# Supplementary Material (ESI) for Chemical Communications
# This journal is © The Royal Society of Chemistry 2005


data_global
_journal_name_full               Chem.Commun.

_journal_coden_Cambridge         0182

_publ_contact_author_name        'Prof R Winpenny'
_publ_contact_author_address     
;
Department of Chemistry
The University of Manchester
Oxford Road
Manchester
M13 9PL
UNITED KINGDOM
;

_publ_contact_author_email       RICHARD.WINPENNY@MAN.AC.UK

_publ_section_title              
;
Synthesis and Characterisation of a {Ni8} Single
Molecule Magnet and A Related Cage
;
loop_
_publ_author_name
'R. Winpenny'
'Guillem. Aromi'
'Aidan Bell'
'S. J. Teat'
'Wolfgang Wernsdorfer'

data_ab148b
_database_code_depnum_ccdc_archive 'CCDC 260899'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C120 H155 F8 N12 Na2 Ni8 O26.5'
_chemical_formula_weight         2913.26

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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Na Na 0.0362 0.0249 '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'

_symmetry_cell_setting           cubic
_symmetry_space_group_name_H-M   I432

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

_cell_length_a                   29.5764(13)
_cell_length_b                   29.5764(13)
_cell_length_c                   29.5764(13)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     25872(2)
_cell_formula_units_Z            6
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    37432
_cell_measurement_theta_min      2.31
_cell_measurement_theta_max      28.86

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.06
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.122
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             9102
_exptl_absorpt_coefficient_mu    0.924
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.82
_exptl_absorpt_correction_T_max  0.90
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.6888
_diffrn_radiation_type           synchrotron
_diffrn_radiation_source         'Daresbury SRS station 9.8'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_measurement_device_type  'Bruker SMART 1K CCD diffractometer'
_diffrn_measurement_method       '\w rotation with narrow frames'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  .
_diffrn_standards_decay_%        .
_diffrn_reflns_number            92274
_diffrn_reflns_av_R_equivalents  0.0625
_diffrn_reflns_av_sigmaI/netI    0.0305
_diffrn_reflns_limit_h_min       -41
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_k_max       42
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_theta_min         1.63
_diffrn_reflns_theta_max         29.57
_reflns_number_total             6537
_reflns_number_gt                6096
_reflns_threshold_expression     I>2\s(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL and local programs'

_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.
All non-hydrogens were refined anisotopically except those with partial
occupancy. From anisotropic dispalcement parameters it can be seen that
the carboxyl group is pivoting about the oxygens and is being displace
perpendicular to its phenyl ring. This has resulted in anisotropic
displacement parameter ration of 6:1 from the furtherest from the carboxyl
group, while this is not ideal it does reflect the movement in this
molecule. It was considered splitting these atom site however no new
chemical information would result. Geometrical and dispalcement parameter
restrains were used to model the t-butyl group. The ROH, OH, and NH
hydrogens were found in the difference map, the other hydrogens were
placed geometrically. The hydrogen on the water could neither be found
and place and were therefore omitted from the refinement. The hydrogens
were then refined with a riding model, except for the hydroxide H which was
allowed to refine freely.
;

_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^)+(0.0925P)^2^+25.4694P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_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   0.045(17)
_refine_ls_number_reflns         6537
_refine_ls_number_parameters     212
_refine_ls_number_restraints     147
_refine_ls_R_factor_all          0.0504
_refine_ls_R_factor_gt           0.0459
_refine_ls_wR_factor_ref         0.1394
_refine_ls_wR_factor_gt          0.1349
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_restrained_S_all      1.108
_refine_ls_shift/su_max          0.003
_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 0.588477(10) 0.971433(10) 0.933863(10) 0.02184(9) Uani 1 1 d . . .
Na1 Na 0.5000 1.0000 1.0000 0.0180(4) Uani 1 8 d S . .
F1 F 0.54659(4) 1.02423(4) 0.93850(4) 0.0197(2) Uani 1 1 d . . .
O1 O 0.61208(12) 1.0000 1.0000 0.0241(6) Uani 1 4 d S . .
H1O H 0.646(3) 1.0000 1.0000 0.05(2) Uiso 1 4 d S . .
N11 N 0.55561(8) 0.94537(8) 0.87860(7) 0.0282(4) Uani 1 1 d . . .
O11 O 0.61645(9) 0.91914(13) 0.83519(11) 0.0611(9) Uani 1 1 d . . .
H11 H 0.6289 0.9173 0.8607 0.092 Uiso 1 1 calc R . .
C11 C 0.57180(12) 0.92713(11) 0.84056(10) 0.0382(6) Uani 1 1 d . . .
N12 N 0.51034(9) 0.94688(8) 0.87196(8) 0.0313(5) Uani 1 1 d . . .
H12A H 0.4910 0.9577 0.8919 0.038 Uiso 1 1 calc R . .
C12 C 0.53752(13) 0.91735(13) 0.81001(11) 0.0457(8) Uani 1 1 d . . .
H12B H 0.5405 0.9047 0.7806 0.055 Uiso 1 1 calc R . .
C13 C 0.49824(13) 0.93002(12) 0.83169(10) 0.0415(7) Uani 1 1 d . . .
C14 C 0.45000(15) 0.9273(2) 0.81792(15) 0.0703(14) Uani 1 1 d . . .
H14A H 0.4331 0.9097 0.8404 0.106 Uiso 1 1 calc R . .
H14B H 0.4478 0.9124 0.7884 0.106 Uiso 1 1 calc R . .
H14C H 0.4373 0.9578 0.8159 0.106 Uiso 1 1 calc R . .
O21 O 0.63495(7) 0.92156(7) 0.92773(7) 0.0341(4) Uani 1 1 d U . .
O22 O 0.63100(7) 0.89152(7) 0.99644(8) 0.0358(4) Uani 1 1 d U . .
C21 C 0.64310(9) 0.89090(9) 0.95607(9) 0.0284(5) Uani 1 1 d U . .
C22 C 0.66938(10) 0.85066(9) 0.94026(10) 0.0332(5) Uani 1 1 d U . .
C23 C 0.66943(15) 0.81141(13) 0.96552(13) 0.0526(9) Uani 1 1 d U . .
H23A H 0.6542 0.8106 0.9938 0.063 Uiso 1 1 calc R . .
C24 C 0.69155(17) 0.77315(14) 0.95006(14) 0.0587(11) Uani 1 1 d U . .
H24A H 0.6903 0.7461 0.9674 0.070 Uiso 1 1 calc R . .
C25 C 0.71539(16) 0.77353(13) 0.90993(13) 0.0552(10) Uani 1 1 d DU A .
C26 C 0.7161(2) 0.81258(17) 0.88588(16) 0.0742(14) Uani 1 1 d U . .
H26A H 0.7328 0.8137 0.8585 0.089 Uiso 1 1 calc R . .
C27 C 0.69289(18) 0.85127(14) 0.90014(15) 0.0638(12) Uani 1 1 d U . .
H27A H 0.6934 0.8779 0.8822 0.077 Uiso 1 1 calc R . .
C28 C 0.73946(17) 0.73105(15) 0.89351(15) 0.0772(14) Uani 1 1 d DU . .
C29 C 0.7868(3) 0.7301(4) 0.9210(4) 0.078(3) Uiso 0.50 1 d PDU A 1
H29A H 0.8042 0.7033 0.9121 0.117 Uiso 0.50 1 calc PR A 1
H29B H 0.7806 0.7289 0.9536 0.117 Uiso 0.50 1 calc PR A 1
H29C H 0.8042 0.7574 0.9140 0.117 Uiso 0.50 1 calc PR A 1
C30 C 0.7548(3) 0.7361(3) 0.8423(3) 0.057(2) Uiso 0.50 1 d PDU A 1
H30A H 0.7702 0.7085 0.8326 0.086 Uiso 0.50 1 calc PR A 1
H30B H 0.7754 0.7619 0.8394 0.086 Uiso 0.50 1 calc PR A 1
H30C H 0.7281 0.7412 0.8232 0.086 Uiso 0.50 1 calc PR A 1
C31 C 0.7147(4) 0.6876(3) 0.9002(5) 0.093(4) Uiso 0.50 1 d PDU A 1
H31A H 0.7330 0.6626 0.8888 0.139 Uiso 0.50 1 calc PR A 1
H31B H 0.6859 0.6887 0.8838 0.139 Uiso 0.50 1 calc PR A 1
H31C H 0.7087 0.6832 0.9325 0.139 Uiso 0.50 1 calc PR A 1
C29' C 0.7589(5) 0.7029(5) 0.9332(4) 0.112(4) Uiso 0.50 1 d PDU A 2
H29D H 0.7739 0.6758 0.9213 0.168 Uiso 0.50 1 calc PR A 2
H29E H 0.7342 0.6938 0.9534 0.168 Uiso 0.50 1 calc PR A 2
H29F H 0.7808 0.7211 0.9500 0.168 Uiso 0.50 1 calc PR A 2
C30' C 0.7678(3) 0.7374(3) 0.8516(3) 0.056(2) Uiso 0.50 1 d PDU A 2
H30D H 0.7821 0.7086 0.8435 0.084 Uiso 0.50 1 calc PR A 2
H30E H 0.7912 0.7601 0.8575 0.084 Uiso 0.50 1 calc PR A 2
H30F H 0.7486 0.7476 0.8267 0.084 Uiso 0.50 1 calc PR A 2
C31' C 0.6970(3) 0.6962(3) 0.8796(3) 0.063(2) Uiso 0.50 1 d PDU A 2
H31D H 0.7095 0.6675 0.8686 0.094 Uiso 0.50 1 calc PR A 2
H31E H 0.6787 0.7101 0.8558 0.094 Uiso 0.50 1 calc PR A 2
H31F H 0.6782 0.6906 0.9063 0.094 Uiso 0.50 1 calc PR A 2
Na2 Na 0.7331(7) 0.9184(7) 1.0280(7) 0.087(5) Uiso 0.13 1 d P . .
O1W O 0.7146(14) 1.0000 1.0000 0.099(11) Uiso 0.25 4 d SP . .

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 0.02288(15) 0.01960(14) 0.02304(15) 0.00089(10) 0.00644(10) 0.00094(10)
Na1 0.0187(11) 0.0176(6) 0.0176(6) 0.000 0.000 0.000
F1 0.0213(6) 0.0193(6) 0.0184(6) 0.0001(4) -0.0009(4) -0.0012(5)
O1 0.0226(15) 0.0249(9) 0.0249(9) 0.000 0.000 0.000
N11 0.0330(11) 0.0266(10) 0.0249(9) -0.0043(8) 0.0103(8) -0.0014(8)
O11 0.0435(14) 0.087(2) 0.0533(15) -0.0348(16) 0.0192(12) -0.0001(14)
C11 0.0428(15) 0.0397(15) 0.0321(13) -0.0105(11) 0.0150(12) -0.0018(12)
N12 0.0355(12) 0.0358(11) 0.0228(10) -0.0051(8) 0.0046(8) 0.0043(9)
C12 0.058(2) 0.0522(18) 0.0273(13) -0.0145(13) 0.0088(13) 0.0027(15)
C13 0.0503(17) 0.0494(17) 0.0249(12) -0.0078(11) 0.0004(12) 0.0062(15)
C14 0.048(2) 0.119(4) 0.045(2) -0.029(2) -0.0111(17) 0.010(2)
O21 0.0383(10) 0.0280(9) 0.0360(10) 0.0026(7) 0.0126(8) 0.0098(8)
O22 0.0400(10) 0.0367(10) 0.0308(9) -0.0017(8) 0.0030(8) 0.0183(8)
C21 0.0259(11) 0.0263(11) 0.0331(12) -0.0044(9) 0.0053(9) 0.0060(9)
C22 0.0350(13) 0.0301(12) 0.0346(13) -0.0025(10) 0.0063(11) 0.0126(10)
C23 0.074(2) 0.0427(17) 0.0414(16) 0.0075(13) 0.0174(17) 0.0288(17)
C24 0.082(3) 0.0451(18) 0.0491(19) 0.0083(15) 0.0143(19) 0.0320(19)
C25 0.078(2) 0.0440(17) 0.0435(16) -0.0081(14) 0.0077(17) 0.0373(17)
C26 0.106(3) 0.060(2) 0.056(2) 0.0088(18) 0.041(2) 0.047(2)
C27 0.087(3) 0.0460(19) 0.059(2) 0.0136(16) 0.040(2) 0.0331(19)
C28 0.111(3) 0.061(2) 0.060(2) -0.0096(18) 0.012(2) 0.053(2)

