# Electronic Supplementary Material (ESI) for Green Chemistry.
# 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_shelx
_database_code_depnum_ccdc_archive 'CCDC 1861933'
loop_
_audit_author_name
_audit_author_address
'Muniappan Sankar'
;Indian Institute of Technology Roorkee
India
;
_audit_update_record             
;
2018-08-14 deposited with the CCDC.	2019-02-19 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C52 H28 Br16 N4 O9 V'
_chemical_formula_sum            'C52 H28 Br16 N4 O9 V'
_chemical_formula_weight         2182.28

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'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   pcab

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

_cell_length_a                   20.733(9)
_cell_length_b                   26.304(12)
_cell_length_c                   28.112(13)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     15331(12)
_cell_formula_units_Z            8
_cell_measurement_temperature    223(2)
_cell_measurement_reflns_used    5640
_cell_measurement_theta_min      2.1
_cell_measurement_theta_max      28.362

_exptl_crystal_description       'square shaped'
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.891
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             8156.0
_exptl_absorpt_coefficient_mu    8.515
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.427
_exptl_absorpt_correction_T_max  0.444
_exptl_absorpt_process_details   '(SADABS; Brucker, 2000)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      223(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            19632
_diffrn_reflns_av_R_equivalents  0.2375
_diffrn_reflns_av_sigmaI/netI    0.2725
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         1.45
_diffrn_reflns_theta_max         19.010
_reflns_number_total             5640
_reflns_number_gt                2634
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker Kappa Apex'
_computing_cell_refinement       'Bruker Kappa Apex'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Bruker SAINT'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1746P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5640
_refine_ls_number_parameters     479
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.2234
_refine_ls_R_factor_gt           0.0783
_refine_ls_wR_factor_ref         0.3034
_refine_ls_wR_factor_gt          0.2369
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_restrained_S_all      1.024
_refine_ls_shift/su_max          0.003
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Br01 Br 0.4541(2) 0.72256(15) 0.56635(13) 0.0818(15) Uani 1 1 d . . .
Br02 Br 0.7840(2) 1.07365(15) 0.48621(15) 0.0906(15) Uani 1 1 d . . .
Br03 Br 0.4675(2) 0.75201(15) 0.41942(14) 0.0834(14) Uani 1 1 d . . .
Br04 Br 0.7817(2) 1.02437(16) 0.62210(14) 0.0874(15) Uani 1 1 d . . .
Br05 Br 0.7522(2) 0.92919(16) 0.32646(13) 0.0821(14) Uani 1 1 d . . .
Br06 Br 0.6201(2) 1.03513(15) 0.35136(15) 0.0905(16) Uani 1 1 d . . .
Br07 Br 0.5139(3) 0.90017(18) 0.68997(14) 0.1016(18) Uani 1 1 d . . .
Br08 Br 0.8573(2) 0.95598(19) 0.41587(15) 0.0970(16) Uani 1 1 d . . .
Br09 Br 0.5607(2) 0.74458(16) 0.65637(13) 0.0890(16) Uani 1 1 d . . .
Br10 Br 0.3646(2) 0.86765(18) 0.57159(15) 0.0959(16) Uani 1 1 d . . .
Br11 Br 0.8452(2) 0.87508(16) 0.55157(17) 0.0955(16) Uani 1 1 d . . .
Br12 Br 0.3557(2) 0.89219(19) 0.42492(16) 0.0997(17) Uani 1 1 d . . .
Br13 Br 0.6934(3) 0.95420(17) 0.69953(13) 0.1037(19) Uani 1 1 d . . .
Br15 Br 0.7462(3) 0.7992(2) 0.64292(18) 0.1174(19) Uani 1 1 d . . .
Br16 Br 0.5854(3) 0.82249(18) 0.33494(19) 0.124(2) Uani 1 1 d . . .
BR17 V 0.6238(3) 0.8811(2) 0.5027(2) 0.0590(19) Uani 1 1 d . . .
O018 O 0.2516(12) 0.8062(9) 0.5509(8) 0.080(8) Uani 1 1 d . . .
O019 N 0.6728(13) 0.9152(9) 0.5583(7) 0.044(8) Uani 1 1 d . . .
O020 C 0.7715(19) 0.9450(12) 0.4251(12) 0.068(11) Uiso 1 1 d . . .
O021 C 0.483(2) 0.9160(13) 0.3947(12) 0.066(11) Uiso 1 1 d . . .
O022 C 0.5102(16) 0.8210(11) 0.5363(10) 0.038(9) Uiso 1 1 d . . .
O023 C 0.4066(17) 0.8072(11) 0.4950(10) 0.049(9) Uiso 1 1 d . . .
O024 O 0.9648(15) 0.9227(13) 0.5742(11) 0.129(12) Uani 1 1 d . . .
O025 C 0.6089(17) 0.9759(12) 0.3134(12) 0.059(10) Uiso 1 1 d . . .
O026 O 0.7433(17) 0.7778(16) 0.7431(10) 0.169(17) Uani 1 1 d . . .
O027 C 0.4476(17) 0.8920(11) 0.4252(10) 0.049(9) Uiso 1 1 d . . .
O028 C 0.588(2) 0.8901(17) 0.2609(16) 0.092(14) Uiso 1 1 d . . .
O029 C 0.6334(18) 0.8491(12) 0.6764(11) 0.052(10) Uiso 1 1 d . . .
O030 O 0.3373(13) 0.7112(9) 0.4156(8) 0.086(8) Uani 1 1 d . . .
N031 O 0.6626(11) 0.8307(8) 0.4901(6) 0.062(7) Uani 1 1 d . . .
N032 N 0.5453(14) 0.8846(9) 0.4532(10) 0.058(8) Uani 1 1 d . . .
N033 C 0.292(2) 0.7580(13) 0.4856(11) 0.072(11) Uiso 1 1 d . . .
H033 H 0.2516 0.7414 0.4824 0.086 Uiso 1 1 calc R . .
N034 N 0.6731(14) 0.9321(9) 0.4606(8) 0.051(8) Uani 1 1 d . . .
N035 N 0.5582(14) 0.8532(9) 0.5510(9) 0.059(8) Uani 1 1 d . . .
N036 C 0.600(2) 0.9765(16) 0.2668(15) 0.080(13) Uiso 1 1 d . . .
C037 C 0.8244(17) 0.9766(12) 0.5233(10) 0.049(9) Uiso 1 1 d . . .
C038 C 0.7186(17) 0.9498(11) 0.5549(10) 0.037(9) Uiso 1 1 d . . .
C039 C 0.589(2) 0.9385(15) 0.2396(14) 0.086(13) Uiso 1 1 d . . .
H039 H 0.5825 0.9427 0.2068 0.104 Uiso 1 1 calc R . .
C040 C 0.5822(16) 0.8352(11) 0.5956(10) 0.044(9) Uiso 1 1 d . . .
C041 O 0.9148(15) 1.0931(11) 0.5187(9) 0.105(10) Uani 1 1 d . . .
C042 C 0.3977(19) 0.7710(13) 0.4599(11) 0.062(10) Uiso 1 1 d . . .
C043 C 0.341(2) 0.7460(14) 0.4532(13) 0.072(11) Uiso 1 1 d . . .
C044 C 0.588(2) 0.8608(15) 0.7087(14) 0.087(13) Uiso 1 1 d . . .
C046 C 0.686(2) 0.8216(14) 0.6881(13) 0.081(12) Uiso 1 1 d . . .
C047 C 0.927(2) 0.9623(17) 0.5530(14) 0.087(13) Uiso 1 1 d . . .
C048 C 0.5940(18) 0.8867(12) 0.3079(12) 0.059(10) Uiso 1 1 d . . .
C049 C 0.5008(17) 0.7799(12) 0.5711(10) 0.051(10) Uiso 1 1 d . . .
