 
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
 'K3.90 Na0.07 O23 S5 Tl0.03 V3' 
_chemical_formula_weight          841.76

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'
 'K'  'K'   0.2009   0.2494
 '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'
 'V'  'V'   0.3005   0.5294
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Na'  'Na'   0.0362   0.0249
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Tl'  'Tl'  -2.8358   9.6688
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 
_space_group_crystal_system       monoclinic
_space_group_IT_number            14
_space_group_name_H-M_alt         'P 21/n'
_space_group_name_Hall            '-P 2yn'
 
_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+1/2, y+1/2, -z+1/2'
 '-x, -y, -z'
 'x-1/2, -y-1/2, z-1/2'
 
_cell_length_a                    8.7209(5)
_cell_length_b                    16.1777(6)
_cell_length_c                    14.4614(7)
_cell_angle_alpha                 90
_cell_angle_beta                  106.744(5)
_cell_angle_gamma                 90
_cell_volume                      1953.77(17)
_cell_formula_units_Z             4
_cell_measurement_temperature     293(2)
_cell_measurement_reflns_used     1441
_cell_measurement_theta_min       1.936
_cell_measurement_theta_max       24.067
 
_exptl_crystal_description        'prism'
_exptl_crystal_colour             ?
_exptl_crystal_density_meas       ?
_exptl_crystal_density_method     ?
_exptl_crystal_density_diffrn     2.862          
_exptl_crystal_F_000              1642
_exptl_transmission_factor_min    ?
_exptl_transmission_factor_max    ?
_exptl_crystal_size_max           ?
_exptl_crystal_size_mid           ?
_exptl_crystal_size_min           ?
_exptl_absorpt_coefficient_mu     3.155
_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       293(2)
_diffrn_radiation_wavelength      0.71073
_diffrn_radiation_type            MoK\a
_diffrn_source                    ?
_diffrn_measurement_device_type   'Bruker Apex 2 Duo'
_diffrn_measurement_method        ?
_diffrn_detector_area_resol_mean  ?
_diffrn_reflns_number             14176
_diffrn_reflns_av_unetI/netI      0.0651
_diffrn_reflns_av_R_equivalents   0.1021
_diffrn_reflns_limit_h_min        -10
_diffrn_reflns_limit_h_max        9
_diffrn_reflns_limit_k_min        -18
_diffrn_reflns_limit_k_max        18
_diffrn_reflns_limit_l_min        -16
_diffrn_reflns_limit_l_max        16
_diffrn_reflns_theta_min          1.936
_diffrn_reflns_theta_max          24.067
_diffrn_reflns_theta_full         24.067
_diffrn_measured_fraction_theta_max   1.000
_diffrn_measured_fraction_theta_full  1.000
_diffrn_reflns_Laue_measured_fraction_max    1.000
_diffrn_reflns_Laue_measured_fraction_full   1.000
_diffrn_reflns_point_group_measured_fraction_max   1.000
_diffrn_reflns_point_group_measured_fraction_full  1.000
_reflns_number_total              3083
_reflns_number_gt                 1907
_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 perfect inversion 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)+(0.0322P)²+17.8704P] 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          3083
_refine_ls_number_parameters      320
_refine_ls_number_restraints      6
_refine_ls_R_factor_all           0.1010
_refine_ls_R_factor_gt            0.0529
_refine_ls_wR_factor_ref          0.1217
_refine_ls_wR_factor_gt           0.1014
_refine_ls_goodness_of_fit_ref    1.035
_refine_ls_restrained_S_all       1.034
_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
V1 V 0.16741(18) 0.35946(9) 0.08679(11) 0.0097(4) Uani 1 1 d . . . . .
V2 V -0.0061(2) 0.10932(8) 0.25246(12) 0.0098(3) Uani 1 1 d . . . . .
V3 V 0.32309(18) 0.13903(9) -0.08165(11) 0.0098(4) Uani 1 1 d . . . . .
S1 S 0.1019(3) 0.15669(13) 0.05946(16) 0.0103(5) Uani 1 1 d . . . . .
S2 S 0.4581(3) 0.17805(14) -0.26364(17) 0.0203(6) Uani 1 1 d . . . . .
S3 S -0.1185(3) 0.16061(14) 0.44267(15) 0.0099(5) Uani 1 1 d . . . . .
S4 S 0.8404(3) 0.56300(14) 0.40012(16) 0.0103(5) Uani 1 1 d . . . . .
S5 S 0.8409(3) 0.43590(14) 0.89987(16) 0.0095(5) Uani 1 1 d . . . . .
K1 K 0.7423(3) 0.24753(16) 0.98865(19) 0.0268(9) Uani 0.93(2) 1 d . . P . .
Na1 Na 0.7423(3) 0.24753(16) 0.98865(19) 0.0268(9) Uani 0.07(2) 1 d . . P . .
