#------------------------------------------------------------------------------
#$Date: 2025-02-15 05:03:45 +0200 (Sat, 15 Feb 2025) $
#$Revision: 297755 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/57/39/1573925.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_1573925
loop_
_publ_author_name
'Khan, Sultana Shakila'
'Howlader, Md. Belayet Hossain'
'Sheikh, Md. Chanmiya'
'Miyatake, Ryuta'
'Zangrando, Ennio'
_publ_section_title
;
Bis{4-(allyloxy)-N′-[4-(octyloxy)benzylidene]benzohydrazidato}nickel(II)
;
_journal_coeditor_code BX4033
_journal_issue 2
_journal_name_full IUCrData
_journal_paper_doi 10.1107/S2414314625001208
_journal_volume 10
_journal_year 2025
_chemical_formula_iupac '[Ni (C25 H31 N2 O3)2]'
_chemical_formula_moiety 'C50 H62 N4 Ni O6'
_chemical_formula_sum 'C50 H62 N4 Ni O6'
_chemical_formula_weight 873.74
_chemical_name_common
Bis{4-(allyloxy)-N'-[4-(octyloxy)benzylidene]benzohydrazidato}nickel(II)
_chemical_name_systematic
Bis(N'-{[4-(octyloxy)phenyl]methylidene}-4-(prop-2-en-1-yloxy)benzohydrazidato)nickel(II)
_space_group_crystal_system triclinic
_space_group_IT_number 2
_space_group_name_Hall '-P 1'
_space_group_name_H-M_alt 'P -1'
_atom_sites_solution_hydrogens geom
_audit_creation_method SHELXL-2019/2
_cell_angle_alpha 86.599(6)
_cell_angle_beta 83.723(6)
_cell_angle_gamma 82.426(6)
_cell_formula_units_Z 1
_cell_length_a 5.5532(3)
_cell_length_b 12.0594(5)
_cell_length_c 17.0230(8)
_cell_measurement_reflns_used 8635
_cell_measurement_temperature 173(2)
_cell_measurement_theta_max 27.46
_cell_measurement_theta_min 2.04
_cell_volume 1122.11(10)
_computing_cell_refinement
;
RAPID-AUTO (Rigaku, 2010)
;
_computing_data_collection
;
RAPID-AUTO (Rigaku, 2010)
;
_computing_data_reduction
;
RAPID-AUTO (Rigaku, 2010)
;
_computing_molecular_graphics
;
CrystalStructure (Rigaku, 2019
;
_computing_structure_refinement
;
SHELXL2019/2 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT2014/5 (Sheldrick, 2015a)
;
_diffrn_ambient_temperature 173(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type 'Rigaku R-AXIS RAPID'
_diffrn_measurement_method \w
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71075
_diffrn_reflns_av_R_equivalents 0.0333
_diffrn_reflns_av_unetI/netI 0.0489
_diffrn_reflns_limit_h_max 6
_diffrn_reflns_limit_h_min -7
_diffrn_reflns_limit_k_max 15
_diffrn_reflns_limit_k_min -15
_diffrn_reflns_limit_l_max 22
_diffrn_reflns_limit_l_min -22
_diffrn_reflns_number 10908
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 27.459
_diffrn_reflns_theta_min 2.889
_exptl_absorpt_coefficient_mu 0.486
_exptl_absorpt_correction_T_max 0.990
_exptl_absorpt_correction_T_min 0.840
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
(ABSCOR; Rigaku, 1995)
;
_exptl_crystal_colour orange
_exptl_crystal_density_diffrn 1.293
_exptl_crystal_description platelet
_exptl_crystal_F_000 466
_exptl_crystal_size_max 0.140
_exptl_crystal_size_mid 0.070
_exptl_crystal_size_min 0.020
_refine_diff_density_max 0.389
_refine_diff_density_min -0.261
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.018
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 278
_refine_ls_number_reflns 5100
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.018
_refine_ls_R_factor_all 0.0661
_refine_ls_R_factor_gt 0.0441
_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^)+(0.0373P)^2^+0.4947P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0871
_refine_ls_wR_factor_ref 0.0944
_reflns_number_gt 4014
_reflns_number_total 5100
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file bx4033.cif
_cod_data_source_block I
_cod_original_cell_volume 1122.13(9)
_cod_database_code 1573925
_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 0.935
_shelx_estimated_absorpt_t_max 0.990
_shelx_hkl_file
;
0 0 3 49.82 0.90
0 0 -3 51.95 0.67
0 0 4 837.41 13.71
0 0 -4 821.62 13.62
0 0 5 166.54 1.96
0 0 -5 165.65 2.38
0 0 6 115.87 1.86
0 0 -6 117.73 1.57
0 0 7 232.33 2.96
0 0 -7 230.25 3.03
0 0 8 1057.69 22.12
0 0 -8 1050.60 23.16
0 0 9 119.03 1.94
0 0 9 120.72 1.81
0 0 -9 122.08 1.87
0 0 10 268.97 4.20
0 0 10 270.14 4.31
0 0 -10 267.99 3.99
0 0 11 27.23 1.14
0 0 11 25.41 0.93
0 0 -11 24.61 1.01
0 0 12 18.89 1.66
0 0 12 13.18 0.88
0 0 -12 12.15 1.48
0 0 13 132.53 2.62