C051 C 0.7284(18) 0.9361(12) 0.3883(11) 0.055(10) Uiso 1 1 d . . .
C052 C 0.487(2) 0.8695(13) 0.4636(11) 0.055(10) Uiso 1 1 d . . .
C053 O 0.543(2) 0.8602(13) 0.7828(10) 0.155(16) Uani 1 1 d . . .
C054 C 0.6026(18) 0.9219(12) 0.3895(11) 0.055(10) Uiso 1 1 d . . .
C055 C 0.864(2) 0.9438(14) 0.5428(12) 0.069(11) Uiso 1 1 d . . .
C056 C 0.975(3) 1.1085(19) 0.5267(16) 0.134(19) Uiso 1 1 d . . .
H05A H 0.9782 1.1444 0.5195 0.202 Uiso 1 1 calc R . .
H05B H 1.0041 1.0894 0.5067 0.202 Uiso 1 1 calc R . .
H05C H 0.9855 1.1029 0.5599 0.202 Uiso 1 1 calc R . .
C057 C 0.3568(18) 0.8172(12) 0.5233(11) 0.052(10) Uiso 1 1 d . . .
C058 C 0.899(2) 1.0431(17) 0.5262(13) 0.087(13) Uiso 1 1 d . . .
C061 O 0.606(2) 1.0236(15) 0.2504(10) 0.161(15) Uani 1 1 d . . .
C064 C 0.5450(18) 0.9094(12) 0.4128(12) 0.049(9) Uiso 1 1 d . . .
C065 O 0.5793(17) 0.8462(12) 0.2364(10) 0.125(11) Uani 1 1 d . . .
C066 C 0.299(2) 0.7933(13) 0.5218(12) 0.065(11) Uiso 1 1 d . . .
C072 C 0.4717(15) 0.8326(11) 0.4984(10) 0.039(9) Uiso 1 1 d . . .
C077 C 0.5980(17) 0.9304(12) 0.3344(11) 0.054(10) Uiso 1 1 d . . .
C082 C 0.599(3) 0.8435(17) 0.7550(17) 0.100(15) Uiso 1 1 d . . .
C086 C 0.6591(17) 0.9046(12) 0.6045(12) 0.054(10) Uiso 1 1 d . . .
C088 C 0.280(2) 0.6801(15) 0.4151(13) 0.098(14) Uiso 1 1 d . . .
H08A H 0.2814 0.6574 0.3880 0.147 Uiso 1 1 calc R . .
H08B H 0.2422 0.7017 0.4128 0.147 Uiso 1 1 calc R . .
H08C H 0.2778 0.6603 0.4442 0.147 Uiso 1 1 calc R . .
C100 C 0.5457(17) 0.7897(12) 0.6044(11) 0.054(10) Uiso 1 1 d . . .
C102 C 0.839(2) 1.0249(14) 0.5133(12) 0.073(11) Uiso 1 1 d . . .
C104 C 0.6246(17) 0.8659(12) 0.6235(11) 0.056(10) Uiso 1 1 d . . .
C110 C 0.9480(19) 1.0127(13) 0.5472(11) 0.068(11) Uiso 1 1 d . . .
H110 H 0.9890 1.0247 0.5560 0.082 Uiso 1 1 calc R . .
C116 C 1.028(2) 0.9364(16) 0.5897(14) 0.112(15) Uiso 1 1 d . . .
H11A H 1.0494 0.9068 0.6032 0.169 Uiso 1 1 calc R . .
H11B H 1.0252 0.9629 0.6136 0.169 Uiso 1 1 calc R . .
H11C H 1.0529 0.9487 0.5628 0.169 Uiso 1 1 calc R . .
C119 C 0.647(2) 0.8216(14) 0.7674(14) 0.084(13) Uiso 1 1 d . . .
H119 H 0.6528 0.8143 0.7998 0.101 Uiso 1 1 calc R . .
C120 C 0.590(3) 0.847(2) 0.1846(19) 0.18(2) Uiso 1 1 d . . .
H12A H 0.5790 0.8140 0.1714 0.263 Uiso 1 1 calc R . .
H12B H 0.6344 0.8548 0.1780 0.263 Uiso 1 1 calc R . .
H12C H 0.5622 0.8727 0.1704 0.263 Uiso 1 1 calc R . .
C131 C 0.6984(16) 0.9382(12) 0.6328(11) 0.052(10) Uiso 1 1 d . . .
C136 C 0.552(4) 1.027(3) 0.205(3) 0.27(4) Uiso 1 1 d . . .
H13A H 0.5531 1.0608 0.1912 0.410 Uiso 1 1 calc R . .
H13B H 0.5088 1.0206 0.2176 0.410 Uiso 1 1 calc R . .
H13C H 0.5621 1.0020 0.1812 0.410 Uiso 1 1 calc R . .
C140 C 0.7559(16) 0.9614(11) 0.5159(10) 0.041(9) Uiso 1 1 d . . .
C144 C 0.551(3) 0.836(2) 0.828(2) 0.21(3) Uiso 1 1 d . . .
H14A H 0.5143 0.8434 0.8482 0.312 Uiso 1 1 calc R . .
H14B H 0.5901 0.8483 0.8431 0.312 Uiso 1 1 calc R . .
H14C H 0.5543 0.7994 0.8235 0.312 Uiso 1 1 calc R . .
C147 C 0.6636(18) 0.9300(12) 0.4107(12) 0.057(10) Uiso 1 1 d . . .
Br47 Br 0.4525(2) 0.95620(19) 0.34750(15) 0.1013(17) Uani 1 1 d . . .
C475 C 0.7339(16) 0.9670(12) 0.6013(10) 0.052(9) Uiso 1 1 d . . .
C476 C 0.736(2) 0.9475(13) 0.4721(12) 0.060(11) Uiso 1 1 d . . .
C477 C 0.188(2) 0.7879(17) 0.5437(15) 0.118(16) Uiso 1 1 d . . .
H47A H 0.1601 0.8020 0.5677 0.176 Uiso 1 1 calc R . .
H47B H 0.1883 0.7511 0.5461 0.176 Uiso 1 1 calc R . .
H47C H 0.1735 0.7980 0.5124 0.176 Uiso 1 1 calc R . .
C515 C 0.752(4) 0.763(3) 0.793(2) 0.26(4) Uiso 1 1 d . . .
H51A H 0.7897 0.7416 0.7959 0.397 Uiso 1 1 calc R . .
H51B H 0.7140 0.7437 0.8033 0.397 Uiso 1 1 calc R . .
H51C H 0.7564 0.7928 0.8126 0.397 Uiso 1 1 calc R . .
C514 C 0.691(3) 0.808(2) 0.7369(18) 0.123(17) Uiso 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
Br01 C049 1.80(3) . ?
Br02 C102 1.88(4) . ?
Br03 C042 1.91(4) . ?
Br04 C475 1.90(3) . ?
Br05 C051 1.81(3) . ?
Br06 O025 1.90(3) . ?
Br07 C044 1.92(4) . ?
Br08 O020 1.82(4) . ?
Br09 C100 1.91(3) . ?
Br10 C057 1.91(3) . ?
Br11 C055 1.87(4) . ?
Br12 O027 1.91(4) . ?
Br13 C131 1.93(3) . ?
Br15 C046 1.88(4) . ?
Br16 C048 1.86(3) . ?
BR17 N031 1.59(2) . ?
BR17 N035 2.06(3) . ?
BR17 N034 2.06(3) . ?
BR17 O019 2.07(2) . ?
BR17 N032 2.14(3) . ?
O018 C066 1.32(4) . ?
O018 C477 1.41(5) . ?
O019 C038 1.32(4) . ?
O019 C086 1.36(3) . ?
O020 C051 1.39(4) . ?
O020 C476 1.52(4) . ?
O021 O027 1.29(4) . ?
O021 C064 1.39(4) . ?
