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_4085379
_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            'C44 H74 Li2 Mg O5'
_chemical_formula_weight         721.22
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                88.063(3)
_cell_angle_beta                 81.313(4)
_cell_angle_gamma                69.075(4)
_cell_formula_units_Z            2
_cell_length_a                   11.3150(5)
_cell_length_b                   11.6395(5)
_cell_length_c                   18.4418(8)
_cell_measurement_reflns_used    9426
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      71.2670
_cell_measurement_theta_min      4.0710
_cell_volume                     2242.06(18)
_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 0.978
_diffrn_measurement_device_type  'Oxford Diffraction Gemini S'
_diffrn_measurement_method       omega-scans
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0252
_diffrn_reflns_av_sigmaI/netI    0.0333
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            22999
_diffrn_reflns_theta_full        70.00
_diffrn_reflns_theta_max         73.19
_diffrn_reflns_theta_min         4.07
_exptl_absorpt_coefficient_mu    0.637
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.79153
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   CrysalisPRO
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.068
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             792
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.504
_refine_diff_density_min         -0.301
_refine_diff_density_rms         0.047
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     504
_refine_ls_number_reflns         8791
_refine_ls_number_restraints     142
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0842
_refine_ls_R_factor_gt           0.0640
_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^)+(0.0881P)^2^+1.2603P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1734
_refine_ls_wR_factor_ref         0.1883
_reflns_number_gt                6636
_reflns_number_total             8791
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            om501225g_si_001.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 4085378--4085382.cif.'
_cod_original_cell_volume        2242.06(17)
_cod_database_code               4085379