data_pbfocl
 
_audit_creation_method            SHELXL-97
_chemical_name_systematic
;
 ?
;
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          ?
_chemical_formula_sum
 'Cl2 F2 O2 Pb4'
_chemical_formula_weight          969.66
 
loop_
 _atom_type_symbol
 _atom_type_description
 _atom_type_scat_dispersion_real
 _atom_type_scat_dispersion_imag
 _atom_type_scat_source
 'Cl'  'Cl'   0.1484   0.1585
 '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'
 'Pb'  'Pb'  -3.3944  10.1111
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'F'  'F'   0.0171   0.0103
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 
_symmetry_cell_setting            ?
_symmetry_space_group_name_H-M    ?
 
loop_
 _symmetry_equiv_pos_as_xyz
 'x, y, z'
 'x, -y, -z'
 '-x, -y, z'
 '-x, y, -z'
 'y, x, -z'
 'y, -x, z'
 '-y, x, z'
 '-y, -x, -z'
 'x+1/2, y+1/2, z+1/2'
 'x+1/2, -y+1/2, -z+1/2'
 '-x+1/2, -y+1/2, z+1/2'
 '-x+1/2, y+1/2, -z+1/2'
 'y+1/2, x+1/2, -z+1/2'
 'y+1/2, -x+1/2, z+1/2'
 '-y+1/2, x+1/2, z+1/2'
 '-y+1/2, -x+1/2, -z+1/2'
 '-x, -y, -z'
 '-x, y, z'
 'x, y, -z'
 'x, -y, z'
 '-y, -x, z'
 '-y, x, -z'
 'y, -x, -z'
 'y, x, z'
 '-x+1/2, -y+1/2, -z+1/2'
 '-x+1/2, y+1/2, z+1/2'
 'x+1/2, y+1/2, -z+1/2'
 'x+1/2, -y+1/2, z+1/2'
 '-y+1/2, -x+1/2, z+1/2'
 '-y+1/2, x+1/2, -z+1/2'
 'y+1/2, -x+1/2, -z+1/2'
 'y+1/2, x+1/2, z+1/2'
 
_cell_length_a                    4.0648(19)
_cell_length_b                    4.0648(19)
_cell_length_c                    12.631(7)
_cell_angle_alpha                 90.00
_cell_angle_beta                  90.00
_cell_angle_gamma                 90.00
_cell_volume                      208.70(18)
_cell_formula_units_Z             1
_cell_measurement_temperature     293(2)
_cell_measurement_reflns_used     ?
_cell_measurement_theta_min       ?
_cell_measurement_theta_max       ?
 
_exptl_crystal_description        ?
_exptl_crystal_colour             ?
_exptl_crystal_size_max           ?
_exptl_crystal_size_mid           ?
_exptl_crystal_size_min           ?
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     7.715
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              396
_exptl_absorpt_coefficient_mu     81.038
_exptl_absorpt_correction_type    ?
_exptl_absorpt_correction_T_min   ?
_exptl_absorpt_correction_T_max   ?
_exptl_absorpt_process_details    ?
 
_exptl_special_details
;
 ?
;
 
_diffrn_ambient_temperature       293(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   ?
_diffrn_measurement_method        ?
_diffrn_detector_area_resol_mean  ?
_diffrn_standards_number          ?
_diffrn_standards_interval_count  ?
_diffrn_standards_interval_time   ?
_diffrn_standards_decay_%         ?
_diffrn_reflns_number             93
_diffrn_reflns_av_R_equivalents   0.0000
_diffrn_reflns_av_sigmaI/netI     0.0651
_diffrn_reflns_limit_h_min        0
_diffrn_reflns_limit_h_max        3
_diffrn_reflns_limit_k_min        0
_diffrn_reflns_limit_k_max        5
_diffrn_reflns_limit_l_min        0
_diffrn_reflns_limit_l_max        16
_diffrn_reflns_theta_min          6.98
_diffrn_reflns_theta_max          27.83
_reflns_number_total              93
_reflns_number_gt                 64
_reflns_threshold_expression      >2sigma(I)
 
_computing_data_collection        ?
_computing_cell_refinement        ?
_computing_data_reduction         ?
_computing_structure_solution     ?
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics     ?
_computing_publication_material   ?
 
