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_4118127
_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         'C60 H48 Cl Fe P4, 2(C4 H8 O)'
_chemical_formula_sum            'C68 H64 Cl Fe O2 P4'
_chemical_formula_weight         1128.37
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 94.248(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   25.3000(10)
_cell_length_b                   25.2876(10)
_cell_length_c                   18.7836(7)
_cell_measurement_reflns_used    9935
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.06
_cell_measurement_theta_min      2.17
_cell_volume                     11984.3(8)
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker Apex II kappa 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  0.0599
_diffrn_reflns_av_sigmaI/netI    0.0545
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            98928
_diffrn_reflns_theta_full        27.52
_diffrn_reflns_theta_max         27.52
_diffrn_reflns_theta_min         1.14
_exptl_absorpt_coefficient_mu    0.447
_exptl_absorpt_correction_T_max  0.2080
_exptl_absorpt_correction_T_min  0.1677
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2008/1'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.251
_exptl_crystal_description       plate
_exptl_crystal_F_000             4728
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.02
_platon_squeeze_details
;
Disordered solvent likely to be two molecules of THF per molecule of complex.
A suitable model could not be obtained.
;
_refine_diff_density_max         0.403
_refine_diff_density_min         -0.376
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.006
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     676
_refine_ls_number_reflns         13772
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.010
_refine_ls_R_factor_all          0.0719
_refine_ls_R_factor_gt           0.0451
_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^)+(0.0740P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1200
_refine_ls_wR_factor_ref         0.1287
_reflns_number_gt                9519
_reflns_number_total             13772
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja303250t_si_001_2.cif
_cod_data_source_block           8a
_cod_database_code               4118127