 
data_s92 
 
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum 
 'Cl H5 O6' 
_chemical_formula_weight          136.49 
 
loop_ 
 _atom_type_symbol 
 _atom_type_description 
 _atom_type_scat_dispersion_real 
 _atom_type_scat_dispersion_imag 
 _atom_type_scat_source 
 'H'  'H'   0.0000   0.0000 
 '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' 
 'Cl'  'Cl'   0.1484   0.1585 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 
_symmetry_cell_setting            Orthorhombic 
_symmetry_space_group_name_H-M    Pna21
_symmetry_space_group_name_hall   'P 2c -2n'
 
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 '-x, -y, z+1/2' 
 'x+1/2, -y+1/2, z' 
 '-x+1/2, y+1/2, z+1/2' 
 
_cell_length_a                    7.9054(3) 
_cell_length_b                    10.5443(4) 
_cell_length_c                    5.9511(2) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  90.00 
_cell_angle_gamma                 90.00 
_cell_volume                      496.07(3) 
_cell_formula_units_Z             4 
_cell_measurement_temperature     150(2) 
_cell_measurement_reflns_used     1747 
_cell_measurement_theta_min       2.91 
_cell_measurement_theta_max       38.57 
 
_exptl_crystal_description        Block 
_exptl_crystal_colour             colourless 
_exptl_crystal_size_max           0.25 
_exptl_crystal_size_mid           0.25 
_exptl_crystal_size_min           0.15 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.828 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              280 
_exptl_absorpt_coefficient_mu     0.706 
_exptl_absorpt_correction_type    Empirical 
_exptl_absorpt_correction_T_min   0.8432 
_exptl_absorpt_correction_T_max   0.9014 
_exptl_absorpt_process_details    'SORTAV (R. H. Blessing, 1995, 1997)'
 
_exptl_special_details 
; 
 ? 
; 
 
_diffrn_ambient_temperature       150(2) 
_diffrn_radiation_wavelength      0.71073 
_diffrn_radiation_type            MoK\a 
_diffrn_radiation_source          'Enraf Nonius FR591 rotating anode'
_diffrn_radiation_monochromator   graphite 
_diffrn_measurement_device_type   'Enraf Nonius KappaCCD area detector'
_diffrn_measurement_method        'ω and φ scans to fill Ewald sphere'
_diffrn_detector_area_resol_mean  '9.091 pixels/mm'
_diffrn_standards_number          'n/a'
_diffrn_standards_interval_count  'n/a'
_diffrn_standards_interval_time   'n/a'
_diffrn_standards_decay_%         'n/a'
_diffrn_reflns_number             2344 
_diffrn_reflns_av_R_equivalents   0.0335 
_diffrn_reflns_av_sigmaI/netI     0.0341 
_diffrn_reflns_limit_h_min        -9 
_diffrn_reflns_limit_h_max        9 
_diffrn_reflns_limit_k_min        -12 
_diffrn_reflns_limit_k_max        12 
_diffrn_reflns_limit_l_min        -5 
_diffrn_reflns_limit_l_max        7 
_diffrn_reflns_theta_min          3.22 
_diffrn_reflns_theta_max          25.09 
_reflns_number_total              716 
_reflns_number_gt                 710 
_reflns_threshold_expression      >2sigma(I) 
 
_computing_cell_refinement        'DENZO and COLLECT'
_computing_data_reduction         'DENZO and COLLECT'
_computing_structure_solution     'SHELXS-97 (Sheldrick, 2008)' 
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 2008)' 
_computing_molecular_graphics     ?
_computing_publication_material   SHELXL-97
 
