# Electronic Supplementary Material (ESI) for New Journal of Chemistry.
# This journal is © The Royal Society of Chemistry and the Centre National de la Recherche Scientifique 2019

####################################################################### 
# 
# 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_lukr999_p-1
_database_code_depnum_ccdc_archive 'CCDC 1909250'
loop_
_audit_author_name
_audit_author_address
'Alexander Roller'
;University of Vienna
Austria
;
_audit_update_record             
;
2019-04-10 deposited with the CCDC.	2019-10-15 downloaded from the CCDC.
;
_audit_creation_date             2019-04-10
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelxl_version_number           2013-2
_chemical_name_systematic        
'bis(2-hydroxyethylpyridinium) [(decaaqua)(mu-decavanadato)dicobalt(II)]ate tetrahydrate'
_chemical_name_common            
'bis(2-hydroxyethylpyridinium) [(decaaqua)(mu-decavanadato)dicobalt(II)]ate tetrahydrate'
_chemical_formula_moiety         'Co2 H20 O38 V10, 2(C7 H10 N O), 4(H2 O)'
_chemical_formula_sum            'C14 H48 Co2 N2 O44 V10'
_chemical_compound_source        crystallization
_chemical_properties_physical    paramagnetic
_chemical_formula_weight         1575.80
_exptl_crystal_recrystallization_method 'evap. from water'
_chemical_melting_point          ?
_exptl_crystal_description       block
_exptl_crystal_colour            'clear orange'
_diffrn_ambient_temperature      100.0
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'
Co Co -2.3653 3.6143 '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'

_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      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
_chemical_absolute_configuration ?
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.4219(5)
_cell_length_b                   11.2451(6)
_cell_length_c                   11.9820(7)
_cell_angle_alpha                78.5909(17)
_cell_angle_beta                 75.1180(17)
_cell_angle_gamma                66.3817(17)
_cell_volume                     1117.66(11)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    9942
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      72.56
_cell_measurement_theta_min      5.707
_shelx_estimated_absorpt_T_max   0.453
_shelx_estimated_absorpt_T_min   0.182
_exptl_absorpt_coefficient_mu    23.514
_exptl_absorpt_correction_T_max  0.7536
_exptl_absorpt_correction_T_min  0.5338
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 
0.1020 before and 0.0565 after correction. The Ratio of minimum to maximum 
transmission is 0.7083. The λ/2 correction factor is Not present.'
;
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    2.341
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             782
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.04
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1267
_diffrn_reflns_av_unetI/netI     0.0827
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            16530
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.229
_diffrn_reflns_theta_min         5.464
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_source                   'sealed xray tube'
_diffrn_source_type              'Incoatec IuS'
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3882
_reflns_number_total             4079
_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 V8.38A (?, 2016)'
_computing_data_collection       'APEX 3'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         1.793
_refine_diff_density_min         -0.996
_refine_diff_density_rms         0.407
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.157
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     337
_refine_ls_number_reflns         4079
_refine_ls_number_restraints     20
_refine_ls_R_factor_all          0.0992
_refine_ls_R_factor_gt           0.0982
_refine_ls_restrained_S_all      1.188
_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)+(0.1705P)²]
 where P=(Fo²+2Fc²)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2196
_refine_ls_wR_factor_ref         0.2218
_refine_special_details          
;
_olex2_refinement_description
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups
2. Restrained distances
 H20-H19B_$2
 2.2 with sigma of 0.02
 H19A_$1-H16B
 2.2 with sigma of 0.02
 H20-O4_$3
 2 with sigma of 0.04
 H15B-O11_$4
 2 with sigma of 0.05
 H1SA-O14_$5
 2 with sigma of 0.05
 H16B-O2
 2.15 with sigma of 0.04
 H2SB-O1S_$1
 1.9 with sigma of 0.03
 H2SA-O2
 1.9 with sigma of 0.03
 H2SB-C2_$1
 3 with sigma of 0.1
 H2SA-H16B
 2.2 with sigma of 0.05
 H18B-O6_$4
 2 with sigma of 0.05
 H17A-O2S
 2 with sigma of 0.05
 H18A-H17B_$4
 2.15 with sigma of 0.02
 H19A-H19B ∼ H16A-H16B
 with sigma of 0.01
 O16-H16A ∼ O16-H16B ∼ O19-H19B ∼ O19-H19A
 with sigma of 0.01
3.a Free rotating group:
 O1S(H1SA,H1SB), O2S(H2SA,H2SB)
3.b Rotating group:
 O15(H15A,H15B), O16(H16A,H16B), O17(H17A,H17B), O18(H18A,H18B), O19(H19A,H19B)
3.c Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C7(H7A,H7B)
3.d Aromatic/amide H refined with riding coordinates:
 N1(H1), C1(H1A), C2(H2), C3(H3), C4(H4)
3.e Idealised tetrahedral OH refined as rotating group:
 O20(H20)
;
_atom_sites_solution_hydrogens   mixed
_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
Co1 Co 0.20852(8) 0.60317(7) 0.46590(5) 0.0396(3) Uani 1 1 d . . . . .
V1 V 0.34943(9) 0.24641(7) 0.56538(6) 0.0384(3) Uani 1 1 d . . . . .
V2 V 0.47903(9) 0.18044(7) 0.31190(6) 0.0393(3) Uani 1 1 d . . . . .
V3 V 0.20875(9) 0.06166(8) 0.74581(6) 0.0403(3) Uani 1 1 d . . . . .
V4 V 0.33203(9) -0.00351(7) 0.49198(6) 0.0382(3) Uani 1 1 d . . . . .
V5 V 0.47766(9) -0.07004(7) 0.23841(6) 0.0401(3) Uani 1 1 d . . . . .
O1 O 0.2887(4) 0.4027(3) 0.5181(3) 0.0406(8) Uani 1 1 d . . . . .
O2 O 0.4220(4) 0.3336(3) 0.2669(3) 0.0448(8) Uani 1 1 d D . . . .
O3 O 0.4543(4) 0.2358(3) 0.6753(3) 0.0410(7) Uani 1 1 d . . . . .
O4 O 0.6868(4) 0.1197(3) 0.2333(3) 0.0410(7) Uani 1 1 d D . . . .
O5 O 0.1755(4) 0.2299(3) 0.6626(3) 0.0409(7) Uani 1 1 d . . . . .
O6 O 0.3005(4) 0.1771(3) 0.4420(3) 0.0384(7) Uani 1 1 d D . . . .
O7 O 0.4091(4) 0.1136(3) 0.2192(3) 0.0407(7) Uani 1 1 d . . . . .
O8 O 0.3234(4) 0.0871(3) 0.8348(3) 0.0413(7) Uani 1 1 d . . . . .
O9 O 0.0398(4) 0.0840(4) 0.8291(3) 0.0467(8) Uani 1 1 d . . . . .
