# Supplementary Material (ESI) for Dalton Transactions
# This journal is © The Royal Society of Chemistry 2000
# CCDC Number: 186/1794


data_pkm5 
 
_audit_creation_method            SHELXL 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_formula_moiety          ? 
_chemical_formula_structural      ? 
_chemical_formula_analytical      ? 
_chemical_formula_sum 
 'C39 H36 F12 N8 Ni P2 S2' 
_chemical_formula_weight      1028.52 
_chemical_melting_point           ? 
_chemical_compound_source         ? 
 
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' 
 'F'  'F'   0.0171   0.0103 
 '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            Monoclinic 
_symmetry_space_group_name_H-M    C2/c
 
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 '-x, y, -z+1/2' 
 'x+1/2, y+1/2, z' 
 '-x+1/2, y+1/2, -z+1/2' 
 '-x, -y, -z' 
 'x, -y, z-1/2' 
 '-x+1/2, -y+1/2, -z' 
 'x+1/2, -y+1/2, z-1/2' 
 
_cell_length_a                    12.4137(10) 
_cell_length_b                    26.0069(10) 
_cell_length_c                    13.3715(10) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  99.644(4) 
_cell_angle_gamma                 90.00 
_cell_volume                      4255.9(5) 
_cell_formula_units_Z             4 
_cell_measurement_temperature     200(2) 
_cell_measurement_reflns_used     7977
_cell_measurement_theta_min       3
_cell_measurement_theta_max      20 
 
_exptl_crystal_description        blocks 
_exptl_crystal_colour             'deep red'
_exptl_crystal_size_max           0.44
_exptl_crystal_size_mid           0.4
_exptl_crystal_size_min           0.4
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.605 
_exptl_crystal_density_method     ? 
_exptl_crystal_F_000              2092 
_exptl_absorpt_coefficient_mu     0.724 
_exptl_absorpt_correction_type    psi-scan
_exptl_absorpt_correction_T_min   0.76
_exptl_absorpt_correction_T_max   0.89
 
_exptl_special_details 
; 
 ? 
; 
 
_diffrn_ambient_temperature       200(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        ? 
_diffrn_measurement_method        ? 
_diffrn_standards_number          ? 
_diffrn_standards_interval_count  ? 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         ? 
_diffrn_reflns_number             12791 
_diffrn_reflns_av_R_equivalents   0.0276 
_diffrn_reflns_av_sigmaI/netI     0.0396 
_diffrn_reflns_limit_h_min        -11 
_diffrn_reflns_limit_h_max        16 
_diffrn_reflns_limit_k_min        -34 
_diffrn_reflns_limit_k_max        33 
_diffrn_reflns_limit_l_min        -15 
_diffrn_reflns_limit_l_max        17 
_diffrn_reflns_theta_min          1.57 
_diffrn_reflns_theta_max          28.52 
_reflns_number_total              4992 
_reflns_number_observed           3700 
_reflns_observed_criterion        >2sigma(I) 
 
_computing_data_collection        ? 
_computing_cell_refinement        ? 
_computing_data_reduction         ? 
_computing_structure_solution     'SHELXS-96 (Sheldrick, 1990)' 
_computing_structure_refinement   'SHELXL-96 (Sheldrick, 1996)' 
_computing_molecular_graphics     ? 
_computing_publication_material   ? 
 
_refine_special_details 
; 
 Refinement of F^2^ against ALL reflections.  Weighted R-factors wR and all 
 goodnesses 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 observed criterion 
 of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0690P)^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     ? 
_refine_ls_extinction_method      none 
_refine_ls_extinction_coef        ? 
_refine_ls_number_reflns          4992 
_refine_ls_number_parameters      302 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.0603 
_refine_ls_R_factor_obs           0.0397 
_refine_ls_wR_factor_all          0.1134 
_refine_ls_wR_factor_obs          0.1036 
_refine_ls_goodness_of_fit_all    0.986 
_refine_ls_goodness_of_fit_obs    1.056 
_refine_ls_restrained_S_all       0.986 
_refine_ls_restrained_S_obs       1.056 
_refine_ls_shift/esd_max          0.029 
_refine_ls_shift/esd_mean         0.001 
 
