# Electronic Supplementary Material (ESI) for ChemComm.
# This journal is © The Royal Society of Chemistry 2022

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
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data_sr21028_0ma
_database_code_depnum_ccdc_archive 'CCDC 2194286'
_audit_update_record             
;
2022-08-02 deposited with the CCDC.	2022-11-11 downloaded from the CCDC.
;
_audit_creation_date             2022-08-02
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6214)
;
_shelx_SHELXL_version_number     2014/7
loop_
_audit_author_email
carsten.streb@uni-mainz.de
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         
'C16 H48 Ba O8 S8, O32 V12, N O3, C8 H24 N4, 4(C2 H6 O S)'
_chemical_formula_sum            'C32 H96 Ba N5 O47 S12 V12'
_chemical_formula_weight         2436.47
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 '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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 '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'

_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.
;
_space_group_crystal_system      tetragonal
_space_group_IT_number           85
_space_group_name_H-M_alt        'P 4/n'
_space_group_name_Hall           '-P 4a'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y+1/2, x, z'
'-x+1/2, -y+1/2, z'
'y, -x+1/2, z'
'-x, -y, -z'
'y-1/2, -x, -z'
'x-1/2, y-1/2, -z'
'-y, x-1/2, -z'

_cell_length_a                   19.6114(12)
_cell_length_b                   19.6114(12)
_cell_length_c                   11.0115(9)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     4235.1(6)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    9486
_cell_measurement_temperature    150.0
_cell_measurement_theta_max      27.37
_cell_measurement_theta_min      2.36
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    2.101
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6595
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1188 before and 0.0629 after correction.
The Ratio of minimum to maximum transmission is 0.8845.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.911
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             2446
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.16
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0555
_diffrn_reflns_av_unetI/netI     0.0099
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            368824
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.542
_diffrn_reflns_theta_min         1.849
_diffrn_ambient_temperature      150.0
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4793
_reflns_number_total             4893
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_refine_diff_density_max         1.207
_refine_diff_density_min         -0.471
_refine_diff_density_rms         0.098
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.127
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     298
_refine_ls_number_reflns         4893
_refine_ls_number_restraints     42
_refine_ls_R_factor_all          0.0262
_refine_ls_R_factor_gt           0.0249
_refine_ls_restrained_S_all      1.128
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0358P)²+5.9095P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0693
_refine_ls_wR_factor_ref         0.0710
_refine_special_details          
;
 Refined as a 2-component twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.5000(8)
 0.5000(8)
2. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 S2-O1 \\sim S2A-O1A
 with sigma of 0.02
 S2-C1 \\sim S2A-C1A
 with sigma of 0.02
 S2-C3 \\sim S2A-C3A
 with sigma of 0.02
 O1-C3 \\sim O1A-C3A
 with sigma of 0.04
 O1-C1 \\sim O1A-C1A
 with sigma of 0.04
 C1-C3 \\sim C1A-C3A
 with sigma of 0.04
4. Rigid body (RIGU) restrains
 S2, O1, C1, C3
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 S2A, O1A, C1A, C3A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(S2A)=Sof(O1A)=Sof(C1A)=Sof(H1AA)=Sof(H1AB)=Sof(H1AC)=Sof(C3A)=Sof(H3AA)=
 Sof(H3AB)=Sof(H3AC)=1-FVAR(1)
 Sof(S2)=Sof(O1)=Sof(C1)=Sof(H1A)=Sof(H1B)=Sof(H1C)=Sof(C3)=Sof(H3A)=Sof(H3B)=
 Sof(H3C)=FVAR(1)
 Fixed Sof: O5(0.5)
6.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), N5(H5D,H5E), C8(H8A,H8B)
6.b Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C4(H4A,H4B,H4C), C7(H7A,H7B,H7C), C10(H10A,H10B,H10C),
 C1(H1A,H1B,H1C), C3(H3A,H3B,H3C), C1A(H1AA,H1AB,H1AC), C3A(H3AA,H3AB,H3AC)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
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
Ba1 Ba 0.7500 0.2500 0.5000 0.01604(7) Uani 1 4 d S T P . .
V2 V 0.42221(3) 0.17430(3) 0.03167(5) 0.01849(11) Uani 1 1 d . . . . .
V3 V 0.42841(3) 0.31880(3) 0.01844(5) 0.01853(11) Uani 1 1 d . . . . .
V5 V 0.36276(3) 0.29821(2) 0.26860(4) 0.01600(10) Uani 1 1 d . . . . .
O2 O 0.41394(9) 0.24865(12) 0.14068(16) 0.0182(3) Uani 1 1 d . . . . .
O7 O 0.37389(11) 0.36442(11) 0.14248(16) 0.0197(4) Uani 1 1 d . . . . .
O8 O 0.38267(13) 0.37827(13) -0.07620(18) 0.0298(5) Uani 1 1 d . . . . .
O11 O 0.43554(12) 0.24376(13) -0.07693(18) 0.0270(4) Uani 1 1 d . . . . .
O13 O 0.50391(13) 0.34763(13) 0.0344(2) 0.0273(5) Uani 1 1 d . . . . .
O14 O 0.49559(12) 0.14185(12) 0.0540(2) 0.0259(5) Uani 1 1 d . . . . .
S5 S 0.72307(5) 0.43500(5) 0.59571(8) 0.02978(18) Uani 1 1 d . . . . .
N1 N 0.7500 0.7500 0.9911(4) 0.0184(8) Uani 1 4 d S T P . .
O4 O 0.7500 0.7500 0.8798(4) 0.0253(8) Uani 1 4 d S T P . .
O12 O 0.72048(14) 0.32788(15) 0.2953(2) 0.0392(6) Uani 1 1 d . . . . .
O16 O 0.68659(14) 0.36872(12) 0.5684(2) 0.0327(6) Uani 1 1 d . . . . .
O3 O 0.42063(11) 0.31784(11) 0.3643(2) 0.0222(4) Uani 1 1 d . . . . .
O6 O 0.28993(11) 0.33759(11) 0.32163(18) 0.0187(4) Uani 1 1 d . . . . .
S1 S 0.77246(5) 0.35417(5) 0.20794(8) 0.03044(19) Uani 1 1 d . . . . .
C5 C 0.7491(3) 0.42864(18) 0.7495(3) 0.0383(8) Uani 1 1 d . . . . .
H5A H 0.7094 0.4184 0.8005 0.057 Uiso 1 1 calc R U . . .
H5B H 0.7693 0.4719 0.7754 0.057 Uiso 1 1 calc R U . . .
H5C H 0.7828 0.3921 0.7577 0.057 Uiso 1 1 calc R U . . .
