# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2014

#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_1_V-COOH

_audit_creation_date             2011-07-05T15:28:29-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C37 H53 N O6 V, C2 H6 O'
_chemical_formula_sum            'C39 H59 N O7 V'
_chemical_formula_weight         704.81
_chemical_compound_source        'synthesis as described'

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P n a 21'
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_Int_Tables_number      33
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z+1/2'
'-x+1/2, y+1/2, z+1/2'
'x+1/2, -y+1/2, z'

_cell_length_a                   18.2255(6)
_cell_length_b                   13.2449(9)
_cell_length_c                   16.4934(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3981.4(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    123(2)
_cell_measurement_reflns_used    4958
_cell_measurement_theta_min      0.407
_cell_measurement_theta_max      27.878
_cell_measurement_wavelength     0.71073

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_description       cube
_exptl_crystal_colour            'dark brown'
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.28
_exptl_crystal_density_diffrn    1.176
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1516
_exptl_special_details           
;
 ?
;

#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    0.295
_exptl_absorpt_correction_T_min  0.6516
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2008)'

#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_source                   'Enraf Nonius FR590'
_diffrn_ambient_temperature      123(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_orient_matrix_type       'by Bruker AXS Collect from scalepack cell'
_diffrn_orient_matrix_ub_11      -0.11688E-2
_diffrn_orient_matrix_ub_12      0.409E-3
_diffrn_orient_matrix_ub_13      0.548613E-1
_diffrn_orient_matrix_ub_21      -0.674387E-1
_diffrn_orient_matrix_ub_22      -0.272543E-1
_diffrn_orient_matrix_ub_23      -0.5924E-3
_diffrn_orient_matrix_ub_31      0.339268E-1
_diffrn_orient_matrix_ub_32      -0.541611E-1
_diffrn_orient_matrix_ub_33      0.7124E-3
_diffrn_measurement_device       '95mm CCD camera on κ-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_reflns_av_unetI/netI     0.0368
_diffrn_reflns_number            8911
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         2.55
_diffrn_reflns_theta_max         27.81
_diffrn_reflns_theta_full        27.81
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_reflns_number_total             8911
_reflns_number_gt                7937
_reflns_threshold_expression     >2σ(I)

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_reduction        
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_structure_solution    'SIR97 (Giacovazzo et al, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'

#----------------------------------------------------------------------------#
#                   STRUCTURE SOLUTION
#----------------------------------------------------------------------------#

_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2σ(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0066P)²+1.6293P] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_number_reflns         8523
_refine_ls_number_parameters     504
_refine_ls_number_restraints     4
_refine_ls_R_factor_all          0.0544
_refine_ls_R_factor_gt           0.0408
_refine_ls_wR_factor_ref         0.0871
_refine_ls_wR_factor_gt          0.081
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_restrained_S_all      1.032
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.027(17)
_refine_diff_density_max         0.192
_refine_diff_density_min         -0.271
_refine_diff_density_rms         0.043

#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

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 0 '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 0.006 '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'

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
V1 V 0.179007(19) 0.79912(2) 0.37776(2) 0.02418(8) Uani 1 1 d . . .
O1 O 0.23778(9) 0.89410(10) 0.33416(9) 0.0277(3) Uani 1 1 d . . .
O2 O 0.12018(8) 0.71747(10) 0.43532(10) 0.0270(3) Uani 1 1 d . . .
O3 O 0.09200(9) 0.86416(11) 0.32799(10) 0.0326(4) Uani 1 1 d . . .
O4 O 0.00434(10) 0.98104(13) 0.33865(11) 0.0422(4) Uani 1 1 d . . .
O5 O 0.19319(10) 0.70838(12) 0.28676(10) 0.0323(4) Uani 1 1 d . . .
O6 O 0.26553(8) 0.73786(11) 0.43410(9) 0.0281(3) Uani 1 1 d . . .
O7 O -0.05210(14) 0.95301(17) 0.18329(15) 0.0561(6) Uani 1 1 d D . .
N8 N 0.15629(10) 0.91174(13) 0.47187(11) 0.0243(4) Uani 1 1 d . . .
C1 C 0.25509(12) 0.99334(15) 0.33892(14) 0.0242(4) Uani 1 1 d . . .
C2 C 0.28193(13) 1.04669(16) 0.27170(13) 0.0262(5) Uani 1 1 d . . .
C3 C 0.30159(13) 1.14719(16) 0.28606(14) 0.0277(5) Uani 1 1 d . . .
H3 H 0.3206 1.1841 0.2429 0.033 Uiso 1 1 calc R . .
C4 C 0.29456(12) 1.19586(16) 0.36082(13) 0.0274(5) Uani 1 1 d . . .
C5 C 0.26485(12) 1.13969(16) 0.42423(14) 0.0266(5) Uani 1 1 d . . .
H5 H 0.2577 1.1704 0.4743 0.032 Uiso 1 1 calc R . .
C6 C 0.24582(12) 1.03935(16) 0.41441(14) 0.0246(5) Uani 1 1 d . . .
C7 C 0.22253(13) 0.97652(17) 0.48586(13) 0.0273(5) Uani 1 1 d . . .
H7A H 0.2631 0.9333 0.5014 0.033 Uiso 1 1 calc R . .
H7B H 0.2126 1.0213 0.5311 0.033 Uiso 1 1 calc R . .
C9 C 0.14077(13) 0.86239(16) 0.55238(13) 0.0268(5) Uani 1 1 d . . .
H9A H 0.1838 0.8242 0.5685 0.032 Uiso 1 1 calc R . .
H9B H 0.1333 0.9149 0.5925 0.032 Uiso 1 1 calc R . .
C10 C 0.07576(12) 0.79333(16) 0.55388(14) 0.0259(5) Uani 1 1 d . . .
C11 C 0.02584(14) 0.79653(18) 0.61729(15) 0.0309(5) Uani 1 1 d . . .
H11 H 0.0287 0.8483 0.6553 0.037 Uiso 1 1 calc R . .
C12 C -0.02832(14) 0.72345(18) 0.62480(17) 0.0347(5) Uani 1 1 d . A .
C13 C -0.03223(13) 0.64949(18) 0.56472(17) 0.0354(6) Uani 1 1 d . . .
H13 H -0.0684 0.6004 0.5696 0.043 Uiso 1 1 calc R . .
C14 C 0.01420(13) 0.64422(17) 0.49826(15) 0.0311(5) Uani 1 1 d . . .
C15 C 0.06971(12) 0.71813(16) 0.49475(14) 0.0271(5) Uani 1 1 d . . .
C16 C 0.09176(13) 0.97307(16) 0.44438(14) 0.0294(5) Uani 1 1 d . . .
H16A H 0.1068 1.043 0.4391 0.035 Uiso 1 1 calc R . .
H16B H 0.0539 0.97 0.4856 0.035 Uiso 1 1 calc R . .
C17 C 0.05969(13) 0.93791(16) 0.36423(15) 0.0309(5) Uani 1 1 d . . .
C18 C 0.28902(13) 0.99755(17) 0.18790(13) 0.0292(5) Uani 1 1 d . . .
C19 C 0.21481(16) 0.9545(2) 0.15964(15) 0.0447(7) Uani 1 1 d . . .
H19A H 0.1788 1.0075 0.1589 0.067 Uiso 1 1 calc R . .
H19B H 0.1994 0.9024 0.1963 0.067 Uiso 1 1 calc R . .
H19C H 0.22 0.9269 0.1061 0.067 Uiso 1 1 calc R . .
C20 C 0.31495(15) 1.07275(19) 0.12355(15) 0.0395(6) Uani 1 1 d . . .
H20A H 0.2824 1.1297 0.1225 0.059 Uiso 1 1 calc R . .
H20B H 0.315 1.0406 0.0714 0.059 Uiso 1 1 calc R . .
H20C H 0.3637 1.0951 0.1364 0.059 Uiso 1 1 calc R . .
C21 C 0.34595(16) 0.91177(19) 0.19141(16) 0.0421(6) Uani 1 1 d . . .
H21A H 0.3488 0.8793 0.1395 0.063 Uiso 1 1 calc R . .
H21B H 0.3315 0.8634 0.2317 0.063 Uiso 1 1 calc R . .
H21C H 0.3931 0.9391 0.2052 0.063 Uiso 1 1 calc R . .
C22 C 0.31872(13) 1.30507(15) 0.3752(2) 0.0332(4) Uani 1 1 d . . .
C23 C 0.34503(17) 1.3566(2) 0.29745(17) 0.0467(7) Uani 1 1 d . . .
H23A H 0.3854 1.3193 0.275 0.07 Uiso 1 1 calc R . .
H23B H 0.3607 1.4242 0.3096 0.07 Uiso 1 1 calc R . .
H23C H 0.3056 1.3588 0.2589 0.07 Uiso 1 1 calc R . .
C24 C 0.38212(18) 1.30521(19) 0.43706(19) 0.0531(8) Uani 1 1 d . . .
H24A H 0.4228 1.2678 0.4155 0.08 Uiso 1 1 calc R . .
H24B H 0.366 1.2745 0.4867 0.08 Uiso 1 1 calc R . .
H24C H 0.3971 1.3735 0.4475 0.08 Uiso 1 1 calc R . .
C25 C 0.25507(18) 1.36660(19) 0.41065(19) 0.0485(7) Uani 1 1 d . . .
H25A H 0.2706 1.4351 0.419 0.073 Uiso 1 1 calc R . .
H25B H 0.2403 1.3377 0.4615 0.073 Uiso 1 1 calc R . .
H25C H 0.2144 1.3655 0.3736 0.073 Uiso 1 1 calc R . .
C26 C 0.00661(14) 0.56276(18) 0.43291(18) 0.0385(6) Uani 1 1 d . . .
C27 C -0.00237(16) 0.6111(2) 0.34964(18) 0.0474(7) Uani 1 1 d . . .
H27A H -0.045 0.6536 0.3496 0.071 Uiso 1 1 calc R . .
H27B H -0.008 0.5592 0.3095 0.071 Uiso 1 1 calc R . .
H27C H 0.0402 0.6508 0.3374 0.071 Uiso 1 1 calc R . .
C28 C 0.07552(17) 0.4954(2) 0.4348(2) 0.0542(8) Uani 1 1 d . . .
H28A H 0.1181 0.5358 0.4237 0.081 Uiso 1 1 calc R . .
H28B H 0.0712 0.4436 0.3944 0.081 Uiso 1 1 calc R . .
H28C H 0.0802 0.465 0.4873 0.081 Uiso 1 1 calc R . .
C29 C -0.06066(18) 0.4954(2) 0.4468(2) 0.0641(9) Uani 1 1 d . . .
H29A H -0.0566 0.4627 0.4985 0.096 Uiso 1 1 calc R . .
H29B H -0.0633 0.4454 0.4048 0.096 Uiso 1 1 calc R . .
H29C H -0.1043 0.5361 0.4458 0.096 Uiso 1 1 calc R . .
C30 C -0.08143(15) 0.7222(2) 0.69632(18) 0.0477(7) Uani 1 1 d . . .
C31A C -0.0801(3) 0.8123(5) 0.7462(3) 0.0578(17) Uani 0.592(5) 1 d P A 1
H31A H -0.1177 0.8078 0.7868 0.087 Uiso 0.592(5) 1 calc PR A 1
H31B H -0.0887 0.8705 0.7128 0.087 Uiso 0.592(5) 1 calc PR A 1
H31C H -0.0331 0.8182 0.7719 0.087 Uiso 0.592(5) 1 calc PR A 1
C32A C -0.0674(3) 0.6256(5) 0.7419(4) 0.070(2) Uani 0.592(5) 1 d P A 1
H32A H -0.1037 0.6177 0.7836 0.104 Uiso 0.592(5) 1 calc PR A 1
H32B H -0.0195 0.6281 0.7661 0.104 Uiso 0.592(5) 1 calc PR A 1
H32C H -0.07 0.5696 0.7052 0.104 Uiso 0.592(5) 1 calc PR A 1
C33A C -0.1635(2) 0.7114(4) 0.6599(3) 0.0481(14) Uani 0.592(5) 1 d P A 1
H33A H -0.1673 0.6495 0.6299 0.072 Uiso 0.592(5) 1 calc PR A 1
H33B H -0.1736 0.7673 0.6246 0.072 Uiso 0.592(5) 1 calc PR A 1
H33C H -0.1984 0.7109 0.7035 0.072 Uiso 0.592(5) 1 calc PR A 1
C31B C -0.0320(4) 0.7271(6) 0.7813(4) 0.048(2) Uani 0.408(5) 1 d P A 2
H31D H -0.0639 0.7215 0.8273 0.071 Uiso 0.408(5) 1 calc PR A 2
H31E H -0.0061 0.7902 0.7836 0.071 Uiso 0.408(5) 1 calc PR A 2
H31F H 0.0026 0.6725 0.7818 0.071 Uiso 0.408(5) 1 calc PR A 2
C32B C -0.1276(5) 0.6322(8) 0.7076(5) 0.079(3) Uani 0.408(5) 1 d P A 2
H32D H -0.1567 0.6401 0.7557 0.118 Uiso 0.408(5) 1 calc PR A 2
H32E H -0.097 0.5737 0.7129 0.118 Uiso 0.408(5) 1 calc PR A 2
H32F H -0.1593 0.6243 0.6615 0.118 Uiso 0.408(5) 1 calc PR A 2
C33B C -0.1202(6) 0.8247(8) 0.7013(7) 0.081(4) Uani 0.408(5) 1 d P A 2
H33D H -0.1515 0.833 0.6549 0.121 Uiso 0.408(5) 1 calc PR A 2
H33E H -0.0842 0.8776 0.7021 0.121 Uiso 0.408(5) 1 calc PR A 2
H33F H -0.1491 0.8277 0.7499 0.121 Uiso 0.408(5) 1 calc PR A 2
C34 C 0.2531(2) 0.6126(2) 0.18649(18) 0.0586(9) Uani 1 1 d . . .
H34A H 0.2122 0.5673 0.1809 0.088 Uiso 1 1 calc R . .
H34B H 0.298 0.5759 0.1789 0.088 Uiso 1 1 calc R . .
H34C H 0.2495 0.665 0.1465 0.088 Uiso 1 1 calc R . .
C35 C 0.25219(16) 0.65914(17) 0.27057(15) 0.0360(6) Uani 1 1 d . . .
C36 C 0.31067(15) 0.64632(18) 0.32193(16) 0.0365(6) Uani 1 1 d . . .
H36 H 0.3516 0.6127 0.3018 0.044 Uiso 1 1 calc R . .
C37 C 0.31350(13) 0.67974(16) 0.40207(14) 0.0284(5) Uani 1 1 d . . .
C38 C 0.37429(14) 0.64533(19) 0.45631(17) 0.0391(6) Uani 1 1 d . . .
H38A H 0.4016 0.7028 0.4749 0.059 Uiso 1 1 calc R . .
H38B H 0.4063 0.601 0.4268 0.059 Uiso 1 1 calc R . .
H38C H 0.3541 0.6101 0.502 0.059 Uiso 1 1 calc R . .
C39A C 0.0013(3) 0.8938(5) 0.1371(3) 0.052(2) Uani 0.546(10) 1 d PD B 3
H39A H 0.0417 0.874 0.172 0.063 Uiso 0.546(10) 1 calc PR B 3
H39B H 0.0208 0.934 0.093 0.063 Uiso 0.546(10) 1 calc PR B 3
C40A C -0.0362(7) 0.8016(7) 0.1040(10) 0.144(7) Uani 0.546(10) 1 d PD B 3
H40A H -0.0492 0.7575 0.1479 0.216 Uiso 0.546(10) 1 calc PR B 3
H40B H -0.0035 0.767 0.0677 0.216 Uiso 0.546(10) 1 calc PR B 3
H40C H -0.0796 0.8214 0.0753 0.216 Uiso 0.546(10) 1 calc PR B 3
C39B C -0.0468(6) 0.8415(7) 0.1621(6) 0.083(4) Uani 0.454(10) 1 d PD B 4
H39C H -0.0619 0.8034 0.2095 0.1 Uiso 0.454(10) 1 calc PR B 4
H39D H -0.0824 0.8279 0.1198 0.1 Uiso 0.454(10) 1 calc PR B 4
C40B C 0.0158(8) 0.8059(14) 0.1383(9) 0.146(8) Uani 0.454(10) 1 d PD B 4
H40D H 0.0303 0.8388 0.089 0.22 Uiso 0.454(10) 1 calc PR B 4
H40E H 0.0114 0.7346 0.129 0.22 Uiso 0.454(10) 1 calc PR B 4
H40F H 0.0521 0.8178 0.1794 0.22 Uiso 0.454(10) 1 calc PR B 4
H07 H -0.033(3) 0.958(3) 0.228(3) 0.106(17) Uiso 1 1 d . . .



