Half-sandwich complexes of ruthenium, osmium, rhodium and iridium with DL-methionine or S-methyl-L-cysteine: A solid state and solution equilibrium study
Patalenszki, János; Bíró, Linda; Benyei, Attila; Muchova, Tereza Radosova; Kasparkova, Jana; Buglyo, Peter; RSC Adv.  (2014) –; doi:10.1039/C4RA15649H

data_7219177
_publ_section_title
;
 Half-sandwich complexes of ruthenium, osmium, rhodium and iridium with
 DL-methionine or S-methyl-L-cysteine: A solid state and solution
 equilibrium study
;
_journal_name_full               'RSC Adv.'
_journal_paper_doi               10.1039/C4RA15649H
_journal_year                    2014
_chemical_absolute_configuration syn
_chemical_formula_moiety         'C14 H22 N1 O2 Ru1 S1, N1 O3'
_chemical_formula_sum            'C14 H22 N2 O5 Ru S'
_chemical_formula_weight         431.46
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_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_date             2014-04-01T09:49:43-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_update_record
;
2014-11-10 deposited with the CCDC.
2014-12-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.510(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.8910(10)
_cell_length_b                   7.6110(10)
_cell_length_c                   18.0410(10)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      15.2
_cell_measurement_theta_min      5.8
_cell_volume                     1745.7(3)
_computing_cell_refinement       'MACH3/PC (Enraf Nonius, 1992)'
_computing_data_collection       'MACH3/PC (Enraf Nonius, 1992)'
_computing_data_reduction        'PROFIT (Streltsov & Zavodnik, 1989)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 2012)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SIR-92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.99
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_device_type  'Enraf Nonius MACH3'
_diffrn_measurement_method       'profiled omega/2theta scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0719
_diffrn_reflns_Laue_measured_fraction_full 0.99
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -2
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            4194
_diffrn_reflns_point_group_measured_fraction_full 0.536
_diffrn_reflns_point_group_measured_fraction_max 0.53
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.373
_diffrn_reflns_theta_min         2.568
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_decay_%        -1
_diffrn_standards_interval_count 147
_diffrn_standards_interval_time  120
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.042
_exptl_absorpt_correction_T_max  0.7941
_exptl_absorpt_correction_T_min  0.6703
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details
;
North A.C.T., Phillips D.C. & Mathews F.S. (1968) Acta. Cryst. A24, 351
        Number of psi-scan sets used was   3
        Theta correction was applied.
        Averaged transmission function was used.
        Fourier smoothing - Window value   5
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.642
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             880
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.962
_refine_diff_density_min         -1.017
_refine_diff_density_rms         0.152
_refine_ls_abs_structure_details
;
 Classical Flack method preferred over Parsons because
 only 1 suitable Friedel pairs available.
;
_refine_ls_abs_structure_Flack   -0.02(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     418
_refine_ls_number_reflns         3395
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.1564
_refine_ls_R_factor_gt           0.0741
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0175P)^2^+23.1159P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.168
_reflns_number_gt                1992
_reflns_number_total             3395
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4ra15649h2.cif
_cod_data_source_block           Ru(S-MeCys)
_cod_database_code               7219177
_publcif_datablock.id            {313bf4a6-25e1-4c7a-9eb2-a7f3d3e8f30a}