# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2021

####################################################################### 
# 
# 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_shelx
_database_code_depnum_ccdc_archive 'CCDC 2087735'
loop_
_audit_author_name
_audit_author_address
'thomas devic'
;cnrs
France
;
_audit_update_record             
;
2021-07-28 deposited with the CCDC.	2021-09-02 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            K3V3O3(pgal)3.2DMF
_chemical_melting_point          ?
_chemical_formula_moiety         C24H23K3N2O14V3
_chemical_formula_sum            'C24 H23 K3 N2 O14 V3'
_chemical_formula_weight         833.57

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0030 0.0010 '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'
N N 0.0050 0.0030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0090 0.0050 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.1860 0.2250 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
V V 0.2870 0.4800 '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                   8.1630(3)
_cell_length_b                   26.1908(8)
_cell_length_c                   15.0823(4)
_cell_angle_alpha                90
_cell_angle_beta                 104.210(3)
_cell_angle_gamma                90
_cell_volume                     3125.87(18)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    5561
_cell_measurement_theta_min      2.5730
_cell_measurement_theta_max      26.6

_exptl_crystal_description       prism
_exptl_crystal_colour            black
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.771
_exptl_crystal_F_000             1676
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.040
_exptl_crystal_size_mid          0.030
_exptl_crystal_size_min          0.020
_exptl_absorpt_coefficient_mu    1.142
_shelx_estimated_absorpt_T_min   0.956
_shelx_estimated_absorpt_T_max   0.978
_exptl_absorpt_correction_T_min  0.89567
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.67173
_diffrn_source                   synchrotron
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_monochromator  synchrotron
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Atlas'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Atlas
_diffrn_detector_area_resol_mean 10.2930
_diffrn_reflns_number            34565
_diffrn_reflns_av_unetI/netI     0.0599
_diffrn_reflns_av_R_equivalents  0.0735
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         2.568
_diffrn_reflns_theta_max         26.604
_diffrn_reflns_theta_full        23.768
_diffrn_measured_fraction_theta_max 0.940
_diffrn_measured_fraction_theta_full 0.965
_diffrn_reflns_Laue_measured_fraction_max 0.940
_diffrn_reflns_Laue_measured_fraction_full 0.965
_diffrn_reflns_point_group_measured_fraction_max 0.940
_diffrn_reflns_point_group_measured_fraction_full 0.965
_reflns_number_total             7285
_reflns_number_gt                5309
_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.
;

