#------------------------------------------------------------------------------
#$Date: 2021-05-22 08:04:56 +0300 (Sat, 22 May 2021) $
#$Revision: 265452 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/24/38/2243837.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_2243837
loop_
_publ_author_name
'Butcher, Ray J.'
'Purdy, Andrew P.'
_publ_section_title
;
\m-Methylene-bis[dibromido(diethyl ether-\kO)aluminium(III)]:
crystal structure and chemical exchange in solution
;
_journal_coeditor_code JQ2003
_journal_issue 6
_journal_name_full 'Acta Crystallographica Section E'
_journal_page_first 647
_journal_page_last 652
_journal_paper_doi 10.1107/S2056989021005302
_journal_volume 77
_journal_year 2021
_chemical_formula_iupac '[Al2 Br4 (C H2) (C4 H10 O)2]'
_chemical_formula_moiety 'C9 H22 Al2 Br4 O2'
_chemical_formula_sum 'C9 H22 Al2 Br4 O2'
_chemical_formula_weight 535.86
_chemical_name_systematic
;
\m-Methylene-bis[dibromido(diethyl ether-\kO)aluminium(III)]
;
_space_group_crystal_system monoclinic
_space_group_IT_number 15
_space_group_name_Hall '-C 2yc'
_space_group_name_H-M_alt 'C 1 2/c 1'
_atom_sites_solution_hydrogens mixed
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_audit_creation_method SHELXL-2018/3
_cell_angle_alpha 90
_cell_angle_beta 95.646(3)
_cell_angle_gamma 90
_cell_formula_units_Z 4
_cell_length_a 8.3872(6)
_cell_length_b 12.1039(6)
_cell_length_c 18.1504(12)
_cell_measurement_reflns_used 4301
_cell_measurement_temperature 100(2)
_cell_measurement_theta_max 32.46
_cell_measurement_theta_min 3.09
_cell_volume 1833.7(2)
_computing_cell_refinement
;
SAINT (Bruker, 2002)
;
_computing_data_collection
;
APEX2 (Bruker, 2005)
;
_computing_data_reduction
;
SAINT (Bruker, 2002)
;
_computing_molecular_graphics
;
SHELXTL (Sheldrick 2008)
;
_computing_publication_material
;
SHELXTL (Sheldrick 2008)
;
_computing_structure_refinement
;
SHELXL2018/3 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT (Sheldrick 2015a)
;
_diffrn_ambient_temperature 100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type 'Bruker APEXII CCD'
_diffrn_measurement_method '\f and \w scans'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0725
_diffrn_reflns_av_unetI/netI 0.0498
_diffrn_reflns_limit_h_max 10
_diffrn_reflns_limit_h_min -9
_diffrn_reflns_limit_k_max 15
_diffrn_reflns_limit_k_min -15
_diffrn_reflns_limit_l_max 23
_diffrn_reflns_limit_l_min -23
_diffrn_reflns_number 10600
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 27.099
_diffrn_reflns_theta_min 2.965
_exptl_absorpt_coefficient_mu 8.865
_exptl_absorpt_correction_T_max 0.7471
_exptl_absorpt_correction_T_min 0.2905
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
(SADABS; Sheldrick, 1996)
;
_exptl_crystal_colour colorless
_exptl_crystal_density_diffrn 1.941
_exptl_crystal_description plate
_exptl_crystal_F_000 1032
_exptl_crystal_size_max 0.31
_exptl_crystal_size_mid 0.25
_exptl_crystal_size_min 0.08
_refine_diff_density_max 0.744
_refine_diff_density_min -0.726
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.073
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 83
_refine_ls_number_reflns 2027
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.073
_refine_ls_R_factor_all 0.0396
_refine_ls_R_factor_gt 0.0305
_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^)+(0.0337P)^2^+0.0465P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0723
_refine_ls_wR_factor_ref 0.0759
