#------------------------------------------------------------------------------
#$Date: 2025-01-15 04:30:19 +0200 (Wed, 15 Jan 2025) $
#$Revision: 297321 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/02/33/2023354.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_2023354
loop_
_publ_author_name
'Groneck, Erin N.'
'Peek, Nathan'
'Lynch, Will E.'
'Padgett, Clifford W.'
_publ_section_title
;
Crystal structures of zinc(II) coordination complexes with isoquinoline
N-oxide
;
_journal_coeditor_code HB8119
_journal_issue 2
_journal_name_full
'Acta Crystallographica Section E Crystallographic Communications'
_journal_paper_doi 10.1107/S2056989025000180
_journal_volume 81
_journal_year 2025
_chemical_formula_iupac '[Zn (C9 H7 N1 O1)6] (Cl O4)2'
_chemical_formula_moiety 'C54 H42 N6 O6 Zn 2+, 2(Cl O4 -)'
_chemical_formula_sum 'C54 H42 Cl2 N6 O14 Zn'
_chemical_formula_weight 1135.20
_chemical_name_systematic
;
Hexakis(isoquinoline N-oxide-\kO)zinc(II)
bis(perchlorate)
;
_space_group_crystal_system trigonal
_space_group_IT_number 148
_space_group_name_Hall '-R 3'
_space_group_name_H-M_alt 'R -3 :H'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary dual
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 120
_cell_formula_units_Z 3
_cell_length_a 12.8217(4)
_cell_length_b 12.8217(4)
_cell_length_c 26.5684(9)
_cell_measurement_reflns_used 13112
_cell_measurement_temperature 170
_cell_measurement_theta_max 33.0330
_cell_measurement_theta_min 2.3710
_cell_volume 3782.6(2)
_computing_cell_refinement
;
CrysAlisPro 1.171.39.46b (Rigaku OD, 2018)
;
_computing_data_collection
;
CrysAlisPro 1.171.39.46b (Rigaku OD, 2018)
;
_computing_data_reduction
;
CrysAlisPro 1.171.39.46b (Rigaku OD, 2018)
;
_computing_molecular_graphics
;
Olex2 1.5 (Dolomanov et al., 2009)
;
_computing_publication_material
;
Olex2 1.5 (Dolomanov et al., 2009)
;
_computing_structure_refinement
;
SHELXL 2018/3 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT (Sheldrick, 2015a)
;
_diffrn_ambient_temperature 170
_diffrn_detector 'CCD plate'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device 'abstract diffractometer'
_diffrn_measurement_device_type 'XtaLAB Mini'
_diffrn_measurement_method '\w scans'
_diffrn_radiation_monochromator graphite
_diffrn_radiation_probe x-ray
_diffrn_radiation_type 'Mo K\a'
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0174
_diffrn_reflns_av_unetI/netI 0.0086
_diffrn_reflns_limit_h_max 15
_diffrn_reflns_limit_h_min -15
_diffrn_reflns_limit_k_max 15
_diffrn_reflns_limit_k_min -15
_diffrn_reflns_limit_l_max 31
_diffrn_reflns_limit_l_min -31
_diffrn_reflns_number 11238
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 25.342
_diffrn_reflns_theta_min 1.988
_diffrn_source 'fine-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu 0.669
_exptl_absorpt_correction_T_max 1.00000
_exptl_absorpt_correction_T_min 0.91346
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
(CrysAlisPro; Rigaku OD, 2019)
;
_exptl_crystal_colour 'clear colourless'
_exptl_crystal_density_diffrn 1.495
_exptl_crystal_description prism
_exptl_crystal_F_000 1752
_exptl_crystal_size_max 0.2
_exptl_crystal_size_mid 0.2
_exptl_crystal_size_min 0.15
_refine_diff_density_max 0.303
_refine_diff_density_min -0.251
