# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2014

#######################################################################
#
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#                                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.
#
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#  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
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#  data retrieval see:
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#  from this site to visualise CIF-encoded structures and 
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data_2009skc0031

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C38 H39 N4 Ni O8.50 P2 S4'
_chemical_formula_weight         936.62

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 '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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P21

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

_cell_length_a                   9.6133(2)
_cell_length_b                   45.6542(12)
_cell_length_c                   10.5801(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 113.2020(10)
_cell_angle_gamma                90.00
_cell_volume                     4267.92(19)
_cell_formula_units_Z            4
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    92767
_cell_measurement_theta_min      2.91
_cell_measurement_theta_max      27.10

_exptl_crystal_description       block
_exptl_crystal_colour            'pale green'
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.458
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1940
_exptl_absorpt_coefficient_mu    0.781
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8408
_exptl_absorpt_correction_T_max  0.9620
_exptl_absorpt_process_details   'SADABS 2007/2 (Sheldrick, G.M., 2007)'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Bruker-Nonius FR591 rotating anode'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  
'Bruker-Nonius Roper CCD camera on κ-goniostat'
_diffrn_measurement_method       'φ & ω scans'
_diffrn_detector_area_resol_mean 9.091
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            44414
_diffrn_reflns_av_R_equivalents  0.0656
_diffrn_reflns_av_sigmaI/netI    0.1062
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -58
_diffrn_reflns_limit_k_max       58
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         2.92
_diffrn_reflns_theta_max         27.12
_reflns_number_total             18504
_reflns_number_gt                13551
_reflns_threshold_expression     >2σ(I)


_computing_data_collection       'COLLECT (Hooft, R.W.W., 1998)'
_computing_cell_refinement       
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)'
#Although determined using DirAx, the cell is refined in the HKL
#package during data reduction
_computing_data_reduction        
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)'
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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 > 2σ(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.

 N-H and water O-H bond distances restrained; thermal parameters of N-H
 hydrogen atoms riding on their parent atom.

 Possible disordered water molecule at 0.3894,1.0787, -0.0175 -on modelling
 the Q-peak as an oxygen atom, the site is found to be approximately 1/4
 occupied. It is not possible to be certain whether this is indeed
 a water molecule or is just an artefact.
;

