# Electronic Supplementary Material (ESI) for New Journal of Chemistry
# This journal is © The Royal Society of Chemistry and The Centre National de la Recherche Scientifique 2011


data_global
_journal_name_full               'New J.Chem.'

_journal_coden_Cambridge         0440
_journal_volume                  ?
_journal_page_first              ?
_journal_year                    ?

_publ_contact_author_name        'Dr Minghuey Shieh'
_publ_contact_author_email       mshieh@ntnu.edu.tw

_publ_section_title              
;
Reactions of the m3-sulfido triiron cluster
[SFe3(CO)9]2- with functionalized organic halides and mercury salts:
selective reactivity, electrochemistry, and theoretical calculations

;
loop_
_publ_author_name
'Minghuey Shieh'
'Chia-Yeh Miu'
'Hsin-Hung Chi'
'Szu-Wei Chen'
;
Jiann-Jang Cherng
;
'Miao-Hsing Hsu'
'Yu-Xin Huang'

# Attachment '- cif-S-Fe-RX-2011-NJC-revised.cif'

data_1
_database_code_depnum_ccdc_archive 'CCDC 817581'
#TrackingRef '- cif-S-Fe-RX-2011-NJC-revised.cif'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C20 H25 Fe3 N O11 S'
_chemical_formula_sum            'C20 H25 Fe3 N O11 S'
_chemical_formula_weight         655.02

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           triclinic
_symmetry_space_group_name_H-M   'P -1'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.4943(9)
_cell_length_b                   10.791(6)
_cell_length_c                   13.2079(17)
_cell_angle_alpha                89.92(3)
_cell_angle_beta                 88.507(9)
_cell_angle_gamma                86.83(2)
_cell_volume                     1350.7(8)
_cell_formula_units_Z            2
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    25
_cell_measurement_theta_min      7.56
_cell_measurement_theta_max      13.92

_exptl_crystal_description       prism
_exptl_crystal_colour            black
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.25
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.611
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             668
_exptl_absorpt_coefficient_mu    1.721
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_correction_T_min  0.5873
_exptl_absorpt_correction_T_max  0.6492
_exptl_absorpt_process_details   
;
?
;

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      298(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  'Enraf Nonius TurboCAD4'
_diffrn_measurement_method       'non-profiled omega/2theta scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         3
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  120
_diffrn_standards_decay_%        4
_diffrn_reflns_number            6447
_diffrn_reflns_av_R_equivalents  0.0148
_diffrn_reflns_av_sigmaI/netI    0.0283
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       0
_diffrn_reflns_theta_min         1.54
_diffrn_reflns_theta_max         27.41
_reflns_number_total             6178
_reflns_number_gt                4613
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CAD4 Express (Enraf Nonius, 1994)'
_computing_cell_refinement       'CAD4 Express (Enraf Nonius, 1994)'
_computing_data_reduction        'XCAD4 (Harms & Wocadlo, 1995)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0402P)^2^+0.1653P] 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    noref
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6178
_refine_ls_number_parameters     400
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0488
_refine_ls_R_factor_gt           0.0261
_refine_ls_wR_factor_ref         0.0761
_refine_ls_wR_factor_gt          0.0679
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_restrained_S_all      1.019
_refine_ls_shift/su_max          0.006
_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
Fe1 Fe 0.41243(3) -0.25588(3) -0.29798(2) 0.03741(8) Uani 1 1 d . . .
Fe2 Fe 0.65932(3) -0.18343(3) -0.34440(2) 0.03675(8) Uani 1 1 d . . .
Fe3 Fe 0.58643(3) -0.21713(3) -0.15347(2) 0.03313(8) Uani 1 1 d . . .
S S 0.61084(6) -0.36029(5) -0.27141(4) 0.03897(12) Uani 1 1 d . . .
O1 O 0.1878(2) -0.3519(2) -0.17067(17) 0.0854(7) Uani 1 1 d . . .
O2 O 0.2850(2) -0.0055(2) -0.3243(2) 0.0905(7) Uani 1 1 d . . .
O3 O 0.3154(3) -0.3631(3) -0.48471(17) 0.0975(8) Uani 1 1 d . . .
O4 O 0.5977(2) 0.06548(19) -0.42589(15) 0.0750(6) Uani 1 1 d . . .
O5 O 0.6582(3) -0.3002(2) -0.54303(15) 0.0861(7) Uani 1 1 d . . .
O6 O 0.9672(2) -0.1785(2) -0.33141(17) 0.0785(6) Uani 1 1 d . . .
O7 O 0.6508(2) 0.03821(17) -0.19342(14) 0.0671(5) Uani 1 1 d . . .
O8 O 0.8647(2) -0.2096(2) -0.06288(17) 0.0847(7) Uani 1 1 d . . .
O9 O 0.3524(2) -0.0814(2) -0.04545(17) 0.0855(7) Uani 1 1 d . . .
O10 O 0.70576(17) -0.37486(18) 0.07646(13) 0.0549(4) Uani 1 1 d . . .
O11 O 0.48620(16) -0.30822(17) 0.11962(12) 0.0514(4) Uani 1 1 d . . .
N N 0.96203(17) -0.71352(17) -0.24457(13) 0.0361(4) Uani 1 1 d . . .
C1 C 0.2778(3) -0.3166(3) -0.21965(19) 0.0520(6) Uani 1 1 d . . .
C2 C 0.3350(3) -0.1034(3) -0.3127(2) 0.0546(6) Uani 1 1 d . . .
C3 C 0.3563(3) -0.3207(3) -0.4124(2) 0.0579(6) Uani 1 1 d . . .
C4 C 0.6183(3) -0.0317(2) -0.39436(17) 0.0498(6) Uani 1 1 d . . .
C5 C 0.6572(3) -0.2546(3) -0.46524(18) 0.0554(6) Uani 1 1 d . . .
C6 C 0.8482(3) -0.1806(2) -0.33558(18) 0.0487(5) Uani 1 1 d . . .
C7 C 0.6303(2) -0.0658(2) -0.20075(17) 0.0444(5) Uani 1 1 d . . .
C8 C 0.7545(3) -0.2176(2) -0.09317(17) 0.0500(6) Uani 1 1 d . . .
C9 C 0.4437(3) -0.1344(3) -0.08738(18) 0.0533(6) Uani 1 1 d . . .
C10 C 0.5324(3) -0.3617(2) -0.05117(18) 0.0487(6) Uani 1 1 d . . .
C11 C 0.5862(2) -0.3490(2) 0.05210(16) 0.0411(5) Uani 1 1 d . . .
C12 C 0.5319(3) -0.2995(3) 0.2222(2) 0.0608(7) Uani 1 1 d . . .
C13 C 1.0585(3) -0.8070(2) -0.1892(2) 0.0485(5) Uani 1 1 d . . .
C14 C 0.9896(4) -0.9117(3) -0.1387(3) 0.0788(10) Uani 1 1 d . . .
C15 C 0.8510(2) -0.6539(3) -0.17202(18) 0.0469(5) Uani 1 1 d . . .
C16 C 0.9083(4) -0.5829(4) -0.0861(2) 0.0703(8) Uani 1 1 d . . .
C17 C 1.0561(3) -0.6177(3) -0.2887(2) 0.0503(6) Uani 1 1 d . . .
C18 C 0.9808(4) -0.5156(4) -0.3472(3) 0.0805(10) Uani 1 1 d . . .
C19 C 0.8820(3) -0.7772(3) -0.32614(18) 0.0483(5) Uani 1 1 d . . .
C20 C 0.9716(4) -0.8401(4) -0.4087(3) 0.0762(9) Uani 1 1 d . . .
H10A H 0.580(3) -0.433(3) -0.082(2) 0.056 Uiso 1 1 d . . .
H10B H 0.435(3) -0.357(2) -0.047(2) 0.056 Uiso 1 1 d . . .
H12A H 0.454(3) -0.273(3) 0.260(2) 0.067 Uiso 1 1 d . . .
H12B H 0.594(3) -0.236(3) 0.231(2) 0.067 Uiso 1 1 d . . .
H12C H 0.577(3) -0.371(3) 0.247(2) 0.067 Uiso 1 1 d . . .
H13A H 1.108(3) -0.760(3) -0.139(2) 0.059 Uiso 1 1 d . . .
H13B H 1.125(3) -0.834(3) -0.239(2) 0.059 Uiso 1 1 d . . .
H14A H 1.052(3) -0.960(3) -0.102(2) 0.082 Uiso 1 1 d . . .
H14B H 0.914(4) -0.883(3) -0.083(2) 0.082 Uiso 1 1 d . . .
H14C H 0.944(4) -0.955(3) -0.180(3) 0.082 Uiso 1 1 d . . .
H15A H 0.800(3) -0.720(3) -0.149(2) 0.057 Uiso 1 1 d . . .
H15B H 0.795(3) -0.596(2) -0.213(2) 0.057 Uiso 1 1 d . . .
H16A H 0.828(3) -0.556(3) -0.039(2) 0.079 Uiso 1 1 d . . .
H16B H 0.965(3) -0.638(3) -0.040(2) 0.079 Uiso 1 1 d . . .
H16C H 0.958(4) -0.520(3) -0.111(2) 0.079 Uiso 1 1 d . . .
H17A H 1.104(3) -0.585(3) -0.229(2) 0.059 Uiso 1 1 d . . .
H17B H 1.116(3) -0.661(3) -0.331(2) 0.059 Uiso 1 1 d . . .
H18A H 1.041(4) -0.470(3) -0.373(3) 0.085 Uiso 1 1 d . . .
H18B H 0.930(4) -0.550(3) -0.411(2) 0.085 Uiso 1 1 d . . .
H18C H 0.924(4) -0.471(3) -0.307(3) 0.085 Uiso 1 1 d . . .
H19A H 0.829(3) -0.833(3) -0.291(2) 0.058 Uiso 1 1 d . . .
H19B H 0.825(3) -0.714(3) -0.353(2) 0.058 Uiso 1 1 d . . .
H20A H 0.913(3) -0.867(3) -0.456(3) 0.081 Uiso 1 1 d . . .
H20B H 1.012(4) -0.784(3) -0.442(3) 0.081 Uiso 1 1 d . . .
H20C H 1.032(3) -0.911(3) -0.377(2) 0.081 Uiso 1 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
Fe1 0.03316(15) 0.04244(17) 0.03722(16) 0.00216(12) -0.00839(12) -0.00400(12)
Fe2 0.03616(15) 0.04399(17) 0.03010(15) 0.00378(12) -0.00023(11) -0.00267(12)
Fe3 0.03594(15) 0.03601(16) 0.02820(14) 0.00331(11) -0.00465(11) -0.00710(11)
S 0.0428(3) 0.0346(3) 0.0391(3) 0.0008(2) -0.0039(2) 0.0026(2)
O1 0.0616(12) 0.1159(19) 0.0813(15) 0.0278(13) 0.0007(11) -0.0323(13)
O2 0.0754(15) 0.0642(14) 0.128(2) 0.0120(13) -0.0002(13) 0.0292(12)
O3 0.1110(19) 0.116(2) 0.0687(14) -0.0202(14) -0.0405(14) -0.0205(16)
O4 0.1012(16) 0.0589(12) 0.0667(13) 0.0236(10) -0.0266(11) -0.0101(11)
O5 0.0971(17) 0.1142(19) 0.0474(11) -0.0245(12) 0.0103(11) -0.0140(14)
O6 0.0413(10) 0.1075(18) 0.0874(15) 0.0017(13) -0.0013(10) -0.0110(10)
O7 0.1052(16) 0.0427(10) 0.0554(11) 0.0007(8) -0.0008(10) -0.0223(10)
O8 0.0597(12) 0.1174(19) 0.0820(14) 0.0401(13) -0.0363(11) -0.0353(12)
O9 0.0744(14) 0.1049(18) 0.0741(14) -0.0230(13) 0.0145(11) 0.0169(13)
O10 0.0444(9) 0.0731(12) 0.0466(9) 0.0063(8) -0.0032(7) 0.0034(8)
O11 0.0402(8) 0.0710(11) 0.0433(9) -0.0008(8) -0.0044(7) -0.0036(8)
N 0.0280(8) 0.0458(10) 0.0347(8) -0.0026(7) -0.0015(6) -0.0023(7)
C1 0.0432(12) 0.0636(16) 0.0506(13) 0.0078(11) -0.0103(10) -0.0118(11)
C2 0.0405(12) 0.0586(16) 0.0640(16) 0.0033(12) -0.0029(11) 0.0047(11)
C3 0.0545(14) 0.0712(17) 0.0494(14) 0.0030(12) -0.0183(11) -0.0082(13)
C4 0.0529(13) 0.0600(15) 0.0374(11) 0.0094(11) -0.0094(10) -0.0069(11)
C5 0.0557(14) 0.0715(17) 0.0392(12) -0.0047(12) 0.0064(10) -0.0084(12)
C6 0.0446(13) 0.0577(14) 0.0438(12) 0.0036(10) 0.0013(9) -0.0057(10)
C7 0.0505(13) 0.0443(13) 0.0393(11) 0.0062(9) -0.0053(9) -0.0091(10)
C8 0.0521(13) 0.0577(14) 0.0422(12) 0.0158(10) -0.0118(10) -0.0169(11)
C9 0.0552(14) 0.0599(15) 0.0446(13) -0.0046(11) 0.0023(11) -0.0043(12)
C10 0.0581(14) 0.0503(14) 0.0396(12) 0.0117(10) -0.0059(10) -0.0195(12)
C11 0.0447(12) 0.0394(11) 0.0402(11) 0.0081(9) -0.0023(9) -0.0104(9)
C12 0.0526(15) 0.088(2) 0.0415(14) -0.0109(14) -0.0021(11) -0.0021(14)
C13 0.0414(12) 0.0507(14) 0.0532(14) -0.0043(11) -0.0121(10) 0.0035(10)
C14 0.092(2) 0.062(2) 0.085(2) 0.0189(17) -0.0361(19) -0.0123(17)
C15 0.0334(11) 0.0630(15) 0.0431(12) -0.0027(11) 0.0046(9) 0.0049(10)
C16 0.0687(19) 0.086(2) 0.0542(17) -0.0247(16) 0.0022(14) 0.0108(16)
C17 0.0406(12) 0.0590(15) 0.0521(14) -0.0014(12) 0.0047(10) -0.0123(11)
C18 0.084(2) 0.077(2) 0.082(2) 0.0288(19) 0.0000(18) -0.0198(18)
C19 0.0436(12) 0.0638(16) 0.0393(12) -0.0020(11) -0.0104(10) -0.0133(11)
C20 0.076(2) 0.097(3) 0.0565(18) -0.0311(18) -0.0020(15) -0.0116(18)

_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 C3 1.773(3) . ?
Fe1 C1 1.776(3) . ?
Fe1 C2 1.777(3) . ?
Fe1 S 2.1771(8) . ?
Fe1 Fe2 2.5705(6) . ?
Fe1 Fe3 2.6057(5) . ?
Fe2 C5 1.773(2) . ?
Fe2 C4 1.791(3) . ?
Fe2 C6 1.802(2) . ?
Fe2 S 2.2027(12) . ?
Fe2 C7 2.286(2) . ?
Fe2 Fe3 2.6277(5) . ?
Fe3 C9 1.789(3) . ?
Fe3 C8 1.802(2) . ?
Fe3 C7 1.814(2) . ?
Fe3 C10 2.137(2) . ?
Fe3 S 2.1945(10) . ?
O1 C1 1.140(3) . ?
O2 C2 1.145(3) . ?
O3 C3 1.146(3) . ?
O4 C4 1.137(3) . ?
O5 C5 1.139(3) . ?
O6 C6 1.134(3) . ?
O7 C7 1.154(3) . ?
O8 C8 1.137(3) . ?
O9 C9 1.143(3) . ?
O10 C11 1.206(3) . ?
O11 C11 1.342(3) . ?
O11 C12 1.438(3) . ?
N C17 1.510(3) . ?
N C19 1.520(3) . ?
N C15 1.523(3) . ?
N C13 1.524(3) . ?
C10 C11 1.478(3) . ?
C10 H10A 0.96(3) . ?
C10 H10B 0.93(3) . ?
C12 H12A 0.92(3) . ?
C12 H12B 0.94(3) . ?
C12 H12C 0.93(3) . ?
C13 C14 1.486(4) . ?
C13 H13A 0.99(3) . ?
C13 H13B 0.93(3) . ?
C14 H14A 0.92(3) . ?
C14 H14B 1.05(3) . ?
C14 H14C 0.86(3) . ?
C15 C16 1.500(4) . ?
C15 H15A 0.93(3) . ?
C15 H15B 0.97(3) . ?
C16 H16A 1.00(3) . ?
C16 H16B 1.00(3) . ?
C16 H16C 0.90(3) . ?
C17 C18 1.504(5) . ?
C17 H17A 1.00(3) . ?
C17 H17B 0.90(3) . ?
C18 H18A 0.84(4) . ?
C18 H18B 1.05(3) . ?
C18 H18C 0.88(3) . ?
C19 C20 1.505(4) . ?
C19 H19A 0.93(3) . ?
C19 H19B 0.93(3) . ?
C20 H20A 0.91(3) . ?
C20 H20B 0.86(3) . ?
C20 H20C 1.03(3) . ?

