# Electronic Supplementary Material (ESI) for Journal of Materials Chemistry C.
# This journal is © The Royal Society of Chemistry 2023

####################################################################### 
# 
# 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_TEA4V4O8tart2x11H2O
_database_code_depnum_ccdc_archive 'CCDC 2221444'
loop_
_audit_author_name
_audit_author_address
'Lidija Andros Dubraja'
;Rudjer Boskovic Institute
Croatia
;
_audit_update_record             
;
2022-11-22 deposited with the CCDC.	2023-01-16 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2017/1
_shelx_SHELXL_version_number     2017/1
_chemical_name_systematic        ?
_chemical_name_common            '(TEA)4 [V4O8(tart)2] x 11H2O'
_chemical_melting_point          ?
_chemical_formula_moiety         'C8 H4 O20 V4, 4(C8 H20 N), 11(H2 O)'
_chemical_formula_sum            'C40 H106 N4 O31 V4'
_chemical_formula_weight         1343.04

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
V V 0.0687 2.1097 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_H-M_alt        'P 21 21 21'
_space_group_name_Hall           'P 2ac 2ab'

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

_cell_length_a                   13.21820(10)
_cell_length_b                   14.01030(10)
_cell_length_c                   34.1579(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     6325.73(9)
_cell_formula_units_Z            4
_cell_measurement_temperature    159.99(10)
_cell_measurement_reflns_used    20815
_cell_measurement_theta_min      3.5530
_cell_measurement_theta_max      78.9310

_exptl_crystal_description       stick
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.410
_exptl_crystal_F_000             2856
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_absorpt_coefficient_mu    5.551
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_T_min  0.37479
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.54a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_diffrn_ambient_temperature      159.99(10)
_diffrn_ambient_environment      N~2~
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_type            HyPix
_diffrn_detector_area_resol_mean 10.0000
_diffrn_reflns_number            28959
_diffrn_reflns_av_unetI/netI     0.0507
_diffrn_reflns_av_R_equivalents  0.0479
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -43
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_theta_min         3.410
_diffrn_reflns_theta_max         79.258
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.948
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.948
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.877
_diffrn_reflns_point_group_measured_fraction_full 0.953
_reflns_number_total             12027
_reflns_number_gt                11456
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.682
_reflns_Friedel_fraction_max     0.791
_reflns_Friedel_fraction_full    0.899

_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       'CrysAlisPro 1.171.42.54a (Rigaku OD, 2022)'
_computing_cell_refinement       'CrysAlisPro 1.171.42.54a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.54a (Rigaku OD, 2022)'
_computing_structure_solution    'SIR-2019 (Burla, 2015)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_molecular_graphics    'Mercury (2020)'
_computing_publication_material  'PLATON (Spek, 2009)'
_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)+(0.0635P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     'SHELXL-2017/1 (Sheldrick 2017)'
_refine_ls_extinction_coef       0.00010(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_abs_structure_details 
;
 Flack x determined using 4426 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.007(3)
_chemical_absolute_configuration rmad
_refine_ls_number_reflns         12027
_refine_ls_number_parameters     817
_refine_ls_number_restraints     33
_refine_ls_R_factor_all          0.0373
_refine_ls_R_factor_gt           0.0355
_refine_ls_wR_factor_ref         0.0920
_refine_ls_wR_factor_gt          0.0908
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_restrained_S_all      1.009
_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
C1 C -0.1420(3) 0.4991(3) 0.69295(13) 0.0339(9) Uani 1 1 d . . . . .
H1A H -0.143652 0.442636 0.709367 0.041 Uiso 1 1 calc R U . . .
H1B H -0.210050 0.525023 0.692265 0.041 Uiso 1 1 calc R U . . .
C2 C -0.1137(3) 0.4690(4) 0.65207(14) 0.0421(11) Uani 1 1 d . . . . .
H2A H -0.111284 0.524098 0.635386 0.063 Uiso 1 1 calc R U . . .
H2B H -0.163194 0.424907 0.642285 0.063 Uiso 1 1 calc R U . . .
H2C H -0.048495 0.438801 0.652473 0.063 Uiso 1 1 calc R U . . .
C3 C 0.0361(3) 0.5392(3) 0.71037(11) 0.0260(7) Uani 1 1 d . . . . .
H3A H 0.055190 0.532257 0.683095 0.031 Uiso 1 1 calc R U . . .