_reflns_number_gt 1736
_reflns_number_total 2027
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file jq2003sup1.cif
_cod_data_source_block I
_cod_original_sg_symbol_H-M 'C 2/c'
_cod_database_code 2243837
_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 -1 0 2.12 0.24
-2 2 0 258.16 19.18
2 -2 0 251.73 19.16
-3 3 0 150.62 11.13
3 -3 0 146.13 11.13
3 -3 0 144.52 11.10
-4 4 0 77.64 5.79
4 -4 0 73.59 5.84
4 -4 0 73.22 5.76
-5 5 0 117.22 8.51
5 -5 0 109.47 8.47
5 -5 0 104.22 8.55
-6 6 0 22.56 2.36
6 -6 0 24.26 2.38
6 -6 0 20.76 2.39
7 -7 0 15.73 1.76
7 -7 0 16.04 1.90
7 -7 0 8.23 2.29
8 -8 0 1.01 1.49
8 -8 0 2.13 1.83
8 -8 0 -1.85 2.79
8 -10 0 1.79 1.89
8 -10 0 -0.42 2.67
8 -10 0 -1.25 1.86
7 -9 0 3.95 1.62
7 -9 0 5.73 2.01
7 -9 0 4.08 2.11
-7 9 0 5.60 1.98
6 -8 0 10.21 1.52
6 -8 0 10.81 1.93
-6 8 0 12.20 1.76
5 -7 0 215.38 16.87
5 -7 0 217.55 16.77
-5 7 0 232.01 16.89
4 -6 0 4.91 0.74
4 -6 0 3.42 0.93
-4 6 0 4.97 1.08
3 -5 0 138.04 10.39
3 -5 0 137.08 10.44
-3 5 0 137.88 10.51
2 -4 0 902.30 68.50
2 -4 0 907.73 68.47
-2 4 0 926.34 68.55
1 -3 0 37.22 2.83
1 -3 0 37.58 2.87
-1 3 0 37.64 2.98
0 -2 0 516.29 38.85
0 -2 0 465.18 38.86
0 2 0 529.99 38.89
0 2 0 558.38 38.85
1 1 0 2.69 0.32
1 1 0 2.55 0.28
1 1 0 2.43 0.28
2 0 0 3.07 0.40
2 0 0 4.19 0.76
3 -1 0 43.19 3.24
3 -1 0 39.53 3.38
4 -2 0 106.20 8.20
4 -2 0 109.41 8.31
4 -2 0 108.13 8.14
5 -3 0 0.28 1.11
5 -3 0 1.59 0.54
5 -3 0 2.71 0.78
6 -4 0 145.35 10.95
6 -4 0 140.85 11.21
6 -4 0 145.69 11.02
7 -5 0 2.70 1.31
7 -5 0 2.42 1.07
7 -5 0 4.18 1.88
8 -6 0 -3.42 2.28
8 -6 0 -3.84 1.49
8 -6 0 0.71 1.68
9 -7 0 6.81 3.11
9 -7 0 14.10 2.33
7 -11 0 16.80 2.92
-7 11 0 19.63 2.69
6 -10 0 14.99 2.00
6 -10 0 20.05 2.49
-6 10 0 22.87 2.52
5 -9 0 92.57 8.14
5 -9 0 112.97 8.11
4 -8 0 148.94 11.29
4 -8 0 143.59 11.16
-4 8 0 150.26 11.40
3 -7 0 72.11 5.45
3 -7 0 67.99 5.30
-3 7 0 69.68 5.61
2 -6 0 306.47 22.93
2 -6 0 306.56 22.87
-2 6 0 300.10 23.02
1 -5 0 17.16 1.39
1 -5 0 18.54 1.51
-1 5 0 18.72 1.81
0 -4 0 27.40 2.20
0 4 0 27.69 2.39
0 4 0 29.64 2.21
1 3 0 35.29 2.78
1 3 0 36.83 2.75
1 3 0 35.57 2.90
2 2 0 232.44 17.73
2 2 0 234.67 17.71
2 2 0 238.65 17.71
3 1 0 38.29 2.91
3 1 0 36.71 3.34
4 0 0 332.16 28.57
4 0 0 419.71 28.43
5 -1 0 12.54 1.26
5 -1 0 8.91 1.88
6 -2 0 12.41 1.47
6 -2 0 14.82 2.11
7 -3 0 29.93 3.29
8 -4 0 1.46 1.56
8 -4 0 6.12 2.55
9 -5 0 1.42 1.92
9 -5 0 4.54 2.95
6 -12 0 8.26 2.33
-6 12 0 7.10 2.26
5 -11 0 9.91 1.93
-5 11 0 11.43 2.16
4 -10 0 123.03 9.43
-4 10 0 119.61 9.63
3 -9 0 71.49 5.75
-3 9 0 75.03 6.50
2 -8 0 10.48 0.88
2 -8 0 8.99 1.12
-2 8 0 8.35 1.55
1 -7 0 94.66 7.37
1 -7 0 100.60 7.46
-1 7 0 98.77 7.69
0 -6 0 14.63 1.74
0 -6 0 15.97 1.41
0 6 0 17.67 1.96
1 5 0 16.04 1.43
1 5 0 18.79 1.53
1 5 0 15.87 1.79
2 4 0 849.25 63.75
2 4 0 844.38 63.81
2 4 0 852.48 63.74
3 3 0 135.21 10.33
3 3 0 136.71 10.31
4 2 0 103.12 7.82
4 2 0 103.63 7.99
4 2 0 100.89 7.77
5 1 0 13.02 1.31
5 1 0 8.79 2.23
6 0 0 63.60 4.87
6 0 0 53.29 5.78
7 -1 0 3.22 2.65
7 -1 0 5.63 1.32
8 -2 0 5.32 2.89
8 -2 0 5.74 1.61
9 -3 0 45.65 4.11
9 -3 0 31.16 4.73
10 -4 0 2.84 3.66
10 -4 0 1.94 2.20
5 -13 0 0.35 2.01
-5 13 0 2.51 2.27
4 -12 0 6.87 1.77
-4 12 0 7.87 2.12
3 -11 0 137.67 10.58
-3 11 0 135.58 10.79
2 -10 0 80.42 6.12
-2 10 0 75.21 6.46
1 -9 0 98.94 7.57
1 -9 0 92.89 7.42
-1 9 0 107.68 8.20
0 -8 0 204.86 16.52
0 -8 0 221.57 16.50
0 8 0 229.41 16.70
-1 -7 0 91.34 7.32
-1 -7 0 88.91 7.57
1 7 0 102.37 7.37
1 7 0 99.16 7.32
1 7 0 96.70 7.58
