# Electronic Supplementary Material (ESI) for Dalton Transactions
# This journal is © The Royal Society of Chemistry 2013

#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_sad

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C28 H30 N4 Ni2 O11 P2'
_chemical_formula_sum            'C28 H30 N4 Ni2 O11 P2'
_chemical_formula_weight         777.92

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'

_space_group_crystal_system      triclinic
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

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

_cell_length_a                   13.9378(9)
_cell_length_b                   15.0600(10)
_cell_length_c                   17.7091(11)
_cell_angle_alpha                72.853(2)
_cell_angle_beta                 71.471(3)
_cell_angle_gamma                64.941(3)
_cell_volume                     3136.7(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    8103
_cell_measurement_theta_min      2.468
_cell_measurement_theta_max      27.828

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.643
_exptl_crystal_F_000             1600
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_exptl_absorpt_coefficient_mu    1.369
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.725
_exptl_absorpt_correction_T_max  0.876
_exptl_absorpt_process_details   'SADABS(Bruker, 2000)'

_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  'Bruker APEX II'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            19145
_diffrn_reflns_av_R_equivalents  0.0031
_diffrn_reflns_av_unetI/netI     0.0733
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         1.52
_diffrn_reflns_theta_max         26.00
_reflns_number_total             12228
_reflns_number_gt                8788
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'SMART (Bruker, 2000)'
_computing_cell_refinement       SMART
_computing_data_reduction        'SAINT (Bruker, 2000)'
_computing_structure_solution    SHELXL-2013
_computing_structure_refinement  SHELXL-2013
_computing_molecular_graphics    SHELXL-2013
_computing_publication_material  SHELXL-2013

