# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2023

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_1
_database_code_depnum_ccdc_archive 'CCDC 2155582'
loop_
_audit_author_name
_audit_author_address
'Ashutosh Ghosh' 'University of Calcutta'
_audit_update_record             
;
2023-01-30 deposited with the CCDC.	2023-02-01 downloaded from the CCDC.
;
_audit_creation_date             2023-01-30
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2016/6
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C20 H22 N2 O5 V, 1.78(H2 O)'
_chemical_formula_sum            'C20 H25.56 N2 O6.78 V'
_chemical_formula_weight         453.4
_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'
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'
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           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
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                   10.1320(15)
_cell_length_b                   19.209(2)
_cell_length_c                   10.8529(15)
_cell_angle_alpha                90
_cell_angle_beta                 105.233(5)
_cell_angle_gamma                90
_cell_volume                     2038.0(5)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9447
_cell_measurement_temperature    132(2)
_cell_measurement_theta_max      26.46
_cell_measurement_theta_min      2.34
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.531
_exptl_absorpt_correction_T_max  0.913
_exptl_absorpt_correction_T_min  0.798
_exptl_absorpt_correction_type   EMPIRICAL
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            GREEN
_exptl_crystal_density_diffrn    1.478
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             947.2
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.18
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0584
_diffrn_reflns_av_unetI/netI     0.0525
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            15069
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.481
_diffrn_reflns_theta_min         2.338
_diffrn_ambient_temperature      132.19
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3483
_reflns_number_total             4163
_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       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         0.636
_refine_diff_density_min         -0.699
_refine_diff_density_rms         0.083
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     275
_refine_ls_number_reflns         4163
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0653
_refine_ls_R_factor_gt           0.0539
_refine_ls_restrained_S_all      1.020
_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)+(0.0698P)²+3.0929P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1359
_refine_ls_wR_factor_ref         0.1473
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Others
 Fixed Sof: O52(0.78) H52A(0.78) H52B(0.78)
3.a Free rotating group:
 O52(H52A,H52B,O51,H51A,H51B)
3.b Secondary CH2 refined with riding coordinates:
 C21(H21A,H21B)
3.c Aromatic/amide H refined with riding coordinates:
 C23(H23), C18(H18), C27(H27), C25(H25), C14(H14), C26(H26), C16(H16), C15(H15)
3.d Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C32(H32A,H32B,H32C), C2(H2A,H2B,H2C), C42(H42A,H42B,H42C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
V1 V 0.45855(4) 0.39549(2) 0.60397(4) 0.02124(16) Uani 1 1 d . . . . .
O30 O 0.49235(18) 0.48375(10) 0.69376(19) 0.0252(4) Uani 1 1 d . . . . .
O11 O 0.65251(18) 0.38673(10) 0.62714(19) 0.0269(4) Uani 1 1 d . . . . .
O31 O 0.5535(2) 0.55556(11) 0.90680(19) 0.0303(5) Uani 1 1 d . . . . .
O1 O 0.4055(2) 0.34524(10) 0.69823(19) 0.0309(5) Uani 1 1 d . . . . .
O41 O 0.9143(2) 0.38547(11) 0.7268(2) 0.0355(5) Uani 1 1 d . . . . .
N22 N 0.2939(2) 0.44342(11) 0.4821(2) 0.0234(5) Uani 1 1 d . . . . .
N19 N 0.4318(2) 0.33668(11) 0.4392(2) 0.0240(5) Uani 1 1 d . . . . .
C29 C 0.3961(3) 0.52557(13) 0.7141(3) 0.0231(5) Uani 1 1 d . . . . .
C24 C 0.2654(3) 0.53325(13) 0.6287(3) 0.0241(6) Uani 1 1 d . . . . .
C23 C 0.2280(3) 0.49603(14) 0.5101(3) 0.0256(6) Uani 1 1 d . . . . .
H23 H 0.148821 0.511182 0.447580 0.031 Uiso 1 1 calc R . . . .
C12 C 0.7217(3) 0.33803(14) 0.5829(3) 0.0258(6) Uani 1 1 d . . . . .
C21 C 0.2514(3) 0.41599(15) 0.3512(3) 0.0270(6) Uani 1 1 d . . . . .
H21A H 0.298275 0.441750 0.295880 0.032 Uiso 1 1 calc R . . . .
H21B H 0.151481 0.421884 0.316070 0.032 Uiso 1 1 calc R . . . .
C17 C 0.6632(3) 0.29176(14) 0.4830(3) 0.0276(6) Uani 1 1 d . . . . .
C28 C 0.4257(3) 0.56641(14) 0.8273(3) 0.0264(6) Uani 1 1 d . . . . .
C18 C 0.5220(3) 0.29625(14) 0.4119(3) 0.0270(6) Uani 1 1 d . . . . .
H18 H 0.492728 0.267166 0.339003 0.032 Uiso 1 1 calc R . . . .
C1 C 0.1961(3) 0.29611(15) 0.4161(3) 0.0297(6) Uani 1 1 d . . . . .
H1A H 0.226901 0.247560 0.423980 0.045 Uiso 1 1 calc GR . . . .
H1B H 0.101623 0.298379 0.362944 0.045 Uiso 1 1 calc GR . . . .
H1C H 0.200533 0.314907 0.501003 0.045 Uiso 1 1 calc GR . . . .
C20 C 0.2886(3) 0.33905(15) 0.3540(3) 0.0262(6) Uani 1 1 d . . . . .
C13 C 0.8652(3) 0.33505(15) 0.6376(3) 0.0291(6) Uani 1 1 d . . . . .
C32 C 0.5861(3) 0.59160(17) 1.0270(3) 0.0368(7) Uani 1 1 d . . . . .
H32A H 0.585039 0.641922 1.011851 0.055 Uiso 1 1 calc GR . . . .
H32B H 0.677164 0.577510 1.077578 0.055 Uiso 1 1 calc GR . . . .
H32C H 0.518203 0.579972 1.073536 0.055 Uiso 1 1 calc GR . . . .
C2 C 0.2769(3) 0.31437(16) 0.2178(3) 0.0321(6) Uani 1 1 d . . . . .
H2A H 0.346815 0.337431 0.184826 0.048 Uiso 1 1 calc GR . . . .
H2B H 0.185928 0.325982 0.163529 0.048 Uiso 1 1 calc GR . . . .
H2C H 0.290257 0.263844 0.217694 0.048 Uiso 1 1 calc GR . . . .
C27 C 0.3295(3) 0.61127(15) 0.8522(3) 0.0326(7) Uani 1 1 d . . . . .
H27 H 0.350733 0.637391 0.929272 0.039 Uiso 1 1 calc R . . . .
C25 C 0.1693(3) 0.58072(15) 0.6553(3) 0.0318(6) Uani 1 1 d . . . . .
H25 H 0.082285 0.586110 0.596174 0.038 Uiso 1 1 calc R . . . .
C14 C 0.9439(3) 0.28526(16) 0.5974(3) 0.0344(7) Uani 1 1 d . . . . .
H14 H 1.039486 0.283069 0.635990 0.041 Uiso 1 1 calc R . . . .
C26 C 0.2012(3) 0.61875(17) 0.7656(3) 0.0368(7) Uani 1 1 d . . . . .
H26 H 0.136279 0.650252 0.783272 0.044 Uiso 1 1 calc R . . . .
C16 C 0.7470(3) 0.24224(15) 0.4421(3) 0.0334(7) Uani 1 1 d . . . . .
H16 H 0.707540 0.211656 0.373568 0.040 Uiso 1 1 calc R . . . .
C15 C 0.8836(3) 0.23821(16) 0.5004(3) 0.0376(7) Uani 1 1 d . . . . .
H15 H 0.937829 0.203453 0.475086 0.045 Uiso 1 1 calc R . . . .
C42 C 1.0589(3) 0.39370(18) 0.7705(4) 0.0446(9) Uani 1 1 d . . . . .
H42A H 1.098851 0.352583 0.819827 0.067 Uiso 1 1 calc GR . . . .
H42B H 1.080052 0.435169 0.824709 0.067 Uiso 1 1 calc GR . . . .
H42C H 1.097211 0.399000 0.696985 0.067 Uiso 1 1 calc GR . . . .
O52 O 0.9685(3) 0.57600(15) 0.9296(3) 0.0578(9) Uani 0.78 1 d . . P . .
H52A H 1.048009 0.559707 0.970637 0.087 Uiso 0.78 1 d G . P . .
H52B H 0.914310 0.540101 0.918939 0.087 Uiso 0.78 1 d G . P . .
O51 O 0.7744(2) 0.45913(11) 0.8885(2) 0.0414(5) Uani 1 1 d G . . . .
H51A H 0.705426 0.487624 0.867226 0.062 Uiso 1 1 d G . . . .
H51B H 0.773342 0.437000 0.818323 0.062 Uiso 1 1 d G . . . .


_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 O30 1.9406(19) . ?
V1 O11 1.9219(19) . ?
V1 O1 1.599(2) . ?
V1 N22 2.055(2) . ?
V1 N19 2.072(2) . ?
O30 C29 1.326(3) . ?
O11 C12 1.332(3) . ?
O31 C28 1.371(3) . ?
O31 C32 1.437(4) . ?
O41 C13 1.367(4) . ?
O41 C42 1.426(4) . ?
N22 C23 1.291(3) . ?
N22 C21 1.470(3) . ?
N19 C18 1.292(4) . ?
N19 C20 1.502(3) . ?
C29 C24 1.411(4) . ?
C29 C28 1.421(4) . ?
C24 C23 1.434(4) . ?
C24 C25 1.418(4) . ?
C23 H23 0.9500 . ?
C12 C17 1.406(4) . ?
C12 C13 1.420(4) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C21 C20 1.524(4) . ?
C17 C18 1.439(4) . ?
C17 C16 1.422(4) . ?
C28 C27 1.380(4) . ?
C18 H18 0.9500 . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C1 C20 1.531(4) . ?
C20 C2 1.526(4) . ?
C13 C14 1.387(4) . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C27 H27 0.9500 . ?
C27 C26 1.397(5) . ?
C25 H25 0.9500 . ?
C25 C26 1.366(5) . ?
C14 H14 0.9500 . ?
C14 C15 1.400(5) . ?
C26 H26 0.9500 . ?
C16 H16 0.9500 . ?
C16 C15 1.364(5) . ?
C15 H15 0.9500 . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?
O52 H52A 0.8701 . ?
O52 H52B 0.8699 . ?
O51 H51A 0.8701 . ?
O51 H51B 0.8699 . ?

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
O30 V1 N22 86.45(8) . . ?
O30 V1 N19 151.12(9) . . ?
O11 V1 O30 88.36(8) . . ?
O11 V1 N22 138.83(9) . . ?
O11 V1 N19 87.87(9) . . ?
O1 V1 O30 104.52(10) . . ?
O1 V1 O11 111.58(10) . . ?
O1 V1 N22 109.25(10) . . ?
O1 V1 N19 103.49(10) . . ?
