# Electronic Supplementary Material for CrystEngComm
# This journal is (c) The Royal Society of Chemistry 2008

data_global
_journal_name_full               CrystEngComm

_journal_coden_Cambridge         1350
_journal_volume                  ?
_journal_page_first              ?
_journal_year                    ?

_publ_contact_author_name        'Liangjie Yuan'
_publ_contact_author_email       LJYUAN@WHU.EDU.CN

_publ_section_title              
;
Hydrogen-bonded assembly of [Ni(Im)6]2+ ion and
phosphorous anions: Different sandwiched-type/tessellate-type
supramolecular architectures and 1D water chains
;
loop_
_publ_author_name
'Liangjie Yuan.'
'Shuoping Chen.'
'Ming Li.'
'Ling-ling Pan.'
'Yong Xiao.'

# Attachment 'S-8.cif'

data_60621lm_0m
_database_code_depnum_ccdc_archive 'CCDC 660451'
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C40 H60 N26 Ni3 O12 P4'
_chemical_formula_weight         1397.15

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'
P P 0.1023 0.0942 '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           triclinic
_symmetry_space_group_name_H-M   P-1

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.0688(5)
_cell_length_b                   14.8670(7)
_cell_length_c                   21.1059(10)
_cell_angle_alpha                69.3820(10)
_cell_angle_beta                 82.8330(10)
_cell_angle_gamma                88.8590(10)
_cell_volume                     2933.0(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    9166
_cell_measurement_theta_min      2.44
_cell_measurement_theta_max      29.82

_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.25
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.582
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1444
_exptl_absorpt_coefficient_mu    1.142
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7257
_exptl_absorpt_correction_T_max  0.7633
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      293(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            19135
_diffrn_reflns_av_R_equivalents  0.0133
_diffrn_reflns_av_sigmaI/netI    0.0268
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         2.08
_diffrn_reflns_theta_max         27.50
_reflns_number_total             13066
_reflns_number_gt                11209
_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 F² against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F², conventional R-factors R are based
on F, with F set to zero for negative F². The threshold expression of
F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F² 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/[σ²(Fo²)+(0.0398P)²+0.5671P] where P=(Fo²+2Fc²)/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     SHELXL
_refine_ls_extinction_coef       0.00077(14)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         13066
_refine_ls_number_parameters     828
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0354
_refine_ls_R_factor_gt           0.0287
_refine_ls_wR_factor_ref         0.0772
_refine_ls_wR_factor_gt          0.0744
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_restrained_S_all      1.063
_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 0.5000 0.5000 0.0000 0.02346(7) Uani 1 2 d S . .
N1 N 0.56718(16) 0.56612(11) 0.06476(7) 0.0288(3) Uani 1 1 d . . .
C2 C 0.4919(2) 0.58194(14) 0.11523(10) 0.0355(4) Uani 1 1 d . . .
H2 H 0.4012 0.5657 0.1269 0.043 Uiso 1 1 calc R . .
N3 N 0.5604(2) 0.62377(14) 0.14758(10) 0.0416(5) Uani 1 1 d . . .
C4 C 0.6879(2) 0.63535(17) 0.11767(12) 0.0482(6) Uani 1 1 d . . .
H4 H 0.7591 0.6620 0.1298 0.058 Uiso 1 1 calc R . .
C5 C 0.6919(2) 0.60040(16) 0.06618(11) 0.0408(5) Uani 1 1 d . . .
H5 H 0.7678 0.5997 0.0363 0.049 Uiso 1 1 calc R . .
N6 N 0.56837(15) 0.36650(11) 0.06207(8) 0.0288(3) Uani 1 1 d . . .
C7 C 0.6369(2) 0.34957(14) 0.11442(9) 0.0327(4) Uani 1 1 d . . .
H7 H 0.6645 0.3969 0.1296 0.039 Uiso 1 1 calc R . .
N8 N 0.66171(19) 0.25661(13) 0.14276(9) 0.0411(4) Uani 1 1 d . . .
C9 C 0.6065(3) 0.21007(16) 0.10709(13) 0.0543(6) Uani 1 1 d . . .
H9 H 0.6078 0.1444 0.1152 0.065 Uiso 1 1 calc R . .
C10 C 0.5494(2) 0.27795(15) 0.05753(12) 0.0451(5) Uani 1 1 d . . .
H10 H 0.5041 0.2664 0.0253 0.054 Uiso 1 1 calc R . .
N11 N 0.30825(16) 0.46908(11) 0.06224(7) 0.0292(3) Uani 1 1 d . . .
C12 C 0.28199(19) 0.40058(14) 0.12242(9) 0.0310(4) Uani 1 1 d . . .
H12 H 0.3459 0.3595 0.1447 0.037 Uiso 1 1 calc R . .
N13 N 0.15303(17) 0.39685(13) 0.14781(9) 0.0347(4) Uani 1 1 d . . .
C14 C 0.0912(2) 0.46659(16) 0.10132(11) 0.0439(5) Uani 1 1 d . . .
H14 H 0.0008 0.4808 0.1046 0.053 Uiso 1 1 calc R . .
C15 C 0.1870(2) 0.51152(16) 0.04905(10) 0.0406(5) Uani 1 1 d . . .
H15 H 0.1730 0.5632 0.0101 0.049 Uiso 1 1 calc R . .
Ni2 Ni 1.0000 1.0000 0.0000 0.02377(7) Uani 1 2 d S . .
N16 N 1.03113(16) 1.09875(11) 0.04854(8) 0.0302(3) Uani 1 1 d . . .
C17 C 0.9566(2) 1.10620(15) 0.10218(10) 0.0374(5) Uani 1 1 d . . .
H17 H 0.8792 1.0694 0.1235 0.045 Uiso 1 1 calc R . .
N18 N 1.0051(2) 1.17254(14) 0.12221(10) 0.0480(5) Uani 1 1 d . . .
C19 C 1.1170(3) 1.2109(2) 0.07966(13) 0.0654(8) Uani 1 1 d . . .
H19 H 1.1724 1.2593 0.0811 0.078 Uiso 1 1 calc R . .
C20 C 1.1322(3) 1.16487(17) 0.03439(12) 0.0516(6) Uani 1 1 d . . .
H20 H 1.2016 1.1766 -0.0012 0.062 Uiso 1 1 calc R . .
N21 N 1.10187(16) 0.89394(11) 0.07268(7) 0.0302(3) Uani 1 1 d . . .
C22 C 1.1468(2) 0.90036(15) 0.12705(9) 0.0353(4) Uani 1 1 d . . .
H22 H 1.1342 0.9532 0.1408 0.042 Uiso 1 1 calc R . .
N23 N 1.21238(18) 0.82256(14) 0.16009(9) 0.0399(4) Uani 1 1 d . . .
C24 C 1.2103(3) 0.76228(17) 0.12528(12) 0.0518(6) Uani 1 1 d . . .
H24 H 1.2485 0.7021 0.1360 0.062 Uiso 1 1 calc R . .
C25 C 1.1424(2) 0.80584(15) 0.07180(11) 0.0458(5) Uani 1 1 d . . .
H25 H 1.1256 0.7800 0.0393 0.055 Uiso 1 1 calc R . .
N26 N 0.81315(16) 0.95423(11) 0.06244(7) 0.0298(3) Uani 1 1 d . . .
C27 C 0.7943(2) 0.88791(15) 0.12414(10) 0.0377(5) Uani 1 1 d . . .
H27 H 0.8635 0.8564 0.1479 0.045 Uiso 1 1 calc R . .
N28 N 0.66564(19) 0.87128(14) 0.14854(9) 0.0399(4) Uani 1 1 d . . .
C29 C 0.5959(2) 0.92980(19) 0.10044(12) 0.0533(6) Uani 1 1 d . . .
H29 H 0.5032 0.9340 0.1030 0.064 Uiso 1 1 calc R . .
C30 C 0.6860(2) 0.98125(17) 0.04777(11) 0.0467(6) Uani 1 1 d . . .
H30 H 0.6652 1.0278 0.0077 0.056 Uiso 1 1 calc R . .
Ni3 Ni 0.87128(2) 0.806668(15) 0.653205(11) 0.02211(6) Uani 1 1 d . . .
N61 N 1.05504(15) 0.89211(10) 0.61929(7) 0.0253(3) Uani 1 1 d . . .
H61A H 1.0635 0.9249 0.5741 0.030 Uiso 1 1 calc R . .
H61B H 1.0588 0.9338 0.6413 0.030 Uiso 1 1 calc R . .
C62 C 1.16072(17) 0.81793(12) 0.63734(9) 0.0235(3) Uani 1 1 d . . .
C63 C 1.30327(19) 0.85934(15) 0.61792(10) 0.0368(4) Uani 1 1 d . . .
H63A H 1.3177 0.8956 0.5699 0.055 Uiso 1 1 calc R . .
H63B H 1.3653 0.8079 0.6287 0.055 Uiso 1 1 calc R . .
H63C H 1.3166 0.9006 0.6429 0.055 Uiso 1 1 calc R . .
P1 P 1.12781(5) 0.74274(3) 0.58814(2) 0.02472(10) Uani 1 1 d . . .
O1 O 0.98293(13) 0.71139(9) 0.61281(6) 0.0289(3) Uani 1 1 d . . .
O2 O 1.13743(15) 0.81733(10) 0.51311(7) 0.0342(3) Uani 1 1 d . . .
O3 O 1.22828(14) 0.66597(9) 0.59254(6) 0.0346(3) Uani 1 1 d . . .
P2 P 1.11983(4) 0.75430(3) 0.73044(2) 0.02099(9) Uani 1 1 d . . .
O4 O 0.96666(12) 0.74466(9) 0.74095(6) 0.0281(3) Uani 1 1 d . . .
O5 O 1.16528(13) 0.82384(8) 0.76321(6) 0.0280(3) Uani 1 1 d . . .
O6 O 1.18954(13) 0.66066(9) 0.75373(7) 0.0313(3) Uani 1 1 d . . .
N31 N 0.72140(15) 0.69935(11) 0.69278(8) 0.0287(3) Uani 1 1 d . . .
C32 C 0.7410(2) 0.60866(14) 0.69906(10) 0.0347(4) Uani 1 1 d . . .
H32 H 0.8244 0.5839 0.6913 0.042 Uiso 1 1 calc R . .
N33 N 0.62635(19) 0.55674(14) 0.71801(9) 0.0421(4) Uani 1 1 d . . .
C34 C 0.5272(2) 0.61803(17) 0.72459(11) 0.0470(6) Uani 1 1 d . . .
H34 H 0.4363 0.6028 0.7371 0.056 Uiso 1 1 calc R . .
C35 C 0.5861(2) 0.70458(16) 0.70948(11) 0.0389(5) Uani 1 1 d . . .
H35 H 0.5419 0.7598 0.7102 0.047 Uiso 1 1 calc R . .
N36 N 0.78550(16) 0.86963(11) 0.56117(8) 0.0321(3) Uani 1 1 d . . .
C37 C 0.8250(2) 0.86244(15) 0.50175(11) 0.0427(5) Uani 1 1 d . . .
H37 H 0.9118 0.8488 0.4877 0.051 Uiso 1 1 calc R . .
N38 N 0.7231(2) 0.87745(14) 0.46352(10) 0.0532(6) Uani 1 1 d . . .
C39 C 0.6131(2) 0.89568(17) 0.49894(12) 0.0485(6) Uani 1 1 d . . .
H39 H 0.5283 0.9082 0.4852 0.058 Uiso 1 1 calc R . .
C40 C 0.6511(2) 0.89204(18) 0.55896(12) 0.0466(5) Uani 1 1 d . . .
H40 H 0.5951 0.9030 0.5939 0.056 Uiso 1 1 calc R . .
N41 N 0.77381(16) 0.90272(11) 0.69299(8) 0.0293(3) Uani 1 1 d . . .
C42 C 0.7562(2) 0.99559(14) 0.66126(11) 0.0377(5) Uani 1 1 d . . .
H42 H 0.7799 1.0278 0.6147 0.045 Uiso 1 1 calc R . .
N43 N 0.70052(19) 1.03696(14) 0.70407(11) 0.0468(5) Uani 1 1 d . . .
C44 C 0.6818(3) 0.96887(18) 0.76675(14) 0.0551(6) Uani 1 1 d . . .
H44 H 0.6453 0.9772 0.8070 0.066 Uiso 1 1 calc R . .
C45 C 0.7264(2) 0.88606(15) 0.75979(11) 0.0430(5) Uani 1 1 d . . .
H45 H 0.7250 0.8269 0.7950 0.052 Uiso 1 1 calc R . .
Ni4 Ni 0.69069(2) 0.697916(15) 0.350534(11) 0.02110(6) Uani 1 1 d . . .
N64 N 0.53178(15) 0.58888(10) 0.39195(7) 0.0266(3) Uani 1 1 d . . .
H64A H 0.5351 0.5483 0.3687 0.032 Uiso 1 1 calc R . .
H64B H 0.5359 0.5551 0.4364 0.032 Uiso 1 1 calc R . .
C65 C 0.40884(17) 0.64802(12) 0.38227(9) 0.0240(3) Uani 1 1 d . . .
C66 C 0.2785(2) 0.58858(16) 0.40652(11) 0.0414(5) Uani 1 1 d . . .
H66A H 0.2768 0.5439 0.3830 0.062 Uiso 1 1 calc R . .
H66B H 0.2040 0.6305 0.3970 0.062 Uiso 1 1 calc R . .
H66C H 0.2726 0.5540 0.4547 0.062 Uiso 1 1 calc R . .
P3 P 0.42645(4) 0.71301(3) 0.28915(2) 0.02158(9) Uani 1 1 d . . .
O7 O 0.57082(13) 0.75283(9) 0.27212(6) 0.0291(3) Uani 1 1 d . . .
O8 O 0.40801(14) 0.63752(9) 0.25760(7) 0.0343(3) Uani 1 1 d . . .
O9 O 0.32472(14) 0.79103(9) 0.27288(7) 0.0342(3) Uani 1 1 d . . .
P4 P 0.42695(5) 0.72811(3) 0.42974(2) 0.02542(10) Uani 1 1 d . . .
O10 O 0.56513(13) 0.77235(9) 0.40373(6) 0.0296(3) Uani 1 1 d . . .
O11 O 0.42508(16) 0.65710(11) 0.50547(7) 0.0370(3) Uani 1 1 d . . .
O12 O 0.31341(14) 0.79603(10) 0.42395(6) 0.0355(3) Uani 1 1 d . . .
N46 N 0.80691(15) 0.82589(10) 0.31067(8) 0.0274(3) Uani 1 1 d . . .
C47 C 0.7488(2) 0.90992(12) 0.29050(9) 0.0300(4) Uani 1 1 d . . .
H47 H 0.6573 0.9176 0.2887 0.036 Uiso 1 1 calc R . .
N48 N 0.83807(18) 0.98266(12) 0.27297(9) 0.0346(4) Uani 1 1 d . . .
C49 C 0.9604(2) 0.94399(15) 0.28188(11) 0.0409(5) Uani 1 1 d . . .
H49 H 1.0418 0.9773 0.2735 0.049 Uiso 1 1 calc R . .
C50 C 0.9409(2) 0.84720(14) 0.30542(11) 0.0374(5) Uani 1 1 d . . .
H50 H 1.0078 0.8023 0.3163 0.045 Uiso 1 1 calc R . .
N51 N 0.80651(15) 0.62460(10) 0.29694(8) 0.0276(3) Uani 1 1 d . . .
C52 C 0.7826(2) 0.53481(14) 0.30243(11) 0.0360(4) Uani 1 1 d . . .
H52 H 0.7129 0.4961 0.3319 0.043 Uiso 1 1 calc R . .
N53 N 0.86928(18) 0.50618(12) 0.26110(9) 0.0382(4) Uani 1 1 d . . .
C54 C 0.9550(2) 0.58074(16) 0.22673(12) 0.0451(5) Uani 1 1 d . . .
H54 H 1.0269 0.5820 0.1941 0.054 Uiso 1 1 calc R . .
C55 C 0.9164(2) 0.65348(14) 0.24875(11) 0.0385(5) Uani 1 1 d . . .
H55 H 0.9581 0.7139 0.2335 0.046 Uiso 1 1 calc R . .
N56 N 0.79365(16) 0.64478(11) 0.43406(8) 0.0289(3) Uani 1 1 d . . .
C57 C 0.7642(2) 0.65737(14) 0.49284(10) 0.0345(4) Uani 1 1 d . . .
H57 H 0.6811 0.6757 0.5081 0.041 Uiso 1 1 calc R . .
N58 N 0.86974(19) 0.64034(12) 0.52773(9) 0.0371(4) Uani 1 1 d . . .
C59 C 0.9719(2) 0.61600(17) 0.49006(11) 0.0452(5) Uani 1 1 d . . .
H59 H 1.0582 0.6011 0.5012 0.054 Uiso 1 1 calc R . .
C60 C 0.9241(2) 0.61756(17) 0.43283(11) 0.0435(5) Uani 1 1 d . . .
H60 H 0.9728 0.6023 0.3977 0.052 Uiso 1 1 calc R . .
H3 H 0.528(3) 0.638(2) 0.1748(14) 0.061(9) Uiso 1 1 d . . .
H8 H 0.710(3) 0.2317(17) 0.1763(12) 0.054(7) Uiso 1 1 d . . .
H13 H 0.112(3) 0.3565(18) 0.1839(13) 0.053(7) Uiso 1 1 d . . .
H18 H 0.974(3) 1.1832(19) 0.1533(14) 0.058(8) Uiso 1 1 d . . .
H23 H 1.243(3) 0.8119(17) 0.1966(13) 0.053(7) Uiso 1 1 d . . .
H28 H 0.634(3) 0.8347(18) 0.1865(13) 0.056(8) Uiso 1 1 d . . .
H33 H 0.616(3) 0.489(2) 0.7262(14) 0.069(8) Uiso 1 1 d . . .
H38 H 0.720(3) 0.863(2) 0.4237(15) 0.080(9) Uiso 1 1 d . . .
H43 H 0.687(3) 1.0963(19) 0.6944(13) 0.063(8) Uiso 1 1 d . . .
H48 H 0.819(3) 1.0443(19) 0.2595(13) 0.059(8) Uiso 1 1 d . . .
H53 H 0.860(2) 0.4509(17) 0.2558(11) 0.044(6) Uiso 1 1 d . . .
H58 H 0.874(3) 0.6535(19) 0.5631(14) 0.065(8) Uiso 1 1 d . . .
H98 H 1.194(3) 0.810(2) 0.4895(15) 0.075(10) Uiso 1 1 d . . .
H99 H 0.367(3) 0.659(2) 0.5281(15) 0.069(10) Uiso 1 1 d . . .


_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 N6 2.1139(15) . ?
Ni1 N6 2.1139(15) 2_665 ?
Ni1 N1 2.1201(15) 2_665 ?
Ni1 N1 2.1201(15) . ?
Ni1 N11 2.1545(15) 2_665 ?
Ni1 N11 2.1545(15) . ?
N1 C2 1.316(2) . ?
N1 C5 1.373(3) . ?
C2 N3 1.327(3) . ?
C2 H2 0.9300 . ?
N3 C4 1.344(3) . ?
N3 H3 0.72(3) . ?
C4 C5 1.356(3) . ?
C4 H4 0.9300 . ?
C5 H5 0.9300 . ?
N6 C7 1.322(2) . ?
N6 C10 1.372(2) . ?
C7 N8 1.331(2) . ?
C7 H7 0.9300 . ?
N8 C9 1.357(3) . ?
N8 H8 0.88(2) . ?
C9 C10 1.352(3) . ?
C9 H9 0.9300 . ?
C10 H10 0.9300 . ?
N11 C12 1.318(2) . ?
N11 C15 1.377(3) . ?
C12 N13 1.336(2) . ?
C12 H12 0.9300 . ?
N13 C14 1.355(3) . ?
N13 H13 0.85(3) . ?
C14 C15 1.355(3) . ?
C14 H14 0.9300 . ?
C15 H15 0.9300 . ?
Ni2 N16 2.1122(15) 2_775 ?
Ni2 N16 2.1122(15) . ?
Ni2 N21 2.1251(15) . ?
Ni2 N21 2.1251(15) 2_775 ?
Ni2 N26 2.1307(15) 2_775 ?
Ni2 N26 2.1307(15) . ?
N16 C17 1.315(2) . ?
N16 C20 1.360(3) . ?
C17 N18 1.325(3) . ?
C17 H17 0.9300 . ?
N18 C19 1.347(3) . ?
N18 H18 0.76(3) . ?
C19 C20 1.351(3) . ?
C19 H19 0.9300 . ?
C20 H20 0.9300 . ?
N21 C22 1.319(2) . ?
N21 C25 1.370(3) . ?
C22 N23 1.333(3) . ?
C22 H22 0.9300 . ?
N23 C24 1.346(3) . ?
N23 H23 0.83(2) . ?
C24 C25 1.350(3) . ?
C24 H24 0.9300 . ?
C25 H25 0.9300 . ?
N26 C27 1.321(2) . ?
N26 C30 1.374(3) . ?
C27 N28 1.327(3) . ?
C27 H27 0.9300 . ?
N28 C29 1.346(3) . ?
N28 H28 0.82(3) . ?
C29 C30 1.350(3) . ?
C29 H29 0.9300 . ?
C30 H30 0.9300 . ?
Ni3 N41 2.0714(15) . ?
Ni3 N31 2.0888(15) . ?
Ni3 O4 2.0996(12) . ?
Ni3 N36 2.1217(15) . ?
Ni3 O1 2.1319(12) . ?
Ni3 N61 2.1615(15) . ?
N61 C62 1.501(2) . ?
N61 H61A 0.9000 . ?
N61 H61B 0.9000 . ?
C62 C63 1.522(2) . ?
C62 P1 1.8318(17) . ?
C62 P2 1.8520(18) . ?
C63 H63A 0.9600 . ?
C63 H63B 0.9600 . ?
C63 H63C 0.9600 . ?
P1 O3 1.4958(13) . ?
P1 O1 1.5110(13) . ?
P1 O2 1.5736(14) . ?
O2 H98 0.74(3) . ?
P2 O6 1.4959(12) . ?
P2 O4 1.5327(13) . ?
P2 O5 1.5357(12) . ?
N31 C32 1.321(2) . ?
N31 C35 1.371(2) . ?
C32 N33 1.338(3) . ?
C32 H32 0.9300 . ?
N33 C34 1.365(3) . ?
N33 H33 0.97(3) . ?
C34 C35 1.343(3) . ?
C34 H34 0.9300 . ?
C35 H35 0.9300 . ?
N36 C37 1.308(3) . ?
N36 C40 1.390(3) . ?
C37 N38 1.350(3) . ?
C37 H37 0.9300 . ?
N38 C39 1.336(3) . ?
N38 H38 0.94(3) . ?
C39 C40 1.351(3) . ?
C39 H39 0.9300 . ?
C40 H40 0.9300 . ?
N41 C42 1.325(2) . ?
N41 C45 1.367(2) . ?
C42 N43 1.327(3) . ?
C42 H42 0.9300 . ?
N43 C44 1.346(3) . ?
N43 H43 0.85(3) . ?
C44 C45 1.352(3) . ?
C44 H44 0.9300 . ?
C45 H45 0.9300 . ?
Ni4 N56 2.0615(15) . ?
Ni4 N51 2.0774(14) . ?
Ni4 O7 2.0904(12) . ?
Ni4 N46 2.1007(15) . ?
Ni4 O10 2.1327(12) . ?
Ni4 N64 2.1699(15) . ?
N64 C65 1.497(2) . ?
N64 H64A 0.9000 . ?
N64 H64B 0.9000 . ?
C65 C66 1.525(2) . ?
C65 P4 1.8299(18) . ?
C65 P3 1.8467(17) . ?
C66 H66A 0.9600 . ?
C66 H66B 0.9600 . ?
C66 H66C 0.9600 . ?
P3 O9 1.5074(13) . ?
P3 O8 1.5177(13) . ?
P3 O7 1.5319(13) . ?
P4 O12 1.4979(13) . ?
P4 O10 1.5037(14) . ?
P4 O11 1.5731(14) . ?
O11 H99 0.72(3) . ?
N46 C47 1.320(2) . ?
N46 C50 1.374(2) . ?
C47 N48 1.337(2) . ?
C47 H47 0.9300 . ?
N48 C49 1.356(3) . ?
N48 H48 0.88(3) . ?
C49 C50 1.356(3) . ?
C49 H49 0.9300 . ?
C50 H50 0.9300 . ?
N51 C52 1.323(2) . ?
N51 C55 1.369(2) . ?
C52 N53 1.327(3) . ?
C52 H52 0.9300 . ?
N53 C54 1.347(3) . ?
N53 H53 0.88(2) . ?
C54 C55 1.352(3) . ?
C54 H54 0.9300 . ?
C55 H55 0.9300 . ?
N56 C57 1.316(2) . ?
N56 C60 1.367(3) . ?
C57 N58 1.337(2) . ?
C57 H57 0.9300 . ?
N58 C59 1.344(3) . ?
N58 H58 0.84(3) . ?
C59 C60 1.348(3) . ?
C59 H59 0.9300 . ?
C60 H60 0.9300 . ?

