Superelectrophilic Tetrakis(carbonyl)palladium(II)- and -platinum(II) Undecafluorodiantimonate(V), [Pd(CO)4][Sb2F11]2 and [Pt(CO)4][Sb2F11]2: Syntheses, Physical and Spectroscopic Properties, Their Crystal, Molecular, and Extended Structures, and Density Functional Calculations: An Experimental, Computational, and Comparative Study
Helge Willner; Matthias Bodenbinder; Raimund Bröchler; Germaine Hwang; Steven J. Rettig; James Trotter; Britta von Ahsen; Ulrich Westphal; Volker Jonas; Walter Thiel; Friedhelm Aubke; Journal of the American Chemical Society 123 (2001) 588–602; doi:10.1021/ja002360s

data_4115424
_publ_contact_author_address
;
University of British Columbia
Department of Chemistry
2036 Main Mall
Vancouver, BC V6T 1Z1
Canada
;
_publ_contact_author_fax         604-822-2847
_publ_contact_author_name        'Prof. F. Aubke'
_publ_section_title
;
 Superelectrophilic Tetrakis(carbonyl)palladium(II)- and -platinum(II)
 Undecafluorodiantimonate(V), [Pd(CO)4][Sb2F11]2 and [Pt(CO)4][Sb2F11]2:
 Syntheses, Physical and Spectroscopic Properties, Their Crystal,
 Molecular, and Extended Structures, and Density Functional Calculations:
 An Experimental, Computational, and Comparative Study
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              588
_journal_page_last               602
_journal_paper_doi               10.1021/ja002360s
_journal_volume                  123
_journal_year                    2001
_chemical_formula_sum            'C4 F22 O4 Pd Sb4'
_chemical_formula_weight         1123.41
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_audit_creation_date             2000-08-29
_audit_creation_method           'by teXsan v1.8'
_audit_update_record
;
?
;
_cell_angle_alpha                90
_cell_angle_beta                 103.1183(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.583(2)
_cell_length_b                   9.8172(9)
_cell_length_c                   17.9895(9)
_cell_measurement_reflns_used    11367
_cell_measurement_temperature    180.2
_cell_measurement_theta_max      30.0
_cell_measurement_theta_min      2.0
_cell_volume                     2164.2(4)
_computing_cell_refinement       'd*TREK (MSC, 1996-1998)'
_computing_data_collection       'd*TREK (MSC, 1996-1998)'
_computing_data_reduction        'd*TREK (MSC, 1996-1998)'
_computing_publication_material  'teXsan (MSC, 1992-1997)'
_computing_structure_refinement  'teXsan (MSC, 1992-1997)'
_computing_structure_solution
;
DIRDIF92 PATTY (Beurskens, 1992)
;
_diffrn_ambient_temperature      180.2
_diffrn_detector_area_resol_mean 11.76
_diffrn_measurement_device_type  'Rigaku/ADSC CCD'
_diffrn_measurement_method       'area detector'
_diffrn_orient_matrix_UB_11      0.00000
_diffrn_orient_matrix_UB_12      0.00000
_diffrn_orient_matrix_UB_13      0.00000
_diffrn_orient_matrix_UB_21      0.00000
_diffrn_orient_matrix_UB_22      0.00000
_diffrn_orient_matrix_UB_23      0.00000
_diffrn_orient_matrix_UB_31      0.00000
_diffrn_orient_matrix_UB_32      0.00000
_diffrn_orient_matrix_UB_33      0.00000
_diffrn_radiation_detector       CCD
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'X-ray tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.03279
_diffrn_reflns_av_sigmaI/netI    0.070
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            19815
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_max         30.01
_diffrn_reflns_theta_min         2.08
_diffrn_standards_decay_%        0.00
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.935
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.644
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
d*TREK (MSC, 1996-1998)
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    3.448
_exptl_crystal_description       prism
_exptl_crystal_F_000             2016.00
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.30
_refine_diff_density_max         1.58
_refine_diff_density_min         -2.07
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.115
_refine_ls_goodness_of_fit_ref   1.110
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     316
_refine_ls_number_reflns         5593
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0560
_refine_ls_R_factor_gt           0.025
_refine_ls_shift/su_max          0.0010
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     'w = 1/[\s^2^(Fo^2^)]'
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_all         0.0466
_refine_ls_wR_factor_ref         0.022
_reflns_number_gt                5593
_reflns_number_total             5593
_reflns_threshold_expression     I>0.00\s(I)
_cod_data_source_file            ja002360s_2.cif
_cod_data_source_block           fa124/[Pd(CO)4][Sb2F11]2
_cod_original_sg_symbol_H-M      'P 21/c '
_cod_original_formula_sum        'C4 F22 O4 Pd Sb4 '
_cod_database_code               4115424