# Electronic Supplementary Material (ESI) for Chemical Science.
# This journal is © The Royal Society of Chemistry 2014

#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_cd1089a

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C42 H44 Cl6 Fe N4'
_chemical_formula_sum            'C42 H44 Cl6 Fe N4'
_chemical_formula_weight         873.36

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'
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   'F d d 2'
_symmetry_space_group_name_Hall  'F 2 -2d'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'x+1/4, -y+1/4, z+1/4'
'-x+1/4, y+1/4, z+1/4'
'x, y+1/2, z+1/2'
'-x, -y+1/2, z+1/2'
'x+1/4, -y+3/4, z+3/4'
'-x+1/4, y+3/4, z+3/4'
'x+1/2, y, z+1/2'
'-x+1/2, -y, z+1/2'
'x+3/4, -y+1/4, z+3/4'
'-x+3/4, y+1/4, z+3/4'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z'
'x+3/4, -y+3/4, z+1/4'
'-x+3/4, y+3/4, z+1/4'

_cell_length_a                   19.230(2)
_cell_length_b                   43.035(5)
_cell_length_c                   10.2776(12)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     8505.4(17)
_cell_formula_units_Z            8
_cell_measurement_temperature    98(2)
_cell_measurement_reflns_used    8164
_cell_measurement_theta_min      2.3
_cell_measurement_theta_max      40.2

_exptl_crystal_description       chip
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.364
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3616
_exptl_absorpt_coefficient_mu    0.766
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.681
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   'ABSCOR (Higashi, 1995)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      98(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  
;
Saturn724 (2x2 bin mode)
;
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean 28.5714
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        <1
_diffrn_reflns_number            5942
_diffrn_reflns_av_R_equivalents  0.0336
_diffrn_reflns_av_sigmaI/netI    0.0396
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       54
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_theta_min         2.66
_diffrn_reflns_theta_max         26.50
_diffrn_reflns_reduction_process 'Lp corrections applied'
_reflns_number_total             3408
_reflns_number_gt                3354
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
;
CrystalClear-SM Expert 2.0 r5 (Rigaku, 2010)
;
_computing_cell_refinement       
;
CrystalClear-SM Expert 2.0 r5 (Rigaku, 2010)
;
_computing_data_reduction        
;
CrystalClear-SM Expert 2.0 r5 (Rigaku, 2010)
;