O10 O 0.4426(4) 0.0300(3) 0.6081(3) 0.0396(8) Uani 1 1 d . . . . .
O11 O 0.1693(4) 0.0225(3) 0.5992(3) 0.0409(7) Uani 1 1 d D . . . .
O12 O 0.4438(4) -0.1828(3) 0.5464(3) 0.0391(7) Uani 1 1 d . . . . .
O13 O 0.2874(4) -0.0349(3) 0.3752(3) 0.0408(7) Uani 1 1 d . . . . .
O14 O 0.4056(4) -0.0993(3) 0.1439(3) 0.0461(8) Uani 1 1 d D . . . .
O15 O 0.1296(4) 0.8003(3) 0.4135(3) 0.0492(8) Uani 1 1 d . . . . .
H15A H 0.1879 0.8449 0.4313 0.074 Uiso 1 1 d GR . . . .
H15B H 0.0256 0.8500 0.4534 0.074 Uiso 1 1 d DGR . . . .
O16 O 0.4251(4) 0.5778(3) 0.3472(3) 0.0440(8) Uani 1 1 d D . . . .
H16A H 0.4353 0.6573 0.3098 0.066 Uiso 1 1 d DGR . . . .
H16B H 0.4371 0.5366 0.2818 0.066 Uiso 1 1 d DGR . . . .
O17 O 0.1001(4) 0.5783(3) 0.3435(3) 0.0423(7) Uani 1 1 d . . . . .
H17A H 0.1454 0.5982 0.2617 0.063 Uiso 1 1 d DGR . . . .
H17B H -0.0101 0.6385 0.3433 0.063 Uiso 1 1 d DGR . . . .
O18 O -0.0059(4) 0.6316(3) 0.5873(3) 0.0437(7) Uani 1 1 d . . . . .
H18A H -0.0539 0.5650 0.5951 0.066 Uiso 1 1 d DGR . . . .
H18B H -0.0985 0.7102 0.5687 0.066 Uiso 1 1 d DGR . . . .
O19 O 0.3126(4) 0.6346(3) 0.5885(3) 0.0422(7) Uani 1 1 d D . . . .
H19A H 0.4009 0.5658 0.6000 0.063 Uiso 1 1 d DGR . . . .
H19B H 0.2500 0.6388 0.6596 0.063 Uiso 1 1 d DGR . . . .
O20 O 1.1323(4) 0.7398(3) 0.7782(3) 0.0480(8) Uani 1 1 d . . . . .
H20 H 1.1910 0.7744 0.7891 0.072 Uiso 1 1 calc DGR . . . .
N1 N 0.7316(5) 0.7280(4) 0.9580(3) 0.0492(9) Uani 1 1 d . . . . .
H1 H 0.6872 0.7811 0.9016 0.059 Uiso 1 1 calc R . . . .
C1 C 0.6751(7) 0.6353(6) 1.0129(5) 0.0571(12) Uani 1 1 d . . . . .
H1A H 0.5891 0.6284 0.9906 0.069 Uiso 1 1 calc R . . . .
C2 C 0.7408(7) 0.5506(6) 1.1007(5) 0.0574(12) Uani 1 1 d D . . . .
H2 H 0.7014 0.4846 1.1400 0.069 Uiso 1 1 calc R . . . .
C3 C 0.8661(7) 0.5628(5) 1.1314(4) 0.0553(12) Uani 1 1 d . . . . .
H3 H 0.9126 0.5052 1.1928 0.066 Uiso 1 1 calc R . . . .
C4 C 0.9236(7) 0.6579(5) 1.0733(4) 0.0517(11) Uani 1 1 d . . . . .
H4 H 1.0110 0.6646 1.0935 0.062 Uiso 1 1 calc R . . . .
C5 C 0.8532(6) 0.7443(5) 0.9849(4) 0.0472(10) Uani 1 1 d . . . . .
C6 C 0.8997(6) 0.8533(5) 0.9176(4) 0.0489(11) Uani 1 1 d . . . . .
H6A H 0.9758 0.8646 0.9542 0.059 Uiso 1 1 calc R . . . .
H6B H 0.8051 0.9349 0.9210 0.059 Uiso 1 1 calc R . . . .
C7 C 0.9744(6) 0.8314(5) 0.7904(4) 0.0480(10) Uani 1 1 d . . . . .
H7A H 0.9109 0.7993 0.7585 0.058 Uiso 1 1 calc R . . . .
H7B H 0.9734 0.9155 0.7452 0.058 Uiso 1 1 calc R . . . .
O1S O 0.6985(6) 0.2109(4) 0.9994(3) 0.0651(10) Uani 1 1 d D . . . .
H1SA H 0.6891 0.1569 0.9615 0.098 Uiso 1 1 d DG . . . .
H1SB H 0.6898 0.1761 1.0712 0.098 Uiso 1 1 d G . . . .
O2S O 0.2931(6) 0.5742(5) 0.1384(3) 0.0673(11) Uani 1 1 d D . . . .
H2SA H 0.3615 0.4955 0.1494 0.101 Uiso 1 1 d DG . . . .
H2SB H 0.3361 0.6076 0.0733 0.101 Uiso 1 1 d DG . . . .


_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
Co1 O1 2.089(3) . ?
Co1 O15 2.057(4) . ?
Co1 O16 2.115(4) . ?
Co1 O17 2.105(4) . ?
Co1 O18 2.111(3) . ?
Co1 O19 2.113(3) . ?
V1 V2 3.0865(9) . ?
V1 V3 3.1151(10) . ?
V1 V5 3.1062(10) 2_656 ?
V1 O1 1.645(3) . ?
V1 O3 1.799(3) . ?
V1 O5 1.805(3) . ?
V1 O6 2.024(3) . ?
V1 O10 2.232(3) . ?
V1 O12 2.006(3) 2_656 ?
V2 V5 3.1186(11) . ?
V2 O2 1.608(4) . ?
V2 O4 1.850(3) . ?
V2 O6 1.985(3) . ?
V2 O7 1.827(3) . ?
V2 O10 2.265(3) 2_656 ?
V2 O12 2.020(3) 2_656 ?
V3 V4 3.0856(9) . ?
V3 V5 3.0482(11) 2_656 ?
V3 O4 1.873(3) 2_656 ?
V3 O5 1.900(3) . ?
V3 O8 1.829(3) . ?
V3 O9 1.598(4) . ?
V3 O10 2.333(3) . ?
V3 O11 2.048(3) . ?
V4 V5 3.0998(9) . ?
V4 O6 1.924(3) . ?
V4 O10 2.088(3) 2_656 ?
V4 O10 2.105(3) . ?
V4 O11 1.692(3) . ?
V4 O12 1.932(3) . ?
V4 O13 1.696(3) . ?
V5 V1 3.1061(10) 2_656 ?
V5 V3 3.0482(11) 2_656 ?
V5 O3 1.891(3) 2_656 ?
V5 O7 1.885(3) . ?