2 6 0 271.22 21.06
2 6 0 280.06 20.92
2 6 0 282.14 20.96
3 5 0 128.13 9.75
3 5 0 126.60 9.60
3 5 0 124.97 9.64
4 4 0 69.16 5.27
4 4 0 67.16 5.33
4 4 0 66.22 5.29
5 3 0 0.85 1.25
5 3 0 2.58 0.72
5 3 0 3.20 0.90
6 2 0 9.22 1.27
6 2 0 12.24 2.23
7 1 0 6.49 1.34
7 1 0 5.74 2.96
8 0 0 97.82 9.17
8 0 0 97.74 7.80
9 -1 0 21.72 2.55
9 -1 0 24.54 4.30
10 -2 0 -0.95 2.13
10 -2 0 0.52 4.24
4 -14 0 36.54 3.76
-4 14 0 39.22 4.82
3 -13 0 69.15 5.72
-3 13 0 65.23 6.25
2 -12 0 3.89 1.40
-2 12 0 4.55 2.01
1 -11 0 34.24 3.19
-1 11 0 36.28 3.78
0 -10 0 83.48 7.25
0 -10 0 99.78 7.34
0 10 0 103.34 7.68
-1 -9 0 79.49 7.29
-1 -9 0 91.39 6.92
1 9 0 94.42 6.90
-2 -8 0 13.72 1.84
2 8 0 6.66 1.58
2 8 0 8.80 1.24
2 8 0 7.78 0.99
3 7 0 65.42 5.07
3 7 0 62.05 4.96
3 7 0 64.30 5.26
4 6 0 3.92 1.02
4 6 0 3.18 1.24
4 6 0 4.23 0.86
5 5 0 105.69 8.06
5 5 0 105.15 8.02
5 5 0 100.33 8.01
6 4 0 132.86 10.33
6 4 0 141.85 10.53
6 4 0 133.24 10.40
7 3 0 29.74 3.51
7 3 0 33.52 3.04
8 2 0 2.44 2.95
8 2 0 9.74 1.66
9 1 0 12.75 4.07
9 1 0 22.12 2.48
10 0 0 3.64 4.33
10 0 0 2.56 2.15
2 -14 0 18.11 2.36
-2 14 0 16.87 2.95
1 -13 0 39.49 3.78
-1 13 0 39.02 4.41
0 -12 0 66.44 5.42
0 -12 0 70.12 5.69
0 12 0 77.47 6.33
-1 -11 0 30.70 3.10
-1 -11 0 31.62 2.95
1 11 0 32.21 3.70
-2 -10 0 70.94 5.82
-2 -10 0 59.22 6.57
2 10 0 77.10 6.26
2 10 0 80.12 5.78
3 9 0 66.44 5.27
3 9 0 61.88 5.57
4 8 0 129.30 10.18
4 8 0 132.88 10.29
4 8 0 138.88 10.48
5 7 0 205.31 15.46
5 7 0 200.98 15.53
5 7 0 201.90 15.39
6 6 0 21.02 2.33
6 6 0 22.70 2.41
6 6 0 18.26 2.40
7 5 0 3.45 1.09
7 5 0 3.64 1.70
7 5 0 2.83 1.39
8 4 0 2.33 1.52
8 4 0 0.30 2.27
9 3 0 29.86 4.34
9 3 0 37.16 3.75
10 2 0 -1.89 2.01
10 2 0 -0.41 3.81
1 -15 0 25.59 2.92
-1 15 0 26.60 3.61
0 -14 0 165.23 12.70
0 14 0 162.49 13.10
-1 -13 0 34.08 3.48
-1 -13 0 40.62 3.60
1 13 0 38.13 4.36
-2 -12 0 3.96 1.38
-2 -12 0 -0.22 2.45
2 12 0 6.45 2.15
-3 -11 0 106.51 10.15
3 11 0 127.40 9.39
3 11 0 124.76 9.82
4 10 0 107.61 8.61
4 10 0 110.27 9.04
4 10 0 118.32 9.05
5 9 0 97.99 8.07
5 9 0 97.04 7.71
5 9 0 102.55 7.87
6 8 0 10.87 1.79
6 8 0 11.44 1.54
6 8 0 10.30 1.91
7 7 0 12.03 1.80
7 7 0 12.24 1.89
7 7 0 13.33 1.83
8 6 0 0.07 1.91
8 6 0 -0.26 1.58
8 6 0 0.98 1.24
9 5 0 5.76 2.51
9 5 0 5.34 2.64
10 4 0 3.50 2.03
-1 -15 0 27.57 2.96
1 15 0 26.24 3.61
-2 -14 0 11.85 2.02
-2 -14 0 13.26 2.45
2 14 0 15.02 2.90
-3 -13 0 52.70 6.38
-3 -13 0 55.87 5.11
3 13 0 58.80 4.90
3 13 0 64.89 5.92
-4 -12 0 7.10 3.35
4 12 0 7.70 1.45
4 12 0 7.56 2.03
4 12 0 5.63 2.42
5 11 0 11.26 1.60
5 11 0 10.75 2.41
5 11 0 11.01 2.13
6 10 0 21.90 2.52
6 10 0 16.94 2.03
6 10 0 19.28 2.67
7 9 0 3.32 1.47
7 9 0 4.21 1.88
7 9 0 2.30 1.84
8 8 0 2.08 1.70
8 8 0 5.32 1.83
8 8 0 1.49 1.92
9 7 0 9.52 2.24
9 7 0 11.68 2.38
-4 -14 0 29.66 4.67
-4 -14 0 23.34 3.03
4 14 0 41.12 4.88
4 14 0 34.34 3.23
-5 -13 0 0.58 3.91
5 13 0 1.74 3.35
5 13 0 0.31 1.57
5 13 0 -1.73 2.25
-6 -12 0 2.78 3.79
6 12 0 4.89 2.32
6 12 0 4.99 1.55
6 12 0 5.18 2.51
7 11 0 16.08 2.80
7 11 0 16.32 3.01
7 11 0 16.86 2.10
8 10 0 -0.38 2.02
8 10 0 3.08 2.24
8 10 -1 9.01 1.76
8 10 -1 10.55 2.22
8 10 -1 5.89 2.23
7 11 -1 0.82 2.17
7 11 -1 2.97 2.17
7 11 -1 2.58 1.46
6 12 -1 66.92 6.07
6 12 -1 61.66 5.81
6 12 -1 59.92 5.30
5 13 -1 8.13 1.62
5 13 -1 5.93 3.52
5 13 -1 13.13 2.52
-5 -13 1 6.84 3.93
4 14 -1 6.65 2.70
4 14 -1 1.64 2.59
-4 -14 1 -0.18 1.91
-4 -14 1 -1.35 3.75
9 7 -1 8.94 2.11
9 7 -1 7.97 2.07
8 8 -1 81.03 6.73
8 8 -1 76.95 6.75
8 8 -1 85.83 6.72
7 9 -1 9.33 1.51