_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)+(0.0550P)²+0.0000P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.048(12)
_refine_ls_number_reflns         18504
_refine_ls_number_parameters     1068
_refine_ls_number_restraints     8
_refine_ls_R_factor_all          0.0894
_refine_ls_R_factor_gt           0.0587
_refine_ls_wR_factor_ref         0.1325
_refine_ls_wR_factor_gt          0.1199
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_restrained_S_all      1.019
_refine_ls_shift/su_max          0.016
_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 -1.3938(7) 1.12820(14) -0.8987(7) 0.0465(16) Uani 1 1 d . . .
H1A H -1.3459 1.1235 -0.9627 0.070 Uiso 1 1 calc R . .
H1B H -1.5039 1.1286 -0.9487 0.070 Uiso 1 1 calc R . .
H1C H -1.3666 1.1133 -0.8264 0.070 Uiso 1 1 calc R . .
C2 C -0.9170(6) 1.14428(14) -0.6790(7) 0.0472(16) Uani 1 1 d . . .
H2A H -0.8737 1.1250 -0.6444 0.071 Uiso 1 1 calc R . .
H2B H -0.8806 1.1586 -0.6041 0.071 Uiso 1 1 calc R . .
H2C H -0.8862 1.1503 -0.7530 0.071 Uiso 1 1 calc R . .
C3 C -1.2898(6) 1.30222(14) -1.1780(7) 0.0501(17) Uani 1 1 d . . .
H3A H -1.3194 1.2845 -1.2349 0.075 Uiso 1 1 calc R . .
H3B H -1.3379 1.3194 -1.2339 0.075 Uiso 1 1 calc R . .
H3C H -1.3223 1.3005 -1.1014 0.075 Uiso 1 1 calc R . .
C4 C -0.8225(6) 1.32466(12) -0.9799(6) 0.0403(15) Uani 1 1 d . . .
H4A H -0.8653 1.3299 -0.9127 0.060 Uiso 1 1 calc R . .
H4B H -0.8638 1.3377 -1.0596 0.060 Uiso 1 1 calc R . .
H4C H -0.7122 1.3267 -0.9376 0.060 Uiso 1 1 calc R . .
C5 C 0.7452(7) 0.88971(13) 0.6333(7) 0.0482(17) Uani 1 1 d . . .
H5A H 0.8169 0.8733 0.6574 0.072 Uiso 1 1 calc R . .
H5B H 0.6609 0.8850 0.6598 0.072 Uiso 1 1 calc R . .
H5C H 0.7966 0.9074 0.6820 0.072 Uiso 1 1 calc R . .
C6 C 0.4908(9) 0.94236(18) 0.1812(7) 0.070(2) Uani 1 1 d . . .
H6A H 0.3994 0.9485 0.1939 0.105 Uiso 1 1 calc R . .
H6B H 0.4632 0.9355 0.0866 0.105 Uiso 1 1 calc R . .
H6C H 0.5604 0.9590 0.1990 0.105 Uiso 1 1 calc R . .
C7 C 0.4994(8) 1.00350(17) 0.9663(7) 0.064(2) Uani 1 1 d . . .
H7A H 0.4234 0.9880 0.9482 0.096 Uiso 1 1 calc R . .
H7B H 0.5296 1.0105 1.0608 0.096 Uiso 1 1 calc R . .
H7C H 0.5882 0.9957 0.9538 0.096 Uiso 1 1 calc R . .
C8 C 0.2684(6) 1.05695(13) 0.5077(6) 0.0395(14) Uani 1 1 d . . .
H8A H 0.1999 1.0414 0.4546 0.059 Uiso 1 1 calc R . .
H8B H 0.3574 1.0576 0.4844 0.059 Uiso 1 1 calc R . .
H8C H 0.2159 1.0758 0.4858 0.059 Uiso 1 1 calc R . .
C22 C -0.7939(6) 1.19745(12) -0.8903(5) 0.0310(12) Uani 1 1 d . . .
H22 H -0.8435 1.1945 -0.9867 0.037 Uiso 1 1 calc R . .
C23 C -0.6502(6) 1.18583(12) -0.8223(5) 0.0319(13) Uani 1 1 d . . .
H23 H -0.6023 1.1753 -0.8714 0.038 Uiso 1 1 calc R . .
C24 C -0.5770(5) 1.18988(11) -0.6799(5) 0.0270(12) Uani 1 1 d . . .
C25 C -0.6494(6) 1.20600(11) -0.6146(5) 0.0300(12) Uani 1 1 d . . .
H25 H -0.6019 1.2094 -0.5183 0.036 Uiso 1 1 calc R . .
C26 C -0.7917(5) 1.21733(11) -0.6894(5) 0.0257(11) Uani 1 1 d . . .
H26 H -0.8389 1.2288 -0.6427 0.031 Uiso 1 1 calc R . .
C28 C -0.3345(6) 1.18074(11) -0.4806(5) 0.0291(12) Uani 1 1 d . . .
C29 C -0.1935(5) 1.16217(11) -0.4308(5) 0.0231(11) Uani 1 1 d . . .
C30 C -0.0590(6) 1.17666(11) -0.3664(5) 0.0272(12) Uani 1 1 d . . .
H30 H -0.0600 1.1972 -0.3538 0.033 Uiso 1 1 calc R . .
C31 C 0.0806(5) 1.16172(12) -0.3184(5) 0.0293(12) Uani 1 1 d . . .
C32 C 0.2210(6) 1.17712(13) -0.2642(6) 0.0442(16) Uani 1 1 d . . .
H32 H 0.2216 1.1978 -0.2554 0.053 Uiso 1 1 calc R . .
C33 C 0.3547(7) 1.16222(15) -0.2250(7) 0.0536(18) Uani 1 1 d . . .
H33 H 0.4477 1.1726 -0.1900 0.064 Uiso 1 1 calc R . .
C34 C 0.3553(6) 1.13098(13) -0.2364(6) 0.0416(15) Uani 1 1 d . . .
H34 H 0.4482 1.1206 -0.2098 0.050 Uiso 1 1 calc R . .
C35 C 0.2224(6) 1.11650(12) -0.2855(6) 0.0338(13) Uani 1 1 d . . .
H35 H 0.2245 1.0957 -0.2908 0.041 Uiso 1 1 calc R . .
C36 C 0.0791(6) 1.13067(11) -0.3298(5) 0.0283(12) Uani 1 1 d . . .
C37 C -0.0611(5) 1.11534(11) -0.3863(5) 0.0265(11) Uani 1 1 d . . .
C38 C -0.1926(5) 1.13151(11) -0.4399(5) 0.0245(11) Uani 1 1 d . . .
C40 C -0.4223(7) 1.11401(15) -0.4367(7) 0.0562(18) Uani 1 1 d . . .
H40A H -0.3967 1.0960 -0.3820 0.084 Uiso 1 1 calc R . .
H40B H -0.5285 1.1133 -0.5013 0.084 Uiso 1 1 calc R . .
H40C H -0.4068 1.1309 -0.3755 0.084 Uiso 1 1 calc R . .
C42 C 0.4648(6) 1.01679(12) 0.3426(5) 0.0315(12) Uani 1 1 d . . .
H42 H 0.5662 1.0222 0.3975 0.038 Uiso 1 1 calc R . .
C43 C 0.3919(6) 1.03094(12) 0.2189(6) 0.0352(13) Uani 1 1 d . . .
H43 H 0.4415 1.0461 0.1913 0.042 Uiso 1 1 calc R . .
C44 C 0.2423(5) 1.02258(12) 0.1334(5) 0.0320(12) Uani 1 1 d . . .
C45 C 0.1733(6) 1.00161(12) 0.1835(5) 0.0339(13) Uani 1 1 d . . .
H45 H 0.0715 0.9959 0.1317 0.041 Uiso 1 1 calc R . .
C46 C 0.2543(6) 0.98910(11) 0.3098(5) 0.0313(12) Uani 1 1 d . . .
H46 H 0.2044 0.9749 0.3427 0.038 Uiso 1 1 calc R . .
C48 C 0.0771(6) 1.02073(11) -0.1089(5) 0.0290(12) Uani 1 1 d . . .
C49 C 0.0081(5) 1.03761(11) -0.2430(5) 0.0269(11) Uani 1 1 d . . .
C50 C -0.0298(5) 1.02127(11) -0.3607(5) 0.0271(11) Uani 1 1 d . . .
H50 H -0.0209 1.0006 -0.3536 0.033 Uiso 1 1 calc R . .
C51 C -0.0812(5) 1.03421(11) -0.4907(5) 0.0260(11) Uani 1 1 d . . .
C52 C -0.1067(5) 1.01695(11) -0.6106(5) 0.0294(12) Uani 1 1 d . . .
H52 H -0.0952 0.9963 -0.6026 0.035 Uiso 1 1 calc R . .
C53 C -0.1475(6) 1.02988(13) -0.7370(6) 0.0375(14) Uani 1 1 d . . .
H53 H -0.1636 1.0183 -0.8162 0.045 Uiso 1 1 calc R . .
C54 C -0.1652(6) 1.06032(13) -0.7483(6) 0.0377(14) Uani 1 1 d . . .
H54 H -0.1951 1.0692 -0.8363 0.045 Uiso 1 1 calc R . .
C55 C -0.1408(6) 1.07766(11) -0.6365(5) 0.0311(12) Uani 1 1 d . . .
H55 H -0.1542 1.0982 -0.6478 0.037 Uiso 1 1 calc R . .
C56 C -0.0954(5) 1.06512(11) -0.5027(5) 0.0262(11) Uani 1 1 d . . .
C57 C -0.0588(5) 1.08238(10) -0.3807(5) 0.0247(11) Uani 1 1 d . . .
C58 C -0.0061(6) 1.06860(12) -0.2544(5) 0.0292(12) Uani 1 1 d . . .
C60 C -0.0794(8) 1.09222(18) -0.0919(7) 0.064(2) Uani 1 1 d . . .
H60A H -0.1303 1.0741 -0.0841 0.095 Uiso 1 1 calc R . .
H60B H -0.1526 1.1053 -0.1590 0.095 Uiso 1 1 calc R . .
H60C H -0.0368 1.1020 -0.0022 0.095 Uiso 1 1 calc R . .
C62 C 0.5503(6) 0.93113(12) 0.8069(6) 0.0341(13) Uani 1 1 d . . .
H62 H 0.4491 0.9257 0.7511 0.041 Uiso 1 1 calc R . .
C63 C -1.6207(6) 1.41735(12) -0.9327(6) 0.0348(13) Uani 1 1 d . . .
H63 H -1.5707 1.4022 -0.9598 0.042 Uiso 1 1 calc R . .
C64 C -1.7674(5) 1.42620(11) -1.0198(5) 0.0293(12) Uani 1 1 d . . .
