# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2020

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_femoco
_database_code_depnum_ccdc_archive 'CCDC 1853085'
loop_
_audit_author_name
_audit_author_address
'Satoru Tsukada'
;Hiroshima University
Japan
;
_audit_update_record             
;
2018-07-03 deposited with the CCDC.	2020-06-17 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT430_femoco              
;
PROBLEM: Short Inter D...A Contact  O1       ..O6               2.83 Ang.
RESPONSE: This is a typical distance for O-H...O hydrogen bond. So PLATON alerts that there may be missing hydrogen atoms in one or both oxygens, it will depend if they are water, hydroxyl, carbonyl,... oxygens. Depending on the data quality and the presence/absence of heavy atoms the hydrogens will show up as residual density peaks at bonding distance from the oxygens.
;
_vrf_PLAT430_femoco_2            
;
PROBLEM: Short Inter D...A Contact  O4       ..O6               2.88 Ang.
RESPONSE: This is a typical distance for O-H...O hydrogen bond. So PLATON alerts that there may be missing hydrogen atoms in one or both oxygens, it will depend if they are water, hydroxyl, carbonyl,... oxygens. Depending on the data quality and the presence/absence of heavy atoms the hydrogens will show up as residual density peaks at bonding distance from the oxygens.
;
# Added during the CSD deposition process: Tuesday 03 July 2018 08:46 AM
# end Validation Reply Form

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C15 H13 Fe Mo O6 P S2'
_chemical_formula_weight         536.13

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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'P2(1)/c  '
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   6.4434(6)
_cell_length_b                   17.1407(15)
_cell_length_c                   17.5328(16)
_cell_angle_alpha                90.00
_cell_angle_beta                 91.3310(10)
_cell_angle_gamma                90.00
_cell_volume                     1935.9(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    103
_cell_measurement_reflns_used    9196
_cell_measurement_theta_min      2.32
_cell_measurement_theta_max      26.40
_exptl_crystal_description       block
_exptl_crystal_colour            black
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.60
_exptl_crystal_size_min          0.30
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.840
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1064
_exptl_absorpt_coefficient_mu    1.723
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.4245
_exptl_absorpt_correction_T_max  0.6259
_exptl_absorpt_process_details   
;
SADABS Sheldrick 1996
;
_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      103
_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  'Bruker APEX CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean 8.333
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            10471
_diffrn_reflns_av_R_equivalents  0.0319
_diffrn_reflns_av_sigmaI/netI    0.0332
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         1.66
_diffrn_reflns_theta_max         26.40
_reflns_number_total             3918
_reflns_number_gt                3786
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'SMART (Bruker AXS)'
_computing_cell_refinement       'SMART (Bruker AXS)'
_computing_data_reduction        'SAINT (Bruker AXS)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'XSHEL (Bruker AXS,2002)'
_computing_publication_material  'XCIF (Bruker AXS, 2001)'
_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² 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/[σ²(Fo²)+(0.0679P)²+1.0711P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3918
_refine_ls_number_parameters     238
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0333
_refine_ls_R_factor_gt           0.0325
_refine_ls_wR_factor_ref         0.0941
_refine_ls_wR_factor_gt          0.0933
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_restrained_S_all      1.057
_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
Mo1 Mo 0.28807(3) 0.702600(10) 0.320252(11) 0.01308(10) Uani 1 1 d . . .
Fe2 Fe 0.13644(5) 0.623342(18) 0.439351(18) 0.01387(11) Uani 1 1 d . . .
S1 S 0.00939(8) 0.74453(3) 0.41123(3) 0.01586(14) Uani 1 1 d . . .
P4 P 0.40094(9) 0.84126(3) 0.29261(3) 0.01612(14) Uani 1 1 d . . .
S2 S 0.44413(8) 0.68896(3) 0.45412(3) 0.01553(14) Uani 1 1 d . . .
O1 O 0.0256(3) 0.61789(11) 0.60098(10) 0.0257(4) Uani 1 1 d . . .
O2 O -0.2413(3) 0.54623(10) 0.37904(10) 0.0221(4) Uani 1 1 d . . .
O3 O 0.3620(3) 0.47460(10) 0.43660(10) 0.0202(4) Uani 1 1 d . . .
O5 O 0.1951(3) 0.53538(10) 0.25811(10) 0.0243(4) Uani 1 1 d . . .
C3 C 0.2237(3) 0.59513(14) 0.28707(13) 0.0172(5) Uani 1 1 d . . .
O6 O 0.0273(3) 0.73251(11) 0.16944(10) 0.0233(4) Uani 1 1 d . . .