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
C3 Fe1 C1 95.82(12) . . ?
C3 Fe1 C2 98.35(13) . . ?
C1 Fe1 C2 98.00(12) . . ?
C3 Fe1 S 102.91(9) . . ?
C1 Fe1 S 108.98(9) . . ?
C2 Fe1 S 143.37(9) . . ?
C3 Fe1 Fe2 103.54(9) . . ?
C1 Fe1 Fe2 156.82(8) . . ?
C2 Fe1 Fe2 91.74(9) . . ?
S Fe1 Fe2 54.53(3) . . ?
C3 Fe1 Fe3 156.22(9) . . ?
C1 Fe1 Fe3 96.45(8) . . ?
C2 Fe1 Fe3 100.00(9) . . ?
S Fe1 Fe3 53.72(2) . . ?
Fe2 Fe1 Fe3 61.010(15) . . ?
C5 Fe2 C4 93.03(12) . . ?
C5 Fe2 C6 97.12(11) . . ?
C4 Fe2 C6 100.65(12) . . ?
C5 Fe2 S 90.29(10) . . ?
C4 Fe2 S 155.14(8) . . ?
C6 Fe2 S 103.37(8) . . ?
C5 Fe2 C7 169.14(11) . . ?
C4 Fe2 C7 77.73(10) . . ?
C6 Fe2 C7 90.28(10) . . ?
S Fe2 C7 95.74(7) . . ?
C5 Fe2 Fe1 91.67(9) . . ?
C4 Fe2 Fe1 101.65(8) . . ?
C6 Fe2 Fe1 155.52(8) . . ?
S Fe2 Fe1 53.60(2) . . ?
C7 Fe2 Fe1 84.71(6) . . ?
C5 Fe2 Fe3 142.09(9) . . ?
C4 Fe2 Fe3 115.85(8) . . ?
C6 Fe2 Fe3 100.71(7) . . ?
S Fe2 Fe3 53.16(3) . . ?
C7 Fe2 Fe3 42.61(6) . . ?
Fe1 Fe2 Fe3 60.156(15) . . ?
C9 Fe3 C8 115.41(12) . . ?
C9 Fe3 C7 85.07(12) . . ?
C8 Fe3 C7 84.94(10) . . ?
C9 Fe3 C10 82.29(12) . . ?
C8 Fe3 C10 87.44(10) . . ?
C7 Fe3 C10 160.75(10) . . ?
C9 Fe3 S 136.95(9) . . ?
C8 Fe3 S 105.56(9) . . ?
C7 Fe3 S 112.00(8) . . ?
C10 Fe3 S 87.07(8) . . ?
C9 Fe3 Fe1 87.84(8) . . ?
C8 Fe3 Fe1 156.47(9) . . ?
C7 Fe3 Fe1 94.08(7) . . ?
C10 Fe3 Fe1 99.87(7) . . ?
S Fe3 Fe1 53.11(2) . . ?
C9 Fe3 Fe2 125.13(8) . . ?
C8 Fe3 Fe2 101.74(8) . . ?
C7 Fe3 Fe2 58.60(8) . . ?
C10 Fe3 Fe2 140.52(8) . . ?
S Fe3 Fe2 53.45(3) . . ?
Fe1 Fe3 Fe2 58.834(15) . . ?
Fe1 S Fe3 73.17(3) . . ?
Fe1 S Fe2 71.87(3) . . ?
Fe3 S Fe2 73.39(4) . . ?
C11 O11 C12 115.19(19) . . ?
C17 N C19 111.79(18) . . ?
C17 N C15 111.03(19) . . ?
C19 N C15 106.34(17) . . ?
C17 N C13 106.24(18) . . ?
C19 N C13 110.80(18) . . ?
C15 N C13 110.72(18) . . ?
O1 C1 Fe1 177.3(3) . . ?
O2 C2 Fe1 178.6(3) . . ?
O3 C3 Fe1 177.5(3) . . ?
O4 C4 Fe2 177.3(2) . . ?
O5 C5 Fe2 178.9(3) . . ?
O6 C6 Fe2 179.1(2) . . ?
O7 C7 Fe3 154.8(2) . . ?
O7 C7 Fe2 126.34(18) . . ?
Fe3 C7 Fe2 78.79(9) . . ?
O8 C8 Fe3 172.9(2) . . ?
O9 C9 Fe3 179.8(3) . . ?
C11 C10 Fe3 114.62(15) . . ?
C11 C10 H10A 108.5(16) . . ?
Fe3 C10 H10A 101.8(16) . . ?
C11 C10 H10B 108.6(17) . . ?
Fe3 C10 H10B 105.2(17) . . ?
H10A C10 H10B 118(2) . . ?
O10 C11 O11 121.8(2) . . ?
O10 C11 C10 125.1(2) . . ?
O11 C11 C10 113.1(2) . . ?
O11 C12 H12A 106.2(18) . . ?
O11 C12 H12B 112.8(18) . . ?
H12A C12 H12B 103(3) . . ?
O11 C12 H12C 115.0(18) . . ?
H12A C12 H12C 113(3) . . ?
H12B C12 H12C 106(3) . . ?
C14 C13 N 116.5(2) . . ?
C14 C13 H13A 109.6(16) . . ?
N C13 H13A 106.6(16) . . ?
C14 C13 H13B 111.9(17) . . ?
N C13 H13B 104.1(17) . . ?
H13A C13 H13B 108(2) . . ?
C13 C14 H14A 112(2) . . ?
C13 C14 H14B 113.1(19) . . ?
H14A C14 H14B 102(3) . . ?
C13 C14 H14C 112(2) . . ?
H14A C14 H14C 113(3) . . ?
H14B C14 H14C 104(3) . . ?
C16 C15 N 115.0(2) . . ?
C16 C15 H15A 111.7(17) . . ?
N C15 H15A 104.0(17) . . ?
C16 C15 H15B 108.0(16) . . ?
N C15 H15B 105.3(15) . . ?
H15A C15 H15B 113(2) . . ?
C15 C16 H16A 108.7(19) . . ?
C15 C16 H16B 111.8(19) . . ?
H16A C16 H16B 100(2) . . ?
C15 C16 H16C 109(2) . . ?
H16A C16 H16C 114(3) . . ?
H16B C16 H16C 112(3) . . ?
C18 C17 N 114.9(2) . . ?
C18 C17 H17A 111.7(16) . . ?
N C17 H17A 103.9(15) . . ?
C18 C17 H17B 109.0(17) . . ?
N C17 H17B 104.6(18) . . ?
H17A C17 H17B 113(2) . . ?
C17 C18 H18A 109(2) . . ?
C17 C18 H18B 111.9(18) . . ?
H18A C18 H18B 103(3) . . ?
C17 C18 H18C 110(2) . . ?
H18A C18 H18C 109(3) . . ?
H18B C18 H18C 114(3) . . ?
C20 C19 N 115.7(2) . . ?
C20 C19 H19A 111.5(17) . . ?
N C19 H19A 104.3(17) . . ?
C20 C19 H19B 109.9(17) . . ?
N C19 H19B 103.8(17) . . ?
H19A C19 H19B 111(2) . . ?
C19 C20 H20A 108(2) . . ?
C19 C20 H20B 108(2) . . ?
H20A C20 H20B 101(3) . . ?
C19 C20 H20C 108.6(18) . . ?
H20A C20 H20C 112(3) . . ?
H20B C20 H20C 119(3) . . ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        27.41
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.376
_refine_diff_density_min         -0.287
_refine_diff_density_rms         0.054

#=============================================END

data_2
_database_code_depnum_ccdc_archive 'CCDC 817582'
#TrackingRef '- cif-S-Fe-RX-2011-NJC-revised.cif'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C20 H26 Cl Fe3 N O9 S'
_chemical_formula_sum            'C20 H26 Cl Fe3 N O9 S'
_chemical_formula_weight         659.48

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'
Br Br -0.2901 2.4595 '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'
O O 0.0106 0.0060 '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'
Cl Cl 0.1484 0.1585 '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'

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                   18.9216(2)
_cell_length_b                   12.3679(2)
_cell_length_c                   23.5577(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 92.5182(5)
_cell_angle_gamma                90.00
_cell_volume                     5507.7(1)
_cell_formula_units_Z            8
_cell_measurement_temperature    200(2)
_cell_measurement_reflns_used    41086
_cell_measurement_theta_min      2.037
_cell_measurement_theta_max      25.028

_exptl_crystal_description       prism
_exptl_crystal_colour            black
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.591
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2688
_exptl_absorpt_coefficient_mu    1.778
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.701
_exptl_absorpt_correction_T_max  0.7734
_exptl_absorpt_process_details   
;
?
;

