#------------------------------------------------------------------------------
#$Date: 2021-06-06 19:14:57 +0300 (Sun, 06 Jun 2021) $
#$Revision: 266201 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/02/23/2022357.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_2022357
loop_
_publ_author_name
'Wang, Li-Fei'
'Liu, Xing-Gui'
'Meng, Mei-Mei'
'Xu, Yong-Kai'
'Zhu, Rui'
'Zhang, Rui'
'Lu, Zhen-Zhong'
'Huang, Wei'
_publ_section_title
;
Three coordination polymers built by quaternary-ammonium-modified
isophthalic acid
;
_journal_coeditor_code OV3146
_journal_issue 5
_journal_name_full 'Acta Crystallographica Section C'
_journal_page_first 221
_journal_page_last 226
_journal_paper_doi 10.1107/S2053229621003296
_journal_volume 77
_journal_year 2021
_chemical_formula_iupac '[Zn Br (C19 H28 N O5)]'
_chemical_formula_moiety 'C19 H28 Br N O5 Zn'
_chemical_formula_sum 'C19 H28 Br N O5 Zn'
_chemical_formula_weight 495.70
_chemical_name_systematic
Poly[bromido{\m~3~-5-[2-(tripropylazaniumyl)ethoxy]benzene-1,3-dicarboxylato}zinc(II)]
_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 geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha 90
_cell_angle_beta 99.813(2)
_cell_angle_gamma 90
_cell_formula_units_Z 4
_cell_length_a 11.5479(7)
_cell_length_b 14.7949(10)
_cell_length_c 12.3782(9)
_cell_measurement_reflns_used 9963
_cell_measurement_temperature 290
_cell_measurement_theta_max 34.176
_cell_measurement_theta_min 2.164
_cell_volume 2083.9(2)
_computing_cell_refinement
;
SAINT (Bruker, 2015)
;
_computing_data_collection
;
APEX2 (Bruker, 2015)
;
_computing_data_reduction
;
SAINT (Bruker, 2015)
;
_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
;
SHELXS2018 (Sheldrick, 2015a)
;
_diffrn_ambient_temperature 290
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type 'Bruker D8'
_diffrn_measurement_method 'phi and omega scans'
_diffrn_radiation_monochromator graphite
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0239
_diffrn_reflns_av_unetI/netI 0.0219
_diffrn_reflns_limit_h_max 12
_diffrn_reflns_limit_h_min -14
_diffrn_reflns_limit_k_max 15
_diffrn_reflns_limit_k_min -18
_diffrn_reflns_limit_l_max 15
_diffrn_reflns_limit_l_min -15
_diffrn_reflns_number 14849
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 25.746
_diffrn_reflns_theta_min 2.621
_exptl_absorpt_coefficient_mu 3.125
_exptl_absorpt_correction_T_max 0.7472
_exptl_absorpt_correction_T_min 0.4181
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2015)
;
_exptl_crystal_colour colorless
_exptl_crystal_density_diffrn 1.580
_exptl_crystal_description prism
_exptl_crystal_F_000 1016
_exptl_crystal_size_max 0.35
_exptl_crystal_size_mid 0.26
_exptl_crystal_size_min 0.21
_refine_diff_density_max 0.717
_refine_diff_density_min -1.248
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.068
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 247
_refine_ls_number_reflns 3966
_refine_ls_number_restraints 5
_refine_ls_restrained_S_all 1.085
_refine_ls_R_factor_all 0.0418
_refine_ls_R_factor_gt 0.0355
_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^)+(0.0492P)^2^+2.8010P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0924
_refine_ls_wR_factor_ref 0.0962
_reflns_number_gt 3523
_reflns_number_total 3966
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file ov3146sup1.cif
_cod_data_source_block 3
_cod_depositor_comments
'Adding full bibliography for 2022355--2022357.cif.'
_cod_database_code 2022357
_cod_database_fobs_code 2022357
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min 0.408
_shelx_estimated_absorpt_t_max 0.560
_shelx_hkl_file
;
-1 0 0 2.26 0.10
-3 0 0 1.46 0.22
-4 0 0 351.38 9.85
-5 0 0 0.40 0.20
-6 0 0 214.84 6.11
-7 0 0 0.39 0.31
-8 0 0 72.00 2.24
-9 0 0 -0.33 0.38
-9 0 0 0.43 0.38
-10 0 0 0.20 0.39
-10 0 0 0.03 0.49
-11 0 0 -0.37 0.53
-11 0 0 0.39 0.45
-12 0 0 -0.25 0.49
-12 0 0 -0.50 0.58
-13 0 0 -0.27 0.65
-13 0 0 0.50 0.55
-14 0 0 0.66 0.72
-14 0 0 1.04 0.64
-15 0 0 0.08 0.72
-15 0 0 -0.70 0.83
-16 0 0 0.25 0.96
-16 0 0 0.92 0.83
-17 0 0 -0.39 0.94
-17 0 0 0.14 1.05
-18 0 0 2.40 1.05
-18 0 0 5.32 1.44
-19 0 0 -0.32 1.19
0 -1 0 0.01 0.03
0 1 0 0.00 0.02
-1 1 0 252.65 7.05
-2 -1 0 250.60 7.01
2 -1 0 230.89 7.00
-2 1 0 252.51 7.00
-2 1 0 250.49 7.00
-2 1 0 268.52 7.00
-3 -1 0 297.43 8.41
-3 1 0 284.18 8.39
-3 1 0 298.13 8.39
-3 1 0 320.45 8.38
-4 -1 0 177.84 5.05
4 -1 0 178.31 4.99
-4 1 0 173.59 5.03
-4 1 0 177.27 5.03
-4 1 0 183.99 4.99
-5 -1 0 106.11 3.08
5 -1 0 107.44 2.99
-5 1 0 106.23 3.06
-5 1 0 106.94 2.99
-5 1 0 103.24 3.05
-6 -1 0 0.14 0.25
-6 1 0 0.02 0.20
-6 1 0 0.28 0.24
-7 -1 0 163.91 4.81
-7 1 0 171.49 4.81
-7 1 0 165.62 4.80
-8 -1 0 1.52 0.37
-8 1 0 1.30 0.36
-8 1 0 1.69 0.33
-9 -1 0 8.46 0.79
-9 1 0 8.80 0.73
-9 1 0 8.38 0.80
-10 -1 0 3.34 0.58
-10 1 0 3.97 0.55
-10 1 0 4.20 0.46
-11 -1 0 1.26 0.55
-11 -1 0 0.79 0.46
-11 1 0 1.12 0.45
-11 1 0 1.20 0.56
-12 -1 0 0.98 0.61
-12 -1 0 0.83 0.49
-12 1 0 0.50 0.58
-12 1 0 0.69 0.51
-13 -1 0 -0.21 0.55
-13 -1 0 -1.01 0.64
-13 1 0 -0.60 0.55
-13 1 0 -0.66 0.60
-14 -1 0 5.21 0.87
-14 -1 0 4.44 0.70
-14 1 0 4.81 0.81
-14 1 0 4.12 0.70
-15 -1 0 3.71 0.91
-15 -1 0 4.65 0.80
-15 1 0 5.10 0.81
-15 1 0 3.97 0.87
-16 -1 0 0.09 1.01
-16 -1 0 1.03 0.84
-16 1 0 -0.83 0.90
-16 1 0 0.89 0.85
-17 -1 0 2.20 1.11
-17 -1 0 1.09 0.92
-17 1 0 1.57 1.09
-17 1 0 2.20 0.98
