# Copyright The Royal Society of Chemistry, 1999
# CCDC Number: 186/1477
 
data_s6 
 
_audit_creation_method            SHELXL 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_formula_moiety          ? 
_chemical_formula_structural      ? 
_chemical_formula_analytical      ? 
_chemical_formula_sum             'C106 H97 F12 N18 Ni O2.50 P2' 
_chemical_formula_weight          2011.67 
_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' 
 '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           '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                    22.705(8) 
_cell_length_b                    16.855(2) 
_cell_length_c                    25.917(4) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  96.44(2) 
_cell_angle_gamma                 90.00 
_cell_volume                      9855.5(40) 
_cell_formula_units_Z             4 
_cell_measurement_temperature     293(2) 
_cell_measurement_reflns_used     28 
_cell_measurement_theta_min       4.82 
_cell_measurement_theta_max       12.01 
 
_exptl_crystal_description        block 
_exptl_crystal_colour             red 
_exptl_crystal_size_max           0.60 
_exptl_crystal_size_mid           0.40 
_exptl_crystal_size_min           0.40 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.356 
_exptl_crystal_density_method     ? 
_exptl_crystal_F_000              4180 
_exptl_absorpt_coefficient_mu     0.313 
_exptl_absorpt_correction_type    'emprical psi-scan' 
_exptl_absorpt_correction_T_min   0.6544 
_exptl_absorpt_correction_T_max   0.6807 
 
_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       '2\q/\w scans'
_diffrn_standards_number            3
_diffrn_standards_interval_count   97
_diffrn_standards_decay_%         12.71 
_diffrn_reflns_number             9717 
_diffrn_reflns_av_R_equivalents   0.0519 
_diffrn_reflns_av_sigmaI/netI     0.0824 
_diffrn_reflns_limit_h_min        -1 
_diffrn_reflns_limit_h_max        23 
_diffrn_reflns_limit_k_min        -1 
_diffrn_reflns_limit_k_max        20 
_diffrn_reflns_limit_l_min        -30 
_diffrn_reflns_limit_l_max        30 
_diffrn_reflns_theta_min          1.75 
_diffrn_reflns_theta_max          25.00 
_reflns_number_total              8372 
_reflns_number_observed           4488 
_reflns_observed_criterion        >2sigma(I) 
 
_computing_data_collection      'Siemens XSCANS'
_computing_cell_refinement      'Siemens XSCANS'
_computing_data_reduction       'Siemens SHELXTL'
_computing_structure_solution   'Siemens SHELXTL'
_computing_structure_refinement 'Siemens SHELXTL'
_computing_molecular_graphics   'Siemens SHELXTL'
_computing_publication_material 'Siemens SHELXTL'

 
_refine_special_details 
; 
 Refinement on F^2^ for ALL reflections except for 25 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. 

 Hydrogen atoms of the water molecule were found from the difmap and refined
 using riding model
 
 Of all the 25 refletion supressed, only 10 were supressed using OMIT, others
 were supressed by the program.

 The PF6 anion were refined disordered with (P-F distanse were fixed at 
 1.540(10), however the s.o.f. of the F atoms were fefined as free variable. 
 
 The oxygen atom of the water molecule at special position was also refined
 disordered with s.o.f. = 0.25.

 The ethanol molecules were also  refined disordered with C-C distance
 was fixed at 1.500(20), C-O was fixed at 1.500(20). The s.o.f were refined 
 as free variable 
 
; 
 
