# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2019

####################################################################### 
# 
# 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_Fe[Si(TMS)3]2(THF)2
_database_code_depnum_ccdc_archive 'CCDC 1884063'
_audit_update_record             
;
2018-12-10 deposited with the CCDC.
2019-02-06 downloaded from the CCDC.
;

#==============================================================================
# CHEMICAL DATA

_chemical_formula_sum            'C34 H70 Fe O4 Si8'
_chemical_formula_moiety         'C34 H70 Fe O4 Si8'
_chemical_formula_weight         823.46
_chemical_melting_point          ?

#==============================================================================
# CRYSTAL DATA
_space_group_crystal_system      monoclinic
_space_group_name_H-M_alt        'P 1 2/c 1'
_space_group_name_Hall           '-P 2yc'
_space_group_IT_number           13
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 +X,+Y,+Z
2 -X,+Y,1/2-Z
3 -X,-Y,-Z
4 +X,-Y,-1/2+Z
#------------------------------------------------------------------------------
_cell_length_a                   13.790(3)
_cell_length_b                   10.428(2)
_cell_length_c                   18.950(5)
_cell_angle_alpha                90.0000
_cell_angle_beta                 111.077(4)
_cell_angle_gamma                90.0000
_cell_volume                     2542.7(10)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    5197
_cell_measurement_theta_min      3.00
_cell_measurement_theta_max      27.49
_cell_measurement_temperature    183
#------------------------------------------------------------------------------
_exptl_crystal_description       prism
_exptl_crystal_colour            pueple
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.100
_exptl_crystal_density_diffrn    1.075
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             888.00
_exptl_absorpt_coefficient_mu    0.513
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_absorpt_correction_T_min  0.841
_exptl_absorpt_correction_T_max  0.950

#==============================================================================
# EXPERIMENTAL DATA

_diffrn_ambient_temperature      183
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_measurement_device_type  'Rigaku Saturn724'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean 7.111
_diffrn_reflns_number            20592
_diffrn_reflns_av_R_equivalents  0.0358
_diffrn_reflns_theta_max         27.475
_diffrn_reflns_theta_min         3.001
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measured_fraction_theta_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.971
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       18
_diffrn_standards_number         0
_diffrn_standards_interval_count .
_diffrn_standards_decay_%        ?
_reflns_number_total             5663
_reflns_number_gt                4573
_reflns_threshold_expression     F²>2.0σ(F²)
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

#==============================================================================
# REFINEMENT DATA

_refine_special_details          
;
    Refinement was performed using all reflections. The weighted 
    R-factor (wR) and goodness of fit (S) are based on F².
    R-factor (gt) are based on F. The threshold expression of
    F² > 2.0 sigma(F²) is used only for calculating R-factor (gt).
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_R_factor_all          0.0634
_refine_ls_R_factor_gt           0.0513
_refine_ls_wR_factor_ref         0.1458
_refine_ls_wR_factor_gt          0.1352
_refine_ls_number_restraints     0
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_reflns         5663
_refine_ls_number_parameters     200
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w = 1/[σ²(Fo²)+(0.0783P)²+1.1831P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_refine_ls_shift/su_max          0.001
_refine_diff_density_max         0.95
_refine_diff_density_min         -0.78
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?

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 for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
H H 0.0000 0.0000
;
International Tables for Crystallography
(Vol. C, Table 6.1.1.4)
;
O O 0.0106 0.0060
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
Fe Fe 0.3463 0.8444
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
Si Si 0.0817 0.0704
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;

#==============================================================================
# ATOMIC COORDINATES AND THERMAL PARAMETERS