_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)+(0.0583P)²+9.1414P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.039(19)
_chemical_absolute_configuration ad
_refine_ls_number_reflns         3408
_refine_ls_number_parameters     240
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0355
_refine_ls_R_factor_gt           0.0349
_refine_ls_wR_factor_ref         0.0926
_refine_ls_wR_factor_gt          0.0921
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_restrained_S_all      1.018
_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 0.0000 0.0000 0.51957(5) 0.01488(14) Uani 1 2 d S . .
Cl3 Cl 0.25511(4) 0.030595(18) 0.22768(8) 0.02374(18) Uani 1 1 d . . .
Cl1 Cl -0.06277(4) 0.031970(18) 0.65161(7) 0.02347(17) Uani 1 1 d . . .
Cl2 Cl 0.21880(4) 0.091019(18) 0.44596(8) 0.02581(18) Uani 1 1 d . . .
C13 C 0.11991(15) -0.00871(7) 0.2351(3) 0.0164(6) Uani 1 1 d . . .
N1 N 0.10884(12) 0.05196(6) 0.4706(2) 0.0162(5) Uani 1 1 d . . .
N2 N 0.12895(12) 0.01561(6) 0.3312(2) 0.0163(5) Uani 1 1 d . . .
C9 C 0.03264(16) 0.09453(7) 0.5356(3) 0.0226(6) Uani 1 1 d . . .
C17 C 0.13400(15) -0.06099(7) 0.1655(3) 0.0211(6) Uani 1 1 d . . .
H17A H 0.1463 -0.0815 0.1830 0.025 Uiso 1 1 calc R . .
C14 C 0.09574(16) 0.00018(7) 0.1117(3) 0.0200(6) Uani 1 1 d . . .
C5 C 0.10848(15) 0.06959(7) 0.6955(3) 0.0204(6) Uani 1 1 d . . .
C4 C 0.08111(15) 0.07199(7) 0.5701(3) 0.0159(6) Uani 1 1 d . . .
C2 C 0.17177(15) 0.05871(7) 0.4106(3) 0.0187(6) Uani 1 1 d . . .
C18 C 0.14162(15) -0.03890(8) 0.2630(3) 0.0196(6) Uani 1 1 d . . .
C1 C 0.08127(14) 0.02500(7) 0.4218(3) 0.0157(6) Uani 1 1 d . . .
C16 C 0.10837(15) -0.05353(8) 0.0415(3) 0.0213(6) Uani 1 1 d . . .
C15 C 0.09103(15) -0.02239(8) 0.0170(3) 0.0229(6) Uani 1 1 d . . .
H15A H 0.0759 -0.0168 -0.0658 0.027 Uiso 1 1 calc R . .
C19 C 0.07771(18) 0.03373(8) 0.0829(3) 0.0262(7) Uani 1 1 d . . .
H19A H 0.0623 0.0355 -0.0057 0.039 Uiso 1 1 calc R . .
H19B H 0.1181 0.0465 0.0957 0.039 Uiso 1 1 calc R . .
H19C H 0.0413 0.0404 0.1403 0.039 Uiso 1 1 calc R . .
C3 C 0.18476(15) 0.03623(7) 0.3247(3) 0.0187(6) Uani 1 1 d . . .
C20 C 0.09946(17) -0.07785(8) -0.0612(4) 0.0265(7) Uani 1 1 d . . .
H20A H 0.1136 -0.0977 -0.0273 0.040 Uiso 1 1 calc R . .
H20B H 0.1276 -0.0727 -0.1353 0.040 Uiso 1 1 calc R . .
H20C H 0.0515 -0.0788 -0.0868 0.040 Uiso 1 1 calc R . .
C21 C 0.17387(17) -0.04746(8) 0.3913(3) 0.0244(7) Uani 1 1 d . . .
H21A H 0.1757 -0.0294 0.4463 0.037 Uiso 1 1 calc R . .
H21B H 0.2201 -0.0551 0.3771 0.037 Uiso 1 1 calc R . .
H21C H 0.1464 -0.0633 0.4325 0.037 Uiso 1 1 calc R . .
C10 C 0.15865(17) 0.04411(9) 0.7295(3) 0.0277(7) Uani 1 1 d . . .
H10A H 0.1666 0.0313 0.6544 0.042 Uiso 1 1 calc R . .
H10B H 0.1396 0.0317 0.7983 0.042 Uiso 1 1 calc R . .
H10C H 0.2019 0.0530 0.7576 0.042 Uiso 1 1 calc R . .
C6 C 0.08738(18) 0.09143(8) 0.7864(3) 0.0269(7) Uani 1 1 d . . .
H6A H 0.1050 0.0903 0.8706 0.032 Uiso 1 1 calc R . .
C8 C 0.01316(18) 0.11590(8) 0.6306(4) 0.0292(8) Uani 1 1 d . . .
H8A H -0.0191 0.1312 0.6100 0.035 Uiso 1 1 calc R . .
C7 C 0.0408(2) 0.11492(8) 0.7555(4) 0.0327(8) Uani 1 1 d . . .
C12 C 0.00314(18) 0.09577(9) 0.4003(4) 0.0322(8) Uani 1 1 d . . .
H12A H -0.0290 0.1128 0.3939 0.048 Uiso 1 1 calc R . .
H12B H -0.0206 0.0767 0.3817 0.048 Uiso 1 1 calc R . .
H12C H 0.0402 0.0987 0.3388 0.048 Uiso 1 1 calc R . .
C11 C 0.0223(3) 0.13925(9) 0.8568(4) 0.0493(12) Uani 1 1 d . . .
H11A H 0.0459 0.1346 0.9368 0.074 Uiso 1 1 calc R . .
H11B H -0.0270 0.1391 0.8714 0.074 Uiso 1 1 calc R . .
H11C H 0.0362 0.1594 0.8264 0.074 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 2.147(3) 2 ?
Fe1 C1 2.147(3) . ?
Fe1 Cl1 2.2785(8) . ?
Fe1 Cl1 2.2785(8) 2 ?
Cl3 C3 1.698(3) . ?
Cl2 C2 1.698(3) . ?
C13 C18 1.394(4) . ?
C13 C14 1.405(4) . ?
C13 N2 1.450(4) . ?
N1 C1 1.371(4) . ?
N1 C2 1.389(4) . ?
N1 C4 1.439(4) . ?
N2 C1 1.368(4) . ?
N2 C3 1.394(4) . ?
C9 C4 1.391(4) . ?
C9 C8 1.393(5) . ?
C9 C12 1.503(5) . ?
C17 C18 1.389(5) . ?
C17 C16 1.404(4) . ?
C17 H17A 0.9300 . ?
C14 C15 1.378(5) . ?
C14 C19 1.514(4) . ?
C5 C6 1.386(5) . ?
C5 C4 1.396(4) . ?
C5 C10 1.502(5) . ?
C2 C3 1.334(4) . ?
C18 C21 1.503(4) . ?
C16 C15 1.404(5) . ?
C16 C20 1.496(4) . ?
C15 H15A 0.9300 . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
C21 H21A 0.9600 . ?
C21 H21B 0.9600 . ?
C21 H21C 0.9600 . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C6 C7 1.388(6) . ?
C6 H6A 0.9300 . ?
C8 C7 1.390(6) . ?
C8 H8A 0.9300 . ?
C7 C11 1.519(5) . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 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
C1 Fe1 C1 124.20(15) 2 . ?
C1 Fe1 Cl1 101.28(8) 2 . ?
C1 Fe1 Cl1 111.21(8) . . ?
C1 Fe1 Cl1 111.21(8) 2 2 ?
C1 Fe1 Cl1 101.28(8) . 2 ?
Cl1 Fe1 Cl1 106.89(5) . 2 ?
C18 C13 C14 122.6(3) . . ?
C18 C13 N2 119.8(3) . . ?
C14 C13 N2 117.3(3) . . ?
C1 N1 C2 110.6(2) . . ?
C1 N1 C4 128.6(2) . . ?
C2 N1 C4 120.8(2) . . ?
C1 N2 C3 111.1(2) . . ?
C1 N2 C13 126.7(2) . . ?
C3 N2 C13 121.3(2) . . ?
C4 C9 C8 117.5(3) . . ?
C4 C9 C12 120.9(3) . . ?
C8 C9 C12 121.6(3) . . ?
C18 C17 C16 122.4(3) . . ?
C18 C17 H17A 118.8 . . ?
C16 C17 H17A 118.8 . . ?
C15 C14 C13 117.9(3) . . ?
C15 C14 C19 121.3(3) . . ?
C13 C14 C19 120.8(3) . . ?
C6 C5 C4 117.5(3) . . ?
C6 C5 C10 121.7(3) . . ?
C4 C5 C10 120.7(3) . . ?
C9 C4 C5 122.6(3) . . ?
C9 C4 N1 119.0(3) . . ?
C5 C4 N1 118.1(3) . . ?
C3 C2 N1 107.8(2) . . ?
C3 C2 Cl2 129.5(2) . . ?
N1 C2 Cl2 122.7(2) . . ?
C17 C18 C13 117.3(3) . . ?
C17 C18 C21 120.6(3) . . ?
C13 C18 C21 122.1(3) . . ?
N2 C1 N1 103.9(2) . . ?
N2 C1 Fe1 131.2(2) . . ?
N1 C1 Fe1 122.3(2) . . ?
C17 C16 C15 117.7(3) . . ?
C17 C16 C20 121.4(3) . . ?
C15 C16 C20 121.0(3) . . ?
C14 C15 C16 122.1(3) . . ?
C14 C15 H15A 119.0 . . ?
C16 C15 H15A 119.0 . . ?
C14 C19 H19A 109.5 . . ?
C14 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C14 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C2 C3 N2 106.6(2) . . ?
C2 C3 Cl3 129.9(2) . . ?
N2 C3 Cl3 123.4(2) . . ?
C16 C20 H20A 109.5 . . ?
C16 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C16 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C18 C21 H21A 109.5 . . ?
C18 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C18 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C5 C10 H10A 109.5 . . ?
C5 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C5 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C5 C6 C7 121.9(3) . . ?
C5 C6 H6A 119.0 . . ?
C7 C6 H6A 119.0 . . ?
C7 C8 C9 121.7(3) . . ?
C7 C8 H8A 119.2 . . ?
C9 C8 H8A 119.2 . . ?
C6 C7 C8 118.7(3) . . ?
C6 C7 C11 119.8(4) . . ?
C8 C7 C11 121.5(4) . . ?
C9 C12 H12A 109.5 . . ?
C9 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C9 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C7 C11 H11A 109.5 . . ?
C7 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C7 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.991
_diffrn_reflns_theta_full        26.50
_diffrn_measured_fraction_theta_full 0.991
_refine_diff_density_max         0.424
_refine_diff_density_min         -0.419
_refine_diff_density_rms         0.064
_database_code_depnum_ccdc_archive 'CCDC 1023546'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_cd0980a

