#------------------------------------------------------------------------------
#$Date: 2024-09-11 00:09:24 +0200 (Wed 11 de Sep de 2024) $
#$Revision: 294701 $
#$URL: svn://www.crystallography.net/cod/cif/1/57/25/1572556.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_1572556
loop_
_publ_author_name
'Hertler, Phoebe'
'Hayton, Trevor W.'
'Sauza-de la Vega, Arturo'
'Daru, Andrea'
'Sarkar, Arup'
'Lewis, Richard A.'
'Wu, Guang'
'Gagliardi, Laura'
_publ_section_title
;
 A Homoleptic Fe(IV) Ketimide Complex with a Low-Lying Excited State
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D4SC04880F
_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
;
2024-06-18 deposited with the CCDC.	2024-09-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 122.075(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   23.477(12)
_cell_length_b                   9.781(5)
_cell_length_c                   21.869(16)
_cell_measurement_reflns_used    3951
_cell_measurement_temperature    287(2)
_cell_measurement_theta_max      23.81
_cell_measurement_theta_min      2.20
_cell_volume                     4255(4)
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      287(2)
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.952
_diffrn_measurement_device_type  'Bruker KAPPA APEX2'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0631
_diffrn_reflns_av_unetI/netI     0.0662
_diffrn_reflns_Laue_measured_fraction_full 0.978
_diffrn_reflns_Laue_measured_fraction_max 0.952
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            13888
_diffrn_reflns_point_group_measured_fraction_full 0.978
_diffrn_reflns_point_group_measured_fraction_max 0.952
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.843
_diffrn_reflns_theta_min         2.047
_exptl_absorpt_coefficient_mu    0.386
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.5162
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.088
_exptl_crystal_description       block
_exptl_crystal_F_000             1496
_exptl_crystal_size_max          0.7
_exptl_crystal_size_mid          0.5
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.347
_refine_diff_density_min         -0.941
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     228
_refine_ls_number_reflns         4352
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0779
_refine_ls_R_factor_gt           0.0581
_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)+(0.0923P)²+1.1504P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1466
_refine_ls_wR_factor_ref         0.1607
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3285
_reflns_number_total             4352
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d4sc04880f2.cif
_cod_data_source_block           complex_2_287K
_cod_original_cell_volume        4255(5)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               1572556
_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 0.87031(4) 0.250000 0.03409(18) Uani 1 2 d S T P . .
N2 N 0.42621(11) 0.83913(19) 0.25259(10) 0.0406(5) Uani 1 1 d . . . . .
N1 N 0.54935(11) 0.88148(18) 0.34488(10) 0.0405(5) Uani 1 1 d . . . . .
C12 C 0.38594(13) 0.7580(2) 0.25526(12) 0.0397(5) Uani 1 1 d . . . . .
C17 C 0.39653(14) 0.6055(2) 0.25739(13) 0.0440(6) Uani 1 1 d . . . . .
C1 C 0.58419(13) 0.8863(2) 0.41261(12) 0.0407(6) Uani 1 1 d . . . . .
C6 C 0.60142(14) 0.7535(3) 0.45365(13) 0.0487(6) Uani 1 1 d . . . . .
C2 C 0.61007(15) 1.0253(3) 0.45249(14) 0.0541(7) Uani 1 1 d . . . . .
C22 C 0.34768(16) 0.5142(3) 0.20870(18) 0.0680(8) Uani 1 1 d . . . . .
H22 H 0.305720 0.546435 0.172799 0.082 Uiso 1 1 calc R U . . .
C13 C 0.32787(15) 0.8169(3) 0.26143(16) 0.0541(7) Uani 1 1 d . . . . .
C11 C 0.63741(19) 0.6558(3) 0.44316(19) 0.0723(9) Uani 1 1 d . . . . .
H11 H 0.652783 0.674959 0.412681 0.087 Uiso 1 1 calc R U . . .
C20 C 0.4219(2) 0.3241(3) 0.2656(2) 0.0798(11) Uani 1 1 d . . . . .
H20 H 0.430249 0.230583 0.268787 0.096 Uiso 1 1 calc R U . . .
C21 C 0.3617(2) 0.3753(3) 0.2138(2) 0.0839(11) Uani 1 1 d . . . . .
H21 H 0.328747 0.315786 0.180783 0.101 Uiso 1 1 calc R U . . .
C18 C 0.45765(17) 0.5523(3) 0.30878(18) 0.0751(10) Uani 1 1 d . . . . .