-18 -1 0 1.33 1.03
-18 -1 0 1.25 1.13
-18 1 0 0.39 1.00
-19 -1 0 0.02 1.21
-19 1 0 0.53 1.23
0 -2 0 101.32 2.64
0 -2 0 93.95 2.69
0 2 0 87.52 2.68
-1 -2 0 67.56 1.89
-1 -2 0 67.78 1.90
1 -2 0 64.16 1.92
-1 2 0 64.99 1.86
-1 2 0 66.73 1.88
-1 2 0 70.23 1.92
1 2 0 63.26 1.91
-2 -2 0 262.63 8.16
2 -2 0 271.54 8.20
2 -2 0 293.29 8.16
-2 -2 0 300.52 8.19
2 2 0 287.43 8.18
-2 2 0 318.30 8.20
-2 2 0 303.60 8.16
-2 2 0 303.64 8.18
-3 -2 0 128.42 3.71
3 -2 0 117.20 3.70
-3 -2 0 126.57 3.65
3 2 0 136.09 3.66
-3 2 0 131.59 3.68
-3 2 0 141.83 3.71
-3 2 0 132.10 3.69
4 -2 0 113.51 3.39
-4 -2 0 118.65 3.42
-4 2 0 121.87 3.40
-4 2 0 111.50 3.38
-4 2 0 130.40 3.39
5 -2 0 53.93 1.55
-5 -2 0 51.48 1.62
-5 2 0 52.12 1.57
-5 2 0 53.05 1.53
-5 2 0 51.11 1.59
-6 -2 0 1.51 0.30
-6 2 0 1.26 0.20
-6 2 0 1.33 0.25
-6 2 0 1.07 0.23
-7 -2 0 4.33 0.53
-7 2 0 4.68 0.55
-7 2 0 5.19 0.51
-7 2 0 4.02 0.24
-8 -2 0 0.19 0.36
8 -2 0 0.74 0.19
-8 2 0 0.60 0.31
-8 2 0 0.57 0.33
-9 -2 0 17.43 0.94
-9 2 0 17.33 0.89
-9 2 0 18.68 0.99
-10 -2 0 0.00 0.49
-10 2 0 0.76 0.39
-10 2 0 -0.11 0.46
-11 -2 0 6.55 0.91
-11 2 0 6.93 0.96
-11 2 0 5.16 0.55
-12 -2 0 0.77 0.50
-12 -2 0 1.19 0.63
-12 2 0 1.22 0.52
-12 2 0 0.26 0.57
-13 -2 0 3.45 0.77
-13 -2 0 3.80 0.63
-13 2 0 3.29 0.63
-13 2 0 3.74 0.69
-14 -2 0 -0.34 0.77
-14 -2 0 -0.33 0.62
-14 2 0 0.04 0.64
-14 2 0 0.16 0.70
-15 -2 0 7.18 0.87
-15 -2 0 11.17 1.64
-15 2 0 7.06 0.88
-15 2 0 10.10 1.42
-16 -2 0 -0.08 0.82
-16 -2 0 0.05 1.00
-16 2 0 -1.18 0.84
-16 2 0 0.91 0.92
-17 -2 0 3.80 0.97
-17 -2 0 4.22 1.20
-17 2 0 4.49 1.01
-18 -2 0 2.06 1.17
-18 -2 0 1.02 1.00
-18 2 0 -2.18 1.01
0 -3 0 0.35 0.15
0 -3 0 0.14 0.07
0 3 0 0.31 0.12
-1 -3 0 108.46 3.04
-1 -3 0 109.28 3.08
1 -3 0 102.12 3.09
-1 3 0 113.61 3.09
1 3 0 102.45 3.08
-1 3 0 109.11 3.03
2 -3 0 649.19 19.34
-2 3 0 759.49 19.34
2 3 0 639.90 19.31
-2 3 0 721.82 19.29
3 -3 0 7.86 0.43
-3 -3 0 9.35 0.35
3 3 0 8.22 0.35
-3 3 0 8.17 0.33
-4 -3 0 7.16 0.29
4 -3 0 5.58 0.39
-4 3 0 7.17 0.35
4 3 0 6.45 0.29
-4 3 0 7.09 0.38
-4 3 0 7.77 0.35
5 -3 0 2.19 0.25
-5 -3 0 2.20 0.29
-5 3 0 2.86 0.27
-5 3 0 2.59 0.34
-5 3 0 1.89 0.22
6 -3 0 7.05 0.42
-6 -3 0 6.33 0.52
-6 3 0 7.63 0.48
-6 3 0 7.30 0.37
-6 3 0 7.05 0.52
-7 -3 0 67.52 2.14
7 -3 0 70.37 2.03
-7 3 0 69.23 2.11
-7 3 0 66.63 2.00
-7 3 0 68.83 2.07
-8 -3 0 26.54 1.12
8 -3 0 27.68 0.90
-8 3 0 26.88 1.03
-8 3 0 27.09 1.06
-8 3 0 25.49 0.86
-9 -3 0 103.74 3.19
9 -3 0 103.96 2.98
-9 3 0 98.44 3.13
-9 3 0 106.13 2.98
-9 3 0 103.89 3.10
10 -3 0 14.07 0.57
-10 -3 0 14.32 1.04
-10 3 0 13.94 0.94
-10 3 0 14.38 0.92
-11 -3 0 69.24 2.43
-11 3 0 72.61 2.35
-11 3 0 71.58 2.38
-12 -3 0 -0.29 0.63
-12 3 0 0.04 0.57
-12 3 0 0.10 0.49
-13 -3 0 19.24 1.43
-13 -3 0 16.57 1.32
-13 3 0 18.29 1.28
-13 3 0 20.83 1.39
-14 -3 0 1.18 0.81
-14 -3 0 0.86 0.66
-14 3 0 1.54 0.67
-14 3 0 0.26 0.69
-15 -3 0 3.44 0.80
-15 -3 0 5.19 1.02
-15 3 0 4.43 0.86
-15 3 0 3.70 0.82
-16 -3 0 6.39 1.12
-16 -3 0 3.31 0.88
-16 3 0 4.86 0.94
-17 -3 0 1.25 0.94
-17 -3 0 3.29 1.20
-17 3 0 0.61 0.99
-18 -3 0 0.44 1.02
-18 -3 0 1.61 1.22
-18 3 0 1.97 1.09
0 -4 0 9.73 0.33
0 4 0 8.76 0.43
1 -4 0 192.11 5.71
-1 -4 0 198.95 5.64
-1 -4 0 205.74 5.69
1 4 0 197.47 5.70
-1 4 0 199.25 5.63
-1 4 0 210.63 5.71
2 -4 0 2.27 0.14
-2 -4 0 2.40 0.25
-2 -4 0 3.31 0.32
2 -4 0 2.14 0.28
2 4 0 2.06 0.26
-2 4 0 2.94 0.26
-3 -4 0 164.41 4.53
-3 -4 0 164.68 4.55
3 -4 0 152.05 4.60
3 -4 0 156.52 4.48
3 4 0 158.79 4.55
-3 4 0 159.35 4.48
-3 4 0 163.74 4.53
-4 -4 0 234.50 6.72
4 -4 0 218.01 6.74
-4 -4 0 236.33 6.66
4 4 0 241.89 6.67
-4 4 0 248.06 6.65
-4 4 0 244.95 6.69
-5 -4 0 87.82 2.51
5 -4 0 84.45 2.61
-5 -4 0 89.33 2.62
-5 4 0 91.14 2.54
-5 4 0 88.56 2.58
5 4 0 87.29 2.52
6 -4 0 83.86 2.45
-6 -4 0 83.23 2.33
-6 -4 0 81.18 2.48
-6 4 0 82.36 2.40
6 4 0 78.75 2.33
-6 4 0 82.78 2.45
7 -4 0 51.64 1.59
-7 -4 0 49.93 1.68
-7 4 0 51.60 1.59
-7 4 0 49.42 1.63
8 -4 0 330.69 9.15
-8 -4 0 318.90 9.25
-8 4 0 324.10 9.20
-8 4 0 323.84 9.17
9 -4 0 32.49 1.09
-9 -4 0 31.62 1.34
-9 4 0 32.20 1.22
-9 4 0 31.45 1.25
10 -4 0 194.06 5.57
-10 -4 0 194.49 5.77
-10 4 0 199.21 5.68
-10 4 0 196.45 5.71
-11 -4 0 1.80 0.62
-11 4 0 1.84 0.50
-11 4 0 2.13 0.49
-12 -4 0 28.43 1.59
-12 4 0 32.86 1.53
-12 4 0 32.45 1.46
-13 -4 0 11.23 1.37
-13 4 0 10.08 1.28
-13 4 0 10.34 1.13
-14 -4 0 27.30 1.81
-14 -4 0 25.87 1.65
-14 4 0 29.59 1.73
-14 4 0 29.24 1.50
-15 -4 0 3.69 0.99
-15 -4 0 2.92 0.81
-15 4 0 1.87 0.84
-16 -4 0 2.21 0.88
-16 -4 0 3.30 1.07
-16 4 0 2.64 0.92
-17 -4 0 7.02 1.27
-17 -4 0 3.26 0.99
-17 4 0 5.27 1.08
-18 -4 0 1.13 1.02
-18 -4 0 0.03 1.23
-18 4 0 0.79 1.10
0 -5 0 1.59 0.27
-1 -5 0 31.11 1.02
-1 -5 0 29.15 0.93
-1 5 0 29.78 0.93
2 -5 0 79.93 2.42
-2 -5 0 82.59 2.37
-2 -5 0 79.28 2.33
2 -5 0 78.08 2.26
-2 5 0 80.63 2.31
-3 -5 0 166.74 4.67
3 -5 0 158.79 4.59
-3 -5 0 172.73 4.67
3 -5 0 163.85 4.75
3 5 0 150.01 4.69
-3 5 0 170.65 4.65
4 -5 0 54.07 1.80
-4 -5 0 57.87 1.76
-4 -5 0 58.57 1.70
-4 5 0 58.81 1.72
4 5 0 55.28 1.72
-4 5 0 58.14 1.65
5 -5 0 99.37 3.06
-5 -5 0 101.47 2.94
-5 -5 0 103.32 3.03
5 5 0 101.81 2.96
-5 5 0 103.03 2.94
-5 5 0 107.53 3.01
-6 -5 0 195.30 5.47
-6 -5 0 191.88 5.60
6 -5 0 197.06 5.59
-6 5 0 200.37 5.50
6 5 0 184.69 5.47
-6 5 0 197.10 5.56
-7 -5 0 69.77 1.93
7 -5 0 69.33 2.08
-7 -5 0 66.69 2.15
7 5 0 61.34 1.93
-7 5 0 68.87 2.03
-7 5 0 66.60 2.09
8 -5 0 2.38 0.36