H3B H 0.078612 0.588498 0.721611 0.031 Uiso 1 1 calc R U . . .
C4 C 0.0578(3) 0.4468(3) 0.73109(13) 0.0395(10) Uani 1 1 d . . . . .
H4A H 0.018493 0.396559 0.719499 0.059 Uiso 1 1 calc R U . . .
H4B H 0.040376 0.452805 0.758260 0.059 Uiso 1 1 calc R U . . .
H4C H 0.128459 0.431885 0.728750 0.059 Uiso 1 1 calc R U . . .
C5 C -0.0797(3) 0.6659(3) 0.69052(13) 0.0308(8) Uani 1 1 d . . . . .
H5A H -0.069103 0.653721 0.662866 0.037 Uiso 1 1 calc R U . . .
H5B H -0.024992 0.706696 0.699387 0.037 Uiso 1 1 calc R U . . .
C6 C -0.1788(3) 0.7197(4) 0.69531(14) 0.0430(11) Uani 1 1 d . . . . .
H6A H -0.180161 0.772878 0.677592 0.064 Uiso 1 1 calc R U . . .
H6B H -0.184449 0.742475 0.721729 0.064 Uiso 1 1 calc R U . . .
H6C H -0.234293 0.677752 0.689643 0.064 Uiso 1 1 calc R U . . .
C7 C -0.1082(3) 0.5816(4) 0.75402(11) 0.0353(9) Uani 1 1 d . . . . .
H7A H -0.178399 0.601766 0.754002 0.042 Uiso 1 1 calc R U . . .
H7B H -0.105250 0.519176 0.766277 0.042 Uiso 1 1 calc R U . . .
C8 C -0.0480(4) 0.6505(4) 0.77838(15) 0.0546(14) Uani 1 1 d . . . . .
H8A H -0.044968 0.711119 0.765315 0.082 Uiso 1 1 calc R U . . .
H8B H 0.019248 0.626262 0.781972 0.082 Uiso 1 1 calc R U . . .
H8C H -0.079959 0.658247 0.803429 0.082 Uiso 1 1 calc R U . . .
C9 C 0.6256(3) 0.0887(3) 0.46619(11) 0.0283(8) Uani 1 1 d . . . . .
H9A H 0.681124 0.105269 0.448884 0.034 Uiso 1 1 calc R U . . .
H9B H 0.619232 0.019778 0.466034 0.034 Uiso 1 1 calc R U . . .
C10 C 0.5290(3) 0.1314(4) 0.44971(14) 0.0403(10) Uani 1 1 d . . . . .
H10A H 0.519506 0.109674 0.423311 0.060 Uiso 1 1 calc R U . . .
H10B H 0.533805 0.199754 0.449968 0.060 Uiso 1 1 calc R U . . .
H10C H 0.472540 0.111689 0.465446 0.060 Uiso 1 1 calc R U . . .
C11 C 0.5665(3) 0.1020(3) 0.53588(12) 0.0311(8) Uani 1 1 d . . . . .
H11A H 0.588097 0.120920 0.561897 0.037 Uiso 1 1 calc R U . . .
H11B H 0.509971 0.142429 0.528637 0.037 Uiso 1 1 calc R U . . .
C12 C 0.5301(4) -0.0004(4) 0.53756(16) 0.0479(12) Uani 1 1 d . . . . .
H12A H 0.503652 -0.018625 0.512465 0.072 Uiso 1 1 calc R U . . .
H12B H 0.477923 -0.006146 0.556974 0.072 Uiso 1 1 calc R U . . .
H12C H 0.585582 -0.041478 0.544298 0.072 Uiso 1 1 calc R U . . .
C13 C 0.7465(3) 0.0643(3) 0.51862(12) 0.0299(8) Uani 1 1 d . . . . .
H13A H 0.729232 -0.002932 0.519336 0.036 Uiso 1 1 calc R U . . .
H13B H 0.797024 0.073006 0.498336 0.036 Uiso 1 1 calc R U . . .
C14 C 0.7925(5) 0.0916(5) 0.55746(16) 0.0611(17) Uani 1 1 d . . . . .
H14A H 0.818835 0.155345 0.555914 0.092 Uiso 1 1 calc R U . . .
H14B H 0.846376 0.048167 0.563675 0.092 Uiso 1 1 calc R U . . .
