Supplementary Material (ESI) for Dalton Transactions
This journal is (c) The Royal Society of Chemistry 2002


data_global

_journal_coden_Cambridge      186

_publ_requested_journal       'Dalton Transactions'

loop_
_publ_author_name
'Evans, D.'
'Barclay, J. Elaine'
'Cramer, Stephen P.'
'Davies, Sian C.'
'Gu, Wei-Wei'
'Hughes, David L.'
'Longhurst, Steven'
'Smith, Matt C.'

_publ_contact_author_name     	'Dr D Evans'  
_publ_contact_author_address 
;
Dept of Biological Chemistry
John Innes Centre
Norwich Research Park
Norwich
Norfolk
NR4 7UH
UK
;

_publ_contact_author_email       'DAVE.EVANS@BBSRC.AC.UK'

_publ_section_title		
;
Nickel-iron-sulfur complexes: approaching structural analogues of
the active sites of NiFe-hydrogenase and carbon monoxide
dehydrogenase/acetyl-CoA synthase
;



data_matt1

_database_code_CSD	181375


_audit_creation_method            SHELXL 
_chemical_name_systematic 
; 
? 
; 
_chemical_name_common             'Complex 3'
_chemical_formula_moiety          'C32 H36 Cl Fe N2 Ni O P2 S3, C2 H3 N'
_chemical_formula_structural      '[{Fe(NO)(N{CH2CH2S}3)-S,S'}NiCl(dppe)]'
_chemical_formula_analytical      ? 
_chemical_formula_sum             'C34 H39 Cl Fe N3 Ni O P2 S3' 
_chemical_formula_weight          813.81 
_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' 
'Cl'  'Cl'   0.1484   0.1585 
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
'Fe'  'Fe'   0.3463   0.8444 
'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' 
'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' 
'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' 

_symmetry_cell_setting            Monoclinic
_symmetry_space_group_name_H-M    'P 21/c'
_symmetry_Int_Tables_number		14

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                    11.9861(15) 
_cell_length_b                    19.719(3) 
_cell_length_c                    15.709(2) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  103.345(10) 
_cell_angle_gamma                 90.00 
_cell_volume                      3612.6(8) 
_cell_formula_units_Z             4 
_cell_measurement_temperature     293(2) 
_cell_measurement_reflns_used     24
_cell_measurement_theta_min       10
_cell_measurement_theta_max       11

_exptl_crystal_description        'rhombic prisms'
_exptl_crystal_colour             'Dark brown'
_exptl_crystal_size_max           0.48
_exptl_crystal_size_mid           0.24
_exptl_crystal_size_min           0.21
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.496 
_exptl_crystal_density_method     ? 
_exptl_crystal_F_000              1684 
_exptl_absorpt_coefficient_mu     1.291 
_exptl_absorpt_correction_type    'semi-empirical psi-scans' 
_exptl_absorpt_correction_T_min   0.955
_exptl_absorpt_correction_T_max   0.997

_exptl_special_details 
; 
? 
; 

_diffrn_ambient_temperature       293(2) 
_diffrn_radiation_wavelength      0.71069 
_diffrn_radiation_type            Mo-K\a 
_diffrn_radiation_source          'fine-focus sealed tube' 
_diffrn_radiation_monochromator   graphite 
_diffrn_measurement_device        'Enraf-Nonius CAD4 diffractometer'
_diffrn_measurement_method        'scintillation counter; \w/\q scans'
_diffrn_standards_number          3 
_diffrn_standards_interval_count  ?
_diffrn_standards_interval_time   '10000 s'
_diffrn_standards_decay_%         0
_diffrn_reflns_number             8511
_diffrn_reflns_av_R_equivalents   0.014 
_diffrn_reflns_av_sigmaI/netI     0.0518 
_diffrn_reflns_limit_h_min        -15 
_diffrn_reflns_limit_h_max        14 
_diffrn_reflns_limit_k_min        -1
_diffrn_reflns_limit_k_max        25 
_diffrn_reflns_limit_l_min        -1
_diffrn_reflns_limit_l_max        20 
_diffrn_reflns_theta_min          1.5 
_diffrn_reflns_theta_max          27.0 
_reflns_number_total              7866 
_reflns_number_observed           5425 
_reflns_observed_criterion        I>2sigma(I) 

_computing_data_collection        'CAD4/EXPRESS (Enraf-Nonius, 1992)'
_computing_cell_refinement        'CAD4/EXPRESS (Enraf-Nonius, 1992)'
_computing_data_reduction         'CAD4 (Hursthouse, 1976)'
_computing_structure_solution     'SHELXS-86 (Sheldrick, 1990)' 
_computing_structure_refinement   'SHELXL-93 (Sheldrick, 1993)' 
_computing_molecular_graphics     'ORTEP (Johnson, 1971)'
_computing_publication_material   'SHELXL-93 (Sheldrick, 1993)' 

_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. 
; 

