#------------------------------------------------------------------------------
#$Date: 2019-06-11 07:19:33 +0300 (Tue, 11 Jun 2019) $
#$Revision: 215810 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/02/16/2021659.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_2021659
loop_
_publ_author_name
'Xu, Jie'
'Zhang, Kou-Lin'
_publ_section_title
;
Preparation, characterization and luminescence-sensing properties of two
ZnII MOFs with mixed 5-amino-2,4,6-tribromoisophthalic acid and
bipyridyl-type ligands
;
_journal_coeditor_code YF3173
_journal_issue 7
_journal_name_full
'Acta Crystallographica Section C Structural Chemistry'
_journal_paper_doi 10.1107/S2053229619007435
_journal_volume 75
_journal_year 2019
_chemical_formula_iupac
'[Zn (C8 H2 Br3 N O4) (C14 H14 N4 O2) (H2 O)2], H2 O'
_chemical_formula_moiety 'C22 H20 Br3 N5 O8 Zn, H2 O'
_chemical_formula_sum 'C22 H22 Br3 N5 O9 Zn'
_chemical_formula_weight 805.54
_chemical_name_systematic
'Poly[[(\m-5-amino-2,4,6-tribromoisophthalato-\k^2^O^1^:O^3^)diaqua[\m-N,N'-bis(pyridin-4-ylmethyl)oxalamide-\k^2^N:N']zinc(II)] monohydrate]'
_space_group_crystal_system orthorhombic
_space_group_IT_number 19
_space_group_name_Hall 'P 2ac 2ab'
_space_group_name_H-M_alt 'P 21 21 21'
_symmetry_space_group_name_Hall 'P 2ac 2ab'
_symmetry_space_group_name_H-M 'P 21 21 21'
_atom_sites_solution_hydrogens mixed
_audit_creation_method SHELXL-2016/6
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_formula_units_Z 4
_cell_length_a 8.5083(5)
_cell_length_b 13.8444(10)
_cell_length_c 22.4960(12)
_cell_measurement_reflns_used 6891
_cell_measurement_temperature 293(2)
_cell_measurement_theta_max 27.0617
_cell_measurement_theta_min 2.3323
_cell_volume 2649.9(3)
_computing_cell_refinement
;
SMART (Bruker, 2008)
;
_computing_data_collection
;
SMART (Bruker, 2008)
;
_computing_data_reduction
;
SAINT (Bruker, 2008)
;
_computing_molecular_graphics
;
SHELXTL (Bruker, 2008)
;
_computing_publication_material
;
SHELXTL (Bruker, 2008)
;
_computing_structure_refinement
;
SHELXL2016 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXL2016 (Sheldrick, 2015a)
;
_diffrn_ambient_temperature 293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type 'Bruker SMART CCD area detector'
_diffrn_measurement_method 'phi and omega scans'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0831
_diffrn_reflns_av_unetI/netI 0.1223
_diffrn_reflns_limit_h_max 10
_diffrn_reflns_limit_h_min -11
_diffrn_reflns_limit_k_max 17
_diffrn_reflns_limit_k_min -18
_diffrn_reflns_limit_l_max 27
_diffrn_reflns_limit_l_min -29
_diffrn_reflns_number 24793
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 27.536
_diffrn_reflns_theta_min 2.333
_exptl_absorpt_coefficient_mu 5.512
_exptl_absorpt_correction_T_max 0.314
_exptl_absorpt_correction_T_min 0.233
_exptl_absorpt_correction_type empirical
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2008)
;
_exptl_crystal_colour white
_exptl_crystal_density_diffrn 2.019
_exptl_crystal_description needle
_exptl_crystal_F_000 396
_exptl_crystal_size_max 0.28
_exptl_crystal_size_mid 0.25
_exptl_crystal_size_min 0.21
_refine_diff_density_max 1.696
_refine_diff_density_min -1.133
_refine_ls_abs_structure_details
;
Flack x determined using 1290 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons et al., 2013)
;
_refine_ls_abs_structure_Flack 0.0(4)
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 0.996
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 361
_refine_ls_number_reflns 6064
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 0.996
_refine_ls_R_factor_all 0.1097
_refine_ls_R_factor_gt 0.0457
_refine_ls_shift/su_max 0.000
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0320P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0688
_refine_ls_wR_factor_ref 0.0788
_reflns_number_gt 4032
_reflns_number_total 6064
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file yf3173sup1.cif
_cod_data_source_block 2
_cod_database_code 2021659
_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 0 0 0.09 0.23
-1 0 0 0.11 0.23
1 0 0 0.40 0.31
1 0 0 0.09 0.18
2 0 0 181.16 7.49
2 0 0 187.76 7.53
-2 0 0 188.33 7.36
-2 0 0 185.50 7.25
3 0 0 -0.81 0.78
3 0 0 -1.15 1.04
-3 0 0 -0.47 0.61
-3 0 0 0.49 0.59
-4 0 0 225.41 9.24
4 0 0 223.60 10.15
4 0 0 220.18 9.91
-4 0 0 226.40 8.96
-5 0 0 0.60 0.83
5 0 0 0.16 1.95
-5 0 0 0.36 1.07
-6 0 0 7.68 1.31
6 0 0 13.28 4.02
-6 0 0 4.24 1.56
6 0 0 6.46 3.16
-7 0 0 1.39 1.12
-7 0 0 -1.02 1.60
7 0 0 0.59 4.05
7 0 0 0.77 5.06
-8 0 0 158.97 7.86
8 0 0 156.23 13.20
8 0 0 159.26 14.63
-8 0 0 152.62 6.87
-9 0 0 2.38 2.32
-9 0 0 1.96 1.60
-10 0 0 48.79 5.51
-10 0 0 46.12 4.71
-11 0 0 3.38 3.54
0 -1 0 -0.54 0.33
0 1 0 -0.08 0.34
0 -1 0 -0.31 0.43
0 1 0 -0.56 0.38
-1 -1 0 92.72 4.26
-1 1 0 88.46 3.40
-1 -1 0 82.90 4.28
1 -1 0 84.65 3.40
1 1 0 91.11 4.34
-1 1 0 82.56 3.34
1 -1 0 91.12 3.41
-2 -1 0 23.03 1.85
-2 1 0 22.19 1.06
2 1 0 22.00 2.56
2 -1 0 24.16 1.36
-2 1 0 23.71 1.29
-2 -1 0 24.82 2.11
2 -1 0 23.24 1.16
2 1 0 23.86 2.28
3 1 0 82.17 4.92
3 1 0 88.41 5.37
3 -1 0 84.57 3.74
3 -1 0 81.10 3.90
-3 -1 0 82.85 4.27
-3 1 0 82.21 3.38
-3 1 0 82.78 3.68
-3 -1 0 84.27 4.21
4 -1 0 -0.36 1.12
4 1 0 -1.96 2.16
-4 1 0 0.18 0.46
4 1 0 -1.27 1.92
4 -1 0 -0.34 1.01
-4 1 0 0.03 0.72
-4 -1 0 -0.12 1.10
-4 -1 0 -0.35 1.07
-5 -1 0 195.11 8.40
5 -1 0 201.26 9.21
5 -1 0 201.96 9.07
-5 1 0 193.76 8.18
5 1 0 191.72 10.71
-5 1 0 182.97 7.97
-5 -1 0 194.93 8.60
5 1 0 190.96 10.22
6 1 0 59.16 6.52
-6 -1 0 59.94 3.74
-6 -1 0 63.59 4.21
6 -1 0 59.00 5.30
-6 1 0 61.56 3.03
6 -1 0 58.52 6.05
-6 1 0 62.32 3.81
6 1 0 65.29 7.13
-7 -1 0 0.67 1.72
-7 -1 0 1.43 1.41
7 -1 0 -2.46 4.38
7 1 0 1.11 5.35
-7 1 0 -0.36 1.53
7 1 0 -5.57 5.64
-7 1 0 -0.18 0.94
7 -1 0 0.61 3.39
8 -1 0 9.68 6.38
-8 1 0 4.87 1.35
-8 1 0 6.96 2.09
8 -1 0 11.20 5.67
8 1 0 22.83 9.65
-8 -1 0 3.81 2.42
8 1 0 26.71 8.07
-8 -1 0 4.96 1.70
-9 1 0 18.86 3.04
-9 -1 0 23.40 2.54
-9 -1 0 23.92 3.54
-9 1 0 20.85 2.52
-10 -1 0 8.05 3.22
-10 -1 0 6.29 2.15
-10 1 0 11.88 4.59
-11 1 0 4.22 3.36
-11 -1 0 0.06 4.88
0 2 0 6.24 1.25
0 -2 0 7.92 1.48
0 -2 0 4.60 1.15
0 2 0 6.63 1.39
-1 2 0 244.05 9.33
1 -2 0 234.78 8.98
1 2 0 244.37 10.63
-1 2 0 236.27 8.99
-1 -2 0 236.89 10.51
1 -2 0 234.20 9.49
-2 -2 0 901.16 34.17
-2 -2 0 919.90 34.03
2 -2 0 816.75 32.49
-2 2 0 828.54 32.44
2 2 0 920.45 34.43
2 -2 0 897.79 32.56
2 -2 0 847.84 32.32
3 -2 0 42.40 1.96
-3 -2 0 40.93 4.33
-3 2 0 41.42 2.34
3 -2 0 39.31 2.24
3 -2 0 45.74 2.03
3 2 0 45.81 4.73
3 2 0 41.14 4.51
-3 -2 0 43.48 3.37
4 -2 0 95.34 4.29