#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_geom_special_details            
;
 All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell s.u.'s are taken
 into account individually in the estimation of s.u.'s in distances, angles
 and torsion angles; correlations between s.u.'s in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
V1 O2 1.7946(15) . ?
V1 O1 1.8021(15) . ?
V1 O5 1.9401(15) . ?
V1 O3 1.9826(16) . ?
V1 O6 2.0020(16) . ?
V1 N8 2.1922(18) . ?
O1 C1 1.354(3) . ?
O2 C15 1.344(3) . ?
O3 C17 1.288(3) . ?
O4 C17 1.234(3) . ?
O5 C35 1.286(3) . ?
O6 C37 1.279(3) . ?
O7 C39A 1.463(7) . ?
O7 C39B 1.520(10) . ?
O7 H07 0.81(5) . ?
N8 C7 1.499(3) . ?
N8 C16 1.500(3) . ?
N8 C9 1.507(3) . ?
C1 C6 1.396(3) . ?
C1 C2 1.403(3) . ?
C2 C3 1.399(3) . ?
C2 C18 1.533(3) . ?
C3 C4 1.397(3) . ?
C3 H3 0.93 . ?
C4 C5 1.393(3) . ?
C4 C22 1.531(3) . ?
C5 C6 1.383(3) . ?
C5 H5 0.93 . ?
C6 C7 1.504(3) . ?
C7 H7A 0.97 . ?
C7 H7B 0.97 . ?
C9 C10 1.497(3) . ?
C9 H9A 0.97 . ?
C9 H9B 0.97 . ?
C10 C11 1.387(3) . ?
C10 C15 1.398(3) . ?
C11 C12 1.388(3) . ?
C11 H11 0.93 . ?
C12 C13 1.395(4) . ?
C12 C30 1.526(4) . ?
C13 C14 1.387(4) . ?
C13 H13 0.93 . ?
C14 C15 1.409(3) . ?
C14 C26 1.531(4) . ?
C16 C17 1.518(3) . ?
C16 H16A 0.97 . ?
C16 H16B 0.97 . ?
C18 C20 1.530(3) . ?
C18 C21 1.540(3) . ?
C18 C19 1.540(4) . ?
C19 H19A 0.96 . ?
C19 H19B 0.96 . ?
C19 H19C 0.96 . ?
C20 H20A 0.96 . ?
C20 H20B 0.96 . ?
C20 H20C 0.96 . ?
C21 H21A 0.96 . ?
C21 H21B 0.96 . ?
C21 H21C 0.96 . ?
C22 C23 1.530(4) . ?
C22 C25 1.533(4) . ?
C22 C24 1.541(4) . ?
C23 H23A 0.96 . ?
C23 H23B 0.96 . ?
C23 H23C 0.96 . ?
C24 H24A 0.96 . ?
C24 H24B 0.96 . ?
C24 H24C 0.96 . ?
C25 H25A 0.96 . ?
C25 H25B 0.96 . ?
C25 H25C 0.96 . ?
C26 C27 1.524(4) . ?
C26 C29 1.533(4) . ?
C26 C28 1.540(4) . ?
C27 H27A 0.96 . ?
C27 H27B 0.96 . ?
C27 H27C 0.96 . ?
C28 H28A 0.96 . ?
C28 H28B 0.96 . ?
C28 H28C 0.96 . ?
C29 H29A 0.96 . ?
C29 H29B 0.96 . ?
C29 H29C 0.96 . ?
C30 C31A 1.449(6) . ?
C30 C32B 1.470(9) . ?
C30 C32A 1.506(6) . ?
C30 C33B 1.532(9) . ?
C30 C33A 1.619(5) . ?
C30 C31B 1.668(8) . ?
C31A H31A 0.96 . ?
C31A H31B 0.96 . ?
C31A H31C 0.96 . ?
C32A H32A 0.96 . ?
C32A H32B 0.96 . ?
C32A H32C 0.96 . ?
C33A H33A 0.96 . ?
C33A H33B 0.96 . ?
C33A H33C 0.96 . ?
C31B H31D 0.96 . ?
C31B H31E 0.96 . ?
C31B H31F 0.96 . ?
C32B H32D 0.96 . ?
C32B H32E 0.96 . ?
C32B H32F 0.96 . ?
C33B H33D 0.96 . ?
C33B H33E 0.96 . ?
C33B H33F 0.96 . ?
C34 C35 1.518(3) . ?
C34 H34A 0.96 . ?
C34 H34B 0.96 . ?
C34 H34C 0.96 . ?
C35 C36 1.372(4) . ?
C36 C37 1.395(4) . ?
C36 H36 0.93 . ?
C37 C38 1.495(3) . ?
C38 H38A 0.96 . ?
C38 H38B 0.96 . ?
C38 H38C 0.96 . ?
C39A C40A 1.501(11) . ?
C39A H39A 0.97 . ?
C39A H39B 0.97 . ?
C40A H40A 0.96 . ?
C40A H40B 0.96 . ?
C40A H40C 0.96 . ?
C39B C40B 1.296(13) . ?
C39B H39C 0.97 . ?
C39B H39D 0.97 . ?
C40B H40D 0.96 . ?
C40B H40E 0.96 . ?
C40B H40F 0.96 . ?

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
O2 V1 O1 170.75(7) . . ?
O2 V1 O5 96.64(7) . . ?
O1 V1 O5 92.55(7) . . ?
O2 V1 O3 90.17(7) . . ?
O1 V1 O3 90.40(7) . . ?
O5 V1 O3 93.18(7) . . ?
O2 V1 O6 88.90(7) . . ?
O1 V1 O6 89.99(7) . . ?
O5 V1 O6 90.18(7) . . ?
O3 V1 O6 176.60(7) . . ?
O2 V1 N8 85.56(7) . . ?
O1 V1 N8 85.40(7) . . ?
O5 V1 N8 173.96(7) . . ?
O3 V1 N8 81.17(7) . . ?
O6 V1 N8 95.50(7) . . ?
C1 O1 V1 142.47(14) . . ?
C15 O2 V1 142.25(13) . . ?
C17 O3 V1 120.21(15) . . ?
C35 O5 V1 125.90(16) . . ?
C37 O6 V1 126.20(15) . . ?
C39A O7 C39B 47.0(4) . . ?
C39A O7 H07 103(3) . . ?
C39B O7 H07 105(3) . . ?
C7 N8 C16 111.60(16) . . ?
C7 N8 C9 105.30(17) . . ?
C16 N8 C9 110.74(17) . . ?
C7 N8 V1 110.27(13) . . ?
C16 N8 V1 107.61(13) . . ?
C9 N8 V1 111.36(12) . . ?
O1 C1 C6 116.57(19) . . ?
O1 C1 C2 121.6(2) . . ?
C6 C1 C2 121.80(19) . . ?
C3 C2 C1 115.8(2) . . ?
C3 C2 C18 122.3(2) . . ?
C1 C2 C18 121.87(19) . . ?
C4 C3 C2 124.4(2) . . ?
C4 C3 H3 117.8 . . ?
C2 C3 H3 117.8 . . ?
C5 C4 C3 116.85(19) . . ?
C5 C4 C22 120.0(2) . . ?
C3 C4 C22 123.1(2) . . ?
C6 C5 C4 121.5(2) . . ?
C6 C5 H5 119.2 . . ?
C4 C5 H5 119.2 . . ?
C5 C6 C1 119.6(2) . . ?
C5 C6 C7 120.72(19) . . ?
C1 C6 C7 119.43(18) . . ?
N8 C7 C6 115.05(18) . . ?
N8 C7 H7A 108.5 . . ?
C6 C7 H7A 108.5 . . ?
N8 C7 H7B 108.5 . . ?
C6 C7 H7B 108.5 . . ?
H7A C7 H7B 107.5 . . ?
C10 C9 N8 115.36(18) . . ?
C10 C9 H9A 108.4 . . ?
N8 C9 H9A 108.4 . . ?
C10 C9 H9B 108.4 . . ?
N8 C9 H9B 108.4 . . ?
H9A C9 H9B 107.5 . . ?
C11 C10 C15 119.7(2) . . ?
C11 C10 C9 120.9(2) . . ?
C15 C10 C9 119.1(2) . . ?
C10 C11 C12 120.8(2) . . ?
C10 C11 H11 119.6 . . ?
C12 C11 H11 119.6 . . ?
C11 C12 C13 117.5(2) . . ?
C11 C12 C30 121.9(3) . . ?
C13 C12 C30 120.6(2) . . ?
C14 C13 C12 124.5(2) . . ?
C14 C13 H13 117.8 . . ?
C12 C13 H13 117.8 . . ?
C13 C14 C15 115.8(2) . . ?
C13 C14 C26 122.5(2) . . ?
C15 C14 C26 121.7(2) . . ?
O2 C15 C10 117.33(19) . . ?
O2 C15 C14 121.1(2) . . ?
C10 C15 C14 121.5(2) . . ?
N8 C16 C17 113.52(17) . . ?
N8 C16 H16A 108.9 . . ?
C17 C16 H16A 108.9 . . ?
N8 C16 H16B 108.9 . . ?
C17 C16 H16B 108.9 . . ?
H16A C16 H16B 107.7 . . ?
O4 C17 O3 124.5(2) . . ?
O4 C17 C16 118.1(2) . . ?
O3 C17 C16 117.4(2) . . ?
C20 C18 C2 112.02(19) . . ?
C20 C18 C21 107.4(2) . . ?
C2 C18 C21 109.64(19) . . ?
C20 C18 C19 107.6(2) . . ?
C2 C18 C19 110.9(2) . . ?
C21 C18 C19 109.3(2) . . ?
C18 C19 H19A 109.5 . . ?
C18 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C18 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C18 C20 H20A 109.5 . . ?
C18 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C18 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C18 C21 H21A 109.5 . . ?
C18 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C18 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C23 C22 C4 112.5(2) . . ?
C23 C22 C25 108.6(2) . . ?
C4 C22 C25 110.1(2) . . ?
C23 C22 C24 108.6(2) . . ?
C4 C22 C24 108.63(19) . . ?
C25 C22 C24 108.3(3) . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C22 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C22 C24 H24A 109.5 . . ?
C22 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C22 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C22 C25 H25A 109.5 . . ?
C22 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C22 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C27 C26 C14 110.38(19) . . ?
C27 C26 C29 107.0(2) . . ?
C14 C26 C29 112.1(2) . . ?
C27 C26 C28 110.4(3) . . ?
C14 C26 C28 108.7(2) . . ?
C29 C26 C28 108.2(2) . . ?
C26 C27 H27A 109.5 . . ?
C26 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C26 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C26 C28 H28A 109.5 . . ?
C26 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C26 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C26 C29 H29A 109.5 . . ?
C26 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C26 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C31A C30 C32B 127.2(5) . . ?
C31A C30 C32A 114.4(5) . . ?
C32B C30 C32A 49.2(5) . . ?
C31A C30 C12 114.8(3) . . ?
C32B C30 C12 118.0(5) . . ?
C32A C30 C12 106.7(3) . . ?
C31A C30 C33B 41.2(5) . . ?
C32B C30 C33B 116.6(6) . . ?
C32A C30 C33B 143.6(5) . . ?
C12 C30 C33B 108.9(4) . . ?
C31A C30 C33A 107.4(4) . . ?
C32B C30 C33A 56.4(5) . . ?
C32A C30 C33A 105.5(4) . . ?
C12 C30 C33A 107.5(3) . . ?
C33B C30 C33A 70.9(5) . . ?
C31A C30 C31B 58.8(4) . . ?
C32B C30 C31B 103.6(5) . . ?
C32A C30 C31B 61.4(4) . . ?
C12 C30 C31B 107.8(3) . . ?
C33B C30 C31B 99.8(6) . . ?
C33A C30 C31B 144.6(3) . . ?
C30 C31A H31A 109.5 . . ?
C30 C31A H31B 109.5 . . ?
C30 C31A H31C 109.5 . . ?
C30 C32A H32A 109.5 . . ?
C30 C32A H32B 109.5 . . ?
C30 C32A H32C 109.5 . . ?
C30 C33A H33A 109.5 . . ?
C30 C33A H33B 109.5 . . ?
C30 C33A H33C 109.5 . . ?
C30 C31B H31D 109.5 . . ?
C30 C31B H31E 109.5 . . ?
H31D C31B H31E 109.5 . . ?
C30 C31B H31F 109.5 . . ?
H31D C31B H31F 109.5 . . ?
H31E C31B H31F 109.5 . . ?
C30 C32B H32D 109.5 . . ?
C30 C32B H32E 109.5 . . ?
H32D C32B H32E 109.5 . . ?
C30 C32B H32F 109.5 . . ?
H32D C32B H32F 109.5 . . ?
H32E C32B H32F 109.5 . . ?
C30 C33B H33D 109.5 . . ?
C30 C33B H33E 109.5 . . ?
H33D C33B H33E 109.5 . . ?
C30 C33B H33F 109.5 . . ?
H33D C33B H33F 109.5 . . ?
H33E C33B H33F 109.5 . . ?
C35 C34 H34A 109.5 . . ?
C35 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
C35 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
O5 C35 C36 125.7(2) . . ?
O5 C35 C34 113.9(2) . . ?
C36 C35 C34 120.4(2) . . ?
C35 C36 C37 125.1(2) . . ?
C35 C36 H36 117.5 . . ?
C37 C36 H36 117.5 . . ?
O6 C37 C36 123.8(2) . . ?
O6 C37 C38 116.3(2) . . ?
C36 C37 C38 119.8(2) . . ?
C37 C38 H38A 109.5 . . ?
C37 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
C37 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
O7 C39A C40A 108.8(6) . . ?
O7 C39A H39A 109.9 . . ?
C40A C39A H39A 109.9 . . ?
O7 C39A H39B 109.9 . . ?
C40A C39A H39B 109.9 . . ?
H39A C39A H39B 108.3 . . ?
C40B C39B O7 118.7(11) . . ?
C40B C39B H39C 107.6 . . ?
O7 C39B H39C 107.6 . . ?
C40B C39B H39D 107.6 . . ?
O7 C39B H39D 107.6 . . ?
H39C C39B H39D 107.1 . . ?

