Alkali Metal Cation Effects for Rapid C–H Activation by Iron(0) Complexes
Hidalgo, Nereida; Southwell, Kendal W.; Donnelly, Ryan; Mercado, Brandon Q.; Krajewski, Sebastian M.; Wang, Xiaoping; Holland, Patrick L.; Chemical Science  (2026) –; doi:10.1039/D6SC01470D

data_1576989
_publ_section_title
;
 Alkali metal cation effects for rapid C-H activation by iron(0)
 complexes.
;
_journal_issue                   20
_journal_name_full               'Chemical science'
_journal_page_first              10061
_journal_page_last               10066
_journal_paper_doi               10.1039/d6sc01470d
_journal_volume                  17
_journal_year                    2026
_chemical_formula_sum            'C70 H94 Cs2 Fe2 N4'
_chemical_formula_weight         1369.01
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2019/3
_audit_update_record
;
2025-12-08 deposited with the CCDC.	2026-03-31 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.0400(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.59130(10)
_cell_length_b                   18.90890(10)
_cell_length_c                   15.32260(10)
_cell_measurement_reflns_used    1377
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      75.449
_cell_measurement_theta_min      7.587
_cell_volume                     3325.38(4)
_computing_cell_refinement       'TOPAZ Mantid Python Program'
_computing_data_collection       'SNS EPICS'
_computing_data_reduction        'TOPAZ Mantid Python Program'
_computing_structure_refinement  'SHELXL-2019/2 (Sheldrick, 2019)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.145
_diffrn_measured_fraction_theta_max 0.141
_diffrn_measurement_device_type  TOPAZ
_diffrn_measurement_method       'time-of-flight Laue'
_diffrn_radiation_type           neutrons
_diffrn_radiation_wavelength     1.0
_diffrn_radiation_wavelength_details 'Based on neutron time of flight'
_diffrn_reflns_av_R_equivalents  0.2079
_diffrn_reflns_av_unetI/netI     0.5557
_diffrn_reflns_Laue_measured_fraction_full 0.145
_diffrn_reflns_Laue_measured_fraction_max 0.141
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            2128
_diffrn_reflns_point_group_measured_fraction_full 0.145
_diffrn_reflns_point_group_measured_fraction_max 0.141
_diffrn_reflns_theta_full        36.870
_diffrn_reflns_theta_max         76.540
_diffrn_reflns_theta_min         7.568
_diffrn_source                   'The ORNL Spallation Neutron Source'
_exptl_absorpt_coefficient_mu    0.2555
_exptl_absorpt_correction_T_max  0.9241
_exptl_absorpt_correction_T_min  0.8031
_exptl_absorpt_correction_type   sphere
_exptl_absorpt_process_details
; 
C. W. Dwiggins, Jr., Acta Cryst. A31, 395 (1975).
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.367
_exptl_crystal_description       plate
_exptl_crystal_F_000             1408
_exptl_crystal_size_max          0.360
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.765
_refine_diff_density_min         -0.728
_refine_diff_density_rms         0.186
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.930
_refine_ls_hydrogen_treatment    refU
_refine_ls_matrix_type           full
_refine_ls_number_parameters     34
_refine_ls_number_reflns         874
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      0.927
_refine_ls_R_factor_all          0.1250
_refine_ls_R_factor_gt           0.0970
_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^)+(0.0476P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1945
_refine_ls_wR_factor_ref         0.2081
_reflns_Friedel_coverage         0.000
_reflns_number_gt                516
_reflns_number_total             874
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d6sc01470d2.cif
_cod_data_source_block           CsLFePhH_neutron
_cod_depositor_comments
'Adding full bibliography for 1576987--1576994.cif.'
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               1576989
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_min   0.967
_shelx_estimated_absorpt_t_max   0.994
_exptl_absorpt_special_details
; 
Neutron linear absorption coefficient is wavelength dependent.
For each peak, the absorption coefficient mu is calculated as:
          mu = 1.4447 + 1.9965/1.7982 * wavelength  [cm^-1^]
where 
 1.4447 cm^-1 is the absorption coefficient for total scattering;
 1.9965 cm^-1 is the absorption coefficient for true absorption at 1.7982 A.
 
The value of 0.2555 (mm^-1^) shown in _exptl_absorpt_coefficient_mu 
is the sample absorption coefficient for neutron wavelength at 1.0 \%A.
;
_shelx_res_checksum              88340