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0500P)^2^+0.5500P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         12228
_refine_ls_number_parameters     847
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0559
_refine_ls_R_factor_gt           0.0503
_refine_ls_wR_factor_ref         0.1238
_refine_ls_wR_factor_gt          0.1228
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_restrained_S_all      1.051
_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 0.58226(4) -0.01125(4) 0.35562(3) 0.02553(13) Uani 1 1 d . . .
Ni2 Ni 0.37978(4) 0.09184(4) 0.10960(3) 0.02538(13) Uani 1 1 d . . .
Ni3 Ni 0.87718(4) 0.59101(4) 0.40704(3) 0.02712(13) Uani 1 1 d . . .
Ni4 Ni 1.07857(4) 0.48991(4) 0.10988(3) 0.02614(13) Uani 1 1 d . . .
P1 P 0.40267(9) 0.14268(8) 0.45386(6) 0.0263(2) Uani 1 1 d . . .
P2 P 0.44096(9) 0.14526(8) -0.07378(6) 0.0285(2) Uani 1 1 d . . .
P3 P 0.93950(9) 0.64602(8) 0.53122(6) 0.0274(2) Uani 1 1 d . . .
P4 P 0.90348(9) 0.64448(8) 0.02052(6) 0.0264(2) Uani 1 1 d . . .
C1 C 0.3472(4) 0.0824(3) 0.4125(3) 0.0369(10) Uani 1 1 d . . .
H1A H 0.2811 0.0759 0.4494 0.044 Uiso 1 1 calc R . .
H1B H 0.3302 0.1217 0.3610 0.044 Uiso 1 1 calc R . .
C2 C 0.5116(4) -0.1407(3) 0.3141(2) 0.0347(10) Uani 1 1 d . . .
C3 C 0.4048(4) -0.0747(3) 0.3626(3) 0.0381(11) Uani 1 1 d . . .
H3 H 0.3676 -0.0255 0.3208 0.046 Uiso 1 1 calc R . .
C4 C 0.3266(4) -0.1263(3) 0.4122(3) 0.0356(10) Uani 1 1 d . . .
C5 C 0.3285(4) -0.1766(3) 0.4909(2) 0.0419(11) Uani 1 1 d . . .
H5 H 0.3835 -0.1857 0.5146 0.050 Uiso 1 1 calc R . .
C6 C 0.2462(4) -0.2137(4) 0.5344(3) 0.0496(13) Uani 1 1 d . . .
H6 H 0.2470 -0.2481 0.5874 0.059 Uiso 1 1 calc R . .
C7 C 0.1632(4) -0.1999(4) 0.4998(3) 0.0479(13) Uani 1 1 d . . .
H7 H 0.1087 -0.2247 0.5297 0.057 Uiso 1 1 calc R . .
C8 C 0.1619(4) -0.1501(3) 0.4222(3) 0.0475(12) Uani 1 1 d . . .
H8 H 0.1059 -0.1405 0.3993 0.057 Uiso 1 1 calc R . .
C9 C 0.2437(4) -0.1135(3) 0.3766(3) 0.0484(13) Uani 1 1 d . . .
H9 H 0.2434 -0.0809 0.3231 0.058 Uiso 1 1 calc R . .
C10 C 0.8016(4) -0.0330(3) 0.2508(3) 0.0449(12) Uani 1 1 d . . .
H10 H 0.7767 -0.0539 0.2187 0.054 Uiso 1 1 calc R . .
C11 C 0.9040(4) -0.0252(4) 0.2217(3) 0.0436(12) Uani 1 1 d . . .
H11 H 0.9454 -0.0418 0.1717 0.052 Uiso 1 1 calc R . .
C12 C 0.9451(4) 0.0067(3) 0.2662(2) 0.0344(10) Uani 1 1 d . . .
C13 C 0.8782(4) 0.0261(4) 0.3427(3) 0.0470(13) Uani 1 1 d . . .
H13 H 0.9006 0.0452 0.3775 0.056 Uiso 1 1 calc R . .
C14 C 0.7780(4) 0.0158(3) 0.3646(3) 0.0397(11) Uani 1 1 d . . .
H14 H 0.7345 0.0302 0.4148 0.048 Uiso 1 1 calc R . .
C15 C 0.4983(4) 0.1971(3) -0.0273(2) 0.0386(11) Uani 1 1 d . . .
H15A H 0.5668 0.2010 -0.0614 0.046 Uiso 1 1 calc R . .
H15B H 0.4490 0.2634 -0.0179 0.046 Uiso 1 1 calc R . .
C16 C 0.5180(4) 0.1011(3) 0.1938(3) 0.0379(11) Uani 1 1 d . . .
C17 C 0.5505(4) 0.1561(3) 0.1065(2) 0.0363(10) Uani 1 1 d . . .
H17 H 0.5066 0.2269 0.1066 0.044 Uiso 1 1 calc R . .
C18 C 0.6646(4) 0.1505(3) 0.0740(2) 0.0371(10) Uani 1 1 d . . .
C19 C 0.7477(4) 0.0617(4) 0.0639(3) 0.0475(12) Uani 1 1 d . . .
H19 H 0.7341 0.0027 0.0835 0.057 Uiso 1 1 calc R . .
C20 C 0.8533(4) 0.0583(4) 0.0244(3) 0.0473(12) Uani 1 1 d . . .
H20 H 0.9089 -0.0027 0.0168 0.057 Uiso 1 1 calc R . .
C21 C 0.8750(4) 0.1450(4) -0.0034(3) 0.0442(12) Uani 1 1 d . . .
H21 H 0.9459 0.1421 -0.0274 0.053 Uiso 1 1 calc R . .
C22 C 0.7928(4) 0.2352(4) 0.0042(3) 0.0526(13) Uani 1 1 d . . .
H22 H 0.8067 0.2940 -0.0172 0.063 Uiso 1 1 calc R . .
C23 C 0.6874(4) 0.2383(4) 0.0445(3) 0.0519(13) Uani 1 1 d . . .
H23 H 0.6318 0.2994 0.0517 0.062 Uiso 1 1 calc R . .
C24 C 0.2187(4) 0.0009(3) 0.1406(3) 0.0372(10) Uani 1 1 d . . .
H24 H 0.2696 -0.0301 0.0986 0.045 Uiso 1 1 calc R . .
C25 C 0.1247(4) -0.0190(3) 0.1710(3) 0.0386(11) Uani 1 1 d . . .
H25 H 0.1131 -0.0620 0.1493 0.046 Uiso 1 1 calc R . .
C26 C 0.0467(4) 0.0254(3) 0.2342(2) 0.0345(10) Uani 1 1 d . . .
C27 C 0.0681(4) 0.0906(3) 0.2610(3) 0.0405(11) Uani 1 1 d . . .
H27 H 0.0173 0.1239 0.3019 0.049 Uiso 1 1 calc R . .
C28 C 0.1644(4) 0.1069(3) 0.2279(3) 0.0392(11) Uani 1 1 d . . .
H28 H 0.1773 0.1508 0.2475 0.047 Uiso 1 1 calc R . .
C29 C 0.9959(4) 0.6986(3) 0.4284(2) 0.0355(10) Uani 1 1 d . . .
H29A H 0.9456 0.7642 0.4101 0.043 Uiso 1 1 calc R . .
H29B H 1.0641 0.7036 0.4254 0.043 Uiso 1 1 calc R . .
C30 C 1.0148(4) 0.5996(3) 0.2488(3) 0.0376(10) Uani 1 1 d . . .
C31 C 1.0517(4) 0.6526(3) 0.2914(2) 0.0351(10) Uani 1 1 d . . .
H31 H 1.0130 0.7243 0.2758 0.042 Uiso 1 1 calc R . .
C32 C 1.1697(4) 0.6367(3) 0.2698(3) 0.0406(11) Uani 1 1 d . . .
C33 C 1.2061(5) 0.7169(4) 0.2346(3) 0.0618(16) Uani 1 1 d . . .
H33 H 1.1576 0.7796 0.2169 0.074 Uiso 1 1 calc R . .
C34 C 1.3140(5) 0.7035(4) 0.2260(3) 0.0528(13) Uani 1 1 d . . .
H34 H 1.3363 0.7577 0.2042 0.063 Uiso 1 1 calc R . .
C35 C 1.3889(4) 0.6097(4) 0.2497(3) 0.0539(14) Uani 1 1 d . . .
H35 H 1.4611 0.6003 0.2436 0.065 Uiso 1 1 calc R . .
C36 C 1.3528(4) 0.5320(4) 0.2822(3) 0.0491(12) Uani 1 1 d . . .
H36 H 1.4022 0.4688 0.2974 0.059 Uiso 1 1 calc R . .
C37 C 1.2446(4) 0.5441(4) 0.2932(3) 0.0449(12) Uani 1 1 d . . .
H37 H 1.2229 0.4897 0.3165 0.054 Uiso 1 1 calc R . .
C38 C 0.6523(4) 0.6059(4) 0.4017(3) 0.0495(13) Uani 1 1 d . . .
H38 H 0.6578 0.6569 0.3575 0.059 Uiso 1 1 calc R . .
C39 C 0.5620(4) 0.5908(4) 0.4232(3) 0.0461(12) Uani 1 1 d . . .
H39 H 0.5058 0.6315 0.3968 0.055 Uiso 1 1 calc R . .
C40 C 0.5498(4) 0.5120(3) 0.4872(2) 0.0359(10) Uani 1 1 d . . .
C41 C 0.6386(4) 0.4564(4) 0.5199(3) 0.0475(12) Uani 1 1 d . . .
H41 H 0.6371 0.4009 0.5603 0.057 Uiso 1 1 calc R . .
C42 C 0.7290(4) 0.4799(3) 0.4949(3) 0.0440(12) Uani 1 1 d . . .
H42 H 0.7863 0.4406 0.5204 0.053 Uiso 1 1 calc R . .
C43 C 0.8451(4) 0.5880(3) 0.1204(2) 0.0387(10) Uani 1 1 d . . .
H43A H 0.8296 0.6279 0.1599 0.046 Uiso 1 1 calc R . .
H43B H 0.7778 0.5836 0.1199 0.046 Uiso 1 1 calc R . .
C44 C 1.0025(4) 0.3641(3) 0.2522(3) 0.0381(11) Uani 1 1 d . . .
C45 C 0.8989(4) 0.4300(3) 0.2209(2) 0.0367(10) Uani 1 1 d . . .
H45 H 0.8593 0.4795 0.2563 0.044 Uiso 1 1 calc R . .
C46 C 0.8212(4) 0.3781(3) 0.2324(3) 0.0397(11) Uani 1 1 d . . .
C47 C 0.8491(4) 0.3031(4) 0.1919(3) 0.0476(12) Uani 1 1 d . . .
H47 H 0.9175 0.2827 0.1577 0.057 Uiso 1 1 calc R . .
C48 C 0.7787(5) 0.2571(4) 0.2003(3) 0.0532(14) Uani 1 1 d . . .
H48 H 0.7986 0.2074 0.1711 0.064 Uiso 1 1 calc R . .
C49 C 0.6788(5) 0.2853(4) 0.2522(3) 0.0564(14) Uani 1 1 d . . .
H49 H 0.6337 0.2505 0.2605 0.068 Uiso 1 1 calc R . .
C50 C 0.6437(4) 0.3602(4) 0.2911(3) 0.0564(14) Uani 1 1 d . . .
H50 H 0.5747 0.3799 0.3246 0.068 Uiso 1 1 calc R . .
C51 C 0.7186(4) 0.4100(4) 0.2789(3) 0.0521(13) Uani 1 1 d . . .
H51 H 0.6959 0.4646 0.3033 0.063 Uiso 1 1 calc R . .
C52 C 1.2803(4) 0.5047(3) -0.0094(3) 0.0420(11) Uani 1 1 d . . .
H52 H 1.2398 0.5149 -0.0461 0.050 Uiso 1 1 calc R . .
C53 C 1.3838(4) 0.5097(3) -0.0397(3) 0.0402(11) Uani 1 1 d . . .
H53 H 1.4113 0.5224 -0.0953 0.048 Uiso 1 1 calc R . .
C54 C 1.4457(4) 0.4955(3) 0.0142(3) 0.0361(10) Uani 1 1 d . . .
C55 C 1.3992(4) 0.4732(3) 0.0944(3) 0.0421(11) Uani 1 1 d . . .
H55 H 1.4376 0.4604 0.1333 0.050 Uiso 1 1 calc R . .
C56 C 1.2979(4) 0.4693(3) 0.1186(3) 0.0428(11) Uani 1 1 d . . .
H56 H 1.2697 0.4537 0.1738 0.051 Uiso 1 1 calc R . .
N1 N 0.4284(3) -0.0153(2) 0.4017(2) 0.0328(8) Uani 1 1 d . . .
H1 H 0.4297 -0.0505 0.4531 0.039 Uiso 1 1 calc R . .
N2 N 0.7391(3) -0.0124(3) 0.3211(2) 0.0344(8) Uani 1 1 d . . .
N3 N 0.5147(3) 0.1274(3) 0.05033(19) 0.0346(8) Uani 1 1 d . . .
H3A H 0.5685 0.0698 0.0369 0.042 Uiso 1 1 calc R . .
N4 N 0.2413(3) 0.0610(2) 0.16726(19) 0.0328(8) Uani 1 1 d . . .
N5 N 1.0122(3) 0.6269(3) 0.38000(19) 0.0322(8) Uani 1 1 d . . .
H5A H 1.0652 0.5697 0.3970 0.039 Uiso 1 1 calc R . .
N6 N 0.7405(3) 0.5566(3) 0.43550(19) 0.0319(8) Uani 1 1 d . . .
N7 N 0.9244(3) 0.4882(3) 0.1410(2) 0.0372(9) Uani 1 1 d . . .
H7A H 0.9256 0.4534 0.1063 0.045 Uiso 1 1 calc R . .
N8 N 1.2378(3) 0.4865(3) 0.0680(2) 0.0346(8) Uani 1 1 d . . .
O1 O 0.3643(2) 0.1286(2) 0.54516(16) 0.0353(7) Uani 1 1 d . . .
