#------------------------------------------------------------------------------
#$Date: 2024-12-06 18:55:03 +0200 (Fri, 06 Dec 2024) $
#$Revision: 296426 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/57/25/1572555.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_1572555
loop_
_publ_author_name
'Hertler, Phoebe R.'
'Sauza-de la Vega, Arturo'
'Darù, Andrea'
'Sarkar, Arup'
'Lewis, Richard A.'
'Wu, Guang'
'Gagliardi, Laura'
'Hayton, Trevor W.'
_publ_section_title
;
 A homoleptic Fe(iv) ketimide complex with a low-lying excited state.
;
_journal_issue                   40
_journal_name_full               'Chemical science'
_journal_page_first              16559
_journal_page_last               16566
_journal_paper_doi               10.1039/d4sc04880f
_journal_volume                  15
_journal_year                    2024
_chemical_formula_sum            'C44 H56 Fe N4'
_chemical_formula_weight         696.77
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_method           SHELXL-2017/1
_audit_update_record
;
2023-04-07 deposited with the CCDC.	2024-09-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 121.565(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   23.042(6)
_cell_length_b                   9.565(3)
_cell_length_c                   21.412(8)
_cell_measurement_reflns_used    2166
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.20
_cell_measurement_theta_min      2.37
_cell_volume                     4021(2)
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  Bruker_KAPPA_APEX_II
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0533
_diffrn_reflns_av_unetI/netI     0.0619
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            13078
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.484
_diffrn_reflns_theta_min         2.075
_exptl_absorpt_coefficient_mu    0.409
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6546
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            dark_brown
_exptl_crystal_density_diffrn    1.151
_exptl_crystal_description       blocks
_exptl_crystal_F_000             1496
_exptl_crystal_size_max          .7
_exptl_crystal_size_mid          .5
_exptl_crystal_size_min          .3
_refine_diff_density_max         0.540
_refine_diff_density_min         -0.506
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.381
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     228
_refine_ls_number_reflns         4131
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.381
_refine_ls_R_factor_all          0.0701
_refine_ls_R_factor_gt           0.0441
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     'w=1/[σ²(Fo²)] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0565
_refine_ls_wR_factor_ref         0.0603
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3054
_reflns_number_total             4131
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d4sc04880f2.cif
_cod_data_source_block           complex_2
_cod_depositor_comments
'Adding full bibliography for 1572554--1572556.cif.'
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               1572555
_shelx_shelxl_version_number     2017/1
_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+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'
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 0.12163(4) 0.750000 0.01387(11) Uani 1 2 d S T P . .
N1 N 0.44982(7) 0.11035(15) 0.65397(9) 0.0143(4) Uani 1 1 d . . . . .
N2 N 0.57440(7) 0.15453(15) 0.74622(8) 0.0152(4) Uani 1 1 d . . . . .
C17 C 0.60120(9) 0.39602(19) 0.74018(10) 0.0143(4) Uani 1 1 d . . . . .
C12 C 0.61414(9) 0.24051(19) 0.74334(10) 0.0138(5) Uani 1 1 d . . . . .
C1 C 0.41336(9) 0.1075(2) 0.58545(11) 0.0140(4) Uani 1 1 d . . . . .
C6 C 0.39438(9) 0.2433(2) 0.54422(11) 0.0157(5) Uani 1 1 d . . . . .
C18 C 0.64991(10) 0.4916(2) 0.78724(11) 0.0200(5) Uani 1 1 d . . . . .
H18 H 0.693934 0.459881 0.823786 0.024 Uiso 1 1 calc R U . . .
C2 C 0.38762(9) -0.03363(19) 0.54384(11) 0.0162(5) Uani 1 1 d . . . . .
C19 C 0.63476(10) 0.6330(2) 0.78128(11) 0.0233(5) Uani 1 1 d . . . . .
H19 H 0.668460 0.697216 0.814062 0.028 Uiso 1 1 calc R U . . .
C13 C 0.67392(9) 0.18429(19) 0.73689(11) 0.0163(5) Uani 1 1 d . . . . .
C20 C 0.57170(10) 0.6813(2) 0.72862(12) 0.0241(5) Uani 1 1 d . . . . .
H20 H 0.561770 0.778486 0.724584 0.029 Uiso 1 1 calc R U . . .
C22 C 0.53727(10) 0.4452(2) 0.68744(12) 0.0237(5) Uani 1 1 d . . . . .
H22 H 0.503122 0.381246 0.655134 0.028 Uiso 1 1 calc R U . . .