-8 -5 0 1.75 0.48
-8 5 0 1.51 0.34
-8 5 0 1.64 0.39
9 -5 0 37.47 1.27
-9 -5 0 37.21 1.49
-9 5 0 38.55 1.32
-9 5 0 35.91 1.38
-10 -5 0 1.80 0.56
10 -5 0 2.59 0.37
-10 5 0 2.66 0.44
-10 5 0 1.43 0.44
11 -5 0 69.83 2.11
-11 -5 0 61.11 2.33
-11 5 0 65.71 2.23
-11 5 0 65.70 2.16
-12 -5 0 0.64 0.71
-12 5 0 0.34 0.53
-12 5 0 1.21 0.62
-13 -5 0 17.70 1.50
-13 5 0 18.32 1.23
-13 5 0 18.67 1.40
-14 -5 0 1.52 0.90
-14 5 0 1.07 0.70
-15 -5 0 6.30 0.89
-15 -5 0 4.54 1.08
-15 5 0 6.27 0.91
-16 -5 0 0.66 1.05
-16 -5 0 1.16 0.83
-16 5 0 0.92 0.94
-17 -5 0 3.39 1.00
-17 -5 0 2.50 1.20
-17 5 0 2.81 1.07
-18 -5 0 -1.38 1.01
-18 -5 0 1.39 1.27
-18 5 0 -1.45 1.08
0 -6 0 53.98 1.72
0 -6 0 54.08 1.58
-1 -6 0 48.66 1.46
-1 -6 0 48.74 1.55
1 -6 0 48.11 1.59
1 -6 0 49.81 1.42
-1 6 0 48.51 1.45
2 -6 0 343.19 9.75
2 -6 0 324.05 9.57
-2 -6 0 342.55 9.64
-2 -6 0 357.22 9.69
-2 6 0 349.31 9.62
-3 -6 0 1.78 0.27
3 -6 0 1.31 0.35
3 -6 0 2.35 0.18
-3 6 0 1.94 0.22
4 -6 0 73.48 2.35
-4 -6 0 77.04 2.24
-4 -6 0 74.73 2.28
-4 6 0 77.81 2.25
-4 6 0 75.14 2.16
-5 -6 0 380.81 10.74
5 -6 0 377.18 10.85
-5 -6 0 385.59 10.81
-5 6 0 384.03 10.77
-5 6 0 386.83 10.70
-6 -6 0 133.70 3.95
6 -6 0 136.36 3.96
-6 -6 0 133.09 3.81
-6 6 0 133.59 3.81
-6 6 0 131.92 3.89
-7 -6 0 318.19 8.77
7 -6 0 332.59 8.93
-7 -6 0 304.69 8.93
7 6 0 295.80 8.78
-7 6 0 313.39 8.81
-7 6 0 314.15 8.88
8 -6 0 2.54 0.43
-8 -6 0 2.66 0.51
-8 6 0 2.61 0.42
8 6 0 2.38 0.28
-8 6 0 2.48 0.33
9 -6 0 56.93 1.86
-9 -6 0 57.79 2.02
-9 6 0 58.01 1.94
-9 6 0 58.28 1.83
10 -6 0 23.04 0.98
-10 -6 0 21.47 1.19
-10 6 0 23.75 1.00
-10 6 0 23.40 1.15
-11 -6 0 0.26 0.61
11 -6 0 0.21 0.36
-11 6 0 0.01 0.49
-11 6 0 0.12 0.42
-12 -6 0 15.28 1.31
-12 6 0 17.13 1.09
-12 6 0 16.51 1.24
-13 -6 0 3.93 0.86
-13 6 0 3.28 0.68
-14 -6 0 -0.38 0.90
-14 6 0 1.41 0.75
-15 -6 0 1.42 1.04
-15 6 0 2.97 0.87
-16 -6 0 1.98 1.12
-16 -6 0 1.39 0.88
-16 6 0 0.49 0.93
-17 -6 0 0.71 0.97
-17 -6 0 1.30 1.20
-17 6 0 -0.16 1.01
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6 -1 -9 16.05 1.00
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5 -1 -9 6.61 0.81
5 1 -9 6.00 0.79
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4 -1 -9 5.59 0.76
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-4 -1 9 5.20 0.50
-4 1 9 6.48 0.46
4 1 -9 7.07 0.75
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3 -1 -9 0.21 0.42
-3 -1 9 2.50 0.41
3 1 -9 1.18 0.44
2 -1 -9 34.53 1.37
-2 1 9 35.55 1.04
-1 -1 9 1.73 0.47
-1 -1 9 0.93 0.35
1 -1 -9 1.03 0.39
1 -1 -9 1.12 0.44
0 -1 9 6.65 0.63
0 -1 -9 5.29 0.70
0 -1 -9 5.86 0.70
0 -1 9 6.85 0.79
0 1 -9 5.92 0.73
-1 -1 -9 9.91 0.82
1 -1 9 10.95 0.72
1 -1 9 10.21 0.87
-1 -1 -9 8.90 0.84
-1 1 -9 9.33 0.83
2 -1 9 90.83 2.67
2 -1 9 88.82 2.80
-2 -1 -9 88.15 2.74
-2 -1 -9 83.04 2.78
-2 1 -9 84.82 2.77
-3 -1 -9 46.92 1.71
3 -1 9 45.23 1.57
3 -1 9 45.76 1.72
-3 1 -9 45.18 1.70
3 1 9 48.19 1.77
3 1 9 46.43 1.60
4 -1 9 195.93 5.91
-4 -1 -9 200.41 5.96
-4 1 -9 202.76 5.97
4 1 9 204.76 5.94
4 1 9 205.18 5.82
5 -1 9 7.35 0.88
-5 -1 -9 6.16 0.89
-5 1 -9 6.57 0.43
-5 1 -9 6.62 0.96
5 1 9 6.52 0.72
5 1 9 7.68 0.91
-6 -1 -9 158.88 4.18
-6 -1 -9 143.66 4.40
6 -1 9 130.84 4.23
-6 1 -9 140.67 4.05
6 1 9 134.53 4.25
-6 1 -9 141.26 4.36
7 -1 9 3.13 0.59
-7 -1 -9 2.70 0.70
7 1 9 3.72 0.58
-7 1 -9 2.50 0.67
-7 1 -9 2.25 0.31
8 -1 9 38.96 1.52
-8 -1 -9 38.31 1.84
-8 1 -9 38.23 1.46
-8 1 -9 37.05 1.79
8 1 9 36.18 1.51
-9 -1 -9 27.19 1.71
-9 1 -9 26.12 1.61
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-10 1 -9 13.60 1.48
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-12 -1 -9 1.91 1.02
-12 1 -9 1.57 0.98
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-13 1 -9 -0.10 1.00
-14 -1 -9 1.58 1.15
-14 1 -9 2.34 1.15
-15 -1 -9 -0.66 1.19
-15 1 -9 -1.11 1.09
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-17 -2 9 2.78 1.41
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-16 -2 9 5.98 1.06
-16 -2 9 3.97 1.01
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-15 -2 9 1.87 0.86
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-14 -2 9 8.13 0.94
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-13 -2 9 1.11 0.69
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-13 2 9 0.48 0.66
12 -2 -9 22.26 1.33
-12 -2 9 24.87 1.40
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-11 -2 9 0.62 0.57
-11 -2 9 1.35 0.62
11 -2 -9 0.64 0.64
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-11 2 9 0.72 0.52
10 -2 -9 32.36 1.50
-10 -2 9 32.19 1.49
-10 -2 9 34.38 1.44
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-10 2 9 33.61 1.43
-9 -2 9 2.77 0.61
-9 -2 9 2.41 0.44
9 -2 -9 2.90 0.63
-9 -2 9 2.04 0.58
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8 -2 -9 63.89 2.29
-8 -2 9 67.81 2.16
-8 -2 9 70.01 2.33
-8 -2 9 65.98 2.30
-8 2 9 66.32 2.22
-8 2 9 68.31 2.21
-7 -2 9 165.87 4.90
7 -2 -9 160.12 4.86
-7 -2 9 166.20 4.77
-7 2 9 159.17 4.73
-6 -2 9 148.40 4.27
-6 -2 9 148.49 4.41
6 -2 -9 138.47 4.35
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-5 -2 9 72.76 2.41
5 -2 -9 70.45 2.38
-5 -2 9 73.15 2.27
-5 2 9 72.08 2.17
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4 -2 -9 26.07 1.19
-4 -2 9 25.83 1.23
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3 -2 -9 50.04 1.78
-3 -2 9 50.59 1.68
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-2 -2 9 18.12 0.84
-2 -2 9 17.05 0.98