C65 C -1.8379(6) 1.44697(12) -0.9680(5) 0.0305(12) Uani 1 1 d . . .
H65 H -1.9389 1.4530 -1.0207 0.037 Uiso 1 1 calc R . .
C66 C -1.7586(5) 1.45868(12) -0.8390(6) 0.0320(12) Uani 1 1 d . . .
H66 H -1.8083 1.4726 -0.8047 0.038 Uiso 1 1 calc R . .
C68 C -1.9404(6) 1.42718(11) -1.2627(5) 0.0288(12) Uani 1 1 d . . .
C69 C -2.0091(6) 1.40887(11) -1.3885(5) 0.0273(12) Uani 1 1 d . . .
C70 C -2.0439(5) 1.42177(10) -1.5143(5) 0.0255(11) Uani 1 1 d . . .
H70 H -2.0303 1.4423 -1.5188 0.031 Uiso 1 1 calc R . .
C71 C -2.0991(5) 1.40552(11) -1.6366(5) 0.0267(12) Uani 1 1 d . . .
C72 C -2.1293(6) 1.41909(12) -1.7674(6) 0.0360(13) Uani 1 1 d . . .
H72 H -2.1165 1.4396 -1.7720 0.043 Uiso 1 1 calc R . .
C73 C -2.1754(7) 1.40303(14) -1.8834(6) 0.0409(14) Uani 1 1 d . . .
H73 H -2.1952 1.4123 -1.9693 0.049 Uiso 1 1 calc R . .
C74 C -2.1942(7) 1.37259(15) -1.8775(6) 0.0454(15) Uani 1 1 d . . .
H74 H -2.2262 1.3616 -1.9603 0.055 Uiso 1 1 calc R . .
C75 C -2.1680(6) 1.35830(12) -1.7568(5) 0.0337(13) Uani 1 1 d . . .
H75 H -2.1818 1.3377 -1.7562 0.040 Uiso 1 1 calc R . .
C76 C -2.1196(5) 1.37465(11) -1.6314(5) 0.0245(11) Uani 1 1 d . . .
C77 C -2.0918(5) 1.36120(10) -1.5016(5) 0.0232(11) Uani 1 1 d . . .
C78 C -2.0408(5) 1.37805(10) -1.3846(5) 0.0236(11) Uani 1 1 d . . .
C80 C -2.1315(6) 1.37313(14) -1.2100(6) 0.0419(14) Uani 1 1 d . . .
H80A H -2.1330 1.3945 -1.2015 0.063 Uiso 1 1 calc R . .
H80B H -2.1071 1.3641 -1.1197 0.063 Uiso 1 1 calc R . .
H80C H -2.2310 1.3663 -1.2740 0.063 Uiso 1 1 calc R . .
C82 C -1.3972(5) 1.25116(11) -0.9571(5) 0.0273(12) Uani 1 1 d . . .
H82 H -1.3464 1.2555 -0.8620 0.033 Uiso 1 1 calc R . .
C83 C -1.5447(5) 1.26103(12) -1.0251(5) 0.0286(12) Uani 1 1 d . . .
H83 H -1.5933 1.2715 -0.9765 0.034 Uiso 1 1 calc R . .
C84 C -1.6209(5) 1.25546(10) -1.1647(5) 0.0236(11) Uani 1 1 d . . .
C85 C -1.5443(5) 1.23902(11) -1.2309(5) 0.0260(11) Uani 1 1 d . . .
H85 H -1.5915 1.2344 -1.3259 0.031 Uiso 1 1 calc R . .
C86 C -1.3986(5) 1.22997(11) -1.1524(5) 0.0247(11) Uani 1 1 d . . .
H86 H -1.3481 1.2187 -1.1969 0.030 Uiso 1 1 calc R . .
C88 C -1.8620(5) 1.26089(11) -1.3661(5) 0.0254(11) Uani 1 1 d . . .
C89 C -2.0011(5) 1.28062(11) -1.4253(5) 0.0233(10) Uani 1 1 d . . .
C90 C -2.1412(5) 1.26764(10) -1.4795(5) 0.0245(11) Uani 1 1 d . . .
H90 H -2.1495 1.2469 -1.4794 0.029 Uiso 1 1 calc R . .
C91 C -2.2738(5) 1.28513(11) -1.5359(5) 0.0258(11) Uani 1 1 d . . .
C92 C -2.4207(5) 1.27184(12) -1.5899(5) 0.0303(12) Uani 1 1 d . . .
H92 H -2.4301 1.2512 -1.5872 0.036 Uiso 1 1 calc R . .
C93 C -2.5470(6) 1.28878(12) -1.6451(6) 0.0362(13) Uani 1 1 d . . .
H93 H -2.6441 1.2799 -1.6844 0.043 Uiso 1 1 calc R . .
C94 C -2.5333(6) 1.31927(13) -1.6437(6) 0.0356(13) Uani 1 1 d . . .
H94 H -2.6223 1.3309 -1.6776 0.043 Uiso 1 1 calc R . .
C95 C -2.3951(6) 1.33279(12) -1.5948(5) 0.0295(12) Uani 1 1 d . . .
H95 H -2.3895 1.3535 -1.5972 0.035 Uiso 1 1 calc R . .
C96 C -2.2591(5) 1.31592(11) -1.5401(5) 0.0261(11) Uani 1 1 d . . .
C97 C -2.1145(5) 1.32893(10) -1.4911(5) 0.0236(11) Uani 1 1 d . . .
C98 C -1.9871(5) 1.31122(11) -1.4328(5) 0.0240(11) Uani 1 1 d . . .
C100 C -1.7616(6) 1.31809(13) -1.4679(6) 0.0416(14) Uani 1 1 d . . .
H10A H -1.8251 1.3226 -1.5640 0.062 Uiso 1 1 calc R . .
H10B H -1.7329 1.2974 -1.4599 0.062 Uiso 1 1 calc R . .
H10C H -1.6702 1.3302 -1.4374 0.062 Uiso 1 1 calc R . .
O1 O -1.3422(4) 1.15633(8) -0.8379(4) 0.0392(9) Uani 1 1 d . . .
O2 O -1.0806(4) 1.14261(8) -0.7314(4) 0.0392(9) Uani 1 1 d . . .
O3 O -1.1288(4) 1.30548(8) -1.1252(4) 0.0378(9) Uani 1 1 d . . .
O4 O -0.8619(4) 1.29444(8) -1.0244(4) 0.0359(9) Uani 1 1 d . . .
O5 O 0.6878(5) 0.89478(9) 0.4866(5) 0.0491(11) Uani 1 1 d . . .
O6 O 0.5637(5) 0.91892(10) 0.2758(5) 0.0528(12) Uani 1 1 d . . .
O7 O 0.4341(4) 1.02823(9) 0.8686(4) 0.0450(10) Uani 1 1 d . . .
O8 O 0.3155(4) 1.05104(8) 0.6524(4) 0.0402(10) Uani 1 1 d . . .
O28 O -0.3528(5) 1.19990(10) -0.4084(4) 0.0521(12) Uani 1 1 d . . .
O39 O -0.3291(4) 1.11669(8) -0.5104(4) 0.0377(9) Uani 1 1 d . . .
O48 O 0.0531(4) 0.99458(8) -0.1071(4) 0.0395(9) Uani 1 1 d . . .
O59 O 0.0392(4) 1.08539(8) -0.1360(3) 0.0350(9) Uani 1 1 d . . .
O68 O -1.9698(4) 1.45351(8) -1.2622(4) 0.0353(9) Uani 1 1 d . . .
O79 O -2.0189(4) 1.36496(8) -1.2612(3) 0.0292(8) Uani 1 1 d . . .
O88 O -1.8457(4) 1.24051(8) -1.4321(4) 0.0369(9) Uani 1 1 d . . .
O99 O -1.8445(4) 1.32399(7) -1.3835(4) 0.0287(8) Uani 1 1 d . . .
P1 P -1.18080(15) 1.16893(3) -0.82280(15) 0.0306(3) Uani 1 1 d . . .
P2 P -1.01881(15) 1.28070(3) -1.03098(14) 0.0288(3) Uani 1 1 d . . .
P3 P 0.59428(17) 0.92454(3) 0.43312(17) 0.0386(4) Uani 1 1 d . . .
P4 P 0.41135(15) 1.02214(3) 0.71351(15) 0.0336(3) Uani 1 1 d . . .
S1 S -1.16039(15) 1.17212(3) -1.00166(14) 0.0328(3) Uani 1 1 d . . .
S2 S -1.14552(15) 1.20628(3) -0.72221(13) 0.0305(3) Uani 1 1 d . . .
S3 S -1.03038(15) 1.27781(3) -0.84832(14) 0.0325(3) Uani 1 1 d . . .
S4 S -1.04724(14) 1.24243(3) -1.12448(13) 0.0294(3) Uani 1 1 d . . .
S5 S 0.40296(15) 0.92526(3) 0.46283(15) 0.0352(3) Uani 1 1 d . . .
S6 S 0.71660(15) 0.96009(3) 0.50616(16) 0.0353(3) Uani 1 1 d . . .
S7 S 0.29407(14) 0.98579(3) 0.63954(15) 0.0323(3) Uani 1 1 d . . .
S8 S 0.60682(15) 1.02197(3) 0.69072(15) 0.0338(3) Uani 1 1 d . . .
Ni1 Ni -1.09450(7) 1.224679(14) -0.92239(6) 0.02336(14) Uani 1 1 d . . .
Ni2 Ni 0.50709(7) 0.973630(15) 0.57484(7) 0.02774(15) Uani 1 1 d . . .
N1 N -0.8664(4) 1.21282(9) -0.8251(4) 0.0253(9) Uani 1 1 d . . .
N2 N 0.3991(4) 0.99554(10) 0.3900(5) 0.0314(10) Uani 1 1 d . . .
N3 N -1.3227(4) 1.23579(9) -1.0188(4) 0.0260(9) Uani 1 1 d . . .
N4 N 0.6166(4) 0.95151(9) 0.7601(4) 0.0299(10) Uani 1 1 d . . .
N27 N -0.4355(5) 1.17593(10) -0.6118(4) 0.0297(10) Uani 1 1 d D . .
N47 N 0.1690(5) 1.03579(10) 0.0053(5) 0.0355(11) Uani 1 1 d D . .
N67 N -1.8378(5) 1.41358(9) -1.1494(4) 0.0305(10) Uani 1 1 d D . .
N87 N -1.7644(4) 1.26745(9) -1.2373(4) 0.0262(10) Uani 1 1 d D . .
H27 H -0.389(5) 1.1667(10) -0.660(4) 0.031 Uiso 1 1 d D . .
H47 H 0.201(5) 1.0537(6) -0.005(5) 0.031 Uiso 1 1 d D . .
H67 H -1.805(5) 1.3955(6) -1.157(5) 0.031 Uiso 1 1 d D . .
H87 H -1.795(5) 1.2768(11) -1.181(4) 0.031 Uiso 1 1 d D . .
O1W O -1.6621(4) 1.36474(9) -1.1812(4) 0.0387(9) Uani 1 1 d D . .
H1W H -1.712(5) 1.3512(8) -1.235(4) 0.032(16) Uiso 1 1 d D . .
H2W H -1.635(5) 1.3752(9) -1.235(4) 0.027(15) Uiso 1 1 d D . .


