#------------------------------------------------------------------------------
#$Date: 2023-08-24 04:44:14 +0300 (Thu, 24 Aug 2023) $
#$Revision: 285855 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/02/28/2022842.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_2022842
loop_
_publ_author_name
'Andriichuk, Irina L.'
'Shova, Sergiu'
'Lampeka, Yaroslaw D.'
_publ_section_title
;
Crystal structures of the complexes containing macrocyclic cations
[M(cyclam)]2+ (M = Ni, Zn) and tetraiodidocadmate(2--) anion
;
_journal_coeditor_code EX2074
_journal_issue 9
_journal_name_full
'Acta Crystallographica Section E Crystallographic Communications'
_journal_paper_doi 10.1107/S2056989023007004
_journal_volume 79
_journal_year 2023
_chemical_formula_iupac '[Ni (C10 H24 N4)] [Cd I4]'
_chemical_formula_moiety 'C10 H24 N4 Ni 2+, Cd I4 2-'
_chemical_formula_sum 'C10 H24 Cd I4 N4 Ni'
_chemical_formula_weight 879.04
_chemical_name_systematic
;
(1,4,8,11-Tetraazacyclotetradecane-\k^4^N)nickel(II)
tetraiodidocadmate(II)
;
_space_group_crystal_system orthorhombic
_space_group_IT_number 62
_space_group_name_Hall '-P 2ac 2n'
_space_group_name_H-M_alt 'P n m a'
_atom_sites_solution_hydrogens mixed
_atom_sites_solution_primary dual
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_formula_units_Z 4
_cell_length_a 15.4317(3)
_cell_length_b 17.2945(3)
_cell_length_c 7.98733(15)
_cell_measurement_reflns_used 5956
_cell_measurement_temperature 199.95(10)
_cell_measurement_theta_max 28.7630
_cell_measurement_theta_min 2.3480
_cell_volume 2131.69(7)
_computing_cell_refinement
;
CrysAlisPro (Rigaku OD, 2022)
;
_computing_data_collection
;
CrysAlisPro (Rigaku OD, 2022)
;
_computing_data_reduction
;
CrysAlisPro (Rigaku OD, 2022)
;
_computing_molecular_graphics
;
Mercury (Macrae et al., 2020)
;
_computing_publication_material
;
publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL2018/3 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT (Sheldrick, 2015a)
;
_diffrn_ambient_temperature 199.95(10)
_diffrn_detector 'CCD plate'
_diffrn_detector_area_resol_mean 16.1593
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.965
_diffrn_measurement_device 'four-circle diffractometer'
_diffrn_measurement_device_type 'Rigaku Xcalibur Eos'
_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 0.0435
_diffrn_reflns_av_unetI/netI 0.0338
_diffrn_reflns_limit_h_max 19
_diffrn_reflns_limit_h_min -19
_diffrn_reflns_limit_k_max 23
_diffrn_reflns_limit_k_min -23
_diffrn_reflns_limit_l_max 10
_diffrn_reflns_limit_l_min -10
_diffrn_reflns_number 16993
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 28.282
_diffrn_reflns_theta_min 2.355
_diffrn_source 'fine-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu 7.671
_exptl_absorpt_correction_T_max 1.00000
_exptl_absorpt_correction_T_min 0.57317
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