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      200(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            54677
_diffrn_reflns_av_R_equivalents  0.0791
_diffrn_reflns_av_sigmaI/netI    0.0569
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_theta_min         2.08
_diffrn_reflns_theta_max         25.01
_reflns_number_total             9688
_reflns_number_gt                6271
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_reduction        
'HKL Denzo and Scalepack (Otwinowski & Minor 19'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0578P)^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    noref
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         9688
_refine_ls_number_parameters     631
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0818
_refine_ls_R_factor_gt           0.0412
_refine_ls_wR_factor_ref         0.1197
_refine_ls_wR_factor_gt          0.0981
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_restrained_S_all      1.024
_refine_ls_shift/su_max          0.001
_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
Fe1 Fe 0.15424(3) 0.80033(5) 0.34964(2) 0.03501(16) Uani 1 1 d . . .
Fe2 Fe 0.26332(3) 0.85472(4) 0.41687(2) 0.03573(16) Uani 1 1 d . . .
Fe3 Fe 0.23859(3) 0.64887(4) 0.39439(2) 0.03278(16) Uani 1 1 d . . .
Fe4 Fe 0.34787(3) 0.22910(4) 0.15133(2) 0.03343(16) Uani 1 1 d . . .
Fe5 Fe 0.25882(3) 0.36728(4) 0.10176(2) 0.03390(16) Uani 1 1 d . . .
Fe6 Fe 0.24202(3) 0.15711(4) 0.08579(2) 0.03483(16) Uani 1 1 d . . .
Cl1 Cl 0.42951(6) 0.60059(10) 0.28035(5) 0.0629(3) Uani 1 1 d . . .
Cl2 Cl 0.06626(6) 0.42408(10) 0.21536(5) 0.0664(4) Uani 1 1 d . . .
S1 S 0.26337(5) 0.77530(8) 0.33701(4) 0.0317(2) Uani 1 1 d . . .
S2 S 0.23762(4) 0.24579(8) 0.16287(4) 0.0312(2) Uani 1 1 d . . .
O1 O 0.07278(15) 0.6495(3) 0.27729(13) 0.0581(9) Uani 1 1 d . . .
O2 O 0.05653(15) 0.8261(3) 0.44164(13) 0.0680(10) Uani 1 1 d . . .
O3 O 0.12144(17) 1.0027(3) 0.28955(17) 0.0867(12) Uani 1 1 d . . .
O4 O 0.19637(15) 0.8408(3) 0.52672(13) 0.0621(9) Uani 1 1 d . . .
O5 O 0.2528(2) 1.0862(3) 0.39284(19) 0.0999(13) Uani 1 1 d . . .
O6 O 0.41179(15) 0.8507(3) 0.45682(12) 0.0566(8) Uani 1 1 d . . .
O7 O 0.36573(16) 0.5774(3) 0.45934(14) 0.0662(10) Uani 1 1 d . . .
O8 O 0.21568(17) 0.4592(3) 0.32154(14) 0.0689(10) Uani 1 1 d . . .
O9 O 0.13720(16) 0.6008(3) 0.48169(14) 0.0696(10) Uani 1 1 d . . .
O13 O 0.38680(17) 0.0382(3) 0.21960(16) 0.0841(12) Uani 1 1 d . . .
O14 O 0.44402(14) 0.2107(3) 0.05787(13) 0.0588(9) Uani 1 1 d . . .
O15 O 0.42840(15) 0.3966(3) 0.21223(14) 0.0698(10) Uani 1 1 d . . .
O16 O 0.36354(16) 0.4243(3) 0.01924(14) 0.0710(10) Uani 1 1 d . . .
O17 O 0.2645(2) 0.5651(3) 0.17025(15) 0.0815(11) Uani 1 1 d . . .
O18 O 0.13226(16) 0.4110(3) 0.02953(14) 0.0651(9) Uani 1 1 d . . .
O19 O 0.09441(15) 0.1317(3) 0.04573(12) 0.0571(8) Uani 1 1 d . . .
O20 O 0.27461(19) -0.0674(3) 0.11610(18) 0.0921(13) Uani 1 1 d . . .
O21 O 0.30676(16) 0.1737(3) -0.02482(13) 0.0668(10) Uani 1 1 d . . .
N1 N 0.50244(17) 0.2602(3) 0.38819(14) 0.0491(10) Uani 1 1 d . . .
N2 N 0.00561(16) 0.2895(3) 0.38946(14) 0.0443(9) Uani 1 1 d . . .
C1 C 0.1059(2) 0.7087(4) 0.30609(17) 0.0402(10) Uani 1 1 d . . .
C2 C 0.0964(2) 0.8149(4) 0.40625(18) 0.0464(11) Uani 1 1 d . . .
C3 C 0.1343(2) 0.9236(4) 0.3139(2) 0.0527(12) Uani 1 1 d . . .
C4 C 0.2219(2) 0.8462(3) 0.4833(2) 0.0453(11) Uani 1 1 d . . .
C5 C 0.2563(2) 0.9948(4) 0.4024(2) 0.0561(12) Uani 1 1 d . . .
C6 C 0.3528(2) 0.8516(3) 0.44182(16) 0.0396(10) Uani 1 1 d . . .
C7 C 0.3170(2) 0.6046(3) 0.43342(18) 0.0428(10) Uani 1 1 d . . .
C8 C 0.2240(2) 0.5336(4) 0.34948(18) 0.0442(11) Uani 1 1 d . . .
C9 C 0.1765(2) 0.6220(3) 0.44757(19) 0.0470(11) Uani 1 1 d . . .
C10 C 0.31727(18) 0.7953(3) 0.27537(15) 0.0371(10) Uani 1 1 d . . .
H10A H 0.3149 0.7314 0.2523 0.045 Uiso 1 1 d R . .
H10B H 0.2996 0.8559 0.2537 0.045 Uiso 1 1 d R . .
C11 C 0.39420(18) 0.8129(3) 0.29318(16) 0.0400(10) Uani 1 1 d . . .
H11A H 0.4207 0.8265 0.2601 0.048 Uiso 1 1 d R . .
H11B H 0.3971 0.8747 0.3179 0.048 Uiso 1 1 d R . .
C12 C 0.43004(19) 0.7186(3) 0.32361(17) 0.0447(11) Uani 1 1 d . . .
H12A H 0.4780 0.7361 0.3349 0.054 Uiso 1 1 d R . .
H12B H 0.4040 0.7029 0.3567 0.054 Uiso 1 1 d R . .
C13 C 0.3722(2) 0.1128(4) 0.19235(19) 0.0504(11) Uani 1 1 d . . .
C14 C 0.4051(2) 0.2164(3) 0.09393(18) 0.0408(10) Uani 1 1 d . . .
C15 C 0.3946(2) 0.3310(4) 0.18903(18) 0.0431(11) Uani 1 1 d . . .
C16 C 0.3228(2) 0.4000(3) 0.05137(18) 0.0470(11) Uani 1 1 d . . .
C17 C 0.2633(2) 0.4879(4) 0.14350(19) 0.0501(11) Uani 1 1 d . . .
C18 C 0.1815(2) 0.3949(3) 0.05823(19) 0.0446(10) Uani 1 1 d . . .
C19 C 0.1532(2) 0.1426(3) 0.06172(17) 0.0422(10) Uani 1 1 d . . .
C20 C 0.2618(2) 0.0214(4) 0.1045(2) 0.0565(12) Uani 1 1 d . . .
C21 C 0.2821(2) 0.1674(4) 0.0191(2) 0.0489(11) Uani 1 1 d . . .
C22 C 0.18248(17) 0.2322(3) 0.22367(16) 0.0375(10) Uani 1 1 d . . .
H22A H 0.1997 0.1735 0.2472 0.045 Uiso 1 1 d R . .
H22B H 0.1844 0.2981 0.2453 0.045 Uiso 1 1 d R . .
C23 C 0.10609(18) 0.2126(3) 0.20580(17) 0.0431(10) Uani 1 1 d . . .
H23A H 0.1036 0.1497 0.1820 0.052 Uiso 1 1 d R . .
H23B H 0.0796 0.2002 0.2390 0.052 Uiso 1 1 d R . .
C24 C 0.07029(19) 0.3040(4) 0.17337(17) 0.0504(12) Uani 1 1 d . . .
H24A H 0.0969 0.3202 0.1406 0.060 Uiso 1 1 d R . .
H24B H 0.0231 0.2834 0.1614 0.060 Uiso 1 1 d R . .
C25 C 0.5770(2) 0.2522(3) 0.36823(17) 0.0446(11) Uani 1 1 d . . .
H25A H 0.5788 0.1990 0.3386 0.054 Uiso 1 1 d R . .
H25B H 0.5911 0.3212 0.3538 0.054 Uiso 1 1 d R . .
C26 C 0.6333(2) 0.2229(4) 0.41333(18) 0.0542(12) Uani 1 1 d . . .
H26A H 0.6791 0.2198 0.3974 0.065 Uiso 1 1 d R . .
H26B H 0.6216 0.1532 0.4282 0.065 Uiso 1 1 d R . .
H26C H 0.6339 0.2754 0.4433 0.065 Uiso 1 1 d R . .
C27 C 0.4979(2) 0.3470(4) 0.43372(18) 0.0520(12) Uani 1 1 d . . .
H27A H 0.4499 0.3541 0.4447 0.062 Uiso 1 1 d R . .
H27B H 0.5274 0.3268 0.4662 0.062 Uiso 1 1 d R . .
C28 C 0.5222(3) 0.4575(4) 0.4175(2) 0.0669(14) Uani 1 1 d . . .
H28A H 0.5174 0.5051 0.4493 0.080 Uiso 1 1 d R . .
H28B H 0.4932 0.4831 0.3858 0.080 Uiso 1 1 d R . .
H28C H 0.5708 0.4558 0.4073 0.080 Uiso 1 1 d R . .
C29 C 0.4558(2) 0.2902(4) 0.33624(18) 0.0648(14) Uani 1 1 d . . .
H29A H 0.4732 0.3567 0.3211 0.078 Uiso 1 1 d R . .
H29B H 0.4581 0.2344 0.3080 0.078 Uiso 1 1 d R . .
C30 C 0.3779(2) 0.3028(6) 0.3462(2) 0.106(2) Uani 1 1 d . . .
H30A H 0.3527 0.3226 0.3115 0.127 Uiso 1 1 d R . .
H30B H 0.3736 0.3594 0.3737 0.127 Uiso 1 1 d R . .
H30C H 0.3585 0.2370 0.3606 0.127 Uiso 1 1 d R . .
C31 C 0.4796(3) 0.1561(4) 0.4146(2) 0.0743(16) Uani 1 1 d . . .
H31A H 0.5085 0.1433 0.4484 0.089 Uiso 1 1 d R . .
H31B H 0.4311 0.1632 0.4242 0.089 Uiso 1 1 d R . .
C32 C 0.4808(4) 0.0596(5) 0.3762(3) 0.134(3) Uani 1 1 d . . .
H32A H 0.4648 -0.0017 0.3971 0.161 Uiso 1 1 d R . .
H32B H 0.5289 0.0484 0.3664 0.161 Uiso 1 1 d R . .
H32C H 0.4515 0.0683 0.3422 0.161 Uiso 1 1 d R . .
C33 C 0.0792(2) 0.2705(3) 0.36763(17) 0.0479(11) Uani 1 1 d . . .
H33A H 0.0826 0.1969 0.3552 0.057 Uiso 1 1 d R . .
H33B H 0.0873 0.3182 0.3364 0.057 Uiso 1 1 d R . .
C34 C 0.1395(2) 0.2849(4) 0.41153(19) 0.0591(13) Uani 1 1 d . . .
H34A H 0.1845 0.2710 0.3958 0.071 Uiso 1 1 d R . .
H34B H 0.1330 0.2373 0.4430 0.071 Uiso 1 1 d R . .
H34C H 0.1378 0.3586 0.4242 0.071 Uiso 1 1 d R . .
C35 C -0.0094(2) 0.2115(4) 0.43671(18) 0.0544(12) Uani 1 1 d . . .
H35A H 0.0239 0.2236 0.4679 0.065 Uiso 1 1 d R . .
H35B H -0.0565 0.2230 0.4490 0.065 Uiso 1 1 d R . .
C36 C -0.0029(3) 0.0930(4) 0.4221(2) 0.097(2) Uani 1 1 d . . .
H36A H -0.0131 0.0514 0.4551 0.116 Uiso 1 1 d R . .
H36B H 0.0440 0.0763 0.4107 0.116 Uiso 1 1 d R . .
H36C H -0.0365 0.0756 0.3917 0.116 Uiso 1 1 d R . .
C37 C -0.0455(2) 0.2739(4) 0.33862(18) 0.0660(15) Uani 1 1 d . . .
H37A H -0.0316 0.3201 0.3083 0.079 Uiso 1 1 d R . .
H37B H -0.0433 0.1998 0.3266 0.079 Uiso 1 1 d R . .
C38 C -0.1223(3) 0.2920(6) 0.3504(2) 0.116(3) Uani 1 1 d . . .
H38A H -0.1511 0.2799 0.3164 0.140 Uiso 1 1 d R . .
H38B H -0.1263 0.3662 0.3618 0.140 Uiso 1 1 d R . .
H38C H -0.1380 0.2459 0.3801 0.140 Uiso 1 1 d R . .
C39 C -0.0003(2) 0.4016(4) 0.41370(18) 0.0498(11) Uani 1 1 d . . .
H39A H -0.0468 0.4136 0.4272 0.060 Uiso 1 1 d R . .
H39B H 0.0340 0.4090 0.4447 0.060 Uiso 1 1 d R . .
C40 C 0.0150(2) 0.4925(4) 0.3734(2) 0.0670(14) Uani 1 1 d . . .
H40A H 0.0112 0.5602 0.3929 0.080 Uiso 1 1 d R . .
H40B H -0.0191 0.4900 0.3420 0.080 Uiso 1 1 d R . .
H40C H 0.0618 0.4854 0.3595 0.080 Uiso 1 1 d R . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Fe1 0.0304(3) 0.0369(4) 0.0381(4) 0.0052(3) 0.0055(2) 0.0046(2)
Fe2 0.0372(3) 0.0323(3) 0.0381(4) -0.0040(3) 0.0066(3) -0.0001(2)
Fe3 0.0335(3) 0.0297(3) 0.0354(4) 0.0021(2) 0.0044(2) 0.0007(2)
Fe4 0.0289(3) 0.0363(4) 0.0353(3) 0.0032(3) 0.0042(2) 0.0015(2)
Fe5 0.0351(3) 0.0305(3) 0.0364(4) 0.0040(3) 0.0047(2) 0.0010(2)
Fe6 0.0346(3) 0.0332(3) 0.0371(4) -0.0046(3) 0.0066(2) -0.0014(2)
Cl1 0.0827(8) 0.0521(8) 0.0542(8) -0.0025(6) 0.0060(6) 0.0225(6)
Cl2 0.0790(8) 0.0622(9) 0.0588(8) 0.0065(6) 0.0111(6) 0.0249(6)
S1 0.0301(5) 0.0313(6) 0.0340(6) 0.0021(4) 0.0047(4) 0.0014(4)
S2 0.0298(5) 0.0319(6) 0.0322(6) 0.0011(4) 0.0051(4) 0.0004(4)
O1 0.060(2) 0.056(2) 0.058(2) -0.0030(17) -0.0097(16) -0.0020(16)
O2 0.0438(18) 0.114(3) 0.047(2) 0.0049(19) 0.0132(15) 0.0139(18)
O3 0.078(2) 0.061(3) 0.121(3) 0.049(2) 0.003(2) 0.0124(19)
O4 0.062(2) 0.082(3) 0.043(2) -0.0113(17) 0.0158(16) -0.0025(17)
O5 0.129(3) 0.031(2) 0.140(4) 0.004(2) 0.006(3) 0.006(2)
O6 0.0436(18) 0.076(2) 0.051(2) -0.0067(16) 0.0023(14) -0.0080(15)
O7 0.054(2) 0.062(2) 0.081(3) 0.0143(19) -0.0220(18) 0.0062(16)
O8 0.087(2) 0.045(2) 0.073(2) -0.0187(19) -0.0041(18) -0.0051(17)
O9 0.073(2) 0.070(2) 0.068(2) 0.0197(19) 0.0362(18) -0.0022(18)
O13 0.070(2) 0.076(3) 0.105(3) 0.051(2) 0.0000(19) 0.0043(19)
O14 0.0431(17) 0.088(3) 0.046(2) -0.0026(17) 0.0138(15) 0.0066(16)
O15 0.057(2) 0.072(2) 0.080(3) -0.024(2) -0.0071(17) -0.0088(18)
O16 0.071(2) 0.069(2) 0.076(2) 0.0340(19) 0.0372(18) 0.0109(18)
O17 0.123(3) 0.044(2) 0.078(3) -0.013(2) 0.011(2) -0.011(2)
O18 0.055(2) 0.063(2) 0.076(2) 0.0080(18) -0.0157(17) 0.0119(17)
O19 0.0453(18) 0.074(2) 0.052(2) -0.0046(16) 0.0000(15) -0.0118(16)
O20 0.087(3) 0.035(2) 0.155(4) 0.004(2) 0.008(2) 0.0076(19)
O21 0.063(2) 0.097(3) 0.042(2) -0.0135(18) 0.0168(16) -0.0056(18)
N1 0.053(2) 0.063(3) 0.033(2) 0.0014(18) 0.0081(17) -0.0150(18)
N2 0.046(2) 0.056(3) 0.031(2) 0.0015(17) 0.0057(16) -0.0032(17)
C1 0.037(2) 0.045(3) 0.039(3) 0.008(2) 0.0050(19) 0.009(2)
C2 0.042(2) 0.061(3) 0.036(3) 0.005(2) 0.000(2) 0.005(2)
C3 0.042(2) 0.049(3) 0.068(3) 0.011(3) 0.009(2) 0.005(2)
C4 0.045(3) 0.042(3) 0.050(3) -0.012(2) 0.004(2) -0.0002(19)
C5 0.064(3) 0.039(3) 0.066(3) -0.001(2) 0.008(2) 0.004(2)
C6 0.044(3) 0.039(3) 0.037(3) -0.0095(19) 0.013(2) -0.0042(19)
C7 0.048(3) 0.033(2) 0.047(3) 0.003(2) 0.004(2) -0.005(2)
C8 0.046(3) 0.040(3) 0.047(3) 0.003(2) 0.003(2) -0.001(2)
C9 0.052(3) 0.038(3) 0.051(3) 0.002(2) 0.006(2) -0.001(2)
C10 0.042(2) 0.040(3) 0.030(2) 0.0081(18) 0.0085(17) 0.0048(18)
C11 0.039(2) 0.042(3) 0.041(3) -0.002(2) 0.0135(18) -0.0093(19)
C12 0.029(2) 0.061(3) 0.044(3) -0.005(2) 0.0020(18) -0.0039(19)
C13 0.039(2) 0.054(3) 0.058(3) 0.012(3) 0.006(2) 0.001(2)
C14 0.039(2) 0.045(3) 0.038(3) 0.001(2) -0.003(2) 0.0054(19)
C15 0.037(2) 0.050(3) 0.042(3) -0.001(2) 0.0047(19) 0.006(2)
C16 0.057(3) 0.039(3) 0.047(3) 0.011(2) 0.013(2) 0.005(2)
C17 0.062(3) 0.040(3) 0.049(3) 0.008(2) 0.007(2) -0.001(2)
C18 0.043(2) 0.037(3) 0.055(3) 0.004(2) 0.007(2) 0.000(2)
C19 0.048(3) 0.038(3) 0.041(3) -0.007(2) 0.014(2) -0.004(2)
C20 0.049(3) 0.045(3) 0.076(4) -0.008(3) 0.009(2) 0.002(2)
C21 0.044(3) 0.054(3) 0.048(3) -0.010(2) -0.001(2) -0.005(2)
C22 0.034(2) 0.044(3) 0.035(2) 0.0033(19) 0.0081(17) 0.0012(18)
C23 0.037(2) 0.051(3) 0.043(3) -0.001(2) 0.0121(19) -0.009(2)
C24 0.030(2) 0.082(4) 0.039(3) 0.000(2) 0.0065(18) -0.002(2)
C25 0.053(3) 0.041(3) 0.041(3) -0.004(2) 0.011(2) -0.005(2)
C26 0.061(3) 0.047(3) 0.056(3) 0.006(2) 0.007(2) 0.009(2)
C27 0.049(3) 0.073(4) 0.036(3) -0.007(2) 0.016(2) 0.001(2)
C28 0.085(4) 0.058(4) 0.058(3) -0.008(3) 0.007(3) 0.010(3)
C29 0.061(3) 0.099(4) 0.034(3) 0.005(3) 0.002(2) -0.011(3)
C30 0.053(3) 0.212(8) 0.053(4) 0.011(4) 0.005(3) -0.015(4)
C31 0.096(4) 0.079(4) 0.049(3) 0.011(3) 0.006(3) -0.048(3)
C32 0.230(8) 0.081(5) 0.092(5) -0.005(4) 0.017(5) -0.089(5)
C33 0.063(3) 0.044(3) 0.039(3) 0.006(2) 0.018(2) 0.008(2)
C34 0.053(3) 0.070(4) 0.056(3) 0.005(3) 0.013(2) 0.013(2)
C35 0.065(3) 0.063(4) 0.035(3) 0.007(2) 0.009(2) -0.016(2)
C36 0.159(6) 0.070(4) 0.060(4) 0.013(3) 0.003(3) -0.046(4)
C37 0.056(3) 0.103(4) 0.038(3) 0.007(3) -0.003(2) -0.013(3)
C38 0.056(3) 0.224(8) 0.068(4) 0.018(5) -0.014(3) -0.034(4)
C39 0.044(2) 0.059(3) 0.048(3) -0.004(2) 0.013(2) 0.009(2)
C40 0.072(3) 0.053(3) 0.077(4) 0.011(3) 0.019(3) 0.024(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
Fe1 C1 1.758(5) . ?
Fe1 C2 1.771(4) . ?
Fe1 C3 1.774(5) . ?
Fe1 S1 2.1219(10) . ?
Fe1 Fe2 2.6333(8) . ?
Fe1 Fe3 2.6495(7) . ?
Fe2 C6 1.768(4) . ?
Fe2 C5 1.770(5) . ?
Fe2 C4 1.783(5) . ?
Fe2 S1 2.1224(11) . ?
Fe2 Fe3 2.6380(8) . ?
Fe3 C9 1.786(5) . ?
Fe3 C8 1.790(5) . ?
Fe3 C7 1.796(4) . ?
Fe3 S1 2.1327(11) . ?
Fe4 C15 1.758(5) . ?
Fe4 C14 1.776(4) . ?
Fe4 C13 1.782(5) . ?
Fe4 S2 2.1255(10) . ?
Fe4 Fe6 2.6299(7) . ?
Fe4 Fe5 2.6364(7) . ?
Fe5 C16 1.779(4) . ?
Fe5 C18 1.782(4) . ?
Fe5 C17 1.787(5) . ?
Fe5 S2 2.1311(11) . ?
Fe5 Fe6 2.6435(8) . ?
Fe6 C19 1.759(4) . ?
Fe6 C20 1.771(5) . ?
Fe6 C21 1.779(5) . ?
Fe6 S2 2.1260(11) . ?
Cl1 C12 1.780(4) . ?
Cl2 C24 1.788(5) . ?
S1 C10 1.827(3) . ?
S2 C22 1.816(4) . ?
O1 C1 1.163(5) . ?
O2 C2 1.157(4) . ?
O3 C3 1.154(5) . ?
O4 C4 1.153(5) . ?
O5 C5 1.154(5) . ?
O6 C6 1.156(4) . ?
O7 C7 1.135(4) . ?
O8 C8 1.138(5) . ?
O9 C9 1.149(5) . ?
O13 C13 1.151(5) . ?
O14 C14 1.151(4) . ?
O15 C15 1.155(5) . ?
O16 C16 1.143(4) . ?
O17 C17 1.144(5) . ?
O18 C18 1.145(4) . ?
O19 C19 1.167(4) . ?
O20 C20 1.155(5) . ?
O21 C21 1.156(5) . ?
N1 C31 1.501(5) . ?
N1 C25 1.509(5) . ?
N1 C27 1.523(5) . ?
N1 C29 1.523(5) . ?
N2 C39 1.505(5) . ?
N2 C35 1.510(5) . ?
N2 C37 1.518(5) . ?
N2 C33 1.524(5) . ?
C10 C11 1.513(5) . ?
C11 C12 1.514(5) . ?
C22 C23 1.507(5) . ?
C23 C24 1.508(6) . ?
C25 C26 1.516(5) . ?
C27 C28 1.497(6) . ?
C29 C30 1.510(6) . ?
C31 C32 1.500(7) . ?
C33 C34 1.517(6) . ?
C35 C36 1.511(7) . ?
C37 C38 1.509(6) . ?
C39 C40 1.509(6) . ?

