#------------------------------------------------------------------------------
#$Date: 2024-11-01 03:54:44 +0100 (Fri, 01 Nov 2024) $
#$Revision: 295710 $
#$URL: svn://www.crystallography.net/cod/cif/2/02/32/2023296.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_2023296
loop_
_publ_author_name
'Mukda, Benjamin A.'
'Dickie, Diane A.'
'Turnbull, Mark M.'
_publ_section_title
;
Salts of 2-amino-5-iodopyridinium
;
_journal_issue 11
_journal_name_full
'Acta Crystallographica Section E Crystallographic Communications'
_journal_page_first 1230
_journal_page_last 1234
_journal_paper_doi 10.1107/S2056989024010259
_journal_volume 80
_journal_year 2024
_chemical_formula_iupac 'C5 H6 I N2 +, Br -'
_chemical_formula_moiety 'C5 H6 I N2 +, Br -'
_chemical_formula_sum 'C5 H6 Br I N2'
_chemical_formula_weight 300.93
_chemical_name_systematic
;
2-Amino-5-iodopyridinium bromide
;
_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 mixed
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_audit_creation_method SHELXL-2019/3
_cell_angle_alpha 93.3762(12)
_cell_angle_beta 104.1108(11)
_cell_angle_gamma 96.4297(12)
_cell_formula_units_Z 2
_cell_length_a 5.2152(2)
_cell_length_b 7.8039(3)
_cell_length_c 10.1294(4)
_cell_measurement_reflns_used 9950
_cell_measurement_temperature 100(2)
_cell_measurement_theta_max 30.51
_cell_measurement_theta_min 2.64
_cell_volume 395.71(3)
_computing_cell_refinement
;
SAINT V8.40B (Bruker, 2022)
;
_computing_data_collection
;
Bruker Instrument Service v8.5.0.27 & APEX4 v2022.10-1 (Bruker, 2022)
;
_computing_data_reduction
;
SAINT 8.40B (Bruker, 2022)
;
_computing_structure_refinement
;
SHELXL2019/2 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS2014 (Sheldrick 2008)
;
_diffrn_ambient_temperature 100(2)
_diffrn_detector CPAD
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device 'Kappa four-circle diffractometer'
_diffrn_measurement_device_type 'Bruker D8 VENTURE dual wavelength Mo/Cu'
_diffrn_measurement_method '\f and \w scans'
_diffrn_radiation_monochromator 'HELIOS double bounce multilayer mirror'
_diffrn_radiation_probe x-ray
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0249
_diffrn_reflns_av_unetI/netI 0.0199
_diffrn_reflns_limit_h_max 7
_diffrn_reflns_limit_h_min -7
_diffrn_reflns_limit_k_max 11
_diffrn_reflns_limit_k_min -11
_diffrn_reflns_limit_l_max 13
_diffrn_reflns_limit_l_min -14
