NH-Tautomerization of 2-Substituted Pyridines and Quinolines on Osmium and Ruthenium: Determining Factors and Mechanism
Esteruelas, Miguel A.; Fernández-Alvarez, Francisco J.; Oñate, Enrique; Organometallics 27 (2008) 6236–; doi:10.1021/om8007772

data_4072338
_publ_section_title
;
 NH-Tautomerization of 2-Substituted Pyridines and Quinolines on Osmium
 and Ruthenium: Determining Factors and Mechanism
;
_journal_issue                   23
_journal_name_full               Organometallics
_journal_page_first              6236
_journal_paper_doi               10.1021/om8007772
_journal_volume                  27
_journal_year                    2008
_chemical_formula_sum            'C25.75 H38.5 Cl2 N3 O0.25 Os P'
_chemical_formula_weight         686.17
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                91.582(2)
_cell_angle_beta                 99.521(2)
_cell_angle_gamma                95.268(2)
_cell_formula_units_Z            4
_cell_length_a                   9.2152(11)
_cell_length_b                   16.7244(19)
_cell_length_c                   18.191(2)
_cell_measurement_reflns_used    943
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      23
_cell_measurement_theta_min      2
_cell_volume                     2750.7(5)
_computing_cell_refinement       'SAINT+ v. 6.02 (Bruker AXS, 1999)'
_computing_data_collection       'SMART v. 5.625 (Bruker AXS, 2000)'
_computing_data_reduction        'SAINT+ v. 6.02 (Bruker AXS, 1999)'
_computing_molecular_graphics    'XP, SHELXTL v. 6.1 (Bruker, 2000)'
_computing_publication_material  'XCIF, SHELXTL v. 6.1 (Bruker, 2000)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.26
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.899
_diffrn_measurement_device_type  'Bruker SMART APEX CCD system'
_diffrn_measurement_method       '\w rotations with narrow frames'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0588
_diffrn_reflns_av_sigmaI/netI    0.1689
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            25797
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         28.86
_diffrn_reflns_theta_min         1.22
_diffrn_standards_decay_%        'no decay'
_exptl_absorpt_coefficient_mu    4.908
_exptl_absorpt_correction_T_max  0.952
_exptl_absorpt_correction_T_min  0.639
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 Absorption correction performed with SADABS program. This is based on the
method of Blessing: Blessing, R. H., Acta Crystallogr., Sect. A 1995, 51, 33.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.657
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1364
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.498
_refine_diff_density_min         -1.201
_refine_diff_density_rms         0.168
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.664
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     598
_refine_ls_number_reflns         12960
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      0.665
_refine_ls_R_factor_all          0.0934
_refine_ls_R_factor_gt           0.0441
_refine_ls_shift/su_max          0.022
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0337P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0768
_refine_ls_wR_factor_ref         0.0907
_reflns_number_gt                7439
_reflns_number_total             12960
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om8007772_si_002.cif
_cod_data_source_block           mae210as
_cod_original_cell_volume        2750.6(6)
_cod_original_formula_sum        'C25.75 H38.50 Cl2 N3 O0.25 Os P'
_cod_database_code               4072338