# Electronic Supplementary Material (ESI) for ChemComm.
# This journal is © The Royal Society of Chemistry 2018

####################################################################### 
# 
# 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_1
_database_code_depnum_ccdc_archive 'CCDC 1434935'
_audit_update_record             
;
2018-08-01 deposited with the CCDC.
2018-10-29 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C20 H36 Cl F6 Fe2 N3 P S2'
_chemical_formula_weight         674.76

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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                   16.1521(9)
_cell_length_b                   17.3762(9)
_cell_length_c                   20.4850(11)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     5749.4(5)
_cell_formula_units_Z            8
_cell_measurement_temperature    299(2)
_cell_measurement_reflns_used    9894
_cell_measurement_theta_min      2.35
_cell_measurement_theta_max      27.26

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.31
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.559
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2776
_exptl_absorpt_coefficient_mu    1.357
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  0.6197
_exptl_absorpt_correction_T_max  0.6784
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      299(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  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            34478
_diffrn_reflns_av_R_equivalents  0.0445
_diffrn_reflns_av_sigmaI/netI    0.0282
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         2.34
_diffrn_reflns_theta_max         25.00
_reflns_number_total             5051
_reflns_number_gt                3889
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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)+(0.1121P)²+9.3000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5051
_refine_ls_number_parameters     314
_refine_ls_number_restraints     25
_refine_ls_R_factor_all          0.0799
_refine_ls_R_factor_gt           0.0618
_refine_ls_wR_factor_ref         0.1887
_refine_ls_wR_factor_gt          0.1773
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_restrained_S_all      1.041
_refine_ls_shift/su_max          0.019
_refine_ls_shift/su_mean         0.002

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 0.76125(4) 0.18317(4) 0.41419(3) 0.0478(2) Uani 1 1 d U . .
Fe2 Fe 0.64209(4) 0.15419(4) 0.53116(3) 0.0515(2) Uani 1 1 d . . .
S2 S 0.73183(9) 0.26096(8) 0.49946(6) 0.0567(4) Uani 1 1 d . . .
S1 S 0.69385(10) 0.07381(8) 0.44498(7) 0.0653(4) Uani 1 1 d U . .
N1 N 0.6438(4) 0.0402(4) 0.5860(3) 0.0906(17) Uani 1 1 d U . .
C15 C 0.6818(4) 0.1881(4) 0.3343(2) 0.0696(17) Uani 1 1 d . . .
N2 N 0.6868(3) 0.1942(3) 0.6294(2) 0.0677(12) Uani 1 1 d U . .
C16 C 0.7580(4) 0.1535(4) 0.3144(3) 0.0676(16) Uani 1 1 d . . .
C17 C 0.8196(4) 0.2093(4) 0.3220(3) 0.0686(16) Uani 1 1 d . . .
C18 C 0.7851(4) 0.2762(3) 0.3481(3) 0.0649(14) Uani 1 1 d . . .
C14 C 0.6989(4) 0.2620(4) 0.3546(2) 0.0710(17) Uani 1 1 d . . .
C4 C 0.7489(5) 0.0104(4) 0.5000(5) 0.100(2) Uani 1 1 d U . .
H4A H 0.7758 -0.0307 0.4761 0.119 Uiso 1 1 calc R . .
H4B H 0.7905 0.0386 0.5244 0.119 Uiso 1 1 calc R . .
C10 C 0.6359(6) 0.3219(6) 0.3742(4) 0.125(4) Uani 1 1 d . . .
H10A H 0.6178 0.3495 0.3361 0.188 Uiso 1 1 calc R . .
H10B H 0.6606 0.3572 0.4045 0.188 Uiso 1 1 calc R . .
H10C H 0.5893 0.2972 0.3943 0.188 Uiso 1 1 calc R . .
C5 C 0.8010(4) 0.2562(4) 0.5693(3) 0.0724(16) Uani 1 1 d U . .
H5A H 0.8558 0.2418 0.5542 0.087 Uiso 1 1 calc R . .
H5B H 0.8050 0.3069 0.5887 0.087 Uiso 1 1 calc R . .
C12 C 0.7681(7) 0.0736(5) 0.2864(4) 0.124(3) Uani 1 1 d . . .
H12A H 0.7640 0.0758 0.2397 0.185 Uiso 1 1 calc R . .
H12B H 0.7255 0.0407 0.3033 0.185 Uiso 1 1 calc R . .
H12C H 0.8214 0.0535 0.2984 0.185 Uiso 1 1 calc R . .
C6 C 0.7746(5) 0.2017(5) 0.6191(4) 0.0943(19) Uani 1 1 d U . .
H6A H 0.7964 0.1514 0.6077 0.113 Uiso 1 1 calc R . .
H6B H 0.7998 0.2167 0.6602 0.113 Uiso 1 1 calc R . .
C8 C 0.6409(7) 0.2566(6) 0.6539(4) 0.138(4) Uani 1 1 d . . .
H8A H 0.6625 0.2714 0.6957 0.207 Uiso 1 1 calc R . .
H8B H 0.5839 0.2418 0.6584 0.207 Uiso 1 1 calc R . .
H8C H 0.6449 0.2993 0.6243 0.207 Uiso 1 1 calc R . .
C13 C 0.9099(5) 0.2011(6) 0.3057(4) 0.113(3) Uani 1 1 d . . .
H13A H 0.9191 0.2170 0.2614 0.169 Uiso 1 1 calc R . .
H13B H 0.9263 0.1484 0.3108 0.169 Uiso 1 1 calc R . .
H13C H 0.9420 0.2329 0.3345 0.169 Uiso 1 1 calc R . .
C7 C 0.5577(7) 0.0114(6) 0.5960(5) 0.142(4) Uani 1 1 d . . .
H7A H 0.5593 -0.0366 0.6191 0.213 Uiso 1 1 calc R . .
H7B H 0.5316 0.0040 0.5543 0.213 Uiso 1 1 calc R . .
H7C H 0.5268 0.0484 0.6208 0.213 Uiso 1 1 calc R . .
C11 C 0.5979(5) 0.1511(7) 0.3283(4) 0.122(4) Uani 1 1 d . . .