_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 Na1 3.3746(3) . ?
Ni1 F1 1.9981(13) . ?
Ni1 F1 2.0050(13) 17_557 ?
Ni1 O1 2.2422(12) . ?
Ni1 N11 2.052(2) . ?
Ni1 O21 2.0242(19) . ?
Ni1 O22 2.013(2) 20_575 ?
Na1 Ni1 3.3746(3) 18_655 ?
Na1 Ni1 3.3746(3) 2_675 ?
Na1 Ni1 3.3746(3) 3_657 ?
Na1 Ni1 3.3746(3) 4_577 ?
Na1 F1 2.3918(13) . ?
Na1 F1 2.3918(13) 2_675 ?
Na1 F1 2.3918(13) 18_655 ?
Na1 F1 2.3918(13) 3_657 ?
Na1 F1 2.3918(13) 19_677 ?
Na1 F1 2.3918(13) 20_575 ?
Na1 F1 2.3918(13) 4_577 ?
Na1 F1 2.3918(13) 17_557 ?
F1 Ni1 2.0050(13) 20_575 ?
O1 Ni1 2.2422(11) 4_577 ?
O1 Ni1 2.2422(11) 17_557 ?
O1 Ni1 2.2422(11) 20_575 ?
N11 C11 1.336(3) . ?
N11 N12 1.354(3) . ?
O11 C11 1.351(4) . ?
C11 C12 1.388(5) . ?
N12 C13 1.340(4) . ?
C12 C13 1.379(5) . ?
C13 C14 1.486(6) . ?
O21 C21 1.258(3) . ?
O22 Ni1 2.0133(19) 17_557 ?
O22 C21 1.247(3) . ?
C21 C22 1.496(3) . ?
C22 C23 1.381(4) . ?
C22 C27 1.376(4) . ?
C23 C24 1.385(5) . ?
C24 C25 1.381(6) . ?
C25 C26 1.356(6) . ?
C25 C28 1.524(5) . ?
C26 C27 1.399(5) . ?
C28 C29 1.620(8) . ?
C28 C30 1.589(8) . ?
C28 C31 1.492(9) . ?
C28 C29' 1.550(9) . ?
C28 C30' 1.508(8) . ?
C28 C31' 1.675(8) . ?
Na2 Na2 3.61(3) 17_557 ?
Na2 Na2 3.61(3) 20_575 ?
Na2 O1W 2.61(2) . ?
O1W Na2 2.61(2) 17_557 ?
O1W Na2 2.61(2) 20_575 ?
O1W Na2 2.61(2) 4_577 ?

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
Na1 Ni1 F1 44.25(4) . . ?
Na1 Ni1 F1 44.29(4) . 17_557 ?
Na1 Ni1 O1 68.98(9) . . ?
Na1 Ni1 N11 100.86(6) . . ?
Na1 Ni1 O21 139.55(6) . . ?
Na1 Ni1 O22 136.62(6) . 20_575 ?
F1 Ni1 F1 87.37(8) . 17_557 ?
F1 Ni1 O1 80.72(7) . . ?
F1 Ni1 O1 80.57(7) 17_557 . ?
F1 Ni1 N11 93.12(8) . . ?
F1 Ni1 N11 90.98(7) 17_557 . ?
F1 Ni1 O21 175.31(8) . . ?
F1 Ni1 O21 96.95(7) 17_557 . ?
F1 Ni1 O22 93.51(8) . 20_575 ?
F1 Ni1 O22 179.09(8) 17_557 20_575 ?
O1 Ni1 N11 169.72(11) . . ?
O1 Ni1 O21 98.13(9) . . ?
O1 Ni1 O22 99.81(9) . 20_575 ?
N11 Ni1 O21 88.66(10) . . ?
N11 Ni1 O22 88.72(9) . 20_575 ?
O21 Ni1 O22 82.18(9) . 20_575 ?
Ni1 Na1 Ni1 53.035(7) 18_655 2_675 ?
Ni1 Na1 Ni1 53.036(7) 18_655 3_657 ?
Ni1 Na1 Ni1 78.309(11) 2_675 3_657 ?
Ni1 Na1 Ni1 153.072(10) 18_655 4_577 ?
Ni1 Na1 Ni1 151.001(10) 2_675 4_577 ?
Ni1 Na1 Ni1 109.148(11) 3_657 4_577 ?
Ni1 Na1 F1 35.83(3) 18_655 2_675 ?
Ni1 Na1 F1 35.66(3) 18_655 18_655 ?
Ni1 Na1 F1 85.26(3) 18_655 3_657 ?
Ni1 Na1 F1 85.36(3) 18_655 19_677 ?
Ni1 Na1 F1 115.47(3) 18_655 . ?
Ni1 Na1 F1 164.27(3) 18_655 20_575 ?
Ni1 Na1 F1 117.61(3) 18_655 4_577 ?
Ni1 Na1 F1 86.04(3) 18_655 17_557 ?
Ni1 Na1 F1 35.66(3) 2_675 2_675 ?
Ni1 Na1 F1 85.26(3) 2_675 18_655 ?
Ni1 Na1 F1 85.36(3) 2_675 3_657 ?
Ni1 Na1 F1 35.83(3) 2_675 19_677 ?
Ni1 Na1 F1 86.04(3) 2_675 . ?
Ni1 Na1 F1 115.47(3) 2_675 20_575 ?
Ni1 Na1 F1 164.27(3) 2_675 4_577 ?
Ni1 Na1 F1 117.61(3) 2_675 17_557 ?
Ni1 Na1 F1 85.36(3) 3_657 2_675 ?
Ni1 Na1 F1 35.83(3) 3_657 18_655 ?
Ni1 Na1 F1 35.66(3) 3_657 3_657 ?
Ni1 Na1 F1 85.26(3) 3_657 19_677 ?
Ni1 Na1 F1 164.27(3) 3_657 . ?
Ni1 Na1 F1 117.61(3) 3_657 20_575 ?
Ni1 Na1 F1 86.04(3) 3_657 4_577 ?
Ni1 Na1 F1 115.47(3) 3_657 17_557 ?
Ni1 Na1 F1 164.27(3) 4_577 2_675 ?
Ni1 Na1 F1 117.61(3) 4_577 18_655 ?
Ni1 Na1 F1 86.04(3) 4_577 3_657 ?
Ni1 Na1 F1 115.47(3) 4_577 19_677 ?
Ni1 Na1 F1 85.36(3) 4_577 . ?
Ni1 Na1 F1 35.83(3) 4_577 20_575 ?
Ni1 Na1 F1 35.66(3) 4_577 4_577 ?
Ni1 Na1 F1 85.26(3) 4_577 17_557 ?
F1 Na1 F1 70.62(3) 2_675 18_655 ?
F1 Na1 F1 109.65(6) 2_675 3_657 ?
F1 Na1 F1 70.62(3) 18_655 3_657 ?
F1 Na1 F1 70.62(3) 2_675 19_677 ?
F1 Na1 F1 109.65(6) 18_655 19_677 ?
F1 Na1 F1 70.62(3) 3_657 19_677 ?
F1 Na1 F1 80.98(6) . 2_675 ?
F1 Na1 F1 141.96(6) . 18_655 ?
F1 Na1 F1 145.13(6) . 3_657 ?
F1 Na1 F1 82.88(6) . 19_677 ?
F1 Na1 F1 141.96(6) 2_675 20_575 ?
F1 Na1 F1 145.13(6) 18_655 20_575 ?
F1 Na1 F1 82.88(6) 3_657 20_575 ?
F1 Na1 F1 80.98(6) 19_677 20_575 ?
F1 Na1 F1 70.62(3) . 20_575 ?
F1 Na1 F1 145.13(6) 2_675 4_577 ?
F1 Na1 F1 82.88(6) 18_655 4_577 ?
F1 Na1 F1 80.98(6) 3_657 4_577 ?
F1 Na1 F1 141.96(6) 19_677 4_577 ?
F1 Na1 F1 109.65(6) . 4_577 ?
F1 Na1 F1 70.62(3) 20_575 4_577 ?
F1 Na1 F1 82.88(6) 2_675 17_557 ?
F1 Na1 F1 80.98(6) 18_655 17_557 ?
F1 Na1 F1 141.96(6) 3_657 17_557 ?
F1 Na1 F1 145.13(6) 19_677 17_557 ?
F1 Na1 F1 70.62(3) . 17_557 ?
F1 Na1 F1 109.65(6) 20_575 17_557 ?
F1 Na1 F1 70.62(3) 4_577 17_557 ?
Ni1 F1 Ni1 97.66(6) . 20_575 ?
Ni1 F1 Na1 100.09(5) . . ?
Ni1 F1 Na1 99.89(5) 20_575 . ?
Ni1 O1 Ni1 143.72(17) . 4_577 ?
Ni1 O1 Ni1 84.44(5) . 17_557 ?
Ni1 O1 Ni1 84.44(5) 4_577 17_557 ?
Ni1 O1 Ni1 84.44(5) . 20_575 ?
Ni1 O1 Ni1 84.44(5) 4_577 20_575 ?
Ni1 O1 Ni1 143.72(17) 17_557 20_575 ?
Ni1 N11 C11 130.7(2) . . ?
Ni1 N11 N12 124.85(16) . . ?
C11 N11 N12 104.2(2) . . ?
N11 C11 O11 121.3(3) . . ?
N11 C11 C12 111.7(3) . . ?
O11 C11 C12 126.9(3) . . ?
N11 N12 C13 112.4(2) . . ?
C11 C12 C13 104.8(3) . . ?
N12 C13 C12 106.8(3) . . ?
N12 C13 C14 121.4(3) . . ?
C12 C13 C14 131.8(3) . . ?
Ni1 O21 C21 126.56(17) . . ?
Ni1 O22 C21 129.84(19) 17_557 . ?
O21 C21 O22 124.9(2) . . ?
O21 C21 C22 117.7(2) . . ?
O22 C21 C22 117.4(2) . . ?
C21 C22 C23 120.0(3) . . ?
C21 C22 C27 121.4(3) . . ?
C23 C22 C27 118.5(3) . . ?
C22 C23 C24 120.6(3) . . ?
C23 C24 C25 121.2(4) . . ?
C24 C25 C26 117.7(3) . . ?
C24 C25 C28 120.4(4) . . ?
C26 C25 C28 121.9(3) . . ?
C25 C26 C27 122.1(4) . . ?
C22 C27 C26 119.8(4) . . ?
C25 C28 C29 105.0(5) . . ?
C25 C28 C30 111.1(5) . . ?
C25 C28 C31 116.0(6) . . ?
C25 C28 C29' 112.0(6) . . ?
C25 C28 C30' 114.8(5) . . ?
C25 C28 C31' 103.6(5) . . ?
C29 C28 C30 103.6(6) . . ?
C29 C28 C31 110.0(7) . . ?
C29 C28 C29' 44.7(7) . . ?
C29 C28 C30' 86.2(6) . . ?
C29 C28 C31' 139.4(6) . . ?
C30 C28 C31 110.4(7) . . ?
C30 C28 C29' 131.9(7) . . ?
C30 C28 C30' 17.4(5) . . ?
C30 C28 C31' 92.2(5) . . ?
C31 C28 C29' 67.6(8) . . ?
C31 C28 C30' 119.3(7) . . ?
C31 C28 C31' 30.1(6) . . ?
C29' C28 C30' 118.9(7) . . ?
C29' C28 C31' 97.6(7) . . ?
C30' C28 C31' 107.0(6) . . ?
Na2 Na2 Na2 90.000(4) 17_557 20_575 ?
Na2 Na2 O1W 46.3(2) 17_557 . ?
Na2 Na2 O1W 46.3(2) 20_575 . ?
Na2 O1W Na2 87.5(4) . 17_557 ?
Na2 O1W Na2 87.5(4) . 20_575 ?
Na2 O1W Na2 156(2) 17_557 20_575 ?
Na2 O1W Na2 156(2) . 4_577 ?
Na2 O1W Na2 87.5(4) 17_557 4_577 ?
Na2 O1W Na2 87.5(4) 20_575 4_577 ?