H14C H 0.741702 0.088580 0.577489 0.092 Uiso 1 1 calc R U . . .
C15 C 0.6724(3) 0.2269(3) 0.50967(10) 0.0222(7) Uani 1 1 d . . . . .
H15A H 0.612128 0.259958 0.500801 0.027 Uiso 1 1 calc R U . . .
H15B H 0.683093 0.244057 0.536860 0.027 Uiso 1 1 calc R U . . .
C16 C 0.7610(3) 0.2621(4) 0.48616(15) 0.0414(11) Uani 1 1 d . . . . .
H16A H 0.752316 0.244314 0.459231 0.062 Uiso 1 1 calc R U . . .
H16B H 0.822141 0.234153 0.496093 0.062 Uiso 1 1 calc R U . . .
H16C H 0.765115 0.330338 0.488159 0.062 Uiso 1 1 calc R U . . .
C17 C 0.5000(3) 0.6461(3) 0.44642(11) 0.0225(7) Uani 1 1 d . . . . .
H17A H 0.512186 0.711272 0.438063 0.027 Uiso 1 1 calc R U . . .
H17B H 0.486665 0.608466 0.423151 0.027 Uiso 1 1 calc R U . . .
C18 C 0.4067(3) 0.6447(3) 0.47193(12) 0.0296(8) Uani 1 1 d . . . . .
H18A H 0.347914 0.655386 0.456042 0.044 Uiso 1 1 calc R U . . .
H18B H 0.411707 0.694081 0.491327 0.044 Uiso 1 1 calc R U . . .
H18C H 0.401321 0.583817 0.484634 0.044 Uiso 1 1 calc R U . . .
C19 C 0.5876(3) 0.5015(3) 0.47270(11) 0.0258(8) Uani 1 1 d . . . . .
H19A H 0.643676 0.481731 0.489101 0.031 Uiso 1 1 calc R U . . .
H19B H 0.525692 0.489130 0.487087 0.031 Uiso 1 1 calc R U . . .
C20 C 0.5875(3) 0.4409(3) 0.43619(14) 0.0371(9) Uani 1 1 d . . . . .
H20A H 0.534656 0.462034 0.418954 0.056 Uiso 1 1 calc R U . . .
H20B H 0.576047 0.375368 0.443166 0.056 Uiso 1 1 calc R U . . .
H20C H 0.651603 0.446595 0.423216 0.056 Uiso 1 1 calc R U . . .
C21 C 0.6818(3) 0.6318(3) 0.43811(10) 0.0229(7) Uani 1 1 d . . . . .
H21A H 0.683744 0.700362 0.434248 0.027 Uiso 1 1 calc R U . . .
H21B H 0.668035 0.602578 0.412922 0.027 Uiso 1 1 calc R U . . .
C22 C 0.7851(3) 0.5989(3) 0.45206(12) 0.0337(9) Uani 1 1 d . . . . .
H22A H 0.834711 0.612409 0.432282 0.050 Uiso 1 1 calc R U . . .
H22B H 0.783472 0.531503 0.457020 0.050 Uiso 1 1 calc R U . . .
H22C H 0.802560 0.632094 0.475714 0.050 Uiso 1 1 calc R U . . .
C23 C 0.6116(3) 0.6538(3) 0.50565(10) 0.0238(7) Uani 1 1 d . . . . .
H23A H 0.557906 0.632851 0.522968 0.029 Uiso 1 1 calc R U . . .
H23B H 0.675095 0.630954 0.516402 0.029 Uiso 1 1 calc R U . . .
C24 C 0.6135(3) 0.7614(3) 0.50525(11) 0.0305(8) Uani 1 1 d . . . . .
H24A H 0.665467 0.783055 0.487763 0.046 Uiso 1 1 calc R U . . .
H24B H 0.626958 0.784589 0.531167 0.046 Uiso 1 1 calc R U . . .
H24C H 0.549081 0.784989 0.496553 0.046 Uiso 1 1 calc R U . . .
C25 C 0.3574(3) 0.6640(3) 0.79974(10) 0.0299(8) Uani 1 1 d . . . . .
H25A H 0.409183 0.641649 0.817651 0.036 Uiso 1 1 calc R U . . .
H25B H 0.322634 0.716702 0.812311 0.036 Uiso 1 1 calc R U . . .
