Dilithiation of arenetricarbonylchromium(0) complexes with enantioselective quench: application to chiral biaryl synthesis
Yen-Ling Tan; Andrew J. P. White; David A. Widdowson; René Wilhelm; David J. Williams; J. Chem. Soc., Perkin Trans. 1  (2001) 3269–3280; doi:10.1039/b108807f

data_7204265
_publ_section_title
;
 Dilithiation of arenetricarbonylchromium(0) complexes with
 enantioselective quench: application to chiral biaryl synthesis
;
_journal_issue                   24
_journal_name_full               'J. Chem. Soc., Perkin Trans. 1'
_journal_page_first              3269
_journal_page_last               3280
_journal_paper_doi               10.1039/b108807f
_journal_year                    2001
_chemical_formula_sum            'C9 H11 B O4'
_chemical_formula_weight         193.99
_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
_cell_angle_alpha                109.348(7)
_cell_angle_beta                 98.654(14)
_cell_angle_gamma                95.745(12)
_cell_formula_units_Z            2
_cell_length_a                   5.666(2)
_cell_length_b                   8.4652(10)
_cell_length_c                   10.4672(9)
_cell_measurement_reflns_used    28
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      55.40
_cell_measurement_theta_min      9.15
_cell_volume                     462.21(18)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens SHELXTL'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Siemens P4/RA'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0147
_diffrn_reflns_av_sigmaI/netI    0.0135
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            1662
_diffrn_reflns_theta_max         63.84
_diffrn_reflns_theta_min         4.57
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.897
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Clear
_exptl_crystal_density_diffrn    1.394
_exptl_crystal_description       plates
_exptl_crystal_F_000             204
_exptl_crystal_size_max          0.70
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.202
_refine_diff_density_min         -0.171
_refine_diff_density_rms         0.041
_refine_ls_extinction_coef       0.0782(97)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.077
_refine_ls_goodness_of_fit_obs   1.097
_refine_ls_matrix_type           full
_refine_ls_number_parameters     132
_refine_ls_number_reflns         1449
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.107
_refine_ls_restrained_S_obs      1.096
_refine_ls_R_factor_all          0.0482
_refine_ls_R_factor_obs          0.0429
_refine_ls_shift/esd_max         0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0750P)^2^+0.0839P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1225
_refine_ls_wR_factor_obs         0.1153
_reflns_number_observed          1356
_reflns_number_total             1493
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b108807f.txt
_cod_data_source_block           dw9902
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0750P)^2^+0.0839P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0750P)^2^+0.0839P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        462.23(15)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7204265