# Supplementary Information (SI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2026

####################################################################### 
# 
# 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_LH
_database_code_depnum_ccdc_archive 'CCDC 2524168'
loop_
_audit_author_name
_audit_author_address
'Mark Elsegood'
;Loughborough University
United Kingdom
;
_audit_update_record             
;
2026-01-19 deposited with the CCDC.	2026-03-10 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2019/3
_shelx_SHELXL_version_number     2019/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C19 H21 Br2 N O'
_chemical_formula_sum            'C19 H21 Br2 N O'
_chemical_formula_weight         439.19

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

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   8.27032(10)
_cell_length_b                   11.96735(15)
_cell_length_c                   19.8419(2)
_cell_angle_alpha                103.1633(10)
_cell_angle_beta                 93.0781(9)
_cell_angle_gamma                105.7365(11)
_cell_volume                     1826.54(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    35740
_cell_measurement_theta_min      1.83
_cell_measurement_theta_max      32.56

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.597
_exptl_crystal_F_000             880
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.070
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.050
_exptl_absorpt_coefficient_mu    4.442
_shelx_estimated_absorpt_T_min   0.746
_shelx_estimated_absorpt_T_max   0.808
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.798
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   
; 
CrysAlisPro 1.171.43.121a (Rigaku Oxford Diffraction, 2024) 
Empirical absorption correction using spherical harmonics, 
implemented in SCALE3 ABSPACK scaling algorithm. 
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Rotating Anode'
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  
; 
Rigaku FRE+ equipped with Arc)Sec VHF Varimax confocal mirrors and an UG2 
goniometer and HyPix 6000HE detector 
;
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_radiation_collimation    0.2
_diffrn_detector_area_resol_mean 10
_diffrn_reflns_number            138537
_diffrn_reflns_av_unetI/netI     0.0369
_diffrn_reflns_av_R_equivalents  0.0657
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_theta_min         1.827
_diffrn_reflns_theta_max         33.140
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             13940
_reflns_number_gt                10574
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
; 
 Reflections were merged by SHELXL according to the crystal 
 class for the calculation of statistics and refinement. 
  
 _reflns_Friedel_fraction is defined as the number of unique 
 Friedel pairs measured divided by the number that would be 
 possible theoretically, ignoring centric projections and 
 systematic absences. 
;

_computing_data_collection       
'CrysAlisPro system (CCD 43.121a 64-bit (release 24-04-2024))'
_computing_cell_refinement       'CrysAlisPro 1.171.43.121a (Rigaku OD, 2024)'
_computing_data_reduction        'CrysAlisPro 1.171.43.121a (Rigaku OD, 2024)'
_computing_structure_solution    'SHELXT-2018/2 (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2019/3 (Sheldrick, 2019)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+3.8831P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         13940
_refine_ls_number_parameters     580
_refine_ls_number_restraints     1131
_refine_ls_R_factor_all          0.0753
_refine_ls_R_factor_gt           0.0498
_refine_ls_wR_factor_ref         0.0911
_refine_ls_wR_factor_gt          0.0858
_refine_ls_goodness_of_fit_ref   1.224
_refine_ls_restrained_S_all      1.217
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
O1 O 0.7028(2) 0.15501(17) 0.62042(10) 0.0206(4) Uani 1 1 d D . . . .
H1 H 0.669(4) 0.216(2) 0.6311(17) 0.024(9) Uiso 1 1 d D . . . .
C1 C 0.6962(3) 0.1241(2) 0.55059(13) 0.0176(5) Uani 1 1 d D . . . .
C2 C 0.7465(3) 0.0256(2) 0.51786(14) 0.0188(5) Uani 1 1 d D . . . .
Br1 Br 0.82587(4) -0.06277(2) 0.57304(2) 0.02474(6) Uani 1 1 d D . . . .
C3 C 0.7399(3) -0.0102(2) 0.44618(14) 0.0207(5) Uani 1 1 d D . . . .
H3 H 0.774162 -0.078313 0.425187 0.025 Uiso 1 1 calc R U . . .
C4 C 0.6829(3) 0.0542(2) 0.40529(13) 0.0210(5) Uani 1 1 d D . . . .
Br2 Br 0.67022(4) 0.00615(3) 0.30694(2) 0.03022(7) Uani 1 1 d D . . . .
C5 C 0.6335(3) 0.1539(2) 0.43564(13) 0.0198(5) Uani 1 1 d D . . . .
H5 H 0.595592 0.198122 0.407243 0.024 Uiso 1 1 calc R U . . .
C6 C 0.6394(3) 0.1895(2) 0.50820(13) 0.0171(5) Uani 1 1 d D . . . .
C7 C 0.5872(3) 0.2950(2) 0.53826(14) 0.0187(5) Uani 1 1 d D . . . .
H7 H 0.549919 0.336810 0.508139 0.022 Uiso 1 1 calc R U . . .
N1 N 0.5903(3) 0.33303(19) 0.60404(11) 0.0180(4) Uani 1 1 d D . . . .
C8 C 0.5499(3) 0.4425(2) 0.62917(13) 0.0173(5) Uani 1 1 d D . . . .
C9 C 0.4097(3) 0.4399(2) 0.66667(13) 0.0193(5) Uani 1 1 d D . . . .
C10 C 0.3670(4) 0.5460(2) 0.68912(14) 0.0224(5) Uani 1 1 d D . . . .
H10 H 0.270851 0.545446 0.713339 0.027 Uiso 1 1 calc R U . . .
C11 C 0.4622(4) 0.6524(2) 0.67673(14) 0.0227(5) Uani 1 1 d D . . . .
H11 H 0.429762 0.723653 0.691335 0.027 Uiso 1 1 calc R U . . .
C12 C 0.6049(4) 0.6544(2) 0.64294(14) 0.0223(5) Uani 1 1 d D . . . .
H12 H 0.671431 0.728238 0.635990 0.027 Uiso 1 1 calc R U . . .
C13 C 0.6535(3) 0.5508(2) 0.61883(13) 0.0190(5) Uani 1 1 d D . . . .
C14 C 0.3060(3) 0.3242(2) 0.68216(15) 0.0234(5) Uani 1 1 d D . . . .
H14 H 0.362996 0.260879 0.665703 0.028 Uiso 1 1 calc R U . . .
C15 C 0.2995(4) 0.3404(3) 0.76059(16) 0.0325(7) Uani 1 1 d D . . . .
H15A H 0.415037 0.368260 0.784864 0.049 Uiso 1 1 calc R U . . .
H15B H 0.239615 0.263529 0.769622 0.049 Uiso 1 1 calc R U . . .
H15C H 0.239773 0.399663 0.777545 0.049 Uiso 1 1 calc R U . . .
C16 C 0.1279(4) 0.2819(3) 0.64271(17) 0.0295(6) Uani 1 1 d D . . . .
H16A H 0.063784 0.207355 0.653191 0.044 Uiso 1 1 calc R U . . .
H16B H 0.134922 0.267712 0.592477 0.044 Uiso 1 1 calc R U . . .
H16C H 0.070509 0.343635 0.657153 0.044 Uiso 1 1 calc R U . . .
C17 C 0.8185(3) 0.5593(2) 0.58697(14) 0.0223(5) Uani 1 1 d D . . . .
H17 H 0.841046 0.479883 0.580997 0.027 Uiso 1 1 calc R U . . .
C18 C 0.9677(4) 0.6543(3) 0.63597(17) 0.0342(7) Uani 1 1 d D . . . .
H18A H 1.073539 0.652813 0.616339 0.051 Uiso 1 1 calc R U . . .
H18B H 0.972759 0.636689 0.681779 0.051 Uiso 1 1 calc R U . . .
H18C H 0.951785 0.733880 0.640990 0.051 Uiso 1 1 calc R U . . .
C19 C 0.8078(4) 0.5848(3) 0.51507(15) 0.0280(6) Uani 1 1 d D . . . .
H19A H 0.784843 0.662070 0.519230 0.042 Uiso 1 1 calc R U . . .
H19B H 0.716334 0.521077 0.483763 0.042 Uiso 1 1 calc R U . . .
H19C H 0.915410 0.587554 0.496097 0.042 Uiso 1 1 calc R U . . .
O2 O 0.7360(6) 0.6457(4) 0.7972(2) 0.0318(10) Uani 0.5234(17) 1 d D . P A 1
H2 H 0.690918 0.701432 0.800429 0.048 Uiso 0.5234(17) 1 calc R U P A 1
C20 C 0.7358(7) 0.6128(5) 0.8575(3) 0.0192(8) Uani 0.5234(17) 1 d D U P A 1
C21 C 0.7832(9) 0.5087(6) 0.8600(3) 0.0196(9) Uani 0.5234(17) 1 d D U P A 1
Br3 Br 0.8405(2) 0.41967(13) 0.77874(8) 0.0325(2) Uani 0.5234(17) 1 d D U P A 1
C22 C 0.7890(12) 0.4722(7) 0.9210(3) 0.0183(10) Uani 0.5234(17) 1 d D U P A 1
H22 H 0.822395 0.402685 0.922196 0.022 Uiso 0.5234(17) 1 calc R U P A 1
C23 C 0.7454(7) 0.5382(5) 0.9809(3) 0.0187(8) Uani 0.5234(17) 1 d D U P A 1
Br4 Br 0.75424(8) 0.48845(7) 1.06472(3) 0.02781(19) Uani 0.5234(17) 1 d D U P A
1
C24 C 0.6978(6) 0.6400(4) 0.9799(3) 0.0187(8) Uani 0.5234(17) 1 d D U P A 1
H24 H 0.668927 0.684546 1.021156 0.022 Uiso 0.5234(17) 1 calc R U P A 1
C25 C 0.6921(6) 0.6775(4) 0.9185(3) 0.0166(7) Uani 0.5234(17) 1 d D U P A 1
C26 C 0.6410(6) 0.7853(4) 0.9189(3) 0.0187(7) Uani 0.5234(17) 1 d D U P A 1
H26 H 0.614673 0.828041 0.961338 0.022 Uiso 0.5234(17) 1 calc R U P A 1
N2 N 0.6303(6) 0.8246(4) 0.8647(3) 0.0225(8) Uani 0.5234(17) 1 d D U P A 1
C27 C 0.5654(8) 0.9421(6) 0.8886(3) 0.0251(9) Uani 0.5234(17) 1 d D U P A 1
C28 C 0.4002(8) 0.9431(6) 0.9026(3) 0.0287(10) Uani 0.5234(17) 1 d D U P A 1
C29 C 0.3433(4) 1.0317(3) 0.88729(17) 0.0328(6) Uani 1 1 d D U . . .
H29 H 0.227025 1.026689 0.888911 0.039 Uiso 0.5234(17) 1 calc R U P A 1
H29X H 0.237855 1.034871 0.903106 0.039 Uiso 0.4766(17) 1 calc R U P A 2
C30 C 0.4485(4) 1.1289(3) 0.86940(15) 0.0285(6) Uani 1 1 d D U . . .
H30 H 0.410091 1.196160 0.867288 0.034 Uiso 1 1 calc R U . . .
C31 C 0.6097(4) 1.1283(2) 0.85457(14) 0.0252(5) Uani 1 1 d D U . . .
H31 H 0.679998 1.193989 0.840578 0.030 Uiso 0.5234(17) 1 calc R U P A 1
H31X H 0.679194 1.195173 0.841350 0.030 Uiso 0.4766(17) 1 calc R U P A 2
C32 C 0.6705(15) 1.0318(12) 0.8599(13) 0.0268(10) Uani 0.5234(17) 1 d D U P A 1
C33 C 0.2776(7) 0.8388(5) 0.9220(3) 0.0274(10) Uani 0.5234(17) 1 d D U P A 1
H33 H 0.343149 0.808621 0.953920 0.033 Uiso 0.5234(17) 1 calc R U P A 1
C34 C 0.1317(7) 0.8681(6) 0.9584(4) 0.0324(12) Uani 0.5234(17) 1 d D U P A 1
H34A H 0.059908 0.795638 0.968727 0.049 Uiso 0.5234(17) 1 calc R U P A 1
H34B H 0.176470 0.930115 1.001972 0.049 Uiso 0.5234(17) 1 calc R U P A 1
H34C H 0.064553 0.897281 0.927971 0.049 Uiso 0.5234(17) 1 calc R U P A 1
C35 C 0.2058(8) 0.7360(6) 0.8547(4) 0.0418(14) Uani 0.5234(17) 1 d D U P A 1
H35A H 0.299604 0.716956 0.831061 0.063 Uiso 0.5234(17) 1 calc R U P A 1
H35B H 0.137009 0.664702 0.867090 0.063 Uiso 0.5234(17) 1 calc R U P A 1
H35C H 0.135485 0.761720 0.823485 0.063 Uiso 0.5234(17) 1 calc R U P A 1
C36 C 0.8483(4) 1.0339(3) 0.84164(19) 0.0357(7) Uani 1 1 d D U . . .
H36 H 0.888647 0.980133 0.865972 0.043 Uiso 1 1 calc R U . A 1
C37 C 0.9760(5) 1.1601(4) 0.8660(3) 0.0594(12) Uani 1 1 d D U . . .
H37A H 1.089320 1.155444 0.856366 0.089 Uiso 1 1 calc R U . . .
H37B H 0.976959 1.191368 0.916211 0.089 Uiso 1 1 calc R U . . .
H37C H 0.942986 1.213742 0.840908 0.089 Uiso 1 1 calc R U . . .
C38 C 0.8446(5) 0.9850(4) 0.7642(2) 0.0565(11) Uani 1 1 d D U . . .
H38A H 0.771888 0.901864 0.750019 0.085 Uiso 1 1 calc R U . . .
H38B H 0.959591 0.987626 0.753386 0.085 Uiso 1 1 calc R U . . .
H38C H 0.799834 1.033777 0.738871 0.085 Uiso 1 1 calc R U . . .
O2X O 0.6732(5) 0.7380(4) 0.9998(2) 0.0231(8) Uani 0.4766(17) 1 d D U P A 2
H2X H 0.650223 0.793923 0.986028 0.035 Uiso 0.4766(17) 1 calc R U P A 2
C20X C 0.7045(7) 0.6604(5) 0.9458(3) 0.0170(8) Uani 0.4766(17) 1 d D U P A 2
C21X C 0.7492(8) 0.5605(5) 0.9577(3) 0.0186(8) Uani 0.4766(17) 1 d D U P A 2
Br3X Br 0.75348(9) 0.53705(8) 1.04845(4) 0.0271(2) Uani 0.4766(17) 1 d D U P A
2
C22X C 0.7879(14) 0.4796(8) 0.9040(4) 0.0189(11) Uani 0.4766(17) 1 d D U P A 2
H22X H 0.818528 0.412827 0.912810 0.023 Uiso 0.4766(17) 1 calc R U P A 2
C23X C 0.7817(10) 0.4967(6) 0.8374(3) 0.0192(10) Uani 0.4766(17) 1 d D U P A 2
Br4X Br 0.8416(2) 0.38832(13) 0.76441(8) 0.0263(2) Uani 0.4766(17) 1 d D U P A
2
C24X C 0.7333(7) 0.5913(5) 0.8235(3) 0.0189(9) Uani 0.4766(17) 1 d D U P A 2
H24X H 0.725047 0.600012 0.777175 0.023 Uiso 0.4766(17) 1 calc R U P A 2
C25X C 0.6966(6) 0.6741(5) 0.8773(3) 0.0160(7) Uani 0.4766(17) 1 d D U P A 2
C26X C 0.6458(7) 0.7751(5) 0.8615(3) 0.0180(8) Uani 0.4766(17) 1 d D U P A 2
H26X H 0.634897 0.780355 0.814480 0.022 Uiso 0.4766(17) 1 calc R U P A 2
N2X N 0.6164(6) 0.8547(4) 0.9089(3) 0.0196(8) Uani 0.4766(17) 1 d D U P A 2
C27X C 0.5628(9) 0.9301(6) 0.8681(4) 0.0254(10) Uani 0.4766(17) 1 d D U P A 2
C28X C 0.3972(9) 0.9250(6) 0.8814(4) 0.0296(11) Uani 0.4766(17) 1 d D U P A 2
C32X C 0.6736(16) 1.0343(13) 0.8582(14) 0.0264(11) Uani 0.4766(17) 1 d D U P A
2
C33X C 0.2751(8) 0.8033(7) 0.8846(4) 0.0327(11) Uani 0.4766(17) 1 d D U P A 2
H33X H 0.341999 0.745506 0.886063 0.039 Uiso 0.4766(17) 1 calc R U P A 2
C34X C 0.1863(12) 0.8163(8) 0.9477(4) 0.0528(19) Uani 0.4766(17) 1 d D U P A 2
H34D H 0.269747 0.847182 0.989458 0.079 Uiso 0.4766(17) 1 calc R U P A 2
H34E H 0.119735 0.872456 0.946605 0.079 Uiso 0.4766(17) 1 calc R U P A 2
H34F H 0.110865 0.738037 0.948668 0.079 Uiso 0.4766(17) 1 calc R U P A 2
C35X C 0.1486(10) 0.7552(7) 0.8181(4) 0.0472(18) Uani 0.4766(17) 1 d D U P A 2
H35D H 0.210078 0.747348 0.777272 0.071 Uiso 0.4766(17) 1 calc R U P A 2
H35E H 0.072968 0.676527 0.818351 0.071 Uiso 0.4766(17) 1 calc R U P A 2
H35F H 0.081838 0.810946 0.816287 0.071 Uiso 0.4766(17) 1 calc R U 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
O1 C1 1.344(3) . ?
O1 H1 0.837(18) . ?
C1 C2 1.390(4) . ?
C1 C6 1.413(3) . ?
C2 C3 1.382(4) . ?
C2 Br1 1.891(3) . ?
C3 C4 1.384(4) . ?
C3 H3 0.9500 . ?
C4 C5 1.384(4) . ?
C4 Br2 1.893(3) . ?
C5 C6 1.399(3) . ?
C5 H5 0.9500 . ?
C6 C7 1.455(3) . ?
C7 N1 1.277(3) . ?
C7 H7 0.9500 . ?
N1 C8 1.427(3) . ?
C8 C9 1.408(3) . ?
C8 C13 1.412(3) . ?
C9 C10 1.392(4) . ?
C9 C14 1.526(3) . ?
C10 C11 1.386(4) . ?
C10 H10 0.9500 . ?
C11 C12 1.386(4) . ?
C11 H11 0.9500 . ?
C12 C13 1.396(4) . ?
C12 H12 0.9500 . ?
C13 C17 1.523(4) . ?
C14 C16 1.527(4) . ?
C14 C15 1.529(4) . ?
C14 H14 1.0000 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 C19 1.528(4) . ?
C17 C18 1.539(4) . ?
C17 H17 1.0000 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
O2 C20 1.342(6) . ?
O2 H2 0.8400 . ?
C20 C25 1.403(7) . ?
C20 C21 1.415(8) . ?
C21 C22 1.380(7) . ?
C21 Br3 1.879(6) . ?
C22 C23 1.392(8) . ?
C22 H22 0.9500 . ?
C23 C24 1.382(7) . ?
C23 Br4 1.894(5) . ?
C24 C25 1.394(6) . ?
C24 H24 0.9500 . ?
C25 C26 1.462(6) . ?
C26 N2 1.274(6) . ?
C26 H26 0.9500 . ?
N2 C27 1.620(8) . ?
C27 C28 1.412(8) . ?
C27 C32 1.434(9) . ?
C28 C29 1.356(7) . ?
C28 C33 1.519(7) . ?
C29 C30 1.382(4) . ?
C29 C28X 1.445(8) . ?
C29 H29 0.9500 . ?
C29 H29X 0.9500 . ?
C30 C31 1.382(4) . ?
C30 H30 0.9500 . ?
C31 C32X 1.380(9) . ?
C31 C32 1.401(8) . ?
C31 H31 0.9500 . ?
C31 H31X 0.9500 . ?
C32 C36 1.529(8) . ?
C33 C34 1.519(8) . ?
C33 C35 1.555(9) . ?
C33 H33 1.0000 . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
C36 C32X 1.500(8) . ?
C36 C38 1.510(5) . ?
C36 C37 1.542(5) . ?
C36 H36 1.0000 . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?
O2X C20X 1.336(6) . ?
O2X H2X 0.8400 . ?
C20X C25X 1.404(7) . ?
C20X C21X 1.408(7) . ?
C21X C22X 1.381(9) . ?
C21X Br3X 1.885(6) . ?
C22X C23X 1.383(8) . ?
C22X H22X 0.9500 . ?
C23X C24X 1.376(8) . ?
C23X Br4X 1.896(6) . ?
C24X C25X 1.389(7) . ?
C24X H24X 0.9500 . ?
C25X C26X 1.473(7) . ?
C26X N2X 1.263(7) . ?
C26X H26X 0.9500 . ?
N2X C27X 1.474(7) . ?
C27X C32X 1.395(10) . ?
C27X C28X 1.396(9) . ?
C28X C33X 1.548(8) . ?
C33X C34X 1.485(10) . ?
C33X C35X 1.530(9) . ?
C33X H33X 1.0000 . ?
C34X H34D 0.9800 . ?
C34X H34E 0.9800 . ?
C34X H34F 0.9800 . ?
C35X H35D 0.9800 . ?
C35X H35E 0.9800 . ?
C35X H35F 0.9800 . ?

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
C1 O1 H1 107(2) . . ?
O1 C1 C2 120.2(2) . . ?
O1 C1 C6 121.9(2) . . ?
C2 C1 C6 117.8(2) . . ?
C3 C2 C1 122.1(2) . . ?
C3 C2 Br1 118.89(19) . . ?
C1 C2 Br1 119.00(19) . . ?
C2 C3 C4 119.4(2) . . ?
C2 C3 H3 120.3 . . ?
C4 C3 H3 120.3 . . ?
C3 C4 C5 120.5(2) . . ?
C3 C4 Br2 120.3(2) . . ?
C5 C4 Br2 119.2(2) . . ?
C4 C5 C6 119.9(2) . . ?
C4 C5 H5 120.0 . . ?
C6 C5 H5 120.0 . . ?
C5 C6 C1 120.2(2) . . ?
C5 C6 C7 118.4(2) . . ?
C1 C6 C7 121.4(2) . . ?
N1 C7 C6 121.8(2) . . ?
N1 C7 H7 119.1 . . ?
C6 C7 H7 119.1 . . ?
C7 N1 C8 117.9(2) . . ?
C9 C8 C13 121.5(2) . . ?
C9 C8 N1 118.3(2) . . ?
C13 C8 N1 120.1(2) . . ?
C10 C9 C8 118.3(2) . . ?
C10 C9 C14 120.5(2) . . ?
C8 C9 C14 121.2(2) . . ?
C11 C10 C9 121.1(2) . . ?
C11 C10 H10 119.4 . . ?
C9 C10 H10 119.4 . . ?
C12 C11 C10 119.7(2) . . ?
C12 C11 H11 120.2 . . ?
C10 C11 H11 120.2 . . ?
C11 C12 C13 121.8(2) . . ?
C11 C12 H12 119.1 . . ?
C13 C12 H12 119.1 . . ?
C12 C13 C8 117.4(2) . . ?
C12 C13 C17 119.7(2) . . ?
C8 C13 C17 122.8(2) . . ?
C9 C14 C16 110.8(2) . . ?
C9 C14 C15 110.9(2) . . ?
C16 C14 C15 110.9(2) . . ?
C9 C14 H14 108.0 . . ?
C16 C14 H14 108.0 . . ?
C15 C14 H14 108.0 . . ?
C14 C15 H15A 109.5 . . ?
C14 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C14 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C14 C16 H16A 109.5 . . ?
C14 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C14 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C13 C17 C19 112.2(2) . . ?
C13 C17 C18 111.1(2) . . ?
C19 C17 C18 110.5(2) . . ?
C13 C17 H17 107.6 . . ?
C19 C17 H17 107.6 . . ?
C18 C17 H17 107.6 . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C17 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C17 C19 H19A 109.5 . . ?
C17 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C17 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C20 O2 H2 109.5 . . ?
O2 C20 C25 123.1(5) . . ?
O2 C20 C21 118.6(5) . . ?
C25 C20 C21 118.3(5) . . ?
C22 C21 C20 121.1(6) . . ?
C22 C21 Br3 119.8(5) . . ?
C20 C21 Br3 119.1(4) . . ?
C21 C22 C23 119.5(6) . . ?
C21 C22 H22 120.3 . . ?
C23 C22 H22 120.3 . . ?
C24 C23 C22 120.7(5) . . ?
C24 C23 Br4 119.9(4) . . ?
C22 C23 Br4 119.4(4) . . ?
C23 C24 C25 120.1(5) . . ?
C23 C24 H24 119.9 . . ?
C25 C24 H24 119.9 . . ?
C24 C25 C20 120.3(5) . . ?
C24 C25 C26 119.0(5) . . ?
C20 C25 C26 120.7(5) . . ?
N2 C26 C25 122.9(5) . . ?
N2 C26 H26 118.6 . . ?
C25 C26 H26 118.6 . . ?
C26 N2 C27 105.9(5) . . ?
C28 C27 C32 121.5(6) . . ?
C28 C27 N2 126.4(5) . . ?
C32 C27 N2 105.7(6) . . ?
C29 C28 C27 117.5(5) . . ?
C29 C28 C33 119.6(5) . . ?
C27 C28 C33 122.1(6) . . ?
C28 C29 C30 122.3(4) . . ?
C30 C29 C28X 118.5(4) . . ?
C28 C29 H29 118.8 . . ?
C30 C29 H29 118.8 . . ?
C30 C29 H29X 120.7 . . ?
C28X C29 H29X 120.7 . . ?
C31 C30 C29 119.9(3) . . ?
C31 C30 H30 120.0 . . ?
C29 C30 H30 120.0 . . ?
C32X C31 C30 122.6(4) . . ?
C30 C31 C32 120.7(4) . . ?
C30 C31 H31 119.6 . . ?
C32 C31 H31 119.6 . . ?
C32X C31 H31X 118.7 . . ?
C30 C31 H31X 118.7 . . ?
C31 C32 C27 116.7(6) . . ?
C31 C32 C36 118.9(6) . . ?
C27 C32 C36 124.2(7) . . ?
C34 C33 C28 115.4(5) . . ?
C34 C33 C35 109.3(5) . . ?
C28 C33 C35 108.6(5) . . ?
C34 C33 H33 107.8 . . ?
C28 C33 H33 107.8 . . ?
C35 C33 H33 107.8 . . ?
C33 C34 H34A 109.5 . . ?
C33 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
C33 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C33 C35 H35A 109.5 . . ?
C33 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
C33 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C32X C36 C38 109.8(11) . . ?
C38 C36 C32 110.6(10) . . ?
C32X C36 C37 112.0(7) . . ?
C38 C36 C37 110.0(3) . . ?
C32 C36 C37 112.8(7) . . ?
C38 C36 H36 107.7 . . ?
C32 C36 H36 107.7 . . ?
C37 C36 H36 107.7 . . ?
C36 C37 H37A 109.5 . . ?
C36 C37 H37B 109.5 . . ?
H37A C37 H37B 109.5 . . ?
C36 C37 H37C 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
C36 C38 H38A 109.5 . . ?
C36 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
C36 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
C20X O2X H2X 109.5 . . ?
O2X C20X C25X 123.2(5) . . ?
O2X C20X C21X 118.8(5) . . ?
C25X C20X C21X 118.0(5) . . ?
C22X C21X C20X 121.1(6) . . ?
C22X C21X Br3X 120.0(5) . . ?
C20X C21X Br3X 118.9(4) . . ?
C21X C22X C23X 119.5(6) . . ?
C21X C22X H22X 120.3 . . ?
C23X C22X H22X 120.3 . . ?
C24X C23X C22X 120.9(6) . . ?
C24X C23X Br4X 119.7(5) . . ?
C22X C23X Br4X 119.4(5) . . ?
C23X C24X C25X 120.0(6) . . ?
C23X C24X H24X 120.0 . . ?
C25X C24X H24X 120.0 . . ?
C24X C25X C20X 120.4(5) . . ?
C24X C25X C26X 119.2(5) . . ?
C20X C25X C26X 120.4(5) . . ?
N2X C26X C25X 121.6(5) . . ?
N2X C26X H26X 119.2 . . ?
C25X C26X H26X 119.2 . . ?
C26X N2X C27X 101.6(5) . . ?
C32X C27X C28X 121.2(7) . . ?
C32X C27X N2X 122.7(9) . . ?
C28X C27X N2X 105.5(5) . . ?
C27X C28X C29 118.8(5) . . ?
C27X C28X C33X 118.7(6) . . ?
C29 C28X C33X 122.4(6) . . ?
C31 C32X C27X 117.9(7) . . ?
C31 C32X C36 122.3(6) . . ?
C27X C32X C36 119.2(7) . . ?
C34X C33X C35X 111.0(6) . . ?
C34X C33X C28X 111.1(7) . . ?
C35X C33X C28X 108.3(6) . . ?
C34X C33X H33X 108.8 . . ?
C35X C33X H33X 108.8 . . ?
C28X C33X H33X 108.8 . . ?
C33X C34X H34D 109.5 . . ?
C33X C34X H34E 109.5 . . ?
H34D C34X H34E 109.5 . . ?
C33X C34X H34F 109.5 . . ?
H34D C34X H34F 109.5 . . ?
H34E C34X H34F 109.5 . . ?
C33X C35X H35D 109.5 . . ?
C33X C35X H35E 109.5 . . ?
H35D C35X H35E 109.5 . . ?
C33X C35X H35F 109.5 . . ?
H35D C35X H35F 109.5 . . ?
H35E C35X H35F 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
O1 C1 C2 C3 179.2(2) . . . . ?
C6 C1 C2 C3 -1.0(4) . . . . ?
O1 C1 C2 Br1 -0.6(3) . . . . ?
C6 C1 C2 Br1 179.23(18) . . . . ?
C1 C2 C3 C4 0.6(4) . . . . ?
Br1 C2 C3 C4 -179.65(19) . . . . ?
C2 C3 C4 C5 0.3(4) . . . . ?
C2 C3 C4 Br2 -179.31(19) . . . . ?
C3 C4 C5 C6 -0.6(4) . . . . ?
Br2 C4 C5 C6 178.94(19) . . . . ?
C4 C5 C6 C1 0.2(4) . . . . ?
C4 C5 C6 C7 179.7(2) . . . . ?
O1 C1 C6 C5 -179.6(2) . . . . ?
C2 C1 C6 C5 0.6(4) . . . . ?
O1 C1 C6 C7 0.9(4) . . . . ?
C2 C1 C6 C7 -178.9(2) . . . . ?
C5 C6 C7 N1 -179.6(2) . . . . ?
C1 C6 C7 N1 -0.1(4) . . . . ?
C6 C7 N1 C8 175.1(2) . . . . ?
C7 N1 C8 C9 119.3(3) . . . . ?
C7 N1 C8 C13 -63.4(3) . . . . ?
C13 C8 C9 C10 4.9(4) . . . . ?
N1 C8 C9 C10 -177.8(2) . . . . ?
C13 C8 C9 C14 -175.5(2) . . . . ?
N1 C8 C9 C14 1.8(4) . . . . ?
C8 C9 C10 C11 -1.8(4) . . . . ?
C14 C9 C10 C11 178.6(3) . . . . ?
C9 C10 C11 C12 -1.6(4) . . . . ?
C10 C11 C12 C13 2.0(4) . . . . ?
C11 C12 C13 C8 1.0(4) . . . . ?
C11 C12 C13 C17 -175.4(3) . . . . ?
C9 C8 C13 C12 -4.4(4) . . . . ?
N1 C8 C13 C12 178.3(2) . . . . ?
C9 C8 C13 C17 171.8(2) . . . . ?
N1 C8 C13 C17 -5.5(4) . . . . ?
C10 C9 C14 C16 66.9(3) . . . . ?
C8 C9 C14 C16 -112.7(3) . . . . ?
C10 C9 C14 C15 -56.7(3) . . . . ?
C8 C9 C14 C15 123.7(3) . . . . ?
C12 C13 C17 C19 -71.8(3) . . . . ?
C8 C13 C17 C19 112.1(3) . . . . ?
C12 C13 C17 C18 52.4(3) . . . . ?
C8 C13 C17 C18 -123.7(3) . . . . ?
O2 C20 C21 C22 178.5(6) . . . . ?
C25 C20 C21 C22 -0.9(9) . . . . ?
O2 C20 C21 Br3 -1.0(8) . . . . ?
C25 C20 C21 Br3 179.5(4) . . . . ?
C20 C21 C22 C23 0.8(11) . . . . ?
Br3 C21 C22 C23 -179.6(6) . . . . ?
C21 C22 C23 C24 -0.5(11) . . . . ?
C21 C22 C23 Br4 -179.7(6) . . . . ?
C22 C23 C24 C25 0.3(9) . . . . ?
Br4 C23 C24 C25 179.6(4) . . . . ?
C23 C24 C25 C20 -0.5(8) . . . . ?
C23 C24 C25 C26 179.9(5) . . . . ?
O2 C20 C25 C24 -178.7(5) . . . . ?
C21 C20 C25 C24 0.8(8) . . . . ?
O2 C20 C25 C26 0.9(8) . . . . ?
C21 C20 C25 C26 -179.6(5) . . . . ?
C24 C25 C26 N2 -179.0(5) . . . . ?
C20 C25 C26 N2 1.4(8) . . . . ?
C25 C26 N2 C27 178.5(5) . . . . ?
C26 N2 C27 C28 -73.5(7) . . . . ?
C26 N2 C27 C32 134.6(11) . . . . ?
C32 C27 C28 C29 0.7(14) . . . . ?
N2 C27 C28 C29 -147.1(5) . . . . ?
C32 C27 C28 C33 170.1(13) . . . . ?
N2 C27 C28 C33 22.3(9) . . . . ?
C27 C28 C29 C30 -10.4(8) . . . . ?
C33 C28 C29 C30 179.9(5) . . . . ?
C28 C29 C30 C31 11.5(6) . . . . ?
C28X C29 C30 C31 -7.8(5) . . . . ?
C29 C30 C31 C32X -1.4(14) . . . . ?
C29 C30 C31 C32 -2.4(13) . . . . ?
C30 C31 C32 C27 -7(2) . . . . ?
C30 C31 C32 C36 178.8(11) . . . . ?
C28 C27 C32 C31 8(2) . . . . ?
N2 C27 C32 C31 161.2(14) . . . . ?
C28 C27 C32 C36 -178.2(13) . . . . ?
N2 C27 C32 C36 -25(2) . . . . ?
C29 C28 C33 C34 -30.5(8) . . . . ?
C27 C28 C33 C34 160.3(6) . . . . ?
C29 C28 C33 C35 92.6(7) . . . . ?
C27 C28 C33 C35 -76.6(7) . . . . ?
C31 C32 C36 C38 -85.3(18) . . . . ?
C27 C32 C36 C38 100.6(19) . . . . ?
C31 C32 C36 C37 38(2) . . . . ?
C27 C32 C36 C37 -135.7(16) . . . . ?
O2X C20X C21X C22X -178.0(7) . . . . ?
C25X C20X C21X C22X 1.4(9) . . . . ?
O2X C20X C21X Br3X 2.7(8) . . . . ?
C25X C20X C21X Br3X -177.9(4) . . . . ?
C20X C21X C22X C23X -0.3(12) . . . . ?
Br3X C21X C22X C23X 178.9(6) . . . . ?
C21X C22X C23X C24X -1.7(12) . . . . ?
C21X C22X C23X Br4X 178.1(7) . . . . ?
C22X C23X C24X C25X 2.6(10) . . . . ?
Br4X C23X C24X C25X -177.1(5) . . . . ?
C23X C24X C25X C20X -1.6(9) . . . . ?
C23X C24X C25X C26X 179.7(6) . . . . ?
O2X C20X C25X C24X 178.9(5) . . . . ?
C21X C20X C25X C24X -0.4(8) . . . . ?
O2X C20X C25X C26X -2.4(8) . . . . ?
C21X C20X C25X C26X 178.3(5) . . . . ?
C24X C25X C26X N2X -177.7(5) . . . . ?
C20X C25X C26X N2X 3.6(8) . . . . ?
C25X C26X N2X C27X -177.1(5) . . . . ?
C26X N2X C27X C32X -96.4(12) . . . . ?
C26X N2X C27X C28X 119.0(6) . . . . ?
C32X C27X C28X C29 -2.2(16) . . . . ?
N2X C27X C28X C29 143.1(6) . . . . ?
C32X C27X C28X C33X 173.9(14) . . . . ?
N2X C27X C28X C33X -40.8(8) . . . . ?
C30 C29 C28X C27X 9.5(8) . . . . ?
C30 C29 C28X C33X -166.5(5) . . . . ?
C30 C31 C32X C27X 9(3) . . . . ?
C30 C31 C32X C36 179.6(13) . . . . ?
C28X C27X C32X C31 -7(3) . . . . ?
N2X C27X C32X C31 -146.0(14) . . . . ?
C28X C27X C32X C36 -177.9(13) . . . . ?
N2X C27X C32X C36 43(2) . . . . ?
C38 C36 C32X C31 -86(2) . . . . ?
C37 C36 C32X C31 36(2) . . . . ?
C38 C36 C32X C27X 84.7(19) . . . . ?
C37 C36 C32X C27X -152.8(16) . . . . ?
C27X C28X C33X C34X 131.5(8) . . . . ?
C29 C28X C33X C34X -52.6(9) . . . . ?
C27X C28X C33X C35X -106.4(8) . . . . ?
C29 C28X C33X C35X 69.6(9) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
O1 H1 N1 0.837(18) 1.86(2) 2.621(3) 150(3) . yes
O1 H1 Br4X 0.837(18) 2.97(3) 3.399(2) 115(3) . yes
O2 H2 N2 0.84 1.91 2.642(7) 144.2 . yes
O2X H2X N2X 0.84 1.88 2.615(6) 145.9 . yes

_refine_diff_density_max         0.578
_refine_diff_density_min         -0.664
_refine_diff_density_rms         0.096

_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: acetonitrile'
####################################################################### 
# 
# 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_7
_database_code_depnum_ccdc_archive 'CCDC 2524172'
loop_
_audit_author_name
_audit_author_address
'Mark Elsegood'
;Loughborough University
United Kingdom
;
_audit_update_record             
;
2026-01-19 deposited with the CCDC.	2026-03-10 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2019/3
_shelx_SHELXL_version_number     2019/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C30 H24 Br4 N2 O3 V'
_chemical_formula_sum            'C30 H24 Br4 N2 O3 V'
_chemical_formula_weight         831.09

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
V V 0.0687 2.1097 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.6763 1.2805 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_H-M_alt        'P n a 21'
_space_group_name_Hall           'P 2c -2n'

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

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

_cell_length_a                   18.00871(7)
_cell_length_b                   21.83197(9)
_cell_length_c                   15.26656(7)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     6002.29(4)
_cell_formula_units_Z            8
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    78353
_cell_measurement_theta_min      3.54
_cell_measurement_theta_max      73.44

_exptl_crystal_description       prism
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.839
_exptl_crystal_F_000             3240
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.122
_exptl_crystal_size_mid          0.108
_exptl_crystal_size_min          0.032
_exptl_absorpt_coefficient_mu    9.286
_shelx_estimated_absorpt_T_min   0.397
_shelx_estimated_absorpt_T_max   0.755
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_correction_T_min  0.408
_exptl_absorpt_correction_T_max  0.756
_exptl_absorpt_process_details   
; 
CrysAlisPro 1.171.43.98a (Rigaku Oxford Diffraction, 2023) 
Analytical numeric absorption correction using a multifaceted crystal 
model based on expressions derived by R.C. Clark & J.S. Reid. 
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) 
Empirical absorption correction using spherical harmonics, 
implemented in SCALE3 ABSPACK scaling algorithm. 
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_source                   'Rotating anode'
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  
; 
Rigaku 007HF diffractometer with HF Varimax confocal mirrors, 
an UG2 goniometer and HyPix 6000HE detector 
;
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_radiation_collimation    0.3
_diffrn_reflns_number            102257
_diffrn_reflns_av_unetI/netI     0.0190
_diffrn_reflns_av_R_equivalents  0.0333
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         3.181
_diffrn_reflns_theta_max         73.725
_diffrn_reflns_theta_full        67.679
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.966
_diffrn_reflns_point_group_measured_fraction_full 0.992
_reflns_number_total             11716
_reflns_number_gt                11493
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.881
_reflns_Friedel_fraction_max     0.942
_reflns_Friedel_fraction_full    0.982

_reflns_special_details          
; 
 Reflections were merged by SHELXL according to the crystal 
 class for the calculation of statistics and refinement. 
  