C15 C 0.67829(10) 0.2680(2) 0.67866(11) 0.0248(5) Uani 1 1 d . . . . .
H15A H 0.715141 0.230667 0.673440 0.037 Uiso 1 1 calc R U . . .
H15B H 0.687493 0.366317 0.693521 0.037 Uiso 1 1 calc R U . . .
H15C H 0.635028 0.260587 0.631701 0.037 Uiso 1 1 calc R U . . .
C11 C 0.35768(9) 0.34049(19) 0.55791(11) 0.0218(5) Uani 1 1 d . . . . .
H11 H 0.342995 0.317823 0.590682 0.026 Uiso 1 1 calc R U . . .
C7 C 0.41564(10) 0.2787(2) 0.49652(11) 0.0237(5) Uani 1 1 d . . . . .
H7 H 0.440409 0.212853 0.486253 0.028 Uiso 1 1 calc R U . . .
C9 C 0.36399(10) 0.5045(2) 0.47738(12) 0.0278(6) Uani 1 1 d . . . . .
H9 H 0.353498 0.593683 0.454440 0.033 Uiso 1 1 calc R U . . .
C5 C 0.32447(9) -0.0121(2) 0.46778(11) 0.0257(5) Uani 1 1 d . . . . .
H5A H 0.304993 -0.103163 0.445812 0.039 Uiso 1 1 calc R U . . .
H5B H 0.337169 0.037982 0.436732 0.039 Uiso 1 1 calc R U . . .
H5C H 0.290730 0.042714 0.471959 0.039 Uiso 1 1 calc R U . . .
C4 C 0.44505(9) -0.1008(2) 0.53775(12) 0.0275(5) Uani 1 1 d . . . . .
H4A H 0.486164 -0.108207 0.586656 0.041 Uiso 1 1 calc R U . . .
H4B H 0.454642 -0.042783 0.506478 0.041 Uiso 1 1 calc R U . . .
H4C H 0.430968 -0.194294 0.516248 0.041 Uiso 1 1 calc R U . . .
C10 C 0.34224(10) 0.4703(2) 0.52423(12) 0.0273(6) Uani 1 1 d . . . . .
H10 H 0.316606 0.535646 0.533510 0.033 Uiso 1 1 calc R U . . .
C8 C 0.40110(10) 0.4093(2) 0.46368(12) 0.0306(6) Uani 1 1 d . . . . .
H8 H 0.416614 0.433330 0.431791 0.037 Uiso 1 1 calc R U . . .
C21 C 0.52278(11) 0.5872(2) 0.68149(12) 0.0299(6) Uani 1 1 d . . . . .
H21 H 0.478982 0.619760 0.644824 0.036 Uiso 1 1 calc R U . . .
C14 C 0.74141(9) 0.1933(2) 0.81112(11) 0.0274(6) Uani 1 1 d . . . . .
H14A H 0.777928 0.151127 0.806844 0.041 Uiso 1 1 calc R U . . .
H14B H 0.736988 0.143071 0.848309 0.041 Uiso 1 1 calc R U . . .
H14C H 0.752313 0.291596 0.825534 0.041 Uiso 1 1 calc R U . . .
C16 C 0.66052(10) 0.03027(19) 0.71353(12) 0.0280(6) Uani 1 1 d . . . . .
H16A H 0.617018 0.022039 0.666889 0.042 Uiso 1 1 calc R U . . .
H16B H 0.658690 -0.024498 0.751141 0.042 Uiso 1 1 calc R U . . .
H16C H 0.697303 -0.005091 0.707644 0.042 Uiso 1 1 calc R U . . .
C3 C 0.36968(10) -0.1288(2) 0.58867(11) 0.0290(5) Uani 1 1 d . . . . .
H3A H 0.333091 -0.086058 0.592638 0.043 Uiso 1 1 calc R U . . .
H3B H 0.409943 -0.141659 0.637796 0.043 Uiso 1 1 calc R U . . .
H3C H 0.354515 -0.219816 0.564334 0.043 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
C C 0.0033 0.0016 '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'
Fe Fe 0.3463 0.8444 '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'
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
N1 Fe1 N1 172.96(10) 2_656 . ?
N1 Fe1 N2 90.99(7) 2_656 2_656 ?
N1 Fe1 N2 90.26(7) . 2_656 ?
N1 Fe1 N2 90.26(7) 2_656 . ?
N1 Fe1 N2 90.98(7) . . ?
N2 Fe1 N2 159.70(10) 2_656 . ?
C1 N1 Fe1 177.62(16) . . ?
