Preparation and NMR Studies of Palladium Complexes with a Silsesquioxanate Ligand
Tanabe, Makoto; Mutou, Kohji; Mintcheva, Neli; Osakada, Kohtaro; Organometallics 27 (2008) 519–; doi:10.1021/om700827f

data_4070598
_publ_section_title
;
 Preparation and NMR Studies of Palladium Complexes with a
 Silsesquioxanate Ligand
;
_journal_issue                   4
_journal_name_full               Organometallics
_journal_page_first              519
_journal_paper_doi               10.1021/om700827f
_journal_volume                  27
_journal_year                    2008
_chemical_formula_moiety         'C51 H88 F5 O12 P2 Pd Si7 '
_chemical_formula_sum            'C51 H88 F5 O12 P2 Pd Si7'
_chemical_formula_weight         1353.19
_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'
_cell_angle_alpha                102.186(7)
_cell_angle_beta                 99.416(5)
_cell_angle_gamma                91.966(7)
_cell_formula_units_Z            2
_cell_length_a                   13.700(6)
_cell_length_b                   14.054(6)
_cell_length_c                   17.196(7)
_cell_measurement_reflns_used    6360
_cell_measurement_temperature    113.1
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.0
_cell_volume                     3185(2)
_computing_cell_refinement       CrystalClear
_computing_data_collection       CrystalClear
_computing_data_reduction        CrystalStructure
_computing_publication_material  'CrystalStructure 3.7.0'
_computing_structure_refinement  CRYSTALS
_computing_structure_solution    SIR97
_diffrn_detector_area_resol_mean 7.31
_diffrn_measured_fraction_theta_full 0.881
_diffrn_measured_fraction_theta_max 0.881
_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  0.027
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            20863
_diffrn_reflns_theta_full        27.45
_diffrn_reflns_theta_max         27.45
_exptl_absorpt_coefficient_mu    0.542
_exptl_absorpt_correction_T_max  0.922
_exptl_absorpt_correction_T_min  0.821
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.411
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1418.00
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.15
_refine_diff_density_max         2.04
_refine_diff_density_min         -1.19
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    mixed
_refine_ls_number_parameters     797
_refine_ls_number_reflns         10188
_refine_ls_R_factor_gt           0.0603
_refine_ls_shift/su_max          0.0008
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[0.0010Fo^2^ + 3.0000\s(Fo^2^) + 0.5000]/(4Fo^2^)'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1326
_reflns_number_gt                10091
_reflns_number_total             12827
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            om700827f-file001.cif
_cod_data_source_block           PdC6F5(Cy7Si7O10(OH)2)(PMe3)2
_cod_original_formula_sum        'C51 H88 F5 O12 P2 Pd Si7 '
_cod_database_code               4070598