C4 C 0.6583(2) 0.49657(19) 0.6162(4) 0.0359(8) Uani 1 1 d . . . . .
H4A H 0.6360 0.5057 0.5383 0.054 Uiso 1 1 calc R U . . .
H4B H 0.6784 0.5388 0.6475 0.054 Uiso 1 1 calc R U . . .
H4C H 0.6246 0.4794 0.6743 0.054 Uiso 1 1 calc R U . . .
C7 C 0.7960(3) 0.4362(2) 0.2632(4) 0.0475(10) Uani 1 1 d . . . . .
H7A H 0.8227 0.4601 0.2012 0.071 Uiso 1 1 calc R U . . .
H7B H 0.8234 0.4311 0.3371 0.071 Uiso 1 1 calc R U . . .
H7C H 0.7548 0.4625 0.2816 0.071 Uiso 1 1 calc R U . . .
C10 C 0.7271(2) 0.3811(2) 0.0769(4) 0.0430(10) Uani 1 1 d . . . . .
H10A H 0.7073 0.3414 0.0362 0.064 Uiso 1 1 calc R U . . .
H10B H 0.7583 0.4044 0.0213 0.064 Uiso 1 1 calc R U . . .
H10C H 0.6906 0.4125 0.1010 0.064 Uiso 1 1 calc R U . . .
O5 O 0.7187(7) 0.7062(5) 1.0487(4) 0.082(3) Uani 0.5 1 d . . P . .
C2 C 0.2609(2) 0.3634(2) 0.6114(3) 0.0427(9) Uani 1 1 d . . . . .
H2A H 0.2599 0.3281 0.5472 0.051 Uiso 1 1 calc R U . . .
H2B H 0.2766 0.4065 0.5741 0.051 Uiso 1 1 calc R U . . .
N5 N 0.3084(2) 0.3432(2) 0.7044(3) 0.0507(10) Uani 1 1 d . . . . .
H5D H 0.2868 0.3144 0.7564 0.061 Uiso 1 1 calc R U . . .
H5E H 0.3206 0.3809 0.7474 0.061 Uiso 1 1 calc R U . . .
C8 C 0.1914(2) 0.3730(2) 0.6594(4) 0.0424(10) Uani 1 1 d . . . . .
H8A H 0.1629 0.3934 0.5948 0.051 Uiso 1 1 calc R U . . .
H8B H 0.1935 0.4060 0.7273 0.051 Uiso 1 1 calc R U . . .
S2 S 0.58944(6) 0.47280(8) 0.24982(13) 0.0353(5) Uani 0.751(6) 1 d D U P A 1
O1 O 0.6273(2) 0.5268(3) 0.3157(5) 0.0399(11) Uani 0.751(6) 1 d D U P A 1
C1 C 0.5134(7) 0.5095(7) 0.1938(10) 0.051(3) Uani 0.751(6) 1 d D U P A 1
H1A H 0.5236 0.5365 0.1211 0.076 Uiso 0.751(6) 1 calc R U P A 1
H1B H 0.4934 0.5390 0.2561 0.076 Uiso 0.751(6) 1 calc R U P A 1
H1C H 0.4810 0.4733 0.1730 0.076 Uiso 0.751(6) 1 calc R U P A 1
C3 C 0.5511(5) 0.4223(4) 0.3674(8) 0.050(2) Uani 0.751(6) 1 d D U P A 1
H3A H 0.5231 0.4516 0.4194 0.075 Uiso 0.751(6) 1 calc R U P A 1
H3B H 0.5870 0.4008 0.4162 0.075 Uiso 0.751(6) 1 calc R U P A 1
H3C H 0.5225 0.3869 0.3307 0.075 Uiso 0.751(6) 1 calc R U P A 1
S2A S 0.5618(4) 0.5058(4) 0.3016(8) 0.079(3) Uani 0.249(6) 1 d D U P A 2
O1A O 0.6305(13) 0.530(2) 0.288(4) 0.148(13) Uani 0.249(6) 1 d D U P A 2
C1A C 0.5641(16) 0.4174(11) 0.328(3) 0.065(8) Uani 0.249(6) 1 d D U P A 2
H1AA H 0.5472 0.4078 0.4102 0.098 Uiso 0.249(6) 1 calc R U P A 2
H1AB H 0.6111 0.4010 0.3206 0.098 Uiso 0.249(6) 1 calc R U P A 2
H1AC H 0.5352 0.3941 0.2685 0.098 Uiso 0.249(6) 1 calc R U P A 2
C3A C 0.514(2) 0.503(2) 0.166(3) 0.059(8) Uani 0.249(6) 1 d D U P A 2
H3AA H 0.5394 0.4772 0.1046 0.089 Uiso 0.249(6) 1 calc R U P A 2
H3AB H 0.5062 0.5494 0.1368 0.089 Uiso 0.249(6) 1 calc R U P A 2
H3AC H 0.4703 0.4806 0.1815 0.089 Uiso 0.249(6) 1 calc R U P A 2


_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 O12 2.783(3) 6_666 ?
Ba1 O12 2.783(2) . ?
Ba1 O12 2.783(2) 3_655 ?
Ba1 O12 2.783(2) 8_656 ?
Ba1 O16 2.745(2) . ?
Ba1 O16 2.745(2) 3_655 ?
Ba1 O16 2.745(2) 8_656 ?
Ba1 O16 2.745(2) 6_666 ?
V2 V3 2.8621(7) 4 ?
V2 O2 1.896(2) . ?
V2 O7 1.915(2) 4 ?
V2 O8 1.844(3) 4 ?
V2 O11 1.831(2) . ?
V2 O14 1.593(2) . ?
V3 V2 2.8621(7) 2 ?
V3 O2 1.945(2) . ?
V3 O7 1.952(2) . ?
V3 O8 1.803(3) . ?
V3 O11 1.813(2) . ?
V3 O13 1.595(3) . ?
V5 O2 1.984(2) . ?
V5 O7 1.914(2) . ?
V5 O3 1.596(2) . ?
V5 O6 1.890(2) 4 ?
V5 O6 1.726(2) . ?
O7 V2 1.915(2) 2 ?
O8 V2 1.844(3) 2 ?
S5 O16 1.514(3) . ?
S5 C5 1.773(4) . ?
S5 C4 1.767(4) . ?
N1 O4 1.226(6) . ?
N1 O5 1.231(6) 3_665 ?
N1 O5 1.231(6) . ?
N1 O5 1.231(6) 2_655 ?
N1 O5 1.231(6) 4_565 ?
O12 S1 1.494(3) . ?