H11A H 0.5747 0.1628 0.2863 0.183 Uiso 1 1 calc R . .
H11B H 0.5621 0.1704 0.3619 0.183 Uiso 1 1 calc R . .
H11C H 0.6034 0.0963 0.3329 0.183 Uiso 1 1 calc R . .
C3 C 0.6817(6) -0.0220(5) 0.5461(5) 0.118(2) Uani 1 1 d U . .
H3A H 0.6391 -0.0471 0.5205 0.142 Uiso 1 1 calc R . .
H3B H 0.7063 -0.0602 0.5747 0.142 Uiso 1 1 calc R . .
C9 C 0.8292(6) 0.3502(5) 0.3623(4) 0.109(3) Uani 1 1 d . . .
H9A H 0.8306 0.3812 0.3235 0.163 Uiso 1 1 calc R . .
H9B H 0.8847 0.3393 0.3762 0.163 Uiso 1 1 calc R . .
H9C H 0.8005 0.3773 0.3962 0.163 Uiso 1 1 calc R . .
Cl1 Cl 0.50832(10) 0.18351(11) 0.51707(9) 0.0817(5) Uani 1 1 d . . .
P1 P 0.45414(10) 0.46980(10) 0.31806(9) 0.0733(5) Uani 1 1 d . . .
N3 N 0.8667(3) 0.1509(3) 0.4481(2) 0.0597(11) Uani 1 1 d . . .
C19 C 0.9304(4) 0.1327(3) 0.4644(3) 0.0581(13) Uani 1 1 d . . .
C20 C 1.0135(3) 0.1097(4) 0.4847(3) 0.0724(16) Uani 1 1 d . . .
H20A H 1.0322 0.0679 0.4578 0.109 Uiso 1 1 calc R . .
H20B H 1.0123 0.0936 0.5295 0.109 Uiso 1 1 calc R . .
H20C H 1.0505 0.1526 0.4800 0.109 Uiso 1 1 calc R . .
C2 C 0.6795(3) 0.0552(6) 0.6489(3) 0.127(4) Uani 1 1 d R . .
H2A H 0.6511 0.0228 0.6803 0.153 Uiso 1 1 calc R . .
H2B H 0.7366 0.0381 0.6475 0.153 Uiso 1 1 calc R . .
C1 C 0.6793(9) 0.1291(6) 0.6733(3) 0.140(4) Uani 1 1 d . . .
H1A H 0.7242 0.1327 0.7046 0.168 Uiso 1 1 calc R . .
H1B H 0.6282 0.1357 0.6976 0.168 Uiso 1 1 calc R . .
F1 F 0.5344(3) 0.4846(3) 0.3601(3) 0.1132(15) Uani 1 1 d . . .
F2 F 0.3710(3) 0.4540(4) 0.2810(3) 0.1244(17) Uani 1 1 d . . .
F3 F 0.4293(5) 0.5533(4) 0.3299(4) 0.191(4) Uani 1 1 d . . .
F4 F 0.4142(6) 0.4447(8) 0.3795(4) 0.296(8) Uani 1 1 d . . .
F5 F 0.4974(5) 0.4910(9) 0.2582(4) 0.280(8) Uani 1 1 d . . .
F6 F 0.4773(7) 0.3884(5) 0.3044(8) 0.295(8) Uani 1 1 d . . .


_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 N3 1.923(5) . ?
Fe1 C15 2.082(5) . ?
Fe1 C14 2.094(5) . ?
Fe1 C16 2.109(5) . ?
Fe1 C18 2.144(6) . ?
Fe1 C17 2.159(5) . ?
Fe1 S2 2.2592(14) . ?
Fe1 S1 2.2791(17) . ?
Fe2 Cl1 2.2385(17) . ?
Fe2 N2 2.248(5) . ?
Fe2 N1 2.278(5) . ?
Fe2 S1 2.4014(16) . ?
Fe2 S2 2.4423(16) . ?
S2 C5 1.817(6) . ?
S1 C4 1.810(8) . ?
N1 C2 1.435(10) . ?
N1 C3 1.487(11) . ?
N1 C7 1.492(11) . ?
C15 C14 1.378(9) . ?
C15 C16 1.430(8) . ?
C15 C11 1.505(9) . ?
N2 C8 1.407(9) . ?
N2 C6 1.440(9) . ?
N2 C1 1.451(10) . ?
C16 C17 1.397(9) . ?
C16 C12 1.511(10) . ?
C17 C18 1.396(9) . ?
C17 C13 1.503(9) . ?
C18 C14 1.420(9) . ?
C18 C9 1.497(10) . ?
C14 C10 1.510(9) . ?
C4 C3 1.545(12) . ?
C5 C6 1.455(10) . ?
P1 F5 1.459(8) . ?
P1 F4 1.479(7) . ?
P1 F6 1.490(7) . ?
P1 F3 1.525(6) . ?
P1 F2 1.567(5) . ?
P1 F1 1.578(4) . ?
N3 C19 1.127(7) . ?
C19 C20 1.460(7) . ?
C2 C1 1.379(13) . ?

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
N3 Fe1 C15 147.3(2) . . ?
N3 Fe1 C14 145.8(3) . . ?
C15 Fe1 C14 38.5(3) . . ?
N3 Fe1 C16 107.5(2) . . ?
C15 Fe1 C16 39.9(2) . . ?
C14 Fe1 C16 65.3(2) . . ?
N3 Fe1 C18 106.8(2) . . ?
C15 Fe1 C18 65.4(3) . . ?
C14 Fe1 C18 39.1(3) . . ?
C16 Fe1 C18 64.9(2) . . ?
N3 Fe1 C17 89.4(2) . . ?
C15 Fe1 C17 64.7(2) . . ?
C14 Fe1 C17 64.0(2) . . ?
C16 Fe1 C17 38.2(2) . . ?
C18 Fe1 C17 37.9(2) . . ?
N3 Fe1 S2 94.69(14) . . ?
C15 Fe1 S2 116.97(18) . . ?
C14 Fe1 S2 87.61(16) . . ?
C16 Fe1 S2 152.93(18) . . ?
C18 Fe1 S2 94.30(17) . . ?