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C35 H54 Fe N2 Si2'
_chemical_formula_sum            'C35 H54 Fe N2 Si2'
_chemical_formula_weight         614.83

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'
Si Si 0.0817 0.0704 '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   C2/c
_symmetry_space_group_name_Hall  '-C 2yc'

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

_cell_length_a                   10.777(6)
_cell_length_b                   19.521(11)
_cell_length_c                   18.542(12)
_cell_angle_alpha                90.00
_cell_angle_beta                 103.339(12)
_cell_angle_gamma                90.00
_cell_volume                     3796(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    98(2)
_cell_measurement_reflns_used    9267
_cell_measurement_theta_min      2.1
_cell_measurement_theta_max      40.3

_exptl_crystal_description       chunk
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.076
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1328
_exptl_absorpt_coefficient_mu    0.483
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.827
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   'ABSCOR (Higashi, 1995)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      98(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  
;
Saturn724 (2x2 bin mode)
;
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean 28.5714
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        <1
_diffrn_reflns_number            14159
_diffrn_reflns_av_R_equivalents  0.0355
_diffrn_reflns_av_sigmaI/netI    0.0299
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         2.09
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_reduction_process 'Lp corrections applied'
_reflns_number_total             4360
_reflns_number_gt                4067
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
;
CrystalClear-SM Expert 2.0 r5 (Rigaku, 2010)
;
_computing_cell_refinement       
;
CrystalClear-SM Expert 2.0 r5 (Rigaku, 2010)
;
_computing_data_reduction        
;
CrystalClear-SM Expert 2.0 r5 (Rigaku, 2010)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  'publCIF (Westrip, 2010)'

