# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2020

####################################################################### 
# 
# 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_160922b
_database_code_depnum_ccdc_archive 'CCDC 2009806'
_audit_update_record             
;
2020-06-15 deposited with the CCDC.	2020-07-13 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C24 H39 Cu N8 O11 V4'
_chemical_formula_weight         882.93

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'
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'
Cu Cu 0.3201 1.2651 '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      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_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, -z'

_cell_length_a                   11.2508(8)
_cell_length_b                   11.9199(9)
_cell_length_c                   15.2277(14)
_cell_angle_alpha                105.431(2)
_cell_angle_beta                 94.1680(10)
_cell_angle_gamma                108.872(2)
_cell_volume                     1834.3(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    1024
_cell_measurement_theta_min      2.688
_cell_measurement_theta_max      23.925

_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.599
_exptl_crystal_F_000             896
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.220
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.180
_exptl_absorpt_coefficient_mu    1.613
_shelx_estimated_absorpt_T_min   0.718
_shelx_estimated_absorpt_T_max   0.760
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7180
_exptl_absorpt_correction_T_max  0.7600
_exptl_absorpt_process_details   sadabs
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      298(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            9366
_diffrn_reflns_av_unetI/netI     0.0576
_diffrn_reflns_av_R_equivalents  0.0240
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         2.458
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_full        24.999
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measured_fraction_theta_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_point_group_measured_fraction_full 0.984
_reflns_number_total             6357
_reflns_number_gt                4308
_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       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1147P)²] 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         6357
_refine_ls_number_parameters     443
_refine_ls_number_restraints     993
_refine_ls_R_factor_all          0.0878
_refine_ls_R_factor_gt           0.0611
_refine_ls_wR_factor_ref         0.1938
_refine_ls_wR_factor_gt          0.1762
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_restrained_S_all      1.076
_refine_ls_shift/su_max          0.012
_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
Cu1 Cu 0.500000 0.500000 1.000000 0.0362(3) Uani 1 2 d S U P . .
Cu2 Cu 0.000000 1.000000 0.500000 0.0450(3) Uani 1 2 d S U P . .
V4 V 0.27925(9) 0.85503(9) 0.45641(6) 0.0381(3) Uani 1 1 d . U . . .
V2 V 0.57158(10) 0.94392(9) 0.85403(6) 0.0387(3) Uani 1 1 d . U . . .
V1 V 0.40076(10) 0.77827(9) 0.98192(7) 0.0435(3) Uani 1 1 d . U . . .
V3 V 0.49777(11) 0.98968(12) 0.65265(7) 0.0524(3) Uani 1 1 d . U . . .
N2 N 0.8872(5) 0.6425(5) 1.1156(3) 0.0521(13) Uani 1 1 d . U . . .
N1 N 0.6792(5) 0.5912(4) 1.0755(3) 0.0404(11) Uani 1 1 d . U . . .
N4 N 0.3361(5) 0.4419(5) 1.2288(3) 0.0465(12) Uani 1 1 d . U . . .
N3 N 0.4267(5) 0.5050(4) 1.1187(3) 0.0393(11) Uani 1 1 d . U . . .
N5 N -0.0054(5) 1.0182(5) 0.3721(3) 0.0498(12) Uani 1 1 d . U . . .
N7 N -0.1278(5) 0.8238(5) 0.4490(3) 0.0500(12) Uani 1 1 d . U . . .
N8 N -0.2055(7) 0.6213(5) 0.3988(4) 0.0701(16) Uani 1 1 d . U . . .
O3 O 0.4816(5) 0.6983(4) 1.0090(3) 0.0574(11) Uani 1 1 d . U . . .
C9 C 0.3581(6) 0.5679(6) 1.2498(4) 0.0450(14) Uani 1 1 d . U . . .
H9 H 0.339067 0.617358 1.301075 0.054 Uiso 1 1 calc R U . . .
O6 O 0.5361(6) 0.9220(5) 0.7332(3) 0.0764(15) Uani 1 1 d . U . . .
O2 O 0.4561(5) 0.8345(4) 0.8861(3) 0.0698(14) Uani 1 1 d . U . . .
C8 C 0.4126(6) 0.6050(6) 1.1815(4) 0.0437(13) Uani 1 1 d . U . . .
H8 H 0.436918 0.685561 1.177466 0.052 Uiso 1 1 calc R U . . .
O8 O 0.3900(5) 0.8801(5) 0.5584(3) 0.0754(15) Uani 1 1 d . U . . .
O9 O 0.2044(5) 0.7074(4) 0.4106(3) 0.0675(13) Uani 1 1 d . U . . .
O5 O 0.5824(6) 1.0881(4) 0.9191(3) 0.0785(15) Uani 1 1 d . U . . .
C7 C 0.3792(6) 0.4096(6) 1.1496(4) 0.0445(14) Uani 1 1 d . U . . .
H7 H 0.375999 0.329360 1.120029 0.053 Uiso 1 1 calc R U . . .
C1 C 0.7816(6) 0.5742(5) 1.0496(4) 0.0457(14) Uani 1 1 d . U . . .
H1 H 0.782417 0.521421 0.992468 0.055 Uiso 1 1 calc R U . . .
C19 C -0.1015(7) 0.7223(6) 0.4304(5) 0.0588(16) Uani 1 1 d . U . . .
H19 H -0.019339 0.720893 0.438412 0.071 Uiso 1 1 calc R U . . .
O11 O 0.1750(5) 0.9204(5) 0.4808(3) 0.0686(13) Uani 1 1 d . U . . .
O4 O 0.7041(5) 0.9249(6) 0.8713(4) 0.0845(17) Uani 1 1 d . U . . .
O10 O 0.3702(5) 0.9203(6) 0.3765(4) 0.0923(18) Uani 1 1 d . U . . .
C18 C -0.2575(7) 0.7819(7) 0.4261(5) 0.0596(16) Uani 1 1 d . U . . .
H18 H -0.305739 0.832928 0.431961 0.071 Uiso 1 1 calc R U . . .
C4 C 1.0185(7) 0.6363(7) 1.1134(5) 0.070(2) Uani 1 1 d . U . . .
H4 H 1.026403 0.607230 1.048267 0.084 Uiso 1 1 calc R U . . .