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
O1 H1O O1W 1.01(9) 2.02(10) 3.03(4) 180.000(4) .
O11 H11 O21 0.84 2.00 2.792(4) 157.9 .
N12 H12A F1 0.88 1.85 2.727(3) 173.3 2_675

_diffrn_measured_fraction_theta_max 0.988
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.778
_refine_diff_density_min         -0.536
_refine_diff_density_rms         0.105

data_13
_database_code_depnum_ccdc_archive 'CCDC 260900'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C77.30 H115 N56 Na2 Ni8 O29.30'
_chemical_formula_weight         2790.53

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'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P2(1)/n

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

_cell_length_a                   16.055(6)
_cell_length_b                   16.408(6)
_cell_length_c                   23.826(9)
_cell_angle_alpha                90.00
_cell_angle_beta                 103.176(7)
_cell_angle_gamma                90.00
_cell_volume                     6111(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    3332
_cell_measurement_theta_min      2.30
_cell_measurement_theta_max      23.47

_exptl_crystal_description       Prismatic
_exptl_crystal_colour            Green
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      0
_exptl_crystal_density_diffrn    1.517
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2857
_exptl_absorpt_coefficient_mu    1.302
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      100(2)
_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  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            31266
_diffrn_reflns_av_R_equivalents  0.1139
_diffrn_reflns_av_sigmaI/netI    0.1450
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_theta_min         1.40
_diffrn_reflns_theta_max         25.03
_reflns_number_total             10805
_reflns_number_gt                6173
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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. The weighting scheme was
not changed from default.

The structure was solved by direct methods. The asymmetric unit contains
half the cluster, with only a single disorded water molecule as solvent.
The arrangement of bound solvate (ethyl acetate) molecules around Na1 is
split into two parts to describe the disorder. The C16T molecule did not
appear in the difference map and was therefore excluded from the refinement,
this is presumably due to the degrees of freedom and the level of disorder.
There are also some relatively large peaks remaining in the electron density
map (1.94 being the largest). These are assumed to be extra disorded
solvate molecules around Na1. These peaks have not been modelled as doing so
proved extremely difficult and added no new structural data, particularly as
the environment surrounding the sodium is magnetically irrelevent. There is
no other significant disorder.

The non-H atoms were refined anisotropically, except for the disordered
atoms. H atoms bonded were included in calculated positions except the
-OH moiety of the pyrazole ring which were found within the electron density
map.

;

_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^)+(0.1000P)^2^+0.0000P] 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_number_reflns         10805
_refine_ls_number_parameters     810
_refine_ls_number_restraints     147
_refine_ls_R_factor_all          0.1077
_refine_ls_R_factor_gt           0.0573
_refine_ls_wR_factor_ref         0.1747
_refine_ls_wR_factor_gt          0.1522
_refine_ls_goodness_of_fit_ref   0.836
_refine_ls_restrained_S_all      0.844
_refine_ls_shift/su_max          0.002
_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 0.31230(5) 1.95156(5) 0.18048(4) 0.0175(2) Uani 1 1 d . . .
Ni2 Ni 0.28427(5) 2.09298(5) 0.04917(3) 0.0153(2) Uani 1 1 d . . .
Ni3 Ni 0.43409(5) 1.96185(5) 0.09512(3) 0.0157(2) Uani 1 1 d . . .
Ni4 Ni 0.42033(5) 2.06286(5) -0.02169(3) 0.0146(2) Uani 1 1 d . . .
Na1 Na 0.69123(19) 1.9664(2) 0.28971(14) 0.0448(9) Uani 1 1 d D . .
N101 N 0.2946(3) 1.9738(3) 0.0876(2) 0.0163(12) Uani 1 1 d . . .
N102 N 0.2524(3) 1.9193(4) 0.0588(2) 0.0181(13) Uani 1 1 d . . .
N103 N 0.2131(4) 1.8685(4) 0.0330(3) 0.0272(14) Uani 1 1 d . . .
N104 N 0.4323(3) 1.9896(3) 0.1783(2) 0.0193(13) Uani 1 1 d . A .
N105 N 0.4888(4) 2.0052(4) 0.2194(3) 0.0306(15) Uani 1 1 d . . .
N106 N 0.5422(4) 2.0195(5) 0.2592(3) 0.059(2) Uani 1 1 d . A .
N107 N 0.4196(3) 2.0810(3) 0.0660(2) 0.0163(12) Uani 1 1 d . . .
N108 N 0.4634(4) 2.1316(4) 0.0977(3) 0.0233(14) Uani 1 1 d . . .
N109 N 0.5027(4) 2.1784(4) 0.1278(3) 0.0399(17) Uani 1 1 d . . .
N110 N 0.2911(3) 2.0395(3) -0.0291(2) 0.0160(12) Uani 1 1 d . . .
N111 N 0.2382(3) 2.0547(3) -0.0736(2) 0.0213(13) Uani 1 1 d . . .
N112 N 0.1871(4) 2.0670(4) -0.1143(3) 0.0323(16) Uani 1 1 d . . .
N113 N 0.4437(3) 1.9385(3) 0.0088(2) 0.0175(12) Uani 1 1 d . . .
N114 N 0.4016(3) 1.8817(3) -0.0179(2) 0.0191(13) Uani 1 1 d . . .
N115 N 0.3645(4) 1.8285(4) -0.0417(3) 0.0316(15) Uani 1 1 d . . .
N116 N 0.5658(3) 1.9621(3) 0.1051(2) 0.0165(12) Uani 1 1 d . . .
N117 N 0.6104(4) 1.9354(4) 0.1480(2) 0.0236(13) Uani 1 1 d . . .
N118 N 0.6522(4) 1.9088(4) 0.1901(3) 0.0393(17) Uani 1 1 d . A .
O11 O 0.3391(3) 1.8286(3) 0.16715(18) 0.0205(11) Uani 1 1 d D . .
O12 O 0.4243(3) 1.8381(3) 0.10577(18) 0.0211(11) Uani 1 1 d D . .
C11 C 0.3773(3) 1.7998(4) 0.1312(2) 0.0205(16) Uani 1 1 d D . .
C12 C 0.3632(4) 1.7097(4) 0.1174(3) 0.0253(17) Uani 1 1 d D . .
C13 C 0.3442(5) 1.6556(5) 0.1583(4) 0.042(2) Uani 1 1 d D . .
H13 H 0.3386 1.6757 0.1946 0.051 Uiso 1 1 calc R . .
C14 C 0.3334(6) 1.5732(5) 0.1464(4) 0.050(2) Uani 1 1 d D . .
H14 H 0.3227 1.5368 0.1749 0.060 Uiso 1 1 calc R . .
C15 C 0.3385(6) 1.5437(5) 0.0921(4) 0.054(3) Uani 1 1 d D . .
H15 H 0.3292 1.4876 0.0829 0.065 Uiso 1 1 calc R . .
C16 C 0.3569(5) 1.5971(5) 0.0525(4) 0.046(2) Uani 1 1 d D . .
H16 H 0.3611 1.5773 0.0158 0.055 Uiso 1 1 calc R . .
C17 C 0.3697(5) 1.6795(5) 0.0647(3) 0.0341(19) Uani 1 1 d D . .
H17 H 0.3830 1.7151 0.0366 0.041 Uiso 1 1 calc R . .
O21 O 0.3529(4) 2.0550(4) 0.3102(2) 0.0382(14) Uani 1 1 d D . .
H21 H 0.323(5) 2.075(5) 0.274(4) 0.057 Uiso 1 1 d . . .
N21 N 0.3449(3) 1.9266(3) 0.2678(2) 0.0233(13) Uani 1 1 d D . .
N22 N 0.3610(3) 1.8490(4) 0.2886(2) 0.0272(14) Uani 1 1 d D . .
H22 H 0.3548 1.8049 0.2671 0.033 Uiso 1 1 calc R . .
C21 C 0.3617(5) 1.9748(5) 0.3136(3) 0.0303(18) Uani 1 1 d D . .
C22 C 0.3900(5) 1.9277(5) 0.3646(3) 0.040(2) Uani 1 1 d D . .
H22' H 0.4070 1.9473 0.4031 0.048 Uiso 1 1 calc R . .
C23 C 0.3875(5) 1.8490(5) 0.3467(3) 0.036(2) Uani 1 1 d D . .
C24 C 0.4088(5) 1.7700(5) 0.3789(3) 0.050(2) Uani 1 1 d D . .
H24A H 0.3623 1.7309 0.3657 0.075 Uiso 1 1 calc R . .
H24B H 0.4157 1.7798 0.4203 0.075 Uiso 1 1 calc R . .
H24C H 0.4621 1.7480 0.3717 0.075 Uiso 1 1 calc R . .
O31 O 0.1127(3) 2.0226(3) 0.1917(2) 0.0284(13) Uani 1 1 d D . .
H31 H 0.154(5) 2.040(5) 0.197(4) 0.043 Uiso 1 1 d . . .
N31 N 0.1885(3) 1.9105(3) 0.1707(2) 0.0196(13) Uani 1 1 d D . .
N32 N 0.1662(3) 1.8319(3) 0.1550(2) 0.0213(13) Uani 1 1 d D . .
H32 H 0.2026 1.7949 0.1485 0.026 Uiso 1 1 calc R . .
C31 C 0.1153(4) 1.9446(4) 0.1753(3) 0.0216(16) Uani 1 1 d D . .
C32 C 0.0484(4) 1.8890(4) 0.1630(3) 0.0245(17) Uani 1 1 d D . .
H32' H -0.0098 1.8988 0.1632 0.029 Uiso 1 1 calc R . .
C33 C 0.0835(4) 1.8178(4) 0.1505(3) 0.0236(16) Uani 1 1 d D . .
C34 C 0.0467(5) 1.7347(4) 0.1347(3) 0.0320(18) Uani 1 1 d D . .
H34A H 0.0838 1.7046 0.1145 0.048 Uiso 1 1 calc R . .
H34B H -0.0105 1.7401 0.1094 0.048 Uiso 1 1 calc R . .
H34C H 0.0427 1.7052 0.1697 0.048 Uiso 1 1 calc R . .
O41 O 0.2722(3) 2.0649(3) 0.20096(18) 0.0197(10) Uani 1 1 d D . .
N41 N 0.2926(3) 2.1517(3) 0.1266(2) 0.0187(13) Uani 1 1 d D . .
N42 N 0.3112(3) 2.2327(3) 0.1255(2) 0.0210(13) Uani 1 1 d D . .
H42 H 0.3168 2.2584 0.0941 0.025 Uiso 1 1 calc R . .
C41 C 0.2898(4) 2.1370(4) 0.1820(3) 0.0182(15) Uani 1 1 d D . .
C42 C 0.3075(4) 2.2096(4) 0.2145(3) 0.0216(16) Uani 1 1 d D . .
H42' H 0.3102 2.2157 0.2545 0.026 Uiso 1 1 calc R . .
C43 C 0.3202(4) 2.2697(4) 0.1769(3) 0.0224(16) Uani 1 1 d D . .
C44 C 0.3407(5) 2.3583(4) 0.1843(3) 0.0283(17) Uani 1 1 d D . .
H44A H 0.3937 2.3696 0.1720 0.042 Uiso 1 1 calc R . .
H44B H 0.3480 2.3732 0.2250 0.042 Uiso 1 1 calc R . .
H44C H 0.2939 2.3902 0.1609 0.042 Uiso 1 1 calc R . .
O51 O 0.1270(3) 2.2133(3) -0.0320(2) 0.0291(13) Uani 1 1 d D . .
H51 H 0.176(5) 2.227(5) -0.018(3) 0.044 Uiso 1 1 d . . .
N51 N 0.1531(3) 2.1021(3) 0.0307(2) 0.0190(12) Uani 1 1 d D . .
N52 N 0.1024(3) 2.0575(3) 0.0579(2) 0.0194(13) Uani 1 1 d D . .
H52 H 0.1209 2.0171 0.0817 0.023 Uiso 1 1 calc R . .
C51 C 0.0999(4) 2.1558(4) -0.0006(3) 0.0211(16) Uani 1 1 d D . .
C52 C 0.0168(4) 2.1444(4) 0.0049(3) 0.0217(16) Uani 1 1 d D . .
H52' H -0.0326 2.1735 -0.0145 0.026 Uiso 1 1 calc R . .
C53 C 0.0203(4) 2.0828(4) 0.0437(3) 0.0193(15) Uani 1 1 d D . .
C54 C -0.0471(4) 2.0468(4) 0.0701(3) 0.0239(16) Uani 1 1 d D . .
H54A H -0.0473 1.9874 0.0656 0.036 Uiso 1 1 calc R . .
H54B H -0.1031 2.0688 0.0508 0.036 Uiso 1 1 calc R . .
H54C H -0.0351 2.0606 0.1112 0.036 Uiso 1 1 calc R . .
O61 O 0.2890(3) 2.2076(3) 0.01250(18) 0.0193(10) Uani 1 1 d D . .
N61 N 0.3970(3) 2.1845(3) -0.0365(2) 0.0173(12) Uani 1 1 d D . .
N62 N 0.4309(3) 2.2311(3) -0.0746(2) 0.0244(14) Uani 1 1 d D . .
H62 H 0.4725 2.2151 -0.0905 0.029 Uiso 1 1 calc R . .
C61 C 0.3367(4) 2.2311(4) -0.0228(3) 0.0202(15) Uani 1 1 d D . .
C62 C 0.3307(4) 2.3063(4) -0.0517(3) 0.0307(19) Uani 1 1 d D . .
H62' H 0.2924 2.3497 -0.0493 0.037 Uiso 1 1 calc R . .
C63 C 0.3914(5) 2.3045(4) -0.0840(3) 0.0323(19) Uani 1 1 d D . .
C64 C 0.4167(5) 2.3650(5) -0.1235(4) 0.054(3) Uani 1 1 d D . .
H64A H 0.4431 2.3368 -0.1513 0.082 Uiso 1 1 calc R . .
H64B H 0.4578 2.4036 -0.1011 0.082 Uiso 1 1 calc R . .
H64C H 0.3659 2.3947 -0.1442 0.082 Uiso 1 1 calc R . .
O1S O 0.8317(4) 1.9421(4) 0.2973(3) 0.072(2) Uani 1 1 d DU A .
O2S O 0.9613(3) 1.9218(4) 0.3469(3) 0.0482(15) Uani 1 1 d DU A .
C1S C 0.9441(6) 1.9967(6) 0.2609(4) 0.063(3) Uani 1 1 d DU A .
H1S1 H 0.9162 1.9814 0.2213 0.094 Uiso 1 1 calc R . .
H1S2 H 1.0051 1.9835 0.2683 0.094 Uiso 1 1 calc R . .
H1S3 H 0.9371 2.0554 0.2661 0.094 Uiso 1 1 calc R . .
C2S C 0.9054(5) 1.9523(6) 0.3008(4) 0.050(2) Uani 1 1 d DU . .
C3S C 0.9276(6) 1.8777(6) 0.3894(4) 0.058(3) Uani 1 1 d DU . .
H3S1 H 0.9025 1.8252 0.3734 0.070 Uiso 1 1 calc R A .
H3S2 H 0.8827 1.9100 0.4016 0.070 Uiso 1 1 calc R . .
C4S C 1.0009(6) 1.8636(6) 0.4389(4) 0.068(3) Uani 1 1 d U A .
H4S1 H 1.0452 1.8325 0.4260 0.102 Uiso 1 1 calc R . .
H4S2 H 0.9816 1.8328 0.4688 0.102 Uiso 1 1 calc R . .
H4S3 H 1.0244 1.9161 0.4546 0.102 Uiso 1 1 calc R . .
O3S O 0.6975(8) 1.9845(8) 0.3913(5) 0.092(4) Uani 0.65 1 d PDU A 1
O4S O 0.6164(8) 1.9574(8) 0.4545(5) 0.087(3) Uani 0.65 1 d PDU A 1
C5S C 0.593(2) 2.0771(19) 0.4051(17) 0.106(9) Uani 0.65 1 d PDU A 1
H5S1 H 0.5754 2.0930 0.4402 0.159 Uiso 0.65 1 calc PR A 1
H5S2 H 0.5426 2.0672 0.3740 0.159 Uiso 0.65 1 calc PR A 1
H5S3 H 0.6275 2.1209 0.3937 0.159 Uiso 0.65 1 calc PR A 1
C6S C 0.6407(13) 2.0083(14) 0.4151(8) 0.083(4) Uani 0.65 1 d PDU A 1
C7S C 0.6446(11) 1.8613(12) 0.4614(7) 0.087(5) Uani 0.65 1 d PDU A 1
H7S1 H 0.6089 1.8277 0.4306 0.104 Uiso 0.65 1 calc PR A 1
H7S2 H 0.7055 1.8542 0.4607 0.104 Uiso 0.65 1 calc PR A 1
C8S C 0.6316(11) 1.8430(11) 0.5099(9) 0.095(6) Uani 0.65 1 d PDU A 1
H8S1 H 0.6672 1.8774 0.5396 0.142 Uiso 0.65 1 calc PR A 1
H8S2 H 0.6462 1.7856 0.5183 0.142 Uiso 0.65 1 calc PR A 1
H8S3 H 0.5711 1.8518 0.5098 0.142 Uiso 0.65 1 calc PR A 1
O5S O 0.7169(7) 2.0977(6) 0.2713(5) 0.071(3) Uiso 0.65 1 d PDU A 1
O6S O 0.7207(6) 2.2202(6) 0.2311(4) 0.064(3) Uiso 0.65 1 d PDU A 1
C9S C 0.7332(6) 2.1072(6) 0.1754(4) 0.019(2) Uiso 0.65 1 d PDU A 1
C10S C 0.7262(10) 2.1361(10) 0.2261(7) 0.063(4) Uiso 0.65 1 d PDU A 1
C11S C 0.6968(11) 2.2558(10) 0.2871(8) 0.072(5) Uiso 0.65 1 d PDU A 1
C12S C 0.6084(9) 2.2539(9) 0.2732(6) 0.057(4) Uiso 0.65 1 d PDU A 1
O5T O 0.7155(7) 2.0906(7) 0.3347(5) 0.015(3) Uiso 0.35 1 d PU A -2
O6T O 0.6356(14) 2.1363(15) 0.3833(11) 0.078(6) Uiso 0.35 1 d PDU A -2
C9T C 0.6714(19) 2.2310(19) 0.3283(13) 0.068(8) Uiso 0.35 1 d PDU A -2
C10T C 0.6731(16) 2.1451(16) 0.3503(11) 0.045(6) Uiso 0.35 1 d PDU A -2
C11T C 0.620(3) 2.073(3) 0.403(3) 0.048(9) Uiso 0.35 1 d PDU A -2
C12T C 0.579(3) 2.065(2) 0.4648(18) 0.104(12) Uiso 0.35 1 d PDU A -2
O7S O 0.6520(10) 1.8613(10) 0.3351(7) 0.119(5) Uiso 0.65 1 d P A 1
O7T O 0.6488(10) 1.8198(10) 0.3137(7) 0.044(4) Uiso 0.35 1 d PD A -2
O8T O 0.6509(10) 1.6964(9) 0.2956(7) 0.049(4) Uiso 0.35 1 d PD A -2
C13T C 0.5414(9) 1.7758(10) 0.2485(7) 0.013(4) Uiso 0.35 1 d PD A -2
C14T C 0.6125(9) 1.7688(9) 0.2886(7) 0.013(4) Uiso 0.35 1 d PD A -2
C15T C 0.7246(14) 1.6770(16) 0.3414(10) 0.056(7) Uiso 0.35 1 d PD A -2
O1W O 0.6187(10) 1.7578(10) 0.3622(7) 0.129(5) Uiso 0.65 1 d P B 1
O1W' O 0.6736(17) 1.7806(17) 0.4319(12) 0.115(9) Uiso 0.35 1 d P C -2