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 0.500000 0.88335(4) 0.250000 0.02655(14) Uani 1 2 d S T P . .
Si1 Si 0.31841(5) 0.97628(6) 0.21698(4) 0.03136(17) Uani 1 1 d . . . . .
Si2 Si 0.18218(5) 0.85507(7) 0.13095(4) 0.03651(18) Uani 1 1 d . . . . .
Si3 Si 0.26501(6) 1.00440(8) 0.32095(4) 0.0420(2) Uani 1 1 d . . . . .
Si4 Si 0.29258(6) 1.18051(7) 0.16088(5) 0.0425(2) Uani 1 1 d . . . . .
O1 O 0.50606(14) 0.73847(17) 0.32890(9) 0.0380(4) Uani 1 1 d . . . . .
O3 O 0.2343(5) 0.4777(6) 0.4029(4) 0.184(2) Uiso 1 1 d . . . . .
C1 C 0.1663(2) 0.8870(3) 0.02911(15) 0.0512(7) Uani 1 1 d . . . . .
H1A H 0.154924 0.978886 0.018466 0.061 Uiso 1 1 calc R U . . .
H1B H 0.229245 0.859939 0.020567 0.061 Uiso 1 1 calc R U . . .
H1C H 0.106510 0.838754 -0.004452 0.061 Uiso 1 1 calc R U . . .
C2 C 0.2037(2) 0.6772(3) 0.14701(17) 0.0514(7) Uani 1 1 d . . . . .
H2A H 0.271531 0.653969 0.145086 0.062 Uiso 1 1 calc R U . . .
H2B H 0.201701 0.654674 0.196693 0.062 Uiso 1 1 calc R U . . .
H2C H 0.148897 0.630380 0.107590 0.062 Uiso 1 1 calc R U . . .
C3 C 0.0502(2) 0.8871(3) 0.13596(18) 0.0550(8) Uani 1 1 d . . . . .
H3A H 0.034135 0.978701 0.128003 0.066 Uiso 1 1 calc R U . . .
H3B H -0.002486 0.837447 0.096698 0.066 Uiso 1 1 calc R U . . .
H3C H 0.050318 0.861741 0.185800 0.066 Uiso 1 1 calc R U . . .
C4 C 0.1502(2) 1.1141(3) 0.3014(2) 0.0587(9) Uani 1 1 d . . . . .
H4A H 0.165592 1.197025 0.283471 0.070 Uiso 1 1 calc R U . . .
H4B H 0.089356 1.075782 0.262528 0.070 Uiso 1 1 calc R U . . .
H4C H 0.135686 1.126575 0.347871 0.070 Uiso 1 1 calc R U . . .
C5 C 0.2270(3) 0.8494(4) 0.35464(19) 0.0598(8) Uani 1 1 d . . . . .
H5A H 0.284389 0.788024 0.365816 0.072 Uiso 1 1 calc R U . . .
H5B H 0.211603 0.865162 0.400502 0.072 Uiso 1 1 calc R U . . .
H5C H 0.165273 0.814369 0.315159 0.072 Uiso 1 1 calc R U . . .
C6 C 0.3703(3) 1.0775(4) 0.40455(18) 0.0708(11) Uani 1 1 d . . . . .
H6A H 0.433131 1.024642 0.417981 0.085 Uiso 1 1 calc R U . . .
H6B H 0.385646 1.164198 0.391592 0.085 Uiso 1 1 calc R U . . .
H6C H 0.346922 1.081605 0.447601 0.085 Uiso 1 1 calc R U . . .
C7 C 0.3585(3) 1.1906(3) 0.0902(2) 0.0632(9) Uani 1 1 d . . . . .
H7A H 0.331032 1.123665 0.051824 0.076 Uiso 1 1 calc R U . . .
H7B H 0.345392 1.274975 0.065792 0.076 Uiso 1 1 calc R U . . .
H7C H 0.433445 1.178390 0.115895 0.076 Uiso 1 1 calc R U . . .
C8 C 0.1525(3) 1.2266(3) 0.1098(2) 0.0637(9) Uani 1 1 d . . . . .
H8A H 0.115052 1.222516 0.145008 0.076 Uiso 1 1 calc R U . . .
H8B H 0.149017 1.314027 0.090145 0.076 Uiso 1 1 calc R U . . .
H8C H 0.120613 1.167090 0.067803 0.076 Uiso 1 1 calc R U . . .
C9 C 0.3490(3) 1.3112(3) 0.2322(2) 0.0646(9) Uani 1 1 d . . . . .
H9A H 0.316356 1.309067 0.270384 0.077 Uiso 1 1 calc R U . . .
H9B H 0.424062 1.297994 0.256785 0.077 Uiso 1 1 calc R U . . .
H9C H 0.336008 1.394579 0.206682 0.077 Uiso 1 1 calc R U . . .
C10 C 0.4362(2) 0.6305(3) 0.31733(16) 0.0455(7) Uani 1 1 d . . . . .
H10A H 0.436503 0.577937 0.273901 0.055 Uiso 1 1 calc R U . . .
H10B H 0.364325 0.659899 0.307812 0.055 Uiso 1 1 calc R U . . .
C11 C 0.4771(3) 0.5561(4) 0.38881(19) 0.0711(11) Uani 1 1 d . . . . .
H11A H 0.533900 0.497986 0.388831 0.085 Uiso 1 1 calc R U . . .
H11B H 0.421535 0.505103 0.396971 0.085 Uiso 1 1 calc R U . . .
C12 C 0.5172(3) 0.6605(4) 0.44866(17) 0.0666(10) Uani 1 1 d . . . . .
H12A H 0.461051 0.692899 0.464877 0.080 Uiso 1 1 calc R U . . .
H12B H 0.574829 0.628190 0.493463 0.080 Uiso 1 1 calc R U . . .
C13 C 0.5541(3) 0.7622(3) 0.40938(15) 0.0526(8) Uani 1 1 d . . . . .
H13A H 0.533961 0.847844 0.422002 0.063 Uiso 1 1 calc R U . . .
H13B H 0.630740 0.759138 0.425138 0.063 Uiso 1 1 calc R U . . .
C14 C 0.0616(10) 0.5182(13) 0.3528(7) 0.110(4) Uiso 0.5 1 d . . P . .
C16 C 0.2148(10) 0.4679(13) 0.4642(7) 0.108(4) Uiso 0.5 1 d . . P . .
C17 C 0.0884(9) 0.4771(11) 0.4352(6) 0.085(3) Uiso 0.5 1 d . . P . .
C18 C 0.0588(9) 0.4523(12) 0.3531(6) 0.097(3) Uiso 0.5 1 d . . P . .
C19 C 0.1019(12) 0.5316(14) 0.4380(8) 0.115(4) Uiso 0.5 1 d . . P . .
C20 C 0.2024(12) 0.5454(16) 0.4694(8) 0.129(4) Uiso 0.5 1 d . . P . .
C21 C 0.1521(6) 0.4875(7) 0.3331(5) 0.144(2) Uiso 1 1 d . . . . .


#==============================================================================
_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_cell_refinement       CrystalClear
_computing_data_reduction        CrystalClear
_computing_structure_solution    'Il Milione (Burla, et al., 2007)'
_computing_structure_refinement  'SHELXL Version 2017/1 (Sheldrick, 2008)'
_computing_publication_material  'CrystalStructure 4.2.5 (Rigaku, 2017)'
_computing_molecular_graphics    'CrystalStructure 4.2.5'