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_thermal_displace_type 
 _atom_site_occupancy 
 _atom_site_calc_flag 
 _atom_site_refinement_flags 
 _atom_site_disorder_group 
Ni1 Ni 0.5000 0.344834(14) 0.2500 0.02623(12) Uani 1 d S . 
S1 S 0.44519(5) 0.55945(2) 0.39893(5) 0.04302(17) Uani 1 d . . 
N1 N 0.58582(15) 0.28937(6) 0.17877(13) 0.0301(4) Uani 1 d . . 
C2 C 0.68185(19) 0.26717(9) 0.21508(17) 0.0372(5) Uani 1 d . . 
H2A H 0.7186 0.2773 0.2802 0.045 Uiso 1 calc R . 
C3 C 0.7298(2) 0.23056(9) 0.16309(19) 0.0435(6) Uani 1 d . . 
H3A H 0.7981 0.2158 0.1916 0.052 Uiso 1 calc R . 
C4 C 0.6771(2) 0.21576(10) 0.0689(2) 0.0479(6) Uani 1 d . . 
H4A H 0.7081 0.1902 0.0316 0.057 Uiso 1 calc R . 
C5 C 0.5785(2) 0.23833(9) 0.02906(19) 0.0427(6) Uani 1 d . . 
H5A H 0.5410 0.2287 -0.0361 0.051 Uiso 1 calc R . 
C6 C 0.53522(18) 0.27524(8) 0.08552(16) 0.0303(5) Uani 1 d . . 
C7 C 0.43113(18) 0.30249(8) 0.04915(15) 0.0305(4) Uani 1 d . . 
N8 N 0.40746(14) 0.33919(6) 0.11253(12) 0.0274(4) Uani 1 d . . 
C9 C 0.31490(17) 0.36683(8) 0.09208(15) 0.0293(4) Uani 1 d . . 
C10 C 0.24000(19) 0.35789(8) 0.00497(16) 0.0353(5) Uani 1 d . . 
H10A H 0.1739 0.3769 -0.0089 0.042 Uiso 1 calc R . 
C11 C 0.2639(2) 0.32049(9) -0.06143(17) 0.0406(5) Uani 1 d . . 
H11A H 0.2138 0.3139 -0.1219 0.049 Uiso 1 calc R . 
C12 C 0.3598(2) 0.29260(9) -0.04083(17) 0.0385(5) Uani 1 d . . 
H12A H 0.3767 0.2673 -0.0870 0.046 Uiso 1 calc R . 
C13 C 0.30493(18) 0.40601(8) 0.17139(16) 0.0302(4) Uani 1 d . . 
N14 N 0.38246(14) 0.40256(6) 0.25526(12) 0.0302(4) Uani 1 d . . 
C15 C 0.38421(19) 0.43854(8) 0.32769(17) 0.0340(5) Uani 1 d . . 
H15A H 0.4379 0.4359 0.3871 0.041 Uiso 1 calc R . 
C16 C 0.31091(19) 0.47955(9) 0.31965(17) 0.0361(5) Uani 1 d . . 
C17 C 0.2310(2) 0.48156(9) 0.23457(18) 0.0410(6) Uani 1 d . . 
H17A H 0.1783 0.5084 0.2273 0.049 Uiso 1 calc R . 
C18 C 0.22751(19) 0.44446(9) 0.15971(19) 0.0399(5) Uani 1 d . . 
H18A H 0.1725 0.4455 0.1011 0.048 Uiso 1 calc R . 
C19 C 0.3244(2) 0.52029(9) 0.40086(19) 0.0421(6) Uani 1 d . . 
H19A H 0.3297 0.5036 0.4681 0.051 Uiso 1 calc R . 
H19B H 0.2590 0.5427 0.3910 0.051 Uiso 1 calc R . 
C20 C 0.4052(2) 0.59124(10) 0.27709(19) 0.0443(6) Uani 1 d . . 
H20A H 0.3831 0.5651 0.2238 0.053 Uiso 1 calc R . 
H20B H 0.3418 0.6139 0.2800 0.053 Uiso 1 calc R . 
C21 C 0.5000 0.62324(14) 0.2500 0.0495(9) Uani 1 d S . 
H21A H 0.4716 0.6457 0.1918 0.059 Uiso 0.5 calc PR . 
H21B H 0.5284 0.6457 0.3082 0.059 Uiso 0.5 calc PR . 
P1 P 0.5000 0.10572(4) 0.2500 0.0454(2) Uani 1 d S . 
F11 F 0.62559(13) 0.10512(7) 0.23911(15) 0.0731(5) Uani 1 d . . 
F12A F 0.4757(2) 0.06075(14) 0.1689(2) 0.1212(17) Uani 0.904(7) d P . 
F13A F 0.47624(17) 0.14672(12) 0.1647(2) 0.1153(17) Uani 0.904(7) d P . 
F12B F 0.4804(17) 0.0953(10) 0.1464(15) 0.062(7) Uiso 0.096(7) d P . 
F13B F 0.5000 0.1673(9) 0.2500 0.054(8) Uiso 0.096(7) d SP . 
F14B F 0.5000 0.0521(10) 0.2500 0.058(8) Uiso 0.096(7) d SP . 
P2 P 0.0000 0.33198(4) 0.2500 0.0439(2) Uani 1 d S . 
F21 F 0.07238(15) 0.33135(8) 0.16225(13) 0.0741(5) Uani 1 d . . 
F22 F -0.10745(14) 0.33164(7) 0.16653(12) 0.0641(5) Uani 1 d . . 
F23 F 0.0000 0.27063(9) 0.2500 0.0690(7) Uani 1 d S . 
F24 F 0.0000 0.39293(9) 0.2500 0.0742(7) Uani 1 d S . 
N001 N 0.7872(4) 0.10003(18) 0.0320(3) 0.1231(17) Uani 1 d . . 
C001 C 0.6996(5) 0.08183(18) 0.0046(3) 0.0964(16) Uani 1 d . . 
C002 C 0.5948(4) 0.0606(2) -0.0291(3) 0.1105(16) Uani 1 d . . 
H02A H 0.5557 0.0575 0.0285 0.166 Uiso 1 calc R . 
H02B H 0.6026 0.0266 -0.0584 0.166 Uiso 1 calc R . 
H02C H 0.5537 0.0831 -0.0806 0.166 Uiso 1 calc 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 0.0310(2) 0.02383(19) 0.02216(19) 0.000 -0.00062(15) 0.000 
S1 0.0464(4) 0.0405(3) 0.0406(3) -0.0071(2) 0.0026(3) -0.0009(3) 
N1 0.0342(10) 0.0264(8) 0.0285(9) -0.0007(7) 0.0018(8) -0.0003(7) 
C2 0.0389(13) 0.0386(12) 0.0321(12) 0.0006(9) 0.0003(10) 0.0036(10) 
C3 0.0405(13) 0.0405(13) 0.0498(15) 0.0025(11) 0.0082(12) 0.0104(11) 
C4 0.0521(16) 0.0423(14) 0.0515(16) -0.0107(11) 0.0153(13) 0.0070(12) 
C5 0.0475(14) 0.0437(14) 0.0364(12) -0.0118(10) 0.0052(11) -0.0011(11) 
C6 0.0354(12) 0.0270(10) 0.0284(11) -0.0012(8) 0.0053(9) -0.0042(9) 
C7 0.0350(11) 0.0283(11) 0.0272(10) 0.0000(8) 0.0028(9) -0.0044(9) 
N8 0.0322(9) 0.0259(9) 0.0230(8) 0.0010(6) 0.0010(7) -0.0029(7) 
C9 0.0325(11) 0.0271(10) 0.0273(10) 0.0048(8) 0.0022(9) -0.0033(9) 
C10 0.0356(12) 0.0347(12) 0.0326(11) 0.0030(9) -0.0030(9) -0.0029(10) 
C11 0.0417(13) 0.0453(14) 0.0297(11) -0.0026(10) -0.0088(10) -0.0072(11) 
C12 0.0475(14) 0.0363(12) 0.0296(11) -0.0074(9) -0.0001(10) -0.0050(10) 
C13 0.0319(11) 0.0273(10) 0.0295(10) 0.0022(8) -0.0001(9) -0.0013(9) 
N14 0.0338(10) 0.0290(9) 0.0266(9) 0.0002(7) 0.0012(7) 0.0017(7) 
C15 0.0395(12) 0.0311(11) 0.0302(11) -0.0041(9) 0.0026(9) 0.0012(9) 
C16 0.0392(12) 0.0312(11) 0.0389(12) -0.0036(9) 0.0098(10) 0.0004(9) 
C17 0.0403(13) 0.0346(12) 0.0473(14) -0.0010(10) 0.0050(11) 0.0100(10) 
C18 0.0350(12) 0.0399(13) 0.0416(13) -0.0001(10) -0.0029(10) 0.0037(10) 
C19 0.0485(14) 0.0362(12) 0.0430(13) -0.0071(10) 0.0114(11) 0.0017(11) 
C20 0.0438(14) 0.0436(14) 0.0453(14) 0.0020(11) 0.0063(11) 0.0040(11) 
C21 0.053(2) 0.0370(19) 0.059(2) 0.000 0.0123(19) 0.000 
P1 0.0358(5) 0.0457(5) 0.0526(6) 0.000 0.0011(4) 0.000 
F11 0.0420(9) 0.0743(12) 0.1036(14) 0.0055(10) 0.0134(9) 0.0045(8) 
F12A 0.111(2) 0.119(3) 0.144(3) -0.086(3) 0.052(2) -0.0507(19) 
F13A 0.0543(14) 0.143(3) 0.138(3) 0.097(2) -0.0144(14) -0.0082(14) 
P2 0.0486(5) 0.0480(5) 0.0343(5) 0.000 0.0044(4) 0.000 
F21 0.0689(12) 0.1052(14) 0.0521(10) -0.0160(9) 0.0215(9) -0.0158(10) 
F22 0.0589(10) 0.0757(11) 0.0519(9) 0.0051(8) -0.0073(8) -0.0024(8) 
F23 0.0719(17) 0.0505(14) 0.0789(17) 0.000 -0.0038(14) 0.000 
F24 0.104(2) 0.0495(13) 0.0622(15) 0.000 -0.0064(14) 0.000 
N001 0.128(4) 0.132(4) 0.102(3) -0.028(3) -0.001(3) 0.069(3) 
C001 0.140(4) 0.091(3) 0.058(2) 0.003(2) 0.016(3) 0.066(3) 
C002 0.120(4) 0.134(4) 0.080(3) 0.018(3) 0.022(3) 0.027(3) 
 