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 0.0173(4) 0.0188(5) 0.0171(5) 0.0033(4) 0.0054(4) -0.0005(4)
Ni2 0.0161(4) 0.0150(5) 0.0154(4) 0.0011(4) 0.0051(3) 0.0005(3)
Ni3 0.0158(4) 0.0157(5) 0.0162(4) 0.0021(4) 0.0046(3) -0.0004(3)
Ni4 0.0152(4) 0.0139(5) 0.0152(4) 0.0027(3) 0.0044(3) 0.0003(3)
Na1 0.0294(17) 0.055(2) 0.048(2) -0.0061(16) 0.0039(15) -0.0061(15)
N101 0.017(3) 0.016(3) 0.016(3) 0.000(2) 0.004(2) -0.001(2)
N102 0.015(3) 0.021(4) 0.019(3) 0.006(3) 0.006(3) 0.002(3)
N103 0.030(3) 0.023(4) 0.026(4) 0.000(3) 0.002(3) -0.004(3)
N104 0.015(3) 0.031(4) 0.012(3) 0.004(2) 0.003(2) -0.003(2)
N105 0.025(3) 0.039(4) 0.030(4) -0.003(3) 0.011(3) 0.002(3)
N106 0.024(4) 0.121(8) 0.031(4) -0.033(4) 0.001(3) -0.002(4)
N107 0.018(3) 0.017(3) 0.015(3) -0.003(2) 0.007(2) -0.002(2)
N108 0.022(3) 0.022(4) 0.026(4) 0.000(3) 0.006(3) -0.003(3)
N109 0.039(4) 0.041(5) 0.041(4) -0.011(3) 0.009(3) -0.009(3)
N110 0.015(3) 0.019(3) 0.015(3) 0.003(2) 0.004(2) 0.001(2)
N111 0.019(3) 0.023(4) 0.025(3) 0.000(3) 0.012(3) -0.002(3)
N112 0.023(3) 0.055(5) 0.017(3) 0.005(3) 0.001(3) 0.004(3)
N113 0.015(3) 0.018(3) 0.019(3) 0.000(2) 0.003(2) -0.003(2)
N114 0.019(3) 0.018(4) 0.022(3) 0.007(3) 0.008(3) 0.004(3)
N115 0.037(4) 0.028(4) 0.027(4) -0.007(3) 0.002(3) -0.015(3)
N116 0.016(3) 0.023(3) 0.011(3) 0.001(2) 0.004(2) 0.002(2)
N117 0.025(3) 0.025(4) 0.022(3) -0.001(3) 0.007(3) 0.000(3)
N118 0.039(4) 0.055(5) 0.023(4) 0.008(3) 0.005(3) 0.006(3)
O11 0.021(2) 0.019(3) 0.025(3) 0.005(2) 0.012(2) 0.005(2)
O12 0.020(2) 0.024(3) 0.022(3) 0.010(2) 0.010(2) 0.002(2)
C11 0.015(3) 0.023(4) 0.022(4) 0.011(3) 0.004(3) 0.005(3)
C12 0.024(4) 0.024(4) 0.032(4) 0.005(3) 0.015(3) 0.002(3)
C13 0.055(5) 0.029(5) 0.052(6) 0.004(4) 0.034(5) 0.001(4)
C14 0.083(7) 0.015(5) 0.064(6) 0.008(4) 0.040(6) -0.005(4)
C15 0.074(7) 0.017(5) 0.083(7) -0.003(5) 0.042(6) -0.002(4)
C16 0.061(6) 0.028(5) 0.057(6) -0.002(4) 0.030(5) -0.002(4)
C17 0.039(5) 0.030(5) 0.039(5) 0.004(4) 0.019(4) -0.005(4)
O21 0.056(4) 0.035(4) 0.019(3) -0.003(2) -0.001(3) -0.007(3)
N21 0.026(3) 0.024(4) 0.021(3) 0.006(3) 0.008(3) -0.002(3)
N22 0.032(3) 0.026(4) 0.023(3) 0.012(3) 0.004(3) 0.002(3)
C21 0.033(4) 0.034(5) 0.025(4) 0.003(4) 0.009(3) -0.008(4)
C22 0.049(5) 0.048(6) 0.018(4) 0.005(4) 0.000(4) -0.015(4)
C23 0.028(4) 0.048(6) 0.031(5) 0.016(4) 0.003(4) -0.006(4)
C24 0.051(6) 0.062(7) 0.030(5) 0.025(4) -0.006(4) -0.011(5)
O31 0.022(3) 0.029(3) 0.036(3) -0.005(2) 0.011(3) -0.002(2)
N31 0.020(3) 0.020(3) 0.020(3) 0.001(2) 0.008(2) 0.000(2)
N32 0.019(3) 0.021(4) 0.026(3) 0.003(3) 0.009(3) 0.000(2)
C31 0.026(4) 0.026(5) 0.013(3) 0.000(3) 0.004(3) -0.001(3)
C32 0.015(3) 0.038(5) 0.022(4) 0.003(3) 0.007(3) -0.001(3)
C33 0.023(4) 0.030(5) 0.018(4) 0.009(3) 0.003(3) -0.005(3)
C34 0.030(4) 0.028(5) 0.036(5) 0.001(4) 0.003(4) -0.004(3)
O41 0.023(2) 0.016(3) 0.022(3) 0.002(2) 0.009(2) -0.004(2)
N41 0.022(3) 0.015(3) 0.020(3) -0.002(2) 0.008(2) -0.001(2)
N42 0.027(3) 0.017(3) 0.021(3) 0.005(2) 0.010(3) -0.003(3)
C41 0.013(3) 0.020(4) 0.022(4) -0.003(3) 0.007(3) 0.000(3)
C42 0.024(4) 0.024(4) 0.020(4) -0.009(3) 0.012(3) -0.003(3)
C43 0.024(4) 0.024(4) 0.019(4) -0.008(3) 0.006(3) -0.003(3)
C44 0.038(4) 0.018(4) 0.031(4) -0.007(3) 0.011(4) -0.005(3)
O51 0.019(3) 0.033(3) 0.034(3) 0.016(2) 0.003(2) 0.000(2)
N51 0.019(3) 0.020(3) 0.018(3) -0.001(2) 0.007(2) -0.001(2)
N52 0.020(3) 0.022(3) 0.019(3) 0.004(2) 0.011(2) 0.000(2)
C51 0.023(4) 0.017(4) 0.024(4) 0.000(3) 0.007(3) 0.001(3)
C52 0.016(3) 0.022(4) 0.026(4) 0.001(3) 0.004(3) 0.004(3)
C53 0.017(3) 0.022(4) 0.019(4) -0.003(3) 0.004(3) -0.003(3)
C54 0.020(4) 0.030(4) 0.022(4) -0.002(3) 0.005(3) -0.001(3)
O61 0.021(2) 0.019(3) 0.020(3) 0.001(2) 0.008(2) 0.0003(19)
N61 0.020(3) 0.017(3) 0.016(3) 0.003(2) 0.005(2) -0.002(2)
N62 0.027(3) 0.020(4) 0.030(3) 0.008(3) 0.015(3) 0.004(3)
C61 0.018(3) 0.016(4) 0.027(4) -0.004(3) 0.006(3) 0.000(3)
C62 0.027(4) 0.018(4) 0.051(5) 0.015(4) 0.019(4) 0.007(3)
C63 0.036(4) 0.019(4) 0.045(5) 0.015(4) 0.015(4) 0.006(3)
C64 0.050(6) 0.040(6) 0.090(8) 0.040(5) 0.049(5) 0.022(4)
O1S 0.033(3) 0.088(6) 0.089(5) -0.020(4) 0.002(3) 0.006(3)
O2S 0.036(3) 0.050(4) 0.060(4) 0.001(3) 0.015(3) 0.005(3)
C1S 0.060(6) 0.088(8) 0.041(6) -0.003(5) 0.013(5) 0.024(5)
C2S 0.034(4) 0.057(6) 0.054(5) -0.021(4) 0.002(4) 0.008(4)
C3S 0.051(5) 0.043(6) 0.088(7) 0.007(5) 0.033(5) -0.001(5)
C4S 0.072(7) 0.062(7) 0.077(7) 0.025(6) 0.032(5) 0.006(6)
O3S 0.091(9) 0.123(10) 0.063(8) 0.014(7) 0.019(6) 0.002(7)
O4S 0.084(8) 0.097(8) 0.081(8) 0.029(6) 0.022(6) 0.013(6)
C5S 0.14(3) 0.074(13) 0.098(18) 0.009(11) 0.02(2) 0.008(14)
C6S 0.091(11) 0.103(10) 0.057(9) 0.010(8) 0.020(7) 0.015(9)
C7S 0.078(10) 0.120(10) 0.062(10) 0.015(9) 0.013(8) 0.061(9)
C8S 0.064(11) 0.095(13) 0.126(14) 0.057(12) 0.023(11) 0.006(10)