-4 -2 0 97.01 5.31
4 -2 0 91.54 4.61
-4 -2 0 94.32 5.51
4 2 0 102.42 7.40
-4 2 0 92.88 4.27
4 2 0 98.30 7.55
-4 2 0 97.00 3.92
-5 2 0 20.92 1.92
-5 2 0 21.06 1.42
5 -2 0 21.58 2.75
5 2 0 24.50 5.11
-5 -2 0 22.75 2.78
-5 -2 0 23.11 2.66
5 -2 0 24.38 2.86
5 2 0 15.12 4.32
6 -2 0 252.45 11.53
-6 -2 0 265.20 11.45
6 2 0 232.48 14.62
6 2 0 256.48 15.20
-6 2 0 248.91 10.41
-6 -2 0 242.35 10.97
-6 2 0 254.04 9.83
7 2 0 25.35 7.68
7 -2 0 23.03 3.86
7 2 0 13.38 6.70
-7 -2 0 26.56 3.35
-7 -2 0 26.07 2.92
7 -2 0 28.00 5.04
-7 2 0 25.22 2.01
-7 2 0 24.57 2.87
8 2 0 8.86 8.96
8 2 0 4.39 9.12
-8 -2 0 5.55 2.09
-8 -2 0 5.39 2.47
8 -2 0 10.99 4.79
8 -2 0 5.83 1.52
-8 2 0 4.61 1.98
8 -2 0 -9.12 5.67
-9 -2 0 20.37 2.84
9 -2 0 17.63 2.40
9 2 0 16.57 16.58
-9 -2 0 18.52 3.45
-9 2 0 22.37 3.07
-10 -2 0 -0.13 3.10
-10 -2 0 -2.86 2.31
0 3 0 -1.01 1.34
0 3 0 1.00 1.61
0 -3 0 0.01 1.50
0 -3 0 0.27 1.13
-1 3 0 100.59 5.03
-1 -3 0 101.99 6.53
1 -3 0 107.09 5.45
-1 3 0 108.47 4.37
-1 -3 0 103.22 7.29
1 -3 0 108.93 4.29
2 -3 0 188.34 8.05
2 3 0 178.71 9.75
2 -3 0 191.20 7.45
-2 3 0 196.64 7.42
-2 3 0 194.12 7.57
3 3 0 9.03 3.56
3 -3 0 6.36 0.91
-3 -3 0 8.23 2.49
3 -3 0 5.46 1.05
-3 -3 0 5.27 2.31
-3 3 0 5.54 0.82
3 -3 0 5.26 0.59
-4 -3 0 88.36 5.78
4 -3 0 90.72 4.33
4 -3 0 91.45 3.81
4 -3 0 86.96 4.04
-4 -3 0 83.80 5.87
4 3 0 93.90 8.24
-4 3 0 87.21 4.00
5 -3 0 91.79 4.31
-5 -3 0 96.33 5.95
5 -3 0 84.37 4.09
-5 3 0 85.15 4.21
5 3 0 86.84 9.08
5 -3 0 90.28 4.83
-5 -3 0 85.58 6.00
-6 -3 0 3.77 2.48
6 3 0 -12.06 5.98
6 3 0 4.57 6.19
6 -3 0 3.79 2.01
6 -3 0 2.87 1.15
-6 -3 0 5.01 2.28
6 -3 0 7.48 2.15
-6 3 0 3.85 1.36
-7 -3 0 -0.17 2.27
7 -3 0 -0.49 2.64
-7 3 0 -1.19 1.42
7 -3 0 -0.32 1.19
7 3 0 1.89 7.26
-7 -3 0 -0.43 2.13
7 -3 0 2.52 3.29
7 3 0 13.75 8.81
-8 3 0 8.59 2.17
8 -3 0 10.95 1.99
-8 -3 0 4.02 2.95
8 -3 0 6.58 5.48
8 -3 0 7.93 4.25
8 3 0 3.81 10.28
-8 -3 0 3.85 2.58
-9 -3 0 78.51 5.81
9 -3 0 78.43 5.19
-9 3 0 81.48 5.48
-9 -3 0 83.16 6.57
-10 -3 0 -5.05 2.61
-10 -3 0 -3.15 3.47
-10 3 0 -1.39 2.62
0 -4 0 286.84 13.26
0 4 0 316.86 14.67
0 -4 0 308.27 14.20
0 4 0 329.41 13.94
-1 -4 0 381.95 17.86
-1 4 0 365.32 15.14
-1 4 0 377.07 14.44
-1 -4 0 355.89 16.64
1 -4 0 346.57 14.04
1 -4 0 374.60 15.93
1 4 0 377.89 16.72
2 -4 0 20.04 1.30
2 -4 0 17.59 2.37
-2 4 0 20.30 1.94
-2 4 0 18.87 1.32
2 4 0 18.62 3.90
-2 -4 0 19.94 3.73
-3 4 0 118.28 4.94
3 4 0 129.80 8.82
3 -4 0 116.65 5.85
-3 4 0 118.80 4.91
-3 -4 0 111.38 7.68
3 -4 0 117.42 5.02
-4 -4 0 163.50 9.25
4 -4 0 159.21 6.85
4 -4 0 155.13 7.22
-4 4 0 162.94 6.60
4 -4 0 156.89 6.30
-4 -4 0 163.87 9.38
4 4 0 156.72 10.98
-5 -4 0 53.70 5.36
5 -4 0 50.77 3.54
5 -4 0 49.66 3.34
5 4 0 53.37 7.38
5 -4 0 49.38 2.71
-5 4 0 48.97 2.89
-5 -4 0 52.43 5.29
6 -4 0 -1.34 1.50
-6 -4 0 -0.93 2.38
6 4 0 7.73 6.51
6 -4 0 -0.16 1.71
-6 4 0 -0.94 1.09
-6 -4 0 0.70 2.70
6 -4 0 -2.04 1.53
-7 4 0 85.14 4.82
7 4 0 87.57 11.90
-7 -4 0 81.18 6.60
-7 -4 0 100.51 6.85
7 -4 0 93.19 6.34
7 -4 0 89.86 6.33
7 -4 0 83.86 5.17
-8 4 0 0.73 1.76
8 -4 0 3.57 2.32
-8 -4 0 -1.38 2.85
8 -4 0 4.49 4.74
-8 -4 0 -3.92 2.85
8 4 0 -3.13 13.03
-9 -4 0 18.93 4.24
-9 -4 0 16.38 3.52
-9 4 0 20.41 2.96
9 -4 0 9.70 3.86
-10 4 0 6.30 3.28
-10 -4 0 1.97 3.34
0 5 0 3.92 2.96
0 5 0 -2.92 2.75
0 -5 0 -0.73 1.66
0 -5 0 -1.86 2.27
-1 -5 0 372.04 18.29
-1 -5 0 410.54 19.51
1 -5 0 374.65 17.67
1 -5 0 391.98 15.33
1 5 0 409.24 18.36
-1 5 0 411.99 16.82
2 -5 0 65.25 5.64
-2 5 0 73.66 3.45
2 5 0 70.69 7.41
-2 -5 0 71.21 6.68
2 -5 0 67.17 3.17
-2 -5 0 68.58 8.29
-2 5 0 67.54 4.13
3 -5 0 147.49 7.93
-3 5 0 152.57 6.46
-3 -5 0 152.98 9.77
-3 5 0 147.05 6.23
3 5 0 157.96 11.10
4 -5 0 7.70 0.92
-4 -5 0 6.00 4.28
4 -5 0 7.67 1.28
4 5 0 12.34 5.66
-4 -5 0 1.06 3.32
4 -5 0 3.81 2.43
-4 5 0 7.75 1.19
5 5 0 58.62 8.46
5 -5 0 47.51 2.51
5 -5 0 48.87 3.35
-5 -5 0 52.40 6.00
-5 -5 0 43.07 5.42
-5 5 0 46.34 2.88
6 -5 0 -0.10 1.73
6 -5 0 2.26 2.06
-6 5 0 1.33 1.29
-6 -5 0 1.60 3.31
6 -5 0 1.27 1.32
6 5 0 -8.64 7.35
-6 -5 0 2.33 3.45
7 -5 0 38.30 4.17
7 -5 0 38.89 4.50
7 5 0 43.21 11.38
-7 -5 0 48.12 6.10
-7 5 0 39.84 3.29
7 -5 0 49.11 4.90
-7 -5 0 42.35 5.57
-8 -5 0 -1.89 3.56
8 -5 0 -4.20 3.92
-8 5 0 1.66 1.80
8 -5 0 0.67 3.17
-8 -5 0 3.39 3.57
-9 -5 0 84.41 7.46
-9 -5 0 91.49 7.97
-9 5 0 85.64 5.59
-10 -5 0 -0.62 6.96
-10 -5 0 6.94 3.86
0 6 0 16.54 3.73
0 -6 0 10.91 2.35
0 6 0 14.04 4.64
0 -6 0 11.43 3.75
1 6 0 81.25 9.68
-1 6 0 76.19 5.83
1 -6 0 82.53 4.13
1 6 0 73.36 7.54
-1 -6 0 76.75 8.03
1 -6 0 78.37 7.13
-1 6 0 82.98 5.74
-1 -6 0 84.45 8.42
2 6 0 5.60 4.16
2 -6 0 4.22 1.05
-2 6 0 3.85 1.19
2 -6 0 4.18 2.98
-2 -6 0 4.48 3.88
-2 6 0 2.59 2.29
-2 -6 0 2.38 5.28
-3 -6 0 16.90 4.52
3 -6 0 16.46 3.61
3 -6 0 23.56 1.86
-3 6 0 27.80 2.01
3 6 0 22.19 6.14
-3 6 0 23.70 2.89
-4 -6 0 366.82 18.59
4 -6 0 388.13 15.04
-4 6 0 384.07 14.90
4 6 0 390.24 21.23
-4 -6 0 383.39 20.78
-4 6 0 378.10 15.14
4 -6 0 374.62 17.04
-5 -6 0 3.99 4.23
5 6 0 1.18 6.82
5 -6 0 2.57 2.97
5 -6 0 2.80 1.53
-5 -6 0 4.67 3.92
-5 6 0 2.78 1.18
5 -6 0 2.35 1.25
6 -6 0 1.14 3.39
6 6 0 7.40 9.28
6 -6 0 4.46 1.85
6 -6 0 2.13 1.16
-6 -6 0 0.26 3.61
-6 6 0 -0.13 1.32
-6 -6 0 2.42 3.70
7 -6 0 89.83 7.55
7 -6 0 100.40 5.55
7 -6 0 96.25 6.61
-7 -6 0 110.80 9.01
-7 6 0 97.90 5.29
-7 -6 0 104.96 8.34
8 -6 0 23.23 4.80
-8 -6 0 29.11 4.95
-8 6 0 28.70 3.06
-8 -6 0 36.26 5.43
-9 6 0 -0.24 2.15
-9 -6 0 4.69 4.58
-9 -6 0 0.17 4.05
-10 -6 0 33.16 5.89
-10 6 0 19.02 4.36
-10 -6 0 20.42 5.30
0 -7 0 0.55 2.28
0 -7 0 4.83 4.06
0 7 0 2.90 3.32
0 7 0 7.91 4.88
1 7 0 156.35 13.75
-1 -7 0 152.53 11.40
-1 7 0 162.39 8.95
1 7 0 130.02 10.20
1 -7 0 142.12 10.20
1 -7 0 121.75 7.01
-1 -7 0 151.50 11.06
-1 7 0 155.14 8.96
-2 7 0 94.77 5.33
2 7 0 85.37 9.13
2 -7 0 93.58 4.39
-2 -7 0 89.51 9.48
-2 7 0 97.55 6.16
2 -7 0 80.92 7.75
3 -7 0 246.52 9.85
-3 -7 0 233.45 18.22
-3 7 0 250.19 10.20
3 7 0 236.66 15.32
-3 -7 0 230.86 14.91
-3 7 0 244.53 10.69
3 -7 0 237.15 13.40
-4 7 0 5.41 1.36
4 -7 0 5.49 1.30
4 -7 0 1.85 3.87
-4 -7 0 1.12 4.16
4 7 0 -1.18 6.68
-4 7 0 1.50 1.33
-4 -7 0 -3.47 5.94
-5 -7 0 173.89 13.30
5 7 0 186.37 17.36
5 -7 0 195.44 8.68
-5 7 0 211.45 8.62
5 -7 0 201.67 8.05
5 -7 0 202.51 11.63
-5 -7 0 187.12 13.12
6 -7 0 5.05 4.03
-6 -7 0 -4.35 4.21
-6 7 0 4.52 1.63
-6 -7 0 4.95 4.62
6 -7 0 2.10 1.19
6 -7 0 4.24 1.88
-7 7 0 37.81 3.62
7 -7 0 55.35 5.22
-7 -7 0 35.78 6.40
-7 -7 0 31.98 6.28
7 -7 0 43.40 6.17
7 -7 0 42.99 3.59
-8 7 0 0.71 1.98
8 -7 0 -4.90 5.08
-8 -7 0 -3.59 8.47
-8 -7 0 -3.70 4.34
-9 7 0 0.48 2.66
-9 -7 0 3.30 5.01
-9 -7 0 2.40 5.44
-10 7 0 7.80 2.99