_computing_data_collection       'CrysAlis (Oxford Diffraction, 2006)'
_computing_cell_refinement       'CrysAlis (Oxford Diffraction, 2006)'
_computing_data_reduction        'CrysAlis (Oxford Diffraction, 2006)'
_computing_structure_solution    SHELXS-86
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_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)+(0.0418P)²+1.6024P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         7285
_refine_ls_number_parameters     419
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0707
_refine_ls_R_factor_gt           0.0426
_refine_ls_wR_factor_ref         0.1035
_refine_ls_wR_factor_gt          0.0919
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_restrained_S_all      1.034
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_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
V3 V 0.09644(7) 0.22551(2) 0.73744(3) 0.01904(12) Uani 1 1 d . . . . .
V1 V 0.28478(7) 0.22361(2) 0.53234(3) 0.02006(13) Uani 1 1 d . . . . .
V2 V 0.05804(7) 0.10515(2) 0.58933(3) 0.01938(13) Uani 1 1 d . . . . .
O24 O -0.0710(3) 0.25470(9) 0.68027(13) 0.0253(5) Uani 1 1 d . . . . .
O1 O 0.4527(3) 0.27880(8) 0.55891(13) 0.0240(5) Uani 1 1 d . . . . .
O11 O 0.1494(3) 0.05033(8) 0.52540(14) 0.0227(5) Uani 1 1 d . . . . .
O3 O 0.2384(3) 0.27476(8) 0.81908(13) 0.0214(5) Uani 1 1 d . . . . .
O14 O -0.1247(3) 0.11837(9) 0.52381(14) 0.0262(5) Uani 1 1 d . . . . .
O4 O 0.1162(3) 0.24799(9) 0.46660(14) 0.0268(5) Uani 1 1 d . . . . .
O2 O 0.2637(3) 0.23692(7) 0.66051(13) 0.0192(4) Uani 1 1 d . . . . .
O22 O 0.0853(3) 0.15066(8) 0.70154(13) 0.0206(5) Uani 1 1 d . . . . .
O12 O 0.2295(3) 0.14830(8) 0.54650(13) 0.0194(4) Uani 1 1 d . . . . .
C5 C 0.5412(4) 0.36569(11) 0.75958(19) 0.0228(7) Uani 1 1 d . . . . .
H5 H 0.606219 0.395000 0.782802 0.027 Uiso 1 1 calc R U . . .
O13 O 0.4169(3) 0.19582(8) 0.45054(13) 0.0219(5) Uani 1 1 d . . . . .
O21 O 0.0431(3) 0.19939(8) 0.84872(13) 0.0236(5) Uani 1 1 d . . . . .
O23 O 0.0355(3) 0.05121(8) 0.67505(14) 0.0261(5) Uani 1 1 d . . . . .
C3 C 0.3428(4) 0.30022(11) 0.77724(18) 0.0195(6) Uani 1 1 d . . . . .
C12 C 0.2951(4) 0.11980(11) 0.48464(18) 0.0192(6) Uani 1 1 d . . . . .
C13 C 0.3953(4) 0.14479(11) 0.43555(19) 0.0202(6) Uani 1 1 d . . . . .
C11 C 0.2540(4) 0.06812(11) 0.47445(19) 0.0198(6) Uani 1 1 d . . . . .
C23 C 0.0098(4) 0.06999(12) 0.7549(2) 0.0241(7) Uani 1 1 d . . . . .
C2 C 0.3552(4) 0.28141(11) 0.69238(18) 0.0192(6) Uani 1 1 d . . . . .
C1 C 0.4547(4) 0.30296(11) 0.63897(19) 0.0206(6) Uani 1 1 d . . . . .
C24 C -0.0359(4) 0.04125(13) 0.8242(2) 0.0290(7) Uani 1 1 d . . . . .
H24 H -0.050996 0.005338 0.818058 0.035 Uiso 1 1 calc R U . . .
C4 C 0.4415(4) 0.34328(11) 0.81202(19) 0.0216(7) Uani 1 1 d . . . . .
H4 H 0.440111 0.356834 0.870265 0.026 Uiso 1 1 calc R U . . .
C14 C 0.4630(4) 0.11608(12) 0.3742(2) 0.0244(7) Uani 1 1 d . . . . .
H14 H 0.534054 0.131657 0.340670 0.029 Uiso 1 1 calc R U . . .
C26 C -0.0372(4) 0.11944(13) 0.91404(19) 0.0268(7) Uani 1 1 d . . . . .
H26 H -0.055874 0.135613 0.967082 0.032 Uiso 1 1 calc R U . . .
C6 C 0.5489(4) 0.34637(12) 0.6731(2) 0.0239(7) Uani 1 1 d . . . . .
H6 H 0.617062 0.362667 0.638778 0.029 Uiso 1 1 calc R U . . .
C16 C 0.3190(4) 0.03924(12) 0.4124(2) 0.0256(7) Uani 1 1 d . . . . .
H16 H 0.293463 0.003947 0.403471 0.031 Uiso 1 1 calc R U . . .
C21 C 0.0126(4) 0.14820(12) 0.84597(19) 0.0212(6) Uani 1 1 d . . . . .
C25 C -0.0587(5) 0.06649(14) 0.9019(2) 0.0314(8) Uani 1 1 d . . . . .
H25 H -0.089917 0.047062 0.948398 0.038 Uiso 1 1 calc R U . . .
C22 C 0.0332(4) 0.12225(12) 0.76864(19) 0.0209(6) Uani 1 1 d . . . . .
C15 C 0.4234(4) 0.06401(13) 0.3636(2) 0.0271(7) Uani 1 1 d . . . . .
H15 H 0.468550 0.044598 0.321896 0.033 Uiso 1 1 calc R U . . .
K1 K 0.85242(10) 0.03758(3) 0.38032(5) 0.02933(18) Uani 1 1 d . . . . .
K2 K 0.73048(9) 0.23354(3) 0.50074(4) 0.02772(17) Uani 1 1 d . . . . .
K3 K 0.22948(9) 0.24601(3) 0.30100(4) 0.02838(17) Uani 1 1 d . . . . .
O31 O 0.6176(3) 0.18408(10) 0.66326(17) 0.0393(6) Uani 1 1 d . . . . .
O41 O 0.6654(3) 0.04778(11) 0.20830(17) 0.0457(7) Uani 1 1 d . . . . .
N31 N 0.5322(4) 0.11381(11) 0.7290(2) 0.0338(7) Uani 1 1 d . . . . .
C31 C 0.5941(4) 0.13761(14) 0.6657(2) 0.0326(8) Uani 1 1 d . . . . .
H31 H 0.621930 0.117272 0.619316 0.039 Uiso 1 1 calc R U . . .
N41 N 0.4904(4) 0.09103(13) 0.0901(2) 0.0468(9) Uani 1 1 d . . . . .
C33 C 0.4963(5) 0.14200(16) 0.8058(2) 0.0433(10) Uani 1 1 d . . . . .
H33A H 0.597050 0.142134 0.856945 0.065 Uiso 1 1 calc R U . . .
H33B H 0.402764 0.125555 0.824909 0.065 Uiso 1 1 calc R U . . .
H33C H 0.465130 0.177199 0.786880 0.065 Uiso 1 1 calc R U . . .
C32 C 0.5093(6) 0.05847(15) 0.7268(3) 0.0525(11) Uani 1 1 d . . . . .
H32A H 0.520918 0.045157 0.667945 0.079 Uiso 1 1 calc R U . . .
H32B H 0.396580 0.050260 0.734637 0.079 Uiso 1 1 calc R U . . .
H32C H 0.595167 0.042858 0.776425 0.079 Uiso 1 1 calc R U . . .
C41 C 0.6253(6) 0.08561(17) 0.1576(3) 0.0535(12) Uani 1 1 d . . . . .
H41 H 0.701171 0.113712 0.169053 0.064 Uiso 1 1 calc R U . . .
C43 C 0.4439(6) 0.13991(16) 0.0431(3) 0.0530(11) Uani 1 1 d . . . . .
H43A H 0.376744 0.160005 0.076204 0.079 Uiso 1 1 calc R U . . .
H43B H 0.377333 0.133568 -0.019378 0.079 Uiso 1 1 calc R U . . .
H43C H 0.546585 0.158812 0.041205 0.079 Uiso 1 1 calc R U . . .
C42 C 0.3620(8) 0.0498(2) 0.0731(5) 0.125(3) Uani 1 1 d . . . . .
H42A H 0.417507 0.016915 0.091184 0.187 Uiso 1 1 calc R U . . .
H42B H 0.304822 0.048934 0.007864 0.187 Uiso 1 1 calc R U . . .
H42C H 0.278973 0.056274 0.108892 0.187 Uiso 1 1 calc R U . . .


