Understanding the Formation of N-H Tautomers from α-Substituted Pyridines: Tautomerization of 2-Ethylpyridine Promoted by Osmium
María L. Buil; Miguel A. Esteruelas; Karin Garcés; Montserrat Oliván; Enrique Oñate; Journal of the American Chemical Society 129 (2007) 10998–10999; doi:10.1021/ja073673r

data_4109914
_publ_contact_author
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  Dr. Enrique O\~nate
  Departamento de Qu\'imica Inorg\'anica - I.C.M.A.
  Universidad de Zaragoza - C.S.I.C.
  50009 Zaragoza, Spain
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_publ_contact_author_email       enriqueo@unizar.es
_publ_section_title
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 Understanding the Formation of N-H Tautomers from \a-Substituted
 Pyridines: Tautomerization of 2-Ethylpyridine Promoted by Osmium
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_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10998
_journal_page_last               10999
_journal_paper_doi               10.1021/ja073673r
_journal_volume                  129
_journal_year                    2007
_chemical_formula_sum            'C38 H62 B F4 N O Os P2'
_chemical_formula_weight         887.84
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
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_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                 125.574(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   23.589(2)
_cell_length_b                   20.399(2)
_cell_length_c                   19.951(2)
_cell_measurement_reflns_used    5720
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      22
_cell_measurement_theta_min      2
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_computing_cell_refinement       'SAINT+ v. 6.1 (Bruker AXS, 2000)'
_computing_data_collection       'SMART v. 5.625 (Bruker AXS, 2000)'
_computing_data_reduction        'SAINT+ v. 6.1 (Bruker AXS, 2000)'
_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 0.999
_diffrn_measured_fraction_theta_max 0.938
_diffrn_measurement_device_type  'Bruker SMART APEX CCD system'
_diffrn_measurement_method       '\w rotations with narrow frames'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
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_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            47097
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         29.00
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_diffrn_standards_decay_%        'no decay'
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;
Absorption correction performed with SADABS program. This is based on the
method of Blessing: Blessing, R. H., Acta Crystallogr., Sect. A 1995, 51, 33.

SADABS: Area-Detector Absorption Correction. Bruker-AXS 
within SAINT+ package, v. 6.1 (2000).
;
_exptl_crystal_colour            'dark red'
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_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.396
_refine_diff_density_min         -1.110
_refine_diff_density_rms         0.121
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.820
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     448
_refine_ls_number_reflns         9748
_refine_ls_number_restraints     26
_refine_ls_restrained_S_all      0.843
_refine_ls_R_factor_all          0.0688
_refine_ls_R_factor_gt           0.0396
_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^)+(0.0293P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0700
_refine_ls_wR_factor_ref         0.0756
_reflns_number_gt                6594
_reflns_number_total             9748
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja073673rsi20070717_033926_2.cif
_cod_data_source_block           mae240as
_cod_original_cell_volume        7808.3(15)
_cod_database_code               4109914