2 -2 -9 17.16 0.98
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1 -2 -9 13.58 0.81
1 -2 -9 12.28 0.88
-1 -2 9 13.61 0.91
0 -2 9 5.23 0.58
0 -2 -9 4.47 0.55
0 -2 9 4.01 0.55
0 -2 -9 5.39 0.67
-1 -2 -9 15.94 0.93
-1 -2 -9 16.63 0.96
1 -2 9 16.60 0.81
1 -2 9 17.76 0.99
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-2 -2 -9 14.81 1.00
-2 -2 -9 15.38 0.95
2 -2 9 14.17 0.97
-2 2 -9 15.64 0.99
3 -2 9 43.26 1.64
-3 -2 -9 41.77 1.61
-3 -2 -9 45.13 1.60
-3 2 -9 43.03 1.64
4 -2 9 3.41 0.56
-4 -2 -9 4.05 0.55
-4 -2 -9 4.11 0.56
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5 -2 9 7.96 0.88
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5 2 9 7.02 0.92
5 2 9 8.14 0.75
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6 -2 9 5.75 0.65
6 2 9 6.11 0.73
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6 2 9 5.93 0.68
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7 -2 9 43.40 1.64
-7 -2 -9 42.18 1.89
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-7 2 -9 40.65 1.41
7 2 9 44.90 1.66
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8 -2 9 5.91 0.66
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-8 2 -9 5.94 0.79
8 2 9 6.10 0.95
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9 -2 9 4.78 0.83
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-12 -2 -9 0.96 1.02
-12 2 -9 2.21 0.97
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-14 -2 -9 0.02 1.14
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-15 -2 -9 -0.52 1.19
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-18 3 9 1.11 1.20
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-15 -3 9 1.26 0.89
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-14 -3 9 0.39 0.79
-14 3 9 0.67 0.75
-13 -3 9 19.89 1.44
-13 3 9 20.29 1.48
-12 -3 9 1.43 0.70
12 -3 -9 0.67 0.67
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-12 3 9 0.93 0.57
-11 -3 9 51.07 1.88
-11 -3 9 52.43 2.04
11 -3 -9 50.28 1.99
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-11 3 9 51.69 1.93
-10 -3 9 18.37 1.14
-10 -3 9 21.11 1.24
10 -3 -9 16.62 1.28
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-10 3 9 18.40 1.02
9 -3 -9 92.23 2.95
-9 -3 9 89.36 2.92
-9 -3 9 86.12 2.86
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-9 3 9 87.66 2.76
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-8 -3 9 34.13 1.56
8 -3 -9 33.33 1.51
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-8 3 9 36.06 1.37
7 -3 -9 42.10 1.68
-7 -3 9 43.42 1.66
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-6 -3 9 72.97 2.29
6 -3 -9 73.19 2.43
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5 -3 -9 53.05 1.94
-5 -3 9 55.94 1.96
-5 -3 9 56.07 1.80
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-4 -3 9 154.29 4.58
4 -3 -9 147.80 4.54
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3 -3 -9 6.18 0.75
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-3 -3 9 6.99 0.82
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2 -3 -9 48.76 1.72
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1 -3 -9 44.52 1.63
1 -3 -9 44.87 1.55
0 -3 9 3.48 0.52
0 -3 -9 2.62 0.52
0 -3 -9 3.57 0.46
1 -3 9 0.00 0.45
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-1 -3 -9 0.29 0.40
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2 -3 9 3.51 0.54
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3 -3 9 3.36 0.56
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4 -3 9 0.68 0.50
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5 -3 9 1.21 0.52
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6 -3 9 0.70 0.54
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8 -3 9 0.15 0.56
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-18 -4 9 1.99 1.15
-18 4 9 -0.87 1.19
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-17 -4 9 0.05 1.06
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-16 -4 9 2.07 1.07
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12 -4 -9 21.11 1.40
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11 -4 -9 0.61 0.67
-11 -4 9 0.32 0.55
-11 4 9 -0.39 0.51
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10 -4 -9 42.19 1.80
-10 -4 9 44.79 1.79
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8 -4 -9 22.16 1.27
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-7 -4 9 91.34 2.89
-7 4 9 90.00 2.73
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-6 -4 9 -0.29 0.49
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5 -4 -9 96.19 3.06
-5 -4 9 96.47 3.06
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4 -4 -9 1.66 0.48
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3 -4 -9 119.52 3.70
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2 -4 -9 11.23 0.77
2 -4 -9 10.58 0.89
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1 -4 -9 19.66 1.06
1 -4 -9 19.70 0.95
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0 -4 -9 42.46 1.51
0 -4 -9 42.91 1.62
0 -4 9 42.46 1.59
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1 -4 9 85.41 2.76
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2 -4 9 25.66 1.22
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5 -4 9 1.81 0.55
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6 -4 9 2.42 0.58
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8 -4 9 1.61 0.61
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-15 -4 -9 -2.14 1.28