C24 C 0.2795(7) 0.3590(7) 1.2828(5) 0.0593(17) Uani 1 1 d . U . . .
H24 H 0.253372 0.273469 1.241390 0.071 Uiso 1 1 calc R U . . .
N6 N -0.0693(6) 1.0257(7) 0.2363(4) 0.0719(17) Uani 1 1 d . U . . .
C13 C 0.0938(6) 1.0348(6) 0.3234(4) 0.0519(15) Uani 1 1 d . U . . .
H13 H 0.176313 1.042612 0.345367 0.062 Uiso 1 1 calc R U . . .
C14 C 0.0536(7) 1.0378(7) 0.2403(5) 0.0616(17) Uani 1 1 d . U . . .
H14 H 0.101610 1.046630 0.193749 0.074 Uiso 1 1 calc R U . . .
C2 C 0.7219(7) 0.6747(6) 1.1641(4) 0.0544(16) Uani 1 1 d . U . . .
H2 H 0.669853 0.704739 1.201158 0.065 Uiso 1 1 calc R U . . .
C3 C 0.8465(7) 0.7062(6) 1.1891(5) 0.0588(17) Uani 1 1 d . U . . .
H3 H 0.896321 0.760568 1.245177 0.071 Uiso 1 1 calc R U . . .
O7 O 0.4256(6) 1.0826(6) 0.7020(5) 0.104(2) Uani 1 1 d . U . . .
C10 C 0.3755(11) 0.3712(11) 1.3605(7) 0.125(4) Uani 1 1 d . U . . .
H10A H 0.447853 0.356790 1.336786 0.187 Uiso 1 1 calc R U . . .
H10B H 0.338385 0.311054 1.391280 0.187 Uiso 1 1 calc R U . . .
H10C H 0.402387 0.453512 1.403540 0.187 Uiso 1 1 calc R U . . .
C12 C -0.1014(7) 1.0143(8) 0.3174(5) 0.0679(18) Uani 1 1 d . U . . .
H12 H -0.181963 1.004851 0.332402 0.082 Uiso 1 1 calc R U . . .
C20 C -0.3053(7) 0.6585(7) 0.3943(5) 0.0663(19) Uani 1 1 d . U . . .
H20 H -0.390652 0.608120 0.373195 0.080 Uiso 1 1 calc R U . . .
C5 C 1.1213(8) 0.7561(9) 1.1558(7) 0.102(3) Uani 1 1 d . U . . .
H5A H 1.116024 0.812882 1.122580 0.152 Uiso 1 1 calc R U . . .
H5B H 1.201992 0.745054 1.153739 0.152 Uiso 1 1 calc R U . . .
H5C H 1.113549 0.789149 1.218982 0.152 Uiso 1 1 calc R U . . .
C11 C 0.1565(9) 0.3791(9) 1.3111(7) 0.102(3) Uani 1 1 d . U . . .
H11A H 0.178600 0.460352 1.354917 0.153 Uiso 1 1 calc R U . . .
H11B H 0.113360 0.316958 1.338565 0.153 Uiso 1 1 calc R U . . .
H11C H 0.101482 0.372448 1.257250 0.153 Uiso 1 1 calc R U . . .
C15 C -0.1755(13) 1.0074(12) 0.1530(7) 0.128(3) Uani 1 1 d D U . . .
H15 H -0.263426 0.975002 0.163356 0.153 Uiso 1 1 calc R U . . .
C23 C -0.2705(12) 0.4225(10) 0.2756(7) 0.140(4) Uani 1 1 d . U . . .
H23A H -0.215301 0.461936 0.238837 0.209 Uiso 1 1 calc R U . . .
H23B H -0.353268 0.427223 0.262611 0.209 Uiso 1 1 calc R U . . .
H23C H -0.278063 0.336770 0.260919 0.209 Uiso 1 1 calc R U . . .
C6 C 1.0335(9) 0.5375(9) 1.1598(6) 0.095(3) Uani 1 1 d . U . . .
H6A H 1.112648 0.525578 1.150486 0.142 Uiso 1 1 calc R U . . .
H6B H 0.963982 0.459866 1.132327 0.142 Uiso 1 1 calc R U . . .
H6C H 1.033186 0.566675 1.224873 0.142 Uiso 1 1 calc R U . . .
C21 C -0.2187(11) 0.4841(9) 0.3708(8) 0.122(3) Uani 1 1 d D U . . .
H21 H -0.295418 0.451812 0.396516 0.147 Uiso 1 1 calc R U . . .
C22 C -0.1285(15) 0.4597(12) 0.4306(10) 0.187(6) Uani 1 1 d D U . . .
H22A H -0.097676 0.396294 0.406712 0.224 Uiso 1 1 calc R U . . .
H22B H -0.101993 0.507513 0.492465 0.224 Uiso 1 1 calc R U . . .
O1 O 0.2528(5) 0.6900(5) 0.9510(4) 0.0809(15) Uani 1 1 d . U . . .
C17 C -0.1486(15) 0.9327(15) 0.0689(8) 0.173(5) Uani 1 1 d . U . . .
H17A H -0.113187 0.984934 0.031969 0.260 Uiso 1 1 calc R U . . .
H17B H -0.226193 0.867506 0.034227 0.260 Uiso 1 1 calc R U . . .
H17C H -0.088638 0.896797 0.085573 0.260 Uiso 1 1 calc R U . . .
C16 C -0.1327(18) 1.1384(13) 0.1500(12) 0.235(7) Uani 1 1 d D U . . .
H16A H -0.058390 1.154818 0.121247 0.353 Uiso 1 1 calc R U . . .
H16B H -0.112361 1.194582 0.211869 0.353 Uiso 1 1 calc R U . . .
H16C H -0.199688 1.150171 0.115030 0.353 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
Cu1 N3 2.035(4) 2_667 ?
Cu1 N3 2.035(4) . ?
Cu1 N1 2.037(5) . ?
Cu1 N1 2.037(5) 2_667 ?
Cu1 O3 2.407(4) . ?
Cu1 O3 2.407(4) 2_667 ?
Cu2 N5 2.016(5) 2_576 ?
Cu2 N5 2.016(5) . ?
Cu2 N7 2.024(5) . ?
Cu2 N7 2.024(5) 2_576 ?
Cu2 O11 2.451(5) . ?
V4 O9 1.611(5) . ?
V4 O11 1.619(5) . ?
V4 O8 1.813(5) . ?
V4 O10 1.818(5) . ?
V2 O4 1.593(5) . ?
V2 O5 1.701(5) . ?
V2 O2 1.722(5) . ?
V2 O6 1.783(4) . ?
V1 O1 1.609(5) . ?
V1 O3 1.619(4) . ?
V1 O5 1.825(5) 2_677 ?
V1 O2 1.829(4) . ?
V3 O7 1.636(6) . ?
V3 O10 1.695(5) 2_676 ?
V3 O8 1.720(5) . ?
V3 O6 1.737(4) . ?
N2 C1 1.361(8) . ?
N2 C3 1.373(8) . ?
N2 C4 1.505(9) . ?
N1 C1 1.304(7) . ?
N1 C2 1.387(7) . ?
N4 C7 1.341(7) . ?
N4 C9 1.382(8) . ?
N4 C24 1.470(7) . ?
N3 C7 1.314(7) . ?
N3 C8 1.378(7) . ?
N5 C12 1.296(8) . ?
N5 C13 1.374(8) . ?
N7 C19 1.301(8) . ?
N7 C18 1.364(8) . ?
N8 C19 1.322(9) . ?
N8 C20 1.337(9) . ?
N8 C21 1.530(11) . ?
C9 C8 1.347(8) . ?
C9 H9 0.9300 . ?
C8 H8 0.9300 . ?
C7 H7 0.9300 . ?
C1 H1 0.9300 . ?
C19 H19 0.9300 . ?
C18 C20 1.327(10) . ?
C18 H18 0.9300 . ?
C4 C5 1.458(11) . ?
C4 C6 1.572(11) . ?
C4 H4 0.9800 . ?
C24 C10 1.486(12) . ?
C24 C11 1.550(10) . ?
C24 H24 0.9800 . ?
N6 C14 1.338(9) . ?
N6 C12 1.340(9) . ?
N6 C15 1.596(12) . ?
C13 C14 1.326(9) . ?
C13 H13 0.9300 . ?
C14 H14 0.9300 . ?
C2 C3 1.325(9) . ?
C2 H2 0.9300 . ?
C3 H3 0.9300 . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C12 H12 0.9300 . ?
C20 H20 0.9300 . ?
C5 H5A 0.9600 . ?
C5 H5B 0.9600 . ?
C5 H5C 0.9600 . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
C15 C17 1.465(16) . ?
C15 C16 1.493(9) . ?
C15 H15 0.9800 . ?
C23 C21 1.420(13) . ?
C23 H23A 0.9600 . ?
C23 H23B 0.9600 . ?
C23 H23C 0.9600 . ?
C6 H6A 0.9600 . ?
C6 H6B 0.9600 . ?
C6 H6C 0.9600 . ?
C21 C22 1.463(9) . ?
C21 H21 0.9800 . ?
C22 H22A 0.9300 . ?
C22 H22B 0.9300 . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?

