Iron/Zinc-Co-catalyzed Directed Arylation and Alkenylation of C(sp3)–H Bonds with Organoborates
Ilies, Laurean; Itabashi, Yuki; Shang, Rui; Nakamura, Eiichi; ACS Catalysis  (2016) 89–; doi:10.1021/acscatal.6b02927

data_4513990
_publ_section_title
;
 Iron/Zinc-Co-catalyzed Directed Arylation and Alkenylation of C(sp3)--H
 Bonds with Organoborates
;
_journal_name_full               'ACS Catalysis'
_journal_page_first              89
_journal_paper_doi               10.1021/acscatal.6b02927
_journal_year                    2016
_chemical_formula_moiety         'C30 H30 O4 P2'
_chemical_formula_sum            'C30 H30 O4 P2'
_chemical_formula_weight         516.48
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 94.688(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   24.0185(9)
_cell_length_b                   5.3968(2)
_cell_length_c                   20.9650(6)
_cell_measurement_reflns_used    10548
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      68.17
_cell_measurement_theta_min      3.70
_cell_volume                     2708.46(16)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Rigaku Rapid II'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54187
_diffrn_reflns_av_R_equivalents  0.1505
_diffrn_reflns_av_unetI/netI     0.3576
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            23601
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        67.687
_diffrn_reflns_theta_max         68.209
_diffrn_reflns_theta_min         3.693
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.727
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.5948
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.267
_exptl_crystal_description       needle
_exptl_crystal_F_000             1088
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.767
_refine_diff_density_min         -0.574
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.887
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     329
_refine_ls_number_reflns         4934
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.887
_refine_ls_R_factor_all          0.2505
_refine_ls_R_factor_gt           0.1068
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1650P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2531
_refine_ls_wR_factor_ref         0.3251
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1546
_reflns_number_total             4934
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs6b02927_si_002.cif
_cod_data_source_block           MeO-dppen
_cod_database_code               4513990
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              926
_shelx_hkl_checksum              68999