O4 O 0.6972(3) 0.64936(12) 0.24247(11) 0.0277(4) Uani 1 1 d . . .
C1 C -0.0967(4) 0.57743(13) 0.40208(13) 0.0165(4) Uani 1 1 d . . .
C6 C 0.2760(3) 0.53217(14) 0.43785(13) 0.0157(5) Uani 1 1 d . . .
C2 C 0.0683(4) 0.62118(13) 0.53863(14) 0.0175(5) Uani 1 1 d . . .
C7 C 0.1580(4) 0.80279(13) 0.47702(14) 0.0183(5) Uani 1 1 d . . .
C15 C 0.1909(4) 0.91233(14) 0.28746(15) 0.0228(5) Uani 1 1 d . . .
H15A H 0.1279 0.9170 0.3376 0.034 Uiso 1 1 calc R . .
H15B H 0.0856 0.8951 0.2499 0.034 Uiso 1 1 calc R . .
H15C H 0.2461 0.9631 0.2721 0.034 Uiso 1 1 calc R . .
C5 C 0.1231(4) 0.72227(14) 0.22440(14) 0.0181(5) Uani 1 1 d . . .
C13 C 0.5249(4) 0.85114(15) 0.20113(15) 0.0242(5) Uani 1 1 d . . .
H13A H 0.5570 0.9062 0.1920 0.036 Uiso 1 1 calc R . .
H13B H 0.4310 0.8320 0.1605 0.036 Uiso 1 1 calc R . .
H13C H 0.6535 0.8206 0.2015 0.036 Uiso 1 1 calc R . .
C9 C 0.0823(4) 0.87192(14) 0.50673(14) 0.0231(5) Uani 1 1 d . . .
H9 H -0.0529 0.8897 0.4927 0.028 Uiso 1 1 calc R . .
C8 C 0.3556(4) 0.77614(13) 0.49801(13) 0.0178(4) Uani 1 1 d . . .
C10 C 0.2078(5) 0.91517(15) 0.55767(15) 0.0279(6) Uani 1 1 d . . .
H10 H 0.1584 0.9630 0.5777 0.034 Uiso 1 1 calc R . .
C4 C 0.5484(4) 0.67145(14) 0.27018(14) 0.0198(5) Uani 1 1 d . . .
C14 C 0.5850(4) 0.88828(15) 0.35766(15) 0.0228(5) Uani 1 1 d . . .
H14A H 0.7082 0.8552 0.3642 0.034 Uiso 1 1 calc R . .
H14B H 0.5205 0.8961 0.4072 0.034 Uiso 1 1 calc R . .
H14C H 0.6255 0.9389 0.3367 0.034 Uiso 1 1 calc R . .
C12 C 0.4788(4) 0.81828(15) 0.54947(14) 0.0215(5) Uani 1 1 d . . .
H12 H 0.6125 0.7997 0.5645 0.026 Uiso 1 1 calc R . .
C11 C 0.4036(4) 0.88829(15) 0.57887(15) 0.0273(6) Uani 1 1 d . . .
H11 H 0.4874 0.9177 0.6137 0.033 Uiso 1 1 calc R . .


_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
Mo1 C3 1.973(2) . ?
Mo1 C4 1.984(3) . ?
Mo1 C5 1.996(2) . ?
Mo1 S1 2.5334(6) . ?
Mo1 P4 2.5356(6) . ?
Mo1 S2 2.5426(6) . ?
Mo1 Fe2 2.6936(4) . ?
Fe2 C6 1.804(2) . ?
Fe2 C1 1.805(2) . ?
Fe2 C2 1.805(2) . ?
Fe2 S1 2.2825(6) . ?
Fe2 S2 2.2888(6) . ?
S1 C7 1.787(3) . ?
P4 C14 1.815(2) . ?
P4 C13 1.816(3) . ?
P4 C15 1.822(2) . ?
S2 C8 1.781(2) . ?
O1 C2 1.135(3) . ?
O2 C1 1.140(3) . ?
O3 C6 1.132(3) . ?
O5 C3 1.156(3) . ?
O6 C5 1.146(3) . ?
O4 C4 1.149(3) . ?
C7 C9 1.388(3) . ?
C7 C8 1.394(3) . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C9 C10 1.402(4) . ?
C9 H9 0.9500 . ?
C8 C12 1.390(3) . ?
C10 C11 1.386(4) . ?
C10 H10 0.9500 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C12 C11 1.397(4) . ?
C12 H12 0.9500 . ?
C11 H11 0.9500 . ?

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 Mo1 C4 78.02(9) . . ?
C3 Mo1 C5 78.77(10) . . ?
C4 Mo1 C5 96.43(10) . . ?