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.063
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 117
_refine_ls_number_reflns 1545
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.063
_refine_ls_R_factor_all 0.0301
_refine_ls_R_factor_gt 0.0277
_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^)+(0.0393P)^2^+4.8988P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0750
_refine_ls_wR_factor_ref 0.0767
_reflns_number_gt 1450
_reflns_number_total 1545
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file hb8119.cif
_cod_data_source_block IV
_cod_original_cell_volume 3782.6(3)
_cod_original_sg_symbol_H-M 'R -3'
_cod_database_code 2023354
_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 0.878
_shelx_estimated_absorpt_t_max 0.906
_shelx_hkl_file
;
0 0 -30 301.766 66.4104 3
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0 0 -27 5410.03 202.646 2
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0 0 -21 614.295 60.6568 3
0 0 -21 648.756 70.0842 2
0 0 -18 6713.42 157.653 3
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0 0 -15 784.466 54.4114 3
0 0 -15 905.984 63.8954 2
0 0 -12 592.766 46.7709 2
0 0 -12 608.166 43.1636 3
0 0 -9 13850.7 156.764 3
0 0 -9 13691.2 172.217 2
0 0 -6 62214.2 293.706 2
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0 0 -3 13690.5 97.3494 2
0 0 -3 13688.9 87.7248 3
0 0 -3 13967.4 79.2195 1
0 0 3 13479.8 79.1847 1
0 0 3 13366.0 88.4669 3
0 0 9 13818.2 141.207 1
0 0 12 652.250 40.0447 1
0 0 15 834.136 47.5092 1
0 0 18 6549.20 140.725 1
0 0 21 732.539 59.7797 1
0 0 24 35270.4 377.393 1
0 0 27 5203.76 158.568 1
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0 1 -28 2238.45 128.027 3
-1 0 -28 2320.61 144.565 2
1 -1 -25 4586.85 156.780 3
1 -1 -25 4762.63 179.355 2
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-11 13 0 1217.97 94.3524 1
-2 -11 3 340.688 59.3275 3
-11 13 3 406.049 66.8393 1
-2 -11 3 411.663 70.8189 2
-11 13 3 334.609 60.9849 3
13 -2 3 175.443 56.9301 1
-2 -11 6 2554.53 131.918 3
-11 13 6 2434.50 139.279 1
-2 -11 6 2649.95 141.930 2
13 -2 6 2871.73 154.854 1
13 -2 9 107.043 55.1398 1
-2 -11 9 206.551 64.1833 3
-11 13 9 90.8099 57.8005 1
-2 -11 9 151.006 58.8470 2
13 -2 12 447.630 78.2019 1
-11 13 12 407.690 87.3336 1
-2 -11 12 484.041 77.9972 2
-1 -12 -10 391.972 84.7633 2
13 -1 -10 437.090 85.2556 1
-12 13 -10 438.929 90.1950 3
13 -1 -7 741.326 103.497 1
-1 -12 -7 769.965 95.9588 2
-12 13 -7 904.291 107.205 3
-1 -12 -4 169.316 66.0240 2
-12 13 -4 96.8948 65.3732 3
13 -1 -4 73.4268 64.6748 1
-1 -12 -1 270.296 65.3284 2
-12 13 -1 268.481 57.9772 1
-12 13 -1 152.695 57.9961 3
13 -1 -1 351.507 77.3869 1
-1 -12 2 743.962 77.4668 3
-12 13 2 767.864 82.2220 1
-1 -12 2 729.482 88.7386 2
13 -1 2 712.348 98.2868 1
-12 13 2 754.310 87.2488 3
-1 -12 5 1013.82 89.4991 3
-12 13 5 969.756 97.4509 1
-1 -12 5 1062.22 102.230 2
13 -1 5 937.194 102.890 1
-12 13 5 882.150 86.3191 3
-12 13 8 2097.11 139.337 1
-1 -12 8 2064.25 130.914 2
13 -1 8 1922.68 133.129 1
-12 13 11 1170.39 116.500 1
-1 -12 11 1031.08 101.122 2
13 -1 11 1032.36 106.842 1
0 -13 -5 1210.35 119.730 2
13 0 -5 1356.25 125.599 1
-13 13 -5 1347.02 122.414 3
0 -13 -2 1055.52 110.710 2
13 0 -2 1371.61 123.970 1
-13 13 -2 1194.26 113.069 3
