data_global
_audit_creation_method                  'APEX3 v2018.1-0'

_publ_requested_journal                 ?

_publ_contact_author_name               'Ralf Haiges'
_publ_contact_author_address            
;

University of Southern California
Loker Hydrocarbon Research Institute and Department of Chemistry
Los Angeles, CA 90089
USA
;
_publ_contact_author_email              haiges@usc.edu
_publ_contact_author_fax                ?
_publ_contact_author_phone              '+1 (213) 740-3197'

_publ_section_title                     
;
;
_publ_section_abstract                  
;
;
_publ_section_references                
;
;
_publ_section_comment                   
;
;

data_BaZrS3_smaller
_chemical_name_systematic               ?
_chemical_name_common                   ?
_chemical_formula_moiety                'S6 Zr2, 2(Ba)'
_chemical_formula_sum                   'Ba S3 Zr'
_chemical_formula_iupac                 ?
_chemical_formula_weight                324.74

_chemical_melting_point                 ?

_space_group_crystal_system             orthorhombic
_space_group_name_H-M_alt               'P n m a'
_space_group_name_Hall                  '-P 2ac 2n'
loop_
    _space_group_symop_operation_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                          7.056(3)
_cell_length_b                          9.962(4)
_cell_length_c                          6.996(3)
_cell_angle_alpha                       90
_cell_angle_beta                        90
_cell_angle_gamma                       90
_cell_volume                            491.8(3)
_cell_formula_units_Z                   4
_cell_measurement_reflns_used           1919
_cell_measurement_theta_min             4.5846
_cell_measurement_theta_max             30.4413
_cell_measurement_temperature           100.(2)

_exptl_crystal_description              plate
_exptl_crystal_colour                   'lustrous dark red'
_exptl_crystal_size_max                 0.008
_exptl_crystal_size_mid                 0.008
_exptl_crystal_size_min                 0.005
_exptl_crystal_density_diffrn           4.386
_exptl_crystal_density_meas             ?
_exptl_crystal_density_method           'not measured'
_exptl_crystal_F_000                    576

_exptl_absorpt_coefficient_mu           11.156
_exptl_absorpt_correction_type          multi-scan
_exptl_absorpt_process_details          'SADABS 2016/2 (Bruker AXS, 2016)'
_exptl_absorpt_correction_T_min         0.69
_exptl_absorpt_correction_T_max         0.90

_exptl_special_details                  
;
; 

_diffrn_ambient_temperature             100.(2)

_diffrn_source                          'fine-focus tube'
_diffrn_source_type                     ?

_diffrn_radiation_type                  'MoK\a '
_diffrn_radiation_wavelength            0.71073
_diffrn_radiation_monochromator         'TRIUMPH curved-crystal'

_diffrn_measurement_device_type         'Bruker APEX II CCD'
_diffrn_measurement_method              'omega- and phi-scans'

_diffrn_detector_area_resol_mean        8.3333

_diffrn_reflns_number                   4218
_diffrn_reflns_av_R_equivalents         0.0533
_diffrn_reflns_av_unetI/netI            0.0455
_diffrn_reflns_theta_min                2.04
_diffrn_reflns_theta_max                30.54
_diffrn_reflns_theta_full               27.50
_diffrn_measured_fraction_theta_max     0.948
_diffrn_measured_fraction_theta_full    1.000
_diffrn_reflns_limit_h_min              -9
_diffrn_reflns_limit_h_max              8
_diffrn_reflns_limit_k_min              -13
_diffrn_reflns_limit_k_max              13
_diffrn_reflns_limit_l_min              -9
_diffrn_reflns_limit_l_max              9

_refine_special_details                 
;

Refined as a 2-component twin.
;

_reflns_number_total                    798
_reflns_number_gt                       623
_reflns_threshold_expression            'I > 2σ(I)'

_refine_ls_structure_factor_coef        Fsqd
_refine_ls_matrix_type                  full
_refine_ls_R_factor_all                 0.0536
_refine_ls_R_factor_gt                  0.0336
_refine_ls_wR_factor_gt                 0.0669
_refine_ls_wR_factor_ref                0.0757
_refine_ls_goodness_of_fit_ref          1.162
_refine_ls_restrained_S_all             1.162
_refine_ls_number_reflns                798
_refine_ls_number_parameters            29
_refine_ls_number_restraints            0
_refine_ls_number_constraints           ?
_refine_ls_hydrogen_treatment           undef
_refine_ls_weighting_scheme             calc
_refine_ls_weighting_details            
    'w=1/[σ²(Fo²)+(0.0131P)²+7.5602P] where P=(Fo²+2Fc²)/3'

_atom_sites_solution_hydrogens          ?
_atom_sites_solution_primary            ?
_atom_sites_solution_secondary          ?