_diffrn_reflns_number 13418
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 30.506
_diffrn_reflns_theta_min 2.081
_diffrn_source 'microfocus sealed X-ray tube'
_exptl_absorpt_coefficient_mu 9.012
_exptl_absorpt_correction_T_max 0.7461
_exptl_absorpt_correction_T_min 0.6046
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
(SADABS; Krause et al., 2015)
;
_exptl_crystal_colour yellow
_exptl_crystal_density_diffrn 2.526
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description block
_exptl_crystal_F_000 276
_exptl_crystal_size_max 0.241
_exptl_crystal_size_mid 0.205
_exptl_crystal_size_min 0.076
_refine_diff_density_max 0.482
_refine_diff_density_min -0.501
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.106
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 91
_refine_ls_number_reflns 2412
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.106
_refine_ls_R_factor_all 0.0129
_refine_ls_R_factor_gt 0.0124
_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^)+0.2575P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0287
_refine_ls_wR_factor_ref 0.0289
_reflns_number_gt 2346
_reflns_number_total 2412
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file zn2039.cif
_cod_data_source_block 1
_cod_database_code 2023296
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min 0.220
_shelx_estimated_absorpt_t_max 0.548
_shelx_hkl_file
;
-1 0 0 94.97 4.69
-2 0 0 390.19 15.63
2 0 0 384.57 15.60
-3 0 0 175.05 5.50
-3 0 0 187.26 5.53
-3 0 0 181.67 5.52
3 0 0 186.12 5.45
3 0 0 183.22 5.52
3 0 0 180.18 5.50
3 0 0 184.78 5.45
3 0 0 186.42 5.38
3 0 0 174.01 5.49
-4 0 0 9.68 0.53
-4 0 0 10.79 0.52
-4 0 0 9.85 0.48
-4 0 0 9.30 0.44
-4 0 0 9.91 0.51
4 0 0 8.90 0.43
4 0 0 9.33 0.33
4 0 0 8.77 0.43
4 0 0 9.10 0.49
4 0 0 8.75 0.32
-5 0 0 0.89 0.24
-5 0 0 1.49 0.29
-5 0 0 1.44 0.29
-5 0 0 1.60 0.22
-5 0 0 1.21 0.26
5 0 0 1.40 0.26
5 0 0 1.76 0.29
-6 0 0 12.93 0.71
-6 0 0 12.32 0.74
-6 0 0 12.12 0.77
6 0 0 12.63 0.75
6 0 0 12.09 0.70
-7 0 0 11.16 0.85
-7 0 0 11.62 0.78
-7 0 0 12.26 0.81
7 0 0 11.13 0.97
7 -1 0 32.35 1.25
-7 1 0 31.88 1.35
-7 1 0 30.24 1.46
-7 1 0 30.20 1.40
6 -1 0 4.74 0.43
-6 1 0 4.78 0.51
-6 1 0 4.15 0.45
5 -1 0 174.82 5.10
5 -1 0 153.97 5.14
5 -1 0 161.87 4.99
-5 1 0 168.80 5.16
-5 1 0 166.91 5.17
-5 1 0 164.86 5.19
-5 1 0 161.78 5.09
4 -1 0 186.65 5.71
4 -1 0 191.41 5.69
4 -1 0 195.17 5.79
4 -1 0 176.45 5.80
