Base Metal Catalysts for Photochemical C-H Borylation That Utilize Metal-Metal Cooperativity
Thomas J. Mazzacano; Neal P. Mankad; Journal of the American Chemical Society 135 (2013) 17258–17261; doi:10.1021/ja408861p

data_4121162
_publ_contact_author_address
;University of Illinois at Chicago
845 W. Taylor St. MC 111
Chicago, IL 60607
;
_publ_contact_author_email       npm@uic.edu
_publ_contact_author_name        'Neal P. Mankad'
_publ_section_title
;
 Base Metal Catalysts for Photochemical C-H Borylation That Utilize
 Metal-Metal Cooperativity
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              17258
_journal_page_last               17261
_journal_paper_doi               10.1021/ja408861p
_journal_volume                  135
_journal_year                    2013
_chemical_formula_sum            'C36 H46 Fe N2 O2 Zn'
_chemical_formula_weight         659.97
_chemical_name_common            (BDI)ZnFp
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   20.923(2)
_cell_length_b                   14.1629(14)
_cell_length_c                   22.317(2)
_cell_measurement_reflns_used    7359
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      22.89
_cell_measurement_theta_min      2.42
_cell_volume                     6613.2(11)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_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 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w 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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0207
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       0
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            4771
_diffrn_reflns_theta_full        23.31
_diffrn_reflns_theta_max         23.31
_diffrn_reflns_theta_min         1.83
_exptl_absorpt_coefficient_mu    1.197
_exptl_absorpt_correction_T_max  0.8196
_exptl_absorpt_correction_T_min  0.5967
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.326
_exptl_crystal_description       blade
_exptl_crystal_F_000             2784
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.39
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.666
_refine_diff_density_min         -0.186
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     389
_refine_ls_number_reflns         4771
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0378
_refine_ls_R_factor_gt           0.0286
_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^)+(0.0447P)^2^+4.4816P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0714
_refine_ls_wR_factor_ref         0.0766
_reflns_number_gt                4064
_reflns_number_total             4771
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja408861p_si_002.cif
_cod_data_source_block           cnmnm5
_cod_database_code               4121162