O2 O 0.5225(2) 0.1022(2) 0.42247(16) 0.0350(7) Uani 1 1 d . . .
O3 O 0.3573(2) 0.2567(2) 0.41579(16) 0.0383(7) Uani 1 1 d . . .
H3B H 0.2948 0.2826 0.4404 0.058 Uiso 1 1 calc R . .
O4 O 0.3466(2) 0.1265(2) -0.00874(15) 0.0340(7) Uani 1 1 d . . .
O5 O 0.5303(2) 0.0562(2) -0.10259(18) 0.0405(7) Uani 1 1 d . . .
O6 O 0.3939(3) 0.2289(2) -0.14253(17) 0.0462(8) Uani 1 1 d . . .
H6A H 0.4316 0.2148 -0.1866 0.069 Uiso 1 1 calc R . .
O7 O 0.8439(2) 0.6293(2) 0.52304(15) 0.0346(7) Uani 1 1 d . . .
O8 O 1.0288(2) 0.5563(2) 0.55822(16) 0.0370(7) Uani 1 1 d . . .
O9 O 0.8972(2) 0.7268(2) 0.58341(16) 0.0382(7) Uani 1 1 d . . .
H9A H 0.9377 0.7111 0.6139 0.057 Uiso 1 1 calc R . .
O10 O 1.0228(2) 0.6042(2) 0.01496(16) 0.0345(7) Uani 1 1 d . . .
O11 O 0.8687(2) 0.62795(19) -0.04464(15) 0.0278(6) Uani 1 1 d . . .
O12 O 0.8582(3) 0.7597(2) 0.02135(17) 0.0414(7) Uani 1 1 d . . .
H12A H 0.7948 0.7846 0.0170 0.062 Uiso 1 1 calc R . .
O13 O 0.5961(2) -0.1220(2) 0.30067(16) 0.0357(7) Uani 1 1 d . . .
O14 O 0.5054(2) -0.2043(2) 0.28529(16) 0.0369(7) Uani 1 1 d . . .
O15 O 0.5671(2) 0.0912(2) 0.24418(16) 0.0362(7) Uani 1 1 d . . .
O16 O 0.4360(2) 0.0772(2) 0.20732(16) 0.0362(7) Uani 1 1 d . . .
O17 O 1.0622(3) 0.5912(2) 0.17761(17) 0.0390(7) Uani 1 1 d . . .
O18 O 0.9334(2) 0.5762(2) 0.28843(16) 0.0368(7) Uani 1 1 d . . .
O19 O 1.0879(3) 0.3807(2) 0.21442(17) 0.0372(7) Uani 1 1 d . . .
O20 O 0.9921(3) 0.3044(2) 0.31751(17) 0.0432(8) Uani 1 1 d . . .
O1W O 0.7972(2) 0.7416(2) 0.36348(16) 0.0369(7) Uani 1 1 d . . .
H1X H 0.7573 0.7759 0.4082 0.044 Uiso 1 1 d R . .
H1Y H 0.7478 0.7470 0.3335 0.044 Uiso 1 1 d R . .
O2W O 0.2976(2) 0.24230(19) 0.11777(16) 0.0342(7) Uani 1 1 d . . .
H2X H 0.2577 0.2760 0.0758 0.041 Uiso 1 1 d R . .
H2Y H 0.2483 0.2482 0.1697 0.041 Uiso 1 1 d R . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ni1 0.0260(3) 0.0285(3) 0.0260(3) -0.0090(2) -0.0080(2) -0.0094(2)
Ni2 0.0254(3) 0.0266(3) 0.0267(3) -0.0077(2) -0.0076(2) -0.0088(2)
Ni3 0.0269(3) 0.0289(3) 0.0283(3) -0.0088(2) -0.0088(2) -0.0086(2)
Ni4 0.0253(3) 0.0291(3) 0.0269(3) -0.0084(2) -0.0083(2) -0.0087(2)
P1 0.0256(6) 0.0272(5) 0.0296(5) -0.0085(4) -0.0106(4) -0.0077(5)
P2 0.0275(6) 0.0259(5) 0.0277(5) -0.0075(4) -0.0024(5) -0.0067(5)
P3 0.0293(6) 0.0262(5) 0.0287(5) -0.0093(4) -0.0088(5) -0.0075(5)
P4 0.0263(6) 0.0278(5) 0.0276(5) -0.0087(4) -0.0077(4) -0.0086(5)
C1 0.031(3) 0.041(3) 0.043(3) -0.015(2) -0.013(2) -0.009(2)
C2 0.039(3) 0.037(2) 0.034(2) -0.0075(19) -0.011(2) -0.016(2)
C3 0.038(3) 0.037(2) 0.041(3) -0.009(2) -0.007(2) -0.016(2)
C4 0.034(3) 0.029(2) 0.043(3) -0.0060(19) -0.006(2) -0.012(2)
C5 0.054(3) 0.048(3) 0.032(2) -0.008(2) -0.013(2) -0.023(3)
C6 0.066(4) 0.048(3) 0.036(3) -0.002(2) -0.007(2) -0.028(3)
C7 0.044(3) 0.046(3) 0.047(3) -0.012(2) 0.006(2) -0.020(3)
C8 0.041(3) 0.048(3) 0.056(3) -0.008(2) -0.016(2) -0.016(3)
C9 0.044(3) 0.039(3) 0.058(3) 0.013(2) -0.023(2) -0.017(3)
C10 0.037(3) 0.047(3) 0.054(3) -0.025(2) 0.009(2) -0.021(3)
C11 0.030(3) 0.058(3) 0.039(3) -0.016(2) 0.006(2) -0.017(3)
C12 0.029(3) 0.038(2) 0.033(2) -0.0049(19) -0.0054(19) -0.011(2)
C13 0.035(3) 0.055(3) 0.061(3) -0.037(3) 0.009(2) -0.023(3)
C14 0.031(3) 0.041(3) 0.044(3) -0.013(2) 0.000(2) -0.013(2)
C15 0.046(3) 0.043(3) 0.031(2) -0.0085(19) 0.000(2) -0.026(2)
C16 0.042(3) 0.043(3) 0.034(2) -0.010(2) -0.013(2) -0.014(2)
C17 0.035(3) 0.036(2) 0.039(2) -0.0090(19) -0.011(2) -0.012(2)
C18 0.035(3) 0.041(3) 0.036(2) -0.005(2) -0.010(2) -0.014(2)
C19 0.040(3) 0.042(3) 0.053(3) -0.007(2) -0.011(2) -0.010(3)
C20 0.037(3) 0.052(3) 0.046(3) -0.015(2) -0.007(2) -0.007(3)
C21 0.041(3) 0.050(3) 0.040(3) -0.010(2) -0.006(2) -0.017(3)
C22 0.048(4) 0.046(3) 0.056(3) -0.007(2) 0.000(3) -0.020(3)
C23 0.045(3) 0.044(3) 0.058(3) -0.011(2) 0.001(3) -0.016(3)
C24 0.033(3) 0.038(2) 0.041(3) -0.012(2) 0.000(2) -0.016(2)
C25 0.038(3) 0.039(3) 0.039(2) -0.012(2) -0.004(2) -0.015(2)
C26 0.027(3) 0.038(2) 0.036(2) -0.0085(19) -0.0051(19) -0.010(2)
C27 0.034(3) 0.050(3) 0.039(3) -0.019(2) 0.002(2) -0.017(2)
C28 0.029(3) 0.042(3) 0.043(3) -0.014(2) -0.007(2) -0.007(2)
C29 0.039(3) 0.037(2) 0.036(2) -0.0090(19) -0.011(2) -0.015(2)
C30 0.035(3) 0.042(3) 0.032(2) -0.013(2) -0.003(2) -0.010(2)
C31 0.039(3) 0.034(2) 0.031(2) -0.0090(18) -0.0035(19) -0.013(2)
C32 0.037(3) 0.039(3) 0.033(2) -0.007(2) -0.001(2) -0.008(2)
C33 0.046(4) 0.059(3) 0.053(3) 0.002(3) 0.015(3) -0.022(3)
C34 0.057(4) 0.055(3) 0.059(3) -0.017(3) -0.024(3) -0.021(3)
C35 0.043(3) 0.066(4) 0.043(3) -0.017(3) 0.009(2) -0.020(3)
C36 0.046(3) 0.050(3) 0.046(3) -0.012(2) -0.010(2) -0.010(3)
C37 0.042(3) 0.048(3) 0.045(3) -0.008(2) -0.015(2) -0.013(3)
C38 0.028(3) 0.051(3) 0.051(3) 0.007(2) -0.013(2) -0.006(3)
C39 0.027(3) 0.046(3) 0.053(3) 0.008(2) -0.011(2) -0.011(2)
C40 0.038(3) 0.033(2) 0.037(2) -0.007(2) -0.012(2) -0.010(2)
C41 0.030(3) 0.054(3) 0.041(3) 0.011(2) -0.009(2) -0.012(3)
C42 0.033(3) 0.034(2) 0.055(3) 0.011(2) -0.020(2) -0.009(2)
C43 0.023(2) 0.042(3) 0.037(2) -0.010(2) -0.0032(19) 0.001(2)
C44 0.038(3) 0.042(3) 0.030(2) -0.009(2) 0.000(2) -0.014(2)
C45 0.034(3) 0.037(2) 0.033(2) -0.0071(19) -0.0024(19) -0.011(2)
C46 0.041(3) 0.035(2) 0.034(2) 0.0037(19) -0.008(2) -0.012(2)
C47 0.053(3) 0.053(3) 0.041(3) -0.009(2) -0.012(2) -0.021(3)
C48 0.064(4) 0.037(3) 0.055(3) 0.013(2) -0.029(3) -0.020(3)
C49 0.060(4) 0.052(3) 0.048(3) 0.015(3) -0.020(3) -0.022(3)
C50 0.039(3) 0.058(3) 0.062(3) 0.002(3) -0.010(3) -0.018(3)
C51 0.043(3) 0.051(3) 0.045(3) 0.005(2) -0.006(2) -0.013(3)
C52 0.035(3) 0.048(3) 0.039(3) -0.009(2) -0.005(2) -0.014(2)
C53 0.038(3) 0.046(3) 0.031(2) -0.005(2) -0.001(2) -0.017(2)
C54 0.033(3) 0.029(2) 0.041(3) -0.0085(19) -0.007(2) -0.005(2)
C55 0.037(3) 0.055(3) 0.040(3) -0.009(2) -0.014(2) -0.018(3)
C56 0.037(3) 0.049(3) 0.049(3) -0.006(2) -0.015(2) -0.020(3)
N1 0.030(2) 0.0326(19) 0.0340(19) -0.0071(15) -0.0052(16) -0.0109(17)
N2 0.030(2) 0.037(2) 0.034(2) -0.0030(16) -0.0025(16) -0.0164(18)
N3 0.031(2) 0.038(2) 0.035(2) -0.0099(16) -0.0053(16) -0.0113(18)
N4 0.025(2) 0.0334(19) 0.0340(19) -0.0092(16) -0.0007(16) -0.0077(17)
N5 0.026(2) 0.0344(19) 0.0342(19) -0.0108(15) -0.0035(15) -0.0092(17)
N6 0.028(2) 0.037(2) 0.0284(18) -0.0048(15) -0.0076(15) -0.0104(18)
N7 0.033(2) 0.034(2) 0.036(2) 0.0036(16) -0.0111(17) -0.0091(18)
N8 0.025(2) 0.046(2) 0.0292(19) -0.0093(16) -0.0027(15) -0.0097(18)
O1 0.0357(19) 0.0306(15) 0.0345(16) -0.0081(12) -0.0102(13) -0.0044(14)
O2 0.0322(18) 0.0340(16) 0.0381(16) -0.0179(13) -0.0072(13) -0.0046(14)
O3 0.0329(19) 0.0366(17) 0.0396(17) -0.0089(13) -0.0075(14) -0.0064(15)
O4 0.0285(17) 0.0432(17) 0.0253(14) -0.0062(12) -0.0074(12) -0.0076(15)
O5 0.0305(18) 0.0316(16) 0.0509(19) -0.0156(14) 0.0003(14) -0.0051(15)
O6 0.039(2) 0.0443(18) 0.0315(16) -0.0115(14) -0.0031(14) 0.0066(16)
O7 0.0321(18) 0.0421(17) 0.0294(15) -0.0133(13) -0.0059(13) -0.0097(15)
O8 0.0301(18) 0.0350(16) 0.0410(17) -0.0107(13) -0.0085(13) -0.0045(15)
O9 0.041(2) 0.0403(17) 0.0341(16) -0.0132(13) -0.0146(14) -0.0072(16)
O10 0.0326(18) 0.0346(16) 0.0333(16) -0.0042(12) -0.0103(13) -0.0086(15)
O11 0.0268(16) 0.0287(14) 0.0304(15) -0.0100(11) -0.0106(12) -0.0064(13)
O12 0.042(2) 0.0297(16) 0.0421(17) -0.0126(13) -0.0116(14) 0.0028(15)
O13 0.0390(19) 0.0349(16) 0.0346(16) -0.0145(13) -0.0065(14) -0.0107(15)
O14 0.0381(19) 0.0419(17) 0.0312(16) -0.0103(13) -0.0031(13) -0.0159(16)
O15 0.0375(19) 0.0396(17) 0.0300(16) -0.0062(13) -0.0094(13) -0.0115(15)
O16 0.0326(18) 0.0424(18) 0.0283(15) 0.0032(13) -0.0125(13) -0.0111(16)
O17 0.043(2) 0.0362(17) 0.0357(17) -0.0158(13) -0.0015(14) -0.0113(16)
O18 0.0352(19) 0.0440(18) 0.0282(15) -0.0106(13) -0.0085(13) -0.0080(16)
O19 0.038(2) 0.0334(16) 0.0372(17) -0.0048(13) -0.0142(14) -0.0077(15)
O20 0.043(2) 0.0433(18) 0.0395(18) 0.0050(14) -0.0129(15) -0.0182(17)
O1W 0.0342(18) 0.0319(16) 0.0413(17) -0.0106(13) -0.0123(14) -0.0037(15)
O2W 0.0334(18) 0.0318(15) 0.0318(15) -0.0053(12) -0.0102(13) -0.0048(14)

