 
data_shelx
 
_audit_creation_method            'SHELXL-2016/6'
_shelx_SHELXL_version_number      '2016/6'
_chemical_name_systematic         ?
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          ?
_chemical_formula_sum
 'Al1.50 Ca3 Ga1.50 O14 Si2 Ta' 
_chemical_formula_weight          726.42

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'
 'Al'  'Al'   0.0645   0.0514
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Si'  'Si'   0.0817   0.0704
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Ca'  'Ca'   0.2262   0.3064
 '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'
 'Ta'  'Ta'  -0.7052   6.5227
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 
_space_group_crystal_system       trigonal
_space_group_IT_number            150
_space_group_name_H-M_alt         'P 3 2 1'
_space_group_name_Hall            'P 3 2"'
 
_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'
 '-y, x-y, z'
 '-x+y, -x, z'
 'y, x, -z'
 'x-y, -y, -z'
 '-x, -x+y, -z'
 
_cell_length_a                    8.0801(6)
_cell_length_b                    8.0801(6)
_cell_length_c                    4.9553(4)
_cell_angle_alpha                 90
_cell_angle_beta                  90
_cell_angle_gamma                 120
_cell_volume                      280.18(5)
_cell_formula_units_Z             1
_cell_measurement_temperature     293(2)
_cell_measurement_reflns_used    6511
_cell_measurement_theta_min        2.91
_cell_measurement_theta_max       46.06

_exptl_crystal_description       'Chunk'
_exptl_crystal_colour            'Clear'
_exptl_crystal_density_meas       ?
_exptl_crystal_density_method     ?
_exptl_crystal_density_diffrn     4.305          
_exptl_crystal_F_000              339
_exptl_transmission_factor_min    ?
_exptl_transmission_factor_max    ?
_exptl_crystal_size_max           0.189
_exptl_crystal_size_mid           0.075
_exptl_crystal_size_min           0.044
_exptl_absorpt_coefficient_mu     15.129
_shelx_estimated_absorpt_T_min    0.162
_shelx_estimated_absorpt_T_max    0.556
_exptl_absorpt_correction_type    multi-scan
_exptl_absorpt_correction_T_min   0.2586
_exptl_absorpt_correction_T_max   0.5055
_exptl_absorpt_process_details
;
CrystalClear (Rigaku, 1997--2002)
;
_diffrn_ambient_temperature       293(2)
_diffrn_radiation_wavelength      0.71073
_diffrn_radiation_type            MoK\a
_diffrn_radiation_source          'Rotating Anode'
_diffrn_radiation_monochromator   'Confocal'
_diffrn_radiation_detector        'CCD'
_diffrn_measurement_device
;
Rigaku AFC11 Saturn724+ (4x4 bin mode)
;
_diffrn_measurement_method        'dtprofit.ref'
_diffrn_detector_area_resol_mean  28.5714
_diffrn_reflns_number             5938
_diffrn_reflns_av_unetI/netI      0.0358
_diffrn_reflns_av_R_equivalents   0.0406
_diffrn_reflns_limit_h_min        -16
_diffrn_reflns_limit_h_max        16
_diffrn_reflns_limit_k_min        -16
_diffrn_reflns_limit_k_max        16
_diffrn_reflns_limit_l_min        -8
_diffrn_reflns_limit_l_max        10
_diffrn_reflns_theta_min          2.911
_diffrn_reflns_theta_max          46.053
_diffrn_reflns_theta_full         25.242
_diffrn_measured_fraction_theta_max   0.989
_diffrn_measured_fraction_theta_full  0.962
_diffrn_reflns_Laue_measured_fraction_max    0.989
_diffrn_reflns_Laue_measured_fraction_full   0.962
_diffrn_reflns_point_group_measured_fraction_max   0.969
_diffrn_reflns_point_group_measured_fraction_full  0.942
_reflns_number_total              1606
_reflns_number_gt                 1605
_reflns_threshold_expression      'I > 2σ(I)'
_reflns_Friedel_coverage          0.723
_reflns_Friedel_fraction_max      0.941
_reflns_Friedel_fraction_full     0.910
 