-13 13 1 2.22264 58.4101 1
0 -13 1-2.24572 61.5331 2
-13 13 1 8.01870 55.2733 3
13 0 1 116.803 66.2168 1
13 0 4-25.0808 61.8738 1
0 -13 4 60.2664 50.2785 3
-13 13 4-14.8079 61.0157 1
0 -13 4 16.0469 58.0627 2
-13 13 4-3.51574 53.0632 3
0 -13 7 1514.88 125.595 2
13 0 7 1777.40 137.173 1
-13 13 7 1779.97 135.939 1
14 -12 -4 681.459 89.8968 1
14 -12 -4 788.728 90.4386 2
-2 14 -4 648.536 83.5220 1
-12 -2 -4 663.504 94.7808 3
14 -12 -1 194.610 61.2920 1
14 -12 -1 203.749 62.9620 2
-2 14 -1 266.819 66.5604 1
-12 -2 -1 250.879 73.7423 3
-12 -2 2 470.576 90.6503 3
-2 14 2 392.289 76.2438 1
14 -12 2 348.918 69.4980 1
14 -12 2 479.366 76.3205 2
-2 14 5 3295.34 176.610 1
14 -12 5 3029.81 163.868 2
-12 -2 5 3282.83 185.723 3
14 -11 -8-15.0579 65.4037 1
-3 14 -8 53.2317 65.7009 3
-11 -3 -8 57.7595 63.8106 3
14 -11 -5 2171.33 144.085 1
-3 14 -5 2276.57 125.419 1
14 -11 -5 2300.40 126.988 2
-3 14 -5 2326.99 134.365 3
-11 -3 -5 2508.07 146.565 3
14 -11 -2 1301.90 110.407 1
-3 14 -2 1313.97 103.561 1
14 -11 -2 1550.27 106.214 2
-11 -3 -2 1371.15 120.312 3
14 -11 1 1578.18 113.740 1
-3 14 1 1450.63 111.894 1
14 -11 1 1893.53 119.078 2
-11 -3 1 1839.11 136.017 3
-11 -3 4 52.9398 61.9378 3
-3 14 4-19.7737 56.3234 1
14 -11 4-16.4485 45.8147 1
14 -11 4 27.6317 50.8497 2
-11 -3 7 64.9293 74.5219 3
-3 14 7 194.755 72.4223 1
14 -11 7 73.3651 56.5100 2
14 -10 -9 54.3861 62.7672 1
-4 14 -9-63.3391 57.0041 3
-10 -4 -9-20.1769 55.4369 3
14 -10 -6 86.6680 56.1042 1
-4 14 -6 173.385 60.1150 3
-4 14 -6 160.356 55.4699 1
-10 -4 -6 231.814 66.2902 3
14 -10 -3 2112.24 136.942 1
-4 14 -3 2095.12 120.842 1
14 -10 -3 2046.98 111.382 2
-4 14 -3 1958.62 115.154 3
-10 -4 -3 2130.92 137.190 3
14 -10 0 6472.83 211.693 1
-4 14 0 6643.56 212.464 1
14 -10 0 6227.49 189.852 2
-10 -4 0 6891.96 235.400 3
14 -10 3 1515.41 105.375 1
14 -10 3 1599.62 106.458 2
-4 14 3 1520.43 117.617 1
-10 -4 3 1611.06 125.662 3
-10 -4 6 374.182 80.3527 3
-4 14 6 316.202 71.7764 1
14 -10 6 352.801 69.4939 2
-10 -4 9 137.623 73.4741 3
-4 14 9 31.9238 65.8155 1
14 -10 9 49.7633 58.7348 2
14 -9 -10 106.244 61.4450 1
-5 14 -10 205.366 68.6177 3
-9 -5 -10 140.701 57.5741 3
14 -9 -7 139.381 60.9995 1
-5 14 -7 88.2029 56.4399 3
-9 -5 -7 76.4602 51.6200 3
-9 -5 -4 703.995 84.9904 3
-5 14 -4 785.191 76.5871 1
14 -9 -4 756.226 88.9716 1
-5 14 -4 728.076 80.2409 3
14 -9 -1 1346.43 106.136 1
-5 14 -1 1344.79 101.101 1
-9 -5 -1 1539.69 118.350 3
-9 -5 2-56.9985 59.3674 3
14 -9 2 16.4363 51.8044 1
-5 14 2 106.755 54.1368 1
14 -9 2 61.5051 49.3584 2
-9 -5 5 556.426 89.5277 3
14 -9 5 609.552 75.2861 1
-5 14 5 660.147 83.5871 1
14 -9 5 440.534 69.1512 2
14 -9 8 2590.96 132.783 2
-5 14 8 2839.29 159.902 1
-9 -5 8 3056.55 167.582 3
14 -9 11 711.405 88.3675 2
-5 14 11 881.079 110.279 1
-9 -5 11 731.808 99.8374 3
14 -8 -11-68.0920 61.6599 1
-6 14 -11-65.6803 65.0243 3
-8 -6 -11-37.8965 53.4292 3
14 -8 -8 2868.08 158.540 1
-6 14 -8 2409.63 140.398 3
-8 -6 -8 2851.81 138.541 3
14 -8 -5 4203.50 184.801 1
-6 14 -5 3889.53 166.920 3
-8 -6 -5 4375.86 171.154 3
14 -8 -2 1751.26 120.457 1
-6 14 -2 1409.75 98.9821 3
-6 14 -2 1685.50 106.155 1
-8 -6 -2 1595.79 112.750 3
-8 -6 1 360.224 73.2141 3
14 -8 1 405.141 69.0708 1
-6 14 1 437.439 69.6651 1
-8 -6 4 497.395 81.4793 3
14 -8 4 605.637 72.5926 1
