Acidic Ruthenium PNNP Complexes of Non-enolized 1,3-Dicarbonyl Compounds as Catalysts for Asymmetric Michael Addition
Santoro, Francesco; Althaus, Martin; Bonaccorsi, Cristina; Gischig, Sebastian; Mezzetti, Antonio; Organometallics 27 (2008) 3866–; doi:10.1021/om800197y

data_4071504
_publ_section_title
;
 Acidic Ruthenium PNNP Complexes of Non-enolized 1,3-Dicarbonyl Compounds
 as Catalysts for Asymmetric Michael Addition
;
_journal_issue                   15
_journal_name_full               Organometallics
_journal_page_first              3866
_journal_paper_doi               10.1021/om800197y
_journal_volume                  27
_journal_year                    2008
_chemical_absolute_configuration rm
_chemical_formula_moiety         'C53 H54 B F10 N2 O3 P3 Ru, C H2 Cl2'
_chemical_formula_sum            'C54 H56 B Cl2 F10 N2 O3 P3 Ru'
_chemical_formula_weight         1246.70
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 92.7020(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.0460(5)
_cell_length_b                   20.6031(9)
_cell_length_c                   20.3481(9)
_cell_measurement_reflns_used    5616
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      25.48
_cell_measurement_theta_min      2.60
_cell_volume                     5044.5(4)
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0385
_diffrn_reflns_av_sigmaI/netI    0.0348
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            44016
_diffrn_reflns_theta_full        26.03
_diffrn_reflns_theta_max         26.03
_diffrn_reflns_theta_min         1.41
_exptl_absorpt_coefficient_mu    0.598
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.642
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       cube
_exptl_crystal_F_000             2544
_exptl_crystal_size_max          0.475
_exptl_crystal_size_mid          0.475
_exptl_crystal_size_min          0.321
_refine_diff_density_max         0.921
_refine_diff_density_min         -0.466
_refine_diff_density_rms         0.108
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.115
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     736
_refine_ls_number_reflns         9948
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.179
_refine_ls_R_factor_all          0.0631
_refine_ls_R_factor_gt           0.0545
_refine_ls_shift/su_max          0.012
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0892P)^2^+5.6361P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1548
_refine_ls_wR_factor_ref         0.1606
_reflns_number_gt                8604
_reflns_number_total             9948
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om800197y-file021.cif
_cod_data_source_block           6
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 

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_sg_symbol_H-M      'P 21/n'
_cod_database_code               4071504