# Supplementary Material (ESI) for Dalton Transactions
# This journal is © The Royal Society of Chemistry 2000
# CCDC Number: 186/1768

 
data_first 
 
_audit_creation_method            SHELXL 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_formula_moiety          ? 
_chemical_formula_structural      ? 
_chemical_formula_analytical      ? 
_chemical_formula_sum             'C18 H31 Cl N4 Ni O4 S' 
_chemical_formula_weight          493.69 
_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' 
 'O'  'O'   0.0106   0.0060 
 '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' 
 'Cl'  'Cl'   0.1484   0.1585 
 '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, y+1/2, -z+1/2' 
 'x+1/2, -y+1/2, -z' 
 
_cell_length_a                    11.030(2) 
_cell_length_b                    12.477(2) 
_cell_length_c                    15.874(3) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  90.00 
_cell_angle_gamma                 90.00 
_cell_volume                      2184.5(6) 
_cell_formula_units_Z             4 
_cell_measurement_temperature     173(2) 
_cell_measurement_reflns_used     50 
_cell_measurement_theta_min       5.6
_cell_measurement_theta_max       11.5 
 
_exptl_crystal_description        prism 
_exptl_crystal_colour             green 
_exptl_crystal_size_max           0.42 
_exptl_crystal_size_mid           0.14 
_exptl_crystal_size_min           0.12 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.501 
_exptl_crystal_density_method     ? 
_exptl_crystal_F_000              1040 
_exptl_absorpt_coefficient_mu     1.138 
_exptl_absorpt_correction_type    Psi-scans 
_exptl_absorpt_correction_T_min   0.422
_exptl_absorpt_correction_T_max   0.600
 
_exptl_special_details 
; 
 ? 
; 
 
_diffrn_ambient_temperature       173(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        'Siemens P4' 
_diffrn_measurement_method        \w-scans
_diffrn_standards_number          3 
_diffrn_standards_interval_count  247 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         3.2
_diffrn_reflns_number             3498 
_diffrn_reflns_av_R_equivalents   0.1053 
_diffrn_reflns_av_sigmaI/netI     0.1138 
_diffrn_reflns_limit_h_min        -12 
_diffrn_reflns_limit_h_max        12 
_diffrn_reflns_limit_k_min        0 
_diffrn_reflns_limit_k_max        14 
_diffrn_reflns_limit_l_min        0 
_diffrn_reflns_limit_l_max        17 
_diffrn_reflns_theta_min          3.04 
_diffrn_reflns_theta_max          23.50 
_reflns_number_total              3220 
_reflns_number_observed           2364 
_reflns_observed_criterion        >2sigma(I) 
 
_computing_data_collection        'Siemens XSCANS'
_computing_cell_refinement        'Siemens XSCANS'
_computing_data_reduction         'Siemens XSCANS'
_computing_structure_solution     'SHELXS-86 (Sheldrick, 1990)' 
_computing_structure_refinement   'SHELXL-93 (Sheldrick, 1993)' 
_computing_molecular_graphics     'Siemens SHELXTL'
_computing_publication_material   'Siemens SHELXTL'
 
_refine_special_details 
; 
 Refinement on F^2^ for ALL reflections except for 24 with very negative F^2^ 
 or flagged by the user for potential systematic errors.  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. 
 The structure was refined as an enantiomeric twin with components 0.44(6), 
 0.56(6). 
; 
 
_refine_ls_structure_factor_coef  Fsqd  
_refine_ls_matrix_type            full 
_refine_ls_weighting_scheme 
 'calc w=1/[\s^2^(Fo^2^)+(0.1607P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' 
_atom_sites_solution_primary      Patterson
_atom_sites_solution_secondary    difmap 
_atom_sites_solution_hydrogens    geom 
_refine_ls_hydrogen_treatment     riding
_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    0.44(6) 
_refine_ls_number_reflns          3196 
_refine_ls_number_parameters      263 
_refine_ls_number_restraints      229 
_refine_ls_R_factor_all           0.1302 
_refine_ls_R_factor_obs           0.0865 
_refine_ls_wR_factor_all          0.3368 
_refine_ls_wR_factor_obs          0.2278 
_refine_ls_goodness_of_fit_all    1.075 
_refine_ls_goodness_of_fit_obs    1.117 
_refine_ls_restrained_S_all       1.392 
_refine_ls_restrained_S_obs       1.064 
_refine_ls_shift/esd_max          0.000 
_refine_ls_shift/esd_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_thermal_displace_type 
 _atom_site_occupancy 
 _atom_site_calc_flag 
 _atom_site_refinement_flags 
 _atom_site_disorder_group 
Ni Ni 0.67778(13) 0.51182(11) 0.10919(9) 0.0187(4) Uani 1 d . . 
S S 0.8151(3) 0.3780(3) 0.1659(2) 0.0327(9) Uani 1 d . . 
N1 N 0.5249(9) 0.4233(8) 0.0990(8) 0.024(2) Uani 1 d U . 
N2 N 0.7191(8) 0.5042(9) -0.0186(6) 0.024(2) Uani 1 d U . 
N3 N 0.5786(9) 0.6496(8) 0.1162(7) 0.024(2) Uani 1 d U . 
H3 H 0.6326(9) 0.6997(8) 0.1380(7) 0.029 Uiso 1 calc R . 
N4 N 0.8332(10) 0.5843(8) 0.1594(7) 0.026(2) Uani 1 d U . 
C1 C 0.5457(14) 0.3203(12) 0.0565(10) 0.035(3) Uani 1 d U . 
H1A H 0.4723(14) 0.2751(12) 0.0607(10) 0.042 Uiso 1 calc R . 
H1B H 0.6137(14) 0.2819(12) 0.0838(10) 0.042 Uiso 1 calc R . 
C2 C 0.5759(12) 0.3418(11) -0.0368(10) 0.033(3) Uani 1 d U . 
H2A H 0.5717(12) 0.2733(11) -0.0681(10) 0.039 Uiso 1 calc R . 
H2B H 0.5136(12) 0.3903(11) -0.0605(10) 0.039 Uiso 1 calc R . 
C3 C 0.7017(13) 0.3920(10) -0.0509(10) 0.034(3) Uani 1 d U . 
H3A H 0.7629(13) 0.3454(10) -0.0237(10) 0.041 Uiso 1 calc R . 
H3B H 0.7186(13) 0.3920(10) -0.1121(10) 0.041 Uiso 1 calc R . 
C4 C 0.6457(12) 0.5786(11) -0.0701(8) 0.027(3) Uani 1 d U . 
H4A H 0.5644(12) 0.5466(11) -0.0784(8) 0.033 Uiso 1 calc R . 
H4B H 0.6840(12) 0.5852(11) -0.1263(8) 0.033 Uiso 1 calc R . 
C5 C 0.6299(13) 0.6919(11) -0.0328(8) 0.031(3) Uani 1 d U . 
H5A H 0.7090(13) 0.7165(11) -0.0106(8) 0.037 Uiso 1 calc R . 
H5B H 0.6058(13) 0.7415(11) -0.0785(8) 0.037 Uiso 1 calc R . 
C6 C 0.5368(12) 0.6982(11) 0.0370(8) 0.025(3) Uani 1 d U . 
H6A H 0.5164(12) 0.7743(11) 0.0473(8) 0.030 Uiso 1 calc R . 
H6B H 0.4619(12) 0.6613(11) 0.0185(8) 0.030 Uiso 1 calc R . 
C7 C 0.4886(11) 0.6357(12) 0.1834(9) 0.026(3) Uani 1 d U . 
C8 C 0.3847(12) 0.5593(10) 0.1577(9) 0.026(3) Uani 1 d U . 
H8A H 0.3336(12) 0.5474(10) 0.2081(9) 0.032 Uiso 1 calc R . 
H8B H 0.3340(12) 0.5971(10) 0.1158(9) 0.032 Uiso 1 calc R . 
C9 C 0.4155(11) 0.4521(11) 0.1222(9) 0.029(3) Uani 1 d U . 
C10 C 0.8493(10) 0.5294(10) -0.0290(8) 0.027(3) Uani 1 d U . 
H10A H 0.8978(10) 0.4801(10) 0.0052(8) 0.032 Uiso 1 calc R . 
H10B H 0.8645(10) 0.6033(10) -0.0108(8) 0.032 Uiso 1 calc R . 
H10C H 0.8718(10) 0.5217(10) -0.0884(8) 0.032 Uiso 1 calc R . 
C11 C 0.5532(13) 0.5964(12) 0.2616(9) 0.030(3) Uani 1 d U . 
H11A H 0.6184(13) 0.6464(12) 0.2763(9) 0.036 Uiso 1 calc R . 
H11B H 0.5877(13) 0.5253(12) 0.2509(9) 0.036 Uiso 1 calc R . 
H11C H 0.4954(13) 0.5920(12) 0.3084(9) 0.036 Uiso 1 calc R . 
C12 C 0.4254(13) 0.7446(11) 0.2074(9) 0.030(3) Uani 1 d U . 
H12A H 0.3823(13) 0.7730(11) 0.1582(9) 0.036 Uiso 1 calc R . 
H12B H 0.4869(13) 0.7963(11) 0.2257(9) 0.036 Uiso 1 calc R . 
H12C H 0.3676(13) 0.7323(11) 0.2533(9) 0.036 Uiso 1 calc R . 
C13 C 0.3038(11) 0.3825(10) 0.1070(10) 0.034(3) Uani 1 d U . 
H13A H 0.3288(11) 0.3132(10) 0.0838(10) 0.041 Uiso 1 calc R . 
H13B H 0.2496(11) 0.4186(10) 0.0671(10) 0.041 Uiso 1 calc R . 
H13C H 0.2611(11) 0.3711(10) 0.1605(10) 0.041 Uiso 1 calc R . 
C14 C 0.8920(10) 0.4948(11) 0.1876(7) 0.025(3) Uani 1 d U . 
C15 C 0.9993(12) 0.5078(13) 0.2318(10) 0.039(3) Uani 1 d U . 
H15 H 1.0407(12) 0.4463(13) 0.2522(10) 0.047 Uiso 1 calc R . 
C16 C 1.0466(13) 0.6062(12) 0.2466(9) 0.030(3) Uani 1 d U . 
H16 H 1.1223(13) 0.6130(12) 0.2747(9) 0.036 Uiso 1 calc R . 
C17 C 0.9841(13) 0.6976(12) 0.2205(9) 0.030(3) Uani 1 d U . 
H17 H 1.0127(13) 0.7675(12) 0.2334(9) 0.036 Uiso 1 calc R . 
C18 C 0.8805(12) 0.6821(12) 0.1760(9) 0.029(3) Uani 1 d U . 
H18 H 0.8389(12) 0.7433(12) 0.1553(9) 0.035 Uiso 1 calc R . 
Cl Cl 0.7136(3) 0.9675(3) 0.0926(2) 0.0298(8) Uani 1 d U . 
O1 O 0.7033(11) 1.0778(7) 0.1162(8) 0.051(3) Uani 1 d U . 
O2 O 0.8374(10) 0.9418(10) 0.0733(11) 0.075(4) Uani 1 d U . 
O3 O 0.6731(12) 0.8997(9) 0.1583(8) 0.060(3) Uani 1 d U . 
O4 O 0.6435(12) 0.9481(9) 0.0181(8) 0.064(4) Uani 1 d U . 
 