-6 14 4 540.904 78.3164 1
14 -8 7 1503.39 103.908 1
14 -8 7 1483.99 100.827 2
-6 14 7 1460.46 117.196 1
-8 -6 7 1607.28 121.048 3
-6 14 10 1778.56 135.570 1
14 -8 10 1651.58 111.172 2
-8 -6 10 1592.45 129.093 3
-8 -6 13 1113.06 115.396 3
-6 14 13 1248.95 127.141 1
14 -8 13 1112.86 103.839 2
-7 -7 -12 233.655 62.3273 2
14 -7 -12 298.413 75.3866 1
-7 14 -12 365.881 82.0100 3
-7 -7 -9 1239.49 94.4749 2
14 -7 -9 1159.58 112.472 1
-7 14 -9 1198.26 107.116 3
-7 -7 -9 1335.48 97.4893 3
-7 -7 -6 386.646 66.5669 3
14 -7 -6 372.450 66.4845 1
-7 14 -6 506.277 75.8571 3
14 -7 -3 2121.44 134.383 1
-7 14 -3 1785.63 114.137 3
-7 14 -3 2109.81 110.681 1
-7 -7 -3 2106.89 123.782 3
14 -7 0 3232.78 152.902 1
-7 14 0 3257.41 143.281 1
-7 -7 0 3450.12 157.653 3
-7 -7 3 127.265 56.8656 3
-7 14 3 184.751 69.1032 1
14 -7 3 24.7300 45.1762 1
14 -7 6 675.371 79.0938 1
-7 14 6 643.687 83.7233 1
-7 -7 6 711.502 90.6372 3
-7 -7 9 2889.37 156.911 3
-7 14 9 3042.92 166.376 1
14 -7 9 2727.78 132.589 1
14 -7 9 2787.05 132.690 2
-7 -7 12-86.1632 67.2980 3
-7 14 12 72.7620 62.6222 1
14 -7 12 17.7735 54.2151 2
-6 -8 -13-28.2370 58.5415 2
14 -6 -13 63.8585 69.6736 1
-8 14 -13-30.8590 63.5366 3
-6 -8 -10 1334.60 105.780 2
14 -6 -10 1382.98 122.348 1
-8 14 -10 1188.57 112.638 3
-6 -8 -7 1450.40 103.866 2
14 -6 -7 1399.56 115.616 1
-8 14 -7 1507.58 114.220 3
-6 -8 -7 1366.20 95.7615 3
-6 -8 -4 50.3714 47.5448 3
-6 -8 -4-33.6268 47.4841 2
14 -6 -4 32.2737 56.1237 1
-8 14 -4 33.4290 53.2978 3
14 -6 -1 1258.67 104.710 1
-8 14 -1 1265.05 95.7314 3
-8 14 -1 1347.82 97.6438 1
-6 -8 -1 1257.14 98.7389 3
-6 -8 2 446.610 72.6539 3
-8 14 2 461.754 75.6292 1
14 -6 2 386.600 70.9703 1
-6 -8 5 453.870 74.0547 3
14 -6 5 333.469 64.7302 1
-8 14 5 432.088 78.7846 1
-6 -8 8 10404.7 279.165 3
-8 14 8 10236.1 291.098 1
14 -6 8 9825.67 247.143 1
-6 -8 11 133.042 67.7925 3
-8 14 11 86.2006 65.8920 1
14 -6 11 22.0954 51.8313 1
-5 -9 -11 575.162 83.6951 2
14 -5 -11 442.138 85.6543 1
-9 14 -11 435.973 86.9866 3
-5 -9 -8 438.772 71.3169 2
14 -5 -8 345.360 73.1140 1
-9 14 -8 528.324 83.0002 3
-5 -9 -5 3275.27 146.867 2
14 -5 -5 3412.88 169.484 1
-9 14 -5 3071.29 153.912 3
-5 -9 -5 3503.73 142.126 3
-9 14 -2 1742.32 107.361 1
-5 -9 -2 1697.20 106.348 2
14 -5 -2 1537.30 122.757 1
-9 14 -2 1365.76 102.895 3
-5 -9 -2 1676.49 104.314 3
-5 -9 1 189.071 58.8388 3
14 -5 1 51.6794 53.7058 1
-9 14 1 7.58944 50.0523 1
-5 -9 4 199.627 58.9062 3
-9 14 4 144.692 60.9686 1
14 -5 4 163.112 59.4333 1
-5 -9 7 696.367 88.1504 3
-9 14 7 595.438 88.9453 1
14 -5 7 622.622 83.0398 1
-5 -9 10 265.414 71.3874 3
-9 14 10 82.4575 70.9808 1
14 -5 10 246.690 66.5163 1
-4 -10 -9-26.0976 57.9829 2
14 -4 -9 101.722 63.7669 1
-10 14 -9-3.95280 68.3845 3
-4 -10 -6 56.6978 54.5044 2
14 -4 -6 18.3079 59.8625 1
-10 14 -6 9.35742 55.3831 3
-4 -10 -3 2984.63 144.945 2
14 -4 -3 3002.54 163.605 1
-10 14 -3 2760.64 145.435 3
-4 -10 -3 2943.68 131.773 3
-4 -10 0 1116.30 89.5074 2
-10 14 0 1171.72 96.2553 1
14 -4 0 1153.74 107.624 1
-10 14 0 1210.68 96.6016 3
-4 -10 0 1002.87 93.2423 3
-4 -10 3 1311.45 104.807 3
-4 -10 3 1194.97 90.7412 2
14 -4 3 1228.73 107.637 1
-10 14 3 1480.50 112.060 1
-4 -10 6 138.239 57.4593 3
-10 14 6 96.2670 62.4656 1
14 -4 6 106.777 54.9294 1
-4 -10 9 208.925 64.0336 3
