Chiral-Auxiliary-Mediated Asymmetric Synthesis of Tris-Heteroleptic Ruthenium Polypyridyl Complexes
Lei Gong; Seann P. Mulcahy; Klaus Harms; Eric Meggers; Journal of the American Chemical Society 131 (2009) 9602–9603; doi:10.1021/ja9031665

data_4104698
_publ_section_title
;
 Chiral-Auxiliary-Mediated Asymmetric Synthesis of Tris-Heteroleptic
 Ruthenium Polypyridyl Complexes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              9602
_journal_page_last               9603
_journal_paper_doi               10.1021/ja9031665
_journal_volume                  131
_journal_year                    2009
_chemical_formula_moiety         'C40 H44 N6 Ru, C4 H10 O, 2(F6 P)'
_chemical_formula_sum            'C44 H54 F12 N6 O P2 Ru'
_chemical_formula_weight         1073.94
_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                 102.632(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.1185(6)
_cell_length_b                   12.5498(6)
_cell_length_c                   19.3212(14)
_cell_measurement_reflns_used    11906
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      4.5
_cell_volume                     2394.1(3)
_computing_cell_refinement       'STOE X-AREA'
_computing_data_collection       'STOE X-AREA'
_computing_data_reduction        'STOE X-AREA'
_computing_molecular_graphics    'DIAMOND 3.1 (Brandenburg, 1999)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR92 (Giacovazzo et al, 1993)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'STOE IPDS2'
_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  0.0594
_diffrn_reflns_av_sigmaI/netI    0.1011
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            12331
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         4.66
_exptl_absorpt_coefficient_mu    0.482
_exptl_absorpt_correction_T_max  1.0153
_exptl_absorpt_correction_T_min  0.9385
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;

;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.490
_exptl_crystal_description       prism
_exptl_crystal_F_000             1100
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.686
_refine_diff_density_min         -0.816
_refine_diff_density_rms         0.077
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.01(4)
_refine_ls_extinction_coef       0.0022(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.952
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     604
_refine_ls_number_reflns         8169
_refine_ls_number_restraints     28
_refine_ls_restrained_S_all      0.962
_refine_ls_R_factor_all          0.0750
_refine_ls_R_factor_gt           0.0530
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0490P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1026
_refine_ls_wR_factor_ref         0.1098
_reflns_number_gt                6400
_reflns_number_total             8169
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ja9031665_si_001.cif
_cod_data_source_block           gl_238
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               4104698