#------------------------------------------------------------------------------
#$Date: 2024-08-07 01:03:12 +0300 (Wed, 07 Aug 2024) $
#$Revision: 293985 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/31/25/2312531.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_2312531
loop_
_publ_author_name
'Blake, Alexander J.'
'Castellano, Carlo'
'Lippolis, Vito'
'Podda, Enrico'
'Schröder, Martin'
_publ_section_title
;
Formation of extended polyiodides at large cation templates.
;
_journal_coeditor_code VP3036
_journal_issue 'Pt 7'
_journal_name_full
'Acta crystallographica. Section C, Structural chemistry'
_journal_page_first 311
_journal_page_last 318
_journal_paper_doi 10.1107/S2053229624004194
_journal_volume 80
_journal_year 2024
_chemical_formula_iupac 'C18 H38 N2 O6 2+, I3 -, I-, 2.5I2, C H2 Cl2'
_chemical_formula_moiety 'C18 H38 N2 O6 2+, I3 -, I-, 2.5(I2), C H2 Cl2'
_chemical_formula_sum 'C19 H40 Cl2 I9 N2 O6'
_chemical_formula_weight 1605.53
_chemical_name_systematic
;
4,7,13,16,21,24-Hexaoxa-1,10-diazoniabicyclo[8.8.8]hexacosane triiodide iodide
hemipenta(diiodine) dichloromethane monosolvate
;
_space_group_crystal_system monoclinic
_space_group_IT_number 14
_space_group_name_Hall '-P 2yn'
_space_group_name_H-M_alt 'P 1 21/n 1'
_atom_sites_solution_hydrogens mixed
_atom_sites_solution_primary dual
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_cell_angle_alpha 90
_cell_angle_beta 96.700(10)
_cell_angle_gamma 90
_cell_formula_units_Z 4
_cell_length_a 13.831(2)
_cell_length_b 14.820(2)
_cell_length_c 20.266(3)
_cell_measurement_reflns_used 1024
_cell_measurement_temperature 293(2)
_cell_measurement_theta_max 24.97
_cell_measurement_theta_min 2.33
_cell_volume 4125.7(10)
_computing_cell_refinement
;
SAINT (Bruker, 2001)
;
_computing_data_collection
;
SAINT (Bruker, 2001)
;
_computing_data_reduction
;
SAINT (Bruker, 2001)
;
_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_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type 'Bruker APEXII CCD'
_diffrn_measurement_method 'omega scan'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0473
_diffrn_reflns_av_unetI/netI 0.0370
_diffrn_reflns_limit_h_max 17
_diffrn_reflns_limit_h_min -17
_diffrn_reflns_limit_k_max 18
_diffrn_reflns_limit_k_min -17
_diffrn_reflns_limit_l_max 24
_diffrn_reflns_limit_l_min -24
_diffrn_reflns_number 30347
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 26.025
_diffrn_reflns_theta_min 1.694
_exptl_absorpt_coefficient_mu 6.923
_exptl_absorpt_correction_T_max 1.000
_exptl_absorpt_correction_T_min 0.569
_exptl_absorpt_correction_type empirical
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2001)
;
_exptl_crystal_colour 'dark brown'
_exptl_crystal_density_diffrn 2.585
_exptl_crystal_description prism
_exptl_crystal_F_000 2908
_exptl_crystal_size_max 0.2
_exptl_crystal_size_mid 0.15
_exptl_crystal_size_min 0.11
_refine_diff_density_max 1.369
_refine_diff_density_min -1.198
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.003
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 349
_refine_ls_number_reflns 8100
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.003
_refine_ls_R_factor_all 0.0621
_refine_ls_R_factor_gt 0.0328
_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^)+(0.0409P)^2^+2.6443P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0757
_refine_ls_wR_factor_ref 0.0878
_reflns_number_gt 5518
_reflns_number_total 8100
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file vp3036.cif
_cod_data_source_block II
_cod_depositor_comments
'Adding full bibliography for 2312530--2312531.cif.'
_cod_original_cell_volume 4125.6(10)
_cod_database_code 2312531
_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 -5 -24 22.86 7.73
2 -5 -24 7.67 7.08
0 -4 -24 11.94 6.52
1 -4 -24 3.10 6.18
2 -4 -24 11.88 6.83
3 -4 -24 4.30 6.65
4 -4 -24 -4.87 6.53
-1 -3 -24 -3.78 5.33
0 -3 -24 22.77 6.92
1 -3 -24 -0.76 5.67
2 -3 -24 -2.12 6.15
3 -3 -24 -5.90 5.75
4 -3 -24 51.24 9.54
5 -3 -24 -1.30 6.41
-2 -2 -24 9.35 5.67
-1 -2 -24 3.51 5.78
0 -2 -24 13.38 6.18
1 -2 -24 21.18 6.99
2 -2 -24 2.19 6.15
3 -2 -24 6.04 6.09
4 -2 -24 -2.21 6.33
5 -2 -24 4.15 6.62
6 -2 -24 14.66 7.23
-2 -1 -24 4.40 5.26
-1 -1 -24 13.82 5.95
0 -1 -24 10.13 5.90
1 -1 -24 18.04 6.67
2 -1 -24 17.35 6.74
3 -1 -24 -0.47 5.91
4 -1 -24 11.58 6.78
5 -1 -24 5.70 6.28
6 -1 -24 -2.31 6.04
-2 0 -24 -0.34 5.15
-1 0 -24 -1.82 5.01
0 0 -24 2.22 5.58
1 0 -24 -0.31 5.76
2 0 -24 11.84 6.86
3 0 -24 2.10 5.87
4 0 -24 -3.69 5.73
5 0 -24 -0.49 5.84
6 0 -24 0.28 5.67
-2 1 -24 2.74 5.13
-1 1 -24 13.02 6.19
0 1 -24 5.47 5.93
1 1 -24 16.40 6.52
2 1 -24 19.05 7.11