7 9 -1 5.16 1.88
7 9 -1 7.57 1.83
6 10 -1 36.03 3.73
6 10 -1 32.72 4.08
6 10 -1 36.82 3.31
5 11 -1 3.09 1.79
5 11 -1 2.36 2.11
5 11 -1 1.02 1.21
4 12 -1 37.87 3.73
4 12 -1 33.49 3.10
4 12 -1 36.63 4.26
-4 -12 1 25.84 2.96
-4 -12 1 35.24 4.38
3 13 -1 1.69 2.24
-3 -13 1 -3.69 3.18
-3 -13 1 -0.30 1.50
2 14 -1 1.29 2.36
-2 -14 1 -2.17 1.95
-2 -14 1 1.14 1.62
1 15 -1 8.60 2.76
-1 -15 1 7.05 2.00
10 4 -1 21.16 3.57
10 4 -1 19.93 2.61
9 5 -1 0.00 2.27
8 6 -1 80.98 6.71
8 6 -1 77.20 6.38
8 6 -1 72.44 6.53
-8 -6 1 86.75 6.42
7 7 -1 18.00 1.92
7 7 -1 16.17 1.99
7 7 -1 13.56 1.93
6 8 -1 27.36 2.61
6 8 -1 25.71 2.55
6 8 -1 23.03 3.02
5 9 -1 9.29 1.98
5 9 -1 10.85 1.72
5 9 -1 11.95 1.40
4 10 -1 2.46 1.83
4 10 -1 4.17 1.49
4 10 -1 2.36 1.03
3 11 -1 2.45 1.87
3 11 -1 3.28 1.08
3 11 -1 4.94 1.53
-3 -11 1 3.95 2.68
-3 -11 1 1.65 1.21
2 12 -1 79.82 6.70
-2 -12 1 60.83 6.91
-2 -12 1 79.34 6.13
1 13 -1 37.50 4.08
-1 -13 1 28.91 3.04
-1 -13 1 34.94 3.34
0 14 -1 18.95 2.95
0 -14 1 16.28 2.24
-1 15 -1 6.25 2.72
1 -15 1 3.78 1.97
10 2 -1 16.73 4.14
10 2 -1 21.77 2.66
9 3 -1 4.35 1.69
9 3 -1 1.04 2.91
8 4 -1 5.89 2.20
8 4 -1 5.91 1.58
7 5 -1 136.18 10.40
7 5 -1 130.85 10.21
7 5 -1 133.76 10.32
6 6 -1 16.24 2.12
6 6 -1 13.80 1.76
6 6 -1 17.79 1.88
5 7 -1 7.01 1.49
5 7 -1 6.08 1.07
4 8 -1 30.52 2.87
4 8 -1 29.53 3.21
4 8 -1 30.79 2.65
3 9 -1 2.52 1.15
3 9 -1 1.81 0.84
3 9 -1 -1.47 1.48
2 10 -1 18.92 2.02
2 10 -1 21.31 2.47
-2 -10 1 19.55 2.14
-2 -10 1 20.50 2.79
1 11 -1 5.10 1.90
-1 -11 1 4.82 1.74
-1 -11 1 7.72 1.25
0 12 -1 115.83 9.34
0 -12 1 115.07 8.99
-1 13 -1 0.72 2.01
1 -13 1 0.68 1.44
-2 14 -1 15.34 2.85
2 -14 1 15.92 2.45
10 0 -1 2.14 2.01
10 0 -1 3.67 4.22
9 1 -1 44.10 5.76
9 1 -1 58.25 4.79
8 2 -1 6.12 1.49
8 2 -1 -0.42 2.81
7 3 -1 66.51 6.41
7 3 -1 65.23 5.29
6 4 -1 15.34 1.82
6 4 -1 20.83 2.01
6 4 -1 18.74 1.98
5 5 -1 1.85 0.96
5 5 -1 -0.05 0.95
5 5 -1 2.24 0.91
4 6 -1 29.96 2.68
4 6 -1 29.38 2.84
4 6 -1 31.12 2.55
3 7 -1 2.58 0.66
3 7 -1 2.14 1.23
3 7 -1 1.09 0.88
2 8 -1 62.56 4.95
2 8 -1 62.03 5.26
2 8 -1 65.71 5.02
-1 -9 1 2.06 0.82
-1 -9 1 1.78 1.92
0 10 -1 27.36 3.20
0 -10 1 27.01 2.45
0 -10 1 35.54 2.69
-1 11 -1 5.99 1.78
1 -11 1 5.18 1.24
-2 12 -1 -0.04 1.89
2 -12 1 1.81 1.37
-3 13 -1 16.12 2.55
3 -13 1 11.16 2.09
-4 14 -1 23.13 3.27
4 -14 1 27.47 3.04
10 -2 -1 14.92 2.80
9 -1 -1 64.77 5.58
9 -1 -1 63.90 6.55
8 0 -1 1.69 1.41
8 0 -1 -0.42 3.23
7 1 -1 4.71 1.15
7 1 -1 7.33 4.96
6 2 -1 65.31 5.07
6 2 -1 60.70 5.86
5 3 -1 110.47 8.53
5 3 -1 109.23 8.48
5 3 -1 115.98 8.67
4 4 -1 39.89 3.15
4 4 -1 37.74 3.13
4 4 -1 38.27 3.19
3 5 -1 12.31 1.37
3 5 -1 11.60 1.38
3 5 -1 12.36 1.23
2 6 -1 147.59 11.64
2 6 -1 154.58 11.50
2 6 -1 154.11 11.54
1 7 -1 11.31 1.11
1 7 -1 10.06 1.00
1 7 -1 9.58 1.42
-1 -7 1 8.65 1.01
-1 -7 1 12.08 1.49
0 8 -1 105.07 7.78
0 -8 1 102.37 7.54
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3 5 19 29.13 7.87
-4 -4 -19 0.30 2.37
4 4 19 2.87 7.05
5 5 -20 15.82 2.61
-5 -5 20 8.70 6.35
4 6 -20 3.54 2.18
-4 -6 20 3.08 5.67
6 2 -20 -0.04 2.05
-6 -2 20 1.46 6.55
5 3 -20 56.30 5.11
-5 -3 20 38.18 8.87
4 4 -20 6.18 2.16
-4 -4 20 6.62 10.04
3 5 -20 30.25 3.02
-3 -5 20 12.92 5.76
2 6 -20 16.36 2.35
-2 -6 20 0.11 5.24
1 7 -20 7.73 2.01
-1 -7 20 -4.17 4.81
6 0 -20 2.85 2.09
-6 0 20 7.99 6.15
5 1 -20 17.62 2.55
-5 -1 20 9.12 6.86
4 2 -20 28.83 3.14
-4 -2 20 29.10 7.12
3 3 -20 2.50 1.90
-3 -3 20 1.37 5.73
2 4 -20 36.78 3.92
1 5 -20 -0.52 1.78
-1 -5 20 -0.16 4.83