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
C1 Fe1 C2 100.51(19) . . ?
C1 Fe1 C3 100.5(2) . . ?
C2 Fe1 C3 98.3(2) . . ?
C1 Fe1 S1 107.97(12) . . ?
C2 Fe1 S1 139.27(13) . . ?
C3 Fe1 S1 104.26(13) . . ?
C1 Fe1 Fe2 152.82(13) . . ?
C2 Fe1 Fe2 90.86(13) . . ?
C3 Fe1 Fe2 102.17(15) . . ?
S1 Fe1 Fe2 51.66(3) . . ?
C1 Fe1 Fe3 93.74(13) . . ?
C2 Fe1 Fe3 98.84(14) . . ?
C3 Fe1 Fe3 155.24(13) . . ?
S1 Fe1 Fe3 51.67(3) . . ?
Fe2 Fe1 Fe3 59.92(2) . . ?
C6 Fe2 C5 98.51(19) . . ?
C6 Fe2 C4 99.12(18) . . ?
C5 Fe2 C4 101.2(2) . . ?
C6 Fe2 S1 104.29(12) . . ?
C5 Fe2 S1 106.57(15) . . ?
C4 Fe2 S1 140.12(13) . . ?
C6 Fe2 Fe1 155.26(12) . . ?
C5 Fe2 Fe1 94.82(15) . . ?
C4 Fe2 Fe1 98.58(13) . . ?
S1 Fe2 Fe1 51.65(3) . . ?
C6 Fe2 Fe3 101.80(13) . . ?
C5 Fe2 Fe3 153.51(15) . . ?
C4 Fe2 Fe3 92.17(13) . . ?
S1 Fe2 Fe3 51.86(3) . . ?
Fe1 Fe2 Fe3 60.35(2) . . ?
C9 Fe3 C8 100.20(19) . . ?
C9 Fe3 C7 97.94(19) . . ?
C8 Fe3 C7 99.34(19) . . ?
C9 Fe3 S1 138.67(14) . . ?
C8 Fe3 S1 104.00(14) . . ?
C7 Fe3 S1 110.39(13) . . ?
C9 Fe3 Fe2 98.94(14) . . ?
C8 Fe3 Fe2 155.36(14) . . ?
C7 Fe3 Fe2 93.23(13) . . ?
S1 Fe3 Fe2 51.51(3) . . ?
C9 Fe3 Fe1 90.43(13) . . ?
C8 Fe3 Fe1 104.68(13) . . ?
C7 Fe3 Fe1 152.72(13) . . ?
S1 Fe3 Fe1 51.30(3) . . ?
Fe2 Fe3 Fe1 59.74(2) . . ?
C15 Fe4 C14 97.96(18) . . ?
C15 Fe4 C13 101.1(2) . . ?
C14 Fe4 C13 100.94(19) . . ?
C15 Fe4 S2 109.90(13) . . ?
C14 Fe4 S2 137.77(12) . . ?
C13 Fe4 S2 103.91(13) . . ?
C15 Fe4 Fe6 153.18(13) . . ?
C14 Fe4 Fe6 89.83(12) . . ?
C13 Fe4 Fe6 102.53(14) . . ?
S2 Fe4 Fe6 51.80(3) . . ?
C15 Fe4 Fe5 93.23(13) . . ?
C14 Fe4 Fe5 96.85(12) . . ?
C13 Fe4 Fe5 155.26(13) . . ?
S2 Fe4 Fe5 51.83(3) . . ?
Fe6 Fe4 Fe5 60.26(2) . . ?
C16 Fe5 C18 97.94(19) . . ?
C16 Fe5 C17 99.21(19) . . ?
C18 Fe5 C17 100.03(19) . . ?
C16 Fe5 S2 139.89(14) . . ?
C18 Fe5 S2 110.47(13) . . ?
C17 Fe5 S2 102.87(14) . . ?
C16 Fe5 Fe4 90.13(13) . . ?
C18 Fe5 Fe4 150.64(14) . . ?
C17 Fe5 Fe4 106.49(14) . . ?
S2 Fe5 Fe4 51.64(3) . . ?
C16 Fe5 Fe6 102.11(14) . . ?
C18 Fe5 Fe6 90.92(14) . . ?
C17 Fe5 Fe6 154.40(14) . . ?
S2 Fe5 Fe6 51.53(3) . . ?
Fe4 Fe5 Fe6 59.75(2) . . ?
C19 Fe6 C20 99.93(19) . . ?
C19 Fe6 C21 99.24(18) . . ?
C20 Fe6 C21 101.2(2) . . ?
C19 Fe6 S2 104.79(13) . . ?
C20 Fe6 S2 107.01(16) . . ?
C21 Fe6 S2 138.73(14) . . ?
C19 Fe6 Fe4 156.34(13) . . ?
C20 Fe6 Fe4 91.58(15) . . ?
C21 Fe6 Fe4 98.71(13) . . ?
S2 Fe6 Fe4 51.78(3) . . ?
C19 Fe6 Fe5 104.67(13) . . ?
C20 Fe6 Fe5 150.88(15) . . ?
C21 Fe6 Fe5 90.11(14) . . ?
S2 Fe6 Fe5 51.70(3) . . ?
Fe4 Fe6 Fe5 59.99(2) . . ?
C10 S1 Fe1 132.23(12) . . ?
C10 S1 Fe2 131.59(13) . . ?
Fe1 S1 Fe2 76.69(4) . . ?
C10 S1 Fe3 138.48(13) . . ?
Fe1 S1 Fe3 77.03(4) . . ?
Fe2 S1 Fe3 76.63(4) . . ?
C22 S2 Fe4 133.84(12) . . ?
C22 S2 Fe6 132.15(13) . . ?
Fe4 S2 Fe6 76.43(4) . . ?
C22 S2 Fe5 136.86(13) . . ?
Fe4 S2 Fe5 76.54(4) . . ?
Fe6 S2 Fe5 76.77(4) . . ?
C31 N1 C25 111.3(4) . . ?
C31 N1 C27 106.6(3) . . ?
C25 N1 C27 110.3(3) . . ?
C31 N1 C29 112.0(3) . . ?
C25 N1 C29 106.4(3) . . ?
C27 N1 C29 110.2(4) . . ?
C39 N2 C35 106.8(3) . . ?
C39 N2 C37 111.1(3) . . ?
C35 N2 C37 111.5(3) . . ?
C39 N2 C33 110.8(3) . . ?
C35 N2 C33 110.7(3) . . ?
C37 N2 C33 105.9(3) . . ?
O1 C1 Fe1 178.6(4) . . ?
O2 C2 Fe1 177.2(4) . . ?
O3 C3 Fe1 178.6(5) . . ?
O4 C4 Fe2 178.7(4) . . ?
O5 C5 Fe2 179.0(4) . . ?
O6 C6 Fe2 178.2(4) . . ?
O7 C7 Fe3 178.2(4) . . ?
O8 C8 Fe3 178.7(4) . . ?
O9 C9 Fe3 177.6(4) . . ?
C11 C10 S1 111.3(3) . . ?
C10 C11 C12 115.2(3) . . ?
C11 C12 Cl1 111.7(3) . . ?
O13 C13 Fe4 178.6(4) . . ?
O14 C14 Fe4 177.3(4) . . ?
O15 C15 Fe4 176.4(4) . . ?
O16 C16 Fe5 177.9(4) . . ?
O17 C17 Fe5 178.4(4) . . ?
O18 C18 Fe5 178.6(4) . . ?
O19 C19 Fe6 179.2(4) . . ?
O20 C20 Fe6 179.3(5) . . ?
O21 C21 Fe6 178.6(4) . . ?
C23 C22 S2 111.8(3) . . ?
C24 C23 C22 115.1(3) . . ?
C23 C24 Cl2 111.8(3) . . ?
N1 C25 C26 115.8(3) . . ?
C28 C27 N1 115.9(3) . . ?
C30 C29 N1 115.9(4) . . ?
C32 C31 N1 114.8(4) . . ?
C34 C33 N2 115.0(3) . . ?
N2 C35 C36 115.7(4) . . ?
C38 C37 N2 114.9(4) . . ?
N2 C39 C40 115.3(3) . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        25.01
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.852
_refine_diff_density_min         -0.929
_refine_diff_density_rms         0.271

#=============================================END

data_3
_database_code_depnum_ccdc_archive 'CCDC 817583'
#TrackingRef '- cif-S-Fe-RX-2011-NJC-revised.cif'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C21 H28 Fe3 I N O9 S'
_chemical_formula_sum            'C21 H28 Fe3 I N O9 S'
_chemical_formula_weight         764.95

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'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 '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/n'

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

_cell_length_a                   10.9444(12)
_cell_length_b                   14.5380(16)
_cell_length_c                   18.351(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 94.977(2)
_cell_angle_gamma                90.00
_cell_volume                     2908.9(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    200(2)
_cell_measurement_reflns_used    0
_cell_measurement_theta_min      0
_cell_measurement_theta_max      0

