# 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_pMeL3H
_database_code_depnum_ccdc_archive 'CCDC 2418239'
loop_
_audit_author_name
_audit_author_address
'Timothy Prior'
;University of Hull
United Kingdom
;
_audit_update_record             
;
2025-01-20 deposited with the CCDC.	2025-12-16 downloaded from the CCDC.
;

_audit_creation_date             2023-06-26
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C29 H34 N2 O'
_chemical_formula_sum            'C29 H34 N2 O'
_chemical_formula_weight         426.58
_chemical_melting_point          ?
_chemical_oxdiff_formula         C63O3N4H64
_chemical_oxdiff_usercomment     'Me o-tBuV'
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'

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

_cell_length_a                   10.4654(2)
_cell_length_b                   14.8091(2)
_cell_length_c                   16.8078(3)
_cell_angle_alpha                74.785(2)
_cell_angle_beta                 81.0860(10)
_cell_angle_gamma                80.4970(10)
_cell_volume                     2462.01(8)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    23242
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      76.6000
_cell_measurement_theta_min      3.0910
_shelx_estimated_absorpt_T_max   0.982
_shelx_estimated_absorpt_T_min   0.897
_exptl_absorpt_coefficient_mu    0.533
_exptl_absorpt_correction_T_max  0.983
_exptl_absorpt_correction_T_min  0.901
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.94a (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   ?
_exptl_crystal_colour            'light yellow'
_exptl_crystal_density_diffrn    1.151
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             920
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 -5 7 0.0867
7 3 4 0.0608
1 -8 -8 0.0113
0 8 8 0.0174
-5 -6 -7 0.0560
0 5 -7 0.1034
-5 5 -3 0.0761
-6 2 2 0.0864
-5 -3 -9 0.0670

_exptl_crystal_size_max          0.208
_exptl_crystal_size_mid          0.155
_exptl_crystal_size_min          0.034
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
0.4502 -5.4446 7.0267 -0.9478 -0.2825 -0.1478
6.5822 3.0977 3.9999 0.1782 -0.6075 -0.7741
0.5794 -7.8880 -7.5711 -0.2475 0.8259 -0.5065
-0.0599 8.0111 7.7690 0.2576 -0.8608 0.4389
-4.9057 -6.4221 -6.9748 -0.2654 0.8960 0.3560
-0.0556 5.3397 -7.1636 0.9551 0.2840 0.0842
-4.9382 4.7312 -2.6738 0.5081 0.1485 0.8484
-6.1100 1.5902 2.4452 -0.1371 -0.0439 0.9896
-4.6938 -2.7622 -8.9598 0.2089 0.8797 0.4272

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0554
_diffrn_reflns_av_unetI/netI     0.0465
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.954
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            47699
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.954
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.010
_diffrn_reflns_theta_min         2.743
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.954
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -82.00  -9.00   0.50    1.00    --  -45.18 114.00  92.00  146
  2  ω      4.00  82.00   0.50    1.00    --   45.18-114.00   2.00  156
  3  ω    -97.00 -27.00   0.50    4.00    --  -97.00 114.00  92.00  140
  4  ω   -166.00-100.00   0.50    4.00    --  -97.00-114.00   2.00  132
  5  ω     94.00 175.00   0.50    4.00    --  109.75 114.00  92.00  162
  6  ω     40.00  97.00   0.50    4.00    --  109.75-114.00   2.00  114
  7  ω    -65.00  18.00   0.50    1.00    --  -45.18  77.00  30.00  166
  8  ω    -30.00  15.00   0.50    1.00    --   45.18 -38.00 150.00   90
  9  ω    -30.00  15.00   0.50    1.00    --   45.18 -38.00 -90.00   90
 10  ω    -30.00  15.00   0.50    1.00    --   45.18 -38.00  30.00   90
 11  ω    -30.00  15.00   0.50    1.00    --   45.18 -38.00-150.00   90
 12  ω     39.00 120.00   0.50    1.00    --   45.18  38.00 150.00  162
 13  ω    -30.00  15.00   0.50    1.00    --   45.18 -38.00-120.00   90
 14  ω    -30.00  15.00   0.50    1.00    --   45.18 -38.00 -60.00   90
 15  ω    -30.00  15.00   0.50    1.00    --   45.18 -38.00   0.00   90
 16  ω    -93.00 -23.00   0.50    4.00    --  -97.00  93.00-105.70  140
 17  ω   -167.00 -94.00   0.50    4.00    --  -97.00-125.00-180.00  146
 18  ω   -140.00 -90.00   0.50    4.00    --  -97.00 -15.00 -30.00  100
 19  ω    -97.00 -27.00   0.50    4.00    --  -97.00 114.00   2.75  140
 20  ω    -93.00 -23.00   0.50    4.00    --  -97.00  93.00 154.40  140
 21  ω   -140.00 -90.00   0.50    4.00    --  -97.00 -15.00-120.00  100
 22  ω    -55.00 -23.00   0.50    4.00    --  -97.00  61.00 120.00   64
 23  ω    -55.00 -23.00   0.50    4.00    --  -97.00  61.00 -30.00   64
 24  ω    -92.00 -23.00   0.50    4.00    --  -97.00  94.00  32.40  138
 25  ω    -93.00 -25.00   0.50    4.00    --  -97.00  97.00 -22.41  136
 26  ω    -93.00 -23.00   0.50    4.00    --  -97.00  93.00-154.69  140
 27  ω    -93.00 -25.00   0.50    4.00    --  -97.00  97.00 108.97  136
 28  ω    -93.00 -23.00   0.50    4.00    --  -97.00  93.00-170.26  140
 29  ω    -55.00 -23.00   0.50    4.00    --  -97.00  61.00 -60.00   64
 30  ω    -55.00 -23.00   0.50    4.00    --  -97.00  61.00-120.00   64
 31  ω   -170.00 -90.00   0.50    4.00    --  -97.00 -30.00-120.00  160
 32  ω    -93.00 -25.00   0.50    4.00    --  -97.00  97.00 -37.78  136
 33  ω    -93.00 -23.00   0.50    4.00    --  -97.00  93.00  89.64  140
 34  ω     39.00 100.00   0.50    4.00    --  109.75-125.00 120.00  122
 35  ω     39.00 100.00   0.50    4.00    --  109.75-125.00-150.00  122
 36  ω    102.00 175.00   0.50    4.00    --  109.75  45.00   0.00  146
 37  ω    104.00 162.00   0.50    4.00    --  109.75  30.00 -30.00  116
 38  ω     37.00  93.00   0.50    4.00    --  109.75 -95.00 -60.00  112
 39  ω     37.00  93.00   0.50    4.00    --  109.75 -95.00-180.00  112
 40  ω    104.00 162.00   0.50    4.00    --  109.75  30.00  90.00  116
 41  ω     37.00  93.00   0.50    4.00    --  109.75 -95.00   0.00  112
 42  ω     37.00  71.00   0.50    4.00    --  109.75 -77.00 120.00   68
 43  ω    104.00 132.00   0.50    4.00    --  109.75  15.00 120.00   56
 44  ω     37.00  93.00   0.50    4.00    --  109.75 -95.00-150.00  112
 45  ω    104.00 132.00   0.50    4.00    --  109.75  15.00-150.00   56
 46  ω     37.00  93.00   0.50    4.00    --  109.75 -95.00  30.00  112
 47  ω     45.00  85.00   0.50    4.00    --  109.75 -95.00  90.00   80
 48  ω     43.00  92.00   0.50    4.00    --  109.75 -95.00 -90.00   98
 49  ω     38.00  65.00   0.50    4.00    --  109.75 -77.00  30.00   54
 50  ω     52.00  92.00   0.50    4.00    --  109.75 -95.00-120.00   80
 51  ω    105.00 131.00   0.50    4.00    --  109.75  15.00  90.00   52
 52  ω     37.00  62.00   0.50    4.00    --  109.75 -77.00  60.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'ROD, Synergy Custom system, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0214660000
_diffrn_orient_matrix_UB_12      0.0939029000
_diffrn_orient_matrix_UB_13      -0.0635039000
_diffrn_orient_matrix_UB_21      -0.0311021000
_diffrn_orient_matrix_UB_22      -0.0403268000
_diffrn_orient_matrix_UB_23      -0.0694566000
_diffrn_orient_matrix_UB_31      -0.1454618000
_diffrn_orient_matrix_UB_32      0.0371454000
_diffrn_orient_matrix_UB_33      0.0170700000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                8356
_reflns_number_total             9932
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.42.94a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.94a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.94a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.310
_refine_diff_density_min         -0.239
_refine_diff_density_rms         0.046
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     593
_refine_ls_number_reflns         9932
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0543
_refine_ls_R_factor_gt           0.0461
_refine_ls_restrained_S_all      1.039
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0763P)²+0.3374P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1233
_refine_ls_wR_factor_ref         0.1299
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C8(H8), C11(H11), C12(H12), C13(H13), C14(H14), C19(H19),
 C22(H22), C23(H23), C24(H24), C25(H25), C33(H33), C35(H35), C38(H38), C41(H41),
  C42(H42), C43(H43), C44(H44), C49(H49), C52(H52), C53(H53), C54(H54), C55(H55)
2.b Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C18(H18A,H18B,
 H18C), C27(H27A,H27B,H27C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C), C37(H37A,
 H37B,H37C), C46(H46A,H46B,H46C), C47(H47A,H47B,H47C), C48(H48A,H48B,H48C),
 C57(H57A,H57B,H57C), C58(H58A,H58B,H58C), C59(H59A,H59B,H59C)
2.c Idealised tetrahedral OH refined as rotating group:
 O1(H1), O2(H2)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
O1 O 0.22013(8) -0.04542(6) 0.94283(6) 0.03087(19) Uani 1 1 d . . . . .
H1 H 0.261913 -0.099162 0.958732 0.046 Uiso 1 1 calc R U . . .
N1 N 0.33321(9) -0.18976(7) 1.04522(7) 0.0292(2) Uani 1 1 d . . . . .
N2 N 0.00700(10) 0.21769(7) 0.90514(7) 0.0291(2) Uani 1 1 d . . . . .
C1 C 0.18295(11) -0.00617(8) 1.00793(8) 0.0277(2) Uani 1 1 d . . . . .
C2 C 0.10762(11) 0.08320(9) 0.99610(8) 0.0288(3) Uani 1 1 d . . . . .
C3 C 0.06642(12) 0.12195(9) 1.06446(8) 0.0306(3) Uani 1 1 d . . . . .
H3 H 0.013779 0.181625 1.056492 0.037 Uiso 1 1 calc R U . . .
C4 C 0.09893(12) 0.07719(9) 1.14364(8) 0.0322(3) Uani 1 1 d . . . . .
C5 C 0.17684(12) -0.00983(9) 1.15345(8) 0.0313(3) Uani 1 1 d . . . . .
H5 H 0.202567 -0.040967 1.206675 0.038 Uiso 1 1 calc R U . . .
C6 C 0.21841(11) -0.05286(8) 1.08768(8) 0.0287(3) Uani 1 1 d . . . . .
C7 C 0.05395(16) 0.12263(10) 1.21498(9) 0.0414(3) Uani 1 1 d . . . . .
H7A H 0.078049 0.078400 1.266605 0.062 Uiso 1 1 calc R U . . .
H7B H -0.041022 0.139353 1.219208 0.062 Uiso 1 1 calc R U . . .
H7C H 0.095486 0.179767 1.205680 0.062 Uiso 1 1 calc R U . . .
C8 C 0.29715(11) -0.14525(9) 1.10254(8) 0.0289(3) Uani 1 1 d . . . . .
H8 H 0.322527 -0.173342 1.156370 0.035 Uiso 1 1 calc R U . . .
C9 C 0.40501(12) -0.28197(9) 1.06427(8) 0.0294(3) Uani 1 1 d . . . . .
C10 C 0.50169(12) -0.31146(9) 1.00438(8) 0.0324(3) Uani 1 1 d . . . . .
C11 C 0.56415(14) -0.40391(10) 1.02700(9) 0.0373(3) Uani 1 1 d . . . . .
H11 H 0.630187 -0.426031 0.988458 0.045 Uiso 1 1 calc R U . . .
C12 C 0.53360(14) -0.46449(10) 1.10331(10) 0.0394(3) Uani 1 1 d . . . . .
H12 H 0.578034 -0.526951 1.115971 0.047 Uiso 1 1 calc R U . . .
C13 C 0.43880(13) -0.43454(9) 1.16116(9) 0.0364(3) Uani 1 1 d . . . . .
H13 H 0.418045 -0.475717 1.213782 0.044 Uiso 1 1 calc R U . . .
C14 C 0.37456(12) -0.34349(9) 1.14110(9) 0.0325(3) Uani 1 1 d . . . . .
H14 H 0.308617 -0.322491 1.180282 0.039 Uiso 1 1 calc R U . . .
C15 C 0.53907(14) -0.24657(10) 0.91884(9) 0.0379(3) Uani 1 1 d . . . . .
C16 C 0.57797(14) -0.15462(10) 0.92830(10) 0.0409(3) Uani 1 1 d . . . . .
H16A H 0.609960 -0.117236 0.873685 0.061 Uiso 1 1 calc R U . . .
H16B H 0.646920 -0.169672 0.964863 0.061 Uiso 1 1 calc R U . . .
H16C H 0.501850 -0.118317 0.952383 0.061 Uiso 1 1 calc R U . . .
C17 C 0.42489(16) -0.22654(11) 0.86612(9) 0.0432(3) Uani 1 1 d . . . . .
H17A H 0.345849 -0.200512 0.896482 0.065 Uiso 1 1 calc R U . . .
H17B H 0.410157 -0.285390 0.854782 0.065 Uiso 1 1 calc R U . . .
H17C H 0.446058 -0.180972 0.813574 0.065 Uiso 1 1 calc R U . . .
C18 C 0.65718(17) -0.29316(12) 0.87043(11) 0.0523(4) Uani 1 1 d . . . . .
H18A H 0.635428 -0.350992 0.860772 0.078 Uiso 1 1 calc R U . . .
H18B H 0.731667 -0.308737 0.902669 0.078 Uiso 1 1 calc R U . . .
H18C H 0.679677 -0.249435 0.817019 0.078 Uiso 1 1 calc R U . . .
C19 C 0.07556(11) 0.13670(9) 0.91332(8) 0.0289(3) Uani 1 1 d . . . . .
H19 H 0.105474 0.111374 0.866327 0.035 Uiso 1 1 calc R U . . .
C20 C -0.02522(11) 0.27265(9) 0.82672(8) 0.0280(2) Uani 1 1 d . . . . .
C21 C -0.04307(11) 0.37230(9) 0.81312(8) 0.0291(3) Uani 1 1 d . . . . .
C22 C -0.08233(12) 0.42402(9) 0.73652(8) 0.0316(3) Uani 1 1 d . . . . .
H22 H -0.092953 0.490974 0.724934 0.038 Uiso 1 1 calc R U . . .
C23 C -0.10647(12) 0.38184(9) 0.67668(8) 0.0325(3) Uani 1 1 d . . . . .
H23 H -0.134215 0.419720 0.625771 0.039 Uiso 1 1 calc R U . . .
C24 C -0.08997(12) 0.28428(9) 0.69142(8) 0.0316(3) Uani 1 1 d . . . . .
H24 H -0.106601 0.254682 0.650989 0.038 Uiso 1 1 calc R U . . .
C25 C -0.04877(11) 0.23044(9) 0.76617(8) 0.0294(3) Uani 1 1 d . . . . .
H25 H -0.036353 0.163570 0.776307 0.035 Uiso 1 1 calc R U . . .
C26 C -0.02407(12) 0.42193(9) 0.87940(8) 0.0322(3) Uani 1 1 d . . . . .
C27 C 0.11285(13) 0.39071(9) 0.90830(9) 0.0348(3) Uani 1 1 d . . . . .
H27A H 0.121554 0.323397 0.936268 0.052 Uiso 1 1 calc R U . . .
H27B H 0.124649 0.427253 0.946904 0.052 Uiso 1 1 calc R U . . .
H27C H 0.179283 0.401662 0.860065 0.052 Uiso 1 1 calc R U . . .
C28 C -0.03777(14) 0.52973(9) 0.84581(10) 0.0391(3) Uani 1 1 d . . . . .
H28A H 0.026350 0.545971 0.796991 0.059 Uiso 1 1 calc R U . . .
H28B H -0.022494 0.559044 0.888828 0.059 Uiso 1 1 calc R U . . .
H28C H -0.125895 0.552879 0.830191 0.059 Uiso 1 1 calc R U . . .
C29 C -0.12891(13) 0.40019(10) 0.95460(9) 0.0366(3) Uani 1 1 d . . . . .
H29A H -0.215587 0.424430 0.936884 0.055 Uiso 1 1 calc R U . . .
H29B H -0.114721 0.430539 0.997188 0.055 Uiso 1 1 calc R U . . .
H29C H -0.123050 0.331779 0.977505 0.055 Uiso 1 1 calc R U . . .
O2 O 0.32322(9) 0.45809(6) 0.45050(6) 0.0316(2) Uani 1 1 d . . . . .
H2 H 0.295768 0.405319 0.466681 0.047 Uiso 1 1 calc R U . . .
N3 N 0.23112(10) 0.31431(7) 0.55429(7) 0.0297(2) Uani 1 1 d . . . . .
N4 N 0.43308(10) 0.72038(7) 0.40803(7) 0.0303(2) Uani 1 1 d . . . . .
C31 C 0.31621(11) 0.49628(8) 0.51557(8) 0.0282(2) Uani 1 1 d . . . . .
C32 C 0.35564(11) 0.58570(8) 0.50240(8) 0.0295(3) Uani 1 1 d . . . . .
C33 C 0.35040(12) 0.62430(9) 0.57037(8) 0.0316(3) Uani 1 1 d . . . . .
H33 H 0.378885 0.684242 0.561310 0.038 Uiso 1 1 calc R U . . .
C34 C 0.30527(12) 0.57875(9) 0.65080(8) 0.0330(3) Uani 1 1 d . . . . .
C35 C 0.26353(12) 0.49128(9) 0.66236(8) 0.0312(3) Uani 1 1 d . . . . .
H35 H 0.230545 0.459430 0.716567 0.037 Uiso 1 1 calc R U . . .
C36 C 0.26866(11) 0.44879(8) 0.59658(8) 0.0293(3) Uani 1 1 d . . . . .
C37 C 0.30206(15) 0.62401(10) 0.72169(9) 0.0404(3) Uani 1 1 d . . . . .
H37A H 0.244211 0.684055 0.712147 0.061 Uiso 1 1 calc R U . . .
H37B H 0.390285 0.635543 0.725338 0.061 Uiso 1 1 calc R U . . .
H37C H 0.269618 0.581886 0.773700 0.061 Uiso 1 1 calc R U . . .
C38 C 0.22401(11) 0.35685(9) 0.61249(8) 0.0296(3) Uani 1 1 d . . . . .
H38 H 0.188912 0.327840 0.667096 0.036 Uiso 1 1 calc R U . . .
C39 C 0.19139(11) 0.22287(8) 0.57238(8) 0.0291(3) Uani 1 1 d . . . . .
C40 C 0.12853(12) 0.19758(9) 0.51426(8) 0.0303(3) Uani 1 1 d . . . . .
C41 C 0.09885(13) 0.10516(9) 0.53492(9) 0.0351(3) Uani 1 1 d . . . . .
H41 H 0.056098 0.085780 0.497501 0.042 Uiso 1 1 calc R U . . .
C42 C 0.12922(14) 0.04028(9) 0.60797(9) 0.0377(3) Uani 1 1 d . . . . .
H42 H 0.108376 -0.022238 0.619251 0.045 Uiso 1 1 calc R U . . .
C43 C 0.18967(13) 0.06675(9) 0.66406(9) 0.0358(3) Uani 1 1 d . . . . .
H43 H 0.209826 0.023020 0.714405 0.043 Uiso 1 1 calc R U . . .
C44 C 0.22057(12) 0.15790(9) 0.64603(8) 0.0323(3) Uani 1 1 d . . . . .
H44 H 0.262301 0.176480 0.684400 0.039 Uiso 1 1 calc R U . . .
C45 C 0.09229(13) 0.26698(9) 0.43282(8) 0.0338(3) Uani 1 1 d . . . . .
C46 C 0.01197(13) 0.35863(9) 0.44945(9) 0.0349(3) Uani 1 1 d . . . . .
H46A H 0.065285 0.391138 0.473164 0.052 Uiso 1 1 calc R U . . .
H46B H -0.065614 0.343252 0.488567 0.052 Uiso 1 1 calc R U . . .
H46C H -0.014830 0.399757 0.397184 0.052 Uiso 1 1 calc R U . . .
C47 C 0.21749(15) 0.28830(10) 0.37338(9) 0.0397(3) Uani 1 1 d . . . . .
H47A H 0.194729 0.336082 0.323272 0.060 Uiso 1 1 calc R U . . .
H47B H 0.261154 0.230397 0.358064 0.060 Uiso 1 1 calc R U . . .
H47C H 0.276116 0.311970 0.401039 0.060 Uiso 1 1 calc R U . . .
C48 C 0.00754(16) 0.22577(11) 0.38827(10) 0.0449(3) Uani 1 1 d . . . . .
H48A H -0.072774 0.210766 0.424623 0.067 Uiso 1 1 calc R U . . .
H48B H 0.055603 0.168147 0.374514 0.067 Uiso 1 1 calc R U . . .
H48C H -0.014458 0.272012 0.337161 0.067 Uiso 1 1 calc R U . . .
C49 C 0.39863(11) 0.63915(9) 0.41820(8) 0.0296(3) Uani 1 1 d . . . . .
H49 H 0.400694 0.613318 0.371835 0.036 Uiso 1 1 calc R U . . .
C50 C 0.47581(11) 0.77503(9) 0.32870(8) 0.0292(3) Uani 1 1 d . . . . .
C51 C 0.45841(12) 0.87462(9) 0.31605(8) 0.0308(3) Uani 1 1 d . . . . .
C52 C 0.50878(12) 0.92636(9) 0.23848(9) 0.0337(3) Uani 1 1 d . . . . .
H52 H 0.497137 0.993276 0.227684 0.040 Uiso 1 1 calc R U . . .
C53 C 0.57512(12) 0.88396(10) 0.17655(9) 0.0352(3) Uani 1 1 d . . . . .
H53 H 0.608641 0.921642 0.124968 0.042 Uiso 1 1 calc R U . . .
C54 C 0.59211(12) 0.78644(10) 0.19044(9) 0.0336(3) Uani 1 1 d . . . . .
H54 H 0.637721 0.756728 0.148704 0.040 Uiso 1 1 calc R U . . .
C55 C 0.54176(12) 0.73287(9) 0.26592(8) 0.0306(3) Uani 1 1 d . . . . .
H55 H 0.552249 0.666103 0.275252 0.037 Uiso 1 1 calc R U . . .
C56 C 0.38895(13) 0.92430(9) 0.38372(9) 0.0346(3) Uani 1 1 d . . . . .
C57 C 0.46539(14) 0.89671(10) 0.45994(9) 0.0386(3) Uani 1 1 d . . . . .
H57A H 0.475572 0.827979 0.481294 0.058 Uiso 1 1 calc R U . . .
H57B H 0.417498 0.926657 0.503237 0.058 Uiso 1 1 calc R U . . .
H57C H 0.551614 0.917970 0.443685 0.058 Uiso 1 1 calc R U . . .
C58 C 0.37753(16) 1.03213(10) 0.35310(10) 0.0447(3) Uani 1 1 d . . . . .
H58A H 0.464954 1.051408 0.337200 0.067 Uiso 1 1 calc R U . . .
H58B H 0.331955 1.061031 0.397609 0.067 Uiso 1 1 calc R U . . .
H58C H 0.328401 1.052822 0.304939 0.067 Uiso 1 1 calc R U . . .
C59 C 0.24926(14) 0.89865(10) 0.41076(9) 0.0388(3) Uani 1 1 d . . . . .
H59A H 0.201145 0.915370 0.362223 0.058 Uiso 1 1 calc R U . . .
H59B H 0.204903 0.933550 0.451529 0.058 Uiso 1 1 calc R U . . .
H59C H 0.252901 0.830709 0.435708 0.058 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
O1 H1 0.8400 . ?
O1 C1 1.3467(15) . ?
N1 C8 1.2820(17) . ?
N1 C9 1.4276(15) . ?
N2 C19 1.2775(16) . ?
N2 C20 1.4133(16) . ?
C1 C2 1.4065(17) . ?
C1 C6 1.4127(17) . ?
C2 C3 1.3951(18) . ?
C2 C19 1.4678(17) . ?
C3 H3 0.9500 . ?
C3 C4 1.3889(18) . ?
C4 C5 1.3914(18) . ?
C4 C7 1.5021(19) . ?
C5 H5 0.9500 . ?
C5 C6 1.3952(19) . ?
C6 C8 1.4580(17) . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 H8 0.9500 . ?
C9 C10 1.4131(19) . ?
C9 C14 1.3965(18) . ?
C10 C11 1.3980(18) . ?
C10 C15 1.5390(19) . ?
C11 H11 0.9500 . ?
C11 C12 1.384(2) . ?
C12 H12 0.9500 . ?
C12 C13 1.381(2) . ?
C13 H13 0.9500 . ?
C13 C14 1.3842(18) . ?
C14 H14 0.9500 . ?
C15 C16 1.537(2) . ?
C15 C17 1.541(2) . ?
C15 C18 1.539(2) . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 H19 0.9500 . ?
C20 C21 1.4178(17) . ?
C20 C25 1.3962(18) . ?
C21 C22 1.3984(18) . ?
C21 C26 1.5387(18) . ?
C22 H22 0.9500 . ?
C22 C23 1.3877(19) . ?
C23 H23 0.9500 . ?
C23 C24 1.3863(19) . ?
C24 H24 0.9500 . ?
C24 C25 1.3887(18) . ?
C25 H25 0.9500 . ?
C26 C27 1.5433(18) . ?
C26 C28 1.5376(18) . ?
C26 C29 1.542(2) . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
O2 H2 0.8400 . ?
O2 C31 1.3444(16) . ?
N3 C38 1.2826(17) . ?
N3 C39 1.4245(16) . ?
N4 C49 1.2738(17) . ?
N4 C50 1.4145(16) . ?
C31 C32 1.4040(17) . ?
C31 C36 1.4140(18) . ?
C32 C33 1.3956(19) . ?
C32 C49 1.4711(18) . ?
C33 H33 0.9500 . ?
C33 C34 1.3908(19) . ?
C34 C35 1.3910(19) . ?
C34 C37 1.507(2) . ?
C35 H35 0.9500 . ?
C35 C36 1.3988(19) . ?
C36 C38 1.4573(17) . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C38 H38 0.9500 . ?
C39 C40 1.4142(19) . ?
C39 C44 1.3950(18) . ?
C40 C41 1.3956(18) . ?
C40 C45 1.5387(18) . ?
C41 H41 0.9500 . ?
C41 C42 1.390(2) . ?
C42 H42 0.9500 . ?
C42 C43 1.380(2) . ?
C43 H43 0.9500 . ?
C43 C44 1.3847(18) . ?
C44 H44 0.9500 . ?
C45 C46 1.5416(18) . ?
C45 C47 1.5427(19) . ?
C45 C48 1.531(2) . ?
C46 H46A 0.9800 . ?
C46 H46B 0.9800 . ?
C46 H46C 0.9800 . ?
C47 H47A 0.9800 . ?
C47 H47B 0.9800 . ?
C47 H47C 0.9800 . ?
C48 H48A 0.9800 . ?
C48 H48B 0.9800 . ?
C48 H48C 0.9800 . ?
C49 H49 0.9500 . ?
C50 C51 1.4185(17) . ?
C50 C55 1.3990(19) . ?
C51 C52 1.4003(18) . ?
C51 C56 1.5395(19) . ?
C52 H52 0.9500 . ?
C52 C53 1.391(2) . ?
C53 H53 0.9500 . ?
C53 C54 1.3866(19) . ?
C54 H54 0.9500 . ?
C54 C55 1.3853(19) . ?
C55 H55 0.9500 . ?
C56 C57 1.544(2) . ?
C56 C58 1.5342(18) . ?
C56 C59 1.5411(19) . ?
C57 H57A 0.9800 . ?
C57 H57B 0.9800 . ?
C57 H57C 0.9800 . ?
C58 H58A 0.9800 . ?
C58 H58B 0.9800 . ?
C58 H58C 0.9800 . ?
C59 H59A 0.9800 . ?
C59 H59B 0.9800 . ?
C59 H59C 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 109.5 . . ?
C8 N1 C9 119.63(11) . . ?
C19 N2 C20 121.58(11) . . ?
O1 C1 C2 119.26(11) . . ?
O1 C1 C6 121.29(11) . . ?
C2 C1 C6 119.44(12) . . ?
C1 C2 C19 121.18(12) . . ?
C3 C2 C1 118.76(11) . . ?
C3 C2 C19 120.04(11) . . ?
C2 C3 H3 118.5 . . ?
C4 C3 C2 122.95(11) . . ?
C4 C3 H3 118.5 . . ?
C3 C4 C5 117.34(12) . . ?
C3 C4 C7 120.91(12) . . ?
C5 C4 C7 121.74(12) . . ?
C4 C5 H5 118.9 . . ?
C4 C5 C6 122.15(12) . . ?
C6 C5 H5 118.9 . . ?
C1 C6 C8 121.23(12) . . ?
C5 C6 C1 119.32(11) . . ?
C5 C6 C8 119.45(11) . . ?
C4 C7 H7A 109.5 . . ?
C4 C7 H7B 109.5 . . ?
C4 C7 H7C 109.5 . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
N1 C8 C6 122.04(11) . . ?
N1 C8 H8 119.0 . . ?
C6 C8 H8 119.0 . . ?
C10 C9 N1 120.02(11) . . ?
C14 C9 N1 119.18(11) . . ?
C14 C9 C10 120.74(11) . . ?
C9 C10 C15 122.86(11) . . ?
C11 C10 C9 116.34(12) . . ?
C11 C10 C15 120.79(12) . . ?
C10 C11 H11 118.7 . . ?
C12 C11 C10 122.61(13) . . ?
C12 C11 H11 118.7 . . ?
C11 C12 H12 119.8 . . ?
C13 C12 C11 120.31(12) . . ?
C13 C12 H12 119.8 . . ?
C12 C13 H13 120.6 . . ?
C12 C13 C14 118.85(13) . . ?
C14 C13 H13 120.6 . . ?
C9 C14 H14 119.4 . . ?
C13 C14 C9 121.14(13) . . ?
C13 C14 H14 119.4 . . ?
C10 C15 C17 109.68(12) . . ?
C16 C15 C10 110.72(12) . . ?
C16 C15 C17 111.34(12) . . ?
C16 C15 C18 106.57(13) . . ?
C18 C15 C10 111.62(11) . . ?
C18 C15 C17 106.82(13) . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C15 C17 H17A 109.5 . . ?
C15 C17 H17B 109.5 . . ?
C15 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C15 C18 H18A 109.5 . . ?
C15 C18 H18B 109.5 . . ?
C15 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
N2 C19 C2 119.29(12) . . ?
N2 C19 H19 120.4 . . ?
C2 C19 H19 120.4 . . ?
N2 C20 C21 118.26(11) . . ?
C25 C20 N2 121.12(11) . . ?
C25 C20 C21 120.44(11) . . ?
C20 C21 C26 122.34(11) . . ?
C22 C21 C20 116.51(12) . . ?
C22 C21 C26 121.14(11) . . ?
C21 C22 H22 118.6 . . ?
C23 C22 C21 122.90(12) . . ?
C23 C22 H22 118.6 . . ?
C22 C23 H23 120.1 . . ?
C24 C23 C22 119.80(12) . . ?
C24 C23 H23 120.1 . . ?
C23 C24 H24 120.5 . . ?
C23 C24 C25 119.02(12) . . ?
C25 C24 H24 120.5 . . ?
C20 C25 H25 119.3 . . ?
C24 C25 C20 121.31(12) . . ?
C24 C25 H25 119.3 . . ?
C21 C26 C27 111.38(10) . . ?
C21 C26 C29 109.92(11) . . ?
C28 C26 C21 111.49(11) . . ?
C28 C26 C27 106.99(11) . . ?
C28 C26 C29 107.34(11) . . ?
C29 C26 C27 109.59(11) . . ?
C26 C27 H27A 109.5 . . ?
C26 C27 H27B 109.5 . . ?
C26 C27 H27C 109.5 . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C26 C28 H28A 109.5 . . ?
C26 C28 H28B 109.5 . . ?
C26 C28 H28C 109.5 . . ?
H28A C28 H28B 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C26 C29 H29A 109.5 . . ?
C26 C29 H29B 109.5 . . ?
C26 C29 H29C 109.5 . . ?
H29A C29 H29B 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C31 O2 H2 109.5 . . ?
C38 N3 C39 120.06(11) . . ?
C49 N4 C50 122.04(11) . . ?
O2 C31 C32 119.13(11) . . ?
O2 C31 C36 121.40(11) . . ?
C32 C31 C36 119.47(12) . . ?
C31 C32 C49 120.73(12) . . ?
C33 C32 C31 118.91(12) . . ?
C33 C32 C49 120.34(11) . . ?
C32 C33 H33 118.6 . . ?
C34 C33 C32 122.81(12) . . ?
C34 C33 H33 118.6 . . ?
C33 C34 C35 117.48(12) . . ?
C33 C34 C37 120.34(12) . . ?
C35 C34 C37 122.17(12) . . ?
C34 C35 H35 119.0 . . ?
C34 C35 C36 121.99(12) . . ?
C36 C35 H35 119.0 . . ?
C31 C36 C38 121.13(12) . . ?
C35 C36 C31 119.31(11) . . ?
C35 C36 C38 119.56(12) . . ?
C34 C37 H37A 109.5 . . ?
C34 C37 H37B 109.5 . . ?
C34 C37 H37C 109.5 . . ?
H37A C37 H37B 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
N3 C38 C36 121.36(12) . . ?
N3 C38 H38 119.3 . . ?
C36 C38 H38 119.3 . . ?
C40 C39 N3 119.94(11) . . ?
C44 C39 N3 119.15(12) . . ?
C44 C39 C40 120.84(12) . . ?
C39 C40 C45 122.89(11) . . ?
C41 C40 C39 116.28(12) . . ?
C41 C40 C45 120.82(12) . . ?
C40 C41 H41 118.6 . . ?
C42 C41 C40 122.75(13) . . ?
C42 C41 H41 118.6 . . ?
C41 C42 H42 120.0 . . ?
C43 C42 C41 119.95(12) . . ?
C43 C42 H42 120.0 . . ?
C42 C43 H43 120.4 . . ?
C42 C43 C44 119.14(13) . . ?
C44 C43 H43 120.4 . . ?
C39 C44 H44 119.5 . . ?
C43 C44 C39 121.03(13) . . ?
C43 C44 H44 119.5 . . ?
C40 C45 C46 111.08(11) . . ?
C40 C45 C47 109.58(11) . . ?
C46 C45 C47 110.89(11) . . ?
C48 C45 C40 111.71(11) . . ?
C48 C45 C46 106.20(11) . . ?
C48 C45 C47 107.28(12) . . ?
C45 C46 H46A 109.5 . . ?
C45 C46 H46B 109.5 . . ?
C45 C46 H46C 109.5 . . ?
H46A C46 H46B 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
C45 C47 H47A 109.5 . . ?
C45 C47 H47B 109.5 . . ?
C45 C47 H47C 109.5 . . ?
H47A C47 H47B 109.5 . . ?
H47A C47 H47C 109.5 . . ?
H47B C47 H47C 109.5 . . ?
C45 C48 H48A 109.5 . . ?
C45 C48 H48B 109.5 . . ?
C45 C48 H48C 109.5 . . ?
H48A C48 H48B 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?
N4 C49 C32 119.38(12) . . ?
N4 C49 H49 120.3 . . ?
C32 C49 H49 120.3 . . ?
N4 C50 C51 117.99(12) . . ?
C55 C50 N4 121.54(11) . . ?
C55 C50 C51 120.31(12) . . ?
C50 C51 C56 122.32(11) . . ?
C52 C51 C50 116.58(12) . . ?
C52 C51 C56 121.10(11) . . ?
C51 C52 H52 118.6 . . ?
C53 C52 C51 122.81(12) . . ?
C53 C52 H52 118.6 . . ?
C52 C53 H53 120.2 . . ?
C54 C53 C52 119.70(12) . . ?
C54 C53 H53 120.2 . . ?
C53 C54 H54 120.4 . . ?
C55 C54 C53 119.20(13) . . ?
C55 C54 H54 120.4 . . ?
C50 C55 H55 119.3 . . ?
C54 C55 C50 121.39(12) . . ?
C54 C55 H55 119.3 . . ?
C51 C56 C57 110.79(11) . . ?
C51 C56 C59 110.57(11) . . ?
C58 C56 C51 111.99(11) . . ?
C58 C56 C57 106.78(12) . . ?
C58 C56 C59 107.07(11) . . ?
C59 C56 C57 109.50(12) . . ?
C56 C57 H57A 109.5 . . ?
C56 C57 H57B 109.5 . . ?
C56 C57 H57C 109.5 . . ?
H57A C57 H57B 109.5 . . ?
H57A C57 H57C 109.5 . . ?
H57B C57 H57C 109.5 . . ?
C56 C58 H58A 109.5 . . ?
C56 C58 H58B 109.5 . . ?
C56 C58 H58C 109.5 . . ?
H58A C58 H58B 109.5 . . ?
H58A C58 H58C 109.5 . . ?
H58B C58 H58C 109.5 . . ?
C56 C59 H59A 109.5 . . ?
C56 C59 H59B 109.5 . . ?
C56 C59 H59C 109.5 . . ?
H59A C59 H59B 109.5 . . ?
H59A C59 H59C 109.5 . . ?
H59B C59 H59C 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 178.14(11) . . . . ?
O1 C1 C2 C19 -3.70(17) . . . . ?
O1 C1 C6 C5 -179.50(11) . . . . ?
O1 C1 C6 C8 0.26(18) . . . . ?
N1 C9 C10 C11 -177.81(12) . . . . ?
N1 C9 C10 C15 2.78(19) . . . . ?
N1 C9 C14 C13 177.92(12) . . . . ?
N2 C20 C21 C22 -176.36(11) . . . . ?
N2 C20 C21 C26 2.11(17) . . . . ?
N2 C20 C25 C24 175.11(11) . . . . ?
C1 C2 C3 C4 1.51(19) . . . . ?
C1 C2 C19 N2 -179.92(11) . . . . ?
C1 C6 C8 N1 -2.83(18) . . . . ?
C2 C1 C6 C5 0.67(17) . . . . ?
C2 C1 C6 C8 -179.57(11) . . . . ?
C2 C3 C4 C5 0.42(19) . . . . ?
C2 C3 C4 C7 178.98(13) . . . . ?
C3 C2 C19 N2 -1.78(18) . . . . ?
C3 C4 C5 C6 -1.86(19) . . . . ?
C4 C5 C6 C1 1.34(19) . . . . ?
C4 C5 C6 C8 -178.43(11) . . . . ?
C5 C6 C8 N1 176.93(11) . . . . ?
C6 C1 C2 C3 -2.03(17) . . . . ?
C6 C1 C2 C19 176.14(11) . . . . ?
C7 C4 C5 C6 179.59(12) . . . . ?
C8 N1 C9 C10 -145.87(12) . . . . ?
C8 N1 C9 C14 36.84(17) . . . . ?
C9 N1 C8 C6 -177.05(11) . . . . ?
C9 C10 C11 C12 0.5(2) . . . . ?
C9 C10 C15 C16 55.01(17) . . . . ?
C9 C10 C15 C17 -68.25(17) . . . . ?
C9 C10 C15 C18 173.57(13) . . . . ?
C10 C9 C14 C13 0.65(19) . . . . ?
C10 C11 C12 C13 -0.5(2) . . . . ?
C11 C10 C15 C16 -124.37(14) . . . . ?
C11 C10 C15 C17 112.36(14) . . . . ?
C11 C10 C15 C18 -5.82(19) . . . . ?
C11 C12 C13 C14 0.5(2) . . . . ?
C12 C13 C14 C9 -0.6(2) . . . . ?
C14 C9 C10 C11 -0.56(18) . . . . ?
C14 C9 C10 C15 -179.97(12) . . . . ?
C15 C10 C11 C12 179.91(13) . . . . ?
C19 N2 C20 C21 -150.15(12) . . . . ?
C19 N2 C20 C25 34.67(17) . . . . ?
C19 C2 C3 C4 -176.68(12) . . . . ?
C20 N2 C19 C2 179.18(11) . . . . ?
C20 C21 C22 C23 1.61(18) . . . . ?
C20 C21 C26 C27 55.57(16) . . . . ?
C20 C21 C26 C28 175.00(11) . . . . ?
C20 C21 C26 C29 -66.10(15) . . . . ?
C21 C20 C25 C24 0.03(18) . . . . ?
C21 C22 C23 C24 -0.9(2) . . . . ?
C22 C21 C26 C27 -126.03(13) . . . . ?
C22 C21 C26 C28 -6.60(17) . . . . ?
C22 C21 C26 C29 112.31(13) . . . . ?
C22 C23 C24 C25 -0.29(19) . . . . ?
C23 C24 C25 C20 0.71(18) . . . . ?
C25 C20 C21 C22 -1.15(17) . . . . ?
C25 C20 C21 C26 177.32(11) . . . . ?
C26 C21 C22 C23 -176.88(12) . . . . ?
O2 C31 C32 C33 -178.85(10) . . . . ?
O2 C31 C32 C49 2.70(17) . . . . ?
O2 C31 C36 C35 179.84(11) . . . . ?
O2 C31 C36 C38 -0.68(17) . . . . ?
N3 C39 C40 C41 176.82(11) . . . . ?
N3 C39 C40 C45 -3.89(18) . . . . ?
N3 C39 C44 C43 -176.68(11) . . . . ?
N4 C50 C51 C52 176.27(11) . . . . ?
N4 C50 C51 C56 -3.25(17) . . . . ?
N4 C50 C55 C54 -175.07(11) . . . . ?
C31 C32 C33 C34 -1.29(18) . . . . ?
C31 C32 C49 N4 179.55(11) . . . . ?
C31 C36 C38 N3 2.80(17) . . . . ?
C32 C31 C36 C35 -0.90(17) . . . . ?
C32 C31 C36 C38 178.59(10) . . . . ?
C32 C33 C34 C35 -0.30(18) . . . . ?
C32 C33 C34 C37 179.95(12) . . . . ?
C33 C32 C49 N4 1.13(17) . . . . ?
C33 C34 C35 C36 1.33(18) . . . . ?
C34 C35 C36 C31 -0.74(18) . . . . ?
C34 C35 C36 C38 179.77(11) . . . . ?
C35 C36 C38 N3 -177.72(11) . . . . ?
C36 C31 C32 C33 1.87(17) . . . . ?
C36 C31 C32 C49 -176.58(10) . . . . ?
C37 C34 C35 C36 -178.93(12) . . . . ?
C38 N3 C39 C40 143.91(12) . . . . ?
C38 N3 C39 C44 -38.96(16) . . . . ?
C39 N3 C38 C36 177.56(10) . . . . ?
C39 C40 C41 C42 -0.39(19) . . . . ?
C39 C40 C45 C46 -53.06(16) . . . . ?
C39 C40 C45 C47 69.81(15) . . . . ?
C39 C40 C45 C48 -171.44(12) . . . . ?
C40 C39 C44 C43 0.42(19) . . . . ?
C40 C41 C42 C43 0.9(2) . . . . ?
C41 C40 C45 C46 126.19(13) . . . . ?
C41 C40 C45 C47 -110.94(13) . . . . ?
C41 C40 C45 C48 7.82(17) . . . . ?
C41 C42 C43 C44 -0.7(2) . . . . ?
C42 C43 C44 C39 0.1(2) . . . . ?
C44 C39 C40 C41 -0.26(18) . . . . ?
C44 C39 C40 C45 179.02(11) . . . . ?
C45 C40 C41 C42 -179.70(12) . . . . ?
C49 N4 C50 C51 153.12(12) . . . . ?
C49 N4 C50 C55 -31.41(17) . . . . ?
C49 C32 C33 C34 177.16(11) . . . . ?
C50 N4 C49 C32 179.76(10) . . . . ?
C50 C51 C52 C53 -1.26(19) . . . . ?
C50 C51 C56 C57 63.47(16) . . . . ?
C50 C51 C56 C58 -177.43(12) . . . . ?
C50 C51 C56 C59 -58.12(16) . . . . ?
C51 C50 C55 C54 0.30(18) . . . . ?
C51 C52 C53 C54 0.7(2) . . . . ?
C52 C51 C56 C57 -116.03(13) . . . . ?
C52 C51 C56 C58 3.07(18) . . . . ?
C52 C51 C56 C59 122.38(13) . . . . ?
C52 C53 C54 C55 0.38(19) . . . . ?
C53 C54 C55 C50 -0.88(18) . . . . ?
C55 C50 C51 C52 0.74(17) . . . . ?
C55 C50 C51 C56 -178.78(11) . . . . ?
C56 C51 C52 C53 178.27(12) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 3.286
_oxdiff_exptl_absorpt_empirical_full_min 0.542
####################################################################### 
# 
# 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_14
_database_code_depnum_ccdc_archive 'CCDC 2418244'
loop_
_audit_author_name
_audit_author_address
'Timothy Prior'
;University of Hull
United Kingdom
;
_audit_update_record             
;
2025-01-20 deposited with the CCDC.	2025-12-16 downloaded from the CCDC.
;
_audit_creation_date             2025-01-16
_audit_creation_method           
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C48 H38 F4 I4 N4 O3 V, C2 H3 N'
_chemical_formula_sum            'C50 H41 F4 I4 N5 O3 V'
_chemical_formula_weight         1394.42
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 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'
F F 0.0727 0.0534 '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'

