

data_x1

 

_audit_creation_method            SHELXL-97

_chemical_name_systematic

;

 ?

;

_chemical_name_common             ?

_chemical_melting_point           ?

_chemical_formula_moiety          ?

_chemical_formula_sum

 'Ag As8 Ba4 Ga5'

_chemical_formula_weight          1605.19

 

loop_

 _atom_type_symbol

 _atom_type_description

 _atom_type_scat_dispersion_real

 _atom_type_scat_dispersion_imag

 _atom_type_scat_source

 'Ga'  'Ga'   0.2307   1.6083

 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

 'As'  'As'   0.0499   2.0058

 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

 'Ag'  'Ag'  -0.8971   1.1015

 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

 'Ba'  'Ba'  -0.3244   2.2819

 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

 

_symmetry_cell_setting            Orthorhombic

_symmetry_space_group_name_H-M    Iba2

 

loop_

 _symmetry_equiv_pos_as_xyz

 'x, y, z'

 '-x, -y, z'

 'x+1/2, -y+1/2, z'

 '-x+1/2, y+1/2, z'

 'x+1/2, y+1/2, z+1/2'

 '-x+1/2, -y+1/2, z+1/2'

 'x+1, -y+1, z+1/2'

 '-x+1, y+1, z+1/2'

 

_cell_length_a                    7.4769(8)

_cell_length_b                    18.5766(19)

_cell_length_c                    6.7590(7)

_cell_angle_alpha                 90.00

_cell_angle_beta                  90.00

_cell_angle_gamma                 90.00

_cell_volume                      938.79(17)

_cell_formula_units_Z             2

_cell_measurement_temperature     296(2)

_cell_measurement_reflns_used     2861

_cell_measurement_theta_min       2.94

_cell_measurement_theta_max       27.23

 

_exptl_crystal_description        needle

_exptl_crystal_colour             black

_exptl_crystal_size_max           0.20

_exptl_crystal_size_mid           0.03

_exptl_crystal_size_min           0.02

_exptl_crystal_density_meas       ?

_exptl_crystal_density_diffrn     5.679

_exptl_crystal_density_method     'not measured'

_exptl_crystal_F_000              1380

_exptl_absorpt_coefficient_mu     30.277

_exptl_absorpt_correction_type    multi-scan

_exptl_absorpt_correction_T_min   0.0647

_exptl_absorpt_correction_T_max   0.5827

_exptl_absorpt_process_details    'SADABS (Sheldrick, 2003)'

 

_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   'Bruker APEX-II CCD'

_diffrn_measurement_method        'φ and ω scans'

_diffrn_detector_area_resol_mean  ?

_diffrn_standards_number          0

_diffrn_standards_interval_count  ?

_diffrn_standards_interval_time   ?

_diffrn_standards_decay_%         ?

_diffrn_reflns_number             5300

_diffrn_reflns_av_R_equivalents   0.0376

_diffrn_reflns_av_sigmaI/netI     0.0281

_diffrn_reflns_limit_h_min        -9

_diffrn_reflns_limit_h_max        9

_diffrn_reflns_limit_k_min        -24

_diffrn_reflns_limit_k_max        23

_diffrn_reflns_limit_l_min        -8

_diffrn_reflns_limit_l_max        8

_diffrn_reflns_theta_min          2.19

_diffrn_reflns_theta_max          27.50

_reflns_number_total              1078

_reflns_number_gt                 1056

_reflns_threshold_expression      >2sigma(I)

 

_computing_data_collection        'Bruker APEX2'

_computing_cell_refinement        'Bruker SAINT'

_computing_data_reduction         'Bruker SAINT'

_computing_structure_solution     'SHELXS-97 (Sheldrick, 1990)'

_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)'

_computing_molecular_graphics     'Bruker SHELXTL'

_computing_publication_material   'Bruker SHELXTL'

 

_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)+(0.0235P)²+0.0000P] where P=(Fo²+2Fc²)/3'

_atom_sites_solution_primary      direct

_atom_sites_solution_secondary    difmap

_atom_sites_solution_hydrogens    ?