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
N6 Ni1 N6 180.00(8) . 2_665 ?
N6 Ni1 N1 90.23(6) . 2_665 ?
N6 Ni1 N1 89.77(6) 2_665 2_665 ?
N6 Ni1 N1 89.77(6) . . ?
N6 Ni1 N1 90.23(6) 2_665 . ?
N1 Ni1 N1 180.00(6) 2_665 . ?
N6 Ni1 N11 90.52(6) . 2_665 ?
N6 Ni1 N11 89.48(6) 2_665 2_665 ?
N1 Ni1 N11 89.89(6) 2_665 2_665 ?
N1 Ni1 N11 90.11(6) . 2_665 ?
N6 Ni1 N11 89.48(6) . . ?
N6 Ni1 N11 90.52(6) 2_665 . ?
N1 Ni1 N11 90.11(6) 2_665 . ?
N1 Ni1 N11 89.89(6) . . ?
N11 Ni1 N11 180.0 2_665 . ?
C2 N1 C5 104.21(16) . . ?
C2 N1 Ni1 125.14(14) . . ?
C5 N1 Ni1 130.64(13) . . ?
N1 C2 N3 112.27(19) . . ?
N1 C2 H2 123.9 . . ?
N3 C2 H2 123.9 . . ?
C2 N3 C4 107.54(18) . . ?
C2 N3 H3 121(2) . . ?
C4 N3 H3 132(2) . . ?
N3 C4 C5 106.2(2) . . ?
N3 C4 H4 126.9 . . ?
C5 C4 H4 126.9 . . ?
C4 C5 N1 109.77(19) . . ?
C4 C5 H5 125.1 . . ?
N1 C5 H5 125.1 . . ?
C7 N6 C10 104.75(16) . . ?
C7 N6 Ni1 127.75(13) . . ?
C10 N6 Ni1 127.50(13) . . ?
N6 C7 N8 111.89(18) . . ?
N6 C7 H7 124.1 . . ?
N8 C7 H7 124.1 . . ?
C7 N8 C9 107.23(17) . . ?
C7 N8 H8 125.5(16) . . ?
C9 N8 H8 127.1(16) . . ?
C10 C9 N8 106.45(19) . . ?
C10 C9 H9 126.8 . . ?
N8 C9 H9 126.8 . . ?
C9 C10 N6 109.68(19) . . ?
C9 C10 H10 125.2 . . ?
N6 C10 H10 125.2 . . ?
C12 N11 C15 104.49(16) . . ?
C12 N11 Ni1 125.86(13) . . ?
C15 N11 Ni1 129.63(13) . . ?
N11 C12 N13 112.26(18) . . ?
N11 C12 H12 123.9 . . ?
N13 C12 H12 123.9 . . ?
C12 N13 C14 107.07(17) . . ?
C12 N13 H13 129.2(17) . . ?
C14 N13 H13 123.4(17) . . ?
C15 C14 N13 106.45(19) . . ?
C15 C14 H14 126.8 . . ?
N13 C14 H14 126.8 . . ?
C14 C15 N11 109.72(18) . . ?
C14 C15 H15 125.1 . . ?
N11 C15 H15 125.1 . . ?
N16 Ni2 N16 180.00(6) 2_775 . ?
N16 Ni2 N21 90.17(6) 2_775 . ?
N16 Ni2 N21 89.83(6) . . ?
N16 Ni2 N21 89.83(6) 2_775 2_775 ?
N16 Ni2 N21 90.17(6) . 2_775 ?
N21 Ni2 N21 180.0 . 2_775 ?
N16 Ni2 N26 90.65(6) 2_775 2_775 ?
N16 Ni2 N26 89.35(6) . 2_775 ?
N21 Ni2 N26 88.98(6) . 2_775 ?
N21 Ni2 N26 91.02(6) 2_775 2_775 ?
N16 Ni2 N26 89.35(6) 2_775 . ?
N16 Ni2 N26 90.65(6) . . ?
N21 Ni2 N26 91.02(6) . . ?
N21 Ni2 N26 88.98(6) 2_775 . ?
N26 Ni2 N26 180.0 2_775 . ?
C17 N16 C20 104.71(17) . . ?
C17 N16 Ni2 126.16(14) . . ?
C20 N16 Ni2 129.08(14) . . ?
N16 C17 N18 111.8(2) . . ?
N16 C17 H17 124.1 . . ?
N18 C17 H17 124.1 . . ?
C17 N18 C19 107.61(19) . . ?
C17 N18 H18 123(2) . . ?
C19 N18 H18 129(2) . . ?
N18 C19 C20 105.9(2) . . ?
N18 C19 H19 127.0 . . ?
C20 C19 H19 127.0 . . ?
C19 C20 N16 110.0(2) . . ?
C19 C20 H20 125.0 . . ?
N16 C20 H20 125.0 . . ?
C22 N21 C25 104.27(16) . . ?
C22 N21 Ni2 127.58(13) . . ?
C25 N21 Ni2 128.06(13) . . ?
N21 C22 N23 112.38(19) . . ?
N21 C22 H22 123.8 . . ?
N23 C22 H22 123.8 . . ?
C22 N23 C24 106.73(18) . . ?
C22 N23 H23 126.3(17) . . ?
C24 N23 H23 126.8(17) . . ?
N23 C24 C25 106.93(19) . . ?
N23 C24 H24 126.5 . . ?
C25 C24 H24 126.5 . . ?
C24 C25 N21 109.69(19) . . ?
C24 C25 H25 125.2 . . ?
N21 C25 H25 125.2 . . ?
C27 N26 C30 104.08(17) . . ?
C27 N26 Ni2 126.57(14) . . ?
C30 N26 Ni2 129.26(13) . . ?
N26 C27 N28 112.53(19) . . ?
N26 C27 H27 123.7 . . ?
N28 C27 H27 123.7 . . ?
C27 N28 C29 106.86(18) . . ?
C27 N28 H28 126.8(19) . . ?
C29 N28 H28 126.2(19) . . ?
N28 C29 C30 107.0(2) . . ?
N28 C29 H29 126.5 . . ?
C30 C29 H29 126.5 . . ?
C29 C30 N26 109.6(2) . . ?
C29 C30 H30 125.2 . . ?
N26 C30 H30 125.2 . . ?
N41 Ni3 N31 95.57(6) . . ?
N41 Ni3 O4 91.66(6) . . ?
N31 Ni3 O4 89.93(5) . . ?
N41 Ni3 N36 90.55(6) . . ?
N31 Ni3 N36 92.21(6) . . ?
O4 Ni3 N36 176.76(6) . . ?
N41 Ni3 O1 176.49(6) . . ?
N31 Ni3 O1 87.45(5) . . ?
O4 Ni3 O1 86.55(5) . . ?
N36 Ni3 O1 91.12(6) . . ?
N41 Ni3 N61 93.56(6) . . ?
N31 Ni3 N61 167.64(6) . . ?
O4 Ni3 N61 81.47(5) . . ?
N36 Ni3 N61 96.03(6) . . ?
O1 Ni3 N61 83.20(5) . . ?
C62 N61 Ni3 102.87(10) . . ?
C62 N61 H61A 111.2 . . ?
Ni3 N61 H61A 111.2 . . ?
C62 N61 H61B 111.2 . . ?
Ni3 N61 H61B 111.2 . . ?
H61A N61 H61B 109.1 . . ?
N61 C62 C63 114.00(14) . . ?
N61 C62 P1 101.93(11) . . ?
C63 C62 P1 111.17(12) . . ?
N61 C62 P2 104.46(11) . . ?
C63 C62 P2 112.42(13) . . ?
P1 C62 P2 112.29(9) . . ?
C62 C63 H63A 109.5 . . ?
C62 C63 H63B 109.5 . . ?
H63A C63 H63B 109.5 . . ?
C62 C63 H63C 109.5 . . ?
H63A C63 H63C 109.5 . . ?
H63B C63 H63C 109.5 . . ?
O3 P1 O1 117.61(8) . . ?
O3 P1 O2 110.40(8) . . ?
O1 P1 O2 108.59(8) . . ?
O3 P1 C62 113.10(8) . . ?
O1 P1 C62 103.20(7) . . ?
O2 P1 C62 102.71(8) . . ?
P1 O1 Ni3 113.50(7) . . ?
P1 O2 H98 114(2) . . ?
O6 P2 O4 114.25(8) . . ?
O6 P2 O5 111.66(7) . . ?
O4 P2 O5 110.08(7) . . ?
O6 P2 C62 111.42(8) . . ?
O4 P2 C62 103.74(7) . . ?
O5 P2 C62 105.03(7) . . ?
P2 O4 Ni3 115.94(7) . . ?
C32 N31 C35 104.96(17) . . ?
C32 N31 Ni3 123.50(13) . . ?
C35 N31 Ni3 131.10(13) . . ?
N31 C32 N33 111.88(19) . . ?
N31 C32 H32 124.1 . . ?
N33 C32 H32 124.1 . . ?
C32 N33 C34 106.53(18) . . ?
C32 N33 H33 126.8(17) . . ?
C34 N33 H33 126.7(17) . . ?
C35 C34 N33 106.84(19) . . ?
C35 C34 H34 126.6 . . ?
N33 C34 H34 126.6 . . ?
C34 C35 N31 109.79(19) . . ?
C34 C35 H35 125.1 . . ?
N31 C35 H35 125.1 . . ?
C37 N36 C40 104.20(17) . . ?
C37 N36 Ni3 127.79(14) . . ?
C40 N36 Ni3 123.56(14) . . ?
N36 C37 N38 111.1(2) . . ?
N36 C37 H37 124.4 . . ?
N38 C37 H37 124.4 . . ?
C39 N38 C37 108.79(19) . . ?
C39 N38 H38 122.2(19) . . ?
C37 N38 H38 127.4(18) . . ?
N38 C39 C40 105.4(2) . . ?
N38 C39 H39 127.3 . . ?
C40 C39 H39 127.3 . . ?
C39 C40 N36 110.5(2) . . ?
C39 C40 H40 124.8 . . ?
N36 C40 H40 124.8 . . ?
C42 N41 C45 104.77(16) . . ?
C42 N41 Ni3 127.91(14) . . ?
C45 N41 Ni3 126.98(13) . . ?
N41 C42 N43 111.6(2) . . ?
N41 C42 H42 124.2 . . ?
N43 C42 H42 124.2 . . ?
C42 N43 C44 107.54(18) . . ?
C42 N43 H43 126.0(18) . . ?
C44 N43 H43 126.2(18) . . ?
N43 C44 C45 106.6(2) . . ?
N43 C44 H44 126.7 . . ?
C45 C44 H44 126.7 . . ?
C44 C45 N41 109.5(2) . . ?
C44 C45 H45 125.2 . . ?
N41 C45 H45 125.2 . . ?
N56 Ni4 N51 92.90(6) . . ?
N56 Ni4 O7 174.64(6) . . ?
N51 Ni4 O7 91.86(6) . . ?
N56 Ni4 N46 92.49(6) . . ?
N51 Ni4 N46 96.06(6) . . ?
O7 Ni4 N46 89.47(5) . . ?
N56 Ni4 O10 88.97(5) . . ?
N51 Ni4 O10 177.73(5) . . ?
O7 Ni4 O10 86.22(5) . . ?
N46 Ni4 O10 85.13(5) . . ?
N56 Ni4 N64 94.28(6) . . ?
N51 Ni4 N64 95.44(6) . . ?
O7 Ni4 N64 82.80(5) . . ?
N46 Ni4 N64 166.33(6) . . ?
O10 Ni4 N64 83.13(5) . . ?
C65 N64 Ni4 102.11(10) . . ?
C65 N64 H64A 111.3 . . ?
Ni4 N64 H64A 111.3 . . ?
C65 N64 H64B 111.3 . . ?
Ni4 N64 H64B 111.3 . . ?
H64A N64 H64B 109.2 . . ?
N64 C65 C66 113.72(15) . . ?
N64 C65 P4 103.85(11) . . ?
C66 C65 P4 112.39(13) . . ?
N64 C65 P3 103.21(11) . . ?
C66 C65 P3 110.84(13) . . ?
P4 C65 P3 112.34(9) . . ?
C65 C66 H66A 109.5 . . ?
C65 C66 H66B 109.5 . . ?
H66A C66 H66B 109.5 . . ?
C65 C66 H66C 109.5 . . ?
H66A C66 H66C 109.5 . . ?
H66B C66 H66C 109.5 . . ?
O9 P3 O8 113.37(8) . . ?
O9 P3 O7 112.73(8) . . ?
O8 P3 O7 111.15(8) . . ?
O9 P3 C65 109.35(8) . . ?
O8 P3 C65 105.84(8) . . ?
O7 P3 C65 103.70(7) . . ?
P3 O7 Ni4 115.16(7) . . ?
O12 P4 O10 116.72(8) . . ?
O12 P4 O11 110.63(8) . . ?
O10 P4 O11 109.11(8) . . ?
O12 P4 C65 111.56(8) . . ?
O10 P4 C65 104.43(7) . . ?
O11 P4 C65 103.43(8) . . ?
P4 O10 Ni4 114.03(7) . . ?
P4 O11 H99 115(2) . . ?
C47 N46 C50 105.22(15) . . ?
C47 N46 Ni4 120.35(13) . . ?
C50 N46 Ni4 134.07(13) . . ?
N46 C47 N48 111.50(18) . . ?
N46 C47 H47 124.2 . . ?
N48 C47 H47 124.2 . . ?
C47 N48 C49 107.43(17) . . ?
C47 N48 H48 125.5(17) . . ?
C49 N48 H48 127.0(17) . . ?
N48 C49 C50 106.46(18) . . ?
N48 C49 H49 126.8 . . ?
C50 C49 H49 126.8 . . ?
C49 C50 N46 109.39(18) . . ?
C49 C50 H50 125.3 . . ?
N46 C50 H50 125.3 . . ?
C52 N51 C55 104.28(15) . . ?
C52 N51 Ni4 124.46(13) . . ?
C55 N51 Ni4 131.23(12) . . ?
N51 C52 N53 112.33(18) . . ?
N51 C52 H52 123.8 . . ?
N53 C52 H52 123.8 . . ?
C52 N53 C54 106.97(17) . . ?
C52 N53 H53 122.1(15) . . ?
C54 N53 H53 130.4(15) . . ?
N53 C54 C55 106.78(18) . . ?
N53 C54 H54 126.6 . . ?
C55 C54 H54 126.6 . . ?
C54 C55 N51 109.64(18) . . ?
C54 C55 H55 125.2 . . ?
N51 C55 H55 125.2 . . ?
C57 N56 C60 104.96(16) . . ?
C57 N56 Ni4 126.33(13) . . ?
C60 N56 Ni4 125.80(13) . . ?
N56 C57 N58 111.06(18) . . ?
N56 C57 H57 124.5 . . ?
N58 C57 H57 124.5 . . ?
C57 N58 C59 107.91(17) . . ?
C57 N58 H58 124.5(19) . . ?
C59 N58 H58 126.6(19) . . ?
N58 C59 C60 106.06(19) . . ?
N58 C59 H59 127.0 . . ?
C60 C59 H59 127.0 . . ?
C59 C60 N56 110.00(19) . . ?
C59 C60 H60 125.0 . . ?
N56 C60 H60 125.0 . . ?

