# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2020

####################################################################### 
# 
# 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_LUC_AL_I_062
_database_code_depnum_ccdc_archive 'CCDC 1906128'
loop_
_audit_author_name
_audit_author_address
'Matthias Zeller'
;Purdue University
United States of America
;
_audit_update_record             
;
2019-03-27 deposited with the CCDC.	2019-12-18 downloaded from the CCDC.
;
_chemical_name_systematic        ?
_chemical_name_common            AL-II-062
_chemical_formula_moiety         ?
_chemical_formula_sum            'C72 H100 N12 O2 V2'
_chemical_formula_iupac          ?
_chemical_formula_weight         1267.51

_chemical_melting_point          ?

_space_group_crystal_system      triclinic
_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                   11.7050(12)
_cell_length_b                   12.9909(14)
_cell_length_c                   13.1353(15)
_cell_angle_alpha                96.537(7)
_cell_angle_beta                 110.688(6)
_cell_angle_gamma                106.507(7)
_cell_volume                     1739.7(3)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    2621
_cell_measurement_theta_min      2.4465
_cell_measurement_theta_max      21.7957
_cell_measurement_temperature    120.(2)

_exptl_crystal_description       plate
_exptl_crystal_colour            brown
_exptl_crystal_size_max          0.377
_exptl_crystal_size_mid          0.315
_exptl_crystal_size_min          0.058
_exptl_crystal_density_diffrn    1.210
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             678

_exptl_absorpt_coefficient_mu    0.321
_exptl_absorpt_correction_type   Multi-Scan
_exptl_absorpt_process_details   
;
SADABS V2016/2 - Bruker AXS area detector scaling and absorption correction
;
_exptl_absorpt_correction_T_min  0.82
_exptl_absorpt_correction_T_max  0.98

_exptl_special_details           
;
;

_diffrn_ambient_temperature      120.(2)

_diffrn_source                   'fine-focus tube'
_diffrn_source_type              ?

_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  graphite

_diffrn_measurement_device_type  'Bruker Kappa APEXII CCD'
_diffrn_measurement_method       'φ and ω scans'

_diffrn_detector_area_resol_mean 8.3333

_diffrn_reflns_number            26521
_diffrn_reflns_av_R_equivalents  0.0915
_diffrn_reflns_av_unetI/netI     0.1087
_diffrn_reflns_theta_min         1.68
_diffrn_reflns_theta_max         26.42
_diffrn_reflns_theta_full        26.42
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       15

_refine_special_details          
;
;

_reflns_number_total             7133
_reflns_number_gt                4226
_reflns_threshold_expression     'I > 2σ(I)'

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_R_factor_all          0.1196
_refine_ls_R_factor_gt           0.0558
_refine_ls_wR_factor_gt          0.1088
_refine_ls_wR_factor_ref         0.1305
_refine_ls_goodness_of_fit_ref   1.003
_refine_ls_restrained_S_all      1.003
_refine_ls_number_reflns         7133
_refine_ls_number_parameters     450
_refine_ls_number_restraints     0
_refine_ls_number_constraints    ?
_refine_ls_hydrogen_treatment    constr
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0513P)²+0.4349P] where P=(Fo²+2Fc²)/3'

_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?

_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         0.465
_refine_diff_density_min         -0.557
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?

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'

_computing_data_collection       'Bruker Instrument Service v2012.12.0.3'
_computing_cell_refinement       'SAINT V8.38A (Bruker AXS Inc., 2017)'
_computing_data_reduction        'SAINT V8.38A (Bruker AXS Inc., 2017)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_refinement_flags_posn
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
V V1 0.11640(5) 0.54729(4) 0.49975(4) 0.01620(15) Uani d . . . 1.0 . .
N N1 0.1814(2) 0.7201(2) 0.58439(18) 0.0170(6) Uani d . . . 1.0 . .
N N2 0.2861(2) 0.7707(2) 0.68613(19) 0.0184(6) Uani d . . . 1.0 . .
N N3 0.3144(2) 0.5779(2) 0.56796(18) 0.0158(5) Uani d . . . 1.0 . .
N N4 0.2214(2) 0.4189(2) 0.35376(18) 0.0188(6) Uani d . . . 1.0 . .
N N5 0.1243(2) 0.4611(2) 0.35050(19) 0.0215(6) Uani d . . . 1.0 . .
N N6 0.0696(2) 0.46426(19) 0.57394(18) 0.0165(6) Uani d . . . 1.0 . .
C C1 0.1356(3) 0.8016(3) 0.5539(2) 0.0190(7) Uani d . . . 1.0 . .
C C2 0.0252(3) 0.7862(3) 0.4441(2) 0.0233(7) Uani d . . . 1.0 . .
H H2 0.00325 0.712016 0.395995 0.028 Uiso calc U . R 1.0 . .
C C3 -0.0957(3) 0.7902(3) 0.4618(3) 0.0373(9) Uani d . . . 1.0 . .
H H3A -0.122188 0.732026 0.498783 0.056 Uiso calc U . R 1.0 . .
H H3B -0.166696 0.778681 0.389136 0.056 Uiso calc U . R 1.0 . .
H H3C -0.075796 0.862519 0.508876 0.056 Uiso calc U . R 1.0 . .
C C4 0.0675(3) 0.8747(3) 0.3842(3) 0.0367(9) Uani d . . . 1.0 . .
H H4A 0.084513 0.947765 0.428147 0.055 Uiso calc U . R 1.0 . .
H H4B -0.001932 0.860433 0.309842 0.055 Uiso calc U . R 1.0 . .
H H4C 0.146982 0.872611 0.376149 0.055 Uiso calc U . R 1.0 . .
C C5 0.2086(3) 0.9000(3) 0.6354(3) 0.0268(8) Uani d . . . 1.0 . .
H H5 0.195254 0.968788 0.63487 0.032 Uiso calc U . R 1.0 . .
C C6 0.3027(3) 0.8780(3) 0.7159(3) 0.0258(8) Uani d . . . 1.0 . .
H H6 0.368998 0.929682 0.782051 0.031 Uiso calc U . R 1.0 . .
C C7 0.3698(3) 0.7157(2) 0.7418(2) 0.0172(7) Uani d . . . 1.0 . .
C C8 0.4470(3) 0.7534(2) 0.8562(2) 0.0202(7) Uani d . . . 1.0 . .
H H8 0.439672 0.814446 0.897363 0.024 Uiso calc U . R 1.0 . .
C C9 0.5349(3) 0.7045(3) 0.9124(2) 0.0204(7) Uani d . . . 1.0 . .
C C10 0.6256(3) 0.7499(3) 1.0379(2) 0.0278(8) Uani d . . . 1.0 . .
C C11 0.7671(3) 0.7835(3) 1.0500(3) 0.0440(10) Uani d . . . 1.0 . .
H H11A 0.781394 0.719722 1.016163 0.066 Uiso calc U . R 1.0 . .
H H11B 0.825857 0.809358 1.129646 0.066 Uiso calc U . R 1.0 . .
H H11C 0.784629 0.843119 1.011996 0.066 Uiso calc U . R 1.0 . .
C C12 0.5994(4) 0.6598(3) 1.1013(3) 0.0472(11) Uani d . . . 1.0 . .
H H12A 0.509022 0.638627 1.093764 0.071 Uiso calc U . R 1.0 . .
H H12B 0.658525 0.68812 1.18069 0.071 Uiso calc U . R 1.0 . .
H H12C 0.614077 0.595001 1.069811 0.071 Uiso calc U . R 1.0 . .
C C13 0.6067(4) 0.8513(3) 1.0907(3) 0.0423(10) Uani d . . . 1.0 . .
H H13A 0.622866 0.909456 1.050781 0.063 Uiso calc U . R 1.0 . .
H H13B 0.66789 0.878268 1.169577 0.063 Uiso calc U . R 1.0 . .
H H13C 0.517218 0.831172 1.085508 0.063 Uiso calc U . R 1.0 . .
C C14 0.5420(3) 0.6126(3) 0.8531(2) 0.0211(7) Uani d . . . 1.0 . .
H H14 0.599393 0.576952 0.890546 0.025 Uiso calc U . R 1.0 . .
C C15 0.4646(3) 0.5725(2) 0.7379(2) 0.0165(6) Uani d . . . 1.0 . .
C C16 0.3807(2) 0.6260(2) 0.6815(2) 0.0151(6) Uani d . . . 1.0 . .
C C17 0.4466(3) 0.4814(2) 0.6532(2) 0.0180(7) Uani d . . . 1.0 . .
C C18 0.4948(3) 0.3952(2) 0.6536(2) 0.0209(7) Uani d . . . 1.0 . .
H H18 0.556488 0.390443 0.721426 0.025 Uiso calc U . R 1.0 . .
C C19 0.4533(3) 0.3155(3) 0.5551(3) 0.0226(7) Uani d . . . 1.0 . .
C C20 0.4969(3) 0.2150(3) 0.5578(3) 0.0314(8) Uani d . . . 1.0 . .
C C21 0.4267(4) 0.1396(3) 0.6143(3) 0.0420(10) Uani d . . . 1.0 . .
H H21A 0.45144 0.179083 0.69131 0.063 Uiso calc U . R 1.0 . .
H H21B 0.451229 0.073499 0.615375 0.063 Uiso calc U . R 1.0 . .
H H21C 0.332319 0.117817 0.572542 0.063 Uiso calc U . R 1.0 . .
C C22 0.6440(3) 0.2512(3) 0.6227(3) 0.0460(10) Uani d . . . 1.0 . .
H H22A 0.687961 0.301728 0.587279 0.069 Uiso calc U . R 1.0 . .
H H22B 0.670548 0.18613 0.62247 0.069 Uiso calc U . R 1.0 . .
H H22C 0.667907 0.288926 0.700159 0.069 Uiso calc U . R 1.0 . .
C C23 0.4616(4) 0.1487(3) 0.4396(3) 0.0489(11) Uani d . . . 1.0 . .
H H23A 0.366575 0.116589 0.399606 0.073 Uiso calc U . R 1.0 . .
H H23B 0.498152 0.089401 0.445265 0.073 Uiso calc U . R 1.0 . .
H H23C 0.497493 0.197896 0.398639 0.073 Uiso calc U . R 1.0 . .
C C24 0.3613(3) 0.3257(3) 0.4569(3) 0.0227(7) Uani d . . . 1.0 . .
H H24 0.331428 0.271798 0.38922 0.027 Uiso calc U . R 1.0 . .
C C25 0.3128(3) 0.4106(2) 0.4550(2) 0.0178(7) Uani d . . . 1.0 . .
C C26 0.3550(3) 0.4901(2) 0.5533(2) 0.0153(6) Uani d . . . 1.0 . .
C C27 0.2157(3) 0.3883(3) 0.2501(2) 0.0286(8) Uani d . . . 1.0 . .
H H27 0.272844 0.357881 0.231784 0.034 Uiso calc U . R 1.0 . .
C C28 0.1140(3) 0.4085(3) 0.1765(3) 0.0395(10) Uani d . . . 1.0 . .
H H28 0.086001 0.394672 0.097375 0.047 Uiso calc U . R 1.0 . .
C C29 0.0585(3) 0.4538(3) 0.2403(2) 0.0347(9) Uani d . . . 1.0 . .
C C30 -0.0414(13) 0.5152(10) 0.1984(12) 0.028(3) Uani d . P . 0.561(12) A 1
H H30 -0.07169 0.530979 0.25879 0.034 Uiso calc U P R 0.561(12) A 1
C C31 0.0112(13) 0.6224(13) 0.1697(14) 0.048(3) Uani d . P . 0.561(12) A 1
H H31A 0.080195 0.675867 0.2375 0.072 Uiso calc U P R 0.561(12) A 1
H H31B -0.059167 0.651448 0.138763 0.072 Uiso calc U P R 0.561(12) A 1
H H31C 0.046794 0.609795 0.114116 0.072 Uiso calc U P R 0.561(12) A 1
C C32 -0.1600(14) 0.4333(11) 0.0954(13) 0.048(3) Uani d . P . 0.561(12) A 1
H H32A -0.135338 0.423827 0.031897 0.071 Uiso calc U P R 0.561(12) A 1
H H32B -0.231566 0.462393 0.075592 0.071 Uiso calc U P R 0.561(12) A 1
H H32C -0.188273 0.361692 0.113352 0.071 Uiso calc U P R 0.561(12) A 1
C C31A -0.0335(18) 0.5813(17) 0.167(2) 0.048(3) Uani d . P . 0.439(12) A 2
H H31D 0.031916 0.636308 0.235479 0.072 Uiso calc U P R 0.439(12) A 2
H H31E -0.111986 0.601103 0.139822 0.072 Uiso calc U P R 0.439(12) A 2
H H31F 0.001584 0.579582 0.109628 0.072 Uiso calc U P R 0.439(12) A 2
C C30A -0.0682(17) 0.4666(12) 0.1929(16) 0.028(3) Uani d . P . 0.439(12) A 2
H H30A -0.101912 0.470524 0.252883 0.034 Uiso calc U P R 0.439(12) A 2
C C32A -0.171(2) 0.3790(14) 0.0925(18) 0.048(3) Uani d . P . 0.439(12) A 2
H H32D -0.143279 0.378577 0.030463 0.071 Uiso calc U P R 0.439(12) A 2
H H32E -0.252739 0.39453 0.070414 0.071 Uiso calc U P R 0.439(12) A 2
H H32F -0.18527 0.306731 0.110936 0.071 Uiso calc U P R 0.439(12) A 2
O O1 0.8546(3) 0.0784(2) 1.0265(2) 0.0537(8) Uani d . . . 1.0 . .
C C33 1.0100(4) 0.1050(4) 1.2099(3) 0.0629(13) Uani d . . . 1.0 . .
H H33A 0.948429 0.04301 1.220882 0.094 Uiso calc U P R 0.519(8) B 1
H H33B 1.001409 0.174395 1.237979 0.094 Uiso calc U P R 0.519(8) B 1
H H33C 1.099125 0.107267 1.250837 0.094 Uiso calc U P R 0.519(8) B 1
H H33D 1.07568 0.104114 1.180076 0.094 Uiso calc U P R 0.481(8) B 2
H H33E 0.970131 0.03106 1.218354 0.094 Uiso calc U P R 0.481(8) B 2
H H33F 1.051637 0.157864 1.283028 0.094 Uiso calc U P R 0.481(8) B 2
C C34 0.9818(7) 0.0908(7) 1.0899(6) 0.049(3) Uani d . P . 0.519(8) B 1
H H34A 1.040636 0.155938 1.078746 0.059 Uiso calc U P R 0.519(8) B 1
H H34B 0.999671 0.024849 1.063746 0.059 Uiso calc U P R 0.519(8) B 1
C C35 0.8193(11) 0.0807(9) 0.9165(8) 0.057(3) Uani d . P . 0.519(8) B 1
H H35A 0.834094 0.019472 0.877031 0.068 Uiso calc U P R 0.519(8) B 1
H H35B 0.875157 0.151098 0.910744 0.068 Uiso calc U P R 0.519(8) B 1
C C36 0.6851(13) 0.0707(12) 0.8624(12) 0.090(4) Uani d . P . 0.519(8) B 1
H H36A 0.660692 0.061704 0.781633 0.134 Uiso calc U P R 0.519(8) B 1
H H36B 0.673065 0.137456 0.892713 0.134 Uiso calc U P R 0.519(8) B 1
H H36C 0.630006 0.00613 0.876089 0.134 Uiso calc U P R 0.519(8) B 1
C C34A 0.9040(10) 0.1399(8) 1.1283(7) 0.067(4) Uani d . P . 0.481(8) B 2
H H34C 0.833639 0.133931 1.154904 0.08 Uiso calc U P R 0.481(8) B 2
H H34D 0.942275 0.218129 1.127565 0.08 Uiso calc U P R 0.481(8) B 2
C C35A 0.7585(14) 0.0962(10) 0.9384(10) 0.063(3) Uani d . P . 0.481(8) B 2
H H35C 0.794277 0.171331 0.928408 0.076 Uiso calc U P R 0.481(8) B 2
H H35D 0.684378 0.093699 0.958981 0.076 Uiso calc U P R 0.481(8) B 2
C C36A 0.7090(15) 0.0147(13) 0.8293(10) 0.084(4) Uani d . P . 0.481(8) B 2
H H36D 0.780032 0.020941 0.804655 0.126 Uiso calc U P R 0.481(8) B 2
H H36E 0.638652 0.030027 0.772927 0.126 Uiso calc U P R 0.481(8) B 2
H H36F 0.675697 -0.060235 0.838554 0.126 Uiso calc U P R 0.481(8) 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_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
V1 N6 . 1.641(2) ?
V1 N6 2_566 1.997(2) ?
V1 N3 . 2.064(2) ?
V1 N1 . 2.172(2) ?
V1 N5 . 2.189(2) ?
V1 V1 2_566 2.6546(11) ?
N1 C1 . 1.354(4) ?
N1 N2 . 1.380(3) ?
N2 C6 . 1.343(4) ?
N2 C7 . 1.420(4) ?
N3 C26 . 1.373(4) ?
N3 C16 . 1.383(3) ?
N4 C27 . 1.347(4) ?
N4 N5 . 1.385(3) ?
N4 C25 . 1.420(3) ?
N5 C29 . 1.355(4) ?
C1 C5 . 1.391(4) ?
C1 C2 . 1.504(4) ?
C2 C3 . 1.527(4) ?
C2 C4 . 1.531(4) ?
C2 H2 . 1.0 ?
C3 H3A . 0.98 ?
C3 H3B . 0.98 ?
C3 H3C . 0.98 ?
C4 H4A . 0.98 ?
C4 H4B . 0.98 ?
C4 H4C . 0.98 ?
C5 C6 . 1.355(4) ?
C5 H5 . 0.95 ?
C6 H6 . 0.95 ?
C7 C8 . 1.391(4) ?
C7 C16 . 1.395(4) ?
C8 C9 . 1.397(4) ?
C8 H8 . 0.95 ?
C9 C14 . 1.389(4) ?
C9 C10 . 1.542(4) ?
C10 C13 . 1.527(5) ?
C10 C11 . 1.531(5) ?
C10 C12 . 1.535(5) ?
C11 H11A . 0.98 ?
C11 H11B . 0.98 ?
C11 H11C . 0.98 ?
C12 H12A . 0.98 ?
C12 H12B . 0.98 ?
C12 H12C . 0.98 ?
C13 H13A . 0.98 ?
C13 H13B . 0.98 ?
C13 H13C . 0.98 ?
C14 C15 . 1.402(4) ?
C14 H14 . 0.95 ?
C15 C16 . 1.410(4) ?
C15 C17 . 1.441(4) ?
C17 C18 . 1.389(4) ?
C17 C26 . 1.412(4) ?
C18 C19 . 1.395(4) ?
C18 H18 . 0.95 ?
C19 C24 . 1.407(4) ?
C19 C20 . 1.531(4) ?
C20 C21 . 1.524(5) ?
C20 C22 . 1.524(5) ?
C20 C23 . 1.537(5) ?
C21 H21A . 0.98 ?
C21 H21B . 0.98 ?
C21 H21C . 0.98 ?
C22 H22A . 0.98 ?
C22 H22B . 0.98 ?
C22 H22C . 0.98 ?
C23 H23A . 0.98 ?
C23 H23B . 0.98 ?
C23 H23C . 0.98 ?
C24 C25 . 1.376(4) ?
C24 H24 . 0.95 ?
C25 C26 . 1.391(4) ?
C27 C28 . 1.359(4) ?
C27 H27 . 0.95 ?
C28 C29 . 1.400(4) ?
C28 H28 . 0.95 ?
C29 C30A . 1.46(2) ?
C29 C30 . 1.576(15) ?
C30 C31 . 1.502(15) ?
C30 C32 . 1.548(17) ?
C30 H30 . 1.0 ?
C31 H31A . 0.98 ?
C31 H31B . 0.98 ?
C31 H31C . 0.98 ?
C32 H32A . 0.98 ?
C32 H32B . 0.98 ?
C32 H32C . 0.98 ?
C31A C30A . 1.54(2) ?
C31A H31D . 0.98 ?
C31A H31E . 0.98 ?
C31A H31F . 0.98 ?
C30A C32A . 1.50(2) ?
C30A H30A . 1.0 ?
C32A H32D . 0.98 ?
C32A H32E . 0.98 ?
C32A H32F . 0.98 ?
O1 C34A . 1.306(8) ?
O1 C35 . 1.362(10) ?
O1 C34 . 1.376(7) ?
O1 C35A . 1.396(12) ?
C33 C34 . 1.469(8) ?
C33 C34A . 1.544(10) ?
C33 H33A . 0.98 ?
C33 H33B . 0.98 ?
C33 H33C . 0.98 ?
C33 H33D . 0.98 ?
C33 H33E . 0.98 ?
C33 H33F . 0.98 ?
C34 H34A . 0.99 ?
C34 H34B . 0.99 ?
C35 C36 . 1.436(17) ?
C35 H35A . 0.99 ?
C35 H35B . 0.99 ?
C36 H36A . 0.98 ?
C36 H36B . 0.98 ?
C36 H36C . 0.98 ?
C34A H34C . 0.99 ?
C34A H34D . 0.99 ?
C35A C36A . 1.493(19) ?
C35A H35C . 0.99 ?
C35A H35D . 0.99 ?
C36A H36D . 0.98 ?
C36A H36E . 0.98 ?
C36A H36F . 0.98 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
N6 V1 N6 . 2_566 86.83(11) ?
N6 V1 N3 . . 100.42(10) ?
N6 V1 N3 2_566 . 172.36(10) ?
N6 V1 N1 . . 111.93(10) ?
N6 V1 N1 2_566 . 93.52(9) ?
N3 V1 N1 . . 81.58(9) ?
N6 V1 N5 . . 113.41(11) ?
N6 V1 N5 2_566 . 96.00(9) ?
N3 V1 N5 . . 83.40(9) ?
N1 V1 N5 . . 134.04(10) ?
N6 V1 V1 . 2_566 48.70(8) ?
N6 V1 V1 2_566 2_566 38.12(7) ?
N3 V1 V1 . 2_566 149.05(8) ?
N1 V1 V1 . 2_566 106.09(7) ?
N5 V1 V1 . 2_566 108.92(7) ?
C1 N1 N2 . . 104.6(2) ?
C1 N1 V1 . . 130.79(18) ?
N2 N1 V1 . . 124.63(18) ?
C6 N2 N1 . . 110.6(2) ?
C6 N2 C7 . . 126.7(2) ?
N1 N2 C7 . . 122.4(2) ?
C26 N3 C16 . . 103.9(2) ?
C26 N3 V1 . . 117.43(18) ?
C16 N3 V1 . . 116.76(18) ?
C27 N4 N5 . . 111.0(2) ?
C27 N4 C25 . . 126.2(2) ?
N5 N4 C25 . . 122.8(2) ?
C29 N5 N4 . . 104.6(2) ?
C29 N5 V1 . . 130.8(2) ?
N4 N5 V1 . . 123.63(16) ?
V1 N6 V1 . 2_566 93.17(11) ?
N1 C1 C5 . . 110.4(3) ?
N1 C1 C2 . . 123.6(3) ?
C5 C1 C2 . . 126.0(3) ?
C1 C2 C3 . . 110.9(3) ?
C1 C2 C4 . . 109.8(3) ?
C3 C2 C4 . . 110.8(3) ?
C1 C2 H2 . . 108.4 ?
C3 C2 H2 . . 108.4 ?
C4 C2 H2 . . 108.4 ?
C2 C3 H3A . . 109.5 ?
C2 C3 H3B . . 109.5 ?
H3A C3 H3B . . 109.5 ?
C2 C3 H3C . . 109.5 ?
H3A C3 H3C . . 109.5 ?
H3B C3 H3C . . 109.5 ?
C2 C4 H4A . . 109.5 ?
C2 C4 H4B . . 109.5 ?
H4A C4 H4B . . 109.5 ?
C2 C4 H4C . . 109.5 ?
H4A C4 H4C . . 109.5 ?
H4B C4 H4C . . 109.5 ?
C6 C5 C1 . . 106.1(3) ?
C6 C5 H5 . . 127.0 ?
C1 C5 H5 . . 127.0 ?
N2 C6 C5 . . 108.3(3) ?
N2 C6 H6 . . 125.8 ?
C5 C6 H6 . . 125.8 ?
C8 C7 C16 . . 118.8(3) ?
C8 C7 N2 . . 120.7(3) ?
C16 C7 N2 . . 120.4(2) ?
C7 C8 C9 . . 122.2(3) ?
C7 C8 H8 . . 118.9 ?
C9 C8 H8 . . 118.9 ?
C14 C9 C8 . . 118.9(3) ?
C14 C9 C10 . . 118.8(3) ?
C8 C9 C10 . . 122.2(3) ?
C13 C10 C11 . . 108.0(3) ?
C13 C10 C12 . . 108.6(3) ?
C11 C10 C12 . . 109.6(3) ?
C13 C10 C9 . . 112.5(3) ?
C11 C10 C9 . . 108.6(3) ?
C12 C10 C9 . . 109.5(3) ?
C10 C11 H11A . . 109.5 ?
C10 C11 H11B . . 109.5 ?
H11A C11 H11B . . 109.5 ?
C10 C11 H11C . . 109.5 ?
H11A C11 H11C . . 109.5 ?
H11B C11 H11C . . 109.5 ?
C10 C12 H12A . . 109.5 ?
C10 C12 H12B . . 109.5 ?
H12A C12 H12B . . 109.5 ?
C10 C12 H12C . . 109.5 ?
H12A C12 H12C . . 109.5 ?
H12B C12 H12C . . 109.5 ?
C10 C13 H13A . . 109.5 ?
C10 C13 H13B . . 109.5 ?
H13A C13 H13B . . 109.5 ?
C10 C13 H13C . . 109.5 ?
H13A C13 H13C . . 109.5 ?
H13B C13 H13C . . 109.5 ?
C9 C14 C15 . . 120.0(3) ?
C9 C14 H14 . . 120.0 ?
C15 C14 H14 . . 120.0 ?
C14 C15 C16 . . 120.2(3) ?
C14 C15 C17 . . 134.5(3) ?
C16 C15 C17 . . 105.3(2) ?
N3 C16 C7 . . 127.5(3) ?
N3 C16 C15 . . 112.8(2) ?
C7 C16 C15 . . 119.7(2) ?
C18 C17 C26 . . 120.7(3) ?
C18 C17 C15 . . 134.6(3) ?
C26 C17 C15 . . 104.6(2) ?
C17 C18 C19 . . 120.5(3) ?
C17 C18 H18 . . 119.7 ?
C19 C18 H18 . . 119.7 ?
C18 C19 C24 . . 117.6(3) ?
C18 C19 C20 . . 120.3(3) ?
C24 C19 C20 . . 121.8(3) ?
C21 C20 C22 . . 110.2(3) ?
C21 C20 C19 . . 107.8(3) ?
C22 C20 C19 . . 110.5(3) ?
C21 C20 C23 . . 108.1(3) ?
C22 C20 C23 . . 108.1(3) ?
C19 C20 C23 . . 112.1(3) ?
C20 C21 H21A . . 109.5 ?
C20 C21 H21B . . 109.5 ?
H21A C21 H21B . . 109.5 ?
C20 C21 H21C . . 109.5 ?
H21A C21 H21C . . 109.5 ?
H21B C21 H21C . . 109.5 ?
C20 C22 H22A . . 109.5 ?
C20 C22 H22B . . 109.5 ?
H22A C22 H22B . . 109.5 ?
C20 C22 H22C . . 109.5 ?
H22A C22 H22C . . 109.5 ?
H22B C22 H22C . . 109.5 ?
C20 C23 H23A . . 109.5 ?
C20 C23 H23B . . 109.5 ?
H23A C23 H23B . . 109.5 ?
C20 C23 H23C . . 109.5 ?
H23A C23 H23C . . 109.5 ?
H23B C23 H23C . . 109.5 ?
C25 C24 C19 . . 122.6(3) ?
C25 C24 H24 . . 118.7 ?
C19 C24 H24 . . 118.7 ?
C24 C25 C26 . . 119.5(3) ?
C24 C25 N4 . . 120.9(3) ?
C26 C25 N4 . . 119.6(3) ?
N3 C26 C25 . . 127.5(2) ?
N3 C26 C17 . . 113.4(2) ?
C25 C26 C17 . . 119.0(3) ?
N4 C27 C28 . . 107.9(3) ?
N4 C27 H27 . . 126.0 ?
C28 C27 H27 . . 126.0 ?
C27 C28 C29 . . 106.3(3) ?
C27 C28 H28 . . 126.8 ?
C29 C28 H28 . . 126.8 ?
N5 C29 C28 . . 110.2(3) ?
N5 C29 C30A . . 124.4(8) ?
C28 C29 C30A . . 123.9(8) ?
N5 C29 C30 . . 122.4(6) ?
C28 C29 C30 . . 125.8(6) ?
C31 C30 C32 . . 110.5(11) ?
C31 C30 C29 . . 115.2(10) ?
C32 C30 C29 . . 106.9(8) ?
C31 C30 H30 . . 108.0 ?
C32 C30 H30 . . 108.0 ?
C29 C30 H30 . . 108.0 ?
C30 C31 H31A . . 109.5 ?
C30 C31 H31B . . 109.5 ?
H31A C31 H31B . . 109.5 ?
C30 C31 H31C . . 109.5 ?
H31A C31 H31C . . 109.5 ?
H31B C31 H31C . . 109.5 ?
C30 C32 H32A . . 109.5 ?
C30 C32 H32B . . 109.5 ?
H32A C32 H32B . . 109.5 ?
C30 C32 H32C . . 109.5 ?
H32A C32 H32C . . 109.5 ?
H32B C32 H32C . . 109.5 ?
C30A C31A H31D . . 109.5 ?
C30A C31A H31E . . 109.5 ?
H31D C31A H31E . . 109.5 ?
C30A C31A H31F . . 109.5 ?
H31D C31A H31F . . 109.5 ?
H31E C31A H31F . . 109.5 ?
C29 C30A C32A . . 116.8(14) ?
C29 C30A C31A . . 102.6(12) ?
C32A C30A C31A . . 112.2(15) ?
C29 C30A H30A . . 108.3 ?
C32A C30A H30A . . 108.3 ?
C31A C30A H30A . . 108.3 ?
C30A C32A H32D . . 109.5 ?
C30A C32A H32E . . 109.5 ?
H32D C32A H32E . . 109.5 ?
C30A C32A H32F . . 109.5 ?
H32D C32A H32F . . 109.5 ?
H32E C32A H32F . . 109.5 ?
C35 O1 C34 . . 118.8(7) ?
C34A O1 C35A . . 121.7(8) ?
C34 C33 H33A . . 109.5 ?
C34 C33 H33B . . 109.5 ?
H33A C33 H33B . . 109.5 ?
C34 C33 H33C . . 109.5 ?
H33A C33 H33C . . 109.5 ?
H33B C33 H33C . . 109.5 ?
C34A C33 H33D . . 109.5 ?
C34A C33 H33E . . 109.5 ?
H33D C33 H33E . . 109.5 ?
C34A C33 H33F . . 109.5 ?
H33D C33 H33F . . 109.5 ?
H33E C33 H33F . . 109.5 ?
O1 C34 C33 . . 112.3(6) ?
O1 C34 H34A . . 109.1 ?
C33 C34 H34A . . 109.1 ?
O1 C34 H34B . . 109.1 ?
C33 C34 H34B . . 109.1 ?
H34A C34 H34B . . 107.9 ?
O1 C35 C36 . . 112.4(12) ?
O1 C35 H35A . . 109.1 ?
C36 C35 H35A . . 109.1 ?
O1 C35 H35B . . 109.1 ?
C36 C35 H35B . . 109.1 ?
H35A C35 H35B . . 107.9 ?
C35 C36 H36A . . 109.5 ?
C35 C36 H36B . . 109.5 ?
H36A C36 H36B . . 109.5 ?
C35 C36 H36C . . 109.5 ?
H36A C36 H36C . . 109.5 ?
H36B C36 H36C . . 109.5 ?
O1 C34A C33 . . 111.7(7) ?
O1 C34A H34C . . 109.3 ?
C33 C34A H34C . . 109.3 ?
O1 C34A H34D . . 109.3 ?
C33 C34A H34D . . 109.3 ?
H34C C34A H34D . . 107.9 ?
O1 C35A C36A . . 114.3(11) ?
O1 C35A H35C . . 108.7 ?
C36A C35A H35C . . 108.7 ?
O1 C35A H35D . . 108.7 ?
C36A C35A H35D . . 108.7 ?
H35C C35A H35D . . 107.6 ?
C35A C36A H36D . . 109.5 ?
C35A C36A H36E . . 109.5 ?
H36D C36A H36E . . 109.5 ?
C35A C36A H36F . . 109.5 ?
H36D C36A H36F . . 109.5 ?
H36E C36A H36F . . 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_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
C1 N1 N2 C6 . . . . 0.1(3) ?
V1 N1 N2 C6 . . . . 179.3(2) ?
C1 N1 N2 C7 . . . . -173.7(3) ?
V1 N1 N2 C7 . . . . 5.5(4) ?
C27 N4 N5 C29 . . . . 0.6(3) ?
C25 N4 N5 C29 . . . . -179.4(3) ?
C27 N4 N5 V1 . . . . -168.9(2) ?
C25 N4 N5 V1 . . . . 11.0(4) ?
N6 V1 N6 V1 2_566 . . 2_566 -0.001(2) ?
N3 V1 N6 V1 . . . 2_566 177.57(9) ?
N1 V1 N6 V1 . . . 2_566 92.52(10) ?
N5 V1 N6 V1 . . . 2_566 -95.16(10) ?
N2 N1 C1 C5 . . . . -0.9(3) ?
V1 N1 C1 C5 . . . . 179.9(2) ?
N2 N1 C1 C2 . . . . 176.3(3) ?
V1 N1 C1 C2 . . . . -2.9(4) ?
N1 C1 C2 C3 . . . . 110.5(3) ?
C5 C1 C2 C3 . . . . -72.7(4) ?
N1 C1 C2 C4 . . . . -126.7(3) ?
C5 C1 C2 C4 . . . . 50.1(4) ?
N1 C1 C5 C6 . . . . 1.4(4) ?
C2 C1 C5 C6 . . . . -175.7(3) ?
N1 N2 C6 C5 . . . . 0.8(4) ?
C7 N2 C6 C5 . . . . 174.2(3) ?
C1 C5 C6 N2 . . . . -1.3(4) ?
C6 N2 C7 C8 . . . . 27.5(5) ?
N1 N2 C7 C8 . . . . -159.8(3) ?
C6 N2 C7 C16 . . . . -149.4(3) ?
N1 N2 C7 C16 . . . . 23.3(4) ?
C16 C7 C8 C9 . . . . 0.0(5) ?
N2 C7 C8 C9 . . . . -176.9(3) ?
C7 C8 C9 C14 . . . . -2.4(5) ?
C7 C8 C9 C10 . . . . 176.8(3) ?
C14 C9 C10 C13 . . . . 179.5(3) ?
C8 C9 C10 C13 . . . . 0.3(4) ?
C14 C9 C10 C11 . . . . 60.0(4) ?
C8 C9 C10 C11 . . . . -119.2(3) ?
C14 C9 C10 C12 . . . . -59.6(4) ?
C8 C9 C10 C12 . . . . 121.2(3) ?
C8 C9 C14 C15 . . . . 1.9(4) ?
C10 C9 C14 C15 . . . . -177.3(3) ?
C9 C14 C15 C16 . . . . 0.9(4) ?
C9 C14 C15 C17 . . . . -179.2(3) ?
C26 N3 C16 C7 . . . . -176.6(3) ?
V1 N3 C16 C7 . . . . -45.7(4) ?
C26 N3 C16 C15 . . . . 1.7(3) ?
V1 N3 C16 C15 . . . . 132.6(2) ?
C8 C7 C16 N3 . . . . -179.0(3) ?
N2 C7 C16 N3 . . . . -2.0(5) ?
C8 C7 C16 C15 . . . . 2.8(4) ?
N2 C7 C16 C15 . . . . 179.8(3) ?
C14 C15 C16 N3 . . . . 178.2(3) ?
C17 C15 C16 N3 . . . . -1.7(3) ?
C14 C15 C16 C7 . . . . -3.3(4) ?
C17 C15 C16 C7 . . . . 176.7(3) ?
C14 C15 C17 C18 . . . . 3.3(6) ?
C16 C15 C17 C18 . . . . -176.8(3) ?
C14 C15 C17 C26 . . . . -178.9(3) ?
C16 C15 C17 C26 . . . . 1.0(3) ?
C26 C17 C18 C19 . . . . -0.1(4) ?
C15 C17 C18 C19 . . . . 177.4(3) ?
C17 C18 C19 C24 . . . . -0.4(4) ?
C17 C18 C19 C20 . . . . -174.4(3) ?
C18 C19 C20 C21 . . . . 71.4(4) ?
C24 C19 C20 C21 . . . . -102.3(4) ?
C18 C19 C20 C22 . . . . -49.1(4) ?
C24 C19 C20 C22 . . . . 137.2(3) ?
C18 C19 C20 C23 . . . . -169.7(3) ?
C24 C19 C20 C23 . . . . 16.5(4) ?
C18 C19 C24 C25 . . . . 0.5(5) ?
C20 C19 C24 C25 . . . . 174.4(3) ?
C19 C24 C25 C26 . . . . -0.2(5) ?
C19 C24 C25 N4 . . . . 179.1(3) ?
C27 N4 C25 C24 . . . . -33.0(5) ?
N5 N4 C25 C24 . . . . 147.1(3) ?
C27 N4 C25 C26 . . . . 146.3(3) ?
N5 N4 C25 C26 . . . . -33.6(4) ?
C16 N3 C26 C25 . . . . 176.6(3) ?
V1 N3 C26 C25 . . . . 46.0(4) ?
C16 N3 C26 C17 . . . . -1.0(3) ?
V1 N3 C26 C17 . . . . -131.6(2) ?
C24 C25 C26 N3 . . . . -177.7(3) ?
N4 C25 C26 N3 . . . . 3.0(5) ?
C24 C25 C26 C17 . . . . -0.2(4) ?
N4 C25 C26 C17 . . . . -179.5(3) ?
C18 C17 C26 N3 . . . . 178.2(3) ?
C15 C17 C26 N3 . . . . 0.0(3) ?
C18 C17 C26 C25 . . . . 0.4(4) ?
C15 C17 C26 C25 . . . . -177.8(3) ?
N5 N4 C27 C28 . . . . -0.7(4) ?
C25 N4 C27 C28 . . . . 179.4(3) ?
N4 C27 C28 C29 . . . . 0.5(4) ?
N4 N5 C29 C28 . . . . -0.3(4) ?
V1 N5 C29 C28 . . . . 168.2(2) ?
N4 N5 C29 C30A . . . . 166.5(7) ?
V1 N5 C29 C30A . . . . -25.0(8) ?
N4 N5 C29 C30 . . . . -166.6(6) ?
V1 N5 C29 C30 . . . . 1.9(7) ?
C27 C28 C29 N5 . . . . -0.1(4) ?
C27 C28 C29 C30A . . . . -167.0(8) ?
C27 C28 C29 C30 . . . . 165.6(6) ?
N5 C29 C30 C31 . . . . 98.6(11) ?
C28 C29 C30 C31 . . . . -65.4(12) ?
N5 C29 C30 C32 . . . . -138.2(8) ?
C28 C29 C30 C32 . . . . 57.7(11) ?
N5 C29 C30A C32A . . . . -130.4(13) ?
C28 C29 C30A C32A . . . . 34.6(17) ?
N5 C29 C30A C31A . . . . 106.4(13) ?
C28 C29 C30A C31A . . . . -88.6(14) ?
C35 O1 C34 C33 . . . . 170.4(7) ?
C34 O1 C35 C36 . . . . -177.9(9) ?
C35A O1 C34A C33 . . . . -178.9(8) ?
C34A O1 C35A C36A . . . . -177.2(10) ?