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
O2 V1 O1 C1 -24.4(6) . . . . ?
O5 V1 O1 C1 162.3(2) . . . . ?
O3 V1 O1 C1 69.1(2) . . . . ?
O6 V1 O1 C1 -107.5(2) . . . . ?
N8 V1 O1 C1 -12.0(2) . . . . ?
O1 V1 O2 C15 27.7(6) . . . . ?
O5 V1 O2 C15 -159.0(2) . . . . ?
O3 V1 O2 C15 -65.8(2) . . . . ?
O6 V1 O2 C15 110.9(2) . . . . ?
N8 V1 O2 C15 15.3(2) . . . . ?
O2 V1 O3 C17 85.81(17) . . . . ?
O1 V1 O3 C17 -84.95(17) . . . . ?
O5 V1 O3 C17 -177.53(16) . . . . ?
O6 V1 O3 C17 11.6(13) . . . . ?
N8 V1 O3 C17 0.33(16) . . . . ?
O2 V1 O5 C35 -107.07(19) . . . . ?
O1 V1 O5 C35 71.85(19) . . . . ?
O3 V1 O5 C35 162.39(19) . . . . ?
O6 V1 O5 C35 -18.15(19) . . . . ?
N8 V1 O5 C35 141.8(6) . . . . ?
O2 V1 O6 C37 109.97(17) . . . . ?
O1 V1 O6 C37 -79.22(17) . . . . ?
O5 V1 O6 C37 13.33(17) . . . . ?
O3 V1 O6 C37 -175.8(11) . . . . ?
N8 V1 O6 C37 -164.60(17) . . . . ?
O2 V1 N8 C7 145.57(14) . . . . ?
O1 V1 N8 C7 -32.44(14) . . . . ?
O5 V1 N8 C7 -102.8(7) . . . . ?
O3 V1 N8 C7 -123.56(14) . . . . ?
O6 V1 N8 C7 57.11(14) . . . . ?
O2 V1 N8 C16 -92.48(14) . . . . ?
O1 V1 N8 C16 89.50(14) . . . . ?
O5 V1 N8 C16 19.1(8) . . . . ?
O3 V1 N8 C16 -1.62(13) . . . . ?
O6 V1 N8 C16 179.05(13) . . . . ?
O2 V1 N8 C9 29.06(14) . . . . ?
O1 V1 N8 C9 -148.96(15) . . . . ?
O5 V1 N8 C9 140.7(7) . . . . ?
O3 V1 N8 C9 119.93(15) . . . . ?
O6 V1 N8 C9 -59.41(15) . . . . ?
V1 O1 C1 C6 28.8(4) . . . . ?
V1 O1 C1 C2 -152.13(19) . . . . ?
O1 C1 C2 C3 -176.5(2) . . . . ?
C6 C1 C2 C3 2.6(3) . . . . ?
O1 C1 C2 C18 3.6(3) . . . . ?
C6 C1 C2 C18 -177.3(2) . . . . ?
C1 C2 C3 C4 -1.4(3) . . . . ?
C18 C2 C3 C4 178.5(2) . . . . ?
C2 C3 C4 C5 -1.0(4) . . . . ?
C2 C3 C4 C22 178.1(2) . . . . ?
C3 C4 C5 C6 2.4(3) . . . . ?
C22 C4 C5 C6 -176.8(2) . . . . ?
C4 C5 C6 C1 -1.3(3) . . . . ?
C4 C5 C6 C7 172.5(2) . . . . ?
O1 C1 C6 C5 177.8(2) . . . . ?
C2 C1 C6 C5 -1.3(3) . . . . ?
O1 C1 C6 C7 3.9(3) . . . . ?
C2 C1 C6 C7 -175.2(2) . . . . ?
C16 N8 C7 C6 -56.0(2) . . . . ?
C9 N8 C7 C6 -176.21(18) . . . . ?
V1 N8 C7 C6 63.6(2) . . . . ?
C5 C6 C7 N8 135.3(2) . . . . ?
C1 C6 C7 N8 -50.9(3) . . . . ?
C7 N8 C9 C10 179.68(18) . . . . ?
C16 N8 C9 C10 58.9(2) . . . . ?
V1 N8 C9 C10 -60.8(2) . . . . ?
N8 C9 C10 C11 -135.7(2) . . . . ?
N8 C9 C10 C15 50.8(3) . . . . ?
C15 C10 C11 C12 2.7(3) . . . . ?
C9 C10 C11 C12 -170.7(2) . . . . ?
C10 C11 C12 C13 -2.4(4) . . . . ?
C10 C11 C12 C30 176.8(2) . . . . ?
C11 C12 C13 C14 0.0(4) . . . . ?
C30 C12 C13 C14 -179.3(2) . . . . ?
C12 C13 C14 C15 2.0(4) . . . . ?
C12 C13 C14 C26 -178.7(2) . . . . ?
V1 O2 C15 C10 -30.1(3) . . . . ?
V1 O2 C15 C14 151.54(19) . . . . ?
C11 C10 C15 O2 -179.0(2) . . . . ?
C9 C10 C15 O2 -5.4(3) . . . . ?
C11 C10 C15 C14 -0.6(3) . . . . ?
C9 C10 C15 C14 173.0(2) . . . . ?
C13 C14 C15 O2 176.6(2) . . . . ?
C26 C14 C15 O2 -2.7(3) . . . . ?
C13 C14 C15 C10 -1.6(3) . . . . ?
C26 C14 C15 C10 179.0(2) . . . . ?
C7 N8 C16 C17 123.67(19) . . . . ?
C9 N8 C16 C17 -119.36(19) . . . . ?
V1 N8 C16 C17 2.6(2) . . . . ?
V1 O3 C17 O4 -178.18(18) . . . . ?
V1 O3 C17 C16 1.1(3) . . . . ?
N8 C16 C17 O4 176.8(2) . . . . ?
N8 C16 C17 O3 -2.6(3) . . . . ?
C3 C2 C18 C20 -3.5(3) . . . . ?
C1 C2 C18 C20 176.4(2) . . . . ?
C3 C2 C18 C21 115.6(2) . . . . ?
C1 C2 C18 C21 -64.5(3) . . . . ?
C3 C2 C18 C19 -123.7(2) . . . . ?
C1 C2 C18 C19 56.2(3) . . . . ?
C5 C4 C22 C23 -176.1(2) . . . . ?
C3 C4 C22 C23 4.8(3) . . . . ?
C5 C4 C22 C25 -54.8(3) . . . . ?
C3 C4 C22 C25 126.1(3) . . . . ?
C5 C4 C22 C24 63.6(3) . . . . ?
C3 C4 C22 C24 -115.5(3) . . . . ?
C13 C14 C26 C27 123.7(3) . . . . ?
C15 C14 C26 C27 -57.0(3) . . . . ?
C13 C14 C26 C29 4.5(4) . . . . ?
C15 C14 C26 C29 -176.2(2) . . . . ?
C13 C14 C26 C28 -115.1(3) . . . . ?
C15 C14 C26 C28 64.2(3) . . . . ?
C11 C12 C30 C31A 11.3(5) . . . . ?
C13 C12 C30 C31A -169.5(4) . . . . ?
C11 C12 C30 C32B -168.7(5) . . . . ?
C13 C12 C30 C32B 10.5(6) . . . . ?
C11 C12 C30 C32A -116.6(4) . . . . ?
C13 C12 C30 C32A 62.6(4) . . . . ?
C11 C12 C30 C33B 55.4(6) . . . . ?
C13 C12 C30 C33B -125.4(6) . . . . ?
C11 C12 C30 C33A 130.6(3) . . . . ?
C13 C12 C30 C33A -50.2(4) . . . . ?
C11 C12 C30 C31B -52.0(4) . . . . ?
C13 C12 C30 C31B 127.3(4) . . . . ?
V1 O5 C35 C36 13.2(4) . . . . ?
V1 O5 C35 C34 -167.32(18) . . . . ?
O5 C35 C36 C37 4.1(4) . . . . ?
C34 C35 C36 C37 -175.3(2) . . . . ?
V1 O6 C37 C36 -2.9(3) . . . . ?
V1 O6 C37 C38 178.64(15) . . . . ?
C35 C36 C37 O6 -9.4(4) . . . . ?
C35 C36 C37 C38 169.0(2) . . . . ?
C39B O7 C39A C40A 25.6(9) . . . . ?
C39A O7 C39B C40B 17.7(9) . . . . ?
_database_code_depnum_ccdc_archive 'CCDC 977973'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_2_v_24072012

_audit_creation_date             2012-07-25T13:12:19-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.3
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C33 H50 N O4 V, C2 H3 N'
_chemical_formula_sum            'C35 H53 N2 O4 V'
_chemical_formula_weight         616.73

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
loop_
_symmetry_equiv_pos_as_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                   12.5241(4)
_cell_length_b                   14.3021(4)
_cell_length_c                   19.6163(10)
_cell_angle_alpha                90
_cell_angle_beta                 100.670(4)
_cell_angle_gamma                90
_cell_volume                     3452.9(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    123(2)
_cell_measurement_reflns_used    8651
_cell_measurement_theta_min      3.0894
_cell_measurement_theta_max      76.575

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_description       block
_exptl_crystal_colour            red-brown
_exptl_crystal_size_max          0.2556
_exptl_crystal_size_mid          0.1686
_exptl_crystal_size_min          0.1172
_exptl_crystal_density_diffrn    1.186
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1328
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-4 -8 2 0.1033
4 8 -2 0.0343
-1 5 11 0.0772
1 -5 -11 0.0772
6 -1 -10 0.0381
-6 1 10 0.0791
2 4 10 0.0833
-2 -4 -10 0.0833
4 -8 1 0.1061
-4 8 -1 0.1061
0 -2 12 0.0684
8 0 0 0.0897
-8 0 0 0.0897

_exptl_special_details           
;
 ?
;

#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    2.693
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
        (compiled Jan 23 2012,18:06:46)
Analytical numeric absorption correction using a multifaceted crystal
                        model based on expressions derived by R.C. Clark & J.S.
        (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_absorpt_correction_T_min  0.671
_exptl_absorpt_correction_T_max  0.794

#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_ambient_temperature      123(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_radiation_monochromator  graphite
_diffrn_detector_area_resol_mean 10.3953
_diffrn_orient_matrix_ub_11      0.0558298
_diffrn_orient_matrix_ub_12      -0.0898834
_diffrn_orient_matrix_ub_13      0.0321808
_diffrn_orient_matrix_ub_21      -0.1105105
_diffrn_orient_matrix_ub_22      -0.0507376
_diffrn_orient_matrix_ub_23      -0.0128521
_diffrn_orient_matrix_ub_31      0.0188137
_diffrn_orient_matrix_ub_32      -0.0310653
_diffrn_orient_matrix_ub_33      -0.071936
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_reflns_av_R_equivalents  0.0244
_diffrn_reflns_av_unetI/netI     0.0278
_diffrn_reflns_number            16497
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         3.85
_diffrn_reflns_theta_max         67
_diffrn_reflns_theta_full        67
_diffrn_measured_fraction_theta_full 1
_diffrn_measured_fraction_theta_max 1
_reflns_number_total             6154
_reflns_number_gt                5687
_reflns_threshold_expression     >2σ(I)

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_data_collection       
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
        (compiled Jan 23 2012,18:06:46)
;
_computing_cell_refinement       
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
        (compiled Jan 23 2012,18:06:46)
;
_computing_data_reduction        
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
        (compiled Jan 23 2012,18:06:46)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'

#----------------------------------------------------------------------------#
#                   STRUCTURE SOLUTION
#----------------------------------------------------------------------------#

_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2σ(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0409P)²+1.5890P] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         6154
_refine_ls_number_parameters     393
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0373
_refine_ls_R_factor_gt           0.0343
_refine_ls_wR_factor_ref         0.0881
_refine_ls_wR_factor_gt          0.0859
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_restrained_S_all      1.019
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_diff_density_max         0.224
_refine_diff_density_min         -0.455
_refine_diff_density_rms         0.042

#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
V V 0.0687 2.1097 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
V1 V 0.16276(2) 0.403928(18) 0.708971(13) 0.01893(8) Uani 1 1 d . . .
O1 O 0.13954(9) 0.50768(8) 0.67852(6) 0.0254(2) Uani 1 1 d . . .
O2 O 0.30858(9) 0.40090(7) 0.71189(6) 0.0223(2) Uani 1 1 d . . .
O3 O 0.08781(9) 0.33507(8) 0.63944(6) 0.0227(2) Uani 1 1 d . . .
O4 O 0.10530(9) 0.41864(8) 0.78613(6) 0.0256(2) Uani 1 1 d . . .
N1 N 0.5639(2) 0.1357(2) 0.54341(13) 0.0760(7) Uani 1 1 d . . .
N8 N 0.19551(10) 0.25812(9) 0.76386(6) 0.0194(3) Uani 1 1 d . . .
C1 C 0.39278(12) 0.33950(11) 0.72209(8) 0.0204(3) Uani 1 1 d . . .
C2 C 0.47615(12) 0.34844(11) 0.68356(8) 0.0210(3) Uani 1 1 d . . .
C3 C 0.56639(12) 0.29002(11) 0.70208(8) 0.0217(3) Uani 1 1 d . . .
H3 H 0.6236 0.2962 0.6782 0.026 Uiso 1 1 calc R . .
C4 C 0.57535(12) 0.22279(11) 0.75466(8) 0.0209(3) Uani 1 1 d . . .
C5 C 0.48700(12) 0.21155(11) 0.78743(8) 0.0211(3) Uani 1 1 d . . .
H5 H 0.4886 0.1645 0.8204 0.025 Uiso 1 1 calc R . .
C6 C 0.39620(12) 0.26898(11) 0.77212(8) 0.0203(3) Uani 1 1 d . . .
C7 C 0.30390(12) 0.25866(11) 0.81043(8) 0.0210(3) Uani 1 1 d . . .
H7A H 0.313 0.2008 0.8367 0.025 Uiso 1 1 calc R . .
H7B H 0.3064 0.3098 0.8432 0.025 Uiso 1 1 calc R . .
C9 C 0.18998(13) 0.17847(11) 0.71490(8) 0.0219(3) Uani 1 1 d . . .
H9A H 0.2017 0.1208 0.7413 0.026 Uiso 1 1 calc R . .
H9B H 0.2483 0.1846 0.6888 0.026 Uiso 1 1 calc R . .
C10 C 0.08347(12) 0.17170(11) 0.66470(8) 0.0207(3) Uani 1 1 d . . .
C11 C 0.03286(13) 0.08551(11) 0.65182(8) 0.0215(3) Uani 1 1 d . . .
H11 H 0.0633 0.0333 0.6763 0.026 Uiso 1 1 calc R . .
C12 C -0.06271(13) 0.07543(11) 0.60294(8) 0.0219(3) Uani 1 1 d . . .
C13 C -0.10723(13) 0.15573(11) 0.56876(8) 0.0216(3) Uani 1 1 d . . .
H13 H -0.1721 0.15 0.5371 0.026 Uiso 1 1 calc R . .
C14 C -0.06000(12) 0.24434(11) 0.57930(7) 0.0193(3) Uani 1 1 d . . .
C15 C 0.03743(12) 0.25073(11) 0.62825(8) 0.0194(3) Uani 1 1 d . . .
C16 C 0.10927(12) 0.25322(11) 0.80563(8) 0.0225(3) Uani 1 1 d . . .
H16A H 0.1281 0.2072 0.8422 0.027 Uiso 1 1 calc R . .
H16B H 0.0413 0.2346 0.7766 0.027 Uiso 1 1 calc R . .
C17 C 0.09673(13) 0.34902(12) 0.83711(8) 0.0250(3) Uani 1 1 d . . .
H17 H 0.1553 0.3581 0.8772 0.03 Uiso 1 1 calc R . .
C18 C -0.01165(15) 0.35830(13) 0.86022(10) 0.0323(4) Uani 1 1 d . . .
H18A H -0.0146 0.4171 0.8834 0.048 Uiso 1 1 calc R . .
H18B H -0.0199 0.3082 0.8914 0.048 Uiso 1 1 calc R . .
H18C H -0.0692 0.3555 0.8205 0.048 Uiso 1 1 calc R . .
C19 C 0.46627(13) 0.41749(12) 0.62248(9) 0.0251(3) Uani 1 1 d . . .
C20 C 0.45430(15) 0.51853(12) 0.64671(10) 0.0317(4) Uani 1 1 d . . .
H20A H 0.4548 0.5606 0.6086 0.048 Uiso 1 1 calc R . .
H20B H 0.5137 0.5333 0.6836 0.048 Uiso 1 1 calc R . .
H20C H 0.387 0.5248 0.663 0.048 Uiso 1 1 calc R . .
C21 C 0.36699(15) 0.39128(14) 0.56687(9) 0.0326(4) Uani 1 1 d . . .
H21A H 0.3594 0.4355 0.5295 0.049 Uiso 1 1 calc R . .
H21B H 0.3027 0.3922 0.587 0.049 Uiso 1 1 calc R . .
H21C H 0.377 0.3298 0.5495 0.049 Uiso 1 1 calc R . .
C22 C 0.56690(16) 0.41415(14) 0.58874(11) 0.0382(4) Uani 1 1 d . . .
H22A H 0.5763 0.3519 0.5726 0.057 Uiso 1 1 calc R . .
H22B H 0.6297 0.4317 0.6222 0.057 Uiso 1 1 calc R . .
H22C H 0.5578 0.4567 0.5503 0.057 Uiso 1 1 calc R . .
C23 C 0.67578(13) 0.16000(11) 0.77474(8) 0.0238(3) Uani 1 1 d . . .
C24 C 0.76707(13) 0.18671(12) 0.73632(10) 0.0307(4) Uani 1 1 d . . .
H24A H 0.7425 0.1787 0.6873 0.046 Uiso 1 1 calc R . .
H24B H 0.829 0.1474 0.7516 0.046 Uiso 1 1 calc R . .
H24C H 0.787 0.2508 0.7459 0.046 Uiso 1 1 calc R . .
C25 C 0.64267(14) 0.05790(11) 0.75730(9) 0.0271(3) Uani 1 1 d . . .
H25A H 0.5847 0.0407 0.7807 0.041 Uiso 1 1 calc R . .
H25B H 0.7039 0.0177 0.7722 0.041 Uiso 1 1 calc R . .
H25C H 0.6187 0.0516 0.7081 0.041 Uiso 1 1 calc R . .
C26 C 0.71953(15) 0.16734(13) 0.85341(9) 0.0333(4) Uani 1 1 d . . .
H26A H 0.7417 0.2305 0.8649 0.05 Uiso 1 1 calc R . .
H26B H 0.7807 0.1263 0.866 0.05 Uiso 1 1 calc R . .
H26C H 0.6635 0.1498 0.8783 0.05 Uiso 1 1 calc R . .
C27 C -0.10964(13) 0.33006(11) 0.53797(8) 0.0227(3) Uani 1 1 d . . .
C28 C -0.03264(15) 0.36340(12) 0.49053(9) 0.0295(4) Uani 1 1 d . . .
H28A H -0.0647 0.4155 0.4633 0.044 Uiso 1 1 calc R . .
H28B H -0.0204 0.3134 0.4603 0.044 Uiso 1 1 calc R . .
H28C H 0.0353 0.3822 0.5183 0.044 Uiso 1 1 calc R . .
C29 C -0.21963(14) 0.30636(12) 0.49207(9) 0.0287(4) Uani 1 1 d . . .
H29A H -0.2689 0.2845 0.5206 0.043 Uiso 1 1 calc R . .
H29B H -0.2096 0.2585 0.4595 0.043 Uiso 1 1 calc R . .
H29C H -0.249 0.3613 0.4674 0.043 Uiso 1 1 calc R . .
C30 C -0.13011(15) 0.40998(12) 0.58642(9) 0.0306(4) Uani 1 1 d . . .
H30A H -0.1724 0.4579 0.5598 0.046 Uiso 1 1 calc R . .
H30B H -0.0619 0.4356 0.609 0.046 Uiso 1 1 calc R . .
H30C H -0.1688 0.3863 0.6207 0.046 Uiso 1 1 calc R . .
C31 C -0.11685(14) -0.02092(12) 0.59034(9) 0.0276(4) Uani 1 1 d . . .
C32 C -0.2080(2) -0.02193(16) 0.52709(13) 0.0629(8) Uani 1 1 d . . .
H32A H -0.1804 -0.0015 0.4871 0.094 Uiso 1 1 calc R . .
H32B H -0.2651 0.0194 0.5348 0.094 Uiso 1 1 calc R . .
H32C H -0.2362 -0.0843 0.5195 0.094 Uiso 1 1 calc R . .
C33 C -0.16298(19) -0.04764(14) 0.65451(12) 0.0446(5) Uani 1 1 d . . .
H33A H -0.1962 -0.1083 0.6478 0.067 Uiso 1 1 calc R . .
H33B H -0.2164 -0.0024 0.6617 0.067 Uiso 1 1 calc R . .
H33C H -0.1054 -0.049 0.6943 0.067 Uiso 1 1 calc R . .
C34 C -0.03358(18) -0.09457(13) 0.57941(12) 0.0432(5) Uani 1 1 d . . .
H34A H 0.0228 -0.0977 0.6198 0.065 Uiso 1 1 calc R . .
H34B H -0.0026 -0.078 0.5398 0.065 Uiso 1 1 calc R . .
H34C H -0.0686 -0.1544 0.5717 0.065 Uiso 1 1 calc R . .
C35 C 0.40514(17) 0.11380(16) 0.60984(11) 0.0444(5) Uani 1 1 d . . .
H35A H 0.3468 0.1551 0.5909 0.067 Uiso 1 1 calc R . .
H35B H 0.4303 0.1285 0.6579 0.067 Uiso 1 1 calc R . .
H35C H 0.3798 0.0503 0.6057 0.067 Uiso 1 1 calc R . .
C36 C 0.4935(2) 0.12506(17) 0.57221(11) 0.0489(5) Uani 1 1 d . . .