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 
Ni 0.0181(7) 0.0114(8) 0.0267(8) 0.0019(7) -0.0012(7) 0.0005(6) 
S 0.027(2) 0.016(2) 0.055(2) 0.013(2) -0.009(2) -0.0013(15) 
N1 0.024(5) 0.010(5) 0.039(6) -0.002(5) 0.005(5) -0.009(4) 
N2 0.022(5) 0.022(5) 0.029(5) -0.007(5) 0.003(4) -0.003(4) 
N3 0.018(5) 0.028(6) 0.026(5) 0.001(5) -0.001(4) 0.001(4) 
N4 0.023(5) 0.018(5) 0.037(6) 0.006(5) -0.002(5) 0.001(4) 
C1 0.040(8) 0.023(7) 0.041(7) -0.020(6) 0.006(6) -0.017(6) 
C2 0.028(7) 0.017(7) 0.052(7) -0.006(6) 0.003(7) 0.003(5) 
C3 0.037(7) 0.016(5) 0.050(8) -0.014(6) 0.006(7) -0.007(5) 
C4 0.034(7) 0.028(6) 0.020(7) 0.004(5) 0.009(5) -0.001(5) 
C5 0.040(8) 0.030(6) 0.022(6) 0.005(6) 0.001(5) 0.005(6) 
C6 0.027(7) 0.019(7) 0.029(6) -0.003(5) -0.003(5) 0.007(5) 
C7 0.013(6) 0.031(7) 0.034(7) 0.000(6) 0.006(5) 0.007(5) 
C8 0.028(6) 0.021(6) 0.031(8) 0.010(5) 0.004(5) 0.005(4) 
C9 0.019(5) 0.031(6) 0.038(8) -0.001(6) 0.000(6) -0.002(5) 
C10 0.023(5) 0.019(6) 0.038(7) 0.000(6) 0.015(5) -0.006(5) 
C11 0.041(8) 0.027(8) 0.023(6) -0.004(6) 0.005(5) -0.002(6) 
C12 0.033(8) 0.021(6) 0.036(8) 0.004(6) 0.011(6) -0.001(5) 
C13 0.018(5) 0.027(6) 0.057(9) 0.001(7) 0.004(7) 0.001(5) 
C14 0.032(6) 0.025(6) 0.018(6) 0.011(6) -0.002(5) -0.002(5) 
C15 0.027(6) 0.029(6) 0.062(9) 0.019(8) -0.012(6) -0.006(6) 
C16 0.032(7) 0.029(7) 0.030(8) -0.002(6) 0.000(6) -0.002(5) 
C17 0.032(7) 0.029(6) 0.029(7) -0.002(6) -0.007(5) 0.003(6) 
C18 0.033(6) 0.027(6) 0.029(7) -0.005(6) 0.000(5) -0.004(5) 
Cl 0.026(2) 0.020(2) 0.043(2) -0.0045(15) 0.0064(14) -0.0001(12) 
O1 0.071(8) 0.014(5) 0.068(8) -0.019(5) 0.018(7) 0.004(5) 
O2 0.027(6) 0.059(8) 0.138(13) -0.011(8) 0.022(7) 0.013(5) 
O3 0.073(8) 0.042(7) 0.063(8) 0.009(6) 0.021(7) 0.007(7) 
O4 0.090(10) 0.041(7) 0.062(8) -0.003(6) -0.041(7) -0.024(6) 
 
_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 
Ni N1 2.022(9) . ? 
Ni N3 2.041(10) . ? 
Ni N2 2.081(10) . ? 
Ni N4 2.095(11) . ? 
Ni S 2.427(4) . ? 
S C14 1.721(14) . ? 
N1 C9 1.31(2) . ? 
N1 C1 1.47(2) . ? 
N2 C4 1.48(2) . ? 
N2 C10 1.479(14) . ? 
N2 C3 1.50(2) . ? 
N3 C7 1.47(2) . ? 
N3 C6 1.47(2) . ? 
N4 C18 1.35(2) . ? 
N4 C14 1.37(2) . ? 
C1 C2 1.54(2) . ? 
C2 C3 1.54(2) . ? 
C4 C5 1.54(2) . ? 
C5 C6 1.51(2) . ? 
C7 C11 1.51(2) . ? 
C7 C8 1.55(2) . ? 
C7 C12 1.57(2) . ? 
C8 C9 1.49(2) . ? 
C9 C13 1.53(2) . ? 
C14 C15 1.39(2) . ? 
C15 C16 1.35(2) . ? 
C16 C17 1.40(2) . ? 
C17 C18 1.36(2) . ? 
Cl O3 1.415(12) . ? 
Cl O1 1.431(9) . ? 
Cl O4 1.433(11) . ? 
Cl O2 1.435(11) . ? 
 
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 Ni N3 91.0(4) . . ? 
N1 Ni N2 94.6(4) . . ? 
N3 Ni N2 102.1(4) . . ? 
N1 Ni N4 161.5(5) . . ? 
N3 Ni N4 93.1(4) . . ? 
N2 Ni N4 102.2(4) . . ? 
N1 Ni S 100.0(3) . . ? 
N3 Ni S 153.4(3) . . ? 
N2 Ni S 101.1(3) . . ? 
N4 Ni S 69.2(3) . . ? 
C14 S Ni 78.4(4) . . ? 
C9 N1 C1 120.8(11) . . ? 
C9 N1 Ni 126.5(9) . . ? 
C1 N1 Ni 112.6(8) . . ? 
C4 N2 C10 109.6(10) . . ? 
C4 N2 C3 109.0(10) . . ? 
C10 N2 C3 106.5(10) . . ? 
C4 N2 Ni 113.0(8) . . ? 
C10 N2 Ni 108.2(8) . . ? 
C3 N2 Ni 110.3(8) . . ? 
C7 N3 C6 117.3(10) . . ? 
C7 N3 Ni 107.6(8) . . ? 
C6 N3 Ni 118.0(8) . . ? 
C18 N4 C14 119.4(11) . . ? 
C18 N4 Ni 141.1(9) . . ? 
C14 N4 Ni 99.2(8) . . ? 
N1 C1 C2 108.9(12) . . ? 
C3 C2 C1 113.9(12) . . ? 
N2 C3 C2 116.4(11) . . ? 
N2 C4 C5 115.1(11) . . ? 
C6 C5 C4 113.9(12) . . ? 
N3 C6 C5 113.1(10) . . ? 
N3 C7 C11 108.4(10) . . ? 
N3 C7 C8 112.5(11) . . ? 
C11 C7 C8 111.4(12) . . ? 
N3 C7 C12 112.0(11) . . ? 
C11 C7 C12 106.8(12) . . ? 
C8 C7 C12 105.6(10) . . ? 
C9 C8 C7 119.0(11) . . ? 
N1 C9 C8 124.2(11) . . ? 
N1 C9 C13 122.8(12) . . ? 
C8 C9 C13 112.7(10) . . ? 
N4 C14 C15 118.4(13) . . ? 
N4 C14 S 113.1(8) . . ? 
C15 C14 S 128.4(11) . . ? 
C16 C15 C14 121.6(14) . . ? 
C15 C16 C17 119.9(13) . . ? 
C18 C17 C16 117.0(14) . . ? 
N4 C18 C17 123.7(14) . . ? 
O3 Cl O1 110.9(7) . . ? 
O3 Cl O4 109.6(8) . . ? 
O1 Cl O4 109.6(8) . . ? 
O3 Cl O2 108.9(8) . . ? 
O1 Cl O2 110.3(7) . . ? 
O4 Cl O2 107.4(9) . . ? 
 
_refine_diff_density_max    0.705 
_refine_diff_density_min   -0.878 
_refine_diff_density_rms    0.145 
 
#===END
 
 
data_dsl05 
 
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum 
 'C17 H30 F6 N5 Ni P S' 
_chemical_formula_weight          540.20 
 
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    P2(1)/c
 
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 '-x, y+1/2, -z+1/2' 
 '-x, -y, -z' 
 'x, -y-1/2, z-1/2' 
 
_cell_length_a                    11.202(3) 
_cell_length_b                    24.771(7) 
_cell_length_c                    16.585(5) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  93.10(2) 
_cell_angle_gamma                 90.00 
_cell_volume                      4595(2) 
_cell_formula_units_Z             8 
_cell_measurement_temperature     291(2)
_cell_measurement_reflns_used     98
_cell_measurement_theta_min        4.565
_cell_measurement_theta_max       12.581
 
_exptl_crystal_description        prism
_exptl_crystal_colour             'deep green '
_exptl_crystal_size_max           0.58 
_exptl_crystal_size_mid           0.52 
_exptl_crystal_size_min           0.46 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.562 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              2240 
_exptl_absorpt_coefficient_mu     1.068 
_exptl_absorpt_correction_type    Psi-scans 
_exptl_absorpt_correction_T_min   0.5764 
_exptl_absorpt_correction_T_max   0.6394 
_exptl_absorpt_process_details    ? 
 