_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 N8 2.0031(17) 2_655 ? 
Ni1 N8 2.0032(17) . Y
Ni1 N14 2.1028(17) 2_655 ? 
Ni1 N14 2.1029(17) . Y 
Ni1 N1 2.1124(17) 2_655 ? 
Ni1 N1 2.1125(17) . Y
S1 C19 1.817(3) . Y 
S1 C20 1.820(2) . Y 
N1 C2 1.340(3) . ? 
N1 C6 1.350(3) . ? 
C2 C3 1.372(3) . ? 
C3 C4 1.373(3) . ? 
C4 C5 1.381(4) . ? 
C5 C6 1.384(3) . ? 
C6 C7 1.482(3) . ? 
C7 N8 1.341(3) . ? 
C7 C12 1.393(3) . ? 
N8 C9 1.344(3) . ? 
C9 C10 1.383(3) . ? 
C9 C13 1.491(3) . ? 
C10 C11 1.382(3) . ? 
C11 C12 1.382(3) . ? 
C13 N14 1.353(3) . ? 
C13 C18 1.377(3) . ? 
N14 C15 1.344(3) . ? 
C15 C16 1.394(3) . ? 
C16 C17 1.380(3) . ? 
C16 C19 1.506(3) . ? 
C17 C18 1.386(3) . ? 
C20 C21 1.533(3) . ? 
C21 C20 1.533(3) 2_655 ? 
P1 F14B 1.39(3) . ? 
P1 F12B 1.39(2) 2_655 ? 
P1 F12B 1.39(2) . ? 
P1 F13A 1.553(2) 2_655 ? 
P1 F13A 1.553(2) . ? 
P1 F12A 1.589(3) . ? 
P1 F12A 1.589(3) 2_655 ? 
P1 F11 1.5900(16) . ? 
P1 F11 1.5901(16) 2_655 ? 
P1 F13B 1.60(2) . ? 
F12A F12B 0.95(2) . ? 
F12A F14B 1.099(7) . ? 
F13A F13B 1.250(11) . ? 
F13A F12B 1.36(2) . ? 
F12B F14B 1.77(3) . ? 
F13B F13A 1.250(11) 2_655 ? 
F14B F12A 1.099(7) 2_655 ? 
F14B F12B 1.77(3) 2_655 ? 
P2 F24 1.585(3) . ? 
P2 F22 1.5893(16) 2 ? 
P2 F22 1.5894(16) . ? 
P2 F21 1.5930(16) 2 ? 
P2 F21 1.5930(16) . ? 
P2 F23 1.595(2) . ? 
N001 C001 1.187(7) . ? 
C001 C002 1.414(7) . ? 
 
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 
N8 Ni1 N8 171.60(10) 2_655 . Y 
N8 Ni1 N14 77.79(7) 2_655 2_655 ? 
N8 Ni1 N14 108.42(7) . 2_655 ? 
N8 Ni1 N14 108.42(7) 2_655 . Y 
N8 Ni1 N14 77.79(7) . . Y 
N14 Ni1 N14 88.90(10) 2_655 . Y 
N8 Ni1 N1 77.95(7) 2_655 2_655 ? 
N8 Ni1 N1 96.24(7) . 2_655 Y 
N14 Ni1 N1 155.19(7) 2_655 2_655 ? 
N14 Ni1 N1 93.85(7) . 2_655 Y 
N8 Ni1 N1 96.24(7) 2_655 . ? 
N8 Ni1 N1 77.95(7) . . Y 
N14 Ni1 N1 93.85(7) 2_655 . ? 
N14 Ni1 N1 155.19(7) . . Y 
N1 Ni1 N1 93.88(9) 2_655 . Y 
C19 S1 C20 99.53(12) . . ? 
C2 N1 C6 117.74(18) . . ? 
C2 N1 Ni1 128.02(15) . . ? 
C6 N1 Ni1 114.24(14) . . ? 
N1 C2 C3 123.4(2) . . ? 
C4 C3 C2 118.6(2) . . ? 
C3 C4 C5 119.3(2) . . ? 
C4 C5 C6 119.0(2) . . ? 
N1 C6 C5 122.0(2) . . ? 
N1 C6 C7 114.72(18) . . ? 
C5 C6 C7 123.3(2) . . ? 
N8 C7 C12 120.1(2) . . ? 
N8 C7 C6 113.83(18) . . ? 
C12 C7 C6 126.03(19) . . ? 
C7 N8 C9 121.49(18) . . ? 
C7 N8 Ni1 118.64(14) . . ? 
C9 N8 Ni1 119.13(13) . . ? 
N8 C9 C10 120.84(19) . . ? 
N8 C9 C13 113.01(18) . . ? 
C10 C9 C13 126.1(2) . . ? 
C11 C10 C9 118.2(2) . . ? 
C10 C11 C12 120.8(2) . . ? 
C11 C12 C7 118.5(2) . . ? 
N14 C13 C18 121.9(2) . . ? 
N14 C13 C9 114.33(18) . . ? 
C18 C13 C9 123.7(2) . . ? 
C15 N14 C13 118.32(18) . . ? 
C15 N14 Ni1 126.41(15) . . ? 
C13 N14 Ni1 114.89(13) . . ? 
N14 C15 C16 123.1(2) . . ? 
C17 C16 C15 117.5(2) . . ? 
C17 C16 C19 123.0(2) . . ? 
C15 C16 C19 119.4(2) . . ? 
C16 C17 C18 120.0(2) . . ? 
C13 C18 C17 119.1(2) . . ? 
C16 C19 S1 112.10(16) . . ? 
C21 C20 S1 110.69(15) . . ? 
C20 C21 C20 114.3(3) 2_655 . ? 
F14B P1 F12B 78.7(10) . 2_655 ? 
F14B P1 F12B 78.7(10) . . ? 
F12B P1 F12B 157(2) 2_655 . ? 
F14B P1 F13A 133.37(14) . 2_655 ? 
F12B P1 F13A 54.8(10) 2_655 2_655 ? 
F12B P1 F13A 147.6(11) . 2_655 ? 
F14B P1 F13A 133.36(14) . . ? 
F12B P1 F13A 147.6(11) 2_655 . ? 
F12B P1 F13A 54.8(10) . . ? 
F13A P1 F13A 93.3(3) 2_655 . ? 
F14B P1 F12A 42.60(16) . . ? 
F12B P1 F12A 121.1(11) 2_655 . ? 
F12B P1 F12A 36.5(9) . . ? 
F13A P1 F12A 175.9(2) 2_655 . ? 
F13A P1 F12A 90.76(19) . . ? 
F14B P1 F12A 42.60(16) . 2_655 ? 
F12B P1 F12A 36.5(9) 2_655 2_655 ? 
F12B P1 F12A 121.1(11) . 2_655 ? 
F13A P1 F12A 90.77(19) 2_655 2_655 ? 
F13A P1 F12A 175.9(2) . 2_655 ? 
F12A P1 F12A 85.2(3) . 2_655 ? 
F14B P1 F11 89.44(8) . . ? 
F12B P1 F11 94.5(9) 2_655 . ? 
F12B P1 F11 85.3(9) . . ? 
F13A P1 F11 90.31(11) 2_655 . ? 
F13A P1 F11 90.46(11) . . ? 
F12A P1 F11 90.42(13) . . ? 
F12A P1 F11 88.75(12) 2_655 . ? 
F14B P1 F11 89.43(8) . 2_655 ? 
F12B P1 F11 85.3(9) 2_655 2_655 ? 
F12B P1 F11 94.5(9) . 2_655 ? 
F13A P1 F11 90.47(11) 2_655 2_655 ? 
F13A P1 F11 90.31(11) . 2_655 ? 
F12A P1 F11 88.75(12) . 2_655 ? 
F12A P1 F11 90.42(13) 2_655 2_655 ? 
F11 P1 F11 178.87(16) . 2_655 ? 
F14B P1 F13B 180.000(2) . . ? 
F12B P1 F13B 101.3(10) 2_655 . ? 
F12B P1 F13B 101.3(10) . . ? 
F13A P1 F13B 46.63(14) 2_655 . ? 
F13A P1 F13B 46.64(14) . . ? 
F12A P1 F13B 137.40(16) . . ? 
F12A P1 F13B 137.40(16) 2_655 . ? 
F11 P1 F13B 90.56(8) . . ? 
F11 P1 F13B 90.57(8) 2_655 . ? 
F12B F12A F14B 119(2) . . ? 
F12B F12A P1 60.4(13) . . ? 
F14B F12A P1 59.2(14) . . ? 
F13B F13A F12B 125.1(13) . . ? 
F13B F13A P1 68.8(10) . . ? 
F12B F13A P1 56.6(8) . . ? 
F12A F12B F13A 150(2) . . ? 
F12A F12B P1 83.1(14) . . ? 
F13A F12B P1 68.6(11) . . ? 
F12A F12B F14B 33.0(11) . . ? 
F13A F12B F14B 119.2(14) . . ? 
P1 F12B F14B 50.7(9) . . ? 
F13A F13B F13A 129(2) 2_655 . ? 
F13A F13B P1 64.6(10) 2_655 . ? 
F13A F13B P1 64.6(10) . . ? 
F12A F14B F12A 156(3) 2_655 . ? 
F12A F14B P1 78.2(14) 2_655 . ? 
F12A F14B P1 78.2(14) . . ? 
F12A F14B F12B 128(2) 2_655 . ? 
F12A F14B F12B 28.1(11) . . ? 
P1 F14B F12B 50.6(9) . . ? 
F12A F14B F12B 28.1(11) 2_655 2_655 ? 
F12A F14B F12B 128(2) . 2_655 ? 
P1 F14B F12B 50.6(9) . 2_655 ? 
F12B F14B F12B 101.1(19) . 2_655 ? 
F24 P2 F22 90.32(7) . 2 ? 
F24 P2 F22 90.32(7) . . ? 
F22 P2 F22 179.36(15) 2 . ? 
F24 P2 F21 90.59(8) . 2 ? 
F22 P2 F21 89.61(9) 2 2 ? 
F22 P2 F21 90.38(9) . 2 ? 
F24 P2 F21 90.59(8) . . ? 
F22 P2 F21 90.38(9) 2 . ? 
F22 P2 F21 89.61(9) . . ? 
F21 P2 F21 178.83(16) 2 . ? 
F24 P2 F23 180.0 . . ? 
F22 P2 F23 89.68(7) 2 . ? 
F22 P2 F23 89.68(7) . . ? 
F21 P2 F23 89.41(8) 2 . ? 
F21 P2 F23 89.41(8) . . ? 
N001 C001 C002 179.3(5) . . ? 
 
