#------------------------------------------------------------------------------
#$Date: 2020-07-06 06:02:36 +0300 (Mon, 06 Jul 2020) $
#$Revision: 253885 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/44/7704437.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7704437
loop_
_publ_author_name
'Elsberg, Josiah G. D.'
'Peterson, Austin'
'Fuller, Amy L.'
'Berreau, Lisa M.'
_publ_section_title
;
 N₃-Ligated nickel(ii) diketonate complexes: synthesis,
 characterization and evaluation of O₂ reactivity.
;
_journal_issue                   22
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              7564
_journal_page_last               7575
_journal_paper_doi               10.1039/d0dt01338b
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C26 H32 N3 Ni O3, Cl O4'
_chemical_formula_sum            'C26 H32 Cl N3 Ni O7'
_chemical_formula_weight         592.70
_chemical_name_systematic        '[(TERPY)NiTbutyl-diketonate]ClO4'
_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   mixed
_audit_creation_date             2020-03-24
_audit_creation_method
;
Olex2 1.3
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032)
;
_audit_update_record
;
2020-03-24 deposited with the CCDC.	2020-05-19 downloaded from the CCDC.
;
_cell_angle_alpha                110.337(3)
_cell_angle_beta                 91.439(2)
_cell_angle_gamma                113.304(3)
_cell_formula_units_Z            2
_cell_length_a                   9.9556(2)
_cell_length_b                   11.6346(4)
_cell_length_c                   14.2457(4)
_cell_measurement_reflns_used    10275
_cell_measurement_temperature    102(3)
_cell_measurement_theta_max      30.3610
_cell_measurement_theta_min      2.0780
_cell_volume                     1395.43(9)
_computing_cell_refinement       'CrysAlisPro 1.171.40.45a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.45a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.45a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      102(3)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.940
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -72.00 -23.00   0.50    3.45    --   20.00  54.00  30.00   98
  2  ω      0.00  38.00   0.50    3.45    --   20.00  54.00 150.00   76
  3  ω    -71.00  69.00   0.50    3.45    --   20.00  54.00 -30.00  280
  4  ω     75.00 110.00   0.50    3.45    --   20.00  54.00 -30.00   70
  5  ω    -72.00 -46.00   0.50    3.45    --   20.00  54.00-150.00   52
  6  ω    -28.00 110.00   0.50    3.45    --   20.00  54.00-150.00  276
  7  ω    -68.00 -40.00   0.50    3.45    --   20.00  54.00   0.00   56
  8  ω     -4.00  31.00   0.50    3.45    --   20.00  54.00   0.00   70
  9  ω     58.00  99.00   0.50    3.45    --   20.00  54.00   0.00   82
 10  ω    -72.00 -43.00   0.50    3.45    --   20.00  54.00-120.00   58
 11  ω      5.00 100.00   0.50    3.45    --   20.00  54.00-120.00  190
 12  ω    -74.00 -46.00   0.50    3.45    --   20.00  54.00 120.00   56
 13  ω     -1.00  24.00   0.50    3.45    --   20.00  54.00 120.00   50
 14  ω     35.00  60.00   0.50    3.45    --   20.00  54.00 120.00   50
 15  ω     85.00 110.00   0.50    3.45    --   20.00  54.00 120.00   50
 16  ω    -26.00  -1.00   0.50    3.45    --   20.00  54.00  60.00   50
 17  ω    -63.00 -36.00   0.50    3.45    --   20.00  54.00  54.96   54
 18  ω     -5.00  20.00   0.50    3.45    --   20.00  54.00  54.96   50
 19  ω     52.00  78.00   0.50    3.45    --   20.00  54.00  54.96   52
 20  ω    -64.00  82.00   0.50    3.45    --   20.00  54.00 -90.00  292
;
_diffrn_measurement_device       'two-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Mini II'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0115902000