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-2 1 -9 444.42 17.18
2 -1 -9 443.07 16.89
-2 1 -9 468.14 16.81
2 1 9 453.35 17.11
-2 1 -9 428.07 16.66
2 -1 -9 457.23 17.24
-3 1 9 210.27 8.48
-3 -1 -9 199.66 10.63
3 1 -9 208.34 9.23
-3 -1 -9 205.69 8.95
3 1 -9 215.46 9.36
3 -1 9 210.21 9.45
-3 1 9 201.17 8.06
3 1 9 207.74 8.48
3 -1 -9 208.35 8.49
-3 1 -9 189.08 8.93
-3 1 -9 203.56 7.89
-3 -1 9 206.56 8.22
-3 -1 9 207.97 8.61
3 -1 -9 204.74 8.67
-3 1 -9 198.95 8.10
4 1 -9 62.85 4.79
-4 1 9 56.62 3.19
-4 -1 -9 50.56 3.52
-4 -1 -9 54.85 6.74
4 -1 9 50.10 4.74
4 1 -9 53.15 4.38
4 1 9 56.45 3.41
4 -1 -9 54.93 3.79
-4 1 -9 58.92 4.53
4 -1 -9 54.60 3.58
-4 -1 9 59.97 3.46
-4 1 -9 56.46 2.99
-4 1 -9 55.09 2.37
5 1 -9 80.99 6.06
-5 1 9 84.73 4.17
-5 -1 -9 78.30 7.48
5 -1 9 82.43 6.69
-5 1 9 83.59 3.91
-5 -1 -9 81.20 4.71
5 1 -9 80.44 6.14
5 1 9 72.44 4.41
5 -1 -9 70.33 4.97
5 -1 -9 78.10 4.97
-5 -1 9 68.53 3.94
-5 -1 9 69.54 4.16
-5 1 -9 76.40 3.64
-5 1 -9 71.83 2.99
-5 1 -9 76.23 3.95
-6 1 9 112.95 5.64
6 1 -9 113.36 9.31
6 1 -9 127.07 9.31
-6 -1 -9 112.31 6.31
-6 -1 -9 113.20 7.77
-6 1 9 114.55 5.80
6 1 9 119.95 6.30
6 -1 -9 116.16 7.80
6 -1 -9 126.80 7.43
-6 1 -9 126.26 5.89
-6 -1 9 125.03 6.11
-6 -1 9 128.34 5.98
7 1 -9 31.91 6.28
-7 1 9 24.01 3.03
-7 1 9 28.44 3.04
-7 -1 -9 30.52 3.63
-7 -1 -9 34.31 3.90
-7 -1 9 29.76 3.09
7 -1 -9 36.06 5.11
-7 1 -9 31.00 3.23
-7 -1 9 32.41 3.34
8 1 -9 22.74 8.66
-8 1 9 17.88 2.55
-8 -1 -9 23.69 2.31
-8 1 9 18.29 2.64
-8 -1 9 20.23 2.83
8 -1 -9 31.29 6.36
-8 -1 9 15.75 2.63
-9 -1 -9 13.18 3.25
-9 -1 9 12.82 2.76
-9 1 -9 8.69 2.66
-10 -1 -9 15.38 3.83
-10 -1 9 11.03 3.16
-10 1 -9 5.48 3.02
10 -1 -9 5.38 3.30
0 2 -9 182.85 7.63
0 2 9 185.11 9.11
0 -2 9 174.64 7.22
0 2 9 184.18 7.48
0 -2 -9 174.79 7.14
0 -2 -9 178.85 8.07
-1 -2 -9 227.59 9.84
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-1 -2 -9 210.58 10.68
1 2 -9 224.79 9.10
-1 -2 9 210.30 10.24
-1 -2 9 201.52 8.58
-1 2 -9 209.57 8.62
1 -2 -9 200.41 8.97
1 -2 -9 207.47 8.15
-1 -2 9 208.34 8.15
1 2 9 212.65 8.75
1 -2 -9 210.15 8.56
-1 2 -9 208.94 8.05
2 2 -9 38.10 3.40
2 2 -9 38.55 4.05
2 -2 9 38.23 2.19
-2 -2 -9 38.32 4.17
-2 2 9 41.51 1.97
-2 2 -9 39.75 2.10
-2 -2 9 39.42 2.13
2 -2 -9 36.05 2.36
-2 2 -9 36.59 1.75
2 -2 -9 40.05 2.75
2 2 9 39.81 2.76
-2 2 -9 40.89 2.25
-2 -2 9 39.02 2.60
2 -2 -9 40.73 2.05
-3 -2 -9 22.62 4.21
3 2 -9 17.99 2.72
-3 2 9 22.18 1.51
3 -2 9 25.68 2.17
-3 -2 -9 24.42 3.11
3 2 -9 24.53 3.77
3 2 9 25.06 2.54
-3 2 -9 23.61 1.48
3 -2 -9 20.19 1.77
-3 2 -9 25.52 1.59
-3 -2 9 27.60 2.39
-3 2 -9 21.73 2.13
3 -2 -9 25.75 2.16
3 -2 -9 23.87 2.20
-3 -2 9 25.15 1.93
4 2 -9 101.85 6.83
-4 -2 -9 91.42 8.45
-4 2 9 91.52 4.33
-4 -2 -9 106.93 5.88
4 -2 9 96.72 5.31
4 2 -9 100.85 7.26
-4 2 9 95.61 4.65
4 -2 -9 95.35 4.86
4 -2 -9 92.05 4.99
4 2 9 105.48 5.54
4 -2 -9 101.43 4.95
-4 -2 9 99.58 5.10
-4 2 -9 100.14 4.36
-5 2 9 17.30 1.77
5 -2 9 19.92 3.24
-5 2 9 16.59 1.95
-5 -2 -9 16.41 2.69
5 2 -9 14.82 3.97
-5 -2 -9 17.44 5.19
5 2 -9 19.12 4.48
5 -2 -9 14.27 1.96
5 -2 -9 14.28 2.20
-5 -2 9 15.49 2.19
-5 -2 9 16.93 2.05
5 2 9 16.41 2.70
5 -2 -9 12.51 2.32
-5 2 -9 13.70 1.77
-6 2 9 13.43 1.93
-6 2 9 12.57 1.81
-6 -2 -9 16.11 4.60
-6 -2 -9 11.85 2.76
6 2 -9 7.44 4.97
-6 -2 9 10.12 1.95
6 -2 -9 14.13 2.15
-6 -2 9 14.69 2.39
6 2 9 10.66 3.05
6 -2 -9 10.91 3.09
-6 2 -9 14.84 1.93
6 -2 -9 15.78 3.10
-7 -2 -9 80.75 6.76
-7 2 9 78.20 4.43
-7 2 9 68.54 4.75
7 2 -9 76.69 9.68
-7 -2 -9 78.24 5.58
-7 -2 9 74.80 4.77
7 -2 -9 77.61 6.54
-7 2 -9 71.81 4.52
-7 -2 9 70.81 4.68
7 2 9 76.24 6.42
7 -2 -9 74.99 4.80
8 2 -9 27.56 9.43
-8 2 9 40.10 3.90
-8 -2 -9 45.38 4.98
-8 -2 9 47.35 4.39
-8 -2 9 39.59 4.18
8 -2 -9 41.04 4.26
8 -2 -9 57.19 6.73
-9 -2 -9 0.45 2.94
9 -2 -9 2.67 2.83
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-9 -2 9 -1.48 2.38
-10 -2 -9 0.76 3.32
10 -2 -9 0.78 4.28
-10 -2 9 0.11 2.99
-10 2 -9 0.07 2.88
0 -3 9 320.35 12.87
0 -3 -9 313.80 12.49
0 3 9 314.95 12.63
0 3 9 314.70 14.88
0 -3 -9 313.06 13.59
0 -3 9 320.28 11.78
0 -3 9 310.26 12.33
0 3 -9 302.66 14.22
0 3 -9 314.44 13.06
-1 3 9 22.82 1.84
-1 -3 -9 25.13 3.55
1 3 -9 28.42 3.21
-1 -3 -9 24.98 4.15
-1 3 9 22.03 2.47
1 -3 9 21.03 1.01
1 -3 9 19.38 1.50
1 -3 -9 20.03 1.75
1 -3 -9 18.44 1.28
1 -3 -9 18.71 2.53
-1 -3 9 16.88 1.84
-1 -3 9 19.03 1.90
-1 3 -9 18.99 1.65
-1 -3 9 19.69 3.45
-1 3 -9 20.25 2.17
1 3 9 18.73 2.25
-2 -3 -9 40.32 5.04
2 3 -9 32.40 3.74
-2 3 9 40.02 2.11
2 -3 9 38.36 1.87
2 -3 9 37.10 1.82
-2 -3 9 35.23 2.46
2 -3 -9 37.79 1.99
-2 3 -9 38.14 2.79
-2 -3 9 41.27 2.72
-2 3 -9 36.24 1.77
2 -3 -9 34.10 3.06
2 3 9 34.61 3.12
2 -3 -9 32.36 2.26
3 -3 9 31.22 2.10
-3 -3 -9 26.17 4.39
-3 3 9 24.99 1.78
-3 -3 -9 31.17 5.28
3 3 -9 32.41 4.13
-3 3 -9 31.19 1.81
-3 -3 9 31.08 2.52
3 3 9 32.09 3.52
3 -3 -9 29.08 2.88
-3 3 -9 31.88 1.72
3 -3 -9 30.08 2.02
3 -3 -9 28.64 2.31
-3 -3 9 35.17 2.86
-3 3 -9 33.50 2.68
4 3 -9 77.58 6.63
-4 3 9 85.21 3.82
4 3 -9 80.41 8.23
-4 -3 -9 71.87 9.05
4 -3 9 81.16 4.37
-4 -3 -9 75.47 6.25
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4 -3 -9 83.32 4.59
4 -3 -9 81.10 4.14
-4 -3 9 84.86 4.71
4 -3 -9 80.52 4.32
4 3 9 85.10 5.72
5 3 -9 18.67 6.15
-5 -3 -9 20.90 3.65
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5 -3 9 22.50 2.93
5 3 -9 28.66 5.31
-5 -3 -9 17.92 5.91
5 3 9 22.87 3.58
-5 3 -9 23.77 2.03
5 -3 -9 24.91 2.72
-5 -3 9 26.20 2.80
5 -3 -9 20.67 2.43
5 -3 -9 24.33 2.96
-5 -3 9 23.70 2.87
6 3 -9 45.40 8.61
-6 -3 -9 28.92 3.87
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-6 -3 -9 32.74 6.25
6 3 9 32.47 4.67
6 -3 -9 34.17 3.58
6 -3 -9 23.11 3.39
6 -3 -9 33.60 3.83
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-6 -3 9 32.58 3.65
-6 -3 9 33.31 3.40
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-7 -3 -9 1.05 4.34
-7 -3 -9 6.12 3.16
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7 3 9 10.89 4.16
7 -3 -9 7.49 2.30
-7 -3 9 8.72 2.44
-7 -3 9 6.33 2.33
-7 3 -9 3.88 1.97
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8 -3 -9 22.89 3.35
-8 -3 9 17.85 3.09
-8 -3 9 22.97 3.42
-9 -3 -9 -0.21 3.57
-9 -3 -9 6.50 3.50
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9 -3 -9 4.78 3.29
-10 -3 -9 18.74 4.40
-10 3 -9 21.40 3.64
-10 -3 9 18.20 3.73
0 4 9 206.96 9.06
0 -4 -9 212.36 8.98
0 4 9 215.79 12.05
0 -4 9 209.67 8.15
0 -4 9 204.59 8.74
0 -4 -9 197.94 10.31
0 4 -9 203.52 9.82
0 4 -9 216.28 12.10
1 4 -9 20.55 3.32
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1 -4 9 22.07 1.85
-1 -4 -9 22.50 4.80
1 -4 9 19.82 1.18
-1 -4 -9 22.87 4.06
-1 4 9 18.39 2.95
-1 4 -9 33.03 4.17
-1 4 -9 26.90 2.77
