Structural Studies of (rac)-BIPHEN Organomagnesiates and Intermediates in the Halogen–Metal Exchange of 2-Bromopyridine
Francos, Javier; Gros, Philippe C.; Kennedy, Alan R.; O’Hara, Charles T.; Organometallics 34 (2015) 2550–; doi:10.1021/om501225g

data_4085382
_publ_section_title
;
 Structural Studies of (rac)-BIPHEN Organomagnesiates and Intermediates in
 the Halogen--Metal Exchange of 2-Bromopyridine
;
_journal_issue                   11
_journal_name_full               Organometallics
_journal_page_first              2550
_journal_paper_doi               10.1021/om501225g
_journal_volume                  34
_journal_year                    2015
_chemical_formula_sum            'C42 H56 Li2 Mg N2 O4'
_chemical_formula_weight         691.08
_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                 103.285(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.4177(14)
_cell_length_b                   12.3325(8)
_cell_length_c                   20.0058(15)
_cell_measurement_reflns_used    4074
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      28.2871
_cell_measurement_theta_min      3.1494
_cell_volume                     3942.2(5)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.931
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur E'
_diffrn_measurement_method       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  0.0385
_diffrn_reflns_av_sigmaI/netI    0.0571
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            10804
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         27.99
_diffrn_reflns_theta_min         3.16
_exptl_absorpt_coefficient_mu    0.087
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.61675
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   CrysalisPRO
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.164
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'cut plate'
_exptl_crystal_F_000             1488
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.578
_refine_diff_density_min         -0.271
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     236
_refine_ls_number_reflns         4441
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0876
_refine_ls_R_factor_gt           0.0606
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0712P)^2^+3.8689P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1480
_refine_ls_wR_factor_ref         0.1679
_reflns_number_gt                3200
_reflns_number_total             4441
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            om501225g_si_001.cif
_cod_data_source_block           5
_cod_depositor_comments
'Adding full bibliography for 4085378--4085382.cif.'
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               4085382