_geom_special_details            
;
 All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell s.u.'s are taken
 into account individually in the estimation of s.u.'s in distances, angles
 and torsion angles; correlations between s.u.'s in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell s.u.'s is used for estimating s.u.'s 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 O1 1.434(7) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 O2 1.448(6) . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C3 O3 1.431(6) . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C4 O4 1.459(6) . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C5 O5 1.446(8) . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 O6 1.444(9) . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 O7 1.492(8) . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 O8 1.440(7) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C22 N1 1.353(6) . ?
C22 C23 1.387(7) . ?
C22 H22 0.9500 . ?
C23 C24 1.401(7) . ?
C23 H23 0.9500 . ?
C24 C25 1.371(7) . ?
C24 N27 1.416(6) . ?
C25 C26 1.383(7) . ?
C25 H25 0.9500 . ?
C26 N1 1.345(6) . ?
C26 H26 0.9500 . ?
C28 O28 1.218(6) . ?
C28 N27 1.363(6) . ?
C28 C29 1.507(7) . ?
C29 C30 1.371(7) . ?
C29 C38 1.403(7) . ?
C30 C31 1.410(7) . ?
C30 H30 0.9500 . ?
C31 C36 1.423(7) . ?
C31 C32 1.427(7) . ?
C32 C33 1.366(8) . ?
C32 H32 0.9500 . ?
C33 C34 1.432(9) . ?
C33 H33 0.9500 . ?
C34 C35 1.348(7) . ?
C34 H34 0.9500 . ?
C35 C36 1.424(7) . ?
C35 H35 0.9500 . ?
C36 C37 1.424(7) . ?
C37 C38 1.378(7) . ?
C37 C57 1.506(7) . ?
C38 O39 1.402(6) . ?
C40 O39 1.406(7) . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C40 H40C 0.9800 . ?
C42 N2 1.357(7) . ?
C42 C43 1.378(7) . ?
C42 H42 0.9500 . ?
C43 C44 1.417(7) . ?
C43 H43 0.9500 . ?
C44 C45 1.384(7) . ?
C44 N47 1.395(7) . ?
C45 C46 1.378(7) . ?
C45 H45 0.9500 . ?
C46 N2 1.347(6) . ?
C46 H46 0.9500 . ?
C48 O48 1.218(6) . ?
C48 N47 1.368(7) . ?
C48 C49 1.519(7) . ?
C49 C50 1.372(7) . ?
C49 C58 1.422(7) . ?
C50 C51 1.396(7) . ?
C50 H50 0.9500 . ?
C51 C56 1.418(7) . ?
C51 C52 1.431(7) . ?
C52 C53 1.370(8) . ?
C52 H52 0.9500 . ?
C53 C54 1.399(8) . ?
C53 H53 0.9500 . ?
C54 C55 1.365(8) . ?
C54 H54 0.9500 . ?
C55 C56 1.427(7) . ?
C55 H55 0.9500 . ?
C56 C57 1.433(7) . ?
C57 C58 1.380(7) . ?
C58 O59 1.384(6) . ?
C60 O59 1.426(7) . ?
C60 H60A 0.9800 . ?
C60 H60B 0.9800 . ?
C60 H60C 0.9800 . ?
C62 N4 1.329(7) . ?
C62 C63 1.384(7) 2_445 ?
C62 H62 0.9500 . ?
C63 C62 1.384(7) 2_455 ?
C63 C64 1.406(7) . ?
C63 H63 0.9500 . ?
C64 N67 1.393(6) . ?
C64 C65 1.396(7) . ?
C65 C66 1.382(7) . ?
C65 H65 0.9500 . ?
C66 N4 1.330(6) 2_455 ?
C66 H66 0.9500 . ?
C68 O68 1.235(6) . ?
C68 N67 1.365(7) . ?
C68 C69 1.488(7) . ?
C69 C70 1.372(7) . ?
C69 C78 1.443(7) . ?
C70 C71 1.402(7) . ?
C70 H70 0.9500 . ?
C71 C76 1.427(7) . ?
C71 C72 1.437(7) . ?
C72 C73 1.346(8) . ?
C72 H72 0.9500 . ?
C73 C74 1.406(8) . ?
C73 H73 0.9500 . ?
C74 C75 1.366(8) . ?
C74 H74 0.9500 . ?
C75 C76 1.432(7) . ?
C75 H75 0.9500 . ?
C76 C77 1.429(7) . ?
C77 C78 1.374(7) . ?
C77 C97 1.500(6) . ?
C78 O79 1.374(6) . ?
C80 O79 1.437(6) . ?
C80 H80A 0.9800 . ?
C80 H80B 0.9800 . ?
C80 H80C 0.9800 . ?
C82 N3 1.342(6) . ?
C82 C83 1.389(6) . ?
C82 H82 0.9500 . ?
C83 C84 1.390(7) . ?
C83 H83 0.9500 . ?
C84 N87 1.399(6) . ?
C84 C85 1.414(7) . ?
C85 C86 1.381(6) . ?
C85 H85 0.9500 . ?
C86 N3 1.337(6) . ?
C86 H86 0.9500 . ?
C88 O88 1.210(6) . ?
C88 N87 1.349(6) . ?
C88 C89 1.527(6) . ?
C89 C90 1.373(7) . ?
C89 C98 1.409(7) . ?
C90 C91 1.421(7) . ?
C90 H90 0.9500 . ?
C91 C96 1.415(7) . ?
C91 C92 1.433(7) . ?
C92 C93 1.362(7) . ?
C92 H92 0.9500 . ?
C93 C94 1.398(8) . ?
C93 H93 0.9500 . ?
C94 C95 1.368(7) . ?
C94 H94 0.9500 . ?
C95 C96 1.429(7) . ?
C95 H95 0.9500 . ?
C96 C97 1.409(7) . ?
C97 C98 1.392(7) . ?
C98 O99 1.389(6) . ?
C100 O99 1.437(7) . ?
C100 H10A 0.9800 . ?
C100 H10B 0.9800 . ?
C100 H10C 0.9800 . ?
O1 P1 1.603(4) . ?
O2 P1 1.604(4) . ?
O3 P2 1.601(4) . ?
O4 P2 1.610(4) . ?
O5 P3 1.604(4) . ?
O6 P3 1.593(4) . ?
O7 P4 1.592(4) . ?
O8 P4 1.594(4) . ?
P1 S2 1.968(2) . ?
P1 S1 1.983(2) . ?
P2 S4 1.973(2) . ?
P2 S3 1.983(2) . ?
P3 S6 1.975(2) . ?
P3 S5 1.984(2) . ?
P4 S7 1.986(2) . ?
P4 S8 1.987(2) . ?
S1 Ni1 2.5386(15) . ?
S2 Ni1 2.5001(14) . ?
S3 Ni1 2.5487(15) . ?
S4 Ni1 2.4900(15) . ?
S5 Ni2 2.5195(15) . ?
S6 Ni2 2.4738(15) . ?
S7 Ni2 2.4648(15) . ?
S8 Ni2 2.5231(15) . ?
Ni1 N3 2.085(4) . ?
Ni1 N1 2.093(4) . ?
Ni2 N2 2.075(4) . ?
Ni2 N4 2.084(4) . ?
N4 C66 1.330(6) 2_445 ?
N27 H27 0.90(2) . ?
N47 H47 0.897(19) . ?
N67 H67 0.898(19) . ?
N87 H87 0.874(19) . ?
O1W H1W 0.853(19) . ?
O1W H2W 0.855(19) . ?