-4 1 0 195.53 5.82
-4 1 0 194.81 5.85
-4 1 0 186.99 6.01
-4 1 0 194.90 5.83
3 -1 0 48.67 1.51
3 -1 0 48.49 1.58
3 -1 0 47.61 1.54
3 -1 0 46.60 1.58
3 -1 0 47.61 1.60
3 -1 0 50.62 1.48
-3 1 0 51.10 1.51
-3 1 0 47.19 1.60
-3 1 0 49.99 1.61
-3 1 0 49.28 1.56
-3 1 0 48.16 1.60
-3 1 0 47.09 1.61
-2 1 0 526.83 19.73
1 -1 0 0.27 0.05
1 -1 0 0.35 0.05
1 -1 0 0.17 0.04
-1 1 0 0.21 0.05
-1 1 0 0.29 0.05
-1 1 0 0.29 0.05
-1 1 0 0.40 0.06
-1 1 0 0.31 0.05
-1 1 0 0.29 0.04
0 -1 0 32.52 0.99
0 -1 0 32.46 1.00
0 -1 0 33.77 1.01
0 -1 0 31.32 0.99
0 -1 0 33.42 1.00
0 1 0 34.64 1.01
0 1 0 33.02 1.00
0 1 0 33.79 0.99
0 1 0 30.82 1.00
0 1 0 32.54 0.99
-1 -1 0 34.83 1.13
-1 -1 0 36.42 1.17
-1 -1 0 36.20 1.13
-1 -1 0 37.31 1.15
1 1 0 36.74 1.13
1 1 0 35.23 1.13
1 1 0 37.40 1.15
1 1 0 37.03 1.14
1 1 0 35.52 1.14
-2 -1 0 84.83 2.57
-2 -1 0 86.34 2.58
-2 -1 0 82.58 2.58
-2 -1 0 83.87 2.60
-2 -1 0 81.58 2.60
-2 -1 0 84.42 2.59
2 1 0 81.92 2.60
2 1 0 83.70 2.57
2 1 0 85.78 2.59
2 1 0 84.49 2.59
2 1 0 84.28 2.56
-3 -1 0 28.59 1.06
-3 -1 0 30.57 1.03
-3 -1 0 29.69 1.04
-3 -1 0 31.63 1.04
-3 -1 0 29.59 1.07
3 1 0 29.79 1.01
3 1 0 28.26 0.94
3 1 0 29.55 1.06
3 1 0 27.80 1.06
3 1 0 30.11 1.06
3 1 0 28.19 1.05
-4 -1 0 200.11 5.84
-4 -1 0 189.90 5.91
-4 -1 0 200.17 5.89
-4 -1 0 178.20 5.89
-4 -1 0 198.26 5.86
4 1 0 186.02 5.72
4 1 0 189.36 5.89
4 1 0 188.61 5.70
4 1 0 199.40 5.93
-5 -1 0 162.92 5.01
-5 -1 0 150.74 5.11
-5 -1 0 163.54 5.09
-5 -1 0 168.22 5.06
-5 -1 0 162.95 5.15
5 1 0 165.69 5.14
5 1 0 162.82 5.08
-6 -1 0 8.09 0.64
-6 -1 0 8.25 0.60
-6 -1 0 7.82 0.58
6 1 0 9.09 0.62
6 1 0 7.20 0.61
-7 -1 0 74.07 2.61
-7 -1 0 70.71 2.72
-7 -1 0 72.38 2.64
7 1 0 72.96 2.55
7 -2 0 58.33 1.94
-7 2 0 56.38 2.12
-7 2 0 54.61 2.23
-7 2 0 61.41 2.24
-6 2 0 33.21 1.34
-6 2 0 34.32 1.39
-6 2 0 32.24 1.42
5 -2 0 25.13 1.01
5 -2 0 23.70 0.83
5 -2 0 24.97 1.03
-5 2 0 24.76 1.04
-5 2 0 23.62 1.02
-5 2 0 24.44 0.97
-5 2 0 23.15 1.05
4 -2 0 56.04 1.94
4 -2 0 57.54 1.75
4 -2 0 59.76 1.89
4 -2 0 56.41 1.77
-4 2 0 56.12 1.89
-4 2 0 57.60 2.04
-4 2 0 57.96 1.95
-4 2 0 59.26 1.98
3 -2 0 15.29 0.58
3 -2 0 14.09 0.59
3 -2 0 13.37 0.59
3 -2 0 15.24 0.48
3 -2 0 15.24 0.55
3 -2 0 14.59 0.61
-3 2 0 14.14 0.61
-3 2 0 14.63 0.62
-3 2 0 14.86 0.57
-3 2 0 14.60 0.53
-3 2 0 15.80 0.62
-3 2 0 14.76 0.62
2 -2 0 20.83 0.75
2 -2 0 20.74 0.74
2 -2 0 20.73 0.71
2 -2 0 20.56 0.69
2 -2 0 22.36 0.75
2 -2 0 20.94 0.73