_refine_ls_structure_factor_coef  Fsqd  
_refine_ls_matrix_type            full 
_refine_ls_weighting_scheme 
 'calc w=1/[\s^2^(Fo^2^)+(0.1064P)^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     'riding model' 
_refine_ls_extinction_method      none 
_refine_ls_extinction_coef        ? 
_refine_ls_number_reflns          8347 
_refine_ls_number_parameters      727 
_refine_ls_number_restraints      72 
_refine_ls_R_factor_all           0.1397 
_refine_ls_R_factor_obs           0.0720 
_refine_ls_wR_factor_all          0.2258 
_refine_ls_wR_factor_obs          0.1735 
_refine_ls_goodness_of_fit_all    1.025 
_refine_ls_goodness_of_fit_obs    1.181 
_refine_ls_restrained_S_all       1.099 
_refine_ls_restrained_S_obs       1.190 
_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 
Ni1 Ni 0.0000 0.27546(5) 0.7500 0.0492(3) Uani 1 d S . 
N1 N -0.1415(3) 0.4956(3) 0.9436(3) 0.113(2) Uani 1 d . . 
C1 C -0.1715(6) 0.4578(5) 0.9781(3) 0.147(4) Uani 1 d . . 
H1A H -0.1553(6) 0.4578(5) 1.0127(3) 0.176 Uiso 1 calc R . 
C2 C -0.2246(6) 0.4192(6) 0.9657(5) 0.165(5) Uani 1 d . . 
H2A H -0.2425(6) 0.3920(6) 0.9910(5) 0.198 Uiso 1 calc R . 
C3 C -0.2496(5) 0.4214(5) 0.9169(5) 0.147(4) Uani 1 d . . 
H3A H -0.2857(5) 0.3965(5) 0.9074(5) 0.176 Uiso 1 calc R . 
C4 C -0.2214(3) 0.4607(4) 0.8813(3) 0.104(2) Uani 1 d . . 
H4A H -0.2389(3) 0.4634(4) 0.8471(3) 0.125 Uiso 1 calc R . 
C5 C -0.1683(3) 0.4961(3) 0.8945(3) 0.086(2) Uani 1 d . . 
N2 N -0.1631(2) 0.5413(2) 0.8076(2) 0.0749(11) Uani 1 d . . 
C6 C -0.1350(2) 0.5369(3) 0.8557(2) 0.0753(14) Uani 1 d . . 
C7 C -0.0785(3) 0.5670(4) 0.8679(3) 0.102(2) Uani 1 d . . 
H7A H -0.0598(3) 0.5645(4) 0.9017(3) 0.122 Uiso 1 calc R . 
C8 C -0.0507(3) 0.6002(4) 0.8293(3) 0.112(2) Uani 1 d . . 
H8A H -0.0122(3) 0.6195(4) 0.8361(3) 0.135 Uiso 1 calc R . 
C9 C -0.0804(3) 0.6049(4) 0.7799(3) 0.108(2) Uani 1 d . . 
H9A H -0.0624(3) 0.6282(4) 0.7532(3) 0.130 Uiso 1 calc R . 
C10 C -0.1357(3) 0.5757(3) 0.7707(2) 0.0796(15) Uani 1 d . . 
C11 C -0.1692(3) 0.5791(4) 0.7174(2) 0.107(2) Uani 1 d . . 
H11A H -0.1468(3) 0.6101(4) 0.6949(2) 0.128 Uiso 1 calc R . 
H11B H -0.2068(3) 0.6057(4) 0.7193(2) 0.128 Uiso 1 calc R . 
C12 C -0.1808(2) 0.4963(4) 0.6941(2) 0.095(2) Uani 1 d . . 
H12A H -0.1991(2) 0.4635(4) 0.7185(2) 0.114 Uiso 1 calc R . 
H12B H -0.2082(2) 0.5006(4) 0.6627(2) 0.114 Uiso 1 calc R . 
N3 N -0.04632(15) 0.3627(2) 0.70367(13) 0.0536(9) Uani 1 d . . 
C13 C -0.0963(2) 0.3993(3) 0.7136(2) 0.0636(12) Uani 1 d . . 
H13A H -0.1129(2) 0.3855(3) 0.7436(2) 0.076 Uiso 1 calc R . 
C14 C -0.1244(2) 0.4567(3) 0.6812(2) 0.0695(13) Uani 1 d . . 
C15 C -0.0985(3) 0.4752(3) 0.6374(2) 0.084(2) Uani 1 d . . 
H15A H -0.1160(3) 0.5134(3) 0.6147(2) 0.100 Uiso 1 calc R . 
C16 C -0.0472(2) 0.4386(3) 0.6259(2) 0.0731(14) Uani 1 d . . 
H16A H -0.0299(2) 0.4518(3) 0.5962(2) 0.088 Uiso 1 calc R . 
