 
data_shelx
 
_audit_creation_method            'SHELXL-2018/3'
_shelx_SHELXL_version_number      '2018/3'
_chemical_name_systematic         ?
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          ?
_chemical_formula_sum
 'O4.50 S Zn1.50' 
_chemical_formula_weight          202.12

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'
 'S'  'S'   0.1246   0.1234
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Zn'  'Zn'   0.2839   1.4301
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 
_space_group_crystal_system       monoclinic
_space_group_IT_number            11
_space_group_name_H-M_alt         'P 21/m'
_space_group_name_Hall            '-P 2yb'
 
_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, y+1/2, -z'
 '-x, -y, -z'
 'x, -y-1/2, z'
 
_cell_length_a                    7.298(18)
_cell_length_b                    6.588(11)
_cell_length_c                    7.840(12)
_cell_angle_alpha                 90
_cell_angle_beta                  117.15(3)
_cell_angle_gamma                 90
_cell_volume                      335.4(11)
_cell_formula_units_Z             4
_cell_measurement_temperature     299(2)
_cell_measurement_reflns_used     239
_cell_measurement_theta_min       2.920
_cell_measurement_theta_max       27.914
 
_exptl_crystal_description        'prism'
_exptl_crystal_colour             ?
_exptl_crystal_density_meas       ?
_exptl_crystal_density_method     ?
_exptl_crystal_density_diffrn     4.003          
_exptl_crystal_F_000              388
_exptl_transmission_factor_min    ?
_exptl_transmission_factor_max    ?
_exptl_crystal_size_max           ?
_exptl_crystal_size_mid           ?
_exptl_crystal_size_min           ?
_exptl_absorpt_coefficient_mu     11.292
_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       299(2)
_diffrn_radiation_wavelength      0.71073
_diffrn_radiation_type            MoK\a
_diffrn_source                    ?
_diffrn_measurement_device_type   'Bruker Apex2 Duo'
_diffrn_measurement_method        ?
_diffrn_detector_area_resol_mean  ?
_diffrn_reflns_number             1135
_diffrn_reflns_av_unetI/netI      0.0614
_diffrn_reflns_av_R_equivalents   0.0410
_diffrn_reflns_limit_h_min        -9
_diffrn_reflns_limit_h_max        9
_diffrn_reflns_limit_k_min        -6
_diffrn_reflns_limit_k_max        5
_diffrn_reflns_limit_l_min        -10
_diffrn_reflns_limit_l_max        9
_diffrn_reflns_theta_min          2.920
_diffrn_reflns_theta_max          27.914
_diffrn_reflns_theta_full         25.242
_diffrn_measured_fraction_theta_max   0.708
_diffrn_measured_fraction_theta_full  0.750
_diffrn_reflns_Laue_measured_fraction_max    0.708
_diffrn_reflns_Laue_measured_fraction_full   0.750
_diffrn_reflns_point_group_measured_fraction_max   0.708
_diffrn_reflns_point_group_measured_fraction_full  0.750
_reflns_number_total              621
_reflns_number_gt                 518
_reflns_threshold_expression      'I > 2σ(I)'
_reflns_Friedel_coverage          0.000
_reflns_Friedel_fraction_max      .
_reflns_Friedel_fraction_full     .
 
_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. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;
 
_computing_data_collection        ?
_computing_cell_refinement        ?
_computing_data_reduction         ?
_computing_structure_solution     ?
_computing_structure_refinement 'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics     ?
_computing_publication_material   ?
_refine_special_details
;
 Refined as a 2-component twin.
;
_refine_ls_structure_factor_coef  Fsqd
_refine_ls_matrix_type            full
_refine_ls_weighting_scheme       calc
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0802P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary      ?
_atom_sites_solution_secondary    ?
_atom_sites_solution_hydrogens    .
_refine_ls_hydrogen_treatment     undef
_refine_ls_extinction_method      none
_refine_ls_extinction_coef        .
_refine_ls_number_reflns          621
_refine_ls_number_parameters      80
_refine_ls_number_restraints      18
_refine_ls_R_factor_all           0.0581
_refine_ls_R_factor_gt            0.0459
_refine_ls_wR_factor_ref          0.1211
_refine_ls_wR_factor_gt           0.1146
_refine_ls_goodness_of_fit_ref    1.021
_refine_ls_restrained_S_all       1.019
_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 0.500000 0.500000 0.000000 0.0154(5) Uani 1 2 d S . P . .
Zn2 Zn -0.1252(4) 0.750000 0.2536(3) 0.0164(7) Uani 1 2 d S T P . .
Zn3 Zn 0.6595(4) 0.750000 0.7708(3) 0.0172(7) Uani 1 2 d S T P . .
S1 S 0.3528(6) 0.750000 0.3051(7) 0.0114(12) Uani 1 2 d S T P . .
S2 S 0.0624(7) 0.750000 0.7181(7) 0.0114(12) Uani 1 2 d S T P . .
O1 O 0.6280(14) 0.750000 1.0096(19) 0.009(2) Uani 1 2 d S TU P . .
O2 O 0.1964(14) 0.9312(19) 0.7636(12) 0.017(2) Uani 1 1 d . . . . .
O3 O -0.079(2) 0.750000 0.5212(19) 0.026(4) Uani 1 2 d S T P . .
O4 O 0.388(2) 0.570(2) 0.2148(16) 0.032(3) Uani 1 1 d . . . . .
O5 O -0.046(2) 0.750000 0.8312(19) 0.030(4) Uani 1 2 d S T P . .
O6 O 0.139(3) 0.750000 0.262(3) 0.077(8) Uani 1 2 d S TU P . .
O7 O 0.479(3) 0.750000 0.497(2) 0.091(10) Uani 1 2 d S TU P . .
 