-2 2 0 20.14 0.76
-2 2 0 20.38 0.74
-2 2 0 21.05 0.74
-2 2 0 22.24 0.72
-2 2 0 21.39 0.71
-2 2 0 20.32 0.74
1 -2 0 25.74 0.75
1 -2 0 21.77 0.76
1 -2 0 23.50 0.70
1 -2 0 23.57 0.76
1 -2 0 22.89 0.76
1 -2 0 23.16 0.78
-1 2 0 23.47 0.76
-1 2 0 22.41 0.75
-1 2 0 22.56 0.77
-1 2 0 23.67 0.70
-1 2 0 20.76 0.77
-1 2 0 22.82 0.76
0 -2 0 722.30 24.59
0 2 0 740.92 24.62
-1 -2 0 142.21 4.28
-2 -2 0 333.10 15.53
-2 -2 0 373.04 16.19
-3 -2 0 242.14 6.98
-3 -2 0 241.19 7.03
3 2 0 217.33 6.93
3 2 0 230.28 6.89
3 2 0 241.78 7.01
3 2 0 232.56 7.04
3 2 0 239.89 7.04
3 2 0 209.87 6.95
-4 -2 0 42.83 1.56
-4 -2 0 42.95 1.50
-4 -2 0 42.55 1.55
-4 -2 0 43.82 1.50
-4 -2 0 44.51 1.51
4 2 0 40.23 1.37
4 2 0 42.72 1.54
4 2 0 40.71 1.55
-5 -2 0 44.78 1.73
-5 -2 0 48.87 1.65
-5 -2 0 40.23 1.69
-5 -2 0 46.46 1.66
-5 -2 0 47.55 1.68
5 2 0 48.90 1.72
5 2 0 45.29 1.47
5 2 0 42.69 1.44
5 2 0 44.46 1.72
-6 -2 0 0.96 0.27
-6 -2 0 0.89 0.27
-6 -2 0 0.91 0.33
-6 -2 0 1.00 0.31
6 2 0 0.65 0.28
6 2 0 0.72 0.33
-7 3 0 0.95 0.35
-7 3 0 1.26 0.34
-7 3 0 0.85 0.32
6 -3 0 1.01 0.20
-6 3 0 1.29 0.33
-6 3 0 0.98 0.29
-6 3 0 0.90 0.32
5 -3 0 44.51 1.51
5 -3 0 45.32 1.66
-5 3 0 45.06 1.66
-5 3 0 46.32 1.62
-5 3 0 47.49 1.70
-5 3 0 46.18 1.73
4 -3 0 79.79 2.49
4 -3 0 81.11 2.46
4 -3 0 81.84 2.52
4 -3 0 81.02 2.61
-4 3 0 77.24 2.48
-4 3 0 79.48 2.62
-4 3 0 79.61 2.62
-4 3 0 81.37 2.66
3 -3 0 120.47 3.69
3 -3 0 124.93 3.71
3 -3 0 123.53 3.78
3 -3 0 124.40 3.70
-3 3 0 114.38 3.78
-3 3 0 122.79 3.79
-3 3 0 126.20 3.80
-3 3 0 124.54 3.72
-3 3 0 122.72 3.82
-3 3 0 119.53 3.73
2 -3 0 580.44 22.44
-2 3 0 562.06 22.54
1 -3 0 0.96 0.13
1 -3 0 1.48 0.09
1 -3 0 1.20 0.11
1 -3 0 1.20 0.13
1 -3 0 1.29 0.11
1 -3 0 1.12 0.11
-1 3 0 1.07 0.12
-1 3 0 1.18 0.12
-1 3 0 1.19 0.12
-1 3 0 1.22 0.12
-1 3 0 1.16 0.12
-1 3 0 1.18 0.14
0 -3 0 691.27 24.93
0 3 0 682.31 24.69
-1 -3 0 83.61 2.60
-1 -3 0 87.44 2.62
-1 -3 0 79.91 2.57
-1 -3 0 83.63 2.58
-1 -3 0 86.41 2.57
1 3 0 82.16 2.58
1 3 0 80.59 2.56
1 3 0 86.60 2.62
1 3 0 81.21 2.57
1 3 0 83.79 2.59
1 3 0 82.96 2.59
-2 -3 0 74.03 2.45
-2 -3 0 79.61 2.45
-2 -3 0 77.90 2.50
-2 -3 0 78.60 2.47
2 3 0 77.33 2.42
2 3 0 77.36 2.43
2 3 0 76.37 2.47
2 3 0 74.60 2.45
2 3 0 81.12 2.51
2 3 0 80.95 2.49
-3 -3 0 8.57 0.51
-3 -3 0 9.90 0.50
-3 -3 0 9.67 0.53
-3 -3 0 9.83 0.48
-3 -3 0 10.13 0.51
3 3 0 9.80 0.52
3 3 0 9.08 0.43
3 3 0 9.79 0.54
-4 -3 0 13.04 0.64
-4 -3 0 13.06 0.65
