Stoichiometric and Catalytic Deuteration of Pyridine and Methylpyridines by H/D Exchange with Benzene-d6Promoted by an Unsaturated Osmium Tetrahydride Species
Eguillor, Beatriz; Esteruelas, Miguel A.; García-Raboso, Jorge; Oliván, Montserrat; Oñate, Enrique; Organometallics 28 (2009) 3700–; doi:10.1021/om900335b

data_4069643
_publ_section_title
;
 Stoichiometric and Catalytic Deuteration of Pyridine and Methylpyridines
 by H/D Exchange with Benzene-d6Promoted by an Unsaturated Osmium
 Tetrahydride Species
;
_journal_issue                   13
_journal_name_full               Organometallics
_journal_page_first              3700
_journal_paper_doi               10.1021/om900335b
_journal_volume                  28
_journal_year                    2009
_chemical_formula_moiety         'C23 H51 N Os P2'
_chemical_formula_sum            'C23 H51 N Os P2'
_chemical_formula_weight         593.79
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 93.388(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.9417(14)
_cell_length_b                   18.470(3)
_cell_length_c                   18.331(3)
_cell_measurement_reflns_used    1826
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      19
_cell_measurement_theta_min      2
_cell_volume                     2684.2(8)
_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 0.997
_diffrn_measured_fraction_theta_max 0.934
_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
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1415
_diffrn_reflns_av_sigmaI/netI    0.1709
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            28194
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         29.01
_diffrn_reflns_theta_min         1.57
_diffrn_standards_decay_%        'no decay'
_exptl_absorpt_coefficient_mu    4.878
_exptl_absorpt_correction_T_max  0.751
_exptl_absorpt_correction_T_min  0.516
_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.

SADABS: Area-Detector Absorption Correction. Bruker-AXS 
within SAINT+ package, v. 6.1 (2000).
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.469
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'irregular block'
_exptl_crystal_F_000             1208
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.924
_refine_diff_density_min         -1.246
_refine_diff_density_rms         0.176
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.746
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     270
_refine_ls_number_reflns         6672
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      0.746
_refine_ls_R_factor_all          0.0958
_refine_ls_R_factor_gt           0.0462
_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^)+(0.0144P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0725
_refine_ls_wR_factor_ref         0.0811
_reflns_number_gt                3929
_reflns_number_total             6672
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om900335b_si_001.cif
_cod_data_source_block           mae267as
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               4069643