O021 Br47 1.81(3) . ?
O022 C072 1.36(4) . ?
O022 N035 1.37(4) . ?
O022 C049 1.47(4) . ?
O023 C057 1.33(4) . ?
O023 C042 1.38(4) . ?
O023 C072 1.51(4) . ?
O024 C116 1.43(5) . ?
O024 C047 1.44(5) . ?
O025 N036 1.32(4) . ?
O025 C077 1.35(4) . ?
O026 C514 1.36(6) . ?
O026 C515 1.47(7) . ?
O027 C052 1.47(4) . ?
O028 C048 1.33(4) . ?
O028 C065 1.36(4) . ?
O028 C039 1.41(5) . ?
O029 C044 1.34(4) . ?
O029 C046 1.35(5) . ?
O029 C104 1.56(4) . ?
O030 C043 1.40(4) . ?
O030 C088 1.44(4) . ?
N032 C064 1.31(4) . ?
N032 C052 1.31(4) . ?
N033 C066 1.39(4) . ?
N033 C043 1.41(5) . ?
N033 H033 0.9400 . ?
N034 C476 1.40(4) . ?
N034 C147 1.42(4) . ?
N035 C040 1.43(4) . ?
N036 C039 1.28(5) . ?
N036 C061 1.33(4) . ?
C037 C055 1.32(4) . ?
C037 C102 1.33(4) . ?
C037 C140 1.49(4) . ?
C038 C140 1.38(4) . ?
C038 C475 1.42(4) . ?
C039 H039 0.9400 . ?
C040 C104 1.43(4) . ?
C040 C100 1.44(4) . ?
C041 C056 1.33(6) . ?
C041 C058 1.37(4) . ?
C042 C043 1.36(5) . ?
C044 C082 1.40(5) . ?
C046 C514 1.42(5) . ?
C047 C110 1.41(5) . ?
C047 C055 1.41(5) . ?
C048 C077 1.37(4) . ?
C049 C100 1.35(4) . ?
C051 C147 1.49(5) . ?
C052 C072 1.41(4) . ?
C053 C144 1.43(6) . ?
C053 C082 1.47(6) . ?
C054 C064 1.40(4) . ?
C054 C147 1.41(4) . ?
C054 C077 1.57(4) . ?
C056 H05A 0.9700 . ?
C056 H05B 0.9700 . ?
C056 H05C 0.9700 . ?
C057 C066 1.35(4) . ?
C058 C102 1.39(5) . ?
C058 C110 1.41(5) . ?
C061 C136 1.70(7) . ?
C065 C120 1.47(5) . ?
C082 C119 1.20(5) . ?
C086 C104 1.35(4) . ?
C086 C131 1.44(4) . ?
C088 H08A 0.9700 . ?
C088 H08B 0.9700 . ?
C088 H08C 0.9700 . ?
C110 H110 0.9400 . ?
C116 H11A 0.9700 . ?
C116 H11B 0.9700 . ?
C116 H11C 0.9700 . ?
C119 C514 1.30(6) . ?
C119 H119 0.9400 . ?
C120 H12A 0.9700 . ?
C120 H12B 0.9700 . ?
C120 H12C 0.9700 . ?
C131 C475 1.38(4) . ?
C136 H13A 0.9700 . ?
C136 H13B 0.9700 . ?
C136 H13C 0.9700 . ?
C140 C476 1.35(4) . ?
C144 H14A 0.9700 . ?
C144 H14B 0.9700 . ?
C144 H14C 0.9700 . ?
C477 H47A 0.9700 . ?
C477 H47B 0.9700 . ?
C477 H47C 0.9700 . ?
C515 H51A 0.9700 . ?
C515 H51B 0.9700 . ?
C515 H51C 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
N031 BR17 N035 100.6(10) . . ?
N031 BR17 N034 99.4(11) . . ?
N035 BR17 N034 160.0(10) . . ?
N031 BR17 O019 106.3(11) . . ?
N035 BR17 O019 88.8(10) . . ?
N034 BR17 O019 84.7(10) . . ?
N031 BR17 N032 106.0(11) . . ?
N035 BR17 N032 86.7(11) . . ?
N034 BR17 N032 88.6(11) . . ?
O019 BR17 N032 147.6(10) . . ?
C066 O018 C477 121(3) . . ?
C038 O019 C086 111(2) . . ?
C038 O019 BR17 126.6(18) . . ?
C086 O019 BR17 122(2) . . ?
C051 O020 C476 110(3) . . ?
C051 O020 Br08 123(3) . . ?
C476 O020 Br08 126(3) . . ?
O027 O021 C064 103(3) . . ?
O027 O021 Br47 125(3) . . ?
C064 O021 Br47 132(3) . . ?
C072 O022 N035 121(3) . . ?
C072 O022 C049 127(3) . . ?
N035 O022 C049 111(3) . . ?
C057 O023 C042 117(3) . . ?
C057 O023 C072 125(3) . . ?
C042 O023 C072 118(3) . . ?
C116 O024 C047 117(4) . . ?
N036 O025 C077 115(3) . . ?
N036 O025 Br06 124(3) . . ?
C077 O025 Br06 120(2) . . ?
C514 O026 C515 112(5) . . ?
O021 O027 C052 112(3) . . ?
O021 O027 Br12 124(3) . . ?
C052 O027 Br12 124(3) . . ?
C048 O028 C065 117(4) . . ?
C048 O028 C039 119(4) . . ?
C065 O028 C039 124(4) . . ?
C044 O029 C046 122(3) . . ?
C044 O029 C104 120(3) . . ?
C046 O029 C104 119(3) . . ?
C043 O030 C088 115(3) . . ?
C064 N032 C052 110(3) . . ?
C064 N032 BR17 126(2) . . ?
C052 N032 BR17 123(2) . . ?
C066 N033 C043 123(4) . . ?
C066 N033 H033 118.5 . . ?
C043 N033 H033 118.5 . . ?
C476 N034 C147 112(3) . . ?
C476 N034 BR17 121(2) . . ?
C147 N034 BR17 118(2) . . ?
O022 N035 C040 108(2) . . ?
O022 N035 BR17 120(2) . . ?
C040 N035 BR17 118(2) . . ?
C039 N036 O025 127(4) . . ?
C039 N036 C061 123(4) . . ?
O025 N036 C061 110(4) . . ?
C055 C037 C102 125(4) . . ?
C055 C037 C140 119(3) . . ?
C102 C037 C140 116(3) . . ?
O019 C038 C140 128(3) . . ?
O019 C038 C475 108(3) . . ?
C140 C038 C475 123(3) . . ?
N036 C039 O028 117(4) . . ?
N036 C039 H039 121.4 . . ?
O028 C039 H039 121.4 . . ?
C104 C040 N035 120(3) . . ?
C104 C040 C100 135(3) . . ?
N035 C040 C100 104(3) . . ?
C056 C041 C058 119(4) . . ?
C043 C042 O023 123(4) . . ?
C043 C042 Br03 116(3) . . ?
O023 C042 Br03 120(3) . . ?
C042 C043 O030 118(4) . . ?
C042 C043 N033 116(4) . . ?
O030 C043 N033 126(4) . . ?
O029 C044 C082 116(4) . . ?
O029 C044 Br07 120(3) . . ?
C082 C044 Br07 124(4) . . ?
O029 C046 C514 115(4) . . ?
O029 C046 Br15 123(3) . . ?
C514 C046 Br15 122(4) . . ?
C110 C047 C055 126(4) . . ?
C110 C047 O024 124(4) . . ?
C055 C047 O024 110(4) . . ?
O028 C048 C077 119(3) . . ?
O028 C048 Br16 117(3) . . ?
C077 C048 Br16 123(3) . . ?
C100 C049 O022 103(3) . . ?
C100 C049 Br01 126(2) . . ?
O022 C049 Br01 130(2) . . ?