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

_cell_length_a                   11.4085(3)
_cell_length_b                   13.1317(4)
_cell_length_c                   17.4790(4)
_cell_angle_alpha                78.084(2)
_cell_angle_beta                 86.776(2)
_cell_angle_gamma                89.036(3)
_cell_volume                     2558.06(12)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    11484
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      70.23
_cell_measurement_theta_min      2.59
_shelx_estimated_absorpt_T_max   0.486
_shelx_estimated_absorpt_T_min   0.156
_exptl_absorpt_coefficient_mu    21.078
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.579
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.43.131a (Rigaku Oxford Diffraction, 2024) 
Empirical absorption correction using spherical harmonics, 
implemented in SCALE3 ABSPACK scaling algorithm. 
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.810
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blade
_exptl_crystal_F_000             1342
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.04
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0596
_diffrn_reflns_av_unetI/netI     0.0499
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.933
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            46832
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.933
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         73.432
_diffrn_reflns_theta_min         2.587
_diffrn_ambient_temperature      100.15
_diffrn_detector_area_resol_mean 10
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.933
_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_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                7851
_reflns_number_total             9620
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.43.131a (Rigaku OD, 2024)'
_computing_data_collection       
'CrysAlisPro system (CCD 43.131a 64-bit (release 19-07-2024))'
_computing_data_reduction        'CrysAlisPro 1.171.43.131a (Rigaku OD, 2024)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT-2018/2 (Sheldrick, 2015)'
_refine_diff_density_max         2.176
_refine_diff_density_min         -1.554
_refine_diff_density_rms         0.132
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     611
_refine_ls_number_reflns         9620
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0682
_refine_ls_R_factor_gt           0.0572
_refine_ls_restrained_S_all      1.048
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0821P)²+7.0433P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1508
_refine_ls_wR_factor_ref         0.1586
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C11(H11), C14(H14), C16(H16), C17(H17), C18(H18), C21(H21),
 C23(H23), C24(H24), C27(H27), C29(H29), C35(H35), C38(H38), C40(H40), C41(H41),
  C42(H42), C45(H45), C47(H47), C48(H48)
2.b Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C32(H32A,H32B,H32C),
 C33(H33A,H33B,H33C), C34(H34A,H34B,H34C), C50(H50A,H50B,H50C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
V1 V 0.83293(9) 0.36232(8) 0.55824(6) 0.0395(2) Uani 1 1 d . . . . .
O3 O 0.9728(4) 0.3747(3) 0.5508(3) 0.0477(10) Uani 1 1 d . . . . .
O1 O 0.7604(4) 0.3724(3) 0.4610(2) 0.0401(9) Uani 1 1 d . . . . .
C1 C 0.7779(5) 0.4487(5) 0.3995(3) 0.0376(12) Uani 1 1 d . . . . .
C2 C 0.7789(5) 0.4278(5) 0.3231(4) 0.0397(13) Uani 1 1 d . . . . .
C3 C 0.8043(5) 0.5072(5) 0.2582(4) 0.0427(14) Uani 1 1 d . . . . .
H3 H 0.804286 0.491585 0.207529 0.051 Uiso 1 1 calc R U . . .
C4 C 0.8297(5) 0.6084(5) 0.2644(3) 0.0409(13) Uani 1 1 d . . . . .
C5 C 0.8226(5) 0.6300(5) 0.3393(4) 0.0419(13) Uani 1 1 d . . . . .
H5 H 0.836099 0.699002 0.345368 0.050 Uiso 1 1 calc R U . . .
C6 C 0.7959(5) 0.5519(5) 0.4066(3) 0.0370(12) Uani 1 1 d . . . . .
C7 C 0.8618(7) 0.6926(5) 0.1920(4) 0.0515(16) Uani 1 1 d . . . . .
C8 C 0.9698(7) 0.6536(7) 0.1478(4) 0.0614(19) Uani 1 1 d . . . . .
H8A H 0.990710 0.705614 0.100394 0.092 Uiso 1 1 calc R U . . .
H8B H 0.950635 0.587802 0.133427 0.092 Uiso 1 1 calc R U . . .
H8C H 1.036299 0.642784 0.181827 0.092 Uiso 1 1 calc R U . . .
C9 C 0.7593(8) 0.7093(6) 0.1380(5) 0.063(2) Uani 1 1 d . . . . .
H9A H 0.691413 0.736395 0.164501 0.095 Uiso 1 1 calc R U . . .
H9B H 0.738787 0.642861 0.125072 0.095 Uiso 1 1 calc R U . . .
H9C H 0.782057 0.759230 0.089800 0.095 Uiso 1 1 calc R U . . .
C10 C 0.8958(8) 0.7943(6) 0.2118(5) 0.063(2) Uani 1 1 d . . . . .
H10A H 0.828759 0.822254 0.238639 0.094 Uiso 1 1 calc R U . . .
H10B H 0.918734 0.844058 0.163558 0.094 Uiso 1 1 calc R U . . .
H10C H 0.961853 0.782629 0.246121 0.094 Uiso 1 1 calc R U . . .
C11 C 0.7918(5) 0.5841(5) 0.4804(3) 0.0378(12) Uani 1 1 d . . . . .
H11 H 0.787872 0.656633 0.479511 0.045 Uiso 1 1 calc R U . . .
N1 N 0.7931(4) 0.5212(4) 0.5480(3) 0.0394(11) Uani 1 1 d . . . . .
C12 C 0.7913(5) 0.5692(5) 0.6144(3) 0.0379(12) Uani 1 1 d . . . . .
C13 C 0.6908(6) 0.6169(5) 0.6404(4) 0.0430(14) Uani 1 1 d . . . . .
I1 I 0.52983(4) 0.61073(4) 0.58805(3) 0.05323(14) Uani 1 1 d . . . . .
C14 C 0.6924(6) 0.6643(5) 0.7041(4) 0.0442(14) Uani 1 1 d . . . . .
H14 H 0.623955 0.696241 0.722275 0.053 Uiso 1 1 calc R U . . .
C15 C 0.7958(7) 0.6637(5) 0.7399(4) 0.0494(15) Uani 1 1 d . . . . .
F1 F 0.7982(4) 0.7127(3) 0.8011(3) 0.0629(11) Uani 1 1 d . . . . .
C16 C 0.8955(6) 0.6158(6) 0.7188(4) 0.0514(16) Uani 1 1 d . . . . .
H16 H 0.964624 0.614851 0.746777 0.062 Uiso 1 1 calc R U . . .
C17 C 0.8927(6) 0.5681(5) 0.6548(4) 0.0488(15) Uani 1 1 d . . . . .
H17 H 0.961128 0.534319 0.638604 0.059 Uiso 1 1 calc R U . . .
C18 C 0.7508(6) 0.3225(5) 0.3146(4) 0.0419(13) Uani 1 1 d . . . . .
H18 H 0.730451 0.270930 0.359921 0.050 Uiso 1 1 calc R U . . .
N2 N 0.7533(5) 0.2991(4) 0.2479(3) 0.0478(13) Uani 1 1 d . . . . .
C19 C 0.7116(7) 0.2004(5) 0.2411(4) 0.0486(16) Uani 1 1 d . . . . .
C20 C 0.7703(7) 0.1486(6) 0.1875(4) 0.0546(17) Uani 1 1 d . . . . .
I2 I 0.92362(6) 0.21347(5) 0.12690(3) 0.0788(2) Uani 1 1 d . . . . .
C21 C 0.7283(10) 0.0557(6) 0.1754(4) 0.068(2) Uani 1 1 d . . . . .
H21 H 0.768173 0.020075 0.139393 0.082 Uiso 1 1 calc R U . . .
C22 C 0.6277(10) 0.0159(6) 0.2165(5) 0.073(3) Uani 1 1 d . . . . .
F2 F 0.5865(6) -0.0761(4) 0.2024(3) 0.0907(18) Uani 1 1 d . . . . .
C23 C 0.5667(8) 0.0634(6) 0.2683(5) 0.063(2) Uani 1 1 d . . . . .
H23 H 0.496507 0.033991 0.295160 0.075 Uiso 1 1 calc R U . . .
C24 C 0.6102(7) 0.1561(6) 0.2808(4) 0.0538(17) Uani 1 1 d . . . . .
H24 H 0.569621 0.190176 0.317410 0.065 Uiso 1 1 calc R U . . .
O2 O 0.7574(4) 0.3415(3) 0.6599(2) 0.0452(10) Uani 1 1 d . . . . .
C25 C 0.7544(6) 0.2601(5) 0.7196(4) 0.0443(14) Uani 1 1 d . . . . .
C26 C 0.7171(6) 0.2739(5) 0.7952(4) 0.0478(15) Uani 1 1 d . . . . .
C27 C 0.7179(7) 0.1897(6) 0.8580(4) 0.0562(18) Uani 1 1 d . . . . .
H27 H 0.696575 0.201136 0.908942 0.067 Uiso 1 1 calc R U . . .
C28 C 0.7485(6) 0.0888(5) 0.8498(4) 0.0493(16) Uani 1 1 d . . . . .
C29 C 0.7802(6) 0.0763(6) 0.7756(4) 0.0482(15) Uani 1 1 d . . . . .
H29 H 0.800128 0.008486 0.767839 0.058 Uiso 1 1 calc R U . . .
C30 C 0.7846(6) 0.1600(5) 0.7101(4) 0.0448(14) Uani 1 1 d . . . . .
C31 C 0.7492(7) -0.0012(6) 0.9211(4) 0.0597(19) Uani 1 1 d . . . . .
C32 C 0.6436(9) 0.0048(10) 0.9751(6) 0.107(5) Uani 1 1 d . . . . .
H32A H 0.572277 0.007777 0.945936 0.161 Uiso 1 1 calc R U . . .
H32B H 0.648207 0.067421 0.997055 0.161 Uiso 1 1 calc R U . . .
H32C H 0.641169 -0.056933 1.017690 0.161 Uiso 1 1 calc R U . . .
C33 C 0.8610(8) 0.0057(6) 0.9637(4) 0.063(2) Uani 1 1 d . . . . .
H33A H 0.857183 -0.044409 1.013767 0.095 Uiso 1 1 calc R U . . .
H33B H 0.868372 0.076243 0.973271 0.095 Uiso 1 1 calc R U . . .
H33C H 0.929157 -0.010105 0.931410 0.095 Uiso 1 1 calc R U . . .
C34 C 0.7460(14) -0.1061(8) 0.8984(6) 0.111(5) Uani 1 1 d . . . . .
H34A H 0.807130 -0.109247 0.857266 0.167 Uiso 1 1 calc R U . . .
H34B H 0.668922 -0.115940 0.878938 0.167 Uiso 1 1 calc R U . . .
H34C H 0.759709 -0.161095 0.944268 0.167 Uiso 1 1 calc R U . . .
C35 C 0.8190(6) 0.1344(5) 0.6361(4) 0.0438(14) Uani 1 1 d . . . . .
H35 H 0.829877 0.062869 0.634972 0.053 Uiso 1 1 calc R U . . .
N3 N 0.8363(5) 0.2010(4) 0.5706(3) 0.0424(11) Uani 1 1 d . . . . .
C36 C 0.8733(6) 0.1565(5) 0.5037(4) 0.0422(13) Uani 1 1 d . . . . .
C37 C 0.7996(6) 0.0961(5) 0.4725(4) 0.0482(15) Uani 1 1 d . . . . .
I3 I 0.62648(4) 0.06967(4) 0.51567(3) 0.06481(16) Uani 1 1 d . . . . .
C38 C 0.8379(7) 0.0524(5) 0.4087(4) 0.0506(16) Uani 1 1 d . . . . .
H38 H 0.788538 0.008478 0.387865 0.061 Uiso 1 1 calc R U . . .
C39 C 0.9488(7) 0.0755(6) 0.3778(4) 0.0546(18) Uani 1 1 d . . . . .
F3 F 0.9870(5) 0.0349(4) 0.3148(3) 0.0731(13) Uani 1 1 d . . . . .
C40 C 1.0235(8) 0.1361(6) 0.4065(5) 0.064(2) Uani 1 1 d . . . . .
H40 H 1.100386 0.149465 0.383222 0.077 Uiso 1 1 calc R U . . .
C41 C 0.9861(7) 0.1781(6) 0.4703(5) 0.0560(17) Uani 1 1 d . . . . .
H41 H 1.036811 0.221074 0.490913 0.067 Uiso 1 1 calc R U . . .
C42 C 0.6773(6) 0.3762(6) 0.8076(4) 0.0523(16) Uani 1 1 d . . . . .
H42 H 0.660921 0.429653 0.763809 0.063 Uiso 1 1 calc R U . . .
N4 N 0.6646(6) 0.3942(5) 0.8761(3) 0.0553(15) Uani 1 1 d . . . . .
C43 C 0.6123(7) 0.4877(6) 0.8879(4) 0.0523(17) Uani 1 1 d . . . . .
C44 C 0.6605(6) 0.5443(6) 0.9363(4) 0.0521(16) Uani 1 1 d . . . . .
I4 I 0.82178(5) 0.49789(6) 0.98361(4) 0.0799(2) Uani 1 1 d . . . . .
C45 C 0.6061(7) 0.6326(6) 0.9542(4) 0.0579(18) Uani 1 1 d . . . . .
H45 H 0.640915 0.671732 0.986884 0.069 Uiso 1 1 calc R U . . .
C46 C 0.4994(7) 0.6613(6) 0.9224(5) 0.061(2) Uani 1 1 d . . . . .
F4 F 0.4475(5) 0.7475(4) 0.9405(3) 0.0795(14) Uani 1 1 d . . . . .
C47 C 0.4474(7) 0.6081(6) 0.8762(4) 0.0579(19) Uani 1 1 d . . . . .
H47 H 0.372748 0.629495 0.856955 0.069 Uiso 1 1 calc R U . . .
C48 C 0.5029(7) 0.5217(6) 0.8566(4) 0.0572(18) Uani 1 1 d . . . . .
H48 H 0.467861 0.485265 0.822198 0.069 Uiso 1 1 calc R U . . .
N5 N 0.6729(8) -0.1630(5) 0.4021(5) 0.0725(19) Uani 1 1 d . . . . .
C49 C 0.6054(8) -0.2100(7) 0.3793(6) 0.066(2) Uani 1 1 d . . . . .
C50 C 0.5204(9) -0.2718(8) 0.3508(7) 0.084(3) Uani 1 1 d . . . . .
H50A H 0.554662 -0.340006 0.348195 0.126 Uiso 1 1 calc R U . . .
H50B H 0.498815 -0.236237 0.298522 0.126 Uiso 1 1 calc R U . . .
H50C H 0.450300 -0.281003 0.386552 0.126 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 1.602(5) . ?
V1 O1 1.911(4) . ?
V1 N1 2.101(5) . ?
V1 O2 1.900(5) . ?
V1 N3 2.084(5) . ?
O1 C1 1.318(7) . ?
C1 C2 1.417(9) . ?
C1 C6 1.406(9) . ?
C2 C3 1.393(9) . ?
C2 C18 1.464(9) . ?
C3 H3 0.9500 . ?
C3 C4 1.391(9) . ?
C4 C5 1.394(9) . ?
C4 C7 1.531(9) . ?
C5 H5 0.9500 . ?
C5 C6 1.414(8) . ?
C6 C11 1.436(8) . ?
C7 C8 1.552(11) . ?
C7 C9 1.529(10) . ?
C7 C10 1.509(11) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 H11 0.9500 . ?
C11 N1 1.296(8) . ?
N1 C12 1.430(8) . ?
C12 C13 1.395(9) . ?
C12 C17 1.387(9) . ?
C13 I1 2.108(6) . ?
C13 C14 1.384(9) . ?
C14 H14 0.9500 . ?
C14 C15 1.365(10) . ?
C15 F1 1.360(8) . ?
C15 C16 1.360(10) . ?
C16 H16 0.9500 . ?
C16 C17 1.392(10) . ?
C17 H17 0.9500 . ?
C18 H18 0.9500 . ?
C18 N2 1.265(8) . ?
N2 C19 1.419(9) . ?
C19 C20 1.400(10) . ?
C19 C24 1.387(11) . ?
C20 I2 2.092(8) . ?
C20 C21 1.380(12) . ?
C21 H21 0.9500 . ?
C21 C22 1.371(14) . ?
C22 F2 1.376(10) . ?
C22 C23 1.358(13) . ?
C23 H23 0.9500 . ?
C23 C24 1.385(11) . ?
C24 H24 0.9500 . ?
O2 C25 1.330(7) . ?
C25 C26 1.413(10) . ?
C25 C30 1.393(10) . ?
C26 C27 1.389(9) . ?
C26 C42 1.465(11) . ?
C27 H27 0.9500 . ?
C27 C28 1.399(11) . ?
C28 C29 1.368(10) . ?
C28 C31 1.531(9) . ?
C29 H29 0.9500 . ?
C29 C30 1.413(9) . ?
C30 C35 1.434(9) . ?
C31 C32 1.501(13) . ?
C31 C33 1.526(11) . ?
C31 C34 1.511(14) . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
C35 H35 0.9500 . ?
C35 N3 1.296(8) . ?
N3 C36 1.451(8) . ?
C36 C37 1.373(10) . ?
C36 C41 1.392(10) . ?
C37 I3 2.083(7) . ?
C37 C38 1.403(10) . ?
C38 H38 0.9500 . ?
C38 C39 1.361(11) . ?
C39 F3 1.366(8) . ?
C39 C40 1.359(12) . ?
C40 H40 0.9500 . ?
C40 C41 1.386(11) . ?
C41 H41 0.9500 . ?
C42 H42 0.9500 . ?
C42 N4 1.267(9) . ?
N4 C43 1.405(10) . ?
C43 C44 1.377(11) . ?
C43 C48 1.418(10) . ?
C44 I4 2.090(7) . ?
C44 C45 1.390(11) . ?
C45 H45 0.9500 . ?
C45 C46 1.380(11) . ?
C46 F4 1.355(9) . ?
C46 C47 1.340(12) . ?
C47 H47 0.9500 . ?
C47 C48 1.385(12) . ?
C48 H48 0.9500 . ?
N5 C49 1.134(12) . ?
C49 C50 1.446(14) . ?
C50 H50A 0.9800 . ?
C50 H50B 0.9800 . ?
C50 H50C 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 O1 114.8(2) . . ?
O3 V1 N1 96.5(2) . . ?
O3 V1 O2 118.0(2) . . ?
O3 V1 N3 94.9(2) . . ?
O1 V1 N1 86.60(18) . . ?
O1 V1 N3 88.77(19) . . ?
O2 V1 O1 127.2(2) . . ?
O2 V1 N1 86.93(19) . . ?
O2 V1 N3 87.6(2) . . ?
N3 V1 N1 168.6(2) . . ?
C1 O1 V1 124.6(4) . . ?
O1 C1 C2 119.9(5) . . ?
O1 C1 C6 122.2(5) . . ?
C6 C1 C2 117.8(5) . . ?
C1 C2 C18 118.4(5) . . ?
C3 C2 C1 119.9(6) . . ?
C3 C2 C18 121.6(6) . . ?
C2 C3 H3 118.5 . . ?
C4 C3 C2 122.9(6) . . ?
C4 C3 H3 118.5 . . ?
C3 C4 C5 117.0(6) . . ?
C3 C4 C7 121.4(6) . . ?
C5 C4 C7 121.5(6) . . ?
C4 C5 H5 119.1 . . ?
C4 C5 C6 121.7(6) . . ?
C6 C5 H5 119.1 . . ?
C1 C6 C5 120.3(6) . . ?
C1 C6 C11 123.4(5) . . ?
C5 C6 C11 116.3(6) . . ?
C4 C7 C8 108.1(6) . . ?
C9 C7 C4 109.4(6) . . ?
C9 C7 C8 108.7(6) . . ?
C10 C7 C4 113.1(6) . . ?
C10 C7 C8 107.2(7) . . ?
C10 C7 C9 110.3(6) . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C7 C9 H9A 109.5 . . ?
C7 C9 H9B 109.5 . . ?
C7 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C7 C10 H10A 109.5 . . ?
C7 C10 H10B 109.5 . . ?
C7 C10 H10C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C6 C11 H11 117.7 . . ?
N1 C11 C6 124.6(6) . . ?
N1 C11 H11 117.7 . . ?
C11 N1 V1 121.6(4) . . ?
C11 N1 C12 115.8(5) . . ?
C12 N1 V1 121.3(4) . . ?
C13 C12 N1 122.4(5) . . ?
C17 C12 N1 119.0(6) . . ?
C17 C12 C13 118.6(6) . . ?
C12 C13 I1 120.8(5) . . ?
C14 C13 C12 121.0(6) . . ?
C14 C13 I1 118.1(5) . . ?
C13 C14 H14 121.2 . . ?
C15 C14 C13 117.7(6) . . ?
C15 C14 H14 121.2 . . ?
F1 C15 C14 117.7(6) . . ?
F1 C15 C16 118.3(6) . . ?
C16 C15 C14 124.0(6) . . ?
C15 C16 H16 121.1 . . ?
C15 C16 C17 117.7(6) . . ?
C17 C16 H16 121.1 . . ?
C12 C17 C16 120.9(6) . . ?
C12 C17 H17 119.6 . . ?
C16 C17 H17 119.6 . . ?
C2 C18 H18 119.5 . . ?
N2 C18 C2 121.0(6) . . ?
N2 C18 H18 119.5 . . ?
C18 N2 C19 119.2(6) . . ?
C20 C19 N2 118.6(7) . . ?
C24 C19 N2 122.9(6) . . ?
C24 C19 C20 118.3(7) . . ?
C19 C20 I2 119.1(6) . . ?
C21 C20 C19 120.6(8) . . ?
C21 C20 I2 120.3(6) . . ?
C20 C21 H21 120.8 . . ?
C22 C21 C20 118.4(8) . . ?
C22 C21 H21 120.8 . . ?
C21 C22 F2 117.3(9) . . ?
C23 C22 C21 123.5(8) . . ?
C23 C22 F2 119.2(9) . . ?
C22 C23 H23 121.1 . . ?
C22 C23 C24 117.7(9) . . ?
C24 C23 H23 121.1 . . ?
C19 C24 H24 119.2 . . ?
C23 C24 C19 121.6(8) . . ?
C23 C24 H24 119.2 . . ?
C25 O2 V1 131.8(4) . . ?
O2 C25 C26 119.5(6) . . ?
O2 C25 C30 122.3(6) . . ?
C30 C25 C26 118.2(6) . . ?
C25 C26 C42 120.4(6) . . ?
C27 C26 C25 119.6(7) . . ?
C27 C26 C42 119.9(7) . . ?
C26 C27 H27 118.5 . . ?
C26 C27 C28 122.9(7) . . ?
C28 C27 H27 118.5 . . ?
C27 C28 C31 120.9(7) . . ?
C29 C28 C27 116.5(6) . . ?
C29 C28 C31 122.5(7) . . ?
C28 C29 H29 118.6 . . ?
C28 C29 C30 122.8(7) . . ?
C30 C29 H29 118.6 . . ?
C25 C30 C29 119.9(6) . . ?
C25 C30 C35 123.8(6) . . ?
C29 C30 C35 116.3(6) . . ?
C32 C31 C28 110.5(7) . . ?
C32 C31 C33 109.9(8) . . ?
C32 C31 C34 106.9(10) . . ?
C33 C31 C28 108.4(6) . . ?
C34 C31 C28 112.2(7) . . ?
C34 C31 C33 108.9(8) . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
H32A C32 H32B 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C31 C33 H33A 109.5 . . ?
C31 C33 H33B 109.5 . . ?
C31 C33 H33C 109.5 . . ?
H33A C33 H33B 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C31 C34 H34A 109.5 . . ?
C31 C34 H34B 109.5 . . ?
C31 C34 H34C 109.5 . . ?
H34A C34 H34B 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C30 C35 H35 117.3 . . ?
N3 C35 C30 125.3(6) . . ?
N3 C35 H35 117.3 . . ?
C35 N3 V1 125.3(5) . . ?
C35 N3 C36 115.2(5) . . ?
C36 N3 V1 119.1(4) . . ?
C37 C36 N3 121.8(6) . . ?
C37 C36 C41 120.0(7) . . ?
C41 C36 N3 118.2(6) . . ?
C36 C37 I3 121.5(5) . . ?
C36 C37 C38 120.8(7) . . ?
C38 C37 I3 117.7(5) . . ?
C37 C38 H38 121.4 . . ?
C39 C38 C37 117.2(7) . . ?
C39 C38 H38 121.4 . . ?
C38 C39 F3 118.0(7) . . ?
C40 C39 C38 123.5(7) . . ?
C40 C39 F3 118.4(7) . . ?
C39 C40 H40 120.4 . . ?
C39 C40 C41 119.2(8) . . ?
C41 C40 H40 120.4 . . ?
C36 C41 H41 120.4 . . ?
C40 C41 C36 119.2(8) . . ?
C40 C41 H41 120.4 . . ?
C26 C42 H42 119.7 . . ?
N4 C42 C26 120.7(6) . . ?
N4 C42 H42 119.7 . . ?
C42 N4 C43 120.0(6) . . ?
N4 C43 C48 121.2(7) . . ?
C44 C43 N4 120.7(6) . . ?
C44 C43 C48 117.8(7) . . ?
C43 C44 I4 119.4(5) . . ?
C43 C44 C45 122.1(7) . . ?
C45 C44 I4 118.5(6) . . ?
C44 C45 H45 121.3 . . ?
C46 C45 C44 117.3(8) . . ?
C46 C45 H45 121.3 . . ?
F4 C46 C45 116.6(8) . . ?
C47 C46 C45 123.1(7) . . ?
C47 C46 F4 120.4(7) . . ?
C46 C47 H47 120.2 . . ?
C46 C47 C48 119.7(7) . . ?
C48 C47 H47 120.2 . . ?
C43 C48 H48 120.0 . . ?
C47 C48 C43 119.9(8) . . ?
C47 C48 H48 120.0 . . ?
N5 C49 C50 178.8(9) . . ?
C49 C50 H50A 109.5 . . ?
C49 C50 H50B 109.5 . . ?
C49 C50 H50C 109.5 . . ?
H50A C50 H50B 109.5 . . ?
H50A C50 H50C 109.5 . . ?
H50B C50 H50C 109.5 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
C35 H35 F3 0.95 2.54 3.137(8) 121.3 2_756 yes
C38 H38 N5 0.95 2.59 3.449(12) 150.6 . yes
C41 H41 O3 0.95 2.54 3.184(9) 125.5 . yes
C47 H47 N2 0.95 2.42 3.287(9) 152.0 2_666 yes
C50 H50B F2 0.98 2.58 3.316(12) 131.7 . yes