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
N3 Cu1 N3 180.0 2_667 . ?
N3 Cu1 N1 89.91(19) 2_667 . ?
N3 Cu1 N1 90.09(18) . . ?
N3 Cu1 N1 90.09(18) 2_667 2_667 ?
N3 Cu1 N1 89.91(19) . 2_667 ?
N1 Cu1 N1 180.0(3) . 2_667 ?
N3 Cu1 O3 91.05(16) 2_667 . ?
N3 Cu1 O3 88.95(16) . . ?
N1 Cu1 O3 89.13(17) . . ?
N1 Cu1 O3 90.87(17) 2_667 . ?
N3 Cu1 O3 88.95(16) 2_667 2_667 ?
N3 Cu1 O3 91.05(16) . 2_667 ?
N1 Cu1 O3 90.87(17) . 2_667 ?
N1 Cu1 O3 89.13(17) 2_667 2_667 ?
O3 Cu1 O3 180.0(2) . 2_667 ?
N5 Cu2 N5 180.0 2_576 . ?
N5 Cu2 N7 89.4(2) 2_576 . ?
N5 Cu2 N7 90.6(2) . . ?
N5 Cu2 N7 90.6(2) 2_576 2_576 ?
N5 Cu2 N7 89.4(2) . 2_576 ?
N7 Cu2 N7 180.0 . 2_576 ?
N5 Cu2 O11 88.73(18) 2_576 . ?
N5 Cu2 O11 91.26(19) . . ?
N7 Cu2 O11 89.91(19) . . ?
N7 Cu2 O11 90.09(19) 2_576 . ?
O9 V4 O11 108.2(3) . . ?
O9 V4 O8 108.5(2) . . ?
O11 V4 O8 112.1(3) . . ?
O9 V4 O10 110.7(3) . . ?
O11 V4 O10 109.1(3) . . ?
O8 V4 O10 108.1(2) . . ?
O4 V2 O5 110.3(3) . . ?
O4 V2 O2 108.8(3) . . ?
O5 V2 O2 108.6(2) . . ?
O4 V2 O6 106.5(3) . . ?
O5 V2 O6 111.9(2) . . ?
O2 V2 O6 110.6(2) . . ?
O1 V1 O3 108.6(3) . . ?
O1 V1 O5 109.3(3) . 2_677 ?
O3 V1 O5 110.4(3) . 2_677 ?
O1 V1 O2 109.0(3) . . ?
O3 V1 O2 110.7(2) . . ?
O5 V1 O2 108.8(2) 2_677 . ?
O7 V3 O10 106.6(4) . 2_676 ?
O7 V3 O8 106.2(3) . . ?
O10 V3 O8 113.1(3) 2_676 . ?
O7 V3 O6 107.2(3) . . ?
O10 V3 O6 111.8(3) 2_676 . ?
O8 V3 O6 111.5(2) . . ?
C1 N2 C3 106.1(5) . . ?
C1 N2 C4 126.6(5) . . ?
C3 N2 C4 126.8(6) . . ?
C1 N1 C2 104.2(5) . . ?
C1 N1 Cu1 124.7(4) . . ?
C2 N1 Cu1 130.9(4) . . ?
C7 N4 C9 106.4(5) . . ?
C7 N4 C24 126.2(5) . . ?
C9 N4 C24 127.4(5) . . ?
C7 N3 C8 105.7(5) . . ?
C7 N3 Cu1 125.9(4) . . ?
C8 N3 Cu1 128.4(4) . . ?
C12 N5 C13 105.2(6) . . ?
C12 N5 Cu2 128.3(5) . . ?
C13 N5 Cu2 126.4(4) . . ?
C19 N7 C18 103.8(6) . . ?
C19 N7 Cu2 126.1(5) . . ?
C18 N7 Cu2 130.1(5) . . ?
C19 N8 C20 107.6(6) . . ?
C19 N8 C21 129.4(8) . . ?
C20 N8 C21 123.0(7) . . ?
V1 O3 Cu1 149.9(3) . . ?
C8 C9 N4 106.7(5) . . ?
C8 C9 H9 126.7 . . ?
N4 C9 H9 126.7 . . ?
V3 O6 V2 143.9(3) . . ?
V2 O2 V1 145.8(3) . . ?
C9 C8 N3 109.4(5) . . ?
C9 C8 H8 125.3 . . ?
N3 C8 H8 125.3 . . ?
V3 O8 V4 145.4(3) . . ?
V2 O5 V1 161.9(3) . 2_677 ?
N3 C7 N4 111.9(5) . . ?
N3 C7 H7 124.0 . . ?
N4 C7 H7 124.0 . . ?
N1 C1 N2 112.2(5) . . ?
N1 C1 H1 123.9 . . ?
N2 C1 H1 123.9 . . ?
N7 C19 N8 112.0(7) . . ?
N7 C19 H19 124.0 . . ?
N8 C19 H19 124.0 . . ?
V4 O11 Cu2 172.9(3) . . ?
V3 O10 V4 154.0(3) 2_676 . ?
C20 C18 N7 110.8(7) . . ?
C20 C18 H18 124.6 . . ?
N7 C18 H18 124.6 . . ?
C5 C4 N2 113.8(6) . . ?
C5 C4 C6 110.4(8) . . ?
N2 C4 C6 109.9(6) . . ?
C5 C4 H4 107.5 . . ?
N2 C4 H4 107.5 . . ?
C6 C4 H4 107.5 . . ?
N4 C24 C10 111.1(7) . . ?
N4 C24 C11 109.7(6) . . ?
C10 C24 C11 115.1(7) . . ?
N4 C24 H24 106.8 . . ?
C10 C24 H24 106.8 . . ?
C11 C24 H24 106.8 . . ?
C14 N6 C12 107.3(6) . . ?
C14 N6 C15 131.8(7) . . ?
C12 N6 C15 120.5(7) . . ?
C14 C13 N5 109.5(6) . . ?
C14 C13 H13 125.3 . . ?
N5 C13 H13 125.3 . . ?
C13 C14 N6 106.9(6) . . ?
C13 C14 H14 126.5 . . ?
N6 C14 H14 126.5 . . ?
C3 C2 N1 111.2(6) . . ?
C3 C2 H2 124.4 . . ?
N1 C2 H2 124.4 . . ?
C2 C3 N2 106.3(6) . . ?
C2 C3 H3 126.8 . . ?
N2 C3 H3 126.8 . . ?
C24 C10 H10A 109.5 . . ?
C24 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C24 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N5 C12 N6 111.1(6) . . ?
N5 C12 H12 124.4 . . ?
N6 C12 H12 124.4 . . ?
C18 C20 N8 105.8(7) . . ?
C18 C20 H20 127.1 . . ?
N8 C20 H20 127.1 . . ?
C4 C5 H5A 109.5 . . ?
C4 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C4 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C24 C11 H11A 109.5 . . ?
C24 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C24 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C17 C15 C16 106.8(12) . . ?
C17 C15 N6 106.8(10) . . ?
C16 C15 N6 98.3(9) . . ?
C17 C15 H15 114.5 . . ?
C16 C15 H15 114.5 . . ?
N6 C15 H15 114.5 . . ?
C21 C23 H23A 109.5 . . ?
C21 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C21 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C4 C6 H6A 109.5 . . ?
C4 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C4 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C23 C21 C22 128.8(11) . . ?
C23 C21 N8 111.9(9) . . ?
C22 C21 N8 112.8(9) . . ?
C23 C21 H21 98.5 . . ?
C22 C21 H21 98.5 . . ?
N8 C21 H21 98.5 . . ?
C21 C22 H22A 120.0 . . ?
C21 C22 H22B 120.0 . . ?
H22A C22 H22B 120.0 . . ?
C15 C17 H17A 109.5 . . ?
C15 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C15 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?

