Ruthenium(II) Complexes Containing 8-(Dimethylphosphino)quinoline (Me2Pqn): Preparation, Crystal Structures, and Electrochemical and Spectroscopic Properties of [Ru(bpy or phen)3-n(Me2Pqn)n](PF6)2(bpy = 2,2'-Bipyridine; phen = 1,10-Phenanthroline; n= 1, 2, or 3)
Takayoshi Suzuki; Takashi Kuchiyama; Shinobu Kishi; Sumio Kaizaki; Hideo D. Takagi; Masako Kato; Inorganic Chemistry 42 (2003) 785–795; doi:10.1021/ic020344l

data_4313008
_publ_contact_author
;
      Dr Takayoshi Suzuki
      Department of Chemistry
      Graduate of Science, Osaka University
      Toyonaka, 560-0043
      Japan
;
_publ_contact_author_email       suzuki@chem.sci.osaka-u.ac.jp
_publ_section_title
;
 Ruthenium(II) Complexes Containing 8-(Dimethylphosphino)quinoline
 (Me2Pqn): Preparation, Crystal Structures, and Electrochemical and
 Spectroscopic Properties of [Ru(bpy or phen)3-n(Me2Pqn)n](PF6)2(bpy =
 2,2'-Bipyridine; phen = 1,10-Phenanthroline; n= 1, 2, or 3)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              785
_journal_page_last               795
_journal_paper_doi               10.1021/ic020344l
_journal_volume                  42
_journal_year                    2003
_chemical_formula_moiety
'(Ru (C10 H8 N2) (C11 H12 N P)2 2+), 2(P F6 1-)'
_chemical_formula_sum            'C32 H32 F12 N4 P4 Ru'
_chemical_formula_weight         925.57
_chemical_name_common            trans(P,P)-[Ru(bpy)(Me~2~Pqn)~2~](PF~6~)~2~
_chemical_name_systematic
;
trans(P,P)-(2,2'-bipyridyl)bis(8-dimethylphosphinoquinoline)ruthenium(II)
Bis(hexafluorophosphate)
;
_space_group_IT_number           43
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'F 2 -2d'
_symmetry_space_group_name_H-M   'F d d 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            16
_cell_length_a                   37.414(8)
_cell_length_b                   40.172(7)
_cell_length_c                   9.9872(13)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      14.4
_cell_measurement_theta_min      12.6
_cell_volume                     15011(5)
_computing_cell_refinement       'Rigaku/AFC Diffractometer Control'
_computing_data_collection       'Rigaku/AFC Diffractometer Control'
_computing_data_reduction        teXsan
_computing_molecular_graphics    'ORTEP in teXsan'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Rigaku AFC7R'
_diffrn_measurement_method       \w-2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Rigaku rotating anode'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0203
_diffrn_reflns_av_sigmaI/netI    0.0706
_diffrn_reflns_limit_h_max       52
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       56
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            7846
_diffrn_reflns_theta_full        30.01
_diffrn_reflns_theta_max         30.01
_diffrn_reflns_theta_min         2.60
_diffrn_standards_decay_%        0.30
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.678
_exptl_absorpt_correction_T_max  0.903
_exptl_absorpt_correction_T_min  0.790
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'Coppens numerical (Coppens, et al., 1965)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.638
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       column
_exptl_crystal_F_000             7424
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.619
_refine_diff_density_min         -0.498
_refine_diff_density_rms         0.084
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.04(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     482
_refine_ls_number_reflns         6424
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.002
_refine_ls_R_factor_all          0.1053
_refine_ls_R_factor_gt           0.0388
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0593P)^2^+9.4366P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0991
_refine_ls_wR_factor_ref         0.1187
_reflns_number_gt                3863
_reflns_number_total             6424
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic020344l_2.cif
_cod_data_source_block           transbis
_cod_original_cell_volume        15011(4)
_cod_database_code               4313008