(CrysAlisPro; Rigaku OD, 2022)
;
_exptl_crystal_colour 'clear dark orange'
_exptl_crystal_density_diffrn 2.739
_exptl_crystal_description prism
_exptl_crystal_F_000 1600
_exptl_crystal_size_max 0.1
_exptl_crystal_size_mid 0.05
_exptl_crystal_size_min 0.03
_refine_diff_density_max 2.574
_refine_diff_density_min -1.233
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.062
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 97
_refine_ls_number_reflns 2644
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.062
_refine_ls_R_factor_all 0.0429
_refine_ls_R_factor_gt 0.0314
_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^)+(0.0237P)^2^+2.5375P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0586
_refine_ls_wR_factor_ref 0.0636
_reflns_number_gt 2204
_reflns_number_total 2644
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file ex2074sup1.cif
_cod_data_source_block I
_cod_database_code 2022842
_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 0.514
_shelx_estimated_absorpt_t_max 0.803
_shelx_hkl_file
;
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0 0 -1 106.476 95.0315 9
0 0 -1 139.748 61.1352 5
0 0 1 364.272 90.4460 5
0 0 -2 460828. 3420.15 4
0 0 2 462769. 3534.31 4
0 0 -2 464392. 4456.40 9
0 0 2 474975. 4449.63 9
0 0 2 459014. 3733.25 5
0 0 3 2.14744 107.170 4
0 0 -3 137.896 101.465 4
0 0 3-3.30125 112.003 9
0 0 -3 114.972 187.538 9
0 0 3 165.173 163.635 5
0 0 4 123759. 2613.72 4
0 0 -4 124960. 2496.26 4
0 0 -4 123506. 3296.00 9
0 0 4 121561. 2764.60 5
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0 0 -5-101.019 169.745 9
0 0 5 240.384 173.433 5
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0 0 -6 20997.8 1670.89 9
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0 0 -7-185.713 254.779 9
0 0 7-145.342 265.656 5
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0 1 -1 92000.3 1004.99 5
0 -1 1 91023.7 1008.57 5
0 1 1 92744.9 1350.04 5
0 1 -2 363.091 118.295 4
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0 1 -4 190.502 113.223 4
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0 -2 0 74049.0 1087.43 3
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-17 11 -2-55.5645 321.357 7
-17 -11 -2-185.736 360.855 7
-17 -11 -2 184.016 326.428 6
-17 -11 -3 2046.07 610.977 6
-17 12 0-17.0180 259.063 7
-17 12 -1 8.00452 202.756 7
18 0 0 4225.89 1083.71 3
-18 0 0 4787.31 902.720 7
18 0 -1 1124.83 558.400 3
18 0 1 571.526 388.904 3
-18 0 1 1007.28 500.161 7
-18 0 -1 1217.65 514.333 7
18 0 -2 3707.06 965.828 3
18 0 2 4155.14 1073.30 3
-18 0 2 3655.66 821.256 7
18 0 -3 641.142 445.874 3
18 0 3 552.135 331.057 3
18 0 -4 31203.8 2725.56 3
18 0 4 29559.5 2625.47 3
18 0 -5 96.0747 392.071 3
18 0 5 2535.95 831.642 3
18 1 0 3238.93 958.901 3
18 -1 0 3413.38 979.512 3
-18 1 0 2797.23 699.729 7
-18 -1 0 3404.29 768.794 7
18 1 -1 1265.18 659.787 3
18 1 1 157.141 360.084 3
18 -1 -1-255.458 418.732 3
