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_7235547
_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_sum            'C78 H72 B Cl P4 Ru'
_chemical_formula_weight         1280.57
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yab'
_space_group_name_H-M_alt        'P 1 21/a 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21/a 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.000(0)
_cell_angle_beta                 97.922(5)
_cell_angle_gamma                90.000(0)
_cell_formula_units_Z            4
_cell_length_a                   17.742(5)
_cell_length_b                   19.095(5)
_cell_length_c                   19.603(5)
_cell_measurement_temperature    293(2)
_cell_volume                     6578(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_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  0.2982
_diffrn_reflns_av_sigmaI/netI    0.2281
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            85071
_diffrn_reflns_theta_full        26.49
_diffrn_reflns_theta_max         26.49
_diffrn_reflns_theta_min         1.05
_exptl_absorpt_coefficient_mu    0.420
_exptl_crystal_density_diffrn    1.293
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2664
_refine_diff_density_max         0.644
_refine_diff_density_min         -0.732
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.964
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     766
_refine_ls_number_reflns         13498
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.964
_refine_ls_R_factor_all          0.2284
_refine_ls_R_factor_gt           0.0732
_refine_ls_shift/su_max          0.020
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0665P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1274
_refine_ls_wR_factor_ref         0.1933
_reflns_number_gt                5385
_reflns_number_total             13498
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4ra01411a2.cif
_cod_data_source_block           shelxl
_cod_original_sg_symbol_H-M      P21/a
_cod_database_code               7235547