Supplementary Material (ESI) for Dalton Transactions
This journal is © The Royal Society of Chemistry 2001

data_steve6 

_database_code_CSD	168689


_journal_coden_Cambridge      186

_publ_requested_journal       'Dalton Transactions'

loop_
_publ_author_name
'Davies, Sian C.'
'Evans, D.'
'Henderson, R.'
'Hughes, David L.'
'Longhurst, Steven'

_publ_contact_author_name     	'Dr R Henderson'  
_publ_contact_author_address 
;
Department of Chemistry
Bedson Building
University of Newcastle
NEWCASTLE UPON TYNE
NE1 7RU
UK
;

_publ_contact_author_email       'r.a.henderson@ncl.ac.uk'

_publ_section_title		
;
Proton Affinity of [Fe4S4{SCH2CH(OH)Me}4[2- in Methanol:  Relevance
to Hydrogen Bonding of Fe-S Clusters in Proteins
;

_audit_creation_method            SHELXL 
_chemical_name_systematic 
; 
? 
; 
_chemical_name_common             steve6
_chemical_formula_moiety          '2(C4 H12 N), C12 H28 Fe4 O4 S8'
_chemical_formula_structural      '(NMe4)2[Fe4S4{SCH2CH(OH)Me}4]'
_chemical_formula_analytical      ? 
_chemical_formula_sum             'C20 H52 Fe4 N2 O4 S8' 
_chemical_formula_weight          864.52 
_chemical_melting_point           ? 
_chemical_compound_source         ? 

loop_ 
_atom_type_symbol 
_atom_type_description 
_atom_type_scat_dispersion_real 
_atom_type_scat_dispersion_imag 
_atom_type_scat_source 
'C'  'C'   0.0033   0.0016 
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
'H'  'H'   0.0000   0.0000 
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
'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' 
'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' 

_symmetry_cell_setting            monoclinic
_symmetry_space_group_name_H-M    'P21/a'  #(equiv. to no. 14)

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

_cell_length_a                    19.004(4) 
_cell_length_b                    10.715(4) 
_cell_length_c                    19.586(8) 
_cell_angle_alpha                 90.00
_cell_angle_beta                  101.37(3) 
_cell_angle_gamma                 90.00
_cell_volume                      3910.1(23) 
_cell_formula_units_Z             4 
_cell_measurement_temperature     293(1) 
_cell_measurement_reflns_used     25
_cell_measurement_theta_min       8
_cell_measurement_theta_max       10 

_exptl_crystal_description        'very thin plates'
_exptl_crystal_colour             black
_exptl_crystal_size_max           0.57
_exptl_crystal_size_mid           0.55
_exptl_crystal_size_min           0.02
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.469 
_exptl_crystal_density_method     ? 
_exptl_crystal_F_000              1800 
_exptl_absorpt_coefficient_mu     1.908 
_exptl_absorpt_correction_type    psi-scan
_exptl_absorpt_correction_T_min   0.107
_exptl_absorpt_correction_T_max   0.165

_exptl_special_details 
; 
? 
; 

_diffrn_ambient_temperature       293(1) 
_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_%         8.3
_diffrn_reflns_number             3794
_diffrn_reflns_av_R_equivalents   0.055
_diffrn_reflns_av_sigmaI/netI     0.1072 
_diffrn_reflns_limit_h_min        0
_diffrn_reflns_limit_h_max        18 
_diffrn_reflns_limit_k_min        0 
_diffrn_reflns_limit_k_max        10 
_diffrn_reflns_limit_l_min        -18 
_diffrn_reflns_limit_l_max        18 
_diffrn_reflns_theta_min          2.1 
_diffrn_reflns_theta_max          20.0 
_reflns_number_total              3641 
_reflns_number_observed           1670 

_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. 

Disorder was identified in two of the thiolate ligands and in one of the 
cations.  Hydrogen atoms were included in idealised positions in the fully 
ordered groups.  The non-hydrogen atoms (except those which are disordered)

were refined with anisotropic parameters, and the hydrogen-atom U(iso)
values 
were set to ride on the U(eq) values of the parent carbon atoms.