_refine_ls_hydrogen_treatment     ?

_refine_ls_extinction_method      SHELXL

_refine_ls_extinction_coef        0.00297(11)

_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    0.12(3)

_refine_ls_number_reflns          1078

_refine_ls_number_parameters      44

_refine_ls_number_restraints      1

_refine_ls_R_factor_all           0.0213

_refine_ls_R_factor_gt            0.0207

_refine_ls_wR_factor_ref          0.0499

_refine_ls_wR_factor_gt           0.0496

_refine_ls_goodness_of_fit_ref    1.172

_refine_ls_restrained_S_all       1.171

_refine_ls_shift/su_max           0.001

_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

Ba Ba 0.80368(4) 0.610100(18) 0.75587(6) 0.01815(12) Uani 1 1 d . . .

Ag Ag 1.0000 1.0000 1.00000(14) 0.01522(17) Uani 0.50 2 d SP . .

Ga1 Ga 0.84459(7) 0.80115(3) 0.74621(13) 0.01073(14) Uani 1 1 d . . .

Ga2 Ga 1.0000 1.0000 1.00000(14) 0.01522(17) Uani 0.50 2 d SP . .

As1 As 0.79006(8) 0.93160(3) 0.74750(15) 0.02013(16) Uani 1 1 d . . .

As2 As 0.58454(8) 0.75922(3) 0.93462(10) 0.01127(15) Uani 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

Ba As2 3.3625(8) 6_664 ?

Ba As1 3.3896(7) 4_645 ?

Ba As2 3.4297(7) 3_565 ?

Ba As2 3.4377(7) . ?

Ba Ga2 3.4730(6) 3_465 ?

Ba Ag 3.4730(6) 3_465 ?

Ba As1 3.4833(11) 6_665 ?

Ba Ag 3.5113(6) 5_444 ?

Ba Ga2 3.5113(6) 5_444 ?

Ba Ga1 3.5628(7) . ?

Ba As1 3.5914(11) 6_664 ?

Ba As1 3.7187(7) 3_565 ?

Ag As1 2.6223(10) 7_465 ?

Ag As1 2.6223(10) 8_645 ?

Ag As1 2.6440(10) . ?

Ag As1 2.6440(10) 2_775 ?

Ag Ag 3.3795(4) 7_464 ?

Ag Ag 3.3795(4) 7_465 ?

Ag Ba 3.4730(6) 4_655 ?

Ag Ba 3.4730(6) 3_565 ?

Ag Ba 3.5113(6) 5 ?

Ag Ba 3.5113(6) 6_665 ?

Ga1 As2 2.4441(10) 6_664 ?

Ga1 As2 2.4514(9) . ?

Ga1 As1 2.4575(8) . ?

Ga1 As2 2.4694(9) 3_565 ?

Ga1 Ba 3.8085(7) 3_565 ?

Ga1 Ba 3.8641(9) 6_664 ?

As1 Ga2 2.6223(10) 7_464 ?

As1 Ag 2.6223(10) 7_464 ?

As1 Ba 3.3896(7) 4_655 ?

As1 Ba 3.4833(11) 6_664 ?

As1 Ba 3.5914(11) 6_665 ?

As1 Ba 3.7187(7) 3_465 ?

As2 Ga1 2.4441(10) 6_665 ?

As2 Ga1 2.4694(9) 3_465 ?

As2 Ba 3.3625(8) 6_665 ?

As2 Ba 3.4297(7) 3_465 ?

 

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

As2 Ba As1 138.32(2) 6_664 4_645 ?

As2 Ba As2 64.167(14) 6_664 3_565 ?

As1 Ba As2 145.58(2) 4_645 3_565 ?

As2 Ba As2 76.329(13) 6_664 . ?

As1 Ba As2 134.07(2) 4_645 . ?

As2 Ba As2 66.275(11) 3_565 . ?