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
N6 Ni1 N1 C2 -95.92(16) . . . . ?
N6 Ni1 N1 C2 84.08(16) 2_665 . . . ?
N1 Ni1 N1 C2 52(100) 2_665 . . . ?
N11 Ni1 N1 C2 173.57(16) 2_665 . . . ?
N11 Ni1 N1 C2 -6.43(16) . . . . ?
N6 Ni1 N1 C5 83.10(18) . . . . ?
N6 Ni1 N1 C5 -96.90(18) 2_665 . . . ?
N1 Ni1 N1 C5 -129(100) 2_665 . . . ?
N11 Ni1 N1 C5 -7.42(18) 2_665 . . . ?
N11 Ni1 N1 C5 172.58(18) . . . . ?
C5 N1 C2 N3 0.3(2) . . . . ?
Ni1 N1 C2 N3 179.52(13) . . . . ?
N1 C2 N3 C4 -0.7(3) . . . . ?
C2 N3 C4 C5 0.9(3) . . . . ?
N3 C4 C5 N1 -0.7(3) . . . . ?
C2 N1 C5 C4 0.3(2) . . . . ?
Ni1 N1 C5 C4 -178.90(15) . . . . ?
N6 Ni1 N6 C7 -47(100) 2_665 . . . ?
N1 Ni1 N6 C7 174.12(17) 2_665 . . . ?
N1 Ni1 N6 C7 -5.88(17) . . . . ?
N11 Ni1 N6 C7 84.23(17) 2_665 . . . ?
N11 Ni1 N6 C7 -95.77(17) . . . . ?
N6 Ni1 N6 C10 132(100) 2_665 . . . ?
N1 Ni1 N6 C10 -7.03(18) 2_665 . . . ?
N1 Ni1 N6 C10 172.97(18) . . . . ?
N11 Ni1 N6 C10 -96.92(18) 2_665 . . . ?
N11 Ni1 N6 C10 83.08(18) . . . . ?
C10 N6 C7 N8 -0.1(2) . . . . ?
Ni1 N6 C7 N8 178.98(13) . . . . ?
N6 C7 N8 C9 0.0(3) . . . . ?
C7 N8 C9 C10 0.0(3) . . . . ?
N8 C9 C10 N6 -0.1(3) . . . . ?
C7 N6 C10 C9 0.1(3) . . . . ?
Ni1 N6 C10 C9 -178.96(17) . . . . ?
N6 Ni1 N11 C12 13.71(15) . . . . ?
N6 Ni1 N11 C12 -166.29(15) 2_665 . . . ?
N1 Ni1 N11 C12 103.95(15) 2_665 . . . ?
N1 Ni1 N11 C12 -76.05(15) . . . . ?
N11 Ni1 N11 C12 -163(100) 2_665 . . . ?
N6 Ni1 N11 C15 -163.98(18) . . . . ?
N6 Ni1 N11 C15 16.02(18) 2_665 . . . ?
N1 Ni1 N11 C15 -73.75(18) 2_665 . . . ?
N1 Ni1 N11 C15 106.25(18) . . . . ?
N11 Ni1 N11 C15 19(100) 2_665 . . . ?
C15 N11 C12 N13 0.2(2) . . . . ?
Ni1 N11 C12 N13 -178.00(12) . . . . ?
N11 C12 N13 C14 0.4(2) . . . . ?
C12 N13 C14 C15 -0.8(2) . . . . ?
N13 C14 C15 N11 0.9(3) . . . . ?
C12 N11 C15 C14 -0.7(2) . . . . ?
Ni1 N11 C15 C14 177.38(14) . . . . ?
N16 Ni2 N16 C17 41(100) 2_775 . . . ?
N21 Ni2 N16 C17 -83.76(16) . . . . ?
N21 Ni2 N16 C17 96.24(16) 2_775 . . . ?
N26 Ni2 N16 C17 -172.74(16) 2_775 . . . ?
N26 Ni2 N16 C17 7.26(16) . . . . ?
N16 Ni2 N16 C20 -142(100) 2_775 . . . ?
N21 Ni2 N16 C20 93.3(2) . . . . ?
N21 Ni2 N16 C20 -86.7(2) 2_775 . . . ?
N26 Ni2 N16 C20 4.3(2) 2_775 . . . ?
N26 Ni2 N16 C20 -175.7(2) . . . . ?
C20 N16 C17 N18 -0.1(2) . . . . ?
Ni2 N16 C17 N18 177.51(14) . . . . ?
N16 C17 N18 C19 0.1(3) . . . . ?
C17 N18 C19 C20 -0.1(3) . . . . ?
N18 C19 C20 N16 0.0(3) . . . . ?
C17 N16 C20 C19 0.0(3) . . . . ?
Ni2 N16 C20 C19 -177.49(19) . . . . ?
N16 Ni2 N21 C22 -174.43(17) 2_775 . . . ?
N16 Ni2 N21 C22 5.57(17) . . . . ?
N21 Ni2 N21 C22 -99.88(19) 2_775 . . . ?
N26 Ni2 N21 C22 94.93(17) 2_775 . . . ?
N26 Ni2 N21 C22 -85.07(17) . . . . ?
N16 Ni2 N21 C25 9.59(19) 2_775 . . . ?
N16 Ni2 N21 C25 -170.41(19) . . . . ?
N21 Ni2 N21 C25 84.14(19) 2_775 . . . ?
N26 Ni2 N21 C25 -81.06(18) 2_775 . . . ?
N26 Ni2 N21 C25 98.94(18) . . . . ?
C25 N21 C22 N23 0.0(2) . . . . ?
Ni2 N21 C22 N23 -176.75(13) . . . . ?
N21 C22 N23 C24 0.2(3) . . . . ?
C22 N23 C24 C25 -0.2(3) . . . . ?
N23 C24 C25 N21 0.2(3) . . . . ?
C22 N21 C25 C24 -0.1(3) . . . . ?
Ni2 N21 C25 C24 176.59(16) . . . . ?
N16 Ni2 N26 C27 94.58(16) 2_775 . . . ?
N16 Ni2 N26 C27 -85.42(16) . . . . ?
N21 Ni2 N26 C27 4.42(17) . . . . ?
N21 Ni2 N26 C27 -175.58(17) 2_775 . . . ?
N26 Ni2 N26 C27 163(100) 2_775 . . . ?
N16 Ni2 N26 C30 -81.46(19) 2_775 . . . ?
N16 Ni2 N26 C30 98.54(19) . . . . ?
N21 Ni2 N26 C30 -171.61(19) . . . . ?
N21 Ni2 N26 C30 8.39(19) 2_775 . . . ?
N26 Ni2 N26 C30 -13(100) 2_775 . . . ?
C30 N26 C27 N28 0.5(2) . . . . ?
Ni2 N26 C27 N28 -176.34(13) . . . . ?
N26 C27 N28 C29 -0.1(3) . . . . ?
C27 N28 C29 C30 -0.4(3) . . . . ?
N28 C29 C30 N26 0.7(3) . . . . ?
C27 N26 C30 C29 -0.7(3) . . . . ?
Ni2 N26 C30 C29 176.00(16) . . . . ?
N41 Ni3 N61 C62 138.76(10) . . . . ?
N31 Ni3 N61 C62 1.2(3) . . . . ?
O4 Ni3 N61 C62 47.61(10) . . . . ?
N36 Ni3 N61 C62 -130.31(10) . . . . ?
O1 Ni3 N61 C62 -39.90(10) . . . . ?
Ni3 N61 C62 C63 179.41(12) . . . . ?
Ni3 N61 C62 P1 59.54(10) . . . . ?
Ni3 N61 C62 P2 -57.51(10) . . . . ?
N61 C62 P1 O3 175.28(10) . . . . ?
C63 C62 P1 O3 53.44(15) . . . . ?
P2 C62 P1 O3 -73.47(11) . . . . ?
N61 C62 P1 O1 -56.58(12) . . . . ?
C63 C62 P1 O1 -178.42(13) . . . . ?
P2 C62 P1 O1 54.66(10) . . . . ?
N61 C62 P1 O2 56.29(12) . . . . ?
C63 C62 P1 O2 -65.55(14) . . . . ?
P2 C62 P1 O2 167.53(9) . . . . ?
O3 P1 O1 Ni3 149.51(7) . . . . ?
O2 P1 O1 Ni3 -84.26(8) . . . . ?
C62 P1 O1 Ni3 24.24(9) . . . . ?
N41 Ni3 O1 P1 -17.5(10) . . . . ?
N31 Ni3 O1 P1 -166.94(8) . . . . ?
O4 Ni3 O1 P1 -76.85(8) . . . . ?
N36 Ni3 O1 P1 100.90(8) . . . . ?
N61 Ni3 O1 P1 4.96(8) . . . . ?
N61 C62 P2 O6 163.55(10) . . . . ?
C63 C62 P2 O6 -72.34(14) . . . . ?
P1 C62 P2 O6 53.90(11) . . . . ?
N61 C62 P2 O4 40.18(12) . . . . ?
C63 C62 P2 O4 164.28(13) . . . . ?
P1 C62 P2 O4 -69.48(10) . . . . ?
N61 C62 P2 O5 -75.39(12) . . . . ?
C63 C62 P2 O5 48.71(14) . . . . ?
P1 C62 P2 O5 174.95(8) . . . . ?
O6 P2 O4 Ni3 -123.40(8) . . . . ?
O5 P2 O4 Ni3 110.03(8) . . . . ?
C62 P2 O4 Ni3 -1.90(9) . . . . ?
N41 Ni3 O4 P2 -116.97(8) . . . . ?
N31 Ni3 O4 P2 147.46(8) . . . . ?
N36 Ni3 O4 P2 16.1(10) . . . . ?
O1 Ni3 O4 P2 60.01(8) . . . . ?
N61 Ni3 O4 P2 -23.62(8) . . . . ?
N41 Ni3 N31 C32 -161.79(15) . . . . ?
O4 Ni3 N31 C32 -70.13(15) . . . . ?
N36 Ni3 N31 C32 107.44(15) . . . . ?
O1 Ni3 N31 C32 16.42(15) . . . . ?
N61 Ni3 N31 C32 -24.4(4) . . . . ?
N41 Ni3 N31 C35 26.94(18) . . . . ?
O4 Ni3 N31 C35 118.60(17) . . . . ?
N36 Ni3 N31 C35 -63.83(18) . . . . ?
O1 Ni3 N31 C35 -154.85(17) . . . . ?
N61 Ni3 N31 C35 164.3(2) . . . . ?
C35 N31 C32 N33 0.6(2) . . . . ?
Ni3 N31 C32 N33 -172.58(13) . . . . ?
N31 C32 N33 C34 -0.3(2) . . . . ?
C32 N33 C34 C35 -0.2(2) . . . . ?
N33 C34 C35 N31 0.5(3) . . . . ?
C32 N31 C35 C34 -0.7(2) . . . . ?
Ni3 N31 C35 C34 171.76(14) . . . . ?
N41 Ni3 N36 C37 161.79(19) . . . . ?
N31 Ni3 N36 C37 -102.61(19) . . . . ?
O4 Ni3 N36 C37 28.7(11) . . . . ?
O1 Ni3 N36 C37 -15.12(19) . . . . ?
N61 Ni3 N36 C37 68.16(19) . . . . ?
N41 Ni3 N36 C40 -45.75(17) . . . . ?
N31 Ni3 N36 C40 49.84(17) . . . . ?
O4 Ni3 N36 C40 -179(100) . . . . ?
O1 Ni3 N36 C40 137.33(17) . . . . ?
N61 Ni3 N36 C40 -139.39(17) . . . . ?
C40 N36 C37 N38 -1.0(2) . . . . ?
Ni3 N36 C37 N38 155.61(15) . . . . ?
N36 C37 N38 C39 0.4(3) . . . . ?
C37 N38 C39 C40 0.4(3) . . . . ?
N38 C39 C40 N36 -1.1(3) . . . . ?
C37 N36 C40 C39 1.3(3) . . . . ?
Ni3 N36 C40 C39 -156.59(16) . . . . ?
N31 Ni3 N41 C42 -132.76(17) . . . . ?
O4 Ni3 N41 C42 137.15(17) . . . . ?
N36 Ni3 N41 C42 -40.49(17) . . . . ?
O1 Ni3 N41 C42 78.0(10) . . . . ?
N61 Ni3 N41 C42 55.59(17) . . . . ?
N31 Ni3 N41 C45 54.99(18) . . . . ?
O4 Ni3 N41 C45 -35.10(17) . . . . ?
N36 Ni3 N41 C45 147.26(17) . . . . ?
O1 Ni3 N41 C45 -94.3(9) . . . . ?
N61 Ni3 N41 C45 -116.66(17) . . . . ?
C45 N41 C42 N43 -0.3(2) . . . . ?
Ni3 N41 C42 N43 -173.91(14) . . . . ?
N41 C42 N43 C44 0.6(3) . . . . ?
C42 N43 C44 C45 -0.7(3) . . . . ?
N43 C44 C45 N41 0.5(3) . . . . ?
C42 N41 C45 C44 -0.1(3) . . . . ?
Ni3 N41 C45 C44 173.56(16) . . . . ?
N56 Ni4 N64 C65 130.35(10) . . . . ?
N51 Ni4 N64 C65 -136.32(10) . . . . ?
O7 Ni4 N64 C65 -45.13(10) . . . . ?
N46 Ni4 N64 C65 10.9(3) . . . . ?
O10 Ni4 N64 C65 41.91(10) . . . . ?
Ni4 N64 C65 C66 179.14(13) . . . . ?
Ni4 N64 C65 P4 -58.40(10) . . . . ?
Ni4 N64 C65 P3 58.98(10) . . . . ?
N64 C65 P3 O9 -168.37(10) . . . . ?
C66 C65 P3 O9 69.53(14) . . . . ?
P4 C65 P3 O9 -57.13(11) . . . . ?
N64 C65 P3 O8 69.18(12) . . . . ?
C66 C65 P3 O8 -52.93(15) . . . . ?
P4 C65 P3 O8 -179.58(9) . . . . ?
N64 C65 P3 O7 -47.90(12) . . . . ?
C66 C65 P3 O7 -170.00(13) . . . . ?
P4 C65 P3 O7 63.34(10) . . . . ?
O9 P3 O7 Ni4 129.63(8) . . . . ?
O8 P3 O7 Ni4 -101.82(8) . . . . ?
C65 P3 O7 Ni4 11.48(9) . . . . ?
N56 Ni4 O7 P3 -41.3(6) . . . . ?
N51 Ni4 O7 P3 111.17(8) . . . . ?
N46 Ni4 O7 P3 -152.78(8) . . . . ?
O10 Ni4 O7 P3 -67.62(8) . . . . ?
N64 Ni4 O7 P3 15.92(8) . . . . ?
N64 C65 P4 O12 178.14(10) . . . . ?
C66 C65 P4 O12 -58.52(15) . . . . ?
P3 C65 P4 O12 67.30(11) . . . . ?
N64 C65 P4 O10 51.21(12) . . . . ?
C66 C65 P4 O10 174.55(13) . . . . ?
P3 C65 P4 O10 -59.62(10) . . . . ?
N64 C65 P4 O11 -62.93(12) . . . . ?
C66 C65 P4 O11 60.41(15) . . . . ?
P3 C65 P4 O11 -173.77(9) . . . . ?
O12 P4 O10 Ni4 -140.15(7) . . . . ?
O11 P4 O10 Ni4 93.56(9) . . . . ?
C65 P4 O10 Ni4 -16.49(9) . . . . ?
N56 Ni4 O10 P4 -105.69(8) . . . . ?
N51 Ni4 O10 P4 39.8(14) . . . . ?
O7 Ni4 O10 P4 71.94(8) . . . . ?
N46 Ni4 O10 P4 161.72(9) . . . . ?
N64 Ni4 O10 P4 -11.25(8) . . . . ?
N56 Ni4 N46 C47 -130.99(14) . . . . ?
N51 Ni4 N46 C47 135.82(14) . . . . ?
O7 Ni4 N46 C47 44.01(14) . . . . ?
O10 Ni4 N46 C47 -42.24(14) . . . . ?
N64 Ni4 N46 C47 -11.3(3) . . . . ?
N56 Ni4 N46 C50 41.02(18) . . . . ?
N51 Ni4 N46 C50 -52.16(18) . . . . ?
O7 Ni4 N46 C50 -143.97(18) . . . . ?
O10 Ni4 N46 C50 129.78(18) . . . . ?
N64 Ni4 N46 C50 160.7(2) . . . . ?
C50 N46 C47 N48 -0.1(2) . . . . ?
Ni4 N46 C47 N48 174.00(12) . . . . ?
N46 C47 N48 C49 0.3(2) . . . . ?
C47 N48 C49 C50 -0.4(2) . . . . ?
N48 C49 C50 N46 0.4(2) . . . . ?
C47 N46 C50 C49 -0.2(2) . . . . ?
Ni4 N46 C50 C49 -173.07(14) . . . . ?
N56 Ni4 N51 C52 85.80(16) . . . . ?
O7 Ni4 N51 C52 -91.72(16) . . . . ?
N46 Ni4 N51 C52 178.62(16) . . . . ?
O10 Ni4 N51 C52 -59.6(14) . . . . ?
N64 Ni4 N51 C52 -8.78(16) . . . . ?
N56 Ni4 N51 C55 -96.48(18) . . . . ?
O7 Ni4 N51 C55 86.00(18) . . . . ?
N46 Ni4 N51 C55 -3.66(19) . . . . ?
O10 Ni4 N51 C55 118.1(14) . . . . ?
N64 Ni4 N51 C55 168.94(18) . . . . ?
C55 N51 C52 N53 -0.1(2) . . . . ?
Ni4 N51 C52 N53 178.08(13) . . . . ?
N51 C52 N53 C54 0.2(3) . . . . ?
C52 N53 C54 C55 -0.1(3) . . . . ?
N53 C54 C55 N51 0.0(3) . . . . ?
C52 N51 C55 C54 0.1(2) . . . . ?
Ni4 N51 C55 C54 -178.00(15) . . . . ?
N51 Ni4 N56 C57 -174.26(16) . . . . ?
O7 Ni4 N56 C57 -21.8(7) . . . . ?
N46 Ni4 N56 C57 89.53(17) . . . . ?
O10 Ni4 N56 C57 4.45(16) . . . . ?
N64 Ni4 N56 C57 -78.58(17) . . . . ?
N51 Ni4 N56 C60 27.99(17) . . . . ?
O7 Ni4 N56 C60 -180(100) . . . . ?
N46 Ni4 N56 C60 -68.21(17) . . . . ?
O10 Ni4 N56 C60 -153.29(17) . . . . ?
N64 Ni4 N56 C60 123.67(17) . . . . ?
C60 N56 C57 N58 0.6(2) . . . . ?
Ni4 N56 C57 N58 -160.86(13) . . . . ?
N56 C57 N58 C59 0.2(2) . . . . ?
C57 N58 C59 C60 -0.9(3) . . . . ?
N58 C59 C60 N56 1.3(3) . . . . ?
C57 N56 C60 C59 -1.2(3) . . . . ?
Ni4 N56 C60 C59 160.40(16) . . . . ?

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
O11 H99 O3 0.72(3) 1.85(3) 2.564(2) 174(3) 1_455
O2 H98 O12 0.74(3) 1.78(3) 2.5193(19) 172(3) 1_655
N58 H58 O1 0.84(3) 2.00(3) 2.745(2) 147(3) .
N53 H53 O6 0.88(2) 1.82(2) 2.693(2) 171(2) 2_766
N48 H48 O5 0.88(3) 1.85(3) 2.705(2) 162(2) 2_776
N43 H43 O12 0.85(3) 2.45(3) 2.973(3) 121(2) 2_676
N43 H43 O9 0.85(3) 2.02(3) 2.768(2) 147(2) 2_676
N38 H38 N46 0.94(3) 2.68(3) 3.570(3) 159(2) .
N38 H38 O10 0.94(3) 2.25(3) 2.925(2) 128(2) .
N33 H33 O8 0.97(3) 1.81(3) 2.770(2) 179(3) 2_666
N28 H28 O7 0.82(3) 1.83(3) 2.651(2) 178(3) .
N23 H23 O9 0.83(2) 1.83(3) 2.652(2) 175(3) 1_655
N18 H18 O5 0.76(3) 2.08(3) 2.801(2) 159(3) 2_776
N13 H13 O4 0.85(3) 1.86(3) 2.703(2) 172(2) 2_666
N8 H8 O5 0.88(2) 1.87(3) 2.741(2) 171(2) 2_766
N3 H3 O8 0.72(3) 1.99(3) 2.687(2) 163(3) .

_diffrn_measured_fraction_theta_max 0.970
_diffrn_reflns_theta_full        27.50
_diffrn_measured_fraction_theta_full 0.970
_refine_diff_density_max         0.434
_refine_diff_density_min         -0.286
_refine_diff_density_rms         0.054

# Attachment 'S-7.cif'

data_60725lm1_0m
_database_code_depnum_ccdc_archive 'CCDC 660452'
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C21 H37 N14 Ni O8 P'
_chemical_formula_weight         703.33

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'
P P 0.1023 0.0942 '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           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                   9.0080(4)
_cell_length_b                   16.1663(8)
_cell_length_c                   22.6665(11)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.0390(10)
_cell_angle_gamma                90.00
_cell_volume                     3300.8(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    9091
_cell_measurement_theta_min      2.19
_cell_measurement_theta_max      29.82

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.22
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.415
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1472
_exptl_absorpt_coefficient_mu    0.700
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.7209
_exptl_absorpt_correction_T_max  0.8612
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      293(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            21931
_diffrn_reflns_av_R_equivalents  0.0191
_diffrn_reflns_av_sigmaI/netI    0.0209
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         2.19
_diffrn_reflns_theta_max         28.00
_reflns_number_total             7978
_reflns_number_gt                6287
_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 F² against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F², conventional R-factors R are based
on F, with F set to zero for negative F². The threshold expression of
F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F² 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/[σ²(Fo²)+(0.0470P)²+0.3213P] where P=(Fo²+2Fc²)/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     SHELXL
_refine_ls_extinction_coef       0.0012(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         7978
_refine_ls_number_parameters     474
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0398
_refine_ls_R_factor_gt           0.0293
_refine_ls_wR_factor_ref         0.0873
_refine_ls_wR_factor_gt          0.0832
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_restrained_S_all      1.066
_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 0.5000 0.5000 0.0000 0.02364(7) Uani 1 2 d S . .
N1 N 0.39596(12) 0.59418(7) 0.05052(5) 0.0296(2) Uani 1 1 d . . .
C2 C 0.30509(15) 0.58389(9) 0.09564(6) 0.0357(3) Uani 1 1 d . . .
H2 H 0.2846 0.5329 0.1129 0.043 Uiso 1 1 calc R . .
N3 N 0.24630(15) 0.65519(8) 0.11347(6) 0.0424(3) Uani 1 1 d . . .
H3 H 0.1769(19) 0.6603(10) 0.1364(8) 0.051(5) Uiso 1 1 d . . .
C4 C 0.30202(19) 0.71561(10) 0.07842(7) 0.0510(4) Uani 1 1 d . . .
H4 H 0.2808 0.7718 0.0804 0.061 Uiso 1 1 calc R . .
C5 C 0.39443(17) 0.67787(8) 0.04008(7) 0.0416(3) Uani 1 1 d . . .
H5 H 0.4490 0.7046 0.0109 0.050 Uiso 1 1 calc R . .
N6 N 0.39875(12) 0.40747(6) 0.05324(5) 0.0292(2) Uani 1 1 d . . .
C7 C 0.45559(15) 0.37373(8) 0.10108(6) 0.0361(3) Uani 1 1 d . . .
H7 H 0.5461 0.3892 0.1174 0.043 Uiso 1 1 calc R . .
N8 N 0.36841(14) 0.31480(8) 0.12336(6) 0.0415(3) Uani 1 1 d . . .
H8 H 0.3812(19) 0.2855(11) 0.1543(8) 0.059(5) Uiso 1 1 d . . .
C9 C 0.2472(2) 0.31037(11) 0.08824(8) 0.0565(5) Uani 1 1 d . . .
H9 H 0.1665 0.2751 0.0927 0.068 Uiso 1 1 calc R . .
C10 C 0.26657(17) 0.36760(10) 0.04514(7) 0.0459(4) Uani 1 1 d . . .
H10 H 0.1999 0.3781 0.0147 0.055 Uiso 1 1 calc R . .
N11 N 0.68725(13) 0.50395(6) 0.05720(5) 0.0292(2) Uani 1 1 d . . .
C12 C 0.71353(15) 0.56066(8) 0.09765(6) 0.0345(3) Uani 1 1 d . . .
H12 H 0.6447 0.6000 0.1097 0.041 Uiso 1 1 calc R . .
N13 N 0.85136(14) 0.55466(8) 0.11914(6) 0.0420(3) Uani 1 1 d . . .
H13 H 0.8937(19) 0.5893(11) 0.1414(8) 0.055(5) Uiso 1 1 d . . .
C14 C 0.91801(19) 0.49017(11) 0.09169(9) 0.0520(4) Uani 1 1 d . . .
H14 H 1.0141 0.4710 0.0979 0.062 Uiso 1 1 calc R . .
C15 C 0.81643(15) 0.45914(10) 0.05334(7) 0.0421(3) Uani 1 1 d . . .
H15 H 0.8319 0.4144 0.0283 0.050 Uiso 1 1 calc R . .
Ni2 Ni 0.0000 1.0000 0.0000 0.02349(7) Uani 1 2 d S . .
N16 N 0.19397(13) 1.00167(6) 0.05300(5) 0.0298(2) Uani 1 1 d . . .
C17 C 0.21662(16) 1.04607(9) 0.10096(6) 0.0372(3) Uani 1 1 d . . .
H17 H 0.1473 1.0823 0.1170 0.045 Uiso 1 1 calc R . .
N18 N 0.35097(14) 1.03276(9) 0.12369(6) 0.0440(3) Uani 1 1 d . . .
H18 H 0.387(2) 1.0539(12) 0.1554(9) 0.068(6) Uiso 1 1 d . . .
C19 C 0.41934(18) 0.97629(12) 0.08897(8) 0.0548(4) Uani 1 1 d . . .
H19 H 0.5142 0.9547 0.0941 0.066 Uiso 1 1 calc R . .
C20 C 0.32263(16) 0.95739(10) 0.04544(7) 0.0433(3) Uani 1 1 d . . .
H20 H 0.3405 0.9201 0.0150 0.052 Uiso 1 1 calc R . .
N21 N -0.09400(12) 1.09573(6) 0.05241(5) 0.0288(2) Uani 1 1 d . . .
C22 C -0.17494(16) 1.08649(9) 0.10040(6) 0.0370(3) Uani 1 1 d . . .
H22 H -0.2006 1.0354 0.1163 0.044 Uiso 1 1 calc R . .
N23 N -0.21574(14) 1.15889(8) 0.12341(6) 0.0428(3) Uani 1 1 d . . .
H23 H -0.268(2) 1.1663(13) 0.1560(10) 0.088(7) Uiso 1 1 d . . .
C24 C -0.1584(2) 1.21882(10) 0.08853(8) 0.0532(4) Uani 1 1 d . . .
H24 H -0.1685 1.2756 0.0935 0.064 Uiso 1 1 calc R . .
C25 C -0.08360(18) 1.17969(8) 0.04502(7) 0.0440(4) Uani 1 1 d . . .
H25 H -0.0327 1.2058 0.0146 0.053 Uiso 1 1 calc R . .
N26 N -0.09288(12) 0.90787(6) 0.05604(5) 0.0296(2) Uani 1 1 d . . .
C27 C -0.02425(16) 0.86656(8) 0.09840(6) 0.0351(3) Uani 1 1 d . . .
H27 H 0.0694 0.8799 0.1129 0.042 Uiso 1 1 calc R . .
N28 N -0.10606(15) 0.80333(8) 0.11780(6) 0.0428(3) Uani 1 1 d . . .
H28 H -0.078(2) 0.7683(11) 0.1417(8) 0.060(6) Uiso 1 1 d . . .
C29 C -0.23536(19) 0.80365(10) 0.08719(8) 0.0521(4) Uani 1 1 d . . .
H29 H -0.3142 0.7670 0.0915 0.063 Uiso 1 1 calc R . .
C30 C -0.22663(16) 0.86815(9) 0.04906(7) 0.0423(3) Uani 1 1 d . . .
H30 H -0.3000 0.8832 0.0223 0.051 Uiso 1 1 calc R . .
N31 N 0.70799(15) 0.98217(8) 0.24132(6) 0.0425(3) Uani 1 1 d . . .
H31 H 0.635(2) 1.0210(12) 0.2346(8) 0.056(5) Uiso 1 1 d . . .
C32 C 0.68865(17) 0.90298(9) 0.25268(8) 0.0481(4) Uani 1 1 d . . .
H32 H 0.5971 0.8765 0.2545 0.058 Uiso 1 1 calc R . .
N33 N 0.81758(14) 0.86677(8) 0.26104(6) 0.0443(3) Uani 1 1 d . . .
H33 H 0.834(2) 0.8097(13) 0.2683(8) 0.073(6) Uiso 1 1 d . . .
C34 C 0.92428(17) 0.92507(10) 0.25429(7) 0.0487(4) Uani 1 1 d . . .
H34 H 1.0262 0.9168 0.2573 0.058 Uiso 1 1 calc R . .
C35 C 0.85576(18) 0.99696(9) 0.24242(8) 0.0479(4) Uani 1 1 d . . .
H35 H 0.9016 1.0477 0.2361 0.058 Uiso 1 1 calc R . .
P1 P 0.50445(3) 0.173503(18) 0.247407(12) 0.02155(8) Uani 1 1 d . . .
O1 O 0.50361(9) 0.17305(5) 0.31461(4) 0.0322(2) Uani 1 1 d . . .
O2 O 0.49197(9) 0.08406(5) 0.22440(4) 0.0336(2) Uani 1 1 d . . .
O3 O 0.37544(10) 0.22451(6) 0.22374(4) 0.0374(2) Uani 1 1 d . . .
O4 O 0.65310(10) 0.20920(6) 0.22526(4) 0.0396(2) Uani 1 1 d . . .
O1W O 0.12700(14) 0.12289(10) 0.23464(7) 0.0655(4) Uani 1 1 d . . .
H1W1 H 0.194(2) 0.1599(13) 0.2267(9) 0.068(6) Uiso 1 1 d . . .
H2W1 H 0.169(4) 0.078(2) 0.2468(15) 0.163(15) Uiso 1 1 d . . .
O2W O 0.29780(19) 0.97947(11) 0.28401(8) 0.0758(5) Uani 1 1 d . . .
H1W2 H 0.291(3) 0.9393(16) 0.2638(11) 0.088(9) Uiso 1 1 d . . .
H2W2 H 0.365(3) 1.0091(13) 0.2674(10) 0.070(7) Uiso 1 1 d . . .
O3W O 0.9192(2) 0.21439(10) 0.29959(7) 0.0759(4) Uani 1 1 d . . .
H1W3 H 0.979(3) 0.1877(17) 0.2804(13) 0.106(9) Uiso 1 1 d . . .
H2W3 H 0.837(3) 0.2073(15) 0.2801(11) 0.088(8) Uiso 1 1 d . . .
O4W O 0.2016(3) 0.33215(10) 0.28672(9) 0.0919(6) Uani 1 1 d . . .
H1W4 H 0.253(3) 0.3007(16) 0.2683(11) 0.088(8) Uiso 1 1 d . . .
H2W4 H 0.137(4) 0.3054(19) 0.2937(15) 0.134(14) Uiso 1 1 d . . .


