# 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.
#
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#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
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#  except for the purpose of generating routine backup copies
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#  data retrieval see:
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#  from this site to visualise CIF-encoded structures and 
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data_1.2MeCN

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C44 H56 N2 O5 V, 2(C2 H3 N)'
_chemical_formula_sum            'C48 H62 N4 O5 V'
_chemical_formula_weight         825.96

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/n'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_Int_Tables_number      14

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                   17.946(4)
_cell_length_b                   9.2015(18)
_cell_length_c                   28.165(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 95.87(3)
_cell_angle_gamma                90.00
_cell_volume                     4626.6(16)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    25257
_cell_measurement_theta_min      1.29
_cell_measurement_theta_max      25.00

_exptl_crystal_description       plate
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.186
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1764
_exptl_absorpt_coefficient_mu    0.262
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_absorpt_correction_T_min  0.6000
_exptl_absorpt_correction_T_max  1.0000

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Saturn724+ CCD'
_diffrn_measurement_method       'ω scans at fixed χ = 45°'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         none
_diffrn_standards_interval_count none
_diffrn_standards_interval_time  none
_diffrn_standards_decay_%        none
_diffrn_reflns_number            25257
_diffrn_reflns_av_R_equivalents  0.0639
_diffrn_reflns_av_unetI/netI     0.0651
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_theta_min         1.29
_diffrn_reflns_theta_max         25.00
_reflns_number_total             8083
_reflns_number_gt                6683
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrystalClear (Rigaku Inc., 2007)'
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2007)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'CAMERON (Watkin et al, 1993)'
_computing_publication_material  'SHELX97 (Sheldrick, 1997)'

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

 Non-hydrogen atoms closer than 1.7 Α were restrainted to have the
 same U(ij) values with an e.s.d. of 0.01 (SIMU 0.01 0.02 1.7). 
 The thermal parameters of non-hydrogen atoms were restrained to
 approximate to isotropic behaviour with an e.s.d. of 0.01
 (ISOR 0.01).
;

_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)+(0.1449P)²+3.5934P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         8083
_refine_ls_number_parameters     570
_refine_ls_number_restraints     762
_refine_ls_R_factor_ref          0.1114
_refine_ls_R_factor_gt           0.0830
_refine_ls_wR_factor_ref         0.2740
_refine_ls_wR_factor_gt          0.2311
_refine_ls_goodness_of_fit_ref   1.218
_refine_ls_restrained_S_all      1.180
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
V1 V 0.98187(4) 0.30488(8) 0.19511(2) 0.0254(2) Uani 1 1 d U . .
O1 O 1.03434(18) 0.1819(4) 0.17635(13) 0.0432(8) Uani 1 1 d U . .
C11 C 0.9436(3) 0.3053(5) 0.35951(15) 0.0348(10) Uani 1 1 d U . .
O3 O 0.98212(16) 0.3291(3) 0.26224(10) 0.0291(7) Uani 1 1 d U . .
O5 O 1.10154(19) 0.7564(4) 0.17640(12) 0.0408(8) Uani 1 1 d U . .
C20 C 1.1385(3) 0.6927(6) 0.09855(17) 0.0416(11) Uani 1 1 d U . .
H20 H 1.1493 0.7910 0.0916 0.050 Uiso 1 1 calc R . .
N2 N 1.06633(19) 0.4686(4) 0.19612(12) 0.0280(8) Uani 1 1 d U . .
N1 N 0.88944(19) 0.1603(4) 0.19613(11) 0.0256(7) Uani 1 1 d U . .
C25 C 0.9099(3) -0.1917(5) 0.29287(19) 0.0471(12) Uani 1 1 d U . .
H25 H 0.9160 -0.2678 0.3157 0.057 Uiso 1 1 calc R . .
C32 C 0.7175(2) 0.3511(5) 0.06500(15) 0.0318(9) Uani 1 1 d U A .
C31 C 0.7441(2) 0.2505(5) 0.09909(14) 0.0284(9) Uani 1 1 d U . .
H31 H 0.7166 0.1636 0.1026 0.034 Uiso 1 1 calc R . .
O4 O 0.77297(17) 0.0885(4) 0.24999(11) 0.0399(8) Uani 1 1 d U . .
C8 C 1.0214(2) 0.4092(5) 0.29574(14) 0.0275(9) Uani 1 1 d U . .
O2 O 0.92099(16) 0.4193(3) 0.14946(10) 0.0295(7) Uani 1 1 d U . .
C40 C 0.7592(2) 0.4802(5) 0.06251(14) 0.0300(9) Uani 1 1 d U . .
H40 H 0.7406 0.5515 0.0399 0.036 Uiso 1 1 calc R . .
C41 C 0.8259(2) 0.5111(5) 0.09087(14) 0.0269(9) Uani 1 1 d U . .
C7 C 1.0807(2) 0.4990(4) 0.28354(14) 0.0268(9) Uani 1 1 d U . .
C10 C 1.0484(2) 0.4929(5) 0.37654(15) 0.0306(9) Uani 1 1 d U . .
H10 H 1.0363 0.4923 0.4086 0.037 Uiso 1 1 calc R . .
C30 C 0.8116(2) 0.2747(5) 0.12887(14) 0.0259(9) Uani 1 1 d U . .
C15 C 1.1008(2) 0.5184(5) 0.23561(15) 0.0292(9) Uani 1 1 d U . .
H15 H 1.1446 0.5743 0.2326 0.035 Uiso 1 1 calc R . .
C12 C 0.9335(3) 0.3220(7) 0.41345(18) 0.0513(14) Uani 1 1 d U . .
H12A H 0.9812 0.3022 0.4325 0.077 Uiso 1 1 calc R . .
H12B H 0.8956 0.2530 0.4222 0.077 Uiso 1 1 calc R . .
H12C H 0.9173 0.4213 0.4197 0.077 Uiso 1 1 calc R . .
C33 C 0.6478(3) 0.3217(5) 0.02976(16) 0.0370(11) Uani 1 1 d U . .
C16 C 1.0969(2) 0.5080(5) 0.15226(15) 0.0321(10) Uani 1 1 d U . .
C4 C 1.1559(3) 0.6712(5) 0.40331(17) 0.0408(11) Uani 1 1 d U . .
C42 C 0.8543(2) 0.4002(5) 0.12392(13) 0.0261(9) Uani 1 1 d U . .
C43 C 0.8685(3) 0.6537(5) 0.08457(15) 0.0326(10) Uani 1 1 d U . .
C45 C 0.9411(2) 0.6201(6) 0.06113(16) 0.0390(11) Uani 1 1 d U . .
H45A H 0.9731 0.5553 0.0819 0.059 Uiso 1 1 calc R . .
H45B H 0.9679 0.7109 0.0564 0.059 Uiso 1 1 calc R . .
H45C H 0.9281 0.5729 0.0302 0.059 Uiso 1 1 calc R . .
C26 C 0.8445(3) -0.1129(5) 0.28851(17) 0.0404(11) Uani 1 1 d U . .
H26 H 0.8054 -0.1382 0.3073 0.048 Uiso 1 1 calc R . .
C9 C 1.0049(2) 0.4051(5) 0.34370(14) 0.0302(9) Uani 1 1 d U . .
C1K C 1.1129(3) 0.6552(5) 0.14220(16) 0.0365(10) Uani 1 1 d U . .
C5 C 1.1072(2) 0.5800(5) 0.36605(15) 0.0319(10) Uani 1 1 d U . .
C6 C 1.1232(2) 0.5820(5) 0.31880(15) 0.0320(10) Uani 1 1 d U . .
H6 H 1.1634 0.6401 0.3101 0.038 Uiso 1 1 calc R . .
C27 C 0.8348(2) 0.0043(5) 0.25671(15) 0.0323(10) Uani 1 1 d U . .
C19 C 1.1478(3) 0.5835(6) 0.06535(17) 0.0434(11) Uani 1 1 d U . .
H19 H 1.1634 0.6094 0.0353 0.052 Uiso 1 1 calc R . .
N3 N 1.2362(3) 0.2824(7) 0.2351(2) 0.0771(17) Uani 1 1 d U . .
C46 C 0.8891(3) 0.7337(5) 0.13248(16) 0.0415(12) Uani 1 1 d U . .
H46A H 0.8433 0.7678 0.1451 0.062 Uiso 1 1 calc R . .
H46B H 0.9213 0.8169 0.1273 0.062 Uiso 1 1 calc R . .
H46C H 0.9157 0.6669 0.1554 0.062 Uiso 1 1 calc R . .
C2 C 1.1256(4) 0.6688(8) 0.4521(2) 0.0663(18) Uani 1 1 d U . .
H2A H 1.0759 0.7137 0.4496 0.099 Uiso 1 1 calc R . .
H2B H 1.1596 0.7231 0.4751 0.099 Uiso 1 1 calc R . .
H2C H 1.1220 0.5680 0.4629 0.099 Uiso 1 1 calc R . .
C22 C 0.8943(2) 0.0370(5) 0.22874(15) 0.0305(9) Uani 1 1 d U . .
C44 C 0.8219(3) 0.7616(6) 0.05186(18) 0.0447(12) Uani 1 1 d U . .
H44A H 0.8122 0.7200 0.0198 0.067 Uiso 1 1 calc R . .
H44B H 0.8497 0.8529 0.0502 0.067 Uiso 1 1 calc R . .
H44C H 0.7742 0.7806 0.0648 0.067 Uiso 1 1 calc R . .
C29 C 0.8307(2) 0.1629(5) 0.16442(14) 0.0265(9) Uani 1 1 d U . .
H29 H 0.7970 0.0832 0.1647 0.032 Uiso 1 1 calc R . .
C17 C 1.1088(2) 0.4039(5) 0.11875(16) 0.0354(10) Uani 1 1 d U . .
H17 H 1.0991 0.3050 0.1255 0.042 Uiso 1 1 calc R . .
C23 C 0.9584(3) -0.0469(5) 0.23324(16) 0.0369(10) Uani 1 1 d U . .
H23 H 0.9978 -0.0250 0.2143 0.044 Uiso 1 1 calc R . .
C18 C 1.1350(3) 0.4393(7) 0.07481(18) 0.0462(12) Uani 1 1 d U . .
H18 H 1.1436 0.3659 0.0523 0.055 Uiso 1 1 calc R . .
C14 C 0.8669(3) 0.3419(7) 0.33153(19) 0.0495(13) Uani 1 1 d U . .
H14A H 0.8285 0.2762 0.3416 0.074 Uiso 1 1 calc R . .
H14B H 0.8704 0.3300 0.2972 0.074 Uiso 1 1 calc R . .
H14C H 0.8534 0.4426 0.3381 0.074 Uiso 1 1 calc R . .
C24 C 0.9664(3) -0.1630(6) 0.26503(19) 0.0481(12) Uani 1 1 d U . .
H24 H 1.0102 -0.2213 0.2674 0.058 Uiso 1 1 calc R . .
C50 C 1.2058(4) 0.2196(8) 0.2616(3) 0.0640(17) Uani 1 1 d U . .
C3 C 1.2349(3) 0.6073(7) 0.4092(2) 0.0612(16) Uani 1 1 d U . .
H3A H 1.2324 0.5044 0.4178 0.092 Uiso 1 1 calc R . .
H3B H 1.2655 0.6599 0.4345 0.092 Uiso 1 1 calc R . .
H3C H 1.2576 0.6169 0.3792 0.092 Uiso 1 1 calc R . .
N4 N 1.0797(4) 0.0387(6) 0.0459(2) 0.0754(16) Uani 1 1 d U . .
C48 C 1.0246(4) 0.1039(7) 0.0478(2) 0.0585(15) Uani 1 1 d U . .
C13 C 0.9656(3) 0.1452(6) 0.35158(17) 0.0460(12) Uani 1 1 d U . .
H13A H 1.0120 0.1226 0.3716 0.069 Uiso 1 1 calc R . .
H13B H 0.9732 0.1306 0.3180 0.069 Uiso 1 1 calc R . .
H13C H 0.9255 0.0810 0.3601 0.069 Uiso 1 1 calc R . .
C21 C 1.1325(3) 0.8974(6) 0.1705(2) 0.0513(14) Uani 1 1 d U . .
H21A H 1.1050 0.9458 0.1431 0.077 Uiso 1 1 calc R . .
H21B H 1.1854 0.8881 0.1649 0.077 Uiso 1 1 calc R . .
H21C H 1.1285 0.9552 0.1993 0.077 Uiso 1 1 calc R . .
C28 C 0.7141(3) 0.0595(7) 0.27969(18) 0.0499(13) Uani 1 1 d U . .
H28A H 0.6717 0.1244 0.2707 0.075 Uiso 1 1 calc R . .
H28B H 0.7327 0.0762 0.3132 0.075 Uiso 1 1 calc R . .
H28C H 0.6978 -0.0417 0.2755 0.075 Uiso 1 1 calc R . .
C1 C 1.1606(4) 0.8283(7) 0.3862(2) 0.0695(18) Uani 1 1 d U . .
H1A H 1.1868 0.8311 0.3574 0.104 Uiso 1 1 calc R . .
H1B H 1.1881 0.8868 0.4113 0.104 Uiso 1 1 calc R . .
H1C H 1.1099 0.8675 0.3791 0.104 Uiso 1 1 calc R . .
C49 C 1.1671(5) 0.1394(9) 0.2967(3) 0.093(2) Uani 1 1 d U . .
H49A H 1.1129 0.1414 0.2873 0.139 Uiso 1 1 calc R . .
H49B H 1.1778 0.1846 0.3282 0.139 Uiso 1 1 calc R . .
H49C H 1.1845 0.0384 0.2981 0.139 Uiso 1 1 calc R . .
C47 C 0.9561(4) 0.1841(8) 0.0488(3) 0.080(2) Uani 1 1 d U . .
H47A H 0.9195 0.1506 0.0230 0.120 Uiso 1 1 calc R . .
H47B H 0.9659 0.2879 0.0447 0.120 Uiso 1 1 calc R . .
H47C H 0.9362 0.1686 0.0796 0.120 Uiso 1 1 calc R . .
C39 C 0.6723(5) 0.3076(9) -0.0223(3) 0.045(2) Uani 0.650(7) 1 d PU A 1
H39A H 0.7005 0.3943 -0.0298 0.068 Uiso 0.650(7) 1 calc PR A 1
H39B H 0.6277 0.2985 -0.0452 0.068 Uiso 0.650(7) 1 calc PR A 1
H39C H 0.7038 0.2213 -0.0241 0.068 Uiso 0.650(7) 1 calc PR A 1
C37 C 0.5926(5) 0.4449(10) 0.0282(4) 0.054(2) Uani 0.650(7) 1 d PU A 1
H37A H 0.5693 0.4480 0.0582 0.081 Uiso 0.650(7) 1 calc PR A 1
H37B H 0.5538 0.4303 0.0015 0.081 Uiso 0.650(7) 1 calc PR A 1
H37C H 0.6186 0.5369 0.0239 0.081 Uiso 0.650(7) 1 calc PR A 1
C35 C 0.6069(5) 0.1808(10) 0.0406(3) 0.051(2) Uani 0.650(7) 1 d PU A 1
H35A H 0.6396 0.0974 0.0366 0.077 Uiso 0.650(7) 1 calc PR A 1
H35B H 0.5611 0.1716 0.0187 0.077 Uiso 0.650(7) 1 calc PR A 1
H35C H 0.5938 0.1834 0.0736 0.077 Uiso 0.650(7) 1 calc PR A 1
C36 C 0.5811(7) 0.2928(18) 0.0609(5) 0.045(3) Uani 0.350(7) 1 d PU A 2
H36A H 0.6011 0.2567 0.0924 0.068 Uiso 0.350(7) 1 calc PR A 2
H36B H 0.5472 0.2202 0.0451 0.068 Uiso 0.350(7) 1 calc PR A 2
H36C H 0.5537 0.3835 0.0646 0.068 Uiso 0.350(7) 1 calc PR A 2
C38 C 0.6275(8) 0.4473(17) -0.0030(6) 0.046(3) Uani 0.350(7) 1 d PU A 2
H38A H 0.6150 0.5318 0.0158 0.069 Uiso 0.350(7) 1 calc PR A 2
H38B H 0.5843 0.4211 -0.0255 0.069 Uiso 0.350(7) 1 calc PR A 2
H38C H 0.6701 0.4709 -0.0208 0.069 Uiso 0.350(7) 1 calc PR A 2
C34 C 0.6621(9) 0.1914(18) 0.0034(6) 0.051(4) Uani 0.350(7) 1 d PU A 2
H34A H 0.7118 0.1979 -0.0080 0.077 Uiso 0.350(7) 1 calc PR A 2
H34B H 0.6241 0.1816 -0.0239 0.077 Uiso 0.350(7) 1 calc PR A 2
H34C H 0.6602 0.1065 0.0243 0.077 Uiso 0.350(7) 1 calc PR A 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
V1 O1 1.596(3) . ?
V1 O3 1.904(3) . ?
V1 O2 1.915(3) . ?
V1 N1 2.129(3) . ?
V1 N2 2.135(4) . ?
C11 C9 1.535(6) . ?
C11 C13 1.547(7) . ?
C11 C14 1.551(7) . ?
C11 C12 1.556(6) . ?
O3 C8 1.339(5) . ?
O5 C1K 1.370(6) . ?
O5 C21 1.429(6) . ?
C20 C19 1.394(7) . ?
C20 C1K 1.399(7) . ?
C20 H20 0.9500 . ?
N2 C15 1.299(5) . ?
N2 C16 1.449(5) . ?
N1 C29 1.311(5) . ?
N1 C22 1.457(5) . ?
C25 C24 1.369(8) . ?
C25 C26 1.373(7) . ?
C25 H25 0.9500 . ?
C32 C31 1.383(6) . ?
C32 C40 1.410(6) . ?
C32 C33 1.539(6) . ?
C31 C30 1.419(5) . ?
C31 H31 0.9500 . ?
O4 C27 1.351(5) . ?
O4 C28 1.438(6) . ?
C8 C9 1.412(6) . ?
C8 C7 1.418(6) . ?
O2 C42 1.343(5) . ?
C40 C41 1.400(6) . ?
C40 H40 0.9500 . ?
C41 C42 1.439(6) . ?
C41 C43 1.537(6) . ?
C7 C6 1.413(6) . ?
C7 C15 1.443(6) . ?
C10 C5 1.381(6) . ?
C10 C9 1.402(6) . ?
C10 H10 0.9500 . ?
C30 C42 1.401(6) . ?
C30 C29 1.452(6) . ?
C15 H15 0.9500 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C33 C34 1.447(17) . ?
C33 C38 1.500(15) . ?
C33 C37 1.504(10) . ?
C33 C35 1.536(10) . ?
C33 C36 1.576(15) . ?
C33 C39 1.578(9) . ?
C16 C17 1.377(7) . ?
C16 C1K 1.418(7) . ?
C4 C1 1.528(8) . ?
C4 C3 1.529(8) . ?
C4 C2 1.529(8) . ?
C4 C5 1.544(6) . ?
C43 C44 1.542(6) . ?
C43 C46 1.548(6) . ?
C43 C45 1.550(7) . ?
C45 H45A 0.9800 . ?
C45 H45B 0.9800 . ?
C45 H45C 0.9800 . ?
C26 C27 1.401(6) . ?
C26 H26 0.9500 . ?
C5 C6 1.390(6) . ?
C6 H6 0.9500 . ?
C27 C22 1.421(6) . ?
C19 C18 1.377(8) . ?
C19 H19 0.9500 . ?
N3 C50 1.126(9) . ?
C46 H46A 0.9800 . ?
C46 H46B 0.9800 . ?
C46 H46C 0.9800 . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C22 C23 1.382(6) . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 0.9800 . ?
C29 H29 0.9500 . ?
C17 C18 1.406(7) . ?
C17 H17 0.9500 . ?
C23 C24 1.391(7) . ?
C23 H23 0.9500 . ?
C18 H18 0.9500 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C24 H24 0.9500 . ?
C50 C49 1.466(11) . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
N4 C48 1.162(8) . ?
C48 C47 1.437(10) . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C49 H49A 0.9800 . ?
C49 H49B 0.9800 . ?
C49 H49C 0.9800 . ?
C47 H47A 0.9800 . ?
C47 H47B 0.9800 . ?
C47 H47C 0.9800 . ?
C39 H39A 0.9800 . ?
C39 H39B 0.9800 . ?
C39 H39C 0.9800 . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 V1 O3 118.06(16) . . ?
O1 V1 O2 118.87(16) . . ?
O3 V1 O2 123.06(13) . . ?
O1 V1 N1 92.77(15) . . ?
O3 V1 N1 88.99(13) . . ?
O2 V1 N1 87.75(13) . . ?
O1 V1 N2 93.59(16) . . ?
O3 V1 N2 88.53(13) . . ?
O2 V1 N2 88.66(13) . . ?
N1 V1 N2 173.60(14) . . ?
C9 C11 C13 109.1(4) . . ?
C9 C11 C14 110.4(4) . . ?
C13 C11 C14 111.1(4) . . ?
C9 C11 C12 112.5(4) . . ?
C13 C11 C12 107.0(4) . . ?
C14 C11 C12 106.8(4) . . ?
C8 O3 V1 135.4(3) . . ?
C1K O5 C21 116.6(4) . . ?
C19 C20 C1K 119.0(5) . . ?
C19 C20 H20 120.5 . . ?
C1K C20 H20 120.5 . . ?
C15 N2 C16 116.9(4) . . ?
C15 N2 V1 122.4(3) . . ?
C16 N2 V1 119.7(3) . . ?
C29 N1 C22 115.8(3) . . ?
C29 N1 V1 123.6(3) . . ?
C22 N1 V1 119.9(3) . . ?
C24 C25 C26 121.5(5) . . ?
C24 C25 H25 119.3 . . ?
C26 C25 H25 119.3 . . ?
C31 C32 C40 116.8(4) . . ?
C31 C32 C33 122.1(4) . . ?
C40 C32 C33 121.1(4) . . ?
C32 C31 C30 121.3(4) . . ?
C32 C31 H31 119.3 . . ?
C30 C31 H31 119.3 . . ?
C27 O4 C28 117.1(4) . . ?
O3 C8 C9 120.9(4) . . ?
O3 C8 C7 120.3(4) . . ?
C9 C8 C7 118.9(4) . . ?
C42 O2 V1 134.7(3) . . ?
C41 C40 C32 124.8(4) . . ?
C41 C40 H40 117.6 . . ?
C32 C40 H40 117.6 . . ?
C40 C41 C42 116.8(4) . . ?
C40 C41 C43 120.9(4) . . ?
C42 C41 C43 122.2(4) . . ?
C6 C7 C8 120.6(4) . . ?
C6 C7 C15 115.0(4) . . ?
C8 C7 C15 124.3(4) . . ?
C5 C10 C9 125.3(4) . . ?
C5 C10 H10 117.3 . . ?
C9 C10 H10 117.3 . . ?
C42 C30 C31 120.8(4) . . ?
C42 C30 C29 124.1(4) . . ?
C31 C30 C29 115.1(4) . . ?
N2 C15 C7 127.9(4) . . ?
N2 C15 H15 116.0 . . ?
C7 C15 H15 116.0 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C34 C33 C38 111.5(10) . . ?
C34 C33 C37 139.6(7) . . ?
C34 C33 C35 61.1(8) . . ?
C38 C33 C35 133.0(7) . . ?
C37 C33 C35 108.4(6) . . ?
C34 C33 C32 107.5(7) . . ?
C38 C33 C32 113.0(7) . . ?
C37 C33 C32 112.1(5) . . ?
C35 C33 C32 113.1(4) . . ?
C34 C33 C36 109.3(10) . . ?
C38 C33 C36 108.8(9) . . ?
C37 C33 C36 66.9(7) . . ?
C35 C33 C36 48.8(7) . . ?
C32 C33 C36 106.5(6) . . ?
C34 C33 C39 51.3(7) . . ?
C38 C33 C39 64.2(8) . . ?
C37 C33 C39 106.3(6) . . ?
C35 C33 C39 107.5(5) . . ?
C32 C33 C39 109.1(4) . . ?
C36 C33 C39 143.4(7) . . ?
C17 C16 C1K 118.6(4) . . ?
C17 C16 N2 120.6(4) . . ?
C1K C16 N2 120.7(4) . . ?
C1 C4 C3 108.5(5) . . ?
C1 C4 C2 109.5(5) . . ?
C3 C4 C2 107.9(5) . . ?
C1 C4 C5 110.2(4) . . ?
C3 C4 C5 108.7(4) . . ?
C2 C4 C5 112.0(4) . . ?
O2 C42 C30 121.4(4) . . ?
O2 C42 C41 119.4(4) . . ?
C30 C42 C41 119.2(4) . . ?
C41 C43 C44 111.9(4) . . ?
C41 C43 C46 112.5(4) . . ?
C44 C43 C46 106.3(4) . . ?
C41 C43 C45 109.2(4) . . ?
C44 C43 C45 107.6(4) . . ?
C46 C43 C45 109.3(4) . . ?
C43 C45 H45A 109.5 . . ?
C43 C45 H45B 109.5 . . ?
H45A C45 H45B 109.5 . . ?
C43 C45 H45C 109.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?
C25 C26 C27 120.8(5) . . ?
C25 C26 H26 119.6 . . ?
C27 C26 H26 119.6 . . ?
C10 C9 C8 117.3(4) . . ?
C10 C9 C11 121.3(4) . . ?
C8 C9 C11 121.3(4) . . ?
O5 C1K C20 122.4(4) . . ?
O5 C1K C16 117.5(4) . . ?
C20 C1K C16 120.1(5) . . ?
C10 C5 C6 116.8(4) . . ?
C10 C5 C4 124.2(4) . . ?
C6 C5 C4 119.0(4) . . ?
C5 C6 C7 121.0(4) . . ?
C5 C6 H6 119.5 . . ?
C7 C6 H6 119.5 . . ?
O4 C27 C26 125.2(4) . . ?
O4 C27 C22 117.0(4) . . ?
C26 C27 C22 117.8(4) . . ?
C18 C19 C20 122.1(5) . . ?
C18 C19 H19 119.0 . . ?
C20 C19 H19 119.0 . . ?
C43 C46 H46A 109.5 . . ?
C43 C46 H46B 109.5 . . ?
H46A C46 H46B 109.5 . . ?
C43 C46 H46C 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
C4 C2 H2A 109.5 . . ?
C4 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
C4 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
C23 C22 C27 119.8(4) . . ?
C23 C22 N1 119.2(4) . . ?
C27 C22 N1 121.0(4) . . ?
C43 C44 H44A 109.5 . . ?
C43 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
C43 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
N1 C29 C30 126.8(4) . . ?
N1 C29 H29 116.6 . . ?
C30 C29 H29 116.6 . . ?
C16 C17 C18 122.1(5) . . ?
C16 C17 H17 118.9 . . ?
C18 C17 H17 118.9 . . ?
C22 C23 C24 121.1(5) . . ?
C22 C23 H23 119.4 . . ?
C24 C23 H23 119.4 . . ?
C19 C18 C17 118.1(5) . . ?
C19 C18 H18 121.0 . . ?
C17 C18 H18 121.0 . . ?
C11 C14 H14A 109.5 . . ?
C11 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C11 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C25 C24 C23 118.9(5) . . ?
C25 C24 H24 120.5 . . ?
C23 C24 H24 120.5 . . ?
N3 C50 C49 178.9(9) . . ?
C4 C3 H3A 109.5 . . ?
C4 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
C4 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
N4 C48 C47 178.5(7) . . ?
C11 C13 H13A 109.5 . . ?
C11 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C11 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
O5 C21 H21A 109.5 . . ?
O5 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
O5 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
O4 C28 H28A 109.5 . . ?
O4 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
O4 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C4 C1 H1A 109.5 . . ?
C4 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
C4 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C50 C49 H49A 109.5 . . ?
C50 C49 H49B 109.5 . . ?
H49A C49 H49B 109.5 . . ?
C50 C49 H49C 109.5 . . ?
H49A C49 H49C 109.5 . . ?
H49B C49 H49C 109.5 . . ?
C48 C47 H47A 109.5 . . ?
C48 C47 H47B 109.5 . . ?
H47A C47 H47B 109.5 . . ?
C48 C47 H47C 109.5 . . ?
H47A C47 H47C 109.5 . . ?
H47B C47 H47C 109.5 . . ?
C33 C39 H39A 109.5 . . ?
C33 C39 H39B 109.5 . . ?
C33 C39 H39C 109.5 . . ?
C33 C37 H37A 109.5 . . ?
C33 C37 H37B 109.5 . . ?
C33 C37 H37C 109.5 . . ?
C33 C35 H35A 109.5 . . ?
C33 C35 H35B 109.5 . . ?
C33 C35 H35C 109.5 . . ?
C33 C36 H36A 109.5 . . ?
C33 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C33 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C33 C38 H38A 109.5 . . ?
C33 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
C33 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
C33 C34 H34A 109.5 . . ?
C33 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
C33 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?

