Proline as Chiral Auxiliary for the Economical Asymmetric Synthesis of Ruthenium(II) Polypyridyl Complexes
Chen Fu; Marianne Wenzel; Elisabeth Treutlein; Klaus Harms; Eric Meggers; Inorganic Chemistry 51 (2012) 10004–10011; doi:10.1021/ic3015157

data_4330412
_publ_section_title
;
 Proline as Chiral Auxiliary for the Economical Asymmetric Synthesis of
 Ruthenium(II) Polypyridyl Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              10004
_journal_page_last               10011
_journal_paper_doi               10.1021/ic3015157
_journal_volume                  51
_journal_year                    2012
_chemical_formula_moiety         '2(C41 H32 N5 O2 Ru, P F6)'
_chemical_formula_sum            'C41 H32 F6 N5 O2 P Ru'
_chemical_formula_weight         872.76
_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
_audit_update_record
;
2012-06-12 # Formatted by publCIF
;
_cell_angle_alpha                90.00
_cell_angle_beta                 106.071(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.0011(5)
_cell_length_b                   18.2927(6)
_cell_length_c                   14.4932(5)
_cell_measurement_reflns_used    23958
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.07
_cell_measurement_theta_min      1.79
_cell_volume                     3566.9(2)
_computing_cell_refinement       'STOE X-AREA'
_computing_data_collection       'STOE X-AREA'
_computing_data_reduction        'STOE X-RED'
_computing_molecular_graphics    'DIAMOND 3.2g'
_computing_publication_material  SHELXL
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'STOE IPDS 2'
_diffrn_measurement_method       'rotation method'
_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  0.0590
_diffrn_reflns_av_sigmaI/netI    0.1126
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            34262
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         1.46
_exptl_absorpt_coefficient_mu    0.562
_exptl_absorpt_correction_T_max  0.7094
_exptl_absorpt_correction_T_min  0.5301
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'[c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.625
_exptl_crystal_description       block
_exptl_crystal_F_000             1768
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.21
_refine_diff_density_max         0.626
_refine_diff_density_min         -0.420
_refine_diff_density_rms         0.059
_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   0.688
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1009
_refine_ls_number_reflns         13276
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.688
_refine_ls_R_factor_all          0.0488
_refine_ls_R_factor_gt           0.0304
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0119P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0485
_refine_ls_wR_factor_ref         0.0506
_reflns_number_gt                9196
_reflns_number_total             13276
_reflns_threshold_expression     >2sigma(I)
_publcif_info_exptl_table_max_cols 6
_cod_data_source_file            ic3015157_si_001_2.cif
_cod_data_source_block           2d
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               4330412