N22 V1 N19 77.78(9) . . ?
C29 O30 V1 124.93(16) . . ?
C12 O11 V1 129.13(17) . . ?
C28 O31 C32 116.9(2) . . ?
C13 O41 C42 117.7(2) . . ?
C23 N22 V1 125.57(19) . . ?
C23 N22 C21 118.0(2) . . ?
C21 N22 V1 116.36(17) . . ?
C18 N19 V1 125.9(2) . . ?
C18 N19 C20 120.2(2) . . ?
C20 N19 V1 113.68(16) . . ?
O30 C29 C24 123.9(2) . . ?
O30 C29 C28 118.8(2) . . ?
C24 C29 C28 117.3(2) . . ?
C29 C24 C23 121.3(2) . . ?
C29 C24 C25 120.7(3) . . ?
C25 C24 C23 118.0(3) . . ?
N22 C23 C24 124.8(3) . . ?
N22 C23 H23 117.6 . . ?
C24 C23 H23 117.6 . . ?
O11 C12 C17 124.5(2) . . ?
O11 C12 C13 117.1(3) . . ?
C17 C12 C13 118.4(2) . . ?
N22 C21 H21A 110.0 . . ?
N22 C21 H21B 110.0 . . ?
N22 C21 C20 108.7(2) . . ?
H21A C21 H21B 108.3 . . ?
C20 C21 H21A 110.0 . . ?
C20 C21 H21B 110.0 . . ?
C12 C17 C18 122.3(2) . . ?
C12 C17 C16 119.8(3) . . ?
C16 C17 C18 117.7(3) . . ?
O31 C28 C29 114.2(2) . . ?
O31 C28 C27 124.8(3) . . ?
C27 C28 C29 121.0(3) . . ?
N19 C18 C17 125.2(3) . . ?
N19 C18 H18 117.4 . . ?
C17 C18 H18 117.4 . . ?
H1A C1 H1B 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C20 C1 H1A 109.5 . . ?
C20 C1 H1B 109.5 . . ?
C20 C1 H1C 109.5 . . ?
N19 C20 C21 103.6(2) . . ?
N19 C20 C1 108.4(2) . . ?
N19 C20 C2 113.8(2) . . ?
C21 C20 C1 110.8(2) . . ?
C21 C20 C2 109.0(2) . . ?
C2 C20 C1 111.0(2) . . ?
O41 C13 C12 114.2(2) . . ?
O41 C13 C14 125.4(3) . . ?
C14 C13 C12 120.4(3) . . ?
O31 C32 H32A 109.5 . . ?
O31 C32 H32B 109.5 . . ?
O31 C32 H32C 109.5 . . ?
H32A C32 H32B 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C20 C2 H2A 109.5 . . ?
C20 C2 H2B 109.5 . . ?
C20 C2 H2C 109.5 . . ?
H2A C2 H2B 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
C28 C27 H27 119.6 . . ?
C28 C27 C26 120.8(3) . . ?
C26 C27 H27 119.6 . . ?
C24 C25 H25 119.8 . . ?
C26 C25 C24 120.3(3) . . ?
C26 C25 H25 119.8 . . ?
C13 C14 H14 119.7 . . ?
C13 C14 C15 120.6(3) . . ?
C15 C14 H14 119.7 . . ?
C27 C26 H26 120.0 . . ?
C25 C26 C27 119.9(3) . . ?
C25 C26 H26 120.0 . . ?
C17 C16 H16 119.7 . . ?
C15 C16 C17 120.7(3) . . ?
C15 C16 H16 119.7 . . ?
C14 C15 H15 120.0 . . ?
C16 C15 C14 120.1(3) . . ?
C16 C15 H15 120.0 . . ?
O41 C42 H42A 109.5 . . ?
O41 C42 H42B 109.5 . . ?
O41 C42 H42C 109.5 . . ?
H42A C42 H42B 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
H52A O52 H52B 104.5 . . ?
H51A O51 H51B 104.5 . . ?

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_1K
_database_code_depnum_ccdc_archive 'CCDC 2155583'
loop_
_audit_author_name
_audit_author_address
'Ashutosh Ghosh' 'University of Calcutta'
_audit_update_record             
;
2023-01-30 deposited with the CCDC.	2023-02-01 downloaded from the CCDC.
;
_audit_creation_date             2023-01-25
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2016/6
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C40 H44 F12 K2 N4 O10 P2 V2, [+ C2H3N]'
_chemical_formula_sum            'C40 H44 F12 K2 N4 O10 P2 V2'
_chemical_formula_weight         1210.81
_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'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 '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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'I 1 2/a 1'
_space_group_name_Hall           '-I 2ya'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y, z'
'-x+1/2, -y+1/2, -z+1/2'
'x, -y+1/2, z+1/2'

_cell_length_a                   24.8898(12)
_cell_length_b                   8.4307(4)
_cell_length_c                   25.4214(10)
_cell_angle_alpha                90
_cell_angle_beta                 100.290(4)
_cell_angle_gamma                90
_cell_volume                     5248.6(4)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    6009
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.519
_cell_measurement_theta_min      2.527
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.673
_exptl_absorpt_correction_T_max  0.920
_exptl_absorpt_correction_T_min  0.785
_exptl_absorpt_correction_type   EMPIRICAL
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            GREEN
_exptl_crystal_density_diffrn    1.532
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             2456
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.11
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0634
_diffrn_reflns_av_unetI/netI     0.0515
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            28657
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.519
_diffrn_reflns_theta_min         2.527
_diffrn_ambient_temperature      100.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5142
_reflns_number_total             6009
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _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       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         0.605
_refine_diff_density_min         -0.584
_refine_diff_density_rms         0.101
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     448
_refine_ls_number_reflns         6009
_refine_ls_number_restraints     84
_refine_ls_R_factor_all          0.0556
_refine_ls_R_factor_gt           0.0485
_refine_ls_restrained_S_all      1.059
_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)+(0.0882P)²+5.4586P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1385
_refine_ls_wR_factor_ref         0.1460
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(P1) \\sim Ueq, Uanis(P1A) \\sim Ueq: with sigma of 0.1 and sigma for
terminal atoms of 0.2
Uanis(F3) \\sim Ueq, Uanis(F3A) \\sim Ueq: with sigma of 0.1 and sigma for
terminal atoms of 0.2
Uanis(F4) \\sim Ueq, Uanis(F4A) \\sim Ueq: with sigma of 0.1 and sigma for
terminal atoms of 0.2
Uanis(F6) \\sim Ueq, Uanis(F6A) \\sim Ueq: with sigma of 0.1 and sigma for
terminal atoms of 0.2
Uanis(F5) \\sim Ueq, Uanis(F5A) \\sim Ueq: with sigma of 0.1 and sigma for
terminal atoms of 0.2
Uanis(F1) \\sim Ueq, Uanis(F1A) \\sim Ueq: with sigma of 0.1 and sigma for
terminal atoms of 0.2
Uanis(F2) \\sim Ueq, Uanis(F2A) \\sim Ueq: with sigma of 0.1 and sigma for
terminal atoms of 0.2
Uanis(F3A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.1
Uanis(P1A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.1
Uanis(F1A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.2
Uanis(C2) = Uanis(C2A)
Uanis(C23) = Uanis(C23A)
Uanis(C18) = Uanis(N19A)
3. Others
 Fixed Sof: P1(0.824) F1(0.824) F2(0.824) F3(0.824) F4(0.824) F5(0.824)
 F6(0.824) N19(0.55) N22(0.55) C1(0.55) H1A(0.55) H1B(0.55) H1C(0.55)
 C21A(0.55) C22A(0.55) H22A(0.55) H22B(0.55) C22B(0.45) C21B(0.45) H21A(0.45)
 H21B(0.45) C1A(0.45) H1AA(0.45) H1AB(0.45) H1AC(0.45) C18A(0.5) H18A(0.5)
 N22A(0.45) P1A(0.176) F3A(0.176) F4A(0.176) F6A(0.176) F5A(0.176) F1A(0.176)
 F2A(0.176) C2(0.5) H2A(0.5) H2B(0.5) H2C(0.5) C23(0.55) H23(0.55) C18(0.5)
 H18(0.5) C2A(0.5) H2AA(0.5) H2AB(0.5) H2AC(0.5) C23A(0.45) H23A(0.45)
 N19A(0.45)
4.a Secondary CH2 refined with riding coordinates:
 C22A(H22A,H22B), C21B(H21A,H21B)
4.b Aromatic/amide H refined with riding coordinates:
 C14(H14), C15(H15), C16(H16), C25(H25), C26(H26), C27(H27), C18A(H18A),
 C23(H23), C18(H18), C23A(H23A)
4.c Idealised Me refined as rotating group:
 C42(H42A,H42B,H42C), C32(H32A,H32B,H32C), C1(H1A,H1B,H1C), C1A(H1AA,H1AB,
 H1AC), C2(H2A,H2B,H2C), C2A(H2AA,H2AB,H2AC)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
V1 V 0.65176(2) 0.46529(4) 0.72171(2) 0.01656(13) Uani 1 1 d . . . . .
K1 K 0.56225(2) 0.49009(6) 0.58809(2) 0.02180(15) Uani 1 1 d . . . . .
P1 P 0.42456(9) 0.36314(19) 0.54950(7) 0.0193(6) Uani 0.824 1 d . U P A 1
F1 F 0.46418(16) 0.2979(3) 0.60102(13) 0.0340(7) Uani 0.824 1 d . U P A 1
F2 F 0.44576(9) 0.5408(2) 0.56547(10) 0.0322(5) Uani 0.824 1 d . U P A 1
F3 F 0.47387(9) 0.3474(3) 0.51618(8) 0.0364(5) Uani 0.824 1 d . U P A 1
F4 F 0.38618(13) 0.4331(3) 0.49657(11) 0.0357(6) Uani 0.824 1 d . U P A 1
F5 F 0.37604(18) 0.3873(4) 0.58211(16) 0.0341(8) Uani 0.824 1 d . U P A 1
F6 F 0.40499(11) 0.1905(3) 0.53294(12) 0.0500(6) Uani 0.824 1 d . U P A 1
O1 O 0.70900(7) 0.53369(19) 0.71181(6) 0.0221(4) Uani 1 1 d . . . . .
O11 O 0.62526(7) 0.31763(19) 0.66513(6) 0.0237(4) Uani 1 1 d . . . . .
O30 O 0.59233(7) 0.60187(19) 0.68859(6) 0.0202(3) Uani 1 1 d . . . . .
O41 O 0.61870(8) 0.2149(2) 0.56697(6) 0.0278(4) Uani 1 1 d . . . . .
O31 O 0.53833(7) 0.79735(19) 0.61680(6) 0.0233(4) Uani 1 1 d . . . . .
N19 N 0.66407(19) 0.2810(7) 0.7750(2) 0.0135(10) Uani 0.55 1 d . . P B 1
N22 N 0.6440(4) 0.5766(8) 0.7937(4) 0.0171(14) Uani 0.55 1 d . . P B 1
C12 C 0.64475(9) 0.1735(3) 0.65931(9) 0.0210(5) Uani 1 1 d . . . . .