_refine_ls_shift/su_max                 0.000
_refine_ls_shift/su_mean                0.000
_refine_diff_density_max                1.804
_refine_diff_density_min                -1.788
_refine_ls_extinction_method            none
_refine_ls_extinction_coef              ?

loop_
    _atom_type_symbol
    _atom_type_description
    _atom_type_scat_dispersion_real
    _atom_type_scat_dispersion_imag
    _atom_type_scat_source
    Ba Ba -0.3244 2.2819
     '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'
    Zr Zr -2.9673 0.5597
     'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_computing_data_collection              
    'Bruker Instrument Service v2012.12.0.3 (Bruker AXS, 2012)'
_computing_cell_refinement              'APEX3 v2018.1-0 (Bruker AXS, 2018)'
_computing_data_reduction               'SAINT V8.38A (Bruker AXS, 2013)'
_computing_structure_solution           'SHELXTL XT 2014/5 (Bruker AXS, 2014)'
_computing_structure_refinement         'SHELXTL XL 2017/1 (Bruker AXS, 2017)'
_computing_molecular_graphics           'shelXle (C.B. Huebschle, rev 882)'
_computing_publication_material         'SHELXTL XL 2017/1 (Bruker AXS, 2017)'

loop_
    _atom_site_type_symbol
    _atom_site_label
    _atom_site_fract_x
    _atom_site_fract_y
    _atom_site_fract_z
    _atom_site_U_iso_or_equiv
    _atom_site_adp_type
    _atom_site_calc_flag
    _atom_site_refinement_flags_adp
    _atom_site_refinement_flags_occupancy
    _atom_site_refinement_flags_posn
    _atom_site_occupancy
    _atom_site_disorder_assembly
    _atom_site_disorder_group
    Ba Ba1 0.54544(10) 0.25 -0.00970(10) 0.00696(17) Uani d T P S 1 . .
    S S1 0.4949(4) 0.25 0.4382(4) 0.0070(6) Uani d T P S 1 . .
    S S2 0.2896(3) 0.46782(19) 0.7896(3) 0.0060(4) Uani d . . . 1 . .
    Zr Zr1 0.5 0.5 0.5 0.0031(2) Uani d . P S 1 . .


_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_site_symmetry_2
    _geom_bond_distance
    _geom_bond_publ_flag
    Ba1 S2 7_564 3.152(2) ?
    Ba1 S2 1_554 3.152(2) ?
    Ba1 S1 . 3.154(3) ?
    Ba1 S1 6_656 3.211(3) ?
    Ba1 S2 4 3.393(2) ?
    Ba1 S2 6_656 3.393(2) ?
    Ba1 S2 5_666 3.410(2) ?
    Ba1 S2 3_646 3.410(2) ?
    Ba1 Zr1 2_664 4.0614(13) ?
    Ba1 Zr1 4 4.0614(13) ?
    Ba1 Zr1 3_645 4.2512(13) ?
    Ba1 Zr1 1_554 4.2512(13) ?
    S1 Zr1 . 2.5281(11) ?
    S1 Zr1 3_646 2.5281(11) ?
    S2 Zr1 . 2.532(2) ?
    S2 Zr1 2_565 2.539(2) ?