_refine_diff_density_max         1.839
_refine_diff_density_min         -0.805
_refine_diff_density_rms         0.110

####################################################################### 
# 
# 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_170225h
_database_code_depnum_ccdc_archive 'CCDC 2009808'
_audit_update_record             
;
2020-06-15 deposited with the CCDC.	2020-07-13 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C48 H80 Cu N16 O28 V10'
_chemical_formula_weight         1902.22

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'
Cu Cu -1.9646 0.5888 '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           56
_space_group_name_H-M_alt        'P c c n'
_space_group_name_Hall           '-P 2ab 2ac'

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

_cell_length_a                   21.7725(7)
_cell_length_b                   21.9575(9)
_cell_length_c                   14.8458(6)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     7097.3(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    6452
_cell_measurement_theta_min      2.8300
_cell_measurement_theta_max      71.3120

_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.780
_exptl_crystal_F_000             3852
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.220
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.190
_exptl_absorpt_coefficient_mu    11.617
_shelx_estimated_absorpt_T_min   0.184
_shelx_estimated_absorpt_T_max   0.216
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.183
_exptl_absorpt_correction_T_max  0.215
_exptl_absorpt_process_details   sadabs
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            44486
_diffrn_reflns_av_unetI/netI     0.0542
_diffrn_reflns_av_R_equivalents  0.1063
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         2.858
_diffrn_reflns_theta_max         66.000
_diffrn_reflns_theta_full        66.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             6194
_reflns_number_gt                4522
_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       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1071P)²+10.4452P] 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         6194
_refine_ls_number_parameters     470
_refine_ls_number_restraints     1183
_refine_ls_R_factor_all          0.0890
_refine_ls_R_factor_gt           0.0650
_refine_ls_wR_factor_ref         0.1946
_refine_ls_wR_factor_gt          0.1738
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_restrained_S_all      1.083
_refine_ls_shift/su_max          0.004
_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
N6 N 0.5428(3) 0.6866(3) 0.6659(4) 0.0587(15) Uani 1 1 d D U . . .
V1 V 0.48485(5) 0.47586(5) 0.72830(7) 0.0351(3) Uani 1 1 d . U . . .
V2 V 0.51374(5) 0.38708(4) 0.57325(7) 0.0347(3) Uani 1 1 d . U . . .
V3 V 0.55819(4) 0.52148(4) 0.56326(7) 0.0305(3) Uani 1 1 d . U . . .
V4 V 0.57781(5) 0.43084(5) 0.39950(7) 0.0346(3) Uani 1 1 d . U . . .
V5 V 0.61988(5) 0.56992(5) 0.39185(7) 0.0368(3) Uani 1 1 d . U . . .
Cu1 Cu 0.500000 0.500000 1.000000 0.0382(3) Uani 1 2 d S U P . .
N1 N 0.5386(2) 0.4178(2) 1.0188(4) 0.0413(11) Uani 1 1 d . U . . .
N2 N 0.5710(2) 0.3372(3) 1.0930(4) 0.0450(12) Uani 1 1 d . U . . .
N3 N 0.5839(2) 0.5380(2) 0.9901(4) 0.0414(12) Uani 1 1 d . U . . .
N4 N 0.6741(2) 0.5769(3) 1.0218(4) 0.0524(14) Uani 1 1 d . U . . .
N5 N 0.5693(3) 0.7210(3) 0.7876(5) 0.0715(18) Uani 1 1 d . U . . .
N7 N 0.7517(3) 0.4383(3) 0.6272(5) 0.0693(18) Uani 1 1 d . U . . .
N8 N 0.7153(4) 0.4554(4) 0.7631(6) 0.089(2) Uani 1 1 d . U . . .
O1 O 0.5004(2) 0.4790(2) 0.8351(3) 0.0436(10) Uani 1 1 d . U . . .
O2 O 0.52457(18) 0.40486(19) 0.6903(3) 0.0377(9) Uani 1 1 d . U . . .
O3 O 0.56337(17) 0.51801(18) 0.6761(3) 0.0357(9) Uani 1 1 d . U . . .
O4 O 0.5440(2) 0.32067(19) 0.5601(3) 0.0460(11) Uani 1 1 d . U . . .
O5 O 0.50535(17) 0.59326(17) 0.5568(3) 0.0323(8) Uani 1 1 d D U . . .
O6 O 0.58149(16) 0.44022(17) 0.5346(3) 0.0323(8) Uani 1 1 d . U . . .
O7 O 0.62252(17) 0.55740(19) 0.5267(3) 0.0378(9) Uani 1 1 d . U . . .
O8 O 0.52878(17) 0.51929(17) 0.4263(2) 0.0311(8) Uani 1 1 d . U . . .
O9 O 0.56923(18) 0.63306(19) 0.4124(3) 0.0391(9) Uani 1 1 d . U . . .
O10 O 0.58916(18) 0.55980(19) 0.2743(3) 0.0379(9) Uani 1 1 d . U . . .
O11 O 0.6854(2) 0.6018(2) 0.3755(3) 0.0481(11) Uani 1 1 d . U . . .
O12 O 0.54863(18) 0.44609(19) 0.2887(3) 0.0373(9) Uani 1 1 d . U . . .
O13 O 0.6089(2) 0.3652(2) 0.3864(3) 0.0484(11) Uani 1 1 d . U . . .
O14 O 0.64358(18) 0.48429(19) 0.3900(3) 0.0378(9) Uani 1 1 d . U . . .
C1 C 0.5485(3) 0.3935(3) 1.0984(5) 0.0458(15) Uani 1 1 d . U . . .
H1 H 0.540747 0.413450 1.152510 0.055 Uiso 1 1 calc R U . . .
C2 C 0.5557(3) 0.3730(3) 0.9587(5) 0.0517(16) Uani 1 1 d . U . . .
H2 H 0.553964 0.376505 0.896302 0.062 Uiso 1 1 calc R U . . .
C3 C 0.5753(3) 0.3238(3) 1.0032(5) 0.0546(17) Uani 1 1 d . U . . .
H3 H 0.589105 0.287564 0.978029 0.066 Uiso 1 1 calc R U . . .
C4 C 0.5828(3) 0.2964(3) 1.1706(5) 0.0518(16) Uani 1 1 d . U . . .
H4A H 0.554753 0.262176 1.167860 0.062 Uiso 1 1 calc R U . . .
H4B H 0.574575 0.318446 1.225961 0.062 Uiso 1 1 calc R U . . .
C5 C 0.6471(4) 0.2731(4) 1.1729(6) 0.076(2) Uani 1 1 d . U . . .
H5A H 0.675298 0.306615 1.183171 0.092 Uiso 1 1 calc R U . . .
H5B H 0.657243 0.254701 1.115334 0.092 Uiso 1 1 calc R U . . .
C6 C 0.6542(5) 0.2256(5) 1.2482(7) 0.100(3) Uani 1 1 d . U . . .
H6A H 0.641763 0.243215 1.304568 0.149 Uiso 1 1 calc R U . . .
H6B H 0.696397 0.213138 1.252110 0.149 Uiso 1 1 calc R U . . .
