Ortho−Nitrosation of Anilines on a Ruthenium Hydridotris(pyrazolyl)borato Complex and Oxidation of the Resulting Coordinated Amine Groups
Arikawa, Yasuhiro; Yamaguchi, Soseki; Otsubo, Yuji; Onishi, Masayoshi; Umakoshi, Keisuke; Organometallics 34 (2015) 1056–; doi:10.1021/om5012769

data_4085579
_publ_section_title
;
 Ortho&#x2212;Nitrosation of Anilines on a Ruthenium
 Hydridotris(pyrazolyl)borato Complex and Oxidation of the Resulting
 Coordinated Amine Groups
;
_journal_issue                   6
_journal_name_full               Organometallics
_journal_page_first              1056
_journal_paper_doi               10.1021/om5012769
_journal_volume                  34
_journal_year                    2015
_chemical_formula_moiety         'C20 H24 B Cl N8 O Ru, C0.50 H3 O'
_chemical_formula_sum            'C20.5 H27 B Cl N8 O2 Ru'
_chemical_formula_weight         564.82
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.0000
_cell_angle_beta                 92.615(5)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            8
_cell_length_a                   12.293(3)
_cell_length_b                   21.318(6)
_cell_length_c                   19.025(5)
_cell_measurement_reflns_used    11339
_cell_measurement_temperature    93
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      3.06
_cell_volume                     4981(2)
_computing_cell_refinement       CrystalClear
_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        CrystalClear
_computing_molecular_graphics    'CrystalStructure 4.0'
_computing_publication_material  'CrystalStructure 4.0 (Rigaku, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'Il Milione (Burla, et al., 2007)'
_diffrn_ambient_temperature      93
_diffrn_detector_area_resol_mean 7.111
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Rigaku Saturn724'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0649
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            40292
_diffrn_reflns_theta_full        27.57
_diffrn_reflns_theta_max         27.57
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.771
_exptl_absorpt_correction_T_max  0.940
_exptl_absorpt_correction_T_min  0.761
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.506
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2304.00
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.130
_exptl_crystal_size_min          0.080
_refine_diff_density_max         2.610
_refine_diff_density_min         -1.330
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.098
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     599
_refine_ls_number_reflns         11411
_refine_ls_number_restraints     0
_refine_ls_R_factor_gt           0.0797
_refine_ls_shift/su_max          0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.1102P)^2^+9.5033P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.2180
_reflns_number_gt                8856
_reflns_number_total             11411
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            om5012769_si_002.cif
_cod_data_source_block           1163a
_cod_depositor_comments
'Adding full bibliography for 4085576--4085580.cif.'
_cod_original_formula_sum        'C20.50 H27 B Cl N8 O2 Ru'
_cod_database_code               4085579