V5 O8 1.804(3) 2_656 ?
V5 O10 2.336(3) 2_656 ?
V5 O13 2.058(3) . ?
V5 O14 1.604(3) . ?
O3 V5 1.891(3) 2_656 ?
O4 V3 1.873(3) 2_656 ?
O8 V5 1.804(3) 2_656 ?
O10 V2 2.265(3) 2_656 ?
O10 V4 2.088(3) 2_656 ?
O10 V5 2.336(3) 2_656 ?
O12 V1 2.006(3) 2_656 ?
O12 V2 2.020(3) 2_656 ?
O20 C7 1.419(7) . ?
N1 C1 1.340(7) . ?
N1 C5 1.353(7) . ?
C1 C2 1.365(8) . ?
C2 C3 1.385(9) . ?
C3 C4 1.378(9) . ?
C4 C5 1.395(7) . ?
C5 C6 1.485(7) . ?
C6 C7 1.528(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
O1 Co1 O16 89.79(14) . . ?
O1 Co1 O17 90.67(13) . . ?
O1 Co1 O18 90.86(13) . . ?
O1 Co1 O19 91.09(13) . . ?
O15 Co1 O1 179.65(15) . . ?
O15 Co1 O16 90.06(15) . . ?
O15 Co1 O17 89.03(15) . . ?
O15 Co1 O18 89.30(15) . . ?
O15 Co1 O19 89.22(15) . . ?
O17 Co1 O16 93.40(14) . . ?
O17 Co1 O18 88.17(14) . . ?
O17 Co1 O19 178.14(13) . . ?
O18 Co1 O16 178.29(13) . . ?
O18 Co1 O19 91.19(13) . . ?
O19 Co1 O16 87.22(13) . . ?
V2 V1 V3 118.74(3) . . ?
V2 V1 V5 120.19(3) . 2_656 ?
V5 V1 V3 58.68(2) 2_656 . ?
O1 V1 V2 89.53(11) . . ?
O1 V1 V3 136.47(12) . . ?
O1 V1 V5 136.25(12) . 2_656 ?
O1 V1 O3 102.94(17) . . ?
O1 V1 O5 102.98(16) . . ?
O1 V1 O6 99.64(15) . . ?
O1 V1 O10 173.42(16) . . ?
O1 V1 O12 99.60(15) . 2_656 ?
O3 V1 V2 129.55(11) . . ?
O3 V1 V3 84.54(11) . . ?
O3 V1 V5 33.61(10) . 2_656 ?
O3 V1 O5 96.95(15) . . ?
O3 V1 O6 154.79(15) . . ?
O3 V1 O10 81.30(14) . . ?
O3 V1 O12 89.45(15) . 2_656 ?
O5 V1 V2 127.91(11) . . ?
O5 V1 V3 33.72(10) . . ?
O5 V1 V5 84.13(11) . 2_656 ?
O5 V1 O6 88.70(15) . . ?
O5 V1 O10 81.29(14) . . ?
O5 V1 O12 154.45(15) . 2_656 ?
O6 V1 V2 39.21(9) . . ?
O6 V1 V3 86.79(9) . . ?
O6 V1 V5 123.85(10) . 2_656 ?
O6 V1 O10 75.29(13) . . ?
O10 V1 V2 83.89(9) . . ?
O10 V1 V3 48.33(9) . . ?
O10 V1 V5 48.57(9) . 2_656 ?
O12 V1 V2 40.10(9) 2_656 . ?
O12 V1 V3 123.54(10) 2_656 . ?
O12 V1 V5 87.82(9) 2_656 2_656 ?
O12 V1 O6 75.78(14) 2_656 . ?
O12 V1 O10 75.24(14) 2_656 . ?
V1 V2 V5 120.80(3) . . ?
O2 V2 V1 90.02(13) . . ?
O2 V2 V5 136.67(13) . . ?
O2 V2 O4 101.85(17) . . ?
O2 V2 O6 100.85(17) . . ?
O2 V2 O7 103.54(17) . . ?
O2 V2 O10 174.63(16) . 2_656 ?
O2 V2 O12 99.28(17) . 2_656 ?
O4 V2 V1 128.65(10) . . ?
O4 V2 V5 82.79(10) . . ?
O4 V2 O6 154.60(15) . . ?
O4 V2 O10 80.18(14) . 2_656 ?
O4 V2 O12 88.88(14) . 2_656 ?
O6 V2 V1 40.13(9) . . ?
O6 V2 V5 88.47(10) . . ?
O6 V2 O10 76.25(13) . 2_656 ?
O6 V2 O12 76.33(14) . 2_656 ?
O7 V2 V1 131.50(11) . . ?
O7 V2 V5 33.42(10) . . ?
O7 V2 O4 94.24(15) . . ?
O7 V2 O6 91.37(15) . . ?
O7 V2 O10 81.16(13) . 2_656 ?
O7 V2 O12 155.77(15) . 2_656 ?
O10 V2 V1 84.87(9) 2_656 . ?
O10 V2 V5 48.28(9) 2_656 . ?
O12 V2 V1 39.77(10) 2_656 . ?
O12 V2 V5 123.99(10) 2_656 . ?
O12 V2 O10 75.71(13) 2_656 2_656 ?
V4 V3 V1 61.73(2) . . ?
V5 V3 V1 60.52(2) 2_656 . ?
V5 V3 V4 92.26(3) 2_656 . ?
O4 V3 V1 123.55(11) 2_656 . ?
O4 V3 V4 78.65(10) 2_656 . ?
O4 V3 V5 84.48(11) 2_656 2_656 ?
O4 V3 O5 153.73(15) 2_656 . ?
O4 V3 O10 77.94(13) 2_656 . ?
O4 V3 O11 83.36(14) 2_656 . ?
O5 V3 V1 31.83(10) . . ?
O5 V3 V4 78.12(10) . . ?
O5 V3 V5 84.34(11) . 2_656 ?
O5 V3 O10 76.75(13) . . ?
O5 V3 O11 83.00(14) . . ?
O8 V3 V1 81.41(11) . . ?
O8 V3 V4 124.96(11) . . ?
O8 V3 V5 32.70(10) . 2_656 ?
O8 V3 O4 91.71(15) . 2_656 ?
O8 V3 O5 91.60(15) . . ?
O8 V3 O10 81.97(13) . . ?
O8 V3 O11 155.80(15) . . ?
O9 V3 V1 133.23(14) . . ?
O9 V3 V4 131.04(14) . . ?
O9 V3 V5 136.69(14) . 2_656 ?
O9 V3 O4 102.92(17) . 2_656 ?
O9 V3 O5 101.53(17) . . ?
O9 V3 O8 103.99(17) . . ?
O9 V3 O10 173.90(16) . . ?
O9 V3 O11 100.20(17) . . ?
O10 V3 V1 45.62(8) . . ?
O10 V3 V4 42.99(8) . . ?
O10 V3 V5 49.28(8) . 2_656 ?
