A Ru(I) Metalloradical That Catalyzes Nitrene Coupling to Azoarenes from Arylazides
Ayumi Takaoka; Marc-Etienne Moret; Jonas C. Peters; Journal of the American Chemical Society 134 (2012) 6695–6706; doi:10.1021/ja211603f

data_4117821
_publ_section_title
;
 A Ru(I) Metalloradical That Catalyzes Nitrene Coupling to Azoarenes from
 Arylazides
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              6695
_journal_page_last               6706
_journal_paper_doi               10.1021/ja211603f
_journal_volume                  134
_journal_year                    2012
_chemical_formula_sum            'C52 H66 F6 N O5 P3 Ru S Si'
_chemical_formula_weight         1153.19
_chemical_name_systematic
; 
 ? 
;
_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                 110.714(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.4556(4)
_cell_length_b                   15.9409(4)
_cell_length_c                   20.2398(5)
_cell_measurement_reflns_used    9433
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      68.11
_cell_measurement_theta_min      2.88
_cell_volume                     5267.8(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.972
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0427
_diffrn_reflns_av_sigmaI/netI    0.0203
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            93228
_diffrn_reflns_theta_full        65.08
_diffrn_reflns_theta_max         65.08
_diffrn_reflns_theta_min         2.88
_exptl_absorpt_coefficient_mu    4.440
_exptl_absorpt_correction_T_max  0.9164
_exptl_absorpt_correction_T_min  0.2244
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.454
_exptl_crystal_description       plate
_exptl_crystal_F_000             2392
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.898
_refine_diff_density_min         -0.767
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     751
_refine_ls_number_reflns         8744
_refine_ls_number_restraints     377
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0355
_refine_ls_R_factor_gt           0.0337
_refine_ls_shift/su_max          0.167
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0618P)^2^+6.2597P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0974
_refine_ls_wR_factor_ref         0.0995
_reflns_number_gt                8293
_reflns_number_total             8744
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja211603f_si_002_4.cif
_cod_data_source_block           d8-09018
_cod_original_sg_symbol_H-M      'P 1 21/n 1 '
_cod_database_code               4117821