18 -1 1 158.768 293.340 3
-18 1 1 780.000 429.582 7
-18 -1 1 749.416 431.991 7
-18 1 -1 834.294 434.384 7
-18 -1 -1 610.554 349.066 7
18 1 -2 3387.35 962.139 3
18 1 2 3488.53 977.823 3
18 -1 -2 4960.64 1143.77 3
18 -1 2 2357.02 831.781 3
-18 1 -2 2912.13 732.703 7
-18 1 2 3592.37 822.983 7
-18 -1 2 3123.95 763.594 7
18 1 -3 3497.05 960.898 3
18 1 3 3628.22 966.629 3
18 -1 -3 4950.54 1145.13 3
18 -1 3 4291.93 1033.83 3
18 1 -4 19.9441 353.656 3
18 1 4 713.100 486.250 3
18 -1 -4 1015.86 609.849 3
18 1 -5 4004.11 986.719 3
18 1 5 2802.46 822.534 3
18 -1 -5 4482.42 1036.78 3
18 -1 5 2961.12 834.368 3
18 2 0 9534.10 1581.25 3
-18 2 0 13519.6 1522.96 7
-18 -2 0 10615.2 1343.96 7
18 2 -1 87.6309 348.220 3
18 2 1 160.110 421.656 3
18 -2 -1 819.752 490.699 3
18 -2 1 223.668 363.883 3
-18 2 1 115.419 292.505 7
-18 -2 1-258.045 330.660 7
-18 2 -1 760.764 426.484 7
-18 -2 -1-49.8398 242.269 7
18 2 -2 266.076 410.405 3
18 2 2 139.130 403.480 3
18 -2 -2-102.442 419.986 3
18 -2 2 99.4071 395.733 3
-18 2 -2 996.589 421.916 7
-18 2 2 1091.75 535.969 7
-18 -2 2 1557.86 538.118 7
18 2 -3 108.862 345.160 3
18 2 3-94.3408 302.043 3
18 -2 -3-53.1137 435.252 3
18 -2 3-378.209 497.062 3
18 -2 -3 1010.11 395.360 8
18 2 -4-0.95165 420.855 3
18 2 4 654.280 413.224 3
18 -2 -4 67.9145 447.974 3
18 -2 4 417.137 489.058 3
18 -2 -4 429.064 277.628 8
18 2 -5 1021.36 563.146 3
18 2 5 1185.45 577.297 3
18 -2 -5 720.814 337.975 3
18 -2 5 1151.83 592.378 3
18 3 0 11220.7 1735.82 3
-18 3 0 11006.9 1390.33 7
-18 -3 0 12980.3 1481.09 7
18 3 -1 32359.0 2932.23 3
18 3 1 33095.2 2960.22 3
-18 3 1 36969.6 2526.67 7
-18 -3 1 37447.1 2479.65 7
-18 3 -1 36615.2 2514.27 7
-18 -3 -1 35896.1 2427.29 7
18 3 -2 4777.27 1174.50 3
18 3 2 4058.64 1041.20 3
-18 3 -2 5859.79 1029.77 7
-18 3 2 4581.48 952.421 7
-18 -3 2 5275.27 968.730 7
18 3 -3 5723.66 1190.84 3
18 3 3 4103.28 1038.81 3
18 -3 -3 3452.80 964.431 3
18 -3 -3 4720.17 796.395 8
18 3 -4 2117.71 765.116 3
18 3 4 363.042 238.647 3
18 -3 -4 1843.23 671.155 3
18 -3 4 1423.57 665.637 3
18 -3 -4 1891.46 552.274 8
18 3 -5 1008.63 509.536 3
18 3 5 572.094 339.392 3
18 -3 -5 1123.18 662.423 3
18 -3 5 1227.47 585.858 3
18 -3 -5 1624.61 531.022 8
18 4 0 16948.0 2158.14 3
-18 4 0 19737.7 1838.31 7
-18 -4 0 18050.8 1716.85 7
18 4 -1-243.464 559.286 3
18 4 1 94.7985 410.402 3
-18 4 1 1066.44 456.884 7
-18 -4 1 325.235 332.596 7
-18 4 -1 361.957 324.171 7
-18 -4 -1 175.638 303.159 7
18 4 -2 15130.9 1999.47 3
18 4 2 16157.0 2046.12 3
-18 4 2 15663.0 1688.67 7
-18 -4 2 16814.4 1687.45 7
-18 4 -2 17201.5 1769.87 7
18 4 -3 361.814 327.547 3
18 4 3 547.142 511.463 3
18 -4 -3 558.951 350.702 8
18 4 4 20.9735 227.109 3
18 -4 -4 574.148 364.194 8
18 4 5 824.468 414.196 3
18 -4 5 1317.96 595.136 3
18 -4 -5 400.633 311.887 8
18 5 0 5178.03 1217.06 3
-18 5 0 5521.54 1020.42 7
-18 -5 0 6180.01 1017.38 7
18 5 -1 22842.2 2506.91 3
18 5 1 17561.2 2195.75 3