O11 V3 V1 81.69(9) . . ?
O11 V3 V4 30.84(9) . . ?
O11 V3 V5 123.10(10) . 2_656 ?
O11 V3 O10 73.83(13) . . ?
V3 V4 V5 176.20(3) . . ?
O6 V4 V3 89.40(9) . . ?
O6 V4 V5 90.13(9) . . ?
O6 V4 O10 80.41(13) . . ?
O6 V4 O10 81.94(13) . 2_656 ?
O6 V4 O12 156.72(16) . . ?
O10 V4 V3 49.07(9) . . ?
O10 V4 V3 127.33(10) 2_656 . ?
O10 V4 V5 127.14(10) . . ?
O10 V4 V5 48.87(9) 2_656 . ?
O10 V4 O10 78.28(15) 2_656 . ?
O11 V4 V3 38.34(11) . . ?
O11 V4 V5 145.45(11) . . ?
O11 V4 O6 96.75(15) . . ?
O11 V4 O10 165.64(15) . 2_656 ?
O11 V4 O10 87.40(15) . . ?
O11 V4 O12 96.84(15) . . ?
O11 V4 O13 107.14(16) . . ?
O12 V4 V3 89.62(9) . . ?
O12 V4 V5 89.32(9) . . ?
O12 V4 O10 81.42(13) . . ?
O12 V4 O10 80.22(14) . 2_656 ?
O13 V4 V3 145.48(12) . . ?
O13 V4 V5 38.31(11) . . ?
O13 V4 O6 97.12(15) . . ?
O13 V4 O10 165.45(15) . . ?
O13 V4 O10 87.19(15) . 2_656 ?
O13 V4 O12 96.81(15) . . ?
V1 V5 V2 91.93(3) 2_656 . ?
V3 V5 V1 60.81(2) 2_656 2_656 ?
V3 V5 V2 61.09(2) 2_656 . ?
V3 V5 V4 91.53(3) 2_656 . ?
V4 V5 V1 61.46(2) . 2_656 ?
V4 V5 V2 60.62(2) . . ?
O3 V5 V1 31.77(10) 2_656 2_656 ?
O3 V5 V2 123.07(10) 2_656 . ?
O3 V5 V3 85.05(10) 2_656 2_656 ?
O3 V5 V4 77.66(10) 2_656 . ?
O3 V5 O10 76.71(13) 2_656 2_656 ?
O3 V5 O13 82.32(14) 2_656 . ?
O7 V5 V1 123.89(10) . 2_656 ?
O7 V5 V2 32.28(10) . . ?
O7 V5 V3 84.73(11) . 2_656 ?
O7 V5 V4 78.30(10) . . ?
O7 V5 O3 153.54(15) . 2_656 ?
O7 V5 O10 78.13(13) . 2_656 ?
O7 V5 O13 82.66(14) . . ?
O8 V5 V1 82.02(11) 2_656 2_656 ?
O8 V5 V2 82.59(11) 2_656 . ?
O8 V5 V3 33.20(10) 2_656 2_656 ?
O8 V5 V4 124.73(11) 2_656 . ?
O8 V5 O3 92.68(15) 2_656 2_656 ?
O8 V5 O7 92.01(16) 2_656 . ?
O8 V5 O10 82.39(14) 2_656 2_656 ?
O8 V5 O13 155.46(15) 2_656 . ?
O10 V5 V1 45.76(8) 2_656 2_656 ?
O10 V5 V2 46.38(8) 2_656 . ?
O10 V5 V3 49.19(8) 2_656 2_656 ?
O10 V5 V4 42.34(8) 2_656 . ?
O13 V5 V1 81.23(9) . 2_656 ?
O13 V5 V2 80.20(9) . . ?
O13 V5 V3 122.26(9) . 2_656 ?
O13 V5 V4 30.73(9) . . ?
O13 V5 O10 73.07(13) . 2_656 ?
O14 V5 V1 132.77(13) . 2_656 ?
O14 V5 V2 135.15(13) . . ?
O14 V5 V3 137.26(14) . 2_656 ?
O14 V5 V4 131.20(14) . . ?
O14 V5 O3 101.15(16) . 2_656 ?
O14 V5 O7 102.91(17) . . ?
O14 V5 O8 104.07(17) . 2_656 ?
O14 V5 O10 173.36(16) . 2_656 ?
O14 V5 O13 100.47(16) . . ?
V1 O1 Co1 177.4(2) . . ?
V1 O3 V5 114.63(17) . 2_656 ?
V2 O4 V3 114.70(17) . 2_656 ?
V1 O5 V3 114.45(17) . . ?
V2 O6 V1 100.66(15) . . ?
V4 O6 V1 107.34(15) . . ?
V4 O6 V2 106.79(15) . . ?
V2 O7 V5 114.30(17) . . ?
V5 O8 V3 114.10(17) 2_656 . ?
V1 O10 V2 168.76(18) . 2_656 ?
V1 O10 V3 86.05(11) . . ?
V1 O10 V5 85.67(12) . 2_656 ?
V2 O10 V3 85.96(12) 2_656 . ?
V2 O10 V5 85.34(11) 2_656 2_656 ?
V3 O10 V5 81.53(12) . 2_656 ?
V4 O10 V1 94.31(13) . . ?
V4 O10 V1 94.39(13) 2_656 . ?
V4 O10 V2 93.29(13) . 2_656 ?
V4 O10 V2 92.16(12) 2_656 2_656 ?
V4 O10 V3 87.94(12) . . ?
V4 O10 V3 170.25(18) 2_656 . ?
V4 O10 V4 101.72(15) 2_656 . ?
V4 O10 V5 88.78(12) 2_656 2_656 ?
V4 O10 V5 169.46(17) . 2_656 ?
V4 O11 V3 110.83(17) . . ?
V1 O12 V2 100.13(15) 2_656 2_656 ?
V4 O12 V1 107.27(15) . 2_656 ?
V4 O12 V2 107.15(15) . 2_656 ?
V4 O13 V5 110.95(17) . . ?
C1 N1 C5 123.5(5) . . ?
N1 C1 C2 120.2(6) . . ?
C1 C2 C3 118.7(5) . . ?
C4 C3 C2 120.4(5) . . ?
C3 C4 C5 119.8(5) . . ?
N1 C5 C4 117.4(5) . . ?
N1 C5 C6 117.0(4) . . ?
C4 C5 C6 125.6(5) . . ?
C5 C6 C7 113.1(4) . . ?
O20 C7 C6 111.5(4) . . ?


####################################################################### 
# 
# 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_lukr050_c2c
_database_code_depnum_ccdc_archive 'CCDC 1909251'
loop_
_audit_author_name
_audit_author_address
'Alexander Roller'
;University of Vienna
Austria
;
_audit_update_record             
;
2019-04-10 deposited with the CCDC.	2019-10-15 downloaded from the CCDC.