_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 N1 2.1235(10) 3_665 ?
Ni1 N1 2.1235(10) . ?
Ni1 N6 2.1277(10) . ?
Ni1 N6 2.1277(10) 3_665 ?
Ni1 N11 2.1278(11) 3_665 ?
Ni1 N11 2.1278(11) . ?
N1 C2 1.3208(16) . ?
N1 C5 1.3736(17) . ?
C2 N3 1.3314(18) . ?
C2 H2 0.9300 . ?
N3 C4 1.356(2) . ?
N3 H3 0.817(18) . ?
C4 C5 1.350(2) . ?
C4 H4 0.9300 . ?
C5 H5 0.9300 . ?
N6 C7 1.3171(17) . ?
N6 C10 1.3662(18) . ?
C7 N8 1.3342(17) . ?
C7 H7 0.9300 . ?
N8 C9 1.353(2) . ?
N8 H8 0.855(19) . ?
C9 C10 1.357(2) . ?
C9 H9 0.9300 . ?
C10 H10 0.9300 . ?
N11 C12 1.3179(17) . ?
N11 C15 1.3735(17) . ?
C12 N13 1.3370(18) . ?
C12 H12 0.9300 . ?
N13 C14 1.355(2) . ?
N13 H13 0.845(18) . ?
C14 C15 1.358(2) . ?
C14 H14 0.9300 . ?
C15 H15 0.9300 . ?
Ni2 N16 2.1199(11) 3_575 ?
Ni2 N16 2.1199(11) . ?
Ni2 N21 2.1271(10) 3_575 ?
Ni2 N21 2.1271(10) . ?
Ni2 N26 2.1292(10) . ?
Ni2 N26 2.1292(10) 3_575 ?
N16 C17 1.3185(17) . ?
N16 C20 1.3731(17) . ?
C17 N18 1.3325(18) . ?
C17 H17 0.9300 . ?
N18 C19 1.354(2) . ?
N18 H18 0.86(2) . ?
C19 C20 1.351(2) . ?
C19 H19 0.9300 . ?
C20 H20 0.9300 . ?
N21 C22 1.3185(16) . ?
N21 C25 1.3708(17) . ?
C22 N23 1.3332(17) . ?
C22 H22 0.9300 . ?
N23 C24 1.353(2) . ?
N23 H23 0.88(2) . ?
C24 C25 1.352(2) . ?
C24 H24 0.9300 . ?
C25 H25 0.9300 . ?
N26 C27 1.3227(17) . ?
N26 C30 1.3743(18) . ?
C27 N28 1.3348(18) . ?
C27 H27 0.9300 . ?
N28 C29 1.355(2) . ?
N28 H28 0.823(19) . ?
C29 C30 1.357(2) . ?
C29 H29 0.9300 . ?
C30 H30 0.9300 . ?
N31 C32 1.317(2) . ?
N31 C35 1.353(2) . ?
N31 H31 0.921(19) . ?
C32 N33 1.3142(19) . ?
C32 H32 0.9300 . ?
N33 C34 1.355(2) . ?
N33 H33 0.95(2) . ?
C34 C35 1.343(2) . ?
C34 H34 0.9300 . ?
C35 H35 0.9300 . ?
P1 O3 1.5222(9) . ?
P1 O1 1.5233(9) . ?
P1 O2 1.5412(9) . ?
P1 O4 1.5424(9) . ?
O1W H1W1 0.87(2) . ?
O1W H2W1 0.87(4) . ?
O2W H1W2 0.80(3) . ?
O2W H2W2 0.86(2) . ?
O3W H1W3 0.81(3) . ?
O3W H2W3 0.87(3) . ?
O4W H1W4 0.80(3) . ?
O4W H2W4 0.74(3) . ?

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
N1 Ni1 N1 180.00(5) 3_665 . ?
N1 Ni1 N6 89.50(4) 3_665 . ?
N1 Ni1 N6 90.50(4) . . ?
N1 Ni1 N6 90.50(4) 3_665 3_665 ?
N1 Ni1 N6 89.50(4) . 3_665 ?
N6 Ni1 N6 180.00(6) . 3_665 ?
N1 Ni1 N11 89.99(4) 3_665 3_665 ?
N1 Ni1 N11 90.01(4) . 3_665 ?
N6 Ni1 N11 89.12(4) . 3_665 ?
N6 Ni1 N11 90.88(4) 3_665 3_665 ?
N1 Ni1 N11 90.01(4) 3_665 . ?
N1 Ni1 N11 89.99(4) . . ?
N6 Ni1 N11 90.88(4) . . ?
N6 Ni1 N11 89.12(4) 3_665 . ?
N11 Ni1 N11 180.00(5) 3_665 . ?
C2 N1 C5 104.56(11) . . ?
C2 N1 Ni1 126.95(9) . . ?
C5 N1 Ni1 128.15(9) . . ?
N1 C2 N3 111.89(12) . . ?
N1 C2 H2 124.1 . . ?
N3 C2 H2 124.1 . . ?
C2 N3 C4 107.36(12) . . ?
C2 N3 H3 125.8(12) . . ?
C4 N3 H3 125.7(12) . . ?
C5 C4 N3 106.28(13) . . ?
C5 C4 H4 126.9 . . ?
N3 C4 H4 126.9 . . ?
C4 C5 N1 109.91(13) . . ?
C4 C5 H5 125.0 . . ?
N1 C5 H5 125.0 . . ?
C7 N6 C10 104.68(11) . . ?
C7 N6 Ni1 126.26(9) . . ?
C10 N6 Ni1 129.00(9) . . ?
N6 C7 N8 112.26(13) . . ?
N6 C7 H7 123.9 . . ?
N8 C7 H7 123.9 . . ?
C7 N8 C9 106.86(12) . . ?
C7 N8 H8 128.9(12) . . ?
C9 N8 H8 124.2(12) . . ?
N8 C9 C10 106.45(13) . . ?
N8 C9 H9 126.8 . . ?
C10 C9 H9 126.8 . . ?
C9 C10 N6 109.74(13) . . ?
C9 C10 H10 125.1 . . ?
N6 C10 H10 125.1 . . ?
C12 N11 C15 105.04(12) . . ?
C12 N11 Ni1 125.92(9) . . ?
C15 N11 Ni1 128.07(9) . . ?
N11 C12 N13 111.67(13) . . ?
N11 C12 H12 124.2 . . ?
N13 C12 H12 124.2 . . ?
C12 N13 C14 107.48(12) . . ?
C12 N13 H13 126.0(12) . . ?
C14 N13 H13 125.8(12) . . ?
N13 C14 C15 106.24(14) . . ?
N13 C14 H14 126.9 . . ?
C15 C14 H14 126.9 . . ?
C14 C15 N11 109.57(13) . . ?
C14 C15 H15 125.2 . . ?
N11 C15 H15 125.2 . . ?
N16 Ni2 N16 180.0 3_575 . ?
N16 Ni2 N21 90.14(4) 3_575 3_575 ?
N16 Ni2 N21 89.86(4) . 3_575 ?
N16 Ni2 N21 89.86(4) 3_575 . ?
N16 Ni2 N21 90.14(4) . . ?
N21 Ni2 N21 180.0 3_575 . ?
N16 Ni2 N26 90.29(4) 3_575 . ?
N16 Ni2 N26 89.71(4) . . ?
N21 Ni2 N26 88.91(4) 3_575 . ?
N21 Ni2 N26 91.09(4) . . ?
N16 Ni2 N26 89.71(4) 3_575 3_575 ?
N16 Ni2 N26 90.29(4) . 3_575 ?
N21 Ni2 N26 91.09(4) 3_575 3_575 ?
N21 Ni2 N26 88.91(4) . 3_575 ?
N26 Ni2 N26 180.00(5) . 3_575 ?
C17 N16 C20 104.87(12) . . ?
C17 N16 Ni2 126.96(9) . . ?
C20 N16 Ni2 128.17(9) . . ?
N16 C17 N18 111.77(13) . . ?
N16 C17 H17 124.1 . . ?
N18 C17 H17 124.1 . . ?
C17 N18 C19 107.31(13) . . ?
C17 N18 H18 127.0(13) . . ?
C19 N18 H18 125.6(13) . . ?
C20 C19 N18 106.48(14) . . ?
C20 C19 H19 126.8 . . ?
N18 C19 H19 126.8 . . ?
C19 C20 N16 109.57(13) . . ?
C19 C20 H20 125.2 . . ?
N16 C20 H20 125.2 . . ?
C22 N21 C25 104.53(11) . . ?
C22 N21 Ni2 126.79(9) . . ?
C25 N21 Ni2 128.68(9) . . ?
N21 C22 N23 112.09(12) . . ?
N21 C22 H22 124.0 . . ?
N23 C22 H22 124.0 . . ?
C22 N23 C24 107.13(12) . . ?
C22 N23 H23 126.4(14) . . ?
C24 N23 H23 126.4(14) . . ?
C25 C24 N23 106.37(13) . . ?
C25 C24 H24 126.8 . . ?
N23 C24 H24 126.8 . . ?
C24 C25 N21 109.88(13) . . ?
C24 C25 H25 125.1 . . ?
N21 C25 H25 125.1 . . ?
C27 N26 C30 104.89(11) . . ?
C27 N26 Ni2 127.06(9) . . ?
C30 N26 Ni2 127.08(9) . . ?
N26 C27 N28 111.59(13) . . ?
N26 C27 H27 124.2 . . ?
N28 C27 H27 124.2 . . ?
C27 N28 C29 107.63(13) . . ?
C27 N28 H28 125.1(13) . . ?
C29 N28 H28 127.0(13) . . ?
N28 C29 C30 106.20(14) . . ?
N28 C29 H29 126.9 . . ?
C30 C29 H29 126.9 . . ?
C29 C30 N26 109.69(14) . . ?
C29 C30 H30 125.2 . . ?
N26 C30 H30 125.2 . . ?
C32 N31 C35 107.37(13) . . ?
C32 N31 H31 126.9(12) . . ?
C35 N31 H31 125.7(12) . . ?
N33 C32 N31 110.12(14) . . ?
N33 C32 H32 124.9 . . ?
N31 C32 H32 124.9 . . ?
C32 N33 C34 107.50(13) . . ?
C32 N33 H33 126.8(12) . . ?
C34 N33 H33 125.6(12) . . ?
C35 C34 N33 107.37(13) . . ?
C35 C34 H34 126.3 . . ?
N33 C34 H34 126.3 . . ?
C34 C35 N31 107.63(13) . . ?
C34 C35 H35 126.2 . . ?
N31 C35 H35 126.2 . . ?
O3 P1 O1 110.53(5) . . ?
O3 P1 O2 109.48(5) . . ?
O1 P1 O2 109.47(5) . . ?
O3 P1 O4 110.20(6) . . ?
O1 P1 O4 109.40(5) . . ?
O2 P1 O4 107.70(5) . . ?
H1W1 O1W H2W1 110(2) . . ?
H1W2 O2W H2W2 105(2) . . ?
H1W3 O3W H2W3 103(2) . . ?
H1W4 O4W H2W4 101(3) . . ?

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
N1 Ni1 N1 C2 -179(100) 3_665 . . . ?
N6 Ni1 N1 C2 -0.81(12) . . . . ?
N6 Ni1 N1 C2 179.19(12) 3_665 . . . ?
N11 Ni1 N1 C2 88.31(11) 3_665 . . . ?
N11 Ni1 N1 C2 -91.69(11) . . . . ?
N1 Ni1 N1 C5 9(100) 3_665 . . . ?
N6 Ni1 N1 C5 -173.02(12) . . . . ?
N6 Ni1 N1 C5 6.98(12) 3_665 . . . ?
N11 Ni1 N1 C5 -83.91(12) 3_665 . . . ?
N11 Ni1 N1 C5 96.09(12) . . . . ?
C5 N1 C2 N3 0.62(16) . . . . ?
Ni1 N1 C2 N3 -173.06(9) . . . . ?
N1 C2 N3 C4 -0.31(18) . . . . ?
C2 N3 C4 C5 -0.15(19) . . . . ?
N3 C4 C5 N1 0.5(2) . . . . ?
C2 N1 C5 C4 -0.71(18) . . . . ?
Ni1 N1 C5 C4 172.87(11) . . . . ?
N1 Ni1 N6 C7 88.63(11) 3_665 . . . ?
N1 Ni1 N6 C7 -91.37(11) . . . . ?
N6 Ni1 N6 C7 -90(100) 3_665 . . . ?
N11 Ni1 N6 C7 178.63(11) 3_665 . . . ?
N11 Ni1 N6 C7 -1.37(11) . . . . ?
N1 Ni1 N6 C10 -88.50(13) 3_665 . . . ?
N1 Ni1 N6 C10 91.50(13) . . . . ?
N6 Ni1 N6 C10 93(100) 3_665 . . . ?
N11 Ni1 N6 C10 1.49(13) 3_665 . . . ?
N11 Ni1 N6 C10 -178.51(13) . . . . ?
C10 N6 C7 N8 0.49(17) . . . . ?
Ni1 N6 C7 N8 -177.21(9) . . . . ?
N6 C7 N8 C9 -0.50(18) . . . . ?
C7 N8 C9 C10 0.3(2) . . . . ?
N8 C9 C10 N6 0.0(2) . . . . ?
C7 N6 C10 C9 -0.29(19) . . . . ?
Ni1 N6 C10 C9 177.32(12) . . . . ?
N1 Ni1 N11 C12 168.93(11) 3_665 . . . ?
N1 Ni1 N11 C12 -11.07(11) . . . . ?
N6 Ni1 N11 C12 -101.57(11) . . . . ?
N6 Ni1 N11 C12 78.43(11) 3_665 . . . ?
N11 Ni1 N11 C12 33(100) 3_665 . . . ?
N1 Ni1 N11 C15 1.91(12) 3_665 . . . ?
N1 Ni1 N11 C15 -178.09(12) . . . . ?
N6 Ni1 N11 C15 91.41(12) . . . . ?
N6 Ni1 N11 C15 -88.59(12) 3_665 . . . ?
N11 Ni1 N11 C15 -134(100) 3_665 . . . ?
C15 N11 C12 N13 0.42(16) . . . . ?
Ni1 N11 C12 N13 -169.03(9) . . . . ?
N11 C12 N13 C14 -0.60(18) . . . . ?
C12 N13 C14 C15 0.52(19) . . . . ?
N13 C14 C15 N11 -0.3(2) . . . . ?
C12 N11 C15 C14 -0.08(18) . . . . ?
Ni1 N11 C15 C14 169.06(11) . . . . ?
N16 Ni2 N16 C17 138.86(13) 3_575 . . . ?
N21 Ni2 N16 C17 -175.51(12) 3_575 . . . ?
N21 Ni2 N16 C17 4.49(12) . . . . ?
N26 Ni2 N16 C17 -86.60(12) . . . . ?
N26 Ni2 N16 C17 93.40(12) 3_575 . . . ?
N16 Ni2 N16 C20 -41.26(13) 3_575 . . . ?
N21 Ni2 N16 C20 4.37(12) 3_575 . . . ?
N21 Ni2 N16 C20 -175.63(12) . . . . ?
N26 Ni2 N16 C20 93.28(12) . . . . ?
N26 Ni2 N16 C20 -86.72(12) 3_575 . . . ?
C20 N16 C17 N18 0.28(17) . . . . ?
Ni2 N16 C17 N18 -179.82(9) . . . . ?
N16 C17 N18 C19 -0.41(19) . . . . ?
C17 N18 C19 C20 0.4(2) . . . . ?
N18 C19 C20 N16 -0.2(2) . . . . ?
C17 N16 C20 C19 -0.04(19) . . . . ?
Ni2 N16 C20 C19 -179.94(12) . . . . ?
N16 Ni2 N21 C22 90.83(12) 3_575 . . . ?
N16 Ni2 N21 C22 -89.17(12) . . . . ?
N21 Ni2 N21 C22 -115(100) 3_575 . . . ?
N26 Ni2 N21 C22 0.54(12) . . . . ?
N26 Ni2 N21 C22 -179.46(12) 3_575 . . . ?
N16 Ni2 N21 C25 -90.10(13) 3_575 . . . ?
N16 Ni2 N21 C25 89.90(13) . . . . ?
N21 Ni2 N21 C25 64(100) 3_575 . . . ?
N26 Ni2 N21 C25 179.61(13) . . . . ?
N26 Ni2 N21 C25 -0.39(13) 3_575 . . . ?
C25 N21 C22 N23 0.03(17) . . . . ?
Ni2 N21 C22 N23 179.28(9) . . . . ?
N21 C22 N23 C24 0.03(18) . . . . ?
C22 N23 C24 C25 -0.1(2) . . . . ?
N23 C24 C25 N21 0.1(2) . . . . ?
C22 N21 C25 C24 -0.08(18) . . . . ?
Ni2 N21 C25 C24 -179.31(11) . . . . ?
N16 Ni2 N26 C27 170.28(11) 3_575 . . . ?
N16 Ni2 N26 C27 -9.72(11) . . . . ?
N21 Ni2 N26 C27 80.14(11) 3_575 . . . ?
N21 Ni2 N26 C27 -99.86(11) . . . . ?
N26 Ni2 N26 C27 -164(100) 3_575 . . . ?
N16 Ni2 N26 C30 3.26(11) 3_575 . . . ?
N16 Ni2 N26 C30 -176.74(11) . . . . ?
N21 Ni2 N26 C30 -86.87(11) 3_575 . . . ?
N21 Ni2 N26 C30 93.13(11) . . . . ?
N26 Ni2 N26 C30 29(100) 3_575 . . . ?
C30 N26 C27 N28 0.57(15) . . . . ?
Ni2 N26 C27 N28 -168.74(9) . . . . ?
N26 C27 N28 C29 -0.70(17) . . . . ?
C27 N28 C29 C30 0.52(19) . . . . ?
N28 C29 C30 N26 -0.18(19) . . . . ?
C27 N26 C30 C29 -0.23(17) . . . . ?
Ni2 N26 C30 C29 169.08(11) . . . . ?
C35 N31 C32 N33 0.1(2) . . . . ?
N31 C32 N33 C34 -0.51(19) . . . . ?
C32 N33 C34 C35 0.73(19) . . . . ?
N33 C34 C35 N31 -0.68(19) . . . . ?
C32 N31 C35 C34 0.37(19) . . . . ?

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
N3 H3 O1 0.817(18) 1.981(18) 2.7953(15) 174.7(18) 2
N8 H8 O3 0.855(19) 1.857(19) 2.7039(15) 170.4(17) .
N13 H13 O1 0.845(18) 1.918(18) 2.7608(15) 174.6(17) 2_655
N18 H18 O2 0.86(2) 1.89(2) 2.7400(16) 169.3(18) 1_565
N23 H23 O4 0.88(2) 1.86(2) 2.7185(15) 164(2) 1_465
N28 H28 O1 0.823(19) 1.949(19) 2.7627(16) 169.5(18) 2
N31 H31 O2 0.921(19) 1.66(2) 2.5779(15) 174.5(19) 1_565
N33 H33 O4 0.95(2) 1.64(2) 2.5797(15) 172.8(19) 2_655
O1W H1W1 O3 0.87(2) 1.94(2) 2.7872(17) 164(2) .
O1W H2W1 O2W 0.87(4) 2.14(4) 2.999(2) 170(3) 1_545
O2W H1W2 O4W 0.80(3) 2.08(3) 2.871(2) 174(2) 2
O2W H2W2 O2 0.86(2) 1.93(2) 2.7833(18) 172(2) 1_565
O3W H1W3 O1W 0.81(3) 1.99(3) 2.804(2) 179(3) 1_655
O3W H2W3 O4 0.87(3) 2.07(3) 2.930(2) 170(2) .
O4W H1W4 O3 0.80(3) 1.94(3) 2.7427(18) 179(3) .
O4W H2W4 O3W 0.74(3) 2.46(3) 3.190(3) 171(4) 1_455

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        28.00
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.255
_refine_diff_density_min         -0.301
_refine_diff_density_rms         0.043

# Attachment 'S-9.cif'

data_60725lm3_0m
_database_code_depnum_ccdc_archive 'CCDC 660453'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C32 H50 N21 Ni2 O9 P2'
_chemical_formula_weight         1052.29

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'
P P 0.1023 0.0942 '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           Triclinic
_symmetry_space_group_name_H-M   P-1

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.9153(10)
_cell_length_b                   12.8275(13)
_cell_length_c                   20.407(2)
_cell_angle_alpha                76.501(2)
_cell_angle_beta                 88.5390(10)
_cell_angle_gamma                68.800(2)
_cell_volume                     2348.1(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    273(2)
_cell_measurement_reflns_used    6506
_cell_measurement_theta_min      2.21
_cell_measurement_theta_max      29.39

