#------------------------------------------------------------------------------
#$Date: 2019-11-26 00:05:27 +0200 (Tue, 26 Nov 2019) $
#$Revision: 242127 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/13/20/4132086.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_4132086
loop_
_publ_author_name
'Duan, Peng-Cheng'
'Manz, Dennis-Helmut'
'Dechert, Sebastian'
'Demeshko, Serhiy'
'Meyer, Franc'
_publ_section_title
;
 Reductive O₂ Binding at a Dihydride Complex Leading to Redox
 Interconvertible μ-1,2-Peroxo and μ-1,2-Superoxo Dinickel(II)
 Intermediates.
;
_journal_issue                   14
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              4929
_journal_page_last               4939
_journal_paper_doi               10.1021/jacs.8b01468
_journal_volume                  140
_journal_year                    2018
_chemical_formula_moiety
'C39 H53 N6 Ni2 O2 -, C28 H40 K O8 +, 3(C4 H8 O)'
_chemical_formula_sum            'C79 H117 K N6 Ni2 O13'
_chemical_formula_weight         1515.30
_space_group_crystal_system      orthorhombic
_space_group_IT_number           57
_space_group_name_Hall           '-P 2c 2b'
_space_group_name_H-M_alt        'P b c m'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2016/6
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.2912(2)
_cell_length_b                   25.8683(4)
_cell_length_c                   27.1074(4)
_cell_measurement_reflns_used    65467
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      25.722
_cell_measurement_theta_min      1.502
_cell_volume                     7917.6(2)
_computing_cell_refinement       'X-AREA (Stoe & Cie, 2015)'
_computing_data_collection       'X-AREA (Stoe & Cie, 2015)'
_computing_data_reduction        'X-AREA (Stoe & Cie, 2015)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 2012)'
_computing_publication_material  'SHELXL-2016 (Sheldrick, 2016)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXT-2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      133(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Stoe IPDS II'
_diffrn_measurement_method       ω
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0468
_diffrn_reflns_av_unetI/netI     0.0189
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            65467
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.722
_diffrn_reflns_theta_min         1.502
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.592
_exptl_absorpt_correction_T_max  0.8007
_exptl_absorpt_correction_T_min  0.6134
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'X-RED (Stoe & Cie, 2015)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.271
_exptl_crystal_description       block
_exptl_crystal_F_000             3248
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.220
_exptl_crystal_size_min          0.200
_refine_diff_density_max         0.457
_refine_diff_density_min         -0.279
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.114
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     577
_refine_ls_number_reflns         7668
_refine_ls_number_restraints     145
_refine_ls_restrained_S_all      1.119
_refine_ls_R_factor_all          0.0600
_refine_ls_R_factor_gt           0.0418
_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)+(0.0478P)²+7.3377P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0994
_refine_ls_wR_factor_ref         0.1144
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6102
_reflns_number_total             7668
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ja8b01468_si_002.cif
_cod_data_source_block           2b-pd212c
_cod_database_code               4132086
_shelx_shelxl_version_number     2016/6
_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   0.756
_shelx_estimated_absorpt_t_max   0.891
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x, -y+1/2, -z'
'-x, -y, -z'
'x, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x, y-1/2, 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 0.38439(2) 0.67845(2) 0.51422(2) 0.02547(10) Uani 1 1 d . . . . .
O1 O 0.48954(14) 0.72478(6) 0.48770(6) 0.0321(4) Uani 1 1 d . . . . .
N1 N 0.26291(17) 0.72575(7) 0.50917(7) 0.0304(4) Uani 1 1 d . . . . .
N2 N 0.25986(17) 0.63547(8) 0.53811(8) 0.0316(4) Uani 1 1 d . . . . .
N3 N 0.50298(17) 0.62672(7) 0.51631(7) 0.0279(4) Uani 1 1 d . . . . .
C1 C 0.0745(3) 0.750000 0.500000 0.0413(9) Uani 1 2 d S T P . .