_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 2.059(3) . ?
Ni1 N2 2.068(3) . ?
Ni1 O13 2.081(3) . ?
Ni1 O2 2.091(3) . ?
Ni1 O15 2.125(3) . ?
Ni1 O1 2.157(3) 2_656 ?
Ni2 O16 2.037(3) . ?
Ni2 N3 2.048(3) . ?
Ni2 N4 2.052(3) . ?
Ni2 O5 2.063(3) 2_655 ?
Ni2 O2W 2.087(3) . ?
Ni2 O4 2.155(3) . ?
Ni3 O18 2.039(3) . ?
Ni3 N5 2.049(3) . ?
Ni3 N6 2.055(3) . ?
Ni3 O8 2.065(3) 2_766 ?
Ni3 O1W 2.087(3) . ?
Ni3 O7 2.152(3) . ?
Ni4 N7 2.051(4) . ?
Ni4 O19 2.080(3) . ?
Ni4 N8 2.088(3) . ?
Ni4 O10 2.094(3) . ?
Ni4 O17 2.104(3) . ?
Ni4 O11 2.142(2) 2_765 ?
P1 O2 1.489(3) . ?
P1 O1 1.513(3) . ?
P1 O3 1.573(3) . ?
P1 C1 1.818(4) . ?
P2 O5 1.481(3) . ?
P2 O4 1.515(3) . ?
P2 O6 1.550(3) . ?
P2 C15 1.804(4) . ?
P3 O8 1.475(3) . ?
P3 O7 1.514(3) . ?
P3 O9 1.546(3) . ?
P3 C29 1.823(4) . ?
P4 O10 1.490(3) . ?
P4 O11 1.502(3) . ?
P4 O12 1.579(3) . ?
P4 C43 1.816(4) . ?
C1 N1 1.448(5) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C2 O14 1.254(5) . ?
C2 O13 1.259(5) . ?
C2 C3 1.542(6) . ?
C3 N1 1.466(5) . ?
C3 C4 1.506(6) . ?
C3 H3 0.9800 . ?
C4 C5 1.379(6) . ?
C4 C9 1.405(6) . ?
C5 C6 1.395(6) . ?
C5 H5 0.9300 . ?
C6 C7 1.389(7) . ?
C6 H6 0.9300 . ?
C7 C8 1.360(6) . ?
C7 H7 0.9300 . ?
C8 C9 1.393(6) . ?
C8 H8 0.9300 . ?
C9 H9 0.9300 . ?
C10 N2 1.310(5) . ?
C10 C11 1.399(6) . ?
C10 H10 0.9300 . ?
C11 C12 1.386(6) . ?
C11 H11 0.9300 . ?
C12 C13 1.410(6) . ?
C12 C26 1.463(6) 1_655 ?
C13 C14 1.387(6) . ?
C13 H13 0.9300 . ?
C14 N2 1.312(5) . ?
C14 H14 0.9300 . ?
C15 N3 1.479(5) . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C16 O15 1.230(5) . ?
C16 O16 1.272(5) . ?
C16 C17 1.548(6) . ?
C17 N3 1.475(5) . ?
C17 C18 1.483(6) . ?
C17 H17 0.9800 . ?
C18 C19 1.364(6) . ?
C18 C23 1.402(6) . ?
C19 C20 1.400(6) . ?
C19 H19 0.9300 . ?
C20 C21 1.379(6) . ?
C20 H20 0.9300 . ?
C21 C22 1.367(7) . ?
C21 H21 0.9300 . ?
C22 C23 1.402(7) . ?
C22 H22 0.9300 . ?
C23 H23 0.9300 . ?
C24 N4 1.315(5) . ?
C24 C25 1.373(6) . ?
C24 H24 0.9300 . ?
C25 C26 1.391(6) . ?
C25 H25 0.9300 . ?
C26 C27 1.375(6) . ?
C26 C12 1.463(6) 1_455 ?
C27 C28 1.377(6) . ?
C27 H27 0.9300 . ?
C28 N4 1.363(5) . ?
C28 H28 0.9300 . ?
C29 N5 1.472(5) . ?
C29 H29A 0.9700 . ?
C29 H29B 0.9700 . ?
C30 O17 1.239(5) . ?
C30 O18 1.260(5) . ?
C30 C31 1.557(6) . ?
C31 N5 1.479(5) . ?
C31 C32 1.493(6) . ?
C31 H31 0.9800 . ?
C32 C37 1.382(6) . ?
C32 C33 1.407(6) . ?
C33 C34 1.394(7) . ?
C33 H33 0.9300 . ?
C34 C35 1.392(7) . ?
C34 H34 0.9300 . ?
C35 C36 1.368(7) . ?
C35 H35 0.9300 . ?
C36 C37 1.394(7) . ?
C36 H36 0.9300 . ?
C37 H37 0.9300 . ?
C38 C39 1.292(6) . ?
C38 N6 1.361(5) . ?
C38 H38 0.9300 . ?
C39 C40 1.406(6) . ?
C39 H39 0.9300 . ?
C40 C41 1.363(6) . ?
C40 C40 1.481(9) 2_666 ?
C41 C42 1.356(6) . ?
C41 H41 0.9300 . ?
C42 N6 1.341(5) . ?
C42 H42 0.9300 . ?
C43 N7 1.462(5) . ?
C43 H43A 0.9700 . ?
C43 H43B 0.9700 . ?
C44 O20 1.248(5) . ?
C44 O19 1.254(5) . ?
C44 C45 1.533(6) . ?
C45 N7 1.453(5) . ?
C45 C46 1.518(6) . ?
C45 H45 0.9800 . ?
C46 C51 1.363(6) . ?
C46 C47 1.368(6) . ?
C47 C48 1.374(6) . ?
C47 H47 0.9300 . ?
C48 C49 1.371(7) . ?
C48 H48 0.9300 . ?
C49 C50 1.328(7) . ?
C49 H49 0.9300 . ?
C50 C51 1.457(7) . ?
C50 H50 0.9300 . ?
C51 H51 0.9300 . ?
C52 N8 1.305(5) . ?
C52 C53 1.397(6) . ?
C52 H52 0.9300 . ?
C53 C54 1.395(6) . ?
C53 H53 0.9300 . ?
C54 C55 1.367(6) . ?
C54 C54 1.488(9) 2_865 ?
C55 C56 1.361(6) . ?
C55 H55 0.9300 . ?
C56 N8 1.315(5) . ?
C56 H56 0.9300 . ?
N1 H1 0.9100 . ?
N3 H3A 0.9100 . ?
N5 H5A 0.9100 . ?
N7 H7A 0.9100 . ?
O1 Ni1 2.157(3) 2_656 ?
O3 H3B 0.8200 . ?
O5 Ni2 2.063(3) 2_655 ?
O6 H6A 0.8200 . ?
O8 Ni3 2.065(3) 2_766 ?
O9 H9A 0.8200 . ?
O11 Ni4 2.142(2) 2_765 ?
O12 H12A 0.8200 . ?
O1W H1X 0.9601 . ?
O1W H1Y 0.9600 . ?
O2W H2X 0.9600 . ?
O2W H2Y 0.9600 . ?