C3 Mo1 S1 107.65(7) . . ?
C4 Mo1 S1 166.82(7) . . ?
C5 Mo1 S1 96.36(7) . . ?
C3 Mo1 P4 151.42(7) . . ?
C4 Mo1 P4 85.33(7) . . ?
C5 Mo1 P4 80.23(7) . . ?
S1 Mo1 P4 93.73(2) . . ?
C3 Mo1 S2 105.21(7) . . ?
C4 Mo1 S2 93.64(7) . . ?
C5 Mo1 S2 169.77(7) . . ?
S1 Mo1 S2 73.49(2) . . ?
P4 Mo1 S2 98.84(2) . . ?
C3 Mo1 Fe2 71.34(7) . . ?
C4 Mo1 Fe2 122.20(7) . . ?
C5 Mo1 Fe2 122.83(7) . . ?
S1 Mo1 Fe2 51.673(15) . . ?
P4 Mo1 Fe2 137.035(17) . . ?
S2 Mo1 Fe2 51.743(15) . . ?
C6 Fe2 C1 91.60(10) . . ?
C6 Fe2 C2 97.40(10) . . ?
C1 Fe2 C2 96.96(10) . . ?
C6 Fe2 S1 164.14(7) . . ?
C1 Fe2 S1 91.56(7) . . ?
C2 Fe2 S1 97.64(7) . . ?
C6 Fe2 S2 89.81(7) . . ?
C1 Fe2 S2 165.17(7) . . ?
C2 Fe2 S2 97.49(7) . . ?
S1 Fe2 S2 83.26(2) . . ?
C6 Fe2 Mo1 103.64(7) . . ?
C1 Fe2 Mo1 104.66(7) . . ?
C2 Fe2 Mo1 149.14(7) . . ?
S1 Fe2 Mo1 60.543(17) . . ?
S2 Fe2 Mo1 60.726(17) . . ?
C7 S1 Fe2 100.66(8) . . ?
C7 S1 Mo1 100.83(9) . . ?
Fe2 S1 Mo1 67.784(17) . . ?
C14 P4 C13 102.67(12) . . ?
C14 P4 C15 102.01(12) . . ?
C13 P4 C15 103.62(12) . . ?
C14 P4 Mo1 118.83(8) . . ?
C13 P4 Mo1 112.96(9) . . ?
C15 P4 Mo1 114.84(9) . . ?
C8 S2 Fe2 100.14(8) . . ?
C8 S2 Mo1 101.42(8) . . ?
Fe2 S2 Mo1 67.532(17) . . ?
O5 C3 Mo1 170.7(2) . . ?
O2 C1 Fe2 177.9(2) . . ?
O3 C6 Fe2 179.4(2) . . ?
O1 C2 Fe2 178.3(2) . . ?
C9 C7 C8 120.5(2) . . ?
C9 C7 S1 122.1(2) . . ?
C8 C7 S1 117.38(18) . . ?
P4 C15 H15A 109.5 . . ?
P4 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
P4 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
O6 C5 Mo1 179.0(2) . . ?
P4 C13 H13A 109.5 . . ?
P4 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
P4 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C7 C9 C10 119.2(3) . . ?
C7 C9 H9 120.4 . . ?
C10 C9 H9 120.4 . . ?
C12 C8 C7 120.4(2) . . ?
C12 C8 S2 122.20(19) . . ?
C7 C8 S2 117.42(18) . . ?
C11 C10 C9 120.2(2) . . ?
C11 C10 H10 119.9 . . ?
C9 C10 H10 119.9 . . ?
O4 C4 Mo1 176.3(2) . . ?
P4 C14 H14A 109.5 . . ?
P4 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
P4 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C8 C12 C11 119.2(2) . . ?
C8 C12 H12 120.4 . . ?
C11 C12 H12 120.4 . . ?
C10 C11 C12 120.5(2) . . ?
C10 C11 H11 119.7 . . ?
C12 C11 H11 119.7 . . ?

