17.45
0 2 20 527.37 17.70
0 -2 20 547.37 17.71
0 2 20 533.40 17.74
0 -2 21 1.58 0.75
0 -2 21 1.13 0.62
0 -2 22 82.96 3.79
0 -2 22 93.22 3.80
0 2 22 90.69 3.85
0 -2 23 4.92 0.89
0 -2 23 5.73 0.84
0 -2 24 65.30 3.02
0 -2 24 70.11 2.92
0 -2 25 3.77 0.77
0 -2 25 3.32 0.66
0 -2 26 196.94 6.80
0 -2 27 1.40 0.49
0 3 0 0.18 0.48
0 3 0 0.81 0.74
0 -3 0 0.21 0.42
0 3 1 1.39 0.63
0 3 -1 1.46 0.79
0 3 1 -0.09 0.43
0 -3 1 -0.17 0.57
0 3 1 0.45 0.71
0 3 2 0.76 0.45
0 3 -2 0.25 0.83
0 3 2 0.69 0.69
0 -3 2 1.29 0.71
0 3 2 -0.04 0.68
0 -3 -2 0.48 0.41
0 3 2 0.12 0.20
0 -3 -2 2.08 0.48
0 3 3 0.75 0.46
0 3 3 0.09 0.72
0 3 -3 0.87 0.84
0 -3 3 0.98 0.80
0 -3 -3 0.74 0.32
0 -3 -3 0.26 0.44
0 3 3 0.33 0.59
0 -3 -4 0.15 0.19
0 -3 4 1.50 0.94
0 -3 -4 -0.28 0.46
0 3 4 0.26 0.55
0 3 4 0.31 0.78
0 3 -4 0.64 0.85
0 3 5 0.31 0.50
0 3 5 0.17 0.38
0 3 -5 0.67 0.89
0 -3 5 0.75 0.90
0 -3 -5 1.47 0.23
0 -3 -5 0.96 0.53
0 3 -6 2.12 1.01
0 3 6 0.28 0.25
0 3 6 0.21 0.39
0 3 6 0.51 0.90
0 -3 -6 2.94 0.59
0 3 6 0.66 0.49
0 -3 6 0.72 0.86
0 3 7 0.64 0.50
0 3 -7 0.81 0.92
0 3 7 -0.07 0.87
0 3 8 0.30 0.84
0 3 -8 0.65 0.85
0 3 9 0.40 0.90
0 3 -9 -0.08 0.80
0 3 10 1.01 0.90
0 3 -10 0.25 0.73
0 3 -11 -0.25 0.77
0 3 11 0.70 0.87
0 3 12 0.71 0.67
0 3 -12 -0.09 0.75
0 3 12 -0.09 0.80
0 3 13 0.57 0.81
0 3 13 1.94 0.77
0 3 14 0.33 0.74
0 3 14 0.49 0.78
0 3 15 0.17 0.69
0 3 -15 -0.35 0.72
0 3 15 1.00 0.88
0 3 16 0.51 0.90
0 3 16 1.17 0.76
0 -3 17 0.42 0.76
0 3 17 -0.21 0.80
0 3 18 0.10 0.96
0 -3 18 -0.41 0.78
0 -3 19 -1.01 0.87
0 3 19 -0.10 0.91
0 -3 20 -0.78 0.82
0 -3 21 -0.54 0.78
0 -3 21 0.39 0.81
0 3 21 -0.37 0.81
0 -3 22 0.34 0.73
0 -3 22 -0.14 0.71
0 -3 22 0.09 0.74
0 -3 23 0.66 0.66
0 -3 23 0.93 0.68
0 -3 24 0.06 0.53
0 -3 24 0.41 0.58
0 -3 25 0.14 0.48
0 -3 25 -0.47 0.56
0 -3 26 -0.28 0.47
0 -4 0 4304.55 133.72
0 4 0 4346.46 134.25
0 4 0 4381.46 133.83
0 4 0 4295.05 134.29
0 4 -1 1.68 0.94
0 4 1 0.93 0.54
0 4 -1 1.80 0.96
0 4 1 1.48 0.54
0 -4 1 1.08 0.53
0 4 1 1.04 0.83
0 4 1 0.91 0.73
0 -4 -1 0.86 0.49
0 4 2 485.73 14.79
0 -4 -2 434.15 14.44
0 -4 2 454.07 14.93
0 4 2 486.58 14.77
0 4 2 465.93 14.96
0 4 2 460.58 15.06
0 4 -2 454.55 15.24
0 -4 3 97.05 3.82
0 4 3 90.89 3.68
0 4 3 95.25 3.56
0 4 3 87.08 3.43
0 4 3 94.27 3.49
0 4 -3 91.50 4.01
0 4 4 72.85 2.96
0 4 4 67.43 2.73
0 4 -4 61.11 3.14
0 4 4 65.95 2.62