C26 C 0.2827(3) 0.5846(4) 0.79329(13) 0.0435(11) Uani 1 1 d . . . . .
H26A H 0.232150 0.604858 0.774895 0.065 Uiso 1 1 calc R U . . .
H26B H 0.250886 0.568522 0.817693 0.065 Uiso 1 1 calc R U . . .
H26C H 0.317262 0.529591 0.783173 0.065 Uiso 1 1 calc R U . . .
C27 C 0.4655(3) 0.6221(3) 0.74220(11) 0.0248(7) Uani 1 1 d . . . . .
H27A H 0.418126 0.571590 0.735849 0.030 Uiso 1 1 calc R U . . .
H27B H 0.491360 0.647303 0.717704 0.030 Uiso 1 1 calc R U . . .
C28 C 0.5526(3) 0.5792(3) 0.76468(14) 0.0377(9) Uani 1 1 d . . . . .
H28A H 0.588607 0.535443 0.748139 0.057 Uiso 1 1 calc R U . . .
H28B H 0.527072 0.545796 0.787143 0.057 Uiso 1 1 calc R U . . .
H28C H 0.597475 0.629037 0.773057 0.057 Uiso 1 1 calc R U . . .
C29 C 0.4808(3) 0.7795(3) 0.77575(11) 0.0300(8) Uani 1 1 d . . . . .
H29A H 0.441824 0.829773 0.788135 0.036 Uiso 1 1 calc R U . . .
H29B H 0.526306 0.753612 0.795349 0.036 Uiso 1 1 calc R U . . .
C30 C 0.5435(4) 0.8232(3) 0.74345(14) 0.0415(10) Uani 1 1 d . . . . .
H30A H 0.499603 0.851390 0.724283 0.062 Uiso 1 1 calc R U . . .
H30B H 0.583917 0.774580 0.731300 0.062 Uiso 1 1 calc R U . . .
H30C H 0.586914 0.871462 0.754233 0.062 Uiso 1 1 calc R U . . .
C31 C 0.3309(3) 0.7374(3) 0.73390(11) 0.0273(8) Uani 1 1 d . . . . .
H31A H 0.366341 0.763274 0.711402 0.033 Uiso 1 1 calc R U . . .
H31B H 0.290591 0.683918 0.724886 0.033 Uiso 1 1 calc R U . . .
C32 C 0.2605(3) 0.8134(4) 0.74996(15) 0.0420(11) Uani 1 1 d . . . . .
H32A H 0.216956 0.835799 0.729432 0.063 Uiso 1 1 calc R U . . .
H32B H 0.299737 0.865767 0.759912 0.063 Uiso 1 1 calc R U . . .
H32C H 0.220393 0.786855 0.770682 0.063 Uiso 1 1 calc R U . . .
C33 C 0.1648(2) 0.3069(2) 0.64387(9) 0.0176(6) Uani 1 1 d . . . . .
C34 C 0.2713(2) 0.2695(2) 0.65353(10) 0.0171(6) Uani 1 1 d . . . . .
H34 H 0.268487 0.209490 0.668251 0.020 Uiso 1 1 calc R U . . .
C35 C 0.3274(2) 0.2569(2) 0.61410(9) 0.0144(6) Uani 1 1 d . . . . .
H35 H 0.289477 0.213051 0.597250 0.017 Uiso 1 1 calc R U . . .
C36 C 0.4337(2) 0.2187(2) 0.62056(9) 0.0163(6) Uani 1 1 d . . . . .
C37 C 0.4147(2) 0.7621(2) 0.62967(9) 0.0147(6) Uani 1 1 d . . . . .
C38 C 0.5068(2) 0.7281(2) 0.60683(9) 0.0142(6) Uani 1 1 d . . . . .
H38 H 0.525197 0.775339 0.586912 0.017 Uiso 1 1 calc R U . . .
C39 C 0.5956(2) 0.7122(2) 0.63494(9) 0.0151(6) Uani 1 1 d . . . . .
H39 H 0.613740 0.770949 0.648862 0.018 Uiso 1 1 calc R U . . .
C40 C 0.6849(2) 0.6730(2) 0.61120(9) 0.0151(6) Uani 1 1 d . . . . .
N1 N -0.0731(2) 0.5723(2) 0.71218(8) 0.0199(6) Uani 1 1 d . . . . .