C17 Fe1 S2 130.0(2) . . ?
N3 Fe1 S1 94.61(15) . . ?
C15 Fe1 S1 87.6(2) . . ?
C14 Fe1 S1 118.5(2) . . ?
C16 Fe1 S1 93.0(2) . . ?
C18 Fe1 S1 152.81(17) . . ?
C17 Fe1 S1 128.7(2) . . ?
S2 Fe1 S1 100.63(6) . . ?
Cl1 Fe2 N2 110.80(14) . . ?
Cl1 Fe2 N1 105.87(18) . . ?
N2 Fe2 N1 79.8(2) . . ?
Cl1 Fe2 S1 111.94(7) . . ?
N2 Fe2 S1 136.56(14) . . ?
N1 Fe2 S1 81.51(18) . . ?
Cl1 Fe2 S2 111.45(7) . . ?
N2 Fe2 S2 79.17(13) . . ?
N1 Fe2 S2 141.67(18) . . ?
S1 Fe2 S2 92.28(5) . . ?
C5 S2 Fe1 116.9(2) . . ?
C5 S2 Fe2 96.9(2) . . ?
Fe1 S2 Fe2 82.87(5) . . ?
C4 S1 Fe1 116.4(3) . . ?
C4 S1 Fe2 93.9(3) . . ?
Fe1 S1 Fe2 83.38(5) . . ?
C2 N1 C3 117.4(7) . . ?
C2 N1 C7 108.2(6) . . ?
C3 N1 C7 102.5(8) . . ?
C2 N1 Fe2 106.8(5) . . ?
C3 N1 Fe2 111.5(5) . . ?
C7 N1 Fe2 110.3(5) . . ?
C14 C15 C16 107.8(6) . . ?
C14 C15 C11 127.2(7) . . ?
C16 C15 C11 124.9(7) . . ?
C14 C15 Fe1 71.2(3) . . ?
C16 C15 Fe1 71.1(3) . . ?
C11 C15 Fe1 126.9(5) . . ?
C8 N2 C6 120.1(7) . . ?
C8 N2 C1 109.6(7) . . ?
C6 N2 C1 104.1(7) . . ?
C8 N2 Fe2 112.9(4) . . ?
C6 N2 Fe2 102.3(4) . . ?
C1 N2 Fe2 106.7(5) . . ?
C17 C16 C15 106.8(6) . . ?
C17 C16 C12 127.1(7) . . ?
C15 C16 C12 126.0(7) . . ?
C17 C16 Fe1 72.8(3) . . ?
C15 C16 Fe1 69.1(3) . . ?
C12 C16 Fe1 126.1(5) . . ?
C18 C17 C16 109.7(5) . . ?
C18 C17 C13 123.4(7) . . ?
C16 C17 C13 126.9(7) . . ?
C18 C17 Fe1 70.5(3) . . ?
C16 C17 Fe1 69.0(3) . . ?
C13 C17 Fe1 126.7(5) . . ?
C17 C18 C14 106.4(6) . . ?
C17 C18 C9 126.9(7) . . ?
C14 C18 C9 126.6(7) . . ?
C17 C18 Fe1 71.6(3) . . ?
C14 C18 Fe1 68.5(3) . . ?
C9 C18 Fe1 127.6(4) . . ?
C15 C14 C18 109.3(5) . . ?
C15 C14 C10 126.0(7) . . ?
C18 C14 C10 124.5(8) . . ?
C15 C14 Fe1 70.3(3) . . ?
C18 C14 Fe1 72.4(3) . . ?
C10 C14 Fe1 128.3(4) . . ?
C3 C4 S1 104.9(6) . . ?
C6 C5 S2 113.7(5) . . ?
N2 C6 C5 116.7(6) . . ?
N1 C3 C4 111.1(7) . . ?
F5 P1 F4 176.5(8) . . ?
F5 P1 F6 87.8(8) . . ?
F4 P1 F6 89.3(8) . . ?
F5 P1 F3 91.1(7) . . ?
F4 P1 F3 91.8(8) . . ?
F6 P1 F3 178.2(6) . . ?
F5 P1 F2 92.7(4) . . ?
F4 P1 F2 89.3(3) . . ?
F6 P1 F2 87.6(4) . . ?
F3 P1 F2 91.0(4) . . ?
F5 P1 F1 91.4(4) . . ?
F4 P1 F1 86.7(3) . . ?
F6 P1 F1 93.0(4) . . ?
F3 P1 F1 88.5(3) . . ?
F2 P1 F1 175.9(3) . . ?
C19 N3 Fe1 176.0(5) . . ?
N3 C19 C20 179.0(6) . . ?
C1 C2 N1 119.7(6) . . ?
C2 C1 N2 120.0(6) . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         1.259
_refine_diff_density_min         -0.631
_refine_diff_density_rms         0.090
####################################################################### 
# 
# 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_2
_database_code_depnum_ccdc_archive 'CCDC 1434939'
_audit_update_record             
;
2016-01-22 deposited with the CCDC.
2018-10-29 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C19 H35 Cl2 Fe2 N2 S2'
_chemical_formula_weight         538.21

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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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                   14.7655(4)
_cell_length_b                   11.1673(3)
_cell_length_c                   14.2254(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 95.3012(11)
_cell_angle_gamma                90.00
_cell_volume                     2335.60(11)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    9045
_cell_measurement_theta_min      3.32
_cell_measurement_theta_max      39.07

_exptl_crystal_description       block
_exptl_crystal_colour            pink
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.24
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.531
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1124
_exptl_absorpt_coefficient_mu    1.658
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  0.6820
_exptl_absorpt_correction_T_max  0.6917
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      173(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  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            39653
_diffrn_reflns_av_R_equivalents  0.0307
_diffrn_reflns_av_sigmaI/netI    0.0160
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         2.29
_diffrn_reflns_theta_max         25.00
_reflns_number_total             4112
_reflns_number_gt                3951
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'


_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)+(0.0594P)²+15.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4112
_refine_ls_number_parameters     244
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0537
_refine_ls_R_factor_gt           0.0521
_refine_ls_wR_factor_ref         0.1328
_refine_ls_wR_factor_gt          0.1318
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_restrained_S_all      1.016
_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 0.77522(4) 0.66724(6) 0.06256(4) 0.02061(18) Uani 1 1 d . . .