#==============================================================================
# MOLECULAR GEOMETRY

_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 O1 2.1060(17) . ?
Fe1 O1 2.1060(17) 2_655 ?
Fe1 Si1 2.5444(8) 2_655 ?
Fe1 Si1 2.5445(8) . ?
Si1 Si4 2.3494(11) . ?
Si1 Si3 2.3565(11) . ?
Si1 Si2 2.3626(10) . ?
Si2 C2 1.886(3) . ?
Si2 C3 1.886(3) . ?
Si2 C1 1.892(3) . ?
Si3 C4 1.879(3) . ?
Si3 C5 1.880(4) . ?
Si3 C6 1.883(3) . ?
Si4 C7 1.873(3) . ?
Si4 C9 1.880(3) . ?
Si4 C8 1.885(3) . ?
O1 C10 1.446(3) . ?
O1 C13 1.449(3) . ?
O3 C16 1.286(12) . ?
O3 C21 1.402(8) . ?
O3 C20 1.637(15) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 C11 1.485(4) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 C12 1.525(5) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 C13 1.486(4) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C14 C18 0.689(16) . ?
C14 C21 1.461(14) . ?
C14 C19 1.514(18) . ?
C14 C17 1.531(17) . ?
C16 C20 0.840(17) . ?
C16 C19 1.599(19) . ?
C16 C17 1.631(17) . ?
C17 C19 0.594(17) . ?
C17 C18 1.482(15) . ?
C17 C20 1.632(19) . ?
C18 C21 1.512(14) . ?
C18 C19 1.714(18) . ?
C19 C20 1.305(18) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Fe1 O1 88.32(10) . 2_655 ?
O1 Fe1 Si1 108.32(5) . 2_655 ?
O1 Fe1 Si1 103.42(5) 2_655 2_655 ?
O1 Fe1 Si1 103.42(5) . . ?
O1 Fe1 Si1 108.32(5) 2_655 . ?
Si1 Fe1 Si1 135.23(4) 2_655 . ?
Si4 Si1 Si3 102.91(4) . . ?
Si4 Si1 Si2 102.66(4) . . ?
Si3 Si1 Si2 103.50(4) . . ?
Si4 Si1 Fe1 115.60(3) . . ?
Si3 Si1 Fe1 114.68(3) . . ?
Si2 Si1 Fe1 115.72(3) . . ?
C2 Si2 C3 105.33(15) . . ?
C2 Si2 C1 106.96(14) . . ?
C3 Si2 C1 105.10(14) . . ?
C2 Si2 Si1 112.03(10) . . ?
C3 Si2 Si1 114.38(11) . . ?
C1 Si2 Si1 112.41(10) . . ?
C4 Si3 C5 105.80(15) . . ?
C4 Si3 C6 105.07(17) . . ?
C5 Si3 C6 106.67(19) . . ?
C4 Si3 Si1 113.90(11) . . ?
C5 Si3 Si1 112.71(11) . . ?
C6 Si3 Si1 112.06(11) . . ?
C7 Si4 C9 106.98(17) . . ?
C7 Si4 C8 106.84(17) . . ?
C9 Si4 C8 105.49(17) . . ?
C7 Si4 Si1 109.94(12) . . ?
C9 Si4 Si1 112.05(13) . . ?
C8 Si4 Si1 115.07(12) . . ?
C10 O1 C13 108.66(19) . . ?
C10 O1 Fe1 126.62(15) . . ?
C13 O1 Fe1 120.75(16) . . ?
C16 O3 C21 119.8(8) . . ?
C16 O3 C20 30.5(7) . . ?
C21 O3 C20 110.2(7) . . ?
Si2 C1 H1A 109.5 . . ?
Si2 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
Si2 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
Si2 C2 H2A 109.5 . . ?
Si2 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
Si2 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
Si2 C3 H3A 109.5 . . ?
Si2 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
Si2 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
Si3 C4 H4A 109.5 . . ?
Si3 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
Si3 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
Si3 C5 H5A 109.5 . . ?
Si3 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
Si3 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
Si3 C6 H6A 109.5 . . ?
Si3 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
Si3 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
Si4 C7 H7A 109.5 . . ?
Si4 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
Si4 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
Si4 C8 H8A 109.5 . . ?
Si4 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
Si4 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
Si4 C9 H9A 109.5 . . ?
Si4 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
Si4 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
O1 C10 C11 104.7(2) . . ?
O1 C10 H10A 110.8 . . ?
C11 C10 H10A 110.8 . . ?
O1 C10 H10B 110.8 . . ?
C11 C10 H10B 110.8 . . ?
H10A C10 H10B 108.9 . . ?
C10 C11 C12 102.9(3) . . ?
C10 C11 H11A 111.2 . . ?
C12 C11 H11A 111.2 . . ?
C10 C11 H11B 111.2 . . ?
C12 C11 H11B 111.2 . . ?
H11A C11 H11B 109.1 . . ?
C13 C12 C11 103.6(3) . . ?
C13 C12 H12A 111.0 . . ?
C11 C12 H12A 111.0 . . ?
C13 C12 H12B 111.0 . . ?
C11 C12 H12B 111.0 . . ?
H12A C12 H12B 109.0 . . ?
O1 C13 C12 107.2(2) . . ?
O1 C13 H13A 110.3 . . ?
C12 C13 H13A 110.3 . . ?
O1 C13 H13B 110.3 . . ?
C12 C13 H13B 110.3 . . ?
H13A C13 H13B 108.5 . . ?
C18 C14 C21 80.8(18) . . ?
C18 C14 C19 94.7(19) . . ?
C21 C14 C19 105.8(10) . . ?
C18 C14 C17 72.8(17) . . ?
C21 C14 C17 106.4(10) . . ?
C19 C14 C17 22.5(7) . . ?
C20 C16 O3 98.5(17) . . ?
C20 C16 C19 54.5(14) . . ?
O3 C16 C19 100.6(10) . . ?
C20 C16 C17 75.2(15) . . ?
O3 C16 C17 103.7(9) . . ?
C19 C16 C17 21.2(6) . . ?
C19 C17 C18 103(2) . . ?
C19 C17 C14 77(2) . . ?
C18 C17 C14 26.4(6) . . ?
C19 C17 C16 76(2) . . ?
C18 C17 C16 101.6(9) . . ?
C14 C17 C16 101.4(9) . . ?
C19 C17 C20 47(2) . . ?
C18 C17 C20 110.9(9) . . ?
C14 C17 C20 97.4(9) . . ?
C16 C17 C20 29.8(6) . . ?
C14 C18 C17 80.8(18) . . ?
C14 C18 C21 72.5(17) . . ?
C17 C18 C21 106.4(9) . . ?
C14 C18 C19 61.7(17) . . ?
C17 C18 C19 19.8(6) . . ?
C21 C18 C19 94.5(8) . . ?
C17 C19 C20 113(3) . . ?
C17 C19 C14 80(2) . . ?
C20 C19 C14 114.8(13) . . ?
C17 C19 C16 82(2) . . ?
C20 C19 C16 31.6(8) . . ?
C14 C19 C16 103.6(11) . . ?
C17 C19 C18 57(2) . . ?
C20 C19 C18 115.8(13) . . ?
C14 C19 C18 23.6(6) . . ?
C16 C19 C18 93.5(9) . . ?
C16 C20 C19 93.9(18) . . ?
C16 C20 C17 75.0(15) . . ?
C19 C20 C17 19.6(8) . . ?
C16 C20 O3 51.0(13) . . ?
C19 C20 O3 97.9(11) . . ?
C17 C20 O3 89.6(8) . . ?
O3 C21 C14 104.5(8) . . ?
O3 C21 C18 102.6(7) . . ?
C14 C21 C18 26.7(6) . . ?