K2 K -0.2535(3) -0.02342(13) 0.37552(17) 0.0279(10) Uani 0.992(2) 1 d . . P . .
Tl1 Tl -0.2535(3) -0.02342(13) 0.37552(17) 0.0279(10) Uani 0.008(2) 1 d . . P . .
K3 K 0.0144(3) 0.30241(12) 0.74146(18) 0.0407(11) Uani 0.983(2) 1 d . . P . .
Tl2 Tl 0.0144(3) 0.30241(12) 0.74146(18) 0.0407(11) Uani 0.017(2) 1 d . . P . .
K4 K 0.2265(3) 0.47358(14) 0.35994(16) 0.0271(10) Uani 0.994(2) 1 d . . P . .
Tl3 Tl 0.2265(3) 0.47358(14) 0.35994(16) 0.0271(10) Uani 0.006(2) 1 d . . P . .
O1 O 0.3507(7) 0.3630(4) 0.8391(4) 0.0174(15) Uani 1 1 d . . . . .
O2 O 0.6260(7) 0.3770(4) 0.6582(4) 0.0175(15) Uani 1 1 d . . . . .
O3 O 0.5377(9) 0.2543(4) 0.7654(5) 0.0297(19) Uani 1 1 d . . . . .
O4 O 0.7703(7) 0.4838(4) 0.4210(4) 0.0157(14) Uani 1 1 d . . . . .
O5 O 0.5614(8) 0.2550(4) 0.5587(4) 0.0173(15) Uani 1 1 d . . . . .
O6 O 0.7194(7) 0.0181(4) 0.5816(4) 0.0158(15) Uani 1 1 d . . . . .
O7 O 0.5033(8) 0.3897(4) 0.0043(4) 0.0217(16) Uani 1 1 d . . . . .
O8 O 0.5537(7) 0.1242(4) 0.6898(4) 0.0166(15) Uani 1 1 d . . . . .
O9 O 0.4312(7) 0.2506(4) 0.9557(4) 0.0168(15) Uani 1 1 d . . . . .
O10 O 0.4756(8) 0.3854(4) 0.4884(5) 0.0212(16) Uani 1 1 d . . . . .
O11 O 0.2231(7) 0.3494(4) 0.9601(4) 0.0128(14) Uani 1 1 d . . . . .
O12 O 0.4479(7) 0.1282(4) 0.8197(4) 0.0159(15) Uani 1 1 d . . . . .
O13 O 0.2940(7) 0.3768(3) 0.6401(4) 0.0110(14) Uani 1 1 d . . . . .
O14 O 0.4867(8) 0.4881(3) 0.7577(5) 0.0232(15) Uani 1 1 d . . . . .
O15 O 0.7015(7) 0.3803(3) 0.8616(4) 0.0135(15) Uani 1 1 d . . . . .
O16 O 0.7614(7) 0.3537(4) 0.5433(4) 0.0138(14) Uani 1 1 d . . . . .
O17 O 0.6593(8) 0.3296(4) 0.3473(4) 0.0212(16) Uani 1 1 d . . . . .
O18 O 0.3329(7) 0.3295(4) 0.1571(4) 0.0214(16) Uani 1 1 d . . . . .
O19 O 0.9287(7) 0.3992(4) 0.9935(4) 0.0144(14) Uani 1 1 d . U . . .
O20 O 0.9354(7) 0.4405(4) 0.8330(4) 0.0166(15) Uani 1 1 d . . . . .
O21 O 0.0643(7) 0.4003(4) 0.5071(4) 0.0189(15) Uani 1 1 d . . . . .
O22 O 0.0686(8) 0.4491(4) 0.6677(5) 0.0187(15) Uani 1 1 d . . . . .
O23 O 0.2971(8) 0.1913(4) 0.6699(5) 0.0335(18) 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
V1 O18 1.583(6) . ?
V1 O8 2.031(6) 4_565 ?
V1 O11 2.033(6) 1_554 ?
V1 O6 2.039(6) 4_565 ?
V1 O5 2.057(6) 4_565 ?
V1 O19 2.224(6) 1_454 ?
V2 O14 1.579(6) 4_565 ?
V2 O13 2.024(6) 4_565 ?
V2 O2 2.035(6) 4_565 ?
V2 O15 2.037(6) 4_565 ?
V2 O1 2.057(6) 4_565 ?
V2 O3 2.237(6) 4_565 ?
V3 O17 1.584(6) 4_565 ?
V3 O16 2.031(6) 4_565 ?
V3 O12 2.036(6) 1_554 ?
V3 O9 2.036(6) 1_554 ?
V3 O4 2.043(6) 4_565 ?
V3 O21 2.218(6) 4_665 ?
S1 O10 1.443(7) 4_565 ?
S1 O5 1.472(6) 4_565 ?
S1 O16 1.485(6) 4_565 ?
S1 O2 1.485(6) 4_565 ?
S1 K1 3.346(3) 1_454 ?