3 1 -24 -5.24 5.72
4 1 -24 12.52 6.78
5 1 -24 -3.13 5.87
6 1 -24 0.40 6.01
-2 2 -24 7.47 5.14
-1 2 -24 6.55 5.41
0 2 -24 1.20 5.32
1 2 -24 22.26 7.02
2 2 -24 12.13 6.52
3 2 -24 2.86 6.03
4 2 -24 0.74 5.90
5 2 -24 0.03 5.85
6 2 -24 6.28 6.37
-1 3 -24 -2.90 4.99
0 3 -24 23.57 7.14
1 3 -24 3.79 5.51
2 3 -24 5.29 5.93
3 3 -24 -2.90 5.58
4 3 -24 69.07 9.63
5 3 -24 -0.16 5.87
-1 4 -24 1.13 5.18
0 4 -24 26.83 6.92
1 4 -24 -4.96 5.26
2 4 -24 14.68 6.68
3 4 -24 -0.28 5.57
4 4 -24 1.35 5.94
1 5 -24 19.11 6.81
2 5 -24 7.38 5.93
3 -7 -23 -3.58 7.08
2 -6 -23 6.01 6.77
3 -6 -23 14.90 7.81
4 -6 -23 1.87 6.77
5 -6 -23 19.17 8.43
0 -5 -23 -2.38 5.53
1 -5 -23 11.58 6.35
2 -5 -23 -5.08 5.95
3 -5 -23 -1.10 6.64
4 -5 -23 52.87 9.57
5 -5 -23 4.58 7.42
6 -5 -23 50.94 10.78
-1 -4 -23 4.00 5.51
0 -4 -23 4.44 5.55
1 -4 -23 69.83 9.18
2 -4 -23 3.75 5.90
3 -4 -23 -0.77 5.78
4 -4 -23 21.54 7.44
5 -4 -23 24.49 7.98
6 -4 -23 -4.07 7.08
7 -4 -23 2.83 7.95
-2 -3 -23 5.67 5.17
-1 -3 -23 2.67 5.10
0 -3 -23 2.81 5.47
1 -3 -23 -2.33 5.78
2 -3 -23 1.14 5.93
3 -3 -23 32.96 7.70
4 -3 -23 3.45 6.40
5 -3 -23 -8.40 6.21
6 -3 -23 19.05 7.44
7 -3 -23 4.99 6.80
-3 -2 -23 7.92 4.89
-2 -2 -23 8.12 5.21
-1 -2 -23 5.70 5.23
0 -2 -23 16.41 6.25
1 -2 -23 12.22 6.41
2 -2 -23 4.24 5.90
3 -2 -23 -0.36 5.66
4 -2 -23 0.68 6.13
5 -2 -23 -5.73 5.61
6 -2 -23 0.41 6.37
7 -2 -23 3.50 6.64
8 -2 -23 18.83 7.85
-4 -1 -23 5.69 4.44
-3 -1 -23 6.83 4.75
-2 -1 -23 1.76 4.75
-1 -1 -23 0.10 5.10
0 -1 -23 0.49 5.36
1 -1 -23 -0.61 5.29
2 -1 -23 11.95 6.25
3 -1 -23 -6.53 5.20
4 -1 -23 3.58 5.81
5 -1 -23 8.07 6.21
6 -1 -23 51.64 9.27
7 -1 -23 0.01 6.09
8 -1 -23 16.00 7.18
-4 0 -23 2.34 4.28
-3 0 -23 1.84 4.58
-2 0 -23 -0.49 4.87
-1 0 -23 59.28 8.00
0 0 -23 3.08 5.38
1 0 -23 117.52 10.98
2 0 -23 1.97 5.61
3 0 -23 4.81 5.76
4 0 -23 0.50 5.60
5 0 -23 9.20 6.19
6 0 -23 -7.75 5.32
7 0 -23 0.06 5.93
8 0 -23 -7.12 5.70
-4 1 -23 8.62 4.89
-3 1 -23 6.67 4.99
-2 1 -23 -2.90 4.38
-1 1 -23 5.45 5.21
0 1 -23 0.00 5.02
1 1 -23 -1.56 5.29
2 1 -23 5.38 5.70
3 1 -23 -0.36 5.23
4 1 -23 1.56 5.78
5 1 -23 9.15 5.97
6 1 -23 61.07 9.26
7 1 -23 0.90 5.81
8 1 -23 20.50 7.48
-4 2 -23 5.61 4.89
-3 2 -23 -1.56 4.33
-2 2 -23 5.73 4.83
-1 2 -23 0.25 5.13
0 2 -23 23.51 6.52
1 2 -23 16.19 6.24
2 2 -23 3.36 5.58
3 2 -23 -7.04 5.14
4 2 -23 6.78 5.91
5 2 -23 -2.00 5.38
6 2 -23 -8.64 5.11
7 2 -23 2.33 5.72
8 2 -23 24.68 7.20
-4 3 -23 6.06 4.71
-3 3 -23 1.96 4.64
-2 3 -23 9.54 5.47
-1 3 -23 2.43 4.80
0 3 -23 7.52 5.54
1 3 -23 -2.12 5.36
2 3 -23 7.66 5.90
3 3 -23 31.08 7.42
4 3 -23 8.06 6.13
5 3 -23 2.12 5.54
6 3 -23 8.24 6.27
7 3 -23 4.56 5.93
-3 4 -23 0.68 4.78
-2 4 -23 -3.14 4.73
-1 4 -23 8.99 5.39
0 4 -23 -3.33 4.96
1 4 -23 60.60 8.46
2 4 -23 -2.16 4.99
3 4 -23 0.92 5.41
4 4 -23 6.35 5.82
5 4 -23 24.14 7.17
6 4 -23 5.94 5.95
7 4 -23 19.63 7.18
-2 5 -23 10.83 5.41
-1 5 -23 12.07 5.66
0 5 -23 3.90 5.26
1 5 -23 14.16 6.37
2 5 -23 -0.52 5.01
3 5 -23 -0.24 5.20
4 5 -23 45.76 8.18
5 5 -23 14.90 6.81
6 5 -23 52.50 8.80
-1 6 -23 20.23 6.18
0 6 -23 7.61 5.47
1 6 -23 -1.19 4.83
2 6 -23 8.16 5.76
3 6 -23 12.25 6.07
4 6 -23 9.78 6.27
5 6 -23 15.75 6.77
1 7 -23 -1.13 5.27
2 7 -23 5.07 5.44
3 7 -23 -1.23 5.20
3 -8 -22 24.99 8.50
4 -8 -22 12.53 8.16
2 -7 -22 5.69 6.52
3 -7 -22 -6.77 6.58
4 -7 -22 7.11 7.92
5 -7 -22 6.83 7.24
6 -7 -22 5.18 7.54
1 -6 -22 -0.19 5.79
2 -6 -22 48.30 8.80
3 -6 -22 8.56 6.89
4 -6 -22 4.75 6.89
5 -6 -22 19.11 7.84
6 -6 -22 5.50 7.24
7 -6 -22 -8.84 6.61
0 -5 -22 12.83 6.25
1 -5 -22 11.97 6.31
2 -5 -22 14.29 6.77
3 -5 -22 18.75 7.42
4 -5 -22 44.07 8.96
5 -5 -22 0.16 6.98
6 -5 -22 2.73 6.70
7 -5 -22 0.71 6.72
8 -5 -22 -2.84 6.67
-1 -4 -22 -1.26 4.81
0 -4 -22 31.86 7.10
1 -4 -22 0.33 5.26
2 -4 -22 7.64 5.61
3 -4 -22 19.55 7.24
4 -4 -22 -0.15 5.84
5 -4 -22 5.29 6.95
6 -4 -22 14.87 7.64
7 -4 -22 3.41 6.25
8 -4 -22 7.39 6.75
-2 -3 -22 6.55 4.96
-1 -3 -22 13.85 5.45
0 -3 -22 63.46 8.09
1 -3 -22 3.07 5.45
2 -3 -22 50.27 8.31
3 -3 -22 21.51 7.32
4 -3 -22 2.36 5.90
5 -3 -22 6.44 6.46
6 -3 -22 9.23 7.07
7 -3 -22 8.03 6.72
8 -3 -22 -3.04 5.88
9 -3 -22 13.30 6.90
-3 -2 -22 28.06 6.00
-2 -2 -22 -0.59 4.49
-1 -2 -22 4.19 4.89
0 -2 -22 26.62 6.18
1 -2 -22 4.10 5.39
2 -2 -22 -6.34 5.02
3 -2 -22 31.25 7.15
4 -2 -22 17.43 6.80
5 -2 -22 5.79 6.52
6 -2 -22 7.14 6.31
7 -2 -22 54.94 9.72
8 -2 -22 14.32 7.81
9 -2 -22 9.73 6.81
-4 -1 -22 5.78 4.30
-3 -1 -22 -1.13 4.06
-2 -1 -22 3.48 4.43
-1 -1 -22 10.84 5.17
0 -1 -22 17.91 5.76
1 -1 -22 2.89 5.39
2 -1 -22 30.66 7.11
3 -1 -22 4.70 5.38
4 -1 -22 -0.90 5.48
5 -1 -22 0.73 5.47
6 -1 -22 10.53 6.65
7 -1 -22 -3.53 5.47
8 -1 -22 -8.53 5.90
9 -1 -22 10.80 7.44
-5 0 -22 -0.79 3.78
-4 0 -22 34.04 5.57