; 

_refine_ls_structure_factor_coef  Fsqd  
_refine_ls_matrix_type            full 
_refine_ls_weighting_scheme 
'calc w=1/[\s^2^(Fo^2^)+(0.1602P)^2^] 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     constr
_refine_ls_extinction_method      none 
_refine_ls_extinction_coef        ? 
_refine_ls_number_reflns          3641 
_refine_ls_number_parameters      349 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.1512 
_refine_ls_R_factor_obs           0.0897 
_refine_ls_wR_factor_all          0.2714 
_refine_ls_wR_factor_obs          0.2111 
_refine_ls_goodness_of_fit_all    0.966 
_refine_ls_goodness_of_fit_obs    1.150 
_refine_ls_restrained_S_all       0.966 
_refine_ls_restrained_S_obs       1.150 
_refine_ls_shift/esd_max          -0.005 
_refine_ls_shift/esd_mean         0.001 

loop_ 
_atom_site_label 
_atom_site_type_symbol 
_atom_site_fract_x 
_atom_site_fract_y 
_atom_site_fract_z 
_atom_site_U_iso_or_equiv 
_atom_site_thermal_displace_type 
_atom_site_occupancy 
_atom_site_calc_flag 
_atom_site_refinement_flags 
_atom_site_disorder_group 
Fe1 Fe 0.23677(13) 0.0393(2) 0.27556(14) 0.0728(9) Uani 1 d . . 
Fe2 Fe 0.09314(13) 0.0763(3) 0.26091(13) 0.0708(9) Uani 1 d . . 
Fe3 Fe 0.14584(14) -0.1590(2) 0.25327(14) 0.0715(9) Uani 1 d . . 
Fe4 Fe 0.14911(14) 0.0103(2) 0.14780(13) 0.0704(9) Uani 1 d . . 
S11 S 0.0494(2) -0.0696(5) 0.1804(2) 0.0776(15) Uani 1 d . . 
S22 S 0.2410(3) -0.1169(5) 0.2002(3) 0.0782(15) Uani 1 d . . 
S33 S 0.1696(3) 0.1898(5) 0.2085(3) 0.080(2) Uani 1 d . . 
S44 S 0.1652(3) -0.0350(5) 0.3476(2) 0.081(2) Uani 1 d . . 
S1 S 0.3432(3) 0.1037(7) 0.3364(4) 0.118(2) Uani 1 d . . 
S2 S 0.0090(3) 0.1906(6) 0.2971(3) 0.107(2) Uani 1 d . . 
S3 S 0.1283(4) -0.3587(5) 0.2781(3) 0.108(2) Uani 1 d . . 
S4 S 0.1464(3) 0.0241(6) 0.0325(3) 0.098(2) Uani 1 d . . 
C11 C 0.3204(18) 0.1758(38) 0.4116(16) 0.182(15) Uani 1 d . . 
C12 C 0.2979(28) 0.3051(54) 0.3967(27) 0.131(16) Uiso 0.60 d P . 
C12X C 0.3401(38) 0.2787(77) 0.4463(38) 0.124(21) Uiso 0.40 d P . 
C13 C 0.3145(23) 0.3748(44) 0.4710(24) 0.281(26) Uani 1 d . . 
O14 O 0.3666(20) 0.3579(27) 0.3797(17) 0.296(16) Uani 1 d . . 
C21 C 0.0578(22) 0.3237(22) 0.3448(17) 0.168(15) Uani 1 d . . 
C22 C 0.1003(31) 0.2991(54) 0.4090(30) 0.103(31) Uiso 0.47(9) d P . 
C22X C 0.0414(37) 0.3631(67) 0.4084(32) 0.145(35) Uiso 0.53(9) d P . 
C23 C 0.1039(20) 0.4424(28) 0.4489(15) 0.172(12) Uani 1 d . . 
O24 O 0.0773(33) 0.2111(56) 0.4456(23) 0.122(30) Uiso 0.37(8) d P . 
O24X O 0.0275(30) 0.2653(42) 0.4503(19) 0.186(22) Uiso 0.63(8) d P . 
C31 C 0.0804(13) -0.4230(21) 0.1983(11) 0.113(8) Uani 1 d . . 
H31A H 0.0717(13) -0.5105(21) 0.2062(11) 0.135 Uiso 1 calc R . 
H31B H 0.0340(13) -0.3822(21) 0.1872(11) 0.135 Uiso 1 calc R . 
C32 C 0.1137(12) -0.4141(22) 0.1371(12) 0.111(8) Uani 1 d . . 
H32 H 0.1204(12) -0.3250(22) 0.1291(12) 0.133 Uiso 1 calc R . 