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
O1 C1 H1A 109.5 . . ?
O1 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
O1 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
O2 C2 H2A 109.5 . . ?
O2 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
O2 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
O3 C3 H3A 109.5 . . ?
O3 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
O3 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
O4 C4 H4A 109.5 . . ?
O4 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
O4 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
O5 C5 H5A 109.5 . . ?
O5 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
O5 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
O6 C6 H6A 109.5 . . ?
O6 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
O6 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
O7 C7 H7A 109.5 . . ?
O7 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
O7 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
O8 C8 H8A 109.5 . . ?
O8 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
O8 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N1 C22 C23 122.8(5) . . ?
N1 C22 H22 118.6 . . ?
C23 C22 H22 118.6 . . ?
C22 C23 C24 118.9(5) . . ?
C22 C23 H23 120.6 . . ?
C24 C23 H23 120.6 . . ?
C25 C24 C23 118.2(5) . . ?
C25 C24 N27 124.2(5) . . ?
C23 C24 N27 117.5(5) . . ?
C24 C25 C26 119.8(5) . . ?
C24 C25 H25 120.1 . . ?
C26 C25 H25 120.1 . . ?
N1 C26 C25 123.1(5) . . ?
N1 C26 H26 118.5 . . ?
C25 C26 H26 118.5 . . ?
O28 C28 N27 122.3(5) . . ?
O28 C28 C29 121.1(4) . . ?
N27 C28 C29 116.5(5) . . ?
C30 C29 C38 119.0(4) . . ?
C30 C29 C28 116.4(4) . . ?
C38 C29 C28 124.5(4) . . ?
C29 C30 C31 121.6(5) . . ?
C29 C30 H30 119.2 . . ?
C31 C30 H30 119.2 . . ?
C30 C31 C36 118.3(5) . . ?
C30 C31 C32 121.5(5) . . ?
C36 C31 C32 120.1(5) . . ?
C33 C32 C31 120.3(6) . . ?
C33 C32 H32 119.8 . . ?
C31 C32 H32 119.8 . . ?
C32 C33 C34 120.3(6) . . ?
C32 C33 H33 119.8 . . ?
C34 C33 H33 119.8 . . ?
C35 C34 C33 119.1(5) . . ?
C35 C34 H34 120.4 . . ?
C33 C34 H34 120.4 . . ?
C34 C35 C36 123.5(5) . . ?
C34 C35 H35 118.3 . . ?
C36 C35 H35 118.3 . . ?
C31 C36 C37 120.1(5) . . ?
C31 C36 C35 116.6(5) . . ?
C37 C36 C35 123.2(5) . . ?
C38 C37 C36 118.2(5) . . ?
C38 C37 C57 123.3(4) . . ?
C36 C37 C57 118.5(4) . . ?
C37 C38 O39 118.3(4) . . ?
C37 C38 C29 122.4(5) . . ?
O39 C38 C29 119.2(4) . . ?
O39 C40 H40A 109.5 . . ?
O39 C40 H40B 109.5 . . ?
H40A C40 H40B 109.5 . . ?
O39 C40 H40C 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
N2 C42 C43 123.3(5) . . ?
N2 C42 H42 118.3 . . ?
C43 C42 H42 118.3 . . ?
C42 C43 C44 119.3(5) . . ?
C42 C43 H43 120.4 . . ?
C44 C43 H43 120.4 . . ?
C45 C44 N47 122.5(5) . . ?
C45 C44 C43 117.4(5) . . ?
N47 C44 C43 120.1(5) . . ?
C46 C45 C44 119.0(5) . . ?
C46 C45 H45 120.5 . . ?
C44 C45 H45 120.5 . . ?
N2 C46 C45 124.7(5) . . ?
N2 C46 H46 117.6 . . ?
C45 C46 H46 117.6 . . ?
O48 C48 N47 122.7(5) . . ?
O48 C48 C49 119.8(5) . . ?
N47 C48 C49 117.5(5) . . ?
C50 C49 C58 118.8(5) . . ?
C50 C49 C48 115.7(5) . . ?
C58 C49 C48 125.2(5) . . ?
C49 C50 C51 121.9(5) . . ?
C49 C50 H50 119.1 . . ?
C51 C50 H50 119.1 . . ?
C50 C51 C56 119.6(5) . . ?
C50 C51 C52 120.7(5) . . ?
C56 C51 C52 119.5(5) . . ?
C53 C52 C51 120.8(5) . . ?
C53 C52 H52 119.6 . . ?
C51 C52 H52 119.6 . . ?
C52 C53 C54 119.3(5) . . ?
C52 C53 H53 120.3 . . ?
C54 C53 H53 120.3 . . ?
C55 C54 C53 121.9(5) . . ?
C55 C54 H54 119.1 . . ?
C53 C54 H54 119.1 . . ?
C54 C55 C56 120.6(5) . . ?
C54 C55 H55 119.7 . . ?
C56 C55 H55 119.7 . . ?
C51 C56 C55 118.0(5) . . ?
C51 C56 C57 119.1(5) . . ?
C55 C56 C57 122.9(5) . . ?
C58 C57 C56 119.2(5) . . ?
C58 C57 C37 119.2(4) . . ?
C56 C57 C37 121.3(4) . . ?
C57 C58 O59 119.2(5) . . ?
C57 C58 C49 121.4(5) . . ?
O59 C58 C49 119.3(5) . . ?
O59 C60 H60A 109.5 . . ?
O59 C60 H60B 109.5 . . ?
H60A C60 H60B 109.5 . . ?
O59 C60 H60C 109.5 . . ?
H60A C60 H60C 109.5 . . ?
H60B C60 H60C 109.5 . . ?
N4 C62 C63 123.5(5) . 2_445 ?
N4 C62 H62 118.2 . . ?
C63 C62 H62 118.2 2_445 . ?
C62 C63 C64 118.9(5) 2_455 . ?
C62 C63 H63 120.6 2_455 . ?
C64 C63 H63 120.6 . . ?
N67 C64 C65 123.0(5) . . ?
N67 C64 C63 119.9(5) . . ?
C65 C64 C63 117.0(5) . . ?
C66 C65 C64 119.1(5) . . ?
C66 C65 H65 120.5 . . ?
C64 C65 H65 120.5 . . ?
N4 C66 C65 123.7(5) 2_455 . ?
N4 C66 H66 118.1 2_455 . ?
C65 C66 H66 118.1 . . ?
O68 C68 N67 121.8(5) . . ?
O68 C68 C69 121.9(5) . . ?
N67 C68 C69 116.2(4) . . ?
C70 C69 C78 118.2(5) . . ?
C70 C69 C68 118.7(5) . . ?
C78 C69 C68 123.1(5) . . ?
C69 C70 C71 121.8(5) . . ?
C69 C70 H70 119.1 . . ?
C71 C70 H70 119.1 . . ?
C70 C71 C76 119.6(5) . . ?
C70 C71 C72 121.3(5) . . ?
C76 C71 C72 119.0(5) . . ?
C73 C72 C71 120.8(5) . . ?
C73 C72 H72 119.6 . . ?
C71 C72 H72 119.6 . . ?
C72 C73 C74 120.0(5) . . ?
C72 C73 H73 120.0 . . ?
C74 C73 H73 120.0 . . ?
C75 C74 C73 122.3(6) . . ?
C75 C74 H74 118.8 . . ?
C73 C74 H74 118.8 . . ?
C74 C75 C76 119.4(5) . . ?
C74 C75 H75 120.3 . . ?
C76 C75 H75 120.3 . . ?
C71 C76 C77 119.0(4) . . ?
C71 C76 C75 118.6(5) . . ?
C77 C76 C75 122.4(5) . . ?
C78 C77 C76 119.4(4) . . ?
C78 C77 C97 119.6(4) . . ?
C76 C77 C97 121.0(4) . . ?
C77 C78 O79 118.6(4) . . ?
C77 C78 C69 121.6(5) . . ?
O79 C78 C69 119.7(4) . . ?
O79 C80 H80A 109.5 . . ?
O79 C80 H80B 109.5 . . ?
H80A C80 H80B 109.5 . . ?
O79 C80 H80C 109.5 . . ?
H80A C80 H80C 109.5 . . ?
H80B C80 H80C 109.5 . . ?
N3 C82 C83 123.3(5) . . ?
N3 C82 H82 118.3 . . ?
C83 C82 H82 118.3 . . ?
C82 C83 C84 119.6(5) . . ?
C82 C83 H83 120.2 . . ?
C84 C83 H83 120.2 . . ?
C83 C84 N87 120.3(4) . . ?
C83 C84 C85 117.7(4) . . ?
N87 C84 C85 121.9(5) . . ?
C86 C85 C84 117.6(4) . . ?
C86 C85 H85 121.2 . . ?
C84 C85 H85 121.2 . . ?
N3 C86 C85 125.3(4) . . ?
N3 C86 H86 117.3 . . ?
C85 C86 H86 117.3 . . ?
O88 C88 N87 123.9(5) . . ?
O88 C88 C89 120.5(4) . . ?
N87 C88 C89 115.5(4) . . ?
C90 C89 C98 120.2(4) . . ?
C90 C89 C88 118.2(4) . . ?
C98 C89 C88 121.4(4) . . ?
C89 C90 C91 120.2(4) . . ?
C89 C90 H90 119.9 . . ?
C91 C90 H90 119.9 . . ?
C96 C91 C90 119.1(4) . . ?
C96 C91 C92 120.2(5) . . ?
C90 C91 C92 120.7(5) . . ?
C93 C92 C91 120.2(5) . . ?
C93 C92 H92 119.9 . . ?
C91 C92 H92 119.9 . . ?
C92 C93 C94 119.8(5) . . ?
C92 C93 H93 120.1 . . ?
C94 C93 H93 120.1 . . ?
C95 C94 C93 121.8(5) . . ?
C95 C94 H94 119.1 . . ?
C93 C94 H94 119.1 . . ?
C94 C95 C96 120.5(5) . . ?
C94 C95 H95 119.8 . . ?
C96 C95 H95 119.8 . . ?
C97 C96 C91 120.2(5) . . ?
C97 C96 C95 122.3(5) . . ?
C91 C96 C95 117.5(4) . . ?
C98 C97 C96 119.1(4) . . ?
C98 C97 C77 118.4(4) . . ?
C96 C97 C77 122.6(4) . . ?
O99 C98 C97 119.2(4) . . ?
O99 C98 C89 119.8(4) . . ?
C97 C98 C89 121.0(4) . . ?
O99 C100 H10A 109.5 . . ?
O99 C100 H10B 109.5 . . ?
H10A C100 H10B 109.5 . . ?
O99 C100 H10C 109.5 . . ?
H10A C100 H10C 109.5 . . ?
H10B C100 H10C 109.5 . . ?
C1 O1 P1 121.1(4) . . ?
C2 O2 P1 119.7(3) . . ?
C3 O3 P2 121.2(3) . . ?
C4 O4 P2 120.1(3) . . ?
C5 O5 P3 116.0(4) . . ?
C6 O6 P3 116.4(4) . . ?
C7 O7 P4 115.5(4) . . ?
C8 O8 P4 118.4(3) . . ?
C38 O39 C40 114.5(4) . . ?
C58 O59 C60 114.2(5) . . ?
C78 O79 C80 112.9(4) . . ?
C98 O99 C100 113.3(4) . . ?
O1 P1 O2 96.8(2) . . ?
O1 P1 S2 108.59(16) . . ?
O2 P1 S2 112.86(16) . . ?
O1 P1 S1 112.77(16) . . ?
O2 P1 S1 111.63(17) . . ?
S2 P1 S1 113.06(9) . . ?
O3 P2 O4 97.4(2) . . ?
O3 P2 S4 112.75(16) . . ?
O4 P2 S4 108.01(16) . . ?
O3 P2 S3 112.14(17) . . ?
O4 P2 S3 113.27(16) . . ?
S4 P2 S3 112.32(9) . . ?
O6 P3 O5 94.5(3) . . ?
O6 P3 S6 112.18(19) . . ?
O5 P3 S6 113.19(17) . . ?
O6 P3 S5 111.55(18) . . ?
O5 P3 S5 112.57(18) . . ?
S6 P3 S5 111.74(9) . . ?
O7 P4 O8 95.5(2) . . ?
O7 P4 S7 112.23(17) . . ?
O8 P4 S7 112.60(16) . . ?
O7 P4 S8 111.92(16) . . ?
O8 P4 S8 112.19(17) . . ?
S7 P4 S8 111.48(9) . . ?
P1 S1 Ni1 81.94(6) . . ?
P1 S2 Ni1 83.25(6) . . ?
P2 S3 Ni1 82.14(6) . . ?
P2 S4 Ni1 83.90(6) . . ?
P3 S5 Ni2 82.41(7) . . ?
P3 S6 Ni2 83.81(7) . . ?
P4 S7 Ni2 83.85(6) . . ?
P4 S8 Ni2 82.30(6) . . ?
N3 Ni1 N1 179.05(17) . . ?
N3 Ni1 S4 90.78(12) . . ?
N1 Ni1 S4 89.78(12) . . ?
N3 Ni1 S2 88.64(12) . . ?
N1 Ni1 S2 90.79(12) . . ?
S4 Ni1 S2 179.00(6) . . ?
N3 Ni1 S1 89.47(12) . . ?
N1 Ni1 S1 89.69(12) . . ?
S4 Ni1 S1 97.48(5) . . ?
S2 Ni1 S1 81.70(5) . . ?
N3 Ni1 S3 89.96(12) . . ?
N1 Ni1 S3 90.88(12) . . ?
S4 Ni1 S3 81.40(5) . . ?
S2 Ni1 S3 99.42(5) . . ?
S1 Ni1 S3 178.74(5) . . ?
N2 Ni2 N4 179.6(2) . . ?
N2 Ni2 S7 89.50(13) . . ?
N4 Ni2 S7 90.86(12) . . ?
N2 Ni2 S6 90.37(13) . . ?
N4 Ni2 S6 89.26(12) . . ?
S7 Ni2 S6 178.25(6) . . ?
N2 Ni2 S5 91.19(13) . . ?
N4 Ni2 S5 88.71(13) . . ?
S7 Ni2 S5 96.22(5) . . ?
S6 Ni2 S5 82.04(5) . . ?
N2 Ni2 S8 89.40(13) . . ?
N4 Ni2 S8 90.72(13) . . ?
S7 Ni2 S8 82.32(5) . . ?
S6 Ni2 S8 99.42(5) . . ?
S5 Ni2 S8 178.42(6) . . ?
C26 N1 C22 117.2(4) . . ?
C26 N1 Ni1 120.0(3) . . ?
C22 N1 Ni1 122.2(3) . . ?
C46 N2 C42 116.1(4) . . ?
C46 N2 Ni2 119.8(4) . . ?
C42 N2 Ni2 124.1(3) . . ?
C86 N3 C82 116.4(4) . . ?
C86 N3 Ni1 120.0(3) . . ?
C82 N3 Ni1 123.3(3) . . ?
C62 N4 C66 117.5(5) . 2_445 ?
C62 N4 Ni2 123.5(3) . . ?
C66 N4 Ni2 119.0(3) 2_445 . ?
C28 N27 C24 127.0(5) . . ?
C28 N27 H27 110(3) . . ?
C24 N27 H27 121(3) . . ?
C48 N47 C44 122.9(5) . . ?
C48 N47 H47 119(3) . . ?
C44 N47 H47 117(3) . . ?
C68 N67 C64 125.4(4) . . ?
C68 N67 H67 120(3) . . ?
C64 N67 H67 114(3) . . ?
C88 N87 C84 127.6(4) . . ?
C88 N87 H87 121(3) . . ?
C84 N87 H87 110(3) . . ?
H1W O1W H2W 101(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
N47 H47 O59 0.897(19) 2.17(4) 2.729(6) 120(4) .
N67 H67 O1W 0.898(19) 2.05(3) 2.895(6) 157(5) .
O1W H1W O99 0.853(19) 2.01(2) 2.856(5) 172(5) .
N27 H27 O1 0.90(2) 2.16(3) 3.002(6) 156(5) 1_655
N87 H87 O4 0.874(19) 2.15(2) 3.022(6) 172(5) 1_455
O1W H2W O6 0.855(19) 2.21(3) 2.960(6) 146(4) 2_454