_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
V3 O24 1.618(2) . ?
V3 O3 1.955(2) . ?
V3 O21 1.958(2) . ?
V3 O2 2.019(2) . ?
V3 O22 2.030(2) . ?
V1 O4 1.617(2) . ?
V1 O1 1.965(2) . ?
V1 O13 1.967(2) . ?
V1 O2 2.0128(19) . ?
V1 O12 2.046(2) . ?
V2 O14 1.612(2) . ?
V2 O23 1.954(2) . ?
V2 O11 1.975(2) . ?
V2 O12 2.024(2) . ?
V2 O22 2.037(2) . ?
O24 K3 2.725(2) 4_566 ?
O24 K2 2.848(2) 1_455 ?
O1 C1 1.360(3) . ?
O1 K2 2.879(2) . ?
O11 C11 1.363(4) . ?
O11 K1 2.708(2) 3_656 ?
O11 K1 2.859(2) 1_455 ?
O3 C3 1.354(4) . ?
O3 K2 2.765(2) 4_566 ?
O14 K1 3.000(2) 1_455 ?
O14 K2 3.227(2) 1_455 ?
O4 K3 2.869(2) . ?
O4 K2 3.335(2) 1_455 ?
O2 C2 1.404(3) . ?
O22 C22 1.404(3) . ?
O12 C12 1.400(3) . ?
C5 C4 1.396(4) . ?
C5 C6 1.414(4) . ?
C5 K3 3.293(3) 4_666 ?
O13 C13 1.360(3) . ?
O13 K2 2.674(2) . ?
O13 K3 2.732(2) . ?
O21 C21 1.362(4) . ?
O21 K3 2.866(2) 4_566 ?
O21 K2 2.993(2) 4_566 ?
O23 C23 1.365(3) . ?
O23 K1 2.705(2) 3_656 ?
C3 C2 1.398(4) . ?
C3 C4 1.410(4) . ?
C3 K3 3.317(3) 4_666 ?
C12 C13 1.394(4) . ?
C12 C11 1.394(4) . ?
C13 C14 1.407(4) . ?
C11 C16 1.405(4) . ?
C23 C22 1.390(4) . ?
C23 C24 1.410(4) . ?
C2 C1 1.396(4) . ?
C2 K3 3.174(3) 4_666 ?
C1 C6 1.398(4) . ?
C1 K3 3.155(3) 4_666 ?
C24 C25 1.398(4) . ?
C4 K3 3.349(3) 4_666 ?
C14 C15 1.402(4) . ?
C26 C25 1.404(5) . ?
C26 C21 1.411(4) . ?
C6 K3 3.217(3) 4_666 ?
C16 C15 1.413(5) . ?
C21 C22 1.395(4) . ?
K1 O41 2.681(3) . ?
K2 O31 3.106(3) . ?
K3 O31 2.751(3) 4_565 ?
O31 C31 1.234(4) . ?
O41 C41 1.245(5) . ?
N31 C31 1.339(4) . ?
N31 C32 1.461(5) . ?
N31 C33 1.462(5) . ?
N41 C41 1.311(5) . ?
N41 C43 1.467(5) . ?
N41 C42 1.483(7) . ?