0 4 4 67.38 2.71
0 4 5 31.17 1.65
0 4 -5 39.81 2.22
0 4 5 37.05 1.76
0 4 5 34.72 1.47
0 4 5 34.31 1.95
0 4 6 1029.68 32.25
0 4 6 1007.02 32.24
0 4 6 1009.67 32.54
0 4 -6 1064.25 32.88
0 4 -7 320.83 11.35
0 4 7 327.42 10.83
0 4 7 328.64 11.18
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11 2 3 1.04 1.21
11 -2 -3 1.04 0.97
11 -2 3 1.76 0.86
-11 2 4 8.78 1.30
-11 2 -4 7.91 1.26
11 2 4 7.77 1.48
11 -2 -4 7.22 1.25
11 -2 4 9.05 1.19
-11 2 -5 0.13 0.84
11 2 5 0.26 1.12
11 -2 -5 -0.11 0.89
11 2 6 54.37 3.08
11 -2 -6 45.23 2.72
11 2 7 1.86 1.13
11 -2 -7 0.55 0.88
11 -2 8 1.53 0.87
11 2 8 1.98 1.08
11 -2 8 1.55 1.01
11 -2 9 2.91 0.89
11 -2 9 3.02 1.02
11 -2 10 9.28 1.13
11 -2 10 11.83 1.34
11 -2 11 1.00 0.72
11 -2 11 2.30 0.85
11 -2 12 69.40 2.94
11 -2 12 69.67 3.12
11 -2 13 0.16 0.62
11 -2 13 0.20 0.72
11 -2 14 63.15 2.59
11 -3 0 0.11 0.90
11 -3 -1 86.28 3.94
11 -3 1 82.58 3.85
11 -3 -2 2.03 0.97
11 -3 2 1.41 0.90
11 -3 -3 52.31 2.82
11 -3 3 45.16 2.56
11 -3 -4 2.88 0.91
11 -3 4 2.82 0.92
11 -3 -5 134.87 5.26
11 -3 5 119.28 4.91
11 -3 -6 3.94 1.00
11 -3 6 3.47 0.82
11 -3 7 16.95 1.45
11 -3 -7 17.00 1.57
11 -3 8 10.01 1.17
11 -3 8 9.89 1.28
11 -3 -8 13.42 1.36
11 -3 9 102.84 4.14
11 -3 9 108.17 4.34
11 -3 10 1.09 0.71
11 -3 10 1.96 0.82
11 -3 11 8.50 0.95
11 -3 11 7.69 1.03
11 -3 12 1.95 0.68
11 -3 13 92.55 3.48
11 -4 0 0.98 0.81
11 -4 -1 0.59 0.83
11 -4 1 0.38 0.82
11 -4 -2 22.88 1.75
11 -4 2 23.12 1.75
11 -4 -3 0.19 0.83
11 -4 3 0.36 0.76
11 -4 -4 0.64 0.78
11 -4 4 0.68 0.73
11 -4 -5 6.92 1.06
11 -4 5 6.04 0.96
11 -4 6 0.48 0.80
11 -4 -6 0.26 0.74
11 -4 6 -0.35 0.65
11 -4 7 2.42 0.85
11 -4 -7 1.30 0.77
11 -4 7 1.99 0.67
11 -4 8 28.46 1.72
11 -4 8 29.62 1.78
11 -4 -8 33.85 1.89
11 -4 9 -0.11 0.66
11 -4 9 -0.35 0.65
11 -4 10 52.43 2.30
11 -5 0 -0.16 0.70
11 -5 -1 95.01 3.85
11 -5 1 89.52 3.79
11 -5 -2 6.07 0.96
11 -5 2 6.69 0.98
11 -5 -3 14.52 1.25
11 -5 3 13.01 1.20
11 -5 -4 5.55 0.90
11 -5 4 4.72 0.86
11 -5 -5 70.09 2.96
11 -5 5 67.07 2.92
11 -5 -6 0.87 0.62
12 0 0 14.13 1.67
12 0 1 1.17 1.10
12 0 -1 1.01 1.11
12 0 2 4.91 1.28
12 0 -2 6.03 1.27
12 0 3 1.26 1.10
12 0 -3 -0.58 1.08
12 0 4 10.60 1.47
12 0 5 -0.43 1.03
12 0 6 0.31 1.03
12 0 7 0.58 0.95
12 0 8 21.07 1.71
12 0 9 0.17 0.84
12 0 10 31.94 1.94
12 0 11 0.74 0.73
12 1 0 49.57 2.86
12 1 -1 55.10 3.07
12 1 1 61.80 3.25