O020 C051 C147 106(3) . . ?
O020 C051 Br05 124(3) . . ?
C147 C051 Br05 130(3) . . ?
N032 C052 C072 124(3) . . ?
N032 C052 O027 103(3) . . ?
C072 C052 O027 132(4) . . ?
C144 C053 C082 104(4) . . ?
C064 C054 C147 127(3) . . ?
C064 C054 C077 116(3) . . ?
C147 C054 C077 117(3) . . ?
C037 C055 C047 116(4) . . ?
C037 C055 Br11 124(3) . . ?
C047 C055 Br11 120(3) . . ?
C041 C056 H05A 109.5 . . ?
C041 C056 H05B 109.5 . . ?
H05A C056 H05B 109.5 . . ?
C041 C056 H05C 109.5 . . ?
H05A C056 H05C 109.5 . . ?
H05B C056 H05C 109.5 . . ?
O023 C057 C066 125(3) . . ?
O023 C057 Br10 120(3) . . ?
C066 C057 Br10 115(3) . . ?
C041 C058 C102 120(4) . . ?
C041 C058 C110 116(4) . . ?
C102 C058 C110 124(4) . . ?
N036 C061 C136 104(4) . . ?
N032 C064 O021 113(3) . . ?
N032 C064 C054 121(3) . . ?
O021 C064 C054 126(4) . . ?
O028 C065 C120 118(4) . . ?
O018 C066 C057 121(3) . . ?
O018 C066 N033 123(4) . . ?
C057 C066 N033 116(4) . . ?
O022 C072 C052 124(3) . . ?
O022 C072 O023 118(3) . . ?
C052 C072 O023 117(3) . . ?
O025 C077 C048 121(3) . . ?
O025 C077 C054 123(3) . . ?
C048 C077 C054 115(3) . . ?
C119 C082 C044 124(5) . . ?
C119 C082 C053 130(5) . . ?
C044 C082 C053 106(4) . . ?
C104 C086 O019 130(3) . . ?
C104 C086 C131 123(3) . . ?
O019 C086 C131 106(3) . . ?
O030 C088 H08A 109.5 . . ?
O030 C088 H08B 109.5 . . ?
H08A C088 H08B 109.5 . . ?
O030 C088 H08C 109.5 . . ?
H08A C088 H08C 109.5 . . ?
H08B C088 H08C 109.5 . . ?
C049 C100 C040 114(3) . . ?
C049 C100 Br09 122(3) . . ?
C040 C100 Br09 124(3) . . ?
C037 C102 C058 118(4) . . ?
C037 C102 Br02 127(3) . . ?
C058 C102 Br02 115(3) . . ?
C086 C104 C040 122(3) . . ?
C086 C104 O029 122(3) . . ?
C040 C104 O029 116(3) . . ?
C047 C110 C058 111(4) . . ?
C047 C110 H110 124.5 . . ?
C058 C110 H110 124.5 . . ?
O024 C116 H11A 109.5 . . ?
O024 C116 H11B 109.5 . . ?
H11A C116 H11B 109.5 . . ?
O024 C116 H11C 109.5 . . ?
H11A C116 H11C 109.5 . . ?
H11B C116 H11C 109.5 . . ?
C082 C119 C514 121(5) . . ?
C082 C119 H119 119.4 . . ?
C514 C119 H119 119.4 . . ?
C065 C120 H12A 109.5 . . ?
C065 C120 H12B 109.5 . . ?
H12A C120 H12B 109.5 . . ?
C065 C120 H12C 109.5 . . ?
H12A C120 H12C 109.5 . . ?
H12B C120 H12C 109.5 . . ?
C475 C131 C086 107(3) . . ?
C475 C131 Br13 122(2) . . ?
C086 C131 Br13 130(3) . . ?
C061 C136 H13A 109.5 . . ?
C061 C136 H13B 109.5 . . ?
H13A C136 H13B 109.5 . . ?
C061 C136 H13C 109.5 . . ?
H13A C136 H13C 109.5 . . ?
H13B C136 H13C 109.5 . . ?
C476 C140 C038 120(3) . . ?
C476 C140 C037 120(3) . . ?
C038 C140 C037 119(3) . . ?
C053 C144 H14A 109.5 . . ?
C053 C144 H14B 109.5 . . ?
H14A C144 H14B 109.5 . . ?
C053 C144 H14C 109.5 . . ?
H14A C144 H14C 109.5 . . ?
H14B C144 H14C 109.5 . . ?
C054 C147 N034 123(3) . . ?
C054 C147 C051 130(3) . . ?
N034 C147 C051 107(3) . . ?
C131 C475 C038 107(3) . . ?
C131 C475 Br04 121(2) . . ?
C038 C475 Br04 131(2) . . ?
C140 C476 N034 125(3) . . ?
C140 C476 O020 131(4) . . ?
N034 C476 O020 104(3) . . ?
O018 C477 H47A 109.5 . . ?
O018 C477 H47B 109.5 . . ?
H47A C477 H47B 109.5 . . ?
O018 C477 H47C 109.5 . . ?
H47A C477 H47C 109.5 . . ?
H47B C477 H47C 109.5 . . ?
O026 C515 H51A 109.5 . . ?
O026 C515 H51B 109.5 . . ?
H51A C515 H51B 109.5 . . ?
O026 C515 H51C 109.5 . . ?
H51A C515 H51C 109.5 . . ?
H51B C515 H51C 109.5 . . ?
C119 C514 O026 130(5) . . ?
C119 C514 C046 121(5) . . ?
O026 C514 C046 109(5) . . ?

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
N031 BR17 O019 C038 92(3) . . . . ?
N035 BR17 O019 C038 -167(3) . . . . ?
N034 BR17 O019 C038 -6(3) . . . . ?
N032 BR17 O019 C038 -85(3) . . . . ?
N031 BR17 O019 C086 -90(2) . . . . ?
N035 BR17 O019 C086 11(2) . . . . ?
N034 BR17 O019 C086 172(2) . . . . ?
N032 BR17 O019 C086 93(3) . . . . ?
C064 O021 O027 C052 0(4) . . . . ?
Br47 O021 O027 C052 -171(2) . . . . ?
C064 O021 O027 Br12 173(2) . . . . ?
Br47 O021 O027 Br12 2(5) . . . . ?
N031 BR17 N032 C064 -95(3) . . . . ?
N035 BR17 N032 C064 165(3) . . . . ?
N034 BR17 N032 C064 5(3) . . . . ?
O019 BR17 N032 C064 83(3) . . . . ?
N031 BR17 N032 C052 98(3) . . . . ?
N035 BR17 N032 C052 -2(3) . . . . ?
N034 BR17 N032 C052 -162(3) . . . . ?
O019 BR17 N032 C052 -84(3) . . . . ?
N031 BR17 N034 C476 -72(3) . . . . ?
N035 BR17 N034 C476 106(4) . . . . ?
O019 BR17 N034 C476 34(2) . . . . ?
N032 BR17 N034 C476 -178(2) . . . . ?
N031 BR17 N034 C147 73(2) . . . . ?
N035 BR17 N034 C147 -110(3) . . . . ?
O019 BR17 N034 C147 178(2) . . . . ?
N032 BR17 N034 C147 -33(2) . . . . ?
C072 O022 N035 C040 170(3) . . . . ?
C049 O022 N035 C040 0(3) . . . . ?
C072 O022 N035 BR17 -50(4) . . . . ?
C049 O022 N035 BR17 139(2) . . . . ?
N031 BR17 N035 O022 -69(2) . . . . ?
N034 BR17 N035 O022 114(3) . . . . ?
O019 BR17 N035 O022 -175(2) . . . . ?
N032 BR17 N035 O022 37(2) . . . . ?
N031 BR17 N035 C040 67(2) . . . . ?
N034 BR17 N035 C040 -111(3) . . . . ?
