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_4107144
_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         'C61 H86 Cu Ge3 I P6 Pd4 '
_chemical_formula_sum            'C61 H86 Cu Ge3 I P6 Pd4'
_chemical_formula_weight         1839.01
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_cell_angle_alpha                90.0000
_cell_angle_beta                 91.426(7)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   14.3194(18)
_cell_length_b                   29.746(6)
_cell_length_c                   16.545(4)
_cell_measurement_reflns_used    14121
_cell_measurement_temperature    113.1
_cell_measurement_theta_max      27.4
_cell_measurement_theta_min      3.0
_cell_volume                     7045(2)
_computing_cell_refinement       CrystalClear
_computing_data_collection       CrystalClear
_computing_data_reduction        CrystalStructure
_computing_publication_material  'CrystalStructure 3.8'
_computing_structure_refinement  SHELXL
_computing_structure_solution    SHELXS97
_diffrn_ambient_temperature      113.1
_diffrn_detector_area_resol_mean 7.31
_diffrn_measured_fraction_theta_full 0.968
_diffrn_measured_fraction_theta_max 0.968
_diffrn_measurement_device_type  'Rigaku Saturn'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.193
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            52551
_diffrn_reflns_theta_full        27.44
_diffrn_reflns_theta_max         27.44
_exptl_absorpt_coefficient_mu    3.163
_exptl_absorpt_correction_T_max  0.603
_exptl_absorpt_correction_T_min  0.265
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.734
_exptl_crystal_description       prism
_exptl_crystal_F_000             3616.00
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.92
_refine_diff_density_min         -2.11
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    refall
_refine_ls_number_parameters     686
_refine_ls_number_reflns         15588
_refine_ls_R_factor_all          0.1090
_refine_ls_R_factor_gt           0.0787
_refine_ls_shift/su_max          0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0555P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1844
_refine_ls_wR_factor_ref         0.2065
_reflns_number_gt                10921
_reflns_number_total             15588
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            ja208565q_si_002_4.cif
_cod_data_source_block           '__complex4'
_cod_original_formula_sum        'C61 H86 Cu Ge3 I P6 Pd4 '
_cod_database_code               4107144