H6C H 0.628949 0.190930 1.235161 0.149 Uiso 1 1 calc R U . . .
C7 C 0.6191(3) 0.5591(3) 1.0546(5) 0.0487(15) Uani 1 1 d . U . . .
H7 H 0.607784 0.561457 1.114892 0.058 Uiso 1 1 calc R U . . .
C8 C 0.6177(3) 0.5430(3) 0.9129(5) 0.0490(15) Uani 1 1 d . U . . .
H8 H 0.604124 0.531570 0.856008 0.059 Uiso 1 1 calc R U . . .
C9 C 0.6729(3) 0.5666(3) 0.9305(5) 0.0530(16) Uani 1 1 d . U . . .
H9 H 0.704134 0.574387 0.889429 0.064 Uiso 1 1 calc R U . . .
C10 C 0.7282(4) 0.6003(4) 1.0702(6) 0.071(2) Uani 1 1 d . U . . .
H10A H 0.758187 0.567837 1.075167 0.085 Uiso 1 1 calc R U . . .
H10B H 0.746523 0.632651 1.034730 0.085 Uiso 1 1 calc R U . . .
C11 C 0.7153(4) 0.6236(5) 1.1599(6) 0.083(2) Uani 1 1 d . U . . .
H11A H 0.698029 0.591513 1.196966 0.100 Uiso 1 1 calc R U . . .
H11B H 0.685545 0.656418 1.156223 0.100 Uiso 1 1 calc R U . . .
C12 C 0.7753(5) 0.6473(6) 1.2028(7) 0.117(4) Uani 1 1 d . U . . .
H12A H 0.804509 0.614631 1.206536 0.176 Uiso 1 1 calc R U . . .
H12B H 0.766840 0.662455 1.262173 0.176 Uiso 1 1 calc R U . . .
H12C H 0.791852 0.679466 1.166401 0.176 Uiso 1 1 calc R U . . .
C13 C 0.5619(4) 0.6699(4) 0.7417(6) 0.067(2) Uani 1 1 d . U . . .
H13 H 0.569181 0.630367 0.761338 0.081 Uiso 1 1 calc R U . . .
C14 C 0.5530(4) 0.7691(4) 0.7329(6) 0.066(2) Uani 1 1 d . U . . .
H14 H 0.555359 0.810276 0.747174 0.079 Uiso 1 1 calc R U . . .
C15 C 0.5332(4) 0.7453(4) 0.6558(6) 0.0659(19) Uani 1 1 d . U . . .
H15 H 0.516455 0.765399 0.606475 0.079 Uiso 1 1 calc R U . . .
C16 C 0.5861(5) 0.7234(4) 0.8918(7) 0.081(2) Uani 1 1 d . U . . .
H16A H 0.559093 0.751374 0.923230 0.097 Uiso 1 1 calc R U . . .
H16B H 0.582119 0.683376 0.918766 0.097 Uiso 1 1 calc R U . . .
C17 C 0.6481(5) 0.7439(5) 0.8965(7) 0.094(3) Uani 1 1 d . U . . .
H17A H 0.653707 0.780713 0.861291 0.113 Uiso 1 1 calc R U . . .
H17B H 0.676050 0.712896 0.874507 0.113 Uiso 1 1 calc R U . . .
C18 C 0.6589(5) 0.7566(5) 1.0000(6) 0.092(3) Uani 1 1 d . U . . .
H18A H 0.640917 0.724459 1.034897 0.138 Uiso 1 1 calc R U . . .
H18B H 0.640242 0.794715 1.016135 0.138 Uiso 1 1 calc R U . . .
H18C H 0.702231 0.758507 1.011895 0.138 Uiso 1 1 calc R U . . .
C19 C 0.6990(4) 0.4430(4) 0.6772(6) 0.071(2) Uani 1 1 d . U . . .
H19 H 0.659071 0.438416 0.655856 0.085 Uiso 1 1 calc R U . . .
C20 C 0.7784(3) 0.4578(3) 0.7643(5) 0.0495(16) Uani 1 1 d . U . . .
H20 H 0.802446 0.466005 0.814582 0.059 Uiso 1 1 calc R U . . .
C21 C 0.7987(4) 0.4467(4) 0.6848(6) 0.071(2) Uani 1 1 d . U . . .
H21 H 0.840047 0.444831 0.669199 0.085 Uiso 1 1 calc R U . . .
C22 C 0.7566(5) 0.4221(5) 0.5304(6) 0.089(2) Uani 1 1 d . U . . .
H22A H 0.798815 0.426569 0.510644 0.107 Uiso 1 1 calc R U . . .
H22B H 0.731264 0.449411 0.494901 0.107 Uiso 1 1 calc R U . . .
C23 C 0.7353(5) 0.3558(5) 0.5159(7) 0.103(3) Uani 1 1 d . U . . .
H23A H 0.756666 0.329383 0.557976 0.123 Uiso 1 1 calc R U . . .
H23B H 0.691680 0.352814 0.528224 0.123 Uiso 1 1 calc R U . . .
C24 C 0.7475(7) 0.3349(6) 0.4230(9) 0.138(5) Uani 1 1 d . U . . .
H24A H 0.727102 0.361455 0.381214 0.207 Uiso 1 1 calc R U . . .
H24B H 0.732291 0.294169 0.415695 0.207 Uiso 1 1 calc R U . . .
H24C H 0.790882 0.335584 0.411825 0.207 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
N6 C13 1.255(10) . ?
N6 C15 1.314(9) . ?
V1 O1 1.623(5) . ?
V1 O10 1.792(4) 5_666 ?
V1 O2 1.870(4) . ?
V1 O12 1.879(4) 5_666 ?
V1 O3 2.093(4) . ?
V1 O8 2.316(4) 5_666 ?
V1 V5 3.0645(14) 5_666 ?
V1 V2 3.0812(15) . ?
V1 V3 3.0915(14) . ?
V1 V4 3.1076(14) 5_666 ?
V2 O4 1.612(4) . ?
V2 O2 1.797(4) . ?
V2 O9 1.872(4) 5_666 ?
V2 O6 1.966(4) . ?
V2 O5 2.021(4) 5_666 ?
V2 O8 2.255(4) 5_666 ?
V2 V4 3.0859(14) . ?
V2 V5 3.1022(14) 5_666 ?
V2 V3 3.1093(14) . ?
V3 O3 1.680(4) . ?
V3 O7 1.697(4) . ?
V3 O6 1.903(4) . ?
V3 O5 1.954(4) . ?
V3 O8 2.100(4) 5_666 ?
V3 O8 2.133(4) . ?
V3 V5 3.0677(14) . ?
V4 O13 1.605(4) . ?
V4 O12 1.795(4) . ?
V4 O14 1.857(4) . ?
V4 O5 1.995(4) 5_666 ?
V4 O6 2.018(4) . ?
V4 O8 2.251(4) . ?
V5 O11 1.608(4) . ?
V5 O9 1.798(4) . ?
V5 O10 1.882(4) . ?
V5 O14 1.950(4) . ?
V5 O7 2.021(4) . ?
V5 O8 2.330(4) . ?
Cu1 N1 2.010(5) 5_667 ?
Cu1 N1 2.010(5) . ?
Cu1 N3 2.013(5) 5_667 ?
Cu1 N3 2.013(5) . ?
Cu1 O1 2.491(4) . ?
N1 C1 1.315(8) . ?
N1 C2 1.380(8) . ?
N2 C1 1.333(8) . ?
N2 C3 1.369(9) . ?
N2 C4 1.481(8) . ?
N3 C7 1.312(8) . ?
N3 C8 1.366(8) . ?
N4 C7 1.349(8) . ?
N4 C9 1.374(9) . ?
N4 C10 1.473(9) . ?
N5 C13 1.321(10) . ?
N5 C14 1.380(11) . ?
N5 C16 1.590(11) . ?
N7 C21 1.347(9) . ?
N7 C19 1.370(11) . ?
N7 C22 1.484(11) . ?
N8 C19 1.351(11) . ?
N8 C20 1.375(10) . ?
C1 H1 0.9300 . ?
C2 C3 1.335(10) . ?
C2 H2 0.9300 . ?
C3 H3 0.9300 . ?
C4 C5 1.492(11) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C5 C6 1.537(11) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C6 H6A 0.9600 . ?
C6 H6B 0.9600 . ?
C6 H6C 0.9600 . ?
C7 H7 0.9300 . ?
C8 C9 1.334(9) . ?
C8 H8 0.9300 . ?
C9 H9 0.9300 . ?
C10 C11 1.454(12) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C11 C12 1.543(12) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C13 H13 0.9300 . ?
C14 C15 1.330(11) . ?
C14 H14 0.9300 . ?
C15 H15 0.9300 . ?
C16 C17 1.424(14) . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C17 C18 1.580(13) . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C19 H19 0.9300 . ?
C20 C21 1.283(11) . ?
C20 H20 0.9300 . ?
C21 H21 0.9300 . ?
C22 C23 1.544(14) . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
C23 C24 1.477(15) . ?
C23 H23A 0.9700 . ?
C23 H23B 0.9700 . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?

