#------------------------------------------------------------------------------
#$Date: 2023-09-28 01:46:11 +0300 (Thu, 28 Sep 2023) $
#$Revision: 286563 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/71/40/7714038.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7714038
loop_
_publ_author_name
'Ishii, Reon'
'Nakagawa, Minesato'
'Wada, Yoshimasa'
'Sunada, Yusuke'
_publ_section_title
;
 Four- and Three-coordinate Planar Iron(II) Complexes Supported by Bulky
 Organosilyl Ligands
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT02219F
_journal_year                    2023
_chemical_formula_moiety         'C32 H78 Fe N4 Si8'
_chemical_formula_sum            'C32 H78 Fe N4 Si8'
_chemical_formula_weight         799.53
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_update_record
;
2023-04-22 deposited with the CCDC.	2023-09-26 downloaded from the CCDC.
;
_cell_angle_alpha                95.209(2)
_cell_angle_beta                 109.339(3)
_cell_angle_gamma                105.223(2)
_cell_formula_units_Z            1
_cell_length_a                   9.4550(3)
_cell_length_b                   11.6117(3)
_cell_length_c                   11.8561(3)
_cell_measurement_reflns_used    16528
_cell_measurement_temperature    123
_cell_measurement_theta_max      31.27
_cell_measurement_theta_min      2.31
_cell_volume                     1162.32(6)
_computing_cell_refinement       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_molecular_graphics    'CrystalStructure 4.2.5'
_computing_publication_material  'CrystalStructure 4.2.5 (Rigaku, 2017)'
_computing_structure_refinement  'SHELXL Version 2017/1 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT Version 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      123
_diffrn_detector_area_resol_mean 28.626
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.903
_diffrn_measurement_device_type  'Rigaku Saturn724'
_diffrn_measurement_method       ω
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0672
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.903
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            19300
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.903
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.103
_diffrn_reflns_theta_min         2.353
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.556
_exptl_absorpt_correction_T_max  0.757
_exptl_absorpt_correction_T_min  0.243
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.93a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.142
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             436.00
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.500
_exptl_crystal_size_min          0.500
_refine_diff_density_max         0.87
_refine_diff_density_min         -0.85
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     218
_refine_ls_number_reflns         6744
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0505
_refine_ls_R_factor_gt           0.0449
_refine_ls_shift/su_max          0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[σ²(Fo²)+(0.0748P)²+0.1103P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1194
_refine_ls_wR_factor_ref         0.1233
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5929
_reflns_number_total             6744
_reflns_threshold_expression     F²>2.0σ(F²)
_cod_data_source_file            d3dt02219f2.cif
_cod_data_source_block           Fe[Si(TMS)3]2(ITMe)2
_cod_database_code               7714038
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 +X,+Y,+Z
2 -X,-Y,-Z
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 0.500000 0.500000 0.01414(9) Uani 1 2 d S . P . .
Si1 Si 0.33740(4) 0.32428(3) 0.32077(3) 0.01576(10) Uani 1 1 d . . . . .
Si2 Si 0.47500(5) 0.24754(4) 0.21330(4) 0.02030(10) Uani 1 1 d . . . . .
Si3 Si 0.17849(5) 0.13730(4) 0.34085(4) 0.02078(11) Uani 1 1 d . . . . .
Si4 Si 0.15066(5) 0.37940(4) 0.16587(3) 0.02010(10) Uani 1 1 d . . . . .
N1 N 0.31575(15) 0.38747(11) 0.64332(11) 0.0202(2) Uani 1 1 d . . . . .
N2 N 0.49671(15) 0.30680(11) 0.65394(11) 0.0215(3) Uani 1 1 d . . . . .
C1 C 0.5440(2) 0.35322(16) 0.11718(15) 0.0293(3) Uani 1 1 d . . . . .
H1A H 0.625732 0.332029 0.097526 0.035 Uiso 1 1 calc R U . . .
