# Electronic Supplementary Material (ESI) for Dalton Transactions.
# 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_complex_2b
_database_code_depnum_ccdc_archive 'CCDC 1430351'
_audit_update_record             
;
2015-10-09 deposited with the CCDC.
2018-02-16 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C26 H39 Fe P3 Si'
_chemical_formula_weight         528.42

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 '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'

_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                   10.5677(9)
_cell_length_b                   17.7146(15)
_cell_length_c                   15.1486(14)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.232(2)
_cell_angle_gamma                90.00
_cell_volume                     2835.8(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    5029
_cell_measurement_theta_min      2.35
_cell_measurement_theta_max      27.51

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.14
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.238
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1120
_exptl_absorpt_coefficient_mu    0.755
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_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_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            13959
_diffrn_reflns_av_R_equivalents  0.0495
_diffrn_reflns_av_unetI/netI     0.0626
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         1.77
_diffrn_reflns_theta_max         25.00
_reflns_number_total             4981
_reflns_number_gt                3838
_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-97 (Sheldrick, 2008)'
_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)+(0.0538P)²+0.8420P] 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         4981
_refine_ls_number_parameters     292
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0668
_refine_ls_R_factor_gt           0.0464
_refine_ls_wR_factor_ref         0.1117
_refine_ls_wR_factor_gt          0.1044
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_restrained_S_all      1.041
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.50497(4) 0.18858(2) 0.26726(3) 0.01737(14) Uani 1 1 d . . .
P1 P 0.41411(7) 0.07944(4) 0.26029(5) 0.0168(2) Uani 1 1 d . . .
Si1 Si 0.69894(8) 0.13779(5) 0.25433(6) 0.0195(2) Uani 1 1 d . . .
P3 P 0.43604(8) 0.24283(5) 0.38854(6) 0.0237(2) Uani 1 1 d . . .
P2 P 0.40637(9) 0.26124(5) 0.17234(6) 0.0288(2) Uani 1 1 d . . .
C13 C 0.3164(3) 0.04717(17) 0.3527(2) 0.0187(7) Uani 1 1 d . . .
C18 C 0.3640(3) -0.00038(18) 0.4182(2) 0.0229(8) Uani 1 1 d . . .
H18 H 0.4435 -0.0244 0.4099 0.027 Uiso 1 1 calc R . .
C1 C 0.5399(3) 0.00728(18) 0.2546(2) 0.0193(7) Uani 1 1 d . . .
C7 C 0.3238(3) 0.05156(17) 0.1611(2) 0.0209(7) Uani 1 1 d . . .
C3 C 0.7592(3) -0.0246(2) 0.2478(2) 0.0270(8) Uani 1 1 d . . .
H3 H 0.8458 -0.0102 0.2463 0.032 Uiso 1 1 calc R . .
C14 C 0.1989(3) 0.08084(18) 0.3668(2) 0.0236(8) Uani 1 1 d . . .
H14 H 0.1646 0.1138 0.3234 0.028 Uiso 1 1 calc R . .
C26 C 0.4119(4) 0.36338(19) 0.1894(3) 0.0432(10) Uani 1 1 d . . .
H26A H 0.3636 0.3887 0.1426 0.065 Uiso 1 1 calc R . .
H26B H 0.5000 0.3805 0.1880 0.065 Uiso 1 1 calc R . .
H26C H 0.3749 0.3757 0.2469 0.065 Uiso 1 1 calc R . .
C8 C 0.3868(3) 0.0571(2) 0.0803(2) 0.0306(9) Uani 1 1 d . . .
H8 H 0.4723 0.0737 0.0797 0.037 Uiso 1 1 calc R . .
C15 C 0.1314(3) 0.0670(2) 0.4432(2) 0.0301(9) Uani 1 1 d . . .
H15 H 0.0507 0.0896 0.4511 0.036 Uiso 1 1 calc R . .
C23 C 0.7944(3) 0.1573(2) 0.1513(2) 0.0350(9) Uani 1 1 d . . .