_exptl_special_details 
; 
 ? 
; 
 
_diffrn_ambient_temperature       291(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   'Siemens P4'
_diffrn_measurement_method        \w-scans 
_diffrn_detector_area_resol_mean  ? 
_diffrn_standards_number          3 
_diffrn_standards_interval_count  247 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         3.5 
_diffrn_reflns_number             11314 
_diffrn_reflns_av_R_equivalents   0.0906 
_diffrn_reflns_av_sigmaI/netI     0.1412 
_diffrn_reflns_limit_h_min        -13 
_diffrn_reflns_limit_h_max        4 
_diffrn_reflns_limit_k_min        0 
_diffrn_reflns_limit_k_max        29 
_diffrn_reflns_limit_l_min        -19 
_diffrn_reflns_limit_l_max        19 
_diffrn_reflns_theta_min          3.07 
_diffrn_reflns_theta_max          25.00 
_reflns_number_total              8055 
_reflns_number_gt                 3971 
_reflns_threshold_expression      >2sigma(I) 
 
_computing_data_collection      'Siemens XSCANS'
_computing_cell_refinement      'Siemens XSCANS'
_computing_data_reduction       'Siemens XSCANS'
_computing_structure_solution   'SHELXS-97 (Sheldrick, 1990)' 
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' 
_computing_molecular_graphics   'Siemens SHELXTL'
_computing_publication_material 'Siemens SHELXTL'
 
_refine_special_details 
; 
 Refinement of F^2^ against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F^2^, conventional R-factors R are based 
 on F, with F set to zero for negative F^2^. The threshold expression of 
 F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F^2^ are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger.
 Both hexafluorophosphate anions are disordered over two sites.
; 
 
_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^)+(0.1231P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' 
_atom_sites_solution_primary      Patterson
_atom_sites_solution_secondary    difmap 
_atom_sites_solution_hydrogens    geom 
_refine_ls_hydrogen_treatment     riding 
_refine_ls_extinction_method      none 
_refine_ls_extinction_coef        ? 
_refine_ls_number_reflns          8055 
_refine_ls_number_parameters      533 
_refine_ls_number_restraints      1287 
_refine_ls_R_factor_all           0.1452 
_refine_ls_R_factor_gt            0.0768 
_refine_ls_wR_factor_ref          0.2213 
_refine_ls_wR_factor_gt           0.1924 
_refine_ls_goodness_of_fit_ref    0.889 
_refine_ls_restrained_S_all       1.144 
_refine_ls_shift/su_max           0.002 
_refine_ls_shift/su_mean          0.000 
 
loop_ 
 _atom_site_label 
 _atom_site_type_symbol 
 _atom_site_fract_x 
 _atom_site_fract_y 
 _atom_site_fract_z 
 _atom_site_U_iso_or_equiv 
 _atom_site_adp_type 
 _atom_site_occupancy 
 _atom_site_symmetry_multiplicity 
 _atom_site_calc_flag 
 _atom_site_refinement_flags 
 _atom_site_disorder_assembly 
 _atom_site_disorder_group 
Ni1 Ni 1.25242(11) 0.49842(5) 1.24079(7) 0.0349(3) Uani 1 1 d . . . 
Ni1A Ni 0.77055(11) 0.67316(5) 0.52452(7) 0.0374(4) Uani 1 1 d . . . 
S1 S 1.1080(3) 0.48144(12) 1.34053(16) 0.0521(7) Uani 1 1 d . . . 
S1A S 0.6216(3) 0.60484(11) 0.54128(16) 0.0496(7) Uani 1 1 d . . . 
N1 N 1.0930(7) 0.4663(3) 1.1873(5) 0.042(2) Uani 1 1 d D . . 
C1 C 1.0291(9) 0.4600(4) 1.2539(6) 0.043(2) Uani 1 1 d D . . 
N2 N 0.9195(9) 0.4375(4) 1.2544(7) 0.067(3) Uani 1 1 d D . . 
C2 C 0.8750(12) 0.4212(5) 1.1815(10) 0.072(4) Uani 1 1 d D . . 
H2 H 0.7983 0.4068 1.1779 0.086 Uiso 1 1 calc R . . 
C3 C 0.9343(12) 0.4246(5) 1.1138(9) 0.075(4) Uani 1 1 d D . . 
H3 H 0.9015 0.4109 1.0654 0.090 Uiso 1 1 calc R . . 
C4 C 1.0425(11) 0.4483(5) 1.1176(7) 0.061(3) Uani 1 1 d D . . 
H4 H 1.0832 0.4521 1.0706 0.073 Uiso 1 1 calc R . . 
N3 N 1.4013(7) 0.5074(3) 1.3143(5) 0.0411(19) Uani 1 1 d . . . 
N4 N 1.3553(7) 0.4779(3) 1.1471(4) 0.0387(19) Uani 1 1 d . . . 
H4A H 1.3039 0.4638 1.1083 0.046 Uiso 1 1 calc R . . 
N5 N 1.2335(8) 0.5805(3) 1.2214(5) 0.051(2) Uani 1 1 d . . . 
C5 C 1.5021(9) 0.4854(4) 1.3078(6) 0.043(2) Uani 1 1 d . . . 
C6 C 1.5289(9) 0.4501(4) 1.2367(6) 0.047(3) Uani 1 1 d . . . 
H6A H 1.5873 0.4693 1.2066 0.057 Uiso 1 1 calc R . . 
H6B H 1.5687 0.4181 1.2588 0.057 Uiso 1 1 calc R . . 
C7 C 1.4350(9) 0.4309(4) 1.1769(6) 0.046(3) Uani 1 1 d . . . 
C8 C 1.4184(10) 0.5220(5) 1.1078(6) 0.054(3) Uani 1 1 d . . . 
H8A H 1.4476 0.5091 1.0572 0.065 Uiso 1 1 calc R . . 
H8B H 1.4869 0.5330 1.1422 0.065 Uiso 1 1 calc R . . 
C9 C 1.3375(11) 0.5702(5) 1.0913(7) 0.062(3) Uani 1 1 d . . . 
H9A H 1.3722 0.5930 1.0513 0.075 Uiso 1 1 calc R . . 
H9B H 1.2607 0.5576 1.0689 0.075 Uiso 1 1 calc R . . 
C10 C 1.3179(10) 0.6033(4) 1.1657(8) 0.062(3) Uani 1 1 d . . . 
H10A H 1.3945 0.6082 1.1949 0.075 Uiso 1 1 calc R . . 
H10B H 1.2893 0.6386 1.1487 0.075 Uiso 1 1 calc R . . 
C11 C 1.2437(11) 0.6092(5) 1.3020(7) 0.065(3) Uani 1 1 d . . . 
H11A H 1.2349 0.6477 1.2924 0.078 Uiso 1 1 calc R . . 
H11B H 1.1776 0.5979 1.3334 0.078 Uiso 1 1 calc R . . 
C12 C 1.3571(11) 0.6003(5) 1.3516(7) 0.068(4) Uani 1 1 d . . . 
H12A H 1.3583 0.6247 1.3973 0.081 Uiso 1 1 calc R . . 
H12B H 1.4234 0.6100 1.3192 0.081 Uiso 1 1 calc R . . 
C13 C 1.3783(10) 0.5439(5) 1.3831(6) 0.059(3) Uani 1 1 d . . . 
H13A H 1.4464 0.5436 1.4218 0.071 Uiso 1 1 calc R . . 
H13B H 1.3087 0.5315 1.4102 0.071 Uiso 1 1 calc R . . 
C14 C 1.6085(10) 0.4911(5) 1.3674(7) 0.063(3) Uani 1 1 d . . . 
H14A H 1.5875 0.5138 1.4113 0.076 Uiso 1 1 calc R . . 
H14B H 1.6740 0.5070 1.3409 0.076 Uiso 1 1 calc R . . 
H14C H 1.6315 0.4562 1.3878 0.076 Uiso 1 1 calc R . . 
C15 C 1.3528(11) 0.3904(4) 1.2126(7) 0.058(3) Uani 1 1 d . . . 
H15A H 1.2943 0.3787 1.1719 0.070 Uiso 1 1 calc R . . 
H15B H 1.3132 0.4068 1.2563 0.070 Uiso 1 1 calc R . . 
H15C H 1.3984 0.3599 1.2325 0.070 Uiso 1 1 calc R . . 
C16 C 1.4954(11) 0.4062(5) 1.1062(7) 0.073(4) Uani 1 1 d . . . 
H16A H 1.4357 0.3935 1.0670 0.088 Uiso 1 1 calc R . . 
H16B H 1.5447 0.3766 1.1248 0.088 Uiso 1 1 calc R . . 
H16C H 1.5441 0.4330 1.0819 0.088 Uiso 1 1 calc R . . 
C17 C 1.1100(10) 0.5904(4) 1.1874(8) 0.062(3) Uani 1 1 d . . . 
H17A H 1.0537 0.5754 1.2228 0.075 Uiso 1 1 calc R . . 
H17B H 1.0998 0.5736 1.1353 0.075 Uiso 1 1 calc R . . 
H17C H 1.0968 0.6286 1.1821 0.075 Uiso 1 1 calc R . . 
N1A N 0.6176(8) 0.7057(3) 0.5774(5) 0.049(2) Uani 1 1 d D . . 
C1A C 0.5529(9) 0.6596(4) 0.5823(5) 0.046(3) Uani 1 1 d D . . 
N2A N 0.4479(8) 0.6561(4) 0.6186(5) 0.054(2) Uani 1 1 d D . . 
C2A C 0.4100(11) 0.7008(6) 0.6500(8) 0.075(4) Uani 1 1 d D . . 
H2A H 0.3379 0.6997 0.6752 0.090 Uiso 1 1 calc R . . 
C3A C 0.4685(12) 0.7491(6) 0.6487(8) 0.076(4) Uani 1 1 d D . . 
H3A H 0.4390 0.7798 0.6730 0.091 Uiso 1 1 calc R . . 
C4A C 0.5725(11) 0.7499(5) 0.6096(8) 0.069(4) Uani 1 1 d D . . 
H4A1 H 0.6133 0.7824 0.6054 0.083 Uiso 1 1 calc R . . 
N3A N 0.9134(7) 0.6255(3) 0.5058(4) 0.0397(19) Uani 1 1 d . . . 
N4A N 0.8809(7) 0.7344(3) 0.5667(5) 0.043(2) Uani 1 1 d . . . 
H4A2 H 0.8326 0.7581 0.5913 0.052 Uiso 1 1 calc R . . 
N5A N 0.7455(8) 0.6932(4) 0.4044(5) 0.053(2) Uani 1 1 d . . . 
C5A C 1.0191(10) 0.6291(4) 0.5405(6) 0.043(2) Uani 1 1 d . . . 
C6A C 1.0516(9) 0.6725(4) 0.5993(6) 0.046(2) Uani 1 1 d . . . 
H6A1 H 1.1100 0.6951 0.5743 0.055 Uiso 1 1 calc R . . 
H6A2 H 1.0932 0.6551 0.6451 0.055 Uiso 1 1 calc R . . 
C7A C 0.9612(9) 0.7105(4) 0.6337(6) 0.046(3) Uani 1 1 d . . . 
C8A C 0.9420(10) 0.7664(4) 0.5065(7) 0.057(3) Uani 1 1 d . . . 
H8A1 H 1.0120 0.7468 0.4908 0.068 Uiso 1 1 calc R . . 
H8A2 H 0.9690 0.8001 0.5310 0.068 Uiso 1 1 calc R . . 
C9A C 0.8640(12) 0.7785(5) 0.4323(8) 0.071(4) Uani 1 1 d . . . 
H9A1 H 0.7884 0.7928 0.4486 0.085 Uiso 1 1 calc R . . 
H9A2 H 0.9021 0.8063 0.4014 0.085 Uiso 1 1 calc R . . 
C10A C 0.8400(12) 0.7307(5) 0.3791(7) 0.071(4) Uani 1 1 d . . . 
H10C H 0.8177 0.7436 0.3251 0.085 Uiso 1 1 calc R . . 
H10D H 0.9138 0.7105 0.3761 0.085 Uiso 1 1 calc R . . 
C11A C 0.7484(11) 0.6424(5) 0.3534(6) 0.064(3) Uani 1 1 d . . . 
H11C H 0.6804 0.6203 0.3659 0.076 Uiso 1 1 calc R . . 
H11D H 0.7376 0.6529 0.2971 0.076 Uiso 1 1 calc R . . 
C12A C 0.8595(11) 0.6079(5) 0.3628(7) 0.066(3) Uani 1 1 d . . . 
H12C H 0.9277 0.6297 0.3497 0.080 Uiso 1 1 calc R . . 
H12D H 0.8525 0.5789 0.3235 0.080 Uiso 1 1 calc R . . 
C13A C 0.8853(11) 0.5829(4) 0.4468(6) 0.057(3) Uani 1 1 d . . . 
H13C H 0.8160 0.5628 0.4625 0.068 Uiso 1 1 calc R . . 
H13D H 0.9521 0.5581 0.4451 0.068 Uiso 1 1 calc R . . 
C14A C 1.1198(9) 0.5909(5) 0.5264(7) 0.063(3) Uani 1 1 d . . . 
H14D H 1.0930 0.5638 0.4881 0.076 Uiso 1 1 calc R . . 
H14E H 1.1453 0.5739 0.5764 0.076 Uiso 1 1 calc R . . 
H14F H 1.1854 0.6105 0.5057 0.076 Uiso 1 1 calc R . . 
C15A C 1.0268(12) 0.7550(5) 0.6814(8) 0.073(4) Uani 1 1 d . . . 
H15A H 0.9697 0.7789 0.7036 0.088 Uiso 1 1 calc R . . 
H15B H 1.0762 0.7748 0.6463 0.088 Uiso 1 1 calc R . . 
H15C H 1.0760 0.7392 0.7244 0.088 Uiso 1 1 calc R . . 
C16A C 0.8803(10) 0.6795(4) 0.6887(6) 0.052(3) Uani 1 1 d . . . 
H16D H 0.8402 0.6511 0.6585 0.062 Uiso 1 1 calc R . . 
H16E H 0.8222 0.7037 0.7091 0.062 Uiso 1 1 calc R . . 
H16F H 0.9277 0.6642 0.7330 0.062 Uiso 1 1 calc R . . 
C17A C 0.6261(11) 0.7175(6) 0.3901(7) 0.072(4) Uani 1 1 d . . . 
H17D H 0.6211 0.7499 0.4216 0.086 Uiso 1 1 calc R . . 
H17E H 0.5662 0.6924 0.4056 0.086 Uiso 1 1 calc R . . 
H17F H 0.6132 0.7261 0.3339 0.086 Uiso 1 1 calc R . . 
P1 P 0.7582(3) 0.59077(13) 1.10237(19) 0.0636(9) Uani 1 1 d D . . 
F1 F 0.8138(7) 0.6426(3) 1.1462(5) 0.113(3) Uani 1 1 d D A . 
F2 F 0.8866(9) 0.5662(5) 1.0901(9) 0.106(2) Uiso 0.581(8) 1 d PD A 1 
F3 F 0.7504(14) 0.5609(5) 1.1840(6) 0.106(2) Uiso 0.581(8) 1 d PD A 1 
F4 F 0.6276(9) 0.6140(5) 1.1056(9) 0.106(2) Uiso 0.581(8) 1 d PD A 1 
F5 F 0.7679(13) 0.6183(5) 1.0153(6) 0.106(2) Uiso 0.581(8) 1 d PD A 1 
F6 F 0.7026(7) 0.5398(3) 1.0569(5) 0.115(3) Uani 1 1 d D A . 
F2' F 0.8688(13) 0.5910(7) 1.0480(10) 0.106(2) Uiso 0.419(8) 1 d PD A 2 
F3' F 0.8290(16) 0.5543(6) 1.1660(9) 0.106(2) Uiso 0.419(8) 1 d PD A 2 
F4' F 0.6515(13) 0.5946(7) 1.1616(10) 0.106(2) Uiso 0.419(8) 1 d PD A 2 
F5' F 0.6912(16) 0.6317(5) 1.0424(9) 0.106(2) Uiso 0.419(8) 1 d PD A 2 
P1A P 0.2715(3) 0.76696(15) 0.4110(3) 0.0780(11) Uani 1 1 d D . . 
F1A F 0.1487(10) 0.7489(6) 0.3708(8) 0.126(2) Uiso 0.636(7) 1 d PD B 1 
F2A F 0.2722(13) 0.7170(5) 0.4674(7) 0.126(2) Uiso 0.636(7) 1 d PD B 1 
F3A F 0.2135(12) 0.8046(5) 0.4701(7) 0.126(2) Uiso 0.636(7) 1 d PD B 1 
F4A F 0.2801(12) 0.8152(5) 0.3465(7) 0.126(2) Uiso 0.636(7) 1 d PD B 1 
F5A F 0.3424(12) 0.7314(5) 0.3472(8) 0.126(2) Uiso 0.636(7) 1 d PD B 1 
F6A F 0.4031(10) 0.7832(6) 0.4469(8) 0.126(2) Uiso 0.636(7) 1 d PD B 1 
F1A' F 0.1757(17) 0.7155(7) 0.4077(12) 0.126(2) Uiso 0.364(7) 1 d PD B 2 
F2A' F 0.3667(17) 0.7244(8) 0.4463(12) 0.126(2) Uiso 0.364(7) 1 d PD B 2 
F3A' F 0.2268(18) 0.7724(9) 0.5055(9) 0.126(2) Uiso 0.364(7) 1 d PD B 2 
F4A' F 0.1612(15) 0.8018(8) 0.3828(12) 0.126(2) Uiso 0.364(7) 1 d PD B 2 
F5A' F 0.2983(19) 0.7495(10) 0.3220(9) 0.126(2) Uiso 0.364(7) 1 d PD B 2 
F6A' F 0.3542(17) 0.8149(7) 0.4308(14) 0.126(2) Uiso 0.364(7) 1 d PD B 2 
 