H1 H -0.009636 0.750000 0.499999 0.050 Uiso 1 2 calc R U P . .
C2 C 0.1499(2) 0.71051(10) 0.51501(9) 0.0338(5) Uani 1 1 d . . . . .
C3 C 0.1393(2) 0.65776(10) 0.53719(11) 0.0382(6) Uani 1 1 d . . . . .
H3A H 0.106861 0.660041 0.571052 0.046 Uiso 1 1 calc R U . . .
H3B H 0.085843 0.635934 0.517086 0.046 Uiso 1 1 calc R U . . .
C4 C 0.2724(2) 0.58810(9) 0.55641(9) 0.0338(5) Uani 1 1 d . . . . .
C5 C 0.3817(2) 0.56325(10) 0.55737(9) 0.0356(6) Uani 1 1 d . . . . .
H5 H 0.383951 0.530799 0.573763 0.043 Uiso 1 1 calc R U . . .
C6 C 0.4888(2) 0.58040(9) 0.53704(9) 0.0308(5) Uani 1 1 d . . . . .
C7 C 0.1667(3) 0.55990(11) 0.57774(12) 0.0481(7) Uani 1 1 d . . . . .
H7A H 0.191125 0.525492 0.588919 0.072 Uiso 1 1 calc R U . . .
H7B H 0.105322 0.556440 0.552371 0.072 Uiso 1 1 calc R U . . .
H7C H 0.135055 0.579509 0.605732 0.072 Uiso 1 1 calc R U . . .
C8 C 0.5916(2) 0.54277(10) 0.53905(11) 0.0391(6) Uani 1 1 d . . . . .
H8A H 0.568191 0.511994 0.557743 0.059 Uiso 1 1 calc R U . . .
H8B H 0.659321 0.559304 0.555254 0.059 Uiso 1 1 calc R U . . .
H8C H 0.613809 0.532681 0.505450 0.059 Uiso 1 1 calc R U . . .
C9 C 0.6184(2) 0.63662(9) 0.49562(9) 0.0288(5) Uani 1 1 d . . . . .
C10 C 0.7078(2) 0.65687(10) 0.52584(9) 0.0336(5) Uani 1 1 d . . . . .
C11 C 0.8207(2) 0.66382(11) 0.50620(11) 0.0435(6) Uani 1 1 d . . . . .
H11 H 0.881857 0.677777 0.526274 0.052 Uiso 1 1 calc R U . . .
C12 C 0.8447(2) 0.65061(13) 0.45783(11) 0.0502(7) Uani 1 1 d . . . . .
H12 H 0.922505 0.654709 0.445034 0.060 Uiso 1 1 calc R U . . .
C13 C 0.7561(3) 0.63154(11) 0.42821(10) 0.0441(7) Uani 1 1 d . . . . .
H13 H 0.773213 0.623183 0.394844 0.053 Uiso 1 1 calc R U . . .
C14 C 0.6412(2) 0.62418(9) 0.44617(9) 0.0339(5) Uani 1 1 d . . . . .
C15 C 0.6851(2) 0.67198(12) 0.57879(10) 0.0466(7) Uani 1 1 d . . . . .
H15 H 0.603455 0.660012 0.587419 0.056 Uiso 1 1 calc R U . . .
C16 C 0.6874(3) 0.73011(13) 0.58474(13) 0.0679(10) Uani 1 1 d . . . . .
H16A H 0.663606 0.739215 0.618402 0.102 Uiso 1 1 calc R U . . .
H16B H 0.632445 0.745890 0.561163 0.102 Uiso 1 1 calc R U . . .
H16C H 0.767747 0.742899 0.578511 0.102 Uiso 1 1 calc R U . . .
C17 C 0.7699(4) 0.64731(13) 0.61530(12) 0.0675(10) Uani 1 1 d . . . . .
