# Supplementary Material (ESI) for Dalton Transactions
# This journal is (c) The Royal Society of Chemistry 2011


data_global
_journal_name_full               'Dalton Trans.'
_journal_coden_cambridge         0222
_journal_year                    ?
_journal_volume                  ?
_journal_page_first              ?
_publ_contact_author_name        'Valerio Bertolasi'
_publ_contact_author_email       m38@unife.it
loop_
_publ_author_name
D.Bacco
V.Bertolasi
F.Dallavalle
L.Galliera
N.Marchetti
L.Marchio
M.Remelli
M.Tegoni

data_(I)
_database_code_depnum_ccdc_archive 'CCDC 770395'
#TrackingRef 'web_deposit_cif_file_0_ValerioBertolasi_1290093777.cif'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '3(C6 H13 N4 Ni O4), 3(K), 5(H2 O)'
_chemical_formula_sum            'C18 H49 K3 N12 Ni3 O17'
_chemical_formula_weight         999.12

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'
O O 0.0106 0.0060 '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'
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Trigonal
_symmetry_space_group_name_H-M   'P 3121'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z+1/3'
'-x+y, -x, z+2/3'
'x-y, -y, -z+2/3'
'-x, -x+y, -z+1/3'
'y, x, -z'

_cell_length_a                   9.6236(2)
_cell_length_b                   9.6236(2)
_cell_length_c                   35.6392(8)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     2858.47(11)
_cell_formula_units_Z            3
_cell_measurement_temperature    295
_cell_measurement_reflns_used    6813
_cell_measurement_theta_min      2.51
_cell_measurement_theta_max      28

_exptl_crystal_description       block
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.741
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1554
_exptl_absorpt_coefficient_mu    1.877
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.80
_exptl_absorpt_correction_T_max  0.89
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      295
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_diffrn_measurement_method       '\f scans and \w scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            6813
_diffrn_reflns_av_R_equivalents  0.0455
_diffrn_reflns_av_sigmaI/netI    0.0569
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       2
_diffrn_reflns_limit_l_min       -46
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_theta_min         2.51
_diffrn_reflns_theta_max         28.00
_reflns_number_total             3815
_reflns_number_gt                3343
_reflns_threshold_expression     I>2sigma(I)

_computing_data_collection       'COLLECT (Nonius, 1998)'
_computing_cell_refinement       'Denzo-SMN (Otwinowski & Minor, 1997)'
_computing_data_reduction        'Denzo-SMN (Otwinowski & Minor, 1997)'
_computing_structure_solution    'SIR97 (Altomare et al., 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'ORTEPIII (Burnett & Johnson, 1996)'
_computing_publication_material  
'SHELXL-97 (Sheldrick, 1997), PARST (Nardelli, 1995), PLATON (Spek, 2003)'