####################################################################### 
# 
# 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_5
_database_code_depnum_ccdc_archive 'CCDC 1906131'
loop_
_audit_author_name
_audit_author_address
'Matthias Zeller'
;Purdue University
United States of America
;
_audit_update_record             
;
2019-03-27 deposited with the CCDC.	2019-12-18 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C68 H88 Cl N10 O3 V2'
_chemical_formula_weight         1230.81

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
V V 0.0687 2.1097 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 '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                   10.5713(9)
_cell_length_b                   16.0342(11)
_cell_length_c                   19.4152(15)
_cell_angle_alpha                94.679(6)
_cell_angle_beta                 95.011(6)
_cell_angle_gamma                99.765(5)
_cell_volume                     3215.2(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    62964
_cell_measurement_theta_min      4.594
_cell_measurement_theta_max      72.364

_exptl_crystal_description       needle
_exptl_crystal_colour            brown
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.271
_exptl_crystal_F_000             1306
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.040
_exptl_absorpt_coefficient_mu    3.238
_shelx_estimated_absorpt_T_min   0.564
_shelx_estimated_absorpt_T_max   0.881
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.662
_exptl_absorpt_correction_T_max  0.881
_exptl_absorpt_process_details   'SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_source                   'microfocus X-ray tube'
_diffrn_radiation_monochromator  'laterally graded multilayer (Goebel) mirror'
_diffrn_measurement_device_type  
'Rigaku Rapid II curved image plate diffractometer'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            62964
_diffrn_reflns_av_unetI/netI     0.1300
_diffrn_reflns_av_R_equivalents  ?
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         4.594
_diffrn_reflns_theta_max         72.364
_diffrn_reflns_theta_full        67.679
_diffrn_measured_fraction_theta_max 0.929
_diffrn_measured_fraction_theta_full 0.967
_diffrn_reflns_Laue_measured_fraction_max 0.929
_diffrn_reflns_Laue_measured_fraction_full 0.967
_diffrn_reflns_point_group_measured_fraction_max 0.929
_diffrn_reflns_point_group_measured_fraction_full 0.967
_reflns_number_total             62964
_reflns_number_gt                31570
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'CrystalClear-SM Expert 2.1 b32 (Rigaku, 2014)'
_computing_cell_refinement       'HKL3000 (Otwinowski & Minor, 1997)'
_computing_data_reduction        'HKL3000 (Otwinowski & Minor, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  
;  
SHELXL-2014/7 (Sheldrick, 2014), 
SHELXLE Rev794 (Hübschle et al., 2011)
;
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          
;
The crystal under investigation was found to be non-merohedrically 
twinned. HKL3000 lacks the ability to simultaneously integrate more 
than one twin domain. Rigaku programs compatible with the diffractometer 
(twinsolve) gave unsatisfactory results. With no usable data set 
obtainable through simultaneous integration of both twin domains, the 
data were instead handled as if not twinned, with only the major domain 
integrated, and converted into an hklf 5 type format hkl file after 
integration using the "Make HKLF5 File" routine as implemented in WinGX. 
The twin law and matrix were obtained using the program ROTAX as 
implemented in WinGX. The twin operation was identified as a 180 degree 
rotation around the reciprocal b-axis, the twin matrix as 

-1.000    0.000    0.000
 0.540    1.000    0.160
 0.000    0.000   -1.000

The Overlap R1 and R2 values in the "Make HKLF5 File" routine 
used were 0.11, i.e. reflections with a discriminator function less 
or equal to overlap radius of 0.11 were counted overlapped, all others
as single. The discriminator function used was the "delta function
on index non-integrality". No reflections were omitted.