loop_ 
 _atom_site_aniso_label 
 _atom_site_aniso_U_11 
 _atom_site_aniso_U_22 
 _atom_site_aniso_U_33 
 _atom_site_aniso_U_23 
 _atom_site_aniso_U_13 
 _atom_site_aniso_U_12 
Ni1 0.0341(7) 0.0310(6) 0.0398(7) -0.0026(5) 0.0029(5) -0.0023(6) 
Ni1A 0.0399(7) 0.0321(7) 0.0404(7) -0.0003(5) 0.0049(5) 0.0010(6) 
S1 0.0488(17) 0.0606(18) 0.0478(15) -0.0025(13) 0.0110(13) -0.0031(14) 
S1A 0.0518(17) 0.0404(15) 0.0567(16) -0.0062(12) 0.0038(13) -0.0062(13) 
N1 0.042(5) 0.038(5) 0.045(5) -0.001(4) 0.002(4) 0.002(4) 
C1 0.035(6) 0.031(5) 0.063(6) 0.008(5) 0.009(5) 0.007(5) 
N2 0.048(6) 0.058(6) 0.097(8) 0.013(6) 0.018(6) -0.006(5) 
C2 0.050(8) 0.050(8) 0.114(12) -0.002(8) -0.015(8) -0.009(6) 
C3 0.061(9) 0.071(9) 0.089(10) -0.022(8) -0.029(8) 0.002(7) 
C4 0.060(8) 0.060(8) 0.062(7) -0.006(6) -0.012(6) -0.003(7) 
N3 0.037(5) 0.038(5) 0.048(5) -0.005(4) 0.002(4) -0.002(4) 
N4 0.044(5) 0.039(4) 0.033(4) -0.002(3) 0.000(4) 0.007(4) 
N5 0.052(6) 0.032(5) 0.068(6) -0.006(4) -0.003(5) 0.003(4) 
C5 0.045(6) 0.037(6) 0.046(6) 0.006(4) -0.004(5) -0.003(5) 
C6 0.045(6) 0.045(6) 0.051(6) 0.002(5) 0.005(5) 0.010(5) 
C7 0.045(6) 0.050(6) 0.044(6) -0.010(5) -0.007(5) 0.015(5) 
C8 0.051(7) 0.065(7) 0.047(6) 0.009(5) 0.017(5) 0.000(6) 
C9 0.062(8) 0.064(8) 0.060(7) 0.018(6) 0.003(6) -0.006(7) 
C10 0.050(7) 0.036(6) 0.099(9) 0.019(6) -0.006(7) -0.009(6) 
C11 0.070(9) 0.042(6) 0.083(8) -0.022(6) 0.001(7) 0.006(6) 
C12 0.070(9) 0.054(8) 0.078(8) -0.037(6) -0.007(7) -0.001(7) 
C13 0.049(7) 0.072(8) 0.057(7) -0.034(6) 0.000(6) 0.001(6) 
C14 0.053(7) 0.060(8) 0.074(8) -0.007(6) -0.013(6) 0.001(6) 
C15 0.082(9) 0.030(6) 0.062(7) -0.005(5) -0.004(6) 0.001(6) 
C16 0.053(8) 0.093(10) 0.073(8) -0.031(7) -0.002(6) 0.032(7) 
C17 0.055(7) 0.038(6) 0.092(9) 0.005(6) -0.009(7) 0.005(6) 
N1A 0.046(5) 0.041(5) 0.062(5) 0.006(4) 0.008(4) 0.002(4) 
C1A 0.050(7) 0.047(6) 0.040(5) 0.009(5) 0.002(5) 0.004(5) 
N2A 0.037(5) 0.062(6) 0.063(6) 0.006(5) 0.008(5) -0.003(5) 
C2A 0.051(8) 0.097(11) 0.079(9) 0.004(8) 0.022(7) 0.017(8) 
C3A 0.063(9) 0.068(9) 0.097(10) -0.028(8) 0.011(8) 0.016(8) 
C4A 0.065(9) 0.040(7) 0.102(10) -0.013(7) 0.001(8) 0.012(6) 
N3A 0.046(5) 0.039(5) 0.034(4) -0.004(3) 0.002(4) -0.003(4) 
N4A 0.041(5) 0.029(4) 0.060(5) -0.006(4) 0.006(4) 0.005(4) 
N5A 0.055(6) 0.056(6) 0.049(5) 0.009(4) 0.003(4) 0.007(5) 
C5A 0.047(7) 0.040(6) 0.042(6) 0.004(4) 0.004(5) 0.003(5) 
C6A 0.041(6) 0.051(6) 0.045(6) 0.004(5) -0.002(5) -0.007(5) 
C7A 0.042(6) 0.042(6) 0.053(6) -0.016(5) -0.003(5) -0.001(5) 
C8A 0.055(7) 0.040(6) 0.076(8) 0.015(5) 0.010(6) -0.011(6) 
C9A 0.079(9) 0.049(7) 0.086(9) 0.035(7) 0.012(7) -0.006(7) 
C10A 0.083(10) 0.080(9) 0.050(7) 0.023(6) 0.003(7) -0.011(8) 
C11A 0.065(8) 0.080(9) 0.045(6) -0.007(6) 0.003(6) 0.000(7) 
C12A 0.062(8) 0.084(9) 0.054(7) -0.026(6) 0.003(6) 0.007(7) 
C13A 0.056(7) 0.052(7) 0.063(7) -0.014(6) 0.009(6) 0.003(6) 
C14A 0.033(6) 0.083(9) 0.072(8) -0.022(7) 0.004(6) 0.004(6) 
C15A 0.084(10) 0.058(8) 0.078(8) -0.017(6) -0.007(7) -0.006(7) 
C16A 0.060(7) 0.049(6) 0.048(6) -0.012(5) 0.002(5) -0.002(6) 
C17A 0.058(8) 0.092(10) 0.065(8) 0.025(7) 0.001(6) 0.018(7) 
P1 0.063(2) 0.063(2) 0.0640(19) -0.0008(16) -0.0071(16) -0.0017(18) 
F1 0.123(7) 0.086(6) 0.131(7) -0.030(5) 0.014(6) -0.046(6) 
F6 0.125(7) 0.097(6) 0.118(7) -0.047(5) -0.025(6) -0.005(6) 
P1A 0.063(2) 0.059(2) 0.112(3) 0.008(2) 0.009(2) -0.0053(19) 
 