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 O3 C8 90.3(4) . . . . ?
O2 V1 O3 C8 -90.5(4) . . . . ?
N1 V1 O3 C8 -177.1(4) . . . . ?
N2 V1 O3 C8 -3.0(4) . . . . ?
O1 V1 N2 C15 -107.5(4) . . . . ?
O3 V1 N2 C15 10.5(3) . . . . ?
O2 V1 N2 C15 133.6(3) . . . . ?
O1 V1 N2 C16 60.7(3) . . . . ?
O3 V1 N2 C16 178.7(3) . . . . ?
O2 V1 N2 C16 -58.1(3) . . . . ?
O1 V1 N1 C29 -105.4(3) . . . . ?
O3 V1 N1 C29 136.5(3) . . . . ?
O2 V1 N1 C29 13.4(3) . . . . ?
O1 V1 N1 C22 64.9(3) . . . . ?
O3 V1 N1 C22 -53.1(3) . . . . ?
O2 V1 N1 C22 -176.3(3) . . . . ?
C40 C32 C31 C30 -2.2(6) . . . . ?
C33 C32 C31 C30 175.1(4) . . . . ?
V1 O3 C8 C9 177.6(3) . . . . ?
V1 O3 C8 C7 -2.9(6) . . . . ?
O1 V1 O2 C42 82.0(4) . . . . ?
O3 V1 O2 C42 -97.2(4) . . . . ?
N1 V1 O2 C42 -9.9(4) . . . . ?
N2 V1 O2 C42 175.4(4) . . . . ?
C31 C32 C40 C41 2.0(7) . . . . ?
C33 C32 C40 C41 -175.3(4) . . . . ?
C32 C40 C41 C42 1.7(6) . . . . ?
C32 C40 C41 C43 178.4(4) . . . . ?
O3 C8 C7 C6 -178.9(4) . . . . ?
C9 C8 C7 C6 0.6(6) . . . . ?
O3 C8 C7 C15 3.6(6) . . . . ?
C9 C8 C7 C15 -176.9(4) . . . . ?
C32 C31 C30 C42 -1.3(6) . . . . ?
C32 C31 C30 C29 177.3(4) . . . . ?
C16 N2 C15 C7 178.0(4) . . . . ?
V1 N2 C15 C7 -13.5(6) . . . . ?
C6 C7 C15 N2 -171.9(4) . . . . ?
C8 C7 C15 N2 5.6(7) . . . . ?
C31 C32 C33 C34 -58.3(9) . . . . ?
C40 C32 C33 C34 118.9(8) . . . . ?
C31 C32 C33 C38 178.2(8) . . . . ?
C40 C32 C33 C38 -4.6(10) . . . . ?
C31 C32 C33 C37 130.0(6) . . . . ?
C40 C32 C33 C37 -52.8(7) . . . . ?
C31 C32 C33 C35 7.1(7) . . . . ?
C40 C32 C33 C35 -175.7(5) . . . . ?
C31 C32 C33 C36 58.7(8) . . . . ?
C40 C32 C33 C36 -124.1(8) . . . . ?
C31 C32 C33 C39 -112.5(6) . . . . ?
C40 C32 C33 C39 64.7(6) . . . . ?
C15 N2 C16 C17 131.4(4) . . . . ?
V1 N2 C16 C17 -37.5(5) . . . . ?
C15 N2 C16 C1K -50.8(6) . . . . ?
V1 N2 C16 C1K 140.3(3) . . . . ?
V1 O2 C42 C30 2.2(6) . . . . ?
V1 O2 C42 C41 -177.9(3) . . . . ?
C31 C30 C42 O2 -175.1(4) . . . . ?
C29 C30 C42 O2 6.5(6) . . . . ?
C31 C30 C42 C41 5.1(6) . . . . ?
C29 C30 C42 C41 -173.4(4) . . . . ?
C40 C41 C42 O2 175.0(4) . . . . ?
C43 C41 C42 O2 -1.6(6) . . . . ?
C40 C41 C42 C30 -5.2(6) . . . . ?
C43 C41 C42 C30 178.2(4) . . . . ?
C40 C41 C43 C44 10.6(6) . . . . ?
C42 C41 C43 C44 -172.9(4) . . . . ?
C40 C41 C43 C46 130.2(4) . . . . ?
C42 C41 C43 C46 -53.3(6) . . . . ?
C40 C41 C43 C45 -108.4(4) . . . . ?
C42 C41 C43 C45 68.1(5) . . . . ?
C24 C25 C26 C27 -2.9(8) . . . . ?
C5 C10 C9 C8 -1.9(7) . . . . ?
C5 C10 C9 C11 176.4(4) . . . . ?
O3 C8 C9 C10 -179.6(4) . . . . ?
C7 C8 C9 C10 0.9(6) . . . . ?
O3 C8 C9 C11 2.1(6) . . . . ?
C7 C8 C9 C11 -177.4(4) . . . . ?
C13 C11 C9 C10 -115.0(4) . . . . ?
C14 C11 C9 C10 122.7(5) . . . . ?
C12 C11 C9 C10 3.6(6) . . . . ?
C13 C11 C9 C8 63.2(5) . . . . ?
C14 C11 C9 C8 -59.1(6) . . . . ?
C12 C11 C9 C8 -178.2(4) . . . . ?
C21 O5 C1K C20 -13.6(6) . . . . ?
C21 O5 C1K C16 166.9(4) . . . . ?
C19 C20 C1K O5 -179.3(4) . . . . ?
C19 C20 C1K C16 0.2(7) . . . . ?
C17 C16 C1K O5 -179.1(4) . . . . ?
N2 C16 C1K O5 3.1(6) . . . . ?
C17 C16 C1K C20 1.4(6) . . . . ?
N2 C16 C1K C20 -176.4(4) . . . . ?
C9 C10 C5 C6 1.2(7) . . . . ?
C9 C10 C5 C4 -177.7(4) . . . . ?
C1 C4 C5 C10 -129.1(5) . . . . ?
C3 C4 C5 C10 112.1(5) . . . . ?
C2 C4 C5 C10 -7.0(7) . . . . ?
C1 C4 C5 C6 52.0(6) . . . . ?
C3 C4 C5 C6 -66.8(6) . . . . ?
C2 C4 C5 C6 174.1(5) . . . . ?
C10 C5 C6 C7 0.3(6) . . . . ?
C4 C5 C6 C7 179.3(4) . . . . ?
C8 C7 C6 C5 -1.2(6) . . . . ?
C15 C7 C6 C5 176.5(4) . . . . ?
C28 O4 C27 C26 3.3(7) . . . . ?
C28 O4 C27 C22 -177.4(4) . . . . ?
C25 C26 C27 O4 -179.8(4) . . . . ?
C25 C26 C27 C22 1.0(7) . . . . ?
C1K C20 C19 C18 -2.3(7) . . . . ?
O4 C27 C22 C23 -178.7(4) . . . . ?
C26 C27 C22 C23 0.6(6) . . . . ?
O4 C27 C22 N1 2.9(6) . . . . ?
C26 C27 C22 N1 -177.8(4) . . . . ?
C29 N1 C22 C23 126.3(4) . . . . ?
V1 N1 C22 C23 -44.8(5) . . . . ?
C29 N1 C22 C27 -55.3(5) . . . . ?
V1 N1 C22 C27 133.6(3) . . . . ?
C22 N1 C29 C30 178.3(4) . . . . ?
V1 N1 C29 C30 -11.0(6) . . . . ?
C42 C30 C29 N1 -1.0(7) . . . . ?
C31 C30 C29 N1 -179.6(4) . . . . ?
C1K C16 C17 C18 -1.0(6) . . . . ?
N2 C16 C17 C18 176.8(4) . . . . ?
C27 C22 C23 C24 -0.4(7) . . . . ?
N1 C22 C23 C24 178.0(4) . . . . ?
C20 C19 C18 C17 2.6(7) . . . . ?
C16 C17 C18 C19 -1.0(7) . . . . ?
C26 C25 C24 C23 3.0(8) . . . . ?
C22 C23 C24 C25 -1.4(7) . . . . ?

_diffrn_measured_fraction_theta_max 0.994
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.994
_refine_diff_density_max         0.714
_refine_diff_density_min         -0.773
_refine_diff_density_rms         0.205

_database_code_depnum_ccdc_archive 'CCDC 980001'
#######################################################################
#
#                 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

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C44 H56 N2 O5 V'
_chemical_formula_sum            'C44 H56 N2 O5 V'
_chemical_formula_weight         743.85

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           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                   15.165(3)
_cell_length_b                   18.182(4)
_cell_length_c                   19.034(4)
_cell_angle_alpha                66.33(3)
_cell_angle_beta                 67.40(3)
_cell_angle_gamma                83.36(3)
_cell_volume                     4433.0(15)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    32972
_cell_measurement_theta_min      1.53
_cell_measurement_theta_max      25.00


_exptl_crystal_description       Plate
_exptl_crystal_colour            brown
_exptl_crystal_size_max          0.406
_exptl_crystal_size_mid          0.331
_exptl_crystal_size_min          0.265
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.115
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1588
_exptl_absorpt_coefficient_mu    0.266
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_absorpt_correction_T_min  0.6777
_exptl_absorpt_correction_T_max  1.0000
_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Saturn724+ CCD'
_diffrn_measurement_method       'ω scans at fixed χ = 45°'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         none
_diffrn_standards_interval_count none
_diffrn_standards_interval_time  none
_diffrn_standards_decay_%        none
_diffrn_reflns_number            32972
_diffrn_reflns_av_R_equivalents  0.0497
_diffrn_reflns_av_unetI/netI     0.0657
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         1.53
_diffrn_reflns_theta_max         25.00
_reflns_number_total             15504
_reflns_number_gt                12526
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrystalClear (Rigaku Inc., 2007)'
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2007)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'CAMERON (Watkin et al, 1993)'
_computing_publication_material  'SHELX97 (Sheldrick, 1997)'

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

 Non-hydrogen atoms closer than 1.7 Α were restrainted to have the
 same U(ij) values with an e.s.d. of 0.01 (SIMU 0.01 0.01 1.7). 
 The thermal parameters of non-hydrogen atoms were restrained to
 approximate to isotropic behaviour with an e.s.d. of 0.01
 (ISOR 0.01).

 The distrance between the atom pairs: C7 C3C, C6A C3C, C6 C3C,
 C8A C3C, C8 C3C and C7A C3C was restrained to 1.54 A.
;