The structure was solved using direct methods with all reflections of 
component 1. The structure was refined using the hklf 5 routine with 
all reflections of component 1 (including the overlapping ones) as 
obtained from WinGX, resulting in a BASF value of 0.216(4).

No Rint value is obtainable for the hklf 5 type file using the WinGX
routine.

The terminal Cl and O atoms of a Cl-V-O-V=O unit are disordered in 
a close to 1:1 ratio. The Uij components of ADPs of the V atoms and 
disordered V and O atoms were restrained to be similar, and the V=O 
bond distances were restrained to be similar as well. The occupancy 
ratio refined to 0.496(12) to 0.504(12). 

A THF molecule was refined as disordered over two orientations. The 
two moieties were restrained to have similar geometries. All O-C and 
C-C bond distances were restrained to be similar, and all 1,3 distances 
to be at least 2.40(2) Angstroms. The occupancy ratio refined to 
0.37(1) to 0.63(1). 
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1315P)²+11.5788P] 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         62964
_refine_ls_number_parameters     843
_refine_ls_number_restraints     248
_refine_ls_R_factor_all          0.2001
_refine_ls_R_factor_gt           0.1087
_refine_ls_wR_factor_ref         0.3430
_refine_ls_wR_factor_gt          0.2749
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_restrained_S_all      1.091
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
O2 O 0.768(3) 0.6400(16) 0.6103(14) 0.189(8) Uani 0.369(10) 1 d D U P A 1
C1 C 0.723(3) 0.5439(15) 0.6029(11) 0.166(8) Uani 0.369(10) 1 d D U P A 1
H1C H 0.7827 0.5152 0.5772 0.200 Uiso 0.369(10) 1 calc R U P A 1
H1D H 0.7192 0.5226 0.6492 0.200 Uiso 0.369(10) 1 calc R U P A 1
C2 C 0.589(3) 0.5261(17) 0.563(2) 0.187(9) Uani 0.369(10) 1 d D U P A 1
H2C H 0.5237 0.5011 0.5929 0.224 Uiso 0.369(10) 1 calc R U P A 1
H2D H 0.5865 0.4855 0.5215 0.224 Uiso 0.369(10) 1 calc R U P A 1
C3 C 0.558(3) 0.610(2) 0.541(3) 0.181(8) Uani 0.369(10) 1 d D U P A 1
H3C H 0.5177 0.6040 0.4928 0.217 Uiso 0.369(10) 1 calc R U P A 1
H3D H 0.5009 0.6339 0.5724 0.217 Uiso 0.369(10) 1 calc R U P A 1
C4 C 0.691(3) 0.6669(18) 0.548(2) 0.191(7) Uani 0.369(10) 1 d D U P A 1
H4C H 0.7344 0.6587 0.5056 0.229 Uiso 0.369(10) 1 calc R U P A 1
H4D H 0.6839 0.7275 0.5563 0.229 Uiso 0.369(10) 1 calc R U P A 1
O2C O 0.6183(17) 0.6842(10) 0.5885(11) 0.188(7) Uani 0.631(10) 1 d D U P A 2
C1C C 0.7604(16) 0.6951(12) 0.5763(16) 0.191(8) Uani 0.631(10) 1 d D U P A 2
H1CA H 0.7833 0.7444 0.5494 0.229 Uiso 0.631(10) 1 calc R U P A 2
H1CB H 0.8149 0.7058 0.6213 0.229 Uiso 0.631(10) 1 calc R U P A 2
C2C C 0.7847(14) 0.6144(14) 0.5362(14) 0.176(7) Uani 0.631(10) 1 d D U P A 2
H2CA H 0.8359 0.6278 0.4969 0.211 Uiso 0.631(10) 1 calc R U P A 2
H2CB H 0.8296 0.5799 0.5668 0.211 Uiso 0.631(10) 1 calc R U P A 2
C3C C 0.6478(17) 0.5694(14) 0.5107(11) 0.170(7) Uani 0.631(10) 1 d D U P A 2
H3CA H 0.6435 0.5076 0.4989 0.204 Uiso 0.631(10) 1 calc R U P A 2
H3CB H 0.6113 0.5944 0.4702 0.204 Uiso 0.631(10) 1 calc R U P A 2
C4C C 0.5815(19) 0.5876(12) 0.5756(12) 0.195(8) Uani 0.631(10) 1 d D U P A 2
H4CA H 0.4868 0.5691 0.5670 0.234 Uiso 0.631(10) 1 calc R U P A 2
H4CB H 0.6150 0.5595 0.6151 0.234 Uiso 0.631(10) 1 calc R U P A 2
O1 O 0.7282(6) 0.9071(4) 0.2341(3) 0.0625(19) Uani 1 1 d . . . . .
V1A V 0.88032(18) 0.88333(12) 0.27578(10) 0.0619(6) Uani 1 1 d D U . . .
Cl1A Cl 0.9988(8) 0.9720(5) 0.3593(5) 0.064(3) Uani 0.496(12) 1 d . U P B 1
O1A O 0.978(2) 0.9349(14) 0.3399(14) 0.089(8) Uani 0.504(12) 1 d D U P B 2
N1A N 1.0045(7) 0.9463(5) 0.2052(4) 0.061(2) Uani 1 1 d . . . . .
N2A N 1.0992(7) 0.9123(5) 0.1733(4) 0.059(2) Uani 1 1 d . . . . .
N3A N 0.9313(7) 0.7774(5) 0.2421(4) 0.053(2) Uani 1 1 d . . . . .
N4A N 0.7261(7) 0.7265(5) 0.3378(4) 0.056(2) Uani 1 1 d . . . . .
N5A N 0.7707(7) 0.8121(5) 0.3481(4) 0.055(2) Uani 1 1 d . . . . .
C1A C 1.1880(10) 0.9743(7) 0.1537(5) 0.064(3) Uani 1 1 d . . . . .
H1A H 1.2626 0.9663 0.1318 0.077 Uiso 1 1 calc R U . . .
C2A C 1.1520(10) 1.0508(7) 0.1709(5) 0.069(3) Uani 1 1 d . . . . .
H2A H 1.1948 1.1057 0.1629 0.082 Uiso 1 1 calc R U . . .
C3A C 1.0392(10) 1.0307(7) 0.2027(6) 0.062(3) Uani 1 1 d . . . . .
C4A C 0.9602(11) 1.0943(7) 0.2311(6) 0.071(3) Uani 1 1 d . . . . .
H4A H 0.8848 1.0624 0.2513 0.086 Uiso 1 1 calc R U . . .
C5A C 1.0417(11) 1.1544(8) 0.2881(8) 0.124(6) Uani 1 1 d . . . . .
H5AA H 1.1139 1.1881 0.2687 0.185 Uiso 1 1 calc R U . . .
H5AB H 1.0753 1.1217 0.3238 0.185 Uiso 1 1 calc R U . . .
H5AC H 0.9890 1.1924 0.3089 0.185 Uiso 1 1 calc R U . . .
C6A C 0.9094(13) 1.1392(8) 0.1707(7) 0.114(5) Uani 1 1 d . . . . .
H6AA H 0.9823 1.1683 0.1487 0.171 Uiso 1 1 calc R U . . .
H6AB H 0.8591 1.1809 0.1881 0.171 Uiso 1 1 calc R U . . .
H6AC H 0.8544 1.0972 0.1365 0.171 Uiso 1 1 calc R U . . .
C7A C 1.0150(9) 0.7633(6) 0.1913(5) 0.056(3) Uani 1 1 d . . . . .
C8A C 1.0891(9) 0.8235(6) 0.1563(6) 0.056(3) Uani 1 1 d . . . . .
C9A C 1.1510(9) 0.7950(6) 0.1003(5) 0.057(3) Uani 1 1 d . . . . .
H9A H 1.1951 0.8355 0.0736 0.069 Uiso 1 1 calc R U . . .
C10A C 1.1494(9) 0.7098(7) 0.0830(6) 0.058(3) Uani 1 1 d . . . . .
C11A C 1.0885(9) 0.6500(6) 0.1232(5) 0.059(3) Uani 1 1 d . . . . .
H11A H 1.0926 0.5915 0.1141 0.071 Uiso 1 1 calc R U . . .
C12A C 1.0225(9) 0.6771(6) 0.1760(5) 0.054(3) Uani 1 1 d . . . . .
C13A C 0.9408(9) 0.6319(6) 0.2233(5) 0.055(3) Uani 1 1 d . . . . .
C14A C 0.9158(9) 0.5481(6) 0.2353(5) 0.059(3) Uani 1 1 d . . . . .
H14A H 0.9558 0.5080 0.2105 0.071 Uiso 1 1 calc R U . . .
C15A C 0.8326(10) 0.5217(7) 0.2833(5) 0.059(3) Uani 1 1 d . . . . .
C16A C 0.7711(9) 0.5831(6) 0.3163(5) 0.059(3) Uani 1 1 d . . . . .
H16A H 0.7113 0.5656 0.3484 0.071 Uiso 1 1 calc R U . . .
C17A C 0.7943(9) 0.6678(6) 0.3038(5) 0.053(3) Uani 1 1 d . . . . .
C18A C 0.8865(9) 0.6961(6) 0.2594(5) 0.052(3) Uani 1 1 d . . . . .
C19A C 1.2047(10) 0.6819(7) 0.0142(6) 0.061(3) Uani 1 1 d . . . . .
C20A C 1.1083(14) 0.6926(11) -0.0440(7) 0.142(7) Uani 1 1 d . . . . .
H20A H 1.1143 0.6530 -0.0843 0.212 Uiso 1 1 calc R U . . .
H20B H 1.1260 0.7511 -0.0566 0.212 Uiso 1 1 calc R U . . .
H20C H 1.0212 0.6806 -0.0292 0.212 Uiso 1 1 calc R U . . .
C21A C 1.3313(12) 0.7356(8) 0.0069(7) 0.123(5) Uani 1 1 d . . . . .
H21A H 1.3641 0.7156 -0.0360 0.184 Uiso 1 1 calc R U . . .
H21B H 1.3927 0.7316 0.0468 0.184 Uiso 1 1 calc R U . . .
H21C H 1.3204 0.7949 0.0050 0.184 Uiso 1 1 calc R U . . .
C22A C 1.2235(14) 0.5908(8) 0.0111(7) 0.124(6) Uani 1 1 d . . . . .
H22A H 1.2588 0.5758 -0.0323 0.187 Uiso 1 1 calc R U . . .
H22B H 1.1403 0.5537 0.0130 0.187 Uiso 1 1 calc R U . . .
H22C H 1.2836 0.5836 0.0507 0.187 Uiso 1 1 calc R U . . .
C23A C 0.8117(11) 0.4295(6) 0.3005(6) 0.060(3) Uani 1 1 d . . . . .
C24A C 0.7708(11) 0.3704(7) 0.2335(6) 0.084(4) Uani 1 1 d . . . . .
H24A H 0.6914 0.3838 0.2105 0.126 Uiso 1 1 calc R U . . .
H24B H 0.7552 0.3112 0.2446 0.126 Uiso 1 1 calc R U . . .
H24C H 0.8393 0.3784 0.2026 0.126 Uiso 1 1 calc R U . . .
C25A C 0.9385(11) 0.4094(7) 0.3339(6) 0.085(4) Uani 1 1 d . . . . .
H25A H 1.0068 0.4236 0.3035 0.127 Uiso 1 1 calc R U . . .
H25B H 0.9275 0.3487 0.3404 0.127 Uiso 1 1 calc R U . . .
H25C H 0.9624 0.4430 0.3790 0.127 Uiso 1 1 calc R U . . .
C26A C 0.7081(11) 0.4116(6) 0.3504(6) 0.085(4) Uani 1 1 d . . . . .
H26A H 0.6271 0.4258 0.3302 0.128 Uiso 1 1 calc R U . . .
H26B H 0.7363 0.4463 0.3948 0.128 Uiso 1 1 calc R U . . .
H26C H 0.6947 0.3512 0.3582 0.128 Uiso 1 1 calc R U . . .
C27A C 0.6226(9) 0.7047(7) 0.3734(6) 0.067(3) Uani 1 1 d . . . . .
H27A H 0.5742 0.6491 0.3736 0.080 Uiso 1 1 calc R U . . .
C28A C 0.6004(9) 0.7764(6) 0.4088(5) 0.060(3) Uani 1 1 d . . . . .
H28A H 0.5343 0.7805 0.4384 0.072 Uiso 1 1 calc R U . . .
C29A C 0.6943(10) 0.8434(7) 0.3931(5) 0.056(3) Uani 1 1 d . . . . .
C30A C 0.7205(10) 0.9330(7) 0.4229(6) 0.070(3) Uani 1 1 d . . . . .
H30A H 0.7571 0.9697 0.3877 0.084 Uiso 1 1 calc R U . . .
C31A C 0.5975(10) 0.9622(7) 0.4449(6) 0.079(4) Uani 1 1 d . . . . .
H31A H 0.5303 0.9508 0.4055 0.118 Uiso 1 1 calc R U . . .
H31B H 0.6164 1.0234 0.4597 0.118 Uiso 1 1 calc R U . . .
H31C H 0.5673 0.9312 0.4835 0.118 Uiso 1 1 calc R U . . .
C32A C 0.8187(11) 0.9428(8) 0.4870(7) 0.099(4) Uani 1 1 d . . . . .
H32A H 0.8923 0.9163 0.4755 0.148 Uiso 1 1 calc R U . . .
H32B H 0.7781 0.9149 0.5246 0.148 Uiso 1 1 calc R U . . .
H32C H 0.8487 1.0033 0.5019 0.148 Uiso 1 1 calc R U . . .
V1B V 0.56156(17) 0.86891(11) 0.19532(10) 0.0591(6) Uani 1 1 d D U . . .
Cl1B Cl 0.4810(11) 0.9343(8) 0.1085(7) 0.070(3) Uani 0.504(12) 1 d . U P B 2
O1B O 0.477(3) 0.916(2) 0.1350(16) 0.101(11) Uani 0.496(12) 1 d D U P B 1
N1B N 0.6304(7) 0.7806(5) 0.1203(4) 0.058(2) Uani 1 1 d . . . . .
N2B N 0.6274(8) 0.6962(5) 0.1281(4) 0.060(2) Uani 1 1 d . . . . .
N3B N 0.4575(7) 0.7689(5) 0.2276(4) 0.055(2) Uani 1 1 d . . . . .
N4B N 0.3663(7) 0.9192(5) 0.3011(4) 0.058(2) Uani 1 1 d . . . . .
N5B N 0.4780(7) 0.9457(5) 0.2697(4) 0.060(2) Uani 1 1 d . . . . .
C1B C 0.7209(9) 0.6669(7) 0.0943(5) 0.066(3) Uani 1 1 d . . . . .
H1B H 0.7414 0.6115 0.0933 0.079 Uiso 1 1 calc R U . . .
C2B C 0.7793(9) 0.7336(7) 0.0619(5) 0.065(3) Uani 1 1 d . . . . .
H2B H 0.8478 0.7323 0.0335 0.078 Uiso 1 1 calc R U . . .
C3B C 0.7210(10) 0.8041(7) 0.0779(5) 0.059(3) Uani 1 1 d . . . . .
C4B C 0.7417(10) 0.8883(7) 0.0511(6) 0.066(3) Uani 1 1 d . . . . .
H4B H 0.7261 0.9318 0.0878 0.079 Uiso 1 1 calc R U . . .
C5B C 0.8772(9) 0.9158(7) 0.0285(6) 0.083(4) Uani 1 1 d . . . . .
H5BA H 0.8895 0.8775 -0.0113 0.124 Uiso 1 1 calc R U . . .
H5BB H 0.9423 0.9133 0.0671 0.124 Uiso 1 1 calc R U . . .
H5BC H 0.8861 0.9741 0.0155 0.124 Uiso 1 1 calc R U . . .
C6B C 0.6452(11) 0.8877(8) -0.0137(7) 0.108(5) Uani 1 1 d . . . . .
H6BA H 0.6638 0.8483 -0.0512 0.161 Uiso 1 1 calc R U . . .
H6BB H 0.6537 0.9451 -0.0288 0.161 Uiso 1 1 calc R U . . .
H6BC H 0.5571 0.8693 -0.0021 0.161 Uiso 1 1 calc R U . . .
C7B C 0.4578(9) 0.6837(6) 0.2076(5) 0.055(3) Uani 1 1 d . . . . .
C8B C 0.5294(10) 0.6465(7) 0.1598(6) 0.059(3) Uani 1 1 d . . . . .
C9B C 0.5034(9) 0.5591(7) 0.1445(6) 0.064(3) Uani 1 1 d . . . . .
H9B H 0.5525 0.5348 0.1121 0.077 Uiso 1 1 calc R U . . .
C10B C 0.4106(9) 0.5044(7) 0.1732(6) 0.058(3) Uani 1 1 d . . . . .
C11B C 0.3473(9) 0.5414(7) 0.2256(5) 0.062(3) Uani 1 1 d . . . . .
H11B H 0.2886 0.5060 0.2498 0.074 Uiso 1 1 calc R U . . .
C12B C 0.3695(9) 0.6288(7) 0.2423(6) 0.059(3) Uani 1 1 d . . . . .
C13B C 0.3173(9) 0.6823(6) 0.2898(5) 0.052(3) Uani 1 1 d . . . . .
C14B C 0.2379(9) 0.6664(6) 0.3423(5) 0.057(3) Uani 1 1 d . . . . .
H14B H 0.2027 0.6095 0.3494 0.068 Uiso 1 1 calc R U . . .
C15B C 0.2100(9) 0.7337(6) 0.3844(5) 0.049(3) Uani 1 1 d . . . . .
C16B C 0.2530(9) 0.8155(6) 0.3675(5) 0.057(3) Uani 1 1 d . . . . .
H16B H 0.2269 0.8611 0.3937 0.068 Uiso 1 1 calc R U . . .
C17B C 0.3304(9) 0.8355(6) 0.3157(5) 0.055(3) Uani 1 1 d . . . . .
C18B C 0.3684(9) 0.7662(6) 0.2769(5) 0.055(3) Uani 1 1 d . . . . .
C19B C 0.3717(10) 0.4095(7) 0.1506(6) 0.067(3) Uani 1 1 d . . . . .
C20B C 0.4532(10) 0.3795(6) 0.0966(6) 0.079(4) Uani 1 1 d . . . . .
H20D H 0.4245 0.3185 0.0833 0.118 Uiso 1 1 calc R U . . .
H20E H 0.5439 0.3900 0.1159 0.118 Uiso 1 1 calc R U . . .
H20F H 0.4442 0.4106 0.0555 0.118 Uiso 1 1 calc R U . . .
C21B C 0.3785(11) 0.3550(6) 0.2115(6) 0.079(4) Uani 1 1 d . . . . .
H21D H 0.3488 0.2950 0.1946 0.119 Uiso 1 1 calc R U . . .
H21E H 0.3233 0.3721 0.2461 0.119 Uiso 1 1 calc R U . . .
H21F H 0.4678 0.3630 0.2328 0.119 Uiso 1 1 calc R U . . .
C22B C 0.2304(10) 0.3917(7) 0.1176(6) 0.080(4) Uani 1 1 d . . . . .
H22D H 0.2232 0.4227 0.0764 0.121 Uiso 1 1 calc R U . . .
H22E H 0.1748 0.4105 0.1514 0.121 Uiso 1 1 calc R U . . .
H22F H 0.2034 0.3306 0.1042 0.121 Uiso 1 1 calc R U . . .
C23B C 0.1422(10) 0.7199(6) 0.4499(6) 0.056(3) Uani 1 1 d . . . . .
C24B C 0.2423(10) 0.7485(7) 0.5127(6) 0.087(4) Uani 1 1 d . . . . .
H24D H 0.3093 0.7131 0.5119 0.130 Uiso 1 1 calc R U . . .
H24E H 0.2002 0.7427 0.5555 0.130 Uiso 1 1 calc R U . . .
H24F H 0.2817 0.8081 0.5110 0.130 Uiso 1 1 calc R U . . .
C25B C 0.0849(10) 0.6270(6) 0.4541(6) 0.077(4) Uani 1 1 d . . . . .
H25D H 0.0311 0.6043 0.4107 0.115 Uiso 1 1 calc R U . . .
H25E H 0.0321 0.6224 0.4931 0.115 Uiso 1 1 calc R U . . .
H25F H 0.1547 0.5944 0.4611 0.115 Uiso 1 1 calc R U . . .
C26B C 0.0337(9) 0.7728(7) 0.4547(6) 0.074(3) Uani 1 1 d . . . . .
H26D H -0.0341 0.7525 0.4164 0.110 Uiso 1 1 calc R U . . .
H26E H 0.0690 0.8328 0.4516 0.110 Uiso 1 1 calc R U . . .
H26F H -0.0027 0.7666 0.4991 0.110 Uiso 1 1 calc R U . . .
C27B C 0.3126(10) 0.9857(6) 0.3230(5) 0.063(3) Uani 1 1 d . . . . .
H27B H 0.2360 0.9829 0.3455 0.076 Uiso 1 1 calc R U . . .
C28B C 0.3885(9) 1.0577(6) 0.3070(6) 0.066(3) Uani 1 1 d . . . . .
H28B H 0.3751 1.1145 0.3162 0.079 Uiso 1 1 calc R U . . .
C29B C 0.4902(9) 1.0314(7) 0.2745(6) 0.064(3) Uani 1 1 d . . . . .
C30B C 0.6001(10) 1.0869(6) 0.2476(6) 0.061(3) Uani 1 1 d . . . . .
H30B H 0.6560 1.0500 0.2258 0.073 Uiso 1 1 calc R U . . .
C31B C 0.6800(10) 1.1435(7) 0.3100(6) 0.076(3) Uani 1 1 d . . . . .
H31D H 0.7574 1.1762 0.2944 0.114 Uiso 1 1 calc R U . . .
H31E H 0.7054 1.1076 0.3454 0.114 Uiso 1 1 calc R U . . .
H31F H 0.6279 1.1827 0.3298 0.114 Uiso 1 1 calc R U . . .
C32B C 0.5476(10) 1.1390(7) 0.1924(6) 0.079(4) Uani 1 1 d . . . . .
H32D H 0.6197 1.1763 0.1758 0.119 Uiso 1 1 calc R U . . .
H32E H 0.4898 1.1737 0.2128 0.119 Uiso 1 1 calc R U . . .
H32F H 0.5000 1.1005 0.1534 0.119 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
O2 C1 1.525(8) . ?
O2 C4 1.525(8) . ?
C1 C2 1.525(8) . ?
C1 H1C 0.9900 . ?
C1 H1D 0.9900 . ?
C2 C3 1.525(8) . ?
C2 H2C 0.9900 . ?
C2 H2D 0.9900 . ?
C3 C4 1.525(8) . ?
C3 H3C 0.9900 . ?
C3 H3D 0.9900 . ?
C4 H4C 0.9900 . ?
C4 H4D 0.9900 . ?
O2C C4C 1.525(8) . ?
O2C C1C 1.525(8) . ?
C1C C2C 1.525(8) . ?
C1C H1CA 0.9900 . ?
C1C H1CB 0.9900 . ?
C2C C3C 1.524(8) . ?
C2C H2CA 0.9900 . ?
C2C H2CB 0.9900 . ?
C3C C4C 1.526(8) . ?
C3C H3CA 0.9900 . ?
C3C H3CB 0.9900 . ?
C4C H4CA 0.9900 . ?
C4C H4CB 0.9900 . ?
O1 V1B 1.836(7) . ?
O1 V1A 1.849(6) . ?
V1A O1A 1.62(3) . ?
V1A N3A 1.949(7) . ?
V1A N1A 2.171(8) . ?
V1A N5A 2.172(8) . ?
V1A Cl1A 2.210(9) . ?
N1A C3A 1.347(11) . ?
N1A N2A 1.386(9) . ?
N2A C1A 1.350(11) . ?
N2A C8A 1.418(11) . ?
N3A C18A 1.387(11) . ?
N3A C7A 1.410(10) . ?
N4A C27A 1.356(10) . ?
N4A N5A 1.366(9) . ?
N4A C17A 1.433(10) . ?
N5A C29A 1.363(10) . ?
C1A C2A 1.369(12) . ?
C1A H1A 0.9500 . ?
C2A C3A 1.392(12) . ?
C2A H2A 0.9500 . ?
C3A C4A 1.523(12) . ?
C4A C5A 1.507(15) . ?
C4A C6A 1.531(14) . ?
C4A H4A 1.0000 . ?
C5A H5AA 0.9800 . ?
C5A H5AB 0.9800 . ?
C5A H5AC 0.9800 . ?
C6A H6AA 0.9800 . ?
C6A H6AB 0.9800 . ?
C6A H6AC 0.9800 . ?
C7A C8A 1.397(12) . ?
C7A C12A 1.408(12) . ?
C8A C9A 1.401(12) . ?
C9A C10A 1.377(12) . ?
C9A H9A 0.9500 . ?
C10A C11A 1.394(12) . ?
C10A C19A 1.566(12) . ?
C11A C12A 1.372(11) . ?
C11A H11A 0.9500 . ?
C12A C13A 1.465(12) . ?
C13A C14A 1.368(12) . ?
C13A C18A 1.426(11) . ?
C14A C15A 1.379(12) . ?
C14A H14A 0.9500 . ?
C15A C16A 1.411(12) . ?
C15A C23A 1.525(12) . ?
C16A C17A 1.384(12) . ?
C16A H16A 0.9500 . ?
C17A C18A 1.400(12) . ?
C19A C21A 1.487(13) . ?
C19A C20A 1.495(15) . ?
C19A C22A 1.505(14) . ?
C20A H20A 0.9800 . ?
C20A H20B 0.9800 . ?
C20A H20C 0.9800 . ?
C21A H21A 0.9800 . ?
C21A H21B 0.9800 . ?
C21A H21C 0.9800 . ?
C22A H22A 0.9800 . ?
C22A H22B 0.9800 . ?
C22A H22C 0.9800 . ?
C23A C24A 1.528(13) . ?
C23A C26A 1.532(12) . ?
C23A C25A 1.533(13) . ?
C24A H24A 0.9800 . ?
C24A H24B 0.9800 . ?
C24A H24C 0.9800 . ?
C25A H25A 0.9800 . ?
C25A H25B 0.9800 . ?
C25A H25C 0.9800 . ?
C26A H26A 0.9800 . ?
C26A H26B 0.9800 . ?
C26A H26C 0.9800 . ?
C27A C28A 1.355(12) . ?
C27A H27A 0.9500 . ?
C28A C29A 1.406(12) . ?
C28A H28A 0.9500 . ?
C29A C30A 1.475(13) . ?
C30A C32A 1.528(15) . ?
C30A C31A 1.538(11) . ?
C30A H30A 1.0000 . ?
C31A H31A 0.9800 . ?
C31A H31B 0.9800 . ?
C31A H31C 0.9800 . ?
C32A H32A 0.9800 . ?
C32A H32B 0.9800 . ?
C32A H32C 0.9800 . ?
V1B O1B 1.72(3) . ?
V1B N3B 1.964(8) . ?
V1B N5B 2.164(8) . ?
V1B N1B 2.203(8) . ?
V1B Cl1B 2.237(12) . ?
N1B C3B 1.343(11) . ?
N1B N2B 1.369(10) . ?
N2B C1B 1.359(10) . ?
N2B C8B 1.414(11) . ?
N3B C7B 1.391(10) . ?
N3B C18B 1.400(10) . ?
N4B C27B 1.346(10) . ?
N4B C17B 1.391(11) . ?
N4B N5B 1.394(9) . ?
N5B C29B 1.354(11) . ?
C1B C2B 1.368(12) . ?
C1B H1B 0.9500 . ?
C2B C3B 1.402(13) . ?
C2B H2B 0.9500 . ?
C3B C4B 1.475(13) . ?
C4B C5B 1.538(12) . ?
C4B C6B 1.547(14) . ?
C4B H4B 1.0000 . ?
C5B H5BA 0.9800 . ?
C5B H5BB 0.9800 . ?
C5B H5BC 0.9800 . ?
C6B H6BA 0.9800 . ?
C6B H6BB 0.9800 . ?
C6B H6BC 0.9800 . ?
C7B C8B 1.405(12) . ?
C7B C12B 1.425(12) . ?
C8B C9B 1.384(12) . ?
C9B C10B 1.387(12) . ?
C9B H9B 0.9500 . ?
C10B C11B 1.411(12) . ?
C10B C19B 1.524(13) . ?
C11B C12B 1.388(12) . ?
C11B H11B 0.9500 . ?
C12B C13B 1.418(12) . ?
C13B C14B 1.390(12) . ?
C13B C18B 1.412(12) . ?
C14B C15B 1.388(12) . ?
C14B H14B 0.9500 . ?
C15B C16B 1.388(12) . ?
C15B C23B 1.527(12) . ?
C16B C17B 1.375(12) . ?
C16B H16B 0.9500 . ?
C17B C18B 1.425(12) . ?
C19B C20B 1.513(12) . ?
C19B C21B 1.531(13) . ?
C19B C22B 1.543(13) . ?
C20B H20D 0.9800 . ?
C20B H20E 0.9800 . ?
C20B H20F 0.9800 . ?
C21B H21D 0.9800 . ?
C21B H21E 0.9800 . ?
C21B H21F 0.9800 . ?
C22B H22D 0.9800 . ?
C22B H22E 0.9800 . ?
C22B H22F 0.9800 . ?
C23B C25B 1.521(12) . ?
C23B C24B 1.529(14) . ?
C23B C26B 1.543(12) . ?
C24B H24D 0.9800 . ?
C24B H24E 0.9800 . ?
C24B H24F 0.9800 . ?
C25B H25D 0.9800 . ?
C25B H25E 0.9800 . ?
C25B H25F 0.9800 . ?
C26B H26D 0.9800 . ?
C26B H26E 0.9800 . ?
C26B H26F 0.9800 . ?
C27B C28B 1.365(12) . ?
C27B H27B 0.9500 . ?
C28B C29B 1.401(12) . ?
C28B H28B 0.9500 . ?
C29B C30B 1.498(12) . ?
C30B C32B 1.535(13) . ?
C30B C31B 1.545(13) . ?
C30B H30B 1.0000 . ?
C31B H31D 0.9800 . ?
C31B H31E 0.9800 . ?
C31B H31F 0.9800 . ?
C32B H32D 0.9800 . ?
C32B H32E 0.9800 . ?
C32B H32F 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 O2 C4 102.0(13) . . ?
C2 C1 O2 107.2(15) . . ?
C2 C1 H1C 110.3 . . ?
O2 C1 H1C 110.3 . . ?
C2 C1 H1D 110.3 . . ?
O2 C1 H1D 110.3 . . ?
H1C C1 H1D 108.5 . . ?
C1 C2 C3 107.6(16) . . ?
C1 C2 H2C 110.2 . . ?
C3 C2 H2C 110.2 . . ?
C1 C2 H2D 110.2 . . ?
C3 C2 H2D 110.2 . . ?
H2C C2 H2D 108.5 . . ?
C4 C3 C2 102.8(14) . . ?
C4 C3 H3C 111.2 . . ?