 _reflns_Friedel_fraction is defined as the number of unique 
 Friedel pairs measured divided by the number that would be 
 possible theoretically, ignoring centric projections and 
 systematic absences. 
;

_computing_data_collection       
'CrysAlisPro system (CCD 43.104a 64-bit (release 22-12-2023))'
_computing_cell_refinement       'CrysAlisPro 1.171.43.98a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.43.98a (Rigaku OD, 2023)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2019/3 (Sheldrick, 2019)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0261P)²+5.3441P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
; 
 Flack x determined using 5220 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). 
;
_refine_ls_abs_structure_Flack   0.001(2)
_chemical_absolute_configuration ad
_refine_ls_number_reflns         11716
_refine_ls_number_parameters     767
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0228
_refine_ls_R_factor_gt           0.0222
_refine_ls_wR_factor_ref         0.0546
_refine_ls_wR_factor_gt          0.0542
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_restrained_S_all      1.029
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
V1 V 0.42134(4) 0.76346(3) 0.27000(6) 0.0191(3) Uani 0.874(3) 1 d . . P A 1
O5 O 0.46234(19) 0.77712(15) 0.3593(2) 0.0287(7) Uani 0.874(3) 1 d . . P A 1
V1X V 0.3938(3) 0.7561(2) 0.2094(4) 0.0190(18) Uani 0.126(3) 1 d . . P A 2
O5X O 0.3554(12) 0.7451(10) 0.1184(16) 0.028(6) Uani 0.126(3) 1 d . . P A 2
N1 N 0.41620(18) 0.66571(15) 0.2716(3) 0.0238(7) Uani 1 1 d . . . . .
C1 C 0.4672(2) 0.63111(18) 0.2393(3) 0.0209(8) Uani 1 1 d . . . . .
H1 H 0.462342 0.588410 0.249788 0.025 Uiso 1 1 calc R U . . .
C2 C 0.5310(2) 0.65002(18) 0.1890(3) 0.0215(8) Uani 1 1 d . . . . .
C3 C 0.5423(2) 0.71152(18) 0.1644(3) 0.0228(8) Uani 1 1 d . . . . .
C4 C 0.6090(2) 0.7246(2) 0.1191(3) 0.0296(9) Uani 1 1 d . . . . .
C5 C 0.6587(2) 0.67977(19) 0.0949(3) 0.0296(9) Uani 1 1 d . . . . .
H5 H 0.702566 0.690069 0.063646 0.035 Uiso 1 1 calc R U . . .
C6 C 0.6439(2) 0.6193(2) 0.1169(3) 0.0265(9) Uani 1 1 d . . . . .
C7 C 0.5816(2) 0.60410(18) 0.1642(3) 0.0238(8) Uani 1 1 d . . . . .
H7 H 0.572740 0.562671 0.180114 0.029 Uiso 1 1 calc R U . . .
O1 O 0.49441(16) 0.75525(12) 0.1806(2) 0.0268(6) Uani 1 1 d . . . . .
Br1 Br 0.62918(3) 0.80659(2) 0.08986(4) 0.04372(14) Uani 1 1 d . . . . .
Br2 Br 0.71023(2) 0.55713(2) 0.07952(3) 0.03277(11) Uani 1 1 d . . . . .
C8 C 0.3573(2) 0.63268(18) 0.3160(3) 0.0232(8) Uani 1 1 d . . . . .
C9 C 0.3026(2) 0.60433(19) 0.2659(3) 0.0281(9) Uani 1 1 d . . . . .
C10 C 0.2475(3) 0.5712(2) 0.3091(4) 0.0328(10) Uani 1 1 d . . . . .
H10 H 0.210078 0.551060 0.276049 0.039 Uiso 1 1 calc R U . . .
C11 C 0.2465(3) 0.5674(2) 0.3992(4) 0.0342(11) Uani 1 1 d . . . . .
H11 H 0.208402 0.544867 0.427809 0.041 Uiso 1 1 calc R U . . .
C12 C 0.3010(3) 0.5963(2) 0.4479(3) 0.0320(10) Uani 1 1 d . . . . .
H12 H 0.299908 0.593413 0.509964 0.038 Uiso 1 1 calc R U . . .
C13 C 0.3573(2) 0.62934(19) 0.4076(3) 0.0279(9) Uani 1 1 d . . . . .
C14 C 0.3030(3) 0.6094(2) 0.1672(3) 0.0384(11) Uani 1 1 d . . . . .
H14A H 0.307463 0.652521 0.150329 0.058 Uiso 1 1 calc R U . . .
H14B H 0.256695 0.592535 0.143747 0.058 Uiso 1 1 calc R U . . .
H14C H 0.345242 0.586338 0.143636 0.058 Uiso 1 1 calc R U . . .
C15 C 0.4172(3) 0.6582(3) 0.4635(4) 0.0431(12) Uani 1 1 d . . . . .
H15A H 0.462523 0.633517 0.459855 0.065 Uiso 1 1 calc R U . . .
H15B H 0.400387 0.660060 0.524471 0.065 Uiso 1 1 calc R U . . .
H15C H 0.427417 0.699728 0.442290 0.065 Uiso 1 1 calc R U . . .
N2 N 0.40597(18) 0.85472(15) 0.2249(2) 0.0215(7) Uani 1 1 d . . . . .
C16 C 0.3504(2) 0.88793(18) 0.2484(3) 0.0212(8) Uani 1 1 d . . . . .
H16 H 0.353173 0.930361 0.234980 0.025 Uiso 1 1 calc R U . . .
C17 C 0.2841(2) 0.86735(18) 0.2930(3) 0.0209(8) Uani 1 1 d . . . . .
C18 C 0.2682(2) 0.80469(18) 0.3058(3) 0.0208(8) Uani 1 1 d . . . . .
C19 C 0.1979(2) 0.79099(17) 0.3411(3) 0.0245(9) Uani 1 1 d . . . . .
C20 C 0.1483(2) 0.83556(19) 0.3686(3) 0.0256(9) Uani 1 1 d . . . . .
H20 H 0.102181 0.824542 0.394433 0.031 Uiso 1 1 calc R U . . .
C21 C 0.1674(2) 0.89673(18) 0.3574(3) 0.0231(8) Uani 1 1 d . . . . .
C22 C 0.2337(2) 0.91302(18) 0.3186(3) 0.0215(8) Uani 1 1 d . . . . .
H22 H 0.245171 0.954979 0.309185 0.026 Uiso 1 1 calc R U . . .
O2 O 0.31478(15) 0.76103(12) 0.2834(2) 0.0269(6) Uani 1 1 d . . . . .
Br3 Br 0.17119(3) 0.70814(2) 0.35446(4) 0.03895(13) Uani 1 1 d . . . . .
Br4 Br 0.09917(2) 0.95840(2) 0.39278(3) 0.02715(10) Uani 1 1 d . . . . .
C23 C 0.4623(2) 0.88877(17) 0.1778(3) 0.0247(9) Uani 1 1 d . . . . .
C24 C 0.4600(3) 0.8880(2) 0.0865(4) 0.0366(11) Uani 1 1 d . . . . .
C25 C 0.5096(4) 0.9246(3) 0.0413(5) 0.063(2) Uani 1 1 d . . . . .
H25 H 0.508015 0.925390 -0.020850 0.076 Uiso 1 1 calc R U . . .
C26 C 0.5608(4) 0.9596(3) 0.0841(6) 0.068(2) Uani 1 1 d . . . . .
H26 H 0.594693 0.984126 0.051747 0.082 Uiso 1 1 calc R U . . .
C27 C 0.5634(3) 0.9594(2) 0.1739(6) 0.062(2) Uani 1 1 d . . . . .
H27 H 0.599422 0.983907 0.202794 0.075 Uiso 1 1 calc R U . . .
C28 C 0.5137(2) 0.9235(2) 0.2248(4) 0.0373(12) Uani 1 1 d . . . . .
C29 C 0.4046(4) 0.8483(3) 0.0388(4) 0.0545(16) Uani 1 1 d . . . . .
H29A H 0.407706 0.806297 0.061011 0.082 Uiso 1 1 calc R U . . .
H29B H 0.415688 0.848666 -0.024011 0.082 Uiso 1 1 calc R U . . .
H29C H 0.354429 0.864314 0.048555 0.082 Uiso 1 1 calc R U . . .
C30 C 0.5166(3) 0.9237(3) 0.3217(4) 0.0517(15) Uani 1 1 d . . . . .
H30A H 0.472279 0.944162 0.344781 0.078 Uiso 1 1 calc R U . . .
H30B H 0.561071 0.945701 0.341141 0.078 Uiso 1 1 calc R U . . .
H30C H 0.518299 0.881464 0.343195 0.078 Uiso 1 1 calc R U . . .
V2 V 0.40242(4) 0.74526(3) 0.77265(6) 0.0194(3) Uani 0.864(3) 1 d . . P B 1
O6 O 0.36247(19) 0.75705(15) 0.8638(2) 0.0273(8) Uani 0.864(3) 1 d . . P B 1
V2X V 0.4335(3) 0.7397(2) 0.7094(4) 0.0230(17) Uani 0.136(3) 1 d . . P B 2
O6X O 0.4763(11) 0.7260(10) 0.6203(16) 0.029(5) Uani 0.136(3) 1 d . . P B 2
C31 C 0.3549(2) 0.61461(18) 0.7406(3) 0.0225(8) Uani 1 1 d . . . . .
H31 H 0.358919 0.571823 0.750890 0.027 Uiso 1 1 calc R U . . .
C32 C 0.2896(2) 0.63457(18) 0.6947(3) 0.0204(8) Uani 1 1 d . . . . .
C33 C 0.2797(2) 0.69629(18) 0.6679(3) 0.0221(8) Uani 1 1 d . . . . .
C34 C 0.2130(2) 0.70950(19) 0.6226(3) 0.0275(9) Uani 1 1 d . . . . .
C35 C 0.1613(2) 0.66535(19) 0.6033(3) 0.0263(9) Uani 1 1 d . . . . .
H35 H 0.117339 0.675937 0.572476 0.032 Uiso 1 1 calc R U . . .
C36 C 0.1734(2) 0.60533(19) 0.6290(3) 0.0213(8) Uani 1 1 d . . . . .
C37 C 0.2361(2) 0.58980(18) 0.6748(3) 0.0213(8) Uani 1 1 d . . . . .
H37 H 0.243349 0.548668 0.693214 0.026 Uiso 1 1 calc R U . . .
O3 O 0.32913(16) 0.73895(12) 0.6826(2) 0.0262(6) Uani 1 1 d . . . . .
N3 N 0.40880(19) 0.64789(15) 0.7696(3) 0.0249(7) Uani 1 1 d . . . . .
Br5 Br 0.19511(3) 0.79105(2) 0.58882(4) 0.04552(15) Uani 1 1 d . . . . .
Br6 Br 0.10253(2) 0.54404(2) 0.60088(3) 0.02712(10) Uani 1 1 d . . . . .
C38 C 0.4693(2) 0.61198(18) 0.8063(3) 0.0231(8) Uani 1 1 d . . . . .
C39 C 0.4766(2) 0.6062(2) 0.8969(3) 0.0318(10) Uani 1 1 d . . . . .
C40 C 0.5315(3) 0.5662(2) 0.9283(4) 0.0400(12) Uani 1 1 d . . . . .
H40 H 0.537665 0.561126 0.989657 0.048 Uiso 1 1 calc R U . . .
C41 C 0.5767(3) 0.5341(2) 0.8715(4) 0.0428(14) Uani 1 1 d . . . . .
H41 H 0.613163 0.506764 0.893899 0.051 Uiso 1 1 calc R U . . .
C42 C 0.5690(2) 0.5416(2) 0.7832(4) 0.0393(12) Uani 1 1 d . . . . .
H42 H 0.600772 0.519692 0.744633 0.047 Uiso 1 1 calc R U . . .
C43 C 0.5156(2) 0.5805(2) 0.7486(3) 0.0317(10) Uani 1 1 d . . . . .
C44 C 0.4289(3) 0.6411(3) 0.9607(4) 0.0450(12) Uani 1 1 d . . . . .
H44A H 0.437904 0.685101 0.953797 0.068 Uiso 1 1 calc R U . . .
H44B H 0.441397 0.628670 1.020575 0.068 Uiso 1 1 calc R U . . .
H44C H 0.376488 0.632222 0.949161 0.068 Uiso 1 1 calc R U . . .
C45 C 0.5101(3) 0.5900(3) 0.6511(4) 0.0431(12) Uani 1 1 d . . . . .
H45A H 0.465218 0.569952 0.628929 0.065 Uiso 1 1 calc R U . . .
H45B H 0.553864 0.572376 0.622445 0.065 Uiso 1 1 calc R U . . .
H45C H 0.507683 0.634002 0.638392 0.065 Uiso 1 1 calc R U . . .
C46 C 0.4756(2) 0.86988(18) 0.7560(3) 0.0236(8) Uani 1 1 d . . . . .
H46 H 0.473432 0.912642 0.744770 0.028 Uiso 1 1 calc R U . . .
C47 C 0.5412(2) 0.84750(18) 0.7999(3) 0.0220(8) Uani 1 1 d . . . . .
C48 C 0.5561(2) 0.78466(18) 0.8082(3) 0.0229(8) Uani 1 1 d . . . . .
C49 C 0.6265(2) 0.76828(19) 0.8410(3) 0.0281(9) Uani 1 1 d . . . . .
C50 C 0.6767(2) 0.8111(2) 0.8705(3) 0.0289(10) Uani 1 1 d . . . . .
H50 H 0.723397 0.798613 0.893225 0.035 Uiso 1 1 calc R U . . .
C51 C 0.6581(2) 0.87247(19) 0.8666(3) 0.0253(8) Uani 1 1 d . . . . .
C52 C 0.5922(2) 0.89176(19) 0.8302(3) 0.0250(8) Uani 1 1 d . . . . .
H52 H 0.581220 0.934198 0.825667 0.030 Uiso 1 1 calc R U . . .
O4 O 0.50869(15) 0.74177(13) 0.7836(2) 0.0273(6) Uani 1 1 d . . . . .
N4 N 0.41956(19) 0.83758(15) 0.7305(3) 0.0251(7) Uani 1 1 d . . . . .
Br7 Br 0.65116(3) 0.68436(2) 0.84815(5) 0.04293(14) Uani 1 1 d . . . . .
Br8 Br 0.72535(2) 0.93127(2) 0.91320(3) 0.03197(11) Uani 1 1 d . . . . .
C53 C 0.3639(2) 0.87190(17) 0.6826(3) 0.0231(8) Uani 1 1 d . . . . .
C54 C 0.3106(2) 0.90455(19) 0.7301(3) 0.0252(9) Uani 1 1 d . . . . .
C55 C 0.2586(2) 0.9376(2) 0.6818(4) 0.0347(11) Uani 1 1 d . . . . .
H55 H 0.221105 0.959947 0.711714 0.042 Uiso 1 1 calc R U . . .
C56 C 0.2604(3) 0.9387(2) 0.5906(4) 0.0419(12) Uani 1 1 d . . . . .
H56 H 0.224468 0.961560 0.558886 0.050 Uiso 1 1 calc R U . . .
C57 C 0.3140(3) 0.9067(2) 0.5469(4) 0.0398(12) Uani 1 1 d . . . . .
H57 H 0.315073 0.907683 0.484659 0.048 Uiso 1 1 calc R U . . .
C58 C 0.3671(2) 0.87272(19) 0.5920(3) 0.0298(9) Uani 1 1 d . . . . .
C59 C 0.3103(3) 0.9068(2) 0.8277(3) 0.0348(10) Uani 1 1 d . . . . .
H59A H 0.352555 0.931314 0.848035 0.052 Uiso 1 1 calc R U . . .
H59B H 0.314309 0.865182 0.851083 0.052 Uiso 1 1 calc R U . . .
H59C H 0.263966 0.925549 0.848008 0.052 Uiso 1 1 calc R U . . .
C60 C 0.4260(3) 0.8366(3) 0.5446(4) 0.0460(13) Uani 1 1 d . . . . .
H60A H 0.474538 0.855723 0.554329 0.069 Uiso 1 1 calc R U . . .
H60B H 0.414953 0.836124 0.481785 0.069 Uiso 1 1 calc R U . . .
H60C H 0.426774 0.794546 0.566983 0.069 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
V1 O5 1.579(4) . ?
V1 O1 1.905(3) . ?
V1 O2 1.931(3) . ?
V1 N2 2.126(3) . ?
V1 N1 2.136(3) . ?
V1X O5X 1.57(2) . ?
V1X O2 1.820(6) . ?
V1X O1 1.864(6) . ?
V1X N2 2.178(6) . ?
V1X N1 2.226(6) . ?
N1 C1 1.288(5) . ?
N1 C8 1.450(5) . ?
C1 C2 1.442(6) . ?
C1 H1 0.9500 . ?
C2 C7 1.406(5) . ?
C2 C3 1.409(6) . ?
C3 O1 1.310(5) . ?
C3 C4 1.416(6) . ?
C4 C5 1.376(6) . ?
C4 Br1 1.880(4) . ?
C5 C6 1.387(6) . ?
C5 H5 0.9500 . ?
C6 C7 1.375(6) . ?
C6 Br2 1.897(4) . ?
C7 H7 0.9500 . ?
C8 C9 1.393(6) . ?
C8 C13 1.399(7) . ?
C9 C10 1.394(6) . ?
C9 C14 1.510(7) . ?
C10 C11 1.377(8) . ?
C10 H10 0.9500 . ?
C11 C12 1.384(7) . ?
C11 H11 0.9500 . ?
C12 C13 1.388(6) . ?
C12 H12 0.9500 . ?
C13 C15 1.513(7) . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
N2 C16 1.287(5) . ?
N2 C23 1.449(5) . ?
C16 C17 1.446(5) . ?
C16 H16 0.9500 . ?
C17 C22 1.403(5) . ?
C17 C18 1.411(5) . ?
C18 O2 1.315(5) . ?
C18 C19 1.407(5) . ?
C19 C20 1.387(6) . ?
C19 Br3 1.883(4) . ?
C20 C21 1.390(6) . ?
C20 H20 0.9500 . ?
C21 C22 1.379(5) . ?
C21 Br4 1.902(4) . ?
C22 H22 0.9500 . ?
C23 C24 1.395(7) . ?
C23 C28 1.396(6) . ?
C24 C25 1.383(7) . ?
C24 C29 1.507(8) . ?
C25 C26 1.364(11) . ?
C25 H25 0.9500 . ?
C26 C27 1.371(12) . ?
C26 H26 0.9500 . ?
C27 C28 1.421(8) . ?
C27 H27 0.9500 . ?
C28 C30 1.479(9) . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
V2 O6 1.588(4) . ?
V2 O3 1.911(3) . ?
V2 O4 1.923(3) . ?
V2 N3 2.130(3) . ?
V2 N4 2.138(4) . ?
V2X O6X 1.59(2) . ?
V2X O4 1.765(6) . ?
V2X O3 1.924(6) . ?
V2X N4 2.175(6) . ?
V2X N3 2.250(6) . ?
C31 N3 1.290(5) . ?
C31 C32 1.437(5) . ?
C31 H31 0.9500 . ?
C32 C37 1.406(5) . ?
C32 C33 1.420(5) . ?
C33 O3 1.309(5) . ?
C33 C34 1.414(6) . ?
C34 C35 1.372(6) . ?
C34 Br5 1.882(4) . ?
C35 C36 1.385(6) . ?
C35 H35 0.9500 . ?
C36 C37 1.371(5) . ?
C36 Br6 1.898(4) . ?
C37 H37 0.9500 . ?
N3 C38 1.455(5) . ?
C38 C39 1.395(6) . ?
C38 C43 1.395(6) . ?
C39 C40 1.404(7) . ?
C39 C44 1.505(7) . ?
C40 C41 1.380(8) . ?
C40 H40 0.9500 . ?
C41 C42 1.366(8) . ?
C41 H41 0.9500 . ?
C42 C43 1.387(6) . ?
C42 H42 0.9500 . ?
C43 C45 1.506(8) . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 0.9800 . ?
C45 H45A 0.9800 . ?
C45 H45B 0.9800 . ?
C45 H45C 0.9800 . ?
C46 N4 1.291(5) . ?
C46 C47 1.444(6) . ?
C46 H46 0.9500 . ?
C47 C48 1.404(6) . ?
C47 C52 1.411(5) . ?
C48 O4 1.322(5) . ?
C48 C49 1.410(6) . ?
C49 C50 1.375(6) . ?
C49 Br7 1.888(4) . ?
C50 C51 1.383(6) . ?
C50 H50 0.9500 . ?
C51 C52 1.376(6) . ?
C51 Br8 1.903(4) . ?
C52 H52 0.9500 . ?
N4 C53 1.450(5) . ?
C53 C58 1.384(7) . ?
C53 C54 1.398(6) . ?
C54 C55 1.393(6) . ?
C54 C59 1.490(7) . ?
C55 C56 1.393(9) . ?
C55 H55 0.9500 . ?
C56 C57 1.365(8) . ?
C56 H56 0.9500 . ?
C57 C58 1.393(6) . ?
C57 H57 0.9500 . ?
C58 C60 1.507(7) . ?
C59 H59A 0.9800 . ?
C59 H59B 0.9800 . ?
C59 H59C 0.9800 . ?
C60 H60A 0.9800 . ?
C60 H60B 0.9800 . ?
C60 H60C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O5 V1 O1 108.28(16) . . ?
O5 V1 O2 112.25(17) . . ?
O1 V1 O2 139.47(14) . . ?
O5 V1 N2 99.41(16) . . ?
O1 V1 N2 86.90(13) . . ?
O2 V1 N2 86.02(13) . . ?
O5 V1 N1 101.47(16) . . ?
O1 V1 N1 86.81(13) . . ?
O2 V1 N1 85.88(12) . . ?
N2 V1 N1 159.12(15) . . ?
O5X V1X O2 102.3(9) . . ?
O5X V1X O1 102.5(9) . . ?
O2 V1X O1 155.1(4) . . ?
O5X V1X N2 106.9(9) . . ?
O2 V1X N2 87.3(2) . . ?
O1 V1X N2 86.4(2) . . ?
O5X V1X N1 108.8(9) . . ?
O2 V1X N1 86.0(2) . . ?
O1 V1X N1 85.2(2) . . ?
N2 V1X N1 144.3(3) . . ?
C1 N1 C8 114.2(3) . . ?
C1 N1 V1 123.4(3) . . ?
C8 N1 V1 122.3(2) . . ?
C1 N1 V1X 119.0(3) . . ?
C8 N1 V1X 120.5(3) . . ?
N1 C1 C2 127.2(4) . . ?
N1 C1 H1 116.4 . . ?
C2 C1 H1 116.4 . . ?
C7 C2 C3 120.9(4) . . ?
C7 C2 C1 117.1(4) . . ?
C3 C2 C1 122.0(4) . . ?
O1 C3 C2 123.3(4) . . ?
O1 C3 C4 120.2(4) . . ?
C2 C3 C4 116.4(4) . . ?
C5 C4 C3 122.6(4) . . ?
C5 C4 Br1 119.2(3) . . ?
C3 C4 Br1 118.2(3) . . ?
C4 C5 C6 119.1(4) . . ?
C4 C5 H5 120.4 . . ?
C6 C5 H5 120.4 . . ?
C7 C6 C5 120.9(4) . . ?
C7 C6 Br2 119.9(3) . . ?
C5 C6 Br2 119.2(3) . . ?
C6 C7 C2 119.8(4) . . ?
C6 C7 H7 120.1 . . ?
C2 C7 H7 120.1 . . ?
C3 O1 V1X 133.7(3) . . ?
C3 O1 V1 131.2(3) . . ?
C9 C8 C13 121.7(4) . . ?
C9 C8 N1 118.8(4) . . ?
C13 C8 N1 119.6(4) . . ?
C8 C9 C10 118.3(4) . . ?
C8 C9 C14 120.8(4) . . ?
C10 C9 C14 120.9(4) . . ?
C11 C10 C9 120.9(5) . . ?
C11 C10 H10 119.5 . . ?
C9 C10 H10 119.5 . . ?
C10 C11 C12 119.9(4) . . ?
C10 C11 H11 120.0 . . ?
C12 C11 H11 120.0 . . ?
C11 C12 C13 121.1(5) . . ?
C11 C12 H12 119.4 . . ?
C13 C12 H12 119.4 . . ?
C12 C13 C8 118.1(4) . . ?
C12 C13 C15 119.1(5) . . ?
C8 C13 C15 122.7(4) . . ?
C9 C14 H14A 109.5 . . ?
C9 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C9 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C13 C15 H15A 109.5 . . ?
C13 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C13 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C16 N2 C23 113.2(3) . . ?
C16 N2 V1 122.6(3) . . ?
C23 N2 V1 123.4(2) . . ?
C16 N2 V1X 120.6(3) . . ?
C23 N2 V1X 121.6(3) . . ?
N2 C16 C17 126.8(4) . . ?
N2 C16 H16 116.6 . . ?
C17 C16 H16 116.6 . . ?
C22 C17 C18 121.3(4) . . ?
C22 C17 C16 116.4(4) . . ?
C18 C17 C16 122.2(3) . . ?
O2 C18 C19 121.3(3) . . ?
O2 C18 C17 122.5(3) . . ?
C19 C18 C17 116.2(3) . . ?
C20 C19 C18 123.1(4) . . ?
C20 C19 Br3 118.5(3) . . ?
C18 C19 Br3 118.4(3) . . ?
C19 C20 C21 118.5(4) . . ?
C19 C20 H20 120.8 . . ?
C21 C20 H20 120.8 . . ?
C22 C21 C20 121.0(4) . . ?
C22 C21 Br4 119.9(3) . . ?
C20 C21 Br4 119.0(3) . . ?
C21 C22 C17 119.7(4) . . ?
C21 C22 H22 120.1 . . ?
C17 C22 H22 120.1 . . ?
C18 O2 V1X 134.7(3) . . ?
C18 O2 V1 129.9(3) . . ?
C24 C23 C28 122.7(4) . . ?
C24 C23 N2 118.0(4) . . ?
C28 C23 N2 119.2(4) . . ?
C25 C24 C23 118.1(6) . . ?
C25 C24 C29 121.3(6) . . ?
C23 C24 C29 120.6(4) . . ?
C26 C25 C24 121.5(7) . . ?
C26 C25 H25 119.3 . . ?
C24 C25 H25 119.3 . . ?
C25 C26 C27 119.9(5) . . ?
C25 C26 H26 120.0 . . ?
C27 C26 H26 120.0 . . ?
C26 C27 C28 121.9(6) . . ?
C26 C27 H27 119.1 . . ?
C28 C27 H27 119.1 . . ?
C23 C28 C27 115.8(6) . . ?
C23 C28 C30 122.6(5) . . ?
C27 C28 C30 121.6(5) . . ?
C24 C29 H29A 109.5 . . ?
C24 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C24 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C28 C30 H30A 109.5 . . ?
C28 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C28 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
O6 V2 O3 109.23(16) . . ?
O6 V2 O4 112.42(17) . . ?
O3 V2 O4 138.34(15) . . ?
O6 V2 N3 101.88(16) . . ?
O3 V2 N3 87.09(13) . . ?
O4 V2 N3 84.76(13) . . ?
O6 V2 N4 100.17(16) . . ?
O3 V2 N4 87.19(13) . . ?
O4 V2 N4 85.39(13) . . ?
N3 V2 N4 157.89(16) . . ?
O6X V2X O4 100.5(8) . . ?
O6X V2X O3 106.8(8) . . ?
O4 V2X O3 152.4(4) . . ?
O6X V2X N4 111.6(9) . . ?
O4 V2X N4 88.2(2) . . ?
O3 V2X N4 85.8(2) . . ?
O6X V2X N3 106.0(9) . . ?
O4 V2X N3 85.0(2) . . ?
O3 V2X N3 83.4(2) . . ?
N4 V2X N3 142.4(3) . . ?
N3 C31 C32 127.7(4) . . ?
N3 C31 H31 116.1 . . ?
C32 C31 H31 116.1 . . ?
C37 C32 C33 120.7(4) . . ?
C37 C32 C31 117.1(4) . . ?
C33 C32 C31 122.2(4) . . ?
O3 C33 C34 121.1(4) . . ?
O3 C33 C32 122.7(3) . . ?
C34 C33 C32 116.2(4) . . ?
C35 C34 C33 122.5(4) . . ?
C35 C34 Br5 119.3(3) . . ?
C33 C34 Br5 118.2(3) . . ?
C34 C35 C36 119.8(4) . . ?
C34 C35 H35 120.1 . . ?
C36 C35 H35 120.1 . . ?
C37 C36 C35 120.5(4) . . ?
C37 C36 Br6 119.6(3) . . ?
C35 C36 Br6 119.8(3) . . ?
C36 C37 C32 120.2(4) . . ?
C36 C37 H37 119.9 . . ?
C32 C37 H37 119.9 . . ?
C33 O3 V2 130.2(3) . . ?
C33 O3 V2X 135.1(3) . . ?
C31 N3 C38 113.1(3) . . ?
C31 N3 V2 122.0(3) . . ?
C38 N3 V2 124.7(3) . . ?
C31 N3 V2X 120.7(3) . . ?
C38 N3 V2X 119.3(3) . . ?
C39 C38 C43 121.7(4) . . ?
C39 C38 N3 120.1(4) . . ?
C43 C38 N3 118.0(4) . . ?
C38 C39 C40 117.4(5) . . ?
C38 C39 C44 122.8(4) . . ?
C40 C39 C44 119.7(5) . . ?
C41 C40 C39 121.2(5) . . ?
C41 C40 H40 119.4 . . ?
C39 C40 H40 119.4 . . ?
C42 C41 C40 119.9(4) . . ?
C42 C41 H41 120.0 . . ?
C40 C41 H41 120.0 . . ?
C41 C42 C43 121.4(5) . . ?
C41 C42 H42 119.3 . . ?
C43 C42 H42 119.3 . . ?
C42 C43 C38 118.4(5) . . ?
C42 C43 C45 120.4(5) . . ?
C38 C43 C45 121.2(4) . . ?
C39 C44 H44A 109.5 . . ?
C39 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
C39 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
C43 C45 H45A 109.5 . . ?
C43 C45 H45B 109.5 . . ?
H45A C45 H45B 109.5 . . ?
C43 C45 H45C 109.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?
N4 C46 C47 126.5(4) . . ?
N4 C46 H46 116.7 . . ?
C47 C46 H46 116.7 . . ?
C48 C47 C52 121.0(4) . . ?
C48 C47 C46 121.9(4) . . ?
C52 C47 C46 117.0(4) . . ?
O4 C48 C47 122.9(4) . . ?
O4 C48 C49 120.2(4) . . ?
C47 C48 C49 116.9(4) . . ?
C50 C49 C48 122.3(4) . . ?
C50 C49 Br7 119.1(3) . . ?
C48 C49 Br7 118.6(3) . . ?
C49 C50 C51 119.1(4) . . ?
C49 C50 H50 120.5 . . ?
C51 C50 H50 120.5 . . ?
C52 C51 C50 121.5(4) . . ?
C52 C51 Br8 119.5(3) . . ?
C50 C51 Br8 119.0(3) . . ?
C51 C52 C47 118.9(4) . . ?
C51 C52 H52 120.5 . . ?
C47 C52 H52 120.5 . . ?
C48 O4 V2X 134.1(3) . . ?
C48 O4 V2 129.8(3) . . ?
C46 N4 C53 114.3(3) . . ?
C46 N4 V2 122.4(3) . . ?
C53 N4 V2 122.6(3) . . ?
C46 N4 V2X 119.4(3) . . ?
C53 N4 V2X 120.9(3) . . ?
C58 C53 C54 122.7(4) . . ?
C58 C53 N4 118.8(4) . . ?
C54 C53 N4 118.5(4) . . ?
C55 C54 C53 116.8(4) . . ?
C55 C54 C59 120.7(4) . . ?
C53 C54 C59 122.5(4) . . ?
C54 C55 C56 121.5(5) . . ?
C54 C55 H55 119.3 . . ?
C56 C55 H55 119.3 . . ?
C57 C56 C55 119.8(4) . . ?
C57 C56 H56 120.1 . . ?
C55 C56 H56 120.1 . . ?
C56 C57 C58 121.0(5) . . ?
C56 C57 H57 119.5 . . ?
C58 C57 H57 119.5 . . ?
C53 C58 C57 118.2(4) . . ?
C53 C58 C60 120.2(4) . . ?
C57 C58 C60 121.6(5) . . ?
C54 C59 H59A 109.5 . . ?
C54 C59 H59B 109.5 . . ?
H59A C59 H59B 109.5 . . ?
C54 C59 H59C 109.5 . . ?
H59A C59 H59C 109.5 . . ?
H59B C59 H59C 109.5 . . ?
C58 C60 H60A 109.5 . . ?
C58 C60 H60B 109.5 . . ?
H60A C60 H60B 109.5 . . ?
C58 C60 H60C 109.5 . . ?
H60A C60 H60C 109.5 . . ?
H60B C60 H60C 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
C8 N1 C1 C2 177.4(4) . . . . ?
V1 N1 C1 C2 -7.4(6) . . . . ?
V1X N1 C1 C2 25.1(6) . . . . ?
N1 C1 C2 C7 176.8(4) . . . . ?
N1 C1 C2 C3 -3.8(7) . . . . ?
C7 C2 C3 O1 175.1(4) . . . . ?
C1 C2 C3 O1 -4.2(7) . . . . ?
C7 C2 C3 C4 -3.9(6) . . . . ?
C1 C2 C3 C4 176.8(4) . . . . ?
O1 C3 C4 C5 -175.2(4) . . . . ?
C2 C3 C4 C5 3.8(7) . . . . ?
O1 C3 C4 Br1 4.0(6) . . . . ?
C2 C3 C4 Br1 -177.0(3) . . . . ?
C3 C4 C5 C6 -1.1(7) . . . . ?
Br1 C4 C5 C6 179.7(3) . . . . ?
C4 C5 C6 C7 -1.7(7) . . . . ?
C4 C5 C6 Br2 177.4(4) . . . . ?
C5 C6 C7 C2 1.6(7) . . . . ?
Br2 C6 C7 C2 -177.6(3) . . . . ?
C3 C2 C7 C6 1.3(6) . . . . ?
C1 C2 C7 C6 -179.3(4) . . . . ?
C2 C3 O1 V1X -18.0(7) . . . . ?
C4 C3 O1 V1X 160.9(4) . . . . ?
C2 C3 O1 V1 26.6(6) . . . . ?
C4 C3 O1 V1 -154.4(3) . . . . ?
O5X V1X O1 C3 -78.8(10) . . . . ?
O2 V1X O1 C3 99.0(8) . . . . ?
N2 V1X O1 C3 174.7(4) . . . . ?
N1 V1X O1 C3 29.4(5) . . . . ?
C1 N1 C8 C9 -78.2(5) . . . . ?
V1 N1 C8 C9 106.6(4) . . . . ?
V1X N1 C8 C9 73.6(5) . . . . ?
C1 N1 C8 C13 101.0(5) . . . . ?
V1 N1 C8 C13 -74.3(5) . . . . ?
V1X N1 C8 C13 -107.2(4) . . . . ?
C13 C8 C9 C10 -1.0(6) . . . . ?
N1 C8 C9 C10 178.2(4) . . . . ?
C13 C8 C9 C14 179.0(4) . . . . ?
N1 C8 C9 C14 -1.8(6) . . . . ?
C8 C9 C10 C11 0.9(7) . . . . ?
C14 C9 C10 C11 -179.1(4) . . . . ?
C9 C10 C11 C12 -0.4(7) . . . . ?
C10 C11 C12 C13 -0.1(7) . . . . ?
C11 C12 C13 C8 0.0(6) . . . . ?
C11 C12 C13 C15 -177.8(4) . . . . ?
C9 C8 C13 C12 0.5(6) . . . . ?
N1 C8 C13 C12 -178.6(4) . . . . ?
C9 C8 C13 C15 178.3(4) . . . . ?
N1 C8 C13 C15 -0.9(6) . . . . ?
C23 N2 C16 C17 177.3(4) . . . . ?
V1 N2 C16 C17 -12.5(6) . . . . ?
V1X N2 C16 C17 21.0(6) . . . . ?
N2 C16 C17 C22 174.7(4) . . . . ?
N2 C16 C17 C18 -9.1(7) . . . . ?
C22 C17 C18 O2 -179.2(4) . . . . ?
C16 C17 C18 O2 4.8(7) . . . . ?
C22 C17 C18 C19 3.1(6) . . . . ?
C16 C17 C18 C19 -173.0(4) . . . . ?
O2 C18 C19 C20 177.5(4) . . . . ?
C17 C18 C19 C20 -4.7(6) . . . . ?
O2 C18 C19 Br3 -0.9(6) . . . . ?
C17 C18 C19 Br3 176.9(3) . . . . ?
C18 C19 C20 C21 2.7(7) . . . . ?
Br3 C19 C20 C21 -178.9(3) . . . . ?
C19 C20 C21 C22 1.1(7) . . . . ?
C19 C20 C21 Br4 178.9(3) . . . . ?
C20 C21 C22 C17 -2.6(6) . . . . ?
Br4 C21 C22 C17 179.6(3) . . . . ?
C18 C17 C22 C21 0.4(6) . . . . ?
C16 C17 C22 C21 176.6(4) . . . . ?
C19 C18 O2 V1X 158.0(4) . . . . ?
C17 C18 O2 V1X -19.7(7) . . . . ?
C19 C18 O2 V1 -157.7(3) . . . . ?
C17 C18 O2 V1 24.6(6) . . . . ?
O5X V1X O2 C18 -82.5(10) . . . . ?
O1 V1X O2 C18 99.7(9) . . . . ?
N2 V1X O2 C18 24.2(5) . . . . ?
N1 V1X O2 C18 169.2(4) . . . . ?
C16 N2 C23 C24 -95.5(4) . . . . ?
V1 N2 C23 C24 94.5(4) . . . . ?
V1X N2 C23 C24 60.6(5) . . . . ?
C16 N2 C23 C28 81.0(5) . . . . ?
V1 N2 C23 C28 -89.0(4) . . . . ?
V1X N2 C23 C28 -122.9(4) . . . . ?
C28 C23 C24 C25 -1.9(6) . . . . ?
N2 C23 C24 C25 174.5(4) . . . . ?
C28 C23 C24 C29 178.4(4) . . . . ?
N2 C23 C24 C29 -5.2(6) . . . . ?
C23 C24 C25 C26 1.6(7) . . . . ?
C29 C24 C25 C26 -178.7(5) . . . . ?
C24 C25 C26 C27 -0.6(8) . . . . ?
C25 C26 C27 C28 -0.1(8) . . . . ?
C24 C23 C28 C27 1.2(6) . . . . ?
N2 C23 C28 C27 -175.2(4) . . . . ?
C24 C23 C28 C30 -179.3(4) . . . . ?
N2 C23 C28 C30 4.4(6) . . . . ?
C26 C27 C28 C23 -0.1(7) . . . . ?
C26 C27 C28 C30 -179.7(5) . . . . ?
N3 C31 C32 C37 -175.9(4) . . . . ?
N3 C31 C32 C33 5.9(7) . . . . ?
C37 C32 C33 O3 -177.8(4) . . . . ?
C31 C32 C33 O3 0.3(6) . . . . ?
C37 C32 C33 C34 1.4(6) . . . . ?
C31 C32 C33 C34 179.5(4) . . . . ?
O3 C33 C34 C35 177.6(4) . . . . ?
C32 C33 C34 C35 -1.7(7) . . . . ?
O3 C33 C34 Br5 -2.9(6) . . . . ?
C32 C33 C34 Br5 177.9(3) . . . . ?
C33 C34 C35 C36 0.4(7) . . . . ?
Br5 C34 C35 C36 -179.1(3) . . . . ?
C34 C35 C36 C37 1.1(7) . . . . ?
C34 C35 C36 Br6 -179.1(3) . . . . ?
C35 C36 C37 C32 -1.4(6) . . . . ?
Br6 C36 C37 C32 178.9(3) . . . . ?
C33 C32 C37 C36 0.1(6) . . . . ?
C31 C32 C37 C36 -178.2(4) . . . . ?
C34 C33 O3 V2 154.3(3) . . . . ?
C32 C33 O3 V2 -26.6(6) . . . . ?
C34 C33 O3 V2X -159.3(4) . . . . ?
C32 C33 O3 V2X 19.9(7) . . . . ?
C32 C31 N3 C38 -174.9(4) . . . . ?
C32 C31 N3 V2 10.5(6) . . . . ?
C32 C31 N3 V2X -24.2(6) . . . . ?
C31 N3 C38 C39 -101.8(5) . . . . ?
V2 N3 C38 C39 72.6(5) . . . . ?
V2X N3 C38 C39 107.0(4) . . . . ?
C31 N3 C38 C43 73.7(5) . . . . ?
V2 N3 C38 C43 -111.9(4) . . . . ?
V2X N3 C38 C43 -77.5(5) . . . . ?
C43 C38 C39 C40 -1.4(6) . . . . ?
N3 C38 C39 C40 173.9(4) . . . . ?
C43 C38 C39 C44 178.0(4) . . . . ?
N3 C38 C39 C44 -6.7(7) . . . . ?
C38 C39 C40 C41 0.3(7) . . . . ?
C44 C39 C40 C41 -179.2(4) . . . . ?
C39 C40 C41 C42 0.8(7) . . . . ?
C40 C41 C42 C43 -0.8(7) . . . . ?
C41 C42 C43 C38 -0.3(7) . . . . ?
C41 C42 C43 C45 177.5(5) . . . . ?
C39 C38 C43 C42 1.5(6) . . . . ?
N3 C38 C43 C42 -174.0(4) . . . . ?
C39 C38 C43 C45 -176.4(4) . . . . ?
N3 C38 C43 C45 8.2(6) . . . . ?
N4 C46 C47 C48 9.9(7) . . . . ?
N4 C46 C47 C52 -173.5(4) . . . . ?
C52 C47 C48 O4 177.5(4) . . . . ?
C46 C47 C48 O4 -6.0(7) . . . . ?
C52 C47 C48 C49 -5.3(6) . . . . ?
C46 C47 C48 C49 171.1(4) . . . . ?
O4 C48 C49 C50 -177.5(4) . . . . ?
C47 C48 C49 C50 5.2(7) . . . . ?
O4 C48 C49 Br7 0.2(6) . . . . ?
C47 C48 C49 Br7 -177.0(3) . . . . ?
C48 C49 C50 C51 -1.2(7) . . . . ?
Br7 C49 C50 C51 -178.9(3) . . . . ?
C49 C50 C51 C52 -3.0(7) . . . . ?
C49 C50 C51 Br8 176.7(3) . . . . ?
C50 C51 C52 C47 2.8(7) . . . . ?
Br8 C51 C52 C47 -176.8(3) . . . . ?
C48 C47 C52 C51 1.5(6) . . . . ?
C46 C47 C52 C51 -175.2(4) . . . . ?
C47 C48 O4 V2X 22.4(7) . . . . ?
C49 C48 O4 V2X -154.7(4) . . . . ?
C47 C48 O4 V2 -25.1(6) . . . . ?
C49 C48 O4 V2 157.8(3) . . . . ?
O6X V2X O4 C48 85.0(10) . . . . ?
O3 V2X O4 C48 -104.2(8) . . . . ?
N4 V2X O4 C48 -26.6(5) . . . . ?
N3 V2X O4 C48 -169.6(4) . . . . ?
C47 C46 N4 C53 -175.9(4) . . . . ?
C47 C46 N4 V2 13.3(6) . . . . ?
C47 C46 N4 V2X -21.8(6) . . . . ?
C46 N4 C53 C58 94.6(5) . . . . ?
V2 N4 C53 C58 -94.6(4) . . . . ?
V2X N4 C53 C58 -59.1(5) . . . . ?
C46 N4 C53 C54 -83.2(5) . . . . ?
V2 N4 C53 C54 87.5(4) . . . . ?
V2X N4 C53 C54 123.1(4) . . . . ?
C58 C53 C54 C55 1.4(6) . . . . ?
N4 C53 C54 C55 179.2(4) . . . . ?
C58 C53 C54 C59 -175.9(4) . . . . ?
N4 C53 C54 C59 1.9(6) . . . . ?
C53 C54 C55 C56 -0.8(6) . . . . ?
C59 C54 C55 C56 176.5(4) . . . . ?
C54 C55 C56 C57 0.1(7) . . . . ?
C55 C56 C57 C58 0.2(7) . . . . ?
C54 C53 C58 C57 -1.2(6) . . . . ?
N4 C53 C58 C57 -178.9(4) . . . . ?
C54 C53 C58 C60 179.9(4) . . . . ?
N4 C53 C58 C60 2.1(6) . . . . ?
C56 C57 C58 C53 0.3(7) . . . . ?
C56 C57 C58 C60 179.3(5) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
C22 H22 Br8 0.95 3.00 3.767(4) 139.3 2_674 yes
C37 H37 Br2 0.95 3.01 3.653(4) 126.4 2_665 yes

_refine_diff_density_max         1.194
_refine_diff_density_min         -0.698
_refine_diff_density_rms         0.060

_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: acetonitrile'
####################################################################### 
# 
# 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_3
_database_code_depnum_ccdc_archive 'CCDC 2524180'
loop_
_audit_author_name
_audit_author_address
'Mark Elsegood'
;Loughborough University
United Kingdom
;
_audit_update_record             
;
2026-01-19 deposited with the CCDC.	2026-03-10 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2019/3
_shelx_SHELXL_version_number     2019/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C28 H30 Br4 N O4 V'
_chemical_formula_sum            'C28 H30 Br4 N O4 V'
_chemical_formula_weight         815.11

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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

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

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

_cell_length_a                   13.0631(2)
_cell_length_b                   16.0877(3)
_cell_length_c                   14.1607(2)
_cell_angle_alpha                90
_cell_angle_beta                 93.7323(16)
_cell_angle_gamma                90
_cell_volume                     2969.63(8)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    32701
_cell_measurement_theta_min      1.91
_cell_measurement_theta_max      36.75

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.823
_exptl_crystal_F_000             1600
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.060
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.020
_exptl_absorpt_coefficient_mu    5.750
_shelx_estimated_absorpt_T_min   0.724
_shelx_estimated_absorpt_T_max   0.894
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.728
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   
; 
CrysAlisPro 1.171.43.143a (Rigaku Oxford Diffraction, 2024) 
Empirical absorption correction using spherical harmonics, 
implemented in SCALE3 ABSPACK scaling algorithm. 
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Rotating Anode'
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  
; 
Rigaku FRE+ equipped with Arc)Sec VHF Varimax confocal mirrors and an UG2 
goniometer and HyPix 6000HE detector 
;
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_radiation_collimation    0.2
_diffrn_detector_area_resol_mean 10
_diffrn_reflns_number            129381
_diffrn_reflns_av_unetI/netI     0.0351
_diffrn_reflns_av_R_equivalents  0.0660
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         1.918
_diffrn_reflns_theta_max         34.336
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             12440
_reflns_number_gt                8840
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
; 
 Reflections were merged by SHELXL according to the crystal 
 class for the calculation of statistics and refinement. 
  
 _reflns_Friedel_fraction is defined as the number of unique 
 Friedel pairs measured divided by the number that would be 
 possible theoretically, ignoring centric projections and 
 systematic absences. 
;

_computing_data_collection       
'CrysAlisPro system (CCD 43.142a 64-bit (release 17-10-2024))'
_computing_cell_refinement       'CrysAlisPro 1.171.43.143a (Rigaku OD, 2024)'
_computing_data_reduction        'CrysAlisPro 1.171.43.143a (Rigaku OD, 2024)'
_computing_structure_solution    'SHELXT-2018/2 (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2019/3 (Sheldrick, 2019)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0364P)²+4.0397P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         12440
_refine_ls_number_parameters     348
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0732
_refine_ls_R_factor_gt           0.0413
_refine_ls_wR_factor_ref         0.0947
_refine_ls_wR_factor_gt          0.0834
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_restrained_S_all      1.012
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
V1 V 0.52896(3) 0.31719(2) 0.18285(3) 0.01789(7) Uani 1 1 d . . . . .
O3 O 0.50665(12) 0.41339(10) 0.18831(12) 0.0222(3) Uani 1 1 d . . . . .
O1 O 0.56581(12) 0.28084(10) 0.29932(11) 0.0224(3) Uani 1 1 d . . . . .
C1 C 0.59813(16) 0.31980(14) 0.38017(15) 0.0191(4) Uani 1 1 d . . . . .
C2 C 0.52854(17) 0.35478(16) 0.43980(17) 0.0238(4) Uani 1 1 d . . . . .
Br1 Br 0.38741(2) 0.34960(2) 0.40337(2) 0.04132(8) Uani 1 1 d . . . . .
C3 C 0.56073(19) 0.39158(16) 0.52474(16) 0.0262(5) Uani 1 1 d . . . . .
H3 H 0.512819 0.415596 0.564425 0.031 Uiso 1 1 calc R U . . .
C4 C 0.6646(2) 0.39245(15) 0.55032(16) 0.0237(4) Uani 1 1 d . . . . .
Br2 Br 0.71175(3) 0.43703(2) 0.66915(2) 0.03568(7) Uani 1 1 d . . . . .
C5 C 0.73563(17) 0.35838(14) 0.49308(15) 0.0195(4) Uani 1 1 d . . . . .
H5 H 0.806675 0.360300 0.512161 0.023 Uiso 1 1 calc R U . . .
C6 C 0.70297(16) 0.32141(13) 0.40776(14) 0.0164(4) Uani 1 1 d . . . . .
C7 C 0.77872(16) 0.27934(13) 0.34680(14) 0.0173(4) Uani 1 1 d . . . . .
H7A H 0.840034 0.262570 0.387087 0.021 Uiso 1 1 calc R U . . .
H7B H 0.747066 0.228350 0.318763 0.021 Uiso 1 1 calc R U . . .
C8 C 0.84065(16) 0.29020(13) 0.18556(14) 0.0174(4) Uani 1 1 d . . . . .
H8A H 0.808917 0.234299 0.182701 0.021 Uiso 1 1 calc R U . . .
H8B H 0.916055 0.282900 0.189543 0.021 Uiso 1 1 calc R U . . .
O2 O 0.63542(12) 0.29816(10) 0.11249(11) 0.0197(3) Uani 1 1 d . . . . .
C9 C 0.70452(17) 0.34087(13) 0.06533(14) 0.0181(4) Uani 1 1 d . . . . .
C10 C 0.67537(19) 0.38456(14) -0.01744(15) 0.0225(4) Uani 1 1 d . . . . .
Br3 Br 0.53573(2) 0.39034(2) -0.05969(2) 0.03086(6) Uani 1 1 d . . . . .
C11 C 0.7477(2) 0.42103(15) -0.07120(16) 0.0269(5) Uani 1 1 d . . . . .
H11 H 0.727244 0.450455 -0.127447 0.032 Uiso 1 1 calc R U . . .
C12 C 0.8500(2) 0.41404(15) -0.04199(16) 0.0274(5) Uani 1 1 d . . . . .
Br4 Br 0.94936(3) 0.45479(2) -0.12180(2) 0.04221(8) Uani 1 1 d . . . . .
C13 C 0.88122(19) 0.37397(15) 0.04199(16) 0.0230(4) Uani 1 1 d . . . . .
H13 H 0.951932 0.371735 0.062258 0.028 Uiso 1 1 calc R U . . .
C14 C 0.80860(17) 0.33715(13) 0.09631(14) 0.0179(4) Uani 1 1 d . . . . .
N1 N 0.81052(13) 0.33324(11) 0.27085(12) 0.0147(3) Uani 1 1 d . . . . .
C15 C 0.87534(15) 0.40188(13) 0.30262(14) 0.0157(4) Uani 1 1 d . . . . .
C16 C 0.83434(16) 0.48270(13) 0.29494(14) 0.0167(4) Uani 1 1 d . . . . .
C17 C 0.89416(18) 0.54967(14) 0.32844(16) 0.0215(4) Uani 1 1 d . . . . .
H17 H 0.867025 0.604404 0.323604 0.026 Uiso 1 1 calc R U . . .
C18 C 0.99235(19) 0.53747(16) 0.36857(17) 0.0260(5) Uani 1 1 d . . . . .
H18 H 1.032100 0.583572 0.391408 0.031 Uiso 1 1 calc R U . . .
C19 C 1.03232(18) 0.45857(15) 0.37535(17) 0.0243(4) Uani 1 1 d . . . . .
H19 H 1.099907 0.450880 0.402922 0.029 Uiso 1 1 calc R U . . .
C20 C 0.97591(16) 0.38932(14) 0.34264(15) 0.0186(4) Uani 1 1 d . . . . .
C21 C 0.72767(16) 0.49932(14) 0.25029(15) 0.0185(4) Uani 1 1 d . . . . .
H21 H 0.696419 0.444446 0.231903 0.022 Uiso 1 1 calc R U . . .
C22 C 0.65809(19) 0.54074(15) 0.31926(18) 0.0263(5) Uani 1 1 d . . . . .
H22A H 0.653303 0.505300 0.375080 0.039 Uiso 1 1 calc R U . . .
H22B H 0.589537 0.548643 0.288175 0.039 Uiso 1 1 calc R U . . .
H22C H 0.686840 0.594825 0.338698 0.039 Uiso 1 1 calc R U . . .
C23 C 0.73219(19) 0.55122(16) 0.16003(17) 0.0257(5) Uani 1 1 d . . . . .
H23A H 0.755755 0.607520 0.176548 0.039 Uiso 1 1 calc R U . . .
H23B H 0.663719 0.553975 0.127507 0.039 Uiso 1 1 calc R U . . .
H23C H 0.779981 0.525393 0.118261 0.039 Uiso 1 1 calc R U . . .
C24 C 1.02760(17) 0.30463(15) 0.35081(17) 0.0225(4) Uani 1 1 d . . . . .
H24 H 0.976478 0.261759 0.327755 0.027 Uiso 1 1 calc R U . . .
C25 C 1.0629(2) 0.28340(18) 0.45355(18) 0.0309(5) Uani 1 1 d . . . . .
H25A H 1.114970 0.323571 0.477000 0.046 Uiso 1 1 calc R U . . .
H25B H 1.092284 0.227321 0.456177 0.046 Uiso 1 1 calc R U . . .
H25C H 1.004122 0.285765 0.493037 0.046 Uiso 1 1 calc R U . . .
C26 C 1.11873(19) 0.30075(18) 0.2878(2) 0.0329(6) Uani 1 1 d . . . . .
H26A H 1.094754 0.311796 0.222019 0.049 Uiso 1 1 calc R U . . .
H26B H 1.149902 0.245368 0.292408 0.049 Uiso 1 1 calc R U . . .
H26C H 1.169744 0.342612 0.308868 0.049 Uiso 1 1 calc R U . . .
O4 O 0.41964(12) 0.26462(11) 0.13911(12) 0.0238(3) Uani 1 1 d . . . . .
C27 C 0.31505(19) 0.28154(19) 0.1115(3) 0.0395(7) Uani 1 1 d . . . . .
H27A H 0.271749 0.255231 0.157986 0.047 Uiso 1 1 calc R U . . .
H27B H 0.298108 0.254883 0.049477 0.047 Uiso 1 1 calc R U . . .
C28 C 0.2875(2) 0.3707(2) 0.1039(3) 0.0431(7) Uani 1 1 d . . . . .
H28A H 0.298041 0.396962 0.166254 0.065 Uiso 1 1 calc R U . . .
H28B H 0.215377 0.376068 0.081179 0.065 Uiso 1 1 calc R U . . .
H28C H 0.330976 0.398010 0.059369 0.065 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
V1 O3 1.5776(17) . ?
V1 O4 1.7387(16) . ?
V1 O1 1.7861(16) . ?
V1 O2 1.7891(16) . ?
O1 C1 1.349(3) . ?
C1 C2 1.399(3) . ?
C1 C6 1.400(3) . ?
C2 C3 1.381(4) . ?
C2 Br1 1.884(2) . ?
C3 C4 1.381(4) . ?
C3 H3 0.9500 . ?
C4 C5 1.385(3) . ?
C4 Br2 1.895(2) . ?
C5 C6 1.389(3) . ?
C5 H5 0.9500 . ?
C6 C7 1.515(3) . ?
C7 N1 1.463(3) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 N1 1.468(3) . ?
C8 C14 1.508(3) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
O2 C9 1.346(3) . ?
C9 C10 1.398(3) . ?
C9 C14 1.402(3) . ?
C10 C11 1.383(3) . ?
C10 Br3 1.885(2) . ?
C11 C12 1.377(4) . ?
C11 H11 0.9500 . ?
C12 C13 1.390(3) . ?
C12 Br4 1.893(2) . ?
C13 C14 1.392(3) . ?
C13 H13 0.9500 . ?
N1 C15 1.445(3) . ?
C15 C16 1.408(3) . ?
C15 C20 1.411(3) . ?
C16 C17 1.396(3) . ?
C16 C21 1.516(3) . ?
C17 C18 1.383(3) . ?
C17 H17 0.9500 . ?
C18 C19 1.373(4) . ?
C18 H18 0.9500 . ?
C19 C20 1.398(3) . ?
C19 H19 0.9500 . ?
C20 C24 1.522(3) . ?
C21 C22 1.530(3) . ?
C21 C23 1.531(3) . ?
C21 H21 1.0000 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 C26 1.534(3) . ?
C24 C25 1.536(3) . ?
C24 H24 1.0000 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
O4 C27 1.423(3) . ?
C27 C28 1.481(4) . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?

