#------------------------------------------------------------------------------
#$Date: 2024-12-07 18:10:59 +0100 (Sat, 07 Dec 2024) $
#$Revision: 296778 $
#$URL: svn://www.crystallography.net/cod/cif/2/02/32/2023283.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_2023283
loop_
_publ_author_name
'Reibenspies, Joseph'
'Small, Nadia'
'Bhuvanesh, Nattamai'
'Chiarella, Gina'
'Salazar, Vivian'
'Pery, Br\'eayshia'
'Smith, Rukiyah'
'Toole, Deja'
'Hewage, Shamika'
'Fernando, Harschica'
'Reinheimer, Eric'
_publ_section_title
;
Crystal structure and Hirshfeld surface analysis of (nitrato-\k2
O,O′)(1,4,7,10-tetraazacyclododecane-\k4 N)nickel(II) nitrate
;
_journal_coeditor_code PK2709
_journal_issue 11
_journal_name_full
'Acta Crystallographica Section E Crystallographic Communications'
_journal_page_first 1157
_journal_page_last 1160
_journal_paper_doi 10.1107/S2056989024009496
_journal_volume 80
_journal_year 2024
_chemical_formula_iupac '[Ni (C8 H20 N4) (N1 O3)] N O3'
_chemical_formula_moiety 'C8 H20 N5 Ni O3 +, N O3 -'
_chemical_formula_sum 'C8 H20 N6 Ni O6'
_chemical_formula_weight 355.01
_chemical_name_systematic
'(Nitrato-\k^2^O,O')(1,4,7,10-tetraazacyclododecane-\k^4^N)nickel(II) nitrate'
_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 dual
_audit_creation_method
;
HOleoux2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_cell_angle_alpha 90
_cell_angle_beta 94.973(5)
_cell_angle_gamma 90
_cell_formula_units_Z 4
_cell_length_a 8.7321(5)
_cell_length_b 15.2444(9)
_cell_length_c 10.8545(6)
_cell_measurement_reflns_used 4001
_cell_measurement_temperature 293
_cell_measurement_theta_max 29.8940
_cell_measurement_theta_min 2.2880
_cell_volume 1439.46(14)
_computing_cell_refinement
;
CrysAlisPro 1.171.43.121a (Rigaku OD, 2024)
;
_computing_data_collection
;
CrysAlisPro 1.171.43.121a (Rigaku OD, 2024)
;
_computing_data_reduction
;
CrysAlisPro 1.171.43.121a (Rigaku OD, 2024)
;
_computing_molecular_graphics
;
Olex2 1.5 (Dolomanov et al., 2009)
;
_computing_publication_material
;
Olex2 1.5 (Dolomanov et al., 2009)
;
_computing_structure_refinement
;
SHELXL2019/2 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT (Sheldrick, 2015a)
;
_diffrn_ambient_temperature 293
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device 'two-circle diffractometer'
_diffrn_measurement_device_type 'XtaLAB Mini II'
_diffrn_measurement_method '\w scans'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0376
_diffrn_reflns_av_unetI/netI 0.0504
_diffrn_reflns_limit_h_max 8
_diffrn_reflns_limit_h_min -10
_diffrn_reflns_limit_k_max 19
_diffrn_reflns_limit_k_min -19
_diffrn_reflns_limit_l_max 13
_diffrn_reflns_limit_l_min -13
_diffrn_reflns_number 12195
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 26.371
_diffrn_reflns_theta_min 2.309
_exptl_absorpt_coefficient_mu 1.386
_exptl_absorpt_correction_T_max 1.00000
_exptl_absorpt_correction_T_min 0.89877
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
(CrysAlisPro; Rigaku OD, 2024)
;
_exptl_crystal_colour blue
_exptl_crystal_density_diffrn 1.638
_exptl_crystal_description plate
_exptl_crystal_F_000 744
_exptl_crystal_size_max 0.4
_exptl_crystal_size_mid 0.3
_exptl_crystal_size_min 0.02
_refine_diff_density_max 0.385
_refine_diff_density_min -0.279
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.086
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 191
_refine_ls_number_reflns 12195
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.086
_refine_ls_R_factor_all 0.0534
_refine_ls_R_factor_gt 0.0362
_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^)+(0.0406P)^2^+0.8788P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0903
_refine_ls_wR_factor_ref 0.1044
_reflns_number_gt 9604
_reflns_number_total 12195
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file pk2709.cif
_cod_data_source_block I
_cod_depositor_comments 'Adding full bibliography for 2023283.cif.'
_cod_original_cell_volume 1439.47(14)
_cod_database_code 2023283
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_hkl_file
;
0 0 1 2.28 0.87 1
0 0 -210935.60 418.68 1
0 0 211214.40 418.64 1
0 0 210926.50 418.68 1
0 0 -211222.40 418.63 1
0 0 210984.90 418.57 1
0 0 -211187.50 418.61 1
0 0 3 -0.22 2.13 1
0 0 -3 -0.36 2.45 1
0 0 3 0.86 2.36 1
0 0 -3 0.76 2.15 1
0 0 -3 1.93 2.14 1
0 0 -3 1.10 0.97 1
0 0 3 1.85 2.25 1
0 0 4 2368.27 89.08 1
0 0 -4 2383.91 89.30 1
0 0 4 2350.91 89.30 1
0 0 -4 2423.66 89.12 1
0 0 4 2468.09 89.01 1
0 0 4 2334.80 88.67 1
0 0 -4 2406.25 89.14 1
0 0 -4 2224.46 88.23 1
0 0 -5 1.04 2.78 1
0 0 5 3.61 2.60 1
0 0 -5 0.17 2.45 1
0 0 5 1.47 2.81 1
0 0 5 -1.01 1.87 1