-10 14 9 217.261 69.5321 1
14 -4 9 140.845 59.1688 1
-3 -11 -7-38.2672 57.2851 2
14 -3 -7-28.1918 63.0181 1
-11 14 -7 15.5071 59.5979 3
-3 -11 -4 548.778 81.0252 2
-11 14 -4 538.747 87.8103 3
14 -3 -4 435.469 85.1716 1
-3 -11 -1-56.6875 48.2690 3
-3 -11 -1 19.4140 51.2021 2
-11 14 -1 15.3218 46.9317 1
-11 14 -1 30.4717 55.8372 3
14 -3 -1-65.4465 64.0928 1
-3 -11 2 579.054 74.9103 3
-3 -11 2 773.316 89.7015 2
-11 14 2 481.068 77.4451 1
14 -3 2 647.196 89.9568 1
-3 -11 5 1588.49 112.759 3
-3 -11 5 1627.63 114.578 2
14 -3 5 1625.14 126.338 1
-11 14 5 1638.95 122.302 1
-3 -11 8 1359.50 108.074 3
14 -3 8 1347.37 115.408 1
-11 14 8 1508.53 122.766 1
-2 -12 -5 277.302 73.9196 2
-12 14 -5 379.360 83.7517 3
14 -2 -5 396.727 84.1289 1
-2 -12 -2 943.369 99.8726 2
-12 14 -2 890.303 102.425 3
14 -2 -2 746.289 97.0625 1
-12 14 1 2.20398 50.9067 1
-2 -12 1 210.583 69.6360 2
-12 14 1 270.671 73.6191 3
14 -2 1 138.118 64.6266 1
-2 -12 4 105.886 53.9359 3
-12 14 4 27.3350 55.0570 1
-2 -12 4 128.054 61.2289 2
14 -2 4 11.8959 65.3740 1
-10 -5 -2-5.10189 56.5743 3
-5 15 -2-7.81823 53.6162 1
15 -10 -2 132.756 67.9080 1
15 -10 1 1617.32 120.380 1
-5 15 1 1820.08 126.549 1
-10 -5 1 2013.54 141.385 3
-10 -5 4 130.097 71.7861 3
15 -10 4-9.84715 51.0508 1
-5 15 4 107.259 64.0329 1
15 -9 -6 297.179 77.4091 1
-6 15 -6 301.580 71.0277 3
-9 -6 -6 293.831 69.5738 3
-9 -6 -3 387.521 74.3072 3
-6 15 -3 290.650 61.6127 1
15 -9 -3 484.037 80.0089 1
15 -9 0 3472.29 165.652 1
-6 15 0 3776.35 163.435 1
-9 -6 0 3670.93 176.162 3
-9 -6 3 113.766 69.8465 3
15 -9 3 153.843 54.0889 1
-6 15 3 90.1530 60.2699 1
15 -9 6 910.892 89.6780 1
-6 15 6 1102.60 112.123 1
-9 -6 6 1129.50 112.878 3
15 -8 -7 1116.51 112.930 1
-7 15 -7 955.676 101.518 3
-8 -7 -7 873.794 90.8579 3
-8 -7 -4 21.4544 51.8647 3
15 -8 -4 108.053 61.9345 1
-7 15 -4 137.382 57.7443 3
-8 -7 -1 141.151 58.1924 3
15 -8 -1 276.594 71.0767 1
-7 15 -1 147.386 52.9315 1
-8 -7 2 36.9742 59.5728 3
15 -8 2 138.802 57.8623 1
-7 15 2-22.2867 54.0148 1
-7 15 5 310.422 73.4834 1
-8 -7 5 289.875 75.9386 3
15 -8 5 358.151 76.9930 1
15 -7 -5 2285.23 147.088 1
-8 15 -5 2060.35 132.199 3
-7 -8 -5 2286.69 131.148 3
-7 -8 -2 504.423 77.1296 3
15 -7 -2 583.786 82.6882 1
-8 15 1 156.504 58.6153 1
-7 -8 1 108.275 60.3100 3
15 -7 1 97.5780 59.4577 1
-8 15 4 713.088 88.9232 1
15 -7 4 1003.96 98.3702 1
-7 -8 4 877.137 97.5339 3
-8 15 7 3814.84 185.690 1
15 -7 7 3929.11 168.121 1
-7 -8 7 3678.04 176.797 3
15 -6 -6 1402.19 127.287 1
-9 15 -6 1351.17 115.425 3
15 -6 -3 704.400 96.8496 1
-9 15 -3 687.275 87.6902 3
-6 -9 -3 786.786 85.8650 3
15 -6 0 1483.05 120.091 1
-6 -9 0 1513.02 113.675 3
-9 15 0 1419.81 107.932 1
-6 -9 3 179.292 64.1842 3
-9 15 3 276.462 68.2022 1
15 -6 3 200.779 59.5211 1
-9 15 6 1530.32 126.859 1
15 -6 6 1435.33 113.948 1
-6 -9 6 1523.35 117.161 3
15 -5 -4 1648.26 132.140 1
-10 15 -4 1615.12 118.911 3
-5 -10 -1 66.9143 51.0429 3
15 -5 -1 66.6447 59.4929 1
15 -5 2 566.582 86.1980 1
-5 -10 2 535.029 85.6091 3
-10 15 2 481.403 76.4602 1
0 0 0 0.00 0.00 0
TITL X117_NP(2) in R3
REM R3 (#146 in standard setting)
CELL 0.71073 12.821749 12.821749 26.568395 90.0000 90.0000 120.0000
ZERR 17.00 0.000400 0.000400 0.000913 0.0000 0.0000 0.0000
LATT -3
SYMM -y, x-y, z
SYMM -x+y,-x, z
