

data_x

 

_audit_creation_method            SHELXL-97

_chemical_name_systematic

;

 ?

;

_chemical_name_common             ?

_chemical_melting_point           ?

_chemical_formula_moiety          ?

_chemical_formula_sum

 'Ag Ba4 Ga5 P8'

_chemical_formula_weight          1253.59

 

loop_

 _atom_type_symbol

 _atom_type_description

 _atom_type_scat_dispersion_real

 _atom_type_scat_dispersion_imag

 _atom_type_scat_source

 'P'  'P'   0.1023   0.0942

 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

 'Ga'  'Ga'   0.2307   1.6083

 '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                    7.294(9)

_cell_length_b                    18.03(2)

_cell_length_c                    6.557(8)

_cell_angle_alpha                 90.00

_cell_angle_beta                  90.00

_cell_angle_gamma                 90.00

_cell_volume                      862.0(18)

_cell_formula_units_Z             2

_cell_measurement_temperature     296(2)

_cell_measurement_reflns_used     1185

_cell_measurement_theta_min       3.01

_cell_measurement_theta_max       27.44

 

_exptl_crystal_description        block

_exptl_crystal_colour             black

_exptl_crystal_size_max           0.12

_exptl_crystal_size_mid           0.05

_exptl_crystal_size_min           0.03

_exptl_crystal_density_meas       ?

_exptl_crystal_density_diffrn     4.830

_exptl_crystal_density_method     'not measured'

_exptl_crystal_F_000              1092

_exptl_absorpt_coefficient_mu     18.478

_exptl_absorpt_correction_type    multi-scan

_exptl_absorpt_correction_T_min   0.2152

_exptl_absorpt_correction_T_max   0.6071

_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   'CCD area detector'

_diffrn_measurement_method        'phi and omega scans'

_diffrn_detector_area_resol_mean  ?

_diffrn_standards_number          ?

_diffrn_standards_interval_count  ?

_diffrn_standards_interval_time   ?

_diffrn_standards_decay_%         ?

_diffrn_reflns_number             2383

_diffrn_reflns_av_R_equivalents   0.0325

_diffrn_reflns_av_sigmaI/netI     0.0433

_diffrn_reflns_limit_h_min        -9

_diffrn_reflns_limit_h_max        9

_diffrn_reflns_limit_k_min        -11

_diffrn_reflns_limit_k_max        23

_diffrn_reflns_limit_l_min        -8

_diffrn_reflns_limit_l_max        8

_diffrn_reflns_theta_min          2.26

_diffrn_reflns_theta_max          27.51

_reflns_number_total              966

_reflns_number_gt                 882

_reflns_threshold_expression      >2sigma(I)

 

_computing_data_collection        'Bruker SMART'

_computing_cell_refinement        'Bruker SMART'

_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)+(0.0575P)²+42.0072P] 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      none

_refine_ls_extinction_coef        ?

_refine_ls_abs_structure_details

 'Flack H D (1983), Acta Cryst. A39, 876-881'

_refine_ls_abs_structure_Flack    0.23(8)

_refine_ls_number_reflns          966

_refine_ls_number_parameters      43

_refine_ls_number_restraints      1

_refine_ls_R_factor_all           0.0488

_refine_ls_R_factor_gt            0.0450

_refine_ls_wR_factor_ref          0.1211

_refine_ls_wR_factor_gt           0.1177

_refine_ls_goodness_of_fit_ref    1.122

_refine_ls_restrained_S_all       1.121

_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

Ba1 Ba 0.81096(10) 0.60903(4) 0.7542(2) 0.0204(2) Uani 1 1 d . . .

Ga2 Ga 1.0000 1.0000 1.0000(5) 0.0190(4) Uani 0.50 2 d SP . .

Ag Ag 1.0000 1.0000 1.0000(5) 0.0190(4) Uani 0.50 2 d SP . .

Ga1 Ga 0.84653(15) 0.80091(6) 0.7492(4) 0.0088(3) Uani 1 1 d . . .

P1 P 0.7961(4) 0.93114(16) 0.7481(13) 0.0210(7) Uani 1 1 d . . .

P2 P 0.5889(5) 0.7568(2) 0.9334(6) 0.0121(7) 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

Ba1 P2 3.287(5) 6_664 ?

Ba1 P1 3.301(5) 4_645 ?

Ba1 P2 3.331(5) . ?

Ba1 P2 3.367(5) 3_565 ?

Ba1 Ag 3.407(3) 3_465 ?

Ba1 Ga2 3.407(3) 3_465 ?

Ba1 P1 3.409(9) 6_665 ?

Ba1 Ga2 3.433(3) 5_444 ?