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
O3 V1 O4 110.15(8) . . ?
O3 V1 O1 108.39(8) . . ?
O4 V1 O1 109.60(8) . . ?
O3 V1 O2 110.36(8) . . ?
O4 V1 O2 111.62(8) . . ?
O1 V1 O2 106.60(8) . . ?
C1 O1 V1 133.03(15) . . ?
O1 C1 C2 121.3(2) . . ?
O1 C1 C6 119.48(19) . . ?
C2 C1 C6 119.1(2) . . ?
C3 C2 C1 121.7(2) . . ?
C3 C2 Br1 119.63(17) . . ?
C1 C2 Br1 118.68(18) . . ?
C4 C3 C2 118.1(2) . . ?
C4 C3 H3 121.0 . . ?
C2 C3 H3 121.0 . . ?
C3 C4 C5 121.8(2) . . ?
C3 C4 Br2 119.59(17) . . ?
C5 C4 Br2 118.55(18) . . ?
C4 C5 C6 119.9(2) . . ?
C4 C5 H5 120.0 . . ?
C6 C5 H5 120.0 . . ?
C5 C6 C1 119.37(19) . . ?
C5 C6 C7 120.80(19) . . ?
C1 C6 C7 119.76(19) . . ?
N1 C7 C6 112.42(17) . . ?
N1 C7 H7A 109.1 . . ?
C6 C7 H7A 109.1 . . ?
N1 C7 H7B 109.1 . . ?
C6 C7 H7B 109.1 . . ?
H7A C7 H7B 107.9 . . ?
N1 C8 C14 112.25(17) . . ?
N1 C8 H8A 109.2 . . ?
C14 C8 H8A 109.2 . . ?
N1 C8 H8B 109.2 . . ?
C14 C8 H8B 109.2 . . ?
H8A C8 H8B 107.9 . . ?
C9 O2 V1 139.44(14) . . ?
O2 C9 C10 121.2(2) . . ?
O2 C9 C14 119.40(19) . . ?
C10 C9 C14 119.3(2) . . ?
C11 C10 C9 121.1(2) . . ?
C11 C10 Br3 119.13(17) . . ?
C9 C10 Br3 119.74(18) . . ?
C12 C11 C10 119.0(2) . . ?
C12 C11 H11 120.5 . . ?
C10 C11 H11 120.5 . . ?
C11 C12 C13 121.3(2) . . ?
C11 C12 Br4 118.80(18) . . ?
C13 C12 Br4 119.8(2) . . ?
C12 C13 C14 119.8(2) . . ?
C12 C13 H13 120.1 . . ?
C14 C13 H13 120.1 . . ?
C13 C14 C9 119.4(2) . . ?
C13 C14 C8 121.0(2) . . ?
C9 C14 C8 119.61(19) . . ?
C15 N1 C7 114.37(16) . . ?
C15 N1 C8 115.69(16) . . ?
C7 N1 C8 115.44(17) . . ?
C16 C15 C20 120.20(19) . . ?
C16 C15 N1 117.99(18) . . ?
C20 C15 N1 121.79(19) . . ?
C17 C16 C15 119.0(2) . . ?
C17 C16 C21 118.99(19) . . ?
C15 C16 C21 121.99(19) . . ?
C18 C17 C16 120.9(2) . . ?
C18 C17 H17 119.5 . . ?
C16 C17 H17 119.5 . . ?
C19 C18 C17 119.9(2) . . ?
C19 C18 H18 120.1 . . ?
C17 C18 H18 120.1 . . ?
C18 C19 C20 121.6(2) . . ?
C18 C19 H19 119.2 . . ?
C20 C19 H19 119.2 . . ?
C19 C20 C15 118.4(2) . . ?
C19 C20 C24 117.82(19) . . ?
C15 C20 C24 123.8(2) . . ?
C16 C21 C22 112.26(18) . . ?
C16 C21 C23 111.10(18) . . ?
C22 C21 C23 110.63(19) . . ?
C16 C21 H21 107.5 . . ?
C22 C21 H21 107.5 . . ?
C23 C21 H21 107.5 . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C21 C23 H23A 109.5 . . ?
C21 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C21 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C20 C24 C26 110.5(2) . . ?
C20 C24 C25 112.1(2) . . ?
C26 C24 C25 110.2(2) . . ?
C20 C24 H24 108.0 . . ?
C26 C24 H24 108.0 . . ?
C25 C24 H24 108.0 . . ?
C24 C25 H25A 109.5 . . ?
C24 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C24 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C24 C26 H26A 109.5 . . ?
C24 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C24 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C27 O4 V1 139.16(17) . . ?
O4 C27 C28 115.4(2) . . ?
O4 C27 H27A 108.4 . . ?
C28 C27 H27A 108.4 . . ?
O4 C27 H27B 108.4 . . ?
C28 C27 H27B 108.4 . . ?
H27A C27 H27B 107.5 . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 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
O3 V1 O1 C1 -16.8(2) . . . . ?
O4 V1 O1 C1 -137.05(19) . . . . ?
O2 V1 O1 C1 102.00(19) . . . . ?
V1 O1 C1 C2 83.1(3) . . . . ?
V1 O1 C1 C6 -100.5(2) . . . . ?
O1 C1 C2 C3 177.1(2) . . . . ?
C6 C1 C2 C3 0.6(3) . . . . ?
O1 C1 C2 Br1 -1.9(3) . . . . ?
C6 C1 C2 Br1 -178.36(16) . . . . ?
C1 C2 C3 C4 -0.6(4) . . . . ?
Br1 C2 C3 C4 178.41(18) . . . . ?
C2 C3 C4 C5 0.5(4) . . . . ?
C2 C3 C4 Br2 -176.73(18) . . . . ?
C3 C4 C5 C6 -0.6(3) . . . . ?
Br2 C4 C5 C6 176.72(16) . . . . ?
C4 C5 C6 C1 0.6(3) . . . . ?
C4 C5 C6 C7 -176.39(19) . . . . ?
O1 C1 C6 C5 -177.20(19) . . . . ?
C2 C1 C6 C5 -0.7(3) . . . . ?
O1 C1 C6 C7 -0.1(3) . . . . ?
C2 C1 C6 C7 176.40(19) . . . . ?
C5 C6 C7 N1 -97.6(2) . . . . ?
C1 C6 C7 N1 85.4(2) . . . . ?
O3 V1 O2 C9 2.9(2) . . . . ?
O4 V1 O2 C9 125.8(2) . . . . ?
O1 V1 O2 C9 -114.6(2) . . . . ?
V1 O2 C9 C10 -69.8(3) . . . . ?
V1 O2 C9 C14 114.3(2) . . . . ?
O2 C9 C10 C11 -173.1(2) . . . . ?
C14 C9 C10 C11 2.8(3) . . . . ?
O2 C9 C10 Br3 4.3(3) . . . . ?
C14 C9 C10 Br3 -179.82(16) . . . . ?
C9 C10 C11 C12 -0.2(3) . . . . ?
Br3 C10 C11 C12 -177.60(18) . . . . ?
C10 C11 C12 C13 -2.5(4) . . . . ?
C10 C11 C12 Br4 174.06(17) . . . . ?
C11 C12 C13 C14 2.6(4) . . . . ?
Br4 C12 C13 C14 -173.98(17) . . . . ?
C12 C13 C14 C9 0.1(3) . . . . ?
C12 C13 C14 C8 177.4(2) . . . . ?
O2 C9 C14 C13 173.24(19) . . . . ?
C10 C9 C14 C13 -2.7(3) . . . . ?
O2 C9 C14 C8 -4.1(3) . . . . ?
C10 C9 C14 C8 179.94(19) . . . . ?
N1 C8 C14 C13 111.3(2) . . . . ?
N1 C8 C14 C9 -71.4(2) . . . . ?
C6 C7 N1 C15 70.2(2) . . . . ?
C6 C7 N1 C8 -151.84(18) . . . . ?
C14 C8 N1 C15 -78.9(2) . . . . ?
C14 C8 N1 C7 143.74(18) . . . . ?
C7 N1 C15 C16 -110.8(2) . . . . ?
C8 N1 C15 C16 111.3(2) . . . . ?
C7 N1 C15 C20 67.5(2) . . . . ?
C8 N1 C15 C20 -70.3(2) . . . . ?
C20 C15 C16 C17 -0.7(3) . . . . ?
N1 C15 C16 C17 177.61(18) . . . . ?
C20 C15 C16 C21 178.49(18) . . . . ?
N1 C15 C16 C21 -3.2(3) . . . . ?
C15 C16 C17 C18 0.1(3) . . . . ?
C21 C16 C17 C18 -179.2(2) . . . . ?
C16 C17 C18 C19 0.3(4) . . . . ?
C17 C18 C19 C20 -0.1(4) . . . . ?
C18 C19 C20 C15 -0.5(3) . . . . ?
C18 C19 C20 C24 178.4(2) . . . . ?
C16 C15 C20 C19 1.0(3) . . . . ?
N1 C15 C20 C19 -177.34(19) . . . . ?
C16 C15 C20 C24 -177.93(19) . . . . ?
N1 C15 C20 C24 3.8(3) . . . . ?
C17 C16 C21 C22 -60.9(3) . . . . ?
C15 C16 C21 C22 119.9(2) . . . . ?
C17 C16 C21 C23 63.6(3) . . . . ?
C15 C16 C21 C23 -115.6(2) . . . . ?
C19 C20 C24 C26 -65.0(3) . . . . ?
C15 C20 C24 C26 113.9(2) . . . . ?
C19 C20 C24 C25 58.2(3) . . . . ?
C15 C20 C24 C25 -122.9(2) . . . . ?
O3 V1 O4 C27 -4.4(3) . . . . ?
O1 V1 O4 C27 114.8(3) . . . . ?
O2 V1 O4 C27 -127.3(3) . . . . ?
V1 O4 C27 C28 10.7(5) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
C8 H8A Br2 0.99 3.04 4.025(2) 178.7 4_565 yes
C11 H11 Br2 0.95 2.88 3.685(2) 142.9 1_554 yes
C27 H27B Br1 0.99 2.96 3.794(3) 142.2 4_565 yes

_refine_diff_density_max         1.677
_refine_diff_density_min         -1.425
_refine_diff_density_rms         0.110

_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: acetonitrile'
####################################################################### 
# 
# 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_5
_database_code_depnum_ccdc_archive 'CCDC 2524182'
loop_
_audit_author_name
_audit_author_address
'Mark Elsegood'
;Loughborough University
United Kingdom
;
_audit_update_record             
;
2026-01-19 deposited with the CCDC.	2026-03-10 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C38 H40 Br4 N2 O3 V'
_chemical_formula_sum            'C38 H40 Br4 N2 O3 V'
_chemical_formula_weight         943.30

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
V V 0.0687 2.1097 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.6763 1.2805 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.34746(10)
_cell_length_b                   9.37245(14)
_cell_length_c                   12.34112(13)
_cell_angle_alpha                68.3876(12)
_cell_angle_beta                 79.1420(9)
_cell_angle_gamma                81.4636(10)
_cell_volume                     983.47(2)
_cell_formula_units_Z            1
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    30524
_cell_measurement_theta_min      3.89
_cell_measurement_theta_max      76.33

_exptl_crystal_description       plate
_exptl_crystal_colour            'dark green'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.593
_exptl_crystal_F_000             469
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.240
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.025
_exptl_absorpt_coefficient_mu    7.158
_shelx_estimated_absorpt_T_min   0.278
_shelx_estimated_absorpt_T_max   0.841
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.367
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   
; 
CrysAlisPro 1.171.42.74a (Rigaku Oxford Diffraction, 2022) 
Empirical absorption correction using spherical harmonics, 
implemented in SCALE3 ABSPACK scaling algorithm. 
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_source                   'Rotating anode'
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  
; 
Rigaku 007HF diffractometer with HF Varimax confocal mirrors, 
an UG2 goniometer and HyPix 6000HE detector 
;
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_detector_area_resol_mean 10
_diffrn_radiation_collimation    0.3
_diffrn_reflns_number            34358
_diffrn_reflns_av_unetI/netI     0.0153
_diffrn_reflns_av_R_equivalents  0.0411
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         3.894
_diffrn_reflns_theta_max         70.060
_diffrn_reflns_theta_full        67.679
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measured_fraction_theta_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_point_group_measured_fraction_full 0.995
_reflns_number_total             3714
_reflns_number_gt                3699
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
; 
 Reflections were merged by SHELXL according to the crystal 
 class for the calculation of statistics and refinement. 
  
 _reflns_Friedel_fraction is defined as the number of unique 
 Friedel pairs measured divided by the number that would be 
 possible theoretically, ignoring centric projections and 
 systematic absences. 
;

_computing_data_collection       'CrysAlisPro 1.171.42.74a (Rigaku OD, 2022)'
_computing_cell_refinement       'CrysAlisPro 1.171.42.74a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.74a (Rigaku OD, 2022)'
_computing_structure_solution    'SHELXT-2018/2 (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0109P)²+2.6018P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_extinction_coef       0.00268(19)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         3714
_refine_ls_number_parameters     231
_refine_ls_number_restraints     84
_refine_ls_R_factor_all          0.0322
_refine_ls_R_factor_gt           0.0321
_refine_ls_wR_factor_ref         0.0698
_refine_ls_wR_factor_gt          0.0697
_refine_ls_goodness_of_fit_ref   1.125
_refine_ls_restrained_S_all      1.120
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
V1 V 0.46115(10) 0.45940(10) 0.49838(8) 0.01475(19) Uani 0.5 1 d . . P . .
O1 O 0.5417(2) 0.3660(2) 0.64261(16) 0.0219(4) Uani 1 1 d . . . . .
O2 O 0.3480(4) 0.3499(5) 0.4974(4) 0.0243(9) Uani 0.5 1 d . . P . .
C1 C 0.6403(3) 0.2496(3) 0.6762(2) 0.0173(5) Uani 1 1 d . . . . .
C2 C 0.6470(3) 0.1675(3) 0.7974(2) 0.0203(6) Uani 1 1 d . . . . .
Br1 Br 0.50999(4) 0.22995(4) 0.90810(3) 0.03078(12) Uani 1 1 d . . . . .
C3 C 0.7490(3) 0.0445(3) 0.8369(2) 0.0211(6) Uani 1 1 d . . . . .
H3 H 0.750039 -0.008250 0.918881 0.025 Uiso 1 1 calc R U . . .
C4 C 0.8501(3) -0.0008(3) 0.7550(2) 0.0213(6) Uani 1 1 d . . . . .
Br2 Br 0.99268(3) -0.16803(4) 0.80692(3) 0.02846(12) Uani 1 1 d . . . . .
C5 C 0.8485(3) 0.0744(3) 0.6365(2) 0.0218(6) Uani 1 1 d . . . . .
H5 H 0.918129 0.042284 0.581360 0.026 Uiso 1 1 calc R U . . .
C6 C 0.7440(3) 0.1991(3) 0.5963(2) 0.0185(5) Uani 1 1 d . . . . .
C7 C 0.7489(3) 0.2719(3) 0.4705(2) 0.0195(6) Uani 1 1 d . . . . .
H7 H 0.821996 0.229756 0.423245 0.023 Uiso 1 1 calc R U . . .
N1 N 0.6660(3) 0.3864(3) 0.4156(2) 0.0251(5) Uani 1 1 d . . . . .
C8 C 0.6981(3) 0.4306(3) 0.2882(2) 0.0188(6) Uani 1 1 d . . . . .
C9 C 0.6311(3) 0.3606(3) 0.2317(3) 0.0268(6) Uani 1 1 d . U . . .
C10 C 0.6755(4) 0.3978(4) 0.1099(3) 0.0408(9) Uani 1 1 d . . . . .
H10 H 0.632128 0.352532 0.068055 0.049 Uiso 1 1 calc R U . . .
C11 C 0.7809(4) 0.4989(4) 0.0500(3) 0.0397(9) Uani 1 1 d . . . . .
H11 H 0.810655 0.521217 -0.032042 0.048 Uiso 1 1 calc R U . . .
C12 C 0.8420(4) 0.5666(4) 0.1081(3) 0.0352(8) Uani 1 1 d . . . . .
H12 H 0.913751 0.636846 0.065512 0.042 Uiso 1 1 calc R U . . .
C13 C 0.8024(3) 0.5356(3) 0.2281(3) 0.0239(6) Uani 1 1 d . U . . .
C14 C 0.5158(4) 0.2495(4) 0.2968(5) 0.0555(12) Uani 1 1 d . U . . .
H14 H 0.493591 0.246050 0.380200 0.067 Uiso 1 1 calc R U . . .
C15 C 0.5707(6) 0.0857(5) 0.2976(8) 0.110(3) Uani 1 1 d . U . . .
H15A H 0.590550 0.086363 0.216509 0.166 Uiso 1 1 calc R U . . .
H15B H 0.495736 0.015039 0.343209 0.166 Uiso 1 1 calc R U . . .
H15C H 0.660579 0.051481 0.333396 0.166 Uiso 1 1 calc R U . . .
C16 C 0.3751(4) 0.3046(5) 0.2413(5) 0.0647(14) Uani 1 1 d . U . . .
H16A H 0.343459 0.410256 0.238348 0.097 Uiso 1 1 calc R U . . .
H16B H 0.298569 0.236953 0.288681 0.097 Uiso 1 1 calc R U . . .
H16C H 0.393355 0.301886 0.161168 0.097 Uiso 1 1 calc R U . . .
C17 C 0.8719(4) 0.6159(4) 0.2888(4) 0.0453(9) Uani 1 1 d . U . . .
H17 H 0.821194 0.586879 0.371895 0.054 Uiso 1 1 calc R U . . .
C18 C 1.0336(6) 0.5595(6) 0.2942(7) 0.092(2) Uani 1 1 d . U . . .
H18A H 1.042955 0.447918 0.336030 0.137 Uiso 1 1 calc R U . . .
H18B H 1.074575 0.611110 0.336038 0.137 Uiso 1 1 calc R U . . .
H18C H 1.086697 0.583470 0.214040 0.137 Uiso 1 1 calc R U . . .
C19 C 0.8508(6) 0.7895(5) 0.2340(6) 0.0742(16) Uani 1 1 d . U . . .
H19A H 0.903444 0.822896 0.153479 0.111 Uiso 1 1 calc R U . . .
H19B H 0.888820 0.836165 0.280801 0.111 Uiso 1 1 calc R U . . .
H19C H 0.746372 0.821957 0.232278 0.111 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
V1 V1 1.1427(19) 2_666 ?
V1 O2 1.583(4) . ?
V1 O1 1.901(2) 2_666 ?
V1 O1 1.914(2) . ?
V1 N1 2.137(2) . ?
V1 N1 2.184(2) 2_666 ?
O1 C1 1.313(3) . ?
C1 C6 1.408(4) . ?
C1 C2 1.416(4) . ?
C2 C3 1.382(4) . ?
C2 Br1 1.886(3) . ?
C3 C4 1.390(4) . ?
C3 H3 0.9500 . ?
C4 C5 1.372(4) . ?
C4 Br2 1.898(3) . ?
C5 C6 1.408(4) . ?
C5 H5 0.9500 . ?
C6 C7 1.442(4) . ?
C7 N1 1.276(4) . ?
C7 H7 0.9500 . ?
N1 C8 1.454(3) . ?
C8 C9 1.389(4) . ?
C8 C13 1.394(4) . ?
C9 C10 1.406(5) . ?
C9 C14 1.511(5) . ?
C10 C11 1.379(6) . ?
C10 H10 0.9500 . ?
C11 C12 1.356(6) . ?
C11 H11 0.9500 . ?
C12 C13 1.387(4) . ?
C12 H12 0.9500 . ?
C13 C17 1.515(5) . ?
C14 C16 1.531(5) . ?
C14 C15 1.542(7) . ?
C14 H14 1.0000 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 C19 1.513(6) . ?
C17 C18 1.530(6) . ?
C17 H17 1.0000 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?

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
V1 V1 O2 177.45(18) 2_666 . ?
V1 V1 O1 73.20(11) 2_666 2_666 ?
O2 V1 O1 107.11(17) . 2_666 ?
V1 V1 O1 71.94(10) 2_666 . ?
O2 V1 O1 107.72(17) . . ?
O1 V1 O1 145.14(6) 2_666 . ?
V1 V1 N1 76.98(11) 2_666 . ?
O2 V1 N1 105.55(16) . . ?
O1 V1 N1 86.11(9) 2_666 . ?
O1 V1 N1 86.15(9) . . ?
V1 V1 N1 72.38(11) 2_666 2_666 ?
O2 V1 N1 105.10(16) . 2_666 ?
O1 V1 N1 85.13(9) 2_666 2_666 ?
O1 V1 N1 84.46(9) . 2_666 ?
N1 V1 N1 149.35(6) . 2_666 ?
C1 O1 V1 131.65(18) . 2_666 ?
C1 O1 V1 131.47(17) . . ?
O1 C1 C6 123.0(2) . . ?
O1 C1 C2 120.6(2) . . ?
C6 C1 C2 116.4(2) . . ?
C3 C2 C1 122.7(2) . . ?
C3 C2 Br1 119.3(2) . . ?
C1 C2 Br1 118.0(2) . . ?
C2 C3 C4 119.1(2) . . ?
C2 C3 H3 120.4 . . ?
C4 C3 H3 120.4 . . ?
C5 C4 C3 120.7(2) . . ?
C5 C4 Br2 119.4(2) . . ?
C3 C4 Br2 120.0(2) . . ?
C4 C5 C6 120.2(3) . . ?
C4 C5 H5 119.9 . . ?
C6 C5 H5 119.9 . . ?
C5 C6 C1 121.0(2) . . ?
C5 C6 C7 116.9(2) . . ?
C1 C6 C7 122.1(2) . . ?
N1 C7 C6 127.3(2) . . ?
N1 C7 H7 116.4 . . ?
C6 C7 H7 116.4 . . ?
C7 N1 C8 113.6(2) . . ?
C7 N1 V1 122.65(19) . . ?
C8 N1 V1 121.02(17) . . ?
C7 N1 V1 121.44(19) . 2_666 ?
C8 N1 V1 122.37(17) . 2_666 ?
C9 C8 C13 122.4(3) . . ?
C9 C8 N1 119.3(3) . . ?
C13 C8 N1 118.1(3) . . ?
C8 C9 C10 116.9(3) . . ?
C8 C9 C14 122.2(3) . . ?
C10 C9 C14 120.9(3) . . ?
C11 C10 C9 121.2(3) . . ?
C11 C10 H10 119.4 . . ?
C9 C10 H10 119.4 . . ?
C12 C11 C10 120.2(3) . . ?
C12 C11 H11 119.9 . . ?
C10 C11 H11 119.9 . . ?
C11 C12 C13 121.5(3) . . ?
C11 C12 H12 119.2 . . ?
C13 C12 H12 119.2 . . ?
C12 C13 C8 117.8(3) . . ?
C12 C13 C17 119.7(3) . . ?
C8 C13 C17 122.5(3) . . ?
C9 C14 C16 110.4(3) . . ?
C9 C14 C15 111.1(4) . . ?
C16 C14 C15 110.2(4) . . ?
C9 C14 H14 108.4 . . ?
C16 C14 H14 108.4 . . ?
C15 C14 H14 108.4 . . ?
C14 C15 H15A 109.5 . . ?
C14 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C14 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C14 C16 H16A 109.5 . . ?
C14 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C14 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C19 C17 C13 112.5(3) . . ?
C19 C17 C18 111.4(4) . . ?
C13 C17 C18 111.4(3) . . ?
C19 C17 H17 107.1 . . ?
C13 C17 H17 107.1 . . ?
C18 C17 H17 107.1 . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C17 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C17 C19 H19A 109.5 . . ?
C17 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C17 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 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
V1 O1 C1 C6 -25.1(4) 2_666 . . . ?
V1 O1 C1 C6 22.1(4) . . . . ?
V1 O1 C1 C2 154.9(2) 2_666 . . . ?
V1 O1 C1 C2 -158.0(2) . . . . ?
O1 C1 C2 C3 -179.8(3) . . . . ?
C6 C1 C2 C3 0.2(4) . . . . ?
O1 C1 C2 Br1 0.3(4) . . . . ?
C6 C1 C2 Br1 -179.8(2) . . . . ?
C1 C2 C3 C4 0.3(4) . . . . ?
Br1 C2 C3 C4 -179.8(2) . . . . ?
C2 C3 C4 C5 -0.4(4) . . . . ?
C2 C3 C4 Br2 179.4(2) . . . . ?
C3 C4 C5 C6 0.1(4) . . . . ?
Br2 C4 C5 C6 -179.7(2) . . . . ?
C4 C5 C6 C1 0.4(4) . . . . ?
C4 C5 C6 C7 -179.7(3) . . . . ?
O1 C1 C6 C5 179.5(3) . . . . ?
C2 C1 C6 C5 -0.5(4) . . . . ?
O1 C1 C6 C7 -0.4(4) . . . . ?
C2 C1 C6 C7 179.6(3) . . . . ?
C5 C6 C7 N1 -179.4(3) . . . . ?
C1 C6 C7 N1 0.5(5) . . . . ?
C6 C7 N1 C8 -179.1(3) . . . . ?
C6 C7 N1 V1 -17.6(4) . . . . ?
C6 C7 N1 V1 18.7(4) . . . 2_666 ?
C7 N1 C8 C9 88.0(3) . . . . ?
V1 N1 C8 C9 -73.8(3) . . . . ?
V1 N1 C8 C9 -110.0(3) 2_666 . . . ?
C7 N1 C8 C13 -88.2(3) . . . . ?
V1 N1 C8 C13 110.0(3) . . . . ?
V1 N1 C8 C13 73.8(3) 2_666 . . . ?
C13 C8 C9 C10 1.3(4) . . . . ?
N1 C8 C9 C10 -174.7(2) . . . . ?
C13 C8 C9 C14 -178.7(3) . . . . ?
N1 C8 C9 C14 5.3(4) . . . . ?
C8 C9 C10 C11 0.2(4) . . . . ?
C14 C9 C10 C11 -179.9(3) . . . . ?
C9 C10 C11 C12 -1.1(5) . . . . ?
C10 C11 C12 C13 0.7(5) . . . . ?
C11 C12 C13 C8 0.7(4) . . . . ?
C11 C12 C13 C17 -179.0(3) . . . . ?
C9 C8 C13 C12 -1.7(4) . . . . ?
N1 C8 C13 C12 174.3(2) . . . . ?
C9 C8 C13 C17 178.0(3) . . . . ?
N1 C8 C13 C17 -6.0(4) . . . . ?
C8 C9 C14 C16 123.6(4) . . . . ?
C10 C9 C14 C16 -56.4(5) . . . . ?
C8 C9 C14 C15 -113.9(5) . . . . ?
C10 C9 C14 C15 66.1(5) . . . . ?
C12 C13 C17 C19 56.6(5) . . . . ?
C8 C13 C17 C19 -123.1(4) . . . . ?
C12 C13 C17 C18 -69.3(5) . . . . ?
C8 C13 C17 C18 111.0(5) . . . . ?

_refine_diff_density_max         0.914
_refine_diff_density_min         -1.046
_refine_diff_density_rms         0.074


#===END
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: acetonitrile'
####################################################################### 
# 
# 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_2
_database_code_depnum_ccdc_archive 'CCDC 2524179'
loop_
_audit_author_name
_audit_author_address
'Mark Elsegood'
;Loughborough University
United Kingdom
;
_audit_update_record             
;
2026-01-19 deposited with the CCDC.	2026-03-10 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C29 H32 Br4 N O4 V'
_chemical_formula_sum            'C29 H32 Br4 N O4 V'
_chemical_formula_weight         829.13

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
V V 0.0687 2.1097 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.6763 1.2805 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.52053(7)
_cell_length_b                   11.43949(10)
_cell_length_c                   14.40070(13)
_cell_angle_alpha                95.0549(7)
_cell_angle_beta                 90.9208(7)
_cell_angle_gamma                96.0612(7)
_cell_volume                     1553.04(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    37235
_cell_measurement_theta_min      3.05
_cell_measurement_theta_max      76.17

_exptl_crystal_description       block
_exptl_crystal_colour            'dark yellow'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.773
_exptl_crystal_F_000             816
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.220
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.090
_exptl_absorpt_coefficient_mu    8.978
_shelx_estimated_absorpt_T_min   0.243
_shelx_estimated_absorpt_T_max   0.499
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.290
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   
; 
CrysAlisPro 1.171.41.122a (Rigaku Oxford Diffraction, 2021) 
Empirical absorption correction using spherical harmonics, 
implemented in SCALE3 ABSPACK scaling algorithm. 
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_source                   'Rotating anode'
_diffrn_measurement_device_type  
; 
Rigaku 007HF diffractometer with HF Varimax confocal mirrors, 
an UG2 goniometer and HyPix 6000HE detector. 
;
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_radiation_collimation    0.3
_diffrn_detector_area_resol_mean 10
_diffrn_reflns_number            41012
_diffrn_reflns_av_unetI/netI     0.0172
_diffrn_reflns_av_R_equivalents  0.0373
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         3.082
_diffrn_reflns_theta_max         70.039
_diffrn_reflns_theta_full        67.679
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measured_fraction_theta_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_point_group_measured_fraction_full 0.995
_reflns_number_total             5854
_reflns_number_gt                5833
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
; 
 Reflections were merged by SHELXL according to the crystal 
 class for the calculation of statistics and refinement. 
  
 _reflns_Friedel_fraction is defined as the number of unique 
 Friedel pairs measured divided by the number that would be 
 possible theoretically, ignoring centric projections and 
 systematic absences. 
;

_computing_data_collection       'CrysAlisPro 1.171.41.122a (Rigaku OD, 2021)'
_computing_cell_refinement       'CrysAlisPro 1.171.41.122a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.122a (Rigaku OD, 2021)'
_computing_structure_solution    'SHELXT-2018/2 (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0304P)²+1.5317P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_extinction_coef       0.00066(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         5854
_refine_ls_number_parameters     359
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0240
_refine_ls_R_factor_gt           0.0239
_refine_ls_wR_factor_ref         0.0623
_refine_ls_wR_factor_gt          0.0622
_refine_ls_goodness_of_fit_ref   1.134
_refine_ls_restrained_S_all      1.134
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
V1 V 0.72384(4) 0.60880(3) 0.79880(2) 0.01522(9) Uani 1 1 d . . . . .
O1 O 0.63752(16) 0.58229(13) 0.68562(10) 0.0186(3) Uani 1 1 d . . . . .
O2 O 0.60980(16) 0.53444(13) 0.87774(10) 0.0181(3) Uani 1 1 d . . . . .
O3 O 0.86881(17) 0.55327(14) 0.79411(11) 0.0206(3) Uani 1 1 d . . . . .
C1 C 0.6646(2) 0.51545(19) 0.60709(15) 0.0168(4) Uani 1 1 d . . . . .
C2 C 0.7737(2) 0.55280(18) 0.54946(15) 0.0176(4) Uani 1 1 d . . . . .
Br1 Br 0.89114(3) 0.69445(2) 0.58509(2) 0.02418(8) Uani 1 1 d . . . . .
C3 C 0.7958(2) 0.4907(2) 0.46476(15) 0.0197(4) Uani 1 1 d . . . . .
H3 H 0.870578 0.516566 0.426048 0.024 Uiso 1 1 calc R U . . .
C4 C 0.7055(3) 0.39008(19) 0.43847(15) 0.0197(4) Uani 1 1 d . . . . .
Br2 Br 0.72380(3) 0.31102(2) 0.31839(2) 0.02516(8) Uani 1 1 d . . . . .
C5 C 0.5983(2) 0.34908(19) 0.49510(15) 0.0187(4) Uani 1 1 d . . . . .
H5 H 0.538966 0.278881 0.475555 0.022 Uiso 1 1 calc R U . . .
C6 C 0.5776(2) 0.41068(19) 0.58052(15) 0.0171(4) Uani 1 1 d . . . . .
C7 C 0.4577(2) 0.37017(19) 0.64230(14) 0.0171(4) Uani 1 1 d . . . . .
H7A H 0.408544 0.438972 0.664659 0.020 Uiso 1 1 calc R U . . .
H7B H 0.388702 0.313273 0.605014 0.020 Uiso 1 1 calc R U . . .
N1 N 0.50707(19) 0.31424(15) 0.72304(12) 0.0150(4) Uani 1 1 d . . . . .
C8 C 0.5418(2) 0.19461(18) 0.70227(14) 0.0151(4) Uani 1 1 d . . . . .
C9 C 0.6853(2) 0.17454(19) 0.70798(14) 0.0164(4) Uani 1 1 d . . . . .
C10 C 0.7211(2) 0.0597(2) 0.68950(16) 0.0204(4) Uani 1 1 d . . . . .
H10 H 0.817590 0.045755 0.692306 0.024 Uiso 1 1 calc R U . . .
C11 C 0.6192(3) -0.0341(2) 0.66726(16) 0.0233(5) Uani 1 1 d . . . . .
H11 H 0.645297 -0.111925 0.656345 0.028 Uiso 1 1 calc R U . . .
C12 C 0.4787(3) -0.0138(2) 0.66096(16) 0.0217(5) Uani 1 1 d . . . . .
H12 H 0.408985 -0.078460 0.644917 0.026 Uiso 1 1 calc R U . . .
C13 C 0.4371(2) 0.09938(19) 0.67762(15) 0.0176(4) Uani 1 1 d . . . . .
C14 C 0.8008(2) 0.2733(2) 0.73622(16) 0.0201(4) Uani 1 1 d . . . . .
H14 H 0.755160 0.347972 0.746962 0.024 Uiso 1 1 calc R U . . .
C15 C 0.9094(3) 0.2908(2) 0.65997(18) 0.0277(5) Uani 1 1 d . . . . .
H15A H 0.956710 0.219125 0.648252 0.042 Uiso 1 1 calc R U . . .
H15B H 0.979618 0.357486 0.680319 0.042 Uiso 1 1 calc R U . . .
H15C H 0.861409 0.307162 0.602556 0.042 Uiso 1 1 calc R U . . .
C16 C 0.8750(3) 0.2531(2) 0.82797(17) 0.0264(5) Uani 1 1 d . . . . .
H16A H 0.804160 0.238654 0.875455 0.040 Uiso 1 1 calc R U . . .
H16B H 0.939681 0.323127 0.848996 0.040 Uiso 1 1 calc R U . . .
H16C H 0.928382 0.184554 0.818044 0.040 Uiso 1 1 calc R U . . .
C17 C 0.2793(2) 0.11189(19) 0.66767(15) 0.0188(4) Uani 1 1 d . . . . .
H17 H 0.265909 0.197397 0.679510 0.023 Uiso 1 1 calc R U . . .
C18 C 0.2229(3) 0.0686(2) 0.56855(17) 0.0283(5) Uani 1 1 d . . . . .
H18A H 0.232867 -0.015729 0.556206 0.043 Uiso 1 1 calc R U . . .
H18B H 0.276937 0.112736 0.523192 0.043 Uiso 1 1 calc R U . . .
H18C H 0.122984 0.081143 0.563103 0.043 Uiso 1 1 calc R U . . .
C19 C 0.1941(2) 0.0439(2) 0.73908(18) 0.0251(5) Uani 1 1 d . . . . .
H19A H 0.203150 -0.040582 0.727149 0.038 Uiso 1 1 calc R U . . .
H19B H 0.094406 0.057201 0.733579 0.038 Uiso 1 1 calc R U . . .
H19C H 0.230322 0.071776 0.802128 0.038 Uiso 1 1 calc R U . . .
C20 C 0.4276(2) 0.33340(19) 0.80876(14) 0.0165(4) Uani 1 1 d . . . . .
H20A H 0.349018 0.269618 0.809876 0.020 Uiso 1 1 calc R U . . .
H20B H 0.386299 0.409258 0.808725 0.020 Uiso 1 1 calc R U . . .
C21 C 0.5203(2) 0.33558(19) 0.89542(14) 0.0162(4) Uani 1 1 d . . . . .
C22 C 0.5145(2) 0.23955(19) 0.94913(15) 0.0170(4) Uani 1 1 d . . . . .
H22 H 0.452197 0.170537 0.931209 0.020 Uiso 1 1 calc R U . . .
C23 C 0.6000(2) 0.2449(2) 1.02883(15) 0.0192(4) Uani 1 1 d . . . . .
Br3 Br 0.58671(2) 0.11690(2) 1.10506(2) 0.02217(7) Uani 1 1 d . . . . .
C24 C 0.6939(2) 0.3425(2) 1.05611(15) 0.0189(4) Uani 1 1 d . . . . .
H24 H 0.753284 0.344112 1.109952 0.023 Uiso 1 1 calc R U . . .
C25 C 0.6995(2) 0.43780(19) 1.00326(15) 0.0170(4) Uani 1 1 d . . . . .
Br4 Br 0.82861(2) 0.57215(2) 1.03900(2) 0.02142(7) Uani 1 1 d . . . . .
C26 C 0.6118(2) 0.43703(19) 0.92427(14) 0.0163(4) Uani 1 1 d . . . . .
O4 O 0.75276(16) 0.75888(13) 0.83271(11) 0.0196(3) Uani 1 1 d . . . . .
C27 C 0.8656(2) 0.8531(2) 0.85152(17) 0.0222(5) Uani 1 1 d . . . . .
H27 H 0.876938 0.897507 0.794850 0.027 Uiso 1 1 calc R U . . .
C28 C 0.8203(3) 0.9354(3) 0.9301(2) 0.0418(7) Uani 1 1 d . . . . .
H28A H 0.729726 0.962373 0.913328 0.063 Uiso 1 1 calc R U . . .
H28B H 0.891806 1.003540 0.941587 0.063 Uiso 1 1 calc R U . . .
H28C H 0.809869 0.893728 0.986669 0.063 Uiso 1 1 calc R U . . .
C29 C 1.0038(3) 0.8063(2) 0.87200(19) 0.0273(5) Uani 1 1 d . . . . .
H29A H 0.995407 0.763589 0.928075 0.041 Uiso 1 1 calc R U . . .
H29B H 1.078556 0.872215 0.882194 0.041 Uiso 1 1 calc R U . . .
H29C H 1.027369 0.752628 0.819072 0.041 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
V1 O3 1.5791(16) . ?
V1 O4 1.7349(15) . ?
V1 O2 1.7915(15) . ?
V1 O1 1.8003(15) . ?
V1 N1 3.8229(18) . ?
O1 C1 1.352(3) . ?
O2 C26 1.352(3) . ?
C1 C2 1.395(3) . ?
C1 C6 1.403(3) . ?
C2 C3 1.387(3) . ?
C2 Br1 1.895(2) . ?
C3 C4 1.383(3) . ?
C3 H3 0.9500 . ?
C4 C5 1.386(3) . ?
C4 Br2 1.899(2) . ?
C5 C6 1.390(3) . ?
C5 H5 0.9500 . ?
C6 C7 1.517(3) . ?
C7 N1 1.469(3) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
N1 C8 1.449(3) . ?
N1 C20 1.470(3) . ?
C8 C9 1.411(3) . ?
C8 C13 1.414(3) . ?
C9 C10 1.396(3) . ?
C9 C14 1.514(3) . ?
C10 C11 1.379(3) . ?
C10 H10 0.9500 . ?
C11 C12 1.385(3) . ?
C11 H11 0.9500 . ?
C12 C13 1.396(3) . ?
C12 H12 0.9500 . ?
C13 C17 1.529(3) . ?
C14 C15 1.532(3) . ?
C14 C16 1.535(3) . ?
C14 H14 1.0000 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 C19 1.535(3) . ?
C17 C18 1.538(3) . ?
C17 H17 1.0000 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 C21 1.513(3) . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C21 C22 1.395(3) . ?
C21 C26 1.403(3) . ?
C22 C23 1.389(3) . ?
C22 H22 0.9500 . ?
C23 C24 1.379(3) . ?
C23 Br3 1.901(2) . ?
C24 C25 1.381(3) . ?
C24 H24 0.9500 . ?
C25 C26 1.399(3) . ?
C25 Br4 1.892(2) . ?
O4 C27 1.444(3) . ?
C27 C28 1.506(4) . ?
C27 C29 1.506(3) . ?
C27 H27 1.0000 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?

