# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 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_01_0301
_database_code_depnum_ccdc_archive 'CCDC 1855753'
loop_
_audit_author_name
_audit_author_address
'Yang-Hui Luo'
;Southeast University
China
;
_audit_update_record             
;
2018-07-13 deposited with the CCDC.	2019-09-17 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C6 H13 K N O9 V'
_chemical_formula_weight         333.21

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'
K K 0.2009 0.2494 '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'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_H-M_alt        'P b c a'
_space_group_name_Hall           '-P 2ac 2ab'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, y-1/2, z'

_cell_length_a                   15.149(4)
_cell_length_b                   7.717(2)
_cell_length_c                   18.928(7)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2212.8(12)
_cell_formula_units_Z            8
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    627
_cell_measurement_theta_min      2.5420
_cell_measurement_theta_max      23.5690

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.000
_exptl_crystal_F_000             1360
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.130
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.110
_exptl_absorpt_coefficient_mu    1.316
_shelx_estimated_absorpt_T_min   0.848
_shelx_estimated_absorpt_T_max   0.869
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.77516
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            5657
_diffrn_reflns_av_unetI/netI     0.1622
_diffrn_reflns_av_R_equivalents  0.1162
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         2.152
_diffrn_reflns_theta_max         24.990
_diffrn_reflns_theta_full        24.990
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measured_fraction_theta_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_point_group_measured_fraction_full 0.994
_reflns_number_total             1941
_reflns_number_gt                1113
_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-2014/7 (Sheldrick, 2014)'
_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)+(0.0601P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         1941
_refine_ls_number_parameters     164
_refine_ls_number_restraints     22
_refine_ls_R_factor_all          0.1461
_refine_ls_R_factor_gt           0.0801
_refine_ls_wR_factor_ref         0.1909
_refine_ls_wR_factor_gt          0.1582
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_restrained_S_all      1.029
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
V1 V 0.60441(9) 0.49799(18) 0.48128(8) 0.0151(4) Uani 1 1 d . . . . .
K1 K 0.80323(12) 0.5245(2) 0.57968(10) 0.0186(5) Uani 1 1 d D . . . .
C1 C 0.4493(5) 0.8273(11) 0.7089(5) 0.016(2) Uani 1 1 d . . . . .
H1A H 0.4581 0.7256 0.7382 0.020 Uiso 1 1 calc R U . . .
H1B H 0.4995 0.9035 0.7158 0.020 Uiso 1 1 calc R U . . .
C2 C 0.4399(5) 0.9303(10) 0.5847(5) 0.0122(14) Uani 1 1 d . U . . .
H2A H 0.4373 0.8961 0.5354 0.015 Uiso 1 1 calc R U . . .
H2B H 0.3866 0.9945 0.5958 0.015 Uiso 1 1 calc R U . . .
C3 C 0.4458(5) 0.7715(10) 0.6309(5) 0.0126(14) Uani 1 1 d . U . . .
C4 C 0.3359(5) 0.5378(10) 0.6688(5) 0.0167(16) Uani 1 1 d . U . . .
H4A H 0.2725 0.5222 0.6651 0.020 Uiso 1 1 calc R U . . .
H4B H 0.3486 0.5869 0.7148 0.020 Uiso 1 1 calc R U . . .
C5 C 0.3816(5) 0.3623(11) 0.6619(5) 0.0164(16) Uani 1 1 d . U . . .
C6 C 0.5275(5) 0.6678(11) 0.6117(5) 0.0164(17) Uani 1 1 d . U . . .
H6A H 0.5796 0.7407 0.6137 0.020 Uiso 1 1 calc R U . . .
H6B H 0.5352 0.5719 0.6443 0.020 Uiso 1 1 calc R U . . .
N00C N 0.3663(4) 0.6601(8) 0.6126(4) 0.0120(16) Uani 1 1 d . . . . .
H00C H 0.3171 0.7374 0.6010 0.014 Uiso 1 1 calc R U . . .
O1 O 0.5158(3) 1.0375(7) 0.5964(3) 0.0174(15) Uani 1 1 d . . . . .
H1C H 0.5000 1.1382 0.6020 0.026 Uiso 1 1 calc R U . . .
O2 O 0.3727(4) 0.9125(7) 0.7307(3) 0.0205(15) Uani 1 1 d . . . . .
H2 H 0.3748 1.0141 0.7181 0.031 Uiso 1 1 calc R U . . .
O3 O 0.3660(4) 0.2520(7) 0.7093(3) 0.0246(16) Uani 1 1 d . . . . .
H3A H 0.3295 0.2911 0.7370 0.037 Uiso 1 1 calc R U . . .
O4 O 0.4326(3) 0.3420(7) 0.6109(3) 0.0158(14) Uani 1 1 d . . . . .
O5 O 0.5146(3) 0.6060(7) 0.5430(3) 0.0141(14) Uani 1 1 d . . . . .
H5A H 0.4626 0.6327 0.5192 0.017 Uiso 1 1 d R U . . .
O6 O 0.6705(4) 0.6926(7) 0.5101(3) 0.0216(15) Uani 1 1 d . . . . .
O7 O 0.7174(4) 0.5941(7) 0.4577(3) 0.0214(16) Uani 1 1 d . . . . .
O8 O 0.6377(3) 0.3505(7) 0.5351(3) 0.0158(14) Uani 1 1 d . . . . .
O9 O 0.7503(3) 0.2820(7) 0.6776(3) 0.0164(14) Uani 1 1 d D . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
V1 O8 1.609(6) . ?
V1 O6 1.885(6) . ?
V1 O7 1.917(6) . ?
V1 O5 1.978(6) . ?
V1 O5 2.026(5) 5_666 ?
V1 N00C 2.200(7) 5_666 ?
V1 O4 2.209(6) 5_666 ?
V1 K1 3.547(2) . ?
K1 O7 2.704(7) . ?
K1 O6 2.732(6) . ?
K1 O9 2.753(5) . ?
K1 O1 2.762(5) 8_755 ?
K1 O8 2.800(6) 8_765 ?
K1 O9 2.835(6) 8_765 ?
K1 O6 2.908(6) 8_755 ?
K1 O8 2.967(6) . ?
K1 K1 4.1819(17) 8_755 ?
K1 K1 4.1819(17) 8_765 ?
C1 O2 1.395(9) . ?
C1 C3 1.539(12) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C2 O1 1.433(9) . ?
C2 C3 1.509(11) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 C6 1.518(11) . ?
C3 N00C 1.520(10) . ?
C4 N00C 1.494(10) . ?
C4 C5 1.527(11) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C5 O4 1.245(10) . ?
C5 O3 1.260(10) . ?
C6 O5 1.399(10) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
N00C V1 2.200(7) 5_666 ?
N00C H00C 0.9800 . ?
O1 K1 2.762(5) 8_765 ?
O1 H1C 0.8200 . ?
O2 H2 0.8200 . ?
O3 H3A 0.8200 . ?
O4 V1 2.209(6) 5_666 ?
O5 V1 2.026(5) 5_666 ?
O5 H5A 0.9300 . ?
O6 O7 1.437(8) . ?
O6 K1 2.908(6) 8_765 ?
O8 K1 2.800(6) 8_755 ?
O9 K1 2.835(6) 8_755 ?

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
O8 V1 O6 102.4(3) . . ?
O8 V1 O7 98.1(3) . . ?
O6 V1 O7 44.4(2) . . ?
O8 V1 O5 98.0(3) . . ?
O6 V1 O5 81.9(2) . . ?
O7 V1 O5 126.1(2) . . ?
O8 V1 O5 98.2(3) . 5_666 ?
O6 V1 O5 148.6(2) . 5_666 ?
O7 V1 O5 153.4(3) . 5_666 ?
O5 V1 O5 71.9(3) . 5_666 ?
O8 V1 N00C 93.2(3) . 5_666 ?
O6 V1 N00C 124.6(2) . 5_666 ?
O7 V1 N00C 81.2(2) . 5_666 ?
O5 V1 N00C 148.1(2) . 5_666 ?
O5 V1 N00C 77.1(2) 5_666 5_666 ?
O8 V1 O4 167.1(3) . 5_666 ?
O6 V1 O4 85.3(2) . 5_666 ?
O7 V1 O4 80.0(2) . 5_666 ?
O5 V1 O4 93.3(2) . 5_666 ?
O5 V1 O4 79.4(2) 5_666 5_666 ?
N00C V1 O4 73.9(2) 5_666 5_666 ?
O8 V1 K1 56.09(19) . . ?
O6 V1 K1 49.56(18) . . ?
O7 V1 K1 48.9(2) . . ?
O5 V1 K1 104.46(18) . . ?
O5 V1 K1 153.83(18) 5_666 . ?
N00C V1 K1 106.55(17) 5_666 . ?
O4 V1 K1 126.70(15) 5_666 . ?
O7 K1 O6 30.65(17) . . ?
O7 K1 O9 124.72(18) . . ?
O6 K1 O9 115.67(17) . . ?
O7 K1 O1 124.65(18) . 8_755 ?
O6 K1 O1 140.25(18) . 8_755 ?
O9 K1 O1 103.67(17) . 8_755 ?
O7 K1 O8 73.64(17) . 8_765 ?
O6 K1 O8 70.33(17) . 8_765 ?
O9 K1 O8 155.04(19) . 8_765 ?
O1 K1 O8 71.62(16) 8_755 8_765 ?
O7 K1 O9 106.33(17) . 8_765 ?
O6 K1 O9 76.81(17) . 8_765 ?
O9 K1 O9 87.33(15) . 8_765 ?
O1 K1 O9 100.58(17) 8_755 8_765 ?
O8 K1 O9 70.04(16) 8_765 8_765 ?
O7 K1 O6 81.58(18) . 8_755 ?
O6 K1 O6 107.5(2) . 8_755 ?
O9 K1 O6 75.28(18) . 8_755 ?
O1 K1 O6 87.03(16) 8_755 8_755 ?