0 0 -5 2.23 2.72 1
0 0 5 -0.94 2.27 1
0 0 -5 0.66 1.04 1
0 0 -6 732.02 30.25 1
0 0 6 723.51 29.27 1
0 0 -6 781.78 30.15 1
0 0 6 774.75 30.36 1
-1 0 7 125.65 7.42 -2
0 0 -7 125.65 7.42 1
-1 0 7 112.19 6.88 -2
0 0 -7 112.19 6.88 1
0 0 -8 27.63 4.49 1
0 0 -8 23.10 4.02 1
0 0 -9 -3.15 3.93 1
0 0 -9 2.08 3.58 1
0 0 -10 93.28 7.43 1
0 0 -10 93.42 7.14 1
0 0 -11 -1.49 4.60 1
0 0 -11 3.88 4.85 1
0 0 -12 31.06 5.95 1
0 0 -13 -0.59 5.57 1
0 0 -14 77.21 8.71 1
0 0 -15 5.49 6.29 1
0 1 -1 189.83 5.40 1
0 1 1 198.54 5.32 1
0 -1 -1 193.69 5.32 1
0 1 -1 216.18 5.54 1
0 1 -1 190.30 5.27 1
0 1 -2 152.41 4.49 1
0 1 2 159.29 4.31 1
0 -1 -2 155.75 4.34 1
0 1 2 150.65 4.41 1
0 -1 2 167.80 4.47 1
0 1 2 160.76 3.99 1
0 1 -2 162.85 4.53 1
0 -1 -2 161.10 4.01 1
0 1 -2 157.20 3.77 1
0 1 -3 13.42 2.68 1
0 1 3 10.74 2.31 1
0 -1 -3 12.28 2.59 1
0 -1 3 11.79 2.34 1
0 1 -3 14.48 2.43 1
0 1 3 11.38 2.66 1
0 1 3 10.35 1.51 1
0 1 -3 12.71 2.61 1
0 -1 -3 15.09 2.25 1
0 -1 3 9.95 2.38 1
0 1 -3 13.31 1.63 1
0 1 3 14.80 2.21 1
0 1 4 108.13 5.63 1
0 1 -4 118.84 6.02 1
0 -1 4 116.22 5.71 1
0 -1 -4 110.42 5.95 1
0 1 -4 109.39 5.80 1
0 1 4 99.42 5.80 1
0 -1 4 122.58 5.80 1
0 1 -4 104.37 5.88 1
0 1 4 112.04 5.49 1
0 -1 -4 111.64 5.58 1
0 1 4 114.73 5.00 1
0 1 -4 110.36 4.92 1
0 1 5 208.82 8.98 1
0 1 -5 187.39 9.26 1
0 -1 -5 197.71 9.26 1
0 -1 5 197.69 9.00 1
0 1 -5 201.19 9.02 1
0 1 5 183.36 9.22 1
0 1 5 183.61 8.13 1
0 1 5 202.75 8.70 1
0 1 -5 194.31 9.17 1
0 -1 5 195.63 8.56 1
0 -1 5 204.70 8.92 1
0 -1 -5 208.91 9.01 1
0 1 -5 180.79 7.97 1
0 -1 -6 1250.97 49.96 1
0 1 -6 1268.34 49.99 1
0 1 6 1313.80 50.10 1
0 -1 -6 1277.83 49.65 1
0 -1 6 1315.20 49.20 1
0 1 6 1286.26 49.36 1
0 1 -6 1307.16 49.91 1
0 1 -6 1220.01 48.57 1
-1 -1 7 404.43 17.54 -2
0 1 -7 404.43 17.54 1
-1 1 7 397.02 17.55 -2
0 -1 -7 397.02 17.55 1
-1 1 7 389.94 17.06 -2
0 -1 -7 389.94 17.06 1
-1 -1 7 399.34 17.38 -2
0 1 -7 399.34 17.38 1
1 -1 -7 403.31 17.53 -2
0 1 7 403.31 17.53 1
0 -1 -8 186.81 10.30 1
0 1 -8 200.74 10.40 1
0 -1 -8 202.36 9.91 1
0 1 -8 185.10 10.13 1
0 1 8 204.00 10.54 1
0 -1 -9 186.98 10.27 1
0 1 -9 165.26 10.15 1
0 -1 -9 184.07 9.73 1
0 1 -9 181.28 9.97 1
0 1 -10 60.75 6.27 1
0 -1 -10 89.69 6.93 1
0 -1 -10 66.62 6.05 1
0 1 -10 69.45 6.49 1
0 1 -11 76.02 7.54 1
0 -1 -11 79.84 7.57 1
0 1 -11 87.94 7.11 1
0 1 -12 21.50 6.00 1
0 -1 -12 21.08 5.65 1
0 1 -12 19.04 5.55 1
0 1 -13 2.41 5.61 1
0 -1 -13 -7.06 5.93 1
0 -1 -14 -1.91 5.77 1
0 1 -14 -9.77 6.32 1
0 -1 -15 4.75 6.29 1
0 1 -15 -0.69 6.29 1
0 2 0 86.80 3.82 -2
0 -2 0 86.80 3.82 1
0 -2 0 85.51 3.81 -2
0 2 0 85.51 3.81 1
0 -2 0 82.70 3.83 -2
0 2 0 82.70 3.83 1
0 2 -1 3103.29 115.92 1
0 2 1 3067.67 115.81 1
0 -2 1 3147.88 115.91 1
0 -2 -1 3098.54 115.83 1
0 2 1 3116.93 115.96 1
0 -2 -1 3041.66 115.99 1
0 2 -1 3025.34 115.86 1
0 2 -1 2998.54 115.98 1
0 -2 1 2866.91 115.93 1
0 -2 1 3069.94 115.87 1
0 2 -1 3245.58 116.00 1
0 2 1 2982.29 115.80 1
0 2 -2 184.60 7.71 1
0 2 2 179.61 7.50 1
0 -2 2 191.08 7.65 1
0 -2 -2 178.46 7.55 1
0 -2 -2 182.81 7.21 1
0 -2 2 147.41 7.54 1
0 2 2 182.67 7.19 1
0 2 -2 183.88 7.76 1
0 2 -2 179.99 7.53 1
0 2 2 173.98 7.00 1
0 -2 3 24.58 2.81 1
0 2 -3 51.10 3.76 1
0 -2 -3 56.55 3.43 1
0 2 3 60.08 3.47 1
0 -2 -3 55.55 3.05 1
0 -2 3 53.36 3.49 1
0 2 3 58.93 3.05 1
0 2 -3 62.10 3.75 1
0 2 -3 53.58 3.12 1
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0 2 -4 260.84 8.14 1
0 -2 -4 256.37 7.93 1
0 2 4 251.48 7.98 1
0 2 -4 262.36 7.86 1
0 2 -4 279.46 8.20 1
0 2 4 257.09 7.18 1
0 -2 -4 243.68 7.27 1
0 -2 4 285.33 7.94 1
0 2 4 254.92 6.40 1
0 2 -4 248.56 6.98 1
0 2 -5 87.24 5.36 1
0 -2 -5 85.64 5.28 1
0 2 5 83.48 5.04 1
0 -2 5 76.64 5.02 1
0 2 5 86.73 5.34 1
0 2 -5 87.15 5.15 1
0 2 5 82.44 3.99 1
0 2 -5 88.32 5.49 1
0 2 5 92.12 4.73 1
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0 -2 -5 85.52 4.81 1
0 2 -5 84.27 4.29 1
0 2 -6 10.42 3.38 1
0 -2 -6 14.75 3.56 1
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0 -2 6 8.21 2.56 1
0 2 -6 15.13 3.46 1
0 -2 -6 11.83 2.89 1
0 2 6 15.19 2.71 1
0 2 -6 19.13 2.68 1
-1 -2 7 63.62 5.23 -2
0 2 -7 63.62 5.23 1
-1 2 7 54.25 5.14 -2
0 -2 -7 54.25 5.14 1
-1 -2 7 67.88 5.44 -2
0 2 -7 67.88 5.44 1
-1 2 7 62.60 4.66 -2
0 -2 -7 62.60 4.66 1
1 -2 -7 58.27 5.34 -2
0 2 7 58.27 5.34 1
0 2 -8 98.89 7.38 1
0 -2 -8 72.53 6.04 1
0 -2 -8 68.94 5.48 1
0 2 -8 82.82 6.39 1
0 2 8 89.38 6.63 1
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0 -2 -9 10.10 3.99 1
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0 -2 -9 4.38 3.55 1
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0 2 -15 45.85 8.01 1
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0 3 0 0.75 1.88 1