C2 C3 H3C 111.2 . . ?
C4 C3 H3D 111.2 . . ?
C2 C3 H3D 111.2 . . ?
H3C C3 H3D 109.1 . . ?
O2 C4 C3 106(2) . . ?
O2 C4 H4C 110.5 . . ?
C3 C4 H4C 110.5 . . ?
O2 C4 H4D 110.5 . . ?
C3 C4 H4D 110.5 . . ?
H4C C4 H4D 108.7 . . ?
C4C O2C C1C 99.7(11) . . ?
C2C C1C O2C 109.0(10) . . ?
C2C C1C H1CA 109.9 . . ?
O2C C1C H1CA 109.9 . . ?
C2C C1C H1CB 109.9 . . ?
O2C C1C H1CB 109.9 . . ?
H1CA C1C H1CB 108.3 . . ?
C3C C2C C1C 101.9(10) . . ?
C3C C2C H2CA 111.4 . . ?
C1C C2C H2CA 111.4 . . ?
C3C C2C H2CB 111.4 . . ?
C1C C2C H2CB 111.4 . . ?
H2CA C2C H2CB 109.3 . . ?
C2C C3C C4C 99.4(12) . . ?
C2C C3C H3CA 111.9 . . ?
C4C C3C H3CA 111.9 . . ?
C2C C3C H3CB 111.9 . . ?
C4C C3C H3CB 111.9 . . ?
H3CA C3C H3CB 109.6 . . ?
O2C C4C C3C 101.6(11) . . ?
O2C C4C H4CA 111.4 . . ?
C3C C4C H4CA 111.4 . . ?
O2C C4C H4CB 111.4 . . ?
C3C C4C H4CB 111.4 . . ?
H4CA C4C H4CB 109.3 . . ?
V1B O1 V1A 149.0(4) . . ?
O1A V1A O1 130.2(9) . . ?
O1A V1A N3A 112.9(9) . . ?
O1 V1A N3A 116.9(3) . . ?
O1A V1A N1A 88.5(9) . . ?
O1 V1A N1A 96.0(3) . . ?
N3A V1A N1A 87.6(3) . . ?
O1A V1A N5A 90.1(9) . . ?
O1 V1A N5A 89.3(3) . . ?
N3A V1A N5A 87.7(3) . . ?
N1A V1A N5A 174.1(3) . . ?
O1 V1A Cl1A 121.2(3) . . ?
N3A V1A Cl1A 121.9(3) . . ?
N1A V1A Cl1A 86.2(3) . . ?
N5A V1A Cl1A 93.3(3) . . ?
C3A N1A N2A 103.9(8) . . ?
C3A N1A V1A 126.9(6) . . ?
N2A N1A V1A 125.4(6) . . ?
C1A N2A N1A 110.9(8) . . ?
C1A N2A C8A 126.5(8) . . ?
N1A N2A C8A 122.0(8) . . ?
C18A N3A C7A 103.2(7) . . ?
C18A N3A V1A 127.8(6) . . ?
C7A N3A V1A 129.0(6) . . ?
C27A N4A N5A 110.7(8) . . ?
C27A N4A C17A 125.3(9) . . ?
N5A N4A C17A 123.2(7) . . ?
C29A N5A N4A 105.6(8) . . ?
C29A N5A V1A 126.1(7) . . ?
N4A N5A V1A 123.8(6) . . ?
N2A C1A C2A 108.2(9) . . ?
N2A C1A H1A 125.9 . . ?
C2A C1A H1A 125.9 . . ?
C1A C2A C3A 105.1(9) . . ?
C1A C2A H2A 127.5 . . ?
C3A C2A H2A 127.5 . . ?
N1A C3A C2A 112.0(9) . . ?
N1A C3A C4A 122.3(9) . . ?
C2A C3A C4A 125.7(10) . . ?
C5A C4A C3A 109.4(10) . . ?
C5A C4A C6A 113.5(11) . . ?
C3A C4A C6A 108.4(9) . . ?
C5A C4A H4A 108.5 . . ?
C3A C4A H4A 108.5 . . ?
C6A C4A H4A 108.5 . . ?
C4A C5A H5AA 109.5 . . ?
C4A C5A H5AB 109.5 . . ?
H5AA C5A H5AB 109.5 . . ?
C4A C5A H5AC 109.5 . . ?
H5AA C5A H5AC 109.5 . . ?
H5AB C5A H5AC 109.5 . . ?
C4A C6A H6AA 109.5 . . ?
C4A C6A H6AB 109.5 . . ?
H6AA C6A H6AB 109.5 . . ?
C4A C6A H6AC 109.5 . . ?
H6AA C6A H6AC 109.5 . . ?
H6AB C6A H6AC 109.5 . . ?
C8A C7A C12A 118.2(9) . . ?
C8A C7A N3A 128.2(9) . . ?
C12A C7A N3A 113.7(9) . . ?
C7A C8A C9A 118.7(9) . . ?
C7A C8A N2A 122.4(9) . . ?
C9A C8A N2A 118.9(9) . . ?
C10A C9A C8A 121.7(10) . . ?
C10A C9A H9A 119.2 . . ?
C8A C9A H9A 119.2 . . ?
C9A C10A C11A 119.6(9) . . ?
C9A C10A C19A 118.8(9) . . ?
C11A C10A C19A 121.3(9) . . ?
C12A C11A C10A 119.0(9) . . ?
C12A C11A H11A 120.5 . . ?
C10A C11A H11A 120.5 . . ?
C11A C12A C7A 122.1(10) . . ?
C11A C12A C13A 132.9(9) . . ?
C7A C12A C13A 104.8(8) . . ?
C14A C13A C18A 123.1(9) . . ?
C14A C13A C12A 132.0(9) . . ?
C18A C13A C12A 104.9(9) . . ?
C13A C14A C15A 120.3(9) . . ?
C13A C14A H14A 119.9 . . ?
C15A C14A H14A 119.9 . . ?
C14A C15A C16A 117.6(10) . . ?
C14A C15A C23A 120.3(9) . . ?
C16A C15A C23A 122.1(9) . . ?
C17A C16A C15A 122.7(9) . . ?
C17A C16A H16A 118.7 . . ?
C15A C16A H16A 118.7 . . ?
C16A C17A C18A 119.8(9) . . ?
C16A C17A N4A 119.7(8) . . ?
C18A C17A N4A 120.4(9) . . ?
N3A C18A C17A 130.4(8) . . ?
N3A C18A C13A 113.4(8) . . ?
C17A C18A C13A 116.2(9) . . ?
C21A C19A C20A 109.6(11) . . ?
C21A C19A C22A 107.8(10) . . ?
C20A C19A C22A 109.8(11) . . ?
C21A C19A C10A 111.6(9) . . ?
C20A C19A C10A 106.3(9) . . ?
C22A C19A C10A 111.8(9) . . ?
C19A C20A H20A 109.5 . . ?
C19A C20A H20B 109.5 . . ?
H20A C20A H20B 109.5 . . ?
C19A C20A H20C 109.5 . . ?
H20A C20A H20C 109.5 . . ?
H20B C20A H20C 109.5 . . ?
C19A C21A H21A 109.5 . . ?
C19A C21A H21B 109.5 . . ?
H21A C21A H21B 109.5 . . ?
C19A C21A H21C 109.5 . . ?
H21A C21A H21C 109.5 . . ?
H21B C21A H21C 109.5 . . ?
C19A C22A H22A 109.5 . . ?
C19A C22A H22B 109.5 . . ?
H22A C22A H22B 109.5 . . ?
C19A C22A H22C 109.5 . . ?
H22A C22A H22C 109.5 . . ?
H22B C22A H22C 109.5 . . ?
C15A C23A C24A 109.4(9) . . ?
C15A C23A C26A 112.1(8) . . ?
C24A C23A C26A 108.8(9) . . ?
C15A C23A C25A 109.5(9) . . ?
C24A C23A C25A 108.2(9) . . ?
C26A C23A C25A 108.7(9) . . ?
C23A C24A H24A 109.5 . . ?
C23A C24A H24B 109.5 . . ?
H24A C24A H24B 109.5 . . ?
C23A C24A H24C 109.5 . . ?
H24A C24A H24C 109.5 . . ?
H24B C24A H24C 109.5 . . ?
C23A C25A H25A 109.5 . . ?
C23A C25A H25B 109.5 . . ?
H25A C25A H25B 109.5 . . ?
C23A C25A H25C 109.5 . . ?
H25A C25A H25C 109.5 . . ?
H25B C25A H25C 109.5 . . ?
C23A C26A H26A 109.5 . . ?
C23A C26A H26B 109.5 . . ?
H26A C26A H26B 109.5 . . ?
C23A C26A H26C 109.5 . . ?
H26A C26A H26C 109.5 . . ?
H26B C26A H26C 109.5 . . ?
C28A C27A N4A 107.9(9) . . ?
C28A C27A H27A 126.1 . . ?
N4A C27A H27A 126.1 . . ?
C27A C28A C29A 106.6(9) . . ?
C27A C28A H28A 126.7 . . ?
C29A C28A H28A 126.7 . . ?
N5A C29A C28A 109.1(9) . . ?
N5A C29A C30A 122.2(9) . . ?
C28A C29A C30A 128.6(9) . . ?
C29A C30A C32A 109.1(9) . . ?
C29A C30A C31A 111.7(9) . . ?
C32A C30A C31A 108.5(9) . . ?
C29A C30A H30A 109.2 . . ?
C32A C30A H30A 109.2 . . ?
C31A C30A H30A 109.2 . . ?
C30A C31A H31A 109.5 . . ?
C30A C31A H31B 109.5 . . ?
H31A C31A H31B 109.5 . . ?
C30A C31A H31C 109.5 . . ?
H31A C31A H31C 109.5 . . ?
H31B C31A H31C 109.5 . . ?
C30A C32A H32A 109.5 . . ?
C30A C32A H32B 109.5 . . ?
H32A C32A H32B 109.5 . . ?
C30A C32A H32C 109.5 . . ?
H32A C32A H32C 109.5 . . ?
H32B C32A H32C 109.5 . . ?
O1B V1B O1 126.6(12) . . ?
O1B V1B N3B 113.1(12) . . ?
O1 V1B N3B 120.1(3) . . ?
O1B V1B N5B 83.9(12) . . ?
O1 V1B N5B 94.4(3) . . ?
N3B V1B N5B 87.2(3) . . ?
O1B V1B N1B 96.4(12) . . ?
O1 V1B N1B 90.0(3) . . ?
N3B V1B N1B 87.4(3) . . ?
N5B V1B N1B 174.3(3) . . ?
O1 V1B Cl1B 119.4(4) . . ?
N3B V1B Cl1B 120.4(4) . . ?
N5B V1B Cl1B 90.4(4) . . ?
N1B V1B Cl1B 90.6(4) . . ?
C3B N1B N2B 107.5(8) . . ?
C3B N1B V1B 124.4(7) . . ?
N2B N1B V1B 123.7(6) . . ?
C1B N2B N1B 110.3(8) . . ?
C1B N2B C8B 126.1(9) . . ?
N1B N2B C8B 123.1(8) . . ?
C7B N3B C18B 103.6(8) . . ?
C7B N3B V1B 127.7(6) . . ?
C18B N3B V1B 128.6(6) . . ?
C27B N4B C17B 126.2(8) . . ?
C27B N4B N5B 111.4(8) . . ?
C17B N4B N5B 121.8(7) . . ?
C29B N5B N4B 104.0(8) . . ?
C29B N5B V1B 125.7(7) . . ?
N4B N5B V1B 125.9(6) . . ?
N2B C1B C2B 106.0(9) . . ?
N2B C1B H1B 127.0 . . ?
C2B C1B H1B 127.0 . . ?
C1B C2B C3B 108.4(9) . . ?
C1B C2B H2B 125.8 . . ?
C3B C2B H2B 125.8 . . ?
N1B C3B C2B 107.6(10) . . ?
N1B C3B C4B 123.0(9) . . ?
C2B C3B C4B 129.3(9) . . ?
C3B C4B C5B 114.3(9) . . ?
C3B C4B C6B 109.7(9) . . ?
C5B C4B C6B 106.4(9) . . ?
C3B C4B H4B 108.8 . . ?
C5B C4B H4B 108.8 . . ?
C6B C4B H4B 108.8 . . ?
C4B C5B H5BA 109.5 . . ?
C4B C5B H5BB 109.5 . . ?
H5BA C5B H5BB 109.5 . . ?
C4B C5B H5BC 109.5 . . ?
H5BA C5B H5BC 109.5 . . ?
H5BB C5B H5BC 109.5 . . ?
C4B C6B H6BA 109.5 . . ?
C4B C6B H6BB 109.5 . . ?
H6BA C6B H6BB 109.5 . . ?
C4B C6B H6BC 109.5 . . ?
H6BA C6B H6BC 109.5 . . ?
H6BB C6B H6BC 109.5 . . ?
N3B C7B C8B 130.1(9) . . ?
N3B C7B C12B 111.9(8) . . ?
C8B C7B C12B 118.1(9) . . ?
C9B C8B C7B 118.7(10) . . ?
C9B C8B N2B 119.9(9) . . ?
C7B C8B N2B 121.4(9) . . ?
C8B C9B C10B 124.6(10) . . ?
C8B C9B H9B 117.7 . . ?
C10B C9B H9B 117.7 . . ?
C9B C10B C11B 116.3(10) . . ?
C9B C10B C19B 124.6(9) . . ?
C11B C10B C19B 119.1(9) . . ?
C12B C11B C10B 120.9(10) . . ?
C12B C11B H11B 119.5 . . ?
C10B C11B H11B 119.5 . . ?
C11B C12B C13B 132.8(10) . . ?
C11B C12B C7B 121.0(9) . . ?
C13B C12B C7B 106.1(9) . . ?
C14B C13B C18B 121.3(9) . . ?
C14B C13B C12B 133.1(10) . . ?
C18B C13B C12B 105.5(8) . . ?
C15B C14B C13B 119.8(9) . . ?
C15B C14B H14B 120.1 . . ?
C13B C14B H14B 120.1 . . ?
C16B C15B C14B 117.7(9) . . ?
C16B C15B C23B 120.4(9) . . ?
C14B C15B C23B 121.8(9) . . ?
C17B C16B C15B 125.0(9) . . ?
C17B C16B H16B 117.5 . . ?
C15B C16B H16B 117.5 . . ?
C16B C17B N4B 121.2(9) . . ?
C16B C17B C18B 116.6(9) . . ?
N4B C17B C18B 122.1(9) . . ?
N3B C18B C13B 112.6(8) . . ?
N3B C18B C17B 128.3(9) . . ?
C13B C18B C17B 119.0(9) . . ?
C20B C19B C10B 112.3(9) . . ?
C20B C19B C21B 108.4(9) . . ?
C10B C19B C21B 112.6(10) . . ?
C20B C19B C22B 107.4(9) . . ?
C10B C19B C22B 108.7(8) . . ?
C21B C19B C22B 107.0(9) . . ?
C19B C20B H20D 109.5 . . ?
C19B C20B H20E 109.5 . . ?
H20D C20B H20E 109.5 . . ?
C19B C20B H20F 109.5 . . ?
H20D C20B H20F 109.5 . . ?
H20E C20B H20F 109.5 . . ?
C19B C21B H21D 109.5 . . ?
C19B C21B H21E 109.5 . . ?
H21D C21B H21E 109.5 . . ?
C19B C21B H21F 109.5 . . ?
H21D C21B H21F 109.5 . . ?
H21E C21B H21F 109.5 . . ?
C19B C22B H22D 109.5 . . ?
C19B C22B H22E 109.5 . . ?
H22D C22B H22E 109.5 . . ?
C19B C22B H22F 109.5 . . ?
H22D C22B H22F 109.5 . . ?
H22E C22B H22F 109.5 . . ?
C25B C23B C15B 112.6(8) . . ?
C25B C23B C24B 107.8(9) . . ?
C15B C23B C24B 108.0(8) . . ?
C25B C23B C26B 108.5(8) . . ?
C15B C23B C26B 111.3(9) . . ?
C24B C23B C26B 108.5(9) . . ?
C23B C24B H24D 109.5 . . ?
C23B C24B H24E 109.5 . . ?
H24D C24B H24E 109.5 . . ?
C23B C24B H24F 109.5 . . ?
H24D C24B H24F 109.5 . . ?
H24E C24B H24F 109.5 . . ?
C23B C25B H25D 109.5 . . ?
C23B C25B H25E 109.5 . . ?
H25D C25B H25E 109.5 . . ?
C23B C25B H25F 109.5 . . ?
H25D C25B H25F 109.5 . . ?
H25E C25B H25F 109.5 . . ?
C23B C26B H26D 109.5 . . ?
C23B C26B H26E 109.5 . . ?
H26D C26B H26E 109.5 . . ?
C23B C26B H26F 109.5 . . ?
H26D C26B H26F 109.5 . . ?
H26E C26B H26F 109.5 . . ?
N4B C27B C28B 107.5(9) . . ?
N4B C27B H27B 126.3 . . ?
C28B C27B H27B 126.3 . . ?
C27B C28B C29B 106.4(9) . . ?
C27B C28B H28B 126.8 . . ?
C29B C28B H28B 126.8 . . ?
N5B C29B C28B 110.7(9) . . ?
N5B C29B C30B 122.3(9) . . ?
C28B C29B C30B 127.1(10) . . ?
C29B C30B C32B 109.7(9) . . ?
C29B C30B C31B 108.1(9) . . ?
C32B C30B C31B 112.5(9) . . ?
C29B C30B H30B 108.8 . . ?
C32B C30B H30B 108.8 . . ?
C31B C30B H30B 108.8 . . ?
C30B C31B H31D 109.5 . . ?
C30B C31B H31E 109.5 . . ?
H31D C31B H31E 109.5 . . ?
C30B C31B H31F 109.5 . . ?
H31D C31B H31F 109.5 . . ?
H31E C31B H31F 109.5 . . ?
C30B C32B H32D 109.5 . . ?
C30B C32B H32E 109.5 . . ?
H32D C32B H32E 109.5 . . ?
C30B C32B H32F 109.5 . . ?
H32D C32B H32F 109.5 . . ?
H32E C32B H32F 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
C4 O2 C1 C2 -26(3) . . . . ?
O2 C1 C2 C3 5(4) . . . . ?
C1 C2 C3 C4 18(5) . . . . ?
C1 O2 C4 C3 38(4) . . . . ?
C2 C3 C4 O2 -35(4) . . . . ?
C4C O2C C1C C2C 18(3) . . . . ?
O2C C1C C2C C3C 14(3) . . . . ?
C1C C2C C3C C4C -41(3) . . . . ?
C1C O2C C4C C3C -44(2) . . . . ?
C2C C3C C4C O2C 54(3) . . . . ?
V1B O1 V1A O1A -139.6(13) . . . . ?
V1B O1 V1A N3A 37.0(8) . . . . ?
V1B O1 V1A N1A 127.3(7) . . . . ?
V1B O1 V1A N5A -50.1(7) . . . . ?
V1B O1 V1A Cl1A -143.5(7) . . . . ?
C3A N1A N2A C1A 1.1(11) . . . . ?
V1A N1A N2A C1A -158.0(7) . . . . ?
C3A N1A N2A C8A -171.0(9) . . . . ?
V1A N1A N2A C8A 30.0(13) . . . . ?
C27A N4A N5A C29A 1.8(11) . . . . ?
C17A N4A N5A C29A -168.4(9) . . . . ?
C27A N4A N5A V1A -155.6(7) . . . . ?
C17A N4A N5A V1A 34.2(12) . . . . ?
N1A N2A C1A C2A -1.4(12) . . . . ?
C8A N2A C1A C2A 170.2(10) . . . . ?
N2A C1A C2A C3A 1.1(13) . . . . ?
N2A N1A C3A C2A -0.3(12) . . . . ?
V1A N1A C3A C2A 158.3(7) . . . . ?
N2A N1A C3A C4A 178.9(10) . . . . ?
V1A N1A C3A C4A -22.5(15) . . . . ?
C1A C2A C3A N1A -0.5(13) . . . . ?
C1A C2A C3A C4A -179.7(11) . . . . ?
N1A C3A C4A C5A 119.5(12) . . . . ?
C2A C3A C4A C5A -61.4(15) . . . . ?
N1A C3A C4A C6A -116.3(12) . . . . ?
C2A C3A C4A C6A 62.8(15) . . . . ?
C18A N3A C7A C8A -178.8(10) . . . . ?
V1A N3A C7A C8A 5.0(16) . . . . ?
C18A N3A C7A C12A 0.7(11) . . . . ?
V1A N3A C7A C12A -175.5(7) . . . . ?
C12A C7A C8A C9A 10.0(15) . . . . ?
N3A C7A C8A C9A -170.6(10) . . . . ?
C12A C7A C8A N2A -173.0(9) . . . . ?
N3A C7A C8A N2A 6.5(17) . . . . ?
C1A N2A C8A C7A 164.6(10) . . . . ?
N1A N2A C8A C7A -24.7(15) . . . . ?
C1A N2A C8A C9A -18.4(15) . . . . ?
N1A N2A C8A C9A 152.3(9) . . . . ?
C7A C8A C9A C10A -5.6(15) . . . . ?
N2A C8A C9A C10A 177.2(9) . . . . ?
C8A C9A C10A C11A -2.1(16) . . . . ?
C8A C9A C10A C19A 172.1(9) . . . . ?
C9A C10A C11A C12A 5.1(15) . . . . ?
C19A C10A C11A C12A -168.9(9) . . . . ?
C10A C11A C12A C7A -0.4(16) . . . . ?
C10A C11A C12A C13A 174.1(10) . . . . ?
C8A C7A C12A C11A -7.2(16) . . . . ?
N3A C7A C12A C11A 173.3(9) . . . . ?
C8A C7A C12A C13A 177.0(9) . . . . ?
N3A C7A C12A C13A -2.6(12) . . . . ?
C11A C12A C13A C14A 9(2) . . . . ?
C7A C12A C13A C14A -176.0(11) . . . . ?
C11A C12A C13A C18A -171.9(11) . . . . ?
C7A C12A C13A C18A 3.3(11) . . . . ?
C18A C13A C14A C15A 1.3(16) . . . . ?
C12A C13A C14A C15A -179.6(10) . . . . ?
C13A C14A C15A C16A 2.9(16) . . . . ?
C13A C14A C15A C23A -175.8(10) . . . . ?
C14A C15A C16A C17A -2.1(16) . . . . ?
C23A C15A C16A C17A 176.6(10) . . . . ?
C15A C16A C17A C18A -3.0(16) . . . . ?
C15A C16A C17A N4A 178.5(9) . . . . ?
C27A N4A C17A C16A -11.8(16) . . . . ?
N5A N4A C17A C16A 156.9(9) . . . . ?
C27A N4A C17A C18A 169.7(10) . . . . ?
N5A N4A C17A C18A -21.5(15) . . . . ?
C7A N3A C18A C17A -175.6(10) . . . . ?
V1A N3A C18A C17A 0.6(16) . . . . ?
C7A N3A C18A C13A 1.7(11) . . . . ?
V1A N3A C18A C13A 177.9(7) . . . . ?
C16A C17A C18A N3A -175.9(10) . . . . ?
N4A C17A C18A N3A 2.6(17) . . . . ?
C16A C17A C18A C13A 6.9(15) . . . . ?
N4A C17A C18A C13A -174.7(9) . . . . ?
C14A C13A C18A N3A 176.1(9) . . . . ?
C12A C13A C18A N3A -3.2(12) . . . . ?
C14A C13A C18A C17A -6.2(15) . . . . ?
C12A C13A C18A C17A 174.4(9) . . . . ?
C9A C10A C19A C21A 46.3(14) . . . . ?
C11A C10A C19A C21A -139.6(11) . . . . ?
C9A C10A C19A C20A -73.1(13) . . . . ?
C11A C10A C19A C20A 101.0(12) . . . . ?
C9A C10A C19A C22A 167.1(10) . . . . ?
C11A C10A C19A C22A -18.8(15) . . . . ?
C14A C15A C23A C24A -54.6(13) . . . . ?
C16A C15A C23A C24A 126.7(10) . . . . ?
C14A C15A C23A C26A -175.4(10) . . . . ?
C16A C15A C23A C26A 5.9(15) . . . . ?
C14A C15A C23A C25A 63.9(12) . . . . ?
C16A C15A C23A C25A -114.8(11) . . . . ?
N5A N4A C27A C28A -1.4(12) . . . . ?
C17A N4A C27A C28A 168.6(9) . . . . ?
N4A C27A C28A C29A 0.3(12) . . . . ?
N4A N5A C29A C28A -1.6(11) . . . . ?
V1A N5A C29A C28A 155.2(7) . . . . ?
N4A N5A C29A C30A 173.5(9) . . . . ?
V1A N5A C29A C30A -29.7(14) . . . . ?
C27A C28A C29A N5A 0.8(12) . . . . ?
C27A C28A C29A C30A -173.9(11) . . . . ?
N5A C29A C30A C32A -84.7(12) . . . . ?
C28A C29A C30A C32A 89.4(13) . . . . ?
N5A C29A C30A C31A 155.5(9) . . . . ?
C28A C29A C30A C31A -30.5(16) . . . . ?
V1A O1 V1B O1B -154.3(15) . . . . ?
V1A O1 V1B N3B 30.6(8) . . . . ?
V1A O1 V1B N5B 119.9(7) . . . . ?
V1A O1 V1B N1B -56.4(7) . . . . ?
V1A O1 V1B Cl1B -147.1(7) . . . . ?
C3B N1B N2B C1B 3.6(12) . . . . ?
V1B N1B N2B C1B -153.7(7) . . . . ?
C3B N1B N2B C8B -169.2(9) . . . . ?
V1B N1B N2B C8B 33.6(13) . . . . ?
C27B N4B N5B C29B 0.7(11) . . . . ?
C17B N4B N5B C29B -170.6(9) . . . . ?
C27B N4B N5B V1B -156.7(7) . . . . ?
C17B N4B N5B V1B 32.0(12) . . . . ?
N1B N2B C1B C2B -2.9(12) . . . . ?
C8B N2B C1B C2B 169.7(10) . . . . ?
N2B C1B C2B C3B 1.1(12) . . . . ?
N2B N1B C3B C2B -2.8(12) . . . . ?
V1B N1B C3B C2B 154.3(7) . . . . ?
N2B N1B C3B C4B 172.8(9) . . . . ?
V1B N1B C3B C4B -30.1(14) . . . . ?
C1B C2B C3B N1B 1.1(13) . . . . ?
C1B C2B C3B C4B -174.2(11) . . . . ?
N1B C3B C4B C5B 157.3(10) . . . . ?
C2B C3B C4B C5B -28.1(17) . . . . ?
N1B C3B C4B C6B -83.3(12) . . . . ?
C2B C3B C4B C6B 91.3(13) . . . . ?
C18B N3B C7B C8B -179.3(11) . . . . ?
V1B N3B C7B C8B -0.6(16) . . . . ?
C18B N3B C7B C12B 1.2(11) . . . . ?
V1B N3B C7B C12B 179.8(7) . . . . ?
N3B C7B C8B C9B -174.3(10) . . . . ?
C12B C7B C8B C9B 5.2(15) . . . . ?
N3B C7B C8B N2B 6.4(18) . . . . ?
C12B C7B C8B N2B -174.1(9) . . . . ?
C1B N2B C8B C9B -15.2(16) . . . . ?
N1B N2B C8B C9B 156.4(10) . . . . ?
C1B N2B C8B C7B 164.1(10) . . . . ?
N1B N2B C8B C7B -24.3(15) . . . . ?
C7B C8B C9B C10B 0.0(17) . . . . ?
N2B C8B C9B C10B 179.3(9) . . . . ?
C8B C9B C10B C11B -5.4(16) . . . . ?
C8B C9B C10B C19B 172.9(11) . . . . ?
C9B C10B C11B C12B 5.6(15) . . . . ?
C19B C10B C11B C12B -172.8(10) . . . . ?
C10B C11B C12B C13B 177.5(11) . . . . ?
C10B C11B C12B C7B -0.7(16) . . . . ?
N3B C7B C12B C11B 174.7(9) . . . . ?
C8B C7B C12B C11B -4.9(16) . . . . ?
N3B C7B C12B C13B -3.9(12) . . . . ?
C8B C7B C12B C13B 176.5(9) . . . . ?
C11B C12B C13B C14B 9(2) . . . . ?
C7B C12B C13B C14B -172.3(11) . . . . ?
C11B C12B C13B C18B -173.5(12) . . . . ?
C7B C12B C13B C18B 4.8(11) . . . . ?
C18B C13B C14B C15B -1.5(15) . . . . ?
C12B C13B C14B C15B 175.2(10) . . . . ?
C13B C14B C15B C16B 6.3(14) . . . . ?
C13B C14B C15B C23B -169.7(9) . . . . ?
C14B C15B C16B C17B -5.8(16) . . . . ?
C23B C15B C16B C17B 170.4(10) . . . . ?
C15B C16B C17B N4B 178.3(9) . . . . ?
C15B C16B C17B C18B 0.0(16) . . . . ?
C27B N4B C17B C16B -14.6(16) . . . . ?
N5B N4B C17B C16B 155.4(9) . . . . ?
C27B N4B C17B C18B 163.6(10) . . . . ?
N5B N4B C17B C18B -26.4(15) . . . . ?
C7B N3B C18B C13B 2.1(11) . . . . ?
V1B N3B C18B C13B -176.5(7) . . . . ?
C7B N3B C18B C17B 179.1(10) . . . . ?
V1B N3B C18B C17B 0.5(15) . . . . ?
C14B C13B C18B N3B 173.1(9) . . . . ?
C12B C13B C18B N3B -4.4(12) . . . . ?
C14B C13B C18B C17B -4.3(15) . . . . ?
C12B C13B C18B C17B 178.2(9) . . . . ?
C16B C17B C18B N3B -172.0(9) . . . . ?
N4B C17B C18B N3B 9.7(17) . . . . ?
C16B C17B C18B C13B 4.9(14) . . . . ?
N4B C17B C18B C13B -173.3(9) . . . . ?
C9B C10B C19B C20B 4.5(16) . . . . ?
C11B C10B C19B C20B -177.2(9) . . . . ?
C9B C10B C19B C21B 127.3(11) . . . . ?
C11B C10B C19B C21B -54.4(13) . . . . ?
C9B C10B C19B C22B -114.2(11) . . . . ?
C11B C10B C19B C22B 64.0(13) . . . . ?
C16B C15B C23B C25B 171.5(9) . . . . ?
C14B C15B C23B C25B -12.5(14) . . . . ?
C16B C15B C23B C24B -69.6(12) . . . . ?
C14B C15B C23B C24B 106.3(11) . . . . ?
C16B C15B C23B C26B 49.4(13) . . . . ?
C14B C15B C23B C26B -134.6(10) . . . . ?
C17B N4B C27B C28B 170.3(10) . . . . ?
N5B N4B C27B C28B -0.5(12) . . . . ?
N4B C27B C28B C29B 0.0(13) . . . . ?
N4B N5B C29B C28B -0.7(12) . . . . ?
V1B N5B C29B C28B 156.8(7) . . . . ?
N4B N5B C29B C30B 179.1(9) . . . . ?
V1B N5B C29B C30B -23.4(15) . . . . ?
C27B C28B C29B N5B 0.4(13) . . . . ?
C27B C28B C29B C30B -179.4(11) . . . . ?
N5B C29B C30B C32B 120.8(11) . . . . ?
C28B C29B C30B C32B -59.4(15) . . . . ?
N5B C29B C30B C31B -116.2(11) . . . . ?
C28B C29B C30B C31B 63.6(14) . . . . ?