_diffrn_orient_matrix_UB_12      0.0577074000
_diffrn_orient_matrix_UB_13      -0.0111528000
_diffrn_orient_matrix_UB_21      -0.0385521000
_diffrn_orient_matrix_UB_22      0.0205665000
_diffrn_orient_matrix_UB_23      0.0389200000
_diffrn_orient_matrix_UB_31      0.0679687000
_diffrn_orient_matrix_UB_32      0.0379539000
_diffrn_orient_matrix_UB_33      0.0358436000
_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  0.0289
_diffrn_reflns_av_unetI/netI     0.0381
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.940
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            25025
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.940
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.608
_diffrn_reflns_theta_min         2.268
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.839
_exptl_absorpt_correction_T_max  0.947
_exptl_absorpt_correction_T_min  0.828
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.45a (Rigaku Oxford Diffraction, 2019)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.411
_exptl_crystal_description       prism
_exptl_crystal_F_000             620
_exptl_crystal_preparation       'See Literature'
_exptl_crystal_recrystallization_method
'Crystallized in CH2Cl2 w one drop CH3CN and EtO2'
_exptl_crystal_size_max          0.369
_exptl_crystal_size_mid          0.229
_exptl_crystal_size_min          0.181
_refine_diff_density_max         0.413
_refine_diff_density_min         -0.536
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     355
_refine_ls_number_reflns         8096
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0434
_refine_ls_R_factor_gt           0.0329
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0338P)²+0.5155P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0774
_refine_ls_wR_factor_ref         0.0812
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6744
_reflns_number_total             8096
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d0dt01338b2.cif
_cod_data_source_block           usu_terpy_ni_tbutyl
_cod_depositor_comments
'Adding full bibliography for 7704434--7704437.cif.'
_cod_original_cell_volume        1395.42(8)
_cod_database_code               7704437
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Ni1 C26 H32 Cl1 O7 N3'
_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.
;
_reflns_odcompleteness_completeness 99.21
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C7(H7), C8(H8), C9(H9), C10(H10), C12(H12), C13(H13),
 C14(H14), C15(H15), C21(H21)
2.b Idealised Me refined as rotating group:
 C18(H18a,H18b,H18c), C19(H19a,H19b,H19c), C20(H20a,H20b,H20c), C24(H24a,H24b,
 H24c), C25(H25a,H25b,H25c), C26(H26a,H26b,H26c)
;
_olex2_exptl_crystal_mounting_method 'Mounted on a loop with paratone oil'
_olex2_submission_original_sample_id USU_TERPY_Ni_Tbutyl
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.093
_oxdiff_exptl_absorpt_empirical_full_min 0.940
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.78624(2) 0.56368(2) 0.71529(2) 0.01092(5) Uani 1 1 d . . . . .
O1 O 0.90305(12) 0.64117(11) 0.85660(8) 0.0153(2) Uani 1 1 d . . . . .
O2 O 0.66573(11) 0.66561(10) 0.76239(8) 0.0141(2) Uani 1 1 d . . . . .
O7 O 0.66416(12) 0.49864(11) 0.56619(8) 0.0137(2) Uani 1 1 d . . . . .
H7A H 0.659(2) 0.565(2) 0.5647(14) 0.020 Uiso 1 1 d . U . . .
H7B H 0.584(2) 0.442(2) 0.5550(14) 0.020 Uiso 1 1 d . U . . .
N1 N 0.89600(13) 0.44958(12) 0.66529(9) 0.0118(2) Uani 1 1 d . . . . .
N2 N 0.96638(13) 0.69136(12) 0.67176(9) 0.0124(2) Uani 1 1 d . . . . .
N3 N 0.64810(14) 0.38339(12) 0.73151(9) 0.0136(2) Uani 1 1 d . . . . .
C1 C 0.84382(16) 0.32634(14) 0.66986(11) 0.0129(3) Uani 1 1 d . . . . .
C2 C 0.92204(17) 0.24745(15) 0.64140(11) 0.0163(3) Uani 1 1 d . . . . .
