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_4085380
_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 H78 Li2 Mg O5 Si2'
_chemical_formula_weight         781.43
_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                91.832(2)
_cell_angle_beta                 98.917(3)
_cell_angle_gamma                105.629(2)
_cell_formula_units_Z            2
_cell_length_a                   11.1354(3)
_cell_length_b                   12.7861(3)
_cell_length_c                   17.7097(6)
_cell_measurement_reflns_used    6670
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      30.1240
_cell_measurement_theta_min      3.0298
_cell_volume                     2391.69(12)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.942
_diffrn_measured_fraction_theta_max 0.942
_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  0.0311
_diffrn_reflns_av_sigmaI/netI    0.0495
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            20870
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         3.04
_exptl_absorpt_coefficient_mu    0.126
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.66702
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   CrysalisPRO
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.085
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             856
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.382
_refine_diff_density_min         -0.963
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     540
_refine_ls_number_reflns         8851
_refine_ls_number_restraints     116
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.1110
_refine_ls_R_factor_gt           0.0786
_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^)+(0.1067P)^2^+3.3986P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2053
_refine_ls_wR_factor_ref         0.2336
_reflns_number_gt                6106
_reflns_number_total             8851
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            om501225g_si_001.cif
_cod_data_source_block           3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

 Adding full bibliography for 4085378--4085382.cif.
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_cod_database_code               4085380