_refine_diff_density_max         1.511
_refine_diff_density_min         -0.902
_refine_diff_density_rms         0.100

####################################################################### 
# 
# 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_LUC_AL_II_025
_database_code_depnum_ccdc_archive 'CCDC 1906129'
loop_
_audit_author_name
_audit_author_address
'Matthias Zeller'
;Purdue University
United States of America
;
_audit_update_record             
;
2019-03-27 deposited with the CCDC.	2019-12-18 downloaded from the CCDC.
;
_chemical_name_systematic        ?
_chemical_name_common            AL_II_025
_chemical_formula_moiety         ?
_chemical_formula_sum            'C39 H48 N11 V'
_chemical_formula_iupac          ?
_chemical_formula_weight         721.82

_chemical_melting_point          ?

_space_group_crystal_system      monoclinic
_space_group_name_H-M_alt        'P 21/n'
_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                   15.0518(4)
_cell_length_b                   14.5044(4)
_cell_length_c                   17.2485(4)
_cell_angle_alpha                90
_cell_angle_beta                 92.868(2)
_cell_angle_gamma                90
_cell_volume                     3760.93(17)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    7141
_cell_measurement_theta_min      2.2460
_cell_measurement_theta_max      25.1887
_cell_measurement_temperature    120.(2)

_exptl_crystal_description       plate
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.290
_exptl_crystal_size_mid          0.243
_exptl_crystal_size_min          0.072
_exptl_crystal_density_diffrn    1.275
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1528

_exptl_absorpt_coefficient_mu    0.308
_exptl_absorpt_correction_type   Multi-Scan
_exptl_absorpt_process_details   
;
SADABS V2016/2 - Bruker AXS area detector scaling and absorption correction
;
_exptl_absorpt_correction_T_min  0.87
_exptl_absorpt_correction_T_max  0.98

_exptl_special_details           
;
;

_diffrn_ambient_temperature      120.(2)

_diffrn_source                   'fine-focus tube'
_diffrn_source_type              ?

_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  graphite

_diffrn_measurement_device_type  'Bruker Kappa APEXII CCD'
_diffrn_measurement_method       'φ and ω scans'

_diffrn_detector_area_resol_mean 8.3333

_diffrn_reflns_number            39499
_diffrn_reflns_av_R_equivalents  0.0520
_diffrn_reflns_av_unetI/netI     0.0634
_diffrn_reflns_theta_min         1.75
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_full        28.28
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22

_refine_special_details          
;
;

_reflns_number_total             9303
_reflns_number_gt                6471
_reflns_threshold_expression     'I > 2σ(I)'

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_R_factor_all          0.0794
_refine_ls_R_factor_gt           0.0462
_refine_ls_wR_factor_gt          0.0982
_refine_ls_wR_factor_ref         0.1119
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_restrained_S_all      1.017
_refine_ls_number_reflns         9303
_refine_ls_number_parameters     471
_refine_ls_number_restraints     0
_refine_ls_number_constraints    ?
_refine_ls_hydrogen_treatment    constr
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0432P)²+1.8145P] where P=(Fo²+2Fc²)/3'

_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?