-1 -4 9 26.31 3.85
-1 -4 9 32.37 3.64
1 4 9 30.67 2.99
1 -4 -9 32.31 3.44
-2 -4 -9 39.78 5.68
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-2 -4 -9 31.73 5.94
2 -4 9 34.31 1.90
2 -4 9 36.15 1.80
2 4 -9 40.84 4.90
-2 4 -9 39.52 3.83
2 -4 -9 33.34 1.99
-2 4 -9 33.55 1.90
2 -4 -9 34.14 2.37
2 4 9 30.98 3.39
-2 -4 9 35.75 3.14
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2 -4 -9 31.20 3.46
3 -4 9 75.14 3.43
3 4 -9 60.33 6.41
-3 -4 -9 62.28 7.54
3 -4 9 76.50 2.97
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3 -4 -9 66.82 3.45
3 4 9 69.30 5.40
-3 -4 9 70.19 4.50
-3 -4 9 67.03 4.45
3 -4 -9 73.26 4.59
-3 4 -9 68.81 3.19
3 -4 -9 72.73 3.83
4 4 -9 20.79 4.97
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-4 -4 -9 15.70 5.84
-4 -4 -9 13.56 4.06
4 -4 9 16.90 1.90
-4 4 -9 13.35 1.42
4 4 9 18.59 3.39
4 -4 -9 15.16 1.84
4 -4 -9 15.14 1.85
4 -4 -9 15.16 2.49
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5 4 -9 16.06 5.92
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-5 -4 -9 13.20 6.29
5 -4 9 13.08 2.15
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5 -4 -9 12.43 2.06
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5 -4 -9 17.32 2.71
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5 -4 -9 18.13 2.26
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-6 -4 -9 27.96 4.57
6 -4 -9 32.19 3.39
-6 -4 9 30.89 3.61
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6 -4 -9 31.54 3.82
6 -4 -9 32.17 3.94
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7 -4 -9 18.31 3.24
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7 -4 -9 25.64 3.73
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8 -4 -9 33.85 4.13
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9 -4 -9 5.68 3.74
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-10 -4 -9 6.50 4.27
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0 -5 9 11.20 1.77
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0 -5 -9 10.48 1.94
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0 -5 -9 8.50 2.94
0 -5 9 14.17 1.48
0 5 -9 10.50 3.50
-1 -5 -9 33.03 5.09
1 -5 9 33.61 1.65
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1 5 -9 29.99 4.41
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-1 -5 -9 29.51 4.88
1 -5 9 33.76 2.53
1 -5 -9 24.21 3.89
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1 5 9 30.98 3.42
1 -5 -9 30.22 2.12
-1 5 -9 27.61 3.76
-1 5 -9 29.54 4.15
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2 5 -9 92.17 7.65
-2 -5 -9 97.51 9.14
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2 -5 9 91.28 4.01
-2 -5 -9 87.31 10.13
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2 -5 -9 97.58 4.31
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2 -5 -9 100.55 6.51
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2 5 9 98.04 6.39
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3 -5 9 7.98 1.11
3 -5 9 8.32 1.03
3 5 -9 8.93 4.56
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3 -5 -9 12.73 1.59
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3 -5 -9 13.89 1.75
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3 -5 -9 7.99 2.52
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4 -5 9 4.15 1.27
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4 -5 -9 6.78 1.40
4 -5 -9 4.42 2.41
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5 -5 -9 13.40 2.08
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5 -5 -9 11.72 1.93
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5 -5 -9 13.37 2.98
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6 -5 -9 39.49 4.08
6 -5 -9 33.66 3.99
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-6 -5 9 46.20 4.52
6 -5 -9 34.53 4.20
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7 -5 -9 44.72 4.98
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7 -5 -9 29.33 4.19
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0 -6 9 44.08 3.59
0 -6 9 39.35 2.73
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0 -6 -9 37.40 3.76
0 6 -9 37.92 5.73
0 6 -9 48.28 7.31
0 -6 -9 41.37 5.88
0 6 9 51.55 7.87
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1 6 -9 96.89 8.54
-1 -6 -9 91.77 8.36
-1 -6 -9 94.98 8.95
1 -6 9 93.45 3.81
1 -6 9 93.86 4.93
1 6 9 81.11 6.09
1 -6 -9 77.44 4.25
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1 -6 -9 85.40 7.05
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2 -6 9 55.21 3.37
2 6 -9 59.51 7.31
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2 -6 9 54.32 2.68
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2 -6 -9 53.87 5.97
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2 -6 -9 56.98 3.07
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3 -6 9 296.87 11.42
3 6 -9 254.87 16.40
3 -6 9 291.64 11.51
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3 -6 -9 313.31 11.81
3 6 9 309.14 14.54
-3 -6 9 295.72 13.28
-3 -6 9 266.67 18.62
3 -6 -9 279.36 13.93
3 -6 -9 290.21 11.90
4 -6 9 105.21 5.25
4 6 -9 119.11 11.81
4 -6 9 107.86 4.38
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-4 -6 -9 97.38 11.92
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4 -6 -9 117.56 5.69
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4 -6 -9 110.46 7.66
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4 -6 -9 124.17 5.59
-5 -6 -9 61.91 10.46
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5 -6 -9 68.34 6.35
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5 -6 -9 69.37 4.29
5 -6 -9 61.78 4.18
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6 -6 -9 35.26 4.81
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-6 -6 9 34.15 4.42
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7 -6 -9 37.40 5.38
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0 -7 9 99.96 5.02
0 -7 -9 104.59 9.29
0 -7 -9 95.33 6.02
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0 7 -9 83.49 9.44
0 -7 9 102.23 6.22
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-1 -7 -9 110.67 8.93
1 -7 9 110.28 6.04
1 -7 9 108.19 4.54
1 7 -9 103.21 10.33
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-1 -7 -9 115.07 11.25
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1 7 9 98.47 7.21
-1 -7 9 83.50 7.41
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-1 7 -9 84.49 9.80
1 -7 -9 92.84 5.03
1 -7 -9 98.30 9.44
2 -7 9 63.11 4.23
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2 -7 9 65.39 3.11
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-2 -6 -25 4.66 7.03
-2 -6 -25 1.03 1.36
-2 -6 25 -0.97 2.84
-2 6 -25 -0.45 6.55