0 -6 20 5.73 4.87
1 -7 20 3.74 5.12
6 -2 -20 0.59 2.07
-6 2 20 4.89 5.03
5 -1 -20 20.03 2.70
-5 1 20 20.60 6.48
-4 0 20 18.14 7.40
3 1 -20 -0.27 1.86
-3 -1 20 -4.66 6.99
2 2 -20 58.37 5.26
-2 -2 20 57.26 8.26
1 3 -20 41.08 4.04
-1 -3 20 36.28 6.58
0 4 -20 75.29 6.27
-1 5 -20 0.76 1.68
1 -5 20 3.39 1.29
1 -5 20 0.47 4.88
-2 6 -20 -0.62 1.58
2 -6 20 0.57 5.05
2 -6 20 1.69 1.67
5 -3 -20 59.17 5.19
-5 3 20 40.45 6.92
4 -2 -20 29.18 3.24
-4 2 20 29.77 7.22
3 -1 -20 -1.25 1.87
-3 1 20 2.64 6.97
2 0 -20 74.33 6.48
-2 0 20 79.15 10.14
1 1 -20 7.61 1.94
-1 -1 20 12.00 6.78
0 2 -20 67.69 5.52
0 -2 20 55.71 8.20
0 -2 20 62.38 5.05
-1 3 -20 -3.95 1.65
1 -3 20 0.03 1.24
-2 4 -20 -2.23 1.63
2 -4 20 7.72 5.24
2 -4 20 -0.86 1.47
-3 5 -20 10.63 1.93
3 -5 20 11.26 5.65
3 -5 20 12.43 2.15
5 -5 -20 12.79 2.54
-5 5 20 14.92 4.96
4 -4 -20 9.14 2.35
4 -4 -20 8.46 1.49
3 -3 -20 3.05 1.07
3 -3 -20 -0.33 2.18
-3 3 20 3.72 6.32
2 -2 -20 60.56 5.57
2 -2 -20 64.67 4.95
-2 2 20 52.06 9.11
1 -1 -20 8.62 2.05
-1 1 20 6.05 1.11
-1 1 20 5.40 7.35
0 0 -20 49.68 4.56
0 0 20 48.16 4.12
0 0 20 48.62 8.76
-1 1 -20 -3.59 1.73
1 -1 20 -0.50 1.31
1 -1 20 -1.47 6.49
-2 2 -20 16.53 2.34
2 -2 20 21.47 10.64
2 -2 20 18.30 2.14
-3 3 -20 34.08 3.62
3 -3 20 25.88 6.55
3 -3 20 35.20 3.29
4 -6 -20 2.06 1.64
4 -6 -20 -0.73 2.31
-4 6 20 6.53 4.93
3 -5 -20 28.60 3.47
3 -5 -20 32.06 3.18
-3 5 20 32.09 6.57
2 -4 -20 36.71 4.00
2 -4 -20 43.62 3.80
1 -3 -20 46.80 4.63
-1 3 20 41.20 3.82
-1 3 20 53.09 8.57
0 -2 -20 76.50 6.31
0 2 20 69.52 5.82
0 2 20 65.36 10.08
-1 -1 -20 -4.13 1.90
1 1 20 -0.69 1.44
1 1 20 -2.12 7.75
-2 0 -20 87.22 7.10
2 0 20 59.91 12.03
2 0 20 86.86 6.90
-3 1 -20 9.60 2.14
3 -1 20 8.85 2.03
3 -1 20 15.80 6.85
-4 2 -20 0.00 1.90
4 -2 20 0.29 6.50
4 -2 20 -1.80 1.92
3 -7 -20 78.25 6.57
3 -7 -20 78.63 7.04
-3 7 20 77.33 8.75
2 -6 -20 18.02 2.21
2 -6 -20 14.91 2.90
-2 6 20 17.82 6.13
1 -5 -20 2.83 1.58
1 -5 -20 0.35 2.17
-1 5 20 1.90 6.36
-1 5 20 0.51 1.45
0 -4 -20 90.46 7.07
0 4 20 76.10 6.67
0 4 20 80.68 11.44
-1 -3 -20 -4.66 3.56
1 3 20 -0.12 1.61
2 2 20 13.53 13.97
2 2 20 18.70 2.41
-3 -1 -20 12.22 2.67
3 1 20 14.13 2.24
3 1 20 10.44 8.04
-4 0 -20 14.37 2.48
4 0 20 13.54 2.45
4 0 20 8.06 7.22
1 -7 -20 6.00 2.65
1 -7 -20 8.50 2.05
-1 7 20 5.62 6.08
-1 7 20 3.63 1.83
0 -6 -20 22.59 3.15
0 6 20 24.59 7.27
0 6 20 22.88 2.67
-1 -5 -20 5.62 2.27
1 5 20 3.96 7.25
1 5 20 5.28 1.92
-2 -4 -20 -4.24 2.05
2 4 20 -3.61 1.82
2 4 20 -5.86 7.46
-3 -3 -20 40.42 3.97
3 3 20 38.79 3.85
3 3 20 31.07 8.71
-4 -2 -20 0.89 2.35
4 2 20 -1.95 2.13
4 2 20 4.80 7.66
-1 -7 -20 42.70 4.97
1 7 20 49.92 4.75
1 7 20 41.42 8.33
-2 -6 -20 1.99 2.37
2 6 20 3.33 2.12
2 6 20 1.39 7.31
-3 -5 -20 16.52 2.85
3 5 20 5.05 7.81
5 3 -21 13.80 2.54
-5 -3 21 10.08 7.29
4 4 -21 -0.79 2.18
-4 -4 21 6.04 6.41
3 5 -21 36.92 3.59
-3 -5 21 24.02 6.72
2 6 -21 2.12 2.10
-2 -6 21 2.15 5.37
5 1 -21 -2.27 2.16
-5 -1 21 4.62 7.28
4 2 -21 -1.81 1.99
-4 -2 21 4.78 6.91
3 3 -21 9.45 2.31
-3 -3 21 11.20 6.67
2 4 -21 -3.09 1.92
-2 -4 21 2.41 5.65
1 5 -21 -1.06 1.87
-1 -5 21 2.28 5.41
0 -6 21 8.40 5.30
5 -1 -21 -1.06 2.11
-5 1 21 1.62 7.61
4 0 -21 -0.64 2.04
3 1 -21 0.65 3.65
-3 -1 21 8.30 9.49
2 2 -21 3.99 2.08
-2 -2 21 7.29 6.65
1 3 -21 5.64 1.99
-1 -3 21 14.02 6.11
0 4 -21 -2.51 1.76
0 -4 21 2.00 5.30
-1 5 -21 48.06 4.35
1 -5 21 46.34 4.08
1 -5 21 32.10 6.63
5 -3 -21 13.79 2.62
-5 3 21 12.89 5.96
4 -2 -21 -0.16 2.14
-4 2 21 4.16 7.32
3 -1 -21 6.62 2.22
-3 1 21 18.15 13.17