O019 BR17 N035 C040 -40(2) . . . . ?
N032 BR17 N035 C040 172(2) . . . . ?
C077 O025 N036 C039 -8(7) . . . . ?
Br06 O025 N036 C039 -176(4) . . . . ?
C077 O025 N036 C061 174(4) . . . . ?
Br06 O025 N036 C061 5(6) . . . . ?
C086 O019 C038 C140 163(3) . . . . ?
BR17 O019 C038 C140 -19(5) . . . . ?
C086 O019 C038 C475 -5(4) . . . . ?
BR17 O019 C038 C475 174(2) . . . . ?
O025 N036 C039 O028 -2(7) . . . . ?
C061 N036 C039 O028 176(5) . . . . ?
C048 O028 C039 N036 5(7) . . . . ?
C065 O028 C039 N036 -178(4) . . . . ?
O022 N035 C040 C104 -169(3) . . . . ?
BR17 N035 C040 C104 51(4) . . . . ?
O022 N035 C040 C100 2(3) . . . . ?
BR17 N035 C040 C100 -139(2) . . . . ?
C057 O023 C042 C043 0(5) . . . . ?
C072 O023 C042 C043 -180(3) . . . . ?
C057 O023 C042 Br03 -177(2) . . . . ?
C072 O023 C042 Br03 3(4) . . . . ?
O023 C042 C043 O030 178(3) . . . . ?
Br03 C042 C043 O030 -4(4) . . . . ?
O023 C042 C043 N033 -2(5) . . . . ?
Br03 C042 C043 N033 176(2) . . . . ?
C088 O030 C043 C042 170(3) . . . . ?
C088 O030 C043 N033 -10(5) . . . . ?
C066 N033 C043 C042 0(5) . . . . ?
C066 N033 C043 O030 -179(3) . . . . ?
C046 O029 C044 C082 1(6) . . . . ?
C104 O029 C044 C082 179(3) . . . . ?
C046 O029 C044 Br07 -180(3) . . . . ?
C104 O029 C044 Br07 -2(5) . . . . ?
C044 O029 C046 C514 -3(6) . . . . ?
C104 O029 C046 C514 180(3) . . . . ?
C044 O029 C046 Br15 174(3) . . . . ?
C104 O029 C046 Br15 -4(5) . . . . ?
C116 O024 C047 C110 0(6) . . . . ?
C116 O024 C047 C055 -176(3) . . . . ?
C065 O028 C048 C077 -175(4) . . . . ?
C039 O028 C048 C077 3(6) . . . . ?
C065 O028 C048 Br16 -2(6) . . . . ?
C039 O028 C048 Br16 175(3) . . . . ?
C072 O022 C049 C100 -171(3) . . . . ?
N035 O022 C049 C100 -1(4) . . . . ?
C072 O022 C049 Br01 21(5) . . . . ?
N035 O022 C049 Br01 -169(2) . . . . ?
C476 O020 C051 C147 -3(4) . . . . ?
Br08 O020 C051 C147 -179(2) . . . . ?
C476 O020 C051 Br05 -179(2) . . . . ?
Br08 O020 C051 Br05 5(4) . . . . ?
C064 N032 C052 C072 165(3) . . . . ?
BR17 N032 C052 C072 -26(5) . . . . ?
C064 N032 C052 O027 -4(4) . . . . ?
BR17 N032 C052 O027 164.7(19) . . . . ?
O021 O027 C052 N032 3(4) . . . . ?
Br12 O027 C052 N032 -171(2) . . . . ?
O021 O027 C052 C072 -166(3) . . . . ?
Br12 O027 C052 C072 21(5) . . . . ?
C102 C037 C055 C047 0(5) . . . . ?
C140 C037 C055 C047 -174(3) . . . . ?
C102 C037 C055 Br11 -174(3) . . . . ?
C140 C037 C055 Br11 12(5) . . . . ?
C110 C047 C055 C037 4(6) . . . . ?
O024 C047 C055 C037 180(3) . . . . ?
C110 C047 C055 Br11 179(3) . . . . ?
O024 C047 C055 Br11 -6(4) . . . . ?
C042 O023 C057 C066 3(5) . . . . ?
C072 O023 C057 C066 -177(3) . . . . ?
C042 O023 C057 Br10 -179(2) . . . . ?
C072 O023 C057 Br10 1(5) . . . . ?
C056 C041 C058 C102 -173(4) . . . . ?
C056 C041 C058 C110 7(5) . . . . ?
C039 N036 C061 C136 37(6) . . . . ?
O025 N036 C061 C136 -145(4) . . . . ?
C052 N032 C064 O021 5(4) . . . . ?
BR17 N032 C064 O021 -164(2) . . . . ?
C052 N032 C064 C054 -169(3) . . . . ?
BR17 N032 C064 C054 23(4) . . . . ?
O027 O021 C064 N032 -3(4) . . . . ?
Br47 O021 C064 N032 167(2) . . . . ?
O027 O021 C064 C054 170(3) . . . . ?
Br47 O021 C064 C054 -20(5) . . . . ?
C147 C054 C064 N032 -28(5) . . . . ?
C077 C054 C064 N032 156(3) . . . . ?
C147 C054 C064 O021 160(3) . . . . ?
C077 C054 C064 O021 -17(5) . . . . ?
C048 O028 C065 C120 -165(4) . . . . ?
C039 O028 C065 C120 18(7) . . . . ?
C477 O018 C066 C057 168(4) . . . . ?
C477 O018 C066 N033 -6(5) . . . . ?
O023 C057 C066 O018 -179(3) . . . . ?
Br10 C057 C066 O018 2(5) . . . . ?
O023 C057 C066 N033 -4(5) . . . . ?
Br10 C057 C066 N033 177(2) . . . . ?
C043 N033 C066 O018 177(3) . . . . ?
C043 N033 C066 C057 2(5) . . . . ?
N035 O022 C072 C052 18(5) . . . . ?
C049 O022 C072 C052 -173(3) . . . . ?
N035 O022 C072 O023 -158(3) . . . . ?
C049 O022 C072 O023 11(5) . . . . ?
N032 C052 C072 O022 24(5) . . . . ?
O027 C052 C072 O022 -169(3) . . . . ?
N032 C052 C072 O023 -160(3) . . . . ?
O027 C052 C072 O023 6(5) . . . . ?
C057 O023 C072 O022 71(4) . . . . ?
C042 O023 C072 O022 -110(3) . . . . ?
C057 O023 C072 C052 -105(4) . . . . ?
C042 O023 C072 C052 75(4) . . . . ?
N036 O025 C077 C048 15(5) . . . . ?
Br06 O025 C077 C048 -176(3) . . . . ?
N036 O025 C077 C054 -177(3) . . . . ?
Br06 O025 C077 C054 -8(5) . . . . ?
O028 C048 C077 O025 -13(6) . . . . ?
Br16 C048 C077 O025 175(3) . . . . ?
O028 C048 C077 C054 178(4) . . . . ?
Br16 C048 C077 C054 7(5) . . . . ?
C064 C054 C077 O025 115(4) . . . . ?
C147 C054 C077 O025 -63(5) . . . . ?
C064 C054 C077 C048 -77(4) . . . . ?
C147 C054 C077 C048 106(4) . . . . ?
O029 C044 C082 C119 4(7) . . . . ?
Br07 C044 C082 C119 -175(4) . . . . ?
O029 C044 C082 C053 -179(3) . . . . ?
Br07 C044 C082 C053 2(5) . . . . ?
C144 C053 C082 C119 -11(7) . . . . ?
C144 C053 C082 C044 172(4) . . . . ?
C038 O019 C086 C104 -167(4) . . . . ?
BR17 O019 C086 C104 15(5) . . . . ?
C038 O019 C086 C131 3(4) . . . . ?
BR17 O019 C086 C131 -175(2) . . . . ?
O022 C049 C100 C040 3(4) . . . . ?