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0 -3 0 -0.54 1.34 1
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0 3 0 -0.04 1.31 1
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0 -3 0 -0.64 1.89 1
0 3 0 0.59 1.29 -2
0 -3 0 0.59 1.29 1
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0 3 0 0.35 1.26 1
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0 3 0 3.21 1.94 1
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0 3 -1 15.46 2.30 1
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0 -3 2 11.85 2.17 1
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0 3 2 9.97 1.32 1
0 3 -2 10.10 2.42 1
0 3 2 10.73 1.65 1
0 -3 -2 11.54 1.38 1
0 3 3 7.54 2.22 1
0 3 -3 9.75 2.55 1
0 -3 -3 9.01 2.24 1
0 -3 3 8.79 2.40 1
0 -3 3 5.36 2.33 1
0 3 -3 7.29 2.69 1
0 -3 3 3.14 2.16 1
0 3 -3 7.84 2.23 1
0 3 3 9.01 1.63 1
0 3 3 7.04 1.27 1
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0 3 -5 337.12 13.52 1
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0 -3 -7 289.52 13.35 1
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0 3 -7 281.42 13.56 1
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0 3 -7 272.45 13.48 1
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0 -3 -7 289.54 12.80 1
1 -3 -7 307.71 13.67 -2
0 3 7 307.71 13.67 1
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0 -3 -8 600.42 25.25 1
0 3 -8 589.47 25.34 1
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0 3 8 606.78 25.44 1
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0 3 -9 35.35 5.35 1
0 3 -9 25.03 4.81 1
0 3 9 21.61 4.78 1
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0 -3 -10 190.58 10.73 1
0 3 -10 184.11 10.60 1
0 3 10 169.38 10.50 1
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0 3 -11 8.23 4.89 1
0 3 11 3.03 4.63 1
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0 3 -12 31.60 6.39 1
0 3 -12 38.28 6.31 1
0 3 -13 -6.17 5.43 1
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0 -3 -14 8.71 6.04 1
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0 -3 -15 -1.33 6.04 1
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0 4 0 1998.39 73.23 -2
0 -4 0 1998.39 73.23 1
0 4 0 1858.81 73.26 -2
0 -4 0 1858.81 73.26 1
0 4 0 1907.94 73.62 -2
0 -4 0 1907.94 73.62 1
0 4 0 1872.90 73.19 -2
0 -4 0 1872.90 73.19 1
0 -4 0 1994.19 73.25 -2
0 4 0 1994.19 73.25 1
0 -4 0 1931.47 73.63 -2
0 4 0 1931.47 73.63 1
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0 4 -1 2306.67 89.01 1
0 -4 1 2417.16 88.98 1
0 -4 -1 2360.58 88.90 1
0 -4 -1 2265.52 89.25 1
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0 4 2 246.54 9.87 1
0 4 2 214.57 8.96 1
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0 4 -2 236.47 10.00 1
0 -4 2 227.14 9.80 1
0 4 -2 233.37 9.56 1
0 4 2 229.19 9.46 1
0 4 2 223.88 9.01 1
0 4 -2 240.23 10.02 1
0 -4 3 558.74 21.04 1
0 4 -3 539.62 21.14 1
0 -4 -3 548.24 20.92 1
0 4 3 545.00 20.81 1
0 4 3 570.92 21.12 1
0 4 3 533.63 20.34 1
0 4 -3 537.60 21.34 1
0 -4 -3 557.33 20.39 1
0 -4 3 553.21 21.00 1
0 4 -3 531.14 21.06 1
0 4 3 511.42 20.41 1
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0 4 4 64.55 4.04 1
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0 -4 -4 60.46 3.48 1
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0 -4 -5 268.85 11.55 1
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0 4 6 4.12 3.17 1
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0 4 -6 0.68 2.37 1
-1 -4 7 163.78 9.54 -2
0 4 -7 163.78 9.54 1
-1 4 7 159.84 9.22 -2
0 -4 -7 159.84 9.22 1
-1 4 7 164.34 8.45 -2
0 -4 -7 164.34 8.45 1
-1 -4 7 188.60 9.71 -2
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1 -4 -7 206.01 9.71 -2
0 4 7 206.01 9.71 1
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-10 -12 3 34.08 7.35 1
-10 -12 2 0.72 6.39 1
-10 -12 2 -2.01 6.06 1
-10 -12 1 21.28 6.90 1
-10 -12 1 3.92 6.08 1
-10 12 0 7.11 6.86 -2
-10 -12 0 7.11 6.86 1
-10 12 0 -2.59 6.10 -2
-10 -12 0 -2.59 6.10 1
-10 -12 -1 6.41 6.75 1
-10 12 -2 11.68 6.46 1
-10 -13 2 19.49 7.02 1
-11 0 6 7.16 6.03 1
-11 0 5 25.97 6.83 1
-11 0 4 -0.61 6.07 1
-11 0 4 -11.07 5.96 1
-11 0 3 99.20 9.30 1
-11 0 3 93.31 8.92 1
-11 0 2 -3.68 6.15 1
-11 0 2 -1.19 5.77 1
-11 0 1 141.44 10.77 1
-11 0 1 124.55 10.16 1
-11 0 0 -2.44 6.04 -2
-11 0 0 -2.44 6.04 1
-11 0 0 2.44 5.74 -2
-11 0 0 2.44 5.74 1
-11 0 -1 93.97 9.42 1
-11 0 -1 112.03 9.67 1
-11 0 -2 -3.17 5.97 1
-11 0 -2 -2.40 5.80 1
-11 0 -3 35.79 7.46 1
-11 0 -3 46.62 7.40 1
-11 0 -4 4.01 6.08 1
-11 0 -5 -0.69 6.52 1
-11 -1 6 22.08 6.68 1
-11 1 5 17.92 6.46 1
-11 -1 5 30.76 6.88 1
-11 -1 5 30.52 6.36 1
-11 1 4 18.11 6.27 1
