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_4335575
_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_moiety         'C39 H81 N3 P3 Pd3, C F3 O3 S'
_chemical_formula_sum            'C40 H81 F3 N3 O3 P3 Pd3 S'
_chemical_formula_weight         1153.25
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 92.257(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.7168(6)
_cell_length_b                   19.8254(12)
_cell_length_c                   28.9139(17)
_cell_measurement_reflns_used    9959
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      53.802
_cell_measurement_theta_min      4.478
_cell_volume                     5565.6(6)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_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      296(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_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  0.0371
_diffrn_reflns_av_sigmaI/netI    0.0375
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            42271
_diffrn_reflns_theta_full        25.72
_diffrn_reflns_theta_max         25.72
_diffrn_reflns_theta_min         1.25
_exptl_absorpt_coefficient_mu    1.126
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.6666
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.376
_exptl_crystal_description       prism
_exptl_crystal_F_000             2368
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.136
_exptl_crystal_size_min          0.091
_refine_diff_density_max         1.680
_refine_diff_density_min         -0.978
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     479
_refine_ls_number_reflns         10556
_refine_ls_number_restraints     114
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0788
_refine_ls_R_factor_gt           0.0516
_refine_ls_shift/su_max          0.049
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0697P)^2^+16.8394P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1286
_refine_ls_wR_factor_ref         0.1465
_reflns_number_gt                7807
_reflns_number_total             10556
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ic4009448_si_002.cif
_cod_data_source_block           tripanit3_0m
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4335575