Br01 C049 C100 C040 171(2) . . . . ?
O022 C049 C100 Br09 -175(2) . . . . ?
Br01 C049 C100 Br09 -6(4) . . . . ?
C104 C040 C100 C049 166(4) . . . . ?
N035 C040 C100 C049 -3(4) . . . . ?
C104 C040 C100 Br09 -17(6) . . . . ?
N035 C040 C100 Br09 174(2) . . . . ?
C055 C037 C102 C058 -3(6) . . . . ?
C140 C037 C102 C058 171(3) . . . . ?
C055 C037 C102 Br02 -179(3) . . . . ?
C140 C037 C102 Br02 -5(4) . . . . ?
C041 C058 C102 C037 -177(3) . . . . ?
C110 C058 C102 C037 4(6) . . . . ?
C041 C058 C102 Br02 0(5) . . . . ?
C110 C058 C102 Br02 -180(3) . . . . ?
O019 C086 C104 C040 -16(6) . . . . ?
C131 C086 C104 C040 175(3) . . . . ?
O019 C086 C104 O029 158(3) . . . . ?
C131 C086 C104 O029 -10(5) . . . . ?
N035 C040 C104 C086 -20(5) . . . . ?
C100 C040 C104 C086 172(4) . . . . ?
N035 C040 C104 O029 165(3) . . . . ?
C100 C040 C104 O029 -2(6) . . . . ?
C044 O029 C104 C086 106(4) . . . . ?
C046 O029 C104 C086 -76(4) . . . . ?
C044 O029 C104 C040 -79(4) . . . . ?
C046 O029 C104 C040 99(4) . . . . ?
C055 C047 C110 C058 -4(6) . . . . ?
O024 C047 C110 C058 -179(4) . . . . ?
C041 C058 C110 C047 -180(3) . . . . ?
C102 C058 C110 C047 0(5) . . . . ?
C044 C082 C119 C514 -7(8) . . . . ?
C053 C082 C119 C514 177(5) . . . . ?
C104 C086 C131 C475 170(3) . . . . ?
O019 C086 C131 C475 0(4) . . . . ?
C104 C086 C131 Br13 -22(5) . . . . ?
O019 C086 C131 Br13 167(2) . . . . ?
O019 C038 C140 C476 19(5) . . . . ?
C475 C038 C140 C476 -174(3) . . . . ?
O019 C038 C140 C037 -145(3) . . . . ?
C475 C038 C140 C037 21(4) . . . . ?
C055 C037 C140 C476 -102(4) . . . . ?
C102 C037 C140 C476 84(4) . . . . ?
C055 C037 C140 C038 62(4) . . . . ?
C102 C037 C140 C038 -112(3) . . . . ?
C064 C054 C147 N034 -8(5) . . . . ?
C077 C054 C147 N034 169(2) . . . . ?
C064 C054 C147 C051 170(3) . . . . ?
C077 C054 C147 C051 -13(5) . . . . ?
C476 N034 C147 C054 -172(3) . . . . ?
BR17 N034 C147 C054 41(4) . . . . ?
C476 N034 C147 C051 10(3) . . . . ?
BR17 N034 C147 C051 -138(2) . . . . ?
O020 C051 C147 C054 178(3) . . . . ?
Br05 C051 C147 C054 -7(5) . . . . ?
O020 C051 C147 N034 -4(3) . . . . ?
Br05 C051 C147 N034 172(2) . . . . ?
C086 C131 C475 C038 -2(4) . . . . ?
Br13 C131 C475 C038 -171(2) . . . . ?
C086 C131 C475 Br04 169(2) . . . . ?
Br13 C131 C475 Br04 1(4) . . . . ?
O019 C038 C475 C131 4(4) . . . . ?
C140 C038 C475 C131 -164(3) . . . . ?
O019 C038 C475 Br04 -166(3) . . . . ?
C140 C038 C475 Br04 25(5) . . . . ?
C038 C140 C476 N034 15(5) . . . . ?
C037 C140 C476 N034 180(3) . . . . ?
C038 C140 C476 O020 -165(3) . . . . ?
C037 C140 C476 O020 -1(5) . . . . ?
C147 N034 C476 C140 168(3) . . . . ?
BR17 N034 C476 C140 -45(4) . . . . ?
C147 N034 C476 O020 -11(3) . . . . ?
BR17 N034 C476 O020 135(2) . . . . ?
C051 O020 C476 C140 -171(3) . . . . ?
Br08 O020 C476 C140 5(5) . . . . ?
C051 O020 C476 N034 9(3) . . . . ?
Br08 O020 C476 N034 -175(2) . . . . ?
C082 C119 C514 O026 -171(5) . . . . ?
C082 C119 C514 C046 5(8) . . . . ?
C515 O026 C514 C119 -5(9) . . . . ?
C515 O026 C514 C046 179(5) . . . . ?
O029 C046 C514 C119 0(7) . . . . ?
Br15 C046 C514 C119 -177(4) . . . . ?
O029 C046 C514 O026 176(4) . . . . ?
Br15 C046 C514 O026 0(6) . . . . ?

_diffrn_measured_fraction_theta_max 0.914
_diffrn_reflns_theta_full        19.01
_diffrn_measured_fraction_theta_full 0.914
_refine_diff_density_max         1.346
_refine_diff_density_min         -0.911
_refine_diff_density_rms         0.233
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: Acetonitrile and Hexane'
####################################################################### 
# 
# 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_ups2724ms_tw_vttp_br_0m
_database_code_depnum_ccdc_archive 'CCDC 1861934'
loop_
_audit_author_name
_audit_author_address
'Muniappan Sankar'
;Indian Institute of Technology Roorkee
India
;
_audit_update_record             
;
2018-08-14 deposited with the CCDC.	2019-02-19 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C27.50 H22 N3 O5 V0.50'
_chemical_formula_weight         499.95

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'

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   pccn

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

_cell_length_a                   13.829(5)
_cell_length_b                   14.439(5)
_cell_length_c                   26.153(5)
_cell_angle_alpha                90.000(5)
_cell_angle_beta                 90.000(5)
_cell_angle_gamma                90.000(5)
_cell_volume                     5222(3)
_cell_formula_units_Z            8
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      2.1
_cell_measurement_theta_max      28.362

_exptl_crystal_description       'square shaped'
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.272
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2076
_exptl_absorpt_coefficient_mu    0.253
_exptl_absorpt_correction_type   multi-scane
_exptl_absorpt_correction_T_min  0.427
_exptl_absorpt_correction_T_max  0.444
_exptl_absorpt_process_details   '(SADABS; Brucker, 2000)'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            57295
_diffrn_reflns_av_R_equivalents  0.0596
_diffrn_reflns_av_sigmaI/netI    0.0456
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_theta_min         1.56
_diffrn_reflns_theta_max         28.38
_reflns_number_total             6490
_reflns_number_gt                3816
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker Kappa Apex'
_computing_cell_refinement       'Bruker Kappa Apex'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Bruker SAINT'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.2000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6490
_refine_ls_number_parameters     333
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.2466
_refine_ls_R_factor_gt           0.1927
_refine_ls_wR_factor_ref         0.5556
_refine_ls_wR_factor_gt          0.5193
_refine_ls_goodness_of_fit_ref   2.181
_refine_ls_restrained_S_all      2.181
_refine_ls_shift/su_max          1.776
_refine_ls_shift/su_mean         0.021

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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
V001 V 0.2500 0.2500 0.14841(7) 0.0347(6) Uani 1 2 d S . .
N102 N 0.2206(4) 0.3860(4) 0.12764(19) 0.0257(12) Uani 1 1 d . . .
O003 O 0.5842(5) 0.6958(4) 0.0481(2) 0.0625(18) Uani 1 1 d . . .
N101 N 0.1072(4) 0.2203(4) 0.1293(2) 0.0264(12) Uani 1 1 d . . .
