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_4117820
_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            'C47 H69 F6 N O2 P4 Ru Si'
_chemical_formula_weight         1047.07
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 92.074(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.6608(6)
_cell_length_b                   13.3290(6)
_cell_length_c                   28.9276(13)
_cell_measurement_reflns_used    9918
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      44.31
_cell_measurement_theta_min      2.35
_cell_volume                     4878.5(4)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_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 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and 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  0.0428
_diffrn_reflns_av_sigmaI/netI    0.0239
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       57
_diffrn_reflns_limit_l_min       -56
_diffrn_reflns_number            350218
_diffrn_reflns_theta_full        45.16
_diffrn_reflns_theta_max         45.16
_diffrn_reflns_theta_min         2.08
_exptl_absorpt_coefficient_mu    0.538
_exptl_absorpt_correction_T_max  0.8595
_exptl_absorpt_correction_T_min  0.8215
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.426
_exptl_crystal_description       block
_exptl_crystal_F_000             2184
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.29
_refine_diff_density_max         2.275
_refine_diff_density_min         -1.046
_refine_diff_density_rms         0.106
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     636
_refine_ls_number_reflns         40397
_refine_ls_number_restraints     474
_refine_ls_restrained_S_all      1.334
_refine_ls_R_factor_all          0.0560
_refine_ls_R_factor_gt           0.0386
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0517P)^2^+2.8559P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1005
_refine_ls_wR_factor_ref         0.1133
_reflns_number_gt                32287
_reflns_number_total             40397
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja211603f_si_002_3.cif
_cod_data_source_block           ayt14
_cod_original_sg_symbol_H-M      'P 1 21/c 1 '
_cod_database_code               4117820