Formation of [Ru(NHC)4(η2-O2)H]+: An Unusual, High Frequency Hydride Chemical Shift and Facile, Reversible Coordination of O2
L. Jonas L. Häller; Elena Mas-Marzá; Aitor Moreno; John P. Lowe; Stuart A. Macgregor; Mary F. Mahon; Paul S. Pregosin; Michael K. Whittlesey; Journal of the American Chemical Society 131 (2009) 9618–9619; doi:10.1021/ja9039345

data_4104706
_publ_section_title
;
 Formation of [Ru(NHC)4(\h2-O2)H]+: An Unusual, High Frequency Hydride
 Chemical Shift and Facile, Reversible Coordination of O2
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              9618
_journal_page_last               9619
_journal_paper_doi               10.1021/ja9039345
_journal_volume                  131
_journal_year                    2009
_chemical_formula_sum            'C77 H93 B F24 N8 O Ru'
_chemical_formula_weight         1714.47
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yab'
_symmetry_space_group_name_H-M   'P 1 21/a 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                 104.875(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.5720(3)
_cell_length_b                   21.1740(3)
_cell_length_c                   20.2440(3)
_cell_measurement_reflns_used    110644
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      2.910
_cell_volume                     8108.3(2)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_data_reduction
'Denzo & Scalepack (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'ORTEX (P.McArdle, 1995)'
_computing_publication_material  'SHELXL-97/2 (Sheldrick,1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  '95mm CCD camera on \k-goniostat'
_diffrn_measurement_method       CCD
_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  0.1177
_diffrn_reflns_av_sigmaI/netI    0.0856
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            77117
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         3.56
_exptl_absorpt_coefficient_mu    0.297
_exptl_absorpt_correction_T_max  0.96
_exptl_absorpt_correction_T_min  0.77
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 ?
;
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.404
_exptl_crystal_description       Block
_exptl_crystal_F_000             3536
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.373
_refine_diff_density_min         -1.113
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1241
_refine_ls_number_reflns         18500
_refine_ls_number_restraints     81
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.1121
_refine_ls_R_factor_gt           0.0664
_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^)+(0.0470P)^2^+15.7987P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1453
_refine_ls_wR_factor_ref         0.1739
_reflns_number_gt                12214
_reflns_number_total             18500
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja9039345_si_002_3.cif
_cod_data_source_block           cpd3_k08mkw15
_cod_database_code               4104706