Preparation of chiral ruthenium(iv) complexes and applications in regio- and enantioselective allylation of phenols.
Sahli, Zeyneb; Derrien, Nolwenn; Pascal, Simon; Demerseman, Bernard; Roisnel, Thierry; Barrière, Frédéric; Achard, Mathieu; Bruneau, Christian; Dalton transactions (Cambridge, England : 2003) 40 (2011) 5625–5630; doi:10.1039/c0dt01812k

data_7015681
_publ_section_title
;
 Preparation of chiral ruthenium(iv) complexes and applications in
 regio- and enantioselective allylation of phenols.
;
_journal_issue                   20
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5625
_journal_page_last               5630
_journal_paper_doi               10.1039/c0dt01812k
_journal_volume                  40
_journal_year                    2011
_chemical_absolute_configuration ad
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         '2(C27 H36 N O2 Ru), 2(F6 P)'
_chemical_formula_sum            'C54 H72 F12 N2 O4 P2 Ru2'
_chemical_formula_weight         1305.22
_chemical_name_systematic
;
?
;
_space_group_IT_number           5
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      5
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 134.2050(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   35.2478(14)
_cell_length_b                   8.9626(4)
_cell_length_c                   24.9400(10)
_cell_measurement_reflns_used    8442
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.44
_cell_measurement_theta_min      2.31
_cell_measurement_wavelength     0.71073
_cell_volume                     5647.9(4)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Altomare et al., 1999)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'APEXII, Bruker-AXS'
_diffrn_measurement_method       'CCD rotation images, thin slices'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0427
_diffrn_reflns_av_unetI/netI     0.0441
_diffrn_reflns_limit_h_max       45
_diffrn_reflns_limit_h_min       -44
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            42236
_diffrn_reflns_theta_full        27.47
_diffrn_reflns_theta_max         27.47
_diffrn_reflns_theta_min         3.42
_exptl_absorpt_coefficient_mu    0.677
_exptl_absorpt_correction_T_max  0.827
_exptl_absorpt_correction_T_min  0.620
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
[Sheldrick, G.M. (2002). SADABS Bruker AXS Inc., Madison, Wisconsin, USA]
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.535
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2672
_exptl_crystal_size_max          0.57
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.28
_platon_squeeze_details
;
;
_refine_diff_density_max         1.209
_refine_diff_density_min         -0.755
_refine_diff_density_rms         0.095
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.03(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.04
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     692
_refine_ls_number_reflns         12429
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.04
_refine_ls_R_factor_all          0.0455
_refine_ls_R_factor_gt           0.0427
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0503P)^2^+20.9699P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1076
_refine_ls_wR_factor_ref         0.1091
_reflns_number_gt                11682
_reflns_number_total             12429
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c0dt01812k.txt
_cod_data_source_block           BD
_cod_original_sg_symbol_H-M      'C 2'
_cod_database_code               7015681