H18 H 0.491354 0.610981 0.341432 0.090 Uiso 1 1 calc R U . . .
C3 C 0.6726(2) 1.0081(4) 0.52658(19) 0.0975(13) Uani 1 1 d . . . . .
H3A H 0.687858 1.096108 0.548937 0.146 Uiso 1 1 calc R U . . .
H3B H 0.707192 0.965604 0.522241 0.146 Uiso 1 1 calc R U . . .
H3C H 0.662637 0.951764 0.555645 0.146 Uiso 1 1 calc R U . . .
C15 C 0.3244(2) 0.7386(4) 0.3203(2) 0.0856(11) Uani 1 1 d . . . . .
H15A H 0.367651 0.740466 0.364402 0.128 Uiso 1 1 calc R U . . .
H15B H 0.311552 0.645552 0.305355 0.128 Uiso 1 1 calc R U . . .
H15C H 0.291771 0.780949 0.327959 0.128 Uiso 1 1 calc R U . . .
C7 C 0.5790(2) 0.7220(4) 0.49919(19) 0.0823(11) Uani 1 1 d . . . . .
H7 H 0.554495 0.785644 0.507576 0.099 Uiso 1 1 calc R U . . .
C19 C 0.4704(2) 0.4129(4) 0.3132(2) 0.0980(14) Uani 1 1 d . . . . .
H19 H 0.512197 0.379496 0.348791 0.118 Uiso 1 1 calc R U . . .
C14 C 0.26006(18) 0.8026(5) 0.1904(2) 0.0969(13) Uani 1 1 d . . . . .
H14A H 0.226032 0.848729 0.194302 0.145 Uiso 1 1 calc R U . . .
H14B H 0.248734 0.707505 0.180360 0.145 Uiso 1 1 calc R U . . .
H14C H 0.262871 0.842523 0.151994 0.145 Uiso 1 1 calc R U . . .
C9 C 0.6291(3) 0.4997(4) 0.5207(2) 0.1040(15) Uani 1 1 d . . . . .
H9 H 0.638265 0.414462 0.542863 0.125 Uiso 1 1 calc R U . . .
C8 C 0.5936(3) 0.5932(5) 0.5326(2) 0.1070(16) Uani 1 1 d . . . . .
H8 H 0.578593 0.571997 0.563205 0.128 Uiso 1 1 calc R U . . .
C10 C 0.6513(2) 0.5305(4) 0.4765(3) 0.1015(14) Uani 1 1 d . . . . .
H10 H 0.676083 0.466500 0.468706 0.122 Uiso 1 1 calc R U . . .
C4 C 0.5548(2) 1.0920(4) 0.4599(3) 0.1078(15) Uani 1 1 d . . . . .
H4A H 0.545867 1.035889 0.489919 0.162 Uiso 1 1 calc R U . . .
H4C H 0.514614 1.101061 0.413103 0.162 Uiso 1 1 calc R U . . .
H4B H 0.569494 1.180744 0.481490 0.162 Uiso 1 1 calc R U . . .
C16 C 0.3417(2) 0.9669(4) 0.2834(3) 0.0975(14) Uani 1 1 d . . . . .
H16A H 0.308199 1.000682 0.292024 0.146 Uiso 1 1 calc R U . . .
H16B H 0.340340 1.018868 0.245401 0.146 Uiso 1 1 calc R U . . .
H16C H 0.385349 0.975612 0.326631 0.146 Uiso 1 1 calc R U . . .
C5 C 0.6231(3) 1.1215(4) 0.4064(2) 0.1065(16) Uani 1 1 d . . . . .
H5A H 0.637388 1.208884 0.429749 0.160 Uiso 1 1 calc R U . . .
H5B H 0.582514 1.132545 0.359978 0.160 Uiso 1 1 calc R U . . .
H5C H 0.657542 1.083827 0.400321 0.160 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'
Fe Fe 0.3463 0.8444 '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'
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 172.90(12) 2_655 . ?
N1 Fe1 N2 90.33(9) 2_655 . ?
N1 Fe1 N2 90.88(10) . . ?
N1 Fe1 N2 90.88(10) 2_655 2_655 ?
N1 Fe1 N2 90.33(9) . 2_655 ?
N2 Fe1 N2 160.37(12) . 2_655 ?
C12 N2 Fe1 150.71(19) . . ?
C1 N1 Fe1 178.54(18) . . ?
N2 C12 C17 120.6(2) . . ?
N2 C12 C13 119.1(2) . . ?
C17 C12 C13 120.2(2) . . ?