S1 K4 3.372(3) 2_545 ?
S2 O3 1.419(7) 1_554 ?
S2 O23 1.470(7) 1_554 ?
S2 O12 1.474(6) 1_554 ?
S2 O8 1.493(6) 1_554 ?
S2 K2 3.224(3) 3 ?
S2 K4 3.504(3) 4_665 ?
S3 O7 1.428(7) 4_566 ?
S3 O11 1.483(6) 4_565 ?
S3 O1 1.493(6) 4_565 ?
S3 O9 1.496(6) 4_565 ?
S3 K2 3.246(3) . ?
S3 K1 3.368(3) 4_565 ?
S4 O22 1.442(6) 3_666 ?
S4 O21 1.484(6) 3_666 ?
S4 O4 1.487(6) . ?
S4 O13 1.506(6) 3_666 ?
S4 K3 3.468(3) 3_666 ?
S5 O20 1.441(6) . ?
S5 O19 1.475(6) . ?
S5 O6 1.482(6) 2_656 ?
S5 O15 1.485(6) . ?
S5 K1 3.509(3) . ?
K1 O9 2.616(6) . ?
K1 O5 2.674(7) 4_666 ?
K1 O23 2.713(8) 4_666 ?
K1 O15 2.783(6) . ?
K1 O21 2.905(7) 4_666 ?
K1 O13 2.912(6) 4_666 ?
K1 O19 2.933(6) . ?
K1 O10 2.962(7) 4_666 ?
K1 O7 3.155(7) 1_556 ?
K2 O7 2.752(7) 2_545 ?
K2 O23 2.794(7) 3_556 ?
K2 O1 2.848(7) 4_565 ?
K2 O20 2.928(6) 4_465 ?
K2 O8 2.997(7) 3_556 ?
K2 O19 3.026(6) 2_546 ?
K2 O11 3.099(6) 4_565 ?
K2 O14 3.111(7) 4_565 ?
K2 O6 3.130(6) 1_455 ?
K3 O22 2.698(6) . ?
K3 O17 2.717(6) 4_566 ?
K3 O18 2.727(7) 4_566 ?
K3 O20 2.783(7) 1_455 ?
K3 O1 3.029(7) . ?
K3 K4 4.233(3) 3_566 ?
K4 O22 2.785(7) 3_566 ?
K4 O2 2.786(6) 3_666 ?
K4 O10 2.807(7) . ?
K4 O12 2.853(6) 4_565 ?
K4 O8 2.948(7) 4_565 ?
K4 O20 3.072(6) 3_666 ?
K4 O21 3.110(7) . ?
K4 O16 3.113(7) 3_666 ?
 
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
O18 V1 O8 96.6(3) . 4_565 ?
O18 V1 O11 98.3(3) . 1_554 ?
O8 V1 O11 164.9(3) 4_565 1_554 ?
O18 V1 O6 98.6(3) . 4_565 ?
O8 V1 O6 93.5(2) 4_565 4_565 ?
O11 V1 O6 86.0(2) 1_554 4_565 ?
O18 V1 O5 97.3(3) . 4_565 ?
O8 V1 O5 88.6(2) 4_565 4_565 ?
O11 V1 O5 87.7(2) 1_554 4_565 ?
O6 V1 O5 163.6(3) 4_565 4_565 ?
O18 V1 O19 177.0(3) . 1_454 ?
O8 V1 O19 80.7(2) 4_565 1_454 ?
O11 V1 O19 84.3(2) 1_554 1_454 ?
O6 V1 O19 82.9(2) 4_565 1_454 ?
O5 V1 O19 81.4(2) 4_565 1_454 ?
O14 V2 O13 96.4(3) 4_565 4_565 ?
O14 V2 O2 100.3(3) 4_565 4_565 ?
O13 V2 O2 88.4(2) 4_565 4_565 ?
O14 V2 O15 94.8(3) 4_565 4_565 ?
O13 V2 O15 168.7(2) 4_565 4_565 ?
O2 V2 O15 87.8(3) 4_565 4_565 ?
O14 V2 O1 98.5(3) 4_565 4_565 ?
O13 V2 O1 86.1(2) 4_565 4_565 ?
O2 V2 O1 160.9(2) 4_565 4_565 ?
O15 V2 O1 94.0(2) 4_565 4_565 ?
O14 V2 O3 171.0(3) 4_565 4_565 ?
O13 V2 O3 92.6(2) 4_565 4_565 ?
O2 V2 O3 80.4(2) 4_565 4_565 ?
O15 V2 O3 76.2(2) 4_565 4_565 ?
O1 V2 O3 81.6(2) 4_565 4_565 ?
O17 V3 O16 97.9(3) 4_565 4_565 ?
O17 V3 O12 97.9(3) 4_565 1_554 ?
O16 V3 O12 163.8(3) 4_565 1_554 ?