#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_geom_special_details            
;
 All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell s.u.'s are taken
 into account individually in the estimation of s.u.'s in distances, angles
 and torsion angles; correlations between s.u.'s in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
V1 O1 1.6059(11) . ?
V1 O3 1.7993(11) . ?
V1 O4 1.8046(11) . ?
V1 O2 1.8170(11) . ?
V1 N8 2.3479(13) . ?
O2 C1 1.3583(19) . ?
O3 C15 1.3601(19) . ?
O4 C17 1.429(2) . ?
N1 C36 1.141(3) . ?
N8 C16 1.4734(19) . ?
N8 C9 1.483(2) . ?
N8 C7 1.4894(19) . ?
C1 C6 1.402(2) . ?
C1 C2 1.404(2) . ?
C2 C3 1.398(2) . ?
C2 C19 1.540(2) . ?
C3 C4 1.399(2) . ?
C3 H3 0.93 . ?
C4 C5 1.388(2) . ?
C4 C23 1.536(2) . ?
C5 C6 1.390(2) . ?
C5 H5 0.93 . ?
C6 C7 1.498(2) . ?
C7 H7A 0.97 . ?
C7 H7B 0.97 . ?
C9 C10 1.507(2) . ?
C9 H9A 0.97 . ?
C9 H9B 0.97 . ?
C10 C11 1.388(2) . ?
C10 C15 1.403(2) . ?
C11 C12 1.396(2) . ?
C11 H11 0.93 . ?
C12 C13 1.393(2) . ?
C12 C31 1.536(2) . ?
C13 C14 1.398(2) . ?
C13 H13 0.93 . ?
C14 C15 1.409(2) . ?
C14 C27 1.536(2) . ?
C16 C17 1.523(2) . ?
C16 H16A 0.97 . ?
C16 H16B 0.97 . ?
C17 C18 1.514(2) . ?
C17 H17 0.98 . ?
C18 H18A 0.96 . ?
C18 H18B 0.96 . ?
C18 H18C 0.96 . ?
C19 C22 1.529(2) . ?
C19 C20 1.537(2) . ?
C19 C21 1.541(2) . ?
C20 H20A 0.96 . ?
C20 H20B 0.96 . ?
C20 H20C 0.96 . ?
C21 H21A 0.96 . ?
C21 H21B 0.96 . ?
C21 H21C 0.96 . ?
C22 H22A 0.96 . ?
C22 H22B 0.96 . ?
C22 H22C 0.96 . ?
C23 C24 1.530(2) . ?
C23 C25 1.539(2) . ?
C23 C26 1.543(2) . ?
C24 H24A 0.96 . ?
C24 H24B 0.96 . ?
C24 H24C 0.96 . ?
C25 H25A 0.96 . ?
C25 H25B 0.96 . ?
C25 H25C 0.96 . ?
C26 H26A 0.96 . ?
C26 H26B 0.96 . ?
C26 H26C 0.96 . ?
C27 C28 1.535(2) . ?
C27 C29 1.537(2) . ?
C27 C30 1.538(2) . ?
C28 H28A 0.96 . ?
C28 H28B 0.96 . ?
C28 H28C 0.96 . ?
C29 H29A 0.96 . ?
C29 H29B 0.96 . ?
C29 H29C 0.96 . ?
C30 H30A 0.96 . ?
C30 H30B 0.96 . ?
C30 H30C 0.96 . ?
C31 C32 1.523(3) . ?
C31 C34 1.525(3) . ?
C31 C33 1.528(3) . ?
C32 H32A 0.96 . ?
C32 H32B 0.96 . ?
C32 H32C 0.96 . ?
C33 H33A 0.96 . ?
C33 H33B 0.96 . ?
C33 H33C 0.96 . ?
C34 H34A 0.96 . ?
C34 H34B 0.96 . ?
C34 H34C 0.96 . ?
C35 C36 1.449(3) . ?
C35 H35A 0.96 . ?
C35 H35B 0.96 . ?
C35 H35C 0.96 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 V1 O3 100.99(5) . . ?
O1 V1 O4 97.55(6) . . ?
O3 V1 O4 117.81(5) . . ?
O1 V1 O2 98.37(5) . . ?
O3 V1 O2 113.02(5) . . ?
O4 V1 O2 122.07(5) . . ?
O1 V1 N8 174.56(5) . . ?
O3 V1 N8 83.33(5) . . ?
O4 V1 N8 77.40(5) . . ?
O2 V1 N8 82.83(5) . . ?
C1 O2 V1 140.21(10) . . ?
C15 O3 V1 140.27(10) . . ?
C17 O4 V1 126.79(10) . . ?
C16 N8 C9 111.87(12) . . ?
C16 N8 C7 109.74(12) . . ?
C9 N8 C7 109.22(12) . . ?
C16 N8 V1 102.32(9) . . ?
C9 N8 V1 113.70(9) . . ?
C7 N8 V1 109.79(9) . . ?
O2 C1 C6 119.36(14) . . ?
O2 C1 C2 119.77(14) . . ?
C6 C1 C2 120.86(14) . . ?
C3 C2 C1 116.85(14) . . ?
C3 C2 C19 122.01(14) . . ?
C1 C2 C19 121.11(14) . . ?
C2 C3 C4 123.56(14) . . ?
C2 C3 H3 118.2 . . ?
C4 C3 H3 118.2 . . ?
C5 C4 C3 117.31(14) . . ?
C5 C4 C23 119.91(14) . . ?
C3 C4 C23 122.74(14) . . ?
C4 C5 C6 121.46(14) . . ?
C4 C5 H5 119.3 . . ?
C6 C5 H5 119.3 . . ?
C5 C6 C1 119.61(14) . . ?
C5 C6 C7 120.65(14) . . ?
C1 C6 C7 119.70(14) . . ?
N8 C7 C6 113.14(12) . . ?
N8 C7 H7A 108.9 . . ?
C6 C7 H7A 108.9 . . ?
N8 C7 H7B 108.9 . . ?
C6 C7 H7B 108.9 . . ?
H7A C7 H7B 107.8 . . ?
N8 C9 C10 113.70(13) . . ?
N8 C9 H9A 108.8 . . ?
C10 C9 H9A 108.8 . . ?
N8 C9 H9B 108.8 . . ?
C10 C9 H9B 108.8 . . ?
H9A C9 H9B 107.7 . . ?
C11 C10 C15 119.48(14) . . ?
C11 C10 C9 119.68(14) . . ?
C15 C10 C9 120.77(14) . . ?
C10 C11 C12 121.43(14) . . ?
C10 C11 H11 119.3 . . ?
C12 C11 H11 119.3 . . ?
C13 C12 C11 117.48(14) . . ?
C13 C12 C31 122.47(14) . . ?
C11 C12 C31 120.01(14) . . ?
C12 C13 C14 123.74(14) . . ?
C12 C13 H13 118.1 . . ?
C14 C13 H13 118.1 . . ?
C13 C14 C15 116.69(14) . . ?
C13 C14 C27 121.77(13) . . ?
C15 C14 C27 121.51(14) . . ?
O3 C15 C10 119.85(13) . . ?
O3 C15 C14 119.00(13) . . ?
C10 C15 C14 121.15(14) . . ?
N8 C16 C17 108.91(13) . . ?
N8 C16 H16A 109.9 . . ?
C17 C16 H16A 109.9 . . ?
N8 C16 H16B 109.9 . . ?
C17 C16 H16B 109.9 . . ?
H16A C16 H16B 108.3 . . ?
O4 C17 C18 109.63(13) . . ?
O4 C17 C16 108.44(12) . . ?
C18 C17 C16 111.45(14) . . ?
O4 C17 H17 109.1 . . ?
C18 C17 H17 109.1 . . ?
C16 C17 H17 109.1 . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C17 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C22 C19 C20 107.38(14) . . ?
C22 C19 C2 111.27(13) . . ?
C20 C19 C2 111.15(14) . . ?
C22 C19 C21 107.92(15) . . ?
C20 C19 C21 109.60(14) . . ?
C2 C19 C21 109.45(13) . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C19 C21 H21A 109.5 . . ?
C19 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C19 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C19 C22 H22A 109.5 . . ?
C19 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C19 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C24 C23 C4 112.26(13) . . ?
C24 C23 C25 108.82(14) . . ?
C4 C23 C25 108.88(13) . . ?
C24 C23 C26 108.45(14) . . ?
C4 C23 C26 109.81(13) . . ?
C25 C23 C26 108.56(14) . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C23 C25 H25A 109.5 . . ?
C23 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C23 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C23 C26 H26A 109.5 . . ?
C23 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C23 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C28 C27 C14 109.24(13) . . ?
C28 C27 C29 107.99(13) . . ?
C14 C27 C29 111.37(13) . . ?
C28 C27 C30 109.82(14) . . ?
C14 C27 C30 111.37(13) . . ?
C29 C27 C30 106.97(13) . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C27 C29 H29A 109.5 . . ?
C27 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C27 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C27 C30 H30A 109.5 . . ?
C27 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C27 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C32 C31 C34 107.94(18) . . ?
C32 C31 C33 109.15(19) . . ?
C34 C31 C33 108.42(16) . . ?
C32 C31 C12 112.45(15) . . ?
C34 C31 C12 110.45(15) . . ?
C33 C31 C12 108.36(14) . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C31 C33 H33A 109.5 . . ?
C31 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
C31 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C31 C34 H34A 109.5 . . ?
C31 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
C31 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C36 C35 H35A 109.5 . . ?
C36 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
C36 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
N1 C36 C35 178.5(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
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O1 V1 O2 C1 -169.48(16) . . . . ?
O3 V1 O2 C1 -63.71(16) . . . . ?
O4 V1 O2 C1 86.11(16) . . . . ?
N8 V1 O2 C1 15.88(16) . . . . ?
O1 V1 O3 C15 -154.46(15) . . . . ?
O4 V1 O3 C15 -49.75(17) . . . . ?
O2 V1 O3 C15 101.45(15) . . . . ?
N8 V1 O3 C15 22.19(15) . . . . ?
O1 V1 O4 C17 178.04(12) . . . . ?
O3 V1 O4 C17 71.35(13) . . . . ?
O2 V1 O4 C17 -77.11(13) . . . . ?
N8 V1 O4 C17 -4.03(12) . . . . ?
O1 V1 N8 C16 47.5(6) . . . . ?
O3 V1 N8 C16 -95.16(9) . . . . ?
O4 V1 N8 C16 25.34(9) . . . . ?
O2 V1 N8 C16 150.54(9) . . . . ?
O1 V1 N8 C9 168.3(5) . . . . ?
O3 V1 N8 C9 25.66(10) . . . . ?
O4 V1 N8 C9 146.16(10) . . . . ?
O2 V1 N8 C9 -88.65(10) . . . . ?
O1 V1 N8 C7 -69.0(6) . . . . ?
O3 V1 N8 C7 148.35(10) . . . . ?
O4 V1 N8 C7 -91.15(10) . . . . ?
O2 V1 N8 C7 34.05(10) . . . . ?
V1 O2 C1 C6 -38.4(2) . . . . ?
V1 O2 C1 C2 142.87(13) . . . . ?
O2 C1 C2 C3 172.81(14) . . . . ?
C6 C1 C2 C3 -5.9(2) . . . . ?
O2 C1 C2 C19 -9.0(2) . . . . ?
C6 C1 C2 C19 172.31(14) . . . . ?
C1 C2 C3 C4 2.0(2) . . . . ?
C19 C2 C3 C4 -176.24(15) . . . . ?
C2 C3 C4 C5 3.1(2) . . . . ?
C2 C3 C4 C23 -179.32(15) . . . . ?
C3 C4 C5 C6 -4.3(2) . . . . ?
C23 C4 C5 C6 177.99(14) . . . . ?
C4 C5 C6 C1 0.5(2) . . . . ?
C4 C5 C6 C7 -177.11(14) . . . . ?
O2 C1 C6 C5 -173.93(14) . . . . ?
C2 C1 C6 C5 4.8(2) . . . . ?
O2 C1 C6 C7 3.7(2) . . . . ?
C2 C1 C6 C7 -177.53(14) . . . . ?
C16 N8 C7 C6 -176.76(13) . . . . ?
C9 N8 C7 C6 60.27(16) . . . . ?
V1 N8 C7 C6 -65.04(14) . . . . ?
C5 C6 C7 N8 -133.60(15) . . . . ?
C1 C6 C7 N8 48.76(19) . . . . ?
C16 N8 C9 C10 58.77(17) . . . . ?
C7 N8 C9 C10 -179.53(12) . . . . ?
V1 N8 C9 C10 -56.53(15) . . . . ?
N8 C9 C10 C11 -135.36(14) . . . . ?
N8 C9 C10 C15 47.76(19) . . . . ?
C15 C10 C11 C12 0.4(2) . . . . ?
C9 C10 C11 C12 -176.47(14) . . . . ?
C10 C11 C12 C13 -1.7(2) . . . . ?
C10 C11 C12 C31 -179.64(14) . . . . ?
C11 C12 C13 C14 1.9(2) . . . . ?
C31 C12 C13 C14 179.81(14) . . . . ?
C12 C13 C14 C15 -0.8(2) . . . . ?
C12 C13 C14 C27 177.26(14) . . . . ?
V1 O3 C15 C10 -38.2(2) . . . . ?
V1 O3 C15 C14 142.52(13) . . . . ?
C11 C10 C15 O3 -178.53(13) . . . . ?
C9 C10 C15 O3 -1.6(2) . . . . ?
C11 C10 C15 C14 0.7(2) . . . . ?
C9 C10 C15 C14 177.58(14) . . . . ?
C13 C14 C15 O3 178.71(13) . . . . ?
C27 C14 C15 O3 0.6(2) . . . . ?
C13 C14 C15 C10 -0.5(2) . . . . ?
C27 C14 C15 C10 -178.61(13) . . . . ?
C9 N8 C16 C17 -162.40(12) . . . . ?
C7 N8 C16 C17 76.21(15) . . . . ?
V1 N8 C16 C17 -40.32(13) . . . . ?
V1 O4 C17 C18 -140.12(12) . . . . ?
V1 O4 C17 C16 -18.23(18) . . . . ?
N8 C16 C17 O4 40.49(16) . . . . ?
N8 C16 C17 C18 161.25(13) . . . . ?
C3 C2 C19 C22 -1.7(2) . . . . ?
C1 C2 C19 C22 -179.80(15) . . . . ?
C3 C2 C19 C20 -121.27(17) . . . . ?
C1 C2 C19 C20 60.6(2) . . . . ?
C3 C2 C19 C21 117.53(17) . . . . ?
C1 C2 C19 C21 -60.6(2) . . . . ?
C5 C4 C23 C24 -176.52(14) . . . . ?
C3 C4 C23 C24 5.9(2) . . . . ?
C5 C4 C23 C25 62.93(19) . . . . ?
C3 C4 C23 C25 -114.62(16) . . . . ?
C5 C4 C23 C26 -55.8(2) . . . . ?
C3 C4 C23 C26 126.65(16) . . . . ?
C13 C14 C27 C28 -113.08(16) . . . . ?
C15 C14 C27 C28 64.91(18) . . . . ?
C13 C14 C27 C29 6.1(2) . . . . ?
C15 C14 C27 C29 -175.89(14) . . . . ?
C13 C14 C27 C30 125.44(16) . . . . ?
C15 C14 C27 C30 -56.57(19) . . . . ?
C13 C12 C31 C32 12.2(2) . . . . ?
C11 C12 C31 C32 -169.99(19) . . . . ?
C13 C12 C31 C34 132.81(17) . . . . ?
C11 C12 C31 C34 -49.3(2) . . . . ?
C13 C12 C31 C33 -108.57(18) . . . . ?
C11 C12 C31 C33 69.3(2) . . . . ?
_database_code_depnum_ccdc_archive 'CCDC 977974'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_3_vt-1
_audit_creation_date             2013-12-02
_audit_creation_method           
;
Olex2 1.2
(compiled 2013.11.15 svn.r2834 for OlexSys, GUI svn.r4720)
;
_shelxl_version_number           2013-4
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C34 H52 N O5 V'
_chemical_formula_sum            'C34 H52 N O5 V'
_chemical_formula_weight         605.70
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C32 H51 N1 O5 V1'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
V V 0.0687 2.1097 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_cell_length_a                   10.8297(3)
_cell_length_b                   10.4967(4)
_cell_length_c                   29.3356(10)
_cell_angle_alpha                90
_cell_angle_beta                 93.008(3)
_cell_angle_gamma                90
_cell_volume                     3330.16(19)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    4536
_cell_measurement_temperature    123.01(10)
_cell_measurement_theta_max      76.2520
_cell_measurement_theta_min      4.5090
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    2.797
_exptl_absorpt_correction_T_max  0.924
_exptl_absorpt_correction_T_min  0.683
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.208
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             1304
_exptl_crystal_size_max          0.2103
_exptl_crystal_size_mid          0.1124
_exptl_crystal_size_min          0.0297
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0368
_diffrn_reflns_av_unetI/netI     0.0608
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       3
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            11251
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         70.979
_diffrn_reflns_theta_min         3.017
_diffrn_ambient_temperature      123.01(10)
_diffrn_detector_area_resol_mean 5.1977
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      0.0740087000
_diffrn_orient_matrix_UB_12      -0.0085825000
_diffrn_orient_matrix_UB_13      0.0462284000
_diffrn_orient_matrix_UB_21      -0.1181402000
_diffrn_orient_matrix_UB_22      0.0298656000
_diffrn_orient_matrix_UB_23      0.0249646000
_diffrn_orient_matrix_UB_31      -0.0290190000
_diffrn_orient_matrix_UB_32      -0.1434692000
_diffrn_orient_matrix_UB_33      0.0025261000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5588
_reflns_number_total             6451
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         0.866
_refine_diff_density_min         -0.466
_refine_diff_density_rms         0.109
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.109
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     404
_refine_ls_number_reflns         6451
_refine_ls_number_restraints     34
_refine_ls_R_factor_all          0.0882
_refine_ls_R_factor_gt           0.0765
_refine_ls_restrained_S_all      1.110
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0933P)²+12.7536P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2104
_refine_ls_wR_factor_ref         0.2262
_refine_special_details          
;
 Refined as a 2-component twin.
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C34B-C32 = C34A-C32 = C35B-C32 = C35A-C32
 1.53 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C35B \\sim C35A: within 1.7A with sigma of 0.003 and sigma for terminal atoms
of 0.01
Uanis(C34B) \\sim Ueq, Uanis(C34A) \\sim Ueq, Uanis(C35B) \\sim Ueq,
Uanis(C35A) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.006
4. Others
 Sof(C34B)=Sof(H34D)=Sof(H34E)=Sof(H34F)=Sof(C35B)=Sof(H35D)=Sof(H35E)=
 Sof(H35F)=1-FVAR(1)
 Sof(C34A)=Sof(H34A)=Sof(H34B)=Sof(H34C)=Sof(C35A)=Sof(H35A)=Sof(H35B)=
 Sof(H35C)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C9(H9A,H9B), C19(H19A,H19B), C18(H18A,H18B), C17(H17A,H17B),
 C16(H16A,H16B)
5.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C3(H3), C11(H11), C13(H13)
5.c Idealised Me refined as rotating group:
 C25(H25A,H25B,H25C), C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C21(H21A,H21B,
 H21C), C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C33(H33A,H33B,H33C),
 C34A(H34A,H34B,H34C), C34B(H34D,H34E,H34F), C35A(H35A,H35B,H35C), C35B(H35D,
 H35E,H35F), C29(H29A,H29B,H29C), C30(H30A,H30B,H30C), C31(H31A,H31B,H31C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
V1 V 0.49131(6) 0.24086(7) 0.24945(2) 0.0131(2) Uani 1 1 d . . . . .
O1 O 0.5489(3) 0.1013(3) 0.25457(11) 0.0193(7) Uani 1 1 d . . . . .
O2 O 0.4945(3) 0.2533(3) 0.18624(10) 0.0173(6) Uani 1 1 d . . . . .
O3 O 0.5130(3) 0.2904(3) 0.31147(10) 0.0172(6) Uani 1 1 d . . . . .
O5 O 0.3250(3) 0.2253(3) 0.25316(11) 0.0186(6) Uani 1 1 d . . . . .
O4 O 0.4244(3) 0.4401(3) 0.23701(11) 0.0194(7) Uani 1 1 d . . . . .
N8 N 0.6646(3) 0.3536(3) 0.24456(12) 0.0147(7) Uani 1 1 d . . . . .
C7 C 0.7537(4) 0.2834(4) 0.21659(15) 0.0164(9) Uani 1 1 d . . . . .
H7A H 0.7886 0.2123 0.2353 0.020 Uiso 1 1 calc R . . . .
H7B H 0.8227 0.3420 0.2107 0.020 Uiso 1 1 calc R . . . .
C6 C 0.7065(4) 0.2289(4) 0.17112(15) 0.0152(8) Uani 1 1 d . . . . .
C5 C 0.7950(4) 0.1914(4) 0.14089(15) 0.0172(9) Uani 1 1 d . . . . .
H5 H 0.8799 0.2058 0.1490 0.021 Uiso 1 1 calc R . . . .
C4 C 0.7625(4) 0.1336(4) 0.09940(16) 0.0183(9) Uani 1 1 d . . . . .
C3 C 0.6361(4) 0.1144(4) 0.08895(15) 0.0172(9) Uani 1 1 d . . . . .
H3 H 0.6125 0.0736 0.0609 0.021 Uiso 1 1 calc R . . . .
C2 C 0.5428(4) 0.1514(4) 0.11708(15) 0.0157(8) Uani 1 1 d . . . . .
C1 C 0.5811(4) 0.2108(4) 0.15888(15) 0.0163(9) Uani 1 1 d . . . . .