_refine_special_details
;
 Refinement of F^2^ against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F^2^, conventional R-factors R are based
 on F, with F set to zero for negative F^2^. The threshold expression of
 F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F^2^ 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/[\s^2^(Fo^2^)+(0.1323P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary      direct
_atom_sites_solution_secondary    difmap
_atom_sites_solution_hydrogens    geom
_refine_ls_hydrogen_treatment     mixed
_refine_ls_extinction_method      SHELXL
_refine_ls_extinction_coef        0.003(5)
_refine_ls_extinction_expression
 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^'
_refine_ls_number_reflns          93
_refine_ls_number_parameters      9
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.0993
_refine_ls_R_factor_gt            0.0709
_refine_ls_wR_factor_ref          0.2148
_refine_ls_wR_factor_gt           0.2023
_refine_ls_goodness_of_fit_ref    1.107
_refine_ls_restrained_S_all       1.107
_refine_ls_shift/su_max           0.000
_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
Pb1 Pb 0.0000 0.0000 0.1469(3) 0.061(2) Uani 1 8 d S . .
Cl1 Cl 0.5000 0.5000 0.0000 0.056(7) Uani 1 16 d S . .
O1 O -0.5000 0.0000 0.2500 0.049(11) Uani 0.50 8 d SP . .
F1 F -0.5000 0.0000 0.2500 0.049(11) Uani 0.50 8 d SP . .
 
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
Pb1 0.065(2) 0.065(2) 0.052(2) 0.000 0.000 0.000
Cl1 0.062(11) 0.062(11) 0.043(14) 0.000 0.000 0.000
O1 0.049(17) 0.049(17) 0.05(2) 0.000 0.000 0.000
F1 0.049(17) 0.049(17) 0.05(2) 0.000 0.000 0.000
 
_geom_special_details
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds 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
Pb1 F1 2.414(2) 25_455 ?
Pb1 F1 2.414(2) 1_655 ?
Pb1 O1 2.414(2) 25_455 ?
Pb1 O1 2.414(2) 1_655 ?
Pb1 F1 2.414(2) 25_445 ?
Pb1 O1 2.414(2) . ?
Pb1 O1 2.414(2) 25_445 ?
Pb1 Cl1 3.421(2) 1_445 ?
Pb1 Cl1 3.421(2) . ?
Pb1 Cl1 3.421(2) 1_455 ?
Pb1 Cl1 3.421(2) 1_545 ?
Cl1 Pb1 3.421(2) 17 ?
Cl1 Pb1 3.421(2) 1_665 ?
Cl1 Pb1 3.421(2) 17_665 ?
Cl1 Pb1 3.421(2) 1_655 ?
Cl1 Pb1 3.421(2) 1_565 ?
Cl1 Pb1 3.421(2) 17_655 ?
Cl1 Pb1 3.421(2) 17_565 ?
O1 Pb1 2.414(2) 25_455 ?
O1 Pb1 2.414(2) 1_455 ?
O1 Pb1 2.414(2) 25_445 ?
 