_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)+(0.0793P)²+3.8039P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         15504
_refine_ls_number_parameters     996
_refine_ls_number_restraints     1326
_refine_ls_R_factor_ref          0.0820
_refine_ls_R_factor_gt           0.0661
_refine_ls_wR_factor_ref         0.1833
_refine_ls_wR_factor_gt          0.1710
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_restrained_S_all      1.055
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
V1 V 0.32562(3) 0.40598(3) 0.04239(3) 0.02266(14) Uani 1 1 d U . .
V2 V 0.67465(3) 0.07721(3) 0.47524(3) 0.02460(14) Uani 1 1 d U . .
C3 C 0.1072(2) 0.20073(19) 0.35156(19) 0.0325(7) Uani 1 1 d U . .
C4 C 0.9072(2) 0.2794(2) 0.1702(2) 0.0362(7) Uani 1 1 d U . .
O2 O 0.23277(14) 0.45768(11) 0.10602(12) 0.0271(5) Uani 1 1 d U . .
N2 N 0.24860(17) 0.29460(14) 0.12510(14) 0.0245(5) Uani 1 1 d U . .
O7 O 0.76088(14) 0.02298(12) 0.41094(12) 0.0285(5) Uani 1 1 d U . .
N3 N 0.60405(17) -0.03623(14) 0.55855(14) 0.0248(5) Uani 1 1 d U . .
N4 N 0.76401(18) 0.18241(15) 0.39607(15) 0.0279(6) Uani 1 1 d U . .
C10 C 0.4391(2) -0.10726(18) 0.77914(18) 0.0284(6) Uani 1 1 d U . .
N1 N 0.38366(17) 0.52178(14) -0.04596(14) 0.0236(5) Uani 1 1 d U . .
O1 O 0.42066(15) 0.37667(12) 0.06104(13) 0.0311(5) Uani 1 1 d U . .
O6 O 0.58358(15) 0.11792(12) 0.45476(13) 0.0319(5) Uani 1 1 d U . .
O8 O 0.69491(15) 0.08588(12) 0.56475(12) 0.0308(5) Uani 1 1 d U . .
O4 O 0.54853(16) 0.65174(14) -0.34519(13) 0.0390(5) Uani 1 1 d U . .
C16 C 0.5421(2) 0.59728(18) -0.26784(18) 0.0277(6) Uani 1 1 d U . .
O9 O 0.42700(16) -0.16229(14) 0.85742(13) 0.0391(6) Uani 1 1 d U . .
C19 C 0.2796(2) 0.33205(18) -0.12777(18) 0.0279(6) Uani 1 1 d U . .
O3 O 0.30800(15) 0.38774(12) -0.04325(12) 0.0293(5) Uani 1 1 d U . .
C1 C 0.4634(2) 0.53025(17) -0.12086(17) 0.0245(6) Uani 1 1 d U . .
O5 O 0.01847(17) 0.16302(16) 0.39684(14) 0.0480(6) Uani 1 1 d U . .
C1A C 0.2827(2) 0.28405(18) 0.24483(18) 0.0280(6) Uani 1 1 d U . .
H1A H 0.3417 0.3135 0.2089 0.034 Uiso 1 1 calc R . .
C1B C 0.2208(2) 0.26861(17) 0.21334(17) 0.0265(6) Uani 1 1 d U . .
C1C C 0.5235(2) -0.04252(18) 0.63324(17) 0.0255(6) Uani 1 1 d U . .
C1D C 0.5178(2) -0.10268(17) 0.70790(18) 0.0265(6) Uani 1 1 d U . .
H1D H 0.5665 -0.1404 0.7109 0.032 Uiso 1 1 calc R . .
C1E C 0.4520(2) 0.01186(19) 0.62757(19) 0.0297(7) Uani 1 1 d U . .
H1E H 0.4566 0.0528 0.5757 0.036 Uiso 1 1 calc R . .
C1F C 0.7920(2) 0.21197(18) 0.30716(18) 0.0295(7) Uani 1 1 d U . .
C1G C 0.5392(2) 0.47968(19) -0.11821(19) 0.0292(7) Uani 1 1 d U . .
H1G H 0.5378 0.4387 -0.0673 0.035 Uiso 1 1 calc R . .
C1H C 0.5808(2) 0.0450(2) 0.7559(2) 0.0405(8) Uani 1 1 d U . .
H1HA H 0.5663 0.0442 0.7103 0.061 Uiso 1 1 calc R . .
H1HB H 0.5507 0.0906 0.7697 0.061 Uiso 1 1 calc R . .
H1HC H 0.5559 -0.0052 0.8043 0.061 Uiso 1 1 calc R . .
O10 O 0.99968(17) 0.31015(16) 0.12538(14) 0.0478(6) Uani 1 1 d U . .
C1J C 0.4646(2) 0.58925(17) -0.19593(18) 0.0264(6) Uani 1 1 d U . .
H1J H 0.4126 0.6236 -0.1977 0.032 Uiso 1 1 calc R . .
C1K C 0.7266(2) 0.20649(18) 0.27445(19) 0.0299(7) Uani 1 1 d U . .
H1K H 0.6657 0.1798 0.3095 0.036 Uiso 1 1 calc R . .
C1L C 0.2557(2) 0.25517(19) 0.32993(19) 0.0311(7) Uani 1 1 d U . .
H1L H 0.2978 0.2647 0.3520 0.037 Uiso 1 1 calc R . .
C1M C 0.4147(3) 0.4304(2) -0.2346(2) 0.0439(9) Uani 1 1 d U . .
H1MA H 0.4301 0.4337 -0.1904 0.066 Uiso 1 1 calc R . .
H1MB H 0.4325 0.4817 -0.2824 0.066 Uiso 1 1 calc R . .
H1MC H 0.4503 0.3875 -0.2507 0.066 Uiso 1 1 calc R . .
C1N C 0.7703(2) -0.05191(17) 0.41559(17) 0.0245(6) Uani 1 1 d U . .
C1O C 0.1334(2) 0.22812(18) 0.26591(18) 0.0314(7) Uani 1 1 d U . .
H1O H 0.0911 0.2189 0.2439 0.038 Uiso 1 1 calc R . .
C1P C 0.1165(3) 0.4324(2) 0.2891(2) 0.0421(8) Uani 1 1 d U . .
H1PA H 0.1737 0.4120 0.2571 0.063 Uiso 1 1 calc R . .
H1PB H 0.0745 0.3871 0.3346 0.063 Uiso 1 1 calc R . .
H1PC H 0.1354 0.4653 0.3115 0.063 Uiso 1 1 calc R . .
C1Q C 0.8495(2) -0.07230(18) 0.35630(18) 0.0275(6) Uani 1 1 d U . .
C1R C 0.0641(2) 0.48308(18) 0.2336(2) 0.0338(7) Uani 1 1 d U . .
C18 C 0.6191(2) 0.54754(19) -0.2658(2) 0.0339(7) Uani 1 1 d U . .
H18 H 0.6722 0.5534 -0.3152 0.041 Uiso 1 1 calc R . .
C1S C 0.7297(2) 0.14290(18) 0.57483(18) 0.0272(6) Uani 1 1 d U . .
C1T C 0.2804(2) 0.32555(17) -0.05091(18) 0.0272(6) Uani 1 1 d U . .
C1U C 0.6172(2) 0.48972(19) -0.19099(19) 0.0324(7) Uani 1 1 d U . .
H1U H 0.6700 0.4563 -0.1892 0.039 Uiso 1 1 calc R . .
C1V C 0.2138(2) 0.53294(17) 0.09796(17) 0.0238(6) Uani 1 1 d U . .
C1W C 0.7862(2) 0.22958(18) 0.42275(19) 0.0294(7) Uani 1 1 d U . .
H1W H 0.8166 0.2797 0.3818 0.035 Uiso 1 1 calc R . .
C1X C 0.3740(2) 0.0057(2) 0.69852(19) 0.0317(7) Uani 1 1 d U . .
H1X H 0.3247 0.0428 0.6950 0.038 Uiso 1 1 calc R . .
C1Y C 0.4690(3) 0.6991(2) -0.3498(2) 0.0471(9) Uani 1 1 d U . .
H1YA H 0.4808 0.7342 -0.4076 0.071 Uiso 1 1 calc R . .
H1YB H 0.4588 0.7321 -0.3176 0.071 Uiso 1 1 calc R . .
H1YC H 0.4120 0.6641 -0.3276 0.071 Uiso 1 1 calc R . .
C1Z C 0.8822(2) 0.24679(19) 0.25563(19) 0.0329(7) Uani 1 1 d U . .
H1Z H 0.9273 0.2485 0.2784 0.039 Uiso 1 1 calc R . .
C21 C 0.8410(2) 0.27881(19) 0.13668(19) 0.0346(7) Uani 1 1 d U . .
H21 H 0.8563 0.3039 0.0787 0.041 Uiso 1 1 calc R . .
C22 C 0.2483(2) 0.25173(18) 0.01802(19) 0.0305(7) Uani 1 1 d U . .
C23 C 0.9697(2) 0.0344(2) 0.3220(2) 0.0409(8) Uani 1 1 d U . .
H23A H 0.9188 0.0600 0.3536 0.061 Uiso 1 1 calc R . .
H23B H 1.0180 0.0754 0.2767 0.061 Uiso 1 1 calc R . .
H23C H 0.9995 -0.0048 0.3584 0.061 Uiso 1 1 calc R . .
C24 C 0.2729(2) 0.59769(17) 0.03084(17) 0.0230(6) Uani 1 1 d U . .
C25 C 0.7373(3) -0.0202(2) 0.7110(2) 0.0458(9) Uani 1 1 d U . .
H25A H 0.7109 -0.0698 0.7598 0.069 Uiso 1 1 calc R . .
H25B H 0.8064 -0.0153 0.6963 0.069 Uiso 1 1 calc R . .
H25C H 0.7251 -0.0219 0.6647 0.069 Uiso 1 1 calc R . .
C26 C 0.6250(2) -0.10216(17) 0.54584(17) 0.0245(6) Uani 1 1 d U . .
H26 H 0.5843 -0.1481 0.5854 0.029 Uiso 1 1 calc R . .
C27 C 0.7029(2) -0.11370(17) 0.47854(17) 0.0244(6) Uani 1 1 d U . .
C28 C 0.3666(2) -0.05335(19) 0.77409(19) 0.0322(7) Uani 1 1 d U . .
H28 H 0.3125 -0.0572 0.8223 0.039 Uiso 1 1 calc R . .
C29 C 0.5038(3) -0.2129(2) 0.8676(2) 0.0476(9) Uani 1 1 d U . .
H29A H 0.5138 -0.2478 0.8375 0.071 Uiso 1 1 calc R . .
H29B H 0.4883 -0.2459 0.9265 0.071 Uiso 1 1 calc R . .
H29C H 0.5622 -0.1797 0.8460 0.071 Uiso 1 1 calc R . .
C2A C 0.6889(2) 0.0532(2) 0.7302(2) 0.0368(7) Uani 1 1 d U . .
C2B C 0.1176(2) 0.63081(18) 0.14603(18) 0.0275(6) Uani 1 1 d U . .
H2BA H 0.0634 0.6424 0.1858 0.033 Uiso 1 1 calc R . .
C2C C 0.7105(2) -0.19174(17) 0.47966(17) 0.0245(6) Uani 1 1 d U . .
H2C H 0.6629 -0.2317 0.5220 0.029 Uiso 1 1 calc R . .
C2D C 0.7574(2) 0.1980(2) 0.6606(2) 0.0360(7) Uani 1 1 d U . .
H2D H 0.7541 0.1918 0.7136 0.043 Uiso 1 1 calc R . .
C2E C 0.2536(2) 0.67770(17) 0.02375(18) 0.0275(6) Uani 1 1 d U . .
H2EA H 0.2956 0.7201 -0.0216 0.033 Uiso 1 1 calc R . .
C2F C 0.7923(3) -0.29978(19) 0.4281(2) 0.0372(8) Uani 1 1 d U . .
C2G C 0.1764(2) 0.69595(17) 0.08010(17) 0.0269(6) Uani 1 1 d U . .
C2H C 0.2327(2) 0.24182(17) 0.10088(18) 0.0287(7) Uani 1 1 d U . .
H2H H 0.2079 0.1905 0.1429 0.034 Uiso 1 1 calc R . .
C2I C 0.7990(2) 0.2796(2) 0.5189(2) 0.0355(7) Uani 1 1 d U . .
H2I H 0.8238 0.3288 0.4730 0.043 Uiso 1 1 calc R . .
C2J C 0.2570(2) 0.26279(19) -0.13231(19) 0.0316(7) Uani 1 1 d U . .
H2J H 0.2585 0.2666 -0.1840 0.038 Uiso 1 1 calc R . .
C2K C 0.1324(2) 0.55011(17) 0.15782(18) 0.0261(6) Uani 1 1 d U . .
C2L C 0.2265(2) 0.18382(19) 0.00892(19) 0.0339(7) Uani 1 1 d U . .
H2L H 0.2075 0.1344 0.0556 0.041 Uiso 1 1 calc R . .
C2M C 0.7524(2) 0.2411(2) 0.18906(19) 0.0349(7) Uani 1 1 d U . .
H2M H 0.7076 0.2387 0.1661 0.042 Uiso 1 1 calc R . .
C2N C 0.7709(2) 0.21639(19) 0.50668(19) 0.0310(7) Uani 1 1 d U . .
C2O C 0.3537(2) 0.58813(16) -0.03580(17) 0.0236(6) Uani 1 1 d U . .
H2O H 0.3893 0.6360 -0.0773 0.028 Uiso 1 1 calc R . .
C2P C 0.7834(2) -0.21263(18) 0.42247(18) 0.0276(6) Uani 1 1 d U . .
C2Q C 0.1696(2) 0.21298(19) 0.38384(19) 0.0348(7) Uani 1 1 d U . .
H2Q H 0.1534 0.1928 0.4419 0.042 Uiso 1 1 calc R . .
C2R C 0.8524(2) -0.15093(18) 0.36217(18) 0.0292(7) Uani 1 1 d U . .
H2R H 0.9050 -0.1643 0.3226 0.035 Uiso 1 1 calc R . .
C2S C 0.2958(3) 0.0536(2) -0.0635(3) 0.0591(11) Uani 1 1 d U . .
H2SA H 0.3578 0.0812 -0.1025 0.089 Uiso 1 1 calc R . .
H2SB H 0.2883 0.0059 -0.0728 0.089 Uiso 1 1 calc R . .
H2SC H 0.2927 0.0375 -0.0069 0.089 Uiso 1 1 calc R . .
C2T C 0.1567(2) 0.78369(18) 0.07039(19) 0.0342(7) Uani 1 1 d U . .
C2U C 0.1502(3) 0.83228(19) -0.0140(2) 0.0414(8) Uani 1 1 d U . .
H2UA H 0.2095 0.8282 -0.0575 0.062 Uiso 1 1 calc R . .
H2UB H 0.1410 0.8888 -0.0213 0.062 Uiso 1 1 calc R . .
H2UC H 0.0961 0.8111 -0.0174 0.062 Uiso 1 1 calc R . .
C2V C 0.2151(3) 0.1109(2) -0.0766(2) 0.0411(8) Uani 1 1 d U . .
C2W C 0.9275(2) -0.00841(19) 0.28662(19) 0.0313(7) Uani 1 1 d U . .
C2X C 0.2321(2) 0.18745(19) -0.0665(2) 0.0334(7) Uani 1 1 d U . .
C2Y C 0.7278(2) 0.13198(19) 0.65371(19) 0.0311(7) Uani 1 1 d U . .
C2Z C 0.7915(2) 0.2724(2) 0.5955(2) 0.0376(8) Uani 1 1 d U A .
C30 C 0.3066(3) 0.4118(2) -0.2036(2) 0.0375(8) Uani 1 1 d U . .
C31 C 0.8848(2) 0.0526(2) 0.22663(19) 0.0362(7) Uani 1 1 d U . .
H31A H 0.8613 0.0251 0.2018 0.054 Uiso 1 1 calc R . .
H31B H 0.9340 0.0937 0.1831 0.054 Uiso 1 1 calc R . .
H31C H 0.8316 0.0780 0.2566 0.054 Uiso 1 1 calc R . .
C32 C 0.2407(3) 0.8194(2) 0.0756(3) 0.0515(10) Uani 1 1 d U . .
H32A H 0.2491 0.7857 0.1276 0.077 Uiso 1 1 calc R . .
H32B H 0.2267 0.8740 0.0737 0.077 Uiso 1 1 calc R . .
H32C H 0.2994 0.8210 0.0290 0.077 Uiso 1 1 calc R . .
C33 C -0.0220(3) 0.5171(2) 0.2848(2) 0.0477(9) Uani 1 1 d U . .
H33A H -0.0639 0.4726 0.3319 0.072 Uiso 1 1 calc R . .
H33B H -0.0575 0.5499 0.2503 0.072 Uiso 1 1 calc R . .
H33C H 0.0005 0.5503 0.3048 0.072 Uiso 1 1 calc R . .
C34 C 0.7074(3) 0.0514(2) 0.8048(2) 0.0499(10) Uani 1 1 d U . .
H34A H 0.6748 0.0955 0.8204 0.075 Uiso 1 1 calc R . .
H34B H 0.7762 0.0577 0.7902 0.075 Uiso 1 1 calc R . .
H34C H 0.6828 0.0000 0.8513 0.075 Uiso 1 1 calc R . .
C35 C 0.0246(2) 0.4310(2) 0.2048(2) 0.0456(9) Uani 1 1 d U . .
H35A H 0.0774 0.4052 0.1750 0.068 Uiso 1 1 calc R . .
H35B H -0.0079 0.4649 0.1681 0.068 Uiso 1 1 calc R . .
H35C H -0.0209 0.3897 0.2529 0.068 Uiso 1 1 calc R . .
C36 C 1.0102(3) -0.0462(2) 0.2371(2) 0.0490(10) Uani 1 1 d U . .
H36A H 1.0372 -0.0875 0.2745 0.074 Uiso 1 1 calc R . .
H36B H 1.0598 -0.0045 0.1953 0.074 Uiso 1 1 calc R . .
H36C H 0.9866 -0.0707 0.2099 0.074 Uiso 1 1 calc R . .
C37 C 0.2500(3) 0.4808(2) -0.1844(2) 0.0480(9) Uani 1 1 d U . .
H37A H 0.1816 0.4693 -0.1673 0.072 Uiso 1 1 calc R . .
H37B H 0.2703 0.5307 -0.2338 0.072 Uiso 1 1 calc R . .
H37C H 0.2616 0.4867 -0.1397 0.072 Uiso 1 1 calc R . .
C38 C 0.2869(3) 0.4071(2) -0.2754(2) 0.0509(10) Uani 1 1 d U . .
H38A H 0.3251 0.3655 -0.2920 0.076 Uiso 1 1 calc R . .
H38B H 0.3042 0.4591 -0.3223 0.076 Uiso 1 1 calc R . .
H38C H 0.2188 0.3938 -0.2574 0.076 Uiso 1 1 calc R . .
C39 C -0.0060(3) 0.1225(3) 0.4835(2) 0.0543(10) Uani 1 1 d U . .
H39A H 0.0416 0.0826 0.4944 0.081 Uiso 1 1 calc R . .
H39B H -0.0692 0.0953 0.5085 0.081 Uiso 1 1 calc R . .
H39C H -0.0071 0.1615 0.5074 0.081 Uiso 1 1 calc R . .
C3A C 0.1191(3) 0.0695(2) -0.0122(3) 0.0599(11) Uani 1 1 d U . .
H3AA H 0.1089 0.0208 -0.0189 0.090 Uiso 1 1 calc R . .
H3AB H 0.0677 0.1061 -0.0198 0.090 Uiso 1 1 calc R . .
H3AC H 0.1189 0.0550 0.0433 0.090 Uiso 1 1 calc R . .
C3B C 0.0634(3) 0.7914(2) 0.1360(2) 0.0507(10) Uani 1 1 d U . .
H3BA H 0.0107 0.7659 0.1349 0.076 Uiso 1 1 calc R . .
H3BB H 0.0516 0.8484 0.1248 0.076 Uiso 1 1 calc R . .
H3BC H 0.0679 0.7648 0.1905 0.076 Uiso 1 1 calc R . .
C3C C 0.8161(3) 0.3432(3) 0.6102(2) 0.0575(10) Uani 1 1 d DU . .
C3D C 0.8629(3) -0.3059(2) 0.3479(2) 0.0536(10) Uani 1 1 d U . .
H3DA H 0.8430 -0.2719 0.3020 0.080 Uiso 1 1 calc R . .
H3DB H 0.8639 -0.3618 0.3532 0.080 Uiso 1 1 calc R . .
H3DC H 0.9270 -0.2878 0.3370 0.080 Uiso 1 1 calc R . .
C3E C 0.2157(3) 0.1290(2) -0.1625(2) 0.0530(10) Uani 1 1 d U . .
H3EA H 0.2784 0.1528 -0.2043 0.080 Uiso 1 1 calc R . .
H3EB H 0.1661 0.1667 -0.1725 0.080 Uiso 1 1 calc R . .
H3EC H 0.2032 0.0790 -0.1657 0.080 Uiso 1 1 calc R . .
C3F C 0.6960(3) -0.3369(3) 0.4476(3) 0.0666(12) Uani 1 1 d U . .
H3FA H 0.6519 -0.3407 0.5026 0.100 Uiso 1 1 calc R . .
H3FB H 0.7049 -0.3907 0.4465 0.100 Uiso 1 1 calc R . .
H3FC H 0.6693 -0.3029 0.4063 0.100 Uiso 1 1 calc R . .
C2 C 0.8270(4) -0.3487(2) 0.4991(2) 0.0640(12) Uani 1 1 d U . .
H2A H 0.8907 -0.3279 0.4860 0.096 Uiso 1 1 calc R . .
H2B H 0.8301 -0.4053 0.5064 0.096 Uiso 1 1 calc R . .
H2E H 0.7824 -0.3439 0.5503 0.096 Uiso 1 1 calc R . .
C5 C 1.0260(3) 0.3557(3) 0.0394(2) 0.0603(11) Uani 1 1 d U . .
H5A H 1.0216 0.3211 0.0124 0.091 Uiso 1 1 calc R . .
H5B H 1.0918 0.3776 0.0161 0.091 Uiso 1 1 calc R . .
H5C H 0.9827 0.4000 0.0302 0.091 Uiso 1 1 calc R . .
C6 C 0.8677(7) 0.4109(6) 0.5320(6) 0.064(2) Uani 0.605(7) 1 d PDU A 1
H6A H 0.9290 0.3931 0.5024 0.096 Uiso 0.605(7) 1 calc PR A 1
H6B H 0.8791 0.4555 0.5443 0.096 Uiso 0.605(7) 1 calc PR A 1
H6C H 0.8291 0.4289 0.4974 0.096 Uiso 0.605(7) 1 calc PR A 1
C7 C 0.8884(6) 0.3088(5) 0.6582(5) 0.069(2) Uani 0.605(7) 1 d PDU A 1
H7A H 0.8586 0.2610 0.7082 0.104 Uiso 0.605(7) 1 calc PR A 1
H7B H 0.9032 0.3500 0.6735 0.104 Uiso 0.605(7) 1 calc PR A 1
H7C H 0.9475 0.2943 0.6222 0.104 Uiso 0.605(7) 1 calc PR A 1
C8 C 0.7298(7) 0.3643(6) 0.6671(6) 0.087(2) Uani 0.605(7) 1 d PDU A 1
H8A H 0.6839 0.3867 0.6398 0.131 Uiso 0.605(7) 1 calc PR A 1
H8B H 0.7470 0.4044 0.6825 0.131 Uiso 0.605(7) 1 calc PR A 1
H8C H 0.7009 0.3161 0.7167 0.131 Uiso 0.605(7) 1 calc PR A 1
C8A C 0.7296(9) 0.4064(8) 0.6005(10) 0.082(3) Uani 0.395(7) 1 d PDU A 2
H8AA H 0.7392 0.4345 0.5419 0.123 Uiso 0.395(7) 1 calc PR A 2
H8AB H 0.7306 0.4457 0.6234 0.123 Uiso 0.395(7) 1 calc PR A 2
H8AC H 0.6677 0.3765 0.6304 0.123 Uiso 0.395(7) 1 calc PR A 2
C7A C 0.8144(12) 0.3280(8) 0.6938(7) 0.081(3) Uani 0.395(7) 1 d PDU A 2
H7AA H 0.7486 0.3144 0.7341 0.122 Uiso 0.395(7) 1 calc PR A 2
H7AB H 0.8384 0.3763 0.6927 0.122 Uiso 0.395(7) 1 calc PR A 2
H7AC H 0.8549 0.2832 0.7095 0.122 Uiso 0.395(7) 1 calc PR A 2
C6A C 0.9004(10) 0.3961(11) 0.5406(10) 0.064(3) Uani 0.395(7) 1 d PDU A 2
H6AA H 0.9564 0.3635 0.5306 0.095 Uiso 0.395(7) 1 calc PR A 2
H6AB H 0.9138 0.4380 0.5556 0.095 Uiso 0.395(7) 1 calc PR A 2
H6AC H 0.8856 0.4210 0.4905 0.095 Uiso 0.395(7) 1 calc PR A 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
V1 O1 1.597(2) . ?
V1 O3 1.905(2) . ?
V1 O2 1.905(2) . ?
V1 N1 2.118(3) . ?
V1 N2 2.126(3) . ?
V2 O6 1.598(2) . ?
V2 O7 1.903(2) . ?
V2 O8 1.911(2) . ?
V2 N4 2.117(3) . ?
V2 N3 2.120(3) . ?
C3 O5 1.369(4) . ?
C3 C2Q 1.388(5) . ?
C3 C1O 1.400(4) . ?
C4 O10 1.374(4) . ?
C4 C21 1.385(5) . ?
C4 C1Z 1.393(4) . ?
O2 C1V 1.324(3) . ?
N2 C2H 1.298(4) . ?
N2 C1B 1.444(4) . ?
O7 C1N 1.323(3) . ?
N3 C26 1.297(4) . ?
N3 C1C 1.447(4) . ?
N4 C1W 1.286(4) . ?
N4 C1F 1.450(4) . ?
C10 O9 1.375(4) . ?
C10 C28 1.391(4) . ?
C10 C1D 1.399(4) . ?
N1 C2O 1.301(4) . ?
N1 C1 1.435(4) . ?
O8 C1S 1.324(3) . ?
O4 C16 1.378(4) . ?
O4 C1Y 1.410(4) . ?
C16 C1J 1.386(4) . ?
C16 C18 1.394(4) . ?
O9 C29 1.422(4) . ?
C19 C2J 1.386(4) . ?
C19 C1T 1.424(4) . ?
C19 C30 1.536(4) . ?
O3 C1T 1.328(3) . ?
C1 C1G 1.390(4) . ?
C1 C1J 1.395(4) . ?
O5 C39 1.421(4) . ?
C1A C1L 1.387(4) . ?
C1A C1B 1.396(4) . ?
C1A H1A 0.9500 . ?
C1B C1O 1.384(4) . ?
C1C C1D 1.379(4) . ?
C1C C1E 1.385(4) . ?
C1D H1D 0.9500 . ?
C1E C1X 1.385(4) . ?
C1E H1E 0.9500 . ?
C1F C1Z 1.380(4) . ?
C1F C1K 1.390(4) . ?
C1G C1U 1.392(4) . ?
C1G H1G 0.9500 . ?
C1H C2A 1.528(5) . ?
C1H H1HA 0.9800 . ?
C1H H1HB 0.9800 . ?
C1H H1HC 0.9800 . ?
O10 C5 1.418(4) . ?
C1J H1J 0.9500 . ?
C1K C2M 1.392(4) . ?
C1K H1K 0.9500 . ?
C1L C2Q 1.385(4) . ?
C1L H1L 0.9500 . ?
C1M C30 1.541(5) . ?
C1M H1MA 0.9800 . ?
C1M H1MB 0.9800 . ?
C1M H1MC 0.9800 . ?
C1N C27 1.409(4) . ?
C1N C1Q 1.430(4) . ?
C1O H1O 0.9500 . ?
C1P C1R 1.514(5) . ?
C1P H1PA 0.9800 . ?
C1P H1PB 0.9800 . ?
C1P H1PC 0.9800 . ?
C1Q C2R 1.385(4) . ?
C1Q C2W 1.544(4) . ?
C1R C33 1.534(4) . ?
C1R C35 1.534(5) . ?
C1R C2K 1.540(4) . ?
C18 C1U 1.381(4) . ?
C18 H18 0.9500 . ?
C1S C2Y 1.422(4) . ?
C1S C2N 1.427(4) . ?
C1T C22 1.416(4) . ?
C1U H1U 0.9500 . ?
C1V C24 1.406(4) . ?
C1V C2K 1.427(4) . ?
C1W C2N 1.444(4) . ?
C1W H1W 0.9500 . ?
C1X C28 1.378(4) . ?
C1X H1X 0.9500 . ?
C1Y H1YA 0.9800 . ?
C1Y H1YB 0.9800 . ?
C1Y H1YC 0.9800 . ?
C1Z H1Z 0.9500 . ?
C21 C2M 1.380(5) . ?
C21 H21 0.9500 . ?
C22 C2L 1.405(4) . ?
C22 C2H 1.439(4) . ?
C23 C2W 1.530(5) . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 C2E 1.412(4) . ?
C24 C2O 1.440(4) . ?
C25 C2A 1.554(5) . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 C27 1.441(4) . ?
C26 H26 0.9500 . ?
C27 C2C 1.402(4) . ?
C28 H28 0.9500 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C2A C34 1.537(5) . ?
C2A C2Y 1.543(4) . ?
C2B C2K 1.397(4) . ?
C2B C2G 1.402(4) . ?
C2B H2BA 0.9500 . ?
C2C C2P 1.364(4) . ?
C2C H2C 0.9500 . ?
C2D C2Y 1.399(4) . ?
C2D C2Z 1.399(5) . ?
C2D H2D 0.9500 . ?
C2E C2G 1.364(4) . ?
C2E H2EA 0.9500 . ?
C2F C3F 1.529(5) . ?
C2F C3D 1.530(4) . ?
C2F C2P 1.538(4) . ?
C2F C2 1.539(5) . ?
C2G C2T 1.538(4) . ?
C2H H2H 0.9500 . ?
C2I C2Z 1.369(4) . ?
C2I C2N 1.401(4) . ?
C2I H2I 0.9500 . ?
C2J C2X 1.402(4) . ?
C2J H2J 0.9500 . ?
C2L C2X 1.379(4) . ?
C2L H2L 0.9500 . ?
C2M H2M 0.9500 . ?
C2O H2O 0.9500 . ?
C2P C2R 1.410(4) . ?
C2Q H2Q 0.9500 . ?
C2R H2R 0.9500 . ?
C2S C2V 1.542(5) . ?
C2S H2SA 0.9800 . ?
C2S H2SB 0.9800 . ?
C2S H2SC 0.9800 . ?
C2T C3B 1.522(5) . ?
C2T C2U 1.527(4) . ?
C2T C32 1.547(5) . ?
C2U H2UA 0.9800 . ?
C2U H2UB 0.9800 . ?
C2U H2UC 0.9800 . ?
C2V C3A 1.526(5) . ?
C2V C3E 1.529(5) . ?
C2V C2X 1.542(4) . ?
C2W C31 1.529(5) . ?
C2W C36 1.532(4) . ?
C2Z C3C 1.535(5) . ?
C30 C37 1.523(5) . ?
C30 C38 1.542(5) . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?
C39 H39A 0.9800 . ?
C39 H39B 0.9800 . ?
C39 H39C 0.9800 . ?
C3A H3AA 0.9800 . ?
C3A H3AB 0.9800 . ?
C3A H3AC 0.9800 . ?
C3B H3BA 0.9800 . ?
C3B H3BB 0.9800 . ?
C3B H3BC 0.9800 . ?
C3C C8 1.470(8) . ?
C3C C6 1.484(9) . ?
C3C C7A 1.492(11) . ?
C3C C6A 1.507(13) . ?
C3C C7 1.607(8) . ?
C3C C8A 1.656(12) . ?
C3D H3DA 0.9800 . ?
C3D H3DB 0.9800 . ?
C3D H3DC 0.9800 . ?
C3E H3EA 0.9800 . ?
C3E H3EB 0.9800 . ?
C3E H3EC 0.9800 . ?
C3F H3FA 0.9800 . ?
C3F H3FB 0.9800 . ?
C3F H3FC 0.9800 . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2E 0.9800 . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C8A H8AA 0.9800 . ?
C8A H8AB 0.9800 . ?
C8A H8AC 0.9800 . ?
C7A H7AA 0.9800 . ?
C7A H7AB 0.9800 . ?
C7A H7AC 0.9800 . ?
C6A H6AA 0.9800 . ?
C6A H6AB 0.9800 . ?
C6A H6AC 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 V1 O3 118.77(11) . . ?
O1 V1 O2 119.60(10) . . ?
O3 V1 O2 121.64(10) . . ?
O1 V1 N1 95.17(10) . . ?
O3 V1 N1 87.50(9) . . ?
O2 V1 N1 87.66(9) . . ?
O1 V1 N2 93.78(10) . . ?
O3 V1 N2 87.02(9) . . ?
O2 V1 N2 89.09(9) . . ?
N1 V1 N2 170.94(9) . . ?
O6 V2 O7 120.55(10) . . ?
O6 V2 O8 118.12(11) . . ?
O7 V2 O8 121.32(10) . . ?
O6 V2 N4 93.53(11) . . ?
O7 V2 N4 88.19(9) . . ?
O8 V2 N4 87.65(9) . . ?
O6 V2 N3 95.35(10) . . ?
O7 V2 N3 87.31(9) . . ?
O8 V2 N3 88.16(9) . . ?
N4 V2 N3 171.12(10) . . ?
O5 C3 C2Q 125.5(3) . . ?
O5 C3 C1O 114.5(3) . . ?
C2Q C3 C1O 120.1(3) . . ?
O10 C4 C21 125.0(3) . . ?
O10 C4 C1Z 114.8(3) . . ?
C21 C4 C1Z 120.2(3) . . ?
C1V O2 V1 135.78(18) . . ?
C2H N2 C1B 115.2(2) . . ?
C2H N2 V1 123.3(2) . . ?
C1B N2 V1 121.03(18) . . ?
C1N O7 V2 135.97(18) . . ?
C26 N3 C1C 115.8(2) . . ?
C26 N3 V2 124.36(19) . . ?
C1C N3 V2 119.81(18) . . ?
C1W N4 C1F 115.5(3) . . ?
C1W N4 V2 122.9(2) . . ?
C1F N4 V2 120.97(19) . . ?
O9 C10 C28 115.2(3) . . ?
O9 C10 C1D 124.5(3) . . ?
C28 C10 C1D 120.3(3) . . ?
C2O N1 C1 116.0(2) . . ?
C2O N1 V1 123.86(19) . . ?
C1 N1 V1 120.08(18) . . ?
C1S O8 V2 134.96(19) . . ?
C16 O4 C1Y 116.7(2) . . ?
O4 C16 C1J 123.8(3) . . ?
O4 C16 C18 115.4(3) . . ?
C1J C16 C18 120.7(3) . . ?
C10 O9 C29 117.6(2) . . ?
C2J C19 C1T 117.4(3) . . ?
C2J C19 C30 121.2(3) . . ?
C1T C19 C30 121.3(3) . . ?
C1T O3 V1 135.76(19) . . ?
C1G C1 C1J 120.3(3) . . ?
C1G C1 N1 119.8(3) . . ?
C1J C1 N1 119.9(3) . . ?
C3 O5 C39 117.1(3) . . ?
C1L C1A C1B 118.2(3) . . ?
C1L C1A H1A 120.9 . . ?
C1B C1A H1A 120.9 . . ?
C1O C1B C1A 120.6(3) . . ?
C1O C1B N2 119.7(3) . . ?
C1A C1B N2 119.7(3) . . ?
C1D C1C C1E 121.2(3) . . ?
C1D C1C N3 120.1(3) . . ?
C1E C1C N3 118.6(3) . . ?
C1C C1D C10 118.9(3) . . ?
C1C C1D H1D 120.5 . . ?
C10 C1D H1D 120.5 . . ?
C1C C1E C1X 119.1(3) . . ?
C1C C1E H1E 120.5 . . ?
C1X C1E H1E 120.5 . . ?
C1Z C1F C1K 120.4(3) . . ?
C1Z C1F N4 120.2(3) . . ?
C1K C1F N4 119.4(3) . . ?
C1 C1G C1U 119.3(3) . . ?
C1 C1G H1G 120.4 . . ?
C1U C1G H1G 120.4 . . ?
C2A C1H H1HA 109.5 . . ?
C2A C1H H1HB 109.5 . . ?
H1HA C1H H1HB 109.5 . . ?
C2A C1H H1HC 109.5 . . ?
H1HA C1H H1HC 109.5 . . ?
H1HB C1H H1HC 109.5 . . ?
C4 O10 C5 118.1(3) . . ?
C16 C1J C1 119.5(3) . . ?
C16 C1J H1J 120.3 . . ?
C1 C1J H1J 120.3 . . ?
C1F C1K C2M 118.3(3) . . ?
C1F C1K H1K 120.8 . . ?
C2M C1K H1K 120.8 . . ?
C2Q C1L C1A 122.3(3) . . ?
C2Q C1L H1L 118.9 . . ?
C1A C1L H1L 118.9 . . ?
C30 C1M H1MA 109.5 . . ?
C30 C1M H1MB 109.5 . . ?
H1MA C1M H1MB 109.5 . . ?
C30 C1M H1MC 109.5 . . ?
H1MA C1M H1MC 109.5 . . ?
H1MB C1M H1MC 109.5 . . ?
O7 C1N C27 121.3(2) . . ?
O7 C1N C1Q 120.6(3) . . ?
C27 C1N C1Q 118.1(3) . . ?
C1B C1O C3 120.0(3) . . ?
C1B C1O H1O 120.0 . . ?
C3 C1O H1O 120.0 . . ?
C1R C1P H1PA 109.5 . . ?
C1R C1P H1PB 109.5 . . ?
H1PA C1P H1PB 109.5 . . ?
C1R C1P H1PC 109.5 . . ?
H1PA C1P H1PC 109.5 . . ?
H1PB C1P H1PC 109.5 . . ?
C2R C1Q C1N 117.7(3) . . ?
C2R C1Q C2W 121.1(3) . . ?
C1N C1Q C2W 121.2(3) . . ?
C1P C1R C33 107.8(3) . . ?
C1P C1R C35 110.5(3) . . ?
C33 C1R C35 107.1(3) . . ?
C1P C1R C2K 109.8(3) . . ?
C33 C1R C2K 112.0(3) . . ?
C35 C1R C2K 109.5(3) . . ?
C1U C18 C16 119.2(3) . . ?
C1U C18 H18 120.4 . . ?
C16 C18 H18 120.4 . . ?
O8 C1S C2Y 120.8(3) . . ?
O8 C1S C2N 120.8(3) . . ?
C2Y C1S C2N 118.4(3) . . ?
O3 C1T C22 120.6(3) . . ?
O3 C1T C19 121.0(3) . . ?
C22 C1T C19 118.4(3) . . ?
C18 C1U C1G 121.0(3) . . ?
C18 C1U H1U 119.5 . . ?
C1G C1U H1U 119.5 . . ?
O2 C1V C24 121.2(3) . . ?
O2 C1V C2K 120.4(3) . . ?
C24 C1V C2K 118.4(3) . . ?
N4 C1W C2N 128.6(3) . . ?
N4 C1W H1W 115.7 . . ?
C2N C1W H1W 115.7 . . ?
C28 C1X C1E 121.1(3) . . ?
C28 C1X H1X 119.5 . . ?
C1E C1X H1X 119.5 . . ?
O4 C1Y H1YA 109.5 . . ?
O4 C1Y H1YB 109.5 . . ?
H1YA C1Y H1YB 109.5 . . ?
O4 C1Y H1YC 109.5 . . ?
H1YA C1Y H1YC 109.5 . . ?
H1YB C1Y H1YC 109.5 . . ?
C1F C1Z C4 120.2(3) . . ?
C1F C1Z H1Z 119.9 . . ?
C4 C1Z H1Z 119.9 . . ?
C2M C21 C4 118.7(3) . . ?
C2M C21 H21 120.6 . . ?
C4 C21 H21 120.6 . . ?
C2L C22 C1T 120.8(3) . . ?
C2L C22 C2H 116.0(3) . . ?
C1T C22 C2H 123.1(3) . . ?
C2W C23 H23A 109.5 . . ?
C2W C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C2W C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C1V C24 C2E 120.9(3) . . ?
C1V C24 C2O 123.4(3) . . ?
C2E C24 C2O 115.7(3) . . ?
C2A C25 H25A 109.5 . . ?
C2A C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C2A C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
N3 C26 C27 127.4(3) . . ?
N3 C26 H26 116.3 . . ?
C27 C26 H26 116.3 . . ?
C2C C27 C1N 120.6(3) . . ?
C2C C27 C26 116.2(3) . . ?
C1N C27 C26 123.2(3) . . ?
C1X C28 C10 119.4(3) . . ?
C1X C28 H28 120.3 . . ?
C10 C28 H28 120.3 . . ?
O9 C29 H29A 109.5 . . ?
O9 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
O9 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C1H C2A C34 107.1(3) . . ?
C1H C2A C2Y 109.3(3) . . ?
C34 C2A C2Y 112.4(3) . . ?
C1H C2A C25 110.0(3) . . ?
C34 C2A C25 107.4(3) . . ?
C2Y C2A C25 110.5(3) . . ?
C2K C2B C2G 125.1(3) . . ?
C2K C2B H2BA 117.5 . . ?
C2G C2B H2BA 117.5 . . ?
C2P C2C C27 122.7(3) . . ?
C2P C2C H2C 118.6 . . ?
C27 C2C H2C 118.6 . . ?
C2Y C2D C2Z 124.9(3) . . ?
C2Y C2D H2D 117.5 . . ?
C2Z C2D H2D 117.5 . . ?
C2G C2E C24 122.0(3) . . ?
C2G C2E H2EA 119.0 . . ?
C24 C2E H2EA 119.0 . . ?
C3F C2F C3D 107.8(3) . . ?
C3F C2F C2P 111.5(3) . . ?
C3D C2F C2P 112.2(3) . . ?
C3F C2F C2 108.3(3) . . ?
C3D C2F C2 109.6(3) . . ?
C2P C2F C2 107.4(3) . . ?
C2E C2G C2B 116.3(3) . . ?
C2E C2G C2T 120.9(3) . . ?
C2B C2G C2T 122.8(3) . . ?
N2 C2H C22 127.8(3) . . ?
N2 C2H H2H 116.1 . . ?
C22 C2H H2H 116.1 . . ?
C2Z C2I C2N 121.6(3) . . ?
C2Z C2I H2I 119.2 . . ?
C2N C2I H2I 119.2 . . ?
C19 C2J C2X 125.1(3) . . ?
C19 C2J H2J 117.5 . . ?
C2X C2J H2J 117.5 . . ?
C2B C2K C1V 117.3(3) . . ?
C2B C2K C1R 120.7(3) . . ?
C1V C2K C1R 122.0(3) . . ?
C2X C2L C22 121.3(3) . . ?
C2X C2L H2L 119.3 . . ?
C22 C2L H2L 119.3 . . ?
C21 C2M C1K 122.0(3) . . ?
C21 C2M H2M 119.0 . . ?
C1K C2M H2M 119.0 . . ?
C2I C2N C1S 120.6(3) . . ?
C2I C2N C1W 116.8(3) . . ?
C1S C2N C1W 122.6(3) . . ?
N1 C2O C24 127.8(3) . . ?
N1 C2O H2O 116.1 . . ?
C24 C2O H2O 116.1 . . ?
C2C C2P C2R 115.8(3) . . ?
C2C C2P C2F 121.4(3) . . ?
C2R C2P C2F 122.7(3) . . ?
C1L C2Q C3 118.8(3) . . ?
C1L C2Q H2Q 120.6 . . ?
C3 C2Q H2Q 120.6 . . ?
C1Q C2R C2P 124.9(3) . . ?
C1Q C2R H2R 117.5 . . ?
C2P C2R H2R 117.5 . . ?
C2V C2S H2SA 109.5 . . ?
C2V C2S H2SB 109.5 . . ?
H2SA C2S H2SB 109.5 . . ?
C2V C2S H2SC 109.5 . . ?
H2SA C2S H2SC 109.5 . . ?
H2SB C2S H2SC 109.5 . . ?
C3B C2T C2U 107.8(3) . . ?
C3B C2T C2G 112.5(3) . . ?
C2U C2T C2G 109.5(3) . . ?
C3B C2T C32 109.4(3) . . ?
C2U C2T C32 108.8(3) . . ?
C2G C2T C32 108.7(3) . . ?
C2T C2U H2UA 109.5 . . ?
C2T C2U H2UB 109.5 . . ?
H2UA C2U H2UB 109.5 . . ?
C2T C2U H2UC 109.5 . . ?
H2UA C2U H2UC 109.5 . . ?
H2UB C2U H2UC 109.5 . . ?
C3A C2V C3E 108.6(3) . . ?
C3A C2V C2S 109.3(3) . . ?
C3E C2V C2S 108.4(3) . . ?
C3A C2V C2X 110.0(3) . . ?
C3E C2V C2X 112.3(3) . . ?
C2S C2V C2X 108.2(3) . . ?
C31 C2W C23 110.1(3) . . ?
C31 C2W C36 107.6(3) . . ?
C23 C2W C36 107.1(3) . . ?
C31 C2W C1Q 109.5(3) . . ?
C23 C2W C1Q 110.9(3) . . ?
C36 C2W C1Q 111.6(3) . . ?
C2L C2X C2J 116.6(3) . . ?
C2L C2X C2V 120.5(3) . . ?
C2J C2X C2V 122.9(3) . . ?
C2D C2Y C1S 117.0(3) . . ?
C2D C2Y C2A 120.7(3) . . ?
C1S C2Y C2A 122.2(3) . . ?
C2I C2Z C2D 117.0(3) . . ?
C2I C2Z C3C 121.8(3) . . ?
C2D C2Z C3C 121.2(3) . . ?
C37 C30 C19 111.9(3) . . ?
C37 C30 C1M 110.4(3) . . ?
C19 C30 C1M 108.8(3) . . ?
C37 C30 C38 106.7(3) . . ?
C19 C30 C38 111.7(3) . . ?
C1M C30 C38 107.1(3) . . ?
C2W C31 H31A 109.5 . . ?
C2W C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C2W C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C2T C32 H32A 109.5 . . ?
C2T C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C2T C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C1R C33 H33A 109.5 . . ?
C1R C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
C1R C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C2A C34 H34A 109.5 . . ?
C2A C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
C2A C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C1R C35 H35A 109.5 . . ?
C1R C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
C1R C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C2W C36 H36A 109.5 . . ?
C2W C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C2W C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C30 C37 H37A 109.5 . . ?
C30 C37 H37B 109.5 . . ?
H37A C37 H37B 109.5 . . ?
C30 C37 H37C 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
C30 C38 H38A 109.5 . . ?
C30 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
C30 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
O5 C39 H39A 109.5 . . ?
O5 C39 H39B 109.5 . . ?
H39A C39 H39B 109.5 . . ?
O5 C39 H39C 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
C2V C3A H3AA 109.5 . . ?
C2V C3A H3AB 109.5 . . ?
H3AA C3A H3AB 109.5 . . ?
C2V C3A H3AC 109.5 . . ?
H3AA C3A H3AC 109.5 . . ?
H3AB C3A H3AC 109.5 . . ?
C2T C3B H3BA 109.5 . . ?
C2T C3B H3BB 109.5 . . ?
H3BA C3B H3BB 109.5 . . ?
C2T C3B H3BC 109.5 . . ?
H3BA C3B H3BC 109.5 . . ?
H3BB C3B H3BC 109.5 . . ?
C8 C3C C6 115.4(7) . . ?
C8 C3C C7A 62.7(7) . . ?
C6 C3C C7A 126.4(7) . . ?
C8 C3C C6A 129.7(9) . . ?
C7A C3C C6A 113.4(9) . . ?
C8 C3C C2Z 109.4(4) . . ?
C6 C3C C2Z 112.5(6) . . ?
C7A C3C C2Z 118.1(6) . . ?
C6A C3C C2Z 114.1(8) . . ?
C8 C3C C7 106.7(6) . . ?
C6 C3C C7 107.0(6) . . ?
C6A C3C C7 85.3(7) . . ?
C2Z C3C C7 105.2(4) . . ?
C6 C3C C8A 78.3(7) . . ?
C7A C3C C8A 103.7(8) . . ?
C6A C3C C8A 99.4(9) . . ?
C2Z C3C C8A 105.1(5) . . ?
C7 C3C C8A 144.1(6) . . ?
C2F C3D H3DA 109.5 . . ?
C2F C3D H3DB 109.5 . . ?
H3DA C3D H3DB 109.5 . . ?
C2F C3D H3DC 109.5 . . ?
H3DA C3D H3DC 109.5 . . ?
H3DB C3D H3DC 109.5 . . ?
C2V C3E H3EA 109.5 . . ?
C2V C3E H3EB 109.5 . . ?
H3EA C3E H3EB 109.5 . . ?
C2V C3E H3EC 109.5 . . ?
H3EA C3E H3EC 109.5 . . ?
H3EB C3E H3EC 109.5 . . ?
C2F C3F H3FA 109.5 . . ?
C2F C3F H3FB 109.5 . . ?
H3FA C3F H3FB 109.5 . . ?
C2F C3F H3FC 109.5 . . ?
H3FA C3F H3FC 109.5 . . ?
H3FB C3F H3FC 109.5 . . ?
C2F C2 H2A 109.5 . . ?
C2F C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
C2F C2 H2E 109.5 . . ?
H2A C2 H2E 109.5 . . ?
H2B C2 H2E 109.5 . . ?
O10 C5 H5A 109.5 . . ?
O10 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
O10 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C3C C6 H6A 109.5 . . ?
C3C C6 H6B 109.5 . . ?
C3C C6 H6C 109.5 . . ?
C3C C7 H7A 109.5 . . ?
C3C C7 H7B 109.5 . . ?
C3C C7 H7C 109.5 . . ?
C3C C8 H8A 109.5 . . ?
C3C C8 H8B 109.5 . . ?
C3C C8 H8C 109.5 . . ?
C3C C8A H8AA 109.5 . . ?
C3C C8A H8AB 109.5 . . ?
H8AA C8A H8AB 109.5 . . ?
C3C C8A H8AC 109.5 . . ?
H8AA C8A H8AC 109.5 . . ?
H8AB C8A H8AC 109.5 . . ?
C3C C7A H7AA 109.5 . . ?
C3C C7A H7AB 109.5 . . ?
H7AA C7A H7AB 109.5 . . ?
C3C C7A H7AC 109.5 . . ?
H7AA C7A H7AC 109.5 . . ?
H7AB C7A H7AC 109.5 . . ?
C3C C6A H6AA 109.5 . . ?
C3C C6A H6AB 109.5 . . ?
H6AA C6A H6AB 109.5 . . ?
C3C C6A H6AC 109.5 . . ?
H6AA C6A H6AC 109.5 . . ?
H6AB C6A H6AC 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O1 V1 O2 C1V 94.5(3) . . . . ?
O3 V1 O2 C1V -85.7(3) . . . . ?
N1 V1 O2 C1V -0.1(3) . . . . ?
N2 V1 O2 C1V -171.7(3) . . . . ?
O1 V1 N2 C2H -103.2(2) . . . . ?
O3 V1 N2 C2H 15.4(2) . . . . ?
O2 V1 N2 C2H 137.2(2) . . . . ?
O1 V1 N2 C1B 68.8(2) . . . . ?
O3 V1 N2 C1B -172.5(2) . . . . ?
O2 V1 N2 C1B -50.8(2) . . . . ?
O6 V2 O7 C1N -93.0(3) . . . . ?
O8 V2 O7 C1N 87.8(3) . . . . ?
N4 V2 O7 C1N 174.0(3) . . . . ?
N3 V2 O7 C1N 1.6(3) . . . . ?
O6 V2 N3 C26 114.5(2) . . . . ?
O7 V2 N3 C26 -5.9(2) . . . . ?
O8 V2 N3 C26 -127.4(2) . . . . ?
O6 V2 N3 C1C -62.0(2) . . . . ?
O7 V2 N3 C1C 177.6(2) . . . . ?
O8 V2 N3 C1C 56.1(2) . . . . ?
O6 V2 N4 C1W 102.4(3) . . . . ?
O7 V2 N4 C1W -137.1(3) . . . . ?
O8 V2 N4 C1W -15.6(3) . . . . ?
O6 V2 N4 C1F -68.0(2) . . . . ?
O7 V2 N4 C1F 52.5(2) . . . . ?
O8 V2 N4 C1F 173.9(2) . . . . ?
O1 V1 N1 C2O -114.8(2) . . . . ?
O3 V1 N1 C2O 126.5(2) . . . . ?
O2 V1 N1 C2O 4.7(2) . . . . ?
O1 V1 N1 C1 62.5(2) . . . . ?
O3 V1 N1 C1 -56.2(2) . . . . ?
O2 V1 N1 C1 -178.0(2) . . . . ?
O6 V2 O8 C1S -78.5(3) . . . . ?
O7 V2 O8 C1S 100.7(3) . . . . ?
N4 V2 O8 C1S 14.2(3) . . . . ?
N3 V2 O8 C1S -173.6(3) . . . . ?
C1Y O4 C16 C1J -2.4(4) . . . . ?
C1Y O4 C16 C18 175.9(3) . . . . ?
C28 C10 O9 C29 -173.0(3) . . . . ?
C1D C10 O9 C29 6.2(5) . . . . ?
O1 V1 O3 C1T 79.0(3) . . . . ?
O2 V1 O3 C1T -100.8(3) . . . . ?
N1 V1 O3 C1T 173.5(3) . . . . ?
N2 V1 O3 C1T -13.7(3) . . . . ?
C2O N1 C1 C1G 134.6(3) . . . . ?
V1 N1 C1 C1G -42.9(3) . . . . ?
C2O N1 C1 C1J -45.3(4) . . . . ?
V1 N1 C1 C1J 137.2(2) . . . . ?
C2Q C3 O5 C39 -10.2(5) . . . . ?
C1O C3 O5 C39 170.0(3) . . . . ?
C1L C1A C1B C1O 2.4(4) . . . . ?
C1L C1A C1B N2 -177.2(3) . . . . ?
C2H N2 C1B C1O -44.6(4) . . . . ?
V1 N2 C1B C1O 142.8(2) . . . . ?
C2H N2 C1B C1A 134.9(3) . . . . ?
V1 N2 C1B C1A -37.7(3) . . . . ?
C26 N3 C1C C1D 49.4(4) . . . . ?
V2 N3 C1C C1D -133.8(2) . . . . ?
C26 N3 C1C C1E -129.3(3) . . . . ?
V2 N3 C1C C1E 47.5(3) . . . . ?
C1E C1C C1D C10 -1.4(4) . . . . ?
N3 C1C C1D C10 179.9(3) . . . . ?
O9 C10 C1D C1C -177.3(3) . . . . ?
C28 C10 C1D C1C 1.9(4) . . . . ?
C1D C1C C1E C1X 0.4(5) . . . . ?
N3 C1C C1E C1X 179.1(3) . . . . ?
C1W N4 C1F C1Z 45.0(4) . . . . ?
V2 N4 C1F C1Z -143.9(2) . . . . ?
C1W N4 C1F C1K -133.6(3) . . . . ?
V2 N4 C1F C1K 37.5(4) . . . . ?
C1J C1 C1G C1U 1.4(4) . . . . ?
N1 C1 C1G C1U -178.5(3) . . . . ?
C21 C4 O10 C5 10.3(5) . . . . ?
C1Z C4 O10 C5 -170.0(3) . . . . ?
O4 C16 C1J C1 177.7(3) . . . . ?
C18 C16 C1J C1 -0.5(4) . . . . ?
C1G C1 C1J C16 -0.3(4) . . . . ?
N1 C1 C1J C16 179.6(3) . . . . ?
C1Z C1F C1K C2M -3.7(5) . . . . ?
N4 C1F C1K C2M 174.8(3) . . . . ?
C1B C1A C1L C2Q -0.9(5) . . . . ?
V2 O7 C1N C27 3.5(4) . . . . ?
V2 O7 C1N C1Q -176.7(2) . . . . ?
C1A C1B C1O C3 -1.4(5) . . . . ?
N2 C1B C1O C3 178.1(3) . . . . ?
O5 C3 C1O C1B 178.8(3) . . . . ?
C2Q C3 C1O C1B -1.0(5) . . . . ?
O7 C1N C1Q C2R -176.8(3) . . . . ?
C27 C1N C1Q C2R 3.0(4) . . . . ?
O7 C1N C1Q C2W 1.5(4) . . . . ?
C27 C1N C1Q C2W -178.7(3) . . . . ?
O4 C16 C18 C1U -178.2(3) . . . . ?
C1J C16 C18 C1U 0.1(5) . . . . ?
V2 O8 C1S C2Y 174.8(2) . . . . ?
V2 O8 C1S C2N -5.9(4) . . . . ?
V1 O3 C1T C22 5.0(5) . . . . ?
V1 O3 C1T C19 -176.8(2) . . . . ?
C2J C19 C1T O3 175.1(3) . . . . ?
C30 C19 C1T O3 -2.5(5) . . . . ?
C2J C19 C1T C22 -6.7(4) . . . . ?
C30 C19 C1T C22 175.7(3) . . . . ?
C16 C18 C1U C1G 1.0(5) . . . . ?
C1 C1G C1U C18 -1.8(5) . . . . ?
V1 O2 C1V C24 -3.7(4) . . . . ?
V1 O2 C1V C2K 176.4(2) . . . . ?
C1F N4 C1W C2N -177.9(3) . . . . ?
V2 N4 C1W C2N 11.2(5) . . . . ?
C1C C1E C1X C28 0.1(5) . . . . ?
C1K C1F C1Z C4 2.3(5) . . . . ?
N4 C1F C1Z C4 -176.2(3) . . . . ?
O10 C4 C1Z C1F -178.1(3) . . . . ?
C21 C4 C1Z C1F 1.6(5) . . . . ?
O10 C4 C21 C2M 175.8(3) . . . . ?
C1Z C4 C21 C2M -3.9(5) . . . . ?
O3 C1T C22 C2L -174.7(3) . . . . ?
C19 C1T C22 C2L 7.1(5) . . . . ?
O3 C1T C22 C2H 7.6(5) . . . . ?
C19 C1T C22 C2H -170.6(3) . . . . ?
O2 C1V C24 C2E -178.4(3) . . . . ?
C2K C1V C24 C2E 1.5(4) . . . . ?
O2 C1V C24 C2O 3.9(4) . . . . ?
C2K C1V C24 C2O -176.3(3) . . . . ?
C1C N3 C26 C27 -177.8(3) . . . . ?
V2 N3 C26 C27 5.6(4) . . . . ?
O7 C1N C27 C2C 176.0(3) . . . . ?
C1Q C1N C27 C2C -3.8(4) . . . . ?
O7 C1N C27 C26 -5.9(4) . . . . ?
C1Q C1N C27 C26 174.3(3) . . . . ?
N3 C26 C27 C2C 179.3(3) . . . . ?
N3 C26 C27 C1N 1.0(5) . . . . ?
C1E C1X C28 C10 0.4(5) . . . . ?
O9 C10 C28 C1X 177.9(3) . . . . ?
C1D C10 C28 C1X -1.4(5) . . . . ?
C1N C27 C2C C2P 1.8(4) . . . . ?
C26 C27 C2C C2P -176.5(3) . . . . ?
C1V C24 C2E C2G -1.4(5) . . . . ?
C2O C24 C2E C2G 176.5(3) . . . . ?
C24 C2E C2G C2B 0.5(4) . . . . ?
C24 C2E C2G C2T -179.5(3) . . . . ?
C2K C2B C2G C2E 0.2(5) . . . . ?
C2K C2B C2G C2T -179.8(3) . . . . ?
C1B N2 C2H C22 176.6(3) . . . . ?
V1 N2 C2H C22 -10.9(5) . . . . ?
C2L C22 C2H N2 178.9(3) . . . . ?
C1T C22 C2H N2 -3.3(5) . . . . ?
C1T C19 C2J C2X 2.0(5) . . . . ?
C30 C19 C2J C2X 179.6(3) . . . . ?
C2G C2B C2K C1V -0.1(5) . . . . ?
C2G C2B C2K C1R 178.8(3) . . . . ?
O2 C1V C2K C2B 179.1(3) . . . . ?
C24 C1V C2K C2B -0.8(4) . . . . ?
O2 C1V C2K C1R 0.2(4) . . . . ?
C24 C1V C2K C1R -179.6(3) . . . . ?
C1P C1R C2K C2B -114.0(3) . . . . ?
C33 C1R C2K C2B 5.7(4) . . . . ?
C35 C1R C2K C2B 124.4(3) . . . . ?
C1P C1R C2K C1V 64.8(4) . . . . ?
C33 C1R C2K C1V -175.5(3) . . . . ?
C35 C1R C2K C1V -56.8(4) . . . . ?
C1T C22 C2L C2X -2.4(5) . . . . ?
C2H C22 C2L C2X 175.5(3) . . . . ?
C4 C21 C2M C1K 2.4(5) . . . . ?
C1F C1K C2M C21 1.4(5) . . . . ?
C2Z C2I C2N C1S 2.6(5) . . . . ?
C2Z C2I C2N C1W -177.2(3) . . . . ?
O8 C1S C2N C2I 173.6(3) . . . . ?
C2Y C1S C2N C2I -7.1(5) . . . . ?
O8 C1S C2N C1W -6.6(5) . . . . ?
C2Y C1S C2N C1W 172.7(3) . . . . ?
N4 C1W C2N C2I -177.6(3) . . . . ?
N4 C1W C2N C1S 2.6(5) . . . . ?
C1 N1 C2O C24 176.7(3) . . . . ?
V1 N1 C2O C24 -5.9(4) . . . . ?
C1V C24 C2O N1 1.3(5) . . . . ?
C2E C24 C2O N1 -176.6(3) . . . . ?
C27 C2C C2P C2R 1.1(4) . . . . ?
C27 C2C C2P C2F 176.8(3) . . . . ?
C3F C2F C2P C2C 44.9(4) . . . . ?
C3D C2F C2P C2C 165.8(3) . . . . ?
C2 C2F C2P C2C -73.7(4) . . . . ?
C3F C2F C2P C2R -139.7(3) . . . . ?
C3D C2F C2P C2R -18.7(5) . . . . ?
C2 C2F C2P C2R 101.8(4) . . . . ?
C1A C1L C2Q C3 -1.4(5) . . . . ?
O5 C3 C2Q C1L -177.4(3) . . . . ?
C1O C3 C2Q C1L 2.4(5) . . . . ?
C1N C1Q C2R C2P -0.2(5) . . . . ?
C2W C1Q C2R C2P -178.5(3) . . . . ?
C2C C2P C2R C1Q -1.9(5) . . . . ?
C2F C2P C2R C1Q -177.6(3) . . . . ?
C2E C2G C2T C3B 175.7(3) . . . . ?
C2B C2G C2T C3B -4.3(5) . . . . ?
C2E C2G C2T C2U 55.8(4) . . . . ?
C2B C2G C2T C2U -124.2(3) . . . . ?
C2E C2G C2T C32 -62.9(4) . . . . ?
C2B C2G C2T C32 117.1(3) . . . . ?
C2R C1Q C2W C31 110.8(3) . . . . ?
C1N C1Q C2W C31 -67.5(4) . . . . ?
C2R C1Q C2W C23 -127.6(3) . . . . ?
C1N C1Q C2W C23 54.2(4) . . . . ?
C2R C1Q C2W C36 -8.2(4) . . . . ?
C1N C1Q C2W C36 173.5(3) . . . . ?
C22 C2L C2X C2J -2.4(5) . . . . ?
C22 C2L C2X C2V 175.5(3) . . . . ?
C19 C2J C2X C2L 2.6(5) . . . . ?
C19 C2J C2X C2V -175.2(3) . . . . ?
C3A C2V C2X C2L 53.8(5) . . . . ?
C3E C2V C2X C2L 174.9(3) . . . . ?
C2S C2V C2X C2L -65.5(4) . . . . ?
C3A C2V C2X C2J -128.4(4) . . . . ?
C3E C2V C2X C2J -7.4(5) . . . . ?
C2S C2V C2X C2J 112.3(4) . . . . ?
C2Z C2D C2Y C1S -2.3(5) . . . . ?
C2Z C2D C2Y C2A -178.4(3) . . . . ?
O8 C1S C2Y C2D -174.0(3) . . . . ?
C2N C1S C2Y C2D 6.7(4) . . . . ?
O8 C1S C2Y C2A 2.1(5) . . . . ?
C2N C1S C2Y C2A -177.2(3) . . . . ?
C1H C2A C2Y C2D 106.7(3) . . . . ?
C34 C2A C2Y C2D -12.1(4) . . . . ?
C25 C2A C2Y C2D -132.1(3) . . . . ?
C1H C2A C2Y C1S -69.3(4) . . . . ?
C34 C2A C2Y C1S 171.9(3) . . . . ?
C25 C2A C2Y C1S 52.0(4) . . . . ?
C2N C2I C2Z C2D 2.0(5) . . . . ?
C2N C2I C2Z C3C -176.0(3) . . . . ?
C2Y C2D C2Z C2I -2.2(5) . . . . ?
C2Y C2D C2Z C3C 175.8(3) . . . . ?
C2J C19 C30 C37 130.2(3) . . . . ?
C1T C19 C30 C37 -52.4(4) . . . . ?
C2J C19 C30 C1M -107.5(3) . . . . ?
C1T C19 C30 C1M 70.0(4) . . . . ?
C2J C19 C30 C38 10.5(5) . . . . ?
C1T C19 C30 C38 -172.0(3) . . . . ?
C2I C2Z C3C C8 116.7(6) . . . . ?
C2D C2Z C3C C8 -61.2(7) . . . . ?
C2I C2Z C3C C6 -12.9(7) . . . . ?
C2D C2Z C3C C6 169.2(6) . . . . ?
C2I C2Z C3C C7A -174.6(9) . . . . ?
C2D C2Z C3C C7A 7.5(10) . . . . ?
C2I C2Z C3C C6A -37.4(9) . . . . ?
C2D C2Z C3C C6A 144.7(8) . . . . ?
C2I C2Z C3C C7 -129.0(5) . . . . ?
C2D C2Z C3C C7 53.0(5) . . . . ?
C2I C2Z C3C C8A 70.5(7) . . . . ?
C2D C2Z C3C C8A -107.4(7) . . . . ?