loop_
    _geom_angle_atom_site_label_1
    _geom_angle_atom_site_label_2
    _geom_angle_atom_site_label_3
    _geom_angle_site_symmetry_1
    _geom_angle_site_symmetry_3
    _geom_angle
    _geom_angle_publ_flag
    S2 Ba1 S2 7_564 1_554 87.00(8) ?
    S2 Ba1 S1 7_564 . 112.19(6) ?
    S2 Ba1 S1 1_554 . 112.19(6) ?
    S2 Ba1 S1 7_564 6_656 129.42(5) ?
    S2 Ba1 S1 1_554 6_656 129.42(5) ?
    S1 Ba1 S1 . 6_656 87.53(7) ?
    S2 Ba1 S2 7_564 4 66.01(4) ?
    S2 Ba1 S2 1_554 4 118.29(4) ?
    S1 Ba1 S2 . 4 129.12(5) ?
    S1 Ba1 S2 6_656 4 65.69(5) ?
    S2 Ba1 S2 7_564 6_656 118.29(4) ?
    S2 Ba1 S2 1_554 6_656 66.01(4) ?
    S1 Ba1 S2 . 6_656 129.12(5) ?
    S1 Ba1 S2 6_656 6_656 65.69(5) ?
    S2 Ba1 S2 4 6_656 79.51(7) ?
    S2 Ba1 S2 7_564 5_666 164.58(4) ?
    S2 Ba1 S2 1_554 5_666 80.15(6) ?
    S1 Ba1 S2 . 5_666 65.79(4) ?
    S1 Ba1 S2 6_656 5_666 65.95(4) ?
    S2 Ba1 S2 4 5_666 127.92(3) ?
    S2 Ba1 S2 6_656 5_666 63.90(3) ?
    S2 Ba1 S2 7_564 3_646 80.15(6) ?
    S2 Ba1 S2 1_554 3_646 164.58(4) ?
    S1 Ba1 S2 . 3_646 65.79(4) ?
    S1 Ba1 S2 6_656 3_646 65.95(4) ?
    S2 Ba1 S2 4 3_646 63.90(3) ?
    S2 Ba1 S2 6_656 3_646 127.92(3) ?
    S2 Ba1 S2 5_666 3_646 111.06(7) ?
    S2 Ba1 Zr1 7_564 2_664 151.85(4) ?
    S2 Ba1 Zr1 1_554 2_664 92.15(5) ?
    S1 Ba1 Zr1 . 2_664 94.17(5) ?
    S1 Ba1 Zr1 6_656 2_664 38.492(18) ?
    S2 Ba1 Zr1 4 2_664 90.04(4) ?
    S2 Ba1 Zr1 6_656 2_664 38.41(4) ?
    S2 Ba1 Zr1 5_666 2_664 38.50(4) ?
    S2 Ba1 Zr1 3_646 2_664 103.21(5) ?
    S2 Ba1 Zr1 7_564 4 92.15(5) ?
    S2 Ba1 Zr1 1_554 4 151.85(4) ?
    S1 Ba1 Zr1 . 4 94.17(5) ?
    S1 Ba1 Zr1 6_656 4 38.492(18) ?
    S2 Ba1 Zr1 4 4 38.41(4) ?
    S2 Ba1 Zr1 6_656 4 90.04(4) ?
    S2 Ba1 Zr1 5_666 4 103.21(5) ?
    S2 Ba1 Zr1 3_646 4 38.50(4) ?
    Zr1 Ba1 Zr1 2_664 4 75.65(3) ?
    S2 Ba1 Zr1 7_564 3_645 36.31(4) ?
    S2 Ba1 Zr1 1_554 3_645 90.04(5) ?
    S1 Ba1 Zr1 . 3_645 142.49(2) ?
    S1 Ba1 Zr1 6_656 3_645 101.55(4) ?
    S2 Ba1 Zr1 4 3_645 36.67(4) ?
    S2 Ba1 Zr1 6_656 3_645 86.97(4) ?
    S2 Ba1 Zr1 5_666 3_645 150.81(4) ?
    S2 Ba1 Zr1 3_646 3_645 84.67(4) ?
    Zr1 Ba1 Zr1 2_664 3_645 115.61(2) ?
    Zr1 Ba1 Zr1 4 3_645 73.368(16) ?
    S2 Ba1 Zr1 7_564 1_554 90.04(5) ?
    S2 Ba1 Zr1 1_554 1_554 36.31(4) ?
    S1 Ba1 Zr1 . 1_554 142.49(2) ?
    S1 Ba1 Zr1 6_656 1_554 101.55(4) ?
    S2 Ba1 Zr1 4 1_554 86.97(4) ?
    S2 Ba1 Zr1 6_656 1_554 36.67(4) ?
