Activation of an Anilido Ligand for Nucleophilic Aromatic Substitution by an Oxidizing Os(IV) Center
Jake D. Soper; Werner Kaminsky; James M. Mayer; Journal of the American Chemical Society 123 (2001) 5594–5595; doi:10.1021/ja0159214

data_4115573
_publ_contact_author
;
    J. M. Mayer
    Department of Chemistry
    University of Washington
    Seattle, WA 98195
    USA
;
_publ_contact_author_email       mayer@chem.washington.edu
_publ_section_title
;
 Activation of an Anilido Ligand for Nucleophilic Aromatic Substitution by
 an Oxidizing Os(IV) Center
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              5594
_journal_page_last               5595
_journal_paper_doi               10.1021/ja0159214
_journal_volume                  123
_journal_year                    2001
_chemical_formula_sum            'C21 H26 B Cl2 N9 Os'
_chemical_formula_weight         676.42
_chemical_name_systematic
; 
TpOs[NH-p-C6H4N(c-C4H8)]Cl2 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/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                 97.632(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.6030(3)
_cell_length_b                   27.5330(11)
_cell_length_c                   10.4560(3)
_cell_measurement_reflns_used    485
_cell_measurement_temperature    130(2)
_cell_volume                     2454.74(15)
_computing_cell_refinement       'HKL SCALEPACK'
_computing_data_collection       KappaCCD
_computing_data_reduction        DENZO
_computing_molecular_graphics    'maXus, Zortep'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SIR92
_diffrn_ambient_temperature      130(2)
_diffrn_measured_fraction_theta_full 0.931
_diffrn_measured_fraction_theta_max 0.931
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       '\f scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0351
_diffrn_reflns_av_sigmaI/netI    0.0598
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            6976
_diffrn_reflns_theta_full        24.74
_diffrn_reflns_theta_max         24.74
_diffrn_reflns_theta_min         2.46
_exptl_absorpt_coefficient_mu    5.442
_exptl_absorpt_correction_T_max  0.6121
_exptl_absorpt_correction_T_min  0.3550
_exptl_absorpt_correction_type   numerical-SORTAV
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.830
_exptl_crystal_description       rod
_exptl_crystal_F_000             1320
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.654
_refine_diff_density_min         -1.263
_refine_diff_density_rms         0.141
_refine_ls_extinction_coef       0.00015(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   1.006
_refine_ls_hydrogen_treatment    'riding and isotropically'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     317
_refine_ls_number_reflns         3987
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.006
_refine_ls_R_factor_all          0.0423
_refine_ls_R_factor_gt           0.0317
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0313P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0694
_refine_ls_wR_factor_ref         0.0729
_reflns_number_gt                3340
_reflns_number_total             3987
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0159214_2.cif
_cod_data_source_block           TpOs[NH-p-C6H4N(c-C4H8)]Cl2.C2H3N
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0313P)^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^)+(0.0313P)^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_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4115573