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
C13 O1 C10 C11 -24.7(3) . . . . ?
Fe1 O1 C10 C11 177.8(2) . . . . ?
O1 C10 C11 C12 35.4(4) . . . . ?
C10 C11 C12 C13 -32.9(4) . . . . ?
C10 O1 C13 C12 3.4(4) . . . . ?
Fe1 O1 C13 C12 162.4(2) . . . . ?
C11 C12 C13 O1 18.5(4) . . . . ?
C21 O3 C16 C20 -79.2(18) . . . . ?
C21 O3 C16 C19 -23.9(14) . . . . ?
C20 O3 C16 C19 55.3(15) . . . . ?
C21 O3 C16 C17 -2.5(14) . . . . ?
C20 O3 C16 C17 76.7(16) . . . . ?
C18 C14 C17 C19 166(3) . . . . ?
C21 C14 C17 C19 92(2) . . . . ?
C21 C14 C17 C18 -74.6(17) . . . . ?
C19 C14 C17 C18 -166(3) . . . . ?
C18 C14 C17 C16 93.2(19) . . . . ?
C21 C14 C17 C16 18.7(12) . . . . ?
C19 C14 C17 C16 -73(2) . . . . ?
C18 C14 C17 C20 123.2(19) . . . . ?
C21 C14 C17 C20 48.7(12) . . . . ?
C19 C14 C17 C20 -43(2) . . . . ?
C20 C16 C17 C19 11(2) . . . . ?
O3 C16 C17 C19 -84(2) . . . . ?
C20 C16 C17 C18 111.9(16) . . . . ?
O3 C16 C17 C18 16.6(13) . . . . ?
C19 C16 C17 C18 101(2) . . . . ?
C20 C16 C17 C14 85.0(17) . . . . ?
O3 C16 C17 C14 -10.3(13) . . . . ?
C19 C16 C17 C14 74(2) . . . . ?
O3 C16 C17 C20 -95.3(17) . . . . ?
C19 C16 C17 C20 -11(2) . . . . ?
C21 C14 C18 C17 110.5(7) . . . . ?
C19 C14 C18 C17 5.2(11) . . . . ?
C19 C14 C18 C21 -105.3(10) . . . . ?
C17 C14 C18 C21 -110.5(7) . . . . ?
C21 C14 C18 C19 105.3(10) . . . . ?
C17 C14 C18 C19 -5.2(11) . . . . ?
C19 C17 C18 C14 -14(3) . . . . ?
C16 C17 C18 C14 -92.2(19) . . . . ?
C20 C17 C18 C14 -63(2) . . . . ?
C19 C17 C18 C21 55(3) . . . . ?
C14 C17 C18 C21 68.6(16) . . . . ?
C16 C17 C18 C21 -23.6(12) . . . . ?
C20 C17 C18 C21 6.0(14) . . . . ?
C14 C17 C18 C19 14(3) . . . . ?
C16 C17 C18 C19 -78(2) . . . . ?
C20 C17 C18 C19 -49(2) . . . . ?
C18 C17 C19 C20 -106.7(18) . . . . ?
C14 C17 C19 C20 -112.9(19) . . . . ?
C16 C17 C19 C20 -7.6(17) . . . . ?
C18 C17 C19 C14 6.2(13) . . . . ?
C16 C17 C19 C14 105.3(8) . . . . ?
C20 C17 C19 C14 112.9(19) . . . . ?
C18 C17 C19 C16 -99.1(12) . . . . ?
C14 C17 C19 C16 -105.3(8) . . . . ?
C20 C17 C19 C16 7.6(17) . . . . ?
C14 C17 C19 C18 -6.2(13) . . . . ?
C16 C17 C19 C18 99.1(12) . . . . ?
C20 C17 C19 C18 106.7(18) . . . . ?
C18 C14 C19 C17 -13(3) . . . . ?
C21 C14 C19 C17 -95(2) . . . . ?
C18 C14 C19 C20 98(2) . . . . ?
C21 C14 C19 C20 16.3(18) . . . . ?
C17 C14 C19 C20 111(3) . . . . ?
C18 C14 C19 C16 67(2) . . . . ?
C21 C14 C19 C16 -15.2(14) . . . . ?
C17 C14 C19 C16 80(2) . . . . ?
C21 C14 C19 C18 -81.7(18) . . . . ?
C17 C14 C19 C18 13(3) . . . . ?
C20 C16 C19 C17 -167(3) . . . . ?
O3 C16 C19 C17 101(2) . . . . ?
O3 C16 C19 C20 -92.9(18) . . . . ?
C17 C16 C19 C20 167(3) . . . . ?
C20 C16 C19 C14 115(2) . . . . ?
O3 C16 C19 C14 22.5(14) . . . . ?
C17 C16 C19 C14 -78(2) . . . . ?
C20 C16 C19 C18 137.0(19) . . . . ?
O3 C16 C19 C18 44.1(11) . . . . ?
C17 C16 C19 C18 -56.5(19) . . . . ?
C14 C18 C19 C17 165(3) . . . . ?
C21 C18 C19 C17 -128(2) . . . . ?
C14 C18 C19 C20 -93(2) . . . . ?
C17 C18 C19 C20 102(3) . . . . ?
C21 C18 C19 C20 -26.0(16) . . . . ?
C17 C18 C19 C14 -165(3) . . . . ?
C21 C18 C19 C14 67.4(18) . . . . ?
C14 C18 C19 C16 -117(2) . . . . ?
C17 C18 C19 C16 79(2) . . . . ?
C21 C18 C19 C16 -49.3(10) . . . . ?
O3 C16 C20 C19 97.0(13) . . . . ?
C17 C16 C20 C19 -5.0(11) . . . . ?
O3 C16 C20 C17 102.0(9) . . . . ?
C19 C16 C20 C17 5.0(11) . . . . ?
C19 C16 C20 O3 -97.0(13) . . . . ?
C17 C16 C20 O3 -102.0(9) . . . . ?
C17 C19 C20 C16 15(3) . . . . ?
C14 C19 C20 C16 -75(2) . . . . ?
C18 C19 C20 C16 -49(2) . . . . ?
C14 C19 C20 C17 -90(3) . . . . ?
C16 C19 C20 C17 -15(3) . . . . ?
C18 C19 C20 C17 -64(2) . . . . ?
C17 C19 C20 O3 66(3) . . . . ?
C14 C19 C20 O3 -24.1(16) . . . . ?
C16 C19 C20 O3 51.2(13) . . . . ?
C18 C19 C20 O3 2.1(16) . . . . ?
C19 C17 C20 C16 -165(3) . . . . ?
C18 C17 C20 C16 -76.6(17) . . . . ?
C14 C17 C20 C16 -100.0(16) . . . . ?
C18 C17 C20 C19 88(3) . . . . ?
C14 C17 C20 C19 65(3) . . . . ?
C16 C17 C20 C19 165(3) . . . . ?
C19 C17 C20 O3 -115(3) . . . . ?
C18 C17 C20 O3 -27.1(12) . . . . ?
C14 C17 C20 O3 -50.5(10) . . . . ?
C16 C17 C20 O3 49.5(12) . . . . ?
C21 O3 C20 C16 114.7(17) . . . . ?
C16 O3 C20 C19 -88.6(19) . . . . ?
C21 O3 C20 C19 26.1(14) . . . . ?
C16 O3 C20 C17 -70.9(16) . . . . ?
C21 O3 C20 C17 43.8(10) . . . . ?
C16 O3 C21 C14 15.0(13) . . . . ?
C20 O3 C21 C14 -17.1(11) . . . . ?
C16 O3 C21 C18 -12.5(12) . . . . ?
C20 O3 C21 C18 -44.6(10) . . . . ?
C18 C14 C21 O3 -89.3(18) . . . . ?
C19 C14 C21 O3 3.0(12) . . . . ?
C17 C14 C21 O3 -20.4(12) . . . . ?
C19 C14 C21 C18 92.3(19) . . . . ?
C17 C14 C21 C18 68.9(17) . . . . ?
C14 C18 C21 O3 97.3(18) . . . . ?
C17 C18 C21 O3 22.7(11) . . . . ?
C19 C18 C21 O3 38.8(9) . . . . ?
C17 C18 C21 C14 -74.5(17) . . . . ?
C19 C18 C21 C14 -58.4(16) . . . . ?