;
_audit_creation_date             2019-04-10
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_chemical_name_systematic        
;
'(2-hydroxyethylpyridinium)(ammonium) 
[(tetraaqua)(bis(2-hydroxyethylpyridine))(mu-decavanadato)dicopper(II)]ate 
tetrahydrate'
;
_chemical_name_common            
;
'(2-hydroxyethylpyridinium)(ammonium) 
[(tetraaqua)(bis(2-hydroxyethylpyridine))(mu-decavanadato)dicopper(II)]ate 
tetrahydrate'
;
_chemical_formula_moiety         'C14 H26 Cu2 N2 O34 V10, 4(O), N, C7 H10 N O'
_chemical_formula_sum            'C21 H36 Cu2 N4 O39 V10'
_chemical_compound_source        crystallization
_chemical_properties_physical    paramagnetic
_chemical_formula_weight         1605.02
_exptl_crystal_recrystallization_method 'evaporation from aqueous solution'
_chemical_melting_point          ?
_exptl_crystal_description       block
_exptl_crystal_colour            'clear green'
_diffrn_ambient_temperature      100.0
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'
Cu Cu 0.3201 1.2651 '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'
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      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yn'
_chemical_absolute_configuration ?
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   27.0345(15)
_cell_length_b                   9.9170(5)
_cell_length_c                   20.5851(12)
_cell_angle_alpha                90
_cell_angle_beta                 119.341(5)
_cell_angle_gamma                90
_cell_volume                     4810.9(5)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9813
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      35.657
_cell_measurement_theta_min      2.228
_shelx_estimated_absorpt_T_max   0.575
_shelx_estimated_absorpt_T_min   0.363
_exptl_absorpt_coefficient_mu    2.824
_exptl_absorpt_correction_T_max  0.7470
_exptl_absorpt_correction_T_min  0.5052
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;  
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. 
wR2(int) was 0.1295 before and 0.0689 after correction. 
The Ratio of minimum to maximum transmission is 0.6763.
The λ/2 correction factor is Not present.
;
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    2.216
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             3160
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.22
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0619
_diffrn_reflns_av_unetI/netI     0.0160
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       44
_diffrn_reflns_limit_h_min       -44
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            343398
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         35.873
_diffrn_reflns_theta_min         2.270
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker X8 APEXII'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'sealed xray tube'
_diffrn_source_type              'Incoatec IuS'
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                9986
_reflns_number_total             11216
_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 V8.38A (?, 2016)'
_computing_data_collection       'APEX 3'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_refine_diff_density_max         0.788
_refine_diff_density_min         -0.655
_refine_diff_density_rms         0.096
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.098
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     421
_refine_ls_number_reflns         11216
_refine_ls_number_restraints     9
_refine_ls_R_factor_all          0.0293
_refine_ls_R_factor_gt           0.0244
_refine_ls_restrained_S_all      1.098
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0328P)²+6.8583P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0675
_refine_ls_wR_factor_ref         0.0705
_refine_special_details          
;
_olex2_refinement_description
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups
2. Restrained distances
 O13-H13
 0.87 with sigma of 0.01
 C7-H13
 1.909547 with sigma of 0.02
 Cu1-H13
 2.593486 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O18S) ∼ Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
4. Others
 Fixed Sof: O18S(0.5) O21S(0.33) N3(0.5) O16(0.5) H16(0.5) N2(0.5) H2A(0.5)
 C8(0.5) H8(0.5) C9(0.5) H9(0.5) C10(0.5) H10(0.5) C11(0.5) H11(0.5) C12(0.5)
 C13(0.5) H13A(0.5) H13B(0.5) C14(0.5) H14C(0.5) H14D(0.5) O17S(0.5) O19S(0.5)
 O20S(0.17)
5.a Rotating group:
 O14(H14A,H14B), O15(H15A,H15B)
5.b Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C7(H7A,H7B), C13(H13A,H13B), C14(H14C,H14D)
5.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), N2(H2A), C8(H8), C9(H9), C10(H10), C11(H11)
5.d Idealised tetrahedral OH refined as rotating group:
 O16(H16)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_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
Cu1 Cu 0.59892(2) 0.96800(2) 0.65108(2) 0.01379(3) Uani 1 1 d D . . . .
V1 V 0.50943(2) 0.62045(2) 0.45294(2) 0.01009(3) Uani 1 1 d . . . . .
V2 V 0.39487(2) 0.52931(2) 0.31837(2) 0.01365(4) Uani 1 1 d . . . . .
V3 V 0.37866(2) 0.30990(2) 0.40912(2) 0.01135(4) Uani 1 1 d . . . . .
V4 V 0.39686(2) 0.59982(2) 0.46846(2) 0.01348(4) Uani 1 1 d . . . . .
V5 V 0.50982(2) 0.68412(2) 0.60340(2) 0.00995(3) Uani 1 1 d . . . . .
O1 O 0.54927(3) 0.54004(7) 0.55786(4) 0.00919(12) Uani 1 1 d . . . . .
O2 O 0.46201(4) 0.65657(9) 0.36186(5) 0.01648(16) Uani 1 1 d . . . . .
O3 O 0.56149(4) 0.73355(9) 0.47979(5) 0.01595(15) Uani 1 1 d . . . . .
O4 O 0.36947(4) 0.64140(9) 0.37038(5) 0.01731(16) Uani 1 1 d . . . . .
O5 O 0.35605(4) 0.44499(10) 0.45034(5) 0.01666(16) Uani 1 1 d . . . . .
O6 O 0.35073(4) 0.39024(8) 0.31978(5) 0.01377(14) Uani 1 1 d . . . . .
O7 O 0.36066(5) 0.58921(10) 0.23564(5) 0.0246(2) Uani 1 1 d . . . . .
O8 O 0.33445(5) 0.19023(11) 0.39586(6) 0.0232(2) Uani 1 1 d . . . . .
O9 O 0.36407(4) 0.70481(11) 0.49368(6) 0.0246(2) Uani 1 1 d . . . . .
O10 O 0.47714(4) 0.78748(10) 0.62910(6) 0.01959(18) Uani 1 1 d . . . . .
O11 O 0.44579(4) 0.41104(9) 0.31250(5) 0.01345(14) Uani 1 1 d . . . . .
O12 O 0.56763(3) 0.79063(8) 0.60876(5) 0.01089(13) Uani 1 1 d . . . . .
O13 O 0.65537(4) 1.11534(9) 0.67795(6) 0.01974(17) Uani 1 1 d D . . . .
H13 H 0.6459(7) 1.1981(10) 0.6622(11) 0.030 Uiso 1 1 d DR . . . .
O14 O 0.54154(4) 1.08413(10) 0.68407(6) 0.02127(18) Uani 1 1 d . . . . .
H14A H 0.506681 1.056637 0.658154 0.032 Uiso 1 1 d GR . . . .
H14B H 0.539700 1.168458 0.671823 0.032 Uiso 1 1 d GR . . . .