0 0 13 130.03 2.90
0 0 -13 133.51 2.51
0 0 14 15.48 1.37
0 0 14 14.25 1.06
0 0 -14 13.11 1.18
0 0 15 26.06 1.58
0 0 15 24.48 1.22
0 0 -15 24.59 2.03
0 0 16 19.52 2.52
0 0 16 17.25 1.22
0 0 -16 16.92 1.41
0 0 17 20.14 1.79
0 0 17 18.28 1.92
0 0 -17 15.95 1.51
0 0 18 12.72 1.82
0 0 18 12.84 1.30
0 0 -18 11.47 1.58
0 0 19 8.66 2.00
0 0 19 7.77 1.40
0 0 -19 8.39 2.58
0 0 20 27.57 3.70
0 0 20 26.90 2.50
0 0 -20 26.03 2.05
0 0 21 45.06 2.86
0 0 21 37.72 1.94
0 0 -21 37.66 2.38
0 1 -21 18.92 2.19
0 -1 21 19.69 2.44
0 -1 21 21.46 1.81
0 1 -20 30.91 3.18
0 -1 20 30.48 2.41
0 -1 20 27.37 1.85
0 1 -19 11.48 1.75
0 -1 19 10.95 1.93
0 -1 19 10.21 2.31
0 1 -18 20.68 1.81
0 -1 18 19.35 2.84
0 -1 18 23.67 1.54
0 1 -17 39.72 2.66
0 -1 17 33.53 1.98
0 -1 17 38.15 1.60
0 1 -16 4.07 1.35
0 -1 16 3.53 1.41
0 -1 16 3.90 1.14
0 1 -15 35.56 1.60
0 -1 15 36.86 2.46
0 -1 15 34.06 2.03
0 1 -14 30.57 1.99
0 -1 14 35.78 1.49
0 -1 14 34.27 1.30
0 1 -13 6.07 1.09
0 -1 13 7.39 1.11
0 -1 13 8.05 0.96
0 1 -12 84.28 1.83
0 -1 12 88.54 1.72
0 1 -11 84.64 2.22
0 -1 11 82.38 2.06
0 1 -10 161.66 2.52
0 -1 10 163.19 2.43
0 1 -9 83.17 1.49
0 -1 9 80.12 1.39
0 1 -8 212.82 3.04
0 -1 8 219.14 2.95
0 1 -7 0.60 0.63
0 -1 7 -0.47 0.62
0 1 -6 2.03 0.99
0 -1 6 2.25 0.57
0 1 -5 17.34 0.68
0 -1 5 16.02 0.97
0 1 -4 950.88 18.12
0 -1 4 948.67 17.19
0 1 -3 77.11 0.97
0 -1 3 77.81 0.97
0 1 -2 48.72 0.60
0 -1 2 49.50 0.83
0 1 0 0.10 0.13
0 -1 0 -0.20 0.14
0 1 2 1200.00 23.42
0 1 2 1224.40 22.33
0 -1 -2 1207.64 23.50
0 -1 -2 1147.87 21.24
0 1 3 1023.27 19.54
0 1 3 1114.30 19.94
0 -1 -3 1016.89 19.36
0 -1 -3 1095.49 19.33
0 1 4 599.68 9.11
0 1 4 616.05 8.91
0 -1 -4 601.62 8.41
0 1 5 0.95 0.61
0 1 5 1.22 0.69
0 1 6 695.83 11.89
0 1 6 689.27 10.95
0 -1 -6 698.99 11.25
0 1 7 118.55 1.79
0 1 7 114.10 1.80
0 -1 -7 118.41 1.59
0 1 8 319.23 4.75
0 1 8 318.12 4.27
0 -1 -8 324.85 4.47
0 1 9 74.02 1.50
0 1 9 74.34 1.58
0 -1 -9 79.01 1.33
0 1 10 40.94 1.22
0 1 10 43.41 0.95
0 -1 -10 42.43 1.03
0 1 11 176.16 3.67
0 1 11 173.71 2.54
0 -1 -11 171.87 3.17
0 1 12 96.20 2.76
0 1 12 94.27 2.06
0 -1 -12 86.07 2.26
0 1 13 37.08 1.54
0 1 13 35.56 1.08
0 -1 -13 33.92 1.23
0 1 14 86.36 2.34
0 1 14 91.84 1.76
0 -1 -14 88.60 2.02
0 1 15 2.95 1.34
0 1 15 0.58 1.40
0 -1 -15 -1.74 1.10
0 1 16 28.83 1.86
0 1 16 31.72 1.34
0 -1 -16 25.79 2.21
0 1 17 40.83 3.14
0 1 17 38.75 1.47
0 -1 -17 36.74 1.73
0 1 18 1.66 1.72
0 1 18 3.26 1.75
0 -1 -18 2.19 1.40
0 1 19 16.63 2.18
0 1 19 17.38 1.41
0 -1 -19 18.13 1.74
0 1 20 -1.16 2.06
0 1 20 1.45 1.28
0 -1 -20 0.25 2.61
0 1 21 15.07 3.63
0 1 21 9.21 2.22
0 -1 -21 15.06 1.99
0 2 -21 10.31 2.14
0 -2 21 13.53 2.27
0 -2 21 11.51 1.78
0 2 -20 25.05 2.24
0 -2 20 29.41 3.42
0 -2 20 27.98 1.91
0 2 -19 6.29 2.82
0 -2 19 10.41 1.84
0 -2 19 11.77 1.57
0 2 -18 -0.88 1.59
0 -2 18 3.34 1.64
0 -2 18 3.59 2.09
0 2 -17 8.12 1.57
0 -2 17 9.31 2.36
0 -2 17 6.50 1.33
0 2 -16 -1.73 2.12
0 -2 16 -2.09 1.36
0 -2 16 0.75 1.20
0 2 -15 25.60 1.57
0 -2 15 24.37 1.53
0 -2 15 26.87 1.40
0 2 -14 39.89 1.61
0 -2 14 44.05 2.10
0 2 -13 61.62 2.40
0 -2 13 64.42 2.23
0 2 -12 44.15 1.42
0 -2 12 42.67 1.30
0 2 -11 0.68 0.92
0 -2 11 1.53 0.81
0 2 -10 10.94 1.43
0 -2 10 16.00 0.89
0 2 -9 335.82 5.19
0 -2 9 328.74 4.92
0 2 -8 311.95 5.38
0 -2 8 324.80 4.72
0 2 -7 290.18 4.08
0 -2 7 286.54 3.98
0 2 -6 40.67 1.34
0 -2 6 39.78 0.91
0 2 -5 6.23 0.64
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0 2 -4 37.55 0.84
0 -2 4 36.90 0.82
0 2 -3 -1.89 0.83
0 -2 3 -1.17 0.85
0 2 -2 1.30 0.65
0 -2 2 -0.24 0.67
0 2 -1 445.10 5.20
0 -2 1 437.02 5.11
0 2 0 577.46 7.14
0 -2 0 581.17 7.15
0 2 1 15.97 0.79
0 2 1 15.94 0.33
0 -2 -1 15.96 0.54
0 2 2 126.81 1.91
0 2 2 123.31 1.20
0 -2 -2 127.03 1.55
0 -2 -2 126.53 1.22
0 2 3 115.23 2.05
0 2 3 120.01 1.11
0 -2 -3 112.80 2.01
0 -2 -3 117.42 1.30
0 2 4 2.85 1.07
0 2 4 3.39 0.33
0 -2 -4 2.67 0.67
0 -2 -4 3.45 0.59
0 2 5 11.13 0.77
0 2 5 9.07 0.63
0 -2 -5 8.90 0.73
0 -2 -5 10.16 0.47
0 2 6 1.42 0.76
0 2 6 1.04 0.63
0 -2 -6 1.93 0.70
0 -2 -6 0.63 0.71
0 2 7 433.67 6.86
0 2 7 448.38 6.52
0 -2 -7 436.19 6.12
0 2 8 252.74 3.88
0 2 8 250.22 3.15
0 -2 -8 255.02 3.32
0 2 9 8.29 1.39
0 2 9 5.79 0.57
0 -2 -9 7.49 0.94
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0 2 10 159.79 2.19
0 -2 -10 160.85 2.77