C13 C 0.64083(10) 0.1117(3) 0.60683(9) 0.0232(5) Uani 1 1 d . . . . .
C14 C 0.65784(11) -0.0406(3) 0.59851(11) 0.0270(5) Uani 1 1 d . . . . .
H14 H 0.654852 -0.080154 0.563108 0.032 Uiso 1 1 calc R . . . .
C15 C 0.67953(10) -0.1373(3) 0.64205(11) 0.0282(5) Uani 1 1 d . . . . .
H15 H 0.690624 -0.242645 0.636089 0.034 Uiso 1 1 calc R . . . .
C16 C 0.68470(10) -0.0803(3) 0.69300(10) 0.0268(5) Uani 1 1 d . . . . .
H16 H 0.699504 -0.146323 0.722310 0.032 Uiso 1 1 calc R . . . .
C17 C 0.66825(10) 0.0759(3) 0.70250(10) 0.0240(5) Uani 1 1 d . . . . .
C24 C 0.58377(10) 0.7787(3) 0.76115(9) 0.0254(5) Uani 1 1 d . . . . .
C25 C 0.56215(11) 0.9213(4) 0.77735(10) 0.0326(6) Uani 1 1 d . . . . .
H25 H 0.566520 0.946040 0.814331 0.039 Uiso 1 1 calc R . . . .
C26 C 0.53489(12) 1.0248(3) 0.74040(11) 0.0328(6) Uani 1 1 d . . . . .
H26 H 0.521506 1.122225 0.751685 0.039 Uiso 1 1 calc R . . . .
C27 C 0.52680(10) 0.9866(3) 0.68606(10) 0.0257(5) Uani 1 1 d . . . . .
H27 H 0.508162 1.058927 0.660469 0.031 Uiso 1 1 calc R . . . .
C28 C 0.54560(9) 0.8450(3) 0.66925(9) 0.0207(5) Uani 1 1 d . . . . .
C29 C 0.57518(9) 0.7369(3) 0.70629(9) 0.0199(4) Uani 1 1 d . . . . .
C42 C 0.62312(16) 0.1690(4) 0.51384(10) 0.0462(9) Uani 1 1 d . . . . .
H42A H 0.600743 0.074526 0.503669 0.069 Uiso 1 1 calc GR . . . .
H42B H 0.661341 0.145316 0.512257 0.069 Uiso 1 1 calc GR . . . .
H42C H 0.610298 0.255827 0.489119 0.069 Uiso 1 1 calc GR . . . .
C32 C 0.51221(12) 0.9088(3) 0.57804(10) 0.0298(6) Uani 1 1 d . . . . .
H32A H 0.510948 0.865557 0.542055 0.045 Uiso 1 1 calc GR . . . .
H32B H 0.532847 1.008408 0.581572 0.045 Uiso 1 1 calc GR . . . .
H32C H 0.474957 0.928802 0.583936 0.045 Uiso 1 1 calc GR . . . .
C1 C 0.71410(19) 0.2263(5) 0.86941(16) 0.0241(9) Uani 0.55 1 d . . P B 1
H1A H 0.719469 0.268253 0.905922 0.036 Uiso 0.55 1 calc GR . P B 1
H1B H 0.747845 0.238868 0.855021 0.036 Uiso 0.55 1 calc GR . P B 1
H1C H 0.704600 0.113505 0.869795 0.036 Uiso 0.55 1 calc GR . P B 1
C21A C 0.66744(19) 0.3179(5) 0.83396(15) 0.0140(7) Uani 0.55 1 d . . P B 1
C22A C 0.6796(2) 0.4974(6) 0.83875(15) 0.0182(8) Uani 0.55 1 d . . P B 1
H22A H 0.671967 0.538326 0.873180 0.022 Uiso 0.55 1 calc R . P B 1
H22B H 0.718449 0.517760 0.837219 0.022 Uiso 0.55 1 calc R . P B 1
C22B C 0.6576(3) 0.4198(9) 0.8409(2) 0.0244(12) Uani 0.45 1 d . . P B 2
C21B C 0.6981(3) 0.3100(6) 0.8231(2) 0.0249(11) Uani 0.45 1 d . . P B 2
H21A H 0.734194 0.362630 0.827537 0.030 Uiso 0.45 1 calc R . P B 2
H21B H 0.701980 0.213447 0.845673 0.030 Uiso 0.45 1 calc R . P B 2
C1A C 0.6832(3) 0.5089(7) 0.8906(2) 0.0309(13) Uani 0.45 1 d . . P B 2
H1AA H 0.711482 0.580427 0.882065 0.046 Uiso 0.45 1 calc GR . P B 2
H1AB H 0.699667 0.433233 0.918084 0.046 Uiso 0.45 1 calc GR . P B 2
H1AC H 0.655137 0.570831 0.903938 0.046 Uiso 0.45 1 calc GR . P B 2
C18A C 0.6711(3) 0.1390(11) 0.7612(3) 0.0126(14) Uani 0.5 1 d . . P B 2
H18A H 0.664928 0.071593 0.789437 0.015 Uiso 0.5 1 calc R . P B 2
N22A N 0.6371(5) 0.5269(10) 0.7943(5) 0.0198(18) Uani 0.45 1 d . . P B 2
P1A P 0.4232(5) 0.3601(17) 0.5485(5) 0.048(5) Uani 0.176 1 d . U P A 2
F3A F 0.4724(6) 0.2635(15) 0.5280(5) 0.054(3) Uani 0.176 1 d . U P A 2
F4A F 0.3891(7) 0.3528(19) 0.4922(6) 0.054(4) Uani 0.176 1 d . U P A 2
F6A F 0.3974(6) 0.1867(14) 0.5624(5) 0.053(3) Uani 0.176 1 d . U P A 2
F5A F 0.3786(9) 0.444(2) 0.5734(9) 0.043(4) Uani 0.176 1 d . U P A 2
F1A F 0.4609(8) 0.355(2) 0.6089(7) 0.045(4) Uani 0.176 1 d . U P A 2
F2A F 0.4513(5) 0.5160(13) 0.5360(5) 0.041(3) Uani 0.176 1 d . U P A 2
C2 C 0.6137(7) 0.2763(16) 0.8471(7) 0.0229(17) Uani 0.5 1 d . . P B 1
H2A H 0.584688 0.323592 0.820571 0.034 Uiso 0.5 1 calc GR . P B 1
H2B H 0.611250 0.316933 0.882691 0.034 Uiso 0.5 1 calc GR . P B 1
H2C H 0.609460 0.160671 0.846679 0.034 Uiso 0.5 1 calc GR . P B 1
C23 C 0.6171(5) 0.6988(10) 0.8021(5) 0.0195(14) Uani 0.55 1 d . . P B 1
H23 H 0.619823 0.736666 0.837696 0.023 Uiso 0.55 1 calc R . P B 1
C18 C 0.6825(4) 0.1214(13) 0.7522(4) 0.0186(13) Uani 0.5 1 d . . P B 1
H18 H 0.705529 0.053169 0.776099 0.022 Uiso 0.5 1 calc R . P B 1
C2A C 0.6075(7) 0.3146(16) 0.8524(7) 0.0229(17) Uani 0.5 1 d . . P B 2
H2AA H 0.591943 0.255343 0.820117 0.034 Uiso 0.5 1 calc GR . P B 2
H2AB H 0.579467 0.383893 0.862667 0.034 Uiso 0.5 1 calc GR . P B 2
H2AC H 0.620382 0.240165 0.881545 0.034 Uiso 0.5 1 calc GR . P B 2
C23A C 0.6096(7) 0.6532(13) 0.8020(6) 0.0195(14) Uani 0.45 1 d . . P B 2
H23A H 0.604742 0.670576 0.837743 0.023 Uiso 0.45 1 calc R . P B 2
N19A N 0.6805(3) 0.2659(10) 0.7676(3) 0.0186(13) Uani 0.45 1 d . . P B 2


_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 K1 3.7206(6) . ?
V1 O1 1.5980(18) . ?
V1 O11 1.9273(16) . ?
V1 O30 1.9437(16) . ?
V1 N19 2.048(6) . ?
V1 N22 2.096(10) . ?
V1 N22A 2.011(13) . ?
V1 N19A 2.097(8) . ?
K1 F1 2.996(4) . ?
K1 F2 2.885(2) . ?
K1 F3 2.977(2) 5_666 ?
K1 F3 2.862(2) . ?
K1 F4 2.772(3) 5_666 ?
K1 O11 2.7042(16) . ?
K1 O30 2.7004(16) . ?
K1 O41 2.8137(18) . ?
K1 O31 2.7844(17) . ?
K1 F4A 2.875(17) 5_666 ?
K1 F1A 2.90(2) . ?
K1 F2A 2.850(11) . ?
P1 F1 1.590(4) . ?
P1 F2 1.615(3) . ?
P1 F3 1.617(3) . ?
P1 F4 1.616(3) . ?
P1 F5 1.595(5) . ?
P1 F6 1.568(3) . ?
O11 C12 1.327(3) . ?
O30 C29 1.323(3) . ?
O41 C13 1.374(3) . ?
O41 C42 1.428(3) . ?
O31 C28 1.373(3) . ?
O31 C32 1.431(3) . ?
N19 C21A 1.519(7) . ?
N19 C18 1.565(13) . ?
N22 C22A 1.476(11) . ?
N22 C23 1.268(18) . ?
C12 C13 1.419(3) . ?
C12 C17 1.412(3) . ?
C13 C14 1.380(3) . ?
C14 H14 0.9500 . ?
C14 C15 1.403(3) . ?
C15 H15 0.9500 . ?
C15 C16 1.366(4) . ?
C16 H16 0.9500 . ?
C16 C17 1.413(4) . ?
C17 C18A 1.573(7) . ?
C17 C18 1.308(10) . ?
C24 C25 1.408(4) . ?
C24 C29 1.417(3) . ?
C24 C23 1.385(13) . ?
C24 C23A 1.539(16) . ?
C25 H25 0.9500 . ?
C25 C26 1.369(4) . ?
C26 H26 0.9500 . ?
C26 C27 1.398(4) . ?
C27 H27 0.9500 . ?
C27 C28 1.378(3) . ?
C28 C29 1.418(3) . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C1 C21A 1.544(6) . ?
C21A C22A 1.544(6) . ?
C21A C2 1.478(18) . ?
C22A H22A 0.9900 . ?
C22A H22B 0.9900 . ?
C22B C21B 1.498(8) . ?
C22B C1A 1.510(8) . ?
C22B N22A 1.505(13) . ?
C22B C2A 1.60(2) . ?
C21B H21A 0.9900 . ?
C21B H21B 0.9900 . ?
C21B N19A 1.450(10) . ?
C1A H1AA 0.9800 . ?
C1A H1AB 0.9800 . ?
C1A H1AC 0.9800 . ?
C18A H18A 0.9500 . ?
