Chiral Ruthenium PNNP Complexes of Non-Enolized 1,3-Dicarbonyl Compounds: Acidity and Involvement in Asymmetric Michael Addition
Althaus, Martin; Bonaccorsi, Cristina; Mezzetti, Antonio; Santoro, Francesco; Organometallics 25 (2006) 3108–; doi:10.1021/om060389k

data_4075588
_publ_section_title
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 Chiral Ruthenium PNNP Complexes of Non-Enolized 1,3-Dicarbonyl
 Compounds:&#x00A0; Acidity and Involvement in Asymmetric Michael Addition
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_journal_issue                   13
_journal_name_full               Organometallics
_journal_page_first              3108
_journal_paper_doi               10.1021/om060389k
_journal_volume                  25
_journal_year                    2006
_chemical_formula_moiety         'C54 H55 F6 N2 O3 P3 Ru1'
_chemical_formula_sum            'C110.22 H110 Cl4.51 F12 N4 O6 P6 Ru2'
_chemical_formula_weight         2362.38
_chemical_name_common            '[Ru(2-t-BuOOC-cyclopentanonato)(PNNP)]PF6'
_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                78.0510(10)
_cell_angle_beta                 74.0360(10)
_cell_angle_gamma                79.2880(10)
_cell_formula_units_Z            2
_cell_length_a                   14.9279(11)
_cell_length_b                   16.6872(12)
_cell_length_c                   23.5871(17)
_cell_measurement_reflns_used    25973
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      28.3705
_cell_measurement_theta_min      2.519
_cell_volume                     5474.5(7)
_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 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'BRUKER APEX'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0265
_diffrn_reflns_av_sigmaI/netI    0.0360
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            49537
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         1.72
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_type              MoK\a
_exptl_absorpt_coefficient_mu    0.549
_exptl_absorpt_correction_T_max  0.8842
_exptl_absorpt_correction_T_min  0.6679
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'sadabs vers. 2.03'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.433
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2420
_exptl_crystal_size_max          0.80
_exptl_crystal_size_mid          0.42
_exptl_crystal_size_min          0.23
_refine_diff_density_max         2.254
_refine_diff_density_min         -0.726
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1351
_refine_ls_number_reflns         22319
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0573
_refine_ls_R_factor_gt           0.0497
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0743P)^2^+9.4397P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1364
_refine_ls_wR_factor_ref         0.1418
_reflns_number_gt                19304
_reflns_number_total             22319
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om060389ksi20060508_124227.cif
_cod_data_source_block           5a
_cod_depositor_comments
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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 
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_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4075588