H2 H 0.886311 0.162034 0.644252 0.020 Uiso 1 1 calc R U . . .
C3 C 1.05496(17) 0.29970(16) 0.60861(11) 0.0176(3) Uani 1 1 d . . . . .
H3 H 1.109334 0.248918 0.589502 0.021 Uiso 1 1 calc R U . . .
C4 C 1.10726(17) 0.42697(15) 0.60414(11) 0.0159(3) Uani 1 1 d . . . . .
H4 H 1.195746 0.461953 0.581688 0.019 Uiso 1 1 calc R U . . .
C5 C 1.02402(16) 0.50098(14) 0.63408(10) 0.0123(3) Uani 1 1 d . . . . .
C6 C 1.06346(16) 0.63930(14) 0.63606(10) 0.0126(3) Uani 1 1 d . . . . .
C7 C 1.18834(16) 0.71055(15) 0.60334(11) 0.0155(3) Uani 1 1 d . . . . .
H7 H 1.254314 0.673517 0.579653 0.019 Uiso 1 1 calc R U . . .
C8 C 1.21265(17) 0.83799(16) 0.60671(11) 0.0179(3) Uani 1 1 d . . . . .
H8 H 1.294924 0.887182 0.584613 0.021 Uiso 1 1 calc R U . . .
C9 C 1.11349(17) 0.89135(16) 0.64323(12) 0.0174(3) Uani 1 1 d . . . . .
H9 H 1.128263 0.976745 0.646263 0.021 Uiso 1 1 calc R U . . .
C10 C 0.99167(17) 0.81496(15) 0.67521(11) 0.0151(3) Uani 1 1 d . . . . .
H10 H 0.925129 0.850791 0.699940 0.018 Uiso 1 1 calc R U . . .
C11 C 0.70225(16) 0.28910(14) 0.70871(11) 0.0133(3) Uani 1 1 d . . . . .
C12 C 0.63092(17) 0.16833(15) 0.72234(11) 0.0163(3) Uani 1 1 d . . . . .
H12 H 0.669562 0.104446 0.705708 0.020 Uiso 1 1 calc R U . . .
C13 C 0.50070(18) 0.14481(16) 0.76132(12) 0.0189(3) Uani 1 1 d . . . . .
H13 H 0.451173 0.064951 0.771698 0.023 Uiso 1 1 calc R U . . .
C14 C 0.44522(17) 0.24108(16) 0.78461(12) 0.0195(3) Uani 1 1 d . . . . .
H14 H 0.358042 0.226960 0.810751 0.023 Uiso 1 1 calc R U . . .
C15 C 0.52170(17) 0.35893(16) 0.76833(12) 0.0171(3) Uani 1 1 d . . . . .
H15 H 0.483940 0.423382 0.783503 0.021 Uiso 1 1 calc R U . . .
C16 C 0.87534(16) 0.71187(14) 0.93656(11) 0.0130(3) Uani 1 1 d . . . . .
C17 C 0.97287(18) 0.74656(16) 1.03681(11) 0.0178(3) Uani 1 1 d . . . . .
C18 C 1.1248(2) 0.7515(2) 1.01629(14) 0.0307(4) Uani 1 1 d . . . . .
H18A H 1.111251 0.666362 0.964818 0.046 Uiso 1 1 calc R U . . .
H18B H 1.183962 0.768000 1.077904 0.046 Uiso 1 1 calc R U . . .
H18C H 1.174571 0.823297 0.993264 0.046 Uiso 1 1 calc R U . . .
C19 C 0.99749(19) 0.88304(18) 1.11996(12) 0.0245(4) Uani 1 1 d . . . . .
H19A H 1.037045 0.953416 1.094174 0.037 Uiso 1 1 calc R U . . .
H19B H 1.066494 0.903372 1.178149 0.037 Uiso 1 1 calc R U . . .
H19C H 0.904334 0.877720 1.139570 0.037 Uiso 1 1 calc R U . . .
