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_4117819
_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            'C75 H73 B F24 N3 O P3 Ru Si'
_chemical_formula_weight         1721.24
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 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                 110.504(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   15.1068(14)
_cell_length_b                   15.2076(12)
_cell_length_c                   17.5911(16)
_cell_measurement_reflns_used    9846
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.07
_cell_measurement_theta_min      2.20
_cell_volume                     3785.3(6)
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_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           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0796
_diffrn_reflns_av_sigmaI/netI    0.0896
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            87565
_diffrn_reflns_theta_full        30.03
_diffrn_reflns_theta_max         30.03
_diffrn_reflns_theta_min         1.24
_exptl_absorpt_coefficient_mu    0.392
_exptl_absorpt_correction_T_max  0.9545
_exptl_absorpt_correction_T_min  0.9257
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_density_diffrn    1.510
_exptl_crystal_density_meas      orange
_exptl_crystal_description       Block
_exptl_crystal_F_000             1752
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.062
_refine_diff_density_min         -0.477
_refine_diff_density_rms         0.096
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.06(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1055
_refine_ls_number_reflns         22047
_refine_ls_number_restraints     1628
_refine_ls_restrained_S_all      1.132
_refine_ls_R_factor_all          0.0964
_refine_ls_R_factor_gt           0.0595
_refine_ls_shift/su_max          0.085
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0741P)^2^+0.7428P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1309
_refine_ls_wR_factor_ref         0.1515
_reflns_number_gt                15667
_reflns_number_total             22047
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja211603f_si_002_2.cif
_cod_data_source_block           09278
_cod_original_sg_symbol_H-M      'P 1 21 1 '
_cod_database_code               4117819