N2 N 0.6529(2) 0.1205(2) 0.50752(8) 0.0223(6) Uani 1 1 d . . . . .
N3 N 0.5959(2) 0.6083(2) 0.46574(8) 0.0183(5) Uani 1 1 d . . . . .
N4 N 0.4085(2) 0.7010(2) 0.76309(8) 0.0195(6) Uani 1 1 d . . . . .
O1 O 0.48043(16) 0.33802(16) 0.53492(7) 0.0182(5) Uani 1 1 d . . . . .
O2 O 0.61315(17) 0.45535(18) 0.66933(7) 0.0213(5) Uani 1 1 d . . . . .
O3 O 0.29140(18) 0.65848(18) 0.55329(7) 0.0233(5) Uani 1 1 d . . . . .
O4 O 0.27797(17) 0.52256(19) 0.69172(7) 0.0226(5) Uani 1 1 d . . . . .
O5 O 0.39338(15) 0.49615(15) 0.55781(6) 0.0138(4) Uani 1 1 d . . . . .
O6 O 0.42905(16) 0.49339(17) 0.64052(7) 0.0189(5) Uani 1 1 d . . . . .
O7 O 0.57375(15) 0.44580(15) 0.59074(7) 0.0149(4) Uani 1 1 d . . . . .
O8 O 0.24984(15) 0.53892(16) 0.61267(7) 0.0161(4) Uani 1 1 d . . . . .
O9 O 0.50374(16) 0.27528(17) 0.60942(7) 0.0188(5) Uani 1 1 d . . . . .
O10 O 0.44665(18) 0.13873(17) 0.63504(8) 0.0246(5) Uani 1 1 d . . . . .
O11 O 0.33190(15) 0.34702(15) 0.59660(6) 0.0138(4) Uani 1 1 d . . . . .
O12 O 0.32068(16) 0.34144(17) 0.67485(6) 0.0165(4) Uani 1 1 d . . . . .
O13 O 0.16084(15) 0.39862(17) 0.64531(6) 0.0165(4) Uani 1 1 d . . . . .
O14 O 0.09593(17) 0.25337(19) 0.63482(8) 0.0268(5) Uani 1 1 d . . . . .
O15 O 0.68729(15) 0.58247(16) 0.61106(7) 0.0160(4) Uani 1 1 d . . . . .
O16 O 0.74427(17) 0.72606(17) 0.59345(7) 0.0211(5) Uani 1 1 d . . . . .
O17 O 0.56766(16) 0.63934(16) 0.66089(6) 0.0160(4) Uani 1 1 d . . . . .
O18 O 0.48597(15) 0.64076(16) 0.58919(7) 0.0154(4) Uani 1 1 d . . . . .
O19 O 0.33863(16) 0.70528(16) 0.62746(7) 0.0180(5) Uani 1 1 d . . . . .
O20 O 0.41614(17) 0.83771(17) 0.64822(7) 0.0216(5) Uani 1 1 d . . . . .
O21 O 0.5678(2) 0.9742(2) 0.63882(12) 0.0413(8) Uani 1 1 d D . . . .
O22 O 0.7587(3) 0.9109(3) 0.6215(2) 0.088(2) Uani 1 1 d D . . . .
O23 O 0.7311(2) 1.2882(2) 0.60788(11) 0.0394(7) Uani 1 1 d D . . . .
O24 O 0.8925(2) 1.2015(2) 0.64824(11) 0.0415(8) Uani 1 1 d D . . . .
O25 O 0.9286(2) 1.0051(2) 0.64400(12) 0.0464(8) Uani 1 1 d D . . . .
O26 O 1.1046(2) 0.9299(2) 0.67098(10) 0.0383(7) Uani 1 1 d D . . . .
O27 O 1.2896(2) 1.0013(2) 0.64791(15) 0.0569(11) Uani 1 1 d D . . . .
O28 O 1.1407(2) 0.7394(2) 0.65817(10) 0.0363(7) Uani 1 1 d D . . . .
O29 O 1.0605(2) 0.6224(3) 0.60060(10) 0.0405(7) Uani 1 1 d D . . . .
O30 O 0.8900(2) 0.6071(2) 0.55299(8) 0.0304(6) Uani 1 1 d D . . . .
O31 O 0.7618(2) 0.4411(2) 0.55060(9) 0.0343(7) Uani 1 1 d D . . . .
