Asymmetric Conjugate Nucleophilic Addition of Organolithiums to Chromium (Menthyloxy)(aryl)carbene Complexes
José Barluenga; Andrés A. Trabanco; Josefa Flórez; Santiago García-Granda; Eduardo Martín; Journal of the American Chemical Society 118 (1996) 13099–13100; doi:10.1021/ja962770+

data_4117225
_publ_section_title
;
 Asymmetric Conjugate Nucleophilic Addition of Organolithiums to Chromium
 (Menthyloxy)(aryl)carbene Complexes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              13099
_journal_page_last               13100
_journal_paper_doi               10.1021/ja962770+
_journal_volume                  118
_journal_year                    1996
_chemical_compound_source        synthesis
_chemical_formula_sum            'C28 H38 Cr O7'
_chemical_formula_weight         538.58
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           19
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_symmetry_space_group_name_Hall  'P 2ac 2ab'
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_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     patterson
_atom_sites_solution_secondary   phasex
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.976(5)
_cell_length_b                   14.584(4)
_cell_length_c                   16.913(5)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      20
_cell_measurement_theta_min      15
_cell_volume                     2954.0(17)
_computing_cell_refinement       'DIRDIF (Beurskens, 1992)'
_computing_data_reduction        'REFLEX (Local Program)'
_computing_molecular_graphics    'Xtal_GX (Hall, 1995)'
_computing_publication_material  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Enraf-Nonius CAD-4 diffactometer'
_diffrn_measurement_method       '\w-2\q scan technique'
_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  0.026
_diffrn_reflns_av_sigmaI/netI    0.0674
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       1
_diffrn_reflns_number            4666
_diffrn_reflns_theta_max         24.97
_diffrn_reflns_theta_min         1.84
_diffrn_standards_decay_%        15
_diffrn_standards_interval_count 200
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.427
_exptl_absorpt_correction_T_max  0.62
_exptl_absorpt_correction_T_min  1.00
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.211
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             1144
_exptl_crystal_size_max          .46
_exptl_crystal_size_mid          .46
_exptl_crystal_size_min          .33
_refine_diff_density_max         0.203
_refine_diff_density_min         -0.219
_refine_diff_density_rms         0.042
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.01(2)
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    isotropic
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_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.050
_refine_ls_restrained_S_obs      1.097
_refine_ls_R_factor_all          0.0810
_refine_ls_R_factor_obs          0.0352
_refine_ls_shift/esd_max         -0.611
_refine_ls_shift/esd_mean        0.006
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0298P)^2^+0.3762P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0845
_refine_ls_wR_factor_obs         0.0725
_reflns_number_observed          3282
_reflns_number_total             4666
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja9627702B.cif
_cod_data_source_block           (+)-10
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0298P)^2^+0.3762P] 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^)+(0.0298P)^2^+0.3762P] 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        2953.9(18)
_cod_database_code               4117225