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_4321844
_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            'C64 H104 N10 O8 Pd4'
_chemical_formula_weight         1567.17
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 98.841(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.433(2)
_cell_length_b                   15.312(2)
_cell_length_c                   29.156(2)
_cell_measurement_temperature    293(2)
_cell_volume                     8572.5(16)
_computing_cell_refinement       NRCCAD
_computing_data_collection       NRCCAD
_computing_data_reduction        NRCVAX
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    NRCVAX
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54060
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0601
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            8796
_diffrn_reflns_theta_full        49.94
_diffrn_reflns_theta_max         49.94
_diffrn_reflns_theta_min         2.30
_exptl_absorpt_coefficient_mu    0.503
_exptl_absorpt_correction_type   'empirical PSI scan'
_exptl_crystal_density_diffrn    1.214
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3224
_refine_diff_density_max         1.690
_refine_diff_density_min         -1.003
_refine_diff_density_rms         0.207
_refine_ls_goodness_of_fit_ref   1.232
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     474
_refine_ls_number_reflns         8796
_refine_ls_number_restraints     208
_refine_ls_restrained_S_all      1.222
_refine_ls_R_factor_all          0.1655
_refine_ls_R_factor_gt           0.0957
_refine_ls_shift/su_max          0.563
_refine_ls_shift/su_mean         0.048
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2931
_refine_ls_wR_factor_ref         0.3399
_reflns_number_gt                4942
_reflns_number_total             8796
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic9811594_1.cif
_cod_data_source_block           2
_cod_original_cell_volume        8572.7(15)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4321844