C33 C 0.1868(10) -0.4743(21) 0.1441(13) 0.120(8) Uani 1 d . . 
H33A H 0.2168(29) -0.4487(121) 0.1872(42) 0.180 Uiso 1 calc R . 
H33B H 0.2083(38) -0.4489(122) 0.1060(48) 0.180 Uiso 1 calc R . 
H33C H 0.1817(13) -0.5634(21) 0.1437(85) 0.180 Uiso 1 calc R . 
O34 O 0.0665(8) -0.4609(15) 0.0754(9) 0.135(6) Uani 1 d . . 
C41 C 0.0875(13) 0.1537(28) 0.0101(14) 0.148(11) Uani 1 d . . 
H41A H 0.0456(13) 0.1251(28) -0.0228(14) 0.177 Uiso 1 calc R . 
H41B H 0.0713(13) 0.1804(28) 0.0517(14) 0.177 Uiso 1 calc R . 
C42 C 0.1151(14) 0.2574(23) -0.0185(15) 0.123(9) Uani 1 d . . 
H42 H 0.1586(14) 0.2799(23) 0.0151(15) 0.147 Uiso 1 calc R . 
C43 C 0.1387(16) 0.2421(26) -0.0860(14) 0.168(13) Uani 1 d . . 
H43A H 0.1677(116) 0.3121(127) -0.0934(65) 0.253 Uiso 1 calc R . 
H43B H 0.0974(16) 0.2376(246) -0.1231(21) 0.253 Uiso 1 calc R . 
H43C H 0.1662(123) 0.1667(133) -0.0850(53) 0.253 Uiso 1 calc R . 
O44 O 0.0707(8) 0.3723(17) -0.0276(8) 0.137(6) Uani 1 d . . 
N5 N 0.3765(9) 0.2159(18) 0.1106(10) 0.093(5) Uani 1 d . . 
C51 C 0.4450(10) 0.2535(25) 0.0943(11) 0.125(9) Uani 1 d . . 
H51A H 0.4380(19) 0.3249(98) 0.0641(73) 0.188 Uiso 1 calc R . 
H51B H 0.4643(45) 0.1860(59) 0.0714(81) 0.188 Uiso 1 calc R . 
H51C H 0.4780(31) 0.2742(158) 0.1365(14) 0.188 Uiso 1 calc R . 
C52 C 0.3305(13) 0.1858(22) 0.0398(15) 0.141(10) Uani 1 d . . 
H52A H 0.3313(89) 0.2551(78) 0.0089(35) 0.212 Uiso 1 calc R . 
H52B H 0.2820(27) 0.1703(189) 0.0449(22) 0.212 Uiso 1 calc R . 
H52C H 0.3491(66) 0.1130(113) 0.0209(49) 0.212 Uiso 1 calc R . 
C53 C 0.3415(13) 0.3161(25) 0.1416(14) 0.155(11) Uani 1 d . . 
H53A H 0.2940(43) 0.2904(78) 0.1453(102) 0.232 Uiso 1 calc R . 
H53B H 0.3386(102) 0.3891(65) 0.1128(59) 0.232 Uiso 1 calc R . 
H53C H 0.3687(62) 0.3348(137) 0.1871(47) 0.232 Uiso 1 calc R . 
C54 C 0.3858(13) 0.1046(24) 0.1539(12) 0.127(9) Uani 1 d . . 
H54A H 0.4088(86) 0.1266(35) 0.2005(25) 0.191 Uiso 1 calc R . 
H54B H 0.4150(79) 0.0455(71) 0.1353(54) 0.191 Uiso 1 calc R . 
H54C H 0.3397(15) 0.0683(94) 0.1545(74) 0.191 Uiso 1 calc R . 
N6 N 0.0796(11) 0.2017(20) 0.6481(10) 0.121(7) Uani 1 d . . 
C61 C 0.0394(26) 0.3241(51) 0.6221(25) 0.131(23) Uiso 0.55(5) d P . 
C61X C 0.0598(44) 0.3135(84) 0.7011(45) 0.191(39) Uiso 0.45(5) d P . 
C62 C 0.0280(14) 0.1193(30) 0.6069(15) 0.176(13) Uani 1 d . . 
H62A H 0.0423(74) 0.1020(195) 0.5635(59) 0.264 Uiso 1 calc R . 
H62B H -0.0184(30) 0.1583(102) 0.5981(113) 0.264 Uiso 1 calc R . 
H62C H 0.0258(102) 0.0426(97) 0.6318(61) 0.264 Uiso 1 calc R . 
C63 C 0.1437(13) 0.2148(32) 0.6184(14) 0.171(13) Uani 1 d . . 
H63A H 0.1314(28) 0.2559(201) 0.5741(60) 0.256 Uiso 1 calc R . 
H63B H 0.1631(72) 0.1338(34) 0.6123(114) 0.256 Uiso 1 calc R . 
H63C H 0.1788(51) 0.2635(190) 0.6491(62) 0.256 Uiso 1 calc R . 
C64 C 0.0808(26) 0.1965(51) 0.7214(24) 0.113(18) Uiso 0.55(5) d P . 
C64X C 0.1109(26) 0.1155(50) 0.7192(23) 0.087(19) Uiso 0.45(5) d P . 

