 
data_o2pdf6
 
_audit_creation_method            SHELXL-97
_chemical_name_systematic
;
 Dioxygenyl trihydrogen dodecafluorido dipalladate
;
_chemical_name_common             Dioxygenyl_hexafluorido_palladate
_chemical_melting_point           ?
_chemical_formula_moiety          F12H3O2Pd2
_chemical_formula_sum
 ' F12 H3 O2 Pd2'
_chemical_formula_weight          475.82
 
loop_
 _atom_type_symbol
 _atom_type_description
 _atom_type_scat_dispersion_real
 _atom_type_scat_dispersion_imag
 _atom_type_scat_source
 'F'  'F'   0.0171   0.0103
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Pd'  'Pd'  -0.9988   1.0072
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'O'  'O'   0.0106   0.0060
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'H'  'H'   0.0000   0.0000
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 
_symmetry_cell_setting            triclinic
_symmetry_space_group_name_H-M    P-1
 
loop_
 _symmetry_equiv_pos_as_xyz
 'x, y, z'
 '-x, -y, -z'
 
_cell_length_a                    5.585(3)
_cell_length_b                    9.744(7)
_cell_length_c                    9.784(6)
_cell_angle_alpha                 112.28(5)
_cell_angle_beta                  100.09(5)
_cell_angle_gamma                 102.60(5)
_cell_volume                      460.8(5)
_cell_formula_units_Z             2
_cell_measurement_temperature     133(2)
_cell_measurement_reflns_used     999
_cell_measurement_theta_min       2.0
_cell_measurement_theta_max       21.1
 
_exptl_crystal_description        platelet
_exptl_crystal_colour             orange
_exptl_crystal_size_max           .1
_exptl_crystal_size_mid           .1
_exptl_crystal_size_min           0.03
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     3.429
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              438
_exptl_absorpt_coefficient_mu     4.082
_exptl_absorpt_correction_type    multi-scan
_exptl_absorpt_correction_T_min   0.687
_exptl_absorpt_correction_T_max   1.000
_exptl_absorpt_process_details    Bruker_2000_NT_Software_Reference_Manual
 
_exptl_special_details
;
 ?
;
 
_diffrn_ambient_temperature       133(2)
_diffrn_radiation_wavelength      0.71073
_diffrn_radiation_type            MoK\a
_diffrn_radiation_source          'fine-focus sealed tube'
_diffrn_radiation_monochromator   graphite
_diffrn_measurement_device_type   Bruker_CCD
_diffrn_measurement_method        omega_scan
_diffrn_detector_area_resol_mean  ?
_diffrn_standards_number          ?
_diffrn_standards_interval_count  ?
_diffrn_standards_interval_time   ?
_diffrn_standards_decay_%         none
_diffrn_reflns_number             3774
_diffrn_reflns_av_R_equivalents   0.0109
_diffrn_reflns_av_sigmaI/netI     0.0210
_diffrn_reflns_limit_h_min        -7
_diffrn_reflns_limit_h_max        7
_diffrn_reflns_limit_k_min        -12
_diffrn_reflns_limit_k_max        11
_diffrn_reflns_limit_l_min        -9
_diffrn_reflns_limit_l_max        13
_diffrn_reflns_theta_min          2.35
_diffrn_reflns_theta_max          30.47
_reflns_number_total              2557
_reflns_number_gt                 2306
_reflns_threshold_expression      >2σ(I)
 
_computing_data_collection        Bruker_ShELXTL
_computing_cell_refinement        Bruker_ShELXTL
_computing_data_reduction         Bruker_ShELXTL
_computing_structure_solution     Bruker_ShELXTL
_computing_structure_refinement   'SHELXL (Sheldrick, 2008)'
_computing_molecular_graphics     ?
_computing_publication_material   ?
 
_refine_special_details
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2σ(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;
 