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 N2 174.25(13) . . ?
N1 Ni1 O13 80.15(12) . . ?
N2 Ni1 O13 102.19(13) . . ?
N1 Ni1 O2 83.52(12) . . ?
N2 Ni1 O2 94.18(12) . . ?
O13 Ni1 O2 163.63(12) . . ?
N1 Ni1 O15 102.57(13) . . ?
N2 Ni1 O15 82.79(12) . . ?
O13 Ni1 O15 89.32(11) . . ?
O2 Ni1 O15 93.01(11) . . ?
N1 Ni1 O1 89.11(12) . 2_656 ?
N2 Ni1 O1 85.79(12) . 2_656 ?
O13 Ni1 O1 87.03(11) . 2_656 ?
O2 Ni1 O1 94.00(10) . 2_656 ?
O15 Ni1 O1 166.99(11) . 2_656 ?
O16 Ni2 N3 80.95(12) . . ?
O16 Ni2 N4 100.03(12) . . ?
N3 Ni2 N4 178.02(14) . . ?
O16 Ni2 O5 90.96(12) . 2_655 ?
N3 Ni2 O5 90.28(13) . 2_655 ?
N4 Ni2 O5 91.42(12) . 2_655 ?
O16 Ni2 O2W 86.40(11) . . ?
N3 Ni2 O2W 86.72(13) . . ?
N4 Ni2 O2W 91.61(12) . . ?
O5 Ni2 O2W 176.29(12) 2_655 . ?
O16 Ni2 O4 166.11(11) . . ?
N3 Ni2 O4 85.71(12) . . ?
N4 Ni2 O4 93.20(12) . . ?
O5 Ni2 O4 92.93(11) 2_655 . ?
O2W Ni2 O4 89.04(11) . . ?
O18 Ni3 N5 80.58(12) . . ?
O18 Ni3 N6 100.23(12) . . ?
N5 Ni3 N6 179.05(13) . . ?
O18 Ni3 O8 90.26(11) . 2_766 ?
N5 Ni3 O8 88.85(13) . 2_766 ?
N6 Ni3 O8 91.64(12) . 2_766 ?
O18 Ni3 O1W 85.99(11) . . ?
N5 Ni3 O1W 85.77(13) . . ?
N6 Ni3 O1W 93.78(13) . . ?
O8 Ni3 O1W 173.89(11) 2_766 . ?
O18 Ni3 O7 165.15(11) . . ?
N5 Ni3 O7 85.42(11) . . ?
N6 Ni3 O7 93.73(12) . . ?
O8 Ni3 O7 94.40(11) 2_766 . ?
O1W Ni3 O7 88.08(11) . . ?
N7 Ni4 O19 79.80(12) . . ?
N7 Ni4 N8 174.34(13) . . ?
O19 Ni4 N8 102.55(13) . . ?
N7 Ni4 O10 84.04(12) . . ?
O19 Ni4 O10 163.72(12) . . ?
N8 Ni4 O10 93.72(12) . . ?
N7 Ni4 O17 101.95(13) . . ?
O19 Ni4 O17 88.79(11) . . ?
N8 Ni4 O17 83.31(12) . . ?
O10 Ni4 O17 92.64(11) . . ?
N7 Ni4 O11 89.04(13) . 2_765 ?
O19 Ni4 O11 86.89(10) . 2_765 ?
N8 Ni4 O11 85.97(12) . 2_765 ?
O10 Ni4 O11 94.85(10) . 2_765 ?
O17 Ni4 O11 167.30(12) . 2_765 ?
O2 P1 O1 115.73(16) . . ?
O2 P1 O3 108.88(16) . . ?
O1 P1 O3 109.57(16) . . ?
O2 P1 C1 105.95(18) . . ?
O1 P1 C1 110.50(18) . . ?
O3 P1 C1 105.70(18) . . ?
O5 P2 O4 116.22(16) . . ?
O5 P2 O6 113.93(17) . . ?
O4 P2 O6 107.90(17) . . ?
O5 P2 C15 106.6(2) . . ?
O4 P2 C15 105.01(17) . . ?
O6 P2 C15 106.41(19) . . ?
O8 P3 O7 116.46(16) . . ?
O8 P3 O9 112.63(16) . . ?
O7 P3 O9 109.04(17) . . ?
O8 P3 C29 106.38(19) . . ?
O7 P3 C29 104.21(17) . . ?
O9 P3 C29 107.37(17) . . ?
O10 P4 O11 115.80(16) . . ?
O10 P4 O12 108.46(17) . . ?
O11 P4 O12 109.58(16) . . ?
O10 P4 C43 105.73(18) . . ?
O11 P4 C43 111.22(19) . . ?
O12 P4 C43 105.48(18) . . ?
N1 C1 P1 107.7(3) . . ?
N1 C1 H1A 110.2 . . ?
P1 C1 H1A 110.2 . . ?
N1 C1 H1B 110.2 . . ?
P1 C1 H1B 110.2 . . ?
H1A C1 H1B 108.5 . . ?
O14 C2 O13 124.6(4) . . ?
O14 C2 C3 116.7(4) . . ?
O13 C2 C3 118.4(4) . . ?
N1 C3 C4 118.1(3) . . ?
N1 C3 C2 109.6(3) . . ?
C4 C3 C2 115.0(4) . . ?
N1 C3 H3 104.1 . . ?
C4 C3 H3 104.1 . . ?
C2 C3 H3 104.1 . . ?
C5 C4 C9 120.3(4) . . ?
C5 C4 C3 123.2(4) . . ?
C9 C4 C3 116.3(4) . . ?
C4 C5 C6 118.8(4) . . ?
C4 C5 H5 120.6 . . ?
C6 C5 H5 120.6 . . ?
C7 C6 C5 121.0(4) . . ?
C7 C6 H6 119.5 . . ?
C5 C6 H6 119.5 . . ?
C8 C7 C6 119.9(5) . . ?
C8 C7 H7 120.1 . . ?
C6 C7 H7 120.1 . . ?
C7 C8 C9 120.6(5) . . ?
C7 C8 H8 119.7 . . ?
C9 C8 H8 119.7 . . ?
C8 C9 C4 119.4(4) . . ?
C8 C9 H9 120.3 . . ?
C4 C9 H9 120.3 . . ?
N2 C10 C11 123.0(4) . . ?
N2 C10 H10 118.5 . . ?
C11 C10 H10 118.5 . . ?
C12 C11 C10 121.3(4) . . ?
C12 C11 H11 119.4 . . ?
C10 C11 H11 119.4 . . ?
C11 C12 C13 115.0(4) . . ?
C11 C12 C26 122.6(4) . 1_655 ?
C13 C12 C26 122.3(4) . 1_655 ?
C14 C13 C12 118.3(4) . . ?
C14 C13 H13 120.8 . . ?
C12 C13 H13 120.8 . . ?
N2 C14 C13 126.0(4) . . ?
N2 C14 H14 117.0 . . ?
C13 C14 H14 117.0 . . ?
N3 C15 P2 104.9(3) . . ?
N3 C15 H15A 110.8 . . ?
P2 C15 H15A 110.8 . . ?
N3 C15 H15B 110.8 . . ?
P2 C15 H15B 110.8 . . ?
H15A C15 H15B 108.8 . . ?
O15 C16 O16 126.2(4) . . ?
O15 C16 C17 118.3(4) . . ?
O16 C16 C17 115.2(3) . . ?
N3 C17 C18 110.6(3) . . ?
N3 C17 C16 109.2(3) . . ?
C18 C17 C16 119.1(4) . . ?
N3 C17 H17 105.6 . . ?
C18 C17 H17 105.6 . . ?
C16 C17 H17 105.6 . . ?
C19 C18 C23 118.5(4) . . ?
C19 C18 C17 121.1(4) . . ?
C23 C18 C17 120.1(4) . . ?
C18 C19 C20 120.8(4) . . ?
C18 C19 H19 119.6 . . ?
C20 C19 H19 119.6 . . ?
C21 C20 C19 120.2(5) . . ?
C21 C20 H20 119.9 . . ?
C19 C20 H20 119.9 . . ?
C22 C21 C20 120.2(5) . . ?
C22 C21 H21 119.9 . . ?
C20 C21 H21 119.9 . . ?
C21 C22 C23 119.4(5) . . ?
C21 C22 H22 120.3 . . ?
C23 C22 H22 120.3 . . ?
C18 C23 C22 120.8(5) . . ?
C18 C23 H23 119.6 . . ?
C22 C23 H23 119.6 . . ?
N4 C24 C25 124.1(4) . . ?
N4 C24 H24 117.9 . . ?
C25 C24 H24 117.9 . . ?
C24 C25 C26 119.7(4) . . ?
C24 C25 H25 120.1 . . ?
C26 C25 H25 120.1 . . ?
C27 C26 C25 116.7(4) . . ?
C27 C26 C12 122.8(4) . 1_455 ?
C25 C26 C12 120.5(4) . 1_455 ?
C26 C27 C28 120.5(4) . . ?
C26 C27 H27 119.7 . . ?
C28 C27 H27 119.7 . . ?
N4 C28 C27 122.2(4) . . ?
N4 C28 H28 118.9 . . ?
C27 C28 H28 118.9 . . ?
N5 C29 P3 103.7(3) . . ?
N5 C29 H29A 111.0 . . ?
P3 C29 H29A 111.0 . . ?
N5 C29 H29B 111.0 . . ?
P3 C29 H29B 111.0 . . ?
H29A C29 H29B 109.0 . . ?
O17 C30 O18 126.2(4) . . ?
O17 C30 C31 117.4(4) . . ?
O18 C30 C31 116.1(3) . . ?
N5 C31 C32 111.4(3) . . ?
N5 C31 C30 108.5(3) . . ?
C32 C31 C30 117.1(3) . . ?
N5 C31 H31 106.4 . . ?
C32 C31 H31 106.4 . . ?
C30 C31 H31 106.4 . . ?
C37 C32 C33 118.1(5) . . ?
C37 C32 C31 120.0(4) . . ?
C33 C32 C31 121.4(4) . . ?
C34 C33 C32 120.6(5) . . ?
C34 C33 H33 119.7 . . ?
C32 C33 H33 119.7 . . ?
C35 C34 C33 120.7(5) . . ?
C35 C34 H34 119.6 . . ?
C33 C34 H34 119.6 . . ?
C36 C35 C34 117.9(5) . . ?
C36 C35 H35 121.0 . . ?
C34 C35 H35 121.0 . . ?
C35 C36 C37 122.4(5) . . ?
C35 C36 H36 118.8 . . ?
C37 C36 H36 118.8 . . ?
C32 C37 C36 120.2(5) . . ?
C32 C37 H37 119.9 . . ?
C36 C37 H37 119.9 . . ?
C39 C38 N6 128.2(4) . . ?
C39 C38 H38 115.9 . . ?
N6 C38 H38 115.9 . . ?
C38 C39 C40 119.0(5) . . ?
C38 C39 H39 120.5 . . ?
C40 C39 H39 120.5 . . ?
C41 C40 C39 115.0(4) . . ?
C41 C40 C40 123.0(5) . 2_666 ?
C39 C40 C40 121.8(5) . 2_666 ?
C42 C41 C40 121.7(4) . . ?
C42 C41 H41 119.1 . . ?
C40 C41 H41 119.1 . . ?
N6 C42 C41 123.8(4) . . ?
N6 C42 H42 118.1 . . ?
C41 C42 H42 118.1 . . ?
N7 C43 P4 107.4(3) . . ?
N7 C43 H43A 110.2 . . ?
P4 C43 H43A 110.2 . . ?
N7 C43 H43B 110.2 . . ?
P4 C43 H43B 110.2 . . ?
H43A C43 H43B 108.5 . . ?
O20 C44 O19 125.5(4) . . ?
O20 C44 C45 116.5(4) . . ?
O19 C44 C45 117.6(4) . . ?
N7 C45 C46 116.7(4) . . ?
N7 C45 C44 110.6(4) . . ?
C46 C45 C44 115.0(4) . . ?
N7 C45 H45 104.3 . . ?
C46 C45 H45 104.3 . . ?
C44 C45 H45 104.3 . . ?
C51 C46 C47 117.9(5) . . ?
C51 C46 C45 120.8(4) . . ?
C47 C46 C45 121.2(4) . . ?
C46 C47 C48 121.8(5) . . ?
C46 C47 H47 119.1 . . ?
C48 C47 H47 119.1 . . ?
C49 C48 C47 119.3(5) . . ?
C49 C48 H48 120.4 . . ?
C47 C48 H48 120.4 . . ?
C50 C49 C48 122.6(5) . . ?
C50 C49 H49 118.7 . . ?
C48 C49 H49 118.7 . . ?
C49 C50 C51 116.8(5) . . ?
C49 C50 H50 121.6 . . ?
C51 C50 H50 121.6 . . ?
C46 C51 C50 121.3(5) . . ?
C46 C51 H51 119.4 . . ?
C50 C51 H51 119.4 . . ?
N8 C52 C53 123.1(4) . . ?
N8 C52 H52 118.5 . . ?
C53 C52 H52 118.5 . . ?
C54 C53 C52 119.4(4) . . ?
C54 C53 H53 120.3 . . ?
C52 C53 H53 120.3 . . ?
C55 C54 C53 115.3(4) . . ?
C55 C54 C54 122.8(5) . 2_865 ?
C53 C54 C54 121.9(5) . 2_865 ?
C56 C55 C54 121.3(4) . . ?
C56 C55 H55 119.4 . . ?
C54 C55 H55 119.4 . . ?
N8 C56 C55 123.5(4) . . ?
N8 C56 H56 118.3 . . ?
C55 C56 H56 118.3 . . ?
C1 N1 C3 117.3(3) . . ?
C1 N1 Ni1 111.9(2) . . ?
C3 N1 Ni1 113.4(3) . . ?
C1 N1 H1 104.1 . . ?
C3 N1 H1 104.1 . . ?
Ni1 N1 H1 104.1 . . ?
C10 N2 C14 116.3(4) . . ?
C10 N2 Ni1 121.2(3) . . ?
C14 N2 Ni1 122.2(3) . . ?
C17 N3 C15 117.5(3) . . ?
C17 N3 Ni2 110.0(2) . . ?
C15 N3 Ni2 110.7(3) . . ?
C17 N3 H3A 105.9 . . ?
C15 N3 H3A 105.9 . . ?
Ni2 N3 H3A 105.9 . . ?
C24 N4 C28 116.7(4) . . ?
C24 N4 Ni2 119.5(3) . . ?
C28 N4 Ni2 123.5(3) . . ?
C29 N5 C31 116.7(3) . . ?
C29 N5 Ni3 111.1(3) . . ?
C31 N5 Ni3 111.3(2) . . ?
C29 N5 H5A 105.6 . . ?
C31 N5 H5A 105.6 . . ?
Ni3 N5 H5A 105.6 . . ?
C42 N6 C38 112.1(4) . . ?
C42 N6 Ni3 120.7(3) . . ?
C38 N6 Ni3 127.2(3) . . ?
C45 N7 C43 117.8(3) . . ?
C45 N7 Ni4 113.5(3) . . ?
C43 N7 Ni4 111.2(3) . . ?
C45 N7 H7A 104.2 . . ?
C43 N7 H7A 104.2 . . ?
Ni4 N7 H7A 104.2 . . ?
C52 N8 C56 117.4(4) . . ?
C52 N8 Ni4 121.4(3) . . ?
C56 N8 Ni4 121.2(3) . . ?
P1 O1 Ni1 134.36(17) . 2_656 ?
P1 O2 Ni1 116.41(16) . . ?
P1 O3 H3B 109.5 . . ?
P2 O4 Ni2 110.28(15) . . ?
P2 O5 Ni2 159.31(19) . 2_655 ?
P2 O6 H6A 109.5 . . ?
P3 O7 Ni3 110.22(15) . . ?
P3 O8 Ni3 161.51(19) . 2_766 ?
P3 O9 H9A 109.5 . . ?
P4 O10 Ni4 116.09(16) . . ?
P4 O11 Ni4 135.69(17) . 2_765 ?
P4 O12 H12A 109.5 . . ?
C2 O13 Ni1 116.3(3) . . ?
C16 O15 Ni1 129.8(3) . . ?
C16 O16 Ni2 117.1(2) . . ?
C30 O17 Ni4 130.2(3) . . ?
C30 O18 Ni3 117.6(3) . . ?
C44 O19 Ni4 116.8(3) . . ?
Ni3 O1W H1X 109.5 . . ?
Ni3 O1W H1Y 108.8 . . ?
H1X O1W H1Y 109.5 . . ?
Ni2 O2W H2X 109.5 . . ?
Ni2 O2W H2Y 109.5 . . ?
H2X O2W H2Y 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.992
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 0.992
_refine_diff_density_max         0.888
_refine_diff_density_min         -0.530
_refine_diff_density_rms         0.119
_database_code_depnum_ccdc_archive 'CCDC 947902'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_111