_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 N104 2.037(5) . ?
Ni1 N31 2.061(5) . ?
Ni1 O41 2.062(5) . ?
Ni1 N21 2.067(6) . ?
Ni1 O11 2.102(5) . ?
Ni1 N101 2.197(5) . ?
Ni2 N51 2.057(5) . ?
Ni2 N41 2.058(5) . ?
Ni2 O61 2.082(4) . ?
Ni2 N110 2.086(5) . ?
Ni2 N107 2.127(5) . ?
Ni2 N101 2.149(5) . ?
Ni3 N104 2.039(5) . ?
Ni3 O12 2.057(5) . ?
Ni3 N107 2.069(5) . ?
Ni3 N116 2.074(5) . ?
Ni3 N113 2.131(5) . ?
Ni3 N101 2.214(5) . ?
Ni4 N61 2.047(5) . ?
Ni4 N110 2.078(5) . ?
Ni4 N116 2.089(5) 3_695 ?
Ni4 N107 2.113(5) . ?
Ni4 N113 2.135(5) 3_695 ?
Ni4 N113 2.170(5) . ?
Na1 O7S 2.203(16) . ?
Na1 O5S 2.255(11) . ?
Na1 O1S 2.255(7) . ?
Na1 O5T 2.294(12) . ?
Na1 O3S 2.418(12) . ?
Na1 N106 2.494(8) . ?
Na1 N118 2.499(7) . ?
Na1 O7T 2.599(17) . ?
N101 N102 1.232(7) . ?
N102 N103 1.137(8) . ?
N104 N105 1.202(8) . ?
N105 N106 1.147(8) . ?
N107 N108 1.229(8) . ?
N108 N109 1.139(8) . ?
N110 N111 1.223(7) . ?
N111 N112 1.137(7) . ?
N113 N114 1.238(7) . ?
N113 Ni4 2.135(5) 3_695 ?
N114 N115 1.133(7) . ?
N116 N117 1.190(7) . ?
N116 Ni4 2.089(5) 3_695 ?
N117 N118 1.157(8) . ?
O11 C11 1.255(7) . ?
O12 C11 1.240(7) . ?
C11 C12 1.520(10) . ?
C12 C17 1.376(10) . ?
C12 C13 1.402(10) . ?
C13 C14 1.384(11) . ?
C14 C15 1.400(12) . ?
C15 C16 1.368(11) . ?
C16 C17 1.388(10) . ?
O21 C21 1.324(9) . ?
N21 C21 1.325(9) . ?
N21 N22 1.369(8) . ?
N22 C23 1.351(9) . ?
C21 C22 1.424(10) . ?
C22 C23 1.358(11) . ?
C23 C24 1.505(11) . ?
O31 C31 1.342(8) . ?
N31 C31 1.327(8) . ?
N31 N32 1.367(7) . ?
N32 C33 1.327(8) . ?
C31 C32 1.388(9) . ?
C32 C33 1.358(10) . ?
C33 C34 1.501(10) . ?
O41 C41 1.320(8) . ?
N41 C41 1.354(8) . ?
N41 N42 1.364(7) . ?
N42 C43 1.346(8) . ?
C41 C42 1.413(9) . ?
C42 C43 1.379(9) . ?
C43 C44 1.491(9) . ?
O51 C51 1.337(8) . ?
N51 C51 1.331(8) . ?
N51 N52 1.362(7) . ?
N52 C53 1.349(8) . ?
C51 C52 1.382(9) . ?
C52 C53 1.363(9) . ?
C53 C54 1.491(9) . ?
O61 C61 1.317(7) . ?
N61 C61 1.332(8) . ?
N61 N62 1.388(7) . ?
N62 C63 1.356(9) . ?
C61 C62 1.406(9) . ?
C62 C63 1.373(10) . ?
C63 C64 1.488(10) . ?
O1S C2S 1.180(9) . ?
O2S C2S 1.346(10) . ?
O2S C3S 1.446(10) . ?
C1S C2S 1.445(12) . ?
C3S C4S 1.483(13) . ?
O3S C6S 1.24(2) . ?
O4S C6S 1.38(2) . ?
O4S C7S 1.64(2) . ?
C5S C6S 1.35(3) . ?
C7S C8S 1.26(2) . ?
O5S C10S 1.284(17) . ?
O6S C10S 1.390(17) . ?
O6S C11S 1.582(19) . ?
C9S C10S 1.326(18) . ?
C11S C12S 1.38(2) . ?
O5T C10T 1.23(3) . ?
O6T C10T 1.10(3) . ?
O6T C11T 1.20(6) . ?
C9T C10T 1.50(4) . ?
C11T C12T 1.75(7) . ?
O7T C14T 1.113(15) . ?
O8T C14T 1.331(16) . ?
O8T C15T 1.450(18) . ?
C13T C14T 1.315(16) . ?