_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)+(0.0750P)²+4.5000P] 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         4360
_refine_ls_number_parameters     203
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0485
_refine_ls_R_factor_gt           0.0462
_refine_ls_wR_factor_ref         0.1287
_refine_ls_wR_factor_gt          0.1261
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_restrained_S_all      1.017
_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 0.5000 0.020143(16) 0.7500 0.01936(12) Uani 1 2 d S . .
Si1 Si 0.25821(5) -0.08772(3) 0.67731(3) 0.02893(15) Uani 1 1 d . . .
N1 N 0.45514(14) 0.17427(7) 0.69245(8) 0.0206(3) Uani 1 1 d . . .
C1 C 0.5000 0.13100(12) 0.7500 0.0182(4) Uani 1 2 d S . .
C3 C 0.39479(16) 0.15217(9) 0.61791(9) 0.0221(3) Uani 1 1 d . . .
C4 C 0.26137(17) 0.15128(10) 0.59818(10) 0.0276(4) Uani 1 1 d . A .
C8 C 0.47188(17) 0.13269(9) 0.56991(10) 0.0251(4) Uani 1 1 d . . .
C2 C 0.47176(19) 0.24259(9) 0.71357(10) 0.0269(4) Uani 1 1 d . . .
C12 C 0.61651(18) 0.13719(10) 0.59087(11) 0.0288(4) Uani 1 1 d . . .
H12A H 0.6423 0.1514 0.6429 0.035 Uiso 1 1 calc R . .
C5 C 0.2050(2) 0.12744(12) 0.52716(11) 0.0377(5) Uani 1 1 d . . .
H5A H 0.1166 0.1256 0.5120 0.045 Uiso 1 1 calc R . .
C15 C 0.3858(2) -0.03016(11) 0.66134(11) 0.0338(5) Uani 1 1 d . . .
H15A H 0.3982 -0.0240 0.6138 0.041 Uiso 1 1 calc R . .
C9 C 0.18024(19) 0.17385(12) 0.65129(12) 0.0373(5) Uani 1 1 d . . .
C7 C 0.4099(2) 0.10943(11) 0.49944(11) 0.0339(4) Uani 1 1 d . . .
H7A H 0.4577 0.0958 0.4661 0.041 Uiso 1 1 calc R . .
C6 C 0.2782(2) 0.10644(13) 0.47876(11) 0.0405(5) Uani 1 1 d . . .
H6A H 0.2385 0.0902 0.4320 0.049 Uiso 1 1 calc R . .
C13 C 0.6775(2) 0.06755(12) 0.58336(15) 0.0428(5) Uani 1 1 d . . .
H13A H 0.6468 0.0344 0.6134 0.064 Uiso 1 1 calc R . .
H13B H 0.7685 0.0713 0.5996 0.064 Uiso 1 1 calc R . .
H13C H 0.6554 0.0533 0.5325 0.064 Uiso 1 1 calc R . .
C17 C 0.1168(2) -0.08902(14) 0.59684(13) 0.0433(5) Uani 1 1 d . . .
H17A H 0.0824 -0.0436 0.5882 0.065 Uiso 1 1 calc R . .
H17B H 0.0530 -0.1192 0.6076 0.065 Uiso 1 1 calc R . .
H17C H 0.1424 -0.1049 0.5535 0.065 Uiso 1 1 calc R . .
C14 C 0.6647(2) 0.19114(12) 0.54378(14) 0.0428(5) Uani 1 1 d . . .
H14A H 0.6266 0.2346 0.5496 0.064 Uiso 1 1 calc R . .
H14B H 0.6419 0.1778 0.4926 0.064 Uiso 1 1 calc R . .
H14C H 0.7558 0.1948 0.5596 0.064 Uiso 1 1 calc R . .
C16 C 0.1980(3) -0.06796(17) 0.76204(14) 0.0572(7) Uani 1 1 d . . .
H16A H 0.1659 -0.0219 0.7590 0.086 Uiso 1 1 calc R . .
H16B H 0.2665 -0.0725 0.8053 0.086 Uiso 1 1 calc R . .
H16C H 0.1309 -0.0993 0.7653 0.086 Uiso 1 1 calc R . .
C18 C 0.3178(2) -0.17884(14) 0.69025(18) 0.0553(7) Uani 1 1 d . . .
H18A H 0.3500 -0.1924 0.6483 0.083 Uiso 1 1 calc R . .
H18B H 0.2490 -0.2086 0.6947 0.083 Uiso 1 1 calc R . .
H18C H 0.3848 -0.1819 0.7344 0.083 Uiso 1 1 calc R . .
C11A C 0.1315(9) 0.2500(5) 0.6198(5) 0.049(2) Uani 0.30 1 d P A 1
H11A H 0.2037 0.2797 0.6237 0.073 Uiso 0.30 1 calc PR A 1
H11B H 0.0755 0.2684 0.6485 0.073 Uiso 0.30 1 calc PR A 1
H11C H 0.0866 0.2464 0.5688 0.073 Uiso 0.30 1 calc PR A 1
C10A C 0.0667(8) 0.1216(7) 0.6466(5) 0.074(4) Uani 0.30 1 d P A 1
H10A H 0.1001 0.0778 0.6654 0.112 Uiso 0.30 1 calc PR A 1
H10B H 0.0210 0.1167 0.5959 0.112 Uiso 0.30 1 calc PR A 1
H10C H 0.0100 0.1383 0.6756 0.112 Uiso 0.30 1 calc PR A 1
C11B C 0.0664(4) 0.2156(3) 0.6174(2) 0.0605(11) Uani 0.70 1 d P A 2
H11D H -0.0088 0.1878 0.6110 0.091 Uiso 0.70 1 calc PR A 2
H11E H 0.0746 0.2324 0.5701 0.091 Uiso 0.70 1 calc PR A 2
H11F H 0.0600 0.2536 0.6492 0.091 Uiso 0.70 1 calc PR A 2
C10B C 0.1491(4) 0.1114(2) 0.6945(3) 0.0637(11) Uani 0.70 1 d P A 2
H10D H 0.2139 0.0772 0.6971 0.096 Uiso 0.70 1 calc PR A 2
H10E H 0.0679 0.0929 0.6697 0.096 Uiso 0.70 1 calc PR A 2
H10F H 0.1460 0.1252 0.7438 0.096 Uiso 0.70 1 calc PR A 2
H2A H 0.446(3) 0.2804(18) 0.677(2) 0.076 Uiso 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 C15 2.061(2) . ?