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0445P)^2^+1.1626P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.01(2)
_refine_ls_number_reflns         3815
_refine_ls_number_parameters     259
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0485
_refine_ls_R_factor_gt           0.0403
_refine_ls_wR_factor_ref         0.0978
_refine_ls_wR_factor_gt          0.0937
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_restrained_S_all      1.076
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.70853(6) 0.26411(6) 0.471890(15) 0.02902(14) Uani 1 1 d . . .
N1 N 0.5985(4) 0.2255(4) 0.51690(10) 0.0331(8) Uani 1 1 d . . .
N2 N 0.8607(4) 0.2413(5) 0.50235(10) 0.0393(8) Uani 1 1 d . . .
H200 H 0.8973 0.1856 0.4896 0.047 Uiso 1 1 calc R . .
H201 H 0.9447 0.3391 0.5073 0.047 Uiso 1 1 calc R . .
N3 N 0.5714(5) 0.3034(5) 0.44312(10) 0.0421(9) Uani 1 1 d . . .
N4 N 0.8167(4) 0.2860(4) 0.42499(10) 0.0352(8) Uani 1 1 d . B .
H400 H 0.9178 0.3689 0.4265 0.042 Uiso 1 1 calc R . .
H401 H 0.8215 0.1964 0.4206 0.042 Uiso 1 1 calc R . .
O1 O 0.4585(4) 0.2344(5) 0.52106(9) 0.0482(9) Uani 1 1 d . . .
H1 H 0.409(11) 0.245(11) 0.482(2) 0.14(3) Uiso 1 1 d . . .
O2 O 0.5672(4) 0.1284(4) 0.57734(9) 0.0433(7) Uani 1 1 d . . .
O3 O 0.4457(5) 0.3174(6) 0.45809(11) 0.0614(11) Uani 1 1 d . . .
O4A O 0.5502(9) 0.4039(9) 0.38390(19) 0.041(2) Uiso 0.441(11) 1 d PD . .
O4B O 0.4681(7) 0.2966(8) 0.38527(16) 0.043(2) Uiso 0.559(11) 1 d PD . .
C1 C 0.6396(5) 0.1701(5) 0.54595(12) 0.0338(9) Uani 1 1 d . . .
C2 C 0.7885(6) 0.1578(6) 0.53811(12) 0.0432(11) Uani 1 1 d . . .
H2 H 0.7528 0.0440 0.5343 0.052 Uiso 1 1 calc R . .
C3 C 0.9071(9) 0.2157(12) 0.57018(18) 0.092(3) Uani 1 1 d . . .
H3A H 1.0031 0.2168 0.5625 0.110 Uiso 1 1 calc R . .
H3B H 0.8609 0.1451 0.5912 0.110 Uiso 1 1 calc R . .
H3C H 0.9325 0.3222 0.5772 0.110 Uiso 1 1 calc R . .
C4 C 0.5898(7) 0.3197(8) 0.40700(15) 0.0650(18) Uani 1 1 d D B .
C5 C 0.7329(7) 0.3136(7) 0.39318(13) 0.0482(12) Uani 1 1 d D . .
H50 H 0.8070 0.4269 0.3876 0.058 Uiso 1 1 calc R A 1
C6A C 0.7323(18) 0.2373(18) 0.3573(3) 0.055(3) Uiso 0.441(11) 1 d PD B 1
H6AA H 0.6571 0.1242 0.3586 0.066 Uiso 0.441(11) 1 calc PR B 1
H6AB H 0.8376 0.2540 0.3524 0.066 Uiso 0.441(11) 1 calc PR B 1
H6AC H 0.7016 0.2838 0.3374 0.066 Uiso 0.441(11) 1 calc PR B 1
C6B C 0.6719(12) 0.1720(11) 0.3657(2) 0.042(2) Uiso 0.559(11) 1 d PD B 2
H6BA H 0.6338 0.1970 0.3433 0.051 Uiso 0.559(11) 1 calc PR B 2
H6BB H 0.5859 0.0779 0.3772 0.051 Uiso 0.559(11) 1 calc PR B 2
H6BC H 0.7579 0.1526 0.3596 0.051 Uiso 0.559(11) 1 calc PR B 2
Ni2 Ni -0.22872(7) -0.22872(7) 0.5000 0.03277(19) Uani 1 2 d S . .
N5 N -0.1298(4) -0.0716(4) 0.46396(10) 0.0341(7) Uani 1 1 d . . .
N6 N -0.3924(5) -0.3329(5) 0.46258(10) 0.0440(9) Uani 1 1 d . D .
H600 H -0.4213 -0.4374 0.4614 0.053 Uiso 1 1 calc R . .
H601 H -0.4793 -0.3266 0.4692 0.053 Uiso 1 1 calc R . .
O5 O 0.0079(3) 0.0780(4) 0.47012(8) 0.0397(7) Uani 1 1 d . . .