O005 O 0.4983(5) 0.7125(4) 0.2229(2) 0.0595(18) Uani 1 1 d . . .
O006 O -0.2260(4) 0.4943(5) 0.2259(2) 0.064(2) Uani 1 1 d . . .
C202 C 0.0413(4) 0.3788(5) 0.1276(2) 0.0278(15) Uani 1 1 d . . .
C201 C 0.0331(5) 0.2840(5) 0.1281(2) 0.0291(15) Uani 1 1 d . . .
O601 O -0.2037(5) 0.5890(5) 0.0519(2) 0.067(2) Uani 1 1 d . . .
C010 C 0.2842(5) 0.4572(5) 0.1267(2) 0.0292(15) Uani 1 1 d . . .
C011 C 0.1296(5) 0.4268(5) 0.1262(2) 0.0295(15) Uani 1 1 d . . .
C012 C 0.0647(5) 0.1348(5) 0.1288(2) 0.0268(14) Uani 1 1 d . . .
C013 C 0.3855(5) 0.4489(5) 0.1284(2) 0.0278(15) Uani 1 1 d . . .
C014 C -0.0991(5) 0.4403(5) 0.1756(3) 0.0365(17) Uani 1 1 d . . .
H014 H -0.0765 0.4078 0.2039 0.044 Uiso 1 1 calc R . .
C015 C 0.4465(5) 0.5859(5) 0.1746(3) 0.0363(17) Uani 1 1 d . . .
H015 H 0.4154 0.5626 0.2034 0.044 Uiso 1 1 calc R . .
O016 O 0.2500 0.2500 0.2087(3) 0.0443(19) Uani 1 2 d S . .
C017 C 0.4436(5) 0.5391(5) 0.1314(2) 0.0287(15) Uani 1 1 d . . .
C018 C 0.4977(5) 0.6736(6) 0.1777(3) 0.0392(17) Uani 1 1 d . . .
C019 C 0.4881(5) 0.5707(5) 0.0861(3) 0.0376(17) Uani 1 1 d . . .
H019 H 0.4854 0.5369 0.0558 0.045 Uiso 1 1 calc R . .
C020 C -0.0499(5) 0.4360(5) 0.1302(3) 0.0338(16) Uani 1 1 d . . .
C021 C 0.1384(5) 0.5262(5) 0.1244(3) 0.0398(18) Uani 1 1 d . . .
H021 H 0.0880 0.5688 0.1232 0.048 Uiso 1 1 calc R . .
C023 C -0.0814(5) 0.4833(5) 0.0887(3) 0.0366(17) Uani 1 1 d . . .
H023 H -0.0466 0.4807 0.0583 0.044 Uiso 1 1 calc R . .
C024 C 0.5371(5) 0.6565(5) 0.0892(3) 0.0375(17) Uani 1 1 d . . .
C025 C 0.2356(5) 0.5458(5) 0.1246(3) 0.0408(19) Uani 1 1 d . . .
H025 H 0.2642 0.6041 0.1235 0.049 Uiso 1 1 calc R . .
C026 C -0.0391(5) 0.1456(5) 0.1272(3) 0.0376(17) Uani 1 1 d . . .
H026 H -0.0843 0.0980 0.1263 0.045 Uiso 1 1 calc R . .
C027 C -0.2164(5) 0.5409(6) 0.1377(3) 0.0420(19) Uani 1 1 d . . .
H027 H -0.2724 0.5762 0.1400 0.050 Uiso 1 1 calc R . .
C028 C 0.5424(5) 0.7067(5) 0.1343(3) 0.0373(17) Uani 1 1 d . . .
H028 H 0.5760 0.7625 0.1353 0.045 Uiso 1 1 calc R . .
C029 C -0.0583(5) 0.2347(5) 0.1273(3) 0.0398(18) Uani 1 1 d . . .
H029 H -0.1195 0.2614 0.1269 0.048 Uiso 1 1 calc R . .
C030 C -0.1655(6) 0.5360(5) 0.0914(3) 0.0420(19) Uani 1 1 d . . .
C031 C -0.1830(5) 0.4933(6) 0.1793(3) 0.0418(19) Uani 1 1 d . . .
N032 N -0.2500 0.2500 0.3327(12) 0.155(11) Uani 1 2 d S . .
C034 C 0.5842(8) 0.6465(8) 0.0006(3) 0.072(3) Uani 1 1 d . . .
H03A H 0.6138 0.5870 0.0053 0.108 Uiso 1 1 calc R . .
H03B H 0.6199 0.6810 -0.0244 0.108 Uiso 1 1 calc R . .
H03C H 0.5188 0.6384 -0.0109 0.108 Uiso 1 1 calc R . .
C035 C 0.5416(8) 0.8036(7) 0.2281(4) 0.069(3) Uani 1 1 d . . .
H03D H 0.5148 0.8444 0.2029 0.103 Uiso 1 1 calc R . .
H03E H 0.6102 0.7990 0.2234 0.103 Uiso 1 1 calc R . .
H03F H 0.5283 0.8275 0.2617 0.103 Uiso 1 1 calc R . .
C036 C -0.3111(7) 0.5470(8) 0.2330(3) 0.063(3) Uani 1 1 d . . .
H03G H -0.2974 0.6112 0.2267 0.095 Uiso 1 1 calc R . .
H03H H -0.3338 0.5395 0.2674 0.095 Uiso 1 1 calc R . .
H03I H -0.3599 0.5262 0.2096 0.095 Uiso 1 1 calc R . .
C037 C -0.1501(8) 0.5943(9) 0.0063(4) 0.081(3) Uani 1 1 d . . .
H03J H -0.0911 0.6275 0.0124 0.121 Uiso 1 1 calc R . .
H03K H -0.1874 0.6260 -0.0192 0.121 Uiso 1 1 calc R . .
H03L H -0.1353 0.5329 -0.0054 0.121 Uiso 1 1 calc R . .
C038 C -0.2500 0.2500 0.2918(14) 0.110(8) Uani 1 2 d S . .
C040 C -0.2500 0.2500 0.2430(16) 0.170(15) Uani 1 2 d S . .
N7 N 0.2500 0.2500 0.1059(9) 0.25(3) Uani 1 2 d S . .
O65 O -0.2500 0.2500 0.2117(16) 1.14(19) Uani 1 2 d S . .
C802 C 0.2500 0.2500 0.089(3) 1.4(3) Uani 1 2 d S . .


_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 N7 1.11(2) . ?
V001 O016 1.577(8) . ?
V001 C802 1.56(7) . ?
V001 N102 2.078(6) 2 ?
V001 N102 2.078(6) . ?
V001 N101 2.081(5) 2 ?
V001 N101 2.081(5) . ?
N102 C010 1.352(9) . ?
N102 C011 1.391(8) . ?
O003 C024 1.379(8) . ?
O003 C034 1.431(11) . ?
N101 C012 1.368(9) . ?
N101 C201 1.378(8) . ?
O005 C018 1.309(9) . ?
O005 C035 1.451(11) . ?
O006 C031 1.357(9) . ?
O006 C036 1.414(10) . ?
C202 C201 1.374(10) . ?
C202 C011 1.404(9) . ?
C202 C020 1.507(9) . ?
C201 C029 1.450(10) . ?
O601 C030 1.388(9) . ?
O601 C037 1.407(12) . ?
C010 C013 1.407(9) . ?
C010 C025 1.446(10) . ?
C011 C021 1.441(10) . ?
C012 C013 1.391(10) 2 ?
C012 C026 1.444(9) . ?
C013 C012 1.391(10) 2 ?
C013 C017 1.532(9) . ?
C014 C020 1.370(10) . ?
C014 C031 1.394(10) . ?
C014 H014 0.9300 . ?
C015 C017 1.317(9) . ?
C015 C018 1.453(10) . ?