Fe2 Fe 0.70637(4) 0.36023(5) 0.15870(4) 0.01599(17) Uani 1 1 d . . .
S1 S 0.78926(8) 0.46300(10) 0.04630(7) 0.0231(3) Uani 1 1 d . . .
Cl1 Cl 0.63160(7) 0.20034(10) 0.09147(8) 0.0254(3) Uani 1 1 d . . .
S5 S 0.61777(8) 0.54524(10) 0.16837(8) 0.0266(3) Uani 1 1 d . . .
Cl2 Cl 0.91292(9) 0.70191(12) 0.14923(9) 0.0371(3) Uani 1 1 d . . .
N7 N 0.8435(2) 0.3191(3) 0.2272(2) 0.0183(7) Uani 1 1 d . . .
C19 C 0.7642(3) 0.8443(4) 0.0113(3) 0.0203(9) Uani 1 1 d . . .
N2 N 0.6734(3) 0.3394(4) 0.3098(3) 0.0261(8) Uani 1 1 d . . .
C18 C 0.6770(3) 0.7923(4) 0.0092(3) 0.0204(9) Uani 1 1 d . . .
C7 C 0.9032(3) 0.4154(5) 0.0881(3) 0.0296(11) Uani 1 1 d . . .
H7A H 0.9169 0.3388 0.0575 0.035 Uiso 1 1 calc R . .
H7B H 0.9475 0.4758 0.0701 0.035 Uiso 1 1 calc R . .
C8 C 0.5977(4) 0.2555(5) 0.3184(3) 0.0322(11) Uani 1 1 d . . .
H8A H 0.5855 0.2492 0.3847 0.048 Uiso 1 1 calc R . .
H8B H 0.6139 0.1765 0.2951 0.048 Uiso 1 1 calc R . .
H8C H 0.5432 0.2849 0.2809 0.048 Uiso 1 1 calc R . .
C9 C 0.8637(3) 0.1936(4) 0.2037(4) 0.0280(10) Uani 1 1 d . . .
H9A H 0.9243 0.1720 0.2326 0.042 Uiso 1 1 calc R . .
H9B H 0.8618 0.1848 0.1350 0.042 Uiso 1 1 calc R . .
H9C H 0.8182 0.1407 0.2280 0.042 Uiso 1 1 calc R . .
C16 C 0.7620(3) 0.6848(4) -0.0898(3) 0.0239(10) Uani 1 1 d . . .
C15 C 0.8160(3) 0.7784(4) -0.0510(3) 0.0224(9) Uani 1 1 d . . .
C13 C 0.5978(3) 0.8407(4) 0.0562(4) 0.0301(11) Uani 1 1 d . . .
H13A H 0.5640 0.8976 0.0139 0.045 Uiso 1 1 calc R . .
H13B H 0.6201 0.8815 0.1149 0.045 Uiso 1 1 calc R . .
H13C H 0.5577 0.7746 0.0707 0.045 Uiso 1 1 calc R . .
C11 C 0.7882(4) 0.5967(5) -0.1622(3) 0.0359(12) Uani 1 1 d . . .
H11A H 0.7737 0.6302 -0.2255 0.054 Uiso 1 1 calc R . .
H11B H 0.7543 0.5221 -0.1564 0.054 Uiso 1 1 calc R . .
H11C H 0.8536 0.5804 -0.1521 0.054 Uiso 1 1 calc R . .
C17 C 0.6754(3) 0.6902(4) -0.0510(3) 0.0229(9) Uani 1 1 d . . .
C14 C 0.7977(3) 0.9529(4) 0.0654(3) 0.0284(10) Uani 1 1 d . . .
H14A H 0.7849 1.0244 0.0265 0.043 Uiso 1 1 calc R . .
H14B H 0.8634 0.9461 0.0818 0.043 Uiso 1 1 calc R . .
H14C H 0.7668 0.9592 0.1232 0.043 Uiso 1 1 calc R . .
C3 C 0.6530(4) 0.4557(5) 0.3507(3) 0.0322(11) Uani 1 1 d . . .
H3A H 0.7100 0.5025 0.3613 0.039 Uiso 1 1 calc R . .
H3B H 0.6294 0.4426 0.4128 0.039 Uiso 1 1 calc R . .
C6 C 0.9138(3) 0.3993(4) 0.1946(3) 0.0247(9) Uani 1 1 d . . .
H6A H 0.9747 0.3656 0.2140 0.030 Uiso 1 1 calc R . .
H6B H 0.9096 0.4784 0.2253 0.030 Uiso 1 1 calc R . .
C2 C 0.5853(4) 0.5264(5) 0.2897(3) 0.0323(11) Uani 1 1 d . . .
H2A H 0.5785 0.6063 0.3183 0.039 Uiso 1 1 calc R . .
H2B H 0.5255 0.4856 0.2871 0.039 Uiso 1 1 calc R . .
C12 C 0.5957(4) 0.6114(5) -0.0793(4) 0.0373(12) Uani 1 1 d . . .
H12A H 0.5609 0.6450 -0.1351 0.056 Uiso 1 1 calc R . .
H12B H 0.5567 0.6064 -0.0273 0.056 Uiso 1 1 calc R . .
H12C H 0.6172 0.5311 -0.0939 0.056 Uiso 1 1 calc R . .
C4 C 0.7554(3) 0.2849(5) 0.3639(3) 0.0303(11) Uani 1 1 d . . .
H4A H 0.7540 0.3026 0.4319 0.036 Uiso 1 1 calc R . .
H4B H 0.7536 0.1968 0.3559 0.036 Uiso 1 1 calc R . .
C5 C 0.8414(3) 0.3321(5) 0.3311(3) 0.0289(10) Uani 1 1 d . . .
H5A H 0.8478 0.4178 0.3483 0.035 Uiso 1 1 calc R . .
H5B H 0.8936 0.2885 0.3636 0.035 Uiso 1 1 calc R . .
C10 C 0.9114(3) 0.8091(5) -0.0729(4) 0.0359(12) Uani 1 1 d . . .