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 C2 145.0(4) . . . . ?
V1 O1 C1 C6 -35.0(7) . . . . ?
V1 N1 C12 C13 -120.0(5) . . . . ?
V1 N1 C12 C17 59.7(7) . . . . ?
V1 O2 C25 C26 163.5(5) . . . . ?
V1 O2 C25 C30 -17.9(9) . . . . ?
V1 N3 C36 C37 -118.6(6) . . . . ?
V1 N3 C36 C41 60.3(7) . . . . ?
O3 V1 O2 C25 -72.0(6) . . . . ?
O1 V1 O2 C25 108.9(5) . . . . ?
O1 C1 C2 C3 -176.2(5) . . . . ?
O1 C1 C2 C18 4.8(8) . . . . ?
O1 C1 C6 C5 175.5(5) . . . . ?
O1 C1 C6 C11 -2.8(9) . . . . ?
C1 C2 C3 C4 0.1(9) . . . . ?
C1 C2 C18 N2 -178.2(6) . . . . ?
C1 C6 C11 N1 13.4(9) . . . . ?
C2 C1 C6 C5 -4.6(8) . . . . ?
C2 C1 C6 C11 177.1(5) . . . . ?
C2 C3 C4 C5 -3.4(9) . . . . ?
C2 C3 C4 C7 177.6(6) . . . . ?
C2 C18 N2 C19 -172.2(6) . . . . ?
C3 C2 C18 N2 2.8(9) . . . . ?
C3 C4 C5 C6 2.7(9) . . . . ?
C3 C4 C7 C8 -56.8(8) . . . . ?
C3 C4 C7 C9 61.4(8) . . . . ?
C3 C4 C7 C10 -175.3(6) . . . . ?
C4 C5 C6 C1 1.3(9) . . . . ?
C4 C5 C6 C11 179.7(5) . . . . ?
C5 C4 C7 C8 124.3(7) . . . . ?
C5 C4 C7 C9 -117.6(7) . . . . ?
C5 C4 C7 C10 5.8(9) . . . . ?
C5 C6 C11 N1 -165.0(6) . . . . ?
C6 C1 C2 C3 3.9(8) . . . . ?
C6 C1 C2 C18 -175.1(5) . . . . ?
C6 C11 N1 V1 11.5(8) . . . . ?
C6 C11 N1 C12 178.6(5) . . . . ?
C7 C4 C5 C6 -178.3(6) . . . . ?
C11 N1 C12 C13 72.9(8) . . . . ?
C11 N1 C12 C17 -107.4(7) . . . . ?
N1 V1 O2 C25 -167.8(6) . . . . ?
N1 C12 C13 I1 4.9(8) . . . . ?
N1 C12 C13 C14 -178.8(6) . . . . ?
N1 C12 C17 C16 178.7(6) . . . . ?
C12 C13 C14 C15 0.7(9) . . . . ?
C13 C12 C17 C16 -1.6(10) . . . . ?
C13 C14 C15 F1 178.3(6) . . . . ?
C13 C14 C15 C16 -2.8(10) . . . . ?
I1 C13 C14 C15 177.0(5) . . . . ?
C14 C15 C16 C17 2.6(11) . . . . ?
C15 C16 C17 C12 -0.3(11) . . . . ?
F1 C15 C16 C17 -178.5(6) . . . . ?
C17 C12 C13 I1 -174.8(5) . . . . ?
C17 C12 C13 C14 1.4(9) . . . . ?
C18 C2 C3 C4 179.1(6) . . . . ?
C18 N2 C19 C20 -142.6(6) . . . . ?
C18 N2 C19 C24 42.3(9) . . . . ?
N2 C19 C20 I2 4.8(8) . . . . ?
N2 C19 C20 C21 -175.8(6) . . . . ?
N2 C19 C24 C23 174.9(6) . . . . ?
C19 C20 C21 C22 0.5(11) . . . . ?
C20 C19 C24 C23 -0.2(10) . . . . ?
C20 C21 C22 F2 179.0(7) . . . . ?
C20 C21 C22 C23 0.3(13) . . . . ?
I2 C20 C21 C22 179.9(6) . . . . ?
C21 C22 C23 C24 -1.0(12) . . . . ?
C22 C23 C24 C19 1.0(11) . . . . ?
F2 C22 C23 C24 -179.7(7) . . . . ?
C24 C19 C20 I2 -179.9(5) . . . . ?
C24 C19 C20 C21 -0.5(10) . . . . ?
O2 C25 C26 C27 -177.8(6) . . . . ?
O2 C25 C26 C42 2.5(10) . . . . ?
O2 C25 C30 C29 179.8(6) . . . . ?
O2 C25 C30 C35 -1.4(10) . . . . ?
C25 C26 C27 C28 -3.3(11) . . . . ?
C25 C26 C42 N4 -166.9(7) . . . . ?
C25 C30 C35 N3 6.5(11) . . . . ?
C26 C25 C30 C29 -1.5(10) . . . . ?
C26 C25 C30 C35 177.2(6) . . . . ?
C26 C27 C28 C29 0.9(11) . . . . ?
C26 C27 C28 C31 179.3(7) . . . . ?
C26 C42 N4 C43 -171.8(7) . . . . ?
C27 C26 C42 N4 13.4(11) . . . . ?
C27 C28 C29 C30 1.2(10) . . . . ?
C27 C28 C31 C32 42.4(11) . . . . ?
C27 C28 C31 C33 -78.1(9) . . . . ?
C27 C28 C31 C34 161.6(9) . . . . ?
C28 C29 C30 C25 -0.9(10) . . . . ?
C28 C29 C30 C35 -179.7(6) . . . . ?
C29 C28 C31 C32 -139.3(9) . . . . ?
C29 C28 C31 C33 100.2(9) . . . . ?
C29 C28 C31 C34 -20.1(12) . . . . ?
C29 C30 C35 N3 -174.7(6) . . . . ?
C30 C25 C26 C27 3.5(10) . . . . ?
C30 C25 C26 C42 -176.2(6) . . . . ?
C30 C35 N3 V1 5.6(9) . . . . ?
C30 C35 N3 C36 178.7(6) . . . . ?
C31 C28 C29 C30 -177.2(6) . . . . ?
C35 N3 C36 C37 67.9(8) . . . . ?
C35 N3 C36 C41 -113.2(7) . . . . ?
N3 V1 O2 C25 22.2(6) . . . . ?
N3 C36 C37 I3 3.0(8) . . . . ?
N3 C36 C37 C38 -178.9(5) . . . . ?
N3 C36 C41 C40 179.7(6) . . . . ?
C36 C37 C38 C39 -2.2(9) . . . . ?
C37 C36 C41 C40 -1.3(10) . . . . ?
C37 C38 C39 F3 -179.0(6) . . . . ?
C37 C38 C39 C40 1.4(10) . . . . ?
I3 C37 C38 C39 176.0(5) . . . . ?
C38 C39 C40 C41 -0.6(11) . . . . ?
C39 C40 C41 C36 0.5(11) . . . . ?
F3 C39 C40 C41 179.9(6) . . . . ?
C41 C36 C37 I3 -175.9(5) . . . . ?
C41 C36 C37 C38 2.2(9) . . . . ?
C42 C26 C27 C28 176.4(7) . . . . ?
C42 N4 C43 C44 -135.0(8) . . . . ?
C42 N4 C43 C48 51.0(10) . . . . ?
N4 C43 C44 I4 6.1(9) . . . . ?
N4 C43 C44 C45 -174.8(7) . . . . ?
N4 C43 C48 C47 173.0(6) . . . . ?
C43 C44 C45 C46 1.2(11) . . . . ?
C44 C43 C48 C47 -1.1(10) . . . . ?
C44 C45 C46 F4 179.9(6) . . . . ?
C44 C45 C46 C47 0.1(11) . . . . ?
I4 C44 C45 C46 -179.7(5) . . . . ?
C45 C46 C47 C48 -1.9(11) . . . . ?
C46 C47 C48 C43 2.4(11) . . . . ?
F4 C46 C47 C48 178.3(6) . . . . ?
C48 C43 C44 I4 -179.7(5) . . . . ?
C48 C43 C44 C45 -0.7(11) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
####################################################################### 
# 
# 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_pMeL5H
_database_code_depnum_ccdc_archive 'CCDC 2418240'
loop_
_audit_author_name
_audit_author_address
'Timothy Prior'
;University of Hull
United Kingdom
;
_audit_update_record             
;
2025-01-20 deposited with the CCDC.	2025-12-16 downloaded from the CCDC.
;

_audit_creation_date             2023-07-04
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C21 H8 F10 N2 O'
_chemical_formula_sum            'C21 H8 F10 N2 O'
_chemical_formula_weight         494.29
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C20 H10 F10 N2 O4 V Al'
_chemical_oxdiff_usercomment     NONC6F5V
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'
F F 0.0727 0.0534 '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'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   21.1845(7)
_cell_length_b                   5.03630(10)
_cell_length_c                   19.2407(7)
_cell_angle_alpha                90
_cell_angle_beta                 116.970(4)
_cell_angle_gamma                90
_cell_volume                     1829.56(11)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    15395
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      72.6810
_cell_measurement_theta_min      4.6100
_shelx_estimated_absorpt_T_max   0.984
_shelx_estimated_absorpt_T_min   0.734
_exptl_absorpt_coefficient_mu    1.645
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.65849
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.90a (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.795
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             984
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0506
_diffrn_reflns_av_unetI/netI     0.0222
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            31527
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         73.664
_diffrn_reflns_theta_min         4.596
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            'HyPix-Arc 100'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     44.00 123.00   0.50    4.50    --   51.51  37.00 116.00  158
  2  ω    -40.00  17.00   0.50    4.50    --  -55.01  37.00 116.00  114
  3  ω   -126.00 -48.00   0.50    4.50    --  -55.01 -37.00 -39.00  156
  4  ω   -151.00 -72.00   0.50   16.00    --  -79.37 -37.00 -39.00  158
  5  ω    -40.00  -8.00   0.50   16.00    --  -79.37  37.00 116.00   64
  6  ω     76.00 155.00   0.50   16.00    --   83.47  37.00 116.00  158
  7  ω     12.00  44.00   0.50   16.00    --   83.47 -37.00 -39.00   64
  8  ω     -8.00  20.00   0.50    4.50    --   20.00  97.00 112.54   56
  9  ω    -18.00  28.00   0.50    4.50    --   51.51 -19.00 150.00   92
 10  ω    -19.00  44.00   0.50    4.50    --   51.51 -37.00 -39.00  126
 11  ω    -24.00  15.00   0.50    4.50    --  -55.01  19.00  60.00   78
 12  ω     12.00  44.00   0.50   16.00    --   83.47 -37.00-150.00   64
 13  ω     12.00  44.00   0.50   16.00    --   83.47 -37.00-180.00   64
 14  ω     16.00  68.00   0.50   16.00    --   83.47 -57.00 150.00  104
 15  ω     12.00  44.00   0.50   16.00    --   83.47 -37.00-120.00   64
 16  ω     30.00  98.00   0.50   16.00    --   92.00 -74.00 -55.54  136
 17  ω     21.00  52.00   0.50   16.00    --   92.00 -44.00   6.87   62
 18  ω     31.00 114.00   0.50   16.00    --   92.00 -85.00-138.04  166
 19  ω     31.00 105.00   0.50   16.00    --   92.00 -93.00 152.45  148
 20  ω     55.00 148.00   0.50   16.00    --   92.00   1.00  -3.96  186
 21  ω     76.00 108.00   0.50   16.00    --   92.00-121.00 146.68   64
 22  ω     40.00  66.00   0.50   16.00    --   92.00-121.00 146.68   52
 23  ω     36.00  82.00   0.50   16.00    --   92.00 -75.00  49.14   92
 24  ω     32.00  57.00   0.50   16.00    --   92.00 -76.00 -11.32   50
 25  ω     68.00  94.00   0.50   16.00    --   92.00 -76.00 -11.32   52
 26  ω     31.00  56.00   0.50   16.00    --   92.00 -74.00   5.48   50
 27  ω     35.00  74.00   0.50    4.50    --   51.51  77.00-180.00   78
 28  ω     13.00  38.00   0.50    4.50    --   36.00  87.00 163.69   50
 29  ω    -11.00  19.00   0.50    4.50    --   51.51 -19.00 -30.00   60
 30  ω    -86.00 -45.00   0.50    4.50    --  -60.00 -74.00-131.73   82
 31  ω    -89.00 -63.00   0.50   16.00    --  -79.37 -77.00 -90.00   52
 32  ω     90.00 116.00   0.50   16.00    --   83.47  57.00-150.00   52
 33  ω     33.00  59.00   0.50   16.00    --   83.47 -57.00  60.00   52
 34  ω     67.00  92.00   0.50   16.00    --   83.47  77.00-120.00   50
 35  ω     13.00  39.00   0.50   16.00    --   83.47 -37.00   0.00   52
 36  ω     67.00  97.00   0.50   16.00    --   83.47  77.00-180.00   60
 37  ω     75.00 101.00   0.50   16.00    --   83.47  77.00 150.00   52
 38  ω    -66.00 -35.00   0.50   16.00    --  -88.00 110.00  84.83   62
 39  ω   -103.00 -77.00   0.50   16.00    --  -88.00 110.00  84.83   52
 40  ω   -145.00 -79.00   0.50   16.00    --  -88.00 -76.00-106.53  132
 41  ω   -112.00 -82.00   0.50   16.00    --  -88.00 -69.00 -95.17   60
 42  ω   -104.00 -78.00   0.50   16.00    --  -88.00 -73.00-133.12   52
 43  ω   -121.00 -89.00   0.50   16.00    --  -88.00 -96.00-129.06   64
 44  ω    119.00 145.00   0.50   16.00    --   92.00  54.00  20.00   52
 45  ω     89.00 151.00   0.50   16.00    --   92.00  91.00 143.54  124
 46  ω     33.00  70.00   0.50   16.00    --   92.00   8.00  35.64   74
 47  ω     86.00 112.00   0.50   16.00    --   92.00  47.00 -15.06   52
 48  ω     98.00 132.00   0.50   16.00    --   92.00 113.00-162.75   68
 49  ω    105.00 131.00   0.50   16.00    --   92.00  13.00-122.87   52
 50  ω      5.00  33.00   0.50    4.50    --   32.00  94.00 -83.61   56
 51  ω     13.00  42.00   0.50    4.50    --   36.00  87.00 -50.99   58
 52  ω     12.00  42.00   0.50    4.50    --   36.00  90.00-178.13   60
 53  ω     16.00  42.00   0.50    4.50    --   40.00  89.00  21.04   52
 54  ω   -126.00 -48.00   0.50    4.50    --  -64.00 -75.00  57.61  156
 55  ω   -127.00 -63.00   0.50    4.50    --  -64.00 -72.00 145.38  128
 56  ω   -134.00 -57.00   0.50    4.50    --  -68.00 -63.00 -64.88  154
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'ROD, Synergy Custom system, HyPix-Arc 100'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0151621000
_diffrn_orient_matrix_UB_12      0.1136271000
_diffrn_orient_matrix_UB_13      -0.0803882000
_diffrn_orient_matrix_UB_21      0.0777333000
_diffrn_orient_matrix_UB_22      0.0904199000
_diffrn_orient_matrix_UB_23      0.0328807000
_diffrn_orient_matrix_UB_31      0.0197308000
_diffrn_orient_matrix_UB_32      -0.2692141000
_diffrn_orient_matrix_UB_33      -0.0228572000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54178
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3088
_reflns_number_total             3642
_reflns_odcompleteness_completeness 99.90
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     69.95
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.42.90a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.90a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.90a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_refine_diff_density_max         0.267
_refine_diff_density_min         -0.253
_refine_diff_density_rms         0.057
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     315
_refine_ls_number_reflns         3642
_refine_ls_number_restraints     4
_refine_ls_R_factor_all          0.0475
_refine_ls_R_factor_gt           0.0409
_refine_ls_restrained_S_all      1.057
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0784P)²+0.4103P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1159
_refine_ls_wR_factor_ref         0.1215
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 C8-H8 = C3-H3 = C5-H5 = C15-H15
 0.97305 with sigma of 0.02
3.a Aromatic/amide H refined with riding coordinates and stretchable bonds:
 C3(H3), C5(H5), C8(H8), C15(H15)
3.b Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C)
3.c Idealised tetrahedral OH refined as rotating group with stretchable bonds:
 O1(H1)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
F1 F 0.57831(5) 1.4411(2) 0.71320(6) 0.0434(3) Uani 1 1 d . . . . .
F2 F 0.44562(6) 1.5228(2) 0.68985(6) 0.0451(3) Uani 1 1 d . . . . .
F3 F 0.33835(5) 1.2066(2) 0.59230(7) 0.0456(3) Uani 1 1 d . . . . .
F4 F 0.36618(5) 0.7948(2) 0.51885(6) 0.0444(3) Uani 1 1 d . . . . .
F5 F 0.49882(5) 0.7062(2) 0.54121(6) 0.0397(3) Uani 1 1 d . . . . .
F6 F 0.73490(5) 0.3342(2) 0.41296(6) 0.0442(3) Uani 1 1 d . . . . .
F7 F 0.74544(5) -0.0695(2) 0.32777(6) 0.0459(3) Uani 1 1 d . . . . .
F8 F 0.86593(6) -0.3647(2) 0.38123(7) 0.0487(3) Uani 1 1 d . . . . .
F9 F 0.97618(6) -0.2522(2) 0.52240(7) 0.0458(3) Uani 1 1 d . . . . .
F10 F 0.96733(5) 0.1540(2) 0.60802(6) 0.0419(3) Uani 1 1 d . . . . .
O1 O 0.67333(6) 0.6726(3) 0.58006(7) 0.0388(3) Uani 1 1 d . . . . .
H1 H 0.6391(11) 0.742(4) 0.5838(11) 0.058 Uiso 1 1 calc R U . . .
N1 N 0.60974(7) 0.9965(3) 0.63228(8) 0.0352(3) Uani 1 1 d . . . . .
N2 N 0.85124(7) 0.4661(3) 0.56346(8) 0.0359(3) Uani 1 1 d . . . . .
C1 C 0.73304(8) 0.8085(4) 0.62474(10) 0.0343(4) Uani 1 1 d . . . . .
C2 C 0.73337(9) 1.0222(4) 0.67244(10) 0.0346(4) Uani 1 1 d . . . . .
C3 C 0.79734(9) 1.1529(4) 0.71839(10) 0.0361(4) Uani 1 1 d D . . . .
H3 H 0.79739(9) 1.303(3) 0.7515(6) 0.043 Uiso 1 1 calc DR U . . .
C4 C 0.86086(8) 1.0782(4) 0.71888(10) 0.0362(4) Uani 1 1 d . . . . .
C5 C 0.85867(9) 0.8707(4) 0.67058(10) 0.0352(4) Uani 1 1 d D . . . .
H5 H 0.9023(8) 0.8174(10) 0.66984(10) 0.042 Uiso 1 1 calc DR U . . .
C6 C 0.79641(9) 0.7347(4) 0.62285(10) 0.0341(4) Uani 1 1 d . . . . .
C7 C 0.92901(9) 1.2208(4) 0.76960(11) 0.0429(4) Uani 1 1 d . . . . .
H7A H 0.919301 1.367422 0.796840 0.064 Uiso 1 1 calc R U . . .
H7B H 0.949738 1.291083 0.737027 0.064 Uiso 1 1 calc R U . . .
H7C H 0.962289 1.096473 0.807881 0.064 Uiso 1 1 calc R U . . .
C8 C 0.66906(9) 1.1132(4) 0.67430(10) 0.0365(4) Uani 1 1 d D . . . .
H8 H 0.67082(9) 1.260(3) 0.7069(6) 0.044 Uiso 1 1 calc DR U . . .
C9 C 0.54403(9) 1.0677(4) 0.62792(9) 0.0341(4) Uani 1 1 d . . . . .
C10 C 0.52773(9) 1.2760(4) 0.66472(10) 0.0355(4) Uani 1 1 d . . . . .
C11 C 0.45898(9) 1.3213(4) 0.65276(10) 0.0373(4) Uani 1 1 d . . . . .
C12 C 0.40436(9) 1.1616(4) 0.60370(10) 0.0369(4) Uani 1 1 d . . . . .
C13 C 0.41852(9) 0.9538(4) 0.56647(10) 0.0364(4) Uani 1 1 d . . . . .
C14 C 0.48702(9) 0.9097(4) 0.57874(10) 0.0342(4) Uani 1 1 d . . . . .
C15 C 0.79605(9) 0.5156(4) 0.57275(10) 0.0357(4) Uani 1 1 d D . . . .
H15 H 0.7536(7) 0.4065(19) 0.5462(5) 0.043 Uiso 1 1 calc DR U . . .
C16 C 0.84973(9) 0.2525(3) 0.51551(10) 0.0346(4) Uani 1 1 d . . . . .
C17 C 0.79453(9) 0.1881(4) 0.44300(10) 0.0377(4) Uani 1 1 d . . . . .
C18 C 0.79974(9) -0.0157(4) 0.39807(10) 0.0380(4) Uani 1 1 d . . . . .
C19 C 0.86112(10) -0.1649(4) 0.42439(11) 0.0391(4) Uani 1 1 d . . . . .
C20 C 0.91684(9) -0.1066(4) 0.49563(11) 0.0386(4) Uani 1 1 d . . . . .
C21 C 0.91139(9) 0.1004(4) 0.53935(10) 0.0361(4) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
F1 C10 1.343(2) . ?
F2 C11 1.343(2) . ?
F3 C12 1.3328(19) . ?
F4 C13 1.338(2) . ?
F5 C14 1.341(2) . ?
F6 C17 1.3447(19) . ?
F7 C18 1.347(2) . ?
F8 C19 1.338(2) . ?
F9 C20 1.340(2) . ?
F10 C21 1.343(2) . ?
O1 H1 0.84(3) . ?
O1 C1 1.350(2) . ?
N1 C8 1.287(2) . ?
N1 C9 1.403(2) . ?
N2 C15 1.285(2) . ?
N2 C16 1.408(2) . ?
C1 C2 1.413(2) . ?
C1 C6 1.409(2) . ?
C2 C3 1.401(2) . ?
C2 C8 1.453(2) . ?
C3 H3 0.987(17) . ?
C3 C4 1.393(2) . ?
C4 C5 1.385(3) . ?
C4 C7 1.508(2) . ?
C5 H5 0.969(17) . ?
C5 C6 1.398(2) . ?
C6 C15 1.463(2) . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 H8 0.960(17) . ?
C9 C10 1.394(2) . ?
C9 C14 1.397(2) . ?
C10 C11 1.386(2) . ?
C11 C12 1.373(3) . ?
C12 C13 1.376(3) . ?
C13 C14 1.378(2) . ?
C15 H15 0.977(17) . ?
C16 C17 1.393(3) . ?
C16 C21 1.400(2) . ?
C17 C18 1.378(3) . ?
C18 C19 1.384(3) . ?
C19 C20 1.375(3) . ?
C20 C21 1.377(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 O1 H1 109.5 . . ?
C8 N1 C9 125.49(15) . . ?
C15 N2 C16 119.20(15) . . ?
O1 C1 C2 121.84(14) . . ?
O1 C1 C6 118.59(16) . . ?
C6 C1 C2 119.57(15) . . ?
C1 C2 C8 121.85(15) . . ?
C3 C2 C1 119.09(15) . . ?
C3 C2 C8 119.05(16) . . ?
C2 C3 H3 118.9 . . ?
C4 C3 C2 122.14(17) . . ?
C4 C3 H3 118.9 . . ?
C3 C4 C7 120.93(17) . . ?
C5 C4 C3 117.44(16) . . ?
C5 C4 C7 121.62(15) . . ?
C4 C5 H5 118.5 . . ?
C4 C5 C6 123.02(15) . . ?
C6 C5 H5 118.5 . . ?
C1 C6 C15 119.70(15) . . ?
C5 C6 C1 118.69(16) . . ?
C5 C6 C15 121.59(15) . . ?
C4 C7 H7A 109.5 . . ?
C4 C7 H7B 109.5 . . ?
C4 C7 H7C 109.5 . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
N1 C8 C2 119.99(16) . . ?
N1 C8 H8 120.0 . . ?
C2 C8 H8 120.0 . . ?
C10 C9 N1 129.05(16) . . ?
C10 C9 C14 115.82(15) . . ?
C14 C9 N1 115.13(15) . . ?
F1 C10 C9 121.02(15) . . ?
F1 C10 C11 117.44(16) . . ?
C11 C10 C9 121.54(16) . . ?
F2 C11 C10 119.66(16) . . ?
F2 C11 C12 119.53(15) . . ?
C12 C11 C10 120.80(16) . . ?
F3 C12 C11 120.51(16) . . ?
F3 C12 C13 120.25(16) . . ?
C11 C12 C13 119.24(15) . . ?
F4 C13 C12 120.22(15) . . ?
F4 C13 C14 120.14(16) . . ?
C12 C13 C14 119.64(16) . . ?
F5 C14 C9 119.02(14) . . ?
F5 C14 C13 118.03(15) . . ?
C13 C14 C9 122.95(16) . . ?
N2 C15 C6 120.33(16) . . ?
N2 C15 H15 119.8 . . ?
C6 C15 H15 119.8 . . ?
C17 C16 N2 126.42(15) . . ?
C17 C16 C21 115.81(16) . . ?
C21 C16 N2 117.57(15) . . ?
F6 C17 C16 120.10(16) . . ?
F6 C17 C18 117.69(16) . . ?
C18 C17 C16 122.15(16) . . ?
F7 C18 C17 120.31(16) . . ?
F7 C18 C19 119.40(16) . . ?
C17 C18 C19 120.28(16) . . ?
F8 C19 C18 120.32(17) . . ?
F8 C19 C20 120.45(17) . . ?
C20 C19 C18 119.23(17) . . ?
F9 C20 C19 119.86(16) . . ?
F9 C20 C21 120.22(17) . . ?
C19 C20 C21 119.92(16) . . ?
F10 C21 C16 119.22(16) . . ?
F10 C21 C20 118.19(15) . . ?
C20 C21 C16 122.58(16) . . ?

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
F1 C10 C11 F2 -0.7(3) . . . . ?
F1 C10 C11 C12 179.68(16) . . . . ?
F2 C11 C12 F3 0.5(3) . . . . ?
F2 C11 C12 C13 -179.35(16) . . . . ?
F3 C12 C13 F4 -0.3(3) . . . . ?
F3 C12 C13 C14 179.95(16) . . . . ?
F4 C13 C14 F5 0.6(3) . . . . ?
F4 C13 C14 C9 -179.75(16) . . . . ?
F6 C17 C18 F7 -2.2(2) . . . . ?
F6 C17 C18 C19 177.01(15) . . . . ?
F7 C18 C19 F8 -1.5(3) . . . . ?
F7 C18 C19 C20 178.96(16) . . . . ?
F8 C19 C20 F9 -0.6(3) . . . . ?
F8 C19 C20 C21 179.67(16) . . . . ?
F9 C20 C21 F10 1.3(3) . . . . ?
F9 C20 C21 C16 -177.59(15) . . . . ?
O1 C1 C2 C3 179.05(16) . . . . ?
O1 C1 C2 C8 -1.9(3) . . . . ?
O1 C1 C6 C5 -178.38(15) . . . . ?
O1 C1 C6 C15 0.3(2) . . . . ?
N1 C9 C10 F1 -1.1(3) . . . . ?
N1 C9 C10 C11 178.83(17) . . . . ?
N1 C9 C14 F5 0.8(2) . . . . ?
N1 C9 C14 C13 -178.88(16) . . . . ?
N2 C16 C17 F6 -1.0(3) . . . . ?
N2 C16 C17 C18 175.86(16) . . . . ?
N2 C16 C21 F10 3.6(2) . . . . ?
N2 C16 C21 C20 -177.49(16) . . . . ?
C1 C2 C3 C4 -0.3(3) . . . . ?
C1 C2 C8 N1 0.7(3) . . . . ?
C1 C6 C15 N2 171.91(17) . . . . ?
C2 C1 C6 C5 2.1(2) . . . . ?
C2 C1 C6 C15 -179.22(15) . . . . ?
C2 C3 C4 C5 1.3(3) . . . . ?
C2 C3 C4 C7 -179.36(17) . . . . ?
C3 C2 C8 N1 179.73(16) . . . . ?
C3 C4 C5 C6 -0.6(3) . . . . ?
C4 C5 C6 C1 -1.1(3) . . . . ?
C4 C5 C6 C15 -179.74(16) . . . . ?
C5 C6 C15 N2 -9.5(3) . . . . ?
C6 C1 C2 C3 -1.5(2) . . . . ?
C6 C1 C2 C8 177.58(16) . . . . ?
C7 C4 C5 C6 -179.94(17) . . . . ?
C8 N1 C9 C10 1.8(3) . . . . ?
C8 N1 C9 C14 -179.43(16) . . . . ?
C8 C2 C3 C4 -179.33(16) . . . . ?
C9 N1 C8 C2 -178.88(16) . . . . ?
C9 C10 C11 F2 179.44(15) . . . . ?
C9 C10 C11 C12 -0.2(3) . . . . ?
C10 C9 C14 F5 179.77(14) . . . . ?
C10 C9 C14 C13 0.1(3) . . . . ?
C10 C11 C12 F3 -179.84(16) . . . . ?
C10 C11 C12 C13 0.3(3) . . . . ?
C11 C12 C13 F4 179.55(16) . . . . ?
C11 C12 C13 C14 -0.2(3) . . . . ?
C12 C13 C14 F5 -179.68(15) . . . . ?
C12 C13 C14 C9 0.0(3) . . . . ?
C14 C9 C10 F1 -179.88(15) . . . . ?
C14 C9 C10 C11 0.0(3) . . . . ?
C15 N2 C16 C17 43.6(3) . . . . ?
C15 N2 C16 C21 -141.74(17) . . . . ?
C16 N2 C15 C6 179.42(15) . . . . ?
C16 C17 C18 F7 -179.13(16) . . . . ?
C16 C17 C18 C19 0.1(3) . . . . ?
C17 C16 C21 F10 178.83(15) . . . . ?
C17 C16 C21 C20 -2.3(3) . . . . ?
C17 C18 C19 F8 179.23(16) . . . . ?
C17 C18 C19 C20 -0.3(3) . . . . ?
C18 C19 C20 F9 178.93(15) . . . . ?
C18 C19 C20 C21 -0.8(3) . . . . ?
C19 C20 C21 F10 -178.91(16) . . . . ?
C19 C20 C21 C16 2.2(3) . . . . ?
C21 C16 C17 F6 -175.73(15) . . . . ?
C21 C16 C17 C18 1.1(3) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.830
_oxdiff_exptl_absorpt_empirical_full_min 0.496
####################################################################### 
# 
# 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 2418245'
loop_
_audit_author_name
_audit_author_address
'Timothy Prior'
;University of Hull
United Kingdom
;
_audit_update_record             
;
2025-01-20 deposited with the CCDC.	2025-12-16 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         'C66 H82 N4 O3 V'
_chemical_formula_sum            'C66 H82 N4 O3 V'
_chemical_formula_weight         1030.29

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'

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

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

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

_cell_length_a                   9.2637(5)
_cell_length_b                   32.1121(19)
_cell_length_c                   10.5093(6)
_cell_angle_alpha                90
_cell_angle_beta                 104.6408(10)
_cell_angle_gamma                90
_cell_volume                     3024.8(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    7618
_cell_measurement_theta_min      2.36
_cell_measurement_theta_max      26.05

