Formation of Ruthenium Nitrosyl Complexes: Reactions of Ru(bpy)(CO)2Cl2 and Its Methyl-Substituted Analogues Ru(4,4'-dmbpy)(CO)2Cl2 and Ru(6,6'-dmbpy)(CO)2Cl2 in Oxidizing Acidic Solutions
Pertti Homanen; Matti Haukka; Markku Ahlgrén; Tapani A. Pakkanen; Inorganic Chemistry 36 (1997) 3794–3797; doi:10.1021/ic970007q

data_4323528
_publ_contact_author
;
        Tapani A. Pakkanen
       Department of Chemistry
        University of Joensuu
        P.O. Box 111
        FIN-80101, Joensuu
        Finland
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_publ_contact_author_email       tap@joyl.joensuu.fi
_publ_contact_author_fax         '358 13 2513344'
_publ_contact_author_phone       '358 13 2513345'
_publ_section_title
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 Formation of Ruthenium Nitrosyl Complexes: Reactions of Ru(bpy)(CO)2Cl2
 and Its Methyl-Substituted Analogues Ru(4,4'-dmbpy)(CO)2Cl2 and
 Ru(6,6'-dmbpy)(CO)2Cl2 in Oxidizing Acidic Solutions
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_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3794
_journal_page_last               3797
_journal_paper_doi               10.1021/ic970007q
_journal_volume                  36
_journal_year                    1997
_chemical_compound_source        HCl/HNO3
_chemical_formula_structural     (RuCl5(NO))(H3O)2
_chemical_formula_sum            'Cl5 H6 N O3 Ru'
_chemical_formula_weight         346.38
_chemical_name_systematic
;
Dioxonium pentachloronitrosylruthenate(II)
;
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.462(5)
_cell_length_b                   6.910(3)
_cell_length_c                   10.526(3)
_cell_measurement_temperature    293(2)
_cell_volume                     979.2(6)
_computing_cell_refinement
;
P3/P4 Diffractometer Program V4.27 (Siemens 1989-1991)
;
_computing_data_collection
;
P3/P4 Diffractometer Program V4.27 (Siemens 1989-1991)
;
_computing_data_reduction
;
P3/P4 Diffractometer Program V4.27 (Siemens 1989-1991)
;
_computing_molecular_graphics    'SHELXTL PLUS (Siemens 1990)'
_computing_publication_material  'SHELXTL PLUS (Siemens 1990)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Syntex P2(1)'
_diffrn_measurement_method       'omega scan'
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0416
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            1184
_diffrn_reflns_theta_max         27.53
_diffrn_reflns_theta_min         3.03
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    2.921
_exptl_crystal_colour            'DARK RED'
_exptl_crystal_density_diffrn    2.350
_exptl_crystal_description       PLATE
_exptl_crystal_F_000             664
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.5
_refine_diff_density_max         1.644
_refine_diff_density_min         -0.804
_refine_diff_density_rms         0.212
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.19(27)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.935
_refine_ls_goodness_of_fit_obs   1.016
_refine_ls_hydrogen_treatment    isotropic
_refine_ls_matrix_type           full
_refine_ls_number_parameters     91
_refine_ls_number_reflns         1184
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.935
_refine_ls_restrained_S_obs      1.016
_refine_ls_R_factor_all          0.0580
_refine_ls_R_factor_obs          0.0427
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0669P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1039
_refine_ls_wR_factor_obs         0.0976
_reflns_number_observed          906
_reflns_number_total             1184
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic970007q_1.cif
_cod_data_source_block           Pentachloronitrosylruthenate
_cod_depositor_comments
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The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0669P)^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^)+(0.0669P)^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 
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_cod_original_formula_sum        'H6 Cl5 N O3 Ru'
_cod_database_code               4323528