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_4075589
_publ_section_title
;
 Chiral Ruthenium PNNP Complexes of Non-Enolized 1,3-Dicarbonyl
 Compounds:&#x00A0; Acidity and Involvement in Asymmetric Michael Addition
;
_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         'C58 H50 N3 O2 P2 Ru, P F6, 3(C H2 Cl2)'
_chemical_formula_sum            'C61.01 H52 Cl6 F6 N3 O2 P3 Ru'
_chemical_formula_weight         1379.92
_chemical_name_common            '[Ru(MeC(O)-N-Bn-d-valerolactamato)(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                96.802(2)
_cell_angle_beta                 97.407(2)
_cell_angle_gamma                93.830(2)
_cell_formula_units_Z            2
_cell_length_a                   11.8816(12)
_cell_length_b                   16.0042(17)
_cell_length_c                   16.4275(17)
_cell_measurement_reflns_used    9634
_cell_measurement_temperature    220(2)
_cell_measurement_theta_max      28.004
_cell_measurement_theta_min      2.2435
_cell_volume                     3065.2(6)
_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      220(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_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  0.0299
_diffrn_reflns_av_sigmaI/netI    0.0511
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            25128
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         1.29
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_type              MoK\a
_exptl_absorpt_coefficient_mu    0.659
_exptl_absorpt_correction_T_max  0.9134
_exptl_absorpt_correction_T_min  0.8578
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'sadabs vers. 2.03'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.495
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1400
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.14
_refine_diff_density_max         1.593
_refine_diff_density_min         -1.027
_refine_diff_density_rms         0.119
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     752
_refine_ls_number_reflns         12434
_refine_ls_number_restraints     19
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0848
_refine_ls_R_factor_gt           0.0620
_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^)+(0.1102P)^2^+5.8351P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1739
_refine_ls_wR_factor_ref         0.1924
_reflns_number_gt                9525
_reflns_number_total             12434
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om060389ksi20060508_124227.cif
_cod_data_source_block           5b
_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_original_cell_volume        3065.2(5)
_cod_database_code               4075589