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
O24 V3 O3 108.44(10) . . ?
O24 V3 O21 106.58(10) . . ?
O3 V3 O21 85.00(9) . . ?
O24 V3 O2 103.04(10) . . ?
O3 V3 O2 83.37(8) . . ?
O21 V3 O2 150.27(9) . . ?
O24 V3 O22 109.74(10) . . ?
O3 V3 O22 141.82(9) . . ?
O21 V3 O22 83.49(8) . . ?
O2 V3 O22 88.96(8) . . ?
O4 V1 O1 106.31(11) . . ?
O4 V1 O13 106.06(10) . . ?
O1 V1 O13 86.42(9) . . ?
O4 V1 O2 105.07(10) . . ?
O1 V1 O2 84.07(8) . . ?
O13 V1 O2 148.85(9) . . ?
O4 V1 O12 105.57(10) . . ?
O1 V1 O12 148.06(9) . . ?
O13 V1 O12 82.97(8) . . ?
O2 V1 O12 89.63(8) . . ?
O14 V2 O23 109.75(11) . . ?
O14 V2 O11 105.10(10) . . ?
O23 V2 O11 84.58(9) . . ?
O14 V2 O12 107.02(10) . . ?
O23 V2 O12 143.08(9) . . ?
O11 V2 O12 82.90(8) . . ?
O14 V2 O22 106.24(10) . . ?
O23 V2 O22 83.24(8) . . ?
O11 V2 O22 148.60(9) . . ?
O12 V2 O22 89.73(8) . . ?
V3 O24 K3 101.88(9) . 4_566 ?
V3 O24 K2 128.59(11) . 1_455 ?
K3 O24 K2 109.89(8) 4_566 1_455 ?
C1 O1 V1 112.27(18) . . ?
C1 O1 K2 128.58(18) . . ?
V1 O1 K2 101.38(8) . . ?
C11 O11 V2 112.99(17) . . ?
C11 O11 K1 132.19(18) . 3_656 ?
V2 O11 K1 108.07(8) . 3_656 ?
C11 O11 K1 98.00(16) . 1_455 ?
V2 O11 K1 96.17(8) . 1_455 ?
K1 O11 K1 100.93(7) 3_656 1_455 ?
C3 O3 V3 112.02(16) . . ?
C3 O3 K2 132.14(16) . 4_566 ?
V3 O3 K2 114.70(9) . 4_566 ?
V2 O14 K1 100.09(10) . 1_455 ?
V2 O14 K2 121.76(10) . 1_455 ?
K1 O14 K2 128.70(7) 1_455 1_455 ?
V1 O4 K3 96.85(10) . . ?
V1 O4 K2 123.65(10) . 1_455 ?
K3 O4 K2 130.59(7) . 1_455 ?
C2 O2 V1 107.98(16) . . ?
C2 O2 V3 107.71(16) . . ?
V1 O2 V3 139.08(11) . . ?
C22 O22 V3 108.73(17) . . ?
C22 O22 V2 107.35(17) . . ?
V3 O22 V2 140.84(10) . . ?
C12 O12 V2 108.80(17) . . ?
C12 O12 V1 108.32(17) . . ?
V2 O12 V1 139.37(11) . . ?
C4 C5 C6 122.4(3) . . ?
C4 C5 K3 80.14(18) . 4_666 ?
C6 C5 K3 74.49(17) . 4_666 ?
C13 O13 V1 113.53(18) . . ?
C13 O13 K2 119.12(18) . . ?
V1 O13 K2 108.66(8) . . ?
C13 O13 K3 108.18(16) . . ?
V1 O13 K3 93.30(8) . . ?
K2 O13 K3 111.05(7) . . ?
C21 O21 V3 113.27(17) . . ?
C21 O21 K3 109.78(18) . 4_566 ?
V3 O21 K3 89.05(8) . 4_566 ?
C21 O21 K2 130.99(17) . 4_566 ?
V3 O21 K2 105.79(9) . 4_566 ?
K3 O21 K2 99.01(6) 4_566 4_566 ?
C23 O23 V2 112.55(19) . . ?
C23 O23 K1 136.01(18) . 3_656 ?
V2 O23 K1 108.88(9) . 3_656 ?
O3 C3 C2 116.6(3) . . ?
O3 C3 C4 126.0(2) . . ?
C2 C3 C4 117.3(3) . . ?
O3 C3 K3 117.47(18) . 4_666 ?
C2 C3 K3 71.91(17) . 4_666 ?
C4 C3 K3 79.07(18) . 4_666 ?
C13 C12 C11 123.6(3) . . ?
C13 C12 O12 118.3(3) . . ?
C11 C12 O12 118.1(3) . . ?
O13 C13 C12 116.3(3) . . ?
O13 C13 C14 125.4(3) . . ?
C12 C13 C14 118.4(3) . . ?
O11 C11 C12 115.9(3) . . ?
O11 C11 C16 125.7(3) . . ?
C12 C11 C16 118.4(3) . . ?
O23 C23 C22 116.1(3) . . ?
O23 C23 C24 126.0(3) . . ?
C22 C23 C24 117.9(3) . . ?
C1 C2 C3 124.7(3) . . ?
C1 C2 O2 118.3(2) . . ?
C3 C2 O2 117.0(3) . . ?
C1 C2 K3 76.51(17) . 4_666 ?
C3 C2 K3 83.34(17) . 4_666 ?
O2 C2 K3 110.66(17) . 4_666 ?
O1 C1 C2 116.3(3) . . ?
O1 C1 C6 126.3(3) . . ?
C2 C1 C6 117.5(3) . . ?
O1 C1 K3 110.47(18) . 4_666 ?
C2 C1 K3 78.02(17) . 4_666 ?
C6 C1 K3 79.81(18) . 4_666 ?
C25 C24 C23 118.9(3) . . ?
C5 C4 C3 119.0(3) . . ?
C5 C4 K3 75.61(18) . 4_666 ?
C3 C4 K3 76.51(17) . 4_666 ?
C15 C14 C13 118.6(3) . . ?
C25 C26 C21 118.8(3) . . ?
C1 C6 C5 119.1(3) . . ?
C1 C6 K3 74.86(17) . 4_666 ?
C5 C6 K3 80.45(17) . 4_666 ?
C11 C16 C15 118.4(3) . . ?
O21 C21 C22 116.5(3) . . ?
O21 C21 C26 125.9(3) . . ?
C22 C21 C26 117.6(3) . . ?
C24 C25 C26 122.5(3) . . ?
C23 C22 C21 124.3(3) . . ?
C23 C22 O22 118.0(3) . . ?
C21 C22 O22 117.7(3) . . ?
C14 C15 C16 122.6(3) . . ?
O41 K1 O23 86.69(8) . 3_656 ?
O41 K1 O11 121.17(8) . 3_656 ?
O23 K1 O11 58.47(6) 3_656 3_656 ?
O41 K1 O11 154.61(8) . 1_655 ?
O23 K1 O11 92.82(7) 3_656 1_655 ?
O11 K1 O11 79.07(7) 3_656 1_655 ?
O41 K1 O14 123.21(8) . 1_655 ?
O23 K1 O14 149.69(7) 3_656 1_655 ?
O11 K1 O14 103.20(6) 3_656 1_655 ?
O11 K1 O14 58.29(6) 1_655 1_655 ?
O13 K2 O3 86.78(6) . 4_665 ?
O13 K2 O24 128.52(7) . 1_655 ?
O3 K2 O24 144.22(7) 4_665 1_655 ?
O13 K2 O1 57.85(6) . . ?
O3 K2 O1 123.09(6) 4_665 . ?
O24 K2 O1 86.39(6) 1_655 . ?
O13 K2 O21 74.11(6) . 4_665 ?
O3 K2 O21 54.48(6) 4_665 4_665 ?
O24 K2 O21 132.74(7) 1_655 4_665 ?
O1 K2 O21 72.50(6) . 4_665 ?
O13 K2 O31 67.70(7) . . ?
O3 K2 O31 146.40(7) 4_665 . ?
O24 K2 O31 62.64(7) 1_655 . ?
O1 K2 O31 61.50(7) . . ?
O21 K2 O31 130.89(7) 4_665 . ?
O13 K2 O14 89.14(6) . 1_655 ?
O3 K2 O14 86.35(6) 4_665 1_655 ?
O24 K2 O14 88.36(6) 1_655 1_655 ?
O1 K2 O14 130.31(6) . 1_655 ?
O21 K2 O14 137.38(6) 4_665 1_655 ?
O31 K2 O14 72.35(6) . 1_655 ?
O13 K2 O4 150.79(6) . 1_655 ?
O3 K2 O4 66.64(6) 4_665 1_655 ?
O24 K2 O4 77.66(6) 1_655 1_655 ?
O1 K2 O4 147.60(6) . 1_655 ?
O21 K2 O4 98.02(6) 4_665 1_655 ?
O31 K2 O4 130.05(6) . 1_655 ?
O14 K2 O4 77.75(6) 1_655 1_655 ?
O24 K3 O13 104.06(7) 4_665 . ?
O24 K3 O31 69.02(7) 4_665 4_565 ?
O13 K3 O31 163.42(8) . 4_565 ?
O24 K3 O21 61.81(6) 4_665 4_665 ?
O13 K3 O21 75.40(6) . 4_665 ?
O31 K3 O21 88.17(7) 4_565 4_665 ?
O24 K3 O4 162.79(7) 4_665 . ?
O13 K3 O4 61.62(6) . . ?
O31 K3 O4 121.82(8) 4_565 . ?
O21 K3 O4 103.37(6) 4_665 . ?
C31 O31 K3 131.2(2) . 4_666 ?
C31 O31 K2 120.9(2) . . ?
K3 O31 K2 102.16(8) 4_666 . ?
C41 O41 K1 132.5(3) . . ?
C31 N31 C32 120.9(3) . . ?
C31 N31 C33 120.9(3) . . ?
C32 N31 C33 118.0(3) . . ?
O31 C31 N31 124.7(3) . . ?
C41 N41 C43 122.5(4) . . ?
C41 N41 C42 118.6(4) . . ?
C43 N41 C42 117.6(4) . . ?
O41 C41 N41 127.4(4) . . ?