C20 C 0.8918(2) 0.6313(2) 1.07268(14) 0.0342(4) Uani 1 1 d . . . . .
H20A H 0.798204 0.630750 1.087755 0.051 Uiso 1 1 calc R U . . .
H20B H 0.951901 0.645005 1.132867 0.051 Uiso 1 1 calc R U . . .
H20C H 0.874695 0.545903 1.019882 0.051 Uiso 1 1 calc R U . . .
C21 C 0.75918(17) 0.75257(16) 0.93932(11) 0.0174(3) Uani 1 1 d . . . . .
H21 H 0.746957 0.801273 1.003155 0.021 Uiso 1 1 calc R U . . .
C22 C 0.66098(16) 0.72645(14) 0.85506(11) 0.0123(3) Uani 1 1 d . . . . .
C23 C 0.53240(16) 0.76942(15) 0.86893(11) 0.0144(3) Uani 1 1 d . . . . .
C24 C 0.5461(2) 0.86090(19) 0.81061(14) 0.0254(4) Uani 1 1 d . . . . .
H24A H 0.637151 0.942477 0.839971 0.038 Uiso 1 1 calc R U . . .
H24B H 0.463169 0.883783 0.814882 0.038 Uiso 1 1 calc R U . . .
H24C H 0.546608 0.813773 0.740427 0.038 Uiso 1 1 calc R U . . .
C25 C 0.5294(2) 0.84368(19) 0.98014(12) 0.0253(4) Uani 1 1 d . . . . .
H25A H 0.517777 0.785381 1.016256 0.038 Uiso 1 1 calc R U . . .
H25B H 0.447578 0.868006 0.983483 0.038 Uiso 1 1 calc R U . . .
H25C H 0.621095 0.924375 1.010636 0.038 Uiso 1 1 calc R U . . .
C26 C 0.38590(18) 0.64045(18) 0.82210(15) 0.0266(4) Uani 1 1 d . . . . .
H26A H 0.387251 0.591543 0.752496 0.040 Uiso 1 1 calc R U . . .
H26B H 0.304140 0.664838 0.824536 0.040 Uiso 1 1 calc R U . . .
H26C H 0.374525 0.584160 0.859915 0.040 Uiso 1 1 calc R U . . .
Cl1 Cl 0.34196(4) 0.16538(3) 0.47535(3) 0.01395(7) Uani 1 1 d . . . . .
O3 O 0.35837(13) 0.30438(11) 0.50346(9) 0.0201(2) Uani 1 1 d . . . . .
O4 O 0.48690(13) 0.16786(13) 0.47643(11) 0.0324(3) Uani 1 1 d . . . . .
O5 O 0.25212(14) 0.08307(12) 0.37513(9) 0.0237(3) Uani 1 1 d . . . . .
O6 O 0.27086(15) 0.11416(13) 0.54740(10) 0.0299(3) Uani 1 1 d . . . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 '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_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 -15 5 0.1462
-7 -7 -4 0.1073
-10 0 -10 0.0928
-9 13 -14 0.1594
3 12 -1 0.1180
9 4 7 0.0823
7 0 14 0.1002
-6 -1 18 0.0955
-13 0 0 0.0889
-2 0 -18 0.0750
3 0 -19 0.0845
13 0 -6 0.1205
2 -7 20 0.1225
1 8 -20 0.1042
4 -12 17 0.1475
4 13 -10 0.1206
10 -13 11 0.1824
0 -14 0 0.1350
13 -11 -2 0.1647
0 -8 -11 0.1131
-5 -4 19 0.1111
11 0 6 0.1017
-6 3 17 0.0932
-10 14 2 0.1569
13 -4 -9 0.1290
7 -4 -16 0.1095
14 -4 0 0.1120
12 -3 9 0.1118
0 -2 19 0.1005
0 10 9 0.1086
10 -3 12 0.1048
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Ni1 O7 174.93(4) . . ?
O1 Ni1 N2 90.88(5) . . ?