O6 V5 1.890(2) 2 ?
S1 C7 1.780(5) . ?
S1 C10 1.776(4) . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
O5 O5 1.493(8) 2_655 ?
O5 O5 1.493(8) 4_565 ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C2 N5 1.441(5) . ?
C2 C8 1.473(6) . ?
N5 H5D 0.9100 . ?
N5 H5E 0.9100 . ?
N5 C8 1.520(6) 4 ?
C8 N5 1.520(6) 2 ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
S2 O1 1.483(5) . ?
S2 C1 1.767(12) . ?
S2 C3 1.794(7) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
S2A O1A 1.439(18) . ?
S2A C1A 1.76(2) . ?
S2A C3A 1.761(18) . ?
C1A H1AA 0.9800 . ?
C1A H1AB 0.9800 . ?
C1A H1AC 0.9800 . ?
C3A H3AA 0.9800 . ?
C3A H3AB 0.9800 . ?
C3A H3AC 0.9800 . ?

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
O12 Ba1 O12 130.97(8) 6_666 3_655 ?
O12 Ba1 O12 130.97(8) 6_666 . ?
O12 Ba1 O12 71.87(13) 3_655 . ?
O12 Ba1 O12 130.97(8) 3_655 8_656 ?
O12 Ba1 O12 71.87(13) 6_666 8_656 ?
O12 Ba1 O12 130.97(8) 8_656 . ?
O16 Ba1 O12 81.36(8) . 6_666 ?
O16 Ba1 O12 81.36(8) 8_656 . ?
O16 Ba1 O12 72.87(8) . 8_656 ?
O16 Ba1 O12 70.29(9) 6_666 6_666 ?
O16 Ba1 O12 81.36(8) 6_666 3_655 ?
O16 Ba1 O12 141.44(9) 8_656 6_666 ?
O16 Ba1 O12 141.44(9) 3_655 . ?
O16 Ba1 O12 72.88(8) 3_655 6_666 ?
O16 Ba1 O12 70.29(9) . . ?
O16 Ba1 O12 72.88(8) 8_656 3_655 ?
O16 Ba1 O12 70.29(9) 8_656 8_656 ?
O16 Ba1 O12 141.44(9) . 3_655 ?
O16 Ba1 O12 70.29(9) 3_655 3_655 ?
O16 Ba1 O12 141.44(9) 6_666 8_656 ?
O16 Ba1 O12 72.88(8) 6_666 . ?
O16 Ba1 O12 81.36(8) 3_655 8_656 ?
O16 Ba1 O16 94.32(3) 6_666 3_655 ?
O16 Ba1 O16 94.32(3) 8_656 3_655 ?
O16 Ba1 O16 94.32(3) . 6_666 ?
O16 Ba1 O16 94.32(3) . 8_656 ?
O16 Ba1 O16 148.13(11) . 3_655 ?
O16 Ba1 O16 148.13(11) 8_656 6_666 ?
O2 V2 V3 120.86(7) . 4 ?
O2 V2 O7 85.73(9) . 4 ?
O7 V2 V3 42.75(6) 4 4 ?
O8 V2 V3 37.80(7) 4 4 ?
O8 V2 O2 146.50(10) 4 . ?
O8 V2 O7 80.50(10) 4 4 ?
O11 V2 V3 126.26(8) . 4 ?
O11 V2 O2 81.58(10) . . ?
O11 V2 O7 150.20(10) . 4 ?
O11 V2 O8 95.55(11) . 4 ?
O14 V2 V3 111.52(9) . 4 ?
O14 V2 O2 106.66(11) . . ?
O14 V2 O7 103.83(11) . 4 ?
O14 V2 O8 106.24(12) . 4 ?
O14 V2 O11 105.61(12) . . ?
O2 V3 V2 111.30(6) . 2 ?
O2 V3 O7 76.12(9) . . ?
O7 V3 V2 41.76(6) . 2 ?
O8 V3 V2 38.82(7) . 2 ?
O8 V3 O2 141.70(10) . . ?
O8 V3 O7 80.53(10) . . ?
O8 V3 O11 103.22(11) . . ?
O11 V3 V2 131.21(8) . 2 ?
O11 V3 O2 80.68(9) . . ?
O11 V3 O7 145.05(10) . . ?
O13 V3 V2 113.36(10) . 2 ?
O13 V3 O2 108.05(11) . . ?
O13 V3 O7 105.60(11) . . ?
O13 V3 O8 107.23(13) . . ?
O13 V3 O11 106.26(12) . . ?
O7 V5 O2 76.08(9) . . ?
O3 V5 O2 103.13(10) . . ?
O3 V5 O7 103.55(10) . . ?
O3 V5 O6 101.68(11) . 4 ?
O3 V5 O6 104.90(11) . . ?
O6 V5 O2 84.46(9) 4 . ?
O6 V5 O2 151.44(9) . . ?
O6 V5 O7 92.08(10) . . ?
O6 V5 O7 150.99(9) 4 . ?
O6 V5 O6 95.09(14) . 4 ?
V2 O2 V3 95.35(8) . . ?
V2 O2 V5 150.42(12) . . ?
V3 O2 V5 102.63(11) . . ?
V2 O7 V3 95.49(8) 2 . ?
V5 O7 V2 143.87(12) . 2 ?
V5 O7 V3 105.03(11) . . ?
V3 O8 V2 103.38(10) . 2 ?
V3 O11 V2 102.38(10) . . ?
O16 S5 C5 105.36(17) . . ?
O16 S5 C4 105.81(17) . . ?
C4 S5 C5 97.6(2) . . ?
O4 N1 O5 121.0(3) . . ?
O4 N1 O5 121.0(3) . 4_565 ?
O4 N1 O5 121.0(3) . 3_665 ?
O4 N1 O5 121.0(3) . 2_655 ?
O5 N1 O5 74.6(3) 3_665 4_565 ?
O5 N1 O5 74.6(3) 4_565 . ?
O5 N1 O5 74.6(3) 2_655 . ?
O5 N1 O5 74.6(3) 3_665 2_655 ?
O5 N1 O5 118.0(6) 3_665 . ?
O5 N1 O5 118.0(6) 2_655 4_565 ?
S1 O12 Ba1 124.69(15) . . ?
S5 O16 Ba1 124.66(15) . . ?
V5 O6 V5 140.29(12) . 2 ?
O12 S1 C7 105.6(2) . . ?
O12 S1 C10 106.50(19) . . ?
C10 S1 C7 98.0(2) . . ?
S5 C5 H5A 109.5 . . ?
S5 C5 H5B 109.5 . . ?
S5 C5 H5C 109.5 . . ?