C18A N19A 1.101(15) . ?
N22A C23A 1.30(2) . ?
P1A F3A 1.631(17) . ?
P1A F4A 1.53(2) . ?
P1A F6A 1.660(18) . ?
P1A F5A 1.54(2) . ?
P1A F1A 1.65(2) . ?
P1A F2A 1.547(18) . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C23 H23 0.9500 . ?
C18 H18 0.9500 . ?
C2A H2AA 0.9800 . ?
C2A H2AB 0.9800 . ?
C2A H2AC 0.9800 . ?
C23A H23A 0.9500 . ?

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 V1 K1 103.96(6) . . ?
O1 V1 O11 108.15(8) . . ?
O1 V1 O30 110.42(8) . . ?
O1 V1 N19 110.22(15) . . ?
O1 V1 N22 101.5(2) . . ?
O1 V1 N22A 111.4(3) . . ?
O1 V1 N19A 98.7(2) . . ?
O11 V1 K1 44.41(5) . . ?
O11 V1 O30 85.80(7) . . ?
O11 V1 N19 89.67(17) . . ?
O11 V1 N22 150.3(2) . . ?
O11 V1 N22A 139.2(3) . . ?
O11 V1 N19A 86.2(2) . . ?
O30 V1 K1 44.43(5) . . ?
O30 V1 N19 138.44(14) . . ?
O30 V1 N22 86.1(3) . . ?
O30 V1 N22A 89.7(4) . . ?
O30 V1 N19A 150.9(2) . . ?
N19 V1 K1 129.85(17) . . ?
N19 V1 N22 77.8(3) . . ?
N22 V1 K1 129.7(3) . . ?
N22A V1 K1 130.2(4) . . ?
N22A V1 N19A 78.3(4) . . ?
N19A V1 K1 129.9(2) . . ?
F2 K1 F1 44.98(7) . . ?
F2 K1 F3 67.75(7) . 5_666 ?
F3 K1 F1 45.14(8) . . ?
F3 K1 F1 102.96(8) 5_666 . ?
F3 K1 F2 45.94(6) . . ?
F3 K1 F3 63.21(9) . 5_666 ?
F3 K1 F4A 96.5(3) . 5_666 ?
F4 K1 F1 135.29(9) 5_666 . ?
F4 K1 F2 113.51(8) 5_666 . ?
F4 K1 F3 90.69(8) 5_666 . ?
F4 K1 F3 46.31(7) 5_666 5_666 ?
F4 K1 O41 74.23(7) 5_666 . ?
F4 K1 O31 97.85(7) 5_666 . ?
F4 K1 F4A 13.9(3) 5_666 5_666 ?
O11 K1 F1 90.47(7) . . ?
O11 K1 F2 131.01(6) . . ?
O11 K1 F3 121.12(7) . . ?
O11 K1 F3 159.44(6) . 5_666 ?
O11 K1 F4 113.50(7) . 5_666 ?
O11 K1 O41 56.63(5) . . ?
O11 K1 O31 115.71(5) . . ?
O11 K1 F4A 119.9(4) . 5_666 ?
O11 K1 F1A 93.9(4) . . ?
O11 K1 F2A 140.0(2) . . ?
O30 K1 F1 100.29(7) . . ?
O30 K1 F2 103.64(6) . . ?
O30 K1 F3 143.38(6) . . ?
O30 K1 F3 132.11(6) . 5_666 ?
O30 K1 F4 124.35(8) . 5_666 ?
O30 K1 O11 58.36(5) . . ?
O30 K1 O41 113.88(5) . . ?
O30 K1 O31 57.55(5) . . ?
O30 K1 F4A 115.5(3) . 5_666 ?
O30 K1 F1A 93.9(3) . . ?
O30 K1 F2A 119.6(3) . . ?
O41 K1 F1 91.11(7) . . ?
O41 K1 F2 127.05(6) . . ?
O41 K1 F3 83.37(6) . . ?
O41 K1 F3 106.94(5) . 5_666 ?
O41 K1 F4A 87.5(4) . 5_666 ?
O41 K1 F1A 101.0(3) . . ?
O41 K1 F2A 116.8(3) . . ?
O31 K1 F1 104.94(7) . . ?
O31 K1 F2 70.13(6) . . ?
O31 K1 F3 76.15(5) . 5_666 ?
O31 K1 F3 112.49(6) . . ?
O31 K1 O41 162.69(6) . . ?
O31 K1 F4A 83.9(3) . 5_666 ?
O31 K1 F1A 94.8(3) . . ?
O31 K1 F2A 79.4(2) . . ?
F4A K1 F1A 143.2(5) 5_666 . ?
F2A K1 F1A 46.6(5) . . ?
K1 P1 K1 85.29(5) . 5_666 ?
F1 P1 K1 56.76(16) . . ?
F1 P1 K1 137.04(18) . 5_666 ?
F1 P1 F2 89.26(17) . . ?
F1 P1 F3 89.20(19) . . ?
F1 P1 F4 177.9(2) . . ?
F1 P1 F5 91.8(2) . . ?
F2 P1 K1 81.40(11) . 5_666 ?
F2 P1 K1 52.86(10) . . ?
F2 P1 F3 87.88(16) . . ?
F2 P1 F4 89.36(15) . . ?
F3 P1 K1 52.03(9) . . ?
F3 P1 K1 48.87(9) . 5_666 ?
F4 P1 K1 41.07(12) . 5_666 ?
F4 P1 K1 121.12(14) . . ?
F4 P1 F3 89.13(16) . . ?
F5 P1 K1 126.86(17) . . ?
F5 P1 K1 129.66(15) . 5_666 ?
F5 P1 F2 89.71(19) . . ?
F5 P1 F3 177.38(19) . . ?
F5 P1 F4 89.8(2) . . ?
F6 P1 K1 126.23(14) . . ?
F6 P1 K1 97.44(13) . 5_666 ?
F6 P1 F1 90.99(17) . . ?
F6 P1 F2 178.5(2) . . ?
F6 P1 F3 90.67(17) . . ?
F6 P1 F4 90.35(17) . . ?
F6 P1 F5 91.7(2) . . ?
P1 F1 K1 96.90(17) . . ?
P1 F2 K1 100.62(12) . . ?
K1 F3 K1 116.80(9) . 5_666 ?
P1 F3 K1 101.52(11) . . ?
P1 F3 K1 106.98(12) . 5_666 ?
P1 F4 K1 116.41(17) . 5_666 ?
V1 O11 K1 105.67(7) . . ?
C12 O11 V1 126.28(14) . . ?
C12 O11 K1 126.02(13) . . ?
V1 O30 K1 105.31(7) . . ?
C29 O30 V1 129.00(13) . . ?
C29 O30 K1 124.79(13) . . ?
C13 O41 K1 121.97(14) . . ?
C13 O41 C42 115.98(19) . . ?
C42 O41 K1 121.94(15) . . ?
C28 O31 K1 121.95(13) . . ?
C28 O31 C32 116.21(18) . . ?
C32 O31 K1 121.50(13) . . ?
C21A N19 V1 118.2(4) . . ?
C21A N19 C18 124.9(7) . . ?
C18 N19 V1 115.3(6) . . ?
C22A N22 V1 109.8(6) . . ?
C23 N22 V1 130.2(9) . . ?
C23 N22 C22A 119.9(9) . . ?
O11 C12 C13 118.42(19) . . ?
O11 C12 C17 123.8(2) . . ?
C17 C12 C13 117.8(2) . . ?
O41 C13 C12 114.3(2) . . ?
O41 C13 C14 124.7(2) . . ?
C14 C13 C12 120.9(2) . . ?
C13 C14 H14 119.8 . . ?
C13 C14 C15 120.3(2) . . ?
C15 C14 H14 119.8 . . ?
C14 C15 H15 119.9 . . ?
C16 C15 C14 120.1(2) . . ?
C16 C15 H15 119.9 . . ?
C15 C16 H16 119.7 . . ?
C15 C16 C17 120.6(2) . . ?
C17 C16 H16 119.7 . . ?
C12 C17 C16 120.2(2) . . ?
C12 C17 C18A 118.8(4) . . ?
C16 C17 C18A 120.8(4) . . ?
C18 C17 C12 125.7(5) . . ?
C18 C17 C16 113.7(5) . . ?
C25 C24 C29 120.1(2) . . ?
C25 C24 C23A 121.7(6) . . ?
C29 C24 C23A 117.6(6) . . ?
C23 C24 C25 113.9(5) . . ?
C23 C24 C29 125.7(5) . . ?
C24 C25 H25 119.6 . . ?
C26 C25 C24 120.8(2) . . ?
C26 C25 H25 119.6 . . ?
C25 C26 H26 120.1 . . ?
C25 C26 C27 119.8(2) . . ?
C27 C26 H26 120.1 . . ?
C26 C27 H27 119.7 . . ?
C28 C27 C26 120.6(2) . . ?
C28 C27 H27 119.7 . . ?
O31 C28 C27 124.1(2) . . ?
O31 C28 C29 114.8(2) . . ?
C27 C28 C29 121.0(2) . . ?
O30 C29 C24 123.2(2) . . ?
O30 C29 C28 119.19(19) . . ?
C24 C29 C28 117.6(2) . . ?
O41 C42 H42A 109.5 . . ?
O41 C42 H42B 109.5 . . ?
O41 C42 H42C 109.5 . . ?
H42A C42 H42B 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
O31 C32 H32A 109.5 . . ?
O31 C32 H32B 109.5 . . ?
O31 C32 H32C 109.5 . . ?
H32A C32 H32B 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
H1A C1 H1B 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C21A C1 H1A 109.5 . . ?
C21A C1 H1B 109.5 . . ?
C21A C1 H1C 109.5 . . ?
N19 C21A C1 112.2(4) . . ?
N19 C21A C22A 104.7(4) . . ?
C1 C21A C22A 109.1(3) . . ?
C2 C21A N19 106.4(8) . . ?
C2 C21A C1 111.5(8) . . ?
C2 C21A C22A 112.8(6) . . ?
N22 C22A C21A 107.5(4) . . ?
N22 C22A H22A 110.2 . . ?
N22 C22A H22B 110.2 . . ?
C21A C22A H22A 110.2 . . ?
C21A C22A H22B 110.2 . . ?
H22A C22A H22B 108.5 . . ?
C21B C22B C1A 110.7(5) . . ?
C21B C22B N22A 106.6(6) . . ?
C21B C22B C2A 107.5(6) . . ?
C1A C22B C2A 110.4(7) . . ?
N22A C22B C1A 113.2(7) . . ?
N22A C22B C2A 108.2(9) . . ?
C22B C21B H21A 109.6 . . ?
C22B C21B H21B 109.6 . . ?
H21A C21B H21B 108.1 . . ?
N19A C21B C22B 110.5(5) . . ?
N19A C21B H21A 109.6 . . ?
N19A C21B H21B 109.6 . . ?
C22B C1A H1AA 109.5 . . ?
C22B C1A H1AB 109.5 . . ?