0 2 11 113.07 2.94
0 2 11 103.23 2.02
0 -2 -11 110.32 2.28
0 2 12 82.04 2.78
0 2 12 81.25 1.47
0 -2 -12 83.52 1.67
0 2 13 138.52 2.92
0 2 13 121.04 2.55
0 -2 -13 134.62 2.35
0 2 14 102.56 2.57
0 2 14 103.00 1.91
0 -2 -14 103.16 2.10
0 2 15 7.73 1.49
0 2 15 8.24 0.92
0 -2 -15 7.19 1.11
0 2 16 36.09 2.02
0 2 16 38.18 1.33
0 -2 -16 35.16 2.17
0 2 17 36.60 2.09
0 2 17 34.07 1.33
0 -2 -17 27.80 2.47
0 2 18 29.45 3.27
0 2 18 31.24 2.06
0 -2 -18 30.93 1.76
0 2 19 19.91 2.29
0 2 19 17.38 1.29
0 -2 -19 14.01 1.70
0 2 20 12.97 2.18
0 2 20 9.47 1.36
0 -2 -20 11.51 2.59
0 2 21 3.88 2.35
0 2 21 2.56 2.05
0 -2 -21 3.12 1.71
0 3 -21 10.14 2.24
0 -3 21 14.13 2.21
0 -3 21 9.00 2.85
0 3 -20 8.76 3.12
0 -3 20 6.14 2.00
0 -3 20 5.86 2.67
0 3 -19 1.82 1.82
0 -3 19 1.65 1.53
0 3 -18 11.54 1.82
0 -3 18 9.59 1.76
0 -3 18 12.28 1.59
0 3 -17 13.14 2.57
0 -3 17 13.74 1.62
0 -3 17 17.12 1.49
0 3 -16 6.41 1.50
0 -3 16 6.80 2.00
0 3 -15 2.20 1.40
0 -3 15 3.93 1.22
0 3 -14 -0.62 1.94
0 -3 14 1.52 1.06
0 3 -13 60.79 1.83
0 -3 13 61.55 1.70
0 3 -12 14.05 1.75
0 -3 12 8.31 1.06
0 3 -11 24.41 1.23
0 -3 11 28.37 1.11
0 3 -10 3.74 0.92
0 -3 10 3.77 1.29
0 3 -9 99.98 2.38
0 -3 9 102.12 2.30
0 3 -8 120.80 1.97
0 -3 8 120.99 2.41
0 3 -7 291.03 4.88
0 -3 7 293.06 4.79
0 3 -6 111.73 1.74
0 -3 6 123.89 1.78
0 3 -5 63.10 1.14
0 -3 5 67.84 1.13
0 3 -4 19.42 0.71
0 -3 4 19.04 0.69
0 3 -3 107.26 1.38
0 -3 3 109.13 1.37
0 3 -2 196.06 2.33
0 -3 2 206.52 2.36
0 3 -1 1939.34 54.96
0 -3 1 1979.40 54.82
0 3 0 106.70 1.15
0 -3 0 105.12 1.39
0 3 1 9.42 0.31
0 -3 -1 8.65 0.77
0 -3 -1 8.76 0.33
0 3 2 128.06 1.81
0 3 2 128.52 1.12
0 3 2 129.26 1.26
0 -3 -2 125.27 1.78
0 3 3 106.87 1.62
0 3 3 106.47 1.23
0 -3 -3 106.70 1.57
0 3 4 36.19 1.44
0 3 4 33.67 0.67
0 -3 -4 32.93 0.96
0 -3 -4 35.88 0.71
0 3 5 3.27 1.23
0 3 5 3.69 0.35
0 -3 -5 5.68 1.14
0 -3 -5 5.24 0.60
0 3 6 11.34 0.91
0 3 6 12.62 0.44
0 -3 -6 9.73 1.18
0 -3 -6 11.78 0.73
0 3 7 513.43 7.20
0 -3 -7 503.10 9.08
0 -3 -7 513.88 7.88
0 3 8 2.11 0.90
0 3 8 2.27 0.45
0 -3 -8 3.27 0.77
0 -3 -8 0.90 0.52
0 3 9 31.11 1.21
0 3 9 32.05 0.72
0 -3 -9 34.57 1.13
0 3 10 44.58 1.49
0 3 10 40.98 1.14
0 -3 -10 45.57 1.34
0 3 11 26.39 1.37
0 -3 -11 22.84 0.89
0 3 12 6.82 1.27
0 3 12 8.55 1.03
0 -3 -12 7.15 0.84
0 3 13 51.83 1.85
0 3 13 49.95 1.16
0 -3 -13 49.59 1.34
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0 3 14 136.78 2.79
0 -3 -14 143.44 3.19
0 3 15 61.63 2.28
0 3 15 61.00 1.43
0 -3 -15 60.54 2.30
0 3 16 164.30 4.08
0 3 16 155.52 3.39
0 -3 -16 155.42 3.93
0 3 17 22.07 2.08
0 3 17 21.27 1.18
0 -3 -17 22.31 1.44
0 3 18 15.41 2.14
0 3 18 18.81 1.22
0 -3 -18 20.02 1.52
0 3 19 13.75 2.33
0 3 19 14.92 1.87
0 -3 -19 15.52 1.58
0 3 20 31.30 1.56
0 -3 -20 35.62 2.89
0 3 21 6.01 3.89
0 3 21 7.00 2.01
0 -3 -21 7.43 2.62
0 4 -20 -0.70 2.04
0 -4 20 1.32 2.87
0 -4 20 2.97 1.78
0 4 -19 16.07 2.17
0 -4 19 16.16 1.97
0 -4 19 23.65 2.71
0 4 -18 1.41 2.69
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0 4 -17 -1.50 1.59
0 -4 17 -1.39 1.46
0 4 -16 2.65 1.53
0 -4 16 0.05 1.36
0 4 -15 3.13 2.19
0 -4 15 0.76 1.25
0 4 -14 48.96 1.89
0 -4 14 52.06 2.47
0 4 -13 48.80 1.79
0 -4 13 49.77 2.32
0 4 -12 3.19 1.21
0 -4 12 6.02 1.65
0 4 -11 85.53 1.99
0 -4 11 86.87 1.86
0 4 -10 19.85 1.74
0 -4 10 26.39 1.11
0 4 -9 81.72 1.68
0 -4 9 81.68 1.62
0 4 -8 2.77 1.21
0 -4 8 0.29 0.80
0 4 -7 7.72 0.82
0 -4 7 12.69 1.18
0 4 -6 34.14 1.41
0 -4 6 33.97 1.34
0 4 -5 35.90 0.96
0 -4 5 37.23 0.91
0 4 -4 9.94 0.65
0 -4 4 11.82 0.64
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0 4 -2 8.10 0.52
0 -4 2 9.54 0.52
0 4 -1 1354.24 30.88
0 -4 1 1345.04 29.93
0 4 0 74.33 0.89
0 -4 0 74.38 0.87
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0 -4 -1 49.47 0.78
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0 4 2 88.95 0.86
0 -4 -2 89.60 1.43
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0 4 3 23.88 0.36
0 4 3 25.51 0.63
0 -4 -3 24.43 0.91
0 4 4 91.04 1.60
0 4 4 91.03 1.13
0 -4 -4 94.48 1.59
0 4 5 83.72 1.62
0 4 5 89.06 1.15
0 -4 -5 87.10 1.57
0 -4 -5 84.15 1.15
0 4 6 30.04 1.61
0 4 6 29.04 0.53
0 -4 -6 28.52 1.49
0 -4 -6 28.77 0.78
0 4 7 69.42 1.58
0 4 7 72.04 1.13
0 -4 -7 72.90 1.49
0 -4 -7 75.07 1.04
0 4 8 4.18 1.57
0 4 8 6.14 0.45
0 -4 -8 6.98 0.88
0 -4 -8 6.14 0.51
0 4 9 128.24 2.46
