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_4111998
_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         'C20 H32 Cl F3 N3 O8 Ru'
_chemical_formula_sum            'C20 H32 Cl F3 N3 O8 Ru'
_chemical_formula_weight         636.01
_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                 95.95(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   31.671(6)
_cell_length_b                   7.705(2)
_cell_length_c                   20.991(4)
_cell_measurement_reflns_used    0
_cell_measurement_temperature    253(2)
_cell_measurement_theta_max      0
_cell_measurement_theta_min      0
_cell_volume                     5094.7(19)
_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 0.555
_diffrn_measured_fraction_theta_max 0.555
_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  0.0553
_diffrn_reflns_av_sigmaI/netI    0.2088
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            4793
_diffrn_reflns_theta_full        23.47
_diffrn_reflns_theta_max         23.47
_diffrn_reflns_theta_min         1.29
_exptl_absorpt_coefficient_mu    0.792
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.658
_exptl_crystal_description       prism
_exptl_crystal_F_000             2600
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.998
_refine_diff_density_min         -0.613
_refine_diff_density_rms         0.131
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.907
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     185
_refine_ls_number_reflns         2089
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.907
_refine_ls_R_factor_all          0.1209
_refine_ls_R_factor_gt           0.0691
_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^)+(0.1008P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1743
_refine_ls_wR_factor_ref         0.2036
_reflns_number_gt                1003
_reflns_number_total             2089
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0528230si20050430_013045.cif
_cod_data_source_block           complex_4b
_cod_original_cell_volume        5094.8(19)
_cod_database_code               4111998