_refine_diff_density_max         0.501
_refine_diff_density_min         -0.518
_refine_diff_density_rms         0.088


_exptl_crystal_preparation       'Magnetic properties'
####################################################################### 
# 
# 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_shelx_CCDC1
_database_code_depnum_ccdc_archive 'CCDC 2087736'
loop_
_audit_author_name
_audit_author_address
'thomas devic'
;cnrs
France
;
_audit_update_record             
;
2021-07-28 deposited with the CCDC.	2021-09-02 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            K3V3O3(pgal)3.4H2O
_chemical_melting_point          ?
_chemical_formula_moiety         C18H17K3O16V3
_chemical_formula_sum            'C18 H17 K3 O16 V3'
_chemical_formula_weight         759.43

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'
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'
V V 0.3005 0.5294 '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/c'
_space_group_name_Hall           '-P 2ybc'

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

_cell_length_a                   13.734(3)
_cell_length_b                   14.379(3)
_cell_length_c                   15.837(3)
_cell_angle_alpha                90
_cell_angle_beta                 114.68(3)
_cell_angle_gamma                90
_cell_volume                     2841.6(12)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    58071
_cell_measurement_theta_min      2.611
_cell_measurement_theta_max      29.998

_exptl_crystal_description       prism
_exptl_crystal_colour            black
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.775
_exptl_crystal_F_000             1516
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.080
_exptl_absorpt_coefficient_mu    1.476
_shelx_estimated_absorpt_T_min   0.666
_shelx_estimated_absorpt_T_max   0.891
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5727
_exptl_absorpt_correction_T_max  0.7460
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            74041
_diffrn_reflns_av_unetI/netI     0.0553
_diffrn_reflns_av_R_equivalents  0.1042
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         2.611
_diffrn_reflns_theta_max         27.103
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             6277
_reflns_number_gt                4076
_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.
;

_computing_data_collection       'KappaCCD Software'
_computing_cell_refinement       'KappaCCD Software'
_computing_data_reduction        'KappaCCD Software'
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_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)+(0.0759P)²+10.8176P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6277
_refine_ls_number_parameters     360
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1137
_refine_ls_R_factor_gt           0.0659
_refine_ls_wR_factor_ref         0.1877
_refine_ls_wR_factor_gt          0.1606
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_restrained_S_all      1.075
_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 0.35417(8) 0.69327(6) 0.39534(6) 0.0300(2) Uani 1 1 d . . . . .
V2 V 0.46722(8) 0.52066(7) 0.28239(7) 0.0334(2) Uani 1 1 d . . . . .
V3 V 0.17479(8) 0.58012(7) 0.17204(6) 0.0332(3) Uani 1 1 d . . . . .
O4 O 0.3676(4) 0.7804(3) 0.3382(3) 0.0430(10) Uani 1 1 d . . . . .
O14 O 0.4907(4) 0.5936(3) 0.2162(3) 0.0504(12) Uani 1 1 d . . . . .
O24 O 0.1928(4) 0.6606(3) 0.1104(3) 0.0534(12) Uani 1 1 d . . . . .
O1 O 0.2565(3) 0.7261(3) 0.4516(3) 0.0383(9) Uani 1 1 d . . . . .
O2 O 0.2237(3) 0.6313(3) 0.3007(2) 0.0309(8) Uani 1 1 d . . . . .
O3 O 0.0348(3) 0.5938(4) 0.1712(3) 0.0546(13) Uani 1 1 d . . . . .
C1 C 0.1533(5) 0.7104(4) 0.3941(4) 0.0386(14) Uani 1 1 d . . . . .
C2 C 0.1361(5) 0.6617(4) 0.3130(4) 0.0376(13) Uani 1 1 d . . . . .
C3 C 0.0369(5) 0.6415(5) 0.2449(5) 0.0511(17) Uani 1 1 d . . . . .
C4 C -0.0536(6) 0.6719(8) 0.2566(6) 0.084(3) Uani 1 1 d . . . . .
H4 H -0.122247 0.661394 0.211052 0.101 Uiso 1 1 calc R U . . .
C5 C -0.0374(7) 0.7187(7) 0.3391(7) 0.089(3) Uani 1 1 d . . . . .
H5 H -0.096940 0.738110 0.348075 0.106 Uiso 1 1 calc R U . . .
C6 C 0.0633(6) 0.7372(6) 0.4075(5) 0.065(2) Uani 1 1 d . . . . .
H6 H 0.071001 0.767266 0.461953 0.078 Uiso 1 1 calc R U . . .
O11 O 0.4676(3) 0.7032(3) 0.5217(3) 0.0401(10) Uani 1 1 d . . . . .
O12 O 0.4487(3) 0.5937(3) 0.3822(3) 0.0318(8) Uani 1 1 d . . . . .
O13 O 0.6026(3) 0.4845(3) 0.3831(3) 0.0425(10) Uani 1 1 d . . . . .
C11 C 0.5543(5) 0.6490(4) 0.5349(4) 0.0341(13) Uani 1 1 d . . . . .
C12 C 0.5444(4) 0.5923(4) 0.4618(4) 0.0322(12) Uani 1 1 d . . . . .
C13 C 0.6253(5) 0.5353(4) 0.4618(4) 0.0384(14) Uani 1 1 d . . . . .
C14 C 0.7204(5) 0.5338(5) 0.5416(4) 0.0440(15) Uani 1 1 d . . . . .
H14 H 0.776115 0.495015 0.545054 0.053 Uiso 1 1 calc R U . . .
C15 C 0.7321(5) 0.5898(5) 0.6152(4) 0.0485(17) Uani 1 1 d . . . . .
H15 H 0.796705 0.589078 0.667850 0.058 Uiso 1 1 calc R U . . .
C16 C 0.6498(5) 0.6478(5) 0.6136(4) 0.0438(15) Uani 1 1 d . . . . .
H16 H 0.659138 0.684999 0.664458 0.053 Uiso 1 1 calc R U . . .
O21 O 0.4723(3) 0.3977(3) 0.2340(3) 0.0415(10) Uani 1 1 d . . . . .
O22 O 0.3080(3) 0.5031(3) 0.2153(3) 0.0335(9) Uani 1 1 d . . . . .
O23 O 0.1124(3) 0.4732(3) 0.0917(3) 0.0429(10) Uani 1 1 d . . . . .
C21 C 0.3768(5) 0.3700(4) 0.1704(4) 0.0368(13) Uani 1 1 d . . . . .
C22 C 0.2902(5) 0.4251(4) 0.1582(4) 0.0333(12) Uani 1 1 d . . . . .
C23 C 0.1864(5) 0.4103(4) 0.0945(4) 0.0382(14) Uani 1 1 d . . . . .
C24 C 0.1673(6) 0.3325(5) 0.0360(5) 0.0467(16) Uani 1 1 d . . . . .
H24 H 0.099271 0.320649 -0.010078 0.056 Uiso 1 1 calc R U . . .
C25 C 0.2531(6) 0.2736(5) 0.0490(5) 0.0522(18) Uani 1 1 d . . . . .
H25 H 0.240461 0.221237 0.011416 0.063 Uiso 1 1 calc R U . . .
C26 C 0.3557(6) 0.2893(4) 0.1149(5) 0.0462(16) Uani 1 1 d . . . . .
H26 H 0.410350 0.247369 0.122614 0.055 Uiso 1 1 calc R U . . .
K1 K 0.40005(17) 0.96617(11) 0.36592(13) 0.0649(5) Uani 1 1 d . . . . .
K3 K 0.37226(14) 0.71148(12) 0.64720(10) 0.0582(5) Uani 1 1 d . . . . .
K2 K 0.09174(15) 0.95650(14) 0.41914(12) 0.0684(5) Uani 1 1 d . . . . .
OW1 O 0.3140(5) 0.9173(4) 0.4947(4) 0.0661(15) Uani 1 1 d . . . . .
OW2 O 0.4313(5) 1.1182(4) 0.4707(4) 0.0699(15) Uani 1 1 d . . . . .
OW3A O 0.215(3) 0.956(2) 0.161(2) 0.279(17) Uiso 0.578(17) 1 d . . P . .
OW4A O 0.045(3) 0.893(3) 0.196(3) 0.35(2) Uiso 0.578(17) 1 d . . P . .
OW3B O 0.1635(14) 0.9450(12) 0.2720(12) 0.093(7) Uiso 0.422(17) 1 d . . P . .
OW4B O 0.245(3) 1.072(3) 0.190(2) 0.210(16) Uiso 0.422(17) 1 d . . P . .