-3 0 -22 -1.27 3.88
-2 0 -22 10.27 4.93
-1 0 -22 4.04 4.83
0 0 -22 110.95 10.01
1 0 -22 4.75 5.21
2 0 -22 15.66 6.27
3 0 -22 -9.18 4.98
4 0 -22 34.97 7.48
5 0 -22 3.38 5.61
6 0 -22 28.41 7.60
7 0 -22 -5.30 5.67
8 0 -22 19.63 7.24
9 0 -22 -4.65 5.78
-6 1 -22 20.69 4.70
-5 1 -22 1.87 3.97
-4 1 -22 7.45 4.53
-3 1 -22 -1.29 4.03
-2 1 -22 -4.92 4.21
-1 1 -22 8.68 5.02
0 1 -22 1.90 4.84
1 1 -22 -0.27 4.98
2 1 -22 34.34 7.42
3 1 -22 4.09 5.57
4 1 -22 1.53 5.32
5 1 -22 4.44 5.39
6 1 -22 6.96 6.10
7 1 -22 -2.34 5.82
8 1 -22 2.73 5.93
9 1 -22 11.70 6.65
-6 2 -22 8.80 4.21
-5 2 -22 26.65 5.23
-4 2 -22 1.51 4.25
-3 2 -22 32.48 6.00
-2 2 -22 1.93 4.40
-1 2 -22 5.36 4.99
0 2 -22 24.53 6.46
1 2 -22 3.45 5.23
2 2 -22 -3.08 4.95
3 2 -22 28.19 7.10
4 2 -22 9.45 6.07
5 2 -22 0.80 5.20
6 2 -22 13.76 6.47
7 2 -22 40.01 7.92
8 2 -22 19.49 7.18
9 2 -22 6.28 5.97
-5 3 -22 10.65 4.27
-4 3 -22 28.38 5.69
-3 3 -22 9.64 4.73
-2 3 -22 0.46 4.67
-1 3 -22 12.00 5.42
0 3 -22 72.61 8.87
1 3 -22 1.56 4.78
2 3 -22 56.21 8.19
3 3 -22 24.68 6.78
4 3 -22 -3.07 4.92
5 3 -22 10.16 6.19
6 3 -22 11.61 6.27
7 3 -22 14.10 6.27
8 3 -22 -1.07 5.10
9 3 -22 12.98 6.16
-5 4 -22 7.57 4.25
-4 4 -22 18.06 5.30
-3 4 -22 3.36 4.41
-2 4 -22 -5.07 4.12
-1 4 -22 3.63 4.65
0 4 -22 36.90 7.05
1 4 -22 7.11 5.14
2 4 -22 6.81 5.33
3 4 -22 16.92 6.27
4 4 -22 2.65 5.51
5 4 -22 10.80 5.93
6 4 -22 12.47 6.33
7 4 -22 -1.26 5.32
8 4 -22 -3.61 5.08
-4 5 -22 20.78 5.45
-3 5 -22 3.01 4.41
-2 5 -22 10.49 5.10
-1 5 -22 10.09 5.10
0 5 -22 15.17 5.23
1 5 -22 7.20 5.24
2 5 -22 14.75 5.95
3 5 -22 13.45 6.07
4 5 -22 38.97 7.61
5 5 -22 1.08 5.42
6 5 -22 6.22 5.87
7 5 -22 4.15 5.93
8 5 -22 0.43 5.64
-4 6 -22 27.46 5.82
-3 6 -22 13.54 5.17
-2 6 -22 22.66 5.78
-1 6 -22 7.75 5.05
0 6 -22 1.96 4.56
1 6 -22 2.46 5.15
2 6 -22 48.91 8.03
3 6 -22 19.52 6.37
4 6 -22 4.83 5.51
5 6 -22 9.48 6.04
6 6 -22 5.07 5.81
7 6 -22 3.42 5.35
-3 7 -22 14.59 5.39
-2 7 -22 11.05 5.10
-1 7 -22 3.02 4.77
0 7 -22 12.52 5.58
1 7 -22 1.08 4.68
2 7 -22 2.40 4.84
3 7 -22 -0.68 4.98
4 7 -22 3.56 5.36
5 7 -22 0.13 5.55
6 7 -22 -0.22 5.41
-1 8 -22 -4.83 4.40
0 8 -22 4.37 4.89
1 8 -22 2.40 5.05
2 8 -22 1.20 5.11
3 8 -22 16.49 6.13
4 8 -22 10.44 6.16
4 -9 -21 4.75 7.47
5 -9 -21 12.74 8.56
-3 -8 -21 3.88 6.25
3 -8 -21 14.61 7.64
4 -8 -21 40.45 8.95
5 -8 -21 29.74 8.81
6 -8 -21 26.72 9.44
7 -8 -21 19.20 8.35
-4 -7 -21 12.32 6.19
1 -7 -21 15.26 6.77
2 -7 -21 3.98 6.10
3 -7 -21 -4.34 6.55
4 -7 -21 6.06 6.49
5 -7 -21 33.02 9.11
6 -7 -21 -2.00 6.83
7 -7 -21 -4.12 6.90
8 -7 -21 6.43 7.66
-5 -6 -21 36.63 7.82
0 -6 -21 74.83 8.64
1 -6 -21 83.37 10.03
2 -6 -21 79.83 9.87
3 -6 -21 -5.04 6.01
4 -6 -21 -1.67 6.28
5 -6 -21 2.37 6.67
6 -6 -21 13.79 7.70
7 -6 -21 -2.74 6.95
8 -6 -21 -1.24 6.65
-6 -5 -21 -1.88 5.54
-1 -5 -21 8.15 5.08
0 -5 -21 14.95 6.00
1 -5 -21 40.93 7.44
2 -5 -21 18.78 6.47
3 -5 -21 20.16 6.86
4 -5 -21 3.95 6.46
5 -5 -21 -10.96 5.41
6 -5 -21 34.87 8.56
7 -5 -21 11.82 7.33
8 -5 -21 1.14 6.59
9 -5 -21 4.38 6.80
-2 -4 -21 2.86 4.40
-1 -4 -21 51.44 7.11
0 -4 -21 4.77 5.08
1 -4 -21 0.04 4.99
2 -4 -21 28.47 7.02
3 -4 -21 43.67 8.49
4 -4 -21 72.20 10.07
5 -4 -21 9.41 7.15
6 -4 -21 8.00 6.72
7 -4 -21 3.58 6.12
8 -4 -21 6.65 6.43
9 -4 -21 1.63 6.13
10 -4 -21 11.84 7.47
-3 -3 -21 57.98 7.23
-2 -3 -21 0.83 4.41
-1 -3 -21 10.46 4.93
0 -3 -21 -0.65 4.38
1 -3 -21 33.46 6.81
2 -3 -21 47.53 7.85
3 -3 -21 -4.24 5.20
4 -3 -21 -0.87 5.41
5 -3 -21 -2.03 5.61
6 -3 -21 -5.01 5.69
7 -3 -21 5.81 6.06
8 -3 -21 9.44 6.56
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-6 5 23 51.19 12.04
-5 5 23 6.56 10.24
-4 5 23 64.91 13.05
-3 5 23 -13.67 9.69
-2 5 23 7.18 10.18
-1 5 23 5.94 10.44
0 5 23 -6.01 9.26
1 5 23 2.49 9.85
2 5 23 -6.37 9.75
-5 6 23 7.78 10.61
-4 6 23 0.93 10.43
-3 6 23 7.32 10.07
-2 6 23 -10.46 9.55
-1 6 23 -20.57 9.08
0 6 23 6.03 9.67
1 6 23 10.35 10.38
-3 7 23 -12.71 9.54
-2 7 23 -7.92 9.87
-1 7 23 -21.43 8.86
-2 -5 24 7.84 11.29
-4 -4 24 -2.78 11.05
-3 -4 24 3.18 11.23
-2 -4 24 3.53 10.96
-1 -4 24 -9.72 10.80
0 -4 24 21.57 10.98
1 -4 24 4.13 10.34
-5 -3 24 5.07 11.29
-4 -3 24 42.68 13.76
-3 -3 24 -18.69 9.44
-2 -3 24 -9.12 10.16
-1 -3 24 1.32 10.01
0 -3 24 26.59 11.12
1 -3 24 -8.37 9.88
-6 -2 24 -9.48 10.93
-5 -2 24 3.79 11.47
-4 -2 24 -9.81 10.46
-3 -2 24 4.09 10.27
-2 -2 24 11.11 10.38
-1 -2 24 11.29 10.72
0 -2 24 1.39 9.79
1 -2 24 -4.55 9.78
2 -2 24 10.25 10.56
-6 -1 24 0.25 10.37
-5 -1 24 -2.16 11.12
-4 -1 24 1.41 10.44
-3 -1 24 0.09 10.12
-2 -1 24 22.97 11.05
-1 -1 24 -0.76 9.24
0 -1 24 -15.79 9.17
1 -1 24 15.48 9.94
2 -1 24 -1.54 10.13
-6 0 24 10.35 10.98
-5 0 24 -13.14 9.70
-4 0 24 -2.78 9.63
-3 0 24 -14.26 9.49
-2 0 24 7.23 10.01