-4 -3 0 14.00 0.71
-4 -3 0 13.73 0.67
-4 -3 0 13.37 0.71
4 3 0 13.53 0.69
4 3 0 12.96 0.71
4 3 0 12.24 0.55
-5 -3 0 30.96 1.26
-5 -3 0 31.71 1.25
-5 -3 0 30.53 1.25
-5 -3 0 31.74 1.35
5 3 0 30.77 1.33
5 3 0 31.50 1.16
5 3 0 32.81 1.31
5 3 0 29.08 1.09
-6 -3 0 0.21 0.25
-6 -3 0 0.26 0.26
-6 -3 0 0.03 0.29
-6 -3 0 -0.19 0.23
6 3 0 0.10 0.28
6 3 0 0.49 0.31
-7 4 0 65.42 2.33
-7 4 0 60.04 2.80
-6 4 0 31.38 1.40
-6 4 0 32.07 1.36
5 -4 0 106.10 3.47
5 -4 0 113.08 3.33
-5 4 0 106.83 3.49
-5 4 0 110.33 3.45
-5 4 0 101.15 3.28
-5 4 0 108.95 3.51
-5 4 0 104.94 3.55
4 -4 0 136.27 4.06
4 -4 0 137.73 4.08
4 -4 0 129.96 4.17
4 -4 0 133.69 4.07
-4 4 0 133.26 4.20
-4 4 0 134.29 4.21
-4 4 0 132.06 4.10
-4 4 0 131.71 4.25
-4 4 0 136.05 4.16
3 -4 0 0.78 0.13
3 -4 0 0.58 0.13
3 -4 0 0.48 0.13
-3 4 0 0.55 0.15
-3 4 0 0.68 0.17
-3 4 0 0.64 0.15
-3 4 0 0.75 0.16
-3 4 0 0.58 0.13
2 -4 0 101.81 3.05
2 -4 0 100.46 3.04
2 -4 0 100.23 3.10
2 -4 0 100.13 2.97
2 -4 0 98.46 3.09
2 -4 0 103.93 3.10
2 -4 0 98.17 3.12
-2 4 0 101.36 3.13
-2 4 0 96.34 3.10
-2 4 0 101.35 3.10
-2 4 0 100.59 3.09
-2 4 0 97.69 3.16
1 -4 0 0.67 0.11
1 -4 0 1.01 0.16
1 -4 0 0.44 0.11
1 -4 0 0.62 0.11
1 -4 0 0.72 0.10
-1 4 0 0.76 0.09
-1 4 0 0.53 0.11
-1 4 0 0.55 0.10
-1 4 0 0.46 0.11
-1 4 0 0.49 0.12
-1 4 0 0.58 0.11
0 -4 0 34.20 1.10
0 -4 0 34.05 1.14
0 -4 0 32.58 1.13
0 -4 0 31.57 1.15
0 -4 0 31.83 1.07
0 -4 0 32.48 1.10
0 -4 0 31.95 1.09
0 4 0 33.65 1.16
0 4 0 33.85 1.13
0 4 0 31.70 1.09
0 4 0 32.09 1.08
0 4 0 33.31 1.09
0 4 0 34.17 1.13
-1 -4 0 1.78 0.19
-1 -4 0 1.92 0.23
-1 -4 0 1.43 0.17
-1 -4 0 1.50 0.14
-1 -4 0 1.46 0.19
1 4 0 1.50 0.20
1 4 0 1.65 0.19
1 4 0 1.15 0.16
1 4 0 1.32 0.19
1 4 0 1.45 0.18
1 4 0 1.71 0.18
-2 -4 0 195.67 5.77
-2 -4 0 185.36 5.71
-2 -4 0 189.39 5.69
-2 -4 0 193.20 5.75
2 4 0 191.30 5.73
2 4 0 177.26 5.72
2 4 0 178.75 5.67
2 4 0 189.82 5.76
-3 -4 0 137.28 4.23
-3 -4 0 137.44 4.32
-3 -4 0 134.69 4.28
-3 -4 0 141.01 4.27
-3 -4 0 131.12 4.32
3 4 0 138.94 4.32
3 4 0 137.78 4.34
-4 -4 0 70.15 2.40
-4 -4 0 66.78 2.28
-4 -4 0 68.69 2.31
-4 -4 0 66.99 2.33
4 4 0 68.22 2.37
4 4 0 67.84 2.40
-5 -4 0 120.14 3.85
-5 -4 0 117.37 3.95
-5 -4 0 118.27 3.81
5 4 0 115.55 3.94
-6 -4 0 2.23 0.44
-6 -4 0 2.14 0.41
-6 -4 0 2.64 0.45
-6 -4 0 2.05 0.37
6 4 0 2.62 0.47
6 -5 0 18.23 0.70
-6 5 0 16.77 0.87
-6 5 0 17.19 0.92
-6 5 0 16.30 0.96
5 -5 0 5.62 0.33
-5 5 0 6.06 0.45