H1B H 0.584202 0.435550 0.161694 0.035 Uiso 1 1 calc R U . . .
H1C H 0.457025 0.345878 0.043393 0.035 Uiso 1 1 calc R U . . .
C2 C 0.3602(2) 0.09863(15) 0.10213(15) 0.0318(4) Uani 1 1 d . . . . .
H2A H 0.325148 0.037339 0.144598 0.038 Uiso 1 1 calc R U . . .
H2B H 0.426574 0.074484 0.064831 0.038 Uiso 1 1 calc R U . . .
H2C H 0.270488 0.108286 0.040394 0.038 Uiso 1 1 calc R U . . .
C3 C 0.65052(19) 0.21297(16) 0.31907(15) 0.0292(3) Uani 1 1 d . . . . .
H3A H 0.703727 0.182816 0.272519 0.035 Uiso 1 1 calc R U . . .
H3B H 0.615651 0.152613 0.362501 0.035 Uiso 1 1 calc R U . . .
H3C H 0.721613 0.285867 0.376086 0.035 Uiso 1 1 calc R U . . .
C4 C 0.0334(2) 0.03752(17) 0.19130(16) 0.0415(5) Uani 1 1 d . . . . .
H4A H 0.078712 0.047403 0.129968 0.050 Uiso 1 1 calc R U . . .
H4B H -0.061322 0.060307 0.167587 0.050 Uiso 1 1 calc R U . . .
H4C H 0.008722 -0.045994 0.200132 0.050 Uiso 1 1 calc R U . . .
C5 C 0.04849(19) 0.15062(16) 0.42789(16) 0.0303(3) Uani 1 1 d . . . . .
H5A H 0.111135 0.175073 0.513429 0.036 Uiso 1 1 calc R U . . .
H5B H -0.029949 0.073334 0.413015 0.036 Uiso 1 1 calc R U . . .
H5C H -0.002334 0.210274 0.401808 0.036 Uiso 1 1 calc R U . . .
C6 C 0.2957(2) 0.03955(15) 0.41750(17) 0.0346(4) Uani 1 1 d . . . . .
H6A H 0.225125 -0.036932 0.417318 0.041 Uiso 1 1 calc R U . . .
H6B H 0.360560 0.079966 0.500018 0.041 Uiso 1 1 calc R U . . .
H6C H 0.361401 0.025626 0.374358 0.041 Uiso 1 1 calc R U . . .
C7 C 0.0062(2) 0.25906(16) 0.02984(15) 0.0358(4) Uani 1 1 d . . . . .
H7A H -0.041486 0.297278 -0.034553 0.043 Uiso 1 1 calc R U . . .
H7B H -0.074111 0.208378 0.052312 0.043 Uiso 1 1 calc R U . . .
H7C H 0.060546 0.210213 0.002444 0.043 Uiso 1 1 calc R U . . .
C8 C 0.2449(2) 0.49878(15) 0.09351(14) 0.0283(3) Uani 1 1 d . . . . .
H8A H 0.175484 0.545490 0.062817 0.034 Uiso 1 1 calc R U . . .
H8B H 0.264575 0.460309 0.027605 0.034 Uiso 1 1 calc R U . . .
H8C H 0.342712 0.551576 0.153115 0.034 Uiso 1 1 calc R U . . .
C9 C 0.02369(19) 0.43857(16) 0.23444(16) 0.0312(4) Uani 1 1 d . . . . .
H9A H -0.042190 0.472919 0.176025 0.037 Uiso 1 1 calc R U . . .
H9B H 0.089773 0.500030 0.305802 0.037 Uiso 1 1 calc R U . . .
H9C H -0.041168 0.372913 0.256409 0.037 Uiso 1 1 calc R U . . .
C10 C 0.43598(17) 0.39206(12) 0.60381(12) 0.0184(3) Uani 1 1 d . . . . .
C11 C 0.20449(19) 0.45299(15) 0.59966(15) 0.0269(3) Uani 1 1 d . . . . .