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
O3 V1 O4 110.25(8) . . ?
O3 V1 O2 109.66(8) . . ?
O4 V1 O2 111.01(7) . . ?
O3 V1 O1 108.46(8) . . ?
O4 V1 O1 110.85(7) . . ?
O2 V1 O1 106.50(7) . . ?
O3 V1 N1 93.24(6) . . ?
O4 V1 N1 156.51(6) . . ?
O2 V1 N1 58.59(6) . . ?
O1 V1 N1 58.89(6) . . ?
C1 O1 V1 132.88(14) . . ?
C26 O2 V1 135.81(14) . . ?
O1 C1 C2 120.6(2) . . ?
O1 C1 C6 119.8(2) . . ?
C2 C1 C6 119.5(2) . . ?
C3 C2 C1 121.6(2) . . ?
C3 C2 Br1 118.80(17) . . ?
C1 C2 Br1 119.58(16) . . ?
C4 C3 C2 117.9(2) . . ?
C4 C3 H3 121.1 . . ?
C2 C3 H3 121.1 . . ?
C3 C4 C5 122.0(2) . . ?
C3 C4 Br2 118.62(17) . . ?
C5 C4 Br2 119.34(17) . . ?
C4 C5 C6 120.0(2) . . ?
C4 C5 H5 120.0 . . ?
C6 C5 H5 120.0 . . ?
C5 C6 C1 119.0(2) . . ?
C5 C6 C7 121.1(2) . . ?
C1 C6 C7 119.83(19) . . ?
N1 C7 C6 112.48(17) . . ?
N1 C7 H7A 109.1 . . ?
C6 C7 H7A 109.1 . . ?
N1 C7 H7B 109.1 . . ?
C6 C7 H7B 109.1 . . ?
H7A C7 H7B 107.8 . . ?
C8 N1 C7 114.80(16) . . ?
C8 N1 C20 114.77(16) . . ?
C7 N1 C20 115.48(16) . . ?
C8 N1 V1 134.04(13) . . ?
C7 N1 V1 87.19(11) . . ?
C20 N1 V1 86.63(11) . . ?
C9 C8 C13 120.04(19) . . ?
C9 C8 N1 117.92(19) . . ?
C13 C8 N1 122.04(19) . . ?
C10 C9 C8 118.9(2) . . ?
C10 C9 C14 119.2(2) . . ?
C8 C9 C14 121.91(19) . . ?
C11 C10 C9 121.4(2) . . ?
C11 C10 H10 119.3 . . ?
C9 C10 H10 119.3 . . ?
C10 C11 C12 119.5(2) . . ?
C10 C11 H11 120.3 . . ?
C12 C11 H11 120.3 . . ?
C11 C12 C13 121.6(2) . . ?
C11 C12 H12 119.2 . . ?
C13 C12 H12 119.2 . . ?
C12 C13 C8 118.6(2) . . ?
C12 C13 C17 117.2(2) . . ?
C8 C13 C17 124.20(19) . . ?
C9 C14 C15 112.44(19) . . ?
C9 C14 C16 111.28(19) . . ?
C15 C14 C16 110.21(19) . . ?
C9 C14 H14 107.6 . . ?
C15 C14 H14 107.6 . . ?
C16 C14 H14 107.6 . . ?
C14 C15 H15A 109.5 . . ?
C14 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C14 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C14 C16 H16A 109.5 . . ?
C14 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C14 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C13 C17 C19 111.22(18) . . ?
C13 C17 C18 111.09(19) . . ?
C19 C17 C18 109.7(2) . . ?
C13 C17 H17 108.2 . . ?
C19 C17 H17 108.2 . . ?
C18 C17 H17 108.2 . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C17 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C17 C19 H19A 109.5 . . ?
C17 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C17 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
N1 C20 C21 111.94(17) . . ?
N1 C20 H20A 109.2 . . ?
C21 C20 H20A 109.2 . . ?
N1 C20 H20B 109.2 . . ?
C21 C20 H20B 109.2 . . ?
H20A C20 H20B 107.9 . . ?
C22 C21 C26 118.79(19) . . ?
C22 C21 C20 121.4(2) . . ?
C26 C21 C20 119.75(19) . . ?
C23 C22 C21 120.0(2) . . ?
C23 C22 H22 120.0 . . ?
C21 C22 H22 120.0 . . ?
C24 C23 C22 121.7(2) . . ?
C24 C23 Br3 118.14(16) . . ?
C22 C23 Br3 120.11(17) . . ?
C23 C24 C25 118.4(2) . . ?
C23 C24 H24 120.8 . . ?
C25 C24 H24 120.8 . . ?
C24 C25 C26 121.4(2) . . ?
C24 C25 Br4 119.04(16) . . ?
C26 C25 Br4 119.54(16) . . ?
O2 C26 C25 120.80(19) . . ?
O2 C26 C21 119.56(19) . . ?
C25 C26 C21 119.6(2) . . ?
C27 O4 V1 141.32(14) . . ?
O4 C27 C28 107.4(2) . . ?
O4 C27 C29 111.63(18) . . ?
C28 C27 C29 113.0(2) . . ?
O4 C27 H27 108.2 . . ?
C28 C27 H27 108.2 . . ?
C29 C27 H27 108.2 . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C27 C29 H29A 109.5 . . ?
C27 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C27 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 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
O3 V1 O1 C1 9.3(2) . . . . ?
O4 V1 O1 C1 130.49(19) . . . . ?
O2 V1 O1 C1 -108.64(19) . . . . ?
N1 V1 O1 C1 -73.10(18) . . . . ?
O3 V1 O2 C26 -9.1(2) . . . . ?
O4 V1 O2 C26 -131.22(19) . . . . ?
O1 V1 O2 C26 108.0(2) . . . . ?
N1 V1 O2 C26 72.35(19) . . . . ?
V1 O1 C1 C2 -76.3(3) . . . . ?
V1 O1 C1 C6 107.2(2) . . . . ?
O1 C1 C2 C3 -174.50(19) . . . . ?
C6 C1 C2 C3 2.0(3) . . . . ?
O1 C1 C2 Br1 3.4(3) . . . . ?
C6 C1 C2 Br1 179.87(15) . . . . ?
C1 C2 C3 C4 0.3(3) . . . . ?
Br1 C2 C3 C4 -177.59(16) . . . . ?
C2 C3 C4 C5 -1.8(3) . . . . ?
C2 C3 C4 Br2 174.83(16) . . . . ?
C3 C4 C5 C6 1.1(3) . . . . ?
Br2 C4 C5 C6 -175.60(16) . . . . ?
C4 C5 C6 C1 1.3(3) . . . . ?
C4 C5 C6 C7 177.8(2) . . . . ?
O1 C1 C6 C5 173.75(19) . . . . ?
C2 C1 C6 C5 -2.8(3) . . . . ?
O1 C1 C6 C7 -2.8(3) . . . . ?
C2 C1 C6 C7 -179.31(19) . . . . ?
C5 C6 C7 N1 105.3(2) . . . . ?
C1 C6 C7 N1 -78.2(2) . . . . ?
C6 C7 N1 C8 -76.6(2) . . . . ?
C6 C7 N1 C20 146.35(18) . . . . ?
C6 C7 N1 V1 61.44(16) . . . . ?
C7 N1 C8 C9 110.5(2) . . . . ?
C20 N1 C8 C9 -112.1(2) . . . . ?
V1 N1 C8 C9 -1.3(3) . . . . ?
C7 N1 C8 C13 -70.0(2) . . . . ?
C20 N1 C8 C13 67.3(2) . . . . ?
V1 N1 C8 C13 178.20(14) . . . . ?
C13 C8 C9 C10 -0.4(3) . . . . ?
N1 C8 C9 C10 179.13(18) . . . . ?
C13 C8 C9 C14 -178.60(19) . . . . ?
N1 C8 C9 C14 0.9(3) . . . . ?
C8 C9 C10 C11 -1.0(3) . . . . ?
C14 C9 C10 C11 177.3(2) . . . . ?
C9 C10 C11 C12 1.5(3) . . . . ?
C10 C11 C12 C13 -0.7(4) . . . . ?
C11 C12 C13 C8 -0.6(3) . . . . ?
C11 C12 C13 C17 179.3(2) . . . . ?
C9 C8 C13 C12 1.1(3) . . . . ?
N1 C8 C13 C12 -178.37(19) . . . . ?
C9 C8 C13 C17 -178.79(19) . . . . ?
N1 C8 C13 C17 1.7(3) . . . . ?
C10 C9 C14 C15 62.3(3) . . . . ?
C8 C9 C14 C15 -119.5(2) . . . . ?
C10 C9 C14 C16 -61.9(3) . . . . ?
C8 C9 C14 C16 116.3(2) . . . . ?
C12 C13 C17 C19 63.0(3) . . . . ?
C8 C13 C17 C19 -117.1(2) . . . . ?
C12 C13 C17 C18 -59.5(3) . . . . ?
C8 C13 C17 C18 120.4(2) . . . . ?
C8 N1 C20 C21 74.2(2) . . . . ?
C7 N1 C20 C21 -148.78(18) . . . . ?
V1 N1 C20 C21 -63.51(16) . . . . ?
N1 C20 C21 C22 -103.7(2) . . . . ?
N1 C20 C21 C26 77.9(2) . . . . ?
C26 C21 C22 C23 -0.9(3) . . . . ?
C20 C21 C22 C23 -179.36(19) . . . . ?
C21 C22 C23 C24 -1.3(3) . . . . ?
C21 C22 C23 Br3 177.32(16) . . . . ?
C22 C23 C24 C25 1.5(3) . . . . ?
Br3 C23 C24 C25 -177.16(16) . . . . ?
C23 C24 C25 C26 0.6(3) . . . . ?
C23 C24 C25 Br4 -179.53(16) . . . . ?
V1 O2 C26 C25 75.5(3) . . . . ?
V1 O2 C26 C21 -107.3(2) . . . . ?
C24 C25 C26 O2 174.38(19) . . . . ?
Br4 C25 C26 O2 -5.5(3) . . . . ?
C24 C25 C26 C21 -2.8(3) . . . . ?
Br4 C25 C26 C21 177.29(15) . . . . ?
C22 C21 C26 O2 -174.28(18) . . . . ?
C20 C21 C26 O2 4.2(3) . . . . ?
C22 C21 C26 C25 2.9(3) . . . . ?
C20 C21 C26 C25 -178.62(19) . . . . ?
O3 V1 O4 C27 6.5(2) . . . . ?
O2 V1 O4 C27 128.2(2) . . . . ?
O1 V1 O4 C27 -113.6(2) . . . . ?
N1 V1 O4 C27 -172.87(17) . . . . ?
V1 O4 C27 C28 -145.0(2) . . . . ?
V1 O4 C27 C29 -20.6(3) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
C20 H20B Br4 0.99 3.03 3.498(2) 110.1 2_667 yes
C24 H24 Br2 0.95 3.07 3.835(2) 138.4 1_556 yes
C28 H28A Br3 0.98 3.05 3.876(3) 142.4 2_667 yes
C29 H29A Br4 0.98 3.14 4.007(3) 149.0 . yes
C29 H29C O3 0.98 2.59 3.144(3) 115.7 . yes
C14 H14 O3 1.00 2.51 3.232(3) 128.7 . yes

_refine_diff_density_max         0.531
_refine_diff_density_min         -0.632
_refine_diff_density_rms         0.075

_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: acetonitrile'
####################################################################### 
# 
# 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_LH2
_database_code_depnum_ccdc_archive 'CCDC 2524169'
loop_
_audit_author_name
_audit_author_address
'Mark Elsegood'
;Loughborough University
United Kingdom
;
_audit_update_record             
;
2026-01-19 deposited with the CCDC.	2026-03-10 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2019/3
_shelx_SHELXL_version_number     2019/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C19 H23 Br2 N O'
_chemical_formula_sum            'C19 H23 Br2 N O'
_chemical_formula_weight         441.20

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'
Cl Cl 0.1484 0.1585 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

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

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

_cell_length_a                   21.4659(4)
_cell_length_b                   12.29544(18)
_cell_length_c                   14.7105(3)
_cell_angle_alpha                90
_cell_angle_beta                 106.191(2)
_cell_angle_gamma                90
_cell_volume                     3728.59(12)
_cell_formula_units_Z            8
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    33691
_cell_measurement_theta_min      2.22
_cell_measurement_theta_max      38.13

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.572
_exptl_crystal_F_000             1776
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.080
_exptl_absorpt_coefficient_mu    4.352
_shelx_estimated_absorpt_T_min   0.476
_shelx_estimated_absorpt_T_max   0.722
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.706
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   
; 
CrysAlisPro 1.171.43.128a (Rigaku Oxford Diffraction, 2024) 
Empirical absorption correction using spherical harmonics, 
implemented in SCALE3 ABSPACK scaling algorithm. 
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Rotating Anode'
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  
; 
Rigaku FRE+ equipped with Arc)Sec VHF Varimax confocal mirrors and an UG2 
goniometer and HyPix 6000HE detector 
;
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_radiation_collimation    0.2
_diffrn_detector_area_resol_mean 10
_diffrn_reflns_number            80499
_diffrn_reflns_av_unetI/netI     0.0215
_diffrn_reflns_av_R_equivalents  0.0357
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         1.976
_diffrn_reflns_theta_max         38.189
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.958
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.958
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.958
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             9858
_reflns_number_gt                7915
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
; 
 Reflections were merged by SHELXL according to the crystal 
 class for the calculation of statistics and refinement. 
  
 _reflns_Friedel_fraction is defined as the number of unique 
 Friedel pairs measured divided by the number that would be 
 possible theoretically, ignoring centric projections and 
 systematic absences. 
;

_computing_data_collection       
'CrysAlisPro system (CCD 43.127a 64-bit (release 16-06-2024))'
_computing_cell_refinement       'CrysAlisPro 1.171.43.128a (Rigaku OD, 2024)'
_computing_data_reduction        'CrysAlisPro 1.171.43.128a (Rigaku OD, 2024)'
_computing_structure_solution    'SHELXT-2018/2 (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2019/3 (Sheldrick, 2019)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0281P)²+1.0987P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         9858
_refine_ls_number_parameters     220
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0393
_refine_ls_R_factor_gt           0.0244
_refine_ls_wR_factor_ref         0.0569
_refine_ls_wR_factor_gt          0.0534
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_restrained_S_all      1.040
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
N1 N 0.60746(4) 0.69968(6) 0.32754(6) 0.01837(13) Uani 1 1 d . . . . .
H1A H 0.5918(7) 0.6867(12) 0.2675(11) 0.033(4) Uiso 1 1 d . . . . .
C1 C 0.63865(4) 0.59913(7) 0.37408(7) 0.01811(15) Uani 1 1 d . . . . .
H1B H 0.660538 0.614807 0.441442 0.022 Uiso 1 1 calc R U . . .
H1C H 0.672163 0.575563 0.343729 0.022 Uiso 1 1 calc R U . . .
C2 C 0.59054(4) 0.50776(7) 0.36824(6) 0.01519(14) Uani 1 1 d . . . . .
C3 C 0.52671(4) 0.52756(7) 0.37092(6) 0.01558(14) Uani 1 1 d . . . . .
C4 C 0.48612(4) 0.43889(7) 0.37215(6) 0.01665(14) Uani 1 1 d . . . . .
C5 C 0.50669(5) 0.33269(7) 0.36886(6) 0.01871(15) Uani 1 1 d . . . . .
H5 H 0.478500 0.273461 0.370013 0.022 Uiso 1 1 calc R U . . .
C6 C 0.56935(5) 0.31477(7) 0.36385(7) 0.01831(15) Uani 1 1 d . . . . .
C7 C 0.61123(4) 0.40095(7) 0.36435(6) 0.01729(14) Uani 1 1 d . . . . .
H7 H 0.654281 0.386966 0.362025 0.021 Uiso 1 1 calc R U . . .
O1 O 0.50318(3) 0.62952(5) 0.37262(5) 0.02015(12) Uani 1 1 d . . . . .
H1 H 0.5314(8) 0.6677(13) 0.3617(12) 0.039(4) Uiso 1 1 d . . . . .
Br1 Br 0.40044(2) 0.46468(2) 0.37768(2) 0.02047(2) Uani 1 1 d . . . . .
Br2 Br 0.59771(2) 0.17066(2) 0.35271(2) 0.02636(3) Uani 1 1 d . . . . .
C8 C 0.65079(4) 0.79203(7) 0.34443(7) 0.01895(16) Uani 1 1 d . . . . .
C9 C 0.68204(4) 0.82322(7) 0.27609(7) 0.02094(17) Uani 1 1 d . . . . .
C10 C 0.72327(5) 0.91345(8) 0.29527(8) 0.02561(19) Uani 1 1 d . . . . .
H10 H 0.744481 0.936049 0.249768 0.031 Uiso 1 1 calc R U . . .
C11 C 0.73374(5) 0.97030(8) 0.37910(9) 0.0282(2) Uani 1 1 d . . . . .
H11 H 0.762289 1.030942 0.391250 0.034 Uiso 1 1 calc R U . . .
C12 C 0.70253(5) 0.93874(8) 0.44542(8) 0.02587(19) Uani 1 1 d . . . . .
H12 H 0.709933 0.978424 0.502863 0.031 Uiso 1 1 calc R U . . .
C13 C 0.66033(4) 0.84968(7) 0.42971(7) 0.02069(16) Uani 1 1 d . . . . .
C14 C 0.66778(5) 0.76462(9) 0.18172(8) 0.02563(19) Uani 1 1 d . . . . .
H14 H 0.661777 0.685721 0.193466 0.031 Uiso 1 1 calc R U . . .
C15 C 0.60361(6) 0.80759(12) 0.11636(9) 0.0355(3) Uani 1 1 d . . . . .
H15A H 0.569753 0.803770 0.149248 0.053 Uiso 1 1 calc R U . . .
H15B H 0.590906 0.763117 0.058852 0.053 Uiso 1 1 calc R U . . .
H15C H 0.609248 0.883269 0.099314 0.053 Uiso 1 1 calc R U . . .
C16 C 0.72137(6) 0.77394(10) 0.13216(10) 0.0352(2) Uani 1 1 d . . . . .
H16A H 0.725525 0.849913 0.114572 0.053 Uiso 1 1 calc R U . . .
H16B H 0.710417 0.728637 0.075084 0.053 Uiso 1 1 calc R U . . .
H16C H 0.762544 0.749235 0.175050 0.053 Uiso 1 1 calc R U . . .
C17 C 0.62255(5) 0.82383(7) 0.50047(7) 0.02192(17) Uani 1 1 d . . . . .
H17 H 0.607013 0.746979 0.489607 0.026 Uiso 1 1 calc R U . . .
C18 C 0.56294(5) 0.89758(10) 0.48063(9) 0.0325(2) Uani 1 1 d . . . . .
H18A H 0.576857 0.973558 0.491294 0.049 Uiso 1 1 calc R U . . .
H18B H 0.536707 0.878205 0.523098 0.049 Uiso 1 1 calc R U . . .
H18C H 0.537041 0.888259 0.414771 0.049 Uiso 1 1 calc R U . . .
C19 C 0.66327(6) 0.83355(11) 0.60318(9) 0.0349(2) Uani 1 1 d . . . . .
H19A H 0.702200 0.788349 0.613160 0.052 Uiso 1 1 calc R U . . .
H19B H 0.637766 0.808947 0.645127 0.052 Uiso 1 1 calc R U . . .
H19C H 0.676009 0.909596 0.617260 0.052 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
N1 C8 1.4447(11) . ?
N1 C1 1.4799(11) . ?
N1 H1A 0.868(16) . ?
C1 C2 1.5121(12) . ?
C1 H1B 0.9900 . ?
C1 H1C 0.9900 . ?
C2 C7 1.3927(12) . ?
C2 C3 1.4029(12) . ?
C3 O1 1.3543(10) . ?
C3 C4 1.3988(12) . ?
C4 C5 1.3835(12) . ?
C4 Br1 1.8903(9) . ?
C5 C6 1.3851(13) . ?
C5 H5 0.9500 . ?
C6 C7 1.3882(12) . ?
C6 Br2 1.8955(9) . ?
C7 H7 0.9500 . ?
O1 H1 0.817(17) . ?
C8 C13 1.4053(14) . ?
C8 C9 1.4085(14) . ?
C9 C10 1.3980(13) . ?
C9 C14 1.5175(15) . ?
C10 C11 1.3804(17) . ?
C10 H10 0.9500 . ?
C11 C12 1.3840(17) . ?
C11 H11 0.9500 . ?
C12 C13 1.3987(13) . ?
C12 H12 0.9500 . ?
C13 C17 1.5207(15) . ?
C14 C16 1.5284(16) . ?
C14 C15 1.5369(16) . ?
C14 H14 1.0000 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 C19 1.5246(15) . ?
C17 C18 1.5286(15) . ?
C17 H17 1.0000 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?

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
C8 N1 C1 112.99(7) . . ?
C8 N1 H1A 111.6(10) . . ?
C1 N1 H1A 108.3(10) . . ?
N1 C1 C2 112.38(7) . . ?
N1 C1 H1B 109.1 . . ?
C2 C1 H1B 109.1 . . ?
N1 C1 H1C 109.1 . . ?
C2 C1 H1C 109.1 . . ?
H1B C1 H1C 107.9 . . ?
C7 C2 C3 119.34(8) . . ?
C7 C2 C1 118.84(8) . . ?
C3 C2 C1 121.76(8) . . ?
O1 C3 C4 118.98(8) . . ?
O1 C3 C2 122.22(8) . . ?
C4 C3 C2 118.80(8) . . ?
C5 C4 C3 121.95(8) . . ?
C5 C4 Br1 118.92(7) . . ?
C3 C4 Br1 119.13(7) . . ?
C4 C5 C6 118.43(8) . . ?
C4 C5 H5 120.8 . . ?
C6 C5 H5 120.8 . . ?
C5 C6 C7 121.02(8) . . ?
C5 C6 Br2 119.56(7) . . ?
C7 C6 Br2 119.39(7) . . ?
C6 C7 C2 120.43(8) . . ?
C6 C7 H7 119.8 . . ?
C2 C7 H7 119.8 . . ?
C3 O1 H1 103.1(11) . . ?
C13 C8 C9 121.33(8) . . ?
C13 C8 N1 118.46(8) . . ?
C9 C8 N1 120.20(9) . . ?
C10 C9 C8 118.21(10) . . ?
C10 C9 C14 121.08(9) . . ?
C8 C9 C14 120.59(8) . . ?
C11 C10 C9 121.22(10) . . ?
C11 C10 H10 119.4 . . ?
C9 C10 H10 119.4 . . ?
C10 C11 C12 119.84(9) . . ?
C10 C11 H11 120.1 . . ?
C12 C11 H11 120.1 . . ?
C11 C12 C13 121.43(10) . . ?
C11 C12 H12 119.3 . . ?
C13 C12 H12 119.3 . . ?
C12 C13 C8 117.96(9) . . ?
C12 C13 C17 119.66(9) . . ?
C8 C13 C17 122.20(8) . . ?
C9 C14 C16 114.46(9) . . ?
C9 C14 C15 109.03(10) . . ?
C16 C14 C15 109.78(9) . . ?
C9 C14 H14 107.8 . . ?
C16 C14 H14 107.8 . . ?
C15 C14 H14 107.8 . . ?
C14 C15 H15A 109.5 . . ?
C14 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C14 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C14 C16 H16A 109.5 . . ?
C14 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C14 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C13 C17 C19 113.21(9) . . ?
C13 C17 C18 108.85(8) . . ?
C19 C17 C18 111.15(10) . . ?
C13 C17 H17 107.8 . . ?
C19 C17 H17 107.8 . . ?
C18 C17 H17 107.8 . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C17 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C17 C19 H19A 109.5 . . ?
C17 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C17 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 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
C8 N1 C1 C2 171.42(8) . . . . ?
N1 C1 C2 C7 148.89(8) . . . . ?
N1 C1 C2 C3 -34.02(12) . . . . ?
C7 C2 C3 O1 -178.50(8) . . . . ?
C1 C2 C3 O1 4.42(13) . . . . ?
C7 C2 C3 C4 1.69(13) . . . . ?
C1 C2 C3 C4 -175.39(8) . . . . ?
O1 C3 C4 C5 178.84(8) . . . . ?
C2 C3 C4 C5 -1.35(13) . . . . ?
O1 C3 C4 Br1 -0.75(11) . . . . ?
C2 C3 C4 Br1 179.06(6) . . . . ?
C3 C4 C5 C6 -0.24(14) . . . . ?
Br1 C4 C5 C6 179.35(7) . . . . ?
C4 C5 C6 C7 1.50(14) . . . . ?
C4 C5 C6 Br2 -176.79(7) . . . . ?
C5 C6 C7 C2 -1.14(14) . . . . ?
Br2 C6 C7 C2 177.14(7) . . . . ?
C3 C2 C7 C6 -0.49(13) . . . . ?
C1 C2 C7 C6 176.68(8) . . . . ?
C1 N1 C8 C13 -82.03(10) . . . . ?
C1 N1 C8 C9 98.48(10) . . . . ?
C13 C8 C9 C10 0.19(13) . . . . ?
N1 C8 C9 C10 179.66(8) . . . . ?
C13 C8 C9 C14 -175.96(9) . . . . ?
N1 C8 C9 C14 3.51(13) . . . . ?
C8 C9 C10 C11 0.52(14) . . . . ?
C14 C9 C10 C11 176.65(9) . . . . ?
C9 C10 C11 C12 -0.69(16) . . . . ?
C10 C11 C12 C13 0.15(16) . . . . ?
C11 C12 C13 C8 0.54(15) . . . . ?
C11 C12 C13 C17 -174.66(9) . . . . ?
C9 C8 C13 C12 -0.70(13) . . . . ?
N1 C8 C13 C12 179.82(8) . . . . ?
C9 C8 C13 C17 174.37(8) . . . . ?
N1 C8 C13 C17 -5.11(13) . . . . ?
C10 C9 C14 C16 26.87(14) . . . . ?
C8 C9 C14 C16 -157.09(9) . . . . ?
C10 C9 C14 C15 -96.51(11) . . . . ?
C8 C9 C14 C15 79.53(11) . . . . ?
C12 C13 C17 C19 -42.79(12) . . . . ?
C8 C13 C17 C19 142.22(10) . . . . ?
C12 C13 C17 C18 81.35(11) . . . . ?
C8 C13 C17 C18 -93.64(11) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
N1 H1A O1 0.868(16) 2.560(16) 3.3399(11) 149.9(13) 2_655 yes
O1 H1 N1 0.817(17) 1.878(18) 2.6500(11) 157.0(16) . yes

_refine_diff_density_max         0.600
_refine_diff_density_min         -0.279
_refine_diff_density_rms         0.070

_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: acetonitrile'
####################################################################### 
# 
# 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_LHEt3NH
_database_code_depnum_ccdc_archive 'CCDC 2524170'
loop_
_audit_author_name
_audit_author_address
'Mark Elsegood'
;Loughborough University
United Kingdom
;
_audit_update_record             
;
2026-01-19 deposited with the CCDC.	2026-03-10 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2019/3
_shelx_SHELXL_version_number     2019/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C26 H26 Br4 N O2 1-, C6 H16 N 1+'
_chemical_formula_sum            'C32 H42 Br4 N2 O2'
_chemical_formula_weight         806.31

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.6763 1.2805 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_H-M_alt        'P 21'
_space_group_name_Hall           'P 2yb'

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

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

_cell_length_a                   11.05269(11)
_cell_length_b                   14.86773(11)
_cell_length_c                   11.54433(11)
_cell_angle_alpha                90
_cell_angle_beta                 114.9069(12)
_cell_angle_gamma                90
_cell_volume                     1720.62(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    24109
_cell_measurement_theta_min      4.21
_cell_measurement_theta_max      73.00

_exptl_crystal_description       rod
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.556
_exptl_crystal_F_000             808
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.175
_exptl_crystal_size_mid          0.043
_exptl_crystal_size_min          0.034
_exptl_absorpt_coefficient_mu    5.935
_shelx_estimated_absorpt_T_min   0.423
_shelx_estimated_absorpt_T_max   0.824
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_correction_T_min  0.612
_exptl_absorpt_correction_T_max  0.854
_exptl_absorpt_process_details   
; 
CrysAlisPro 1.171.43.98a (Rigaku Oxford Diffraction, 2023) 
Analytical numeric absorption correction using a multifaceted crystal 
model based on expressions derived by R.C. Clark & J.S. Reid. 
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) 
Empirical absorption correction using spherical harmonics, 
implemented in SCALE3 ABSPACK scaling algorithm. 
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_source                   'Rotating anode'
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  
; 
Rigaku 007HF diffractometer with HF Varimax confocal mirrors, 
an UG2 goniometer and HyPix Arc-100 detector 
;
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_radiation_collimation    0.3
_diffrn_detector_area_resol_mean 10
_diffrn_reflns_number            27863
_diffrn_reflns_av_unetI/netI     0.0273
_diffrn_reflns_av_R_equivalents  0.0321
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         4.222
_diffrn_reflns_theta_max         73.713
_diffrn_reflns_theta_full        67.679
_diffrn_measured_fraction_theta_max 0.949
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.949
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.850
_diffrn_reflns_point_group_measured_fraction_full 0.907
_reflns_number_total             5912
_reflns_number_gt                5792
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.721
_reflns_Friedel_fraction_max     0.742
_reflns_Friedel_fraction_full    0.806

_reflns_special_details          
; 
 Reflections were merged by SHELXL according to the crystal 
 class for the calculation of statistics and refinement. 
  
 _reflns_Friedel_fraction is defined as the number of unique 
 Friedel pairs measured divided by the number that would be 
 possible theoretically, ignoring centric projections and 
 systematic absences. 
;

_computing_data_collection       
'CrysAlisPro system (CCD 43.101a 64-bit (release 13-12-2023))'
_computing_cell_refinement       'CrysAlisPro 1.171.43.98a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.43.98a (Rigaku OD, 2023)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2019/3 (Sheldrick, 2019)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0213P)²+0.4885P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
; 
 Flack x determined using 2351 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). 
;
_refine_ls_abs_structure_Flack   -0.034(9)
_chemical_absolute_configuration ad
_refine_ls_number_reflns         5912
_refine_ls_number_parameters     376
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0207
_refine_ls_R_factor_gt           0.0201
_refine_ls_wR_factor_ref         0.0455
_refine_ls_wR_factor_gt          0.0452
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_restrained_S_all      1.026
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
N1 N 0.7623(3) 0.47322(18) 0.5543(2) 0.0162(5) Uani 1 1 d . . . . .
C1 C 0.6840(3) 0.5500(2) 0.5613(3) 0.0181(6) Uani 1 1 d . . . . .
H1A H 0.681929 0.595712 0.498157 0.022 Uiso 1 1 calc R U . . .
H1B H 0.727828 0.577361 0.647308 0.022 Uiso 1 1 calc R U . . .
C2 C 0.5432(3) 0.5246(2) 0.5359(3) 0.0174(6) Uani 1 1 d . . . . .
C3 C 0.4437(3) 0.5167(2) 0.4099(3) 0.0192(7) Uani 1 1 d . . . . .
C4 C 0.3128(3) 0.5000(2) 0.3933(3) 0.0212(7) Uani 1 1 d . . . . .
C5 C 0.2783(3) 0.4897(3) 0.4945(3) 0.0218(6) Uani 1 1 d . . . . .
H5 H 0.188349 0.479339 0.480501 0.026 Uiso 1 1 calc R U . . .
C6 C 0.3785(3) 0.4948(2) 0.6163(3) 0.0201(6) Uani 1 1 d . . . . .
C7 C 0.5086(3) 0.5126(2) 0.6379(3) 0.0187(6) Uani 1 1 d . . . . .
H7 H 0.575283 0.516696 0.723067 0.022 Uiso 1 1 calc R U . . .
O1 O 0.4661(3) 0.52751(18) 0.3053(2) 0.0266(6) Uani 1 1 d . . . . .
H1 H 0.551(5) 0.528(3) 0.319(4) 0.044(14) Uiso 1 1 d . . . . .
Br1 Br 0.17605(3) 0.49375(3) 0.22599(3) 0.03188(9) Uani 1 1 d . . . . .
Br2 Br 0.33200(3) 0.48617(3) 0.75668(3) 0.02791(9) Uani 1 1 d . . . . .
C8 C 0.8783(3) 0.4925(2) 0.5268(3) 0.0174(6) Uani 1 1 d . . . . .
H8A H 0.961121 0.477326 0.602686 0.021 Uiso 1 1 calc R U . . .
H8B H 0.880501 0.557557 0.509695 0.021 Uiso 1 1 calc R U . . .
C9 C 0.8738(3) 0.4396(2) 0.4133(3) 0.0175(6) Uani 1 1 d . . . . .
C10 C 0.7703(3) 0.4599(2) 0.2923(3) 0.0176(6) Uani 1 1 d . . . . .
C11 C 0.7668(3) 0.4081(2) 0.1900(3) 0.0205(7) Uani 1 1 d . . . . .
C12 C 0.8608(4) 0.3423(2) 0.2016(3) 0.0217(7) Uani 1 1 d . . . . .
H12 H 0.855694 0.309120 0.129296 0.026 Uiso 1 1 calc R U . . .
C13 C 0.9611(3) 0.3266(2) 0.3206(3) 0.0221(7) Uani 1 1 d . . . . .
C14 C 0.9678(3) 0.3741(2) 0.4270(3) 0.0200(7) Uani 1 1 d . . . . .
H14 H 1.036857 0.361610 0.508892 0.024 Uiso 1 1 calc R U . . .
O2 O 0.6841(2) 0.52462(15) 0.2789(2) 0.0194(5) Uani 1 1 d . . . . .
Br3 Br 0.62688(3) 0.42983(2) 0.02560(3) 0.02470(8) Uani 1 1 d . . . . .
Br4 Br 1.09527(4) 0.24021(3) 0.34020(4) 0.03279(10) Uani 1 1 d . . . . .
C15 C 0.7822(3) 0.4027(2) 0.6463(3) 0.0181(7) Uani 1 1 d . . . . .
C16 C 0.7130(3) 0.3216(2) 0.6035(3) 0.0224(7) Uani 1 1 d . . . . .
C17 C 0.7349(4) 0.2520(3) 0.6920(4) 0.0311(8) Uani 1 1 d . . . . .
H17 H 0.689548 0.196396 0.664434 0.037 Uiso 1 1 calc R U . . .
C18 C 0.8217(4) 0.2634(3) 0.8191(4) 0.0334(9) Uani 1 1 d . . . . .
H18 H 0.836215 0.215386 0.877756 0.040 Uiso 1 1 calc R U . . .
C19 C 0.8867(4) 0.3433(3) 0.8605(3) 0.0294(8) Uani 1 1 d . . . . .
H19 H 0.945117 0.350299 0.948183 0.035 Uiso 1 1 calc R U . . .
C20 C 0.8693(3) 0.4148(2) 0.7768(3) 0.0222(7) Uani 1 1 d . . . . .
C21 C 0.6160(3) 0.3073(2) 0.4650(4) 0.0259(7) Uani 1 1 d . . . . .
H21 H 0.606613 0.365638 0.418966 0.031 Uiso 1 1 calc R U . . .
C22 C 0.6675(4) 0.2372(3) 0.4002(4) 0.0334(8) Uani 1 1 d . . . . .
H22A H 0.753187 0.257086 0.402887 0.050 Uiso 1 1 calc R U . . .
H22B H 0.602963 0.229935 0.311057 0.050 Uiso 1 1 calc R U . . .
H22C H 0.679384 0.179578 0.444861 0.050 Uiso 1 1 calc R U . . .
C23 C 0.4777(4) 0.2805(3) 0.4549(4) 0.0346(9) Uani 1 1 d . . . . .
H23A H 0.482405 0.220420 0.491587 0.052 Uiso 1 1 calc R U . . .
H23B H 0.413735 0.279887 0.364926 0.052 Uiso 1 1 calc R U . . .
H23C H 0.448653 0.323990 0.501770 0.052 Uiso 1 1 calc R U . . .
C24 C 0.9441(3) 0.5018(3) 0.8284(3) 0.0242(7) Uani 1 1 d . . . . .
H24 H 0.923487 0.543559 0.754565 0.029 Uiso 1 1 calc R U . . .
C25 C 1.0955(3) 0.4863(3) 0.8906(3) 0.0328(8) Uani 1 1 d . . . . .
H25A H 1.119696 0.450377 0.968345 0.049 Uiso 1 1 calc R U . . .
H25B H 1.141532 0.544396 0.912378 0.049 Uiso 1 1 calc R U . . .
H25C H 1.121950 0.454217 0.830731 0.049 Uiso 1 1 calc R U . . .
C26 C 0.8988(4) 0.5476(3) 0.9228(3) 0.0307(8) Uani 1 1 d . . . . .
H26A H 0.803033 0.560474 0.879992 0.046 Uiso 1 1 calc R U . . .
H26B H 0.948071 0.603992 0.953084 0.046 Uiso 1 1 calc R U . . .
H26C H 0.916403 0.507648 0.995680 0.046 Uiso 1 1 calc R U . . .
N2 N 0.6794(3) 0.6768(2) 0.1694(3) 0.0221(6) Uani 1 1 d . . . . .
H2 H 0.674(5) 0.619(4) 0.193(5) 0.053(15) Uiso 1 1 d . . . . .
C27 C 0.7911(4) 0.7238(3) 0.2763(4) 0.0317(9) Uani 1 1 d . . . . .
H27A H 0.775484 0.719785 0.354560 0.038 Uiso 1 1 calc R U . . .
H27B H 0.789993 0.788234 0.254332 0.038 Uiso 1 1 calc R U . . .
C28 C 0.9276(4) 0.6853(3) 0.3042(4) 0.0402(10) Uani 1 1 d . . . . .
H28A H 0.925694 0.619826 0.313356 0.060 Uiso 1 1 calc R U . . .
H28B H 0.993756 0.711334 0.383632 0.060 Uiso 1 1 calc R U . . .
H28C H 0.951574 0.699789 0.233755 0.060 Uiso 1 1 calc R U . . .
C29 C 0.6957(4) 0.6741(3) 0.0465(4) 0.0315(8) Uani 1 1 d . . . . .
H29A H 0.622617 0.637617 -0.016418 0.038 Uiso 1 1 calc R U . . .
H29B H 0.780904 0.643797 0.062186 0.038 Uiso 1 1 calc R U . . .
C30 C 0.6947(6) 0.7664(3) -0.0104(4) 0.0504(12) Uani 1 1 d . . . . .
H30A H 0.609744 0.796362 -0.028382 0.076 Uiso 1 1 calc R U . . .
H30B H 0.705690 0.759722 -0.089938 0.076 Uiso 1 1 calc R U . . .
H30C H 0.768209 0.802540 0.050286 0.076 Uiso 1 1 calc R U . . .
C31 C 0.5486(4) 0.7143(3) 0.1564(4) 0.0295(8) Uani 1 1 d . . . . .
H31A H 0.545057 0.779090 0.135313 0.035 Uiso 1 1 calc R U . . .
H31B H 0.542865 0.708847 0.239349 0.035 Uiso 1 1 calc R U . . .
C32 C 0.4296(4) 0.6674(3) 0.0544(4) 0.0377(9) Uani 1 1 d . . . . .
H32A H 0.425553 0.681716 -0.030023 0.057 Uiso 1 1 calc R U . . .
H32B H 0.347600 0.687955 0.059253 0.057 Uiso 1 1 calc R U . . .
H32C H 0.438651 0.602239 0.068051 0.057 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
N1 C15 1.442(4) . ?
N1 C1 1.455(4) . ?
N1 C8 1.472(4) . ?
C1 C2 1.505(4) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 C7 1.395(4) . ?
C2 C3 1.412(4) . ?
C3 O1 1.341(4) . ?
C3 C4 1.400(4) . ?
C4 C5 1.381(4) . ?
C4 Br1 1.888(3) . ?
C5 C6 1.378(4) . ?
C5 H5 0.9500 . ?
C6 C7 1.377(4) . ?
C6 Br2 1.900(3) . ?
C7 H7 0.9500 . ?
O1 H1 0.88(5) . ?
C8 C9 1.510(4) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 C14 1.384(5) . ?
C9 C10 1.416(4) . ?
C10 O2 1.317(4) . ?
C10 C11 1.397(4) . ?
C11 C12 1.392(5) . ?
C11 Br3 1.904(3) . ?
C12 C13 1.374(5) . ?
C12 H12 0.9500 . ?
C13 C14 1.391(5) . ?
C13 Br4 1.902(3) . ?
C14 H14 0.9500 . ?
C15 C16 1.403(5) . ?
C15 C20 1.416(5) . ?
C16 C17 1.401(5) . ?
C16 C21 1.519(5) . ?
C17 C18 1.384(6) . ?
C17 H17 0.9500 . ?
C18 C19 1.367(6) . ?
C18 H18 0.9500 . ?
C19 C20 1.394(5) . ?
C19 H19 0.9500 . ?
C20 C24 1.516(5) . ?
C21 C22 1.526(5) . ?
C21 C23 1.536(5) . ?
C21 H21 1.0000 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 C25 1.535(4) . ?
C24 C26 1.538(5) . ?
C24 H24 1.0000 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
N2 C31 1.496(5) . ?
N2 C27 1.501(5) . ?
N2 C29 1.504(4) . ?
N2 H2 0.92(5) . ?
C27 C28 1.516(6) . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 C30 1.519(6) . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C31 C32 1.516(6) . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?

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
C15 N1 C1 116.0(2) . . ?
C15 N1 C8 115.1(2) . . ?
C1 N1 C8 116.9(3) . . ?
N1 C1 C2 112.5(3) . . ?
N1 C1 H1A 109.1 . . ?
C2 C1 H1A 109.1 . . ?
N1 C1 H1B 109.1 . . ?
C2 C1 H1B 109.1 . . ?
H1A C1 H1B 107.8 . . ?
C7 C2 C3 119.2(3) . . ?
C7 C2 C1 119.8(3) . . ?
C3 C2 C1 121.0(3) . . ?
O1 C3 C4 118.1(3) . . ?
O1 C3 C2 124.0(3) . . ?
C4 C3 C2 117.9(3) . . ?
C5 C4 C3 122.8(3) . . ?
C5 C4 Br1 118.2(2) . . ?
C3 C4 Br1 119.0(2) . . ?
C6 C5 C4 117.9(3) . . ?
C6 C5 H5 121.1 . . ?
C4 C5 H5 121.1 . . ?
C7 C6 C5 121.7(3) . . ?
C7 C6 Br2 119.7(2) . . ?
C5 C6 Br2 118.5(2) . . ?
C6 C7 C2 120.5(3) . . ?
C6 C7 H7 119.7 . . ?
C2 C7 H7 119.7 . . ?
C3 O1 H1 115(3) . . ?
N1 C8 C9 111.8(3) . . ?
N1 C8 H8A 109.3 . . ?
C9 C8 H8A 109.3 . . ?
N1 C8 H8B 109.3 . . ?
C9 C8 H8B 109.3 . . ?
H8A C8 H8B 107.9 . . ?
C14 C9 C10 121.2(3) . . ?
C14 C9 C8 121.2(3) . . ?
C10 C9 C8 117.6(3) . . ?
O2 C10 C11 122.8(3) . . ?
O2 C10 C9 121.0(3) . . ?
C11 C10 C9 116.1(3) . . ?
C12 C11 C10 123.5(3) . . ?
C12 C11 Br3 118.4(2) . . ?
C10 C11 Br3 118.1(2) . . ?
C13 C12 C11 118.0(3) . . ?
C13 C12 H12 121.0 . . ?
C11 C12 H12 121.0 . . ?
C12 C13 C14 121.2(3) . . ?
C12 C13 Br4 119.6(3) . . ?
C14 C13 Br4 119.2(3) . . ?
C9 C14 C13 119.8(3) . . ?
C9 C14 H14 120.1 . . ?
C13 C14 H14 120.1 . . ?
C16 C15 C20 120.6(3) . . ?
C16 C15 N1 118.3(3) . . ?
C20 C15 N1 121.1(3) . . ?
C17 C16 C15 118.5(3) . . ?
C17 C16 C21 119.5(3) . . ?
C15 C16 C21 122.0(3) . . ?
C18 C17 C16 120.8(4) . . ?
C18 C17 H17 119.6 . . ?
C16 C17 H17 119.6 . . ?
C19 C18 C17 120.3(3) . . ?
C19 C18 H18 119.9 . . ?
C17 C18 H18 119.9 . . ?
C18 C19 C20 121.4(3) . . ?
C18 C19 H19 119.3 . . ?
C20 C19 H19 119.3 . . ?
C19 C20 C15 118.3(3) . . ?
C19 C20 C24 119.0(3) . . ?
C15 C20 C24 122.7(3) . . ?
C16 C21 C22 111.6(3) . . ?
C16 C21 C23 110.8(3) . . ?
C22 C21 C23 110.5(3) . . ?
C16 C21 H21 107.9 . . ?
C22 C21 H21 107.9 . . ?
C23 C21 H21 107.9 . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C21 C23 H23A 109.5 . . ?
C21 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C21 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C20 C24 C25 111.2(3) . . ?
C20 C24 C26 111.7(3) . . ?
C25 C24 C26 110.6(3) . . ?
C20 C24 H24 107.7 . . ?
C25 C24 H24 107.7 . . ?
C26 C24 H24 107.7 . . ?
C24 C25 H25A 109.5 . . ?
C24 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C24 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C24 C26 H26A 109.5 . . ?
C24 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C24 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C31 N2 C27 109.5(3) . . ?
C31 N2 C29 114.1(3) . . ?
C27 N2 C29 113.8(3) . . ?
C31 N2 H2 102(3) . . ?
C27 N2 H2 109(3) . . ?
C29 N2 H2 108(3) . . ?
N2 C27 C28 113.5(3) . . ?
N2 C27 H27A 108.9 . . ?
C28 C27 H27A 108.9 . . ?
N2 C27 H27B 108.9 . . ?
C28 C27 H27B 108.9 . . ?
H27A C27 H27B 107.7 . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
N2 C29 C30 113.8(3) . . ?
N2 C29 H29A 108.8 . . ?
C30 C29 H29A 108.8 . . ?
N2 C29 H29B 108.8 . . ?
C30 C29 H29B 108.8 . . ?
H29A C29 H29B 107.7 . . ?
C29 C30 H30A 109.5 . . ?
C29 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C29 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
N2 C31 C32 113.1(3) . . ?
N2 C31 H31A 109.0 . . ?
C32 C31 H31A 109.0 . . ?
N2 C31 H31B 109.0 . . ?
C32 C31 H31B 109.0 . . ?
H31A C31 H31B 107.8 . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 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
C15 N1 C1 C2 -62.6(3) . . . . ?
C8 N1 C1 C2 156.6(3) . . . . ?
N1 C1 C2 C7 99.9(3) . . . . ?
N1 C1 C2 C3 -83.0(4) . . . . ?
C7 C2 C3 O1 179.5(3) . . . . ?
C1 C2 C3 O1 2.5(5) . . . . ?
C7 C2 C3 C4 2.1(5) . . . . ?
C1 C2 C3 C4 -174.9(3) . . . . ?
O1 C3 C4 C5 -178.6(3) . . . . ?
C2 C3 C4 C5 -1.1(5) . . . . ?
O1 C3 C4 Br1 0.0(4) . . . . ?
C2 C3 C4 Br1 177.5(2) . . . . ?
C3 C4 C5 C6 -1.0(6) . . . . ?
Br1 C4 C5 C6 -179.6(3) . . . . ?
C4 C5 C6 C7 2.1(6) . . . . ?
C4 C5 C6 Br2 177.2(3) . . . . ?
C5 C6 C7 C2 -1.0(5) . . . . ?
Br2 C6 C7 C2 -176.1(2) . . . . ?
C3 C2 C7 C6 -1.2(5) . . . . ?
C1 C2 C7 C6 176.0(3) . . . . ?
C15 N1 C8 C9 92.9(3) . . . . ?
C1 N1 C8 C9 -125.9(3) . . . . ?
N1 C8 C9 C14 -114.2(3) . . . . ?
N1 C8 C9 C10 66.1(4) . . . . ?
C14 C9 C10 O2 -177.4(3) . . . . ?
C8 C9 C10 O2 2.3(4) . . . . ?
C14 C9 C10 C11 2.1(5) . . . . ?
C8 C9 C10 C11 -178.3(3) . . . . ?
O2 C10 C11 C12 177.0(3) . . . . ?
C9 C10 C11 C12 -2.5(5) . . . . ?
O2 C10 C11 Br3 -2.4(4) . . . . ?
C9 C10 C11 Br3 178.2(2) . . . . ?
C10 C11 C12 C13 1.0(5) . . . . ?
Br3 C11 C12 C13 -179.6(3) . . . . ?
C11 C12 C13 C14 0.9(5) . . . . ?
C11 C12 C13 Br4 -177.8(3) . . . . ?
C10 C9 C14 C13 -0.3(5) . . . . ?
C8 C9 C14 C13 -179.9(3) . . . . ?
C12 C13 C14 C9 -1.2(5) . . . . ?
Br4 C13 C14 C9 177.5(2) . . . . ?
C1 N1 C15 C16 107.5(3) . . . . ?
C8 N1 C15 C16 -111.0(3) . . . . ?
C1 N1 C15 C20 -72.5(4) . . . . ?
C8 N1 C15 C20 69.0(4) . . . . ?
C20 C15 C16 C17 -1.8(5) . . . . ?
N1 C15 C16 C17 178.2(3) . . . . ?
C20 C15 C16 C21 178.3(3) . . . . ?
N1 C15 C16 C21 -1.7(5) . . . . ?
C15 C16 C17 C18 0.7(5) . . . . ?
C21 C16 C17 C18 -179.4(3) . . . . ?
C16 C17 C18 C19 0.6(5) . . . . ?
C17 C18 C19 C20 -0.8(6) . . . . ?
C18 C19 C20 C15 -0.3(5) . . . . ?
C18 C19 C20 C24 180.0(3) . . . . ?
C16 C15 C20 C19 1.6(5) . . . . ?
N1 C15 C20 C19 -178.4(3) . . . . ?
C16 C15 C20 C24 -178.6(3) . . . . ?
N1 C15 C20 C24 1.3(5) . . . . ?
C17 C16 C21 C22 -67.2(4) . . . . ?
C15 C16 C21 C22 112.7(4) . . . . ?
C17 C16 C21 C23 56.4(4) . . . . ?
C15 C16 C21 C23 -123.7(3) . . . . ?
C19 C20 C24 C25 59.0(4) . . . . ?
C15 C20 C24 C25 -120.8(3) . . . . ?
C19 C20 C24 C26 -65.1(4) . . . . ?
C15 C20 C24 C26 115.1(3) . . . . ?
C31 N2 C27 C28 175.3(3) . . . . ?
C29 N2 C27 C28 -55.6(4) . . . . ?
C31 N2 C29 C30 63.3(5) . . . . ?
C27 N2 C29 C30 -63.4(5) . . . . ?
C27 N2 C31 C32 -177.2(3) . . . . ?
C29 N2 C31 C32 53.8(4) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
C1 H1B Br4 0.99 3.08 3.592(3) 113.8 2_756 yes
O1 H1 O2 0.88(5) 1.73(5) 2.553(3) 156(4) . yes
N2 H2 O2 0.92(5) 1.69(5) 2.581(4) 164(5) . yes
C29 H29A Br3 0.99 3.12 3.698(4) 118.3 . yes
C31 H31A Br3 0.99 3.02 3.874(4) 145.4 2_655 yes

_refine_diff_density_max         0.664
_refine_diff_density_min         -0.404
_refine_diff_density_rms         0.048


#===END
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: acetonitrile'
####################################################################### 
# 
# 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_6
_database_code_depnum_ccdc_archive 'CCDC 2524171'
loop_
_audit_author_name
_audit_author_address
'Mark Elsegood'
;Loughborough University
United Kingdom
;
_audit_update_record             
;
2026-01-19 deposited with the CCDC.	2026-03-10 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C38 H40 Br4 N2 O3 V'
_chemical_formula_sum            'C38 H40 Br4 N2 O3 V'
_chemical_formula_weight         943.30

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
V V 0.0687 2.1097 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.6763 1.2805 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   8.68820(9)
_cell_length_b                   10.9641(2)
_cell_length_c                   11.34682(16)
_cell_angle_alpha                62.6056(16)
_cell_angle_beta                 86.1615(10)
_cell_angle_gamma                82.3521(11)
_cell_volume                     951.11(3)
_cell_formula_units_Z            1
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    23360
_cell_measurement_theta_min      4.34
_cell_measurement_theta_max      75.17

_exptl_crystal_description       block
_exptl_crystal_colour            'dark green'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.647
_exptl_crystal_F_000             469
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.060
_exptl_absorpt_coefficient_mu    7.402
_shelx_estimated_absorpt_T_min   0.319
_shelx_estimated_absorpt_T_max   0.665
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.696
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   
; 
CrysAlisPro 1.171.42.74a (Rigaku Oxford Diffraction, 2022) 
Empirical absorption correction using spherical harmonics, 
implemented in SCALE3 ABSPACK scaling algorithm. 
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_source                   'Rotating anode'
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  
; 
Rigaku 007HF diffractometer with HF Varimax confocal mirrors, 
an UG2 goniometer and HyPix 6000HE detector 
;
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_radiation_collimation    0.3
_diffrn_detector_area_resol_mean 10
_diffrn_reflns_number            32631
_diffrn_reflns_av_unetI/netI     0.0153
_diffrn_reflns_av_R_equivalents  0.0333
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         4.389
_diffrn_reflns_theta_max         70.062
_diffrn_reflns_theta_full        67.679
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measured_fraction_theta_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_point_group_measured_fraction_full 0.995
_reflns_number_total             3587
_reflns_number_gt                3463
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
; 
 Reflections were merged by SHELXL according to the crystal 
 class for the calculation of statistics and refinement. 
  