H17A H 0.745803 0.656198 0.648976 0.101 Uiso 1 1 calc R U . . .
H17B H 0.850299 0.660144 0.609269 0.101 Uiso 1 1 calc R U . . .
H17C H 0.768456 0.609677 0.611220 0.101 Uiso 1 1 calc R U . . .
C18 C 0.5438(3) 0.60431(10) 0.41311(9) 0.0398(6) Uani 1 1 d . . . . .
H18 H 0.487852 0.583710 0.433897 0.048 Uiso 1 1 calc R U . . .
C19 C 0.4746(3) 0.64958(11) 0.39092(10) 0.0447(7) Uani 1 1 d . . . . .
H19A H 0.406483 0.636315 0.372454 0.067 Uiso 1 1 calc R U . . .
H19B H 0.526294 0.669123 0.368642 0.067 Uiso 1 1 calc R U . . .
H19C H 0.446861 0.672288 0.417443 0.067 Uiso 1 1 calc R U . . .
C20 C 0.5878(3) 0.56939(12) 0.37134(11) 0.0579(9) Uani 1 1 d . . . . .
H20A H 0.520513 0.551099 0.356649 0.087 Uiso 1 1 calc R U . . .
H20B H 0.644406 0.544223 0.384561 0.087 Uiso 1 1 calc R U . . .
H20C H 0.626774 0.590515 0.346092 0.087 Uiso 1 1 calc R U . . .
K1 K 0.21459(7) 0.72834(3) 0.750000 0.03763(19) Uani 1 2 d S T P . .
O11 O 0.38756(17) 0.67348(7) 0.70292(6) 0.0408(4) Uani 1 1 d . . . . .
O12 O 0.21755(17) 0.73055(7) 0.64788(6) 0.0407(4) Uani 1 1 d . . . . .
O13 O 0.03469(16) 0.77878(8) 0.70210(6) 0.0405(4) Uani 1 1 d . . . . .
C21 C 0.5467(3) 0.55126(13) 0.72477(12) 0.0611(9) Uani 1 1 d . . . . .
H21 H 0.583146 0.523617 0.707406 0.073 Uiso 1 1 calc R U . . .
C22 C 0.4939(3) 0.59125(12) 0.69871(12) 0.0523(7) Uani 1 1 d . . . . .
H22 H 0.493658 0.590953 0.663667 0.063 Uiso 1 1 calc R U . . .
C23 C 0.4416(2) 0.63152(11) 0.72418(10) 0.0401(6) Uani 1 1 d . . . . .
C24 C 0.3890(3) 0.67693(12) 0.65011(9) 0.0455(7) Uani 1 1 d . . . . .
H24A H 0.339493 0.649279 0.635571 0.055 Uiso 1 1 calc R U . . .
H24B H 0.470945 0.672992 0.637627 0.055 Uiso 1 1 calc R U . . .
C25 C 0.3411(3) 0.72889(11) 0.63641(10) 0.0446(7) Uani 1 1 d . . . . .
H25A H 0.383478 0.756193 0.654934 0.054 Uiso 1 1 calc R U . . .
H25B H 0.352974 0.735127 0.600718 0.054 Uiso 1 1 calc R U . . .
C26 C 0.1662(3) 0.77879(11) 0.63393(10) 0.0458(7) Uani 1 1 d . . . . .
H26A H 0.172796 0.783546 0.597795 0.055 Uiso 1 1 calc R U . . .
H26B H 0.208788 0.807516 0.650311 0.055 Uiso 1 1 calc R U . . .
C27 C 0.0388(3) 0.77911(12) 0.64895(9) 0.0465(7) Uani 1 1 d . . . . .
H27A H -0.001026 0.810382 0.635989 0.056 Uiso 1 1 calc R U . . .
H27B H -0.002095 0.748275 0.635619 0.056 Uiso 1 1 calc R U . . .
C28 C -0.0744(2) 0.78091(11) 0.72402(10) 0.0419(6) Uani 1 1 d . . . . .