_refine_ls_structure_factor_coef  Fsqd  
_refine_ls_matrix_type            full 
_refine_ls_weighting_scheme 
'calc w=1/[\s^2^(Fo^2^)+(0.0310P)^2^+0.1485P] 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     
;
Hydrogen coordinates were initially located in idealised positions and 
subsequently refined freely except those of the disordered carbons, which
were set to ride on the parent atoms.  All isotropic thermal displacement
parameters were refined freely.
;
_refine_ls_extinction_method      none 
_refine_ls_extinction_coef        ? 
_refine_ls_number_reflns          7866 
_refine_ls_number_parameters      581 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.0599 
_refine_ls_R_factor_obs           0.0347 
_refine_ls_wR_factor_all          0.0843 
_refine_ls_wR_factor_obs          0.0714 
_refine_ls_goodness_of_fit_all    1.044 
_refine_ls_goodness_of_fit_obs    1.082 
_refine_ls_restrained_S_all       1.044 
_refine_ls_restrained_S_obs       1.082 
_refine_ls_shift/esd_max          0.001 
_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 0.29004(3) 0.14600(2) 0.13027(2) 0.03028(9) Uani 1 d . . 
Cl Cl 0.22895(6) 0.23745(4) 0.02591(4) 0.0425(2) Uani 1 d . . 
P1 P 0.22138(5) 0.16788(4) 0.24494(4) 0.0330(2) Uani 1 d . . 
C111 C 0.0887(2) 0.21719(13) 0.2271(2) 0.0354(6) Uani 1 d . . 
C112 C 0.0198(2) 0.2251(2) 0.1450(2) 0.0448(7) Uani 1 d . . 
H112 H 0.0414(22) 0.2109(14) 0.0994(18) 0.039(8) Uiso 1 d . . 
C113 C -0.0817(3) 0.2616(2) 0.1323(2) 0.0559(8) Uani 1 d . . 
H113 H -0.1271(24) 0.2644(14) 0.0744(20) 0.049(8) Uiso 1 d . . 
C114 C -0.1142(3) 0.2903(2) 0.2019(2) 0.0549(8) Uani 1 d . . 
H114 H -0.1778(30) 0.3162(17) 0.1937(22) 0.074(11) Uiso 1 d . . 
C115 C -0.0458(3) 0.2828(2) 0.2846(2) 0.0582(9) Uani 1 d . . 
H115 H -0.0677(28) 0.3041(17) 0.3350(22) 0.072(10) Uiso 1 d . . 
C116 C 0.0547(3) 0.2460(2) 0.2979(2) 0.0486(7) Uani 1 d . . 
H116 H 0.1045(23) 0.2424(14) 0.3582(19) 0.046(8) Uiso 1 d . . 
C121 C 0.1919(3) 0.09385(14) 0.3051(2) 0.0425(7) Uani 1 d . . 
C122 C 0.0855(3) 0.0649(2) 0.2889(2) 0.0560(9) Uani 1 d . . 
H122 H 0.0252(26) 0.0850(15) 0.2524(20) 0.052(9) Uiso 1 d . . 
C123 C 0.0676(5) 0.0040(2) 0.3285(3) 0.0770(13) Uani 1 d . . 
H123 H -0.0057(33) -0.0061(19) 0.3155(25) 0.079(13) Uiso 1 d . . 
C124 C 0.1550(5) -0.0261(2) 0.3865(3) 0.0875(15) Uani 1 d . . 
H124 H 0.1497(39) -0.0627(22) 0.4181(30) 0.113(16) Uiso 1 d . . 
C125 C 0.2606(5) 0.0032(3) 0.4069(4) 0.109(2) Uani 1 d . . 
H125 H 0.3332(48) -0.0191(29) 0.4461(36) 0.164(22) Uiso 1 d . . 
C126 C 0.2801(3) 0.0625(2) 0.3657(3) 0.0801(13) Uani 1 d . . 
