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_4322098
_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            'C13 H13 Cl3 N2 O5 Ru'
_chemical_formula_weight         484.67
_chemical_name_common            '[Ru(bpy)(CO)3Cl]+[Cl]-.(H5O2)+(Cl)-'
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           60
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_space_group_name_H-M   'P b c n'
_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            8
_cell_length_a                   20.856(4)
_cell_length_b                   13.523(3)
_cell_length_c                   13.203(3)
_cell_measurement_temperature    293(2)
_cell_volume                     3723.7(14)
_computing_cell_refinement       'Denzo/Scalepack (Otwinowski, Minor, 1997)'
_computing_data_collection       'kcd (Nonius, 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 0.892
_diffrn_measured_fraction_theta_max 0.892
_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  0.0107
_diffrn_reflns_av_sigmaI/netI    0.0291
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            7155
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         4.26
_exptl_absorpt_coefficient_mu    1.296
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'pale yellow (nearly colourless)'
_exptl_crystal_density_diffrn    1.729
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'rectangular blocks'
_exptl_crystal_F_000             1920
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.484
_refine_diff_density_min         -0.400
_refine_diff_density_rms         0.049
_refine_ls_extinction_coef       0.00121(15)
_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   0.934
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     270
_refine_ls_number_reflns         3792
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.934
_refine_ls_R_factor_all          0.0251
_refine_ls_R_factor_gt           0.0203
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0308P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0498
_refine_ls_wR_factor_ref         0.0505
_reflns_number_gt                3045
_reflns_number_total             3792
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic981266y_1.cif
_cod_data_source_block           '[Ru(bpy)(CO)3Cl]+[Cl]-.(H5O2)+(Cl)-'
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' tag value 'Orthorombic' was replaced with
'orthorhombic' value as specified in the replacement file
'/home/robertas/cod-tools/perl-scripts/inputs/replacement_values.lst'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0308P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0308P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4322098