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.131
_exptl_crystal_F_000             1106
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.600
_exptl_crystal_size_mid          0.580
_exptl_crystal_size_min          0.180
_exptl_absorpt_coefficient_mu    0.211
_shelx_estimated_absorpt_T_min   0.884
_shelx_estimated_absorpt_T_max   0.963
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.884
_exptl_absorpt_correction_T_max  0.963
_exptl_absorpt_process_details   'SADABS v2004/1, Sheldrick, G.M., (2004)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker SMART 1000 CCD diffractometer'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_method       'ω rotation with narrow frames'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            21757
_diffrn_reflns_av_unetI/netI     0.0309
_diffrn_reflns_av_R_equivalents  0.0360
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         2.101
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_full        24.999
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             5329
_reflns_number_gt                4315
_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       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS (Sheldrick, 2008)'
_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)+(0.0422P)²+7.7250P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_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_number_reflns         5329
_refine_ls_number_parameters     466
_refine_ls_number_restraints     891
_refine_ls_R_factor_all          0.1300
_refine_ls_R_factor_gt           0.1135
_refine_ls_wR_factor_ref         0.2562
_refine_ls_wR_factor_gt          0.2462
_refine_ls_goodness_of_fit_ref   1.209
_refine_ls_restrained_S_all      1.163
_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 0.05198(17) 0.50559(5) 0.52305(15) 0.0406(4) Uani 0.5 1 d . . P . .
O2 O 0.2077(7) 0.5235(2) 0.6004(6) 0.0495(16) Uani 0.5 1 d . . P . .
O1 O 0.0059(4) 0.53381(9) 0.3620(3) 0.0511(8) Uani 1 1 d . . . . .
C1 C 0.0665(5) 0.53075(15) 0.2601(4) 0.0453(11) Uani 1 1 d . . . . .
C2 C 0.1357(5) 0.49418(15) 0.2337(4) 0.0462(11) Uani 1 1 d . . . . .
C3 C 0.1963(6) 0.49187(18) 0.1233(5) 0.0600(14) Uani 1 1 d . . . . .
H3 H 0.238589 0.466399 0.104211 0.072 Uiso 1 1 calc R U . . .
C4 C 0.1954(6) 0.5257(2) 0.0432(5) 0.0618(14) Uani 1 1 d . . . . .
C5 C 0.1269(6) 0.56109(19) 0.0701(5) 0.0603(14) Uani 1 1 d . . . . .
H5 H 0.123567 0.584372 0.013671 0.072 Uiso 1 1 calc R U . . .
C6 C 0.0619(5) 0.56512(16) 0.1753(5) 0.0520(12) Uani 1 1 d . . . . .
C7 C 0.1489(6) 0.45771(15) 0.3147(5) 0.0508(12) Uani 1 1 d . . . . .
H7 H 0.194638 0.434253 0.286053 0.061 Uiso 1 1 calc R U . . .
N1 N 0.1067(5) 0.45278(11) 0.4213(4) 0.0492(10) Uani 1 1 d . . . . .
C8 C 0.2676(7) 0.5236(2) -0.0717(5) 0.084(2) Uani 1 1 d . . . . .
H8A H 0.373477 0.516624 -0.038968 0.126 Uiso 1 1 calc R U . . .
H8B H 0.257775 0.550650 -0.116139 0.126 Uiso 1 1 calc R U . . .
H8C H 0.217898 0.502160 -0.133878 0.126 Uiso 1 1 calc R U . . .
C9 C 0.1428(6) 0.41240(14) 0.4825(5) 0.0513(10) Uani 1 1 d . U . . .
C10 C 0.0440(7) 0.37999(16) 0.4438(6) 0.0674(13) Uani 1 1 d . U . . .
C11 C 0.0886(9) 0.34070(18) 0.5017(8) 0.0913(19) Uani 1 1 d . U . . .
H11 H 0.023585 0.317542 0.477645 0.110 Uiso 1 1 calc R U . . .
C12 C 0.2209(10) 0.3353(2) 0.5900(8) 0.102(2) Uani 1 1 d . U . . .
H12 H 0.248208 0.308637 0.627349 0.122 Uiso 1 1 calc R U . . .
C13 C 0.3142(8) 0.3678(2) 0.6250(7) 0.0901(18) Uani 1 1 d . U . . .
H13 H 0.407197 0.363502 0.687025 0.108 Uiso 1 1 calc R U . . .
C14 C 0.2794(7) 0.40758(18) 0.5736(6) 0.0660(12) Uani 1 1 d . U . . .
C15 C -0.1035(7) 0.3846(2) 0.3438(7) 0.0829(16) Uani 1 1 d D U . . .
H15 H -0.119656 0.414548 0.317844 0.099 Uiso 0.753(18) 1 calc R U P A 1
H15X H -0.072035 0.409987 0.302619 0.099 Uiso 0.247(18) 1 calc R U P A 2
C16 C -0.1206(11) 0.3583(2) 0.2222(7) 0.116(3) Uani 1 1 d D U . . .
H16A H -0.030768 0.360828 0.189647 0.174 Uiso 1 1 calc R U . . .
H16B H -0.207486 0.367829 0.154298 0.174 Uiso 1 1 calc R U . . .
H16C H -0.134680 0.329118 0.243609 0.174 Uiso 1 1 calc R U . . .
C17 C -0.2298(11) 0.3699(6) 0.4072(11) 0.119(5) Uani 0.753(18) 1 d D U P A 1
H17A H -0.224984 0.385920 0.487516 0.143 Uiso 0.753(18) 1 calc R U P A 1
H17B H -0.326989 0.374276 0.344978 0.143 Uiso 0.753(18) 1 calc R U P A 1
H17C H -0.216790 0.340227 0.428954 0.143 Uiso 0.753(18) 1 calc R U P A 1
C17X C -0.233(2) 0.4058(11) 0.378(3) 0.082(8) Uani 0.247(18) 1 d D U P A 2
H17D H -0.197341 0.421231 0.460061 0.098 Uiso 0.247(18) 1 calc R U P A 2
H17E H -0.278874 0.425189 0.306961 0.098 Uiso 0.247(18) 1 calc R U P A 2
H17F H -0.305965 0.384949 0.387738 0.098 Uiso 0.247(18) 1 calc R U P A 2
C18 C 0.3882(8) 0.4429(2) 0.6117(7) 0.0914(18) Uani 1 1 d D U . . .
H18 H 0.335263 0.469380 0.578563 0.110 Uiso 1 1 calc R U . . .
C19 C 0.4466(10) 0.4463(3) 0.7605(8) 0.134(3) Uani 1 1 d D U . . .
H19A H 0.362615 0.450015 0.800369 0.201 Uiso 1 1 calc R U . . .
H19B H 0.513893 0.470264 0.781970 0.201 Uiso 1 1 calc R U . . .
H19C H 0.500899 0.420827 0.794779 0.201 Uiso 1 1 calc R U . . .
C20 C 0.5194(10) 0.4380(4) 0.5495(10) 0.154(4) Uani 1 1 d D U . . .
H20A H 0.572967 0.412139 0.580936 0.231 Uiso 1 1 calc R U . . .
H20B H 0.587172 0.461708 0.574049 0.231 Uiso 1 1 calc R U . . .
H20C H 0.482185 0.436892 0.453594 0.231 Uiso 1 1 calc R U . . .
C21 C -0.0089(7) 0.60418(17) 0.1925(6) 0.0684(16) Uani 1 1 d . . . . .
H21 H -0.051516 0.607712 0.265114 0.082 Uiso 1 1 calc R U . . .
N2 N -0.0143(7) 0.63365(17) 0.1114(6) 0.0909(16) Uani 1 1 d D U . . .
C22 C -0.0998(14) 0.6706(3) 0.1121(15) 0.093(3) Uani 0.658(8) 1 d D U P B 1
C23 C -0.2458(17) 0.6757(4) 0.0310(17) 0.114(3) Uani 0.658(8) 1 d D U P B 1
C24 C -0.3177(17) 0.7130(4) 0.0388(17) 0.130(4) Uani 0.658(8) 1 d D U P B 1
H24 H -0.418864 0.716467 -0.008385 0.156 Uiso 0.658(8) 1 calc R U P B 1
C25 C -0.2411(19) 0.7459(4) 0.1169(18) 0.128(4) Uani 0.658(8) 1 d D U P B 1
H25 H -0.289240 0.771876 0.119647 0.153 Uiso 0.658(8) 1 calc R U P B 1
C26 C -0.1010(19) 0.7402(4) 0.1863(17) 0.114(3) Uani 0.658(8) 1 d D U P B 1
H26 H -0.049840 0.762512 0.237969 0.137 Uiso 0.658(8) 1 calc R U P B 1
C27 C -0.0280(17) 0.7027(3) 0.1854(13) 0.097(3) Uani 0.658(8) 1 d D U P B 1
C28 C -0.310(2) 0.6393(5) -0.066(2) 0.138(4) Uani 0.658(8) 1 d D U P B 1
H28 H -0.229580 0.617853 -0.055461 0.166 Uiso 0.658(8) 1 calc R U P B 1
C29 C -0.435(2) 0.6196(7) -0.0249(18) 0.198(7) Uani 0.658(8) 1 d D U P B 1
H29A H -0.402950 0.612155 0.068413 0.297 Uiso 0.658(8) 1 calc R U P B 1
H29B H -0.518853 0.639141 -0.038761 0.297 Uiso 0.658(8) 1 calc R U P B 1
H29C H -0.466453 0.594429 -0.077348 0.297 Uiso 0.658(8) 1 calc R U P B 1
C30 C -0.354(2) 0.6508(5) -0.2045(17) 0.148(5) Uani 0.658(8) 1 d D U P B 1
H30A H -0.268939 0.663801 -0.229061 0.221 Uiso 0.658(8) 1 calc R U P B 1
H30B H -0.384619 0.625853 -0.258057 0.221 Uiso 0.658(8) 1 calc R U P B 1
H30C H -0.437019 0.670565 -0.219471 0.221 Uiso 0.658(8) 1 calc R U P B 1
C31 C 0.1310(18) 0.6988(4) 0.2676(13) 0.107(3) Uani 0.658(8) 1 d D U P B 1
H31 H 0.139141 0.671190 0.312884 0.128 Uiso 0.658(8) 1 calc R U P B 1
C32 C 0.189(2) 0.7312(4) 0.3731(13) 0.136(5) Uani 0.658(8) 1 d D U P B 1
H32A H 0.292990 0.724780 0.418178 0.204 Uiso 0.658(8) 1 calc R U P B 1
H32B H 0.184141 0.758802 0.332578 0.204 Uiso 0.658(8) 1 calc R U P B 1
H32C H 0.128137 0.730896 0.436875 0.204 Uiso 0.658(8) 1 calc R U P B 1
C33 C 0.2395(19) 0.6977(9) 0.1765(19) 0.143(6) Uani 0.658(8) 1 d D U P B 1
H33A H 0.342380 0.695176 0.230101 0.215 Uiso 0.658(8) 1 calc R U P B 1
H33B H 0.215540 0.673757 0.116972 0.215 Uiso 0.658(8) 1 calc R U P B 1
H33C H 0.229124 0.723423 0.124812 0.215 Uiso 0.658(8) 1 calc R U P B 1
C22X C -0.052(2) 0.6746(6) 0.156(3) 0.100(4) Uani 0.342(8) 1 d D U P B 2
C23X C -0.204(3) 0.6879(6) 0.100(3) 0.114(4) Uani 0.342(8) 1 d D U P B 2
C24X C -0.240(3) 0.7286(7) 0.127(4) 0.124(4) Uani 0.342(8) 1 d D U P B 2
H24X H -0.334037 0.740001 0.083144 0.149 Uiso 0.342(8) 1 calc R U P B 2
C25X C -0.136(3) 0.7528(7) 0.218(3) 0.123(5) Uani 0.342(8) 1 d D U P B 2
H25X H -0.169107 0.777961 0.249141 0.148 Uiso 0.342(8) 1 calc R U P B 2
C26X C 0.007(3) 0.7416(6) 0.264(3) 0.117(4) Uani 0.342(8) 1 d D U P B 2
H26X H 0.078591 0.759830 0.316291 0.140 Uiso 0.342(8) 1 calc R U P B 2
C27X C 0.047(3) 0.7016(6) 0.230(3) 0.103(4) Uani 0.342(8) 1 d D U P B 2
C28X C -0.308(2) 0.6567(9) 0.009(3) 0.123(5) Uani 0.342(8) 1 d D U P B 2
H28X H -0.286176 0.629182 0.054995 0.148 Uiso 0.342(8) 1 calc R U P B 2
C29X C -0.471(2) 0.6632(10) -0.010(3) 0.152(7) Uani 0.342(8) 1 d D U P B 2
H29D H -0.492733 0.666813 0.076166 0.227 Uiso 0.342(8) 1 calc R U P B 2
H29E H -0.501768 0.688177 -0.063208 0.227 Uiso 0.342(8) 1 calc R U P B 2
H29F H -0.525059 0.638982 -0.054310 0.227 Uiso 0.342(8) 1 calc R U P B 2
C30X C -0.269(4) 0.6511(12) -0.117(3) 0.144(8) Uani 0.342(8) 1 d D U P B 2
H30D H -0.160928 0.646862 -0.101386 0.215 Uiso 0.342(8) 1 calc R U P B 2
H30E H -0.321486 0.626752 -0.162890 0.215 Uiso 0.342(8) 1 calc R U P B 2
H30F H -0.298195 0.675947 -0.171788 0.215 Uiso 0.342(8) 1 calc R U P B 2
C31X C 0.212(3) 0.6904(7) 0.284(2) 0.111(5) Uani 0.342(8) 1 d D U P B 2
H31X H 0.212615 0.660484 0.310390 0.133 Uiso 0.342(8) 1 calc R U P B 2
C32X C 0.304(3) 0.7130(9) 0.404(3) 0.144(8) Uani 0.342(8) 1 d D U P B 2
H32D H 0.406246 0.702218 0.425561 0.217 Uiso 0.342(8) 1 calc R U P B 2
H32E H 0.305250 0.742890 0.385045 0.217 Uiso 0.342(8) 1 calc R U P B 2
H32F H 0.260257 0.708565 0.478535 0.217 Uiso 0.342(8) 1 calc R U P B 2
C33X C 0.292(4) 0.6920(17) 0.172(3) 0.139(8) Uani 0.342(8) 1 d D U P B 2
H33D H 0.232043 0.677350 0.095229 0.208 Uiso 0.342(8) 1 calc R U P B 2
H33E H 0.305467 0.721044 0.149556 0.208 Uiso 0.342(8) 1 calc R U P B 2
H33F H 0.389739 0.678487 0.201696 0.208 Uiso 0.342(8) 1 calc R U P B 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
V1 V1 1.027(3) 3_566 ?
V1 O2 1.575(7) . ?
V1 O1 1.872(3) . ?
V1 O1 1.917(3) 3_566 ?
V1 N1 2.133(4) . ?
V1 N1 2.173(4) 3_566 ?
O1 C1 1.332(5) . ?
C1 C2 1.399(6) . ?
C1 C6 1.412(6) . ?
C2 C3 1.413(6) . ?
C2 C7 1.435(7) . ?
C3 C4 1.372(8) . ?
C3 H3 0.9500 . ?
C4 C5 1.367(8) . ?
C4 C8 1.522(7) . ?
C5 C6 1.393(7) . ?
C5 H5 0.9500 . ?
C6 C21 1.448(7) . ?
C7 N1 1.286(6) . ?
C7 H7 0.9500 . ?
N1 C9 1.448(6) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 C10 1.378(7) . ?
C9 C14 1.389(7) . ?
C10 C11 1.416(8) . ?
C10 C15 1.506(9) . ?
C11 C12 1.349(10) . ?
C11 H11 0.9500 . ?
C12 C13 1.346(10) . ?
C12 H12 0.9500 . ?
C13 C14 1.391(8) . ?
C13 H13 0.9500 . ?
C14 C18 1.503(9) . ?
C15 C17X 1.494(17) . ?
C15 C16 1.506(9) . ?
C15 C17 1.559(11) . ?
C15 H15 1.0000 . ?
C15 H15X 1.0000 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C17X H17D 0.9800 . ?
C17X H17E 0.9800 . ?
C17X H17F 0.9800 . ?
C18 C19 1.523(9) . ?
C18 C20 1.527(10) . ?
C18 H18 1.0000 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 N2 1.266(7) . ?
C21 H21 0.9500 . ?
N2 C22 1.428(11) . ?
N2 C22X 1.468(15) . ?
C22 C27 1.355(15) . ?
C22 C23 1.414(16) . ?
C23 C24 1.383(16) . ?
C23 C28 1.56(2) . ?
C24 C25 1.41(2) . ?
C24 H24 0.9500 . ?
C25 C26 1.33(2) . ?
C25 H25 0.9500 . ?
C26 C27 1.383(15) . ?
C26 H26 0.9500 . ?
C27 C31 1.513(16) . ?
C28 C30 1.46(2) . ?
C28 C29 1.474(19) . ?
C28 H28 1.0000 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C31 C32 1.516(13) . ?
C31 C33 1.555(14) . ?
C31 H31 1.0000 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C22X C27X 1.356(19) . ?
C22X C23X 1.44(2) . ?
C23X C24X 1.39(2) . ?
C23X C28X 1.54(2) . ?
C24X C25X 1.41(3) . ?
C24X H24X 0.9500 . ?
C25X C26X 1.34(3) . ?
C25X H25X 0.9500 . ?
C26X C27X 1.404(19) . ?
C26X H26X 0.9500 . ?
C27X C31X 1.53(2) . ?
C28X C30X 1.48(3) . ?
C28X C29X 1.49(2) . ?
C28X H28X 1.0000 . ?
C29X H29D 0.9800 . ?
C29X H29E 0.9800 . ?
C29X H29F 0.9800 . ?
C30X H30D 0.9800 . ?
C30X H30E 0.9800 . ?
C30X H30F 0.9800 . ?
C31X C32X 1.516(16) . ?
C31X C33X 1.542(18) . ?
C31X H31X 1.0000 . ?
C32X H32D 0.9800 . ?
C32X H32E 0.9800 . ?
C32X H32F 0.9800 . ?
C33X H33D 0.9800 . ?
C33X H33E 0.9800 . ?
C33X H33F 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 176.8(3) 3_566 . ?
V1 V1 O1 76.7(2) 3_566 . ?
O2 V1 O1 105.0(3) . . ?
V1 V1 O1 71.9(2) 3_566 3_566 ?
O2 V1 O1 106.4(3) . 3_566 ?
O1 V1 O1 148.57(10) . 3_566 ?
V1 V1 N1 78.4(2) 3_566 . ?
O2 V1 N1 104.3(3) . . ?
O1 V1 N1 87.73(15) . . ?
O1 V1 N1 86.04(15) 3_566 . ?
V1 V1 N1 74.0(2) 3_566 3_566 ?
O2 V1 N1 103.3(3) . 3_566 ?
O1 V1 N1 86.00(15) . 3_566 ?
O1 V1 N1 85.44(15) 3_566 3_566 ?
N1 V1 N1 152.42(9) . 3_566 ?
C1 O1 V1 130.2(3) . . ?
C1 O1 V1 134.4(3) . 3_566 ?
O1 C1 C2 121.9(4) . . ?
O1 C1 C6 119.8(4) . . ?
C2 C1 C6 118.3(4) . . ?
C1 C2 C3 120.3(5) . . ?
C1 C2 C7 122.8(4) . . ?
C3 C2 C7 116.9(4) . . ?
C4 C3 C2 121.4(5) . . ?
C4 C3 H3 119.3 . . ?
C2 C3 H3 119.3 . . ?
C5 C4 C3 117.5(5) . . ?
C5 C4 C8 121.4(5) . . ?
C3 C4 C8 121.1(6) . . ?
C4 C5 C6 123.9(5) . . ?
C4 C5 H5 118.0 . . ?
C6 C5 H5 118.0 . . ?
C5 C6 C1 118.6(5) . . ?
C5 C6 C21 118.7(5) . . ?
C1 C6 C21 122.7(4) . . ?
N1 C7 C2 128.2(4) . . ?
N1 C7 H7 115.9 . . ?
C2 C7 H7 115.9 . . ?
C7 N1 C9 114.2(4) . . ?
C7 N1 V1 120.1(3) . . ?
C9 N1 V1 123.2(3) . . ?
C7 N1 V1 122.2(3) . 3_566 ?
C9 N1 V1 121.9(3) . 3_566 ?
C4 C8 H8A 109.5 . . ?
C4 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C4 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C10 C9 C14 122.7(5) . . ?
C10 C9 N1 118.9(5) . . ?
C14 C9 N1 118.3(5) . . ?
C9 C10 C11 116.5(6) . . ?
C9 C10 C15 123.3(5) . . ?
C11 C10 C15 120.1(6) . . ?
C12 C11 C10 121.7(7) . . ?
C12 C11 H11 119.2 . . ?
C10 C11 H11 119.2 . . ?
C13 C12 C11 119.9(7) . . ?
C13 C12 H12 120.1 . . ?
C11 C12 H12 120.1 . . ?
C12 C13 C14 122.4(7) . . ?
C12 C13 H13 118.8 . . ?
C14 C13 H13 118.8 . . ?
C9 C14 C13 116.8(6) . . ?
C9 C14 C18 122.2(5) . . ?
C13 C14 C18 120.9(6) . . ?
C17X C15 C16 122.6(12) . . ?
C17X C15 C10 121.2(11) . . ?
C16 C15 C10 114.8(6) . . ?
C16 C15 C17 105.3(8) . . ?
C10 C15 C17 108.6(7) . . ?
C16 C15 H15 109.4 . . ?
C10 C15 H15 109.4 . . ?
C17 C15 H15 109.4 . . ?
C17X C15 H15X 94.0 . . ?
C16 C15 H15X 94.0 . . ?
C10 C15 H15X 94.0 . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C15 C17 H17A 109.5 . . ?
C15 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C15 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C15 C17X H17D 109.5 . . ?
C15 C17X H17E 109.5 . . ?
H17D C17X H17E 109.5 . . ?
C15 C17X H17F 109.5 . . ?
H17D C17X H17F 109.5 . . ?
H17E C17X H17F 109.5 . . ?
C14 C18 C19 111.6(7) . . ?
C14 C18 C20 111.1(6) . . ?
C19 C18 C20 109.4(7) . . ?
C14 C18 H18 108.2 . . ?
C19 C18 H18 108.2 . . ?
C20 C18 H18 108.2 . . ?
C18 C19 H19A 109.5 . . ?
C18 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C18 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C18 C20 H20A 109.5 . . ?
C18 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C18 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
N2 C21 C6 120.4(6) . . ?
N2 C21 H21 119.8 . . ?
C6 C21 H21 119.8 . . ?
C21 N2 C22 123.1(8) . . ?
C21 N2 C22X 115.1(14) . . ?
C27 C22 C23 120.8(11) . . ?
C27 C22 N2 116.2(10) . . ?
C23 C22 N2 122.7(11) . . ?
C24 C23 C22 117.7(14) . . ?
C24 C23 C28 125.1(14) . . ?
C22 C23 C28 117.1(11) . . ?
C23 C24 C25 120.2(14) . . ?
C23 C24 H24 119.9 . . ?
C25 C24 H24 119.9 . . ?
C26 C25 C24 119.5(13) . . ?
C26 C25 H25 120.3 . . ?
C24 C25 H25 120.3 . . ?
C25 C26 C27 121.8(15) . . ?
C25 C26 H26 119.1 . . ?
C27 C26 H26 119.1 . . ?
C22 C27 C26 119.7(14) . . ?
C22 C27 C31 122.0(10) . . ?
C26 C27 C31 118.4(13) . . ?
C30 C28 C29 111.1(15) . . ?
C30 C28 C23 115.0(13) . . ?
C29 C28 C23 109.2(18) . . ?
C30 C28 H28 107.0 . . ?
C29 C28 H28 107.0 . . ?
C23 C28 H28 107.0 . . ?
C28 C29 H29A 109.5 . . ?
C28 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C28 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 . . ?
C27 C31 C32 118.4(13) . . ?
C27 C31 C33 109.7(11) . . ?
C32 C31 C33 107.5(13) . . ?
C27 C31 H31 106.9 . . ?
C32 C31 H31 106.9 . . ?
C33 C31 H31 106.9 . . ?
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 . . ?
C31 C33 H33A 109.5 . . ?
C31 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
C31 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C27X C22X C23X 119.3(16) . . ?
C27X C22X N2 125.0(16) . . ?
C23X C22X N2 115.1(15) . . ?
C24X C23X C22X 117(2) . . ?
C24X C23X C28X 126(2) . . ?
C22X C23X C28X 116.6(16) . . ?
C23X C24X C25X 120(2) . . ?
C23X C24X H24X 120.1 . . ?
C25X C24X H24X 120.1 . . ?
C26X C25X C24X 123(2) . . ?
C26X C25X H25X 118.7 . . ?
C24X C25X H25X 118.7 . . ?
C25X C26X C27X 117(2) . . ?
C25X C26X H26X 121.5 . . ?
C27X C26X H26X 121.5 . . ?
C22X C27X C26X 123(2) . . ?
C22X C27X C31X 122.0(16) . . ?
C26X C27X C31X 114.8(18) . . ?
C30X C28X C29X 112(2) . . ?
C30X C28X C23X 112(2) . . ?
C29X C28X C23X 116(2) . . ?
C30X C28X H28X 105.1 . . ?
C29X C28X H28X 105.1 . . ?
C23X C28X H28X 105.1 . . ?
C28X C29X H29D 109.5 . . ?
C28X C29X H29E 109.5 . . ?
H29D C29X H29E 109.5 . . ?
C28X C29X H29F 109.5 . . ?
H29D C29X H29F 109.5 . . ?
H29E C29X H29F 109.5 . . ?
C28X C30X H30D 109.5 . . ?
C28X C30X H30E 109.5 . . ?
H30D C30X H30E 109.5 . . ?
C28X C30X H30F 109.5 . . ?
H30D C30X H30F 109.5 . . ?
H30E C30X H30F 109.5 . . ?
C32X C31X C27X 120(2) . . ?
C32X C31X C33X 109.7(19) . . ?
C27X C31X C33X 109.7(18) . . ?
C32X C31X H31X 105.5 . . ?
C27X C31X H31X 105.5 . . ?
C33X C31X H31X 105.5 . . ?
C31X C32X H32D 109.5 . . ?
C31X C32X H32E 109.5 . . ?
H32D C32X H32E 109.5 . . ?
C31X C32X H32F 109.5 . . ?
H32D C32X H32F 109.5 . . ?
H32E C32X H32F 109.5 . . ?
C31X C33X H33D 109.5 . . ?
C31X C33X H33E 109.5 . . ?
H33D C33X H33E 109.5 . . ?
C31X C33X H33F 109.5 . . ?
H33D C33X H33F 109.5 . . ?
H33E C33X H33F 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 -112.0(4) 3_566 . . . ?
O2 V1 O1 C1 70.8(5) . . . . ?
O1 V1 O1 C1 -112.0(4) 3_566 . . . ?
N1 V1 O1 C1 -33.4(4) . . . . ?
N1 V1 O1 C1 173.5(4) 3_566 . . . ?
O2 V1 O1 V1 -177.2(3) . . . 3_566 ?
O1 V1 O1 V1 -0.002(1) 3_566 . . 3_566 ?
N1 V1 O1 V1 78.62(19) . . . 3_566 ?
N1 V1 O1 V1 -74.50(19) 3_566 . . 3_566 ?
V1 O1 C1 C2 26.8(7) . . . . ?
V1 O1 C1 C2 -15.8(7) 3_566 . . . ?
V1 O1 C1 C6 -153.2(4) . . . . ?
V1 O1 C1 C6 164.2(4) 3_566 . . . ?
O1 C1 C2 C3 178.9(4) . . . . ?
C6 C1 C2 C3 -1.2(7) . . . . ?
O1 C1 C2 C7 -1.1(7) . . . . ?
C6 C1 C2 C7 178.9(5) . . . . ?
C1 C2 C3 C4 3.1(8) . . . . ?
C7 C2 C3 C4 -177.0(5) . . . . ?
C2 C3 C4 C5 -3.2(8) . . . . ?
C2 C3 C4 C8 177.0(5) . . . . ?
C3 C4 C5 C6 1.6(8) . . . . ?
C8 C4 C5 C6 -178.6(5) . . . . ?
C4 C5 C6 C1 0.1(8) . . . . ?
C4 C5 C6 C21 -179.3(5) . . . . ?
O1 C1 C6 C5 179.6(4) . . . . ?
C2 C1 C6 C5 -0.3(7) . . . . ?
O1 C1 C6 C21 -1.0(8) . . . . ?
C2 C1 C6 C21 179.1(5) . . . . ?
C1 C2 C7 N1 -2.3(8) . . . . ?
C3 C2 C7 N1 177.8(5) . . . . ?
C2 C7 N1 C9 -177.4(5) . . . . ?
C2 C7 N1 V1 -14.9(7) . . . . ?
C2 C7 N1 V1 17.3(7) . . . 3_566 ?
C7 N1 C9 C10 -87.4(6) . . . . ?
V1 N1 C9 C10 110.7(5) . . . . ?
V1 N1 C9 C10 77.9(5) 3_566 . . . ?
C7 N1 C9 C14 89.7(6) . . . . ?
V1 N1 C9 C14 -72.1(5) . . . . ?
V1 N1 C9 C14 -104.9(5) 3_566 . . . ?
C14 C9 C10 C11 -0.3(8) . . . . ?
N1 C9 C10 C11 176.7(5) . . . . ?
C14 C9 C10 C15 -179.2(5) . . . . ?
N1 C9 C10 C15 -2.1(8) . . . . ?
C9 C10 C11 C12 0.0(10) . . . . ?
C15 C10 C11 C12 178.9(7) . . . . ?
C10 C11 C12 C13 0.0(12) . . . . ?
C11 C12 C13 C14 0.3(12) . . . . ?
C10 C9 C14 C13 0.5(8) . . . . ?
N1 C9 C14 C13 -176.5(5) . . . . ?
C10 C9 C14 C18 178.1(5) . . . . ?
N1 C9 C14 C18 1.0(7) . . . . ?
C12 C13 C14 C9 -0.5(10) . . . . ?
C12 C13 C14 C18 -178.1(7) . . . . ?
C9 C10 C15 C17X -74.8(19) . . . . ?
C11 C10 C15 C17X 106.3(19) . . . . ?
C9 C10 C15 C16 118.6(7) . . . . ?
C11 C10 C15 C16 -60.3(9) . . . . ?
C9 C10 C15 C17 -124.0(9) . . . . ?
C11 C10 C15 C17 57.2(10) . . . . ?
C9 C14 C18 C19 132.2(7) . . . . ?
C13 C14 C18 C19 -50.3(9) . . . . ?
C9 C14 C18 C20 -105.3(8) . . . . ?
C13 C14 C18 C20 72.1(9) . . . . ?
C5 C6 C21 N2 1.7(9) . . . . ?
C1 C6 C21 N2 -177.7(6) . . . . ?
C6 C21 N2 C22 171.0(8) . . . . ?
C6 C21 N2 C22X -164.8(11) . . . . ?
C21 N2 C22 C27 91.1(14) . . . . ?
C21 N2 C22 C23 -95.4(15) . . . . ?
C27 C22 C23 C24 -6(2) . . . . ?
N2 C22 C23 C24 -179.4(13) . . . . ?
C27 C22 C23 C28 170.9(15) . . . . ?
N2 C22 C23 C28 -2(2) . . . . ?
C22 C23 C24 C25 6(2) . . . . ?
C28 C23 C24 C25 -171.3(16) . . . . ?
C23 C24 C25 C26 -2(3) . . . . ?
C24 C25 C26 C27 -1(3) . . . . ?
C23 C22 C27 C26 3(2) . . . . ?
N2 C22 C27 C26 177.1(13) . . . . ?
C23 C22 C27 C31 -176.8(14) . . . . ?
N2 C22 C27 C31 -3.2(19) . . . . ?
C25 C26 C27 C22 0(3) . . . . ?
C25 C26 C27 C31 -179.8(15) . . . . ?
C24 C23 C28 C30 55(3) . . . . ?
C22 C23 C28 C30 -121.4(17) . . . . ?
C24 C23 C28 C29 -70(2) . . . . ?
C22 C23 C28 C29 112.9(18) . . . . ?
C22 C27 C31 C32 -164.0(14) . . . . ?
C26 C27 C31 C32 15.8(18) . . . . ?
C22 C27 C31 C33 72.1(18) . . . . ?
C26 C27 C31 C33 -108.1(17) . . . . ?
C21 N2 C22X C27X 86(3) . . . . ?
C21 N2 C22X C23X -103(2) . . . . ?
C27X C22X C23X C24X 0(4) . . . . ?
N2 C22X C23X C24X -172(3) . . . . ?
C27X C22X C23X C28X 176(3) . . . . ?
N2 C22X C23X C28X 4(4) . . . . ?
C22X C23X C24X C25X -8(5) . . . . ?
C28X C23X C24X C25X 176(3) . . . . ?
C23X C24X C25X C26X 13(5) . . . . ?
C24X C25X C26X C27X -8(5) . . . . ?
C23X C22X C27X C26X 5(5) . . . . ?
N2 C22X C27X C26X 176(2) . . . . ?
C23X C22X C27X C31X -176(3) . . . . ?
N2 C22X C27X C31X -5(5) . . . . ?
C25X C26X C27X C22X -1(4) . . . . ?
C25X C26X C27X C31X 180(3) . . . . ?
C24X C23X C28X C30X 105(4) . . . . ?
C22X C23X C28X C30X -71(3) . . . . ?
C24X C23X C28X C29X -25(4) . . . . ?
C22X C23X C28X C29X 159(3) . . . . ?
C22X C27X C31X C32X -157(3) . . . . ?
C26X C27X C31X C32X 23(4) . . . . ?
C22X C27X C31X C33X 75(4) . . . . ?
C26X C27X C31X C33X -106(3) . . . . ?