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
C13 N6 C15 116.1(7) . . ?
O1 V1 O10 103.1(2) . 5_666 ?
O1 V1 O2 103.5(2) . . ?
O10 V1 O2 92.58(19) 5_666 . ?
O1 V1 O12 100.0(2) . 5_666 ?
O10 V1 O12 92.68(19) 5_666 5_666 ?
O2 V1 O12 154.06(18) . 5_666 ?
O1 V1 O3 99.97(19) . . ?
O10 V1 O3 156.87(18) 5_666 . ?
O2 V1 O3 83.06(17) . . ?
O12 V1 O3 82.17(16) 5_666 . ?
O1 V1 O8 173.12(19) . 5_666 ?
O10 V1 O8 83.30(16) 5_666 5_666 ?
O2 V1 O8 78.40(16) . 5_666 ?
O12 V1 O8 77.03(16) 5_666 5_666 ?
O3 V1 O8 73.57(15) . 5_666 ?
O1 V1 V5 137.53(16) . 5_666 ?
O10 V1 V5 34.40(13) 5_666 5_666 ?
O2 V1 V5 83.98(13) . 5_666 ?
O12 V1 V5 86.14(13) 5_666 5_666 ?
O3 V1 V5 122.49(12) . 5_666 ?
O8 V1 V5 48.94(10) 5_666 5_666 ?
O1 V1 V2 135.55(16) . . ?
O10 V1 V2 83.73(14) 5_666 . ?
O2 V1 V2 32.09(13) . . ?
O12 V1 V2 123.78(13) 5_666 . ?
O3 V1 V2 80.57(11) . . ?
O8 V1 V2 46.78(10) 5_666 . ?
V5 V1 V2 60.63(3) 5_666 . ?
O1 V1 V3 130.77(16) . . ?
O10 V1 V3 126.07(13) 5_666 . ?
O2 V1 V3 78.01(13) . . ?
O12 V1 V3 78.38(13) 5_666 . ?
O3 V1 V3 30.81(11) . . ?
O8 V1 V3 42.78(10) 5_666 . ?
V5 V1 V3 91.68(4) 5_666 . ?
V2 V1 V3 60.49(3) . . ?
O1 V1 V4 131.34(16) . 5_666 ?
O10 V1 V4 83.10(14) 5_666 5_666 ?
O2 V1 V4 124.65(13) . 5_666 ?
O12 V1 V4 31.44(12) 5_666 5_666 ?
O3 V1 V4 80.84(11) . 5_666 ?
O8 V1 V4 46.26(10) 5_666 5_666 ?
V5 V1 V4 62.24(3) 5_666 5_666 ?
V2 V1 V4 92.90(4) . 5_666 ?
V3 V1 V4 61.92(3) . 5_666 ?
O4 V2 O2 105.1(2) . . ?
O4 V2 O9 101.2(2) . 5_666 ?
O2 V2 O9 93.91(19) . 5_666 ?
O4 V2 O6 101.2(2) . . ?
O2 V2 O6 93.15(18) . . ?
O9 V2 O6 153.80(17) 5_666 . ?
O4 V2 O5 99.3(2) . 5_666 ?
O2 V2 O5 154.74(18) . 5_666 ?
O9 V2 O5 87.73(17) 5_666 5_666 ?
O6 V2 O5 75.45(16) . 5_666 ?
O4 V2 O8 173.2(2) . 5_666 ?
O2 V2 O8 81.53(16) . 5_666 ?
O9 V2 O8 79.56(16) 5_666 5_666 ?
O6 V2 O8 76.58(15) . 5_666 ?
O5 V2 O8 73.97(15) 5_666 5_666 ?
O4 V2 V1 138.29(17) . . ?
O2 V2 V1 33.57(13) . . ?
O9 V2 V1 82.39(14) 5_666 . ?
O6 V2 V1 89.76(12) . . ?
O5 V2 V1 122.44(11) 5_666 . ?
O8 V2 V1 48.46(10) 5_666 . ?
O4 V2 V4 89.73(17) . . ?
O2 V2 V4 132.96(14) . . ?
O9 V2 V4 127.21(14) 5_666 . ?
O6 V2 V4 39.84(12) . . ?
O5 V2 V4 39.48(11) 5_666 . ?
O8 V2 V4 84.51(10) 5_666 . ?
V1 V2 V4 121.32(4) . . ?
O4 V2 V5 132.75(17) . 5_666 ?
O2 V2 V5 84.00(13) . 5_666 ?
O9 V2 V5 31.56(13) 5_666 5_666 ?
O6 V2 V5 124.87(11) . 5_666 ?
O5 V2 V5 84.36(11) 5_666 5_666 ?
O8 V2 V5 48.47(10) 5_666 5_666 ?
V1 V2 V5 59.42(3) . 5_666 ?
V4 V2 V5 117.96(4) . 5_666 ?
O4 V2 V3 136.52(17) . . ?
O2 V2 V3 78.41(14) . . ?
O9 V2 V3 122.01(14) 5_666 . ?
O6 V2 V3 35.84(11) . . ?
O5 V2 V3 79.38(11) 5_666 . ?
O8 V2 V3 42.48(10) 5_666 . ?
V1 V2 V3 59.92(3) . . ?
V4 V2 V3 61.57(3) . . ?
V5 V2 V3 90.63(4) 5_666 . ?
O3 V3 O7 106.6(2) . . ?
O3 V3 O6 99.35(18) . . ?
O7 V3 O6 98.29(18) . . ?
O3 V3 O5 97.20(18) . . ?
O7 V3 O5 95.47(18) . . ?
O6 V3 O5 154.45(16) . . ?
O3 V3 O8 88.13(17) . 5_666 ?
O7 V3 O8 165.03(18) . 5_666 ?
O6 V3 O8 81.79(15) . 5_666 ?
O5 V3 O8 79.43(15) . 5_666 ?
O3 V3 O8 165.83(17) . . ?
O7 V3 O8 87.30(17) . . ?
O6 V3 O8 81.12(16) . . ?
O5 V3 O8 78.13(15) . . ?
O8 V3 O8 77.90(16) 5_666 . ?
O3 V3 V5 144.40(14) . . ?
O7 V3 V5 37.98(14) . . ?
O6 V3 V5 91.31(12) . . ?
O5 V3 V5 86.39(12) . . ?
O8 V3 V5 127.16(11) 5_666 . ?
O8 V3 V5 49.33(10) . . ?
O3 V3 V1 39.65(13) . . ?
O7 V3 V1 146.19(15) . . ?
O6 V3 V1 90.63(12) . . ?
O5 V3 V1 89.79(12) . . ?
O8 V3 V1 48.50(10) 5_666 . ?
O8 V3 V1 126.40(11) . . ?
V5 V3 V1 174.85(4) . . ?
O3 V3 V2 86.00(14) . . ?
O7 V3 V2 135.51(15) . . ?
O6 V3 V2 37.23(11) . . ?
O5 V3 V2 125.79(11) . . ?
O8 V3 V2 46.47(10) 5_666 . ?
O8 V3 V2 86.02(11) . . ?
V5 V3 V2 120.33(4) . . ?
V1 V3 V2 59.59(3) . . ?
O13 V4 O12 101.9(2) . . ?
O13 V4 O14 103.5(2) . . ?
O12 V4 O14 94.89(19) . . ?
O13 V4 O5 100.6(2) . 5_666 ?
O12 V4 O5 91.52(17) . 5_666 ?
O14 V4 O5 153.18(17) . 5_666 ?
O13 V4 O6 101.3(2) . . ?
O12 V4 O6 154.96(17) . . ?
O14 V4 O6 88.89(17) . . ?
O5 V4 O6 74.90(15) 5_666 . ?
O13 V4 O8 175.2(2) . . ?
O12 V4 O8 80.39(16) . . ?
O14 V4 O8 80.44(16) . . ?
O5 V4 O8 74.99(15) 5_666 . ?
O6 V4 O8 75.84(14) . . ?
O13 V4 V2 90.69(17) . . ?
O12 V4 V2 131.62(13) . . ?
O14 V4 V2 127.53(13) . . ?
O5 V4 V2 40.10(11) 5_666 . ?
O6 V4 V2 38.63(11) . . ?
O8 V4 V2 84.65(10) . . ?
O13 V4 V1 134.70(17) . 5_666 ?
O12 V4 V1 33.09(13) . 5_666 ?
O14 V4 V1 82.84(13) . 5_666 ?
O5 V4 V1 88.58(12) 5_666 5_666 ?
O6 V4 V1 123.85(11) . 5_666 ?
O8 V4 V1 48.01(10) . 5_666 ?
V2 V4 V1 121.14(4) . 5_666 ?
O11 V5 O9 103.6(2) . . ?
O11 V5 O10 103.1(2) . . ?
O9 V5 O10 91.76(19) . . ?
O11 V5 O14 100.5(2) . . ?
O9 V5 O14 155.29(18) . . ?
O10 V5 O14 88.10(18) . . ?
O11 V5 O7 100.6(2) . . ?
O9 V5 O7 87.36(18) . . ?
O10 V5 O7 155.81(17) . . ?