_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         0.397
_refine_diff_density_min         -0.433
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?

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'
V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_computing_data_collection       'Bruker Instrument Service v2012.12.0.3'
_computing_cell_refinement       'SAINT V8.38A (Bruker AXS Inc., 2017)'
_computing_data_reduction        'SAINT V8.38A (Bruker AXS Inc., 2017)'
_computing_structure_solution    'SHELXT, VERSION 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_refinement_flags_posn
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
V V1 0.40388(2) 0.52953(2) 0.26965(2) 0.01217(9) Uani d . . . 1 . .
N N1 0.44689(11) 0.39143(11) 0.25913(9) 0.0140(3) Uani d . . . 1 . .
N N2 0.43110(11) 0.32148(11) 0.31040(9) 0.0143(3) Uani d . . . 1 . .
N N3 0.38017(10) 0.50622(11) 0.37561(9) 0.0131(3) Uani d . . . 1 . .
N N4 0.31884(11) 0.70345(10) 0.34562(9) 0.0141(3) Uani d . . . 1 . .
N N5 0.35372(10) 0.66543(11) 0.28071(8) 0.0135(3) Uani d . . . 1 . .
N N6 0.30655(11) 0.49689(11) 0.19382(9) 0.0180(4) Uani d . . . 1 . .
N N7 0.23856(12) 0.53340(12) 0.16861(9) 0.0187(4) Uani d . . . 1 . .
N N8 0.17327(13) 0.56300(14) 0.14256(11) 0.0327(5) Uani d . . . 1 . .
N N9 0.51957(11) 0.57858(11) 0.24722(9) 0.0176(4) Uani d . . . 1 . .
N N10 0.59602(13) 0.55377(12) 0.24496(10) 0.0216(4) Uani d . . . 1 . .
N N11 0.67028(14) 0.53608(15) 0.24288(13) 0.0391(5) Uani d . . . 1 . .
C C1 0.46153(13) 0.34940(14) 0.19117(11) 0.0159(4) Uani d . . . 1 . .
C C2 0.48417(14) 0.40133(14) 0.11937(11) 0.0191(4) Uani d . . . 1 . .
H H2 0.482807 0.468867 0.130905 0.023 Uiso calc U . R 1 . .
C C3 0.57797(15) 0.37550(17) 0.09667(13) 0.0306(5) Uani d . . . 1 . .
H H3A 0.620794 0.39053 0.13947 0.046 Uiso calc U . R 1 . .
H H3B 0.592746 0.410166 0.050279 0.046 Uiso calc U . R 1 . .
H H3C 0.580419 0.309277 0.085731 0.046 Uiso calc U . R 1 . .
C C4 0.41643(16) 0.38102(16) 0.05222(12) 0.0282(5) Uani d . . . 1 . .
H H4A 0.412582 0.314278 0.043847 0.042 Uiso calc U . R 1 . .
H H4B 0.43542 0.411007 0.004896 0.042 Uiso calc U . R 1 . .
H H4C 0.35799 0.404781 0.064971 0.042 Uiso calc U . R 1 . .
C C5 0.45432(14) 0.25411(14) 0.19919(11) 0.0199(4) Uani d . . . 1 . .
H H5 0.461782 0.20894 0.160169 0.024 Uiso calc U . R 1 . .
C C6 0.43439(14) 0.23880(14) 0.27442(11) 0.0192(4) Uani d . . . 1 . .
H H6 0.424563 0.180413 0.297442 0.023 Uiso calc U . R 1 . .
C C7 0.42006(12) 0.33819(13) 0.39060(10) 0.0131(4) Uani d . . . 1 . .
C C8 0.43015(13) 0.26627(13) 0.44357(11) 0.0152(4) Uani d . . . 1 . .
H H8 0.446838 0.207368 0.425097 0.018 Uiso calc U . R 1 . .
C C9 0.41690(13) 0.27653(13) 0.52275(11) 0.0154(4) Uani d . . . 1 . .
C C10 0.42144(14) 0.19124(13) 0.57650(11) 0.0180(4) Uani d . . . 1 . .
C C11 0.49792(19) 0.12741(18) 0.55639(16) 0.0445(7) Uani d . . . 1 . .
H H11A 0.486401 0.102242 0.504125 0.067 Uiso calc U . R 1 . .
H H11B 0.502605 0.076774 0.593997 0.067 Uiso calc U . R 1 . .
H H11C 0.55372 0.162329 0.55818 0.067 Uiso calc U . R 1 . .
C C12 0.33451(18) 0.13777(18) 0.56608(15) 0.0432(7) Uani d . . . 1 . .
H H12A 0.284885 0.177437 0.579565 0.065 Uiso calc U . R 1 . .
H H12B 0.336797 0.083577 0.600047 0.065 Uiso calc U . R 1 . .
H H12C 0.325939 0.117918 0.51191 0.065 Uiso calc U . R 1 . .
C C13 0.43585(19) 0.21783(16) 0.66092(13) 0.0384(6) Uani d . . . 1 . .
H H13A 0.489287 0.256198 0.667464 0.058 Uiso calc U . R 1 . .
H H13B 0.443385 0.162021 0.692591 0.058 Uiso calc U . R 1 . .
H H13C 0.38421 0.25251 0.67743 0.058 Uiso calc U . R 1 . .
C C14 0.39552(13) 0.36409(13) 0.54951(11) 0.0159(4) Uani d . . . 1 . .
H H14 0.387501 0.373815 0.603177 0.019 Uiso calc U . R 1 . .
C C15 0.38595(13) 0.43720(13) 0.49755(10) 0.0141(4) Uani d . . . 1 . .
C C16 0.39709(12) 0.42478(13) 0.41773(10) 0.0131(4) Uani d . . . 1 . .
C C17 0.35604(12) 0.57086(13) 0.43108(10) 0.0135(4) Uani d . . . 1 . .
C C18 0.36063(13) 0.53329(13) 0.50638(10) 0.0148(4) Uani d . . . 1 . .
C C19 0.34084(13) 0.58585(13) 0.57091(11) 0.0163(4) Uani d . . . 1 . .
H H19 0.345029 0.559391 0.621344 0.02 Uiso calc U . R 1 . .
C C20 0.31490(13) 0.67736(14) 0.56098(11) 0.0156(4) Uani d . . . 1 . .
C C21 0.28902(13) 0.73876(14) 0.62879(11) 0.0180(4) Uani d . . . 1 . .
C C22 0.31728(16) 0.69654(17) 0.70746(12) 0.0303(5) Uani d . . . 1 . .
H H22A 0.284616 0.63895 0.714569 0.045 Uiso calc U . R 1 . .
H H22B 0.304036 0.739844 0.748936 0.045 Uiso calc U . R 1 . .
H H22C 0.38128 0.683762 0.709274 0.045 Uiso calc U . R 1 . .
C C23 0.18849(15) 0.75031(18) 0.62487(13) 0.0318(6) Uani d . . . 1 . .
H H23A 0.169426 0.779237 0.575454 0.048 Uiso calc U . R 1 . .
H H23B 0.171074 0.789382 0.667903 0.048 Uiso calc U . R 1 . .
H H23C 0.160182 0.689746 0.628719 0.048 Uiso calc U . R 1 . .
C C24 0.33377(17) 0.83359(16) 0.62486(14) 0.0345(6) Uani d . . . 1 . .
H H24A 0.398518 0.825802 0.626678 0.052 Uiso calc U . R 1 . .
H H24B 0.317022 0.871147 0.669047 0.052 Uiso calc U . R 1 . .
H H24C 0.314359 0.864373 0.576353 0.052 Uiso calc U . R 1 . .
C C25 0.30837(13) 0.71294(13) 0.48543(11) 0.0156(4) Uani d . . . 1 . .
H H25 0.289489 0.774997 0.478319 0.019 Uiso calc U . R 1 . .
C C26 0.32814(13) 0.66190(13) 0.42046(10) 0.0141(4) Uani d . . . 1 . .
C C27 0.28334(14) 0.78693(14) 0.32771(11) 0.0183(4) Uani d . . . 1 . .
H H27 0.255063 0.826857 0.362516 0.022 Uiso calc U . R 1 . .
C C28 0.29509(13) 0.80395(14) 0.25109(11) 0.0175(4) Uani d . . . 1 . .
H H28 0.276763 0.857183 0.22246 0.021 Uiso calc U . R 1 . .
C C29 0.33953(12) 0.72715(13) 0.22336(10) 0.0138(4) Uani d . . . 1 . .
C C30 0.37222(13) 0.71366(13) 0.14316(10) 0.0153(4) Uani d . . . 1 . .
H H30 0.377975 0.645972 0.133585 0.018 Uiso calc U . R 1 . .
C C31 0.46371(13) 0.75810(15) 0.13616(12) 0.0218(5) Uani d . . . 1 . .
H H31A 0.458737 0.824971 0.142779 0.033 Uiso calc U . R 1 . .
H H31B 0.485694 0.74466 0.084834 0.033 Uiso calc U . R 1 . .
H H31C 0.505271 0.733105 0.176368 0.033 Uiso calc U . R 1 . .
C C32 0.30625(15) 0.75328(16) 0.08202(12) 0.0261(5) Uani d . . . 1 . .
H H32A 0.247738 0.725054 0.087494 0.039 Uiso calc U . R 1 . .
H H32B 0.326833 0.740132 0.030158 0.039 Uiso calc U . R 1 . .
H H32C 0.301754 0.820125 0.08911 0.039 Uiso calc U . R 1 . .
C C33 -0.15432(17) 0.58360(18) 0.39960(16) 0.0402(6) Uani d . . . 1 . .
H H33A -0.168098 0.647048 0.383587 0.06 Uiso calc U . R 1 . .
H H33B -0.165234 0.576192 0.454788 0.06 Uiso calc U . R 1 . .
H H33C -0.192226 0.540809 0.368936 0.06 Uiso calc U . R 1 . .
C C34 -0.05839(15) 0.56332(15) 0.38655(13) 0.0256(5) Uani d . . . 1 . .
C C35 -0.03308(16) 0.52443(15) 0.31699(13) 0.0277(5) Uani d . . . 1 . .
H H35 -0.077372 0.508901 0.27801 0.033 Uiso calc U . R 1 . .
C C36 0.05549(17) 0.50813(15) 0.30393(14) 0.0328(6) Uani d . . . 1 . .
H H36 0.07129 0.481701 0.25614 0.039 Uiso calc U . R 1 . .
C C37 0.12104(17) 0.52990(15) 0.35961(15) 0.0346(6) Uani d . . . 1 . .
H H37 0.181817 0.518956 0.350309 0.042 Uiso calc U . R 1 . .
C C38 0.09740(17) 0.56769(16) 0.42888(14) 0.0335(6) Uani d . . . 1 . .
H H38 0.142098 0.582496 0.467727 0.04 Uiso calc U . R 1 . .
C C39 0.00887(16) 0.58423(15) 0.44221(13) 0.0281(5) Uani d . . . 1 . .
H H39 -0.006325 0.610364 0.490285 0.034 Uiso calc U . R 1 . .


_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_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
V1 N3 . 1.9097(15) ?
V1 N9 . 1.9379(17) ?
V1 N6 . 1.9721(17) ?
V1 N1 . 2.1156(16) ?
V1 N5 . 2.1228(16) ?
N1 C1 . 1.349(2) ?
N1 N2 . 1.374(2) ?
N2 C6 . 1.352(2) ?
N2 C7 . 1.422(2) ?
N3 C17 . 1.400(2) ?
N3 C16 . 1.403(2) ?
N4 C27 . 1.353(2) ?
N4 N5 . 1.376(2) ?
N4 C26 . 1.425(2) ?
N5 C29 . 1.343(2) ?
N6 N7 . 1.213(2) ?
N7 N8 . 1.143(2) ?
N9 N10 . 1.208(2) ?
N10 N11 . 1.149(2) ?
C1 C5 . 1.394(3) ?
C1 C2 . 1.503(3) ?
C2 C3 . 1.530(3) ?
C2 C4 . 1.533(3) ?
C2 H2 . 1.0 ?
C3 H3A . 0.98 ?
C3 H3B . 0.98 ?
C3 H3C . 0.98 ?
C4 H4A . 0.98 ?
C4 H4B . 0.98 ?
C4 H4C . 0.98 ?
C5 C6 . 1.365(3) ?
C5 H5 . 0.95 ?
C6 H6 . 0.95 ?
C7 C16 . 1.390(3) ?
C7 C8 . 1.390(3) ?
C8 C9 . 1.398(3) ?
C8 H8 . 0.95 ?
C9 C14 . 1.395(3) ?
C9 C10 . 1.545(3) ?
C10 C13 . 1.511(3) ?
C10 C12 . 1.524(3) ?
C10 C11 . 1.531(3) ?
C11 H11A . 0.98 ?
C11 H11B . 0.98 ?
C11 H11C . 0.98 ?
C12 H12A . 0.98 ?
C12 H12B . 0.98 ?
C12 H12C . 0.98 ?
C13 H13A . 0.98 ?
C13 H13B . 0.98 ?
C13 H13C . 0.98 ?
C14 C15 . 1.391(3) ?
C14 H14 . 0.95 ?
C15 C16 . 1.407(2) ?
C15 C18 . 1.455(3) ?
C17 C26 . 1.395(3) ?
C17 C18 . 1.407(3) ?
C18 C19 . 1.394(3) ?
C19 C20 . 1.392(3) ?
C19 H19 . 0.95 ?
C20 C25 . 1.400(3) ?
C20 C21 . 1.536(3) ?
C21 C23 . 1.521(3) ?
C21 C22 . 1.529(3) ?
C21 C24 . 1.535(3) ?
C22 H22A . 0.98 ?
C22 H22B . 0.98 ?
C22 H22C . 0.98 ?
C23 H23A . 0.98 ?
C23 H23B . 0.98 ?
C23 H23C . 0.98 ?
C24 H24A . 0.98 ?
C24 H24B . 0.98 ?
C24 H24C . 0.98 ?
C25 C26 . 1.388(3) ?
C25 H25 . 0.95 ?
C27 C28 . 1.365(3) ?
C27 H27 . 0.95 ?
C28 C29 . 1.396(3) ?
C28 H28 . 0.95 ?
C29 C30 . 1.504(2) ?
C30 C32 . 1.524(3) ?
C30 C31 . 1.531(3) ?
C30 H30 . 1.0 ?
C31 H31A . 0.98 ?
C31 H31B . 0.98 ?
C31 H31C . 0.98 ?
C32 H32A . 0.98 ?
C32 H32B . 0.98 ?
C32 H32C . 0.98 ?
C33 C34 . 1.501(3) ?
C33 H33A . 0.98 ?
C33 H33B . 0.98 ?
C33 H33C . 0.98 ?
C34 C39 . 1.393(3) ?
C34 C35 . 1.396(3) ?
C35 C36 . 1.383(3) ?
C35 H35 . 0.95 ?
C36 C37 . 1.379(3) ?
C36 H36 . 0.95 ?
C37 C38 . 1.377(3) ?
C37 H37 . 0.95 ?
C38 C39 . 1.384(3) ?
C38 H38 . 0.95 ?
C39 H39 . 0.95 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
N3 V1 N9 . . 117.96(7) ?
N3 V1 N6 . . 115.09(7) ?
N9 V1 N6 . . 126.93(7) ?
N3 V1 N1 . . 89.26(6) ?
N9 V1 N1 . . 92.79(7) ?
N6 V1 N1 . . 86.34(7) ?
N3 V1 N5 . . 89.66(6) ?
N9 V1 N5 . . 90.24(7) ?
N6 V1 N5 . . 91.53(7) ?
N1 V1 N5 . . 176.95(6) ?
C1 N1 N2 . . 105.45(15) ?
C1 N1 V1 . . 124.50(13) ?
N2 N1 V1 . . 125.47(11) ?
C6 N2 N1 . . 110.36(15) ?
C6 N2 C7 . . 127.31(16) ?
N1 N2 C7 . . 122.17(15) ?
C17 N3 C16 . . 104.86(14) ?
C17 N3 V1 . . 127.05(13) ?
C16 N3 V1 . . 127.35(12) ?
C27 N4 N5 . . 109.60(15) ?
C27 N4 C26 . . 127.23(16) ?
N5 N4 C26 . . 122.92(15) ?
C29 N5 N4 . . 106.20(15) ?
C29 N5 V1 . . 126.65(12) ?
N4 N5 V1 . . 126.68(11) ?
N7 N6 V1 . . 135.90(14) ?
N8 N7 N6 . . 175.9(2) ?
N10 N9 V1 . . 139.81(15) ?
N11 N10 N9 . . 175.6(2) ?
N1 C1 C5 . . 110.18(17) ?
N1 C1 C2 . . 122.89(17) ?
C5 C1 C2 . . 126.92(17) ?
C1 C2 C3 . . 109.77(17) ?
C1 C2 C4 . . 110.89(17) ?
C3 C2 C4 . . 110.30(17) ?
C1 C2 H2 . . 108.6 ?
C3 C2 H2 . . 108.6 ?
C4 C2 H2 . . 108.6 ?
C2 C3 H3A . . 109.5 ?
C2 C3 H3B . . 109.5 ?
H3A C3 H3B . . 109.5 ?
C2 C3 H3C . . 109.5 ?
H3A C3 H3C . . 109.5 ?
H3B C3 H3C . . 109.5 ?
C2 C4 H4A . . 109.5 ?
C2 C4 H4B . . 109.5 ?
H4A C4 H4B . . 109.5 ?
C2 C4 H4C . . 109.5 ?
H4A C4 H4C . . 109.5 ?
H4B C4 H4C . . 109.5 ?
C6 C5 C1 . . 106.12(17) ?
C6 C5 H5 . . 126.9 ?
C1 C5 H5 . . 126.9 ?
N2 C6 C5 . . 107.87(17) ?
N2 C6 H6 . . 126.1 ?
C5 C6 H6 . . 126.1 ?
C16 C7 C8 . . 118.53(17) ?
C16 C7 N2 . . 121.64(16) ?
C8 C7 N2 . . 119.81(17) ?
C7 C8 C9 . . 123.09(18) ?
C7 C8 H8 . . 118.5 ?
C9 C8 H8 . . 118.5 ?
C14 C9 C8 . . 117.83(17) ?
C14 C9 C10 . . 122.30(17) ?
C8 C9 C10 . . 119.79(17) ?
C13 C10 C12 . . 108.94(19) ?
C13 C10 C11 . . 107.4(2) ?
C12 C10 C11 . . 108.5(2) ?
C13 C10 C9 . . 111.94(17) ?
C12 C10 C9 . . 108.94(17) ?
C11 C10 C9 . . 111.06(17) ?
C10 C11 H11A . . 109.5 ?
C10 C11 H11B . . 109.5 ?
H11A C11 H11B . . 109.5 ?
C10 C11 H11C . . 109.5 ?
H11A C11 H11C . . 109.5 ?
H11B C11 H11C . . 109.5 ?
C10 C12 H12A . . 109.5 ?
C10 C12 H12B . . 109.5 ?
H12A C12 H12B . . 109.5 ?
C10 C12 H12C . . 109.5 ?
H12A C12 H12C . . 109.5 ?
H12B C12 H12C . . 109.5 ?
C10 C13 H13A . . 109.5 ?
C10 C13 H13B . . 109.5 ?
H13A C13 H13B . . 109.5 ?
C10 C13 H13C . . 109.5 ?
H13A C13 H13C . . 109.5 ?
H13B C13 H13C . . 109.5 ?
C15 C14 C9 . . 119.94(17) ?
C15 C14 H14 . . 120.0 ?
C9 C14 H14 . . 120.0 ?
C14 C15 C16 . . 121.28(17) ?
C14 C15 C18 . . 133.00(17) ?
C16 C15 C18 . . 105.65(16) ?
C7 C16 N3 . . 128.90(17) ?
C7 C16 C15 . . 119.28(17) ?
N3 C16 C15 . . 111.80(16) ?
C26 C17 N3 . . 129.11(17) ?
C26 C17 C18 . . 119.24(16) ?
N3 C17 C18 . . 111.64(16) ?
C19 C18 C17 . . 121.52(18) ?
C19 C18 C15 . . 132.47(17) ?
C17 C18 C15 . . 105.99(16) ?
C20 C19 C18 . . 119.56(17) ?
C20 C19 H19 . . 120.2 ?
C18 C19 H19 . . 120.2 ?
C19 C20 C25 . . 118.18(17) ?
C19 C20 C21 . . 122.65(17) ?
C25 C20 C21 . . 119.10(17) ?
C23 C21 C22 . . 108.39(17) ?
C23 C21 C24 . . 109.72(19) ?
C22 C21 C24 . . 107.15(18) ?
C23 C21 C20 . . 108.65(17) ?
C22 C21 C20 . . 111.94(17) ?
C24 C21 C20 . . 110.94(16) ?
C21 C22 H22A . . 109.5 ?
C21 C22 H22B . . 109.5 ?
H22A C22 H22B . . 109.5 ?
C21 C22 H22C . . 109.5 ?
H22A C22 H22C . . 109.5 ?
H22B C22 H22C . . 109.5 ?
C21 C23 H23A . . 109.5 ?
C21 C23 H23B . . 109.5 ?
H23A C23 H23B . . 109.5 ?
C21 C23 H23C . . 109.5 ?
H23A C23 H23C . . 109.5 ?
H23B C23 H23C . . 109.5 ?
C21 C24 H24A . . 109.5 ?
C21 C24 H24B . . 109.5 ?
H24A C24 H24B . . 109.5 ?
C21 C24 H24C . . 109.5 ?
H24A C24 H24C . . 109.5 ?
H24B C24 H24C . . 109.5 ?
C26 C25 C20 . . 123.16(18) ?
C26 C25 H25 . . 118.4 ?
C20 C25 H25 . . 118.4 ?
C25 C26 C17 . . 118.31(17) ?
C25 C26 N4 . . 119.38(17) ?
C17 C26 N4 . . 122.31(16) ?
N4 C27 C28 . . 108.31(17) ?
N4 C27 H27 . . 125.8 ?
C28 C27 H27 . . 125.8 ?
C27 C28 C29 . . 105.96(17) ?
C27 C28 H28 . . 127.0 ?
C29 C28 H28 . . 127.0 ?
N5 C29 C28 . . 109.93(16) ?
N5 C29 C30 . . 122.90(17) ?
C28 C29 C30 . . 127.11(17) ?
C29 C30 C32 . . 110.82(16) ?
C29 C30 C31 . . 110.78(16) ?
C32 C30 C31 . . 110.13(16) ?
C29 C30 H30 . . 108.3 ?
C32 C30 H30 . . 108.3 ?
C31 C30 H30 . . 108.3 ?
C30 C31 H31A . . 109.5 ?
C30 C31 H31B . . 109.5 ?
H31A C31 H31B . . 109.5 ?
C30 C31 H31C . . 109.5 ?
H31A C31 H31C . . 109.5 ?
H31B C31 H31C . . 109.5 ?
C30 C32 H32A . . 109.5 ?
C30 C32 H32B . . 109.5 ?
H32A C32 H32B . . 109.5 ?
C30 C32 H32C . . 109.5 ?
H32A C32 H32C . . 109.5 ?
H32B C32 H32C . . 109.5 ?
C34 C33 H33A . . 109.5 ?
C34 C33 H33B . . 109.5 ?
H33A C33 H33B . . 109.5 ?
C34 C33 H33C . . 109.5 ?
H33A C33 H33C . . 109.5 ?
H33B C33 H33C . . 109.5 ?
C39 C34 C35 . . 117.4(2) ?
C39 C34 C33 . . 121.7(2) ?
C35 C34 C33 . . 120.9(2) ?
C36 C35 C34 . . 121.0(2) ?
C36 C35 H35 . . 119.5 ?
C34 C35 H35 . . 119.5 ?
C37 C36 C35 . . 120.6(2) ?
C37 C36 H36 . . 119.7 ?
C35 C36 H36 . . 119.7 ?
C38 C37 C36 . . 119.2(2) ?
C38 C37 H37 . . 120.4 ?
C36 C37 H37 . . 120.4 ?
C37 C38 C39 . . 120.4(2) ?
C37 C38 H38 . . 119.8 ?
C39 C38 H38 . . 119.8 ?
C38 C39 C34 . . 121.3(2) ?
C38 C39 H39 . . 119.3 ?
C34 C39 H39 . . 119.3 ?