Ba1 Ag 3.433(3) 5_444 ?

Ba1 Ga1 3.468(4) . ?

Ba1 P1 3.485(9) 6_664 ?

Ba1 P1 3.612(5) 3_565 ?

Ga2 P1 2.529(7) 8_645 ?

Ga2 P1 2.529(7) 7_465 ?

Ga2 P1 2.546(7) . ?

Ga2 P1 2.546(7) 2_775 ?

Ga2 Ba1 3.407(3) 4_655 ?

Ga2 Ba1 3.407(3) 3_565 ?

Ga2 Ba1 3.433(3) 5 ?

Ga2 Ba1 3.433(3) 6_665 ?

Ga1 P2 2.365(5) 6_664 ?

Ga1 P2 2.371(4) . ?

Ga1 P1 2.376(4) . ?

Ga1 P2 2.380(4) 3_565 ?

Ga1 Ba1 3.756(4) 3_565 ?

Ga1 Ba1 3.807(4) 6_664 ?

Ga1 Ba1 3.862(5) 6_665 ?

P1 Ag 2.529(7) 7_464 ?

P1 Ga2 2.529(7) 7_464 ?

P1 Ba1 3.301(5) 4_655 ?

P1 Ba1 3.409(9) 6_664 ?

P1 Ba1 3.485(9) 6_665 ?

P1 Ba1 3.612(5) 3_465 ?

P2 Ga1 2.365(5) 6_665 ?

P2 Ga1 2.380(4) 3_465 ?

P2 Ba1 3.287(5) 6_665 ?

P2 Ba1 3.367(5) 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

P2 Ba1 P1 139.43(18) 6_664 4_645 ?

P2 Ba1 P2 75.25(10) 6_664 . ?

P1 Ba1 P2 131.75(13) 4_645 . ?

P2 Ba1 P2 63.97(10) 6_664 3_565 ?

P1 Ba1 P2 147.61(13) 4_645 3_565 ?

P2 Ba1 P2 66.13(9) . 3_565 ?

P2 Ba1 Ag 151.06(7) 6_664 3_465 ?

P1 Ba1 Ag 44.57(12) 4_645 3_465 ?

P2 Ba1 Ag 88.32(11) . 3_465 ?

P2 Ba1 Ag 130.55(11) 3_565 3_465 ?

P2 Ba1 Ga2 151.06(7) 6_664 3_465 ?

P1 Ba1 Ga2 44.57(12) 4_645 3_465 ?

P2 Ba1 Ga2 88.32(11) . 3_465 ?

P2 Ba1 Ga2 130.55(11) 3_565 3_465 ?

Ag Ba1 Ga2 0.0 3_465 3_465 ?

P2 Ba1 P1 144.58(10) 6_664 6_665 ?

P1 Ba1 P1 75.57(12) 4_645 6_665 ?

P2 Ba1 P1 73.94(10) . 6_665 ?

P2 Ba1 P1 87.65(11) 3_565 6_665 ?

Ag Ba1 P1 43.57(9) 3_465 6_665 ?

Ga2 Ba1 P1 43.57(9) 3_465 6_665 ?

P2 Ba1 Ga2 104.91(11) 6_664 5_444 ?

P1 Ba1 Ga2 44.08(12) 4_645 5_444 ?

P2 Ba1 Ga2 107.92(10) . 5_444 ?

P2 Ba1 Ga2 168.06(8) 3_565 5_444 ?

Ag Ba1 Ga2 57.28(7) 3_465 5_444 ?

Ga2 Ba1 Ga2 57.28(7) 3_465 5_444 ?

P1 Ba1 Ga2 100.85(11) 6_665 5_444 ?

P2 Ba1 Ag 104.91(11) 6_664 5_444 ?

P1 Ba1 Ag 44.08(12) 4_645 5_444 ?

P2 Ba1 Ag 107.92(10) . 5_444 ?

P2 Ba1 Ag 168.06(8) 3_565 5_444 ?

Ag Ba1 Ag 57.28(7) 3_465 5_444 ?

Ga2 Ba1 Ag 57.28(7) 3_465 5_444 ?

P1 Ba1 Ag 100.85(11) 6_665 5_444 ?

Ga2 Ba1 Ag 0.0 5_444 5_444 ?

P2 Ba1 Ga1 40.87(9) 6_664 . ?

P1 Ba1 Ga1 170.52(7) 4_645 . ?

P2 Ba1 Ga1 40.75(8) . . ?

P2 Ba1 Ga1 40.72(8) 3_565 . ?

Ag Ba1 Ga1 129.01(6) 3_465 . ?

Ga2 Ba1 Ga1 129.01(6) 3_465 . ?