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-16 -5 9 0.76 1.14
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11 -5 -9 5.42 0.83
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10 -5 -9 9.02 1.23
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9 -5 -9 4.89 0.75
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8 -5 -9 44.99 1.82
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7 -5 -9 2.75 0.63
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6 -5 -9 94.28 3.06
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5 -5 -9 53.18 1.94
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4 -5 -9 63.74 2.20
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3 -5 -9 79.76 2.61
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2 -5 -9 127.84 3.82
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1 -5 -9 205.05 5.98
1 -5 -9 207.55 6.07
0 -5 9 131.71 4.01
0 -5 -9 133.36 4.03
0 -5 -9 131.81 3.94
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3 -5 9 10.29 0.90
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-15 -5 -9 1.41 1.42
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9 -6 -9 11.29 1.22
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8 -6 -9 5.69 0.75
-8 -6 9 4.50 0.71
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7 -6 -9 21.16 1.27
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6 -6 -9 7.39 0.94
-6 -6 9 8.76 0.95
-6 6 9 8.19 0.67
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5 -6 -9 23.36 1.23
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4 -6 -9 10.54 0.96
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-4 6 9 11.52 0.60
3 -6 -9 1.79 0.51
-3 -6 9 1.01 0.54
-3 6 9 1.34 0.22
2 -6 -9 280.87 7.94
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2 -6 -9 273.36 8.06
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1 -6 -9 65.12 2.08
1 -6 -9 64.74 2.22
0 -6 -9 183.29 5.28
0 -6 9 178.78 5.27
0 -6 -9 169.29 5.16
-1 -6 -9 34.91 1.48
1 -6 9 34.29 1.46
-1 -6 -9 35.64 1.39
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2 -6 9 115.99 3.60
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3 -6 9 0.08 0.52
-3 -6 -9 0.18 0.52
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4 -6 9 51.50 1.89
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5 -6 9 4.22 0.63
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6 -6 9 41.81 1.71
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2 5 18 -0.73 1.77
3 -5 18 0.51 1.83
3 5 18 0.20 1.38
3 5 18 1.58 1.89
-4 -5 -18 7.46 1.74
4 5 18 0.98 1.65
4 5 18 3.02 2.27
-5 -5 -18 3.31 1.85
-11 -6 18 0.39 1.70
-10 -6 18 -0.16 1.63
-7 -6 18 1.56 1.66
7 -6 -18 2.31 1.67
6 -6 -18 3.43 1.65
-6 -6 18 -2.18 1.53
5 -6 -18 1.36 1.56
-5 -6 18 0.78 1.60
4 -6 -18 4.04 1.62
-4 -6 18 2.70 1.64
-3 -6 18 0.49 1.58
3 -6 -18 0.02 1.48
2 -6 -18 2.82 1.55
-2 -6 18 0.12 1.57
1 -6 -18 0.64 1.47
-1 -6 18 2.02 1.61
-1 6 18 -2.59 1.60
-1 6 18 -0.98 1.22
0 -6 18 0.73 1.56
0 6 18 -0.93 1.24
0 6 18 0.32 1.70
1 -6 18 0.74 1.62
1 6 18 2.07 1.74
1 6 18 2.67 1.32
2 -6 18 0.20 2.27
2 6 18 0.99 1.37
2 6 18 1.36 1.79
3 6 18 3.56 1.79
3 6 18 4.00 2.30
-4 -6 -18 3.29 1.75
-5 -6 -18 8.13 2.05
-10 -7 18 0.27 1.70
-6 -7 18 0.42 1.96
-5 -7 18 -0.14 1.71
5 -7 -18 3.17 1.78
-4 -7 18 0.63 1.64
4 -7 -18 2.62 1.67
-3 -7 18 -0.76 1.61
3 -7 -18 1.80 1.58
-2 -7 18 0.84 1.62
2 -7 -18 1.40 1.55
1 -7 -18 -1.84 1.43
-1 -7 18 1.08 1.59
0 -7 18 -0.08 1.71
0 -7 -18 0.53 1.53
1 7 18 -0.40 1.42
1 7 18 0.88 1.93
-3 -7 -18 5.67 1.77
-4 -7 -18 7.66 1.95
-9 -8 18 -0.49 1.74
2 -8 -18 1.15 2.30
1 -8 -18 0.95 2.12
-3 -8 -18 6.97 1.86
-4 -8 -18 5.06 1.96
-9 -9 18 1.35 2.26
-3 -9 -18 0.57 1.68
-8 -10 18 1.65 1.92
-5 0 19 6.06 2.27
-4 0 19 2.44 1.72
-3 0 19 8.76 1.85
-2 0 19 1.09 1.72
-1 0 19 3.38 1.89
0 0 19 -1.02 2.08
-10 -1 19 0.27 1.58
-5 -1 19 0.21 2.05
-5 1 19 1.86 1.99
-5 1 19 0.95 1.54
-4 -1 19 6.42 1.79
-4 1 19 5.58 1.31
-4 1 19 6.28 1.72
-3 -1 19 4.60 1.77
-3 1 19 3.10 1.69
-3 1 19 5.16 1.31
-2 -1 19 1.40 1.81
-2 1 19 2.32 1.75
-1 -1 19 1.12 1.86
-1 1 19 -1.08 1.82
0 -1 19 0.47 2.04
0 1 19 0.38 2.17
-10 -2 19 0.01 1.61
-5 -2 19 3.37 1.96
-5 2 19 3.06 1.41
-4 -2 19 1.08 2.11
-4 2 19 1.52 1.42
-4 2 19 0.50 2.05
-3 -2 19 2.69 2.02
-3 2 19 2.18 1.25
-3 2 19 3.12 1.78
-2 -2 19 2.10 1.87
-2 2 19 2.35 1.40
-2 2 19 3.54 1.87
-1 -2 19 -0.03 2.14
-1 2 19 1.45 1.34
-1 2 19 0.63 1.78
0 2 19 4.09 2.62
-10 -3 19 0.24 1.72
-3 3 19 -0.25 1.48
-3 3 19 2.91 1.91
-2 -3 19 -2.15 1.84
-2 3 19 0.39 2.06
-2 3 19 -1.82 2.57
-1 3 19 3.93 2.04
-1 3 19 3.51 2.60
0 0 0 0.00 0.00
;
_shelx_hkl_checksum 96525
_shelx_res_file
;
TITL P21N in P2(1)/n
p21n.res
created by SHELXL-2018/3 at 19:51:43 on 11-Mar-2020
CELL 0.71073 11.5479 14.7949 12.3782 90 99.813 90
ZERR 4 0.0007 0.001 0.0009 0 0.002 0
LATT 1
SYMM 0.5-X,0.5+Y,0.5-Z
SFAC C H N O Zn Br
UNIT 76 112 4 20 4 4
DELU 0.001 0.001 Zn1 O2 C8
DELU 0.001 0.001 O2 C8 O3
L.S. 4
PLAN 5
SIZE 0.21 0.26 0.35
TEMP 16.85
BOND
fmap 2
acta
OMIT 0 51.5
OMIT 1 1 0
OMIT 0 1 1
REM
REM
REM
WGHT 0.049200 2.801000
FVAR 0.19999
O5 4 0.627710 0.034222 0.540565 11.00000 0.02938 0.02125 =
0.02774 0.00004 0.00299 -0.00091
C1 1 0.762892 -0.050019 0.667351 11.00000 0.02481 0.01769 =
0.02560 -0.00129 0.00654 -0.00101
N1 3 1.168402 0.244693 0.809525 11.00000 0.02366 0.02003 =
0.03076 -0.00614 0.00539 -0.00063
