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_7204269
_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            'C30 H42 Cr O9 Si'
_chemical_formula_weight         626.73
_chemical_name_systematic
; 
? 
;
_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                91.132(9)
_cell_angle_beta                 91.211(10)
_cell_angle_gamma                110.571(10)
_cell_formula_units_Z            2
_cell_length_a                   8.3515(13)
_cell_length_b                   10.1419(12)
_cell_length_c                   20.393(2)
_cell_measurement_reflns_used    22
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24.01
_cell_measurement_theta_min      10.57
_cell_volume                     1616.1(4)
_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'
_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  0.0342
_diffrn_reflns_av_sigmaI/netI    0.0570
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -4
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            4781
_diffrn_reflns_theta_max         59.99
_diffrn_reflns_theta_min         4.34
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    3.679
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.5198
_exptl_absorpt_correction_type   'Lamina [0 0 1]'
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.288
_exptl_crystal_description       'platy needles'
_exptl_crystal_F_000             664
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.384
_refine_diff_density_min         -0.239
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.031
_refine_ls_goodness_of_fit_obs   1.088
_refine_ls_matrix_type           full
_refine_ls_number_parameters     403
_refine_ls_number_reflns         4125
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.056
_refine_ls_restrained_S_obs      1.087
_refine_ls_R_factor_all          0.0828
_refine_ls_R_factor_obs          0.0576
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0896P)^2^+0.1521P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1625
_refine_ls_wR_factor_obs         0.1421
_reflns_number_observed          3284
_reflns_number_total             4429
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b108807f.txt
_cod_data_source_block           DW9907
_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^)+(0.0896P)^2^+0.1521P] 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^)+(0.0896P)^2^+0.1521P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C30 H42 O9 Si Cr'
_cod_database_code               7204269