#==============================================================================

#==============================================================================
# Additional structures and associated data_? identifiers
# should be added at this point if there is more than one 
# structure analysis in the CIF.


####################################################################### 
# 
# 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_Fe[Si(TMS)3]2(py)2
_database_code_depnum_ccdc_archive 'CCDC 1884064'
_audit_update_record             
;
2018-12-10 deposited with the CCDC.
2019-02-06 downloaded from the CCDC.
;

#==============================================================================
# CHEMICAL DATA

_chemical_formula_sum            'C28 H64 Fe N2 Si8'
_chemical_formula_moiety         'C28 H64 Fe N2 Si8'
_chemical_formula_weight         709.36
_chemical_melting_point          ?

#==============================================================================
# CRYSTAL DATA
_space_group_crystal_system      triclinic
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
_space_group_IT_number           2
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 +X,+Y,+Z
2 -X,-Y,-Z
#------------------------------------------------------------------------------
_cell_length_a                   10.760(3)
_cell_length_b                   12.605(2)
_cell_length_c                   18.063(4)
_cell_angle_alpha                73.466(10)
_cell_angle_beta                 81.042(11)
_cell_angle_gamma                70.518(9)
_cell_volume                     2209.0(9)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    4446
_cell_measurement_theta_min      3.06
_cell_measurement_theta_max      27.49
_cell_measurement_temperature    193
#------------------------------------------------------------------------------
_exptl_crystal_description       block
_exptl_crystal_colour            darkbrown
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_exptl_crystal_density_diffrn    1.066
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             768.00
_exptl_absorpt_coefficient_mu    0.576
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_absorpt_correction_T_min  0.778
_exptl_absorpt_correction_T_max  0.891

#==============================================================================
# EXPERIMENTAL DATA

_diffrn_ambient_temperature      193
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_measurement_device_type  'Rigaku Saturn724'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean 7.111
_diffrn_reflns_number            18470
_diffrn_reflns_av_R_equivalents  0.0382
_diffrn_reflns_theta_max         27.488
_diffrn_reflns_theta_min         3.060
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.963
_diffrn_measured_fraction_theta_full 0.981
_diffrn_reflns_Laue_measured_fraction_max 0.963
_diffrn_reflns_Laue_measured_fraction_full 0.981
_diffrn_reflns_point_group_measured_fraction_max 0.963
_diffrn_reflns_point_group_measured_fraction_full 0.981
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_standards_number         0
_diffrn_standards_interval_count .
_diffrn_standards_decay_%        ?
_reflns_number_total             9756
_reflns_number_gt                6397
_reflns_threshold_expression     F²>2.0σ(F²)
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

#==============================================================================
# REFINEMENT DATA

_refine_special_details          
;
    Refinement was performed using all reflections. The weighted 
    R-factor (wR) and goodness of fit (S) are based on F².
    R-factor (gt) are based on F. The threshold expression of
    F² > 2.0 sigma(F²) is used only for calculating R-factor (gt).
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_R_factor_all          0.0856
_refine_ls_R_factor_gt           0.0495
_refine_ls_wR_factor_ref         0.1100
_refine_ls_wR_factor_gt          0.0964
_refine_ls_number_restraints     0
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_reflns         9756
_refine_ls_number_parameters     352
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w = 1/[σ²(Fo²)+(0.0424P)²+0.3108P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_refine_ls_shift/su_max          0.000
_refine_diff_density_max         0.35
_refine_diff_density_min         -0.27
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?

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 for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
N N 0.0061 0.0033
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
Fe Fe 0.3463 0.8444
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
Si Si 0.0817 0.0704
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
H H 0.0000 0.0000
;
International Tables for Crystallography
(Vol. C, Table 6.1.1.4)
;

#==============================================================================
# ATOMIC COORDINATES AND THERMAL PARAMETERS