C9 C 0.7318(4) 0.3845(4) 0.28969(15) 0.0171(9) Uani 1 1 d . . . . .
H9A H 0.8194 0.4030 0.2841 0.020 Uiso 1 1 calc R . . . .
H9B H 0.6955 0.4630 0.3021 0.020 Uiso 1 1 calc R . . . .
C10 C 0.7280(4) 0.2816(4) 0.32519(15) 0.0166(9) Uani 1 1 d . . . . .
C11 C 0.8335(4) 0.2376(4) 0.34930(15) 0.0182(9) Uani 1 1 d . . . . .
H11 H 0.9127 0.2665 0.3415 0.022 Uiso 1 1 calc R . . . .
C12 C 0.8232(4) 0.1508(4) 0.38508(16) 0.0208(10) Uani 1 1 d . . . . .
C13 C 0.7057(5) 0.1129(5) 0.39558(16) 0.0221(10) Uani 1 1 d . . . . .
H13 H 0.6988 0.0533 0.4197 0.026 Uiso 1 1 calc R . . . .
C14 C 0.5954(4) 0.1565(5) 0.37307(16) 0.0205(9) Uani 1 1 d . . . . .
C15 C 0.6102(4) 0.2409(4) 0.33666(15) 0.0165(8) Uani 1 1 d . . . . .
C24 C 0.8569(4) 0.0910(5) 0.06533(16) 0.0213(10) Uani 1 1 d . . . . .
C25 C 0.9901(5) 0.1054(7) 0.0848(2) 0.0354(13) Uani 1 1 d . . . . .
H25A H 1.0010 0.0559 0.1131 0.053 Uiso 1 1 calc GR . . . .
H25B H 1.0072 0.1955 0.0914 0.053 Uiso 1 1 calc GR . . . .
H25C H 1.0473 0.0742 0.0626 0.053 Uiso 1 1 calc GR . . . .
C26 C 0.8402(5) 0.1734(6) 0.02199(18) 0.0312(12) Uani 1 1 d . . . . .
H26A H 0.8541 0.2631 0.0299 0.047 Uiso 1 1 calc GR . . . .
H26B H 0.7560 0.1627 0.0086 0.047 Uiso 1 1 calc GR . . . .
H26C H 0.8998 0.1468 -0.0001 0.047 Uiso 1 1 calc GR . . . .
C27 C 0.8343(5) -0.0501(5) 0.05282(18) 0.0257(10) Uani 1 1 d . . . . .
H27A H 0.7524 -0.0592 0.0373 0.039 Uiso 1 1 calc GR . . . .
H27B H 0.8383 -0.1017 0.0807 0.039 Uiso 1 1 calc GR . . . .
H27C H 0.8977 -0.0789 0.0325 0.039 Uiso 1 1 calc GR . . . .
C20 C 0.4062(4) 0.1254(4) 0.10449(16) 0.0192(9) Uani 1 1 d . . . . .
C21 C 0.3860(5) 0.0636(5) 0.05745(17) 0.0268(11) Uani 1 1 d . . . . .
H21A H 0.4280 -0.0190 0.0574 0.040 Uiso 1 1 calc GR . . . .
H21B H 0.4197 0.1190 0.0343 0.040 Uiso 1 1 calc GR . . . .
H21C H 0.2972 0.0513 0.0506 0.040 Uiso 1 1 calc GR . . . .
C22 C 0.3303(4) 0.2488(5) 0.10350(19) 0.0265(10) Uani 1 1 d . . . . .
H22A H 0.3605 0.3062 0.0802 0.040 Uiso 1 1 calc GR . . . .
H22B H 0.3387 0.2903 0.1334 0.040 Uiso 1 1 calc GR . . . .
H22C H 0.2431 0.2288 0.0962 0.040 Uiso 1 1 calc GR . . . .
C23 C 0.3554(5) 0.0332(5) 0.13962(17) 0.0265(11) Uani 1 1 d . . . . .
H23A H 0.3667 0.0701 0.1702 0.040 Uiso 1 1 calc GR . . . .
H23B H 0.3999 -0.0480 0.1386 0.040 Uiso 1 1 calc GR . . . .
H23C H 0.2671 0.0186 0.1324 0.040 Uiso 1 1 calc GR . . . .
C32 C 0.9364(4) 0.1087(5) 0.41483(17) 0.0252(10) Uani 1 1 d D . . . .
C33 C 0.9157(5) -0.0210(5) 0.4372(2) 0.0319(12) Uani 1 1 d . . . . .
H33A H 0.8934 -0.0841 0.4136 0.048 Uiso 1 1 calc GR . . . .
H33B H 0.8487 -0.0140 0.4583 0.048 Uiso 1 1 calc GR . . . .
H33C H 0.9918 -0.0478 0.4541 0.048 Uiso 1 1 calc GR . . . .
C34A C 0.977(2) 0.2155(15) 0.4474(7) 0.037(4) Uani 0.52(5) 1 d D U P A 1
H34A H 1.0545 0.1918 0.4638 0.055 Uiso 0.52(5) 1 calc GR . P A 1
H34B H 0.9128 0.2296 0.4692 0.055 Uiso 0.52(5) 1 calc GR . P A 1
H34C H 0.9890 0.2937 0.4300 0.055 Uiso 0.52(5) 1 calc GR . P A 1
C34B C 0.940(2) 0.2016(14) 0.4572(5) 0.024(4) Uani 0.48(5) 1 d D U P A 2
H34D H 1.0131 0.1837 0.4771 0.036 Uiso 0.48(5) 1 calc GR . P A 2
H34E H 0.8652 0.1888 0.4743 0.036 Uiso 0.48(5) 1 calc GR . P A 2
H34F H 0.9425 0.2900 0.4465 0.036 Uiso 0.48(5) 1 calc GR . P A 2
C35A C 1.0499(14) 0.083(2) 0.3844(6) 0.028(3) Uani 0.52(5) 1 d D U P A 1
H35A H 1.0269 0.0193 0.3611 0.042 Uiso 0.52(5) 1 calc GR . P A 1
H35B H 1.1201 0.0518 0.4037 0.042 Uiso 0.52(5) 1 calc GR . P A 1
H35C H 1.0731 0.1626 0.3695 0.042 Uiso 0.52(5) 1 calc GR . P A 1
C35B C 1.0562(16) 0.115(3) 0.3911(8) 0.034(4) Uani 0.48(5) 1 d D U P A 2
H35D H 1.0497 0.0628 0.3633 0.051 Uiso 0.48(5) 1 calc GR . P A 2
H35E H 1.1236 0.0827 0.4115 0.051 Uiso 0.48(5) 1 calc GR . P A 2
H35F H 1.0733 0.2036 0.3829 0.051 Uiso 0.48(5) 1 calc GR . P A 2
C28 C 0.4672(5) 0.1153(5) 0.38785(17) 0.0251(10) Uani 1 1 d . . . . .
C29 C 0.4767(6) 0.0409(7) 0.4329(2) 0.0453(16) Uani 1 1 d . . . . .
H29A H 0.5195 0.0929 0.4565 0.068 Uiso 1 1 calc GR . . . .
H29B H 0.5232 -0.0380 0.4287 0.068 Uiso 1 1 calc GR . . . .
H29C H 0.3935 0.0201 0.4422 0.068 Uiso 1 1 calc GR . . . .
C30 C 0.3861(5) 0.2326(6) 0.3951(2) 0.0332(12) Uani 1 1 d . . . . .
H30A H 0.3692 0.2759 0.3658 0.050 Uiso 1 1 calc GR . . . .
H30B H 0.4293 0.2910 0.4165 0.050 Uiso 1 1 calc GR . . . .
H30C H 0.3080 0.2058 0.4075 0.050 Uiso 1 1 calc GR . . . .
C31 C 0.4045(5) 0.0286(6) 0.35115(19) 0.0316(12) Uani 1 1 d . . . . .
H31A H 0.4561 -0.0466 0.3468 0.047 Uiso 1 1 calc GR . . . .
H31B H 0.3940 0.0755 0.3223 0.047 Uiso 1 1 calc GR . . . .
H31C H 0.3234 0.0018 0.3610 0.047 Uiso 1 1 calc GR . . . .
C19 C 0.2458(4) 0.3330(5) 0.2512(2) 0.0275(11) Uani 1 1 d . . . . .
H19A H 0.1793 0.3212 0.2727 0.033 Uiso 1 1 calc R . . . .
H19B H 0.2070 0.3411 0.2200 0.033 Uiso 1 1 calc R . . . .
C18 C 0.3169(4) 0.4530(5) 0.26335(19) 0.0247(10) Uani 1 1 d . . . . .
H18A H 0.2688 0.5300 0.2544 0.030 Uiso 1 1 calc R . . . .
H18B H 0.3397 0.4568 0.2964 0.030 Uiso 1 1 calc R . . . .
C17 C 0.5184(4) 0.5348(4) 0.24192(16) 0.0199(9) Uani 1 1 d . . . . .
H17A H 0.5363 0.5555 0.2745 0.024 Uiso 1 1 calc R . . . .
H17B H 0.4928 0.6136 0.2255 0.024 Uiso 1 1 calc R . . . .
C16 C 0.6316(4) 0.4757(4) 0.22111(16) 0.0185(9) Uani 1 1 d . . . . .
H16A H 0.6135 0.4599 0.1882 0.022 Uiso 1 1 calc R . . . .
H16B H 0.7022 0.5355 0.2243 0.022 Uiso 1 1 calc R . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
V1 O1 1.597(3) . ?
V1 O2 1.861(3) . ?
V1 O3 1.895(3) . ?
V1 O5 1.817(3) . ?
V1 O4 2.237(3) . ?
V1 N8 2.230(4) . ?
O2 C1 1.343(5) . ?
O3 C15 1.358(5) . ?
O5 C19 1.418(6) . ?
O4 C18 1.437(6) . ?
O4 C17 1.424(6) . ?
N8 C7 1.493(5) . ?
N8 C9 1.512(5) . ?
N8 C16 1.490(6) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C7 C6 1.516(6) . ?
C6 C5 1.396(6) . ?
C6 C1 1.399(6) . ?
C5 H5 0.9500 . ?
C5 C4 1.388(7) . ?
C4 C3 1.402(6) . ?
C4 C24 1.533(6) . ?
C3 H3 0.9500 . ?
C3 C2 1.392(6) . ?
C2 C1 1.418(6) . ?
C2 C20 1.530(6) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C9 C10 1.503(6) . ?
C10 C11 1.391(6) . ?
C10 C15 1.403(6) . ?
C11 H11 0.9500 . ?
C11 C12 1.399(7) . ?
C12 C13 1.383(7) . ?
C12 C32 1.532(6) . ?
C13 H13 0.9500 . ?
C13 C14 1.411(7) . ?
C14 C15 1.403(6) . ?
C14 C28 1.538(7) . ?
C24 C25 1.531(7) . ?
C24 C26 1.541(7) . ?
C24 C27 1.542(7) . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C20 C21 1.530(7) . ?
C20 C22 1.534(7) . ?
C20 C23 1.537(6) . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C32 C33 1.533(7) . ?
C32 C34A 1.521(12) . ?
C32 C34B 1.579(12) . ?
C32 C35A 1.579(14) . ?
C32 C35B 1.506(15) . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C34A H34A 0.9800 . ?
C34A H34B 0.9800 . ?
C34A H34C 0.9800 . ?
C34B H34D 0.9800 . ?
C34B H34E 0.9800 . ?
C34B H34F 0.9800 . ?
C35A H35A 0.9800 . ?
C35A H35B 0.9800 . ?
C35A H35C 0.9800 . ?
C35B H35D 0.9800 . ?
C35B H35E 0.9800 . ?
C35B H35F 0.9800 . ?
C28 C29 1.534(7) . ?
C28 C30 1.533(8) . ?
C28 C31 1.540(7) . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C19 C18 1.510(7) . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C17 C16 1.529(6) . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 V1 O2 97.51(16) . . ?
O1 V1 O3 97.68(16) . . ?
O1 V1 O5 107.18(16) . . ?
O1 V1 O4 174.27(15) . . ?
O1 V1 N8 99.61(15) . . ?
O2 V1 O3 158.36(14) . . ?
O2 V1 O4 78.14(13) . . ?
O2 V1 N8 80.74(14) . . ?
O3 V1 O4 85.56(13) . . ?
O3 V1 N8 81.60(14) . . ?
O5 V1 O2 97.83(14) . . ?
O5 V1 O3 92.30(14) . . ?
O5 V1 O4 77.32(13) . . ?
O5 V1 N8 153.10(15) . . ?
N8 V1 O4 76.11(13) . . ?
C1 O2 V1 128.5(3) . . ?
C15 O3 V1 118.1(3) . . ?
C19 O5 V1 121.7(3) . . ?
C18 O4 V1 105.4(3) . . ?
C17 O4 V1 114.3(3) . . ?
C17 O4 C18 118.3(4) . . ?
C7 N8 V1 110.1(3) . . ?
C7 N8 C9 107.0(3) . . ?
C9 N8 V1 115.2(3) . . ?
C16 N8 V1 107.7(3) . . ?
C16 N8 C7 108.5(3) . . ?
C16 N8 C9 108.2(3) . . ?
N8 C7 H7A 107.8 . . ?
N8 C7 H7B 107.8 . . ?
N8 C7 C6 118.2(4) . . ?
H7A C7 H7B 107.1 . . ?
C6 C7 H7A 107.8 . . ?
C6 C7 H7B 107.8 . . ?
C5 C6 C7 117.0(4) . . ?
C5 C6 C1 119.2(4) . . ?
C1 C6 C7 123.7(4) . . ?
C6 C5 H5 119.0 . . ?
C4 C5 C6 122.0(4) . . ?
C4 C5 H5 119.0 . . ?
C5 C4 C3 117.0(4) . . ?
C5 C4 C24 123.5(4) . . ?
C3 C4 C24 119.5(4) . . ?
C4 C3 H3 117.9 . . ?
C2 C3 C4 124.1(4) . . ?
C2 C3 H3 117.9 . . ?
C3 C2 C1 116.5(4) . . ?
C3 C2 C20 121.9(4) . . ?
C1 C2 C20 121.5(4) . . ?
O2 C1 C6 120.0(4) . . ?
O2 C1 C2 118.8(4) . . ?
C6 C1 C2 121.2(4) . . ?
N8 C9 H9A 108.5 . . ?
N8 C9 H9B 108.5 . . ?
H9A C9 H9B 107.5 . . ?
C10 C9 N8 115.0(4) . . ?
C10 C9 H9A 108.5 . . ?
C10 C9 H9B 108.5 . . ?
C11 C10 C9 122.6(4) . . ?
C11 C10 C15 120.7(4) . . ?
C15 C10 C9 116.4(4) . . ?
C10 C11 H11 119.9 . . ?
C10 C11 C12 120.1(4) . . ?
C12 C11 H11 119.9 . . ?
C11 C12 C32 121.5(4) . . ?
C13 C12 C11 117.7(4) . . ?
C13 C12 C32 120.5(4) . . ?
C12 C13 H13 117.7 . . ?
C12 C13 C14 124.7(4) . . ?
C14 C13 H13 117.7 . . ?
C13 C14 C28 122.1(4) . . ?
C15 C14 C13 115.7(4) . . ?
C15 C14 C28 122.2(4) . . ?
O3 C15 C10 116.2(4) . . ?
O3 C15 C14 122.7(4) . . ?
C10 C15 C14 121.1(4) . . ?
C4 C24 C26 108.7(4) . . ?
C4 C24 C27 109.4(4) . . ?
C25 C24 C4 112.0(4) . . ?
C25 C24 C26 108.7(4) . . ?
C25 C24 C27 108.6(4) . . ?
C26 C24 C27 109.4(4) . . ?
C24 C25 H25A 109.5 . . ?
C24 C25 H25B 109.5 . . ?
C24 C25 H25C 109.5 . . ?
H25A C25 H25B 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C24 C26 H26A 109.5 . . ?
C24 C26 H26B 109.5 . . ?
C24 C26 H26C 109.5 . . ?
H26A C26 H26B 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C24 C27 H27A 109.5 . . ?
C24 C27 H27B 109.5 . . ?
C24 C27 H27C 109.5 . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C2 C20 C21 112.6(4) . . ?
C2 C20 C22 111.4(4) . . ?
C2 C20 C23 109.0(4) . . ?
C21 C20 C22 106.8(4) . . ?
C21 C20 C23 107.3(4) . . ?
C22 C20 C23 109.5(4) . . ?
C20 C21 H21A 109.5 . . ?
C20 C21 H21B 109.5 . . ?
C20 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C20 C22 H22A 109.5 . . ?
C20 C22 H22B 109.5 . . ?
C20 C22 H22C 109.5 . . ?
H22A C22 H22B 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C20 C23 H23A 109.5 . . ?
C20 C23 H23B 109.5 . . ?
C20 C23 H23C 109.5 . . ?
H23A C23 H23B 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C12 C32 C33 111.7(4) . . ?
C12 C32 C34B 104.7(7) . . ?
C12 C32 C35A 110.5(7) . . ?
C33 C32 C34B 102.1(8) . . ?
C33 C32 C35A 103.1(8) . . ?
C34A C32 C12 109.9(7) . . ?
C34A C32 C33 115.4(10) . . ?
C34A C32 C35A 105.8(10) . . ?
C35B C32 C12 114.0(9) . . ?
C35B C32 C33 112.7(10) . . ?
C35B C32 C34B 110.7(10) . . ?
C32 C33 H33A 109.5 . . ?
C32 C33 H33B 109.5 . . ?
C32 C33 H33C 109.5 . . ?
H33A C33 H33B 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C32 C34A H34A 109.5 . . ?
C32 C34A H34B 109.5 . . ?
C32 C34A H34C 109.5 . . ?
H34A C34A H34B 109.5 . . ?
H34A C34A H34C 109.5 . . ?
H34B C34A H34C 109.5 . . ?
C32 C34B H34D 109.5 . . ?
C32 C34B H34E 109.5 . . ?
C32 C34B H34F 109.5 . . ?
H34D C34B H34E 109.5 . . ?
H34D C34B H34F 109.5 . . ?
H34E C34B H34F 109.5 . . ?
C32 C35A H35A 109.5 . . ?
C32 C35A H35B 109.5 . . ?
C32 C35A H35C 109.5 . . ?
H35A C35A H35B 109.5 . . ?
H35A C35A H35C 109.5 . . ?
H35B C35A H35C 109.5 . . ?
C32 C35B H35D 109.5 . . ?
C32 C35B H35E 109.5 . . ?
C32 C35B H35F 109.5 . . ?
H35D C35B H35E 109.5 . . ?
H35D C35B H35F 109.5 . . ?
H35E C35B H35F 109.5 . . ?
C14 C28 C31 109.9(4) . . ?
C29 C28 C14 111.4(4) . . ?
C29 C28 C31 107.9(5) . . ?
C30 C28 C14 110.2(4) . . ?
C30 C28 C29 107.6(5) . . ?
C30 C28 C31 109.6(5) . . ?
C28 C29 H29A 109.5 . . ?
C28 C29 H29B 109.5 . . ?
C28 C29 H29C 109.5 . . ?
H29A C29 H29B 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C28 C30 H30A 109.5 . . ?
C28 C30 H30B 109.5 . . ?
C28 C30 H30C 109.5 . . ?
H30A C30 H30B 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C28 C31 H31A 109.5 . . ?
C28 C31 H31B 109.5 . . ?
C28 C31 H31C 109.5 . . ?
H31A C31 H31B 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
O5 C19 H19A 109.5 . . ?
O5 C19 H19B 109.5 . . ?
O5 C19 C18 110.8(4) . . ?
H19A C19 H19B 108.1 . . ?
C18 C19 H19A 109.5 . . ?
C18 C19 H19B 109.5 . . ?
O4 C18 C19 102.2(4) . . ?
O4 C18 H18A 111.3 . . ?
O4 C18 H18B 111.3 . . ?
C19 C18 H18A 111.3 . . ?
C19 C18 H18B 111.3 . . ?
H18A C18 H18B 109.2 . . ?
O4 C17 H17A 110.7 . . ?
O4 C17 H17B 110.7 . . ?
O4 C17 C16 105.1(4) . . ?
H17A C17 H17B 108.8 . . ?
C16 C17 H17A 110.7 . . ?
C16 C17 H17B 110.7 . . ?
N8 C16 C17 110.0(4) . . ?
N8 C16 H16A 109.7 . . ?
N8 C16 H16B 109.7 . . ?
C17 C16 H16A 109.7 . . ?
C17 C16 H16B 109.7 . . ?
H16A C16 H16B 108.2 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
V1 O2 C1 C6 -43.8(6) . . . . ?
V1 O2 C1 C2 138.2(3) . . . . ?
V1 O3 C15 C10 68.8(5) . . . . ?
V1 O3 C15 C14 -113.0(4) . . . . ?
V1 O5 C19 C18 -21.1(6) . . . . ?
V1 O4 C18 C19 -47.1(4) . . . . ?
V1 O4 C17 C16 39.3(4) . . . . ?
V1 N8 C7 C6 48.1(4) . . . . ?
V1 N8 C9 C10 36.4(5) . . . . ?
V1 N8 C16 C17 47.1(4) . . . . ?
O1 V1 O2 C1 -37.9(4) . . . . ?
O1 V1 O3 C15 30.5(3) . . . . ?
O1 V1 O5 C19 178.2(4) . . . . ?
O2 V1 O3 C15 -103.8(4) . . . . ?
O2 V1 O5 C19 -81.4(4) . . . . ?
O3 V1 O2 C1 96.3(5) . . . . ?
O3 V1 O5 C19 79.4(4) . . . . ?
O5 V1 O2 C1 -146.5(4) . . . . ?
O5 V1 O3 C15 138.1(3) . . . . ?
O5 C19 C18 O4 46.1(5) . . . . ?
O4 V1 O2 C1 138.3(4) . . . . ?
O4 V1 O3 C15 -144.8(3) . . . . ?
O4 V1 O5 C19 -5.5(4) . . . . ?
O4 C17 C16 N8 -57.3(5) . . . . ?
N8 V1 O2 C1 60.7(4) . . . . ?
N8 V1 O3 C15 -68.2(3) . . . . ?
N8 V1 O5 C19 3.5(6) . . . . ?
N8 C7 C6 C5 165.0(4) . . . . ?
N8 C7 C6 C1 -17.2(6) . . . . ?
N8 C9 C10 C11 130.0(4) . . . . ?
N8 C9 C10 C15 -56.8(5) . . . . ?
C7 N8 C9 C10 -86.4(4) . . . . ?
C7 N8 C16 C17 166.2(4) . . . . ?
C7 C6 C5 C4 176.3(4) . . . . ?
C7 C6 C1 O2 6.3(7) . . . . ?
C7 C6 C1 C2 -175.7(4) . . . . ?
C6 C5 C4 C3 0.1(7) . . . . ?
C6 C5 C4 C24 -180.0(4) . . . . ?
C5 C6 C1 O2 -175.9(4) . . . . ?
C5 C6 C1 C2 2.1(7) . . . . ?
C5 C4 C3 C2 1.1(7) . . . . ?
C5 C4 C24 C25 6.6(7) . . . . ?
C5 C4 C24 C26 -113.5(5) . . . . ?
C5 C4 C24 C27 127.1(5) . . . . ?
C4 C3 C2 C1 -0.6(7) . . . . ?
C4 C3 C2 C20 -178.6(4) . . . . ?
C3 C4 C24 C25 -173.4(5) . . . . ?
C3 C4 C24 C26 66.5(6) . . . . ?
C3 C4 C24 C27 -52.9(6) . . . . ?
C3 C2 C1 O2 177.0(4) . . . . ?
C3 C2 C1 C6 -1.0(6) . . . . ?
C3 C2 C20 C21 -3.5(6) . . . . ?
C3 C2 C20 C22 -123.5(5) . . . . ?
C3 C2 C20 C23 115.5(5) . . . . ?
C1 C6 C5 C4 -1.6(7) . . . . ?
C1 C2 C20 C21 178.6(4) . . . . ?
C1 C2 C20 C22 58.6(6) . . . . ?
C1 C2 C20 C23 -62.3(5) . . . . ?
C9 N8 C7 C6 174.0(4) . . . . ?
C9 N8 C16 C17 -78.1(4) . . . . ?
C9 C10 C11 C12 173.6(4) . . . . ?
C9 C10 C15 O3 5.9(6) . . . . ?
C9 C10 C15 C14 -172.3(4) . . . . ?
C10 C11 C12 C13 -0.9(7) . . . . ?
C10 C11 C12 C32 -175.0(4) . . . . ?
C11 C10 C15 O3 179.2(4) . . . . ?
C11 C10 C15 C14 1.0(7) . . . . ?
C11 C12 C13 C14 -0.6(7) . . . . ?
C11 C12 C32 C33 -156.4(5) . . . . ?
C11 C12 C32 C34A 74.2(13) . . . . ?
C11 C12 C32 C34B 93.9(10) . . . . ?
C11 C12 C32 C35A -42.2(11) . . . . ?
C11 C12 C32 C35B -27.2(14) . . . . ?
C12 C13 C14 C15 2.2(7) . . . . ?
C12 C13 C14 C28 -177.1(5) . . . . ?
C13 C12 C32 C33 29.7(6) . . . . ?
C13 C12 C32 C34A -99.7(13) . . . . ?
C13 C12 C32 C34B -80.0(11) . . . . ?
C13 C12 C32 C35A 143.9(10) . . . . ?
C13 C12 C32 C35B 158.9(13) . . . . ?
C13 C14 C15 O3 179.6(4) . . . . ?
C13 C14 C15 C10 -2.3(7) . . . . ?
C13 C14 C28 C29 8.6(7) . . . . ?
C13 C14 C28 C30 128.0(5) . . . . ?
C13 C14 C28 C31 -111.1(5) . . . . ?
C15 C10 C11 C12 0.7(7) . . . . ?
C15 C14 C28 C29 -170.8(5) . . . . ?
C15 C14 C28 C30 -51.3(6) . . . . ?
C15 C14 C28 C31 69.6(6) . . . . ?
C24 C4 C3 C2 -178.9(4) . . . . ?
C20 C2 C1 O2 -5.0(6) . . . . ?
C20 C2 C1 C6 177.0(4) . . . . ?
C32 C12 C13 C14 173.5(4) . . . . ?
C28 C14 C15 O3 -1.1(7) . . . . ?
C28 C14 C15 C10 177.0(4) . . . . ?
C18 O4 C17 C16 164.4(4) . . . . ?
C17 O4 C18 C19 -176.5(4) . . . . ?
C16 N8 C7 C6 -69.5(5) . . . . ?
C16 N8 C9 C10 156.9(4) . . . . ?

loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-1 -7 1 0.1099 -1.0027 -7.0051 1.0060 0.0324 -0.0656 1.0367
-5 4 -5 0.0887 -5.0035 3.9996 -5.0104 -0.6363 0.5855 -0.4413
-7 0 -3 0.0498 -7.0066 -0.0032 -3.0071 -0.6575 0.7526 0.1962
7 -1 3 0.0510 7.0064 -0.9976 3.0080 0.6662 -0.7824 -0.0526
-1 0 19 0.0214 -1.0036 0.0073 19.0119 0.8046 0.5934 0.0761
1 0 -19 0.0084 1.0036 -0.0073 -19.0119 -0.8046 -0.5934 -0.0761
3 -5 -10 0.0873 3.0033 -5.0069 -10.0001 -0.1970 -0.7540 0.6059
-5 0 13 0.0364 -5.0068 0.0037 13.0050 0.2306 0.9163 0.1776
5 0 -13 0.0380 5.0068 -0.0037 -13.0050 -0.2306 -0.9163 -0.1776
1 7 0 0.0986 1.0025 7.0055 -0.0053 0.0138 0.0907 -1.0342
_database_code_depnum_ccdc_archive 'CCDC 977975'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_S4_VO_COOH

_audit_creation_date             2012-03-05T16:44:25-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.3
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C34 H52 N O6 V'
_chemical_formula_sum            'C34 H52 N O6 V'
_chemical_formula_weight         621.71
_chemical_compound_source        'synthesis as described'
_chemical_absolute_configuration unk