-18 5 1 20268.0 1955.19 7
-18 -5 1 21815.8 1888.74 7
-18 5 -1 21142.9 1940.84 7
-18 -5 -1 20741.0 1841.52 7
18 5 -2 4947.38 1185.51 3
18 5 2 5801.77 1247.56 3
-18 5 -2 4308.58 890.491 7
-18 -5 2 6197.56 1051.23 7
-18 5 2 6489.87 1120.26 7
18 5 -3 3224.38 930.578 3
18 5 3 2790.39 872.118 3
18 -5 -3 3444.58 752.814 8
18 5 -4 1184.87 452.472 3
18 5 4 1463.87 687.682 3
18 -5 -4 1238.07 468.159 8
18 -5 -5 1252.17 487.181 8
18 6 0 6593.17 1401.09 3
-18 6 0 7187.05 1142.33 7
-18 -6 0 5926.45 986.517 7
18 6 -1 471.217 526.016 3
18 6 1 178.279 424.856 3
-18 6 1-60.7854 333.766 7
-18 -6 1 154.307 285.844 7
-18 6 -1 652.191 420.854 7
-18 -6 -1-51.4142 256.558 7
18 6 -2 1493.39 741.640 3
18 6 2 1875.42 796.708 3
-18 6 -2 1717.60 619.977 7
-18 -6 -2 1999.41 609.170 7
-18 6 2 1248.94 485.680 7
18 6 -3 360.846 351.065 3
18 6 3 723.361 531.294 3
18 -6 -3 886.234 421.963 8
18 6 4 1936.96 697.370 3
18 -6 -4 2117.03 597.677 8
18 7 0 2291.63 858.252 3
-18 7 0 1128.41 482.907 7
-18 -7 0 2554.87 690.933 7
18 7 -1-359.913 515.937 3
-18 7 1-6.65501 235.596 7
-18 -7 1-82.0609 284.447 7
-18 7 -1 193.311 223.552 7
-18 -7 -1 179.593 244.969 7
18 7 -2 1310.59 701.931 3
18 7 2 862.185 512.568 3
-18 7 -2 1688.30 601.990 7
-18 -7 -2 2108.50 590.509 7
18 -7 -3 6335.17 1027.59 8
18 -7 -4 292.501 333.973 8
-18 8 0 3913.42 880.262 7
-18 -8 0 6231.26 1014.01 7
-18 8 1 486.100 373.009 7
-18 -8 1-7.16043 319.326 7
-18 8 -1-174.942 275.600 7
-18 -8 -1 805.477 420.223 7
-18 -8 -2 4720.31 900.912 7
-18 -8 -2 5648.72 977.381 6
18 -8 -3 1596.37 579.043 8
-18 -8 -3 980.946 427.127 6
-18 9 0 5074.72 986.447 7
-18 -9 0 4931.62 892.422 7
-18 -9 1 2068.39 587.427 7
-18 -9 -1 1482.00 546.507 7
-18 -9 -2 3042.09 701.239 7
-18 -9 -2 2616.55 683.838 6
-18 -9 -3 1992.29 622.752 6
-18 -10 0 13502.7 1446.67 7
-18 -10 -1 284.867 341.222 7
-18 -10 1 330.305 303.615 7
-18 -10 -2-160.870 238.962 7
-18 -10 -2 229.697 323.182 6
-18 -10 -3 441.471 331.658 6
19 0 0-139.766 390.316 3
-19 0 0-265.540 249.898 7
19 0 -1 1320.54 666.634 3
19 0 1 3331.49 1068.71 3
-19 0 1 2501.87 681.480 7
-19 0 -1 2801.79 772.357 7
19 0 -2 607.508 533.118 3
19 0 2 1683.14 768.868 3
-19 0 -2 1876.09 592.158 7
-19 0 2 1010.62 509.031 7
19 0 3 400.413 396.134 3
19 1 0 72.1674 332.768 3
19 -1 0 134.491 376.743 3
-19 1 0 247.845 355.516 7
-19 -1 0 171.270 213.617 7
19 1 -1 429.139 426.732 3
19 1 1-135.078 452.238 3
19 -1 -1-426.861 626.266 3
19 -1 1 348.556 437.864 3
-19 1 1-193.458 340.854 7
-19 -1 1 425.200 415.224 7
-19 1 -1 269.423 303.434 7
-19 -1 -1 265.033 295.104 7
19 1 -2-360.493 530.264 3
19 1 2 376.973 417.617 3
19 -1 -2-397.349 521.681 3
19 -1 2 8.75536 360.938 3
-19 -1 -2 123.620 240.644 7
-19 1 2 296.525 322.471 7
-19 -1 2-317.760 233.412 7
19 1 3-1115.59 607.383 3
19 -1 3-54.9260 281.757 3
19 2 0-186.135 520.804 3
19 -2 0 715.656 542.969 3
-19 2 0 767.605 489.521 7
-19 -2 0-213.302 274.857 7