 _reflns_Friedel_fraction is defined as the number of unique 
 Friedel pairs measured divided by the number that would be 
 possible theoretically, ignoring centric projections and 
 systematic absences. 
;

_computing_data_collection       'CrysAlisPro 1.171.42.74a (Rigaku OD, 2022)'
_computing_cell_refinement       'CrysAlisPro 1.171.42.74a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.74a (Rigaku OD, 2022)'
_computing_structure_solution    'SHELXT-2018/2 (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0114P)²+2.3167P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_extinction_coef       0.00053(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         3587
_refine_ls_number_parameters     231
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0330
_refine_ls_R_factor_gt           0.0320
_refine_ls_wR_factor_ref         0.0670
_refine_ls_wR_factor_gt          0.0665
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_restrained_S_all      1.046
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
V1 V 0.45174(10) 0.52984(9) 0.47828(8) 0.01963(19) Uani 0.5 1 d . . P . .
O2 O 0.2929(4) 0.6230(4) 0.4196(4) 0.0260(8) Uani 0.5 1 d . . P . .
O1 O 0.3976(3) 0.3479(2) 0.57452(19) 0.0345(5) Uani 1 1 d . . . . .
C1 C 0.3619(3) 0.2596(3) 0.5356(3) 0.0252(6) Uani 1 1 d . . . . .
C2 C 0.2718(3) 0.1522(3) 0.6167(3) 0.0291(6) Uani 1 1 d . . . . .
Br1 Br 0.19772(5) 0.14340(4) 0.78087(3) 0.04666(12) Uani 1 1 d . . . . .
C3 C 0.2320(3) 0.0576(3) 0.5798(3) 0.0273(6) Uani 1 1 d . . . . .
H3 H 0.170883 -0.012867 0.637088 0.033 Uiso 1 1 calc R U . . .
C4 C 0.2822(3) 0.0661(3) 0.4576(3) 0.0255(6) Uani 1 1 d . . . . .
Br2 Br 0.22603(4) -0.06312(3) 0.40523(3) 0.03320(10) Uani 1 1 d . . . . .
C5 C 0.3688(3) 0.1684(3) 0.3740(3) 0.0247(6) Uani 1 1 d . . . . .
H5 H 0.402235 0.173498 0.290604 0.030 Uiso 1 1 calc R U . . .
C6 C 0.4084(3) 0.2658(3) 0.4113(3) 0.0226(5) Uani 1 1 d . . . . .
C7 C 0.4933(3) 0.3744(3) 0.3150(3) 0.0239(5) Uani 1 1 d . . . . .
H7 H 0.519164 0.370755 0.233907 0.029 Uiso 1 1 calc R U . . .
N1 N 0.5376(3) 0.4753(2) 0.3269(2) 0.0259(5) Uani 1 1 d . . . . .
C8 C 0.6179(3) 0.5697(3) 0.2091(3) 0.0243(5) Uani 1 1 d . . . . .
C9 C 0.5315(3) 0.6844(3) 0.1105(3) 0.0274(6) Uani 1 1 d . . . . .
C10 C 0.6102(4) 0.7690(3) -0.0029(3) 0.0309(6) Uani 1 1 d . . . . .
H10 H 0.554723 0.848551 -0.070401 0.037 Uiso 1 1 calc R U . . .
C11 C 0.7673(4) 0.7397(3) -0.0194(3) 0.0326(6) Uani 1 1 d . . . . .
H11 H 0.818869 0.797928 -0.098058 0.039 Uiso 1 1 calc R U . . .
C12 C 0.8492(3) 0.6252(3) 0.0790(3) 0.0315(6) Uani 1 1 d . . . . .
H12 H 0.956957 0.604787 0.066561 0.038 Uiso 1 1 calc R U . . .
C13 C 0.7774(3) 0.5393(3) 0.1959(3) 0.0265(6) Uani 1 1 d . . . . .
C14 C 0.3584(4) 0.7195(3) 0.1226(4) 0.0404(7) Uani 1 1 d . . . . .
H14 H 0.321024 0.646078 0.207853 0.048 Uiso 1 1 calc R U . . .
C15 C 0.2709(4) 0.7226(5) 0.0081(5) 0.0639(12) Uani 1 1 d . . . . .
H15A H 0.309386 0.791196 -0.076603 0.096 Uiso 1 1 calc R U . . .
H15B H 0.159651 0.747371 0.016882 0.096 Uiso 1 1 calc R U . . .
H15C H 0.287832 0.631098 0.010946 0.096 Uiso 1 1 calc R U . . .
C16 C 0.3251(4) 0.8581(4) 0.1267(4) 0.0446(8) Uani 1 1 d . . . . .
H16A H 0.383595 0.854771 0.199251 0.067 Uiso 1 1 calc R U . . .
H16B H 0.213755 0.876296 0.141221 0.067 Uiso 1 1 calc R U . . .
H16C H 0.356673 0.932120 0.042225 0.067 Uiso 1 1 calc R U . . .
C17 C 0.8734(3) 0.4166(3) 0.3035(3) 0.0336(7) Uani 1 1 d . . . . .
H17 H 0.803069 0.371268 0.380964 0.040 Uiso 1 1 calc R U . . .
C18 C 0.9373(5) 0.3103(4) 0.2573(4) 0.0529(10) Uani 1 1 d . . . . .
H18A H 0.851752 0.282048 0.226904 0.079 Uiso 1 1 calc R U . . .
H18B H 0.990570 0.229377 0.331007 0.079 Uiso 1 1 calc R U . . .
H18C H 1.010834 0.350548 0.184042 0.079 Uiso 1 1 calc R U . . .
C19 C 1.0041(5) 0.4634(4) 0.3511(4) 0.0655(12) Uani 1 1 d . . . . .
H19A H 1.054566 0.384442 0.428136 0.098 Uiso 1 1 calc R U . . .
H19B H 0.960943 0.535574 0.376043 0.098 Uiso 1 1 calc R U . . .
H19C H 1.080453 0.500159 0.279488 0.098 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
V1 V1 0.9934(17) 2_666 ?
V1 O2 1.586(4) . ?
V1 O1 1.869(2) 2_666 ?
V1 O1 1.889(2) . ?
V1 N1 2.126(2) . ?
V1 N1 2.193(2) 2_666 ?
O1 C1 1.312(3) . ?
C1 C6 1.414(4) . ?
C1 C2 1.414(4) . ?
C2 C3 1.374(4) . ?
C2 Br1 1.893(3) . ?
C3 C4 1.390(4) . ?
C3 H3 0.9500 . ?
C4 C5 1.369(4) . ?
C4 Br2 1.896(3) . ?
C5 C6 1.404(4) . ?
C5 H5 0.9500 . ?
C6 C7 1.443(4) . ?
C7 N1 1.284(4) . ?
C7 H7 0.9500 . ?
N1 C8 1.462(3) . ?
C8 C13 1.396(4) . ?
C8 C9 1.401(4) . ?
C9 C10 1.392(4) . ?
C9 C14 1.515(4) . ?
C10 C11 1.381(4) . ?
C10 H10 0.9500 . ?
C11 C12 1.381(4) . ?
C11 H11 0.9500 . ?
C12 C13 1.389(4) . ?
C12 H12 0.9500 . ?
C13 C17 1.524(4) . ?
C14 C16 1.530(5) . ?
C14 C15 1.533(5) . ?
C14 H14 1.0000 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 C18 1.515(5) . ?
C17 C19 1.527(5) . ?
C17 H17 1.0000 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?

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
V1 V1 O2 175.75(18) 2_666 . ?
V1 V1 O1 75.81(12) 2_666 2_666 ?
O2 V1 O1 105.71(16) . 2_666 ?
V1 V1 O1 73.54(12) 2_666 . ?
O2 V1 O1 104.87(16) . . ?
O1 V1 O1 149.35(6) 2_666 . ?
V1 V1 N1 80.50(12) 2_666 . ?
O2 V1 N1 103.45(15) . . ?
O1 V1 N1 87.70(9) 2_666 . ?
O1 V1 N1 87.30(9) . . ?
V1 V1 N1 72.96(11) 2_666 2_666 ?
O2 V1 N1 103.07(15) . 2_666 ?
O1 V1 N1 85.86(9) 2_666 2_666 ?
O1 V1 N1 85.26(9) . 2_666 ?
N1 V1 N1 153.47(5) . 2_666 ?
C1 O1 V1 133.72(18) . 2_666 ?
C1 O1 V1 131.67(17) . . ?
O1 C1 C6 123.0(2) . . ?
O1 C1 C2 121.1(2) . . ?
C6 C1 C2 115.9(2) . . ?
C3 C2 C1 123.0(3) . . ?
C3 C2 Br1 119.0(2) . . ?
C1 C2 Br1 118.0(2) . . ?
C2 C3 C4 119.3(3) . . ?
C2 C3 H3 120.4 . . ?
C4 C3 H3 120.4 . . ?
C5 C4 C3 120.6(2) . . ?
C5 C4 Br2 120.0(2) . . ?
C3 C4 Br2 119.5(2) . . ?
C4 C5 C6 120.2(2) . . ?
C4 C5 H5 119.9 . . ?
C6 C5 H5 119.9 . . ?
C5 C6 C1 121.1(2) . . ?
C5 C6 C7 116.8(2) . . ?
C1 C6 C7 122.1(2) . . ?
N1 C7 C6 127.2(2) . . ?
N1 C7 H7 116.4 . . ?
C6 C7 H7 116.4 . . ?
C7 N1 C8 113.4(2) . . ?
C7 N1 V1 122.70(18) . . ?
C8 N1 V1 122.02(17) . . ?
C7 N1 V1 121.25(18) . 2_666 ?
C8 N1 V1 123.26(17) . 2_666 ?
C13 C8 C9 122.1(2) . . ?
C13 C8 N1 118.8(2) . . ?
C9 C8 N1 119.0(2) . . ?
C10 C9 C8 117.7(3) . . ?
C10 C9 C14 119.3(3) . . ?
C8 C9 C14 123.0(3) . . ?
C11 C10 C9 121.4(3) . . ?
C11 C10 H10 119.3 . . ?
C9 C10 H10 119.3 . . ?
C10 C11 C12 119.6(3) . . ?
C10 C11 H11 120.2 . . ?
C12 C11 H11 120.2 . . ?
C11 C12 C13 121.5(3) . . ?
C11 C12 H12 119.3 . . ?
C13 C12 H12 119.3 . . ?
C12 C13 C8 117.8(3) . . ?
C12 C13 C17 119.6(3) . . ?
C8 C13 C17 122.6(2) . . ?
C9 C14 C16 110.3(3) . . ?
C9 C14 C15 110.8(3) . . ?
C16 C14 C15 110.7(3) . . ?
C9 C14 H14 108.3 . . ?
C16 C14 H14 108.3 . . ?
C15 C14 H14 108.3 . . ?
C14 C15 H15A 109.5 . . ?
C14 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C14 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C14 C16 H16A 109.5 . . ?
C14 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C14 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C18 C17 C13 111.5(3) . . ?
C18 C17 C19 110.8(3) . . ?
C13 C17 C19 111.3(3) . . ?
C18 C17 H17 107.7 . . ?
C13 C17 H17 107.7 . . ?
C19 C17 H17 107.7 . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C17 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C17 C19 H19A 109.5 . . ?
C17 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C17 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 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
V1 V1 O1 C1 -108.2(3) 2_666 . . . ?
O2 V1 O1 C1 75.9(3) . . . . ?
O1 V1 O1 C1 -108.2(3) 2_666 . . . ?
N1 V1 O1 C1 -27.4(3) . . . . ?
N1 V1 O1 C1 178.1(3) 2_666 . . . ?
O2 V1 O1 V1 -175.90(19) . . . 2_666 ?
O1 V1 O1 V1 -0.004(1) 2_666 . . 2_666 ?
N1 V1 O1 V1 80.89(11) . . . 2_666 ?
N1 V1 O1 V1 -73.62(11) 2_666 . . 2_666 ?
V1 O1 C1 C6 -19.0(4) 2_666 . . . ?
V1 O1 C1 C6 23.0(4) . . . . ?
V1 O1 C1 C2 161.6(2) 2_666 . . . ?
V1 O1 C1 C2 -156.3(2) . . . . ?
O1 C1 C2 C3 -180.0(3) . . . . ?
C6 C1 C2 C3 0.7(4) . . . . ?
O1 C1 C2 Br1 2.2(4) . . . . ?
C6 C1 C2 Br1 -177.12(19) . . . . ?
C1 C2 C3 C4 0.3(4) . . . . ?
Br1 C2 C3 C4 178.1(2) . . . . ?
C2 C3 C4 C5 -0.8(4) . . . . ?
C2 C3 C4 Br2 -179.4(2) . . . . ?
C3 C4 C5 C6 0.2(4) . . . . ?
Br2 C4 C5 C6 178.87(19) . . . . ?
C4 C5 C6 C1 0.8(4) . . . . ?
C4 C5 C6 C7 -177.0(2) . . . . ?
O1 C1 C6 C5 179.4(3) . . . . ?
C2 C1 C6 C5 -1.2(4) . . . . ?
O1 C1 C6 C7 -2.9(4) . . . . ?
C2 C1 C6 C7 176.5(2) . . . . ?
C5 C6 C7 N1 178.2(3) . . . . ?
C1 C6 C7 N1 0.4(4) . . . . ?
C6 C7 N1 C8 -178.5(2) . . . . ?
C6 C7 N1 V1 -13.9(4) . . . . ?
C6 C7 N1 V1 17.5(4) . . . 2_666 ?
C7 N1 C8 C13 -86.0(3) . . . . ?
V1 N1 C8 C13 109.2(3) . . . . ?
V1 N1 C8 C13 77.6(3) 2_666 . . . ?
C7 N1 C8 C9 91.2(3) . . . . ?
V1 N1 C8 C9 -73.5(3) . . . . ?
V1 N1 C8 C9 -105.1(3) 2_666 . . . ?
C13 C8 C9 C10 -0.1(4) . . . . ?
N1 C8 C9 C10 -177.3(2) . . . . ?
C13 C8 C9 C14 -180.0(3) . . . . ?
N1 C8 C9 C14 2.8(4) . . . . ?
C8 C9 C10 C11 1.4(4) . . . . ?
C14 C9 C10 C11 -178.8(3) . . . . ?
C9 C10 C11 C12 -0.9(5) . . . . ?
C10 C11 C12 C13 -0.9(5) . . . . ?
C11 C12 C13 C8 2.1(4) . . . . ?
C11 C12 C13 C17 -178.2(3) . . . . ?
C9 C8 C13 C12 -1.6(4) . . . . ?
N1 C8 C13 C12 175.7(2) . . . . ?
C9 C8 C13 C17 178.7(3) . . . . ?
N1 C8 C13 C17 -4.1(4) . . . . ?
C10 C9 C14 C16 -64.0(4) . . . . ?
C8 C9 C14 C16 115.8(3) . . . . ?
C10 C9 C14 C15 59.0(4) . . . . ?
C8 C9 C14 C15 -121.2(3) . . . . ?
C12 C13 C17 C18 -65.3(4) . . . . ?
C8 C13 C17 C18 114.4(3) . . . . ?
C12 C13 C17 C19 59.0(4) . . . . ?
C8 C13 C17 C19 -121.3(3) . . . . ?

_refine_diff_density_max         1.656
_refine_diff_density_min         -1.772
_refine_diff_density_rms         0.067

_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: acetonitrile'
####################################################################### 
# 
# 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_10
_database_code_depnum_ccdc_archive 'CCDC 2524175'
loop_
_audit_author_name
_audit_author_address
'Mark Elsegood'
;Loughborough University
United Kingdom
;
_audit_update_record             
;
2026-01-19 deposited with the CCDC.	2026-03-10 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2019/3
_shelx_SHELXL_version_number     2019/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C38 H43 I4 N2 O3 V, 0.5(C2 H3 N)'
_chemical_formula_sum            'C39 H44.50 I4 N2.50 O3 V'
_chemical_formula_weight         1154.81

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
V V 0.0687 2.1097 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.3257 6.8362 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

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

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

_cell_length_a                   25.3991(6)
_cell_length_b                   12.4635(3)
_cell_length_c                   27.4973(8)
_cell_angle_alpha                90
_cell_angle_beta                 106.109(3)
_cell_angle_gamma                90
_cell_volume                     8362.8(4)
_cell_formula_units_Z            8
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    43357
_cell_measurement_theta_min      1.83
_cell_measurement_theta_max      69.82

_exptl_crystal_description       plate
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.834
_exptl_crystal_F_000             4440
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.052
_exptl_crystal_size_mid          0.043
_exptl_crystal_size_min          0.005
_exptl_absorpt_coefficient_mu    25.463
_shelx_estimated_absorpt_T_min   0.351
_shelx_estimated_absorpt_T_max   0.883
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_correction_T_min  0.356
_exptl_absorpt_correction_T_max  0.893
_exptl_absorpt_process_details   
; 
CrysAlisPro 1.171.43.130a (Rigaku Oxford Diffraction, 2024) 
Numerical absorption correction based on gaussian integration over 
a multifaceted crystal model 
Empirical absorption correction using spherical harmonics, 
implemented in SCALE3 ABSPACK scaling algorithm. 
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_source                   'Rotating anode'
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  
; 
Rigaku 007HF diffractometer with HF Varimax confocal mirrors, 
an UG2 goniometer and HyPix Arc-100 detector 
;
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_radiation_collimation    0.3
_diffrn_detector_area_resol_mean 10
_diffrn_reflns_number            135095
_diffrn_reflns_av_unetI/netI     0.0498
_diffrn_reflns_av_R_equivalents  0.0894
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_theta_min         1.810
_diffrn_reflns_theta_max         71.000
_diffrn_reflns_theta_full        67.679
_diffrn_measured_fraction_theta_max 0.961
_diffrn_measured_fraction_theta_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.961
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.961
_diffrn_reflns_point_group_measured_fraction_full 0.992
_reflns_number_total             15531
_reflns_number_gt                12215
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
; 
 Reflections were merged by SHELXL according to the crystal 
 class for the calculation of statistics and refinement. 
  
 _reflns_Friedel_fraction is defined as the number of unique 
 Friedel pairs measured divided by the number that would be 
 possible theoretically, ignoring centric projections and 
 systematic absences. 
;

_computing_data_collection       
'CrysAlisPro system (CCD 43.127a 64-bit (release 16-06-2024))'
_computing_cell_refinement       'CrysAlisPro 1.171.43.130a (Rigaku OD, 2024)'
_computing_data_reduction        'CrysAlisPro 1.171.43.130a (Rigaku OD, 2024)'
_computing_structure_solution    'SHELXT-2018/2 (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2019/3 (Sheldrick, 2019)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0288P)²+58.7809P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     'SHELXL-2019/3 (Sheldrick 2019)'
_refine_ls_extinction_coef       0.000010(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         15531
_refine_ls_number_parameters     910
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0680
_refine_ls_R_factor_gt           0.0463
_refine_ls_wR_factor_ref         0.1005
_refine_ls_wR_factor_gt          0.0920
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_restrained_S_all      1.022
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
V1 V 0.90634(4) 0.52741(8) 0.60982(4) 0.0181(2) Uani 1 1 d . . . . .
O3 O 0.90539(17) 0.5678(3) 0.66478(16) 0.0243(10) Uani 1 1 d . . . . .
O1 O 0.84268(16) 0.4724(3) 0.56475(16) 0.0221(10) Uani 1 1 d . . . . .
C1 C 0.8306(2) 0.3693(5) 0.5523(2) 0.0212(14) Uani 1 1 d . . . . .
C2 C 0.7755(3) 0.3357(5) 0.5358(3) 0.0254(15) Uani 1 1 d . . . . .
I1 I 0.71340(2) 0.44540(4) 0.53843(2) 0.04287(14) Uani 1 1 d . . . . .
C3 C 0.7617(3) 0.2308(5) 0.5215(2) 0.0236(15) Uani 1 1 d . . . . .
H3 H 0.724231 0.210311 0.509825 0.028 Uiso 1 1 calc R U . . .
C4 C 0.8025(3) 0.1557(5) 0.5242(2) 0.0227(14) Uani 1 1 d . . . . .
I2 I 0.78114(2) -0.00382(3) 0.50409(2) 0.02990(11) Uani 1 1 d . . . . .
C5 C 0.8575(3) 0.1844(5) 0.5433(2) 0.0214(14) Uani 1 1 d . . . . .
H5 H 0.885573 0.131992 0.547093 0.026 Uiso 1 1 calc R U . . .
C6 C 0.8708(2) 0.2910(5) 0.5567(2) 0.0191(13) Uani 1 1 d . . . . .
C7 C 0.9300(2) 0.3230(5) 0.5809(2) 0.0212(14) Uani 1 1 d . . . . .
H7A H 0.952904 0.257974 0.590745 0.025 Uiso 1 1 calc R U . . .
H7B H 0.944170 0.364058 0.556345 0.025 Uiso 1 1 calc R U . . .
N1 N 0.93287(19) 0.3894(4) 0.62600(19) 0.0190(11) Uani 1 1 d . . . . .
C8 C 0.9506(2) 0.3379(5) 0.6751(2) 0.0200(14) Uani 1 1 d . . . . .
C9 C 0.9129(3) 0.2978(5) 0.6985(2) 0.0243(15) Uani 1 1 d . . . . .
C10 C 0.9332(3) 0.2517(6) 0.7464(3) 0.0340(17) Uani 1 1 d . . . . .
H10 H 0.908328 0.223582 0.763408 0.041 Uiso 1 1 calc R U . . .
C11 C 0.9892(3) 0.2464(6) 0.7695(3) 0.0406(19) Uani 1 1 d . . . . .
H11 H 1.002173 0.215007 0.802175 0.049 Uiso 1 1 calc R U . . .
C12 C 1.0264(3) 0.2866(6) 0.7453(3) 0.0368(18) Uani 1 1 d . . . . .
H12 H 1.064632 0.281651 0.761337 0.044 Uiso 1 1 calc R U . . .
C13 C 1.0080(3) 0.3338(5) 0.6979(3) 0.0273(15) Uani 1 1 d . . . . .
C14 C 0.8509(3) 0.3045(6) 0.6760(3) 0.0289(16) Uani 1 1 d . . . . .
H14 H 0.844084 0.336703 0.641509 0.035 Uiso 1 1 calc R U . . .
C15 C 0.8251(3) 0.3783(6) 0.7066(3) 0.0415(19) Uani 1 1 d . . . . .
H15A H 0.828664 0.346621 0.739992 0.062 Uiso 1 1 calc R U . . .
H15B H 0.786183 0.388117 0.688952 0.062 Uiso 1 1 calc R U . . .
H15C H 0.843638 0.448054 0.710712 0.062 Uiso 1 1 calc R U . . .
C16 C 0.8245(3) 0.1934(7) 0.6694(3) 0.047(2) Uani 1 1 d . . . . .
H16A H 0.841518 0.148713 0.648673 0.071 Uiso 1 1 calc R U . . .
H16B H 0.785182 0.200291 0.652709 0.071 Uiso 1 1 calc R U . . .
H16C H 0.829769 0.159918 0.702695 0.071 Uiso 1 1 calc R U . . .
C17 C 1.0484(3) 0.3822(6) 0.6727(3) 0.0290(16) Uani 1 1 d . . . . .
H17 H 1.027964 0.398086 0.636809 0.035 Uiso 1 1 calc R U . . .
C18 C 1.0957(3) 0.3083(7) 0.6719(3) 0.043(2) Uani 1 1 d . . . . .
H18A H 1.116168 0.289970 0.706690 0.065 Uiso 1 1 calc R U . . .
H18B H 1.120149 0.344662 0.655173 0.065 Uiso 1 1 calc R U . . .
H18C H 1.081431 0.242574 0.653342 0.065 Uiso 1 1 calc R U . . .
C19 C 1.0698(3) 0.4896(6) 0.6984(3) 0.043(2) Uani 1 1 d . . . . .
H19A H 1.038858 0.537525 0.697049 0.065 Uiso 1 1 calc R U . . .
H19B H 1.094172 0.523026 0.680657 0.065 Uiso 1 1 calc R U . . .
H19C H 1.090135 0.476710 0.733785 0.065 Uiso 1 1 calc R U . . .
O2 O 0.96687(16) 0.5695(3) 0.58711(18) 0.0242(10) Uani 1 1 d . . . . .
C20 C 0.9875(2) 0.6614(5) 0.5760(2) 0.0211(14) Uani 1 1 d . . . . .
C21 C 1.0361(2) 0.6610(5) 0.5607(2) 0.0216(14) Uani 1 1 d . . . . .
I3 I 1.07363(2) 0.51439(3) 0.55354(2) 0.02854(11) Uani 1 1 d . . . . .
C22 C 1.0611(3) 0.7547(5) 0.5518(2) 0.0258(15) Uani 1 1 d . . . . .
H22 H 1.093589 0.752248 0.541196 0.031 Uiso 1 1 calc R U . . .
C23 C 1.0381(3) 0.8517(5) 0.5587(3) 0.0247(15) Uani 1 1 d . . . . .
I4 I 1.07996(2) 0.99467(4) 0.55278(2) 0.03866(13) Uani 1 1 d . . . . .
C24 C 0.9883(2) 0.8559(5) 0.5701(2) 0.0241(15) Uani 1 1 d . . . . .
H24 H 0.971572 0.923068 0.572681 0.029 Uiso 1 1 calc R U . . .
C25 C 0.9632(2) 0.7613(5) 0.5778(2) 0.0210(14) Uani 1 1 d . . . . .
C26 C 0.9088(3) 0.7704(6) 0.5877(5) 0.063(3) Uani 1 1 d . . . . .
H26A H 0.914703 0.782727 0.624428 0.076 Uiso 1 1 calc R U . . .
H26B H 0.890072 0.834632 0.569800 0.076 Uiso 1 1 calc R U . . .
N2 N 0.87348(18) 0.6823(4) 0.57343(19) 0.0157(11) Uani 1 1 d . . . . .
H2 H 0.878278 0.669358 0.539025 0.019 Uiso 1 1 calc R U . . .
C27 C 0.8148(2) 0.7079(5) 0.5587(2) 0.0160(13) Uani 1 1 d . . . . .
C28 C 0.7862(2) 0.6953(5) 0.5074(2) 0.0189(13) Uani 1 1 d . . . . .
C29 C 0.7301(3) 0.7206(5) 0.4931(3) 0.0260(15) Uani 1 1 d . . . . .
H29 H 0.709732 0.713963 0.458599 0.031 Uiso 1 1 calc R U . . .
C30 C 0.7043(3) 0.7543(5) 0.5276(3) 0.0283(16) Uani 1 1 d . . . . .
H30 H 0.666342 0.771228 0.517003 0.034 Uiso 1 1 calc R U . . .
C31 C 0.7329(2) 0.7639(5) 0.5776(3) 0.0244(15) Uani 1 1 d . . . . .
H31 H 0.714030 0.785419 0.601401 0.029 Uiso 1 1 calc R U . . .
C32 C 0.7891(2) 0.7429(5) 0.5945(2) 0.0191(13) Uani 1 1 d . . . . .
C33 C 0.8146(3) 0.6579(6) 0.4687(2) 0.0272(15) Uani 1 1 d . . . . .
H33 H 0.844170 0.607138 0.486510 0.033 Uiso 1 1 calc R U . . .
C34 C 0.7763(3) 0.5959(9) 0.4249(3) 0.071(3) Uani 1 1 d . . . . .
H34A H 0.758682 0.537530 0.438388 0.107 Uiso 1 1 calc R U . . .
H34B H 0.797543 0.566028 0.403281 0.107 Uiso 1 1 calc R U . . .
H34C H 0.748221 0.644566 0.404929 0.107 Uiso 1 1 calc R U . . .
C35 C 0.8420(4) 0.7488(7) 0.4489(3) 0.057(3) Uani 1 1 d . . . . .
H35A H 0.814146 0.799072 0.430008 0.086 Uiso 1 1 calc R U . . .
H35B H 0.862563 0.719964 0.426434 0.086 Uiso 1 1 calc R U . . .
H35C H 0.867208 0.786206 0.477310 0.086 Uiso 1 1 calc R U . . .
C36 C 0.8185(3) 0.7592(7) 0.6499(3) 0.0359(18) Uani 1 1 d . . . . .
H36 H 0.857858 0.739096 0.655333 0.043 Uiso 1 1 calc R U . . .
C37 C 0.7945(3) 0.6866(8) 0.6826(3) 0.056(3) Uani 1 1 d . . . . .
H37A H 0.756738 0.708444 0.679774 0.084 Uiso 1 1 calc R U . . .
H37B H 0.816480 0.692359 0.717960 0.084 Uiso 1 1 calc R U . . .
H37C H 0.794901 0.612197 0.671195 0.084 Uiso 1 1 calc R U . . .
C38 C 0.8162(4) 0.8782(7) 0.6648(3) 0.055(3) Uani 1 1 d . . . . .
H38A H 0.832593 0.922904 0.643620 0.082 Uiso 1 1 calc R U . . .
H38B H 0.836489 0.887682 0.700478 0.082 Uiso 1 1 calc R U . . .
H38C H 0.777885 0.899473 0.659887 0.082 Uiso 1 1 calc R U . . .
V2 V 0.62313(4) 0.85911(9) 0.68893(4) 0.0231(2) Uani 1 1 d . . . . .
O6 O 0.66362(18) 0.7804(4) 0.67165(17) 0.0310(11) Uani 1 1 d . . . . .
O4 O 0.64376(18) 1.0041(4) 0.70094(17) 0.0295(11) Uani 1 1 d . . . . .
C39 C 0.6841(3) 1.0597(6) 0.7325(2) 0.0261(15) Uani 1 1 d . . . . .
C40 C 0.6848(3) 1.1711(6) 0.7295(3) 0.0287(16) Uani 1 1 d . . . . .
I5 I 0.61986(2) 1.25157(4) 0.67807(2) 0.04278(14) Uani 1 1 d . . . . .
C41 C 0.7259(3) 1.2317(6) 0.7608(3) 0.0332(17) Uani 1 1 d . . . . .
H41 H 0.725725 1.307616 0.757720 0.040 Uiso 1 1 calc R U . . .
C42 C 0.7677(3) 1.1805(6) 0.7970(3) 0.0309(16) Uani 1 1 d . . . . .
I6 I 0.82793(2) 1.27107(4) 0.84718(2) 0.04431(14) Uani 1 1 d . . . . .
C43 C 0.7674(3) 1.0708(6) 0.8016(3) 0.0278(16) Uani 1 1 d . . . . .
H43 H 0.795724 1.036390 0.826691 0.033 Uiso 1 1 calc R U . . .
C44 C 0.7264(3) 1.0099(6) 0.7702(3) 0.0274(15) Uani 1 1 d . . . . .
C45 C 0.7262(3) 0.8900(6) 0.7765(3) 0.0350(18) Uani 1 1 d . . . . .
H45A H 0.740428 0.855290 0.750297 0.042 Uiso 1 1 calc R U . . .
H45B H 0.750395 0.869962 0.810107 0.042 Uiso 1 1 calc R U . . .
N3 N 0.6690(2) 0.8514(4) 0.77169(19) 0.0216(12) Uani 1 1 d . . . . .
H3A H 0.653432 0.915259 0.784800 0.026 Uiso 1 1 calc R U . . .
C46 C 0.6628(3) 0.7700(5) 0.8074(2) 0.0238(15) Uani 1 1 d . . . . .
C47 C 0.6894(3) 0.6696(6) 0.8102(3) 0.0288(16) Uani 1 1 d . . . . .
C48 C 0.6851(3) 0.5987(6) 0.8485(3) 0.0328(17) Uani 1 1 d . . . . .
H48 H 0.702738 0.530894 0.851181 0.039 Uiso 1 1 calc R U . . .
C49 C 0.6563(3) 0.6243(6) 0.8821(3) 0.0321(17) Uani 1 1 d . . . . .
H49 H 0.655294 0.576127 0.908600 0.039 Uiso 1 1 calc R U . . .
C50 C 0.6285(3) 0.7207(6) 0.8773(3) 0.0296(16) Uani 1 1 d . . . . .
H50 H 0.607902 0.737144 0.900294 0.036 Uiso 1 1 calc R U . . .
C51 C 0.6299(3) 0.7943(6) 0.8398(2) 0.0260(15) Uani 1 1 d . . . . .
C52 C 0.7198(3) 0.6321(6) 0.7735(3) 0.0359(18) Uani 1 1 d . . . . .
H52 H 0.722265 0.693853 0.751050 0.043 Uiso 1 1 calc R U . . .
C53 C 0.6874(4) 0.5428(7) 0.7404(3) 0.053(2) Uani 1 1 d . . . . .
H53A H 0.683844 0.481697 0.761740 0.080 Uiso 1 1 calc R U . . .
H53B H 0.706589 0.520018 0.715819 0.080 Uiso 1 1 calc R U . . .
H53C H 0.650813 0.569326 0.722446 0.080 Uiso 1 1 calc R U . . .
C54 C 0.7779(3) 0.5962(7) 0.8005(3) 0.050(2) Uani 1 1 d . . . . .
H54A H 0.798001 0.655822 0.820547 0.075 Uiso 1 1 calc R U . . .
H54B H 0.796575 0.573873 0.775394 0.075 Uiso 1 1 calc R U . . .
H54C H 0.776552 0.535730 0.822917 0.075 Uiso 1 1 calc R U . . .
C55 C 0.5979(3) 0.8981(6) 0.8367(3) 0.0324(17) Uani 1 1 d . . . . .
H55 H 0.591730 0.926851 0.801600 0.039 Uiso 1 1 calc R U . . .
C56 C 0.6304(3) 0.9811(6) 0.8727(3) 0.049(2) Uani 1 1 d . . . . .
H56A H 0.639674 0.953029 0.907345 0.073 Uiso 1 1 calc R U . . .
H56B H 0.608359 1.046443 0.870646 0.073 Uiso 1 1 calc R U . . .
H56C H 0.664075 0.997843 0.863542 0.073 Uiso 1 1 calc R U . . .
C57 C 0.5412(3) 0.8797(7) 0.8454(3) 0.049(2) Uani 1 1 d . . . . .
H57A H 0.522184 0.821787 0.823279 0.073 Uiso 1 1 calc R U . . .
H57B H 0.519516 0.945753 0.837573 0.073 Uiso 1 1 calc R U . . .
H57C H 0.545732 0.859946 0.880806 0.073 Uiso 1 1 calc R U . . .
O5 O 0.56909(17) 0.7977(4) 0.71416(16) 0.0251(10) Uani 1 1 d . . . . .
C58 C 0.5140(3) 0.7969(5) 0.6931(2) 0.0218(14) Uani 1 1 d . . . . .
C59 C 0.4816(3) 0.7227(5) 0.7092(2) 0.0264(15) Uani 1 1 d . . . . .
I7 I 0.51926(2) 0.60442(4) 0.76127(2) 0.03593(12) Uani 1 1 d . . . . .
C60 C 0.4245(3) 0.7229(6) 0.6887(3) 0.0330(17) Uani 1 1 d . . . . .
H60 H 0.402239 0.674106 0.700676 0.040 Uiso 1 1 calc R U . . .
C61 C 0.4015(3) 0.7948(6) 0.6512(3) 0.0304(16) Uani 1 1 d . . . . .
I8 I 0.31619(2) 0.78980(4) 0.61739(2) 0.03898(13) Uani 1 1 d . . . . .
C62 C 0.4329(3) 0.8670(5) 0.6334(3) 0.0278(15) Uani 1 1 d . . . . .
H62 H 0.415788 0.914758 0.606796 0.033 Uiso 1 1 calc R U . . .
C63 C 0.4895(3) 0.8706(5) 0.6541(3) 0.0264(15) Uani 1 1 d . . . . .
C64 C 0.5255(3) 0.9466(6) 0.6355(3) 0.0252(15) Uani 1 1 d . . . . .
H64A H 0.504378 0.979764 0.603249 0.030 Uiso 1 1 calc R U . . .
H64B H 0.538450 1.004516 0.660585 0.030 Uiso 1 1 calc R U . . .
N4 N 0.5730(2) 0.8879(4) 0.6276(2) 0.0237(12) Uani 1 1 d . . . . .
C65 C 0.5688(2) 0.8593(6) 0.5751(2) 0.0249(15) Uani 1 1 d . . . . .
C66 C 0.5793(3) 0.9415(6) 0.5438(3) 0.0291(16) Uani 1 1 d . . . . .
C67 C 0.5693(3) 0.9176(7) 0.4922(3) 0.0387(19) Uani 1 1 d . . . . .
H67 H 0.574904 0.971494 0.469735 0.046 Uiso 1 1 calc R U . . .
C68 C 0.5515(3) 0.8181(8) 0.4736(3) 0.043(2) Uani 1 1 d . . . . .
H68 H 0.543963 0.804562 0.438345 0.051 Uiso 1 1 calc R U . . .
C69 C 0.5444(3) 0.7381(7) 0.5052(3) 0.040(2) Uani 1 1 d . . . . .
H69 H 0.533400 0.668837 0.491750 0.048 Uiso 1 1 calc R U . . .
C70 C 0.5533(3) 0.7569(6) 0.5574(3) 0.0312(16) Uani 1 1 d . . . . .
C71 C 0.6045(3) 1.0476(6) 0.5654(3) 0.0328(17) Uani 1 1 d . . . . .
H71 H 0.588468 1.068045 0.593468 0.039 Uiso 1 1 calc R U . . .
C72 C 0.6672(3) 1.0359(7) 0.5882(3) 0.0397(19) Uani 1 1 d . . . . .
H72A H 0.674777 0.979294 0.613927 0.060 Uiso 1 1 calc R U . . .
H72B H 0.682472 1.103975 0.603782 0.060 Uiso 1 1 calc R U . . .
H72C H 0.684080 1.017196 0.561322 0.060 Uiso 1 1 calc R U . . .
C73 C 0.5940(3) 1.1400(7) 0.5272(3) 0.051(2) Uani 1 1 d . . . . .
H73A H 0.612833 1.125427 0.501252 0.077 Uiso 1 1 calc R U . . .
H73B H 0.608008 1.207021 0.544748 0.077 Uiso 1 1 calc R U . . .
H73C H 0.554581 1.146711 0.511257 0.077 Uiso 1 1 calc R U . . .
C74 C 0.5445(3) 0.6647(6) 0.5904(3) 0.0411(19) Uani 1 1 d . . . . .
H74 H 0.551027 0.692809 0.625679 0.049 Uiso 1 1 calc R U . . .
C75 C 0.5865(4) 0.5745(8) 0.5919(4) 0.068(3) Uani 1 1 d . . . . .
H75A H 0.581701 0.546625 0.557581 0.101 Uiso 1 1 calc R U . . .
H75B H 0.580775 0.516478 0.613911 0.101 Uiso 1 1 calc R U . . .
H75C H 0.623685 0.603083 0.605004 0.101 Uiso 1 1 calc R U . . .
C76 C 0.4858(4) 0.6232(8) 0.5733(4) 0.064(3) Uani 1 1 d . . . . .
H76A H 0.460339 0.682061 0.573790 0.096 Uiso 1 1 calc R U . . .
H76B H 0.480955 0.566282 0.596352 0.096 Uiso 1 1 calc R U . . .
H76C H 0.478253 0.594429 0.538926 0.096 Uiso 1 1 calc R U . . .
N5 N 1.0465(4) 0.5547(8) 0.8583(3) 0.092(4) Uani 1 1 d . . . . .
C77 C 1.0063(5) 0.5388(7) 0.8293(4) 0.060(3) Uani 1 1 d . . . . .
C78 C 0.9541(4) 0.5189(7) 0.7923(3) 0.061(3) Uani 1 1 d . . . . .
H78A H 0.937255 0.587460 0.778952 0.091 Uiso 1 1 calc R U . . .
H78B H 0.929858 0.480365 0.808485 0.091 Uiso 1 1 calc R U . . .
H78C H 0.959983 0.475583 0.764554 0.091 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
V1 O3 1.599(4) . ?
V1 N1 1.856(5) . ?
V1 O1 1.873(4) . ?
V1 O2 1.887(4) . ?
V1 N2 2.228(5) . ?
O1 C1 1.344(7) . ?
C1 C6 1.392(8) . ?
C1 C2 1.409(8) . ?
C2 C3 1.383(9) . ?
C2 I1 2.104(6) . ?
C3 C4 1.384(9) . ?
C3 H3 0.9500 . ?
C4 C5 1.396(8) . ?
C4 I2 2.094(6) . ?
C5 C6 1.396(8) . ?
C5 H5 0.9500 . ?
C6 C7 1.520(8) . ?
C7 N1 1.477(8) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
N1 C8 1.450(8) . ?
C8 C9 1.386(9) . ?
C8 C13 1.420(9) . ?
C9 C10 1.398(9) . ?
C9 C14 1.526(9) . ?
C10 C11 1.389(10) . ?
C10 H10 0.9500 . ?
C11 C12 1.393(11) . ?
C11 H11 0.9500 . ?
C12 C13 1.388(10) . ?
C12 H12 0.9500 . ?
C13 C17 1.512(10) . ?
C14 C15 1.514(10) . ?
C14 C16 1.528(10) . ?
C14 H14 1.0000 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 C18 1.521(9) . ?
C17 C19 1.541(10) . ?
C17 H17 1.0000 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
O2 C20 1.331(7) . ?
C20 C25 1.397(9) . ?
C20 C21 1.410(9) . ?
C21 C22 1.382(9) . ?
C21 I3 2.096(6) . ?
C22 C23 1.378(9) . ?
C22 H22 0.9500 . ?
C23 C24 1.387(9) . ?
C23 I4 2.104(6) . ?
C24 C25 1.385(9) . ?
C24 H24 0.9500 . ?
C25 C26 1.485(9) . ?
C26 N2 1.402(9) . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
N2 C27 1.468(7) . ?
N2 H2 1.0000 . ?
C27 C32 1.393(9) . ?
C27 C28 1.407(8) . ?
C28 C29 1.404(8) . ?
C28 C33 1.513(9) . ?
C29 C30 1.361(10) . ?
C29 H29 0.9500 . ?
C30 C31 1.371(9) . ?
C30 H30 0.9500 . ?
C31 C32 1.399(8) . ?
C31 H31 0.9500 . ?
C32 C36 1.511(9) . ?
C33 C35 1.509(11) . ?
C33 C34 1.532(10) . ?
C33 H33 1.0000 . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
C36 C37 1.517(11) . ?
C36 C38 1.545(11) . ?
C36 H36 1.0000 . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?
V2 O6 1.587(5) . ?
V2 N4 1.845(5) . ?
V2 O5 1.865(4) . ?
V2 O4 1.885(5) . ?
V2 N3 2.253(5) . ?
O4 C39 1.339(8) . ?
C39 C40 1.391(9) . ?
C39 C44 1.412(9) . ?
C40 C41 1.380(10) . ?
C40 I5 2.106(6) . ?
C41 C42 1.391(10) . ?
C41 H41 0.9500 . ?
C42 C43 1.373(10) . ?
C42 I6 2.085(7) . ?
C43 C44 1.381(9) . ?
C43 H43 0.9500 . ?
C44 C45 1.505(9) . ?
C45 N3 1.500(8) . ?
C45 H45A 0.9900 . ?
C45 H45B 0.9900 . ?
N3 C46 1.451(8) . ?
N3 H3A 1.0000 . ?
C46 C47 1.413(9) . ?
C46 C51 1.414(9) . ?
C47 C48 1.402(10) . ?
C47 C52 1.505(10) . ?
C48 C49 1.366(10) . ?
C48 H48 0.9500 . ?
C49 C50 1.380(10) . ?
C49 H49 0.9500 . ?
C50 C51 1.388(10) . ?
C50 H50 0.9500 . ?
C51 C55 1.516(10) . ?
C52 C54 1.524(10) . ?
C52 C53 1.527(11) . ?
C52 H52 1.0000 . ?
C53 H53A 0.9800 . ?
C53 H53B 0.9800 . ?
C53 H53C 0.9800 . ?
C54 H54A 0.9800 . ?
C54 H54B 0.9800 . ?
C54 H54C 0.9800 . ?
C55 C56 1.509(10) . ?
C55 C57 1.543(10) . ?
C55 H55 1.0000 . ?
C56 H56A 0.9800 . ?
C56 H56B 0.9800 . ?
C56 H56C 0.9800 . ?
C57 H57A 0.9800 . ?
C57 H57B 0.9800 . ?
C57 H57C 0.9800 . ?
O5 C58 1.359(7) . ?
C58 C59 1.389(9) . ?
C58 C63 1.418(9) . ?
C59 C60 1.402(9) . ?
C59 I7 2.092(6) . ?
C60 C61 1.369(10) . ?
C60 H60 0.9500 . ?
C61 C62 1.379(10) . ?
C61 I8 2.108(6) . ?
C62 C63 1.391(9) . ?
C62 H62 0.9500 . ?
C63 C64 1.503(9) . ?
C64 N4 1.477(8) . ?
C64 H64A 0.9900 . ?
C64 H64B 0.9900 . ?
N4 C65 1.462(8) . ?
C65 C70 1.385(10) . ?
C65 C66 1.410(10) . ?
C66 C67 1.401(10) . ?
C66 C71 1.517(11) . ?
C67 C68 1.370(12) . ?
C67 H67 0.9500 . ?
C68 C69 1.366(11) . ?
C68 H68 0.9500 . ?
C69 C70 1.410(10) . ?
C69 H69 0.9500 . ?
C70 C74 1.519(10) . ?
C71 C73 1.532(10) . ?
C71 C72 1.547(9) . ?
C71 H71 1.0000 . ?
C72 H72A 0.9800 . ?
C72 H72B 0.9800 . ?
C72 H72C 0.9800 . ?
C73 H73A 0.9800 . ?
C73 H73B 0.9800 . ?
C73 H73C 0.9800 . ?
C74 C76 1.525(12) . ?
C74 C75 1.543(11) . ?
C74 H74 1.0000 . ?
C75 H75A 0.9800 . ?
C75 H75B 0.9800 . ?
C75 H75C 0.9800 . ?
C76 H76A 0.9800 . ?
C76 H76B 0.9800 . ?
C76 H76C 0.9800 . ?
N5 C77 1.124(12) . ?
C77 C78 1.451(13) . ?
C78 H78A 0.9800 . ?
C78 H78B 0.9800 . ?
C78 H78C 0.9800 . ?