Fe1 C15 2.061(2) 2_656 ?
Fe1 C1 2.164(3) . ?
Si1 C15 1.851(2) . ?
Si1 C17 1.871(2) . ?
Si1 C16 1.873(3) . ?
Si1 C18 1.888(3) . ?
N1 C1 1.359(2) . ?
N1 C2 1.390(2) . ?
N1 C3 1.451(2) . ?
C1 N1 1.359(2) 2_656 ?
C3 C4 1.400(3) . ?
C3 C8 1.403(3) . ?
C4 C5 1.397(3) . ?
C4 C9 1.525(3) . ?
C8 C7 1.399(3) . ?
C8 C12 1.519(3) . ?
C2 C2 1.348(4) 2_656 ?
C2 H2A 0.99(4) . ?
C12 C13 1.530(3) . ?
C12 C14 1.533(3) . ?
C12 H12A 0.9800 . ?
C5 C6 1.387(3) . ?
C5 H5A 0.9300 . ?
C15 H15A 0.9300 . ?
C9 C11B 1.486(4) . ?
C9 C10B 1.538(5) . ?
C9 C10A 1.580(10) . ?
C9 C11A 1.638(10) . ?
C7 C6 1.383(3) . ?
C7 H7A 0.9300 . ?
C6 H6A 0.9300 . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C11A H11A 0.9600 . ?
C11A H11B 0.9600 . ?
C11A H11C 0.9600 . ?
C10A H10A 0.9600 . ?
C10A H10B 0.9600 . ?
C10A H10C 0.9600 . ?
C11B H11D 0.9600 . ?
C11B H11E 0.9600 . ?
C11B H11F 0.9600 . ?
C10B H10D 0.9600 . ?
C10B H10E 0.9600 . ?
C10B H10F 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
C15 Fe1 C15 123.09(13) . 2_656 ?
C15 Fe1 C1 118.45(6) . . ?
C15 Fe1 C1 118.45(6) 2_656 . ?
C15 Si1 C17 112.27(11) . . ?
C15 Si1 C16 115.02(11) . . ?
C17 Si1 C16 107.20(13) . . ?
C15 Si1 C18 110.40(12) . . ?
C17 Si1 C18 106.22(13) . . ?
C16 Si1 C18 105.13(15) . . ?
C1 N1 C2 112.07(15) . . ?
C1 N1 C3 124.27(14) . . ?
C2 N1 C3 123.65(14) . . ?
N1 C1 N1 103.2(2) 2_656 . ?
N1 C1 Fe1 128.42(10) 2_656 . ?
N1 C1 Fe1 128.42(10) . . ?
C4 C3 C8 123.64(16) . . ?
C4 C3 N1 117.41(15) . . ?
C8 C3 N1 118.95(16) . . ?
C5 C4 C3 116.60(17) . . ?
C5 C4 C9 121.04(18) . . ?
C3 C4 C9 122.35(17) . . ?
C7 C8 C3 117.08(17) . . ?
C7 C8 C12 119.90(17) . . ?
C3 C8 C12 123.01(16) . . ?
C2 C2 N1 106.35(10) 2_656 . ?
C2 C2 H2A 132(2) 2_656 . ?
N1 C2 H2A 122(2) . . ?
C8 C12 C13 111.23(17) . . ?
C8 C12 C14 110.87(16) . . ?
C13 C12 C14 110.45(18) . . ?
C8 C12 H12A 108.1 . . ?
C13 C12 H12A 108.1 . . ?
C14 C12 H12A 108.1 . . ?
C6 C5 C4 121.33(19) . . ?
C6 C5 H5A 119.3 . . ?
C4 C5 H5A 119.3 . . ?
Si1 C15 Fe1 119.37(11) . . ?
Si1 C15 H15A 120.3 . . ?
Fe1 C15 H15A 120.3 . . ?
C11B C9 C4 115.2(2) . . ?
C11B C9 C10B 113.4(3) . . ?
C4 C9 C10B 109.5(2) . . ?
C11B C9 C10A 77.2(6) . . ?
C4 C9 C10A 109.2(4) . . ?
C4 C9 C11A 102.5(3) . . ?
C10B C9 C11A 144.5(4) . . ?
C10A C9 C11A 112.7(6) . . ?
C6 C7 C8 120.74(19) . . ?
C6 C7 H7A 119.6 . . ?
C8 C7 H7A 119.6 . . ?
C7 C6 C5 120.58(19) . . ?
C7 C6 H6A 119.7 . . ?
C5 C6 H6A 119.7 . . ?
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 . . ?
Si1 C17 H17A 109.5 . . ?
Si1 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
Si1 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C12 C14 H14A 109.5 . . ?
C12 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C12 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
Si1 C16 H16A 109.5 . . ?
Si1 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
Si1 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
Si1 C18 H18A 109.5 . . ?
Si1 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
Si1 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C9 C11A H11A 109.5 . . ?
C9 C11A H11B 109.5 . . ?
H11A C11A H11B 109.5 . . ?
C9 C11A H11C 109.5 . . ?
H11A C11A H11C 109.5 . . ?
H11B C11A H11C 109.5 . . ?
C9 C10A H10A 109.5 . . ?
C9 C10A H10B 109.5 . . ?
H10A C10A H10B 109.5 . . ?
C9 C10A H10C 109.5 . . ?
H10A C10A H10C 109.5 . . ?
H10B C10A H10C 109.5 . . ?
C9 C11B H11D 109.5 . . ?
C9 C11B H11E 109.5 . . ?
H11D C11B H11E 109.5 . . ?
C9 C11B H11F 109.5 . . ?
H11D C11B H11F 109.5 . . ?
H11E C11B H11F 109.5 . . ?
C9 C10B H10D 109.5 . . ?
C9 C10B H10E 109.5 . . ?
H10D C10B H10E 109.5 . . ?
C9 C10B H10F 109.5 . . ?
H10D C10B H10F 109.5 . . ?
H10E C10B H10F 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        27.50
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.708
_refine_diff_density_min         -0.468
_refine_diff_density_rms         0.065
_database_code_depnum_ccdc_archive 'CCDC 1023547'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_neikm03