-1 0 24 0.09 9.04
0 0 24 -5.73 9.58
1 0 24 -16.69 9.27
2 0 24 10.12 10.15
-6 1 24 -4.07 10.34
-5 1 24 -1.51 10.59
-4 1 24 2.68 10.61
-3 1 24 4.30 9.39
-2 1 24 2.95 9.95
-1 1 24 4.40 10.49
0 1 24 -2.22 10.03
1 1 24 1.97 10.06
2 1 24 -11.76 8.83
-6 2 24 7.55 10.74
-5 2 24 4.44 10.34
-4 2 24 -3.54 9.84
-3 2 24 -5.50 9.78
-2 2 24 -0.77 10.19
-1 2 24 5.69 10.41
0 2 24 -18.35 9.42
1 2 24 -19.73 8.83
2 2 24 -12.21 9.45
-5 3 24 -3.81 10.31
-4 3 24 64.81 12.84
-3 3 24 -12.15 9.91
-2 3 24 -8.49 10.19
-1 3 24 -8.55 9.61
0 3 24 17.63 10.83
1 3 24 -5.24 9.91
-4 4 24 -14.62 9.41
-3 4 24 -7.02 10.09
-2 4 24 -6.53 9.98
-1 4 24 -0.12 9.81
0 4 24 6.58 10.95
-2 5 24 2.58 10.35
0 0 0 0.00 0.00
_computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)'
;
_shelx_hkl_checksum 87709
_shelx_res_file
;
TITL II.res in P2(1)/n
ii.res
created by SHELXL-2018/3 at 17:51:18 on 08-Jan-2024
REM Old TITL II.res in P2(1)/n
REM SHELXT solution in P2(1)/n: R1 0.154, Rweak 0.008, Alpha 0.014
REM 0.610 for 334 systematic absences, Orientation as input
REM Formula found by SHELXT: I5 Cl2 O6 N2 C19
CELL 0.71073 13.8313 14.8196 20.2656 90 96.7 90
ZERR 4 0.002 0.0021 0.003 0 0.01 0
LATT 1
SYMM 0.5-X,0.5+Y,0.5-Z
SFAC I Cl O N C H
UNIT 36 8 24 8 76 160
L.S. 10
PLAN 28
TEMP 20(2)
CONF
list 4
MORE -1
BOND $H
fmap 2 53
acta
OMIT 0 2 1
REM
REM
REM
WGHT 0.040900 2.644300
FVAR 0.11166
I3 1 0.975325 0.098146 -0.091539 11.00000 0.05001 0.05291 =
0.05788 0.01122 0.02081 0.01159
I6 1 1.181183 0.252270 0.290993 11.00000 0.03743 0.06862 =
0.05892 -0.00570 0.01235 -0.00092
I8 1 1.025639 0.122006 0.440478 11.00000 0.06634 0.04976 =
0.04904 -0.00352 -0.00714 0.00149
I1 1 1.041901 0.415928 -0.003674 11.00000 0.05634 0.07928 =
0.04877 0.01202 0.01328 -0.00362
I5 1 1.146166 0.365732 0.180212 11.00000 0.05499 0.08091 =
0.06494 0.00905 0.00316 0.00427
I9 1 0.840166 0.129124 0.482786 11.00000 0.05655 0.08286 =
0.07091 -0.01177 -0.00696 0.00293
I2 1 1.119197 0.197107 0.002829 11.00000 0.05561 0.07824 =
0.08166 -0.01413 0.01093 0.00734
I4 1 0.844213 -0.006471 -0.180759 11.00000 0.05699 0.07629 =
0.08698 0.00795 0.00798 -0.01162
I7 1 1.237234 0.116572 0.405165 11.00000 0.07504 0.09880 =
0.06893 0.01996 0.01682 0.01947
CL1 2 0.954945 0.386739 0.321369 11.00000 0.06510 0.08551 =
0.10104 -0.01962 0.02394 0.01095
CL2 2 0.772563 0.392065 0.375825 11.00000 0.10554 0.06745 =
0.15211 -0.00791 0.08149 -0.00636
O3 3 1.013770 0.594784 0.417272 11.00000 0.04117 0.05854 =
0.05295 -0.00468 0.00818 -0.00443
O4 3 0.815307 0.626191 0.446755 11.00000 0.03949 0.06679 =
0.04628 0.00628 0.00949 0.00260
O6 3 0.731826 0.855903 0.346795 11.00000 0.04609 0.06652 =
0.06158 -0.01094 0.01674 -0.01036
O5 3 0.937935 0.831328 0.330104 11.00000 0.04525 0.05061 =
0.07212 -0.00381 0.02473 -0.00092
O2 3 0.896780 0.625954 0.231634 11.00000 0.04194 0.08548 =
0.03922 0.00014 0.00278 0.00113
O1 3 0.702005 0.601357 0.261080 11.00000 0.04808 0.06669 =
0.05739 0.00046 0.01036 0.01240
N2 4 1.057390 0.689460 0.302611 11.00000 0.02633 0.05322 =
0.04849 0.00660 0.01565 0.00527
H2 6 1.000537 0.686020 0.313524 11.00000 -1.20000
N1 4 0.645152 0.687665 0.376050 11.00000 0.03267 0.03782 =
0.05552 -0.01148 0.01378 -0.00451
H1 6 0.699027 0.690885 0.361638 11.00000 -1.20000
C11 5 0.728330 0.607696 0.475324 11.00000 0.05425 0.06168 =
0.05267 0.00776 0.02311 -0.00238
AFIX 23
H11A 6 0.716852 0.654111 0.507249 11.00000 -1.20000
H11B 6 0.733234 0.549923 0.497966 11.00000 -1.20000
AFIX 0
C7 5 1.129577 0.683223 0.363382 11.00000 0.03023 0.05786 =
0.05346 0.00695 0.00354 -0.00284
AFIX 23
H7A 6 1.125640 0.737570 0.389610 11.00000 -1.20000
H7B 6 1.194607 0.680113 0.350046 11.00000 -1.20000
AFIX 0
C9 5 0.987753 0.655223 0.466316 11.00000 0.04658 0.05681 =
0.05955 -0.00153 0.00012 -0.00620
AFIX 23
H9A 6 0.975004 0.714386 0.446738 11.00000 -1.20000
H9B 6 1.041407 0.660797 0.501438 11.00000 -1.20000
AFIX 0
C2 5 0.603231 0.601001 0.270579 11.00000 0.04866 0.07717 =
0.05636 -0.01693 0.00451 -0.00761
AFIX 23
H2A 6 0.587977 0.544205 0.290791 11.00000 -1.20000
H2B 6 0.564287 0.604898 0.227653 11.00000 -1.20000
AFIX 0
C15 5 0.811332 0.873018 0.395116 11.00000 0.04379 0.06388 =
0.05490 -0.00761 0.00756 -0.00016
AFIX 23
H15A 6 0.827712 0.818663 0.420665 11.00000 -1.20000
H15B 6 0.793995 0.919471 0.425342 11.00000 -1.20000
AFIX 0
C8 5 1.113536 0.602770 0.405686 11.00000 0.03811 0.06622 =
0.06008 0.01068 0.01359 0.00817
AFIX 23
H8A 6 1.132992 0.548567 0.383870 11.00000 -1.20000
H8B 6 1.154018 0.608160 0.447929 11.00000 -1.20000
AFIX 0
C12 5 0.646643 0.606057 0.419377 11.00000 0.04798 0.04558 =
0.07523 -0.00543 0.02396 -0.00490
AFIX 23