0 4 9 131.28 1.64
0 -4 -9 124.59 2.22
0 -4 -9 135.28 1.79
0 4 10 123.44 2.53
0 4 10 122.49 1.63
0 -4 -10 123.48 2.16
0 4 11 3.54 1.21
0 4 11 3.67 0.87
0 -4 -11 2.44 0.66
0 4 12 3.85 1.29
0 4 12 1.30 0.61
0 4 13 34.40 1.78
0 4 13 33.67 0.94
0 -4 -13 33.24 1.13
0 4 14 10.89 1.56
0 4 14 6.55 0.78
0 -4 -14 8.57 0.95
0 4 15 4.62 1.77
0 4 15 5.54 0.80
0 -4 -15 5.37 1.01
0 4 16 158.35 4.12
0 4 16 143.49 2.56
0 -4 -16 150.13 2.98
0 4 17 27.83 2.25
0 4 17 31.51 1.70
0 -4 -17 32.69 1.53
0 4 18 45.35 2.67
0 4 18 40.08 1.40
0 -4 -18 44.06 1.77
0 4 19 10.97 2.24
0 4 19 6.95 1.67
0 -4 -19 7.97 1.44
0 4 20 11.76 2.42
0 4 20 11.74 1.26
0 -4 -20 15.25 2.43
0 4 21 7.25 2.64
0 4 21 8.91 1.95
0 -4 -21 8.41 2.56
0 5 -20 6.88 2.23
0 -5 20 8.08 1.90
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-7 -1 -6 5.25 1.54
-7 -1 -6 -2.18 3.45
-7 -1 -7 12.00 2.40
-7 -1 -7 9.77 2.29
-7 -2 2 0.09 3.49
-7 -2 1 2.15 2.18
-7 -2 0 6.12 3.45
-7 -2 -1 3.42 2.09
-7 -2 -2 1.42 2.11
-7 -2 -3 0.33 2.10
-7 -2 -4 8.85 1.57
-7 -2 -4 11.88 2.22
-7 -2 -5 4.41 1.45
-7 -2 -5 5.09 3.29
-7 -2 -6 13.62 2.38
-7 -2 -6 14.26 2.32
-7 -2 -7 6.45 1.44
-7 -2 -7 3.97 2.13
-7 -3 2 5.07 2.27
-7 -3 1 8.72 3.41
-7 -3 0 20.28 2.38
-7 -3 -1 1.09 1.96
-7 -3 -2 0.92 3.10
-7 -3 -3 -0.16 1.95
-7 -3 -4 2.43 1.90
-7 -3 -4 0.14 1.37
-7 -3 -4 4.47 2.96
-7 -3 -5 0.37 1.85
-7 -3 -5 3.58 2.06
-7 -3 -5 4.54 1.98
-7 -3 -6 21.61 2.31
-7 -3 -6 18.41 2.25
-7 -3 -7 1.45 1.31
-7 -3 -7 4.39 3.01
-7 -4 1 7.18 3.34
-7 -4 0 5.43 2.05
-7 -4 -1 0.16 2.98
-7 -4 -2 11.78 2.05
-7 -4 -3 2.94 1.88
-7 -4 -4 3.68 1.45
-7 -4 -4 4.35 1.36
-7 -4 -4 3.81 1.93
-7 -4 -5 -0.26 1.38
-7 -4 -5 2.03 1.97
-7 -4 -5 2.18 1.84
-7 -4 -6 1.82 1.36
-7 -4 -6 1.30 1.28
-7 -4 -6 5.21 2.77
-7 -5 0 8.46 2.06
-7 -5 -1 13.27 3.22
-7 -5 -2 2.14 1.90
-7 -5 -3 4.39 2.85
-7 -5 -4 1.32 1.61
-7 -5 -4 0.56 1.77
-7 -5 -5 -0.22 2.42
-7 -5 -5 0.73 1.93
-7 -5 -5 -3.04 1.75
0 0 0 0.00 0.00
;
_shelx_hkl_checksum 45135
_shelx_res_file
;
TITL SH231
shelx.res
created by SHELXL-2019/2 at 09:39:47 on 17-Jan-2025
CELL 0.71075 5.55324 12.05945 17.02304 86.59900 83.72300 82.42600
ZERR 1 0.00026 0.00050 0.00081 0.00610 0.00590 0.00580
LATT 1
SFAC C H N NI O
UNIT 50 62 4 1 6
OMIT 0 1 0
L.S. 5
FMAP 2
PLAN 10
HTAB
BOND $H
CONF
ACTA
TEMP -100.0
SIZE 0.140 0.070 0.020
WGHT 0.037300 0.494700
FVAR 0.39997
NI1 4 1.000000 0.500000 1.000000 10.50000 0.02768 0.03295 =
0.01594 -0.00230 -0.00241 -0.00290
O2 5 1.315620 0.391781 0.514874 11.00000 0.03005 0.03224 =
0.01801 -0.00448 -0.00294 0.00329
O1 5 0.707500 0.589574 0.992377 11.00000 0.03230 0.03988 =
0.02208 -0.00120 -0.00445 -0.00451
O3 5 -0.175620 0.889932 0.843893 11.00000 0.04108 0.05403 =
0.03804 0.00178 -0.00496 0.01009
N1 3 0.993558 0.487348 0.891406 11.00000 0.03070 0.03358 =
0.02217 -0.00254 -0.00202 -0.00332
N2 3 0.783666 0.543964 0.861720 11.00000 0.02915 0.03876 =
0.02291 -0.00261 -0.00409 -0.00029
C1 1 0.965722 -0.135426 0.303372 11.00000 0.06780 0.04535 =
0.05590 -0.00401 -0.02123 -0.02095
AFIX 137
H1A 2 0.924174 -0.061646 0.277505 11.00000 -1.20000
H1B 2 0.836194 -0.181922 0.298985 11.00000 -1.20000
H1C 2 1.120435 -0.171450 0.277660 11.00000 -1.20000
AFIX 0
C2 1 0.990940 -0.121956 0.389630 11.00000 0.03699 0.02816 =
0.04848 -0.00065 -0.00535 -0.00543
AFIX 23
H2A 2 1.016646 -0.197144 0.416317 11.00000 -1.20000
H2B 2 0.836226 -0.082433 0.414423 11.00000 -1.20000
AFIX 0
C3 1 1.199497 -0.057758 0.403388 11.00000 0.03859 0.02660 =
0.03999 0.00007 -0.00995 -0.00325
AFIX 23
H3A 2 1.351869 -0.093339 0.374511 11.00000 -1.20000
H3B 2 1.221544 -0.063783 0.460479 11.00000 -1.20000
AFIX 0
C4 1 1.160505 0.065733 0.377059 11.00000 0.03380 0.02540 =
0.03687 -0.00091 -0.01091 -0.00339
AFIX 23
H4A 2 1.144580 0.071857 0.319556 11.00000 -1.20000
H4B 2 1.005242 0.100830 0.404511 11.00000 -1.20000
AFIX 0
C5 1 1.365348 0.130032 0.393615 11.00000 0.03402 0.02756 =
0.03633 -0.00252 -0.00890 -0.00316
AFIX 23
H5A 2 1.516692 0.101308 0.360912 11.00000 -1.20000
H5B 2 1.395144 0.116517 0.449873 11.00000 -1.20000
AFIX 0
C6 1 1.309304 0.255466 0.376221 11.00000 0.03364 0.02552 =
0.02484 -0.00182 -0.00559 -0.00288
AFIX 23
H6A 2 1.156858 0.283582 0.408611 11.00000 -1.20000
H6B 2 1.279765 0.268496 0.319913 11.00000 -1.20000
AFIX 0
C7 1 1.510628 0.322943 0.392632 11.00000 0.03531 0.02569 =
