Asymmetric cleavage of 2,2'-pyridil to a picolinic acid anion radical coordinated to ruthenium(II): splitting of water to hydrogen
Manas Kumar Biswas; Sarat Chandra Patra; Amarendra Nath Maity; Shyue-Chu Ke; Thomas Weyhermullerc; Prasanta Ghosh; Chem.Commun. 49 (2013) 4522–; doi:10.1039/c3cc40956b

data_7109255
_publ_section_title
;
 Asymmetric cleavage of 2,2'-pyridil to a picolinic acid anion radical
 coordinated to ruthenium(II): splitting of water to hydrogen
;
_journal_name_full               Chem.Commun.
_journal_page_first              4522
_journal_paper_doi               10.1039/c3cc40956b
_journal_volume                  49
_journal_year                    2013
_chemical_formula_moiety         'C43 H34 Cl N O3 P2 Ru, 0.5(C7 H8)'
_chemical_formula_sum            'C46.5 H38 Cl N O3 P2 Ru'
_chemical_formula_weight         857.24
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                89.57(3)
_cell_angle_beta                 75.48(3)
_cell_angle_gamma                80.19(3)
_cell_formula_units_Z            2
_cell_length_a                   11.123(2)
_cell_length_b                   11.397(2)
_cell_length_c                   18.288(4)
_cell_measurement_reflns_used    9957
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      23.48
_cell_measurement_theta_min      2.30
_cell_volume                     2210.0(8)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_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  0.0661
_diffrn_reflns_av_sigmaI/netI    0.0770
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            29035
_diffrn_reflns_theta_full        23.27
_diffrn_reflns_theta_max         23.27
_diffrn_reflns_theta_min         2.11
_exptl_absorpt_coefficient_mu    0.526
_exptl_absorpt_correction_T_max  0.997
_exptl_absorpt_correction_T_min  0.978
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            greenish_yellow
_exptl_crystal_density_diffrn    1.288
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'transparent parallelepiped'
_exptl_crystal_F_000             878
_exptl_crystal_size_max          0.03
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.255
_refine_diff_density_min         -0.740
_refine_diff_density_rms         0.127
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.140
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     515
_refine_ls_number_reflns         6240
_refine_ls_number_restraints     157
_refine_ls_restrained_S_all      1.133
_refine_ls_R_factor_all          0.1243
_refine_ls_R_factor_gt           0.0765
_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^)+(0.1125P)^2^+6.1911P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1941
_refine_ls_wR_factor_ref         0.2413
_reflns_number_gt                4098
_reflns_number_total             6240
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3cc40956b.txt
_cod_data_source_block           c3ac.1/2toluene
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C46.50 H38 Cl N O3 P2 Ru'
_cod_database_code               7109255