O8 K1 O6 127.67(18) 8_765 8_755 ?
O9 K1 O6 162.29(18) 8_765 8_755 ?
O7 K1 O8 55.98(16) . . ?
O6 K1 O8 57.03(16) . . ?
O9 K1 O8 68.74(17) . . ?
O1 K1 O8 152.63(17) 8_755 . ?
O8 K1 O8 126.25(19) 8_765 . ?
O9 K1 O8 105.13(16) 8_765 . ?
O6 K1 O8 65.67(16) 8_755 . ?
O7 K1 V1 32.28(12) . . ?
O6 K1 V1 31.69(13) . . ?
O9 K1 V1 93.84(12) . . ?
O1 K1 V1 154.87(15) 8_755 . ?
O8 K1 V1 99.51(13) 8_765 . ?
O9 K1 V1 98.08(12) 8_765 . ?
O6 K1 V1 80.06(12) 8_755 . ?
O8 K1 V1 26.75(11) . . ?
O7 K1 K1 89.86(13) . 8_755 ?
O6 K1 K1 98.87(14) . 8_755 ?
O9 K1 K1 42.30(12) . 8_755 ?
O1 K1 K1 114.60(12) 8_755 8_755 ?
O8 K1 K1 162.21(13) 8_765 8_755 ?
O9 K1 K1 122.43(12) 8_765 8_755 ?
O6 K1 K1 40.54(12) 8_755 8_755 ?
O8 K1 K1 41.96(11) . 8_755 ?
V1 K1 K1 67.62(5) . 8_755 ?
O7 K1 K1 68.37(13) . 8_765 ?
O6 K1 K1 43.78(13) . 8_765 ?
O9 K1 K1 121.00(13) . 8_765 ?
O1 K1 K1 110.45(12) 8_755 8_765 ?
O8 K1 K1 45.12(11) 8_765 8_765 ?
O9 K1 K1 40.80(11) 8_765 8_765 ?
O6 K1 K1 149.94(13) 8_755 8_765 ?
O8 K1 K1 95.26(12) . 8_765 ?
V1 K1 K1 74.08(6) . 8_765 ?
K1 K1 K1 134.63(9) 8_755 8_765 ?
O2 C1 C3 112.7(7) . . ?
O2 C1 H1A 109.0 . . ?
C3 C1 H1A 109.0 . . ?
O2 C1 H1B 109.0 . . ?
C3 C1 H1B 109.0 . . ?
H1A C1 H1B 107.8 . . ?
O1 C2 C3 109.4(6) . . ?
O1 C2 H2A 109.8 . . ?
C3 C2 H2A 109.8 . . ?
O1 C2 H2B 109.8 . . ?
C3 C2 H2B 109.8 . . ?
H2A C2 H2B 108.3 . . ?
C2 C3 C6 109.7(7) . . ?
C2 C3 N00C 106.3(6) . . ?
C6 C3 N00C 107.1(6) . . ?
C2 C3 C1 109.3(7) . . ?
C6 C3 C1 110.5(7) . . ?
N00C C3 C1 113.9(7) . . ?
N00C C4 C5 111.1(7) . . ?
N00C C4 H4A 109.4 . . ?
C5 C4 H4A 109.4 . . ?
N00C C4 H4B 109.4 . . ?
C5 C4 H4B 109.4 . . ?
H4A C4 H4B 108.0 . . ?
O4 C5 O3 125.7(8) . . ?
O4 C5 C4 117.3(8) . . ?
O3 C5 C4 117.0(8) . . ?
O5 C6 C3 106.7(6) . . ?
O5 C6 H6A 110.4 . . ?
C3 C6 H6A 110.4 . . ?
O5 C6 H6B 110.4 . . ?
C3 C6 H6B 110.4 . . ?
H6A C6 H6B 108.6 . . ?
C4 N00C C3 116.0(6) . . ?
C4 N00C V1 106.7(4) . 5_666 ?
C3 N00C V1 109.8(5) . 5_666 ?
C4 N00C H00C 108.0 . . ?
C3 N00C H00C 108.0 . . ?
V1 N00C H00C 108.0 5_666 . ?
C2 O1 K1 139.2(4) . 8_765 ?
C2 O1 H1C 109.5 . . ?
K1 O1 H1C 109.8 8_765 . ?
C1 O2 H2 109.5 . . ?
C5 O3 H3A 109.5 . . ?
C5 O4 V1 112.6(5) . 5_666 ?
C6 O5 V1 126.6(5) . . ?
C6 O5 V1 118.1(5) . 5_666 ?
V1 O5 V1 108.1(3) . 5_666 ?
C6 O5 H5A 119.6 . . ?
V1 O5 H5A 112.9 . . ?
V1 O5 H5A 39.2 5_666 . ?
O7 O6 V1 69.0(3) . . ?
O7 O6 K1 73.6(3) . . ?
V1 O6 K1 98.8(2) . . ?
O7 O6 K1 135.3(4) . 8_765 ?
V1 O6 K1 154.8(3) . 8_765 ?
K1 O6 K1 95.68(19) . 8_765 ?
O6 O7 V1 66.6(3) . . ?
O6 O7 K1 75.7(4) . . ?
V1 O7 K1 98.9(3) . . ?
V1 O8 K1 157.9(3) . 8_755 ?
V1 O8 K1 97.2(2) . . ?
K1 O8 K1 92.92(15) 8_755 . ?
K1 O9 K1 96.89(18) . 8_755 ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O1 C2 C3 C6 -61.5(8) . . . . ?
O1 C2 C3 N00C -176.9(6) . . . . ?
O1 C2 C3 C1 59.8(8) . . . . ?
O2 C1 C3 C2 63.5(8) . . . . ?
O2 C1 C3 C6 -175.7(6) . . . . ?
O2 C1 C3 N00C -55.2(9) . . . . ?
N00C C4 C5 O4 -3.2(10) . . . . ?
N00C C4 C5 O3 175.2(7) . . . . ?
C2 C3 C6 O5 -65.9(8) . . . . ?
N00C C3 C6 O5 49.0(8) . . . . ?
C1 C3 C6 O5 173.5(7) . . . . ?
C5 C4 N00C C3 -90.3(8) . . . . ?
C5 C4 N00C V1 32.4(7) . . . 5_666 ?
C2 C3 N00C C4 -155.4(6) . . . . ?
C6 C3 N00C C4 87.3(8) . . . . ?
C1 C3 N00C C4 -35.0(9) . . . . ?
C2 C3 N00C V1 83.6(6) . . . 5_666 ?
C6 C3 N00C V1 -33.6(7) . . . 5_666 ?
C1 C3 N00C V1 -156.0(5) . . . 5_666 ?
C3 C2 O1 K1 63.7(10) . . . 8_765 ?
O3 C5 O4 V1 153.1(7) . . . 5_666 ?
C4 C5 O4 V1 -28.6(8) . . . 5_666 ?
C3 C6 O5 V1 168.3(5) . . . . ?
C3 C6 O5 V1 -45.0(8) . . . 5_666 ?
O8 V1 O6 O7 89.0(4) . . . . ?
O5 V1 O6 O7 -174.5(4) . . . . ?
O5 V1 O6 O7 -141.3(5) 5_666 . . . ?
N00C V1 O6 O7 -13.7(5) 5_666 . . . ?
O4 V1 O6 O7 -80.5(3) 5_666 . . . ?
K1 V1 O6 O7 68.6(3) . . . . ?
O8 V1 O6 K1 20.4(3) . . . . ?
O7 V1 O6 K1 -68.6(3) . . . . ?
O5 V1 O6 K1 116.9(2) . . . . ?
O5 V1 O6 K1 150.1(4) 5_666 . . . ?
N00C V1 O6 K1 -82.3(3) 5_666 . . . ?
O4 V1 O6 K1 -149.1(2) 5_666 . . . ?
O8 V1 O6 K1 -103.9(7) . . . 8_765 ?
O7 V1 O6 K1 167.1(9) . . . 8_765 ?
O5 V1 O6 K1 -7.4(7) . . . 8_765 ?
O5 V1 O6 K1 25.8(11) 5_666 . . 8_765 ?
N00C V1 O6 K1 153.4(6) 5_666 . . 8_765 ?
O4 V1 O6 K1 86.6(7) 5_666 . . 8_765 ?
K1 V1 O6 K1 -124.3(8) . . . 8_765 ?
K1 O6 O7 V1 106.4(2) . . . . ?
K1 O6 O7 V1 -172.2(5) 8_765 . . . ?
V1 O6 O7 K1 -106.4(2) . . . . ?
K1 O6 O7 K1 81.3(5) 8_765 . . . ?
O6 V1 O8 K1 -135.1(7) . . . 8_755 ?
O7 V1 O8 K1 -90.2(8) . . . 8_755 ?
O5 V1 O8 K1 141.5(7) . . . 8_755 ?
O5 V1 O8 K1 68.7(8) 5_666 . . 8_755 ?
N00C V1 O8 K1 -8.7(8) 5_666 . . 8_755 ?
O4 V1 O8 K1 -9.6(17) 5_666 . . 8_755 ?
K1 V1 O8 K1 -116.5(8) . . . 8_755 ?
O6 V1 O8 K1 -18.7(3) . . . . ?
O7 V1 O8 K1 26.3(3) . . . . ?
O5 V1 O8 K1 -102.1(2) . . . . ?
O5 V1 O8 K1 -174.8(2) 5_666 . . . ?
N00C V1 O8 K1 107.8(2) 5_666 . . . ?
O4 V1 O8 K1 106.9(11) 5_666 . . . ?

_refine_diff_density_max         0.677
_refine_diff_density_min         -0.562
_refine_diff_density_rms         0.148

####################################################################### 
# 
# 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_11_0306
_database_code_depnum_ccdc_archive 'CCDC 1855754'
loop_
_audit_author_name
_audit_author_address
'Yang-Hui Luo'
;Southeast University
China
;
_audit_update_record             
;
2018-07-13 deposited with the CCDC.	2019-09-17 downloaded from the CCDC.