_refine_ls_structure_factor_coef  Fsqd
_refine_ls_matrix_type            full
_refine_ls_weighting_scheme       calc
_refine_ls_weighting_details
 'calc w=1/[σ²(Fo²)+(0.0263P)²+0.9277P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary      direct
_atom_sites_solution_secondary    difmap
_atom_sites_solution_hydrogens    refall
_refine_ls_hydrogen_treatment     refall
_refine_ls_extinction_method      none
_refine_ls_extinction_coef        none
_refine_ls_number_reflns          2557
_refine_ls_number_parameters      157
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.0260
_refine_ls_R_factor_gt            0.0220
_refine_ls_wR_factor_ref          0.0541
_refine_ls_wR_factor_gt           0.0521
_refine_ls_goodness_of_fit_ref    1.054
_refine_ls_restrained_S_all       1.054
_refine_ls_shift/su_max           0.001
_refine_ls_shift/su_mean          0.000
 
loop_
 _atom_site_label
 _atom_site_type_symbol
 _atom_site_fract_x
 _atom_site_fract_y
 _atom_site_fract_z
 _atom_site_U_iso_or_equiv
 _atom_site_adp_type
 _atom_site_occupancy
 _atom_site_symmetry_multiplicity
 _atom_site_calc_flag
 _atom_site_refinement_flags
 _atom_site_disorder_assembly
 _atom_site_disorder_group
F1 F -0.1786(3) 0.1579(2) -0.3149(2) 0.0187(4) Uani 1 1 d . . .
F2 F 0.0685(3) 0.3712(2) -0.0377(2) 0.0193(4) Uani 1 1 d . . .
F3 F 0.2450(3) 0.3723(2) -0.2654(2) 0.0181(4) Uani 1 1 d . . .
F4 F 0.5135(3) 0.3007(2) -0.0636(2) 0.0183(4) Uani 1 1 d . . .
F5 F 0.2460(4) 0.0707(2) -0.3563(2) 0.0186(4) Uani 1 1 d . . .
F6 F 0.0610(3) 0.0681(2) -0.1128(2) 0.0155(3) Uani 1 1 d . . .
F7 F 0.3908(4) 0.2109(2) 0.4353(2) 0.0219(4) Uani 1 1 d . . .
F8 F 0.2828(3) 0.3011(2) 0.2136(2) 0.0192(4) Uani 1 1 d . . .
F9 F 0.7205(4) 0.4462(2) 0.4349(2) 0.0211(4) Uani 1 1 d . . .
F10 F 0.7202(3) 0.2710(2) 0.1416(2) 0.0176(4) Uani 1 1 d . . .
F11 F 0.8310(3) 0.1792(2) 0.3785(2) 0.0188(4) Uani 1 1 d . . .
F12 F 0.3698(3) 0.0202(2) 0.1411(2) 0.0167(3) Uani 1 1 d . . .
O1 O 0.7099(5) 0.3937(4) 0.7260(4) 0.0372(7) Uani 1 1 d . . .
O2 O 0.8520(6) 0.4669(4) 0.7114(4) 0.0394(7) Uani 1 1 d . . .
Pd1 Pd 0.15618(4) 0.22448(2) -0.19048(2) 0.01104(6) Uani 1 1 d . . .
Pd2 Pd 0.54808(4) 0.24040(3) 0.29358(2) 0.01161(6) Uani 1 1 d . . .
H2 H 0.621(12) 0.281(7) 0.057(7) 0.08(2) Uiso 1 1 d . . .
H3 H 0.198(11) -0.053(7) -0.369(7) 0.060(17) Uiso 1 1 d . . .
H1 H 0.218(14) -0.006(8) 0.128(8) 0.09(2) Uiso 1 1 d . . .
 
loop_
 _atom_site_aniso_label
 _atom_site_aniso_U_11
 _atom_site_aniso_U_22
 _atom_site_aniso_U_33
 _atom_site_aniso_U_23
 _atom_site_aniso_U_13
 _atom_site_aniso_U_12
F1 0.0128(7) 0.0216(10) 0.0193(9) 0.0098(8) -0.0013(6) 0.0038(7)
F2 0.0224(8) 0.0159(9) 0.0194(9) 0.0051(7) 0.0089(7) 0.0082(7)
F3 0.0218(8) 0.0154(9) 0.0230(9) 0.0133(7) 0.0083(7) 0.0067(7)
F4 0.0126(7) 0.0224(10) 0.0198(9) 0.0127(8) 0.0015(6) 0.0015(7)
F5 0.0255(9) 0.0176(9) 0.0190(9) 0.0101(7) 0.0102(7) 0.0113(7)
F6 0.0150(7) 0.0154(9) 0.0194(8) 0.0120(7) 0.0046(6) 0.0034(6)
F7 0.0248(9) 0.0276(11) 0.0196(9) 0.0128(8) 0.0137(7) 0.0091(8)
F8 0.0174(8) 0.0206(10) 0.0227(9) 0.0116(8) 0.0035(7) 0.0095(7)
F9 0.0249(9) 0.0105(9) 0.0206(9) 0.0035(7) 0.0009(7) 0.0023(7)
F10 0.0141(7) 0.0247(10) 0.0186(9) 0.0138(8) 0.0059(7) 0.0057(7)
F11 0.0175(8) 0.0167(9) 0.0225(9) 0.0104(7) 0.0017(7) 0.0057(7)
F12 0.0153(8) 0.0115(9) 0.0191(8) 0.0042(7) 0.0040(7) 0.0015(6)
O1 0.0299(14) 0.061(2) 0.0426(16) 0.0326(16) 0.0193(12) 0.0299(14)
O2 0.0325(14) 0.0332(17) 0.058(2) 0.0308(15) 0.0022(13) 0.0088(12)
Pd1 0.01114(9) 0.01102(11) 0.01269(10) 0.00667(8) 0.00351(7) 0.00384(7)
Pd2 0.01176(9) 0.01139(11) 0.01250(10) 0.00625(8) 0.00307(7) 0.00356(7)
 