As2 Ba Ga2 153.443(17) 6_664 3_465 ?

As1 Ba Ga2 45.303(16) 4_645 3_465 ?

As2 Ba Ga2 130.52(2) 3_565 3_465 ?

As2 Ba Ga2 89.768(16) . 3_465 ?

As2 Ba Ag 153.443(17) 6_664 3_465 ?

As1 Ba Ag 45.303(16) 4_645 3_465 ?

As2 Ba Ag 130.52(2) 3_565 3_465 ?

As2 Ba Ag 89.768(16) . 3_465 ?

Ga2 Ba Ag 0.0 3_465 3_465 ?

As2 Ba As1 145.751(19) 6_664 6_665 ?

As1 Ba As1 75.921(18) 4_645 6_665 ?

As2 Ba As1 86.823(18) 3_565 6_665 ?

As2 Ba As1 75.407(17) . 6_665 ?

Ga2 Ba As1 44.292(18) 3_465 6_665 ?

Ag Ba As1 44.292(18) 3_465 6_665 ?

As2 Ba Ag 105.26(2) 6_664 5_444 ?

As1 Ba Ag 44.623(16) 4_645 5_444 ?

As2 Ba Ag 169.03(2) 3_565 5_444 ?

As2 Ba Ag 109.527(16) . 5_444 ?

Ga2 Ba Ag 57.874(8) 3_465 5_444 ?

Ag Ba Ag 57.874(8) 3_465 5_444 ?

As1 Ba Ag 102.13(2) 6_665 5_444 ?

As2 Ba Ga2 105.26(2) 6_664 5_444 ?

As1 Ba Ga2 44.623(16) 4_645 5_444 ?

As2 Ba Ga2 169.03(2) 3_565 5_444 ?

As2 Ba Ga2 109.527(16) . 5_444 ?

Ga2 Ba Ga2 57.874(8) 3_465 5_444 ?

Ag Ba Ga2 57.874(8) 3_465 5_444 ?

As1 Ba Ga2 102.13(2) 6_665 5_444 ?

Ag Ba Ga2 0.0 5_444 5_444 ?

As2 Ba Ga1 41.205(18) 6_664 . ?

As1 Ba Ga1 172.710(19) 4_645 . ?

As2 Ba Ga1 41.305(16) 3_565 . ?

As2 Ba Ga1 40.947(15) . . ?

Ga2 Ba Ga1 130.654(16) 3_465 . ?

Ag Ba Ga1 130.654(16) 3_465 . ?

As1 Ba Ga1 104.852(19) 6_665 . ?

Ag Ba Ga1 128.809(17) 5_444 . ?

Ga2 Ba Ga1 128.809(17) 5_444 . ?

As2 Ba As1 65.572(18) 6_664 6_664 ?

As1 Ba As1 74.494(18) 4_645 6_664 ?

As2 Ba As1 127.533(19) 3_565 6_664 ?

As2 Ba As1 114.649(18) . 6_664 ?

Ga2 Ba As1 101.534(19) 3_465 6_664 ?

Ag Ba As1 101.534(19) 3_465 6_664 ?

As1 Ba As1 145.63(2) 6_665 6_664 ?

Ag Ba As1 43.692(17) 5_444 6_664 ?

Ga2 Ba As1 43.692(17) 5_444 6_664 ?

Ga1 Ba As1 102.363(19) . 6_664 ?

As2 Ba As1 84.117(17) 6_664 3_565 ?

As1 Ba As1 89.895(16) 4_645 3_565 ?

As2 Ba As1 63.516(16) 3_565 3_565 ?

As2 Ba As1 129.742(18) . 3_565 ?

Ga2 Ba As1 121.594(17) 3_465 3_565 ?

Ag Ba As1 121.594(17) 3_465 3_565 ?

As1 Ba As1 99.49(2) 6_665 3_565 ?

Ag Ba As1 120.234(17) 5_444 3_565 ?