_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 N3 2.024(8) . ? 
Ni1 N4 2.048(8) . ? 
Ni1 N5 2.066(8) . ? 
Ni1 N1 2.107(8) . ? 
Ni1 S1 2.413(3) . ? 
Ni1A N3A 2.026(8) . ? 
Ni1A N4A 2.056(8) . ? 
Ni1A N5A 2.058(8) . ? 
Ni1A N1A 2.125(9) . ? 
Ni1A S1A 2.403(3) . ? 
S1 C1 1.729(11) . ? 
S1A C1A 1.719(11) . ? 
N1 C4 1.336(13) . ? 
N1 C1 1.357(12) . ? 
C1 N2 1.349(13) . ? 
N2 C2 1.345(16) . ? 
C2 C3 1.338(18) . ? 
C3 C4 1.345(17) . ? 
N3 C5 1.263(12) . ? 
N3 C13 1.488(12) . ? 
N4 C8 1.473(12) . ? 
N4 C7 1.532(12) . ? 
N5 C10 1.470(14) . ? 
N5 C17 1.486(13) . ? 
N5 C11 1.515(14) . ? 
C5 C6 1.511(13) . ? 
C5 C14 1.514(14) . ? 
C6 C7 1.485(14) . ? 
C7 C15 1.506(15) . ? 
C7 C16 1.514(14) . ? 
C8 C9 1.515(15) . ? 
C9 C10 1.506(16) . ? 
C11 C12 1.492(16) . ? 
C12 C13 1.505(16) . ? 
N1A C4A 1.330(13) . ? 
N1A C1A 1.356(13) . ? 
C1A N2A 1.352(13) . ? 
N2A C2A 1.305(16) . ? 
C2A C3A 1.365(19) . ? 
C3A C4A 1.363(17) . ? 
N3A C5A 1.291(12) . ? 
N3A C13A 1.463(12) . ? 
N4A C8A 1.472(12) . ? 
N4A C7A 1.513(13) . ? 
N5A C17A 1.475(13) . ? 
N5A C10A 1.486(14) . ? 
N5A C11A 1.516(14) . ? 
C5A C6A 1.483(13) . ? 
C5A C14A 1.501(14) . ? 
C6A C7A 1.516(14) . ? 
C7A C15A 1.522(14) . ? 
C7A C16A 1.527(14) . ? 
C8A C9A 1.501(16) . ? 
C9A C10A 1.492(17) . ? 
C11A C12A 1.511(15) . ? 
C12A C13A 1.537(16) . ? 
P1 F3 1.550(10) . ? 
P1 F3' 1.571(11) . ? 
P1 F2' 1.572(11) . ? 
P1 F4 1.575(10) . ? 
P1 F5' 1.581(11) . ? 
P1 F6 1.582(7) . ? 
P1 F1 1.586(7) . ? 
P1 F2 1.586(10) . ? 
P1 F4' 1.590(11) . ? 
P1 F5 1.606(10) . ? 
P1A F3A 1.524(10) . ? 
P1A F6A' 1.530(14) . ? 
P1A F2A 1.552(10) . ? 
P1A F4A' 1.559(13) . ? 
P1A F1A 1.561(10) . ? 
P1A F5A' 1.582(14) . ? 
P1A F2A' 1.589(13) . ? 
P1A F6A 1.611(11) . ? 
P1A F4A 1.611(10) . ? 
P1A F5A 1.618(11) . ? 
P1A F1A' 1.665(13) . ? 
P1A F3A' 1.676(13) . ? 
 