C29 C -0.1806(3) 0.78276(14) 0.69898(12) 0.0595(9) Uani 1 1 d . . . . .
H29 H -0.180989 0.783411 0.663945 0.071 Uiso 1 1 calc R U . . .
C30 C -0.2864(3) 0.78369(19) 0.72460(14) 0.0836(13) Uani 1 1 d . . . . .
H30 H -0.359346 0.784323 0.707118 0.100 Uiso 1 1 calc R U . . .
O14 O 0.2911(3) 0.82922(13) 0.7441(15) 0.050(5) Uani 0.5 1 d D . P A -1
C31 C 0.4101(4) 0.8474(2) 0.7467(15) 0.049(3) Uani 0.5 1 d D . P A -1
H31A H 0.452374 0.840211 0.715482 0.059 Uiso 0.5 1 calc R U P A -1
H31B H 0.452963 0.830293 0.774069 0.059 Uiso 0.5 1 calc R U P A -1
C32 C 0.4020(5) 0.9059(2) 0.7558(10) 0.057(4) Uani 0.5 1 d D . P A -1
H32A H 0.398017 0.914041 0.791398 0.068 Uiso 0.5 1 calc R U P A -1
H32B H 0.469649 0.924505 0.740766 0.068 Uiso 0.5 1 calc R U P A -1
C33 C 0.2864(5) 0.9185(2) 0.7297(2) 0.0478(13) Uani 0.5 1 d D . P A -1
H33A H 0.295440 0.918544 0.693411 0.057 Uiso 0.5 1 calc R U P A -1
H33B H 0.253295 0.952024 0.740674 0.057 Uiso 0.5 1 calc R U P A -1
C34 C 0.2117(4) 0.87297(18) 0.7476(17) 0.055(2) Uani 0.5 1 d D . P A -1
H34A H 0.185162 0.878322 0.781979 0.066 Uiso 0.5 1 calc R U P A -1
H34B H 0.141449 0.868018 0.726243 0.066 Uiso 0.5 1 calc R U P A -1
O15 O 0.0689(4) 0.64533(18) 0.7479(8) 0.0735(16) Uani 0.5 1 d D . P A -2
C41 C -0.0185(10) 0.6369(5) 0.7111(5) 0.080(4) Uani 0.5 1 d D . P A -2
H41A H 0.014610 0.616452 0.683514 0.096 Uiso 0.5 1 calc R U P A -2
H41B H -0.047919 0.670226 0.698052 0.096 Uiso 0.5 1 calc R U P A -2
C42 C -0.1159(10) 0.6080(5) 0.7359(4) 0.124(6) Uani 0.5 1 d D . P A -2
H42A H -0.148877 0.581237 0.713616 0.149 Uiso 0.5 1 calc R U P A -2
H42B H -0.180417 0.631701 0.745818 0.149 Uiso 0.5 1 calc R U P A -2
C43 C -0.0594(9) 0.5835(4) 0.7804(4) 0.079(3) Uani 0.5 1 d D . P A -2
H43A H -0.116023 0.581365 0.808192 0.094 Uiso 0.5 1 calc R U P A -2
H43B H -0.029778 0.548397 0.772698 0.094 Uiso 0.5 1 calc R U P A -2
C44 C 0.0381(13) 0.6187(6) 0.7917(4) 0.106(5) Uani 0.5 1 d D . P A -2
H44A H 0.013513 0.643610 0.817474 0.128 Uiso 0.5 1 calc R U P A -2
H44B H 0.107016 0.598958 0.804150 0.128 Uiso 0.5 1 calc R U P A -2
O21A O 0.9060(6) 0.4009(2) 0.6228(2) 0.0729(17) Uani 0.505(6) 1 d D . P B 3
C51A C 0.8423(17) 0.4058(6) 0.5803(5) 0.089(5) Uani 0.505(6) 1 d D . P B 3
H51A H 0.757023 0.399441 0.586194 0.107 Uiso 0.505(6) 1 calc R U P B 3
H51B H 0.871115 0.381646 0.554639 0.107 Uiso 0.505(6) 1 calc R U P B 3
C52A C 0.864(2) 0.4584(6) 0.5666(7) 0.175(10) Uani 0.505(6) 1 d D . P B 3
H52A H 0.796638 0.471071 0.546331 0.209 Uiso 0.505(6) 1 calc R U P B 3