_exptl_crystal_description       prism
_exptl_crystal_colour            red-brown(dark)
_exptl_crystal_size_max          0.58
_exptl_crystal_size_mid          0.47
_exptl_crystal_size_min          0.41
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.747
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1520
_exptl_absorpt_coefficient_mu    2.654
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.3082
_exptl_absorpt_correction_T_max  0.4091
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      200(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            19812
_diffrn_reflns_av_R_equivalents  0.0261
_diffrn_reflns_av_sigmaI/netI    0.0250
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         1.79
_diffrn_reflns_theta_max         25.01
_reflns_number_total             5033
_reflns_number_gt                4285
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1986)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0297P)^2^+6.7890P] 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    noref
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5033
_refine_ls_number_parameters     323
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0447
_refine_ls_R_factor_gt           0.0360
_refine_ls_wR_factor_ref         0.0844
_refine_ls_wR_factor_gt          0.0801
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_restrained_S_all      1.035
_refine_ls_shift/su_max          0.001
_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
C1 C 0.8871(4) 0.6992(3) 0.2452(2) 0.0401(10) Uani 1 1 d . . .
C2 C 0.6339(4) 0.7096(3) 0.2346(2) 0.0452(10) Uani 1 1 d . . .
C3 C 0.7615(4) 0.8345(3) 0.1727(2) 0.0396(9) Uani 1 1 d . . .
C4 C 0.4870(4) 0.6771(3) 0.0874(2) 0.0495(11) Uani 1 1 d . . .
C5 C 0.6290(4) 0.8040(3) 0.0269(2) 0.0427(10) Uani 1 1 d . . .
C6 C 0.5986(4) 0.6362(4) -0.0360(3) 0.0528(12) Uani 1 1 d . . .
C7 C 0.9080(4) 0.7968(3) 0.0521(2) 0.0368(9) Uani 1 1 d . . .
C8 C 0.8800(4) 0.6392(3) -0.0301(2) 0.0396(9) Uani 1 1 d . . .
C9 C 1.0201(4) 0.6393(3) 0.1005(2) 0.0368(9) Uani 1 1 d . . .
C10 C 0.7535(5) 0.4694(3) 0.1311(3) 0.0595(13) Uani 1 1 d . A .
H10A H 0.8208 0.4558 0.1692 0.071 Uiso 1 1 calc R . .
H10B H 0.6754 0.4513 0.1507 0.071 Uiso 1 1 calc R . .
C11 C 0.7707(5) 0.4140(3) 0.0660(3) 0.0575(13) Uani 1 1 d . . .
H11A H 0.8537 0.4236 0.0498 0.069 Uiso 1 1 d R A .
H11B H 0.7090 0.4304 0.0254 0.069 Uiso 1 1 d R . .
C12 C 0.7536(6) 0.3120(4) 0.0905(3) 0.0423(14) Uiso 0.70 1 d PD A 1
H12A H 0.7997 0.3018 0.1387 0.051 Uiso 0.70 1 calc PR A 1
H12B H 0.6657 0.3003 0.0959 0.051 Uiso 0.70 1 calc PR A 1
C13 C 0.7975(7) 0.2478(5) 0.0366(4) 0.0624(19) Uiso 0.70 1 d PD A 1
H13A H 0.8868 0.2564 0.0342 0.075 Uiso 0.70 1 calc PR A 1
H13B H 0.7563 0.2617 -0.0123 0.075 Uiso 0.70 1 calc PR A 1
C12' C 0.8118(14) 0.3124(12) 0.0547(10) 0.064(5) Uiso 0.30 1 d PD A 2
H12C H 0.8282 0.3010 0.0033 0.076 Uiso 0.30 1 calc PR A 2
H12D H 0.8861 0.2971 0.0871 0.076 Uiso 0.30 1 calc PR A 2
C13' C 0.7049(13) 0.2593(11) 0.0746(9) 0.051(4) Uiso 0.30 1 d PD A 2
H13C H 0.6316 0.2733 0.0409 0.061 Uiso 0.30 1 calc PR A 2
H13D H 0.6864 0.2733 0.1253 0.061 Uiso 0.30 1 calc PR A 2
C14 C 0.3665(4) 0.9909(3) 0.2123(2) 0.0433(10) Uani 1 1 d . . .
H14A H 0.3794 1.0563 0.2260 0.052 Uiso 1 1 calc R . .
H14B H 0.3891 0.9535 0.2565 0.052 Uiso 1 1 calc R . .
C15 C 0.4521(5) 0.9669(4) 0.1552(3) 0.0726(16) Uani 1 1 d . . .
H15A H 0.5368 0.9794 0.1744 0.109 Uiso 1 1 calc R . .
H15B H 0.4318 1.0042 0.1113 0.109 Uiso 1 1 calc R . .
H15C H 0.4434 0.9016 0.1428 0.109 Uiso 1 1 calc R . .
C16 C 0.2061(4) 0.8779(3) 0.1681(2) 0.0457(10) Uani 1 1 d . . .
H16A H 0.2516 0.8636 0.1251 0.055 Uiso 1 1 calc R . .
H16B H 0.1175 0.8715 0.1528 0.055 Uiso 1 1 calc R . .
C17 C 0.2406(5) 0.8080(3) 0.2273(3) 0.0577(13) Uani 1 1 d . . .
H17A H 0.2212 0.7461 0.2086 0.087 Uiso 1 1 calc R . .
H17B H 0.1944 0.8203 0.2697 0.087 Uiso 1 1 calc R . .
H17C H 0.3287 0.8123 0.2420 0.087 Uiso 1 1 calc R . .
C18 C 0.1639(4) 1.0029(3) 0.2559(2) 0.0381(9) Uani 1 1 d . . .
H18A H 0.1988 0.9671 0.2987 0.046 Uiso 1 1 calc R . .
H18B H 0.1793 1.0688 0.2668 0.046 Uiso 1 1 calc R . .
C19 C 0.0276(4) 0.9872(4) 0.2468(3) 0.0581(13) Uani 1 1 d . . .
H19A H -0.0085 1.0058 0.2916 0.087 Uiso 1 1 calc R . .
H19B H 0.0111 0.9218 0.2375 0.087 Uiso 1 1 calc R . .
H19C H -0.0085 1.0237 0.2055 0.087 Uiso 1 1 calc R . .
C20 C 0.1901(4) 1.0360(3) 0.1243(2) 0.0421(10) Uani 1 1 d . . .
H20A H 0.2375 1.0180 0.0830 0.051 Uiso 1 1 calc R . .
H20B H 0.1027 1.0225 0.1097 0.051 Uiso 1 1 calc R . .
C21 C 0.2038(5) 1.1379(3) 0.1358(2) 0.0527(12) Uani 1 1 d . . .
H21A H 0.1737 1.1703 0.0910 0.079 Uiso 1 1 calc R . .
H21B H 0.2905 1.1528 0.1480 0.079 Uiso 1 1 calc R . .
H21C H 0.1562 1.1570 0.1760 0.079 Uiso 1 1 calc R . .
N1 N 0.2315(3) 0.9766(2) 0.18987(15) 0.0314(7) Uani 1 1 d . . .
O1 O 0.9710(3) 0.6933(3) 0.28705(18) 0.0632(9) Uani 1 1 d . . .
O2 O 0.5507(3) 0.7126(3) 0.26884(19) 0.0707(10) Uani 1 1 d . . .
O3 O 0.7620(3) 0.9137(2) 0.17203(19) 0.0586(9) Uani 1 1 d . . .
O4 O 0.3927(3) 0.6721(3) 0.1108(2) 0.0813(12) Uani 1 1 d . . .
O5 O 0.6247(3) 0.8797(2) 0.00975(19) 0.0620(9) Uani 1 1 d . . .
O6 O 0.5756(4) 0.6059(3) -0.0928(2) 0.0919(14) Uani 1 1 d . . .
O7 O 0.9337(3) 0.8731(2) 0.04512(18) 0.0539(8) Uani 1 1 d . . .
O8 O 0.8858(3) 0.6165(2) -0.08944(17) 0.0618(9) Uani 1 1 d . . .
O9 O 1.1129(3) 0.6124(2) 0.12526(18) 0.0581(9) Uani 1 1 d . . .
S1 S 0.75034(9) 0.59214(6) 0.11342(5) 0.0336(2) Uani 1 1 d . . .
Fe1 Fe 0.75902(5) 0.71306(4) 0.17939(3) 0.03174(14) Uani 1 1 d . A .
Fe2 Fe 0.63255(5) 0.68568(4) 0.05228(3) 0.03381(14) Uani 1 1 d . A .
Fe3 Fe 0.87461(5) 0.67807(4) 0.06202(3) 0.02938(14) Uani 1 1 d . A .
I1 I 0.76226(4) 0.10768(2) 0.064010(17) 0.06474(13) Uani 1 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
C1 0.043(3) 0.040(2) 0.038(2) -0.0044(18) 0.0072(19) 0.0058(19)
C2 0.045(3) 0.052(3) 0.039(2) -0.004(2) 0.006(2) -0.003(2)
C3 0.038(2) 0.043(3) 0.037(2) -0.0024(18) -0.0008(17) 0.0007(19)
C4 0.038(3) 0.062(3) 0.048(2) -0.005(2) 0.001(2) -0.005(2)
C5 0.036(2) 0.057(3) 0.036(2) 0.003(2) 0.0021(17) 0.004(2)
C6 0.039(3) 0.069(3) 0.050(3) -0.015(2) 0.000(2) 0.006(2)
C7 0.029(2) 0.041(3) 0.040(2) 0.0038(18) 0.0012(16) 0.0002(18)
C8 0.038(2) 0.039(2) 0.042(2) 0.0020(19) 0.0042(18) -0.0007(19)
C9 0.037(2) 0.039(2) 0.035(2) 0.0039(17) 0.0093(18) 0.0004(19)
C10 0.091(4) 0.033(2) 0.054(3) 0.012(2) 0.004(3) -0.011(2)
C11 0.055(3) 0.030(2) 0.086(4) -0.004(2) 0.000(3) 0.003(2)
C14 0.034(2) 0.047(3) 0.049(2) 0.001(2) 0.0028(18) -0.0030(19)
C15 0.055(3) 0.078(4) 0.089(4) 0.005(3) 0.032(3) 0.011(3)
C16 0.058(3) 0.032(2) 0.046(2) -0.0073(18) -0.004(2) -0.005(2)
C17 0.082(4) 0.031(2) 0.059(3) 0.004(2) 0.004(3) 0.002(2)
C18 0.040(2) 0.042(2) 0.0322(19) -0.0017(17) 0.0063(17) 0.0015(19)
C19 0.039(3) 0.070(3) 0.066(3) 0.014(3) 0.007(2) 0.002(2)
C20 0.058(3) 0.040(2) 0.0278(19) 0.0019(17) -0.0010(18) 0.005(2)
C21 0.081(4) 0.035(2) 0.043(2) 0.0055(19) 0.012(2) 0.011(2)
N1 0.0391(19) 0.0288(17) 0.0258(15) -0.0037(13) -0.0011(13) 0.0001(14)
O1 0.051(2) 0.082(3) 0.0539(19) -0.0041(18) -0.0106(16) 0.0199(18)
O2 0.048(2) 0.106(3) 0.061(2) -0.008(2) 0.0210(17) -0.005(2)
O3 0.065(2) 0.039(2) 0.071(2) -0.0051(16) -0.0008(17) 0.0022(16)
O4 0.036(2) 0.135(4) 0.075(2) -0.001(2) 0.0160(18) -0.010(2)
O5 0.065(2) 0.053(2) 0.068(2) 0.0181(18) 0.0045(17) 0.0086(17)
O6 0.075(3) 0.139(4) 0.058(2) -0.051(2) -0.0163(19) 0.013(3)
O7 0.057(2) 0.0376(19) 0.067(2) 0.0084(15) 0.0046(16) -0.0108(15)
O8 0.072(2) 0.076(2) 0.0382(18) -0.0118(16) 0.0091(15) -0.0009(19)
O9 0.0399(19) 0.071(2) 0.062(2) 0.0131(17) -0.0030(15) 0.0157(17)
S1 0.0405(6) 0.0272(5) 0.0337(5) -0.0001(4) 0.0062(4) -0.0038(4)
Fe1 0.0328(3) 0.0326(3) 0.0300(3) -0.0029(2) 0.0037(2) -0.0003(2)
Fe2 0.0292(3) 0.0398(3) 0.0323(3) -0.0035(2) 0.0022(2) -0.0012(2)
Fe3 0.0297(3) 0.0285(3) 0.0302(3) 0.0015(2) 0.0040(2) 0.0007(2)
I1 0.1136(3) 0.02868(17) 0.05236(19) -0.00196(13) 0.00966(18) -0.01101(17)