_diffrn_measured_fraction_theta_max 0.994
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.994
_refine_diff_density_max         0.353
_refine_diff_density_min         -0.293
_refine_diff_density_rms         0.075
# SQUEEZE RESULTS (APPEND TO CIF)
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
1 0.500 0.552 0.448 527.5 146.9
_platon_squeeze_details          
; ?
;

_database_code_depnum_ccdc_archive 'CCDC 980002'
#######################################################################
#
#                 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_3.2MeCN

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C44 H56 N2 O5 V, 2(C2 H3 N)'
_chemical_formula_sum            'C48 H62 N4 O5 V'
_chemical_formula_weight         825.96

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           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                   10.979(2)
_cell_length_b                   13.256(3)
_cell_length_c                   15.575(3)
_cell_angle_alpha                101.47(3)
_cell_angle_beta                 91.71(3)
_cell_angle_gamma                92.44(3)
_cell_volume                     2217.7(8)
_cell_formula_units_Z            2
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    28054
_cell_measurement_theta_min      1.34
_cell_measurement_theta_max      27.52

_exptl_crystal_description       Plate
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.498
_exptl_crystal_size_mid          0.441
_exptl_crystal_size_min          0.215
_exptl_crystal_density_meas      28054
_exptl_crystal_density_diffrn    1.237
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             882
_exptl_absorpt_coefficient_mu    0.273
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_absorpt_correction_T_min  0.5762
_exptl_absorpt_correction_T_max  1.0000


_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Saturn724+ CCD'
_diffrn_measurement_method       'ω scans at fixed χ = 45°'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         none
_diffrn_standards_interval_count none
_diffrn_standards_interval_time  none
_diffrn_standards_decay_%        none
_diffrn_reflns_number            28054
_diffrn_reflns_av_R_equivalents  0.0576
_diffrn_reflns_av_unetI/netI     0.0578
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         1.34
_diffrn_reflns_theta_max         27.52
_reflns_number_total             10097
_reflns_number_gt                9224
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrystalClear (Rigaku Inc., 2007)'
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2007)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'CAMERON (Watkin et al, 1993)'
_computing_publication_material  'SHELX97 (Sheldrick, 1997)'


