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_4074887
_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 H40 N O2 P Ru 2+, 2(C F3 O3 S 1-)'
_chemical_formula_sum            'C36 H40 F6 N O8 P Ru S2'
_chemical_formula_weight         924.85
_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                 94.730(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.3493(15)
_cell_length_b                   10.9548(16)
_cell_length_c                   17.044(2)
_cell_measurement_reflns_used    12933
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      29.50
_cell_measurement_theta_min      2.32
_cell_volume                     1925.8(5)
_computing_cell_refinement       'SAINT+ v. 7.06a (Bruker AXS, 2003)'
_computing_data_collection       'SMART v. 5.630 (Bruker AXS, 2003)'
_computing_data_reduction        'SAINT+ v. 7.06a (Bruker AXS, 2003)'
_computing_molecular_graphics    'XP program, SHELXTL v6.12, Bruker2000'
_computing_publication_material  'XCIF program, SHELXTLv6.12, BrukerAXS'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Giacovazzo, 1999)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 8.26
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.901
_diffrn_measurement_device_type  'BrukerAXS SMART APEX2 CCD diffractometer'
_diffrn_measurement_method       '\w rotations with narrow frames'
_diffrn_radiation_monochromator  'Silicon 111'
_diffrn_radiation_source         'Daresbury SRS Station 9.8'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.6894
_diffrn_reflns_av_R_equivalents  0.0261
_diffrn_reflns_av_sigmaI/netI    0.0452
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            16037
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         30.57
_diffrn_reflns_theta_min         2.21
_diffrn_standards_decay_%        'no decay'
_exptl_absorpt_coefficient_mu    0.638
_exptl_absorpt_correction_T_max  0.9874
_exptl_absorpt_correction_T_min  0.9390
_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            orange
_exptl_crystal_density_diffrn    1.595
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             944
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.008
_refine_diff_density_min         -0.492
_refine_diff_density_rms         0.106
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.017(19)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     582
_refine_ls_number_reflns         10002
_refine_ls_number_restraints     58
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0363
_refine_ls_R_factor_gt           0.0347
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0582P)^2^+0.3766P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0897
_refine_ls_wR_factor_ref         0.0909
_reflns_number_gt                9604
_reflns_number_total             10002
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om050973dsi20051111_011910.cif
_cod_data_source_block           compound7c
_cod_original_sg_symbol_H-M      P21
_cod_database_code               4074887