12 -1 1 66.89 3.38
12 1 2 182.64 6.88
12 -1 2 164.39 6.75
12 1 3 108.80 4.74
12 -1 3 103.36 4.67
12 1 4 87.00 3.98
12 -1 4 77.69 3.78
12 1 5 37.94 2.45
12 -1 5 35.91 2.30
12 1 6 164.16 6.49
12 -1 6 169.95 6.44
12 1 7 124.15 5.04
12 -1 7 117.68 4.89
12 1 8 26.22 1.90
12 -1 8 30.08 1.94
12 1 9 5.46 1.05
12 -1 9 4.99 1.03
12 -1 10 168.76 6.19
12 -1 11 82.49 3.41
12 -2 0 18.02 1.50
12 -2 -1 0.45 0.80
12 -2 1 -0.75 0.82
12 2 2 2.91 1.06
12 -2 -2 2.68 0.88
12 -2 2 1.72 0.85
12 2 3 0.65 0.97
12 -2 -3 1.51 0.89
12 -2 4 16.93 1.60
12 -2 5 1.20 0.85
12 -2 6 15.83 1.48
12 -2 7 0.41 0.80
12 -2 8 5.09 0.95
12 -2 9 0.71 0.78
12 -2 10 0.38 0.73
12 -3 0 104.45 4.25
12 -3 -1 56.58 2.74
12 -3 1 55.10 2.66
12 -3 -2 163.76 5.90
12 -3 2 145.55 5.63
12 -3 -3 70.56 3.13
12 -3 3 61.68 2.83
12 -3 -4 20.23 1.58
12 -3 4 15.42 1.24
12 -3 5 20.22 1.56
12 -3 -5 19.92 1.55
12 -3 6 157.39 5.82
12 -3 7 59.97 2.72
12 -3 8 47.56 2.27
12 -4 0 19.90 1.41
12 -4 -1 0.97 0.70
12 -4 1 0.13 0.67
12 -4 -2 3.81 0.82
12 -4 -3 0.90 0.65
12 -4 -4 15.28 1.26
12 -4 -5 1.19 0.65
13 0 0 0.74 0.88
13 0 1 0.78 0.88
13 0 2 134.96 5.22
13 0 3 -0.08 0.92
13 0 4 0.08 0.86
13 0 5 -1.25 0.87
13 0 6 50.30 2.44
13 -1 0 0.16 0.84
13 -1 1 8.15 1.21
13 -1 -1 8.65 1.19
13 -1 2 0.32 0.90
13 -1 3 1.71 0.93
13 -1 4 -0.75 0.91
13 -1 5 22.32 1.57
13 -1 6 2.99 0.85
13 -2 0 -0.43 0.85
13 -2 1 2.61 0.88
13 -2 2 75.57 3.26
13 -2 3 0.89 0.79
0 0 0 0.00 0.00
TITL Oct_Sample12 in Pbca
REM Pbca (#61, found as Pcab in ba-c setting)
CELL 1.54184 11.039248 8.175612 23.367346 90.0000 90.0000 90.0000
ZERR 9.00 0.000249 0.000171 0.000448 0.0000 0.0000 0.0000
LATT 1
SYMM -x+1/2,-y, z+1/2
SYMM -x, y+1/2,-z+1/2
SYMM x+1/2,-y+1/2,-z
SFAC C H N S I
UNIT 72.00 36.00 18.00 9.00 18.00
SIZE 0.03 0.05 0.06
TREF
HKLF 4
END
_computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)'
;
_shelx_hkl_checksum 97206
_shelx_res_file
;
TITL oct_sample12_a.res in Pbca
oct_sample12.res
created by SHELXL-2018/3 at 11:48:22 on 04-Aug-2022
REM Old TITL oct_sample12_a.res in Pbca
REM SHELXT solution in Pbca: R1 0.062, Rweak 0.001, Alpha 0.016
REM 0.916 for 320 systematic absences, Orientation as input
REM Formula found by SHELXT: C10 I2 S
CELL 1.54184 11.0392 8.1756 23.3673 90 90 90
ZERR 8 0.0002 0.0002 0.0004 0 0 0
LATT 1
SYMM 0.5-X,-Y,0.5+Z
SYMM -X,0.5+Y,0.5-Z
SYMM 0.5+X,0.5-Y,-Z
