Different Reactivities of Pyrid-2-yl- and 6-Picol-2-yl-Functionalized NHC Ligands with [Ru3(CO)12]: C(sp2)−H and Double C(sp3)−H Bond Activation Reactions
Cabeza, Javier A.; Damonte, Marina; García-Álvarez, Pablo; Organometallics 30 (2011) 2371–; doi:10.1021/om200109n

data_4064436
_publ_section_title
;
 Different Reactivities of Pyrid-2-yl- and 6-Picol-2-yl-Functionalized NHC
 Ligands with [Ru3(CO)12]: C(sp2)&#x2212;H and Double C(sp3)&#x2212;H Bond
 Activation Reactions
;
_journal_issue                   8
_journal_name_full               Organometallics
_journal_page_first              2371
_journal_paper_doi               10.1021/om200109n
_journal_volume                  30
_journal_year                    2011
_chemical_formula_sum            'C19 H11 N3 O9 Ru3'
_chemical_formula_weight         728.52
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
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_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 102.3040(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.80480(10)
_cell_length_b                   15.42840(10)
_cell_length_c                   17.37680(10)
_cell_measurement_reflns_used    10511
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      74.4223
_cell_measurement_theta_min      2.5989
_cell_volume                     2306.31(3)
_computing_cell_refinement
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.31.5 (release 28-08-2006 CrysAlis171 .NET)
(compiled Aug 28 2006,13:05:05)
;
_computing_data_collection
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.31.5 (release 28-08-2006 CrysAlis171 .NET)
(compiled Aug 28 2006,13:05:05)
;
_computing_data_reduction
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.31.5 (release 28-08-2006 CrysAlis171 .NET)
(compiled Aug 28 2006,13:05:05)
;
_computing_molecular_graphics    'PLATON (Spek, 2008)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'DIRDIF-08 (Beurskens et al., 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.952
_diffrn_measurement_device_type  'Goniometer Xcalibur'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0229
_diffrn_reflns_av_sigmaI/netI    0.0190
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            15115
_diffrn_reflns_theta_full        70.00
_diffrn_reflns_theta_max         74.64
_diffrn_reflns_theta_min         3.87
_exptl_absorpt_coefficient_mu    16.211
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.49055
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.31.5 (release 28-08-2006 CrysAlis171 .NET)
(compiled Aug 28 2006,13:05:05)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.098
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       fragment
_exptl_crystal_F_000             1400
_exptl_crystal_size_max          0.1759
_exptl_crystal_size_mid          0.0907
_exptl_crystal_size_min          0.0495
_refine_diff_density_max         0.357
_refine_diff_density_min         -0.438
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     351
_refine_ls_number_reflns         4496
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0244
_refine_ls_R_factor_gt           0.0195
_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^)+(0.0355P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0500
_refine_ls_wR_factor_ref         0.0554
_reflns_number_gt                3854
_reflns_number_total             4496
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om200109n_si_002.cif
_cod_data_source_block           l7ef4
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               4064436