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_4074884
_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 Cl N O P Ru +, F6 Sb -'
_chemical_formula_sum            'C34 H38 Cl F6 N O P Ru Sb'
_chemical_formula_weight         879.89
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.8061(5)
_cell_length_b                   14.6680(8)
_cell_length_c                   27.1709(17)
_cell_measurement_reflns_used    42
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      15
_cell_measurement_theta_min      12.5
_cell_volume                     3509.6(4)
_computing_cell_refinement       'XSCANS v. 2.1 (Siemens)'
_computing_data_collection       'XSCANS v. 2.1 (Siemens)'
_computing_data_reduction        'XSCANS v. 2.1 (Siemens)'
_computing_molecular_graphics    'XP program, SHELXTL v6.10,Bruker2000'
_computing_publication_material  'XCIF program, SHELXTL v6.10,Bruker'
_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  'four circle diffractometer,Siemens P4'
_diffrn_measurement_method       '\w/2\q 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  0.0093
_diffrn_reflns_av_sigmaI/netI    0.0178
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            7742
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         2.04
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 100
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.382
_exptl_absorpt_correction_T_max  0.700
_exptl_absorpt_correction_T_min  0.542
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details
; 
 Azimuthal psi-scans of 14 reflections at 10\% intervals.
 Data corrected with the program XPREP (SHELXTL v. 5 Bruker)
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.665
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'irregular block'
_exptl_crystal_F_000             1752
_exptl_crystal_size_max          0.372
_exptl_crystal_size_mid          0.291
_exptl_crystal_size_min          0.260
_refine_diff_density_max         0.669
_refine_diff_density_min         -0.613
_refine_diff_density_rms         0.079
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.03(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     536
_refine_ls_number_reflns         6866
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0356
_refine_ls_R_factor_gt           0.0321
_refine_ls_shift/su_max          0.024
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0454P)^2^+4.6528P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0793
_refine_ls_wR_factor_ref         0.0813
_reflns_number_gt                6456
_reflns_number_total             6866
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om050973dsi20051111_011753.cif
_cod_data_source_block           compound1a
_cod_original_sg_symbol_Hall     'P 2ac 2ab''
_cod_original_sg_symbol_H-M      P212121
_cod_database_code               4074884