C17 C -0.0221(2) 0.3810(2) 0.6606(2) 0.0536(11) Uani 1 d . . 
N4 N 0.05290(14) 0.2857(2) 0.68966(13) 0.0513(9) Uani 1 d . . 
C18 C 0.0330(2) 0.3380(3) 0.6522(2) 0.0554(11) Uani 1 d . . 
C19 C 0.0632(2) 0.3490(3) 0.6094(2) 0.0743(14) Uani 1 d . . 
H19A H 0.0490(2) 0.3845(3) 0.5834(2) 0.089 Uiso 1 calc R . 
C20 C 0.1151(2) 0.3066(3) 0.6054(2) 0.0766(15) Uani 1 d . . 
H20A H 0.1354(2) 0.3136(3) 0.5765(2) 0.092 Uiso 1 calc R . 
C21 C 0.1365(2) 0.2544(3) 0.6438(2) 0.0611(12) Uani 1 d . . 
C22 C 0.1032(2) 0.2463(3) 0.6845(2) 0.0562(11) Uani 1 d . . 
H22A H 0.1166(2) 0.2106(3) 0.7106(2) 0.067 Uiso 1 calc R . 
C23 C 0.1927(2) 0.2087(3) 0.6410(2) 0.081(2) Uani 1 d . . 
H23A H 0.2004(2) 0.1766(3) 0.6721(2) 0.097 Uiso 1 calc R . 
H23B H 0.2252(2) 0.2459(3) 0.6406(2) 0.097 Uiso 1 calc R . 
C24 C 0.1912(3) 0.1559(4) 0.5944(2) 0.090(2) Uani 1 d . . 
H24A H 0.1890(3) 0.1881(4) 0.5632(2) 0.108 Uiso 1 calc R . 
H24B H 0.2275(3) 0.1251(4) 0.5964(2) 0.108 Uiso 1 calc R . 
N5 N 0.1396(2) 0.0471(3) 0.6293(2) 0.0757(12) Uani 1 d . . 
C25 C 0.1396(3) 0.1014(4) 0.5913(2) 0.081(2) Uani 1 d . . 
C26 C 0.0931(4) 0.1074(5) 0.5532(3) 0.115(2) Uani 1 d . . 
H26A H 0.0934(4) 0.1450(5) 0.5270(3) 0.138 Uiso 1 calc R . 
C27 C 0.0450(4) 0.0560(6) 0.5543(4) 0.134(3) Uani 1 d . . 
H27A H 0.0131(4) 0.0592(6) 0.5285(4) 0.161 Uiso 1 calc R . 
C28 C 0.0445(3) -0.0009(5) 0.5945(4) 0.122(3) Uani 1 d . . 
H28A H 0.0127(3) -0.0353(5) 0.5962(4) 0.146 Uiso 1 calc R . 
C29 C 0.0940(3) -0.0029(4) 0.6315(3) 0.087(2) Uani 1 d . . 
N6 N 0.0559(3) -0.1162(4) 0.6702(3) 0.153(3) Uani 1 d . . 
C30 C 0.0996(3) -0.0619(4) 0.6746(3) 0.101(2) Uani 1 d . . 
C31 C 0.1450(4) -0.0591(4) 0.7143(3) 0.116(2) Uani 1 d . . 
H31A H 0.1745(4) -0.0207(4) 0.7152(3) 0.139 Uiso 1 calc R . 
C32 C 0.1450(5) -0.1147(6) 0.7523(4) 0.165(4) Uani 1 d . . 
H32A H 0.1743(5) -0.1126(6) 0.7804(4) 0.198 Uiso 1 calc R . 
C33 C 0.1042(7) -0.1727(7) 0.7508(4) 0.173(5) Uani 1 d . . 
H33A H 0.1052(7) -0.2120(7) 0.7761(4) 0.208 Uiso 1 calc R . 
C34 C 0.0613(6) -0.1696(6) 0.7097(5) 0.173(5) Uani 1 d . . 
H34A H 0.0322(6) -0.2086(6) 0.7085(5) 0.207 Uiso 1 calc R . 
N7 N 0.3876(2) 0.2139(3) 1.0489(2) 0.100(2) Uani 1 d . . 
C35 C 0.4378(3) 0.2470(5) 1.0376(4) 0.125(3) Uani 1 d . . 
H35A H 0.4647(3) 0.2627(5) 1.0655(4) 0.150 Uiso 1 calc R . 
C36 C 0.4526(3) 0.2596(5) 0.9912(4) 0.126(3) Uani 1 d . . 
H36A H 0.4893(3) 0.2815(5) 0.9867(4) 0.151 Uiso 1 calc R . 
C37 C 0.4127(4) 0.2396(5) 0.9487(4) 0.136(3) Uani 1 d . . 
H37A H 0.4211(4) 0.2500(5) 0.9150(4) 0.163 Uiso 1 calc R . 
C38 C 0.3595(3) 0.2037(4) 0.9578(3) 0.110(2) Uani 1 d . . 
H38A H 0.3319(3) 0.1885(4) 0.9303(3) 0.132 Uiso 1 calc R . 
C39 C 0.3492(2) 0.1915(3) 1.0080(2) 0.0758(14) Uani 1 d . . 
N8 N 0.2522(2) 0.1385(2) 0.97926(14) 0.0629(10) Uani 1 d . . 
C40 C 0.2926(2) 0.1548(3) 1.0199(2) 0.0634(12) Uani 1 d . . 
C41 C 0.2825(3) 0.1373(3) 1.0706(2) 0.085(2) Uani 1 d . . 
