Iron-Catalyzed Borylation of Alkyl, Allyl, and Aryl Halides: Isolation of an Iron(I) Boryl Complex
Bedford, Robin B.; Brenner, Peter B.; Carter, Emma; Gallagher, Timothy; Murphy, Damien M.; Pye, Dominic R.; Organometallics 33 (2014) 5940–; doi:10.1021/om500847j

data_4084544
_publ_section_title
;
 Iron-Catalyzed Borylation of Alkyl, Allyl, and Aryl Halides: Isolation of
 an Iron(I) Boryl Complex
;
_journal_issue                   21
_journal_name_full               Organometallics
_journal_page_first              5940
_journal_paper_doi               10.1021/om500847j
_journal_volume                  33
_journal_year                    2014
_chemical_formula_moiety         'C66 H60 B Fe O2 P4'
_chemical_formula_sum            'C66 H60 B Fe O2 P4'
_chemical_formula_weight         1075.68
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_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     iterative
_audit_creation_date             2014-07-01
_audit_creation_method
;
Olex2 1.2
(compiled 2014.06.27 svn.r2953 for OlexSys, GUI svn.r4855)
;
_cell_angle_alpha                90
_cell_angle_beta                 104.589(16)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.065(7)
_cell_length_b                   24.029(14)
_cell_length_c                   19.407(12)
_cell_measurement_reflns_used    9904
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      66.96
_cell_measurement_theta_min      3.67
_cell_volume                     5445(6)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2013)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0380
_diffrn_reflns_av_unetI/netI     0.0302
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            25884
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         67.069
_diffrn_reflns_theta_min         3.679
_exptl_absorpt_coefficient_mu    3.684
_exptl_absorpt_correction_T_max  0.7529
_exptl_absorpt_correction_T_min  0.3772
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.312
_exptl_crystal_description       needle
_exptl_crystal_F_000             2252
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.603
_refine_diff_density_min         -0.464
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     337
_refine_ls_number_reflns         4810
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0332
_refine_ls_R_factor_gt           0.0330
_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^)+(0.0481P)^2^+6.7956P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0868
_refine_ls_wR_factor_ref         0.0870
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4785
_reflns_number_total             4810
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om500847j_si_002.cif
_cod_data_source_block           test
_cod_depositor_comments          'Adding full bibliography for 4084544.cif.'
_cod_database_code               4084544
_shelxl_version_number           2013-4
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C24(H24), C8(H8), C18(H18), C30(H30), C11(H11), C23(H23), C29(H29), C16(H16),
 C20(H20), C3(H3), C17(H17), C26(H26), C2(H2), C22(H22), C6(H6), C14(H14),
 C15(H15), C27(H27), C28(H28), C10(H10), C4(H4), C9(H9), C5(H5), C21(H21)
2.b Idealised Me refined as rotating group:
 C34(H34A,H34B,H34C), C35(H35A,H35B,H35C)
;
_shelx_res_checksum              22579
_shelx_hkl_checksum              88131
_olex2_submission_special_instructions 'No special instructions were received'