Mono- and di-nuclear palladium(ii) complexes with bulky arsino(phosphino)methanes in different coordination modes
Schmidt, Ulrich; Ilg, Kerstin; Brandt, Carsten D.; Werner, Helmut; Journal of the Chemical Society, Dalton Transactions  (2002) 2815–; doi:10.1039/b202879b

data_7011688
_publ_section_title
;
 Mono- and di-nuclear palladium(ii) complexes with bulky
 arsino(phosphino)methanes in different coordination modes
;
_journal_issue                   14
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              2815
_journal_paper_doi               10.1039/b202879b
_journal_year                    2002
_chemical_formula_sum            'C18 H39 As F6 P2 Pd'
_chemical_formula_weight         612.75
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 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                 113.81(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.0217(18)
_cell_length_b                   17.072(3)
_cell_length_c                   9.0882(18)
_cell_measurement_reflns_used    5000
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.00
_cell_measurement_theta_min      2.28
_cell_volume                     1280.6(5)
_computing_cell_refinement       'IPDS (STOE)'
_computing_data_collection       'IPDS (STOE)'
_computing_data_reduction        'IPDS (STOE)'
_computing_molecular_graphics    'Zortep (Zsolnay)'
_computing_publication_material  'Zortep (Zsolnay)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'IPDS (STOE)'
_diffrn_measurement_method       'IPDS (STOE)'
_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  0.0414
_diffrn_reflns_av_sigmaI/netI    0.0323
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            17768
_diffrn_reflns_theta_full        27.99
_diffrn_reflns_theta_max         27.99
_diffrn_reflns_theta_min         2.39
_exptl_absorpt_coefficient_mu    2.177
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.589
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             620
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.30
_refine_diff_density_max         1.014
_refine_diff_density_min         -0.567
_refine_diff_density_rms         0.069
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.002(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     347
_refine_ls_number_reflns         6094
_refine_ls_number_restraints     121
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0278
_refine_ls_R_factor_gt           0.0251
_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^)+(0.0373P)^2^+0.1233P] where 
P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0610
_refine_ls_wR_factor_ref         0.0620
_reflns_number_gt                5713
_reflns_number_total             6094
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b202879b.txt
_cod_data_source_block           us2cbm
_cod_original_cell_volume        1280.6(4)
_cod_original_sg_symbol_H-M      P21
_cod_database_code               7011688