H12A 6 0.653090 0.552702 0.392511 11.00000 -1.20000
H12B 6 0.585150 0.601838 0.437805 11.00000 -1.20000
AFIX 0
C4 5 0.813657 0.638414 0.183847 11.00000 0.05020 0.09558 =
0.03897 0.00088 0.00105 0.00179
AFIX 23
H4A 6 0.797239 0.581965 0.161018 11.00000 -1.20000
H4B 6 0.828128 0.682662 0.151120 11.00000 -1.20000
AFIX 0
C6 5 1.066959 0.612508 0.255737 11.00000 0.04692 0.06375 =
0.06140 -0.00781 0.01719 0.00280
AFIX 23
H6A 6 1.069183 0.556145 0.280203 11.00000 -1.20000
H6B 6 1.127538 0.618509 0.236363 11.00000 -1.20000
AFIX 0
C17 5 1.029417 0.855156 0.309638 11.00000 0.06026 0.04370 =
0.08481 0.01276 0.03138 -0.00445
AFIX 23
H17A 6 1.077173 0.864245 0.348067 11.00000 -1.20000
H17B 6 1.023659 0.910587 0.284027 11.00000 -1.20000
AFIX 0
C13 5 0.624157 0.773365 0.411765 11.00000 0.05009 0.04735 =
0.06458 -0.01452 0.02774 -0.00333
AFIX 23
H13A 6 0.557033 0.772228 0.421256 11.00000 -1.20000
H13B 6 0.665384 0.775461 0.453878 11.00000 -1.20000
AFIX 0
C18 5 1.059992 0.779179 0.267999 11.00000 0.05144 0.06911 =
0.06617 0.02771 0.02739 0.01185
AFIX 23
H18A 6 1.125533 0.790410 0.257413 11.00000 -1.20000
H18B 6 1.017123 0.777002 0.226584 11.00000 -1.20000
AFIX 0
C16 5 0.896768 0.902950 0.362524 11.00000 0.05062 0.04304 =
0.08045 -0.00301 0.01060 -0.00733
AFIX 23
H16A 6 0.876653 0.949941 0.330521 11.00000 -1.20000
H16B 6 0.945446 0.928241 0.395730 11.00000 -1.20000
AFIX 0
C3 5 0.729371 0.669974 0.217854 11.00000 0.05326 0.06730 =
0.05606 0.00555 0.00500 0.00878
AFIX 23
H3A 6 0.747298 0.724232 0.243136 11.00000 -1.20000
H3B 6 0.674802 0.684256 0.184983 11.00000 -1.20000
AFIX 0
C10 5 0.899120 0.622468 0.494989 11.00000 0.05576 0.06715 =
0.04436 0.00626 0.01115 0.00265
AFIX 23
H10A 6 0.909439 0.560824 0.510303 11.00000 -1.20000
H10B 6 0.888319 0.659487 0.532918 11.00000 -1.20000
AFIX 0
C5 5 0.983441 0.610066 0.201223 11.00000 0.05353 0.08398 =
0.04926 -0.00507 0.00869 0.00184
AFIX 23
H5A 6 0.991440 0.656283 0.168403 11.00000 -1.20000
H5B 6 0.980229 0.551744 0.179350 11.00000 -1.20000
AFIX 0
C14 5 0.640454 0.857305 0.373203 11.00000 0.04788 0.04525 =
0.09483 -0.01122 0.02313 -0.00026
AFIX 23
H14A 6 0.588429 0.863464 0.337011 11.00000 -1.20000
H14B 6 0.638214 0.909355 0.402005 11.00000 -1.20000
AFIX 0
C1 5 0.575392 0.678340 0.314290 11.00000 0.03721 0.06124 =
0.06945 -0.01623 0.00221 0.00403
AFIX 23
H1A 6 0.574059 0.734240 0.289300 11.00000 -1.20000
H1B 6 0.510513 0.667798 0.326374 11.00000 -1.20000
AFIX 0
C19 5 0.849296 0.448656 0.327016 11.00000 0.06843 0.07180 =
0.10649 0.02242 0.03957 0.01986
AFIX 23
H19A 6 0.815558 0.458231 0.282869 11.00000 -1.20000
H19B 6 0.866206 0.507217 0.346411 11.00000 -1.20000
AFIX 0
HKLF 4
REM II.res in P2(1)/n
REM wR2 = 0.0878, GooF = S = 1.003, Restrained GooF = 1.003 for all data
REM R1 = 0.0328 for 5518 Fo > 4sig(Fo) and 0.0621 for all 8100 data
REM 349 parameters refined using 0 restraints
END
WGHT 0.0409 2.6580
REM Highest difference peak 1.369, deepest hole -1.198, 1-sigma level 0.125
Q1 1 1.1982 0.0850 0.3743 11.00000 0.05 1.37
Q2 1 0.7259 0.3962 0.3310 11.00000 0.05 0.97
Q3 1 1.0751 0.2162 -0.0256 11.00000 0.05 0.88
Q4 1 0.8289 0.1812 0.4678 11.00000 0.05 0.86
Q5 1 0.9970 0.0992 -0.1368 11.00000 0.05 0.72
Q6 1 1.1990 0.4060 0.1705 11.00000 0.05 0.66
Q7 1 1.1895 0.4211 0.1721 11.00000 0.05 0.64
Q8 1 1.1124 0.3767 0.2225 11.00000 0.05 0.64
Q9 1 1.1013 0.2541 -0.0196 11.00000 0.05 0.64
Q10 1 1.1218 0.2424 0.3008 11.00000 0.05 0.61
Q11 1 0.7979 0.3781 0.3793 11.00000 0.05 0.59
Q12 1 1.2165 0.2632 0.2574 11.00000 0.05 0.57
Q13 1 0.9013 0.4595 -0.0410 11.00000 0.05 0.56
Q14 1 0.9218 0.4058 0.2883 11.00000 0.05 0.52
Q15 1 1.0013 0.4393 0.0248 11.00000 0.05 0.52
Q16 1 0.8139 -0.0241 -0.1355 11.00000 0.05 0.50
Q17 1 1.2533 0.1063 0.4225 11.00000 0.05 0.50
Q18 1 1.2419 0.2240 0.2763 11.00000 0.05 0.49
Q19 1 1.0552 0.3554 0.1805 11.00000 0.05 0.49
Q20 1 1.2559 0.1066 0.3552 11.00000 0.05 0.49
Q21 1 1.1166 0.2792 -0.0062 11.00000 0.05 0.48
Q22 1 1.0576 0.4212 -0.0621 11.00000 0.05 0.48
Q23 1 0.7917 0.1000 0.4850 11.00000 0.05 0.47
Q24 1 1.0818 0.4511 0.0339 11.00000 0.05 0.47
Q25 1 0.9535 0.0981 -0.0377 11.00000 0.05 0.46
Q26 1 1.1789 0.3077 0.2767 11.00000 0.05 0.45
Q27 1 0.9592 0.1194 0.4473 11.00000 0.05 0.45
Q28 1 0.9183 0.1300 0.4729 11.00000 0.05 0.44
;
_shelx_res_checksum 21517
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -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 I3 0.97532(3) 0.09815(3) -0.09154(2) 0.05246(13) Uani d 1 . .
I I6 1.18118(3) 0.25227(3) 0.29099(2) 0.05446(13) Uani d 1 . .
I I8 1.02564(4) 0.12201(3) 0.44048(2) 0.05614(13) Uani d 1 . .
I I1 1.04190(4) 0.41593(4) -0.00367(2) 0.06090(14) Uani d 1 . .