_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 > 2sigma(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)+(0.0001P)²+0.7857P] where P=(Fo²+2Fc²)/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        0.105(16) 
_refine_ls_extinction_expression 
 'Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^' 
_refine_ls_abs_structure_details 
 'Flack H D (1983), Acta Cryst. A39, 876-881' 
_refine_ls_abs_structure_Flack    0.5(2) 
_refine_ls_number_reflns          716 
_refine_ls_number_parameters      78 
_refine_ls_number_restraints      7 
_refine_ls_R_factor_all           0.0376 
_refine_ls_R_factor_gt            0.0374 
_refine_ls_wR_factor_ref          0.0971 
_refine_ls_wR_factor_gt           0.0970 
_refine_ls_goodness_of_fit_ref    1.663 
_refine_ls_restrained_S_all       1.654 
_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 
Cl1 Cl 0.25730(11) 0.42310(8) 0.2448(3) 0.0082(4) Uani 1 1 d . . . 
O1 O 0.2119(4) 0.5588(3) 0.2175(7) 0.0113(8) Uani 1 1 d . . . 
O2 O 0.4391(4) 0.4052(3) 0.2067(6) 0.0140(8) Uani 1 1 d . . . 
O3 O 0.1599(4) 0.3459(3) 0.0828(6) 0.0114(8) Uani 1 1 d . . . 
O4 O 0.2125(4) 0.3835(3) 0.4753(5) 0.0108(8) Uani 1 1 d . . . 
O5 O 0.0180(4) 0.8006(3) 0.2565(9) 0.0251(9) Uani 1 1 d D . . 
H1 H -0.091(3) 0.844(3) 0.275(10) 0.030 Uiso 1 1 d D . . 
H2 H 0.092(5) 0.834(4) 0.138(7) 0.030 Uiso 1 1 d D . . 
H3 H 0.016(5) 0.7078(10) 0.272(11) 0.030 Uiso 1 1 d D . . 
O6 O 0.1821(4) 0.6045(3) 0.7438(9) 0.0260(9) Uani 1 1 d G . . 
H4 H 0.0806 0.6293 0.7161 0.031 Uiso 1 1 d G . . 
H5 H 0.2068 0.5521 0.6430 0.031 Uiso 1 1 d G . . 
 
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 
Cl1 0.0087(5) 0.0086(5) 0.0072(6) -0.0011(6) -0.0006(5) 0.0008(3) 
O1 0.0155(13) 0.0060(14) 0.012(2) 0.0028(16) -0.0025(19) 0.0009(11) 
O2 0.0063(14) 0.0205(16) 0.015(2) -0.0044(16) 0.0018(14) 0.0035(12) 
O3 0.0153(15) 0.0107(15) 0.0083(16) -0.0042(15) -0.0038(15) -0.0008(13) 
O4 0.0178(15) 0.0118(16) 0.0029(17) 0.0019(14) 0.0031(15) -0.0028(14) 
O5 0.0271(18) 0.0203(17) 0.028(2) 0.006(2) 0.005(2) 0.0009(14) 
O6 0.0251(17) 0.0234(18) 0.030(2) 0.000(2) 0.005(2) 0.0038(14) 
 
_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 
Cl1 O2 1.467(3) . ? 
Cl1 O4 1.477(4) . ? 
Cl1 O3 1.478(4) . ? 
Cl1 O1 1.484(3) . ? 
 
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 
O2 Cl1 O4 110.0(2) . . ? 
O2 Cl1 O3 109.8(2) . . ? 
O4 Cl1 O3 109.0(2) . . ? 
O2 Cl1 O1 110.14(18) . . ? 
O4 Cl1 O1 108.4(2) . . ? 
O3 Cl1 O1 109.5(2) . . ? 
 
loop_ 
 _geom_hbond_atom_site_label_D 
 _geom_hbond_atom_site_label_H 
 _geom_hbond_atom_site_label_A 
 _geom_hbond_distance_DH 
 _geom_hbond_distance_HA 
 _geom_hbond_distance_DA 
 _geom_hbond_angle_DHA 
 _geom_hbond_site_symmetry_A 
O5 H1 O1  0.979(8) 1.899(18) 2.847(4) 162(5) 3_465 
O5 H2 O4  0.982(8) 1.896(18) 2.847(5) 162(4) 4_554 
O5 H3 O1  0.983(8) 2.23(3) 2.984(4) 132(3) . 
O6 H4 O3  0.86 2.08 2.916(5) 165.0 2_565 
O6 H5 O4  0.84 2.04 2.835(5) 158.3 . 
 
_diffrn_measured_fraction_theta_max    0.986 
_diffrn_reflns_theta_full              25.09 
_diffrn_measured_fraction_theta_full   0.986 
_refine_diff_density_max    0.472 
_refine_diff_density_min   -0.398 
_refine_diff_density_rms    0.091 