H5 H 0.063(8) 0.063(8) 0.5000 0.07(2) Uiso 1 2 d S . .
O6 O -0.1335(4) 0.0048(4) 0.40304(8) 0.0456(7) Uani 1 1 d . . .
C7 C -0.1887(5) -0.0946(6) 0.42958(12) 0.0354(9) Uani 1 1 d . D .
C8 C -0.3368(6) -0.2593(7) 0.42537(14) 0.0522(13) Uani 1 1 d D . .
H8 H -0.3159 -0.3283 0.4089 0.063 Uiso 1 1 calc R C 3
C9A C -0.4675(13) -0.229(2) 0.4090(4) 0.071(4) Uiso 0.57(3) 1 d PD D 3
H9AA H -0.4333 -0.1776 0.3850 0.085 Uiso 0.57(3) 1 calc PR D 3
H9AB H -0.4855 -0.1615 0.4257 0.085 Uiso 0.57(3) 1 calc PR D 3
H9AC H -0.5653 -0.3296 0.4060 0.085 Uiso 0.57(3) 1 calc PR D 3
C9B C -0.4634(12) -0.2868(15) 0.3975(3) 0.036(4) Uiso 0.43(3) 1 d PD D 4
H9BA H -0.4162 -0.2551 0.3731 0.043 Uiso 0.43(3) 1 calc PR D 4
H9BB H -0.5123 -0.2245 0.4044 0.043 Uiso 0.43(3) 1 calc PR D 4
H9BC H -0.5435 -0.3986 0.3972 0.043 Uiso 0.43(3) 1 calc PR D 4
K1 K 0.20020(11) 0.29092(11) 0.41704(3) 0.0365(2) Uani 1 1 d . . .
K2 K -0.05184(18) 0.0000 0.3333 0.0525(4) Uani 1 2 d S . .
O1W O 0.1503(5) 0.3266(5) 0.33774(14) 0.0658(11) Uani 1 1 d D . .
H11W H 0.082(6) 0.362(7) 0.3384(18) 0.079 Uiso 1 1 d D . .
H12W H 0.243(4) 0.356(8) 0.3271(16) 0.079 Uiso 1 1 d D . .
O2W O 0.2264(10) 0.0000 0.3333 0.145(4) Uani 1 2 d SD . .
H2W H 0.290(12) 0.106(4) 0.330(4) 0.174 Uiso 1 1 d D . .
O3WA O 0.1070(10) 0.6917(10) 0.3520(2) 0.0538(19) Uiso 0.45 1 d P . .
O3WB O 0.0551(7) 0.5598(8) 0.34735(17) 0.0500(15) Uiso 0.55 1 d P . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ni1 0.0230(2) 0.0335(3) 0.0349(3) 0.0006(2) 0.0015(2) 0.0174(2)
N1 0.0253(16) 0.0393(19) 0.0400(19) -0.0042(16) 0.0033(14) 0.0201(14)
N2 0.0321(19) 0.052(2) 0.042(2) 0.0022(17) 0.0020(16) 0.0272(17)
N3 0.044(2) 0.064(2) 0.038(2) -0.0075(18) -0.0030(16) 0.0412(19)
N4 0.0316(17) 0.038(2) 0.041(2) 0.0015(15) 0.0041(15) 0.0218(16)
O1 0.0325(15) 0.080(3) 0.0481(19) 0.0045(17) 0.0111(14) 0.0403(17)
O2 0.0454(18) 0.0476(18) 0.0343(16) 0.0027(14) 0.0062(14) 0.0214(15)
O3 0.062(2) 0.121(4) 0.042(2) -0.015(2) -0.0097(17) 0.077(3)
C1 0.033(2) 0.035(2) 0.035(2) -0.0008(17) 0.0010(17) 0.0181(18)
C2 0.049(3) 0.062(3) 0.036(2) 0.006(2) 0.004(2) 0.040(2)
C3 0.081(4) 0.187(9) 0.051(4) -0.011(4) -0.014(3) 0.098(6)
C4 0.084(4) 0.121(6) 0.039(3) -0.010(3) -0.013(3) 0.088(4)
C5 0.059(3) 0.071(3) 0.030(2) 0.010(2) 0.007(2) 0.044(3)
Ni2 0.0314(3) 0.0314(3) 0.0304(4) 0.00133(16) -0.00133(16) 0.0119(3)
N5 0.0299(17) 0.0366(18) 0.0333(18) 0.0011(14) 0.0013(14) 0.0148(16)
N6 0.0353(19) 0.042(2) 0.041(2) 0.0044(17) -0.0021(16) 0.0094(17)
O5 0.0348(15) 0.0344(15) 0.0366(17) 0.0041(13) -0.0002(13) 0.0073(13)
O6 0.0462(18) 0.0546(19) 0.0336(16) 0.0078(15) 0.0036(14) 0.0233(16)
C7 0.032(2) 0.050(3) 0.024(2) 0.0020(18) 0.0027(16) 0.021(2)
C8 0.037(2) 0.062(3) 0.036(3) 0.002(2) -0.0042(19) 0.009(3)
K1 0.0355(5) 0.0429(5) 0.0359(5) -0.0037(4) -0.0036(4) 0.0231(4)
K2 0.0688(8) 0.0514(9) 0.0315(7) -0.0012(6) -0.0006(3) 0.0257(4)
O1W 0.056(2) 0.058(2) 0.086(3) -0.004(2) 0.004(2) 0.030(2)
O2W 0.104(4) 0.155(9) 0.193(10) 0.120(9) 0.060(4) 0.078(4)