19 2 -1 93.3257 387.086 3
19 2 1-468.000 481.784 3
19 -2 -1 511.400 464.571 3
19 -2 1 38.3375 404.946 3
-19 2 1 673.575 429.025 7
-19 -2 1 852.333 482.646 7
-19 2 -1 867.486 424.258 7
-19 -2 -1-221.105 269.471 7
19 2 -2 1481.43 696.758 3
19 2 2 1286.71 688.217 3
19 -2 -2 972.843 542.155 3
19 -2 2 93.7348 425.721 3
-19 -2 -2 1169.20 479.014 7
-19 -2 2 1644.25 603.997 7
19 3 0 155.915 374.997 3
-19 3 0 280.261 312.290 7
-19 -3 0 252.324 254.618 7
19 3 -1 1851.83 835.256 3
19 3 1 1657.66 738.731 3
-19 3 1 550.605 390.583 7
-19 -3 1 1241.84 554.564 7
-19 3 -1 1233.13 529.653 7
-19 -3 -1 770.471 373.676 7
19 3 2-576.948 493.303 3
19 -3 2 325.295 459.397 3
-19 -3 -2 341.294 347.837 7
-19 -3 2 204.598 229.418 7
19 4 0 333.139 489.577 3
-19 4 0 257.347 381.124 7
-19 -4 0-95.1759 286.372 7
-19 -4 1 1303.07 522.866 7
-19 -4 -1 983.852 452.722 7
-19 -4 -2 1364.28 533.706 7
-19 -4 2 2829.04 781.827 7
19 -4 -4 370.488 295.068 8
-19 -5 0 321.563 292.152 7
-19 -5 1 933.306 416.805 7
-19 -5 -1 392.269 367.612 7
-19 -5 -2 180.224 240.149 7
19 -5 -4 575.308 366.206 8
-19 -6 0 208.518 316.364 7
-19 -6 1-12.0703 193.550 7
-19 -6 -1 380.584 332.131 7
-19 -6 -2 161.192 260.243 7
-19 -7 0-134.006 367.201 7
-19 -7 1 683.434 384.891 7
-19 -7 -1 580.240 367.380 7
-19 -7 -2 551.513 346.011 7
-19 -8 0-192.230 236.900 7
-19 -8 1 731.095 464.801 7
-19 -8 -1 1769.75 584.205 7
-19 -8 -2 1934.34 640.034 7
-19 -9 0 280.348 337.885 7
-19 -9 -1 200.739 244.130 7
-19 -9 1 92.5224 325.040 7
-19 -10 0-13.3797 209.790 7
-19 -10 -1 556.879 294.606 7
0 0 0 0.00 0.00 0
TITL I in Pnma
REM Pnma (#62, found as Pbnm in bca setting)
CELL 0.71073 15.431682 17.294546 7.987326 90.0000 90.0000 90.0000
ZERR 4.00 0.000282 0.000303 0.000153 0.0000 0.0000 0.0000
LATT 1
SYMM -x+1/2,-y, z+1/2
SYMM -x, y+1/2,-z
SYMM x+1/2,-y+1/2,-z+1/2
SFAC C H N O Cd I
UNIT 80.00 80.00 16.00 24.00 4.00 12.00
REM CrysAlisPro recorded range (K): Min=199.9; max=200.0; aver:199.9
TEMP -73
TREF
HKLF 4
END
;
_shelx_hkl_checksum 35881
_shelx_res_file
;
TITL I in Pnma #62
I.res
created by SHELXL-2018/3 at 10:23:52 on 15-Jan-2023
REM reset to Pnma #62
CELL 0.71073 15.431682 17.294546 7.987326 90 90 90
ZERR 4 0.000282 0.000303 0.000153 0 0 0
LATT 1
SYMM 0.5-X,-Y,0.5+Z
SYMM 0.5+X,0.5-Y,0.5-Z
SYMM -X,0.5+Y,-Z
SFAC C H Cd I N Ni
UNIT 40 96 4 16 16 4
EQIV $1 1-X,1-Y,1-Z
EQIV $2 0.5+X,+Y,1.5-Z
EQIV $3 +X,+Y,-1+Z
L.S. 17
PLAN 7
SIZE 0.03 0.05 0.1
TEMP -73
CONF
HTAB N2 I1
HTAB N2 I3_$2
HTAB N1 I1
HTAB N1 I2
HTAB C2 I1_$2
HTAB C1 I1_$3
HTAB C3 I1_$1
BIND I1 Ni1
htab
MORE -1
BOND $H
fmap 2
acta
SHEL 999 0.75
REM
REM
REM
WGHT 0.023700 2.537500
FVAR 1.09913
I1 4 0.387621 0.619521 0.751072 11.00000 0.02646 0.02180 =
0.02917 0.00314 0.00288 0.00438
I3 4 0.131652 0.750000 0.684585 10.50000 0.02215 0.03517 =
0.03999 0.00000 0.00396 0.00000
I2 4 0.342605 0.750000 0.274688 10.50000 0.02898 0.02744 =
0.02851 0.00000 -0.00008 0.00000