_refine_diff_density_max    0.542 
_refine_diff_density_min   -0.358 
_refine_diff_density_rms    0.062 

 
data_pkb21 
 
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum 
 'C38.50 H35 F12 N7 Ni O0.25 P2 S2' 
_chemical_formula_weight          1012.51 
 
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' 
 'F'  'F'   0.0171   0.0103 
 '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' 
 'O'  'O'   0.0106   0.0060 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 
_symmetry_cell_setting            Orthorhombic 
_symmetry_space_group_name_H-M    Pna2(1)
 
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 '-x, -y, z+1/2' 
 'x+1/2, -y+1/2, z' 
 '-x+1/2, y+1/2, z+1/2' 
 
_cell_length_a                    26.8148(3) 
_cell_length_b                    11.2892(2) 
_cell_length_c                    14.9759(2) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  90.00 
_cell_angle_gamma                 90.00 
_cell_volume                      4533.47(11) 
_cell_formula_units_Z             4 
_cell_measurement_temperature     200(2) 
_cell_measurement_reflns_used     6422 
_cell_measurement_theta_min       3
_cell_measurement_theta_max       15 
 
_exptl_crystal_description        plates
_exptl_crystal_colour             golden-yellow
_exptl_crystal_size_max           0.36
_exptl_crystal_size_mid           0.36
_exptl_crystal_size_min           0.12
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.483 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              2060 
_exptl_absorpt_coefficient_mu     0.678 
_exptl_absorpt_correction_type    psi-scan
_exptl_absorpt_correction_T_min   0.67
_exptl_absorpt_correction_T_max   0.93
_exptl_absorpt_process_details    ? 
 
_exptl_special_details 
; 
 ? 
; 
 
_diffrn_ambient_temperature       200(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   ? 
_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             19958 
_diffrn_reflns_av_R_equivalents   0.0541 
_diffrn_reflns_av_sigmaI/netI     0.0658 
_diffrn_reflns_limit_h_min        -23 
_diffrn_reflns_limit_h_max        30 
_diffrn_reflns_limit_k_min        -12 
_diffrn_reflns_limit_k_max        12 
_diffrn_reflns_limit_l_min        -17 
_diffrn_reflns_limit_l_max        17 
_diffrn_reflns_theta_min          2.04 
_diffrn_reflns_theta_max          24.00 
_reflns_number_total              7019 
_reflns_number_gt                 3998 
_reflns_threshold_expression      >2sigma(I) 
 
_computing_data_collection        ? 
_computing_cell_refinement        ? 
_computing_data_reduction         ? 
_computing_structure_solution     'SHELXS-97 (Sheldrick, 1990)' 
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)' 
_computing_molecular_graphics     ? 
_computing_publication_material   ? 
 
_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^)+(0.0859P)^2^+1.9161P] where P=(Fo^2^+2Fc^2^)/3' 
_atom_sites_solution_primary      direct 
_atom_sites_solution_secondary    difmap 
_atom_sites_solution_hydrogens    geom 
_refine_ls_hydrogen_treatment     mixed 
_refine_ls_extinction_method      none 
_refine_ls_extinction_coef        ? 
_refine_ls_abs_structure_details 
 'Flack H D (1983), Acta Cryst. A39, 876-881' 
_refine_ls_abs_structure_Flack    0.49(4) 
_refine_ls_number_reflns          7019 
_refine_ls_number_parameters      607 
_refine_ls_number_restraints      3 
_refine_ls_R_factor_all           0.1267 
_refine_ls_R_factor_gt            0.0606 
_refine_ls_wR_factor_ref          0.1826 
_refine_ls_wR_factor_gt           0.1407 
_refine_ls_goodness_of_fit_ref    1.057 
_refine_ls_restrained_S_all       1.058 
_refine_ls_shift/su_max           0.741 
_refine_ls_shift/su_mean          0.139 
 