O17 V3 O9 98.6(3) 4_565 1_554 ?
O16 V3 O9 86.2(2) 4_565 1_554 ?
O12 V3 O9 87.8(2) 1_554 1_554 ?
O17 V3 O4 99.1(3) 4_565 4_565 ?
O16 V3 O4 85.4(2) 4_565 4_565 ?
O12 V3 O4 95.7(2) 1_554 4_565 ?
O9 V3 O4 161.3(3) 1_554 4_565 ?
O17 V3 O21 174.3(3) 4_565 4_665 ?
O16 V3 O21 87.2(2) 4_565 4_665 ?
O12 V3 O21 76.8(2) 1_554 4_665 ?
O9 V3 O21 79.1(2) 1_554 4_665 ?
O4 V3 O21 83.8(2) 4_565 4_665 ?
O10 S1 O5 108.7(4) 4_565 4_565 ?
O10 S1 O16 113.1(4) 4_565 4_565 ?
O5 S1 O16 110.0(4) 4_565 4_565 ?
O10 S1 O2 112.3(4) 4_565 4_565 ?
O5 S1 O2 109.3(4) 4_565 4_565 ?
O16 S1 O2 103.3(4) 4_565 4_565 ?
O10 S1 K1 62.2(3) 4_565 1_454 ?
O5 S1 K1 50.9(3) 4_565 1_454 ?
O16 S1 K1 147.1(3) 4_565 1_454 ?
O2 S1 K1 108.4(3) 4_565 1_454 ?
O10 S1 K4 90.2(3) 4_565 2_545 ?
O5 S1 K4 159.7(3) 4_565 2_545 ?
O16 S1 K4 67.2(3) 4_565 2_545 ?
O2 S1 K4 54.5(2) 4_565 2_545 ?
K1 S1 K4 140.82(9) 1_454 2_545 ?
O3 S2 O23 111.1(4) 1_554 1_554 ?
O3 S2 O12 111.9(4) 1_554 1_554 ?
O23 S2 O12 110.0(4) 1_554 1_554 ?
O3 S2 O8 110.6(4) 1_554 1_554 ?
O23 S2 O8 110.0(4) 1_554 1_554 ?
O12 S2 O8 102.9(3) 1_554 1_554 ?
O3 S2 K2 167.4(3) 1_554 3 ?
O23 S2 K2 59.9(3) 1_554 3 ?
O12 S2 K2 80.3(3) 1_554 3 ?
O8 S2 K2 67.8(3) 1_554 3 ?
O3 S2 K4 105.1(3) 1_554 4_665 ?
O23 S2 K4 143.8(3) 1_554 4_665 ?
O12 S2 K4 52.3(2) 1_554 4_665 ?
O8 S2 K4 56.2(2) 1_554 4_665 ?
K2 S2 K4 84.52(7) 3 4_665 ?
O7 S3 O11 113.2(4) 4_566 4_565 ?
O7 S3 O1 111.5(4) 4_566 4_565 ?
O11 S3 O1 103.6(4) 4_565 4_565 ?
O7 S3 O9 109.4(4) 4_566 4_565 ?
O11 S3 O9 109.5(3) 4_565 4_565 ?
O1 S3 O9 109.5(4) 4_565 4_565 ?
O7 S3 K2 78.7(3) 4_566 . ?
O11 S3 K2 71.0(2) 4_565 . ?
O1 S3 K2 61.3(3) 4_565 . ?
O9 S3 K2 170.1(3) 4_565 . ?
O7 S3 K1 69.1(3) 4_566 4_565 ?
O11 S3 K1 151.4(3) 4_565 4_565 ?
O1 S3 K1 101.5(3) 4_565 4_565 ?
O9 S3 K1 48.0(2) 4_565 4_565 ?
K2 S3 K1 134.55(9) . 4_565 ?
O22 S4 O21 113.2(4) 3_666 3_666 ?
O22 S4 O4 111.2(4) 3_666 . ?
O21 S4 O4 108.5(4) 3_666 . ?
O22 S4 O13 110.2(4) 3_666 3_666 ?
O21 S4 O13 105.2(4) 3_666 3_666 ?
O4 S4 O13 108.4(4) . 3_666 ?
O22 S4 K3 46.9(3) 3_666 3_666 ?
O21 S4 K3 94.4(3) 3_666 3_666 ?
O4 S4 K3 154.4(3) . 3_666 ?
O13 S4 K3 75.1(2) 3_666 3_666 ?
O20 S5 O19 113.0(4) . . ?
O20 S5 O6 112.1(4) . 2_656 ?
O19 S5 O6 108.2(4) . 2_656 ?
O20 S5 O15 110.3(4) . . ?
O19 S5 O15 104.5(4) . . ?
O6 S5 O15 108.4(4) 2_656 . ?
O20 S5 K1 122.6(3) . . ?
O19 S5 K1 55.3(2) . . ?