2 -6 -25 1.87 8.91
-3 -6 -25 24.23 15.22
-3 -6 -25 2.77 4.75
3 -6 -25 14.66 8.64
-3 -6 25 4.08 3.40
-4 -6 -25 27.16 18.23
4 -6 -25 19.30 9.57
0 -7 -25 -5.76 11.56
0 -7 25 2.50 2.87
-1 -7 -25 13.57 13.21
1 -7 -25 15.48 11.06
-2 -7 -25 21.04 15.11
-2 -7 25 6.30 3.31
2 -7 -25 19.20 9.75
-3 -7 -25 9.30 16.97
-3 -7 -25 12.98 6.99
-3 -7 25 9.85 3.46
3 -7 -25 1.51 10.31
0 -8 -25 22.76 14.14
1 -8 25 27.95 3.87
-1 -8 -25 28.94 15.68
-1 -8 25 26.55 4.36
1 -8 -25 8.09 11.60
-2 -8 -25 -9.08 15.95
-2 -8 25 1.02 2.96
2 -8 -25 -0.96 11.85
-2 8 -25 -0.78 2.97
0 -9 25 5.34 3.33
0 -9 -25 4.43 14.49
1 -9 25 1.04 2.96
-1 -9 -25 8.88 16.61
1 -9 -25 34.84 15.73
-1 -9 25 8.38 3.55
0 0 -26 62.53 7.74
1 0 -26 6.77 5.12
-1 0 -26 8.99 5.61
2 0 -26 -1.09 4.28
-2 0 -26 10.94 6.36
-3 0 -26 9.57 8.10
3 0 -26 7.09 4.53
-4 0 -26 22.95 10.67
4 0 -26 -2.02 4.71
5 0 -26 -0.99 4.89
0 1 -26 2.42 4.47
0 -1 -26 0.81 5.76
1 1 -26 1.69 4.29
-1 -1 -26 2.62 6.41
-1 1 -26 7.19 5.14
1 -1 -26 4.50 5.43
2 1 -26 -5.54 4.06
-2 -1 -26 5.88 7.37
2 -1 -26 13.44 5.72
-2 1 -26 0.94 5.56
-3 -1 -26 8.42 9.17
3 1 -26 13.44 4.62
3 -1 -26 10.69 7.72
-3 1 -26 12.07 8.51
3 -1 -26 13.70 5.75
-4 -1 -26 5.30 11.75
4 1 -26 -7.79 4.39
4 -1 -26 5.82 5.32
-4 1 -26 23.93 10.17
0 -2 -26 19.07 6.79
0 2 -26 9.66 4.43
1 2 -26 7.31 4.12
-1 -2 -26 14.81 7.34
-1 2 -26 20.92 4.90
1 -2 -26 9.25 6.47
-2 -2 -26 15.10 8.62
2 2 -26 7.62 4.30
2 -2 -26 1.88 5.65
2 -2 -26 9.71 3.74
-2 2 -26 11.85 5.05
3 2 -26 7.36 3.87
-3 -2 -26 4.86 9.84
3 -2 -26 7.90 5.98
3 -2 -26 13.41 4.80
-3 2 -26 4.74 6.63
-4 -2 -26 -8.27 12.56
4 2 -26 2.80 4.36
4 -2 -26 6.87 6.09
0 3 -26 2.92 3.99
0 -3 -26 7.86 7.67
-1 -3 -26 -9.21 7.95
1 3 -26 16.27 4.19
1 -3 -26 16.73 2.49
1 -3 -26 28.01 7.90
-1 3 -26 8.27 4.37
2 3 -26 3.18 3.73
-2 -3 -26 11.34 9.61
2 -3 -26 5.98 6.45
-2 3 -26 11.18 4.86
3 3 -26 0.68 3.74
-3 -3 -26 3.15 11.38
-3 3 -26 10.08 5.82
3 -3 -26 10.84 3.66
3 -3 -26 17.90 6.77
-4 -3 -26 36.78 14.40
4 3 -26 7.27 3.84
4 -3 -26 -4.23 6.24
-4 -3 26 2.57 3.54
0 -4 -26 5.56 8.09
0 -4 -26 7.05 1.37
0 4 -26 9.60 4.11
1 4 -26 8.29 3.65
-1 -4 -26 6.05 2.76
-1 -4 -26 8.05 1.08
-1 -4 -26 15.20 9.61
-1 4 -26 9.19 3.94
1 -4 -26 7.41 7.25
-2 -4 -26 18.37 2.01
-2 -4 -26 46.32 11.92
2 4 -26 15.38 3.94
-2 -4 -26 16.96 1.50
2 -4 -26 24.95 2.90
-2 4 -26 9.16 4.64
-2 -4 26 20.85 3.90
2 -4 -26 24.71 8.26
-3 -4 -26 5.51 1.09
3 4 -26 1.73 3.65
-3 -4 -26 7.62 13.95
-3 -4 -26 7.38 1.80
3 -4 -26 15.06 7.23
-3 -4 26 3.38 3.27
-3 4 -26 6.33 5.38
-4 -4 -26 26.41 2.81
-4 -4 -26 29.44 16.85
-4 -4 -26 33.04 3.20
-4 -4 26 22.00 4.35
4 -4 -26 30.57 8.44
0 -5 -26 4.56 9.86
0 5 -26 2.79 3.46
-1 -5 -26 -6.95 10.17
-1 -5 -26 10.48 1.39
1 5 -26 9.32 3.74
1 -5 -26 12.56 2.05
-1 5 -26 13.55 3.86
-1 -5 26 13.75 3.38
1 -5 -26 24.87 9.97
-2 -5 -26 1.97 12.80
-2 -5 -26 9.59 3.91
-2 5 -26 10.15 4.19
2 -5 -26 13.76 7.82
-2 -5 26 1.35 3.07
-3 -5 -26 5.70 13.57
-3 -5 -26 0.01 1.34
-3 -5 -26 0.59 2.82
3 -5 -26 6.27 8.37
-3 -5 26 -1.57 3.15
-4 -5 -26 -9.82 17.51
0 -6 -26 -4.29 10.56
0 -6 -26 0.33 1.38
0 -6 26 1.11 2.84
0 6 -26 -2.37 3.17
-1 -6 -26 4.83 11.37
-1 -6 26 0.45 3.21
-1 6 -26 2.83 3.58
1 -6 -26 9.45 9.76
-2 -6 -26 -4.27 14.13
-2 -6 -26 14.93 6.81
-2 6 -26 13.35 4.14
2 -6 -26 15.20 9.92
-2 -6 26 2.64 3.14
-3 -6 -26 -7.58 15.93
-3 -6 -26 3.78 4.40
-3 -6 26 1.57 3.28
3 -6 -26 -6.01 8.41
0 -7 -26 17.19 12.22
0 -7 26 5.24 3.33
-1 -7 -26 0.35 13.37
-1 7 -26 -2.70 3.42
-1 -7 26 2.63 3.22
1 -7 -26 9.73 11.94
-2 -7 -26 17.04 15.84
2 -7 -26 18.52 10.50
-2 7 -26 11.36 3.86
-2 -7 26 12.04 3.76
0 -8 -26 -12.22 14.11
0 -8 26 2.42 3.27
1 -8 26 1.88 3.14
-1 -8 -26 -38.07 14.92
-1 -8 26 5.16 3.47
-1 8 -26 -2.39 3.39
1 -8 -26 -7.36 12.47
0 0 -27 3.37 5.45
1 0 -27 -0.52 5.04
-1 0 -27 8.07 6.39
2 0 -27 3.18 5.41
-2 0 -27 11.41 7.48
-3 0 -27 2.86 8.55
3 0 -27 -9.78 4.81
4 0 -27 0.78 5.00
0 1 -27 16.16 5.53
0 -1 -27 6.08 6.47
1 1 -27 25.43 5.51
-1 -1 -27 39.64 8.04
1 -1 -27 14.42 6.48
-1 1 -27 15.74 6.19
-2 -1 -27 1.37 8.14
2 1 -27 12.09 5.21
2 -1 -27 1.31 5.87
-2 1 -27 1.43 6.31
-3 -1 -27 2.76 9.95
3 1 -27 14.70 5.32
-3 1 -27 33.06 9.07
3 -1 -27 21.00 6.40
-4 -1 -27 -2.30 13.24
4 1 -27 -6.13 4.27
4 -1 -27 4.09 5.77
0 2 -27 -4.27 4.45
0 -2 -27 14.28 7.76
1 2 -27 2.19 4.35
-1 -2 -27 15.60 8.32
1 -2 -27 10.89 7.19
-1 2 -27 6.85 5.46
-2 -2 -27 -3.09 8.79
2 2 -27 5.12 4.50
2 -2 -27 8.35 6.55
2 -2 -27 -2.23 4.74
-2 2 -27 -2.32 5.84
-3 -2 -27 16.10 10.68
3 2 -27 16.29 4.92
3 -2 -27 0.03 5.71
-3 2 -27 3.75 7.31
3 -2 -27 11.13 5.37
4 2 -27 10.01 4.99
-4 -2 -27 6.24 13.59
4 -2 -27 1.54 5.98
0 -3 -27 -7.48 7.66
0 3 -27 9.59 4.52
1 3 -27 2.84 3.99
-1 -3 -27 -1.64 9.24
1 -3 -27 1.36 2.53
-1 3 -27 5.81 5.02
1 -3 -27 3.51 7.14
-2 -3 -27 2.34 10.18
2 3 -27 6.79 4.21
2 -3 -27 20.98 3.87
2 -3 -27 8.00 7.50
-2 3 -27 12.78 5.84
-3 -3 -27 5.76 12.12
3 3 -27 1.68 4.25
-3 3 -27 2.75 6.50
3 -3 -27 0.95 6.60
0 4 -27 9.77 4.06
0 -4 -27 18.77 10.07
-1 -4 -27 -4.76 9.22
1 4 -27 4.28 4.13
1 -4 -27 -0.16 9.09
1 -4 -27 2.16 1.98
-1 4 -27 1.47 4.23
2 4 -27 -8.48 5.78
-2 -4 -27 -5.65 11.75
2 -4 -27 16.47 8.03
2 -4 -27 4.35 2.48
-2 4 -27 6.97 5.18
3 4 -27 8.89 4.26
-3 -4 -27 13.40 14.00
-3 -4 27 -1.99 3.56
3 -4 -27 1.83 7.97
0 5 -27 10.29 4.29
0 -5 -27 23.63 11.41
0 -5 -27 12.48 1.78
-1 -5 -27 3.18 1.19
1 5 -27 -2.28 3.59
-1 -5 -27 5.47 5.28
-1 -5 -27 16.01 12.12
1 -5 -27 7.21 1.94
1 -5 -27 3.47 10.02
-1 5 -27 -1.41 3.82
-2 -5 -27 6.36 14.26
2 5 -27 1.35 3.90
-2 -5 -27 6.49 2.96
-2 -5 -27 6.35 1.21
-2 -5 27 5.14 3.61
-2 5 -27 10.88 4.98
2 -5 -27 8.15 9.49
0 6 -27 7.23 3.83
0 -6 -27 33.52 13.11
0 -6 -27 13.59 2.45
-1 -6 -27 15.74 13.44
-1 -6 -27 3.55 1.38
1 6 -27 -1.78 3.68
1 -6 -27 28.03 11.02
-1 -6 27 3.90 3.34
-1 6 -27 1.84 4.11
-2 -6 -27 36.31 16.71
-2 -6 -27 13.55 5.45
-2 -6 27 11.41 4.00
2 -6 -27 0.03 10.73
-2 6 -27 22.23 4.85
0 0 -28 6.40 6.56
-1 0 -28 35.20 8.13
1 0 -28 41.68 7.79
-2 0 -28 4.27 7.87
2 0 -28 2.68 5.72
3 0 -28 14.97 5.82
-3 0 -28 24.57 10.56
0 1 -28 4.31 5.83
0 -1 -28 8.12 7.20
1 1 -28 5.12 5.85
-1 -1 -28 -2.53 7.39
1 -1 -28 11.60 7.38
-1 1 -28 4.28 6.01
2 1 -28 1.12 5.11
-2 -1 -28 18.34 9.81
-2 1 -28 11.18 7.43
2 -1 -28 17.41 6.58
-3 -1 -28 28.21 11.69
3 1 -28 0.73 5.29
-3 1 -28 12.19 9.13
3 -1 -28 5.00 5.98
0 2 -28 0.52 5.39
0 -2 -28 2.93 8.31
1 2 -28 -6.28 4.71
-1 -2 -28 -3.09 8.11
-1 2 -28 1.31 5.76
1 -2 -28 -1.18 7.41
2 2 -28 3.01 5.06
-2 -2 -28 12.01 9.27
2 -2 -28 3.45 7.02
-2 2 -28 8.04 6.80
0 -3 -28 11.47 9.39
0 3 -28 -6.88 4.50
1 3 -28 -0.22 4.33
-1 -3 -28 5.27 10.14
1 -3 -28 -2.50 8.60
-1 3 -28 11.90 5.71
2 3 -28 -0.11 4.43
-2 -3 -28 5.66 11.01