_diffrn_measured_fraction_theta_max 0.989
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.994
_refine_diff_density_max         1.943
_refine_diff_density_min         -1.402
_refine_diff_density_rms         0.137
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: dichloromethane/hexane'
_chemical_properties_physical    Air-sensitive
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_p1pme3f
_database_code_depnum_ccdc_archive 'CCDC 1853087'
loop_
_audit_author_name
_audit_author_address
'Satoru Tsukada'
;Hiroshima University
Japan
;
_audit_update_record             
;
2018-07-03 deposited with the CCDC.	2020-06-17 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C22 H26 Fe2 Mo0 O4 P2 S4'
_chemical_formula_weight         656.31

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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'P2(1)/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                   9.5169(14)
_cell_length_b                   13.9270(19)
_cell_length_c                   10.8610(16)
_cell_angle_alpha                90.00
_cell_angle_beta                 110.696(3)
_cell_angle_gamma                90.00
_cell_volume                     1346.6(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    103
_cell_measurement_reflns_used    676
_cell_measurement_theta_min      2.45
_cell_measurement_theta_max      24.06
_exptl_crystal_description       block
_exptl_crystal_colour            black
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.619
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             672
_exptl_absorpt_coefficient_mu    1.534
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.9136
_exptl_absorpt_correction_T_max  0.9273
_exptl_absorpt_process_details   
;
SADABS Sheldrick 1996
;
_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      103
_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  'Bruker APEX CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean 8.333
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            6740
_diffrn_reflns_av_R_equivalents  0.0896
_diffrn_reflns_av_sigmaI/netI    0.1184
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         2.45
_diffrn_reflns_theta_max         25.41
_reflns_number_total             2473
_reflns_number_gt                1564
_reflns_threshold_expression     >2sigma

_computing_data_collection       'SMART '
_computing_cell_refinement       'SMART (Bruker AXS)'
_computing_data_reduction        'SAINT (Bruker AXS)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'XSHEL (Bruker AXS,2002)'
_computing_publication_material  'XCIF (Bruker AXS, 2001)'
_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² 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/[σ²(Fo²)+(0.0580P)²+3.4413P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         2473
_refine_ls_number_parameters     157
_refine_ls_number_restraints     43
_refine_ls_R_factor_all          0.1273
_refine_ls_R_factor_gt           0.0737
_refine_ls_wR_factor_ref         0.1616
_refine_ls_wR_factor_gt          0.1434
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_restrained_S_all      1.067
_refine_ls_shift/su_max          0.000
_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 0.86553(10) 0.00177(8) 0.57210(9) 0.0110(3) Uani 1 1 d . . .
S4 S 1.07931(18) 0.08904(14) 0.58147(16) 0.0112(4) Uani 1 1 d . . .
P1 P 0.8354(2) 0.08723(16) 0.73703(18) 0.0156(5) Uani 1 1 d . . .
S2 S 1.02901(19) -0.09647(14) 0.73253(17) 0.0140(5) Uani 1 1 d . . .
O2 O 0.6530(6) 0.1215(4) 0.3712(5) 0.0235(13) Uani 1 1 d . . .
C20 C 0.7402(8) 0.0766(6) 0.4486(7) 0.0152(17) Uani 1 1 d . . .
O1 O 0.6278(6) -0.1341(4) 0.5587(5) 0.0248(14) Uani 1 1 d . . .
C8 C 0.7191(7) -0.0808(6) 0.5668(6) 0.0121(16) Uani 1 1 d . . .
C9 C 1.0225(7) 0.1999(5) 0.4952(7) 0.0118(15) Uani 1 1 d U . .
C10 C 0.9083(7) 0.2876(6) 0.2940(7) 0.0136(16) Uani 1 1 d U . .
H10 H 0.8684 0.2900 0.2006 0.016 Uiso 1 1 calc R . .
C11 C 1.0250(8) 0.2842(6) 0.5668(7) 0.0180(16) Uani 1 1 d U . .
H11 H 1.0665 0.2835 0.6603 0.022 Uiso 1 1 calc R . .
C12 C 0.9668(7) 0.3682(6) 0.5008(7) 0.0153(16) Uani 1 1 d U . .
H12 H 0.9683 0.4256 0.5485 0.018 Uiso 1 1 calc R . .
C13 C 0.9068(8) 0.3681(6) 0.3655(7) 0.0175(16) Uani 1 1 d U . .
H13 H 0.8632 0.4253 0.3207 0.021 Uiso 1 1 calc R . .
C15 C 1.0058(8) 0.1210(6) 0.8688(7) 0.0178(18) Uani 1 1 d . . .
H15A H 1.0618 0.1672 0.8358 0.027 Uiso 1 1 calc R . .
H15B H 1.0677 0.0638 0.9018 0.027 Uiso 1 1 calc R . .
H15C H 0.9805 0.1504 0.9403 0.027 Uiso 1 1 calc R . .
C16 C 0.7334(8) 0.1994(6) 0.6910(7) 0.0189(18) Uani 1 1 d . . .
H16A H 0.7216 0.2286 0.7689 0.028 Uiso 1 1 calc R . .
H16B H 0.6342 0.1870 0.6246 0.028 Uiso 1 1 calc R . .
H16C H 0.7894 0.2432 0.6547 0.028 Uiso 1 1 calc R . .
