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_4129252
_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         'C80 H110 Fe P2'
_chemical_formula_sum            'C80 H110 Fe P2'
_chemical_formula_weight         1189.46
_chemical_name_common            neima07
_space_group_crystal_system      tetragonal
_space_group_IT_number           86
_space_group_name_Hall           '-P 4bc'
_space_group_name_H-M_alt        'P 42/n :2'
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.837(3)
_cell_length_b                   19.837(3)
_cell_length_c                   21.423(3)
_cell_measurement_reflns_used    3920
_cell_measurement_temperature    100.0(5)
_cell_measurement_theta_max      27.39
_cell_measurement_theta_min      2.39
_cell_volume                     8430(2)
_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 0.998
_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  0.0809
_diffrn_reflns_av_unetI/netI     0.0274
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            166415
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        27.485
_diffrn_reflns_theta_max         27.490
_diffrn_reflns_theta_min         1.399
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.251
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6519
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2012)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    0.937
_exptl_crystal_description       block
_exptl_crystal_F_000             2584
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.16
_platon_squeeze_details
;
TITL neima07 in P4(2)/n 
CELL   19.8370   19.8370   21.4230     90.00     90.00     90.00 
SPGR P42/n 
C101 0.249 0.250 0.750 !       1.79 eA-3 
C102 0.299 0.263 0.750 !       1.70 eA-3 
C103 0.045 0.268 0.289 !       1.70 eA-3 
C104 0.128 0.347 0.752 !       1.68 eA-3 
C105 0.252 0.250 0.359 !       1.62 eA-3 
C106 0.741 0.516 0.767 !       1.58 eA-3 
C107 0.237 0.192 0.749 !       1.58 eA-3 
C108 0.146 0.278 0.335 !       1.42 eA-3 
C109 0.277 0.405 0.216 !       1.38 eA-3 
C110 0.685 0.715 0.674 !       1.36 eA-3 
Q111 0.626 0.185 0.382 !       1.21 eA-3 
Q112 0.742 0.453 0.812 !       1.16 eA-3 
Q113 0.932 0.314 0.337 !       1.10 eA-3 
C114 0.710 0.811 0.662 !       1.06 eA-3 
Q115 0.419 0.700 0.678 !       1.01 eA-3 
Q116 0.663 0.236 0.395 !       0.95 eA-3 
Q117 0.673 0.374 0.374 !       0.87 eA-3 
C118 0.337 0.250 0.163 !       0.81 eA-3 
C119 0.206 0.341 0.211 !       0.73 eA-3 
C120 0.323 0.361 0.237 !       0.72 eA-3 
C121 0.775 0.610 0.764 !       0.70 eA-3 
C122 0.842 0.685 0.704 !       0.69 eA-3 
C123 0.239 0.345 0.290 !       0.67 eA-3 
Q124 0.647 0.110 0.404 !       0.64 eA-3 
C125 0.342 0.311 0.240 !       0.63 eA-3 
C126 0.672 0.795 0.764 !       0.60 eA-3 
C127 0.699 0.706 0.791 !       0.60 eA-3 
Q128 0.015 0.296 0.565 !       0.58 eA-3 
Q129 0.549 0.409 0.188 !       0.57 eA-3 
C130 0.142 0.280 0.184 !       0.56 eA-3 
Q131 0.066 0.219 0.751 !       0.53 eA-3 
Q132 0.407 0.264 0.985 !       0.52 eA-3 
;
_refine_diff_density_max         1.151
_refine_diff_density_min         -0.325
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     416
_refine_ls_number_reflns         9657
_refine_ls_number_restraints     14
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0828
_refine_ls_R_factor_gt           0.0613
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0940P)^2^+8.5105P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1666
_refine_ls_wR_factor_ref         0.1845
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7411
_reflns_number_total             9657
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja503596m_si_005.cif
_cod_data_source_block           neima07
_cod_original_sg_symbol_H-M      'P 42/n'
_cod_database_code               4129252
_shelx_estimated_absorpt_t_min   0.951
_shelx_estimated_absorpt_t_max   0.961
_shelxl_version_number           2014-3
_shelx_res_checksum              1584
_shelx_hkl_checksum              68850
_shelx_fab_checksum              36470