O1 Ni1 N3 91.52(5) . . ?
O2 Ni1 O1 91.33(4) . . ?
O2 Ni1 O7 85.19(4) . . ?
O2 Ni1 N1 176.30(5) . . ?
O2 Ni1 N2 105.13(5) . . ?
O2 Ni1 N3 98.43(5) . . ?
N1 Ni1 O1 90.31(4) . . ?
N1 Ni1 O7 93.38(4) . . ?
N1 Ni1 N2 78.16(5) . . ?
N1 Ni1 N3 78.21(5) . . ?
N2 Ni1 O7 86.49(4) . . ?
N2 Ni1 N3 156.26(5) . . ?
N3 Ni1 O7 92.63(5) . . ?
C16 O1 Ni1 125.89(9) . . ?
C22 O2 Ni1 125.70(9) . . ?
Ni1 O7 H7A 104.9(14) . . ?
Ni1 O7 H7B 114.1(14) . . ?
H7A O7 H7B 108.2(19) . . ?
C1 N1 Ni1 118.95(9) . . ?
C5 N1 Ni1 119.20(10) . . ?
C5 N1 C1 121.72(12) . . ?
C6 N2 Ni1 114.57(9) . . ?
C10 N2 Ni1 126.59(10) . . ?
C10 N2 C6 118.84(12) . . ?
C11 N3 Ni1 114.36(9) . . ?
C15 N3 Ni1 126.67(10) . . ?
C15 N3 C11 118.77(13) . . ?
N1 C1 C2 120.54(13) . . ?
N1 C1 C11 113.51(12) . . ?
C2 C1 C11 125.94(13) . . ?
C1 C2 H2 120.9 . . ?
C3 C2 C1 118.23(14) . . ?
C3 C2 H2 120.9 . . ?
C2 C3 H3 119.7 . . ?
C4 C3 C2 120.58(13) . . ?
C4 C3 H3 119.7 . . ?
C3 C4 H4 120.8 . . ?
C3 C4 C5 118.35(14) . . ?
C5 C4 H4 120.8 . . ?
N1 C5 C4 120.58(13) . . ?
N1 C5 C6 113.46(12) . . ?
C4 C5 C6 125.96(13) . . ?
N2 C6 C5 114.53(12) . . ?
N2 C6 C7 121.85(13) . . ?
C7 C6 C5 123.62(13) . . ?
C6 C7 H7 120.6 . . ?
C8 C7 C6 118.71(14) . . ?
C8 C7 H7 120.6 . . ?
C7 C8 H8 120.3 . . ?
C9 C8 C7 119.49(14) . . ?
C9 C8 H8 120.3 . . ?
C8 C9 H9 120.6 . . ?
C8 C9 C10 118.71(14) . . ?
C10 C9 H9 120.6 . . ?
N2 C10 C9 122.39(14) . . ?
N2 C10 H10 118.8 . . ?
C9 C10 H10 118.8 . . ?
N3 C11 C1 114.76(12) . . ?
N3 C11 C12 122.01(13) . . ?
C12 C11 C1 123.23(13) . . ?
C11 C12 H12 120.7 . . ?
C11 C12 C13 118.60(14) . . ?
C13 C12 H12 120.7 . . ?
C12 C13 H13 120.3 . . ?
C14 C13 C12 119.44(14) . . ?
C14 C13 H13 120.3 . . ?
C13 C14 H14 120.6 . . ?
C13 C14 C15 118.84(14) . . ?
C15 C14 H14 120.6 . . ?
N3 C15 C14 122.34(14) . . ?
N3 C15 H15 118.8 . . ?
C14 C15 H15 118.8 . . ?
O1 C16 C17 115.40(12) . . ?
O1 C16 C21 124.82(13) . . ?
C21 C16 C17 119.68(13) . . ?
C18 C17 C16 109.25(13) . . ?
C18 C17 C19 108.51(14) . . ?
C18 C17 C20 109.87(15) . . ?