H5A C5 H5B 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
S5 C4 H4A 109.5 . . ?
S5 C4 H4B 109.5 . . ?
S5 C4 H4C 109.5 . . ?
H4A C4 H4B 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
S1 C7 H7A 109.5 . . ?
S1 C7 H7B 109.5 . . ?
S1 C7 H7C 109.5 . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
S1 C10 H10A 109.5 . . ?
S1 C10 H10B 109.5 . . ?
S1 C10 H10C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N1 O5 O5 52.69(14) . 2_655 ?
N1 O5 O5 52.69(14) . 4_565 ?
O5 O5 O5 89.998(6) 2_655 4_565 ?
H2A C2 H2B 107.9 . . ?
N5 C2 H2A 109.2 . . ?
N5 C2 H2B 109.2 . . ?
N5 C2 C8 112.2(3) . . ?
C8 C2 H2A 109.2 . . ?
C8 C2 H2B 109.2 . . ?
C2 N5 H5D 108.4 . . ?
C2 N5 H5E 108.4 . . ?
C2 N5 C8 115.5(3) . 4 ?
H5D N5 H5E 107.5 . . ?
C8 N5 H5D 108.4 4 . ?
C8 N5 H5E 108.4 4 . ?
C2 C8 N5 115.1(4) . 2 ?
C2 C8 H8A 108.5 . . ?
C2 C8 H8B 108.5 . . ?
N5 C8 H8A 108.5 2 . ?
N5 C8 H8B 108.5 2 . ?
H8A C8 H8B 107.5 . . ?
O1 S2 C1 107.7(5) . . ?
O1 S2 C3 104.5(3) . . ?
C1 S2 C3 97.1(5) . . ?
S2 C1 H1A 109.5 . . ?
S2 C1 H1B 109.5 . . ?
S2 C1 H1C 109.5 . . ?
H1A C1 H1B 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
S2 C3 H3A 109.5 . . ?
S2 C3 H3B 109.5 . . ?
S2 C3 H3C 109.5 . . ?
H3A C3 H3B 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
O1A S2A C1A 108.9(19) . . ?
O1A S2A C3A 115(2) . . ?
C1A S2A C3A 97.1(15) . . ?
S2A C1A H1AA 109.5 . . ?
S2A C1A H1AB 109.5 . . ?
S2A C1A H1AC 109.5 . . ?
H1AA C1A H1AB 109.5 . . ?
H1AA C1A H1AC 109.5 . . ?
H1AB C1A H1AC 109.5 . . ?
S2A C3A H3AA 109.5 . . ?
S2A C3A H3AB 109.5 . . ?
S2A C3A H3AC 109.5 . . ?
H3AA C3A H3AB 109.5 . . ?
H3AA C3A H3AC 109.5 . . ?
H3AB C3A H3AC 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Ba1 O12 S1 C7 -90.9(2) . . . . ?
Ba1 O12 S1 C10 165.7(2) . . . . ?
V2 V3 O11 V2 -110.06(10) 2 . . . ?
V3 V2 O2 V3 -127.30(6) 4 . . . ?
V3 V2 O2 V5 0.3(3) 4 . . . ?
V3 V2 O11 V3 122.15(9) 4 . . . ?
O2 V2 O11 V3 -0.16(10) . . . . ?
O2 V3 O8 V2 50.3(2) . . . 2 ?
O2 V3 O11 V2 0.16(10) . . . . ?
O2 V5 O6 V5 -4.7(3) . . . 2 ?
O7 V2 O2 V3 -152.81(9) 4 . . . ?
O7 V2 O2 V5 -25.2(2) 4 . . . ?
O7 V2 O11 V3 65.6(2) 4 . . . ?
O7 V3 O8 V2 -2.56(10) . . . 2 ?
O7 V3 O11 V2 -48.6(2) . . . . ?
O7 V5 O6 V5 59.4(2) . . . 2 ?
O8 V2 O2 V3 -87.20(18) 4 . . . ?
O8 V2 O2 V5 40.4(3) 4 . . . ?
O8 V2 O11 V3 146.20(12) 4 . . . ?
O8 V3 O11 V2 -140.96(12) . . . . ?
O11 V2 O2 V3 0.15(9) . . . . ?
O11 V2 O2 V5 127.7(2) . . . . ?
O11 V3 O8 V2 141.96(11) . . . 2 ?
O13 V3 O8 V2 -106.08(14) . . . 2 ?
O13 V3 O11 V2 106.37(13) . . . . ?
O14 V2 O2 V3 104.01(11) . . . . ?
O14 V2 O2 V5 -128.4(2) . . . . ?
O14 V2 O11 V3 -105.21(14) . . . . ?
O4 N1 O5 O5 -117.2(2) . . . 4_565 ?
O4 N1 O5 O5 117.2(2) . . . 2_655 ?
O3 V5 O6 V5 164.01(19) . . . 2 ?
O6 V5 O6 V5 -92.46(19) 4 . . 2 ?
C5 S5 O16 Ba1 -84.3(2) . . . . ?
C4 S5 O16 Ba1 172.91(18) . . . . ?
O5 N1 O5 O5 -62.8(2) 3_665 . . 2_655 ?
O5 N1 O5 O5 125.5(4) 2_655 . . 4_565 ?
O5 N1 O5 O5 -125.5(4) 4_565 . . 2_655 ?
O5 N1 O5 O5 62.8(2) 3_665 . . 4_565 ?
N5 C2 C8 N5 -66.7(5) . . . 2 ?
C8 C2 N5 C8 159.2(4) . . . 4 ?


_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.5000(8)
2 0.5000(8)

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_sr21075_0ma
_database_code_depnum_ccdc_archive 'CCDC 2194313'
_audit_update_record             
;
2022-08-02 deposited with the CCDC.	2022-11-11 downloaded from the CCDC.
;
_audit_creation_date             2022-08-02
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6214)
;
_shelx_SHELXL_version_number     2014/7
loop_
_audit_author_email
carsten.streb@uni-mainz.de
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         
'C16 H48 La O8 S8, O32 V12, N O3, 4(C2 H6 O S), C8 H24 N4'
_chemical_formula_sum            'C32 H96 La N5 O47 S12 V12'
_chemical_formula_weight         2438.04
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
La La -0.2871 2.4523 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 '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'

_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.