_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 O4 1.600(4) . ?
V1 O1 1.953(4) . ?
V1 O11 1.962(4) . ?
V1 O12 2.001(4) . ?
V1 O2 2.002(4) . ?
V2 O14 1.608(4) . ?
V2 O21 1.940(4) . ?
V2 O13 1.948(4) . ?
V2 O12 2.001(4) . ?
V2 O22 2.008(4) . ?
V3 O24 1.598(5) . ?
V3 O3 1.926(4) . ?
V3 O23 1.950(4) . ?
V3 O22 1.999(4) . ?
V3 O2 2.001(4) . ?
O4 K1 2.714(4) . ?
O4 K3 3.055(4) 4_575 ?
O14 K1 2.988(5) 2_645 ?
O14 K3 3.196(5) 4_575 ?
O24 K3 2.932(5) 4_575 ?
O24 K2 3.228(5) 4_575 ?
O1 C1 1.345(7) . ?
O1 K3 2.839(4) . ?
O2 C2 1.367(7) . ?
O3 C3 1.346(8) . ?
O3 K2 2.624(5) 2_545 ?
C1 C6 1.393(9) . ?
C1 C2 1.394(8) . ?
C2 C3 1.370(9) . ?
C3 C4 1.400(10) . ?
C4 C5 1.402(11) . ?
C5 C6 1.380(11) . ?
C6 K2 3.173(9) . ?
O11 C11 1.364(7) . ?
O11 K3 2.801(4) . ?
O12 C12 1.391(7) . ?
O13 C13 1.362(7) . ?
O13 K3 2.904(5) 3_666 ?
C11 C12 1.375(8) . ?
C11 C16 1.382(8) . ?
C12 C13 1.380(8) . ?
C13 C14 1.388(9) . ?
C14 C15 1.370(10) . ?
C15 C16 1.396(10) . ?
O21 C21 1.338(7) . ?
O21 K3 2.684(4) 3_666 ?
O21 K1 2.977(5) 2_645 ?
O22 C22 1.395(6) . ?
O23 C23 1.348(7) . ?
O23 K2 2.746(5) 2_545 ?
O23 K2 2.815(5) 4_575 ?
C21 C22 1.374(8) . ?
C21 C26 1.410(8) . ?
C22 C23 1.377(8) . ?
C23 C24 1.405(8) . ?
C23 K2 3.170(6) 4_575 ?
C24 C25 1.396(10) . ?
C24 K2 3.478(7) 4_575 ?
C25 C26 1.377(10) . ?
K1 OW2 2.669(5) . ?
K1 OW1 2.840(5) . ?
K1 OW2 2.920(7) 3_676 ?
K1 OW3B 2.971(17) . ?
K1 OW4B 3.11(3) . ?
K1 OW3A 3.18(3) . ?
K3 OW3A 3.30(4) 4_576 ?
K2 OW1 2.831(6) . ?
K2 OW3B 2.889(17) . ?
OW3A OW4B 1.73(4) . ?
OW4A OW3B 1.73(4) . ?

