Chiral pyridylamino-ruthenium(ii) complexes: synthesis, structure and catalytic properties in Diels‒Alder reactions
Carmona, Daniel; Lamata, M. Pilar; Viguri, Fernando; Rodríguez, Ricardo; Lahoz, Fernando J.; Dobrinovitch, Isabel T.; Oro, Luis A.; Dalton Transactions  (2008) 3328–3338; doi:10.1039/B802381F

data_7004074
_publ_section_title
;
 Chiral pyridylamino-ruthenium(ii) complexes: synthesis, structure and
 catalytic properties in Diels--Alder reactions
;
_journal_issue                   25
_journal_name_full               'Dalton Transactions'
_journal_page_first              3328
_journal_page_last               3338
_journal_paper_doi               10.1039/B802381F
_journal_year                    2008
_chemical_absolute_configuration rmad
_chemical_formula_moiety
'C26 H40 N2 O Ru, C4 H10 O, 2(F6 Sb), C H2 Cl2'
_chemical_formula_sum            'C31 H52 Cl2 F12 N2 O2 Ru Sb2'
_chemical_formula_weight         1128.22
_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                   10.395(3)
_cell_length_b                   11.073(3)
_cell_length_c                   36.007(9)
_cell_measurement_reflns_used    3337
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      21.19
_cell_measurement_theta_min      2.26
_cell_volume                     4144.5(19)
_computing_cell_refinement       'SAINT+ v. 6.01 (Bruker AXS, 2000)'
_computing_data_collection       'SMART v. 5.611 (Bruker AXS, 2000)'
_computing_data_reduction        'SAINT+ v. 6.01 (Bruker AXS, 2000)'
_computing_molecular_graphics    'XP program, SHELXTL v6.10, Bruker2000'
_computing_publication_material  'XCIF program, SHELXTLv6.10, BrukerAXS'
_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 0.997
_diffrn_measured_fraction_theta_max 0.951
_diffrn_measurement_device_type  'Bruker SMART APEX CCD system'
_diffrn_measurement_method       '\w rotations with narrow frames'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0659
_diffrn_reflns_av_sigmaI/netI    0.1368
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       46
_diffrn_reflns_limit_l_min       -46
_diffrn_reflns_number            27547
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         28.56
_diffrn_reflns_theta_min         1.92
_diffrn_standards_decay_%        'no decay'
_exptl_absorpt_coefficient_mu    1.867
_exptl_absorpt_correction_T_max  0.813
_exptl_absorpt_correction_T_min  0.672
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS: Area-Detector Absorption Correction. (1996) Bruker-AXS
within SAINT+ package, v. 6.01.
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.808
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'irregular lamina'
_exptl_crystal_F_000             2224
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.434
_refine_diff_density_min         -0.942
_refine_diff_density_rms         0.115
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.038(19)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.783
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     478
_refine_ls_number_reflns         9745
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.783
_refine_ls_R_factor_all          0.0702
_refine_ls_R_factor_gt           0.0447
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0591
_refine_ls_wR_factor_ref         0.0631
_reflns_number_gt                6439
_reflns_number_total             9745
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            B802381F.txt
_cod_data_source_block           compound_12a
_cod_original_sg_symbol_H-M      'P 212121'
_cod_database_code               7004074