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            neikm03
_chemical_melting_point          ?
_chemical_formula_moiety         'C6 H18 Cl2 Fe P2'
_chemical_formula_sum            'C6 H18 Cl2 Fe P2'
_chemical_formula_weight         278.89

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'
P P 0.1023 0.0942 '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'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_shelx_space_group_comment       
; 
The symmetry employed for this shelxl refinement is uniquely defined 
by the following loop, which should always be used as a source of 
symmetry information in preference to the above space-group names. 
They are only intended as comments. 
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   7.6475(8)
_cell_length_b                   12.4439(12)
_cell_length_c                   15.3186(15)
_cell_angle_alpha                102.743(2)
_cell_angle_beta                 95.406(2)
_cell_angle_gamma                101.351(2)
_cell_volume                     1379.6(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    223(2)
_cell_measurement_reflns_used    3704
_cell_measurement_theta_min      2.74
_cell_measurement_theta_max      37.56

_exptl_crystal_description       block
_exptl_crystal_colour            'pale green'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.343
_exptl_crystal_F_000             576
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_exptl_absorpt_coefficient_mu    1.666
_shelx_estimated_absorpt_T_min   0.555
_shelx_estimated_absorpt_T_max   0.732
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5863
_exptl_absorpt_correction_T_max  0.7476
_exptl_absorpt_process_details   'TWINABS (Sheldrick, 2012)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      223(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker SMART APEX II CCD platform'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            84868
_diffrn_reflns_av_unetI/netI     0.0265
_diffrn_reflns_av_R_equivalents  0.0339
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         1.377
_diffrn_reflns_theta_max         38.737
_diffrn_reflns_theta_full        37.785
_diffrn_measured_fraction_theta_max 0.944
_diffrn_measured_fraction_theta_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.944
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.944
_diffrn_reflns_point_group_measured_fraction_full 0.984
_reflns_number_total             14854
_reflns_number_gt                10782
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
; 
 _reflns_Friedel_fraction is defined as the number of unique 
 Friedel pairs measured divided by the number that would be 
 possible theoretically, ignoring centric projections and 
 systematic absences. 
;

_computing_data_collection       'APEX2 (Bruker, 2013)'
_computing_cell_refinement       'SAINT (Bruker, 2013)'
_computing_data_reduction        'SAINT (Bruker, 2013)'
_computing_structure_solution    'SIR2011 (Burla et al., 2012)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'