-11 -1 4 -3.65 5.86 1
-11 -1 4 7.75 5.63 1
-11 1 3 10.33 6.29 1
-11 -1 3 33.55 7.08 1
-11 1 3 17.74 6.25 1
-11 -1 3 20.45 6.19 1
-11 1 2 6.10 5.99 1
-11 -1 2 6.10 6.19 1
-11 1 2 4.05 5.64 1
-11 -1 2 5.45 6.01 1
-11 1 1 -0.61 6.09 1
-11 -1 1 -2.45 6.09 1
-11 1 1 1.18 5.69 1
-11 -1 1 -1.22 5.68 1
-11 1 0 3.06 6.11 -2
-11 -1 0 3.06 6.11 1
-11 -1 0 -5.40 6.17 -2
-11 1 0 -5.40 6.17 1
-11 1 0 3.72 6.06 -2
-11 -1 0 3.72 6.06 1
-11 -1 0 -1.83 6.07 -2
-11 1 0 -1.83 6.07 1
-11 -1 -1 4.86 6.08 1
-11 1 -1 -3.02 6.39 1
-11 1 -1 -3.67 5.95 1
-11 -1 -1 1.89 5.84 1
-11 -1 -2 18.64 6.22 1
-11 1 -2 13.15 6.37 1
-11 -1 -2 19.24 6.67 1
-11 1 -2 26.89 6.78 1
-11 1 -3 15.42 6.30 1
-11 -1 -3 35.45 6.67 1
-11 1 -3 19.36 6.56 1
-11 -1 -3 18.99 6.63 1
-11 1 -4 36.63 7.71 1
-11 -1 -4 49.13 7.67 1
-11 1 -4 34.69 6.98 1
-11 1 -5 8.90 6.44 1
-11 -1 -5 -1.38 6.27 1
-11 1 -6 19.61 7.15 1
-11 -2 6 20.50 6.56 1
-11 -2 6 25.44 6.72 1
-11 -2 5 -1.83 6.07 1
-11 2 5 13.62 6.31 1
-11 -2 5 4.94 5.64 1
-11 -2 4 30.00 6.83 1
-11 2 4 14.39 6.55 1
-11 -2 4 27.56 6.56 1
-11 -2 3 -1.23 6.25 1
-11 2 3 -1.81 6.13 1
-11 -2 3 1.23 5.64 1
-11 -2 2 99.71 9.45 1
-11 2 2 120.74 9.80 1
-11 -2 2 106.39 9.56 1
-11 -2 1 20.23 6.71 1
-11 2 1 42.51 7.27 1
-11 2 1 34.03 6.84 1
-11 -2 1 51.80 7.43 1
-11 2 0 70.09 8.46 -2
-11 -2 0 70.09 8.46 1
-11 -2 0 54.18 7.81 -2
-11 2 0 54.18 7.81 1
-11 2 0 83.40 8.53 -2
-11 -2 0 83.40 8.53 1
-11 -2 0 67.92 8.29 -2
-11 2 0 67.92 8.29 1
-11 -2 -1 14.66 6.51 1
-11 2 -1 7.24 6.27 1
-11 2 -1 12.63 6.24 1
-11 -2 -1 6.40 5.99 1
-11 -2 -2 44.60 7.28 1
-11 2 -2 40.18 7.16 1
-11 -2 -2 53.27 7.70 1
-11 2 -2 40.99 7.05 1
-11 -2 -3 -1.19 5.96 1
-11 2 -3 -4.47 6.37 1
-11 -2 -3 7.26 6.20 1
-11 2 -4 10.58 6.83 1
-11 -2 -4 27.06 7.17 1
-11 2 -5 5.46 6.55 1
-11 -2 -5 19.43 7.13 1
-10 3 -7 25.04 6.65 -2
-11 -3 7 25.04 6.65 1
-11 -3 6 19.62 6.40 1
-11 -3 6 7.67 6.01 1
-11 -3 5 3.09 6.20 1
-11 -3 5 2.54 5.79 1
-11 3 5 13.50 6.21 1
-11 -3 4 23.52 6.72 1
-11 -3 4 33.99 6.75 1
-11 3 4 14.28 6.26 1
-11 -3 3 -8.06 6.05 1
-11 3 3 0.60 6.06 1
-11 -3 3 5.64 5.89 1
-11 -3 2 -3.71 6.07 1
-11 3 2 3.02 5.98 1
-11 -3 2 4.42 5.89 1
-11 -3 1 -4.71 5.57 1
-11 -3 1 -3.08 6.27 1
-11 3 1 -5.45 6.36 1
-11 -3 1 6.35 6.16 1
-11 3 0 21.35 6.14 -2
-11 -3 0 21.35 6.14 1
-11 3 0 27.04 6.66 -2
-11 -3 0 27.04 6.66 1
-11 -3 0 14.00 6.37 -2
-11 3 0 14.00 6.37 1
-11 -3 0 16.12 5.85 -2
-11 3 0 16.12 5.85 1
-11 3 0 21.79 6.85 -2
-11 -3 0 21.79 6.85 1
-11 -3 -1 19.65 6.21 1
-11 -3 -1 7.90 6.25 1
-11 3 -1 10.06 5.97 1
-11 -3 -1 14.26 6.70 1
-11 3 -1 19.55 6.43 1
-11 -3 -2 9.65 6.29 1
-11 -3 -2 13.92 6.15 1
-11 3 -2 5.51 5.79 1
-11 -3 -2 13.80 6.27 1
-11 -3 -3 24.96 6.73 1
-11 -3 -3 19.11 6.47 1
-11 3 -3 24.10 6.98 1
-11 -3 -3 34.62 6.78 1
-11 -3 -4 14.68 6.44 1
-11 3 -4 19.66 6.63 1
-11 -3 -4 10.83 6.59 1
-11 -3 -5 69.92 8.27 1
-11 3 -5 51.72 8.12 1
-11 3 -5 46.08 8.03 1
-11 -3 -5 50.57 7.94 1
-10 4 -7 25.71 6.88 -2
-11 -4 7 25.71 6.88 1
-11 -4 6 -1.97 6.08 1
-11 -4 5 6.36 6.02 1
-11 4 5 5.27 5.96 1
-11 -4 5 12.36 6.18 1
-11 -4 4 5.62 5.91 1
-11 4 4 -0.59 5.96 1
-11 -4 4 3.88 5.79 1
-11 -4 3 9.91 6.09 1
-11 4 3 11.45 6.32 1
-11 -4 3 2.55 5.93 1
-11 -4 2 40.99 7.28 1
-11 -4 2 45.74 7.45 1
-11 -4 2 35.95 7.38 1
-11 4 2 32.85 7.00 1
-11 -4 1 27.43 6.64 1
-11 -4 1 33.59 6.87 1
-11 -4 1 18.71 6.47 1
-11 4 1 28.84 6.84 1
-11 4 0 72.55 8.37 -2
-11 -4 0 72.55 8.37 1
-11 4 0 61.04 7.86 -2
-11 -4 0 61.04 7.86 1
-11 4 0 65.56 8.06 -2
-11 -4 0 65.56 8.06 1
-11 -4 -1 4.32 5.81 1
-11 -4 -1 7.95 5.94 1
-11 -4 -1 1.97 6.02 1
-11 -4 -2 7.51 5.96 1
-11 -4 -2 -7.23 6.24 1
-11 4 -2 -1.21 5.56 1
-11 -4 -2 -12.61 6.65 1
-11 -4 -3 33.89 6.95 1
-11 -4 -3 19.07 6.78 1
-11 4 -3 18.82 6.37 1
-11 -4 -3 24.80 6.83 1
-11 -4 -4 3.28 6.03 1
-11 4 -4 3.45 6.55 1
-11 4 -4 5.85 6.14 1
-11 -4 -4 3.40 6.18 1
-11 -4 -5 20.85 6.92 1
-11 4 -5 31.81 7.41 1
-11 4 -5 20.86 6.94 1
-10 5 -7 4.21 6.68 -2
-11 -5 7 4.21 6.68 1
-10 5 -7 1.35 6.12 -2
-11 -5 7 1.35 6.12 1
-11 -5 6 34.20 7.81 1
-11 -5 6 34.19 7.31 1
-11 -5 5 -1.97 6.19 1
-11 -5 5 -1.33 6.00 1
-11 -5 4 1.94 6.03 1
-11 -5 4 7.92 6.31 1
-11 -5 3 -6.41 5.95 1
-11 -5 3 -0.65 5.87 1
-11 -5 2 -6.34 6.07 1
-11 -5 2 1.96 6.07 1
-11 -5 1 -2.52 6.01 1
-11 -5 1 -6.55 6.34 1
-11 5 0 7.00 5.98 -2
-11 -5 0 7.00 5.98 1
-11 5 0 4.99 6.13 -2
-11 -5 0 4.99 6.13 1
-11 5 0 3.29 6.19 -2
-11 -5 0 3.29 6.19 1
-11 -5 -1 3.20 5.97 1
-11 -5 -1 5.54 6.16 1
-11 -5 -1 -2.65 5.97 1
-11 -5 -2 1.21 5.92 1
-11 -5 -2 1.94 6.09 1
-11 -5 -2 -5.36 6.15 1
-11 -5 -3 7.20 6.06 1
-11 5 -3 -1.24 5.86 1
-11 -5 -3 0.68 6.05 1
-11 -5 -4 18.81 6.56 1
-11 5 -4 25.60 7.70 1
-11 5 -4 7.72 6.43 1
-11 -5 -4 5.45 6.21 1