_refine_diff_density_max         0.476
_refine_diff_density_min         -0.329
_refine_diff_density_rms         0.056


_chemical_properties_physical    Air-sensitive,Moisture-sensitive
####################################################################### 
# 
# 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 2418241'
loop_
_audit_author_name
_audit_author_address
'Timothy Prior'
;University of Hull
United Kingdom
;
_audit_update_record             
;
2025-01-20 deposited with the CCDC.	2025-12-16 downloaded from the CCDC.
;
_audit_creation_date             2023-05-18
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C50 H50 N4 O3 V'
_chemical_formula_sum            'C50 H50 N4 O3 V'
_chemical_formula_weight         805.88
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C40 H40 N4 O4 V Al'
_chemical_oxdiff_usercomment     'NONMe V'
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'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   8.39860(10)
_cell_length_b                   22.0578(3)
_cell_length_c                   11.60800(10)
_cell_angle_alpha                90
_cell_angle_beta                 96.2020(10)
_cell_angle_gamma                90
_cell_volume                     2137.85(4)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    16465
_cell_measurement_temperature    99.99(10)
_cell_measurement_theta_max      74.9460
_cell_measurement_theta_min      4.0030
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    2.304
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.77972
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.90a (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'dark green'
_exptl_crystal_density_diffrn    1.252
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       blade
_exptl_crystal_F_000             850
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.03
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0258
_diffrn_reflns_av_unetI/netI     0.0153
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.968
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            25035
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.968
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         75.121
_diffrn_reflns_theta_min         4.008
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.99(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.968
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -119.00 -52.00   0.50    1.50    --  -48.43-160.00-152.00  134
  2  ω     39.00 117.00   0.50    1.50    --   48.43-160.00-152.00  156
  3  ω     19.00  87.00   0.50    1.50    --   48.43-117.00  -1.00  136
  4  ω     58.00 119.00   0.50    1.50    --   48.43 160.00-122.00  122
  5  ω     32.00 109.00   0.50    6.00    --  100.00-117.00  -1.00  154
  6  ω     39.00 135.00   0.50    6.00    --  100.00-160.00-152.00  192
  7  ω     58.00 158.00   0.50    6.00    --  100.00 160.00-122.00  200
  8  ω   -170.00 -81.00   0.50    6.00    -- -102.00-117.00  -1.00  178
  9  ω    -95.00 -52.00   0.50    6.00    -- -102.00 160.00-122.00   86
 10  ω   -106.00 -70.00   0.50    6.00    -- -102.00 117.00  86.00   72
 11  ω    -22.00  19.00   0.50    1.50    --  -48.43  19.00  30.00   82
 12  ω    -24.00   2.00   0.50    1.50    --  -48.43  19.00   0.00   52
 13  ω    -17.00  20.00   0.50    1.50    --  -48.43  19.00-120.00   74
 14  ω    -23.00  27.00   0.50    1.50    --   48.43 -19.00 150.00  100
 15  ω     94.00 172.00   0.50    6.00    --  100.00  30.00  90.00  156
 16  ω     58.00 112.00   0.50    6.00    --  100.00-125.00  60.00  108
 17  ω    133.00 171.00   0.50    6.00    --  100.00  45.00  60.00   76
 18  ω     28.00 102.00   0.50    6.00    --  100.00 -94.00-180.00  148
 19  ω     98.00 124.00   0.50    6.00    --  100.00  45.00  60.00   52
 20  ω     28.00  86.00   0.50    6.00    --  100.00 -94.00   0.00  116
 21  ω     39.00  66.00   0.50    6.00    --  100.00 -61.00   0.00   54
 22  ω    -68.00 -31.00   0.50    6.00    -- -102.00  61.00  90.00   74
 23  ω   -174.00-140.00   0.50    6.00    -- -102.00 -15.00-120.00   68
 24  ω    -69.00 -32.00   0.50    6.00    -- -102.00  61.00 -60.00   74
 25  ω    -68.00 -33.00   0.50    6.00    -- -102.00  61.00 -90.00   70
 26  ω     54.00  79.00   0.50    1.50    --   48.43-160.00-152.00   50
 27  ω   -119.00 -28.00   0.50    1.50    --  -48.43 -77.00 -90.00  182
 28  ω   -119.00 -28.00   0.50    1.50    --  -48.43 -77.00 150.00  182
 29  ω     36.00 119.00   0.50    1.50    --   48.43  57.00  30.00  166
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'ROD, Synergy Custom system, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0543604000
_diffrn_orient_matrix_UB_12      -0.0508211000
_diffrn_orient_matrix_UB_13      0.0779356000
_diffrn_orient_matrix_UB_21      0.0920146000
_diffrn_orient_matrix_UB_22      -0.0468256000
_diffrn_orient_matrix_UB_23      -0.0659565000
_diffrn_orient_matrix_UB_31      0.1504013000
_diffrn_orient_matrix_UB_32      0.0100957000
_diffrn_orient_matrix_UB_33      0.0859940000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54178
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3931
_reflns_number_total             4275
_reflns_odcompleteness_completeness 99.48
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     69.95
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.42.90a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.90a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.90a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_refine_diff_density_max         0.228
_refine_diff_density_min         -0.255
_refine_diff_density_rms         0.032
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     351
_refine_ls_number_reflns         4275
_refine_ls_number_restraints     19
_refine_ls_R_factor_all          0.0386
_refine_ls_R_factor_gt           0.0359
_refine_ls_restrained_S_all      1.041
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0584P)²+0.4104P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1028
_refine_ls_wR_factor_ref         0.1046
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C18-C23 \\sim C18A-C23A
 with sigma of 0.02
 C18-C19 \\sim C18A-C19A
 with sigma of 0.02
 C21-C20 \\sim C21A-C20A
 with sigma of 0.02
 C21-C22 \\sim C21A-C22A
 with sigma of 0.02
 C23-C22 \\sim C23A-C22A
 with sigma of 0.02
 C23-C25 \\sim C23A-C25A
 with sigma of 0.02
 C20-C22 \\sim C20A-C22A
 with sigma of 0.04
 C19-C20 \\sim C19A-C20A
 with sigma of 0.02
 C19-C24 \\sim C19A-C24A
 with sigma of 0.02
 C23-C19 \\sim C23A-C19A
 with sigma of 0.04
 C20-C24 \\sim C20A-C24A
 with sigma of 0.04
 C18-C20 \\sim C18A-C20A
 with sigma of 0.04
 C18-C22 \\sim C18A-C22A
 with sigma of 0.04
 C18-C24 \\sim C18A-C24A
 with sigma of 0.04
 C18-C25 \\sim C18A-C25A
 with sigma of 0.04
 C22-C25 \\sim C22A-C25A
 with sigma of 0.04
 C21-C23 \\sim C21A-C23A
 with sigma of 0.04
 C21-C19 \\sim C21A-C19A
 with sigma of 0.04
 N2-C18A \\sim N2-C18
 with sigma of 0.02
3. Others
 Sof(C18A)=Sof(C19A)=Sof(C20A)=Sof(H20A)=Sof(C21A)=Sof(H21A)=Sof(C22A)=
 Sof(H22A)=Sof(C23A)=Sof(C24A)=Sof(H24D)=Sof(H24E)=Sof(H24F)=Sof(C25A)=
 Sof(H25D)=Sof(H25E)=Sof(H25F)=1-FVAR(1)
 Sof(C18)=Sof(C19)=Sof(C20)=Sof(H20)=Sof(C21)=Sof(H21)=Sof(C22)=Sof(H22)=
 Sof(C23)=Sof(C24)=Sof(H24A)=Sof(H24B)=Sof(H24C)=Sof(C25)=Sof(H25A)=Sof(H25B)=
 Sof(H25C)=FVAR(1)
 Fixed Sof: V1(0.5) O2(0.5)
4.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C8(H8), C11(H11), C12(H12), C13(H13), C17(H17), C20(H20),
 C20A(H20A), C21(H21), C21A(H21A), C22(H22), C22A(H22A)
4.b Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C24(H24A,H24B,
 H24C), C24A(H24D,H24E,H24F), C25(H25A,H25B,H25C), C25A(H25D,H25E,H25F)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
V1 V 0.53887(5) 0.51552(2) -0.00158(3) 0.03508(13) Uani 0.5 1 d . . P A -1
O1 O 0.63238(13) 0.44825(4) 0.08638(7) 0.0501(3) Uani 1 1 d . . . A -1
O2 O 0.6781(3) 0.56395(9) 0.00101(17) 0.0520(5) Uani 0.5 1 d . . P A -1
N1 N 0.91965(14) 0.30600(5) 0.19386(10) 0.0449(3) Uani 1 1 d . . . . .
N2 N 0.43356(13) 0.53855(5) 0.14992(8) 0.0365(2) Uani 1 1 d D . . . .
C1 C 0.68669(16) 0.44544(6) 0.19730(10) 0.0387(3) Uani 1 1 d . . . . .
C2 C 0.79790(16) 0.39995(6) 0.23767(11) 0.0399(3) Uani 1 1 d . . . . .
C3 C 0.86143(15) 0.39941(6) 0.35346(11) 0.0406(3) Uani 1 1 d . . . . .
H3 H 0.938623 0.369361 0.378342 0.049 Uiso 1 1 calc R U . . .
C4 C 0.81690(16) 0.44094(6) 0.43453(11) 0.0417(3) Uani 1 1 d . . . . .
C5 C 0.70263(16) 0.48350(6) 0.39646(11) 0.0399(3) Uani 1 1 d . . . . .
H5 H 0.668092 0.511685 0.450433 0.048 Uiso 1 1 calc R U . . .
C6 C 0.63573(15) 0.48636(6) 0.28000(10) 0.0370(3) Uani 1 1 d . . . . .
C7 C 0.88533(19) 0.43751(7) 0.55977(12) 0.0526(4) Uani 1 1 d . . . . .
H7A H 0.834183 0.404223 0.597894 0.079 Uiso 1 1 calc R U . . .
H7B H 0.865354 0.475803 0.598532 0.079 Uiso 1 1 calc R U . . .
H7C H 1.000965 0.430261 0.564376 0.079 Uiso 1 1 calc R U . . .
C8 C 0.84100(17) 0.35258(6) 0.15726(11) 0.0438(3) Uani 1 1 d . . . . .
H8 H 0.809439 0.356948 0.076606 0.053 Uiso 1 1 calc R U . . .
C9 C 0.94905(17) 0.25999(6) 0.11304(12) 0.0449(3) Uani 1 1 d . . . . .
C10 C 1.10354(18) 0.25477(7) 0.07963(13) 0.0507(3) Uani 1 1 d . . . . .
C11 C 1.1334(2) 0.20771(8) 0.00491(16) 0.0635(4) Uani 1 1 d . . . . .
H11 H 1.237245 0.203428 -0.019355 0.076 Uiso 1 1 calc R U . . .
C12 C 1.0144(2) 0.16712(8) -0.03455(18) 0.0695(5) Uani 1 1 d . . . . .
H12 H 1.036658 0.135663 -0.086357 0.083 Uiso 1 1 calc R U . . .
C13 C 0.8634(2) 0.17212(8) 0.00103(16) 0.0633(4) Uani 1 1 d . . . . .
H13 H 0.782943 0.143571 -0.025389 0.076 Uiso 1 1 calc R U . . .
C14 C 0.82776(18) 0.21868(7) 0.07539(14) 0.0519(3) Uani 1 1 d . . . . .
C15 C 1.22973(18) 0.30000(8) 0.12143(16) 0.0584(4) Uani 1 1 d . . . . .
H15A H 1.206489 0.338838 0.082189 0.088 Uiso 1 1 calc R U . . .
H15B H 1.334654 0.285261 0.104172 0.088 Uiso 1 1 calc R U . . .
H15C H 1.230635 0.305487 0.205273 0.088 Uiso 1 1 calc R U . . .
C16 C 0.66304(19) 0.22450(8) 0.11333(16) 0.0603(4) Uani 1 1 d . . . . .
H16A H 0.671685 0.233528 0.196436 0.090 Uiso 1 1 calc R U . . .
H16B H 0.604611 0.186368 0.098198 0.090 Uiso 1 1 calc R U . . .
H16C H 0.605338 0.257392 0.070118 0.090 Uiso 1 1 calc R U . . .
C17 C 0.50933(16) 0.52908(6) 0.25064(10) 0.0378(3) Uani 1 1 d . . . . .
H17 H 0.478016 0.553043 0.312354 0.045 Uiso 1 1 calc R U . . .
C18 C 0.3203(9) 0.5877(3) 0.1476(10) 0.0356(13) Uani 0.549(4) 1 d D . P A 1
C18A C 0.2861(10) 0.5746(4) 0.1469(13) 0.040(2) Uani 0.451(4) 1 d D . P A 2
C19 C 0.1603(6) 0.5741(2) 0.1486(3) 0.0420(8) Uani 0.549(4) 1 d D . P A 1
C19A C 0.1393(6) 0.5450(3) 0.1407(3) 0.0412(10) Uani 0.451(4) 1 d D . P A 2
C20 C 0.0567(6) 0.6229(2) 0.1517(4) 0.0541(13) Uani 0.549(4) 1 d D . P A 1
H20 H -0.054712 0.615605 0.152457 0.065 Uiso 0.549(4) 1 calc R U P A 1
C20A C 0.0009(5) 0.5788(2) 0.1429(3) 0.0551(11) Uani 0.451(4) 1 d D . P A 2
H20A H -0.100218 0.559193 0.139083 0.066 Uiso 0.451(4) 1 calc R U P A 2
C21 C 0.1128(10) 0.6821(3) 0.1538(7) 0.0506(15) Uani 0.549(4) 1 d D . P A 1
H21 H 0.039822 0.714830 0.155963 0.061 Uiso 0.549(4) 1 calc R U P A 1
C21A C 0.0102(7) 0.6415(3) 0.1506(5) 0.0589(17) Uani 0.451(4) 1 d D . P A 2
H21A H -0.085089 0.664655 0.151560 0.071 Uiso 0.451(4) 1 calc R U P A 2
C22 C 0.2749(5) 0.69364(13) 0.1528(2) 0.0486(8) Uani 0.549(4) 1 d D . P A 1
H22 H 0.312240 0.734321 0.155010 0.058 Uiso 0.549(4) 1 calc R U P A 1
C22A C 0.1566(11) 0.6709(4) 0.1569(9) 0.058(2) Uani 0.451(4) 1 d D . P A 2
H22A H 0.160755 0.713734 0.164460 0.069 Uiso 0.451(4) 1 calc R U P A 2
C23 C 0.3824(6) 0.64661(17) 0.1487(2) 0.0398(8) Uani 0.549(4) 1 d D . P A 1
C23A C 0.2976(7) 0.6385(2) 0.1524(3) 0.0447(10) Uani 0.451(4) 1 d D . P A 2
C24 C 0.0987(4) 0.5105(3) 0.1508(3) 0.0554(9) Uani 0.549(4) 1 d D . P A 1
H24A H 0.118705 0.489679 0.079247 0.083 Uiso 0.549(4) 1 calc R U P A 1
H24B H -0.016735 0.511228 0.157200 0.083 Uiso 0.549(4) 1 calc R U P A 1
H24C H 0.153613 0.489005 0.217528 0.083 Uiso 0.549(4) 1 calc R U P A 1
C24A C 0.1346(5) 0.4766(2) 0.1323(4) 0.0525(10) Uani 0.451(4) 1 d D . P A 2
H24D H 0.181015 0.459058 0.205911 0.079 Uiso 0.451(4) 1 calc R U P A 2
H24E H 0.196390 0.463341 0.069933 0.079 Uiso 0.451(4) 1 calc R U P A 2
H24F H 0.023304 0.463145 0.115622 0.079 Uiso 0.451(4) 1 calc R U P A 2
C25 C 0.5580(5) 0.65844(14) 0.1413(3) 0.0500(8) Uani 0.549(4) 1 d D . P A 1
H25A H 0.620570 0.643150 0.211472 0.075 Uiso 0.549(4) 1 calc R U P A 1
H25B H 0.575780 0.702138 0.134453 0.075 Uiso 0.549(4) 1 calc R U P A 1
H25C H 0.591612 0.637713 0.073318 0.075 Uiso 0.549(4) 1 calc R U P A 1
C25A C 0.4563(8) 0.66921(19) 0.1534(4) 0.0561(12) Uani 0.451(4) 1 d D . P A 2
H25D H 0.506402 0.657302 0.084411 0.084 Uiso 0.451(4) 1 calc R U P A 2
H25E H 0.525516 0.657243 0.223082 0.084 Uiso 0.451(4) 1 calc R U P A 2
H25F H 0.440982 0.713255 0.153378 0.084 Uiso 0.451(4) 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
V1 O1 1.9204(10) . ?
V1 O2 1.582(2) . ?
V1 N2 2.1139(10) . ?
O1 C1 1.3202(15) . ?
N1 C8 1.2696(17) . ?
N1 C9 1.4218(18) . ?
N2 C17 1.2864(16) . ?
N2 C18 1.441(7) . ?
N2 C18A 1.470(9) . ?
C1 C2 1.4157(18) . ?
C1 C6 1.4171(17) . ?
C2 C3 1.3916(18) . ?
C2 C8 1.4720(18) . ?
C3 H3 0.9500 . ?
C3 C4 1.3932(19) . ?
C4 C5 1.3805(19) . ?
C4 C7 1.5063(17) . ?
C5 H5 0.9500 . ?
C5 C6 1.4083(17) . ?
C6 C17 1.4328(18) . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 H8 0.9500 . ?
C9 C10 1.399(2) . ?
C9 C14 1.401(2) . ?
C10 C11 1.393(2) . ?
C10 C15 1.498(2) . ?
C11 H11 0.9500 . ?
C11 C12 1.382(3) . ?
C12 H12 0.9500 . ?
C12 C13 1.380(3) . ?
C13 H13 0.9500 . ?
C13 C14 1.395(2) . ?
C14 C16 1.502(2) . ?
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 H17 0.9500 . ?
C18 C19 1.378(7) . ?
C18 C23 1.399(7) . ?
C18A C19A 1.390(8) . ?
C18A C23A 1.412(8) . ?
C19 C20 1.387(6) . ?
C19 C24 1.496(5) . ?
C19A C20A 1.384(6) . ?
C19A C24A 1.513(6) . ?
C20 H20 0.9500 . ?
C20 C21 1.388(11) . ?
C20A H20A 0.9500 . ?
C20A C21A 1.388(8) . ?
C21 H21 0.9500 . ?
C21 C22 1.386(9) . ?
C21A H21A 0.9500 . ?
C21A C22A 1.384(14) . ?
C22 H22 0.9500 . ?
C22 C23 1.380(4) . ?
C22A H22A 0.9500 . ?
C22A C23A 1.389(8) . ?
C23 C25 1.509(5) . ?
C23A C25A 1.494(6) . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C24A H24D 0.9800 . ?
C24A H24E 0.9800 . ?
C24A H24F 0.9800 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C25A H25D 0.9800 . ?
C25A H25E 0.9800 . ?
C25A H25F 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
O1 V1 N2 85.83(4) . . ?
O2 V1 O1 104.64(9) . . ?
O2 V1 N2 101.35(8) . . ?
C1 O1 V1 129.28(8) . . ?
C8 N1 C9 118.57(11) . . ?
C17 N2 V1 120.45(9) . . ?
C17 N2 C18 113.6(5) . . ?
C17 N2 C18A 116.3(6) . . ?
C18 N2 V1 120.0(5) . . ?
O1 C1 C2 120.14(11) . . ?
O1 C1 C6 122.22(11) . . ?
C2 C1 C6 117.64(11) . . ?
C1 C2 C8 119.46(11) . . ?
C3 C2 C1 119.75(12) . . ?
C3 C2 C8 120.76(12) . . ?
C2 C3 H3 118.5 . . ?
C2 C3 C4 122.95(12) . . ?
C4 C3 H3 118.5 . . ?
C3 C4 C7 121.10(12) . . ?
C5 C4 C3 117.32(12) . . ?
C5 C4 C7 121.51(12) . . ?
C4 C5 H5 119.0 . . ?
C4 C5 C6 121.96(12) . . ?
C6 C5 H5 119.0 . . ?
C1 C6 C17 121.87(11) . . ?
C5 C6 C1 120.23(12) . . ?
C5 C6 C17 117.80(11) . . ?
C4 C7 H7A 109.5 . . ?
C4 C7 H7B 109.5 . . ?
C4 C7 H7C 109.5 . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
N1 C8 C2 121.13(12) . . ?
N1 C8 H8 119.4 . . ?
C2 C8 H8 119.4 . . ?
C10 C9 N1 118.30(13) . . ?
C10 C9 C14 121.68(13) . . ?
C14 C9 N1 119.86(12) . . ?
C9 C10 C15 120.05(14) . . ?
C11 C10 C9 117.95(15) . . ?
C11 C10 C15 121.98(14) . . ?
C10 C11 H11 119.4 . . ?
C12 C11 C10 121.12(15) . . ?
C12 C11 H11 119.4 . . ?
C11 C12 H12 119.9 . . ?
C13 C12 C11 120.26(16) . . ?
C13 C12 H12 119.9 . . ?
C12 C13 H13 119.7 . . ?
C12 C13 C14 120.65(17) . . ?
C14 C13 H13 119.7 . . ?
C9 C14 C16 120.98(14) . . ?
C13 C14 C9 118.33(14) . . ?
C13 C14 C16 120.69(15) . . ?
C10 C15 H15A 109.5 . . ?
C10 C15 H15B 109.5 . . ?
C10 C15 H15C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C14 C16 H16A 109.5 . . ?
C14 C16 H16B 109.5 . . ?
C14 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
N2 C17 C6 127.16(11) . . ?
N2 C17 H17 116.4 . . ?
C6 C17 H17 116.4 . . ?
C19 C18 N2 118.5(4) . . ?
C19 C18 C23 124.4(5) . . ?
C23 C18 N2 117.0(5) . . ?
C19A C18A N2 119.2(6) . . ?
C19A C18A C23A 121.8(7) . . ?
C23A C18A N2 119.0(6) . . ?
C18 C19 C20 116.5(5) . . ?
C18 C19 C24 123.0(4) . . ?
C20 C19 C24 120.5(5) . . ?
C18A C19A C24A 119.3(5) . . ?
C20A C19A C18A 119.2(6) . . ?
C20A C19A C24A 121.5(5) . . ?
C19 C20 H20 119.4 . . ?
C19 C20 C21 121.1(5) . . ?
C21 C20 H20 119.4 . . ?
C19A C20A H20A 120.1 . . ?
C19A C20A C21A 119.8(5) . . ?
C21A C20A H20A 120.1 . . ?
C20 C21 H21 119.8 . . ?
C22 C21 C20 120.4(4) . . ?
C22 C21 H21 119.8 . . ?
C20A C21A H21A 119.6 . . ?
C22A C21A C20A 120.8(5) . . ?
C22A C21A H21A 119.6 . . ?
C21 C22 H22 119.7 . . ?
C23 C22 C21 120.6(4) . . ?
C23 C22 H22 119.7 . . ?
C21A C22A H22A 119.5 . . ?
C21A C22A C23A 120.9(8) . . ?
C23A C22A H22A 119.5 . . ?
C18 C23 C25 121.7(4) . . ?
C22 C23 C18 117.0(5) . . ?
C22 C23 C25 121.3(4) . . ?
C18A C23A C25A 120.6(5) . . ?
C22A C23A C18A 117.4(7) . . ?
C22A C23A C25A 122.0(6) . . ?
C19 C24 H24A 109.5 . . ?
C19 C24 H24B 109.5 . . ?
C19 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C19A C24A H24D 109.5 . . ?
C19A C24A H24E 109.5 . . ?
C19A C24A H24F 109.5 . . ?
H24D C24A H24E 109.5 . . ?
H24D C24A H24F 109.5 . . ?
H24E C24A H24F 109.5 . . ?
C23 C25 H25A 109.5 . . ?
C23 C25 H25B 109.5 . . ?
C23 C25 H25C 109.5 . . ?
H25A C25 H25B 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C23A C25A H25D 109.5 . . ?
C23A C25A H25E 109.5 . . ?
C23A C25A H25F 109.5 . . ?
H25D C25A H25E 109.5 . . ?
H25D C25A H25F 109.5 . . ?
H25E C25A H25F 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 C2 -158.56(10) . . . . ?
V1 O1 C1 C6 22.39(19) . . . . ?
V1 N2 C17 C6 -23.07(18) . . . . ?
V1 N2 C18 C19 106.1(8) . . . . ?
V1 N2 C18 C23 -76.1(9) . . . . ?
O1 C1 C2 C3 176.37(12) . . . . ?
O1 C1 C2 C8 -5.57(19) . . . . ?
O1 C1 C6 C5 -176.95(12) . . . . ?
O1 C1 C6 C17 6.9(2) . . . . ?
N1 C9 C10 C11 176.87(13) . . . . ?
N1 C9 C10 C15 -4.8(2) . . . . ?
N1 C9 C14 C13 -176.54(13) . . . . ?
N1 C9 C14 C16 3.9(2) . . . . ?
N2 C18 C19 C20 177.1(6) . . . . ?
N2 C18 C19 C24 -0.6(12) . . . . ?
N2 C18 C23 C22 -176.6(6) . . . . ?
N2 C18 C23 C25 5.5(11) . . . . ?
N2 C18A C19A C20A 177.2(7) . . . . ?
N2 C18A C19A C24A -2.5(15) . . . . ?
N2 C18A C23A C22A -175.9(9) . . . . ?
N2 C18A C23A C25A 4.0(15) . . . . ?
C1 C2 C3 C4 2.1(2) . . . . ?
C1 C2 C8 N1 -168.72(13) . . . . ?
C1 C6 C17 N2 -3.9(2) . . . . ?
C2 C1 C6 C5 3.97(19) . . . . ?
C2 C1 C6 C17 -172.15(12) . . . . ?
C2 C3 C4 C5 1.02(19) . . . . ?
C2 C3 C4 C7 178.21(13) . . . . ?
C3 C2 C8 N1 9.3(2) . . . . ?
C3 C4 C5 C6 -1.62(19) . . . . ?
C4 C5 C6 C1 -0.9(2) . . . . ?
C4 C5 C6 C17 175.37(12) . . . . ?
C5 C6 C17 N2 179.89(13) . . . . ?
C6 C1 C2 C3 -4.54(19) . . . . ?
C6 C1 C2 C8 173.52(12) . . . . ?
C7 C4 C5 C6 -178.79(13) . . . . ?
C8 N1 C9 C10 105.90(16) . . . . ?
C8 N1 C9 C14 -78.60(17) . . . . ?
C8 C2 C3 C4 -175.91(12) . . . . ?
C9 N1 C8 C2 176.09(13) . . . . ?
C9 C10 C11 C12 -0.4(3) . . . . ?
C10 C9 C14 C13 -1.2(2) . . . . ?
C10 C9 C14 C16 179.21(14) . . . . ?
C10 C11 C12 C13 -0.9(3) . . . . ?
C11 C12 C13 C14 1.2(3) . . . . ?
C12 C13 C14 C9 -0.1(3) . . . . ?
C12 C13 C14 C16 179.45(17) . . . . ?
C14 C9 C10 C11 1.5(2) . . . . ?
C14 C9 C10 C15 179.79(13) . . . . ?
C15 C10 C11 C12 -178.70(16) . . . . ?
C17 N2 C18 C19 -101.0(8) . . . . ?
C17 N2 C18 C23 76.8(9) . . . . ?
C17 N2 C18A C19A -97.6(11) . . . . ?
C17 N2 C18A C23A 81.3(11) . . . . ?
C18 N2 C17 C6 -175.8(3) . . . . ?
C18 C19 C20 C21 0.0(9) . . . . ?
C18A N2 C17 C6 166.7(4) . . . . ?
C18A C19A C20A C21A 0.3(9) . . . . ?
C19 C18 C23 C22 1.1(12) . . . . ?
C19 C18 C23 C25 -176.8(7) . . . . ?
C19 C20 C21 C22 0.0(9) . . . . ?
C19A C18A C23A C22A 3.0(16) . . . . ?
C19A C18A C23A C25A -177.1(8) . . . . ?
C19A C20A C21A C22A -0.4(8) . . . . ?
C20 C21 C22 C23 0.6(9) . . . . ?
C20A C21A C22A C23A 1.8(12) . . . . ?
C21 C22 C23 C18 -1.1(8) . . . . ?
C21 C22 C23 C25 176.8(5) . . . . ?
C21A C22A C23A C18A -3.0(13) . . . . ?
C21A C22A C23A C25A 177.1(6) . . . . ?
C23 C18 C19 C20 -0.5(13) . . . . ?
C23 C18 C19 C24 -178.2(6) . . . . ?
C23A C18A C19A C20A -1.6(16) . . . . ?
C23A C18A C19A C24A 178.7(8) . . . . ?
C24 C19 C20 C21 177.7(5) . . . . ?
C24A C19A C20A C21A 180.0(4) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.169
_oxdiff_exptl_absorpt_empirical_full_min 0.722
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
####################################################################### 
# 
# 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_12
_database_code_depnum_ccdc_archive 'CCDC 2418243'
loop_
_audit_author_name
_audit_author_address
'Timothy Prior'
;University of Hull
United Kingdom
;
_audit_update_record             
;
2025-01-20 deposited with the CCDC.	2025-12-16 downloaded from the CCDC.
;
_audit_creation_date             2022-08-22
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C52 H42 F12 N4 O3 V, C7 H8'
_chemical_formula_sum            'C59 H50 F12 N4 O3 V'
_chemical_formula_weight         1141.97
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C59 H50 F12 N4 O3 V'
_chemical_oxdiff_usercomment     VCF3
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'
F F 0.0727 0.0534 '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'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
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                   34.8959(7)
_cell_length_b                   10.6717(3)
_cell_length_c                   30.5882(7)
_cell_angle_alpha                90
_cell_angle_beta                 109.452(2)
_cell_angle_gamma                90
_cell_volume                     10740.8(5)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    5745
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      74.5220
_cell_measurement_theta_min      2.6720
_shelx_estimated_absorpt_T_max   0.783
_shelx_estimated_absorpt_T_min   0.503
_exptl_absorpt_coefficient_mu    2.340
_exptl_absorpt_correction_T_max  0.820
_exptl_absorpt_correction_T_min  0.582
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.64a (Rigaku Oxford Diffraction, 2022)
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   ?
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.412
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             4696
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-21 -1 0 0.0514
16 -1 -17 0.1483
-4 -1 19 0.1165
-10 -6 3 0.0323
6 7 -3 0.0697
-22 0 1 0.0611
22 1 -2 0.0722
7 -6 -9 0.0981
-11 6 9 0.1185
14 4 -14 0.1183

_exptl_crystal_size_max          0.341
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.11
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-21.2903 -0.5528 0.0010 0.0739 -0.0372 0.9966
16.4410 -1.3215 -17.1648 0.7711 -0.3671 -0.5202
-3.5564 -1.0369 19.3135 -0.6465 0.7577 -0.0890
-10.1337 -6.1961 3.4417 0.4583 0.7490 0.4785
6.3864 6.6252 -3.3859 -0.4968 -0.8112 -0.3084
-21.7909 0.2855 1.3133 -0.0549 -0.0863 0.9948
21.8574 0.5335 -1.6841 -0.0076 -0.0157 -0.9998
6.9426 -6.0365 -9.1830 0.9142 0.3781 -0.1461
-11.4117 5.5982 9.0216 -0.8622 -0.3562 0.3602
13.9238 3.9994 -14.1417 0.1578 -0.8573 -0.4901