_exptl_crystal_description       ?
_exptl_crystal_colour            ?
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.24
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.488
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1094
_exptl_absorpt_coefficient_mu    0.942
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.7462
_exptl_absorpt_correction_T_max  0.8054
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      273(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            15623
_diffrn_reflns_av_R_equivalents  0.0159
_diffrn_reflns_av_sigmaI/netI    0.0373
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         2.06
_diffrn_reflns_theta_max         28.00
_reflns_number_total             10907
_reflns_number_gt                8585
_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 F² against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F², conventional R-factors R are based
on F, with F set to zero for negative F². The threshold expression of
F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F² 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/[σ²(Fo²)+(0.0695P)²+0.2599P] where P=(Fo²+2Fc²)/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         10907
_refine_ls_number_parameters     676
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0505
_refine_ls_R_factor_gt           0.0376
_refine_ls_wR_factor_ref         0.1234
_refine_ls_wR_factor_gt          0.1166
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_restrained_S_all      1.100
_refine_ls_shift/su_max          0.000
_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
C1 C 0.2370(2) 0.58715(19) 0.22463(11) 0.0234(4) Uani 1 1 d . . .
C2 C 0.1231(3) 0.7063(2) 0.22412(12) 0.0325(5) Uani 1 1 d . . .
H2A H 0.1559 0.7398 0.2549 0.049 Uiso 1 1 calc R . .
H2B H 0.0331 0.6986 0.2377 0.049 Uiso 1 1 calc R . .
H2C H 0.1090 0.7552 0.1794 0.049 Uiso 1 1 calc R . .
C4 C 0.6303(3) 0.3979(2) 0.07112(12) 0.0382(6) Uani 1 1 d . . .
H4 H 0.6195 0.3280 0.0739 0.046 Uiso 1 1 calc R . .
C6 C 0.6794(4) 0.5513(3) 0.03202(14) 0.0459(7) Uani 1 1 d . . .
H6 H 0.7080 0.6073 0.0044 0.055 Uiso 1 1 calc R . .
C7 C 0.6277(3) 0.5524(2) 0.09385(13) 0.0382(6) Uani 1 1 d . . .
H7 H 0.6147 0.6104 0.1162 0.046 Uiso 1 1 calc R . .
C9 C 0.5488(3) 0.1675(2) 0.25293(14) 0.0403(6) Uani 1 1 d . . .
H9 H 0.4544 0.1902 0.2666 0.048 Uiso 1 1 calc R . .
C11 C 0.7626(5) 0.0591(3) 0.2342(2) 0.0707(11) Uani 1 1 d . . .
H11 H 0.8442 -0.0047 0.2316 0.085 Uiso 1 1 calc R . .
C12 C 0.7475(3) 0.1702(3) 0.21304(17) 0.0536(8) Uani 1 1 d . . .
H12 H 0.8187 0.1964 0.1935 0.064 Uiso 1 1 calc R . .
C14 C 0.8080(3) 0.4340(2) 0.24179(14) 0.0395(6) Uani 1 1 d . . .
H14 H 0.8438 0.4165 0.2015 0.047 Uiso 1 1 calc R . .
C16 C 0.7940(3) 0.4815(3) 0.33752(16) 0.0500(8) Uani 1 1 d . . .
H16 H 0.8156 0.5025 0.3754 0.060 Uiso 1 1 calc R . .
C17 C 0.6729(3) 0.4639(3) 0.32395(14) 0.0409(6) Uani 1 1 d . . .
H17 H 0.5955 0.4711 0.3515 0.049 Uiso 1 1 calc R . .
C19 C 0.7303(3) 0.1764(2) 0.40939(13) 0.0380(6) Uani 1 1 d . . .
H19 H 0.7893 0.2052 0.3804 0.046 Uiso 1 1 calc R . .
C21 C 0.5392(3) 0.1531(3) 0.45240(17) 0.0578(9) Uani 1 1 d . . .
H21 H 0.4436 0.1607 0.4600 0.069 Uiso 1 1 calc R . .
C22 C 0.6588(3) 0.0774(3) 0.49056(15) 0.0508(8) Uani 1 1 d . . .
H22 H 0.6586 0.0231 0.5297 0.061 Uiso 1 1 calc R . .
C24 C 1.1273(3) -0.2147(2) 0.44065(14) 0.0394(6) Uani 1 1 d . . .
H24 H 1.2165 -0.2364 0.4638 0.047 Uiso 1 1 calc R . .
C26 C 0.9591(4) -0.2166(3) 0.37678(17) 0.0558(8) Uani 1 1 d . . .
H26 H 0.9080 -0.2373 0.3477 0.067 Uiso 1 1 calc R . .
C27 C 0.9087(3) -0.1238(3) 0.40275(15) 0.0478(7) Uani 1 1 d . . .
H27 H 0.8151 -0.0690 0.3946 0.057 Uiso 1 1 calc R . .
C29 C 1.0917(3) 0.1974(2) 0.41733(14) 0.0396(6) Uani 1 1 d . . .
H29 H 1.0713 0.2346 0.4524 0.047 Uiso 1 1 calc R . .
C31 C 1.1599(4) 0.1600(3) 0.32162(17) 0.0634(10) Uani 1 1 d . . .
H31 H 1.1945 0.1640 0.2787 0.076 Uiso 1 1 calc R . .
C32 C 1.1132(4) 0.0783(3) 0.35718(15) 0.0545(8) Uani 1 1 d . . .
H32 H 1.1110 0.0154 0.3426 0.065 Uiso 1 1 calc R . .
C34 C 0.7510(3) 0.7742(2) 0.07485(13) 0.0355(6) Uani 1 1 d . . .
H34 H 0.7931 0.7629 0.0346 0.043 Uiso 1 1 calc R . .
C36 C 0.7159(3) 0.7498(3) 0.18160(14) 0.0468(7) Uani 1 1 d . . .
H36 H 0.7263 0.7206 0.2282 0.056 Uiso 1 1 calc R . .
C37 C 0.6061(3) 0.8436(3) 0.14646(14) 0.0440(7) Uani 1 1 d . . .
H37 H 0.5279 0.8906 0.1652 0.053 Uiso 1 1 calc R . .
C39 C 0.3296(3) 0.8383(3) 0.04358(15) 0.0456(7) Uani 1 1 d . . .
H39 H 0.3955 0.7976 0.0806 0.055 Uiso 1 1 calc R . .
C41 C 0.1503(4) 0.8873(3) -0.02721(18) 0.0582(9) Uani 1 1 d . . .
H41 H 0.0684 0.8900 -0.0497 0.070 Uiso 1 1 calc R . .
C42 C 0.2241(4) 0.9579(3) -0.04616(16) 0.0520(8) Uani 1 1 d . . .
H42 H 0.2006 1.0186 -0.0845 0.062 Uiso 1 1 calc R . .
C44 C 0.4142(3) 1.1714(2) 0.09200(14) 0.0405(6) Uani 1 1 d . . .
H44 H 0.4993 1.1855 0.0833 0.049 Uiso 1 1 calc R . .
C46 C 0.2055(4) 1.1850(4) 0.12850(18) 0.0652(10) Uani 1 1 d . . .
H46 H 0.1175 1.2087 0.1484 0.078 Uiso 1 1 calc R . .
C47 C 0.2541(4) 1.0981(3) 0.09681(17) 0.0569(9) Uani 1 1 d . . .
H47 H 0.2050 1.0503 0.0925 0.068 Uiso 1 1 calc R . .
C49 C 0.5677(4) 0.2472(4) 0.65599(18) 0.0649(10) Uani 1 1 d . . .
H49 H 0.6268 0.2870 0.6617 0.078 Uiso 1 1 calc R . .
C50 C 0.5571(6) 0.1526(5) 0.6982(2) 0.0940(16) Uani 1 1 d . . .
H50 H 0.6135 0.1135 0.7383 0.113 Uiso 1 1 calc R . .
C52 C 0.4068(6) 0.1949(5) 0.6176(3) 0.0953(16) Uani 1 1 d . . .
H52 H 0.3347 0.1946 0.5894 0.114 Uiso 1 1 calc R . .
H5 H 0.707(4) 0.431(3) -0.0157(18) 0.059(11) Uiso 1 1 d . . .
H10 H 0.620(4) 0.003(4) 0.279(2) 0.074(13) Uiso 1 1 d . . .
H15 H 0.964(4) 0.466(4) 0.2856(19) 0.079(13) Uiso 1 1 d . . .
H20 H 0.530(4) 0.271(3) 0.3704(18) 0.063(11) Uiso 1 1 d . . .
H25 H 1.154(4) -0.326(3) 0.3868(18) 0.062(11) Uiso 1 1 d . . .
H30 H 1.162(3) 0.294(3) 0.3497(15) 0.043(9) Uiso 1 1 d . . .
H35 H 0.887(3) 0.647(3) 0.1444(15) 0.043(9) Uiso 1 1 d . . .
H40 H 0.199(4) 0.752(3) 0.0565(17) 0.056(10) Uiso 1 1 d . . .
H45 H 0.312(4) 1.302(4) 0.143(2) 0.085(12) Uiso 1 1 d . . .
H48 H 0.457(5) 0.325(4) 0.567(2) 0.090(15) Uiso 1 1 d . . .
H1W1 H 0.46(2) 0.484(19) 0.495(11) 0.17(9) Uiso 0.50 1 d P . .
H2W1 H 0.368(7) 0.500(6) 0.444(4) 0.17(3) Uiso 1 1 d . . .
H3W1 H 0.302(19) 0.476(15) 0.504(8) 0.17(9) Uiso 0.50 1 d P . .
H1W2 H 0.096(6) 0.448(5) 0.432(3) 0.11(2) Uiso 1 1 d . . .
H2W2 H 0.180(14) 0.456(10) 0.480(6) 0.11(5) Uiso 0.50 1 d P . .
H3W2 H 0.045(12) 0.462(9) 0.492(7) 0.11(5) Uiso 0.50 1 d P . .
H2W3 H 0.99(8) 0.54(4) 0.99(4) 0.4(2) Uiso 1 1 d . . .
H1W3 H 1.06(5) 0.61(5) 0.97(3) 0.4(3) Uiso 0.50 1 d P . .
H3W3 H 0.94(6) 0.62(5) 0.95(2) 0.4(3) Uiso 0.50 1 d P . .
N1 N 0.3824(2) 0.59183(17) 0.20699(10) 0.0278(4) Uani 1 1 d . . .
H1A H 0.4172 0.6189 0.2370 0.033 Uiso 1 1 calc R . .
H1B H 0.3781 0.6366 0.1653 0.033 Uiso 1 1 calc R . .
N3 N 0.5974(2) 0.45462(18) 0.11850(10) 0.0312(5) Uani 1 1 d . . .
N5 N 0.6814(3) 0.4528(2) 0.01821(12) 0.0444(6) Uani 1 1 d . . .
N8 N 0.6116(2) 0.23914(18) 0.22465(10) 0.0325(5) Uani 1 1 d . . .
N10 N 0.6362(4) 0.0583(2) 0.25978(15) 0.0561(8) Uani 1 1 d . . .
N13 N 0.6812(2) 0.43335(19) 0.26297(11) 0.0332(5) Uani 1 1 d . . .
N15 N 0.8782(3) 0.4626(2) 0.28496(14) 0.0457(6) Uani 1 1 d . . .
N18 N 0.7795(2) 0.09175(18) 0.46386(10) 0.0316(5) Uani 1 1 d . . .
N20 N 0.5868(3) 0.2159(2) 0.40069(12) 0.0431(6) Uani 1 1 d . . .
N23 N 1.0156(2) -0.12185(18) 0.44318(10) 0.0323(5) Uani 1 1 d . . .
N25 N 1.0985(3) -0.2744(2) 0.40111(13) 0.0454(6) Uani 1 1 d . . .
N28 N 1.0695(2) 0.10188(18) 0.41811(10) 0.0331(5) Uani 1 1 d . . .
N30 N 1.1468(3) 0.2345(2) 0.36025(13) 0.0464(6) Uani 1 1 d . . .
N33 N 0.6287(2) 0.85839(18) 0.07876(10) 0.0338(5) Uani 1 1 d . . .
N35 N 0.8079(3) 0.7066(2) 0.13589(12) 0.0390(5) Uani 1 1 d . . .
N38 N 0.3390(2) 0.92728(18) -0.00076(10) 0.0339(5) Uani 1 1 d . . .
N40 N 0.2177(3) 0.8121(2) 0.03052(13) 0.0441(6) Uani 1 1 d . . .
N43 N 0.3854(2) 1.09049(19) 0.07211(10) 0.0357(5) Uani 1 1 d . . .
N45 N 0.3096(3) 1.2308(2) 0.12576(12) 0.0443(6) Uani 1 1 d . . .
N48 N 0.4721(4) 0.2706(3) 0.60334(19) 0.0749(10) Uani 1 1 d . . .
N51 N 0.4545(5) 0.1217(3) 0.6748(2) 0.0955(14) Uani 1 1 d . . .
Ni1 Ni 0.51331(3) 0.41503(3) 0.211536(14) 0.02485(9) Uani 1 1 d . . .
Ni2 Ni 1.0000 0.0000 0.5000 0.02613(11) Uani 1 2 d S . .
Ni3 Ni 0.5000 1.0000 0.0000 0.02910(11) Uani 1 2 d S . .
O1 O 0.40899(17) 0.38712(14) 0.30174(8) 0.0272(3) Uani 1 1 d . . .
O2 O 0.30763(19) 0.55488(16) 0.35608(8) 0.0340(4) Uani 1 1 d . . .
O3 O 0.14474(17) 0.45614(16) 0.33000(8) 0.0321(4) Uani 1 1 d . . .
O4 O 0.32192(17) 0.41367(14) 0.16334(8) 0.0288(4) Uani 1 1 d . . .
O5 O 0.1914(2) 0.61503(15) 0.09262(8) 0.0345(4) Uani 1 1 d . . .
O6 O 0.04912(17) 0.51377(15) 0.16885(8) 0.0314(4) Uani 1 1 d . . .
O1W O 0.3902(10) 0.4597(5) 0.4869(2) 0.139(2) Uani 1 1 d . . .
O2W O 0.1204(6) 0.4252(4) 0.47264(19) 0.0944(12) Uani 1 1 d . . .
O3W O 0.981(2) 0.609(3) 0.9826(18) 0.374(11) Uani 1 1 d U . .
P1 P 0.27457(6) 0.48891(5) 0.30952(3) 0.02224(13) Uani 1 1 d . . .
P2 P 0.19339(6) 0.52704(5) 0.15784(3) 0.02304(13) Uani 1 1 d . . .


_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
C1 N1 1.496(3) . ?
C1 C2 1.535(3) . ?
C1 P2 1.844(2) . ?
C1 P1 1.844(2) . ?
C2 H2A 0.9600 . ?
C2 H2B 0.9600 . ?
C2 H2C 0.9600 . ?
C4 N3 1.308(3) . ?
C4 N5 1.339(3) . ?
C4 H4 0.9300 . ?
C6 N5 1.351(4) . ?
C6 C7 1.351(4) . ?
C6 H6 0.9300 . ?
C7 N3 1.374(3) . ?
C7 H7 0.9300 . ?
C9 N8 1.309(3) . ?
C9 N10 1.331(4) . ?
C9 H9 0.9300 . ?
C11 C12 1.342(5) . ?
C11 N10 1.349(5) . ?
C11 H11 0.9300 . ?
C12 N8 1.369(4) . ?
C12 H12 0.9300 . ?
C14 N13 1.322(3) . ?
C14 N15 1.327(4) . ?
C14 H14 0.9300 . ?
C16 C17 1.346(4) . ?
C16 N15 1.355(4) . ?
C16 H16 0.9300 . ?
C17 N13 1.381(3) . ?
C17 H17 0.9300 . ?
C19 N18 1.317(3) . ?
C19 N20 1.327(4) . ?
C19 H19 0.9300 . ?
C21 C22 1.348(4) . ?
C21 N20 1.356(4) . ?
C21 H21 0.9300 . ?
C22 N18 1.358(3) . ?
C22 H22 0.9300 . ?
C24 N23 1.312(3) . ?
C24 N25 1.333(4) . ?
C24 H24 0.9300 . ?
C26 C27 1.341(4) . ?
C26 N25 1.352(4) . ?
C26 H26 0.9300 . ?
C27 N23 1.371(4) . ?
C27 H27 0.9300 . ?
C29 N28 1.318(4) . ?
C29 N30 1.334(3) . ?
C29 H29 0.9300 . ?
C31 N30 1.345(5) . ?
C31 C32 1.348(4) . ?
C31 H31 0.9300 . ?
C32 N28 1.371(4) . ?
C32 H32 0.9300 . ?
C34 N33 1.316(3) . ?
C34 N35 1.341(3) . ?
C34 H34 0.9300 . ?
C36 C37 1.356(4) . ?
C36 N35 1.357(4) . ?
C36 H36 0.9300 . ?
C37 N33 1.374(3) . ?
C37 H37 0.9300 . ?
C39 N38 1.312(3) . ?
C39 N40 1.320(4) . ?
C39 H39 0.9300 . ?
C41 C42 1.344(4) . ?
C41 N40 1.345(4) . ?
C41 H41 0.9300 . ?
C42 N38 1.368(4) . ?
C42 H42 0.9300 . ?
C44 N43 1.319(3) . ?
C44 N45 1.330(4) . ?
C44 H44 0.9300 . ?
C46 C47 1.351(5) . ?
C46 N45 1.354(4) . ?
C46 H46 0.9300 . ?
C47 N43 1.363(4) . ?
C47 H47 0.9300 . ?
C49 C50 1.351(6) . ?
C49 N48 1.356(5) . ?
C49 H49 0.9300 . ?
C50 N51 1.350(7) . ?
C50 H50 0.9300 . ?
C52 N51 1.290(6) . ?
C52 N48 1.326(5) . ?
C52 H52 0.9300 . ?
N1 Ni1 2.148(2) . ?
N1 H1A 0.9000 . ?
N1 H1B 0.9000 . ?
N3 Ni1 2.0819(19) . ?
N5 H5 0.80(4) . ?
N8 Ni1 2.062(2) . ?
N10 H10 0.79(4) . ?
N13 Ni1 2.101(2) . ?
N15 H15 0.87(4) . ?
N18 Ni2 2.127(2) . ?
N20 H20 0.85(4) . ?
N23 Ni2 2.115(2) . ?
N25 H25 0.80(4) . ?
N28 Ni2 2.133(2) . ?
N30 H30 0.81(3) . ?
N33 Ni3 2.139(2) . ?
N35 H35 0.87(3) . ?
N38 Ni3 2.122(2) . ?
N40 H40 0.90(3) . ?
N43 Ni3 2.136(2) . ?
N45 H45 1.07(4) . ?
N48 H48 0.86(4) . ?
Ni1 O1 2.1095(15) . ?
Ni1 O4 2.1670(16) . ?
Ni2 N23 2.115(2) 2_756 ?
Ni2 N18 2.127(2) 2_756 ?
Ni2 N28 2.133(2) 2_756 ?
Ni3 N38 2.122(2) 2_675 ?
Ni3 N43 2.136(2) 2_675 ?
Ni3 N33 2.139(2) 2_675 ?
O1 P1 1.5277(17) . ?
O2 P1 1.5226(18) . ?
O3 P1 1.5135(17) . ?
O4 P2 1.5305(17) . ?
O5 P2 1.5264(16) . ?
O6 P2 1.5059(17) . ?
O1W H1W1 0.85(14) . ?
O1W H2W1 0.90(8) . ?
O1W H3W1 0.90(16) . ?
O2W H1W2 0.82(6) . ?
O2W H2W2 0.86(15) . ?
O2W H3W2 0.87(10) . ?
O3W H2W3 0.9(5) . ?
O3W H1W3 0.9(4) . ?
O3W H3W3 0.9(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
_geom_angle_publ_flag
N1 C1 C2 112.49(19) . . ?
N1 C1 P2 102.37(14) . . ?
C2 C1 P2 111.67(15) . . ?
N1 C1 P1 102.99(14) . . ?
C2 C1 P1 112.27(16) . . ?
P2 C1 P1 114.31(12) . . ?
C1 C2 H2A 109.5 . . ?
C1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
C1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
N3 C4 N5 111.8(2) . . ?
N3 C4 H4 124.1 . . ?
N5 C4 H4 124.1 . . ?
N5 C6 C7 106.5(2) . . ?
N5 C6 H6 126.7 . . ?
C7 C6 H6 126.7 . . ?
C6 C7 N3 109.4(3) . . ?
C6 C7 H7 125.3 . . ?
N3 C7 H7 125.3 . . ?
N8 C9 N10 111.8(3) . . ?
N8 C9 H9 124.1 . . ?
N10 C9 H9 124.1 . . ?
C12 C11 N10 106.4(3) . . ?
C12 C11 H11 126.8 . . ?
N10 C11 H11 126.8 . . ?
C11 C12 N8 109.8(3) . . ?
C11 C12 H12 125.1 . . ?
N8 C12 H12 125.1 . . ?
N13 C14 N15 111.8(3) . . ?
N13 C14 H14 124.1 . . ?
N15 C14 H14 124.1 . . ?
C17 C16 N15 106.3(3) . . ?
C17 C16 H16 126.8 . . ?
N15 C16 H16 126.8 . . ?
C16 C17 N13 109.7(3) . . ?
C16 C17 H17 125.1 . . ?
N13 C17 H17 125.1 . . ?
N18 C19 N20 112.2(2) . . ?
N18 C19 H19 123.9 . . ?
N20 C19 H19 123.9 . . ?
C22 C21 N20 105.9(3) . . ?
C22 C21 H21 127.1 . . ?
N20 C21 H21 127.1 . . ?
C21 C22 N18 110.5(3) . . ?
C21 C22 H22 124.8 . . ?
N18 C22 H22 124.8 . . ?
N23 C24 N25 112.4(3) . . ?
N23 C24 H24 123.8 . . ?
N25 C24 H24 123.8 . . ?
C27 C26 N25 106.7(3) . . ?
C27 C26 H26 126.6 . . ?
N25 C26 H26 126.6 . . ?
C26 C27 N23 109.9(3) . . ?
C26 C27 H27 125.1 . . ?
N23 C27 H27 125.1 . . ?
N28 C29 N30 112.1(3) . . ?
N28 C29 H29 124.0 . . ?
N30 C29 H29 124.0 . . ?
N30 C31 C32 106.8(3) . . ?
N30 C31 H31 126.6 . . ?
C32 C31 H31 126.6 . . ?
C31 C32 N28 109.7(3) . . ?
C31 C32 H32 125.2 . . ?
N28 C32 H32 125.2 . . ?
N33 C34 N35 111.9(2) . . ?
N33 C34 H34 124.0 . . ?
N35 C34 H34 124.0 . . ?
C37 C36 N35 106.9(2) . . ?
C37 C36 H36 126.5 . . ?
N35 C36 H36 126.5 . . ?
C36 C37 N33 109.2(3) . . ?
C36 C37 H37 125.4 . . ?
N33 C37 H37 125.4 . . ?
N38 C39 N40 113.5(3) . . ?
N38 C39 H39 123.3 . . ?
N40 C39 H39 123.3 . . ?
C42 C41 N40 106.9(3) . . ?
C42 C41 H41 126.5 . . ?
N40 C41 H41 126.5 . . ?
C41 C42 N38 109.9(3) . . ?
C41 C42 H42 125.1 . . ?
N38 C42 H42 125.1 . . ?
N43 C44 N45 113.4(3) . . ?
N43 C44 H44 123.3 . . ?
N45 C44 H44 123.3 . . ?
C47 C46 N45 106.7(3) . . ?
C47 C46 H46 126.6 . . ?
N45 C46 H46 126.6 . . ?
C46 C47 N43 110.3(3) . . ?
C46 C47 H47 124.9 . . ?
N43 C47 H47 124.9 . . ?
C50 C49 N48 103.8(4) . . ?
C50 C49 H49 128.1 . . ?
N48 C49 H49 128.1 . . ?
N51 C50 C49 111.6(4) . . ?
N51 C50 H50 124.2 . . ?
C49 C50 H50 124.2 . . ?
N51 C52 N48 112.5(5) . . ?
N51 C52 H52 123.8 . . ?
N48 C52 H52 123.8 . . ?
C1 N1 Ni1 103.14(13) . . ?
C1 N1 H1A 111.1 . . ?
Ni1 N1 H1A 111.1 . . ?
C1 N1 H1B 111.1 . . ?
Ni1 N1 H1B 111.1 . . ?
H1A N1 H1B 109.1 . . ?
C4 N3 C7 105.1(2) . . ?
C4 N3 Ni1 129.99(18) . . ?
C7 N3 Ni1 124.87(18) . . ?
C4 N5 C6 107.2(2) . . ?
C4 N5 H5 126(3) . . ?
C6 N5 H5 127(3) . . ?
C9 N8 C12 104.8(2) . . ?
C9 N8 Ni1 122.58(19) . . ?
C12 N8 Ni1 132.51(19) . . ?
C9 N10 C11 107.2(3) . . ?
C9 N10 H10 126(3) . . ?
C11 N10 H10 126(3) . . ?
C14 N13 C17 104.5(2) . . ?
C14 N13 Ni1 128.98(19) . . ?
C17 N13 Ni1 126.01(17) . . ?
C14 N15 C16 107.7(2) . . ?
C14 N15 H15 132(3) . . ?
C16 N15 H15 120(3) . . ?
C19 N18 C22 104.4(2) . . ?
C19 N18 Ni2 126.78(18) . . ?
C22 N18 Ni2 128.78(17) . . ?
C19 N20 C21 107.0(2) . . ?
C19 N20 H20 130(2) . . ?
C21 N20 H20 123(2) . . ?
C24 N23 C27 104.4(2) . . ?
C24 N23 Ni2 128.02(18) . . ?
C27 N23 Ni2 127.54(19) . . ?
C24 N25 C26 106.6(3) . . ?
C24 N25 H25 129(3) . . ?
C26 N25 H25 123(3) . . ?
C29 N28 C32 104.4(2) . . ?
C29 N28 Ni2 127.14(18) . . ?
C32 N28 Ni2 128.2(2) . . ?
C29 N30 C31 107.0(3) . . ?
C29 N30 H30 126(2) . . ?
C31 N30 H30 127(2) . . ?
C34 N33 C37 105.2(2) . . ?
C34 N33 Ni3 128.75(18) . . ?
C37 N33 Ni3 125.74(18) . . ?
C34 N35 C36 106.7(2) . . ?
C34 N35 H35 127(2) . . ?
C36 N35 H35 127(2) . . ?
C39 N38 C42 103.5(2) . . ?
C39 N38 Ni3 126.61(19) . . ?
C42 N38 Ni3 129.89(18) . . ?
C39 N40 C41 106.2(2) . . ?
C39 N40 H40 123(2) . . ?
C41 N40 H40 131(2) . . ?
C44 N43 C47 103.6(2) . . ?
C44 N43 Ni3 125.53(19) . . ?
C47 N43 Ni3 129.6(2) . . ?
C44 N45 C46 105.9(3) . . ?
C44 N45 H45 124(2) . . ?
C46 N45 H45 130(2) . . ?
C52 N48 C49 107.7(4) . . ?
C52 N48 H48 126(3) . . ?
C49 N48 H48 126(3) . . ?
C52 N51 C50 104.2(4) . . ?
N8 Ni1 N3 94.70(8) . . ?
N8 Ni1 N13 95.34(9) . . ?
N3 Ni1 N13 91.92(8) . . ?
N8 Ni1 O1 89.25(7) . . ?
N3 Ni1 O1 174.54(7) . . ?
N13 Ni1 O1 91.46(7) . . ?
N8 Ni1 N1 170.44(8) . . ?
N3 Ni1 N1 93.39(8) . . ?
N13 Ni1 N1 89.47(8) . . ?
O1 Ni1 N1 82.35(7) . . ?
N8 Ni1 O4 90.66(8) . . ?
N3 Ni1 O4 91.48(7) . . ?
N13 Ni1 O4 172.84(8) . . ?
O1 Ni1 O4 84.70(6) . . ?
N1 Ni1 O4 84.04(7) . . ?
N23 Ni2 N23 180.00(8) . 2_756 ?
N23 Ni2 N18 90.11(8) . . ?
N23 Ni2 N18 89.89(8) 2_756 . ?
N23 Ni2 N18 89.89(8) . 2_756 ?
N23 Ni2 N18 90.11(8) 2_756 2_756 ?
N18 Ni2 N18 180.00(11) . 2_756 ?
N23 Ni2 N28 91.09(8) . . ?
N23 Ni2 N28 88.91(8) 2_756 . ?
N18 Ni2 N28 91.01(8) . . ?
N18 Ni2 N28 88.99(8) 2_756 . ?
N23 Ni2 N28 88.91(8) . 2_756 ?
N23 Ni2 N28 91.09(8) 2_756 2_756 ?
N18 Ni2 N28 88.99(8) . 2_756 ?
N18 Ni2 N28 91.01(8) 2_756 2_756 ?
N28 Ni2 N28 180.000(1) . 2_756 ?
N38 Ni3 N38 180.00(11) . 2_675 ?
N38 Ni3 N43 90.46(8) . 2_675 ?
N38 Ni3 N43 89.54(8) 2_675 2_675 ?
N38 Ni3 N43 89.54(8) . . ?
N38 Ni3 N43 90.46(8) 2_675 . ?
N43 Ni3 N43 180.000(1) 2_675 . ?
N38 Ni3 N33 88.00(8) . 2_675 ?
N38 Ni3 N33 92.00(8) 2_675 2_675 ?
N43 Ni3 N33 91.24(8) 2_675 2_675 ?
N43 Ni3 N33 88.76(8) . 2_675 ?
N38 Ni3 N33 92.00(8) . . ?
N38 Ni3 N33 88.00(8) 2_675 . ?
N43 Ni3 N33 88.76(8) 2_675 . ?
N43 Ni3 N33 91.24(8) . . ?
N33 Ni3 N33 180.00(15) 2_675 . ?
P1 O1 Ni1 115.13(9) . . ?
P2 O4 Ni1 111.54(9) . . ?
H1W1 O1W H2W1 96(10) . . ?
H1W1 O1W H3W1 128(10) . . ?
H2W1 O1W H3W1 102(10) . . ?
H1W2 O2W H2W2 107(8) . . ?
H1W2 O2W H3W2 105(9) . . ?
H2W2 O2W H3W2 101(10) . . ?
O3 P1 O2 111.99(10) . . ?
O3 P1 O1 113.46(10) . . ?
O2 P1 O1 111.59(10) . . ?
O3 P1 C1 110.08(10) . . ?
O2 P1 C1 105.55(10) . . ?
O1 P1 C1 103.54(9) . . ?
O6 P2 O5 112.66(10) . . ?
O6 P2 O4 114.45(10) . . ?
O5 P2 O4 111.26(10) . . ?
O6 P2 C1 109.56(10) . . ?
O5 P2 C1 103.91(10) . . ?
O4 P2 C1 104.07(10) . . ?