-11 5 -5 6.04 6.45 1
-10 6 -7 0.72 6.54 -2
-11 -6 7 0.72 6.54 1
-11 -6 6 6.30 6.95 1
-11 -6 6 15.75 6.74 1
-11 -6 5 0.68 6.37 1
-11 -6 5 20.39 6.78 1
-11 -6 4 17.38 6.96 1
-11 -6 4 10.10 6.63 1
-11 -6 3 41.73 7.56 1
-11 -6 3 37.98 7.69 1
-11 -6 2 -0.65 6.09 1
-11 -6 2 3.97 5.71 1
-11 -6 1 61.90 8.29 1
-11 -6 1 80.45 8.68 1
-11 6 0 -2.63 6.25 -2
-11 -6 0 -2.63 6.25 1
-11 6 0 10.00 6.22 -2
-11 -6 0 10.00 6.22 1
-11 -6 -1 33.60 6.98 1
-11 -6 -1 29.84 7.07 1
-11 -6 -1 39.54 7.33 1
-11 -6 -2 6.10 6.29 1
-11 -6 -2 7.99 6.16 1
-11 -6 -2 5.39 6.02 1
-11 -6 -3 25.57 6.91 1
-11 6 -3 5.51 6.78 1
-11 -6 -3 6.11 6.62 1
-11 -6 -4 15.84 7.08 1
-11 -6 -4 14.34 6.90 1
-11 -7 6 7.20 6.50 1
-11 -7 5 29.36 7.17 1
-11 -7 5 30.45 7.20 1
-11 -7 4 -0.69 6.45 1
-11 -7 4 5.49 6.19 1
-11 -7 3 -0.68 6.12 1
-11 -7 3 8.84 6.12 1
-11 -7 2 4.05 6.13 1
-11 -7 2 8.73 6.21 1
-11 -7 1 6.70 6.28 1
-11 -7 1 4.04 6.03 1
-11 7 0 16.88 6.56 -2
-11 -7 0 16.88 6.56 1
-11 7 0 26.26 6.95 -2
-11 -7 0 26.26 6.95 1
-11 -7 -1 10.83 6.53 1
-11 -7 -1 -0.67 6.01 1
-11 -7 -2 9.24 6.20 1
-11 -7 -2 0.68 6.45 1
-11 7 -2 4.76 6.70 1
-11 -7 -2 8.13 6.21 1
-11 -7 -3 17.25 6.82 1
-11 7 -3 14.43 6.89 1
-11 -7 -3 12.94 6.30 1
-11 -8 5 -5.02 6.40 1
-11 -8 4 16.23 7.05 1
-11 -8 4 9.75 6.52 1
-11 -8 3 -4.21 6.42 1
-11 -8 3 2.07 6.16 1
-11 -8 2 84.46 9.33 1
-11 -8 2 69.98 8.73 1
-11 -8 1 -3.44 6.36 1
-11 -8 1 -0.68 6.18 1
-11 8 0 83.18 8.88 -2
-11 -8 0 83.18 8.88 1
-11 -8 0 56.63 8.23 -2
-11 8 0 56.63 8.23 1
-11 8 0 67.92 8.66 -2
-11 -8 0 67.92 8.66 1
-11 -8 -1 2.78 6.23 1
-11 8 -1 -9.34 6.31 1
-11 -8 -1 0.68 6.23 1
-11 8 -2 55.50 8.28 1
-11 -8 -2 50.33 7.83 1
-11 -8 -3 2.73 6.26 1
-11 -9 3 4.31 6.48 1
-11 -9 3 -1.40 6.52 1
-11 -9 2 -7.09 6.42 1
-11 -9 2 7.55 6.28 1
-11 -9 1 -2.82 6.76 1
-11 -9 1 -3.43 6.15 1
-11 9 0 -0.71 6.20 -2
-11 -9 0 -0.71 6.20 1
-11 -9 0 1.29 6.14 -2
-11 9 0 1.29 6.14 1
-11 9 0 -1.37 6.55 -2
-11 -9 0 -1.37 6.55 1
-11 9 -1 -0.66 6.41 1
-11 -9 -1 -0.68 6.18 1
-12 0 5 -7.10 6.55 1
-12 0 4 45.67 7.77 1
-12 0 3 -0.66 6.41 1
-12 0 3 6.30 6.19 1
-12 0 2 -3.95 6.27 1
-12 0 2 0.64 6.04 1
-12 0 1 9.87 6.89 1
-12 0 1 1.29 6.22 1
-12 0 0 3.28 6.09 -2
-12 0 0 3.28 6.09 1
-12 0 0 8.52 6.49 -2
-12 0 0 8.52 6.49 1
-12 0 -1 -4.54 6.44 1
-12 0 -1 4.66 6.06 1
-12 0 -2 29.17 7.20 1
-12 0 -2 19.81 6.79 1
-12 1 5 9.60 6.61 1
-12 -1 5 -3.92 6.62 1
-12 -1 4 29.65 7.16 1
-12 1 4 33.70 7.30 1
-12 -1 4 40.33 7.24 1
-12 -1 3 41.70 7.60 1
-12 1 3 56.08 8.06 1
-12 -1 3 40.00 7.40 1
-12 -1 2 30.53 7.39 1
-12 1 2 30.73 7.38 1
-12 -1 2 20.83 6.77 1
-12 -1 1 54.21 8.11 1
-12 1 1 40.49 7.79 1
-12 1 1 47.59 7.52 1
-12 -1 1 53.98 7.80 1
-12 1 0 12.49 6.58 -2
-12 -1 0 12.49 6.58 1
-12 -1 0 12.89 6.42 -2
-12 1 0 12.89 6.42 1
-12 1 0 8.02 6.30 -2
-12 -1 0 8.02 6.30 1
-12 -1 0 14.32 6.57 -2
-12 1 0 14.32 6.57 1
-12 -1 -1 23.46 7.04 1
-12 1 -1 40.08 7.51 1
-12 1 -1 19.67 7.00 1
-12 -1 -1 29.09 7.14 1
-12 1 -2 26.33 7.09 1
-12 1 -2 27.53 7.07 1
-12 -1 -2 16.70 6.90 1
-12 2 5 22.80 6.92 1
-12 -2 5 20.14 6.71 1
-12 -2 4 7.88 6.35 1
-12 2 4 -0.64 6.29 1
-12 -2 4 10.47 6.43 1
-12 -2 3 18.46 7.16 1
-12 2 3 12.28 6.78 1
-12 -2 3 -2.63 6.40 1
-12 -2 2 5.97 6.42 1
-12 -2 2 -3.32 6.10 1
-12 2 2 -3.25 6.33 1
-12 -2 1 3.33 6.56 1
-12 2 1 -5.21 6.85 1
-12 -2 1 0.67 6.37 1
-12 2 0 -1.98 6.34 -2
-12 -2 0 -1.98 6.34 1
-12 -2 0 -0.65 6.34 -2
-12 2 0 -0.65 6.34 1
-12 -2 0 5.69 6.39 -2
-12 2 0 5.69 6.39 1
-12 2 0 4.74 6.41 -2
-12 -2 0 4.74 6.41 1
-12 -2 -1 -0.65 6.26 1
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-12 -2 -1 -10.29 6.61 1
-12 2 -1 3.90 6.29 1
-12 -2 -2 7.08 6.49 1
-12 2 -2 5.97 6.24 1
-12 3 4 15.93 6.55 1
-12 -3 4 21.36 6.65 1
-12 -3 3 0.67 6.54 1
-12 3 3 5.16 6.17 1
-12 -3 3 -1.34 6.00 1
-12 -3 2 55.96 8.36 1
-12 3 2 64.43 8.43 1
-12 -3 2 41.23 7.61 1
-12 -3 1 -1.32 6.41 1
-12 -3 1 0.68 6.08 1
-12 3 1 7.20 6.41 1
-12 3 0 57.50 8.21 -2
-12 -3 0 57.50 8.21 1
-12 3 0 44.61 7.72 -2
-12 -3 0 44.61 7.72 1
-12 -3 0 36.12 7.46 -2
-12 3 0 36.12 7.46 1
-12 -3 -1 9.85 6.55 1
-12 -3 -1 0.69 6.38 1
-12 -3 -2 3.23 6.35 1
-12 3 -2 2.62 5.94 1
-12 4 3 -4.55 6.67 1
-12 -4 3 3.42 6.24 1
-12 -4 2 1.34 6.64 1
-12 -4 2 -4.81 6.31 1
-12 -4 1 12.00 6.74 1
-12 -4 1 2.76 6.64 1
-12 4 0 -5.95 6.64 -2
-12 -4 0 -5.95 6.64 1
-12 4 0 9.03 6.66 -2
-12 -4 0 9.03 6.66 1
-12 -4 -1 0.65 6.49 1
-12 -5 2 16.55 6.87 1
-12 -5 1 29.30 7.25 1
-12 5 0 6.01 6.42 -2
-12 -5 0 6.01 6.42 1
-12 -5 -1 18.11 7.13 1
0 0 0 0.00 0.00 0
0 0 0
CELL 8.732111 15.244393 10.854535 90.0 94.9731 90.0
REM TWIN 1 0 0.1395 0 -1 0 0 0 -1
BASF 0.1722
HKLF 5
;
_shelx_hkl_checksum 89565
_shelx_res_file
;
TITL ni(cyclen([no3]2_2_auto_a.res in P2(1)/n
