Reactions of Ruthenium Bipyridine Catalyst Precursors: Synthetic, Structural, and Theoretical Studies on Ruthenium Mono(bipyridine) Carbonyls in Ethylene Glycol Solutions
Matti Haukka; Pipsa Hirva; Saija Luukkanen; Mirja Kallinen; Markku Ahlgrén; Tapani A. Pakkanen; Inorganic Chemistry 38 (1999) 3182–3189; doi:10.1021/ic981266y

data_4322099
_publ_contact_author
;
        Matti Haukka
        Department of Chemistry
        University of Joensuu
        PO Box 111, FIN-80101
        Finland
;
_publ_contact_author_email       matti.haukka@joensuu.fi
_publ_contact_author_fax         358-13-2513344
_publ_contact_author_phone       358-13-2513345
_publ_section_title
;
 Reactions of Ruthenium Bipyridine Catalyst Precursors: Synthetic,
 Structural, and Theoretical Studies on Ruthenium Mono(bipyridine)
 Carbonyls in Ethylene Glycol Solutions
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3182
_journal_page_last               3189
_journal_paper_doi               10.1021/ic981266y
_journal_volume                  38
_journal_year                    1999
_chemical_formula_sum            'C15.5 H14.5 Cl N2 O5.5 Ru'
_chemical_formula_weight         453.31
_chemical_name_common            Ru(bpy)(CO)2Cl(C(O)OCH2CH2OH).1/4(HOCH2CH2OH)
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_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                90.00
_cell_angle_beta                 112.01(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            16
_cell_length_a                   27.889(3)
_cell_length_b                   10.270(2)
_cell_length_c                   26.563(2)
_cell_measurement_temperature    293(2)
_cell_volume                     7054(2)
_computing_cell_refinement       'Denzo/Scalepack (Otwinowski, Minor, 1997)'
_computing_data_collection       'kcd (Nonius B.V., 1997)'
_computing_data_reduction        'Denzo/Scalepack (Otwinowski, Minor, 1997)'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_diffrn_measurement_method       phi/omega-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  0.0555
_diffrn_reflns_av_sigmaI/netI    0.0816
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            25676
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.88
_exptl_absorpt_coefficient_mu    1.071
_exptl_crystal_colour            'Pale yellow (nearly colourless)'
_exptl_crystal_density_diffrn    1.707
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Irregular
_exptl_crystal_F_000             3624
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.481
_refine_diff_density_min         -0.291
_refine_diff_density_rms         0.056
_refine_ls_extinction_coef       0.000033(14)
_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   0.773
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     454
_refine_ls_number_reflns         6204
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.773
_refine_ls_R_factor_all          0.0560
_refine_ls_R_factor_gt           0.0275
_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^)+(0.0059P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0464
_refine_ls_wR_factor_ref         0.0489
_reflns_number_gt                3798
_reflns_number_total             6204
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic981266y_2.cif
_cod_data_source_block           Ru(bpy)(CO)2Cl(C(O)OCH2CH2OH).1/4(HOCH2CH2OH)
_cod_original_cell_volume        7053.7(17)
_cod_original_formula_sum        'C15.50 H14.50 Cl N2 O5.50 Ru'
_cod_database_code               4322099