H126 H 0.3527(34) 0.0812(18) 0.3740(25) 0.085(13) Uiso 1 d . . 
C12 C 0.3270(3) 0.2174(2) 0.3243(2) 0.0421(7) Uani 1 d . . 
H12A H 0.2937(23) 0.2422(14) 0.3606(18) 0.044(8) Uiso 1 d . . 
H12B H 0.3769(26) 0.1859(16) 0.3595(20) 0.058(9) Uiso 1 d . . 
C21 C 0.3907(3) 0.2621(2) 0.2733(2) 0.0427(7) Uani 1 d . . 
H21A H 0.4545(24) 0.2847(15) 0.3105(18) 0.047(8) Uiso 1 d . . 
H21B H 0.3404(26) 0.2954(15) 0.2393(20) 0.057(9) Uiso 1 d . . 
P2 P 0.43653(5) 0.20722(4) 0.19401(4) 0.0336(2) Uani 1 d . . 
C211 C 0.5582(2) 0.16020(14) 0.2584(2) 0.0381(6) Uani 1 d . . 
C212 C 0.5484(3) 0.0920(2) 0.2755(2) 0.0450(7) Uani 1 d . . 
H212 H 0.4833(26) 0.0721(14) 0.2537(19) 0.046(9) Uiso 1 d . . 
C213 C 0.6403(3) 0.0548(2) 0.3215(2) 0.0567(8) Uani 1 d . . 
H213 H 0.6356(29) 0.0055(17) 0.3310(22) 0.071(11) Uiso 1 d . . 
C214 C 0.7434(3) 0.0869(2) 0.3518(2) 0.0671(11) Uani 1 d . . 
H214 H 0.8102(29) 0.0644(15) 0.3805(21) 0.062(10) Uiso 1 d . . 
C215 C 0.7553(3) 0.1540(2) 0.3376(2) 0.0662(10) Uani 1 d . . 
H215 H 0.8179(29) 0.1787(17) 0.3616(22) 0.070(11) Uiso 1 d . . 
C216 C 0.6633(3) 0.1919(2) 0.2907(2) 0.0521(8) Uani 1 d . . 
H216 H 0.6659(25) 0.2395(16) 0.2799(20) 0.054(9) Uiso 1 d . . 
C221 C 0.4986(2) 0.26278(14) 0.1256(2) 0.0376(6) Uani 1 d . . 
C222 C 0.5674(2) 0.2364(2) 0.0737(2) 0.0423(7) Uani 1 d . . 
H222 H 0.5808(23) 0.1890(15) 0.0730(18) 0.045(8) Uiso 1 d . . 
C223 C 0.6084(3) 0.2769(2) 0.0167(2) 0.0480(7) Uani 1 d . . 
H223 H 0.6489(27) 0.2559(16) -0.0240(22) 0.065(10) Uiso 1 d . . 
C224 C 0.5821(3) 0.3442(2) 0.0107(2) 0.0571(9) Uani 1 d . . 
H224 H 0.6070(30) 0.3706(18) -0.0326(24) 0.079(11) Uiso 1 d . . 
C225 C 0.5146(3) 0.3715(2) 0.0622(3) 0.0649(10) Uani 1 d . . 
H225 H 0.4940(29) 0.4152(18) 0.0567(22) 0.067(10) Uiso 1 d . . 
C226 C 0.4728(3) 0.3313(2) 0.1187(2) 0.0551(8) Uani 1 d . . 
H226 H 0.4344(26) 0.3499(15) 0.1548(20) 0.052(9) Uiso 1 d . . 
S1 S 0.13636(5) 0.07355(3) 0.08676(4) 0.0360(2) Uani 1 d . . 
S2 S 0.42172(5) 0.08464(3) 0.06957(4) 0.0356(2) Uani 1 d . . 
Fe Fe 0.28298(3) 0.00083(2) 0.06767(2) 0.03722(10) Uani 1 d . . 
S3 S 0.26257(7) -0.10581(4) 0.01398(6) 0.0543(2) Uani 1 d . . 
N4 N 0.2249(2) 0.03256(11) -0.07423(13) 0.0362(5) Uani 1 d . . 
C14 C 0.0659(2) 0.0912(2) -0.0270(2) 0.0408(7) Uani 1 d . . 
H14A H -0.0164(2) 0.0899(2) -0.0331(2) 0.058(18) Uiso 0.50 calc PR 1 
H14B H 0.0860(2) 0.1367(2) -0.0414(2) 0.046(16) Uiso 0.50 calc PR 1 
H14C H 0.0073(2) 0.0572(2) -0.0474(2) 0.046(16) Uiso 0.50 calc PR 2 
H14D H 0.0285(2) 0.1350(2) -0.0305(2) 0.060(19) Uiso 0.50 calc PR 2 