P1 Ba1 Ga1 103.76(8) 6_665 . ?

Ga2 Ba1 Ga1 128.01(6) 5_444 . ?

Ag Ba1 Ga1 128.01(6) 5_444 . ?

P2 Ba1 P1 66.01(12) 6_664 6_664 ?

P1 Ba1 P1 74.55(13) 4_645 6_664 ?

P2 Ba1 P1 113.14(9) . 6_664 ?

P2 Ba1 P1 128.05(10) 3_565 6_664 ?

Ag Ba1 P1 100.45(10) 3_465 6_664 ?

Ga2 Ba1 P1 100.45(10) 3_465 6_664 ?

P1 Ba1 P1 144.00(11) 6_665 6_664 ?

Ga2 Ba1 P1 43.17(8) 5_444 6_664 ?

Ag Ba1 P1 43.17(8) 5_444 6_664 ?

Ga1 Ba1 P1 102.42(8) . 6_664 ?

P2 Ba1 P1 85.57(12) 6_664 3_565 ?

P1 Ba1 P1 92.12(8) 4_645 3_565 ?

P2 Ba1 P1 129.82(10) . 3_565 ?

P2 Ba1 P1 63.77(11) 3_565 3_565 ?

Ag Ba1 P1 122.80(11) 3_465 3_565 ?

Ga2 Ba1 P1 122.80(11) 3_465 3_565 ?

P1 Ba1 P1 101.09(17) 6_665 3_565 ?

Ga2 Ba1 P1 121.81(11) 5_444 3_565 ?

Ag Ba1 P1 121.81(11) 5_444 3_565 ?

Ga1 Ba1 P1 97.27(6) . 3_565 ?

P1 Ba1 P1 99.64(17) 6_664 3_565 ?

P1 Ga2 P1 100.0(3) 8_645 7_465 ?

P1 Ga2 P1 121.43(15) 8_645 . ?

P1 Ga2 P1 108.25(15) 7_465 . ?

P1 Ga2 P1 108.25(15) 8_645 2_775 ?

P1 Ga2 P1 121.43(15) 7_465 2_775 ?

P1 Ga2 P1 99.1(3) . 2_775 ?

P1 Ga2 Ba1 168.18(19) 8_645 4_655 ?

P1 Ga2 Ba1 68.27(18) 7_465 4_655 ?

P1 Ga2 Ba1 65.50(12) . 4_655 ?

P1 Ga2 Ba1 78.50(14) 2_775 4_655 ?

P1 Ga2 Ba1 68.27(18) 8_645 3_565 ?

P1 Ga2 Ba1 168.18(19) 7_465 3_565 ?

P1 Ga2 Ba1 78.50(14) . 3_565 ?

P1 Ga2 Ba1 65.50(12) 2_775 3_565 ?

Ba1 Ga2 Ba1 123.52(12) 4_655 3_565 ?

P1 Ga2 Ba1 65.19(12) 8_645 5 ?

P1 Ga2 Ba1 78.19(14) 7_465 5 ?

P1 Ga2 Ba1 168.55(19) . 5 ?

P1 Ga2 Ba1 69.50(18) 2_775 5 ?

Ba1 Ga2 Ba1 109.83(9) 4_655 5 ?

Ba1 Ga2 Ba1 96.90(9) 3_565 5 ?

P1 Ga2 Ba1 78.19(14) 8_645 6_665 ?

P1 Ga2 Ba1 65.19(12) 7_465 6_665 ?

P1 Ga2 Ba1 69.50(18) . 6_665 ?

P1 Ga2 Ba1 168.55(19) 2_775 6_665 ?

Ba1 Ga2 Ba1 96.90(9) 4_655 6_665 ?

Ba1 Ga2 Ba1 109.83(9) 3_565 6_665 ?

Ba1 Ga2 Ba1 121.92(12) 5 6_665 ?

P2 Ga1 P2 117.14(11) 6_664 . ?

P2 Ga1 P1 117.6(3) 6_664 . ?

P2 Ga1 P1 102.14(17) . . ?

P2 Ga1 P2 95.98(13) 6_664 3_565 ?

P2 Ga1 P2 100.59(17) . 3_565 ?

P1 Ga1 P2 123.24(19) . 3_565 ?

P2 Ga1 Ba1 65.45(10) 6_664 . ?

P2 Ga1 Ba1 66.51(9) . . ?

P1 Ga1 Ba1 166.81(9) . . ?

P2 Ga1 Ba1 67.36(10) 3_565 . ?

P2 Ga1 Ba1 91.03(10) 6_664 3_565 ?

P2 Ga1 Ba1 148.79(15) . 3_565 ?