CD1 3 0.307338 0.750000 0.618866 10.50000 0.02274 0.01977 =
0.03149 0.00000 0.00133 0.00000
NI1 6 0.500000 0.500000 0.500000 10.50000 0.01713 0.01644 =
0.01788 0.00129 -0.00145 -0.00197
N2 5 0.601027 0.561063 0.559938 11.00000 0.01754 0.02098 =
0.02875 -0.00116 0.00244 -0.00054
AFIX 3
H2 2 0.577167 0.604133 0.607128 11.00000 -1.20000
AFIX 0
N1 5 0.469317 0.566367 0.313295 11.00000 0.02601 0.01947 =
0.02017 -0.00076 -0.00014 0.00349
AFIX 3
H1 2 0.448687 0.609197 0.366795 11.00000 -1.20000
AFIX 0
C2 1 0.655446 0.515178 0.675035 11.00000 0.02524 0.03954 =
0.03265 -0.00304 -0.01005 -0.00264
AFIX 23
H2A 2 0.694792 0.549462 0.738857 11.00000 -1.20000
H2B 2 0.690905 0.477600 0.611403 11.00000 -1.20000
AFIX 0
C1 1 0.405026 0.526453 0.208035 11.00000 0.03202 0.03945 =
0.02895 0.00277 -0.00953 0.00317
AFIX 23
H1A 2 0.434068 0.489215 0.132448 11.00000 -1.20000
H1B 2 0.372638 0.564247 0.139112 11.00000 -1.20000
AFIX 0
C5 1 0.655023 0.596494 0.426913 11.00000 0.02322 0.02934 =
0.04233 -0.00018 0.00113 -0.01065
AFIX 23
H5A 2 0.682907 0.555079 0.360435 11.00000 -1.20000
H5B 2 0.701410 0.627786 0.479260 11.00000 -1.20000
AFIX 0
C4 1 0.602102 0.647316 0.311879 11.00000 0.04338 0.02161 =
0.04476 0.00447 0.01226 -0.00642
AFIX 23
H4A 2 0.641638 0.675793 0.236207 11.00000 -1.20000
H4B 2 0.570150 0.685815 0.379726 11.00000 -1.20000
AFIX 0
C3 1 0.537696 0.601172 0.207234 11.00000 0.03243 0.02638 =
0.02950 0.00714 0.00781 -0.00070
AFIX 23
H3A 2 0.510613 0.635643 0.123246 11.00000 -1.20000
H3B 2 0.568819 0.559713 0.146499 11.00000 -1.20000
AFIX 0
HKLF 4
REM I in Pnma #62
REM wR2 = 0.0636, GooF = S = 1.062, Restrained GooF = 1.062 for all data
REM R1 = 0.0314 for 2204 Fo > 4sig(Fo) and 0.0429 for all 2644 data
REM 97 parameters refined using 0 restraints
END
WGHT 0.0237 2.5375
REM Instructions for potential hydrogen bonds
HTAB N2 I1
HTAB N2 I3_$2
HTAB N1 I1
HTAB N1 I2
HTAB C2 I1_$2
HTAB C1 I1_$3
HTAB C3 I1_$1
REM Highest difference peak 2.574, deepest hole -1.233, 1-sigma level 0.178
Q1 1 0.1364 0.7500 0.8021 10.50000 0.05 2.57
Q2 1 0.3137 0.7500 0.8656 10.50000 0.05 2.00
Q3 1 0.3424 0.7500 0.1699 10.50000 0.05 1.51
Q4 1 0.5014 0.4992 0.0223 11.00000 0.05 0.92
Q5 1 0.3899 0.6212 0.6419 11.00000 0.05 0.87
Q6 1 0.1342 0.7500 0.5471 10.50000 0.05 0.82
Q7 1 0.3405 0.7500 0.3990 10.50000 0.05 0.71
;
_shelx_res_checksum 61322
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-x, y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'-x-1/2, y-1/2, z-1/2'
'x, -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
_atom_site_disorder_assembly
_atom_site_disorder_group
I I1 0.38762(2) 0.61952(2) 0.75107(4) 0.02581(10) Uani d 1 . .
I I3 0.13165(3) 0.750000 0.68459(7) 0.03244(13) Uani d 1 . .
I I2 0.34261(3) 0.750000 0.27469(6) 0.02831(12) Uani d 1 . .
Cd Cd1 0.30734(3) 0.750000 0.61887(7) 0.02466(13) Uani d 1 . .
Ni Ni1 0.500000 0.500000 0.500000 0.01715(18) Uani d 1 . .