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_Int_Tables_number      2
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.35040(10)
_cell_length_b                   12.4992(2)
_cell_length_c                   15.3633(2)
_cell_angle_alpha                106.2400(10)
_cell_angle_beta                 103.0330(10)
_cell_angle_gamma                91.5820(10)
_cell_volume                     1671.58(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    123(2)
_cell_measurement_reflns_used    6778
_cell_measurement_theta_min      0.998
_cell_measurement_theta_max      27.103
_cell_measurement_wavelength     0.71073

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_description       cube
_exptl_crystal_colour            brown
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_exptl_crystal_density_diffrn    1.235
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             668
_exptl_special_details           
;
 ?
;

#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    0.34
_exptl_absorpt_correction_T_min  0.6662
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2008)'

#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_source                   'Enraf Nonius FR590'
_diffrn_ambient_temperature      123(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_orient_matrix_type       'by Bruker AXS Collect from scalepack cell'
_diffrn_orient_matrix_ub_11      0.594956E-1
_diffrn_orient_matrix_ub_12      0.734314E-1
_diffrn_orient_matrix_ub_13      0.346011E-1
_diffrn_orient_matrix_ub_21      -0.908722E-1
_diffrn_orient_matrix_ub_22      0.335439E-1
_diffrn_orient_matrix_ub_23      0.144783E-1
_diffrn_orient_matrix_ub_31      0.191684E-1
_diffrn_orient_matrix_ub_32      -0.221909E-1
_diffrn_orient_matrix_ub_33      0.589733E-1
_diffrn_measurement_device       '95mm CCD camera on κ-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_reflns_av_R_equivalents  0.0358
_diffrn_reflns_av_unetI/netI     0.0321
_diffrn_reflns_number            26912
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.85
_diffrn_reflns_theta_max         26
_diffrn_reflns_theta_full        26
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_reflns_number_total             6518
_reflns_number_gt                5845
_reflns_threshold_expression     >2σ(I)

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_cell_refinement       'HKL Scalepack (OtwinO4ski & Minor 1997)'
_computing_data_reduction        
'HKL Denzo and Scalepack (OtwinO4ski & Minor 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Ortep-3 for WindO4s (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'

#----------------------------------------------------------------------------#
#                   STRUCTURE SOLUTION
#----------------------------------------------------------------------------#

_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2σ(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0287P)²+1.2712P] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         6518
_refine_ls_number_parameters     424
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0444
_refine_ls_R_factor_gt           0.0378
_refine_ls_wR_factor_ref         0.0918
_refine_ls_wR_factor_gt          0.0874
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_restrained_S_all      1.088
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_diff_density_max         0.322
_refine_diff_density_min         -0.31
_refine_diff_density_rms         0.047

#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

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 0 '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 0.006 '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'

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.79366(18) 0.38461(14) 1.13826(11) 0.0178(3) Uani 1 1 d . . .
C2 C 0.76629(18) 0.43828(14) 1.22649(11) 0.0180(3) Uani 1 1 d . . .
C3 C 0.87381(19) 0.51843(14) 1.28890(11) 0.0197(3) Uani 1 1 d . . .
H3 H 0.8554 0.5566 1.346 0.024 Uiso 1 1 calc R . .
C4 C 1.00903(18) 0.54585(14) 1.27156(11) 0.0183(3) Uani 1 1 d . . .
C5 C 1.03467(18) 0.48804(14) 1.18622(11) 0.0184(3) Uani 1 1 d . . .
H5 H 1.1245 0.5027 1.1734 0.022 Uiso 1 1 calc R . .
C6 C 0.92854(18) 0.40808(14) 1.11886(11) 0.0174(3) Uani 1 1 d . . .
C7 C 0.96681(18) 0.35126(14) 1.02672(11) 0.0192(3) Uani 1 1 d . . .
H7A H 0.9613 0.4045 0.9909 0.023 Uiso 1 1 calc R . .
H7B H 1.0683 0.3336 1.0403 0.023 Uiso 1 1 calc R . .
C9 C 0.91777(18) 0.21021(14) 0.87622(11) 0.0181(3) Uani 1 1 d . . .
H9A H 1.0193 0.1925 0.8885 0.022 Uiso 1 1 calc R . .
H9B H 0.9132 0.2718 0.8492 0.022 Uiso 1 1 calc R . .
C10 C 0.82308(18) 0.11001(14) 0.80642(11) 0.0180(3) Uani 1 1 d . . .
C11 C 0.88114(18) 0.01174(14) 0.76759(11) 0.0187(3) Uani 1 1 d . . .
H11 H 0.9809 0.0049 0.7883 0.022 Uiso 1 1 calc R . .
C12 C 0.79200(19) -0.07696(14) 0.69793(11) 0.0191(3) Uani 1 1 d . A .
C13 C 0.64352(19) -0.06200(14) 0.66810(11) 0.0204(3) Uani 1 1 d . . .
H13 H 0.5838 -0.1197 0.6205 0.024 Uiso 1 1 calc R . .
C14 C 0.57919(18) 0.03432(14) 0.70536(11) 0.0189(3) Uani 1 1 d . . .
C15 C 0.67183(18) 0.12017(14) 0.77736(11) 0.0175(3) Uani 1 1 d . . .
C16 C 0.89355(18) 0.15830(14) 1.01361(12) 0.0191(3) Uani 1 1 d . . .
H16A H 0.9133 0.1914 1.0808 0.023 Uiso 1 1 calc R . .
H16B H 0.9775 0.1192 0.9996 0.023 Uiso 1 1 calc R . .
C17 C 0.75705(18) 0.07684(14) 0.98040(11) 0.0188(3) Uani 1 1 d . . .
C18 C 0.62505(19) 0.40422(15) 1.25244(12) 0.0212(4) Uani 1 1 d . . .
C19 C 0.48430(19) 0.41860(17) 1.18363(12) 0.0261(4) Uani 1 1 d . . .
H19A H 0.3991 0.3957 1.2015 0.039 Uiso 1 1 calc R . .
H19B H 0.4832 0.3733 1.1216 0.039 Uiso 1 1 calc R . .
H19C H 0.4828 0.4958 1.1849 0.039 Uiso 1 1 calc R . .
C20 C 0.6274(2) 0.28147(16) 1.25353(14) 0.0288(4) Uani 1 1 d . . .
H20A H 0.7123 0.2745 1.2995 0.043 Uiso 1 1 calc R . .
H20B H 0.6318 0.2347 1.193 0.043 Uiso 1 1 calc R . .
H20C H 0.5395 0.2586 1.2687 0.043 Uiso 1 1 calc R . .
C21 C 0.6183(2) 0.47578(17) 1.35043(12) 0.0279(4) Uani 1 1 d . . .
H21A H 0.5293 0.4529 1.3644 0.042 Uiso 1 1 calc R . .
H21B H 0.6193 0.5532 1.3523 0.042 Uiso 1 1 calc R . .
H21C H 0.702 0.4659 1.3958 0.042 Uiso 1 1 calc R . .
C22 C 1.12002(19) 0.63593(14) 1.34700(11) 0.0203(3) Uani 1 1 d . . .
C23 C 1.0536(2) 0.74918(15) 1.36118(13) 0.0269(4) Uani 1 1 d . . .
H23A H 1.0334 0.7682 1.3035 0.04 Uiso 1 1 calc R . .
H23B H 1.1224 0.8062 1.4083 0.04 Uiso 1 1 calc R . .
H23C H 0.9636 0.7438 1.3805 0.04 Uiso 1 1 calc R . .
C24 C 1.2675(2) 0.64748(16) 1.32159(13) 0.0264(4) Uani 1 1 d . . .
H24A H 1.3094 0.5771 1.3123 0.04 Uiso 1 1 calc R . .
H24B H 1.3337 0.7035 1.3714 0.04 Uiso 1 1 calc R . .
H24C H 1.252 0.6691 1.2652 0.04 Uiso 1 1 calc R . .
C25 C 1.1520(2) 0.60590(16) 1.43974(12) 0.0275(4) Uani 1 1 d . . .
H25A H 1.0616 0.5994 1.4584 0.041 Uiso 1 1 calc R . .
H25B H 1.2193 0.6636 1.4871 0.041 Uiso 1 1 calc R . .
H25C H 1.195 0.536 1.4315 0.041 Uiso 1 1 calc R . .
C26 C 0.41437(18) 0.04587(15) 0.67006(12) 0.0218(4) Uani 1 1 d . . .
C27 C 0.3353(2) 0.04992(16) 0.74843(13) 0.0258(4) Uani 1 1 d . . .
H27A H 0.341 -0.0196 0.7636 0.039 Uiso 1 1 calc R . .
H27B H 0.2337 0.0616 0.7278 0.039 Uiso 1 1 calc R . .
H27C H 0.3818 0.1103 0.8028 0.039 Uiso 1 1 calc R . .
C28 C 0.3389(2) -0.05292(17) 0.58509(13) 0.0300(4) Uani 1 1 d . . .
H28A H 0.3876 -0.058 0.5356 0.045 Uiso 1 1 calc R . .
H28B H 0.2373 -0.0414 0.5643 0.045 Uiso 1 1 calc R . .
H28C H 0.3446 -0.1211 0.6024 0.045 Uiso 1 1 calc R . .
C29 C 0.3948(2) 0.15256(17) 0.63949(13) 0.0283(4) Uani 1 1 d . . .
H29A H 0.4393 0.2166 0.6912 0.042 Uiso 1 1 calc R . .
H29B H 0.2916 0.1596 0.619 0.042 Uiso 1 1 calc R . .
H29C H 0.4414 0.1482 0.5891 0.042 Uiso 1 1 calc R . .
C30 C 0.8569(2) -0.18487(15) 0.65506(13) 0.0253(4) Uani 1 1 d D . .
C31A C 0.7405(3) -0.2734(2) 0.5836(2) 0.0306(6) Uani 0.846(4) 1 d P A 1
H31A H 0.6948 -0.2446 0.5334 0.046 Uiso 0.846(4) 1 calc PR A 1
H31B H 0.6671 -0.292 0.6131 0.046 Uiso 0.846(4) 1 calc PR A 1
H31C H 0.7865 -0.3392 0.5593 0.046 Uiso 0.846(4) 1 calc PR A 1
C32A C 0.9679(3) -0.1540(2) 0.60201(17) 0.0354(7) Uani 0.846(4) 1 d P A 1
H32A H 1.0118 -0.2197 0.5749 0.053 Uiso 0.846(4) 1 calc PR A 1
H32B H 1.0436 -0.0987 0.645 0.053 Uiso 0.846(4) 1 calc PR A 1
H32C H 0.9168 -0.1245 0.5535 0.053 Uiso 0.846(4) 1 calc PR A 1
C33A C 0.9369(3) -0.2312(2) 0.73040(17) 0.0386(8) Uani 0.846(4) 1 d P A 1
H33A H 0.8693 -0.2483 0.7644 0.058 Uiso 0.846(4) 1 calc PR A 1
H33B H 1.0147 -0.1769 0.7723 0.058 Uiso 0.846(4) 1 calc PR A 1
H33C H 0.9781 -0.2982 0.7028 0.058 Uiso 0.846(4) 1 calc PR A 1
C33B C 0.802(2) -0.2731(11) 0.7126(11) 0.045(4) Uani 0.154(4) 1 d PD A 2
H33D H 0.697 -0.2884 0.6941 0.068 Uiso 0.154(4) 1 calc PR A 2
H33E H 0.8329 -0.2381 0.7788 0.068 Uiso 0.154(4) 1 calc PR A 2
H33F H 0.8469 -0.342 0.6969 0.068 Uiso 0.154(4) 1 calc PR A 2
C32B C 1.0261(13) -0.1898(13) 0.6943(12) 0.047(5) Uani 0.154(4) 1 d PD A 2
H32D H 1.0516 -0.2643 0.67 0.07 Uiso 0.154(4) 1 calc PR A 2
H32E H 1.0481 -0.17 0.7613 0.07 Uiso 0.154(4) 1 calc PR A 2
H32F H 1.0818 -0.1382 0.6757 0.07 Uiso 0.154(4) 1 calc PR A 2
C31B C 0.800(3) -0.2469(19) 0.5596(9) 0.061(7) Uani 0.154(4) 1 d PD A 2
H31D H 0.8437 -0.3164 0.5466 0.092 Uiso 0.154(4) 1 calc PR A 2
H31E H 0.8228 -0.2043 0.5204 0.092 Uiso 0.154(4) 1 calc PR A 2
H31F H 0.6949 -0.2617 0.5473 0.092 Uiso 0.154(4) 1 calc PR A 2
C34 C 0.3378(2) 0.35012(17) 0.90135(15) 0.0315(4) Uani 1 1 d . . .
H34A H 0.386 0.4233 0.9129 0.047 Uiso 1 1 calc R . .
H34B H 0.2579 0.3562 0.9317 0.047 Uiso 1 1 calc R . .
H34C H 0.3001 0.3169 0.8353 0.047 Uiso 1 1 calc R . .
C35 C 0.6605(2) -0.10810(18) 0.9570(2) 0.0466(6) Uani 1 1 d . . .
H35A H 0.5895 -0.0847 0.9932 0.07 Uiso 1 1 calc R . .
H35B H 0.6934 -0.1777 0.9646 0.07 Uiso 1 1 calc R . .
H35C H 0.6158 -0.1177 0.8922 0.07 Uiso 1 1 calc R . .
N8 N 0.87282(15) 0.24710(11) 0.96704(9) 0.0164(3) Uani 1 1 d . . .
O2 O 0.68970(12) 0.30717(9) 1.07417(8) 0.0184(2) Uani 1 1 d . . .
O3 O 0.62113(12) 0.21582(9) 0.81995(8) 0.0186(2) Uani 1 1 d . . .
O4 O 0.63469(12) 0.10193(10) 0.95153(8) 0.0193(3) Uani 1 1 d . . .
O5 O 0.78583(13) -0.02329(10) 0.98872(10) 0.0277(3) Uani 1 1 d . . .
O1 O 0.67705(13) 0.41198(10) 0.94493(8) 0.0213(3) Uani 1 1 d . . .
O6 O 0.44032(12) 0.28221(10) 0.93705(8) 0.0202(3) Uani 1 1 d . . .
V1 V 0.63430(3) 0.28854(2) 0.946322(19) 0.01607(9) Uani 1 1 d . . .



#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_geom_special_details            
;
 All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell s.u.'s are taken
 into account individually in the estimation of s.u.'s in distances, angles
 and torsion angles; correlations between s.u.'s in cell parameters are only
 used when they are defined by crystal symmetry.  An apprO1imate (isotropic)
 treatment of cell s.u.'s is used for estimating s.u.'s 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 O2 1.354(2) . ?
C1 C6 1.401(2) . ?
C1 C2 1.418(2) . ?
C2 C3 1.381(2) . ?
C2 C18 1.545(2) . ?
C3 C4 1.402(2) . ?
C3 H3 0.93 . ?
C4 C5 1.386(2) . ?
C4 C22 1.533(2) . ?
C5 C6 1.399(2) . ?
C5 H5 0.93 . ?
C6 C7 1.522(2) . ?
C7 N8 1.488(2) . ?
C7 H7A 0.97 . ?
C7 H7B 0.97 . ?
C9 N8 1.500(2) . ?
C9 C10 1.504(2) . ?
C9 H9A 0.97 . ?
C9 H9B 0.97 . ?
C10 C11 1.390(2) . ?
C10 C15 1.404(2) . ?
C11 C12 1.397(2) . ?
C11 H11 0.93 . ?
C12 C13 1.396(2) . ?
C12 C30 1.533(2) . ?
C13 C14 1.396(2) . ?
C13 H13 0.93 . ?
C14 C15 1.406(2) . ?
C14 C26 1.539(2) . ?
C15 O3 1.3475(19) . ?
C16 N8 1.475(2) . ?
C16 C17 1.507(2) . ?
C16 H16A 0.97 . ?
C16 H16B 0.97 . ?
C17 O4 1.214(2) . ?
C17 O5 1.322(2) . ?
C18 C21 1.537(2) . ?
C18 C20 1.540(3) . ?
C18 C19 1.541(2) . ?
C19 H19A 0.96 . ?
C19 H19B 0.96 . ?
C19 H19C 0.96 . ?
C20 H20A 0.96 . ?
C20 H20B 0.96 . ?
C20 H20C 0.96 . ?
C21 H21A 0.96 . ?
C21 H21B 0.96 . ?
C21 H21C 0.96 . ?
C22 C24 1.529(2) . ?
C22 C25 1.541(2) . ?
C22 C23 1.541(2) . ?
C23 H23A 0.96 . ?
C23 H23B 0.96 . ?
C23 H23C 0.96 . ?
C24 H24A 0.96 . ?
C24 H24B 0.96 . ?
C24 H24C 0.96 . ?
C25 H25A 0.96 . ?
C25 H25B 0.96 . ?
C25 H25C 0.96 . ?
C26 C29 1.535(3) . ?
C26 C28 1.537(2) . ?
C26 C27 1.539(2) . ?
C27 H27A 0.96 . ?
C27 H27B 0.96 . ?
C27 H27C 0.96 . ?
C28 H28A 0.96 . ?
C28 H28B 0.96 . ?
C28 H28C 0.96 . ?
C29 H29A 0.96 . ?
C29 H29B 0.96 . ?
C29 H29C 0.96 . ?
C30 C31B 1.423(14) . ?
C30 C33A 1.498(3) . ?
C30 C31A 1.526(3) . ?
C30 C32A 1.558(3) . ?
C30 C32B 1.570(12) . ?
C30 C33B 1.725(12) . ?
C31A H31A 0.96 . ?
C31A H31B 0.96 . ?
C31A H31C 0.96 . ?
C32A H32A 0.96 . ?
C32A H32B 0.96 . ?
C32A H32C 0.96 . ?
C33A H33A 0.96 . ?
C33A H33B 0.96 . ?
C33A H33C 0.96 . ?
C33B H33D 0.96 . ?
C33B H33E 0.96 . ?
C33B H33F 0.96 . ?
C32B H32D 0.96 . ?
C32B H32E 0.96 . ?
C32B H32F 0.96 . ?
C31B H31D 0.96 . ?
C31B H31E 0.96 . ?
C31B H31F 0.96 . ?
C34 O6 1.417(2) . ?
C34 H34A 0.96 . ?
C34 H34B 0.96 . ?
C34 H34C 0.96 . ?
C35 O5 1.456(2) . ?
C35 H35A 0.96 . ?
C35 H35B 0.96 . ?
C35 H35C 0.96 . ?
N8 V1 2.2759(14) . ?
O2 V1 1.8599(11) . ?
O3 V1 1.8735(11) . ?
O4 V1 2.3561(12) . ?
O1 V1 1.5903(12) . ?
O6 V1 1.7848(11) . ?