SFAC C H N O
UNIT 187.00 170.00 17.00 17.00
TREF
HKLF 4
END
;
_shelx_hkl_checksum 35488
_shelx_res_file
;
TITL x117_np(2)_a.res in R-3
x117_np(2).res
created by SHELXL-2018/3 at 13:36:10 on 01-Nov-2024
REM Old TITL X117_NP(2) in R3
REM SHELXT solution in R-3
REM R1 0.229, Rweak 0.015, Alpha 0.027, Orientation as input
REM Formula found by SHELXT: C62 N8 O6 Br
CELL 0.71073 12.8217 12.8217 26.5684 90 90 120
ZERR 3 0.0004 0.0004 0.0009 0 0 0
LATT 3
SYMM -Y,+X-Y,+Z
SYMM +Y-X,-X,+Z
SFAC C H Cl N O Zn
UNIT 162 126 6 18 42 3
L.S. 10
PLAN 5
SIZE 0.15 0.2 0.2
TEMP -103.15
CONF
BOND $H
list 4
fmap 2
acta
MORE -1
REM
REM
REM
WGHT 0.039300 4.898800
FVAR 1.35693
C1 1 0.578122 0.424648 0.460486 11.00000 0.03006 0.03003 =
0.03536 0.00212 0.00419 0.01769
AFIX 43
H1 2 0.516846 0.343592 0.466025 11.00000 -1.20000
AFIX 0
N1 4 0.612674 0.462729 0.413834 11.00000 0.03192 0.03229 =
0.03085 -0.00150 0.00126 0.01827
O1 5 0.562347 0.386245 0.375523 11.00000 0.03609 0.04088 =
0.03146 -0.00741 -0.00163 0.01914
ZN1 6 0.666667 0.333333 0.333333 10.16667 0.03368 0.03368 =
0.02476 0.00000 0.00000 0.01684
C2 1 0.630250 0.501697 0.502000 11.00000 0.03518 0.03668 =
0.03334 -0.00084 0.00120 0.02514
C3 1 0.597634 0.459639 0.552157 11.00000 0.05094 0.04990 =
0.03551 0.00279 0.00413 0.03642
AFIX 43
H3 2 0.538797 0.378022 0.558427 11.00000 -1.20000
AFIX 0
C4 1 0.651650 0.537645 0.591437 11.00000 0.07049 0.07642 =
0.03398 -0.00488 -0.00390 0.05601
AFIX 43
H4 2 0.630487 0.509631 0.625046 11.00000 -1.20000
AFIX 0
C5 1 0.738276 0.658999 0.582449 11.00000 0.06699 0.06995 =
0.04668 -0.02486 -0.01798 0.04569
AFIX 43
H5 2 0.774576 0.711886 0.610150 11.00000 -1.20000
AFIX 0
C6 1 0.770926 0.701867 0.534666 11.00000 0.04661 0.04473 =
0.05987 -0.01830 -0.01026 0.02629
AFIX 43
H6 2 0.829315 0.784090 0.529361 11.00000 -1.20000
AFIX 0
C7 1 0.718064 0.624196 0.492883 11.00000 0.03565 0.03574 =
0.04391 -0.00588 -0.00196 0.02259
C8 1 0.748359 0.660400 0.442058 11.00000 0.03792 0.02894 =
0.05059 0.00219 0.00525 0.01634
AFIX 43
H8 2 0.805433 0.741987 0.434702 11.00000 -1.20000
AFIX 0
C9 1 0.697559 0.581008 0.403864 11.00000 0.03946 0.03424 =
0.03830 0.00721 0.00806 0.01983
AFIX 43
H9 2 0.720339 0.606689 0.370095 11.00000 -1.20000
AFIX 0
CL1 3 1.000000 1.000000 0.384856 10.33333 0.04185 0.04185 =
0.03428 0.00000 0.00000 0.02093
O2 5 1.000000 1.000000 0.438967 10.33333 0.07980 0.07980 =
0.03260 0.00000 0.00000 0.03990
O3 5 0.935302 0.880660 0.367305 11.00000 0.14785 0.05073 =
0.06551 -0.01100 -0.03384 0.01986
HKLF 4
REM x117_np(2)_a.res in R-3
REM wR2 = 0.0767, GooF = S = 1.063, Restrained GooF = 1.063 for all data
REM R1 = 0.0277 for 1450 Fo > 4sig(Fo) and 0.0301 for all 1545 data
REM 117 parameters refined using 0 restraints
END
WGHT 0.0391 4.9047
REM Highest difference peak 0.303, deepest hole -0.251, 1-sigma level 0.039
Q1 1 0.8829 0.9210 0.3677 11.00000 0.05 0.30
Q2 1 1.0145 0.9125 0.3746 11.00000 0.05 0.22
Q3 1 0.9986 0.9091 0.3470 11.00000 0.05 0.20
Q4 1 0.6747 0.5662 0.4989 11.00000 0.05 0.19
Q5 1 0.7479 0.6548 0.5136 11.00000 0.05 0.19
;
_shelx_res_checksum 56771
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
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
C C1 0.57812(14) 0.42465(14) 0.46049(6) 0.0306(3) Uani d 1 . .
