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_4085378
_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            'C68 H104 Li4 O9'
_chemical_formula_weight         1093.27
_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                 91.798(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.9337(4)
_cell_length_b                   21.4472(6)
_cell_length_c                   18.7634(4)
_cell_measurement_reflns_used    6602
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      28.9128
_cell_measurement_theta_min      3.1171
_cell_volume                     6408.9(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.950
_diffrn_measurement_device_type  'Oxford Diffraction Xcaibur 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  0.0333
_diffrn_reflns_av_sigmaI/netI    0.0465
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            21498
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         28.00
_diffrn_reflns_theta_min         3.12
_exptl_absorpt_coefficient_mu    0.072
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.89018
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   CrysalisPRO
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.133
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2384
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.294
_refine_diff_density_min         -0.218
_refine_diff_density_rms         0.043
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     413
_refine_ls_number_reflns         7361
_refine_ls_number_restraints     92
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0815
_refine_ls_R_factor_gt           0.0526
_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^)+(0.0487P)^2^+5.5080P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1139
_refine_ls_wR_factor_ref         0.1292
_reflns_number_gt                5316
_reflns_number_total             7361
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            om501225g_si_001.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 4085378--4085382.cif.'
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4085378