data_shelxl
 
_audit_creation_method            SHELXL-97
_chemical_name_systematic
;
 ?
;
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          ?
_chemical_formula_sum
 'H I O Pb'
_chemical_formula_weight          351.10
 
loop_
 _atom_type_symbol
 _atom_type_description
 _atom_type_scat_dispersion_real
 _atom_type_scat_dispersion_imag
 _atom_type_scat_source
 'O'  'O'   0.0106   0.0060
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'I'  'I'  -0.4742   1.8119
 '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'
 'H'  'H'   0.0000   0.0000
 '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+1/2, -y, z+1/2'
 '-x, y+1/2, -z'
 'x+1/2, -y+1/2, -z+1/2'
 '-x, -y, -z'
 'x-1/2, y, -z-1/2'
 'x, -y-1/2, z'
 '-x-1/2, y-1/2, z-1/2'
 
_cell_length_a                    7.8244(8)
_cell_length_b                    4.2107(4)
_cell_length_c                    10.4724(10)
_cell_angle_alpha                 90.00
_cell_angle_beta                  90.00
_cell_angle_gamma                 90.00
_cell_volume                      345.03(6)
_cell_formula_units_Z             4
_cell_measurement_temperature     296(2)
_cell_measurement_reflns_used     ?
_cell_measurement_theta_min       ?
_cell_measurement_theta_max       ?
 
_exptl_crystal_description        ?
_exptl_crystal_colour             ?
_exptl_crystal_size_max           0.12
_exptl_crystal_size_mid           0.10
_exptl_crystal_size_min           0.09
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     6.759
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              576
_exptl_absorpt_coefficient_mu     57.576
_exptl_absorpt_correction_type    ?
_exptl_absorpt_correction_T_min   ?
_exptl_absorpt_correction_T_max   ?
_exptl_absorpt_process_details    ?
 
_exptl_special_details
;
 ?
;
 
_diffrn_ambient_temperature       296(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             166
_diffrn_reflns_av_R_equivalents   0.0201
_diffrn_reflns_av_sigmaI/netI     0.0317
_diffrn_reflns_limit_h_min        -3
_diffrn_reflns_limit_h_max        5
_diffrn_reflns_limit_k_min        -5
_diffrn_reflns_limit_k_max        1
_diffrn_reflns_limit_l_min        -7
_diffrn_reflns_limit_l_max        13
_diffrn_reflns_theta_min          3.89
_diffrn_reflns_theta_max          29.52
_reflns_number_total              146
_reflns_number_gt                 129
_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^)+(0.0083P)^2^+65.1995P] 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        0.0000(12)
_refine_ls_extinction_expression
 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^'
_refine_ls_number_reflns          146
_refine_ls_number_parameters      22
_refine_ls_number_restraints      2
_refine_ls_R_factor_all           0.0521
_refine_ls_R_factor_gt            0.0405
_refine_ls_wR_factor_ref          0.1146
_refine_ls_wR_factor_gt           0.0766
_refine_ls_goodness_of_fit_ref    1.314
_refine_ls_restrained_S_all       1.312
_refine_ls_shift/su_max           0.418
_refine_ls_shift/su_mean          0.064
 
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 0.8194(6) 0.2500 0.58142(19) 0.0169(18) Uani 1 2 d S . .
I1 I 0.5471(9) 0.2500 0.3206(3) 0.017(3) Uani 1 2 d SD . .
O1 O 0.881(6) -0.2500 0.473(3) 0.02(3) Uani 1 2 d SD . .
H1 H 0.76(4) -0.2500 0.41(5) 0.050 Uiso 1 2 d SD . .
 
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 0.011(5) 0.0159(11) 0.0239(14) 0.000 0.0065(15) 0.000
I1 0.021(8) 0.0146(15) 0.0148(18) 0.000 0.002(2) 0.000
O1 0.03(9) 0.006(15) 0.02(2) 0.000 -0.01(3) 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 O1 2.42(5) 5_756 ?
Pb1 O1 2.44(2) . ?
Pb1 O1 2.44(2) 1_565 ?
Pb1 I1 3.435(4) 2_665 ?
Pb1 I1 3.435(4) 2_655 ?
Pb1 I1 3.464(6) . ?
Pb1 I1 3.703(6) 5_656 ?
Pb1 I1 3.703(6) 5_666 ?
Pb1 Pb1 3.915(7) 5_766 ?
Pb1 Pb1 3.915(7) 5_756 ?
Pb1 Pb1 4.2107(4) 1_565 ?
Pb1 Pb1 4.2107(4) 1_545 ?
I1 Pb1 3.435(4) 2_654 ?
I1 Pb1 3.435(4) 2_664 ?
I1 Pb1 3.703(6) 5_656 ?
I1 Pb1 3.703(6) 5_666 ?
O1 Pb1 2.42(5) 5_756 ?
O1 Pb1 2.44(2) 1_545 ?
 