H10A H 0.9087 0.8614 -0.1284 0.054 Uiso 1 1 calc R . .
H10B H 0.9441 0.7355 -0.0857 0.054 Uiso 1 1 calc R . .
H10C H 0.9432 0.8505 -0.0187 0.054 Uiso 1 1 calc R . .
C1 C 0.7128(3) 0.6451(4) 0.1823(3) 0.0301(11) Uani 1 1 d . . .
H1A H 0.7575 0.6138 0.2324 0.036 Uiso 1 1 calc R . .
H1B H 0.6918 0.7241 0.2032 0.036 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 C1 2.025(5) . ?
Fe1 C17 2.100(4) . ?
Fe1 C18 2.104(4) . ?
Fe1 C19 2.109(4) . ?
Fe1 C15 2.166(4) . ?
Fe1 C16 2.167(4) . ?
Fe1 S1 2.3038(13) . ?
Fe1 Cl2 2.3109(14) . ?
Fe2 N7 2.213(3) . ?
Fe2 N2 2.259(4) . ?
Fe2 Cl1 2.2642(12) . ?
Fe2 S1 2.3945(12) . ?
Fe2 S5 2.4561(12) . ?
S1 C7 1.812(5) . ?
S5 C1 1.789(5) . ?
S5 C2 1.846(5) . ?
N7 C6 1.476(6) . ?
N7 C9 1.478(6) . ?
N7 C5 1.488(6) . ?
C19 C18 1.410(6) . ?
C19 C15 1.428(6) . ?
C19 C14 1.495(6) . ?
N2 C3 1.466(6) . ?
N2 C8 1.472(6) . ?
N2 C4 1.502(6) . ?
C18 C17 1.426(6) . ?
C18 C13 1.500(6) . ?
C7 C6 1.520(7) . ?
C16 C15 1.397(7) . ?
C16 C17 1.440(7) . ?
C16 C11 1.500(6) . ?
C15 C10 1.509(7) . ?
C17 C12 1.494(7) . ?
C3 C2 1.489(7) . ?
C4 C5 1.488(7) . ?

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 C17 108.68(19) . . ?
C1 Fe1 C18 91.87(19) . . ?
C17 Fe1 C18 39.65(17) . . ?
C1 Fe1 C19 112.26(18) . . ?
C17 Fe1 C19 66.02(17) . . ?
C18 Fe1 C19 39.12(17) . . ?
C1 Fe1 C15 151.24(19) . . ?
C17 Fe1 C15 65.19(17) . . ?
C18 Fe1 C15 65.20(16) . . ?
C19 Fe1 C15 38.99(16) . . ?
C1 Fe1 C16 147.8(2) . . ?
C17 Fe1 C16 39.42(18) . . ?
C18 Fe1 C16 65.41(17) . . ?
C19 Fe1 C16 64.70(17) . . ?
C15 Fe1 C16 37.63(17) . . ?
C1 Fe1 S1 90.89(14) . . ?
C17 Fe1 S1 96.13(13) . . ?
C18 Fe1 S1 133.35(13) . . ?
C19 Fe1 S1 153.97(12) . . ?
C15 Fe1 S1 117.30(12) . . ?
C16 Fe1 S1 89.40(12) . . ?
C1 Fe1 Cl2 91.03(15) . . ?
C17 Fe1 Cl2 155.59(13) . . ?
C18 Fe1 Cl2 128.63(13) . . ?
C19 Fe1 Cl2 93.62(12) . . ?
C15 Fe1 Cl2 90.58(13) . . ?
C16 Fe1 Cl2 120.79(14) . . ?
S1 Fe1 Cl2 97.85(5) . . ?
N7 Fe2 N2 80.12(14) . . ?
N7 Fe2 Cl1 114.40(10) . . ?
N2 Fe2 Cl1 100.44(11) . . ?
N7 Fe2 S1 83.69(10) . . ?
N2 Fe2 S1 148.54(11) . . ?
Cl1 Fe2 S1 110.81(4) . . ?
N7 Fe2 S5 128.34(10) . . ?
N2 Fe2 S5 82.57(11) . . ?
Cl1 Fe2 S5 116.46(5) . . ?
S1 Fe2 S5 86.67(4) . . ?
C7 S1 Fe1 110.29(18) . . ?
C7 S1 Fe2 99.01(15) . . ?
Fe1 S1 Fe2 110.56(5) . . ?
C1 S5 C2 103.7(2) . . ?
C1 S5 Fe2 96.54(17) . . ?
C2 S5 Fe2 98.17(17) . . ?
C6 N7 C9 110.0(3) . . ?
C6 N7 C5 109.4(4) . . ?
C9 N7 C5 109.9(4) . . ?
C6 N7 Fe2 112.1(3) . . ?
C9 N7 Fe2 107.0(3) . . ?
C5 N7 Fe2 108.3(3) . . ?
C18 C19 C15 108.3(4) . . ?
C18 C19 C14 127.1(4) . . ?
C15 C19 C14 124.5(4) . . ?
C18 C19 Fe1 70.3(2) . . ?
C15 C19 Fe1 72.7(2) . . ?
C14 C19 Fe1 124.8(3) . . ?
C3 N2 C8 110.2(4) . . ?
C3 N2 C4 109.9(4) . . ?
C8 N2 C4 106.4(4) . . ?
C3 N2 Fe2 110.9(3) . . ?
C8 N2 Fe2 112.1(3) . . ?
C4 N2 Fe2 107.1(3) . . ?
C19 C18 C17 107.9(4) . . ?
C19 C18 C13 126.1(4) . . ?
C17 C18 C13 125.9(4) . . ?
C19 C18 Fe1 70.6(2) . . ?
C17 C18 Fe1 70.0(2) . . ?
C13 C18 Fe1 128.1(3) . . ?
C6 C7 S1 111.6(3) . . ?
C15 C16 C17 108.2(4) . . ?
C15 C16 C11 126.0(4) . . ?
C17 C16 C11 125.8(5) . . ?
C15 C16 Fe1 71.2(2) . . ?
C17 C16 Fe1 67.8(2) . . ?
C11 C16 Fe1 128.5(3) . . ?
