 
data_r
 
_audit_creation_method            'SHELXL-2014/7'
_shelx_SHELXL_version_number      '2014/7'
_chemical_name_systematic         ?
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          ?
_chemical_formula_sum
 'H14 O11 S Zn' 
_chemical_formula_weight          287.54

loop_
 _atom_type_symbol
 _atom_type_description
 _atom_type_scat_dispersion_real
 _atom_type_scat_dispersion_imag
 _atom_type_scat_source
 'Zn'  'Zn'   0.2839   1.4301
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'S'  'S'   0.1246   0.1234
 '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'
 
_space_group_crystal_system       orthorhombic
_space_group_IT_number            19
_space_group_name_H-M_alt         'P 21 21 21'
_space_group_name_Hall            'P 2ac 2ab'
 
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
 
loop_
 _space_group_symop_operation_xyz
 'x, y, z'
 '-x+1/2, -y, z+1/2'
 'x+1/2, -y+1/2, -z'
 '-x, y+1/2, -z+1/2'
 
_cell_length_a                    6.82070(10)
_cell_length_b                    11.8048(2)
_cell_length_c                    12.0553(3)
_cell_angle_alpha                 90
_cell_angle_beta                  90
_cell_angle_gamma                 90
_cell_volume                      970.66(3)
_cell_formula_units_Z             4
_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_density_meas       ?
_exptl_crystal_density_method     ?
_exptl_crystal_density_diffrn     1.968          
_exptl_crystal_F_000              592
_exptl_transmission_factor_min    ?
_exptl_transmission_factor_max    ?
_exptl_crystal_size_max           ?
_exptl_crystal_size_mid           ?
_exptl_crystal_size_min           ?
_exptl_absorpt_coefficient_mu     2.785
_shelx_estimated_absorpt_T_min    ?
_shelx_estimated_absorpt_T_max    ?
_exptl_absorpt_correction_type    ?
_exptl_absorpt_correction_T_min   ?
_exptl_absorpt_correction_T_max   ?
_exptl_absorpt_process_details    ?
_exptl_absorpt_special_details    ?
_diffrn_ambient_temperature       293(2)
_diffrn_radiation_wavelength      0.71073
_diffrn_radiation_type            MoK\a
_diffrn_source                    ?
_diffrn_measurement_device_type   ?
_diffrn_measurement_method        ?
_diffrn_detector_area_resol_mean  ?
_diffrn_reflns_number             13772
_diffrn_reflns_av_unetI/netI      0.0265
_diffrn_reflns_av_R_equivalents   0.0611
_diffrn_reflns_limit_h_min        -8
_diffrn_reflns_limit_h_max        6
_diffrn_reflns_limit_k_min        -14
_diffrn_reflns_limit_k_max        14
_diffrn_reflns_limit_l_min        -13
_diffrn_reflns_limit_l_max        15
_diffrn_reflns_theta_min          6.834
_diffrn_reflns_theta_max          26.499
_diffrn_reflns_theta_full         25.242
_diffrn_measured_fraction_theta_max   0.977
_diffrn_measured_fraction_theta_full  0.974
_diffrn_reflns_Laue_measured_fraction_max    0.977
_diffrn_reflns_Laue_measured_fraction_full   0.974
_diffrn_reflns_point_group_measured_fraction_max   0.983
_diffrn_reflns_point_group_measured_fraction_full  0.980
_reflns_number_total              1978
_reflns_number_gt                 1925
_reflns_threshold_expression      'I > 2σ(I)'
_reflns_Friedel_coverage          0.707
_reflns_Friedel_fraction_max      0.990
_reflns_Friedel_fraction_full     0.989
 