H23A H 0.8080 0.2118 0.1454 0.053 Uiso 1 1 calc R . .
H23B H 0.7483 0.1386 0.0995 0.053 Uiso 1 1 calc R . .
H23C H 0.8764 0.1317 0.1556 0.053 Uiso 1 1 calc R . .
C4 C 0.7283(4) -0.1005(2) 0.2449(2) 0.0344(9) Uani 1 1 d . . .
H4 H 0.7936 -0.1373 0.2426 0.041 Uiso 1 1 calc R . .
C5 C 0.6032(3) -0.1231(2) 0.2453(3) 0.0341(9) Uani 1 1 d . . .
H5 H 0.5822 -0.1752 0.2429 0.041 Uiso 1 1 calc R . .
C12 C 0.1999(3) 0.02623(18) 0.1592(2) 0.0274(8) Uani 1 1 d . . .
H12 H 0.1546 0.0209 0.2129 0.033 Uiso 1 1 calc R . .
C2 C 0.6659(3) 0.03157(18) 0.2530(2) 0.0196(7) Uani 1 1 d . . .
C19 C 0.2763(4) 0.2829(2) 0.3972(3) 0.0393(10) Uani 1 1 d . . .
H19A H 0.2135 0.2425 0.3916 0.059 Uiso 1 1 calc R . .
H19B H 0.2633 0.3200 0.3500 0.059 Uiso 1 1 calc R . .
H19C H 0.2669 0.3077 0.4546 0.059 Uiso 1 1 calc R . .
C22 C 0.8222(3) 0.1562(2) 0.3425(2) 0.0321(9) Uani 1 1 d . . .
H22A H 0.8986 0.1270 0.3295 0.048 Uiso 1 1 calc R . .
H22B H 0.7889 0.1412 0.4001 0.048 Uiso 1 1 calc R . .
H22C H 0.8430 0.2101 0.3435 0.048 Uiso 1 1 calc R . .
C21 C 0.5314(4) 0.3224(2) 0.4256(3) 0.0395(10) Uani 1 1 d . . .
H21A H 0.4994 0.3406 0.4824 0.059 Uiso 1 1 calc R . .
H21B H 0.5264 0.3631 0.3819 0.059 Uiso 1 1 calc R . .
H21C H 0.6196 0.3064 0.4325 0.059 Uiso 1 1 calc R . .
C11 C 0.1416(4) 0.0086(2) 0.0803(3) 0.0372(9) Uani 1 1 d . . .
H11 H 0.0563 -0.0084 0.0805 0.045 Uiso 1 1 calc R . .
C20 C 0.4397(4) 0.18660(19) 0.4895(2) 0.0334(9) Uani 1 1 d . . .
H20A H 0.5248 0.1659 0.4982 0.050 Uiso 1 1 calc R . .
H20B H 0.3787 0.1451 0.4845 0.050 Uiso 1 1 calc R . .
H20C H 0.4175 0.2186 0.5399 0.050 Uiso 1 1 calc R . .
C16 C 0.1809(3) 0.0207(2) 0.5081(2) 0.0321(9) Uani 1 1 d . . .
H16 H 0.1353 0.0121 0.5611 0.038 Uiso 1 1 calc R . .
C17 C 0.2972(3) -0.01306(19) 0.4952(2) 0.0295(8) Uani 1 1 d . . .
H17 H 0.3315 -0.0452 0.5394 0.035 Uiso 1 1 calc R . .
C10 C 0.2044(4) 0.0152(2) 0.0018(3) 0.0381(10) Uani 1 1 d . . .
H10 H 0.1629 0.0032 -0.0522 0.046 Uiso 1 1 calc R . .
C6 C 0.5089(3) -0.06937(19) 0.2491(2) 0.0276(8) Uani 1 1 d . . .
H6 H 0.4227 -0.0844 0.2479 0.033 Uiso 1 1 calc R . .
C9 C 0.3280(4) 0.0393(2) 0.0019(3) 0.0373(9) Uani 1 1 d . . .
