Preparation, Spectroscopic Characterization, and Theoretical Study of the [Pd4(dmb)4(PPh3)2]Cl2 Complex (dmb = 1,8-Diisocyano-p-menthane) and Its Organometallic Polymer {[Pd4(dmb)5](CH3CO2)2}n: The First Examples of 58-Electron Linear Pd4 Clusters
Tianle Zhang; Marc Drouin; Pierre D. Harvey; Inorganic Chemistry 38 (1999) 1305–1315; doi:10.1021/ic9811594

data_4321845
_publ_contact_author
;
Pierre D. Harvey
Department de chimie
Universite de Sherbrooke
2500 boul. Universite, Sherbrooke
Que., J1K 2R1
CANADA
;
_publ_contact_author_email       pharvey@courrier.usherb.ca
_publ_contact_author_fax         819-821-8017
_publ_contact_author_phone       819-821-7092
_publ_section_title
;
 Preparation, Spectroscopic Characterization, and Theoretical Study of the
 [Pd4(dmb)4(PPh3)2]Cl2 Complex (dmb = 1,8-Diisocyano-p-menthane) and Its
 Organometallic Polymer {[Pd4(dmb)5](CH3CO2)2}n: The First Examples of
 58-Electron Linear Pd4 Clusters
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1305
_journal_page_last               1315
_journal_paper_doi               10.1021/ic9811594
_journal_volume                  38
_journal_year                    1999
_chemical_formula_sum            'C48 H44 Cl0.5 N12 Pd'
_chemical_formula_weight         913.08
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                108.267(10)
_cell_angle_beta                 104.834(10)
_cell_angle_gamma                101.221(10)
_cell_formula_units_Z            2
_cell_length_a                   13.314(2)
_cell_length_b                   13.490(2)
_cell_length_c                   14.645(2)
_cell_measurement_temperature    293(2)
_cell_volume                     2303.8(6)
_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_source         'fine-focus sealed tube'
_diffrn_radiation_wavelength     1.54060
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0453
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            8739
_diffrn_reflns_theta_full        69.87
_diffrn_reflns_theta_max         69.87
_diffrn_reflns_theta_min         3.38
_exptl_absorpt_coefficient_mu    0.845
_exptl_crystal_density_diffrn    1.316
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             941
_refine_diff_density_max         1.626
_refine_diff_density_min         -1.243
_refine_diff_density_rms         0.101
_refine_ls_extinction_coef       0.0028(4)
_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   1.002
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     514
_refine_ls_number_reflns         8739
_refine_ls_number_restraints     84
_refine_ls_restrained_S_all      1.004
_refine_ls_R_factor_all          0.1192
_refine_ls_R_factor_gt           0.0739
_refine_ls_shift/su_max          0.011
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1524P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1961
_refine_ls_wR_factor_ref         0.2241
_reflns_number_gt                5313
_reflns_number_total             8739
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic9811594_2.cif
_cod_data_source_block           3
_cod_original_formula_sum        'C48 H44 Cl0.50 N12 Pd'
_cod_database_code               4321845