A combined Mössbauer, magnetic circular dichroism, and density functional theory approach for iron cross-coupling catalysis: electronic structure, in situ formation, and reactivity of iron-mesityl-bisphosphines.
Daifuku, Stephanie L.; Al-Afyouni, Malik H; Snyder, Benjamin E. R.; Kneebone, Jared L.; Neidig, Michael L.; Journal of the American Chemical Society 136 (2014) 9132–9143; doi:10.1021/ja503596m

data_4129255
_publ_section_title
;
 A combined M\"ossbauer, magnetic circular dichroism, and density
 functional theory approach for iron cross-coupling catalysis: electronic
 structure, in situ formation, and reactivity of
 iron-mesityl-bisphosphines.
;
_journal_issue                   25
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              9132
_journal_page_last               9143
_journal_paper_doi               10.1021/ja503596m
_journal_volume                  136
_journal_year                    2014
_chemical_formula_moiety         'C71 H99 Br0.80 Cl0.20 Fe P2, C4 H10 O'
_chemical_formula_sum            'C75 H109 Br0.8 Cl0.2 Fe O P2'
_chemical_formula_weight         1215.20
_chemical_name_common            neima05
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                90
_cell_angle_beta                 113.906(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.205(4)
_cell_length_b                   23.705(6)
_cell_length_c                   19.398(5)
_cell_measurement_reflns_used    3825
_cell_measurement_temperature    100.0(5)
_cell_measurement_theta_max      29.84
_cell_measurement_theta_min      2.18
_cell_volume                     7233(3)
_computing_cell_refinement       'SAINT (Bruker, 2013)'
_computing_data_collection       'APEX2 (Bruker, 2013)'
_computing_data_reduction        'SAINT (Bruker, 2013)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SIR2011 (Burla et al., 2012)'
_diffrn_ambient_temperature      100.0(5)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker SMART APEX II CCD platform'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0908
_diffrn_reflns_av_unetI/netI     0.0694
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            127652
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        30.508
_diffrn_reflns_theta_max         31.514
_diffrn_reflns_theta_min         1.590
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.739
_exptl_absorpt_correction_T_max  0.7462
_exptl_absorpt_correction_T_min  0.6449
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2012)'
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.116
_exptl_crystal_description       block
_exptl_crystal_F_000             2617
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.053
_refine_diff_density_min         -0.605
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     767
_refine_ls_number_reflns         24063
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0951
_refine_ls_R_factor_gt           0.0536
_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^)+(0.0593P)^2^+3.1615P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1186
_refine_ls_wR_factor_ref         0.1359
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16070
_reflns_number_total             24063
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja503596m_si_003.cif
_cod_data_source_block           neima05
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_original_formula_sum        'C75 H109 Br0.80 Cl0.20 Fe O P2'
_cod_database_code               4129255
_shelx_estimated_absorpt_t_min   0.777
_shelx_estimated_absorpt_t_max   0.866
_shelxl_version_number           2014-3
_shelx_res_checksum              60302
_shelx_hkl_checksum              80814