H9 H 0.3728 0.0436 -0.0522 0.045 Uiso 1 1 calc R . .
C24 C 0.4689(5) 0.2583(3) 0.0598(3) 0.0601(14) Uani 1 1 d . . .
H24A H 0.4547 0.2081 0.0346 0.090 Uiso 1 1 calc R . .
H24B H 0.5598 0.2691 0.0611 0.090 Uiso 1 1 calc R . .
H24C H 0.4256 0.2962 0.0236 0.090 Uiso 1 1 calc R . .
C25 C 0.2371(4) 0.2489(2) 0.1516(3) 0.0522(12) Uani 1 1 d . . .
H25A H 0.1903 0.2572 0.2065 0.078 Uiso 1 1 calc R . .
H25B H 0.2213 0.1976 0.1302 0.078 Uiso 1 1 calc R . .
H25C H 0.2090 0.2854 0.1071 0.078 Uiso 1 1 calc R . .
H H 0.604(3) 0.2438(19) 0.264(2) 0.044(11) 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 P1 2.1612(9) . ?
Fe1 P2 2.1904(10) . ?
Fe1 P3 2.2000(10) . ?
Fe1 Si1 2.2479(10) . ?
Fe1 H 1.44(4) . ?
P1 C13 1.834(3) . ?
P1 C7 1.844(3) . ?
P1 C1 1.847(3) . ?
Si1 C22 1.890(4) . ?
Si1 C23 1.894(3) . ?
Si1 C2 1.914(3) . ?
P3 C21 1.820(4) . ?
P3 C20 1.825(4) . ?
P3 C19 1.836(4) . ?
P2 C25 1.828(4) . ?
P2 C26 1.829(4) . ?
P2 C24 1.831(4) . ?
C13 C18 1.395(4) . ?
C13 C14 1.395(4) . ?
C18 C17 1.384(4) . ?
C18 H18 0.9500 . ?
C1 C6 1.399(5) . ?
C1 C2 1.400(4) . ?
C7 C12 1.385(4) . ?
C7 C8 1.398(4) . ?
C3 C4 1.384(5) . ?
C3 C2 1.403(4) . ?
C3 H3 0.9500 . ?
C14 C15 1.383(4) . ?
C14 H14 0.9500 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C8 C9 1.376(5) . ?
C8 H8 0.9500 . ?
C15 C16 1.381(5) . ?
C15 H15 0.9500 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C4 C5 1.382(5) . ?
C4 H4 0.9500 . ?
C5 C6 1.379(5) . ?
C5 H5 0.9500 . ?
C12 C11 1.378(5) . ?
C12 H12 0.9500 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C11 C10 1.370(5) . ?
C11 H11 0.9500 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C16 C17 1.381(5) . ?
C16 H16 0.9500 . ?
C17 H17 0.9500 . ?
C10 C9 1.375(5) . ?
C10 H10 0.9500 . ?
C6 H6 0.9500 . ?
C9 H9 0.9500 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 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
P1 Fe1 P2 106.47(4) . . ?
P1 Fe1 P3 106.44(4) . . ?
P2 Fe1 P3 97.66(4) . . ?
P1 Fe1 Si1 92.45(3) . . ?
P2 Fe1 Si1 127.55(4) . . ?
P3 Fe1 Si1 123.56(4) . . ?
P1 Fe1 H 158.9(14) . . ?
P2 Fe1 H 85.8(15) . . ?
P3 Fe1 H 88.4(14) . . ?
Si1 Fe1 H 66.6(14) . . ?
C13 P1 C7 104.31(14) . . ?
C13 P1 C1 103.16(14) . . ?
C7 P1 C1 98.44(14) . . ?
C13 P1 Fe1 119.54(10) . . ?
C7 P1 Fe1 120.51(11) . . ?
C1 P1 Fe1 107.56(11) . . ?
C22 Si1 C23 100.53(17) . . ?
C22 Si1 C2 107.62(15) . . ?
C23 Si1 C2 105.58(15) . . ?
C22 Si1 Fe1 119.69(12) . . ?