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 0.18295(2) -0.00051(17) 0.4857(2) 0.0418(2) Uani 1 1 d . . . 
S1 S 0.37441(19) -0.2727(5) 0.4845(4) 0.1085(19) Uani 1 1 d . . . 
S2 S 0.37457(19) 0.2730(5) 0.4903(4) 0.1048(18) Uani 1 1 d . . . 
N1 N 0.1286(3) 0.1239(8) 0.5263(8) 0.053(3) Uani 1 1 d . . . 
C2 C 0.1074(5) 0.1272(12) 0.6084(10) 0.069(4) Uani 1 1 d . . . 
H2A H 0.1165 0.0720 0.6534 0.083 Uiso 1 1 calc R . . 
C3 C 0.0698(5) 0.2193(14) 0.6256(13) 0.096(7) Uani 1 1 d . . . 
H3A H 0.0520 0.2190 0.6805 0.115 Uiso 1 1 calc R . . 
C4 C 0.0603(6) 0.3015(16) 0.5664(16) 0.101(7) Uani 1 1 d . . . 
H4A H 0.0395 0.3666 0.5816 0.121 Uiso 1 1 calc R . . 
C5 C 0.0812(5) 0.2934(12) 0.4797(12) 0.073(4) Uani 1 1 d . . . 
H5A H 0.0724 0.3485 0.4344 0.088 Uiso 1 1 calc R . . 
C6 C 0.1135(5) 0.2065(12) 0.4633(10) 0.060(4) Uani 1 1 d . . . 
C7 C 0.1413(5) 0.1937(12) 0.3803(10) 0.058(4) Uani 1 1 d . . . 
N8 N 0.1781(4) 0.1067(10) 0.3793(8) 0.054(3) Uani 1 1 d . . . 
C9 C 0.2036(4) 0.0856(11) 0.3105(9) 0.049(4) Uani 1 1 d . . . 
C10 C 0.1983(6) 0.1456(13) 0.2305(8) 0.069(5) Uani 1 1 d . . . 
H10A H 0.2179 0.1291 0.1792 0.083 Uiso 1 1 calc R . . 
C11 C 0.1625(7) 0.2299(16) 0.2322(12) 0.090(6) Uani 1 1 d . . . 
H11A H 0.1574 0.2734 0.1787 0.108 Uiso 1 1 calc R . . 
C12 C 0.1330(7) 0.2586(13) 0.3032(11) 0.080(5) Uani 1 1 d . . . 
H12A H 0.1083 0.3189 0.3000 0.096 Uiso 1 1 calc R . . 
C13 C 0.2417(5) -0.0129(10) 0.3235(9) 0.043(3) Uani 1 1 d . . . 
N14 N 0.2365(4) -0.0714(9) 0.3997(6) 0.048(3) Uani 1 1 d . . . 
C15 C 0.2671(5) -0.1672(12) 0.4167(10) 0.070(4) Uani 1 1 d . . . 
H15A H 0.2613 -0.2135 0.4686 0.084 Uiso 1 1 calc R . . 
C16 C 0.3060(6) -0.1979(16) 0.3605(12) 0.084(5) Uani 1 1 d . . . 
C17 C 0.3076(5) -0.1451(15) 0.2788(11) 0.083(5) Uani 1 1 d . . . 
H17A H 0.3295 -0.1774 0.2352 0.100 Uiso 1 1 calc R . . 
C18 C 0.2794(6) -0.0471(17) 0.2554(10) 0.085(5) Uani 1 1 d . . . 
H18A H 0.2837 -0.0056 0.2008 0.103 Uiso 1 1 calc R . . 
C19 C 0.3395(7) -0.2948(18) 0.3866(13) 0.121(7) Uani 1 1 d . . . 
H19A H 0.3630 -0.3096 0.3369 0.145 Uiso 1 1 calc R . . 
H19B H 0.3192 -0.3674 0.3944 0.145 Uiso 1 1 calc R . . 
C20 C 0.4192(6) -0.132(2) 0.4678(18) 0.218(15) Uani 1 1 d . . . 
H20A H 0.4478 -0.1400 0.5090 0.262 Uiso 1 1 calc R . . 
H20B H 0.4325 -0.1340 0.4061 0.262 Uiso 1 1 calc R . . 
C21 C 0.3937(4) -0.0065(17) 0.484(2) 0.124(4) Uani 1 1 d . . . 
H21A H 0.3726 0.0104 0.4313 0.149 Uiso 1 1 calc R . . 
H21B H 0.3708 -0.0155 0.5356 0.149 Uiso 1 1 calc R . . 
C22 C 0.4242(7) 0.1002(16) 0.5008(12) 0.139(7) Uani 1 1 d . . . 
H22A H 0.4572 0.0688 0.5186 0.167 Uiso 1 1 calc R . . 
H22B H 0.4291 0.1355 0.4409 0.167 Uiso 1 1 calc R . . 
C24 C 0.3365(7) 0.3070(15) 0.5894(13) 0.102(6) Uani 1 1 d . . . 
H24A H 0.3586 0.3277 0.6399 0.123 Uiso 1 1 calc R . . 
H24B H 0.3150 0.3763 0.5767 0.123 Uiso 1 1 calc R . . 
C23 C 0.4168(6) 0.1945(19) 0.5554(12) 0.156(8) Uani 1 1 d . . . 
H23A H 0.4479 0.2396 0.5656 0.187 Uiso 1 1 calc R . . 
H23B H 0.4022 0.1707 0.6134 0.187 Uiso 1 1 calc R . . 
C25 C 0.3038(6) 0.2016(16) 0.6157(10) 0.077(5) Uani 1 1 d . . . 
C26 C 0.2689(4) 0.1584(10) 0.5539(7) 0.043(3) Uani 1 1 d . . . 
H26A H 0.2676 0.1943 0.4966 0.051 Uiso 1 1 calc R . . 
N27 N 0.2389(3) 0.0736(9) 0.5705(7) 0.042(2) Uani 1 1 d . . . 
C28 C 0.2425(6) 0.0177(13) 0.6552(11) 0.064(4) Uani 1 1 d . . . 
C29 C 0.2765(5) 0.0464(15) 0.7100(10) 0.071(4) Uani 1 1 d . . . 
H29A H 0.2787 0.0058 0.7654 0.085 Uiso 1 1 calc R . . 
C30 C 0.3094(6) 0.1323(18) 0.6920(12) 0.108(6) Uani 1 1 d . . . 
H30A H 0.3366 0.1460 0.7313 0.129 Uiso 1 1 calc R . . 
C31 C 0.2093(4) -0.0809(13) 0.6642(8) 0.053(4) Uani 1 1 d . . . 
N32 N 0.1801(3) -0.1076(8) 0.5894(7) 0.038(2) Uani 1 1 d . . . 
C33 C 0.1470(5) -0.1902(13) 0.5932(9) 0.056(4) Uani 1 1 d . . . 
C34 C 0.1373(6) -0.2564(13) 0.6687(11) 0.082(5) Uani 1 1 d . . . 
H34A H 0.1125 -0.3165 0.6668 0.098 Uiso 1 1 calc R . . 
C35 C 0.1628(7) -0.2363(14) 0.7460(12) 0.085(5) Uani 1 1 d . . . 
H35A H 0.1561 -0.2804 0.7987 0.102 Uiso 1 1 calc R . . 
C36 C 0.1998(5) -0.1468(14) 0.7442(11) 0.076(5) Uani 1 1 d . . . 
H36A H 0.2185 -0.1303 0.7966 0.091 Uiso 1 1 calc R . . 
C37 C 0.1202(4) -0.2013(12) 0.5051(12) 0.062(4) Uani 1 1 d . . . 
N38 N 0.1284(4) -0.1219(9) 0.4441(8) 0.055(3) Uani 1 1 d . . . 
C39 C 0.1053(4) -0.1304(12) 0.3665(10) 0.067(4) Uani 1 1 d . . . 
H39A H 0.1125 -0.0715 0.3231 0.081 Uiso 1 1 calc R . . 
C40 C 0.0733(5) -0.2126(14) 0.3442(11) 0.083(5) Uani 1 1 d . . . 
H40A H 0.0598 -0.2150 0.2856 0.100 Uiso 1 1 calc R . . 
C41 C 0.0598(6) -0.2944(18) 0.4058(13) 0.102(6) Uani 1 1 d . . . 
H41A H 0.0339 -0.3496 0.3936 0.122 Uiso 1 1 calc R . . 
C42 C 0.0836(6) -0.2958(16) 0.4846(17) 0.104(7) Uani 1 1 d . . . 
H42A H 0.0772 -0.3567 0.5267 0.125 Uiso 1 1 calc R . . 
P1 P 0.21018(11) -0.5007(5) 0.4850(5) 0.0905(8) Uani 1 1 d . . . 
F11 F 0.2112(6) -0.6061(8) 0.5538(6) 0.169(5) Uani 1 1 d . A . 
F12 F 0.1971(4) -0.3942(11) 0.4256(7) 0.153(5) Uani 1 1 d . A . 
F13A F 0.2364(7) -0.5883(16) 0.4245(9) 0.155(8) Uani 0.709(10) 1 d P A 1 
F14A F 0.2210(6) -0.3930(11) 0.5519(9) 0.121(6) Uani 0.709(10) 1 d P A 1 
F15A F 0.2602(7) -0.4944(15) 0.5313(11) 0.175(8) Uani 0.709(10) 1 d P A 1 
F16A F 0.1565(7) -0.5227(13) 0.4401(12) 0.156(7) Uani 0.709(10) 1 d P A 1 
F13B F 0.1890(9) -0.5804(18) 0.4117(13) 0.055(6) Uiso 0.291(10) 1 d P A 2 
F14B F 0.1611(8) -0.442(2) 0.5515(15) 0.062(7) Uiso 0.291(10) 1 d P A 2 
F15B F 0.2632(8) -0.455(2) 0.4243(15) 0.071(6) Uiso 0.291(10) 1 d P A 2 
F16B F 0.1699(14) -0.506(3) 0.555(3) 0.109(13) Uiso 0.291(10) 1 d P A 2 
P2 P 0.4997(3) 0.0529(2) 0.2373(5) 0.0844(7) Uani 1 1 d . . . 
F21 F 0.4835(4) 0.0521(11) 0.1360(7) 0.127(4) Uani 1 1 d . B . 
F22 F 0.5195(4) 0.0580(10) 0.3373(7) 0.114(3) Uani 1 1 d . B . 
F23A F 0.5332(11) 0.1676(18) 0.2136(17) 0.208(14) Uani 0.70(3) 1 d P B 1 
F24A F 0.4761(12) -0.0709(19) 0.2628(12) 0.181(12) Uani 0.70(3) 1 d P B 1 
F25A F 0.4546(7) 0.123(2) 0.2643(12) 0.190(15) Uani 0.70(3) 1 d P B 1 
F26A F 0.5425(10) -0.030(3) 0.2102(15) 0.246(18) Uani 0.70(3) 1 d P B 1 
F23B F 0.4924(16) 0.188(4) 0.251(2) 0.110(13) Uiso 0.30(3) 1 d P B 2 
F24B F 0.5086(7) -0.0741(16) 0.2277(15) 0.038(7) Uiso 0.30(3) 1 d P B 2 
F25B F 0.4419(11) 0.008(3) 0.251(2) 0.085(10) Uiso 0.30(3) 1 d P B 2 
F26B F 0.5547(12) 0.073(3) 0.204(2) 0.081(10) Uiso 0.30(3) 1 d P B 2 
N011 N 0.4383(6) 0.5118(13) 0.2977(12) 0.133(6) Uani 1 1 d . . . 
C011 C 0.4607(7) 0.4541(16) 0.3289(13) 0.101(6) Uani 1 1 d . . . 
C012 C 0.4947(5) 0.4021(14) 0.3760(11) 0.110(5) Uani 1 1 d . . . 
H02A H 0.4862 0.3183 0.3832 0.165 Uiso 1 1 calc R . . 
H02B H 0.4968 0.4398 0.4348 0.165 Uiso 1 1 calc R . . 
H02C H 0.5270 0.4089 0.3457 0.165 Uiso 1 1 calc R . . 
C021 C 0.4624(10) 0.532(3) 0.6339(19) 0.016(7) Uiso 0.25 1 d PD . . 
O021 O 0.4190(9) 0.505(2) 0.677(2) 0.063(8) Uiso 0.25 1 d PD . . 
C022 C 0.4958(11) 0.613(3) 0.578(2) 0.036(8) Uiso 0.25 1 d PD . . 
 