H52B H 0.936374 0.460355 0.546368 0.209 Uiso 0.505(6) 1 calc R U P B 3
C53A C 0.8770(18) 0.4919(7) 0.6109(7) 0.094(7) Uani 0.505(6) 1 d D . P B 3
H53A H 0.801201 0.499740 0.627750 0.113 Uiso 0.505(6) 1 calc R U P B 3
H53B H 0.922477 0.523989 0.604650 0.113 Uiso 0.505(6) 1 calc R U P B 3
C54A C 0.9490(7) 0.4496(3) 0.6361(3) 0.077(2) Uani 0.505(6) 1 d D . P B 3
H54A H 1.033181 0.452575 0.626226 0.093 Uiso 0.505(6) 1 calc R U P B 3
H54B H 0.944223 0.453745 0.672304 0.093 Uiso 0.505(6) 1 calc R U P B 3
O21B O 0.7952(10) 0.4232(4) 0.6314(2) 0.140(5) Uani 0.495(6) 1 d D . P B 4
C51B C 0.8043(8) 0.4758(4) 0.6416(3) 0.083(3) Uani 0.495(6) 1 d D . P B 4
H51C H 0.833360 0.481957 0.675540 0.100 Uiso 0.495(6) 1 calc R U P B 4
H51D H 0.727588 0.493638 0.636994 0.100 Uiso 0.495(6) 1 calc R U P B 4
C52B C 0.8942(15) 0.4926(7) 0.6035(6) 0.063(3) Uani 0.495(6) 1 d D . P B 4
H52C H 0.884332 0.529745 0.595825 0.076 Uiso 0.495(6) 1 calc R U P B 4
H52D H 0.975546 0.486937 0.615930 0.076 Uiso 0.495(6) 1 calc R U P B 4
C53B C 0.8729(8) 0.4606(5) 0.5583(5) 0.061(3) Uani 0.495(6) 1 d D . P B 4
H53C H 0.822760 0.478805 0.533829 0.074 Uiso 0.495(6) 1 calc R U P B 4
H53D H 0.947758 0.449469 0.542508 0.074 Uiso 0.495(6) 1 calc R U P B 4
C54B C 0.8111(15) 0.4180(6) 0.5815(5) 0.090(5) Uani 0.495(6) 1 d D . P B 4
H54C H 0.732541 0.414252 0.565684 0.108 Uiso 0.495(6) 1 calc R U P B 4
H54D H 0.856039 0.385825 0.575190 0.108 Uiso 0.495(6) 1 calc R U P B 4
O31 O 0.1076(7) 0.4900(3) 0.7017(3) 0.129(3) Uani 0.5 1 d D . P C -5
C61 C 0.0992(10) 0.4381(4) 0.7172(4) 0.111(3) Uani 0.5 1 d D . P C -5
H61A H 0.113692 0.414650 0.688991 0.133 Uiso 0.5 1 calc R U P C -5
H61B H 0.018934 0.431104 0.730301 0.133 Uiso 0.5 1 calc R U P C -5
C62 C 0.1905(9) 0.4294(3) 0.7567(10) 0.100(4) Uani 0.5 1 d D . P C -5
H62A H 0.153869 0.415108 0.786959 0.120 Uiso 0.5 1 calc R U P C -5
H62B H 0.253204 0.405519 0.745200 0.120 Uiso 0.5 1 calc R U P C -5
C63 C 0.2385(10) 0.4819(4) 0.7655(4) 0.102(4) Uani 0.5 1 d D . P C -5
H63A H 0.324846 0.480402 0.771714 0.122 Uiso 0.5 1 calc R U P C -5
H63B H 0.199506 0.498049 0.794399 0.122 Uiso 0.5 1 calc R U P C -5
C64 C 0.2127(9) 0.5123(4) 0.7192(4) 0.089(3) Uani 0.5 1 d D . P C -5
H64A H 0.201360 0.549449 0.726727 0.107 Uiso 0.5 1 calc R U P C -5
H64B H 0.277516 0.508585 0.694918 0.107 Uiso 0.5 1 calc R U P C -5
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'
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
O1 Ni1 N1 91.08(8) . .
