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_4105117
_publ_contact_author_address
;Universitat Jaume I
Avda. Vicent Sos Baynat s/n
12071 Castell\'on (Spain)
;
_publ_contact_author_email       jmata@qio.uji.es
_publ_contact_author_fax         964728214
_publ_contact_author_name        'Jose A. Mata'
_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         'C20H29Cl4IrN4Pd, 2.5(C H Cl3)'
_chemical_formula_sum            'C23 H32 Cl12.5 Ir N4 Pd'
_chemical_formula_weight         1106.25
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_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                 126.6400(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   28.9630(8)
_cell_length_b                   13.9348(4)
_cell_length_c                   23.0014(7)
_cell_measurement_temperature    273(2)
_cell_volume                     7448.9(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      273(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_method       'Bruker CCD'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0383
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            8493
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.72
_exptl_absorpt_coefficient_mu    4.972
_exptl_absorpt_correction_T_max  0.6632
_exptl_absorpt_correction_T_min  0.5642
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            Reddish
_exptl_crystal_density_diffrn    1.973
_exptl_crystal_description       Prism
_exptl_crystal_F_000             4268
_exptl_crystal_recrystallization_method 'Evaporation of a chloroform solution'
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.09
_refine_diff_density_max         2.026
_refine_diff_density_min         -1.357
_refine_diff_density_rms         0.181
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     381
_refine_ls_number_reflns         8493
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0628
_refine_ls_R_factor_gt           0.0485
_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^)+(0.0988P)^2^+4.0421P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1346
_refine_ls_wR_factor_ref         0.1442
_reflns_number_gt                6724
_reflns_number_total             8493
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja906028g_si_003.cif
_cod_data_source_block           str1040m
_cod_depositor_comments
;

2021-05-03
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_moiety     '2(C20H29Cl4IrN4Pd),C2 H2 Cl5,4(C H Cl3)'
_cod_original_formula_sum        'C46 H64 Cl25 Ir2 N8 Pd2'
_cod_original_formula_units_Z    4
_cod_original_formula_weight     2212.50
_cod_database_code               4105117