0.02160 -0.00355 -0.00120 -0.00387
AFIX 23
H7A 2 1.667812 0.288387 0.366078 11.00000 -1.20000
H7B 2 1.476372 0.399690 0.369053 11.00000 -1.20000
AFIX 0
C8 1 1.537026 0.330395 0.479698 11.00000 0.02851 0.02647 =
0.02336 -0.00525 -0.00112 -0.00026
AFIX 23
H8A 2 1.562562 0.254437 0.505230 11.00000 -1.20000
H8B 2 1.678896 0.369471 0.486457 11.00000 -1.20000
AFIX 0
C9 1 1.289011 0.401521 0.595043 11.00000 0.02880 0.02030 =
0.01868 -0.00138 -0.00192 -0.00563
C10 1 1.066355 0.457834 0.625847 11.00000 0.02630 0.02885 =
0.02230 -0.00143 -0.00692 -0.00170
AFIX 43
H10 2 0.947015 0.486275 0.591372 11.00000 -1.20000
AFIX 0
C11 1 1.018045 0.472572 0.706259 11.00000 0.02480 0.02998 =
0.02277 -0.00356 -0.00201 0.00105
AFIX 43
H11 2 0.865513 0.510709 0.726758 11.00000 -1.20000
AFIX 0
C12 1 1.194374 0.431195 0.757924 11.00000 0.02713 0.02456 =
0.01994 -0.00205 -0.00267 -0.00404
C13 1 1.415657 0.376856 0.725351 11.00000 0.02762 0.02662 =
0.02327 -0.00047 -0.00825 -0.00219
AFIX 43
H13 2 1.536885 0.349306 0.759374 11.00000 -1.20000
AFIX 0
C14 1 1.465657 0.361449 0.644848 11.00000 0.02391 0.02523 =
0.02450 -0.00402 -0.00216 -0.00116
AFIX 43
H14 2 1.618655 0.323997 0.624127 11.00000 -1.20000
AFIX 0
C15 1 1.167344 0.440055 0.843775 11.00000 0.03253 0.03161 =
0.02067 -0.00140 -0.00404 -0.00511
AFIX 43
H15 2 1.303146 0.404296 0.869019 11.00000 -1.20000
AFIX 0
C16 1 0.649428 0.596090 0.920438 11.00000 0.03050 0.03401 =
0.02336 -0.00194 0.00032 -0.00895
C17 1 0.425683 0.670204 0.902490 11.00000 0.02952 0.03381 =
0.02550 -0.00146 -0.00173 -0.00767
C18 1 0.273174 0.723256 0.962311 11.00000 0.03484 0.04214 =
0.02375 -0.00252 -0.00215 -0.00714
AFIX 43
H18 2 0.308620 0.708848 1.015579 11.00000 -1.20000
AFIX 0
C19 1 0.067795 0.797695 0.945997 11.00000 0.03466 0.04316 =
0.03093 -0.00537 0.00186 -0.00251
AFIX 43
H19 2 -0.034176 0.834476 0.987607 11.00000 -1.20000
AFIX 0
C20 1 0.015021 0.817084 0.868436 11.00000 0.03440 0.03833 =
0.03449 0.00435 -0.00291 -0.00409
C21 1 0.163642 0.760763 0.807984 11.00000 0.04295 0.04915 =
0.02605 0.00102 -0.00614 0.00039
AFIX 43
H21 2 0.124748 0.772476 0.754906 11.00000 -1.20000
AFIX 0
C22 1 0.365602 0.688584 0.824963 11.00000 0.03958 0.04076 =
0.02361 -0.00134 -0.00006 -0.00159
AFIX 43
H22 2 0.465618 0.650708 0.783432 11.00000 -1.20000
AFIX 0
C23 1 -0.334948 0.951065 0.902350 11.00000 0.03893 0.04484 =
0.04678 -0.00226 -0.00344 0.00307
AFIX 23
H23A 2 -0.243037 0.999510 0.929629 11.00000 -1.20000
H23B 2 -0.408270 0.898833 0.942242 11.00000 -1.20000
AFIX 0
C24 1 -0.529601 1.020655 0.861099 11.00000 0.04505 0.04810 =
0.05619 -0.00466 -0.01295 0.00217
AFIX 43
H24 2 -0.606909 0.985027 0.824224 11.00000 -1.20000
AFIX 0
C25 1 -0.601541 1.125597 0.871513 11.00000 0.09199 0.05659 =
0.05195 -0.00388 -0.02344 0.01525
AFIX 93
H25A 2 -0.528832 1.164291 0.907875 11.00000 -1.20000
H25B 2 -0.727128 1.164038 0.842807 11.00000 -1.20000
AFIX 0
HKLF 4
REM SH231
REM wR2 = 0.0944, GooF = S = 1.018, Restrained GooF = 1.018 for all data
REM R1 = 0.0441 for 4014 Fo > 4sig(Fo) and 0.0661 for all 5100 data
REM 278 parameters refined using 0 restraints
END
WGHT 0.0373 0.4947
REM Instructions for potential hydrogen bonds
EQIV $1 -x+2, -y+1, -z+2
HTAB C15 O1_$1
REM Highest difference peak 0.389, deepest hole -0.261, 1-sigma level 0.057
Q1 1 1.1547 0.4378 0.9033 11.00000 0.05 0.39
Q2 1 1.3767 0.3774 0.9169 11.00000 0.05 0.34
Q3 1 1.1116 0.4571 0.7322 11.00000 0.05 0.33
Q4 1 1.0127 0.4594 0.9408 11.00000 0.05 0.32
Q5 1 1.1593 0.4286 0.7915 11.00000 0.05 0.31
Q6 1 1.0816 0.4839 0.6623 11.00000 0.05 0.31
Q7 1 0.9193 0.4841 1.0515 11.00000 0.05 0.29
Q8 1 0.5720 0.6382 1.0094 11.00000 0.05 0.28
Q9 1 1.5049 0.3396 0.4342 11.00000 0.05 0.28
Q10 1 1.3661 0.3784 0.6221 11.00000 0.05 0.28
;
_shelx_res_checksum 44638
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -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
Ni Ni1 1.000000 0.500000 1.000000 0.02555(11) Uani d 1 . .
O O2 1.3156(2) 0.39178(11) 0.51487(7) 0.0272(3) Uani d 1 . .
O O1 0.7075(2) 0.58957(11) 0.99238(7) 0.0313(3) Uani d 1 . .
O O3 -0.1756(3) 0.88993(14) 0.84389(9) 0.0459(4) Uani d 1 . .
N N1 0.9936(3) 0.48735(14) 0.89141(9) 0.0289(4) Uani d 1 . .
N N2 0.7837(3) 0.54396(14) 0.86172(9) 0.0305(4) Uani d 1 . .