ni(cyclen([no3]2_2.res
created by SHELXL-2019/2 at 13:39:16 on 26-Aug-2024
REM Old TITL Ni(cyclen([NO3]2_2_auto in P2(1)/n
REM SHELXT solution in P2(1)/n
REM R1 0.124, Rweak 0.012, Alpha 0.057, Orientation as input
REM Formula found by SHELXT: C4 O10 Ni
CELL 0.71073 8.732111 15.244393 10.854535 90 94.9731 90
ZERR 4 0.000482 0.000937 0.000581 0 0.0052 0
LATT 1
SYMM 0.5-X,0.5+Y,0.5-Z
SFAC C H N Ni O
UNIT 32 80 24 4 24
EQIV $1 0.5-X,0.5+Y,1.5-Z
EQIV $2 1-X,1-Y,1-Z
EQIV $3 1+X,+Y,+Z
L.S. 30
PLAN 5
TEMP 19.85
CONF
HTAB N2 O4_$1
HTAB N5 O3_$2
HTAB N11 O4
HTAB N8 O5_$3
HTAB N8 O6_$3
MORE -1
BOND $H
fmap 2
acta
SHEL 15 0.8
OMIT -1 5 7
OMIT 1 5 7
OMIT 2 3 7
REM
REM
REM
WGHT 0.040600 0.878800
BASF 0.17700
FVAR 0.46686
NI1 4 0.474287 0.401780 0.718681 11.00000 0.02293 0.02942 =
0.02635 0.00140 0.00153 -0.00228
O1 5 0.664070 0.442902 0.844985 11.00000 0.03602 0.04988 =
0.03435 0.00177 0.00080 -0.00970
O2 5 0.855060 0.513912 0.773858 11.00000 0.02626 0.05935 =
0.10139 -0.00049 0.00092 -0.01733
O3 5 0.657172 0.472173 0.650034 11.00000 0.04137 0.04764 =
0.03546 0.00566 0.00567 -0.00927
N1 3 0.730338 0.477511 0.757542 11.00000 0.02916 0.03590 =
0.05334 -0.00119 0.00355 -0.00345
N2 3 0.323363 0.504600 0.747960 11.00000 0.03477 0.02898 =
0.03280 -0.00208 0.00048 -0.00169
AFIX 13
H2 2 0.381537 0.558870 0.764991 11.00000 -1.20000
AFIX 0
N5 3 0.343989 0.383119 0.554656 11.00000 0.02762 0.03256 =
0.02734 0.00255 0.00203 -0.00055
AFIX 13
H5 2 0.392730 0.413234 0.488510 11.00000 -1.20000
AFIX 0
N8 3 0.561483 0.276186 0.690949 11.00000 0.02213 0.03636 =
0.03530 0.00055 0.00233 0.00227
AFIX 13
H8 2 0.674094 0.277112 0.700910 11.00000 -1.20000
AFIX 0
N11 3 0.350761 0.338502 0.846116 11.00000 0.02713 0.03397 =
0.02840 0.00290 0.00279 0.00073
AFIX 13
H11 2 0.255201 0.314213 0.805949 11.00000 -1.20000
AFIX 0
C1 1 0.236157 0.481839 0.856256 11.00000 0.03812 0.05043 =
0.03747 -0.00781 0.00745 0.00941
AFIX 23
H1A 2 0.133206 0.462931 0.827328 11.00000 -1.20000
H1B 2 0.227560 0.533312 0.907739 11.00000 -1.20000
AFIX 0
C3 1 0.224327 0.513548 0.630457 11.00000 0.04122 0.03713 =
0.03975 0.00384 -0.00087 0.01023
AFIX 23
H3A 2 0.274368 0.551436 0.574398 11.00000 -1.20000
H3B 2 0.127546 0.540508 0.646862 11.00000 -1.20000
AFIX 0
C4 1 0.193729 0.424882 0.570325 11.00000 0.03089 0.04495 =
0.03177 -0.00170 -0.00252 0.00556
AFIX 23
H4A 2 0.134359 0.388525 0.621993 11.00000 -1.20000
H4B 2 0.135815 0.431978 0.490575 11.00000 -1.20000
AFIX 0
C6 1 0.344134 0.287287 0.531069 11.00000 0.03458 0.04071 =
0.02762 -0.00564 0.00123 -0.00120
AFIX 23
H6A 2 0.310735 0.275553 0.445087 11.00000 -1.20000
H6B 2 0.274129 0.258079 0.582361 11.00000 -1.20000
AFIX 0
C7 1 0.506703 0.253409 0.561392 11.00000 0.04064 0.03791 =
0.03781 -0.00633 0.00669 0.00382
AFIX 23
H7A 2 0.508492 0.190241 0.550862 11.00000 -1.20000
H7B 2 0.574574 0.279217 0.505188 11.00000 -1.20000
AFIX 0
C9 1 0.501273 0.216368 0.783208 11.00000 0.03661 0.03121 =
0.04531 0.00611 0.00063 0.00649
AFIX 23
H9A 2 0.579747 0.173954 0.810634 11.00000 -1.20000
H9B 2 0.413183 0.184602 0.745263 11.00000 -1.20000
AFIX 0
C10 1 0.454357 0.267777 0.893394 11.00000 0.04395 0.03958 =
0.03594 0.01124 0.00271 -0.00321
AFIX 23
H10A 2 0.402253 0.229681 0.947894 11.00000 -1.20000
H10B 2 0.544393 0.292262 0.939630 11.00000 -1.20000
AFIX 0
C12 1 0.317706 0.408987 0.931983 11.00000 0.03911 0.04513 =
0.03139 -0.00038 0.00883 -0.00450
AFIX 23
H12A 2 0.412467 0.430823 0.974336 11.00000 -1.20000
H12B 2 0.252712 0.387293 0.993362 11.00000 -1.20000
AFIX 0
O4 5 0.114625 0.204236 0.748694 11.00000 0.03088 0.06363 =
0.10452 0.00524 0.00664 0.00289
O5 5 -0.066947 0.298372 0.730187 11.00000 0.08689 0.04549 =
0.12753 0.02036 0.04502 0.02549
O6 5 -0.119354 0.163014 0.728631 11.00000 0.05371 0.07453 =
0.11348 -0.02631 0.01152 -0.02893
N3 3 -0.025210 0.222108 0.734323 11.00000 0.03660 0.04433 =
0.03944 0.00037 0.00921 -0.00105
HKLF 5
REM ni(cyclen([no3]2_2_auto_a.res in P2(1)/n
REM wR2 = 0.1044, GooF = S = 1.086, Restrained GooF = 1.086 for all data
REM R1 = 0.0362 for 9604 Fo > 4sig(Fo) and 0.0534 for all 12195 data
REM 191 parameters refined using 0 restraints
END
WGHT 0.0397 0.8752
REM Highest difference peak 0.385, deepest hole -0.279, 1-sigma level 0.065
Q1 1 0.0254 0.2989 0.7812 11.00000 0.05 0.39
Q2 1 0.0592 0.1772 0.6656 11.00000 0.05 0.29
Q3 1 -0.0681 0.1553 0.7784 11.00000 0.05 0.27
Q4 1 0.3282 0.5408 0.7602 11.00000 0.05 0.26
Q5 1 0.3445 0.4463 0.7281 11.00000 0.05 0.25
;
_shelx_res_checksum 62206
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
Ni Ni1 0.47429(5) 0.40178(3) 0.71868(4) 0.02627(16) Uani d 1 . .