C19 C17 C16 113.20(13) . . ?
C20 C17 C16 106.25(13) . . ?
C20 C17 C19 109.73(14) . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
C17 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C17 C19 H19A 109.5 . . ?
C17 C19 H19B 109.5 . . ?
C17 C19 H19C 109.5 . . ?
H19A C19 H19B 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C17 C20 H20A 109.5 . . ?
C17 C20 H20B 109.5 . . ?
C17 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C16 C21 H21 117.0 . . ?
C22 C21 C16 125.90(14) . . ?
C22 C21 H21 117.0 . . ?
O2 C22 C21 125.03(13) . . ?
O2 C22 C23 114.25(12) . . ?
C21 C22 C23 120.71(12) . . ?
C24 C23 C22 108.49(12) . . ?
C24 C23 C26 108.93(14) . . ?
C25 C23 C22 113.62(12) . . ?
C25 C23 C24 109.43(13) . . ?
C25 C23 C26 108.59(13) . . ?
C26 C23 C22 107.70(12) . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C23 C25 H25A 109.5 . . ?
C23 C25 H25B 109.5 . . ?
C23 C25 H25C 109.5 . . ?
H25A C25 H25B 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C23 C26 H26A 109.5 . . ?
C23 C26 H26B 109.5 . . ?
C23 C26 H26C 109.5 . . ?
H26A C26 H26B 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
O4 Cl1 O3 108.48(7) . . ?
O4 Cl1 O5 110.25(8) . . ?
O5 Cl1 O3 108.94(7) . . ?
O6 Cl1 O3 108.66(7) . . ?
O6 Cl1 O4 110.59(8) . . ?
O6 Cl1 O5 109.87(8) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 O1 2.0023(10) . ?
Ni1 O2 1.9772(10) . ?
Ni1 O7 2.1416(11) . ?
Ni1 N1 1.9982(12) . ?
Ni1 N2 2.0966(12) . ?
Ni1 N3 2.1012(12) . ?
O1 C16 1.2626(17) . ?
O2 C22 1.2752(16) . ?
O7 H7A 0.80(2) . ?
O7 H7B 0.77(2) . ?
N1 C1 1.3443(18) . ?
N1 C5 1.3379(18) . ?
N2 C6 1.3540(18) . ?
N2 C10 1.3407(18) . ?
N3 C11 1.3522(18) . ?
N3 C15 1.3391(18) . ?
C1 C2 1.3913(19) . ?
C1 C11 1.4843(19) . ?
C2 H2 0.9300 . ?
C2 C3 1.390(2) . ?
C3 H3 0.9300 . ?
C3 C4 1.387(2) . ?
C4 H4 0.9300 . ?
C4 C5 1.3919(19) . ?
C5 C6 1.488(2) . ?
C6 C7 1.390(2) . ?
C7 H7 0.9300 . ?
C7 C8 1.388(2) . ?
C8 H8 0.9300 . ?
C8 C9 1.384(2) . ?
C9 H9 0.9300 . ?
C9 C10 1.387(2) . ?
C10 H10 0.9300 . ?
C11 C12 1.387(2) . ?
C12 H12 0.9300 . ?
C12 C13 1.387(2) . ?
C13 H13 0.9300 . ?
C13 C14 1.382(2) . ?
C14 H14 0.9300 . ?
C14 C15 1.385(2) . ?
C15 H15 0.9300 . ?
C16 C17 1.538(2) . ?
C16 C21 1.409(2) . ?
C17 C18 1.530(2) . ?
C17 C19 1.534(2) . ?
C17 C20 1.534(2) . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
C21 H21 0.9300 . ?
C21 C22 1.393(2) . ?
C22 C23 1.5421(19) . ?
C23 C24 1.532(2) . ?
C23 C25 1.526(2) . ?
C23 C26 1.532(2) . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
C25 H25A 0.9600 . ?
C25 H25B 0.9600 . ?
