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_4074889
_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         'C42 H42 N O2 P Ru, 2(F6 Sb)'
_chemical_formula_structural
;
 [(C10 H14) Ru (C4 H6 O) (C28 H22 N O P)] [Sb F6]2
;
_chemical_formula_sum            'C42 H42 F12 N O2 P Ru Sb2'
_chemical_formula_weight         1196.32
_chemical_name_systematic
; 
(eta-6-p-cymene){(3aS,8aR)-2-(2-diphenylphosphinophenyl)-3a,8a-
dihydroindane[1,2-d]oxazole}(methacrolein)ruthenium(ii)
bis(hexafluoroantimoniate)
;
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.3401(8)
_cell_length_b                   18.2209(12)
_cell_length_c                   20.7142(13)
_cell_measurement_reflns_used    92
_cell_measurement_temperature    200.0(2)
_cell_measurement_theta_max      19.5
_cell_measurement_theta_min      12.5
_cell_volume                     4280.1(5)
_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, SHELXTL v. 5 (SIEMENS)'
_computing_publication_material  'CIFTAB (Sheldrick, 1993)'
_computing_structure_refinement  'XL, SHELXTL v. 5 (SIEMENS)'
_computing_structure_solution    'SIR92 (Giacovazzo, 1994)'
_diffrn_ambient_temperature      200.0(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'SIEMENS P4'
_diffrn_measurement_method       '\q/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  0.0224
_diffrn_reflns_av_sigmaI/netI    0.0531
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            8444
_diffrn_reflns_theta_full        25.02
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         2.05
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 100
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.729
_exptl_absorpt_correction_T_max  0.977
_exptl_absorpt_correction_T_min  0.530
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details
; 
 Azimuthal psi-scans of 12 reflections at 10\% intervals.
 Data corrected with the program XPREP (SHELXTL v. 5 Bruker)
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.857
_exptl_crystal_density_meas      ?
_exptl_crystal_description       'irregular block'
_exptl_crystal_F_000             2344
_exptl_crystal_size_max          0.69
_exptl_crystal_size_mid          0.48
_exptl_crystal_size_min          0.38
_refine_diff_density_max         0.722
_refine_diff_density_min         -0.747
_refine_diff_density_rms         0.123
_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_all   1.058
_refine_ls_goodness_of_fit_obs   1.031
_refine_ls_hydrogen_treatment    refU
_refine_ls_matrix_type           full
_refine_ls_number_parameters     570
_refine_ls_number_reflns         7508
_refine_ls_number_restraints     72
_refine_ls_restrained_S_all      1.090
_refine_ls_restrained_S_obs      1.040
_refine_ls_R_factor_all          0.0636
_refine_ls_R_factor_obs          0.0431
_refine_ls_shift/esd_max         -0.009
_refine_ls_shift/esd_mean        0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0287P)^2^+16.21260P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0950
_refine_ls_wR_factor_obs         0.0817
_reflns_number_observed          6232
_reflns_number_total             7521
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            om050973dsi20051111_012123.cif
_cod_data_source_block           compound15a'
_cod_depositor_comments
;
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_Hall     'P 2ac 2ab''
_cod_database_code               4074889