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
O2 C1 C6 120.38(14) . . ?
O2 C1 C2 119.04(14) . . ?
C6 C1 C2 120.53(15) . . ?
C3 C2 C1 117.09(15) . . ?
C3 C2 C18 121.87(15) . . ?
C1 C2 C18 120.99(15) . . ?
C2 C3 C4 124.07(15) . . ?
C2 C3 H3 118 . . ?
C4 C3 H3 118 . . ?
C5 C4 C3 117.19(15) . . ?
C5 C4 C22 123.73(15) . . ?
C3 C4 C22 119.07(15) . . ?
C4 C5 C6 121.56(15) . . ?
C4 C5 H5 119.2 . . ?
C6 C5 H5 119.2 . . ?
C5 C6 C1 119.45(15) . . ?
C5 C6 C7 117.26(14) . . ?
C1 C6 C7 123.28(15) . . ?
N8 C7 C6 116.19(13) . . ?
N8 C7 H7A 108.2 . . ?
C6 C7 H7A 108.2 . . ?
N8 C7 H7B 108.2 . . ?
C6 C7 H7B 108.2 . . ?
H7A C7 H7B 107.4 . . ?
N8 C9 C10 113.53(13) . . ?
N8 C9 H9A 108.9 . . ?
C10 C9 H9A 108.9 . . ?
N8 C9 H9B 108.9 . . ?
C10 C9 H9B 108.9 . . ?
H9A C9 H9B 107.7 . . ?
C11 C10 C15 119.97(15) . . ?
C11 C10 C9 122.43(15) . . ?
C15 C10 C9 117.54(15) . . ?
C10 C11 C12 121.07(15) . . ?
C10 C11 H11 119.5 . . ?
C12 C11 H11 119.5 . . ?
C13 C12 C11 117.31(15) . . ?
C13 C12 C30 121.86(15) . . ?
C11 C12 C30 120.82(15) . . ?
C12 C13 C14 123.97(16) . . ?
C12 C13 H13 118 . . ?
C14 C13 H13 118 . . ?
C13 C14 C15 116.86(15) . . ?
C13 C14 C26 121.69(15) . . ?
C15 C14 C26 121.45(15) . . ?
O3 C15 C10 117.22(14) . . ?
O3 C15 C14 122.05(15) . . ?
C10 C15 C14 120.72(15) . . ?
N8 C16 C17 109.94(13) . . ?
N8 C16 H16A 109.7 . . ?
C17 C16 H16A 109.7 . . ?
N8 C16 H16B 109.7 . . ?
C17 C16 H16B 109.7 . . ?
H16A C16 H16B 108.2 . . ?
O4 C17 O5 124.36(16) . . ?
O4 C17 C16 123.35(15) . . ?
O5 C17 C16 112.26(14) . . ?
C21 C18 C20 107.64(14) . . ?
C21 C18 C19 107.04(14) . . ?
C20 C18 C19 110.28(15) . . ?
C21 C18 C2 111.46(14) . . ?
C20 C18 C2 108.42(14) . . ?
C19 C18 C2 111.92(14) . . ?
C18 C19 H19A 109.5 . . ?
C18 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C18 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C18 C20 H20A 109.5 . . ?
C18 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C18 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C18 C21 H21A 109.5 . . ?
C18 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C18 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C24 C22 C4 112.60(14) . . ?
C24 C22 C25 107.30(15) . . ?
C4 C22 C25 109.84(14) . . ?
C24 C22 C23 108.96(15) . . ?
C4 C22 C23 108.87(14) . . ?
C25 C22 C23 109.21(14) . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C22 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C22 C24 H24A 109.5 . . ?
C22 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C22 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C22 C25 H25A 109.5 . . ?
C22 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C22 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C29 C26 C28 106.97(15) . . ?
C29 C26 C27 109.95(15) . . ?
C28 C26 C27 107.94(14) . . ?
C29 C26 C14 110.36(14) . . ?
C28 C26 C14 112.18(14) . . ?
C27 C26 C14 109.38(14) . . ?
C26 C27 H27A 109.5 . . ?
C26 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C26 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C26 C28 H28A 109.5 . . ?
C26 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C26 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C26 C29 H29A 109.5 . . ?
C26 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C26 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C31B C30 C33A 125.6(8) . . ?
C31B C30 C31A 32.9(11) . . ?
C33A C30 C31A 110.2(2) . . ?
C31B C30 C12 120.5(7) . . ?
C33A C30 C12 110.21(16) . . ?
C31A C30 C12 112.75(17) . . ?
C31B C30 C32A 74.3(12) . . ?
C33A C30 C32A 109.30(19) . . ?
C31A C30 C32A 107.00(19) . . ?
C12 C30 C32A 107.23(16) . . ?
C31B C30 C32B 115.0(10) . . ?
C33A C30 C32B 48.9(7) . . ?
C31A C30 C32B 130.7(6) . . ?
C12 C30 C32B 116.5(6) . . ?
C32A C30 C32B 61.1(7) . . ?
C31B C30 C33B 102.3(13) . . ?
C33A C30 C33B 46.5(6) . . ?
C31A C30 C33B 72.8(6) . . ?
C12 C30 C33B 101.5(5) . . ?
C32A C30 C33B 148.3(5) . . ?
C32B C30 C33B 94.3(9) . . ?
C30 C31A H31A 109.5 . . ?
C30 C31A H31B 109.5 . . ?
C30 C31A H31C 109.5 . . ?
C30 C32A H32A 109.5 . . ?
C30 C32A H32B 109.5 . . ?
C30 C32A H32C 109.5 . . ?
C30 C33A H33A 109.5 . . ?
C30 C33A H33B 109.5 . . ?
C30 C33A H33C 109.5 . . ?
C30 C33B H33D 109.5 . . ?
C30 C33B H33E 109.5 . . ?
H33D C33B H33E 109.5 . . ?
C30 C33B H33F 109.5 . . ?
H33D C33B H33F 109.5 . . ?
H33E C33B H33F 109.5 . . ?
C30 C32B H32D 109.5 . . ?
C30 C32B H32E 109.5 . . ?
H32D C32B H32E 109.5 . . ?
C30 C32B H32F 109.5 . . ?
H32D C32B H32F 109.5 . . ?
H32E C32B H32F 109.5 . . ?
C30 C31B H31D 109.5 . . ?
C30 C31B H31E 109.5 . . ?
H31D C31B H31E 109.5 . . ?
C30 C31B H31F 109.5 . . ?
H31D C31B H31F 109.5 . . ?
H31E C31B H31F 109.5 . . ?
O6 C34 H34A 109.5 . . ?
O6 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
O6 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
O5 C35 H35A 109.5 . . ?
O5 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
O5 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C16 N8 C7 110.17(13) . . ?
C16 N8 C9 109.47(13) . . ?
C7 N8 C9 108.23(12) . . ?
C16 N8 V1 109.76(10) . . ?
C7 N8 V1 107.23(10) . . ?
C9 N8 V1 111.96(9) . . ?
C1 O2 V1 126.59(10) . . ?
C15 O3 V1 131.73(10) . . ?
C17 O4 V1 113.06(11) . . ?
C17 O5 C35 116.10(14) . . ?
C34 O6 V1 127.98(12) . . ?
O1 V1 O6 104.30(6) . . ?
O1 V1 O2 100.15(6) . . ?
O6 V1 O2 96.09(5) . . ?
O1 V1 O3 97.48(6) . . ?
O6 V1 O3 96.03(5) . . ?
O2 V1 O3 155.40(5) . . ?
O1 V1 N8 92.56(6) . . ?
O6 V1 N8 162.90(5) . . ?
O2 V1 N8 77.84(5) . . ?
O3 V1 N8 84.38(5) . . ?
O1 V1 O4 165.59(5) . . ?
O6 V1 O4 90.12(5) . . ?
O2 V1 O4 77.96(5) . . ?
O3 V1 O4 80.69(5) . . ?
N8 V1 O4 73.04(4) . . ?

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
O2 C1 C2 C3 -178.59(14) . . . . ?
C6 C1 C2 C3 3.9(2) . . . . ?
O2 C1 C2 C18 4.0(2) . . . . ?
C6 C1 C2 C18 -173.55(15) . . . . ?
C1 C2 C3 C4 -2.7(2) . . . . ?
C18 C2 C3 C4 174.63(15) . . . . ?
C2 C3 C4 C5 -0.1(3) . . . . ?
C2 C3 C4 C22 -179.50(15) . . . . ?
C3 C4 C5 C6 1.9(2) . . . . ?
C22 C4 C5 C6 -178.70(15) . . . . ?
C4 C5 C6 C1 -0.8(2) . . . . ?
C4 C5 C6 C7 178.74(15) . . . . ?
O2 C1 C6 C5 -179.72(14) . . . . ?
C2 C1 C6 C5 -2.2(2) . . . . ?
O2 C1 C6 C7 0.8(2) . . . . ?
C2 C1 C6 C7 178.29(15) . . . . ?
C5 C6 C7 N8 164.20(14) . . . . ?
C1 C6 C7 N8 -16.3(2) . . . . ?
N8 C9 C10 C11 -122.72(17) . . . . ?
N8 C9 C10 C15 60.3(2) . . . . ?
C15 C10 C11 C12 1.6(2) . . . . ?
C9 C10 C11 C12 -175.31(15) . . . . ?
C10 C11 C12 C13 1.0(2) . . . . ?
C10 C11 C12 C30 179.70(16) . . . . ?
C11 C12 C13 C14 -1.8(3) . . . . ?
C30 C12 C13 C14 179.56(16) . . . . ?
C12 C13 C14 C15 -0.1(3) . . . . ?
C12 C13 C14 C26 -179.62(16) . . . . ?
C11 C10 C15 O3 177.66(14) . . . . ?
C9 C10 C15 O3 -5.3(2) . . . . ?
C11 C10 C15 C14 -3.6(2) . . . . ?
C9 C10 C15 C14 173.44(15) . . . . ?
C13 C14 C15 O3 -178.49(15) . . . . ?
C26 C14 C15 O3 1.0(2) . . . . ?
C13 C14 C15 C10 2.9(2) . . . . ?
C26 C14 C15 C10 -177.66(15) . . . . ?
N8 C16 C17 O4 -26.7(2) . . . . ?
N8 C16 C17 O5 154.98(14) . . . . ?
C3 C2 C18 C21 4.0(2) . . . . ?
C1 C2 C18 C21 -178.70(15) . . . . ?
C3 C2 C18 C20 -114.28(18) . . . . ?
C1 C2 C18 C20 63.0(2) . . . . ?
C3 C2 C18 C19 123.86(17) . . . . ?
C1 C2 C18 C19 -58.9(2) . . . . ?
C5 C4 C22 C24 -5.3(2) . . . . ?
C3 C4 C22 C24 174.09(15) . . . . ?
C5 C4 C22 C25 -124.78(17) . . . . ?
C3 C4 C22 C25 54.6(2) . . . . ?
C5 C4 C22 C23 115.67(18) . . . . ?
C3 C4 C22 C23 -64.96(19) . . . . ?
C13 C14 C26 C29 -125.28(17) . . . . ?
C15 C14 C26 C29 55.3(2) . . . . ?
C13 C14 C26 C28 -6.1(2) . . . . ?
C15 C14 C26 C28 174.43(16) . . . . ?
C13 C14 C26 C27 113.63(18) . . . . ?
C15 C14 C26 C27 -65.8(2) . . . . ?
C13 C12 C30 C31B 31.8(14) . . . . ?
C11 C12 C30 C31B -146.8(14) . . . . ?
C13 C12 C30 C33A -127.7(2) . . . . ?
C11 C12 C30 C33A 53.7(2) . . . . ?
C13 C12 C30 C31A -4.0(3) . . . . ?
C11 C12 C30 C31A 177.35(19) . . . . ?
C13 C12 C30 C32A 113.47(19) . . . . ?
C11 C12 C30 C32A -65.1(2) . . . . ?
C13 C12 C30 C32B 179.2(8) . . . . ?
C11 C12 C30 C32B 0.6(8) . . . . ?
C13 C12 C30 C33B -80.0(7) . . . . ?
C11 C12 C30 C33B 101.4(7) . . . . ?
C17 C16 N8 C7 153.42(13) . . . . ?
C17 C16 N8 C9 -87.68(15) . . . . ?
C17 C16 N8 V1 35.57(15) . . . . ?
C6 C7 N8 C16 -65.79(18) . . . . ?
C6 C7 N8 C9 174.56(13) . . . . ?
C6 C7 N8 V1 53.61(15) . . . . ?
C10 C9 N8 C16 64.23(17) . . . . ?
C10 C9 N8 C7 -175.68(14) . . . . ?
C10 C9 N8 V1 -57.71(15) . . . . ?
C6 C1 O2 V1 -42.7(2) . . . . ?
C2 C1 O2 V1 139.77(13) . . . . ?
C10 C15 O3 V1 -54.5(2) . . . . ?
C14 C15 O3 V1 126.86(15) . . . . ?
O5 C17 O4 V1 -179.20(13) . . . . ?
C16 C17 O4 V1 2.6(2) . . . . ?
O4 C17 O5 C35 2.5(3) . . . . ?
C16 C17 O5 C35 -179.12(17) . . . . ?
C34 O6 V1 O1 21.77(15) . . . . ?
C34 O6 V1 O2 123.89(14) . . . . ?
C34 O6 V1 O3 -77.56(15) . . . . ?
C34 O6 V1 N8 -168.05(17) . . . . ?
C34 O6 V1 O4 -158.21(14) . . . . ?
C1 O2 V1 O1 -25.88(13) . . . . ?
C1 O2 V1 O6 -131.62(12) . . . . ?
C1 O2 V1 O3 109.24(16) . . . . ?
C1 O2 V1 N8 64.58(12) . . . . ?
C1 O2 V1 O4 139.56(13) . . . . ?
C15 O3 V1 O1 135.24(14) . . . . ?
C15 O3 V1 O6 -119.44(14) . . . . ?
C15 O3 V1 O2 -0.3(2) . . . . ?
C15 O3 V1 N8 43.38(14) . . . . ?
C15 O3 V1 O4 -30.31(14) . . . . ?
C16 N8 V1 O1 154.48(11) . . . . ?
C7 N8 V1 O1 34.81(11) . . . . ?
C9 N8 V1 O1 -83.75(11) . . . . ?
C16 N8 V1 O6 -16.0(2) . . . . ?
C7 N8 V1 O6 -135.67(17) . . . . ?
C9 N8 V1 O6 105.77(19) . . . . ?
C16 N8 V1 O2 54.65(10) . . . . ?
C7 N8 V1 O2 -65.02(10) . . . . ?
C9 N8 V1 O2 176.42(11) . . . . ?
C16 N8 V1 O3 -108.25(10) . . . . ?
C7 N8 V1 O3 132.08(10) . . . . ?
C9 N8 V1 O3 13.52(10) . . . . ?
C16 N8 V1 O4 -26.30(10) . . . . ?
C7 N8 V1 O4 -145.96(10) . . . . ?
C9 N8 V1 O4 95.48(10) . . . . ?
C17 O4 V1 O1 16.7(3) . . . . ?
C17 O4 V1 O6 -163.37(11) . . . . ?
C17 O4 V1 O2 -67.16(11) . . . . ?
C17 O4 V1 O3 100.54(12) . . . . ?
C17 O4 V1 N8 13.62(11) . . . . ?

# END of CIF

_database_code_depnum_ccdc_archive 'CCDC 977976'