V1 V 0.45870(3) 0.39188(4) 0.57536(2) 0.01073(11) Uani 1 1 d . . . . .
V2 V 0.56245(4) 0.52033(4) 0.63614(2) 0.01196(12) Uani 1 1 d . . . . .
V3 V 0.34749(4) 0.59690(4) 0.58609(2) 0.01202(12) Uani 1 1 d . . . . .
V4 V 0.29746(4) 0.46101(4) 0.65334(2) 0.01310(12) Uani 1 1 d . . . . .
H21D H 0.537(3) 1.029(2) 0.6384(16) 0.039(13) Uiso 1 1 d D . . . .
H21E H 0.526(3) 0.928(2) 0.6411(15) 0.035(13) Uiso 1 1 d D . . . .
H22D H 0.705(4) 0.932(5) 0.632(2) 0.10(3) Uiso 1 1 d D . . . .
H22E H 0.755(4) 0.855(2) 0.6117(15) 0.043(14) Uiso 1 1 d D . . . .
H23D H 0.750(3) 1.329(3) 0.5914(12) 0.031(13) Uiso 1 1 d D . . . .
H23E H 0.669(3) 1.287(5) 0.615(2) 0.08(2) Uiso 1 1 d D . . . .
H24D H 0.845(3) 1.227(5) 0.6347(18) 0.07(2) Uiso 1 1 d D . . . .
H24E H 0.951(2) 1.227(4) 0.6443(16) 0.050(15) Uiso 1 1 d D . . . .
H25D H 0.919(4) 1.0653(19) 0.6480(16) 0.039(14) Uiso 1 1 d D . . . .
H25E H 0.874(2) 0.977(3) 0.6372(13) 0.021(10) Uiso 1 1 d D . . . .
H26D H 1.157(3) 0.958(5) 0.663(2) 0.08(2) Uiso 1 1 d D . . . .
H26E H 1.048(3) 0.955(4) 0.6634(16) 0.049(16) Uiso 1 1 d D . . . .
H27D H 1.329(4) 1.048(3) 0.642(2) 0.08(2) Uiso 1 1 d D . . . .
H27E H 1.316(5) 0.946(2) 0.648(2) 0.08(2) Uiso 1 1 d D . . . .
H28D H 1.124(4) 0.798(2) 0.6633(17) 0.052(17) Uiso 1 1 d D . . . .
H28E H 1.202(2) 0.732(3) 0.6518(13) 0.027(11) Uiso 1 1 d D . . . .
H29D H 1.074(4) 0.669(3) 0.6168(15) 0.054(17) Uiso 1 1 d D . . . .
H29E H 1.104(4) 0.579(3) 0.6023(17) 0.055(17) Uiso 1 1 d D . . . .
H30D H 0.942(2) 0.605(4) 0.5664(13) 0.036(13) Uiso 1 1 d D . . . .
H30E H 0.845(3) 0.641(3) 0.5632(14) 0.041(14) Uiso 1 1 d D . . . .
H31D H 0.808(3) 0.485(3) 0.5523(18) 0.049(16) Uiso 1 1 d D . . . .
H31E H 0.706(2) 0.460(4) 0.5610(15) 0.040(14) Uiso 1 1 d 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
C1 C2 1.506(7) . ?
C1 N1 1.521(5) . ?
C3 C4 1.503(6) . ?
C3 N1 1.518(4) . ?
C5 N1 1.509(5) . ?
C5 C6 1.520(6) . ?
C7 C8 1.503(7) . ?
C7 N1 1.508(4) . ?
C9 C10 1.519(6) . ?
C9 N2 1.523(4) . ?
C11 C12 1.515(6) . ?
C11 N2 1.519(4) . ?
C13 C14 1.509(6) . ?
C13 N2 1.514(5) . ?
C15 C16 1.504(5) . ?
C15 N2 1.514(5) . ?
C17 C18 1.510(5) . ?
C17 N3 1.524(4) . ?
C19 C20 1.509(6) . ?
C19 N3 1.518(4) . ?
C21 N3 1.513(4) . ?
C21 C22 1.518(5) . ?
C23 C24 1.507(6) . ?
C23 N3 1.519(4) . ?
C25 C26 1.504(7) . ?
C25 N4 1.514(4) . ?
C27 C28 1.508(6) . ?
C27 N4 1.516(4) . ?
C29 C30 1.510(6) . ?