C16 C15 C19 108.2(4) . . ?
C16 C15 C10 126.7(4) . . ?
C19 C15 C10 125.0(4) . . ?
C16 C15 Fe1 71.2(2) . . ?
C19 C15 Fe1 68.3(2) . . ?
C10 C15 Fe1 127.8(3) . . ?
C18 C17 C16 107.3(4) . . ?
C18 C17 C12 127.0(4) . . ?
C16 C17 C12 125.3(4) . . ?
C18 C17 Fe1 70.4(2) . . ?
C16 C17 Fe1 72.8(3) . . ?
C12 C17 Fe1 127.9(3) . . ?
N2 C3 C2 112.9(4) . . ?
N7 C6 C7 112.0(4) . . ?
C3 C2 S5 112.8(3) . . ?
C5 C4 N2 111.5(4) . . ?
N7 C5 C4 112.0(4) . . ?
S5 C1 Fe1 113.4(2) . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         2.373
_refine_diff_density_min         -1.105
_refine_diff_density_rms         0.115
####################################################################### 
# 
# 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_2_CCDC1
_database_code_depnum_ccdc_archive 'CCDC 1447555'
_audit_update_record             
;
2018-08-01 deposited with the CCDC.
2018-10-29 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C21 H38 Cl F6 Fe2 N3 P S2'
_chemical_formula_weight         688.78

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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                   11.7179(6)
_cell_length_b                   15.2415(8)
_cell_length_c                   33.0452(17)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     5901.8(5)
_cell_formula_units_Z            8
_cell_measurement_temperature    295(2)
_cell_measurement_reflns_used    50650
_cell_measurement_theta_min      4.553
_cell_measurement_theta_max      54.989

_exptl_crystal_description       block
_exptl_crystal_colour            brown
_exptl_crystal_size_max          0.53
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.32
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.550
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2840
_exptl_absorpt_coefficient_mu    1.324
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.5405
_exptl_absorpt_correction_T_max  0.6767
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      295(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  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            37751
_diffrn_reflns_av_R_equivalents  0.0666
_diffrn_reflns_av_sigmaI/netI    0.0490
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_theta_min         2.13
_diffrn_reflns_theta_max         25.00
_reflns_number_total             5071
_reflns_number_gt                3595
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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)+(0.0695P)²+40.8597P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5071
_refine_ls_number_parameters     325
_refine_ls_number_restraints     15
_refine_ls_R_factor_all          0.1161
_refine_ls_R_factor_gt           0.0797
_refine_ls_wR_factor_ref         0.1950
_refine_ls_wR_factor_gt          0.1799
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_restrained_S_all      1.025
_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 0.86311(8) 0.05148(6) 0.63691(3) 0.0379(3) Uani 1 1 d . . .
Fe2 Fe 1.07000(9) 0.23932(6) 0.65898(3) 0.0400(3) Uani 1 1 d U . .
S1 S 1.05528(18) 0.10888(14) 0.62955(6) 0.0591(5) Uani 1 1 d U . .
S2 S 0.8158(2) 0.18346(13) 0.67501(7) 0.0623(6) Uani 1 1 d U . .
Cl1 Cl 0.8474(3) -0.05901(14) 0.68131(7) 0.0858(8) Uani 1 1 d . . .
C4 C 1.1281(8) 0.3321(5) 0.7013(2) 0.057(2) Uani 1 1 d . . .
N3 N 1.0881(6) 0.3081(5) 0.61076(18) 0.0566(17) Uani 1 1 d . . .
C6 C 0.9003(7) 0.2645(6) 0.6548(2) 0.063(2) Uani 1 1 d U . .
H6A H 0.8841 0.3192 0.6686 0.076 Uiso 1 1 calc R . .
H6B H 0.8805 0.2721 0.6265 0.076 Uiso 1 1 calc R . .
N2 N 0.8910(6) 0.0041(5) 0.57475(18) 0.0616(18) Uani 1 1 d U . .
C8 C 1.1364(9) 0.1838(5) 0.7126(2) 0.063(2) Uani 1 1 d . . .
C9 C 0.6657(8) 0.1703(7) 0.6122(3) 0.080(3) Uani 1 1 d . . .
H9A H 0.7171 0.2021 0.5945 0.096 Uiso 1 1 calc R . .
H9B H 0.5885 0.1798 0.6025 0.096 Uiso 1 1 calc R . .
C10 C 1.2241(7) 0.2974(5) 0.6813(2) 0.058(2) Uani 1 1 d . . .
N1 N 0.6917(6) 0.0773(5) 0.6100(2) 0.0644(19) Uani 1 1 d . . .
C12 C 1.1080(7) 0.3519(6) 0.5838(2) 0.062(2) Uani 1 1 d . . .
C13 C 0.9784(10) 0.2720(8) 0.7509(3) 0.104(4) Uani 1 1 d . . .
H13A H 1.0092 0.2831 0.7774 0.156 Uiso 1 1 calc R . .
H13B H 0.9337 0.2192 0.7516 0.156 Uiso 1 1 calc R . .
H13C H 0.9309 0.3203 0.7429 0.156 Uiso 1 1 calc R . .
C14 C 1.0720(8) 0.2617(6) 0.7218(2) 0.064(2) Uani 1 1 d . . .
C15 C 1.1349(9) 0.4097(7) 0.5499(3) 0.089(3) Uani 1 1 d . . .
H15A H 1.0744 0.4072 0.5304 0.133 Uiso 1 1 calc R . .
H15B H 1.2050 0.3910 0.5376 0.133 Uiso 1 1 calc R . .
H15C H 1.1430 0.4687 0.5596 0.133 Uiso 1 1 calc R . .
C16 C 0.6755(8) 0.2059(6) 0.6532(4) 0.084(3) Uani 1 1 d . . .
H16A H 0.6171 0.1801 0.6703 0.101 Uiso 1 1 calc R . .
H16B H 0.6631 0.2688 0.6525 0.101 Uiso 1 1 calc R . .
C18 C 1.3119(8) 0.3493(7) 0.6575(3) 0.089(3) Uani 1 1 d . . .
H18A H 1.3716 0.3682 0.6754 0.133 Uiso 1 1 calc R . .
