Catalytic, asymmetric Michael reactions of cyclic diketones with beta,gamma-unsaturated alpha-ketoesters.
Calter, Michael A.; Wang, Jun; Organic letters 11 (2009) 2205–2208; doi:10.1021/ol900586f

data_1503904
_publ_section_title
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 Catalytic, asymmetric Michael reactions of cyclic diketones with
 beta,gamma-unsaturated alpha-ketoesters.
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_journal_issue                   10
_journal_name_full               'Organic letters'
_journal_page_first              2205
_journal_page_last               2208
_journal_paper_doi               10.1021/ol900586f
_journal_volume                  11
_journal_year                    2009
_chemical_absolute_configuration ad
_chemical_formula_sum            'C20 H23 Br O5'
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_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
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_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
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_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.795(2)
_cell_length_b                   12.833(3)
_cell_length_c                   13.549(3)
_cell_measurement_temperature    173(2)
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_computing_cell_refinement       Denzo
_computing_data_collection       'Nonius Collect'
_computing_data_reduction        Denzo
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
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_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
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_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
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_diffrn_reflns_theta_max         28.94
_diffrn_reflns_theta_min         3.40
_exptl_absorpt_coefficient_mu    2.218
_exptl_absorpt_correction_T_max  0.7321
_exptl_absorpt_correction_T_min  0.7321
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.498
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             872
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_exptl_crystal_size_mid          0.15
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_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
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_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0350P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0716
_refine_ls_wR_factor_ref         0.0799
_reflns_number_gt                3556
_reflns_number_total             4732
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ol900586f_si_001.cif
_cod_data_source_block           mc01
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        1877.1(7)
_cod_original_sg_symbol_H-M      P2(1)2(1)2(1)
_cod_database_code               1503904