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0669
_diffrn_reflns_av_unetI/netI     0.0517
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.961
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -43
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            50560
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.961
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.326
_diffrn_reflns_theta_min         2.686
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'hybrid pixel array detector'
_diffrn_detector_area_resol_mean 10
_diffrn_detector_dtime           0.000
_diffrn_detector_type            'Rigaku, HyPix 6000HE'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.961
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -66.00 -33.00   0.50    0.05    -- -103.00  61.00 -90.00   66
  2  ω   -103.00 -57.00   0.50    0.05    -- -103.00  77.00  30.00   92
  3  ω    -58.00 -32.00   0.50    0.05    -- -103.00  61.00  60.00   52
  4  ω    -21.00  29.00   0.50    0.05    --  -46.61  19.00  90.00  100
  5  ω    -22.00  28.00   0.50    0.05    --  -46.61  19.00-180.00  100
  6  ω   -118.00 -64.00   0.50    0.05    --  -46.61-143.00  21.00  108
  7  ω   -162.00 -85.00   0.50    0.05    -- -103.00-143.00  21.00  154
  8  ω   -125.00 -79.00   0.50    0.05    -- -103.00-127.00-168.00   92
  9  ω   -106.00 -81.00   0.50    0.05    -- -103.00 -74.00 -75.57   50
 10  ω   -174.00 -86.00   0.50    0.05    -- -103.00 -61.00-157.37  176
 11  ω   -155.00-128.00   0.50    0.05    -- -103.00 -74.00 -75.57   54
 12  ω   -125.00 -63.00   0.50    0.05    -- -103.00 143.00  77.00  124
 13  ω     32.00 105.00   0.50    0.05    --   46.61-143.00  21.00  146
 14  ω     32.00 125.00   0.50    0.05    --  101.75-143.00  21.00  186
 15  ω     39.00  78.00   0.50    0.05    --  101.75-125.00-120.00   78
 16  ω     31.00 113.00   0.50    0.05    --  101.75-127.00-168.00  164
 17  ω     84.00 112.00   0.50    0.05    --  101.75-125.00-120.00   56
 18  ω     25.00  94.00   0.50    0.05    --   46.61-127.00-168.00  138
 19  ω     29.00 106.00   0.50    0.05    --  101.75 -94.00-180.00  154
 20  ω    -24.00  28.00   0.50    0.05    --   46.61 -19.00-120.00  104
 21  ω     53.00 105.00   0.50    0.05    --  101.75-101.00  36.70  104
 22  ω     95.00 170.00   0.50    0.05    --  101.75  61.00   0.00  150
 23  ω     70.00 118.00   0.50    0.05    --   46.61 143.00  77.00   96
 24  ω     70.00 171.00   0.50    0.05    --  101.75 143.00  77.00  202
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_details 'Rigaku, UG2 κ goniometer'
_diffrn_measurement_device_type  
'Rigaku 007HF equipped with Arc)Sec VHF Varimax confocal mirrors and a UG2 goniometer and HyPix 6000HE detector'
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_measurement_specimen_support 'MiTeGen loops'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0010398000
_diffrn_orient_matrix_UB_12      -0.0937661000
_diffrn_orient_matrix_UB_13      -0.0387005000
_diffrn_orient_matrix_UB_21      0.0045881000
_diffrn_orient_matrix_UB_22      -0.1093857000
_diffrn_orient_matrix_UB_23      0.0342030000
_diffrn_orient_matrix_UB_31      -0.0465855000
_diffrn_orient_matrix_UB_32      -0.0086170000
_diffrn_orient_matrix_UB_33      -0.0136500000
_diffrn_radiation_collimation    'Arc)Sec VHF Varimax focusing mirrors'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'Rotating anode'
_diffrn_source_current           30.0
_diffrn_source_power             1.2
_diffrn_source_target            Cu
_diffrn_source_type              'Rigaku 007 HF'
_diffrn_source_voltage           40.0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                9036
_reflns_number_total             10685
_reflns_odcompleteness_completeness 99.51
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     68.13
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.42.64a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.64a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.64a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         1.096
_refine_diff_density_min         -0.465
_refine_diff_density_rms         0.069
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     719
_refine_ls_number_reflns         10685
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0607
_refine_ls_R_factor_gt           0.0522
_refine_ls_restrained_S_all      1.066
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0880P)²+7.8994P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1446
_refine_ls_wR_factor_ref         0.1506
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C7(H7), C12(H12), C15(H15), C16(H16), C17(H17), C18(H18),
 C22(H22), C23(H23), C24(H24), C25(H25), C29(H29), C31(H31), C33(H33), C40(H40),
  C41(H41), C42(H42), C43(H43), C45(H45), C48(H48), C49(H49), C50(H50),
 C51(H51), C53(H53), C54(H54), C56(H56), C57(H57), C58(H58)
2.b Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C35(H35A,H35B,
 H35C), C36(H36A,H36B,H36C), C37(H37A,H37B,H37C), C59(H59A,H59B,H59C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
V1 V 0.66190(2) 0.67766(3) 0.47094(2) 0.01834(11) Uani 1 1 d . . . . .
F1 F 0.67065(5) 0.82223(18) 0.18204(5) 0.0500(4) Uani 1 1 d . . . . .
F2 F 0.68796(4) 0.97016(16) 0.23228(5) 0.0401(4) Uani 1 1 d . . . . .
F3 F 0.68751(4) 0.77916(16) 0.25453(5) 0.0392(3) Uani 1 1 d . . . . .
F4 F 0.64746(4) 1.03908(14) 0.54723(6) 0.0426(4) Uani 1 1 d . . . . .
F5 F 0.61887(5) 0.98003(18) 0.59587(6) 0.0505(4) Uani 1 1 d . . . . .
F6 F 0.61111(4) 0.87385(15) 0.53392(5) 0.0400(4) Uani 1 1 d . . . . .
F7 F 0.58334(6) 0.7777(2) 0.63363(7) 0.0671(5) Uani 1 1 d . . . . .
F8 F 0.57671(7) 0.8148(2) 0.69980(8) 0.0746(6) Uani 1 1 d . . . . .
F9 F 0.55792(6) 0.6383(2) 0.66676(9) 0.0700(6) Uani 1 1 d . . . . .
F10 F 0.54852(5) 0.7252(2) 0.37440(6) 0.0581(5) Uani 1 1 d . . . . .
F11 F 0.52386(5) 0.5464(2) 0.34976(7) 0.0620(5) Uani 1 1 d . . . . .
F12 F 0.51875(5) 0.69394(19) 0.30174(5) 0.0524(5) Uani 1 1 d . . . . .
O1 O 0.65093(4) 0.80936(14) 0.42494(5) 0.0196(3) Uani 1 1 d . . . . .
O2 O 0.63891(4) 0.61301(14) 0.51525(5) 0.0227(3) Uani 1 1 d . . . . .
O3 O 0.70204(4) 0.60448(16) 0.47235(5) 0.0266(3) Uani 1 1 d . . . . .
N1 N 0.64608(5) 0.95091(19) 0.29866(6) 0.0259(4) Uani 1 1 d . . . . .
N2 N 0.68870(5) 0.81716(17) 0.52047(6) 0.0198(4) Uani 1 1 d . . . . .
N3 N 0.61855(6) 0.5230(2) 0.63564(7) 0.0336(5) Uani 1 1 d . . . . .
N4 N 0.61854(5) 0.57209(17) 0.41977(5) 0.0195(3) Uani 1 1 d . . . . .
C1 C 0.67569(6) 0.9018(2) 0.42377(7) 0.0185(4) Uani 1 1 d . . . . .
C2 C 0.70417(6) 0.9527(2) 0.46427(7) 0.0192(4) Uani 1 1 d . . . . .
C3 C 0.73122(6) 1.0466(2) 0.46158(7) 0.0205(4) Uani 1 1 d . . . . .
H3 H 0.749836 1.078984 0.489530 0.025 Uiso 1 1 calc R U . . .
C4 C 0.73195(6) 1.0942(2) 0.41978(7) 0.0213(4) Uani 1 1 d . . . . .
C5 C 0.70243(6) 1.0478(2) 0.37999(7) 0.0221(4) Uani 1 1 d . . . . .
H5 H 0.701266 1.080982 0.350755 0.027 Uiso 1 1 calc R U . . .
C6 C 0.67475(6) 0.9557(2) 0.38109(7) 0.0201(4) Uani 1 1 d . . . . .
C7 C 0.64422(6) 0.9139(2) 0.33747(7) 0.0221(4) Uani 1 1 d . . . . .
H7 H 0.623030 0.858988 0.338283 0.027 Uiso 1 1 calc R U . . .
C8 C 0.76274(7) 1.1929(2) 0.41663(8) 0.0259(5) Uani 1 1 d . . . . .
C9 C 0.79728(7) 1.2088(2) 0.46365(8) 0.0306(5) Uani 1 1 d . . . . .
H9A H 0.817543 1.267738 0.460036 0.046 Uiso 1 1 calc R U . . .
H9B H 0.810169 1.127431 0.473912 0.046 Uiso 1 1 calc R U . . .
H9C H 0.785987 1.241174 0.486766 0.046 Uiso 1 1 calc R U . . .
C10 C 0.74095(8) 1.3184(2) 0.40196(8) 0.0322(5) Uani 1 1 d . . . . .
H10A H 0.730590 1.348108 0.426221 0.048 Uiso 1 1 calc R U . . .
H10B H 0.718246 1.307399 0.372959 0.048 Uiso 1 1 calc R U . . .
H10C H 0.760068 1.379996 0.397320 0.048 Uiso 1 1 calc R U . . .
C11 C 0.78224(8) 1.1508(3) 0.38083(9) 0.0375(6) Uani 1 1 d . . . . .
H11A H 0.802758 1.212198 0.379645 0.056 Uiso 1 1 calc R U . . .
H11B H 0.761251 1.144526 0.350230 0.056 Uiso 1 1 calc R U . . .
H11C H 0.795143 1.068869 0.389776 0.056 Uiso 1 1 calc R U . . .
C12 C 0.70675(6) 0.9124(2) 0.50991(7) 0.0201(4) Uani 1 1 d . . . . .
H12 H 0.723508 0.960960 0.535060 0.024 Uiso 1 1 calc R U . . .
C13 C 0.61423(7) 0.9181(2) 0.25806(7) 0.0262(5) Uani 1 1 d . . . . .
C14 C 0.62352(7) 0.8760(3) 0.21921(8) 0.0314(5) Uani 1 1 d . . . . .
C15 C 0.59231(8) 0.8461(3) 0.17847(8) 0.0405(6) Uani 1 1 d . . . . .
H15 H 0.598621 0.814768 0.152603 0.049 Uiso 1 1 calc R U . . .
C16 C 0.55212(8) 0.8618(3) 0.17545(9) 0.0456(7) Uani 1 1 d . . . . .
H16 H 0.530911 0.841826 0.147506 0.055 Uiso 1 1 calc R U . . .
C17 C 0.54294(8) 0.9066(3) 0.21319(9) 0.0392(6) Uani 1 1 d . . . . .
H17 H 0.515362 0.918205 0.210947 0.047 Uiso 1 1 calc R U . . .
C18 C 0.57352(7) 0.9346(2) 0.25412(8) 0.0323(5) Uani 1 1 d . . . . .
H18 H 0.566806 0.965358 0.279809 0.039 Uiso 1 1 calc R U . . .
C19 C 0.66692(8) 0.8621(3) 0.22225(8) 0.0338(5) Uani 1 1 d . . . . .
C20 C 0.69762(6) 0.8006(2) 0.56974(7) 0.0202(4) Uani 1 1 d . . . . .
C21 C 0.67508(6) 0.8616(2) 0.59340(7) 0.0228(4) Uani 1 1 d . . . . .
C22 C 0.68727(7) 0.8542(2) 0.64146(7) 0.0258(5) Uani 1 1 d . . . . .
H22 H 0.672035 0.895619 0.657734 0.031 Uiso 1 1 calc R U . . .
C23 C 0.72173(7) 0.7862(2) 0.66568(7) 0.0289(5) Uani 1 1 d . . . . .
H23 H 0.730582 0.783697 0.698588 0.035 Uiso 1 1 calc R U . . .
C24 C 0.74324(7) 0.7221(2) 0.64205(7) 0.0286(5) Uani 1 1 d . . . . .
H24 H 0.766239 0.673143 0.658597 0.034 Uiso 1 1 calc R U . . .
C25 C 0.73099(6) 0.7297(2) 0.59385(7) 0.0259(5) Uani 1 1 d . . . . .
H25 H 0.745699 0.685784 0.577535 0.031 Uiso 1 1 calc R U . . .
C26 C 0.63800(7) 0.9374(2) 0.56771(8) 0.0279(5) Uani 1 1 d . . . . .
C27 C 0.61186(6) 0.5252(2) 0.51351(7) 0.0194(4) Uani 1 1 d . . . . .
C28 C 0.60350(6) 0.4910(2) 0.55418(7) 0.0217(4) Uani 1 1 d . . . . .
C29 C 0.57327(6) 0.4035(2) 0.55163(7) 0.0221(4) Uani 1 1 d . . . . .
H29 H 0.568115 0.382773 0.579359 0.027 Uiso 1 1 calc R U . . .
C30 C 0.55008(6) 0.3446(2) 0.51061(7) 0.0206(4) Uani 1 1 d . . . . .
C31 C 0.55972(6) 0.3736(2) 0.47141(7) 0.0201(4) Uani 1 1 d . . . . .
H31 H 0.545439 0.332628 0.443097 0.024 Uiso 1 1 calc R U . . .
C32 C 0.59003(6) 0.46209(19) 0.47195(7) 0.0190(4) Uani 1 1 d . . . . .
C33 C 0.62654(6) 0.5481(2) 0.59909(7) 0.0245(4) Uani 1 1 d . . . . .
H33 H 0.647887 0.605135 0.600702 0.029 Uiso 1 1 calc R U . . .
C34 C 0.51573(6) 0.2548(2) 0.51037(7) 0.0225(4) Uani 1 1 d . . . . .
C35 C 0.48836(7) 0.3168(2) 0.53433(10) 0.0355(6) Uani 1 1 d . . . . .
H35A H 0.466064 0.259874 0.533393 0.053 Uiso 1 1 calc R U . . .
H35B H 0.477192 0.394877 0.518242 0.053 Uiso 1 1 calc R U . . .
H35C H 0.504335 0.335260 0.566661 0.053 Uiso 1 1 calc R U . . .
C36 C 0.48902(7) 0.2208(3) 0.46100(8) 0.0332(5) Uani 1 1 d . . . . .
H36A H 0.505437 0.176955 0.445301 0.050 Uiso 1 1 calc R U . . .
H36B H 0.477715 0.297369 0.443883 0.050 Uiso 1 1 calc R U . . .
H36C H 0.466815 0.166167 0.462203 0.050 Uiso 1 1 calc R U . . .
C37 C 0.53415(7) 0.1351(2) 0.53680(8) 0.0291(5) Uani 1 1 d . . . . .
H37A H 0.512299 0.080095 0.538759 0.044 Uiso 1 1 calc R U . . .
H37B H 0.551854 0.157070 0.568122 0.044 Uiso 1 1 calc R U . . .
H37C H 0.550067 0.091712 0.520395 0.044 Uiso 1 1 calc R U . . .
C38 C 0.64288(7) 0.5758(2) 0.67824(8) 0.0311(5) Uani 1 1 d . . . . .
C39 C 0.62821(8) 0.6743(3) 0.69838(9) 0.0356(6) Uani 1 1 d . . . . .
C40 C 0.65277(9) 0.7263(3) 0.74032(9) 0.0423(6) Uani 1 1 d . . . . .
H40 H 0.643109 0.794979 0.753460 0.051 Uiso 1 1 calc R U . . .
C41 C 0.69077(9) 0.6784(3) 0.76249(9) 0.0455(7) Uani 1 1 d . . . . .
H41 H 0.707546 0.715070 0.790675 0.055 Uiso 1 1 calc R U . . .
C42 C 0.70482(8) 0.5767(3) 0.74395(9) 0.0448(7) Uani 1 1 d . . . . .
H42 H 0.730753 0.542005 0.760082 0.054 Uiso 1 1 calc R U . . .
C43 C 0.68115(8) 0.5256(3) 0.70200(9) 0.0373(6) Uani 1 1 d . . . . .
H43 H 0.690979 0.456328 0.689356 0.045 Uiso 1 1 calc R U . . .
C44 C 0.58696(10) 0.7252(3) 0.67472(11) 0.0495(7) Uani 1 1 d . . . . .
C45 C 0.59524(6) 0.4874(2) 0.42819(7) 0.0202(4) Uani 1 1 d . . . . .
H45 H 0.580046 0.436891 0.402740 0.024 Uiso 1 1 calc R U . . .
C46 C 0.61860(6) 0.5806(2) 0.37280(7) 0.0213(4) Uani 1 1 d . . . . .
C47 C 0.58384(7) 0.6080(2) 0.33489(7) 0.0268(5) Uani 1 1 d . . . . .
C48 C 0.58645(8) 0.6088(2) 0.29018(8) 0.0327(5) Uani 1 1 d . . . . .
H48 H 0.562794 0.624908 0.264296 0.039 Uiso 1 1 calc R U . . .
C49 C 0.62288(8) 0.5864(2) 0.28326(8) 0.0346(5) Uani 1 1 d . . . . .
H49 H 0.624157 0.585205 0.252716 0.042 Uiso 1 1 calc R U . . .
C50 C 0.65735(8) 0.5657(2) 0.32061(8) 0.0323(5) Uani 1 1 d . . . . .
H50 H 0.682679 0.553695 0.315918 0.039 Uiso 1 1 calc R U . . .
C51 C 0.65541(7) 0.5622(2) 0.36525(8) 0.0270(5) Uani 1 1 d . . . . .
H51 H 0.679402 0.547176 0.390831 0.032 Uiso 1 1 calc R U . . .
C52 C 0.54416(7) 0.6431(3) 0.34029(8) 0.0366(6) Uani 1 1 d . . . . .
C53 C 0.53947(11) 1.1400(4) 0.35728(13) 0.0615(9) Uani 1 1 d . . . . .
H53 H 0.517072 1.099391 0.362327 0.074 Uiso 1 1 calc R U . . .
C54 C 0.60962(12) 1.1899(4) 0.38145(17) 0.0742(12) Uani 1 1 d . . . . .
H54 H 0.636033 1.185925 0.403955 0.089 Uiso 1 1 calc R U . . .
C55 C 0.57671(12) 1.1278(4) 0.38991(13) 0.0618(9) Uani 1 1 d . . . . .
C56 C 0.60363(15) 1.2557(4) 0.34102(18) 0.0764(12) Uani 1 1 d . . . . .
H56 H 0.625908 1.294855 0.335208 0.092 Uiso 1 1 calc R U . . .
C57 C 0.53260(15) 1.2074(5) 0.31770(15) 0.0786(12) Uani 1 1 d . . . . .
H57 H 0.505792 1.215306 0.296313 0.094 Uiso 1 1 calc R U . . .
C58 C 0.5647(2) 1.2644(4) 0.30866(17) 0.0898(15) Uani 1 1 d . . . . .
H58 H 0.560188 1.309261 0.280568 0.108 Uiso 1 1 calc R U . . .
C59 C 0.58379(19) 1.0497(6) 0.43314(16) 0.110(2) Uani 1 1 d . . . . .
H59A H 0.558012 1.012875 0.432935 0.166 Uiso 1 1 calc R U . . .
H59B H 0.594744 1.102978 0.460594 0.166 Uiso 1 1 calc R U . . .
H59C H 0.603211 0.982747 0.433898 0.166 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 O1 1.9347(15) . ?
V1 O2 1.9186(14) . ?
V1 O3 1.5918(15) . ?
V1 N2 2.1076(17) . ?
V1 N4 2.1050(17) . ?
F1 C19 1.348(3) . ?
F2 C19 1.347(3) . ?
F3 C19 1.342(3) . ?
F4 C26 1.348(3) . ?
F5 C26 1.333(3) . ?
F6 C26 1.328(3) . ?
F7 C44 1.343(4) . ?
F8 C44 1.347(4) . ?
F9 C44 1.335(4) . ?
F10 C52 1.331(3) . ?
F11 C52 1.337(3) . ?
F12 C52 1.332(3) . ?
O1 C1 1.320(3) . ?
O2 C27 1.318(2) . ?
N1 C7 1.273(3) . ?
N1 C13 1.407(3) . ?
N2 C12 1.292(3) . ?
N2 C20 1.445(3) . ?
N3 C33 1.268(3) . ?
N3 C38 1.414(3) . ?
N4 C45 1.298(3) . ?
N4 C46 1.440(3) . ?
C1 C2 1.413(3) . ?
C1 C6 1.417(3) . ?
C2 C3 1.398(3) . ?
C2 C12 1.435(3) . ?
C3 H3 0.9500 . ?
C3 C4 1.384(3) . ?
C4 C5 1.398(3) . ?
C4 C8 1.530(3) . ?
C5 H5 0.9500 . ?
C5 C6 1.386(3) . ?
C6 C7 1.472(3) . ?
C7 H7 0.9500 . ?
C8 C9 1.547(3) . ?
C8 C10 1.531(3) . ?
C8 C11 1.536(3) . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12 0.9500 . ?
C13 C14 1.406(3) . ?
C13 C18 1.396(3) . ?
C14 C15 1.392(3) . ?
C14 C19 1.493(4) . ?
C15 H15 0.9500 . ?
C15 C16 1.385(4) . ?
C16 H16 0.9500 . ?
C16 C17 1.382(4) . ?
C17 H17 0.9500 . ?
C17 C18 1.380(3) . ?
C18 H18 0.9500 . ?
C20 C21 1.395(3) . ?
C20 C25 1.379(3) . ?
C21 C22 1.390(3) . ?
C21 C26 1.507(3) . ?
C22 H22 0.9500 . ?
C22 C23 1.388(3) . ?
C23 H23 0.9500 . ?
C23 C24 1.384(3) . ?
C24 H24 0.9500 . ?
C24 C25 1.394(3) . ?
C25 H25 0.9500 . ?
C27 C28 1.417(3) . ?
C27 C32 1.416(3) . ?
C28 C29 1.391(3) . ?
C28 C33 1.473(3) . ?
C29 H29 0.9500 . ?
C29 C30 1.396(3) . ?
C30 C31 1.384(3) . ?
C30 C34 1.533(3) . ?
C31 H31 0.9500 . ?
C31 C32 1.414(3) . ?
C32 C45 1.435(3) . ?
C33 H33 0.9500 . ?
C34 C35 1.534(3) . ?
C34 C36 1.531(3) . ?
C34 C37 1.534(3) . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C38 C39 1.398(4) . ?
C38 C43 1.397(4) . ?
C39 C40 1.399(4) . ?
C39 C44 1.483(4) . ?
C40 H40 0.9500 . ?
C40 C41 1.371(4) . ?
C41 H41 0.9500 . ?
C41 C42 1.387(5) . ?
C42 H42 0.9500 . ?
C42 C43 1.386(4) . ?
C43 H43 0.9500 . ?
C45 H45 0.9500 . ?
C46 C47 1.402(3) . ?
C46 C51 1.393(3) . ?
C47 C48 1.401(3) . ?
C47 C52 1.496(3) . ?
C48 H48 0.9500 . ?
C48 C49 1.378(4) . ?
C49 H49 0.9500 . ?
C49 C50 1.373(4) . ?
C50 H50 0.9500 . ?
C50 C51 1.390(3) . ?
C51 H51 0.9500 . ?
C53 H53 0.9500 . ?
C53 C55 1.356(5) . ?
C53 C57 1.359(6) . ?
C54 H54 0.9500 . ?
C54 C55 1.422(6) . ?
C54 C56 1.376(7) . ?
C55 C59 1.512(6) . ?
C56 H56 0.9500 . ?
C56 C58 1.393(7) . ?
C57 H57 0.9500 . ?
C57 C58 1.380(7) . ?
C58 H58 0.9500 . ?
C59 H59A 0.9800 . ?
C59 H59B 0.9800 . ?
C59 H59C 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
O1 V1 N2 86.71(7) . . ?
O1 V1 N4 85.92(6) . . ?
O2 V1 O1 138.33(6) . . ?
O2 V1 N2 86.34(6) . . ?
O2 V1 N4 88.09(6) . . ?
O3 V1 O1 109.59(7) . . ?
O3 V1 O2 112.07(8) . . ?
O3 V1 N2 98.70(7) . . ?
O3 V1 N4 99.54(8) . . ?
N4 V1 N2 161.71(7) . . ?
C1 O1 V1 126.16(12) . . ?
C27 O2 V1 133.57(13) . . ?
C7 N1 C13 118.37(19) . . ?
C12 N2 V1 120.84(14) . . ?
C12 N2 C20 113.77(17) . . ?
C20 N2 V1 123.61(14) . . ?
C33 N3 C38 119.18(19) . . ?
C45 N4 V1 124.61(13) . . ?
C45 N4 C46 116.79(17) . . ?
C46 N4 V1 117.95(13) . . ?
O1 C1 C2 122.61(18) . . ?
O1 C1 C6 120.91(18) . . ?
C2 C1 C6 116.47(18) . . ?
C1 C2 C12 122.40(19) . . ?
C3 C2 C1 121.01(18) . . ?
C3 C2 C12 116.59(18) . . ?
C2 C3 H3 118.7 . . ?
C4 C3 C2 122.57(19) . . ?
C4 C3 H3 118.7 . . ?
C3 C4 C5 116.06(19) . . ?
C3 C4 C8 122.69(19) . . ?
C5 C4 C8 121.25(19) . . ?
C4 C5 H5 118.4 . . ?
C6 C5 C4 123.21(19) . . ?
C6 C5 H5 118.4 . . ?
C1 C6 C7 119.99(19) . . ?
C5 C6 C1 120.50(18) . . ?
C5 C6 C7 119.51(18) . . ?
N1 C7 C6 120.3(2) . . ?
N1 C7 H7 119.8 . . ?
C6 C7 H7 119.8 . . ?
C4 C8 C9 111.26(18) . . ?
C4 C8 C10 109.25(18) . . ?
C4 C8 C11 109.29(19) . . ?
C10 C8 C9 109.5(2) . . ?
C10 C8 C11 110.0(2) . . ?
C11 C8 C9 107.56(19) . . ?
C8 C9 H9A 109.5 . . ?
C8 C9 H9B 109.5 . . ?
C8 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C8 C10 H10A 109.5 . . ?
C8 C10 H10B 109.5 . . ?
C8 C10 H10C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C8 C11 H11A 109.5 . . ?
C8 C11 H11B 109.5 . . ?
C8 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
N2 C12 C2 126.95(19) . . ?
N2 C12 H12 116.5 . . ?
C2 C12 H12 116.5 . . ?
C14 C13 N1 119.3(2) . . ?
C18 C13 N1 121.8(2) . . ?
C18 C13 C14 118.8(2) . . ?
C13 C14 C19 119.6(2) . . ?
C15 C14 C13 119.9(2) . . ?
C15 C14 C19 120.5(2) . . ?
C14 C15 H15 119.8 . . ?
C16 C15 C14 120.3(2) . . ?
C16 C15 H15 119.8 . . ?
C15 C16 H16 120.1 . . ?
C17 C16 C15 119.8(2) . . ?
C17 C16 H16 120.1 . . ?
C16 C17 H17 119.7 . . ?
C18 C17 C16 120.6(2) . . ?
C18 C17 H17 119.7 . . ?
C13 C18 H18 119.7 . . ?
C17 C18 C13 120.5(2) . . ?
C17 C18 H18 119.7 . . ?
F1 C19 C14 112.3(2) . . ?
F2 C19 F1 105.5(2) . . ?
F2 C19 C14 113.2(2) . . ?
F3 C19 F1 105.8(2) . . ?
F3 C19 F2 106.22(19) . . ?
F3 C19 C14 113.2(2) . . ?
C21 C20 N2 121.45(19) . . ?
C25 C20 N2 118.38(18) . . ?
C25 C20 C21 120.02(19) . . ?
C20 C21 C26 120.97(19) . . ?
C22 C21 C20 119.7(2) . . ?
C22 C21 C26 119.31(19) . . ?
C21 C22 H22 120.0 . . ?
C23 C22 C21 120.0(2) . . ?
C23 C22 H22 120.0 . . ?
C22 C23 H23 119.9 . . ?
C24 C23 C22 120.2(2) . . ?
C24 C23 H23 119.9 . . ?
C23 C24 H24 120.2 . . ?
C23 C24 C25 119.7(2) . . ?
C25 C24 H24 120.2 . . ?
C20 C25 C24 120.3(2) . . ?
C20 C25 H25 119.8 . . ?
C24 C25 H25 119.8 . . ?
F4 C26 C21 111.97(18) . . ?
F5 C26 F4 106.2(2) . . ?
F5 C26 C21 111.97(19) . . ?
F6 C26 F4 105.57(19) . . ?
F6 C26 F5 107.53(18) . . ?
F6 C26 C21 113.16(19) . . ?
O2 C27 C28 120.09(18) . . ?
O2 C27 C32 122.57(18) . . ?
C32 C27 C28 117.34(18) . . ?
C27 C28 C33 120.28(19) . . ?
C29 C28 C27 119.83(19) . . ?
C29 C28 C33 119.89(19) . . ?
C28 C29 H29 118.2 . . ?
C28 C29 C30 123.68(19) . . ?
C30 C29 H29 118.2 . . ?
C29 C30 C34 120.30(18) . . ?
C31 C30 C29 116.26(19) . . ?
C31 C30 C34 123.44(19) . . ?
C30 C31 H31 118.8 . . ?
C30 C31 C32 122.42(19) . . ?
C32 C31 H31 118.8 . . ?
C27 C32 C45 123.39(18) . . ?
C31 C32 C27 120.33(18) . . ?
C31 C32 C45 116.20(18) . . ?
N3 C33 C28 121.5(2) . . ?
N3 C33 H33 119.2 . . ?
C28 C33 H33 119.2 . . ?
C30 C34 C35 109.79(18) . . ?
C30 C34 C37 109.16(17) . . ?
C35 C34 C37 109.00(19) . . ?
C36 C34 C30 111.81(18) . . ?
C36 C34 C35 107.59(19) . . ?
C36 C34 C37 109.43(19) . . ?
C34 C35 H35A 109.5 . . ?
C34 C35 H35B 109.5 . . ?
C34 C35 H35C 109.5 . . ?
H35A C35 H35B 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C34 C36 H36A 109.5 . . ?
C34 C36 H36B 109.5 . . ?
C34 C36 H36C 109.5 . . ?
H36A C36 H36B 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C34 C37 H37A 109.5 . . ?
C34 C37 H37B 109.5 . . ?
C34 C37 H37C 109.5 . . ?
H37A C37 H37B 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
C39 C38 N3 120.7(2) . . ?
C43 C38 N3 120.2(2) . . ?
C43 C38 C39 119.0(2) . . ?
C38 C39 C40 120.0(3) . . ?
C38 C39 C44 119.9(2) . . ?
C40 C39 C44 120.1(3) . . ?
C39 C40 H40 119.9 . . ?
C41 C40 C39 120.1(3) . . ?
C41 C40 H40 119.9 . . ?
C40 C41 H41 119.9 . . ?
C40 C41 C42 120.3(2) . . ?
C42 C41 H41 119.9 . . ?
C41 C42 H42 119.9 . . ?
C43 C42 C41 120.2(3) . . ?
C43 C42 H42 119.9 . . ?
C38 C43 H43 119.9 . . ?
C42 C43 C38 120.2(3) . . ?
C42 C43 H43 119.9 . . ?
F7 C44 F8 106.1(3) . . ?
F7 C44 C39 112.5(3) . . ?
F8 C44 C39 112.4(2) . . ?
F9 C44 F7 106.9(3) . . ?
F9 C44 F8 105.5(3) . . ?
F9 C44 C39 112.9(3) . . ?
N4 C45 C32 126.76(19) . . ?
N4 C45 H45 116.6 . . ?
C32 C45 H45 116.6 . . ?
C47 C46 N4 123.38(19) . . ?
C51 C46 N4 117.67(18) . . ?
C51 C46 C47 118.94(19) . . ?
C46 C47 C52 122.6(2) . . ?
C48 C47 C46 119.3(2) . . ?
C48 C47 C52 118.0(2) . . ?
C47 C48 H48 119.6 . . ?
C49 C48 C47 120.8(2) . . ?
C49 C48 H48 119.6 . . ?
C48 C49 H49 120.1 . . ?
C50 C49 C48 119.8(2) . . ?
C50 C49 H49 120.1 . . ?
C49 C50 H50 119.8 . . ?
C49 C50 C51 120.4(2) . . ?
C51 C50 H50 119.8 . . ?
C46 C51 H51 119.7 . . ?
C50 C51 C46 120.6(2) . . ?
C50 C51 H51 119.7 . . ?
F10 C52 F11 105.6(2) . . ?
F10 C52 F12 107.1(2) . . ?
F10 C52 C47 112.5(2) . . ?
F11 C52 C47 114.0(2) . . ?
F12 C52 F11 105.2(2) . . ?
F12 C52 C47 111.8(2) . . ?
C55 C53 H53 118.4 . . ?
C55 C53 C57 123.2(4) . . ?
C57 C53 H53 118.4 . . ?
C55 C54 H54 119.6 . . ?
C56 C54 H54 119.6 . . ?
C56 C54 C55 120.7(4) . . ?
C53 C55 C54 117.1(4) . . ?
C53 C55 C59 122.3(4) . . ?
C54 C55 C59 120.6(4) . . ?
C54 C56 H56 120.2 . . ?
C54 C56 C58 119.5(4) . . ?
C58 C56 H56 120.2 . . ?
C53 C57 H57 120.1 . . ?
C53 C57 C58 119.8(4) . . ?
C58 C57 H57 120.1 . . ?
C56 C58 H58 120.2 . . ?
C57 C58 C56 119.5(4) . . ?
C57 C58 H58 120.2 . . ?
C55 C59 H59A 109.5 . . ?
C55 C59 H59B 109.5 . . ?
C55 C59 H59C 109.5 . . ?
H59A C59 H59B 109.5 . . ?
H59A C59 H59C 109.5 . . ?
H59B C59 H59C 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 C2 -30.2(3) . . . . ?
V1 O1 C1 C6 150.01(15) . . . . ?
V1 O2 C27 C28 174.55(15) . . . . ?
V1 O2 C27 C32 -5.8(3) . . . . ?
V1 N2 C12 C2 14.3(3) . . . . ?
V1 N2 C20 C21 -108.2(2) . . . . ?
V1 N2 C20 C25 76.3(2) . . . . ?
V1 N4 C45 C32 9.8(3) . . . . ?
V1 N4 C46 C47 -128.08(19) . . . . ?
V1 N4 C46 C51 50.9(2) . . . . ?
O1 C1 C2 C3 176.95(18) . . . . ?
O1 C1 C2 C12 -3.6(3) . . . . ?
O1 C1 C6 C5 -176.28(19) . . . . ?
O1 C1 C6 C7 3.7(3) . . . . ?
O2 C27 C28 C29 176.27(19) . . . . ?
O2 C27 C28 C33 -3.4(3) . . . . ?
O2 C27 C32 C31 -176.43(19) . . . . ?
O2 C27 C32 C45 0.1(3) . . . . ?
N1 C13 C14 C15 -178.5(2) . . . . ?
N1 C13 C14 C19 2.3(4) . . . . ?
N1 C13 C18 C17 177.2(2) . . . . ?
N2 C20 C21 C22 -173.04(19) . . . . ?
N2 C20 C21 C26 5.9(3) . . . . ?
N2 C20 C25 C24 173.2(2) . . . . ?
N3 C38 C39 C40 -179.4(2) . . . . ?
N3 C38 C39 C44 -0.8(4) . . . . ?
N3 C38 C43 C42 -179.4(2) . . . . ?
N4 C46 C47 C48 -177.2(2) . . . . ?
N4 C46 C47 C52 6.0(4) . . . . ?
N4 C46 C51 C50 178.2(2) . . . . ?
C1 C2 C3 C4 -0.4(3) . . . . ?
C1 C2 C12 N2 10.2(3) . . . . ?
C1 C6 C7 N1 -171.8(2) . . . . ?
C2 C1 C6 C5 3.9(3) . . . . ?
C2 C1 C6 C7 -176.03(18) . . . . ?
C2 C3 C4 C5 3.3(3) . . . . ?
C2 C3 C4 C8 -177.27(19) . . . . ?
C3 C2 C12 N2 -170.4(2) . . . . ?
C3 C4 C5 C6 -2.7(3) . . . . ?
C3 C4 C8 C9 12.4(3) . . . . ?
C3 C4 C8 C10 -108.6(2) . . . . ?
C3 C4 C8 C11 131.0(2) . . . . ?
C4 C5 C6 C1 -1.0(3) . . . . ?
C4 C5 C6 C7 179.0(2) . . . . ?
C5 C4 C8 C9 -168.2(2) . . . . ?
C5 C4 C8 C10 70.7(3) . . . . ?
C5 C4 C8 C11 -49.6(3) . . . . ?
C5 C6 C7 N1 8.2(3) . . . . ?
C6 C1 C2 C3 -3.3(3) . . . . ?
C6 C1 C2 C12 176.17(19) . . . . ?
C7 N1 C13 C14 -136.2(2) . . . . ?
C7 N1 C13 C18 48.4(3) . . . . ?
C8 C4 C5 C6 178.0(2) . . . . ?
C12 N2 C20 C21 87.0(2) . . . . ?
C12 N2 C20 C25 -88.5(2) . . . . ?
C12 C2 C3 C4 -179.88(19) . . . . ?
C13 N1 C7 C6 -174.2(2) . . . . ?
C13 C14 C15 C16 2.3(4) . . . . ?
C13 C14 C19 F1 -179.3(2) . . . . ?
C13 C14 C19 F2 -60.0(3) . . . . ?
C13 C14 C19 F3 60.9(3) . . . . ?
C14 C13 C18 C17 1.8(4) . . . . ?
C14 C15 C16 C17 -0.4(5) . . . . ?
C15 C14 C19 F1 1.5(4) . . . . ?
C15 C14 C19 F2 120.8(3) . . . . ?
C15 C14 C19 F3 -118.3(3) . . . . ?
C15 C16 C17 C18 -0.7(5) . . . . ?
C16 C17 C18 C13 0.0(4) . . . . ?
C18 C13 C14 C15 -2.9(4) . . . . ?
C18 C13 C14 C19 177.9(2) . . . . ?
C19 C14 C15 C16 -178.6(3) . . . . ?
C20 N2 C12 C2 179.64(19) . . . . ?
C20 C21 C22 C23 -0.1(3) . . . . ?
C20 C21 C26 F4 -65.8(3) . . . . ?
C20 C21 C26 F5 175.1(2) . . . . ?
C20 C21 C26 F6 53.4(3) . . . . ?
C21 C20 C25 C24 -2.3(3) . . . . ?
C21 C22 C23 C24 -2.2(4) . . . . ?
C22 C21 C26 F4 113.2(2) . . . . ?
C22 C21 C26 F5 -6.0(3) . . . . ?
C22 C21 C26 F6 -127.7(2) . . . . ?
C22 C23 C24 C25 2.3(4) . . . . ?
C23 C24 C25 C20 0.0(4) . . . . ?
C25 C20 C21 C22 2.4(3) . . . . ?
C25 C20 C21 C26 -178.7(2) . . . . ?
C26 C21 C22 C23 -179.0(2) . . . . ?
C27 C28 C29 C30 0.5(3) . . . . ?
C27 C28 C33 N3 177.1(2) . . . . ?
C27 C32 C45 N4 -3.0(3) . . . . ?
C28 C27 C32 C31 3.2(3) . . . . ?
C28 C27 C32 C45 179.74(19) . . . . ?
C28 C29 C30 C31 2.6(3) . . . . ?
C28 C29 C30 C34 -176.5(2) . . . . ?
C29 C28 C33 N3 -2.6(3) . . . . ?
C29 C30 C31 C32 -2.8(3) . . . . ?
C29 C30 C34 C35 49.5(3) . . . . ?
C29 C30 C34 C36 168.8(2) . . . . ?
C29 C30 C34 C37 -69.9(3) . . . . ?
C30 C31 C32 C27 -0.1(3) . . . . ?
C30 C31 C32 C45 -176.87(19) . . . . ?
C31 C30 C34 C35 -129.6(2) . . . . ?
C31 C30 C34 C36 -10.3(3) . . . . ?
C31 C30 C34 C37 111.0(2) . . . . ?
C31 C32 C45 N4 173.7(2) . . . . ?
C32 C27 C28 C29 -3.4(3) . . . . ?
C32 C27 C28 C33 176.89(19) . . . . ?
C33 N3 C38 C39 105.6(3) . . . . ?
C33 N3 C38 C43 -77.9(3) . . . . ?
C33 C28 C29 C30 -179.8(2) . . . . ?
C34 C30 C31 C32 176.35(19) . . . . ?
C38 N3 C33 C28 177.0(2) . . . . ?
C38 C39 C40 C41 -2.1(4) . . . . ?
C38 C39 C44 F7 -63.6(3) . . . . ?
C38 C39 C44 F8 176.7(3) . . . . ?
C38 C39 C44 F9 57.5(4) . . . . ?
C39 C38 C43 C42 -2.8(4) . . . . ?
C39 C40 C41 C42 -1.2(4) . . . . ?
C40 C39 C44 F7 115.0(3) . . . . ?
C40 C39 C44 F8 -4.6(4) . . . . ?
C40 C39 C44 F9 -123.9(3) . . . . ?
C40 C41 C42 C43 2.4(4) . . . . ?
C41 C42 C43 C38 -0.4(4) . . . . ?
C43 C38 C39 C40 4.0(4) . . . . ?
C43 C38 C39 C44 -177.4(2) . . . . ?
C44 C39 C40 C41 179.3(3) . . . . ?
C45 N4 C46 C47 60.7(3) . . . . ?
C45 N4 C46 C51 -120.3(2) . . . . ?
C46 N4 C45 C32 -179.65(19) . . . . ?
C46 C47 C48 C49 -1.8(4) . . . . ?
C46 C47 C52 F10 44.1(3) . . . . ?
C46 C47 C52 F11 -76.1(3) . . . . ?
C46 C47 C52 F12 164.8(2) . . . . ?
C47 C46 C51 C50 -2.8(3) . . . . ?
C47 C48 C49 C50 -1.4(4) . . . . ?
C48 C47 C52 F10 -132.8(2) . . . . ?
C48 C47 C52 F11 107.0(3) . . . . ?
C48 C47 C52 F12 -12.1(3) . . . . ?
C48 C49 C50 C51 2.6(4) . . . . ?
C49 C50 C51 C46 -0.5(4) . . . . ?
C51 C46 C47 C48 3.9(3) . . . . ?
C51 C46 C47 C52 -173.0(2) . . . . ?
C52 C47 C48 C49 175.2(2) . . . . ?
C53 C57 C58 C56 -2.1(6) . . . . ?
C54 C56 C58 C57 0.3(6) . . . . ?
C55 C53 C57 C58 2.0(7) . . . . ?
C55 C54 C56 C58 1.8(5) . . . . ?
C56 C54 C55 C53 -2.0(5) . . . . ?
C56 C54 C55 C59 176.6(4) . . . . ?
C57 C53 C55 C54 0.1(6) . . . . ?
C57 C53 C55 C59 -178.5(4) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
- B-factor correction
;
_oxdiff_exptl_absorpt_empirical_full_max 2.420
_oxdiff_exptl_absorpt_empirical_full_min 0.392
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_11
_database_code_depnum_ccdc_archive 'CCDC 2418242'
loop_
_audit_author_name
_audit_author_address
'Timothy Prior'
;University of Hull
United Kingdom
;
_audit_update_record             
;
2025-01-20 deposited with the CCDC.	2025-12-16 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         'C46 H30 F12 N4 O3 V, C2 H3 N'
_chemical_formula_sum            'C48 H33 F12 N5 O3 V'
_chemical_formula_weight         1006.73