O1 Ni1 N3 90.90(8) . .
N1 Ni1 N3 175.89(9) . .
O1 Ni1 N2 172.80(8) . .
N1 Ni1 N2 82.16(8) . .
N3 Ni1 N2 95.69(8) . .
O1 O1 Ni1 113.81(12) 4_566 .
C2 N1 N1 108.43(14) . 4_566
C2 N1 Ni1 120.16(16) . .
N1 N1 Ni1 130.13(8) 4_566 .
C4 N2 C3 117.6(2) . .
C4 N2 Ni1 125.87(17) . .
C3 N2 Ni1 116.48(15) . .
C6 N3 C9 115.62(19) . .
C6 N3 Ni1 124.23(16) . .
C9 N3 Ni1 120.13(15) . .
C2 C1 C2 104.5(3) . 4_566
N1 C2 C1 109.3(2) . .
N1 C2 C3 113.0(2) . .
C1 C2 C3 137.6(2) . .
N2 C3 C2 106.77(19) . .
N2 C4 C5 121.8(2) . .
N2 C4 C7 120.2(2) . .
C5 C4 C7 118.0(2) . .
C4 C5 C6 127.7(2) . .
N3 C6 C5 123.7(2) . .
N3 C6 C8 120.0(2) . .
C5 C6 C8 116.3(2) . .
C10 C9 C14 120.8(2) . .
C10 C9 N3 119.3(2) . .
C14 C9 N3 119.8(2) . .
C11 C10 C9 118.9(2) . .
C11 C10 C15 119.0(2) . .
C9 C10 C15 122.0(2) . .
C12 C11 C10 120.7(3) . .
C13 C12 C11 120.0(3) . .
C12 C13 C14 121.4(3) . .
C13 C14 C9 118.1(2) . .
C13 C14 C18 121.1(2) . .
C9 C14 C18 120.8(2) . .
C10 C15 C16 110.8(3) . .
C10 C15 C17 113.8(3) . .
C16 C15 C17 109.7(2) . .
C14 C18 C19 110.2(2) . .
C14 C18 C20 113.8(2) . .
C19 C18 C20 109.0(2) . .
O15 K1 O11 90.7(2) . .
O11 K1 O11 55.73(8) . 6_557
O15 K1 O13 85.2(2) . .
O11 K1 O13 123.78(5) . .
O11 K1 O13 177.07(7) 6_557 .
O11 K1 O13 177.07(7) . 6_557
O11 K1 O13 123.77(5) 6_557 6_557
O13 K1 O13 56.55(7) . 6_557
O11 K1 O14 104.0(4) . .
O11 K1 O14 107.2(4) 6_557 .
O13 K1 O14 75.8(4) . .
O13 K1 O14 79.0(4) 6_557 .
O15 K1 O12 90.2(5) . .
O11 K1 O12 62.28(5) . .
O11 K1 O12 117.99(6) 6_557 .
O13 K1 O12 61.68(5) . .
O13 K1 O12 118.21(6) 6_557 .
O14 K1 O12 85.3(9) . .