O14 V5 O7 82.85(17) . . ?
O11 V5 O8 174.93(19) . . ?
O9 V5 O8 78.96(16) . . ?
O10 V5 O8 81.04(15) . . ?
O14 V5 O8 76.60(15) . . ?
O7 V5 O8 75.06(14) . . ?
O11 V5 V1 135.69(17) . 5_666 ?
O9 V5 V1 84.00(14) . 5_666 ?
O10 V5 V1 32.55(12) . 5_666 ?
O14 V5 V1 82.66(13) . 5_666 ?
O7 V5 V1 123.57(11) . 5_666 ?
O8 V5 V1 48.54(9) . 5_666 ?
O11 V5 V3 131.64(17) . . ?
O9 V5 V3 81.83(14) . . ?
O10 V5 V3 124.92(13) . . ?
O14 V5 V3 78.08(12) . . ?
O7 V5 V3 31.11(11) . . ?
O8 V5 V3 43.96(9) . . ?
V1 V5 V3 92.48(4) 5_666 . ?
O11 V5 V2 136.50(18) . 5_666 ?
O9 V5 V2 33.03(13) . 5_666 ?
O10 V5 V2 81.80(12) . 5_666 ?
O14 V5 V2 122.95(13) . 5_666 ?
O7 V5 V2 84.41(11) . 5_666 ?
O8 V5 V2 46.40(9) . 5_666 ?
V1 V5 V2 59.95(3) 5_666 5_666 ?
V3 V5 V2 63.66(3) . 5_666 ?
N1 Cu1 N1 180.0 5_667 . ?
N1 Cu1 N3 90.2(2) 5_667 5_667 ?
N1 Cu1 N3 89.9(2) . 5_667 ?
N1 Cu1 N3 89.8(2) 5_667 . ?
N1 Cu1 N3 90.1(2) . . ?
N3 Cu1 N3 180.0(3) 5_667 . ?
N1 Cu1 O1 91.81(18) 5_667 . ?
N1 Cu1 O1 88.19(18) . . ?
N3 Cu1 O1 89.90(18) 5_667 . ?
N3 Cu1 O1 90.10(18) . . ?
C1 N1 C2 104.3(6) . . ?
C1 N1 Cu1 123.9(4) . . ?
C2 N1 Cu1 131.6(5) . . ?
C1 N2 C3 106.4(6) . . ?
C1 N2 C4 125.3(6) . . ?
C3 N2 C4 128.1(6) . . ?
C7 N3 C8 105.5(5) . . ?
C7 N3 Cu1 128.6(5) . . ?
C8 N3 Cu1 125.7(4) . . ?
C7 N4 C9 106.9(6) . . ?
C7 N4 C10 129.4(6) . . ?
C9 N4 C10 123.6(6) . . ?
C13 N5 C14 108.3(7) . . ?
C13 N5 C16 124.0(8) . . ?
C14 N5 C16 127.3(6) . . ?
C21 N7 C19 106.4(7) . . ?
C21 N7 C22 126.3(8) . . ?
C19 N7 C22 127.1(7) . . ?
C19 N8 C20 106.4(8) . . ?
V1 O1 Cu1 165.3(3) . . ?
V2 O2 V1 114.3(2) . . ?
V3 O3 V1 109.55(19) . . ?
V3 O5 V4 107.71(18) . 5_666 ?
V3 O5 V2 109.91(18) . 5_666 ?
V4 O5 V2 100.42(17) 5_666 5_666 ?
V3 O6 V2 106.93(17) . . ?
V3 O6 V4 107.90(18) . . ?
V2 O6 V4 101.52(17) . . ?
V3 O7 V5 110.9(2) . . ?
V3 O8 V3 102.10(16) 5_666 . ?
V3 O8 V4 94.18(15) 5_666 . ?
V3 O8 V4 92.60(14) . . ?
V3 O8 V2 91.04(14) 5_666 5_666 ?
V3 O8 V2 95.72(15) . 5_666 ?
V4 O8 V2 169.04(19) . 5_666 ?
V3 O8 V1 88.71(14) 5_666 5_666 ?
V3 O8 V1 169.16(19) . 5_666 ?
V4 O8 V1 85.73(14) . 5_666 ?
V2 O8 V1 84.76(13) 5_666 5_666 ?
V3 O8 V5 170.72(19) 5_666 . ?
V3 O8 V5 86.72(13) . . ?
V4 O8 V5 88.24(13) . . ?
V2 O8 V5 85.13(13) 5_666 . ?
V1 O8 V5 82.53(13) 5_666 . ?
V5 O9 V2 115.4(2) . 5_666 ?
V1 O10 V5 113.1(2) 5_666 . ?
V4 O12 V1 115.5(2) . 5_666 ?
V4 O14 V5 113.8(2) . . ?
N1 C1 N2 112.5(6) . . ?
N1 C1 H1 123.7 . . ?
N2 C1 H1 123.7 . . ?
C3 C2 N1 110.0(6) . . ?
C3 C2 H2 125.0 . . ?
N1 C2 H2 125.0 . . ?
C2 C3 N2 106.7(6) . . ?
C2 C3 H3 126.6 . . ?
N2 C3 H3 126.6 . . ?
N2 C4 C5 112.9(6) . . ?
N2 C4 H4A 109.0 . . ?
C5 C4 H4A 109.0 . . ?
N2 C4 H4B 109.0 . . ?
C5 C4 H4B 109.0 . . ?
H4A C4 H4B 107.8 . . ?
C4 C5 C6 110.1(8) . . ?
C4 C5 H5A 109.6 . . ?
C6 C5 H5A 109.6 . . ?
C4 C5 H5B 109.6 . . ?
C6 C5 H5B 109.6 . . ?
H5A C5 H5B 108.2 . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C5 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
N3 C7 N4 110.9(6) . . ?
N3 C7 H7 124.5 . . ?
N4 C7 H7 124.5 . . ?
C9 C8 N3 110.7(6) . . ?
C9 C8 H8 124.7 . . ?
N3 C8 H8 124.7 . . ?
C8 C9 N4 105.9(6) . . ?
C8 C9 H9 127.0 . . ?
N4 C9 H9 127.0 . . ?
C11 C10 N4 114.5(7) . . ?
C11 C10 H10A 108.6 . . ?
N4 C10 H10A 108.6 . . ?
C11 C10 H10B 108.6 . . ?
N4 C10 H10B 108.6 . . ?
H10A C10 H10B 107.6 . . ?
C10 C11 C12 109.4(8) . . ?
C10 C11 H11A 109.8 . . ?
C12 C11 H11A 109.8 . . ?
C10 C11 H11B 109.8 . . ?
C12 C11 H11B 109.8 . . ?
H11A C11 H11B 108.2 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
N6 C13 N5 104.9(8) . . ?
N6 C13 H13 127.6 . . ?
N5 C13 H13 127.6 . . ?
C15 C14 N5 106.8(7) . . ?
C15 C14 H14 126.6 . . ?
N5 C14 H14 126.6 . . ?
N6 C15 C14 103.7(8) . . ?
N6 C15 H15 128.1 . . ?
C14 C15 H15 128.1 . . ?
C17 C16 N5 106.0(9) . . ?
C17 C16 H16A 110.5 . . ?
N5 C16 H16A 110.5 . . ?
C17 C16 H16B 110.5 . . ?
N5 C16 H16B 110.5 . . ?
H16A C16 H16B 108.7 . . ?
C16 C17 C18 104.2(9) . . ?
C16 C17 H17A 110.9 . . ?
C18 C17 H17A 110.9 . . ?
C16 C17 H17B 110.9 . . ?
C18 C17 H17B 110.9 . . ?
H17A C17 H17B 108.9 . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C17 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
N8 C19 N7 107.8(7) . . ?
N8 C19 H19 126.1 . . ?
N7 C19 H19 126.1 . . ?
C21 C20 N8 109.0(7) . . ?
C21 C20 H20 125.5 . . ?
N8 C20 H20 125.5 . . ?
C20 C21 N7 110.3(8) . . ?
C20 C21 H21 124.9 . . ?
N7 C21 H21 124.9 . . ?
N7 C22 C23 109.8(8) . . ?
N7 C22 H22A 109.7 . . ?
C23 C22 H22A 109.7 . . ?
N7 C22 H22B 109.7 . . ?
C23 C22 H22B 109.7 . . ?
H22A C22 H22B 108.2 . . ?
C24 C23 C22 111.6(12) . . ?
C24 C23 H23A 109.3 . . ?
C22 C23 H23A 109.3 . . ?
C24 C23 H23B 109.3 . . ?
C22 C23 H23B 109.3 . . ?
H23A C23 H23B 108.0 . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?