_geom_special_details
;
 All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell s.u.'s are taken
 into account individually in the estimation of s.u.'s in distances, angles
 and torsion angles; correlations between s.u.'s in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes.
;
 
loop_
 _geom_bond_atom_site_label_1
 _geom_bond_atom_site_label_2
 _geom_bond_distance
 _geom_bond_site_symmetry_2
 _geom_bond_publ_flag
F1 Pd1 1.864(2) . ?
F2 Pd1 1.860(2) . ?
F3 Pd1 1.864(2) . ?
F4 Pd1 1.965(2) . ?
F4 H2 1.33(7) . ?
F5 Pd1 1.975(2) . ?
F5 H3 1.13(6) . ?
F6 Pd1 1.961(2) . ?
F7 Pd2 1.843(2) . ?
F8 Pd2 1.866(2) . ?
F9 Pd2 1.857(3) . ?
F10 Pd2 1.984(2) . ?
F10 H2 0.96(7) . ?
F11 Pd2 1.967(2) . ?
F12 Pd2 1.985(3) . ?
F12 H1 0.80(7) . ?
O1 O2 1.014(4) . ?
 
loop_
 _geom_angle_atom_site_label_1
 _geom_angle_atom_site_label_2
 _geom_angle_atom_site_label_3
 _geom_angle
 _geom_angle_site_symmetry_1
 _geom_angle_site_symmetry_3
 _geom_angle_publ_flag
Pd1 F4 H2 131(3) . . ?
Pd1 F5 H3 118(3) . . ?
Pd2 F10 H2 118(4) . . ?
Pd2 F12 H1 113(5) . . ?
F2 Pd1 F1 88.43(11) . . ?
F2 Pd1 F3 88.21(10) . . ?
F1 Pd1 F3 89.38(10) . . ?
F2 Pd1 F6 91.93(10) . . ?
F1 Pd1 F6 90.30(9) . . ?
F3 Pd1 F6 179.65(8) . . ?
F2 Pd1 F4 91.77(10) . . ?
F1 Pd1 F4 177.50(8) . . ?
F3 Pd1 F4 88.14(9) . . ?
F6 Pd1 F4 92.18(9) . . ?
F2 Pd1 F5 178.57(8) . . ?
F1 Pd1 F5 90.71(10) . . ?
F3 Pd1 F5 90.64(10) . . ?
F6 Pd1 F5 89.22(9) . . ?
F4 Pd1 F5 89.04(10) . . ?
F7 Pd2 F9 89.75(10) . . ?
F7 Pd2 F8 91.51(10) . . ?
F9 Pd2 F8 90.37(11) . . ?
F7 Pd2 F11 88.92(9) . . ?
F9 Pd2 F11 88.97(11) . . ?
F8 Pd2 F11 179.21(8) . . ?
F7 Pd2 F10 179.35(8) . . ?
F9 Pd2 F10 90.37(10) . . ?
F8 Pd2 F10 89.13(9) . . ?
F11 Pd2 F10 90.44(9) . . ?
F7 Pd2 F12 91.16(10) . . ?
F9 Pd2 F12 178.87(8) . . ?
F8 Pd2 F12 90.28(11) . . ?
F11 Pd2 F12 90.37(10) . . ?
F10 Pd2 F12 88.72(9) . . ?
 
_diffrn_measured_fraction_theta_max    0.974
_diffrn_reflns_theta_full              30.47
_diffrn_measured_fraction_theta_full   0.914
_refine_diff_density_max    0.871
_refine_diff_density_min   -1.038
_refine_diff_density_rms    0.142