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
O4 V1 O1 109.4(2) . . ?
O4 V1 O11 106.9(2) . . ?
O1 V1 O11 85.48(17) . . ?
O4 V1 O12 105.6(2) . . ?
O1 V1 O12 145.05(17) . . ?
O11 V1 O12 83.39(16) . . ?
O4 V1 O2 101.8(2) . . ?
O1 V1 O2 83.00(16) . . ?
O11 V1 O2 151.28(17) . . ?
O12 V1 O2 91.18(16) . . ?
O14 V2 O21 106.6(2) . . ?
O14 V2 O13 109.0(2) . . ?
O21 V2 O13 84.32(18) . . ?
O14 V2 O12 107.4(2) . . ?
O21 V2 O12 145.93(18) . . ?
O13 V2 O12 83.44(17) . . ?
O14 V2 O22 102.0(2) . . ?
O21 V2 O22 83.52(17) . . ?
O13 V2 O22 148.84(18) . . ?
O12 V2 O22 90.85(16) . . ?
O24 V3 O3 109.3(2) . . ?
O24 V3 O23 108.1(2) . . ?
O3 V3 O23 84.85(19) . . ?
O24 V3 O22 104.9(2) . . ?
O3 V3 O22 145.8(2) . . ?
O23 V3 O22 82.91(17) . . ?
O24 V3 O2 106.5(2) . . ?
O3 V3 O2 83.06(17) . . ?
O23 V3 O2 145.39(18) . . ?
O22 V3 O2 89.16(16) . . ?
V1 O4 K1 136.8(2) . . ?
V1 O4 K3 130.1(2) . 4_575 ?
K1 O4 K3 93.01(13) . 4_575 ?
V2 O14 K1 99.1(2) . 2_645 ?
V2 O14 K3 125.6(2) . 4_575 ?
K1 O14 K3 131.72(15) 2_645 4_575 ?
V3 O24 K3 131.6(2) . 4_575 ?
V3 O24 K2 94.6(2) . 4_575 ?
K3 O24 K2 120.66(16) 4_575 4_575 ?
C1 O1 V1 112.4(3) . . ?
C1 O1 K3 132.7(4) . . ?
V1 O1 K3 107.53(17) . . ?
C2 O2 V3 108.8(3) . . ?
C2 O2 V1 108.5(3) . . ?
V3 O2 V1 137.8(2) . . ?
C3 O3 V3 112.8(4) . . ?
C3 O3 K2 128.7(4) . 2_545 ?
V3 O3 K2 111.05(19) . 2_545 ?
O1 C1 C6 126.9(6) . . ?
O1 C1 C2 115.7(5) . . ?
C6 C1 C2 117.4(6) . . ?
O2 C2 C3 117.8(5) . . ?
O2 C2 C1 118.1(5) . . ?
C3 C2 C1 124.2(6) . . ?
O3 C3 C2 116.4(6) . . ?
O3 C3 C4 125.2(6) . . ?
C2 C3 C4 118.5(6) . . ?
C3 C4 C5 117.9(7) . . ?
C6 C5 C4 122.8(7) . . ?
C5 C6 C1 119.2(6) . . ?
C5 C6 K2 107.2(7) . . ?
C1 C6 K2 100.9(5) . . ?
C11 O11 V1 112.6(3) . . ?
C11 O11 K3 123.6(3) . . ?
V1 O11 K3 108.65(18) . . ?
C12 O12 V2 108.9(3) . . ?
C12 O12 V1 109.0(3) . . ?
V2 O12 V1 139.5(2) . . ?
C13 O13 V2 112.4(4) . . ?
C13 O13 K3 132.3(3) . 3_666 ?
V2 O13 K3 105.20(18) . 3_666 ?
O11 C11 C12 116.0(5) . . ?
O11 C11 C16 125.7(5) . . ?
C12 C11 C16 118.3(6) . . ?
C11 C12 C13 123.8(6) . . ?
C11 C12 O12 118.5(5) . . ?
C13 C12 O12 117.7(5) . . ?
O13 C13 C12 116.2(5) . . ?
O13 C13 C14 126.4(6) . . ?
C12 C13 C14 117.4(6) . . ?
C15 C14 C13 119.8(6) . . ?
C14 C15 C16 122.0(6) . . ?
C11 C16 C15 118.7(6) . . ?
C21 O21 V2 112.5(3) . . ?
C21 O21 K3 126.6(4) . 3_666 ?
V2 O21 K3 113.90(19) . 3_666 ?
C21 O21 K1 108.0(3) . 2_645 ?
V2 O21 K1 92.01(16) . 2_645 ?
K3 O21 K1 95.38(13) 3_666 2_645 ?
C22 O22 V3 109.6(3) . . ?
C22 O22 V2 107.5(3) . . ?
V3 O22 V2 138.6(2) . . ?
C23 O23 V3 112.8(4) . . ?
C23 O23 K2 132.8(4) . 2_545 ?
V3 O23 K2 105.61(17) . 2_545 ?
C23 O23 K2 92.3(3) . 4_575 ?
V3 O23 K2 100.89(18) . 4_575 ?
K2 O23 K2 106.51(15) 2_545 4_575 ?
O21 C21 C22 116.9(5) . . ?
O21 C21 C26 126.5(6) . . ?
C22 C21 C26 116.6(6) . . ?
C21 C22 C23 125.7(5) . . ?
C21 C22 O22 117.8(5) . . ?
C23 C22 O22 116.5(5) . . ?
O23 C23 C22 117.2(5) . . ?
O23 C23 C24 125.6(6) . . ?
C22 C23 C24 117.2(6) . . ?
O23 C23 K2 62.5(3) . 4_575 ?
C22 C23 K2 118.0(4) . 4_575 ?
C24 C23 K2 90.5(4) . 4_575 ?
C25 C24 C23 118.2(6) . . ?
C25 C24 K2 130.8(5) . 4_575 ?
C23 C24 K2 65.7(4) . 4_575 ?
C26 C25 C24 123.1(6) . . ?
C25 C26 C21 119.1(6) . . ?
OW2 K1 O4 151.60(17) . . ?
OW2 K1 OW1 76.28(17) . . ?
O4 K1 OW1 77.47(14) . . ?
OW2 K1 OW2 85.82(18) . 3_676 ?
O4 K1 OW2 75.54(14) . 3_676 ?
OW1 K1 OW2 71.04(17) . 3_676 ?