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 0.0381(4) 0.0454(4) 0.0419(4) -0.0030(4) 0.0005(11) 0.0022(9) 
S1 0.095(3) 0.133(5) 0.098(4) 0.035(4) 0.011(3) 0.058(3) 
S2 0.086(3) 0.142(5) 0.085(4) 0.037(4) -0.013(3) -0.040(3) 
N1 0.041(6) 0.048(7) 0.071(9) -0.013(6) 0.001(6) -0.005(5) 
C2 0.074(10) 0.075(11) 0.058(10) -0.005(8) -0.002(8) -0.002(8) 
C3 0.057(10) 0.102(14) 0.127(16) -0.072(12) 0.011(10) 0.037(9) 
C4 0.071(12) 0.085(13) 0.147(18) -0.039(14) -0.022(12) 0.041(9) 
C5 0.068(9) 0.071(9) 0.080(11) -0.012(9) -0.012(8) 0.042(7) 
C6 0.055(8) 0.060(8) 0.065(10) -0.017(7) -0.021(7) 0.023(7) 
C7 0.058(8) 0.044(8) 0.071(11) -0.009(8) -0.018(7) 0.013(6) 
N8 0.050(7) 0.064(8) 0.049(8) -0.005(6) -0.016(6) 0.003(6) 
C9 0.036(7) 0.043(8) 0.069(10) 0.002(7) -0.013(6) 0.001(5) 
C10 0.107(12) 0.073(11) 0.028(7) 0.025(7) -0.023(7) 0.000(9) 
C11 0.104(14) 0.096(14) 0.070(13) 0.030(10) -0.049(11) 0.004(11) 
C12 0.098(13) 0.066(10) 0.075(13) 0.018(9) -0.013(10) 0.018(9) 
C13 0.048(8) 0.060(9) 0.021(6) -0.009(6) 0.006(5) -0.007(6) 
N14 0.048(6) 0.058(7) 0.038(6) 0.010(6) 0.006(5) -0.010(5) 
C15 0.084(11) 0.049(8) 0.077(11) 0.004(7) -0.020(9) 0.019(7) 
C16 0.084(11) 0.103(14) 0.065(11) 0.003(10) 0.034(9) 0.021(9) 
C17 0.070(10) 0.130(13) 0.050(9) -0.005(9) -0.002(8) 0.050(9) 
C18 0.090(11) 0.132(14) 0.035(9) 0.012(9) 0.014(8) 0.001(11) 
C19 0.106(14) 0.177(18) 0.079(12) -0.007(14) 0.019(11) 0.083(14) 
C20 0.063(10) 0.37(4) 0.22(2) 0.16(3) 0.048(13) 0.110(17) 
C21 0.068(6) 0.137(9) 0.167(11) -0.047(8) -0.019(17) -0.040(12) 
C22 0.199(18) 0.133(13) 0.086(11) -0.018(10) -0.034(11) -0.073(12) 
C24 0.116(14) 0.100(12) 0.091(13) 0.008(11) -0.027(11) -0.061(11) 
C23 0.072(9) 0.27(2) 0.127(13) -0.018(15) -0.041(9) -0.018(11) 
C25 0.075(10) 0.105(13) 0.052(9) -0.015(9) 0.007(8) -0.055(9) 
C26 0.037(6) 0.061(8) 0.030(6) 0.002(6) -0.019(5) -0.003(6) 
N27 0.037(5) 0.044(6) 0.044(7) -0.015(5) 0.001(5) -0.005(5) 
C28 0.062(10) 0.078(11) 0.052(10) 0.011(8) 0.003(8) -0.003(8) 
C29 0.048(8) 0.116(12) 0.048(9) 0.015(8) -0.014(7) -0.032(9) 
C30 0.106(14) 0.155(17) 0.062(11) 0.009(12) -0.051(10) -0.014(12) 
C31 0.056(8) 0.069(10) 0.033(7) 0.002(7) 0.004(6) 0.012(7) 
N32 0.037(6) 0.032(6) 0.047(7) -0.002(5) 0.008(5) -0.005(4) 
C33 0.048(8) 0.071(9) 0.049(9) 0.005(7) 0.026(6) 0.004(7) 
C34 0.100(12) 0.074(11) 0.071(13) -0.018(9) 0.043(10) -0.033(9) 
C35 0.119(15) 0.064(11) 0.071(12) 0.017(9) 0.022(11) -0.008(10) 
C36 0.065(10) 0.085(12) 0.078(12) -0.008(10) 0.000(8) 0.010(8) 
C37 0.030(6) 0.053(8) 0.102(13) -0.018(8) 0.031(7) -0.009(5) 
N38 0.046(7) 0.065(8) 0.054(8) -0.014(7) 0.016(6) -0.014(6) 
C39 0.036(8) 0.082(11) 0.084(12) -0.041(9) -0.003(8) -0.021(7) 
C40 0.071(10) 0.110(13) 0.069(10) -0.001(10) 0.008(8) 0.003(9) 
C41 0.094(14) 0.130(16) 0.082(13) -0.049(13) 0.000(11) -0.046(12) 
C42 0.086(12) 0.085(12) 0.141(18) -0.023(13) 0.066(12) -0.011(9) 
P1 0.155(2) 0.0695(13) 0.0469(11) -0.0032(12) -0.017(4) 0.005(4) 
F11 0.338(15) 0.102(7) 0.067(5) 0.026(5) 0.063(7) 0.103(8) 
F12 0.155(8) 0.178(11) 0.128(8) 0.053(7) 0.034(6) 0.054(8) 
F13A 0.187(16) 0.216(19) 0.063(8) -0.013(10) 0.037(8) 0.114(14) 
F14A 0.202(16) 0.075(7) 0.086(9) -0.036(6) 0.033(9) 0.031(9) 
F15A 0.200(14) 0.160(15) 0.165(15) 0.035(14) -0.103(11) -0.083(12) 
F16A 0.178(15) 0.114(11) 0.175(16) 0.025(12) -0.103(12) 0.015(10) 
P2 0.0923(18) 0.0865(16) 0.0743(14) -0.006(4) -0.0330(12) 0.008(4) 
F21 0.140(9) 0.160(9) 0.082(7) 0.021(7) -0.066(6) -0.035(7) 
F22 0.141(9) 0.102(7) 0.099(8) -0.015(6) -0.036(7) -0.013(6) 
F23A 0.27(3) 0.121(17) 0.24(2) 0.108(14) -0.10(2) -0.09(2) 
F24A 0.29(3) 0.170(13) 0.084(11) 0.035(10) -0.027(15) -0.128(18) 
F25A 0.129(15) 0.30(3) 0.141(13) -0.038(16) -0.071(11) 0.17(2) 
F26A 0.19(3) 0.41(4) 0.141(17) 0.09(2) 0.043(16) 0.18(3) 
N011 0.096(11) 0.162(14) 0.141(13) -0.008(9) 0.034(10) 0.042(9) 
C011 0.104(12) 0.087(11) 0.112(12) 0.009(9) -0.026(9) -0.009(8) 
C012 0.089(9) 0.120(11) 0.121(12) 0.030(9) -0.032(8) -0.027(7) 
 