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'
F F 0.0727 0.0534 '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                   12.19953(12)
_cell_length_b                   14.8420(2)
_cell_length_c                   26.2894(2)
_cell_angle_alpha                93.4728(9)
_cell_angle_beta                 99.0009(8)
_cell_angle_gamma                106.4579(10)
_cell_volume                     4481.12(9)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    69634
_cell_measurement_theta_min      3.12
_cell_measurement_theta_max      72.57

_exptl_crystal_description       block
_exptl_crystal_colour            'dark green'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.492
_exptl_crystal_F_000             2044
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.070
_exptl_crystal_size_min          0.040
_exptl_absorpt_coefficient_mu    2.731
_shelx_estimated_absorpt_T_min   0.735
_shelx_estimated_absorpt_T_max   0.899
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.931
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   
; 
CrysAlisPro 1.171.43.136a (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     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            142364
_diffrn_reflns_av_unetI/netI     0.0188
_diffrn_reflns_av_R_equivalents  0.0351
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_theta_min         1.712
_diffrn_reflns_theta_max         73.839
_diffrn_reflns_theta_full        67.679
_diffrn_measured_fraction_theta_max 0.937
_diffrn_measured_fraction_theta_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.937
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.937
_diffrn_reflns_point_group_measured_fraction_full 0.993
_reflns_number_total             17015
_reflns_number_gt                15992
_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 43.137a 64-bit (release 10-09-2024))'
_computing_cell_refinement       'CrysAlisPro 1.171.43.136a (Rigaku OD, 2024)'
_computing_data_reduction        'CrysAlisPro 1.171.43.136a (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)+(0.0949P)²+9.4212P] 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         17015
_refine_ls_number_parameters     1249
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0717
_refine_ls_R_factor_gt           0.0690
_refine_ls_wR_factor_ref         0.2021
_refine_ls_wR_factor_gt          0.2003
_refine_ls_goodness_of_fit_ref   1.173
_refine_ls_restrained_S_all      1.173
_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 0.90096(5) 0.62188(4) 0.54338(2) 0.02162(15) Uani 1 1 d . . . . .
O1 O 0.9659(2) 0.72309(17) 0.50482(9) 0.0258(5) Uani 1 1 d . . . . .
O2 O 0.8803(2) 0.62121(18) 0.61412(9) 0.0263(5) Uani 1 1 d . . . . .
O3 O 0.8567(2) 0.51977(18) 0.51121(10) 0.0286(5) Uani 1 1 d . . . . .
N1 N 1.0732(2) 0.6201(2) 0.56980(11) 0.0227(6) Uani 1 1 d . . . . .
N3 N 0.7432(2) 0.6551(2) 0.52701(11) 0.0235(6) Uani 1 1 d . . . . .
C1 C 1.0688(3) 0.7578(2) 0.49259(13) 0.0225(7) Uani 1 1 d . . . . .
C2 C 1.1664(3) 0.7269(2) 0.51191(13) 0.0229(7) Uani 1 1 d . . . . .
C3 C 1.2746(3) 0.7666(3) 0.49820(13) 0.0257(7) Uani 1 1 d . . . . .
H3 H 1.338097 0.744791 0.511785 0.031 Uiso 1 1 calc R U . . .
C4 C 1.2918(3) 0.8372(3) 0.46513(14) 0.0274(7) Uani 1 1 d . . . . .
C5 C 1.1963(3) 0.8667(3) 0.44624(13) 0.0257(7) Uani 1 1 d . . . . .
H5 H 1.206048 0.915029 0.423744 0.031 Uiso 1 1 calc R U . . .
C6 C 1.0874(3) 0.8290(2) 0.45871(12) 0.0226(7) Uani 1 1 d . . . . .
C7 C 1.1608(3) 0.6577(2) 0.54867(13) 0.0233(7) Uani 1 1 d . . . . .
H7 H 1.228406 0.638329 0.558048 0.028 Uiso 1 1 calc R U . . .
C8 C 1.4089(3) 0.8810(3) 0.45108(16) 0.0350(8) Uani 1 1 d . . . . .
H8A H 1.448658 0.940048 0.473605 0.053 Uiso 1 1 calc R U . . .
H8B H 1.398612 0.894319 0.414868 0.053 Uiso 1 1 calc R U . . .
H8C H 1.455537 0.837142 0.455612 0.053 Uiso 1 1 calc R U . . .
C9 C 0.9905(3) 0.8647(2) 0.43803(13) 0.0238(7) Uani 1 1 d . . . . .
H9 H 0.923183 0.851367 0.453538 0.029 Uiso 1 1 calc R U . . .
N2 N 0.9954(3) 0.9134(2) 0.39963(11) 0.0279(6) Uani 1 1 d . . . . .
C10 C 0.9022(3) 0.9508(3) 0.38532(14) 0.0266(7) Uani 1 1 d . . . . .
C11 C 0.8372(3) 0.9286(3) 0.33454(14) 0.0272(7) Uani 1 1 d . . . . .
C12 C 0.7448(3) 0.9645(3) 0.32103(15) 0.0315(8) Uani 1 1 d . . . . .
H12 H 0.698916 0.947346 0.287255 0.038 Uiso 1 1 calc R U . . .
C13 C 0.7184(3) 1.0248(3) 0.35584(15) 0.0326(8) Uani 1 1 d . . . . .
H13 H 0.654818 1.048982 0.346105 0.039 Uiso 1 1 calc R U . . .
C14 C 0.7849(4) 1.0499(3) 0.40503(16) 0.0338(8) Uani 1 1 d . . . . .
H14 H 0.768425 1.092852 0.428838 0.041 Uiso 1 1 calc R U . . .
C15 C 0.8758(3) 1.0122(3) 0.41972(14) 0.0309(8) Uani 1 1 d . . . . .
H15 H 0.920216 1.028886 0.453789 0.037 Uiso 1 1 calc R U . . .
C16 C 0.8661(4) 0.8663(3) 0.29587(14) 0.0326(8) Uani 1 1 d . . . . .
F1 F 0.8660(3) 0.78159(17) 0.31163(10) 0.0480(6) Uani 1 1 d . . . . .
F2 F 0.7924(2) 0.8480(2) 0.25036(9) 0.0472(6) Uani 1 1 d . . . . .
F3 F 0.9723(2) 0.90359(19) 0.28396(9) 0.0437(6) Uani 1 1 d . . . . .
C17 C 1.0920(3) 0.5570(2) 0.60806(13) 0.0235(7) Uani 1 1 d . . . . .
C18 C 1.1661(3) 0.5915(2) 0.65600(13) 0.0241(7) Uani 1 1 d . . . . .
C19 C 1.1823(3) 0.5270(3) 0.69089(13) 0.0263(7) Uani 1 1 d . . . . .
H19 H 1.231434 0.549434 0.723657 0.032 Uiso 1 1 calc R U . . .
C20 C 1.1283(3) 0.4316(3) 0.67855(14) 0.0285(7) Uani 1 1 d . . . . .
H20 H 1.141618 0.388597 0.702405 0.034 Uiso 1 1 calc R U . . .
C21 C 1.0539(3) 0.3980(3) 0.63099(14) 0.0292(8) Uani 1 1 d . . . . .
H21 H 1.016289 0.332181 0.622354 0.035 Uiso 1 1 calc R U . . .
C22 C 1.0355(3) 0.4617(3) 0.59636(14) 0.0268(7) Uani 1 1 d . . . . .
H22 H 0.983421 0.439244 0.564324 0.032 Uiso 1 1 calc R U . . .
C23 C 1.2246(3) 0.6945(3) 0.67143(14) 0.0295(8) Uani 1 1 d . . . . .
F4 F 1.1509(2) 0.74680(16) 0.66483(10) 0.0419(6) Uani 1 1 d . . . . .
F5 F 1.3100(2) 0.73213(17) 0.64531(9) 0.0402(5) Uani 1 1 d . . . . .
F6 F 1.2757(2) 0.71274(16) 0.72153(8) 0.0384(5) Uani 1 1 d . . . . .
C24 C 0.7898(3) 0.6164(2) 0.63651(13) 0.0240(7) Uani 1 1 d . . . . .
C25 C 0.6821(3) 0.6221(2) 0.60955(13) 0.0241(7) Uani 1 1 d . . . . .
C26 C 0.5875(3) 0.6134(3) 0.63572(14) 0.0278(7) Uani 1 1 d . . . . .
H26 H 0.515597 0.616122 0.616946 0.033 Uiso 1 1 calc R U . . .
C27 C 0.5961(3) 0.6011(2) 0.68754(14) 0.0267(7) Uani 1 1 d . . . . .
C28 C 0.7028(3) 0.5959(2) 0.71387(14) 0.0264(7) Uani 1 1 d . . . . .
H28 H 0.710645 0.587890 0.749698 0.032 Uiso 1 1 calc R U . . .
C29 C 0.7977(3) 0.6021(2) 0.68952(13) 0.0247(7) Uani 1 1 d . . . . .
C30 C 0.6654(3) 0.6408(2) 0.55655(13) 0.0253(7) Uani 1 1 d . . . . .
H30 H 0.590253 0.642927 0.541568 0.030 Uiso 1 1 calc R U . . .
C31 C 0.4969(3) 0.5948(3) 0.71588(16) 0.0337(8) Uani 1 1 d . . . . .
H31A H 0.432262 0.606452 0.692802 0.051 Uiso 1 1 calc R U . . .
H31B H 0.522392 0.642285 0.746253 0.051 Uiso 1 1 calc R U . . .
H31C H 0.471385 0.531624 0.727095 0.051 Uiso 1 1 calc R U . . .
C32 C 0.9062(3) 0.5915(2) 0.71844(13) 0.0262(7) Uani 1 1 d . . . . .
H32 H 0.976667 0.614932 0.705886 0.031 Uiso 1 1 calc R U . . .
N4 N 0.9071(3) 0.5518(2) 0.75983(11) 0.0290(6) Uani 1 1 d . . . . .
C33 C 1.0154(3) 0.5472(3) 0.78549(13) 0.0275(7) Uani 1 1 d . . . . .
C34 C 1.0310(4) 0.4589(3) 0.79500(14) 0.0309(8) Uani 1 1 d . . . . .
C35 C 1.1394(4) 0.4551(3) 0.81946(14) 0.0341(8) Uani 1 1 d . . . . .
H35 H 1.150885 0.395440 0.824863 0.041 Uiso 1 1 calc R U . . .
C36 C 1.2300(4) 0.5363(3) 0.83590(14) 0.0343(8) Uani 1 1 d . . . . .
H36 H 1.303095 0.532592 0.852744 0.041 Uiso 1 1 calc R U . . .
C37 C 1.2143(4) 0.6237(3) 0.82783(15) 0.0362(9) Uani 1 1 d . . . . .
H37 H 1.276390 0.679960 0.839391 0.043 Uiso 1 1 calc R U . . .
C38 C 1.1072(3) 0.6284(3) 0.80270(14) 0.0313(8) Uani 1 1 d . . . . .
H38 H 1.096747 0.688369 0.797239 0.038 Uiso 1 1 calc R U . . .
C39 C 0.9341(4) 0.3713(3) 0.77755(17) 0.0377(9) Uani 1 1 d . . . . .
F7 F 0.8892(2) 0.36237(18) 0.72657(10) 0.0483(6) Uani 1 1 d . . . . .
F8 F 0.8452(2) 0.36352(19) 0.80254(11) 0.0503(6) Uani 1 1 d . . . . .
F9 F 0.9668(3) 0.29277(18) 0.78490(13) 0.0599(8) Uani 1 1 d . . . . .
C40 C 0.7075(3) 0.6797(3) 0.47643(13) 0.0242(7) Uani 1 1 d . . . . .
C41 C 0.6904(3) 0.7680(3) 0.46937(13) 0.0252(7) Uani 1 1 d . . . . .
C42 C 0.6546(3) 0.7886(3) 0.41925(14) 0.0282(7) Uani 1 1 d . . . . .
H42 H 0.642885 0.848243 0.414138 0.034 Uiso 1 1 calc R U . . .
C43 C 0.6364(3) 0.7223(3) 0.37749(14) 0.0324(8) Uani 1 1 d . . . . .
H43 H 0.611110 0.736357 0.343654 0.039 Uiso 1 1 calc R U . . .
C44 C 0.6544(3) 0.6356(3) 0.38414(14) 0.0323(8) Uani 1 1 d . . . . .
H44 H 0.641426 0.590333 0.355021 0.039 Uiso 1 1 calc R U . . .
C45 C 0.6916(3) 0.6149(3) 0.43382(14) 0.0310(8) Uani 1 1 d . . . . .
H45 H 0.706114 0.556029 0.438383 0.037 Uiso 1 1 calc R U . . .
C46 C 0.7118(3) 0.8416(3) 0.51421(14) 0.0288(7) Uani 1 1 d . . . . .
F10 F 0.6312(2) 0.82014(17) 0.54494(9) 0.0377(5) Uani 1 1 d . . . . .
F11 F 0.8151(2) 0.85609(17) 0.54510(9) 0.0400(5) Uani 1 1 d . . . . .
F12 F 0.7094(2) 0.92586(15) 0.49895(9) 0.0371(5) Uani 1 1 d . . . . .
V2 V 0.60087(5) 0.87602(4) 0.95979(2) 0.02202(15) Uani 1 1 d . . . . .
O4 O 0.5352(2) 0.88191(18) 0.88911(9) 0.0258(5) Uani 1 1 d . . . . .
O5 O 0.6231(2) 0.77205(17) 0.99541(9) 0.0261(5) Uani 1 1 d . . . . .
O6 O 0.6443(2) 0.97493(18) 0.99534(10) 0.0294(5) Uani 1 1 d . . . . .
N5 N 0.4287(2) 0.8358(2) 0.97413(11) 0.0232(6) Uani 1 1 d . . . . .
N7 N 0.7583(3) 0.8848(2) 0.93412(11) 0.0246(6) Uani 1 1 d . . . . .
C47 C 0.4325(3) 0.8835(2) 0.86599(13) 0.0223(7) Uani 1 1 d . . . . .
C48 C 0.3354(3) 0.8701(2) 0.89150(13) 0.0229(7) Uani 1 1 d . . . . .
C49 C 0.2280(3) 0.8722(2) 0.86486(14) 0.0273(7) Uani 1 1 d . . . . .
H49 H 0.164610 0.863131 0.882856 0.033 Uiso 1 1 calc R U . . .
C50 C 0.2105(3) 0.8871(2) 0.81314(14) 0.0264(7) Uani 1 1 d . . . . .
C51 C 0.3060(3) 0.8999(2) 0.78837(13) 0.0249(7) Uani 1 1 d . . . . .
H51 H 0.296152 0.909676 0.752763 0.030 Uiso 1 1 calc R U . . .
C52 C 0.4144(3) 0.8992(2) 0.81322(13) 0.0241(7) Uani 1 1 d . . . . .
C53 C 0.3406(3) 0.8484(2) 0.94464(13) 0.0235(7) Uani 1 1 d . . . . .
H53 H 0.272668 0.842960 0.959119 0.028 Uiso 1 1 calc R U . . .
C54 C 0.0938(3) 0.8876(3) 0.78415(15) 0.0330(8) Uani 1 1 d . . . . .
H54A H 0.058547 0.828783 0.760942 0.050 Uiso 1 1 calc R U . . .
H54B H 0.104015 0.941563 0.763759 0.050 Uiso 1 1 calc R U . . .
H54C H 0.043078 0.892828 0.808922 0.050 Uiso 1 1 calc R U . . .
C55 C 0.5111(3) 0.9116(2) 0.78445(13) 0.0256(7) Uani 1 1 d . . . . .
H55 H 0.578143 0.894868 0.798671 0.031 Uiso 1 1 calc R U . . .
N6 N 0.5062(3) 0.9444(2) 0.74095(12) 0.0294(7) Uani 1 1 d . . . . .
C56 C 0.5992(3) 0.9475(3) 0.71464(13) 0.0286(7) Uani 1 1 d . . . . .
C57 C 0.6638(3) 1.0337(3) 0.70033(13) 0.0292(8) Uani 1 1 d . . . . .
C58 C 0.7568(3) 1.0368(3) 0.67576(14) 0.0342(8) Uani 1 1 d . . . . .
H58 H 0.802283 1.095603 0.667582 0.041 Uiso 1 1 calc R U . . .
C59 C 0.7843(4) 0.9547(3) 0.66290(15) 0.0373(9) Uani 1 1 d . . . . .
H59 H 0.848504 0.957277 0.646126 0.045 Uiso 1 1 calc R U . . .
C60 C 0.7178(4) 0.8695(3) 0.67469(15) 0.0370(9) Uani 1 1 d . . . . .
H60 H 0.734668 0.812883 0.664967 0.044 Uiso 1 1 calc R U . . .
C61 C 0.6262(3) 0.8658(3) 0.70065(14) 0.0323(8) Uani 1 1 d . . . . .
H61 H 0.581580 0.806732 0.708941 0.039 Uiso 1 1 calc R U . . .
C62 C 0.6339(4) 1.1225(3) 0.71249(15) 0.0345(8) Uani 1 1 d . . . . .
F13 F 0.5275(2) 1.12008(18) 0.68839(10) 0.0463(6) Uani 1 1 d . . . . .
F14 F 0.7068(2) 1.19829(17) 0.69838(11) 0.0492(6) Uani 1 1 d . . . . .
F15 F 0.6362(3) 1.14211(18) 0.76345(9) 0.0499(7) Uani 1 1 d . . . . .
C63 C 0.4101(3) 0.8097(2) 1.02476(13) 0.0236(7) Uani 1 1 d . . . . .
C64 C 0.3384(3) 0.7204(2) 1.03152(13) 0.0248(7) Uani 1 1 d . . . . .
C65 C 0.3211(3) 0.6994(3) 1.08099(14) 0.0263(7) Uani 1 1 d . . . . .
H65 H 0.273380 0.638813 1.085708 0.032 Uiso 1 1 calc R U . . .
C66 C 0.3726(3) 0.7660(3) 1.12338(14) 0.0294(8) Uani 1 1 d . . . . .
H66 H 0.358811 0.751608 1.156971 0.035 Uiso 1 1 calc R U . . .
C67 C 0.4448(3) 0.8542(3) 1.11678(14) 0.0294(8) Uani 1 1 d . . . . .
H67 H 0.480938 0.899784 1.145947 0.035 Uiso 1 1 calc R U . . .
C68 C 0.4639(3) 0.8755(3) 1.06750(14) 0.0273(7) Uani 1 1 d . . . . .
H68 H 0.513932 0.935367 1.063133 0.033 Uiso 1 1 calc R U . . .
C69 C 0.2822(3) 0.6457(3) 0.98651(14) 0.0288(7) Uani 1 1 d . . . . .
F16 F 0.3575(2) 0.63276(17) 0.95670(9) 0.0399(5) Uani 1 1 d . . . . .
F17 F 0.1966(2) 0.66517(16) 0.95446(8) 0.0375(5) Uani 1 1 d . . . . .
F18 F 0.2335(2) 0.56154(16) 1.00162(9) 0.0383(5) Uani 1 1 d . . . . .
C70 C 0.7145(3) 0.7423(2) 1.00894(13) 0.0244(7) Uani 1 1 d . . . . .
C71 C 0.8218(3) 0.7801(3) 0.99238(13) 0.0250(7) Uani 1 1 d . . . . .
C72 C 0.9170(3) 0.7470(3) 1.00913(14) 0.0284(7) Uani 1 1 d . . . . .
H72 H 0.988806 0.774829 0.998505 0.034 Uiso 1 1 calc R U . . .
C73 C 0.9090(3) 0.6747(3) 1.04077(14) 0.0282(7) Uani 1 1 d . . . . .
C74 C 0.8034(3) 0.6380(3) 1.05700(13) 0.0264(7) Uani 1 1 d . . . . .
H74 H 0.796251 0.588768 1.078838 0.032 Uiso 1 1 calc R U . . .
C75 C 0.7075(3) 0.6707(2) 1.04250(13) 0.0240(7) Uani 1 1 d . . . . .
C76 C 0.8373(3) 0.8499(3) 0.95654(14) 0.0264(7) Uani 1 1 d . . . . .
H76 H 0.912838 0.872895 0.948417 0.032 Uiso 1 1 calc R U . . .
C77 C 1.0086(4) 0.6357(3) 1.05632(17) 0.0385(9) Uani 1 1 d . . . . .
H77A H 0.992297 0.573225 1.037217 0.058 Uiso 1 1 calc R U . . .
H77B H 1.018795 0.630223 1.093608 0.058 Uiso 1 1 calc R U . . .
H77C H 1.079797 0.678306 1.048303 0.058 Uiso 1 1 calc R U . . .
C78 C 0.5993(3) 0.6312(2) 1.06176(13) 0.0243(7) Uani 1 1 d . . . . .
H78 H 0.528647 0.637273 1.043449 0.029 Uiso 1 1 calc R U . . .
N8 N 0.5981(3) 0.5889(2) 1.10262(11) 0.0284(6) Uani 1 1 d . . . . .
C79 C 0.4883(3) 0.5494(3) 1.11650(13) 0.0266(7) Uani 1 1 d . . . . .
C80 C 0.4692(3) 0.5783(3) 1.16521(14) 0.0303(8) Uani 1 1 d . . . . .
C81 C 0.3602(4) 0.5404(3) 1.17864(15) 0.0332(8) Uani 1 1 d . . . . .
H81 H 0.345664 0.561358 1.211098 0.040 Uiso 1 1 calc R U . . .
C82 C 0.2741(4) 0.4732(3) 1.14513(15) 0.0344(8) Uani 1 1 d . . . . .
H82 H 0.200526 0.447716 1.154691 0.041 Uiso 1 1 calc R U . . .
C83 C 0.2935(4) 0.4421(3) 1.09761(15) 0.0347(8) Uani 1 1 d . . . . .
H83 H 0.233838 0.395009 1.074798 0.042 Uiso 1 1 calc R U . . .
C84 C 0.4009(4) 0.4805(3) 1.08348(14) 0.0319(8) Uani 1 1 d . . . . .
H84 H 0.414585 0.459223 1.050903 0.038 Uiso 1 1 calc R U . . .
C85 C 0.5625(4) 0.6500(3) 1.20189(15) 0.0361(9) Uani 1 1 d . . . . .
F19 F 0.5256(2) 0.6761(2) 1.24439(10) 0.0549(7) Uani 1 1 d . . . . .
F20 F 0.6531(2) 0.61917(19) 1.21943(10) 0.0462(6) Uani 1 1 d . . . . .
F21 F 0.6065(2) 0.73047(17) 1.18123(9) 0.0436(6) Uani 1 1 d . . . . .
C86 C 0.7930(3) 0.9469(2) 0.89606(13) 0.0247(7) Uani 1 1 d . . . . .
C87 C 0.8109(3) 0.9126(3) 0.84800(14) 0.0266(7) Uani 1 1 d . . . . .
C88 C 0.8463(3) 0.9762(3) 0.81241(14) 0.0289(7) Uani 1 1 d . . . . .
H88 H 0.858390 0.953473 0.779814 0.035 Uiso 1 1 calc R U . . .
C89 C 0.8637(3) 1.0713(3) 0.82423(15) 0.0315(8) Uani 1 1 d . . . . .
H89 H 0.888911 1.113973 0.799962 0.038 Uiso 1 1 calc R U . . .
C90 C 0.8447(3) 1.1055(3) 0.87139(16) 0.0336(8) Uani 1 1 d . . . . .
H90 H 0.856561 1.171201 0.879316 0.040 Uiso 1 1 calc R U . . .
C91 C 0.8082(3) 1.0431(3) 0.90691(15) 0.0308(8) Uani 1 1 d . . . . .
H91 H 0.793589 1.066272 0.938863 0.037 Uiso 1 1 calc R U . . .
C92 C 0.7895(3) 0.8095(3) 0.83351(14) 0.0304(8) Uani 1 1 d . . . . .
F22 F 0.7935(2) 0.78933(16) 0.78363(8) 0.0391(5) Uani 1 1 d . . . . .
F23 F 0.6865(2) 0.75651(16) 0.84158(10) 0.0409(5) Uani 1 1 d . . . . .
F24 F 0.8698(2) 0.77464(17) 0.86039(9) 0.0392(5) Uani 1 1 d . . . . .
N9 N 0.4136(3) 0.6027(3) 0.47198(17) 0.0489(9) Uani 1 1 d . . . . .
C93 C 0.3656(4) 0.6114(3) 0.4329(2) 0.0427(10) Uani 1 1 d . . . . .
C94 C 0.3038(5) 0.6237(4) 0.3828(2) 0.0582(14) Uani 1 1 d . . . . .
H94A H 0.219931 0.596875 0.381174 0.087 Uiso 1 1 calc R U . . .
H94B H 0.328121 0.591251 0.355022 0.087 Uiso 1 1 calc R U . . .
H94C H 0.321865 0.691211 0.378684 0.087 Uiso 1 1 calc R U . . .
N10 N 1.0875(3) 0.9948(3) 0.93229(16) 0.0493(9) Uani 1 1 d . . . . .
C95 C 1.1360(4) 1.0479(3) 0.90811(17) 0.0407(10) Uani 1 1 d . . . . .
C96 C 1.1994(6) 1.1149(4) 0.8773(2) 0.0615(15) Uani 1 1 d . . . . .
H96A H 1.282815 1.131834 0.891298 0.092 Uiso 1 1 calc R U . . .
H96B H 1.173917 1.171810 0.878505 0.092 Uiso 1 1 calc R U . . .
H96C H 1.184373 1.086283 0.841375 0.092 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 1.594(3) . ?
V1 O2 1.916(2) . ?
V1 O1 1.916(2) . ?
V1 N3 2.106(3) . ?
V1 N1 2.116(3) . ?
O1 C1 1.313(4) . ?
O2 C24 1.317(4) . ?
N1 C7 1.284(5) . ?
N1 C17 1.450(4) . ?
N3 C30 1.298(5) . ?
N3 C40 1.435(4) . ?
C1 C6 1.415(5) . ?
C1 C2 1.426(5) . ?
C2 C3 1.397(5) . ?
C2 C7 1.447(5) . ?
C3 C4 1.394(5) . ?
C3 H3 0.9500 . ?
C4 C5 1.389(5) . ?
C4 C8 1.505(5) . ?
C5 C6 1.387(5) . ?
C5 H5 0.9500 . ?
C6 C9 1.471(5) . ?
C7 H7 0.9500 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 N2 1.275(4) . ?
C9 H9 0.9500 . ?
N2 C10 1.412(5) . ?
C10 C15 1.382(5) . ?
C10 C11 1.410(5) . ?
C11 C12 1.386(5) . ?
C11 C16 1.482(5) . ?
C12 C13 1.377(6) . ?
C12 H12 0.9500 . ?
C13 C14 1.382(5) . ?
C13 H13 0.9500 . ?
C14 C15 1.391(5) . ?
C14 H14 0.9500 . ?
C15 H15 0.9500 . ?
C16 F2 1.341(4) . ?
C16 F1 1.347(5) . ?
C16 F3 1.351(5) . ?
C17 C22 1.379(5) . ?
C17 C18 1.404(5) . ?
C18 C19 1.398(5) . ?
C18 C23 1.493(5) . ?
C19 C20 1.376(5) . ?
C19 H19 0.9500 . ?
C20 C21 1.396(5) . ?
C20 H20 0.9500 . ?
C21 C22 1.391(5) . ?
C21 H21 0.9500 . ?
C22 H22 0.9500 . ?
C23 F6 1.342(4) . ?
C23 F4 1.342(4) . ?
C23 F5 1.346(4) . ?
C24 C29 1.415(5) . ?
C24 C25 1.420(5) . ?
C25 C26 1.413(5) . ?
C25 C30 1.432(5) . ?
C26 C27 1.377(5) . ?
C26 H26 0.9500 . ?
C27 C28 1.399(5) . ?
C27 C31 1.502(5) . ?
C28 C29 1.392(5) . ?
C28 H28 0.9500 . ?
C29 C32 1.473(5) . ?
C30 H30 0.9500 . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C32 N4 1.269(5) . ?
C32 H32 0.9500 . ?
N4 C33 1.409(5) . ?
C33 C38 1.386(5) . ?
C33 C34 1.407(5) . ?
C34 C35 1.395(6) . ?
C34 C39 1.479(6) . ?
C35 C36 1.376(6) . ?
C35 H35 0.9500 . ?
C36 C37 1.386(6) . ?
C36 H36 0.9500 . ?
C37 C38 1.392(6) . ?
C37 H37 0.9500 . ?
C38 H38 0.9500 . ?
C39 F8 1.335(5) . ?
C39 F7 1.349(5) . ?
C39 F9 1.350(5) . ?
C40 C45 1.384(5) . ?
C40 C41 1.403(5) . ?
C41 C42 1.402(5) . ?
C41 C46 1.496(5) . ?
C42 C43 1.375(6) . ?
C42 H42 0.9500 . ?
C43 C44 1.382(6) . ?
C43 H43 0.9500 . ?
C44 C45 1.396(5) . ?
C44 H44 0.9500 . ?
C45 H45 0.9500 . ?
C46 F11 1.341(4) . ?
C46 F12 1.343(4) . ?
C46 F10 1.350(4) . ?
V2 O6 1.596(3) . ?
V2 O5 1.914(2) . ?
V2 O4 1.922(2) . ?
V2 N7 2.106(3) . ?
V2 N5 2.116(3) . ?
O4 C47 1.311(4) . ?
O5 C70 1.319(4) . ?
N5 C53 1.289(4) . ?
N5 C63 1.442(4) . ?
N7 C76 1.299(5) . ?
N7 C86 1.433(4) . ?
C47 C52 1.414(5) . ?
C47 C48 1.423(5) . ?
C48 C49 1.396(5) . ?
C48 C53 1.448(5) . ?
C49 C50 1.384(5) . ?
C49 H49 0.9500 . ?
C50 C51 1.394(5) . ?
C50 C54 1.508(5) . ?
C51 C52 1.384(5) . ?
C51 H51 0.9500 . ?
C52 C55 1.473(5) . ?
C53 H53 0.9500 . ?
C54 H54A 0.9800 . ?
C54 H54B 0.9800 . ?
C54 H54C 0.9800 . ?
C55 N6 1.269(5) . ?
C55 H55 0.9500 . ?
N6 C56 1.410(5) . ?
C56 C61 1.387(6) . ?
C56 C57 1.407(5) . ?
C57 C58 1.382(6) . ?
C57 C62 1.493(6) . ?
C58 C59 1.389(6) . ?
C58 H58 0.9500 . ?
C59 C60 1.378(6) . ?
C59 H59 0.9500 . ?
C60 C61 1.387(6) . ?
C60 H60 0.9500 . ?
C61 H61 0.9500 . ?
C62 F14 1.335(4) . ?
C62 F13 1.341(5) . ?
C62 F15 1.348(5) . ?
C63 C68 1.385(5) . ?
C63 C64 1.406(5) . ?
C64 C65 1.389(5) . ?
C64 C69 1.502(5) . ?
C65 C66 1.381(5) . ?
C65 H65 0.9500 . ?
C66 C67 1.394(5) . ?
C66 H66 0.9500 . ?
C67 C68 1.391(5) . ?
C67 H67 0.9500 . ?
C68 H68 0.9500 . ?
C69 F18 1.335(4) . ?
C69 F16 1.342(4) . ?
C69 F17 1.345(4) . ?
C70 C75 1.414(5) . ?
C70 C71 1.418(5) . ?
C71 C72 1.405(5) . ?
C71 C76 1.435(5) . ?
C72 C73 1.388(5) . ?
C72 H72 0.9500 . ?
C73 C74 1.394(5) . ?
C73 C77 1.500(5) . ?