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 
Fe1 0.056(2) 0.069(2) 0.093(2) 0.0021(15) 0.0143(14) -0.0073(14) 
Fe2 0.059(2) 0.073(2) 0.084(2) 0.0012(14) 0.0200(14) 0.0038(14) 
Fe3 0.060(2) 0.064(2) 0.092(2) 0.0060(15) 0.0205(14) -0.0060(14) 
Fe4 0.064(2) 0.066(2) 0.085(2) 0.0033(14) 0.0228(14) -0.0041(14) 
S11 0.053(3) 0.087(4) 0.090(3) -0.007(3) 0.008(2) -0.011(3) 
S22 0.062(3) 0.076(4) 0.103(4) 0.000(3) 0.032(3) 0.000(3) 
S33 0.074(3) 0.060(3) 0.107(4) 0.002(3) 0.023(3) -0.004(3) 
S44 0.067(3) 0.093(4) 0.082(3) 0.010(3) 0.013(3) -0.001(3) 
S1 0.068(4) 0.133(6) 0.151(6) -0.017(4) 0.014(4) -0.026(4) 
S2 0.086(4) 0.122(5) 0.122(5) 0.000(4) 0.042(4) 0.027(4) 
S3 0.126(5) 0.081(4) 0.119(5) 0.019(4) 0.030(4) -0.019(4) 
S4 0.101(4) 0.118(5) 0.079(3) 0.012(3) 0.030(3) 0.006(4) 
C11 0.183(31) 0.216(38) 0.165(26) -0.112(28) 0.079(24) -0.078(29) 
C13 0.245(44) 0.279(50) 0.346(55) -0.220(46) 0.126(41) -0.063(38) 
O14 0.378(43) 0.213(29) 0.366(37) -0.049(27) 0.241(34) -0.036(28) 
C21 0.310(44) 0.057(16) 0.173(27) -0.038(18) 0.137(33) -0.060(21) 
C23 0.220(35) 0.129(26) 0.164(26) -0.014(20) 0.031(24) -0.032(25) 
C31 0.153(23) 0.094(18) 0.101(17) 0.010(14) 0.049(17) 0.007(16) 
C32 0.104(19) 0.096(18) 0.121(19) -0.044(15) -0.010(16) -0.027(15) 
C33 0.053(14) 0.122(20) 0.193(24) 0.013(17) 0.040(15) 0.008(14) 
O34 0.087(11) 0.133(14) 0.172(15) -0.053(12) -0.008(11) 0.023(10) 
C41 0.123(22) 0.191(31) 0.152(22) 0.074(22) 0.083(19) 0.062(21) 
C42 0.113(20) 0.085(18) 0.174(26) 0.044(18) 0.037(18) 0.054(16) 
C43 0.202(30) 0.170(27) 0.176(25) 0.088(22) 0.142(24) 0.070(23) 
O44 0.100(12) 0.156(16) 0.158(14) -0.011(12) 0.031(11) 0.041(12) 
N5 0.068(12) 0.111(16) 0.106(13) -0.024(12) 0.036(11) -0.038(11) 
C51 0.069(15) 0.181(25) 0.138(20) -0.024(18) 0.053(14) -0.041(16) 
C52 0.092(18) 0.106(21) 0.237(32) -0.030(20) 0.060(21) -0.036(15) 
C53 0.121(22) 0.159(27) 0.205(28) -0.046(23) 0.081(21) 0.028(20) 
C54 0.136(23) 0.128(22) 0.128(19) 0.032(18) 0.050(17) -0.028(18) 
N6 0.126(17) 0.121(18) 0.126(16) -0.015(14) 0.049(14) -0.060(15) 
C62 0.111(22) 0.204(34) 0.203(30) 0.025(27) 0.007(21) -0.055(23) 
C63 0.092(19) 0.278(40) 0.161(24) -0.007(25) 0.070(19) -0.032(23) 