H41A H 0.3110(3) 0.1493(3) 1.0981(2) 0.102 Uiso 1 calc R . 
C42 C 0.2307(3) 0.1025(4) 1.0796(2) 0.095(2) Uani 1 d . . 
H42A H 0.2232(3) 0.0907(4) 1.1133(2) 0.114 Uiso 1 calc R . 
C43 C 0.1895(2) 0.0849(3) 1.0381(2) 0.081(2) Uani 1 d . . 
H43A H 0.1540(2) 0.0601(3) 1.0433(2) 0.097 Uiso 1 calc R . 
C44 C 0.2013(2) 0.1045(3) 0.9889(2) 0.0636(12) Uani 1 d . . 
C45 C 0.1555(2) 0.0874(3) 0.9432(2) 0.0781(15) Uani 1 d . . 
H45A H 0.1532(2) 0.0304(3) 0.9380(2) 0.094 Uiso 1 calc R . 
H45B H 0.1171(2) 0.1051(3) 0.9518(2) 0.094 Uiso 1 calc R . 
C46 C 0.1675(2) 0.1258(3) 0.8933(2) 0.0728(14) Uani 1 d . . 
H46A H 0.2027(2) 0.1023(3) 0.8817(2) 0.087 Uiso 1 calc R . 
H46B H 0.1752(2) 0.1818(3) 0.8994(2) 0.087 Uiso 1 calc R . 
C47 C 0.0903(2) 0.1824(3) 0.8259(2) 0.0557(11) Uani 1 d . . 
H47A H 0.1046(2) 0.2322(3) 0.8365(2) 0.067 Uiso 1 calc R . 
C48 C 0.1164(2) 0.1168(3) 0.8507(2) 0.0605(12) Uani 1 d . . 
C49 C 0.0942(2) 0.0436(3) 0.8342(2) 0.080(2) Uani 1 d . . 
H49A H 0.1102(2) -0.0025(3) 0.8498(2) 0.096 Uiso 1 calc R . 
C50 C 0.0481(2) 0.0386(3) 0.7948(2) 0.0718(14) Uani 1 d . . 
H50A H 0.0331(2) -0.0107(3) 0.7839(2) 0.086 Uiso 1 calc R . 
C51 C 0.0244(2) 0.1070(2) 0.77132(15) 0.0502(10) Uani 1 d . . 
N9 N 0.04525(14) 0.1789(2) 0.78719(12) 0.0497(9) Uani 1 d . . 
P1 P -0.11576(10) -0.2634(2) 0.58846(9) 0.1263(8) Uani 1 d D . 
F1 F -0.0654(11) -0.2851(27) 0.6298(9) 0.235(14) Uani 0.53(2) d PD 1 
F2 F -0.1327(14) -0.3509(6) 0.5905(8) 0.270(14) Uani 0.53(2) d PD 1 
F3 F -0.1040(10) -0.1740(6) 0.5868(12) 0.243(12) Uani 0.53(2) d PD 1 
F4 F -0.1583(8) -0.2419(12) 0.6293(8) 0.155(7) Uani 0.53(2) d PD 1 
F5 F -0.1741(8) -0.2388(16) 0.5574(10) 0.254(14) Uani 0.53(2) d PD 1 
F6 F -0.0942(10) -0.2845(13) 0.5355(6) 0.198(8) Uani 0.53(2) d PD 1 
F3' F -0.0660(15) -0.2042(22) 0.5807(10) 0.268(16) Uani 0.47(2) d PD 2 
F2' F -0.0709(8) -0.3163(17) 0.5640(11) 0.248(14) Uani 0.47(2) d PD 2 
F1' F -0.1409(19) -0.2025(23) 0.6248(11) 0.301(22) Uani 0.47(2) d PD 2 
F4' F -0.1576(12) -0.2447(15) 0.5396(8) 0.225(15) Uani 0.47(2) d PD 2 
F5' F -0.1559(5) -0.3364(7) 0.5931(7) 0.139(8) Uani 0.47(2) d PD 2 
F6' F -0.0857(12) -0.2835(31) 0.6434(6) 0.189(11) Uani 0.47(2) d PD 2 
O1W O 0.0000 0.5000 1.0000 0.244(12) Uani 0.50 d SP . 
H1WA H 0.0191 0.4572 1.0000 0.366 Uiso 0.25 d PR . 
H1WB H 0.0188 0.5543 0.9903 0.366 Uiso 0.25 d PR . 
C52 C 0.2506(11) 0.2425(15) 0.8016(13) 0.209(8) Uani 0.639(9) d PDU 1 
H52A H 0.2229(11) 0.2190(15) 0.8231(13) 0.250 Uiso 0.639(9) calc PR 1 
H52D H 0.2582(11) 0.2012(15) 0.7771(13) 0.250 Uiso 0.639(9) calc PR 1 
O1 O 0.3053(7) 0.2432(10) 0.8365(6) 0.274(7) Uani 0.639(9) d PDU 1 
H1B H 0.3123(7) 0.1983(10) 0.8478(6) 0.411 Uiso 0.639(9) calc PR 1 
C53 C 0.2123(8) 0.2976(12) 0.7687(8) 0.227(8) Uani 0.639(9) d PDU 1 
H53A H 0.1790(8) 0.2692(12) 0.7517(8) 0.340 Uiso 0.639(9) calc PR 1 
H53B H 0.2345(8) 0.3207(12) 0.7430(8) 0.340 Uiso 0.639(9) calc PR 1 