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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1179P)²+2.3724P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         10097
_refine_ls_number_parameters     539
_refine_ls_number_restraints     0
_refine_ls_R_factor_ref          0.0750
_refine_ls_R_factor_gt           0.0642
_refine_ls_wR_factor_ref         0.2105
_refine_ls_wR_factor_gt          0.1839
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_restrained_S_all      1.040
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
V1 V 0.81865(4) 0.05010(3) 0.37926(3) 0.02151(14) Uani 1 1 d . . .
O3 O 0.81664(16) 0.18243(14) 0.34820(13) 0.0269(4) Uani 1 1 d . . .
O2 O 0.81702(16) -0.07731(14) 0.29556(12) 0.0264(4) Uani 1 1 d . . .
O4 O 1.27510(18) 0.39750(15) 0.56852(13) 0.0325(4) Uani 1 1 d . . .
O1 O 0.82137(16) 0.05089(14) 0.48188(13) 0.0284(4) Uani 1 1 d . . .
N1 N 1.01118(19) 0.05629(16) 0.36818(14) 0.0232(4) Uani 1 1 d . . .
N2 N 0.62616(19) 0.03731(16) 0.36084(14) 0.0240(4) Uani 1 1 d . . .
C7 C 1.2368(2) 0.2803(2) 0.42755(18) 0.0266(5) Uani 1 1 d . . .
H7 H 1.2958 0.3159 0.3997 0.032 Uiso 1 1 calc R . .
C8 C 1.2164(2) 0.31404(19) 0.51566(18) 0.0256(5) Uani 1 1 d . . .
C9 C 1.0235(2) -0.10310(19) 0.25732(17) 0.0249(5) Uani 1 1 d . . .
O5 O 0.35162(19) -0.29153(16) 0.44917(15) 0.0370(5) Uani 1 1 d . . .
C11 C 0.8583(2) -0.21722(19) 0.17930(17) 0.0254(5) Uani 1 1 d . . .
C12 C 1.0630(2) 0.17609(19) 0.50793(17) 0.0257(5) Uani 1 1 d . . .
H12 H 1.0040 0.1404 0.5357 0.031 Uiso 1 1 calc R . .
C13 C 0.6719(2) 0.38145(19) 0.25833(17) 0.0259(5) Uani 1 1 d . . .
H13 H 0.6936 0.4442 0.2406 0.031 Uiso 1 1 calc R . .
C14 C 0.5186(2) 0.2576(2) 0.27712(18) 0.0265(5) Uani 1 1 d . . .
H14 H 0.4356 0.2332 0.2738 0.032 Uiso 1 1 calc R . .
C15 C 0.7323(2) 0.23631(18) 0.31806(16) 0.0227(5) Uani 1 1 d . . .
C16 C 0.5482(2) 0.3470(2) 0.24897(17) 0.0255(5) Uani 1 1 d . . .
C17 C 0.9445(2) 0.3958(2) 0.39426(18) 0.0304(6) Uani 1 1 d . . .
H17A H 0.8948 0.4474 0.4289 0.046 Uiso 1 1 calc R . .
H17B H 1.0297 0.4221 0.3978 0.046 Uiso 1 1 calc R . .
H17C H 0.9392 0.3322 0.4173 0.046 Uiso 1 1 calc R . .
C18 C 1.1708(2) 0.1942(2) 0.37970(18) 0.0266(5) Uani 1 1 d . . .
H18 H 1.1864 0.1706 0.3195 0.032 Uiso 1 1 calc R . .
C19 C 0.7646(2) 0.33040(18) 0.29151(16) 0.0231(5) Uani 1 1 d . . .
C20 C 0.9474(2) -0.2724(2) 0.13192(18) 0.0278(5) Uani 1 1 d . . .
H20 H 0.9214 -0.3313 0.0888 0.033 Uiso 1 1 calc R . .
C21 C 1.1289(2) 0.2611(2) 0.55606(18) 0.0274(5) Uani 1 1 d . . .
H21 H 1.1148 0.2836 0.6166 0.033 Uiso 1 1 calc R . .
C22 C 0.6083(2) 0.20112(19) 0.31088(17) 0.0232(5) Uani 1 1 d . . .
C23 C 0.5637(2) 0.10763(19) 0.33564(18) 0.0254(5) Uani 1 1 d . . .
H23 H 0.4776 0.0961 0.3332 0.030 Uiso 1 1 calc R . .
C24 C 0.7221(2) -0.2481(2) 0.16106(18) 0.0277(5) Uani 1 1 d . . .
C25 C 0.5558(2) -0.04997(19) 0.37919(17) 0.0246(5) Uani 1 1 d . . .
C26 C 0.5249(2) -0.1794(2) 0.46669(18) 0.0295(5) Uani 1 1 d . . .
H26 H 0.5526 -0.2121 0.5121 0.035 Uiso 1 1 calc R . .
C27 C 1.1625(3) -0.3161(2) 0.08591(18) 0.0301(6) Uani 1 1 d . . .
C28 C 1.1086(2) -0.16194(19) 0.20557(17) 0.0260(5) Uani 1 1 d . . .
H28 H 1.1928 -0.1417 0.2142 0.031 Uiso 1 1 calc R . .
C29 C 0.9767(2) 0.2949(2) 0.24125(19) 0.0305(6) Uani 1 1 d . . .
H29A H 1.0619 0.3213 0.2470 0.046 Uiso 1 1 calc R . .
H29B H 0.9482 0.2843 0.1797 0.046 Uiso 1 1 calc R . .
H29C H 0.9705 0.2291 0.2610 0.046 Uiso 1 1 calc R . .
C30 C 0.8973(2) 0.3732(2) 0.29793(17) 0.0253(5) Uani 1 1 d . . .
C31 C 1.0826(2) 0.14259(19) 0.41889(17) 0.0245(5) Uani 1 1 d . . .
C32 C 1.0720(2) -0.01328(19) 0.31882(17) 0.0259(5) Uani 1 1 d . . .
H32 H 1.1584 -0.0039 0.3238 0.031 Uiso 1 1 calc R . .
C33 C 0.4541(2) 0.4087(2) 0.20920(19) 0.0287(5) Uani 1 1 d . . .
C34 C 0.8977(2) -0.12997(18) 0.24613(17) 0.0238(5) Uani 1 1 d . . .
C35 C 0.5947(2) -0.0991(2) 0.44626(18) 0.0267(5) Uani 1 1 d . . .
H35 H 0.6696 -0.0769 0.4778 0.032 Uiso 1 1 calc R . .
C36 C 0.4156(2) -0.2130(2) 0.42234(19) 0.0289(5) Uani 1 1 d . . .
C37 C 0.6683(3) -0.2810(2) 0.24150(19) 0.0308(6) Uani 1 1 d . . .
H37A H 0.7099 -0.3410 0.2535 0.046 Uiso 1 1 calc R . .
H37B H 0.5810 -0.2990 0.2301 0.046 Uiso 1 1 calc R . .
H37C H 0.6796 -0.2241 0.2923 0.046 Uiso 1 1 calc R . .
C38 C 1.0733(2) -0.2477(2) 0.14307(17) 0.0266(5) Uani 1 1 d . . .
C39 C 0.3769(2) -0.1665(2) 0.35390(19) 0.0306(6) Uani 1 1 d . . .
H39 H 0.3020 -0.1892 0.3225 0.037 Uiso 1 1 calc R . .
C40 C 1.3592(3) 0.4563(2) 0.5279(2) 0.0368(6) Uani 1 1 d . . .
H40A H 1.3185 0.4763 0.4774 0.055 Uiso 1 1 calc R . .
H40B H 1.4286 0.4147 0.5082 0.055 Uiso 1 1 calc R . .
H40C H 1.3883 0.5183 0.5702 0.055 Uiso 1 1 calc R . .
C41 C 0.7024(3) -0.3390(2) 0.0827(2) 0.0380(7) Uani 1 1 d . . .
H41A H 0.7335 -0.3188 0.0299 0.057 Uiso 1 1 calc R . .
H41B H 0.6151 -0.3582 0.0736 0.057 Uiso 1 1 calc R . .
H41C H 0.7462 -0.3980 0.0946 0.057 Uiso 1 1 calc R . .
C42 C 0.4477(2) -0.0875(2) 0.33196(19) 0.0294(5) Uani 1 1 d . . .
H42 H 0.4224 -0.0581 0.2839 0.035 Uiso 1 1 calc R . .
C43 C 0.9114(3) 0.4741(2) 0.2647(2) 0.0329(6) Uani 1 1 d . . .
H43A H 0.8610 0.5257 0.2988 0.049 Uiso 1 1 calc R . .
H43B H 0.8850 0.4621 0.2027 0.049 Uiso 1 1 calc R . .
H43C H 0.9971 0.4991 0.2714 0.049 Uiso 1 1 calc R . .
C44 C 0.4997(3) 0.4337(3) 0.1235(2) 0.0372(6) Uani 1 1 d . . .
H44A H 0.5746 0.4778 0.1357 0.056 Uiso 1 1 calc R . .
H44B H 0.4372 0.4697 0.0969 0.056 Uiso 1 1 calc R . .
H44C H 0.5165 0.3696 0.0830 0.056 Uiso 1 1 calc R . .
C45 C 0.4349(3) 0.5100(2) 0.2744(2) 0.0397(7) Uani 1 1 d . . .
H45A H 0.3988 0.4945 0.3274 0.060 Uiso 1 1 calc R . .
H45B H 0.3800 0.5521 0.2472 0.060 Uiso 1 1 calc R . .
H45C H 0.5136 0.5479 0.2900 0.060 Uiso 1 1 calc R . .
C46 C 1.2949(3) -0.2766(3) 0.1071(2) 0.0411(7) Uani 1 1 d . . .
H46A H 1.3039 -0.2048 0.1004 0.062 Uiso 1 1 calc R . .
H46B H 1.3484 -0.3188 0.0669 0.062 Uiso 1 1 calc R . .
H46C H 1.3173 -0.2810 0.1676 0.062 Uiso 1 1 calc R . .
C47 C 0.6530(3) -0.1576(2) 0.1385(2) 0.0356(6) Uani 1 1 d . . .
H47A H 0.6614 -0.0988 0.1880 0.053 Uiso 1 1 calc R . .
H47B H 0.5664 -0.1785 0.1267 0.053 Uiso 1 1 calc R . .
H47C H 0.6870 -0.1378 0.0864 0.053 Uiso 1 1 calc R . .
C48 C 0.2299(3) -0.3137(2) 0.4156(2) 0.0396(7) Uani 1 1 d . . .
H48A H 0.2302 -0.3432 0.3527 0.059 Uiso 1 1 calc R . .
H48B H 0.1856 -0.2500 0.4249 0.059 Uiso 1 1 calc R . .
H48C H 0.1898 -0.3632 0.4460 0.059 Uiso 1 1 calc R . .
C49 C 1.1488(3) -0.4264(2) 0.1019(2) 0.0428(7) Uani 1 1 d . . .
H49A H 1.1704 -0.4265 0.1634 0.064 Uiso 1 1 calc R . .
H49B H 1.2031 -0.4705 0.0639 0.064 Uiso 1 1 calc R . .
H49C H 1.0642 -0.4527 0.0886 0.064 Uiso 1 1 calc R . .
C50 C 1.1315(3) -0.3162(3) -0.0107(2) 0.0449(8) Uani 1 1 d . . .
H50A H 1.0494 -0.3476 -0.0264 0.067 Uiso 1 1 calc R . .
H50B H 1.1907 -0.3559 -0.0476 0.067 Uiso 1 1 calc R . .
H50C H 1.1345 -0.2452 -0.0200 0.067 Uiso 1 1 calc R . .
C51 C 0.3317(3) 0.3485(3) 0.1887(2) 0.0402(7) Uani 1 1 d . . .
H51A H 0.3430 0.2834 0.1478 0.060 Uiso 1 1 calc R . .
H51B H 0.2746 0.3893 0.1621 0.060 Uiso 1 1 calc R . .
H51C H 0.2987 0.3341 0.2431 0.060 Uiso 1 1 calc R . .
C52 C 0.6061(5) 0.1146(4) 0.0772(3) 0.0794(15) Uani 1 1 d . . .
H52A H 0.5899 0.1022 0.0136 0.119 Uiso 1 1 calc R . .
H52B H 0.5960 0.1875 0.1024 0.119 Uiso 1 1 calc R . .
H52C H 0.5486 0.0718 0.1032 0.119 Uiso 1 1 calc R . .
N4 N 0.8236(5) 0.0677(4) 0.1086(4) 0.1022(17) Uani 1 1 d . . .
C54 C 0.7270(5) 0.0890(3) 0.0948(3) 0.0667(13) Uani 1 1 d . . .
N3 N 1.3231(4) 0.0370(4) 0.1496(3) 0.0790(12) Uani 1 1 d . . .
C56 C 1.2332(4) 0.0588(4) 0.1231(3) 0.0667(12) Uani 1 1 d . . .
C59 C 1.1200(5) 0.0895(6) 0.0878(5) 0.129(3) Uani 1 1 d . . .
H59A H 1.1230 0.0794 0.0239 0.193 Uiso 1 1 calc R . .
H59B H 1.1088 0.1624 0.1125 0.193 Uiso 1 1 calc R . .
H59C H 1.0516 0.0475 0.1033 0.193 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 1.596(2) . ?
V1 O3 1.9109(19) . ?
V1 O2 1.9165(19) . ?
V1 N2 2.119(2) . ?
V1 N1 2.126(2) . ?
O3 C15 1.324(3) . ?
O2 C34 1.320(3) . ?
O4 C8 1.365(3) . ?
O4 C40 1.424(3) . ?
N1 C32 1.300(3) . ?
N1 C31 1.440(3) . ?
N2 C23 1.295(3) . ?
N2 C25 1.444(3) . ?
C7 C8 1.384(4) . ?
C7 C18 1.394(4) . ?
C8 C21 1.402(4) . ?
C9 C28 1.409(4) . ?
C9 C34 1.410(3) . ?
C9 C32 1.442(3) . ?
O5 C36 1.371(3) . ?
O5 C48 1.417(4) . ?
C11 C20 1.388(4) . ?
C11 C34 1.435(3) . ?
C11 C24 1.537(4) . ?
C12 C21 1.385(4) . ?
C12 C31 1.396(4) . ?
C13 C19 1.388(3) . ?
C13 C16 1.409(4) . ?
C14 C16 1.373(4) . ?
C14 C22 1.413(3) . ?
C15 C22 1.414(3) . ?
C15 C19 1.424(3) . ?
C16 C33 1.534(4) . ?
C17 C30 1.540(4) . ?
C18 C31 1.387(4) . ?
C19 C30 1.534(3) . ?
C20 C38 1.404(4) . ?
C22 C23 1.440(3) . ?
C24 C37 1.532(4) . ?
C24 C41 1.538(4) . ?
C24 C47 1.539(4) . ?
C25 C42 1.396(4) . ?
C25 C35 1.402(4) . ?
C26 C36 1.378(4) . ?
C26 C35 1.379(4) . ?
C27 C46 1.527(4) . ?
C27 C50 1.533(4) . ?
C27 C49 1.533(4) . ?
C27 C38 1.543(4) . ?
C28 C38 1.374(4) . ?
C29 C30 1.541(4) . ?
C30 C43 1.530(4) . ?
C33 C51 1.525(4) . ?
C33 C44 1.531(4) . ?
C33 C45 1.541(4) . ?
C36 C39 1.398(4) . ?
C39 C42 1.381(4) . ?
C52 C54 1.417(8) . ?
N4 C54 1.134(7) . ?
N3 C56 1.130(6) . ?
C56 C59 1.451(8) . ?

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 115.50(10) . . ?
O1 V1 O2 120.63(9) . . ?
O3 V1 O2 123.87(9) . . ?
O1 V1 N2 96.22(9) . . ?
O3 V1 N2 88.61(8) . . ?
O2 V1 N2 85.43(9) . . ?
O1 V1 N1 95.74(9) . . ?
O3 V1 N1 88.28(8) . . ?
O2 V1 N1 86.54(9) . . ?
N2 V1 N1 167.82(9) . . ?
C15 O3 V1 135.00(16) . . ?
C34 O2 V1 136.14(16) . . ?
C8 O4 C40 116.7(2) . . ?
C32 N1 C31 115.9(2) . . ?
C32 N1 V1 124.96(17) . . ?
C31 N1 V1 119.13(16) . . ?
C23 N2 C25 115.7(2) . . ?
C23 N2 V1 122.92(17) . . ?
C25 N2 V1 121.34(16) . . ?
C8 C7 C18 120.0(2) . . ?
O4 C8 C7 125.0(2) . . ?
O4 C8 C21 115.5(2) . . ?
C7 C8 C21 119.5(2) . . ?
C28 C9 C34 120.8(2) . . ?
C28 C9 C32 116.5(2) . . ?
C34 C9 C32 122.7(2) . . ?
C36 O5 C48 116.9(2) . . ?
C20 C11 C34 117.7(2) . . ?
C20 C11 C24 121.3(2) . . ?
C34 C11 C24 120.9(2) . . ?
C21 C12 C31 120.4(2) . . ?
C19 C13 C16 124.8(2) . . ?
C16 C14 C22 121.7(2) . . ?
O3 C15 C22 120.6(2) . . ?
O3 C15 C19 120.7(2) . . ?
C22 C15 C19 118.7(2) . . ?
C14 C16 C13 116.6(2) . . ?
C14 C16 C33 123.2(2) . . ?
C13 C16 C33 120.2(2) . . ?
C31 C18 C7 120.7(2) . . ?
C13 C19 C15 117.6(2) . . ?
C13 C19 C30 121.0(2) . . ?
C15 C19 C30 121.3(2) . . ?
C11 C20 C38 124.8(2) . . ?
C12 C21 C8 120.2(2) . . ?
C14 C22 C15 120.6(2) . . ?
C14 C22 C23 115.3(2) . . ?
C15 C22 C23 124.1(2) . . ?
N2 C23 C22 128.2(2) . . ?
C37 C24 C11 109.8(2) . . ?
C37 C24 C41 108.0(2) . . ?
C11 C24 C41 111.3(2) . . ?
C37 C24 C47 110.0(2) . . ?
C11 C24 C47 110.4(2) . . ?
C41 C24 C47 107.3(2) . . ?
C42 C25 C35 118.1(2) . . ?
C42 C25 N2 121.7(2) . . ?
C35 C25 N2 120.2(2) . . ?
C36 C26 C35 121.2(2) . . ?
C46 C27 C50 109.0(3) . . ?
C46 C27 C49 108.6(3) . . ?
C50 C27 C49 109.5(3) . . ?
C46 C27 C38 111.7(2) . . ?
C50 C27 C38 108.7(2) . . ?
C49 C27 C38 109.4(2) . . ?
C38 C28 C9 122.0(2) . . ?
C43 C30 C19 112.5(2) . . ?
C43 C30 C17 107.1(2) . . ?
C19 C30 C17 109.9(2) . . ?
C43 C30 C29 107.1(2) . . ?
C19 C30 C29 109.6(2) . . ?
C17 C30 C29 110.6(2) . . ?
C18 C31 C12 119.1(2) . . ?
C18 C31 N1 120.5(2) . . ?
C12 C31 N1 120.4(2) . . ?
N1 C32 C9 127.5(2) . . ?
C51 C33 C44 107.8(2) . . ?
C51 C33 C16 111.7(2) . . ?
C44 C33 C16 110.0(2) . . ?
C51 C33 C45 108.8(3) . . ?
C44 C33 C45 109.2(2) . . ?
C16 C33 C45 109.3(2) . . ?
O2 C34 C9 121.6(2) . . ?
O2 C34 C11 120.2(2) . . ?
C9 C34 C11 118.2(2) . . ?
C26 C35 C25 120.4(2) . . ?
O5 C36 C26 116.6(2) . . ?
O5 C36 C39 124.2(3) . . ?
C26 C36 C39 119.1(2) . . ?
C28 C38 C20 116.5(2) . . ?
C28 C38 C27 124.2(2) . . ?
C20 C38 C27 119.4(2) . . ?
C42 C39 C36 119.9(3) . . ?
C39 C42 C25 121.2(3) . . ?
N4 C54 C52 179.4(6) . . ?
N3 C56 C59 178.1(6) . . ?

_diffrn_measured_fraction_theta_max 0.990
_diffrn_reflns_theta_full        27.52
_diffrn_measured_fraction_theta_full 0.990
_refine_diff_density_max         0.461
_refine_diff_density_min         -0.579
_refine_diff_density_rms         0.146

_database_code_depnum_ccdc_archive 'CCDC 980003'
#######################################################################
#
#                 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_4

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C46 H60 N2 O5 V'
_chemical_formula_sum            'C46 H60 N2 O5 V'
_chemical_formula_weight         771.90

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/n'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_Int_Tables_number      14

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                   13.997(3)
_cell_length_b                   18.580(4)
_cell_length_c                   17.898(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 104.38(3)
_cell_angle_gamma                90.00
_cell_volume                     4508.7(18)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    25974
_cell_measurement_theta_min      1.61
_cell_measurement_theta_max      25.00

_exptl_crystal_description       Plate
_exptl_crystal_colour            brown
_exptl_crystal_size_max          0.501
_exptl_crystal_size_mid          0.464
_exptl_crystal_size_min          0.353
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.137
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1652
_exptl_absorpt_coefficient_mu    0.263
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_absorpt_correction_T_min  0.5637
_exptl_absorpt_correction_T_max  1.0000

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Saturn724+ CCD'
_diffrn_measurement_method       'ω scans at fixed χ = 45°'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         none
_diffrn_standards_interval_count none
_diffrn_standards_interval_time  none
_diffrn_standards_decay_%        none
_diffrn_reflns_number            25974
_diffrn_reflns_av_R_equivalents  0.0619
_diffrn_reflns_av_unetI/netI     0.0601
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         1.61
_diffrn_reflns_theta_max         25.00
_reflns_number_total             7916
_reflns_number_gt                6970
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrystalClear (Rigaku Inc., 2007)'
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2007)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'CAMERON (Watkin et al, 1993)'
_computing_publication_material  'SHELX97 (Sheldrick, 1997)'


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

 Non-hydrogen atoms closer than 1.7 Α were restrainted to have the
 same U(ij) values with an e.s.d. of 0.01 (SIMU 0.01 0.01 1.7). 
 The thermal parameters of non-hydrogen atoms were restrained to
 approximate to isotropic behaviour with an e.s.d. of 0.01
 (ISOR 0.01).
;