C C1 0.9657(5) -0.1354(2) 0.30337(15) 0.0539(7) Uani d 1 . .
H H1A 0.924174 -0.061646 0.277505 0.065 Uiso calc 1 . .
H H1B 0.836194 -0.181922 0.298985 0.065 Uiso calc 1 . .
H H1C 1.120435 -0.171450 0.277660 0.065 Uiso calc 1 . .
C C2 0.9909(4) -0.12196(17) 0.38963(13) 0.0377(5) Uani d 1 . .
H H2A 1.016646 -0.197144 0.416317 0.045 Uiso calc 1 . .
H H2B 0.836226 -0.082433 0.414423 0.045 Uiso calc 1 . .
C C3 1.1995(4) -0.05776(16) 0.40339(12) 0.0348(5) Uani d 1 . .
H H3A 1.351869 -0.093339 0.374511 0.042 Uiso calc 1 . .
H H3B 1.221544 -0.063783 0.460479 0.042 Uiso calc 1 . .
C C4 1.1605(4) 0.06573(16) 0.37706(12) 0.0315(4) Uani d 1 . .
H H4A 1.144580 0.071857 0.319556 0.038 Uiso calc 1 . .
H H4B 1.005242 0.100830 0.404511 0.038 Uiso calc 1 . .
C C5 1.3653(4) 0.13003(16) 0.39362(12) 0.0323(4) Uani d 1 . .
H H5A 1.516692 0.101308 0.360912 0.039 Uiso calc 1 . .
H H5B 1.395144 0.116517 0.449873 0.039 Uiso calc 1 . .
C C6 1.3093(4) 0.25547(15) 0.37622(11) 0.0279(4) Uani d 1 . .
H H6A 1.156858 0.283582 0.408611 0.033 Uiso calc 1 . .
H H6B 1.279765 0.268496 0.319913 0.033 Uiso calc 1 . .
C C7 1.5106(4) 0.32294(16) 0.39263(10) 0.0276(4) Uani d 1 . .
H H7A 1.667812 0.288387 0.366078 0.033 Uiso calc 1 . .
H H7B 1.476372 0.399690 0.369053 0.033 Uiso calc 1 . .
C C8 1.5370(3) 0.33040(16) 0.47970(10) 0.0263(4) Uani d 1 . .
H H8A 1.562562 0.254437 0.505230 0.032 Uiso calc 1 . .
H H8B 1.678896 0.369471 0.486457 0.032 Uiso calc 1 . .
C C9 1.2890(3) 0.40152(14) 0.59504(10) 0.0224(4) Uani d 1 . .
C C10 1.0664(3) 0.45783(16) 0.62585(10) 0.0256(4) Uani d 1 . .
H H10 0.947015 0.486275 0.591372 0.031 Uiso calc 1 . .
C C11 1.0180(3) 0.47257(16) 0.70626(10) 0.0262(4) Uani d 1 . .
H H11 0.865513 0.510709 0.726758 0.031 Uiso calc 1 . .
C C12 1.1944(3) 0.43120(15) 0.75792(10) 0.0237(4) Uani d 1 . .
C C13 1.4157(3) 0.37686(15) 0.72535(10) 0.0256(4) Uani d 1 . .
H H13 1.536885 0.349306 0.759374 0.031 Uiso calc 1 . .
C C14 1.4657(3) 0.36145(15) 0.64485(10) 0.0246(4) Uani d 1 . .
H H14 1.618655 0.323997 0.624127 0.030 Uiso calc 1 . .
C C15 1.1673(4) 0.44005(16) 0.84378(10) 0.0281(4) Uani d 1 . .
H H15 1.303146 0.404296 0.869019 0.034 Uiso calc 1 . .
C C16 0.6494(4) 0.59609(17) 0.92044(11) 0.0291(4) Uani d 1 . .
C C17 0.4257(4) 0.67020(17) 0.90249(11) 0.0294(4) Uani d 1 . .
C C18 0.2732(4) 0.72326(18) 0.96231(11) 0.0334(5) Uani d 1 . .
H H18 0.308620 0.708848 1.015579 0.040 Uiso calc 1 . .
C C19 0.0678(4) 0.79769(18) 0.94600(12) 0.0367(5) Uani d 1 . .
H H19 -0.034176 0.834476 0.987607 0.044 Uiso calc 1 . .
C C20 0.0150(4) 0.81708(18) 0.86844(12) 0.0361(5) Uani d 1 . .
C C21 0.1636(4) 0.76076(19) 0.80798(12) 0.0399(5) Uani d 1 . .
H H21 0.124748 0.772476 0.754906 0.048 Uiso calc 1 . .
C C22 0.3656(4) 0.68858(18) 0.82496(11) 0.0352(5) Uani d 1 . .
H H22 0.465618 0.650708 0.783432 0.042 Uiso calc 1 . .
C C23 -0.3349(4) 0.9511(2) 0.90235(14) 0.0443(5) Uani d 1 . .
H H23A -0.243037 0.999510 0.929629 0.053 Uiso calc 1 . .
H H23B -0.408270 0.898833 0.942242 0.053 Uiso calc 1 . .
C C24 -0.5296(5) 1.0207(2) 0.86110(15) 0.0498(6) Uani d 1 . .
H H24 -0.606909 0.985027 0.824224 0.060 Uiso calc 1 . .
C C25 -0.6015(6) 1.1256(2) 0.87151(16) 0.0678(8) Uani d 1 . .
H H25A -0.528832 1.164291 0.907875 0.081 Uiso calc 1 . .