C24 C 0.4021(2) 0.1028(2) -0.0463(2) 0.0424(7) Uani 1 d . . 
H24A H 0.4285(2) 0.1484(2) -0.0538(2) 0.028(13) Uiso 0.50 calc PR 1 
H24B H 0.4477(2) 0.0715(2) -0.0718(2) 0.081(23) Uiso 0.50 calc PR 1 
H24C H 0.3625(2) 0.1458(2) -0.0591(2) 0.046(17) Uiso 0.50 calc PR 2 
H24D H 0.4767(2) 0.1074(2) -0.0598(2) 0.009(10) Uiso 0.50 calc PR 2 
C34 C 0.2222(4) -0.0910(2) -0.1032(2) 0.0661(10) Uani 1 d . . 
H34A H 0.2628(4) -0.1230(2) -0.1319(2) 0.087(26) Uiso 0.50 calc PR 1 
H34B H 0.1408(4) -0.0998(2) -0.1238(2) 0.094(28) Uiso 0.50 calc PR 1 
H34C H 0.2901(4) -0.0948(2) -0.1266(2) 0.110(33) Uiso 0.50 calc PR 2 
H34D H 0.1691(4) -0.1262(2) -0.1301(2) 0.065(20) Uiso 0.50 calc PR 2 
C41 C 0.0957(5) 0.0445(3) -0.0889(4) 0.0429(13) Uani 0.50 d P 1 
H41A H 0.0668(5) 0.0619(3) -0.1476(4) 0.027(13) Uiso 0.50 calc PR 1 
H41B H 0.0582(5) 0.0014(3) -0.0848(4) 0.048(17) Uiso 0.50 calc PR 1 
C42 C 0.2761(5) 0.0963(3) -0.0939(3) 0.0443(14) Uani 0.50 d P 1 
H42A H 0.2335(5) 0.1339(3) -0.0773(3) 0.095(32) Uiso 0.50 calc PR 1 
H42B H 0.2699(5) 0.0991(3) -0.1565(3) 0.055(17) Uiso 0.50 calc PR 1 
C43 C 0.2462(7) -0.0230(4) -0.1284(4) 0.053(2) Uani 0.50 d P 1 
H43A H 0.2012(7) -0.0152(4) -0.1873(4) 0.058(25) Uiso 0.50 calc PR 1 
H43B H 0.3263(7) -0.0213(4) -0.1309(4) 0.058(19) Uiso 0.50 calc PR 1 
C41B C 0.1511(4) 0.0911(3) -0.0876(3) 0.0346(11) Uani 0.50 d P 2 
H41C H 0.1084(4) 0.0922(3) -0.1481(3) 0.030(13) Uiso 0.50 calc PR 2 
H41D H 0.1978(4) 0.1318(3) -0.0769(3) 0.023(14) Uiso 0.50 calc PR 2 
C42B C 0.3356(4) 0.0494(3) -0.1039(3) 0.0384(12) Uani 0.50 d P 2 
H42C H 0.3820(4) 0.0088(3) -0.1013(3) 0.036(14) Uiso 0.50 calc PR 2 
H42D H 0.3164(4) 0.0652(3) -0.1640(3) 0.044(15) Uiso 0.50 calc PR 2 
C43B C 0.1703(6) -0.0266(3) -0.1272(4) 0.0447(14) Uani 0.50 d P 2 
H43C H 0.0909(6) -0.0290(3) -0.1232(4) 0.063(19) Uiso 0.50 calc PR 2 
H43D H 0.1706(6) -0.0181(3) -0.1880(4) 0.095(36) Uiso 0.50 calc PR 2 
N5 N 0.3291(3) -0.03087(14) 0.1725(2) 0.0602(7) Uani 1 d . . 
O5A O 0.4130(9) -0.0664(6) 0.2166(7) 0.062(3) Uiso 0.25 d P . 
O5B O 0.3005(10) -0.0736(6) 0.2259(7) 0.061(3) Uiso 0.25 d P . 
O5C O 0.3545(12) -0.0845(6) 0.2132(7) 0.055(3) Uiso 0.25 d P . 
O5D O 0.3603(15) -0.0611(7) 0.2362(9) 0.072(4) Uiso 0.25 d P . 
N61 N 0.1984(4) 0.0961(2) 0.6652(3) 0.1114(14) Uani 1 d . . 
C62 C 0.1450(4) 0.1062(2) 0.5983(3) 0.0718(11) Uani 1 d . . 
C63 C 0.0728(5) 0.1194(3) 0.5132(3) 0.0862(14) Uani 1 d . . 
H63A H 0.0421(54) 0.0802(31) 0.4904(41) 0.165(25) Uiso 1 d . . 
H63B H 0.1320(62) 0.1189(34) 0.4806(48) 0.205(33) Uiso 1 d . . 
H63C H 0.0244(68) 0.1550(41) 0.5056(54) 0.248(45) Uiso 1 d . . 