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
N5 C6 C7 N3 0.0(4) . . . . ?
N10 C11 C12 N8 -0.6(5) . . . . ?
N15 C16 C17 N13 0.2(3) . . . . ?
N20 C21 C22 N18 0.0(4) . . . . ?
N25 C26 C27 N23 0.4(4) . . . . ?
N30 C31 C32 N28 0.5(4) . . . . ?
N35 C36 C37 N33 0.6(4) . . . . ?
N40 C41 C42 N38 0.4(4) . . . . ?
N45 C46 C47 N43 -2.0(4) . . . . ?
N48 C49 C50 N51 -3.1(5) . . . . ?
C2 C1 N1 Ni1 -179.63(15) . . . . ?
P2 C1 N1 Ni1 -59.63(13) . . . . ?
P1 C1 N1 Ni1 59.27(13) . . . . ?
N5 C4 N3 C7 0.8(3) . . . . ?
N5 C4 N3 Ni1 179.65(19) . . . . ?
C6 C7 N3 C4 -0.5(3) . . . . ?
C6 C7 N3 Ni1 -179.4(2) . . . . ?
N3 C4 N5 C6 -0.8(4) . . . . ?
C7 C6 N5 C4 0.5(4) . . . . ?
N10 C9 N8 C12 0.0(3) . . . . ?
N10 C9 N8 Ni1 -176.0(2) . . . . ?
C11 C12 N8 C9 0.4(4) . . . . ?
C11 C12 N8 Ni1 175.8(3) . . . . ?
N8 C9 N10 C11 -0.3(4) . . . . ?
C12 C11 N10 C9 0.6(4) . . . . ?
N15 C14 N13 C17 -0.1(3) . . . . ?
N15 C14 N13 Ni1 171.71(18) . . . . ?
C16 C17 N13 C14 -0.1(3) . . . . ?
C16 C17 N13 Ni1 -172.2(2) . . . . ?
N13 C14 N15 C16 0.2(3) . . . . ?
C17 C16 N15 C14 -0.3(3) . . . . ?
N20 C19 N18 C22 0.2(3) . . . . ?
N20 C19 N18 Ni2 -179.87(19) . . . . ?
C21 C22 N18 C19 -0.2(4) . . . . ?
C21 C22 N18 Ni2 179.9(2) . . . . ?
N18 C19 N20 C21 -0.2(4) . . . . ?
C22 C21 N20 C19 0.1(4) . . . . ?
N25 C24 N23 C27 0.5(3) . . . . ?
N25 C24 N23 Ni2 178.07(18) . . . . ?
C26 C27 N23 C24 -0.5(3) . . . . ?
C26 C27 N23 Ni2 -178.1(2) . . . . ?
N23 C24 N25 C26 -0.3(4) . . . . ?
C27 C26 N25 C24 -0.1(4) . . . . ?
N30 C29 N28 C32 -0.3(3) . . . . ?
N30 C29 N28 Ni2 174.57(18) . . . . ?
C31 C32 N28 C29 -0.1(4) . . . . ?
C31 C32 N28 Ni2 -174.9(2) . . . . ?
N28 C29 N30 C31 0.6(4) . . . . ?
C32 C31 N30 C29 -0.6(4) . . . . ?
N35 C34 N33 C37 0.0(3) . . . . ?
N35 C34 N33 Ni3 174.11(17) . . . . ?
C36 C37 N33 C34 -0.4(3) . . . . ?
C36 C37 N33 Ni3 -174.7(2) . . . . ?
N33 C34 N35 C36 0.4(3) . . . . ?
C37 C36 N35 C34 -0.6(3) . . . . ?
N40 C39 N38 C42 -1.2(4) . . . . ?
N40 C39 N38 Ni3 179.8(2) . . . . ?
C41 C42 N38 C39 0.4(4) . . . . ?
C41 C42 N38 Ni3 179.4(2) . . . . ?
N38 C39 N40 C41 1.4(4) . . . . ?
C42 C41 N40 C39 -1.1(4) . . . . ?
N45 C44 N43 C47 -1.6(3) . . . . ?
N45 C44 N43 Ni3 166.42(19) . . . . ?
C46 C47 N43 C44 2.1(4) . . . . ?
C46 C47 N43 Ni3 -165.2(2) . . . . ?
N43 C44 N45 C46 0.4(4) . . . . ?
C47 C46 N45 C44 0.9(4) . . . . ?
N51 C52 N48 C49 -1.6(6) . . . . ?
C50 C49 N48 C52 2.7(5) . . . . ?
N48 C52 N51 C50 -0.3(6) . . . . ?
C49 C50 N51 C52 2.2(6) . . . . ?
C9 N8 Ni1 N3 -143.3(2) . . . . ?
C12 N8 Ni1 N3 42.0(3) . . . . ?
C9 N8 Ni1 N13 124.3(2) . . . . ?
C12 N8 Ni1 N13 -50.4(3) . . . . ?
C9 N8 Ni1 O1 32.9(2) . . . . ?
C12 N8 Ni1 O1 -141.8(3) . . . . ?
C9 N8 Ni1 N1 4.4(6) . . . . ?
C12 N8 Ni1 N1 -170.3(4) . . . . ?
C9 N8 Ni1 O4 -51.8(2) . . . . ?
C12 N8 Ni1 O4 133.5(3) . . . . ?
C4 N3 Ni1 N8 31.2(2) . . . . ?
C7 N3 Ni1 N8 -150.2(2) . . . . ?
C4 N3 Ni1 N13 126.7(2) . . . . ?
C7 N3 Ni1 N13 -54.6(2) . . . . ?
C4 N3 Ni1 O1 -105.1(8) . . . . ?
C7 N3 Ni1 O1 73.6(9) . . . . ?
C4 N3 Ni1 N1 -143.7(2) . . . . ?
C7 N3 Ni1 N1 34.9(2) . . . . ?
C4 N3 Ni1 O4 -59.6(2) . . . . ?
C7 N3 Ni1 O4 119.0(2) . . . . ?
C14 N13 Ni1 N8 77.6(2) . . . . ?
C17 N13 Ni1 N8 -112.3(2) . . . . ?
C14 N13 Ni1 N3 -17.3(2) . . . . ?
C17 N13 Ni1 N3 152.8(2) . . . . ?
C14 N13 Ni1 O1 166.9(2) . . . . ?
C17 N13 Ni1 O1 -22.9(2) . . . . ?
C14 N13 Ni1 N1 -110.7(2) . . . . ?
C17 N13 Ni1 N1 59.4(2) . . . . ?
C14 N13 Ni1 O4 -135.6(5) . . . . ?
C17 N13 Ni1 O4 34.5(7) . . . . ?
C1 N1 Ni1 N8 -16.2(5) . . . . ?
C1 N1 Ni1 N3 131.62(13) . . . . ?
C1 N1 Ni1 N13 -136.49(13) . . . . ?
C1 N1 Ni1 O1 -44.94(13) . . . . ?
C1 N1 Ni1 O4 40.49(12) . . . . ?
C24 N23 Ni2 N23 -44(100) . . . 2_756 ?
C27 N23 Ni2 N23 133(100) . . . 2_756 ?
C24 N23 Ni2 N18 -177.8(2) . . . . ?
C27 N23 Ni2 N18 -0.7(2) . . . . ?
C24 N23 Ni2 N18 2.2(2) . . . 2_756 ?
C27 N23 Ni2 N18 179.3(2) . . . 2_756 ?
C24 N23 Ni2 N28 91.2(2) . . . . ?
C27 N23 Ni2 N28 -91.7(2) . . . . ?
C24 N23 Ni2 N28 -88.8(2) . . . 2_756 ?
C27 N23 Ni2 N28 88.3(2) . . . 2_756 ?
C19 N18 Ni2 N23 -90.6(2) . . . . ?
C22 N18 Ni2 N23 89.3(3) . . . . ?
C19 N18 Ni2 N23 89.4(2) . . . 2_756 ?
C22 N18 Ni2 N23 -90.7(3) . . . 2_756 ?
C19 N18 Ni2 N18 104(100) . . . 2_756 ?
C22 N18 Ni2 N18 -77(100) . . . 2_756 ?
C19 N18 Ni2 N28 0.5(2) . . . . ?
C22 N18 Ni2 N28 -179.6(3) . . . . ?
C19 N18 Ni2 N28 -179.5(2) . . . 2_756 ?
C22 N18 Ni2 N28 0.4(3) . . . 2_756 ?
C29 N28 Ni2 N23 -177.5(2) . . . . ?
C32 N28 Ni2 N23 -3.9(3) . . . . ?
C29 N28 Ni2 N23 2.5(2) . . . 2_756 ?
C32 N28 Ni2 N23 176.1(3) . . . 2_756 ?
C29 N28 Ni2 N18 92.3(2) . . . . ?
C32 N28 Ni2 N18 -94.0(3) . . . . ?
C29 N28 Ni2 N18 -87.7(2) . . . 2_756 ?
C32 N28 Ni2 N18 86.0(3) . . . 2_756 ?
C29 N28 Ni2 N28 -31(100) . . . 2_756 ?
C32 N28 Ni2 N28 142(100) . . . 2_756 ?
C39 N38 Ni3 N38 -3(100) . . . 2_675 ?
C42 N38 Ni3 N38 178(100) . . . 2_675 ?
C39 N38 Ni3 N43 99.0(2) . . . 2_675 ?
C42 N38 Ni3 N43 -79.7(3) . . . 2_675 ?
C39 N38 Ni3 N43 -81.0(2) . . . . ?
C42 N38 Ni3 N43 100.3(3) . . . . ?
C39 N38 Ni3 N33 -169.8(3) . . . 2_675 ?
C42 N38 Ni3 N33 11.5(3) . . . 2_675 ?
C39 N38 Ni3 N33 10.2(3) . . . . ?
C42 N38 Ni3 N33 -168.5(3) . . . . ?
C44 N43 Ni3 N38 -170.5(2) . . . . ?
C47 N43 Ni3 N38 -5.7(3) . . . . ?
C44 N43 Ni3 N38 9.5(2) . . . 2_675 ?
C47 N43 Ni3 N38 174.3(3) . . . 2_675 ?
C44 N43 Ni3 N43 48(100) . . . 2_675 ?
C47 N43 Ni3 N43 -147(100) . . . 2_675 ?
C44 N43 Ni3 N33 -82.5(2) . . . 2_675 ?
C47 N43 Ni3 N33 82.3(3) . . . 2_675 ?
C44 N43 Ni3 N33 97.5(2) . . . . ?
C47 N43 Ni3 N33 -97.7(3) . . . . ?
C34 N33 Ni3 N38 106.8(2) . . . . ?
C37 N33 Ni3 N38 -80.2(2) . . . . ?
C34 N33 Ni3 N38 -73.2(2) . . . 2_675 ?
C37 N33 Ni3 N38 99.8(2) . . . 2_675 ?
C34 N33 Ni3 N43 16.3(2) . . . 2_675 ?
C37 N33 Ni3 N43 -170.7(2) . . . 2_675 ?
C34 N33 Ni3 N43 -163.7(2) . . . . ?
C37 N33 Ni3 N43 9.3(2) . . . . ?
C34 N33 Ni3 N33 -81(100) . . . 2_675 ?
C37 N33 Ni3 N33 92(100) . . . 2_675 ?
N8 Ni1 O1 P1 -159.96(11) . . . . ?
N3 Ni1 O1 P1 -23.5(9) . . . . ?
N13 Ni1 O1 P1 104.71(11) . . . . ?
N1 Ni1 O1 P1 15.45(10) . . . . ?
O4 Ni1 O1 P1 -69.23(10) . . . . ?
N8 Ni1 O4 P2 166.05(10) . . . . ?
N3 Ni1 O4 P2 -99.23(10) . . . . ?
N13 Ni1 O4 P2 19.1(6) . . . . ?
O1 Ni1 O4 P2 76.86(10) . . . . ?
N1 Ni1 O4 P2 -5.98(9) . . . . ?
Ni1 O1 P1 O3 131.26(10) . . . . ?
Ni1 O1 P1 O2 -101.11(11) . . . . ?
Ni1 O1 P1 C1 11.96(12) . . . . ?
N1 C1 P1 O3 -169.26(14) . . . . ?
C2 C1 P1 O3 69.49(19) . . . . ?
P2 C1 P1 O3 -59.04(15) . . . . ?
N1 C1 P1 O2 69.72(16) . . . . ?
C2 C1 P1 O2 -51.53(19) . . . . ?
P2 C1 P1 O2 179.93(11) . . . . ?
N1 C1 P1 O1 -47.66(16) . . . . ?
C2 C1 P1 O1 -168.91(16) . . . . ?
P2 C1 P1 O1 62.56(14) . . . . ?
Ni1 O4 P2 O6 -142.42(9) . . . . ?
Ni1 O4 P2 O5 88.45(11) . . . . ?
Ni1 O4 P2 C1 -22.87(11) . . . . ?
N1 C1 P2 O6 178.77(13) . . . . ?
C2 C1 P2 O6 -60.66(18) . . . . ?
P1 C1 P2 O6 68.18(14) . . . . ?
N1 C1 P2 O5 -60.61(15) . . . . ?
C2 C1 P2 O5 59.96(18) . . . . ?
P1 C1 P2 O5 -171.20(12) . . . . ?
N1 C1 P2 O4 55.95(15) . . . . ?
C2 C1 P2 O4 176.52(15) . . . . ?
P1 C1 P2 O4 -54.64(14) . . . . ?

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
N48 H48 O1W 0.86(4) 2.00(5) 2.858(6) 171(4) .
O2W H3W2 O2W 0.87(10) 2.00(10) 2.860(10) 169(12) 2_566
O2W H2W2 O1W 0.86(15) 2.11(14) 2.896(11) 153(11) .
O2W H1W2 O3 0.82(6) 2.11(6) 2.861(4) 151(5) .
O1W H3W1 O2W 0.90(16) 2.27(19) 2.896(11) 126(14) .
O1W H2W1 O2 0.90(8) 1.80(8) 2.676(4) 166(7) .
O1W H1W1 O1W 0.85(14) 1.99(15) 2.836(18) 180(28) 2_666
N45 H45 O4 1.07(4) 1.61(4) 2.675(3) 175(3) 1_565
N40 H40 O5 0.90(3) 1.77(4) 2.651(3) 165(3) .
N35 H35 O6 0.87(3) 1.84(3) 2.705(3) 175(3) 1_655
N30 H30 O3 0.81(3) 1.96(3) 2.758(3) 164(3) 1_655
N25 H25 O2 0.80(4) 1.94(4) 2.738(3) 172(4) 1_645
N20 H20 O1 0.85(4) 1.85(4) 2.706(3) 177(4) .
N15 H15 O6 0.87(4) 2.52(4) 2.965(3) 113(3) 1_655
N15 H15 O3 0.87(4) 1.98(4) 2.787(3) 154(4) 1_655
N10 H10 N51 0.79(4) 2.03(4) 2.815(4) 171(4) 2_656
N5 H5 O5 0.80(4) 1.94(4) 2.728(3) 167(4) 2_665

_diffrn_measured_fraction_theta_max 0.964
_diffrn_reflns_theta_full        28.00
_diffrn_measured_fraction_theta_full 0.964
_refine_diff_density_max         1.097
_refine_diff_density_min         -0.901
_refine_diff_density_rms         0.071

# Attachment 'S-10.cif'

data_61128csp1_0m
_database_code_depnum_ccdc_archive 'CCDC 660454'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C36 H68 N23 Ni2 O17 P3'
_chemical_formula_weight         1305.46

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'
P P 0.1023 0.0942 '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           Monoclinic
_symmetry_space_group_name_H-M   P2(1)/c

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

_cell_length_a                   9.3330(6)
_cell_length_b                   23.5953(14)
_cell_length_c                   26.7989(16)
_cell_angle_alpha                90.00
_cell_angle_beta                 97.7650(10)
_cell_angle_gamma                90.00
_cell_volume                     5847.4(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    273(2)
_cell_measurement_reflns_used    6816
_cell_measurement_theta_min      2.31
_cell_measurement_theta_max      29.40

