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_7001072
_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            'C76 H68 Br4 O2 P4 Pd4'
_chemical_formula_weight         1882.42
_chemical_name_systematic
;
?
;
_space_group_IT_number           96
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'P 4nw 2abw'
_symmetry_space_group_name_H-M   'P 43 21 2'
_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                90.00
_cell_formula_units_Z            4
_cell_length_a                   22.135(3)
_cell_length_b                   22.135(3)
_cell_length_c                   15.515(3)
_cell_measurement_reflns_used    30291
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      0.998
_cell_volume                     7602(2)
_computing_cell_refinement       'Denzo & Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect(Nonius BV, 1997-2000)'
_computing_data_reduction        'Denzo & Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  0.2001
_diffrn_reflns_av_sigmaI/netI    0.1059
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            22385
_diffrn_reflns_theta_full        22.04
_diffrn_reflns_theta_max         22.04
_diffrn_reflns_theta_min         1.30
_exptl_absorpt_coefficient_mu    3.161
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.645
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             3696
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.005
_refine_diff_density_min         -2.103
_refine_diff_density_rms         0.363
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.03(2)
_refine_ls_extinction_coef       0.0050(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.192
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     384
_refine_ls_number_reflns         4670
_refine_ls_number_restraints     357
_refine_ls_restrained_S_all      1.156
_refine_ls_R_factor_all          0.0899
_refine_ls_R_factor_gt           0.0758
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1027P)^2^+18.7012P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1883
_refine_ls_wR_factor_ref         0.2020
_reflns_number_gt                4111
_reflns_number_total             4670
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b816803b.txt
_cod_data_source_block           SS-1
_cod_original_cell_volume        7601(2)
_cod_original_sg_symbol_H-M      P43212
_cod_database_code               7001072