C29 N4 1.520(5) . ?
C31 C32 1.517(6) . ?
C31 N4 1.519(4) . ?
C33 O14 1.219(4) . ?
C33 O13 1.287(4) . ?
C33 C34 1.538(4) . ?
C34 O12 1.404(4) . ?
C34 C35 1.548(4) . ?
C35 O11 1.398(4) . ?
C35 C36 1.520(4) . ?
C36 O10 1.237(4) . ?
C36 O9 1.277(4) . ?
C37 O20 1.235(4) . ?
C37 O19 1.285(4) . ?
C37 C38 1.522(4) . ?
C38 O18 1.391(4) . ?
C38 C39 1.533(4) . ?
C39 O17 1.402(4) . ?
C39 C40 1.533(4) . ?
C40 O16 1.239(4) . ?
C40 O15 1.269(4) . ?
O1 V1 1.600(2) . ?
O2 V2 1.601(2) . ?
O3 V3 1.597(2) . ?
O4 V4 1.590(3) . ?
O5 V1 1.800(2) . ?
O5 V3 1.815(2) . ?
O6 V2 1.810(2) . ?
O6 V4 1.850(2) . ?
O7 V1 1.777(2) . ?
O7 V2 1.876(2) . ?
O8 V3 1.775(2) . ?
O8 V4 1.876(2) . ?
O9 V1 2.092(2) . ?
O11 V1 1.932(2) . ?
O12 V4 1.855(2) . ?
O13 V4 2.025(2) . ?
O15 V2 2.053(2) . ?
O17 V2 1.871(2) . ?
O18 V3 1.934(2) . ?
O19 V3 2.078(2) . ?
V1 V2 3.0707(7) . ?
V3 V4 3.0561(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
C2 C1 N1 116.1(3) . . ?
C4 C3 N1 115.2(3) . . ?
N1 C5 C6 115.3(3) . . ?
C8 C7 N1 114.7(4) . . ?
C10 C9 N2 115.3(3) . . ?
C12 C11 N2 115.1(3) . . ?
C14 C13 N2 114.7(3) . . ?
C16 C15 N2 115.5(3) . . ?
C18 C17 N3 115.1(3) . . ?
C20 C19 N3 115.2(3) . . ?
N3 C21 C22 114.4(3) . . ?
C24 C23 N3 114.5(3) . . ?
C26 C25 N4 115.2(3) . . ?
C28 C27 N4 115.5(3) . . ?
C30 C29 N4 115.5(3) . . ?
C32 C31 N4 114.4(3) . . ?
O14 C33 O13 126.4(3) . . ?
O14 C33 C34 121.9(3) . . ?
O13 C33 C34 111.6(3) . . ?
O12 C34 C33 107.0(3) . . ?
O12 C34 C35 108.1(2) . . ?
C33 C34 C35 106.9(3) . . ?
O11 C35 C36 109.9(2) . . ?
O11 C35 C34 106.9(2) . . ?
C36 C35 C34 110.9(3) . . ?
O10 C36 O9 125.6(3) . . ?
O10 C36 C35 120.3(3) . . ?
O9 C36 C35 114.1(3) . . ?
O20 C37 O19 125.0(3) . . ?
O20 C37 C38 121.3(3) . . ?
O19 C37 C38 113.7(3) . . ?
O18 C38 C37 109.8(2) . . ?
O18 C38 C39 107.2(2) . . ?
C37 C38 C39 109.7(3) . . ?
O17 C39 C38 107.4(2) . . ?
O17 C39 C40 106.0(2) . . ?
C38 C39 C40 108.0(3) . . ?
O16 C40 O15 125.6(3) . . ?
O16 C40 C39 122.1(3) . . ?
O15 C40 C39 112.3(3) . . ?
C7 N1 C5 111.8(3) . . ?
C7 N1 C3 111.0(3) . . ?
C5 N1 C3 107.5(3) . . ?
C7 N1 C1 106.5(3) . . ?
C5 N1 C1 109.9(3) . . ?
C3 N1 C1 110.3(3) . . ?
C13 N2 C15 111.1(3) . . ?
C13 N2 C11 111.5(3) . . ?
C15 N2 C11 105.3(3) . . ?
C13 N2 C9 105.9(3) . . ?
C15 N2 C9 111.9(3) . . ?
C11 N2 C9 111.3(3) . . ?