2 -3 -28 13.45 4.22
2 -3 -28 10.23 8.35
-2 3 -28 16.35 6.49
0 4 -28 4.83 4.75
0 -4 -28 -9.76 10.03
1 4 -28 2.96 4.60
-1 -4 -28 -25.26 10.30
-1 4 -28 16.36 5.16
1 -4 -28 0.85 2.37
1 -4 -28 14.16 9.43
0 5 -28 17.16 4.69
0 -5 -28 17.52 1.98
0 -5 -28 33.44 12.46
0 0 -29 4.18 6.66
1 0 -29 -4.74 6.39
-1 0 -29 -13.93 7.67
0 1 -29 2.54 6.56
0 -1 -29 9.25 8.49
-1 -1 -29 2.02 9.17
1 1 -29 10.15 6.32
1 -1 -29 21.87 7.96
-1 1 -29 28.63 7.76
0 2 -29 9.64 6.17
0 -2 -29 21.22 9.69
0 0 0 0.00 0.00
;
_shelx_hkl_checksum 60456
_shelx_res_file
;
TITL
XJ.res
created by SHELXL-2016/6 at 19:25:55 on 31-Oct-2018
CELL 0.71073 8.5083 13.8444 22.4960 90.000 90.000 90.000
ZERR 4.00 0.0005 0.0010 0.0012 0.000 0.000 0.000
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 N O Zn Br
UNIT 22 22 5 9 1 3
L.S. 10
ACTA
BOND $H
FMAP 2
PLAN 5
EQIV $8 1/2-x,1-y,1/2+z
HTAB O3W O3_$8
EQIV $4 1-x,1/2+y,1/2-z
HTAB O2W O3_$4
EQIV $6 1+x,y,z
HTAB O2W O3W_$6
HTAB O1W O3W_$6
HTAB N2 O2_$6
EQIV $7 -1/2+x,3/2-y,-z
HTAB N3 O6_$7
EQIV $5 2-x,-1/2+y,1/2-z
HTAB N4 O2W_$5
HTAB O1W O5_$5
EQIV $3 3/2-x,1-y,1/2+z
HTAB C21 N3_$3
HTAB O2W Br3_$3
HTAB O3W O6_$3
HTAB
CONF
FREE O1 O2
FREE Zn1 H1WB
FREE Zn1 H2WB
WGHT 0.032000
FVAR 0.11849
MOLE 2
O4 4 0.400481 0.239748 0.154598 11.00000 0.03222 0.03056 =
0.02610 0.00345 -0.00015 -0.00452
MOLE 1
BR1 6 0.994780 0.576280 0.151892 11.00000 0.02293 0.04831 =
0.05686 -0.01140 0.00551 -0.01151
BR2 6 0.359511 0.482572 0.192775 11.00000 0.01891 0.03811 =
0.05277 -0.01796 0.00532 -0.00184
BR3 6 0.738989 0.224885 0.062556 11.00000 0.05534 0.03746 =
0.03714 -0.01684 0.00450 0.00659
C1 1 0.673000 0.592559 0.215978 11.00000 0.00662 0.02948 =
0.03564 -0.00467 -0.00082 -0.00601
C2 1 0.685461 0.510102 0.171401 11.00000 0.02356 0.01329 =
0.01775 0.00036 -0.00508 0.00134
C3 1 0.560189 0.448656 0.161965 11.00000 0.02272 0.02251 =
0.01906 -0.00394 0.00147 0.00542
C4 1 0.571108 0.365413 0.128675 11.00000 0.02471 0.01629 =
0.01593 0.00164 -0.00498 -0.00105
C5 1 0.719003 0.343561 0.104785 11.00000 0.03387 0.02545 =
0.01789 -0.00430 0.00227 0.00707
C6 1 0.848833 0.402951 0.110849 11.00000 0.02268 0.03445 =
0.01744 -0.00268 0.01000 0.00451
C7 1 0.825764 0.487285 0.144047 11.00000 0.02026 0.02628 =
0.02342 -0.00059 -0.00134 0.00108
MOLE 2
C8 1 0.430701 0.302775 0.116781 11.00000 0.02888 0.02513 =
0.02103 -0.00581 0.00566 -0.00640
MOLE 1
C9 1 0.930900 0.773874 0.273011 11.00000 0.02922 0.02852 =
0.03550 0.00511 0.00392 0.00894
AFIX 43
H9 2 0.831663 0.802030 0.272725 11.00000 -1.20000
AFIX 0
C10 1 1.049984 0.817106 0.240013 11.00000 0.03501 0.02988 =
0.03085 0.01492 0.00231 0.00374
AFIX 43
H10 2 1.030355 0.872952 0.218270 11.00000 -1.20000
AFIX 0
C11 1 1.196944 0.776082 0.240028 11.00000 0.02764 0.02413 =
0.01255 -0.00794 -0.00017 0.00098
C12 1 1.219456 0.695451 0.273582 11.00000 0.02327 0.03141 =
0.03150 0.00413 -0.00452 0.00469
AFIX 43
H12 2 1.318121 0.666639 0.275046 11.00000 -1.20000
AFIX 0
C13 1 1.096527 0.656376 0.305390 11.00000 0.02775 0.02925 =
0.03348 0.00757 -0.00422 0.00235
AFIX 43
H13 2 1.114525 0.601386 0.328136 11.00000 -1.20000
AFIX 0
C14 1 1.331439 0.819478 0.204084 11.00000 0.02437 0.03412 =
0.02232 -0.00271 0.00127 -0.00195
AFIX 23
H14A 2 1.304531 0.885056 0.192818 11.00000 -1.20000
H14B 2 1.425171 0.822048 0.228578 11.00000 -1.20000
AFIX 0
C15 1 1.279494 0.771957 0.101589 11.00000 0.02151 0.02233 =
0.02826 -0.00122 0.00680 -0.00281
C16 1 1.333769 0.712183 0.048674 11.00000 0.03099 0.02415 =
0.02775 -0.00204 0.00093 -0.00296
C17 1 1.269321 0.679445 -0.055807 11.00000 0.03502 0.04433 =
0.02645 -0.01176 -0.00269 -0.00755
AFIX 23
H17A 2 1.373986 0.651669 -0.055767 11.00000 -1.20000
H17B 2 1.266971 0.729025 -0.086261 11.00000 -1.20000
AFIX 0
C18 1 1.153635 0.601537 -0.072583 11.00000 0.02458 0.02054 =
0.02965 -0.00408 -0.00509 0.00833
C19 1 1.156226 0.563277 -0.128767 11.00000 0.02321 0.04568 =
0.02401 -0.01089 -0.00010 -0.00589
AFIX 43
H19 2 1.233512 0.582581 -0.155478 11.00000 -1.20000
AFIX 0
C20 1 0.568619 0.498896 0.444781 11.00000 0.04792 0.05329 =
0.01880 -0.01054 0.00037 -0.01619
AFIX 43
H20 2 0.645206 0.520586 0.471084 11.00000 -1.20000
AFIX 0
C21 1 0.461882 0.432514 0.465355 11.00000 0.04089 0.03478 =
0.02395 -0.00157 0.00356 -0.01033
AFIX 43
H21 2 0.467101 0.410624 0.504389 11.00000 -1.20000
AFIX 0
C22 1 0.454535 0.503410 0.354057 11.00000 0.02656 0.04583 =
0.03107 0.01278 0.00253 0.00512
AFIX 43
H22 2 0.448721 0.528192 0.315696 11.00000 -1.20000
AFIX 0
N1 3 0.952348 0.694679 0.304720 11.00000 0.02856 0.01937 =
0.02300 0.00105 0.00032 -0.00070
N2 3 1.364401 0.762782 0.150344 11.00000 0.02239 0.02461 =
0.02055 0.00325 0.00163 0.00148
AFIX 43
H2 2 1.441254 0.722437 0.150657 11.00000 -1.20000
AFIX 0
N3 3 1.242636 0.724668 0.001036 11.00000 0.02154 0.04339 =
0.03418 -0.01317 -0.00445 0.00165
AFIX 43
H3 2 1.162610 0.762205 0.004460 11.00000 -1.20000
AFIX 0
N4 3 0.990193 0.381887 0.083682 11.00000 0.03052 0.04329 =
0.04234 -0.00813 0.01407 0.00246
AFIX 93
H4A 2 0.999273 0.330692 0.062304 11.00000 -1.20000
H4B 2 1.069191 0.419958 0.088133 11.00000 -1.20000
AFIX 0
N5 3 0.570146 0.534627 0.389428 11.00000 0.02979 0.02191 =
0.02912 0.00104 0.00521 0.00124
O1 4 0.704925 0.562857 0.268691 11.00000 0.03845 0.02351 =
0.02207 -0.00497 0.00372 -0.00788
MOLE 2
O2 4 0.636855 0.673254 0.200106 11.00000 0.04897 0.02312 =
0.04852 -0.00467 -0.01300 0.01225
O3 4 0.353810 0.323070 0.071338 11.00000 0.05210 0.04163 =
0.03083 0.01104 -0.01971 -0.02674
MOLE 1
O5 4 1.162734 0.823557 0.097198 11.00000 0.03350 0.04435 =
0.03347 -0.01471 -0.00581 0.01230
O6 4 1.452472 0.660391 0.050908 11.00000 0.04201 0.04735 =
0.02796 -0.00881 -0.00207 0.01659
MOLE 2
O1W 4 0.922527 0.507042 0.376680 11.00000 0.04480 0.03219 =
0.04396 0.01483 -0.00930 -0.00436
AFIX 3
H1WA 2 0.881540 0.442380 0.378767 11.00000 -1.50000
H1WB 2 1.012260 0.516110 0.404962 11.00000 -1.50000
AFIX 0
O3W 4 0.022322 0.534387 0.497199 11.00000 0.07879 0.03543 =
0.03539 0.00050 -0.01744 -0.00092
AFIX 3
H3WA 2 -0.002527 0.481500 0.513991 11.00000 -1.50000
H3WB 2 0.054357 0.574599 0.522777 11.00000 -1.50000
AFIX 0
MOLE 1
ZN1 5 0.755878 0.625280 0.347712 11.00000 0.02971 0.02169 =
0.02270 -0.00183 0.00445 -0.00149
O2W 4 0.839647 0.676898 0.431560 11.00000 0.05111 0.04856 =
0.04248 0.00036 -0.00666 0.01035
AFIX 3
H2WA 2 0.782861 0.713443 0.453277 11.00000 -1.50000
H2WB 2 0.863352 0.626235 0.451095 11.00000 -1.50000
AFIX 0
HKLF 4
REM
REM R1 = 0.0457 for 4032 Fo > 4sig(Fo) and 0.1097 for all 6064 data
REM 361 parameters refined using 0 restraints
END
WGHT 0.0314 0.0000
