Dynamic effects on ligand field from rapid hydride motion in an iron(ii) dimer with an S = 3 ground state
McWilliams, Sean F.; Mercado, Brandon Q.; MacLeod, K. Cory; Fataftah, Majed S.; Tarrago, Maxime; Wang, Xiaoping; Bill, Eckhard; Ye, Shengfa; Holland, Patrick L.; Chemical Science 14 (2023) 2303–2312; doi:10.1039/D2SC06412J

data_1568447
_publ_section_title
;
 Dynamic effects on ligand field from rapid hydride motion in an iron(ii)
 dimer with an S = 3 ground state
;
_journal_issue                   9
_journal_name_full               'Chemical Science'
_journal_page_first              2303
_journal_page_last               2312
_journal_paper_doi               10.1039/D2SC06412J
_journal_volume                  14
_journal_year                    2023
_chemical_formula_moiety         'C44 H56 Fe2 N4'
_chemical_formula_sum            'C44 H56 Fe2 N4'
_chemical_formula_weight         752.62
_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   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2022-07-13 deposited with the CCDC.	2023-01-18 downloaded from the CCDC.
;
_cell_angle_alpha                103.931(2)
_cell_angle_beta                 93.575(2)
_cell_angle_gamma                116.835(4)
_cell_formula_units_Z            2
_cell_length_a                   11.1005(4)
_cell_length_b                   11.3249(4)
_cell_length_c                   18.9146(4)
_cell_measurement_reflns_used    9966
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      32.12
_cell_measurement_theta_min      2.38
_cell_volume                     2018.76(14)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_molecular_graphics
;
Dolomanov, O.V.; Bourhis, L.J.; Gildea, R.J.; Howard, J.A.K.; Puschmann, H., 
OLEX2: A complete structure solution, refinement and analysis program
(2009). J. Appl. Cryst., 42, 339-341.
;
_computing_publication_material  'SHELXL-2013/2 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT-2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      93(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Rigaku Saturn 944+ CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  confocal
_diffrn_radiation_source         'microfocus rotating anode'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_unetI/netI     0.1260
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            15047
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.670
_diffrn_reflns_theta_min         2.455
_exptl_absorpt_coefficient_mu    6.012
_exptl_absorpt_correction_T_max  0.13661
_exptl_absorpt_correction_T_min  0.04665
_exptl_absorpt_correction_type   sphere
_exptl_absorpt_process_details
; 
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015) 
Spherical absorption correction 
 using equivalent radius and absorption coefficient. 
Empirical absorption correction using spherical harmonics, 
 implemented in SCALE3 ABSPACK scaling algorithm. 
;
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    1.238
_exptl_crystal_description       Needle
_exptl_crystal_F_000             800
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.040
_exptl_crystal_size_rad          0.040
_refine_diff_density_max         0.967
_refine_diff_density_min         -0.596
_refine_diff_density_rms         0.136
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     474
_refine_ls_number_reflns         15047
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0909
_refine_ls_R_factor_gt           0.0708
_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/[\s^2^(Fo^2^)+(0.1498P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2625
_refine_ls_wR_factor_ref         0.2948
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9224
_reflns_number_total             15047
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc06412j2.cif
_cod_data_source_block           007-14051
_cod_depositor_comments
'Adding full bibliography for 1568447--1568450.cif.'
_cod_original_cell_volume        2018.76(13)
_cod_database_code               1568447
_shelx_shelxl_version_number     2014/7
_xtal_radius
;
0.040
;
_shelx_estimated_absorpt_t_min   0.379
_shelx_estimated_absorpt_t_max   0.795
_shelx_res_checksum              79922
_shelx_hkl_checksum              48149