Stabilisation of a triply-bridging cyclopentadienyl ligand in a tetrapalladium cluster
Kirill Monakhov; Christophe Gourlaouen; Pierre Braunstein; Chem.Commun. 48 (2012) 8317–; doi:10.1039/c2cc32886k

data_7108162
_publ_section_title
;
 Stabilisation of a triply-bridging cyclopentadienyl ligand in a
 tetrapalladium cluster
;
_journal_name_full               Chem.Commun.
_journal_page_first              8317
_journal_paper_doi               10.1039/c2cc32886k
_journal_volume                  48
_journal_year                    2012
_chemical_formula_moiety         'C18 H22 O8 Pd4'
_chemical_formula_sum            'C18 H22 O8 Pd4'
_chemical_formula_weight         791.96
_chemical_name_systematic
;
?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_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                 90.703(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   30.142(4)
_cell_length_b                   8.6063(10)
_cell_length_c                   18.248(2)
_cell_measurement_reflns_used    4176
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.77
_cell_measurement_theta_min      2.23
_cell_volume                     4733.4(10)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  0.0476
_diffrn_reflns_av_sigmaI/netI    0.0639
_diffrn_reflns_limit_h_max       39
_diffrn_reflns_limit_h_min       -39
_diffrn_reflns_limit_k_max       4
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            15929
_diffrn_reflns_theta_full        28.03
_diffrn_reflns_theta_max         28.03
_diffrn_reflns_theta_min         2.23
_exptl_absorpt_coefficient_mu    3.029
_exptl_absorpt_correction_T_max  0.7937
_exptl_absorpt_correction_T_min  0.5555
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    2.223
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             3024
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_platon_squeeze_details
;
The residual electron density was assigned to half a molecule of the
diethyl ether solvent [119/8 = 15 e per asymmetric unit; half a
molecule of C4H10O would give 21e].
;
_refine_diff_density_max         1.594
_refine_diff_density_min         -1.557
_refine_diff_density_rms         0.212
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     275
_refine_ls_number_reflns         5715
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.1125
_refine_ls_R_factor_gt           0.0674
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0593P)^2^+106.2891P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1518
_refine_ls_wR_factor_ref         0.1693
_reflns_number_gt                3531
_reflns_number_total             5715
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            c2cc32886k.txt
_cod_data_source_block           pbkm110322
_cod_original_cell_volume        4733.5(10)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7108162