C22B C1A H1AC 109.5 . . ?
H1AA C1A H1AB 109.5 . . ?
H1AA C1A H1AC 109.5 . . ?
H1AB C1A H1AC 109.5 . . ?
C17 C18A H18A 121.9 . . ?
N19A C18A C17 116.2(9) . . ?
N19A C18A H18A 121.9 . . ?
C22B N22A V1 118.4(7) . . ?
C23A N22A V1 122.5(10) . . ?
C23A N22A C22B 119.1(12) . . ?
K1 P1A K1 84.8(3) . 5_666 ?
F3A P1A K1 60.2(7) . . ?
F3A P1A F6A 88.2(9) . . ?
F3A P1A F1A 87.1(10) . . ?
F4A P1A K1 128.2(9) . . ?
F4A P1A F3A 90.1(11) . . ?
F4A P1A F6A 89.5(11) . . ?
F4A P1A F5A 94.8(13) . . ?
F4A P1A F1A 176.1(13) . . ?
F4A P1A F2A 92.1(10) . . ?
F6A P1A K1 126.8(8) . . ?
F5A P1A K1 118.1(11) . . ?
F5A P1A F3A 174.4(13) . . ?
F5A P1A F6A 89.1(10) . . ?
F5A P1A F1A 87.8(12) . . ?
F5A P1A F2A 94.5(11) . . ?
F1A P1A K1 52.3(8) . . ?
F1A P1A F6A 87.6(11) . . ?
F2A P1A K1 49.6(6) . . ?
F2A P1A F3A 88.1(9) . . ?
F2A P1A F6A 176.0(11) . . ?
F2A P1A F1A 90.6(11) . . ?
P1A F3A K1 92.9(8) . . ?
P1A F1A K1 100.9(10) . . ?
K1 F2A K1 112.9(5) . 5_666 ?
P1A F2A K1 106.0(7) . . ?
C21A C2 H2A 109.5 . . ?
C21A C2 H2B 109.5 . . ?
C21A C2 H2C 109.5 . . ?
H2A C2 H2B 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
N22 C23 C24 122.2(10) . . ?
N22 C23 H23 118.9 . . ?
C24 C23 H23 118.9 . . ?
N19 C18 H18 117.9 . . ?
C17 C18 N19 124.2(9) . . ?
C17 C18 H18 117.9 . . ?
C22B C2A H2AA 109.5 . . ?
C22B C2A H2AB 109.5 . . ?
C22B C2A H2AC 109.5 . . ?
H2AA C2A H2AB 109.5 . . ?
H2AA C2A H2AC 109.5 . . ?
H2AB C2A H2AC 109.5 . . ?
C24 C23A H23A 115.5 . . ?
N22A C23A C24 129.0(13) . . ?
N22A C23A H23A 115.5 . . ?
C21B N19A V1 110.5(5) . . ?
C18A N19A V1 130.8(9) . . ?
C18A N19A C21B 114.3(9) . . ?

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
V1 O11 C12 C13 -149.97(18) . . . . ?
V1 O11 C12 C17 31.4(3) . . . . ?
V1 O30 C29 C24 -24.2(3) . . . . ?
V1 O30 C29 C28 157.31(16) . . . . ?
V1 N19 C21A C1 -136.8(3) . . . . ?
V1 N19 C21A C22A -18.6(5) . . . . ?
V1 N19 C21A C2 101.0(7) . . . . ?
V1 N19 C18 C17 -31.2(11) . . . . ?
V1 N22 C22A C21A -51.2(6) . . . . ?
V1 N22 C23 C24 3.5(12) . . . . ?
V1 N22A C23A C24 -0.6(16) . . . . ?
K1 P1 F1 K1 32.0(2) 5_666 . . . ?
K1 P1 F2 K1 -90.60(8) 5_666 . . . ?
K1 P1 F3 K1 122.91(13) 5_666 . . . ?
K1 P1 F3 K1 -122.91(13) . . . 5_666 ?
K1 P1 F4 K1 33.0(2) . . . 5_666 ?
K1 O11 C12 C13 11.5(3) . . . . ?
K1 O11 C12 C17 -167.11(17) . . . . ?
K1 O30 C29 C24 168.33(17) . . . . ?
K1 O30 C29 C28 -10.2(3) . . . . ?
K1 O41 C13 C12 -14.7(3) . . . . ?
K1 O41 C13 C14 164.6(2) . . . . ?
K1 O31 C28 C27 -169.63(18) . . . . ?
K1 O31 C28 C29 11.1(3) . . . . ?
K1 P1A F3A K1 95.1(3) 5_666 . . . ?
K1 P1A F4A K1 -10.8(15) . . . 5_666 ?
K1 P1A F1A K1 -3.7(13) 5_666 . . . ?
K1 P1A F2A K1 -118.8(7) 5_666 . . . ?
K1 P1A F2A K1 118.8(7) . . . 5_666 ?
F1 P1 F2 K1 47.32(18) . . . . ?
F1 P1 F3 K1 -169.71(14) . . . 5_666 ?
F1 P1 F3 K1 -46.80(15) . . . . ?
F2 P1 F1 K1 -44.49(14) . . . . ?
F2 P1 F3 K1 42.49(13) . . . . ?
F2 P1 F3 K1 -80.42(13) . . . 5_666 ?
F2 P1 F4 K1 77.60(17) . . . 5_666 ?
F3 P1 F1 K1 43.41(13) . . . . ?
F3 P1 F2 K1 -41.91(13) . . . . ?
F3 P1 F4 K1 -10.29(17) . . . 5_666 ?
F4 P1 F2 K1 -131.06(15) . . . . ?
F4 P1 F3 K1 131.88(14) . . . . ?
F4 P1 F3 K1 8.97(15) . . . 5_666 ?
F5 P1 F1 K1 -134.17(16) . . . . ?
F5 P1 F2 K1 139.14(16) . . . . ?
F5 P1 F4 K1 167.31(18) . . . 5_666 ?
F6 P1 F1 K1 134.06(15) . . . . ?
F6 P1 F3 K1 -137.78(14) . . . . ?
F6 P1 F3 K1 99.31(14) . . . 5_666 ?
F6 P1 F4 K1 -100.96(18) . . . 5_666 ?
O11 C12 C13 O41 2.7(3) . . . . ?
O11 C12 C13 C14 -176.6(2) . . . . ?
O11 C12 C17 C16 175.7(2) . . . . ?
O11 C12 C17 C18A 0.9(5) . . . . ?
O11 C12 C17 C18 -12.3(6) . . . . ?
O41 C13 C14 C15 -179.4(2) . . . . ?
O31 C28 C29 O30 -1.0(3) . . . . ?
O31 C28 C29 C24 -179.6(2) . . . . ?
N19 C21A C22A N22 43.5(6) . . . . ?
C12 C13 C14 C15 -0.1(4) . . . . ?
C12 C17 C18A N19A -38.5(9) . . . . ?
C12 C17 C18 N19 14.6(11) . . . . ?
C13 C12 C17 C16 -2.9(3) . . . . ?
C13 C12 C17 C18A -177.7(4) . . . . ?
C13 C12 C17 C18 169.0(5) . . . . ?
C13 C14 C15 C16 -1.0(4) . . . . ?
C14 C15 C16 C17 0.2(4) . . . . ?
C15 C16 C17 C12 1.8(4) . . . . ?
C15 C16 C17 C18A 176.6(4) . . . . ?
C15 C16 C17 C18 -171.0(5) . . . . ?
C16 C17 C18A N19A 146.6(7) . . . . ?
C16 C17 C18 N19 -173.0(7) . . . . ?
C17 C12 C13 O41 -178.6(2) . . . . ?
C17 C12 C13 C14 2.1(4) . . . . ?
C17 C18A N19A V1 43.0(10) . . . . ?
C17 C18A N19A C21B -163.2(5) . . . . ?
C24 C25 C26 C27 2.1(4) . . . . ?
C25 C24 C29 O30 -177.1(2) . . . . ?
C25 C24 C29 C28 1.5(4) . . . . ?
C25 C24 C23 N22 -173.1(7) . . . . ?
C25 C24 C23A N22A -170.5(9) . . . . ?
C25 C26 C27 C28 0.6(4) . . . . ?
C26 C27 C28 O31 178.6(2) . . . . ?
C26 C27 C28 C29 -2.2(4) . . . . ?
C27 C28 C29 O30 179.7(2) . . . . ?
C27 C28 C29 C24 1.1(3) . . . . ?
C29 C24 C25 C26 -3.1(4) . . . . ?
C29 C24 C23 N22 0.3(10) . . . . ?
C29 C24 C23A N22A 18.5(14) . . . . ?
C42 O41 C13 C12 169.0(3) . . . . ?
C42 O41 C13 C14 -11.6(4) . . . . ?
C32 O31 C28 C27 3.8(3) . . . . ?
C32 O31 C28 C29 -175.5(2) . . . . ?
C1 C21A C22A N22 163.7(6) . . . . ?
C21A N19 C18 C17 163.4(6) . . . . ?
C22A N22 C23 C24 179.1(6) . . . . ?
C22B C21B N19A V1 43.9(7) . . . . ?
C22B C21B N19A C18A -115.2(8) . . . . ?
C22B N22A C23A C24 -179.0(9) . . . . ?
C21B C22B N22A V1 14.9(9) . . . . ?
C21B C22B N22A C23A -166.6(9) . . . . ?
C1A C22B C21B N19A -160.8(6) . . . . ?
C1A C22B N22A V1 136.8(6) . . . . ?
C1A C22B N22A C23A -44.7(12) . . . . ?
N22A C22B C21B N19A -37.3(9) . . . . ?
F3A P1A F4A K1 -61.6(11) . . . 5_666 ?
F3A P1A F1A K1 53.8(8) . . . . ?
F3A P1A F2A K1 67.5(8) . . . 5_666 ?
F3A P1A F2A K1 -51.3(9) . . . . ?
F4A P1A F3A K1 135.4(8) . . . . ?
F4A P1A F2A K1 -141.4(9) . . . . ?
F4A P1A F2A K1 -22.6(10) . . . 5_666 ?
F6A P1A F3A K1 -135.1(7) . . . . ?
F6A P1A F4A K1 -149.8(9) . . . 5_666 ?
F6A P1A F1A K1 142.2(7) . . . . ?
F5A P1A F4A K1 121.1(10) . . . 5_666 ?
F5A P1A F1A K1 -128.7(9) . . . . ?
F5A P1A F2A K1 -117.6(10) . . . 5_666 ?
F5A P1A F2A K1 123.6(11) . . . . ?
F1A P1A F3A K1 -47.5(9) . . . . ?
F1A P1A F2A K1 35.8(9) . . . . ?
F1A P1A F2A K1 154.5(7) . . . 5_666 ?
F2A P1A F3A K1 43.3(7) . . . . ?
F2A P1A F4A K1 26.5(11) . . . 5_666 ?
F2A P1A F1A K1 -34.2(8) . . . . ?
C2 C21A C22A N22 -71.8(10) . . . . ?