H53C H 0.1985(8) 0.3389(12) 0.7899(8) 0.340 Uiso 0.639(9) calc PR 1 
C52' C 0.2154(12) 0.2037(18) 0.7824(16) 0.228(9) Uani 0.361(9) d PDU 2 
H52B H 0.1945(12) 0.2203(18) 0.7495(16) 0.273 Uiso 0.361(9) calc PR 2 
H52C H 0.1867(12) 0.2091(18) 0.8073(16) 0.273 Uiso 0.361(9) calc PR 2 
C53' C 0.2190(11) 0.1158(17) 0.7760(10) 0.231(14) Uani 0.361(9) d PDU 2 
H53D H 0.1800(11) 0.0948(17) 0.7666(10) 0.347 Uiso 0.361(9) calc PR 2 
H53E H 0.2357(11) 0.0924(17) 0.8081(10) 0.347 Uiso 0.361(9) calc PR 2 
H53F H 0.2436(11) 0.1038(17) 0.7493(10) 0.347 Uiso 0.361(9) calc PR 2 
O1' O 0.2556(16) 0.2709(16) 0.7958(17) 0.207(9) Uani 0.361(9) d PDU 2 
H1'A H 0.2368(16) 0.3125(16) 0.7931(17) 0.311 Uiso 0.361(9) calc PR 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 0.0451(4) 0.0475(5) 0.0535(5) 0.000 -0.0011(3) 0.000 
N1 0.170(6) 0.083(4) 0.088(4) -0.005(3) 0.021(4) 0.017(4) 
C1 0.258(12) 0.094(6) 0.097(6) -0.003(5) 0.061(8) 0.040(7) 
C2 0.226(13) 0.097(7) 0.197(12) 0.033(8) 0.131(12) 0.039(8) 
C3 0.153(8) 0.091(6) 0.211(10) 0.027(7) 0.083(9) 0.014(5) 
C4 0.097(5) 0.089(5) 0.132(6) 0.017(4) 0.034(4) 0.004(4) 
C5 0.105(5) 0.064(4) 0.093(5) -0.004(3) 0.023(4) 0.008(3) 
N2 0.076(3) 0.067(3) 0.081(3) -0.002(2) 0.009(3) 0.012(2) 
C6 0.079(4) 0.061(3) 0.084(4) -0.013(3) 0.000(3) 0.009(3) 
C7 0.098(5) 0.097(5) 0.107(5) -0.017(4) -0.002(4) -0.004(4) 
C8 0.080(4) 0.120(6) 0.138(6) -0.017(5) 0.016(5) -0.025(4) 
C9 0.115(6) 0.089(5) 0.126(6) 0.012(4) 0.036(5) 0.005(4) 
C10 0.085(4) 0.061(3) 0.094(4) -0.005(3) 0.015(4) 0.024(3) 
C11 0.133(5) 0.091(4) 0.097(5) 0.006(4) 0.018(4) 0.062(4) 
C12 0.086(4) 0.109(5) 0.086(4) -0.003(3) -0.008(3) 0.045(4) 
N3 0.053(2) 0.050(2) 0.056(2) -0.003(2) -0.001(2) 0.003(2) 
C13 0.063(3) 0.063(3) 0.063(3) -0.005(2) 0.001(2) 0.009(3) 
C14 0.066(3) 0.071(3) 0.068(3) -0.004(3) -0.009(3) 0.021(3) 
C15 0.100(4) 0.076(4) 0.072(4) 0.008(3) -0.003(3) 0.027(3) 
C16 0.082(3) 0.074(3) 0.064(3) 0.015(3) 0.011(3) 0.021(3) 
C17 0.057(3) 0.048(3) 0.055(3) -0.003(2) 0.000(2) 0.002(2) 
N4 0.051(2) 0.046(2) 0.056(2) -0.002(2) 0.001(2) -0.001(2) 
C18 0.063(3) 0.045(2) 0.058(3) 0.001(2) 0.005(2) -0.005(2) 
C19 0.085(3) 0.068(3) 0.073(3) 0.020(3) 0.023(3) 0.009(3) 
C20 0.079(3) 0.069(3) 0.088(4) 0.008(3) 0.036(3) 0.004(3) 
C21 0.058(3) 0.058(3) 0.070(3) 0.002(2) 0.019(2) -0.005(2) 
C22 0.049(3) 0.055(3) 0.065(3) 0.004(2) 0.005(2) 0.001(2) 
C23 0.064(3) 0.082(4) 0.103(4) 0.009(3) 0.036(3) 0.008(3) 
C24 0.091(4) 0.088(4) 0.098(4) 0.012(3) 0.044(3) 0.019(4) 
N5 0.075(3) 0.074(3) 0.081(3) -0.013(3) 0.018(2) 0.013(3) 
C25 0.096(4) 0.078(4) 0.068(3) -0.003(3) 0.008(3) 0.035(3) 
C26 0.133(6) 0.107(6) 0.100(5) -0.010(4) -0.013(5) 0.036(5) 
C27 0.124(6) 0.124(7) 0.141(7) -0.037(6) -0.042(6) 0.029(6) 
C28 0.093(5) 0.104(6) 0.164(8) -0.039(5) -0.005(5) 0.002(4) 
C29 0.075(4) 0.084(4) 0.102(5) -0.032(4) 0.010(4) 0.006(3) 