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 0.0267(2) 0.0381(2) 0.0269(2) -0.00149(14) 0.00798(12) -0.00278(14) 
Cl 0.0456(4) 0.0444(4) 0.0371(3) 0.0046(3) 0.0085(3) 0.0009(3) 
P1 0.0302(3) 0.0414(4) 0.0290(3) -0.0004(3) 0.0100(3) -0.0015(3) 
C111 0.0311(13) 0.0389(15) 0.0388(14) -0.0018(12) 0.0132(11) -0.0057(11) 
C112 0.039(2) 0.055(2) 0.043(2) -0.0011(14) 0.0160(13) 0.0045(13) 
C113 0.041(2) 0.065(2) 0.059(2) 0.010(2) 0.006(2) 0.009(2) 
C114 0.040(2) 0.047(2) 0.081(3) 0.000(2) 0.021(2) 0.0073(15) 
C115 0.048(2) 0.063(2) 0.068(2) -0.018(2) 0.023(2) 0.002(2) 
C116 0.043(2) 0.057(2) 0.046(2) -0.0103(15) 0.0126(14) -0.0003(14) 
C121 0.051(2) 0.045(2) 0.0369(15) 0.0026(13) 0.0227(13) 0.0028(14) 
C122 0.066(2) 0.060(2) 0.041(2) 0.005(2) 0.011(2) -0.020(2) 
C123 0.103(4) 0.078(3) 0.052(2) 0.000(2) 0.022(2) -0.041(3) 
C124 0.133(5) 0.051(2) 0.094(3) 0.026(2) 0.060(3) 0.009(3) 
C125 0.086(3) 0.100(4) 0.157(5) 0.077(4) 0.060(4) 0.040(3) 
C126 0.054(2) 0.082(3) 0.113(3) 0.052(3) 0.037(2) 0.020(2) 
C12 0.0364(15) 0.060(2) 0.0308(14) -0.0071(14) 0.0096(12) -0.0023(14) 
C21 0.040(2) 0.049(2) 0.042(2) -0.0105(14) 0.0149(13) -0.0063(14) 
P2 0.0297(3) 0.0402(4) 0.0322(3) -0.0031(3) 0.0098(3) -0.0047(3) 
C211 0.0326(13) 0.054(2) 0.0280(13) -0.0014(12) 0.0078(11) -0.0031(12) 
C212 0.043(2) 0.056(2) 0.0358(15) -0.0008(14) 0.0075(13) -0.0010(15) 
C213 0.061(2) 0.062(2) 0.045(2) 0.003(2) 0.010(2) 0.016(2) 
C214 0.042(2) 0.105(3) 0.052(2) 0.009(2) 0.008(2) 0.023(2) 
C215 0.032(2) 0.103(3) 0.060(2) 0.010(2) 0.003(2) -0.008(2) 
C216 0.040(2) 0.070(2) 0.046(2) 0.006(2) 0.0074(14) -0.011(2) 
C221 0.0339(14) 0.043(2) 0.0345(14) -0.0035(12) 0.0059(11) -0.0093(12) 
C222 0.0373(15) 0.046(2) 0.046(2) 0.0012(14) 0.0146(13) -0.0037(13) 
C223 0.044(2) 0.061(2) 0.043(2) 0.0009(15) 0.0161(14) -0.0115(15) 
C224 0.065(2) 0.060(2) 0.049(2) 0.008(2) 0.020(2) -0.018(2) 
C225 0.085(3) 0.038(2) 0.078(3) 0.005(2) 0.032(2) -0.008(2) 
C226 0.064(2) 0.042(2) 0.066(2) -0.005(2) 0.029(2) -0.010(2) 
S1 0.0296(3) 0.0448(4) 0.0348(3) -0.0039(3) 0.0101(3) -0.0049(3) 
S2 0.0282(3) 0.0447(4) 0.0341(3) -0.0036(3) 0.0079(3) -0.0009(3) 
Fe 0.0343(2) 0.0395(2) 0.0378(2) 0.0000(2) 0.0080(2) -0.0002(2) 
S3 0.0581(5) 0.0404(4) 0.0650(5) -0.0049(4) 0.0151(4) 0.0010(4) 
N4 0.0346(12) 0.0415(12) 0.0328(11) -0.0056(10) 0.0085(9) -0.0005(10) 
C14 0.0272(14) 0.058(2) 0.0355(14) -0.0046(13) 0.0028(11) -0.0010(13) 
C24 0.0366(15) 0.058(2) 0.0359(15) -0.0044(13) 0.0148(12) -0.0070(14) 
C34 0.080(3) 0.051(2) 0.063(2) -0.020(2) 0.008(2) -0.006(2) 
C41 0.035(3) 0.058(4) 0.034(3) -0.005(3) 0.006(2) -0.002(3) 
C42 0.039(3) 0.068(4) 0.027(3) -0.002(3) 0.010(2) -0.007(3) 
C43 0.051(4) 0.063(4) 0.045(4) -0.014(3) 0.008(3) 0.005(4) 
C41B 0.031(3) 0.041(3) 0.028(3) -0.005(2) 0.000(2) 0.004(2) 
C42B 0.031(3) 0.052(3) 0.035(3) -0.006(3) 0.014(2) -0.001(3) 
C43B 0.038(3) 0.050(4) 0.043(4) -0.011(3) 0.003(3) -0.005(3) 