O15 O 0.55774(5) 1.03996(9) 0.54810(6) 0.0227(2) Uani 1 1 d . . . . .
H15A H 0.556992 1.117359 0.541248 0.034 Uiso 1 1 d GR . . . .
H15B H 0.577275 1.026183 0.525998 0.034 Uiso 1 1 d GR . . . .
O18 O 0.46618(4) 0.71084(8) 0.49277(5) 0.01250(13) Uani 1 1 d . . . . .
O2AA O 0.54489(4) 0.47077(8) 0.43327(5) 0.01241(13) Uani 1 1 d . . . . .
N1 N 0.63950(4) 0.89481(10) 0.75370(6) 0.01439(16) Uani 1 1 d . . . . .
C1 C 0.60852(5) 0.83569(12) 0.78066(7) 0.01556(19) Uani 1 1 d . . . . .
H1 H 0.568412 0.833661 0.750334 0.019 Uiso 1 1 calc R . . . .
C2 C 0.63256(6) 0.77788(16) 0.85052(7) 0.0213(2) Uani 1 1 d . . . . .
H2 H 0.609729 0.734836 0.867712 0.026 Uiso 1 1 calc R . . . .
C3 C 0.69099(6) 0.7845(2) 0.89485(8) 0.0326(4) Uani 1 1 d . . . . .
H3 H 0.708890 0.746376 0.943421 0.039 Uiso 1 1 calc R . . . .
C4 C 0.72316(6) 0.8469(2) 0.86792(8) 0.0287(3) Uani 1 1 d . . . . .
H4 H 0.763229 0.852409 0.898052 0.034 Uiso 1 1 calc R . . . .
C5 C 0.69646(5) 0.90159(13) 0.79646(7) 0.0169(2) Uani 1 1 d . . . . .
C6 C 0.72968(5) 0.96969(13) 0.76516(8) 0.0200(2) Uani 1 1 d . . . . .
H6A H 0.725317 0.917648 0.721619 0.024 Uiso 1 1 calc R . . . .
H6B H 0.770390 0.968748 0.803213 0.024 Uiso 1 1 calc R . . . .
C7 C 0.71143(6) 1.11444(14) 0.74128(9) 0.0260(3) Uani 1 1 d D . . . .
H7A H 0.711700 1.165390 0.782809 0.031 Uiso 1 1 calc R . . . .
H7B H 0.738271 1.158409 0.728226 0.031 Uiso 1 1 calc R . . . .
O18S O 0.43245(13) 0.1482(3) 0.67465(17) 0.0250(5) Uani 0.5 1 d . U P A -2
O21S O 0.6232(2) 0.0081(4) 0.4826(2) 0.0254(8) Uani 0.33 1 d . . P B -2
N3 N 0.43600(12) 0.3775(3) 0.66977(14) 0.0218(4) Uani 0.5 1 d . . P C -2
O16 O 0.34241(11) 0.4168(3) 0.56975(13) 0.0310(5) Uani 0.5 1 d . . P D -1
H16 H 0.342510 0.412656 0.529049 0.047 Uiso 0.5 1 calc GR . P D -1
N2 N 0.33119(10) 0.1042(2) 0.54664(13) 0.0201(4) Uani 0.5 1 d . . P D -1
H2A H 0.361103 0.135954 0.586394 0.024 Uiso 0.5 1 calc R . P D -1
C8 C 0.3389(3) 0.0072(8) 0.5075(4) 0.0241(9) Uani 0.5 1 d . . P D -1
H8 H 0.375591 -0.030411 0.524714 0.029 Uiso 0.5 1 calc R . P D -1
C9 C 0.29356(15) -0.0383(3) 0.44210(16) 0.0248(5) Uani 0.5 1 d . . P D -1
H9 H 0.298800 -0.104429 0.412607 0.030 Uiso 0.5 1 calc R . P D -1
C10 C 0.24063(15) 0.0138(3) 0.42044(18) 0.0296(6) Uani 0.5 1 d . . P D -1
H10 H 0.208839 -0.016139 0.375548 0.036 Uiso 0.5 1 calc R . P D -1
C11 C 0.23359(17) 0.1106(4) 0.4643(2) 0.0292(8) Uani 0.5 1 d . . P D -1
H11 H 0.196873 0.145161 0.449957 0.035 Uiso 0.5 1 calc R . P D -1
C12 C 0.27978(12) 0.1560(3) 0.52830(16) 0.0212(4) Uani 0.5 1 d . . P D -1
C13 C 0.27680(14) 0.2620(3) 0.57833(18) 0.0256(5) Uani 0.5 1 d . . P D -1
H13A H 0.306055 0.243395 0.630486 0.031 Uiso 0.5 1 calc R . P D -1
H13B H 0.239198 0.258044 0.575494 0.031 Uiso 0.5 1 calc R . P D -1
C14 C 0.28606(19) 0.4031(4) 0.5566(2) 0.0261(6) Uani 0.5 1 d . . P D -1
H14C H 0.259056 0.419180 0.503203 0.031 Uiso 0.5 1 calc R . P D -1
H14D H 0.278794 0.471218 0.586090 0.031 Uiso 0.5 1 calc R . P D -1
O17S O 0.45238(12) 0.4481(3) 0.69638(14) 0.0303(5) Uani 0.5 1 d . . P E -1
O19S O 0.56834(14) 0.8985(3) 0.33830(16) 0.0234(5) Uani 0.5 1 d . . P F -1
O20S O 0.6446(7) 0.0004(19) 0.4810(12) 0.040(5) Uani 0.17 1 d . . P G -1


_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
Cu1 O12 1.9612(8) . ?
Cu1 O13 1.9857(9) . ?
Cu1 O14 2.2860(10) . ?
Cu1 O15 1.9824(10) . ?
Cu1 N1 1.9802(11) . ?
V1 V2 3.1105(4) . ?
V1 V3 3.0453(4) 5_666 ?
V1 O1 2.1807(8) 5_666 ?
V1 O1 2.0448(8) . ?
V1 O2 1.7122(9) . ?
V1 O3 1.6678(9) . ?
V1 O18 1.9451(9) . ?
V1 O2AA 1.9147(8) . ?
V2 V3 3.0362(3) . ?
V2 V5 3.1059(3) 5_666 ?
V2 O1 2.3397(8) 5_666 ?
V2 O2 2.0240(9) . ?
V2 O4 1.8905(10) . ?
V2 O6 1.8331(9) . ?
V2 O7 1.6015(10) . ?
V2 O11 1.8570(9) . ?
V3 V4 3.0678(3) . ?
V3 O1 2.2749(8) 5_666 ?
V3 O3 2.0993(10) 5_666 ?
V3 O5 1.8430(9) . ?
V3 O6 1.7963(9) . ?
V3 O8 1.6099(10) . ?
V3 O12 1.9394(8) 5_666 ?
V4 V5 3.0704(4) . ?
