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_1568449
_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 H54.15 D1.85 Fe2 N4, C7 H8'
_chemical_formula_sum            'C51 H62.15 D1.85 Fe2 N4'
_chemical_formula_weight         846.62
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2019-07-12 deposited with the CCDC.	2023-01-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.329(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.8009(5)
_cell_length_b                   10.9639(4)
_cell_length_c                   17.4087(7)
_cell_measurement_reflns_used    17321
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      78.74
_cell_measurement_theta_min      7.31
_cell_volume                     2245.98(16)
_computing_cell_refinement       Mantidplot
_computing_data_collection       'SNS PyDas'
_computing_data_reduction        'Mantidplot and ANVRED3'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.941
_diffrn_measured_fraction_theta_max 0.925
_diffrn_measurement_device_type  TOPAZ
_diffrn_measurement_method       'time-of-flight Laue'
_diffrn_radiation_type           neutrons
_diffrn_radiation_wavelength     0.6
_diffrn_radiation_wavelength_details 'Based on neutron time of flight'
_diffrn_reflns_av_unetI/netI     0.0982
_diffrn_reflns_Laue_measured_fraction_full 0.941
_diffrn_reflns_Laue_measured_fraction_max 0.925
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            23195
_diffrn_reflns_point_group_measured_fraction_full 0.873
_diffrn_reflns_point_group_measured_fraction_max 0.850
_diffrn_reflns_theta_full        25.214
_diffrn_reflns_theta_max         78.445
_diffrn_reflns_theta_min         7.410
_diffrn_source                   'The ORNL Spallation Neutron Scource'
_exptl_absorpt_coefficient_mu    0.2533
_exptl_absorpt_correction_T_max  0.8684
_exptl_absorpt_correction_T_min  0.6445
_exptl_absorpt_correction_type   sphere
_exptl_absorpt_process_details
; 
C. W. Dwiggins, Jr., Acta Cryst. A31, 395 (1975).
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.252
_exptl_crystal_description       prism
_exptl_crystal_F_000             1248
_exptl_crystal_size_max          2.040
_exptl_crystal_size_mid          0.720
_exptl_crystal_size_min          0.700
_refine_diff_density_max         1.067
_refine_diff_density_min         -1.241
_refine_diff_density_rms         0.146
_refine_ls_abs_structure_details
;
 All f" are zero, so absolute structure could not be determined
;
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1098
_refine_ls_number_reflns         23195
_refine_ls_number_restraints     254
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0689
_refine_ls_R_factor_gt           0.0642
_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^)+(0.0363P)^2^+18.3075P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1228
_refine_ls_wR_factor_ref         0.1261
_reflns_Friedel_coverage         0.744
_reflns_Friedel_fraction_full    0.796
_reflns_Friedel_fraction_max     0.766
_reflns_number_gt                21555
_reflns_number_total             23195
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc06412j2.cif
_cod_data_source_block           FeD
_cod_depositor_comments
'Adding full bibliography for 1568447--1568450.cif.'
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               1568449
_shelx_shelxl_version_number     2014/7
_exptl_absorpt_special_details
; 
Neutron linear absorption coefficient is wavelength dependent.
For each peak, the absorption coefficient mu is calculated as:
          mu = 1.4650 + 1.9200/1.7982 * wavelength  [cm^-1^]
where 
 1.4650 cm^-1 is the absorption coefficient for total scattering;
 1.9200 cm^-1 is the absorption coefficient for true absorption at 1.7982 A.
 
The value of 0.2533 (mm^-1^) shown in _exptl_absorpt_coefficient_mu 
is the sample absorption coefficient for neutron wavelength at 1.0 \%A.
;
_shelx_res_checksum              55444
_shelx_hkl_checksum              14834