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 0.11671(4) 0.29098(3) 0.26500(2) 0.02998(11) Uani 1 1 d . . . . .
Si1 Si -0.11543(7) 0.42150(6) 0.28608(4) 0.03161(17) Uani 1 1 d . . . . .
Si2 Si -0.23210(7) 0.48690(6) 0.17440(4) 0.03260(18) Uani 1 1 d . . . . .
Si3 Si -0.11542(9) 0.59710(7) 0.30757(5) 0.0449(2) Uani 1 1 d . . . . .
Si4 Si -0.26267(8) 0.35748(7) 0.38526(5) 0.0460(2) Uani 1 1 d . . . . .
Si5 Si 0.21126(7) 0.11299(6) 0.21017(4) 0.03216(18) Uani 1 1 d . . . . .
Si6 Si 0.09494(9) 0.07596(7) 0.12502(5) 0.0463(2) Uani 1 1 d . . . . .
Si7 Si 0.42456(8) 0.09755(7) 0.14867(5) 0.0426(2) Uani 1 1 d . . . . .
Si8 Si 0.24432(8) -0.05625(6) 0.31183(5) 0.03522(18) Uani 1 1 d . . . . .
N1 N 0.2090(2) 0.23889(18) 0.37219(13) 0.0335(5) Uani 1 1 d . . . . .
N2 N 0.2172(2) 0.41325(18) 0.20260(13) 0.0342(5) Uani 1 1 d . . . . .
C1 C -0.3029(3) 0.3754(3) 0.16304(19) 0.0528(8) Uani 1 1 d . . . . .
H1A H -0.2309 0.3054 0.1574 0.063 Uiso 1 1 calc R U . . .
H1B H -0.3538 0.4069 0.1170 0.063 Uiso 1 1 calc R U . . .
H1C H -0.3608 0.3558 0.2089 0.063 Uiso 1 1 calc R U . . .
C2 C -0.1208(3) 0.5205(3) 0.08664(16) 0.0469(8) Uani 1 1 d . . . . .
H2A H -0.0761 0.5728 0.0936 0.056 Uiso 1 1 calc R U . . .
H2B H -0.1732 0.5579 0.0412 0.056 Uiso 1 1 calc R U . . .
H2C H -0.0549 0.4482 0.0791 0.056 Uiso 1 1 calc R U . . .
C3 C -0.3727(3) 0.6248(2) 0.17051(18) 0.0464(7) Uani 1 1 d . . . . .
H3A H -0.4349 0.6135 0.2156 0.056 Uiso 1 1 calc R U . . .
H3B H -0.4182 0.6453 0.1231 0.056 Uiso 1 1 calc R U . . .
H3C H -0.3384 0.6876 0.1708 0.056 Uiso 1 1 calc R U . . .
C4 C -0.2817(3) 0.6862(3) 0.3417(2) 0.0699(11) Uani 1 1 d . . . . .
H4A H -0.2753 0.7596 0.3466 0.084 Uiso 1 1 calc R U . . .
H4B H -0.3099 0.6429 0.3921 0.084 Uiso 1 1 calc R U . . .
H4C H -0.3464 0.7024 0.3041 0.084 Uiso 1 1 calc R U . . .
C5 C -0.0626(3) 0.6944(3) 0.2176(2) 0.0580(9) Uani 1 1 d . . . . .
H5A H -0.0574 0.7637 0.2297 0.070 Uiso 1 1 calc R U . . .
H5B H -0.1272 0.7176 0.1787 0.070 Uiso 1 1 calc R U . . .
H5C H 0.0242 0.6527 0.1972 0.070 Uiso 1 1 calc R U . . .
C6 C -0.0015(4) 0.5707(3) 0.3850(2) 0.0694(11) Uani 1 1 d . . . . .
H6A H -0.0075 0.6450 0.3946 0.083 Uiso 1 1 calc R U . . .
H6B H 0.0896 0.5332 0.3678 0.083 Uiso 1 1 calc R U . . .
H6C H -0.0275 0.5201 0.4328 0.083 Uiso 1 1 calc R U . . .
C7 C -0.2416(3) 0.2005(3) 0.3953(2) 0.0650(10) Uani 1 1 d . . . . .
H7A H -0.2738 0.1925 0.3499 0.078 Uiso 1 1 calc R U . . .
H7B H -0.2921 0.1711 0.4421 0.078 Uiso 1 1 calc R U . . .
H7C H -0.1478 0.1558 0.3990 0.078 Uiso 1 1 calc R U . . .
C8 C -0.4429(3) 0.4377(3) 0.3702(2) 0.0634(10) Uani 1 1 d . . . . .
H8A H -0.4626 0.4384 0.3189 0.076 Uiso 1 1 calc R U . . .
H8B H -0.4624 0.5178 0.3739 0.076 Uiso 1 1 calc R U . . .
H8C H -0.4973 0.3987 0.4100 0.076 Uiso 1 1 calc R U . . .
C9 C -0.2349(4) 0.3719(3) 0.48190(18) 0.0693(11) Uani 1 1 d . . . . .
H9A H -0.1453 0.3242 0.4962 0.083 Uiso 1 1 calc R U . . .
H9B H -0.2993 0.3456 0.5212 0.083 Uiso 1 1 calc R U . . .
H9C H -0.2458 0.4534 0.4786 0.083 Uiso 1 1 calc R U . . .
C10 C 0.0340(4) 0.2058(3) 0.0430(2) 0.0715(11) Uani 1 1 d . . . . .
H10A H -0.0278 0.2695 0.0636 0.086 Uiso 1 1 calc R U . . .
H10B H -0.0112 0.1857 0.0084 0.086 Uiso 1 1 calc R U . . .
H10C H 0.1090 0.2302 0.0143 0.086 Uiso 1 1 calc R U . . .