_refine_special_details          
; 
 Refined as a 2-component twin. The refinement stalled at R1 = 0.064, at
 which point twin modeling was required. After the non-merohedral twin law,
 [ -0.004 -0.013 -0.502 / 0 -1 0 / -1.993 0.025 0.004 ], a 180 degree
 rotation about reciprocal lattice [ -1 0 2 ], was determined, the data
 were re-integrated, and a new absorption correction was applied. There
 were 10792 unique reflections solely in the first component, 10783 unique
 reflections solely in the second component, and 5682 unique overlapping
 reflections. The mass ratio of the two components refined to 68:32.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0323P)²+0.2552P] 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         14854
_refine_ls_number_parameters     212
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0563
_refine_ls_R_factor_gt           0.0338
_refine_ls_wR_factor_ref         0.0870
_refine_ls_wR_factor_gt          0.0767
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_restrained_S_all      1.020
_refine_ls_shift/su_max          0.002
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.11566(3) 0.74338(2) 0.43305(2) 0.02749(4) Uani 1 1 d . . . . .
Cl1 Cl 0.20800(6) 0.90567(3) 0.39366(3) 0.04362(9) Uani 1 1 d . . . . .
Cl2 Cl 0.20025(6) 0.58414(4) 0.37240(4) 0.04947(10) Uani 1 1 d . . . . .
P1 P 0.19270(6) 0.79596(3) 0.59645(3) 0.03061(7) Uani 1 1 d . . . . .
C1 C 0.4189(2) 0.87899(18) 0.63923(14) 0.0605(5) Uani 1 1 d . . . . .
H1A H 0.4339 0.9012 0.7048 0.091 Uiso 1 1 calc R U . . .
H1B H 0.4388 0.9460 0.6157 0.091 Uiso 1 1 calc R U . . .
H1C H 0.5053 0.8343 0.6201 0.091 Uiso 1 1 calc R U . . .
C2 C 0.1787(3) 0.68029(15) 0.65073(12) 0.0558(5) Uani 1 1 d . . . . .
H2A H 0.2067 0.7100 0.7158 0.084 Uiso 1 1 calc R U . . .
H2B H 0.2642 0.6357 0.6299 0.084 Uiso 1 1 calc R U . . .
H2C H 0.0577 0.6330 0.6357 0.084 Uiso 1 1 calc R U . . .
C3 C 0.0552(3) 0.88333(16) 0.65445(12) 0.0515(4) Uani 1 1 d . . . . .
H3A H 0.1000 0.9062 0.7187 0.077 Uiso 1 1 calc R U . . .
H3B H -0.0686 0.8407 0.6449 0.077 Uiso 1 1 calc R U . . .
H3C H 0.0604 0.9499 0.6308 0.077 Uiso 1 1 calc R U . . .
P2 P -0.21184(5) 0.69769(3) 0.41173(3) 0.02860(7) Uani 1 1 d . . . . .
C4 C -0.3196(2) 0.62865(17) 0.49185(12) 0.0516(4) Uani 1 1 d . . . . .
H4A H -0.4492 0.6092 0.4739 0.077 Uiso 1 1 calc R U . . .
H4B H -0.2903 0.6794 0.5517 0.077 Uiso 1 1 calc R U . . .
H4C H -0.2768 0.5604 0.4926 0.077 Uiso 1 1 calc R U . . .
C5 C -0.3102(2) 0.81904(14) 0.41547(14) 0.0520(4) Uani 1 1 d . . . . .
H5A H -0.4405 0.7948 0.4063 0.078 Uiso 1 1 calc R U . . .
H5B H -0.2726 0.8551 0.3682 0.078 Uiso 1 1 calc R U . . .
H5C H -0.2702 0.8723 0.4739 0.078 Uiso 1 1 calc R U . . .
C6 C -0.3166(2) 0.60363(16) 0.30354(11) 0.0510(4) Uani 1 1 d . . . . .
H6A H -0.4464 0.5867 0.3017 0.077 Uiso 1 1 calc R U . . .
H6B H -0.2742 0.5341 0.2956 0.077 Uiso 1 1 calc R U . . .
H6C H -0.2852 0.6398 0.2554 0.077 Uiso 1 1 calc R U . . .
Fe2 Fe 0.14495(3) 0.75282(2) 0.93651(2) 0.03110(4) Uani 1 1 d . . . . .
Cl3 Cl 0.26415(7) 0.90869(4) 0.89324(3) 0.05167(11) Uani 1 1 d . . . . .
Cl4 Cl 0.22878(6) 0.58901(4) 0.89445(3) 0.05040(11) Uani 1 1 d . . . . .
P3 P 0.18571(6) 0.80440(3) 1.10109(3) 0.03426(8) Uani 1 1 d . . . . .
C7 C 0.4014(3) 0.7970(2) 1.15705(13) 0.0637(5) Uani 1 1 d . . . . .
H7A H 0.4023 0.8160 1.2220 0.096 Uiso 1 1 calc R U . . .
H7B H 0.4970 0.8501 1.1414 0.096 Uiso 1 1 calc R U . . .
H7C H 0.4203 0.7211 1.1377 0.096 Uiso 1 1 calc R U . . .
C8 C 0.0271(3) 0.72134(18) 1.15464(12) 0.0606(5) Uani 1 1 d . . . . .
H8A H 0.0616 0.7449 1.2197 0.091 Uiso 1 1 calc R U . . .
H8B H 0.0275 0.6420 1.1336 0.091 Uiso 1 1 calc R U . . .
H8C H -0.0928 0.7326 1.1392 0.091 Uiso 1 1 calc R U . . .
C9 C 0.1746(3) 0.94894(15) 1.14832(12) 0.0575(5) Uani 1 1 d . . . . .
H9A H 0.1858 0.9631 1.2137 0.086 Uiso 1 1 calc R U . . .
H9B H 0.0600 0.9615 1.1249 0.086 Uiso 1 1 calc R U . . .
H9C H 0.2721 0.9997 1.1317 0.086 Uiso 1 1 calc R U . . .
P4 P -0.18141(6) 0.70330(3) 0.89888(3) 0.03462(8) Uani 1 1 d . . . . .
C10 C -0.2744(3) 0.55931(15) 0.90176(15) 0.0573(5) Uani 1 1 d . . . . .
H10A H -0.4048 0.5439 0.8894 0.086 Uiso 1 1 calc R U . . .
H10B H -0.2383 0.5485 0.9611 0.086 Uiso 1 1 calc R U . . .
H10C H -0.2299 0.5081 0.8563 0.086 Uiso 1 1 calc R U . . .
C11 C -0.3045(2) 0.78726(17) 0.97124(13) 0.0543(4) Uani 1 1 d . . . . .
H11A H -0.4318 0.7647 0.9472 0.081 Uiso 1 1 calc R U . . .
H11B H -0.2605 0.8666 0.9736 0.081 Uiso 1 1 calc R U . . .
H11C H -0.2873 0.7755 1.0317 0.081 Uiso 1 1 calc R U . . .
C12 C -0.2753(3) 0.70670(18) 0.78617(13) 0.0588(5) Uani 1 1 d . . . . .
H12A H -0.4058 0.6854 0.7793 0.088 Uiso 1 1 calc R U . . .
H12B H -0.2319 0.6540 0.7414 0.088 Uiso 1 1 calc R U . . .
H12C H -0.2382 0.7824 0.7777 0.088 Uiso 1 1 calc R U . . .


_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 Cl1 2.2355(5) . ?
Fe1 Cl2 2.2392(5) . ?
Fe1 P1 2.4267(5) . ?
Fe1 P2 2.4302(5) . ?
P1 C2 1.8051(17) . ?
P1 C1 1.8093(18) . ?
P1 C3 1.8106(17) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C1 H1C 0.9700 . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C2 H2C 0.9700 . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C3 H3C 0.9700 . ?
P2 C5 1.8073(16) . ?
P2 C6 1.8120(16) . ?
P2 C4 1.8167(16) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C4 H4C 0.9700 . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C5 H5C 0.9700 . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C6 H6C 0.9700 . ?
Fe2 Cl4 2.2348(5) . ?
Fe2 Cl3 2.2399(5) . ?
Fe2 P4 2.4306(5) . ?
Fe2 P3 2.4341(5) . ?
P3 C9 1.8063(18) . ?
P3 C8 1.8113(19) . ?
P3 C7 1.815(2) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C7 H7C 0.9700 . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C8 H8C 0.9700 . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C9 H9C 0.9700 . ?
P4 C10 1.8049(18) . ?
P4 C11 1.8111(17) . ?
P4 C12 1.8190(19) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C10 H10C 0.9700 . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C11 H11C 0.9700 . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C12 H12C 0.9700 . ?