_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        'CrystalClear (Rigaku, 1997--2002)'
_computing_cell_refinement        'CrystalClear (Rigaku, 1997--2002)'
_computing_data_reduction         'CrystalClear (Rigaku, 1997--2002)'
_computing_structure_solution     'SHELXT (Sheldrick, 2014)'
_computing_structure_refinement 'SHELXL-2016/6 (Sheldrick, 2016)'
_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)+(0.0305P)²+0.0430P] 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      'SHELXL-2016/6 (Sheldrick 2016)'
_refine_ls_extinction_coef        0.128(8)
_refine_ls_extinction_expression
 'Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^'
_refine_ls_abs_structure_details
;
 Flack x determined using 673 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack    0.018(5)
_chemical_absolute_configuration  ?
_refine_ls_number_reflns          1606
_refine_ls_number_parameters      43
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.0237
_refine_ls_R_factor_gt            0.0237
_refine_ls_wR_factor_ref          0.0597
_refine_ls_wR_factor_gt           0.0597
_refine_ls_goodness_of_fit_ref    1.212
_refine_ls_restrained_S_all       1.212
_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
Ta Ta 1.000000 1.000000 1.000000 0.00643(7) Uani 1 6 d S T P . .
Al Al 0.74508(8) 1.000000 0.500000 0.00696(9) Uani 0.5 2 d S T P . .
Ga Ga 0.74508(8) 1.000000 0.500000 0.00696(9) Uani 0.5 2 d S T P . .
Ca Ca 0.42426(11) 1.000000 0.000000 0.01125(13) Uani 1 2 d S T P . .
Si Si 0.333333 0.666667 0.4534(2) 0.00642(14) Uani 1 3 d S T P . .
O1 O 0.333333 0.666667 0.7756(6) 0.0116(4) Uani 1 3 d S T P . .
O2 O 0.5261(3) 0.8438(4) 0.3162(5) 0.0114(3) Uani 1 1 d . . . . .
O3 O 0.7744(3) 0.8632(3) 0.7623(4) 0.0100(3) 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
Ta O3 1.979(2) . ?
Ta O3 1.979(2) 6_767 ?
Ta O3 1.979(2) 5_677 ?
Ta O3 1.979(2) 2_765 ?
Ta O3 1.979(2) 4_557 ?
Ta O3 1.979(2) 3_675 ?
Ta Ca 3.4280(9) 3_566 ?
Ta Ca 3.4280(9) 1_656 ?
Ta Ca 3.4280(9) 2_776 ?
Ga O3 1.797(2) 5_676 ?
Ga O3 1.797(2) . ?
Ga O2 1.822(2) . ?
Ga O2 1.822(2) 5_676 ?
Ga Ca 3.5859(8) . ?
Ga Ca 3.5859(8) 1_556 ?
Ca O3 2.373(2) 2_664 ?
Ca O3 2.373(2) 6_666 ?
Ca O2 2.400(3) . ?
Ca O2 2.400(3) 5_675 ?
Ca O1 2.6555(12) 4_566 ?
Ca O1 2.6555(12) 1_554 ?
Ca O2 2.859(3) 2_665 ?
Ca O2 2.859(3) 6_665 ?
Ca Si 3.2958(8) . ?
Ca Si 3.2958(8) 4_565 ?
Si O1 1.597(3) . ?
Si O2 1.645(2) 2_665 ?
Si O2 1.645(2) . ?
Si O2 1.645(2) 3_565 ?
 
