Slow Hydrogen Atom Self-Exchange between Os(IV) Anilide and Os(III) Aniline Complexes: Relationships with Electron and Proton Transfer Self-Exchange
Jake D. Soper; James M. Mayer; Journal of the American Chemical Society 125 (2003) 12217–12229; doi:10.1021/ja036328k

data_4114236
_publ_contact_author
;
      Mayer, James M.
    Department of Chemistry, BOX 351700
    University of Washington
    Seattle, WA 98195
    USA
;
_publ_contact_author_email       mayer@chem.washington.edu
_publ_section_title
;
 Slow Hydrogen Atom Self-Exchange between Os(IV) Anilide and Os(III)
 Aniline Complexes: Relationships with Electron and Proton Transfer
 Self-Exchange
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              12217
_journal_page_last               12229
_journal_paper_doi               10.1021/ja036328k
_journal_volume                  125
_journal_year                    2003
_chemical_formula_moiety         'C16 H18 B Cl2 N7 Os'
_chemical_formula_sum            'C16 H18 B Cl2 N7 Os'
_chemical_formula_weight         580.28
_chemical_name_common            JDS-IV-17
_chemical_name_systematic        JDS-IV-17
_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                 125.7020(13)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.6560(2)
_cell_length_b                   20.6880(5)
_cell_length_c                   11.7720(2)
_cell_measurement_reflns_used    286
_cell_measurement_temperature    130(2)
_cell_volume                     1909.66(8)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       KappaCCD
_computing_data_reduction        HKL2000
_computing_molecular_graphics    'maXus, Zortep'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SIR97
_diffrn_ambient_temperature      130(2)
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       '\f and \w scans'
_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  0.0320
_diffrn_reflns_av_sigmaI/netI    0.0517
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            5463
_diffrn_reflns_theta_full        24.71
_diffrn_reflns_theta_max         24.71
_diffrn_reflns_theta_min         3.46
_exptl_absorpt_coefficient_mu    6.974
_exptl_absorpt_correction_T_max  0.5422
_exptl_absorpt_correction_T_min  0.2854
_exptl_absorpt_correction_type   denzo2000
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    2.018
_exptl_crystal_description       cut-block
_exptl_crystal_F_000             1112
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.810
_refine_diff_density_min         -0.893
_refine_diff_density_rms         0.132
_refine_ls_extinction_coef       0.00043(13)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    'H atoms riding'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     246
_refine_ls_number_reflns         3184
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.000
_refine_ls_R_factor_all          0.0348
_refine_ls_R_factor_gt           0.0250
_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^)+(0.0112P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0517
_refine_ls_wR_factor_ref         0.0541
_reflns_number_gt                2651
_reflns_number_total             3184
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja036328ksi20030528_060600.cif
_cod_data_source_block           shelxl
_cod_original_cell_volume        1909.66(7)
_cod_database_code               4114236