_diffrn_measured_fraction_theta_max 0.992
_diffrn_reflns_theta_full        27.12
_diffrn_measured_fraction_theta_full 0.992
_refine_diff_density_max         0.748
_refine_diff_density_min         -0.362
_refine_diff_density_rms         0.084
_database_code_depnum_ccdc_archive 'CCDC 1002587'
#######################################################################
#
#                 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_2009skc0029p212121

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C42 H46 N4 Ni O8 P2 S4'
_chemical_formula_weight         983.72

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'
S S 0.1246 0.1234 '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           orthorhombic
_symmetry_space_group_name_H-M   P2(1)2(1)2(1)

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

_cell_length_a                   15.332(2)
_cell_length_b                   8.6055(10)
_cell_length_c                   34.795(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     4590.8(10)
_cell_formula_units_Z            4
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    78682
_cell_measurement_theta_min      2.91
_cell_measurement_theta_max      27.48

_exptl_crystal_description       lath
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.423
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2048
_exptl_absorpt_coefficient_mu    0.729
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8800
_exptl_absorpt_correction_T_max  0.9927
_exptl_absorpt_process_details   'SADABS 2007/2 (Sheldrick, G.M., 2007)'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Bruker-Nonius FR591 rotating anode'
_diffrn_radiation_monochromator  '10cm confocal mirrors'
_diffrn_measurement_device_type  
'Bruker-Nonius APEX II CCD camera on κ-goniostat'
_diffrn_measurement_method       'φ & ω scans'
_diffrn_detector_area_resol_mean '4096x4096pixels / 62x62mm'
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            26414
_diffrn_reflns_av_R_equivalents  0.1577
_diffrn_reflns_av_sigmaI/netI    0.1638
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_theta_min         2.95
_diffrn_reflns_theta_max         25.00
_reflns_number_total             7285
_reflns_number_gt                4710
_reflns_threshold_expression     >2σ(I)

_computing_data_collection       'COLLECT (Hooft, R.W.W., 1998)'
_computing_cell_refinement       
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)'
#Although determined using DirAx, the cell is refined in the HKL
#package during data reduction
_computing_data_reduction        
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)'
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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 > 2σ(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.

 ISOR restraint was used for the non-positive definite C25. DELU and SIMU
 were also used due to the poor data from the weakly diffracting crystal.

 The carbond and hydrogen atom Ueq(max)/Ueq(min) ratio is larger than
 expected due to the slight rotation of the methyl group C63 creating a
 larger ellipsoid. This could not be modelled as disordered.

 The diffrn_measured_fraction_theta_full value is lower than usual and
 the second WGHT parameter is higher than expected due to the small size
 and weakly diffracting nature of the crystals. Similarly the R values
 are higher than usual, however the gross connectivity of the structure 
 can be seen.
 

;

_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)+(0.0001P)²+95.4905P] where P=(Fo²+2Fc²)/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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.27(6)
_refine_ls_number_reflns         7285
_refine_ls_number_parameters     539
_refine_ls_number_restraints     517
_refine_ls_R_factor_all          0.2125
_refine_ls_R_factor_gt           0.1495
_refine_ls_wR_factor_ref         0.3147
_refine_ls_wR_factor_gt          0.2815
_refine_ls_goodness_of_fit_ref   1.162
_refine_ls_restrained_S_all      1.127
_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
C2 C 0.9382(12) -0.0013(18) 0.9014(5) 0.039(4) Uani 1 1 d U . .
H2 H 0.9634 -0.0997 0.8959 0.047 Uiso 1 1 calc R . .
C3 C 0.9788(12) 0.1239(18) 0.8853(5) 0.035(4) Uani 1 1 d U . .
H3 H 1.0318 0.1102 0.8716 0.042 Uiso 1 1 calc R . .
C4 C 0.9429(11) 0.2708(18) 0.8888(5) 0.032(4) Uani 1 1 d U . .
C5 C 0.8580(12) 0.267(2) 0.9108(5) 0.040(4) Uani 1 1 d U . .
H5 H 0.8237 0.3583 0.9135 0.048 Uiso 1 1 calc R . .
C6 C 0.8327(12) 0.1358(19) 0.9261(5) 0.037(4) Uani 1 1 d U . .
H6 H 0.7811 0.1407 0.9412 0.044 Uiso 1 1 calc R . .
C8 C 1.0470(12) 0.439(2) 0.8546(5) 0.038(4) Uani 1 1 d U . .
C9 C 1.0467(12) 0.594(2) 0.8364(5) 0.040(4) Uani 1 1 d U . .
C10 C 0.9723(12) 0.6487(19) 0.8187(5) 0.036(4) Uani 1 1 d U . .
H10 H 0.9231 0.5819 0.8173 0.043 Uiso 1 1 calc R . .
C11 C 0.9656(12) 0.796(2) 0.8027(5) 0.038(4) Uani 1 1 d U . .
C12 C 0.8882(12) 0.850(2) 0.7866(6) 0.052(5) Uani 1 1 d U . .
H12 H 0.8390 0.7832 0.7851 0.062 Uiso 1 1 calc R . .
C13 C 0.8827(14) 0.994(2) 0.7733(6) 0.054(5) Uani 1 1 d U . .
H13 H 0.8283 1.0308 0.7639 0.065 Uiso 1 1 calc R . .
C14 C 0.9578(14) 1.098(2) 0.7727(6) 0.051(5) Uani 1 1 d U . .
H14 H 0.9530 1.1994 0.7624 0.061 Uiso 1 1 calc R . .
C15 C 1.0350(13) 1.046(2) 0.7872(5) 0.041(4) Uani 1 1 d U . .
H15 H 1.0851 1.1103 0.7865 0.050 Uiso 1 1 calc R . .
C16 C 1.0401(12) 0.8957(18) 0.8032(5) 0.032(3) Uani 1 1 d U . .
C17 C 1.1196(12) 0.8308(19) 0.8179(5) 0.033(3) Uani 1 1 d U . .
C18 C 1.1228(11) 0.6899(19) 0.8359(5) 0.034(2) Uani 1 1 d U . .
C20 C 1.2584(12) 0.570(3) 0.8274(6) 0.050(4) Uani 1 1 d U . .
H20A H 1.2418 0.4619 0.8230 0.075 Uiso 1 1 calc R . .
H20B H 1.3173 0.5742 0.8383 0.075 Uiso 1 1 calc R . .
H20C H 1.2574 0.6271 0.8030 0.075 Uiso 1 1 calc R . .
C22 C 0.8623(12) 0.033(2) 1.0116(6) 0.043(4) Uani 1 1 d U . .
H22 H 0.9112 0.0465 0.9952 0.051 Uiso 1 1 calc R . .
C23 C 0.8551(12) 0.126(2) 1.0446(5) 0.044(4) Uani 1 1 d U . .
H23 H 0.8989 0.2008 1.0501 0.052 Uiso 1 1 calc R . .
C24 C 0.7854(12) 0.1106(19) 1.0690(5) 0.036(4) Uani 1 1 d U . .
C25 C 0.7233(11) -0.0039(17) 1.0576(4) 0.028(3) Uani 1 1 d U . .
H25 H 0.6737 -0.0203 1.0735 0.034 Uiso 1 1 calc R . .
C26 C 0.7316(11) -0.0918(19) 1.0248(5) 0.031(4) Uani 1 1 d U . .
H26 H 0.6874 -0.1639 1.0179 0.037 Uiso 1 1 calc R . .
C28 C 0.8321(13) 0.2810(19) 1.1207(5) 0.043(4) Uani 1 1 d U . .
C29 C 0.8019(13) 0.3782(19) 1.1534(5) 0.039(4) Uani 1 1 d U . .
C30 C 0.8490(12) 0.3659(18) 1.1855(5) 0.041(4) Uani 1 1 d U . .
H30 H 0.8996 0.3021 1.1852 0.049 Uiso 1 1 calc R . .
C31 C 1.3257(12) 1.052(2) 0.7782(5) 0.043(4) Uani 1 1 d U . .
C32 C 1.3678(15) 1.065(2) 0.7438(6) 0.059(5) Uani 1 1 d U . .
H32 H 1.4221 1.1177 0.7429 0.070 Uiso 1 1 calc R . .
C33 C 1.3348(16) 1.005(2) 0.7107(6) 0.058(5) Uani 1 1 d U . .
H33 H 1.3596 1.0291 0.6865 0.070 Uiso 1 1 calc R . .
C34 C 1.2638(15) 0.907(2) 0.7137(6) 0.053(5) Uani 1 1 d U . .
H34 H 1.2446 0.8532 0.6914 0.064 Uiso 1 1 calc R . .
C35 C 1.2209(13) 0.884(2) 0.7466(5) 0.046(4) Uani 1 1 d U . .
H35 H 1.1711 0.8185 0.7465 0.055 Uiso 1 1 calc R . .
C36 C 1.2463(13) 0.954(2) 0.7815(5) 0.038(4) Uani 1 1 d U . .
C37 C 1.2011(11) 0.936(2) 0.8157(5) 0.036(3) Uani 1 1 d U . .
C38 C 1.2243(12) 1.0190(19) 0.8485(5) 0.034(2) Uani 1 1 d U . .
C40 C 1.2080(12) 0.939(3) 0.9128(6) 0.050(4) Uani 1 1 d U . .
H40A H 1.2152 0.8281 0.9077 0.075 Uiso 1 1 calc R . .
H40B H 1.1664 0.9536 0.9339 0.075 Uiso 1 1 calc R . .
H40C H 1.2644 0.9843 0.9200 0.075 Uiso 1 1 calc R . .
C42 C 0.9321(12) -0.293(2) 1.0639(5) 0.041(3) Uani 1 1 d U . .
H42A H 0.9784 -0.2223 1.0545 0.049 Uiso 1 1 calc R . .
H42B H 0.8751 -0.2421 1.0595 0.049 Uiso 1 1 calc R . .
C43 C 0.9438(13) -0.319(3) 1.1044(5) 0.058(6) Uani 1 1 d U . .
H43A H 0.9548 -0.2198 1.1173 0.087 Uiso 1 1 calc R . .
H43B H 0.9936 -0.3887 1.1085 0.087 Uiso 1 1 calc R . .
H43C H 0.8911 -0.3668 1.1151 0.087 Uiso 1 1 calc R . .
C52 C 1.0474(12) -0.6492(19) 1.0023(6) 0.041(3) Uani 1 1 d U . .
H52A H 1.0840 -0.5560 0.9981 0.049 Uiso 1 1 calc R . .
H52B H 1.0493 -0.6754 1.0300 0.049 Uiso 1 1 calc R . .
C53 C 1.0800(13) -0.775(2) 0.9804(6) 0.057(5) Uani 1 1 d U . .
H53A H 1.0609 -0.7645 0.9537 0.085 Uiso 1 1 calc R . .
H53B H 1.0579 -0.8730 0.9910 0.085 Uiso 1 1 calc R . .
H53C H 1.1439 -0.7751 0.9814 0.085 Uiso 1 1 calc R . .
C62 C 0.6822(19) -0.039(2) 0.8404(6) 0.074(6) Uani 1 1 d U . .
H62A H 0.6690 0.0348 0.8613 0.089 Uiso 1 1 calc R . .
H62B H 0.7459 -0.0382 0.8357 0.089 Uiso 1 1 calc R . .
C63 C 0.636(2) 0.005(4) 0.8059(8) 0.113(11) Uani 1 1 d U . .
H63A H 0.6503 0.1126 0.7995 0.170 Uiso 1 1 calc R . .
H63B H 0.5734 -0.0054 0.8102 0.170 Uiso 1 1 calc R . .
H63C H 0.6540 -0.0634 0.7848 0.170 Uiso 1 1 calc R . .
C72 C 0.6224(15) -0.543(2) 0.9127(7) 0.061(6) Uani 1 1 d U . .
H72A H 0.6750 -0.5372 0.9291 0.073 Uiso 1 1 calc R . .
H72B H 0.5704 -0.5338 0.9295 0.073 Uiso 1 1 calc R . .
C73 C 0.6206(13) -0.686(2) 0.8935(7) 0.062(6) Uani 1 1 d U . .
H73A H 0.5729 -0.6865 0.8747 0.093 Uiso 1 1 calc R . .
H73B H 0.6115 -0.7701 0.9121 0.093 Uiso 1 1 calc R . .
H73C H 0.6762 -0.7024 0.8801 0.093 Uiso 1 1 calc R . .
N1 N 0.8695(10) -0.0033(17) 0.9233(4) 0.039(3) Uani 1 1 d U . .
N7 N 0.9723(9) 0.4034(16) 0.8734(5) 0.042(4) Uani 1 1 d U . .
H7 H 0.9363 0.4824 0.8760 0.050 Uiso 1 1 calc R . .
N21 N 0.8029(9) -0.0751(15) 1.0024(4) 0.036(3) Uani 1 1 d U . .
N27 N 0.7692(10) 0.2019(17) 1.1006(4) 0.045(4) Uani 1 1 d U . .
H62 H 0.7149 0.2100 1.1086 0.053 Uiso 1 1 calc R . .
O19 O 1.2001(8) 0.6382(13) 0.8528(3) 0.039(3) Uani 1 1 d U . .
O21 O 1.1072(8) 0.3448(13) 0.8537(3) 0.040(3) Uani 1 1 d U . .
O39 O 1.1765(8) 1.0134(13) 0.8798(3) 0.039(3) Uani 1 1 d U . .
O41 O 0.9355(8) -0.4367(13) 1.0425(4) 0.043(3) Uani 1 1 d U . .
O48 O 0.9097(9) 0.2645(16) 1.1147(4) 0.057(4) Uani 1 1 d U . .
O51 O 0.9553(9) -0.6162(13) 0.9904(4) 0.046(3) Uani 1 1 d U . .
O61 O 0.6541(9) -0.1964(15) 0.8514(4) 0.054(3) Uani 1 1 d U . .
O71 O 0.6232(9) -0.4144(13) 0.8847(4) 0.049(3) Uani 1 1 d U . .
P1 P 0.6858(4) -0.2709(6) 0.88925(15) 0.0501(13) Uani 1 1 d U . .
P2 P 0.9165(4) -0.4478(6) 0.99913(16) 0.0433(12) Uani 1 1 d U . .
S1 S 0.8125(4) -0.3287(5) 0.88681(15) 0.0500(13) Uani 1 1 d U . .
S2 S 0.6663(3) -0.1488(5) 0.93564(14) 0.0457(12) Uani 1 1 d U . .
S3 S 0.9756(3) -0.2804(6) 0.96840(15) 0.0474(12) Uani 1 1 d U . .
S4 S 0.7895(4) -0.4508(6) 0.98743(14) 0.0480(13) Uani 1 1 d U . .
Ni1 Ni 0.82254(17) -0.2008(2) 0.95160(7) 0.0403(6) Uani 1 1 d U . .