O6 S5 K1 125.1(3) 2_656 . ?
O15 S5 K1 49.5(2) . . ?
O9 K1 O5 168.8(2) . 4_666 ?
O9 K1 O23 93.1(2) . 4_666 ?
O5 K1 O23 76.4(2) 4_666 4_666 ?
O9 K1 O15 86.35(19) . . ?
O5 K1 O15 100.5(2) 4_666 . ?
O23 K1 O15 108.0(2) 4_666 . ?
O9 K1 O21 58.60(19) . 4_666 ?
O5 K1 O21 118.57(19) 4_666 4_666 ?
O23 K1 O21 99.3(2) 4_666 4_666 ?
O15 K1 O21 136.58(19) . 4_666 ?
O9 K1 O13 94.49(19) . 4_666 ?
O5 K1 O13 77.63(18) 4_666 4_666 ?
O23 K1 O13 65.12(19) 4_666 4_666 ?
O15 K1 O13 173.1(2) . 4_666 ?
O21 K1 O13 48.18(17) 4_666 4_666 ?
O9 K1 O19 121.80(19) . . ?
O5 K1 O19 59.61(18) 4_666 . ?
O23 K1 O19 74.3(2) 4_666 . ?
O15 K1 O19 48.27(18) . . ?
O21 K1 O19 173.5(2) 4_666 . ?
O13 K1 O19 126.53(18) 4_666 . ?
O9 K1 O10 133.7(2) . 4_666 ?
O5 K1 O10 49.38(18) 4_666 4_666 ?
O23 K1 O10 109.7(2) 4_666 4_666 ?
O15 K1 O10 121.12(19) . 4_666 ?
O21 K1 O10 77.76(18) 4_666 4_666 ?
O13 K1 O10 62.72(17) 4_666 4_666 ?
O19 K1 O10 103.36(18) . 4_666 ?
O9 K1 O7 47.73(18) . 1_556 ?
O5 K1 O7 128.4(2) 4_666 1_556 ?
O23 K1 O7 66.48(19) 4_666 1_556 ?
O15 K1 O7 61.52(18) . 1_556 ?
O21 K1 O7 102.23(19) 4_666 1_556 ?
O13 K1 O7 114.34(18) 4_666 1_556 ?
O19 K1 O7 76.21(17) . 1_556 ?
O10 K1 O7 176.1(2) 4_666 1_556 ?
O9 K1 S1 153.59(17) . 1_656 ?
O5 K1 S1 25.28(13) 4_666 1_656 ?
O23 K1 S1 88.61(17) 4_666 1_656 ?
O15 K1 S1 118.13(15) . 1_656 ?
O21 K1 S1 95.10(14) 4_666 1_656 ?
O13 K1 S1 62.47(13) 4_666 1_656 ?
O19 K1 S1 84.01(13) . 1_656 ?
O10 K1 S1 25.52(13) 4_666 1_656 ?
O7 K1 S1 151.46(15) 1_556 1_656 ?
O9 K1 S3 25.16(14) . 4_666 ?
O5 K1 S3 153.20(16) 4_666 4_666 ?
O23 K1 S3 85.66(17) 4_666 4_666 ?
O15 K1 S3 66.08(14) . 4_666 ?
O21 K1 S3 83.56(14) 4_666 4_666 ?
O13 K1 S3 112.76(14) 4_666 4_666 ?
O19 K1 S3 96.64(14) . 4_666 ?
O10 K1 S3 157.41(16) 4_666 4_666 ?
O7 K1 S3 25.01(12) 1_556 4_666 ?
S1 K1 S3 173.82(10) 1_656 4_666 ?
O9 K1 S5 105.51(16) . . ?
O5 K1 S5 79.25(15) 4_666 . ?
O23 K1 S5 92.47(17) 4_666 . ?
O15 K1 S5 23.92(13) . . ?
O21 K1 S5 160.47(15) 4_666 . ?
O13 K1 S5 150.94(15) 4_666 . ?
O19 K1 S5 24.43(12) . . ?
O10 K1 S5 112.90(15) 4_666 . ?
O7 K1 S5 68.28(13) 1_556 . ?
S1 K1 S5 100.74(8) 1_656 . ?
S3 K1 S5 81.85(8) 4_666 . ?
O7 K2 O23 71.4(2) 2_545 3_556 ?
O7 K2 O1 110.2(2) 2_545 4_565 ?
O23 K2 O1 150.6(2) 3_556 4_565 ?
O7 K2 O20 152.2(2) 2_545 4_465 ?
O23 K2 O20 109.9(2) 3_556 4_465 ?
O1 K2 O20 82.52(19) 4_565 4_465 ?
O7 K2 O8 112.5(2) 2_545 3_556 ?
O23 K2 O8 49.43(18) 3_556 3_556 ?
O1 K2 O8 137.21(19) 4_565 3_556 ?
O20 K2 O8 60.70(17) 4_465 3_556 ?
