Synthesis and Spectroscopic and Spectroelectrochemical Characterization of a New Family of 44e-Tris-Phosphido-Bridged Palladium Triangles
Veronica Bonuccelli; Tiziana Funaioli; Piero Leoni; Fabio Marchetti; Lorella Marchetti; Inorganic Chemistry 52 (2013) 8759–8769; doi:10.1021/ic4009448

data_4335574
_publ_section_title
;
 Synthesis and Spectroscopic and Spectroelectrochemical Characterization
 of a New Family of 44e-Tris-Phosphido-Bridged Palladium Triangles
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8759
_journal_page_last               8769
_journal_paper_doi               10.1021/ic4009448
_journal_volume                  52
_journal_year                    2013
_chemical_formula_sum            'C26 H52 Br O2 P3 Pd3'
_chemical_formula_weight         888.70
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.084(2)
_cell_length_b                   17.808(2)
_cell_length_c                   11.8374(14)
_cell_measurement_temperature    293(2)
_cell_volume                     3812.1(8)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_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_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0458
_diffrn_reflns_av_sigmaI/netI    0.1012
_diffrn_reflns_limit_h_max       1
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       1
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -1
_diffrn_reflns_number            5080
_diffrn_reflns_theta_full        26.50
_diffrn_reflns_theta_max         26.50
_diffrn_reflns_theta_min         2.06
_exptl_absorpt_coefficient_mu    2.592
_exptl_crystal_density_diffrn    1.548
_exptl_crystal_F_000             1768
_refine_diff_density_max         0.712
_refine_diff_density_min         -0.564
_refine_diff_density_rms         0.128
_refine_ls_extinction_coef       0.00042(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.986
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     179
_refine_ls_number_reflns         4090
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.986
_refine_ls_R_factor_all          0.1273
_refine_ls_R_factor_gt           0.0560
_refine_ls_shift/su_max          0.636
_refine_ls_shift/su_mean         0.009
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0371P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0966
_refine_ls_wR_factor_ref         0.1191
_reflns_number_gt                2282
_reflns_number_total             4090
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ic4009448_si_001.cif
_cod_data_source_block           trip
_cod_database_code               4335574