C25 H25C 0.9600 . ?
C26 H26A 0.9600 . ?
C26 H26B 0.9600 . ?
C26 H26C 0.9600 . ?
Cl1 O3 1.4628(11) . ?
Cl1 O4 1.4313(12) . ?
Cl1 O5 1.4364(12) . ?
Cl1 O6 1.4276(12) . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
O7 H7A O3 0.80(2) 2.12(2) 2.8747(15) 156.2(18) 2_666 yes
O7 H7B Cl1 0.77(2) 2.94(2) 3.6689(12) 157.4(18) . yes
O7 H7B O3 0.77(2) 2.10(2) 2.8619(16) 168.6(19) . yes
C2 H2 O5 0.93 2.54 3.4531(19) 168.8 2_656 yes
C4 H4 O7 0.93 2.63 3.4632(18) 149.8 2_766 yes
C9 H9 O6 0.93 2.53 3.2236(19) 131.2 1_665 yes
C10 H10 O5 0.93 2.53 3.2549(19) 135.0 2_666 yes
C12 H12 O5 0.93 2.52 3.4339(19) 168.5 2_656 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
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Ni1 O1 C16 C17 174.00(10) . . . . ?
Ni1 O1 C16 C21 -2.4(2) . . . . ?
Ni1 O2 C22 C21 12.2(2) . . . . ?
Ni1 O2 C22 C23 -166.81(9) . . . . ?
Ni1 N1 C1 C2 -176.17(11) . . . . ?
Ni1 N1 C1 C11 2.77(16) . . . . ?
Ni1 N1 C5 C4 176.44(11) . . . . ?
Ni1 N1 C5 C6 -3.26(16) . . . . ?
Ni1 N2 C6 C5 0.16(15) . . . . ?
Ni1 N2 C6 C7 179.55(11) . . . . ?
Ni1 N2 C10 C9 -179.05(11) . . . . ?
Ni1 N3 C11 C1 -3.94(15) . . . . ?
Ni1 N3 C11 C12 175.20(11) . . . . ?
Ni1 N3 C15 C14 -174.04(12) . . . . ?
O1 C16 C17 C18 28.60(19) . . . . ?
O1 C16 C17 C19 149.63(14) . . . . ?
O1 C16 C17 C20 -89.87(16) . . . . ?
O1 C16 C21 C22 -2.7(3) . . . . ?
O2 C22 C23 C24 -57.32(17) . . . . ?
O2 C22 C23 C25 -179.25(13) . . . . ?
O2 C22 C23 C26 60.43(16) . . . . ?
N1 C1 C2 C3 0.2(2) . . . . ?
N1 C1 C11 N3 0.95(18) . . . . ?
N1 C1 C11 C12 -178.16(13) . . . . ?
N1 C5 C6 N2 1.91(18) . . . . ?
N1 C5 C6 C7 -177.47(13) . . . . ?
N2 C6 C7 C8 -0.6(2) . . . . ?
N3 C11 C12 C13 -0.5(2) . . . . ?
C1 N1 C5 C4 0.6(2) . . . . ?
C1 N1 C5 C6 -179.09(12) . . . . ?
C1 C2 C3 C4 -0.3(2) . . . . ?
C1 C11 C12 C13 178.56(13) . . . . ?
C2 C1 C11 N3 179.83(14) . . . . ?
C2 C1 C11 C12 0.7(2) . . . . ?
C2 C3 C4 C5 0.5(2) . . . . ?
C3 C4 C5 N1 -0.7(2) . . . . ?
C3 C4 C5 C6 178.95(14) . . . . ?
C4 C5 C6 N2 -177.77(14) . . . . ?
C4 C5 C6 C7 2.8(2) . . . . ?
C5 N1 C1 C2 -0.3(2) . . . . ?
C5 N1 C1 C11 178.60(12) . . . . ?
C5 C6 C7 C8 178.72(13) . . . . ?
C6 N2 C10 C9 0.2(2) . . . . ?