O7 K2 O19 81.07(18) 2_545 2_546 ?
O23 K2 O19 71.7(2) 3_556 2_546 ?
O1 K2 O19 137.58(18) 4_565 2_546 ?
O20 K2 O19 73.54(17) 4_465 2_546 ?
O8 K2 O19 54.51(16) 3_556 2_546 ?
O7 K2 O11 110.19(19) 2_545 4_565 ?
O23 K2 O11 162.9(2) 3_556 4_565 ?
O1 K2 O11 46.06(16) 4_565 4_565 ?
O20 K2 O11 60.31(17) 4_465 4_565 ?
O8 K2 O11 117.90(17) 3_556 4_565 ?
O19 K2 O11 91.52(16) 2_546 4_565 ?
O7 K2 O14 84.45(19) 2_545 4_565 ?
O23 K2 O14 96.7(2) 3_556 4_565 ?
O1 K2 O14 55.26(16) 4_565 4_565 ?
O20 K2 O14 122.01(18) 4_465 4_565 ?
O8 K2 O14 126.32(18) 3_556 4_565 ?
O19 K2 O14 163.76(18) 2_546 4_565 ?
O11 K2 O14 100.39(16) 4_565 4_565 ?
O7 K2 O6 76.81(18) 2_545 1_455 ?
O23 K2 O6 113.0(2) 3_556 1_455 ?
O1 K2 O6 95.52(17) 4_565 1_455 ?
O20 K2 O6 77.42(17) 4_465 1_455 ?
O8 K2 O6 96.79(16) 3_556 1_455 ?
O19 K2 O6 45.77(16) 2_546 1_455 ?
O11 K2 O6 52.98(15) 4_565 1_455 ?
O14 K2 O6 136.87(18) 4_565 1_455 ?
O7 K2 S2 98.29(16) 2_545 3 ?
O23 K2 S2 27.10(14) 3_556 3 ?
O1 K2 S2 140.73(15) 4_565 3 ?
O20 K2 S2 84.53(14) 4_465 3 ?
O8 K2 S2 27.47(12) 3_556 3 ?
O19 K2 S2 71.75(13) 2_546 3 ?
O11 K2 S2 144.38(14) 4_565 3 ?
O14 K2 S2 103.32(14) 4_565 3 ?
O6 K2 S2 117.49(13) 1_455 3 ?
O7 K2 S3 97.25(16) 2_545 . ?
O23 K2 S3 167.14(17) 3_556 . ?
O1 K2 S3 27.37(13) 4_565 . ?
O20 K2 S3 82.95(14) 4_465 . ?
O8 K2 S3 143.34(14) 3_556 . ?
O19 K2 S3 113.42(14) 2_546 . ?
O11 K2 S3 26.90(11) 4_565 . ?
O14 K2 S3 75.62(12) 4_565 . ?
O6 K2 S3 68.82(12) 1_455 . ?
S2 K2 S3 164.25(10) 3 . ?
O7 K2 K1 48.99(15) 2_545 2_546 ?
O23 K2 K1 39.87(15) 3_556 2_546 ?
O1 K2 K1 158.20(15) 4_565 2_546 ?
O20 K2 K1 113.53(14) 4_465 2_546 ?
O8 K2 K1 64.28(13) 3_556 2_546 ?
O19 K2 K1 44.52(12) 2_546 2_546 ?
O11 K2 K1 127.94(13) 4_565 2_546 ?
O14 K2 K1 119.47(13) 4_565 2_546 ?
O6 K2 K1 74.97(12) 1_455 2_546 ?
S2 K2 K1 58.87(6) 3 2_546 ?
S3 K2 K1 135.63(9) . 2_546 ?
O22 K3 O17 143.9(2) . 4_566 ?
O22 K3 O18 131.0(2) . 4_566 ?
O17 K3 O18 75.67(18) 4_566 4_566 ?
O22 K3 O20 65.01(16) . 1_455 ?
O17 K3 O20 120.1(2) 4_566 1_455 ?
O18 K3 O20 130.5(2) 4_566 1_455 ?
O22 K3 O1 69.11(18) . . ?
O17 K3 O1 76.18(19) 4_566 . ?
O18 K3 O1 145.2(2) 4_566 . ?
O20 K3 O1 81.80(18) 1_455 . ?
O22 K3 S4 22.98(13) . 3_666 ?
O17 K3 S4 129.51(17) 4_566 3_666 ?
O18 K3 S4 119.42(16) 4_566 3_666 ?
O20 K3 S4 87.66(13) 1_455 3_666 ?
O1 K3 S4 66.60(13) . 3_666 ?
O22 K3 K4 40.21(14) . 3_566 ?
O17 K3 K4 166.30(16) 4_566 3_566 ?
O18 K3 K4 110.42(15) 4_566 3_566 ?
O20 K3 K4 46.47(13) 1_455 3_566 ?