Ga2 Ba As1 120.234(17) 5_444 3_565 ?

Ga1 Ba As1 97.082(15) . 3_565 ?

As1 Ba As1 97.55(2) 6_664 3_565 ?

As1 Ag As1 100.73(5) 7_465 8_645 ?

As1 Ag As1 106.81(2) 7_465 . ?

As1 Ag As1 122.30(2) 8_645 . ?

As1 Ag As1 122.30(2) 7_465 2_775 ?

As1 Ag As1 106.81(2) 8_645 2_775 ?

As1 Ag As1 99.60(5) . 2_775 ?

As1 Ag Ag 129.64(2) 7_465 7_464 ?

As1 Ag Ag 129.64(2) 8_645 7_464 ?

As1 Ag Ag 49.80(2) . 7_464 ?

As1 Ag Ag 49.80(2) 2_775 7_464 ?

As1 Ag Ag 50.36(2) 7_465 7_465 ?

As1 Ag Ag 50.36(2) 8_645 7_465 ?

As1 Ag Ag 130.20(2) . 7_465 ?

As1 Ag Ag 130.20(2) 2_775 7_465 ?

Ag Ag Ag 180.000(1) 7_464 7_465 ?

As1 Ag Ba 68.06(2) 7_465 4_655 ?

As1 Ag Ba 168.46(3) 8_645 4_655 ?

As1 Ag Ba 65.68(2) . 4_655 ?

As1 Ag Ba 78.37(2) 2_775 4_655 ?

Ag Ag Ba 61.632(15) 7_464 4_655 ?

Ag Ag Ba 118.368(15) 7_465 4_655 ?

As1 Ag Ba 168.46(3) 7_465 3_565 ?

As1 Ag Ba 68.06(2) 8_645 3_565 ?

As1 Ag Ba 78.37(2) . 3_565 ?

As1 Ag Ba 65.681(19) 2_775 3_565 ?

Ag Ag Ba 61.632(15) 7_464 3_565 ?

Ag Ag Ba 118.368(15) 7_465 3_565 ?

Ba Ag Ba 123.26(3) 4_655 3_565 ?

As1 Ag Ba 77.92(2) 7_465 5 ?

As1 Ag Ba 65.23(2) 8_645 5 ?

As1 Ag Ba 169.02(3) . 5 ?

As1 Ag Ba 69.76(2) 2_775 5 ?

Ag Ag Ba 119.506(15) 7_464 5 ?

Ag Ag Ba 60.494(15) 7_465 5 ?

Ba Ag Ba 108.285(13) 4_655 5 ?

Ba Ag Ba 98.875(13) 3_565 5 ?

As1 Ag Ba 65.23(2) 7_465 6_665 ?

As1 Ag Ba 77.92(2) 8_645 6_665 ?

As1 Ag Ba 69.76(2) . 6_665 ?

As1 Ag Ba 169.02(3) 2_775 6_665 ?

Ag Ag Ba 119.506(15) 7_464 6_665 ?

Ag Ag Ba 60.494(15) 7_465 6_665 ?

Ba Ag Ba 98.875(13) 4_655 6_665 ?

Ba Ag Ba 108.285(12) 3_565 6_665 ?

Ba Ag Ba 120.99(3) 5 6_665 ?

As2 Ga1 As2 118.28(3) 6_664 . ?

As2 Ga1 As1 119.44(5) 6_664 . ?

As2 Ga1 As1 100.36(3) . . ?

As2 Ga1 As2 94.50(3) 6_664 3_565 ?

As2 Ga1 As2 99.44(3) . 3_565 ?

As1 Ga1 As2 124.51(4) . 3_565 ?

As2 Ga1 Ba 65.00(2) 6_664 . ?

As2 Ga1 Ba 66.788(19) . . ?

As1 Ga1 Ba 165.47(3) . . ?

As2 Ga1 Ba 66.46(2) 3_565 . ?

As2 Ga1 Ba 91.03(2) 6_664 3_565 ?