;
_audit_creation_date             2018-03-17
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_shelx_SHELXL_version_number     2017/1
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '0.5(C36 K2 N4 O14 V2)'
_chemical_formula_sum            'C18 K N2 O7 V'
_chemical_formula_weight         446.24
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2009 0.2494 '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           11
_space_group_name_H-M_alt        'P 1 21/m 1'
_space_group_name_Hall           '-P 2yb'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z'
'-x, -y, -z'
'x, -y-1/2, z'

_cell_length_a                   7.0360(5)
_cell_length_b                   5.8774(5)
_cell_length_c                   12.6598(9)
_cell_angle_alpha                90
_cell_angle_beta                 90.168(7)
_cell_angle_gamma                90
_cell_volume                     523.52(7)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    3374
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      28.8100
_cell_measurement_theta_min      3.2130
_shelx_estimated_absorpt_T_max   0.859
_shelx_estimated_absorpt_T_min   0.837
_exptl_absorpt_coefficient_mu    1.423
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.71935
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43f (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.831
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             440
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.11
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0635
_diffrn_reflns_av_unetI/netI     0.0472
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.936
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            9277
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.936
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.405
_diffrn_reflns_theta_min         2.895
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2684
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.936
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -87.00 -38.00   1.00    1.00    --  -11.59 153.00 165.33   49
  2  ω    -85.00 -37.00   1.00    1.00    --  -11.59 151.00  38.06   48
  3  ω    -21.00  88.00   1.00    1.00    --   11.74  77.00-150.00  109
  4  ω    -20.00  53.00   1.00    1.00    --   11.74 -99.00  60.00   73
  5  ω    -60.00  40.00   1.00    1.00    --   11.74 -57.00 -60.00  100
  6  ω     35.00  91.00   1.00    1.00    --   11.74 178.00 -30.00   56
  7  ω    -29.00  88.00   1.00    1.00    --   11.74  19.00  30.00  117
  8  ω    -13.00  82.00   1.00    1.00    --   11.74  37.00 120.00   95
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0181987000
_diffrn_orient_matrix_UB_12      0.0730606000
_diffrn_orient_matrix_UB_13      0.0434683000
_diffrn_orient_matrix_UB_21      0.0963553000
_diffrn_orient_matrix_UB_22      0.0094277000
_diffrn_orient_matrix_UB_23      -0.0157407000
_diffrn_orient_matrix_UB_31      -0.0233598000
_diffrn_orient_matrix_UB_32      0.0956650000
_diffrn_orient_matrix_UB_33      -0.0316097000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1328
_reflns_number_total             1475
_reflns_odcompleteness_completeness 99.92
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_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    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         1.623
_refine_diff_density_min         -1.961
_refine_diff_density_rms         0.465
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.200
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     139
_refine_ls_number_reflns         1475
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1561
_refine_ls_R_factor_gt           0.1476
_refine_ls_restrained_S_all      1.200
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1387P)²+33.6056P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3932
_refine_ls_wR_factor_ref         0.3987
_refine_special_details          ?
_olex2_refinement_description    
;
;
_atom_sites_solution_hydrogens   .
_atom_sites_solution_primary     dual
_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
V001 V 0.3661(3) 0.250000 0.72862(19) 0.0069(7) Uani 1 2 d S T P . .
K002 K 0.4263(5) 0.250000 0.3846(2) 0.0105(8) Uani 1 2 d S T P . .
O5 O 0.5296(15) 0.250000 0.6093(8) 0.0054(19) Uani 1 2 d S T P . .
O4 O -0.0305(18) 0.750000 0.6257(11) 0.025(3) Uani 1 2 d S T P . .
O3 O -0.031(3) 0.250000 0.6417(18) 0.107(15) Uani 1 2 d S T P . .
O1 O 0.572(3) 0.437(3) 0.7880(11) 0.061(4) Uani 1 1 d . . . . .
C8 C 0.234(2) 0.550(3) 0.6851(11) 0.028(3) Uani 1 1 d . . . . .
C9 C 0.3484(18) 0.354(3) 0.5852(11) 0.024(3) Uani 1 1 d . . . . .
C6 C 0.072(2) 0.356(3) 0.7168(12) 0.036(3) Uani 1 1 d . . . . .
C1 C 0.4230(18) 0.499(3) 0.7828(12) 0.025(3) Uani 1 1 d . . . . .
N00B N 0.254(2) 0.344(3) 0.8795(13) 0.045(4) Uani 1 1 d . . . . .
O2 O 0.678(2) 0.646(2) 0.9218(12) 0.052(4) Uani 1 1 d . . . . .
C4 C 0.041(3) 0.350(4) 0.8838(17) 0.050(5) Uani 1 1 d . . . . .
C7 C 0.063(3) 0.547(4) 0.6536(15) 0.044(4) Uani 1 1 d . . . . .
C0AA C -0.017(3) 0.363(4) 0.8220(15) 0.048(5) Uani 1 1 d . . . . .
C3 C 0.345(3) 0.556(4) 0.9173(16) 0.048(5) Uani 1 1 d . . . . .
C2 C 0.545(3) 0.554(4) 0.8770(15) 0.055(5) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
V001 O5 1.902(11) . ?
V001 O1 1.967(16) . ?
V001 O1 1.967(16) 4_565 ?
V001 C8 2.066(15) . ?
V001 C8 2.066(15) 4_565 ?
V001 C9 1.919(15) 4_565 ?
V001 C9 1.919(15) . ?
V001 C6 2.167(17) 4_565 ?
V001 C1 1.665(15) 4_565 ?
V001 C1 1.665(15) . ?
V001 N00B 2.141(17) 4_565 ?
V001 N00B 2.141(17) . ?
K002 O5 2.934(10) . ?
K002 O4 2.788(13) 3_566 ?
K002 O1 2.857(16) 3_666 ?
K002 O1 2.857(16) 2_646 ?
K002 C8 2.809(15) 3_666 ?
K002 C8 2.809(15) 2_646 ?
K002 C9 2.840(15) 2_646 ?
K002 C9 2.672(14) 4_565 ?
K002 C9 2.672(14) . ?
K002 C9 2.840(15) 3_666 ?
K002 C1 2.793(15) 2_646 ?
K002 C1 2.793(16) 3_666 ?
O5 C9 1.446(15) . ?
O5 C9 1.446(16) 4_565 ?
O4 C7 1.41(2) 4_575 ?
O4 C7 1.41(2) . ?
O3 C6 1.35(3) 4_565 ?
O3 C6 1.35(3) . ?
O3 C7 1.87(2) . ?
O3 C7 1.87(2) 4_565 ?
O1 C1 1.11(2) . ?
O1 C2 1.33(3) . ?
C8 C9 1.89(2) . ?
C8 C6 1.66(2) . ?
C8 C1 1.84(2) . ?
C8 C7 1.27(2) . ?
C9 C9 1.22(3) 4_565 ?
C6 C6 1.24(4) 4_565 ?
C6 C7 1.38(3) . ?
C6 C0AA 1.47(2) . ?
C6 C0AA 1.95(3) 4_565 ?
C1 N00B 1.94(2) . ?
C1 C3 1.82(2) . ?
C1 C2 1.50(2) . ?
N00B N00B 1.11(3) 4_565 ?
N00B C4 1.50(2) . ?
N00B C4 1.89(3) 4_565 ?
N00B C3 1.48(3) . ?
O2 O2 1.23(3) 4_575 ?
O2 C2 1.22(2) . ?
C4 C4 1.18(5) 4_565 ?
C4 C0AA 0.89(2) . ?
C4 C0AA 1.53(3) 4_565 ?
C0AA C0AA 1.32(5) 4_565 ?
C3 C2 1.50(3) . ?

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
O5 V001 O1 81.8(5) . . ?
O5 V001 O1 81.8(5) . 4_565 ?
O5 V001 C8 93.5(4) . . ?
O5 V001 C8 93.5(4) . 4_565 ?
O5 V001 C9 44.5(5) . . ?
O5 V001 C9 44.5(5) . 4_565 ?
O5 V001 C6 121.7(5) . 4_565 ?
O5 V001 N00B 159.0(5) . 4_565 ?
O5 V001 N00B 159.0(5) . . ?
O1 V001 O1 67.9(11) . 4_565 ?
O1 V001 C8 155.4(7) 4_565 . ?
O1 V001 C8 155.4(7) . 4_565 ?
O1 V001 C8 87.5(7) . . ?
O1 V001 C8 87.5(7) 4_565 4_565 ?
O1 V001 C6 124.7(7) 4_565 4_565 ?
O1 V001 C6 152.8(7) . 4_565 ?
O1 V001 N00B 77.7(6) 4_565 4_565 ?
O1 V001 N00B 94.3(6) 4_565 . ?
O1 V001 N00B 94.3(6) . 4_565 ?
O1 V001 N00B 77.7(6) . . ?
C8 V001 C8 117.0(9) 4_565 . ?
C8 V001 C6 78.2(7) . 4_565 ?
C8 V001 C6 46.2(7) 4_565 4_565 ?
C8 V001 N00B 107.0(6) . 4_565 ?
C8 V001 N00B 81.5(6) 4_565 4_565 ?
C8 V001 N00B 107.0(6) 4_565 . ?
C8 V001 N00B 81.5(6) . . ?
C9 V001 O1 125.8(6) . 4_565 ?
C9 V001 O1 125.8(6) 4_565 . ?
C9 V001 O1 103.2(6) 4_565 4_565 ?
C9 V001 O1 103.2(6) . . ?
C9 V001 C8 89.5(6) . 4_565 ?
C9 V001 C8 56.5(6) 4_565 4_565 ?
C9 V001 C8 89.5(6) 4_565 . ?
C9 V001 C8 56.5(6) . . ?
C9 V001 C9 37.2(9) . 4_565 ?
C9 V001 C6 88.1(6) . 4_565 ?
