Isolation of enantiomerically pure organometallic palladium compounds: synthesis of the triangles prepared from enantiopure [cis-Pd2(C6H4PPh2)2(NCCH3)4]2+
Koshevoy, Igor O.; Gutierrez-Puebla, Enrique; Lahuerta, Pascual; Monge, Angeles; Ubeda, M.Angeles; Sanaú, Mercedes; Dalton Transactions  (2009) 2993–2998; doi:10.1039/b816803b

data_7001070
_publ_section_title
;
 Isolation of enantiomerically pure organometallic palladium compounds:
 synthesis of the triangles prepared from enantiopure
 [cis-Pd2(C6H4PPh2)2(NCCH3)4]2+
;
_journal_issue                   16
_journal_name_full               'Dalton Transactions'
_journal_page_first              2993
_journal_page_last               2998
_journal_paper_doi               10.1039/b816803b
_journal_year                    2009
_chemical_formula_sum            'C150 H108 O12 P6 Pd6'
_chemical_formula_weight         2926.58
_chemical_name_systematic
;
?
;
_space_group_IT_number           146
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  'R 3'
_symmetry_space_group_name_H-M   'R 3 :H'
_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                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            3
_cell_length_a                   25.531(2)
_cell_length_b                   25.531(2)
_cell_length_c                   21.106(3)
_cell_measurement_reflns_used    4361
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      23.51
_cell_measurement_theta_min      2.62
_cell_volume                     11914(2)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0715
_diffrn_reflns_av_sigmaI/netI    0.0844
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            24992
_diffrn_reflns_theta_full        23.82
_diffrn_reflns_theta_max         24.74
_diffrn_reflns_theta_min         1.33
_exptl_absorpt_coefficient_mu    0.776
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.224
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             4410
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.18
_platon_squeeze_details
;
;
_refine_diff_density_max         3.360
_refine_diff_density_min         -0.498
_refine_diff_density_rms         0.144
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.09(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     416
_refine_ls_number_reflns         7621
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.0974
_refine_ls_R_factor_gt           0.0783
_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^)+(0.1371P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1920
_refine_ls_wR_factor_ref         0.2036
_reflns_number_gt                5884
_reflns_number_total             8343
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b816803b.txt
_cod_data_source_block           1bca
_cod_original_sg_symbol_H-M      R3
_cod_database_code               7001070