H H25B -0.727128 1.164038 0.842807 0.081 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
Ni1 0.0277(2) 0.0329(2) 0.01594(16) -0.00290(15) -0.00241(13) -0.00230(14)
O2 0.0301(7) 0.0322(7) 0.0180(6) 0.0033(6) -0.0029(5) -0.0045(5)
O1 0.0323(8) 0.0399(8) 0.0221(6) -0.0045(6) -0.0045(5) -0.0012(6)
O3 0.0411(9) 0.0540(10) 0.0380(8) 0.0101(8) -0.0050(7) 0.0018(7)
N1 0.0307(9) 0.0336(9) 0.0222(7) -0.0033(7) -0.0020(6) -0.0025(7)
N2 0.0291(9) 0.0388(9) 0.0229(8) -0.0003(7) -0.0041(7) -0.0026(7)
C1 0.0678(18) 0.0453(14) 0.0559(15) -0.0210(13) -0.0212(13) -0.0040(12)
C2 0.0370(12) 0.0282(11) 0.0485(12) -0.0054(9) -0.0053(10) -0.0006(9)
C3 0.0386(12) 0.0266(10) 0.0400(11) -0.0033(9) -0.0100(9) 0.0001(9)
C4 0.0338(11) 0.0254(10) 0.0369(10) -0.0034(8) -0.0109(9) -0.0009(8)
C5 0.0340(11) 0.0276(10) 0.0363(10) -0.0032(9) -0.0089(9) -0.0025(8)
C6 0.0336(11) 0.0255(10) 0.0248(9) -0.0029(8) -0.0056(8) -0.0018(8)
C7 0.0353(11) 0.0257(10) 0.0216(8) -0.0039(8) -0.0012(8) -0.0035(7)
C8 0.0285(10) 0.0265(9) 0.0234(8) -0.0003(8) -0.0011(7) -0.0053(7)
C9 0.0288(10) 0.0203(9) 0.0187(8) -0.0056(7) -0.0019(7) -0.0014(7)
C10 0.0263(10) 0.0288(10) 0.0223(8) -0.0017(8) -0.0069(7) -0.0014(7)
C11 0.0248(10) 0.0300(10) 0.0228(8) 0.0010(8) -0.0020(7) -0.0036(7)
C12 0.0271(10) 0.0246(9) 0.0199(8) -0.0040(8) -0.0027(7) -0.0021(7)
C13 0.0276(10) 0.0266(9) 0.0233(8) -0.0022(8) -0.0083(7) -0.0005(7)
C14 0.0239(10) 0.0252(9) 0.0245(8) -0.0012(8) -0.0022(7) -0.0040(7)
C15 0.0325(11) 0.0316(10) 0.0207(8) -0.0051(9) -0.0040(8) -0.0014(8)
C16 0.0305(11) 0.0340(10) 0.0234(9) -0.0090(8) 0.0003(8) -0.0019(8)
C17 0.0295(10) 0.0338(11) 0.0255(9) -0.0077(8) -0.0017(8) -0.0015(8)
C18 0.0348(12) 0.0421(12) 0.0237(9) -0.0071(9) -0.0021(8) -0.0025(8)
C19 0.0347(12) 0.0432(12) 0.0309(10) -0.0025(10) 0.0019(9) -0.0054(9)
C20 0.0344(12) 0.0383(12) 0.0345(10) -0.0041(9) -0.0029(9) 0.0043(9)
C21 0.0429(13) 0.0491(13) 0.0260(10) 0.0004(10) -0.0061(9) 0.0010(9)
C22 0.0396(12) 0.0408(12) 0.0236(9) -0.0016(10) -0.0001(8) -0.0013(8)
C23 0.0389(13) 0.0448(13) 0.0468(13) 0.0031(10) -0.0034(10) -0.0023(11)
C24 0.0450(14) 0.0481(14) 0.0562(15) 0.0022(11) -0.0129(12) -0.0047(12)
C25 0.092(2) 0.0566(17) 0.0520(15) 0.0152(16) -0.0234(15) -0.0039(13)
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
O1 Ni1 O1 . 2_767 180.00(8) ?
O1 Ni1 N1 . . 83.79(6) ?
O1 Ni1 N1 2_767 . 96.21(6) ?
O1 Ni1 N1 . 2_767 96.21(6) ?
O1 Ni1 N1 2_767 2_767 83.79(6) ?
N1 Ni1 N1 . 2_767 180.00(10) ?
C9 O2 C8 . . 118.00(13) ?
C16 O1 Ni1 . . 110.83(12) ?
C20 O3 C23 . . 118.14(17) ?
C15 N1 N2 . . 119.86(16) ?
C15 N1 Ni1 . . 126.02(14) ?
N2 N1 Ni1 . . 113.90(11) ?
C16 N2 N1 . . 107.83(15) ?
C2 C1 H1A . . 109.5 ?
C2 C1 H1B . . 109.5 ?
H1A C1 H1B . . 109.5 ?
C2 C1 H1C . . 109.5 ?
H1A C1 H1C . . 109.5 ?
H1B C1 H1C . . 109.5 ?
C1 C2 C3 . . 113.89(19) ?
C1 C2 H2A . . 108.8 ?
C3 C2 H2A . . 108.8 ?
C1 C2 H2B . . 108.8 ?
C3 C2 H2B . . 108.8 ?
H2A C2 H2B . . 107.7 ?
C2 C3 C4 . . 113.93(17) ?
C2 C3 H3A . . 108.8 ?
C4 C3 H3A . . 108.8 ?
C2 C3 H3B . . 108.8 ?
C4 C3 H3B . . 108.8 ?
H3A C3 H3B . . 107.7 ?
C5 C4 C3 . . 113.58(16) ?
C5 C4 H4A . . 108.9 ?
C3 C4 H4A . . 108.9 ?
C5 C4 H4B . . 108.9 ?
C3 C4 H4B . . 108.9 ?
H4A C4 H4B . . 107.7 ?
C4 C5 C6 . . 112.82(16) ?
C4 C5 H5A . . 109.0 ?
C6 C5 H5A . . 109.0 ?
C4 C5 H5B . . 109.0 ?
C6 C5 H5B . . 109.0 ?
H5A C5 H5B . . 107.8 ?
C5 C6 C7 . . 114.30(16) ?
C5 C6 H6A . . 108.7 ?
C7 C6 H6A . . 108.7 ?
C5 C6 H6B . . 108.7 ?
C7 C6 H6B . . 108.7 ?
H6A C6 H6B . . 107.6 ?
C8 C7 C6 . . 113.99(16) ?
C8 C7 H7A . . 108.8 ?
C6 C7 H7A . . 108.8 ?
C8 C7 H7B . . 108.8 ?
C6 C7 H7B . . 108.8 ?
H7A C7 H7B . . 107.7 ?
O2 C8 C7 . . 107.42(15) ?
O2 C8 H8A . . 110.2 ?
C7 C8 H8A . . 110.2 ?
O2 C8 H8B . . 110.2 ?
C7 C8 H8B . . 110.2 ?
H8A C8 H8B . . 108.5 ?
O2 C9 C14 . . 124.71(16) ?
O2 C9 C10 . . 115.20(15) ?
C14 C9 C10 . . 120.08(16) ?
C11 C10 C9 . . 120.45(16) ?
C11 C10 H10 . . 119.8 ?
C9 C10 H10 . . 119.8 ?
C10 C11 C12 . . 120.25(17) ?
C10 C11 H11 . . 119.9 ?
C12 C11 H11 . . 119.9 ?
C13 C12 C11 . . 117.96(16) ?
C13 C12 C15 . . 115.99(16) ?
C11 C12 C15 . . 126.05(17) ?
C14 C13 C12 . . 122.23(16) ?
C14 C13 H13 . . 118.9 ?
C12 C13 H13 . . 118.9 ?
C9 C14 C13 . . 119.02(17) ?
C9 C14 H14 . . 120.5 ?
C13 C14 H14 . . 120.5 ?
N1 C15 C12 . . 131.82(18) ?
N1 C15 H15 . . 114.1 ?
C12 C15 H15 . . 114.1 ?
O1 C16 N2 . . 123.60(18) ?
O1 C16 C17 . . 118.14(16) ?
N2 C16 C17 . . 118.20(16) ?
C18 C17 C22 . . 118.66(19) ?
C18 C17 C16 . . 120.56(17) ?
C22 C17 C16 . . 120.77(17) ?
C17 C18 C19 . . 121.30(18) ?
C17 C18 H18 . . 119.3 ?
C19 C18 H18 . . 119.3 ?
C20 C19 C18 . . 119.10(19) ?
C20 C19 H19 . . 120.4 ?
C18 C19 H19 . . 120.4 ?
O3 C20 C19 . . 125.21(19) ?
O3 C20 C21 . . 114.91(18) ?