O1 K3 K4 101.63(13) . 3_566 ?
S4 K3 K4 59.16(6) 3_666 3_566 ?
O22 K3 K2 48.07(14) . 4_666 ?
O17 K3 K2 108.56(16) 4_566 4_666 ?
O18 K3 K2 173.04(16) 4_566 4_666 ?
O20 K3 K2 42.66(13) 1_455 4_666 ?
O1 K3 K2 41.53(12) . 4_666 ?
S4 K3 K2 62.50(6) 3_666 4_666 ?
K4 K3 K2 64.23(5) 3_566 4_666 ?
O22 K4 O2 91.7(2) 3_566 3_666 ?
O22 K4 O10 146.1(2) 3_566 . ?
O2 K4 O10 102.3(2) 3_666 . ?
O22 K4 O12 62.14(18) 3_566 4_565 ?
O2 K4 O12 150.6(2) 3_666 4_565 ?
O10 K4 O12 107.0(2) . 4_565 ?
O22 K4 O8 83.82(19) 3_566 4_565 ?
O2 K4 O8 121.75(18) 3_666 4_565 ?
O10 K4 O8 113.0(2) . 4_565 ?
O12 K4 O8 47.12(15) 4_565 4_565 ?
O22 K4 O20 60.17(16) 3_566 3_666 ?
O2 K4 O20 68.04(17) 3_666 3_666 ?
O10 K4 O20 153.67(19) . 3_666 ?
O12 K4 O20 86.24(18) 4_565 3_666 ?
O8 K4 O20 59.61(17) 4_565 3_666 ?
O22 K4 O21 71.69(18) 3_566 . ?
O2 K4 O21 135.12(19) 3_666 . ?
O10 K4 O21 76.78(18) . . ?
O12 K4 O21 52.47(17) 4_565 . ?
O8 K4 O21 98.19(17) 4_565 . ?
O20 K4 O21 127.83(17) 3_666 . ?
O22 K4 O16 64.62(18) 3_566 3_666 ?
O2 K4 O16 46.11(16) 3_666 3_666 ?
O10 K4 O16 103.84(19) . 3_666 ?
O12 K4 O16 121.75(18) 4_565 3_666 ?
O8 K4 O16 143.12(18) 4_565 3_666 ?
O20 K4 O16 87.12(17) 3_666 3_666 ?
O21 K4 O16 89.87(16) . 3_666 ?
O22 K4 S1 87.39(15) 3_566 2 ?
O2 K4 S1 25.73(13) 3_666 2 ?
O10 K4 S1 92.06(16) . 2 ?
O12 K4 S1 147.64(15) 4_565 2 ?
O8 K4 S1 146.03(14) 4_565 2 ?
O20 K4 S1 87.63(13) 3_666 2 ?
O21 K4 S1 110.03(14) . 2 ?
O16 K4 S1 26.08(11) 3_666 2 ?
O22 K4 S2 77.73(15) 3_566 4_566 ?
O2 K4 S2 144.90(15) 3_666 4_566 ?
O10 K4 S2 104.93(16) . 4_566 ?
O12 K4 S2 24.14(12) 4_565 4_566 ?
O8 K4 S2 24.90(12) 4_565 4_566 ?
O20 K4 S2 77.80(13) 3_666 4_566 ?
O21 K4 S2 73.34(13) . 4_566 ?
O16 K4 S2 142.06(14) 3_666 4_566 ?
S1 K4 S2 162.95(9) 2 4_566 ?
O22 K4 K1 111.94(14) 3_566 4_565 ?
O2 K4 K1 149.46(15) 3_666 4_565 ?
O10 K4 K1 47.48(14) . 4_565 ?
O12 K4 K1 59.59(13) 4_565 4_565 ?
O8 K4 K1 81.36(13) 4_565 4_565 ?
O20 K4 K1 140.27(14) 3_666 4_565 ?
O21 K4 K1 45.96(12) . 4_565 ?
O16 K4 K1 126.78(13) 3_666 4_565 ?
S1 K4 K1 132.05(8) 2 4_565 ?
S2 K4 K1 62.71(6) 4_566 4_565 ?
O22 K4 K3 38.72(13) 3_566 3_566 ?
O2 K4 K3 54.63(14) 3_666 3_566 ?
O10 K4 K3 151.22(16) . 3_566 ?
O12 K4 K3 96.61(14) 4_565 3_566 ?
O8 K4 K3 94.99(13) 4_565 3_566 ?
O20 K4 K3 41.06(12) 3_666 3_566 ?
O21 K4 K3 106.57(14) . 3_566 ?
O16 K4 K3 48.44(12) 3_666 3_566 ?
S1 K4 K3 59.61(6) 2 3_566 ?
S2 K4 K3 103.33(7) 4_566 3_566 ?
K1 K4 K3 150.48(8) 4_565 3_566 ?
S3 O1 V2 134.6(4) 4_666 4_666 ?