V4 O1 2.2609(8) 5_666 ?
V4 O4 1.8246(10) . ?
V4 O5 1.8196(9) . ?
V4 O9 1.6096(9) . ?
V4 O18 2.0137(9) . ?
V4 O2AA 1.9849(9) 5_666 ?
V5 O1 2.2444(8) . ?
V5 O10 1.6028(9) . ?
V5 O11 1.8143(9) 5_666 ?
V5 O12 1.8444(8) . ?
V5 O18 2.0038(9) . ?
V5 O2AA 2.0057(8) 5_666 ?
O13 C7 1.4353(17) . ?
N1 C1 1.3449(17) . ?
N1 C5 1.3499(15) . ?
C1 C2 1.3795(19) . ?
C2 C3 1.385(2) . ?
C3 C4 1.386(2) . ?
C4 C5 1.392(2) . ?
C5 C6 1.4982(19) . ?
C6 C7 1.5193(19) . ?
O16 C14 1.417(5) . ?
N2 C8 1.335(9) . ?
N2 C12 1.351(4) . ?
C8 C9 1.380(8) . ?
C9 C10 1.374(5) . ?
C10 C11 1.394(6) . ?
C11 C12 1.373(5) . ?
C12 C13 1.501(4) . ?
C12 C13 2.128(4) 7_556 ?
C13 C14 1.526(5) . ?

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 Cu1 O13 152.75(4) . . ?
O12 Cu1 O14 112.09(4) . . ?
O12 Cu1 O15 87.35(4) . . ?
O12 Cu1 N1 92.18(4) . . ?
O13 Cu1 O14 95.01(4) . . ?
O15 Cu1 O13 89.15(4) . . ?
O15 Cu1 O14 91.67(4) . . ?
N1 Cu1 O13 91.38(4) . . ?
N1 Cu1 O14 88.26(4) . . ?
N1 Cu1 O15 179.47(5) . . ?
V3 V1 V2 175.590(8) 5_666 . ?
O1 V1 V2 48.69(2) 5_666 . ?
O1 V1 V2 127.34(2) . . ?
O1 V1 V3 48.33(2) . 5_666 ?
O1 V1 V3 126.97(2) 5_666 5_666 ?
O1 V1 O1 78.66(3) . 5_666 ?
O2 V1 V2 36.97(3) . . ?
O2 V1 V3 147.39(3) . 5_666 ?
O2 V1 O1 164.25(4) . . ?
O2 V1 O1 85.64(4) . 5_666 ?
O2 V1 O18 94.75(4) . . ?
O2 V1 O2AA 96.58(4) . . ?
O3 V1 V2 143.21(3) . . ?
O3 V1 V3 41.15(3) . 5_666 ?
O3 V1 O1 168.05(4) . 5_666 ?
O3 V1 O1 89.43(4) . . ?
O3 V1 O2 106.24(4) . . ?
O3 V1 O18 97.72(4) . . ?
O3 V1 O2AA 99.38(4) . . ?
O18 V1 V2 88.13(3) . . ?
O18 V1 V3 91.73(3) . 5_666 ?
O18 V1 O1 79.72(3) . 5_666 ?
O18 V1 O1 81.29(3) . . ?
O2AA V1 V2 88.26(3) . . ?
O2AA V1 V3 90.08(3) . 5_666 ?
O2AA V1 O1 82.06(3) . . ?
O2AA V1 O1 80.06(3) . 5_666 ?
O2AA V1 O18 155.93(4) . . ?
V3 V2 V1 92.363(8) . . ?
V3 V2 V5 61.693(7) . 5_666 ?
V5 V2 V1 61.652(8) 5_666 . ?
O1 V2 V1 44.429(19) 5_666 . ?
O1 V2 V3 47.942(19) 5_666 . ?
O1 V2 V5 46.069(19) 5_666 5_666 ?
O2 V2 V1 30.58(2) . . ?
O2 V2 V3 122.91(3) . . ?
O2 V2 V5 81.91(3) . 5_666 ?
O2 V2 O1 75.00(3) . 5_666 ?
O4 V2 V1 78.71(3) . . ?
O4 V2 V3 82.59(3) . . ?
O4 V2 V5 123.12(3) . 5_666 ?
O4 V2 O1 77.05(3) . 5_666 ?
O4 V2 O2 83.03(4) . . ?
O6 V2 V1 125.19(3) . . ?
O6 V2 V3 32.84(3) . . ?
O6 V2 V5 81.96(3) . 5_666 ?
O6 V2 O1 80.76(3) . 5_666 ?
O6 V2 O2 155.75(4) . . ?
O6 V2 O4 90.78(4) . . ?
O6 V2 O11 92.00(4) . . ?
O7 V2 V1 130.05(4) . . ?
O7 V2 V3 137.55(4) . . ?
O7 V2 V5 134.77(5) . 5_666 ?
O7 V2 O1 174.41(5) . 5_666 ?
O7 V2 O2 99.47(5) . . ?
O7 V2 O4 101.73(5) . . ?
O7 V2 O6 104.75(5) . . ?
O7 V2 O11 103.03(5) . . ?
O11 V2 V1 78.17(3) . . ?
O11 V2 V3 85.55(3) . . ?
O11 V2 V5 31.81(3) . 5_666 ?
O11 V2 O1 77.39(3) . 5_666 ?
O11 V2 O2 83.68(4) . . ?
O11 V2 O4 153.48(4) . . ?
V1 V3 V4 61.571(6) 5_666 . ?
V2 V3 V1 91.963(8) . 5_666 ?
V2 V3 V4 61.965(7) . . ?
O1 V3 V1 42.18(2) 5_666 5_666 ?
O1 V3 V2 49.78(2) 5_666 . ?
O1 V3 V4 47.25(2) 5_666 . ?
O3 V3 V1 31.52(2) 5_666 5_666 ?
O3 V3 V2 123.42(2) 5_666 . ?
O3 V3 V4 82.59(3) 5_666 . ?
O3 V3 O1 73.66(3) 5_666 5_666 ?
O5 V3 V1 78.92(3) . 5_666 ?
O5 V3 V2 86.72(3) . . ?
O5 V3 V4 32.87(3) . . ?
O5 V3 O1 79.38(3) . 5_666 ?
O5 V3 O3 84.27(4) . 5_666 ?
O5 V3 O12 155.37(4) . 5_666 ?
O6 V3 V1 125.54(3) . 5_666 ?
O6 V3 V2 33.60(3) . . ?
O6 V3 V4 84.08(3) . . ?
O6 V3 O1 83.37(3) . 5_666 ?
O6 V3 O3 156.82(4) . 5_666 ?
O6 V3 O5 94.66(4) . . ?
O6 V3 O12 90.68(4) . 5_666 ?
O8 V3 V1 129.87(4) . 5_666 ?
O8 V3 V2 137.99(4) . . ?
O8 V3 V4 136.00(4) . . ?