C2 1 0.820449 0.028917 0.707660 11.00000 0.02462 0.01433 =
0.02911 0.00269 0.00233 0.00035
AFIX 43
H2 2 0.793506 0.084924 0.679920 11.00000 -1.20000
AFIX 0
C3 1 0.898681 -0.137991 0.793994 11.00000 0.03672 0.01908 =
0.03412 0.00915 0.01466 0.00789
C9 1 0.957670 0.180233 0.776819 11.00000 0.02348 0.02012 =
0.04852 0.00014 -0.00102 0.00005
AFIX 23
H9A 2 0.877783 0.198673 0.780298 11.00000 -1.20000
H9B 2 0.964954 0.173597 0.700304 11.00000 -1.20000
AFIX 0
C10 1 1.042539 0.250816 0.829984 11.00000 0.02372 0.02208 =
0.04448 -0.00741 0.00809 0.00078
AFIX 23
H10A 2 1.044118 0.248118 0.908518 11.00000 -1.20000
H10B 2 1.011841 0.309683 0.805254 11.00000 -1.20000
AFIX 0
C4 1 0.801405 -0.133182 0.711281 11.00000 0.03497 0.01580 =
0.03422 0.00025 0.01269 -0.00200
AFIX 43
H4 2 0.761982 -0.185707 0.685258 11.00000 -1.20000
AFIX 0
O1 4 0.982484 0.096520 0.832192 11.00000 0.03664 0.02475 =
0.04412 0.00526 -0.01256 -0.00850
C5 1 0.957778 -0.060135 0.832429 11.00000 0.02939 0.02864 =
0.03060 0.00833 0.00272 0.00475
AFIX 43
H5 2 1.023901 -0.063376 0.886931 11.00000 -1.20000
AFIX 0
C6 1 0.660600 -0.042925 0.575582 11.00000 0.02661 0.02166 =
0.02851 -0.00298 0.00722 -0.00419
C16 1 1.230113 0.159472 0.858012 11.00000 0.02960 0.02787 =
0.03568 -0.00167 0.00596 0.00749
AFIX 23
H16A 2 1.188629 0.107773 0.821950 11.00000 -1.20000
H16B 2 1.308733 0.158960 0.840231 11.00000 -1.20000
AFIX 0
C7 1 0.917776 0.023093 0.789117 11.00000 0.02634 0.01988 =
0.03204 0.00263 0.00412 -0.00303
C11 1 1.175246 0.241199 0.687823 11.00000 0.03652 0.02945 =
0.02841 -0.00803 0.00616 0.00037
AFIX 23
H11A 2 1.257539 0.239072 0.680621 11.00000 -1.20000
H11B 2 1.139721 0.184978 0.658536 11.00000 -1.20000
AFIX 0
C13 1 1.227642 0.329149 0.863482 11.00000 0.03226 0.02550 =
0.03642 -0.01166 0.00681 -0.00849
AFIX 23
H13A 2 1.184349 0.381604 0.831575 11.00000 -1.20000
H13B 2 1.221987 0.327893 0.940759 11.00000 -1.20000
AFIX 0
C12 1 1.118360 0.317155 0.617316 11.00000 0.06675 0.04126 =
0.03862 0.00173 0.00586 0.00673
AFIX 23
H12A 2 1.151002 0.374520 0.645730 11.00000 -1.20000
H12B 2 1.034542 0.317846 0.618245 11.00000 -1.20000
AFIX 0
C8 1 0.943482 -0.227351 0.842782 11.00000 0.06682 0.02749 =
0.04106 0.01553 0.02653 0.02177
C14 1 1.355108 0.340888 0.853192 11.00000 0.03709 0.06125 =
0.06219 -0.02546 0.01481 -0.02221
AFIX 23
H14A 2 1.362331 0.345540 0.776457 11.00000 -1.20000
H14B 2 1.399997 0.288818 0.884093 11.00000 -1.20000
AFIX 0
C17 1 1.240254 0.146741 0.980202 11.00000 0.06323 0.05106 =
0.03602 0.00309 0.00977 0.01734
AFIX 23
H17A 2 1.162833 0.149449 1.000526 11.00000 -1.20000
H17B 2 1.287675 0.194831 1.018348 11.00000 -1.20000
AFIX 0
C15 1 1.402757 0.425629 0.913402 11.00000 0.06385 0.08471 =
0.07102 -0.03819 0.02435 -0.04870
AFIX 137
H15A 2 1.358855 0.477058 0.881770 11.00000 -1.50000
H15B 2 1.483990 0.432983 0.907311 11.00000 -1.50000
H15C 2 1.395652 0.420603 0.989319 11.00000 -1.50000
AFIX 0
C18 1 1.296212 0.056438 1.013193 11.00000 0.07342 0.06642 =
0.05062 0.02103 0.01144 0.02626
AFIX 137
H18A 2 1.305587 0.049750 1.091343 11.00000 -1.50000
H18B 2 1.371736 0.053264 0.990847 11.00000 -1.50000
H18C 2 1.246893 0.008879 0.978367 11.00000 -1.50000
AFIX 0
O4 4 0.615173 -0.115819 0.536392 11.00000 0.04238 0.02179 =
0.04373 -0.00794 -0.00726 -0.00586
O2 4 0.872959 -0.290533 0.842167 11.00000 0.08000 0.02178 =
0.10771 0.03006 0.04272 0.02394
O3 4 1.048102 -0.235709 0.883741 11.00000 0.08384 0.04797 =
0.06604 0.01710 -0.01071 0.03120
C20 1 1.139949 0.304148 0.501261 11.00000 0.08420 0.06527 =
0.03526 0.00419 0.00129 -0.00009
AFIX 137
H20A 2 1.222957 0.304751 0.500619 11.00000 -1.50000
H20B 2 1.102976 0.352185 0.455846 11.00000 -1.50000
H20C 2 1.107624 0.247248 0.473613 11.00000 -1.50000
AFIX 0
ZN1 5 0.993869 -0.389714 0.902429 11.00000 0.03115 0.01738 =
0.03124 0.00360 0.00376 0.00365
BR1 6 1.042863 -0.465925 0.749630 11.00000 0.06508 0.04044 =
0.04195 -0.00023 0.02288 0.00433
HKLF 4
REM P21N in P2(1)/n
REM wR2 = 0.0962, GooF = S = 1.068, Restrained GooF = 1.085 for all data
REM R1 = 0.0355 for 3523 Fo > 4sig(Fo) and 0.0418 for all 3966 data
REM 247 parameters refined using 5 restraints
END
WGHT 0.0492 2.7987
REM Highest difference peak 0.717, deepest hole -1.248, 1-sigma level 0.078
Q1 1 0.9819 -0.2545 0.8961 11.00000 0.05 0.72
Q2 1 0.9012 -0.3114 0.8637 11.00000 0.05 0.61
Q3 1 0.8434 -0.2957 0.7679 11.00000 0.05 0.59
Q4 1 1.1089 -0.4496 0.8011 11.00000 0.05 0.52
Q5 1 1.0035 -0.3902 0.8393 11.00000 0.05 0.46
;
_shelx_res_checksum 32813
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
O O5 0.62771(16) 0.03422(12) 0.54057(16) 0.0263(4) Uani d 1 . .
C C1 0.7629(2) -0.05002(17) 0.6674(2) 0.0224(5) Uani d 1 . .
N N1 1.16840(19) 0.24469(15) 0.80952(19) 0.0247(5) Uani d 1 . .
C C2 0.8204(2) 0.02892(17) 0.7077(2) 0.0230(5) Uani d 1 . .
H H2 0.793506 0.084924 0.679920 0.028 Uiso calc 1 . .
C C3 0.8987(3) -0.13799(19) 0.7940(2) 0.0290(6) Uani d 1 . .
C C9 0.9577(2) 0.18023(19) 0.7768(3) 0.0315(6) Uani d 1 . .
H H9A 0.877783 0.198673 0.780298 0.038 Uiso calc 1 . .
H H9B 0.964954 0.173597 0.700304 0.038 Uiso calc 1 . .
C C10 1.0425(2) 0.25082(19) 0.8300(3) 0.0298(6) Uani d 1 . .
H H10A 1.044118 0.248118 0.908518 0.036 Uiso calc 1 . .
H H10B 1.011841 0.309683 0.805254 0.036 Uiso calc 1 . .
C C4 0.8014(2) -0.13318(18) 0.7113(2) 0.0275(6) Uani d 1 . .
H H4 0.761982 -0.185707 0.685258 0.033 Uiso calc 1 . .