N6 0.157(6) 0.093(5) 0.220(8) -0.012(5) 0.072(6) -0.015(5) 
C30 0.115(5) 0.056(4) 0.144(7) -0.009(4) 0.068(5) -0.004(4) 
C31 0.162(7) 0.103(5) 0.084(5) 0.015(4) 0.019(5) -0.007(5) 
C32 0.261(12) 0.102(6) 0.139(8) 0.017(6) 0.061(8) -0.005(8) 
C33 0.274(15) 0.113(8) 0.144(9) 0.042(7) 0.074(9) 0.009(9) 
C34 0.229(13) 0.098(7) 0.212(12) 0.019(8) 0.117(11) -0.001(8) 
N7 0.069(3) 0.100(4) 0.121(4) 0.002(3) -0.027(3) -0.005(3) 
C35 0.069(5) 0.112(6) 0.189(9) -0.008(6) -0.008(5) -0.006(4) 
C36 0.079(5) 0.126(6) 0.179(8) -0.055(6) 0.038(6) -0.018(4) 
C37 0.149(7) 0.122(6) 0.150(7) -0.041(5) 0.078(6) -0.045(5) 
C38 0.107(5) 0.116(5) 0.111(5) -0.026(4) 0.034(4) -0.039(4) 
C39 0.076(4) 0.056(3) 0.095(4) -0.010(3) 0.010(3) 0.009(3) 
N8 0.065(2) 0.056(2) 0.064(2) 0.005(2) -0.005(2) 0.006(2) 
C40 0.063(3) 0.053(3) 0.071(3) 0.001(2) -0.007(3) 0.011(2) 
C41 0.087(4) 0.093(4) 0.069(4) 0.015(3) -0.020(3) -0.001(3) 
C42 0.100(4) 0.115(5) 0.065(4) 0.022(3) -0.006(3) -0.011(4) 
C43 0.077(3) 0.087(4) 0.077(4) 0.025(3) -0.002(3) -0.009(3) 
C44 0.063(3) 0.057(3) 0.067(3) 0.014(2) -0.014(2) 0.004(2) 
C45 0.073(3) 0.086(4) 0.072(3) 0.013(3) -0.009(3) -0.008(3) 
C46 0.061(3) 0.077(3) 0.075(3) 0.011(3) -0.015(3) 0.005(3) 
C47 0.052(2) 0.056(3) 0.057(3) 0.001(2) -0.005(2) 0.000(2) 
C48 0.057(3) 0.062(3) 0.060(3) 0.004(2) -0.007(2) 0.008(2) 
C49 0.088(4) 0.056(3) 0.089(4) 0.009(3) -0.017(3) 0.015(3) 
C50 0.088(3) 0.049(3) 0.073(3) -0.001(2) -0.014(3) 0.005(3) 
C51 0.050(2) 0.046(3) 0.054(3) 0.000(2) 0.005(2) -0.001(2) 
N9 0.045(2) 0.053(2) 0.051(2) 0.001(2) 0.001(2) 0.002(2) 
P1 0.111(2) 0.147(2) 0.124(2) 0.033(2) 0.0301(14) 0.007(2) 
F1 0.115(13) 0.266(22) 0.298(29) -0.025(33) -0.089(17) 0.097(17) 
F2 0.545(41) 0.079(8) 0.182(14) 0.011(8) 0.017(22) 0.084(16) 
F3 0.227(18) 0.137(11) 0.380(33) 0.078(17) 0.105(19) -0.029(11) 
F4 0.126(8) 0.170(13) 0.177(13) -0.013(10) 0.051(8) -0.006(10) 
F5 0.163(12) 0.221(20) 0.372(35) -0.037(19) -0.002(17) 0.085(12) 
F6 0.164(16) 0.290(19) 0.149(11) 0.025(12) 0.054(11) 0.010(13) 
F3' 0.282(27) 0.318(29) 0.221(18) -0.085(20) 0.110(20) -0.203(24) 
F2' 0.120(12) 0.458(43) 0.177(18) -0.078(22) 0.068(13) 0.005(15) 
F1' 0.356(50) 0.362(50) 0.181(20) -0.012(26) 0.012(25) 0.220(37) 
F4' 0.332(36) 0.193(19) 0.124(11) 0.094(12) -0.091(16) -0.021(20) 
F5' 0.076(7) 0.172(17) 0.171(13) 0.079(12) 0.017(6) -0.023(7) 
F6' 0.180(23) 0.249(23) 0.139(12) -0.009(13) 0.020(13) 0.054(22) 
O1W 0.212(17) 0.453(38) 0.053(8) -0.060(13) -0.045(10) 0.032(21) 
C52 0.184(14) 0.261(20) 0.195(15) -0.027(16) 0.080(12) -0.067(16) 
O1 0.224(13) 0.260(15) 0.325(18) 0.040(13) -0.034(13) 0.052(12) 
C53 0.152(13) 0.245(20) 0.270(19) -0.069(17) -0.033(13) -0.007(14) 
C52' 0.185(17) 0.301(22) 0.204(17) -0.006(19) 0.055(15) -0.051(18) 
C53' 0.155(19) 0.369(34) 0.185(22) 0.146(25) 0.089(17) 0.118(23) 
O1' 0.202(17) 0.190(18) 0.232(19) -0.030(17) 0.029(16) -0.043(16) 
 