C17 C 1.0315(7) -0.2013(6) 0.6418(7) 0.0131(17) Uani 1 1 d . . .
C18 C 0.7318(9) 0.0227(5) 0.8234(7) 0.0180(18) Uani 1 1 d . . .
H18A H 0.7771 -0.0408 0.8497 0.027 Uiso 1 1 calc R . .
H18B H 0.6270 0.0151 0.7651 0.027 Uiso 1 1 calc R . .
H18C H 0.7356 0.0589 0.9018 0.027 Uiso 1 1 calc R . .


_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 C20 1.783(8) . ?
Fe1 C8 1.793(8) . ?
Fe1 P1 2.252(2) . ?
Fe1 S4 2.297(2) 3_756 ?
Fe1 S2 2.326(2) . ?
Fe1 S4 2.341(2) . ?
S4 C9 1.788(7) . ?
S4 Fe1 2.297(2) 3_756 ?
P1 C15 1.805(7) . ?
P1 C16 1.814(8) . ?
P1 C18 1.821(7) . ?
S2 C17 1.766(8) . ?
O2 C20 1.137(8) . ?
O1 C8 1.121(8) . ?
C9 C17 1.391(10) 3_756 ?
C9 C11 1.404(10) . ?
C10 C13 1.365(10) . ?
C10 C17 1.407(10) 3_756 ?
C10 H10 0.9500 . ?
C11 C12 1.382(10) . ?
C11 H11 0.9500 . ?
C12 C13 1.376(10) . ?
C12 H12 0.9500 . ?
C13 H13 0.9500 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 C9 1.391(10) 3_756 ?
C17 C10 1.407(10) 3_756 ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?

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
C20 Fe1 C8 92.6(3) . . ?
C20 Fe1 P1 92.9(2) . . ?
C8 Fe1 P1 92.8(2) . . ?
C20 Fe1 S4 92.3(2) . 3_756 ?
C8 Fe1 S4 89.9(2) . 3_756 ?
P1 Fe1 S4 174.11(8) . 3_756 ?
C20 Fe1 S2 179.7(3) . . ?
C8 Fe1 S2 87.3(2) . . ?
P1 Fe1 S2 87.39(8) . . ?
S4 Fe1 S2 87.48(7) 3_756 . ?
C20 Fe1 S4 94.0(2) . . ?
C8 Fe1 S4 171.3(2) . . ?
P1 Fe1 S4 92.52(8) . . ?
S4 Fe1 S4 84.22(7) 3_756 . ?
S2 Fe1 S4 86.10(7) . . ?
C9 S4 Fe1 101.5(2) . 3_756 ?
C9 S4 Fe1 109.2(2) . . ?
Fe1 S4 Fe1 95.78(7) 3_756 . ?
C15 P1 C16 103.7(4) . . ?
C15 P1 C18 102.6(4) . . ?
C16 P1 C18 103.5(4) . . ?
C15 P1 Fe1 115.9(2) . . ?
C16 P1 Fe1 116.2(3) . . ?
C18 P1 Fe1 113.2(3) . . ?
C17 S2 Fe1 101.8(2) . . ?
O2 C20 Fe1 175.6(7) . . ?
O1 C8 Fe1 177.1(7) . . ?
C17 C9 C11 120.6(7) 3_756 . ?
C17 C9 S4 120.1(6) 3_756 . ?
C11 C9 S4 119.2(6) . . ?
C13 C10 C17 120.2(7) . 3_756 ?
C13 C10 H10 119.9 . . ?
C17 C10 H10 119.9 3_756 . ?
C12 C11 C9 119.7(7) . . ?
C12 C11 H11 120.2 . . ?
C9 C11 H11 120.2 . . ?
C13 C12 C11 119.5(7) . . ?
C13 C12 H12 120.3 . . ?
C11 C12 H12 120.3 . . ?
C10 C13 C12 121.7(7) . . ?
C10 C13 H13 119.2 . . ?
C12 C13 H13 119.2 . . ?
P1 C15 H15A 109.5 . . ?
P1 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
P1 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
P1 C16 H16A 109.5 . . ?
P1 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
P1 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C9 C17 C10 118.3(7) 3_756 3_756 ?
C9 C17 S2 120.8(6) 3_756 . ?
C10 C17 S2 120.9(5) 3_756 . ?
P1 C18 H18A 109.5 . . ?