_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
C1 O1 1.148(5) . ?
C1 Fe1 1.781(4) . ?
C2 O2 1.152(5) . ?
C2 Fe1 1.773(4) . ?
C3 O3 1.151(5) . ?
C3 Fe1 1.771(5) . ?
C4 O4 1.153(5) . ?
C4 Fe2 1.774(5) . ?
C5 O5 1.144(5) . ?
C5 Fe2 1.782(5) . ?
C6 O6 1.140(5) . ?
C6 Fe2 1.781(5) . ?
C7 O7 1.155(5) . ?
C7 Fe3 1.777(4) . ?
C8 O8 1.146(5) . ?
C8 Fe3 1.787(4) . ?
C9 O9 1.145(5) . ?
C9 Fe3 1.776(4) . ?
C10 C11 1.467(7) . ?
C10 S1 1.813(4) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 C12' 1.564(19) . ?
C11 C12 1.565(8) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 C13 1.472(8) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C13 I1 2.141(8) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C12' C13' 1.474(9) . ?
C12' H12C 0.9900 . ?
C12' H12D 0.9900 . ?
C13' I1 2.305(16) . ?
C13' H13C 0.9900 . ?
C13' H13D 0.9900 . ?
C14 C15 1.505(6) . ?
C14 N1 1.514(5) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 N1 1.508(5) . ?
C16 C17 1.512(6) . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 C19 1.504(6) . ?
C18 N1 1.523(5) . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 C21 1.502(6) . ?
C20 N1 1.519(5) . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
S1 Fe2 2.1258(11) . ?
S1 Fe3 2.1268(11) . ?
S1 Fe1 2.1319(11) . ?
Fe1 Fe2 2.6372(8) . ?
Fe1 Fe3 2.6403(8) . ?
Fe2 Fe3 2.6420(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
O1 C1 Fe1 177.6(4) . . ?
O2 C2 Fe1 175.9(4) . . ?
O3 C3 Fe1 176.5(4) . . ?
O4 C4 Fe2 179.3(5) . . ?
O5 C5 Fe2 178.6(4) . . ?
O6 C6 Fe2 178.7(5) . . ?
O7 C7 Fe3 177.7(4) . . ?
O8 C8 Fe3 177.9(4) . . ?
O9 C9 Fe3 178.5(4) . . ?
C11 C10 S1 113.3(3) . . ?
C11 C10 H10A 108.9 . . ?
S1 C10 H10A 108.9 . . ?
C11 C10 H10B 108.9 . . ?
S1 C10 H10B 108.9 . . ?
H10A C10 H10B 107.7 . . ?
C10 C11 C12' 133.3(8) . . ?
C10 C11 C12 105.0(4) . . ?
C12' C11 C12 35.5(6) . . ?
C10 C11 H11A 110.8 . . ?
C12' C11 H11A 79.1 . . ?
C12 C11 H11A 110.8 . . ?
C10 C11 H11B 110.7 . . ?
C12' C11 H11B 108.3 . . ?
C12 C11 H11B 110.7 . . ?
H11A C11 H11B 108.8 . . ?
C13 C12 C11 110.7(5) . . ?
C13 C12 H12A 109.5 . . ?
C11 C12 H12A 109.5 . . ?
C13 C12 H12B 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 108.1 . . ?
C12 C13 I1 111.7(5) . . ?
C12 C13 H13A 109.3 . . ?
I1 C13 H13A 109.3 . . ?
C12 C13 H13B 109.3 . . ?
I1 C13 H13B 109.3 . . ?
H13A C13 H13B 107.9 . . ?
C13' C12' C11 102.6(13) . . ?
C13' C12' H12C 111.3 . . ?
C11 C12' H12C 111.3 . . ?
C13' C12' H12D 111.3 . . ?
C11 C12' H12D 111.3 . . ?
H12C C12' H12D 109.2 . . ?
C12' C13' I1 104.6(11) . . ?
C12' C13' H13C 110.8 . . ?
I1 C13' H13C 110.8 . . ?
C12' C13' H13D 110.8 . . ?
I1 C13' H13D 110.8 . . ?
H13C C13' H13D 108.9 . . ?
C15 C14 N1 115.5(4) . . ?
C15 C14 H14A 108.4 . . ?
N1 C14 H14A 108.4 . . ?
C15 C14 H14B 108.4 . . ?
N1 C14 H14B 108.4 . . ?
H14A C14 H14B 107.5 . . ?
C14 C15 H15A 109.5 . . ?
C14 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C14 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
N1 C16 C17 114.8(3) . . ?
N1 C16 H16A 108.6 . . ?
C17 C16 H16A 108.6 . . ?
N1 C16 H16B 108.6 . . ?
C17 C16 H16B 108.6 . . ?
H16A C16 H16B 107.5 . . ?
C16 C17 H17A 109.5 . . ?
C16 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C16 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C19 C18 N1 114.8(3) . . ?
C19 C18 H18A 108.6 . . ?
N1 C18 H18A 108.6 . . ?
C19 C18 H18B 108.6 . . ?
N1 C18 H18B 108.6 . . ?
H18A C18 H18B 107.6 . . ?
C18 C19 H19A 109.5 . . ?
C18 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C18 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C21 C20 N1 115.4(3) . . ?
C21 C20 H20A 108.4 . . ?
N1 C20 H20A 108.4 . . ?
C21 C20 H20B 108.4 . . ?
N1 C20 H20B 108.4 . . ?
H20A C20 H20B 107.5 . . ?
C20 C21 H21A 109.5 . . ?
C20 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C20 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C16 N1 C14 110.9(3) . . ?
C16 N1 C20 107.2(3) . . ?
C14 N1 C20 110.8(3) . . ?
C16 N1 C18 111.0(3) . . ?
C14 N1 C18 106.2(3) . . ?
C20 N1 C18 110.9(3) . . ?
C10 S1 Fe2 136.48(18) . . ?
C10 S1 Fe3 130.90(19) . . ?
Fe2 S1 Fe3 76.82(4) . . ?
C10 S1 Fe1 135.26(16) . . ?
Fe2 S1 Fe1 76.54(4) . . ?
Fe3 S1 Fe1 76.63(4) . . ?
C3 Fe1 C2 94.9(2) . . ?
C3 Fe1 C1 98.30(19) . . ?
C2 Fe1 C1 102.18(19) . . ?
C3 Fe1 S1 141.53(13) . . ?
C2 Fe1 S1 107.60(15) . . ?
C1 Fe1 S1 106.58(13) . . ?
C3 Fe1 Fe2 95.67(13) . . ?
C2 Fe1 Fe2 97.41(14) . . ?
C1 Fe1 Fe2 154.77(13) . . ?
S1 Fe1 Fe2 51.62(3) . . ?
C3 Fe1 Fe3 97.12(13) . . ?
C2 Fe1 Fe3 155.36(14) . . ?
C1 Fe1 Fe3 97.27(13) . . ?
S1 Fe1 Fe3 51.60(3) . . ?
Fe2 Fe1 Fe3 60.08(2) . . ?
C4 Fe2 C6 100.3(2) . . ?
C4 Fe2 C5 99.4(2) . . ?
C6 Fe2 C5 98.9(2) . . ?
C4 Fe2 S1 106.62(16) . . ?
C6 Fe2 S1 106.89(16) . . ?
C5 Fe2 S1 138.93(14) . . ?
C4 Fe2 Fe1 96.23(14) . . ?
C6 Fe2 Fe1 156.49(15) . . ?
C5 Fe2 Fe1 94.77(13) . . ?
S1 Fe2 Fe1 51.83(3) . . ?
C4 Fe2 Fe3 154.08(15) . . ?
C6 Fe2 Fe3 99.97(14) . . ?
C5 Fe2 Fe3 93.26(14) . . ?
S1 Fe2 Fe3 51.61(3) . . ?
Fe1 Fe2 Fe3 60.02(2) . . ?
C9 Fe3 C7 99.40(18) . . ?
C9 Fe3 C8 100.01(18) . . ?
C7 Fe3 C8 100.71(19) . . ?
C9 Fe3 S1 102.89(13) . . ?
C7 Fe3 S1 139.59(13) . . ?
C8 Fe3 S1 107.96(14) . . ?
C9 Fe3 Fe1 102.30(12) . . ?
C7 Fe3 Fe1 90.82(13) . . ?
C8 Fe3 Fe1 152.80(13) . . ?
S1 Fe3 Fe1 51.77(3) . . ?
C9 Fe3 Fe2 154.03(13) . . ?
C7 Fe3 Fe2 99.59(13) . . ?
C8 Fe3 Fe2 93.69(13) . . ?
S1 Fe3 Fe2 51.57(3) . . ?
Fe1 Fe3 Fe2 59.90(2) . . ?
C13 I1 C13' 33.5(4) . . ?

_diffrn_measured_fraction_theta_max 0.985
_diffrn_reflns_theta_full        25.01
_diffrn_measured_fraction_theta_full 0.985
_refine_diff_density_max         0.932
_refine_diff_density_min         -1.459
_refine_diff_density_rms         0.075

#=============================================END

data_4
_database_code_depnum_ccdc_archive 'CCDC 817584'
#TrackingRef '- cif-S-Fe-RX-2011-NJC-revised.cif'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C34 H40 Fe6 Hg N2 O18 S2'
_chemical_formula_sum            'C34 H40 Fe6 Hg N2 O18 S2'
_chemical_formula_weight         1364.49

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'
Hg Hg -2.3894 9.2266 '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   'P 2/n'

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

_cell_length_a                   13.0224(2)
_cell_length_b                   8.5294(1)
_cell_length_c                   22.1409(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 103.8128(9)
_cell_angle_gamma                90.00
_cell_volume                     2388.14(6)
_cell_formula_units_Z            2
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    16881
_cell_measurement_theta_min      2.037
_cell_measurement_theta_max      25.028

_exptl_crystal_description       prism
_exptl_crystal_colour            black
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.22
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.898
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1340
_exptl_absorpt_coefficient_mu    5.129
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.2451
_exptl_absorpt_correction_T_max  0.3104
_exptl_absorpt_process_details   
;
?
;

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      298(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  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            12887
_diffrn_reflns_av_R_equivalents  0.0378
_diffrn_reflns_av_sigmaI/netI    0.0362
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         2.05
_diffrn_reflns_theta_max         25.04
_reflns_number_total             4205
_reflns_number_gt                3830
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_reduction        
'HKL Denzo and Scalepack (Otwinowski & Minor 19'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0587P)^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    noref
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.0102(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_number_reflns         4205
_refine_ls_number_parameters     286
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0441
_refine_ls_R_factor_gt           0.0348
_refine_ls_wR_factor_ref         0.0978
_refine_ls_wR_factor_gt          0.0885
_refine_ls_goodness_of_fit_ref   1.183
_refine_ls_restrained_S_all      1.183
_refine_ls_shift/su_max          0.009
_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
Hg1 Hg 0.7500 0.82181(3) 0.2500 0.04064(13) Uani 1 2 d S . .
Fe1 Fe 0.57397(5) 0.96635(7) 0.27018(3) 0.04373(19) Uani 1 1 d . . .
Fe2 Fe 0.55801(6) 0.88068(9) 0.38036(3) 0.0502(2) Uani 1 1 d . . .
Fe3 Fe 0.62974(6) 0.66755(7) 0.31737(3) 0.04197(19) Uani 1 1 d . . .
S1 S 0.47321(10) 0.77808(15) 0.29208(5) 0.0470(3) Uani 1 1 d . . .
O1 O 0.5466(3) 0.9813(5) 0.13502(16) 0.0706(11) Uani 1 1 d . . .
O2 O 0.4125(5) 1.2080(6) 0.2547(3) 0.1090(19) Uani 1 1 d . . .
O3 O 0.7371(4) 1.1956(4) 0.3271(2) 0.0715(11) Uani 1 1 d . . .
O4 O 0.4118(4) 1.1227(6) 0.4016(3) 0.0986(16) Uani 1 1 d . . .
O5 O 0.7587(4) 1.0019(6) 0.4552(2) 0.1002(16) Uani 1 1 d . . .
O6 O 0.5204(5) 0.6821(5) 0.4799(2) 0.0943(17) Uani 1 1 d . . .
O7 O 0.8445(4) 0.6666(5) 0.39801(19) 0.0762(12) Uani 1 1 d . . .
O8 O 0.5727(4) 0.4119(5) 0.3896(2) 0.0833(13) Uani 1 1 d . . .
O9 O 0.6123(3) 0.4469(4) 0.21399(18) 0.0693(10) Uani 1 1 d . . .
N1 N 0.3100(3) 0.5587(5) 0.08589(16) 0.0527(10) Uani 1 1 d . . .
C1 C 0.5618(4) 0.9693(6) 0.1876(2) 0.0511(11) Uani 1 1 d . . .
C2 C 0.4757(5) 1.1113(7) 0.2625(3) 0.0647(14) Uani 1 1 d . . .
C3 C 0.6768(5) 1.1017(6) 0.3053(2) 0.0531(12) Uani 1 1 d . . .
C4 C 0.4704(6) 1.0325(7) 0.3929(3) 0.0686(15) Uani 1 1 d . . .
C5 C 0.6800(5) 0.9564(7) 0.4243(2) 0.0709(17) Uani 1 1 d . . .
C6 C 0.5348(5) 0.7574(7) 0.4399(2) 0.0624(14) Uani 1 1 d . . .
C7 C 0.7619(5) 0.6721(5) 0.3653(2) 0.0524(13) Uani 1 1 d . . .
C8 C 0.5939(4) 0.5146(6) 0.3622(2) 0.0561(13) Uani 1 1 d . . .
C9 C 0.6224(4) 0.5373(5) 0.2532(2) 0.0487(11) Uani 1 1 d . . .
C10 C 0.2827(5) 0.5999(8) 0.0174(2) 0.0742(17) Uani 1 1 d . . .
H10A H 0.2559 0.5072 -0.0056 0.089 Uiso 1 1 d R . .
H10B H 0.2295 0.6802 0.0093 0.089 Uiso 1 1 d R . .
C11 C 0.3730(8) 0.6594(8) -0.0079(4) 0.108(3) Uani 1 1 d . . .
H11A H 0.3455 0.6790 -0.0515 0.129 Uiso 1 1 d R . .
H11B H 0.4278 0.5818 -0.0025 0.129 Uiso 1 1 d R . .
H11C H 0.4014 0.7548 0.0125 0.129 Uiso 1 1 d R . .
C12 C 0.3566(5) 0.6964(6) 0.1260(3) 0.0671(15) Uani 1 1 d . . .
H12A H 0.3750 0.6654 0.1689 0.081 Uiso 1 1 d R . .
H12B H 0.4190 0.7304 0.1139 0.081 Uiso 1 1 d R . .
C13 C 0.2845(6) 0.8386(7) 0.1211(4) 0.087(2) Uani 1 1 d . . .
H13A H 0.3193 0.9220 0.1473 0.105 Uiso 1 1 d R . .
H13B H 0.2217 0.8085 0.1338 0.105 Uiso 1 1 d R . .
H13C H 0.2658 0.8735 0.0787 0.105 Uiso 1 1 d R . .
C14 C 0.2087(5) 0.5023(7) 0.1016(3) 0.0757(17) Uani 1 1 d . . .
H14A H 0.1569 0.5842 0.0917 0.091 Uiso 1 1 d R . .
H14B H 0.1832 0.4108 0.0774 0.091 Uiso 1 1 d R . .
C15 C 0.2180(6) 0.4602(9) 0.1683(3) 0.097(2) Uani 1 1 d . . .
H15A H 0.1506 0.4271 0.1742 0.116 Uiso 1 1 d R . .
H15B H 0.2419 0.5500 0.1940 0.116 Uiso 1 1 d R . .
H15C H 0.2682 0.3766 0.1797 0.116 Uiso 1 1 d R . .
C16 C 0.3938(5) 0.4317(7) 0.0993(2) 0.0656(14) Uani 1 1 d . . .
H16A H 0.4541 0.4684 0.0855 0.079 Uiso 1 1 d R . .
H16B H 0.4143 0.4097 0.1430 0.079 Uiso 1 1 d R . .
C17 C 0.3634(8) 0.2817(8) 0.0646(4) 0.103(3) Uani 1 1 d . . .
H17A H 0.4199 0.2067 0.0738 0.124 Uiso 1 1 d R . .
H17B H 0.3435 0.3004 0.0206 0.124 Uiso 1 1 d R . .
H17C H 0.3037 0.2417 0.0782 0.124 Uiso 1 1 d R . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Hg1 0.04231(18) 0.03783(19) 0.04182(18) 0.000 0.01014(11) 0.000
Fe1 0.0471(4) 0.0378(4) 0.0465(4) 0.0021(3) 0.0114(3) 0.0046(3)
Fe2 0.0609(5) 0.0473(4) 0.0434(4) -0.0067(3) 0.0145(3) -0.0069(3)
Fe3 0.0459(4) 0.0361(4) 0.0431(4) 0.0016(2) 0.0090(3) -0.0033(3)
S1 0.0424(7) 0.0491(7) 0.0487(6) -0.0037(5) 0.0094(5) -0.0039(5)
O1 0.075(3) 0.087(3) 0.0463(19) 0.0101(18) 0.0078(17) 0.009(2)
O2 0.108(4) 0.107(4) 0.116(4) 0.019(3) 0.035(3) 0.069(3)
O3 0.085(3) 0.050(2) 0.080(3) -0.0141(19) 0.021(2) -0.015(2)
O4 0.114(4) 0.070(3) 0.125(4) -0.022(3) 0.055(3) 0.017(3)
O5 0.108(4) 0.100(4) 0.078(3) -0.008(2) -0.008(3) -0.046(3)
O6 0.128(5) 0.099(4) 0.054(2) 0.011(2) 0.018(3) -0.039(3)
O7 0.060(3) 0.096(3) 0.060(2) 0.0156(19) -0.008(2) -0.005(2)
O8 0.102(4) 0.068(3) 0.085(3) 0.021(2) 0.032(3) -0.021(3)
O9 0.079(3) 0.058(2) 0.067(2) -0.0201(19) 0.0104(19) -0.007(2)
N1 0.055(3) 0.053(2) 0.043(2) -0.0017(18) -0.0006(17) 0.000(2)
C1 0.045(3) 0.047(3) 0.061(3) 0.005(2) 0.011(2) 0.006(2)
C2 0.074(4) 0.058(3) 0.065(3) 0.004(3) 0.023(3) 0.014(3)
C3 0.068(3) 0.040(3) 0.053(3) 0.001(2) 0.017(2) 0.007(3)
C4 0.085(4) 0.065(4) 0.062(3) -0.014(3) 0.030(3) -0.009(3)
C5 0.092(5) 0.065(4) 0.052(3) -0.005(3) 0.011(3) -0.021(3)
C6 0.071(4) 0.064(3) 0.050(3) -0.009(3) 0.009(3) -0.019(3)
C7 0.060(4) 0.051(3) 0.045(3) 0.007(2) 0.012(3) -0.003(2)
C8 0.058(3) 0.049(3) 0.061(3) 0.000(2) 0.013(2) -0.005(2)
C9 0.047(3) 0.042(3) 0.055(3) 0.001(2) 0.009(2) -0.002(2)
C10 0.098(5) 0.066(4) 0.051(3) 0.009(3) 0.004(3) 0.017(3)
C11 0.161(9) 0.094(6) 0.084(5) 0.035(4) 0.059(5) 0.047(5)
C12 0.067(4) 0.065(4) 0.067(3) -0.012(3) 0.011(3) -0.007(3)
C13 0.101(6) 0.064(4) 0.101(5) -0.016(3) 0.032(4) -0.002(4)
C14 0.047(3) 0.067(4) 0.104(5) 0.010(3) 0.001(3) -0.004(3)
C15 0.086(5) 0.105(6) 0.111(5) 0.035(4) 0.043(4) 0.009(4)
C16 0.064(4) 0.072(4) 0.059(3) 0.008(3) 0.009(3) 0.013(3)
C17 0.153(8) 0.063(4) 0.095(5) 0.010(4) 0.034(5) 0.027(5)