O O1 0.98248(19) 0.09652(14) 0.83219(19) 0.0374(5) Uani d 1 . .
C C5 0.9578(2) -0.0601(2) 0.8324(2) 0.0298(6) Uani d 1 . .
H H5 1.023901 -0.063376 0.886931 0.036 Uiso calc 1 . .
C C6 0.6606(2) -0.04292(18) 0.5756(2) 0.0253(6) Uani d 1 . .
C C16 1.2301(2) 0.1595(2) 0.8580(2) 0.0310(6) Uani d 1 . .
H H16A 1.188629 0.107773 0.821950 0.037 Uiso calc 1 . .
H H16B 1.308733 0.158960 0.840231 0.037 Uiso calc 1 . .
C C7 0.9178(2) 0.02309(18) 0.7891(2) 0.0262(6) Uani d 1 . .
C C11 1.1752(3) 0.2412(2) 0.6878(2) 0.0314(6) Uani d 1 . .
H H11A 1.257539 0.239072 0.680621 0.038 Uiso calc 1 . .
H H11B 1.139721 0.184978 0.658536 0.038 Uiso calc 1 . .
C C13 1.2276(2) 0.3291(2) 0.8635(3) 0.0313(6) Uani d 1 . .
H H13A 1.184349 0.381604 0.831575 0.038 Uiso calc 1 . .
H H13B 1.221987 0.327893 0.940759 0.038 Uiso calc 1 . .
C C12 1.1184(4) 0.3172(3) 0.6173(3) 0.0492(9) Uani d 1 . .
H H12A 1.151002 0.374520 0.645730 0.059 Uiso calc 1 . .
H H12B 1.034542 0.317846 0.618245 0.059 Uiso calc 1 . .
C C8 0.9435(3) -0.2274(2) 0.8428(3) 0.0431(7) Uani d 1 . .
C C14 1.3551(3) 0.3409(3) 0.8532(3) 0.0528(10) Uani d 1 . .
H H14A 1.362331 0.345540 0.776457 0.063 Uiso calc 1 . .
H H14B 1.399997 0.288818 0.884093 0.063 Uiso calc 1 . .
C C17 1.2403(4) 0.1467(3) 0.9802(3) 0.0499(9) Uani d 1 . .
H H17A 1.162833 0.149449 1.000526 0.060 Uiso calc 1 . .
H H17B 1.287675 0.194831 1.018348 0.060 Uiso calc 1 . .
C C15 1.4028(4) 0.4256(3) 0.9134(4) 0.0717(14) Uani d 1 . .
H H15A 1.358855 0.477058 0.881770 0.108 Uiso calc 1 . .
H H15B 1.483990 0.432983 0.907311 0.108 Uiso calc 1 . .
H H15C 1.395652 0.420603 0.989319 0.108 Uiso calc 1 . .
C C18 1.2962(4) 0.0564(3) 1.0132(4) 0.0634(11) Uani d 1 . .
H H18A 1.305587 0.049750 1.091343 0.095 Uiso calc 1 . .
H H18B 1.371736 0.053264 0.990847 0.095 Uiso calc 1 . .
H H18C 1.246893 0.008879 0.978367 0.095 Uiso calc 1 . .
O O4 0.61517(19) -0.11582(13) 0.53639(19) 0.0377(5) Uani d 1 . .
O O2 0.8730(3) -0.29053(16) 0.8422(3) 0.0667(8) Uani d 1 . .
O O3 1.0481(3) -0.2357(2) 0.8837(3) 0.0687(8) Uani d 1 . .
C C20 1.1399(4) 0.3041(3) 0.5013(3) 0.0626(11) Uani d 1 . .
H H20A 1.222957 0.304751 0.500619 0.094 Uiso calc 1 . .
H H20B 1.102976 0.352185 0.455846 0.094 Uiso calc 1 . .
H H20C 1.107624 0.247248 0.473613 0.094 Uiso calc 1 . .
Zn Zn1 0.99387(3) -0.38971(2) 0.90243(3) 0.02677(11) Uani d 1 . .
Br Br1 1.04286(3) -0.46593(2) 0.74963(3) 0.04755(13) Uani d 1 . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
O5 0.0294(10) 0.0213(10) 0.0277(10) -0.0009(7) 0.0030(8) 0.0000(8)
C1 0.0248(12) 0.0177(12) 0.0256(13) -0.0010(10) 0.0065(10) -0.0013(10)
N1 0.0237(11) 0.0200(11) 0.0308(12) -0.0006(9) 0.0054(9) -0.0061(9)
C2 0.0246(12) 0.0143(12) 0.0291(14) 0.0004(9) 0.0023(10) 0.0027(10)
C3 0.0367(15) 0.0191(13) 0.0341(15) 0.0079(11) 0.0147(12) 0.0092(11)
C9 0.0235(13) 0.0201(13) 0.0485(18) 0.0001(10) -0.0010(12) 0.0001(12)
C10 0.0237(13) 0.0221(13) 0.0445(17) 0.0008(11) 0.0081(11) -0.0074(12)
C4 0.0350(14) 0.0158(12) 0.0342(15) -0.0020(10) 0.0127(11) 0.0002(11)
O1 0.0366(11) 0.0248(10) 0.0441(13) -0.0085(9) -0.0126(9) 0.0053(9)
C5 0.0294(14) 0.0286(15) 0.0306(15) 0.0047(11) 0.0027(11) 0.0083(12)
C6 0.0266(13) 0.0217(13) 0.0285(14) -0.0042(10) 0.0072(10) -0.0030(11)
C16 0.0296(14) 0.0279(15) 0.0357(16) 0.0075(11) 0.0060(11) -0.0017(12)
C7 0.0263(13) 0.0199(13) 0.0320(15) -0.0030(10) 0.0041(11) 0.0026(11)
C11 0.0365(15) 0.0295(15) 0.0284(15) 0.0004(12) 0.0062(11) -0.0080(12)
C13 0.0323(15) 0.0255(14) 0.0364(16) -0.0085(11) 0.0068(11) -0.0117(12)
C12 0.067(2) 0.041(2) 0.0386(19) 0.0067(17) 0.0059(16) 0.0017(16)
C8 0.0668(14) 0.0275(10) 0.0411(18) 0.0218(10) 0.0265(13) 0.0155(13)
C14 0.0371(18) 0.061(2) 0.062(2) -0.0222(17) 0.0148(16) -0.025(2)
C17 0.063(2) 0.051(2) 0.0360(18) 0.0173(18) 0.0098(16) 0.0031(16)
C15 0.064(3) 0.085(3) 0.071(3) -0.049(2) 0.024(2) -0.038(3)
C18 0.073(3) 0.066(3) 0.051(2) 0.026(2) 0.011(2) 0.021(2)
O4 0.0424(12) 0.0218(10) 0.0437(13) -0.0059(9) -0.0073(9) -0.0079(9)
O2 0.0800(14) 0.0218(11) 0.108(2) 0.0239(8) 0.0427(15) 0.0301(13)
O3 0.0838(14) 0.0480(16) 0.0660(18) 0.0312(12) -0.0107(15) 0.0171(14)
C20 0.084(3) 0.065(3) 0.0353(19) 0.000(2) 0.0013(18) 0.0042(19)
Zn1 0.03115(18) 0.01738(17) 0.0312(2) 0.00365(12) 0.00376(13) 0.00360(12)
Br1 0.0651(2) 0.0404(2) 0.0419(2) 0.00433(16) 0.02288(16) -0.00023(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'
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
_geom_angle_publ_flag
Br1 Zn1 O3 . . 106.07(8) ?
Br1 Zn1 C8 . . 107.03(8) ?
O2 Zn1 Br1 . . 106.82(10) ?
O2 Zn1 O3 . . 57.39(11) ?
O2 Zn1 C8 . . 28.79(12) ?
O3 Zn1 C8 . . 28.71(11) ?
O4 Zn1 Br1 4_656 . 117.39(7) ?
O4 Zn1 O2 4_656 . 127.45(12) ?
O4 Zn1 O3 4_656 . 83.21(9) ?