P1 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
P1 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.994
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.995
_refine_diff_density_max         0.923
_refine_diff_density_min         -0.693
_refine_diff_density_rms         0.155
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: Chloroform/hexane'
_chemical_properties_physical    Air-sensitive
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_femop2
_database_code_depnum_ccdc_archive 'CCDC 1853086'
loop_
_audit_author_name
_audit_author_address
'Satoru Tsukada'
;Hiroshima University
Japan
;
_audit_update_record             
;
2018-07-03 deposited with the CCDC.	2020-06-17 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C17 H22 Fe Mo O5 P2 S2'
_chemical_formula_weight         584.20

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   'Pbca '
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, y-1/2, z'

_cell_length_a                   13.9751(11)
_cell_length_b                   12.7350(10)
_cell_length_c                   25.293(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     4501.4(6)
_cell_formula_units_Z            8
_cell_measurement_temperature    103
_cell_measurement_reflns_used    5245
_cell_measurement_theta_min      2.70
_cell_measurement_theta_max      25.36
_exptl_crystal_description       block
_exptl_crystal_colour            black
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.04
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.724
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2352
_exptl_absorpt_coefficient_mu    1.554
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.6528
_exptl_absorpt_correction_T_max  0.9404
_exptl_absorpt_process_details   
;
SADABS Sheldrick 1996
;
_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      103
_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  'Bruker APEX CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean 8.333
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            21635
_diffrn_reflns_av_R_equivalents  0.0356
_diffrn_reflns_av_sigmaI/netI    0.0276
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_theta_min         1.61
_diffrn_reflns_theta_max         25.38
_reflns_number_total             4119
_reflns_number_gt                3476
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'SMART (Bruker AXS)'
_computing_cell_refinement       'SMART (Bruker AXS)'
_computing_data_reduction        'SAINT (Bruker AXS)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'XSHEL (Bruker AXS,2002)'
_computing_publication_material  'XCIF (Bruker AXS, 2001)'
_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² 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/[σ²(Fo²)+(0.0351P)²+7.7803P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4119
_refine_ls_number_parameters     259
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0430
_refine_ls_R_factor_gt           0.0325
_refine_ls_wR_factor_ref         0.0742
_refine_ls_wR_factor_gt          0.0705
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_restrained_S_all      1.070
_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
Mo1 Mo 1.032215(19) 0.36273(2) 0.144750(10) 0.01120(9) Uani 1 1 d . . .
Fe2 Fe 1.00006(3) 0.23882(4) 0.060543(18) 0.01322(12) Uani 1 1 d . . .
S1 S 0.94579(5) 0.40882(6) 0.05875(3) 0.01285(18) Uani 1 1 d . . .
P1 P 1.10782(6) 0.53693(7) 0.13501(3) 0.01322(19) Uani 1 1 d . . .
S2 S 0.90342(6) 0.22741(6) 0.13300(3) 0.01414(18) Uani 1 1 d . . .
P2 P 0.92726(6) 0.44359(7) 0.21521(3) 0.01527(19) Uani 1 1 d . . .
O4 O 0.87304(19) 0.1453(2) -0.01960(10) 0.0301(6) Uani 1 1 d . . .
O5 O 1.09697(17) 0.0494(2) 0.09850(10) 0.0253(6) Uani 1 1 d . . .
O1 O 1.24294(17) 0.30638(19) 0.11641(9) 0.0217(5) Uani 1 1 d . . .
O2 O 1.12006(18) 0.26172(19) 0.24583(10) 0.0235(6) Uani 1 1 d . . .
C11 C 1.0603(2) 0.1231(3) 0.08272(13) 0.0169(7) Uani 1 1 d . . .
C13 C 0.7518(2) 0.4575(3) 0.06243(13) 0.0182(7) Uani 1 1 d . . .
H13 H 0.7647 0.5130 0.0383 0.022 Uiso 1 1 calc R . .
C16 C 0.7138(2) 0.2943(3) 0.13252(13) 0.0186(7) Uani 1 1 d . . .
H16 H 0.7008 0.2387 0.1565 0.022 Uiso 1 1 calc R . .
C17 C 0.8048(2) 0.3081(3) 0.11298(13) 0.0152(7) Uani 1 1 d . . .
O3 O 1.15691(18) 0.3003(2) -0.00990(10) 0.0279(6) Uani 1 1 d . . .
C1 C 1.1627(2) 0.3265(3) 0.12313(12) 0.0152(7) Uani 1 1 d . . .
C9 C 1.0959(2) 0.2755(3) 0.01715(13) 0.0180(7) Uani 1 1 d . . .
C8 C 0.9889(3) 0.5215(3) 0.26545(13) 0.0213(8) Uani 1 1 d . . .
H8A H 1.0160 0.5846 0.2491 0.032 Uiso 1 1 calc R . .
H8B H 1.0404 0.4797 0.2812 0.032 Uiso 1 1 calc R . .