_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
Hg1 Fe1 2.7318(7) 2_655 ?
Hg1 Fe1 2.7318(7) . ?
Hg1 Fe3 2.7430(7) 2_655 ?
Hg1 Fe3 2.7430(7) . ?
Fe1 C2 1.758(6) . ?
Fe1 C3 1.798(6) . ?
Fe1 C1 1.797(5) . ?
Fe1 S1 2.1997(14) . ?
Fe1 Fe2 2.6020(9) . ?
Fe1 Fe3 2.7842(9) . ?
Fe2 C6 1.767(6) . ?
Fe2 C5 1.774(6) . ?
Fe2 C4 1.791(7) . ?
Fe2 S1 2.1852(13) . ?
Fe2 Fe3 2.5969(10) . ?
Fe3 C8 1.768(5) . ?
Fe3 C9 1.789(5) . ?
Fe3 C7 1.794(6) . ?
Fe3 S1 2.1936(14) . ?
O1 C1 1.138(6) . ?
O2 C2 1.148(7) . ?
O3 C3 1.145(6) . ?
O4 C4 1.132(7) . ?
O5 C5 1.155(7) . ?
O6 C6 1.146(7) . ?
O7 C7 1.145(7) . ?
O8 C8 1.135(6) . ?
O9 C9 1.145(5) . ?
N1 C10 1.514(6) . ?
N1 C12 1.510(6) . ?
N1 C16 1.515(7) . ?
N1 C14 1.520(7) . ?
C10 C11 1.507(11) . ?
C10 H10A 0.9599 . ?
C10 H10B 0.9601 . ?
C11 H11A 0.9607 . ?
C11 H11B 0.9596 . ?
C11 H11C 0.9608 . ?
C12 C13 1.522(8) . ?
C12 H12A 0.9596 . ?
C12 H12B 0.9592 . ?
C13 H13A 0.9604 . ?
C13 H13B 0.9610 . ?
C13 H13C 0.9592 . ?
C14 C15 1.498(9) . ?
C14 H14A 0.9594 . ?
C14 H14B 0.9599 . ?
C15 H15A 0.9601 . ?
C15 H15B 0.9606 . ?
C15 H15C 0.9595 . ?
C16 C17 1.496(9) . ?
C16 H16A 0.9605 . ?
C16 H16B 0.9588 . ?
C17 H17A 0.9594 . ?
C17 H17B 0.9597 . ?
C17 H17C 0.9608 . ?

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
Fe1 Hg1 Fe1 126.35(3) 2_655 . ?
Fe1 Hg1 Fe3 61.132(19) 2_655 2_655 ?
Fe1 Hg1 Fe3 156.302(19) . 2_655 ?
Fe1 Hg1 Fe3 156.302(19) 2_655 . ?
Fe1 Hg1 Fe3 61.132(19) . . ?
Fe3 Hg1 Fe3 122.67(3) 2_655 . ?
C2 Fe1 C3 92.3(3) . . ?
C2 Fe1 C1 90.4(2) . . ?
C3 Fe1 C1 107.8(2) . . ?
C2 Fe1 S1 94.4(2) . . ?
C3 Fe1 S1 142.70(16) . . ?
C1 Fe1 S1 108.79(16) . . ?
C2 Fe1 Fe2 93.98(18) . . ?
C3 Fe1 Fe2 89.62(16) . . ?
C1 Fe1 Fe2 161.86(16) . . ?
S1 Fe1 Fe2 53.34(4) . . ?
C2 Fe1 Hg1 157.1(2) . . ?
C3 Fe1 Hg1 78.04(17) . . ?
C1 Fe1 Hg1 73.34(16) . . ?
S1 Fe1 Hg1 105.94(4) . . ?
Fe2 Fe1 Hg1 106.53(3) . . ?
C2 Fe1 Fe3 143.0(2) . . ?
C3 Fe1 Fe3 108.96(16) . . ?
C1 Fe1 Fe3 110.25(15) . . ?
S1 Fe1 Fe3 50.58(4) . . ?
Fe2 Fe1 Fe3 57.53(2) . . ?
Hg1 Fe1 Fe3 59.63(2) . . ?
C6 Fe2 C5 95.6(3) . . ?
C6 Fe2 C4 94.9(3) . . ?
C5 Fe2 C4 99.9(3) . . ?
C6 Fe2 S1 106.80(17) . . ?
C5 Fe2 S1 146.24(19) . . ?
C4 Fe2 S1 102.9(2) . . ?
C6 Fe2 Fe3 97.5(2) . . ?
C5 Fe2 Fe3 99.2(2) . . ?
C4 Fe2 Fe3 156.01(19) . . ?
S1 Fe2 Fe3 53.77(4) . . ?
C6 Fe2 Fe1 158.79(18) . . ?
C5 Fe2 Fe1 98.67(18) . . ?
C4 Fe2 Fe1 97.98(19) . . ?
S1 Fe2 Fe1 53.86(4) . . ?
Fe3 Fe2 Fe1 64.76(2) . . ?
C8 Fe3 C9 91.0(2) . . ?
C8 Fe3 C7 91.6(2) . . ?
C9 Fe3 C7 110.2(2) . . ?
C8 Fe3 S1 96.13(18) . . ?
C9 Fe3 S1 101.20(16) . . ?
C7 Fe3 S1 147.52(17) . . ?
C8 Fe3 Fe2 92.17(18) . . ?
C9 Fe3 Fe2 154.67(16) . . ?
C7 Fe3 Fe2 94.85(17) . . ?
S1 Fe3 Fe2 53.48(4) . . ?
C8 Fe3 Hg1 157.03(18) . . ?
C9 Fe3 Hg1 78.14(15) . . ?
C7 Fe3 Hg1 73.73(16) . . ?
S1 Fe3 Hg1 105.75(4) . . ?
Fe2 Fe3 Hg1 106.35(3) . . ?
C8 Fe3 Fe1 143.70(18) . . ?
C9 Fe3 Fe1 108.09(15) . . ?
C7 Fe3 Fe1 109.26(15) . . ?
S1 Fe3 Fe1 50.77(4) . . ?
Fe2 Fe3 Fe1 57.71(2) . . ?
Hg1 Fe3 Fe1 59.236(19) . . ?
Fe2 S1 Fe3 72.75(5) . . ?
Fe2 S1 Fe1 72.80(4) . . ?
Fe3 S1 Fe1 78.65(5) . . ?
C10 N1 C12 112.0(4) . . ?
C10 N1 C16 110.4(4) . . ?
C12 N1 C16 105.7(4) . . ?
C10 N1 C14 107.0(4) . . ?
C12 N1 C14 111.2(4) . . ?
C16 N1 C14 110.6(4) . . ?
O1 C1 Fe1 173.5(5) . . ?
O2 C2 Fe1 176.6(5) . . ?
O3 C3 Fe1 175.3(5) . . ?
O4 C4 Fe2 176.5(6) . . ?
O5 C5 Fe2 176.9(5) . . ?
O6 C6 Fe2 177.5(5) . . ?
O7 C7 Fe3 175.4(4) . . ?
O8 C8 Fe3 177.1(5) . . ?
O9 C9 Fe3 174.5(4) . . ?
C11 C10 N1 115.6(6) . . ?
C11 C10 H10A 107.3 . . ?
N1 C10 H10A 108.0 . . ?
C11 C10 H10B 106.4 . . ?
N1 C10 H10B 109.8 . . ?
H10A C10 H10B 109.5 . . ?
C10 C11 H11A 107.2 . . ?
C10 C11 H11B 110.2 . . ?
H11A C11 H11B 109.4 . . ?
C10 C11 H11C 111.0 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
N1 C12 C13 115.0(5) . . ?
N1 C12 H12A 109.8 . . ?
C13 C12 H12A 107.1 . . ?
N1 C12 H12B 108.6 . . ?
C13 C12 H12B 106.8 . . ?
H12A C12 H12B 109.4 . . ?
C12 C13 H13A 110.7 . . ?
C12 C13 H13B 108.6 . . ?
H13A C13 H13B 109.4 . . ?
C12 C13 H13C 109.0 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C15 C14 N1 115.6(5) . . ?
C15 C14 H14A 106.7 . . ?
N1 C14 H14A 108.6 . . ?
C15 C14 H14B 107.0 . . ?
N1 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C14 C15 H15A 110.1 . . ?
C14 C15 H15B 109.4 . . ?
H15A C15 H15B 109.3 . . ?
C14 C15 H15C 109.1 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.4 . . ?
C17 C16 N1 114.9(5) . . ?
C17 C16 H16A 104.6 . . ?
N1 C16 H16A 108.1 . . ?
C17 C16 H16B 109.0 . . ?
N1 C16 H16B 110.6 . . ?
H16A C16 H16B 109.5 . . ?
C16 C17 H17A 111.5 . . ?
C16 C17 H17B 110.7 . . ?
H17A C17 H17B 109.5 . . ?
C16 C17 H17C 106.1 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.992
_diffrn_reflns_theta_full        25.04
_diffrn_measured_fraction_theta_full 0.992
_refine_diff_density_max         1.091
_refine_diff_density_min         -1.640
_refine_diff_density_rms         0.400

#=============================================END

data_5
_database_code_depnum_ccdc_archive 'CCDC 817585'
#TrackingRef '- cif-S-Fe-RX-2011-NJC-revised.cif'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C34 H40 Fe6 Hg2 I2 N2 O18 S2'
_chemical_formula_sum            'C34 H40 Fe6 Hg2 I2 N2 O18 S2'
_chemical_formula_weight         1818.88

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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Hg Hg -2.3894 9.2266 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 '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'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.3653(2)
_cell_length_b                   11.1757(2)
_cell_length_c                   13.0749(2)
_cell_angle_alpha                91.0870(10)
_cell_angle_beta                 94.6200(10)
_cell_angle_gamma                103.5120(10)
_cell_volume                     1325.26(4)
_cell_formula_units_Z            1
_cell_measurement_temperature    200(2)
_cell_measurement_reflns_used    13991
_cell_measurement_theta_min      2.037
_cell_measurement_theta_max      25.35

_exptl_crystal_description       prism
_exptl_crystal_colour            black
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.5
_exptl_crystal_size_min          0.33
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.279
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             856
_exptl_absorpt_coefficient_mu    8.670
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.0293
_exptl_absorpt_correction_T_max  0.0712
_exptl_absorpt_process_details   
;
?
;