I I5 1.14617(4) 0.36573(4) 0.18021(3) 0.06725(15) Uani d 1 . .
I I9 0.84017(4) 0.12912(4) 0.48279(3) 0.07124(16) Uani d 1 . .
I I2 1.11920(4) 0.19711(4) 0.00283(3) 0.07161(16) Uani d 1 . .
I I4 0.84421(4) -0.00647(4) -0.18076(3) 0.07345(17) Uani d 1 . .
I I7 1.23723(4) 0.11657(4) 0.40516(3) 0.08026(18) Uani d 1 . .
Cl Cl1 0.95495(16) 0.38674(16) 0.32137(13) 0.0828(6) Uani d 1 . .
Cl Cl2 0.7726(2) 0.39206(15) 0.37582(16) 0.1031(9) Uani d 1 . .
O O3 1.0138(3) 0.5948(3) 0.4173(2) 0.0507(11) Uani d 1 . .
O O4 0.8153(3) 0.6262(3) 0.4468(2) 0.0505(11) Uani d 1 . .
O O6 0.7318(3) 0.8559(3) 0.3468(2) 0.0572(12) Uani d 1 . .
O O5 0.9379(3) 0.8313(3) 0.3301(2) 0.0546(12) Uani d 1 . .
O O2 0.8968(3) 0.6260(3) 0.2316(2) 0.0557(12) Uani d 1 . .
O O1 0.7020(3) 0.6014(3) 0.2611(2) 0.0571(12) Uani d 1 . .
N N2 1.0574(4) 0.6895(4) 0.3026(3) 0.0418(12) Uani d 1 . .
H H2 1.001(5) 0.686(4) 0.314(3) 0.050 Uiso d 1 . .
N N1 0.6452(4) 0.6877(3) 0.3760(3) 0.0413(12) Uani d 1 . .
H H1 0.699(5) 0.691(4) 0.362(3) 0.050 Uiso d 1 . .
C C11 0.7283(5) 0.6077(5) 0.4753(4) 0.0549(18) Uani d 1 . .
H H11A 0.716852 0.654111 0.507249 0.066 Uiso calc 1 . .
H H11B 0.733234 0.549923 0.497966 0.066 Uiso calc 1 . .
C C7 1.1296(4) 0.6832(4) 0.3634(3) 0.0473(16) Uani d 1 . .
H H7A 1.125640 0.737570 0.389610 0.057 Uiso calc 1 . .
H H7B 1.194607 0.680113 0.350046 0.057 Uiso calc 1 . .
C C9 0.9878(5) 0.6552(5) 0.4663(4) 0.0548(18) Uani d 1 . .
H H9A 0.975004 0.714386 0.446738 0.066 Uiso calc 1 . .
H H9B 1.041407 0.660797 0.501438 0.066 Uiso calc 1 . .
C C2 0.6032(5) 0.6010(5) 0.2706(4) 0.0609(19) Uani d 1 . .
H H2A 0.587977 0.544205 0.290791 0.073 Uiso calc 1 . .
H H2B 0.564287 0.604898 0.227653 0.073 Uiso calc 1 . .
C C15 0.8113(5) 0.8730(5) 0.3951(4) 0.0540(17) Uani d 1 . .
H H15A 0.827712 0.818663 0.420665 0.065 Uiso calc 1 . .
H H15B 0.793995 0.919471 0.425342 0.065 Uiso calc 1 . .
C C8 1.1135(5) 0.6028(5) 0.4057(4) 0.0542(18) Uani d 1 . .
H H8A 1.132992 0.548567 0.383870 0.065 Uiso calc 1 . .
H H8B 1.154018 0.608160 0.447929 0.065 Uiso calc 1 . .
C C12 0.6466(5) 0.6061(4) 0.4194(4) 0.0549(18) Uani d 1 . .
H H12A 0.653090 0.552702 0.392511 0.066 Uiso calc 1 . .
H H12B 0.585150 0.601838 0.437805 0.066 Uiso calc 1 . .
C C4 0.8137(5) 0.6384(6) 0.1838(3) 0.062(2) Uani d 1 . .
H H4A 0.797239 0.581965 0.161018 0.074 Uiso calc 1 . .
H H4B 0.828128 0.682662 0.151120 0.074 Uiso calc 1 . .
C C6 1.0670(5) 0.6125(5) 0.2557(4) 0.0565(18) Uani d 1 . .
H H6A 1.069183 0.556145 0.280203 0.068 Uiso calc 1 . .
H H6B 1.127538 0.618509 0.236363 0.068 Uiso calc 1 . .
C C17 1.0294(5) 0.8552(5) 0.3096(4) 0.061(2) Uani d 1 . .
H H17A 1.077173 0.864245 0.348067 0.073 Uiso calc 1 . .
H H17B 1.023659 0.910587 0.284027 0.073 Uiso calc 1 . .
C C13 0.6242(5) 0.7734(4) 0.4118(4) 0.0523(17) Uani d 1 . .
H H13A 0.557033 0.772228 0.421256 0.063 Uiso calc 1 . .
H H13B 0.665384 0.775461 0.453878 0.063 Uiso calc 1 . .
C C18 1.0600(5) 0.7792(5) 0.2680(4) 0.061(2) Uani d 1 . .
H H18A 1.125533 0.790410 0.257413 0.073 Uiso calc 1 . .
H H18B 1.017123 0.777002 0.226584 0.073 Uiso calc 1 . .
C C16 0.8968(5) 0.9029(5) 0.3625(4) 0.0578(19) Uani d 1 . .
H H16A 0.876653 0.949941 0.330521 0.069 Uiso calc 1 . .
H H16B 0.945446 0.928241 0.395730 0.069 Uiso calc 1 . .
C C3 0.7294(5) 0.6700(5) 0.2179(4) 0.0590(19) Uani d 1 . .
H H3A 0.747298 0.724232 0.243136 0.071 Uiso calc 1 . .
H H3B 0.674802 0.684256 0.184983 0.071 Uiso calc 1 . .
C C10 0.8991(5) 0.6225(5) 0.4950(3) 0.0553(18) Uani d 1 . .
H H10A 0.909439 0.560824 0.510303 0.066 Uiso calc 1 . .
H H10B 0.888319 0.659487 0.532918 0.066 Uiso calc 1 . .
C C5 0.9834(5) 0.6101(6) 0.2012(4) 0.062(2) Uani d 1 . .
H H5A 0.991440 0.656283 0.168403 0.074 Uiso calc 1 . .
H H5B 0.980229 0.551744 0.179350 0.074 Uiso calc 1 . .
C C14 0.6405(5) 0.8573(5) 0.3732(4) 0.061(2) Uani d 1 . .
H H14A 0.588429 0.863464 0.337011 0.074 Uiso calc 1 . .
H H14B 0.638214 0.909355 0.402005 0.074 Uiso calc 1 . .
C C1 0.5754(5) 0.6783(5) 0.3143(4) 0.0563(18) Uani d 1 . .
H H1A 0.574059 0.734240 0.289300 0.068 Uiso calc 1 . .
H H1B 0.510513 0.667798 0.326374 0.068 Uiso calc 1 . .
C C19 0.8493(6) 0.4487(6) 0.3270(5) 0.080(3) Uani d 1 . .
H H19A 0.815558 0.458231 0.282869 0.096 Uiso calc 1 . .