_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 
Fe1 S1 2.243(6) . ? 
Fe1 S22 2.244(6) . ? 
Fe1 S44 2.287(6) . ? 
Fe1 S33 2.301(6) . ? 
Fe1 Fe2 2.717(4) . ? 
Fe1 Fe3 2.720(4) . ? 
Fe1 Fe4 2.737(4) . ? 
Fe2 S2 2.237(6) . ? 
Fe2 S11 2.260(6) . ? 
Fe2 S33 2.287(5) . ? 
Fe2 S44 2.296(5) . ? 
Fe2 Fe3 2.729(4) . ? 
Fe2 Fe4 2.733(4) . ? 
Fe3 S3 2.234(6) . ? 
Fe3 S44 2.247(6) . ? 
Fe3 S11 2.299(5) . ? 
Fe3 S22 2.302(5) . ? 
Fe3 Fe4 2.759(4) . ? 
Fe4 S4 2.254(6) . ? 
Fe4 S33 2.254(6) . ? 
Fe4 S11 2.283(5) . ? 
Fe4 S22 2.293(6) . ? 
S1 C11 1.79(3) . ? 
S2 C21 1.85(3) . ? 
S3 C31 1.78(2) . ? 
S4 C41 1.78(2) . ? 
C11 C12X 1.31(8) . ? 
C11 C12 1.46(5) . ? 
C12 O14 1.52(5) . ? 
C12 C13 1.61(6) . ? 
C12X C13 1.27(8) . ? 
C12X O14 1.71(7) . ? 
C21 C22 1.38(5) . ? 
C21 C22X 1.41(6) . ? 
C22 O24 1.31(6) . ? 
C22 C23 1.72(6) . ? 
C22X O24X 1.39(6) . ? 
C22X C23 1.55(6) . ? 
C31 C32 1.47(3) . ? 
C32 O34 1.44(2) . ? 
C32 C33 1.51(3) . ? 
C41 C42 1.39(3) . ? 
C42 O44 1.48(2) . ? 
C42 C43 1.49(3) . ? 
N5 C54 1.45(3) . ? 
N5 C51 1.46(2) . ? 
N5 C53 1.46(2) . ? 
N5 C52 1.52(3) . ? 
N6 C64 1.43(5) . ? 
N6 C62 1.44(3) . ? 
N6 C63 1.46(3) . ? 
N6 C61 1.55(5) . ? 
N6 C61X 1.67(9) . ? 
N6 C64X 1.68(5) . ? 