C11 C -0.0525(3) 0.0345(3) 0.1781(2) 0.0698(11) Uani 1 1 d . . . . .
H11A H -0.0933 0.0825 0.2149 0.084 Uiso 1 1 calc R U . . .
H11B H -0.0247 -0.0476 0.2063 0.084 Uiso 1 1 calc R U . . .
H11C H -0.1165 0.0469 0.1411 0.084 Uiso 1 1 calc R U . . .
C12 C 0.1957(4) -0.0435(3) 0.0771(2) 0.0720(11) Uani 1 1 d . . . . .
H12A H 0.1421 -0.0515 0.0410 0.086 Uiso 1 1 calc R U . . .
H12B H 0.2234 -0.1169 0.1167 0.086 Uiso 1 1 calc R U . . .
H12C H 0.2739 -0.0243 0.0487 0.086 Uiso 1 1 calc R U . . .
C13 C 0.0931(3) -0.0479(3) 0.38038(19) 0.0571(9) Uani 1 1 d . . . . .
H13A H 0.0772 0.0163 0.4045 0.069 Uiso 1 1 calc R U . . .
H13B H 0.1065 -0.1211 0.4205 0.069 Uiso 1 1 calc R U . . .
H13C H 0.0167 -0.0347 0.3519 0.069 Uiso 1 1 calc R U . . .
C14 C 0.3846(3) -0.0796(3) 0.37073(17) 0.0472(8) Uani 1 1 d . . . . .
H14A H 0.3658 -0.0139 0.3939 0.057 Uiso 1 1 calc R U . . .
H14B H 0.4663 -0.0856 0.3373 0.057 Uiso 1 1 calc R U . . .
H14C H 0.3949 -0.1515 0.4118 0.057 Uiso 1 1 calc R U . . .
C15 C 0.2803(3) -0.1954(2) 0.28144(18) 0.0510(8) Uani 1 1 d . . . . .
H15A H 0.2967 -0.2613 0.3271 0.061 Uiso 1 1 calc R U . . .
H15B H 0.3585 -0.2045 0.2450 0.061 Uiso 1 1 calc R U . . .
H15C H 0.2043 -0.1926 0.2564 0.061 Uiso 1 1 calc R U . . .
C16 C 0.5269(3) -0.0544(3) 0.1462(2) 0.0566(9) Uani 1 1 d . . . . .
H16A H 0.4945 -0.0790 0.1081 0.068 Uiso 1 1 calc R U . . .
H16B H 0.5203 -0.1068 0.1975 0.068 Uiso 1 1 calc R U . . .
H16C H 0.6193 -0.0570 0.1319 0.068 Uiso 1 1 calc R U . . .
C17 C 0.5235(3) 0.1503(3) 0.1983(2) 0.0676(11) Uani 1 1 d . . . . .
H17A H 0.4799 0.2327 0.1963 0.081 Uiso 1 1 calc R U . . .
H17B H 0.6122 0.1402 0.1723 0.081 Uiso 1 1 calc R U . . .
H17C H 0.5304 0.1055 0.2525 0.081 Uiso 1 1 calc R U . . .
C18 C 0.4191(4) 0.1861(3) 0.04529(19) 0.0749(12) Uani 1 1 d . . . . .
H18A H 0.3783 0.1546 0.0151 0.090 Uiso 1 1 calc R U . . .
H18B H 0.5092 0.1828 0.0234 0.090 Uiso 1 1 calc R U . . .
H18C H 0.3670 0.2670 0.0435 0.090 Uiso 1 1 calc R U . . .
C19 C 0.3366(3) 0.2212(3) 0.37865(19) 0.0464(7) Uani 1 1 d . . . . .
H19 H 0.3892 0.2429 0.3331 0.056 Uiso 1 1 calc R U . . .
C20 C 0.3963(3) 0.1729(3) 0.4480(2) 0.0541(9) Uani 1 1 d . . . . .
H20 H 0.4874 0.1626 0.4499 0.065 Uiso 1 1 calc R U . . .
C21 C 0.3226(3) 0.1403(3) 0.51339(19) 0.0551(9) Uani 1 1 d . . . . .
H21 H 0.3613 0.1065 0.5618 0.066 Uiso 1 1 calc R U . . .
C22 C 0.1919(3) 0.1571(3) 0.50831(19) 0.0624(10) Uani 1 1 d . . . . .
H22 H 0.1383 0.1345 0.5531 0.075 Uiso 1 1 calc R U . . .
C23 C 0.1391(3) 0.2071(3) 0.43764(18) 0.0488(8) Uani 1 1 d . . . . .
H23 H 0.0476 0.2198 0.4351 0.059 Uiso 1 1 calc R U . . .
C24 C 0.2632(3) 0.4758(2) 0.23414(18) 0.0428(7) Uani 1 1 d . . . . .
H24 H 0.2623 0.4581 0.2889 0.051 Uiso 1 1 calc R U . . .
C25 C 0.3115(3) 0.5641(3) 0.1912(2) 0.0542(9) Uani 1 1 d . . . . .
H25 H 0.3432 0.6061 0.2161 0.065 Uiso 1 1 calc R U . . .
C26 C 0.3135(3) 0.5910(3) 0.1128(2) 0.0613(9) Uani 1 1 d . . . . .
H26 H 0.3466 0.6519 0.0820 0.074 Uiso 1 1 calc R U . . .
C27 C 0.2668(4) 0.5282(3) 0.0790(2) 0.0636(10) Uani 1 1 d . . . . .
H27 H 0.2659 0.5455 0.0243 0.076 Uiso 1 1 calc R U . . .
C28 C 0.2213(3) 0.4400(3) 0.12568(17) 0.0448(7) Uani 1 1 d . . . . .
H28 H 0.1911 0.3959 0.1018 0.054 Uiso 1 1 calc R U . . .