2 0 -21 -0.87 2.02
1 1 -21 76.05 6.53
-1 -1 21 85.87 11.26
0 2 -21 0.33 1.87
0 -2 21 -0.54 1.01
0 -2 21 11.54 6.07
-1 3 -21 25.76 2.80
1 -3 21 26.42 6.47
1 -3 21 24.48 2.39
-2 4 -21 37.24 3.82
2 -4 21 37.04 3.69
2 -4 21 30.70 6.65
4 -4 -21 -0.54 1.28
4 -4 -21 2.98 2.31
-4 4 21 4.84 6.13
3 -3 -21 8.74 2.46
3 -3 -21 10.47 1.36
-3 3 21 8.04 6.99
2 -2 -21 7.63 1.15
2 -2 -21 2.71 2.25
-2 2 21 16.73 8.57
1 -1 -21 73.65 6.29
-1 1 21 56.53 4.88
-1 1 21 73.70 10.77
0 0 -21 -2.11 1.95
0 0 21 0.21 7.22
0 0 21 -1.04 1.13
-1 1 -21 -1.12 1.79
1 -1 21 3.72 7.05
1 -1 21 -0.16 1.36
-2 2 -21 33.85 3.79
2 -2 21 37.69 7.45
2 -2 21 34.06 3.60
-3 3 -21 3.25 1.90
3 -3 21 3.96 1.88
3 -3 21 7.95 6.22
3 -5 -21 39.33 3.68
-3 5 21 33.43 7.30
2 -4 -21 -1.63 2.25
-2 4 21 -6.89 6.71
1 -3 -21 12.42 2.21
1 -3 -21 9.05 2.30
-1 3 21 3.80 1.62
-1 3 21 -1.33 7.76
0 -2 -21 2.89 2.18
0 2 21 1.94 2.06
0 2 21 2.38 7.98
-1 -1 -21 -0.84 3.37
1 1 21 -1.89 1.46
1 1 21 0.80 8.05
-2 0 -21 -4.80 3.68
2 0 21 -2.04 1.62
2 0 21 -2.77 7.15
-3 1 -21 25.77 2.98
3 -1 21 24.37 2.77
3 -1 21 19.85 7.50
2 -6 -21 5.02 1.69
2 -6 -21 0.79 2.59
-2 6 21 3.04 6.44
1 -5 -21 2.98 1.61
1 -5 -21 -0.55 2.28
-1 5 21 0.45 1.54
-1 5 21 0.40 7.24
0 -4 -21 -2.67 2.11
0 4 21 -9.59 7.63
0 4 21 -1.38 1.51
-1 -3 -21 25.85 3.24
1 3 21 17.71 8.51
1 3 21 31.57 2.93
-2 -2 -21 38.83 3.80
2 2 21 37.33 4.05
2 2 21 28.74 8.73
-3 -1 -21 27.25 3.14
3 1 21 16.50 8.20
3 1 21 25.32 2.93
0 -6 -21 37.06 3.79
0 6 21 31.25 3.29
0 6 21 22.07 7.99
-1 -5 -21 61.73 5.56
1 5 21 54.96 5.26
1 5 21 50.63 9.59
-2 -4 -21 43.04 4.53
2 4 21 41.23 4.47
2 4 21 36.10 9.09
-3 -3 -21 8.09 2.33
3 3 21 2.73 2.15
3 3 21 6.60 7.84
4 2 -22 26.65 3.28
-4 -2 22 24.63 7.83
3 3 -22 12.88 2.51
-3 -3 22 14.30 6.90
2 4 -22 22.92 3.09
-2 -4 22 19.39 6.59
1 5 -22 4.49 2.05
-1 -5 22 3.53 5.95
4 0 -22 34.95 3.74
-4 0 22 33.13 8.76
3 1 -22 3.93 2.21
-3 -1 22 3.51 7.73
2 2 -22 2.08 2.17
-2 -2 22 7.88 7.14
1 3 -22 -3.37 1.93
-1 -3 22 -1.68 6.04
0 4 -22 3.53 1.95
0 -4 22 7.42 5.83
4 -2 -22 28.89 3.48
-4 2 22 29.52 7.87
3 -1 -22 6.25 2.29
-3 1 22 12.30 8.33
2 0 -22 -1.06 2.13
-2 0 22 7.72 7.98
1 1 -22 -5.21 2.37
-1 -1 22 3.27 7.29
0 2 -22 6.79 2.21
0 -2 22 10.23 6.82
-1 3 -22 -2.53 1.85
1 -3 22 0.67 5.85
1 -3 22 -2.00 1.29
3 -3 -22 19.60 2.86
-3 3 22 14.09 7.83
2 -2 -22 1.89 1.23
2 -2 -22 -1.00 2.14
-2 2 22 1.31 7.96
1 -1 -22 -3.36 2.11
1 -1 -22 3.05 1.00
-1 1 22 -0.84 0.95
-1 1 22 -0.49 8.00
0 0 -22 60.52 5.07
0 0 22 46.51 4.35
0 0 22 62.11 9.51
-1 1 -22 -3.59 1.98
1 -1 22 -2.01 2.26
1 -1 22 9.32 7.12
-2 2 -22 -3.48 1.94
2 -2 22 -0.28 1.53
2 -2 22 10.41 6.87
2 -4 -22 25.13 3.46
2 -4 -22 31.25 2.99
-2 4 22 26.47 8.33
1 -3 -22 -0.13 1.38
1 -3 -22 -2.91 2.23
-1 3 22 -1.45 1.41
-1 3 22 -5.48 8.17
0 -2 -22 2.96 2.20
0 2 22 7.01 8.22
0 2 22 6.52 1.51
-1 -1 -22 0.14 2.03
1 1 22 1.09 8.10
1 1 22 0.84 1.54
-2 0 -22 0.14 2.04
2 0 22 0.63 1.70
2 0 22 -0.92 7.47
1 -5 -22 5.62 2.53
1 -5 -22 7.83 1.76
-1 5 22 2.39 1.64
-1 5 22 4.30 7.83
0 -4 -22 4.33 2.42
0 4 22 9.35 8.13
0 4 22 3.91 1.75
-1 -3 -22 -2.97 2.22
1 3 22 0.81 8.33
1 3 22 -1.93 1.71
-2 -2 -22 2.12 2.30
2 2 22 -0.38 1.81
2 2 22 -6.11 7.73
2 0 -23 -0.90 2.22
-2 0 23 3.93 7.93
1 1 -23 9.81 2.30
-1 -1 23 19.83 7.59
1 -1 -23 7.48 2.39
-1 1 23 15.20 8.24
0 0 -23 -3.95 1.99
0 0 23 5.14 7.60
0 0 0 0.00 0.00
;
_shelx_hkl_checksum 67454
_shelx_res_file
;
TITL shelxt_a.res in C2/c
shelx.res
created by SHELXL-2018/3 at 12:17:42 on 10-Feb-2021