As2 Ga1 Ba 147.51(4) . 3_565 ?

As1 Ga1 Ba 73.89(2) . 3_565 ?

As2 Ga1 Ba 62.16(2) 3_565 3_565 ?

Ba Ga1 Ba 120.551(18) . 3_565 ?

As2 Ga1 Ba 61.24(2) 6_664 6_664 ?

As2 Ga1 Ba 110.71(3) . 6_664 ?

As1 Ga1 Ba 62.27(3) . 6_664 ?

As2 Ga1 Ba 147.62(3) 3_565 6_664 ?

Ba Ga1 Ba 114.59(2) . 6_664 ?

Ba Ga1 Ba 95.082(18) 3_565 6_664 ?

Ga1 As1 Ga2 112.10(4) . 7_464 ?

Ga1 As1 Ag 112.10(4) . 7_464 ?

Ga2 As1 Ag 0.00(3) 7_464 7_464 ?

Ga1 As1 Ag 112.19(4) . . ?

Ga2 As1 Ag 79.839(17) 7_464 . ?

Ag As1 Ag 79.839(17) 7_464 . ?

Ga1 As1 Ba 177.50(3) . 4_655 ?

Ga2 As1 Ba 70.150(17) 7_464 4_655 ?

Ag As1 Ba 70.150(17) 7_464 4_655 ?

Ag As1 Ba 69.017(16) . 4_655 ?

Ga1 As1 Ba 79.09(3) . 6_664 ?

Ga2 As1 Ba 67.64(3) 7_464 6_664 ?

Ag As1 Ba 67.64(3) 7_464 6_664 ?

Ag As1 Ba 147.36(3) . 6_664 ?

Ba As1 Ba 101.06(2) 4_655 6_664 ?

Ga1 As1 Ba 79.81(3) . 6_665 ?

Ga2 As1 Ba 146.27(3) 7_464 6_665 ?

Ag As1 Ba 146.27(3) 7_464 6_665 ?

Ag As1 Ba 66.54(3) . 6_665 ?

Ba As1 Ba 98.90(2) 4_655 6_665 ?

Ba As1 Ba 145.63(2) 6_664 6_665 ?

Ga1 As1 Ba 87.53(2) . 3_465 ?

Ga2 As1 Ba 134.11(3) 7_464 3_465 ?

Ag As1 Ba 134.11(3) 7_464 3_465 ?

Ag As1 Ba 132.13(3) . 3_465 ?

Ba As1 Ba 90.076(16) 4_655 3_465 ?

Ba As1 Ba 76.785(17) 6_664 3_465 ?

Ba As1 Ba 75.502(17) 6_665 3_465 ?

Ga1 As2 Ga1 114.93(3) 6_665 . ?

Ga1 As2 Ga1 113.18(3) 6_665 3_465 ?

Ga1 As2 Ga1 116.91(4) . 3_465 ?

Ga1 As2 Ba 73.80(2) 6_665 6_665 ?

Ga1 As2 Ba 84.77(3) . 6_665 ?

Ga1 As2 Ba 147.29(3) 3_465 6_665 ?

Ga1 As2 Ba 139.56(3) 6_665 3_465 ?

Ga1 As2 Ba 94.46(2) . 3_465 ?

Ga1 As2 Ba 72.24(2) 3_465 3_465 ?

Ba As2 Ba 82.452(17) 6_665 3_465 ?

Ga1 As2 Ba 80.20(2) 6_665 . ?

Ga1 As2 Ba 72.27(2) . . ?

Ga1 As2 Ba 78.41(2) 3_465 . ?

Ba As2 Ba 133.65(2) 6_665 . ?

Ba As2 Ba 137.59(2) 3_465 . ?

 

_diffrn_measured_fraction_theta_max    1.000

_diffrn_reflns_theta_full              27.50

_diffrn_measured_fraction_theta_full   1.000

_refine_diff_density_max    1.796

_refine_diff_density_min   -1.055

_refine_diff_density_rms    0.279