_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;

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 N3 1.853(4) . ?
Ni1 N1 1.854(3) . ?
Ni1 N2 1.921(4) . ?
Ni1 N4 1.924(3) . ?
N1 C1 1.313(5) . ?
N1 O1 1.399(4) . ?
N2 C2 1.481(6) . ?
N2 H200 0.9000 . ?
N2 H201 0.9000 . ?
N3 C4 1.298(6) . ?
N3 O3 1.389(5) . ?
N4 C5 1.490(6) . ?
N4 H400 0.9000 . ?
N4 H401 0.9000 . ?
O1 K1 2.654(3) 6_556 ?
O1 H1 1.48(9) . ?
O2 C1 1.272(5) . ?
O2 K1 3.069(3) 6_556 ?
O3 K1 2.681(3) . ?
O3 H1 1.06(9) . ?
O4A O4B 0.937(8) . ?
O4A C4 1.338(7) . ?
O4A K1 3.203(8) . ?
O4B C4 1.327(7) . ?
O4B K1 2.791(6) . ?
C1 C2 1.521(6) . ?
C2 C3 1.511(8) . ?
C2 H2 0.9800 . ?
C3 H3A 0.9600 . ?
C3 H3B 0.9600 . ?
C3 H3C 0.9600 . ?
C4 C5 1.490(7) . ?
C5 C6A 1.475(10) . ?
C5 C6B 1.536(8) . ?
C5 H50 0.9800 . ?
C6A H6AA 0.9600 . ?
C6A H6AB 0.9600 . ?
C6A H6AC 0.9600 . ?
C6B H6BA 0.9600 . ?
C6B H6BB 0.9600 . ?
C6B H6BC 0.9600 . ?
Ni2 N5 1.845(3) 6_556 ?
Ni2 N5 1.845(3) . ?
Ni2 N6 1.920(4) . ?
Ni2 N6 1.920(4) 6_556 ?
N5 C7 1.322(5) . ?
N5 O5 1.403(5) . ?
N6 C8 1.472(6) . ?
N6 H600 0.9000 . ?
N6 H601 0.9000 . ?
O5 K1 2.722(3) . ?
O5 H5 1.230(12) . ?
O6 C7 1.258(5) . ?
O6 K2 2.613(3) . ?
O6 K1 3.050(3) . ?
C7 C8 1.519(7) . ?
C8 C9B 1.489(9) . ?
C8 C9A 1.541(10) . ?
C8 H8 0.9800 . ?
C9A H9AA 0.9600 . ?
C9A H9AB 0.9600 . ?
C9A H9AC 0.9600 . ?
C9B H9BA 0.9600 . ?
C9B H9BB 0.9600 . ?
C9B H9BC 0.9600 . ?
K1 O1 2.654(3) 6_556 ?
K1 O1W 2.916(5) . ?
K1 O2 3.069(3) 6_556 ?
K1 K2 3.9788(10) . ?
K2 O6 2.613(3) 4 ?
K2 O2W 2.678(9) . ?
K2 O1W 2.752(4) . ?
K2 O1W 2.752(4) 4 ?
K2 K1 3.9788(10) 4 ?
K2 H11W 3.06(6) . ?
K2 H2W 2.92(11) . ?
O1W H11W 0.88(2) . ?
O1W H12W 0.87(2) . ?
O2W H2W 0.90(2) . ?
O3WA O3WB 1.120(9) . ?