_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 N32 1.969(10) . Y 
Ni1 N8 2.005(12) . Y 
Ni1 N14 2.089(10) . Y 
Ni1 N38 2.099(10) . Y 
Ni1 N1 2.114(10) . Y 
Ni1 N27 2.137(9) . Y 
S1 C19 1.76(2) . Y 
S1 C20 2.01(2) . Y 
S2 C23 1.737(18) . Y 
S2 C24 1.84(2) . Y 
N1 C2 1.355(16) . ? 
N1 C6 1.386(16) . ? 
C2 C3 1.471(17) . ? 
C3 C4 1.31(2) . ? 
C4 C5 1.42(2) . ? 
C5 C6 1.331(16) . ? 
C6 C7 1.46(2) . ? 
C7 C12 1.386(18) . ? 
C7 N8 1.391(15) . ? 
N8 C9 1.260(16) . ? 
C9 C10 1.383(17) . ? 
C9 C13 1.523(17) . ? 
C10 C11 1.35(2) . ? 
C11 C12 1.37(2) . ? 
C13 N14 1.326(16) . ? 
C13 C18 1.486(19) . ? 
N14 C15 1.381(15) . ? 
C15 C16 1.385(17) . ? 
C16 C17 1.36(2) . ? 
C16 C19 1.47(2) . ? 
C17 C18 1.39(2) . ? 
C20 C21 1.59(3) . ? 
C21 C22 1.48(2) . ? 
C22 C23 1.36(2) . ? 
C24 C25 1.53(2) . ? 
C25 C26 1.403(15) . ? 
C25 C30 1.39(2) . ? 
C26 N27 1.275(13) . ? 
N27 C28 1.420(18) . ? 
C28 C29 1.268(19) . ? 
C28 C31 1.43(2) . ? 
C29 C30 1.34(2) . ? 
C31 N32 1.400(15) . ? 
C31 C36 1.433(19) . ? 
N32 C33 1.290(15) . ? 
C33 C34 1.380(18) . ? 
C33 C37 1.51(2) . ? 
C34 C35 1.36(2) . ? 
C35 C36 1.42(2) . ? 
C37 N38 1.299(17) . ? 
C37 C42 1.482(19) . ? 
N38 C39 1.320(17) . ? 
C39 C40 1.308(17) . ? 
C40 C41 1.36(2) . ? 
C41 C42 1.34(3) . ? 
P1 F13A 1.514(13) . ? 
P1 F13B 1.527(19) . ? 
P1 F15A 1.513(15) . ? 
P1 F12 1.536(11) . ? 
P1 F16A 1.608(16) . ? 
P1 F16B 1.50(4) . ? 
P1 F11 1.574(10) . ? 
P1 F14A 1.603(14) . ? 
P1 F15B 1.76(2) . ? 
P1 F14B 1.78(2) . ? 
F11 F16B 1.59(4) . ? 
F12 F16A 1.83(2) . ? 
F14A F15A 1.59(2) . ? 
F14B F16B 0.75(3) . ? 
P2 F24B 1.461(18) . ? 
P2 F25A 1.498(13) . ? 
P2 F26A 1.54(2) . ? 
P2 F23B 1.55(4) . ? 
P2 F26B 1.58(3) . ? 
P2 F21 1.577(11) . ? 
P2 F24A 1.581(18) . ? 
P2 F22 1.590(12) . ? 
P2 F23A 1.615(18) . ? 
P2 F25B 1.64(3) . ? 
N011 C011 1.003(17) . ? 
C011 C012 1.293(16) . ? 
C021 O021 1.370(19) . ? 
C021 C022 1.525(10) . ? 
 