_geom_special_details            
;
 All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell s.u.'s are taken
 into account individually in the estimation of s.u.'s in distances, angles
 and torsion angles; correlations between s.u.'s in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell s.u.'s is used for estimating s.u.'s 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
C2 N1 1.30(2) . ?
C2 C3 1.37(2) . ?
C2 H2 0.9500 . ?
C3 C4 1.38(2) . ?
C3 H3 0.9500 . ?
C4 N7 1.34(2) . ?
C4 C5 1.51(2) . ?
C5 C6 1.31(2) . ?
C5 H5 0.9500 . ?
C6 N1 1.33(2) . ?
C6 H6 0.9500 . ?
C8 O21 1.23(2) . ?
C8 N7 1.35(2) . ?
C8 C9 1.48(2) . ?
C9 C10 1.38(2) . ?
C9 C18 1.43(2) . ?
C10 C11 1.39(2) . ?
C10 H10 0.9500 . ?
C11 C12 1.39(3) . ?
C11 C16 1.43(2) . ?
C12 C13 1.33(3) . ?
C12 H12 0.9500 . ?
C13 C14 1.45(3) . ?
C13 H13 0.9500 . ?
C14 C15 1.36(3) . ?
C14 H14 0.9500 . ?
C15 C16 1.41(2) . ?
C15 H15 0.9500 . ?
C16 C17 1.43(2) . ?
C17 C18 1.37(2) . ?
C17 C37 1.54(2) . ?
C18 O19 1.398(19) . ?
C20 O19 1.39(2) . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C22 N21 1.34(2) . ?
C22 C23 1.41(2) . ?
C22 H22 0.9500 . ?
C23 C24 1.37(2) . ?
C23 H23 0.9500 . ?
C24 N27 1.38(2) . ?
C24 C25 1.43(2) . ?
C25 C26 1.38(2) . ?
C25 H25 0.9500 . ?
C26 N21 1.35(2) . ?
C26 H26 0.9500 . ?
C28 O48 1.22(2) . ?
C28 N27 1.37(2) . ?
C28 C29 1.49(2) . ?
C29 C30 1.33(2) . ?
C29 C38 1.48(2) 3_467 ?
C30 C31 1.49(3) 3_467 ?
C30 H30 0.9500 . ?
C31 C32 1.36(3) . ?
C31 C36 1.48(3) . ?
C31 C30 1.49(3) 3_567 ?
C32 C33 1.36(3) . ?
C32 H32 0.9500 . ?
C33 C34 1.38(3) . ?
C33 H33 0.9500 . ?
C34 C35 1.33(3) . ?
C34 H34 0.9500 . ?
C35 C36 1.41(2) . ?
C35 H35 0.9500 . ?
C36 C37 1.38(2) . ?
C37 C38 1.39(2) . ?
C38 O39 1.31(2) . ?
C38 C29 1.48(2) 3_567 ?
C40 O39 1.40(2) . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C40 H40C 0.9800 . ?
C42 C43 1.44(2) . ?
C42 O41 1.44(2) . ?
C42 H42A 0.9900 . ?
C42 H42B 0.9900 . ?
C43 H43A 0.9800 . ?
C43 H43B 0.9800 . ?
C43 H43C 0.9800 . ?
C52 C53 1.42(2) . ?
C52 O51 1.50(2) . ?
C52 H52A 0.9900 . ?
C52 H52B 0.9900 . ?
C53 H53A 0.9800 . ?
C53 H53B 0.9800 . ?
C53 H53C 0.9800 . ?
C62 C63 1.44(3) . ?
C62 O61 1.47(2) . ?
C62 H62A 0.9900 . ?
C62 H62B 0.9900 . ?
C63 H63A 0.9800 . ?
C63 H63B 0.9800 . ?
C63 H63C 0.9800 . ?
C72 C73 1.40(3) . ?
C72 O71 1.47(2) . ?
C72 H72A 0.9900 . ?
C72 H72B 0.9900 . ?
C73 H73A 0.9800 . ?
C73 H73B 0.9800 . ?
C73 H73C 0.9800 . ?
N1 Ni1 2.092(15) . ?
N7 H7 0.8800 . ?
N21 Ni1 2.095(14) . ?
N27 H62 0.8800 . ?
O41 P2 1.539(13) . ?
O51 P2 1.596(13) . ?
O61 P1 1.544(14) . ?
O71 P1 1.573(13) . ?
P1 S2 1.949(7) . ?
P1 S1 2.007(8) . ?
P2 S4 1.990(8) . ?
P2 S3 2.009(7) . ?
S1 Ni1 2.514(6) . ?
S2 Ni1 2.499(6) . ?
S3 Ni1 2.513(6) . ?
S4 Ni1 2.538(6) . ?