N5 0.076(2) 0.057(2) 0.0427(15) 0.0124(13) 0.0031(14) 0.0034(15) 
N61 0.123(4) 0.100(3) 0.102(3) 0.030(3) 0.009(3) -0.014(3) 
C62 0.089(3) 0.056(2) 0.075(3) 0.003(2) 0.028(2) -0.014(2) 
C63 0.107(4) 0.083(3) 0.072(3) -0.015(3) 0.026(3) -0.028(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 
Ni P2 2.1750(7) . ? 
Ni P1 2.1892(7) . ? 
Ni S1 2.3065(7) . ? 
Ni S2 2.3577(7) . ? 
Ni Cl 2.4334(8) . ? 
P1 C121 1.818(3) . ? 
P1 C111 1.829(3) . ? 
P1 C12 1.839(3) . ? 
C111 C112 1.371(4) . ? 
C111 C116 1.392(4) . ? 
C112 C113 1.386(4) . ? 
C112 H112 0.86(3) . ? 
C113 C114 1.366(5) . ? 
C113 H113 0.95(3) . ? 
C114 C115 1.374(5) . ? 
C114 H114 0.90(3) . ? 
C115 C116 1.381(4) . ? 
C115 H115 0.98(3) . ? 
C116 H116 1.00(3) . ? 
C121 C122 1.367(4) . ? 
C121 C126 1.393(5) . ? 
C122 C123 1.392(5) . ? 
C122 H122 0.90(3) . ? 
C123 C124 1.356(6) . ? 
C123 H123 0.88(4) . ? 
C124 C125 1.361(7) . ? 
C124 H124 0.89(4) . ? 
C125 C126 1.383(5) . ? 
C125 H125 1.04(5) . ? 
C126 H126 0.93(4) . ? 
C12 C21 1.512(4) . ? 
C12 H12A 0.91(3) . ? 
C12 H12B 0.95(3) . ? 
C21 P2 1.827(3) . ? 
C21 H21A 0.96(3) . ? 
C21 H21B 0.97(3) . ? 
P2 C221 1.811(3) . ? 
P2 C211 1.824(3) . ? 
C211 C212 1.381(4) . ? 
C211 C216 1.394(4) . ? 
C212 C213 1.381(4) . ? 
C212 H212 0.87(3) . ? 
C213 C214 1.372(5) . ? 
C213 H213 0.99(3) . ? 
C214 C215 1.355(6) . ? 
C214 H214 0.93(3) . ? 
C215 C216 1.393(5) . ? 
C215 H215 0.90(3) . ? 
C216 H216 0.96(3) . ? 
C221 C226 1.385(4) . ? 
C221 C222 1.388(4) . ? 
C222 C223 1.374(4) . ? 
C222 H222 0.95(3) . ? 
C223 C224 1.362(5) . ? 
C223 H223 0.98(3) . ? 
C224 C225 1.379(5) . ? 
C224 H224 0.96(4) . ? 
C225 C226 1.368(5) . ? 
C225 H225 0.90(3) . ? 
C226 H226 0.89(3) . ? 
S1 C14 1.825(3) . ? 
S1 Fe 2.3405(8) . ? 
S2 C24 1.817(3) . ? 
S2 Fe 2.3397(8) . ? 
Fe N5 1.728(3) . ? 
Fe S3 2.2579(9) . ? 
Fe N4 2.265(2) . ? 
S3 C34 1.816(4) . ? 
N4 C41B 1.440(5) . ? 
N4 C43 1.447(7) . ? 
N4 C42 1.462(6) . ? 
N4 C43B 1.493(6) . ? 
N4 C41 1.531(6) . ? 
N4 C42B 1.540(5) . ? 
C14 C41 1.442(6) . ? 
C14 C41B 1.549(6) . ? 
C14 H14A 0.97 . ? 
C14 H14B 0.97 . ? 
C14 H14C 0.97 . ? 
C14 H14D 0.97 . ? 
C24 C42B 1.493(6) . ? 
C24 C42 1.527(6) . ? 
C24 H24A 0.97 . ? 
C24 H24B 0.97 . ? 
C24 H24C 0.97 . ? 
C24 H24D 0.97 . ? 
C34 C43B 1.426(7) . ? 
C34 C43 1.446(8) . ? 
C34 H34A 0.97 . ? 
C34 H34B 0.97 . ? 
C34 H34C 0.97 . ? 
C34 H34D 0.97 . ? 
C41 H41A 0.97 . ? 
C41 H41B 0.97 . ? 
C42 H42A 0.97 . ? 
C42 H42B 0.97 . ? 
C43 H43A 0.97 . ? 
C43 H43B 0.97 . ? 
C41B H41C 0.97 . ? 
C41B H41D 0.97 . ? 
C42B H42C 0.97 . ? 
C42B H42D 0.97 . ? 
C43B H43C 0.97 . ? 
C43B H43D 0.97 . ? 
N5 O5D 1.151(12) . ? 
N5 O5C 1.236(11) . ? 
N5 O5A 1.289(10) . ? 
N5 O5B 1.291(10) . ? 
O5A O5D 0.77(2) . ? 
O5A O5C 0.776(14) . ? 
O5A O5B 1.396(15) . ? 
O5B O5D 0.74(2) . ? 
O5B O5C 0.751(14) . ? 
O5C O5D 0.58(2) . ? 
N61 C62 1.115(5) . ? 
C62 C63 1.439(7) . ? 
C63 H63A 0.89(6) . ? 
C63 H63B 0.97(8) . ? 
C63 H63C 0.90(8) . ? 