;
_space_group_crystal_system      tetragonal
_space_group_IT_number           85
_space_group_name_H-M_alt        'P 4/n'
_space_group_name_Hall           '-P 4a'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y+1/2, x, z'
'-x+1/2, -y+1/2, z'
'y, -x+1/2, z'
'-x, -y, -z'
'y-1/2, -x, -z'
'x-1/2, y-1/2, -z'
'-y, x-1/2, -z'

_cell_length_a                   19.6892(16)
_cell_length_b                   19.6892(16)
_cell_length_c                   10.9971(13)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     4263.2(8)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    9802
_cell_measurement_temperature    150.0
_cell_measurement_theta_max      27.38
_cell_measurement_theta_min      2.36
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    2.122
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.4756
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1453 before and 0.0866 after correction.
The Ratio of minimum to maximum transmission is 0.6379.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.899
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             2448
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.13
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0942
_diffrn_reflns_av_unetI/netI     0.0255
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            189090
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.592
_diffrn_reflns_theta_min         1.852
_diffrn_ambient_temperature      150.0
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4794
_reflns_number_total             4937
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.3 (Bourhis et al., 2015)'
_refine_diff_density_max         1.281
_refine_diff_density_min         -0.791
_refine_diff_density_rms         0.121
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     298
_refine_ls_number_reflns         4937
_refine_ls_number_restraints     42
_refine_ls_R_factor_all          0.0374
_refine_ls_R_factor_gt           0.0357
_refine_ls_restrained_S_all      1.086
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0468P)²+9.4793P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0915
_refine_ls_wR_factor_ref         0.0926
_refine_special_details          
;
 Refined as a 2-component twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.6457(10)
 0.3543(10)
2. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 S3-O6 \\sim S3A-O6A
 with sigma of 0.02
 S3-C3 \\sim S3A-C3A
 with sigma of 0.02
 S3-C5 \\sim S3A-C5A
 with sigma of 0.02
 O6-C5 \\sim O6A-C5A
 with sigma of 0.04
 O6-C3 \\sim O6A-C3A
 with sigma of 0.04
 C3-C5 \\sim C3A-C5A
 with sigma of 0.04
4. Rigid body (RIGU) restrains
 S3, O6, C3, C5
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 S3A, O6A, C3A, C5A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(S3A)=Sof(O6A)=Sof(C3A)=Sof(H3AA)=Sof(H3AB)=Sof(H3AC)=Sof(C5A)=Sof(H5AA)=
 Sof(H5AB)=Sof(H5AC)=1-FVAR(1)
 Sof(S3)=Sof(O6)=Sof(C3)=Sof(H3A)=Sof(H3B)=Sof(H3C)=Sof(C5)=Sof(H5A)=Sof(H5B)=
 Sof(H5C)=FVAR(1)
 Fixed Sof: O12(0.5)
6.a Secondary CH2 refined with riding coordinates:
 N1(H1D,H1E), C4(H4A,H4B), C2(H2A,H2B)
6.b Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C6(H6A,H6B,H6C), C8(H8A,H8B,H8C), C11(H11A,H11B,H11C),
 C3(H3A,H3B,H3C), C5(H5A,H5B,H5C), C3A(H3AA,H3AB,H3AC), C5A(H5AA,H5AB,H5AC)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   ?
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
La1 La 0.2500 0.7500 0.0000 0.01721(10) Uani 1 4 d S T P . .
V2 V -0.18849(4) 0.56943(3) -0.47406(6) 0.02067(14) Uani 1 1 d . . . . .
V3 V -0.33140(4) 0.58218(3) -0.46143(6) 0.01989(14) Uani 1 1 d . . . . .
V4 V -0.20576(4) 0.63656(4) -0.22321(6) 0.02073(14) Uani 1 1 d . . . . .
O3 O -0.25719(15) 0.58697(14) -0.3525(2) 0.0222(5) Uani 1 1 d . . . . .
O8 O -0.12730(16) 0.61252(16) -0.5684(3) 0.0285(6) Uani 1 1 d . . . . .
O11 O -0.26301(15) 0.56635(15) -0.5706(2) 0.0246(6) Uani 1 1 d . . . . .
O13 O -0.16342(17) 0.49263(16) -0.4581(3) 0.0309(7) Uani 1 1 d . . . . .
O14 O -0.18779(16) 0.57824(15) -0.1283(3) 0.0275(6) Uani 1 1 d . . . . .
O15 O -0.36528(16) 0.50966(15) -0.4395(3) 0.0280(6) Uani 1 1 d . . . . .
S1 S 0.32420(6) 0.59897(6) 0.14997(11) 0.0323(2) Uani 1 1 d . . . . .
S2 S 0.20533(8) 0.88547(6) -0.21984(12) 0.0383(3) Uani 1 1 d . . . . .
O1 O -0.16310(15) 0.70693(15) -0.1696(3) 0.0249(6) Uani 1 1 d . . . . .
O2 O 0.2436(2) 0.82092(14) -0.1908(3) 0.0318(7) Uani 1 1 d . . . . .
N3 N -0.2500 0.7500 -0.4738(5) 0.0190(12) Uani 1 4 d S T P . .
O4 O -0.2500 0.7500 -0.3606(5) 0.0263(11) Uani 1 4 d S T P . .
O9 O 0.2800(2) 0.63139(16) 0.0530(3) 0.0352(8) Uani 1 1 d . . . . .
O5 O -0.37820(14) 0.64063(14) -0.3500(2) 0.0220(6) Uani 1 1 d . . . . .
S3 S 0.01121(15) 0.56895(14) -0.7493(3) 0.0499(10) Uani 0.562(6) 1 d D U P A 1
N1 N -0.1646(2) 0.6930(2) -0.7897(3) 0.0289(8) Uani 1 1 d . . . . .
H1D H -0.1985 0.7154 -0.7503 0.035 Uiso 1 1 calc R U . . .
H1E H -0.1313 0.6842 -0.7345 0.035 Uiso 1 1 calc R U . . .
C4 C -0.1913(2) 0.6282(2) -0.8358(4) 0.0258(8) Uani 1 1 d . . . . .
H4A H -0.1916 0.5943 -0.7693 0.031 Uiso 1 1 calc R U . . .
H4B H -0.1614 0.6111 -0.9012 0.031 Uiso 1 1 calc R U . . .
C2 C -0.2624(2) 0.6368(2) -0.8845(4) 0.0244(8) Uani 1 1 d . . . . .
H2A H -0.2617 0.6679 -0.9552 0.029 Uiso 1 1 calc R U . . .
H2B H -0.2801 0.5924 -0.9121 0.029 Uiso 1 1 calc R U . . .
C1 C 0.2024(5) 0.8876(4) -0.3838(6) 0.073(2) Uani 1 1 d . . . . .
H1A H 0.2470 0.8755 -0.4167 0.109 Uiso 1 1 calc R U . . .