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
O3 V1 N1 99.5(2) . . ?
O3 V1 O1 120.3(2) . . ?
N1 V1 O1 90.5(2) . . ?
O3 V1 O2 116.9(2) . . ?
N1 V1 O2 93.5(2) . . ?
O1 V1 O2 121.0(2) . . ?
O3 V1 N2 92.8(2) . . ?
N1 V1 N2 167.6(2) . . ?
O1 V1 N2 82.72(17) . . ?
O2 V1 N2 81.29(18) . . ?
C1 O1 V1 127.9(4) . . ?
O1 C1 C6 122.5(5) . . ?
O1 C1 C2 120.2(5) . . ?
C6 C1 C2 117.3(6) . . ?
C3 C2 C1 121.6(6) . . ?
C3 C2 I1 119.4(5) . . ?
C1 C2 I1 118.9(5) . . ?
C2 C3 C4 119.8(6) . . ?
C2 C3 H3 120.1 . . ?
C4 C3 H3 120.1 . . ?
C3 C4 C5 120.3(6) . . ?
C3 C4 I2 119.5(4) . . ?
C5 C4 I2 120.1(5) . . ?
C6 C5 C4 119.1(6) . . ?
C6 C5 H5 120.5 . . ?
C4 C5 H5 120.5 . . ?
C1 C6 C5 121.8(6) . . ?
C1 C6 C7 117.9(5) . . ?
C5 C6 C7 120.1(5) . . ?
N1 C7 C6 109.0(5) . . ?
N1 C7 H7A 109.9 . . ?
C6 C7 H7A 109.9 . . ?
N1 C7 H7B 109.9 . . ?
C6 C7 H7B 109.9 . . ?
H7A C7 H7B 108.3 . . ?
C8 N1 C7 117.7(5) . . ?
C8 N1 V1 129.2(4) . . ?
C7 N1 V1 112.9(4) . . ?
C9 C8 C13 122.6(6) . . ?
C9 C8 N1 121.1(5) . . ?
C13 C8 N1 116.3(6) . . ?
C8 C9 C10 117.7(6) . . ?
C8 C9 C14 124.0(6) . . ?
C10 C9 C14 118.3(6) . . ?
C11 C10 C9 120.9(7) . . ?
C11 C10 H10 119.6 . . ?
C9 C10 H10 119.6 . . ?
C10 C11 C12 120.6(7) . . ?
C10 C11 H11 119.7 . . ?
C12 C11 H11 119.7 . . ?
C13 C12 C11 120.4(7) . . ?
C13 C12 H12 119.8 . . ?
C11 C12 H12 119.8 . . ?
C12 C13 C8 117.8(6) . . ?
C12 C13 C17 120.3(6) . . ?
C8 C13 C17 121.8(6) . . ?
C15 C14 C9 111.5(6) . . ?
C15 C14 C16 111.8(6) . . ?
C9 C14 C16 111.6(6) . . ?
C15 C14 H14 107.2 . . ?
C9 C14 H14 107.2 . . ?
C16 C14 H14 107.2 . . ?
C14 C15 H15A 109.5 . . ?
C14 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C14 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C14 C16 H16A 109.5 . . ?
C14 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C14 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C13 C17 C18 113.9(6) . . ?
C13 C17 C19 109.7(6) . . ?
C18 C17 C19 110.6(6) . . ?
C13 C17 H17 107.5 . . ?
C18 C17 H17 107.5 . . ?
C19 C17 H17 107.5 . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C17 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C17 C19 H19A 109.5 . . ?
C17 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C17 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C20 O2 V1 136.4(4) . . ?
O2 C20 C25 123.5(6) . . ?
O2 C20 C21 119.9(6) . . ?
C25 C20 C21 116.5(6) . . ?
C22 C21 C20 122.2(6) . . ?
C22 C21 I3 118.5(5) . . ?
C20 C21 I3 119.3(5) . . ?
C23 C22 C21 119.0(6) . . ?
C23 C22 H22 120.5 . . ?
C21 C22 H22 120.5 . . ?
C22 C23 C24 120.8(6) . . ?
C22 C23 I4 119.4(5) . . ?
C24 C23 I4 119.9(5) . . ?
C25 C24 C23 119.4(6) . . ?
C25 C24 H24 120.3 . . ?
C23 C24 H24 120.3 . . ?
C24 C25 C20 121.7(6) . . ?
C24 C25 C26 117.1(6) . . ?
C20 C25 C26 121.2(6) . . ?
N2 C26 C25 116.4(7) . . ?
N2 C26 H26A 108.2 . . ?
C25 C26 H26A 108.2 . . ?
N2 C26 H26B 108.2 . . ?
C25 C26 H26B 108.2 . . ?
H26A C26 H26B 107.4 . . ?
C26 N2 C27 115.4(5) . . ?
C26 N2 V1 114.9(5) . . ?
C27 N2 V1 122.5(4) . . ?
C26 N2 H2 99.0 . . ?
C27 N2 H2 99.0 . . ?
V1 N2 H2 99.0 . . ?
C32 C27 C28 122.2(5) . . ?
C32 C27 N2 120.8(5) . . ?
C28 C27 N2 117.0(5) . . ?
C29 C28 C27 117.1(6) . . ?
C29 C28 C33 121.2(6) . . ?
C27 C28 C33 121.7(5) . . ?
C30 C29 C28 121.5(6) . . ?
C30 C29 H29 119.2 . . ?
C28 C29 H29 119.2 . . ?
C29 C30 C31 120.2(6) . . ?
C29 C30 H30 119.9 . . ?
C31 C30 H30 119.9 . . ?
C30 C31 C32 121.7(6) . . ?
C30 C31 H31 119.2 . . ?
C32 C31 H31 119.2 . . ?
C27 C32 C31 117.3(6) . . ?
C27 C32 C36 123.8(5) . . ?
C31 C32 C36 118.9(6) . . ?
C35 C33 C28 112.4(6) . . ?
C35 C33 C34 110.5(7) . . ?
C28 C33 C34 112.7(6) . . ?
C35 C33 H33 107.0 . . ?
C28 C33 H33 107.0 . . ?
C34 C33 H33 107.0 . . ?
C33 C34 H34A 109.5 . . ?
C33 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
C33 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C33 C35 H35A 109.5 . . ?
C33 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
C33 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C32 C36 C37 110.5(7) . . ?
C32 C36 C38 110.6(6) . . ?
C37 C36 C38 111.3(7) . . ?
C32 C36 H36 108.1 . . ?
C37 C36 H36 108.1 . . ?
C38 C36 H36 108.1 . . ?
C36 C37 H37A 109.5 . . ?
C36 C37 H37B 109.5 . . ?
H37A C37 H37B 109.5 . . ?
C36 C37 H37C 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
C36 C38 H38A 109.5 . . ?
C36 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
C36 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
O6 V2 N4 100.8(2) . . ?
O6 V2 O5 117.6(2) . . ?
N4 V2 O5 91.6(2) . . ?
O6 V2 O4 118.3(2) . . ?
N4 V2 O4 93.5(2) . . ?
O5 V2 O4 121.7(2) . . ?
O6 V2 N3 94.5(2) . . ?
N4 V2 N3 164.7(2) . . ?
O5 V2 N3 80.50(18) . . ?
O4 V2 N3 79.80(19) . . ?
C39 O4 V2 137.4(4) . . ?
O4 C39 C40 119.9(6) . . ?
O4 C39 C44 122.5(6) . . ?
C40 C39 C44 117.6(6) . . ?
C41 C40 C39 121.9(6) . . ?
C41 C40 I5 118.3(5) . . ?
C39 C40 I5 119.7(5) . . ?
C40 C41 C42 119.3(7) . . ?
C40 C41 H41 120.3 . . ?
C42 C41 H41 120.3 . . ?
C43 C42 C41 120.0(6) . . ?
C43 C42 I6 120.0(5) . . ?
C41 C42 I6 119.9(5) . . ?
C42 C43 C44 120.8(6) . . ?
C42 C43 H43 119.6 . . ?
C44 C43 H43 119.6 . . ?
C43 C44 C39 120.3(6) . . ?
C43 C44 C45 120.0(6) . . ?
C39 C44 C45 119.7(6) . . ?
N3 C45 C44 110.0(6) . . ?
N3 C45 H45A 109.7 . . ?
C44 C45 H45A 109.7 . . ?
N3 C45 H45B 109.7 . . ?
C44 C45 H45B 109.7 . . ?
H45A C45 H45B 108.2 . . ?
C46 N3 C45 116.7(5) . . ?
C46 N3 V2 126.2(4) . . ?
C45 N3 V2 107.0(4) . . ?
C46 N3 H3A 100.6 . . ?
C45 N3 H3A 100.6 . . ?
V2 N3 H3A 100.6 . . ?
C47 C46 C51 120.8(6) . . ?
C47 C46 N3 121.1(6) . . ?
C51 C46 N3 118.1(6) . . ?
C48 C47 C46 117.7(6) . . ?
C48 C47 C52 118.0(6) . . ?
C46 C47 C52 124.3(6) . . ?
C49 C48 C47 121.9(7) . . ?
C49 C48 H48 119.1 . . ?
C47 C48 H48 119.1 . . ?
C48 C49 C50 119.5(7) . . ?
C48 C49 H49 120.2 . . ?
C50 C49 H49 120.2 . . ?
C49 C50 C51 122.0(7) . . ?
C49 C50 H50 119.0 . . ?
C51 C50 H50 119.0 . . ?
C50 C51 C46 117.8(6) . . ?
C50 C51 C55 118.8(6) . . ?
C46 C51 C55 123.3(6) . . ?
C47 C52 C54 111.9(6) . . ?
C47 C52 C53 109.5(6) . . ?
C54 C52 C53 111.4(7) . . ?
C47 C52 H52 107.9 . . ?
C54 C52 H52 107.9 . . ?
C53 C52 H52 107.9 . . ?
C52 C53 H53A 109.5 . . ?
C52 C53 H53B 109.5 . . ?
H53A C53 H53B 109.5 . . ?
C52 C53 H53C 109.5 . . ?
H53A C53 H53C 109.5 . . ?
H53B C53 H53C 109.5 . . ?
C52 C54 H54A 109.5 . . ?
C52 C54 H54B 109.5 . . ?
H54A C54 H54B 109.5 . . ?
C52 C54 H54C 109.5 . . ?
H54A C54 H54C 109.5 . . ?
H54B C54 H54C 109.5 . . ?
C56 C55 C51 111.2(6) . . ?
C56 C55 C57 111.3(7) . . ?
C51 C55 C57 111.9(6) . . ?
C56 C55 H55 107.4 . . ?
C51 C55 H55 107.4 . . ?
C57 C55 H55 107.4 . . ?
C55 C56 H56A 109.5 . . ?
C55 C56 H56B 109.5 . . ?
H56A C56 H56B 109.5 . . ?
C55 C56 H56C 109.5 . . ?
H56A C56 H56C 109.5 . . ?
H56B C56 H56C 109.5 . . ?
C55 C57 H57A 109.5 . . ?
C55 C57 H57B 109.5 . . ?
H57A C57 H57B 109.5 . . ?
C55 C57 H57C 109.5 . . ?
H57A C57 H57C 109.5 . . ?
H57B C57 H57C 109.5 . . ?
C58 O5 V2 128.5(4) . . ?
O5 C58 C59 120.0(6) . . ?
O5 C58 C63 120.1(6) . . ?
C59 C58 C63 119.9(6) . . ?
C58 C59 C60 120.5(6) . . ?
C58 C59 I7 119.3(5) . . ?
C60 C59 I7 120.1(5) . . ?
C61 C60 C59 118.8(7) . . ?
C61 C60 H60 120.6 . . ?
C59 C60 H60 120.6 . . ?
C60 C61 C62 121.7(6) . . ?
C60 C61 I8 119.0(5) . . ?
C62 C61 I8 119.2(5) . . ?
C61 C62 C63 120.6(6) . . ?
C61 C62 H62 119.7 . . ?
C63 C62 H62 119.7 . . ?
C62 C63 C58 118.4(6) . . ?
C62 C63 C64 122.6(6) . . ?
C58 C63 C64 119.0(6) . . ?
N4 C64 C63 109.7(5) . . ?
N4 C64 H64A 109.7 . . ?
C63 C64 H64A 109.7 . . ?
N4 C64 H64B 109.7 . . ?
C63 C64 H64B 109.7 . . ?
H64A C64 H64B 108.2 . . ?
C65 N4 C64 115.3(5) . . ?
C65 N4 V2 134.3(4) . . ?
C64 N4 V2 110.3(4) . . ?
C70 C65 C66 122.7(6) . . ?
C70 C65 N4 120.4(6) . . ?
C66 C65 N4 116.8(6) . . ?
C67 C66 C65 116.8(7) . . ?
C67 C66 C71 121.4(7) . . ?
C65 C66 C71 121.6(6) . . ?
C68 C67 C66 121.3(8) . . ?
C68 C67 H67 119.4 . . ?
C66 C67 H67 119.4 . . ?
C69 C68 C67 120.8(8) . . ?
C69 C68 H68 119.6 . . ?
C67 C68 H68 119.6 . . ?
C68 C69 C70 120.9(8) . . ?
C68 C69 H69 119.5 . . ?
C70 C69 H69 119.5 . . ?
C65 C70 C69 117.4(7) . . ?
C65 C70 C74 124.2(6) . . ?
C69 C70 C74 118.4(7) . . ?
C66 C71 C73 114.3(7) . . ?
C66 C71 C72 110.6(6) . . ?
C73 C71 C72 108.2(6) . . ?
C66 C71 H71 107.8 . . ?
C73 C71 H71 107.8 . . ?
C72 C71 H71 107.8 . . ?
C71 C72 H72A 109.5 . . ?
C71 C72 H72B 109.5 . . ?
H72A C72 H72B 109.5 . . ?
C71 C72 H72C 109.5 . . ?
H72A C72 H72C 109.5 . . ?
H72B C72 H72C 109.5 . . ?
C71 C73 H73A 109.5 . . ?
C71 C73 H73B 109.5 . . ?
H73A C73 H73B 109.5 . . ?
C71 C73 H73C 109.5 . . ?
H73A C73 H73C 109.5 . . ?
H73B C73 H73C 109.5 . . ?
C70 C74 C76 111.5(7) . . ?
C70 C74 C75 110.5(7) . . ?
C76 C74 C75 111.8(8) . . ?
C70 C74 H74 107.6 . . ?
C76 C74 H74 107.6 . . ?
C75 C74 H74 107.6 . . ?
C74 C75 H75A 109.5 . . ?
C74 C75 H75B 109.5 . . ?
H75A C75 H75B 109.5 . . ?
C74 C75 H75C 109.5 . . ?
H75A C75 H75C 109.5 . . ?
H75B C75 H75C 109.5 . . ?
C74 C76 H76A 109.5 . . ?
C74 C76 H76B 109.5 . . ?
H76A C76 H76B 109.5 . . ?
C74 C76 H76C 109.5 . . ?
H76A C76 H76C 109.5 . . ?
H76B C76 H76C 109.5 . . ?
N5 C77 C78 179.3(14) . . ?
C77 C78 H78A 109.5 . . ?
C77 C78 H78B 109.5 . . ?
H78A C78 H78B 109.5 . . ?
C77 C78 H78C 109.5 . . ?
H78A C78 H78C 109.5 . . ?
H78B C78 H78C 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
O3 V1 O1 C1 -104.5(5) . . . . ?
N1 V1 O1 C1 -3.2(5) . . . . ?
O2 V1 O1 C1 91.2(5) . . . . ?
N2 V1 O1 C1 166.5(5) . . . . ?
V1 O1 C1 C6 -24.0(9) . . . . ?
V1 O1 C1 C2 153.5(5) . . . . ?
O1 C1 C2 C3 178.4(6) . . . . ?
C6 C1 C2 C3 -4.0(10) . . . . ?
O1 C1 C2 I1 -6.4(8) . . . . ?
C6 C1 C2 I1 171.2(5) . . . . ?
C1 C2 C3 C4 1.3(10) . . . . ?
I1 C2 C3 C4 -173.9(5) . . . . ?
C2 C3 C4 C5 2.7(10) . . . . ?
C2 C3 C4 I2 178.6(5) . . . . ?
C3 C4 C5 C6 -3.8(10) . . . . ?
I2 C4 C5 C6 -179.6(5) . . . . ?
O1 C1 C6 C5 -179.6(6) . . . . ?
C2 C1 C6 C5 2.8(9) . . . . ?
O1 C1 C6 C7 5.4(9) . . . . ?
C2 C1 C6 C7 -172.2(6) . . . . ?
C4 C5 C6 C1 1.0(9) . . . . ?
C4 C5 C6 C7 175.9(6) . . . . ?
C1 C6 C7 N1 43.3(8) . . . . ?
C5 C6 C7 N1 -131.8(6) . . . . ?
C6 C7 N1 C8 100.6(6) . . . . ?
C6 C7 N1 V1 -74.1(5) . . . . ?
O3 V1 N1 C8 -3.5(5) . . . . ?
O1 V1 N1 C8 -124.3(5) . . . . ?
O2 V1 N1 C8 114.6(5) . . . . ?
N2 V1 N1 C8 179(58) . . . . ?
O3 V1 N1 C7 170.5(4) . . . . ?
O1 V1 N1 C7 49.7(4) . . . . ?
O2 V1 N1 C7 -71.5(4) . . . . ?
N2 V1 N1 C7 -6.7(11) . . . . ?
C7 N1 C8 C9 -95.3(7) . . . . ?
V1 N1 C8 C9 78.4(7) . . . . ?
C7 N1 C8 C13 86.4(7) . . . . ?
V1 N1 C8 C13 -99.9(6) . . . . ?
C13 C8 C9 C10 -0.1(10) . . . . ?
N1 C8 C9 C10 -178.4(6) . . . . ?
C13 C8 C9 C14 177.7(6) . . . . ?
N1 C8 C9 C14 -0.6(10) . . . . ?
C8 C9 C10 C11 0.0(10) . . . . ?
C14 C9 C10 C11 -178.0(7) . . . . ?
C9 C10 C11 C12 -0.3(12) . . . . ?
C10 C11 C12 C13 0.8(12) . . . . ?
C11 C12 C13 C8 -0.9(11) . . . . ?
C11 C12 C13 C17 177.0(7) . . . . ?
C9 C8 C13 C12 0.6(10) . . . . ?
N1 C8 C13 C12 179.0(6) . . . . ?
C9 C8 C13 C17 -177.3(6) . . . . ?
N1 C8 C13 C17 1.1(9) . . . . ?
C8 C9 C14 C15 -112.6(7) . . . . ?
C10 C9 C14 C15 65.2(8) . . . . ?
C8 C9 C14 C16 121.5(7) . . . . ?
C10 C9 C14 C16 -60.7(8) . . . . ?
C12 C13 C17 C18 49.9(9) . . . . ?
C8 C13 C17 C18 -132.2(7) . . . . ?
C12 C13 C17 C19 -74.6(8) . . . . ?
C8 C13 C17 C19 103.2(7) . . . . ?
O3 V1 O2 C20 -63.8(6) . . . . ?
N1 V1 O2 C20 -166.3(6) . . . . ?
O1 V1 O2 C20 101.0(6) . . . . ?
N2 V1 O2 C20 25.0(6) . . . . ?
V1 O2 C20 C25 -2.5(10) . . . . ?
V1 O2 C20 C21 178.4(4) . . . . ?
O2 C20 C21 C22 -175.8(6) . . . . ?
C25 C20 C21 C22 5.0(9) . . . . ?
O2 C20 C21 I3 2.0(8) . . . . ?
C25 C20 C21 I3 -177.2(4) . . . . ?
C20 C21 C22 C23 0.7(9) . . . . ?
I3 C21 C22 C23 -177.1(5) . . . . ?
C21 C22 C23 C24 -5.4(10) . . . . ?
C21 C22 C23 I4 173.6(5) . . . . ?
C22 C23 C24 C25 4.0(10) . . . . ?
I4 C23 C24 C25 -175.0(5) . . . . ?
C23 C24 C25 C20 2.1(10) . . . . ?
C23 C24 C25 C26 -177.4(8) . . . . ?
O2 C20 C25 C24 174.5(6) . . . . ?
C21 C20 C25 C24 -6.4(9) . . . . ?
O2 C20 C25 C26 -6.1(11) . . . . ?
C21 C20 C25 C26 173.0(8) . . . . ?
C24 C25 C26 N2 152.4(7) . . . . ?
C20 C25 C26 N2 -27.1(12) . . . . ?
C25 C26 N2 C27 -150.1(7) . . . . ?
C25 C26 N2 V1 58.7(10) . . . . ?
C26 N2 C27 C32 -69.2(9) . . . . ?
V1 N2 C27 C32 79.6(6) . . . . ?
C26 N2 C27 C28 110.8(8) . . . . ?
V1 N2 C27 C28 -100.3(6) . . . . ?
C32 C27 C28 C29 0.6(9) . . . . ?
N2 C27 C28 C29 -179.5(5) . . . . ?
C32 C27 C28 C33 179.5(6) . . . . ?
N2 C27 C28 C33 -0.5(9) . . . . ?
C27 C28 C29 C30 -1.0(10) . . . . ?
C33 C28 C29 C30 -179.9(6) . . . . ?
C28 C29 C30 C31 -0.3(11) . . . . ?
C29 C30 C31 C32 2.0(10) . . . . ?
C28 C27 C32 C31 1.0(9) . . . . ?
N2 C27 C32 C31 -179.0(5) . . . . ?
C28 C27 C32 C36 -179.0(6) . . . . ?
N2 C27 C32 C36 1.0(9) . . . . ?
C30 C31 C32 C27 -2.3(9) . . . . ?
C30 C31 C32 C36 177.7(6) . . . . ?
C29 C28 C33 C35 94.9(8) . . . . ?
C27 C28 C33 C35 -84.0(8) . . . . ?
C29 C28 C33 C34 -30.7(10) . . . . ?
C27 C28 C33 C34 150.4(7) . . . . ?
C27 C32 C36 C37 -119.3(7) . . . . ?
C31 C32 C36 C37 60.7(8) . . . . ?
C27 C32 C36 C38 117.0(7) . . . . ?
C31 C32 C36 C38 -62.9(9) . . . . ?
O6 V2 O4 C39 -62.3(7) . . . . ?
N4 V2 O4 C39 -166.5(7) . . . . ?
O5 V2 O4 C39 99.4(7) . . . . ?
N3 V2 O4 C39 27.4(6) . . . . ?
V2 O4 C39 C40 -179.7(5) . . . . ?
V2 O4 C39 C44 -0.8(11) . . . . ?
O4 C39 C40 C41 -179.2(7) . . . . ?
C44 C39 C40 C41 1.9(11) . . . . ?
O4 C39 C40 I5 3.6(9) . . . . ?
C44 C39 C40 I5 -175.3(5) . . . . ?
C39 C40 C41 C42 -0.7(11) . . . . ?
I5 C40 C41 C42 176.4(5) . . . . ?
C40 C41 C42 C43 -0.6(11) . . . . ?
C40 C41 C42 I6 -176.9(5) . . . . ?
C41 C42 C43 C44 0.8(11) . . . . ?
I6 C42 C43 C44 177.1(5) . . . . ?
C42 C43 C44 C39 0.3(11) . . . . ?
C42 C43 C44 C45 -178.8(7) . . . . ?
O4 C39 C44 C43 179.5(6) . . . . ?
C40 C39 C44 C43 -1.7(10) . . . . ?
O4 C39 C44 C45 -1.4(11) . . . . ?
C40 C39 C44 C45 177.5(7) . . . . ?
C43 C44 C45 N3 137.8(7) . . . . ?
C39 C44 C45 N3 -41.3(9) . . . . ?
C44 C45 N3 C46 -137.9(6) . . . . ?
C44 C45 N3 V2 74.4(6) . . . . ?
C45 N3 C46 C47 -59.4(8) . . . . ?
V2 N3 C46 C47 81.2(7) . . . . ?
C45 N3 C46 C51 119.8(7) . . . . ?
V2 N3 C46 C51 -99.5(6) . . . . ?
C51 C46 C47 C48 -4.5(10) . . . . ?
N3 C46 C47 C48 174.8(6) . . . . ?
C51 C46 C47 C52 172.7(6) . . . . ?
N3 C46 C47 C52 -8.1(10) . . . . ?
C46 C47 C48 C49 0.2(10) . . . . ?
C52 C47 C48 C49 -177.1(7) . . . . ?
C47 C48 C49 C50 2.7(11) . . . . ?
C48 C49 C50 C51 -1.4(10) . . . . ?
C49 C50 C51 C46 -2.7(10) . . . . ?
C49 C50 C51 C55 179.5(6) . . . . ?
C47 C46 C51 C50 5.7(9) . . . . ?
N3 C46 C51 C50 -173.6(6) . . . . ?
C47 C46 C51 C55 -176.6(6) . . . . ?
N3 C46 C51 C55 4.1(9) . . . . ?
C48 C47 C52 C54 -55.9(9) . . . . ?
C46 C47 C52 C54 126.9(7) . . . . ?
C48 C47 C52 C53 68.1(8) . . . . ?
C46 C47 C52 C53 -109.0(8) . . . . ?
C50 C51 C55 C56 83.9(8) . . . . ?
C46 C51 C55 C56 -93.8(8) . . . . ?
C50 C51 C55 C57 -41.4(9) . . . . ?
C46 C51 C55 C57 141.0(7) . . . . ?
O6 V2 O5 C58 -111.7(5) . . . . ?
N4 V2 O5 C58 -8.7(5) . . . . ?
O4 V2 O5 C58 86.5(5) . . . . ?
N3 V2 O5 C58 158.1(5) . . . . ?
V2 O5 C58 C59 161.4(5) . . . . ?
V2 O5 C58 C63 -17.7(9) . . . . ?
O5 C58 C59 C60 178.3(6) . . . . ?
C63 C58 C59 C60 -2.6(10) . . . . ?
O5 C58 C59 I7 -5.5(8) . . . . ?
C63 C58 C59 I7 173.6(5) . . . . ?
C58 C59 C60 C61 2.5(11) . . . . ?
I7 C59 C60 C61 -173.7(5) . . . . ?
C59 C60 C61 C62 -0.5(11) . . . . ?
C59 C60 C61 I8 176.7(5) . . . . ?
C60 C61 C62 C63 -1.4(11) . . . . ?
I8 C61 C62 C63 -178.5(5) . . . . ?
C61 C62 C63 C58 1.2(10) . . . . ?
C61 C62 C63 C64 179.0(6) . . . . ?
O5 C58 C63 C62 179.9(6) . . . . ?
C59 C58 C63 C62 0.7(10) . . . . ?
O5 C58 C63 C64 2.0(9) . . . . ?
C59 C58 C63 C64 -177.1(6) . . . . ?
C62 C63 C64 N4 -132.4(6) . . . . ?
C58 C63 C64 N4 45.4(8) . . . . ?
C63 C64 N4 C65 100.5(6) . . . . ?
C63 C64 N4 V2 -75.6(6) . . . . ?
O6 V2 N4 C65 -4.5(7) . . . . ?
O5 V2 N4 C65 -122.9(6) . . . . ?
O4 V2 N4 C65 115.2(6) . . . . ?
N3 V2 N4 C65 178.7(7) . . . . ?
O6 V2 N4 C64 170.5(4) . . . . ?
O5 V2 N4 C64 52.1(4) . . . . ?
O4 V2 N4 C64 -69.8(4) . . . . ?
N3 V2 N4 C64 -6.3(11) . . . . ?
C64 N4 C65 C70 -99.4(7) . . . . ?
V2 N4 C65 C70 75.4(8) . . . . ?
C64 N4 C65 C66 78.4(7) . . . . ?
V2 N4 C65 C66 -106.8(7) . . . . ?
C70 C65 C66 C67 4.7(9) . . . . ?
N4 C65 C66 C67 -173.0(5) . . . . ?
C70 C65 C66 C71 -170.5(6) . . . . ?
N4 C65 C66 C71 11.8(9) . . . . ?
C65 C66 C67 C68 -1.7(10) . . . . ?
C71 C66 C67 C68 173.6(6) . . . . ?
C66 C67 C68 C69 -1.8(11) . . . . ?
C67 C68 C69 C70 2.4(11) . . . . ?
C66 C65 C70 C69 -4.2(10) . . . . ?
N4 C65 C70 C69 173.4(6) . . . . ?
C66 C65 C70 C74 176.7(6) . . . . ?
N4 C65 C70 C74 -5.7(10) . . . . ?
C68 C69 C70 C65 0.6(10) . . . . ?
C68 C69 C70 C74 179.7(7) . . . . ?
C67 C66 C71 C73 26.4(9) . . . . ?
C65 C66 C71 C73 -158.6(6) . . . . ?
C67 C66 C71 C72 -96.0(8) . . . . ?
C65 C66 C71 C72 79.0(8) . . . . ?
C65 C70 C74 C76 119.2(8) . . . . ?
C69 C70 C74 C76 -59.9(9) . . . . ?
C65 C70 C74 C75 -115.9(8) . . . . ?
C69 C70 C74 C75 65.0(9) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
C7 H7B I3 0.99 3.30 4.193(7) 151.4 3_766 yes
C24 H24 N5 0.95 2.64 3.429(11) 140.3 2_756 yes
C45 H45A O6 0.99 2.65 3.187(9) 114.4 . yes
C64 H64B O4 0.99 2.60 3.126(8) 113.6 . yes
C64 H64B I7 0.99 3.17 3.875(7) 129.2 2_656 yes

_refine_diff_density_max         1.659
_refine_diff_density_min         -1.574
_refine_diff_density_rms         0.147


#===END
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: acetonitrile'
####################################################################### 
# 
# 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_4
_database_code_depnum_ccdc_archive 'CCDC 2524181'
loop_
_audit_author_name
_audit_author_address
'Mark Elsegood'
;Loughborough University
United Kingdom
;
_audit_update_record             
;
2026-01-19 deposited with the CCDC.	2026-03-10 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2019/3
_shelx_SHELXL_version_number     2019/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C38 H43 Br4 N2 O3 V'
_chemical_formula_sum            'C38 H43 Br4 N2 O3 V'
_chemical_formula_weight         946.32

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'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.54854(9)
_cell_length_b                   12.30121(10)
_cell_length_c                   13.94099(11)
_cell_angle_alpha                76.1324(7)
_cell_angle_beta                 86.8450(6)
_cell_angle_gamma                87.7059(6)
_cell_volume                     1919.09(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    79282
_cell_measurement_theta_min      2.25
_cell_measurement_theta_max      38.01

_exptl_crystal_description       slab
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.638
_exptl_crystal_F_000             944
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.035
_exptl_absorpt_coefficient_mu    4.460
_shelx_estimated_absorpt_T_min   0.501
_shelx_estimated_absorpt_T_max   0.860
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.793
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   
; 
CrysAlisPro 1.171.43.95a (Rigaku Oxford Diffraction, 2023) 
Empirical absorption correction using spherical harmonics, 
implemented in SCALE3 ABSPACK scaling algorithm. 
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Rotating Anode'
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  
; 
Rigaku FRE+ equipped with Arc)Sec VHF Varimax confocal mirrors and an UG2 
goniometer and HyPix 6000HE detector 
;
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_radiation_collimation    0.2
_diffrn_detector_area_resol_mean 10
_diffrn_reflns_number            186991
_diffrn_reflns_av_unetI/netI     0.0210
_diffrn_reflns_av_R_equivalents  0.0339
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         1.989
_diffrn_reflns_theta_max         38.223
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.956
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.956
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.956
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             20278
_reflns_number_gt                16380
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
; 
 Reflections were merged by SHELXL according to the crystal 
 class for the calculation of statistics and refinement. 
  
 _reflns_Friedel_fraction is defined as the number of unique 
 Friedel pairs measured divided by the number that would be 
 possible theoretically, ignoring centric projections and 
 systematic absences. 
;

_computing_data_collection       
'CrysAlisPro system (CCD 43.95a 64-bit (release 03-11-2023))'
_computing_cell_refinement       'CrysAlisPro 1.171.43.95a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.43.95a (Rigaku OD, 2023)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2019/3 (Sheldrick, 2019)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0289P)²+0.8596P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         20278
_refine_ls_number_parameters     445
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0420
_refine_ls_R_factor_gt           0.0276
_refine_ls_wR_factor_ref         0.0647
_refine_ls_wR_factor_gt          0.0607
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_restrained_S_all      1.018
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
V1 V 0.32620(2) 0.30425(2) 0.71326(2) 0.01197(3) Uani 1 1 d . . . . .
O3 O 0.32620(7) 0.36320(7) 0.59810(6) 0.01819(14) Uani 1 1 d . . . . .
O1 O 0.35054(7) 0.39803(7) 0.79809(6) 0.01779(14) Uani 1 1 d . . . . .
C1 C 0.43193(9) 0.47003(8) 0.80373(8) 0.01431(16) Uani 1 1 d . . . . .
C2 C 0.41276(9) 0.54094(9) 0.86902(8) 0.01529(16) Uani 1 1 d . . . . .
C3 C 0.49195(10) 0.62054(9) 0.87598(9) 0.01918(19) Uani 1 1 d . . . . .
H3 H 0.477095 0.667703 0.920423 0.023 Uiso 1 1 calc R U . . .
C4 C 0.59307(10) 0.62957(9) 0.81665(9) 0.01968(19) Uani 1 1 d . . . . .
C5 C 0.61692(9) 0.55893(9) 0.75397(9) 0.01898(19) Uani 1 1 d . . . . .
H5 H 0.687655 0.565210 0.715150 0.023 Uiso 1 1 calc R U . . .
C6 C 0.53792(9) 0.47857(9) 0.74735(8) 0.01638(17) Uani 1 1 d . . . . .
Br1 Br 0.27575(2) 0.52747(2) 0.95076(2) 0.02048(2) Uani 1 1 d . . . . .
Br2 Br 0.70108(2) 0.73905(2) 0.82211(2) 0.03060(3) Uani 1 1 d . . . . .
C7 C 0.56808(10) 0.40359(10) 0.67760(10) 0.0225(2) Uani 1 1 d . . . . .
H7A H 0.535456 0.436996 0.612539 0.027 Uiso 1 1 calc R U . . .
H7B H 0.653442 0.397635 0.667768 0.027 Uiso 1 1 calc R U . . .
N1 N 0.52112(8) 0.28978(7) 0.71778(7) 0.01399(14) Uani 1 1 d . . . . .
H1 H 0.5216(16) 0.2829(15) 0.7794(14) 0.027(4) Uiso 1 1 d . . . . .
C8 C 0.59505(9) 0.19793(9) 0.69711(8) 0.01491(16) Uani 1 1 d . . . . .
C9 C 0.61093(9) 0.18187(9) 0.60109(8) 0.01727(17) Uani 1 1 d . . . . .
C10 C 0.68526(11) 0.09393(10) 0.58662(9) 0.0229(2) Uani 1 1 d . . . . .
H10 H 0.696728 0.081319 0.522112 0.028 Uiso 1 1 calc R U . . .
C11 C 0.74230(11) 0.02506(11) 0.66379(10) 0.0249(2) Uani 1 1 d . . . . .
H11 H 0.793737 -0.033035 0.651961 0.030 Uiso 1 1 calc R U . . .
C12 C 0.72421(10) 0.04105(10) 0.75846(9) 0.0218(2) Uani 1 1 d . . . . .
H12 H 0.763215 -0.006873 0.811435 0.026 Uiso 1 1 calc R U . . .
C13 C 0.64995(10) 0.12601(9) 0.77741(8) 0.01803(18) Uani 1 1 d . . . . .
C14 C 0.54904(10) 0.25086(10) 0.51259(8) 0.01935(19) Uani 1 1 d . . . . .
H14 H 0.504240 0.312881 0.534062 0.023 Uiso 1 1 calc R U . . .
C15 C 0.46239(11) 0.17787(12) 0.47902(9) 0.0259(2) Uani 1 1 d . . . . .
H15A H 0.504042 0.114734 0.459947 0.039 Uiso 1 1 calc R U . . .
H15B H 0.421917 0.222771 0.422249 0.039 Uiso 1 1 calc R U . . .
H15C H 0.405833 0.149472 0.533413 0.039 Uiso 1 1 calc R U . . .
C16 C 0.63434(12) 0.30368(12) 0.42754(9) 0.0263(2) Uani 1 1 d . . . . .
H16A H 0.686008 0.352728 0.450168 0.039 Uiso 1 1 calc R U . . .
H16B H 0.591079 0.347612 0.372067 0.039 Uiso 1 1 calc R U . . .
H16C H 0.680441 0.244434 0.406047 0.039 Uiso 1 1 calc R U . . .
C17 C 0.63144(12) 0.13886(11) 0.88335(9) 0.0261(2) Uani 1 1 d . . . . .
H17 H 0.549428 0.165491 0.891894 0.031 Uiso 1 1 calc R U . . .
C18 C 0.64909(18) 0.02803(15) 0.96055(11) 0.0402(4) Uani 1 1 d . . . . .
H18A H 0.605882 -0.030736 0.942850 0.060 Uiso 1 1 calc R U . . .
H18B H 0.620825 0.037122 1.025827 0.060 Uiso 1 1 calc R U . . .
H18C H 0.731826 0.006967 0.962244 0.060 Uiso 1 1 calc R U . . .
C19 C 0.71090(18) 0.22738(15) 0.90264(14) 0.0446(4) Uani 1 1 d . . . . .
H19A H 0.792097 0.203283 0.894978 0.067 Uiso 1 1 calc R U . . .
H19B H 0.694968 0.236572 0.970063 0.067 Uiso 1 1 calc R U . . .
H19C H 0.696467 0.298892 0.855217 0.067 Uiso 1 1 calc R U . . .
O2 O 0.34480(7) 0.14735(6) 0.76067(6) 0.01554(13) Uani 1 1 d . . . . .
C20 C 0.26229(9) 0.07250(8) 0.79586(7) 0.01385(15) Uani 1 1 d . . . . .
C21 C 0.28080(9) -0.04012(8) 0.79328(8) 0.01550(16) Uani 1 1 d . . . . .
C22 C 0.19623(10) -0.11919(9) 0.82802(8) 0.01733(17) Uani 1 1 d . . . . .
H22 H 0.209971 -0.195231 0.825807 0.021 Uiso 1 1 calc R U . . .
C23 C 0.09127(10) -0.08459(9) 0.86601(8) 0.01745(17) Uani 1 1 d . . . . .
C24 C 0.07022(9) 0.02578(9) 0.87153(8) 0.01652(17) Uani 1 1 d . . . . .
H24 H -0.001841 0.047732 0.898450 0.020 Uiso 1 1 calc R U . . .
C25 C 0.15606(9) 0.10375(8) 0.83711(7) 0.01441(16) Uani 1 1 d . . . . .
Br3 Br 0.42604(2) -0.08431(2) 0.74506(2) 0.02373(3) Uani 1 1 d . . . . .
Br4 Br -0.02743(2) -0.19025(2) 0.90859(2) 0.02423(3) Uani 1 1 d . . . . .
C26 C 0.13852(9) 0.22521(8) 0.84038(7) 0.01495(16) Uani 1 1 d . . . . .
H26A H 0.056799 0.240119 0.859894 0.018 Uiso 1 1 calc R U . . .
H26B H 0.188918 0.242952 0.889460 0.018 Uiso 1 1 calc R U . . .
N2 N 0.16828(7) 0.29505(7) 0.74085(6) 0.01289(13) Uani 1 1 d . . . . .
C27 C 0.07184(8) 0.33722(8) 0.68085(7) 0.01390(15) Uani 1 1 d . . . . .
C28 C 0.00964(9) 0.43048(9) 0.70134(8) 0.01554(16) Uani 1 1 d . . . . .
C29 C -0.08412(9) 0.47307(10) 0.64370(9) 0.02000(19) Uani 1 1 d . . . . .
H29 H -0.126390 0.536974 0.655143 0.024 Uiso 1 1 calc R U . . .
C30 C -0.11701(10) 0.42394(11) 0.56984(9) 0.0220(2) Uani 1 1 d . . . . .
H30 H -0.181480 0.453841 0.531533 0.026 Uiso 1 1 calc R U . . .
C31 C -0.05527(10) 0.33100(11) 0.55228(9) 0.0211(2) Uani 1 1 d . . . . .
H31 H -0.079496 0.296673 0.502811 0.025 Uiso 1 1 calc R U . . .
C32 C 0.04183(9) 0.28664(9) 0.60570(8) 0.01676(17) Uani 1 1 d . . . . .
C33 C 0.04568(9) 0.48724(9) 0.78011(8) 0.01676(17) Uani 1 1 d . . . . .
H33 H 0.114150 0.444270 0.812502 0.020 Uiso 1 1 calc R U . . .
C34 C -0.05064(12) 0.48619(12) 0.86020(9) 0.0260(2) Uani 1 1 d . . . . .
H34A H -0.119298 0.527111 0.830233 0.039 Uiso 1 1 calc R U . . .
H34B H -0.023755 0.522154 0.910188 0.039 Uiso 1 1 calc R U . . .
H34C H -0.070540 0.408622 0.891471 0.039 Uiso 1 1 calc R U . . .
C35 C 0.08330(14) 0.60704(11) 0.73341(10) 0.0285(3) Uani 1 1 d . . . . .
H35A H 0.145982 0.605679 0.683341 0.043 Uiso 1 1 calc R U . . .
H35B H 0.110826 0.640574 0.784739 0.043 Uiso 1 1 calc R U . . .
H35C H 0.017182 0.651528 0.702250 0.043 Uiso 1 1 calc R U . . .
C36 C 0.11019(10) 0.18863(10) 0.58006(9) 0.01993(19) Uani 1 1 d . . . . .
H36 H 0.178135 0.171843 0.623229 0.024 Uiso 1 1 calc R U . . .
C37 C 0.03809(14) 0.08302(12) 0.60011(11) 0.0316(3) Uani 1 1 d . . . . .
H37A H 0.009563 0.064452 0.669454 0.047 Uiso 1 1 calc R U . . .
H37B H 0.086484 0.020607 0.586613 0.047 Uiso 1 1 calc R U . . .
H37C H -0.027895 0.096417 0.557095 0.047 Uiso 1 1 calc R U . . .
C38 C 0.15711(12) 0.21845(12) 0.47226(10) 0.0274(2) Uani 1 1 d . . . . .
H38A H 0.092116 0.232749 0.428174 0.041 Uiso 1 1 calc R U . . .
H38B H 0.205586 0.156007 0.458942 0.041 Uiso 1 1 calc R U . . .
H38C H 0.203625 0.285665 0.460728 0.041 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
V1 O3 1.5954(8) . ?
V1 N2 1.8452(9) . ?
V1 O1 1.8775(8) . ?
V1 O2 1.8918(8) . ?
V1 N1 2.2542(9) . ?
O1 C1 1.3350(12) . ?
C1 C2 1.4075(14) . ?
C1 C6 1.4113(14) . ?
C2 C3 1.3899(14) . ?
C2 Br1 1.8872(11) . ?
C3 C4 1.3857(17) . ?
C3 H3 0.9500 . ?
C4 C5 1.3831(16) . ?
C4 Br2 1.8893(10) . ?
C5 C6 1.3940(14) . ?
C5 H5 0.9500 . ?
C6 C7 1.5114(16) . ?
C7 N1 1.4898(14) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
N1 C8 1.4629(13) . ?
N1 H1 0.843(19) . ?
C8 C9 1.4004(15) . ?
C8 C13 1.4129(15) . ?
C9 C10 1.3997(16) . ?
C9 C14 1.5166(16) . ?
C10 C11 1.3803(19) . ?
C10 H10 0.9500 . ?
C11 C12 1.3838(18) . ?
C11 H11 0.9500 . ?
C12 C13 1.3905(16) . ?
C12 H12 0.9500 . ?
C13 C17 1.5252(16) . ?
C14 C15 1.5335(17) . ?
C14 C16 1.5335(17) . ?
C14 H14 1.0000 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 C19 1.532(2) . ?
C17 C18 1.535(2) . ?
C17 H17 1.0000 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
O2 C20 1.3411(12) . ?
C20 C21 1.4020(14) . ?
C20 C25 1.4050(14) . ?
C21 C22 1.3902(15) . ?
C21 Br3 1.8812(10) . ?
C22 C23 1.3882(16) . ?
C22 H22 0.9500 . ?
C23 C24 1.3892(15) . ?
C23 Br4 1.8984(10) . ?
C24 C25 1.3914(14) . ?
C24 H24 0.9500 . ?
C25 C26 1.5110(14) . ?
C26 N2 1.4769(13) . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
N2 C27 1.4344(13) . ?
C27 C32 1.4051(14) . ?
C27 C28 1.4079(14) . ?
C28 C29 1.3933(15) . ?
C28 C33 1.5191(15) . ?
C29 C30 1.3890(17) . ?
C29 H29 0.9500 . ?
C30 C31 1.3875(17) . ?
C30 H30 0.9500 . ?
C31 C32 1.3993(16) . ?
C31 H31 0.9500 . ?
C32 C36 1.5180(16) . ?
C33 C34 1.5303(16) . ?
C33 C35 1.5312(17) . ?
C33 H33 1.0000 . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
C36 C37 1.5317(18) . ?
C36 C38 1.5325(18) . ?
C36 H36 1.0000 . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?