_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 N4 2.083(3) 2_556 ? 
Ni1 N4 2.083(3) . ? 
Ni1 N9 2.100(3) 2_556 ? 
Ni1 N9 2.100(3) . ? 
Ni1 N3 2.104(3) 2_556 ? 
Ni1 N3 2.104(3) . ? 
N1 C1 1.345(11) . ? 
N1 C5 1.347(7) . ? 
C1 C2 1.376(13) . ? 
C2 C3 1.328(13) . ? 
C3 C4 1.353(10) . ? 
C4 C5 1.355(8) . ? 
C5 C6 1.492(8) . ? 
N2 C10 1.331(7) . ? 
N2 C6 1.338(6) . ? 
C6 C7 1.383(8) . ? 
C7 C8 1.361(9) . ? 
C8 C9 1.380(8) . ? 
C9 C10 1.345(8) . ? 
C10 C11 1.502(8) . ? 
C11 C12 1.532(8) . ? 
C12 C14 1.514(7) . ? 
N3 C17 1.335(5) . ? 
N3 C13 1.341(5) . ? 
C13 C14 1.387(6) . ? 
C14 C15 1.373(7) . ? 
C15 C16 1.378(7) . ? 
C16 C17 1.400(6) . ? 
C17 C18 1.482(6) . ? 
N4 C22 1.341(5) . ? 
N4 C18 1.352(5) . ? 
C18 C19 1.382(6) . ? 
C19 C20 1.392(7) . ? 
C20 C21 1.377(7) . ? 
C21 C22 1.371(6) . ? 
C21 C23 1.498(6) . ? 
C23 C24 1.499(7) . ? 
C24 C25 1.483(8) . ? 
N5 C29 1.341(7) . ? 
N5 C25 1.345(7) . ? 
C25 C26 1.367(8) . ? 
C26 C27 1.395(10) . ? 
C27 C28 1.418(11) . ? 
C28 C29 1.392(9) . ? 
C29 C30 1.490(9) . ? 
N6 C30 1.346(9) . ? 
N6 C34 1.357(12) . ? 
C30 C31 1.373(9) . ? 
C31 C32 1.359(10) . ? 
C32 C33 1.344(13) . ? 
C33 C34 1.362(14) . ? 
N7 C35 1.330(8) . ? 
N7 C39 1.349(6) . ? 
C35 C36 1.303(10) . ? 
C36 C37 1.389(10) . ? 
C37 C38 1.394(9) . ? 
C38 C39 1.365(8) . ? 
C39 C40 1.490(7) . ? 
N8 C44 1.338(6) . ? 
N8 C40 1.346(5) . ? 
C40 C41 1.390(7) . ? 
C41 C42 1.357(7) . ? 
C42 C43 1.378(7) . ? 
C43 C44 1.372(6) . ? 
C44 C45 1.511(6) . ? 
C45 C46 1.500(6) . ? 
C46 C48 1.516(6) . ? 
C47 N9 1.351(5) . ? 
C47 C48 1.380(6) . ? 
C48 C49 1.383(7) . ? 
C49 C50 1.380(6) . ? 
C50 C51 1.383(6) . ? 
C51 N9 1.350(5) . ? 
C51 C51 1.473(8) 2_556 ? 
P1 F1 1.521(9) . ? 
P1 F2 1.526(9) . ? 
P1 F5 1.528(9) . ? 
P1 F4' 1.529(8) . ? 
P1 F3 1.532(9) . ? 
P1 F3' 1.537(9) . ? 
P1 F2' 1.542(9) . ? 
P1 F5' 1.543(8) . ? 
P1 F1' 1.544(10) . ? 
P1 F6' 1.546(9) . ? 
P1 F6 1.550(9) . ? 
P1 F4 1.554(9) . ? 
C52 O1 1.452(10) . ? 
C52 C53 1.476(10) . ? 
C52' O1' 1.472(10) . ? 
C52' C53' 1.494(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 
N4 Ni1 N4 170.5(2) 2_556 . ? 
N4 Ni1 N9 96.60(13) 2_556 2_556 ? 
N4 Ni1 N9 90.76(12) . 2_556 ? 
N4 Ni1 N9 90.76(12) 2_556 . ? 
N4 Ni1 N9 96.60(13) . . ? 
N9 Ni1 N9 78.4(2) 2_556 . ? 
N4 Ni1 N3 78.88(14) 2_556 2_556 ? 
N4 Ni1 N3 94.43(13) . 2_556 ? 
N9 Ni1 N3 172.29(13) 2_556 2_556 ? 
N9 Ni1 N3 95.29(13) . 2_556 ? 
N4 Ni1 N3 94.43(13) 2_556 . ? 
N4 Ni1 N3 78.88(14) . . ? 
N9 Ni1 N3 95.29(13) 2_556 . ? 
N9 Ni1 N3 172.30(13) . . ? 
N3 Ni1 N3 91.3(2) 2_556 . ? 
C1 N1 C5 115.0(7) . . ? 
N1 C1 C2 124.3(10) . . ? 
C3 C2 C1 118.6(11) . . ? 
C2 C3 C4 118.6(11) . . ? 
C3 C4 C5 121.3(8) . . ? 
N1 C5 C4 122.1(6) . . ? 
N1 C5 C6 115.4(6) . . ? 
C4 C5 C6 122.5(6) . . ? 
C10 N2 C6 118.7(5) . . ? 
N2 C6 C7 121.7(6) . . ? 
N2 C6 C5 115.3(5) . . ? 
C7 C6 C5 122.9(6) . . ? 
C8 C7 C6 118.6(6) . . ? 
C7 C8 C9 119.1(6) . . ? 
C10 C9 C8 119.5(6) . . ? 
N2 C10 C9 122.4(6) . . ? 
N2 C10 C11 116.6(6) . . ? 
C9 C10 C11 121.0(7) . . ? 
C10 C11 C12 112.0(5) . . ? 
C14 C12 C11 112.2(5) . . ? 