O11 K1 O12 117.99(6) . 6_557
O11 K1 O12 62.28(5) 6_557 6_557
O13 K1 O12 118.21(6) . 6_557
O13 K1 O12 61.68(5) 6_557 6_557
O14 K1 O12 92.0(9) . 6_557
O12 K1 O12 177.26(9) . 6_557
O15 K1 C25 103.9(4) . .
O11 K1 C25 43.72(6) . .
O11 K1 C25 97.19(7) 6_557 .
O13 K1 C25 83.11(6) . .
O13 K1 C25 137.69(6) 6_557 .
O14 K1 C25 79.1(8) . .
O12 K1 C25 24.21(6) . .
O12 K1 C25 154.39(7) 6_557 .
O11 K1 C25 97.19(7) . 6_557
O11 K1 C25 43.72(6) 6_557 6_557
O13 K1 C25 137.69(6) . 6_557
O13 K1 C25 83.11(6) 6_557 6_557
O14 K1 C25 85.2(8) . 6_557
O12 K1 C25 154.39(7) . 6_557
O12 K1 C25 24.21(6) 6_557 6_557
C25 K1 C25 130.23(11) . 6_557
O15 K1 C26 100.6(4) . .
O11 K1 C26 83.31(6) . .
O11 K1 C26 137.40(7) 6_557 .
O13 K1 C26 43.17(6) . .
O13 K1 C26 97.74(6) 6_557 .
O14 K1 C26 68.8(8) . .
O12 K1 C26 23.41(6) . .
O12 K1 C26 154.94(7) 6_557 .
C25 K1 C26 40.33(7) . .
C25 K1 C26 153.17(8) 6_557 .
O11 K1 C26 137.40(7) . 6_557
O11 K1 C26 83.31(6) 6_557 6_557
O13 K1 C26 97.74(6) . 6_557
O13 K1 C26 43.17(6) 6_557 6_557
O14 K1 C26 75.2(8) . 6_557
O12 K1 C26 154.94(7) . 6_557
O12 K1 C26 23.41(6) 6_557 6_557
C25 K1 C26 153.17(8) . 6_557
C25 K1 C26 40.33(7) 6_557 6_557
C26 K1 C26 131.58(10) . 6_557
C23 O11 C24 117.6(2) . .
C23 O11 K1 122.19(15) . .
C24 O11 K1 116.26(15) . .
C26 O12 C25 111.4(2) . .
C26 O12 K1 106.15(14) . .
C25 O12 K1 103.21(14) . .
C28 O13 C27 117.6(2) . .
C28 O13 K1 118.71(15) . .
C27 O13 K1 116.90(15) . .
C21 C21 C22 120.61(19) 6_557 .
C23 C22 C21 119.4(3) . .
O11 C23 C22 125.2(2) . .
O11 C23 C23 114.84(13) . 6_557
C22 C23 C23 119.96(17) . 6_557
O11 C24 C25 107.4(2) . .
O12 C25 C24 109.0(2) . .
O12 C25 K1 52.58(11) . .
C24 C25 K1 85.60(14) . .
O12 C26 C27 108.9(2) . .
O12 C26 K1 50.44(11) . .
C27 C26 K1 84.61(14) . .
O13 C27 C26 107.6(2) . .
O13 C28 C29 124.8(2) . .
O13 C28 C28 115.73(13) . 6_557
C29 C28 C28 119.50(18) . 6_557
C28 C29 C30 120.3(3) . .
C30 C30 C29 120.1(2) 6_557 .
C31 O14 C34 108.8(5) . .
C31 O14 K1 127.3(4) . .
C34 O14 K1 122.9(4) . .
O14 C31 C32 106.1(6) . .
C33 C32 C31 100.8(11) . .
C32 C33 C34 99.3(11) . .
O14 C34 C33 104.0(11) . .
C44 O15 C41 110.1(7) . .
C44 O15 K1 121.2(11) . .
C41 O15 K1 124.0(9) . .
O15 C41 C42 106.0(10) . .