REM Instructions for potential hydrogen bonds
HTAB C9 Br2_$4
HTAB C13 O1W
EQIV $9 -x+2, y+1/2, -z+1/2
HTAB C14 O1_$9
EQIV $10 x+1/2, -y+3/2, -z
HTAB C17 O5_$10
HTAB C22 Br2
HTAB C22 O1
HTAB N2 O2_$6
HTAB N3 O6_$7
HTAB N4 Br3
HTAB N4 O2W_$5
HTAB N4 Br1
HTAB O1W O5_$5
HTAB O1W O3W_$6
HTAB O3W O6_$3
HTAB O3W O3_$8
HTAB O2W Br3_$3
HTAB O2W O3_$4
HTAB O2W O3W_$6
REM Highest difference peak 1.696, deepest hole -1.133, 1-sigma level 0.116
Q1 1 0.7295 0.2702 0.0316 11.00000 0.05 1.70
Q2 1 0.7520 0.1233 0.0546 11.00000 0.05 0.49
Q3 1 0.1546 0.4445 0.4839 11.00000 0.05 0.47
Q4 1 0.7347 0.4333 0.0494 11.00000 0.05 0.44
Q5 1 0.6176 0.4112 0.1983 11.00000 0.05 0.42
;
_shelx_res_checksum 1617
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'
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
O O4 0.4005(5) 0.2397(4) 0.1546(2) 0.0296(12) Uani d 1
Br Br1 0.99478(8) 0.57628(7) 0.15189(4) 0.0427(2) Uani d 1
Br Br2 0.35951(8) 0.48257(6) 0.19278(3) 0.0366(2) Uani d 1
Br Br3 0.73899(10) 0.22488(7) 0.06256(3) 0.0433(2) Uani d 1
C C1 0.6730(7) 0.5926(6) 0.2160(3) 0.0239(18) Uani d 1
C C2 0.6855(7) 0.5101(5) 0.1714(3) 0.0182(16) Uani d 1
C C3 0.5602(7) 0.4487(6) 0.1620(3) 0.0214(18) Uani d 1
C C4 0.5711(7) 0.3654(6) 0.1287(3) 0.0190(16) Uani d 1
C C5 0.7190(8) 0.3436(6) 0.1048(3) 0.0257(18) Uani d 1
C C6 0.8488(7) 0.4030(6) 0.1108(3) 0.0249(18) Uani d 1
C C7 0.8258(7) 0.4873(6) 0.1440(3) 0.0233(17) Uani d 1
C C8 0.4307(8) 0.3028(6) 0.1168(3) 0.0250(19) Uani d 1
C C9 0.9309(8) 0.7739(6) 0.2730(3) 0.031(2) Uani d 1
H H9 0.831663 0.802030 0.272725 0.037 Uiso calc 1
C C10 1.0500(8) 0.8171(6) 0.2400(3) 0.032(2) Uani d 1
H H10 1.030355 0.872952 0.218270 0.038 Uiso calc 1
C C11 1.1969(7) 0.7761(6) 0.2400(3) 0.0214(17) Uani d 1
C C12 1.2195(8) 0.6955(6) 0.2736(3) 0.0287(19) Uani d 1
H H12 1.318121 0.666639 0.275046 0.034 Uiso calc 1
C C13 1.0965(7) 0.6564(6) 0.3054(3) 0.0302(19) Uani d 1
H H13 1.114525 0.601386 0.328136 0.036 Uiso calc 1
C C14 1.3314(7) 0.8195(6) 0.2041(3) 0.0269(18) Uani d 1
H H14A 1.304531 0.885056 0.192818 0.032 Uiso calc 1
H H14B 1.425171 0.822048 0.228578 0.032 Uiso calc 1
C C15 1.2795(7) 0.7720(6) 0.1016(3) 0.0240(17) Uani d 1
C C16 1.3338(8) 0.7122(6) 0.0487(3) 0.0276(19) Uani d 1
C C17 1.2693(9) 0.6794(6) -0.0558(3) 0.035(2) Uani d 1
H H17A 1.373986 0.651669 -0.055767 0.042 Uiso calc 1
H H17B 1.266971 0.729025 -0.086261 0.042 Uiso calc 1
C C18 1.1536(7) 0.6015(5) -0.0726(3) 0.0249(18) Uani d 1
C C19 1.1562(8) 0.5633(6) -0.1288(3) 0.031(2) Uani d 1
H H19 1.233512 0.582581 -0.155478 0.037 Uiso calc 1
C C20 0.5686(9) 0.4989(7) 0.4448(3) 0.040(2) Uani d 1
H H20 0.645206 0.520586 0.471084 0.048 Uiso calc 1
C C21 0.4619(8) 0.4325(7) 0.4654(3) 0.033(2) Uani d 1
H H21 0.467101 0.410624 0.504389 0.040 Uiso calc 1
C C22 0.4545(7) 0.5034(6) 0.3541(3) 0.034(2) Uani d 1
H H22 0.448721 0.528192 0.315696 0.041 Uiso calc 1
N N1 0.9523(6) 0.6947(5) 0.3047(2) 0.0236(15) Uani d 1
N N2 1.3644(6) 0.7628(4) 0.1503(2) 0.0225(13) Uani d 1
H H2 1.441254 0.722437 0.150657 0.027 Uiso calc 1
N N3 1.2426(7) 0.7247(5) 0.0010(2) 0.0330(16) Uani d 1
H H3 1.162610 0.762205 0.004460 0.040 Uiso calc 1
N N4 0.9902(7) 0.3819(5) 0.0837(2) 0.0387(17) Uani d 1
H H4A 0.999273 0.330692 0.062304 0.046 Uiso calc 1
H H4B 1.069191 0.419958 0.088133 0.046 Uiso calc 1
N N5 0.5701(6) 0.5346(5) 0.3894(2) 0.0269(16) Uani d 1
O O1 0.7049(5) 0.5629(4) 0.26869(18) 0.0280(12) Uani d 1
O O2 0.6369(6) 0.6733(4) 0.2001(2) 0.0402(14) Uani d 1
O O3 0.3538(6) 0.3231(4) 0.0713(2) 0.0415(15) Uani d 1
O O5 1.1627(6) 0.8236(4) 0.0972(2) 0.0371(14) Uani d 1
O O6 1.4525(6) 0.6604(4) 0.0509(2) 0.0391(15) Uani d 1
O O1W 0.9225(6) 0.5070(4) 0.3767(2) 0.0403(15) Uani d 1
H H1WA 0.881540 0.442380 0.378767 0.060 Uiso d 1
H H1WB 1.012260 0.516110 0.404962 0.060 Uiso d 1
O O3W 0.0223(7) 0.5344(4) 0.4972(2) 0.0499(16) Uani d 1
H H3WA -0.002527 0.481500 0.513991 0.075 Uiso d 1
H H3WB 0.054357 0.574599 0.522777 0.075 Uiso d 1
Zn Zn1 0.75588(9) 0.62528(6) 0.34771(3) 0.0247(2) Uani d 1
O O2W 0.8396(6) 0.6769(4) 0.4316(2) 0.0474(15) Uani d 1
H H2WA 0.782861 0.713443 0.453277 0.071 Uiso d 1
H H2WB 0.863352 0.626235 0.451095 0.071 Uiso 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
O4 0.032(3) 0.031(4) 0.026(2) -0.005(3) 0.000(2) 0.003(3)
Br1 0.0229(3) 0.0483(6) 0.0569(5) -0.0115(4) 0.0055(4) -0.0114(5)
Br2 0.0189(3) 0.0381(6) 0.0528(4) -0.0018(4) 0.0053(3) -0.0180(4)
Br3 0.0553(5) 0.0375(6) 0.0371(4) 0.0066(5) 0.0045(4) -0.0168(4)
C1 0.007(3) 0.029(6) 0.036(4) -0.006(3) -0.001(3) -0.005(4)
C2 0.024(3) 0.013(5) 0.018(3) 0.001(3) -0.005(2) 0.000(3)
C3 0.023(3) 0.023(5) 0.019(3) 0.005(3) 0.001(3) -0.004(3)
C4 0.025(3) 0.016(5) 0.016(3) -0.001(3) -0.005(3) 0.002(3)
C5 0.034(4) 0.025(5) 0.018(3) 0.007(4) 0.002(3) -0.004(3)
C6 0.023(3) 0.034(6) 0.017(3) 0.005(4) 0.010(3) -0.003(4)
C7 0.020(3) 0.026(5) 0.023(3) 0.001(3) -0.001(3) -0.001(4)
C8 0.029(4) 0.025(6) 0.021(4) -0.006(4) 0.006(3) -0.006(4)
C9 0.029(4) 0.029(6) 0.035(4) 0.009(4) 0.004(3) 0.005(4)
C10 0.035(4) 0.030(6) 0.031(4) 0.004(4) 0.002(3) 0.015(4)
C11 0.028(4) 0.024(5) 0.013(3) 0.001(3) 0.000(3) -0.008(3)
C12 0.023(4) 0.031(6) 0.032(4) 0.005(4) -0.005(3) 0.004(4)
C13 0.028(4) 0.029(6) 0.033(4) 0.002(4) -0.004(3) 0.008(4)
C14 0.024(4) 0.034(5) 0.022(4) -0.002(4) 0.001(3) -0.003(4)
C15 0.022(4) 0.022(5) 0.028(4) -0.003(4) 0.007(3) -0.001(4)
C16 0.031(4) 0.024(5) 0.028(4) -0.003(4) 0.001(3) -0.002(4)
C17 0.035(4) 0.044(6) 0.026(4) -0.008(4) -0.003(3) -0.012(4)
C18 0.025(3) 0.021(5) 0.030(4) 0.008(3) -0.005(3) -0.004(3)
C19 0.023(3) 0.046(6) 0.024(4) -0.006(4) 0.000(3) -0.011(4)
C20 0.048(4) 0.053(7) 0.019(4) -0.016(5) 0.000(3) -0.011(4)
C21 0.041(4) 0.035(6) 0.024(4) -0.010(4) 0.004(3) -0.002(4)
C22 0.027(3) 0.046(7) 0.031(4) 0.005(4) 0.003(3) 0.013(4)
N1 0.029(3) 0.019(4) 0.023(3) -0.001(3) 0.000(2) 0.001(3)
N2 0.022(3) 0.025(4) 0.021(3) 0.001(3) 0.002(3) 0.003(3)
N3 0.022(3) 0.043(5) 0.034(3) 0.002(4) -0.004(3) -0.013(3)
N4 0.031(3) 0.043(5) 0.042(3) 0.002(4) 0.014(3) -0.008(3)
N5 0.030(3) 0.022(5) 0.029(3) 0.001(3) 0.005(3) 0.001(3)
O1 0.038(3) 0.024(3) 0.022(2) -0.008(2) 0.004(2) -0.005(2)
O2 0.049(3) 0.023(4) 0.049(3) 0.012(3) -0.013(3) -0.005(3)
O3 0.052(3) 0.042(4) 0.031(3) -0.027(3) -0.020(3) 0.011(3)
O5 0.034(3) 0.044(4) 0.033(3) 0.012(3) -0.006(2) -0.015(3)
O6 0.042(3) 0.047(4) 0.028(3) 0.017(3) -0.002(2) -0.009(3)
O1W 0.045(3) 0.032(4) 0.044(3) -0.004(3) -0.009(2) 0.015(3)
O3W 0.079(4) 0.035(4) 0.035(3) -0.001(3) -0.017(3) 0.001(3)
Zn1 0.0297(4) 0.0217(5) 0.0227(4) -0.0015(4) 0.0045(4) -0.0018(4)