SFAC C H I N S
UNIT 64 32 16 16 8
L.S. 10
PLAN 4
CONF
BOND
list 4
MORE -1
BOND $H
fmap 2
acta
REM
REM
REM
WGHT 0.038800 4.615300
FVAR 0.11194
C1 1 0.645534 0.401456 0.406753 11.00000 0.02098 0.01800 =
0.01977 -0.00031 0.00060 -0.00003
C2 1 0.528396 0.453992 0.395442 11.00000 0.01930 0.02020 =
0.02326 -0.00207 0.00161 -0.00043
AFIX 43
H2 2 0.465059 0.421230 0.419049 11.00000 -1.20000
AFIX 0
C3 1 0.505400 0.555583 0.348868 11.00000 0.02083 0.02047 =
0.02080 0.00020 0.00009 0.00202
AFIX 43
H3 2 0.427089 0.591795 0.341467 11.00000 -1.20000
AFIX 0
C4 1 0.600608 0.602372 0.313535 11.00000 0.02819 0.01629 =
0.02078 -0.00014 0.00047 0.00164
C5 1 0.718617 0.551445 0.324468 11.00000 0.02734 0.01905 =
0.02704 -0.00577 0.00667 -0.00203
AFIX 43
H5 2 0.782009 0.584936 0.301019 11.00000 -1.20000
AFIX 0
C6 1 0.740184 0.449777 0.370974 11.00000 0.02057 0.01715 =
0.02812 -0.00520 0.00264 -0.00103
AFIX 43
H6 2 0.818500 0.413535 0.378344 11.00000 -1.20000
AFIX 0
C7 1 0.671153 0.297410 0.456536 11.00000 0.02186 0.01936 =
0.02024 0.00021 -0.00086 -0.00138
N8 4 0.780092 0.252480 0.471008 11.00000 0.02104 0.02741 =
0.02409 0.00228 -0.00221 0.00147
N9 4 0.782719 0.158349 0.520105 11.00000 0.02358 0.02714 =
0.02229 0.00147 -0.00209 0.00367
C10 1 0.674500 0.137166 0.540447 11.00000 0.02163 0.01779 =
0.02415 -0.00230 -0.00401 0.00026
S11 5 0.559403 0.228501 0.502826 11.00000 0.01868 0.02832 =
0.02665 0.00531 -0.00037 0.00128
I12 3 0.640842 0.009121 0.615901 11.00000 0.02787 0.02557 =
0.02293 0.00194 -0.00234 0.00177
I13 3 0.563749 0.751476 0.242721 11.00000 0.03494 0.02059 =
0.02173 0.00162 -0.00195 -0.00176
HKLF 4
REM oct_sample12_a.res in Pbca
REM wR2 = 0.0709, GooF = S = 1.088, Restrained GooF = 1.088 for all data
REM R1 = 0.0262 for 1753 Fo > 4sig(Fo) and 0.0293 for all 1942 data
REM 118 parameters refined using 0 restraints
END
WGHT 0.0388 4.6152
REM Highest difference peak 1.328, deepest hole -1.221, 1-sigma level 0.148
Q1 1 0.6279 -0.0676 0.6483 11.00000 0.05 1.33
Q2 1 0.5389 0.8267 0.2672 11.00000 0.05 0.58
Q3 1 0.5686 0.8223 0.2165 11.00000 0.05 0.57
Q4 1 0.4729 0.7485 0.2430 11.00000 0.05 0.54
;
_shelx_res_checksum 13062
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'
'-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
C C1 0.6455(4) 0.4015(5) 0.40675(18) 0.0196(9) Uani d 1 . .
