Synthesis, structure and catalytic properties of [Ru(dppp)2(CH3CN)Cl][BPh4] and isolation of catalytically active [Ru(dppp)2Cl][BPh4]: ruthenium catalysed alkyne homocoupling and tandem alkyne‒azide cycloaddition
Das, Uttam Kumar; Jena, Rajesh K.; Bhattacharjee, Manish; RSC Adv. 4 (2014) 21964–; doi:10.1039/C4RA01411A

data_7235546
_publ_section_title
;
 Synthesis, structure and catalytic properties of
 [Ru(dppp)2(CH3CN)Cl][BPh4] and isolation of catalytically active
 [Ru(dppp)2Cl][BPh4]: ruthenium catalysed alkyne homocoupling and tandem
 alkyne--azide cycloaddition
;
_journal_issue                   42
_journal_name_full               'RSC Adv.'
_journal_page_first              21964
_journal_paper_doi               10.1039/C4RA01411A
_journal_volume                  4
_journal_year                    2014
_chemical_formula_moiety         'C80 H75 B1 Cl1 N1 P4 Ru1'
_chemical_formula_sum            'C80 H75 B Cl N P4 Ru'
_chemical_formula_weight         1321.62
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2013-06-20T18:13:55-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                92.440(5)
_cell_angle_beta                 96.936(5)
_cell_angle_gamma                94.388(5)
_cell_formula_units_Z            2
_cell_length_a                   12.620(5)
_cell_length_b                   13.935(5)
_cell_length_c                   19.343(5)
_cell_measurement_reflns_used    0
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      0
_cell_measurement_theta_min      0
_cell_volume                     3362(2)
_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-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.879
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1009
_diffrn_reflns_av_unetI/netI     0.181
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            49741
_diffrn_reflns_theta_full        25
_diffrn_reflns_theta_max         30.64
_diffrn_reflns_theta_min         1.06
_exptl_absorpt_coefficient_mu    0.413
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.305
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1376
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.456
_refine_diff_density_min         -0.43
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.92
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     794
_refine_ls_number_reflns         18227
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.92
_refine_ls_R_factor_all          0.1871
_refine_ls_R_factor_gt           0.0619
_refine_ls_shift/su_max          0.03
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0569P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1574
_reflns_number_gt                7764
_reflns_number_total             18227
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4ra01411a2.cif
_cod_data_source_block           mb_ukd_catdppp_0m
_cod_database_code               7235546