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_4072337
_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            'C24 H51 Cl2 N Os P2'
_chemical_formula_weight         676.70
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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                 96.759(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.750(2)
_cell_length_b                   18.705(5)
_cell_length_c                   17.512(5)
_cell_measurement_reflns_used    2748
_cell_measurement_temperature    105(2)
_cell_measurement_theta_max      22
_cell_measurement_theta_min      2
_cell_volume                     2846.2(13)
_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      105(2)
_diffrn_detector_area_resol_mean 8.26
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.941
_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  0.0944
_diffrn_reflns_av_sigmaI/netI    0.0886
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            32647
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         28.83
_diffrn_reflns_theta_min         1.60
_diffrn_standards_decay_%        'no decay'
_exptl_absorpt_coefficient_mu    4.793
_exptl_absorpt_correction_T_max  0.831
_exptl_absorpt_correction_T_min  0.623
_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            orange
_exptl_crystal_density_diffrn    1.579
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'irregular block'
_exptl_crystal_F_000             1368
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.04
_refine_diff_density_max         2.394
_refine_diff_density_min         -1.130
_refine_diff_density_rms         0.277
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     296
_refine_ls_number_reflns         7009
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0792
_refine_ls_R_factor_gt           0.0509
_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^)+(0.0565P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1150
_refine_ls_wR_factor_ref         0.1286
_reflns_number_gt                5089
_reflns_number_total             7009
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om8007772_si_002.cif
_cod_data_source_block           mae281as
_cod_original_cell_volume        2846.3(12)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4072337