C9 V001 C6 77.5(6) 4_565 4_565 ?
C9 V001 N00B 154.6(6) . 4_565 ?
C9 V001 N00B 137.6(6) . . ?
C9 V001 N00B 154.6(6) 4_565 . ?
C9 V001 N00B 137.6(6) 4_565 4_565 ?
C1 V001 O5 100.5(5) 4_565 . ?
C1 V001 O5 100.5(5) . . ?
C1 V001 O1 34.4(7) . . ?
C1 V001 O1 99.1(8) 4_565 . ?
C1 V001 O1 99.1(8) . 4_565 ?
C1 V001 O1 34.4(7) 4_565 4_565 ?
C1 V001 C8 165.3(6) 4_565 . ?
C1 V001 C8 57.9(7) 4_565 4_565 ?
C1 V001 C8 165.3(6) . 4_565 ?
C1 V001 C8 57.9(7) . . ?
C1 V001 C9 97.1(7) . . ?
C1 V001 C9 133.2(7) . 4_565 ?
C1 V001 C9 97.1(7) 4_565 4_565 ?
C1 V001 C9 133.2(7) 4_565 . ?
C1 V001 C6 120.6(7) . 4_565 ?
C1 V001 C6 90.3(7) 4_565 4_565 ?
C1 V001 C1 123.1(11) 4_565 . ?
C1 V001 N00B 59.6(7) . . ?
C1 V001 N00B 59.6(7) 4_565 4_565 ?
C1 V001 N00B 87.0(7) 4_565 . ?
C1 V001 N00B 87.0(7) . 4_565 ?
N00B V001 C6 77.4(6) . 4_565 ?
N00B V001 C6 68.5(6) 4_565 4_565 ?
N00B V001 N00B 30.0(9) . 4_565 ?
O4 K002 O5 106.9(4) 3_566 . ?
O4 K002 O1 88.3(4) 3_566 2_646 ?
O4 K002 O1 88.3(4) 3_566 3_666 ?
O4 K002 C8 146.8(4) 3_566 2_646 ?
O4 K002 C8 146.8(4) 3_566 3_666 ?
O4 K002 C9 124.3(3) 3_566 3_666 ?
O4 K002 C9 124.3(3) 3_566 2_646 ?
O4 K002 C1 110.2(4) 3_566 3_666 ?
O4 K002 C1 110.2(4) 3_566 2_646 ?
O1 K002 O5 137.7(3) 3_666 . ?
O1 K002 O5 137.7(3) 2_646 . ?
O1 K002 O1 80.2(6) 2_646 3_666 ?
C8 K002 O5 95.5(4) 3_666 . ?
C8 K002 O5 95.5(4) 2_646 . ?
C8 K002 O1 59.0(5) 2_646 2_646 ?
C8 K002 O1 91.4(5) 2_646 3_666 ?
C8 K002 O1 91.4(5) 3_666 2_646 ?
C8 K002 O1 59.0(5) 3_666 3_666 ?
C8 K002 C8 49.6(7) 3_666 2_646 ?
C8 K002 C9 84.9(4) 2_646 3_666 ?
C8 K002 C9 39.1(4) 2_646 2_646 ?
C8 K002 C9 39.1(4) 3_666 3_666 ?
C8 K002 C9 84.9(4) 3_666 2_646 ?
C9 K002 O5 74.5(3) 2_646 . ?
C9 K002 O5 29.4(3) . . ?
C9 K002 O5 29.4(3) 4_565 . ?
C9 K002 O5 74.5(3) 3_666 . ?
C9 K002 O4 80.6(4) 4_565 3_566 ?
C9 K002 O4 80.6(4) . 3_566 ?
C9 K002 O1 151.2(5) 4_565 3_666 ?
C9 K002 O1 151.2(5) . 2_646 ?
C9 K002 O1 64.7(4) 3_666 3_666 ?
C9 K002 O1 64.7(4) 2_646 2_646 ?
C9 K002 O1 128.8(5) 3_666 2_646 ?
C9 K002 O1 125.5(5) 4_565 2_646 ?
C9 K002 O1 128.8(5) 2_646 3_666 ?
C9 K002 O1 125.5(5) . 3_666 ?
C9 K002 C8 124.9(4) . 2_646 ?
C9 K002 C8 112.3(4) 4_565 2_646 ?
C9 K002 C8 124.9(4) 4_565 3_666 ?
C9 K002 C8 112.3(4) . 3_666 ?
C9 K002 C9 100.1(3) 4_565 3_666 ?
C9 K002 C9 110.0(6) 3_666 2_646 ?
C9 K002 C9 78.5(5) . 3_666 ?
C9 K002 C9 100.1(3) . 2_646 ?
C9 K002 C9 26.5(7) 4_565 . ?
C9 K002 C9 78.5(5) 4_565 2_646 ?
C9 K002 C1 157.2(4) . 2_646 ?
C9 K002 C1 157.2(4) 4_565 3_666 ?
C9 K002 C1 132.8(5) 4_565 2_646 ?
C9 K002 C1 132.8(5) . 3_666 ?
C1 K002 O5 129.9(3) 3_666 . ?
C1 K002 O5 129.9(3) 2_646 . ?
C1 K002 O1 76.0(5) 3_666 2_646 ?
C1 K002 O1 76.0(5) 2_646 3_666 ?
C1 K002 O1 22.7(4) 2_646 2_646 ?
C1 K002 O1 22.7(4) 3_666 3_666 ?
C1 K002 C8 38.3(4) 2_646 2_646 ?
C1 K002 C8 70.0(5) 2_646 3_666 ?
C1 K002 C8 70.0(5) 3_666 2_646 ?
C1 K002 C8 38.3(4) 3_666 3_666 ?
C1 K002 C9 57.1(4) 3_666 3_666 ?
C1 K002 C9 108.8(4) 3_666 2_646 ?
C1 K002 C9 108.8(4) 2_646 3_666 ?
C1 K002 C9 57.1(4) 2_646 2_646 ?
C1 K002 C1 63.8(6) 2_646 3_666 ?
V001 O5 K002 128.4(5) . . ?
V001 O5 K002 92.4(2) . 3_656 ?
V001 O5 K002 92.4(2) . 3_666 ?
K002 O5 K002 92.9(2) . 3_666 ?
K002 O5 K002 167.6(4) 3_666 3_656 ?
K002 O5 K002 92.9(2) . 3_656 ?
C9 O5 V001 68.4(7) . . ?
C9 O5 V001 68.4(7) 4_565 . ?
C9 O5 K002 121.2(7) 4_565 3_666 ?
C9 O5 K002 65.2(7) 4_565 . ?
C9 O5 K002 121.2(7) . 3_656 ?
C9 O5 K002 71.2(6) . 3_666 ?
C9 O5 K002 65.2(7) . . ?
C9 O5 K002 71.2(6) 4_565 3_656 ?
C9 O5 C9 50.1(13) 4_565 . ?
C7 O4 K002 118.5(9) . 3_566 ?
C7 O4 K002 118.5(9) 4_575 3_566 ?
C7 O4 C7 116.2(18) 4_575 . ?
C6 O3 C6 54.9(18) . 4_565 ?
C6 O3 C7 47.5(10) 4_565 4_565 ?
C6 O3 C7 100.5(14) . 4_565 ?
C6 O3 C7 100.5(14) 4_565 . ?
C6 O3 C7 47.5(10) . . ?
C7 O3 C7 137.5(16) . 4_565 ?
V001 O1 K002 94.1(6) . 3_666 ?
C1 O1 V001 57.8(11) . . ?
C1 O1 K002 75.4(12) . 3_666 ?
C1 O1 C2 75.2(16) . . ?
C2 O1 V001 120.2(15) . . ?
C2 O1 K002 108.3(14) . 3_666 ?
V001 C8 K002 93.3(5) . 3_666 ?
C9 C8 V001 57.8(6) . . ?
C9 C8 K002 71.3(6) . 3_666 ?
C6 C8 V001 70.1(8) . . ?
C6 C8 K002 161.5(11) . 3_666 ?
C6 C8 C9 92.2(11) . . ?
C6 C8 C1 102.8(11) . . ?
C1 C8 V001 50.1(6) . . ?
C1 C8 K002 70.4(6) . 3_666 ?
C1 C8 C9 92.4(9) . . ?
C7 C8 V001 119.9(15) . . ?
C7 C8 K002 135.7(13) . 3_666 ?
C7 C8 C9 100.8(14) . . ?
C7 C8 C6 54.2(13) . . ?
C7 C8 C1 153.5(15) . . ?
V001 C9 K002 95.7(5) . 3_666 ?
V001 C9 K002 144.4(7) . . ?
K002 C9 K002 101.5(5) . 3_666 ?
O5 C9 V001 67.1(7) . . ?
O5 C9 K002 85.4(7) . . ?
O5 C9 K002 80.0(6) . 3_666 ?
O5 C9 C8 119.6(10) . . ?
C8 C9 V001 65.7(6) . . ?
C8 C9 K002 149.8(9) . . ?
C8 C9 K002 69.6(7) . 3_666 ?
C9 C9 V001 71.4(5) 4_565 . ?
C9 C9 K002 145.0(3) 4_565 3_666 ?
C9 C9 K002 76.8(3) 4_565 . ?
C9 C9 O5 65.0(6) 4_565 . ?
C9 C9 C8 127.4(7) 4_565 . ?
O3 C6 V001 115.5(13) . . ?
O3 C6 C8 120.9(15) . . ?
O3 C6 C7 86.6(13) . . ?
O3 C6 C0AA 90.3(14) . 4_565 ?
O3 C6 C0AA 115.0(18) . . ?
C8 C6 V001 63.7(7) . . ?
C8 C6 C0AA 146.8(12) . 4_565 ?
C6 C6 V001 73.4(5) 4_565 . ?
C6 C6 O3 62.6(9) 4_565 . ?
C6 C6 C8 133.3(8) 4_565 . ?
C6 C6 C7 144.4(11) 4_565 . ?