O O1 0.6641(3) 0.44290(18) 0.8450(2) 0.0402(7) Uani d 1 . .
O O2 0.8551(3) 0.5139(2) 0.7739(3) 0.0626(10) Uani d 1 . .
O O3 0.6572(3) 0.47217(18) 0.6500(2) 0.0414(8) Uani d 1 . .
N N1 0.7303(4) 0.4775(2) 0.7575(3) 0.0395(9) Uani d 1 . .
N N2 0.3234(4) 0.5046(2) 0.7480(3) 0.0323(8) Uani d 1 . .
H H2 0.381537 0.558870 0.764991 0.039 Uiso calc 1 . .
N N5 0.3440(3) 0.38312(19) 0.5547(3) 0.0292(8) Uani d 1 . .
H H5 0.392730 0.413234 0.488510 0.035 Uiso calc 1 . .
N N8 0.5615(3) 0.2762(2) 0.6909(3) 0.0313(8) Uani d 1 . .
H H8 0.674094 0.277112 0.700910 0.038 Uiso calc 1 . .
N N11 0.3508(3) 0.3385(2) 0.8461(3) 0.0298(8) Uani d 1 . .
H H11 0.255201 0.314213 0.805949 0.036 Uiso calc 1 . .
C C1 0.2362(5) 0.4818(3) 0.8563(4) 0.0418(11) Uani d 1 . .
H H1A 0.133206 0.462931 0.827328 0.050 Uiso calc 1 . .
H H1B 0.227560 0.533312 0.907739 0.050 Uiso calc 1 . .
C C3 0.2243(5) 0.5135(3) 0.6305(4) 0.0396(11) Uani d 1 . .
H H3A 0.274368 0.551436 0.574398 0.048 Uiso calc 1 . .
H H3B 0.127546 0.540508 0.646862 0.048 Uiso calc 1 . .
C C4 0.1937(4) 0.4249(3) 0.5703(4) 0.0362(10) Uani d 1 . .
H H4A 0.134359 0.388525 0.621993 0.043 Uiso calc 1 . .
H H4B 0.135815 0.431978 0.490575 0.043 Uiso calc 1 . .
C C6 0.3441(4) 0.2873(3) 0.5311(3) 0.0344(10) Uani d 1 . .
H H6A 0.310735 0.275553 0.445087 0.041 Uiso calc 1 . .
H H6B 0.274129 0.258079 0.582361 0.041 Uiso calc 1 . .
C C7 0.5067(5) 0.2534(3) 0.5614(4) 0.0386(11) Uani d 1 . .
H H7A 0.508492 0.190241 0.550862 0.046 Uiso calc 1 . .
H H7B 0.574574 0.279217 0.505188 0.046 Uiso calc 1 . .
C C9 0.5013(5) 0.2164(3) 0.7832(4) 0.0379(11) Uani d 1 . .
H H9A 0.579747 0.173954 0.810634 0.045 Uiso calc 1 . .
H H9B 0.413183 0.184602 0.745263 0.045 Uiso calc 1 . .
C C10 0.4544(5) 0.2678(3) 0.8934(4) 0.0399(11) Uani d 1 . .
H H10A 0.402253 0.229681 0.947894 0.048 Uiso calc 1 . .
H H10B 0.544393 0.292262 0.939630 0.048 Uiso calc 1 . .
C C12 0.3177(5) 0.4090(3) 0.9320(3) 0.0382(10) Uani d 1 . .
H H12A 0.412467 0.430823 0.974336 0.046 Uiso calc 1 . .
H H12B 0.252712 0.387293 0.993362 0.046 Uiso calc 1 . .
O O4 0.1146(4) 0.2042(2) 0.7487(3) 0.0663(10) Uani d 1 . .
O O5 -0.0669(4) 0.2984(2) 0.7302(4) 0.0846(13) Uani d 1 . .
O O6 -0.1194(4) 0.1630(2) 0.7286(4) 0.0803(12) Uani d 1 . .
N N3 -0.0252(4) 0.2221(3) 0.7343(3) 0.0398(9) 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
Ni1 0.0229(3) 0.0294(3) 0.0263(3) -0.0023(3) 0.0015(2) 0.0014(3)
O1 0.0360(17) 0.050(2) 0.0343(16) -0.0097(15) 0.0008(13) 0.0018(14)
O2 0.0263(17) 0.059(2) 0.101(3) -0.0173(17) 0.0009(18) 0.000(2)
O3 0.0414(17) 0.048(2) 0.0355(16) -0.0093(16) 0.0057(14) 0.0057(15)
N1 0.029(2) 0.036(2) 0.053(2) -0.0034(18) 0.0035(18) -0.0012(19)
N2 0.0348(19) 0.0290(19) 0.0328(18) -0.0017(17) 0.0005(15) -0.0021(16)
N5 0.0276(18) 0.033(2) 0.0273(17) -0.0006(16) 0.0020(14) 0.0025(15)
N8 0.0221(17) 0.036(2) 0.0353(19) 0.0023(16) 0.0023(15) 0.0006(16)
N11 0.0271(18) 0.034(2) 0.0284(18) 0.0007(16) 0.0028(14) 0.0029(16)
C1 0.038(3) 0.050(3) 0.037(2) 0.009(2) 0.007(2) -0.008(2)
C3 0.041(3) 0.037(3) 0.040(2) 0.010(2) -0.001(2) 0.004(2)
C4 0.031(2) 0.045(3) 0.032(2) 0.006(2) -0.0025(18) -0.002(2)
C6 0.035(2) 0.041(3) 0.028(2) -0.001(2) 0.0012(18) -0.006(2)
C7 0.041(3) 0.038(3) 0.038(2) 0.004(2) 0.007(2) -0.006(2)
C9 0.037(3) 0.031(2) 0.045(2) 0.006(2) 0.001(2) 0.006(2)
C10 0.044(3) 0.040(3) 0.036(2) -0.003(2) 0.003(2) 0.011(2)
C12 0.039(2) 0.045(3) 0.031(2) -0.004(2) 0.0088(19) 0.000(2)
O4 0.0309(18) 0.064(2) 0.105(3) 0.0029(18) 0.0066(19) 0.005(2)
O5 0.087(3) 0.045(2) 0.128(4) 0.025(2) 0.045(3) 0.020(2)
O6 0.054(2) 0.075(3) 0.113(3) -0.029(2) 0.012(2) -0.026(2)
N3 0.037(2) 0.044(3) 0.039(2) -0.001(2) 0.0092(18) 0.000(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'
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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O3 Ni1 O1 . . 60.82(10) ?
N2 Ni1 O1 . . 98.38(11) ?
N2 Ni1 O3 . . 100.29(12) ?
N2 Ni1 N8 . . 161.91(12) ?
N5 Ni1 O1 . . 159.07(12) ?
N5 Ni1 O3 . . 98.27(11) ?
N5 Ni1 N2 . . 85.77(12) ?
N5 Ni1 N8 . . 85.96(12) ?
N5 Ni1 N11 . . 103.55(12) ?
N8 Ni1 O1 . . 95.08(11) ?
N8 Ni1 O3 . . 96.80(11) ?
N11 Ni1 O1 . . 97.33(12) ?
N11 Ni1 O3 . . 158.13(11) ?
N11 Ni1 N2 . . 82.85(12) ?
N11 Ni1 N8 . . 83.49(12) ?
N1 O1 Ni1 . . 91.2(2) ?
N1 O3 Ni1 . . 92.5(2) ?
O1 N1 O3 . . 115.5(3) ?