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 
N32 Ni1 N8 174.0(2) . . Y 
N32 Ni1 N14 106.1(4) . . Y 
N8 Ni1 N14 77.7(4) . . Y 
N32 Ni1 N38 78.9(4) . . Y 
N8 Ni1 N38 96.5(5) . . Y 
N14 Ni1 N38 92.6(4) . . Y 
N32 Ni1 N1 98.9(4) . . Y 
N8 Ni1 N1 77.4(4) . . Y 
N14 Ni1 N1 155.0(5) . . Y 
N38 Ni1 N1 92.22(18) . . Y 
N32 Ni1 N27 78.4(4) . . Y 
N8 Ni1 N27 106.4(4) . . Y 
N14 Ni1 N27 91.91(17) . . Y 
N38 Ni1 N27 157.2(5) . . Y 
N1 Ni1 N27 93.1(4) . . Y 
C19 S1 C20 109.1(10) . . Y 
C23 S2 C24 90.9(9) . . Y 
C2 N1 C6 118.5(12) . . ? 
C2 N1 Ni1 124.6(10) . . ? 
C6 N1 Ni1 116.9(9) . . ? 
N1 C2 C3 117.7(14) . . ? 
C4 C3 C2 121.1(16) . . ? 
C3 C4 C5 119.8(14) . . ? 
C6 C5 C4 118.3(15) . . ? 
C5 C6 N1 124.0(15) . . ? 
C5 C6 C7 124.3(15) . . ? 
N1 C6 C7 111.4(11) . . ? 
C12 C7 N8 118.7(14) . . ? 
C12 C7 C6 125.1(13) . . ? 
N8 C7 C6 116.2(13) . . ? 
C9 N8 C7 121.8(12) . . ? 
C9 N8 Ni1 120.0(9) . . ? 
C7 N8 Ni1 117.6(10) . . ? 
N8 C9 C10 124.1(13) . . ? 
N8 C9 C13 113.4(12) . . ? 
C10 C9 C13 122.5(13) . . ? 
C11 C10 C9 113.7(15) . . ? 
C12 C11 C10 126.4(16) . . ? 
C11 C12 C7 115.4(15) . . ? 
N14 C13 C18 122.1(12) . . ? 
N14 C13 C9 113.8(11) . . ? 
C18 C13 C9 123.9(12) . . ? 
C13 N14 C15 119.1(12) . . ? 
C13 N14 Ni1 114.3(8) . . ? 
C15 N14 Ni1 126.5(9) . . ? 
N14 C15 C16 122.1(14) . . ? 
C17 C16 C15 117.4(15) . . ? 
C17 C16 C19 123.2(15) . . ? 
C15 C16 C19 119.0(15) . . ? 
C16 C17 C18 124.0(15) . . ? 
C17 C18 C13 113.9(14) . . ? 
C16 C19 S1 116.2(14) . . ? 
C21 C20 S1 115.3(10) . . ? 
C22 C21 C20 120.9(13) . . ? 
C23 C22 C21 131(2) . . ? 
C25 C24 S2 111.3(12) . . ? 
C22 C23 S2 99.1(13) . . ? 
C26 C25 C30 114.7(13) . . ? 
C26 C25 C24 118.9(14) . . ? 
C30 C25 C24 125.9(15) . . ? 
N27 C26 C25 123.6(12) . . ? 
C26 N27 C28 117.8(11) . . ? 
C26 N27 Ni1 128.4(9) . . ? 
C28 N27 Ni1 113.8(8) . . ? 
C29 C28 N27 120.8(14) . . ? 
C29 C28 C31 125.8(15) . . ? 
N27 C28 C31 112.8(13) . . ? 
C28 C29 C30 122.0(15) . . ? 
C29 C30 C25 120.0(14) . . ? 
N32 C31 C36 117.3(12) . . ? 
N32 C31 C28 116.1(12) . . ? 
C36 C31 C28 126.3(13) . . ? 
C33 N32 C31 120.3(11) . . ? 
C33 N32 Ni1 120.4(9) . . ? 
C31 N32 Ni1 118.6(8) . . ? 
N32 C33 C34 124.0(14) . . ? 
N32 C33 C37 110.4(11) . . ? 
C34 C33 C37 125.6(14) . . ? 
C33 C34 C35 120.7(15) . . ? 
C34 C35 C36 117.0(16) . . ? 
C35 C36 C31 120.7(15) . . ? 
N38 C37 C42 117.5(17) . . ? 
N38 C37 C33 118.6(11) . . ? 
C42 C37 C33 123.8(17) . . ? 
C37 N38 C39 119.4(12) . . ? 
C37 N38 Ni1 111.0(9) . . ? 
C39 N38 Ni1 129.5(10) . . ? 
C40 C39 N38 125.8(15) . . ? 
C39 C40 C41 119.0(15) . . ? 
C40 C41 C42 118.6(16) . . ? 
C41 C42 C37 119.4(19) . . ? 
F13A P1 F13B 50.1(9) . . ? 
F13A P1 F15A 83.9(11) . . ? 
F13B P1 F15A 133.4(13) . . ? 
F13A P1 F12 105.7(9) . . ? 
F13B P1 F12 87.7(10) . . ? 
F15A P1 F12 115.6(9) . . ? 
F13A P1 F16A 93.7(10) . . ? 
F13B P1 F16A 43.7(10) . . ? 
F15A P1 F16A 173.4(9) . . ? 
F12 P1 F16A 71.0(7) . . ? 
F13A P1 F16B 136.5(15) . . ? 
F13B P1 F16B 102.1(15) . . ? 
F15A P1 F16B 108.7(17) . . ? 
F12 P1 F16B 105.5(14) . . ? 
F16A P1 F16B 69.0(13) . . ? 
F13A P1 F11 83.7(7) . . ? 
F13B P1 F11 91.8(9) . . ? 
F15A P1 F11 73.7(8) . . ? 
F12 P1 F11 167.0(6) . . ? 
F16A P1 F11 99.9(9) . . ? 
F16B P1 F11 62.0(14) . . ? 
F13A P1 F14A 141.8(10) . . ? 
F13B P1 F14A 164.4(12) . . ? 
F15A P1 F14A 61.1(9) . . ? 
F12 P1 F14A 79.0(7) . . ? 
F16A P1 F14A 122.7(10) . . ? 
F16B P1 F14A 73.9(14) . . ? 
F11 P1 F14A 99.3(8) . . ? 
F13A P1 F15B 60.5(11) . . ? 
F13B P1 F15B 95.8(11) . . ? 
F15A P1 F15B 60.5(8) . . ? 
F12 P1 F15B 70.1(9) . . ? 
F16A P1 F15B 123.5(11) . . ? 
F16B P1 F15B 161.4(15) . . ? 
F11 P1 F15B 122.9(11) . . ? 
F14A P1 F15B 87.5(10) . . ? 
F13A P1 F14B 157.2(12) . . ? 
F13B P1 F14B 110.3(14) . . ? 
F15A P1 F14B 112.4(11) . . ? 
F12 P1 F14B 82.2(9) . . ? 
F16A P1 F14B 68.2(10) . . ? 
F16B P1 F14B 24.8(13) . . ? 
F11 P1 F14B 85.8(9) . . ? 
F14A P1 F14B 60.1(9) . . ? 
F15B P1 F14B 141.1(13) . . ? 
P1 F11 F16B 56.9(15) . . ? 
P1 F12 F16A 56.3(6) . . ? 
P1 F14A F15A 56.7(6) . . ? 
P1 F15A F14A 62.3(10) . . ? 
P1 F16A F12 52.7(6) . . ? 
F16B F14B P1 57(4) . . ? 
F14B F16B P1 98(4) . . ? 
F14B F16B F11 153(5) . . ? 
P1 F16B F11 61.2(16) . . ? 
F24B P2 F25A 132.4(15) . . ? 
F24B P2 F26A 41.6(13) . . ? 
F25A P2 F26A 174.1(19) . . ? 
F24B P2 F23B 176.9(19) . . ? 
F25A P2 F23B 49.2(12) . . ? 
F26A P2 F23B 137(2) . . ? 
F24B P2 F26B 87.5(14) . . ? 
F25A P2 F26B 140.0(16) . . ? 
F26A P2 F26B 45.9(17) . . ? 
F23B P2 F26B 91.1(16) . . ? 
F24B P2 F21 86.8(10) . . ? 
F25A P2 F21 92.4(8) . . ? 
F26A P2 F21 87.0(10) . . ? 
F23B P2 F21 95.8(15) . . ? 
F26B P2 F21 87.2(13) . . ? 
F24B P2 F24A 38.9(10) . . ? 
F25A P2 F24A 94.4(17) . . ? 
F26A P2 F24A 79.8(12) . . ? 
F23B P2 F24A 141.9(18) . . ? 
F26B P2 F24A 125.4(17) . . ? 
F21 P2 F24A 96.7(8) . . ? 
F24B P2 F22 94.2(10) . . ? 
F25A P2 F22 89.9(8) . . ? 
F26A P2 F22 91.1(11) . . ? 
F23B P2 F22 83.1(15) . . ? 
F26B P2 F22 88.9(14) . . ? 
F21 P2 F22 175.9(9) . . ? 
F24A P2 F22 86.5(7) . . ? 
F24B P2 F23A 132.3(16) . . ? 
F25A P2 F23A 95.0(13) . . ? 
F26A P2 F23A 90.8(18) . . ? 
F23B P2 F23A 46.5(13) . . ? 
F26B P2 F23A 45.0(14) . . ? 
F21 P2 F23A 86.9(9) . . ? 
F24A P2 F23A 169.7(17) . . ? 
F22 P2 F23A 89.5(9) . . ? 
F24B P2 F25B 82.3(12) . . ? 
F25A P2 F25B 50.7(12) . . ? 
F26A P2 F25B 123.4(16) . . ? 
F23B P2 F25B 99.6(17) . . ? 
F26B P2 F25B 165.6(17) . . ? 
F21 P2 F25B 82.2(13) . . ? 
F24A P2 F25B 47.2(12) . . ? 
F22 P2 F25B 101.9(13) . . ? 
F23A P2 F25B 143.1(15) . . ? 
N011 C011 C012 166(3) . . ? 
O021 C021 C022 154(3) . . ? 
 
_diffrn_measured_fraction_theta_max    0.998 
_diffrn_reflns_theta_full              24.00 
_diffrn_measured_fraction_theta_full   0.998 
_refine_diff_density_max    0.672 
_refine_diff_density_min   -0.312 
_refine_diff_density_rms    0.069