H8C H 0.9433 0.5421 0.2930 0.032 Uiso 1 1 calc R . .
C15 C 0.6410(2) 0.3620(3) 0.11703(14) 0.0204(8) Uani 1 1 d . . .
H15 H 0.5781 0.3525 0.1306 0.025 Uiso 1 1 calc R . .
C10 C 0.9209(2) 0.1819(3) 0.01130(14) 0.0186(7) Uani 1 1 d . . .
C2 C 1.0873(2) 0.3005(2) 0.20824(13) 0.0157(7) Uani 1 1 d . . .
C12 C 0.8243(2) 0.3908(3) 0.07820(13) 0.0136(7) Uani 1 1 d . . .
C7 C 0.8698(3) 0.3444(3) 0.25681(14) 0.0210(8) Uani 1 1 d . . .
H7A H 0.8373 0.3789 0.2864 0.031 Uiso 1 1 calc R . .
H7B H 0.9184 0.2960 0.2705 0.031 Uiso 1 1 calc R . .
H7C H 0.8230 0.3051 0.2358 0.031 Uiso 1 1 calc R . .
C6 C 0.8267(2) 0.5258(3) 0.19497(13) 0.0180(7) Uani 1 1 d . . .
H6A H 0.7724 0.4812 0.1852 0.027 Uiso 1 1 calc R . .
H6B H 0.8456 0.5687 0.1645 0.027 Uiso 1 1 calc R . .
H6C H 0.8082 0.5718 0.2243 0.027 Uiso 1 1 calc R . .
C3 C 1.1692(2) 0.5519(3) 0.07216(13) 0.0176(7) Uani 1 1 d . . .
H3A H 1.1965 0.6226 0.0698 0.026 Uiso 1 1 calc R . .
H3B H 1.1237 0.5413 0.0432 0.026 Uiso 1 1 calc R . .
H3C H 1.2206 0.4998 0.0696 0.026 Uiso 1 1 calc R . .
C14 C 0.6592(2) 0.4428(3) 0.08216(14) 0.0212(8) Uani 1 1 d . . .
H14 H 0.6090 0.4885 0.0716 0.025 Uiso 1 1 calc R . .
C4 C 1.0299(2) 0.6524(3) 0.13252(14) 0.0183(7) Uani 1 1 d . . .
H4A H 1.0683 0.7149 0.1249 0.028 Uiso 1 1 calc R . .
H4B H 0.9977 0.6610 0.1667 0.028 Uiso 1 1 calc R . .
H4C H 0.9819 0.6429 0.1046 0.028 Uiso 1 1 calc R . .
C5 C 1.1997(2) 0.5755(3) 0.18205(13) 0.0173(7) Uani 1 1 d . . .
H5A H 1.2534 0.5263 0.1800 0.026 Uiso 1 1 calc R . .
H5B H 1.1730 0.5746 0.2179 0.026 Uiso 1 1 calc R . .
H5C H 1.2221 0.6465 0.1737 0.026 Uiso 1 1 calc R . .


_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
Mo1 C2 1.949(3) . ?
Mo1 C1 1.959(3) . ?
Mo1 P1 2.4696(9) . ?
Mo1 S2 2.5095(9) . ?
Mo1 P2 2.5274(9) . ?
Mo1 S1 2.5562(8) . ?
Mo1 Fe2 2.6885(6) . ?
Fe2 C11 1.787(4) . ?
Fe2 C9 1.794(4) . ?
Fe2 C10 1.816(4) . ?
Fe2 S2 2.2812(9) . ?
Fe2 S1 2.2945(9) . ?
S1 C12 1.782(3) . ?
P1 C3 1.816(3) . ?
P1 C5 1.818(3) . ?
P1 C4 1.831(3) . ?
S2 C17 1.792(3) . ?
P2 C6 1.826(3) . ?
P2 C8 1.828(3) . ?
P2 C7 1.830(3) . ?
O4 C10 1.130(4) . ?
O5 C11 1.142(4) . ?
O1 C1 1.163(4) . ?
O2 C2 1.165(4) . ?
C13 C12 1.381(5) . ?
C13 C14 1.400(5) . ?
C13 H13 0.9500 . ?
C16 C17 1.376(5) . ?
C16 C15 1.390(5) . ?
C16 H16 0.9500 . ?
C17 C12 1.399(5) . ?
O3 C9 1.137(4) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C15 C14 1.379(5) . ?
C15 H15 0.9500 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C14 H14 0.9500 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?

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
C2 Mo1 C1 76.52(13) . . ?
C2 Mo1 P1 106.18(10) . . ?