O4 Zn1 O5 4_656 2_646 99.50(9) ?
O4 Zn1 C8 4_656 . 107.28(11) ?
O5 Zn1 Br1 2_646 . 106.91(6) ?
O5 Zn1 O2 2_646 . 93.12(10) ?
O5 Zn1 O3 2_646 . 140.95(10) ?
O5 Zn1 C8 2_646 . 119.23(10) ?
C7 O1 C9 . . 116.8(2) ?
C8 O2 Zn1 . . 97.5(2) ?
C8 O3 Zn1 . . 83.1(2) ?
C6 O4 Zn1 . 4 118.39(19) ?
C6 O5 Zn1 . 2_656 124.98(18) ?
C10 N1 C11 . . 112.3(2) ?
C10 N1 C13 . . 104.4(2) ?
C10 N1 C16 . . 112.4(2) ?
C11 N1 C13 . . 111.5(2) ?
C16 N1 C11 . . 105.2(2) ?
C16 N1 C13 . . 111.2(2) ?
C2 C1 C6 . . 118.7(2) ?
C4 C1 C2 . . 120.1(2) ?
C4 C1 C6 . . 121.2(2) ?
C1 C2 H2 . . 120.4 ?
C7 C2 C1 . . 119.3(2) ?
C7 C2 H2 . . 120.4 ?
C4 C3 C8 . . 121.3(3) ?
C5 C3 C4 . . 120.1(2) ?
C5 C3 C8 . . 118.5(3) ?
C1 C4 H4 . . 120.0 ?
C3 C4 C1 . . 120.0(3) ?
C3 C4 H4 . . 120.0 ?
C3 C5 H5 . . 120.2 ?
C3 C5 C7 . . 119.6(3) ?
C7 C5 H5 . . 120.2 ?
O4 C6 C1 . . 117.1(2) ?
O5 C6 O4 . . 124.3(3) ?
O5 C6 C1 . . 118.6(2) ?
O1 C7 C2 . . 123.8(2) ?
O1 C7 C5 . . 115.3(2) ?
C2 C7 C5 . . 120.9(3) ?
O2 C8 Zn1 . . 53.74(17) ?
O2 C8 C3 . . 118.6(3) ?
O3 C8 Zn1 . . 68.14(19) ?
O3 C8 O2 . . 121.6(3) ?
O3 C8 C3 . . 119.8(3) ?
C3 C8 Zn1 . . 170.9(3) ?
O1 C9 H9A . . 109.8 ?
O1 C9 H9B . . 109.8 ?
O1 C9 C10 . . 109.3(2) ?
H9A C9 H9B . . 108.3 ?
C10 C9 H9A . . 109.8 ?
C10 C9 H9B . . 109.8 ?
N1 C10 H10A . . 108.0 ?
N1 C10 H10B . . 108.0 ?
C9 C10 N1 . . 117.1(2) ?
C9 C10 H10A . . 108.0 ?
C9 C10 H10B . . 108.0 ?
H10A C10 H10B . . 107.3 ?
N1 C11 H11A . . 108.0 ?
N1 C11 H11B . . 108.0 ?
H11A C11 H11B . . 107.2 ?
C12 C11 N1 . . 117.2(3) ?
C12 C11 H11A . . 108.0 ?
C12 C11 H11B . . 108.0 ?
C11 C12 H12A . . 109.8 ?
C11 C12 H12B . . 109.8 ?
C11 C12 C20 . . 109.3(3) ?
H12A C12 H12B . . 108.3 ?
C20 C12 H12A . . 109.8 ?
C20 C12 H12B . . 109.8 ?
N1 C13 H13A . . 108.4 ?
N1 C13 H13B . . 108.4 ?
H13A C13 H13B . . 107.5 ?
C14 C13 N1 . . 115.4(2) ?
C14 C13 H13A . . 108.4 ?
C14 C13 H13B . . 108.4 ?
C13 C14 H14A . . 109.8 ?
C13 C14 H14B . . 109.8 ?
C13 C14 C15 . . 109.4(3) ?
H14A C14 H14B . . 108.2 ?
C15 C14 H14A . . 109.8 ?
C15 C14 H14B . . 109.8 ?
C14 C15 H15A . . 109.5 ?
C14 C15 H15B . . 109.5 ?
C14 C15 H15C . . 109.5 ?
H15A C15 H15B . . 109.5 ?
H15A C15 H15C . . 109.5 ?
H15B C15 H15C . . 109.5 ?
N1 C16 H16A . . 108.1 ?
N1 C16 H16B . . 108.1 ?
H16A C16 H16B . . 107.3 ?
C17 C16 N1 . . 116.8(2) ?
C17 C16 H16A . . 108.1 ?
C17 C16 H16B . . 108.1 ?
C16 C17 H17A . . 109.7 ?
C16 C17 H17B . . 109.7 ?
C16 C17 C18 . . 109.8(3) ?
H17A C17 H17B . . 108.2 ?
C18 C17 H17A . . 109.7 ?
C18 C17 H17B . . 109.7 ?
C17 C18 H18A . . 109.5 ?
C17 C18 H18B . . 109.5 ?
C17 C18 H18C . . 109.5 ?
H18A C18 H18B . . 109.5 ?
H18A C18 H18C . . 109.5 ?
H18B C18 H18C . . 109.5 ?
C12 C20 H20A . . 109.5 ?
C12 C20 H20B . . 109.5 ?
C12 C20 H20C . . 109.5 ?
H20A C20 H20B . . 109.5 ?
H20A C20 H20C . . 109.5 ?
H20B C20 H20C . . 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
Br1 Zn1 . 2.3523(5) ?
Zn1 O2 . 2.075(2) ?
Zn1 O3 . 2.385(3) ?
Zn1 O4 4_656 1.982(2) ?
Zn1 O5 2_646 2.0182(19) ?
Zn1 C8 . 2.551(3) ?
O1 C7 . 1.374(3) ?
O1 C9 . 1.421(3) ?
O2 C8 . 1.239(5) ?
O3 C8 . 1.234(5) ?
O4 C6 . 1.260(3) ?
O5 C6 . 1.256(3) ?
N1 C10 . 1.520(3) ?
N1 C11 . 1.523(4) ?
N1 C13 . 1.523(3) ?
N1 C16 . 1.521(4) ?
C1 C2 . 1.393(4) ?
C1 C4 . 1.387(4) ?
C1 C6 . 1.496(4) ?
C2 H2 . 0.9300 ?
C2 C7 . 1.379(4) ?
C3 C4 . 1.387(4) ?
C3 C5 . 1.381(4) ?
C3 C8 . 1.508(4) ?
C4 H4 . 0.9300 ?
C5 H5 . 0.9300 ?
C5 C7 . 1.390(4) ?
C9 H9A . 0.9700 ?
C9 H9B . 0.9700 ?
C9 C10 . 1.505(4) ?
C10 H10A . 0.9700 ?
C10 H10B . 0.9700 ?
C11 H11A . 0.9700 ?
C11 H11B . 0.9700 ?
C11 C12 . 1.504(5) ?
C12 H12A . 0.9700 ?
C12 H12B . 0.9700 ?
C12 C20 . 1.512(5) ?
C13 H13A . 0.9700 ?
C13 H13B . 0.9700 ?
C13 C14 . 1.509(4) ?
C14 H14A . 0.9700 ?
C14 H14B . 0.9700 ?
C14 C15 . 1.513(5) ?
C15 H15A . 0.9600 ?
C15 H15B . 0.9600 ?
C15 H15C . 0.9600 ?
C16 H16A . 0.9700 ?
C16 H16B . 0.9700 ?
C16 C17 . 1.509(5) ?
C17 H17A . 0.9700 ?
C17 H17B . 0.9700 ?
C17 C18 . 1.510(5) ?
C18 H18A . 0.9600 ?
C18 H18B . 0.9600 ?
C18 H18C . 0.9600 ?
C20 H20A . 0.9600 ?
C20 H20B . 0.9600 ?
C20 H20C . 0.9600 ?