H11A H 0.242628 0.510634 0.555058 0.032 Uiso 1 1 calc R U . . .
H11B H 0.192484 0.495221 0.667673 0.032 Uiso 1 1 calc R U . . .
H11C H 0.104364 0.396669 0.547224 0.032 Uiso 1 1 calc R U . . .
C12 C 0.30400(19) 0.30291(13) 0.71884(13) 0.0248(3) Uani 1 1 d . . . . .
C13 C 0.1815(2) 0.28198(17) 0.77413(17) 0.0362(4) Uani 1 1 d . . . . .
H13A H 0.078895 0.248193 0.710924 0.043 Uiso 1 1 calc R U . . .
H13B H 0.188203 0.357870 0.818502 0.043 Uiso 1 1 calc R U . . .
H13C H 0.198295 0.226363 0.828641 0.043 Uiso 1 1 calc R U . . .
C14 C 0.4178(2) 0.25258(13) 0.72576(13) 0.0257(3) Uani 1 1 d . . . . .
C15 C 0.4644(3) 0.15809(16) 0.79323(17) 0.0387(4) Uani 1 1 d . . . . .
H15A H 0.394555 0.130787 0.835243 0.046 Uiso 1 1 calc R U . . .
H15B H 0.570596 0.192058 0.851193 0.046 Uiso 1 1 calc R U . . .
H15C H 0.458146 0.090512 0.736743 0.046 Uiso 1 1 calc R U . . .
C16 C 0.63081(19) 0.28079(15) 0.63799(15) 0.0287(3) Uani 1 1 d . . . . .
H16A H 0.654740 0.320487 0.575957 0.034 Uiso 1 1 calc R U . . .
H16B H 0.606674 0.194512 0.614083 0.034 Uiso 1 1 calc R U . . .
H16C H 0.720195 0.310074 0.713325 0.034 Uiso 1 1 calc R U . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
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)
;
N N 0.0061 0.0033
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
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)
;
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
C10 Fe1 C10 180.00(8) . 2_666 ?
C10 Fe1 Si1 92.65(4) . 2_666 ?
C10 Fe1 Si1 87.35(4) 2_666 2_666 ?
C10 Fe1 Si1 87.35(4) . . ?
C10 Fe1 Si1 92.65(4) 2_666 . ?
Si1 Fe1 Si1 180.0 2_666 . ?
Si4 Si1 Si2 102.273(19) . . ?
Si4 Si1 Si3 101.10(2) . . ?
Si2 Si1 Si3 99.218(19) . . ?
Si4 Si1 Fe1 111.868(17) . . ?
Si2 Si1 Fe1 116.914(17) . . ?
Si3 Si1 Fe1 122.514(18) . . ?
C3 Si2 C1 108.57(8) . . ?
C3 Si2 C2 102.96(8) . . ?
C1 Si2 C2 103.64(8) . . ?
C3 Si2 Si1 111.82(5) . . ?
C1 Si2 Si1 113.15(5) . . ?
C2 Si2 Si1 115.85(6) . . ?
C5 Si3 C6 105.28(9) . . ?
C5 Si3 C4 102.43(9) . . ?
C6 Si3 C4 104.95(9) . . ?
C5 Si3 Si1 115.65(6) . . ?
C6 Si3 Si1 113.35(6) . . ?
C4 Si3 Si1 113.95(6) . . ?
C8 Si4 C7 102.48(8) . . ?
C8 Si4 C9 109.27(8) . . ?
C7 Si4 C9 104.60(8) . . ?
C8 Si4 Si1 112.64(5) . . ?
C7 Si4 Si1 118.92(6) . . ?
C9 Si4 Si1 108.35(6) . . ?
C10 N1 C12 111.83(13) . . ?
C10 N1 C11 122.72(13) . . ?
C12 N1 C11 125.08(13) . . ?
C10 N2 C14 111.59(13) . . ?
C10 N2 C16 123.28(13) . . ?