H H1 0.516846 0.343592 0.466025 0.037 Uiso calc 1 . .
N N1 0.61267(12) 0.46273(12) 0.41383(5) 0.0307(3) Uani d 1 . .
O O1 0.56235(10) 0.38624(11) 0.37552(4) 0.0362(3) Uani d 1 . .
Zn Zn1 0.666667 0.333333 0.333333 0.03070(15) Uani d 1 . .
C C2 0.63025(14) 0.50170(15) 0.50200(6) 0.0319(4) Uani d 1 . .
C C3 0.59763(17) 0.45964(18) 0.55216(6) 0.0405(4) Uani d 1 . .
H H3 0.538797 0.378022 0.558427 0.049 Uiso calc 1 . .
C C4 0.6517(2) 0.5376(2) 0.59144(7) 0.0517(5) Uani d 1 . .
H H4 0.630487 0.509631 0.625046 0.062 Uiso calc 1 . .
C C5 0.7383(2) 0.6590(2) 0.58245(8) 0.0561(6) Uani d 1 . .
H H5 0.774576 0.711886 0.610150 0.067 Uiso calc 1 . .
C C6 0.77093(18) 0.70187(19) 0.53467(8) 0.0489(5) Uani d 1 . .
H H6 0.829315 0.784090 0.529361 0.059 Uiso calc 1 . .
C C7 0.71806(15) 0.62420(15) 0.49288(7) 0.0363(4) Uani d 1 . .
C C8 0.74836(16) 0.66040(15) 0.44206(7) 0.0393(4) Uani d 1 . .
H H8 0.805433 0.741987 0.434702 0.047 Uiso calc 1 . .
C C9 0.69756(16) 0.58101(15) 0.40386(7) 0.0367(4) Uani d 1 . .
H H9 0.720339 0.606689 0.370095 0.044 Uiso calc 1 . .
Cl Cl1 1.000000 1.000000 0.38486(3) 0.03933(19) Uani d 1 . .
O O2 1.000000 1.000000 0.43897(9) 0.0641(7) Uani d 1 . .
O O3 0.9353(2) 0.88066(16) 0.36730(7) 0.1013(8) 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
C1 0.0301(8) 0.0300(8) 0.0354(8) 0.0177(7) 0.0042(6) 0.0021(6)
N1 0.0319(7) 0.0323(7) 0.0308(7) 0.0183(6) 0.0013(5) -0.0015(5)
O1 0.0361(6) 0.0409(7) 0.0315(6) 0.0191(5) -0.0016(5) -0.0074(5)
Zn1 0.03368(18) 0.03368(18) 0.0248(2) 0.01684(9) 0.000 0.000
C2 0.0352(8) 0.0367(9) 0.0333(8) 0.0251(7) 0.0012(6) -0.0008(7)
C3 0.0509(10) 0.0499(10) 0.0355(9) 0.0364(9) 0.0041(8) 0.0028(8)
C4 0.0705(14) 0.0764(15) 0.0340(9) 0.0560(13) -0.0039(9) -0.0049(9)
C5 0.0670(14) 0.0700(14) 0.0467(11) 0.0457(12) -0.0180(10) -0.0249(10)
C6 0.0466(11) 0.0447(11) 0.0599(13) 0.0263(9) -0.0103(9) -0.0183(9)
C7 0.0356(9) 0.0357(9) 0.0439(10) 0.0226(7) -0.0020(7) -0.0059(7)
C8 0.0379(9) 0.0289(8) 0.0506(10) 0.0163(7) 0.0052(8) 0.0022(7)
C9 0.0395(9) 0.0342(9) 0.0383(9) 0.0198(8) 0.0081(7) 0.0072(7)
Cl1 0.0419(3) 0.0419(3) 0.0343(4) 0.02093(13) 0.000 0.000
O2 0.0798(12) 0.0798(12) 0.0326(13) 0.0399(6) 0.000 0.000
O3 0.148(2) 0.0507(10) 0.0655(11) 0.0199(11) -0.0338(12) -0.0110(8)
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'
Cl Cl 0.1484 0.1585 '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'
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
N1 C1 H1 . . 119.3 ?
N1 C1 C2 . . 121.39(15) ?
C2 C1 H1 . . 119.3 ?
C1 N1 O1 . . 119.54(13) ?
C1 N1 C9 . . 121.29(14) ?
O1 N1 C9 . . 119.15(13) ?
N1 O1 Zn1 . . 119.49(9) ?
O1 Zn1 O1 17 3_665 85.82(4) ?