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
Cl1 Fe1 Cl2 122.879(18) . . ?
Cl1 Fe1 P1 103.419(17) . . ?
Cl2 Fe1 P1 111.223(19) . . ?
Cl1 Fe1 P2 108.195(17) . . ?
Cl2 Fe1 P2 106.584(18) . . ?
P1 Fe1 P2 102.802(13) . . ?
C2 P1 C1 102.84(10) . . ?
C2 P1 C3 104.43(9) . . ?
C1 P1 C3 102.51(10) . . ?
C2 P1 Fe1 115.86(6) . . ?
C1 P1 Fe1 115.41(7) . . ?
C3 P1 Fe1 114.11(6) . . ?
P1 C1 H1A 109.5 . . ?
P1 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
P1 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
P1 C2 H2A 109.5 . . ?
P1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
P1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 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 . . ?
C5 P2 C6 103.08(9) . . ?
C5 P2 C4 104.03(9) . . ?
C6 P2 C4 102.76(9) . . ?
C5 P2 Fe1 113.80(6) . . ?
C6 P2 Fe1 114.67(6) . . ?
C4 P2 Fe1 116.82(6) . . ?
P2 C4 H4A 109.5 . . ?
P2 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
P2 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
P2 C5 H5A 109.5 . . ?
P2 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
P2 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 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 . . ?
Cl4 Fe2 Cl3 123.30(2) . . ?
Cl4 Fe2 P4 104.494(18) . . ?
Cl3 Fe2 P4 111.27(2) . . ?
Cl4 Fe2 P3 107.076(19) . . ?
Cl3 Fe2 P3 106.605(18) . . ?
P4 Fe2 P3 102.095(14) . . ?
C9 P3 C8 104.55(11) . . ?
C9 P3 C7 102.35(11) . . ?
C8 P3 C7 102.43(11) . . ?
C9 P3 Fe2 113.43(6) . . ?
C8 P3 Fe2 116.48(6) . . ?
C7 P3 Fe2 115.86(7) . . ?
P3 C7 H7A 109.5 . . ?
P3 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
P3 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
P3 C8 H8A 109.5 . . ?
P3 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
P3 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
P3 C9 H9A 109.5 . . ?
P3 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
P3 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C10 P4 C11 104.77(10) . . ?
C10 P4 C12 102.04(10) . . ?
C11 P4 C12 102.78(10) . . ?
C10 P4 Fe2 111.90(6) . . ?
C11 P4 Fe2 116.43(6) . . ?
C12 P4 Fe2 117.19(7) . . ?
P4 C10 H10A 109.5 . . ?
P4 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
P4 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
P4 C11 H11A 109.5 . . ?
P4 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
P4 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
P4 C12 H12A 109.5 . . ?
P4 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
P4 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Cl1 Fe1 P1 C2 -168.10(8) . . . . ?
Cl2 Fe1 P1 C2 -34.36(9) . . . . ?
P2 Fe1 P1 C2 79.35(8) . . . . ?
Cl1 Fe1 P1 C1 -47.85(9) . . . . ?
Cl2 Fe1 P1 C1 85.89(9) . . . . ?
P2 Fe1 P1 C1 -160.40(9) . . . . ?
Cl1 Fe1 P1 C3 70.53(8) . . . . ?
Cl2 Fe1 P1 C3 -155.73(8) . . . . ?
P2 Fe1 P1 C3 -42.01(8) . . . . ?
Cl1 Fe1 P2 C5 -23.88(8) . . . . ?
Cl2 Fe1 P2 C5 -157.83(8) . . . . ?
P1 Fe1 P2 C5 85.10(8) . . . . ?
Cl1 Fe1 P2 C6 94.48(8) . . . . ?
Cl2 Fe1 P2 C6 -39.48(8) . . . . ?
P1 Fe1 P2 C6 -156.54(7) . . . . ?
Cl1 Fe1 P2 C4 -145.21(8) . . . . ?
Cl2 Fe1 P2 C4 80.83(8) . . . . ?
P1 Fe1 P2 C4 -36.23(8) . . . . ?
Cl4 Fe2 P3 C9 166.60(9) . . . . ?
Cl3 Fe2 P3 C9 32.90(9) . . . . ?
P4 Fe2 P3 C9 -83.91(9) . . . . ?
Cl4 Fe2 P3 C8 -71.95(9) . . . . ?
Cl3 Fe2 P3 C8 154.35(9) . . . . ?
P4 Fe2 P3 C8 37.54(9) . . . . ?
Cl4 Fe2 P3 C7 48.63(10) . . . . ?
Cl3 Fe2 P3 C7 -85.08(10) . . . . ?
P4 Fe2 P3 C7 158.12(9) . . . . ?
Cl4 Fe2 P4 C10 27.79(8) . . . . ?
Cl3 Fe2 P4 C10 162.95(8) . . . . ?
P3 Fe2 P4 C10 -83.65(8) . . . . ?
Cl4 Fe2 P4 C11 148.24(8) . . . . ?
Cl3 Fe2 P4 C11 -76.60(8) . . . . ?
P3 Fe2 P4 C11 36.79(8) . . . . ?
Cl4 Fe2 P4 C12 -89.54(8) . . . . ?
Cl3 Fe2 P4 C12 45.62(8) . . . . ?
P3 Fe2 P4 C12 159.01(8) . . . . ?

_refine_diff_density_max         0.630
_refine_diff_density_min         -0.383
_refine_diff_density_rms         0.064

_shelxl_version_number           2014-1

_database_code_depnum_ccdc_archive 'CCDC 1023548'