H1B H 0.1901 0.9334 -0.4109 0.109 Uiso 1 1 calc R U . . .
H1C H 0.1684 0.8551 -0.4130 0.109 Uiso 1 1 calc R U . . .
O6 O -0.0254(8) 0.6177(5) -0.8132(10) 0.041(2) Uani 0.562(6) 1 d D U P A 1
C6 C 0.2708(4) 0.5946(3) 0.2789(5) 0.0590(19) Uani 1 1 d . . . . .
H6A H 0.2628 0.6405 0.3102 0.089 Uiso 1 1 calc R U . . .
H6B H 0.2927 0.5670 0.3419 0.089 Uiso 1 1 calc R U . . .
H6C H 0.2274 0.5738 0.2560 0.089 Uiso 1 1 calc R U . . .
C8 C 0.2636(3) 0.9529(3) -0.2012(6) 0.0472(14) Uani 1 1 d . . . . .
H8A H 0.2755 0.9572 -0.1150 0.071 Uiso 1 1 calc R U . . .
H8B H 0.2429 0.9953 -0.2295 0.071 Uiso 1 1 calc R U . . .
H8C H 0.3047 0.9435 -0.2486 0.071 Uiso 1 1 calc R U . . .
C11 C 0.3266(3) 0.5118(2) 0.1120(5) 0.0367(11) Uani 1 1 d . . . . .
H11A H 0.2802 0.4950 0.1003 0.055 Uiso 1 1 calc R U . . .
H11B H 0.3484 0.4864 0.1779 0.055 Uiso 1 1 calc R U . . .
H11C H 0.3526 0.5057 0.0368 0.055 Uiso 1 1 calc R U . . .
O12 O -0.2831(4) 0.7074(4) -0.5316(5) 0.0421(18) Uani 0.5 1 d . . P . .
C3 C 0.0732(8) 0.5203(11) -0.8277(15) 0.070(5) Uani 0.562(6) 1 d D U P A 1
H3A H 0.0507 0.4843 -0.8744 0.105 Uiso 0.562(6) 1 calc R U P A 1
H3B H 0.1045 0.4998 -0.7689 0.105 Uiso 0.562(6) 1 calc R U P A 1
H3C H 0.0986 0.5498 -0.8832 0.105 Uiso 0.562(6) 1 calc R U P A 1
C5 C -0.0439(8) 0.5015(6) -0.7142(16) 0.075(4) Uani 0.562(6) 1 d D U P A 1
H5A H -0.0801 0.5178 -0.6606 0.112 Uiso 0.562(6) 1 calc R U P A 1
H5B H -0.0184 0.4654 -0.6731 0.112 Uiso 0.562(6) 1 calc R U P A 1
H5C H -0.0638 0.4836 -0.7893 0.112 Uiso 0.562(6) 1 calc R U P A 1
S3A S -0.01759(15) 0.54023(17) -0.8130(3) 0.0428(11) Uani 0.438(6) 1 d D U P A
2
O6A O -0.0216(13) 0.6067(8) -0.8535(16) 0.069(6) Uani 0.438(6) 1 d D U P A 2
C3A C -0.0011(9) 0.5198(8) -0.6583(12) 0.058(4) Uani 0.438(6) 1 d D U P A 2
H3AA H 0.0392 0.5446 -0.6306 0.087 Uiso 0.438(6) 1 calc R U P A 2
H3AB H 0.0069 0.4709 -0.6507 0.087 Uiso 0.438(6) 1 calc R U P A 2
H3AC H -0.0402 0.5327 -0.6084 0.087 Uiso 0.438(6) 1 calc R U P A 2
C5A C 0.0611(9) 0.5179(14) -0.8758(18) 0.065(5) Uani 0.438(6) 1 d D U P A 2
H5AA H 0.0648 0.5369 -0.9579 0.097 Uiso 0.438(6) 1 calc R U P A 2
H5AB H 0.0648 0.4683 -0.8798 0.097 Uiso 0.438(6) 1 calc R U P A 2
H5AC H 0.0977 0.5360 -0.8248 0.097 Uiso 0.438(6) 1 calc R U P A 2


_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
La1 O2 2.524(3) . ?
La1 O2 2.524(3) 6_565 ?
La1 O2 2.524(3) 8_665 ?
La1 O2 2.524(3) 3_565 ?
La1 O9 2.478(3) 6_565 ?
La1 O9 2.479(3) . ?
La1 O9 2.478(3) 8_665 ?
La1 O9 2.478(3) 3_565 ?
V2 V3 2.8283(10) . ?
V2 V3 2.8658(10) 2_565 ?
V2 V4 3.0778(10) . ?
V2 O3 1.932(3) . ?
V2 O8 1.802(3) . ?
V2 O11 1.812(3) . ?
V2 O13 1.600(3) . ?
V2 O5 1.953(3) 2_565 ?
V3 V2 2.8658(10) 4_455 ?
V3 O3 1.891(3) . ?
V3 O8 1.842(3) 4_455 ?
V3 O11 1.831(3) . ?
V3 O15 1.594(3) . ?
V3 O5 1.917(3) . ?
V4 O3 2.000(3) . ?
V4 O14 1.592(3) . ?
V4 O1 1.891(3) 4_455 ?
V4 O1 1.724(3) . ?
V4 O5 1.916(3) 2_565 ?
O8 V3 1.842(3) 2_565 ?
S1 O9 1.517(3) . ?
S1 C6 1.766(6) . ?
S1 C11 1.767(5) . ?
S2 O2 1.512(3) . ?
S2 C1 1.805(6) . ?
S2 C8 1.766(6) . ?
O1 V4 1.891(3) 2_565 ?
N3 O4 1.245(8) . ?
N3 O12 1.239(7) 4_455 ?
N3 O12 1.239(7) . ?
N3 O12 1.239(7) 3_465 ?
N3 O12 1.239(7) 2_565 ?
O5 V2 1.952(3) 4_455 ?
O5 V4 1.916(3) 4_455 ?
S3 O6 1.391(9) . ?
S3 C3 1.775(13) . ?
S3 C5 1.758(13) . ?
N1 H1D 0.9100 . ?
N1 H1E 0.9100 . ?
N1 C4 1.470(5) . ?
N1 C2 1.468(5) 2_565 ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C4 C2 1.508(6) . ?
C2 N1 1.468(5) 4_455 ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
O12 O12 1.503(9) 4_455 ?
O12 O12 1.503(9) 2_565 ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
S3A O6A 1.385(13) . ?
S3A C3A 1.778(13) . ?
S3A C5A 1.752(15) . ?
C3A H3AA 0.9800 . ?