C41 C42 C43 105.0(9) . .
C44 C43 C42 103.1(9) . .
O15 C44 C43 108.2(9) . .
C51A O21A C54A 108.5(8) . .
O21A C51A C52A 102.7(14) . .
C51A C52A C53A 111.2(15) . .
C52A C53A C54A 89.7(13) . .
O21A C54A C53A 110.3(9) . .
C54B O21B C51B 106.3(8) . .
O21B C51B C52B 101.3(9) . .
C53B C52B C51B 107.1(11) . .
C54B C53B C52B 98.1(11) . .
O21B C54B C53B 114.7(10) . .
C64 O31 C61 110.4(8) . .
O31 C61 C62 108.0(9) . .
C63 C62 C61 103.2(11) . .
C62 C63 C64 105.8(12) . .
O31 C64 C63 103.3(9) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ni1 O1 1.8337(16) .
Ni1 N1 1.8432(19) .
Ni1 N3 1.8939(19) .
Ni1 N2 1.906(2) .
O1 O1 1.465(3) 4_566
N1 C2 1.344(3) .
N1 N1 1.349(4) 4_566
N2 C4 1.329(3) .
N2 C3 1.479(3) .
N3 C6 1.333(3) .
N3 C9 1.442(3) .
C1 C2 1.391(3) .
C1 C2 1.391(3) 4_566
C2 C3 1.496(4) .
C4 C5 1.392(4) .
C4 C7 1.514(3) .
C5 C6 1.401(3) .
C6 C8 1.516(3) .
C9 C10 1.401(3) .
C9 C14 1.402(3) .
C10 C11 1.393(4) .
C10 C15 1.510(4) .
C11 C12 1.382(4) .
C12 C13 1.375(4) .
C13 C14 1.398(4) .
C14 C18 1.509(4) .
C15 C16 1.513(4) .
C15 C17 1.518(4) .
C18 C19 1.531(4) .
C18 C20 1.532(4) .
K1 O15 2.706(5) .
K1 O11 2.7307(19) .
K1 O11 2.7307(19) 6_557
K1 O13 2.7413(19) .
K1 O13 2.7414(19) 6_557
K1 O14 2.753(4) .
K1 O12 2.7689(17) .
K1 O12 2.7690(17) 6_557
K1 C25 3.394(3) .
K1 C25 3.394(3) 6_557
K1 C26 3.450(3) .
K1 C26 3.450(3) 6_557
O11 C23 1.372(3) .
O11 C24 1.434(3) .
O12 C26 1.427(3) .
O12 C25 1.430(3) .
O13 C28 1.369(3) .
O13 C27 1.441(3) .
C21 C21 1.368(7) 6_557
C21 C22 1.387(4) .
C22 C23 1.382(4) .
C23 C23 1.400(5) 6_557
C24 C25 1.496(4) .
C26 C27 1.496(4) .
C28 C29 1.378(4) .
C28 C28 1.408(5) 6_557
C29 C30 1.383(5) .
C30 C30 1.377(7) 6_557
O14 C31 1.426(6) .
O14 C34 1.446(7) .
C31 C32 1.535(10) .
C32 C33 1.519(13) .
C33 C34 1.526(15) .
O15 C44 1.417(16) .
O15 C41 1.419(14) .
C41 C42 1.490(13) .
C42 C43 1.504(12) .
C43 C44 1.461(14) .
O21A C51A 1.363(14) .
O21A C54A 1.397(8) .
C51A C52A 1.431(15) .
C52A C53A 1.491(15) .
C53A C54A 1.526(16) .
O21B C54B 1.372(13) .
O21B C51B 1.391(10) .
C51B C52B 1.512(14) .
C52B C53B 1.497(14) .
C53B C54B 1.448(12) .
O31 C64 1.403(11) .
O31 C61 1.408(11) .
C61 C62 1.504(17) .
C62 C63 1.483(11) .
C63 C64 1.509(10) .