C18 C17 C22 117.4(3) . . ?
C18 C17 C12 118.9(2) . . ?
C22 C17 C12 123.6(3) . . ?
N1 C1 C6 118.1(2) . . ?
N1 C1 C2 120.7(2) . . ?
C6 C1 C2 121.2(2) . . ?
C11 C6 C7 117.8(3) . . ?
C11 C6 C1 119.6(2) . . ?
C7 C6 C1 122.4(3) . . ?
C3 C2 C5 110.8(3) . . ?
C3 C2 C4 109.2(3) . . ?
C5 C2 C4 106.6(3) . . ?
C3 C2 C1 111.9(2) . . ?
C5 C2 C1 109.0(2) . . ?
C4 C2 C1 109.3(3) . . ?
C21 C22 C17 120.1(3) . . ?
C21 C22 H22 120.0 . . ?
C17 C22 H22 120.0 . . ?
C16 C13 C14 109.9(3) . . ?
C16 C13 C15 108.2(3) . . ?
C14 C13 C15 108.4(3) . . ?
C16 C13 C12 109.6(2) . . ?
C14 C13 C12 111.5(2) . . ?
C15 C13 C12 109.2(2) . . ?
C6 C11 C10 121.7(3) . . ?
C6 C11 H11 119.1 . . ?
C10 C11 H11 119.1 . . ?
C21 C20 C19 118.6(3) . . ?
C21 C20 H20 120.7 . . ?
C19 C20 H20 120.7 . . ?
C20 C21 C22 121.8(3) . . ?
C20 C21 H21 119.1 . . ?
C22 C21 H21 119.1 . . ?
C17 C18 C19 121.5(3) . . ?
C17 C18 H18 119.3 . . ?
C19 C18 H18 119.3 . . ?
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 . . ?
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 . . ?
C6 C7 C8 119.6(4) . . ?
C6 C7 H7 120.2 . . ?
C8 C7 H7 120.2 . . ?
C20 C19 C18 120.6(4) . . ?
C20 C19 H19 119.7 . . ?
C18 C19 H19 119.7 . . ?
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 . . ?
C10 C9 C8 119.8(4) . . ?
C10 C9 H9 120.1 . . ?
C8 C9 H9 120.1 . . ?
C9 C8 C7 120.7(4) . . ?
C9 C8 H8 119.6 . . ?
C7 C8 H8 119.6 . . ?
C9 C10 C11 120.3(4) . . ?
C9 C10 H10 119.8 . . ?
C11 C10 H10 119.8 . . ?
C2 C4 H4A 109.5 . . ?
C2 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
C2 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
H4C C4 H4B 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 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 . . ?
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 1.763(2) 2_655 ?
Fe1 N1 1.763(2) . ?
Fe1 N2 1.789(2) . ?
Fe1 N2 1.789(2) 2_655 ?
N2 C12 1.259(3) . ?
N1 C1 1.256(3) . ?
C12 C17 1.509(3) . ?
C12 C13 1.551(4) . ?
C17 C18 1.371(4) . ?
C17 C22 1.396(4) . ?
C1 C6 1.507(3) . ?
C1 C2 1.554(3) . ?
C6 C11 1.373(4) . ?
C6 C7 1.386(4) . ?
C2 C3 1.511(5) . ?
C2 C5 1.525(4) . ?
C2 C4 1.536(5) . ?
C22 C21 1.388(5) . ?
C22 H22 0.9300 . ?
C13 C16 1.525(5) . ?
C13 C14 1.530(5) . ?
C13 C15 1.537(4) . ?
C11 C10 1.375(5) . ?
C11 H11 0.9300 . ?
C20 C21 1.354(5) . ?
C20 C19 1.369(5) . ?
C20 H20 0.9300 . ?
C21 H21 0.9300 . ?
C18 C19 1.389(4) . ?
C18 H18 0.9300 . ?
C3 H3A 0.9600 . ?
C3 H3B 0.9600 . ?
C3 H3C 0.9600 . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C7 C8 1.404(6) . ?
C7 H7 0.9300 . ?
C19 H19 0.9300 . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C9 C10 1.353(6) . ?
C9 C8 1.353(6) . ?
C9 H9 0.9300 . ?
C8 H8 0.9300 . ?
C10 H10 0.9300 . ?
C4 H4A 0.9600 . ?
C4 H4C 0.9600 . ?
C4 H4B 0.9600 . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C5 H5A 0.9600 . ?
C5 H5B 0.9600 . ?
C5 H5C 0.9600 . ?
