Preparation, Characterization, and Reactivity of Azido Complex Containing a Tp(tBuNC)(PPh3)Ru Fragment and Ruthenium-Catalyzed Cycloaddition of Organic Azides with Alkynes in Organic and Aqueous Media
Lo, Yih-Hsing; Wang, Tsang-Hsiu; Lee, Chia-Yi; Feng, Ying-Hsuan; Organometallics 31 (2012) 6887–; doi:10.1021/om300687a

data_4079336
_publ_section_title
;
 Preparation, Characterization, and Reactivity of Azido Complex Containing
 a Tp(tBuNC)(PPh3)Ru Fragment and Ruthenium-Catalyzed Cycloaddition of
 Organic Azides with Alkynes in Organic and Aqueous Media
;
_journal_issue                   19
_journal_name_full               Organometallics
_journal_page_first              6887
_journal_paper_doi               10.1021/om300687a
_journal_volume                  31
_journal_year                    2012
_chemical_formula_moiety         'C36 H40 B F6 N7 O P2 Ru'
_chemical_formula_sum            'C36 H40 B F6 N7 O P2 Ru'
_chemical_formula_weight         874.57
_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                 91.8560(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.63080(10)
_cell_length_b                   21.9750(3)
_cell_length_c                   18.3342(2)
_cell_measurement_reflns_used    36879
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      25.028
_cell_measurement_theta_min      2.037
_cell_volume                     4280.84(8)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction        'HKL Denzo and Scalepack'
_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    'SHELXS-86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      200(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_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  0.0631
_diffrn_reflns_av_sigmaI/netI    0.0371
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            38941
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         2.13
_exptl_absorpt_coefficient_mu    0.503
_exptl_absorpt_correction_T_max  0.9686
_exptl_absorpt_correction_T_min  0.7679
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 ?
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.357
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1784
_exptl_crystal_size_max          0.57
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.316
_refine_diff_density_min         -1.109
_refine_diff_density_rms         0.218
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    fixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     487
_refine_ls_number_reflns         7562
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0660
_refine_ls_R_factor_gt           0.0546
_refine_ls_shift/su_max          0.016
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1047P)^2^+6.6889P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1604
_refine_ls_wR_factor_ref         0.1700
_reflns_number_gt                6413
_reflns_number_total             7562
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om300687a_si_003.cif
_cod_data_source_block           11
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4079336