Iron(I) in Negishi Cross-Coupling Reactions
Christopher J. Adams; Robin B. Bedford; Emma Carter; Nicholas J. Gower; Mairi F. Haddow; Jeremy N. Harvey; Michael Huwe; M. Ángeles Cartes; Stephen M. Mansell; Carla Mendoza; Damien M. Murphy; Emily C. Neeve; Joshua Nunn; Journal of the American Chemical Society 134 (2012) 10333–10336; doi:10.1021/ja303250t

data_4118126
_publ_section_title
;
 Iron(I) in Negishi Cross-Coupling Reactions
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10333
_journal_page_last               10336
_journal_paper_doi               10.1021/ja303250t
_journal_volume                  134
_journal_year                    2012
_chemical_formula_moiety         'C71 H61 Fe O P4, 0.5(C7 H8)'
_chemical_formula_sum            'C74.5 H69 Fe O P4'
_chemical_formula_weight         1160.03
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_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                71.056(3)
_cell_angle_beta                 75.038(3)
_cell_angle_gamma                67.531(3)
_cell_formula_units_Z            2
_cell_length_a                   13.4958(11)
_cell_length_b                   14.3753(12)
_cell_length_c                   17.9042(17)
_cell_measurement_reflns_used    9934
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.37
_cell_measurement_theta_min      2.23
_cell_volume                     3000.0(5)
_computing_cell_refinement       'Bruker Apex II'
_computing_data_collection       'Bruker Apex II'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker ShelXTL'
_computing_publication_material  'Bruker ShelXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0381
_diffrn_reflns_av_sigmaI/netI    0.0443
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            42267
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.22
_exptl_absorpt_coefficient_mu    0.404
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6462
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V20081/'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.284
_exptl_crystal_description       block
_exptl_crystal_F_000             1220
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.648
_refine_diff_density_min         -0.483
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     750
_refine_ls_number_reflns         13722
_refine_ls_number_restraints     43
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0621
_refine_ls_R_factor_gt           0.0415
_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^)+(0.0576P)^2^+1.3033P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1034
_refine_ls_wR_factor_ref         0.1169
_reflns_number_gt                10583
_reflns_number_total             13722
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja303250t_si_001_1.cif
_cod_data_source_block           7
_cod_original_sg_symbol_Hall     -P1
_cod_original_formula_sum        'C74.50 H69 Fe O P4'
_cod_database_code               4118126