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 C2 C3 128.3(16) . . ?
N1 C2 H2 115.8 . . ?
C3 C2 H2 115.8 . . ?
C2 C3 C4 120.3(17) . . ?
C2 C3 H3 119.9 . . ?
C4 C3 H3 119.9 . . ?
N7 C4 C3 127.6(16) . . ?
N7 C4 C5 120.7(14) . . ?
C3 C4 C5 111.6(15) . . ?
C6 C5 C4 118.7(17) . . ?
C6 C5 H5 120.6 . . ?
C4 C5 H5 120.6 . . ?
C5 C6 N1 128.5(17) . . ?
C5 C6 H6 115.7 . . ?
N1 C6 H6 115.7 . . ?
O21 C8 N7 120.0(17) . . ?
O21 C8 C9 125.9(18) . . ?
N7 C8 C9 114.1(16) . . ?
C10 C9 C18 118.3(16) . . ?
C10 C9 C8 120.0(17) . . ?
C18 C9 C8 121.7(17) . . ?
C9 C10 C11 123.4(17) . . ?
C9 C10 H10 118.3 . . ?
C11 C10 H10 118.3 . . ?
C10 C11 C12 122.0(18) . . ?
C10 C11 C16 119.1(16) . . ?
C12 C11 C16 118.9(16) . . ?
C13 C12 C11 120.5(19) . . ?
C13 C12 H12 119.7 . . ?
C11 C12 H12 119.7 . . ?
C12 C13 C14 121.8(19) . . ?
C12 C13 H13 119.1 . . ?
C14 C13 H13 119.1 . . ?
C15 C14 C13 118.8(17) . . ?
C15 C14 H14 120.6 . . ?
C13 C14 H14 120.6 . . ?
C14 C15 C16 119.7(18) . . ?
C14 C15 H15 120.1 . . ?
C16 C15 H15 120.1 . . ?
C15 C16 C11 120.2(17) . . ?
C15 C16 C17 123.1(17) . . ?
C11 C16 C17 116.6(14) . . ?
C18 C17 C16 122.7(16) . . ?
C18 C17 C37 121.0(16) . . ?
C16 C17 C37 116.2(14) . . ?
C17 C18 O19 120.5(16) . . ?
C17 C18 C9 119.3(16) . . ?
O19 C18 C9 120.3(14) . . ?
O19 C20 H20A 109.5 . . ?
O19 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
O19 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
N21 C22 C23 122.5(17) . . ?
N21 C22 H22 118.8 . . ?
C23 C22 H22 118.8 . . ?
C24 C23 C22 120.7(18) . . ?
C24 C23 H23 119.6 . . ?
C22 C23 H23 119.6 . . ?
C23 C24 N27 125.5(17) . . ?
C23 C24 C25 114.6(16) . . ?
N27 C24 C25 119.7(16) . . ?
C26 C25 C24 123.2(16) . . ?
C26 C25 H25 118.4 . . ?
C24 C25 H25 118.4 . . ?
N21 C26 C25 119.7(16) . . ?
N21 C26 H26 120.1 . . ?
C25 C26 H26 120.1 . . ?
O48 C28 N27 122.9(16) . . ?
O48 C28 C29 120.2(18) . . ?
N27 C28 C29 116.7(17) . . ?
C30 C29 C38 121.3(16) . 3_467 ?
C30 C29 C28 115.3(17) . . ?
C38 C29 C28 123.4(16) 3_467 . ?
C29 C30 C31 122.8(17) . 3_467 ?
C29 C30 H30 118.6 . . ?
C31 C30 H30 118.6 3_467 . ?
C32 C31 C36 120.2(18) . . ?
C32 C31 C30 126.3(18) . 3_567 ?
C36 C31 C30 113.4(16) . 3_567 ?
C33 C32 C31 122(2) . . ?
C33 C32 H32 118.8 . . ?
C31 C32 H32 118.8 . . ?
C32 C33 C34 118(2) . . ?
C32 C33 H33 121.2 . . ?
C34 C33 H33 121.2 . . ?
C35 C34 C33 123(2) . . ?
C35 C34 H34 118.6 . . ?
C33 C34 H34 118.6 . . ?
C34 C35 C36 123(2) . . ?
C34 C35 H35 118.7 . . ?
C36 C35 H35 118.7 . . ?
C37 C36 C35 123.4(17) . . ?
C37 C36 C31 122.9(17) . . ?
C35 C36 C31 113.6(17) . . ?
C36 C37 C38 121.1(17) . . ?
C36 C37 C17 121.0(16) . . ?
C38 C37 C17 117.8(15) . . ?
O39 C38 C37 121.3(16) . . ?
O39 C38 C29 120.3(15) . 3_567 ?
C37 C38 C29 118.3(17) . 3_567 ?
O39 C40 H40A 109.5 . . ?
O39 C40 H40B 109.5 . . ?
H40A C40 H40B 109.5 . . ?
O39 C40 H40C 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
C43 C42 O41 111.6(16) . . ?
C43 C42 H42A 109.3 . . ?
O41 C42 H42A 109.3 . . ?
C43 C42 H42B 109.3 . . ?
O41 C42 H42B 109.3 . . ?
H42A C42 H42B 108.0 . . ?
C42 C43 H43A 109.5 . . ?
C42 C43 H43B 109.5 . . ?
H43A C43 H43B 109.5 . . ?
C42 C43 H43C 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
C53 C52 O51 109.2(16) . . ?
C53 C52 H52A 109.8 . . ?
O51 C52 H52A 109.8 . . ?
C53 C52 H52B 109.8 . . ?
O51 C52 H52B 109.8 . . ?
H52A C52 H52B 108.3 . . ?
C52 C53 H53A 109.5 . . ?
C52 C53 H53B 109.5 . . ?
H53A C53 H53B 109.5 . . ?
C52 C53 H53C 109.5 . . ?
H53A C53 H53C 109.5 . . ?
H53B C53 H53C 109.5 . . ?
C63 C62 O61 108(2) . . ?
C63 C62 H62A 110.0 . . ?
O61 C62 H62A 110.0 . . ?
C63 C62 H62B 110.0 . . ?
O61 C62 H62B 110.0 . . ?
H62A C62 H62B 108.4 . . ?
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 . . ?
C73 C72 O71 110.2(18) . . ?
C73 C72 H72A 109.6 . . ?
O71 C72 H72A 109.6 . . ?
C73 C72 H72B 109.6 . . ?
O71 C72 H72B 109.6 . . ?
H72A C72 H72B 108.1 . . ?
C72 C73 H73A 109.5 . . ?
C72 C73 H73B 109.5 . . ?
H73A C73 H73B 109.5 . . ?
C72 C73 H73C 109.5 . . ?
H73A C73 H73C 109.5 . . ?
H73B C73 H73C 109.5 . . ?
C2 N1 C6 112.1(15) . . ?
C2 N1 Ni1 124.4(12) . . ?
C6 N1 Ni1 123.5(12) . . ?
C4 N7 C8 132.0(16) . . ?
C4 N7 H7 114.0 . . ?
C8 N7 H7 114.0 . . ?
C22 N21 C26 119.2(15) . . ?
C22 N21 Ni1 117.4(12) . . ?
C26 N21 Ni1 123.3(11) . . ?
C28 N27 C24 124.3(16) . . ?
C28 N27 H62 117.9 . . ?
C24 N27 H62 117.9 . . ?
C20 O19 C18 114.3(14) . . ?
C38 O39 C40 120.4(14) . . ?
C42 O41 P2 123.5(11) . . ?
C52 O51 P2 118.1(10) . . ?
C62 O61 P1 120.7(13) . . ?
C72 O71 P1 121.9(13) . . ?
O61 P1 O71 92.8(8) . . ?
O61 P1 S2 115.8(6) . . ?
O71 P1 S2 114.4(6) . . ?
O61 P1 S1 111.8(6) . . ?
O71 P1 S1 113.1(6) . . ?
S2 P1 S1 108.5(3) . . ?
O41 P2 O51 99.9(7) . . ?
O41 P2 S4 112.7(6) . . ?
O51 P2 S4 108.3(6) . . ?
O41 P2 S3 113.1(5) . . ?
O51 P2 S3 112.5(6) . . ?
S4 P2 S3 110.0(3) . . ?
P1 S1 Ni1 85.0(2) . . ?
P1 S2 Ni1 86.6(3) . . ?
P2 S3 Ni1 84.2(2) . . ?
P2 S4 Ni1 83.9(2) . . ?
N1 Ni1 N21 91.6(6) . . ?
N1 Ni1 S2 94.6(4) . . ?
N21 Ni1 S2 87.5(4) . . ?
N1 Ni1 S3 90.5(4) . . ?
N21 Ni1 S3 94.5(4) . . ?
S2 Ni1 S3 174.43(19) . . ?
N1 Ni1 S1 87.4(4) . . ?
N21 Ni1 S1 167.0(4) . . ?
S2 Ni1 S1 79.65(18) . . ?
S3 Ni1 S1 98.42(19) . . ?
N1 Ni1 S4 171.4(5) . . ?
N21 Ni1 S4 89.7(4) . . ?
S2 Ni1 S4 93.98(18) . . ?
S3 Ni1 S4 80.87(18) . . ?
S1 Ni1 S4 93.27(18) . . ?

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
N7 H7 S1 0.88 2.53 3.396(16) 169.4 1_565
N27 H62 O21 0.88 2.16 2.976(19) 153.5 3_457
N27 H62 O39 0.88 2.48 2.912(18) 110.5 3_467

_diffrn_measured_fraction_theta_max 0.941
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.941
_refine_diff_density_max         1.159
_refine_diff_density_min         -0.730
_refine_diff_density_rms         0.150
_database_code_depnum_ccdc_archive 'CCDC 1002588'
