Alkene cis-Dihydroxylation by [(Me3tacn)(CF3CO2)RuVIO2]ClO4 (Me3tacn = 1,4,7-Trimethyl-1,4,7-triazacyclononane): Structural Characterization of [3 + 2] Cycloadducts and Kinetic Studies
Wing-Ping Yip; Wing-Yiu Yu; Nianyong Zhu; Chi-Ming Che; Journal of the American Chemical Society 127 (2005) 14239–14249; doi:10.1021/ja0528230

data_4111996
_publ_section_title
;
 Alkene cis-Dihydroxylation by [(Me3tacn)(CF3CO2)RuVIO2]ClO4 (Me3tacn =
 1,4,7-Trimethyl-1,4,7-triazacyclononane): Structural Characterization of
 [3 + 2] Cycloadducts and Kinetic Studies
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              14239
_journal_page_last               14249
_journal_paper_doi               10.1021/ja0528230
_journal_volume                  127
_journal_year                    2005
_chemical_formula_moiety         'C23.50 H45 Cl2 F6 N6 O13.50 Ru2'
_chemical_formula_sum            'C23.5 H45 Cl2 F6 N6 O13.5 Ru2'
_chemical_formula_weight         1014.70
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 94.21(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   28.367(6)
_cell_length_b                   14.059(3)
_cell_length_c                   20.140(4)
_cell_measurement_reflns_used    0
_cell_measurement_temperature    253(2)
_cell_measurement_theta_max      0
_cell_measurement_theta_min      0
_cell_volume                     8010(3)
_computing_cell_refinement       Scalepack
_computing_data_collection       Marcontrol
_computing_data_reduction        Denzo
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SIR-97
_diffrn_ambient_temperature      253(2)
_diffrn_measured_fraction_theta_full 0.903
_diffrn_measured_fraction_theta_max 0.903
_diffrn_measurement_device_type  'marresearch IPDS mar300'
_diffrn_measurement_method       Oscillation
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0476
_diffrn_reflns_av_sigmaI/netI    0.0744
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            22994
_diffrn_reflns_theta_full        25.35
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         1.44
_exptl_absorpt_coefficient_mu    0.979
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.683
_exptl_crystal_description       prism
_exptl_crystal_F_000             4096
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.196
_refine_diff_density_min         -0.816
_refine_diff_density_rms         0.211
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.986
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     466
_refine_ls_number_reflns         6623
_refine_ls_number_restraints     193
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0975
_refine_ls_R_factor_gt           0.0693
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1586P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2066
_refine_ls_wR_factor_ref         0.2220
_reflns_number_gt                4345
_reflns_number_total             6623
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0528230si20050430_013016.cif
_cod_data_source_block           complex_3
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_original_formula_sum        'C23.50 H45 Cl2 F6 N6 O13.50 Ru2'
_cod_database_code               4111996