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
N104 Ni1 N31 172.1(2) . . ?
N104 Ni1 O41 94.5(2) . . ?
N31 Ni1 O41 88.6(2) . . ?
N104 Ni1 N21 93.6(2) . . ?
N31 Ni1 N21 93.79(19) . . ?
O41 Ni1 N21 87.8(2) . . ?
N104 Ni1 O11 93.6(2) . . ?
N31 Ni1 O11 83.92(19) . . ?
O41 Ni1 O11 170.65(17) . . ?
N21 Ni1 O11 87.0(2) . . ?
N104 Ni1 N101 80.2(2) . . ?
N31 Ni1 N101 92.29(19) . . ?
O41 Ni1 N101 96.48(18) . . ?
N21 Ni1 N101 172.7(2) . . ?
O11 Ni1 N101 89.49(18) . . ?
N51 Ni2 N41 90.68(19) . . ?
N51 Ni2 O61 88.75(19) . . ?
N41 Ni2 O61 87.24(19) . . ?
N51 Ni2 N110 95.67(19) . . ?
N41 Ni2 N110 172.8(2) . . ?
O61 Ni2 N110 89.44(19) . . ?
N51 Ni2 N107 178.2(2) . . ?
N41 Ni2 N107 91.13(19) . . ?
O61 Ni2 N107 91.70(19) . . ?
N110 Ni2 N107 82.5(2) . . ?
N51 Ni2 N101 97.6(2) . . ?
N41 Ni2 N101 93.5(2) . . ?
O61 Ni2 N101 173.57(18) . . ?
N110 Ni2 N101 89.1(2) . . ?
N107 Ni2 N101 81.9(2) . . ?
N104 Ni3 O12 94.7(2) . . ?
N104 Ni3 N107 95.1(2) . . ?
O12 Ni3 N107 165.45(19) . . ?
N104 Ni3 N116 97.4(2) . . ?
O12 Ni3 N116 95.29(19) . . ?
N107 Ni3 N116 94.0(2) . . ?
N104 Ni3 N113 175.9(2) . . ?
O12 Ni3 N113 88.03(19) . . ?
N107 Ni3 N113 82.7(2) . . ?
N116 Ni3 N113 79.32(19) . . ?
N104 Ni3 N101 79.7(2) . . ?
O12 Ni3 N101 89.62(18) . . ?
N107 Ni3 N101 81.65(19) . . ?
N116 Ni3 N101 174.5(2) . . ?
N113 Ni3 N101 103.40(19) . . ?
N61 Ni4 N110 91.4(2) . . ?
N61 Ni4 N116 94.7(2) . 3_695 ?
N110 Ni4 N116 101.8(2) . 3_695 ?
N61 Ni4 N107 89.5(2) . . ?
N110 Ni4 N107 83.1(2) . . ?
N116 Ni4 N107 173.5(2) 3_695 . ?
N61 Ni4 N113 100.1(2) . 3_695 ?
N110 Ni4 N113 168.4(2) . 3_695 ?
N116 Ni4 N113 78.9(2) 3_695 3_695 ?
N107 Ni4 N113 95.5(2) . 3_695 ?
N61 Ni4 N113 170.3(2) . . ?
N110 Ni4 N113 87.0(2) . . ?
N116 Ni4 N113 95.0(2) 3_695 . ?
N107 Ni4 N113 80.8(2) . . ?
N113 Ni4 N113 81.4(2) 3_695 . ?
O7S Na1 O5S 158.3(5) . . ?
O7S Na1 O1S 102.4(5) . . ?
O5S Na1 O1S 87.7(3) . . ?
O7S Na1 O5T 120.2(5) . . ?
O5S Na1 O5T 39.1(4) . . ?
O1S Na1 O5T 93.4(4) . . ?
O7S Na1 O3S 63.6(5) . . ?
O5S Na1 O3S 96.3(4) . . ?
O1S Na1 O3S 97.4(4) . . ?
O5T Na1 O3S 57.2(4) . . ?
O7S Na1 N106 93.1(5) . . ?
O5S Na1 N106 79.4(4) . . ?
O1S Na1 N106 163.7(3) . . ?
O5T Na1 N106 82.8(4) . . ?
O3S Na1 N106 93.9(4) . . ?
O7S Na1 N118 97.6(5) . . ?
O5S Na1 N118 101.2(3) . . ?
O1S Na1 N118 92.3(3) . . ?
O5T Na1 N118 139.4(4) . . ?
O3S Na1 N118 160.3(4) . . ?
N106 Na1 N118 80.7(2) . . ?
O7S Na1 O7T 18.0(5) . . ?
O5S Na1 O7T 174.7(5) . . ?
O1S Na1 O7T 97.3(4) . . ?
O5T Na1 O7T 138.1(5) . . ?
O3S Na1 O7T 81.2(5) . . ?
N106 Na1 O7T 96.0(4) . . ?
N118 Na1 O7T 80.6(4) . . ?
N102 N101 Ni2 116.3(4) . . ?
N102 N101 Ni1 111.7(4) . . ?
Ni2 N101 Ni1 124.1(2) . . ?
N102 N101 Ni3 113.5(4) . . ?
Ni2 N101 Ni3 95.4(2) . . ?
Ni1 N101 Ni3 90.42(19) . . ?
N103 N102 N101 178.9(7) . . ?
N105 N104 Ni1 125.9(5) . . ?
N105 N104 Ni3 131.7(5) . . ?
Ni1 N104 Ni3 100.3(2) . . ?
N106 N105 N104 179.1(8) . . ?
N105 N106 Na1 131.0(6) . . ?
N108 N107 Ni3 115.3(4) . . ?
N108 N107 Ni4 124.8(4) . . ?
Ni3 N107 Ni4 100.0(2) . . ?
N108 N107 Ni2 118.0(4) . . ?
Ni3 N107 Ni2 100.5(2) . . ?
Ni4 N107 Ni2 93.6(2) . . ?
N109 N108 N107 178.5(7) . . ?
N111 N110 Ni4 121.2(4) . . ?
N111 N110 Ni2 121.5(4) . . ?
Ni4 N110 Ni2 95.8(2) . . ?
N112 N111 N110 177.6(7) . . ?
N114 N113 Ni3 118.7(4) . . ?
N114 N113 Ni4 119.0(4) . 3_695 ?
Ni3 N113 Ni4 99.2(2) . 3_695 ?
N114 N113 Ni4 120.2(4) . . ?
Ni3 N113 Ni4 96.3(2) . . ?
Ni4 N113 Ni4 98.6(2) 3_695 . ?
N115 N114 N113 178.5(8) . . ?
N117 N116 Ni3 119.7(4) . . ?
N117 N116 Ni4 124.9(4) . 3_695 ?
Ni3 N116 Ni4 102.6(2) . 3_695 ?
N118 N117 N116 178.5(7) . . ?
N117 N118 Na1 130.6(6) . . ?
C11 O11 Ni1 127.8(4) . . ?
C11 O12 Ni3 129.2(4) . . ?
O12 C11 O11 126.2(6) . . ?
O12 C11 C12 117.7(6) . . ?
O11 C11 C12 116.1(6) . . ?
C17 C12 C13 118.5(7) . . ?
C17 C12 C11 120.6(6) . . ?
C13 C12 C11 120.9(7) . . ?
C14 C13 C12 120.9(8) . . ?
C13 C14 C15 119.7(8) . . ?
C16 C15 C14 118.8(8) . . ?
C15 C16 C17 121.6(8) . . ?
C12 C17 C16 120.3(7) . . ?
C21 N21 N22 105.7(6) . . ?
C21 N21 Ni1 131.9(5) . . ?
N22 N21 Ni1 122.2(4) . . ?
C23 N22 N21 111.1(6) . . ?
O21 C21 N21 122.9(7) . . ?
O21 C21 C22 126.9(7) . . ?
N21 C21 C22 110.2(7) . . ?
C23 C22 C21 105.5(7) . . ?
N22 C23 C22 107.6(7) . . ?
N22 C23 C24 120.2(8) . . ?
C22 C23 C24 132.2(8) . . ?
C31 N31 N32 103.8(5) . . ?
C31 N31 Ni1 134.6(5) . . ?
N32 N31 Ni1 121.6(4) . . ?
C33 N32 N31 112.3(5) . . ?
N31 C31 O31 120.9(6) . . ?
N31 C31 C32 111.3(6) . . ?
O31 C31 C32 127.8(6) . . ?
C33 C32 C31 105.7(6) . . ?
N32 C33 C32 106.9(6) . . ?
N32 C33 C34 120.5(6) . . ?
C32 C33 C34 132.6(6) . . ?
C41 O41 Ni1 128.7(4) . . ?
C41 N41 N42 104.4(5) . . ?
C41 N41 Ni2 141.4(5) . . ?
N42 N41 Ni2 114.1(4) . . ?
C43 N42 N41 113.6(5) . . ?
O41 C41 N41 123.4(6) . . ?
O41 C41 C42 126.9(6) . . ?
N41 C41 C42 109.7(6) . . ?
C43 C42 C41 106.8(6) . . ?
N42 C43 C42 105.5(6) . . ?
N42 C43 C44 121.5(6) . . ?
C42 C43 C44 133.0(6) . . ?
C51 N51 N52 104.2(5) . . ?
C51 N51 Ni2 131.5(5) . . ?
N52 N51 Ni2 123.6(4) . . ?
C53 N52 N51 111.8(5) . . ?
N51 C51 O51 122.1(6) . . ?
N51 C51 C52 111.5(6) . . ?
O51 C51 C52 126.3(6) . . ?
C53 C52 C51 105.9(6) . . ?
N52 C53 C52 106.5(6) . . ?
N52 C53 C54 122.3(6) . . ?
C52 C53 C54 131.2(6) . . ?
C61 O61 Ni2 127.9(4) . . ?
C61 N61 N62 105.1(5) . . ?
C61 N61 Ni4 129.2(4) . . ?
N62 N61 Ni4 124.5(4) . . ?
C63 N62 N61 111.0(5) . . ?
O61 C61 N61 123.4(6) . . ?
O61 C61 C62 125.8(6) . . ?
N61 C61 C62 110.8(6) . . ?
C63 C62 C61 106.1(6) . . ?
N62 C63 C62 107.0(6) . . ?
N62 C63 C64 120.9(6) . . ?
C62 C63 C64 132.2(7) . . ?
C2S O1S Na1 161.7(7) . . ?
C2S O2S C3S 118.1(7) . . ?
O1S C2S O2S 118.4(9) . . ?
O1S C2S C1S 126.8(9) . . ?
O2S C2S C1S 114.7(7) . . ?
O2S C3S C4S 106.2(7) . . ?
C6S O3S Na1 128.9(12) . . ?
C6S O4S C7S 122.6(14) . . ?
O3S C6S C5S 129(3) . . ?
O3S C6S O4S 118.1(19) . . ?
C5S C6S O4S 113(2) . . ?
C8S C7S O4S 102.9(15) . . ?
C10S O5S Na1 133.9(11) . . ?
C10S O6S C11S 118.0(11) . . ?
O5S C10S C9S 129.6(15) . . ?
O5S C10S O6S 113.3(14) . . ?
C9S C10S O6S 116.9(13) . . ?
C12S C11S O6S 102.8(13) . . ?
C10T O5T Na1 137.7(14) . . ?
C10T O6T C11T 126(3) . . ?
O6T C10T O5T 123(3) . . ?
O6T C10T C9T 114(3) . . ?
O5T C10T C9T 123(2) . . ?
O6T C11T C12T 123(4) . . ?
C14T O7T Na1 135.2(15) . . ?
C14T O8T C15T 124.5(16) . . ?
O7T C14T C13T 125.8(17) . . ?
O7T C14T O8T 115.6(16) . . ?
C13T C14T O8T 118.0(15) . . ?