CELL 0.71073 8.3872 12.1039 18.1504 90.000 95.646 90.000
ZERR 4.00 0.0006 0.0006 0.0012 0.000 0.003 0.000
LATT 7
SYMM - X, Y, 1/2 - Z
SFAC C H AL BR O
UNIT 36 88 8 16 8
TEMP -173.13
L.S. 10
acta
conf
bond $h
htab
HTAB C2 Br1
EQIV $2 -x+1/2, -y+3/2, -z+1
HTAB C5 Br1_$2
WGHT 0.033700 0.046500
FVAR 0.08154
AL 3 0.116188 0.714229 0.329185 11.00000 0.01223 0.00618 =
0.01263 0.00071 0.00134 -0.00017
BR1 4 -0.028764 0.772399 0.423464 11.00000 0.02233 0.01703 =
0.01919 -0.00335 0.00634 0.00542
BR2 4 0.270350 0.857134 0.291581 11.00000 0.02347 0.01272 =
0.02788 0.00757 -0.00023 -0.00778
O1 5 0.272048 0.623885 0.380738 11.00000 0.01100 0.01017 =
0.01269 0.00284 0.00251 0.00115
C1 1 0.000000 0.632692 0.250000 10.50000 0.01630 0.00880 =
0.01410 0.00000 0.00113 0.00000
H1 2 -0.066075 0.588813 0.272269 11.00000 -1.20000
C2 1 0.243642 0.554995 0.444838 11.00000 0.01671 0.01506 =
0.01279 0.00445 -0.00012 0.00086
AFIX 23
H2A 2 0.204255 0.601947 0.483872 11.00000 -1.20000
H2B 2 0.345754 0.520776 0.465274 11.00000 -1.20000
AFIX 0
C3 1 0.122368 0.465506 0.423408 11.00000 0.01988 0.01594 =
0.02533 0.00419 0.00507 -0.00232
AFIX 137
H3A 2 0.111673 0.417489 0.466116 11.00000 -1.50000
H3B 2 0.158243 0.421669 0.382748 11.00000 -1.50000
H3C 2 0.018501 0.499297 0.407455 11.00000 -1.50000
AFIX 0
C4 1 0.405479 0.584246 0.340736 11.00000 0.01627 0.01426 =
0.01567 -0.00300 0.00636 0.00157
AFIX 23
H4A 2 0.388925 0.608372 0.288425 11.00000 -1.20000
H4B 2 0.408161 0.502482 0.341600 11.00000 -1.20000
AFIX 0
C5 1 0.561819 0.628790 0.375791 11.00000 0.01469 0.02569 =
0.02063 -0.00209 0.00587 0.00147
AFIX 137
H5A 2 0.650079 0.596834 0.351275 11.00000 -1.50000
H5B 2 0.574490 0.609271 0.428443 11.00000 -1.50000
H5C 2 0.563012 0.709361 0.370553 11.00000 -1.50000
AFIX 0
HKLF 4
REM shelxt_a.res in C2/c
REM wR2 = 0.0759, GooF = S = 1.073, Restrained GooF = 1.073 for all data
REM R1 = 0.0305 for 1736 Fo > 4sig(Fo) and 0.0396 for all 2027 data
REM 83 parameters refined using 0 restraints
END
WGHT 0.0336 0.0837
REM Instructions for potential hydrogen bonds
HTAB C2 Br1
HTAB C5 Br1_$2
REM Highest difference peak 0.744, deepest hole -0.726, 1-sigma level 0.135
Q1 1 0.3017 0.8531 0.3363 11.00000 0.05 0.74
Q2 1 0.0484 0.7479 0.4596 11.00000 0.05 0.70
Q3 1 0.1893 0.8794 0.2606 11.00000 0.05 0.66
Q4 1 -0.1124 0.7498 0.3856 11.00000 0.05 0.64
Q5 1 -0.0588 0.7732 0.3700 11.00000 0.05 0.60
Q6 1 0.2378 0.8419 0.2362 11.00000 0.05 0.59
Q7 1 0.0115 0.7807 0.4712 11.00000 0.05 0.59
Q8 1 -0.1120 0.7993 0.3878 11.00000 0.05 0.57
Q9 1 0.2106 0.6563 0.3649 11.00000 0.05 0.47
Q10 1 0.0565 0.6628 0.2788 11.00000 0.05 0.42
Q11 1 0.1569 0.4213 0.4578 11.00000 0.05 0.41
Q12 1 0.1115 0.8439 0.2198 11.00000 0.05 0.41
Q13 1 -0.1358 0.6920 0.4372 11.00000 0.05 0.37
Q14 1 0.2052 0.6024 0.3605 11.00000 0.05 0.36
Q15 1 0.7647 0.7177 0.3689 11.00000 0.05 0.35
Q16 1 0.3432 0.6344 0.4042 11.00000 0.05 0.35
Q17 1 0.5872 0.6403 0.4161 11.00000 0.05 0.35
Q18 1 0.4266 0.9431 0.2919 11.00000 0.05 0.34
Q19 1 0.3552 0.4947 0.5260 11.00000 0.05 0.34
Q20 1 0.3620 0.4244 0.3082 11.00000 0.05 0.33
;
_shelx_res_checksum 63807
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -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
Al Al 0.11619(11) 0.71423(7) 0.32918(6) 0.0103(2) Uani d 1 . .
Br Br1 -0.02876(4) 0.77240(3) 0.42346(2) 0.01923(12) Uani d 1 . .
Br Br2 0.27035(4) 0.85713(3) 0.29158(2) 0.02154(12) Uani d 1 . .
O O1 0.2720(3) 0.62389(16) 0.38074(13) 0.0112(4) Uani d 1 . .