H H19B 0.866206 0.507217 0.346411 0.096 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
I3 0.0500(3) 0.0529(3) 0.0579(3) 0.0116(2) 0.0208(2) 0.0112(2)
I6 0.0374(2) 0.0686(3) 0.0589(3) -0.0009(2) 0.0123(2) -0.0057(2)
I8 0.0663(3) 0.0498(3) 0.0490(3) 0.0015(2) -0.0071(2) -0.0035(2)
I1 0.0563(3) 0.0793(3) 0.0488(3) -0.0036(2) 0.0133(2) 0.0120(2)
I5 0.0550(3) 0.0809(4) 0.0649(3) 0.0043(3) 0.0032(2) 0.0090(3)
I9 0.0566(3) 0.0829(4) 0.0709(4) 0.0029(3) -0.0070(3) -0.0118(3)
I2 0.0556(3) 0.0782(4) 0.0817(4) 0.0073(3) 0.0109(3) -0.0141(3)
I4 0.0570(3) 0.0763(4) 0.0870(4) -0.0116(3) 0.0080(3) 0.0080(3)
I7 0.0750(4) 0.0988(4) 0.0689(4) 0.0195(3) 0.0168(3) 0.0200(3)
Cl1 0.0651(12) 0.0855(15) 0.1010(17) 0.0109(11) 0.0239(12) -0.0196(13)
Cl2 0.1055(19) 0.0674(14) 0.152(3) -0.0064(13) 0.0815(19) -0.0079(14)
O3 0.041(2) 0.059(3) 0.053(3) -0.004(2) 0.008(2) -0.005(2)
O4 0.039(2) 0.067(3) 0.046(3) 0.003(2) 0.009(2) 0.006(2)
O6 0.046(3) 0.067(3) 0.062(3) -0.010(2) 0.017(2) -0.011(2)
O5 0.045(3) 0.051(3) 0.072(3) -0.001(2) 0.025(2) -0.004(2)
O2 0.042(3) 0.085(4) 0.039(3) 0.001(2) 0.003(2) 0.000(2)
O1 0.048(3) 0.067(3) 0.057(3) 0.012(2) 0.010(2) 0.000(2)
N2 0.026(2) 0.053(3) 0.048(3) 0.005(2) 0.016(2) 0.007(3)
N1 0.033(3) 0.038(3) 0.056(3) -0.005(2) 0.014(2) -0.011(2)
C11 0.054(4) 0.062(4) 0.053(4) -0.002(3) 0.023(3) 0.008(3)
C7 0.030(3) 0.058(4) 0.053(4) -0.003(3) 0.004(3) 0.007(3)
C9 0.047(4) 0.057(4) 0.060(5) -0.006(3) 0.000(3) -0.002(4)
C2 0.049(4) 0.077(5) 0.056(5) -0.008(4) 0.005(3) -0.017(4)
C15 0.044(4) 0.064(4) 0.055(4) 0.000(3) 0.008(3) -0.008(4)
C8 0.038(4) 0.066(5) 0.060(5) 0.008(3) 0.014(3) 0.011(4)
C12 0.048(4) 0.046(4) 0.075(5) -0.005(3) 0.024(4) -0.005(4)
C4 0.050(4) 0.096(6) 0.039(4) 0.002(4) 0.001(3) 0.001(4)
C6 0.047(4) 0.064(5) 0.061(5) 0.003(3) 0.017(3) -0.008(4)
C17 0.060(4) 0.044(4) 0.085(6) -0.004(3) 0.031(4) 0.013(4)
C13 0.050(4) 0.047(4) 0.065(5) -0.003(3) 0.028(3) -0.015(3)
C18 0.051(4) 0.069(5) 0.066(5) 0.012(4) 0.027(4) 0.028(4)
C16 0.051(4) 0.043(4) 0.080(5) -0.007(3) 0.011(4) -0.003(4)
C3 0.053(4) 0.067(5) 0.056(5) 0.009(4) 0.005(3) 0.006(4)
C10 0.056(4) 0.067(5) 0.044(4) 0.003(4) 0.011(3) 0.006(3)
C5 0.054(4) 0.084(6) 0.049(4) 0.002(4) 0.009(3) -0.005(4)
C14 0.048(4) 0.045(4) 0.095(6) 0.000(3) 0.023(4) -0.011(4)
C1 0.037(3) 0.061(4) 0.069(5) 0.004(3) 0.002(3) -0.016(4)
C19 0.068(5) 0.072(5) 0.106(7) 0.020(4) 0.040(5) 0.022(5)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
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
I4 I3 I2 . . 176.54(2) ?
I5 I6 I7 . . 173.63(2) ?
I9 I8 I7 . . 175.52(2) ?
I8 I7 I6 . . 89.70(2) ?
C9 O3 C8 . . 113.1(5) ?
C11 O4 C10 . . 111.8(5) ?
C15 O6 C14 . . 113.0(6) ?
C16 O5 C17 . . 111.9(5) ?
C4 O2 C5 . . 112.2(5) ?
C2 O1 C3 . . 114.9(5) ?
C7 N2 H2 . . 110(5) ?
C7 N2 C6 . . 112.0(5) ?
C7 N2 C18 . . 112.9(5) ?
C6 N2 H2 . . 106(4) ?
C6 N2 C18 . . 111.6(6) ?
C18 N2 H2 . . 104(4) ?
C12 N1 H1 . . 108(5) ?
C12 N1 C13 . . 113.0(5) ?
C12 N1 C1 . . 112.4(5) ?
C13 N1 H1 . . 111(5) ?
C1 N1 H1 . . 103(5) ?
C1 N1 C13 . . 109.8(5) ?
O4 C11 H11A . . 110.3 ?
O4 C11 H11B . . 110.3 ?
O4 C11 C12 . . 107.0(6) ?
H11A C11 H11B . . 108.6 ?
C12 C11 H11A . . 110.3 ?
C12 C11 H11B . . 110.3 ?
N2 C7 H7A . . 109.0 ?
N2 C7 H7B . . 109.0 ?
N2 C7 C8 . . 113.0(5) ?
H7A C7 H7B . . 107.8 ?
C8 C7 H7A . . 109.0 ?
C8 C7 H7B . . 109.0 ?
O3 C9 H9A . . 109.5 ?
O3 C9 H9B . . 109.5 ?
O3 C9 C10 . . 110.7(6) ?
H9A C9 H9B . . 108.1 ?
C10 C9 H9A . . 109.5 ?
C10 C9 H9B . . 109.5 ?
O1 C2 H2A . . 108.9 ?
O1 C2 H2B . . 108.9 ?
O1 C2 C1 . . 113.1(6) ?
H2A C2 H2B . . 107.8 ?
C1 C2 H2A . . 108.9 ?
C1 C2 H2B . . 108.9 ?
O6 C15 H15A . . 109.7 ?
O6 C15 H15B . . 109.7 ?
O6 C15 C16 . . 110.0(6) ?
H15A C15 H15B . . 108.2 ?
C16 C15 H15A . . 109.7 ?
C16 C15 H15B . . 109.7 ?
O3 C8 C7 . . 111.7(5) ?
O3 C8 H8A . . 109.3 ?
O3 C8 H8B . . 109.3 ?
C7 C8 H8A . . 109.3 ?
C7 C8 H8B . . 109.3 ?
H8A C8 H8B . . 107.9 ?
N1 C12 C11 . . 112.8(5) ?
N1 C12 H12A . . 109.0 ?
N1 C12 H12B . . 109.0 ?
C11 C12 H12A . . 109.0 ?
C11 C12 H12B . . 109.0 ?
H12A C12 H12B . . 107.8 ?
O2 C4 H4A . . 109.7 ?
O2 C4 H4B . . 109.7 ?
O2 C4 C3 . . 109.7(6) ?
H4A C4 H4B . . 108.2 ?
C3 C4 H4A . . 109.7 ?
C3 C4 H4B . . 109.7 ?
N2 C6 H6A . . 109.3 ?
N2 C6 H6B . . 109.3 ?
N2 C6 C5 . . 111.5(6) ?
H6A C6 H6B . . 108.0 ?
C5 C6 H6A . . 109.3 ?
C5 C6 H6B . . 109.3 ?
O5 C17 H17A . . 110.3 ?
O5 C17 H17B . . 110.3 ?
O5 C17 C18 . . 107.3(6) ?
H17A C17 H17B . . 108.5 ?
C18 C17 H17A . . 110.3 ?
C18 C17 H17B . . 110.3 ?