_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)+(0.1515P)²+3.4597P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         7916
_refine_ls_number_parameters     532
_refine_ls_number_restraints     714
_refine_ls_R_factor_ref          0.1043
_refine_ls_R_factor_gt           0.0857
_refine_ls_wR_factor_ref         0.2769
_refine_ls_wR_factor_gt          0.2459
_refine_ls_goodness_of_fit_ref   1.222
_refine_ls_restrained_S_all      1.227
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
V1 V 0.72014(5) 0.05035(3) 0.72338(4) 0.0295(3) Uani 1 1 d U . .
O1 O 0.8263(2) 0.04443(16) 0.78291(18) 0.0415(7) Uani 1 1 d U . .
N2 N 0.7329(2) -0.05195(17) 0.67197(19) 0.0295(7) Uani 1 1 d U . .
O3 O 0.6095(2) 0.01236(15) 0.75462(16) 0.0356(7) Uani 1 1 d U . .
O2 O 0.70758(19) 0.09452(14) 0.62413(16) 0.0315(6) Uani 1 1 d U . .
O4 O 0.5335(3) 0.22647(19) 0.7989(2) 0.0535(9) Uani 1 1 d U . .
O5 O 0.6872(2) -0.11940(16) 0.52793(17) 0.0387(7) Uani 1 1 d U . .
N1 N 0.6894(2) 0.15406(18) 0.76382(19) 0.0324(7) Uani 1 1 d U . .
C25 C 0.9010(3) -0.0361(2) 0.6579(3) 0.0356(9) Uani 1 1 d U . .
H25 H 0.9170 -0.0138 0.7072 0.043 Uiso 1 1 calc R . .
C15 C 0.6141(3) -0.1148(2) 0.7312(2) 0.0311(8) Uani 1 1 d U . .
C26 C 0.9726(3) -0.0425(2) 0.6163(3) 0.0407(10) Uani 1 1 d U . .
H26 H 1.0374 -0.0248 0.6372 0.049 Uiso 1 1 calc R . .
C33 C 0.6108(3) 0.0559(2) 0.4601(3) 0.0420(10) Uani 1 1 d U . .
H33A H 0.6166 0.0169 0.4245 0.063 Uiso 1 1 calc R . .
H33B H 0.5451 0.0776 0.4438 0.063 Uiso 1 1 calc R . .
H33C H 0.6206 0.0365 0.5123 0.063 Uiso 1 1 calc R . .
C28 C 0.8562(3) -0.1018(2) 0.5147(3) 0.0373(9) Uani 1 1 d U . .
H28 H 0.8420 -0.1251 0.4659 0.045 Uiso 1 1 calc R . .
C14 C 0.5761(3) -0.0542(2) 0.7618(2) 0.0301(8) Uani 1 1 d U . .
C29 C 0.7819(3) -0.0957(2) 0.5548(2) 0.0338(9) Uani 1 1 d U . .
C27 C 0.9487(3) -0.0744(2) 0.5450(3) 0.0409(10) Uani 1 1 d U . .
H27 H 0.9971 -0.0777 0.5162 0.049 Uiso 1 1 calc R . .
C17 C 0.5182(3) -0.1971(2) 0.7894(2) 0.0293(8) Uani 1 1 d U . .
C24 C 0.8058(3) -0.0623(2) 0.6274(2) 0.0311(8) Uani 1 1 d U . .
C32 C 0.7937(3) 0.0811(2) 0.4815(3) 0.0376(10) Uani 1 1 d U . .
H32A H 0.8087 0.0649 0.5352 0.056 Uiso 1 1 calc R . .
H32B H 0.8420 0.1174 0.4755 0.056 Uiso 1 1 calc R . .
H32C H 0.7968 0.0400 0.4478 0.056 Uiso 1 1 calc R . .
C40 C 0.6732(3) 0.2910(2) 0.6145(2) 0.0331(9) Uani 1 1 d U . .
H40 H 0.6698 0.3297 0.6485 0.040 Uiso 1 1 calc R . .
C41 C 0.6668(3) 0.3060(2) 0.5386(2) 0.0380(9) Uani 1 1 d U A .
C34 C 0.6733(4) 0.1406(3) 0.3757(2) 0.0438(11) Uani 1 1 d U . .
H34A H 0.6736 0.0996 0.3414 0.066 Uiso 1 1 calc R . .
H34B H 0.7261 0.1741 0.3722 0.066 Uiso 1 1 calc R . .
H34C H 0.6095 0.1653 0.3602 0.066 Uiso 1 1 calc R . .
C30 C 0.6601(3) -0.1471(3) 0.4501(3) 0.0439(10) Uani 1 1 d U . .
H30A H 0.6969 -0.1920 0.4467 0.053 Uiso 1 1 calc R . .
H30B H 0.6760 -0.1115 0.4139 0.053 Uiso 1 1 calc R . .
C38 C 0.6845(3) 0.2207(2) 0.6441(2) 0.0315(8) Uani 1 1 d U . .
C13 C 0.4984(3) -0.0651(2) 0.8002(2) 0.0337(9) Uani 1 1 d U . .
C23 C 0.6866(3) -0.1098(2) 0.6864(2) 0.0293(8) Uani 1 1 d U . .
H23 H 0.7027 -0.1535 0.6648 0.035 Uiso 1 1 calc R . .
C35 C 0.6899(3) 0.1137(2) 0.4593(2) 0.0323(8) Uani 1 1 d U . .
C16 C 0.5852(3) -0.1853(2) 0.7460(2) 0.0293(8) Uani 1 1 d U . .
H16 H 0.6126 -0.2253 0.7255 0.035 Uiso 1 1 calc R . .
C37 C 0.6932(3) 0.1612(2) 0.5961(2) 0.0290(8) Uani 1 1 d U . .
C42 C 0.6718(3) 0.2463(2) 0.4913(2) 0.0355(9) Uani 1 1 d U . .
H42 H 0.6659 0.2553 0.4381 0.043 Uiso 1 1 calc R . .
C36 C 0.6846(3) 0.1753(2) 0.5160(2) 0.0292(8) Uani 1 1 d U . .
C39 C 0.6840(3) 0.2129(2) 0.7239(2) 0.0333(9) Uani 1 1 d U . .
H39 H 0.6790 0.2563 0.7508 0.040 Uiso 1 1 calc R . .
C9 C 0.4096(4) 0.0540(3) 0.7636(3) 0.0541(13) Uani 1 1 d U . .
H9A H 0.4665 0.0738 0.7478 0.081 Uiso 1 1 calc R . .
H9B H 0.3747 0.0930 0.7826 0.081 Uiso 1 1 calc R . .
H9C H 0.3650 0.0308 0.7193 0.081 Uiso 1 1 calc R . .
C22 C 0.3782(3) -0.2834(3) 0.7895(3) 0.0463(11) Uani 1 1 d U . .
H22A H 0.3461 -0.2452 0.8122 0.069 Uiso 1 1 calc R . .
H22B H 0.3616 -0.3303 0.8077 0.069 Uiso 1 1 calc R . .
H22C H 0.3553 -0.2813 0.7331 0.069 Uiso 1 1 calc R . .
C20 C 0.5391(3) -0.3327(2) 0.7779(3) 0.0463(11) Uani 1 1 d U . .
H20A H 0.5198 -0.3286 0.7216 0.069 Uiso 1 1 calc R . .
H20B H 0.5181 -0.3795 0.7934 0.069 Uiso 1 1 calc R . .
H20C H 0.6110 -0.3285 0.7960 0.069 Uiso 1 1 calc R . .
C18 C 0.4754(3) -0.1362(2) 0.8139(2) 0.0327(9) Uani 1 1 d U . .
H18 H 0.4269 -0.1438 0.8420 0.039 Uiso 1 1 calc R . .
C19 C 0.4903(3) -0.2727(2) 0.8134(3) 0.0362(9) Uani 1 1 d U . .
C5 C 0.6056(4) 0.2025(2) 0.8603(3) 0.0462(11) Uani 1 1 d U . .
C6 C 0.6850(4) 0.1650(2) 0.8437(2) 0.0415(10) Uani 1 1 d U . .
C12 C 0.4453(4) -0.0017(2) 0.8281(3) 0.0457(10) Uani 1 1 d U . .
C7 C 0.7600(4) 0.1377(3) 0.9026(3) 0.0491(11) Uani 1 1 d U . .
H7 H 0.8132 0.1120 0.8909 0.059 Uiso 1 1 calc R . .
C21 C 0.5258(4) -0.2778(3) 0.9017(3) 0.0497(12) Uani 1 1 d U . .
H21A H 0.5976 -0.2721 0.9173 0.075 Uiso 1 1 calc R . .
H21B H 0.5077 -0.3249 0.9188 0.075 Uiso 1 1 calc R . .
H21C H 0.4946 -0.2398 0.9253 0.075 Uiso 1 1 calc R . .
C49 C 0.6563(5) 0.3828(3) 0.5070(3) 0.0585(12) Uani 1 1 d U . .
C11 C 0.3531(4) -0.0269(3) 0.8544(4) 0.0639(14) Uani 1 1 d U . .
H11A H 0.3105 -0.0555 0.8134 0.096 Uiso 1 1 calc R . .
H11B H 0.3167 0.0151 0.8655 0.096 Uiso 1 1 calc R . .
H11C H 0.3740 -0.0564 0.9011 0.096 Uiso 1 1 calc R . .
C31 C 0.5523(4) -0.1617(3) 0.4303(3) 0.0594(14) Uani 1 1 d U . .
H31A H 0.5309 -0.1774 0.3765 0.089 Uiso 1 1 calc R . .
H31B H 0.5169 -0.1177 0.4372 0.089 Uiso 1 1 calc R . .
H31C H 0.5380 -0.1995 0.4641 0.089 Uiso 1 1 calc R . .
C8 C 0.7569(5) 0.1481(3) 0.9801(3) 0.0639(14) Uani 1 1 d U . .
H8 H 0.8082 0.1302 1.0211 0.077 Uiso 1 1 calc R . .
C10 C 0.5174(5) 0.0339(3) 0.8980(3) 0.0592(14) Uani 1 1 d U . .
H10A H 0.5307 0.0005 0.9418 0.089 Uiso 1 1 calc R . .
H10B H 0.4879 0.0781 0.9121 0.089 Uiso 1 1 calc R . .
H10C H 0.5793 0.0455 0.8845 0.089 Uiso 1 1 calc R . .
C2 C 0.4526(4) 0.2682(3) 0.8143(4) 0.0678(15) Uani 1 1 d U . .
H2A H 0.4784 0.3093 0.8486 0.081 Uiso 1 1 calc R . .
H2B H 0.4118 0.2378 0.8397 0.081 Uiso 1 1 calc R . .
C1 C 0.3916(5) 0.2950(4) 0.7372(4) 0.087(2) Uani 1 1 d U . .
H1A H 0.3742 0.2544 0.7015 0.131 Uiso 1 1 calc R . .
H1B H 0.4299 0.3302 0.7160 0.131 Uiso 1 1 calc R . .
H1C H 0.3313 0.3178 0.7442 0.131 Uiso 1 1 calc R . .
C3 C 0.6038(5) 0.2126(3) 0.9373(3) 0.0584(13) Uani 1 1 d U . .
H3 H 0.5513 0.2385 0.9498 0.070 Uiso 1 1 calc R . .
C4 C 0.6789(5) 0.1845(3) 0.9952(3) 0.0628(14) Uani 1 1 d U . .
H4 H 0.6762 0.1907 1.0473 0.075 Uiso 1 1 calc R . .
C45 C 0.6216(14) 0.3922(8) 0.4244(8) 0.082(3) Uani 0.464(7) 1 d PU A 1
H45A H 0.6001 0.4420 0.4131 0.123 Uiso 0.464(7) 1 calc PR A 1
H45B H 0.5661 0.3596 0.4045 0.123 Uiso 0.464(7) 1 calc PR A 1
H45C H 0.6751 0.3812 0.3998 0.123 Uiso 0.464(7) 1 calc PR A 1
C43 C 0.7647(12) 0.4178(8) 0.5312(10) 0.086(3) Uani 0.464(7) 1 d PU A 1
H43A H 0.8048 0.3985 0.4981 0.128 Uiso 0.464(7) 1 calc PR A 1
H43B H 0.7957 0.4059 0.5852 0.128 Uiso 0.464(7) 1 calc PR A 1
H43C H 0.7595 0.4702 0.5252 0.128 Uiso 0.464(7) 1 calc PR A 1
C47 C 0.5845(13) 0.4300(8) 0.5401(10) 0.079(3) Uani 0.464(7) 1 d PU A 1
H47A H 0.5759 0.4768 0.5140 0.119 Uiso 0.464(7) 1 calc PR A 1
H47B H 0.6120 0.4372 0.5955 0.119 Uiso 0.464(7) 1 calc PR A 1
H47C H 0.5205 0.4058 0.5316 0.119 Uiso 0.464(7) 1 calc PR A 1
C48 C 0.6597(10) 0.4379(5) 0.5685(7) 0.063(3) Uani 0.536(7) 1 d PU A 2
H48A H 0.6444 0.4854 0.5447 0.095 Uiso 0.536(7) 1 calc PR A 2
H48B H 0.7257 0.4387 0.6035 0.095 Uiso 0.536(7) 1 calc PR A 2
H48C H 0.6110 0.4257 0.5975 0.095 Uiso 0.536(7) 1 calc PR A 2
C46 C 0.5416(11) 0.3845(7) 0.4551(8) 0.084(3) Uani 0.536(7) 1 d PU A 2
H46A H 0.5294 0.4296 0.4259 0.125 Uiso 0.536(7) 1 calc PR A 2
H46B H 0.4968 0.3812 0.4893 0.125 Uiso 0.536(7) 1 calc PR A 2
H46C H 0.5301 0.3437 0.4193 0.125 Uiso 0.536(7) 1 calc PR A 2
C44 C 0.7101(12) 0.3935(7) 0.4480(8) 0.083(3) Uani 0.536(7) 1 d PU A 2
H44A H 0.6947 0.3542 0.4103 0.125 Uiso 0.536(7) 1 calc PR A 2
H44B H 0.7811 0.3939 0.4720 0.125 Uiso 0.536(7) 1 calc PR A 2
H44C H 0.6907 0.4395 0.4219 0.125 Uiso 0.536(7) 1 calc PR A 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
V1 O1 1.603(3) . ?
V1 O3 1.908(3) . ?
V1 O2 1.925(3) . ?
V1 N2 2.138(3) . ?
V1 N1 2.139(3) . ?
N2 C23 1.313(5) . ?
N2 C24 1.455(5) . ?
O3 C14 1.340(5) . ?
O2 C37 1.333(5) . ?
O4 C5 1.368(6) . ?
O4 C2 1.454(6) . ?
O5 C29 1.365(5) . ?
O5 C30 1.444(5) . ?
N1 C39 1.298(5) . ?
N1 C6 1.459(5) . ?
C25 C26 1.394(6) . ?
C25 C24 1.396(6) . ?
C25 H25 0.9500 . ?
C15 C14 1.412(6) . ?
C15 C16 1.416(6) . ?
C15 C23 1.445(5) . ?
C26 C27 1.370(7) . ?
C26 H26 0.9500 . ?
C33 C35 1.545(6) . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C28 C27 1.372(6) . ?
C28 C29 1.408(6) . ?
C28 H28 0.9500 . ?
C14 C13 1.437(6) . ?
C29 C24 1.404(6) . ?
C27 H27 0.9500 . ?
C17 C16 1.377(5) . ?
C17 C18 1.401(6) . ?
C17 C19 1.546(5) . ?
C32 C35 1.533(6) . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C40 C41 1.368(6) . ?
C40 C38 1.405(6) . ?
C40 H40 0.9500 . ?
C41 C42 1.407(6) . ?
C41 C49 1.528(6) . ?
C34 C35 1.540(6) . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
C30 C31 1.486(6) . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C38 C37 1.423(6) . ?
C38 C39 1.438(6) . ?
C13 C18 1.395(6) . ?
C13 C12 1.542(6) . ?
C23 H23 0.9500 . ?
C35 C36 1.543(6) . ?
C16 H16 0.9500 . ?
C37 C36 1.433(5) . ?
C42 C36 1.388(6) . ?
C42 H42 0.9500 . ?
C39 H39 0.9500 . ?
C9 C12 1.538(7) . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C22 C19 1.533(6) . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C20 C19 1.526(6) . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C18 H18 0.9500 . ?
C19 C21 1.537(6) . ?
C5 C3 1.398(7) . ?
C5 C6 1.405(7) . ?
C6 C7 1.387(7) . ?
C12 C10 1.547(8) . ?
C12 C11 1.552(7) . ?
C7 C8 1.412(7) . ?
C7 H7 0.9500 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C49 C45 1.446(15) . ?
C49 C44 1.454(14) . ?
C49 C48 1.496(12) . ?
C49 C47 1.559(16) . ?
C49 C43 1.607(16) . ?
C49 C46 1.644(15) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C8 C4 1.366(9) . ?
C8 H8 0.9500 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C2 C1 1.515(9) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C3 C4 1.382(9) . ?
C3 H3 0.9500 . ?
C4 H4 0.9500 . ?
C45 H45A 0.9800 . ?
C45 H45B 0.9800 . ?
C45 H45C 0.9800 . ?
C43 H43A 0.9800 . ?
C43 H43B 0.9800 . ?
C43 H43C 0.9800 . ?
C47 H47A 0.9800 . ?
C47 H47B 0.9800 . ?
C47 H47C 0.9800 . ?
C48 H48A 0.9800 . ?
C48 H48B 0.9800 . ?
C48 H48C 0.9800 . ?
C46 H46A 0.9800 . ?
C46 H46B 0.9800 . ?
C46 H46C 0.9800 . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 V1 O3 117.76(15) . . ?
O1 V1 O2 119.99(14) . . ?
O3 V1 O2 122.24(13) . . ?
O1 V1 N2 93.58(14) . . ?
O3 V1 N2 87.58(12) . . ?
O2 V1 N2 88.87(12) . . ?
O1 V1 N1 93.90(14) . . ?
O3 V1 N1 89.31(12) . . ?
O2 V1 N1 87.03(12) . . ?
N2 V1 N1 172.50(13) . . ?
C23 N2 C24 116.5(3) . . ?
C23 N2 V1 123.0(3) . . ?
C24 N2 V1 119.9(2) . . ?
C14 O3 V1 134.2(3) . . ?
C37 O2 V1 135.6(3) . . ?
C5 O4 C2 118.4(4) . . ?
C29 O5 C30 117.0(3) . . ?
C39 N1 C6 114.2(3) . . ?
C39 N1 V1 124.2(3) . . ?
C6 N1 V1 121.2(3) . . ?
C26 C25 C24 120.3(4) . . ?
C26 C25 H25 119.8 . . ?
C24 C25 H25 119.8 . . ?
C14 C15 C16 120.9(4) . . ?
C14 C15 C23 123.3(4) . . ?
C16 C15 C23 115.8(3) . . ?
C27 C26 C25 119.5(4) . . ?
C27 C26 H26 120.2 . . ?
C25 C26 H26 120.2 . . ?
C35 C33 H33A 109.5 . . ?
C35 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
C35 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C27 C28 C29 120.8(4) . . ?
C27 C28 H28 119.6 . . ?
C29 C28 H28 119.6 . . ?
O3 C14 C15 121.6(3) . . ?
O3 C14 C13 120.0(3) . . ?
C15 C14 C13 118.4(3) . . ?
O5 C29 C24 117.1(3) . . ?
O5 C29 C28 124.7(4) . . ?
C24 C29 C28 118.1(4) . . ?
C26 C27 C28 121.1(4) . . ?
C26 C27 H27 119.4 . . ?
C28 C27 H27 119.4 . . ?
C16 C17 C18 116.9(4) . . ?
C16 C17 C19 123.8(4) . . ?
C18 C17 C19 119.3(3) . . ?
C25 C24 C29 120.1(4) . . ?
C25 C24 N2 118.1(4) . . ?
C29 C24 N2 121.8(3) . . ?
C35 C32 H32A 109.5 . . ?
C35 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C35 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C41 C40 C38 122.5(4) . . ?
C41 C40 H40 118.8 . . ?
C38 C40 H40 118.8 . . ?
C40 C41 C42 115.8(4) . . ?
C40 C41 C49 122.3(4) . . ?
C42 C41 C49 121.9(4) . . ?
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 C30 C31 107.7(4) . . ?
O5 C30 H30A 110.2 . . ?
C31 C30 H30A 110.2 . . ?
O5 C30 H30B 110.2 . . ?
C31 C30 H30B 110.2 . . ?
H30A C30 H30B 108.5 . . ?
C40 C38 C37 120.9(4) . . ?
C40 C38 C39 116.1(4) . . ?
C37 C38 C39 123.0(4) . . ?
C18 C13 C14 116.9(4) . . ?
C18 C13 C12 121.0(4) . . ?
C14 C13 C12 122.0(4) . . ?
N2 C23 C15 127.6(4) . . ?
N2 C23 H23 116.2 . . ?
C15 C23 H23 116.2 . . ?
C32 C35 C34 106.5(3) . . ?
C32 C35 C36 108.7(3) . . ?
C34 C35 C36 112.2(3) . . ?
C32 C35 C33 110.9(3) . . ?
C34 C35 C33 107.4(4) . . ?
C36 C35 C33 111.0(3) . . ?
C17 C16 C15 121.3(4) . . ?
C17 C16 H16 119.4 . . ?
C15 C16 H16 119.4 . . ?
O2 C37 C38 121.5(4) . . ?
O2 C37 C36 120.9(3) . . ?
C38 C37 C36 117.6(3) . . ?
C36 C42 C41 125.5(4) . . ?
C36 C42 H42 117.3 . . ?
C41 C42 H42 117.3 . . ?
C42 C36 C37 117.6(4) . . ?
C42 C36 C35 121.3(4) . . ?
C37 C36 C35 121.1(3) . . ?
N1 C39 C38 128.1(4) . . ?
N1 C39 H39 116.0 . . ?
C38 C39 H39 116.0 . . ?
C12 C9 H9A 109.5 . . ?
C12 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C12 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 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 . . ?
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 . . ?
C13 C18 C17 125.0(4) . . ?
C13 C18 H18 117.5 . . ?
C17 C18 H18 117.5 . . ?
C20 C19 C22 108.8(4) . . ?
C20 C19 C21 108.6(4) . . ?
C22 C19 C21 109.0(4) . . ?
C20 C19 C17 112.2(3) . . ?
C22 C19 C17 110.6(3) . . ?
C21 C19 C17 107.6(4) . . ?
O4 C5 C3 123.9(5) . . ?
O4 C5 C6 117.1(4) . . ?
C3 C5 C6 119.0(5) . . ?
C7 C6 C5 120.6(4) . . ?
C7 C6 N1 119.1(4) . . ?
C5 C6 N1 120.3(4) . . ?
C9 C12 C13 111.3(4) . . ?
C9 C12 C10 110.2(4) . . ?
C13 C12 C10 108.6(4) . . ?
C9 C12 C11 107.0(4) . . ?
C13 C12 C11 111.8(4) . . ?
C10 C12 C11 108.0(4) . . ?
C6 C7 C8 119.7(5) . . ?
C6 C7 H7 120.2 . . ?
C8 C7 H7 120.2 . . ?
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 . . ?
C45 C49 C44 49.1(9) . . ?
C45 C49 C48 127.6(8) . . ?
C44 C49 C48 120.9(8) . . ?
C45 C49 C41 117.9(7) . . ?
C44 C49 C41 112.1(6) . . ?
C48 C49 C41 112.6(6) . . ?
C45 C49 C47 103.7(10) . . ?
C44 C49 C47 134.3(8) . . ?
C41 C49 C47 113.3(7) . . ?
C45 C49 C43 106.4(10) . . ?
C44 C49 C43 61.2(9) . . ?
C48 C49 C43 70.7(9) . . ?
C41 C49 C43 106.3(6) . . ?
C47 C49 C43 108.9(10) . . ?
C45 C49 C46 52.2(8) . . ?
C44 C49 C46 101.3(9) . . ?
C48 C49 C46 104.5(8) . . ?
C41 C49 C46 102.5(6) . . ?
C47 C49 C46 64.7(9) . . ?
C43 C49 C46 150.3(8) . . ?
C12 C11 H11A 109.5 . . ?
C12 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C12 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C30 C31 H31A 109.5 . . ?
C30 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C30 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C4 C8 C7 118.9(6) . . ?
C4 C8 H8 120.6 . . ?
C7 C8 H8 120.6 . . ?
C12 C10 H10A 109.5 . . ?
C12 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C12 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
O4 C2 C1 107.0(5) . . ?
O4 C2 H2A 110.3 . . ?
C1 C2 H2A 110.3 . . ?
O4 C2 H2B 110.3 . . ?
C1 C2 H2B 110.3 . . ?
H2A C2 H2B 108.6 . . ?
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
C2 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C4 C3 C5 119.5(5) . . ?
C4 C3 H3 120.3 . . ?
C5 C3 H3 120.3 . . ?
C8 C4 C3 122.3(5) . . ?
C8 C4 H4 118.8 . . ?
C3 C4 H4 118.8 . . ?
C49 C45 H45A 109.5 . . ?
C49 C45 H45B 109.5 . . ?
C49 C45 H45C 109.5 . . ?
C49 C43 H43A 109.5 . . ?
C49 C43 H43B 109.5 . . ?
C49 C43 H43C 109.5 . . ?
C49 C47 H47A 109.5 . . ?
C49 C47 H47B 109.5 . . ?
C49 C47 H47C 109.5 . . ?
C49 C48 H48A 109.5 . . ?
C49 C48 H48B 109.5 . . ?
H48A C48 H48B 109.5 . . ?
C49 C48 H48C 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?
C49 C46 H46A 109.5 . . ?
C49 C46 H46B 109.5 . . ?
H46A C46 H46B 109.5 . . ?
C49 C46 H46C 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
C49 C44 H44A 109.5 . . ?
C49 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
C49 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O1 V1 N2 C23 103.9(3) . . . . ?
O3 V1 N2 C23 -13.8(3) . . . . ?
O2 V1 N2 C23 -136.2(3) . . . . ?
O1 V1 N2 C24 -67.1(3) . . . . ?
O3 V1 N2 C24 175.2(3) . . . . ?
O2 V1 N2 C24 52.9(3) . . . . ?
O1 V1 O3 C14 -75.0(4) . . . . ?
O2 V1 O3 C14 104.9(4) . . . . ?
N2 V1 O3 C14 17.8(4) . . . . ?
N1 V1 O3 C14 -169.0(4) . . . . ?
O1 V1 O2 C37 -88.6(4) . . . . ?
O3 V1 O2 C37 91.5(3) . . . . ?
N2 V1 O2 C37 177.9(3) . . . . ?
N1 V1 O2 C37 4.2(3) . . . . ?
O1 V1 N1 C39 111.6(3) . . . . ?
O3 V1 N1 C39 -130.7(3) . . . . ?
O2 V1 N1 C39 -8.3(3) . . . . ?
O1 V1 N1 C6 -60.6(3) . . . . ?
O3 V1 N1 C6 57.2(3) . . . . ?
O2 V1 N1 C6 179.5(3) . . . . ?
C24 C25 C26 C27 0.3(7) . . . . ?
V1 O3 C14 C15 -12.2(6) . . . . ?
V1 O3 C14 C13 169.0(3) . . . . ?
C16 C15 C14 O3 173.6(4) . . . . ?
C23 C15 C14 O3 -3.8(6) . . . . ?
C16 C15 C14 C13 -7.7(6) . . . . ?
C23 C15 C14 C13 175.0(4) . . . . ?
C30 O5 C29 C24 174.0(4) . . . . ?
C30 O5 C29 C28 -5.4(6) . . . . ?
C27 C28 C29 O5 178.0(4) . . . . ?
C27 C28 C29 C24 -1.4(6) . . . . ?
C25 C26 C27 C28 -1.5(7) . . . . ?
C29 C28 C27 C26 2.1(7) . . . . ?
C26 C25 C24 C29 0.4(6) . . . . ?
C26 C25 C24 N2 -177.8(4) . . . . ?
O5 C29 C24 C25 -179.3(4) . . . . ?
C28 C29 C24 C25 0.2(6) . . . . ?
O5 C29 C24 N2 -1.1(6) . . . . ?
C28 C29 C24 N2 178.3(4) . . . . ?
C23 N2 C24 C25 -126.4(4) . . . . ?
V1 N2 C24 C25 45.2(5) . . . . ?
C23 N2 C24 C29 55.4(5) . . . . ?
V1 N2 C24 C29 -133.0(3) . . . . ?
C38 C40 C41 C42 0.3(6) . . . . ?
C38 C40 C41 C49 -178.8(4) . . . . ?
C29 O5 C30 C31 -173.6(4) . . . . ?
C41 C40 C38 C37 2.1(6) . . . . ?
C41 C40 C38 C39 -176.2(4) . . . . ?
O3 C14 C13 C18 -172.5(4) . . . . ?
C15 C14 C13 C18 8.7(6) . . . . ?
O3 C14 C13 C12 5.0(6) . . . . ?
C15 C14 C13 C12 -173.7(4) . . . . ?
C24 N2 C23 C15 177.6(4) . . . . ?
V1 N2 C23 C15 6.4(6) . . . . ?
C14 C15 C23 N2 5.4(6) . . . . ?
C16 C15 C23 N2 -172.1(4) . . . . ?
C18 C17 C16 C15 4.1(6) . . . . ?
C19 C17 C16 C15 -174.7(4) . . . . ?
C14 C15 C16 C17 1.1(6) . . . . ?
C23 C15 C16 C17 178.6(3) . . . . ?
V1 O2 C37 C38 0.9(6) . . . . ?
V1 O2 C37 C36 -178.2(3) . . . . ?
C40 C38 C37 O2 177.5(3) . . . . ?
C39 C38 C37 O2 -4.3(6) . . . . ?
C40 C38 C37 C36 -3.3(5) . . . . ?
C39 C38 C37 C36 174.9(3) . . . . ?
C40 C41 C42 C36 -1.5(6) . . . . ?
C49 C41 C42 C36 177.7(4) . . . . ?
C41 C42 C36 C37 0.2(6) . . . . ?
C41 C42 C36 C35 -179.5(4) . . . . ?
O2 C37 C36 C42 -178.7(3) . . . . ?
C38 C37 C36 C42 2.2(5) . . . . ?
O2 C37 C36 C35 1.0(5) . . . . ?
C38 C37 C36 C35 -178.1(3) . . . . ?
C32 C35 C36 C42 114.1(4) . . . . ?
C34 C35 C36 C42 -3.4(5) . . . . ?
C33 C35 C36 C42 -123.6(4) . . . . ?
C32 C35 C36 C37 -65.5(4) . . . . ?
C34 C35 C36 C37 176.9(4) . . . . ?
C33 C35 C36 C37 56.7(5) . . . . ?
C6 N1 C39 C38 -178.9(4) . . . . ?
V1 N1 C39 C38 8.4(6) . . . . ?
C40 C38 C39 N1 177.2(4) . . . . ?
C37 C38 C39 N1 -1.0(6) . . . . ?
C14 C13 C18 C17 -3.8(6) . . . . ?
C12 C13 C18 C17 178.7(4) . . . . ?
C16 C17 C18 C13 -2.7(6) . . . . ?
C19 C17 C18 C13 176.1(4) . . . . ?
C16 C17 C19 C20 -4.6(6) . . . . ?
C18 C17 C19 C20 176.7(4) . . . . ?
C16 C17 C19 C22 -126.3(4) . . . . ?
C18 C17 C19 C22 55.0(5) . . . . ?
C16 C17 C19 C21 114.7(4) . . . . ?
C18 C17 C19 C21 -64.0(5) . . . . ?
C2 O4 C5 C3 3.4(7) . . . . ?
C2 O4 C5 C6 -177.4(4) . . . . ?
O4 C5 C6 C7 -178.6(4) . . . . ?
C3 C5 C6 C7 0.6(7) . . . . ?
O4 C5 C6 N1 1.2(6) . . . . ?
C3 C5 C6 N1 -179.6(4) . . . . ?
C39 N1 C6 C7 -125.0(4) . . . . ?
V1 N1 C6 C7 47.8(5) . . . . ?
C39 N1 C6 C5 55.1(5) . . . . ?
V1 N1 C6 C5 -132.0(4) . . . . ?
C18 C13 C12 C9 -132.1(4) . . . . ?
C14 C13 C12 C9 50.5(6) . . . . ?
C18 C13 C12 C10 106.4(5) . . . . ?
C14 C13 C12 C10 -71.0(5) . . . . ?
C18 C13 C12 C11 -12.5(6) . . . . ?
C14 C13 C12 C11 170.1(4) . . . . ?
C5 C6 C7 C8 -0.5(7) . . . . ?
N1 C6 C7 C8 179.7(4) . . . . ?
C40 C41 C49 C45 -162.3(10) . . . . ?
C42 C41 C49 C45 18.6(11) . . . . ?
C40 C41 C49 C44 143.5(8) . . . . ?
C42 C41 C49 C44 -35.6(9) . . . . ?
C40 C41 C49 C48 3.1(9) . . . . ?
C42 C41 C49 C48 -176.0(7) . . . . ?
C40 C41 C49 C47 -41.0(10) . . . . ?
C42 C41 C49 C47 139.9(8) . . . . ?
C40 C41 C49 C43 78.6(9) . . . . ?
C42 C41 C49 C43 -100.5(8) . . . . ?
C40 C41 C49 C46 -108.6(7) . . . . ?
C42 C41 C49 C46 72.3(8) . . . . ?
C6 C7 C8 C4 0.8(8) . . . . ?
C5 O4 C2 C1 173.2(5) . . . . ?
O4 C5 C3 C4 178.1(5) . . . . ?
C6 C5 C3 C4 -1.0(7) . . . . ?
C7 C8 C4 C3 -1.2(8) . . . . ?
C5 C3 C4 C8 1.4(8) . . . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.882
_refine_diff_density_min         -0.717
_refine_diff_density_rms         0.190

_database_code_depnum_ccdc_archive 'CCDC 980004'
#######################################################################
#
#                 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_5

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C44 H50 F6 N2 O5 V '
_chemical_formula_sum            'C44 H50 F6 N2 O5 V '
_chemical_formula_weight         851.80

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           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                   14.096(3)
_cell_length_b                   15.274(3)
_cell_length_c                   24.527(5)
_cell_angle_alpha                87.65(3)
_cell_angle_beta                 75.73(3)
_cell_angle_gamma                64.15(3)
_cell_volume                     4592.1(16)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    35870
_cell_measurement_theta_min      0.86
_cell_measurement_theta_max      25.00

_exptl_crystal_description       plate
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.320
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.140
_exptl_crystal_density_meas      35870
_exptl_crystal_density_diffrn    1.232
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1780
_exptl_absorpt_coefficient_mu    0.283
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_absorpt_correction_T_min  0.6663
_exptl_absorpt_correction_T_max  1.0000

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'MM007-HF CCD(Saturn 724+)'
_diffrn_measurement_method       'ω scans at fixed χ = 45°'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         none
_diffrn_standards_interval_count none
_diffrn_standards_interval_time  none
_diffrn_standards_decay_%        none
_diffrn_reflns_number            35870
_diffrn_reflns_av_R_equivalents  0.0739
_diffrn_reflns_av_unetI/netI     0.1066
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         0.86
_diffrn_reflns_theta_max         25.00
_reflns_number_total             16108
_reflns_number_gt                11635
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrystalClear (Rigaku Inc., 2007)'
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2007)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'CAMERON (Watkin et al, 1993)'
_computing_publication_material  'SHELX97 (Sheldrick, 1997)'


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

 Non-hydrogen atoms closer than 1.7 Α were restrainted to have the
 same U(ij) values with an e.s.d. of 0.01 (SIMU 0.01 0.01 1.7). 
 The thermal parameters of non-hydrogen atoms were restrained to
 approximate to isotropic behaviour with an e.s.d. of 0.01
 (ISOR 0.01).
;