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
O3 V1 N2 99.40(4) . . ?
O3 V1 O1 116.08(4) . . ?
N2 V1 O1 95.17(4) . . ?
O3 V1 O2 122.37(4) . . ?
N2 V1 O2 90.61(4) . . ?
O1 V1 O2 119.27(4) . . ?
O3 V1 N1 94.53(4) . . ?
N2 V1 N1 165.94(4) . . ?
O1 V1 N1 80.23(3) . . ?
O2 V1 N1 80.30(3) . . ?
C1 O1 V1 134.85(7) . . ?
O1 C1 C2 119.20(9) . . ?
O1 C1 C6 123.10(9) . . ?
C2 C1 C6 117.70(9) . . ?
C3 C2 C1 122.18(10) . . ?
C3 C2 Br1 118.56(8) . . ?
C1 C2 Br1 119.26(7) . . ?
C4 C3 C2 118.51(10) . . ?
C4 C3 H3 120.7 . . ?
C2 C3 H3 120.7 . . ?
C5 C4 C3 121.06(10) . . ?
C5 C4 Br2 119.30(9) . . ?
C3 C4 Br2 119.64(8) . . ?
C4 C5 C6 120.48(10) . . ?
C4 C5 H5 119.8 . . ?
C6 C5 H5 119.8 . . ?
C5 C6 C1 119.98(10) . . ?
C5 C6 C7 118.38(10) . . ?
C1 C6 C7 121.63(9) . . ?
N1 C7 C6 110.83(9) . . ?
N1 C7 H7A 109.5 . . ?
C6 C7 H7A 109.5 . . ?
N1 C7 H7B 109.5 . . ?
C6 C7 H7B 109.5 . . ?
H7A C7 H7B 108.1 . . ?
C8 N1 C7 114.80(8) . . ?
C8 N1 V1 126.46(6) . . ?
C7 N1 V1 107.97(7) . . ?
C8 N1 H1 105.8(12) . . ?
C7 N1 H1 102.6(12) . . ?
V1 N1 H1 94.3(13) . . ?
C9 C8 C13 121.15(9) . . ?
C9 C8 N1 121.18(9) . . ?
C13 C8 N1 117.67(9) . . ?
C10 C9 C8 117.92(10) . . ?
C10 C9 C14 117.93(10) . . ?
C8 C9 C14 124.11(10) . . ?
C11 C10 C9 121.61(11) . . ?
C11 C10 H10 119.2 . . ?
C9 C10 H10 119.2 . . ?
C10 C11 C12 119.69(11) . . ?
C10 C11 H11 120.2 . . ?
C12 C11 H11 120.2 . . ?
C11 C12 C13 121.16(11) . . ?
C11 C12 H12 119.4 . . ?
C13 C12 H12 119.4 . . ?
C12 C13 C8 118.41(10) . . ?
C12 C13 C17 119.10(10) . . ?
C8 C13 C17 122.48(10) . . ?
C9 C14 C15 109.57(10) . . ?
C9 C14 C16 112.00(10) . . ?
C15 C14 C16 111.28(10) . . ?
C9 C14 H14 107.9 . . ?
C15 C14 H14 107.9 . . ?
C16 C14 H14 107.9 . . ?
C14 C15 H15A 109.5 . . ?
C14 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C14 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C14 C16 H16A 109.5 . . ?
C14 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C14 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C13 C17 C19 110.98(13) . . ?
C13 C17 C18 112.75(11) . . ?
C19 C17 C18 109.85(13) . . ?
C13 C17 H17 107.7 . . ?
C19 C17 H17 107.7 . . ?
C18 C17 H17 107.7 . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C17 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C17 C19 H19A 109.5 . . ?
C17 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C17 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C20 O2 V1 127.96(7) . . ?
O2 C20 C21 120.41(9) . . ?
O2 C20 C25 121.44(9) . . ?
C21 C20 C25 118.15(9) . . ?
C22 C21 C20 121.64(10) . . ?
C22 C21 Br3 119.92(8) . . ?
C20 C21 Br3 118.41(8) . . ?
C23 C22 C21 118.54(10) . . ?
C23 C22 H22 120.7 . . ?
C21 C22 H22 120.7 . . ?
C22 C23 C24 121.63(10) . . ?
C22 C23 Br4 119.02(8) . . ?
C24 C23 Br4 119.33(8) . . ?
C23 C24 C25 119.13(10) . . ?
C23 C24 H24 120.4 . . ?
C25 C24 H24 120.4 . . ?
C24 C25 C20 120.89(9) . . ?
C24 C25 C26 121.82(9) . . ?
C20 C25 C26 117.28(9) . . ?
N2 C26 C25 108.10(8) . . ?
N2 C26 H26A 110.1 . . ?
C25 C26 H26A 110.1 . . ?
N2 C26 H26B 110.1 . . ?
C25 C26 H26B 110.1 . . ?
H26A C26 H26B 108.4 . . ?
C27 N2 C26 115.64(8) . . ?
C27 N2 V1 131.36(7) . . ?
C26 N2 V1 112.86(7) . . ?
C32 C27 C28 122.29(9) . . ?
C32 C27 N2 120.89(9) . . ?
C28 C27 N2 116.82(9) . . ?
C29 C28 C27 117.78(10) . . ?
C29 C28 C33 120.34(9) . . ?
C27 C28 C33 121.82(9) . . ?
C30 C29 C28 121.30(11) . . ?
C30 C29 H29 119.3 . . ?
C28 C29 H29 119.3 . . ?
C31 C30 C29 119.69(11) . . ?
C31 C30 H30 120.2 . . ?
C29 C30 H30 120.2 . . ?
C30 C31 C32 121.56(10) . . ?
C30 C31 H31 119.2 . . ?
C32 C31 H31 119.2 . . ?
C31 C32 C27 117.33(10) . . ?
C31 C32 C36 119.55(10) . . ?
C27 C32 C36 123.12(9) . . ?
C28 C33 C34 111.84(9) . . ?
C28 C33 C35 110.69(9) . . ?
C34 C33 C35 110.80(10) . . ?
C28 C33 H33 107.8 . . ?
C34 C33 H33 107.8 . . ?
C35 C33 H33 107.8 . . ?
C33 C34 H34A 109.5 . . ?
C33 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
C33 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C33 C35 H35A 109.5 . . ?
C33 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
C33 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C32 C36 C37 111.90(11) . . ?
C32 C36 C38 111.04(10) . . ?
C37 C36 C38 110.41(10) . . ?
C32 C36 H36 107.8 . . ?
C37 C36 H36 107.8 . . ?
C38 C36 H36 107.8 . . ?
C36 C37 H37A 109.5 . . ?
C36 C37 H37B 109.5 . . ?
H37A C37 H37B 109.5 . . ?
C36 C37 H37C 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
C36 C38 H38A 109.5 . . ?
C36 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
C36 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 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
O3 V1 O1 C1 -54.20(11) . . . . ?
N2 V1 O1 C1 -157.31(10) . . . . ?
O2 V1 O1 C1 109.08(10) . . . . ?
N1 V1 O1 C1 36.09(10) . . . . ?
V1 O1 C1 C2 169.74(8) . . . . ?
V1 O1 C1 C6 -10.62(17) . . . . ?
O1 C1 C2 C3 -177.65(10) . . . . ?
C6 C1 C2 C3 2.69(16) . . . . ?
O1 C1 C2 Br1 2.78(14) . . . . ?
C6 C1 C2 Br1 -176.87(8) . . . . ?
C1 C2 C3 C4 -0.22(17) . . . . ?
Br1 C2 C3 C4 179.35(9) . . . . ?
C2 C3 C4 C5 -1.98(17) . . . . ?
C2 C3 C4 Br2 178.63(8) . . . . ?
C3 C4 C5 C6 1.62(18) . . . . ?
Br2 C4 C5 C6 -179.00(9) . . . . ?
C4 C5 C6 C1 0.97(17) . . . . ?
C4 C5 C6 C7 179.90(11) . . . . ?
O1 C1 C6 C5 177.32(10) . . . . ?
C2 C1 C6 C5 -3.03(16) . . . . ?
O1 C1 C6 C7 -1.57(17) . . . . ?
C2 C1 C6 C7 178.07(11) . . . . ?
C5 C6 C7 N1 146.35(10) . . . . ?
C1 C6 C7 N1 -34.74(15) . . . . ?
C6 C7 N1 C8 -144.03(10) . . . . ?
C6 C7 N1 V1 69.04(10) . . . . ?
C7 N1 C8 C9 -69.66(13) . . . . ?
V1 N1 C8 C9 70.15(12) . . . . ?
C7 N1 C8 C13 110.31(11) . . . . ?
V1 N1 C8 C13 -109.89(10) . . . . ?
C13 C8 C9 C10 -1.56(16) . . . . ?
N1 C8 C9 C10 178.41(10) . . . . ?
C13 C8 C9 C14 175.93(10) . . . . ?
N1 C8 C9 C14 -4.11(16) . . . . ?
C8 C9 C10 C11 -0.46(18) . . . . ?
C14 C9 C10 C11 -178.10(12) . . . . ?
C9 C10 C11 C12 1.5(2) . . . . ?
C10 C11 C12 C13 -0.4(2) . . . . ?
C11 C12 C13 C8 -1.50(18) . . . . ?
C11 C12 C13 C17 178.99(12) . . . . ?
C9 C8 C13 C12 2.52(16) . . . . ?
N1 C8 C13 C12 -177.44(10) . . . . ?
C9 C8 C13 C17 -177.98(11) . . . . ?
N1 C8 C13 C17 2.05(16) . . . . ?
C10 C9 C14 C15 66.59(13) . . . . ?
C8 C9 C14 C15 -110.89(12) . . . . ?
C10 C9 C14 C16 -57.40(14) . . . . ?
C8 C9 C14 C16 125.12(12) . . . . ?
C12 C13 C17 C19 96.25(14) . . . . ?
C8 C13 C17 C19 -83.24(15) . . . . ?
C12 C13 C17 C18 -27.48(18) . . . . ?
C8 C13 C17 C18 153.03(13) . . . . ?
O3 V1 O2 C20 -100.30(9) . . . . ?
N2 V1 O2 C20 1.25(9) . . . . ?
O1 V1 O2 C20 97.52(9) . . . . ?
N1 V1 O2 C20 170.47(9) . . . . ?
V1 O2 C20 C21 155.90(8) . . . . ?
V1 O2 C20 C25 -24.82(14) . . . . ?
O2 C20 C21 C22 -179.12(10) . . . . ?
C25 C20 C21 C22 1.56(16) . . . . ?
O2 C20 C21 Br3 2.85(14) . . . . ?
C25 C20 C21 Br3 -176.46(8) . . . . ?
C20 C21 C22 C23 0.00(16) . . . . ?
Br3 C21 C22 C23 177.99(8) . . . . ?
C21 C22 C23 C24 -1.17(17) . . . . ?
C21 C22 C23 Br4 177.38(8) . . . . ?
C22 C23 C24 C25 0.71(17) . . . . ?
Br4 C23 C24 C25 -177.83(8) . . . . ?
C23 C24 C25 C20 0.92(16) . . . . ?
C23 C24 C25 C26 179.62(10) . . . . ?
O2 C20 C25 C24 178.67(10) . . . . ?
C21 C20 C25 C24 -2.02(15) . . . . ?
O2 C20 C25 C26 -0.08(15) . . . . ?
C21 C20 C25 C26 179.22(9) . . . . ?
C24 C25 C26 N2 -128.74(10) . . . . ?
C20 C25 C26 N2 50.00(12) . . . . ?
C25 C26 N2 C27 99.70(10) . . . . ?
C25 C26 N2 V1 -76.41(9) . . . . ?
O3 V1 N2 C27 -5.41(9) . . . . ?
O1 V1 N2 C27 112.14(9) . . . . ?
O2 V1 N2 C27 -128.39(9) . . . . ?
N1 V1 N2 C27 -177.74(11) . . . . ?
O3 V1 N2 C26 169.92(7) . . . . ?
O1 V1 N2 C26 -72.53(7) . . . . ?
O2 V1 N2 C26 46.94(7) . . . . ?
N1 V1 N2 C26 -2.41(18) . . . . ?
C26 N2 C27 C32 -101.37(11) . . . . ?
V1 N2 C27 C32 73.86(12) . . . . ?
C26 N2 C27 C28 78.45(11) . . . . ?
V1 N2 C27 C28 -106.32(10) . . . . ?
C32 C27 C28 C29 -0.42(16) . . . . ?
N2 C27 C28 C29 179.77(9) . . . . ?
C32 C27 C28 C33 -177.59(10) . . . . ?
N2 C27 C28 C33 2.59(15) . . . . ?
C27 C28 C29 C30 1.38(17) . . . . ?
C33 C28 C29 C30 178.59(11) . . . . ?
C28 C29 C30 C31 -0.39(18) . . . . ?
C29 C30 C31 C32 -1.62(19) . . . . ?
C30 C31 C32 C27 2.50(17) . . . . ?
C30 C31 C32 C36 -176.81(11) . . . . ?
C28 C27 C32 C31 -1.47(16) . . . . ?
N2 C27 C32 C31 178.34(10) . . . . ?
C28 C27 C32 C36 177.81(10) . . . . ?
N2 C27 C32 C36 -2.38(16) . . . . ?
C29 C28 C33 C34 61.93(14) . . . . ?
C27 C28 C33 C34 -120.96(11) . . . . ?
C29 C28 C33 C35 -62.15(14) . . . . ?
C27 C28 C33 C35 114.96(12) . . . . ?
C31 C32 C36 C37 -64.81(14) . . . . ?
C27 C32 C36 C37 115.92(12) . . . . ?
C31 C32 C36 C38 59.06(14) . . . . ?
C27 C32 C36 C38 -120.21(12) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
C7 H7A O3 0.99 2.65 3.1614(15) 112.3 . yes
C14 H14 O3 1.00 2.32 3.1813(14) 144.1 . yes

_refine_diff_density_max         1.529
_refine_diff_density_min         -1.265
_refine_diff_density_rms         0.079

_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: acetonitrile'
####################################################################### 
# 
# 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 2524178'
loop_
_audit_author_name
_audit_author_address
'Mark Elsegood'
;Loughborough University
United Kingdom
;
_audit_update_record             
;
2026-01-19 deposited with the CCDC.	2026-03-10 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C38 H43 Br4 N2 O3 V'
_chemical_formula_sum            'C38 H43 Br4 N2 O3 V'
_chemical_formula_weight         946.32

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
V V 0.0687 2.1097 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.6763 1.2805 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.80158(12)
_cell_length_b                   12.16142(14)
_cell_length_c                   13.69665(13)
_cell_angle_alpha                77.3250(9)
_cell_angle_beta                 86.4467(8)
_cell_angle_gamma                89.4045(9)
_cell_volume                     1914.19(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    39503
_cell_measurement_theta_min      3.28
_cell_measurement_theta_max      76.49

_exptl_crystal_description       block
_exptl_crystal_colour            'dark orange'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.642
_exptl_crystal_F_000             944
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.040
_exptl_absorpt_coefficient_mu    7.356
_shelx_estimated_absorpt_T_min   0.321
_shelx_estimated_absorpt_T_max   0.757
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.598
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   
; 
CrysAlisPro 1.171.41.122a (Rigaku Oxford Diffraction, 2021) 
Empirical absorption correction using spherical harmonics, 
implemented in SCALE3 ABSPACK scaling algorithm. 
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_source                   'Rotating anode'
_diffrn_measurement_device_type  
; 
Rigaku 007HF diffractometer with HF Varimax confocal mirrors, 
an UG2 goniometer and HyPix 6000HE detector. 
;
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_radiation_collimation    0.3
_diffrn_detector_area_resol_mean 10
_diffrn_reflns_number            51853
_diffrn_reflns_av_unetI/netI     0.0139
_diffrn_reflns_av_R_equivalents  0.0264
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         3.313
_diffrn_reflns_theta_max         70.062
_diffrn_reflns_theta_full        67.679
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_point_group_measured_fraction_full 0.996
_reflns_number_total             7245
_reflns_number_gt                7121
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
; 
 Reflections were merged by SHELXL according to the crystal 
 class for the calculation of statistics and refinement. 
  
 _reflns_Friedel_fraction is defined as the number of unique 
 Friedel pairs measured divided by the number that would be 
 possible theoretically, ignoring centric projections and 
 systematic absences. 
;

_computing_data_collection       'CrysAlisPro 1.171.41.122a (Rigaku OD, 2021)'
_computing_cell_refinement       'CrysAlisPro 1.171.41.122a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.122a (Rigaku OD, 2021)'
_computing_structure_solution    'SHELXT-2018/2 (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0196P)²+2.5825P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_extinction_coef       0.00018(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         7245
_refine_ls_number_parameters     445
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0261
_refine_ls_R_factor_gt           0.0257
_refine_ls_wR_factor_ref         0.0591
_refine_ls_wR_factor_gt          0.0589
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_restrained_S_all      1.042
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
V1 V 0.33907(3) 0.31986(3) 0.70460(3) 0.02700(9) Uani 1 1 d . . . . .
O1 O 0.35448(12) 0.16323(12) 0.75754(11) 0.0238(3) Uani 1 1 d . . . . .
O3 O 0.33581(13) 0.37502(13) 0.58802(12) 0.0299(3) Uani 1 1 d . . . . .
C1 C 0.27349(17) 0.08633(17) 0.79428(15) 0.0223(4) Uani 1 1 d . . . . .
C2 C 0.29046(18) -0.02713(18) 0.79200(16) 0.0237(4) Uani 1 1 d . . . . .
Br1 Br 0.43395(2) -0.07014(2) 0.74386(2) 0.03102(7) Uani 1 1 d . . . . .
C3 C 0.20650(19) -0.10746(18) 0.82484(16) 0.0265(4) Uani 1 1 d . . . . .
H3 H 0.219198 -0.183987 0.821996 0.032 Uiso 1 1 calc R U . . .
C4 C 0.10318(19) -0.07329(19) 0.86205(16) 0.0270(5) Uani 1 1 d . . . . .
Br2 Br -0.01640(2) -0.18043(2) 0.90222(2) 0.03629(7) Uani 1 1 d . . . . .
C5 C 0.08394(18) 0.03698(19) 0.86943(16) 0.0260(4) Uani 1 1 d . . . . .
H5 H 0.013215 0.058079 0.896844 0.031 Uiso 1 1 calc R U . . .
C6 C 0.16952(18) 0.11671(18) 0.83619(16) 0.0237(4) Uani 1 1 d . . . . .
C7 C 0.15324(18) 0.23830(18) 0.84181(16) 0.0249(4) Uani 1 1 d . . . . .
H7A H 0.074142 0.250249 0.865759 0.030 Uiso 1 1 calc R U . . .
H7B H 0.204796 0.257779 0.889843 0.030 Uiso 1 1 calc R U . . .
N1 N 0.17792(15) 0.31163(15) 0.74087(14) 0.0266(4) Uani 1 1 d . . . . .
C8 C 0.08037(17) 0.34239(18) 0.68275(17) 0.0249(4) Uani 1 1 d . . . . .
C9 C 0.05264(18) 0.28579(19) 0.60834(17) 0.0286(5) Uani 1 1 d . . . . .
C10 C -0.0450(2) 0.3195(2) 0.55774(19) 0.0355(5) Uani 1 1 d . . . . .
H10 H -0.066973 0.280783 0.508684 0.043 Uiso 1 1 calc R U . . .
C11 C -0.1105(2) 0.4076(3) 0.5772(2) 0.0411(6) Uani 1 1 d . . . . .
H11 H -0.175750 0.430364 0.540613 0.049 Uiso 1 1 calc R U . . .
C12 C -0.0812(2) 0.4628(2) 0.6501(2) 0.0391(6) Uani 1 1 d . . . . .
H12 H -0.126528 0.523672 0.662852 0.047 Uiso 1 1 calc R U . . .
C13 C 0.01333(19) 0.4311(2) 0.70503(18) 0.0303(5) Uani 1 1 d . . . . .
C14 C 0.1237(2) 0.1919(2) 0.57873(19) 0.0341(5) Uani 1 1 d . . . . .
H14 H 0.191223 0.180056 0.620416 0.041 Uiso 1 1 calc R U . . .
C15 C 0.0577(3) 0.0805(2) 0.5986(2) 0.0475(7) Uani 1 1 d . . . . .
H15A H 0.028677 0.061190 0.668842 0.071 Uiso 1 1 calc R U . . .
H15B H 0.108268 0.020572 0.584682 0.071 Uiso 1 1 calc R U . . .
H15C H -0.005934 0.088426 0.554910 0.071 Uiso 1 1 calc R U . . .
C16 C 0.1667(2) 0.2258(3) 0.4682(2) 0.0429(6) Uani 1 1 d . . . . .
H16A H 0.101921 0.237143 0.425692 0.064 Uiso 1 1 calc R U . . .
H16B H 0.215310 0.166065 0.451160 0.064 Uiso 1 1 calc R U . . .
H16C H 0.210487 0.296019 0.457054 0.064 Uiso 1 1 calc R U . . .
C17 C 0.0459(2) 0.4958(2) 0.78226(19) 0.0368(5) Uani 1 1 d . . . . .
H17 H 0.109979 0.454250 0.818247 0.044 Uiso 1 1 calc R U . . .
C18 C -0.0483(4) 0.5014(3) 0.8597(3) 0.0718(12) Uani 1 1 d . . . . .
H18A H -0.021308 0.540028 0.909562 0.108 Uiso 1 1 calc R U . . .
H18B H -0.072823 0.424835 0.892797 0.108 Uiso 1 1 calc R U . . .
H18C H -0.112434 0.542976 0.827236 0.108 Uiso 1 1 calc R U . . .
C19 C 0.0894(2) 0.6124(2) 0.7321(2) 0.0444(6) Uani 1 1 d . . . . .
H19A H 0.028013 0.656625 0.697719 0.067 Uiso 1 1 calc R U . . .
H19B H 0.152168 0.606162 0.683308 0.067 Uiso 1 1 calc R U . . .
H19C H 0.116367 0.649768 0.782882 0.067 Uiso 1 1 calc R U . . .
O2 O 0.35876(12) 0.41998(13) 0.78942(12) 0.0277(3) Uani 1 1 d . . . . .
C20 C 0.44021(18) 0.49018(17) 0.80211(16) 0.0247(4) Uani 1 1 d . . . . .
C21 C 0.42099(19) 0.55731(18) 0.87244(17) 0.0270(4) Uani 1 1 d . . . . .
Br3 Br 0.28233(2) 0.54151(2) 0.95161(2) 0.03412(7) Uani 1 1 d . . . . .
C22 C 0.4995(2) 0.63560(19) 0.88618(19) 0.0328(5) Uani 1 1 d . . . . .
H22 H 0.484233 0.680377 0.934230 0.039 Uiso 1 1 calc R U . . .
C23 C 0.6001(2) 0.64684(19) 0.8284(2) 0.0359(5) Uani 1 1 d . . . . .
Br4 Br 0.70789(3) 0.75569(2) 0.84334(3) 0.05603(10) Uani 1 1 d . . . . .
C24 C 0.6243(2) 0.57994(19) 0.76017(19) 0.0333(5) Uani 1 1 d . . . . .
H24 H 0.695061 0.588047 0.722208 0.040 Uiso 1 1 calc R U . . .
C25 C 0.54584(19) 0.50088(18) 0.74675(17) 0.0272(4) Uani 1 1 d . . . . .
C26 C 0.5749(2) 0.42848(19) 0.67241(18) 0.0307(5) Uani 1 1 d . . . . .
H26A H 0.542758 0.462532 0.607622 0.037 Uiso 1 1 calc R U . . .
H26B H 0.658408 0.425175 0.660955 0.037 Uiso 1 1 calc R U . . .
N2 N 0.52853(15) 0.31124(15) 0.71019(14) 0.0244(4) Uani 1 1 d . . . . .
H2 H 0.526(2) 0.303(2) 0.772(2) 0.029 Uiso 1 1 d . U . . .
C27 C 0.60449(18) 0.22150(19) 0.69003(17) 0.0262(4) Uani 1 1 d . . . . .
C28 C 0.6694(2) 0.1657(2) 0.76822(18) 0.0317(5) Uani 1 1 d . . . . .
C29 C 0.7368(2) 0.0759(2) 0.75241(19) 0.0363(5) Uani 1 1 d . . . . .
H29 H 0.779703 0.035808 0.805233 0.044 Uiso 1 1 calc R U . . .
C30 C 0.7427(2) 0.0438(2) 0.66153(19) 0.0358(5) Uani 1 1 d . . . . .
H30 H 0.787872 -0.018707 0.652471 0.043 Uiso 1 1 calc R U . . .
C31 C 0.6825(2) 0.1034(2) 0.58409(18) 0.0331(5) Uani 1 1 d . . . . .
H31 H 0.688516 0.082529 0.521071 0.040 Uiso 1 1 calc R U . . .
C32 C 0.61284(19) 0.19366(19) 0.59604(17) 0.0281(5) Uani 1 1 d . . . . .
C33 C 0.6700(2) 0.2004(2) 0.86899(19) 0.0394(6) Uani 1 1 d . . . . .
H33 H 0.643356 0.280300 0.858026 0.047 Uiso 1 1 calc R U . . .
C34 C 0.5862(3) 0.1301(3) 0.9439(2) 0.0535(7) Uani 1 1 d . . . . .
H34A H 0.510591 0.137795 0.917369 0.080 Uiso 1 1 calc R U . . .
H34B H 0.584204 0.155854 1.006904 0.080 Uiso 1 1 calc R U . . .
H34C H 0.609334 0.050866 0.956013 0.080 Uiso 1 1 calc R U . . .
C35 C 0.7886(2) 0.1972(3) 0.9083(2) 0.0481(7) Uani 1 1 d . . . . .
H35A H 0.787630 0.235539 0.964230 0.072 Uiso 1 1 calc R U . . .
H35B H 0.842422 0.235415 0.854410 0.072 Uiso 1 1 calc R U . . .
H35C H 0.811916 0.118705 0.931306 0.072 Uiso 1 1 calc R U . . .
C36 C 0.5504(2) 0.2557(2) 0.50651(17) 0.0319(5) Uani 1 1 d . . . . .
H36 H 0.509261 0.320619 0.526056 0.038 Uiso 1 1 calc R U . . .
C37 C 0.4625(2) 0.1778(2) 0.47903(18) 0.0364(5) Uani 1 1 d . . . . .
H37A H 0.500833 0.112120 0.461826 0.055 Uiso 1 1 calc R U . . .
H37B H 0.422582 0.218639 0.421423 0.055 Uiso 1 1 calc R U . . .
H37C H 0.407786 0.152815 0.536246 0.055 Uiso 1 1 calc R U . . .
C38 C 0.6340(2) 0.3026(2) 0.41731(19) 0.0399(6) Uani 1 1 d . . . . .
H38A H 0.684664 0.357345 0.435338 0.060 Uiso 1 1 calc R U . . .
H38B H 0.591812 0.339679 0.359776 0.060 Uiso 1 1 calc R U . . .
H38C H 0.679010 0.240764 0.399767 0.060 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
V1 O3 1.5932(16) . ?
V1 O2 1.8832(15) . ?
V1 O1 1.8948(15) . ?
V1 N1 1.9335(18) . ?
V1 N2 2.2426(18) . ?
O1 C1 1.339(2) . ?
C1 C2 1.399(3) . ?
C1 C6 1.403(3) . ?
C2 C3 1.382(3) . ?
C2 Br1 1.890(2) . ?
C3 C4 1.387(3) . ?
C3 H3 0.9500 . ?
C4 C5 1.382(3) . ?
C4 Br2 1.902(2) . ?
C5 C6 1.392(3) . ?
C5 H5 0.9500 . ?
C6 C7 1.507(3) . ?
C7 N1 1.485(3) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
N1 C8 1.440(3) . ?
C8 C9 1.405(3) . ?
C8 C13 1.407(3) . ?
C9 C10 1.393(3) . ?
C9 C14 1.521(3) . ?
C10 C11 1.379(4) . ?
C10 H10 0.9500 . ?
C11 C12 1.381(4) . ?
C11 H11 0.9500 . ?
C12 C13 1.388(3) . ?
C12 H12 0.9500 . ?
C13 C17 1.520(3) . ?
C14 C15 1.533(4) . ?
C14 C16 1.535(4) . ?
C14 H14 1.0000 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 C18 1.500(4) . ?
C17 C19 1.513(4) . ?
C17 H17 1.0000 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
O2 C20 1.336(3) . ?
C20 C21 1.400(3) . ?
C20 C25 1.410(3) . ?
C21 C22 1.385(3) . ?
C21 Br3 1.894(2) . ?
C22 C23 1.377(4) . ?
C22 H22 0.9500 . ?
C23 C24 1.383(4) . ?
C23 Br4 1.897(2) . ?
C24 C25 1.390(3) . ?
C24 H24 0.9500 . ?
C25 C26 1.508(3) . ?
C26 N2 1.503(3) . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
N2 C27 1.467(3) . ?
N2 H2 0.83(3) . ?
C27 C32 1.399(3) . ?
C27 C28 1.402(3) . ?
C28 C29 1.392(3) . ?
C28 C33 1.530(3) . ?
C29 C30 1.381(4) . ?
C29 H29 0.9500 . ?
C30 C31 1.378(4) . ?
C30 H30 0.9500 . ?
C31 C32 1.397(3) . ?
C31 H31 0.9500 . ?
C32 C36 1.520(3) . ?
C33 C34 1.506(4) . ?
C33 C35 1.528(4) . ?
C33 H33 1.0000 . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
C36 C37 1.530(3) . ?
C36 C38 1.532(3) . ?
C36 H36 1.0000 . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?

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
O3 V1 O2 116.26(8) . . ?
O3 V1 O1 123.96(8) . . ?
O2 V1 O1 118.55(7) . . ?
O3 V1 N1 99.44(8) . . ?
O2 V1 N1 90.53(7) . . ?
O1 V1 N1 90.95(7) . . ?
O3 V1 N2 97.02(8) . . ?
O2 V1 N2 80.94(7) . . ?
O1 V1 N2 80.93(6) . . ?
N1 V1 N2 163.49(8) . . ?
C1 O1 V1 128.89(13) . . ?
O1 C1 C2 120.72(18) . . ?
O1 C1 C6 121.27(19) . . ?
C2 C1 C6 118.01(19) . . ?
C3 C2 C1 122.03(19) . . ?
C3 C2 Br1 119.80(16) . . ?
C1 C2 Br1 118.16(16) . . ?
C2 C3 C4 118.2(2) . . ?
C2 C3 H3 120.9 . . ?
C4 C3 H3 120.9 . . ?
C5 C4 C3 121.9(2) . . ?
C5 C4 Br2 118.92(16) . . ?
C3 C4 Br2 119.22(16) . . ?
C4 C5 C6 119.2(2) . . ?
C4 C5 H5 120.4 . . ?
C6 C5 H5 120.4 . . ?
C5 C6 C1 120.64(19) . . ?
C5 C6 C7 121.53(19) . . ?
C1 C6 C7 117.81(18) . . ?
N1 C7 C6 109.39(17) . . ?
N1 C7 H7A 109.8 . . ?
C6 C7 H7A 109.8 . . ?
N1 C7 H7B 109.8 . . ?
C6 C7 H7B 109.8 . . ?
H7A C7 H7B 108.2 . . ?
C8 N1 C7 115.02(17) . . ?
C8 N1 V1 132.11(14) . . ?
C7 N1 V1 111.42(13) . . ?
C9 C8 C13 121.6(2) . . ?
C9 C8 N1 121.71(19) . . ?
C13 C8 N1 116.68(19) . . ?
C10 C9 C8 117.7(2) . . ?
C10 C9 C14 118.3(2) . . ?
C8 C9 C14 124.0(2) . . ?
C11 C10 C9 121.5(2) . . ?
C11 C10 H10 119.2 . . ?
C9 C10 H10 119.2 . . ?
C10 C11 C12 119.8(2) . . ?
C10 C11 H11 120.1 . . ?
C12 C11 H11 120.1 . . ?
C11 C12 C13 121.3(2) . . ?
C11 C12 H12 119.3 . . ?
C13 C12 H12 119.3 . . ?
C12 C13 C8 118.0(2) . . ?
C12 C13 C17 120.1(2) . . ?
C8 C13 C17 121.7(2) . . ?
C9 C14 C15 111.9(2) . . ?
C9 C14 C16 110.5(2) . . ?
C15 C14 C16 110.4(2) . . ?
C9 C14 H14 108.0 . . ?
C15 C14 H14 108.0 . . ?
C16 C14 H14 108.0 . . ?
C14 C15 H15A 109.5 . . ?
C14 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C14 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C14 C16 H16A 109.5 . . ?
C14 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C14 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C18 C17 C19 111.2(2) . . ?
C18 C17 C13 113.0(2) . . ?
C19 C17 C13 111.0(2) . . ?
C18 C17 H17 107.1 . . ?
C19 C17 H17 107.1 . . ?
C13 C17 H17 107.1 . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C17 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C17 C19 H19A 109.5 . . ?
C17 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C17 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C20 O2 V1 136.15(14) . . ?
O2 C20 C21 119.4(2) . . ?
O2 C20 C25 122.8(2) . . ?
C21 C20 C25 117.8(2) . . ?
C22 C21 C20 122.5(2) . . ?
C22 C21 Br3 118.48(18) . . ?
C20 C21 Br3 119.01(16) . . ?
C23 C22 C21 118.3(2) . . ?
C23 C22 H22 120.9 . . ?
C21 C22 H22 120.9 . . ?
C22 C23 C24 121.3(2) . . ?
C22 C23 Br4 119.25(19) . . ?
C24 C23 Br4 119.47(19) . . ?
C23 C24 C25 120.5(2) . . ?
C23 C24 H24 119.8 . . ?
C25 C24 H24 119.8 . . ?
C24 C25 C20 119.7(2) . . ?
C24 C25 C26 119.3(2) . . ?
C20 C25 C26 121.05(19) . . ?
N2 C26 C25 110.81(18) . . ?
N2 C26 H26A 109.5 . . ?
C25 C26 H26A 109.5 . . ?
N2 C26 H26B 109.5 . . ?
C25 C26 H26B 109.5 . . ?
H26A C26 H26B 108.1 . . ?
C27 N2 C26 114.56(17) . . ?
C27 N2 V1 127.99(14) . . ?
C26 N2 V1 107.87(13) . . ?
C27 N2 H2 104.2(18) . . ?
C26 N2 H2 103.9(19) . . ?
V1 N2 H2 93.0(18) . . ?
C32 C27 C28 121.3(2) . . ?
C32 C27 N2 121.3(2) . . ?
C28 C27 N2 117.42(19) . . ?
C29 C28 C27 118.2(2) . . ?
C29 C28 C33 119.0(2) . . ?
C27 C28 C33 122.7(2) . . ?
C30 C29 C28 121.4(2) . . ?
C30 C29 H29 119.3 . . ?
C28 C29 H29 119.3 . . ?
C31 C30 C29 119.4(2) . . ?
C31 C30 H30 120.3 . . ?
C29 C30 H30 120.3 . . ?
C30 C31 C32 121.6(2) . . ?
C30 C31 H31 119.2 . . ?
C32 C31 H31 119.2 . . ?
C31 C32 C27 117.9(2) . . ?
C31 C32 C36 118.2(2) . . ?
C27 C32 C36 123.8(2) . . ?
C34 C33 C35 112.1(2) . . ?
C34 C33 C28 110.2(2) . . ?
C35 C33 C28 112.6(2) . . ?
C34 C33 H33 107.2 . . ?
C35 C33 H33 107.2 . . ?
C28 C33 H33 107.2 . . ?
C33 C34 H34A 109.5 . . ?
C33 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
C33 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C33 C35 H35A 109.5 . . ?
C33 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
C33 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C32 C36 C37 110.1(2) . . ?
C32 C36 C38 110.9(2) . . ?
C37 C36 C38 111.5(2) . . ?
C32 C36 H36 108.1 . . ?
C37 C36 H36 108.1 . . ?
C38 C36 H36 108.1 . . ?
C36 C37 H37A 109.5 . . ?
C36 C37 H37B 109.5 . . ?
H37A C37 H37B 109.5 . . ?
C36 C37 H37C 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
C36 C38 H38A 109.5 . . ?
C36 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
C36 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 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
O3 V1 O1 C1 -96.54(18) . . . . ?
O2 V1 O1 C1 96.64(17) . . . . ?
N1 V1 O1 C1 5.52(17) . . . . ?
N2 V1 O1 C1 171.07(18) . . . . ?
V1 O1 C1 C2 153.50(16) . . . . ?
V1 O1 C1 C6 -26.6(3) . . . . ?
O1 C1 C2 C3 -176.78(19) . . . . ?
C6 C1 C2 C3 3.3(3) . . . . ?
O1 C1 C2 Br1 4.1(3) . . . . ?
C6 C1 C2 Br1 -175.86(15) . . . . ?
C1 C2 C3 C4 -0.8(3) . . . . ?
Br1 C2 C3 C4 178.38(16) . . . . ?
C2 C3 C4 C5 -1.8(3) . . . . ?
C2 C3 C4 Br2 177.20(16) . . . . ?
C3 C4 C5 C6 1.7(3) . . . . ?
Br2 C4 C5 C6 -177.30(16) . . . . ?
C4 C5 C6 C1 1.0(3) . . . . ?
C4 C5 C6 C7 179.7(2) . . . . ?
O1 C1 C6 C5 176.71(19) . . . . ?
C2 C1 C6 C5 -3.4(3) . . . . ?
O1 C1 C6 C7 -2.0(3) . . . . ?
C2 C1 C6 C7 177.87(19) . . . . ?
C5 C6 C7 N1 -125.4(2) . . . . ?
C1 C6 C7 N1 53.3(3) . . . . ?
C6 C7 N1 C8 94.4(2) . . . . ?
C6 C7 N1 V1 -73.55(19) . . . . ?
C7 N1 C8 C9 -98.9(2) . . . . ?
V1 N1 C8 C9 65.9(3) . . . . ?
C7 N1 C8 C13 80.3(2) . . . . ?
V1 N1 C8 C13 -114.9(2) . . . . ?
C13 C8 C9 C10 -0.8(3) . . . . ?
N1 C8 C9 C10 178.3(2) . . . . ?
C13 C8 C9 C14 178.0(2) . . . . ?
N1 C8 C9 C14 -2.8(3) . . . . ?
C8 C9 C10 C11 2.1(4) . . . . ?
C14 C9 C10 C11 -176.8(2) . . . . ?
C9 C10 C11 C12 -1.6(4) . . . . ?
C10 C11 C12 C13 -0.3(4) . . . . ?
C11 C12 C13 C8 1.5(4) . . . . ?
C11 C12 C13 C17 177.9(3) . . . . ?
C9 C8 C13 C12 -0.9(4) . . . . ?
N1 C8 C13 C12 179.9(2) . . . . ?
C9 C8 C13 C17 -177.3(2) . . . . ?
N1 C8 C13 C17 3.5(3) . . . . ?
C10 C9 C14 C15 -63.1(3) . . . . ?
C8 C9 C14 C15 118.0(3) . . . . ?
C10 C9 C14 C16 60.3(3) . . . . ?
C8 C9 C14 C16 -118.6(3) . . . . ?
C12 C13 C17 C18 55.9(4) . . . . ?
C8 C13 C17 C18 -127.8(3) . . . . ?
C12 C13 C17 C19 -69.8(3) . . . . ?
C8 C13 C17 C19 106.5(3) . . . . ?
O3 V1 O2 C20 -64.2(2) . . . . ?
O1 V1 O2 C20 103.6(2) . . . . ?
N1 V1 O2 C20 -165.0(2) . . . . ?
N2 V1 O2 C20 29.2(2) . . . . ?
V1 O2 C20 C21 176.87(15) . . . . ?
V1 O2 C20 C25 -2.6(3) . . . . ?
O2 C20 C21 C22 -176.9(2) . . . . ?
C25 C20 C21 C22 2.5(3) . . . . ?
O2 C20 C21 Br3 2.7(3) . . . . ?
C25 C20 C21 Br3 -177.78(16) . . . . ?
C20 C21 C22 C23 -0.3(3) . . . . ?
Br3 C21 C22 C23 -179.95(17) . . . . ?
C21 C22 C23 C24 -1.8(4) . . . . ?
C21 C22 C23 Br4 178.62(17) . . . . ?
C22 C23 C24 C25 1.4(4) . . . . ?
Br4 C23 C24 C25 -178.95(17) . . . . ?
C23 C24 C25 C20 0.9(3) . . . . ?
C23 C24 C25 C26 -179.5(2) . . . . ?
O2 C20 C25 C24 176.6(2) . . . . ?
C21 C20 C25 C24 -2.8(3) . . . . ?
O2 C20 C25 C26 -2.9(3) . . . . ?
C21 C20 C25 C26 177.7(2) . . . . ?
C24 C25 C26 N2 143.2(2) . . . . ?
C20 C25 C26 N2 -37.3(3) . . . . ?
C25 C26 N2 C27 -140.24(19) . . . . ?
C25 C26 N2 V1 70.6(2) . . . . ?
C26 N2 C27 C32 -80.2(3) . . . . ?
V1 N2 C27 C32 61.6(3) . . . . ?
C26 N2 C27 C28 99.1(2) . . . . ?
V1 N2 C27 C28 -119.2(2) . . . . ?
C32 C27 C28 C29 -4.5(4) . . . . ?
N2 C27 C28 C29 176.2(2) . . . . ?
C32 C27 C28 C33 174.7(2) . . . . ?
N2 C27 C28 C33 -4.5(3) . . . . ?
C27 C28 C29 C30 1.8(4) . . . . ?
C33 C28 C29 C30 -177.5(2) . . . . ?
C28 C29 C30 C31 1.4(4) . . . . ?
C29 C30 C31 C32 -1.9(4) . . . . ?
C30 C31 C32 C27 -0.8(4) . . . . ?
C30 C31 C32 C36 179.3(2) . . . . ?
C28 C27 C32 C31 4.1(3) . . . . ?
N2 C27 C32 C31 -176.7(2) . . . . ?
C28 C27 C32 C36 -176.1(2) . . . . ?
N2 C27 C32 C36 3.1(3) . . . . ?
C29 C28 C33 C34 -85.3(3) . . . . ?
C27 C28 C33 C34 95.4(3) . . . . ?
C29 C28 C33 C35 40.6(3) . . . . ?
C27 C28 C33 C35 -138.6(3) . . . . ?
C31 C32 C36 C37 66.1(3) . . . . ?
C27 C32 C36 C37 -113.7(2) . . . . ?
C31 C32 C36 C38 -57.7(3) . . . . ?
C27 C32 C36 C38 122.4(2) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
C7 H7A Br2 0.99 3.14 3.692(2) 116.9 2_557 yes
C36 H36 O3 1.00 2.31 3.170(3) 143.1 . yes

_refine_diff_density_max         0.783
_refine_diff_density_min         -0.690
_refine_diff_density_rms         0.055

_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: acetonitrile'
####################################################################### 
# 
# 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_9
_database_code_depnum_ccdc_archive 'CCDC 2524174'
loop_
_audit_author_name
_audit_author_address
'Mark Elsegood'
;Loughborough University
United Kingdom
;
_audit_update_record             
;
2026-01-19 deposited with the CCDC.	2026-03-10 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2019/3
_shelx_SHELXL_version_number     2019/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C38 H40 Cl4 N2 O3 V'
_chemical_formula_sum            'C38 H40 Cl4 N2 O3 V'
_chemical_formula_weight         765.46

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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

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

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

_cell_length_a                   12.4676(5)
_cell_length_b                   29.7770(9)
_cell_length_c                   10.7464(5)
_cell_angle_alpha                90
_cell_angle_beta                 113.769(5)
_cell_angle_gamma                90
_cell_volume                     3651.2(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    11261
_cell_measurement_theta_min      1.78
_cell_measurement_theta_max      33.14

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.393
_exptl_crystal_F_000             1588
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.210
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.130
_exptl_absorpt_coefficient_mu    0.604
_shelx_estimated_absorpt_T_min   0.884
_shelx_estimated_absorpt_T_max   0.926
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_correction_T_min  0.884
_exptl_absorpt_correction_T_max  0.923
_exptl_absorpt_process_details   
; 
CrysAlisPro 1.171.43.125a (Rigaku Oxford Diffraction, 2024) 
Analytical numeric absorption correction using a multifaceted crystal 
model based on expressions derived by R.C. Clark & J.S. Reid. 
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) 
Empirical absorption correction using spherical harmonics, 
implemented in SCALE3 ABSPACK scaling algorithm. 
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Rotating Anode'
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  
; 
Rigaku FRE+ equipped with Arc)Sec VHF Varimax confocal mirrors and an UG2 
goniometer and HyPix 6000HE detector 
;
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_radiation_collimation    0.2
_diffrn_detector_area_resol_mean 10
_diffrn_reflns_number            121756
_diffrn_reflns_av_unetI/netI     0.0262
_diffrn_reflns_av_R_equivalents  0.0445
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -45
_diffrn_reflns_limit_k_max       45
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         1.785
_diffrn_reflns_theta_max         33.184
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             13953
_reflns_number_gt                12120
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
; 
 Reflections were merged by SHELXL according to the crystal 
 class for the calculation of statistics and refinement. 
  