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
N51 Ni2 N101 N102 53.2(5) . . . . ?
N41 Ni2 N101 N102 144.4(4) . . . . ?
O61 Ni2 N101 N102 -119.0(16) . . . . ?
N110 Ni2 N101 N102 -42.4(4) . . . . ?
N107 Ni2 N101 N102 -125.0(5) . . . . ?
N51 Ni2 N101 Ni1 -93.1(3) . . . . ?
N41 Ni2 N101 Ni1 -1.9(3) . . . . ?
O61 Ni2 N101 Ni1 94.7(16) . . . . ?
N110 Ni2 N101 Ni1 171.3(3) . . . . ?
N107 Ni2 N101 Ni1 88.7(3) . . . . ?
N51 Ni2 N101 Ni3 172.75(19) . . . . ?
N41 Ni2 N101 Ni3 -96.1(2) . . . . ?
O61 Ni2 N101 Ni3 0.6(17) . . . . ?
N110 Ni2 N101 Ni3 77.2(2) . . . . ?
N107 Ni2 N101 Ni3 -5.44(19) . . . . ?
N104 Ni1 N101 N102 137.5(5) . . . . ?
N31 Ni1 N101 N102 -40.2(4) . . . . ?
O41 Ni1 N101 N102 -129.1(4) . . . . ?
N21 Ni1 N101 N102 105.5(17) . . . . ?
O11 Ni1 N101 N102 43.7(4) . . . . ?
N104 Ni1 N101 Ni2 -74.9(3) . . . . ?
N31 Ni1 N101 Ni2 107.4(3) . . . . ?
O41 Ni1 N101 Ni2 18.5(3) . . . . ?
N21 Ni1 N101 Ni2 -106.8(17) . . . . ?
O11 Ni1 N101 Ni2 -168.7(3) . . . . ?
N104 Ni1 N101 Ni3 21.9(2) . . . . ?
N31 Ni1 N101 Ni3 -155.8(2) . . . . ?
O41 Ni1 N101 Ni3 115.29(18) . . . . ?
N21 Ni1 N101 Ni3 -10.1(18) . . . . ?
O11 Ni1 N101 Ni3 -71.91(18) . . . . ?
N104 Ni3 N101 N102 -135.8(5) . . . . ?
O12 Ni3 N101 N102 -41.0(4) . . . . ?
N107 Ni3 N101 N102 127.4(5) . . . . ?
N116 Ni3 N101 N102 166.0(19) . . . . ?
N113 Ni3 N101 N102 46.9(5) . . . . ?
N104 Ni3 N101 Ni2 102.4(2) . . . . ?
O12 Ni3 N101 Ni2 -162.72(19) . . . . ?
N107 Ni3 N101 Ni2 5.6(2) . . . . ?
N116 Ni3 N101 Ni2 44(2) . . . . ?
N113 Ni3 N101 Ni2 -74.8(2) . . . . ?
N104 Ni3 N101 Ni1 -21.9(2) . . . . ?
O12 Ni3 N101 Ni1 73.01(19) . . . . ?
N107 Ni3 N101 Ni1 -118.7(2) . . . . ?
N116 Ni3 N101 Ni1 -80(2) . . . . ?
N113 Ni3 N101 Ni1 160.89(19) . . . . ?
Ni2 N101 N102 N103 -142(37) . . . . ?
Ni1 N101 N102 N103 8(37) . . . . ?
Ni3 N101 N102 N103 109(37) . . . . ?
N31 Ni1 N104 N105 -172.2(14) . . . . ?
O41 Ni1 N104 N105 74.8(6) . . . . ?
N21 Ni1 N104 N105 -13.3(6) . . . . ?
O11 Ni1 N104 N105 -100.6(6) . . . . ?
N101 Ni1 N104 N105 170.6(6) . . . . ?
N31 Ni1 N104 Ni3 -7.1(17) . . . . ?
O41 Ni1 N104 Ni3 -120.1(2) . . . . ?
N21 Ni1 N104 Ni3 151.8(2) . . . . ?
O11 Ni1 N104 Ni3 64.6(2) . . . . ?
N101 Ni1 N104 Ni3 -24.3(2) . . . . ?
O12 Ni3 N104 N105 99.2(7) . . . . ?
N107 Ni3 N104 N105 -91.5(7) . . . . ?
N116 Ni3 N104 N105 3.2(7) . . . . ?
N113 Ni3 N104 N105 -33(3) . . . . ?
N101 Ni3 N104 N105 -172.0(7) . . . . ?
O12 Ni3 N104 Ni1 -64.7(2) . . . . ?
N107 Ni3 N104 Ni1 104.6(2) . . . . ?
N116 Ni3 N104 Ni1 -160.6(2) . . . . ?
N113 Ni3 N104 Ni1 163(3) . . . . ?
N101 Ni3 N104 Ni1 24.1(2) . . . . ?
Ni1 N104 N105 N106 19(59) . . . . ?
Ni3 N104 N105 N106 -142(59) . . . . ?
N104 N105 N106 Na1 107(59) . . . . ?
O7S Na1 N106 N105 -87.5(10) . . . . ?
O5S Na1 N106 N105 113.1(9) . . . . ?
O1S Na1 N106 N105 75.1(15) . . . . ?
O5T Na1 N106 N105 152.5(9) . . . . ?
O3S Na1 N106 N105 -151.2(9) . . . . ?
N118 Na1 N106 N105 9.8(9) . . . . ?
O7T Na1 N106 N105 -69.7(10) . . . . ?
N104 Ni3 N107 N108 43.5(5) . . . . ?
O12 Ni3 N107 N108 176.0(6) . . . . ?
N116 Ni3 N107 N108 -54.3(5) . . . . ?
N113 Ni3 N107 N108 -132.9(5) . . . . ?
N101 Ni3 N107 N108 122.3(5) . . . . ?
N104 Ni3 N107 Ni4 179.9(2) . . . . ?
O12 Ni3 N107 Ni4 -47.6(8) . . . . ?
N116 Ni3 N107 Ni4 82.1(2) . . . . ?
N113 Ni3 N107 Ni4 3.5(2) . . . . ?
N101 Ni3 N107 Ni4 -101.3(2) . . . . ?
N104 Ni3 N107 Ni2 -84.5(2) . . . . ?
O12 Ni3 N107 Ni2 48.0(8) . . . . ?
N116 Ni3 N107 Ni2 177.7(2) . . . . ?
N113 Ni3 N107 Ni2 99.0(2) . . . . ?
N101 Ni3 N107 Ni2 -5.7(2) . . . . ?
N61 Ni4 N107 N108 -53.3(6) . . . . ?
N110 Ni4 N107 N108 -144.7(6) . . . . ?
N116 Ni4 N107 N108 77(2) 3_695 . . . ?
N113 Ni4 N107 N108 46.9(6) 3_695 . . . ?
N113 Ni4 N107 N108 127.2(6) . . . . ?
N61 Ni4 N107 Ni3 176.2(2) . . . . ?
N110 Ni4 N107 Ni3 84.7(2) . . . . ?
N116 Ni4 N107 Ni3 -53.5(19) 3_695 . . . ?
N113 Ni4 N107 Ni3 -83.7(2) 3_695 . . . ?
N113 Ni4 N107 Ni3 -3.4(2) . . . . ?
N61 Ni4 N107 Ni2 74.8(2) . . . . ?
N110 Ni4 N107 Ni2 -16.7(2) . . . . ?
N116 Ni4 N107 Ni2 -154.9(18) 3_695 . . . ?
N113 Ni4 N107 Ni2 174.9(2) 3_695 . . . ?
N113 Ni4 N107 Ni2 -104.8(2) . . . . ?
N51 Ni2 N107 N108 164(7) . . . . ?
N41 Ni2 N107 N108 -26.9(5) . . . . ?
O61 Ni2 N107 N108 60.4(5) . . . . ?
N110 Ni2 N107 N108 149.6(5) . . . . ?
N101 Ni2 N107 N108 -120.3(5) . . . . ?
N51 Ni2 N107 Ni3 -70(7) . . . . ?
N41 Ni2 N107 Ni3 99.3(2) . . . . ?
O61 Ni2 N107 Ni3 -173.4(2) . . . . ?
N110 Ni2 N107 Ni3 -84.2(2) . . . . ?
N101 Ni2 N107 Ni3 5.9(2) . . . . ?
N51 Ni2 N107 Ni4 31(7) . . . . ?
N41 Ni2 N107 Ni4 -159.9(2) . . . . ?
O61 Ni2 N107 Ni4 -72.6(2) . . . . ?
N110 Ni2 N107 Ni4 16.6(2) . . . . ?
N101 Ni2 N107 Ni4 106.7(2) . . . . ?
Ni3 N107 N108 N109 -79(33) . . . . ?
Ni4 N107 N108 N109 156(33) . . . . ?
Ni2 N107 N108 N109 39(33) . . . . ?
N61 Ni4 N110 N111 60.2(5) . . . . ?
N116 Ni4 N110 N111 -34.9(5) 3_695 . . . ?
N107 Ni4 N110 N111 149.6(5) . . . . ?
N113 Ni4 N110 N111 -126.9(10) 3_695 . . . ?
N113 Ni4 N110 N111 -129.4(5) . . . . ?
N61 Ni4 N110 Ni2 -72.3(2) . . . . ?
N116 Ni4 N110 Ni2 -167.4(2) 3_695 . . . ?
N107 Ni4 N110 Ni2 17.1(2) . . . . ?
N113 Ni4 N110 Ni2 100.6(10) 3_695 . . . ?
N113 Ni4 N110 Ni2 98.2(2) . . . . ?
N51 Ni2 N110 N111 31.2(5) . . . . ?
N41 Ni2 N110 N111 -120.2(16) . . . . ?
O61 Ni2 N110 N111 -57.5(5) . . . . ?
N107 Ni2 N110 N111 -149.3(5) . . . . ?
N101 Ni2 N110 N111 128.7(5) . . . . ?
N51 Ni2 N110 Ni4 163.5(2) . . . . ?
N41 Ni2 N110 Ni4 12.1(18) . . . . ?
O61 Ni2 N110 Ni4 74.8(2) . . . . ?
N107 Ni2 N110 Ni4 -17.0(2) . . . . ?
N101 Ni2 N110 Ni4 -98.9(2) . . . . ?
Ni4 N110 N111 N112 163(17) . . . . ?
Ni2 N110 N111 N112 -76(17) . . . . ?
N104 Ni3 N113 N114 168(3) . . . . ?
O12 Ni3 N113 N114 35.7(5) . . . . ?
N107 Ni3 N113 N114 -133.0(5) . . . . ?
N116 Ni3 N113 N114 131.5(5) . . . . ?
N101 Ni3 N113 N114 -53.4(5) . . . . ?
N104 Ni3 N113 Ni4 38(3) . . . 3_695 ?
O12 Ni3 N113 Ni4 -94.8(2) . . . 3_695 ?
N107 Ni3 N113 Ni4 96.5(2) . . . 3_695 ?
N116 Ni3 N113 Ni4 1.0(2) . . . 3_695 ?
N101 Ni3 N113 Ni4 176.1(2) . . . 3_695 ?
N104 Ni3 N113 Ni4 -62(3) . . . . ?
O12 Ni3 N113 Ni4 165.39(19) . . . . ?
N107 Ni3 N113 Ni4 -3.34(19) . . . . ?
N116 Ni3 N113 Ni4 -98.9(2) . . . . ?
N101 Ni3 N113 Ni4 76.3(2) . . . . ?
N61 Ni4 N113 N114 129.3(11) . . . . ?
N110 Ni4 N113 N114 48.4(5) . . . . ?
N116 Ni4 N113 N114 -53.1(5) 3_695 . . . ?
N107 Ni4 N113 N114 131.9(5) . . . . ?
N113 Ni4 N113 N114 -131.1(6) 3_695 . . . ?
N61 Ni4 N113 Ni3 0.7(13) . . . . ?
N110 Ni4 N113 Ni3 -80.2(2) . . . . ?
N116 Ni4 N113 Ni3 178.3(2) 3_695 . . . ?
N107 Ni4 N113 Ni3 3.28(19) . . . . ?
N113 Ni4 N113 Ni3 100.3(2) 3_695 . . . ?
N61 Ni4 N113 Ni4 -99.6(11) . . . 3_695 ?
N110 Ni4 N113 Ni4 179.5(2) . . . 3_695 ?
N116 Ni4 N113 Ni4 77.9(2) 3_695 . . 3_695 ?
N107 Ni4 N113 Ni4 -97.0(2) . . . 3_695 ?
N113 Ni4 N113 Ni4 0.0 3_695 . . 3_695 ?
Ni3 N113 N114 N115 -79(27) . . . . ?
Ni4 N113 N114 N115 42(27) 3_695 . . . ?
Ni4 N113 N114 N115 164(27) . . . . ?
N104 Ni3 N116 N117 38.1(5) . . . . ?
O12 Ni3 N116 N117 -57.4(5) . . . . ?
N107 Ni3 N116 N117 133.8(5) . . . . ?
N113 Ni3 N116 N117 -144.3(5) . . . . ?
N101 Ni3 N116 N117 96(2) . . . . ?
N104 Ni3 N116 Ni4 -178.6(2) . . . 3_695 ?
O12 Ni3 N116 Ni4 86.0(2) . . . 3_695 ?
N107 Ni3 N116 Ni4 -82.9(2) . . . 3_695 ?
N113 Ni3 N116 Ni4 -1.0(2) . . . 3_695 ?
N101 Ni3 N116 Ni4 -121(2) . . . 3_695 ?
Ni3 N116 N117 N118 13(30) . . . . ?
Ni4 N116 N117 N118 -122(30) 3_695 . . . ?
N116 N117 N118 Na1 -88(30) . . . . ?
O7S Na1 N118 N117 127.7(8) . . . . ?
O5S Na1 N118 N117 -41.3(8) . . . . ?
O1S Na1 N118 N117 -129.4(7) . . . . ?
O5T Na1 N118 N117 -31.5(10) . . . . ?
O3S Na1 N118 N117 111.1(12) . . . . ?
N106 Na1 N118 N117 35.8(7) . . . . ?
