Unusual chemical transformations of acetone thiosemicarbazone mediated by ruthenium: C‒H bond activation, thiolation, and C‒N bond cleavage
Paul, Piyali; Seth, Dipravath Kumar; Richmond, Michael G.; Bhattacharya, Samaresh; RSC Adv. 4 (2014) 1432–; doi:10.1039/C3RA44329A

data_7239268
_publ_section_title
;
 Unusual chemical transformations of acetone thiosemicarbazone mediated by
 ruthenium: C--H bond activation, thiolation, and C--N bond cleavage
;
_journal_issue                   3
_journal_name_full               'RSC Adv.'
_journal_page_first              1432
_journal_paper_doi               10.1039/C3RA44329A
_journal_volume                  4
_journal_year                    2014
_chemical_formula_sum            'C41 H37.5 N4.5 O P2 Ru S2'
_chemical_formula_weight         868.92
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        '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                94.291(5)
_cell_angle_beta                 94.205(5)
_cell_angle_gamma                104.931(5)
_cell_formula_units_Z            2
_cell_length_a                   12.436(5)
_cell_length_b                   12.863(5)
_cell_length_c                   13.394(5)
_cell_measurement_temperature    293(2)
_cell_volume                     2054.9(14)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0657
_diffrn_reflns_av_sigmaI/netI    0.0863
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            26178
_diffrn_reflns_theta_full        23.03
_diffrn_reflns_theta_max         23.03
_diffrn_reflns_theta_min         1.53
_exptl_absorpt_coefficient_mu    0.601
_exptl_crystal_density_diffrn    1.404
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             892
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.998
_refine_diff_density_min         -0.403
_refine_diff_density_rms         0.104
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     488
_refine_ls_number_reflns         5733
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.1089
_refine_ls_R_factor_gt           0.0611
_refine_ls_shift/su_max          0.053
_refine_ls_shift/su_mean         0.005
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1106P)^2^+0.3421P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1669
_refine_ls_wR_factor_ref         0.1947
_reflns_number_gt                3642
_reflns_number_total             5733
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3ra44329a.txt
_cod_data_source_block           try-1
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7239268