C74 C75 1.398(5) . ?
C74 H74 0.9500 . ?
C75 C78 1.465(5) . ?
C76 H76 0.9500 . ?
C77 H77A 0.9800 . ?
C77 H77B 0.9800 . ?
C77 H77C 0.9800 . ?
C78 N8 1.277(4) . ?
C78 H78 0.9500 . ?
N8 C79 1.416(5) . ?
C79 C84 1.386(5) . ?
C79 C80 1.400(5) . ?
C80 C81 1.398(6) . ?
C80 C85 1.485(6) . ?
C81 C82 1.373(6) . ?
C81 H81 0.9500 . ?
C82 C83 1.383(6) . ?
C82 H82 0.9500 . ?
C83 C84 1.392(6) . ?
C83 H83 0.9500 . ?
C84 H84 0.9500 . ?
C85 F20 1.339(5) . ?
C85 F19 1.344(5) . ?
C85 F21 1.348(5) . ?
C86 C91 1.392(5) . ?
C86 C87 1.405(5) . ?
C87 C88 1.398(5) . ?
C87 C92 1.492(5) . ?
C88 C89 1.376(5) . ?
C88 H88 0.9500 . ?
C89 C90 1.389(6) . ?
C89 H89 0.9500 . ?
C90 C91 1.388(5) . ?
C90 H90 0.9500 . ?
C91 H91 0.9500 . ?
C92 F23 1.337(4) . ?
C92 F22 1.339(4) . ?
C92 F24 1.358(4) . ?
N9 C93 1.133(6) . ?
C93 C94 1.460(7) . ?
C94 H94A 0.9800 . ?
C94 H94B 0.9800 . ?
C94 H94C 0.9800 . ?
N10 C95 1.136(6) . ?
C95 C96 1.448(7) . ?
C96 H96A 0.9800 . ?
C96 H96B 0.9800 . ?
C96 H96C 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 113.89(12) . . ?
O3 V1 O1 114.65(12) . . ?
O2 V1 O1 131.46(11) . . ?
O3 V1 N3 96.82(12) . . ?
O2 V1 N3 87.21(11) . . ?
O1 V1 N3 87.47(11) . . ?
O3 V1 N1 96.56(12) . . ?
O2 V1 N1 87.37(11) . . ?
O1 V1 N1 86.97(11) . . ?
N3 V1 N1 166.61(12) . . ?
C1 O1 V1 133.9(2) . . ?
C24 O2 V1 132.9(2) . . ?
C7 N1 C17 115.6(3) . . ?
C7 N1 V1 125.1(2) . . ?
C17 N1 V1 118.2(2) . . ?
C30 N3 C40 115.6(3) . . ?
C30 N3 V1 124.4(2) . . ?
C40 N3 V1 119.1(2) . . ?
O1 C1 C6 120.4(3) . . ?
O1 C1 C2 123.0(3) . . ?
C6 C1 C2 116.5(3) . . ?
C3 C2 C1 121.0(3) . . ?
C3 C2 C7 116.6(3) . . ?
C1 C2 C7 122.3(3) . . ?
C4 C3 C2 121.8(3) . . ?
C4 C3 H3 119.1 . . ?
C2 C3 H3 119.1 . . ?
C5 C4 C3 117.0(3) . . ?
C5 C4 C8 121.3(3) . . ?
C3 C4 C8 121.7(3) . . ?
C6 C5 C4 123.0(3) . . ?
C6 C5 H5 118.5 . . ?
C4 C5 H5 118.5 . . ?
C5 C6 C1 120.7(3) . . ?
C5 C6 C9 120.2(3) . . ?
C1 C6 C9 119.1(3) . . ?
N1 C7 C2 126.1(3) . . ?
N1 C7 H7 116.9 . . ?
C2 C7 H7 116.9 . . ?
C4 C8 H8A 109.5 . . ?
C4 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C4 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N2 C9 C6 121.1(3) . . ?
N2 C9 H9 119.5 . . ?
C6 C9 H9 119.5 . . ?
C9 N2 C10 116.7(3) . . ?
C15 C10 C11 118.9(3) . . ?
C15 C10 N2 121.2(3) . . ?
C11 C10 N2 119.9(3) . . ?
C12 C11 C10 119.6(3) . . ?
C12 C11 C16 120.0(3) . . ?
C10 C11 C16 120.5(3) . . ?
C13 C12 C11 121.0(3) . . ?
C13 C12 H12 119.5 . . ?
C11 C12 H12 119.5 . . ?
C12 C13 C14 119.7(4) . . ?
C12 C13 H13 120.2 . . ?
C14 C13 H13 120.2 . . ?
C13 C14 C15 120.1(4) . . ?
C13 C14 H14 120.0 . . ?
C15 C14 H14 120.0 . . ?
C10 C15 C14 120.8(3) . . ?
C10 C15 H15 119.6 . . ?
C14 C15 H15 119.6 . . ?
F2 C16 F1 106.1(3) . . ?
F2 C16 F3 104.9(3) . . ?
F1 C16 F3 105.5(3) . . ?
F2 C16 C11 113.1(3) . . ?
F1 C16 C11 113.3(3) . . ?
F3 C16 C11 113.2(3) . . ?
C22 C17 C18 120.3(3) . . ?
C22 C17 N1 118.5(3) . . ?
C18 C17 N1 121.2(3) . . ?
C19 C18 C17 118.5(3) . . ?
C19 C18 C23 119.2(3) . . ?
C17 C18 C23 122.2(3) . . ?
C20 C19 C18 121.1(3) . . ?
C20 C19 H19 119.5 . . ?
C18 C19 H19 119.5 . . ?
C19 C20 C21 120.0(3) . . ?
C19 C20 H20 120.0 . . ?
C21 C20 H20 120.0 . . ?
C22 C21 C20 119.4(3) . . ?
C22 C21 H21 120.3 . . ?
C20 C21 H21 120.3 . . ?
C17 C22 C21 120.7(3) . . ?
C17 C22 H22 119.7 . . ?
C21 C22 H22 119.7 . . ?
F6 C23 F4 106.3(3) . . ?
F6 C23 F5 104.8(3) . . ?
F4 C23 F5 106.1(3) . . ?
F6 C23 C18 112.1(3) . . ?
F4 C23 C18 112.9(3) . . ?
F5 C23 C18 113.9(3) . . ?
O2 C24 C29 119.3(3) . . ?
O2 C24 C25 123.1(3) . . ?
C29 C24 C25 117.6(3) . . ?
C26 C25 C24 120.0(3) . . ?
C26 C25 C30 117.3(3) . . ?
C24 C25 C30 122.6(3) . . ?
C27 C26 C25 122.2(3) . . ?
C27 C26 H26 118.9 . . ?
C25 C26 H26 118.9 . . ?
C26 C27 C28 117.5(3) . . ?
C26 C27 C31 122.4(3) . . ?
C28 C27 C31 120.2(3) . . ?
C29 C28 C27 122.5(3) . . ?
C29 C28 H28 118.8 . . ?
C27 C28 H28 118.8 . . ?
C28 C29 C24 120.2(3) . . ?
C28 C29 C32 120.2(3) . . ?
C24 C29 C32 119.5(3) . . ?
N3 C30 C25 126.3(3) . . ?
N3 C30 H30 116.9 . . ?
C25 C30 H30 116.9 . . ?
C27 C31 H31A 109.5 . . ?
C27 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C27 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
N4 C32 C29 121.2(3) . . ?
N4 C32 H32 119.4 . . ?
C29 C32 H32 119.4 . . ?
C32 N4 C33 117.0(3) . . ?
C38 C33 C34 118.9(3) . . ?
C38 C33 N4 121.3(3) . . ?
C34 C33 N4 119.8(3) . . ?
C35 C34 C33 119.3(4) . . ?
C35 C34 C39 120.7(3) . . ?
C33 C34 C39 119.9(4) . . ?
C36 C35 C34 121.0(4) . . ?
C36 C35 H35 119.5 . . ?
C34 C35 H35 119.5 . . ?
C35 C36 C37 119.9(4) . . ?
C35 C36 H36 120.0 . . ?
C37 C36 H36 120.0 . . ?
C36 C37 C38 119.6(4) . . ?
C36 C37 H37 120.2 . . ?
C38 C37 H37 120.2 . . ?
C33 C38 C37 121.2(4) . . ?
C33 C38 H38 119.4 . . ?
C37 C38 H38 119.4 . . ?
F8 C39 F7 106.3(3) . . ?
F8 C39 F9 105.4(3) . . ?
F7 C39 F9 105.3(4) . . ?
F8 C39 C34 113.4(4) . . ?
F7 C39 C34 113.4(3) . . ?
F9 C39 C34 112.3(4) . . ?
C45 C40 C41 119.7(3) . . ?
C45 C40 N3 118.7(3) . . ?
C41 C40 N3 121.6(3) . . ?
C42 C41 C40 119.5(3) . . ?
C42 C41 C46 119.2(3) . . ?
C40 C41 C46 121.3(3) . . ?
C43 C42 C41 120.0(3) . . ?
C43 C42 H42 120.0 . . ?
C41 C42 H42 120.0 . . ?
C42 C43 C44 120.8(3) . . ?
C42 C43 H43 119.6 . . ?
C44 C43 H43 119.6 . . ?
C43 C44 C45 119.7(4) . . ?
C43 C44 H44 120.1 . . ?
C45 C44 H44 120.1 . . ?
C40 C45 C44 120.3(4) . . ?
C40 C45 H45 119.9 . . ?
C44 C45 H45 119.9 . . ?
F11 C46 F12 106.6(3) . . ?
F11 C46 F10 106.3(3) . . ?
F12 C46 F10 105.2(3) . . ?
F11 C46 C41 112.9(3) . . ?
F12 C46 C41 112.3(3) . . ?
F10 C46 C41 113.1(3) . . ?
O6 V2 O5 113.96(12) . . ?
O6 V2 O4 114.68(12) . . ?
O5 V2 O4 131.36(11) . . ?
O6 V2 N7 97.05(13) . . ?
O5 V2 N7 87.23(11) . . ?
O4 V2 N7 87.16(11) . . ?
O6 V2 N5 96.75(12) . . ?
O5 V2 N5 87.29(11) . . ?
O4 V2 N5 86.98(11) . . ?
N7 V2 N5 166.20(12) . . ?
C47 O4 V2 133.6(2) . . ?
C70 O5 V2 132.9(2) . . ?
C53 N5 C63 115.6(3) . . ?
C53 N5 V2 124.9(2) . . ?
C63 N5 V2 118.3(2) . . ?
C76 N7 C86 115.5(3) . . ?
C76 N7 V2 124.1(2) . . ?
C86 N7 V2 119.4(2) . . ?
O4 C47 C52 120.0(3) . . ?
O4 C47 C48 123.1(3) . . ?
C52 C47 C48 116.9(3) . . ?
C49 C48 C47 120.6(3) . . ?
C49 C48 C53 116.9(3) . . ?
C47 C48 C53 122.4(3) . . ?
C50 C49 C48 122.3(3) . . ?
C50 C49 H49 118.9 . . ?
C48 C49 H49 118.9 . . ?
C49 C50 C51 116.8(3) . . ?
C49 C50 C54 122.2(3) . . ?
C51 C50 C54 121.0(3) . . ?
C52 C51 C50 123.1(3) . . ?
C52 C51 H51 118.5 . . ?
C50 C51 H51 118.5 . . ?
C51 C52 C47 120.4(3) . . ?
C51 C52 C55 120.2(3) . . ?
C47 C52 C55 119.4(3) . . ?
N5 C53 C48 126.2(3) . . ?
N5 C53 H53 116.9 . . ?
C48 C53 H53 116.9 . . ?
C50 C54 H54A 109.5 . . ?
C50 C54 H54B 109.5 . . ?
H54A C54 H54B 109.5 . . ?
C50 C54 H54C 109.5 . . ?
H54A C54 H54C 109.5 . . ?
H54B C54 H54C 109.5 . . ?
N6 C55 C52 121.1(3) . . ?
N6 C55 H55 119.5 . . ?
C52 C55 H55 119.5 . . ?
C55 N6 C56 116.9(3) . . ?
C61 C56 C57 118.7(3) . . ?
C61 C56 N6 121.1(3) . . ?
C57 C56 N6 120.2(3) . . ?
C58 C57 C56 120.0(4) . . ?
C58 C57 C62 119.7(3) . . ?
C56 C57 C62 120.3(3) . . ?
C57 C58 C59 120.6(4) . . ?
C57 C58 H58 119.7 . . ?
C59 C58 H58 119.7 . . ?
C60 C59 C58 119.4(4) . . ?
C60 C59 H59 120.3 . . ?
C58 C59 H59 120.3 . . ?
C59 C60 C61 120.4(4) . . ?
C59 C60 H60 119.8 . . ?
C61 C60 H60 119.8 . . ?
C56 C61 C60 120.7(4) . . ?
C56 C61 H61 119.7 . . ?
C60 C61 H61 119.7 . . ?
F14 C62 F13 105.6(3) . . ?
F14 C62 F15 106.0(3) . . ?
F13 C62 F15 106.0(3) . . ?
F14 C62 C57 112.6(3) . . ?
F13 C62 C57 113.0(3) . . ?
F15 C62 C57 112.9(3) . . ?
C68 C63 C64 119.7(3) . . ?
C68 C63 N5 118.5(3) . . ?
C64 C63 N5 121.8(3) . . ?
C65 C64 C63 119.6(3) . . ?
C65 C64 C69 119.0(3) . . ?
C63 C64 C69 121.4(3) . . ?
C66 C65 C64 120.6(3) . . ?
C66 C65 H65 119.7 . . ?
C64 C65 H65 119.7 . . ?
C65 C66 C67 119.9(3) . . ?
C65 C66 H66 120.1 . . ?
C67 C66 H66 120.1 . . ?
C68 C67 C66 120.0(3) . . ?
C68 C67 H67 120.0 . . ?
C66 C67 H67 120.0 . . ?
C63 C68 C67 120.2(3) . . ?
C63 C68 H68 119.9 . . ?
C67 C68 H68 119.9 . . ?
F18 C69 F16 106.5(3) . . ?
F18 C69 F17 105.5(3) . . ?
F16 C69 F17 105.7(3) . . ?
F18 C69 C64 112.3(3) . . ?
F16 C69 C64 112.8(3) . . ?
F17 C69 C64 113.3(3) . . ?
O5 C70 C75 119.2(3) . . ?
O5 C70 C71 123.2(3) . . ?
C75 C70 C71 117.6(3) . . ?
C72 C71 C70 120.5(3) . . ?
C72 C71 C76 117.0(3) . . ?
C70 C71 C76 122.4(3) . . ?
C73 C72 C71 121.9(3) . . ?
C73 C72 H72 119.1 . . ?
C71 C72 H72 119.1 . . ?
C72 C73 C74 117.3(3) . . ?
C72 C73 C77 121.9(4) . . ?
C74 C73 C77 120.8(3) . . ?
C73 C74 C75 122.8(3) . . ?
C73 C74 H74 118.6 . . ?
C75 C74 H74 118.6 . . ?
C74 C75 C70 119.9(3) . . ?
C74 C75 C78 120.5(3) . . ?
C70 C75 C78 119.6(3) . . ?
N7 C76 C71 126.4(3) . . ?
N7 C76 H76 116.8 . . ?
C71 C76 H76 116.8 . . ?
C73 C77 H77A 109.5 . . ?
C73 C77 H77B 109.5 . . ?
H77A C77 H77B 109.5 . . ?
C73 C77 H77C 109.5 . . ?
H77A C77 H77C 109.5 . . ?
H77B C77 H77C 109.5 . . ?
N8 C78 C75 121.4(3) . . ?
N8 C78 H78 119.3 . . ?
C75 C78 H78 119.3 . . ?
C78 N8 C79 116.9(3) . . ?
C84 C79 C80 119.5(3) . . ?
C84 C79 N8 121.2(3) . . ?
C80 C79 N8 119.3(3) . . ?
C81 C80 C79 119.3(4) . . ?
C81 C80 C85 120.1(3) . . ?
C79 C80 C85 120.5(4) . . ?
C82 C81 C80 120.3(4) . . ?
C82 C81 H81 119.8 . . ?
C80 C81 H81 119.8 . . ?
C81 C82 C83 120.7(4) . . ?
C81 C82 H82 119.6 . . ?
C83 C82 H82 119.6 . . ?
C82 C83 C84 119.5(4) . . ?
C82 C83 H83 120.3 . . ?
C84 C83 H83 120.3 . . ?
C79 C84 C83 120.6(4) . . ?
C79 C84 H84 119.7 . . ?
C83 C84 H84 119.7 . . ?
F20 C85 F19 105.5(3) . . ?
F20 C85 F21 106.1(3) . . ?
F19 C85 F21 105.8(3) . . ?
F20 C85 C80 113.1(3) . . ?
F19 C85 C80 112.5(4) . . ?
F21 C85 C80 113.3(3) . . ?
C91 C86 C87 119.5(3) . . ?
C91 C86 N7 119.1(3) . . ?
C87 C86 N7 121.4(3) . . ?
C88 C87 C86 119.3(3) . . ?
C88 C87 C92 119.3(3) . . ?
C86 C87 C92 121.4(3) . . ?
C89 C88 C87 120.5(3) . . ?
C89 C88 H88 119.7 . . ?
C87 C88 H88 119.7 . . ?
C88 C89 C90 120.5(3) . . ?
C88 C89 H89 119.8 . . ?
C90 C89 H89 119.8 . . ?
C91 C90 C89 119.7(4) . . ?
C91 C90 H90 120.1 . . ?
C89 C90 H90 120.1 . . ?
C90 C91 C86 120.5(4) . . ?
C90 C91 H91 119.7 . . ?
C86 C91 H91 119.7 . . ?
F23 C92 F22 106.8(3) . . ?
F23 C92 F24 105.8(3) . . ?
F22 C92 F24 104.8(3) . . ?
F23 C92 C87 113.1(3) . . ?
F22 C92 C87 112.5(3) . . ?
F24 C92 C87 113.1(3) . . ?
N9 C93 C94 179.3(5) . . ?
C93 C94 H94A 109.5 . . ?
C93 C94 H94B 109.5 . . ?
H94A C94 H94B 109.5 . . ?
C93 C94 H94C 109.5 . . ?
H94A C94 H94C 109.5 . . ?
H94B C94 H94C 109.5 . . ?
N10 C95 C96 179.0(5) . . ?
C95 C96 H96A 109.5 . . ?
C95 C96 H96B 109.5 . . ?
H96A C96 H96B 109.5 . . ?
C95 C96 H96C 109.5 . . ?
H96A C96 H96C 109.5 . . ?
H96B C96 H96C 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 173.9(2) . . . . ?
V1 O1 C1 C2 -5.9(5) . . . . ?
O1 C1 C2 C3 -179.4(3) . . . . ?
C6 C1 C2 C3 0.8(5) . . . . ?
O1 C1 C2 C7 -3.0(5) . . . . ?
C6 C1 C2 C7 177.1(3) . . . . ?
C1 C2 C3 C4 -0.3(5) . . . . ?
C7 C2 C3 C4 -176.8(3) . . . . ?
C2 C3 C4 C5 0.0(5) . . . . ?
C2 C3 C4 C8 179.0(3) . . . . ?
C3 C4 C5 C6 -0.3(5) . . . . ?
C8 C4 C5 C6 -179.3(3) . . . . ?
C4 C5 C6 C1 0.8(5) . . . . ?
C4 C5 C6 C9 178.9(3) . . . . ?
O1 C1 C6 C5 179.1(3) . . . . ?
C2 C1 C6 C5 -1.1(5) . . . . ?
O1 C1 C6 C9 1.0(5) . . . . ?
C2 C1 C6 C9 -179.2(3) . . . . ?
C17 N1 C7 C2 -176.1(3) . . . . ?
V1 N1 C7 C2 16.3(5) . . . . ?
C3 C2 C7 N1 173.0(3) . . . . ?
C1 C2 C7 N1 -3.5(5) . . . . ?
C5 C6 C9 N2 16.7(5) . . . . ?
C1 C6 C9 N2 -165.2(3) . . . . ?
C6 C9 N2 C10 -175.1(3) . . . . ?
C9 N2 C10 C15 59.8(5) . . . . ?
C9 N2 C10 C11 -122.7(4) . . . . ?
C15 C10 C11 C12 -3.4(5) . . . . ?
N2 C10 C11 C12 179.0(3) . . . . ?
C15 C10 C11 C16 177.4(3) . . . . ?
N2 C10 C11 C16 -0.1(5) . . . . ?
C10 C11 C12 C13 2.7(5) . . . . ?
C16 C11 C12 C13 -178.1(4) . . . . ?
C11 C12 C13 C14 -0.1(6) . . . . ?
C12 C13 C14 C15 -1.9(6) . . . . ?
C11 C10 C15 C14 1.5(6) . . . . ?
N2 C10 C15 C14 179.0(3) . . . . ?
C13 C14 C15 C10 1.1(6) . . . . ?
C12 C11 C16 F2 -2.5(5) . . . . ?
C10 C11 C16 F2 176.6(3) . . . . ?
C12 C11 C16 F1 -123.3(4) . . . . ?
C10 C11 C16 F1 55.8(5) . . . . ?
C12 C11 C16 F3 116.6(4) . . . . ?
C10 C11 C16 F3 -64.2(4) . . . . ?
C7 N1 C17 C22 -110.9(4) . . . . ?
V1 N1 C17 C22 57.6(4) . . . . ?
C7 N1 C17 C18 68.9(4) . . . . ?
V1 N1 C17 C18 -122.6(3) . . . . ?
C22 C17 C18 C19 1.0(5) . . . . ?
N1 C17 C18 C19 -178.8(3) . . . . ?
C22 C17 C18 C23 -177.0(3) . . . . ?
N1 C17 C18 C23 3.2(5) . . . . ?
C17 C18 C19 C20 0.8(5) . . . . ?
C23 C18 C19 C20 178.8(3) . . . . ?
C18 C19 C20 C21 -1.4(5) . . . . ?
C19 C20 C21 C22 0.2(6) . . . . ?
C18 C17 C22 C21 -2.2(5) . . . . ?
N1 C17 C22 C21 177.6(3) . . . . ?
C20 C21 C22 C17 1.6(5) . . . . ?
C19 C18 C23 F6 -8.0(5) . . . . ?
C17 C18 C23 F6 169.9(3) . . . . ?
C19 C18 C23 F4 -128.0(3) . . . . ?
C17 C18 C23 F4 49.9(5) . . . . ?
C19 C18 C23 F5 110.8(4) . . . . ?
C17 C18 C23 F5 -71.3(4) . . . . ?
V1 O2 C24 C29 169.9(2) . . . . ?
V1 O2 C24 C25 -8.2(5) . . . . ?
O2 C24 C25 C26 178.0(3) . . . . ?
C29 C24 C25 C26 -0.1(5) . . . . ?
O2 C24 C25 C30 -4.9(5) . . . . ?
C29 C24 C25 C30 177.0(3) . . . . ?
C24 C25 C26 C27 1.2(5) . . . . ?
C30 C25 C26 C27 -176.0(3) . . . . ?
C25 C26 C27 C28 -1.0(5) . . . . ?
C25 C26 C27 C31 178.1(3) . . . . ?
C26 C27 C28 C29 -0.4(5) . . . . ?
C31 C27 C28 C29 -179.5(3) . . . . ?
C27 C28 C29 C24 1.6(5) . . . . ?
C27 C28 C29 C32 -177.0(3) . . . . ?
O2 C24 C29 C28 -179.4(3) . . . . ?
C25 C24 C29 C28 -1.3(5) . . . . ?
O2 C24 C29 C32 -0.8(5) . . . . ?
C25 C24 C29 C32 177.3(3) . . . . ?
C40 N3 C30 C25 -175.3(3) . . . . ?
V1 N3 C30 C25 15.8(5) . . . . ?
C26 C25 C30 N3 176.8(3) . . . . ?
C24 C25 C30 N3 -0.4(6) . . . . ?
C28 C29 C32 N4 19.7(5) . . . . ?
C24 C29 C32 N4 -158.8(3) . . . . ?
C29 C32 N4 C33 -178.4(3) . . . . ?
C32 N4 C33 C38 58.8(5) . . . . ?
C32 N4 C33 C34 -122.5(4) . . . . ?
C38 C33 C34 C35 -2.7(5) . . . . ?
N4 C33 C34 C35 178.7(3) . . . . ?
C38 C33 C34 C39 179.3(3) . . . . ?
N4 C33 C34 C39 0.7(5) . . . . ?
C33 C34 C35 C36 2.1(6) . . . . ?
C39 C34 C35 C36 -179.9(4) . . . . ?
C34 C35 C36 C37 -0.5(6) . . . . ?
C35 C36 C37 C38 -0.6(6) . . . . ?
C34 C33 C38 C37 1.7(6) . . . . ?
N4 C33 C38 C37 -179.7(3) . . . . ?
C36 C37 C38 C33 0.0(6) . . . . ?
C35 C34 C39 F8 115.0(4) . . . . ?
C33 C34 C39 F8 -67.0(5) . . . . ?
C35 C34 C39 F7 -123.6(4) . . . . ?
C33 C34 C39 F7 54.4(5) . . . . ?
C35 C34 C39 F9 -4.4(5) . . . . ?
C33 C34 C39 F9 173.6(3) . . . . ?
C30 N3 C40 C45 -110.2(4) . . . . ?
V1 N3 C40 C45 59.3(4) . . . . ?
C30 N3 C40 C41 70.8(4) . . . . ?
V1 N3 C40 C41 -119.7(3) . . . . ?
C45 C40 C41 C42 1.6(5) . . . . ?
N3 C40 C41 C42 -179.5(3) . . . . ?
C45 C40 C41 C46 -177.2(3) . . . . ?
N3 C40 C41 C46 1.7(5) . . . . ?
C40 C41 C42 C43 0.1(5) . . . . ?
C46 C41 C42 C43 178.9(3) . . . . ?
C41 C42 C43 C44 -0.8(6) . . . . ?
C42 C43 C44 C45 -0.1(6) . . . . ?
C41 C40 C45 C44 -2.5(6) . . . . ?
N3 C40 C45 C44 178.5(3) . . . . ?
C43 C44 C45 C40 1.7(6) . . . . ?
C42 C41 C46 F11 -129.6(3) . . . . ?
C40 C41 C46 F11 49.2(5) . . . . ?
C42 C41 C46 F12 -9.1(5) . . . . ?
C40 C41 C46 F12 169.7(3) . . . . ?
C42 C41 C46 F10 109.7(4) . . . . ?
C40 C41 C46 F10 -71.5(4) . . . . ?
V2 O4 C47 C52 172.7(2) . . . . ?
V2 O4 C47 C48 -7.4(5) . . . . ?
O4 C47 C48 C49 -179.8(3) . . . . ?
C52 C47 C48 C49 0.2(5) . . . . ?
O4 C47 C48 C53 -3.4(5) . . . . ?
C52 C47 C48 C53 176.6(3) . . . . ?
C47 C48 C49 C50 0.1(5) . . . . ?
C53 C48 C49 C50 -176.5(3) . . . . ?
C48 C49 C50 C51 0.1(5) . . . . ?
C48 C49 C50 C54 178.9(3) . . . . ?
C49 C50 C51 C52 -0.6(5) . . . . ?
C54 C50 C51 C52 -179.4(3) . . . . ?
C50 C51 C52 C47 0.9(5) . . . . ?
C50 C51 C52 C55 179.0(3) . . . . ?
O4 C47 C52 C51 179.3(3) . . . . ?
C48 C47 C52 C51 -0.7(5) . . . . ?
O4 C47 C52 C55 1.2(5) . . . . ?
C48 C47 C52 C55 -178.8(3) . . . . ?
C63 N5 C53 C48 -176.7(3) . . . . ?
V2 N5 C53 C48 16.0(5) . . . . ?
C49 C48 C53 N5 174.1(3) . . . . ?
C47 C48 C53 N5 -2.4(6) . . . . ?
C51 C52 C55 N6 16.4(5) . . . . ?
C47 C52 C55 N6 -165.5(3) . . . . ?
C52 C55 N6 C56 -175.6(3) . . . . ?
C55 N6 C56 C61 59.4(5) . . . . ?
C55 N6 C56 C57 -123.0(4) . . . . ?
C61 C56 C57 C58 -4.1(5) . . . . ?
N6 C56 C57 C58 178.3(3) . . . . ?
C61 C56 C57 C62 177.2(3) . . . . ?
N6 C56 C57 C62 -0.5(5) . . . . ?
C56 C57 C58 C59 2.9(6) . . . . ?
C62 C57 C58 C59 -178.4(4) . . . . ?
C57 C58 C59 C60 0.2(6) . . . . ?
C58 C59 C60 C61 -2.1(6) . . . . ?
C57 C56 C61 C60 2.3(6) . . . . ?
N6 C56 C61 C60 179.9(3) . . . . ?
C59 C60 C61 C56 0.8(6) . . . . ?
C58 C57 C62 F14 -1.6(5) . . . . ?
C56 C57 C62 F14 177.1(3) . . . . ?
C58 C57 C62 F13 118.0(4) . . . . ?
C56 C57 C62 F13 -63.3(4) . . . . ?
C58 C57 C62 F15 -121.7(4) . . . . ?
C56 C57 C62 F15 57.1(5) . . . . ?
C53 N5 C63 C68 -109.0(4) . . . . ?
V2 N5 C63 C68 59.3(4) . . . . ?
C53 N5 C63 C64 70.2(4) . . . . ?
V2 N5 C63 C64 -121.5(3) . . . . ?
C68 C63 C64 C65 0.8(5) . . . . ?
N5 C63 C64 C65 -178.4(3) . . . . ?
C68 C63 C64 C69 -177.6(3) . . . . ?
N5 C63 C64 C69 3.2(5) . . . . ?
C63 C64 C65 C66 0.8(5) . . . . ?
C69 C64 C65 C66 179.2(3) . . . . ?
C64 C65 C66 C67 -1.5(5) . . . . ?
C65 C66 C67 C68 0.7(6) . . . . ?
C64 C63 C68 C67 -1.6(5) . . . . ?
N5 C63 C68 C67 177.7(3) . . . . ?
C66 C67 C68 C63 0.8(6) . . . . ?
C65 C64 C69 F18 -8.6(5) . . . . ?
C63 C64 C69 F18 169.7(3) . . . . ?
C65 C64 C69 F16 -129.0(3) . . . . ?
C63 C64 C69 F16 49.4(5) . . . . ?
C65 C64 C69 F17 110.9(4) . . . . ?
C63 C64 C69 F17 -70.8(4) . . . . ?
V2 O5 C70 C75 170.1(2) . . . . ?
V2 O5 C70 C71 -8.5(5) . . . . ?
O5 C70 C71 C72 178.5(3) . . . . ?
C75 C70 C71 C72 -0.1(5) . . . . ?
O5 C70 C71 C76 -4.3(5) . . . . ?
C75 C70 C71 C76 177.1(3) . . . . ?
C70 C71 C72 C73 2.1(5) . . . . ?
C76 C71 C72 C73 -175.3(3) . . . . ?
C71 C72 C73 C74 -2.2(5) . . . . ?
C71 C72 C73 C77 176.6(4) . . . . ?
C72 C73 C74 C75 0.4(5) . . . . ?
C77 C73 C74 C75 -178.5(3) . . . . ?
C73 C74 C75 C70 1.6(5) . . . . ?
C73 C74 C75 C78 -178.4(3) . . . . ?
O5 C70 C75 C74 179.7(3) . . . . ?
C71 C70 C75 C74 -1.7(5) . . . . ?
O5 C70 C75 C78 -0.3(5) . . . . ?
C71 C70 C75 C78 178.4(3) . . . . ?
C86 N7 C76 C71 -174.2(3) . . . . ?
V2 N7 C76 C71 17.7(5) . . . . ?
C72 C71 C76 N7 175.4(3) . . . . ?
C70 C71 C76 N7 -2.0(6) . . . . ?
C74 C75 C78 N8 21.1(5) . . . . ?
C70 C75 C78 N8 -159.0(3) . . . . ?
C75 C78 N8 C79 -177.0(3) . . . . ?
C78 N8 C79 C84 60.2(5) . . . . ?
C78 N8 C79 C80 -122.1(4) . . . . ?
C84 C79 C80 C81 -3.2(5) . . . . ?
N8 C79 C80 C81 179.0(3) . . . . ?
C84 C79 C80 C85 178.2(3) . . . . ?
N8 C79 C80 C85 0.4(5) . . . . ?
C79 C80 C81 C82 2.3(6) . . . . ?
C85 C80 C81 C82 -179.1(4) . . . . ?
C80 C81 C82 C83 -0.3(6) . . . . ?
C81 C82 C83 C84 -0.8(6) . . . . ?
C80 C79 C84 C83 2.2(6) . . . . ?
N8 C79 C84 C83 179.9(3) . . . . ?
C82 C83 C84 C79 -0.2(6) . . . . ?
C81 C80 C85 F20 114.4(4) . . . . ?
C79 C80 C85 F20 -67.0(5) . . . . ?
C81 C80 C85 F19 -4.9(5) . . . . ?
C79 C80 C85 F19 173.7(3) . . . . ?
C81 C80 C85 F21 -124.7(4) . . . . ?
C79 C80 C85 F21 53.8(5) . . . . ?
C76 N7 C86 C91 -109.6(4) . . . . ?
V2 N7 C86 C91 59.2(4) . . . . ?
C76 N7 C86 C87 70.9(4) . . . . ?
V2 N7 C86 C87 -120.3(3) . . . . ?
C91 C86 C87 C88 1.4(5) . . . . ?
N7 C86 C87 C88 -179.1(3) . . . . ?
C91 C86 C87 C92 -176.7(3) . . . . ?
N7 C86 C87 C92 2.8(5) . . . . ?
C86 C87 C88 C89 0.2(5) . . . . ?
C92 C87 C88 C89 178.3(3) . . . . ?
C87 C88 C89 C90 -1.0(6) . . . . ?
C88 C89 C90 C91 0.2(6) . . . . ?
C89 C90 C91 C86 1.4(6) . . . . ?
C87 C86 C91 C90 -2.2(6) . . . . ?
N7 C86 C91 C90 178.3(3) . . . . ?
C88 C87 C92 F23 -129.2(4) . . . . ?
C86 C87 C92 F23 48.9(5) . . . . ?
C88 C87 C92 F22 -8.0(5) . . . . ?
C86 C87 C92 F22 170.1(3) . . . . ?
C88 C87 C92 F24 110.6(4) . . . . ?
C86 C87 C92 F24 -71.4(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
C22 H22 O3 0.95 2.52 3.207(4) 129.4 . yes
C30 H30 N9 0.95 2.50 3.381(5) 154.1 . yes
C45 H45 O3 0.95 2.63 3.296(4) 127.6 . yes
C68 H68 O6 0.95 2.56 3.229(4) 128.0 . yes
C76 H76 N10 0.95 2.49 3.376(5) 155.9 . yes
C91 H91 O6 0.95 2.66 3.320(4) 127.5 . yes

_refine_diff_density_max         1.481
_refine_diff_density_min         -0.473
_refine_diff_density_rms         0.114

_chemical_properties_physical    Air-sensitive,Moisture-sensitive