C19 C20 C21 . . 119.9(2) ?
C22 C21 C20 . . 120.26(19) ?
C22 C21 H21 . . 119.9 ?
C20 C21 H21 . . 119.9 ?
C21 C22 C17 . . 120.74(19) ?
C21 C22 H22 . . 119.6 ?
C17 C22 H22 . . 119.6 ?
O3 C23 C24 . . 107.57(19) ?
O3 C23 H23A . . 110.2 ?
C24 C23 H23A . . 110.2 ?
O3 C23 H23B . . 110.2 ?
C24 C23 H23B . . 110.2 ?
H23A C23 H23B . . 108.5 ?
C25 C24 C23 . . 125.2(2) ?
C25 C24 H24 . . 117.4 ?
C23 C24 H24 . . 117.4 ?
C24 C25 H25A . . 120.0 ?
C24 C25 H25B . . 120.0 ?
H25A C25 H25B . . 120.0 ?
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
Ni1 O1 . 1.8409(14) ?
Ni1 O1 2_767 1.8410(14) ?
Ni1 N1 . 1.8685(15) ?
Ni1 N1 2_767 1.8685(15) ?
O2 C9 . 1.3669(19) ?
O2 C8 . 1.439(2) ?
O1 C16 . 1.295(2) ?
O3 C20 . 1.369(3) ?
O3 C23 . 1.428(3) ?
N1 C15 . 1.286(2) ?
N1 N2 . 1.399(2) ?
N2 C16 . 1.318(2) ?
C1 C2 . 1.510(3) ?
C1 H1A . 0.9800 ?
C1 H1B . 0.9800 ?
C1 H1C . 0.9800 ?
C2 C3 . 1.521(3) ?
C2 H2A . 0.9900 ?
C2 H2B . 0.9900 ?
C3 C4 . 1.524(3) ?
C3 H3A . 0.9900 ?
C3 H3B . 0.9900 ?
C4 C5 . 1.518(3) ?
C4 H4A . 0.9900 ?
C4 H4B . 0.9900 ?
C5 C6 . 1.522(3) ?
C5 H5A . 0.9900 ?
C5 H5B . 0.9900 ?
C6 C7 . 1.525(3) ?
C6 H6A . 0.9900 ?
C6 H6B . 0.9900 ?
C7 C8 . 1.514(2) ?
C7 H7A . 0.9900 ?
C7 H7B . 0.9900 ?
C8 H8A . 0.9900 ?
C8 H8B . 0.9900 ?
C9 C14 . 1.387(2) ?
C9 C10 . 1.394(3) ?
C10 C11 . 1.383(2) ?
C10 H10 . 0.9500 ?
C11 C12 . 1.410(2) ?
C11 H11 . 0.9500 ?
C12 C13 . 1.389(3) ?
C12 C15 . 1.462(2) ?
C13 C14 . 1.387(2) ?
C13 H13 . 0.9500 ?
C14 H14 . 0.9500 ?
C15 H15 . 0.9500 ?
C16 C17 . 1.481(3) ?
C17 C18 . 1.382(3) ?
C17 C22 . 1.394(3) ?
C18 C19 . 1.398(3) ?
C18 H18 . 0.9500 ?
C19 C20 . 1.383(3) ?
C19 H19 . 0.9500 ?
C20 C21 . 1.397(3) ?
C21 C22 . 1.372(3) ?
C21 H21 . 0.9500 ?
C22 H22 . 0.9500 ?
C23 C24 . 1.491(3) ?
C23 H23A . 0.9900 ?
C23 H23B . 0.9900 ?
C24 C25 . 1.292(4) ?
C24 H24 . 0.9500 ?
C25 H25A . 0.9500 ?
C25 H25B . 0.9500 ?
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
N1 Ni1 O1 C16 . . . . 0.87(13) ?
N1 Ni1 O1 C16 2_767 . . . -179.13(13) ?
O1 Ni1 N1 C15 . . . . 172.55(18) ?
O1 Ni1 N1 C15 2_767 . . . -7.45(18) ?
O1 Ni1 N1 N2 . . . . -2.05(13) ?
O1 Ni1 N1 N2 2_767 . . . 177.95(13) ?
C15 N1 N2 C16 . . . . -172.28(18) ?
Ni1 N1 N2 C16 . . . . 2.7(2) ?
C1 C2 C3 C4 . . . . 68.1(2) ?
C2 C3 C4 C5 . . . . 177.99(17) ?
C3 C4 C5 C6 . . . . -173.03(17) ?
C4 C5 C6 C7 . . . . 179.67(16) ?
C5 C6 C7 C8 . . . . -70.8(2) ?
C9 O2 C8 C7 . . . . 174.85(15) ?
C6 C7 C8 O2 . . . . -64.7(2) ?
C8 O2 C9 C14 . . . . 3.5(3) ?
C8 O2 C9 C10 . . . . -177.39(15) ?
O2 C9 C10 C11 . . . . 179.80(17) ?
C14 C9 C10 C11 . . . . -1.1(3) ?
C9 C10 C11 C12 . . . . 0.3(3) ?
C10 C11 C12 C13 . . . . 0.6(3) ?
C10 C11 C12 C15 . . . . -179.54(18) ?
C11 C12 C13 C14 . . . . -0.7(3) ?
C15 C12 C13 C14 . . . . 179.38(17) ?
O2 C9 C14 C13 . . . . 179.96(17) ?
C10 C9 C14 C13 . . . . 0.9(3) ?
C12 C13 C14 C9 . . . . 0.0(3) ?
N2 N1 C15 C12 . . . . -0.6(3) ?
Ni1 N1 C15 C12 . . . . -174.90(16) ?
C13 C12 C15 N1 . . . . 177.3(2) ?
C11 C12 C15 N1 . . . . -2.6(3) ?
Ni1 O1 C16 N2 . . . . 0.6(2) ?
Ni1 O1 C16 C17 . . . . -176.57(14) ?
N1 N2 C16 O1 . . . . -2.2(3) ?
N1 N2 C16 C17 . . . . 174.98(16) ?
O1 C16 C17 C18 . . . . -5.3(3) ?
N2 C16 C17 C18 . . . . 177.36(19) ?
O1 C16 C17 C22 . . . . 174.15(19) ?
N2 C16 C17 C22 . . . . -3.2(3) ?
C22 C17 C18 C19 . . . . -2.7(3) ?
C16 C17 C18 C19 . . . . 176.84(19) ?
C17 C18 C19 C20 . . . . 1.0(3) ?
C23 O3 C20 C19 . . . . -0.3(3) ?
C23 O3 C20 C21 . . . . -179.7(2) ?
C18 C19 C20 O3 . . . . -178.1(2) ?
C18 C19 C20 C21 . . . . 1.3(3) ?
O3 C20 C21 C22 . . . . 177.7(2) ?
C19 C20 C21 C22 . . . . -1.8(3) ?
C20 C21 C22 C17 . . . . 0.0(3) ?
C18 C17 C22 C21 . . . . 2.1(3) ?
C16 C17 C22 C21 . . . . -177.4(2) ?
C20 O3 C23 C24 . . . . -178.13(19) ?
O3 C23 C24 C25 . . . . -132.8(3) ?