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 
S1 Fe1 S22 115.7(2) . . ? 
S1 Fe1 S44 111.2(2) . . ? 
S22 Fe1 S44 104.4(2) . . ? 
S1 Fe1 S33 115.4(3) . . ? 
S22 Fe1 S33 103.6(2) . . ? 
S44 Fe1 S33 105.4(2) . . ? 
S1 Fe1 Fe2 142.4(2) . . ? 
S22 Fe1 Fe2 101.8(2) . . ? 
S44 Fe1 Fe2 53.79(14) . . ? 
S33 Fe1 Fe2 53.44(14) . . ? 
S1 Fe1 Fe3 143.4(2) . . ? 
S22 Fe1 Fe3 54.24(14) . . ? 
S44 Fe1 Fe3 52.5(2) . . ? 
S33 Fe1 Fe3 101.1(2) . . ? 
Fe2 Fe1 Fe3 60.25(10) . . ? 
S1 Fe1 Fe4 147.4(2) . . ? 
S22 Fe1 Fe4 53.7(2) . . ? 
S44 Fe1 Fe4 101.3(2) . . ? 
S33 Fe1 Fe4 52.29(15) . . ? 
Fe2 Fe1 Fe4 60.14(9) . . ? 
Fe3 Fe1 Fe4 60.76(10) . . ? 
S2 Fe2 S11 114.3(2) . . ? 
S2 Fe2 S33 114.1(2) . . ? 
S11 Fe2 S33 103.5(2) . . ? 
S2 Fe2 S44 114.2(2) . . ? 
S11 Fe2 S44 103.9(2) . . ? 
S33 Fe2 S44 105.6(2) . . ? 
S2 Fe2 Fe1 144.3(2) . . ? 
S11 Fe2 Fe1 101.3(2) . . ? 
S33 Fe2 Fe1 53.92(15) . . ? 
S44 Fe2 Fe1 53.50(14) . . ? 
S2 Fe2 Fe3 144.7(2) . . ? 
S11 Fe2 Fe3 53.89(15) . . ? 
S33 Fe2 Fe3 101.2(2) . . ? 
S44 Fe2 Fe3 52.3(2) . . ? 
Fe1 Fe2 Fe3 59.92(10) . . ? 
S2 Fe2 Fe4 144.6(2) . . ? 
S11 Fe2 Fe4 53.39(15) . . ? 
S33 Fe2 Fe4 52.46(15) . . ? 
S44 Fe2 Fe4 101.2(2) . . ? 
Fe1 Fe2 Fe4 60.29(10) . . ? 
Fe3 Fe2 Fe4 60.70(10) . . ? 
S3 Fe3 S44 113.3(2) . . ? 
S3 Fe3 S11 113.5(2) . . ? 
S44 Fe3 S11 104.2(2) . . ? 
S3 Fe3 S22 116.8(2) . . ? 
S44 Fe3 S22 103.9(2) . . ? 
S11 Fe3 S22 103.8(2) . . ? 
S3 Fe3 Fe1 146.2(2) . . ? 
S44 Fe3 Fe1 53.83(15) . . ? 
S11 Fe3 Fe1 100.2(2) . . ? 
S22 Fe3 Fe1 52.28(15) . . ? 
S3 Fe3 Fe2 143.3(2) . . ? 
S44 Fe3 Fe2 53.91(15) . . ? 
S11 Fe3 Fe2 52.59(15) . . ? 
S22 Fe3 Fe2 100.0(2) . . ? 
Fe1 Fe3 Fe2 59.82(10) . . ? 
S3 Fe3 Fe4 145.0(2) . . ? 
S44 Fe3 Fe4 101.7(2) . . ? 
S11 Fe3 Fe4 52.70(14) . . ? 
S22 Fe3 Fe4 52.93(15) . . ? 
Fe1 Fe3 Fe4 59.93(10) . . ? 
Fe2 Fe3 Fe4 59.73(10) . . ? 
S4 Fe4 S33 116.1(2) . . ? 
S4 Fe4 S11 116.6(2) . . ? 
S33 Fe4 S11 103.8(2) . . ? 
S4 Fe4 S22 110.6(2) . . ? 
S33 Fe4 S22 103.5(2) . . ? 
S11 Fe4 S22 104.7(2) . . ? 
S4 Fe4 Fe2 149.3(2) . . ? 
S33 Fe4 Fe2 53.54(15) . . ? 
S11 Fe4 Fe2 52.64(14) . . ? 