P1 Ga1 Ba1 73.30(10) . 3_565 ?

P2 Ga1 Ba1 60.96(11) 3_565 3_565 ?

Ba1 Ga1 Ba1 119.89(5) . 3_565 ?

P2 Ga1 Ba1 60.06(13) 6_664 6_664 ?

P2 Ga1 Ba1 109.76(12) . 6_664 ?

P1 Ga1 Ba1 61.9(2) . 6_664 ?

P2 Ga1 Ba1 147.46(12) 3_565 6_664 ?

Ba1 Ga1 Ba1 114.24(8) . 6_664 ?

Ba1 Ga1 Ba1 95.46(7) 3_565 6_664 ?

P2 Ga1 Ba1 174.16(10) 6_664 6_665 ?

P2 Ga1 Ba1 57.91(12) . 6_665 ?

P1 Ga1 Ba1 62.7(2) . 6_665 ?

P2 Ga1 Ba1 88.27(14) 3_565 6_665 ?

Ba1 Ga1 Ba1 112.88(8) . 6_665 ?

Ba1 Ga1 Ba1 94.54(7) 3_565 6_665 ?

Ba1 Ga1 Ba1 117.52(9) 6_664 6_665 ?

Ga1 P1 Ag 113.3(2) . 7_464 ?

Ga1 P1 Ga2 113.3(2) . 7_464 ?

Ag P1 Ga2 0.00(11) 7_464 7_464 ?

Ga1 P1 Ga2 112.9(2) . . ?

Ag P1 Ga2 80.48(12) 7_464 . ?

Ga2 P1 Ga2 80.48(12) 7_464 . ?

Ga1 P1 Ba1 175.13(15) . 4_655 ?

Ag P1 Ba1 70.74(11) 7_464 4_655 ?

Ga2 P1 Ba1 70.74(11) 7_464 4_655 ?

Ga2 P1 Ba1 69.92(10) . 4_655 ?

Ga1 P1 Ba1 80.1(2) . 6_664 ?

Ag P1 Ba1 68.2(2) 7_464 6_664 ?

Ga2 P1 Ba1 68.2(2) 7_464 6_664 ?

Ga2 P1 Ba1 148.6(2) . 6_664 ?

Ba1 P1 Ba1 99.41(18) 4_655 6_664 ?

Ga1 P1 Ba1 80.0(2) . 6_665 ?

Ag P1 Ba1 147.8(2) 7_464 6_665 ?

Ga2 P1 Ba1 147.8(2) 7_464 6_665 ?

Ga2 P1 Ba1 67.3(2) . 6_665 ?

Ba1 P1 Ba1 97.90(18) 4_655 6_665 ?

Ba1 P1 Ba1 144.00(11) 6_664 6_665 ?

Ga1 P1 Ba1 87.33(10) . 3_465 ?

Ag P1 Ba1 132.9(3) 7_464 3_465 ?

Ga2 P1 Ba1 132.9(3) 7_464 3_465 ?

Ga2 P1 Ba1 131.5(3) . 3_465 ?

Ba1 P1 Ba1 87.87(8) 4_655 3_465 ?

Ba1 P1 Ba1 75.13(11) 6_664 3_465 ?

Ba1 P1 Ba1 74.24(11) 6_665 3_465 ?

Ga1 P2 Ga1 115.83(16) 6_665 . ?

Ga1 P2 Ga1 113.57(16) 6_665 3_465 ?

Ga1 P2 Ga1 118.5(2) . 3_465 ?

Ga1 P2 Ba1 73.68(14) 6_665 6_665 ?

Ga1 P2 Ba1 84.43(13) . 6_665 ?

Ga1 P2 Ba1 144.20(14) 3_465 6_665 ?

Ga1 P2 Ba1 81.98(13) 6_665 . ?

Ga1 P2 Ba1 72.74(12) . . ?

Ga1 P2 Ba1 80.38(13) 3_465 . ?

Ba1 P2 Ba1 134.90(12) 6_665 . ?

Ga1 P2 Ba1 137.84(15) 6_665 3_465 ?

Ga1 P2 Ba1 93.36(14) . 3_465 ?

Ga1 P2 Ba1 71.92(12) 3_465 3_465 ?

Ba1 P2 Ba1 80.13(11) 6_665 3_465 ?

Ba1 P2 Ba1 138.06(14) . 3_465 ?

 

_diffrn_measured_fraction_theta_max    0.989

_diffrn_reflns_theta_full              27.51

_diffrn_measured_fraction_theta_full   0.989

_refine_diff_density_max    2.480

_refine_diff_density_min   -2.961

_refine_diff_density_rms    0.462