C6 C6 C0AA 91.6(12) 4_565 . ?
C6 C6 C0AA 49.0(9) 4_565 4_565 ?
C7 C6 V001 108.4(13) . . ?
C7 C6 C8 48.1(11) . . ?
C7 C6 C0AA 156.2(16) . 4_565 ?
C7 C6 C0AA 118.8(17) . . ?
C0AA C6 V001 94.2(10) 4_565 . ?
C0AA C6 V001 110.8(12) . . ?
C0AA C6 C8 119.5(16) . . ?
C0AA C6 C0AA 42.7(16) . 4_565 ?
V001 C1 K002 104.1(7) . 3_666 ?
V001 C1 C8 72.1(8) . . ?
V001 C1 N00B 72.5(8) . . ?
V001 C1 C3 118.4(11) . . ?
O1 C1 V001 87.8(13) . . ?
O1 C1 K002 81.9(11) . 3_666 ?
O1 C1 C8 140.7(14) . . ?
O1 C1 N00B 112.8(15) . . ?
O1 C1 C3 106.9(14) . . ?
O1 C1 C2 59.1(13) . . ?
C8 C1 K002 71.3(7) . 3_666 ?
C8 C1 N00B 93.3(9) . . ?
N00B C1 K002 164.4(8) . 3_666 ?
C3 C1 K002 136.6(10) . 3_666 ?
C3 C1 C8 112.4(10) . . ?
C3 C1 N00B 46.3(9) . . ?
C2 C1 V001 130.7(15) . . ?
C2 C1 K002 105.8(12) . 3_666 ?
C2 C1 C8 155.5(15) . . ?
C2 C1 N00B 87.0(13) . . ?
C2 C1 C3 52.4(12) . . ?
C1 N00B V001 47.9(6) . . ?
N00B N00B V001 75.0(5) 4_565 . ?
N00B N00B C1 118.1(7) 4_565 . ?
N00B N00B C4 91.4(12) 4_565 . ?
N00B N00B C4 52.7(9) 4_565 4_565 ?
N00B N00B C3 147.4(10) 4_565 . ?
C4 N00B V001 99.4(10) 4_565 . ?
C4 N00B V001 114.1(12) . . ?
C4 N00B C1 128.7(14) . . ?
C4 N00B C1 142.4(12) 4_565 . ?
C4 N00B C4 38.7(16) . 4_565 ?
C3 N00B V001 110.3(12) . . ?
C3 N00B C1 62.8(11) . . ?
C3 N00B C4 147.6(15) . 4_565 ?
C3 N00B C4 113.5(16) . . ?
C2 O2 O2 116.2(14) . 4_575 ?
N00B C4 N00B 35.9(12) . 4_565 ?
N00B C4 C0AA 103.3(17) . 4_565 ?
C4 C4 N00B 88.6(11) 4_565 . ?
C4 C4 N00B 52.7(8) 4_565 4_565 ?
C4 C4 C0AA 35.2(11) 4_565 4_565 ?
C0AA C4 N00B 116(2) . . ?
C0AA C4 N00B 113(2) . 4_565 ?
C0AA C4 N00B 72.7(14) 4_565 4_565 ?
C0AA C4 C4 95(2) . 4_565 ?
C0AA C4 C0AA 60(3) . 4_565 ?
O4 C7 O3 127.3(13) . . ?
C8 C7 O4 120.6(18) . . ?
C8 C7 O3 111.9(17) . . ?
C8 C7 C6 77.7(15) . . ?
C6 C7 O4 148.9(18) . . ?
C6 C7 O3 45.9(12) . . ?
C6 C0AA C6 39.4(13) . 4_565 ?
C6 C0AA C4 108.9(16) . 4_565 ?
C4 C0AA C6 113(2) . 4_565 ?
C4 C0AA C6 74.0(13) 4_565 4_565 ?
C4 C0AA C6 127(2) . . ?
C4 C0AA C4 50(3) . 4_565 ?
C4 C0AA C0AA 85(2) . 4_565 ?
C0AA C0AA C6 49.0(8) 4_565 4_565 ?
C0AA C0AA C6 88.4(12) 4_565 . ?
C0AA C0AA C4 35.2(11) 4_565 4_565 ?
N00B C3 C1 70.9(12) . . ?
N00B C3 C2 106.7(18) . . ?
C2 C3 C1 52.7(11) . . ?
O1 C2 K002 50.5(11) . 3_666 ?
O1 C2 C1 45.7(11) . . ?
O1 C2 C3 115.5(19) . . ?
C1 C2 K002 49.9(9) . 3_666 ?
C1 C2 C3 74.8(14) . . ?
O2 C2 K002 104.3(15) . 3_666 ?
O2 C2 O1 121(2) . . ?
O2 C2 C1 154(2) . . ?
O2 C2 C3 124(2) . . ?
C3 C2 K002 112.0(13) . 3_666 ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.441
_oxdiff_exptl_absorpt_empirical_full_min 0.569
####################################################################### 
# 
# 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_X
_database_code_depnum_ccdc_archive 'CCDC 1855755'
loop_
_audit_author_name
_audit_author_address
'Yang-Hui Luo'
;Southeast University
China
;
_audit_update_record             
;
2018-07-13 deposited with the CCDC.	2019-09-17 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C12 H16 K2 N4 O18 V2'
_chemical_formula_weight         685.38

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'
K K 0.2009 0.2494 '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'

_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                   21.717(4)
_cell_length_b                   7.8360(16)
_cell_length_c                   15.792(3)
_cell_angle_alpha                90
_cell_angle_beta                 108.90(3)
_cell_angle_gamma                90
_cell_volume                     2542.5(10)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    25
_cell_measurement_theta_min      9
_cell_measurement_theta_max      13

_exptl_crystal_description       block
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.791
_exptl_crystal_F_000             1380
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_absorpt_coefficient_mu    1.150
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_correction_T_min  0.8026
_exptl_absorpt_correction_T_max  0.8937
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Nonius CAD4'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            4677
_diffrn_reflns_av_unetI/netI     0.0556
_diffrn_reflns_av_R_equivalents  0.0582
_diffrn_reflns_limit_h_min       ?
_diffrn_reflns_limit_h_max       ?
_diffrn_reflns_limit_k_min       ?
_diffrn_reflns_limit_k_max       ?
_diffrn_reflns_limit_l_min       ?
_diffrn_reflns_limit_l_max       ?
_diffrn_reflns_theta_min         1.982
_diffrn_reflns_theta_max         25.530
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             4677
_reflns_number_gt                3275
_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-2014/7 (Sheldrick, 2014)'
_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)+(0.1035P)²+4.7446P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4677
_refine_ls_number_parameters     343
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.1081
_refine_ls_R_factor_gt           0.0753
_refine_ls_wR_factor_ref         0.2037
_refine_ls_wR_factor_gt          0.1826
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_restrained_S_all      1.077
_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
K3 K 0.56176(8) 0.9795(3) 0.91071(10) 0.0592(5) Uani 1 1 d . . . . .
O18 O 0.9261(2) 0.6999(6) 0.6180(3) 0.0412(11) Uani 1 1 d . . . . .
O9 O 0.9660(2) 0.6654(7) 0.5084(3) 0.0525(13) Uani 1 1 d . . . . .
C56 C 0.9204(3) 0.6862(8) 0.5347(4) 0.0378(15) Uani 1 1 d . . . . .
V V 0.66553(6) 1.30036(14) 0.82974(6) 0.0380(3) Uani 1 1 d . . . . .
V1 V 0.84478(5) 0.68826(12) 0.65550(6) 0.0317(3) Uani 1 1 d . . . . .
K2 K 0.94685(7) 0.99920(18) 0.84386(8) 0.0413(4) Uani 1 1 d . . . . .
O2 O 0.5601(3) 1.4266(9) 0.5779(3) 0.0755(18) Uani 1 1 d . . . . .
O5 O 0.6379(2) 1.0377(6) 0.7998(3) 0.0452(11) Uani 1 1 d . . . . .
O7 O 0.6513(3) 0.7270(7) 0.5374(3) 0.0535(13) Uani 1 1 d . . . . .
O8 O 0.7561(2) 1.2005(5) 0.8928(2) 0.0379(10) Uani 1 1 d . . . . .
O10 O 0.6578(3) 1.2611(8) 0.9430(3) 0.0687(16) Uani 1 1 d . . . . .
O12 O 0.5890(2) 1.3313(6) 0.7157(3) 0.0450(11) Uani 1 1 d . . . . .
O14 O 0.8635(3) 0.9673(5) 0.6648(3) 0.0446(12) Uani 1 1 d . . . . .
O20 O 0.8276(2) 0.4938(5) 0.6253(3) 0.0419(11) Uani 1 1 d . . . . .
O21 O 0.6911(3) 1.4897(6) 0.8322(3) 0.0537(13) Uani 1 1 d . . . . .
O22 O 0.7504(2) 0.7507(6) 0.6332(3) 0.0444(11) Uani 1 1 d . . . . .
O23 O 0.8584(2) 1.1921(5) 0.8944(3) 0.0435(11) Uani 1 1 d . . . . .
O24 O 0.9081(3) 0.6719(6) 0.7680(3) 0.0473(12) Uani 1 1 d . . . . .
O25 O 1.0344(3) 0.8489(6) 0.7511(3) 0.0541(13) Uani 1 1 d . . . . .
O26 O 0.5309(4) 0.6726(11) 0.7802(7) 0.125(3) Uani 1 1 d . U . . .
O81 O 0.5985(3) 1.3162(7) 0.8795(3) 0.0604(14) Uani 1 1 d . . . . .
O88 O 0.8444(3) 0.6948(6) 0.7720(3) 0.0522(13) Uani 1 1 d . . . . .
N1 N 0.7037(2) 1.2393(6) 0.7216(3) 0.0312(11) Uani 1 1 d . . . . .
N2 N 0.8088(3) 0.7721(6) 0.5171(3) 0.0329(12) Uani 1 1 d . . . . .
