Tri(allyl)- and tri(methylallyl)arsine complexes of palladium(ii) and platinum(ii): synthesis, spectroscopy, photochemistry and structures
Phadnis, Prasad P.; Jain, Vimal K.; Klein, Axel; Schurr, Thilo; Kaim, Wolfgang; New Journal of Chemistry 27 (2003) 1584–; doi:10.1039/b303990k

data_7050607
_publ_section_title
;
 Tri(allyl)- and tri(methylallyl)arsine complexes of palladium(ii) and
 platinum(ii): synthesis, spectroscopy, photochemistry and structures
;
_journal_issue                   11
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              1584
_journal_paper_doi               10.1039/b303990k
_journal_volume                  27
_journal_year                    2003
_chemical_formula_sum            'C18 H30 As2 Br2 Pd'
_chemical_formula_weight         662.49
_chemical_name_common            trans-Dibromobis(triallylarsine)palladium(ii)
_chemical_name_systematic        trans-Dibromobis(triallylarsine)palladium(II)
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_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                 90.000(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            12
_cell_length_a                   8.21980(10)
_cell_length_b                   18.41340(10)
_cell_length_c                   49.8803(5)
_cell_measurement_temperature    293(2)
_cell_volume                     7549.61(13)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.964
_diffrn_measured_fraction_theta_max 0.964
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       CCD
_diffrn_orient_matrix_type       'by Nonius Collect from scalepack cell'
_diffrn_orient_matrix_UB_11      -0.0035058
_diffrn_orient_matrix_UB_12      0.0460827
_diffrn_orient_matrix_UB_13      0.0105923
_diffrn_orient_matrix_UB_21      0.1130941
_diffrn_orient_matrix_UB_22      0.0117867
_diffrn_orient_matrix_UB_23      -0.0059715
_diffrn_orient_matrix_UB_31      -0.0446987
_diffrn_orient_matrix_UB_32      0.0262078
_diffrn_orient_matrix_UB_33      -0.0159394
_diffrn_radiation_monochromator  'horizonally mounted graphite crystal'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0633
_diffrn_reflns_av_sigmaI/netI    0.0418
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       57
_diffrn_reflns_limit_l_min       -52
_diffrn_reflns_number            33313
_diffrn_reflns_theta_full        24.12
_diffrn_reflns_theta_max         24.12
_diffrn_reflns_theta_min         2.61
_exptl_absorpt_coefficient_mu    6.521
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   '94 reflections'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.749
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             3840
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.550
_refine_diff_density_min         -0.466
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.301
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     304
_refine_ls_number_reflns         5797
_refine_ls_number_restraints     17
_refine_ls_restrained_S_all      1.299
_refine_ls_R_factor_all          0.0841
_refine_ls_R_factor_gt           0.0539
_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^)+(0.0571P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1183
_refine_ls_wR_factor_ref         0.1270
_reflns_number_gt                4184
_reflns_number_total             5797
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b303990k.txt
_cod_data_source_block           akfeb03
_cod_original_sg_symbol_H-M      Pbca
_cod_database_code               7050607