_refine_diff_density_max         1.389
_refine_diff_density_min         -1.092
_refine_diff_density_rms         0.128

####################################################################### 
# 
# 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_170224d
_database_code_depnum_ccdc_archive 'CCDC 2009807'
_audit_update_record             
;
2020-06-15 deposited with the CCDC.	2020-07-13 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C12 H20 Cu N4 O6 V2'
_chemical_formula_weight         481.74

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'
Cu Cu -1.9646 0.5888 '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                   9.2616(7)
_cell_length_b                   5.5433(4)
_cell_length_c                   17.1092(11)
_cell_angle_alpha                90
_cell_angle_beta                 93.4420(10)
_cell_angle_gamma                90
_cell_volume                     876.80(11)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    1945
_cell_measurement_theta_min      5.2650
_cell_measurement_theta_max      70.9060

_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.825
_exptl_crystal_F_000             486
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.220
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.180
_exptl_absorpt_coefficient_mu    10.510
_shelx_estimated_absorpt_T_min   0.206
_shelx_estimated_absorpt_T_max   0.253
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.3910
_exptl_absorpt_correction_T_max  0.4514
_exptl_absorpt_process_details   sadabs
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            4513
_diffrn_reflns_av_unetI/netI     0.0478
_diffrn_reflns_av_R_equivalents  0.0423
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         4.783
_diffrn_reflns_theta_max         65.982
_diffrn_reflns_theta_full        65.982
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             1533
_reflns_number_gt                1265
_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       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0621P)²] 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     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_extinction_coef       0.0010(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         1533
_refine_ls_number_parameters     118
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0561
_refine_ls_R_factor_gt           0.0400
_refine_ls_wR_factor_ref         0.1136
_refine_ls_wR_factor_gt          0.1054
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_restrained_S_all      1.043
_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
Cu1 Cu 0.000000 0.500000 0.000000 0.0200(2) Uani 1 2 d S . P . .
V1 V -0.05011(7) 0.48475(10) 0.19738(3) 0.0210(2) Uani 1 1 d . . . . .
N1 N 0.1336(3) 0.2208(5) 0.00860(15) 0.0239(7) Uani 1 1 d . . . . .
N2 N 0.2796(3) -0.0523(5) 0.06333(18) 0.0279(7) Uani 1 1 d . . . . .
O1 O 0.0230(3) 0.5444(5) 0.11179(14) 0.0301(6) Uani 1 1 d . . . . .
O2 O 0.0591(3) 0.2559(4) 0.24572(13) 0.0341(7) Uani 1 1 d . . . . .
O3 O -0.2114(3) 0.3852(6) 0.18090(19) 0.0508(8) Uani 1 1 d . . . . .
C1 C 0.2013(4) 0.1472(7) 0.0745(2) 0.0291(8) Uani 1 1 d . . . . .
H1 H 0.195375 0.223940 0.122542 0.035 Uiso 1 1 calc R U . . .
C2 C 0.1677(4) 0.0558(7) -0.0476(2) 0.0291(8) Uani 1 1 d . . . . .
H2 H 0.134933 0.060624 -0.100007 0.035 Uiso 1 1 calc R U . . .
C3 C 0.2564(4) -0.1143(7) -0.0144(2) 0.0305(8) Uani 1 1 d . . . . .
H3 H 0.294318 -0.247257 -0.039283 0.037 Uiso 1 1 calc R U . . .
C4 C 0.3665(4) -0.1814(7) 0.1265(2) 0.0349(9) Uani 1 1 d . . . . .
H4 H 0.300379 -0.272803 0.157946 0.042 Uiso 1 1 calc R U . . .
C5 C 0.4690(5) -0.3552(9) 0.0914(3) 0.0495(12) Uani 1 1 d . . . . .
H5A H 0.414787 -0.476526 0.062327 0.074 Uiso 1 1 calc R U . . .
H5B H 0.528268 -0.430373 0.132438 0.074 Uiso 1 1 calc R U . . .
H5C H 0.529302 -0.269809 0.057046 0.074 Uiso 1 1 calc R U . . .
C6 C 0.4464(6) -0.0006(7) 0.1789(3) 0.0483(13) Uani 1 1 d . . . . .
H6A H 0.506704 0.097895 0.148167 0.072 Uiso 1 1 calc R U . . .
H6B H 0.505362 -0.084280 0.218204 0.072 Uiso 1 1 calc R U . . .
H6C H 0.378004 0.099645 0.203643 0.072 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
Cu1 O1 1.928(2) . ?
Cu1 O1 1.928(2) 3_565 ?
Cu1 N1 1.981(3) 3_565 ?
Cu1 N1 1.981(3) . ?
V1 O3 1.601(3) . ?
V1 O1 1.683(2) . ?
V1 O2 1.793(2) . ?
V1 O2 1.796(2) 2 ?
N1 C1 1.321(4) . ?
N1 C2 1.377(5) . ?
N2 C1 1.343(5) . ?
N2 C3 1.379(5) . ?
N2 C4 1.491(5) . ?
C1 H1 0.9300 . ?
C2 C3 1.353(5) . ?
C2 H2 0.9300 . ?
C3 H3 0.9300 . ?
C4 C5 1.503(6) . ?
C4 C6 1.508(5) . ?
C4 H4 0.9800 . ?
C5 H5A 0.9600 . ?
C5 H5B 0.9600 . ?
C5 H5C 0.9600 . ?
C6 H6A 0.9600 . ?
C6 H6B 0.9600 . ?
C6 H6C 0.9600 . ?

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 Cu1 O1 180.0 . 3_565 ?
O1 Cu1 N1 90.30(11) . 3_565 ?
O1 Cu1 N1 89.69(11) 3_565 3_565 ?
O1 Cu1 N1 89.70(11) . . ?
O1 Cu1 N1 90.30(11) 3_565 . ?
N1 Cu1 N1 180.0 3_565 . ?
O3 V1 O1 109.53(15) . . ?
O3 V1 O2 109.38(16) . . ?
O1 V1 O2 107.17(12) . . ?
O3 V1 O2 108.11(15) . 2 ?
O1 V1 O2 109.96(12) . 2 ?
O2 V1 O2 112.66(5) . 2 ?
C1 N1 C2 105.9(3) . . ?
C1 N1 Cu1 124.5(2) . . ?
C2 N1 Cu1 129.4(2) . . ?
C1 N2 C3 106.8(3) . . ?
C1 N2 C4 124.4(3) . . ?
C3 N2 C4 128.8(3) . . ?
V1 O1 Cu1 144.31(18) . . ?
V1 O2 V1 143.06(17) . 2_545 ?
N1 C1 N2 111.5(3) . . ?
N1 C1 H1 124.3 . . ?
N2 C1 H1 124.3 . . ?
C3 C2 N1 109.2(3) . . ?
C3 C2 H2 125.4 . . ?
N1 C2 H2 125.4 . . ?
C2 C3 N2 106.6(3) . . ?
C2 C3 H3 126.7 . . ?
N2 C3 H3 126.7 . . ?
N2 C4 C5 110.1(3) . . ?
N2 C4 C6 109.6(3) . . ?
C5 C4 C6 111.4(4) . . ?
N2 C4 H4 108.5 . . ?
C5 C4 H4 108.5 . . ?
C6 C4 H4 108.5 . . ?
C4 C5 H5A 109.5 . . ?
C4 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C4 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C4 C6 H6A 109.5 . . ?
C4 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C4 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
C1 H1 O1 0.93 2.39 2.847(4) 110.3 . yes
C1 H1 O2 0.93 2.53 3.338(4) 145.9 . yes
C3 H3 O3 0.93 2.61 3.224(4) 123.9 3 yes

_refine_diff_density_max         0.564
_refine_diff_density_min         -0.405
_refine_diff_density_rms         0.090

