Iron(II) Active Species in Iron-Bisphosphine Catalyzed Kumada and Suzuki-Miyaura Cross-Couplings of Phenyl Nucleophiles and Secondary Alkyl Halides.
Daifuku, Stephanie L.; Kneebone, Jared L.; Snyder, Benjamin E. R.; Neidig, Michael L.; Journal of the American Chemical Society 137 (2015) 11432–11444; doi:10.1021/jacs.5b06648

data_4129466
_publ_section_title
;
 Iron(II) Active Species in Iron-Bisphosphine Catalyzed Kumada and
 Suzuki-Miyaura Cross-Couplings of Phenyl Nucleophiles and Secondary Alkyl
 Halides.
;
_journal_issue                   35
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              11432
_journal_page_last               11444
_journal_paper_doi               10.1021/jacs.5b06648
_journal_volume                  137
_journal_year                    2015
_chemical_formula_moiety
'0.834(C74 H98 Fe P2), 0.166(C68 H94 Fe P2), 0.166(C6 H14), 0.25(C3 H8 O)'
_chemical_formula_sum            'C74.75 H101.66 Fe O0.25 P2'
_chemical_formula_weight         1122.01
_chemical_name_common            neibs06
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                77.487(3)
_cell_angle_beta                 80.874(3)
_cell_angle_gamma                71.734(3)
_cell_formula_units_Z            4
_cell_length_a                   14.922(3)
_cell_length_b                   21.309(4)
_cell_length_c                   22.714(4)
_cell_measurement_reflns_used    2152
_cell_measurement_temperature    100.0(5)
_cell_measurement_theta_max      17.30
_cell_measurement_theta_min      2.22
_cell_volume                     6663(2)
_computing_cell_refinement       'SAINT (Bruker, 2009)'
_computing_data_collection       'APEX2 (Bruker, 2012)'
_computing_data_reduction        'SAINT (Bruker, 2009)'
_computing_molecular_graphics    'SHELXL-97 (Sheldrick, 2008)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR97 (Altomare et al., 1999)'
_diffrn_ambient_temperature      100.0(5)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker SMART APEX II CCD Platform'
_diffrn_measurement_method       'area detector, \w scans per \f'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.3618
_diffrn_reflns_av_sigmaI/netI    0.3504
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_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            87423
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         1.79
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.315
_exptl_absorpt_correction_T_max  0.9814
_exptl_absorpt_correction_T_min  0.9455
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_crystal_colour            red-purple
_exptl_crystal_density_diffrn    1.118
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2433
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.427
_refine_diff_density_min         -0.448
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.931
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1502
_refine_ls_number_reflns         23523
_refine_ls_number_restraints     44
_refine_ls_restrained_S_all      0.930
_refine_ls_R_factor_all          0.2742
_refine_ls_R_factor_gt           0.0880
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0502P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1455
_refine_ls_wR_factor_ref         0.2103
_reflns_number_gt                7831
_reflns_number_total             23523
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja5b06648_si_002.cif
_cod_data_source_block           neibs06
_cod_original_cell_volume        6664(2)
_cod_database_code               4129466