_exptl_crystal_description       ?
_exptl_crystal_colour            ?
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.22
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.483
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2728
_exptl_absorpt_coefficient_mu    0.809
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.7594
_exptl_absorpt_correction_T_max  0.8421
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      273(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            39037
_diffrn_reflns_av_R_equivalents  0.0201
_diffrn_reflns_av_sigmaI/netI    0.0248
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_theta_min         2.31
_diffrn_reflns_theta_max         28.00
_reflns_number_total             14058
_reflns_number_gt                11036
_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 F² against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F², conventional R-factors R are based
on F, with F set to zero for negative F². The threshold expression of
F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F² 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/[σ²(Fo²)+(0.1115P)²+17.0883P] where P=(Fo²+2Fc²)/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         14058
_refine_ls_number_parameters     846
_refine_ls_number_restraints     48
_refine_ls_R_factor_all          0.0933
_refine_ls_R_factor_gt           0.0774
_refine_ls_wR_factor_ref         0.2339
_refine_ls_wR_factor_gt          0.2225
_refine_ls_goodness_of_fit_ref   1.143
_refine_ls_restrained_S_all      1.182
_refine_ls_shift/su_max          0.000
_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
C1 C 0.6568(4) 0.75144(15) 0.77398(14) 0.0209(7) Uani 1 1 d . . .
C2 C 0.7260(5) 0.74902(16) 0.82952(15) 0.0247(8) Uani 1 1 d . . .
H2A H 0.6731 0.7746 0.8487 0.030 Uiso 1 1 calc R . .
H2B H 0.7131 0.7110 0.8420 0.030 Uiso 1 1 calc R . .
C3 C 0.8868(5) 0.76397(19) 0.84030(15) 0.0279(8) Uani 1 1 d . . .
H3A H 0.8991 0.8036 0.8324 0.033 Uiso 1 1 calc R . .
H3B H 0.9392 0.7418 0.8183 0.033 Uiso 1 1 calc R . .
C4 C 0.2142(7) 0.6530(2) 0.7194(3) 0.0526(14) Uani 1 1 d . . .
H4 H 0.2138 0.6684 0.7513 0.063 Uiso 1 1 calc R . .
C6 C 0.1661(7) 0.5971(3) 0.6550(3) 0.0675(19) Uani 1 1 d . . .
H6 H 0.1298 0.5678 0.6338 0.081 Uiso 1 1 calc R . .
C7 C 0.2558(7) 0.6390(3) 0.6440(3) 0.0569(15) Uani 1 1 d . . .
H7 H 0.2907 0.6435 0.6134 0.068 Uiso 1 1 calc R . .
C9 C 0.5041(6) 0.7477(2) 0.5842(2) 0.0394(11) Uani 1 1 d . . .
H9 H 0.6005 0.7412 0.5969 0.047 Uiso 1 1 calc R . .
C11 C 0.3081(7) 0.7619(3) 0.5312(2) 0.0547(15) Uani 1 1 d . . .
H11 H 0.2439 0.7669 0.5018 0.066 Uiso 1 1 calc R . .
C12 C 0.2762(6) 0.7622(3) 0.5794(2) 0.0510(14) Uani 1 1 d . . .
H12 H 0.1847 0.7678 0.5886 0.061 Uiso 1 1 calc R . .
C13 C 0.1405(5) 0.7921(2) 0.71624(19) 0.0393(10) Uani 1 1 d . . .
H13 H 0.1163 0.7576 0.7297 0.047 Uiso 1 1 calc R . .
C15 C 0.1269(6) 0.8790(3) 0.6918(3) 0.0600(17) Uani 1 1 d . . .
H15 H 0.0943 0.9157 0.6848 0.072 Uiso 1 1 calc R . .
C16 C 0.2533(6) 0.8563(2) 0.6820(3) 0.0537(15) Uani 1 1 d . . .
H16 H 0.3237 0.8754 0.6671 0.064 Uiso 1 1 calc R . .
C18 C 0.3297(6) 0.4025(2) 1.04044(19) 0.0385(10) Uani 1 1 d . . .
H18 H 0.3095 0.3878 1.0080 0.046 Uiso 1 1 calc R . .
C20 C 0.3296(7) 0.4135(3) 1.1206(2) 0.0531(14) Uani 1 1 d . . .
H20 H 0.3118 0.4092 1.1537 0.064 Uiso 1 1 calc R . .
C21 C 0.4156(6) 0.4528(3) 1.10301(19) 0.0468(13) Uani 1 1 d . . .
H21 H 0.4674 0.4805 1.1225 0.056 Uiso 1 1 calc R . .
C23 C 0.2741(6) 0.5944(2) 0.96561(19) 0.0393(11) Uani 1 1 d . . .
H23 H 0.3350 0.6105 0.9447 0.047 Uiso 1 1 calc R . .
C25 C 0.0863(7) 0.5793(3) 1.0028(3) 0.070(2) Uani 1 1 d . . .
H25 H -0.0047 0.5818 1.0130 0.084 Uiso 1 1 calc R . .
C26 C 0.1907(6) 0.5414(3) 1.0189(3) 0.0575(16) Uani 1 1 d . . .
H26 H 0.1827 0.5130 1.0425 0.069 Uiso 1 1 calc R . .
C28 C 0.4618(5) 0.40717(19) 0.91768(17) 0.0345(9) Uani 1 1 d . . .
H28 H 0.5474 0.3896 0.9314 0.041 Uiso 1 1 calc R . .
C30 C 0.2680(6) 0.4272(2) 0.8665(2) 0.0479(13) Uani 1 1 d . . .
H30 H 0.1954 0.4272 0.8391 0.057 Uiso 1 1 calc R . .
C31 C 0.2791(6) 0.4626(2) 0.9069(2) 0.0414(11) Uani 1 1 d . . .
H31 H 0.2131 0.4908 0.9119 0.050 Uiso 1 1 calc R . .
C33 C 0.3156(6) 0.0935(2) 1.0389(2) 0.0419(11) Uani 1 1 d . . .
H33 H 0.3040 0.1105 1.0073 0.050 Uiso 1 1 calc R . .
C35 C 0.2960(10) 0.0776(3) 1.1167(2) 0.075(2) Uani 1 1 d . . .
H35 H 0.2711 0.0802 1.1491 0.090 Uiso 1 1 calc R . .
C36 C 0.3797(8) 0.0373(3) 1.0994(2) 0.0621(18) Uani 1 1 d . . .
H36 H 0.4221 0.0072 1.1183 0.075 Uiso 1 1 calc R . .
C38 C 0.4377(6) 0.0908(2) 0.91791(18) 0.0374(10) Uani 1 1 d . . .
H38 H 0.5189 0.1109 0.9320 0.045 Uiso 1 1 calc R . .
C40 C 0.2480(6) 0.0663(3) 0.8666(2) 0.0488(13) Uani 1 1 d . . .
H40 H 0.1740 0.0652 0.8396 0.059 Uiso 1 1 calc R . .
C41 C 0.2694(6) 0.0294(2) 0.9056(2) 0.0440(12) Uani 1 1 d . . .
H41 H 0.2114 -0.0019 0.9098 0.053 Uiso 1 1 calc R . .
C43 C 0.3158(6) -0.1068(2) 0.9656(2) 0.0445(12) Uani 1 1 d . . .
H43 H 0.3884 -0.1203 0.9482 0.053 Uiso 1 1 calc R . .
C45 C 0.1123(8) -0.0997(3) 0.9948(3) 0.0670(19) Uani 1 1 d . . .
H45 H 0.0192 -0.1066 1.0020 0.080 Uiso 1 1 calc R . .
C46 C 0.1975(7) -0.0557(3) 1.0110(3) 0.0554(15) Uani 1 1 d . . .
H46 H 0.1717 -0.0265 1.0314 0.066 Uiso 1 1 calc R . .
C48 C 0.6281(8) 0.4885(3) 0.7392(3) 0.0656(18) Uani 1 1 d . . .
C50 C 0.4729(10) 0.5499(3) 0.7519(5) 0.106(4) Uani 1 1 d . . .
H50 H 0.4287 0.5840 0.7580 0.127 Uiso 1 1 calc R . .
C51 C 0.4074(9) 0.4990(3) 0.7460(4) 0.091(3) Uani 1 1 d . . .
H51 H 0.3099 0.4918 0.7474 0.110 Uiso 1 1 calc R . .
C53 C 0.8961(7) 0.7027(3) 0.5823(2) 0.0484(13) Uani 1 1 d . . .
H53 H 0.9018 0.6634 0.5839 0.058 Uiso 1 1 calc R . .
C55 C 0.8812(7) 0.7892(3) 0.6030(2) 0.0563(15) Uani 1 1 d . . .
H55 H 0.8743 0.8220 0.6218 0.068 Uiso 1 1 calc R . .
C56 C 0.8848(7) 0.7875(3) 0.5528(2) 0.0572(15) Uani 1 1 d . . .
H56 H 0.8815 0.8184 0.5312 0.069 Uiso 1 1 calc R . .
H48 H 0.7161 0.4718 0.7348 0.069 Uiso 1 1 d R . .
N1 N 0.4986(4) 0.73681(15) 0.76916(13) 0.0250(7) Uani 1 1 d . . .
H1A H 0.4510 0.7610 0.7870 0.030 Uiso 1 1 calc R . .
H1B H 0.4857 0.7012 0.7798 0.030 Uiso 1 1 calc R . .
N2 N 0.2874(4) 0.67399(18) 0.68487(17) 0.0402(9) Uani 1 1 d . . .
N5 N 0.1395(6) 0.6059(2) 0.7025(3) 0.0629(15) Uani 1 1 d . . .
N8 N 0.4004(4) 0.75278(17) 0.61214(15) 0.0356(9) Uani 1 1 d . . .
N10 N 0.4543(6) 0.7528(2) 0.53493(18) 0.0469(11) Uani 1 1 d . . .
N13 N 0.2613(4) 0.80128(17) 0.69731(15) 0.0333(8) Uani 1 1 d . . .
N14 N 0.0574(5) 0.8378(2) 0.71380(18) 0.0464(11) Uani 1 1 d . . .
H14 H -0.0254 0.8406 0.7243 0.056 Uiso 1 1 calc R . .
N17 N 0.4152(4) 0.44590(16) 1.05224(14) 0.0309(8) Uani 1 1 d . . .
N19 N 0.2746(5) 0.3814(2) 1.08041(17) 0.0433(10) Uani 1 1 d . . .
N22 N 0.3095(4) 0.55090(16) 0.99562(14) 0.0308(8) Uani 1 1 d . . .
N24 N 0.1396(5) 0.6128(2) 0.9688(2) 0.0466(11) Uani 1 1 d . . .
N27 N 0.4024(4) 0.45030(15) 0.93895(13) 0.0297(7) Uani 1 1 d . . .
N29 N 0.3837(5) 0.39185(19) 0.87403(16) 0.0387(9) Uani 1 1 d . . .
N32 N 0.3926(4) 0.04751(16) 1.05011(14) 0.0319(8) Uani 1 1 d . . .
N34 N 0.2556(6) 0.1132(2) 1.07800(19) 0.0515(12) Uani 1 1 d . . .
N37 N 0.3893(4) 0.04497(15) 0.93792(14) 0.0306(8) Uani 1 1 d . . .
N39 N 0.3558(5) 0.1052(2) 0.87473(17) 0.0400(9) Uani 1 1 d . . .
N42 N 0.3271(4) -0.05990(16) 0.99319(15) 0.0332(8) Uani 1 1 d . . .
N44 N 0.1888(6) -0.1323(2) 0.9657(2) 0.0536(12) Uani 1 1 d . . .
N47 N 0.5061(6) 0.4610(2) 0.7381(2) 0.0495(11) Uani 1 1 d . . .
N49 N 0.6109(7) 0.5428(2) 0.7473(2) 0.0555(14) Uani 1 1 d . . .
N52 N 0.8941(5) 0.7326(2) 0.54012(18) 0.0460(11) Uani 1 1 d . . .
N54 N 0.8891(5) 0.7358(2) 0.62183(16) 0.0461(11) Uani 1 1 d . . .
Ni1 Ni 0.42564(6) 0.74488(2) 0.68940(2) 0.02583(15) Uani 1 1 d . . .
Ni2 Ni 0.5000 0.5000 1.0000 0.02315(17) Uani 1 2 d S . .
Ni3 Ni 0.5000 0.0000 1.0000 0.02401(18) Uani 1 2 d S . .
O1 O 0.6098(3) 0.69096(13) 0.68865(11) 0.0307(6) Uani 1 1 d . . .
O2 O 0.8695(3) 0.71845(15) 0.71705(13) 0.0328(7) Uani 1 1 d . . .
O3 O 0.7539(4) 0.64377(12) 0.76487(12) 0.0336(7) Uani 1 1 d . . .
O4 O 0.5729(3) 0.81296(13) 0.69336(11) 0.0288(6) Uani 1 1 d . . .
O5 O 0.5581(4) 0.85635(13) 0.77909(12) 0.0364(7) Uani 1 1 d . . .
O6 O 0.7982(3) 0.84971(13) 0.74664(13) 0.0336(7) Uani 1 1 d . . .
O7 O 0.9564(4) 0.68761(13) 0.91394(13) 0.0359(7) Uani 1 1 d . . .
O8 O 1.1191(4) 0.77260(17) 0.91113(15) 0.0463(9) Uani 1 1 d . . .
O9 O 0.8744(4) 0.78433(16) 0.93854(12) 0.0407(8) Uani 1 1 d . . .
O1W O 0.9761(9) 0.5253(4) 0.7474(4) 0.101(2) Uani 1 1 d U . .
O2W O 1.0010(6) 0.6225(2) 0.8301(2) 0.0676(13) Uani 1 1 d U . .
O3W O 0.5914(9) 0.7519(3) 0.9507(3) 0.097(2) Uani 1 1 d U . .
O4W O 0.3557(11) 0.7359(11) 0.8779(5) 0.164(4) Uani 1 1 d U . .
O5W O 0.038(2) 0.4295(5) 0.7014(6) 0.146(4) Uani 1 1 d U . .
O6W O 0.2986(17) 0.6266(8) 0.8367(4) 0.158(4) Uani 1 1 d U . .
O7W O 0.956(3) 0.5133(12) 0.8496(9) 0.227(8) Uani 1 1 d U . .
O8W O 0.260(5) 0.8607(10) 0.8323(10) 0.258(10) Uani 1.00(5) 1 d U . .
P1 P 0.72614(11) 0.69692(4) 0.73368(4) 0.0223(2) Uani 1 1 d . . .
P2 P 0.65111(11) 0.82323(4) 0.74628(4) 0.0224(2) Uani 1 1 d . . .
P3 P 0.96457(12) 0.75136(4) 0.90492(4) 0.0251(2) Uani 1 1 d . . .
H1 H 0.879(9) 0.722(4) 0.688(3) 0.08(3) Uiso 1 1 d . . .
H5 H 0.086(8) 0.585(3) 0.717(3) 0.06(2) Uiso 1 1 d . . .
H10 H 0.510(8) 0.750(3) 0.511(3) 0.06(2) Uiso 1 1 d . . .
H19 H 0.212(9) 0.357(4) 1.084(3) 0.08(3) Uiso 1 1 d . . .
H24 H 0.091(8) 0.638(3) 0.953(3) 0.07(2) Uiso 1 1 d . . .
H29 H 0.406(7) 0.364(3) 0.855(3) 0.057(19) Uiso 1 1 d . . .
H34 H 0.194(8) 0.138(3) 1.076(3) 0.07(3) Uiso 1 1 d . . .
H39 H 0.378(7) 0.129(3) 0.856(2) 0.046(18) Uiso 1 1 d . . .
H44 H 0.161(9) -0.167(4) 0.949(3) 0.08(2) Uiso 1 1 d . . .
H47 H 0.477(11) 0.425(5) 0.730(4) 0.13(4) Uiso 1 1 d . . .
H49 H 0.662(8) 0.569(4) 0.750(3) 0.07(2) Uiso 1 1 d . . .
H52 H 0.900(8) 0.730(3) 0.513(3) 0.06(2) Uiso 1 1 d . . .
H1W1 H 0.995(13) 0.495(5) 0.733(5) 0.12(5) Uiso 1 1 d . . .
H2W1 H 0.969(13) 0.522(5) 0.779(5) 0.12(5) Uiso 1 1 d . . .
H1W2 H 1.003(9) 0.640(4) 0.858(3) 0.08(3) Uiso 1 1 d . . .
H2W2 H 0.922(10) 0.624(4) 0.810(3) 0.08(3) Uiso 1 1 d . . .
H1W3 H 0.669(14) 0.758(4) 0.940(5) 0.12(4) Uiso 1 1 d . . .
H2W3 H 0.526(14) 0.750(4) 0.925(5) 0.12(4) Uiso 1 1 d . . .
H1W4 H 0.33(2) 0.710(8) 0.896(7) 0.20(10) Uiso 1 1 d . . .
H2W4 H 0.31(2) 0.765(8) 0.885(8) 0.20(9) Uiso 1 1 d . . .
H1W5 H 0.091(18) 0.405(8) 0.718(6) 0.18(9) Uiso 1 1 d . . .
H2W5 H -0.044(17) 0.418(8) 0.692(6) 0.18(8) Uiso 1 1 d . . .
H1W6 H 0.348(19) 0.657(8) 0.831(7) 0.19(9) Uiso 1 1 d . . .
H2W6 H 0.211(18) 0.638(7) 0.831(6) 0.19(8) Uiso 1 1 d . . .
H1W7 H 0.99(3) 0.547(10) 0.857(9) 0.27(14) Uiso 1 1 d . . .
H2W7 H 0.94(3) 0.485(10) 0.868(9) 0.27(14) Uiso 1 1 d . . .
H1W8 H 0.22(3) 0.850(13) 0.857(12) 0.3(2) Uiso 1 1 d . . .
H2W8 H 0.34(3) 0.860(12) 0.819(11) 0.3(2) Uiso 1 1 d . . .


_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
C1 N1 1.505(5) . ?
C1 C2 1.541(5) . ?
C1 P2 1.847(4) . ?
C1 P1 1.852(4) . ?
C2 C3 1.531(6) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 P3 1.810(4) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 N2 1.319(7) . ?
C4 N5 1.356(8) . ?
C4 H4 0.9300 . ?
C6 N5 1.345(10) . ?
C6 C7 1.354(9) . ?
C6 H6 0.9300 . ?
C7 N2 1.370(7) . ?
C7 H7 0.9300 . ?
C9 N8 1.307(7) . ?
C9 N10 1.345(7) . ?
C9 H9 0.9300 . ?
C11 C12 1.364(8) . ?
C11 N10 1.371(8) . ?
C11 H11 0.9300 . ?
C12 N8 1.374(7) . ?
C12 H12 0.9300 . ?
C13 N13 1.316(6) . ?
C13 N14 1.325(7) . ?
C13 H13 0.9300 . ?
C15 N14 1.346(8) . ?
C15 C16 1.354(8) . ?
C15 H15 0.9300 . ?
C16 N13 1.361(7) . ?
C16 H16 0.9300 . ?
C18 N17 1.311(6) . ?
C18 N19 1.344(7) . ?
C18 H18 0.9300 . ?
C20 C21 1.353(9) . ?
C20 N19 1.360(7) . ?
C20 H20 0.9300 . ?
C21 N17 1.370(6) . ?
C21 H21 0.9300 . ?
C23 N22 1.319(6) . ?
C23 N24 1.341(7) . ?
C23 H23 0.9300 . ?
C25 C26 1.350(10) . ?
C25 N24 1.350(9) . ?
C25 H25 0.9300 . ?
C26 N22 1.363(7) . ?
C26 H26 0.9300 . ?
C28 N27 1.324(6) . ?
C28 N29 1.342(6) . ?
C28 H28 0.9300 . ?
C30 N29 1.357(7) . ?
C30 C31 1.358(8) . ?
C30 H30 0.9300 . ?
C31 N27 1.371(6) . ?
C31 H31 0.9300 . ?
C33 N32 1.314(7) . ?
C33 N34 1.335(8) . ?
C33 H33 0.9300 . ?
C35 N34 1.350(9) . ?
C35 C36 1.351(11) . ?
C35 H35 0.9300 . ?
C36 N32 1.364(7) . ?
C36 H36 0.9300 . ?
C38 N37 1.315(6) . ?
C38 N39 1.341(7) . ?
C38 H38 0.9300 . ?
C40 C41 1.355(8) . ?
C40 N39 1.358(7) . ?
C40 H40 0.9300 . ?
C41 N37 1.369(6) . ?
C41 H41 0.9300 . ?
C43 N42 1.327(7) . ?
C43 N44 1.330(8) . ?
C43 H43 0.9300 . ?
C45 C46 1.344(11) . ?
C45 N44 1.364(8) . ?
C45 H45 0.9300 . ?
C46 N42 1.363(7) . ?
C46 H46 0.9300 . ?
C48 N47 1.308(8) . ?
C48 N49 1.313(9) . ?
C48 H48 0.9324 . ?
C50 N49 1.321(11) . ?
C50 C51 1.348(10) . ?
C50 H50 0.9300 . ?
C51 N47 1.324(9) . ?
C51 H51 0.9300 . ?
C53 N54 1.324(7) . ?
C53 N52 1.331(7) . ?
C53 H53 0.9300 . ?
C55 C56 1.351(9) . ?
C55 N54 1.355(8) . ?
C55 H55 0.9300 . ?
C56 N52 1.344(9) . ?
C56 H56 0.9300 . ?
N1 Ni1 2.162(4) . ?
N1 H1A 0.9000 . ?
N1 H1B 0.9000 . ?
N2 Ni1 2.106(4) . ?
N5 H5 0.84(7) . ?
N8 Ni1 2.061(4) . ?
N10 H10 0.88(8) . ?
N13 Ni1 2.063(4) . ?
N14 H14 0.8600 . ?
N17 Ni2 2.125(4) . ?
N19 H19 0.84(9) . ?
N22 Ni2 2.136(4) . ?
N24 H24 0.82(8) . ?
N27 Ni2 2.117(4) . ?
N29 H29 0.88(7) . ?
N32 Ni3 2.104(4) . ?
N34 H34 0.82(8) . ?
N37 Ni3 2.120(4) . ?
N39 H39 0.80(6) . ?
N42 Ni3 2.134(4) . ?
N44 H44 0.95(8) . ?
N47 H47 0.91(11) . ?
N49 H49 0.78(8) . ?
N52 H52 0.74(8) . ?
Ni1 O4 2.107(3) . ?
Ni1 O1 2.141(3) . ?
Ni2 N27 2.117(4) 3_667 ?
Ni2 N17 2.125(4) 3_667 ?
Ni2 N22 2.136(4) 3_667 ?
Ni3 N32 2.104(4) 3_657 ?
Ni3 N37 2.120(4) 3_657 ?
Ni3 N42 2.134(4) 3_657 ?
O1 P1 1.517(3) . ?
O2 P1 1.552(3) . ?
O2 H1 0.79(8) . ?
O3 P1 1.510(3) . ?
O4 P2 1.524(3) . ?
O5 P2 1.531(3) . ?
O6 P2 1.507(3) . ?
O7 P3 1.527(3) . ?
O8 P3 1.514(4) . ?
O9 P3 1.526(3) . ?
O1W H1W1 0.84(12) . ?
O1W H2W1 0.86(13) . ?
O2W H1W2 0.85(9) . ?
O2W H2W2 0.85(9) . ?
O3W H1W3 0.82(13) . ?
O3W H2W3 0.85(14) . ?
O4W H1W4 0.84(18) . ?
O4W H2W4 0.85(18) . ?
O5W H1W5 0.86(16) . ?
O5W H2W5 0.82(16) . ?
O6W H1W6 0.87(17) . ?
O6W H2W6 0.86(17) . ?
O7W H1W7 0.8(2) . ?
O7W H2W7 0.9(2) . ?
O8W H1W8 0.8(3) . ?
O8W H2W8 0.9(3) . ?

