X-ray Crystal and NMR Structure of a Highly Reactive Bidentate 1,2-Diamine-OsO4 Complex, Formally a 20-Electron Outer Valence Shell Species. Mechanistic Implications for the 1,2-Diamine-Accelerated Dihydroxylation of Olefins by OsO4
E. J. Corey; Sepehr Sarshar; Mihai D. Azimioara; Ronald C. Newbold; Mark C. Noe; Journal of the American Chemical Society 118 (1996) 7851–7852; doi:10.1021/ja960536d

data_4117159
_publ_section_title
;
 X-ray Crystal and NMR Structure of a Highly Reactive Bidentate
 1,2-Diamine-OsO4 Complex, Formally a 20-Electron Outer Valence Shell
 Species. Mechanistic Implications for the 1,2-Diamine-Accelerated
 Dihydroxylation of Olefins by OsO4
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              7851
_journal_page_last               7852
_journal_paper_doi               10.1021/ja960536d
_journal_volume                  118
_journal_year                    1996
_chemical_compound_source        'Ronald C. Newbold'
_chemical_formula_analytical     'C14 H26 N2 O4 Os'
_chemical_formula_moiety         'C14 H26 N2 O4 Os'
_chemical_formula_structural     'C14 H26 N2 O4 Os'
_chemical_formula_sum            'C14 H26 N2 O4 Os'
_chemical_formula_weight         476.57
_chemical_name_common            'OsO4-diamine complex'
_chemical_name_systematic
; 
 Osmium tetraoxide - (R,R)-trans-1,2-bispyrollidinecyclohexane complex
;
_chemical_temperature_decomposition 233
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.987(3)
_cell_length_b                   11.250(2)
_cell_length_c                   12.389(2)
_cell_measurement_reflns_used    100
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      15
_cell_measurement_theta_min      10
_cell_volume                     1531.3(6)
_computing_cell_refinement       'Siemens XDISK'
_computing_data_collection       'Siemens P3'
_computing_data_reduction        'Siemens SHELXTL PLUS'
_computing_molecular_graphics    'Siemens SHELXTL PLUS'
_computing_publication_material  'Siemens SHELXTL PLUS'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Siemens R3m'
_diffrn_measurement_method       'omega 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  0.0518
_diffrn_reflns_av_sigmaI/netI    0.0555
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            2469
_diffrn_reflns_theta_max         22.54
_diffrn_reflns_theta_min         2.45
_diffrn_standards_decay_%        1.2
_diffrn_standards_interval_count 47
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    8.345
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.067
_exptl_crystal_description       needle
_exptl_crystal_F_000             928
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.542
_refine_diff_density_min         -1.322
_refine_diff_density_rms         0.148
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.03(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.003
_refine_ls_goodness_of_fit_obs   1.012
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     190
_refine_ls_number_reflns         1998
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.011
_refine_ls_restrained_S_obs      1.012
_refine_ls_R_factor_all          0.0534
_refine_ls_R_factor_obs          0.0441
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0790P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1114
_refine_ls_wR_factor_obs         0.1041
_reflns_number_observed          1760
_reflns_number_total             2001
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja960536d.cif
_cod_data_source_block           ron
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0790P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0790P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4117159