H18B H 1.2760 0.3996 0.6456 0.133 Uiso 1 1 calc R . .
H18C H 1.3436 0.3130 0.6366 0.133 Uiso 1 1 calc R . .
C19 C 1.2298(8) 0.2068(5) 0.6881(3) 0.064(2) Uani 1 1 d . . .
C22 C 1.1129(11) 0.0937(6) 0.7289(3) 0.103(4) Uani 1 1 d . . .
H22A H 1.1537 0.0858 0.7539 0.155 Uiso 1 1 calc R . .
H22B H 1.1374 0.0505 0.7097 0.155 Uiso 1 1 calc R . .
H22C H 1.0326 0.0873 0.7338 0.155 Uiso 1 1 calc R . .
C23 C 1.3189(9) 0.1454(7) 0.6717(4) 0.106(4) Uani 1 1 d . . .
H23A H 1.3811 0.1415 0.6906 0.159 Uiso 1 1 calc R . .
H23B H 1.3465 0.1672 0.6463 0.159 Uiso 1 1 calc R . .
H23C H 1.2861 0.0883 0.6679 0.159 Uiso 1 1 calc R . .
C26 C 1.0946(10) 0.4270(5) 0.7041(3) 0.089(3) Uani 1 1 d . . .
H26A H 1.1343 0.4540 0.7262 0.133 Uiso 1 1 calc R . .
H26B H 1.0138 0.4313 0.7084 0.133 Uiso 1 1 calc R . .
H26C H 1.1144 0.4563 0.6793 0.133 Uiso 1 1 calc R . .
C27 C 0.9993(11) 0.0397(10) 0.5579(3) 0.126(4) Uani 1 1 d U . .
H27A H 1.0575 -0.0052 0.5606 0.151 Uiso 1 1 calc R . .
H27B H 0.9881 0.0497 0.5292 0.151 Uiso 1 1 calc R . .
P1 P 0.3693(2) 0.19934(18) 0.51835(8) 0.0700(7) Uani 1 1 d . . .
F25 F 0.3557(10) 0.2040(10) 0.5632(2) 0.243(6) Uani 1 1 d . . .
F29 F 0.3777(18) 0.1064(6) 0.5159(4) 0.310(10) Uani 1 1 d . . .
F5 F 0.3788(8) 0.1953(7) 0.4719(2) 0.171(4) Uani 1 1 d . . .
C30 C 0.6025(9) 0.0278(7) 0.6317(4) 0.095(3) Uani 1 1 d . . .
H30A H 0.5295 0.0397 0.6197 0.143 Uiso 1 1 calc R . .
H30B H 0.6015 0.0455 0.6596 0.143 Uiso 1 1 calc R . .
H30C H 0.6184 -0.0338 0.6300 0.143 Uiso 1 1 calc R . .
C29 C 0.7979(10) 0.0356(9) 0.5510(3) 0.115(4) Uani 1 1 d DU . .
H29A H 0.8209 0.0916 0.5398 0.138 Uiso 1 1 calc R . .
H29B H 0.7888 -0.0044 0.5284 0.138 Uiso 1 1 calc R . .
F4 F 0.4967(7) 0.2104(9) 0.5216(3) 0.220(6) Uani 1 1 d . . .
C3 C 1.0429(12) 0.1188(9) 0.5753(3) 0.129(6) Uani 1 1 d . . .
H3A H 0.9923 0.1671 0.5687 0.155 Uiso 1 1 calc R . .
H3B H 1.1172 0.1316 0.5638 0.155 Uiso 1 1 calc R . .
C2 C 0.6921(9) 0.0472(10) 0.5678(3) 0.121(5) Uani 1 1 d D . .
H2A H 0.6512 -0.0080 0.5664 0.145 Uiso 1 1 calc R . .
H2B H 0.6505 0.0894 0.5516 0.145 Uiso 1 1 calc R . .
F2 F 0.3713(13) 0.2983(7) 0.5170(4) 0.240(6) Uani 1 1 d . . .
F1 F 0.2464(7) 0.1975(13) 0.5136(3) 0.285(9) Uani 1 1 d . . .
C1 C 0.8955(14) -0.0906(7) 0.5735(4) 0.143(6) Uani 1 1 d . . .
H1A H 0.9081 -0.1095 0.5462 0.214 Uiso 1 1 calc R . .
H1B H 0.8245 -0.1142 0.5832 0.214 Uiso 1 1 calc R . .
H1C H 0.9567 -0.1109 0.5904 0.214 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 N2 2.202(6) . ?
Fe1 N1 2.232(7) . ?
Fe1 Cl1 2.241(2) . ?
Fe1 S1 2.428(2) . ?
Fe1 S2 2.437(2) . ?
Fe2 N3 1.919(6) . ?
Fe2 C6 2.030(8) . ?
Fe2 C4 2.102(7) . ?
Fe2 C8 2.111(7) . ?
Fe2 C14 2.105(7) . ?
Fe2 C10 2.142(8) . ?
Fe2 C19 2.162(8) . ?
Fe2 S1 2.220(2) . ?
S1 C3 1.806(10) . ?
S2 C6 1.718(9) . ?
S2 C16 1.826(10) . ?
C4 C10 1.408(12) . ?
C4 C14 1.430(11) . ?
C4 C26 1.501(11) . ?
N3 C12 1.138(9) . ?
N2 C1 1.444(13) . ?
N2 C29 1.427(12) . ?
N2 C27 1.488(13) . ?
C8 C19 1.405(12) . ?
C8 C14 1.441(12) . ?
C8 C22 1.501(11) . ?
C9 C16 1.465(13) . ?
C9 N1 1.453(11) . ?
C10 C19 1.400(11) . ?
C10 C18 1.516(12) . ?
N1 C2 1.466(11) . ?
N1 C30 1.476(12) . ?
C12 C15 1.457(11) . ?
C13 C14 1.468(13) . ?
C19 C23 1.503(13) . ?
C27 C3 1.430(15) . ?
P1 F29 1.422(10) . ?
P1 F1 1.449(9) . ?
P1 F25 1.492(8) . ?
P1 F4 1.507(9) . ?