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
O3 Ta O3 168.75(12) . 6_767 ?
O3 Ta O3 100.17(13) . 5_677 ?
O3 Ta O3 88.20(9) 6_767 5_677 ?
O3 Ta O3 88.20(9) . 2_765 ?
O3 Ta O3 84.59(12) 6_767 2_765 ?
O3 Ta O3 168.75(12) 5_677 2_765 ?
O3 Ta O3 84.59(12) . 4_557 ?
O3 Ta O3 88.20(9) 6_767 4_557 ?
O3 Ta O3 88.20(9) 5_677 4_557 ?
O3 Ta O3 100.17(13) 2_765 4_557 ?
O3 Ta O3 88.20(9) . 3_675 ?
O3 Ta O3 100.17(13) 6_767 3_675 ?
O3 Ta O3 84.59(12) 5_677 3_675 ?
O3 Ta O3 88.20(9) 2_765 3_675 ?
O3 Ta O3 168.75(12) 4_557 3_675 ?
O3 Ta Ca 42.29(6) . 3_566 ?
O3 Ta Ca 129.92(6) 6_767 3_566 ?
O3 Ta Ca 95.63(6) 5_677 3_566 ?
O3 Ta Ca 95.63(6) 2_765 3_566 ?
O3 Ta Ca 42.29(6) 4_557 3_566 ?
O3 Ta Ca 129.92(6) 3_675 3_566 ?
O3 Ta Ca 129.92(6) . 1_656 ?
O3 Ta Ca 42.29(6) 6_767 1_656 ?
O3 Ta Ca 129.92(6) 5_677 1_656 ?
O3 Ta Ca 42.29(6) 2_765 1_656 ?
O3 Ta Ca 95.63(6) 4_557 1_656 ?
O3 Ta Ca 95.63(6) 3_675 1_656 ?
Ca Ta Ca 120.0 3_566 1_656 ?
O3 Ta Ca 95.63(6) . 2_776 ?
O3 Ta Ca 95.63(6) 6_767 2_776 ?
O3 Ta Ca 42.29(6) 5_677 2_776 ?
O3 Ta Ca 129.92(6) 2_765 2_776 ?
O3 Ta Ca 129.92(6) 4_557 2_776 ?
O3 Ta Ca 42.29(6) 3_675 2_776 ?
Ca Ta Ca 120.000(1) 3_566 2_776 ?
Ca Ta Ca 120.0 1_656 2_776 ?
O3 Ga O3 127.85(14) 5_676 . ?
O3 Ga O2 103.45(10) 5_676 . ?
O3 Ga O2 108.46(10) . . ?
O3 Ga O2 108.46(10) 5_676 5_676 ?
O3 Ga O2 103.45(10) . 5_676 ?
O2 Ga O2 102.66(17) . 5_676 ?
O3 Ga Ca 79.52(7) 5_676 . ?
O3 Ga Ca 144.83(7) . . ?
O2 Ga Ca 37.15(8) . . ?
O2 Ga Ca 83.90(8) 5_676 . ?
O3 Ga Ca 144.83(7) 5_676 1_556 ?
O3 Ga Ca 79.52(7) . 1_556 ?
O2 Ga Ca 83.90(8) . 1_556 ?
O2 Ga Ca 37.15(8) 5_676 1_556 ?
Ca Ga Ca 87.41(3) . 1_556 ?
O3 Ca O3 68.28(10) 2_664 6_666 ?
O3 Ca O2 134.91(8) 2_664 . ?
O3 Ca O2 107.24(8) 6_666 . ?
O3 Ca O2 107.24(8) 2_664 5_675 ?
O3 Ca O2 134.91(8) 6_666 5_675 ?
O2 Ca O2 105.46(12) . 5_675 ?
O3 Ca O1 128.94(6) 2_664 4_566 ?
O3 Ca O1 75.70(6) 6_666 4_566 ?
O2 Ca O1 89.26(7) . 4_566 ?
O2 Ca O1 74.56(8) 5_675 4_566 ?
O3 Ca O1 75.70(6) 2_664 1_554 ?
O3 Ca O1 128.94(6) 6_666 1_554 ?
O2 Ca O1 74.56(8) . 1_554 ?
O2 Ca O1 89.26(7) 5_675 1_554 ?
O1 Ca O1 153.35(4) 4_566 1_554 ?
O3 Ca O2 79.23(7) 2_664 2_665 ?
O3 Ca O2 71.11(7) 6_666 2_665 ?
O2 Ca O2 58.34(10) . 2_665 ?
O2 Ca O2 153.96(4) 5_675 2_665 ?
O1 Ca O2 121.65(7) 4_566 2_665 ?
O1 Ca O2 67.51(7) 1_554 2_665 ?
O3 Ca O2 71.11(7) 2_664 6_665 ?
O3 Ca O2 79.23(7) 6_666 6_665 ?
O2 Ca O2 153.96(4) . 6_665 ?
O2 Ca O2 58.34(10) 5_675 6_665 ?
O1 Ca O2 67.51(7) 4_566 6_665 ?
O1 Ca O2 121.65(7) 1_554 6_665 ?
O2 Ca O2 144.06(10) 2_665 6_665 ?
O3 Ca Si 107.87(5) 2_664 . ?
O3 Ca Si 90.03(5) 6_666 . ?
O2 Ca Si 28.41(5) . . ?
O2 Ca Si 130.90(6) 5_675 . ?
O1 Ca Si 107.07(5) 4_566 . ?
O1 Ca Si 67.72(6) 1_554 . ?
O2 Ca Si 29.95(5) 2_665 . ?
O2 Ca Si 168.83(5) 6_665 . ?
O3 Ca Si 90.03(5) 2_664 4_565 ?
O3 Ca Si 107.87(5) 6_666 4_565 ?