C23 N22 C22A C21A 132.4(7) . . . . ?
C23 C24 C25 C26 170.7(5) . . . . ?
C23 C24 C29 O30 9.9(6) . . . . ?
C23 C24 C29 C28 -171.6(5) . . . . ?
C18 N19 C21A C1 28.1(8) . . . . ?
C18 N19 C21A C22A 146.4(7) . . . . ?
C18 N19 C21A C2 -94.0(9) . . . . ?
C2A C22B C21B N19A 78.5(9) . . . . ?
C2A C22B N22A V1 -100.5(8) . . . . ?
C2A C22B N22A C23A 78.0(11) . . . . ?
C23A C24 C25 C26 -173.9(6) . . . . ?
C23A C24 C29 O30 -5.9(7) . . . . ?
C23A C24 C29 C28 172.7(6) . . . . ?

_smtbx_masks_special_details     
;
A solvent mask was calculated and 76 electrons were 
found in a volume of 492Å³ in 1 void per unit cell. 
This is consistent with the presence of 1[C2H3N] per Formula Unit 
which account for 88 electrons per unit cell.
;
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.250 0.216 0.500 123.0 19.1 '1 MeCN'
2 0.250 0.016 1.000 123.0 19.1 '1 MeCN'
3 0.750 -0.366 0.000 123.0 19.1 '1 MeCN'
4 0.750 0.403 0.500 123.0 19.1 '1 MeCN'

_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_1Ba
_database_code_depnum_ccdc_archive 'CCDC 2155584'
loop_
_audit_author_name
_audit_author_address
'Ashutosh Ghosh' 'University of Calcutta'
_audit_update_record             
;
2023-01-30 deposited with the CCDC.	2023-02-01 downloaded from the CCDC.
;
_audit_creation_date             2023-01-23
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2016/6
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C20 H22 Ba Cl2 N2 O14 V'
_chemical_formula_sum            'C20 H22 Ba Cl2 N2 O14 V'
_chemical_formula_weight         773.57
_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'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ba Ba -0.3244 2.2819 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 '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      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.5816(4)
_cell_length_b                   12.2757(4)
_cell_length_c                   12.4432(4)
_cell_angle_alpha                61.5850(10)
_cell_angle_beta                 62.3390(10)
_cell_angle_gamma                71.1370(10)
_cell_volume                     1366.16(8)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    4806
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.115
_cell_measurement_theta_min      2.244
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    2.041
_exptl_absorpt_correction_T_max  0.801
_exptl_absorpt_correction_T_min  0.479
_exptl_absorpt_correction_type   EMPIRICAL
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            GREEN
_exptl_crystal_density_diffrn    1.881
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             762
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.12
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0247
_diffrn_reflns_av_unetI/netI     0.0275
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            13715
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        25.115
_diffrn_reflns_theta_max         25.115
_diffrn_reflns_theta_min         2.244
_diffrn_ambient_temperature      100.39
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4473
_reflns_number_total             4806
_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       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         2.340
_refine_diff_density_min         -1.226
_refine_diff_density_rms         0.113
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.090
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     481
_refine_ls_number_reflns         4806
_refine_ls_number_restraints     24
_refine_ls_R_factor_all          0.0512
_refine_ls_R_factor_gt           0.0473
_refine_ls_restrained_S_all      1.088
_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)+(0.0349P)²+8.4129P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1104
_refine_ls_wR_factor_ref         0.1139
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid bond restraints
 O7A, O7
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C23A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
O7A \\sim O7: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
Uanis(C23A) \\sim Ueq: with sigma of 0.05 and sigma for terminal atoms of 0.1
Uanis(O7A) \\sim Ueq, Uanis(O7) \\sim Ueq: with sigma of 0.05 and sigma for
terminal atoms of 0.1
Uanis(C2) = Uanis(C2A)
Uanis(O8) = Uanis(O8A)
Uanis(O7) = Uanis(O7A)
Uanis(N19) = Uanis(N19A)
Uanis(C18) = Uanis(C18A)
4. Others
 Fixed Sof: N19(0.65) N22(0.65) C23(0.65) H23(0.65) C18(0.65) H18(0.65)
 Cl2(0.6) O7(0.7) O8(0.65) O9(0.69) O9A(0.31) Cl1(0.75) O2(0.75) O5(0.67)
 Cl1A(0.25) O5A(0.33) O10(0.7) O10A(0.3) Cl2A(0.4) O2A(0.25) C21(0.65)
 H21A(0.65) H21B(0.65) C2(0.65) H2A(0.65) H2B(0.65) H2C(0.65) C20(0.65)
 C1(0.65) H1A(0.65) H1B(0.65) H1C(0.65) C1A(0.35) H1AA(0.35) H1AB(0.35)
 H1AC(0.35) C21A(0.35) C20A(0.35) H20A(0.35) H20B(0.35) N22A(0.35) C23A(0.35)
 H23A(0.35) C2A(0.35) H2AA(0.35) H2AB(0.35) H2AC(0.35) O8A(0.35) O7A(0.3)
 N19A(0.35) C18A(0.35) H18A(0.35)
5.a Secondary CH2 refined with riding coordinates:
 C21(H21A,H21B), C20A(H20A,H20B)
5.b Aromatic/amide H refined with riding coordinates:
 C25(H25), C26(H26), C27(H27), C23(H23), C14(H14), C18(H18), C15(H15),
 C16(H16), C23A(H23A), C18A(H18A)
5.c Idealised Me refined as rotating group:
 C42(H42A,H42B,H42C), C32(H32A,H32B,H32C), C2(H2A,H2B,H2C), C1(H1A,H1B,H1C),
 C1A(H1AA,H1AB,H1AC), C2A(H2AA,H2AB,H2AC)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
V1 V 0.39345(9) 0.32683(9) 0.58717(9) 0.0323(2) Uani 1 1 d . . . . .
O11 O 0.3221(4) 0.4642(4) 0.4636(4) 0.0349(9) Uani 1 1 d . . . . .
O30 O 0.5456(4) 0.3195(3) 0.4330(3) 0.0336(8) Uani 1 1 d . . . . .
O1 O 0.4245(4) 0.3791(4) 0.6655(4) 0.0427(10) Uani 1 1 d . . . . .
O41 O 0.3007(4) 0.6964(4) 0.3036(4) 0.0451(10) Uani 1 1 d . . . . .
O31 O 0.7622(4) 0.3996(4) 0.2405(4) 0.0482(11) Uani 1 1 d . . . . .
N19 N 0.2147(18) 0.2639(9) 0.704(2) 0.045(3) Uani 0.65 1 d . . P A 1
C29 C 0.6552(6) 0.2394(5) 0.4315(5) 0.0345(12) Uani 1 1 d . . . . .
C12 C 0.2046(5) 0.5315(6) 0.4945(6) 0.0385(13) Uani 1 1 d . . . . .
N22 N 0.4447(13) 0.1372(10) 0.6802(9) 0.031(2) Uani 0.65 1 d . . P A 1
C28 C 0.7738(6) 0.2786(6) 0.3278(6) 0.0399(13) Uani 1 1 d . . . . .
C25 C 0.7808(8) 0.0372(6) 0.5129(8) 0.059(2) Uani 1 1 d . . . . .
H25 H 0.783774 -0.045958 0.576259 0.071 Uiso 1 1 calc R . . . .
C13 C 0.1888(6) 0.6565(6) 0.4100(6) 0.0421(14) Uani 1 1 d . . . . .
C24 C 0.6589(7) 0.1170(6) 0.5271(6) 0.0454(15) Uani 1 1 d . . . . .
C26 C 0.8931(7) 0.0782(7) 0.4099(8) 0.0556(18) Uani 1 1 d . . . . .
H26 H 0.973355 0.023212 0.401540 0.067 Uiso 1 1 calc R . . . .
C27 C 0.8913(7) 0.1988(7) 0.3175(7) 0.0523(17) Uani 1 1 d . . . . .
H27 H 0.970524 0.227358 0.246913 0.063 Uiso 1 1 calc R . . . .
C42 C 0.2946(7) 0.8272(6) 0.2221(7) 0.0535(17) Uani 1 1 d . . . . .
H42A H 0.231289 0.849931 0.180802 0.080 Uiso 1 1 calc GR . . . .
H42B H 0.381676 0.845643 0.153584 0.080 Uiso 1 1 calc GR . . . .
H42C H 0.266748 0.875406 0.276109 0.080 Uiso 1 1 calc GR . . . .
C23 C 0.5540(14) 0.0701(13) 0.6436(13) 0.032(3) Uani 0.65 1 d . . P A 1
H23 H 0.563949 -0.015829 0.698648 0.038 Uiso 0.65 1 calc R . P A 1
C14 C 0.0678(7) 0.7293(8) 0.4371(9) 0.063(2) Uani 1 1 d . . . . .
H14 H 0.057859 0.814916 0.381268 0.076 Uiso 1 1 calc R . . . .
C32 C 0.8831(7) 0.4460(8) 0.1371(8) 0.073(3) Uani 1 1 d . . . . .
H32A H 0.943864 0.437039 0.176228 0.109 Uiso 1 1 calc GR . . . .
H32B H 0.864330 0.534378 0.083879 0.109 Uiso 1 1 calc GR . . . .
H32C H 0.923272 0.398083 0.081106 0.109 Uiso 1 1 calc GR . . . .
C18 C 0.108(2) 0.3400(13) 0.701(2) 0.053(4) Uani 0.65 1 d . . P A 1
H18 H 0.028469 0.306848 0.763337 0.063 Uiso 0.65 1 calc R . P A 1
C17 C 0.0946(6) 0.4809(8) 0.6057(8) 0.0587(19) Uani 1 1 d . . . . .
C15 C -0.0394(7) 0.6755(11) 0.5474(11) 0.087(3) Uani 1 1 d . . . . .
H15 H -0.122934 0.725014 0.564916 0.104 Uiso 1 1 calc R . . . .
C16 C -0.0272(8) 0.5553(11) 0.6293(10) 0.089(3) Uani 1 1 d . . . . .
H16 H -0.101774 0.520815 0.703568 0.107 Uiso 1 1 calc R . . . .
Ba1 Ba 0.51556(3) 0.52398(3) 0.21646(3) 0.03478(13) Uani 1 1 d . . . . .
Cl2 Cl 0.7109(6) 0.3504(4) -0.0001(5) 0.0637(14) Uani 0.6 1 d . . P B 1
O6 O 0.6932(8) 0.4553(10) -0.0027(10) 0.129(3) Uani 1 1 d . . . . .