N N2 0.6010(2) 0.5611(2) 0.5599(5) 0.0224(8) Uani d 1 . .
H H2 0.577167 0.604133 0.607128 0.027 Uiso d 1 . .
N N1 0.4693(2) 0.5664(2) 0.3133(5) 0.0219(8) Uani d 1 . .
H H1 0.448687 0.609197 0.366795 0.026 Uiso d 1 . .
C C2 0.6554(3) 0.5152(3) 0.6750(7) 0.0325(12) Uani d 1 . .
H H2A 0.694792 0.549462 0.738857 0.039 Uiso calc 1 . .
H H2B 0.690905 0.477600 0.611403 0.039 Uiso calc 1 . .
C C1 0.4050(3) 0.5265(3) 0.2080(7) 0.0335(12) Uani d 1 . .
H H1A 0.434068 0.489215 0.132448 0.040 Uiso calc 1 . .
H H1B 0.372638 0.564247 0.139112 0.040 Uiso calc 1 . .
C C5 0.6550(3) 0.5965(3) 0.4269(7) 0.0316(12) Uani d 1 . .
H H5A 0.682907 0.555079 0.360435 0.038 Uiso calc 1 . .
H H5B 0.701410 0.627786 0.479260 0.038 Uiso calc 1 . .
C C4 0.6021(4) 0.6473(3) 0.3119(7) 0.0366(13) Uani d 1 . .
H H4A 0.641638 0.675793 0.236207 0.044 Uiso calc 1 . .
H H4B 0.570150 0.685815 0.379726 0.044 Uiso calc 1 . .
C C3 0.5377(3) 0.6012(3) 0.2072(6) 0.0294(11) Uani d 1 . .
H H3A 0.510613 0.635643 0.123246 0.035 Uiso calc 1 . .
H H3B 0.568819 0.559713 0.146499 0.035 Uiso calc 1 . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
I1 0.02646(18) 0.02180(17) 0.0292(2) 0.00438(12) 0.00288(13) 0.00314(13)
I3 0.0221(2) 0.0352(3) 0.0400(3) 0.000 0.0040(2) 0.000
I2 0.0290(3) 0.0274(2) 0.0285(3) 0.000 -0.0001(2) 0.000
Cd1 0.0227(3) 0.0198(2) 0.0315(3) 0.000 0.0013(2) 0.000
Ni1 0.0171(4) 0.0164(4) 0.0179(4) -0.0020(3) -0.0014(3) 0.0013(3)
N2 0.018(2) 0.021(2) 0.029(2) -0.0005(15) 0.0024(17) -0.0012(17)
N1 0.026(2) 0.0195(19) 0.020(2) 0.0035(16) -0.0001(17) -0.0008(16)
C2 0.025(3) 0.040(3) 0.033(3) -0.003(2) -0.010(2) -0.003(2)
C1 0.032(3) 0.039(3) 0.029(3) 0.003(2) -0.010(2) 0.003(2)
C5 0.023(3) 0.029(3) 0.042(3) -0.011(2) 0.001(2) 0.000(2)
C4 0.043(3) 0.022(3) 0.045(3) -0.006(2) 0.012(3) 0.004(2)
C3 0.032(3) 0.026(3) 0.030(3) -0.001(2) 0.008(2) 0.007(2)
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'
Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 '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'
Ni Ni 0.3393 1.1124 '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
Cd1 I1 Ni1 . . 120.129(15) ?
I1 Cd1 I1 8_575 . 108.39(2) ?
I1 Cd1 I2 8_575 . 106.608(15) ?
I1 Cd1 I2 . . 106.608(15) ?
I3 Cd1 I1 . . 111.407(15) ?
I3 Cd1 I1 . 8_575 111.407(15) ?
I3 Cd1 I2 . . 112.16(2) ?
N2 Ni1 I1 . . 86.14(11) ?
N2 Ni1 I1 5_666 . 93.86(11) ?
N2 Ni1 N2 5_666 . 180.0 ?
N1 Ni1 I1 5_666 . 91.78(11) ?
N1 Ni1 I1 . . 88.22(11) ?
N1 Ni1 N2 . 5_666 86.35(16) ?
N1 Ni1 N2 5_666 5_666 93.65(16) ?
N1 Ni1 N2 5_666 . 86.35(16) ?
N1 Ni1 N2 . . 93.65(16) ?
N1 Ni1 N1 5_666 . 180.0 ?
Ni1 N2 H2 . . 102.8 ?
