Revelation of the Difference between Arylzinc Reagents Prepared from Aryl Grignard and Aryllithium Reagents Respectively: Kinetic and Structural Features
Liqun Jin; Chao Liu; Jing Liu; Fang Hu; Yu Lan; Andrei S. Batsanov; Judith A. K. Howard; Todd B. Marder; Aiwen Lei; Journal of the American Chemical Society 131 (2009) 16656–16657; doi:10.1021/ja908198d

data_4105397
_publ_contact_author             'Andrei S.Batsanov'
_publ_contact_author_email       a.s.batsanov@durham.ac.uk
_publ_section_title
;
 Revelation of the Difference between Arylzinc Reagents Prepared from Aryl
 Grignard and Aryllithium Reagents Respectively: Kinetic and Structural
 Features
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              16656
_journal_page_last               16657
_journal_paper_doi               10.1021/ja908198d
_journal_volume                  131
_journal_year                    2009
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C4 H8 Cl Li O2'
_chemical_formula_sum            'C4 H8 Cl Li O2'
_chemical_formula_weight         130.49
_chemical_name_systematic
; 
 catena-{(\m2-Chloro)-(\m2-dioxane-O,O')-lithium(i)} 
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.1229(4)
_cell_length_b                   7.7500(4)
_cell_length_c                   11.4030(7)
_cell_measurement_reflns_used    5258
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      34.99
_cell_measurement_theta_min      3.18
_cell_volume                     629.47(6)
_computing_cell_refinement       'SAINT version 7.46A (Bruker, 2007)'
_computing_data_collection       'SMART version 5.625 (Bruker, 2001)'
_computing_data_reduction        'SAINT version 7.46A (Bruker, 2007)'
_computing_molecular_graphics    'SHELXTL version 6.14 (Bruker, 2003)'
_computing_publication_material  'SHELXTL version 6.14 (Bruker, 2003)'
_computing_structure_refinement  'SHELXTL version 6.14 (Bruker, 2003)'
_computing_structure_solution    'SHELXTL version 6.14 (Bruker, 2003)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 5.6
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  'Bruker SMART 6K CCD area detector'
_diffrn_measurement_method       '\w 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  0.0230
_diffrn_reflns_av_sigmaI/netI    0.0159
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            14336
_diffrn_reflns_theta_full        35.00
_diffrn_reflns_theta_max         35.00
_diffrn_reflns_theta_min         3.18
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.506
_exptl_absorpt_correction_T_max  0.8623
_exptl_absorpt_correction_T_min  0.6260
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
'SADABS 2006/1 (Bruker), R(int)=0.106 before correction'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.377
_exptl_crystal_description       lump
_exptl_crystal_F_000             272
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.40
_refine_diff_density_max         0.356
_refine_diff_density_min         -0.137
_refine_diff_density_rms         0.050
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     106
_refine_ls_number_reflns         2675
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0211
_refine_ls_R_factor_gt           0.0201
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0332P)^2^+0.0268P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0518
_refine_ls_wR_factor_ref         0.0523
_reflns_Friedel_coverage         0.70
_reflns_number_gt                2592
_reflns_number_total             2675
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ja908198d_si_001_1.cif
_cod_data_source_block           09srv210
_cod_database_code               4105397