O7 O 0.639(3) 0.249(3) 0.161(3) 0.130(8) Uani 0.7 1 d . U P B 1
O8 O 0.8101(11) 0.2589(14) -0.0342(14) 0.102(4) Uani 0.65 1 d . . P B 1
O9 O 0.5982(10) 0.3210(8) -0.0293(9) 0.067(2) Uani 0.69 1 d . . P B 1
O9A O 0.697(2) 0.3603(17) -0.0988(19) 0.066(5) Uani 0.31 1 d . . P B 2
Cl1 Cl 0.6885(7) 0.7871(5) -0.0850(7) 0.0479(11) Uani 0.75 1 d . . P C 1
O2 O 0.6726(10) 0.7157(7) 0.0395(6) 0.080(3) Uani 0.75 1 d . . P C 1
O3 O 0.8032(9) 0.8611(8) -0.1226(8) 0.114(3) Uani 1 1 d . . . . .
O4 O 0.6069(13) 0.9084(8) -0.0846(11) 0.158(4) Uani 1 1 d . . . . .
O5 O 0.690(2) 0.7916(14) -0.1906(13) 0.141(8) Uani 0.67 1 d . . P C 1
Cl1A Cl 0.7063(16) 0.8200(14) -0.0901(16) 0.028(2) Uani 0.25 1 d . . P C 2
O5A O 0.778(3) 0.741(3) -0.175(2) 0.105(11) Uani 0.33 1 d . . P C 2
O10 O 0.3771(10) 0.3528(11) 0.2591(9) 0.078(3) Uani 0.7 1 d . . P C 1
O10A O 0.3550(17) 0.4151(19) 0.1947(18) 0.053(4) Uani 0.3 1 d . . P C 2
Cl2A Cl 0.6768(6) 0.2996(8) 0.0390(8) 0.0551(17) Uani 0.4 1 d . . P B 2
O2A O 0.722(3) 0.6526(19) -0.032(3) 0.085(8) Uani 0.25 1 d . . P C 2
C21 C 0.3431(11) 0.0826(9) 0.8095(11) 0.049(2) Uani 0.65 1 d . . P A 1
H21A H 0.341667 0.110218 0.873026 0.059 Uiso 0.65 1 calc R . P A 1
H21B H 0.361124 -0.009782 0.843363 0.059 Uiso 0.65 1 calc R . P A 1
C2 C 0.219(4) 0.050(3) 0.710(3) 0.077(6) Uani 0.65 1 d . . P A 2
H2A H 0.241609 -0.039438 0.729200 0.116 Uiso 0.65 1 calc GR . P A 2
H2B H 0.254382 0.097031 0.614002 0.116 Uiso 0.65 1 calc GR . P A 2
H2C H 0.123459 0.071518 0.743980 0.116 Uiso 0.65 1 calc GR . P A 2
C20 C 0.2122(17) 0.1265(13) 0.7920(18) 0.066(6) Uani 0.65 1 d . . P A 1
C1 C 0.1058(13) 0.1094(16) 0.9299(16) 0.122(8) Uani 0.65 1 d . . P A 1
H1A H 0.102185 0.176151 0.953858 0.183 Uiso 0.65 1 calc GR . P A 1
H1B H 0.127210 0.028213 0.994217 0.183 Uiso 0.65 1 calc GR . P A 1
H1C H 0.020250 0.112960 0.929493 0.183 Uiso 0.65 1 calc GR . P A 1
C1A C 0.311(2) -0.0168(18) 0.8956(19) 0.055(5) Uani 0.35 1 d . . P A 2
H1AA H 0.229462 -0.036397 0.972612 0.083 Uiso 0.35 1 calc GR . P A 2
H1AB H 0.366625 0.014063 0.912819 0.083 Uiso 0.35 1 calc GR . P A 2
H1AC H 0.358363 -0.092347 0.878002 0.083 Uiso 0.35 1 calc GR . P A 2
C21A C 0.279(2) 0.085(2) 0.7743(18) 0.037(4) Uani 0.35 1 d . . P A 2
C20A C 0.187(2) 0.183(2) 0.814(2) 0.045(6) Uani 0.35 1 d . . P A 2
H20A H 0.206033 0.190702 0.879849 0.054 Uiso 0.35 1 calc R . P A 2
H20B H 0.096836 0.161396 0.855873 0.054 Uiso 0.35 1 calc R . P A 2
N22A N 0.405(2) 0.139(3) 0.657(2) 0.067(9) Uani 0.35 1 d . . P A 2
C23A C 0.513(4) 0.076(4) 0.630(4) 0.067(11) Uani 0.35 1 d . U P A 2
H23A H 0.512008 -0.011510 0.677247 0.080 Uiso 0.35 1 calc R . P A 2
C2A C 0.190(8) 0.072(6) 0.743(6) 0.077(6) Uani 0.35 1 d . . P A 1
H2AA H 0.152054 0.132646 0.677622 0.116 Uiso 0.35 1 calc GR . P A 1
H2AB H 0.128231 0.011838 0.812644 0.116 Uiso 0.35 1 calc GR . P A 1
H2AC H 0.272573 0.026960 0.700764 0.116 Uiso 0.35 1 calc GR . P A 1
O8A O 0.851(2) 0.303(3) -0.024(3) 0.102(4) Uani 0.35 1 d . . P B 2
O7A O 0.629(8) 0.301(8) 0.132(7) 0.130(8) Uani 0.3 1 d . U P B 2
N19A N 0.195(4) 0.306(2) 0.699(4) 0.045(3) Uani 0.35 1 d . . P A 2
C18A C 0.090(5) 0.384(3) 0.691(5) 0.053(4) Uani 0.35 1 d . . P A 2
H18A H 0.006331 0.359864 0.755803 0.063 Uiso 0.35 1 calc R . P A 2


_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 O11 1.924(4) . ?
V1 O30 1.927(4) . ?
V1 O1 1.600(4) . ?
V1 N19 2.041(19) . ?
V1 N22 2.071(11) . ?
V1 Ba1 3.8298(9) . ?
V1 N22A 2.03(3) . ?
V1 N19A 2.09(4) . ?
O11 C12 1.331(7) . ?
O11 Ba1 2.745(4) . ?
O30 C29 1.330(6) . ?
O30 Ba1 2.748(4) . ?
O1 Ba1 2.683(4) 2_666 ?
O41 C13 1.368(8) . ?
O41 C42 1.434(7) . ?
O41 Ba1 2.850(4) . ?
O31 C28 1.370(7) . ?
O31 C32 1.444(8) . ?
O31 Ba1 2.849(4) . ?
N19 C18 1.29(2) . ?
N19 C20 1.513(17) . ?
C29 C28 1.404(8) . ?
C29 C24 1.407(8) . ?
C12 C13 1.398(9) . ?
C12 C17 1.408(9) . ?
N22 C23 1.28(2) . ?
N22 C21 1.466(14) . ?
C28 C27 1.387(8) . ?
C25 H25 0.9500 . ?
C25 C24 1.422(10) . ?
C25 C26 1.360(11) . ?
C13 C14 1.383(9) . ?
C24 C23 1.390(16) . ?
C24 C23A 1.63(4) . ?
C26 H26 0.9500 . ?
C26 C27 1.377(10) . ?
C27 H27 0.9500 . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?
C23 H23 0.9500 . ?
C14 H14 0.9500 . ?
C14 C15 1.395(13) . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C18 H18 0.9500 . ?
C18 C17 1.570(16) . ?
C17 C16 1.395(11) . ?
C17 C18A 1.16(4) . ?
C15 H15 0.9500 . ?
C15 C16 1.343(14) . ?
C16 H16 0.9500 . ?
Ba1 O6 2.870(7) . ?
Ba1 O9 2.791(7) 2_665 ?
Ba1 O9A 3.053(18) 2_665 ?
Ba1 O2 2.795(7) . ?
Ba1 O10 2.756(10) . ?
Ba1 O10A 2.782(18) . ?
Ba1 O2A 2.95(3) . ?
Cl2 O6 1.223(10) . ?
Cl2 O7 1.74(3) . ?
Cl2 O8 1.389(12) . ?
Cl2 O9 1.684(10) . ?
O6 Cl2A 1.777(12) . ?
O9A Cl2A 1.44(2) . ?
Cl1 O2 1.323(9) . ?
Cl1 O3 1.615(9) . ?
Cl1 O4 1.484(11) . ?
Cl1 O5 1.281(14) . ?
O3 Cl1A 1.195(15) . ?
O4 Cl1A 1.30(2) . ?
Cl1A O5A 1.54(3) . ?
Cl1A O2A 1.80(3) . ?
O5A O2A 1.52(4) . ?
Cl2A O8A 1.80(3) . ?
Cl2A O7A 1.04(7) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C21 C20 1.517(19) . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C2 C21A 1.53(3) . ?
C20 C1 1.54(2) . ?
C20 C2A 1.24(5) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C1A H1AA 0.9800 . ?
C1A H1AB 0.9800 . ?
C1A H1AC 0.9800 . ?
C1A C21A 1.55(3) . ?
C21A C20A 1.44(3) . ?
C21A N22A 1.56(3) . ?
C20A H20A 0.9900 . ?
C20A H20B 0.9900 . ?
C20A N19A 1.50(3) . ?
N22A C23A 1.23(6) . ?
C23A H23A 0.9500 . ?
C2A H2AA 0.9800 . ?
C2A H2AB 0.9800 . ?
C2A H2AC 0.9800 . ?
N19A C18A 1.30(5) . ?
C18A H18A 0.9500 . ?

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
O11 V1 O30 84.89(16) . . ?
O11 V1 N19 91.4(4) . . ?
O11 V1 N22 151.0(3) . . ?
O11 V1 Ba1 42.68(11) . . ?
O11 V1 N22A 133.6(6) . . ?
O11 V1 N19A 82.1(10) . . ?
O30 V1 N19 141.2(6) . . ?
O30 V1 N22 87.3(3) . . ?
O30 V1 Ba1 42.82(11) . . ?
O30 V1 N22A 88.2(8) . . ?
O30 V1 N19A 148.1(13) . . ?
O1 V1 O11 109.1(2) . . ?
O1 V1 O30 110.7(2) . . ?
O1 V1 N19 107.0(6) . . ?
O1 V1 N22 99.8(3) . . ?
O1 V1 Ba1 111.79(16) . . ?
O1 V1 N22A 116.2(7) . . ?
O1 V1 N19A 101.1(13) . . ?
N19 V1 N22 77.5(4) . . ?
N19 V1 Ba1 127.1(5) . . ?
N22 V1 Ba1 127.2(3) . . ?
N22A V1 Ba1 121.0(8) . . ?
N22A V1 N19A 80.2(10) . . ?
N19A V1 Ba1 121.7(11) . . ?
V1 O11 Ba1 108.95(15) . . ?
C12 O11 V1 125.7(4) . . ?
C12 O11 Ba1 124.7(3) . . ?
V1 O30 Ba1 108.71(15) . . ?
C29 O30 V1 126.3(3) . . ?
C29 O30 Ba1 124.4(3) . . ?
V1 O1 Ba1 176.7(2) . 2_666 ?
C13 O41 C42 116.8(5) . . ?
C13 O41 Ba1 121.4(3) . . ?
C42 O41 Ba1 120.5(4) . . ?
C28 O31 C32 116.2(5) . . ?
C28 O31 Ba1 120.8(3) . . ?
C32 O31 Ba1 120.4(4) . . ?