 
_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 O1 1.878(5) 3_666 ?
Zn1 O1 1.878(5) 1_554 ?
Zn1 O2 2.191(10) 4_574 ?
Zn1 O2 2.191(10) 2_646 ?
Zn1 O4 2.230(10) . ?
Zn1 O4 2.230(10) 3_665 ?
Zn1 Zn2 3.031(5) 1_655 ?
Zn1 Zn2 3.031(5) 3_565 ?
Zn1 Zn3 3.034(4) 3_666 ?
Zn1 Zn3 3.034(4) 1_554 ?
Zn2 O6 1.902(17) . ?
Zn2 O1 1.939(12) 1_454 ?
Zn2 O3 1.967(14) . ?
Zn2 O2 2.153(13) 2_546 ?
Zn2 O2 2.153(13) 3_576 ?
Zn3 O7 1.938(15) . ?
Zn3 O5 1.977(14) 1_655 ?
Zn3 O1 1.987(13) . ?
Zn3 O4 2.144(15) 3_666 ?
Zn3 O4 2.144(15) 2_656 ?
S1 O7 1.361(15) . ?
S1 O6 1.435(18) . ?
S1 O4 1.465(13) 4_575 ?
S1 O4 1.465(13) . ?
S2 O3 1.413(14) . ?
S2 O5 1.435(13) . ?
S2 O2 1.480(12) 4_575 ?
S2 O2 1.480(12) . ?
 