C21 N3 C19 111.5(3) . . ?
C21 N3 C23 111.4(3) . . ?
C19 N3 C23 106.4(3) . . ?
C21 N3 C17 106.2(3) . . ?
C19 N3 C17 110.5(3) . . ?
C23 N3 C17 110.9(3) . . ?
C25 N4 C27 111.2(3) . . ?
C25 N4 C31 110.9(3) . . ?
C27 N4 C31 105.8(3) . . ?
C25 N4 C29 107.0(3) . . ?
C27 N4 C29 110.4(3) . . ?
C31 N4 C29 111.6(3) . . ?
V1 O5 V3 127.90(13) . . ?
V2 O6 V4 170.71(15) . . ?
V1 O7 V2 114.39(11) . . ?
V3 O8 V4 113.65(11) . . ?
C36 O9 V1 116.4(2) . . ?
C35 O11 V1 119.43(17) . . ?
C34 O12 V4 111.48(18) . . ?
C33 O13 V4 113.58(19) . . ?
C40 O15 V2 113.71(19) . . ?
C39 O17 V2 111.93(18) . . ?
C38 O18 V3 119.37(18) . . ?
C37 O19 V3 116.64(19) . . ?
O1 V1 O7 107.58(11) . . ?
O1 V1 O5 100.44(11) . . ?
O7 V1 O5 99.44(10) . . ?
O1 V1 O11 109.06(11) . . ?
O7 V1 O11 140.33(10) . . ?
O5 V1 O11 88.45(9) . . ?
O1 V1 O9 93.48(11) . . ?
O7 V1 O9 85.64(10) . . ?
O5 V1 O9 162.87(10) . . ?
O11 V1 O9 77.53(9) . . ?
O1 V1 V2 141.25(8) . . ?
O7 V1 V2 33.80(7) . . ?
O5 V1 V2 87.93(7) . . ?
O11 V1 V2 108.92(7) . . ?
O9 V1 V2 87.40(7) . . ?
O2 V2 O6 103.34(12) . . ?
O2 V2 O17 99.88(12) . . ?
O6 V2 O17 100.63(10) . . ?
O2 V2 O7 103.62(12) . . ?
O6 V2 O7 91.71(10) . . ?
O17 V2 O7 150.11(10) . . ?
O2 V2 O15 101.54(11) . . ?
O6 V2 O15 154.99(10) . . ?
O17 V2 O15 77.35(9) . . ?
O7 V2 O15 80.04(9) . . ?
O2 V2 V1 109.41(9) . . ?
O6 V2 V1 59.89(8) . . ?
O17 V2 V1 147.60(7) . . ?
O7 V2 V1 31.81(6) . . ?
O15 V2 V1 108.98(7) . . ?
O3 V3 O8 105.57(12) . . ?
O3 V3 O5 101.65(12) . . ?
O8 V3 O5 99.17(10) . . ?
O3 V3 O18 107.84(12) . . ?
O8 V3 O18 143.69(10) . . ?
O5 V3 O18 87.70(9) . . ?
O3 V3 O19 93.23(12) . . ?
O8 V3 O19 86.88(10) . . ?
O5 V3 O19 161.69(9) . . ?
O18 V3 O19 77.52(9) . . ?
O3 V3 V4 139.78(9) . . ?
O8 V3 V4 34.21(7) . . ?
O5 V3 V4 89.31(7) . . ?
O18 V3 V4 111.20(7) . . ?
O19 V3 V4 86.09(7) . . ?
O4 V4 O6 102.38(12) . . ?
O4 V4 O12 100.96(12) . . ?
O6 V4 O12 99.18(10) . . ?
O4 V4 O8 103.93(12) . . ?
O6 V4 O8 89.85(10) . . ?
O12 V4 O8 150.99(10) . . ?
O4 V4 O13 101.62(11) . . ?
O6 V4 O13 155.80(10) . . ?
O12 V4 O13 79.13(10) . . ?
O8 V4 O13 81.46(9) . . ?
O4 V4 V3 108.48(10) . . ?
O6 V4 V3 57.71(7) . . ?
O12 V4 V3 145.54(7) . . ?
O8 V4 V3 32.14(6) . . ?
O13 V4 V3 111.10(7) . . ?

_refine_diff_density_max         0.467
_refine_diff_density_min         -0.412
_refine_diff_density_rms         0.065