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 
P2 Ni P1 85.91(3) . . ? 
P2 Ni S1 169.98(3) . . ? 
P1 Ni S1 86.54(3) . . ? 
P2 Ni S2 85.78(3) . . ? 
P1 Ni S2 147.97(3) . . ? 
S1 Ni S2 97.22(3) . . ? 
P2 Ni Cl 89.10(3) . . ? 
P1 Ni Cl 107.25(3) . . ? 
S1 Ni Cl 99.43(3) . . ? 
S2 Ni Cl 103.49(3) . . ? 
C121 P1 C111 103.89(12) . . ? 
C121 P1 C12 105.05(14) . . ? 
C111 P1 C12 105.06(14) . . ? 
C121 P1 Ni 115.14(9) . . ? 
C111 P1 Ni 117.20(9) . . ? 
C12 P1 Ni 109.38(9) . . ? 
C112 C111 C116 118.8(3) . . ? 
C112 C111 P1 121.3(2) . . ? 
C116 C111 P1 119.9(2) . . ? 
C111 C112 C113 120.8(3) . . ? 
C111 C112 H112 120.8(18) . . ? 
C113 C112 H112 118.1(18) . . ? 
C114 C113 C112 120.2(3) . . ? 
C114 C113 H113 122.5(17) . . ? 
C112 C113 H113 117.3(18) . . ? 
C113 C114 C115 119.5(3) . . ? 
C113 C114 H114 120.5(23) . . ? 
C115 C114 H114 119.8(23) . . ? 
C114 C115 C116 120.6(3) . . ? 
C114 C115 H115 120.2(20) . . ? 
C116 C115 H115 119.2(20) . . ? 
C115 C116 C111 120.0(3) . . ? 
C115 C116 H116 119.4(16) . . ? 
C111 C116 H116 120.5(16) . . ? 
C122 C121 C126 118.1(3) . . ? 
C122 C121 P1 121.6(2) . . ? 
C126 C121 P1 120.2(2) . . ? 
C121 C122 C123 120.7(4) . . ? 
C121 C122 H122 120.6(20) . . ? 
C123 C122 H122 118.7(20) . . ? 
C124 C123 C122 120.2(4) . . ? 
C124 C123 H123 129.3(26) . . ? 
C122 C123 H123 109.9(26) . . ? 
C123 C124 C125 120.4(4) . . ? 
C123 C124 H124 126.0(31) . . ? 
C125 C124 H124 113.3(31) . . ? 
C124 C125 C126 119.8(5) . . ? 
C124 C125 H125 124.5(32) . . ? 
C126 C125 H125 115.2(32) . . ? 
C125 C126 C121 120.8(4) . . ? 
C125 C126 H126 121.7(24) . . ? 
C121 C126 H126 117.4(24) . . ? 
C21 C12 P1 107.6(2) . . ? 
C21 C12 H12A 111.5(17) . . ? 
P1 C12 H12A 112.2(17) . . ? 
C21 C12 H12B 111.3(18) . . ? 
P1 C12 H12B 106.9(18) . . ? 
H12A C12 H12B 107.3(25) . . ? 
C12 C21 P2 106.5(2) . . ? 
C12 C21 H21A 112.2(17) . . ? 
P2 C21 H21A 111.6(17) . . ? 
C12 C21 H21B 111.2(18) . . ? 
P2 C21 H21B 105.8(18) . . ? 
H21A C21 H21B 109.3(24) . . ? 
C221 P2 C211 104.53(12) . . ? 
C221 P2 C21 106.01(13) . . ? 
C211 P2 C21 104.50(14) . . ? 
C221 P2 Ni 117.47(8) . . ? 
C211 P2 Ni 115.48(9) . . ? 
C21 P2 Ni 107.74(10) . . ? 
C212 C211 C216 118.4(3) . . ? 
C212 C211 P2 120.6(2) . . ? 
C216 C211 P2 120.9(2) . . ? 
C211 C212 C213 121.7(3) . . ? 
C211 C212 H212 118.2(19) . . ? 
C213 C212 H212 120.0(19) . . ? 
C214 C213 C212 118.8(4) . . ? 
C214 C213 H213 118.7(20) . . ? 
C212 C213 H213 122.4(21) . . ? 
C215 C214 C213 120.9(3) . . ? 
C215 C214 H214 115.6(20) . . ? 
C213 C214 H214 123.4(20) . . ? 
C214 C215 C216 120.7(3) . . ? 
C214 C215 H215 124.6(22) . . ? 
C216 C215 H215 114.3(22) . . ? 
C215 C216 C211 119.3(3) . . ? 
C215 C216 H216 124.6(19) . . ? 
C211 C216 H216 116.1(19) . . ? 
C226 C221 C222 118.2(3) . . ? 
C226 C221 P2 121.5(2) . . ? 
C222 C221 P2 120.2(2) . . ? 
C223 C222 C221 121.0(3) . . ? 
C223 C222 H222 118.6(17) . . ? 
C221 C222 H222 120.2(17) . . ? 
C224 C223 C222 120.0(3) . . ? 
C224 C223 H223 120.7(19) . . ? 
C222 C223 H223 118.9(19) . . ? 
C223 C224 C225 119.8(3) . . ? 
C223 C224 H224 118.3(21) . . ? 
C225 C224 H224 121.7(21) . . ? 
C226 C225 C224 120.5(3) . . ? 
C226 C225 H225 119.1(23) . . ? 
C224 C225 H225 120.3(23) . . ? 
C225 C226 C221 120.5(3) . . ? 
C225 C226 H226 119.7(20) . . ? 
C221 C226 H226 119.5(20) . . ? 
C14 S1 Ni 109.24(10) . . ? 
C14 S1 Fe 100.50(9) . . ? 
Ni S1 Fe 81.11(3) . . ? 
C24 S2 Fe 101.48(9) . . ? 
C24 S2 Ni 111.11(10) . . ? 
Fe S2 Ni 80.07(3) . . ? 
N5 Fe S3 90.13(10) . . ? 
N5 Fe N4 174.67(11) . . ? 
S3 Fe N4 84.69(6) . . ? 
N5 Fe S2 99.97(10) . . ? 
S3 Fe S2 132.69(3) . . ? 
N4 Fe S2 82.73(6) . . ? 
N5 Fe S1 100.61(10) . . ? 
S3 Fe S1 126.77(3) . . ? 
N4 Fe S1 83.54(6) . . ? 
S2 Fe S1 96.78(3) . . ? 