P1 F2 1.510(11) . ?
P1 F5 1.540(7) . ?
C29 C2 1.369(9) . ?

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
N2 Fe1 N1 79.6(3) . . ?
N2 Fe1 Cl1 112.1(2) . . ?
N1 Fe1 Cl1 108.6(2) . . ?
N2 Fe1 S1 83.5(2) . . ?
N1 Fe1 S1 137.0(2) . . ?
Cl1 Fe1 S1 114.36(10) . . ?
N2 Fe1 S2 141.9(2) . . ?
N1 Fe1 S2 81.73(19) . . ?
Cl1 Fe1 S2 105.26(9) . . ?
S1 Fe1 S2 88.02(8) . . ?
N3 Fe2 C6 87.1(3) . . ?
N3 Fe2 C4 98.5(3) . . ?
C6 Fe2 C4 103.6(4) . . ?
N3 Fe2 C8 151.0(3) . . ?
C6 Fe2 C8 119.6(4) . . ?
C4 Fe2 C8 66.0(3) . . ?
N3 Fe2 C14 136.8(3) . . ?
C6 Fe2 C14 92.7(3) . . ?
C4 Fe2 C14 39.7(3) . . ?
C8 Fe2 C14 40.0(3) . . ?
N3 Fe2 C10 88.1(3) . . ?
C6 Fe2 C10 140.5(4) . . ?
C4 Fe2 C10 38.7(3) . . ?
C8 Fe2 C10 64.3(3) . . ?
C14 Fe2 C10 65.4(3) . . ?
N3 Fe2 C19 113.5(3) . . ?
C6 Fe2 C19 157.2(4) . . ?
C4 Fe2 C19 65.0(3) . . ?
C8 Fe2 C19 38.4(3) . . ?
C14 Fe2 C19 65.7(4) . . ?
C10 Fe2 C19 38.0(3) . . ?
N3 Fe2 S1 97.7(2) . . ?
C6 Fe2 S1 93.6(3) . . ?
C4 Fe2 S1 156.8(2) . . ?
C8 Fe2 S1 92.1(2) . . ?
C14 Fe2 S1 125.3(2) . . ?
C10 Fe2 S1 125.9(3) . . ?
C19 Fe2 S1 93.3(2) . . ?
C3 S1 Fe2 111.5(4) . . ?
C3 S1 Fe1 93.2(4) . . ?
Fe2 S1 Fe1 110.54(9) . . ?
C6 S2 C16 103.3(4) . . ?
C6 S2 Fe1 105.2(3) . . ?
C16 S2 Fe1 99.0(3) . . ?
C10 C4 C14 108.0(7) . . ?
C10 C4 C26 126.8(8) . . ?
C14 C4 C26 125.0(9) . . ?
C10 C4 Fe2 72.2(4) . . ?
C14 C4 Fe2 70.2(4) . . ?
C26 C4 Fe2 127.2(6) . . ?
C12 N3 Fe2 173.5(7) . . ?
S2 C6 Fe2 113.7(5) . . ?
C1 N2 C29 110.4(9) . . ?
C1 N2 C27 108.8(10) . . ?
C29 N2 C27 108.9(9) . . ?
C1 N2 Fe1 111.1(6) . . ?
C29 N2 Fe1 106.8(6) . . ?
C27 N2 Fe1 110.8(5) . . ?
C19 C8 C14 108.9(7) . . ?
C19 C8 C22 125.4(9) . . ?
C14 C8 C22 125.5(9) . . ?
C19 C8 Fe2 72.8(4) . . ?
C14 C8 Fe2 69.8(4) . . ?
C22 C8 Fe2 127.0(6) . . ?
C16 C9 N1 113.1(8) . . ?
C4 C10 C19 109.4(8) . . ?
C4 C10 C18 126.1(8) . . ?
C19 C10 C18 124.4(9) . . ?
C4 C10 Fe2 69.1(4) . . ?
C19 C10 Fe2 71.8(5) . . ?
C18 C10 Fe2 127.6(6) . . ?
C2 N1 C9 110.8(9) . . ?
C2 N1 C30 107.8(9) . . ?
C9 N1 C30 108.9(7) . . ?
C2 N1 Fe1 108.7(5) . . ?
C9 N1 Fe1 109.9(5) . . ?
C30 N1 Fe1 110.7(6) . . ?
N3 C12 C15 178.6(10) . . ?
C4 C14 C13 125.1(9) . . ?
C4 C14 C8 106.1(8) . . ?
C13 C14 C8 128.2(9) . . ?
C4 C14 Fe2 70.0(4) . . ?
C13 C14 Fe2 131.0(7) . . ?
C8 C14 Fe2 70.2(4) . . ?
C9 C16 S2 111.5(7) . . ?
C8 C19 C10 107.6(8) . . ?
C8 C19 C23 126.3(9) . . ?
C10 C19 C23 126.1(10) . . ?
C8 C19 Fe2 68.8(5) . . ?
C10 C19 Fe2 70.2(5) . . ?
C23 C19 Fe2 125.8(6) . . ?
C3 C27 N2 117.5(9) . . ?
F29 P1 F1 92.6(10) . . ?
F29 P1 F25 96.4(8) . . ?
F1 P1 F25 90.2(6) . . ?
F29 P1 F4 92.7(10) . . ?
F1 P1 F4 174.2(10) . . ?
F25 P1 F4 91.7(6) . . ?
F29 P1 F2 173.1(9) . . ?
F1 P1 F2 91.8(9) . . ?
F25 P1 F2 89.0(8) . . ?
F4 P1 F2 82.8(7) . . ?
F29 P1 F5 84.2(7) . . ?
F1 P1 F5 87.9(5) . . ?
F25 P1 F5 178.0(7) . . ?
F4 P1 F5 90.2(6) . . ?
F2 P1 F5 90.5(7) . . ?
C2 C29 N2 120.9(9) . . ?
C27 C3 S1 110.9(9) . . ?
C29 C2 N1 115.3(8) . . ?

_diffrn_measured_fraction_theta_max 0.977
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.977
_refine_diff_density_max         1.937
_refine_diff_density_min         -0.668
_refine_diff_density_rms         0.108