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C38 H38 Co3 N6 O12 P2, 4(H2 O)'
_chemical_formula_sum            'C38 H46 Co3 N6 O16 P2'
_chemical_formula_weight         1081.54

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'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'P 21/c'
_symmetry_space_group_name_Hall  '-P 2ybc'

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                   10.787(19)
_cell_length_b                   23.30(4)
_cell_length_c                   9.916(17)
_cell_angle_alpha                90.00
_cell_angle_beta                 116.00(3)
_cell_angle_gamma                90.00
_cell_volume                     2240(7)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    950
_cell_measurement_theta_min      2.446
_cell_measurement_theta_max      24.203

_exptl_crystal_description       block
_exptl_crystal_colour            pink
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.603
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1110
_exptl_absorpt_coefficient_mu    1.246
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7887
_exptl_absorpt_correction_T_max  0.8855
_exptl_absorpt_process_details   'SADABS(Bruker, 2000)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(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  'Bruker APEX DUO'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            7559
_diffrn_reflns_av_R_equivalents  0.1008
_diffrn_reflns_av_unetI/netI     0.2085
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_theta_min         1.75
_diffrn_reflns_theta_max         25.00
_reflns_number_total             3880
_reflns_number_gt                1951
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'SMART (Bruker, 2000)'
_computing_cell_refinement       SMART
_computing_data_reduction        'SAINT (Bruker, 2000)'
_computing_structure_solution    'SHELXTL (Bruker, 2000)'
_computing_structure_refinement  SHELXTL
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0504P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3880
_refine_ls_number_parameters     295
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1695
_refine_ls_R_factor_gt           0.0688
_refine_ls_wR_factor_ref         0.1495
_refine_ls_wR_factor_gt          0.1221
_refine_ls_goodness_of_fit_ref   0.978
_refine_ls_restrained_S_all      0.978
_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
O3W O 0.3166(4) 0.11129(19) 0.2964(6) 0.0393(14) Uani 1 1 d . . .
N2 N 0.9394(5) 0.0920(2) 0.9496(7) 0.0248(15) Uani 1 1 d . . .
O1 O 0.7262(4) 0.01880(17) 1.1072(5) 0.0242(12) Uani 1 1 d . . .
Co1 Co 1.0000 0.0000 1.0000 0.0232(4) Uani 1 2 d S . .
O2 O 0.7930(4) -0.02181(17) 0.9101(5) 0.0271(12) Uani 1 1 d . . .
P1 P 0.67442(15) -0.00248(8) 0.9460(2) 0.0250(5) Uani 1 1 d . . .
Co2 Co 0.36793(8) -0.03109(4) 0.75437(11) 0.0272(3) Uani 1 1 d . . .
C1 C 0.5860(6) 0.0575(3) 0.8228(8) 0.033(2) Uani 1 1 d . . .
H1A H 0.6261 0.0934 0.8717 0.040 Uiso 1 1 calc R . .
H1B H 0.5967 0.0549 0.7309 0.040 Uiso 1 1 calc R . .
C2 C 0.3461(6) 0.0938(3) 0.6634(7) 0.0226(18) Uani 1 1 d . . .
H2 H 0.4002 0.1072 0.6119 0.027 Uiso 1 1 calc R . .
C3 C 0.2990(6) 0.1469(3) 0.7181(8) 0.0240(18) Uani 1 1 d . . .
C4 C 0.3329(6) 0.2015(3) 0.6894(8) 0.032(2) Uani 1 1 d . . .
H4 H 0.3848 0.2056 0.6358 0.038 Uiso 1 1 calc R . .
C5 C 0.2901(8) 0.2509(3) 0.7403(9) 0.043(2) Uani 1 1 d . . .
H5 H 0.3107 0.2874 0.7180 0.051 Uiso 1 1 calc R . .
C6 C 0.2176(7) 0.2439(3) 0.8232(9) 0.043(2) Uani 1 1 d . . .
H6 H 0.1908 0.2761 0.8592 0.052 Uiso 1 1 calc R . .
C7 C 0.1829(7) 0.1893(4) 0.8548(9) 0.045(2) Uani 1 1 d . . .
H7 H 0.1340 0.1855 0.9117 0.054 Uiso 1 1 calc R . .
C8 C 0.2220(6) 0.1406(3) 0.8005(8) 0.031(2) Uani 1 1 d . . .
H8 H 0.1972 0.1043 0.8189 0.037 Uiso 1 1 calc R . .
C9 C 0.1672(6) -0.1303(3) 0.6098(8) 0.030(2) Uani 1 1 d . . .
H9 H 0.1094 -0.1004 0.5568 0.037 Uiso 1 1 calc R . .
C10 C 0.3751(6) -0.1615(3) 0.7870(9) 0.036(2) Uani 1 1 d . . .
H10 H 0.4642 -0.1536 0.8590 0.044 Uiso 1 1 calc R . .
C11 C 0.9582(6) 0.1311(3) 1.0580(9) 0.0248(19) Uani 1 1 d . . .
H11 H 1.0010 0.1193 1.1576 0.030 Uiso 1 1 calc R . .
C12 C 0.9162(6) 0.1883(3) 1.0273(9) 0.029(2) Uani 1 1 d . . .
H12 H 0.9351 0.2141 1.1055 0.035 Uiso 1 1 calc R . .
C13 C 0.8461(6) 0.2067(3) 0.8791(9) 0.0259(19) Uani 1 1 d . . .
C14 C 0.8237(6) 0.1660(3) 0.7685(9) 0.029(2) Uani 1 1 d . . .
H14 H 0.7761 0.1761 0.6680 0.035 Uiso 1 1 calc R . .
C15 C 0.8725(6) 0.1096(3) 0.8075(9) 0.027(2) Uani 1 1 d . . .
H15 H 0.8576 0.0835 0.7311 0.032 Uiso 1 1 calc R . .
C16 C 0.2002(6) -0.2319(3) 0.6553(8) 0.0225(18) Uani 1 1 d . . .
C17 C 0.3325(6) -0.2185(3) 0.7633(8) 0.033(2) Uani 1 1 d . . .
H17 H 0.3920 -0.2475 0.8192 0.039 Uiso 1 1 calc R . .
C18 C 0.1162(6) -0.1860(3) 0.5788(8) 0.028(2) Uani 1 1 d . . .
H18 H 0.0262 -0.1926 0.5072 0.034 Uiso 1 1 calc R . .
C19 C 0.2229(6) 0.0581(3) 0.5477(8) 0.0243(19) Uani 1 1 d . . .
N1 N 0.2959(5) -0.1174(2) 0.7127(6) 0.0261(16) Uani 1 1 d . . .
N3 N 0.4369(4) 0.0559(2) 0.7874(6) 0.0232(15) Uani 1 1 d . . .
H3A H 0.4305 0.0683 0.8702 0.028 Uiso 1 1 d R . .
O3 O 0.5642(4) -0.05033(17) 0.9058(5) 0.0255(12) Uani 1 1 d . . .
O4 O 0.2119(4) 0.0053(2) 0.5723(6) 0.0343(13) Uani 1 1 d . . .
O5 O 0.1456(4) 0.08523(19) 0.4316(5) 0.0293(13) Uani 1 1 d . . .
O1W O 0.4523(5) -0.0481(2) 0.5749(6) 0.0491(16) Uani 1 1 d . . .
H1WA H 0.4134 -0.0251 0.5018 0.074 Uiso 1 1 d R . .
H1WB H 0.5397 -0.0454 0.6151 0.074 Uiso 1 1 d R . .
O2W O 1.0001(4) 0.00531(17) 1.2140(5) 0.0291(13) Uani 1 1 d . . .
H2WA H 1.0583 0.0305 1.2663 0.044 Uiso 1 1 d R . .
H2WB H 0.9201 0.0149 1.2029 0.044 Uiso 1 1 d R . .
H3WA H 0.3045 0.0982 0.2116 0.044 Uiso 1 1 d R . .
H3WB H 0.2396 0.1053 0.2984 0.044 Uiso 1 1 d R . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
O3W 0.035(3) 0.039(4) 0.045(4) -0.009(3) 0.019(2) 0.000(2)
N2 0.016(3) 0.029(4) 0.024(4) -0.011(4) 0.003(2) -0.006(2)
O1 0.019(2) 0.022(3) 0.028(3) -0.007(3) 0.0069(19) 0.0007(18)
Co1 0.0153(6) 0.0152(8) 0.0325(10) 0.0006(7) 0.0044(5) -0.0001(5)
O2 0.019(2) 0.025(3) 0.033(3) -0.012(3) 0.0070(19) -0.0032(19)
P1 0.0158(8) 0.0178(12) 0.0367(14) -0.0036(11) 0.0070(8) -0.0003(7)
Co2 0.0162(4) 0.0187(6) 0.0383(7) -0.0024(6) 0.0043(4) -0.0019(4)
C1 0.017(3) 0.034(5) 0.046(6) 0.000(4) 0.012(3) -0.004(3)
C2 0.016(3) 0.025(5) 0.020(5) 0.006(4) 0.002(3) -0.001(3)
C3 0.023(3) 0.012(4) 0.025(5) -0.007(4) -0.001(3) -0.002(3)
C4 0.028(4) 0.031(5) 0.037(6) -0.002(5) 0.015(3) -0.004(3)
C5 0.050(5) 0.020(5) 0.050(7) 0.003(5) 0.014(4) -0.005(4)
C6 0.033(4) 0.029(6) 0.047(7) -0.005(5) -0.001(4) 0.012(3)
C7 0.033(4) 0.038(6) 0.056(7) -0.001(5) 0.012(4) 0.007(4)
C8 0.016(3) 0.033(5) 0.040(6) 0.008(4) 0.008(3) 0.009(3)
C9 0.014(3) 0.035(5) 0.034(5) 0.006(4) 0.003(3) -0.001(3)
C10 0.019(3) 0.026(5) 0.051(6) 0.002(5) 0.004(3) -0.005(3)
C11 0.015(3) 0.029(5) 0.030(5) 0.007(4) 0.008(3) 0.003(3)
C12 0.028(4) 0.025(5) 0.028(5) 0.005(4) 0.007(3) 0.007(3)
C13 0.019(3) 0.027(5) 0.032(6) 0.001(5) 0.011(3) -0.003(3)
C14 0.025(4) 0.022(5) 0.032(5) 0.003(4) 0.004(3) 0.003(3)
C15 0.022(3) 0.024(5) 0.032(6) -0.006(4) 0.008(3) -0.002(3)
C16 0.026(4) 0.014(4) 0.026(5) -0.011(4) 0.011(3) -0.004(3)
C17 0.024(4) 0.015(5) 0.045(6) 0.003(4) 0.003(3) 0.005(3)
C18 0.026(4) 0.020(5) 0.035(5) 0.002(4) 0.011(3) -0.008(3)
C19 0.020(3) 0.026(5) 0.023(5) -0.010(5) 0.005(3) -0.003(3)
N1 0.023(3) 0.017(4) 0.034(4) -0.001(3) 0.009(3) 0.002(2)
N3 0.016(3) 0.017(4) 0.029(4) -0.003(3) 0.003(2) 0.002(2)
O3 0.018(2) 0.014(3) 0.041(3) 0.000(3) 0.010(2) -0.0005(17)
O4 0.039(3) 0.020(3) 0.036(4) 0.000(3) 0.008(2) -0.007(2)
O5 0.018(2) 0.028(3) 0.031(3) 0.003(3) 0.001(2) 0.0013(19)
O1W 0.031(3) 0.049(4) 0.053(4) 0.011(3) 0.005(2) 0.006(2)
O2W 0.019(2) 0.022(3) 0.040(3) -0.006(3) 0.007(2) -0.0038(18)

