Synthesis and Characterization of Low-Spin and Cation Radical Complexes of Ruthenium(III) of a Tridentate Pyridine Bis-Amide Ligand
Akhilesh Kumar Singh; V. Balamurugan; Rabindranath Mukherjee; Inorganic Chemistry 42 (2003) 6497–6502; doi:10.1021/ic034356y

data_4314348
_publ_section_title
;
 Synthesis and Characterization of Low-Spin and Cation Radical Complexes
 of Ruthenium(III) of a Tridentate Pyridine Bis-Amide Ligand
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6497
_journal_page_last               6502
_journal_paper_doi               10.1021/ic034356y
_journal_volume                  42
_journal_year                    2003
_chemical_formula_moiety         'H20,(C38 H26 N6 O4 Ru)1-,(C8 H20 N)1+'
_chemical_formula_sum            'C46 H48 N7 O5 Ru'
_chemical_formula_weight         879.98
_chemical_melting_point          'Decomposes above 200 degree celsius'
_chemical_name_systematic
;

   ?

;
_space_group_IT_number           15
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.0(0)
_cell_angle_beta                 103.67(4)
_cell_angle_gamma                90.0(0)
_cell_formula_units_Z            4
_cell_length_a                   9.809(7)
_cell_length_b                   22.876(5)
_cell_length_c                   19.734(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24.96
_cell_measurement_theta_min      2.76
_cell_volume                     4303(3)
_computing_cell_refinement       'CAD4 Express (Enraf Nonius, 1994)'
_computing_data_collection       'CAD4 Express (Enraf Nonius, 1994)'
_computing_data_reduction        'XCAD4 (Harms & Wocadlo, 1995)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'CAD4 mach'
_diffrn_measurement_method       'non-profiled omega/2theta scans'
_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  0.0180
_diffrn_reflns_av_sigmaI/netI    0.0435
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            3009
_diffrn_reflns_theta_full        22.48
_diffrn_reflns_theta_max         22.48
_diffrn_reflns_theta_min         1.78
_diffrn_standards_decay_%        1.48
_diffrn_standards_interval_count 90
_diffrn_standards_interval_time  'one hour'
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.418
_exptl_absorpt_correction_T_max  0.9210
_exptl_absorpt_correction_T_min  0.9051
_exptl_absorpt_correction_type   analytical
_exptl_crystal_colour            'Reddish brown'
_exptl_crystal_density_diffrn    1.359
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1828
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         2.471
_refine_diff_density_min         -2.711
_refine_diff_density_rms         0.263
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.301
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     289
_refine_ls_number_reflns         2814
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.301
_refine_ls_R_factor_all          0.1151
_refine_ls_R_factor_gt           0.0945
_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^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2665
_refine_ls_wR_factor_ref         0.2899
_reflns_number_gt                2247
_reflns_number_total             2814
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic034356ysi20030409_054507.cif
_cod_data_source_block           20nov
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Analytical' changed to
'analytical' according to the built-in table from CIF Core dictionary
named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_cell_volume        4302(3)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4314348