C23 Si1 Fe1 119.19(13) . . ?
C2 Si1 Fe1 103.19(10) . . ?
C21 P3 C20 98.89(18) . . ?
C21 P3 C19 100.71(18) . . ?
C20 P3 C19 99.64(18) . . ?
C21 P3 Fe1 114.29(13) . . ?
C20 P3 Fe1 117.09(12) . . ?
C19 P3 Fe1 122.42(13) . . ?
C25 P2 C26 99.95(18) . . ?
C25 P2 C24 101.2(2) . . ?
C26 P2 C24 98.5(2) . . ?
C25 P2 Fe1 120.34(14) . . ?
C26 P2 Fe1 118.27(14) . . ?
C24 P2 Fe1 114.96(15) . . ?
C18 C13 C14 117.9(3) . . ?
C18 C13 P1 121.9(2) . . ?
C14 C13 P1 119.2(2) . . ?
C17 C18 C13 120.9(3) . . ?
C17 C18 H18 119.5 . . ?
C13 C18 H18 119.5 . . ?
C6 C1 C2 121.3(3) . . ?
C6 C1 P1 120.4(2) . . ?
C2 C1 P1 118.2(2) . . ?
C12 C7 C8 117.3(3) . . ?
C12 C7 P1 126.1(3) . . ?
C8 C7 P1 116.6(2) . . ?
C4 C3 C2 121.6(3) . . ?
C4 C3 H3 119.2 . . ?
C2 C3 H3 119.2 . . ?
C15 C14 C13 121.0(3) . . ?
C15 C14 H14 119.5 . . ?
C13 C14 H14 119.5 . . ?
P2 C26 H26A 109.5 . . ?
P2 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
P2 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C9 C8 C7 121.6(3) . . ?
C9 C8 H8 119.2 . . ?
C7 C8 H8 119.2 . . ?
C16 C15 C14 120.3(3) . . ?
C16 C15 H15 119.8 . . ?
C14 C15 H15 119.8 . . ?
Si1 C23 H23A 109.5 . . ?
Si1 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
Si1 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C5 C4 C3 120.5(3) . . ?
C5 C4 H4 119.8 . . ?
C3 C4 H4 119.8 . . ?
C6 C5 C4 119.4(3) . . ?
C6 C5 H5 120.3 . . ?
C4 C5 H5 120.3 . . ?
C11 C12 C7 120.7(3) . . ?
C11 C12 H12 119.6 . . ?
C7 C12 H12 119.6 . . ?
C1 C2 C3 116.9(3) . . ?
C1 C2 Si1 118.4(2) . . ?
C3 C2 Si1 124.7(2) . . ?
P3 C19 H19A 109.5 . . ?
P3 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
P3 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
Si1 C22 H22A 109.5 . . ?
Si1 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
Si1 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
P3 C21 H21A 109.5 . . ?
P3 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
P3 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C10 C11 C12 121.2(3) . . ?
C10 C11 H11 119.4 . . ?
C12 C11 H11 119.4 . . ?
P3 C20 H20A 109.5 . . ?
P3 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
P3 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C17 C16 C15 119.4(3) . . ?
C17 C16 H16 120.3 . . ?
C15 C16 H16 120.3 . . ?
C16 C17 C18 120.4(3) . . ?
C16 C17 H17 119.8 . . ?
C18 C17 H17 119.8 . . ?
C11 C10 C9 119.3(3) . . ?
C11 C10 H10 120.4 . . ?
C9 C10 H10 120.4 . . ?
C5 C6 C1 120.2(3) . . ?
C5 C6 H6 119.9 . . ?
C1 C6 H6 119.9 . . ?
C10 C9 C8 119.9(3) . . ?
C10 C9 H9 120.1 . . ?
C8 C9 H9 120.1 . . ?
P2 C24 H24A 109.5 . . ?
P2 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
P2 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
P2 C25 H25A 109.5 . . ?
P2 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
P2 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.835
_refine_diff_density_min         -0.365
_refine_diff_density_rms         0.079