_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
O3W H3WA 0.8493 . ?
O3W H3WB 0.8511 . ?
N2 C15 1.335(8) . ?
N2 C11 1.355(8) . ?
N2 Co1 2.233(7) . ?
O1 P1 1.527(5) . ?
O1 Co2 2.054(5) 3_657 ?
Co1 O2 2.072(5) . ?
Co1 O2 2.072(5) 3_757 ?
Co1 O2W 2.125(6) . ?
Co1 O2W 2.125(6) 3_757 ?
Co1 N2 2.233(7) 3_757 ?
O2 P1 1.538(5) . ?
P1 O3 1.549(5) . ?
P1 C1 1.825(7) . ?
Co2 O4 2.036(5) . ?
Co2 O3 2.038(5) . ?
Co2 O1 2.054(5) 3_657 ?
Co2 N1 2.131(6) . ?
Co2 N3 2.133(6) . ?
Co2 O1W 2.360(6) . ?
C1 N3 1.489(7) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C2 N3 1.482(8) . ?
C2 C3 1.525(9) . ?
C2 C19 1.561(9) . ?
C2 H2 0.9800 . ?
C3 C4 1.387(9) . ?
C3 C8 1.404(9) . ?
C4 C5 1.414(10) . ?
C4 H4 0.9300 . ?
C5 C6 1.370(11) . ?
C5 H5 0.9300 . ?
C6 C7 1.398(10) . ?
C6 H6 0.9300 . ?
C7 C8 1.399(9) . ?
C7 H7 0.9300 . ?
C8 H8 0.9300 . ?
C9 N1 1.348(8) . ?
C9 C18 1.390(8) . ?
C9 H9 0.9300 . ?
C10 N1 1.332(8) . ?
C10 C17 1.392(9) . ?
C10 H10 0.9300 . ?
C11 C12 1.399(9) . ?
C11 H11 0.9300 . ?
C12 C13 1.393(9) . ?
C12 H12 0.9300 . ?
C13 C14 1.388(9) . ?
C13 C16 1.506(9) 2_656 ?
C14 C15 1.404(9) . ?
C14 H14 0.9300 . ?
C15 H15 0.9300 . ?
C16 C18 1.392(8) . ?
C16 C17 1.393(9) . ?
C16 C13 1.506(9) 2_646 ?
C17 H17 0.9300 . ?
C18 H18 0.9300 . ?
C19 O5 1.256(8) . ?
C19 O4 1.271(8) . ?
N3 H3A 0.9001 . ?
O1W H1WA 0.8499 . ?
O1W H1WB 0.8499 . ?
O2W H2WA 0.8501 . ?
O2W H2WB 0.8500 . ?