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_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
C1 N1 N2 C6 . . . . -1.1(2) ?
V1 N1 N2 C6 . . . . 155.62(14) ?
C1 N1 N2 C7 . . . . 174.62(17) ?
V1 N1 N2 C7 . . . . -28.7(2) ?
C27 N4 N5 C29 . . . . 0.4(2) ?
C26 N4 N5 C29 . . . . -174.21(17) ?
C27 N4 N5 V1 . . . . -172.07(13) ?
C26 N4 N5 V1 . . . . 13.3(2) ?
N2 N1 C1 C5 . . . . 0.5(2) ?
V1 N1 C1 C5 . . . . -156.48(14) ?
N2 N1 C1 C2 . . . . -178.23(17) ?
V1 N1 C1 C2 . . . . 24.8(3) ?
N1 C1 C2 C3 . . . . 115.7(2) ?
C5 C1 C2 C3 . . . . -62.9(3) ?
N1 C1 C2 C4 . . . . -122.2(2) ?
C5 C1 C2 C4 . . . . 59.3(3) ?
N1 C1 C5 C6 . . . . 0.2(2) ?
C2 C1 C5 C6 . . . . 178.9(2) ?
N1 N2 C6 C5 . . . . 1.2(2) ?
C7 N2 C6 C5 . . . . -174.18(18) ?
C1 C5 C6 N2 . . . . -0.9(2) ?
C6 N2 C7 C16 . . . . -164.73(19) ?
N1 N2 C7 C16 . . . . 20.3(3) ?
C6 N2 C7 C8 . . . . 13.7(3) ?
N1 N2 C7 C8 . . . . -161.26(17) ?
C16 C7 C8 C9 . . . . 1.1(3) ?
N2 C7 C8 C9 . . . . -177.39(17) ?
C7 C8 C9 C14 . . . . -2.2(3) ?
C7 C8 C9 C10 . . . . 174.66(18) ?
C14 C9 C10 C13 . . . . -22.1(3) ?
C8 C9 C10 C13 . . . . 161.2(2) ?
C14 C9 C10 C12 . . . . 98.5(2) ?
C8 C9 C10 C12 . . . . -78.3(2) ?
C14 C9 C10 C11 . . . . -142.1(2) ?
C8 C9 C10 C11 . . . . 41.1(3) ?
C8 C9 C14 C15 . . . . 1.5(3) ?
C10 C9 C14 C15 . . . . -175.27(18) ?
C9 C14 C15 C16 . . . . 0.3(3) ?
C9 C14 C15 C18 . . . . 176.7(2) ?
C8 C7 C16 N3 . . . . -177.44(18) ?
N2 C7 C16 N3 . . . . 1.0(3) ?
C8 C7 C16 C15 . . . . 0.8(3) ?
N2 C7 C16 C15 . . . . 179.22(17) ?
C17 N3 C16 C7 . . . . 177.20(19) ?
V1 N3 C16 C7 . . . . -12.2(3) ?
C17 N3 C16 C15 . . . . -1.1(2) ?
V1 N3 C16 C15 . . . . 169.48(13) ?
C14 C15 C16 C7 . . . . -1.5(3) ?
C18 C15 C16 C7 . . . . -178.79(17) ?
C14 C15 C16 N3 . . . . 177.08(17) ?
C18 C15 C16 N3 . . . . -0.3(2) ?
C16 N3 C17 C26 . . . . -176.51(19) ?
V1 N3 C17 C26 . . . . 12.8(3) ?
C16 N3 C17 C18 . . . . 2.2(2) ?
V1 N3 C17 C18 . . . . -168.47(13) ?
C26 C17 C18 C19 . . . . -2.2(3) ?
N3 C17 C18 C19 . . . . 178.94(17) ?
C26 C17 C18 C15 . . . . 176.47(17) ?
N3 C17 C18 C15 . . . . -2.4(2) ?
C14 C15 C18 C19 . . . . 3.1(4) ?
C16 C15 C18 C19 . . . . -180.0(2) ?
C14 C15 C18 C17 . . . . -175.3(2) ?
C16 C15 C18 C17 . . . . 1.6(2) ?
C17 C18 C19 C20 . . . . 0.8(3) ?
C15 C18 C19 C20 . . . . -177.5(2) ?
C18 C19 C20 C25 . . . . 1.0(3) ?
C18 C19 C20 C21 . . . . 177.91(18) ?
C19 C20 C21 C23 . . . . -105.3(2) ?
C25 C20 C21 C23 . . . . 71.6(2) ?
C19 C20 C21 C22 . . . . 14.4(3) ?
C25 C20 C21 C22 . . . . -168.70(18) ?
C19 C20 C21 C24 . . . . 134.0(2) ?
C25 C20 C21 C24 . . . . -49.1(3) ?
C19 C20 C25 C26 . . . . -1.3(3) ?
C21 C20 C25 C26 . . . . -178.35(18) ?
C20 C25 C26 C17 . . . . -0.1(3) ?
C20 C25 C26 N4 . . . . 179.43(17) ?
N3 C17 C26 C25 . . . . -179.51(19) ?
C18 C17 C26 C25 . . . . 1.9(3) ?
N3 C17 C26 N4 . . . . 0.9(3) ?
C18 C17 C26 N4 . . . . -177.70(17) ?
C27 N4 C26 C25 . . . . -7.4(3) ?
N5 N4 C26 C25 . . . . 166.27(17) ?
C27 N4 C26 C17 . . . . 172.14(19) ?
N5 N4 C26 C17 . . . . -14.2(3) ?
N5 N4 C27 C28 . . . . -0.2(2) ?
C26 N4 C27 C28 . . . . 174.19(18) ?
N4 C27 C28 C29 . . . . -0.2(2) ?
N4 N5 C29 C28 . . . . -0.5(2) ?
V1 N5 C29 C28 . . . . 171.98(13) ?
N4 N5 C29 C30 . . . . 176.78(17) ?
V1 N5 C29 C30 . . . . -10.7(3) ?
C27 C28 C29 N5 . . . . 0.4(2) ?
C27 C28 C29 C30 . . . . -176.75(19) ?
N5 C29 C30 C32 . . . . 144.85(19) ?
C28 C29 C30 C32 . . . . -38.3(3) ?
N5 C29 C30 C31 . . . . -92.6(2) ?
C28 C29 C30 C31 . . . . 84.3(2) ?
C39 C34 C35 C36 . . . . -0.5(3) ?
C33 C34 C35 C36 . . . . 178.1(2) ?
C34 C35 C36 C37 . . . . 0.1(3) ?
C35 C36 C37 C38 . . . . 0.4(3) ?
C36 C37 C38 C39 . . . . -0.5(3) ?
C37 C38 C39 C34 . . . . 0.0(3) ?
C35 C34 C39 C38 . . . . 0.4(3) ?
C33 C34 C39 C38 . . . . -178.2(2) ?

####################################################################### 
# 
# 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_JG-V
_database_code_depnum_ccdc_archive 'CCDC 1906130'
loop_
_audit_author_name
_audit_author_address
'Matthias Zeller'
;Purdue University
United States of America
;
_audit_update_record             
;
2019-03-27 deposited with the CCDC.	2019-12-18 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C32 H40 Cl2 N5 V, C7 H8'
_chemical_formula_sum            'C39 H48 Cl2 N5 V'
_chemical_formula_weight         708.66

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'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
V V 0.0687 2.1097 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      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                   11.5972(2)
_cell_length_b                   14.7064(3)
_cell_length_c                   21.9685(5)
_cell_angle_alpha                90
_cell_angle_beta                 95.6135(16)
_cell_angle_gamma                90
_cell_volume                     3728.83(13)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    54489
_cell_measurement_theta_min      6.091
_cell_measurement_theta_max      72.256

_exptl_crystal_description       plate
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.262
_exptl_crystal_F_000             1496
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.220
_exptl_crystal_size_mid          0.210
_exptl_crystal_size_min          0.160
_exptl_absorpt_coefficient_mu    3.796
_shelx_estimated_absorpt_T_min   0.489
_shelx_estimated_absorpt_T_max   0.582
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.441
_exptl_absorpt_correction_T_max  0.582
_exptl_absorpt_process_details   'SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_source                   'microfocus X-ray tube'
_diffrn_radiation_monochromator  'laterally graded multilayer (Goebel) mirror'
_diffrn_measurement_device_type  
'Rigaku Rapid II curved image plate diffractometer'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            54489
_diffrn_reflns_av_unetI/netI     0.0182
_diffrn_reflns_av_R_equivalents  0.0372
_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       -26
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         6.091
_diffrn_reflns_theta_max         72.256
_diffrn_reflns_theta_full        67.679
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measured_fraction_theta_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_point_group_measured_fraction_full 0.995
_reflns_number_total             7200
_reflns_number_gt                6843
_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       'CrystalClear-SM Expert 2.1 b32 (Rigaku, 2014)'
_computing_cell_refinement       'HKL3000 (Otwinowski & Minor, 1997)'
_computing_data_reduction        'HKL3000 (Otwinowski & Minor, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  
;  
SHELXL-2014/7 (Sheldrick, 2014), 
SHELXLE Rev714 (Hübschle et al., 2011)
;
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          
;
A toluene molecule is disordered with two alternative orientations. 
The two moieties were restrained to have similar geometries, and Uij 
components of ADPs were restrained to be similar for atoms closer than 
2.0 Angstrom. Subject to these conditions the occupancy ratio refined 
to 0.852(5) to 0.148(5).
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0481P)²+2.7433P] 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     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_extinction_coef       0.00115(12)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         7200
_refine_ls_number_parameters     501
_refine_ls_number_restraints     219
_refine_ls_R_factor_all          0.0380
_refine_ls_R_factor_gt           0.0361
_refine_ls_wR_factor_ref         0.0958
_refine_ls_wR_factor_gt          0.0943
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_restrained_S_all      1.052
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.35876(15) 0.24717(12) 0.18837(8) 0.0202(3) Uani 1 1 d . . . . .
C2 C 0.24410(15) 0.25700(12) 0.21448(8) 0.0214(4) Uani 1 1 d . . . . .
H2 H 0.226645 0.323307 0.217796 0.026 Uiso 1 1 calc R U . . .
C3 C 0.24947(17) 0.21542(14) 0.27837(9) 0.0283(4) Uani 1 1 d . . . . .
H3A H 0.175186 0.224690 0.295227 0.042 Uiso 1 1 calc R U . . .
H3B H 0.311375 0.244735 0.304956 0.042 Uiso 1 1 calc R U . . .
H3C H 0.265307 0.150127 0.275935 0.042 Uiso 1 1 calc R U . . .
C4 C 0.14752(15) 0.21312(13) 0.17141(9) 0.0255(4) Uani 1 1 d . . . . .
H4A H 0.144225 0.242316 0.131176 0.038 Uiso 1 1 calc R U . . .
H4B H 0.073063 0.220921 0.188360 0.038 Uiso 1 1 calc R U . . .
H4C H 0.163656 0.148132 0.167211 0.038 Uiso 1 1 calc R U . . .
C5 C 0.42473(15) 0.16769(12) 0.18535(8) 0.0234(4) Uani 1 1 d . . . . .
H5 H 0.407793 0.109487 0.200987 0.028 Uiso 1 1 calc R U . . .
C6 C 0.51801(15) 0.19076(12) 0.15546(8) 0.0232(4) Uani 1 1 d . . . . .
H6 H 0.578625 0.151121 0.146260 0.028 Uiso 1 1 calc R U . . .
C7 C 0.58070(14) 0.33198(12) 0.10491(8) 0.0194(3) Uani 1 1 d . . . . .
C8 C 0.66590(15) 0.28788(12) 0.07513(8) 0.0223(4) Uani 1 1 d . . . . .
H8 H 0.674511 0.223953 0.079860 0.027 Uiso 1 1 calc R U . . .
C9 C 0.73932(15) 0.33421(13) 0.03848(8) 0.0228(4) Uani 1 1 d . . . . .
C10 C 0.83501(15) 0.28505(13) 0.00765(8) 0.0250(4) Uani 1 1 d . . . . .
C11 C 0.95008(19) 0.3348(2) 0.02293(16) 0.0680(10) Uani 1 1 d . . . . .
H11A H 1.011343 0.303523 0.003401 0.102 Uiso 1 1 calc R U . . .
H11B H 0.969552 0.335349 0.067354 0.102 Uiso 1 1 calc R U . . .
H11C H 0.943024 0.397469 0.007820 0.102 Uiso 1 1 calc R U . . .
C12 C 0.8050(2) 0.28725(17) -0.06113(9) 0.0399(5) Uani 1 1 d . . . . .
H12A H 0.866497 0.257203 -0.081243 0.060 Uiso 1 1 calc R U . . .
H12B H 0.797701 0.350533 -0.074953 0.060 Uiso 1 1 calc R U . . .
H12C H 0.731503 0.255450 -0.071619 0.060 Uiso 1 1 calc R U . . .
C13 C 0.8504(3) 0.18655(18) 0.02750(12) 0.0571(8) Uani 1 1 d . . . . .
H13A H 0.777446 0.153647 0.017655 0.086 Uiso 1 1 calc R U . . .
H13B H 0.872225 0.183961 0.071695 0.086 Uiso 1 1 calc R U . . .
H13C H 0.911355 0.158468 0.005946 0.086 Uiso 1 1 calc R U . . .
C14 C 0.72407(15) 0.42749(13) 0.03036(8) 0.0227(4) Uani 1 1 d . . . . .
H14 H 0.770285 0.460100 0.004397 0.027 Uiso 1 1 calc R U . . .
C15 C 0.64104(15) 0.47263(12) 0.06039(8) 0.0210(4) Uani 1 1 d . . . . .
C16 C 0.56983(14) 0.42576(12) 0.09840(8) 0.0189(3) Uani 1 1 d . . . . .
C17 C 0.52914(14) 0.57323(12) 0.10732(8) 0.0188(3) Uani 1 1 d . . . . .
C18 C 0.61347(14) 0.56823(12) 0.06545(8) 0.0203(3) Uani 1 1 d . . . . .
C19 C 0.65723(15) 0.64615(12) 0.03998(8) 0.0217(4) Uani 1 1 d . . . . .
H19 H 0.713915 0.641196 0.011728 0.026 Uiso 1 1 calc R U . . .
C20 C 0.61756(14) 0.73137(12) 0.05611(8) 0.0202(3) Uani 1 1 d . . . . .
C21 C 0.66552(16) 0.82057(12) 0.03195(8) 0.0240(4) Uani 1 1 d . . . . .
C22 C 0.73109(17) 0.80331(13) -0.02394(9) 0.0288(4) Uani 1 1 d . . . . .
H22A H 0.679669 0.773189 -0.055810 0.043 Uiso 1 1 calc R U . . .
H22B H 0.798183 0.764315 -0.012346 0.043 Uiso 1 1 calc R U . . .
H22C H 0.757502 0.861364 -0.039526 0.043 Uiso 1 1 calc R U . . .
C23 C 0.7481(2) 0.86383(16) 0.08211(10) 0.0418(6) Uani 1 1 d . . . . .
H23A H 0.812909 0.822427 0.093256 0.063 Uiso 1 1 calc R U . . .
H23B H 0.706578 0.875593 0.118085 0.063 Uiso 1 1 calc R U . . .
H23C H 0.777668 0.921242 0.067186 0.063 Uiso 1 1 calc R U . . .
C24 C 0.5662(2) 0.88681(15) 0.01269(12) 0.0428(6) Uani 1 1 d . . . . .
H24A H 0.597170 0.940639 -0.006354 0.064 Uiso 1 1 calc R U . . .
H24B H 0.528581 0.905219 0.048806 0.064 Uiso 1 1 calc R U . . .
H24C H 0.509405 0.856834 -0.016651 0.064 Uiso 1 1 calc R U . . .
C25 C 0.53413(14) 0.73543(12) 0.09834(8) 0.0197(3) Uani 1 1 d . . . . .
H25 H 0.506063 0.793283 0.109248 0.024 Uiso 1 1 calc R U . . .
C26 C 0.49102(14) 0.65829(12) 0.12477(8) 0.0185(3) Uani 1 1 d . . . . .
C27 C 0.38127(15) 0.74554(12) 0.19712(8) 0.0210(3) Uani 1 1 d . . . . .
H27 H 0.418708 0.802786 0.195265 0.025 Uiso 1 1 calc R U . . .
C28 C 0.28776(15) 0.72668(12) 0.22813(8) 0.0214(4) Uani 1 1 d . . . . .
H28 H 0.247293 0.767936 0.251646 0.026 Uiso 1 1 calc R U . . .
C29 C 0.26348(14) 0.63440(12) 0.21833(8) 0.0191(3) Uani 1 1 d . . . . .
C30 C 0.16465(15) 0.58268(12) 0.24090(8) 0.0218(4) Uani 1 1 d . . . . .
H30 H 0.173836 0.516757 0.231298 0.026 Uiso 1 1 calc R U . . .
C31 C 0.16392(17) 0.59346(14) 0.30999(9) 0.0300(4) Uani 1 1 d . . . . .
H31A H 0.159955 0.658180 0.320201 0.045 Uiso 1 1 calc R U . . .
H31B H 0.234913 0.567162 0.330654 0.045 Uiso 1 1 calc R U . . .
H31C H 0.096414 0.561954 0.323460 0.045 Uiso 1 1 calc R U . . .
C32 C 0.05105(15) 0.61719(13) 0.20681(10) 0.0290(4) Uani 1 1 d . . . . .
H32A H 0.050414 0.603494 0.163123 0.044 Uiso 1 1 calc R U . . .
H32B H 0.045000 0.683055 0.212460 0.044 Uiso 1 1 calc R U . . .
H32C H -0.014728 0.587017 0.223113 0.044 Uiso 1 1 calc R U . . .
C33 C 0.2670(2) 0.95747(17) 0.13239(12) 0.0365(7) Uani 0.852(5) 1 d D U P A 1
H33A H 0.253794 0.909322 0.101659 0.055 Uiso 0.852(5) 1 calc R U P A 1
H33B H 0.349216 0.958794 0.147776 0.055 Uiso 0.852(5) 1 calc R U P A 1
H33C H 0.244810 1.016269 0.113793 0.055 Uiso 0.852(5) 1 calc R U P A 1
C34 C 0.1953(3) 0.93910(19) 0.18443(15) 0.0277(6) Uani 0.852(5) 1 d D U P A 1
C35 C 0.2412(3) 0.9522(3) 0.24471(16) 0.0269(7) Uani 0.852(5) 1 d D U P A 1
H35 H 0.318108 0.974377 0.252834 0.032 Uiso 0.852(5) 1 calc R U P A 1
C36 C 0.1763(3) 0.9334(4) 0.2934(2) 0.0282(9) Uani 0.852(5) 1 d D U P A 1
H36 H 0.209377 0.941930 0.334284 0.034 Uiso 0.852(5) 1 calc R U P A 1
C37 C 0.0630(4) 0.9020(4) 0.28202(18) 0.0294(9) Uani 0.852(5) 1 d D U P A 1
H37 H 0.017906 0.889997 0.314942 0.035 Uiso 0.852(5) 1 calc R U P A 1
C38 C 0.0168(4) 0.8886(3) 0.22205(18) 0.0309(8) Uani 0.852(5) 1 d D U P A 1
H38 H -0.059939 0.865980 0.213953 0.037 Uiso 0.852(5) 1 calc R U P A 1
C39 C 0.0814(3) 0.9077(2) 0.17395(14) 0.0302(7) Uani 0.852(5) 1 d D U P A 1
H39 H 0.047849 0.899382 0.133129 0.036 Uiso 0.852(5) 1 calc R U P A 1
C33B C 0.0772(15) 0.9510(11) 0.1078(6) 0.045(4) Uani 0.148(5) 1 d D U P A 2
H33D H 0.148144 0.957575 0.087359 0.068 Uiso 0.148(5) 1 calc R U P A 2
H33E H 0.030126 1.006203 0.101329 0.068 Uiso 0.148(5) 1 calc R U P A 2
H33F H 0.032969 0.898600 0.090718 0.068 Uiso 0.148(5) 1 calc R U P A 2
C34B C 0.1080(17) 0.9370(13) 0.1747(7) 0.028(2) Uani 0.148(5) 1 d D U P A 2
C35B C 0.2148(15) 0.9609(12) 0.2024(9) 0.027(2) Uani 0.148(5) 1 d D U P A 2
H35B H 0.272819 0.983332 0.178612 0.032 Uiso 0.148(5) 1 calc R U P A 2
C36B C 0.237(2) 0.9525(18) 0.2645(10) 0.027(3) Uani 0.148(5) 1 d D U P A 2
H36B H 0.312237 0.967583 0.283370 0.032 Uiso 0.148(5) 1 calc R U P A 2
C37B C 0.154(3) 0.923(3) 0.2999(12) 0.028(3) Uani 0.148(5) 1 d D U P A 2
H37B H 0.168562 0.923517 0.343237 0.033 Uiso 0.148(5) 1 calc R U P A 2
C38B C 0.050(3) 0.891(2) 0.2722(11) 0.028(3) Uani 0.148(5) 1 d D U P A 2
H38B H -0.003302 0.860030 0.295234 0.033 Uiso 0.148(5) 1 calc R U P A 2
C39B C 0.024(2) 0.9056(19) 0.2102(11) 0.030(3) Uani 0.148(5) 1 d D U P A 2
H39B H -0.052109 0.893983 0.191681 0.036 Uiso 0.148(5) 1 calc R U P A 2
N1 N 0.41041(12) 0.31609(10) 0.16186(6) 0.0185(3) Uani 1 1 d . . . . .
N2 N 0.50897(12) 0.28058(10) 0.14112(7) 0.0193(3) Uani 1 1 d . . . . .
N3 N 0.49834(12) 0.48645(10) 0.12721(7) 0.0187(3) Uani 1 1 d . . . . .
N4 N 0.41110(12) 0.66778(9) 0.16943(6) 0.0179(3) Uani 1 1 d . . . . .
N5 N 0.33893(11) 0.59818(9) 0.18267(6) 0.0172(3) Uani 1 1 d . . . . .
Cl1 Cl 0.20018(3) 0.44059(3) 0.11041(2) 0.02174(11) Uani 1 1 d . . . . .
Cl2 Cl 0.41578(4) 0.44476(3) 0.27515(2) 0.02211(11) Uani 1 1 d . . . . .
V1 V 0.37014(2) 0.45687(2) 0.17079(2) 0.01616(10) 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
C1 N1 1.339(2) . ?
C1 C5 1.402(2) . ?
C1 C2 1.506(2) . ?
C2 C3 1.527(3) . ?
C2 C4 1.536(2) . ?
C2 H2 1.0000 . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C5 C6 1.362(3) . ?
C5 H5 0.9500 . ?
C6 N2 1.360(2) . ?
C6 H6 0.9500 . ?
C7 C16 1.391(2) . ?
C7 C8 1.397(2) . ?
C7 N2 1.423(2) . ?
C8 C9 1.404(3) . ?
C8 H8 0.9500 . ?
C9 C14 1.392(3) . ?
C9 C10 1.536(2) . ?
C10 C12 1.517(3) . ?
C10 C13 1.518(3) . ?
C10 C11 1.530(3) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 C15 1.388(2) . ?
C14 H14 0.9500 . ?
C15 C16 1.410(2) . ?
C15 C18 1.449(2) . ?
C16 N3 1.410(2) . ?
C17 C26 1.393(2) . ?
C17 N3 1.406(2) . ?
C17 C18 1.409(2) . ?
C18 C19 1.392(2) . ?
C19 C20 1.393(2) . ?
C19 H19 0.9500 . ?
C20 C25 1.406(2) . ?
C20 C21 1.539(2) . ?
C21 C23 1.526(3) . ?
C21 C22 1.527(3) . ?
C21 C24 1.536(3) . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 C26 1.390(2) . ?
C25 H25 0.9500 . ?
C26 N4 1.421(2) . ?
C27 N4 1.356(2) . ?
C27 C28 1.364(2) . ?
C27 H27 0.9500 . ?
C28 C29 1.399(2) . ?
C28 H28 0.9500 . ?
C29 N5 1.341(2) . ?
C29 C30 1.500(2) . ?
C30 C31 1.527(3) . ?
C30 C32 1.537(2) . ?
C30 H30 1.0000 . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C33 C34 1.503(4) . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C34 C35 1.391(4) . ?
C34 C39 1.396(4) . ?
C35 C36 1.395(5) . ?
C35 H35 0.9500 . ?
C36 C37 1.391(5) . ?
C36 H36 0.9500 . ?
C37 C38 1.387(5) . ?
C37 H37 0.9500 . ?
C38 C39 1.383(5) . ?
C38 H38 0.9500 . ?
C39 H39 0.9500 . ?
C33B C34B 1.492(15) . ?
C33B H33D 0.9800 . ?
C33B H33E 0.9800 . ?
C33B H33F 0.9800 . ?
C34B C35B 1.372(15) . ?
C34B C39B 1.385(17) . ?
C35B C36B 1.370(16) . ?
C35B H35B 0.9500 . ?
C36B C37B 1.368(17) . ?
C36B H36B 0.9500 . ?
C37B C38B 1.385(19) . ?
C37B H37B 0.9500 . ?
C38B C39B 1.383(18) . ?
C38B H38B 0.9500 . ?
C39B H39B 0.9500 . ?
N1 N2 1.3743(19) . ?
N1 V1 2.1357(14) . ?
N3 V1 1.8961(15) . ?
N4 N5 1.3713(19) . ?
N5 V1 2.1298(14) . ?
Cl1 V1 2.2783(5) . ?
Cl2 V1 2.3088(5) . ?