C12 N2 Fe1 149.24(14) . . ?
C22 C17 C18 118.54(18) . . ?
C22 C17 C12 118.09(17) . . ?
C18 C17 C12 123.37(17) . . ?
N2 C12 C17 120.97(16) . . ?
N2 C12 C13 118.81(17) . . ?
C17 C12 C13 120.05(16) . . ?
N1 C1 C6 118.72(18) . . ?
N1 C1 C2 120.74(18) . . ?
C6 C1 C2 120.54(17) . . ?
C7 C6 C11 118.78(18) . . ?
C7 C6 C1 122.57(17) . . ?
C11 C6 C1 118.53(18) . . ?
C19 C18 C17 120.46(18) . . ?
C19 C18 H18 119.8 . . ?
C17 C18 H18 119.8 . . ?
C5 C2 C3 109.29(16) . . ?
C5 C2 C4 110.37(17) . . ?
C3 C2 C4 109.39(16) . . ?
C5 C2 C1 111.04(16) . . ?
C3 C2 C1 107.75(17) . . ?
C4 C2 C1 108.95(15) . . ?
C20 C19 C18 120.81(19) . . ?
C20 C19 H19 119.6 . . ?
C18 C19 H19 119.6 . . ?
C15 C13 C16 108.96(17) . . ?
C15 C13 C14 110.55(16) . . ?
C16 C13 C14 108.24(15) . . ?
C15 C13 C12 109.38(16) . . ?
C16 C13 C12 108.99(15) . . ?
C14 C13 C12 110.68(16) . . ?
C19 C20 C21 119.26(19) . . ?
C19 C20 H20 120.4 . . ?
C21 C20 H20 120.4 . . ?
C17 C22 C21 120.56(19) . . ?
C17 C22 H22 119.7 . . ?
C21 C22 H22 119.7 . . ?
C13 C15 H15A 109.5 . . ?
C13 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C13 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C10 C11 C6 120.6(2) . . ?
C10 C11 H11 119.7 . . ?
C6 C11 H11 119.7 . . ?
C8 C7 C6 120.6(2) . . ?
C8 C7 H7 119.7 . . ?
C6 C7 H7 119.7 . . ?
C10 C9 C8 120.0(2) . . ?
C10 C9 H9 120.0 . . ?
C8 C9 H9 120.0 . . ?
C2 C5 H5A 109.5 . . ?
C2 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C2 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C2 C4 H4A 109.5 . . ?
C2 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
C2 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C9 C10 C11 120.1(2) . . ?
C9 C10 H10 120.0 . . ?
C11 C10 H10 120.0 . . ?
C9 C8 C7 119.9(2) . . ?
C9 C8 H8 120.0 . . ?
C7 C8 H8 120.0 . . ?
C20 C21 C22 120.4(2) . . ?
C20 C21 H21 119.8 . . ?
C22 C21 H21 119.8 . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C13 C16 H16A 109.5 . . ?
C13 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C13 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C2 C3 H3A 109.5 . . ?
C2 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
C2 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 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 N1 1.7570(17) 2_656 ?
Fe1 N1 1.7571(17) . ?
Fe1 N2 1.7858(15) 2_656 ?
Fe1 N2 1.7859(15) . ?
N1 C1 1.253(2) . ?
N2 C12 1.256(2) . ?
C17 C22 1.388(2) . ?
C17 C18 1.388(2) . ?
C17 C12 1.512(2) . ?
C12 C13 1.551(2) . ?
C1 C6 1.501(3) . ?
C1 C2 1.554(3) . ?
C6 C7 1.386(3) . ?
C6 C11 1.387(2) . ?
C18 C19 1.386(2) . ?
C18 H18 0.9500 . ?
C2 C5 1.527(3) . ?
C2 C3 1.529(3) . ?
C2 C4 1.537(2) . ?
C19 C20 1.372(3) . ?
C19 H19 0.9500 . ?
C13 C15 1.528(3) . ?
C13 C16 1.534(2) . ?
C13 C14 1.538(3) . ?
C20 C21 1.382(3) . ?
C20 H20 0.9500 . ?
C22 C21 1.388(2) . ?
C22 H22 0.9500 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C11 C10 1.385(3) . ?
C11 H11 0.9500 . ?
C7 C8 1.386(3) . ?
C7 H7 0.9500 . ?
C9 C10 1.375(3) . ?
C9 C8 1.382(3) . ?
C9 H9 0.9500 . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C10 H10 0.9500 . ?
C8 H8 0.9500 . ?
C21 H21 0.9500 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