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 
N3 Ni1 N4 90.3(3) . . ? 
N3 Ni1 N5 93.5(3) . . ? 
N4 Ni1 N5 100.6(3) . . ? 
N3 Ni1 N1 161.3(3) . . ? 
N4 Ni1 N1 94.9(3) . . ? 
N5 Ni1 N1 103.2(3) . . ? 
N3 Ni1 S1 99.6(2) . . ? 
N4 Ni1 S1 154.5(2) . . ? 
N5 Ni1 S1 102.2(3) . . ? 
N1 Ni1 S1 68.8(2) . . ? 
N3A Ni1A N4A 91.0(3) . . ? 
N3A Ni1A N5A 93.4(3) . . ? 
N4A Ni1A N5A 101.5(3) . . ? 
N3A Ni1A N1A 161.0(3) . . ? 
N4A Ni1A N1A 93.6(3) . . ? 
N5A Ni1A N1A 103.7(3) . . ? 
N3A Ni1A S1A 99.6(2) . . ? 
N4A Ni1A S1A 152.7(2) . . ? 
N5A Ni1A S1A 102.9(3) . . ? 
N1A Ni1A S1A 68.8(2) . . ? 
C1 S1 Ni1 79.4(3) . . ? 
C1A S1A Ni1A 79.5(4) . . ? 
C4 N1 C1 116.7(9) . . ? 
C4 N1 Ni1 143.1(8) . . ? 
C1 N1 Ni1 100.0(6) . . ? 
N2 C1 N1 124.9(10) . . ? 
N2 C1 S1 123.1(8) . . ? 
N1 C1 S1 111.9(7) . . ? 
C2 N2 C1 114.3(11) . . ? 
C3 C2 N2 124.0(12) . . ? 
C2 C3 C4 118.4(12) . . ? 
N1 C4 C3 121.6(12) . . ? 
C5 N3 C13 121.3(9) . . ? 
C5 N3 Ni1 127.7(7) . . ? 
C13 N3 Ni1 110.9(6) . . ? 
C8 N4 C7 114.8(8) . . ? 
C8 N4 Ni1 117.1(6) . . ? 
C7 N4 Ni1 106.7(5) . . ? 
C10 N5 C17 108.4(9) . . ? 
C10 N5 C11 110.7(9) . . ? 
C17 N5 C11 106.3(9) . . ? 
C10 N5 Ni1 114.3(7) . . ? 
C17 N5 Ni1 107.9(6) . . ? 
C11 N5 Ni1 108.9(7) . . ? 
N3 C5 C6 122.2(9) . . ? 
N3 C5 C14 125.5(10) . . ? 
C6 C5 C14 112.3(9) . . ? 
C7 C6 C5 122.9(9) . . ? 
C6 C7 C15 112.1(9) . . ? 
C6 C7 C16 108.5(9) . . ? 
C15 C7 C16 110.2(10) . . ? 
C6 C7 N4 110.6(8) . . ? 
C15 C7 N4 105.9(8) . . ? 
C16 C7 N4 109.5(8) . . ? 
N4 C8 C9 111.5(9) . . ? 
C10 C9 C8 113.2(9) . . ? 
N5 C10 C9 115.6(9) . . ? 
C12 C11 N5 115.9(9) . . ? 
C11 C12 C13 116.3(10) . . ? 
N3 C13 C12 109.2(9) . . ? 
C4A N1A C1A 116.9(10) . . ? 
C4A N1A Ni1A 144.1(8) . . ? 
C1A N1A Ni1A 98.7(7) . . ? 
N2A C1A N1A 124.2(10) . . ? 
N2A C1A S1A 122.9(8) . . ? 
N1A C1A S1A 112.8(8) . . ? 
C2A N2A C1A 115.6(10) . . ? 
N2A C2A C3A 124.8(12) . . ? 
C4A C3A C2A 116.3(12) . . ? 
N1A C4A C3A 122.2(12) . . ? 
C5A N3A C13A 120.5(9) . . ? 
C5A N3A Ni1A 127.2(7) . . ? 
C13A N3A Ni1A 112.3(7) . . ? 
C8A N4A C7A 115.4(8) . . ? 
C8A N4A Ni1A 117.3(7) . . ? 
C7A N4A Ni1A 106.5(6) . . ? 
C17A N5A C10A 110.7(9) . . ? 
C17A N5A C11A 107.2(9) . . ? 
C10A N5A C11A 108.9(9) . . ? 
C17A N5A Ni1A 109.2(7) . . ? 
C10A N5A Ni1A 111.2(7) . . ? 
C11A N5A Ni1A 109.5(7) . . ? 
N3A C5A C6A 122.0(9) . . ? 
N3A C5A C14A 124.4(9) . . ? 
C6A C5A C14A 113.6(9) . . ? 
C5A C6A C7A 123.5(9) . . ? 
N4A C7A C6A 110.4(8) . . ? 
N4A C7A C15A 110.4(9) . . ? 
C6A C7A C15A 109.4(9) . . ? 
N4A C7A C16A 106.6(8) . . ? 
C6A C7A C16A 110.1(9) . . ? 
C15A C7A C16A 109.8(9) . . ? 
N4A C8A C9A 113.2(9) . . ? 
C10A C9A C8A 113.8(10) . . ? 
N5A C10A C9A 116.0(10) . . ? 
C12A C11A N5A 117.1(9) . . ? 
C11A C12A C13A 115.7(10) . . ? 
N3A C13A C12A 109.9(9) . . ? 
F3 P1 F3' 35.7(7) . . ? 
F3 P1 F2' 125.9(8) . . ? 
F3' P1 F2' 90.2(7) . . ? 
F3 P1 F4 92.8(6) . . ? 
F3' P1 F4 128.5(8) . . ? 
F2' P1 F4 141.3(8) . . ? 
F3 P1 F5' 144.0(8) . . ? 
F3' P1 F5' 175.2(8) . . ? 
F2' P1 F5' 89.9(7) . . ? 
F4 P1 F5' 51.5(7) . . ? 
F3 P1 F6 89.7(5) . . ? 
F3' P1 F6 91.9(6) . . ? 
F2' P1 F6 91.8(6) . . ? 
F4 P1 F6 88.0(5) . . ? 
F5' P1 F6 92.9(6) . . ? 
F3 P1 F1 91.5(5) . . ? 
F3' P1 F1 89.2(6) . . ? 
F2' P1 F1 87.5(6) . . ? 
F4 P1 F1 91.8(5) . . ? 
F5' P1 F1 86.0(6) . . ? 
F6 P1 F1 178.8(5) . . ? 
F3 P1 F2 91.3(6) . . ? 
F3' P1 F2 55.7(7) . . ? 
F2' P1 F2 34.8(7) . . ? 
F4 P1 F2 174.4(7) . . ? 
F5' P1 F2 124.6(8) . . ? 
F6 P1 F2 88.2(5) . . ? 
F1 P1 F2 91.9(5) . . ? 
F3 P1 F4' 53.8(7) . . ? 
F3' P1 F4' 89.3(7) . . ? 
F2' P1 F4' 175.2(8) . . ? 
F4 P1 F4' 39.4(7) . . ? 
F5' P1 F4' 90.2(7) . . ? 
F6 P1 F4' 93.0(6) . . ? 
F1 P1 F4' 87.6(6) . . ? 
F2 P1 F4' 145.0(8) . . ? 
F3 P1 F5 176.5(7) . . ? 
F3' P1 F5 142.4(8) . . ? 
F2' P1 F5 52.3(7) . . ? 
F4 P1 F5 89.1(6) . . ? 
F5' P1 F5 38.3(6) . . ? 
F6 P1 F5 87.4(5) . . ? 
F1 P1 F5 91.4(5) . . ? 
F2 P1 F5 86.7(6) . . ? 
F4' P1 F5 128.3(8) . . ? 
F3A P1A F6A' 70.2(10) . . ? 
F3A P1A F2A 95.1(6) . . ? 
F6A' P1A F2A 120.4(9) . . ? 
F3A P1A F4A' 59.7(8) . . ? 
F6A' P1A F4A' 95.5(9) . . ? 
F2A P1A F4A' 127.0(9) . . ? 
F3A P1A F1A 93.0(6) . . ? 
F6A' P1A F1A 145.4(9) . . ? 
F2A P1A F1A 90.3(6) . . ? 
F4A' P1A F1A 50.5(8) . . ? 
F3A P1A F5A' 151.2(9) . . ? 
F6A' P1A F5A' 105.6(13) . . ? 
F2A P1A F5A' 110.4(10) . . ? 
F4A' P1A F5A' 93.3(8) . . ? 
F1A P1A F5A' 74.4(10) . . ? 
F3A P1A F2A' 118.0(9) . . ? 
F6A' P1A F2A' 92.8(8) . . ? 
F2A P1A F2A' 42.8(8) . . ? 
F4A' P1A F2A' 169.7(10) . . ? 
F1A P1A F2A' 121.7(9) . . ? 
F5A' P1A F2A' 90.3(8) . . ? 
F3A P1A F6A 91.3(7) . . ? 
F6A' P1A F6A 36.4(8) . . ? 
F2A P1A F6A 90.1(6) . . ? 
F4A' P1A F6A 131.9(9) . . ? 
F1A P1A F6A 175.6(8) . . ? 
F5A' P1A F6A 101.4(10) . . ? 
F2A' P1A F6A 56.4(8) . . ? 
F3A P1A F4A 90.9(6) . . ? 
F6A' P1A F4A 60.7(9) . . ? 
F2A P1A F4A 173.8(7) . . ? 
F4A' P1A F4A 57.6(8) . . ? 
F1A P1A F4A 90.6(6) . . ? 
F5A' P1A F4A 64.0(9) . . ? 
F2A' P1A F4A 132.4(9) . . ? 
F6A P1A F4A 88.5(6) . . ? 
F3A P1A F5A 174.6(8) . . ? 
F6A' P1A F5A 104.5(10) . . ? 
F2A P1A F5A 88.4(6) . . ? 
F4A' P1A F5A 121.0(9) . . ? 
F1A P1A F5A 91.0(7) . . ? 
F5A' P1A F5A 28.0(8) . . ? 
F2A' P1A F5A 62.4(8) . . ? 
F6A P1A F5A 84.6(8) . . ? 
F4A P1A F5A 85.5(6) . . ? 
F3A P1A F1A' 101.1(9) . . ? 
F6A' P1A F1A' 169.2(11) . . ? 
F2A P1A F1A' 52.5(8) . . ? 
F4A' P1A F1A' 85.1(8) . . ? 
F1A P1A F1A' 38.3(7) . . ? 
F5A' P1A F1A' 85.1(9) . . ? 
F2A' P1A F1A' 85.6(8) . . ? 
F6A P1A F1A' 141.1(9) . . ? 
F4A P1A F1A' 127.4(9) . . ? 
F5A P1A F1A' 84.2(9) . . ? 
F3A P1A F3A' 35.9(8) . . ? 
F6A' P1A F3A' 86.8(9) . . ? 
F2A P1A F3A' 59.5(8) . . ? 
F4A' P1A F3A' 87.9(8) . . ? 
F1A P1A F3A' 96.9(9) . . ? 
F5A' P1A F3A' 167.3(11) . . ? 
F2A' P1A F3A' 86.4(8) . . ? 
F6A P1A F3A' 87.0(9) . . ? 
F4A P1A F3A' 126.4(8) . . ? 
F5A P1A F3A' 146.8(9) . . ? 
F1A' P1A F3A' 82.4(8) . . ? 
 
_diffrn_measured_fraction_theta_max    0.995 
_diffrn_reflns_theta_full              25.00 
_diffrn_measured_fraction_theta_full   0.995 
_refine_diff_density_max    0.923 
_refine_diff_density_min   -0.898 
_refine_diff_density_rms    0.116 
 
#===END
 
 
data_dsl02 
 
_audit_creation_method            SHELXL 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_formula_moiety          ? 
_chemical_formula_structural      ? 
_chemical_formula_analytical      ? 
_chemical_formula_sum             'C20 H32 F6 N5 Ni P S' 
_chemical_formula_weight          578.25 
_chemical_melting_point           ? 
_chemical_compound_source         'slow evaporation acetone solution' 
 
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    P2(1)/c
 
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 '-x, y+1/2, -z+1/2' 
 '-x, -y, -z' 
 'x, -y-1/2, z-1/2' 
 
_cell_length_a                    10.938(2) 
_cell_length_b                    14.318(2) 
_cell_length_c                    15.938(2) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  92.728(12) 
_cell_angle_gamma                 90.00 
_cell_volume                      2493.2(6) 
_cell_formula_units_Z             4 
_cell_measurement_temperature     293(2) 
_cell_measurement_reflns_used     73
_cell_measurement_theta_min        3.700
_cell_measurement_theta_max       12.28
 
_exptl_crystal_description       'plate'
_exptl_crystal_colour            'blue'
_exptl_crystal_size_max           0.64 
_exptl_crystal_size_mid           0.28 
_exptl_crystal_size_min           0.06 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.541 
_exptl_crystal_density_method     ? 
_exptl_crystal_F_000              1200 
_exptl_absorpt_coefficient_mu     0.990 
_exptl_absorpt_correction_type    'Psi scans'
_exptl_absorpt_correction_T_min   0.704
_exptl_absorpt_correction_T_max   0.831
 
_exptl_special_details 
; 
 ? 
; 
 
_diffrn_ambient_temperature       293(2) 
_diffrn_radiation_wavelength      0.71073 
_diffrn_radiation_type            MoK\a 
_diffrn_radiation_source          'fine-focus sealed tube' 
_diffrn_radiation_monochromator   graphite 
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       '\w scans'
_diffrn_standards_number            3
_diffrn_standards_interval_count  247
_diffrn_standards_decay_%            2.04
_diffrn_reflns_number             4797 
_diffrn_reflns_av_R_equivalents   0.0378 
_diffrn_reflns_av_sigmaI/netI     0.1122 
_diffrn_reflns_limit_h_min        -13 
_diffrn_reflns_limit_h_max        13 
_diffrn_reflns_limit_k_min        0 
_diffrn_reflns_limit_k_max        17 
_diffrn_reflns_limit_l_min        -18 
_diffrn_reflns_limit_l_max        18 
_diffrn_reflns_theta_min          3.09 
_diffrn_reflns_theta_max          25.00 
_reflns_number_total              4373 
_reflns_number_observed           2268 
_reflns_observed_criterion        >2sigma(I) 
 