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
H3WA O3W H3WB 103.7 . . ?
C15 N2 C11 117.0(6) . . ?
C15 N2 Co1 120.1(5) . . ?
C11 N2 Co1 122.7(5) . . ?
P1 O1 Co2 133.1(2) . 3_657 ?
O2 Co1 O2 179.998(1) . 3_757 ?
O2 Co1 O2W 88.42(17) . . ?
O2 Co1 O2W 91.58(17) 3_757 . ?
O2 Co1 O2W 91.58(17) . 3_757 ?
O2 Co1 O2W 88.42(17) 3_757 3_757 ?
O2W Co1 O2W 180.0 . 3_757 ?
O2 Co1 N2 89.12(18) . . ?
O2 Co1 N2 90.88(18) 3_757 . ?
O2W Co1 N2 92.3(2) . . ?
O2W Co1 N2 87.7(2) 3_757 . ?
O2 Co1 N2 90.88(18) . 3_757 ?
O2 Co1 N2 89.12(18) 3_757 3_757 ?
O2W Co1 N2 87.7(2) . 3_757 ?
O2W Co1 N2 92.3(2) 3_757 3_757 ?
N2 Co1 N2 179.999(1) . 3_757 ?
P1 O2 Co1 132.7(3) . . ?
O1 P1 O2 112.2(2) . . ?
O1 P1 O3 113.0(3) . . ?
O2 P1 O3 110.6(3) . . ?
O1 P1 C1 107.2(3) . . ?
O2 P1 C1 108.3(3) . . ?
O3 P1 C1 105.2(3) . . ?
O4 Co2 O3 158.90(18) . . ?
O4 Co2 O1 94.4(2) . 3_657 ?
O3 Co2 O1 101.3(2) . 3_657 ?
O4 Co2 N1 97.5(2) . . ?
O3 Co2 N1 96.21(19) . . ?
O1 Co2 N1 90.92(19) 3_657 . ?
O4 Co2 N3 80.7(2) . . ?
O3 Co2 N3 85.18(18) . . ?
O1 Co2 N3 90.34(19) 3_657 . ?
N1 Co2 N3 177.9(2) . . ?
O4 Co2 O1W 81.0(2) . . ?
O3 Co2 O1W 84.2(2) . . ?
O1 Co2 O1W 173.78(16) 3_657 . ?
N1 Co2 O1W 85.6(2) . . ?
N3 Co2 O1W 92.95(19) . . ?
N3 C1 P1 109.4(4) . . ?
N3 C1 H1A 109.8 . . ?
P1 C1 H1A 109.8 . . ?
N3 C1 H1B 109.8 . . ?
P1 C1 H1B 109.8 . . ?
H1A C1 H1B 108.2 . . ?
N3 C2 C3 113.0(6) . . ?
N3 C2 C19 109.4(6) . . ?
C3 C2 C19 112.6(5) . . ?
N3 C2 H2 107.2 . . ?
C3 C2 H2 107.2 . . ?
C19 C2 H2 107.2 . . ?
C4 C3 C8 119.4(6) . . ?
C4 C3 C2 120.8(7) . . ?
C8 C3 C2 119.8(6) . . ?
C3 C4 C5 121.1(7) . . ?
C3 C4 H4 119.5 . . ?
C5 C4 H4 119.5 . . ?
C6 C5 C4 118.6(7) . . ?
C6 C5 H5 120.7 . . ?
C4 C5 H5 120.7 . . ?
C5 C6 C7 121.5(7) . . ?
C5 C6 H6 119.2 . . ?
C7 C6 H6 119.2 . . ?
C6 C7 C8 119.7(8) . . ?
C6 C7 H7 120.2 . . ?
C8 C7 H7 120.2 . . ?
C7 C8 C3 119.7(7) . . ?
C7 C8 H8 120.2 . . ?
C3 C8 H8 120.2 . . ?
N1 C9 C18 123.6(6) . . ?
N1 C9 H9 118.2 . . ?
C18 C9 H9 118.2 . . ?
N1 C10 C17 123.9(6) . . ?
N1 C10 H10 118.1 . . ?
C17 C10 H10 118.1 . . ?
N2 C11 C12 123.1(7) . . ?
N2 C11 H11 118.4 . . ?
C12 C11 H11 118.4 . . ?
C13 C12 C11 119.8(7) . . ?
C13 C12 H12 120.1 . . ?
C11 C12 H12 120.1 . . ?
C14 C13 C12 116.7(7) . . ?
C14 C13 C16 123.0(7) . 2_656 ?
C12 C13 C16 120.2(7) . 2_656 ?
C13 C14 C15 120.4(7) . . ?
C13 C14 H14 119.8 . . ?
C15 C14 H14 119.8 . . ?
N2 C15 C14 122.8(7) . . ?
N2 C15 H15 118.6 . . ?
C14 C15 H15 118.6 . . ?
C18 C16 C17 116.8(6) . . ?
C18 C16 C13 122.3(6) . 2_646 ?
C17 C16 C13 120.9(6) . 2_646 ?
C10 C17 C16 119.7(6) . . ?
C10 C17 H17 120.2 . . ?
C16 C17 H17 120.2 . . ?
C9 C18 C16 119.7(6) . . ?
C9 C18 H18 120.2 . . ?
C16 C18 H18 120.1 . . ?
O5 C19 O4 125.6(7) . . ?
O5 C19 C2 114.6(7) . . ?
O4 C19 C2 119.7(6) . . ?
C10 N1 C9 116.4(6) . . ?
C10 N1 Co2 121.9(4) . . ?
C9 N1 Co2 121.7(5) . . ?
C2 N3 C1 115.7(5) . . ?
C2 N3 Co2 112.3(4) . . ?
C1 N3 Co2 109.1(4) . . ?
C2 N3 H3A 106.2 . . ?
C1 N3 H3A 106.4 . . ?
Co2 N3 H3A 106.6 . . ?
P1 O3 Co2 117.6(3) . . ?
C19 O4 Co2 117.6(4) . . ?
Co2 O1W H1WA 109.2 . . ?
Co2 O1W H1WB 110.5 . . ?
H1WA O1W H1WB 112.7 . . ?
Co1 O2W H2WA 109.0 . . ?
Co1 O2W H2WB 109.3 . . ?
H2WA O2W H2WB 109.5 . . ?

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
C15 N2 Co1 O2 -65.9(4) . . . . ?
C11 N2 Co1 O2 108.9(4) . . . . ?
C15 N2 Co1 O2 114.1(4) . . . 3_757 ?
C11 N2 Co1 O2 -71.1(4) . . . 3_757 ?
C15 N2 Co1 O2W -154.3(4) . . . . ?
C11 N2 Co1 O2W 20.5(4) . . . . ?
C15 N2 Co1 O2W 25.7(4) . . . 3_757 ?
C11 N2 Co1 O2W -159.5(4) . . . 3_757 ?
C15 N2 Co1 N2 39(7) . . . 3_757 ?
C11 N2 Co1 N2 -146(7) . . . 3_757 ?
O2 Co1 O2 P1 -26(15) 3_757 . . . ?
O2W Co1 O2 P1 36.2(4) . . . . ?
O2W Co1 O2 P1 -143.8(4) 3_757 . . . ?
N2 Co1 O2 P1 -56.1(4) . . . . ?
N2 Co1 O2 P1 123.9(4) 3_757 . . . ?
Co2 O1 P1 O2 -161.9(3) 3_657 . . . ?
Co2 O1 P1 O3 -36.0(4) 3_657 . . . ?
Co2 O1 P1 C1 79.4(4) 3_657 . . . ?
Co1 O2 P1 O1 -25.1(5) . . . . ?
Co1 O2 P1 O3 -152.3(3) . . . . ?
Co1 O2 P1 C1 93.0(4) . . . . ?
O1 P1 C1 N3 -91.1(5) . . . . ?
O2 P1 C1 N3 147.6(4) . . . . ?
O3 P1 C1 N3 29.4(5) . . . . ?
N3 C2 C3 C4 118.7(7) . . . . ?
C19 C2 C3 C4 -116.7(7) . . . . ?
N3 C2 C3 C8 -60.4(7) . . . . ?
C19 C2 C3 C8 64.2(8) . . . . ?
C8 C3 C4 C5 -0.7(10) . . . . ?
C2 C3 C4 C5 -179.7(6) . . . . ?
C3 C4 C5 C6 2.0(11) . . . . ?
C4 C5 C6 C7 -1.5(12) . . . . ?
C5 C6 C7 C8 -0.3(11) . . . . ?
C6 C7 C8 C3 1.7(10) . . . . ?
C4 C3 C8 C7 -1.2(10) . . . . ?
C2 C3 C8 C7 177.9(6) . . . . ?
C15 N2 C11 C12 -2.7(8) . . . . ?
Co1 N2 C11 C12 -177.7(4) . . . . ?
N2 C11 C12 C13 3.0(9) . . . . ?
C11 C12 C13 C14 -1.1(9) . . . . ?
C11 C12 C13 C16 179.7(5) . . . 2_656 ?
C12 C13 C14 C15 -0.9(9) . . . . ?
C16 C13 C14 C15 178.3(5) 2_656 . . . ?
C11 N2 C15 C14 0.6(8) . . . . ?
Co1 N2 C15 C14 175.7(4) . . . . ?
C13 C14 C15 N2 1.2(9) . . . . ?
N1 C10 C17 C16 0.6(12) . . . . ?
C18 C16 C17 C10 -1.5(11) . . . . ?
C13 C16 C17 C10 176.5(6) 2_646 . . . ?
N1 C9 C18 C16 -0.5(11) . . . . ?
C17 C16 C18 C9 1.4(10) . . . . ?
C13 C16 C18 C9 -176.5(6) 2_646 . . . ?
N3 C2 C19 O5 -174.5(5) . . . . ?
C3 C2 C19 O5 59.0(8) . . . . ?
N3 C2 C19 O4 2.0(8) . . . . ?
C3 C2 C19 O4 -124.5(7) . . . . ?
C17 C10 N1 C9 0.3(11) . . . . ?
C17 C10 N1 Co2 -179.9(5) . . . . ?
C18 C9 N1 C10 -0.4(10) . . . . ?
C18 C9 N1 Co2 179.8(5) . . . . ?
O4 Co2 N1 C10 167.7(6) . . . . ?
O3 Co2 N1 C10 3.7(6) . . . . ?
O1 Co2 N1 C10 -97.8(6) 3_657 . . . ?
N3 Co2 N1 C10 135(5) . . . . ?
O1W Co2 N1 C10 87.4(6) . . . . ?
O4 Co2 N1 C9 -12.5(6) . . . . ?
O3 Co2 N1 C9 -176.5(5) . . . . ?
O1 Co2 N1 C9 82.0(6) 3_657 . . . ?
N3 Co2 N1 C9 -45(5) . . . . ?
O1W Co2 N1 C9 -92.8(6) . . . . ?
C3 C2 N3 C1 -105.5(6) . . . . ?
C19 C2 N3 C1 128.2(6) . . . . ?
C3 C2 N3 Co2 128.4(5) . . . . ?
C19 C2 N3 Co2 2.1(6) . . . . ?
P1 C1 N3 C2 -167.2(5) . . . . ?
P1 C1 N3 Co2 -39.5(5) . . . . ?
O4 Co2 N3 C2 -3.7(4) . . . . ?
O3 Co2 N3 C2 160.6(4) . . . . ?
O1 Co2 N3 C2 -98.0(4) 3_657 . . . ?
N1 Co2 N3 C2 29(5) . . . . ?
O1W Co2 N3 C2 76.7(4) . . . . ?
O4 Co2 N3 C1 -133.3(5) . . . . ?
O3 Co2 N3 C1 31.0(4) . . . . ?
O1 Co2 N3 C1 132.4(4) 3_657 . . . ?
N1 Co2 N3 C1 -101(5) . . . . ?
O1W Co2 N3 C1 -52.9(4) . . . . ?
O1 P1 O3 Co2 111.9(3) . . . . ?
O2 P1 O3 Co2 -121.4(3) . . . . ?
C1 P1 O3 Co2 -4.7(4) . . . . ?
O4 Co2 O3 P1 35.0(7) . . . . ?
O1 Co2 O3 P1 -102.3(3) 3_657 . . . ?
N1 Co2 O3 P1 165.5(3) . . . . ?
N3 Co2 O3 P1 -12.9(3) . . . . ?
O1W Co2 O3 P1 80.5(3) . . . . ?
O5 C19 O4 Co2 170.6(5) . . . . ?
C2 C19 O4 Co2 -5.5(8) . . . . ?
O3 Co2 O4 C19 -43.5(8) . . . . ?
O1 Co2 O4 C19 94.7(5) 3_657 . . . ?
N1 Co2 O4 C19 -173.8(5) . . . . ?
N3 Co2 O4 C19 5.1(5) . . . . ?
O1W Co2 O4 C19 -89.4(5) . . . . ?

_diffrn_measured_fraction_theta_max 0.987
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.987
_refine_diff_density_max         0.641
_refine_diff_density_min         -0.825
_refine_diff_density_rms         0.115
_database_code_depnum_ccdc_archive 'CCDC 947903'