Tetrapalladium Complex with Bridging Germylene Ligands. Structural Change of the Planar Pd4Ge3 Core
Makoto Tanabe; Naoko Ishikawa; Mai Chiba; Tomohito Ide; Kohtaro Osakada; Tomoaki Tanase; Journal of the American Chemical Society 133 (2011) 18598–18601; doi:10.1021/ja208565q

data_4107143
_publ_contact_author_email       kosakada@res.titech.ac.jp
_publ_contact_author_fax         +81-45-924-5224
_publ_contact_author_name        'Kohtaro Osakada'
_publ_contact_author_phone       +81-45-924-5223
_publ_section_title
;
 Tetrapalladium Complex with Bridging Germylene Ligands. Structural Change
 of the Planar Pd4Ge3 Core
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              18598
_journal_page_last               18601
_journal_paper_doi               10.1021/ja208565q
_journal_volume                  133
_journal_year                    2011
_chemical_formula_moiety         'C110 H136 Ge6 P6 Pd6 S2'
_chemical_formula_sum            'C110 H136 Ge6 P6 Pd6 S2'
_chemical_formula_weight         2782.19
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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                98.179(9)
_cell_angle_beta                 99.519(7)
_cell_angle_gamma                102.421(8)
_cell_formula_units_Z            1
_cell_length_a                   13.830(7)
_cell_length_b                   14.631(8)
_cell_length_c                   16.860(8)
_cell_measurement_reflns_used    8732
_cell_measurement_temperature    163
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      3.07
_cell_volume                     3229(3)
_computing_cell_refinement       CrystalClear
_computing_data_collection       'CrystalClear (Rigaku/MSC Inc., 2006)'
_computing_data_reduction        CrystalClear
_computing_molecular_graphics    'CrystalStructure 3.8'
_computing_publication_material  'CrystalStructure 3.8'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    SIR97
_diffrn_ambient_temperature      163
_diffrn_detector_area_resol_mean 7.314
_diffrn_measured_fraction_theta_full 0.957
_diffrn_measured_fraction_theta_max 0.957
_diffrn_measurement_device_type  'Rigaku Saturn70'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0445
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            26252
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.332
_exptl_absorpt_correction_T_max  0.911
_exptl_absorpt_correction_T_min  0.578
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.431
_exptl_crystal_description       prism
_exptl_crystal_F_000             1386.00
_exptl_crystal_size_max          0.140
_exptl_crystal_size_mid          0.130
_exptl_crystal_size_min          0.040
_refine_diff_density_max         1.830
_refine_diff_density_min         -1.600
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    mixed
_refine_ls_number_parameters     590
_refine_ls_number_reflns         14137
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1080
_refine_ls_R_factor_gt           0.0789
_refine_ls_shift/su_max          0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.1391P)^2^+12.7702P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2363
_refine_ls_wR_factor_ref         0.2672
_reflns_number_gt                9787
_reflns_number_total             14137
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            ja208565q_si_002_3.cif
_cod_data_source_block           '_complex3'
_cod_database_code               4107143