C1 Mo1 P1 77.60(10) . . ?
C2 Mo1 S2 95.82(10) . . ?
C1 Mo1 S2 118.23(10) . . ?
P1 Mo1 S2 155.77(3) . . ?
C2 Mo1 P2 79.27(10) . . ?
C1 Mo1 P2 146.41(10) . . ?
P1 Mo1 P2 87.28(3) . . ?
S2 Mo1 P2 86.96(3) . . ?
C2 Mo1 S1 168.80(10) . . ?
C1 Mo1 S1 104.85(9) . . ?
P1 Mo1 S1 84.89(3) . . ?
S2 Mo1 S1 73.63(3) . . ?
P2 Mo1 S1 103.43(3) . . ?
C2 Mo1 Fe2 118.69(9) . . ?
C1 Mo1 Fe2 78.25(9) . . ?
P1 Mo1 Fe2 121.32(2) . . ?
S2 Mo1 Fe2 51.92(2) . . ?
P2 Mo1 Fe2 134.49(3) . . ?
S1 Mo1 Fe2 51.81(2) . . ?
C11 Fe2 C9 93.14(15) . . ?
C11 Fe2 C10 99.99(15) . . ?
C9 Fe2 C10 98.01(15) . . ?
C11 Fe2 S2 88.53(11) . . ?
C9 Fe2 S2 161.85(11) . . ?
C10 Fe2 S2 99.49(11) . . ?
C11 Fe2 S1 160.01(11) . . ?
C9 Fe2 S1 89.37(11) . . ?
C10 Fe2 S1 99.29(11) . . ?
S2 Fe2 S1 83.12(3) . . ?
C11 Fe2 Mo1 99.00(11) . . ?
C9 Fe2 Mo1 101.94(11) . . ?
C10 Fe2 Mo1 151.52(11) . . ?
S2 Fe2 Mo1 59.99(2) . . ?
S1 Fe2 Mo1 61.12(2) . . ?
C12 S1 Fe2 100.82(11) . . ?
C12 S1 Mo1 100.69(11) . . ?
Fe2 S1 Mo1 67.07(2) . . ?
C3 P1 C5 102.17(16) . . ?
C3 P1 C4 99.59(16) . . ?
C5 P1 C4 103.04(16) . . ?
C3 P1 Mo1 112.55(11) . . ?
C5 P1 Mo1 118.67(11) . . ?
C4 P1 Mo1 118.05(12) . . ?
C17 S2 Fe2 101.05(11) . . ?
C17 S2 Mo1 101.02(11) . . ?
Fe2 S2 Mo1 68.09(3) . . ?
C6 P2 C8 104.25(16) . . ?
C6 P2 C7 102.71(16) . . ?
C8 P2 C7 100.48(17) . . ?
C6 P2 Mo1 118.85(11) . . ?
C8 P2 Mo1 115.97(12) . . ?
C7 P2 Mo1 112.25(11) . . ?
O5 C11 Fe2 177.6(3) . . ?
C12 C13 C14 119.5(3) . . ?
C12 C13 H13 120.2 . . ?
C14 C13 H13 120.2 . . ?
C17 C16 C15 119.8(3) . . ?
C17 C16 H16 120.1 . . ?
C15 C16 H16 120.1 . . ?
C16 C17 C12 120.2(3) . . ?
C16 C17 S2 122.4(3) . . ?
C12 C17 S2 117.3(2) . . ?
O1 C1 Mo1 172.1(3) . . ?
O3 C9 Fe2 178.9(3) . . ?
P2 C8 H8A 109.5 . . ?
P2 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
P2 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C14 C15 C16 120.5(3) . . ?
C14 C15 H15 119.8 . . ?
C16 C15 H15 119.8 . . ?
O4 C10 Fe2 178.7(3) . . ?
O2 C2 Mo1 178.9(3) . . ?
C13 C12 C17 120.1(3) . . ?
C13 C12 S1 122.7(3) . . ?
C17 C12 S1 117.2(2) . . ?
P2 C7 H7A 109.5 . . ?
P2 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
P2 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
P2 C6 H6A 109.5 . . ?
P2 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
P2 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
P1 C3 H3A 109.5 . . ?
P1 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
P1 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
C15 C14 C13 119.9(3) . . ?
C15 C14 H14 120.0 . . ?
C13 C14 H14 120.0 . . ?
P1 C4 H4A 109.5 . . ?
P1 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
P1 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
P1 C5 H5A 109.5 . . ?
P1 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
P1 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.711
_refine_diff_density_min         -0.999
_refine_diff_density_rms         0.095
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: dichloromethane/hexane'
_chemical_properties_physical    Air-sensitive