_computing_data_collection      'Siemens XSCANS'
_computing_cell_refinement      'Siemens XSCANS'
_computing_data_reduction       'Siemens XSCANS'
_computing_structure_solution   'Siemens SHELXTL'
_computing_structure_refinement   'SHELXL-93 (Sheldrick, 1993)' 
_computing_molecular_graphics   'Siemens SHELXTL'
_computing_publication_material 'Siemens SHELXTL'
 
_refine_special_details 
; 
 Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ 
 or flagged by the user for potential systematic errors.  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. 
 The hexafluorphosphate anion is disordered over two sites.
; 
 
_refine_ls_structure_factor_coef  Fsqd  
_refine_ls_matrix_type            full 
_refine_ls_weighting_scheme 
 'calc w=1/[\s^2^(Fo^2^)+(0.1128P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' 
_atom_sites_solution_primary      Patterson
_atom_sites_solution_secondary    difmap 
_atom_sites_solution_hydrogens    geom 
_refine_ls_hydrogen_treatment     
'NH free, rigid methyls others riding'
_refine_ls_extinction_method      none 
_refine_ls_extinction_coef        ? 
_refine_ls_number_reflns          4373 
_refine_ls_number_parameters      301 
_refine_ls_number_restraints      598 
_refine_ls_R_factor_all           0.1318 
_refine_ls_R_factor_obs           0.0673 
_refine_ls_wR_factor_all          0.2004 
_refine_ls_wR_factor_obs          0.1707 
_refine_ls_goodness_of_fit_all    0.904 
_refine_ls_goodness_of_fit_obs    1.096 
_refine_ls_restrained_S_all       0.959 
_refine_ls_restrained_S_obs       1.139 
_refine_ls_shift/esd_max          0.002 
_refine_ls_shift/esd_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_thermal_displace_type 
 _atom_site_occupancy 
 _atom_site_calc_flag 
 _atom_site_refinement_flags 
 _atom_site_disorder_group 
Ni Ni 0.41260(8) 0.28594(6) 0.46740(5) 0.0323(3) Uani 1 d . . 
S S 0.5069(2) 0.2871(2) 0.61938(12) 0.0473(5) Uani 1 d . . 
N1 N 0.4137(5) 0.3162(4) 0.3425(3) 0.0320(13) Uani 1 d DU . 
H1 H 0.4604(60) 0.2932(50) 0.3252(46) 0.038 Uiso 1 d D . 
N2 N 0.2817(5) 0.3824(4) 0.4832(3) 0.0374(14) Uani 1 d U . 
N3 N 0.2951(6) 0.1735(4) 0.4678(4) 0.0442(15) Uani 1 d U . 
C1 C 0.4388(6) 0.4191(5) 0.3358(4) 0.036(2) Uani 1 d U . 
C2 C 0.3274(7) 0.4744(5) 0.3605(4) 0.044(2) Uani 1 d U . 
H2A H 0.3517(7) 0.5395(5) 0.3627(4) 0.052 Uiso 1 calc R . 
H2B H 0.2667(7) 0.4686(5) 0.3144(4) 0.052 Uiso 1 calc R . 
C3 C 0.2624(6) 0.4551(5) 0.4397(4) 0.037(2) Uani 1 d U . 
C4 C 0.2070(7) 0.3609(6) 0.5558(5) 0.047(2) Uani 1 d U . 
H4A H 0.1498(7) 0.4116(6) 0.5638(5) 0.056 Uiso 1 calc R . 
H4B H 0.2600(7) 0.3561(6) 0.6062(5) 0.056 Uiso 1 calc R . 
C5 C 0.1371(7) 0.2710(6) 0.5430(5) 0.054(2) Uani 1 d U . 
H5A H 0.0808(7) 0.2650(6) 0.5880(5) 0.064 Uiso 1 calc R . 
H5B H 0.0883(7) 0.2757(6) 0.4908(5) 0.064 Uiso 1 calc R . 
C6 C 0.2118(7) 0.1828(6) 0.5403(5) 0.049(2) Uani 1 d U . 
H6A H 0.1560(7) 0.1300(6) 0.5387(5) 0.059 Uiso 1 calc R . 
H6B H 0.2615(7) 0.1784(6) 0.5922(5) 0.059 Uiso 1 calc R . 
C7 C 0.2175(7) 0.1625(6) 0.3894(5) 0.050(2) Uani 1 d U . 
H7A H 0.1498(7) 0.2061(6) 0.3909(5) 0.060 Uiso 1 calc R . 
H7B H 0.1834(7) 0.1000(6) 0.3881(5) 0.060 Uiso 1 calc R . 
C8 C 0.2837(8) 0.1785(6) 0.3090(5) 0.050(2) Uani 1 d U . 
H8A H 0.3611(8) 0.1454(6) 0.3129(5) 0.060 Uiso 1 calc R . 
H8B H 0.2351(8) 0.1520(6) 0.2623(5) 0.060 Uiso 1 calc R . 
C9 C 0.3080(7) 0.2801(5) 0.2904(4) 0.041(2) Uani 1 d U . 
H9A H 0.3244(7) 0.2870(5) 0.2315(4) 0.049 Uiso 1 calc R . 
H9B H 0.2358(7) 0.3166(5) 0.3014(4) 0.049 Uiso 1 calc R . 
C10 C 0.5497(7) 0.4398(5) 0.3966(4) 0.043(2) Uani 1 d U . 
H10A H 0.5712(25) 0.5046(8) 0.3928(20) 0.051 Uiso 1 calc R . 
H10B H 0.6179(14) 0.4020(22) 0.3817(17) 0.051 Uiso 1 calc R . 
H10C H 0.5289(15) 0.4255(28) 0.4530(5) 0.051 Uiso 1 calc R . 
C11 C 0.4721(8) 0.4462(6) 0.2473(4) 0.054(2) Uani 1 d U . 
H11A H 0.4921(43) 0.5115(9) 0.2460(8) 0.064 Uiso 1 calc R . 
H11B H 0.4039(17) 0.4341(32) 0.2087(6) 0.064 Uiso 1 calc R . 
H11C H 0.5414(28) 0.4102(25) 0.2314(12) 0.064 Uiso 1 calc R . 
C12 C 0.1683(8) 0.5298(6) 0.4571(5) 0.059(2) Uani 1 d U . 
H12A H 0.0882(9) 0.5023(9) 0.4561(30) 0.071 Uiso 1 calc R . 
H12B H 0.1704(32) 0.5775(18) 0.4148(18) 0.071 Uiso 1 calc R . 
H12C H 0.1867(27) 0.5569(24) 0.5113(14) 0.071 Uiso 1 calc R . 
C13 C 0.3683(8) 0.0860(5) 0.4833(6) 0.059(2) Uani 1 d U . 
H13A H 0.4199(33) 0.0933(14) 0.5333(18) 0.071 Uiso 1 calc R . 
H13B H 0.4180(34) 0.0744(19) 0.4364(15) 0.071 Uiso 1 calc R . 
H13C H 0.3138(8) 0.0343(8) 0.4902(31) 0.071 Uiso 1 calc R . 
N4 N 0.5817(5) 0.2249(4) 0.4757(4) 0.0399(14) Uani 1 d U . 
N5 N 0.7201(6) 0.1960(5) 0.5769(4) 0.049(2) Uani 1 d DU . 
H5 H 0.7424(81) 0.2024(66) 0.6155(38) 0.059 Uiso 1 d D . 
C20 C 0.6089(7) 0.2334(5) 0.5567(4) 0.038(2) Uani 1 d U . 
C21 C 0.7663(7) 0.1598(5) 0.5054(5) 0.042(2) Uani 1 d DU . 
C22 C 0.6804(7) 0.1788(5) 0.4417(5) 0.040(2) Uani 1 d DU . 
C23 C 0.7000(8) 0.1518(6) 0.3595(5) 0.054(2) Uani 1 d DU . 
H23 H 0.6426(8) 0.1647(6) 0.3161(5) 0.065 Uiso 1 calc R . 
C24 C 0.8069(8) 0.1054(6) 0.3444(6) 0.062(2) Uani 1 d DU . 
H24 H 0.8227(8) 0.0876(6) 0.2899(6) 0.074 Uiso 1 calc R . 
C25 C 0.8921(8) 0.0848(6) 0.4097(6) 0.064(2) Uani 1 d DU . 
H25 H 0.9625(8) 0.0517(6) 0.3983(6) 0.077 Uiso 1 calc R . 
C26 C 0.8735(8) 0.1124(6) 0.4904(6) 0.060(2) Uani 1 d DU . 
H26 H 0.9310(8) 0.0998(6) 0.5338(6) 0.071 Uiso 1 calc R . 
P P 0.9253(2) 0.3962(2) 0.26982(14) 0.0566(6) Uani 1 d DU . 
F1 F 1.0340(10) 0.3898(9) 0.2063(7) 0.1126(14) Uiso 0.504(5) d PDU 1 
F2 F 0.9809(12) 0.4990(8) 0.2951(7) 0.1126(14) Uiso 0.504(5) d PDU 1 
F3 F 0.8451(11) 0.4517(9) 0.1990(7) 0.1126(14) Uiso 0.504(5) d PDU 1 
F4 F 0.8687(13) 0.3041(8) 0.2376(8) 0.1126(14) Uiso 0.504(5) d PDU 1 
F5 F 1.0156(11) 0.3501(9) 0.3356(7) 0.1126(14) Uiso 0.504(5) d PDU 1 
F6 F 0.8278(11) 0.4118(10) 0.3341(7) 0.1126(14) Uiso 0.504(5) d PDU 1 
F1' F 1.0511(11) 0.4389(9) 0.2717(8) 0.1126(14) Uiso 0.496(5) d PDU 2 
F2' F 0.8657(12) 0.4807(9) 0.3157(8) 0.1126(14) Uiso 0.496(5) d PDU 2 
F3' F 0.8910(12) 0.4400(10) 0.1808(7) 0.1126(14) Uiso 0.496(5) d PDU 2 
F4' F 0.9652(13) 0.3046(8) 0.2220(8) 0.1126(14) Uiso 0.496(5) d PDU 2 
F5' F 0.9511(12) 0.3505(9) 0.3586(7) 0.1126(14) Uiso 0.496(5) d PDU 2 
F6' F 0.7907(11) 0.3446(9) 0.2663(8) 0.1126(14) Uiso 0.496(5) d PDU 2 
 