C C2 0.5284(4) 0.4540(6) 0.39544(19) 0.0209(9) Uani d 1 . .
H H2 0.465059 0.421230 0.419049 0.025 Uiso calc 1 . .
C C3 0.5054(4) 0.5556(5) 0.34887(18) 0.0207(9) Uani d 1 . .
H H3 0.427089 0.591795 0.341467 0.025 Uiso calc 1 . .
C C4 0.6006(4) 0.6024(5) 0.31353(18) 0.0218(9) Uani d 1 . .
C C5 0.7186(4) 0.5514(5) 0.32447(19) 0.0245(10) Uani d 1 . .
H H5 0.782009 0.584936 0.301019 0.029 Uiso calc 1 . .
C C6 0.7402(4) 0.4498(6) 0.37097(18) 0.0219(9) Uani d 1 . .
H H6 0.818500 0.413535 0.378344 0.026 Uiso calc 1 . .
C C7 0.6712(4) 0.2974(5) 0.45654(18) 0.0205(9) Uani d 1 . .
N N8 0.7801(3) 0.2525(4) 0.47101(17) 0.0242(9) Uani d 1 . .
N N9 0.7827(3) 0.1583(5) 0.52011(16) 0.0243(8) Uani d 1 . .
C C10 0.6745(4) 0.1372(5) 0.54045(18) 0.0212(9) Uani d 1 . .
S S11 0.55940(10) 0.22850(15) 0.50283(5) 0.0246(3) Uani d 1 . .
I I12 0.64084(3) 0.00912(3) 0.61590(2) 0.02546(12) Uani d 1 . .
I I13 0.56375(3) 0.75148(3) 0.24272(2) 0.02576(12) Uani d 1 . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
C1 0.021(2) 0.018(2) 0.020(2) 0.0000(17) 0.0006(17) -0.0003(18)
C2 0.019(2) 0.020(2) 0.023(2) -0.0004(18) 0.0016(18) -0.0021(18)
C3 0.021(2) 0.020(2) 0.021(2) 0.0020(18) 0.0001(18) 0.0002(18)
C4 0.028(2) 0.0163(19) 0.021(2) 0.0016(18) 0.0005(19) -0.0001(17)
C5 0.027(2) 0.019(2) 0.027(2) -0.0020(19) 0.0067(18) -0.0058(19)
C6 0.021(2) 0.017(2) 0.028(2) -0.0010(18) 0.0026(19) -0.0052(18)
C7 0.022(2) 0.019(2) 0.020(2) -0.0014(18) -0.0009(18) 0.0002(18)
N8 0.021(2) 0.027(2) 0.0241(19) 0.0015(16) -0.0022(15) 0.0023(16)
N9 0.024(2) 0.027(2) 0.0223(17) 0.0037(17) -0.0021(16) 0.0015(16)
C10 0.022(2) 0.018(2) 0.024(2) 0.0003(18) -0.0040(19) -0.0023(18)
S11 0.0187(6) 0.0283(6) 0.0267(6) 0.0013(4) -0.0004(4) 0.0053(5)
I12 0.0279(2) 0.02557(18) 0.02293(18) 0.00177(11) -0.00234(11) 0.00194(11)
I13 0.0349(2) 0.02059(18) 0.02173(18) -0.00176(11) -0.00195(11) 0.00162(11)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.3257 6.8362 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 '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
-2 0 1 0.0191
2 0 -1 0.0401
1 4 1 0.0265
-1 0 -5 0.0202
1 0 5 0.0067
1 4 11 0.0191
-1 -4 -11 0.0172
0 0 1 0.0081
0 0 -1 0.0256
0 -1 2 0.0194
-1 0 5 0.0085
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
C2 C1 C6 . . 119.7(4) ?
