Effect of TMEDA on Iron-Catalyzed Coupling Reactions of ArMgX with Alkyl Halides
Daisuke Noda; Yusuke Sunada; Takuji Hatakeyama; Masaharu Nakamura; Hideo Nagashima; Journal of the American Chemical Society 131 (2009) 6078–6079; doi:10.1021/ja901262g

data_4104321
_publ_section_title
;
 Effect of TMEDA on Iron-Catalyzed Coupling Reactions of ArMgX with Alkyl
 Halides
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              6078
_journal_page_last               6079
_journal_paper_doi               10.1021/ja901262g
_journal_volume                  131
_journal_year                    2009
_chemical_absolute_configuration 'CHOOSE rm ad rmad syn or unk'
_chemical_formula_moiety         'C15 H27 Br Fe N2 '
_chemical_formula_sum            'C15 H27 Br Fe N2'
_chemical_formula_weight         371.14
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      33
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_cell_angle_alpha                90.0000
_cell_angle_beta                 90.0000
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   15.405(2)
_cell_length_b                   8.5940(9)
_cell_length_c                   13.0859(16)
_cell_measurement_reflns_used    5990
_cell_measurement_temperature    123.1
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.1
_cell_volume                     1732.4(4)
_computing_cell_refinement       CrystalClear
_computing_data_collection       CrystalClear
_computing_data_reduction        CrystalStructure
_computing_publication_material  'CrystalStructure 3.8'
_computing_structure_refinement  CRYSTALS
_computing_structure_solution    SIR92
_diffrn_detector_area_resol_mean 7.31
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Rigaku Saturn'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.121
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            13035
_diffrn_reflns_theta_full        27.47
_diffrn_reflns_theta_max         27.47
_exptl_absorpt_coefficient_mu    3.174
_exptl_absorpt_correction_T_max  0.565
_exptl_absorpt_correction_T_min  0.286
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.423
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             768.00
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.18
_refine_diff_density_max         2.34
_refine_diff_density_min         -1.25
_refine_ls_abs_structure_details
'Flack, H. D. (1983), Acta Cryst. A39, 876-881.  1819 Friedel Pairs'
_refine_ls_abs_structure_Flack   0.018(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.958
_refine_ls_hydrogen_treatment    refall
_refine_ls_number_parameters     200
_refine_ls_number_reflns         3879
_refine_ls_R_factor_gt           0.0482
_refine_ls_shift/su_max          0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     'w = 1/[1.0000\s(Fo^2^)]/(4Fo^2^)'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1197
_reflns_number_gt                3601
_reflns_number_total             3879
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            ja901262g_si_002.cif
_cod_data_source_block           '__n4e-TMEDAFeMesBr'
_cod_original_cell_volume        1732.5(4)
_cod_original_formula_sum        'C15 H27 Br Fe N2 '
_cod_database_code               4104321