-5 5 0 4.46 0.43
-5 5 0 5.58 0.47
-5 5 0 5.32 0.61
-5 5 0 5.07 0.35
4 -5 0 2.98 0.30
4 -5 0 3.26 0.25
4 -5 0 3.46 0.29
4 -5 0 3.14 0.25
-4 5 0 3.25 0.33
-4 5 0 3.15 0.37
-4 5 0 2.90 0.28
-4 5 0 3.01 0.32
-4 5 0 3.31 0.33
3 -5 0 85.45 2.59
3 -5 0 83.14 2.51
3 -5 0 80.36 2.50
3 -5 0 81.21 2.59
-3 5 0 83.85 2.62
-3 5 0 81.84 2.64
-3 5 0 78.31 2.58
-3 5 0 80.05 2.68
-3 5 0 71.50 2.57
2 -5 0 242.74 7.01
2 -5 0 246.15 7.11
2 -5 0 235.61 7.09
2 -5 0 211.18 7.04
2 -5 0 252.19 6.97
-2 5 0 222.06 7.33
-2 5 0 240.92 6.96
-2 5 0 233.52 7.08
-2 5 0 231.83 7.12
1 -5 0 6.03 0.29
1 -5 0 5.41 0.29
1 -5 0 5.30 0.29
1 -5 0 5.09 0.33
1 -5 0 5.24 0.34
1 -5 0 5.46 0.30
-1 5 0 6.09 0.32
-1 5 0 5.35 0.33
-1 5 0 6.20 0.47
-1 5 0 5.29 0.27
-1 5 0 5.34 0.36
-1 5 0 4.88 0.30
-1 5 0 5.33 0.33
0 -5 0 455.16 13.56
-1 -5 0 130.80 3.97
-1 -5 0 123.62 3.91
-1 -5 0 133.67 4.00
-1 -5 0 120.32 4.04
-1 -5 0 132.88 4.03
1 5 0 130.19 4.02
1 5 0 130.08 4.05
1 5 0 129.06 4.01
-2 -5 0 131.42 3.99
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TITL mo_ClarkU_Turnbull_BM_I_121c_X in P-1
bm121.res
created by SHELXL-2019/3 at 15:41:10 on 07-Sep-2024
CELL 0.71073 5.21520 7.80390 10.12940 93.3762 104.1108 96.4297
ZERR 2.00 0.00020 0.00030 0.00040 0.0012 0.0011 0.0012
LATT 1
SFAC C H N BR I
UNIT 10 12 4 2 2
TEMP -173.150
SIZE 0.076 0.205 0.241
L.S. 4
ACTA
BOND $H
CONF
HTAB
HTAB N11 Br1
EQIV $1 -x, -y+1, -z
HTAB N12 Br1_$1
EQIV $2 x, y+1, z
HTAB N12 Br1_$2
WGHT 0.000000 0.257500
FVAR 0.22027
N11 3 0.594724 0.681931 0.181780 11.00000 0.01680 0.01029 =
0.01408 -0.00024 0.00346 -0.00156
H11 2 0.482421 0.603422 0.144649 11.00000 -1.20000
C12 1 0.546437 0.846050 0.163867 11.00000 0.01492 0.01210 =
0.01181 0.00050 0.00509 0.00034
N12 3 0.319604 0.878441 0.082278 11.00000 0.01496 0.01492 =
0.01707 0.00076 0.00077 -0.00005
H12A 2 0.196892 0.800779 0.034358 11.00000 -1.20000
H12B 2 0.292234 0.983443 0.080855 11.00000 -1.20000
C13 1 0.745936 0.980602 0.234854 11.00000 0.01666 0.01061 =
0.01448 0.00200 0.00289 0.00096
AFIX 43
H13 2 0.722951 1.097926 0.221414 11.00000 -1.20000
AFIX 0
C14 1 0.971091 0.942054 0.322512 11.00000 0.01490 0.01271 =
0.01474 0.00065 0.00232 -0.00050
AFIX 43
H14 2 1.103592 1.032609 0.371018 11.00000 -1.20000
AFIX 0
I15 5 1.332211 0.705186 0.486911 11.00000 0.01575 0.01769 =
0.01789 0.00494 0.00364 0.00603
C15 1 1.007536 0.767659 0.341274 11.00000 0.01540 0.01436 =