 _reflns_Friedel_fraction is defined as the number of unique 
 Friedel pairs measured divided by the number that would be 
 possible theoretically, ignoring centric projections and 
 systematic absences. 
;

_computing_data_collection       
'CrysAlisPro system (CCD 43.130a 64-bit (release 05-07-2024))'
_computing_cell_refinement       'CrysAlisPro 1.171.43.125a (Rigaku OD, 2024)'
_computing_data_reduction        'CrysAlisPro 1.171.43.125a (Rigaku OD, 2024)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2019/3 (Sheldrick, 2019)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0330P)²+5.2218P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         13953
_refine_ls_number_parameters     475
_refine_ls_number_restraints     182
_refine_ls_R_factor_all          0.0663
_refine_ls_R_factor_gt           0.0567
_refine_ls_wR_factor_ref         0.1274
_refine_ls_wR_factor_gt          0.1233
_refine_ls_goodness_of_fit_ref   1.114
_refine_ls_restrained_S_all      1.141
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
V1 V 0.68568(2) 0.65032(2) 0.54458(3) 0.01757(6) Uani 1 1 d . . . . .
O3 O 0.6980(2) 0.69245(6) 0.4607(2) 0.0533(6) Uani 1 1 d . . . . .
O1 O 0.53061(12) 0.62709(6) 0.45187(16) 0.0360(4) Uani 1 1 d . . . . .
C1 C 0.48036(14) 0.60572(6) 0.33625(18) 0.0214(3) Uani 1 1 d . . . . .
C2 C 0.35890(15) 0.61035(6) 0.25794(18) 0.0217(3) Uani 1 1 d . . . . .
Cl1 Cl 0.27904(4) 0.64470(2) 0.31767(6) 0.03782(13) Uani 1 1 d . . . . .
C3 C 0.30284(15) 0.58815(6) 0.13604(18) 0.0222(3) Uani 1 1 d . . . . .
H3 H 0.221280 0.592305 0.084381 0.027 Uiso 1 1 calc R U . . .
C4 C 0.36696(15) 0.55970(6) 0.08977(17) 0.0200(3) Uani 1 1 d . . . . .
Cl2 Cl 0.29537(4) 0.53061(2) -0.06197(5) 0.03289(11) Uani 1 1 d . . . . .
C5 C 0.48540(14) 0.55345(6) 0.16251(17) 0.0187(3) Uani 1 1 d . . . . .
H5 H 0.528110 0.533723 0.129857 0.022 Uiso 1 1 calc R U . . .
C6 C 0.54206(14) 0.57655(6) 0.28518(17) 0.0202(3) Uani 1 1 d . . . . .
C7 C 0.66610(17) 0.56838(10) 0.3612(2) 0.0411(6) Uani 1 1 d . . . . .
H7 H 0.697219 0.541289 0.342724 0.049 Uiso 1 1 calc R U . . .
N1 N 0.73927(12) 0.59531(5) 0.45362(17) 0.0217(3) Uani 1 1 d . . . . .
C8 C 0.86019(14) 0.57975(6) 0.50663(17) 0.0181(3) Uani 1 1 d . . . . .
C9 C 0.93124(15) 0.59341(6) 0.44070(19) 0.0220(3) Uani 1 1 d . . . . .
C10 C 1.04603(15) 0.57711(6) 0.49112(19) 0.0227(3) Uani 1 1 d . . . . .
H10 H 1.097379 0.586563 0.450667 0.027 Uiso 1 1 calc R U . . .
C11 C 1.08595(15) 0.54733(6) 0.59938(18) 0.0215(3) Uani 1 1 d . . . . .
H11 H 1.163548 0.535897 0.630779 0.026 Uiso 1 1 calc R U . . .
C12 C 1.01360(15) 0.53418(6) 0.66185(18) 0.0213(3) Uani 1 1 d . . . . .
H12 H 1.041893 0.513540 0.735423 0.026 Uiso 1 1 calc R U . . .
C13 C 0.89947(14) 0.55073(6) 0.61864(17) 0.0194(3) Uani 1 1 d . . . . .
C14 C 0.88787(18) 0.62485(8) 0.3187(2) 0.0349(5) Uani 1 1 d D U . . .
H14 H 0.800406 0.622804 0.275993 0.042 Uiso 0.531(19) 1 calc R U P A 1
H14X H 0.805080 0.632434 0.302156 0.042 Uiso 0.469(19) 1 calc R U P A 2
C15 C 0.9362(13) 0.6092(2) 0.2046(7) 0.052(2) Uani 0.531(19) 1 d D U P A 1
H15A H 0.916645 0.577569 0.181621 0.078 Uiso 0.531(19) 1 calc R U P A 1
H15B H 0.899417 0.627654 0.122748 0.078 Uiso 0.531(19) 1 calc R U P A 1
H15C H 1.021420 0.613094 0.241190 0.078 Uiso 0.531(19) 1 calc R U P A 1
C16 C 0.9186(13) 0.6719(2) 0.3500(11) 0.049(2) Uani 0.531(19) 1 d D U P A 1
H16A H 0.887267 0.689565 0.265906 0.074 Uiso 0.531(19) 1 calc R U P A 1
H16B H 0.885110 0.682866 0.412637 0.074 Uiso 0.531(19) 1 calc R U P A 1
H16C H 1.004068 0.675011 0.392432 0.074 Uiso 0.531(19) 1 calc R U P A 1
C15X C 0.8833(9) 0.6051(3) 0.1959(7) 0.0413(16) Uani 0.469(19) 1 d D U P A 2
H15D H 0.854683 0.627265 0.122426 0.062 Uiso 0.469(19) 1 calc R U P A 2
H15E H 0.961900 0.595122 0.208410 0.062 Uiso 0.469(19) 1 calc R U P A 2
H15F H 0.830110 0.579230 0.172425 0.062 Uiso 0.469(19) 1 calc R U P A 2
C16X C 0.9575(6) 0.6695(3) 0.3601(10) 0.0313(15) Uani 0.469(19) 1 d D U P A 2
H16D H 0.955748 0.680480 0.445268 0.047 Uiso 0.469(19) 1 calc R U P A 2
H16E H 1.038860 0.664335 0.372830 0.047 Uiso 0.469(19) 1 calc R U P A 2
H16F H 0.921745 0.691901 0.288400 0.047 Uiso 0.469(19) 1 calc R U P A 2
C17 C 0.82202(17) 0.53652(7) 0.6905(2) 0.0264(4) Uani 1 1 d . U . . .
H17 H 0.753805 0.557589 0.661146 0.032 Uiso 1 1 calc R U . . .
C18 C 0.7736(3) 0.48950(9) 0.6493(4) 0.0558(8) Uani 1 1 d . U . . .
H18A H 0.738325 0.487204 0.549902 0.084 Uiso 1 1 calc R U . . .
H18B H 0.713947 0.483365 0.684767 0.084 Uiso 1 1 calc R U . . .
H18C H 0.837289 0.467589 0.686630 0.084 Uiso 1 1 calc R U . . .
C19 C 0.8852(3) 0.54001(17) 0.8461(3) 0.0731(12) Uani 1 1 d . U . . .
H19A H 0.952206 0.519410 0.878409 0.110 Uiso 1 1 calc R U . . .
H19B H 0.830837 0.532008 0.887625 0.110 Uiso 1 1 calc R U . . .
H19C H 0.912959 0.570846 0.871319 0.110 Uiso 1 1 calc R U . . .
O2 O 0.83102(13) 0.64334(6) 0.69614(19) 0.0448(5) Uani 1 1 d . . . . .
C20 C 0.88170(16) 0.66828(7) 0.8054(2) 0.0261(4) Uani 1 1 d . . . . .
C21 C 1.00455(14) 0.66762(6) 0.87583(17) 0.0185(3) Uani 1 1 d . . . . .
Cl3 Cl 1.08601(4) 0.63510(2) 0.81265(5) 0.02452(9) Uani 1 1 d . . . . .
C22 C 1.06164(15) 0.69240(6) 0.99223(17) 0.0190(3) Uani 1 1 d . . . . .
H22 H 1.144612 0.691264 1.037649 0.023 Uiso 1 1 calc R U . . .
C23 C 0.99661(15) 0.71913(6) 1.04270(17) 0.0195(3) Uani 1 1 d . . . . .
Cl4 Cl 1.06865(4) 0.75007(2) 1.18957(5) 0.03063(10) Uani 1 1 d . . . . .
C24 C 0.87627(16) 0.72104(6) 0.97812(18) 0.0206(3) Uani 1 1 d . . . . .
H24 H 0.832751 0.739440 1.013291 0.025 Uiso 1 1 calc R U . . .
C25 C 0.81854(15) 0.69562(6) 0.8601(2) 0.0252(4) Uani 1 1 d . . . . .
C26 C 0.69146(18) 0.69529(8) 0.8019(3) 0.0394(6) Uani 1 1 d . . . . .
H26 H 0.654262 0.707240 0.856334 0.047 Uiso 1 1 calc R U . . .
N2 N 0.62316(13) 0.68016(5) 0.68183(15) 0.0197(3) Uani 1 1 d . . . . .
C27 C 0.49957(14) 0.67782(6) 0.65761(17) 0.0184(3) Uani 1 1 d . . . . .
C28 C 0.42676(16) 0.71474(6) 0.60250(19) 0.0228(3) Uani 1 1 d . . . . .
C29 C 0.31007(17) 0.71103(7) 0.5853(2) 0.0265(4) Uani 1 1 d . . . . .
H29 H 0.258030 0.735393 0.546726 0.032 Uiso 1 1 calc R U . . .
C30 C 0.26858(18) 0.67261(8) 0.6233(2) 0.0317(4) Uani 1 1 d . . . . .
H30 H 0.189234 0.671020 0.612599 0.038 Uiso 1 1 calc R U . . .
C31 C 0.34277(18) 0.63647(7) 0.6768(2) 0.0308(4) Uani 1 1 d . . . . .
H31 H 0.313703 0.610131 0.702372 0.037 Uiso 1 1 calc R U . . .
C32 C 0.45951(16) 0.63821(6) 0.6937(2) 0.0228(3) Uani 1 1 d . . . . .
C33 C 0.47130(19) 0.75688(7) 0.5602(3) 0.0361(5) Uani 1 1 d D U . . .
H33 H 0.546824 0.748035 0.555169 0.043 Uiso 0.651(10) 1 calc R U P B 1
H33X H 0.556246 0.758927 0.622146 0.043 Uiso 0.349(10) 1 calc R U P B 2
C34 C 0.3907(6) 0.7708(2) 0.4159(4) 0.0580(19) Uani 0.651(10) 1 d D U P B 1
H34A H 0.373320 0.744540 0.355853 0.087 Uiso 0.651(10) 1 calc R U P B 1
H34B H 0.317475 0.782860 0.415685 0.087 Uiso 0.651(10) 1 calc R U P B 1
H34C H 0.429379 0.793801 0.383509 0.087 Uiso 0.651(10) 1 calc R U P B 1
C35 C 0.4997(11) 0.7937(2) 0.6524(6) 0.091(3) Uani 0.651(10) 1 d D U P B 1
H35A H 0.527374 0.818916 0.614806 0.136 Uiso 0.651(10) 1 calc R U P B 1
H35B H 0.429837 0.802789 0.666433 0.136 Uiso 0.651(10) 1 calc R U P B 1
H35C H 0.561397 0.784638 0.739574 0.136 Uiso 0.651(10) 1 calc R U P B 1
C34X C 0.4672(12) 0.7594(3) 0.4347(10) 0.055(3) Uani 0.349(10) 1 d D U P B 2
H34D H 0.498759 0.788374 0.422318 0.082 Uiso 0.349(10) 1 calc R U P B 2
H34E H 0.514048 0.735046 0.420621 0.082 Uiso 0.349(10) 1 calc R U P B 2
H34F H 0.385738 0.756549 0.368773 0.082 Uiso 0.349(10) 1 calc R U P B 2
C35X C 0.4104(18) 0.7997(3) 0.5957(19) 0.087(5) Uani 0.349(10) 1 d D U P B 2
H35D H 0.414859 0.796862 0.688476 0.130 Uiso 0.349(10) 1 calc R U P B 2
H35E H 0.451042 0.827134 0.588497 0.130 Uiso 0.349(10) 1 calc R U P B 2
H35F H 0.328019 0.801324 0.531583 0.130 Uiso 0.349(10) 1 calc R U P B 2
C36 C 0.53885(19) 0.59796(7) 0.7514(3) 0.0342(5) Uani 1 1 d . U . . .
H36 H 0.612724 0.603367 0.738137 0.041 Uiso 1 1 calc R U . . .
C37 C 0.4846(3) 0.55461(9) 0.6770(5) 0.0749(12) Uani 1 1 d . U . . .
H37A H 0.413509 0.547712 0.691245 0.112 Uiso 1 1 calc R U . . .
H37B H 0.540849 0.529967 0.712334 0.112 Uiso 1 1 calc R U . . .
H37C H 0.464491 0.558313 0.579498 0.112 Uiso 1 1 calc R U . . .
C38 C 0.5720(3) 0.59398(15) 0.9051(4) 0.0746(11) Uani 1 1 d . U . . .
H38A H 0.617627 0.620376 0.951365 0.112 Uiso 1 1 calc R U . . .
H38B H 0.618988 0.566816 0.939785 0.112 Uiso 1 1 calc R U . . .
H38C H 0.500587 0.592219 0.922075 0.112 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
V1 O3 1.5880(17) . ?
V1 O2 1.8974(15) . ?
V1 O1 1.9120(14) . ?
V1 N2 2.1212(15) . ?
V1 N1 2.1472(15) . ?
O1 C1 1.309(2) . ?
C1 C6 1.410(2) . ?
C1 C2 1.412(2) . ?
C2 C3 1.380(2) . ?
C2 Cl1 1.7218(18) . ?
C3 C4 1.387(3) . ?
C3 H3 0.9500 . ?
C4 C5 1.377(2) . ?
C4 Cl2 1.7415(17) . ?
C5 C6 1.400(2) . ?
C5 H5 0.9500 . ?
C6 C7 1.449(3) . ?
C7 N1 1.316(3) . ?
C7 H7 0.9500 . ?
N1 C8 1.456(2) . ?
C8 C9 1.399(3) . ?
C8 C13 1.400(2) . ?
C9 C10 1.397(2) . ?
C9 C14 1.522(3) . ?
C10 C11 1.386(3) . ?
C10 H10 0.9500 . ?
C11 C12 1.381(3) . ?
C11 H11 0.9500 . ?
C12 C13 1.397(2) . ?
C12 H12 0.9500 . ?
C13 C17 1.520(3) . ?
C14 C15X 1.425(7) . ?
C14 C16 1.456(8) . ?
C14 C16X 1.552(7) . ?
C14 C15 1.636(8) . ?
C14 H14 1.0000 . ?
C14 H14X 1.0000 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C15X H15D 0.9800 . ?
C15X H15E 0.9800 . ?
C15X H15F 0.9800 . ?
C16X H16D 0.9800 . ?
C16X H16E 0.9800 . ?
C16X H16F 0.9800 . ?
C17 C18 1.518(4) . ?
C17 C19 1.538(3) . ?
C17 H17 1.0000 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
O2 C20 1.316(2) . ?
C20 C21 1.409(2) . ?
C20 C25 1.414(3) . ?
C21 C22 1.378(2) . ?
C21 Cl3 1.7280(17) . ?
C22 C23 1.393(2) . ?
C22 H22 0.9500 . ?
C23 C24 1.377(2) . ?
C23 Cl4 1.7333(17) . ?
C24 C25 1.402(2) . ?
C24 H24 0.9500 . ?
C25 C26 1.450(3) . ?
C26 N2 1.307(3) . ?
C26 H26 0.9500 . ?
N2 C27 1.457(2) . ?
C27 C32 1.396(2) . ?
C27 C28 1.396(2) . ?
C28 C29 1.395(3) . ?
C28 C33 1.514(3) . ?
C29 C30 1.383(3) . ?
C29 H29 0.9500 . ?
C30 C31 1.384(3) . ?
C30 H30 0.9500 . ?
C31 C32 1.393(3) . ?
C31 H31 0.9500 . ?
C32 C36 1.518(3) . ?
C33 C34X 1.331(8) . ?
C33 C35 1.423(5) . ?
C33 C34 1.527(5) . ?
C33 C35X 1.607(9) . ?
C33 H33 1.0000 . ?
C33 H33X 1.0000 . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
C34X H34D 0.9800 . ?
C34X H34E 0.9800 . ?
C34X H34F 0.9800 . ?
C35X H35D 0.9800 . ?
C35X H35E 0.9800 . ?
C35X H35F 0.9800 . ?
C36 C37 1.526(4) . ?
C36 C38 1.537(4) . ?
C36 H36 1.0000 . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?

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
O3 V1 O2 107.22(12) . . ?
O3 V1 O1 107.41(11) . . ?
O2 V1 O1 145.38(9) . . ?
O3 V1 N2 102.16(8) . . ?
O2 V1 N2 86.58(7) . . ?
O1 V1 N2 86.33(6) . . ?
O3 V1 N1 103.00(8) . . ?
O2 V1 N1 86.71(6) . . ?
O1 V1 N1 85.51(6) . . ?
N2 V1 N1 154.83(6) . . ?
C1 O1 V1 131.83(12) . . ?
O1 C1 C6 122.78(15) . . ?
O1 C1 C2 120.43(16) . . ?
C6 C1 C2 116.77(16) . . ?
C3 C2 C1 122.04(16) . . ?
C3 C2 Cl1 119.39(13) . . ?
C1 C2 Cl1 118.57(14) . . ?
C2 C3 C4 119.23(15) . . ?
C2 C3 H3 120.4 . . ?
C4 C3 H3 120.4 . . ?
C5 C4 C3 121.34(16) . . ?
C5 C4 Cl2 119.48(14) . . ?
C3 C4 Cl2 119.17(13) . . ?
C4 C5 C6 119.15(16) . . ?
C4 C5 H5 120.4 . . ?
C6 C5 H5 120.4 . . ?
C5 C6 C1 121.46(15) . . ?
C5 C6 C7 117.86(16) . . ?
C1 C6 C7 120.65(16) . . ?
N1 C7 C6 125.51(19) . . ?
N1 C7 H7 117.2 . . ?
C6 C7 H7 117.2 . . ?
C7 N1 C8 113.25(15) . . ?
C7 N1 V1 124.07(13) . . ?
C8 N1 V1 121.86(11) . . ?
C9 C8 C13 122.77(15) . . ?
C9 C8 N1 118.44(16) . . ?
C13 C8 N1 118.76(16) . . ?
C10 C9 C8 117.46(17) . . ?
C10 C9 C14 120.04(18) . . ?
C8 C9 C14 122.51(16) . . ?
C11 C10 C9 120.86(17) . . ?
C11 C10 H10 119.6 . . ?
C9 C10 H10 119.6 . . ?
C12 C11 C10 120.37(16) . . ?
C12 C11 H11 119.8 . . ?
C10 C11 H11 119.8 . . ?
C11 C12 C13 121.07(17) . . ?
C11 C12 H12 119.5 . . ?
C13 C12 H12 119.5 . . ?
C12 C13 C8 117.40(16) . . ?
C12 C13 C17 120.24(16) . . ?
C8 C13 C17 122.35(15) . . ?
C15X C14 C9 114.3(4) . . ?
C16 C14 C9 115.1(5) . . ?
C15X C14 C16X 115.4(5) . . ?
C9 C14 C16X 108.5(4) . . ?
C16 C14 C15 107.7(4) . . ?
C9 C14 C15 111.1(3) . . ?
C16 C14 H14 107.5 . . ?
C9 C14 H14 107.5 . . ?
C15 C14 H14 107.5 . . ?
C15X C14 H14X 106.0 . . ?
C9 C14 H14X 106.0 . . ?
C16X C14 H14X 106.0 . . ?
C14 C15 H15A 109.5 . . ?
C14 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C14 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C14 C16 H16A 109.5 . . ?
C14 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C14 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C14 C15X H15D 109.5 . . ?
C14 C15X H15E 109.5 . . ?
H15D C15X H15E 109.5 . . ?
C14 C15X H15F 109.5 . . ?
H15D C15X H15F 109.5 . . ?
H15E C15X H15F 109.5 . . ?
C14 C16X H16D 109.5 . . ?
C14 C16X H16E 109.5 . . ?
H16D C16X H16E 109.5 . . ?
C14 C16X H16F 109.5 . . ?
H16D C16X H16F 109.5 . . ?
H16E C16X H16F 109.5 . . ?
C18 C17 C13 111.58(18) . . ?
C18 C17 C19 110.4(3) . . ?
C13 C17 C19 112.43(19) . . ?
C18 C17 H17 107.4 . . ?
C13 C17 H17 107.4 . . ?
C19 C17 H17 107.4 . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C17 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C17 C19 H19A 109.5 . . ?
C17 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C17 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C20 O2 V1 130.79(13) . . ?
O2 C20 C21 119.90(16) . . ?
O2 C20 C25 123.23(16) . . ?
C21 C20 C25 116.85(16) . . ?
C22 C21 C20 122.15(16) . . ?
C22 C21 Cl3 119.11(13) . . ?
C20 C21 Cl3 118.73(13) . . ?
C21 C22 C23 119.40(16) . . ?
C21 C22 H22 120.3 . . ?
C23 C22 H22 120.3 . . ?
C24 C23 C22 120.96(15) . . ?
C24 C23 Cl4 119.75(14) . . ?
C22 C23 Cl4 119.28(13) . . ?
C23 C24 C25 119.43(16) . . ?
C23 C24 H24 120.3 . . ?
C25 C24 H24 120.3 . . ?
C24 C25 C20 121.20(16) . . ?
C24 C25 C26 117.84(17) . . ?
C20 C25 C26 120.76(17) . . ?
N2 C26 C25 126.3(2) . . ?
N2 C26 H26 116.9 . . ?
C25 C26 H26 116.9 . . ?
C26 N2 C27 114.46(16) . . ?
C26 N2 V1 123.73(14) . . ?
C27 N2 V1 120.95(11) . . ?
C32 C27 C28 122.62(16) . . ?
C32 C27 N2 117.51(15) . . ?
C28 C27 N2 119.87(15) . . ?
C29 C28 C27 117.31(17) . . ?
C29 C28 C33 120.99(17) . . ?
C27 C28 C33 121.69(17) . . ?
C30 C29 C28 121.37(18) . . ?
C30 C29 H29 119.3 . . ?
C28 C29 H29 119.3 . . ?
C29 C30 C31 119.92(18) . . ?
C29 C30 H30 120.0 . . ?
C31 C30 H30 120.0 . . ?
C30 C31 C32 120.90(19) . . ?
C30 C31 H31 119.5 . . ?
C32 C31 H31 119.5 . . ?
C31 C32 C27 117.85(17) . . ?
C31 C32 C36 119.91(17) . . ?
C27 C32 C36 122.23(16) . . ?
C34X C33 C28 118.8(5) . . ?
C35 C33 C28 116.6(4) . . ?
C35 C33 C34 112.1(4) . . ?
C28 C33 C34 111.0(2) . . ?
C34X C33 C35X 111.5(6) . . ?
C28 C33 C35X 108.7(4) . . ?
C35 C33 H33 105.4 . . ?
C28 C33 H33 105.4 . . ?
C34 C33 H33 105.4 . . ?
C34X C33 H33X 105.6 . . ?
C28 C33 H33X 105.6 . . ?
C35X C33 H33X 105.6 . . ?
C33 C34 H34A 109.5 . . ?
C33 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
C33 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C33 C35 H35A 109.5 . . ?
C33 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
C33 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C33 C34X H34D 109.5 . . ?
C33 C34X H34E 109.5 . . ?
H34D C34X H34E 109.5 . . ?
C33 C34X H34F 109.5 . . ?
H34D C34X H34F 109.5 . . ?
H34E C34X H34F 109.5 . . ?
C33 C35X H35D 109.5 . . ?
C33 C35X H35E 109.5 . . ?
H35D C35X H35E 109.5 . . ?
C33 C35X H35F 109.5 . . ?
H35D C35X H35F 109.5 . . ?
H35E C35X H35F 109.5 . . ?
C32 C36 C37 112.1(2) . . ?
C32 C36 C38 110.4(2) . . ?
C37 C36 C38 111.6(3) . . ?
C32 C36 H36 107.5 . . ?
C37 C36 H36 107.5 . . ?
C38 C36 H36 107.5 . . ?
C36 C37 H37A 109.5 . . ?
C36 C37 H37B 109.5 . . ?
H37A C37 H37B 109.5 . . ?
C36 C37 H37C 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
C36 C38 H38A 109.5 . . ?
C36 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
C36 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 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
V1 O1 C1 C6 32.0(3) . . . . ?
V1 O1 C1 C2 -149.56(17) . . . . ?
O1 C1 C2 C3 -179.6(2) . . . . ?
C6 C1 C2 C3 -1.1(3) . . . . ?
O1 C1 C2 Cl1 0.2(3) . . . . ?
C6 C1 C2 Cl1 178.68(15) . . . . ?
C1 C2 C3 C4 1.3(3) . . . . ?
Cl1 C2 C3 C4 -178.52(15) . . . . ?
C2 C3 C4 C5 -0.5(3) . . . . ?
C2 C3 C4 Cl2 178.38(15) . . . . ?
C3 C4 C5 C6 -0.4(3) . . . . ?
Cl2 C4 C5 C6 -179.25(14) . . . . ?
C4 C5 C6 C1 0.5(3) . . . . ?
C4 C5 C6 C7 178.4(2) . . . . ?
O1 C1 C6 C5 178.67(19) . . . . ?
C2 C1 C6 C5 0.2(3) . . . . ?
O1 C1 C6 C7 0.8(3) . . . . ?
C2 C1 C6 C7 -177.6(2) . . . . ?
C5 C6 C7 N1 159.1(2) . . . . ?
C1 C6 C7 N1 -23.0(4) . . . . ?
C6 C7 N1 C8 -176.1(2) . . . . ?
C6 C7 N1 V1 14.1(4) . . . . ?
C7 N1 C8 C9 89.6(2) . . . . ?
V1 N1 C8 C9 -100.33(17) . . . . ?
C7 N1 C8 C13 -88.5(2) . . . . ?
V1 N1 C8 C13 81.55(18) . . . . ?
C13 C8 C9 C10 -0.3(3) . . . . ?
N1 C8 C9 C10 -178.34(16) . . . . ?
C13 C8 C9 C14 179.81(18) . . . . ?
N1 C8 C9 C14 1.8(3) . . . . ?
C8 C9 C10 C11 2.2(3) . . . . ?
C14 C9 C10 C11 -177.93(18) . . . . ?
C9 C10 C11 C12 -1.8(3) . . . . ?
C10 C11 C12 C13 -0.6(3) . . . . ?
C11 C12 C13 C8 2.3(3) . . . . ?
C11 C12 C13 C17 -178.83(17) . . . . ?
C9 C8 C13 C12 -1.9(3) . . . . ?
N1 C8 C13 C12 176.12(15) . . . . ?
C9 C8 C13 C17 179.29(17) . . . . ?
N1 C8 C13 C17 -2.7(2) . . . . ?
C10 C9 C14 C15X 64.7(5) . . . . ?
C8 C9 C14 C15X -115.5(5) . . . . ?
C10 C9 C14 C16 -82.6(6) . . . . ?
C8 C9 C14 C16 97.2(6) . . . . ?
C10 C9 C14 C16X -65.6(5) . . . . ?
C8 C9 C14 C16X 114.3(4) . . . . ?
C10 C9 C14 C15 40.1(6) . . . . ?
C8 C9 C14 C15 -140.0(5) . . . . ?
C12 C13 C17 C18 -76.9(3) . . . . ?
C8 C13 C17 C18 101.8(2) . . . . ?
C12 C13 C17 C19 47.8(3) . . . . ?
C8 C13 C17 C19 -133.5(3) . . . . ?
O3 V1 O2 C20 69.4(3) . . . . ?
O1 V1 O2 C20 -110.8(2) . . . . ?
N2 V1 O2 C20 -32.3(2) . . . . ?
N1 V1 O2 C20 172.0(2) . . . . ?
V1 O2 C20 C21 -154.48(18) . . . . ?
V1 O2 C20 C25 27.2(4) . . . . ?
O2 C20 C21 C22 -178.7(2) . . . . ?
C25 C20 C21 C22 -0.2(3) . . . . ?
O2 C20 C21 Cl3 2.1(3) . . . . ?
C25 C20 C21 Cl3 -179.50(16) . . . . ?
C20 C21 C22 C23 -0.1(3) . . . . ?
Cl3 C21 C22 C23 179.18(13) . . . . ?
C21 C22 C23 C24 0.1(3) . . . . ?
C21 C22 C23 Cl4 179.72(14) . . . . ?
C22 C23 C24 C25 0.1(3) . . . . ?
Cl4 C23 C24 C25 -179.44(15) . . . . ?
C23 C24 C25 C20 -0.5(3) . . . . ?
C23 C24 C25 C26 174.5(2) . . . . ?
O2 C20 C25 C24 178.9(2) . . . . ?
C21 C20 C25 C24 0.5(3) . . . . ?
O2 C20 C25 C26 4.0(4) . . . . ?
C21 C20 C25 C26 -174.3(2) . . . . ?
C24 C25 C26 N2 167.6(2) . . . . ?
C20 C25 C26 N2 -17.3(4) . . . . ?
C25 C26 N2 C27 171.3(2) . . . . ?
C25 C26 N2 V1 1.8(4) . . . . ?
C26 N2 C27 C32 -89.3(2) . . . . ?
V1 N2 C27 C32 80.51(19) . . . . ?
C26 N2 C27 C28 89.6(2) . . . . ?
V1 N2 C27 C28 -100.62(17) . . . . ?
C32 C27 C28 C29 0.6(3) . . . . ?
N2 C27 C28 C29 -178.16(17) . . . . ?
C32 C27 C28 C33 -178.15(19) . . . . ?
N2 C27 C28 C33 3.0(3) . . . . ?
C27 C28 C29 C30 1.0(3) . . . . ?
C33 C28 C29 C30 179.8(2) . . . . ?
C28 C29 C30 C31 -1.4(3) . . . . ?
C29 C30 C31 C32 0.2(4) . . . . ?
C30 C31 C32 C27 1.3(3) . . . . ?
C30 C31 C32 C36 -179.4(2) . . . . ?
C28 C27 C32 C31 -1.8(3) . . . . ?
N2 C27 C32 C31 177.05(18) . . . . ?
C28 C27 C32 C36 179.0(2) . . . . ?
N2 C27 C32 C36 -2.2(3) . . . . ?
C29 C28 C33 C34X -90.8(7) . . . . ?
C27 C28 C33 C34X 88.0(7) . . . . ?
C29 C28 C33 C35 80.7(6) . . . . ?
C27 C28 C33 C35 -100.5(6) . . . . ?
C29 C28 C33 C34 -49.3(4) . . . . ?
C27 C28 C33 C34 129.5(4) . . . . ?
C29 C28 C33 C35X 38.2(9) . . . . ?
C27 C28 C33 C35X -143.1(9) . . . . ?
C31 C32 C36 C37 50.9(3) . . . . ?
C27 C32 C36 C37 -129.8(3) . . . . ?
C31 C32 C36 C38 -74.1(3) . . . . ?
C27 C32 C36 C38 105.1(3) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
C24 H24 O3 0.95 2.55 3.358(3) 143.3 4_576 yes

_refine_diff_density_max         1.102
_refine_diff_density_min         -1.070
_refine_diff_density_rms         0.076

_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: acetonitrile'
####################################################################### 
# 
# 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_8
_database_code_depnum_ccdc_archive 'CCDC 2524173'
loop_
_audit_author_name
_audit_author_address
'Mark Elsegood'
;Loughborough University
United Kingdom
;
_audit_update_record             
;
2026-01-19 deposited with the CCDC.	2026-03-10 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2019/3
_shelx_SHELXL_version_number     2019/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C38 H40 Cl4 N2 O3 V'
_chemical_formula_sum            'C38 H40 Cl4 N2 O3 V'
_chemical_formula_weight         765.46

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
V V 0.0687 2.1097 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   8.7572(3)
_cell_length_b                   10.6468(3)
_cell_length_c                   11.3332(3)
_cell_angle_alpha                63.781(3)
_cell_angle_beta                 85.416(2)
_cell_angle_gamma                79.177(3)
_cell_volume                     931.08(5)
_cell_formula_units_Z            1
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    6062
_cell_measurement_theta_min      12.45
_cell_measurement_theta_max      69.29

_exptl_crystal_description       parallelepiped
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.365
_exptl_crystal_F_000             397
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_rad          0.027
_exptl_crystal_size_max          0.140
_exptl_crystal_size_mid          0.030
_exptl_crystal_size_min          0.020
_exptl_absorpt_coefficient_mu    5.173
_shelx_estimated_absorpt_T_min   0.531
_shelx_estimated_absorpt_T_max   0.904
_exptl_absorpt_correction_type   sphere
_exptl_absorpt_correction_T_min  0.725
_exptl_absorpt_correction_T_max  0.740
_exptl_absorpt_process_details   
; 
CrysAlisPro 1.171.43.125a (Rigaku Oxford Diffraction, 2024) 
Spherical absorption correction 
using equivalent radius and absorption coefficient. 
Empirical absorption correction using spherical harmonics, 
implemented in SCALE3 ABSPACK scaling algorithm. 
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_source                   'Rotating anode'
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  
; 
Rigaku 007HF diffractometer with HF Varimax confocal mirrors, 
an UG2 goniometer and HyPix Arc-100 detector 
;
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_radiation_collimation    0.3
_diffrn_detector_area_resol_mean 10
_diffrn_reflns_number            58938
_diffrn_reflns_av_unetI/netI     0.0115
_diffrn_reflns_av_R_equivalents  0.0388
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         4.698
_diffrn_reflns_theta_max         73.291
_diffrn_reflns_theta_full        67.679
_diffrn_measured_fraction_theta_max 0.950
_diffrn_measured_fraction_theta_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.950
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.950
_diffrn_reflns_point_group_measured_fraction_full 0.992
_reflns_number_total             7491
_reflns_number_gt                6971
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
; 
 _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. Completness statistics refer to single and 
 composite reflections containing twin component 1 only. 
;

_computing_data_collection       
'CrysAlisPro system (CCD 43.130a 64-bit (release 05-07-2024))'
_computing_cell_refinement       'CrysAlisPro 1.171.43.125a (Rigaku OD, 2024)'
_computing_data_reduction        'CrysAlisPro 1.171.43.125a (Rigaku OD, 2024)'
_computing_structure_solution    'SHELXT-2018/2 (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2019/3 (Sheldrick, 2019)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          
; 
 Refined as a 2-component twin with twin ratio 0.5854:0.4146(10) via
 a 2.5 degree rotation about [0.96 -0.28 -0.07] (reciprocal)
 or [0.94 -0.34 0.05] (direct).
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0442P)²+0.4650P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     'SHELXL-2019/3 (Sheldrick 2019)'
_refine_ls_extinction_coef       0.0026(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         7491
_refine_ls_number_parameters     232
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0442
_refine_ls_R_factor_gt           0.0413
_refine_ls_wR_factor_ref         0.1038
_refine_ls_wR_factor_gt          0.1021
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_restrained_S_all      1.047
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
V1 V 0.44916(7) 0.52997(7) 0.47953(6) 0.02346(17) Uani 0.5 1 d . . P . .
O2 O 0.2841(3) 0.6232(3) 0.4269(3) 0.0303(6) Uani 0.5 1 d . . P . .
O1 O 0.5897(2) 0.65566(18) 0.42220(15) 0.0416(4) Uani 1 1 d . . . . .
C1 C 0.6289(2) 0.7452(2) 0.4604(2) 0.0296(5) Uani 1 1 d . . . . .
C2 C 0.7133(3) 0.8520(2) 0.3754(2) 0.0347(5) Uani 1 1 d . . . . .
Cl1 Cl 0.76243(10) 0.86031(7) 0.22159(6) 0.0569(2) Uani 1 1 d . . . . .
C3 C 0.7588(3) 0.9467(2) 0.4112(2) 0.0334(5) Uani 1 1 d . . . . .
H3 H 0.816876 1.016070 0.352115 0.040 Uiso 1 1 calc R U . . .
C4 C 0.7193(2) 0.9405(2) 0.5347(2) 0.0298(5) Uani 1 1 d . . . . .
Cl2 Cl 0.77675(7) 1.06078(6) 0.57973(6) 0.03839(16) Uani 1 1 d . . . . .
C5 C 0.6375(2) 0.8392(2) 0.6211(2) 0.0287(4) Uani 1 1 d . . . . .
H5 H 0.610726 0.835775 0.705265 0.034 Uiso 1 1 calc R U . . .
C6 C 0.5932(2) 0.7403(2) 0.5855(2) 0.0261(4) Uani 1 1 d . . . . .
C7 C 0.5140(2) 0.6317(2) 0.6839(2) 0.0310(5) Uani 1 1 d . . . . .
H7 H 0.492173 0.636933 0.765216 0.037 Uiso 1 1 calc R U . . .
N1 N 0.4701(2) 0.52893(19) 0.67211(17) 0.0287(4) Uani 1 1 d . . . . .
C8 C 0.3966(2) 0.4336(2) 0.7896(2) 0.0262(4) Uani 1 1 d . . . . .
C9 C 0.4902(2) 0.3167(2) 0.8849(2) 0.0308(5) Uani 1 1 d . . . . .
C10 C 0.4181(3) 0.2293(2) 0.9981(2) 0.0336(5) Uani 1 1 d . . . . .
H10 H 0.478801 0.148353 1.063605 0.040 Uiso 1 1 calc R U . . .
C11 C 0.2602(3) 0.2584(2) 1.0165(2) 0.0338(5) Uani 1 1 d . . . . .
H11 H 0.213181 0.198537 1.094649 0.041 Uiso 1 1 calc R U . . .
C12 C 0.1705(2) 0.3748(2) 0.9209(2) 0.0322(5) Uani 1 1 d . . . . .
H12 H 0.062029 0.394732 0.934760 0.039 Uiso 1 1 calc R U . . .
C13 C 0.2361(2) 0.4635(2) 0.8046(2) 0.0294(5) Uani 1 1 d . . . . .
C14 C 0.6648(3) 0.2801(3) 0.8702(3) 0.0429(6) Uani 1 1 d . . . . .
H14 H 0.696795 0.354959 0.785557 0.052 Uiso 1 1 calc R U . . .
C15 C 0.7070(3) 0.1367(3) 0.8638(3) 0.0477(6) Uani 1 1 d . . . . .
H15A H 0.679966 0.061200 0.947231 0.072 Uiso 1 1 calc R U . . .
H15B H 0.818854 0.117905 0.848271 0.072 Uiso 1 1 calc R U . . .
H15C H 0.649219 0.139544 0.791904 0.072 Uiso 1 1 calc R U . . .
C16 C 0.7532(3) 0.2786(3) 0.9821(4) 0.0644(9) Uani 1 1 d . . . . .
H16A H 0.728112 0.372082 0.982393 0.097 Uiso 1 1 calc R U . . .
H16B H 0.865188 0.256319 0.969189 0.097 Uiso 1 1 calc R U . . .
H16C H 0.722786 0.206347 1.066254 0.097 Uiso 1 1 calc R U . . .
C17 C 0.1331(3) 0.5873(3) 0.6997(2) 0.0368(5) Uani 1 1 d . . . . .
H17 H 0.199969 0.635012 0.622753 0.044 Uiso 1 1 calc R U . . .
C18 C 0.0081(3) 0.5368(3) 0.6524(3) 0.0601(8) Uani 1 1 d . . . . .
H18A H 0.057427 0.465045 0.622944 0.090 Uiso 1 1 calc R U . . .
H18B H -0.050049 0.617684 0.579250 0.090 Uiso 1 1 calc R U . . .
H18C H -0.063267 0.495292 0.724875 0.090 Uiso 1 1 calc R U . . .
C19 C 0.0579(4) 0.6956(3) 0.7491(3) 0.0566(8) Uani 1 1 d . . . . .
H19A H -0.012103 0.652335 0.822034 0.085 Uiso 1 1 calc R U . . .
H19B H -0.001391 0.777536 0.677535 0.085 Uiso 1 1 calc R U . . .
H19C H 0.138737 0.726883 0.779565 0.085 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
V1 V1 1.0033(13) 2_666 ?
V1 O2 1.583(3) . ?
V1 O1 1.8572(17) . ?
V1 O1 1.8732(17) 2_666 ?
V1 N1 2.1067(18) 2_666 ?
V1 N1 2.1999(19) . ?
O1 C1 1.313(3) . ?
C1 C6 1.407(3) . ?
C1 C2 1.415(3) . ?
C2 C3 1.371(3) . ?
C2 Cl1 1.729(2) . ?
C3 C4 1.390(3) . ?
C3 H3 0.9500 . ?
C4 C5 1.371(3) . ?
C4 Cl2 1.736(2) . ?
C5 C6 1.406(3) . ?
C5 H5 0.9500 . ?
C6 C7 1.449(3) . ?
C7 N1 1.288(3) . ?
C7 H7 0.9500 . ?
N1 C8 1.460(3) . ?
C8 C13 1.395(3) . ?
C8 C9 1.400(3) . ?
C9 C10 1.395(3) . ?
C9 C14 1.520(3) . ?
C10 C11 1.379(3) . ?
C10 H10 0.9500 . ?
C11 C12 1.382(3) . ?
C11 H11 0.9500 . ?
C12 C13 1.393(3) . ?
C12 H12 0.9500 . ?
C13 C17 1.518(3) . ?
C14 C16 1.529(4) . ?
C14 C15 1.534(4) . ?
C14 H14 1.0000 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 C19 1.518(4) . ?
C17 C18 1.531(4) . ?
C17 H17 1.0000 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?

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
V1 V1 O2 175.17(14) 2_666 . ?
V1 V1 O1 75.28(9) 2_666 . ?
O2 V1 O1 106.13(13) . . ?
V1 V1 O1 73.52(9) 2_666 2_666 ?
O2 V1 O1 104.97(13) . 2_666 ?
O1 V1 O1 148.80(5) . 2_666 ?
V1 V1 N1 81.77(9) 2_666 2_666 ?
O2 V1 N1 102.83(12) . 2_666 ?
O1 V1 N1 87.98(7) . 2_666 ?
O1 V1 N1 87.61(7) 2_666 2_666 ?
V1 V1 N1 71.40(8) 2_666 . ?
O2 V1 N1 103.99(12) . . ?
O1 V1 N1 85.29(7) . . ?
O1 V1 N1 84.87(7) 2_666 . ?
N1 V1 N1 153.17(4) 2_666 . ?
C1 O1 V1 135.19(15) . . ?
C1 O1 V1 130.46(14) . 2_666 ?
O1 C1 C6 123.22(19) . . ?
O1 C1 C2 120.3(2) . . ?
C6 C1 C2 116.51(19) . . ?
C3 C2 C1 122.5(2) . . ?
C3 C2 Cl1 119.34(17) . . ?
C1 C2 Cl1 118.15(17) . . ?
C2 C3 C4 119.5(2) . . ?
C2 C3 H3 120.2 . . ?
C4 C3 H3 120.2 . . ?
C5 C4 C3 120.4(2) . . ?
C5 C4 Cl2 120.15(17) . . ?
C3 C4 Cl2 119.41(17) . . ?
C4 C5 C6 120.2(2) . . ?
C4 C5 H5 119.9 . . ?
C6 C5 H5 119.9 . . ?
C5 C6 C1 120.86(19) . . ?
C5 C6 C7 117.25(19) . . ?
C1 C6 C7 121.86(19) . . ?
N1 C7 C6 126.6(2) . . ?
N1 C7 H7 116.7 . . ?
C6 C7 H7 116.7 . . ?
C7 N1 C8 114.13(17) . . ?
C7 N1 V1 122.49(14) . 2_666 ?
C8 N1 V1 121.34(13) . 2_666 ?
C7 N1 V1 122.21(15) . . ?
C8 N1 V1 121.68(13) . . ?
C13 C8 C9 122.12(19) . . ?
C13 C8 N1 119.09(18) . . ?
C9 C8 N1 118.77(18) . . ?
C10 C9 C8 117.80(19) . . ?
C10 C9 C14 118.9(2) . . ?
C8 C9 C14 123.3(2) . . ?
C11 C10 C9 121.1(2) . . ?
C11 C10 H10 119.4 . . ?
C9 C10 H10 119.4 . . ?
C10 C11 C12 119.9(2) . . ?
C10 C11 H11 120.1 . . ?
C12 C11 H11 120.1 . . ?
C11 C12 C13 121.3(2) . . ?
C11 C12 H12 119.4 . . ?
C13 C12 H12 119.4 . . ?
C12 C13 C8 117.7(2) . . ?
C12 C13 C17 119.83(19) . . ?
C8 C13 C17 122.44(19) . . ?
C9 C14 C16 111.3(2) . . ?
C9 C14 C15 110.5(2) . . ?
C16 C14 C15 110.6(2) . . ?
C9 C14 H14 108.1 . . ?
C16 C14 H14 108.1 . . ?
C15 C14 H14 108.1 . . ?
C14 C15 H15A 109.5 . . ?
C14 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C14 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C14 C16 H16A 109.5 . . ?
C14 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C14 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C19 C17 C13 111.1(2) . . ?
C19 C17 C18 110.0(2) . . ?
C13 C17 C18 111.5(2) . . ?
C19 C17 H17 108.0 . . ?
C13 C17 H17 108.0 . . ?
C18 C17 H17 108.0 . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C17 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C17 C19 H19A 109.5 . . ?
C17 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C17 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 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
V1 V1 O1 C1 -96.6(2) 2_666 . . . ?
O2 V1 O1 C1 78.6(2) . . . . ?
O1 V1 O1 C1 -96.6(2) 2_666 . . . ?
N1 V1 O1 C1 -178.6(2) 2_666 . . . ?
N1 V1 O1 C1 -24.6(2) . . . . ?
O2 V1 O1 V1 175.20(15) . . . 2_666 ?
O1 V1 O1 V1 -0.002(1) 2_666 . . 2_666 ?
N1 V1 O1 V1 -82.02(9) 2_666 . . 2_666 ?
N1 V1 O1 V1 71.98(8) . . . 2_666 ?
V1 O1 C1 C6 17.1(4) . . . . ?
V1 O1 C1 C6 -25.5(3) 2_666 . . . ?
V1 O1 C1 C2 -163.90(18) . . . . ?
V1 O1 C1 C2 153.54(18) 2_666 . . . ?
O1 C1 C2 C3 -179.1(2) . . . . ?
C6 C1 C2 C3 0.0(3) . . . . ?
O1 C1 C2 Cl1 -0.1(3) . . . . ?
C6 C1 C2 Cl1 179.02(16) . . . . ?
C1 C2 C3 C4 -1.1(4) . . . . ?
Cl1 C2 C3 C4 179.89(18) . . . . ?
C2 C3 C4 C5 1.0(3) . . . . ?
C2 C3 C4 Cl2 -179.89(17) . . . . ?
C3 C4 C5 C6 0.2(3) . . . . ?
Cl2 C4 C5 C6 -178.95(15) . . . . ?
C4 C5 C6 C1 -1.3(3) . . . . ?
C4 C5 C6 C7 176.95(19) . . . . ?
O1 C1 C6 C5 -179.7(2) . . . . ?
C2 C1 C6 C5 1.2(3) . . . . ?
O1 C1 C6 C7 2.1(3) . . . . ?
C2 C1 C6 C7 -177.0(2) . . . . ?
C5 C6 C7 N1 -177.0(2) . . . . ?
C1 C6 C7 N1 1.3(3) . . . . ?
C6 C7 N1 C8 178.39(19) . . . . ?
C6 C7 N1 V1 14.5(3) . . . 2_666 ?
C6 C7 N1 V1 -17.4(3) . . . . ?
C7 N1 C8 C13 89.4(2) . . . . ?
V1 N1 C8 C13 -106.47(19) 2_666 . . . ?
V1 N1 C8 C13 -74.9(2) . . . . ?
C7 N1 C8 C9 -89.2(2) . . . . ?
V1 N1 C8 C9 75.0(2) 2_666 . . . ?
V1 N1 C8 C9 106.54(19) . . . . ?
C13 C8 C9 C10 -0.3(3) . . . . ?
N1 C8 C9 C10 178.22(19) . . . . ?
C13 C8 C9 C14 179.0(2) . . . . ?
N1 C8 C9 C14 -2.5(3) . . . . ?
C8 C9 C10 C11 -1.1(3) . . . . ?
C14 C9 C10 C11 179.6(2) . . . . ?
C9 C10 C11 C12 0.9(3) . . . . ?
C10 C11 C12 C13 0.7(3) . . . . ?
C11 C12 C13 C8 -2.0(3) . . . . ?
C11 C12 C13 C17 177.7(2) . . . . ?
C9 C8 C13 C12 1.8(3) . . . . ?
N1 C8 C13 C12 -176.71(19) . . . . ?
C9 C8 C13 C17 -177.9(2) . . . . ?
N1 C8 C13 C17 3.6(3) . . . . ?
C10 C9 C14 C16 -59.7(3) . . . . ?
C8 C9 C14 C16 121.0(3) . . . . ?
C10 C9 C14 C15 63.6(3) . . . . ?
C8 C9 C14 C15 -115.7(3) . . . . ?
C12 C13 C17 C19 64.3(3) . . . . ?
C8 C13 C17 C19 -115.9(3) . . . . ?
C12 C13 C17 C18 -58.8(3) . . . . ?
C8 C13 C17 C18 120.9(3) . . . . ?

_refine_diff_density_max         0.334
_refine_diff_density_min         -0.561
_refine_diff_density_rms         0.050

_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: acetonitrile'