_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)+(0.1861P)²+5.1950P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         16108
_refine_ls_number_parameters     1069
_refine_ls_number_restraints     1404
_refine_ls_R_factor_ref          0.1416
_refine_ls_R_factor_gt           0.1081
_refine_ls_wR_factor_ref         0.3372
_refine_ls_wR_factor_gt          0.3030
_refine_ls_goodness_of_fit_ref   1.111
_refine_ls_restrained_S_all      1.108
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
V1 V 0.38615(7) 0.74319(6) -0.02634(4) 0.0211(3) Uani 1 1 d U . .
V2 V 0.38132(8) 0.63253(7) 0.42199(4) 0.0259(3) Uani 1 1 d U . .
O1 O 0.5069(3) 0.7151(3) -0.06486(17) 0.0301(9) Uani 1 1 d U . .
N3 N 0.4537(4) 0.4774(4) 0.4227(2) 0.0315(11) Uani 1 1 d U . .
O7 O 0.5179(3) 0.6165(3) 0.37364(17) 0.0307(9) Uani 1 1 d U . .
O5 O 0.2216(4) 0.5814(3) -0.09026(19) 0.0366(10) Uani 1 1 d U . .
O3 O 0.3709(3) 0.6962(3) 0.04730(15) 0.0238(8) Uani 1 1 d U . .
C10 C 0.3203(6) 0.5667(4) -0.1895(3) 0.0356(14) Uani 1 1 d U . .
H10 H 0.2681 0.5539 -0.2014 0.043 Uiso 1 1 calc R . .
C11 C 0.2063(5) 0.4299(4) 0.1489(3) 0.0323(13) Uani 1 1 d U . .
F2 F 0.1747(3) 1.1416(3) 0.1129(2) 0.0574(12) Uani 1 1 d U . .
C14 C 0.3320(5) 0.4614(5) 0.5082(3) 0.0344(13) Uani 1 1 d U . .
H14 H 0.3285 0.5180 0.5250 0.041 Uiso 1 1 calc R . .
C15 C 0.2193(6) 0.4869(5) 0.3415(3) 0.0421(16) Uani 1 1 d U . .
H15A H 0.2336 0.4192 0.3486 0.063 Uiso 1 1 calc R . .
H15B H 0.2783 0.4994 0.3482 0.063 Uiso 1 1 calc R . .
H15C H 0.2154 0.4980 0.3023 0.063 Uiso 1 1 calc R . .
F11 F 0.3471(4) 1.0384(3) 0.2806(2) 0.0646(12) Uani 1 1 d U . .
F3 F 0.3445(4) 1.1119(3) 0.08536(19) 0.0542(11) Uani 1 1 d U . .
C19 C 0.5574(5) 0.4221(4) 0.4039(2) 0.0282(12) Uani 1 1 d U . .
H19 H 0.5827 0.3566 0.4141 0.034 Uiso 1 1 calc R . .
F5 F 0.2704(4) 0.4253(3) -0.1147(2) 0.0698(14) Uani 1 1 d U . .
C1A C 0.2214(5) 0.8305(4) 0.3929(3) 0.0299(13) Uani 1 1 d U . .
H1A H 0.1971 0.8988 0.3908 0.036 Uiso 1 1 calc R . .
O4 O 0.2961(3) 0.9934(3) 0.11198(18) 0.0329(10) Uani 1 1 d U . .
F4 F 0.1195(4) 0.5342(4) -0.1254(2) 0.0753(14) Uani 1 1 d U . .
O10 O 0.3552(4) 0.9045(3) 0.32244(18) 0.0351(10) Uani 1 1 d U . .
O2 O 0.2721(3) 0.8251(3) -0.05962(16) 0.0273(9) Uani 1 1 d U . .
N1 N 0.3758(4) 0.8716(3) 0.0113(2) 0.0264(10) Uani 1 1 d U . .
F12 F 0.2516(4) 0.9690(4) 0.2658(2) 0.0681(13) Uani 1 1 d U . .
C1H C 0.3624(4) 0.5527(4) -0.0225(2) 0.0220(11) Uani 1 1 d U . .
H1H H 0.3704 0.4956 -0.0411 0.026 Uiso 1 1 calc R . .
N2 N 0.3731(4) 0.6200(3) -0.05425(19) 0.0227(10) Uani 1 1 d U . .
F10 F 0.2084(4) 1.0474(3) 0.3449(2) 0.0658(13) Uani 1 1 d U . .
C1K C 0.3217(5) 0.9583(4) -0.0033(2) 0.0274(12) Uani 1 1 d U . .
H1K H 0.3355 1.0085 0.0093 0.033 Uiso 1 1 calc R . .
C1N C 0.4368(6) 0.9627(5) 0.3799(3) 0.0416(15) Uani 1 1 d U . .
H1N H 0.4502 1.0037 0.3519 0.050 Uiso 1 1 calc R . .
C1O C 0.4713(5) 0.6071(4) -0.1544(3) 0.0312(13) Uani 1 1 d U . .
H1O H 0.5227 0.6221 -0.1431 0.037 Uiso 1 1 calc R . .
C1P C 0.0484(5) 1.2367(5) -0.0765(3) 0.0431(15) Uani 1 1 d U . .
C1Q C 0.7830(5) 0.6556(5) 0.2500(3) 0.0362(14) Uani 1 1 d U . .
H1QA H 0.7990 0.6129 0.2169 0.054 Uiso 1 1 calc R . .
H1QB H 0.8460 0.6307 0.2663 0.054 Uiso 1 1 calc R . .
H1QC H 0.7677 0.7217 0.2388 0.054 Uiso 1 1 calc R . .
F6 F 0.1378(4) 0.5020(4) -0.0426(2) 0.0674(13) Uani 1 1 d U . .
O8 O 0.2613(3) 0.6273(3) 0.40122(17) 0.0304(9) Uani 1 1 d U . .
C1R C 0.0873(5) 1.0605(4) -0.0960(3) 0.0313(13) Uani 1 1 d U . .
H1R H 0.0337 1.0864 -0.1168 0.038 Uiso 1 1 calc R . .
O6 O 0.3635(4) 0.6530(3) 0.48819(17) 0.0363(10) Uani 1 1 d U . .
C1T C 0.2367(5) 0.8063(4) 0.1602(3) 0.0338(14) Uani 1 1 d U . .
H1TA H 0.2620 0.8205 0.1215 0.051 Uiso 1 1 calc R . .
H1TB H 0.2371 0.8523 0.1868 0.051 Uiso 1 1 calc R . .
H1TC H 0.1625 0.8128 0.1662 0.051 Uiso 1 1 calc R . .
F1 F 0.2697(4) 1.1100(3) 0.17273(18) 0.0599(12) Uani 1 1 d U . .
C1V C 0.2599(5) 0.4938(4) 0.1203(2) 0.0256(12) Uani 1 1 d U . .
C1W C 0.6837(5) 0.6577(4) 0.2939(3) 0.0306(12) Uani 1 1 d U . .
C1X C 0.4745(6) 0.9126(5) 0.1320(3) 0.0418(15) Uani 1 1 d U . .
H1X H 0.4470 0.9532 0.1660 0.050 Uiso 1 1 calc R . .
C1Y C 0.8018(5) 0.4767(4) 0.2983(3) 0.0300(13) Uani 1 1 d U . .
H1Y H 0.8595 0.4861 0.2735 0.036 Uiso 1 1 calc R . .
C1Z C 0.2765(5) 0.3576(5) 0.1843(3) 0.0395(15) Uani 1 1 d U . .
H1ZA H 0.2973 0.3923 0.2083 0.059 Uiso 1 1 calc R . .
H1ZB H 0.3422 0.3076 0.1592 0.059 Uiso 1 1 calc R . .
H1ZC H 0.2348 0.3265 0.2080 0.059 Uiso 1 1 calc R . .
C21 C -0.1167(6) 0.9008(6) 0.3343(4) 0.0524(17) Uani 1 1 d U . .
C22 C 0.5809(6) 0.8433(5) 0.1172(3) 0.0439(16) Uani 1 1 d U . .
H22 H 0.6276 0.8367 0.1408 0.053 Uiso 1 1 calc R . .
C23 C 0.3106(5) 0.5809(4) -0.1318(3) 0.0302(13) Uani 1 1 d U . .
C24 C 0.3847(5) 0.6017(4) -0.1144(2) 0.0243(11) Uani 1 1 d U . .
C25 C 0.4080(5) 0.9227(4) 0.0969(3) 0.0327(13) Uani 1 1 d U . .
N4 N 0.3156(4) 0.7813(4) 0.4046(2) 0.0298(11) Uani 1 1 d U . .
C27 C 0.4453(5) 0.8645(4) 0.0475(3) 0.0298(12) Uani 1 1 d U . .
C28 C 0.3398(4) 0.5572(4) 0.0373(2) 0.0215(11) Uani 1 1 d U . .
C29 C 0.1100(6) 0.5567(5) 0.3817(3) 0.0368(13) Uani 1 1 d U . .
C2A C 0.3922(5) 0.4274(4) 0.4540(2) 0.0302(12) Uani 1 1 d U . .
C13 C 0.3918(5) 0.3478(4) 0.4294(2) 0.0321(13) Uani 1 1 d U . .
C1L C 0.1393(5) 0.9592(4) -0.0947(2) 0.0283(12) Uani 1 1 d U . .
C1M C 0.1715(5) 0.6926(4) 0.3867(2) 0.0279(12) Uani 1 1 d U . .
C2B C 0.3667(5) 0.8429(4) 0.4126(3) 0.0300(12) Uani 1 1 d U . .
C2C C 0.3006(4) 0.4900(4) 0.0625(2) 0.0241(11) Uani 1 1 d U . .
H2C H 0.3024 0.4411 0.0390 0.029 Uiso 1 1 calc R . .
C2D C 0.3843(5) 0.9057(4) 0.3734(3) 0.0337(13) Uani 1 1 d U . .
C2E C 0.1079(5) 1.1275(4) -0.0688(3) 0.0330(13) Uani 1 1 d U . .
C2F C 0.9459(6) 0.1981(5) 0.3054(3) 0.0476(17) Uani 1 1 d U . .
H2FA H 0.9298 0.1968 0.3466 0.071 Uiso 1 1 calc R . .
H2FB H 1.0187 0.1463 0.2885 0.071 Uiso 1 1 calc R . .
H2FC H 0.8917 0.1877 0.2917 0.071 Uiso 1 1 calc R . .
C2G C 0.2737(6) 1.0854(5) 0.1208(3) 0.0456(15) Uani 1 1 d U . .
C2H C 0.4522(6) 0.8947(5) 0.4704(3) 0.0449(16) Uani 1 1 d U . .
H2H H 0.4742 0.8921 0.5043 0.054 Uiso 1 1 calc R . .
C2I C 0.3415(4) 0.6280(4) 0.0704(2) 0.0222(11) Uani 1 1 d U . .
C2J C 0.6162(5) 0.5421(4) 0.3532(2) 0.0291(12) Uani 1 1 d U . .
C2K C 0.5860(5) 0.6991(5) 0.2663(2) 0.0329(14) Uani 1 1 d U . .
H2KA H 0.5207 0.7018 0.2935 0.049 Uiso 1 1 calc R . .
H2KB H 0.6028 0.6566 0.2330 0.049 Uiso 1 1 calc R . .
H2KC H 0.5730 0.7648 0.2551 0.049 Uiso 1 1 calc R . .
C2L C 0.2200(4) 0.9224(4) -0.0633(2) 0.0260(12) Uani 1 1 d U . .
C2N C 0.0577(5) 0.8596(5) 0.3663(3) 0.0345(14) Uani 1 1 d U . .
H2N H 0.0462 0.9256 0.3638 0.041 Uiso 1 1 calc R . .
C2O C 0.2753(6) 0.4113(5) 0.5387(3) 0.0410(15) Uani 1 1 d U . .
H2O H 0.2370 0.4317 0.5772 0.049 Uiso 1 1 calc R . .
C2P C 0.1505(5) 0.7906(4) 0.3827(2) 0.0285(12) Uani 1 1 d U . .
C2Q C 0.0958(5) 0.6612(4) 0.3750(2) 0.0287(12) Uani 1 1 d U . .
C2R C 0.1883(5) 1.0881(4) -0.0400(3) 0.0326(13) Uani 1 1 d U . .
H2R H 0.2071 1.1299 -0.0220 0.039 Uiso 1 1 calc R . .
C2 C 0.4036(6) 0.8368(5) 0.4612(3) 0.0404(15) Uani 1 1 d U . .
H2 H 0.3953 0.7926 0.4882 0.048 Uiso 1 1 calc R . .
C2S C 0.5529(5) 0.7947(5) 0.0339(3) 0.0378(14) Uani 1 1 d U . .
H2S H 0.5809 0.7538 0.0000 0.045 Uiso 1 1 calc R . .
C2T C 0.2417(5) 0.9881(4) -0.0371(2) 0.0280(12) Uani 1 1 d U . .
C2U C 0.6204(5) 0.7836(5) 0.0689(3) 0.0401(15) Uani 1 1 d U . .
H2U H 0.6937 0.7348 0.0593 0.048 Uiso 1 1 calc R . .
C2V C 0.0063(5) 0.7319(5) 0.3596(3) 0.0346(14) Uani 1 1 d U . .
H2V H -0.0446 0.7119 0.3521 0.042 Uiso 1 1 calc R . .
C2W C 0.3128(5) 0.7017(4) 0.1698(3) 0.0303(12) Uani 1 1 d U . .
C2X C 0.1131(5) 0.8929(4) -0.1268(3) 0.0283(12) Uani 1 1 d U . .
C2Y C 0.2676(4) 0.5633(4) 0.1529(2) 0.0248(12) Uani 1 1 d U . .
H2Y H 0.2439 0.5649 0.1928 0.030 Uiso 1 1 calc R . .
C2Z C 0.3325(6) 0.2996(5) 0.4586(3) 0.0402(15) Uani 1 1 d U . .
H2Z H 0.3319 0.2454 0.4413 0.048 Uiso 1 1 calc R . .
C30 C -0.0166(5) 0.8317(5) 0.3539(3) 0.0377(14) Uani 1 1 d U . .
C31 C 0.6607(5) 0.7287(4) 0.3435(3) 0.0316(13) Uani 1 1 d U . .
H31A H 0.7238 0.7046 0.3597 0.047 Uiso 1 1 calc R . .
H31B H 0.5964 0.7335 0.3724 0.047 Uiso 1 1 calc R . .
H31C H 0.6474 0.7933 0.3299 0.047 Uiso 1 1 calc R . .
C32 C 0.3071(4) 0.6289(4) 0.1309(2) 0.0244(11) Uani 1 1 d U . .
C33 C 0.2152(5) 0.8344(5) -0.1754(3) 0.0357(14) Uani 1 1 d U . .
H33A H 0.2380 0.8797 -0.1979 0.054 Uiso 1 1 calc R . .
H33B H 0.1974 0.7972 -0.1995 0.054 Uiso 1 1 calc R . .
H33C H 0.2746 0.7894 -0.1596 0.054 Uiso 1 1 calc R . .
C34 C 0.8252(5) 0.3828(4) 0.3142(3) 0.0287(12) Uani 1 1 d U . .
C35 C 0.6384(5) 0.4479(4) 0.3698(2) 0.0284(12) Uani 1 1 d U . .
C36 C 0.9420(6) 0.2981(5) 0.2889(3) 0.0396(14) Uani 1 1 d U . .
C37 C 0.7006(5) 0.5593(4) 0.3153(2) 0.0259(12) Uani 1 1 d U . .
C38 C 0.4682(6) 0.9551(5) 0.4308(3) 0.0471(16) Uani 1 1 d U . .
H38 H 0.5021 0.9939 0.4377 0.056 Uiso 1 1 calc R . .
C39 C 0.7429(5) 0.3701(4) 0.3502(3) 0.0302(13) Uani 1 1 d U . .
H39 H 0.7561 0.3070 0.3625 0.036 Uiso 1 1 calc R . .
C3A C 0.1863(7) 0.5141(6) -0.0942(4) 0.0510(16) Uani 1 1 d U . .
C3B C 0.4325(5) 0.6879(5) 0.1576(3) 0.0340(14) Uani 1 1 d U . .
H3BA H 0.4584 0.6958 0.1176 0.051 Uiso 1 1 calc R . .
H3BB H 0.4790 0.6225 0.1666 0.051 Uiso 1 1 calc R . .
H3BC H 0.4355 0.7369 0.1809 0.051 Uiso 1 1 calc R . .
C3C C 0.2760(6) 0.6879(5) 0.2322(3) 0.0415(16) Uani 1 1 d U . .
H3CA H 0.3187 0.6202 0.2396 0.062 Uiso 1 1 calc R . .
H3CB H 0.1986 0.7029 0.2419 0.062 Uiso 1 1 calc R . .
H3CC H 0.2873 0.7318 0.2553 0.062 Uiso 1 1 calc R . .
C3D C 0.2749(6) 0.3339(5) 0.5137(3) 0.0431(16) Uani 1 1 d U . .
H3D H 0.2339 0.3025 0.5346 0.052 Uiso 1 1 calc R . .
C3E C 0.0787(5) 0.8254(5) -0.0876(3) 0.0365(15) Uani 1 1 d U . .
H3EA H 0.1416 0.7778 -0.0751 0.055 Uiso 1 1 calc R . .
H3EB H 0.0515 0.7911 -0.1079 0.055 Uiso 1 1 calc R . .
H3EC H 0.0210 0.8642 -0.0546 0.055 Uiso 1 1 calc R . .
C3G C 0.0193(5) 0.9537(5) -0.1552(3) 0.0414(16) Uani 1 1 d U . .
H3GA H 0.0021 0.9096 -0.1744 0.062 Uiso 1 1 calc R . .
H3GB H 0.0422 0.9935 -0.1827 0.062 Uiso 1 1 calc R . .
H3GC H -0.0455 0.9964 -0.1263 0.062 Uiso 1 1 calc R . .
C3H C 0.2916(6) 0.9889(5) 0.3054(3) 0.0458(15) Uani 1 1 d U . .
C3I C 0.0194(6) 0.5432(5) 0.3651(3) 0.0500(18) Uani 1 1 d U . .
H3IA H 0.0230 0.4794 0.3756 0.075 Uiso 1 1 calc R . .
H3IB H 0.0286 0.5467 0.3243 0.075 Uiso 1 1 calc R . .
H3IC H -0.0515 0.5948 0.3848 0.075 Uiso 1 1 calc R . .
C3J C 0.0928(5) 0.4954(5) 0.1874(3) 0.0389(15) Uani 1 1 d U . .
H3JA H 0.1004 0.5350 0.2149 0.058 Uiso 1 1 calc R . .
H3JB H 0.0600 0.4543 0.2072 0.058 Uiso 1 1 calc R . .
H3JC H 0.0460 0.5383 0.1643 0.058 Uiso 1 1 calc R . .
C3K C -0.0742(6) 1.2689(5) -0.0640(4) 0.0508(18) Uani 1 1 d U . .
H3KA H -0.0886 1.2305 -0.0892 0.076 Uiso 1 1 calc R . .
H3KB H -0.1111 1.3383 -0.0701 0.076 Uiso 1 1 calc R . .
H3KC H -0.1016 1.2585 -0.0247 0.076 Uiso 1 1 calc R . .
C3M C 0.9668(6) 0.2960(5) 0.2252(3) 0.0444(16) Uani 1 1 d U . .
H3MA H 1.0386 0.2424 0.2089 0.067 Uiso 1 1 calc R . .
H3MB H 0.9665 0.3580 0.2130 0.067 Uiso 1 1 calc R . .
H3MC H 0.9112 0.2862 0.2124 0.067 Uiso 1 1 calc R . .
C3N C 0.1069(6) 0.5324(5) 0.4420(3) 0.0468(17) Uani 1 1 d U . .
H3NA H 0.1177 0.4647 0.4455 0.070 Uiso 1 1 calc R . .
H3NB H 0.0360 0.5762 0.4665 0.070 Uiso 1 1 calc R . .
H3NC H 0.1648 0.5403 0.4533 0.070 Uiso 1 1 calc R . .
C3O C -0.1101(7) 0.8596(6) 0.2768(4) 0.061(2) Uani 1 1 d U . .
H3OA H -0.1134 0.7968 0.2809 0.091 Uiso 1 1 calc R . .
H3OB H -0.0414 0.8504 0.2502 0.091 Uiso 1 1 calc R . .
H3OC H -0.1714 0.9054 0.2625 0.091 Uiso 1 1 calc R . .
C3P C 0.4806(6) 0.5901(5) -0.2108(3) 0.0393(15) Uani 1 1 d U . .
H3P H 0.5408 0.5914 -0.2381 0.047 Uiso 1 1 calc R . .
C3Q C -0.2206(7) 0.9079(7) 0.3758(4) 0.069(2) Uani 1 1 d U . .
H3QA H -0.2148 0.8422 0.3821 0.103 Uiso 1 1 calc R . .
H3QB H -0.2832 0.9452 0.3601 0.103 Uiso 1 1 calc R . .
H3QC H -0.2306 0.9408 0.4116 0.103 Uiso 1 1 calc R . .
C3R C 0.4067(6) 0.5715(5) -0.2286(3) 0.0398(15) Uani 1 1 d U . .
H3R H 0.4145 0.5618 -0.2678 0.048 Uiso 1 1 calc R . .
C3T C 0.1902(6) 0.3715(5) 0.1065(3) 0.0447(16) Uani 1 1 d U . .
H3TA H 0.1456 0.4161 0.0831 0.067 Uiso 1 1 calc R . .
H3TB H 0.1533 0.3336 0.1265 0.067 Uiso 1 1 calc R . .
H3TC H 0.2612 0.3271 0.0824 0.067 Uiso 1 1 calc R . .
C9 C 1.0261(6) 0.3142(6) 0.3103(4) 0.0541(19) Uani 1 1 d U . .
H9A H 1.0351 0.3700 0.2931 0.081 Uiso 1 1 calc R . .
H9B H 1.0960 0.2557 0.3003 0.081 Uiso 1 1 calc R . .
H9C H 1.0015 0.3272 0.3515 0.081 Uiso 1 1 calc R . .
C16 C 0.0577(7) 1.2998(5) -0.0296(4) 0.063(2) Uani 1 1 d U . .
H16A H 0.0169 1.2928 0.0076 0.095 Uiso 1 1 calc R . .
H16B H 0.0274 1.3686 -0.0377 0.095 Uiso 1 1 calc R . .
H16C H 0.1345 1.2767 -0.0298 0.095 Uiso 1 1 calc R . .
C2M C -0.1237(7) 1.0023(6) 0.3281(4) 0.062(2) Uani 1 1 d U . .
H2MA H -0.1856 1.0426 0.3126 0.093 Uiso 1 1 calc R . .
H2MB H -0.0562 0.9984 0.3025 0.093 Uiso 1 1 calc R . .
H2MC H -0.1337 1.0317 0.3651 0.093 Uiso 1 1 calc R . .
C3F C 0.0993(8) 1.2573(7) -0.1301(4) 0.088(3) Uani 1 1 d U . .
H3FA H 0.0669 1.2475 -0.1590 0.132 Uiso 1 1 calc R . .
H3FB H 0.1775 1.2135 -0.1397 0.132 Uiso 1 1 calc R . .
H3FC H 0.0885 1.3252 -0.1284 0.132 Uiso 1 1 calc R . .
O9 O 0.4498(4) 0.3217(3) 0.37126(18) 0.0388(10) Uani 1 1 d U . .
F9 F 0.5741(5) 0.2233(3) 0.3028(2) 0.0756(15) Uani 1 1 d U . .
F7 F 0.5715(6) 0.1800(4) 0.3880(3) 0.117(2) Uani 1 1 d U . .
F8 F 0.4571(7) 0.1803(5) 0.3491(3) 0.121(2) Uani 1 1 d U . .
C6 C 0.5108(9) 0.2293(7) 0.3539(4) 0.073(2) Uani 1 1 d U . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
V1 O1 1.605(4) . ?
V1 O2 1.904(4) . ?
V1 O3 1.913(4) . ?
V1 N2 2.125(5) . ?
V1 N1 2.134(5) . ?
V2 O6 1.603(4) . ?
V2 O7 1.913(4) . ?
V2 O8 1.917(4) . ?
V2 N4 2.118(5) . ?
V2 N3 2.134(5) . ?
N3 C19 1.299(8) . ?
N3 C2A 1.457(8) . ?
O7 C2J 1.338(7) . ?
O5 C3A 1.338(8) . ?
O5 C23 1.405(8) . ?
O3 C2I 1.338(6) . ?
C10 C3R 1.380(10) . ?
C10 C23 1.404(8) . ?
C10 H10 0.9500 . ?
C11 C3T 1.517(9) . ?
C11 C1V 1.530(8) . ?
C11 C1Z 1.530(9) . ?
C11 C3J 1.545(8) . ?
F2 C2G 1.340(8) . ?
C14 C2A 1.370(9) . ?
C14 C2O 1.406(9) . ?
C14 H14 0.9500 . ?
C15 C29 1.545(9) . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
F11 C3H 1.342(8) . ?
F3 C2G 1.347(9) . ?
C19 C35 1.434(8) . ?
C19 H19 0.9500 . ?
F5 C3A 1.364(9) . ?
C1A N4 1.308(8) . ?
C1A C2P 1.449(8) . ?
C1A H1A 0.9500 . ?
O4 C2G 1.313(8) . ?
O4 C25 1.432(7) . ?
F4 C3A 1.285(9) . ?
O10 C3H 1.331(8) . ?
O10 C2D 1.413(7) . ?
O2 C2L 1.351(6) . ?
N1 C1K 1.296(7) . ?
N1 C27 1.445(8) . ?
F12 C3H 1.340(8) . ?
C1H N2 1.302(7) . ?
C1H C28 1.420(8) . ?
C1H H1H 0.9500 . ?
N2 C24 1.468(7) . ?
F10 C3H 1.307(9) . ?
C1K C2T 1.465(8) . ?
C1K H1K 0.9500 . ?
C1N C2D 1.400(9) . ?
C1N C38 1.408(10) . ?
C1N H1N 0.9500 . ?
C1O C3P 1.381(9) . ?
C1O C24 1.398(8) . ?
C1O H1O 0.9500 . ?
C1P C3F 1.429(11) . ?
C1P C3K 1.528(10) . ?
C1P C2E 1.533(8) . ?
C1P C16 1.596(11) . ?
C1Q C1W 1.529(9) . ?
C1Q H1QA 0.9800 . ?
C1Q H1QB 0.9800 . ?
C1Q H1QC 0.9800 . ?
F6 C3A 1.329(9) . ?
O8 C1M 1.347(7) . ?
C1R C1L 1.397(8) . ?
C1R C2E 1.409(9) . ?
C1R H1R 0.9500 . ?
C1T C2W 1.534(8) . ?
C1T H1TA 0.9800 . ?
C1T H1TB 0.9800 . ?
C1T H1TC 0.9800 . ?
F1 C2G 1.324(8) . ?
C1V C2C 1.387(8) . ?
C1V C2Y 1.410(8) . ?
C1W C37 1.509(8) . ?
C1W C31 1.538(8) . ?
C1W C2K 1.555(8) . ?
C1X C22 1.371(10) . ?
C1X C25 1.382(9) . ?
C1X H1X 0.9500 . ?
C1Y C34 1.387(8) . ?
C1Y C37 1.407(8) . ?
C1Y H1Y 0.9500 . ?
C1Z H1ZA 0.9800 . ?
C1Z H1ZB 0.9800 . ?
C1Z H1ZC 0.9800 . ?
C21 C2M 1.515(11) . ?
C21 C3Q 1.526(11) . ?
C21 C30 1.526(10) . ?
C21 C3O 1.533(12) . ?
C22 C2U 1.366(10) . ?
C22 H22 0.9500 . ?
C23 C24 1.376(8) . ?
C25 C27 1.378(9) . ?
N4 C2B 1.456(8) . ?
C27 C2S 1.385(8) . ?
C28 C2I 1.391(8) . ?
C28 C2C 1.419(8) . ?
C29 C3N 1.506(9) . ?
C29 C2Q 1.526(8) . ?
C29 C3I 1.527(10) . ?
C2A C13 1.383(9) . ?
C13 C2Z 1.396(9) . ?
C13 O9 1.431(7) . ?
C1L C2L 1.429(8) . ?
C1L C2X 1.522(8) . ?
C1M C2P 1.397(8) . ?
C1M C2Q 1.434(8) . ?
C2B C2D 1.386(9) . ?
C2B C2 1.398(9) . ?
C2C H2C 0.9500 . ?
C2E C2R 1.382(9) . ?
C2F C36 1.546(9) . ?
C2F H2FA 0.9800 . ?
C2F H2FB 0.9800 . ?
C2F H2FC 0.9800 . ?
C2H C38 1.359(10) . ?
C2H C2 1.387(9) . ?
C2H H2H 0.9500 . ?
C2I C32 1.443(8) . ?
C2J C35 1.398(8) . ?
C2J C37 1.434(8) . ?
C2K H2KA 0.9800 . ?
C2K H2KB 0.9800 . ?
C2K H2KC 0.9800 . ?
C2L C2T 1.389(8) . ?
C2N C30 1.389(9) . ?
C2N C2P 1.416(9) . ?
C2N H2N 0.9500 . ?
C2O C3D 1.357(10) . ?
C2O H2O 0.9500 . ?
C2Q C2V 1.383(9) . ?
C2R C2T 1.385(8) . ?
C2R H2R 0.9500 . ?
C2 H2 0.9500 . ?
C2S C2U 1.385(9) . ?
C2S H2S 0.9500 . ?
C2U H2U 0.9500 . ?
C2V C30 1.422(9) . ?
C2V H2V 0.9500 . ?
C2W C3C 1.529(9) . ?
C2W C32 1.535(8) . ?
C2W C3B 1.558(8) . ?
C2X C3E 1.532(8) . ?
C2X C33 1.553(9) . ?
C2X C3G 1.559(8) . ?
C2Y C32 1.378(8) . ?
C2Y H2Y 0.9500 . ?
C2Z C3D 1.380(9) . ?
C2Z H2Z 0.9500 . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C34 C39 1.355(9) . ?
C34 C36 1.573(9) . ?
C35 C39 1.409(8) . ?
C36 C3M 1.513(10) . ?
C36 C9 1.522(10) . ?
C38 H38 0.9500 . ?
C39 H39 0.9500 . ?
C3B H3BA 0.9800 . ?
C3B H3BB 0.9800 . ?
C3B H3BC 0.9800 . ?
C3C H3CA 0.9800 . ?
C3C H3CB 0.9800 . ?
C3C H3CC 0.9800 . ?
C3D H3D 0.9500 . ?
C3E H3EA 0.9800 . ?
C3E H3EB 0.9800 . ?
C3E H3EC 0.9800 . ?
C3G H3GA 0.9800 . ?
C3G H3GB 0.9800 . ?
C3G H3GC 0.9800 . ?
C3I H3IA 0.9800 . ?
C3I H3IB 0.9800 . ?
C3I H3IC 0.9800 . ?
C3J H3JA 0.9800 . ?
C3J H3JB 0.9800 . ?
C3J H3JC 0.9800 . ?
C3K H3KA 0.9800 . ?
C3K H3KB 0.9800 . ?
C3K H3KC 0.9800 . ?
C3M H3MA 0.9800 . ?
C3M H3MB 0.9800 . ?
C3M H3MC 0.9800 . ?
C3N H3NA 0.9800 . ?
C3N H3NB 0.9800 . ?
C3N H3NC 0.9800 . ?
C3O H3OA 0.9800 . ?
C3O H3OB 0.9800 . ?
C3O H3OC 0.9800 . ?
C3P C3R 1.362(10) . ?
C3P H3P 0.9500 . ?
C3Q H3QA 0.9800 . ?
C3Q H3QB 0.9800 . ?
C3Q H3QC 0.9800 . ?
C3R H3R 0.9500 . ?
C3T H3TA 0.9800 . ?
C3T H3TB 0.9800 . ?
C3T H3TC 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C2M H2MA 0.9800 . ?
C2M H2MB 0.9800 . ?
C2M H2MC 0.9800 . ?
C3F H3FA 0.9800 . ?
C3F H3FB 0.9800 . ?
C3F H3FC 0.9800 . ?
O9 C6 1.312(10) . ?
F9 C6 1.327(10) . ?
F7 C6 1.320(12) . ?
F8 C6 1.300(12) . ?