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 Zn1 O1 180.0(9) 3_666 1_554 ?
O1 Zn1 O2 81.7(5) 3_666 4_574 ?
O1 Zn1 O2 98.3(5) 1_554 4_574 ?
O1 Zn1 O2 98.3(5) 3_666 2_646 ?
O1 Zn1 O2 81.7(5) 1_554 2_646 ?
O2 Zn1 O2 180.0(6) 4_574 2_646 ?
O1 Zn1 O4 82.1(5) 3_666 . ?
O1 Zn1 O4 97.9(5) 1_554 . ?
O2 Zn1 O4 91.1(4) 4_574 . ?
O2 Zn1 O4 88.9(4) 2_646 . ?
O1 Zn1 O4 97.9(5) 3_666 3_665 ?
O1 Zn1 O4 82.1(5) 1_554 3_665 ?
O2 Zn1 O4 88.9(4) 4_574 3_665 ?
O2 Zn1 O4 91.1(4) 2_646 3_665 ?
O4 Zn1 O4 180.0 . 3_665 ?
O1 Zn1 Zn2 141.9(4) 3_666 1_655 ?
O1 Zn1 Zn2 38.1(4) 1_554 1_655 ?
O2 Zn1 Zn2 134.8(3) 4_574 1_655 ?
O2 Zn1 Zn2 45.2(3) 2_646 1_655 ?
O4 Zn1 Zn2 85.7(4) . 1_655 ?
O4 Zn1 Zn2 94.3(4) 3_665 1_655 ?
O1 Zn1 Zn2 38.1(4) 3_666 3_565 ?
O1 Zn1 Zn2 141.9(4) 1_554 3_565 ?
O2 Zn1 Zn2 45.2(3) 4_574 3_565 ?
O2 Zn1 Zn2 134.8(3) 2_646 3_565 ?
O4 Zn1 Zn2 94.3(4) . 3_565 ?
O4 Zn1 Zn2 85.7(4) 3_665 3_565 ?
Zn2 Zn1 Zn2 180.0 1_655 3_565 ?
O1 Zn1 Zn3 39.6(4) 3_666 3_666 ?
O1 Zn1 Zn3 140.4(4) 1_554 3_666 ?
O2 Zn1 Zn3 95.7(3) 4_574 3_666 ?
O2 Zn1 Zn3 84.3(3) 2_646 3_666 ?
O4 Zn1 Zn3 44.9(4) . 3_666 ?
O4 Zn1 Zn3 135.1(4) 3_665 3_666 ?
Zn2 Zn1 Zn3 112.44(13) 1_655 3_666 ?
Zn2 Zn1 Zn3 67.56(13) 3_565 3_666 ?
O1 Zn1 Zn3 140.4(4) 3_666 1_554 ?
O1 Zn1 Zn3 39.6(4) 1_554 1_554 ?
O2 Zn1 Zn3 84.3(3) 4_574 1_554 ?
O2 Zn1 Zn3 95.7(3) 2_646 1_554 ?
O4 Zn1 Zn3 135.1(4) . 1_554 ?
O4 Zn1 Zn3 44.9(4) 3_665 1_554 ?
Zn2 Zn1 Zn3 67.56(13) 1_655 1_554 ?
Zn2 Zn1 Zn3 112.44(13) 3_565 1_554 ?
Zn3 Zn1 Zn3 180.0 3_666 1_554 ?
O6 Zn2 O1 120.3(7) . 1_454 ?
O6 Zn2 O3 106.7(7) . . ?
O1 Zn2 O3 132.9(6) 1_454 . ?
O6 Zn2 O2 102.4(3) . 2_546 ?
O1 Zn2 O2 81.3(2) 1_454 2_546 ?
O3 Zn2 O2 89.2(3) . 2_546 ?
O6 Zn2 O2 102.4(3) . 3_576 ?
O1 Zn2 O2 81.3(2) 1_454 3_576 ?
O3 Zn2 O2 89.2(3) . 3_576 ?
O2 Zn2 O2 154.6(5) 2_546 3_576 ?
O6 Zn2 Zn1 128.4(5) . 1_455 ?
O1 Zn2 Zn1 36.74(15) 1_454 1_455 ?
O3 Zn2 Zn1 111.3(4) . 1_455 ?
O2 Zn2 Zn1 46.3(2) 2_546 1_455 ?
O2 Zn2 Zn1 111.7(3) 3_576 1_455 ?
O6 Zn2 Zn1 128.4(5) . 2 ?
O1 Zn2 Zn1 36.74(15) 1_454 2 ?
O3 Zn2 Zn1 111.3(4) . 2 ?
O2 Zn2 Zn1 111.7(3) 2_546 2 ?
O2 Zn2 Zn1 46.3(2) 3_576 2 ?
Zn1 Zn2 Zn1 65.83(14) 1_455 2 ?
O7 Zn3 O5 112.3(8) . 1_655 ?
O7 Zn3 O1 137.0(8) . . ?
O5 Zn3 O1 110.7(5) 1_655 . ?
O7 Zn3 O4 90.8(4) . 3_666 ?
O5 Zn3 O4 99.9(3) 1_655 3_666 ?
O1 Zn3 O4 81.9(3) . 3_666 ?
O7 Zn3 O4 90.8(3) . 2_656 ?
O5 Zn3 O4 99.9(3) 1_655 2_656 ?
O1 Zn3 O4 81.9(3) . 2_656 ?
O4 Zn3 O4 158.0(6) 3_666 2_656 ?
O7 Zn3 Zn1 114.0(6) . 2_656 ?
O5 Zn3 Zn1 121.8(3) 1_655 2_656 ?
O1 Zn3 Zn1 37.03(14) . 2_656 ?
O4 Zn3 Zn1 112.8(3) 3_666 2_656 ?
O4 Zn3 Zn1 47.3(3) 2_656 2_656 ?
O7 Zn3 Zn1 114.0(6) . 1_556 ?
O5 Zn3 Zn1 121.8(3) 1_655 1_556 ?
O1 Zn3 Zn1 37.03(14) . 1_556 ?
O4 Zn3 Zn1 47.3(3) 3_666 1_556 ?
O4 Zn3 Zn1 112.8(3) 2_656 1_556 ?
Zn1 Zn3 Zn1 65.76(13) 2_656 1_556 ?
O7 S1 O6 112.2(12) . . ?
O7 S1 O4 110.7(8) . 4_575 ?
O6 S1 O4 107.3(7) . 4_575 ?
O7 S1 O4 110.7(8) . . ?
O6 S1 O4 107.3(7) . . ?
O4 S1 O4 108.5(9) 4_575 . ?
O3 S2 O5 109.8(9) . . ?
O3 S2 O2 109.7(5) . 4_575 ?
O5 S2 O2 110.0(5) . 4_575 ?
O3 S2 O2 109.7(5) . . ?
O5 S2 O2 110.0(5) . . ?
O2 S2 O2 107.5(9) 4_575 . ?
Zn1 O1 Zn1 122.6(5) 1_556 2_656 ?
Zn1 O1 Zn2 105.1(4) 1_556 1_656 ?
Zn1 O1 Zn2 105.1(4) 2_656 1_656 ?
Zn1 O1 Zn3 103.4(4) 1_556 . ?
Zn1 O1 Zn3 103.4(4) 2_656 . ?
Zn2 O1 Zn3 118.3(5) 1_656 . ?
S2 O2 Zn2 131.1(6) . 3_576 ?
S2 O2 Zn1 132.3(7) . 2_656 ?
Zn2 O2 Zn1 88.5(4) 3_576 2_656 ?
S2 O3 Zn2 148.0(11) . . ?
S1 O4 Zn3 134.7(6) . 3_666 ?
S1 O4 Zn1 137.5(8) . . ?
Zn3 O4 Zn1 87.8(5) 3_666 . ?
S2 O5 Zn3 134.3(9) . 1_455 ?
S1 O6 Zn2 169.6(15) . . ?
S1 O7 Zn3 179.9(18) . . ?
 
_refine_diff_density_max    1.130
_refine_diff_density_min   -1.450
_refine_diff_density_rms    0.242