OW2 K1 OW3B 104.7(4) . . ?
O4 K1 OW3B 75.3(3) . . ?
OW1 K1 OW3B 68.8(4) . . ?
OW2 K1 OW3B 134.3(4) 3_676 . ?
OW2 K1 O21 128.63(16) . 2_655 ?
O4 K1 O21 71.44(12) . 2_655 ?
OW1 K1 O21 144.48(15) . 2_655 ?
OW2 K1 O21 84.72(14) 3_676 2_655 ?
OW3B K1 O21 117.6(3) . 2_655 ?
OW2 K1 O14 77.82(15) . 2_655 ?
O4 K1 O14 127.71(14) . 2_655 ?
OW1 K1 O14 154.09(15) . 2_655 ?
OW2 K1 O14 106.47(16) 3_676 2_655 ?
OW3B K1 O14 119.2(3) . 2_655 ?
O21 K1 O14 57.15(12) 2_655 2_655 ?
OW2 K1 OW4B 91.7(7) . . ?
O4 K1 OW4B 109.4(7) . . ?
OW1 K1 OW4B 115.6(7) . . ?
OW2 K1 OW4B 172.2(7) 3_676 . ?
OW3B K1 OW4B 53.5(7) . . ?
O21 K1 OW4B 91.0(7) 2_655 . ?
O14 K1 OW4B 65.7(7) 2_655 . ?
OW2 K1 OW3A 121.7(7) . . ?
O4 K1 OW3A 77.4(7) . . ?
OW1 K1 OW3A 109.1(7) . . ?
OW2 K1 OW3A 152.2(7) 3_676 . ?
OW3B K1 OW3A 41.0(7) . . ?
O21 K1 OW3A 80.7(6) 2_655 . ?
O14 K1 OW3A 85.2(6) 2_655 . ?
OW4B K1 OW3A 32.0(8) . . ?
O21 K3 O11 90.12(13) 3_666 . ?
O21 K3 O1 136.69(13) 3_666 . ?
O11 K3 O1 56.21(12) . . ?
O21 K3 O13 55.52(13) 3_666 3_666 ?
O11 K3 O13 73.64(13) . 3_666 ?
O1 K3 O13 86.71(13) . 3_666 ?
O21 K3 O24 149.58(14) 3_666 4_576 ?
O11 K3 O24 119.25(13) . 4_576 ?
O1 K3 O24 72.25(12) . 4_576 ?
O13 K3 O24 136.40(15) 3_666 4_576 ?
O21 K3 O4 70.57(12) 3_666 4_576 ?
O11 K3 O4 155.96(14) . 4_576 ?
O1 K3 O4 147.59(13) . 4_576 ?
O13 K3 O4 104.72(12) 3_666 4_576 ?
O24 K3 O4 79.01(13) 4_576 4_576 ?
O21 K3 O14 97.52(14) 3_666 4_576 ?
O11 K3 O14 87.59(13) . 4_576 ?
O1 K3 O14 106.34(13) . 4_576 ?
O13 K3 O14 146.01(14) 3_666 4_576 ?
O24 K3 O14 77.49(13) 4_576 4_576 ?
O4 K3 O14 81.14(12) 4_576 4_576 ?
O21 K3 OW3A 83.0(6) 3_666 4_576 ?
O11 K3 OW3A 121.8(6) . 4_576 ?
O1 K3 OW3A 92.4(6) . 4_576 ?
O13 K3 OW3A 55.2(6) 3_666 4_576 ?
O24 K3 OW3A 87.3(6) 4_576 4_576 ?
O4 K3 OW3A 71.3(6) 4_576 4_576 ?
O14 K3 OW3A 150.6(6) 4_576 4_576 ?
O3 K2 O23 58.22(13) 2 2 ?
O3 K2 O23 91.96(16) 2 4_576 ?
O23 K2 O23 73.49(15) 2 4_576 ?
O3 K2 OW1 137.05(16) 2 . ?
O23 K2 OW1 159.39(15) 2 . ?
O23 K2 OW1 90.42(15) 4_576 . ?
O3 K2 OW3B 88.6(4) 2 . ?
O23 K2 OW3B 129.6(4) 2 . ?
O23 K2 OW3B 150.9(4) 4_576 . ?
OW1 K2 OW3B 70.1(4) . . ?
O3 K2 C23 87.65(17) 2 4_576 ?
O23 K2 C23 92.09(16) 2 4_576 ?
O23 K2 C23 25.13(14) 4_576 4_576 ?
OW1 K2 C23 76.98(16) . 4_576 ?
OW3B K2 C23 126.0(4) . 4_576 ?
O3 K2 C6 132.7(2) 2 . ?
O23 K2 C6 89.19(17) 2 . ?
O23 K2 C6 111.90(18) 4_576 . ?
OW1 K2 C6 84.92(18) . . ?
OW3B K2 C6 88.4(4) . . ?
C23 K2 C6 130.27(19) 4_576 . ?
O3 K2 O24 146.18(15) 2 4_576 ?
O23 K2 O24 97.60(14) 2 4_576 ?
O23 K2 O24 56.41(12) 4_576 4_576 ?
OW1 K2 O24 62.25(14) . 4_576 ?
OW3B K2 O24 124.7(3) . 4_576 ?
C23 K2 O24 68.58(14) 4_576 4_576 ?
C6 K2 O24 62.00(17) . 4_576 ?
O3 K2 C24 67.45(17) 2 4_576 ?
O23 K2 C24 91.54(16) 2 4_576 ?
O23 K2 C24 44.25(13) 4_576 4_576 ?
OW1 K2 C24 85.37(17) . 4_576 ?
OW3B K2 C24 110.7(4) . 4_576 ?
C23 K2 C24 23.83(14) 4_576 4_576 ?
C6 K2 C24 154.10(19) . 4_576 ?
O24 K2 C24 92.27(14) 4_576 4_576 ?
K2 OW1 K1 110.2(2) . . ?
K1 OW2 K1 94.18(17) . 3_676 ?
OW4B OW3A K1 71.7(17) . . ?
OW4B OW3A K3 129(2) . 4_575 ?
K1 OW3A K3 80.6(8) . 4_575 ?
OW4A OW3B K2 92.7(16) . . ?
OW4A OW3B K1 154.5(17) . . ?
K2 OW3B K1 105.1(5) . . ?
OW3A OW4B K1 76.4(17) . . ?

_refine_diff_density_max         1.001
_refine_diff_density_min         -0.456
_refine_diff_density_rms         0.123


_exptl_crystal_preparation       'Magnetic properties'