C2 N2 Ni1 . . 108.5(3) ?
C2 N2 H2 . . 114.3 ?
C2 N2 C5 . . 110.4(4) ?
C5 N2 Ni1 . . 119.9(3) ?
C5 N2 H2 . . 100.7 ?
Ni1 N1 H1 . . 101.9 ?
C1 N1 Ni1 . . 109.0(3) ?
C1 N1 H1 . . 114.4 ?
C1 N1 C3 . . 110.1(4) ?
C3 N1 Ni1 . . 120.4(3) ?
C3 N1 H1 . . 100.7 ?
N2 C2 H2A . . 110.3 ?
N2 C2 H2B . . 110.3 ?
N2 C2 C1 . 5_666 106.9(4) ?
H2A C2 H2B . . 108.6 ?
C1 C2 H2A 5_666 . 110.3 ?
C1 C2 H2B 5_666 . 110.3 ?
N1 C1 C2 . 5_666 106.7(4) ?
N1 C1 H1A . . 110.4 ?
N1 C1 H1B . . 110.4 ?
C2 C1 H1A 5_666 . 110.4 ?
C2 C1 H1B 5_666 . 110.4 ?
H1A C1 H1B . . 108.6 ?
N2 C5 H5A . . 109.2 ?
N2 C5 H5B . . 109.2 ?
N2 C5 C4 . . 111.9(4) ?
H5A C5 H5B . . 107.9 ?
C4 C5 H5A . . 109.2 ?
C4 C5 H5B . . 109.2 ?
C5 C4 H4A . . 109.1 ?
C5 C4 H4B . . 109.1 ?
C5 C4 C3 . . 112.4(4) ?
H4A C4 H4B . . 107.9 ?
C3 C4 H4A . . 109.1 ?
C3 C4 H4B . . 109.1 ?
N1 C3 C4 . . 111.3(4) ?
N1 C3 H3A . . 109.4 ?
N1 C3 H3B . . 109.4 ?
C4 C3 H3A . . 109.4 ?
C4 C3 H3B . . 109.4 ?
H3A C3 H3B . . 108.0 ?
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
I1 Cd1 . 2.7825(4) ?
I1 Ni1 . 3.3618(3) ?
I3 Cd1 . 2.7615(7) ?
I2 Cd1 . 2.8024(7) ?
Ni1 N2 . 1.943(4) ?
Ni1 N2 5_666 1.943(4) ?
Ni1 N1 5_666 1.940(4) ?
Ni1 N1 . 1.940(4) ?
N2 H2 . 0.9124 ?
N2 C2 . 1.477(6) ?
N2 C5 . 1.483(6) ?
N1 H1 . 0.9125 ?
N1 C1 . 1.472(6) ?
N1 C3 . 1.481(6) ?
C2 H2A . 0.9900 ?
C2 H2B . 0.9900 ?
C2 C1 5_666 1.504(7) ?
C1 H1A . 0.9900 ?
C1 H1B . 0.9900 ?
C5 H5A . 0.9900 ?
C5 H5B . 0.9900 ?
C5 C4 . 1.511(7) ?
C4 H4A . 0.9900 ?
C4 H4B . 0.9900 ?
C4 C3 . 1.524(7) ?
C3 H3A . 0.9900 ?
C3 H3B . 0.9900 ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
. . . . . . . . .
N1 H1 I1 . 0.91 3.22 3.829(4) 127 yes
N2 H2 I1 . 0.91 3.15 3.768(4) 126 yes
N1 H1 I2 . 0.91 3.03 3.742(4) 137 yes
N2 H2 I3 6_657 0.91 3.14 3.881(4) 140 yes
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
Ni1 N2 C2 C1 . . . 5_666 -39.7(5) ?
Ni1 N2 C5 C4 . . . . 55.7(5) ?
Ni1 N1 C1 C2 . . . 5_666 39.1(5) ?
Ni1 N1 C3 C4 . . . . -55.5(5) ?
N2 C5 C4 C3 . . . . -67.2(6) ?
C2 N2 C5 C4 . . . . -177.0(4) ?
C1 N1 C3 C4 . . . . 176.4(4) ?
C5 N2 C2 C1 . . . 5_666 -173.1(4) ?
C5 C4 C3 N1 . . . . 66.9(5) ?
C3 N1 C1 C2 . . . 5_666 173.2(4) ?
_cod_database_fobs_code 2022842