C2 C1 C7 . . 120.6(4) ?
C6 C1 C7 . . 119.6(4) ?
C1 C2 H2 . . 119.9 ?
C1 C2 C3 . . 120.2(4) ?
C3 C2 H2 . . 119.9 ?
C2 C3 H3 . . 120.3 ?
C4 C3 C2 . . 119.4(4) ?
C4 C3 H3 . . 120.3 ?
C3 C4 C5 . . 121.1(4) ?
C3 C4 I13 . . 118.8(3) ?
C5 C4 I13 . . 120.1(3) ?
C4 C5 H5 . . 120.5 ?
C6 C5 C4 . . 118.9(4) ?
C6 C5 H5 . . 120.5 ?
C1 C6 H6 . . 119.7 ?
C5 C6 C1 . . 120.7(4) ?
C5 C6 H6 . . 119.7 ?
C1 C7 S11 . . 123.0(3) ?
N8 C7 C1 . . 123.2(4) ?
N8 C7 S11 . . 113.8(3) ?
C7 N8 N9 . . 113.1(4) ?
C10 N9 N8 . . 111.1(3) ?
N9 C10 S11 . . 115.9(3) ?
N9 C10 I12 . . 122.8(3) ?
S11 C10 I12 . . 121.3(2) ?
C10 S11 C7 . . 86.2(2) ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
C1 C2 . 1.388(6) ?
C1 C6 . 1.395(6) ?
C1 C7 . 1.469(6) ?
C2 H2 . 0.9300 ?
C2 C3 . 1.392(6) ?
C3 H3 . 0.9300 ?
C3 C4 . 1.390(6) ?
C4 C5 . 1.391(6) ?
C4 I13 . 2.095(4) ?
C5 H5 . 0.9300 ?
C5 C6 . 1.389(6) ?
C6 H6 . 0.9300 ?
C7 N8 . 1.302(6) ?
C7 S11 . 1.735(4) ?
N8 N9 . 1.382(5) ?
N9 C10 . 1.297(6) ?
C10 S11 . 1.716(4) ?
C10 I12 . 2.084(4) ?
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
C1 C2 C3 C4 . . . . 0.7(7) ?
C1 C7 N8 N9 . . . . 178.4(4) ?
C1 C7 S11 C10 . . . . -178.5(4) ?
C2 C1 C6 C5 . . . . 0.7(7) ?
C2 C1 C7 N8 . . . . -175.9(4) ?
C2 C1 C7 S11 . . . . 1.9(6) ?
C2 C3 C4 C5 . . . . -1.0(6) ?
C2 C3 C4 I13 . . . . 178.8(3) ?
C3 C4 C5 C6 . . . . 1.2(6) ?
C4 C5 C6 C1 . . . . -1.0(7) ?
C6 C1 C2 C3 . . . . -0.5(7) ?
C6 C1 C7 N8 . . . . 3.2(7) ?
C6 C1 C7 S11 . . . . -179.0(3) ?
C7 C1 C2 C3 . . . . 178.6(4) ?
C7 C1 C6 C5 . . . . -178.4(4) ?
C7 N8 N9 C10 . . . . -0.1(5) ?
N8 C7 S11 C10 . . . . -0.4(4) ?
N8 N9 C10 S11 . . . . -0.2(5) ?
N8 N9 C10 I12 . . . . -177.7(3) ?
N9 C10 S11 C7 . . . . 0.3(4) ?
S11 C7 N8 N9 . . . . 0.4(5) ?
I12 C10 S11 C7 . . . . 177.9(3) ?
I13 C4 C5 C6 . . . . -178.6(3) ?