S22 Fe4 Fe2 100.1(2) . . ? 
S4 Fe4 Fe1 143.0(2) . . ? 
S33 Fe4 Fe1 53.86(15) . . ? 
S11 Fe4 Fe1 100.2(2) . . ? 
S22 Fe4 Fe1 52.09(15) . . ? 
Fe2 Fe4 Fe1 59.57(10) . . ? 
S4 Fe4 Fe3 142.6(2) . . ? 
S33 Fe4 Fe3 101.1(2) . . ? 
S11 Fe4 Fe3 53.24(14) . . ? 
S22 Fe4 Fe3 53.25(14) . . ? 
Fe2 Fe4 Fe3 59.58(10) . . ? 
Fe1 Fe4 Fe3 59.32(10) . . ? 
Fe2 S11 Fe4 74.0(2) . . ? 
Fe2 S11 Fe3 73.5(2) . . ? 
Fe4 S11 Fe3 74.1(2) . . ? 
Fe1 S22 Fe4 74.2(2) . . ? 
Fe1 S22 Fe3 73.5(2) . . ? 
Fe4 S22 Fe3 73.8(2) . . ? 
Fe4 S33 Fe2 74.0(2) . . ? 
Fe4 S33 Fe1 73.9(2) . . ? 
Fe2 S33 Fe1 72.6(2) . . ? 
Fe3 S44 Fe1 73.7(2) . . ? 
Fe3 S44 Fe2 73.8(2) . . ? 
Fe1 S44 Fe2 72.7(2) . . ? 
C11 S1 Fe1 103.4(11) . . ? 
C21 S2 Fe2 105.3(12) . . ? 
C31 S3 Fe3 104.6(8) . . ? 
C41 S4 Fe4 100.8(8) . . ? 
C12X C11 S1 134.4(40) . . ? 
C12 C11 S1 110.7(33) . . ? 
C11 C12 O14 99.6(36) . . ? 
C11 C12 C13 105.2(39) . . ? 
O14 C12 C13 90.1(35) . . ? 
C13 C12X C11 141.8(68) . . ? 
C13 C12X O14 94.6(52) . . ? 
C11 C12X O14 96.9(49) . . ? 
C22 C21 S2 117.2(30) . . ? 
C22X C21 S2 120.1(33) . . ? 
O24 C22 C21 116.0(50) . . ? 
O24 C22 C23 112.4(47) . . ? 
C21 C22 C23 101.9(37) . . ? 
O24X C22X C21 113.4(57) . . ? 
O24X C22X C23 109.1(47) . . ? 
C21 C22X C23 109.7(46) . . ? 
C32 C31 S3 117.6(17) . . ? 
O34 C32 C31 111.4(20) . . ? 
O34 C32 C33 109.6(19) . . ? 
C31 C32 C33 115.8(21) . . ? 
C42 C41 S4 116.9(17) . . ? 
C41 C42 O44 117.4(22) . . ? 
C41 C42 C43 118.3(25) . . ? 
O44 C42 C43 104.4(20) . . ? 
C54 N5 C51 110.1(19) . . ? 
C54 N5 C53 112.0(19) . . ? 
C51 N5 C53 112.9(19) . . ? 
C54 N5 C52 109.9(18) . . ? 
C51 N5 C52 103.7(16) . . ? 
C53 N5 C52 107.9(19) . . ? 
C64 N6 C62 114.3(25) . . ? 
C64 N6 C63 123.8(27) . . ? 
C62 N6 C63 111.4(21) . . ? 
C64 N6 C61 105.8(31) . . ? 
C62 N6 C61 95.6(25) . . ? 
C63 N6 C61 100.6(24) . . ? 
C62 N6 C61X 125.0(34) . . ? 
C63 N6 C61X 119.1(34) . . ? 
C62 N6 C64X 102.5(23) . . ? 
C63 N6 C64X 101.4(24) . . ? 
C61X N6 C64X 88.1(34) . . ? 

_refine_diff_density_max    0.588 
_refine_diff_density_min   -0.906 
_refine_diff_density_rms    0.147