N3 N 0.8869(3) 1.1787(7) 0.5832(4) 0.0519(16) Uani 1 1 d . . . . .
H3A H 0.9115 1.2305 0.6300 0.062 Uiso 1 1 d R U . . .
H3B H 0.8814 1.2206 0.5309 0.062 Uiso 1 1 d R U . . .
N11 N 0.6182(3) 0.8274(8) 0.6937(4) 0.0597(17) Uani 1 1 d . . . . .
H11C H 0.6181 0.7523 0.7359 0.072 Uiso 1 1 d R U . . .
H11D H 0.6402 0.7846 0.6599 0.072 Uiso 1 1 d R U . . .
H11E H 0.5775 0.8491 0.6597 0.072 Uiso 1 1 d R U . . .
C1 C 0.5994(3) 1.3725(9) 0.6437(5) 0.0448(16) Uani 1 1 d . . . . .
C2 C 0.8580(3) 1.0364(7) 0.5915(4) 0.0360(14) Uani 1 1 d . . . . .
C3 C 0.8109(4) 0.9583(7) 0.5083(4) 0.0439(17) Uani 1 1 d . . . . .
H3C H 0.7678 1.0053 0.4984 0.053 Uiso 1 1 calc R U . . .
H3D H 0.8242 0.9867 0.4570 0.053 Uiso 1 1 calc R U . . .
C4 C 0.6707(3) 1.3591(9) 0.6501(4) 0.0430(16) Uani 1 1 d . . . . .
H4A H 0.6741 1.3194 0.5936 0.052 Uiso 1 1 calc R U . . .
H4B H 0.6912 1.4705 0.6628 0.052 Uiso 1 1 calc R U . . .
C5 C 0.7106(4) 0.7339(8) 0.5519(4) 0.0409(16) Uani 1 1 d . . . . .
C6 C 0.6465(3) 0.9715(8) 0.7320(4) 0.0368(14) Uani 1 1 d . . . . .
C7 C 0.8516(3) 0.6857(8) 0.4735(4) 0.0347(14) Uani 1 1 d . . . . .
H7A H 0.8488 0.7440 0.4182 0.042 Uiso 1 1 d R U . . .
H7B H 0.8371 0.5689 0.4590 0.042 Uiso 1 1 d R U . . .
C9 C 0.7410(3) 0.7059(9) 0.4806(4) 0.0393(15) Uani 1 1 d . . . . .
H9A H 0.7412 0.5853 0.4667 0.047 Uiso 1 1 calc R U . . .
H9B H 0.7171 0.7668 0.4265 0.047 Uiso 1 1 calc R U . . .
C10 C 0.6918(4) 1.0620(8) 0.6930(4) 0.0384(15) Uani 1 1 d . . . . .
H10A H 0.7330 1.0016 0.7102 0.046 Uiso 1 1 calc R U . . .
H10B H 0.6736 1.0587 0.6283 0.046 Uiso 1 1 calc R U . . .
C11 C 0.7766(3) 1.2725(8) 0.7597(3) 0.0355(14) Uani 1 1 d . . . . .
H11A H 0.7993 1.2097 0.7259 0.043 Uiso 1 1 calc R U . . .
H11B H 0.7855 1.3931 0.7562 0.043 Uiso 1 1 calc R U . . .
C35 C 0.7993(4) 1.2144(8) 0.8563(4) 0.0442(17) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
K3 O2 2.741(6) 2_646 ?
K3 O2 2.752(5) 4_586 ?
K3 O7 2.807(5) 4_576 ?
K3 O5 2.808(4) . ?
K3 O81 2.845(6) . ?
K3 O10 2.964(7) . ?
K3 O26 3.097(10) . ?
K3 O26 3.390(11) 2_656 ?
K3 C1 3.426(7) 2_646 ?
K3 V 3.860(2) . ?
K3 K3 4.489(3) 3_677 ?
O18 C56 1.286(6) . ?
O18 V1 2.038(5) . ?
O18 K2 3.062(5) 2_746 ?
O9 C56 1.202(8) . ?
O9 K2 2.804(5) 2_746 ?
O9 K2 2.808(5) 4_575 ?
C56 C7 1.495(9) . ?
C56 K2 3.249(7) 2_746 ?
V O21 1.580(5) . ?
V O81 1.870(5) . ?
V O10 1.876(4) . ?
V O12 2.032(5) . ?
V O8 2.050(5) . ?
V O5 2.153(5) . ?
V N1 2.179(4) . ?
V1 O20 1.604(4) . ?
V1 O88 1.843(4) . ?
V1 O24 1.865(5) . ?
V1 O22 2.024(5) . ?
V1 N2 2.170(4) . ?
V1 O14 2.220(4) . ?
V1 K2 3.9277(19) . ?
K2 O23 2.758(5) . ?
K2 O9 2.804(5) 2_756 ?
K2 O9 2.808(5) 4_576 ?
K2 O14 2.832(5) . ?
K2 O24 2.840(5) . ?
K2 O25 2.992(5) . ?
K2 O18 3.062(5) 2_756 ?
K2 O88 3.208(6) . ?
K2 O25 3.212(5) 2_756 ?
K2 C56 3.249(7) 2_756 ?
K2 K2 4.720(3) 3_777 ?
O2 C1 1.189(8) . ?
O2 K3 2.741(6) 2_656 ?
O2 K3 2.752(5) 4_585 ?
O5 C6 1.257(7) . ?
O7 C5 1.235(8) . ?
O7 K3 2.808(5) 4_575 ?
O8 C35 1.257(8) . ?
O10 O81 1.420(8) . ?
O12 C1 1.270(7) . ?
O14 C2 1.247(7) . ?
O22 C5 1.302(8) . ?
O23 C35 1.239(8) . ?
O24 O88 1.416(7) . ?
O25 K2 3.212(5) 2_746 ?
O26 K3 3.390(11) 2_646 ?
N1 C10 1.457(7) . ?
N1 C4 1.466(7) . ?
N1 C11 1.522(8) . ?
N2 C3 1.468(7) . ?
N2 C7 1.487(7) . ?
N2 C9 1.489(8) . ?
N3 C2 1.308(8) . ?
N3 H3A 0.8600 . ?
N3 H3B 0.8599 . ?
N11 C6 1.334(8) . ?
N11 H11C 0.8900 . ?
N11 H11D 0.8901 . ?
N11 H11E 0.8900 . ?
C1 C4 1.523(9) . ?
C1 K3 3.426(7) 2_656 ?
C2 C3 1.509(9) . ?
C3 H3C 0.9700 . ?
C3 H3D 0.9700 . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C5 C9 1.495(8) . ?
C6 C10 1.497(9) . ?
C7 H7A 0.9699 . ?
C7 H7B 0.9700 . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C11 C35 1.512(8) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 K3 O2 70.38(18) 2_646 4_586 ?
O2 K3 O7 109.03(18) 2_646 4_576 ?
O2 K3 O7 72.04(18) 4_586 4_576 ?
O2 K3 O5 147.28(16) 2_646 . ?
O2 K3 O5 138.47(17) 4_586 . ?
O7 K3 O5 97.29(15) 4_576 . ?
O2 K3 O81 118.8(2) 2_646 . ?
O2 K3 O81 90.58(18) 4_586 . ?
O7 K3 O81 119.35(17) 4_576 . ?
O5 K3 O81 59.12(14) . . ?
O2 K3 O10 137.85(19) 2_646 . ?
O2 K3 O10 82.14(16) 4_586 . ?
O7 K3 O10 91.17(17) 4_576 . ?
O5 K3 O10 57.54(13) . . ?
O81 K3 O10 28.20(16) . . ?
O2 K3 O26 85.5(2) 2_646 . ?
O2 K3 O26 141.2(2) 4_586 . ?
O7 K3 O26 88.7(2) 4_576 . ?
O5 K3 O26 75.82(17) . . ?
O81 K3 O26 128.11(18) . . ?
O10 K3 O26 132.95(17) . . ?
O2 K3 O26 79.55(18) 2_646 2_656 ?
O2 K3 O26 123.0(2) 4_586 2_656 ?
O7 K3 O26 164.89(17) 4_576 2_656 ?
O5 K3 O26 70.87(16) . 2_656 ?
O81 K3 O26 63.30(18) . 2_656 ?
O10 K3 O26 90.14(18) . 2_656 ?
O26 K3 O26 79.42(11) . 2_656 ?
O2 K3 C1 18.25(15) 2_646 2_646 ?
O2 K3 C1 88.63(17) 4_586 2_646 ?
O7 K3 C1 116.92(17) 4_576 2_646 ?
O5 K3 C1 130.01(16) . 2_646 ?
O81 K3 C1 120.28(18) . 2_646 ?
O10 K3 C1 146.07(19) . 2_646 ?
O26 K3 C1 70.09(19) . 2_646 ?
O26 K3 C1 67.83(18) 2_656 2_646 ?
O2 K3 V 143.11(17) 2_646 . ?
O2 K3 V 109.53(15) 4_586 . ?
O7 K3 V 105.54(12) 4_576 . ?
O5 K3 V 33.16(10) . . ?
O81 K3 V 27.40(10) . . ?
O10 K3 V 28.20(8) . . ?
O26 K3 V 108.01(14) . . ?
O26 K3 V 69.92(13) 2_656 . ?
C1 K3 V 137.29(13) 2_646 . ?
O2 K3 K3 35.27(11) 2_646 3_677 ?
O2 K3 K3 35.11(11) 4_586 3_677 ?
O7 K3 K3 90.58(11) 4_576 3_677 ?
O5 K3 K3 166.56(13) . 3_677 ?
O81 K3 K3 107.50(12) . 3_677 ?
O10 K3 K3 111.64(11) . 3_677 ?
O26 K3 K3 115.40(15) . 3_677 ?
O26 K3 K3 102.91(14) 2_656 3_677 ?
C1 K3 K3 53.52(12) 2_646 3_677 ?