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
N3 Ni1 N1 97.23(15) . . ?
N3 Ni1 N2 175.47(18) . . ?
N1 Ni1 N2 83.10(15) . . ?
N3 Ni1 N4 84.16(15) . . ?
N1 Ni1 N4 175.41(16) . . ?
N2 Ni1 N4 95.86(15) . . ?
C1 N1 O1 115.9(3) . . ?
C1 N1 Ni1 120.4(3) . . ?
O1 N1 Ni1 123.4(3) . . ?
C2 N2 Ni1 111.8(3) . . ?
C2 N2 H200 109.3 . . ?
Ni1 N2 H200 109.3 . . ?
C2 N2 H201 109.3 . . ?
Ni1 N2 H201 109.3 . . ?
H200 N2 H201 107.9 . . ?
C4 N3 O3 116.3(4) . . ?
C4 N3 Ni1 120.3(3) . . ?
O3 N3 Ni1 123.4(3) . . ?
C5 N4 Ni1 111.7(3) . . ?
C5 N4 H400 109.3 . . ?
Ni1 N4 H400 109.3 . . ?
C5 N4 H401 109.3 . . ?
Ni1 N4 H401 109.3 . . ?
H400 N4 H401 108.0 . . ?
N1 O1 K1 128.6(2) . 6_556 ?
N1 O1 H1 105(3) . . ?
K1 O1 H1 126(3) 6_556 . ?
C1 O2 K1 112.7(3) . 6_556 ?
N3 O3 K1 123.4(3) . . ?
N3 O3 H1 106(5) . . ?
K1 O3 H1 113(5) . . ?
O4B O4A C4 68.8(5) . . ?
O4B O4A K1 56.1(5) . . ?
C4 O4A K1 97.9(4) . . ?
O4A O4B C4 70.0(5) . . ?
O4A O4B K1 107.7(6) . . ?
C4 O4B K1 119.7(4) . . ?
O2 C1 N1 126.3(4) . . ?
O2 C1 C2 121.7(4) . . ?
N1 C1 C2 111.9(4) . . ?
N2 C2 C3 112.8(5) . . ?
N2 C2 C1 108.7(3) . . ?
C3 C2 C1 113.5(4) . . ?
N2 C2 H2 107.1 . . ?
C3 C2 H2 107.1 . . ?
C1 C2 H2 107.1 . . ?
C2 C3 H3A 109.5 . . ?
C2 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
C2 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
N3 C4 O4B 120.2(5) . . ?
N3 C4 O4A 128.3(5) . . ?
O4B C4 O4A 41.2(4) . . ?
N3 C4 C5 113.3(4) . . ?
O4B C4 C5 123.8(5) . . ?
O4A C4 C5 111.7(5) . . ?
C6A C5 N4 116.1(6) . . ?
C6A C5 C4 122.2(7) . . ?
N4 C5 C4 110.4(4) . . ?
C6A C5 C6B 25.9(5) . . ?
N4 C5 C6B 109.1(5) . . ?
C4 C5 C6B 107.1(6) . . ?
C6A C5 H50 101.3 . . ?
N4 C5 H50 101.3 . . ?
C4 C5 H50 101.3 . . ?
C6B C5 H50 126.8 . . ?
C5 C6A H6AA 109.5 . . ?
C5 C6A H6AB 109.5 . . ?
C5 C6A H6AC 109.5 . . ?
C5 C6B H6BA 109.5 . . ?
C5 C6B H6BB 109.5 . . ?
H6BA C6B H6BB 109.5 . . ?
C5 C6B H6BC 109.5 . . ?
H6BA C6B H6BC 109.5 . . ?
H6BB C6B H6BC 109.5 . . ?
N5 Ni2 N5 96.2(2) 6_556 . ?
N5 Ni2 N6 179.66(17) 6_556 . ?
N5 Ni2 N6 84.08(15) . . ?
N5 Ni2 N6 84.08(15) 6_556 6_556 ?
N5 Ni2 N6 179.66(17) . 6_556 ?
N6 Ni2 N6 95.7(2) . 6_556 ?
C7 N5 O5 115.0(3) . . ?
C7 N5 Ni2 120.4(3) . . ?
O5 N5 Ni2 124.6(3) . . ?
C8 N6 Ni2 111.6(3) . . ?
C8 N6 H600 109.3 . . ?
Ni2 N6 H600 109.3 . . ?
C8 N6 H601 109.3 . . ?
Ni2 N6 H601 109.3 . . ?
H600 N6 H601 108.0 . . ?
N5 O5 K1 127.0(2) . . ?
N5 O5 H5 105(4) . . ?
K1 O5 H5 121(3) . . ?
C7 O6 K2 135.8(3) . . ?
C7 O6 K1 114.6(3) . . ?
K2 O6 K1 88.92(9) . . ?
O6 C7 N5 125.9(4) . . ?
O6 C7 C8 122.6(4) . . ?
N5 C7 C8 111.5(4) . . ?
N6 C8 C9B 116.5(6) . . ?
N6 C8 C7 109.8(4) . . ?
C9B C8 C7 120.6(6) . . ?
N6 C8 C9A 107.3(6) . . ?