C C1 0.000000 0.6327(3) 0.250000 0.0131(9) Uani d 1 . .
H H1 -0.066(4) 0.589(3) 0.272(2) 0.016 Uiso d 1 . .
C C2 0.2436(4) 0.5550(2) 0.44484(19) 0.0150(7) Uani d 1 . .
H H2A 0.204255 0.601947 0.483872 0.018 Uiso calc 1 . .
H H2B 0.345754 0.520776 0.465274 0.018 Uiso calc 1 . .
C C3 0.1224(4) 0.4655(3) 0.4234(2) 0.0202(8) Uani d 1 . .
H H3A 0.111673 0.417489 0.466116 0.030 Uiso calc 1 . .
H H3B 0.158243 0.421669 0.382748 0.030 Uiso calc 1 . .
H H3C 0.018501 0.499297 0.407455 0.030 Uiso calc 1 . .
C C4 0.4055(4) 0.5842(3) 0.34074(19) 0.0151(7) Uani d 1 . .
H H4A 0.388925 0.608372 0.288425 0.018 Uiso calc 1 . .
H H4B 0.408161 0.502482 0.341600 0.018 Uiso calc 1 . .
C C5 0.5618(4) 0.6288(3) 0.3758(2) 0.0201(7) Uani d 1 . .
H H5A 0.650079 0.596834 0.351275 0.030 Uiso calc 1 . .
H H5B 0.574490 0.609271 0.428443 0.030 Uiso calc 1 . .
H H5C 0.563012 0.709361 0.370553 0.030 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
Al 0.0122(5) 0.0062(4) 0.0126(5) -0.0002(3) 0.0013(4) 0.0007(3)
Br1 0.0223(2) 0.01703(18) 0.0192(2) 0.00542(12) 0.00634(15) -0.00335(13)
Br2 0.0235(2) 0.01272(17) 0.0279(2) -0.00778(12) -0.00023(15) 0.00757(13)
O1 0.0110(11) 0.0102(10) 0.0127(12) 0.0012(8) 0.0025(9) 0.0028(8)
C1 0.016(2) 0.0088(19) 0.014(2) 0.000 0.0011(19) 0.000
C2 0.0167(17) 0.0151(15) 0.0128(17) 0.0009(12) -0.0001(13) 0.0045(13)
C3 0.0199(18) 0.0159(16) 0.025(2) -0.0023(13) 0.0051(15) 0.0042(14)
C4 0.0163(17) 0.0143(14) 0.0157(17) 0.0016(12) 0.0064(14) -0.0030(13)
C5 0.0147(18) 0.0257(17) 0.0206(19) 0.0015(13) 0.0059(14) -0.0021(14)
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'
Al Al 0.0645 0.0514 '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'
O O 0.0106 0.0060 '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
O1 Al C1 . . 110.42(13) y
O1 Al Br2 . . 101.60(7) y
C1 Al Br2 . . 114.90(9) y
O1 Al Br1 . . 101.52(8) y
C1 Al Br1 . . 116.44(5) y
Br2 Al Br1 . . 110.07(4) y
C2 O1 C4 . . 113.3(2) ?
C2 O1 Al . . 124.38(19) ?
C4 O1 Al . . 117.9(2) ?
Al C1 Al . 2 118.4(2) ?
Al C1 H1 . . 105(2) ?
Al C1 H1 2 . 111(2) ?
Al C1 H1 . 2 111(2) ?
Al C1 H1 2 2 105(2) ?
H1 C1 H1 . 2 107(5) ?
O1 C2 C3 . . 111.1(3) ?
O1 C2 H2A . . 109.4 ?
C3 C2 H2A . . 109.4 ?
O1 C2 H2B . . 109.4 ?
C3 C2 H2B . . 109.4 ?
H2A C2 H2B . . 108.0 ?
C2 C3 H3A . . 109.5 ?
C2 C3 H3B . . 109.5 ?
H3A C3 H3B . . 109.5 ?
C2 C3 H3C . . 109.5 ?
H3A C3 H3C . . 109.5 ?
H3B C3 H3C . . 109.5 ?
O1 C4 C5 . . 110.4(3) ?
O1 C4 H4A . . 109.6 ?
C5 C4 H4A . . 109.6 ?
O1 C4 H4B . . 109.6 ?
C5 C4 H4B . . 109.6 ?
H4A C4 H4B . . 108.1 ?
C4 C5 H5A . . 109.5 ?
C4 C5 H5B . . 109.5 ?
H5A C5 H5B . . 109.5 ?
C4 C5 H5C . . 109.5 ?
H5A C5 H5C . . 109.5 ?
H5B C5 H5C . . 109.5 ?
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
Al O1 . 1.881(2) y
Al C1 . 1.927(2) y
Al Br2 . 2.3029(9) y
Al Br1 . 2.3046(10) y
O1 C2 . 1.470(4) ?
O1 C4 . 1.473(4) ?
C1 H1 . 0.89(4) ?
C1 H1 2 0.89(4) ?
C2 C3 . 1.510(4) ?
C2 H2A . 0.9900 ?
C2 H2B . 0.9900 ?
C3 H3A . 0.9800 ?
C3 H3B . 0.9800 ?
C3 H3C . 0.9800 ?
C4 C5 . 1.500(5) ?
C4 H4A . 0.9900 ?
C4 H4B . 0.9900 ?
C5 H5A . 0.9800 ?
C5 H5B . 0.9800 ?
C5 H5C . 0.9800 ?
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
C2 H2A Br1 . 0.99 2.98 3.481(3) 112.8 yes
C5 H5B Br1 7_566 0.98 3.10 3.871(4) 136.3 yes
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
C1 Al O1 C2 . . . . -89.5(2) ?
Br2 Al O1 C2 . . . . 148.1(2) ?
Br1 Al O1 C2 . . . . 34.6(2) ?
C1 Al O1 C4 . . . . 65.4(2) ?
Br2 Al O1 C4 . . . . -57.0(2) ?
Br1 Al O1 C4 . . . . -170.52(18) ?
C4 O1 C2 C3 . . . . -91.5(3) ?
Al O1 C2 C3 . . . . 64.4(3) ?
C2 O1 C4 C5 . . . . -85.6(3) ?
Al O1 C4 C5 . . . . 116.9(3) ?
_cod_database_fobs_code 2243837