loop_ 
 _atom_site_aniso_label 
 _atom_site_aniso_U_11 
 _atom_site_aniso_U_22 
 _atom_site_aniso_U_33 
 _atom_site_aniso_U_23 
 _atom_site_aniso_U_13 
 _atom_site_aniso_U_12 
Ni 0.0316(5) 0.0313(5) 0.0336(5) 0.0005(4) -0.0038(3) -0.0008(5) 
S 0.0500(12) 0.0469(11) 0.0447(10) 0.0020(10) -0.0009(9) 0.0006(11) 
N1 0.031(3) 0.035(3) 0.031(3) -0.003(2) 0.002(2) 0.002(3) 
N2 0.036(3) 0.039(3) 0.038(3) -0.004(3) -0.002(3) -0.002(3) 
N3 0.047(4) 0.039(3) 0.047(3) 0.004(3) -0.001(3) -0.007(3) 
C1 0.035(4) 0.033(4) 0.041(4) 0.001(3) 0.000(3) -0.003(3) 
C2 0.047(4) 0.035(4) 0.049(4) 0.004(3) 0.000(3) 0.002(4) 
C3 0.032(4) 0.039(4) 0.039(4) -0.007(3) -0.008(3) 0.001(3) 
C4 0.042(5) 0.054(4) 0.045(4) 0.001(4) 0.009(3) 0.008(4) 
C5 0.034(4) 0.078(6) 0.049(4) 0.000(4) 0.009(3) -0.013(4) 
C6 0.048(5) 0.053(4) 0.047(4) 0.006(4) 0.003(3) -0.019(4) 
C7 0.052(5) 0.046(5) 0.051(4) -0.006(4) -0.001(3) -0.018(4) 
C8 0.053(5) 0.053(4) 0.045(4) -0.016(4) -0.001(4) -0.011(4) 
C9 0.047(4) 0.049(4) 0.027(3) -0.003(3) -0.004(3) -0.009(4) 
C10 0.042(4) 0.036(4) 0.051(4) 0.000(3) 0.000(3) -0.002(3) 
C11 0.069(6) 0.051(5) 0.042(4) 0.006(4) 0.010(4) -0.006(5) 
C12 0.053(5) 0.060(5) 0.064(5) -0.001(4) 0.000(4) 0.020(4) 
C13 0.062(6) 0.027(4) 0.087(6) 0.010(4) 0.004(4) -0.004(4) 
N4 0.037(3) 0.036(4) 0.046(3) 0.004(3) -0.009(3) 0.003(3) 
N5 0.041(4) 0.055(5) 0.050(4) 0.008(4) -0.012(3) 0.002(3) 
C20 0.043(4) 0.031(4) 0.041(4) 0.010(3) 0.000(3) -0.007(3) 
C21 0.035(4) 0.037(4) 0.055(4) 0.001(3) -0.004(3) -0.004(3) 
C22 0.029(4) 0.032(4) 0.059(4) 0.000(3) 0.000(3) -0.003(3) 
C23 0.052(5) 0.049(5) 0.060(4) -0.008(4) -0.004(4) -0.001(4) 
C24 0.044(5) 0.059(6) 0.082(6) -0.018(5) 0.011(4) -0.003(4) 
C25 0.032(4) 0.050(5) 0.111(7) -0.009(5) 0.012(4) -0.002(4) 
C26 0.035(4) 0.052(5) 0.091(5) 0.006(5) -0.005(4) 0.001(4) 
P 0.0500(14) 0.073(2) 0.0460(12) -0.0057(11) -0.0049(10) 0.0008(13) 
 
_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 
Ni N2 2.014(6) . ? 
Ni N1 2.039(6) . ? 
Ni N4 2.044(6) . ? 
Ni N3 2.061(6) . ? 
Ni S 2.587(2) . ? 
S C20 1.714(8) . ? 
N1 C9 1.484(9) . ? 
N1 C1 1.503(9) . ? 
N2 C3 1.263(9) . ? 
N2 C4 1.480(9) . ? 
N3 C7 1.484(9) . ? 
N3 C13 1.501(10) . ? 
N3 C6 1.512(9) . ? 
C1 C2 1.521(10) . ? 
C1 C11 1.523(9) . ? 
C1 C10 1.544(9) . ? 
C2 C3 1.504(10) . ? 
C3 C12 1.519(10) . ? 
C4 C5 1.506(11) . ? 
C5 C6 1.506(11) . ? 
C7 C8 1.520(10) . ? 
C8 C9 1.510(11) . ? 
N4 C20 1.317(9) . ? 
N4 C22 1.396(9) . ? 
N5 C20 1.354(10) . ? 
N5 C21 1.370(10) . ? 
C21 C22 1.377(10) . ? 
C21 C26 1.385(11) . ? 
C22 C23 1.394(10) . ? 
C23 C24 1.376(11) . ? 
C24 C25 1.394(12) . ? 
C25 C26 1.370(12) . ? 
P F1' 1.504(12) . ? 
P F6 1.531(10) . ? 
P F4 1.535(10) . ? 
P F5 1.552(10) . ? 
P F2' 1.572(11) . ? 
P F5' 1.572(11) . ? 
P F3' 1.580(11) . ? 
P F4' 1.588(11) . ? 
P F1 1.601(10) . ? 
P F3 1.607(10) . ? 
P F2 1.636(10) . ? 
P F6' 1.646(12) . ? 
 
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 
N2 Ni N1 90.8(2) . . ? 
N2 Ni N4 158.7(2) . . ? 
N1 Ni N4 96.1(2) . . ? 
N2 Ni N3 95.1(2) . . ? 
N1 Ni N3 101.6(2) . . ? 
N4 Ni N3 103.2(2) . . ? 
N2 Ni S 97.6(2) . . ? 
N1 Ni S 153.2(2) . . ? 
N4 Ni S 67.8(2) . . ? 
N3 Ni S 102.9(2) . . ? 
C20 S Ni 72.1(2) . . ? 
C9 N1 C1 116.3(6) . . ? 
C9 N1 Ni 115.5(4) . . ? 
C1 N1 Ni 106.7(4) . . ? 
C3 N2 C4 121.1(6) . . ? 
C3 N2 Ni 126.7(5) . . ? 
C4 N2 Ni 112.2(5) . . ? 
C7 N3 C13 109.3(6) . . ? 
C7 N3 C6 108.1(6) . . ? 
C13 N3 C6 106.5(6) . . ? 
C7 N3 Ni 114.3(5) . . ? 
C13 N3 Ni 108.9(5) . . ? 
C6 N3 Ni 109.4(4) . . ? 
N1 C1 C2 109.9(6) . . ? 
N1 C1 C11 111.6(6) . . ? 
C2 C1 C11 109.7(6) . . ? 
N1 C1 C10 106.5(6) . . ? 
C2 C1 C10 110.7(6) . . ? 
C11 C1 C10 108.5(6) . . ? 
C3 C2 C1 122.6(6) . . ? 
N2 C3 C2 122.6(7) . . ? 
N2 C3 C12 125.3(7) . . ? 
C2 C3 C12 112.0(6) . . ? 
N2 C4 C5 111.6(6) . . ? 
C6 C5 C4 116.6(6) . . ? 
C5 C6 N3 116.3(6) . . ? 
N3 C7 C8 114.7(6) . . ? 
C9 C8 C7 113.9(6) . . ? 
N1 C9 C8 111.5(6) . . ? 
C20 N4 C22 106.3(6) . . ? 
C20 N4 Ni 100.7(5) . . ? 
C22 N4 Ni 153.0(5) . . ? 
C20 N5 C21 108.3(6) . . ? 
N4 C20 N5 110.8(6) . . ? 
N4 C20 S 119.3(6) . . ? 
N5 C20 S 129.9(6) . . ? 
N5 C21 C22 105.8(7) . . ? 
N5 C21 C26 132.6(8) . . ? 
C22 C21 C26 121.6(8) . . ? 
C21 C22 C23 120.6(7) . . ? 
C21 C22 N4 108.7(7) . . ? 
C23 C22 N4 130.7(7) . . ? 
C24 C23 C22 117.9(8) . . ? 
C23 C24 C25 121.0(9) . . ? 
C26 C25 C24 121.0(8) . . ? 
C25 C26 C21 117.9(8) . . ? 
F6 P F4 93.8(7) . . ? 
F6 P F5 92.9(6) . . ? 
F4 P F5 95.4(7) . . ? 
F1' P F2' 94.4(7) . . ? 
F1' P F5' 91.5(6) . . ? 
F2' P F5' 87.8(6) . . ? 
F1' P F3' 92.0(6) . . ? 
F2' P F3' 91.5(6) . . ? 
F5' P F3' 176.5(7) . . ? 
F1' P F4' 94.2(7) . . ? 
F2' P F4' 171.3(7) . . ? 
F5' P F4' 92.7(6) . . ? 
F3' P F4' 87.5(6) . . ? 
F6 P F1 173.9(7) . . ? 
F4 P F1 92.2(6) . . ? 
F5 P F1 86.3(6) . . ? 
F6 P F3 91.3(6) . . ? 
F4 P F3 89.5(6) . . ? 
F5 P F3 173.2(7) . . ? 
F1 P F3 88.9(6) . . ? 
F6 P F2 88.1(6) . . ? 
F4 P F2 174.2(6) . . ? 
F5 P F2 90.0(6) . . ? 
F1 P F2 85.9(6) . . ? 
F3 P F2 84.9(6) . . ? 
F1' P F6' 177.2(7) . . ? 
F2' P F6' 88.4(6) . . ? 
F5' P F6' 88.0(6) . . ? 
F3' P F6' 88.5(6) . . ? 
F4' P F6' 83.0(6) . . ? 
 
_refine_diff_density_max    0.816 
_refine_diff_density_min   -0.654 
_refine_diff_density_rms    0.100 
 
#===END