V K3 K3 133.90(8) . 3_677 ?
C56 O18 V1 119.3(4) . . ?
C56 O18 K2 86.5(4) . 2_746 ?
V1 O18 K2 136.92(18) . 2_746 ?
C56 O9 K2 100.6(4) . 2_746 ?
C56 O9 K2 119.4(4) . 4_575 ?
K2 O9 K2 114.48(17) 2_746 4_575 ?
O9 C56 O18 123.3(6) . . ?
O9 C56 C7 122.6(5) . . ?
O18 C56 C7 113.9(5) . . ?
O9 C56 K2 58.0(3) . 2_746 ?
O18 C56 K2 70.2(3) . 2_746 ?
C7 C56 K2 153.0(4) . 2_746 ?
O21 V O81 104.1(3) . . ?
O21 V O10 105.7(3) . . ?
O81 V O10 44.6(2) . . ?
O21 V O12 95.2(2) . . ?
O81 V O12 80.8(2) . . ?
O10 V O12 124.4(2) . . ?
O21 V O8 94.1(2) . . ?
O81 V O8 125.2(2) . . ?
O10 V O8 80.9(2) . . ?
O12 V O8 148.99(17) . . ?
O21 V O5 166.8(2) . . ?
O81 V O5 87.5(2) . . ?
O10 V O5 87.0(2) . . ?
O12 V O5 80.16(19) . . ?
O8 V O5 84.11(18) . . ?
O21 V N1 90.3(2) . . ?
O81 V N1 152.8(2) . . ?
O10 V N1 152.3(2) . . ?
O12 V N1 75.02(18) . . ?
O8 V N1 75.41(17) . . ?
O5 V N1 76.57(17) . . ?
O21 V K3 147.32(18) . . ?
O81 V K3 44.46(18) . . ?
O10 V K3 48.3(2) . . ?
O12 V K3 88.48(14) . . ?
O8 V K3 99.29(12) . . ?
O5 V K3 45.50(11) . . ?
N1 V K3 121.85(14) . . ?
O20 V1 O88 104.3(2) . . ?
O20 V1 O24 104.3(2) . . ?
O88 V1 O24 44.9(2) . . ?
O20 V1 O22 93.0(2) . . ?
O88 V1 O22 80.5(2) . . ?
O24 V1 O22 125.10(18) . . ?
O20 V1 O18 95.5(2) . . ?
O88 V1 O18 125.0(2) . . ?
O24 V1 O18 80.72(19) . . ?
O22 V1 O18 149.59(17) . . ?
O20 V1 N2 90.84(19) . . ?
O88 V1 N2 151.6(2) . . ?
O24 V1 N2 153.3(2) . . ?
O22 V1 N2 74.78(18) . . ?
O18 V1 N2 75.96(18) . . ?
O20 V1 O14 167.20(17) . . ?
O88 V1 O14 88.07(19) . . ?
O24 V1 O14 86.67(19) . . ?
O22 V1 O14 85.79(19) . . ?
O18 V1 O14 79.53(18) . . ?
N2 V1 O14 76.53(17) . . ?
O20 V1 K2 146.56(16) . . ?
O88 V1 K2 53.88(17) . . ?
O24 V1 K2 42.30(15) . . ?
O22 V1 K2 105.85(13) . . ?
O18 V1 K2 82.12(12) . . ?
N2 V1 K2 120.38(14) . . ?
O14 V1 K2 44.98(11) . . ?
O23 K2 O9 81.40(15) . 2_756 ?
O23 K2 O9 83.81(14) . 4_576 ?
O9 K2 O9 65.52(17) 2_756 4_576 ?
O23 K2 O14 93.28(14) . . ?
O9 K2 O14 155.91(14) 2_756 . ?
O9 K2 O14 137.59(15) 4_576 . ?
O23 K2 O24 118.56(15) . . ?
O9 K2 O24 142.97(15) 2_756 . ?
O9 K2 O24 84.87(14) 4_576 . ?
O14 K2 O24 59.52(13) . . ?
O23 K2 O25 165.97(14) . . ?
O9 K2 O25 103.03(15) 2_756 . ?
O9 K2 O25 110.19(15) 4_576 . ?
O14 K2 O25 77.21(14) . . ?
O24 K2 O25 65.56(13) . . ?
O23 K2 O18 109.26(14) . 2_756 ?
O9 K2 O18 43.56(12) 2_756 2_756 ?
O9 K2 O18 101.54(14) 4_576 2_756 ?
O14 K2 O18 119.06(13) . 2_756 ?
O24 K2 O18 132.18(14) . 2_756 ?
O25 K2 O18 67.87(13) . 2_756 ?
O23 K2 O88 92.39(14) . . ?
O9 K2 O88 147.52(13) 2_756 . ?
O9 K2 O88 82.17(13) 4_576 . ?
O14 K2 O88 55.61(12) . . ?
O24 K2 O88 26.19(13) . . ?
O25 K2 O88 90.67(13) . . ?
O18 K2 O88 158.27(13) 2_756 . ?
O23 K2 O25 82.72(13) . 2_756 ?
O9 K2 O25 80.73(13) 2_756 2_756 ?
O9 K2 O25 145.13(14) 4_576 2_756 ?
O14 K2 O25 75.28(13) . 2_756 ?
O24 K2 O25 129.65(12) . 2_756 ?
O25 K2 O25 84.86(8) . 2_756 ?
O18 K2 O25 53.93(13) 2_756 2_756 ?
O88 K2 O25 130.34(12) . 2_756 ?
O23 K2 C56 98.63(15) . 2_756 ?
O9 K2 C56 21.32(13) 2_756 2_756 ?
O9 K2 C56 79.86(15) 4_576 2_756 ?
O14 K2 C56 141.94(15) . 2_756 ?
O24 K2 C56 137.84(16) . 2_756 ?
O25 K2 C56 83.32(14) . 2_756 ?
O18 K2 C56 23.27(12) 2_756 2_756 ?
O88 K2 C56 157.72(15) . 2_756 ?
O25 K2 C56 70.63(15) 2_756 2_756 ?
O23 K2 V1 106.49(11) . . ?
O9 K2 V1 168.99(12) 2_756 . ?
O9 K2 V1 107.09(11) 4_576 . ?
O14 K2 V1 33.65(9) . . ?
O24 K2 V1 26.23(9) . . ?
O25 K2 V1 71.17(10) . . ?
O18 K2 V1 135.98(9) 2_756 . ?
O88 K2 V1 27.64(7) . . ?
O25 K2 V1 107.54(9) 2_756 . ?
C56 K2 V1 154.44(11) 2_756 . ?
O23 K2 K2 81.20(10) . 3_777 ?
O9 K2 K2 32.79(10) 2_756 3_777 ?
O9 K2 K2 32.74(10) 4_576 3_777 ?
O14 K2 K2 169.03(12) . 3_777 ?
O24 K2 K2 114.91(10) . 3_777 ?
O25 K2 K2 109.83(11) . 3_777 ?
O18 K2 K2 71.85(8) 2_756 3_777 ?
O88 K2 K2 114.85(9) . 3_777 ?
O25 K2 K2 113.11(10) 2_756 3_777 ?
C56 K2 K2 48.83(10) 2_756 3_777 ?
V1 K2 K2 139.29(6) . 3_777 ?
C1 O2 K3 115.5(4) . 2_656 ?
C1 O2 K3 134.8(5) . 4_585 ?
K3 O2 K3 109.62(18) 2_656 4_585 ?
C6 O5 V 118.3(4) . . ?
C6 O5 K3 138.2(4) . . ?
V O5 K3 101.34(16) . . ?
C5 O7 K3 126.7(4) . 4_575 ?
C35 O8 V 119.1(4) . . ?
O81 O10 V 67.5(3) . . ?
O81 O10 K3 71.2(3) . . ?
V O10 K3 103.5(2) . . ?
C1 O12 V 119.5(4) . . ?
C2 O14 V1 113.9(4) . . ?
C2 O14 K2 136.5(4) . . ?
V1 O14 K2 101.36(15) . . ?
C5 O22 V1 117.3(4) . . ?
C35 O23 K2 130.1(4) . . ?
O88 O24 V1 66.7(3) . . ?
O88 O24 K2 91.5(3) . . ?
V1 O24 K2 111.48(19) . . ?
K2 O25 K2 139.57(17) . 2_746 ?
K3 O26 K3 151.3(3) . 2_646 ?
O10 O81 V 68.0(3) . . ?
O10 O81 K3 80.6(3) . . ?
V O81 K3 108.1(2) . . ?
O24 O88 V1 68.4(2) . . ?
O24 O88 K2 62.3(3) . . ?
V1 O88 K2 98.5(2) . . ?
C10 N1 C4 112.2(5) . . ?
C10 N1 C11 110.1(5) . . ?
C4 N1 C11 112.4(5) . . ?
C10 N1 V 112.2(3) . . ?
C4 N1 V 104.3(4) . . ?
C11 N1 V 105.3(3) . . ?
C3 N2 C7 111.4(5) . . ?
C3 N2 C9 111.5(5) . . ?
C7 N2 C9 110.4(4) . . ?
C3 N2 V1 112.6(3) . . ?
C7 N2 V1 104.7(3) . . ?
C9 N2 V1 105.9(3) . . ?
C2 N3 H3A 120.1 . . ?
C2 N3 H3B 119.9 . . ?
H3A N3 H3B 120.0 . . ?
C6 N11 H11C 109.5 . . ?
C6 N11 H11D 109.4 . . ?
H11C N11 H11D 109.5 . . ?
C6 N11 H11E 109.5 . . ?
H11C N11 H11E 109.5 . . ?
H11D N11 H11E 109.5 . . ?
O2 C1 O12 126.0(6) . . ?
O2 C1 C4 120.6(6) . . ?
O12 C1 C4 113.2(6) . . ?
O2 C1 K3 46.2(4) . 2_656 ?
O12 C1 K3 79.9(4) . 2_656 ?