_reflns_special_details
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
 
_computing_data_collection        ?
_computing_cell_refinement        ?
_computing_data_reduction         ?
_computing_structure_solution     ?
_computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics     ?
_computing_publication_material   ?
_refine_special_details           ?
_refine_ls_structure_factor_coef  Fsqd
_refine_ls_matrix_type            full
_refine_ls_weighting_scheme       calc
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0525P)²+0.0314P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary      ?
_atom_sites_solution_secondary    ?
_atom_sites_solution_hydrogens    difmap
_refine_ls_hydrogen_treatment     refall
_refine_ls_extinction_method      'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_extinction_coef        0.019(4)
_refine_ls_extinction_expression
 'Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^'
_refine_ls_abs_structure_details
;
 Flack x determined using 782 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack    0.006(13)
_chemical_absolute_configuration  ?
_refine_ls_number_reflns          1978
_refine_ls_number_parameters      175
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.0270
_refine_ls_R_factor_gt            0.0261
_refine_ls_wR_factor_ref          0.0679
_refine_ls_wR_factor_gt           0.0672
_refine_ls_goodness_of_fit_ref    1.061
_refine_ls_restrained_S_all       1.061
_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_site_symmetry_order  
 _atom_site_calc_flag
 _atom_site_refinement_flags_posn
 _atom_site_refinement_flags_adp
 _atom_site_refinement_flags_occupancy
 _atom_site_disorder_assembly
 _atom_site_disorder_group
Zn1 Zn 0.03991(6) 0.57773(3) 0.10609(3) 0.01802(18) Uani 1 1 d . . . . .
O11 O 0.2268(5) 0.0332(3) 0.3275(3) 0.0306(7) Uani 1 1 d . . . . .
H11 H 0.254(8) 0.012(5) 0.819(5) 0.019(15) Uiso 1 1 d . . . . .
H12 H 0.301(8) 0.074(5) 0.283(5) 0.030(12) Uiso 1 1 d . . . . .
O12 O 0.0039(5) 0.7392(2) 0.1704(3) 0.0280(6) Uani 1 1 d . . . . .
H21 H 0.095(11) 0.265(6) 0.311(5) 0.047(17) Uiso 1 1 d . . . . .
H22 H 0.079(8) 0.755(4) 0.213(4) 0.019(12) Uiso 1 1 d . . . . .
O13 O 0.1945(4) 0.5289(2) 0.2515(2) 0.0216(5) Uani 1 1 d . . . . .
H31 H 0.292(10) 0.579(5) 0.263(5) 0.048(15) Uiso 1 1 d . . . . .
H32 H 0.234(10) 0.467(6) 0.248(6) 0.049(18) Uiso 1 1 d . . . . .
O14 O 0.0729(5) 0.4143(3) 0.0484(3) 0.0334(7) Uani 1 1 d . . . . .
H41 H 0.532(10) 0.112(5) 0.012(6) 0.046(15) Uiso 1 1 d . . . . .
H42 H 0.174(15) 0.389(7) 0.051(8) 0.08(3) Uiso 1 1 d . . . . .
O15 O 0.1093(6) 0.1267(3) 0.5406(3) 0.0263(6) Uani 1 1 d . . . . .
H51 H 0.037(11) 0.130(6) 0.607(6) 0.049(17) Uiso 1 1 d . . . . .
H52 H 0.183(9) 0.097(5) 0.546(5) 0.022(16) Uiso 1 1 d . . . . .
O16 O 0.2033(5) 0.3640(3) 0.5365(3) 0.0344(8) Uani 1 1 d . . . . .
H61 H 0.117(11) 0.394(6) 0.508(5) 0.043(17) Uiso 1 1 d . . . . .
H62 H 0.192(12) 0.312(6) 0.523(6) 0.05(2) Uiso 1 1 d . . . . .
S1 S 0.49092(11) 0.27330(7) 0.18310(7) 0.0169(2) Uani 1 1 d . . . . .
O1S O 0.4827(4) 0.1490(2) 0.1857(3) 0.0305(7) Uani 1 1 d . . . . .
O2S O 0.4269(5) 0.3159(3) 0.0752(3) 0.0393(8) Uani 1 1 d . . . . .
O3S O 0.3620(4) 0.3193(2) 0.2713(2) 0.0276(6) Uani 1 1 d . . . . .
O4S O 0.6925(4) 0.3113(2) 0.2048(3) 0.0330(7) Uani 1 1 d . . . . .
O1 O 0.0657(5) 0.0098(3) 0.0621(3) 0.0342(7) Uani 1 1 d . . . . .
H1 H -0.053(10) 0.577(6) 0.469(6) 0.050(17) Uiso 1 1 d . . . . .
H2 H 0.022(10) 0.016(5) 0.113(5) 0.034(16) Uiso 1 1 d . . . . .
 
 
_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
Zn1 O11 2.056(3) 4 ?
Zn1 O16 2.060(3) 2_564 ?
Zn1 O14 2.063(3) . ?
Zn1 O12 2.072(3) . ?
Zn1 O15 2.120(3) 4 ?
Zn1 O13 2.125(3) . ?
O11 Zn1 2.056(3) 4_545 ?
O11 H12 0.88(6) . ?
O12 H22 0.75(6) . ?
O13 H31 0.90(7) . ?
O13 H32 0.78(7) . ?
O14 H42 0.75(10) . ?
O15 Zn1 2.120(3) 4_545 ?
O15 H51 0.94(7) . ?
O15 H52 0.62(6) . ?
O16 Zn1 2.060(3) 2_565 ?
O16 H61 0.77(8) . ?
O16 H62 0.64(7) . ?
S1 O2S 1.461(3) . ?
S1 O1S 1.469(2) . ?
S1 O4S 1.470(3) . ?
S1 O3S 1.483(3) . ?
O1 H2 0.68(6) . ?
 
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
O11 Zn1 O16 175.00(16) 4 2_564 ?
O11 Zn1 O14 89.33(14) 4 . ?
O16 Zn1 O14 94.74(15) 2_564 . ?
O11 Zn1 O12 89.11(13) 4 . ?
O16 Zn1 O12 86.91(14) 2_564 . ?
O14 Zn1 O12 177.62(14) . . ?
O11 Zn1 O15 88.28(14) 4 4 ?
O16 Zn1 O15 88.70(16) 2_564 4 ?
O14 Zn1 O15 91.49(14) . 4 ?
O12 Zn1 O15 90.26(14) . 4 ?
O11 Zn1 O13 92.76(13) 4 . ?
O16 Zn1 O13 90.28(14) 2_564 . ?
O14 Zn1 O13 88.29(13) . . ?
O12 Zn1 O13 89.98(13) . . ?
O15 Zn1 O13 178.94(13) 4 . ?
Zn1 O11 H12 127(3) 4_545 . ?
Zn1 O12 H22 114(4) . . ?
Zn1 O13 H31 108(4) . . ?
Zn1 O13 H32 112(5) . . ?
H31 O13 H32 112(6) . . ?
Zn1 O14 H42 117(7) . . ?
Zn1 O15 H51 118(4) 4_545 . ?
Zn1 O15 H52 109(5) 4_545 . ?
H51 O15 H52 110(7) . . ?
Zn1 O16 H61 133(5) 2_565 . ?
Zn1 O16 H62 122(7) 2_565 . ?
H61 O16 H62 104(8) . . ?
O2S S1 O1S 110.6(2) . . ?
O2S S1 O4S 109.4(2) . . ?
O1S S1 O4S 109.70(17) . . ?
O2S S1 O3S 109.57(19) . . ?
O1S S1 O3S 109.13(17) . . ?
O4S S1 O3S 108.38(19) . . ?
 
_refine_diff_density_max    0.441
_refine_diff_density_min   -0.419
_refine_diff_density_rms    0.072