O2 Ca Si 130.90(6) . 4_565 ?
O2 Ca Si 28.41(5) 5_675 4_565 ?
O1 Ca Si 67.72(6) 4_566 4_565 ?
O1 Ca Si 107.07(5) 1_554 4_565 ?
O2 Ca Si 168.83(5) 2_665 4_565 ?
O2 Ca Si 29.95(5) 6_665 4_565 ?
Si Ca Si 158.60(3) . 4_565 ?
O3 Ca Ta 34.14(5) 2_664 1_454 ?
O3 Ca Ta 34.14(5) 6_666 1_454 ?
O2 Ca Ta 127.27(6) . 1_454 ?
O2 Ca Ta 127.27(6) 5_675 1_454 ?
O1 Ca Ta 103.324(19) 4_566 1_454 ?
O1 Ca Ta 103.325(19) 1_554 1_454 ?
O2 Ca Ta 72.03(5) 2_665 1_454 ?
O2 Ca Ta 72.03(5) 6_665 1_454 ?
Si Ca Ta 100.702(15) . 1_454 ?
Si Ca Ta 100.701(15) 4_565 1_454 ?
O3 Ca Al 104.79(5) 2_664 1_554 ?
O3 Ca Al 160.28(5) 6_666 1_554 ?
O2 Ca Al 90.76(7) . 1_554 ?
O2 Ca Al 27.29(6) 5_675 1_554 ?
O1 Ca Al 97.05(4) 4_566 1_554 ?
O1 Ca Al 62.88(4) 1_554 1_554 ?
O2 Ca Al 126.98(5) 2_665 1_554 ?
O2 Ca Al 81.05(5) 6_665 1_554 ?
Si Ca Al 109.68(2) . 1_554 ?
Si Ca Al 52.756(11) 4_565 1_554 ?
Ta Ca Al 136.295(13) 1_454 1_554 ?
O1 Si O2 114.41(9) . 2_665 ?
O1 Si O2 114.41(9) . . ?
O2 Si O2 104.11(10) 2_665 . ?
O1 Si O2 114.41(9) . 3_565 ?
O2 Si O2 104.11(10) 2_665 3_565 ?
O2 Si O2 104.11(10) . 3_565 ?
O1 Si Ca 132.973(14) . . ?
O2 Si Ca 60.18(10) 2_665 . ?
O2 Si Ca 43.96(9) . . ?
O2 Si Ca 111.84(9) 3_565 . ?
O1 Si Ca 132.972(14) . 2_665 ?
O2 Si Ca 43.96(9) 2_665 2_665 ?
O2 Si Ca 111.84(9) . 2_665 ?
O2 Si Ca 60.18(10) 3_565 2_665 ?
Ca Si Ca 78.64(2) . 2_665 ?
O1 Si Ca 132.972(14) . 3_565 ?
O2 Si Ca 111.84(9) 2_665 3_565 ?
O2 Si Ca 60.18(10) . 3_565 ?
O2 Si Ca 43.96(9) 3_565 3_565 ?
Ca Si Ca 78.64(2) . 3_565 ?
Ca Si Ca 78.64(2) 2_665 3_565 ?
O1 Si Ca 41.678(12) . 1_556 ?
O2 Si Ca 96.47(9) 2_665 1_556 ?
O2 Si Ca 84.86(9) . 1_556 ?
O2 Si Ca 154.53(9) 3_565 1_556 ?
Ca Si Ca 91.295(8) . 1_556 ?
Ca Si Ca 138.797(5) 2_665 1_556 ?
Ca Si Ca 138.797(5) 3_565 1_556 ?
O1 Si Ca 41.678(12) . 2_666 ?
O2 Si Ca 84.86(9) 2_665 2_666 ?
O2 Si Ca 154.53(9) . 2_666 ?
O2 Si Ca 96.47(9) 3_565 2_666 ?
Ca Si Ca 138.798(5) . 2_666 ?
Ca Si Ca 91.295(8) 2_665 2_666 ?
Ca Si Ca 138.797(5) 3_565 2_666 ?
Ca Si Ca 70.319(19) 1_556 2_666 ?
O1 Si Ca 41.678(12) . 3_566 ?
O2 Si Ca 154.53(9) 2_665 3_566 ?
O2 Si Ca 96.47(9) . 3_566 ?
O2 Si Ca 84.86(9) 3_565 3_566 ?
Ca Si Ca 138.797(5) . 3_566 ?
Ca Si Ca 138.797(5) 2_665 3_566 ?
Ca Si Ca 91.295(8) 3_565 3_566 ?
Ca Si Ca 70.319(19) 1_556 3_566 ?
Ca Si Ca 70.319(19) 2_666 3_566 ?
Si O1 Ca 114.75(6) . 1_556 ?
Si O1 Ca 114.75(6) . 2_666 ?
Ca O1 Ca 103.71(6) 1_556 2_666 ?
Si O1 Ca 114.75(6) . 3_566 ?
Ca O1 Ca 103.71(6) 1_556 3_566 ?
Ca O1 Ca 103.71(6) 2_666 3_566 ?
Si O2 Ga 124.40(14) . . ?
Si O2 Ca 107.64(12) . . ?
Ga O2 Ca 115.56(12) . . ?
Si O2 Ca 89.87(11) . 3_565 ?
Ga O2 Ca 110.06(11) . 3_565 ?
Ca O2 Ca 104.80(8) . 3_565 ?
Ga O3 Ta 117.06(10) . . ?
Ga O3 Ca 136.74(11) . 3_566 ?
Ta O3 Ca 103.57(8) . 3_566 ?
 
_refine_diff_density_max    4.046
_refine_diff_density_min   -3.012
_refine_diff_density_rms    0.687