C34 S3 Fe 102.11(11) . . ? 
C43 N4 C42 112.8(4) . . ? 
C41B N4 C43B 111.7(4) . . ? 
C43 N4 C41 109.7(4) . . ? 
C42 N4 C41 107.2(4) . . ? 
C41B N4 C42B 109.0(3) . . ? 
C43B N4 C42B 107.3(4) . . ? 
C41B N4 Fe 113.9(2) . . ? 
C43 N4 Fe 108.3(3) . . ? 
C42 N4 Fe 113.4(2) . . ? 
C43B N4 Fe 109.2(3) . . ? 
C41 N4 Fe 105.1(2) . . ? 
C42B N4 Fe 105.5(2) . . ? 
C41 C14 S1 114.1(3) . . ? 
C41B C14 S1 112.4(2) . . ? 
C41 C14 H14A 108.7(2) . . ? 
S1 C14 H14A 108.73(9) . . ? 
C41 C14 H14B 108.7(3) . . ? 
S1 C14 H14B 108.73(10) . . ? 
H14A C14 H14B 107.6 . . ? 
C41B C14 H14C 109.1(2) . . ? 
S1 C14 H14C 109.13(9) . . ? 
C41B C14 H14D 109.1(2) . . ? 
S1 C14 H14D 109.13(10) . . ? 
H14C C14 H14D 107.9 . . ? 
C42B C24 S2 113.3(3) . . ? 
C42 C24 S2 111.0(2) . . ? 
C42 C24 H24A 109.4(3) . . ? 
S2 C24 H24A 109.44(10) . . ? 
C42 C24 H24B 109.4(3) . . ? 
S2 C24 H24B 109.44(10) . . ? 
H24A C24 H24B 108.0 . . ? 
C42B C24 H24C 108.9(3) . . ? 
S2 C24 H24C 108.92(10) . . ? 
C42B C24 H24D 108.9(2) . . ? 
S2 C24 H24D 108.92(9) . . ? 
H24C C24 H24D 107.7 . . ? 
C43B C34 S3 114.1(3) . . ? 
C43 C34 S3 113.8(3) . . ? 
C43 C34 H34A 108.8(3) . . ? 
S3 C34 H34A 108.80(12) . . ? 
C43 C34 H34B 108.8(3) . . ? 
S3 C34 H34B 108.80(14) . . ? 
H34A C34 H34B 107.7 . . ? 
C43B C34 H34C 108.7(3) . . ? 
S3 C34 H34C 108.72(14) . . ? 
C43B C34 H34D 108.7(3) . . ? 
S3 C34 H34D 108.72(12) . . ? 
H34C C34 H34D 107.6 . . ? 
C14 C41 N4 113.3(4) . . ? 
C14 C41 H41A 108.9(3) . . ? 
N4 C41 H41A 108.9(2) . . ? 
C14 C41 H41B 108.9(3) . . ? 
N4 C41 H41B 108.9(3) . . ? 
H41A C41 H41B 107.7 . . ? 
N4 C42 C24 112.6(4) . . ? 
N4 C42 H42A 109.1(3) . . ? 
C24 C42 H42A 109.1(3) . . ? 
N4 C42 H42B 109.1(2) . . ? 
C24 C42 H42B 109.1(2) . . ? 
H42A C42 H42B 107.8 . . ? 
C34 C43 N4 117.9(5) . . ? 
C34 C43 H43A 107.8(3) . . ? 
N4 C43 H43A 107.8(3) . . ? 
C34 C43 H43B 107.8(4) . . ? 
N4 C43 H43B 107.8(3) . . ? 
H43A C43 H43B 107.2 . . ? 
N4 C41B C14 112.3(4) . . ? 
N4 C41B H41C 109.1(2) . . ? 
C14 C41B H41C 109.1(2) . . ? 
N4 C41B H41D 109.1(2) . . ? 
C14 C41B H41D 109.1(2) . . ? 
H41C C41B H41D 107.9 . . ? 
C24 C42B N4 110.2(3) . . ? 
C24 C42B H42C 109.6(3) . . ? 
N4 C42B H42C 109.6(2) . . ? 
C24 C42B H42D 109.6(2) . . ? 
N4 C42B H42D 109.6(2) . . ? 
H42C C42B H42D 108.1 . . ? 
C34 C43B N4 116.1(4) . . ? 
C34 C43B H43C 108.2(3) . . ? 
N4 C43B H43C 108.2(3) . . ? 
C34 C43B H43D 108.2(3) . . ? 
N4 C43B H43D 108.2(3) . . ? 
H43C C43B H43D 107.4 . . ? 
O5D N5 O5C 27.8(8) . . ? 
O5D N5 O5A 36.3(8) . . ? 
O5C N5 O5A 35.7(6) . . ? 
O5D N5 O5B 34.7(8) . . ? 
O5C N5 O5B 34.5(6) . . ? 
O5A N5 O5B 65.5(7) . . ? 
O5D N5 Fe 169.8(7) . . ? 
O5C N5 Fe 142.0(6) . . ? 
O5A N5 Fe 138.4(6) . . ? 
O5B N5 Fe 141.4(6) . . ? 
O5D O5A O5C 44.0(13) . . ? 
O5D O5A N5 62.1(12) . . ? 
O5C O5A N5 68.4(11) . . ? 
O5D O5A O5B 21.9(13) . . ? 
O5C O5A O5B 23.5(11) . . ? 
N5 O5A O5B 57.3(6) . . ? 
O5D O5B O5C 45.8(14) . . ? 
O5D O5B N5 62.3(13) . . ? 
O5C O5B N5 68.7(12) . . ? 
O5D O5B O5A 22.9(14) . . ? 
O5C O5B O5A 24.4(12) . . ? 
N5 O5B O5A 57.1(6) . . ? 
O5D O5C O5B 66.1(22) . . ? 
O5D O5C O5A 67.5(23) . . ? 
O5B O5C O5A 132.1(21) . . ? 
O5D O5C N5 67.9(18) . . ? 
O5B O5C N5 76.8(12) . . ? 
O5A O5C N5 75.8(12) . . ? 
O5C O5D O5B 68.2(23) . . ? 
O5C O5D O5A 68.5(23) . . ? 
O5B O5D O5A 135.2(26) . . ? 
O5C O5D N5 84.2(19) . . ? 
O5B O5D N5 83.1(15) . . ? 
O5A O5D N5 81.6(14) . . ? 
N61 C62 C63 178.1(5) . . ? 
C62 C63 H63A 108.6(40) . . ? 
C62 C63 H63B 97.7(43) . . ? 
H63A C63 H63B 93.7(51) . . ? 
C62 C63 H63C 119.7(54) . . ? 
H63A C63 H63C 115.3(63) . . ? 
H63B C63 H63C 117.7(60) . . ? 

_refine_diff_density_max    0.349 
_refine_diff_density_min   -0.265 
_refine_diff_density_rms    0.061 

#===END