C18 N19 V1 120.1(11) . . ?
C18 N19 C20 121.9(16) . . ?
C20 N19 V1 118.0(10) . . ?
O30 C29 C28 118.2(5) . . ?
O30 C29 C24 123.6(5) . . ?
C28 C29 C24 118.2(5) . . ?
O11 C12 C13 118.5(5) . . ?
O11 C12 C17 122.8(6) . . ?
C13 C12 C17 118.7(6) . . ?
C23 N22 V1 128.1(8) . . ?
C23 N22 C21 119.4(11) . . ?
C21 N22 V1 112.1(8) . . ?
O31 C28 C29 114.5(5) . . ?
O31 C28 C27 124.1(6) . . ?
C27 C28 C29 121.4(6) . . ?
C24 C25 H25 119.5 . . ?
C26 C25 H25 119.5 . . ?
C26 C25 C24 121.0(6) . . ?
O41 C13 C12 114.3(5) . . ?
O41 C13 C14 125.3(6) . . ?
C14 C13 C12 120.4(6) . . ?
C29 C24 C25 119.0(6) . . ?
C29 C24 C23A 113.4(14) . . ?
C25 C24 C23A 126.7(16) . . ?
C23 C24 C29 124.8(8) . . ?
C23 C24 C25 115.9(8) . . ?
C25 C26 H26 119.7 . . ?
C25 C26 C27 120.5(6) . . ?
C27 C26 H26 119.7 . . ?
C28 C27 H27 120.1 . . ?
C26 C27 C28 119.9(7) . . ?
C26 C27 H27 120.1 . . ?
O41 C42 H42A 109.5 . . ?
O41 C42 H42B 109.5 . . ?
O41 C42 H42C 109.5 . . ?
H42A C42 H42B 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
N22 C23 C24 123.1(12) . . ?
N22 C23 H23 118.5 . . ?
C24 C23 H23 118.5 . . ?
C13 C14 H14 120.3 . . ?
C13 C14 C15 119.3(8) . . ?
C15 C14 H14 120.3 . . ?
O31 C32 H32A 109.5 . . ?
O31 C32 H32B 109.5 . . ?
O31 C32 H32C 109.5 . . ?
H32A C32 H32B 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
N19 C18 H18 116.0 . . ?
N19 C18 C17 128.0(17) . . ?
C17 C18 H18 116.0 . . ?
C12 C17 C18 119.9(9) . . ?
C16 C17 C12 119.9(8) . . ?
C16 C17 C18 120.2(10) . . ?
C18A C17 C12 129(2) . . ?
C18A C17 C16 111(2) . . ?
C14 C15 H15 119.3 . . ?
C16 C15 C14 121.4(7) . . ?
C16 C15 H15 119.3 . . ?
C17 C16 H16 119.9 . . ?
C15 C16 C17 120.3(8) . . ?
C15 C16 H16 119.9 . . ?
O11 Ba1 O30 56.48(11) . . ?
O11 Ba1 O41 55.31(12) . . ?
O11 Ba1 O31 108.68(11) . . ?
O11 Ba1 O6 149.1(2) . . ?
O11 Ba1 O9 109.3(2) . 2_665 ?
O11 Ba1 O9A 89.1(4) . 2_665 ?
O11 Ba1 O2 137.0(2) . . ?
O11 Ba1 O10 70.2(2) . . ?
O11 Ba1 O10A 78.7(3) . . ?
O11 Ba1 O2A 162.4(6) . . ?
O30 Ba1 O41 108.76(11) . . ?
O30 Ba1 O31 55.39(11) . . ?
O30 Ba1 O6 104.5(2) . . ?
O30 Ba1 O9 156.4(2) . 2_665 ?
O30 Ba1 O9A 135.2(4) . 2_665 ?
O30 Ba1 O2 129.2(2) . . ?
O30 Ba1 O10 75.0(2) . . ?
O30 Ba1 O10A 93.2(4) . . ?
O30 Ba1 O2A 128.2(5) . . ?
O1 Ba1 O11 76.24(12) 2_666 . ?
O1 Ba1 O30 76.99(12) 2_666 . ?
O1 Ba1 O41 69.77(13) 2_666 . ?
O1 Ba1 O31 70.84(13) 2_666 . ?
O1 Ba1 O6 126.6(2) 2_666 . ?
O1 Ba1 O9 120.41(18) 2_666 2_665 ?
O1 Ba1 O9A 125.7(4) 2_666 2_665 ?
O1 Ba1 O2 66.56(19) 2_666 . ?
O1 Ba1 O10 144.4(2) 2_666 . ?
O1 Ba1 O10A 154.5(3) 2_666 . ?
O1 Ba1 O2A 88.1(6) 2_666 . ?
O41 Ba1 O6 145.9(2) . . ?
O41 Ba1 O9A 59.4(4) . 2_665 ?
O41 Ba1 O2A 111.8(5) . . ?
O31 Ba1 O41 140.09(13) . . ?
O31 Ba1 O6 67.8(2) . . ?
O31 Ba1 O9A 159.1(4) . 2_665 ?
O31 Ba1 O2A 72.8(5) . . ?
O6 Ba1 O9A 91.3(4) . 2_665 ?
O6 Ba1 O2A 48.3(6) . . ?
O9 Ba1 O41 67.75(19) 2_665 . ?
O9 Ba1 O31 142.0(2) 2_665 . ?
O9 Ba1 O6 78.7(3) 2_665 . ?
O9 Ba1 O9A 22.2(4) 2_665 2_665 ?
O9 Ba1 O2 74.3(3) 2_665 . ?
O2 Ba1 O41 90.9(2) . . ?
O2 Ba1 O31 79.2(2) . . ?
O2 Ba1 O6 73.7(3) . . ?
O2 Ba1 O9A 95.3(4) . 2_665 ?
O10 Ba1 O41 99.2(2) . . ?
O10 Ba1 O31 109.1(3) . . ?
O10 Ba1 O6 81.9(3) . . ?
O10 Ba1 O9 82.5(3) . 2_665 ?
O10 Ba1 O9A 66.0(4) . 2_665 ?
O10 Ba1 O2 149.0(3) . . ?
O10A Ba1 O41 92.0(4) . . ?
O10A Ba1 O31 122.7(4) . . ?
O10A Ba1 O6 78.5(4) . . ?
O10A Ba1 O9A 48.7(6) . 2_665 ?
O10A Ba1 O2A 115.8(7) . . ?
O2A Ba1 O9A 93.6(6) . 2_665 ?
O6 Cl2 O7 109.1(13) . . ?
O6 Cl2 O8 141.8(9) . . ?
O6 Cl2 O9 114.9(6) . . ?
O8 Cl2 O7 93.7(11) . . ?
O8 Cl2 O9 96.6(7) . . ?
O9 Cl2 O7 85.4(11) . . ?
Cl2 O6 Ba1 123.5(7) . . ?
Cl2A O6 Ba1 108.2(5) . . ?
Cl2 O9 Ba1 128.6(5) . 2_665 ?
O2 Cl1 O3 99.1(6) . . ?
O2 Cl1 O4 105.6(7) . . ?
O4 Cl1 O3 81.9(6) . . ?
O5 Cl1 O2 144.6(8) . . ?
O5 Cl1 O3 109.2(10) . . ?
O5 Cl1 O4 99.2(10) . . ?
Cl1 O2 Ba1 128.8(5) . . ?
O3 Cl1A O4 109.0(11) . . ?
O3 Cl1A O5A 93.7(15) . . ?
O3 Cl1A O2A 115.5(16) . . ?
O4 Cl1A O5A 134.7(18) . . ?
O4 Cl1A O2A 134.2(13) . . ?
O5A Cl1A O2A 53.3(15) . . ?
O2A O5A Cl1A 72.3(16) . . ?
O6 Cl2A O8A 74.8(10) . . ?
O9A Cl2A O6 76.6(9) . . ?
O9A Cl2A O8A 82.7(13) . . ?
O7A Cl2A O6 81(5) . . ?
O7A Cl2A O9A 148(4) . . ?
O7A Cl2A O8A 113(5) . . ?
Cl1A O2A Ba1 117.2(15) . . ?
O5A O2A Ba1 155.9(19) . . ?
O5A O2A Cl1A 54.4(14) . . ?
N22 C21 H21A 110.2 . . ?
N22 C21 H21B 110.2 . . ?
N22 C21 C20 107.4(11) . . ?
H21A C21 H21B 108.5 . . ?
C20 C21 H21A 110.2 . . ?
C20 C21 H21B 110.2 . . ?
H2A C2 H2B 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
C21A C2 H2A 109.5 . . ?
C21A C2 H2B 109.5 . . ?
C21A C2 H2C 109.5 . . ?
N19 C20 C21 105.1(13) . . ?
N19 C20 C1 110.3(14) . . ?
C21 C20 C1 106.1(14) . . ?
C2A C20 N19 110(4) . . ?
C2A C20 C21 116(4) . . ?
C2A C20 C1 110(4) . . ?
C20 C1 H1A 109.5 . . ?
C20 C1 H1B 109.5 . . ?
C20 C1 H1C 109.5 . . ?
H1A C1 H1B 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
H1AA C1A H1AB 109.5 . . ?
H1AA C1A H1AC 109.5 . . ?
H1AB C1A H1AC 109.5 . . ?
C21A C1A H1AA 109.5 . . ?
C21A C1A H1AB 109.5 . . ?
C21A C1A H1AC 109.5 . . ?
C2 C21A C1A 119.5(19) . . ?
C2 C21A N22A 102(2) . . ?
C1A C21A N22A 111.6(19) . . ?
C20A C21A C2 106(2) . . ?
C20A C21A C1A 107.5(17) . . ?
C20A C21A N22A 109.9(19) . . ?
C21A C20A H20A 109.3 . . ?
C21A C20A H20B 109.3 . . ?
C21A C20A N19A 112(2) . . ?
H20A C20A H20B 108.0 . . ?
N19A C20A H20A 109.3 . . ?
N19A C20A H20B 109.3 . . ?
C21A N22A V1 114(2) . . ?
C23A N22A V1 119(2) . . ?
C23A N22A C21A 124(3) . . ?
C24 C23A H23A 114.4 . . ?
N22A C23A C24 131(3) . . ?
N22A C23A H23A 114.4 . . ?
C20 C2A H2AA 109.5 . . ?
C20 C2A H2AB 109.5 . . ?
C20 C2A H2AC 109.5 . . ?
H2AA C2A H2AB 109.5 . . ?
H2AA C2A H2AC 109.5 . . ?
H2AB C2A H2AC 109.5 . . ?
Cl2A O7A Ba1 130(6) . . ?
C20A N19A V1 108(2) . . ?
C18A N19A V1 131(3) . . ?
C18A N19A C20A 121(4) . . ?
C17 C18A N19A 121(4) . . ?
C17 C18A H18A 119.3 . . ?
N19A C18A H18A 119.3 . . ?

_olex2_submission_special_instructions 'No special instructions were received'