C3A H3AB 0.9800 . ?
C3A H3AC 0.9800 . ?
C5A H5AA 0.9800 . ?
C5A H5AB 0.9800 . ?
C5A H5AC 0.9800 . ?

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
O2 La1 O2 133.74(9) . 6_565 ?
O2 La1 O2 67.50(13) . 3_565 ?
O2 La1 O2 133.74(9) 6_565 3_565 ?
O2 La1 O2 133.74(9) . 8_665 ?
O2 La1 O2 133.74(9) 3_565 8_665 ?
O2 La1 O2 67.50(14) 6_565 8_665 ?
O9 La1 O2 70.27(10) 6_565 8_665 ?
O9 La1 O2 83.65(12) 6_565 . ?
O9 La1 O2 136.79(11) 6_565 6_565 ?
O9 La1 O2 70.27(10) . 3_565 ?
O9 La1 O2 136.79(11) 8_665 8_665 ?
O9 La1 O2 83.65(12) 3_565 6_565 ?
O9 La1 O2 73.70(12) 3_565 8_665 ?
O9 La1 O2 83.65(12) 8_665 3_565 ?
O9 La1 O2 73.70(12) . 6_565 ?
O9 La1 O2 136.79(11) . . ?
O9 La1 O2 136.79(11) 3_565 3_565 ?
O9 La1 O2 73.70(12) 8_665 . ?
O9 La1 O2 70.27(10) 3_565 . ?
O9 La1 O2 73.70(12) 6_565 3_565 ?
O9 La1 O2 70.27(10) 8_665 6_565 ?
O9 La1 O2 83.65(12) . 8_665 ?
O9 La1 O9 152.78(16) 3_565 . ?
O9 La1 O9 93.17(4) 8_665 . ?
O9 La1 O9 93.17(4) 6_565 . ?
O9 La1 O9 93.17(4) 6_565 3_565 ?
O9 La1 O9 93.17(4) 8_665 3_565 ?
O9 La1 O9 152.78(16) 6_565 8_665 ?
V3 V2 V3 131.59(4) . 2_565 ?
V3 V2 V4 75.21(3) 2_565 . ?
V3 V2 V4 78.93(3) . . ?
O3 V2 V3 41.74(9) . . ?
O3 V2 V3 110.85(9) . 2_565 ?
O3 V2 V4 39.30(8) . . ?
O3 V2 O5 76.13(12) . 2_565 ?
O8 V2 V3 130.67(11) . . ?
O8 V2 V3 38.64(10) . 2_565 ?
O8 V2 V4 112.81(10) . . ?
O8 V2 O3 141.44(13) . . ?
O8 V2 O11 102.70(14) . . ?
O8 V2 O5 80.27(12) . 2_565 ?
O11 V2 V3 39.31(9) . . ?
O11 V2 V3 129.98(10) . 2_565 ?
O11 V2 V4 116.75(9) . . ?
O11 V2 O3 81.05(12) . . ?
O11 V2 O5 144.87(12) . 2_565 ?
O13 V2 V3 114.41(13) . 2_565 ?
O13 V2 V3 112.66(13) . . ?
O13 V2 V4 109.98(13) . . ?
O13 V2 O3 108.00(15) . . ?
O13 V2 O8 107.55(17) . . ?
O13 V2 O11 106.39(16) . . ?
O13 V2 O5 105.89(15) . 2_565 ?
O5 V2 V3 41.74(8) 2_565 2_565 ?
O5 V2 V3 113.51(9) 2_565 . ?
O5 V2 V4 36.89(8) 2_565 . ?
V2 V3 V2 137.75(4) . 4_455 ?
O3 V3 V2 42.86(9) . . ?
O3 V3 V2 121.37(9) . 4_455 ?
O3 V3 O5 86.38(12) . . ?
O8 V3 V2 37.65(10) 4_455 4_455 ?
O8 V3 V2 127.44(10) 4_455 . ?
O8 V3 O3 147.51(14) 4_455 . ?
O8 V3 O5 80.24(13) 4_455 . ?
O11 V3 V2 126.41(10) . 4_455 ?
O11 V3 V2 38.83(9) . . ?
O11 V3 O3 81.69(12) . . ?
O11 V3 O8 95.98(14) . 4_455 ?
O11 V3 O5 151.04(13) . . ?
O15 V3 V2 110.13(12) . . ?
O15 V3 V2 112.11(12) . 4_455 ?
O15 V3 O3 105.79(15) . . ?
O15 V3 O8 106.12(16) . 4_455 ?
O15 V3 O11 104.74(15) . . ?
O15 V3 O5 103.88(14) . . ?
O5 V3 V2 124.26(9) . . ?
O5 V3 V2 42.69(9) . 4_455 ?
O3 V4 V2 37.72(8) . . ?
O14 V4 V2 104.69(12) . . ?
O14 V4 O3 103.11(14) . . ?
O14 V4 O1 101.36(15) . 4_455 ?
O14 V4 O1 104.31(15) . . ?
O14 V4 O5 102.66(14) . 2_565 ?
O1 V4 V2 126.70(10) . . ?
O1 V4 V2 119.90(9) 4_455 . ?
O1 V4 O3 151.87(13) . . ?
O1 V4 O3 84.05(13) 4_455 . ?
O1 V4 O1 96.6(2) . 4_455 ?
O1 V4 O5 92.56(13) . 2_565 ?
O1 V4 O5 151.27(12) 4_455 2_565 ?
O5 V4 V2 37.71(9) 2_565 . ?
O5 V4 O3 75.37(12) 2_565 . ?
V2 O3 V4 102.98(14) . . ?
V3 O3 V2 95.40(12) . . ?
V3 O3 V4 149.93(16) . . ?
V2 O8 V3 103.71(15) . 2_565 ?
V2 O11 V3 101.86(14) . . ?
O9 S1 C6 104.1(3) . . ?
O9 S1 C11 105.0(2) . . ?
C6 S1 C11 99.1(3) . . ?
O2 S2 C1 104.3(3) . . ?
O2 S2 C8 106.5(3) . . ?
C8 S2 C1 96.9(3) . . ?
V4 O1 V4 139.34(17) . 2_565 ?
S2 O2 La1 131.74(19) . . ?
O12 N3 O4 120.9(4) 4_455 . ?
O12 N3 O4 120.9(4) 2_565 . ?
O12 N3 O4 120.9(4) . . ?
O12 N3 O4 120.9(4) 3_465 . ?
O12 N3 O12 74.7(3) 2_565 . ?
O12 N3 O12 118.2(7) 3_465 . ?
O12 N3 O12 74.7(3) 4_455 3_465 ?