O2 N1 O1 . . 122.6(4) ?
O2 N1 O3 . . 121.9(4) ?
Ni1 N2 H2 . . 109.8 ?
C1 N2 Ni1 . . 108.4(2) ?
C1 N2 H2 . . 109.8 ?
C3 N2 Ni1 . . 105.5(2) ?
C3 N2 H2 . . 109.8 ?
C3 N2 C1 . . 113.5(3) ?
Ni1 N5 H5 . . 109.1 ?
C4 N5 Ni1 . . 105.7(2) ?
C4 N5 H5 . . 109.1 ?
C4 N5 C6 . . 117.2(3) ?
C6 N5 Ni1 . . 106.2(2) ?
C6 N5 H5 . . 109.1 ?
Ni1 N8 H8 . . 110.2 ?
C7 N8 Ni1 . . 105.0(2) ?
C7 N8 H8 . . 110.2 ?
C9 N8 Ni1 . . 108.1(2) ?
C9 N8 H8 . . 110.2 ?
C9 N8 C7 . . 113.0(3) ?
Ni1 N11 H11 . . 110.6 ?
C10 N11 Ni1 . . 103.6(2) ?
C10 N11 H11 . . 110.6 ?
C12 N11 Ni1 . . 103.1(2) ?
C12 N11 H11 . . 110.6 ?
C12 N11 C10 . . 117.6(3) ?
N2 C1 H1A . . 109.6 ?
N2 C1 H1B . . 109.6 ?
N2 C1 C12 . . 110.3(3) ?
H1A C1 H1B . . 108.1 ?
C12 C1 H1A . . 109.6 ?
C12 C1 H1B . . 109.6 ?
N2 C3 H3A . . 109.5 ?
N2 C3 H3B . . 109.5 ?
N2 C3 C4 . . 110.9(3) ?
H3A C3 H3B . . 108.1 ?
C4 C3 H3A . . 109.5 ?
C4 C3 H3B . . 109.5 ?
N5 C4 C3 . . 107.9(3) ?
N5 C4 H4A . . 110.1 ?
N5 C4 H4B . . 110.1 ?
C3 C4 H4A . . 110.1 ?
C3 C4 H4B . . 110.1 ?
H4A C4 H4B . . 108.4 ?
N5 C6 H6A . . 110.1 ?
N5 C6 H6B . . 110.1 ?
N5 C6 C7 . . 108.2(3) ?
H6A C6 H6B . . 108.4 ?
C7 C6 H6A . . 110.1 ?
C7 C6 H6B . . 110.1 ?
N8 C7 C6 . . 110.1(3) ?
N8 C7 H7A . . 109.6 ?
N8 C7 H7B . . 109.6 ?
C6 C7 H7A . . 109.6 ?
C6 C7 H7B . . 109.6 ?
H7A C7 H7B . . 108.2 ?
N8 C9 H9A . . 109.5 ?
N8 C9 H9B . . 109.5 ?
N8 C9 C10 . . 110.5(3) ?
H9A C9 H9B . . 108.1 ?
C10 C9 H9A . . 109.5 ?
C10 C9 H9B . . 109.5 ?
N11 C10 C9 . . 107.7(3) ?
N11 C10 H10A . . 110.2 ?
N11 C10 H10B . . 110.2 ?
C9 C10 H10A . . 110.2 ?
C9 C10 H10B . . 110.2 ?
H10A C10 H10B . . 108.5 ?
N11 C12 C1 . . 107.5(3) ?
N11 C12 H12A . . 110.2 ?
N11 C12 H12B . . 110.2 ?
C1 C12 H12A . . 110.2 ?
C1 C12 H12B . . 110.2 ?
H12A C12 H12B . . 108.5 ?
O5 N3 O4 . . 120.0(4) ?
O5 N3 O6 . . 120.4(4) ?
O6 N3 O4 . . 119.6(4) ?
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
Ni1 O1 . 2.151(3) ?
Ni1 O3 . 2.113(3) ?
Ni1 N2 . 2.090(3) ?
Ni1 N5 . 2.048(3) ?
Ni1 N8 . 2.092(3) ?
Ni1 N11 . 2.065(3) ?
O1 N1 . 1.269(4) ?
O2 N1 . 1.221(4) ?
O3 N1 . 1.283(4) ?
N2 H2 . 0.9800 ?
N2 C1 . 1.496(5) ?
N2 C3 . 1.484(4) ?
N5 H5 . 0.9800 ?
N5 C4 . 1.481(4) ?
N5 C6 . 1.483(4) ?
N8 H8 . 0.9800 ?
N8 C7 . 1.487(4) ?
N8 C9 . 1.484(4) ?
N11 H11 . 0.9800 ?
N11 C10 . 1.471(4) ?
N11 C12 . 1.467(4) ?
C1 H1A . 0.9700 ?
C1 H1B . 0.9700 ?
C1 C12 . 1.521(5) ?
C3 H3A . 0.9700 ?
C3 H3B . 0.9700 ?
C3 C4 . 1.515(5) ?
C4 H4A . 0.9700 ?
C4 H4B . 0.9700 ?
C6 H6A . 0.9700 ?
C6 H6B . 0.9700 ?
C6 C7 . 1.520(5) ?
C7 H7A . 0.9700 ?
C7 H7B . 0.9700 ?
C9 H9A . 0.9700 ?
C9 H9B . 0.9700 ?
C9 C10 . 1.516(5) ?
C10 H10A . 0.9700 ?
C10 H10B . 0.9700 ?
C12 H12A . 0.9700 ?
C12 H12B . 0.9700 ?
O4 N3 . 1.248(4) ?
O5 N3 . 1.218(4) ?
O6 N3 . 1.218(4) ?
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
N2 H2 O4 2_556 0.98 2.22 3.091(5) 147.2 yes
N5 H5 O3 3_666 0.98 2.32 3.130(4) 139.3 yes
N8 H8 O5 1_655 0.98 2.28 3.253(5) 172.4 yes
N8 H8 O6 1_655 0.98 2.50 3.273(5) 135.1 yes
N11 H11 O4 . 0.98 2.14 3.030(5) 150.6 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 O1 N1 O2 . . . . -179.3(3) ?
Ni1 O1 N1 O3 . . . . 1.0(3) ?
Ni1 O3 N1 O1 . . . . -1.0(3) ?
Ni1 O3 N1 O2 . . . . 179.3(3) ?
Ni1 N2 C1 C12 . . . . 17.8(4) ?
Ni1 N2 C3 C4 . . . . 34.8(4) ?
Ni1 N5 C4 C3 . . . . 45.1(3) ?
Ni1 N5 C6 C7 . . . . -43.1(3) ?
Ni1 N8 C7 C6 . . . . -38.1(4) ?
Ni1 N8 C9 C10 . . . . -22.5(4) ?
Ni1 N11 C10 C9 . . . . -53.5(3) ?
Ni1 N11 C12 C1 . . . . 55.7(3) ?
N2 C1 C12 N11 . . . . -50.0(4) ?
N2 C3 C4 N5 . . . . -55.3(4) ?
N5 C6 C7 N8 . . . . 56.3(4) ?
N8 C9 C10 N11 . . . . 52.0(4) ?
C1 N2 C3 C4 . . . . -83.8(4) ?
C3 N2 C1 C12 . . . . 134.6(3) ?
C4 N5 C6 C7 . . . . -160.9(3) ?
C6 N5 C4 C3 . . . . 163.1(3) ?
C7 N8 C9 C10 . . . . -138.3(3) ?
C9 N8 C7 C6 . . . . 79.5(4) ?
C10 N11 C12 C1 . . . . 168.9(3) ?
C12 N11 C10 C9 . . . . -166.4(3) ?
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.823(3)
2 0.177(3)