C4 C1 K3 165.4(4) . 2_656 ?
O14 C2 N3 124.0(6) . . ?
O14 C2 C3 117.8(5) . . ?
N3 C2 C3 118.1(5) . . ?
N2 C3 C2 110.7(5) . . ?
N2 C3 H3C 109.5 . . ?
C2 C3 H3C 109.5 . . ?
N2 C3 H3D 109.5 . . ?
C2 C3 H3D 109.5 . . ?
H3C C3 H3D 108.1 . . ?
N1 C4 C1 109.2(5) . . ?
N1 C4 H4A 109.8 . . ?
C1 C4 H4A 109.8 . . ?
N1 C4 H4B 109.8 . . ?
C1 C4 H4B 109.8 . . ?
H4A C4 H4B 108.3 . . ?
O7 C5 O22 120.4(6) . . ?
O7 C5 C9 122.9(6) . . ?
O22 C5 C9 116.3(6) . . ?
O5 C6 N11 124.1(6) . . ?
O5 C6 C10 117.0(5) . . ?
N11 C6 C10 118.9(5) . . ?
N2 C7 C56 110.1(5) . . ?
N2 C7 H7A 109.7 . . ?
C56 C7 H7A 109.7 . . ?
N2 C7 H7B 109.6 . . ?
C56 C7 H7B 109.5 . . ?
H7A C7 H7B 108.2 . . ?
N2 C9 C5 106.2(5) . . ?
N2 C9 H9A 110.5 . . ?
C5 C9 H9A 110.5 . . ?
N2 C9 H9B 110.5 . . ?
C5 C9 H9B 110.5 . . ?
H9A C9 H9B 108.7 . . ?
N1 C10 C6 113.5(5) . . ?
N1 C10 H10A 108.9 . . ?
C6 C10 H10A 108.9 . . ?
N1 C10 H10B 108.9 . . ?
C6 C10 H10B 108.9 . . ?
H10A C10 H10B 107.7 . . ?
C35 C11 N1 107.8(5) . . ?
C35 C11 H11A 110.2 . . ?
N1 C11 H11A 110.2 . . ?
C35 C11 H11B 110.2 . . ?
N1 C11 H11B 110.2 . . ?
H11A C11 H11B 108.5 . . ?
O23 C35 O8 125.0(6) . . ?
O23 C35 C11 118.7(6) . . ?
O8 C35 C11 116.1(6) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
K2 O9 C56 O18 27.4(7) 2_746 . . . ?
K2 O9 C56 O18 153.5(5) 4_575 . . . ?
K2 O9 C56 C7 -147.9(5) 2_746 . . . ?
K2 O9 C56 C7 -21.8(8) 4_575 . . . ?
K2 O9 C56 K2 126.1(4) 4_575 . . 2_746 ?
V1 O18 C56 O9 -168.1(5) . . . . ?
K2 O18 C56 O9 -24.5(6) 2_746 . . . ?
V1 O18 C56 C7 7.6(7) . . . . ?
K2 O18 C56 C7 151.2(5) 2_746 . . . ?
V1 O18 C56 K2 -143.6(3) . . . 2_746 ?
O21 V O10 O81 94.3(4) . . . . ?
O12 V O10 O81 -13.5(5) . . . . ?
O8 V O10 O81 -173.9(4) . . . . ?
O5 V O10 O81 -89.4(4) . . . . ?
N1 V O10 O81 -142.6(5) . . . . ?
K3 V O10 O81 -62.8(3) . . . . ?
O21 V O10 K3 157.1(2) . . . . ?
O81 V O10 K3 62.8(3) . . . . ?
O12 V O10 K3 49.3(3) . . . . ?
O8 V O10 K3 -111.2(2) . . . . ?
O5 V O10 K3 -26.7(2) . . . . ?
N1 V O10 K3 -79.8(5) . . . . ?
O20 V1 O24 O88 -96.1(3) . . . . ?
O22 V1 O24 O88 8.1(4) . . . . ?
O18 V1 O24 O88 170.5(3) . . . . ?
N2 V1 O24 O88 141.2(4) . . . . ?
O14 V1 O24 O88 90.6(3) . . . . ?
K2 V1 O24 O88 82.1(3) . . . . ?
O20 V1 O24 K2 -178.1(2) . . . . ?
O88 V1 O24 K2 -82.1(3) . . . . ?
O22 V1 O24 K2 -73.9(3) . . . . ?
O18 V1 O24 K2 88.5(2) . . . . ?
N2 V1 O24 K2 59.1(5) . . . . ?
O14 V1 O24 K2 8.5(2) . . . . ?
K3 O10 O81 V -114.06(19) . . . . ?
V O10 O81 K3 114.06(19) . . . . ?
O21 V O81 O10 -98.2(4) . . . . ?
O12 V O81 O10 168.8(4) . . . . ?
O8 V O81 O10 7.3(5) . . . . ?
O5 V O81 O10 88.3(4) . . . . ?
N1 V O81 O10 141.8(5) . . . . ?
K3 V O81 O10 71.4(3) . . . . ?
O21 V O81 K3 -169.6(2) . . . . ?
O10 V O81 K3 -71.4(3) . . . . ?
O12 V O81 K3 97.3(2) . . . . ?
O8 V O81 K3 -64.1(3) . . . . ?
O5 V O81 K3 16.9(2) . . . . ?
N1 V O81 K3 70.4(5) . . . . ?
K2 O24 O88 V1 112.78(16) . . . . ?
V1 O24 O88 K2 -112.78(16) . . . . ?
O20 V1 O88 O24 96.0(3) . . . . ?
O22 V1 O88 O24 -173.3(3) . . . . ?
O18 V1 O88 O24 -11.4(4) . . . . ?
N2 V1 O88 O24 -143.6(4) . . . . ?
O14 V1 O88 O24 -87.2(3) . . . . ?
K2 V1 O88 O24 -55.6(3) . . . . ?
O20 V1 O88 K2 151.6(2) . . . . ?
O24 V1 O88 K2 55.6(3) . . . . ?
O22 V1 O88 K2 -117.68(19) . . . . ?
O18 V1 O88 K2 44.2(3) . . . . ?
N2 V1 O88 K2 -88.0(5) . . . . ?
O14 V1 O88 K2 -31.62(17) . . . . ?
K3 O2 C1 O12 3.2(11) 2_656 . . . ?
K3 O2 C1 O12 -178.0(5) 4_585 . . . ?
K3 O2 C1 C4 -172.1(5) 2_656 . . . ?
K3 O2 C1 C4 6.7(12) 4_585 . . . ?
K3 O2 C1 K3 178.8(11) 4_585 . . 2_656 ?
V O12 C1 O2 -164.3(7) . . . . ?
V O12 C1 C4 11.4(8) . . . . ?
V O12 C1 K3 -161.9(3) . . . 2_656 ?
V1 O14 C2 N3 -155.6(6) . . . . ?
K2 O14 C2 N3 -14.3(11) . . . . ?
V1 O14 C2 C3 29.6(7) . . . . ?
K2 O14 C2 C3 170.9(4) . . . . ?
C7 N2 C3 C2 -97.2(6) . . . . ?
C9 N2 C3 C2 138.8(5) . . . . ?
V1 N2 C3 C2 20.0(7) . . . . ?
O14 C2 C3 N2 -33.9(9) . . . . ?
N3 C2 C3 N2 151.0(6) . . . . ?
C10 N1 C4 C1 79.8(6) . . . . ?
C11 N1 C4 C1 -155.4(5) . . . . ?
V N1 C4 C1 -41.8(6) . . . . ?
O2 C1 C4 N1 -161.0(7) . . . . ?
O12 C1 C4 N1 23.1(8) . . . . ?
K3 C1 C4 N1 175.9(16) 2_656 . . . ?
K3 O7 C5 O22 -141.9(5) 4_575 . . . ?
K3 O7 C5 C9 31.6(9) 4_575 . . . ?
V1 O22 C5 O7 161.5(5) . . . . ?
V1 O22 C5 C9 -12.4(7) . . . . ?
V O5 C6 N11 -163.3(6) . . . . ?
K3 O5 C6 N11 -4.1(11) . . . . ?
V O5 C6 C10 16.9(8) . . . . ?
K3 O5 C6 C10 176.1(4) . . . . ?
C3 N2 C7 C56 81.9(6) . . . . ?
C9 N2 C7 C56 -153.5(5) . . . . ?
V1 N2 C7 C56 -40.0(5) . . . . ?
O9 C56 C7 N2 -160.3(6) . . . . ?
O18 C56 C7 N2 23.9(7) . . . . ?
K2 C56 C7 N2 117.0(7) 2_746 . . . ?
C3 N2 C9 C5 -80.8(6) . . . . ?
C7 N2 C9 C5 154.7(5) . . . . ?
V1 N2 C9 C5 41.9(5) . . . . ?
O7 C5 C9 N2 164.4(6) . . . . ?
O22 C5 C9 N2 -21.9(7) . . . . ?
C4 N1 C10 C6 -106.9(6) . . . . ?
C11 N1 C10 C6 127.1(6) . . . . ?
V N1 C10 C6 10.2(7) . . . . ?
O5 C6 C10 N1 -18.0(9) . . . . ?
N11 C6 C10 N1 162.2(6) . . . . ?
C10 N1 C11 C35 -82.8(5) . . . . ?
C4 N1 C11 C35 151.3(5) . . . . ?
V N1 C11 C35 38.3(5) . . . . ?
K2 O23 C35 O8 130.9(5) . . . . ?
K2 O23 C35 C11 -52.7(8) . . . . ?
V O8 C35 O23 164.4(5) . . . . ?
V O8 C35 C11 -12.1(7) . . . . ?
N1 C11 C35 O23 163.4(5) . . . . ?
N1 C11 C35 O8 -19.9(7) . . . . ?

_refine_diff_density_max         0.861
_refine_diff_density_min         -0.825
_refine_diff_density_rms         0.117