C9B C8 C9A 26.8(5) . . ?
C7 C8 C9A 105.6(7) . . ?
N6 C8 H8 111.3 . . ?
C9B C8 H8 84.7 . . ?
C7 C8 H8 111.3 . . ?
C9A C8 H8 111.3 . . ?
C8 C9A H9AA 109.5 . . ?
C8 C9A H9AB 109.5 . . ?
C8 C9A H9AC 109.5 . . ?
C8 C9B H9BA 109.5 . . ?
C8 C9B H9BB 109.5 . . ?
C8 C9B H9BC 109.5 . . ?
O1 K1 O3 69.71(11) 6_556 . ?
O1 K1 O5 73.20(10) 6_556 . ?
O3 K1 O5 85.85(12) . . ?
O1 K1 O4B 119.51(15) 6_556 . ?
O3 K1 O4B 57.17(13) . . ?
O5 K1 O4B 124.78(15) . . ?
O1 K1 O1W 135.37(11) 6_556 . ?
O3 K1 O1W 135.00(12) . . ?
O5 K1 O1W 132.24(11) . . ?
O4B K1 O1W 79.02(14) . . ?
O1 K1 O6 116.05(11) 6_556 . ?
O3 K1 O6 130.95(13) . . ?
O5 K1 O6 54.65(9) . . ?
O4B K1 O6 119.79(15) . . ?
O1W K1 O6 77.68(10) . . ?
O1 K1 O2 55.43(9) 6_556 6_556 ?
O3 K1 O2 116.84(11) . 6_556 ?
O5 K1 O2 104.11(10) . 6_556 ?
O4B K1 O2 127.96(15) . 6_556 ?
O1W K1 O2 80.76(10) . 6_556 ?
O6 K1 O2 101.60(9) . 6_556 ?
O1 K1 O4A 108.08(16) 6_556 . ?
O3 K1 O4A 56.06(15) . . ?
O5 K1 O4A 135.69(13) . . ?
O4B K1 O4A 16.17(15) . . ?
O1W K1 O4A 79.04(14) . . ?
O6 K1 O4A 134.44(15) . . ?
O2 K1 O4A 112.57(14) 6_556 . ?
O1 K1 K2 153.82(9) 6_556 . ?
O3 K1 K2 132.40(9) . . ?
O5 K1 K2 92.61(7) . . ?
O4B K1 K2 86.66(12) . . ?
O1W K1 K2 43.76(8) . . ?
O6 K1 K2 41.04(6) . . ?
O2 K1 K2 109.66(7) 6_556 . ?
O4A K1 K2 97.47(14) . . ?
O6 K2 O6 143.91(16) 4 . ?
O6 K2 O2W 108.04(8) 4 . ?
O6 K2 O2W 108.04(8) . . ?
O6 K2 O1W 96.40(13) 4 . ?
O6 K2 O1W 88.43(12) . . ?
O2W K2 O1W 82.20(9) . . ?
O6 K2 O1W 88.43(12) 4 4 ?
O6 K2 O1W 96.40(13) . 4 ?
O2W K2 O1W 82.20(9) . 4 ?
O1W K2 O1W 164.39(18) . 4 ?
O6 K2 K1 50.04(7) 4 4 ?
O6 K2 K1 143.32(8) . 4 ?
O2W K2 K1 75.06(3) . 4 ?
O1W K2 K1 127.63(10) . 4 ?
O1W K2 K1 47.11(10) 4 4 ?
O6 K2 K1 143.32(8) 4 . ?
O6 K2 K1 50.04(7) . . ?
O2W K2 K1 75.06(3) . . ?
O1W K2 K1 47.11(10) . . ?
O1W K2 K1 127.63(10) 4 . ?
K1 K2 K1 150.12(6) 4 . ?
O6 K2 H11W 91.4(12) 4 . ?
O6 K2 H11W 83.3(12) . . ?
O2W K2 H11W 98.6(7) . . ?
O1W K2 H11W 16.4(7) . . ?
O1W K2 H11W 179.2(7) 4 . ?
K1 K2 H11W 133.2(12) 4 . ?
K1 K2 H11W 52.6(11) . . ?
O6 K2 H2W 105(2) 4 . ?
O6 K2 H2W 109(2) . . ?
O2W K2 H2W 17.7(11) . . ?
O1W K2 H2W 64.8(12) . . ?
O1W K2 H2W 99.6(11) 4 . ?
K1 K2 H2W 85(2) 4 . ?
K1 K2 H2W 66(2) . . ?
H11W K2 H2W 81.2(13) . . ?
K2 O1W K1 89.13(13) . . ?
K2 O1W H11W 102(4) . . ?
K1 O1W H11W 103(4) . . ?
K2 O1W H12W 112(4) . . ?
K1 O1W H12W 105(4) . . ?
H11W O1W H12W 136(6) . . ?
K2 O2W H2W 97(8) . . ?

_diffrn_measured_fraction_theta_max 0.970
_diffrn_reflns_theta_full        28.00
_diffrn_measured_fraction_theta_full 0.970
_refine_diff_density_max         0.507
_refine_diff_density_min         -0.448
_refine_diff_density_rms         0.090