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      200(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_detector_area_resol_mean 9
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            18053
_diffrn_reflns_av_R_equivalents  0.0561
_diffrn_reflns_av_sigmaI/netI    0.0360
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         2.56
_diffrn_reflns_theta_max         25.33
_reflns_number_total             4827
_reflns_number_gt                4414
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_reduction        'HKL Denzo and Scalepack'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1986)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0475P)^2^+1.4522P] 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    noref
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4827
_refine_ls_number_parameters     298
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0373
_refine_ls_R_factor_gt           0.0331
_refine_ls_wR_factor_ref         0.0867
_refine_ls_wR_factor_gt          0.0844
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_restrained_S_all      1.088
_refine_ls_shift/su_max          0.001
_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
Hg1 Hg 0.51217(2) 0.891126(19) 0.358467(17) 0.04294(10) Uani 1 1 d . . .
I1 I 0.63053(4) 1.12927(3) 0.41557(3) 0.04701(12) Uani 1 1 d . . .
Fe1 Fe 0.33927(8) 0.76561(7) 0.20424(6) 0.03653(18) Uani 1 1 d . . .
Fe2 Fe 0.57180(8) 0.68097(6) 0.30330(6) 0.03220(17) Uani 1 1 d . . .
Fe3 Fe 0.55753(9) 0.72636(7) 0.10878(6) 0.03665(19) Uani 1 1 d . . .
S1 S 0.40091(15) 0.58996(12) 0.18413(10) 0.0369(3) Uani 1 1 d . . .
O1 O 0.4055(7) 1.0199(5) 0.1354(5) 0.0804(16) Uani 1 1 d . . .
O2 O 0.1112(7) 0.7079(7) 0.0363(5) 0.099(2) Uani 1 1 d . . .
O3 O 0.1194(6) 0.7183(5) 0.3551(4) 0.0713(14) Uani 1 1 d . . .
O4 O 0.4506(7) 0.6092(4) 0.4989(4) 0.0654(14) Uani 1 1 d . . .
O5 O 0.7140(6) 0.4762(4) 0.2989(4) 0.0620(13) Uani 1 1 d . . .
O6 O 0.8641(5) 0.8505(5) 0.3295(5) 0.0767(16) Uani 1 1 d . . .
O7 O 0.7728(6) 0.5915(5) 0.0508(4) 0.0722(14) Uani 1 1 d . . .
O8 O 0.7452(6) 0.9771(4) 0.1181(4) 0.0698(14) Uani 1 1 d . . .
O9 O 0.4131(7) 0.7150(6) -0.0990(4) 0.0827(18) Uani 1 1 d . . .
N1 N 0.9034(5) 0.7446(4) 0.7184(3) 0.0364(10) Uani 1 1 d . . .
C1 C 0.3843(7) 0.9221(6) 0.1670(5) 0.0501(15) Uani 1 1 d . . .
C2 C 0.2014(8) 0.7287(7) 0.1026(5) 0.0591(17) Uani 1 1 d . . .
C3 C 0.2086(7) 0.7420(6) 0.2978(5) 0.0481(14) Uani 1 1 d . . .
C4 C 0.4998(7) 0.6399(5) 0.4242(5) 0.0432(13) Uani 1 1 d . . .
C5 C 0.6576(7) 0.5557(6) 0.2997(4) 0.0422(13) Uani 1 1 d . . .
C6 C 0.7461(7) 0.7891(6) 0.3195(5) 0.0516(15) Uani 1 1 d . . .
C7 C 0.6890(7) 0.6428(6) 0.0737(5) 0.0476(14) Uani 1 1 d . . .
C8 C 0.6715(7) 0.8782(6) 0.1138(5) 0.0487(15) Uani 1 1 d . . .
C9 C 0.4697(7) 0.7220(6) -0.0182(5) 0.0516(16) Uani 1 1 d . . .
C10 C 0.8143(7) 0.6467(6) 0.6431(5) 0.0491(15) Uani 1 1 d . . .
H10A H 0.7300 0.6749 0.6139 0.059 Uiso 1 1 calc R . .
H10B H 0.7768 0.5735 0.6806 0.059 Uiso 1 1 calc R . .
C11 C 0.8943(10) 0.6113(8) 0.5566(5) 0.071(2) Uani 1 1 d . . .
H11A H 0.8287 0.5479 0.5137 0.107 Uiso 1 1 calc R . .
H11B H 0.9770 0.5813 0.5842 0.107 Uiso 1 1 calc R . .
H11C H 0.9285 0.6819 0.5168 0.107 Uiso 1 1 calc R . .
C12 C 0.8050(6) 0.7639(6) 0.8006(5) 0.0448(14) Uani 1 1 d . . .
H12A H 0.7191 0.7868 0.7678 0.054 Uiso 1 1 calc R . .
H12B H 0.7708 0.6862 0.8329 0.054 Uiso 1 1 calc R . .
C13 C 0.8762(9) 0.8600(7) 0.8827(5) 0.0639(19) Uani 1 1 d . . .
H13A H 0.8063 0.8663 0.9312 0.096 Uiso 1 1 calc R . .
H13B H 0.9083 0.9380 0.8521 0.096 Uiso 1 1 calc R . .
H13C H 0.9595 0.8370 0.9175 0.096 Uiso 1 1 calc R . .
C14 C 1.0392(6) 0.7062(5) 0.7651(4) 0.0401(12) Uani 1 1 d . . .
H14A H 1.1037 0.7025 0.7113 0.048 Uiso 1 1 calc R . .
H14B H 1.0917 0.7695 0.8153 0.048 Uiso 1 1 calc R . .
C15 C 1.0088(7) 0.5842(5) 0.8164(5) 0.0451(13) Uani 1 1 d . . .
H15A H 1.1003 0.5674 0.8433 0.068 Uiso 1 1 calc R . .
H15B H 0.9592 0.5202 0.7671 0.068 Uiso 1 1 calc R . .
H15C H 0.9477 0.5874 0.8714 0.068 Uiso 1 1 calc R . .
C16 C 0.9595(6) 0.8640(5) 0.6642(5) 0.0439(14) Uani 1 1 d . . .
H16A H 1.0207 0.9240 0.7137 0.053 Uiso 1 1 calc R . .
H16B H 1.0213 0.8483 0.6118 0.053 Uiso 1 1 calc R . .
C17 C 0.8392(8) 0.9195(7) 0.6143(6) 0.0603(18) Uani 1 1 d . . .
H17A H 0.8831 0.9945 0.5827 0.090 Uiso 1 1 calc R . .
H17B H 0.7781 0.9368 0.6655 0.090 Uiso 1 1 calc R . .
H17C H 0.7801 0.8623 0.5630 0.090 Uiso 1 1 calc R . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Hg1 0.04724(15) 0.03008(13) 0.05095(16) -0.00764(9) -0.00502(11) 0.01188(9)
I1 0.0546(2) 0.03019(19) 0.0542(2) -0.00589(16) 0.02421(19) 0.00004(16)
Fe1 0.0353(4) 0.0372(4) 0.0366(4) 0.0004(3) -0.0006(3) 0.0089(3)
Fe2 0.0374(4) 0.0275(4) 0.0329(4) 0.0007(3) 0.0033(3) 0.0101(3)
Fe3 0.0403(4) 0.0343(4) 0.0330(4) 0.0017(3) 0.0065(3) 0.0031(3)
S1 0.0407(7) 0.0296(6) 0.0365(7) -0.0015(5) 0.0043(6) 0.0005(5)
O1 0.093(4) 0.056(3) 0.099(4) 0.036(3) 0.009(3) 0.027(3)
O2 0.078(4) 0.136(6) 0.076(4) -0.020(4) -0.042(3) 0.029(4)
O3 0.052(3) 0.086(4) 0.073(3) -0.007(3) 0.021(3) 0.007(3)
O4 0.118(4) 0.049(3) 0.046(3) 0.014(2) 0.035(3) 0.043(3)
O5 0.090(4) 0.057(3) 0.056(3) 0.003(2) 0.019(3) 0.047(3)
O6 0.042(3) 0.054(3) 0.128(5) 0.004(3) -0.007(3) 0.005(2)
O7 0.076(3) 0.079(4) 0.073(3) 0.010(3) 0.031(3) 0.034(3)
O8 0.074(3) 0.044(3) 0.077(3) -0.001(2) 0.019(3) -0.019(2)
O9 0.094(4) 0.096(4) 0.041(3) 0.007(3) -0.013(3) -0.008(3)
N1 0.035(2) 0.041(2) 0.034(2) 0.0025(19) 0.0069(19) 0.0069(19)
C1 0.051(4) 0.052(4) 0.049(4) 0.002(3) -0.005(3) 0.018(3)
C2 0.055(4) 0.069(5) 0.052(4) 0.003(3) -0.001(3) 0.015(3)
C3 0.038(3) 0.051(4) 0.054(4) -0.003(3) -0.001(3) 0.010(3)
C4 0.062(4) 0.034(3) 0.041(3) 0.002(2) 0.008(3) 0.024(3)
C5 0.053(3) 0.043(3) 0.032(3) 0.002(2) 0.010(3) 0.012(3)
C6 0.050(4) 0.042(3) 0.064(4) 0.001(3) 0.001(3) 0.014(3)
C7 0.051(4) 0.050(4) 0.043(3) 0.006(3) 0.013(3) 0.012(3)
C8 0.050(3) 0.058(4) 0.038(3) 0.003(3) 0.010(3) 0.011(3)
C9 0.056(4) 0.048(4) 0.044(4) 0.006(3) 0.009(3) -0.004(3)
C10 0.046(3) 0.048(3) 0.046(3) -0.002(3) -0.004(3) 0.000(3)
C11 0.094(6) 0.074(5) 0.043(4) -0.012(3) 0.001(4) 0.015(4)
C12 0.032(3) 0.057(4) 0.048(3) 0.009(3) 0.015(3) 0.009(3)
C13 0.071(5) 0.077(5) 0.049(4) -0.009(3) 0.013(4) 0.028(4)
C14 0.032(3) 0.045(3) 0.043(3) -0.001(2) 0.004(2) 0.009(2)
C15 0.053(3) 0.039(3) 0.046(3) 0.005(2) 0.003(3) 0.014(3)
C16 0.039(3) 0.043(3) 0.049(3) 0.014(3) 0.009(3) 0.006(2)
C17 0.061(4) 0.061(4) 0.062(4) 0.018(3) 0.006(3) 0.018(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
Hg1 Fe2 2.6385(7) . ?
Hg1 Fe1 2.6384(8) . ?
Hg1 I1 2.6985(4) . ?
Hg1 C1 2.751(6) . ?
Hg1 I1 3.3296(4) 2_676 ?
I1 Hg1 3.3296(4) 2_676 ?
Fe1 C2 1.749(7) . ?
Fe1 C3 1.780(7) . ?
Fe1 C1 1.787(7) . ?
Fe1 S1 2.1887(16) . ?
Fe1 Fe3 2.5958(11) . ?
Fe1 Fe2 2.8053(11) . ?
Fe2 C5 1.771(6) . ?
Fe2 C6 1.784(7) . ?
Fe2 C4 1.794(6) . ?
Fe2 S1 2.1911(15) . ?
Fe2 Fe3 2.6018(10) . ?
Fe3 C8 1.778(7) . ?
Fe3 C9 1.787(7) . ?
Fe3 C7 1.792(7) . ?
Fe3 S1 2.1658(14) . ?
O1 C1 1.155(8) . ?
O2 C2 1.140(8) . ?
O3 C3 1.155(7) . ?
O4 C4 1.137(7) . ?
O5 C5 1.134(7) . ?
O6 C6 1.152(8) . ?
O7 C7 1.129(8) . ?
O8 C8 1.156(8) . ?
O9 C9 1.136(8) . ?
N1 C10 1.504(7) . ?
N1 C12 1.515(7) . ?
N1 C16 1.525(7) . ?
N1 C14 1.521(7) . ?
C10 C11 1.502(10) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
C12 C13 1.503(10) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C14 C15 1.508(8) . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C16 C17 1.518(9) . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?

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
Fe2 Hg1 Fe1 64.23(2) . . ?
Fe2 Hg1 I1 144.67(2) . . ?
Fe1 Hg1 I1 137.68(2) . . ?
Fe2 Hg1 C1 93.49(14) . . ?
Fe1 Hg1 C1 38.67(14) . . ?
I1 Hg1 C1 99.33(14) . . ?
Fe2 Hg1 I1 110.857(18) . 2_676 ?
Fe1 Hg1 I1 115.341(19) . 2_676 ?
I1 Hg1 I1 85.669(11) . 2_676 ?
C1 Hg1 I1 129.67(14) . 2_676 ?
Hg1 I1 Hg1 94.331(11) . 2_676 ?
C2 Fe1 C3 92.5(3) . . ?
C2 Fe1 C1 90.3(3) . . ?
C3 Fe1 C1 111.8(3) . . ?
C2 Fe1 S1 92.1(3) . . ?
C3 Fe1 S1 106.0(2) . . ?
C1 Fe1 S1 142.0(2) . . ?
C2 Fe1 Fe3 98.4(2) . . ?
C3 Fe1 Fe3 156.4(2) . . ?
C1 Fe1 Fe3 89.1(2) . . ?
S1 Fe1 Fe3 53.00(4) . . ?
C2 Fe1 Hg1 160.0(3) . . ?
C3 Fe1 Hg1 82.3(2) . . ?
C1 Fe1 Hg1 74.1(2) . . ?
S1 Fe1 Hg1 107.88(5) . . ?
Fe3 Fe1 Hg1 93.73(3) . . ?
C2 Fe1 Fe2 142.0(3) . . ?
C3 Fe1 Fe2 101.9(2) . . ?
C1 Fe1 Fe2 115.7(2) . . ?
S1 Fe1 Fe2 50.21(4) . . ?
Fe3 Fe1 Fe2 57.44(3) . . ?
Hg1 Fe1 Fe2 57.89(2) . . ?
C5 Fe2 C6 91.5(3) . . ?
C5 Fe2 C4 93.1(2) . . ?
C6 Fe2 C4 111.8(3) . . ?
C5 Fe2 S1 91.0(2) . . ?
C6 Fe2 S1 141.5(2) . . ?
C4 Fe2 S1 106.4(2) . . ?
C5 Fe2 Fe3 99.26(18) . . ?
C6 Fe2 Fe3 88.8(2) . . ?
C4 Fe2 Fe3 155.7(2) . . ?
S1 Fe2 Fe3 52.89(4) . . ?
C5 Fe2 Hg1 161.1(2) . . ?
C6 Fe2 Hg1 74.9(2) . . ?
C4 Fe2 Hg1 80.32(17) . . ?
S1 Fe2 Hg1 107.80(5) . . ?
Fe3 Fe2 Hg1 93.59(3) . . ?
C5 Fe2 Fe1 141.0(2) . . ?
C6 Fe2 Fe1 116.1(2) . . ?
C4 Fe2 Fe1 100.64(19) . . ?
S1 Fe2 Fe1 50.13(4) . . ?
Fe3 Fe2 Fe1 57.23(3) . . ?
Hg1 Fe2 Fe1 57.88(2) . . ?
C8 Fe3 C9 99.6(3) . . ?
C8 Fe3 C7 99.2(3) . . ?
C9 Fe3 C7 94.8(3) . . ?
C8 Fe3 S1 147.1(2) . . ?
C9 Fe3 S1 102.57(19) . . ?
C7 Fe3 S1 102.9(2) . . ?
C8 Fe3 Fe1 99.9(2) . . ?
C9 Fe3 Fe1 96.5(2) . . ?
C7 Fe3 Fe1 155.87(19) . . ?
S1 Fe3 Fe1 53.81(4) . . ?
C8 Fe3 Fe2 99.7(2) . . ?
C9 Fe3 Fe2 155.5(2) . . ?
C7 Fe3 Fe2 96.9(2) . . ?
S1 Fe3 Fe2 53.78(4) . . ?
Fe1 Fe3 Fe2 65.33(3) . . ?
Fe3 S1 Fe1 73.18(5) . . ?
Fe3 S1 Fe2 73.33(5) . . ?
Fe1 S1 Fe2 79.66(5) . . ?
C10 N1 C12 107.7(4) . . ?
C10 N1 C16 110.5(4) . . ?
C12 N1 C16 110.8(4) . . ?
C10 N1 C14 110.6(5) . . ?
C12 N1 C14 110.9(4) . . ?
C16 N1 C14 106.4(4) . . ?
O1 C1 Fe1 174.2(6) . . ?
O1 C1 Hg1 118.6(5) . . ?
Fe1 C1 Hg1 67.27(19) . . ?
O2 C2 Fe1 178.2(8) . . ?
O3 C3 Fe1 175.0(6) . . ?
O4 C4 Fe2 177.0(6) . . ?
O5 C5 Fe2 178.9(6) . . ?
O6 C6 Fe2 174.2(6) . . ?
O7 C7 Fe3 179.0(6) . . ?
O8 C8 Fe3 179.3(6) . . ?
O9 C9 Fe3 177.7(6) . . ?
N1 C10 C11 115.9(5) . . ?
N1 C10 H10A 108.3 . . ?
C11 C10 H10A 108.3 . . ?
N1 C10 H10B 108.3 . . ?
C11 C10 H10B 108.3 . . ?
H10A C10 H10B 107.4 . . ?
C10 C11 H11A 109.5 . . ?
C10 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C10 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C13 C12 N1 115.1(5) . . ?
C13 C12 H12A 108.5 . . ?
N1 C12 H12A 108.5 . . ?
C13 C12 H12B 108.5 . . ?
N1 C12 H12B 108.5 . . ?
H12A C12 H12B 107.5 . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C15 C14 N1 115.2(5) . . ?
C15 C14 H14A 108.5 . . ?
N1 C14 H14A 108.5 . . ?
C15 C14 H14B 108.5 . . ?
N1 C14 H14B 108.5 . . ?
H14A C14 H14B 107.5 . . ?
C14 C15 H15A 109.5 . . ?
C14 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C14 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C17 C16 N1 114.5(5) . . ?
C17 C16 H16A 108.6 . . ?
N1 C16 H16A 108.6 . . ?
C17 C16 H16B 108.6 . . ?
N1 C16 H16B 108.6 . . ?
H16A C16 H16B 107.6 . . ?
C16 C17 H17A 109.5 . . ?
C16 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C16 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.993
_diffrn_reflns_theta_full        25.33
_diffrn_measured_fraction_theta_full 0.993
_refine_diff_density_max         1.656
_refine_diff_density_min         -1.798
_refine_diff_density_rms         0.174