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
F1 Pb1 F1 73.08(7) 25_455 1_655 ?
F1 Pb1 O1 0.0 25_455 25_455 ?
F1 Pb1 O1 73.08(7) 1_655 25_455 ?
F1 Pb1 O1 73.08(7) 25_455 1_655 ?
F1 Pb1 O1 0.0 1_655 1_655 ?
O1 Pb1 O1 73.08(7) 25_455 1_655 ?
F1 Pb1 F1 114.71(16) 25_455 25_445 ?
F1 Pb1 F1 73.08(7) 1_655 25_445 ?
O1 Pb1 F1 114.71(16) 25_455 25_445 ?
O1 Pb1 F1 73.08(7) 1_655 25_445 ?
F1 Pb1 O1 73.08(7) 25_455 . ?
F1 Pb1 O1 114.71(16) 1_655 . ?
O1 Pb1 O1 73.08(7) 25_455 . ?
O1 Pb1 O1 114.71(16) 1_655 . ?
F1 Pb1 O1 73.08(7) 25_445 . ?
F1 Pb1 O1 114.71(16) 25_455 25_445 ?
F1 Pb1 O1 73.08(7) 1_655 25_445 ?
O1 Pb1 O1 114.71(16) 25_455 25_445 ?
O1 Pb1 O1 73.08(7) 1_655 25_445 ?
F1 Pb1 O1 0.0 25_445 25_445 ?
O1 Pb1 O1 73.08(7) . 25_445 ?
F1 Pb1 Cl1 142.448(10) 25_455 1_445 ?
F1 Pb1 Cl1 142.448(10) 1_655 1_445 ?
O1 Pb1 Cl1 142.448(10) 25_455 1_445 ?
O1 Pb1 Cl1 142.448(10) 1_655 1_445 ?
F1 Pb1 Cl1 78.02(4) 25_445 1_445 ?
O1 Pb1 Cl1 78.02(4) . 1_445 ?
O1 Pb1 Cl1 78.02(4) 25_445 1_445 ?
F1 Pb1 Cl1 78.02(4) 25_455 . ?
F1 Pb1 Cl1 78.02(4) 1_655 . ?
O1 Pb1 Cl1 78.02(4) 25_455 . ?
O1 Pb1 Cl1 78.02(4) 1_655 . ?
F1 Pb1 Cl1 142.448(10) 25_445 . ?
O1 Pb1 Cl1 142.448(10) . . ?
O1 Pb1 Cl1 142.448(10) 25_445 . ?
Cl1 Pb1 Cl1 114.30(11) 1_445 . ?
F1 Pb1 Cl1 78.02(4) 25_455 1_455 ?
F1 Pb1 Cl1 142.448(10) 1_655 1_455 ?
O1 Pb1 Cl1 78.02(4) 25_455 1_455 ?
O1 Pb1 Cl1 142.448(10) 1_655 1_455 ?
F1 Pb1 Cl1 142.448(10) 25_445 1_455 ?
O1 Pb1 Cl1 78.02(4) . 1_455 ?
O1 Pb1 Cl1 142.448(10) 25_445 1_455 ?
Cl1 Pb1 Cl1 72.89(5) 1_445 1_455 ?
Cl1 Pb1 Cl1 72.89(5) . 1_455 ?
F1 Pb1 Cl1 142.448(10) 25_455 1_545 ?
F1 Pb1 Cl1 78.02(4) 1_655 1_545 ?
O1 Pb1 Cl1 142.448(10) 25_455 1_545 ?
O1 Pb1 Cl1 78.02(4) 1_655 1_545 ?
F1 Pb1 Cl1 78.02(4) 25_445 1_545 ?
O1 Pb1 Cl1 142.448(10) . 1_545 ?
O1 Pb1 Cl1 78.02(4) 25_445 1_545 ?
Cl1 Pb1 Cl1 72.89(5) 1_445 1_545 ?
Cl1 Pb1 Cl1 72.89(5) . 1_545 ?
Cl1 Pb1 Cl1 114.30(11) 1_455 1_545 ?
Pb1 Cl1 Pb1 180.00(11) 17 1_665 ?
Pb1 Cl1 Pb1 65.70(11) 17 . ?
Pb1 Cl1 Pb1 114.30(11) 1_665 . ?
Pb1 Cl1 Pb1 114.30(11) 17 17_665 ?
Pb1 Cl1 Pb1 65.70(11) 1_665 17_665 ?
Pb1 Cl1 Pb1 180.00(11) . 17_665 ?
Pb1 Cl1 Pb1 107.11(5) 17 1_655 ?
Pb1 Cl1 Pb1 72.89(5) 1_665 1_655 ?
Pb1 Cl1 Pb1 72.89(5) . 1_655 ?
Pb1 Cl1 Pb1 107.11(5) 17_665 1_655 ?
Pb1 Cl1 Pb1 107.11(5) 17 1_565 ?
Pb1 Cl1 Pb1 72.89(5) 1_665 1_565 ?
Pb1 Cl1 Pb1 72.89(5) . 1_565 ?
Pb1 Cl1 Pb1 107.11(5) 17_665 1_565 ?
Pb1 Cl1 Pb1 114.30(11) 1_655 1_565 ?
Pb1 Cl1 Pb1 72.89(5) 17 17_655 ?
Pb1 Cl1 Pb1 107.11(5) 1_665 17_655 ?
Pb1 Cl1 Pb1 107.11(5) . 17_655 ?
Pb1 Cl1 Pb1 72.89(5) 17_665 17_655 ?
Pb1 Cl1 Pb1 65.70(11) 1_655 17_655 ?
Pb1 Cl1 Pb1 180.0 1_565 17_655 ?
Pb1 Cl1 Pb1 72.89(5) 17 17_565 ?
Pb1 Cl1 Pb1 107.11(5) 1_665 17_565 ?
Pb1 Cl1 Pb1 107.11(5) . 17_565 ?
Pb1 Cl1 Pb1 72.89(5) 17_665 17_565 ?
Pb1 Cl1 Pb1 180.00(11) 1_655 17_565 ?
Pb1 Cl1 Pb1 65.70(11) 1_565 17_565 ?
Pb1 Cl1 Pb1 114.30(11) 17_655 17_565 ?
Pb1 O1 Pb1 106.92(7) 25_455 1_455 ?
Pb1 O1 Pb1 114.71(16) 25_455 25_445 ?
Pb1 O1 Pb1 106.92(8) 1_455 25_445 ?
Pb1 O1 Pb1 106.92(8) 25_455 . ?
Pb1 O1 Pb1 114.71(16) 1_455 . ?
Pb1 O1 Pb1 106.92(8) 25_445 . ?
 
_diffrn_measured_fraction_theta_max    0.930
_diffrn_reflns_theta_full              27.83
_diffrn_measured_fraction_theta_full   0.930
_refine_diff_density_max    2.900
_refine_diff_density_min   -2.366
_refine_diff_density_rms    0.643