0.01359 0.00330 0.00527 0.00350
C16 1 0.817632 0.640346 0.267545 11.00000 0.01928 0.01245 =
0.01446 0.00290 0.00630 0.00285
AFIX 43
H16 2 0.841544 0.522265 0.276282 11.00000 -1.20000
AFIX 0
BR1 4 0.236273 0.311095 0.144452 11.00000 0.01538 0.01065 =
0.01964 0.00055 0.00095 -0.00109
HKLF 4
REM mo_ClarkU_Turnbull_BM_I_121c_X in P-1
REM wR2 = 0.0289, GooF = S = 1.106, Restrained GooF = 1.106 for all data
REM R1 = 0.0124 for 2346 Fo > 4sig(Fo) and 0.0129 for all 2412 data
REM 91 parameters refined using 0 restraints
END
WGHT 0.0000 0.2577
REM Instructions for potential hydrogen bonds
HTAB N11 Br1
HTAB N12 Br1_$1
HTAB N12 Br1_$2
EQIV $3 -x+2, -y+1, -z+1
HTAB C16 I15_$3
REM Highest difference peak 0.482, deepest hole -0.501, 1-sigma level 0.087
Q1 1 0.8406 0.9465 0.2764 11.00000 0.05 0.48
Q2 1 0.9955 0.8555 0.3223 11.00000 0.05 0.48
Q3 1 0.9287 0.7056 0.2860 11.00000 0.05 0.39
Q4 1 0.1713 0.3445 0.2034 11.00000 0.05 0.38
Q5 1 0.5206 1.1780 0.1502 11.00000 0.05 0.35
Q6 1 1.3521 0.8057 0.5833 11.00000 0.05 0.33
Q7 1 1.3162 0.6005 0.3252 11.00000 0.05 0.30
Q8 1 0.2594 0.2068 0.0666 11.00000 0.05 0.28
Q9 1 1.1514 0.7522 0.3899 11.00000 0.05 0.27
Q10 1 1.2533 0.7449 0.5458 11.00000 0.05 0.27
Q11 1 0.5744 0.7630 0.1714 11.00000 0.05 0.26
Q12 1 0.4365 0.8552 0.1225 11.00000 0.05 0.25
Q13 1 0.1913 0.5689 0.1579 11.00000 0.05 0.25
Q14 1 1.4540 0.6602 0.4391 11.00000 0.05 0.25
Q15 1 0.4086 0.9835 -0.0134 11.00000 0.05 0.24
Q16 1 0.1644 0.3789 0.0977 11.00000 0.05 0.24
Q17 1 0.3884 0.4238 0.3330 11.00000 0.05 0.24
Q18 1 0.7055 0.6658 0.2256 11.00000 0.05 0.23
Q19 1 1.4935 0.7691 0.4238 11.00000 0.05 0.23
Q20 1 0.6435 1.2195 0.1630 11.00000 0.05 0.23
;
_shelx_res_checksum 68184
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
N N11 0.5947(2) 0.68193(15) 0.18178(12) 0.0141(2) Uani d 1 . .
H H11 0.482(4) 0.603(3) 0.145(2) 0.017 Uiso d 1 . .
C C12 0.5464(3) 0.84605(17) 0.16387(13) 0.0128(2) Uani d 1 . .
N N12 0.3196(2) 0.87844(17) 0.08228(13) 0.0164(2) Uani d 1 . .
H H12A 0.197(4) 0.801(3) 0.034(2) 0.020 Uiso d 1 . .
H H12B 0.292(4) 0.983(3) 0.081(2) 0.020 Uiso d 1 . .
C C13 0.7459(3) 0.98060(17) 0.23485(14) 0.0141(2) Uani d 1 . .
H H13 0.722951 1.097926 0.221414 0.017 Uiso calc 1 . .
C C14 0.9711(3) 0.94205(17) 0.32251(14) 0.0146(2) Uani d 1 . .
H H14 1.103592 1.032609 0.371018 0.017 Uiso calc 1 . .
I I15 1.33221(2) 0.70519(2) 0.48691(2) 0.01678(3) Uani d 1 . .
