Bis-cyclooctatetraene tripalladium sandwich complexes
Tetsuro Murahashi; Seita Kimura; Kohei Takase; Tomohito Uemura; Sensuke Ogoshi; Koji Yamamoto; Chem.Commun. 50 (2014) 820–; doi:10.1039/c3cc47515h

data_7110254
_publ_section_title
;
 Bis-cyclooctatetraene tripalladium sandwich complexes
;
_journal_name_full               Chem.Commun.
_journal_page_first              820
_journal_paper_doi               10.1039/c3cc47515h
_journal_volume                  50
_journal_year                    2014
_chemical_formula_moiety         'C80 H68 P4 Pd2, 2(B F4), C H2 Cl2'
_chemical_formula_sum            'C81 H70 B2 Cl2 F8 P4 Pd2'
_chemical_formula_weight         1624.57
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 93.6780(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   25.3856(12)
_cell_length_b                   24.7751(10)
_cell_length_c                   11.8833(6)
_cell_measurement_reflns_used    15270
_cell_measurement_temperature    123
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      3.09
_cell_volume                     7458.4(6)
_computing_cell_refinement       'RAPID AUTO'
_computing_data_collection       'RAPID AUTO (Rigaku)'
_computing_data_reduction        'RAPID AUTO'
_computing_molecular_graphics    'CrystalStructure 4.0'
_computing_publication_material  'CrystalStructure 4.0 (Rigaku, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR92 (Altomare, et al., 1994)'
_diffrn_ambient_temperature      123(2)
_diffrn_detector_area_resol_mean 10.000
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Mo K\a'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0764
_diffrn_reflns_av_sigmaI/netI    0.0688
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            36530
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.08
_exptl_absorpt_coefficient_mu    0.703
_exptl_absorpt_correction_T_max  0.9330
_exptl_absorpt_correction_T_min  0.9330
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Rigaku, 1995)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.447
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             3296
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_platon_squeeze_details
;
The cell contains 4 methylene chloride molecules which have been
treated as a diffuse contribution to the overall scattering without
specific atom positions by SQUEEZE/PLATON.
;
_refine_diff_density_max         0.980
_refine_diff_density_min         -1.791
_refine_diff_density_rms         0.142
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.913
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     408
_refine_ls_number_reflns         8540
_refine_ls_number_restraints     58
_refine_ls_restrained_S_all      0.914
_refine_ls_R_factor_all          0.1153
_refine_ls_R_factor_gt           0.0727
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2067
_refine_ls_wR_factor_ref         0.2643
_reflns_number_gt                5150
_reflns_number_total             8540
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3cc47515h.txt
_cod_data_source_block           1
_cod_database_code               7110254