O1 Zn1 O1 18_545 2_655 85.82(4) ?
O1 Zn1 O1 18_545 3_665 180.0 ?
O1 Zn1 O1 16_655 . 180.00(6) ?
O1 Zn1 O1 16_655 3_665 85.82(4) ?
O1 Zn1 O1 17 . 85.82(4) ?
O1 Zn1 O1 3_665 . 94.18(4) ?
O1 Zn1 O1 2_655 3_665 94.18(4) ?
O1 Zn1 O1 16_655 18_545 94.18(4) ?
O1 Zn1 O1 18_545 . 85.82(4) ?
O1 Zn1 O1 16_655 17 94.18(4) ?
O1 Zn1 O1 2_655 . 94.18(4) ?
O1 Zn1 O1 18_545 17 94.18(4) ?
O1 Zn1 O1 16_655 2_655 85.82(4) ?
O1 Zn1 O1 17 2_655 180.0 ?
C1 C2 C3 . . 121.52(16) ?
C1 C2 C7 . . 118.53(15) ?
C3 C2 C7 . . 119.95(16) ?
C2 C3 H3 . . 120.3 ?
C4 C3 C2 . . 119.50(19) ?
C4 C3 H3 . . 120.3 ?
C3 C4 H4 . . 119.7 ?
C3 C4 C5 . . 120.60(19) ?
C5 C4 H4 . . 119.7 ?
C4 C5 H5 . . 119.4 ?
C6 C5 C4 . . 121.12(18) ?
C6 C5 H5 . . 119.4 ?
C5 C6 H6 . . 119.9 ?
C5 C6 C7 . . 120.2(2) ?
C7 C6 H6 . . 119.9 ?
C6 C7 C2 . . 118.61(17) ?
C6 C7 C8 . . 124.03(17) ?
C8 C7 C2 . . 117.36(15) ?
C7 C8 H8 . . 119.4 ?
C9 C8 C7 . . 121.24(16) ?
C9 C8 H8 . . 119.4 ?
N1 C9 H9 . . 119.9 ?
C8 C9 N1 . . 120.12(16) ?
C8 C9 H9 . . 119.9 ?
O3 Cl1 O2 2_765 . 109.37(8) ?
O3 Cl1 O2 3_675 . 109.37(8) ?
O3 Cl1 O2 . . 109.37(8) ?
O3 Cl1 O3 . 3_675 109.58(8) ?
O3 Cl1 O3 2_765 . 109.58(8) ?
O3 Cl1 O3 2_765 3_675 109.57(8) ?
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
C1 H1 . 0.9500 ?
C1 N1 . 1.325(2) ?
C1 C2 . 1.407(2) ?
N1 O1 . 1.3346(17) ?
N1 C9 . 1.380(2) ?
O1 Zn1 . 2.1008(11) ?
C2 C3 . 1.420(2) ?
C2 C7 . 1.423(2) ?
C3 H3 . 0.9500 ?
C3 C4 . 1.370(3) ?
C4 H4 . 0.9500 ?
C4 C5 . 1.408(3) ?
C5 H5 . 0.9500 ?
C5 C6 . 1.363(3) ?
C6 H6 . 0.9500 ?
C6 C7 . 1.417(3) ?
C7 C8 . 1.418(3) ?
C8 H8 . 0.9500 ?
C8 C9 . 1.352(3) ?
C9 H9 . 0.9500 ?
Cl1 O2 . 1.438(2) ?
Cl1 O3 3_675 1.4063(18) ?
Cl1 O3 2_765 1.4062(18) ?
Cl1 O3 . 1.4063(18) ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
C1 N1 O1 Zn1 . . . . -112.28(13) ?
C1 N1 C9 C8 . . . . 0.8(2) ?
C1 C2 C3 C4 . . . . 179.35(15) ?
C1 C2 C7 C6 . . . . -179.82(15) ?
C1 C2 C7 C8 . . . . -0.7(2) ?
N1 C1 C2 C3 . . . . -176.87(15) ?
N1 C1 C2 C7 . . . . 2.8(2) ?
O1 N1 C9 C8 . . . . 179.02(15) ?
C2 C1 N1 O1 . . . . 178.91(13) ?
C2 C1 N1 C9 . . . . -2.9(2) ?
C2 C3 C4 C5 . . . . 0.5(3) ?
C2 C7 C8 C9 . . . . -1.3(2) ?
C3 C2 C7 C6 . . . . -0.2(2) ?
C3 C2 C7 C8 . . . . 178.97(15) ?
C3 C4 C5 C6 . . . . -0.2(3) ?
C4 C5 C6 C7 . . . . -0.2(3) ?
C5 C6 C7 C2 . . . . 0.4(3) ?
C5 C6 C7 C8 . . . . -178.66(18) ?
C6 C7 C8 C9 . . . . 177.79(17) ?
C7 C2 C3 C4 . . . . -0.3(2) ?
C7 C8 C9 N1 . . . . 1.3(3) ?
C9 N1 O1 Zn1 . . . . 69.45(16) ?