O8 V3 O1 171.46(5) . 5_666 ?
O8 V3 O3 98.35(5) . 5_666 ?
O8 V3 O5 103.16(5) . . ?
O8 V3 O6 104.41(5) . . ?
O8 V3 O12 98.72(5) . 5_666 ?
O12 V3 V1 78.43(3) 5_666 5_666 ?
O12 V3 V2 84.52(3) 5_666 . ?
O12 V3 V4 124.63(2) 5_666 . ?
O12 V3 O1 77.39(3) 5_666 5_666 ?
O12 V3 O3 81.49(4) 5_666 5_666 ?
V3 V4 V5 120.650(8) . . ?
O1 V4 V3 47.63(2) 5_666 . ?
O1 V4 V5 84.95(2) 5_666 . ?
O4 V4 V3 82.66(3) . . ?
O4 V4 V5 128.61(3) . . ?
O4 V4 O1 80.41(4) . 5_666 ?
O4 V4 O18 88.58(4) . . ?
O4 V4 O2AA 153.70(4) . 5_666 ?
O5 V4 V3 33.35(3) . . ?
O5 V4 V5 130.51(3) . . ?
O5 V4 O1 80.23(3) . 5_666 ?
O5 V4 O4 95.01(4) . . ?
O5 V4 O18 155.41(4) . . ?
O5 V4 O2AA 90.56(4) . 5_666 ?
O9 V4 V3 136.75(4) . . ?
O9 V4 V5 89.59(4) . . ?
O9 V4 O1 174.52(4) . 5_666 ?
O9 V4 O4 102.81(5) . . ?
O9 V4 O5 103.73(5) . . ?
O9 V4 O18 99.13(5) . . ?
O9 V4 O2AA 100.76(5) . 5_666 ?
O18 V4 V3 124.03(2) . . ?
O18 V4 V5 40.04(2) . . ?
O18 V4 O1 76.39(3) . 5_666 ?
O2AA V4 V3 88.14(2) 5_666 . ?
O2AA V4 V5 39.95(2) 5_666 . ?
O2AA V4 O1 75.25(3) 5_666 5_666 ?
O2AA V4 O18 76.27(3) 5_666 . ?
V4 V5 V2 119.224(8) . 5_666 ?
O1 V5 V2 48.66(2) . 5_666 ?
O1 V5 V4 85.08(2) . . ?
O10 V5 V2 135.73(4) . 5_666 ?
O10 V5 V4 90.46(4) . . ?
O10 V5 O1 175.23(4) . . ?
O10 V5 O11 103.38(5) . 5_666 ?
O10 V5 O12 101.66(4) . . ?
O10 V5 O18 100.24(5) . . ?
O10 V5 O2AA 100.95(4) . 5_666 ?
O11 V5 V2 32.65(3) 5_666 5_666 ?
O11 V5 V4 128.41(3) 5_666 . ?
O11 V5 O1 80.79(3) 5_666 . ?
O11 V5 O12 95.50(4) 5_666 . ?
O11 V5 O18 154.03(4) 5_666 . ?
O11 V5 O2AA 88.96(4) 5_666 5_666 ?
O12 V5 V2 84.02(3) . 5_666 ?
O12 V5 V4 130.39(3) . . ?
O12 V5 O1 80.06(3) . . ?
O12 V5 O18 90.12(4) . . ?
O12 V5 O2AA 155.24(4) . 5_666 ?
O18 V5 V2 123.80(2) . 5_666 ?
O18 V5 V4 40.28(3) . . ?
O18 V5 O1 75.24(3) . . ?
O18 V5 O2AA 76.03(4) . 5_666 ?
O2AA V5 V2 86.83(3) 5_666 5_666 ?
O2AA V5 V4 39.45(3) 5_666 . ?
O2AA V5 O1 76.64(3) 5_666 . ?
V1 O1 V1 101.35(3) . 5_666 ?
V1 O1 V2 86.88(3) 5_666 5_666 ?
V1 O1 V2 171.76(4) . 5_666 ?
V1 O1 V3 169.08(4) 5_666 5_666 ?
V1 O1 V3 89.49(3) . 5_666 ?
V1 O1 V4 93.08(3) . 5_666 ?
V1 O1 V4 92.86(3) 5_666 5_666 ?
V1 O1 V5 92.08(3) 5_666 . ?
V1 O1 V5 94.64(3) . . ?
V3 O1 V2 82.27(3) 5_666 5_666 ?
V4 O1 V2 86.14(3) 5_666 5_666 ?
V4 O1 V3 85.12(3) 5_666 5_666 ?
V5 O1 V2 85.27(3) . 5_666 ?
V5 O1 V3 88.36(3) . 5_666 ?
V5 O1 V4 169.85(4) . 5_666 ?
V1 O2 V2 112.46(4) . . ?
V1 O3 V3 107.32(4) . 5_666 ?
V4 O4 V2 115.51(5) . . ?
V4 O5 V3 113.77(5) . . ?
V3 O6 V2 113.55(5) . . ?
V5 O11 V2 115.55(4) 5_666 . ?
V3 O12 Cu1 110.21(4) 5_666 . ?
V5 O12 Cu1 135.12(5) . . ?
V5 O12 V3 112.68(4) . 5_666 ?
C7 O13 Cu1 125.01(8) . . ?
V1 O18 V4 108.77(4) . . ?
V1 O18 V5 106.10(4) . . ?
V5 O18 V4 99.68(4) . . ?
V1 O2AA V4 106.70(4) . 5_666 ?
V1 O2AA V5 108.67(4) . 5_666 ?
V4 O2AA V5 100.60(4) 5_666 5_666 ?
C1 N1 Cu1 117.93(8) . . ?
C1 N1 C5 119.65(11) . . ?
C5 N1 Cu1 122.42(9) . . ?
N1 C1 C2 122.74(11) . . ?
C1 C2 C3 118.01(13) . . ?
C2 C3 C4 119.62(14) . . ?
C3 C4 C5 119.64(13) . . ?
N1 C5 C4 120.32(12) . . ?
N1 C5 C6 118.34(11) . . ?
C4 C5 C6 121.34(11) . . ?
C5 C6 C7 113.39(12) . . ?
O13 C7 C6 109.32(11) . . ?
C8 N2 C12 123.3(3) . . ?
N2 C8 C9 119.8(5) . . ?
C10 C9 C8 118.7(4) . . ?
C9 C10 C11 120.0(3) . . ?
C12 C11 C10 119.9(4) . . ?
N2 C12 C11 118.1(3) . . ?
N2 C12 C13 123.7(2) . 7_556 ?
N2 C12 C13 117.9(3) . . ?
C11 C12 C13 43.9(2) . 7_556 ?
C11 C12 C13 123.9(3) . . ?
C13 C12 C13 100.8(2) . 7_556 ?
C12 C13 C14 111.7(3) . . ?
O16 C14 C13 110.3(3) . . ?