C6 C7 C8 C9 0.6(2) . . . . ?
C7 C8 C9 C10 -0.2(2) . . . . ?
C8 C9 C10 N2 -0.2(2) . . . . ?
C10 N2 C6 C5 -179.18(12) . . . . ?
C10 N2 C6 C7 0.2(2) . . . . ?
C11 N3 C15 C14 0.5(2) . . . . ?
C11 C1 C2 C3 -178.64(14) . . . . ?
C11 C12 C13 C14 0.5(2) . . . . ?
C12 C13 C14 C15 0.0(2) . . . . ?
C13 C14 C15 N3 -0.5(2) . . . . ?
C15 N3 C11 C1 -179.15(13) . . . . ?
C15 N3 C11 C12 0.0(2) . . . . ?
C16 C21 C22 O2 -2.7(3) . . . . ?
C16 C21 C22 C23 176.32(14) . . . . ?
C17 C16 C21 C22 -178.92(15) . . . . ?
C21 C16 C17 C18 -154.85(15) . . . . ?
C21 C16 C17 C19 -33.8(2) . . . . ?
C21 C16 C17 C20 86.68(17) . . . . ?
C21 C22 C23 C24 123.58(16) . . . . ?
C21 C22 C23 C25 1.6(2) . . . . ?
C21 C22 C23 C26 -118.67(16) . . . . ?
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-0.2317 -14.8035 5.1245 -0.9141 -0.0961 -0.3939
-6.9151 -7.1446 -4.2754 -0.4448 -0.0467 -0.8944
-9.6795 0.0826 -9.6316 0.0000 0.0000 -1.0000
-9.0731 12.6871 -13.5891 0.7785 0.0818 -0.6222
3.3411 12.2015 -1.0990 0.7551 0.0794 0.6508
8.5029 3.6866 7.1012 0.2321 0.0244 0.9724
6.8654 -0.2234 13.9403 -0.0888 0.2733 0.9578
-5.8676 -0.5076 18.2101 -0.3004 0.9245 0.2346
-12.5796 -0.1817 -0.0520 -0.1557 0.4792 -0.8638
-2.0760 0.3850 -17.9035 0.1978 -0.6089 -0.7682
2.5259 0.4778 -19.0237 0.2690 -0.8280 -0.4921
12.6215 0.3342 -6.5000 0.2381 -0.7327 0.6376
1.6577 -7.2624 19.8535 -0.6213 0.5594 0.5487
1.1867 8.2409 -19.5415 0.7073 -0.6368 -0.3070
3.7537 -12.3878 17.4983 -0.8665 0.2815 0.4122
3.8353 12.5585 -10.2092 0.8830 -0.2869 0.3714
10.4916 -12.9921 10.9906 -0.7507 -0.2439 0.6139
-0.1300 -13.9465 0.4661 -0.8115 -0.2637 -0.5215
12.9737 -10.8509 -1.7307 -0.4565 -0.7907 0.4079
0.1453 -8.3193 -11.1941 -0.3536 -0.6124 -0.7071
-4.8958 -3.8365 18.9721 -0.4897 0.8482 0.2017
11.2859 0.0300 5.7810 0.0681 -0.2095 0.9754
-6.3674 2.7825 16.7922 -0.1005 0.9563 0.2747
-9.5642 13.9391 2.2386 0.6686 0.7425 -0.0408
12.7851 -4.2446 -8.6760 -0.0000 -0.9179 0.3969
6.8534 -4.4053 -15.6719 -0.0000 -0.9648 -0.2631
13.7392 -3.7919 0.2813 -0.0627 -0.5967 0.8000
11.5241 -3.2749 8.7724 -0.1533 -0.1702 0.9734
-0.2929 -1.8120 19.3553 -0.3238 0.7273 0.6051
0.3552 9.8039 8.6728 0.4731 0.5255 0.7071
9.6278 -3.1685 12.3527 -0.2090 0.0444 0.9769
