Asymmetric Diels-Alder Reactions of Unsaturated β-Ketoesters Catalyzed by Chiral Ruthenium PNNP Complexes
Christoph Schotes; Antonio Mezzetti; Journal of the American Chemical Society 132 (2010) 3652–3653; doi:10.1021/ja910039e

data_4102122
_publ_section_title
;
 Asymmetric Diels-Alder Reactions of Unsaturated \b-Ketoesters Catalyzed
 by Chiral Ruthenium PNNP Complexes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              3652
_journal_page_last               3653
_journal_paper_doi               10.1021/ja910039e
_journal_volume                  132
_journal_year                    2010
_chemical_absolute_configuration rm
_chemical_formula_moiety         'C56 H58 Cl4 F12 N2 O3 P4 Ru'
_chemical_formula_sum            'C56 H58 Cl4 F12 N2 O3 P4 Ru'
_chemical_formula_weight         1401.79
_chemical_name_common            '[Ru(3a)(PNNP)](PF6)2'
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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-97
_cell_angle_alpha                96.8860(10)
_cell_angle_beta                 93.7550(10)
_cell_angle_gamma                113.0850(10)
_cell_formula_units_Z            2
_cell_length_a                   11.5110(7)
_cell_length_b                   13.8903(8)
_cell_length_c                   20.6616(12)
_cell_measurement_reflns_used    5145
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      28.19
_cell_measurement_theta_min      2.19
_cell_volume                     2994.2(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_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      200(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'BRUKER APEX'
_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  0.0252
_diffrn_reflns_av_sigmaI/netI    0.0371
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            26500
_diffrn_reflns_theta_full        26.02
_diffrn_reflns_theta_max         26.02
_diffrn_reflns_theta_min         1.00
_exptl_absorpt_coefficient_mu    0.630
_exptl_absorpt_correction_T_max  0.9060
_exptl_absorpt_correction_T_min  0.7221
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'Sadabs vers. 2.03'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.555
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1424
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.260
_refine_diff_density_min         -0.758
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     739
_refine_ls_number_reflns         11770
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0559
_refine_ls_R_factor_gt           0.0504
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0705P)^2^+5.0946P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1290
_refine_ls_wR_factor_ref         0.1337
_reflns_number_gt                10527
_reflns_number_total             11770
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja910039e_si_003.cif
_cod_data_source_block           MA_C_40_3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_database_code               4102122