N1 C13 H13A . . 108.9 ?
N1 C13 H13B . . 108.9 ?
H13A C13 H13B . . 107.7 ?
C14 C13 N1 . . 113.6(6) ?
C14 C13 H13A . . 108.9 ?
C14 C13 H13B . . 108.9 ?
N2 C18 H18A . . 109.2 ?
N2 C18 H18B . . 109.2 ?
C17 C18 N2 . . 112.2(6) ?
C17 C18 H18A . . 109.2 ?
C17 C18 H18B . . 109.2 ?
H18A C18 H18B . . 107.9 ?
O5 C16 C15 . . 111.7(6) ?
O5 C16 H16A . . 109.3 ?
O5 C16 H16B . . 109.3 ?
C15 C16 H16A . . 109.3 ?
C15 C16 H16B . . 109.3 ?
H16A C16 H16B . . 107.9 ?
O1 C3 C4 . . 109.7(6) ?
O1 C3 H3A . . 109.7 ?
O1 C3 H3B . . 109.7 ?
C4 C3 H3A . . 109.7 ?
C4 C3 H3B . . 109.7 ?
H3A C3 H3B . . 108.2 ?
O4 C10 C9 . . 111.0(5) ?
O4 C10 H10A . . 109.4 ?
O4 C10 H10B . . 109.4 ?
C9 C10 H10A . . 109.4 ?
C9 C10 H10B . . 109.4 ?
H10A C10 H10B . . 108.0 ?
O2 C5 C6 . . 106.9(6) ?
O2 C5 H5A . . 110.3 ?
O2 C5 H5B . . 110.3 ?
C6 C5 H5A . . 110.3 ?
C6 C5 H5B . . 110.3 ?
H5A C5 H5B . . 108.6 ?
O6 C14 C13 . . 112.1(6) ?
O6 C14 H14A . . 109.2 ?
O6 C14 H14B . . 109.2 ?
C13 C14 H14A . . 109.2 ?
C13 C14 H14B . . 109.2 ?
H14A C14 H14B . . 107.9 ?
N1 C1 C2 . . 111.9(5) ?
N1 C1 H1A . . 109.2 ?
N1 C1 H1B . . 109.2 ?
C2 C1 H1A . . 109.2 ?
C2 C1 H1B . . 109.2 ?
H1A C1 H1B . . 107.9 ?
Cl1 C19 Cl2 . . 110.7(5) ?
Cl1 C19 H19A . . 109.5 ?
Cl1 C19 H19B . . 109.5 ?
Cl2 C19 H19A . . 109.5 ?
Cl2 C19 H19B . . 109.5 ?
H19A C19 H19B . . 108.1 ?
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
I3 I2 . 2.9799(8) ?
I3 I4 . 2.8629(8) ?
I6 I5 . 2.8015(8) ?
I6 I7 . 3.0952(8) ?
I8 I9 . 2.8001(8) ?
I8 I7 . 3.0940(9) ?
I1 I1 3_765 2.7595(11) ?
Cl1 C19 . 1.741(8) ?
Cl2 C19 . 1.747(8) ?
O3 C9 . 1.415(8) ?
O3 C8 . 1.431(8) ?
O4 C11 . 1.421(8) ?
O4 C10 . 1.428(8) ?
O6 C15 . 1.408(8) ?
O6 C14 . 1.429(8) ?
O5 C17 . 1.421(8) ?
O5 C16 . 1.403(8) ?
O2 C4 . 1.426(8) ?
O2 C5 . 1.430(8) ?
O1 C2 . 1.402(8) ?
O1 C3 . 1.422(8) ?
N2 H2 . 0.84(7) ?
N2 C7 . 1.495(8) ?
N2 C6 . 1.500(8) ?
N2 C18 . 1.506(8) ?
N1 H1 . 0.83(7) ?
N1 C12 . 1.493(8) ?
N1 C13 . 1.507(8) ?
N1 C1 . 1.495(9) ?
C11 H11A . 0.9700 ?
C11 H11B . 0.9700 ?
C11 C12 . 1.505(10) ?
C7 H7A . 0.9700 ?
C7 H7B . 0.9700 ?
C7 C8 . 1.500(9) ?
C9 H9A . 0.9700 ?
C9 H9B . 0.9700 ?
C9 C10 . 1.497(9) ?
C2 H2A . 0.9700 ?
C2 H2B . 0.9700 ?
C2 C1 . 1.525(9) ?
C15 H15A . 0.9700 ?
C15 H15B . 0.9700 ?
C15 C16 . 1.487(10) ?
C8 H8A . 0.9700 ?
C8 H8B . 0.9700 ?
C12 H12A . 0.9700 ?
C12 H12B . 0.9700 ?
C4 H4A . 0.9700 ?
C4 H4B . 0.9700 ?
C4 C3 . 1.497(10) ?
C6 H6A . 0.9700 ?
C6 H6B . 0.9700 ?
C6 C5 . 1.503(10) ?
C17 H17A . 0.9700 ?
C17 H17B . 0.9700 ?
C17 C18 . 1.497(10) ?
C13 H13A . 0.9700 ?
C13 H13B . 0.9700 ?
C13 C14 . 1.500(10) ?
C18 H18A . 0.9700 ?
C18 H18B . 0.9700 ?
C16 H16A . 0.9700 ?
C16 H16B . 0.9700 ?
C3 H3A . 0.9700 ?
C3 H3B . 0.9700 ?
C10 H10A . 0.9700 ?
C10 H10B . 0.9700 ?
C5 H5A . 0.9700 ?
C5 H5B . 0.9700 ?
C14 H14A . 0.9700 ?
C14 H14B . 0.9700 ?
C1 H1A . 0.9700 ?
C1 H1B . 0.9700 ?
C19 H19A . 0.9700 ?
C19 H19B . 0.9700 ?
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
O3 C9 C10 O4 . . . . -67.8(7) ?
O4 C11 C12 N1 . . . . -51.0(7) ?
O6 C15 C16 O5 . . . . -72.6(8) ?
O5 C17 C18 N2 . . . . -52.5(8) ?
O2 C4 C3 O1 . . . . -65.1(8) ?
O1 C2 C1 N1 . . . . -47.5(9) ?
N2 C7 C8 O3 . . . . -48.4(8) ?
N2 C6 C5 O2 . . . . -43.6(8) ?
N1 C13 C14 O6 . . . . -47.8(9) ?
C11 O4 C10 C9 . . . . -171.7(6) ?
C7 N2 C6 C5 . . . . 169.8(6) ?
C7 N2 C18 C17 . . . . -65.1(7) ?
C9 O3 C8 C7 . . . . -77.9(7) ?
C2 O1 C3 C4 . . . . -150.6(6) ?
C15 O6 C14 C13 . . . . -75.9(8) ?
C8 O3 C9 C10 . . . . -158.4(5) ?
C12 N1 C13 C14 . . . . 169.3(6) ?
C12 N1 C1 C2 . . . . -62.5(8) ?
C4 O2 C5 C6 . . . . 171.4(6) ?
C6 N2 C7 C8 . . . . -65.1(7) ?
C6 N2 C18 C17 . . . . 167.7(6) ?
C17 O5 C16 C15 . . . . -169.0(6) ?
C13 N1 C12 C11 . . . . -65.1(7) ?
C13 N1 C1 C2 . . . . 170.9(6) ?
C18 N2 C7 C8 . . . . 167.9(5) ?
C18 N2 C6 C5 . . . . -62.6(7) ?
C16 O5 C17 C18 . . . . -172.5(6) ?
C3 O1 C2 C1 . . . . -73.2(8) ?
C10 O4 C11 C12 . . . . -175.5(6) ?
C5 O2 C4 C3 . . . . -170.5(6) ?
C14 O6 C15 C16 . . . . -159.8(6) ?
C1 N1 C12 C11 . . . . 170.0(5) ?
C1 N1 C13 C14 . . . . -64.4(7) ?