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
N1 C1 C2 110.6(3) . . ?
N1 C1 P2 101.6(2) . . ?
C2 C1 P2 114.1(3) . . ?
N1 C1 P1 101.9(2) . . ?
C2 C1 P1 113.8(3) . . ?
P2 C1 P1 113.3(2) . . ?
C3 C2 C1 116.5(3) . . ?
C3 C2 H2A 108.2 . . ?
C1 C2 H2A 108.2 . . ?
C3 C2 H2B 108.2 . . ?
C1 C2 H2B 108.2 . . ?
H2A C2 H2B 107.3 . . ?
C2 C3 P3 113.5(3) . . ?
C2 C3 H3A 108.9 . . ?
P3 C3 H3A 108.9 . . ?
C2 C3 H3B 108.9 . . ?
P3 C3 H3B 108.9 . . ?
H3A C3 H3B 107.7 . . ?
N2 C4 N5 111.4(6) . . ?
N2 C4 H4 124.3 . . ?
N5 C4 H4 124.3 . . ?
N5 C6 C7 106.9(6) . . ?
N5 C6 H6 126.5 . . ?
C7 C6 H6 126.5 . . ?
C6 C7 N2 109.8(6) . . ?
C6 C7 H7 125.1 . . ?
N2 C7 H7 125.1 . . ?
N8 C9 N10 111.7(5) . . ?
N8 C9 H9 124.2 . . ?
N10 C9 H9 124.2 . . ?
C12 C11 N10 105.9(5) . . ?
C12 C11 H11 127.0 . . ?
N10 C11 H11 127.0 . . ?
C11 C12 N8 109.3(5) . . ?
C11 C12 H12 125.3 . . ?
N8 C12 H12 125.3 . . ?
N13 C13 N14 111.9(5) . . ?
N13 C13 H13 124.1 . . ?
N14 C13 H13 124.1 . . ?
N14 C15 C16 106.5(5) . . ?
N14 C15 H15 126.7 . . ?
C16 C15 H15 126.7 . . ?
C15 C16 N13 109.3(5) . . ?
C15 C16 H16 125.3 . . ?
N13 C16 H16 125.3 . . ?
N17 C18 N19 112.5(5) . . ?
N17 C18 H18 123.8 . . ?
N19 C18 H18 123.8 . . ?
C21 C20 N19 106.4(5) . . ?
C21 C20 H20 126.8 . . ?
N19 C20 H20 126.8 . . ?
C20 C21 N17 110.1(5) . . ?
C20 C21 H21 125.0 . . ?
N17 C21 H21 125.0 . . ?
N22 C23 N24 111.9(5) . . ?
N22 C23 H23 124.1 . . ?
N24 C23 H23 124.1 . . ?
C26 C25 N24 106.8(6) . . ?
C26 C25 H25 126.6 . . ?
N24 C25 H25 126.6 . . ?
C25 C26 N22 109.9(6) . . ?
C25 C26 H26 125.1 . . ?
N22 C26 H26 125.1 . . ?
N27 C28 N29 111.9(4) . . ?
N27 C28 H28 124.1 . . ?
N29 C28 H28 124.1 . . ?
N29 C30 C31 106.7(5) . . ?
N29 C30 H30 126.7 . . ?
C31 C30 H30 126.7 . . ?
C30 C31 N27 109.6(5) . . ?
C30 C31 H31 125.2 . . ?
N27 C31 H31 125.2 . . ?
N32 C33 N34 112.5(5) . . ?
N32 C33 H33 123.7 . . ?
N34 C33 H33 123.7 . . ?
N34 C35 C36 106.7(6) . . ?
N34 C35 H35 126.6 . . ?
C36 C35 H35 126.6 . . ?
C35 C36 N32 109.9(6) . . ?
C35 C36 H36 125.1 . . ?
N32 C36 H36 125.1 . . ?
N37 C38 N39 111.9(4) . . ?
N37 C38 H38 124.1 . . ?
N39 C38 H38 124.1 . . ?
C41 C40 N39 106.4(5) . . ?
C41 C40 H40 126.8 . . ?
N39 C40 H40 126.8 . . ?
C40 C41 N37 109.7(5) . . ?
C40 C41 H41 125.1 . . ?
N37 C41 H41 125.1 . . ?
N42 C43 N44 112.4(5) . . ?
N42 C43 H43 123.8 . . ?
N44 C43 H43 123.8 . . ?
C46 C45 N44 106.8(6) . . ?
C46 C45 H45 126.6 . . ?
N44 C45 H45 126.6 . . ?
C45 C46 N42 110.2(6) . . ?
C45 C46 H46 124.9 . . ?
N42 C46 H46 124.9 . . ?
N47 C48 N49 111.3(7) . . ?
N47 C48 H48 124.5 . . ?
N49 C48 H48 124.2 . . ?
N49 C50 C51 108.0(7) . . ?
N49 C50 H50 126.0 . . ?
C51 C50 H50 126.0 . . ?
N47 C51 C50 107.9(7) . . ?
N47 C51 H51 126.0 . . ?
C50 C51 H51 126.0 . . ?
N54 C53 N52 111.7(6) . . ?
N54 C53 H53 124.1 . . ?
N52 C53 H53 124.1 . . ?
C56 C55 N54 109.5(6) . . ?
C56 C55 H55 125.2 . . ?
N54 C55 H55 125.2 . . ?
N52 C56 C55 107.0(6) . . ?
N52 C56 H56 126.5 . . ?
C55 C56 H56 126.5 . . ?
C1 N1 Ni1 103.8(2) . . ?
C1 N1 H1A 111.0 . . ?
Ni1 N1 H1A 111.0 . . ?
C1 N1 H1B 111.0 . . ?
Ni1 N1 H1B 111.0 . . ?
H1A N1 H1B 109.0 . . ?
C4 N2 C7 104.9(5) . . ?
C4 N2 Ni1 129.0(4) . . ?
C7 N2 Ni1 126.0(4) . . ?
C6 N5 C4 106.9(6) . . ?
C6 N5 H5 124(5) . . ?
C4 N5 H5 129(5) . . ?
C9 N8 C12 106.0(4) . . ?
C9 N8 Ni1 125.0(4) . . ?
C12 N8 Ni1 128.9(4) . . ?
C9 N10 C11 107.1(5) . . ?
C9 N10 H10 124(5) . . ?
C11 N10 H10 129(5) . . ?
C13 N13 C16 105.0(4) . . ?
C13 N13 Ni1 128.4(4) . . ?
C16 N13 Ni1 126.6(3) . . ?
C13 N14 C15 107.2(5) . . ?
C13 N14 H14 126.4 . . ?
C15 N14 H14 126.4 . . ?
C18 N17 C21 104.6(4) . . ?
C18 N17 Ni2 125.4(3) . . ?
C21 N17 Ni2 129.2(4) . . ?
C18 N19 C20 106.4(5) . . ?
C18 N19 H19 135(6) . . ?
C20 N19 H19 118(6) . . ?
C23 N22 C26 104.8(5) . . ?
C23 N22 Ni2 127.6(3) . . ?
C26 N22 Ni2 127.2(4) . . ?
C23 N24 C25 106.7(5) . . ?
C23 N24 H24 131(6) . . ?
C25 N24 H24 123(6) . . ?
C28 N27 C31 104.9(4) . . ?
C28 N27 Ni2 126.6(3) . . ?
C31 N27 Ni2 127.2(3) . . ?
C28 N29 C30 106.9(5) . . ?
C28 N29 H29 124(5) . . ?
C30 N29 H29 129(5) . . ?
C33 N32 C36 104.4(5) . . ?
C33 N32 Ni3 126.0(3) . . ?
C36 N32 Ni3 129.5(4) . . ?
C33 N34 C35 106.5(6) . . ?
C33 N34 H34 124(6) . . ?
C35 N34 H34 128(6) . . ?
C38 N37 C41 105.1(4) . . ?
C38 N37 Ni3 125.0(3) . . ?
C41 N37 Ni3 129.1(3) . . ?
C38 N39 C40 106.9(5) . . ?
C38 N39 H39 123(5) . . ?
C40 N39 H39 129(5) . . ?
C43 N42 C46 104.4(5) . . ?
C43 N42 Ni3 127.0(4) . . ?
C46 N42 Ni3 128.2(4) . . ?
C43 N44 C45 106.3(6) . . ?
C43 N44 H44 125(5) . . ?
C45 N44 H44 129(5) . . ?
C48 N47 C51 106.4(6) . . ?
C48 N47 H47 135(7) . . ?
C51 N47 H47 118(7) . . ?
C48 N49 C50 106.3(6) . . ?
C48 N49 H49 135(6) . . ?
C50 N49 H49 119(6) . . ?
C53 N52 C56 106.8(5) . . ?
C53 N52 H52 143(6) . . ?
C56 N52 H52 110(6) . . ?
C53 N54 C55 104.9(5) . . ?
N8 Ni1 N13 93.38(16) . . ?
N8 Ni1 N2 91.60(17) . . ?
N13 Ni1 N2 93.45(16) . . ?
N8 Ni1 O4 88.11(14) . . ?
N13 Ni1 O4 89.53(14) . . ?
N2 Ni1 O4 177.02(15) . . ?
N8 Ni1 O1 91.56(14) . . ?
N13 Ni1 O1 173.39(14) . . ?
N2 Ni1 O1 90.79(15) . . ?
O4 Ni1 O1 86.25(12) . . ?
N8 Ni1 N1 168.34(15) . . ?
N13 Ni1 N1 95.42(15) . . ?
N2 Ni1 N1 95.49(15) . . ?
O4 Ni1 N1 84.33(12) . . ?
O1 Ni1 N1 79.11(12) . . ?
N27 Ni2 N27 180.000(1) . 3_667 ?
N27 Ni2 N17 90.96(14) . . ?
N27 Ni2 N17 89.04(14) 3_667 . ?
N27 Ni2 N17 89.04(14) . 3_667 ?
N27 Ni2 N17 90.96(14) 3_667 3_667 ?
N17 Ni2 N17 180.000(1) . 3_667 ?
N27 Ni2 N22 90.05(14) . . ?
N27 Ni2 N22 89.95(14) 3_667 . ?
N17 Ni2 N22 89.57(14) . . ?
N17 Ni2 N22 90.43(14) 3_667 . ?
N27 Ni2 N22 89.95(14) . 3_667 ?
N27 Ni2 N22 90.05(14) 3_667 3_667 ?
N17 Ni2 N22 90.43(14) . 3_667 ?
N17 Ni2 N22 89.57(14) 3_667 3_667 ?
N22 Ni2 N22 180.0(2) . 3_667 ?
N32 Ni3 N32 180.00(15) . 3_657 ?
N32 Ni3 N37 90.60(14) . . ?
N32 Ni3 N37 89.40(14) 3_657 . ?
N32 Ni3 N37 89.40(14) . 3_657 ?
N32 Ni3 N37 90.60(14) 3_657 3_657 ?
N37 Ni3 N37 180.00(14) . 3_657 ?
N32 Ni3 N42 90.70(15) . 3_657 ?
N32 Ni3 N42 89.30(15) 3_657 3_657 ?
N37 Ni3 N42 91.05(14) . 3_657 ?
N37 Ni3 N42 88.95(14) 3_657 3_657 ?
N32 Ni3 N42 89.30(15) . . ?
N32 Ni3 N42 90.70(15) 3_657 . ?
N37 Ni3 N42 88.95(14) . . ?
N37 Ni3 N42 91.05(14) 3_657 . ?
N42 Ni3 N42 180.00(15) 3_657 . ?
P1 O1 Ni1 115.25(16) . . ?
P1 O2 H1 122(6) . . ?
P2 O4 Ni1 113.28(16) . . ?
H1W1 O1W H2W1 115(10) . . ?
H1W2 O2W H2W2 116(8) . . ?
H1W3 O3W H2W3 108(10) . . ?
H1W4 O4W H2W4 105(10) . . ?
H1W5 O5W H2W5 113(10) . . ?
H1W6 O6W H2W6 103(10) . . ?
H1W7 O7W H2W7 131(10) . . ?
H1W8 O8W H2W8 144(10) . . ?
O3 P1 O1 114.48(19) . . ?
O3 P1 O2 109.9(2) . . ?
O1 P1 O2 110.73(19) . . ?
O3 P1 C1 107.55(18) . . ?
O1 P1 C1 105.05(17) . . ?
O2 P1 C1 108.82(18) . . ?
O6 P2 O4 113.15(18) . . ?
O6 P2 O5 111.8(2) . . ?
O4 P2 O5 112.21(19) . . ?
O6 P2 C1 113.63(18) . . ?
O4 P2 C1 102.25(17) . . ?
O5 P2 C1 103.01(18) . . ?
O8 P3 O9 111.1(2) . . ?
O8 P3 O7 112.1(2) . . ?
O9 P3 O7 111.4(2) . . ?
O8 P3 C3 107.7(2) . . ?
O9 P3 C3 107.4(2) . . ?
O7 P3 C3 106.93(19) . . ?

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
N1 C1 C2 C3 -179.0(3) . . . . ?
P2 C1 C2 C3 -65.2(4) . . . . ?
P1 C1 C2 C3 67.0(4) . . . . ?
C1 C2 C3 P3 -172.5(3) . . . . ?
N5 C6 C7 N2 0.8(8) . . . . ?
N10 C11 C12 N8 -0.6(8) . . . . ?
N14 C15 C16 N13 0.6(8) . . . . ?
N19 C20 C21 N17 0.0(6) . . . . ?
N24 C25 C26 N22 0.3(7) . . . . ?
N29 C30 C31 N27 1.2(6) . . . . ?
N34 C35 C36 N32 0.2(8) . . . . ?
N39 C40 C41 N37 0.1(6) . . . . ?
N44 C45 C46 N42 -0.6(7) . . . . ?
N49 C50 C51 N47 0.3(13) . . . . ?
N54 C55 C56 N52 0.4(7) . . . . ?
C2 C1 N1 Ni1 178.7(2) . . . . ?
P2 C1 N1 Ni1 57.3(2) . . . . ?
P1 C1 N1 Ni1 -59.9(2) . . . . ?
N5 C4 N2 C7 0.9(7) . . . . ?
N5 C4 N2 Ni1 -178.6(4) . . . . ?
C6 C7 N2 C4 -1.0(7) . . . . ?
C6 C7 N2 Ni1 178.4(5) . . . . ?
C7 C6 N5 C4 -0.2(8) . . . . ?
N2 C4 N5 C6 -0.4(8) . . . . ?
N10 C9 N8 C12 -0.4(6) . . . . ?
N10 C9 N8 Ni1 177.6(3) . . . . ?
C11 C12 N8 C9 0.6(7) . . . . ?
C11 C12 N8 Ni1 -177.3(4) . . . . ?
N8 C9 N10 C11 0.0(6) . . . . ?
C12 C11 N10 C9 0.4(7) . . . . ?
N14 C13 N13 C16 0.0(6) . . . . ?
N14 C13 N13 Ni1 -177.9(3) . . . . ?
C15 C16 N13 C13 -0.4(7) . . . . ?
C15 C16 N13 Ni1 177.5(4) . . . . ?
N13 C13 N14 C15 0.4(7) . . . . ?
C16 C15 N14 C13 -0.6(7) . . . . ?
N19 C18 N17 C21 0.5(6) . . . . ?
N19 C18 N17 Ni2 -170.1(3) . . . . ?
C20 C21 N17 C18 -0.3(6) . . . . ?
C20 C21 N17 Ni2 169.8(4) . . . . ?
N17 C18 N19 C20 -0.5(6) . . . . ?
C21 C20 N19 C18 0.3(6) . . . . ?
N24 C23 N22 C26 0.0(6) . . . . ?
N24 C23 N22 Ni2 173.1(3) . . . . ?
C25 C26 N22 C23 -0.2(6) . . . . ?
C25 C26 N22 Ni2 -173.3(4) . . . . ?
N22 C23 N24 C25 0.2(6) . . . . ?
C26 C25 N24 C23 -0.3(7) . . . . ?
N29 C28 N27 C31 0.4(5) . . . . ?
N29 C28 N27 Ni2 -167.7(3) . . . . ?
C30 C31 N27 C28 -1.0(5) . . . . ?
C30 C31 N27 Ni2 167.0(3) . . . . ?
N27 C28 N29 C30 0.4(6) . . . . ?
C31 C30 N29 C28 -1.0(6) . . . . ?
N34 C33 N32 C36 0.4(6) . . . . ?
N34 C33 N32 Ni3 177.5(3) . . . . ?
C35 C36 N32 C33 -0.4(7) . . . . ?
C35 C36 N32 Ni3 -177.4(4) . . . . ?
N32 C33 N34 C35 -0.3(7) . . . . ?
C36 C35 N34 C33 0.0(7) . . . . ?
N39 C38 N37 C41 -0.2(5) . . . . ?
N39 C38 N37 Ni3 170.7(3) . . . . ?
C40 C41 N37 C38 0.1(6) . . . . ?
C40 C41 N37 Ni3 -170.3(4) . . . . ?
N37 C38 N39 C40 0.2(6) . . . . ?
C41 C40 N39 C38 -0.2(6) . . . . ?
N44 C43 N42 C46 -1.0(6) . . . . ?
N44 C43 N42 Ni3 -174.1(3) . . . . ?
C45 C46 N42 C43 0.9(6) . . . . ?
C45 C46 N42 Ni3 174.0(4) . . . . ?
N42 C43 N44 C45 0.6(6) . . . . ?
C46 C45 N44 C43 0.0(7) . . . . ?
N49 C48 N47 C51 -0.4(9) . . . . ?
C50 C51 N47 C48 0.1(11) . . . . ?
N47 C48 N49 C50 0.5(10) . . . . ?
C51 C50 N49 C48 -0.5(12) . . . . ?
N54 C53 N52 C56 -0.2(7) . . . . ?
C55 C56 N52 C53 -0.1(7) . . . . ?
N52 C53 N54 C55 0.5(7) . . . . ?
C56 C55 N54 C53 -0.5(7) . . . . ?
C9 N8 Ni1 N13 149.4(4) . . . . ?
C12 N8 Ni1 N13 -33.1(5) . . . . ?
C9 N8 Ni1 N2 -117.1(4) . . . . ?
C12 N8 Ni1 N2 60.4(5) . . . . ?
C9 N8 Ni1 O4 59.9(4) . . . . ?
C12 N8 Ni1 O4 -122.5(5) . . . . ?
C9 N8 Ni1 O1 -26.3(4) . . . . ?
C12 N8 Ni1 O1 151.3(5) . . . . ?
C9 N8 Ni1 N1 10.4(10) . . . . ?
C12 N8 Ni1 N1 -172.1(7) . . . . ?
C13 N13 Ni1 N8 118.9(4) . . . . ?
C16 N13 Ni1 N8 -58.5(5) . . . . ?
C13 N13 Ni1 N2 27.1(4) . . . . ?
C16 N13 Ni1 N2 -150.3(5) . . . . ?
C13 N13 Ni1 O4 -153.0(4) . . . . ?
C16 N13 Ni1 O4 29.6(5) . . . . ?
C13 N13 Ni1 O1 -102.7(13) . . . . ?
C16 N13 Ni1 O1 79.9(14) . . . . ?
C13 N13 Ni1 N1 -68.8(4) . . . . ?
C16 N13 Ni1 N1 113.8(5) . . . . ?
C4 N2 Ni1 N8 -158.3(5) . . . . ?
C7 N2 Ni1 N8 22.4(5) . . . . ?
C4 N2 Ni1 N13 -64.8(5) . . . . ?
C7 N2 Ni1 N13 115.9(5) . . . . ?
C4 N2 Ni1 O4 117(3) . . . . ?
C7 N2 Ni1 O4 -62(3) . . . . ?
C4 N2 Ni1 O1 110.1(5) . . . . ?
C7 N2 Ni1 O1 -69.2(5) . . . . ?
C4 N2 Ni1 N1 31.0(5) . . . . ?
C7 N2 Ni1 N1 -148.4(5) . . . . ?
C1 N1 Ni1 N8 13.8(9) . . . . ?
C1 N1 Ni1 N13 -125.0(2) . . . . ?
C1 N1 Ni1 N2 140.9(2) . . . . ?
C1 N1 Ni1 O4 -36.1(2) . . . . ?
C1 N1 Ni1 O1 51.2(2) . . . . ?
C28 N27 Ni2 N27 10(100) . . . 3_667 ?
C31 N27 Ni2 N27 -156(100) . . . 3_667 ?
C28 N27 Ni2 N17 -91.9(4) . . . . ?
C31 N27 Ni2 N17 102.7(4) . . . . ?
C28 N27 Ni2 N17 88.1(4) . . . 3_667 ?
C31 N27 Ni2 N17 -77.3(4) . . . 3_667 ?
C28 N27 Ni2 N22 178.5(4) . . . . ?
C31 N27 Ni2 N22 13.1(4) . . . . ?
C28 N27 Ni2 N22 -1.5(4) . . . 3_667 ?
C31 N27 Ni2 N22 -166.9(4) . . . 3_667 ?
C18 N17 Ni2 N27 -3.1(4) . . . . ?
C21 N17 Ni2 N27 -171.4(4) . . . . ?
C18 N17 Ni2 N27 176.9(4) . . . 3_667 ?
C21 N17 Ni2 N27 8.6(4) . . . 3_667 ?
C18 N17 Ni2 N17 -86(32) . . . 3_667 ?
C21 N17 Ni2 N17 105(32) . . . 3_667 ?
C18 N17 Ni2 N22 86.9(4) . . . . ?
C21 N17 Ni2 N22 -81.3(4) . . . . ?
C18 N17 Ni2 N22 -93.1(4) . . . 3_667 ?
C21 N17 Ni2 N22 98.7(4) . . . 3_667 ?
C23 N22 Ni2 N27 -83.7(4) . . . . ?
C26 N22 Ni2 N27 87.9(4) . . . . ?
C23 N22 Ni2 N27 96.3(4) . . . 3_667 ?
C26 N22 Ni2 N27 -92.1(4) . . . 3_667 ?
C23 N22 Ni2 N17 -174.7(4) . . . . ?
C26 N22 Ni2 N17 -3.1(4) . . . . ?
C23 N22 Ni2 N17 5.3(4) . . . 3_667 ?
C26 N22 Ni2 N17 176.9(4) . . . 3_667 ?
C23 N22 Ni2 N22 -131(14) . . . 3_667 ?
C26 N22 Ni2 N22 41(14) . . . 3_667 ?
C33 N32 Ni3 N32 134(73) . . . 3_657 ?
C36 N32 Ni3 N32 -50(73) . . . 3_657 ?
C33 N32 Ni3 N37 -11.8(4) . . . . ?
C36 N32 Ni3 N37 164.6(5) . . . . ?
C33 N32 Ni3 N37 168.2(4) . . . 3_657 ?
C36 N32 Ni3 N37 -15.4(5) . . . 3_657 ?
C33 N32 Ni3 N42 79.3(4) . . . 3_657 ?
C36 N32 Ni3 N42 -104.3(5) . . . 3_657 ?
C33 N32 Ni3 N42 -100.7(4) . . . . ?
C36 N32 Ni3 N42 75.7(5) . . . . ?
C38 N37 Ni3 N32 92.5(4) . . . . ?
C41 N37 Ni3 N32 -99.0(4) . . . . ?
C38 N37 Ni3 N32 -87.5(4) . . . 3_657 ?
C41 N37 Ni3 N32 81.0(4) . . . 3_657 ?
C38 N37 Ni3 N37 139(100) . . . 3_657 ?
C41 N37 Ni3 N37 -52(100) . . . 3_657 ?
C38 N37 Ni3 N42 1.7(4) . . . 3_657 ?
C41 N37 Ni3 N42 170.3(4) . . . 3_657 ?
C38 N37 Ni3 N42 -178.3(4) . . . . ?
C41 N37 Ni3 N42 -9.7(4) . . . . ?
C43 N42 Ni3 N32 -179.6(4) . . . . ?
C46 N42 Ni3 N32 8.9(4) . . . . ?
C43 N42 Ni3 N32 0.4(4) . . . 3_657 ?
C46 N42 Ni3 N32 -171.1(4) . . . 3_657 ?
C43 N42 Ni3 N37 89.8(4) . . . . ?
C46 N42 Ni3 N37 -81.8(4) . . . . ?
C43 N42 Ni3 N37 -90.2(4) . . . 3_657 ?
C46 N42 Ni3 N37 98.2(4) . . . 3_657 ?
C43 N42 Ni3 N42 -43(17) . . . 3_657 ?
C46 N42 Ni3 N42 145(17) . . . 3_657 ?
N8 Ni1 O1 P1 146.3(2) . . . . ?
N13 Ni1 O1 P1 7.8(14) . . . . ?
N2 Ni1 O1 P1 -122.1(2) . . . . ?
O4 Ni1 O1 P1 58.3(2) . . . . ?
N1 Ni1 O1 P1 -26.66(19) . . . . ?
N8 Ni1 O4 P2 -171.9(2) . . . . ?
N13 Ni1 O4 P2 94.6(2) . . . . ?
N2 Ni1 O4 P2 -88(3) . . . . ?
O1 Ni1 O4 P2 -80.26(19) . . . . ?
N1 Ni1 O4 P2 -0.84(19) . . . . ?
Ni1 O1 P1 O3 118.2(2) . . . . ?
Ni1 O1 P1 O2 -116.8(2) . . . . ?
Ni1 O1 P1 C1 0.5(2) . . . . ?
N1 C1 P1 O3 -83.1(3) . . . . ?
C2 C1 P1 O3 36.0(3) . . . . ?
P2 C1 P1 O3 168.6(2) . . . . ?
N1 C1 P1 O1 39.3(3) . . . . ?
C2 C1 P1 O1 158.4(3) . . . . ?
P2 C1 P1 O1 -69.1(2) . . . . ?
N1 C1 P1 O2 157.9(2) . . . . ?
C2 C1 P1 O2 -83.0(3) . . . . ?
P2 C1 P1 O2 49.5(3) . . . . ?
Ni1 O4 P2 O6 152.36(17) . . . . ?
Ni1 O4 P2 O5 -80.0(2) . . . . ?
Ni1 O4 P2 C1 29.7(2) . . . . ?
N1 C1 P2 O6 179.2(2) . . . . ?
C2 C1 P2 O6 60.2(3) . . . . ?
P1 C1 P2 O6 -72.2(3) . . . . ?
N1 C1 P2 O4 -58.5(3) . . . . ?
C2 C1 P2 O4 -177.5(3) . . . . ?
P1 C1 P2 O4 50.1(2) . . . . ?
N1 C1 P2 O5 58.0(3) . . . . ?
C2 C1 P2 O5 -61.0(3) . . . . ?
P1 C1 P2 O5 166.6(2) . . . . ?
C2 C3 P3 O8 -175.2(3) . . . . ?
C2 C3 P3 O9 -55.5(4) . . . . ?
C2 C3 P3 O7 64.2(3) . . . . ?

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
O1W H2W1 O7W 0.86(13) 1.93(13) 2.79(3) 179(13) .
O1W H1W1 O5W 0.84(12) 1.83(12) 2.675(15) 180(14) 1_655
O2W H1W2 O7 0.85(9) 1.97(9) 2.799(7) 165(8) .
O2W H2W2 O3 0.85(9) 1.91(9) 2.746(6) 168(8) .
O3W H1W3 O9 0.82(13) 2.02(13) 2.810(9) 160(12) .
O3W H2W3 O4W 0.85(14) 1.93(14) 2.761(15) 167(12) .
O4W H2W4 O8 0.85(18) 2.0(2) 2.637(13) 131(20) 1_455
O4W H2W4 O8W 0.85(18) 2.7(2) 3.27(3) 128(19) .
O5W H1W5 O6 0.86(16) 1.83(16) 2.69(2) 178(20) 2_646
O5W H2W5 O8W 0.82(16) 2.44(18) 3.24(4) 165(18) 2_546
O6W H1W6 O4W 0.87(17) 2.26(18) 2.83(3) 123(16) .
O6W H2W6 O2W 0.86(17) 1.99(17) 2.761(17) 150(17) 1_455
O7W H1W7 O2W 0.8(2) 1.9(2) 2.67(3) 143(24) .
O8W H1W8 O8 0.8(3) 2.6(3) 3.36(4) 152(26) 1_455
O8W H2W8 O5 0.9(3) 2.4(3) 3.29(5) 177(25) .
N14 H14 O6 0.86 1.84 2.699(5) 177.8 1_455
N52 H52 O9 0.74(8) 2.00(8) 2.733(6) 168(8) 4_575
N49 H49 O3 0.78(8) 1.98(8) 2.740(6) 165(8) .
N47 H47 O5 0.91(11) 1.66(11) 2.567(6) 172(11) 2_646
N44 H44 O8 0.95(8) 1.76(8) 2.709(7) 173(7) 1_445
N39 H39 O1 0.80(6) 1.90(7) 2.689(6) 168(7) 2_646
N34 H34 O9 0.82(8) 1.96(8) 2.714(7) 153(8) 3_667
N29 H29 O4 0.88(7) 1.79(7) 2.662(6) 169(7) 2_646
N24 H24 O7 0.82(8) 1.93(8) 2.743(6) 171(8) 1_455
N19 H19 O7 0.84(9) 1.89(9) 2.722(6) 167(8) 3_667
N10 H10 O3W 0.88(8) 1.88(8) 2.744(8) 168(7) 4_575
N5 H5 O1W 0.84(7) 1.98(8) 2.808(10) 171(7) 1_455
O2 H1 N54 0.79(8) 1.83(9) 2.615(6) 174(9) .

_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_theta_full        28.00
_diffrn_measured_fraction_theta_full 0.995
_refine_diff_density_max         2.060
_refine_diff_density_min         -1.655
_refine_diff_density_rms         0.125