O2W 0.051(3) 0.049(4) 0.042(3) 0.010(3) -0.007(3) 0.000(3)
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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.2839 1.4301 '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'
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
C8 O4 Zn1 . 3_645 130.7(4)
O2 C1 O1 . . 128.4(7)
O2 C1 C2 . . 121.0(6)
O1 C1 C2 . . 110.7(7)
C7 C2 C3 . . 117.3(6)
C7 C2 C1 . . 121.7(6)
C3 C2 C1 . . 120.6(5)
C4 C3 C2 . . 123.2(6)
C4 C3 Br2 . . 117.7(5)
C2 C3 Br2 . . 119.0(5)
C3 C4 C5 . . 116.7(6)
C3 C4 C8 . . 121.8(6)
C5 C4 C8 . . 121.5(7)
C6 C5 C4 . . 123.4(7)
C6 C5 Br3 . . 119.4(5)
C4 C5 Br3 . . 117.2(5)
N4 C6 C5 . . 121.8(7)
N4 C6 C7 . . 122.3(7)
C5 C6 C7 . . 115.9(5)
C2 C7 C6 . . 123.4(6)
C2 C7 Br1 . . 117.7(5)
C6 C7 Br1 . . 118.9(4)
O4 C8 O3 . . 127.6(7)
O4 C8 C4 . . 116.6(6)
O3 C8 C4 . . 115.7(7)
N1 C9 C10 . . 123.0(7)
N1 C9 H9 . . 118.5
C10 C9 H9 . . 118.5
C11 C10 C9 . . 119.0(7)
C11 C10 H10 . . 120.5
C9 C10 H10 . . 120.5
C12 C11 C10 . . 117.9(6)
C12 C11 C14 . . 120.8(6)
C10 C11 C14 . . 121.4(7)
C11 C12 C13 . . 120.2(7)
C11 C12 H12 . . 119.9
C13 C12 H12 . . 119.9
N1 C13 C12 . . 122.4(7)
N1 C13 H13 . . 118.8
C12 C13 H13 . . 118.8
N2 C14 C11 . . 111.7(6)
N2 C14 H14A . . 109.3
C11 C14 H14A . . 109.3
N2 C14 H14B . . 109.3
C11 C14 H14B . . 109.3
H14A C14 H14B . . 107.9
O5 C15 N2 . . 124.5(6)
O5 C15 C16 . . 119.9(6)
N2 C15 C16 . . 115.6(6)
O6 C16 N3 . . 125.5(6)
O6 C16 C15 . . 122.0(6)
N3 C16 C15 . . 112.4(6)
N3 C17 C18 . . 115.4(6)
N3 C17 H17A . . 108.4
C18 C17 H17A . . 108.4
N3 C17 H17B . . 108.4
C18 C17 H17B . . 108.4
H17A C17 H17B . . 107.5
C19 C18 C21 . 2_664 116.6(7)
C19 C18 C17 . . 119.8(6)
C21 C18 C17 2_664 . 123.5(6)
C18 C19 C22 . 2_664 120.5(7)
C18 C19 H19 . . 119.7
C22 C19 H19 2_664 . 119.7
N5 C20 C21 . . 124.5(7)
N5 C20 H20 . . 117.7
C21 C20 H20 . . 117.7
C20 C21 C18 . 2_665 119.3(7)
C20 C21 H21 . . 120.3
C18 C21 H21 2_665 . 120.3
N5 C22 C19 . 2_665 123.7(6)
N5 C22 H22 . . 118.2
C19 C22 H22 2_665 . 118.2
C9 N1 C13 . . 117.5(6)
C9 N1 Zn1 . . 120.3(4)
C13 N1 Zn1 . . 122.0(5)
C15 N2 C14 . . 121.9(6)
C15 N2 H2 . . 119.1
C14 N2 H2 . . 119.1
C16 N3 C17 . . 124.4(6)
C16 N3 H3 . . 117.8
C17 N3 H3 . . 117.8
C6 N4 H4A . . 120.0
C6 N4 H4B . . 120.0
H4A N4 H4B . . 120.0
C22 N5 C20 . . 115.3(6)
C22 N5 Zn1 . . 117.0(5)
C20 N5 Zn1 . . 127.4(5)
C1 O1 Zn1 . . 136.0(5)
Zn1 O1W H1WA . . 117.4
Zn1 O1W H1WB . . 124.8
H1WA O1W H1WB . . 111.2
H3WA O3W H3WB . . 110.2
O1 Zn1 O4 . 3_655 99.63(19)
O1 Zn1 O2W . . 171.3(2)
O4 Zn1 O2W 3_655 . 88.9(2)
O1 Zn1 N1 . . 87.84(19)
O4 Zn1 N1 3_655 . 98.4(2)
O2W Zn1 N1 . . 89.3(2)
O1 Zn1 N5 . . 88.7(2)
O4 Zn1 N5 3_655 . 89.2(2)
O2W Zn1 N5 . . 93.0(2)
N1 Zn1 N5 . . 172.1(2)
O1 Zn1 O1W . . 94.5(2)
O4 Zn1 O1W 3_655 . 164.67(18)
O2W Zn1 O1W . . 77.2(2)
N1 Zn1 O1W . . 88.0(2)
N5 Zn1 O1W . . 85.2(2)
Zn1 O2W H2WA . . 120.9
Zn1 O2W H2WB . . 105.0
H2WA O2W H2WB . . 109.1
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
O4 C8 . 1.245(8)
O4 Zn1 3_645 2.070(5)
Br1 C7 . 1.902(7)
Br2 C3 . 1.902(6)
Br3 C5 . 1.905(7)
C1 O2 . 1.213(9)
C1 O1 . 1.284(8)
C1 C2 . 1.523(10)
C2 C7 . 1.380(8)
C2 C3 . 1.380(9)
C3 C4 . 1.378(10)
C4 C5 . 1.401(9)
C4 C8 . 1.500(9)
C5 C6 . 1.384(10)
C6 N4 . 1.380(8)
C6 C7 . 1.400(10)
C8 O3 . 1.246(8)
C9 N1 . 1.321(9)
C9 C10 . 1.391(9)
C9 H9 . 0.9300
C10 C11 . 1.373(9)
C10 H10 . 0.9300
C11 C12 . 1.361(10)
C11 C14 . 1.525(9)
C12 C13 . 1.378(9)
C12 H12 . 0.9300
C13 N1 . 1.337(8)
C13 H13 . 0.9300
C14 N2 . 1.468(8)
C14 H14A . 0.9700
C14 H14B . 0.9700
C15 O5 . 1.228(8)
C15 N2 . 1.319(8)
C15 C16 . 1.522(10)
C16 O6 . 1.240(8)
C16 N3 . 1.334(8)
C17 N3 . 1.442(8)
C17 C18 . 1.508(10)
C17 H17A . 0.9700
C17 H17B . 0.9700
C18 C19 . 1.371(9)
C18 C21 2_664 1.384(9)
C19 C22 2_664 1.375(10)
C19 H19 . 0.9300
C20 N5 . 1.340(9)
C20 C21 . 1.372(11)
C20 H20 . 0.9300
C21 H21 . 0.9300
C22 N5 . 1.337(8)
C22 H22 . 0.9300
N1 Zn1 . 2.157(5)
N2 H2 . 0.8600
N3 H3 . 0.8600
N4 H4A . 0.8600
N4 H4B . 0.8600
N5 Zn1 . 2.226(6)
O1 Zn1 . 2.024(4)
O1W Zn1 . 2.262(5)
O1W H1WA . 0.9619
O1W H1WB . 1.0017
O3W H3WA . 0.8506
O3W H3WB . 0.8458
Zn1 O2W . 2.139(5)
O2W H2WA . 0.8533
O2W H2WB . 0.8519
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
O3W H3WB O3 2_565 0.85 1.95 2.790(7) 170.9
O2W H2WA O3 3_655 0.85 1.99 2.609(8) 128.6
O2W H2WB O3W 1_655 0.85 2.13 2.914(7) 153.4
O1W H1WB O3W 1_655 1.00 2.09 2.866(6) 132.6
N2 H2 O2 1_655 0.86 2.11 2.857(8) 144.3
N3 H3 O6 4_465 0.86 2.43 3.161(8) 143.5
N4 H4A O2W 3_745 0.86 2.54 3.204(9) 135.2
O1W H1WA O5 3_745 0.96 1.77 2.706(8) 162.9
C21 H21 N3 2_665 0.93 2.59 2.900(10) 100.1
O2W H2WA Br3 2_665 0.85 2.61 3.314(5) 140.7
O3W H3WA O6 2_665 0.85 2.17 2.963(8) 154.0
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_4
_geom_torsion
O2 C1 C2 C7 . . 92.3(8)
O1 C1 C2 C7 . . -87.8(7)
O2 C1 C2 C3 . . -95.0(8)
O1 C1 C2 C3 . . 84.9(7)
C7 C2 C3 C4 . . 2.3(10)
C1 C2 C3 C4 . . -170.7(6)
C7 C2 C3 Br2 . . -174.5(5)
C1 C2 C3 Br2 . . 12.5(9)
C2 C3 C4 C5 . . 1.1(10)
Br2 C3 C4 C5 . . 177.9(5)
C2 C3 C4 C8 . . -176.9(7)
Br2 C3 C4 C8 . . -0.1(9)
C3 C4 C5 C6 . . -3.0(10)
C8 C4 C5 C6 . . 175.0(6)
C3 C4 C5 Br3 . . 176.4(5)
C8 C4 C5 Br3 . . -5.5(9)
C4 C5 C6 N4 . . -176.0(6)
Br3 C5 C6 N4 . . 4.5(9)
C4 C5 C6 C7 . . 1.4(10)
Br3 C5 C6 C7 . . -178.1(5)
C3 C2 C7 C6 . . -4.1(10)
C1 C2 C7 C6 . . 168.8(7)
C3 C2 C7 Br1 . . 175.5(5)
C1 C2 C7 Br1 . . -11.6(9)
N4 C6 C7 C2 . . 179.7(6)
C5 C6 C7 C2 . . 2.3(10)
N4 C6 C7 Br1 . . 0.2(9)
C5 C6 C7 Br1 . . -177.2(5)
Zn1 O4 C8 O3 3_645 . 13.9(11)
Zn1 O4 C8 C4 3_645 . -169.7(4)
C3 C4 C8 O4 . . -87.4(9)
C5 C4 C8 O4 . . 94.7(8)
C3 C4 C8 O3 . . 89.5(8)
C5 C4 C8 O3 . . -88.4(9)
N1 C9 C10 C11 . . 0.1(12)
C9 C10 C11 C12 . . -1.2(11)
C9 C10 C11 C14 . . 179.2(6)
C10 C11 C12 C13 . . 1.1(10)
C14 C11 C12 C13 . . -179.3(6)
C11 C12 C13 N1 . . 0.2(11)
C12 C11 C14 N2 . . 75.7(7)
C10 C11 C14 N2 . . -104.8(8)
O5 C15 C16 O6 . . 178.8(7)
N2 C15 C16 O6 . . -1.9(10)
O5 C15 C16 N3 . . 0.5(10)
N2 C15 C16 N3 . . 179.8(6)
N3 C17 C18 C19 . . 171.4(7)
N3 C17 C18 C21 . 2_664 -6.2(11)
C21 C18 C19 C22 2_664 2_664 1.8(11)
C17 C18 C19 C22 . 2_664 -175.9(7)
N5 C20 C21 C18 . 2_665 0.1(13)
C10 C9 N1 C13 . . 1.2(11)
C10 C9 N1 Zn1 . . -174.2(6)
C12 C13 N1 C9 . . -1.3(10)
C12 C13 N1 Zn1 . . 173.9(5)
O5 C15 N2 C14 . . -3.8(11)
C16 C15 N2 C14 . . 176.9(6)
C11 C14 N2 C15 . . 80.7(8)
O6 C16 N3 C17 . . -0.2(12)
C15 C16 N3 C17 . . 178.0(7)
C18 C17 N3 C16 . . 109.2(8)
C19 C22 N5 C20 2_665 . -2.4(11)
C19 C22 N5 Zn1 2_665 . 171.0(6)
C21 C20 N5 C22 . . 2.1(12)
C21 C20 N5 Zn1 . . -170.4(6)
O2 C1 O1 Zn1 . . -14.4(10)
C2 C1 O1 Zn1 . . 165.7(4)
_cod_database_fobs_code 2021659