Well-Defined Ir/Pd Complexes with a Triazolyl-diylidene Bridge as Catalysts for Multiple Tandem Reactions
Alessandro Zanardi; José A. Mata; Eduardo Peris; Journal of the American Chemical Society 131 (2009) 14531–14537; doi:10.1021/ja906028g

data_4105115
_publ_contact_author_address
;Dept. Qu\'imica Inorg\`anica i Org\`anica
Universitat Jaume I
Avda. Vicent Sos Bayn/n
12071 Castell\'o (Spain)
;
_publ_contact_author_email       jmata@qio.uji.es
_publ_contact_author_fax         964728214
_publ_contact_author_name        'Jose A. Mata Martinez'
_publ_contact_author_phone       964729166
_publ_section_title
;
 Well-Defined Ir/Pd Complexes with a Triazolyl-diylidene Bridge as
 Catalysts for Multiple Tandem Reactions
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              14531
_journal_page_last               14537
_journal_paper_doi               10.1021/ja906028g
_journal_volume                  131
_journal_year                    2009
_chemical_formula_moiety         'C31 H50 Cl8 Ir2 N6 Pd, CH2Cl2'
_chemical_formula_sum            'C32 H52 Cl10 Ir2 N6 Pd'
_chemical_formula_weight         1366.10
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_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                 99.2250(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   8.6071(5)
_cell_length_b                   17.8320(9)
_cell_length_c                   14.8374(7)
_cell_measurement_temperature    293(2)
_cell_volume                     2247.8(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0596
_diffrn_reflns_av_sigmaI/netI    0.0718
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            15388
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.80
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    6.927
_exptl_absorpt_correction_T_max  0.5442
_exptl_absorpt_correction_T_min  0.4662
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    2.018
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1312
_exptl_crystal_recrystallization_method
'mixtures of MeCN/CH2Cl2 slow evaporation'
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.583
_refine_diff_density_min         -0.836
_refine_diff_density_rms         0.162
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     238
_refine_ls_number_reflns         5166
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0697
_refine_ls_R_factor_gt           0.0373
_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^)+(0.0309P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0745
_refine_ls_wR_factor_ref         0.0841
_reflns_number_gt                3669
_reflns_number_total             5166
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja906028g_si_001.cif
_cod_data_source_block           str1022m
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4105115