O12 N3 O12 74.7(3) 4_455 . ?
O12 N3 O12 118.2(7) 4_455 2_565 ?
O12 N3 O12 74.7(3) 3_465 2_565 ?
S1 O9 La1 134.3(2) . . ?
V3 O5 V2 95.56(12) . 4_455 ?
V4 O5 V2 105.40(14) 4_455 4_455 ?
V4 O5 V3 142.55(16) 4_455 . ?
O6 S3 C3 118.9(8) . . ?
O6 S3 C5 108.2(9) . . ?
C5 S3 C3 97.0(8) . . ?
H1D N1 H1E 107.6 . . ?
C4 N1 H1D 108.7 . . ?
C4 N1 H1E 108.7 . . ?
C2 N1 H1D 108.7 2_565 . ?
C2 N1 H1E 108.7 2_565 . ?
C2 N1 C4 114.0(3) 2_565 . ?
N1 C4 H4A 109.5 . . ?
N1 C4 H4B 109.5 . . ?
N1 C4 C2 110.9(4) . . ?
H4A C4 H4B 108.0 . . ?
C2 C4 H4A 109.5 . . ?
C2 C4 H4B 109.5 . . ?
N1 C2 C4 110.1(3) 4_455 . ?
N1 C2 H2A 109.6 4_455 . ?
N1 C2 H2B 109.6 4_455 . ?
C4 C2 H2A 109.6 . . ?
C4 C2 H2B 109.6 . . ?
H2A C2 H2B 108.1 . . ?
S2 C1 H1A 109.5 . . ?
S2 C1 H1B 109.5 . . ?
S2 C1 H1C 109.5 . . ?
H1A C1 H1B 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
S1 C6 H6A 109.5 . . ?
S1 C6 H6B 109.5 . . ?
S1 C6 H6C 109.5 . . ?
H6A C6 H6B 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
S2 C8 H8A 109.5 . . ?
S2 C8 H8B 109.5 . . ?
S2 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
S1 C11 H11A 109.5 . . ?
S1 C11 H11B 109.5 . . ?
S1 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
N3 O12 O12 52.65(16) . 4_455 ?
N3 O12 O12 52.65(16) . 2_565 ?
O12 O12 O12 90.000(1) 4_455 2_565 ?
S3 C3 H3A 109.5 . . ?
S3 C3 H3B 109.5 . . ?
S3 C3 H3C 109.5 . . ?
H3A C3 H3B 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
S3 C5 H5A 109.5 . . ?
S3 C5 H5B 109.5 . . ?
S3 C5 H5C 109.5 . . ?
H5A C5 H5B 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
O6A S3A C3A 122.1(10) . . ?
O6A S3A C5A 99.2(12) . . ?
C5A S3A C3A 99.1(8) . . ?
S3A C3A H3AA 109.5 . . ?
S3A C3A H3AB 109.5 . . ?
S3A C3A H3AC 109.5 . . ?
H3AA C3A H3AB 109.5 . . ?
H3AA C3A H3AC 109.5 . . ?
H3AB C3A H3AC 109.5 . . ?
S3A C5A H5AA 109.5 . . ?
S3A C5A H5AB 109.5 . . ?
S3A C5A H5AC 109.5 . . ?
H5AA C5A H5AB 109.5 . . ?
H5AA C5A H5AC 109.5 . . ?
H5AB C5A H5AC 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
V2 V3 O3 V2 -128.13(8) 4_455 . . . ?
V2 V3 O3 V4 -0.3(3) 4_455 . . . ?
V2 V3 O3 V4 127.8(4) . . . . ?
V2 V3 O11 V2 123.40(10) 4_455 . . . ?
V2 V4 O1 V4 44.4(3) . . . 2_565 ?
V3 V2 O8 V3 109.07(14) . . . 2_565 ?
V3 V2 O11 V3 -110.07(12) 2_565 . . . ?
V4 V2 O8 V3 14.09(17) . . . 2_565 ?
V4 V2 O11 V3 -17.23(16) . . . . ?
O3 V2 O8 V3 49.1(3) . . . 2_565 ?
O3 V2 O11 V3 -0.30(13) . . . . ?
O3 V3 O11 V2 0.30(13) . . . . ?
O3 V4 O1 V4 -1.3(5) . . . 2_565 ?
O8 V2 O11 V3 -141.19(14) . . . . ?
O8 V3 O3 V2 -88.4(3) 4_455 . . . ?
O8 V3 O3 V4 39.5(5) 4_455 . . . ?
O8 V3 O11 V2 147.64(15) 4_455 . . . ?
O11 V2 O8 V3 140.63(15) . . . 2_565 ?
O11 V3 O3 V2 -0.28(12) . . . . ?
O11 V3 O3 V4 127.6(3) . . . . ?
O13 V2 O8 V3 -107.37(18) . . . 2_565 ?
O13 V2 O11 V3 105.95(17) . . . . ?
O14 V4 O1 V4 165.5(3) . . . 2_565 ?
O15 V3 O3 V2 102.77(15) . . . . ?
O15 V3 O3 V4 -129.4(3) . . . . ?
O15 V3 O11 V2 -103.93(17) . . . . ?
O1 V4 O1 V4 -90.9(3) 4_455 . . 2_565 ?
O4 N3 O12 O12 -117.2(2) . . . 2_565 ?
O4 N3 O12 O12 117.2(2) . . . 4_455 ?
O5 V2 O8 V3 -3.65(14) 2_565 . . 2_565 ?
O5 V2 O11 V3 -50.1(3) 2_565 . . . ?
O5 V3 O3 V2 -153.82(13) . . . . ?
O5 V3 O3 V4 -26.0(3) . . . . ?
O5 V3 O11 V2 67.0(3) . . . . ?
O5 V4 O1 V4 61.8(3) 2_565 . . 2_565 ?
N1 C4 C2 N1 -57.1(5) . . . 4_455 ?
C2 N1 C4 C2 -81.9(5) 2_565 . . . ?
C1 S2 O2 La1 -160.4(4) . . . . ?
C6 S1 O9 La1 83.6(4) . . . . ?
C8 S2 O2 La1 97.9(3) . . . . ?
C11 S1 O9 La1 -172.7(3) . . . . ?
O12 N3 O12 O12 -62.8(2) 3_465 . . 4_455 ?
O12 N3 O12 O12 125.6(5) 4_455 . . 2_565 ?
O12 N3 O12 O12 -125.6(5) 2_565 . . 4_455 ?
O12 N3 O12 O12 62.8(2) 3_465 . . 2_565 ?


_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.6457(10)
2 0.3543(10)

