Oxidative ortho-C-N Fusion of Aniline by OsO4. Isolation, Characterization of Oxo-Amido Osmium(VI) Complexes, and their Catalytic Activities for Oxidative C-C Bond Cleavage of Unsaturated Hydrocarbons
Subhas Samanta; Laksmikanta Adak; Ranjan Jana; Golam Mostafa; Heikki M. Tuononen; Brindaban C. Ranu; Sreebrata Goswami; Inorganic Chemistry 47 (2008) 11062–11070; doi:10.1021/ic801352d

data_4306530
_publ_section_title
;
Oxidative ortho-C-N Fusion of Aniline by OsO4. Isolation, Characterization
of Oxo-Amido Osmium(VI) Complexes, and their Catalytic Activities for
Oxidative C-C Bond Cleavage of Unsaturated Hydrocarbons
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              11062
_journal_page_last               11070
_journal_paper_doi               10.1021/ic801352d
_journal_volume                  47
_journal_year                    2008
_chemical_formula_moiety         'C24 H20 N4 O Os'
_chemical_formula_sum            'C24 H20 N4 O Os'
_chemical_formula_weight         570.68
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           13
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      13
_symmetry_space_group_name_Hall  '-P 2yac'
_symmetry_space_group_name_H-M   'P 1 2/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                 95.070(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   14.036(2)
_cell_length_b                   4.9270(9)
_cell_length_c                   14.698(3)
_cell_measurement_reflns_used    6343
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.36
_cell_measurement_theta_min      2.78
_cell_volume                     1012.5(3)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'ORTEP-3 for windows (Farrugia,1997)'
_computing_publication_material  'Platon99 (Spek,1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker SMART APEX CCD'
_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  0.0424
_diffrn_reflns_av_sigmaI/netI    0.0669
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            6343
_diffrn_reflns_theta_full        28.36
_diffrn_reflns_theta_max         28.36
_diffrn_reflns_theta_min         2.78
_exptl_absorpt_coefficient_mu    6.321
_exptl_absorpt_correction_T_max  0.468
_exptl_absorpt_correction_T_min  0.269
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            Brown
_exptl_crystal_density_diffrn    1.872
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Parallelopiped
_exptl_crystal_F_000             552
_exptl_crystal_size_max          .32
_exptl_crystal_size_mid          .16
_exptl_crystal_size_min          .12
_refine_diff_density_max         1.436
_refine_diff_density_min         -1.353
_refine_diff_density_rms         0.232
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.144
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     206
_refine_ls_number_reflns         2514
_refine_ls_number_restraints     46
_refine_ls_restrained_S_all      2.258
_refine_ls_R_factor_all          0.0449
_refine_ls_R_factor_gt           0.0393
_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^)+(0.0258P)^2^+6.2114P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0873
_refine_ls_wR_factor_ref         0.0893
_reflns_number_gt                2309
_reflns_number_total             2514
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic801352d_si_002.cif
_cod_data_source_block           26_gm
_cod_depositor_comments
;

The second occurence of the _vrf_plat215_26_gm tag was renamed to
_vrf_PLAT215_26_gm_second.

Saulius Gra\<zulis
2010.05.12

The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      'P 2/n'
_cod_database_code               4306530