S3 O1 K2 91.3(3) 4_666 4_666 ?
V2 O1 K2 101.3(2) 4_666 4_666 ?
S3 O1 K3 104.8(3) 4_666 . ?
V2 O1 K3 117.5(3) 4_666 . ?
K2 O1 K3 93.64(19) 4_666 . ?
S1 O2 V2 137.2(4) 4_666 4_666 ?
S1 O2 K4 99.7(3) 4_666 3_666 ?
V2 O2 K4 109.5(3) 4_666 3_666 ?
S2 O3 V2 140.9(5) 1_556 4_666 ?
S4 O4 V3 136.5(4) . 4_666 ?
S1 O5 V1 141.2(4) 4_666 4_666 ?
S1 O5 K1 103.8(3) 4_666 4_565 ?
V1 O5 K1 114.9(3) 4_666 4_565 ?
S5 O6 V1 140.4(4) 2_646 4_666 ?
S5 O6 K2 96.2(3) 2_646 1_655 ?
V1 O6 K2 108.8(2) 4_666 1_655 ?
S3 O7 K2 175.6(4) 4_665 2 ?
S3 O7 K1 85.9(3) 4_665 1_554 ?
K2 O7 K1 89.9(2) 2 1_554 ?
S2 O8 V1 135.1(4) 1_556 4_666 ?
S2 O8 K4 98.9(3) 1_556 4_666 ?
V1 O8 K4 116.2(3) 4_666 4_666 ?
S2 O8 K2 84.8(3) 1_556 3_556 ?
V1 O8 K2 114.0(2) 4_666 3_556 ?
K4 O8 K2 99.28(18) 4_666 3_556 ?
S3 O9 V3 136.3(4) 4_666 1_556 ?
S3 O9 K1 106.8(3) 4_666 . ?
V3 O9 K1 114.1(3) 1_556 . ?
S1 O10 K4 176.2(4) 4_666 . ?
S1 O10 K1 92.3(3) 4_666 4_565 ?
K4 O10 K1 88.21(19) . 4_565 ?
S3 O11 V1 129.6(4) 4_666 1_556 ?
S3 O11 K2 82.1(2) 4_666 4_666 ?
V1 O11 K2 110.1(2) 1_556 4_666 ?
S2 O12 V3 134.2(4) 1_556 1_556 ?
S2 O12 K4 103.5(3) 1_556 4_666 ?
V3 O12 K4 120.2(2) 1_556 4_666 ?
S4 O13 V2 129.3(4) 3_666 4_666 ?
S4 O13 K1 102.8(3) 3_666 4_565 ?
V2 O13 K1 126.2(2) 4_666 4_565 ?
V2 O14 K2 104.6(3) 4_666 4_666 ?
S5 O15 V2 133.5(4) . 4_666 ?
S5 O15 K1 106.6(3) . . ?
V2 O15 K1 119.4(2) 4_666 . ?
S1 O16 V3 130.3(4) 4_666 4_666 ?
S1 O16 K4 86.7(3) 4_666 3_666 ?
V3 O16 K4 111.4(2) 4_666 3_666 ?
V3 O17 K3 143.5(4) 4_666 4_665 ?
V1 O18 K3 146.2(3) . 4_665 ?
S5 O19 V1 145.1(4) . 1_656 ?
S5 O19 K1 100.2(3) . . ?
V1 O19 K1 100.9(2) 1_656 . ?
S5 O19 K2 100.7(3) . 2_556 ?
V1 O19 K2 107.0(2) 1_656 2_556 ?
K1 O19 K2 89.13(17) . 2_556 ?
S5 O20 K3 123.0(3) . 1_655 ?
S5 O20 K2 123.8(3) . 4_766 ?
K3 O20 K2 97.24(19) 1_655 4_766 ?
S5 O20 K4 115.5(3) . 3_666 ?
K3 O20 K4 92.47(18) 1_655 3_666 ?
K2 O20 K4 98.00(18) 4_766 3_666 ?
S4 O21 V3 146.0(4) 3_666 4_566 ?
S4 O21 K1 103.8(3) 3_666 4_565 ?
V3 O21 K1 98.8(2) 4_566 4_565 ?
S4 O21 K4 102.7(3) 3_666 . ?
V3 O21 K4 104.8(2) 4_566 . ?
K1 O21 K4 83.71(17) 4_565 . ?
S4 O22 K3 110.1(3) 3_666 . ?
S4 O22 K4 129.1(4) 3_666 3_566 ?
K3 O22 K4 101.1(2) . 3_566 ?
S2 O23 K1 123.6(4) 1_556 4_565 ?
S2 O23 K2 93.0(3) 1_556 3_556 ?
K1 O23 K2 98.8(2) 4_565 3_556 ?
 
_refine_diff_density_max    2.027
_refine_diff_density_min   -0.936
_refine_diff_density_rms    0.165