O7T Na1 N118 N117 133.6(8) . . . . ?
N104 Ni1 O11 C11 -45.4(4) . . . . ?
N31 Ni1 O11 C11 127.1(4) . . . . ?
O41 Ni1 O11 C11 164.6(9) . . . . ?
N21 Ni1 O11 C11 -138.8(4) . . . . ?
N101 Ni1 O11 C11 34.7(4) . . . . ?
N104 Ni3 O12 C11 43.8(4) . . . . ?
N107 Ni3 O12 C11 -88.7(8) . . . . ?
N116 Ni3 O12 C11 141.7(4) . . . . ?
N113 Ni3 O12 C11 -139.3(4) . . . . ?
N101 Ni3 O12 C11 -35.8(4) . . . . ?
Ni3 O12 C11 O11 -17.5(6) . . . . ?
Ni3 O12 C11 C12 161.8(4) . . . . ?
Ni1 O11 C11 O12 18.3(6) . . . . ?
Ni1 O11 C11 C12 -161.0(4) . . . . ?
O12 C11 C12 C17 -26.9(8) . . . . ?
O11 C11 C12 C17 152.5(6) . . . . ?
O12 C11 C12 C13 152.5(6) . . . . ?
O11 C11 C12 C13 -28.1(8) . . . . ?
C17 C12 C13 C14 1.0(12) . . . . ?
C11 C12 C13 C14 -178.4(7) . . . . ?
C12 C13 C14 C15 -2.4(13) . . . . ?
C13 C14 C15 C16 2.2(14) . . . . ?
C14 C15 C16 C17 -0.8(14) . . . . ?
C13 C12 C17 C16 0.5(11) . . . . ?
C11 C12 C17 C16 179.9(7) . . . . ?
C15 C16 C17 C12 -0.6(13) . . . . ?
N104 Ni1 N21 C21 72.9(6) . . . . ?
N31 Ni1 N21 C21 -110.0(6) . . . . ?
O41 Ni1 N21 C21 -21.5(6) . . . . ?
O11 Ni1 N21 C21 166.3(6) . . . . ?
N101 Ni1 N21 C21 104.4(17) . . . . ?
N104 Ni1 N21 N22 -100.9(4) . . . . ?
N31 Ni1 N21 N22 76.2(4) . . . . ?
O41 Ni1 N21 N22 164.7(4) . . . . ?
O11 Ni1 N21 N22 -7.5(4) . . . . ?
N101 Ni1 N21 N22 -69.4(18) . . . . ?
C21 N21 N22 C23 -0.2(6) . . . . ?
Ni1 N21 N22 C23 175.1(5) . . . . ?
N22 N21 C21 O21 -179.7(6) . . . . ?
Ni1 N21 C21 O21 5.7(10) . . . . ?
N22 N21 C21 C22 0.8(7) . . . . ?
Ni1 N21 C21 C22 -173.7(5) . . . . ?
O21 C21 C22 C23 179.4(7) . . . . ?
N21 C21 C22 C23 -1.2(9) . . . . ?
N21 N22 C23 C22 -0.6(8) . . . . ?
N21 N22 C23 C24 179.9(6) . . . . ?
C21 C22 C23 N22 1.0(8) . . . . ?
C21 C22 C23 C24 -179.6(8) . . . . ?
N104 Ni1 N31 C31 -112.7(16) . . . . ?
O41 Ni1 N31 C31 0.6(6) . . . . ?
N21 Ni1 N31 C31 88.3(6) . . . . ?
O11 Ni1 N31 C31 175.0(6) . . . . ?
N101 Ni1 N31 C31 -95.8(6) . . . . ?
N104 Ni1 N31 N32 65.9(17) . . . . ?
O41 Ni1 N31 N32 179.3(4) . . . . ?
N21 Ni1 N31 N32 -93.0(4) . . . . ?
O11 Ni1 N31 N32 -6.4(4) . . . . ?
N101 Ni1 N31 N32 82.9(4) . . . . ?
C31 N31 N32 C33 -0.5(6) . . . . ?
Ni1 N31 N32 C33 -179.5(4) . . . . ?
N32 N31 C31 O31 178.3(5) . . . . ?
Ni1 N31 C31 O31 -2.9(10) . . . . ?
N32 N31 C31 C32 0.1(7) . . . . ?
Ni1 N31 C31 C32 179.0(4) . . . . ?
N31 C31 C32 C33 0.2(8) . . . . ?
O31 C31 C32 C33 -177.8(6) . . . . ?
N31 N32 C33 C32 0.6(7) . . . . ?
N31 N32 C33 C34 -179.0(5) . . . . ?
C31 C32 C33 N32 -0.5(7) . . . . ?
C31 C32 C33 C34 179.1(7) . . . . ?
N104 Ni1 O41 C41 38.4(5) . . . . ?
N31 Ni1 O41 C41 -134.3(5) . . . . ?
N21 Ni1 O41 C41 131.8(5) . . . . ?
O11 Ni1 O41 C41 -171.6(9) . . . . ?
N101 Ni1 O41 C41 -42.2(5) . . . . ?
N51 Ni2 N41 C41 85.7(7) . . . . ?
O61 Ni2 N41 C41 174.4(7) . . . . ?
N110 Ni2 N41 C41 -122.8(16) . . . . ?
N107 Ni2 N41 C41 -94.0(7) . . . . ?
N101 Ni2 N41 C41 -12.0(7) . . . . ?
N51 Ni2 N41 N42 -98.8(3) . . . . ?
O61 Ni2 N41 N42 -10.0(3) . . . . ?
N110 Ni2 N41 N42 52.8(18) . . . . ?
N107 Ni2 N41 N42 81.6(3) . . . . ?
N101 Ni2 N41 N42 163.6(3) . . . . ?
C41 N41 N42 C43 -0.1(6) . . . . ?
Ni2 N41 N42 C43 -177.2(4) . . . . ?
Ni1 O41 C41 N41 40.5(8) . . . . ?
Ni1 O41 C41 C42 -140.2(5) . . . . ?
N42 N41 C41 O41 179.0(5) . . . . ?
Ni2 N41 C41 O41 -5.2(10) . . . . ?
N42 N41 C41 C42 -0.4(6) . . . . ?
Ni2 N41 C41 C42 175.4(5) . . . . ?
O41 C41 C42 C43 -178.7(6) . . . . ?
N41 C41 C42 C43 0.7(7) . . . . ?
N41 N42 C43 C42 0.5(7) . . . . ?
N41 N42 C43 C44 180.0(5) . . . . ?
C41 C42 C43 N42 -0.7(7) . . . . ?
C41 C42 C43 C44 179.9(7) . . . . ?
N41 Ni2 N51 C51 96.6(6) . . . . ?
O61 Ni2 N51 C51 9.4(6) . . . . ?
N110 Ni2 N51 C51 -79.9(6) . . . . ?
N107 Ni2 N51 C51 -95(7) . . . . ?
N101 Ni2 N51 C51 -169.8(6) . . . . ?
N41 Ni2 N51 N52 -72.0(4) . . . . ?
O61 Ni2 N51 N52 -159.2(4) . . . . ?
N110 Ni2 N51 N52 111.5(4) . . . . ?
N107 Ni2 N51 N52 97(7) . . . . ?
N101 Ni2 N51 N52 21.6(4) . . . . ?
C51 N51 N52 C53 0.1(6) . . . . ?
Ni2 N51 N52 C53 171.3(4) . . . . ?
N52 N51 C51 O51 177.2(6) . . . . ?
Ni2 N51 C51 O51 7.0(10) . . . . ?
N52 N51 C51 C52 -1.9(7) . . . . ?
Ni2 N51 C51 C52 -172.1(4) . . . . ?
N51 C51 C52 C53 3.0(8) . . . . ?
O51 C51 C52 C53 -176.1(7) . . . . ?
N51 N52 C53 C52 1.7(7) . . . . ?
N51 N52 C53 C54 -176.7(5) . . . . ?
C51 C52 C53 N52 -2.7(7) . . . . ?
C51 C52 C53 C54 175.5(7) . . . . ?
N51 Ni2 O61 C61 -136.5(5) . . . . ?
N41 Ni2 O61 C61 132.8(5) . . . . ?
N110 Ni2 O61 C61 -40.8(5) . . . . ?
N107 Ni2 O61 C61 41.7(5) . . . . ?
N101 Ni2 O61 C61 35.8(19) . . . . ?
N110 Ni4 N61 C61 32.0(5) . . . . ?
N116 Ni4 N61 C61 134.0(5) 3_695 . . . ?
N107 Ni4 N61 C61 -51.0(5) . . . . ?
N113 Ni4 N61 C61 -146.5(5) 3_695 . . . ?
N113 Ni4 N61 C61 -48.5(14) . . . . ?
N110 Ni4 N61 N62 -133.3(4) . . . . ?
N116 Ni4 N61 N62 -31.3(4) 3_695 . . . ?
N107 Ni4 N61 N62 143.7(4) . . . . ?
N113 Ni4 N61 N62 48.2(4) 3_695 . . . ?
N113 Ni4 N61 N62 146.2(10) . . . . ?
C61 N61 N62 C63 -0.4(6) . . . . ?
Ni4 N61 N62 C63 167.8(5) . . . . ?
Ni2 O61 C61 N61 -6.4(9) . . . . ?
Ni2 O61 C61 C62 172.2(5) . . . . ?
N62 N61 C61 O61 179.4(5) . . . . ?
Ni4 N61 C61 O61 11.9(9) . . . . ?
N62 N61 C61 C62 0.6(7) . . . . ?
Ni4 N61 C61 C62 -166.9(5) . . . . ?
O61 C61 C62 C63 -179.3(7) . . . . ?
N61 C61 C62 C63 -0.6(8) . . . . ?
N61 N62 C63 C62 0.1(8) . . . . ?
N61 N62 C63 C64 -179.8(7) . . . . ?
C61 C62 C63 N62 0.3(9) . . . . ?
C61 C62 C63 C64 -179.8(9) . . . . ?
O7S Na1 O1S C2S -151(2) . . . . ?
O5S Na1 O1S C2S 10(2) . . . . ?
O5T Na1 O1S C2S -29(2) . . . . ?
O3S Na1 O1S C2S -86(2) . . . . ?
N106 Na1 O1S C2S 47(3) . . . . ?
N118 Na1 O1S C2S 111(2) . . . . ?
O7T Na1 O1S C2S -168(2) . . . . ?
Na1 O1S C2S O2S 122(2) . . . . ?
Na1 O1S C2S C1S -56(3) . . . . ?
C3S O2S C2S O1S 0.5(12) . . . . ?
C3S O2S C2S C1S 179.0(8) . . . . ?
C2S O2S C3S C4S -170.9(8) . . . . ?
O7S Na1 O3S C6S -88.2(19) . . . . ?
O5S Na1 O3S C6S 83.0(18) . . . . ?
O1S Na1 O3S C6S 171.5(18) . . . . ?
O5T Na1 O3S C6S 82.2(18) . . . . ?
N106 Na1 O3S C6S 3.3(19) . . . . ?
N118 Na1 O3S C6S -70(2) . . . . ?
O7T Na1 O3S C6S -92.2(19) . . . . ?
Na1 O3S C6S C5S -54(4) . . . . ?
Na1 O3S C6S O4S 121.4(16) . . . . ?
C7S O4S C6S O3S -13(3) . . . . ?
C7S O4S C6S C5S 163(2) . . . . ?
C6S O4S C7S C8S 162.5(17) . . . . ?
O7S Na1 O5S C10S -161.1(15) . . . . ?
O1S Na1 O5S C10S 80.2(14) . . . . ?
O5T Na1 O5S C10S 178.4(17) . . . . ?
O3S Na1 O5S C10S 177.3(14) . . . . ?
N106 Na1 O5S C10S -89.9(14) . . . . ?
N118 Na1 O5S C10S -11.7(14) . . . . ?
O7T Na1 O5S C10S -121(5) . . . . ?
Na1 O5S C10S C9S -9(3) . . . . ?
Na1 O5S C10S O6S 165.2(9) . . . . ?
C11S O6S C10S O5S -4.9(18) . . . . ?
C11S O6S C10S C9S 169.9(12) . . . . ?
C10S O6S C11S C12S -85.7(15) . . . . ?
O7S Na1 O5T C10T -71(2) . . . . ?
O5S Na1 O5T C10T 101(2) . . . . ?
O1S Na1 O5T C10T -177(2) . . . . ?
O3S Na1 O5T C10T -81(2) . . . . ?
N106 Na1 O5T C10T 19(2) . . . . ?
N118 Na1 O5T C10T 85(2) . . . . ?
O7T Na1 O5T C10T -72(2) . . . . ?
C11T O6T C10T O5T -11(5) . . . . ?
C11T O6T C10T C9T 172(4) . . . . ?
Na1 O5T C10T O6T 63(4) . . . . ?
Na1 O5T C10T C9T -120(2) . . . . ?
C10T O6T C11T C12T 167(4) . . . . ?
O7S Na1 O7T C14T 144(3) . . . . ?
O5S Na1 O7T C14T 93(5) . . . . ?
O1S Na1 O7T C14T -108(2) . . . . ?
O5T Na1 O7T C14T 148.9(18) . . . . ?
O3S Na1 O7T C14T 156(2) . . . . ?
N106 Na1 O7T C14T 63(2) . . . . ?
N118 Na1 O7T C14T -16.6(19) . . . . ?
Na1 O7T C14T C13T -41(3) . . . . ?
Na1 O7T C14T O8T 130.1(17) . . . . ?
C15T O8T C14T O7T 14(3) . . . . ?
C15T O8T C14T C13T -173.7(19) . . . . ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        25.03
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         1.945
_refine_diff_density_min         -0.514
_refine_diff_density_rms         0.125