Synthesis and Spectroelectrochemical Studies of Mixed Heteroleptic Chelate Complexes of Ruthenium(II) with 1,8-Bis(2-pyridyl)-3,6-dithiaoctane (pdto) and Substituted 1,10-Phenanthrolines
Luis A. Ortiz-Frade; Lena Ruiz-Ramírez; Ignacio González; Armando Marín-Becerra; Manuel Alcarazo; José G. Alvarado-Rodriguez; Rafael Moreno-Esparza; Inorganic Chemistry 42 (2003) 1825–1834; doi:10.1021/ic025849q

data_4313381
_publ_contact_author             'Ruiz-Ram\'irez L.'
_publ_contact_author_email       lena@servidor.unam.mx
_publ_section_title
;
 Synthesis and Spectroelectrochemical Studies of Mixed Heteroleptic
 Chelate Complexes of Ruthenium(II) with
 1,8-Bis(2-pyridyl)-3,6-dithiaoctane (pdto) and Substituted
 1,10-Phenanthrolines
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1825
_journal_page_last               1834
_journal_paper_doi               10.1021/ic025849q
_journal_volume                  42
_journal_year                    2003
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C20 H28 Cl2 N4 O1 Ru1 S2'
_chemical_formula_structural
'[RU1 (C16 H20 N2 S2) (C2 H3 N)2] (CL)2 0.5(H2 O)'
_chemical_formula_sum            'C20 H28 Cl2 N4 O Ru S2'
_chemical_formula_weight         576.55
_chemical_name_systematic
;
 Bis(acetonitrile) 1,8-bis(2-pyridyl)-3,6-dithiaoctane ruthenium (II) chloride
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_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_date             2002-07-02T12:41:14-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 102.16(1)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.601(1)
_cell_length_b                   16.313(1)
_cell_length_c                   11.326(1)
_cell_measurement_reflns_used    6193
_cell_measurement_temperature    294(2)
_cell_measurement_theta_max      24.99
_cell_measurement_theta_min      1.98
_cell_measurement_wavelength     0.71073
_cell_volume                     2456.6(3)
_computing_cell_refinement       'SADABS (Siemens, 1996)'
_computing_data_collection       'SMART (Siemens, 1993)'
_computing_data_reduction        'SHELXTL (Siemens, 1996)'
_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      294(2)
_diffrn_detector                 'CCD Area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'Brucker 6000 CCD area detector'
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0198
_diffrn_reflns_av_unetI/netI     0.0159
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            7318
_diffrn_reflns_theta_full        24.99
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         1.98
_diffrn_source                   'fine focus sealed tube'
_exptl_absorpt_coefficient_mu    1.045
_exptl_absorpt_correction_T_max  0.8182
_exptl_absorpt_correction_T_min  0.6799
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.559
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prismatic
_exptl_crystal_F_000             1176
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.322
_refine_diff_density_min         -0.46
_refine_diff_density_rms         0.117
_refine_ls_extinction_coef       0.0119(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.216
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     147
_refine_ls_number_reflns         2167
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.216
_refine_ls_R_factor_all          0.0402
_refine_ls_R_factor_gt           0.0388
_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^)+(0.0618P)^2^+11.8907P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1263
_refine_ls_wR_factor_ref         0.127
_reflns_number_gt                2054
_reflns_number_total             2167
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ic025849qsi20021022_074802_3.cif
_cod_data_source_block           rme3
_cod_original_cell_volume        2456.5(3)
_cod_original_formula_sum        'C20 H28 Cl2 N4 O1 Ru1 S2'
_cod_database_code               4313381