C015 H015 0.9300 . ?
C017 C019 1.411(9) . ?
C018 C028 1.379(10) . ?
C019 C024 1.415(10) . ?
C019 H019 0.9300 . ?
C020 C023 1.355(10) . ?
C021 C025 1.374(10) . ?
C021 H021 0.9300 . ?
C023 C030 1.392(10) . ?
C023 H023 0.9300 . ?
C024 C028 1.387(10) . ?
C025 H025 0.9300 . ?
C026 C029 1.313(11) . ?
C026 H026 0.9300 . ?
C027 C031 1.368(11) . ?
C027 C030 1.402(11) . ?
C027 H027 0.9300 . ?
C028 H028 0.9300 . ?
C029 H029 0.9300 . ?
N032 C038 1.07(3) . ?
C034 H03A 0.9600 . ?
C034 H03B 0.9600 . ?
C034 H03C 0.9600 . ?
C035 H03D 0.9600 . ?
C035 H03E 0.9600 . ?
C035 H03F 0.9600 . ?
C036 H03G 0.9600 . ?
C036 H03H 0.9600 . ?
C036 H03I 0.9600 . ?
C037 H03J 0.9600 . ?
C037 H03K 0.9600 . ?
C037 H03L 0.9600 . ?
C038 C040 1.27(5) . ?
C040 O65 0.82(5) . ?
N7 C802 0.45(7) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N7 V001 O016 180.000(1) . . ?
N7 V001 C802 0.000(2) . . ?
O016 V001 C802 180.000(5) . . ?
N7 V001 N102 74.85(14) . 2 ?
O016 V001 N102 105.15(14) . 2 ?
C802 V001 N102 74.85(14) . 2 ?
N7 V001 N102 74.85(14) . . ?
O016 V001 N102 105.15(14) . . ?
C802 V001 N102 74.85(14) . . ?
N102 V001 N102 149.7(3) 2 . ?
N7 V001 N101 76.14(15) . 2 ?
O016 V001 N101 103.86(15) . 2 ?
C802 V001 N101 76.14(15) . 2 ?
N102 V001 N101 86.9(2) 2 2 ?
N102 V001 N101 85.9(2) . 2 ?
N7 V001 N101 76.14(15) . . ?
O016 V001 N101 103.86(15) . . ?
C802 V001 N101 76.14(15) . . ?
N102 V001 N101 85.9(2) 2 . ?
N102 V001 N101 86.9(2) . . ?
N101 V001 N101 152.3(3) 2 . ?
C010 N102 C011 105.5(6) . . ?
C010 N102 V001 126.6(4) . . ?
C011 N102 V001 125.7(4) . . ?
C024 O003 C034 118.1(6) . . ?
C012 N101 C201 106.4(5) . . ?
C012 N101 V001 126.6(4) . . ?
C201 N101 V001 125.0(5) . . ?
C018 O005 C035 118.5(6) . . ?
C031 O006 C036 119.2(6) . . ?
C201 C202 C011 124.3(6) . . ?
C201 C202 C020 118.4(6) . . ?
C011 C202 C020 117.3(6) . . ?
C202 C201 N101 127.2(6) . . ?
C202 C201 C029 124.1(6) . . ?
N101 C201 C029 108.7(6) . . ?
C030 O601 C037 117.4(7) . . ?
N102 C010 C013 125.6(6) . . ?
N102 C010 C025 111.8(6) . . ?
C013 C010 C025 122.6(6) . . ?
N102 C011 C202 125.4(6) . . ?
N102 C011 C021 110.2(6) . . ?
C202 C011 C021 124.4(6) . . ?
N101 C012 C013 124.8(6) . 2 ?
N101 C012 C026 109.3(6) . . ?
C013 C012 C026 125.9(6) 2 . ?
C012 C013 C010 124.6(6) 2 . ?
C012 C013 C017 118.6(6) 2 . ?
C010 C013 C017 116.9(6) . . ?
C020 C014 C031 119.9(6) . . ?
C020 C014 H014 120.0 . . ?
C031 C014 H014 120.0 . . ?
C017 C015 C018 120.7(6) . . ?
C017 C015 H015 119.7 . . ?
C018 C015 H015 119.7 . . ?
C015 C017 C019 122.7(6) . . ?
C015 C017 C013 119.8(6) . . ?
C019 C017 C013 117.4(6) . . ?
O005 C018 C028 126.3(7) . . ?
O005 C018 C015 115.4(6) . . ?
C028 C018 C015 118.4(6) . . ?
C017 C019 C024 116.4(6) . . ?
C017 C019 H019 121.8 . . ?
C024 C019 H019 121.8 . . ?
C023 C020 C014 120.8(7) . . ?
C023 C020 C202 120.7(6) . . ?
C014 C020 C202 118.6(6) . . ?
C025 C021 C011 106.8(6) . . ?
C025 C021 H021 126.6 . . ?
C011 C021 H021 126.6 . . ?
C020 C023 C030 120.3(7) . . ?
C020 C023 H023 119.8 . . ?
C030 C023 H023 119.8 . . ?
O003 C024 C028 115.0(6) . . ?
O003 C024 C019 122.9(7) . . ?
C028 C024 C019 122.1(6) . . ?
C021 C025 C010 105.8(7) . . ?
C021 C025 H025 127.1 . . ?
C010 C025 H025 127.1 . . ?
C029 C026 C012 107.9(7) . . ?
C029 C026 H026 126.1 . . ?
C012 C026 H026 126.1 . . ?
C031 C027 C030 119.5(7) . . ?
C031 C027 H027 120.2 . . ?
C030 C027 H027 120.2 . . ?
C018 C028 C024 119.7(7) . . ?
C018 C028 H028 120.2 . . ?
C024 C028 H028 120.1 . . ?
C026 C029 C201 107.8(7) . . ?
C026 C029 H029 126.1 . . ?
C201 C029 H029 126.1 . . ?
C023 C030 O601 125.6(7) . . ?
C023 C030 C027 119.4(6) . . ?
O601 C030 C027 115.0(6) . . ?
O006 C031 C027 124.2(7) . . ?
O006 C031 C014 115.6(7) . . ?
C027 C031 C014 120.1(7) . . ?
O003 C034 H03A 109.5 . . ?
O003 C034 H03B 109.5 . . ?
H03A C034 H03B 109.5 . . ?
O003 C034 H03C 109.5 . . ?
H03A C034 H03C 109.5 . . ?
H03B C034 H03C 109.5 . . ?
O005 C035 H03D 109.5 . . ?
O005 C035 H03E 109.5 . . ?
H03D C035 H03E 109.5 . . ?
O005 C035 H03F 109.5 . . ?
H03D C035 H03F 109.5 . . ?
H03E C035 H03F 109.5 . . ?
O006 C036 H03G 109.5 . . ?
O006 C036 H03H 109.5 . . ?
H03G C036 H03H 109.5 . . ?
O006 C036 H03I 109.5 . . ?
H03G C036 H03I 109.5 . . ?
H03H C036 H03I 109.5 . . ?
O601 C037 H03J 109.5 . . ?
O601 C037 H03K 109.5 . . ?
H03J C037 H03K 109.5 . . ?
O601 C037 H03L 109.5 . . ?
H03J C037 H03L 109.5 . . ?
H03K C037 H03L 109.5 . . ?
N032 C038 C040 180.000(8) . . ?
O65 C040 C038 180.000(8) . . ?
C802 N7 V001 180.000(7) . . ?
N7 C802 V001 0.000(3) . . ?

_diffrn_measured_fraction_theta_max 0.989
_diffrn_reflns_theta_full        28.38
_diffrn_measured_fraction_theta_full 0.989
_refine_diff_density_max         5.504
_refine_diff_density_min         -2.157
_refine_diff_density_rms         0.326
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: Dichloromethane, Acetonitrile and Methanol'
