Chiral Phosphinooxazoline−Ruthenium(II) and −Osmium(II) Complexes as Catalysts in Diels−Alder Reactions
Carmona, Daniel; Vega, Cristina; García, Néstor; Lahoz, Fernando J.; Elipe, Sergio; Oro, Luis A.; Lamata, M. Pilar; Viguri, Fernando; Borao, Rosana; Organometallics 25 (2006) 1592–; doi:10.1021/om050973d

data_4074888
_publ_section_title
;
 Chiral Phosphinooxazoline&#x2212;Ruthenium(II) and &#x2212;Osmium(II)
 Complexes as Catalysts in Diels&#x2212;Alder Reactions
;
_journal_issue                   7
_journal_name_full               Organometallics
_journal_page_first              1592
_journal_paper_doi               10.1021/om050973d
_journal_volume                  25
_journal_year                    2006
_chemical_absolute_configuration rmad
_chemical_formula_moiety         'C34 H38 F2 N O3 P2 Ru, F6 P'
_chemical_formula_sum            'C34 H38 F8 N O3 P3 Ru'
_chemical_formula_weight         854.63
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 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                 99.5550(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.9134(6)
_cell_length_b                   25.1523(15)
_cell_length_c                   13.8912(8)
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.284
_cell_measurement_theta_min      2.199
_cell_volume                     3415.6(4)
_computing_cell_refinement       'SAINT+ v. 6.22 (Bruker AXS, 2001)'
_computing_data_collection       'SMART v. 5.625 (Bruker AXS, 2001)'
_computing_data_reduction        'SAINT+ v. 6.22 (Bruker AXS, 2001)'
_computing_molecular_graphics    'XP, SHELXTL v. 6.10 (Bruker, 2000)'
_computing_publication_material  'XCIF, SHELXTL v. 6.10 (Bruker, 2000)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.26
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.943
_diffrn_measurement_device_type  'Bruker SMART APEX CCD system'
_diffrn_measurement_method       '\w rotations with narrow frames'
_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  0.0330
_diffrn_reflns_av_sigmaI/netI    0.0684
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            23054
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         28.32
_diffrn_reflns_theta_min         1.49
_diffrn_standards_number         'no decay'
_exptl_absorpt_coefficient_mu    0.681
_exptl_absorpt_correction_T_max  0.914
_exptl_absorpt_correction_T_min  0.850
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; SADABS: Area-Detector Absorption Correction. Bruker-AXS 
  within SAINT+ package, v. 6.22 (2001).
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.662
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1736
_exptl_crystal_size_max          0.247
_exptl_crystal_size_mid          0.143
_exptl_crystal_size_min          0.135
_refine_diff_density_max         0.729
_refine_diff_density_min         -0.376
_refine_diff_density_rms         0.084
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.004(17)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1013
_refine_ls_number_reflns         14908
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.008
_refine_ls_R_factor_all          0.0490
_refine_ls_R_factor_gt           0.0418
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0356P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0828
_refine_ls_wR_factor_ref         0.0863
_reflns_number_gt                13421
_reflns_number_total             14908
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om050973dsi20051111_011930.cif
_cod_data_source_block           compound13
_cod_original_sg_symbol_H-M      P2(1)
_cod_database_code               4074888