#==============================================================================
_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_cell_refinement       CrystalClear
_computing_data_reduction        CrystalClear
_computing_structure_solution    'Il Milione (Burla, et al., 2007)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_publication_material  'CrystalStructure 4.2.5 (Rigaku, 2017)'
_computing_molecular_graphics    'CrystalStructure 4.2.5'

#==============================================================================
# MOLECULAR GEOMETRY

_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 2.135(2) . ?
Fe1 N1 2.146(2) . ?
Fe1 Si1 2.5317(9) . ?
Fe1 Si5 2.5451(9) . ?
Si1 Si2 2.3402(12) . ?
Si1 Si4 2.3487(12) . ?
Si1 Si3 2.3536(11) . ?
Si2 C2 1.868(3) . ?
Si2 C1 1.877(3) . ?
Si2 C3 1.877(3) . ?
Si3 C5 1.874(3) . ?
Si3 C4 1.885(3) . ?
Si3 C6 1.888(3) . ?
Si4 C7 1.873(3) . ?
Si4 C9 1.884(3) . ?
Si4 C8 1.886(3) . ?
Si5 Si8 2.3488(12) . ?
Si5 Si6 2.3552(12) . ?
Si5 Si7 2.3601(12) . ?
Si6 C11 1.872(4) . ?
Si6 C10 1.873(3) . ?
Si6 C12 1.885(3) . ?
Si7 C17 1.868(3) . ?
Si7 C16 1.873(3) . ?
Si7 C18 1.881(3) . ?
Si8 C14 1.877(3) . ?
Si8 C13 1.877(3) . ?
Si8 C15 1.886(3) . ?
N1 C19 1.333(3) . ?
N1 C23 1.333(4) . ?
N2 C28 1.331(3) . ?
N2 C24 1.340(3) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 C20 1.382(4) . ?
C19 H19 0.9500 . ?
C20 C21 1.357(4) . ?
C20 H20 0.9500 . ?
C21 C22 1.364(4) . ?
C21 H21 0.9500 . ?
C22 C23 1.371(4) . ?
C22 H22 0.9500 . ?
C23 H23 0.9500 . ?
C24 C25 1.371(4) . ?
C24 H24 0.9500 . ?
C25 C26 1.358(5) . ?
C25 H25 0.9500 . ?
C26 C27 1.375(4) . ?
C26 H26 0.9500 . ?
C27 C28 1.373(4) . ?
C27 H27 0.9500 . ?
C28 H28 0.9500 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 Fe1 N1 97.97(9) . . ?
N2 Fe1 Si1 102.21(6) . . ?
N1 Fe1 Si1 107.02(6) . . ?
N2 Fe1 Si5 106.99(6) . . ?
N1 Fe1 Si5 103.74(6) . . ?
Si1 Fe1 Si5 133.60(3) . . ?
Si2 Si1 Si4 104.29(5) . . ?
Si2 Si1 Si3 101.96(4) . . ?
Si4 Si1 Si3 103.78(4) . . ?
Si2 Si1 Fe1 111.83(4) . . ?
Si4 Si1 Fe1 121.14(4) . . ?
Si3 Si1 Fe1 111.83(4) . . ?
C2 Si2 C1 108.11(14) . . ?
C2 Si2 C3 105.13(14) . . ?
C1 Si2 C3 106.93(14) . . ?
C2 Si2 Si1 110.27(10) . . ?
C1 Si2 Si1 111.76(11) . . ?
C3 Si2 Si1 114.25(10) . . ?
C5 Si3 C4 105.73(17) . . ?
C5 Si3 C6 107.99(17) . . ?
C4 Si3 C6 105.16(16) . . ?
C5 Si3 Si1 111.93(10) . . ?
C4 Si3 Si1 114.04(12) . . ?
C6 Si3 Si1 111.51(12) . . ?
C7 Si4 C9 107.52(17) . . ?
C7 Si4 C8 106.33(16) . . ?
C9 Si4 C8 105.31(16) . . ?
C7 Si4 Si1 110.13(11) . . ?
C9 Si4 Si1 112.27(13) . . ?
C8 Si4 Si1 114.83(11) . . ?
Si8 Si5 Si6 102.44(4) . . ?
Si8 Si5 Si7 103.53(4) . . ?
Si6 Si5 Si7 105.11(5) . . ?
Si8 Si5 Fe1 109.59(4) . . ?
Si6 Si5 Fe1 121.57(4) . . ?
Si7 Si5 Fe1 112.75(4) . . ?
C11 Si6 C10 107.47(18) . . ?
C11 Si6 C12 107.51(17) . . ?
C10 Si6 C12 104.84(17) . . ?
C11 Si6 Si5 110.07(12) . . ?
C10 Si6 Si5 112.36(12) . . ?
C12 Si6 Si5 114.21(12) . . ?
C17 Si7 C16 105.37(16) . . ?
C17 Si7 C18 106.52(18) . . ?
C16 Si7 C18 106.29(15) . . ?
C17 Si7 Si5 111.75(11) . . ?
C16 Si7 Si5 114.19(11) . . ?
C18 Si7 Si5 112.14(13) . . ?
C14 Si8 C13 106.60(15) . . ?
C14 Si8 C15 105.64(14) . . ?
C13 Si8 C15 105.55(15) . . ?
C14 Si8 Si5 112.70(10) . . ?
C13 Si8 Si5 110.55(11) . . ?
C15 Si8 Si5 115.18(10) . . ?
C19 N1 C23 116.1(3) . . ?
C19 N1 Fe1 125.2(2) . . ?
C23 N1 Fe1 118.18(19) . . ?
C28 N2 C24 116.5(3) . . ?
C28 N2 Fe1 117.66(18) . . ?
C24 N2 Fe1 125.3(2) . . ?
Si2 C1 H1A 109.5 . . ?
Si2 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
Si2 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
Si2 C2 H2A 109.5 . . ?
Si2 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
Si2 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
Si2 C3 H3A 109.5 . . ?
Si2 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
Si2 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
Si3 C4 H4A 109.5 . . ?
Si3 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
Si3 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
Si3 C5 H5A 109.5 . . ?
Si3 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
Si3 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
Si3 C6 H6A 109.5 . . ?
Si3 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
Si3 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
Si4 C7 H7A 109.5 . . ?
Si4 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
Si4 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
Si4 C8 H8A 109.5 . . ?
Si4 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
Si4 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
Si4 C9 H9A 109.5 . . ?
Si4 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
Si4 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
Si6 C10 H10A 109.5 . . ?
Si6 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
Si6 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
Si6 C11 H11A 109.5 . . ?
Si6 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
Si6 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
Si6 C12 H12A 109.5 . . ?
Si6 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
Si6 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
Si8 C13 H13A 109.5 . . ?
Si8 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
Si8 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
Si8 C14 H14A 109.5 . . ?
Si8 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
Si8 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
Si8 C15 H15A 109.5 . . ?
Si8 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
Si8 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
Si7 C16 H16A 109.5 . . ?
Si7 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
Si7 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
Si7 C17 H17A 109.5 . . ?
Si7 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
Si7 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
Si7 C18 H18A 109.5 . . ?
Si7 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
Si7 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
N1 C19 C20 123.5(3) . . ?
N1 C19 H19 118.3 . . ?
C20 C19 H19 118.3 . . ?
C21 C20 C19 118.9(3) . . ?
C21 C20 H20 120.6 . . ?
C19 C20 H20 120.6 . . ?
C20 C21 C22 118.8(3) . . ?
C20 C21 H21 120.6 . . ?
C22 C21 H21 120.6 . . ?
C21 C22 C23 119.1(3) . . ?
C21 C22 H22 120.5 . . ?
C23 C22 H22 120.5 . . ?
N1 C23 C22 123.7(3) . . ?
N1 C23 H23 118.2 . . ?
C22 C23 H23 118.2 . . ?
N2 C24 C25 123.2(3) . . ?
N2 C24 H24 118.4 . . ?
C25 C24 H24 118.4 . . ?
C26 C25 C24 119.4(3) . . ?
C26 C25 H25 120.3 . . ?
C24 C25 H25 120.3 . . ?
C25 C26 C27 118.5(3) . . ?
C25 C26 H26 120.7 . . ?
C27 C26 H26 120.7 . . ?
C28 C27 C26 118.8(3) . . ?
C28 C27 H27 120.6 . . ?
C26 C27 H27 120.6 . . ?
N2 C28 C27 123.5(3) . . ?
N2 C28 H28 118.3 . . ?
C27 C28 H28 118.3 . . ?

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
C23 N1 C19 C20 0.0(4) . . . . ?
Fe1 N1 C19 C20 -171.0(2) . . . . ?
N1 C19 C20 C21 0.7(5) . . . . ?
C19 C20 C21 C22 -0.4(5) . . . . ?
C20 C21 C22 C23 -0.6(5) . . . . ?
C19 N1 C23 C22 -1.1(4) . . . . ?
Fe1 N1 C23 C22 170.6(3) . . . . ?
C21 C22 C23 N1 1.3(5) . . . . ?
C28 N2 C24 C25 0.6(4) . . . . ?
Fe1 N2 C24 C25 -171.1(2) . . . . ?
N2 C24 C25 C26 0.1(5) . . . . ?
C24 C25 C26 C27 0.0(5) . . . . ?
C25 C26 C27 C28 -0.7(5) . . . . ?
C24 N2 C28 C27 -1.4(4) . . . . ?
Fe1 N2 C28 C27 171.0(3) . . . . ?
C26 C27 C28 N2 1.5(5) . . . . ?

#==============================================================================

#==============================================================================
# Additional structures and associated data_? identifiers
# should be added at this point if there is more than one 
# structure analysis in the CIF.

_shelxl_version_number           2014-1