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
N1 C1 C5 109.94(15) . . ?
N1 C1 C2 122.83(15) . . ?
C5 C1 C2 127.19(16) . . ?
C1 C2 C3 110.70(15) . . ?
C1 C2 C4 110.06(14) . . ?
C3 C2 C4 111.09(15) . . ?
C1 C2 H2 108.3 . . ?
C3 C2 H2 108.3 . . ?
C4 C2 H2 108.3 . . ?
C2 C3 H3A 109.5 . . ?
C2 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
C2 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
C2 C4 H4A 109.5 . . ?
C2 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
C2 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C6 C5 C1 106.14(16) . . ?
C6 C5 H5 126.9 . . ?
C1 C5 H5 126.9 . . ?
N2 C6 C5 107.86(15) . . ?
N2 C6 H6 126.1 . . ?
C5 C6 H6 126.1 . . ?
C16 C7 C8 118.25(16) . . ?
C16 C7 N2 122.14(15) . . ?
C8 C7 N2 119.61(15) . . ?
C7 C8 C9 122.66(17) . . ?
C7 C8 H8 118.7 . . ?
C9 C8 H8 118.7 . . ?
C14 C9 C8 118.35(16) . . ?
C14 C9 C10 119.70(16) . . ?
C8 C9 C10 121.95(16) . . ?
C12 C10 C13 108.38(18) . . ?
C12 C10 C11 108.6(2) . . ?
C13 C10 C11 108.6(2) . . ?
C12 C10 C9 108.90(15) . . ?
C13 C10 C9 113.08(16) . . ?
C11 C10 C9 109.28(16) . . ?
C10 C11 H11A 109.5 . . ?
C10 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C10 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C10 C12 H12A 109.5 . . ?
C10 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C10 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C10 C13 H13A 109.5 . . ?
C10 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C10 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C15 C14 C9 119.71(17) . . ?
C15 C14 H14 120.1 . . ?
C9 C14 H14 120.1 . . ?
C14 C15 C16 121.41(17) . . ?
C14 C15 C18 132.00(17) . . ?
C16 C15 C18 106.40(15) . . ?
C7 C16 N3 129.27(16) . . ?
C7 C16 C15 119.54(16) . . ?
N3 C16 C15 111.14(15) . . ?
C26 C17 N3 129.22(15) . . ?
C26 C17 C18 119.08(16) . . ?
N3 C17 C18 111.67(15) . . ?
C19 C18 C17 121.54(16) . . ?
C19 C18 C15 132.53(16) . . ?
C17 C18 C15 105.86(15) . . ?
C18 C19 C20 119.73(16) . . ?
C18 C19 H19 120.1 . . ?
C20 C19 H19 120.1 . . ?
C19 C20 C25 118.16(16) . . ?
C19 C20 C21 122.66(15) . . ?
C25 C20 C21 119.12(15) . . ?
C23 C21 C22 108.86(16) . . ?
C23 C21 C24 109.57(19) . . ?
C22 C21 C24 107.63(16) . . ?
C23 C21 C20 109.18(15) . . ?
C22 C21 C20 111.14(15) . . ?
C24 C21 C20 110.42(15) . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C21 C23 H23A 109.5 . . ?
C21 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C21 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C21 C24 H24A 109.5 . . ?
C21 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C21 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C26 C25 C20 122.69(16) . . ?
C26 C25 H25 118.7 . . ?
C20 C25 H25 118.7 . . ?
C25 C26 C17 118.76(15) . . ?
C25 C26 N4 119.60(15) . . ?
C17 C26 N4 121.63(15) . . ?
N4 C27 C28 107.62(15) . . ?
N4 C27 H27 126.2 . . ?
C28 C27 H27 126.2 . . ?
C27 C28 C29 106.15(15) . . ?
C27 C28 H28 126.9 . . ?
C29 C28 H28 126.9 . . ?
N5 C29 C28 110.03(15) . . ?
N5 C29 C30 123.73(15) . . ?
C28 C29 C30 126.17(15) . . ?
C29 C30 C31 110.77(14) . . ?
C29 C30 C32 108.54(15) . . ?
C31 C30 C32 111.24(15) . . ?
C29 C30 H30 108.7 . . ?
C31 C30 H30 108.7 . . ?
C32 C30 H30 108.7 . . ?
C30 C31 H31A 109.5 . . ?
C30 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C30 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C30 C32 H32A 109.5 . . ?
C30 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C30 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C34 C33 H33A 109.5 . . ?
C34 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
C34 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C35 C34 C39 118.1(3) . . ?
C35 C34 C33 120.7(3) . . ?
C39 C34 C33 121.2(3) . . ?
C34 C35 C36 121.2(3) . . ?
C34 C35 H35 119.4 . . ?
C36 C35 H35 119.4 . . ?
C37 C36 C35 119.9(4) . . ?
C37 C36 H36 120.0 . . ?
C35 C36 H36 120.0 . . ?
C38 C37 C36 119.2(4) . . ?
C38 C37 H37 120.4 . . ?
C36 C37 H37 120.4 . . ?
C39 C38 C37 120.5(4) . . ?
C39 C38 H38 119.7 . . ?
C37 C38 H38 119.7 . . ?
C38 C39 C34 121.0(3) . . ?
C38 C39 H39 119.5 . . ?
C34 C39 H39 119.5 . . ?
C34B C33B H33D 109.5 . . ?
C34B C33B H33E 109.5 . . ?
H33D C33B H33E 109.5 . . ?
C34B C33B H33F 109.5 . . ?
H33D C33B H33F 109.5 . . ?
H33E C33B H33F 109.5 . . ?
C35B C34B C39B 119.3(15) . . ?
C35B C34B C33B 121.3(16) . . ?
C39B C34B C33B 119.1(16) . . ?
C36B C35B C34B 119.7(17) . . ?
C36B C35B H35B 120.1 . . ?
C34B C35B H35B 120.1 . . ?
C37B C36B C35B 121(2) . . ?
C37B C36B H36B 119.4 . . ?
C35B C36B H36B 119.4 . . ?
C36B C37B C38B 120(2) . . ?
C36B C37B H37B 120.2 . . ?
C38B C37B H37B 120.2 . . ?
C39B C38B C37B 118(2) . . ?
C39B C38B H38B 120.8 . . ?
C37B C38B H38B 120.8 . . ?
C38B C39B C34B 121(2) . . ?
C38B C39B H39B 119.6 . . ?
C34B C39B H39B 119.6 . . ?
C1 N1 N2 106.17(13) . . ?
C1 N1 V1 125.63(11) . . ?
N2 N1 V1 126.53(11) . . ?
C6 N2 N1 109.89(14) . . ?
C6 N2 C7 127.55(15) . . ?
N1 N2 C7 122.28(14) . . ?
C17 N3 C16 104.87(14) . . ?
C17 N3 V1 126.91(11) . . ?
C16 N3 V1 127.31(12) . . ?
C27 N4 N5 110.28(13) . . ?
C27 N4 C26 127.22(14) . . ?
N5 N4 C26 121.73(13) . . ?
C29 N5 N4 105.91(13) . . ?
C29 N5 V1 125.99(11) . . ?
N4 N5 V1 126.00(10) . . ?
N3 V1 N5 89.37(6) . . ?
N3 V1 N1 89.24(6) . . ?
N5 V1 N1 176.83(5) . . ?
N3 V1 Cl1 113.99(5) . . ?
N5 V1 Cl1 91.50(4) . . ?
N1 V1 Cl1 91.67(4) . . ?
N3 V1 Cl2 113.84(5) . . ?
N5 V1 Cl2 88.79(4) . . ?
N1 V1 Cl2 89.17(4) . . ?
Cl1 V1 Cl2 132.169(19) . . ?

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
N1 C1 C2 C3 -132.56(17) . . . . ?
C5 C1 C2 C3 50.2(2) . . . . ?
N1 C1 C2 C4 104.25(19) . . . . ?
C5 C1 C2 C4 -73.0(2) . . . . ?
N1 C1 C5 C6 -0.5(2) . . . . ?
C2 C1 C5 C6 177.04(17) . . . . ?
C1 C5 C6 N2 0.1(2) . . . . ?
C16 C7 C8 C9 -0.9(3) . . . . ?
N2 C7 C8 C9 179.70(15) . . . . ?
C7 C8 C9 C14 -1.8(3) . . . . ?
C7 C8 C9 C10 178.09(16) . . . . ?
C14 C9 C10 C12 -66.9(2) . . . . ?
C8 C9 C10 C12 113.3(2) . . . . ?
C14 C9 C10 C13 172.6(2) . . . . ?
C8 C9 C10 C13 -7.3(3) . . . . ?
C14 C9 C10 C11 51.6(3) . . . . ?
C8 C9 C10 C11 -128.3(2) . . . . ?
C8 C9 C14 C15 2.7(3) . . . . ?
C10 C9 C14 C15 -177.15(16) . . . . ?
C9 C14 C15 C16 -1.1(3) . . . . ?
C9 C14 C15 C18 173.30(18) . . . . ?
C8 C7 C16 N3 -174.34(16) . . . . ?
N2 C7 C16 N3 5.1(3) . . . . ?
C8 C7 C16 C15 2.5(2) . . . . ?
N2 C7 C16 C15 -178.06(15) . . . . ?
C14 C15 C16 C7 -1.6(3) . . . . ?
C18 C15 C16 C7 -177.27(15) . . . . ?
C14 C15 C16 N3 175.79(15) . . . . ?
C18 C15 C16 N3 0.14(19) . . . . ?
C26 C17 C18 C19 -1.7(3) . . . . ?
N3 C17 C18 C19 -179.67(15) . . . . ?
C26 C17 C18 C15 175.65(15) . . . . ?
N3 C17 C18 C15 -2.34(19) . . . . ?
C14 C15 C18 C19 3.2(3) . . . . ?
C16 C15 C18 C19 178.22(18) . . . . ?
C14 C15 C18 C17 -173.71(18) . . . . ?
C16 C15 C18 C17 1.30(18) . . . . ?
C17 C18 C19 C20 0.2(3) . . . . ?
C15 C18 C19 C20 -176.33(18) . . . . ?
C18 C19 C20 C25 0.3(2) . . . . ?
C18 C19 C20 C21 177.38(16) . . . . ?
C19 C20 C21 C23 -103.2(2) . . . . ?
C25 C20 C21 C23 73.8(2) . . . . ?
C19 C20 C21 C22 16.9(2) . . . . ?
C25 C20 C21 C22 -166.12(16) . . . . ?
C19 C20 C21 C24 136.24(19) . . . . ?
C25 C20 C21 C24 -46.7(2) . . . . ?
C19 C20 C25 C26 0.6(3) . . . . ?
C21 C20 C25 C26 -176.52(15) . . . . ?
C20 C25 C26 C17 -2.1(2) . . . . ?
C20 C25 C26 N4 176.84(15) . . . . ?
N3 C17 C26 C25 -179.83(16) . . . . ?
C18 C17 C26 C25 2.6(2) . . . . ?
N3 C17 C26 N4 1.2(3) . . . . ?
C18 C17 C26 N4 -176.36(15) . . . . ?
N4 C27 C28 C29 0.5(2) . . . . ?
C27 C28 C29 N5 -0.1(2) . . . . ?
C27 C28 C29 C30 -177.08(16) . . . . ?
N5 C29 C30 C31 129.32(18) . . . . ?
C28 C29 C30 C31 -54.1(2) . . . . ?
N5 C29 C30 C32 -108.28(19) . . . . ?
C28 C29 C30 C32 68.3(2) . . . . ?
C39 C34 C35 C36 0.9(5) . . . . ?
C33 C34 C35 C36 -178.5(4) . . . . ?
C34 C35 C36 C37 -0.9(7) . . . . ?
C35 C36 C37 C38 1.0(8) . . . . ?
C36 C37 C38 C39 -1.3(7) . . . . ?
C37 C38 C39 C34 1.4(6) . . . . ?
C35 C34 C39 C38 -1.2(4) . . . . ?
C33 C34 C39 C38 178.2(3) . . . . ?
C39B C34B C35B C36B 1(3) . . . . ?
C33B C34B C35B C36B 176(2) . . . . ?
C34B C35B C36B C37B -2(4) . . . . ?
C35B C36B C37B C38B 7(5) . . . . ?
C36B C37B C38B C39B -11(5) . . . . ?
C37B C38B C39B C34B 11(5) . . . . ?
C35B C34B C39B C38B -5(4) . . . . ?
C33B C34B C39B C38B 179(3) . . . . ?
C5 C1 N1 N2 0.71(19) . . . . ?
C2 C1 N1 N2 -177.00(15) . . . . ?
C5 C1 N1 V1 -165.31(12) . . . . ?
C2 C1 N1 V1 17.0(2) . . . . ?
C5 C6 N2 N1 0.3(2) . . . . ?
C5 C6 N2 C7 -173.61(16) . . . . ?
C1 N1 N2 C6 -0.62(18) . . . . ?
V1 N1 N2 C6 165.23(12) . . . . ?
C1 N1 N2 C7 173.66(15) . . . . ?
V1 N1 N2 C7 -20.5(2) . . . . ?
C16 C7 N2 C6 -173.50(17) . . . . ?
C8 C7 N2 C6 5.9(3) . . . . ?
C16 C7 N2 N1 13.3(2) . . . . ?
C8 C7 N2 N1 -167.32(15) . . . . ?
C26 C17 N3 C16 -175.34(17) . . . . ?
C18 C17 N3 C16 2.39(18) . . . . ?
C26 C17 N3 V1 15.0(3) . . . . ?
C18 C17 N3 V1 -167.31(12) . . . . ?
C7 C16 N3 C17 175.58(17) . . . . ?
C15 C16 N3 C17 -1.51(18) . . . . ?
C7 C16 N3 V1 -14.8(3) . . . . ?
C15 C16 N3 V1 168.14(12) . . . . ?
C28 C27 N4 N5 -0.74(19) . . . . ?
C28 C27 N4 C26 169.27(16) . . . . ?
C25 C26 N4 C27 -10.0(3) . . . . ?
C17 C26 N4 C27 168.92(16) . . . . ?
C25 C26 N4 N5 158.96(15) . . . . ?
C17 C26 N4 N5 -22.1(2) . . . . ?
C28 C29 N5 N4 -0.33(18) . . . . ?
C30 C29 N5 N4 176.73(15) . . . . ?
C28 C29 N5 V1 163.93(11) . . . . ?
C30 C29 N5 V1 -19.0(2) . . . . ?
C27 N4 N5 C29 0.66(18) . . . . ?
C26 N4 N5 C29 -169.99(14) . . . . ?
C27 N4 N5 V1 -163.60(11) . . . . ?
C26 N4 N5 V1 25.8(2) . . . . ?
C17 N3 V1 N5 -9.09(14) . . . . ?
C16 N3 V1 N5 -176.54(14) . . . . ?
C17 N3 V1 N1 173.76(14) . . . . ?
C16 N3 V1 N1 6.30(14) . . . . ?
C17 N3 V1 Cl1 82.27(14) . . . . ?
C16 N3 V1 Cl1 -85.18(14) . . . . ?
C17 N3 V1 Cl2 -97.48(13) . . . . ?
C16 N3 V1 Cl2 95.06(13) . . . . ?

_refine_diff_density_max         0.475
_refine_diff_density_min         -0.481
_refine_diff_density_rms         0.052

