Trapping of the putative 1,2-dinitrosoarene intermediate of benzofuroxan tautomerization by coordination at ruthenium and exploration of its redox non-innocence
Chan, Siu-Chung; England, Jason; Wieghardt, Karl; Wong, Chun-Yuen; Chemical Science 5 (2014) 3883–; doi:10.1039/C4SC01185F

data_1516506
_publ_section_title
;
 Trapping of the putative 1,2-dinitrosoarene intermediate of benzofuroxan
 tautomerization by coordination at ruthenium and exploration of its redox
 non-innocence
;
_journal_issue                   10
_journal_name_full               'Chemical Science'
_journal_page_first              3883
_journal_paper_doi               10.1039/C4SC01185F
_journal_volume                  5
_journal_year                    2014
_chemical_formula_sum            'C28 H24 Cl2 F6 N6 O3 P Ru'
_chemical_formula_weight         809.47
_space_group_IT_number           60
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_space_group_name_H-M   'P b c n'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   14.1173(2)
_cell_length_b                   15.5837(2)
_cell_length_c                   28.1669(5)
_cell_measurement_reflns_used    10497
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      71.5194
_cell_measurement_theta_min      3.1278
_cell_volume                     6196.71(16)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 16.1270
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini ultra'
_diffrn_measurement_method       '\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  0.0264
_diffrn_reflns_av_sigmaI/netI    0.0210
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            23669
_diffrn_reflns_theta_full        67.50
_diffrn_reflns_theta_max         67.50
_diffrn_reflns_theta_min         4.23
_exptl_absorpt_coefficient_mu    6.885
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.42971
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'CrysAlisPro, Agilent Technologies, Version 1.171.35.21'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.735
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3240
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.867
_refine_diff_density_min         -0.777
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     425
_refine_ls_number_reflns         5585
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0555
_refine_ls_R_factor_gt           0.0482
_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^)+(0.0704P)^2^+18.5764P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1333
_refine_ls_wR_factor_ref         0.1407
_reflns_number_gt                4846
_reflns_number_total             5585
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4sc01185f2.cif
_cod_data_source_block           complex-2b-anionic-radical
_cod_depositor_comments
'Adding full bibliography for 1516502--1516506.cif.'
_cod_original_sg_symbol_H-M      Pbcn
_cod_database_code               1516506