C17 N3 C13 119.4(4) . . ? 
C17 N3 Ni1 114.4(3) . . ? 
C13 N3 Ni1 126.2(3) . . ? 
N3 C13 C14 123.1(4) . . ? 
C15 C14 C13 116.6(4) . . ? 
C15 C14 C12 122.2(5) . . ? 
C13 C14 C12 121.2(5) . . ? 
C14 C15 C16 121.8(5) . . ? 
C15 C16 C17 117.7(5) . . ? 
N3 C17 C16 121.4(4) . . ? 
N3 C17 C18 116.3(4) . . ? 
C16 C17 C18 122.3(4) . . ? 
C22 N4 C18 118.1(4) . . ? 
C22 N4 Ni1 127.1(3) . . ? 
C18 N4 Ni1 114.7(3) . . ? 
N4 C18 C19 120.5(4) . . ? 
N4 C18 C17 115.7(4) . . ? 
C19 C18 C17 123.8(4) . . ? 
C18 C19 C20 119.5(5) . . ? 
C21 C20 C19 120.5(5) . . ? 
C22 C21 C20 116.1(4) . . ? 
C22 C21 C23 122.1(4) . . ? 
C20 C21 C23 121.8(4) . . ? 
N4 C22 C21 125.2(4) . . ? 
C21 C23 C24 113.8(5) . . ? 
C25 C24 C23 110.9(4) . . ? 
C29 N5 C25 121.6(5) . . ? 
N5 C25 C26 120.9(7) . . ? 
N5 C25 C24 116.6(5) . . ? 
C26 C25 C24 122.4(6) . . ? 
C25 C26 C27 118.9(7) . . ? 
C26 C27 C28 120.3(7) . . ? 
C29 C28 C27 116.8(7) . . ? 
N5 C29 C28 121.4(7) . . ? 
N5 C29 C30 116.7(6) . . ? 
C28 C29 C30 121.8(7) . . ? 
C30 N6 C34 112.6(9) . . ? 
N6 C30 C31 124.8(8) . . ? 
N6 C30 C29 112.9(8) . . ? 
C31 C30 C29 122.2(6) . . ? 
C32 C31 C30 117.2(9) . . ? 
C33 C32 C31 122.5(11) . . ? 
C32 C33 C34 115.1(10) . . ? 
N6 C34 C33 127.7(12) . . ? 
C35 N7 C39 116.1(6) . . ? 
C36 C35 N7 126.0(8) . . ? 
C35 C36 C37 118.7(7) . . ? 
C36 C37 C38 118.1(7) . . ? 
C39 C38 C37 118.2(7) . . ? 
N7 C39 C38 122.8(5) . . ? 
N7 C39 C40 116.8(5) . . ? 
C38 C39 C40 120.3(5) . . ? 
C44 N8 C40 118.0(4) . . ? 
N8 C40 C41 121.8(5) . . ? 
N8 C40 C39 116.8(4) . . ? 
C41 C40 C39 121.5(5) . . ? 
C42 C41 C40 119.5(5) . . ? 
C41 C42 C43 118.9(5) . . ? 
C44 C43 C42 119.2(5) . . ? 
N8 C44 C43 122.6(4) . . ? 
N8 C44 C45 117.9(4) . . ? 
C43 C44 C45 119.5(5) . . ? 
C46 C45 C44 114.7(4) . . ? 
C45 C46 C48 112.8(4) . . ? 
N9 C47 C48 124.1(4) . . ? 
C47 C48 C49 116.7(4) . . ? 
C47 C48 C46 120.8(4) . . ? 
C49 C48 C46 122.5(4) . . ? 
C50 C49 C48 120.1(4) . . ? 
C49 C50 C51 120.1(5) . . ? 
N9 C51 C50 120.5(4) . . ? 
N9 C51 C51 115.9(2) . 2_556 ? 
C50 C51 C51 123.6(3) . 2_556 ? 
C51 N9 C47 118.4(4) . . ? 
C51 N9 Ni1 114.8(3) . . ? 
C47 N9 Ni1 126.7(3) . . ? 
F1 P1 F2 85.1(20) . . ? 
F1 P1 F5 167.1(15) . . ? 
F2 P1 F5 94.3(15) . . ? 
F1 P1 F3 97.8(21) . . ? 
F2 P1 F3 175.4(13) . . ? 
F5 P1 F3 82.1(14) . . ? 
F4' P1 F3' 98.9(17) . . ? 
F4' P1 F2' 99.0(13) . . ? 
F3' P1 F2' 78.0(17) . . ? 
F4' P1 F5' 85.0(10) . . ? 
F3' P1 F5' 167.5(17) . . ? 
F2' P1 F5' 89.7(12) . . ? 
F4' P1 F1' 97.5(18) . . ? 
F3' P1 F1' 88.5(18) . . ? 
F2' P1 F1' 160.1(19) . . ? 
F5' P1 F1' 102.8(20) . . ? 
F4' P1 F6' 167.9(16) . . ? 
F3' P1 F6' 90.4(19) . . ? 
F2' P1 F6' 90.5(14) . . ? 
F5' P1 F6' 87.6(20) . . ? 
F1' P1 F6' 74.9(19) . . ? 
F1 P1 F6 106.4(13) . . ? 
F2 P1 F6 85.2(12) . . ? 
F5 P1 F6 86.4(11) . . ? 
F3 P1 F6 97.3(14) . . ? 
F1 P1 F4 92.9(15) . . ? 
F2 P1 F4 91.4(11) . . ? 
F5 P1 F4 74.2(15) . . ? 
F3 P1 F4 85.0(12) . . ? 
F6 P1 F4 160.0(13) . . ? 
O1 C52 C53 139.7(18) . . ? 
O1' C52' C53' 138.5(23) . . ? 
 
_refine_diff_density_max    0.584 
_refine_diff_density_min   -0.635 
_refine_diff_density_rms    0.057