C14 N2 C16 125.07(13) . . ?
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 . . ?
N1 C10 N2 103.49(12) . . ?
N1 C10 Fe1 126.15(11) . . ?
N2 C10 Fe1 130.36(11) . . ?
N1 C11 H11A 109.5 . . ?
N1 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
N1 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C14 C12 N1 106.41(14) . . ?
C14 C12 C13 131.78(16) . . ?
N1 C12 C13 121.81(15) . . ?
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 . . ?
C12 C14 N2 106.65(14) . . ?
C12 C14 C15 131.24(16) . . ?
N2 C14 C15 122.10(16) . . ?
C14 C15 H15A 109.5 . . ?
C14 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C14 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
N2 C16 H16A 109.5 . . ?
N2 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
N2 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
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 C10 1.9563(15) . ?
Fe1 C10 1.9564(15) 2_666 ?
Fe1 Si1 2.5385(4) 2_666 ?
Fe1 Si1 2.5385(4) . ?
Si1 Si4 2.3578(5) . ?
Si1 Si2 2.3687(5) . ?
Si1 Si3 2.3760(6) . ?
Si2 C3 1.8843(16) . ?
Si2 C1 1.8856(18) . ?
Si2 C2 1.8863(16) . ?
Si3 C5 1.8737(17) . ?
Si3 C6 1.8771(17) . ?
Si3 C4 1.8841(17) . ?
Si4 C8 1.8773(18) . ?
Si4 C7 1.8838(16) . ?
Si4 C9 1.8848(16) . ?
N1 C10 1.3565(19) . ?
N1 C12 1.3951(19) . ?
N1 C11 1.444(2) . ?
N2 C10 1.3574(18) . ?
N2 C14 1.396(2) . ?
N2 C16 1.444(2) . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C2 H2A 0.9600 . ?
C2 H2B 0.9600 . ?
C2 H2C 0.9600 . ?
C3 H3A 0.9600 . ?
C3 H3B 0.9600 . ?
C3 H3C 0.9600 . ?
C4 H4A 0.9600 . ?
C4 H4B 0.9600 . ?
C4 H4C 0.9600 . ?
C5 H5A 0.9600 . ?
C5 H5B 0.9600 . ?
C5 H5C 0.9600 . ?
C6 H6A 0.9600 . ?
C6 H6B 0.9600 . ?
C6 H6C 0.9600 . ?
C7 H7A 0.9600 . ?
C7 H7B 0.9600 . ?
C7 H7C 0.9600 . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
C12 C14 1.337(2) . ?
C12 C13 1.488(2) . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C14 C15 1.489(2) . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
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
C12 N1 C10 N2 1.31(15) . . . . ?
C11 N1 C10 N2 -172.11(12) . . . . ?
C12 N1 C10 Fe1 -178.28(10) . . . . ?
C11 N1 C10 Fe1 8.30(19) . . . . ?
C14 N2 C10 N1 -1.48(15) . . . . ?
C16 N2 C10 N1 -178.96(12) . . . . ?
C14 N2 C10 Fe1 178.08(10) . . . . ?
C16 N2 C10 Fe1 0.6(2) . . . . ?
C10 N1 C12 C14 -0.67(16) . . . . ?
C11 N1 C12 C14 172.56(13) . . . . ?
C10 N1 C12 C13 179.64(13) . . . . ?
C11 N1 C12 C13 -7.1(2) . . . . ?
N1 C12 C14 N2 -0.27(16) . . . . ?
C13 C12 C14 N2 179.38(16) . . . . ?
N1 C12 C14 C15 179.36(16) . . . . ?
C13 C12 C14 C15 -1.0(3) . . . . ?
C10 N2 C14 C12 1.13(16) . . . . ?
C16 N2 C14 C12 178.56(13) . . . . ?
C10 N2 C14 C15 -178.54(14) . . . . ?
C16 N2 C14 C15 -1.1(2) . . . . ?