    S2 Ba1 Zr1 5_666 1_554 84.67(4) ?
    S2 Ba1 Zr1 3_646 1_554 150.81(4) ?
    Zr1 Ba1 Zr1 2_664 1_554 73.368(16) ?
    Zr1 Ba1 Zr1 4 1_554 115.61(2) ?
    Zr1 Ba1 Zr1 3_645 1_554 71.73(3) ?
    Zr1 S1 Zr1 . 3_646 160.24(13) ?
    Zr1 S1 Ba1 . . 99.69(6) ?
    Zr1 S1 Ba1 3_646 . 99.69(6) ?
    Zr1 S1 Ba1 . 6_556 89.28(7) ?
    Zr1 S1 Ba1 3_646 6_556 89.28(7) ?
    Ba1 S1 Ba1 . 6_556 105.45(9) ?
    Zr1 S2 Zr1 . 2_565 156.89(9) ?
    Zr1 S2 Ba1 . 1_556 96.20(7) ?
    Zr1 S2 Ba1 2_565 1_556 106.84(7) ?
    Zr1 S2 Ba1 . 6_556 85.22(6) ?
    Zr1 S2 Ba1 2_565 6_556 90.38(6) ?
    Ba1 S2 Ba1 1_556 6_556 96.18(6) ?
    Zr1 S2 Ba1 . 5_666 93.26(6) ?
    Zr1 S2 Ba1 2_565 5_666 84.77(6) ?
    Ba1 S2 Ba1 1_556 5_666 99.85(6) ?
    Ba1 S2 Ba1 6_556 5_666 163.97(7) ?
    S1 Zr1 S1 5_666 . 180.0 ?
    S1 Zr1 S2 5_666 . 89.78(8) ?
    S1 Zr1 S2 . . 90.22(8) ?
    S1 Zr1 S2 5_666 5_666 90.22(8) ?
    S1 Zr1 S2 . 5_666 89.78(8) ?
    S2 Zr1 S2 . 5_666 180.0 ?
    S1 Zr1 S2 5_666 6_657 90.79(8) ?
    S1 Zr1 S2 . 6_657 89.21(8) ?
    S2 Zr1 S2 . 6_657 89.54(3) ?
    S2 Zr1 S2 5_666 6_657 90.46(3) ?
    S1 Zr1 S2 5_666 2_564 89.21(8) ?
    S1 Zr1 S2 . 2_564 90.79(8) ?
    S2 Zr1 S2 . 2_564 90.46(3) ?
    S2 Zr1 S2 5_666 2_564 89.54(3) ?
    S2 Zr1 S2 6_657 2_564 180.0 ?
    S1 Zr1 Ba1 5_666 2_665 52.23(7) ?
    S1 Zr1 Ba1 . 2_665 127.77(7) ?
    S2 Zr1 Ba1 . 2_665 123.64(5) ?
    S2 Zr1 Ba1 5_666 2_665 56.36(5) ?
    S2 Zr1 Ba1 6_657 2_665 56.73(5) ?
    S2 Zr1 Ba1 2_564 2_665 123.27(5) ?
    S1 Zr1 Ba1 5_666 6_556 127.77(7) ?
    S1 Zr1 Ba1 . 6_556 52.23(7) ?
    S2 Zr1 Ba1 . 6_556 56.36(5) ?
    S2 Zr1 Ba1 5_666 6_556 123.64(5) ?
    S2 Zr1 Ba1 6_657 6_556 123.27(5) ?
    S2 Zr1 Ba1 2_564 6_556 56.73(5) ?
    Ba1 Zr1 Ba1 2_665 6_556 180.0 ?
    S1 Zr1 Ba1 5_666 1_556 115.98(7) ?
    S1 Zr1 Ba1 . 1_556 64.02(7) ?
    S2 Zr1 Ba1 . 1_556 47.49(5) ?
    S2 Zr1 Ba1 5_666 1_556 132.51(5) ?
    S2 Zr1 Ba1 6_657 1_556 52.95(5) ?
    S2 Zr1 Ba1 2_564 1_556 127.05(5) ?
    Ba1 Zr1 Ba1 2_665 1_556 108.251(19) ?
    Ba1 Zr1 Ba1 6_556 1_556 71.749(18) ?
    S1 Zr1 Ba1 5_666 5_665 64.02(7) ?
    S1 Zr1 Ba1 . 5_665 115.98(7) ?
    S2 Zr1 Ba1 . 5_665 132.51(5) ?
    S2 Zr1 Ba1 5_666 5_665 47.49(5) ?
    S2 Zr1 Ba1 6_657 5_665 127.05(5) ?
    S2 Zr1 Ba1 2_564 5_665 52.95(5) ?
    Ba1 Zr1 Ba1 2_665 5_665 71.749(19) ?
    Ba1 Zr1 Ba1 6_556 5_665 108.251(19) ?
    Ba1 Zr1 Ba1 1_556 5_665 180.0 ?