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
O1 Pb1 O1 72.5(12) 5_756 . ?
O1 Pb1 O1 72.5(12) 5_756 1_565 ?
O1 Pb1 O1 119.3(17) . 1_565 ?
O1 Pb1 I1 82.9(6) 5_756 2_665 ?
O1 Pb1 I1 144.0(9) . 2_665 ?
O1 Pb1 I1 75.6(7) 1_565 2_665 ?
O1 Pb1 I1 82.9(6) 5_756 2_655 ?
O1 Pb1 I1 75.6(7) . 2_655 ?
O1 Pb1 I1 144.0(9) 1_565 2_655 ?
I1 Pb1 I1 75.61(9) 2_665 2_655 ?
O1 Pb1 I1 114.3(8) 5_756 . ?
O1 Pb1 I1 75.8(9) . . ?
O1 Pb1 I1 75.8(9) 1_565 . ?
I1 Pb1 I1 139.65(8) 2_665 . ?
I1 Pb1 I1 139.65(8) 2_655 . ?
O1 Pb1 I1 144.89(14) 5_756 5_656 ?
O1 Pb1 I1 77.9(11) . 5_656 ?
O1 Pb1 I1 140.5(11) 1_565 5_656 ?
I1 Pb1 I1 112.46(11) 2_665 5_656 ?
I1 Pb1 I1 71.63(6) 2_655 5_656 ?
I1 Pb1 I1 75.06(12) . 5_656 ?
O1 Pb1 I1 144.89(15) 5_756 5_666 ?
O1 Pb1 I1 140.5(11) . 5_666 ?
O1 Pb1 I1 77.9(11) 1_565 5_666 ?
I1 Pb1 I1 71.63(6) 2_665 5_666 ?
I1 Pb1 I1 112.46(11) 2_655 5_666 ?
I1 Pb1 I1 75.06(12) . 5_666 ?
I1 Pb1 I1 69.31(13) 5_656 5_666 ?
O1 Pb1 Pb1 36.5(3) 5_756 5_766 ?
O1 Pb1 Pb1 96.9(11) . 5_766 ?
O1 Pb1 Pb1 36.0(11) 1_565 5_766 ?
I1 Pb1 Pb1 76.61(11) 2_665 5_766 ?
I1 Pb1 Pb1 115.3(2) 2_655 5_766 ?
I1 Pb1 Pb1 95.77(10) . 5_766 ?
I1 Pb1 Pb1 170.26(13) 5_656 5_766 ?
I1 Pb1 Pb1 111.96(7) 5_666 5_766 ?
O1 Pb1 Pb1 36.5(3) 5_756 5_756 ?
O1 Pb1 Pb1 36.0(11) . 5_756 ?
O1 Pb1 Pb1 96.9(11) 1_565 5_756 ?
I1 Pb1 Pb1 115.3(2) 2_665 5_756 ?
I1 Pb1 Pb1 76.61(11) 2_655 5_756 ?
I1 Pb1 Pb1 95.77(10) . 5_756 ?
I1 Pb1 Pb1 111.96(7) 5_656 5_756 ?
I1 Pb1 Pb1 170.26(13) 5_666 5_756 ?
Pb1 Pb1 Pb1 65.06(13) 5_766 5_756 ?
O1 Pb1 Pb1 90.000(2) 5_756 1_565 ?
O1 Pb1 Pb1 149.7(8) . 1_565 ?
O1 Pb1 Pb1 30.3(8) 1_565 1_565 ?
I1 Pb1 Pb1 52.20(5) 2_665 1_565 ?
I1 Pb1 Pb1 127.80(5) 2_655 1_565 ?
I1 Pb1 Pb1 90.0 . 1_565 ?
I1 Pb1 Pb1 124.65(7) 5_656 1_565 ?
I1 Pb1 Pb1 55.35(7) 5_666 1_565 ?
Pb1 Pb1 Pb1 57.47(7) 5_766 1_565 ?
Pb1 Pb1 Pb1 122.53(7) 5_756 1_565 ?
O1 Pb1 Pb1 90.000(2) 5_756 1_545 ?
O1 Pb1 Pb1 30.3(8) . 1_545 ?
O1 Pb1 Pb1 149.7(8) 1_565 1_545 ?
I1 Pb1 Pb1 127.80(5) 2_665 1_545 ?
I1 Pb1 Pb1 52.20(5) 2_655 1_545 ?
I1 Pb1 Pb1 90.000(1) . 1_545 ?
I1 Pb1 Pb1 55.35(7) 5_656 1_545 ?
I1 Pb1 Pb1 124.65(7) 5_666 1_545 ?
Pb1 Pb1 Pb1 122.53(7) 5_766 1_545 ?
Pb1 Pb1 Pb1 57.47(7) 5_756 1_545 ?
Pb1 Pb1 Pb1 180.0(3) 1_565 1_545 ?
Pb1 I1 Pb1 75.61(9) 2_654 2_664 ?
Pb1 I1 Pb1 112.83(16) 2_654 . ?
Pb1 I1 Pb1 112.83(16) 2_664 . ?
Pb1 I1 Pb1 95.11(8) 2_654 5_656 ?
Pb1 I1 Pb1 141.83(19) 2_664 5_656 ?
Pb1 I1 Pb1 104.94(12) . 5_656 ?
Pb1 I1 Pb1 141.83(19) 2_654 5_666 ?
Pb1 I1 Pb1 95.11(8) 2_664 5_666 ?
Pb1 I1 Pb1 104.94(12) . 5_666 ?
Pb1 I1 Pb1 69.31(13) 5_656 5_666 ?
Pb1 O1 Pb1 107.5(12) 5_756 . ?
Pb1 O1 Pb1 107.5(12) 5_756 1_545 ?
Pb1 O1 Pb1 119.3(16) . 1_545 ?
 
_diffrn_measured_fraction_theta_max    0.268
_diffrn_reflns_theta_full              29.52
_diffrn_measured_fraction_theta_full   0.268
_refine_diff_density_max    1.537
_refine_diff_density_min   -1.570
_refine_diff_density_rms    0.485