C C15 1.0075(3) 0.76766(17) 0.34127(13) 0.0140(2) Uani d 1 . .
C C16 0.8176(3) 0.64035(18) 0.26754(14) 0.0149(2) Uani d 1 . .
H H16 0.841544 0.522265 0.276282 0.018 Uiso calc 1 . .
Br Br1 0.23627(3) 0.31109(2) 0.14445(2) 0.01608(4) 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
N11 0.0168(5) 0.0103(5) 0.0141(5) -0.0016(4) 0.0035(4) -0.0002(4)
C12 0.0149(6) 0.0121(5) 0.0118(5) 0.0003(4) 0.0051(4) 0.0005(4)
N12 0.0150(5) 0.0149(5) 0.0171(5) 0.0000(4) 0.0008(4) 0.0008(4)
C13 0.0167(6) 0.0106(5) 0.0145(6) 0.0010(4) 0.0029(5) 0.0020(4)
C14 0.0149(6) 0.0127(6) 0.0147(6) -0.0005(4) 0.0023(5) 0.0007(5)
I15 0.01575(5) 0.01769(5) 0.01789(5) 0.00603(3) 0.00364(3) 0.00494(3)
C15 0.0154(6) 0.0144(6) 0.0136(6) 0.0035(5) 0.0053(5) 0.0033(5)
C16 0.0193(6) 0.0125(6) 0.0145(6) 0.0029(5) 0.0063(5) 0.0029(5)
Br1 0.01538(6) 0.01065(6) 0.01964(7) -0.00109(4) 0.00095(5) 0.00055(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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 '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
C12 N11 C16 . . 123.45(12) ?
C12 N11 H11 . . 119.3(14) ?
C16 N11 H11 . . 117.1(14) ?
N12 C12 N11 . . 120.62(13) ?
N12 C12 C13 . . 121.90(12) ?
N11 C12 C13 . . 117.49(12) ?
C12 N12 H12A . . 124.8(13) ?
C12 N12 H12B . . 116.8(14) ?
H12A N12 H12B . . 118.3(19) ?
C14 C13 C12 . . 120.10(12) ?
C14 C13 H13 . . 120.0 ?
C12 C13 H13 . . 120.0 ?
C13 C14 C15 . . 120.09(12) ?
C13 C14 H14 . . 120.0 ?
C15 C14 H14 . . 120.0 ?
C16 C15 C14 . . 118.68(13) ?
C16 C15 I15 . . 120.29(10) ?
C14 C15 I15 . . 120.93(10) ?
N11 C16 C15 . . 120.10(12) ?
N11 C16 H16 . . 119.9 ?
C15 C16 H16 . . 119.9 ?
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
N11 C12 . 1.3469(17) ?
N11 C16 . 1.3553(18) ?
N11 H11 . 0.80(2) ?
C12 N12 . 1.3271(18) ?
C12 C13 . 1.4155(18) ?
N12 H12A . 0.86(2) ?
N12 H12B . 0.85(2) ?
C13 C14 . 1.3638(19) ?
C13 H13 . 0.9500 ?
C14 C15 . 1.4125(18) ?
C14 H14 . 0.9500 ?
I15 C15 . 2.0815(14) ?
C15 C16 . 1.3628(19) ?
C16 H16 . 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
N11 H11 Br1 . 0.80(2) 2.49(2) 3.2136(12) 150.8(18) yes
N12 H12A Br1 2_565 0.86(2) 2.55(2) 3.3556(12) 155.5(17) yes
N12 H12B Br1 1_565 0.85(2) 2.67(2) 3.4924(13) 165.5(18) 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 N11 C12 N12 . . . . -177.42(13) ?
C16 N11 C12 C13 . . . . 2.67(19) ?
N12 C12 C13 C14 . . . . 177.04(13) ?
N11 C12 C13 C14 . . . . -3.05(19) ?
C12 C13 C14 C15 . . . . 0.9(2) ?
C13 C14 C15 C16 . . . . 1.8(2) ?
C13 C14 C15 I15 . . . . -174.50(10) ?
C12 N11 C16 C15 . . . . 0.0(2) ?
C14 C15 C16 N11 . . . . -2.25(19) ?
I15 C15 C16 N11 . . . . 174.05(10) ?