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 114.7(2) . . ?
O1 V1 O3 118.20(19) . . ?
O2 V1 O3 127.08(17) . . ?
O1 V1 N2 96.4(2) . . ?
O2 V1 N2 89.19(17) . . ?
O3 V1 N2 86.87(17) . . ?
O1 V1 N1 92.5(2) . . ?
O2 V1 N1 88.27(18) . . ?
O3 V1 N1 87.77(18) . . ?
N2 V1 N1 170.99(18) . . ?
O6 V2 O7 116.8(2) . . ?
O6 V2 O8 115.2(2) . . ?
O7 V2 O8 128.02(18) . . ?
O6 V2 N4 95.5(2) . . ?
O7 V2 N4 88.10(19) . . ?
O8 V2 N4 87.05(19) . . ?
O6 V2 N3 95.4(2) . . ?
O7 V2 N3 86.48(19) . . ?
O8 V2 N3 88.86(19) . . ?
N4 V2 N3 169.10(19) . . ?
C19 N3 C2A 114.3(5) . . ?
C19 N3 V2 123.6(4) . . ?
C2A N3 V2 121.2(4) . . ?
C2J O7 V2 136.4(4) . . ?
C3A O5 C23 120.1(5) . . ?
C2I O3 V1 134.0(4) . . ?
C3R C10 C23 119.2(6) . . ?
C3R C10 H10 120.4 . . ?
C23 C10 H10 120.4 . . ?
C3T C11 C1V 112.1(5) . . ?
C3T C11 C1Z 107.7(5) . . ?
C1V C11 C1Z 110.6(5) . . ?
C3T C11 C3J 107.5(5) . . ?
C1V C11 C3J 109.4(5) . . ?
C1Z C11 C3J 109.4(5) . . ?
C2A C14 C2O 119.0(6) . . ?
C2A C14 H14 120.5 . . ?
C2O C14 H14 120.5 . . ?
C29 C15 H15A 109.5 . . ?
C29 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C29 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
N3 C19 C35 127.8(5) . . ?
N3 C19 H19 116.1 . . ?
C35 C19 H19 116.1 . . ?
N4 C1A C2P 126.2(6) . . ?
N4 C1A H1A 116.9 . . ?
C2P C1A H1A 116.9 . . ?
C2G O4 C25 118.6(5) . . ?
C3H O10 C2D 118.4(5) . . ?
C2L O2 V1 134.3(4) . . ?
C1K N1 C27 115.7(5) . . ?
C1K N1 V1 122.8(4) . . ?
C27 N1 V1 120.5(4) . . ?
N2 C1H C28 125.8(5) . . ?
N2 C1H H1H 117.1 . . ?
C28 C1H H1H 117.1 . . ?
C1H N2 C24 114.8(5) . . ?
C1H N2 V1 125.2(4) . . ?
C24 N2 V1 119.9(3) . . ?
N1 C1K C2T 127.7(5) . . ?
N1 C1K H1K 116.1 . . ?
C2T C1K H1K 116.1 . . ?
C2D C1N C38 115.3(7) . . ?
C2D C1N H1N 122.3 . . ?
C38 C1N H1N 122.3 . . ?
C3P C1O C24 118.5(6) . . ?
C3P C1O H1O 120.8 . . ?
C24 C1O H1O 120.8 . . ?
C3F C1P C3K 116.7(7) . . ?
C3F C1P C2E 109.3(6) . . ?
C3K C1P C2E 110.2(6) . . ?
C3F C1P C16 107.1(8) . . ?
C3K C1P C16 102.9(6) . . ?
C2E C1P C16 110.3(6) . . ?
C1W C1Q H1QA 109.5 . . ?
C1W C1Q H1QB 109.5 . . ?
H1QA C1Q H1QB 109.5 . . ?
C1W C1Q H1QC 109.5 . . ?
H1QA C1Q H1QC 109.5 . . ?
H1QB C1Q H1QC 109.5 . . ?
C1M O8 V2 135.5(4) . . ?
C1L C1R C2E 125.3(6) . . ?
C1L C1R H1R 117.4 . . ?
C2E C1R H1R 117.4 . . ?
C2W C1T H1TA 109.5 . . ?
C2W C1T H1TB 109.5 . . ?
H1TA C1T H1TB 109.5 . . ?
C2W C1T H1TC 109.5 . . ?
H1TA C1T H1TC 109.5 . . ?
H1TB C1T H1TC 109.5 . . ?
C2C C1V C2Y 116.0(5) . . ?
C2C C1V C11 123.8(5) . . ?
C2Y C1V C11 120.2(5) . . ?
C37 C1W C1Q 113.5(5) . . ?
C37 C1W C31 109.3(5) . . ?
C1Q C1W C31 106.7(5) . . ?
C37 C1W C2K 110.6(5) . . ?
C1Q C1W C2K 107.4(5) . . ?
C31 C1W C2K 109.3(5) . . ?
C22 C1X C25 119.1(7) . . ?
C22 C1X H1X 120.4 . . ?
C25 C1X H1X 120.4 . . ?
C34 C1Y C37 126.1(6) . . ?
C34 C1Y H1Y 116.9 . . ?
C37 C1Y H1Y 116.9 . . ?
C11 C1Z H1ZA 109.5 . . ?
C11 C1Z H1ZB 109.5 . . ?
H1ZA C1Z H1ZB 109.5 . . ?
C11 C1Z H1ZC 109.5 . . ?
H1ZA C1Z H1ZC 109.5 . . ?
H1ZB C1Z H1ZC 109.5 . . ?
C2M C21 C3Q 108.8(7) . . ?
C2M C21 C30 112.3(6) . . ?
C3Q C21 C30 110.5(7) . . ?
C2M C21 C3O 108.4(7) . . ?
C3Q C21 C3O 108.2(7) . . ?
C30 C21 C3O 108.6(7) . . ?
C2U C22 C1X 120.6(6) . . ?
C2U C22 H22 119.7 . . ?
C1X C22 H22 119.7 . . ?
C24 C23 C10 120.6(6) . . ?
C24 C23 O5 117.7(5) . . ?
C10 C23 O5 121.5(6) . . ?
C23 C24 C1O 119.7(5) . . ?
C23 C24 N2 121.0(5) . . ?
C1O C24 N2 119.3(5) . . ?
C27 C25 C1X 121.8(6) . . ?
C27 C25 O4 118.1(5) . . ?
C1X C25 O4 120.1(6) . . ?
C1A N4 C2B 112.8(5) . . ?
C1A N4 V2 125.4(4) . . ?
C2B N4 V2 121.3(4) . . ?
C25 C27 C2S 117.7(6) . . ?
C25 C27 N1 122.6(5) . . ?
C2S C27 N1 119.7(6) . . ?
C2I C28 C2C 120.6(5) . . ?
C2I C28 C1H 124.6(5) . . ?
C2C C28 C1H 114.3(5) . . ?
C3N C29 C2Q 110.3(5) . . ?
C3N C29 C3I 108.4(6) . . ?
C2Q C29 C3I 110.9(5) . . ?
C3N C29 C15 111.1(6) . . ?
C2Q C29 C15 108.6(5) . . ?
C3I C29 C15 107.5(6) . . ?
C14 C2A C13 119.6(6) . . ?
C14 C2A N3 119.3(6) . . ?
C13 C2A N3 121.2(5) . . ?
C2A C13 C2Z 121.9(6) . . ?
C2A C13 O9 116.0(5) . . ?
C2Z C13 O9 122.0(6) . . ?
C1R C1L C2L 116.2(6) . . ?
C1R C1L C2X 121.2(5) . . ?
C2L C1L C2X 122.6(5) . . ?
O8 C1M C2P 121.3(5) . . ?
O8 C1M C2Q 119.6(5) . . ?
C2P C1M C2Q 119.2(5) . . ?
C2D C2B C2 117.6(6) . . ?
C2D C2B N4 123.3(5) . . ?
C2 C2B N4 119.1(6) . . ?
C1V C2C C28 121.9(5) . . ?
C1V C2C H2C 119.1 . . ?
C28 C2C H2C 119.1 . . ?
C2B C2D C1N 123.7(6) . . ?
C2B C2D O10 116.7(5) . . ?
C1N C2D O10 119.3(6) . . ?
C2R C2E C1R 116.3(5) . . ?
C2R C2E C1P 124.1(6) . . ?
C1R C2E C1P 119.4(6) . . ?
C36 C2F H2FA 109.5 . . ?
C36 C2F H2FB 109.5 . . ?
H2FA C2F H2FB 109.5 . . ?
C36 C2F H2FC 109.5 . . ?
H2FA C2F H2FC 109.5 . . ?
H2FB C2F H2FC 109.5 . . ?
O4 C2G F1 114.1(6) . . ?
O4 C2G F2 108.9(6) . . ?
F1 C2G F2 106.0(6) . . ?
O4 C2G F3 113.2(6) . . ?
F1 C2G F3 107.0(6) . . ?
F2 C2G F3 107.2(6) . . ?
C38 C2H C2 119.8(7) . . ?
C38 C2H H2H 120.1 . . ?
C2 C2H H2H 120.1 . . ?
O3 C2I C28 121.5(5) . . ?
O3 C2I C32 120.0(5) . . ?
C28 C2I C32 118.5(5) . . ?
O7 C2J C35 120.6(6) . . ?
O7 C2J C37 120.0(5) . . ?
C35 C2J C37 119.5(5) . . ?
C1W C2K H2KA 109.5 . . ?
C1W C2K H2KB 109.5 . . ?
H2KA C2K H2KB 109.5 . . ?
C1W C2K H2KC 109.5 . . ?
H2KA C2K H2KC 109.5 . . ?
H2KB C2K H2KC 109.5 . . ?
O2 C2L C2T 122.2(5) . . ?
O2 C2L C1L 119.1(5) . . ?
C2T C2L C1L 118.7(5) . . ?
C30 C2N C2P 120.5(6) . . ?
C30 C2N H2N 119.7 . . ?
C2P C2N H2N 119.7 . . ?
C3D C2O C14 120.4(6) . . ?
C3D C2O H2O 119.8 . . ?
C14 C2O H2O 119.8 . . ?
C1M C2P C2N 121.9(6) . . ?
C1M C2P C1A 124.1(6) . . ?
C2N C2P C1A 113.9(5) . . ?
C2V C2Q C1M 116.4(5) . . ?
C2V C2Q C29 121.5(6) . . ?
C1M C2Q C29 122.1(5) . . ?
C2E C2R C2T 120.7(6) . . ?
C2E C2R H2R 119.7 . . ?
C2T C2R H2R 119.7 . . ?
C2H C2 C2B 120.6(6) . . ?
C2H C2 H2 119.7 . . ?
C2B C2 H2 119.7 . . ?
C2U C2S C27 121.1(7) . . ?
C2U C2S H2S 119.5 . . ?
C27 C2S H2S 119.5 . . ?
C2R C2T C2L 122.8(5) . . ?
C2R C2T C1K 113.9(5) . . ?
C2L C2T C1K 123.2(5) . . ?
C22 C2U C2S 119.7(6) . . ?
C22 C2U H2U 120.2 . . ?
C2S C2U H2U 120.2 . . ?
C2Q C2V C30 126.1(6) . . ?
C2Q C2V H2V 117.0 . . ?
C30 C2V H2V 117.0 . . ?
C3C C2W C1T 106.7(5) . . ?
C3C C2W C32 112.4(5) . . ?
C1T C2W C32 109.8(5) . . ?
C3C C2W C3B 107.9(5) . . ?
C1T C2W C3B 110.6(5) . . ?
C32 C2W C3B 109.5(5) . . ?
C1L C2X C3E 111.3(5) . . ?
C1L C2X C33 108.0(5) . . ?
C3E C2X C33 111.8(5) . . ?
C1L C2X C3G 110.9(5) . . ?
C3E C2X C3G 108.4(5) . . ?
C33 C2X C3G 106.3(5) . . ?
C32 C2Y C1V 124.6(5) . . ?
C32 C2Y H2Y 117.7 . . ?
C1V C2Y H2Y 117.7 . . ?
C3D C2Z C13 117.3(6) . . ?
C3D C2Z H2Z 121.4 . . ?
C13 C2Z H2Z 121.4 . . ?
C2N C30 C2V 115.9(6) . . ?
C2N C30 C21 123.8(6) . . ?
C2V C30 C21 120.3(6) . . ?
C1W C31 H31A 109.5 . . ?
C1W C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C1W C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C2Y C32 C2I 118.1(5) . . ?
C2Y C32 C2W 120.9(5) . . ?
C2I C32 C2W 120.9(5) . . ?
C2X C33 H33A 109.5 . . ?
C2X C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
C2X C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C39 C34 C1Y 116.6(6) . . ?
C39 C34 C36 124.2(5) . . ?
C1Y C34 C36 119.1(5) . . ?
C2J C35 C39 120.8(6) . . ?
C2J C35 C19 123.5(6) . . ?
C39 C35 C19 115.6(5) . . ?
C3M C36 C9 111.0(6) . . ?
C3M C36 C2F 107.1(6) . . ?
C9 C36 C2F 109.4(6) . . ?
C3M C36 C34 108.7(5) . . ?
C9 C36 C34 109.9(6) . . ?
C2F C36 C34 110.7(6) . . ?
C1Y C37 C2J 115.1(5) . . ?
C1Y C37 C1W 121.5(5) . . ?
C2J C37 C1W 123.3(5) . . ?
C2H C38 C1N 122.8(7) . . ?
C2H C38 H38 118.6 . . ?
C1N C38 H38 118.6 . . ?
C34 C39 C35 121.8(6) . . ?
C34 C39 H39 119.1 . . ?
C35 C39 H39 119.1 . . ?
F4 C3A F6 108.4(7) . . ?
F4 C3A O5 115.1(7) . . ?
F6 C3A O5 108.5(6) . . ?
F4 C3A F5 106.6(6) . . ?
F6 C3A F5 106.0(6) . . ?
O5 C3A F5 111.7(6) . . ?
C2W C3B H3BA 109.5 . . ?
C2W C3B H3BB 109.5 . . ?
H3BA C3B H3BB 109.5 . . ?
C2W C3B H3BC 109.5 . . ?
H3BA C3B H3BC 109.5 . . ?
H3BB C3B H3BC 109.5 . . ?
C2W C3C H3CA 109.5 . . ?
C2W C3C H3CB 109.5 . . ?
H3CA C3C H3CB 109.5 . . ?
C2W C3C H3CC 109.5 . . ?
H3CA C3C H3CC 109.5 . . ?
H3CB C3C H3CC 109.5 . . ?
C2O C3D C2Z 121.7(6) . . ?
C2O C3D H3D 119.1 . . ?
C2Z C3D H3D 119.1 . . ?
C2X C3E H3EA 109.5 . . ?
C2X C3E H3EB 109.5 . . ?
H3EA C3E H3EB 109.5 . . ?
C2X C3E H3EC 109.5 . . ?
H3EA C3E H3EC 109.5 . . ?
H3EB C3E H3EC 109.5 . . ?
C2X C3G H3GA 109.5 . . ?
C2X C3G H3GB 109.5 . . ?
H3GA C3G H3GB 109.5 . . ?
C2X C3G H3GC 109.5 . . ?
H3GA C3G H3GC 109.5 . . ?
H3GB C3G H3GC 109.5 . . ?
F10 C3H O10 115.0(6) . . ?
F10 C3H F12 107.2(6) . . ?
O10 C3H F12 107.9(6) . . ?
F10 C3H F11 108.0(6) . . ?
O10 C3H F11 112.4(6) . . ?
F12 C3H F11 106.0(6) . . ?
C29 C3I H3IA 109.5 . . ?
C29 C3I H3IB 109.5 . . ?
H3IA C3I H3IB 109.5 . . ?
C29 C3I H3IC 109.5 . . ?
H3IA C3I H3IC 109.5 . . ?
H3IB C3I H3IC 109.5 . . ?
C11 C3J H3JA 109.5 . . ?
C11 C3J H3JB 109.5 . . ?
H3JA C3J H3JB 109.5 . . ?
C11 C3J H3JC 109.5 . . ?
H3JA C3J H3JC 109.5 . . ?
H3JB C3J H3JC 109.5 . . ?
C1P C3K H3KA 109.5 . . ?
C1P C3K H3KB 109.5 . . ?
H3KA C3K H3KB 109.5 . . ?
C1P C3K H3KC 109.5 . . ?
H3KA C3K H3KC 109.5 . . ?
H3KB C3K H3KC 109.5 . . ?
C36 C3M H3MA 109.5 . . ?
C36 C3M H3MB 109.5 . . ?
H3MA C3M H3MB 109.5 . . ?
C36 C3M H3MC 109.5 . . ?
H3MA C3M H3MC 109.5 . . ?
H3MB C3M H3MC 109.5 . . ?
C29 C3N H3NA 109.5 . . ?
C29 C3N H3NB 109.5 . . ?
H3NA C3N H3NB 109.5 . . ?
C29 C3N H3NC 109.5 . . ?
H3NA C3N H3NC 109.5 . . ?
H3NB C3N H3NC 109.5 . . ?
C21 C3O H3OA 109.5 . . ?
C21 C3O H3OB 109.5 . . ?
H3OA C3O H3OB 109.5 . . ?
C21 C3O H3OC 109.5 . . ?
H3OA C3O H3OC 109.5 . . ?
H3OB C3O H3OC 109.5 . . ?
C3R C3P C1O 122.4(7) . . ?
C3R C3P H3P 118.8 . . ?
C1O C3P H3P 118.8 . . ?
C21 C3Q H3QA 109.5 . . ?
C21 C3Q H3QB 109.5 . . ?
H3QA C3Q H3QB 109.5 . . ?
C21 C3Q H3QC 109.5 . . ?
H3QA C3Q H3QC 109.5 . . ?
H3QB C3Q H3QC 109.5 . . ?
C3P C3R C10 119.6(6) . . ?
C3P C3R H3R 120.2 . . ?
C10 C3R H3R 120.2 . . ?
C11 C3T H3TA 109.5 . . ?
C11 C3T H3TB 109.5 . . ?
H3TA C3T H3TB 109.5 . . ?
C11 C3T H3TC 109.5 . . ?
H3TA C3T H3TC 109.5 . . ?
H3TB C3T H3TC 109.5 . . ?
C36 C9 H9A 109.5 . . ?
C36 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C36 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C1P C16 H16A 109.5 . . ?
C1P C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C1P C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C21 C2M H2MA 109.5 . . ?
C21 C2M H2MB 109.5 . . ?
H2MA C2M H2MB 109.5 . . ?
C21 C2M H2MC 109.5 . . ?
H2MA C2M H2MC 109.5 . . ?
H2MB C2M H2MC 109.5 . . ?
C1P C3F H3FA 109.5 . . ?
C1P C3F H3FB 109.5 . . ?
H3FA C3F H3FB 109.5 . . ?
C1P C3F H3FC 109.5 . . ?
H3FA C3F H3FC 109.5 . . ?
H3FB C3F H3FC 109.5 . . ?
C6 O9 C13 119.4(6) . . ?
F8 C6 O9 114.8(9) . . ?
F8 C6 F7 104.0(8) . . ?
O9 C6 F7 113.3(9) . . ?
F8 C6 F9 106.0(8) . . ?
O9 C6 F9 108.8(7) . . ?
F7 C6 F9 109.6(9) . . ?

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
O6 V2 N3 C19 -104.3(5) . . . . ?
O7 V2 N3 C19 12.3(5) . . . . ?
O8 V2 N3 C19 140.5(5) . . . . ?
N4 V2 N3 C19 72.6(12) . . . . ?
O6 V2 N3 C2A 64.1(4) . . . . ?
O7 V2 N3 C2A -179.2(4) . . . . ?
O8 V2 N3 C2A -51.0(4) . . . . ?
N4 V2 N3 C2A -119.0(10) . . . . ?
O6 V2 O7 C2J 89.9(6) . . . . ?
O8 V2 O7 C2J -90.1(5) . . . . ?
N4 V2 O7 C2J -174.9(5) . . . . ?
N3 V2 O7 C2J -4.3(5) . . . . ?
O1 V1 O3 C2I -107.9(5) . . . . ?
O2 V1 O3 C2I 74.3(5) . . . . ?
N2 V1 O3 C2I -12.4(5) . . . . ?
N1 V1 O3 C2I 160.4(5) . . . . ?
C2A N3 C19 C35 176.9(5) . . . . ?
V2 N3 C19 C35 -14.0(8) . . . . ?
O1 V1 O2 C2L -84.0(5) . . . . ?
O3 V1 O2 C2L 93.9(5) . . . . ?
N2 V1 O2 C2L 179.4(5) . . . . ?
N1 V1 O2 C2L 8.0(5) . . . . ?
O1 V1 N1 C1K 102.3(5) . . . . ?
O2 V1 N1 C1K -12.4(5) . . . . ?
O3 V1 N1 C1K -139.6(5) . . . . ?
O1 V1 N1 C27 -66.5(4) . . . . ?
O2 V1 N1 C27 178.8(4) . . . . ?
O3 V1 N1 C27 51.6(4) . . . . ?
C28 C1H N2 C24 -173.7(5) . . . . ?
C28 C1H N2 V1 10.9(8) . . . . ?
O1 V1 N2 C1H 116.7(4) . . . . ?
O2 V1 N2 C1H -128.5(4) . . . . ?
O3 V1 N2 C1H -1.3(4) . . . . ?
O1 V1 N2 C24 -58.4(4) . . . . ?
O2 V1 N2 C24 56.3(4) . . . . ?
O3 V1 N2 C24 -176.5(4) . . . . ?
C27 N1 C1K C2T -176.7(6) . . . . ?
V1 N1 C1K C2T 14.0(8) . . . . ?
O6 V2 O8 C1M 90.0(5) . . . . ?
O7 V2 O8 C1M -89.9(5) . . . . ?
N4 V2 O8 C1M -4.7(5) . . . . ?
N3 V2 O8 C1M -174.6(5) . . . . ?
C3T C11 C1V C2C -7.2(8) . . . . ?
C1Z C11 C1V C2C 113.0(6) . . . . ?
C3J C11 C1V C2C -126.3(6) . . . . ?
C3T C11 C1V C2Y 171.1(5) . . . . ?
C1Z C11 C1V C2Y -68.7(7) . . . . ?
C3J C11 C1V C2Y 51.9(7) . . . . ?
C3R C10 C23 C24 1.6(9) . . . . ?
C3R C10 C23 O5 177.0(5) . . . . ?
C3A O5 C23 C24 -140.7(6) . . . . ?
C3A O5 C23 C10 43.8(8) . . . . ?
C10 C23 C24 C1O -1.1(9) . . . . ?
O5 C23 C24 C1O -176.7(5) . . . . ?
C10 C23 C24 N2 177.9(5) . . . . ?
O5 C23 C24 N2 2.4(8) . . . . ?
C3P C1O C24 C23 -0.7(8) . . . . ?
C3P C1O C24 N2 -179.8(5) . . . . ?
C1H N2 C24 C23 52.4(7) . . . . ?
V1 N2 C24 C23 -132.0(5) . . . . ?
C1H N2 C24 C1O -128.5(6) . . . . ?
V1 N2 C24 C1O 47.1(6) . . . . ?
C22 C1X C25 C27 0.5(10) . . . . ?
C22 C1X C25 O4 178.9(6) . . . . ?
C2G O4 C25 C27 -123.8(6) . . . . ?
C2G O4 C25 C1X 57.7(8) . . . . ?
C2P C1A N4 C2B -179.8(6) . . . . ?
C2P C1A N4 V2 -8.2(9) . . . . ?
O6 V2 N4 C1A -107.5(5) . . . . ?
O7 V2 N4 C1A 135.7(5) . . . . ?
O8 V2 N4 C1A 7.5(5) . . . . ?
N3 V2 N4 C1A 75.6(12) . . . . ?
O6 V2 N4 C2B 63.5(5) . . . . ?
O7 V2 N4 C2B -53.3(4) . . . . ?
O8 V2 N4 C2B 178.5(4) . . . . ?
N3 V2 N4 C2B -113.4(11) . . . . ?
C1X C25 C27 C2S -0.1(9) . . . . ?
O4 C25 C27 C2S -178.6(5) . . . . ?
C1X C25 C27 N1 177.7(6) . . . . ?
O4 C25 C27 N1 -0.7(9) . . . . ?
C1K N1 C27 C25 52.1(8) . . . . ?
V1 N1 C27 C25 -138.4(5) . . . . ?
C1K N1 C27 C2S -130.1(6) . . . . ?
V1 N1 C27 C2S 39.4(7) . . . . ?
N2 C1H C28 C2I -9.9(9) . . . . ?
N2 C1H C28 C2C 162.3(5) . . . . ?
C2O C14 C2A C13 3.2(10) . . . . ?
C2O C14 C2A N3 -178.3(6) . . . . ?
C19 N3 C2A C14 123.0(6) . . . . ?
V2 N3 C2A C14 -46.4(7) . . . . ?
C19 N3 C2A C13 -58.5(8) . . . . ?
V2 N3 C2A C13 132.1(5) . . . . ?
C14 C2A C13 C2Z -0.9(10) . . . . ?
N3 C2A C13 C2Z -179.4(6) . . . . ?
C14 C2A C13 O9 175.2(6) . . . . ?
N3 C2A C13 O9 -3.2(9) . . . . ?
C2E C1R C1L C2L -0.3(9) . . . . ?
C2E C1R C1L C2X -178.5(6) . . . . ?
V2 O8 C1M C2P 1.7(8) . . . . ?
V2 O8 C1M C2Q -178.2(4) . . . . ?
C1A N4 C2B C2D -53.4(8) . . . . ?
V2 N4 C2B C2D 134.5(5) . . . . ?
C1A N4 C2B C2 128.8(6) . . . . ?
V2 N4 C2B C2 -43.3(7) . . . . ?
C2Y C1V C2C C28 -4.8(8) . . . . ?
C11 C1V C2C C28 173.6(5) . . . . ?
C2I C28 C2C C1V 2.0(8) . . . . ?
C1H C28 C2C C1V -170.6(5) . . . . ?
C2 C2B C2D C1N 0.1(10) . . . . ?
N4 C2B C2D C1N -177.7(6) . . . . ?
C2 C2B C2D O10 174.6(6) . . . . ?
N4 C2B C2D O10 -3.2(9) . . . . ?
C38 C1N C2D C2B -2.2(10) . . . . ?
C38 C1N C2D O10 -176.5(6) . . . . ?
C3H O10 C2D C2B 128.6(7) . . . . ?
C3H O10 C2D C1N -56.6(8) . . . . ?
C1L C1R C2E C2R 1.7(9) . . . . ?
C1L C1R C2E C1P 176.8(6) . . . . ?
C3F C1P C2E C2R 96.4(9) . . . . ?
C3K C1P C2E C2R -134.1(7) . . . . ?
C16 C1P C2E C2R -21.2(9) . . . . ?
C3F C1P C2E C1R -78.3(9) . . . . ?
C3K C1P C2E C1R 51.2(8) . . . . ?
C16 C1P C2E C1R 164.1(6) . . . . ?
C25 O4 C2G F1 -85.2(8) . . . . ?
C25 O4 C2G F2 156.7(5) . . . . ?
C25 O4 C2G F3 37.6(8) . . . . ?
V1 O3 C2I C28 16.2(8) . . . . ?
V1 O3 C2I C32 -161.6(4) . . . . ?
C2C C28 C2I O3 -175.3(5) . . . . ?
C1H C28 C2I O3 -3.5(8) . . . . ?
C2C C28 C2I C32 2.6(8) . . . . ?
C1H C28 C2I C32 174.4(5) . . . . ?
V2 O7 C2J C35 -3.7(9) . . . . ?
V2 O7 C2J C37 178.1(4) . . . . ?
V1 O2 C2L C2T -3.5(8) . . . . ?
V1 O2 C2L C1L 177.0(4) . . . . ?
C1R C1L C2L O2 178.9(5) . . . . ?
C2X C1L C2L O2 -3.0(9) . . . . ?
C1R C1L C2L C2T -0.6(8) . . . . ?
C2X C1L C2L C2T 177.5(5) . . . . ?
C2A C14 C2O C3D -4.0(10) . . . . ?
O8 C1M C2P C2N 178.6(5) . . . . ?
C2Q C1M C2P C2N -1.5(9) . . . . ?
O8 C1M C2P C1A 0.8(9) . . . . ?
C2Q C1M C2P C1A -179.3(6) . . . . ?
C30 C2N C2P C1M 0.6(10) . . . . ?
C30 C2N C2P C1A 178.6(6) . . . . ?
N4 C1A C2P C1M 3.1(10) . . . . ?
N4 C1A C2P C2N -174.9(6) . . . . ?
O8 C1M C2Q C2V -179.2(5) . . . . ?
C2P C1M C2Q C2V 0.9(8) . . . . ?
O8 C1M C2Q C29 3.5(8) . . . . ?
C2P C1M C2Q C29 -176.4(5) . . . . ?
C3N C29 C2Q C2V -115.9(7) . . . . ?
C3I C29 C2Q C2V 4.2(9) . . . . ?
C15 C29 C2Q C2V 122.1(6) . . . . ?
C3N C29 C2Q C1M 61.3(8) . . . . ?
C3I C29 C2Q C1M -178.6(6) . . . . ?
C15 C29 C2Q C1M -60.6(7) . . . . ?
C1R C2E C2R C2T -2.1(9) . . . . ?
C1P C2E C2R C2T -177.0(6) . . . . ?
C38 C2H C2 C2B -2.7(11) . . . . ?
C2D C2B C2 C2H 2.4(10) . . . . ?
N4 C2B C2 C2H -179.7(6) . . . . ?
C25 C27 C2S C2U 0.4(10) . . . . ?
N1 C27 C2S C2U -177.5(6) . . . . ?
C2E C2R C2T C2L 1.3(10) . . . . ?
C2E C2R C2T C1K -177.9(6) . . . . ?
O2 C2L C2T C2R -179.4(5) . . . . ?
C1L C2L C2T C2R 0.2(9) . . . . ?
O2 C2L C2T C1K -0.3(9) . . . . ?
C1L C2L C2T C1K 179.2(5) . . . . ?
N1 C1K C2T C2R 172.8(6) . . . . ?
N1 C1K C2T C2L -6.4(10) . . . . ?
C1X C22 C2U C2S 1.4(11) . . . . ?
C27 C2S C2U C22 -1.0(10) . . . . ?
C1M C2Q C2V C30 0.6(10) . . . . ?
C29 C2Q C2V C30 177.9(6) . . . . ?
C1R C1L C2X C3E -124.7(6) . . . . ?
C2L C1L C2X C3E 57.3(7) . . . . ?
C1R C1L C2X C33 112.2(6) . . . . ?
C2L C1L C2X C33 -65.8(7) . . . . ?
C1R C1L C2X C3G -3.9(8) . . . . ?
C2L C1L C2X C3G 178.0(6) . . . . ?
C2C C1V C2Y C32 3.3(8) . . . . ?
C11 C1V C2Y C32 -175.1(5) . . . . ?
C2A C13 C2Z C3D -0.8(10) . . . . ?
O9 C13 C2Z C3D -176.7(6) . . . . ?
C2P C2N C30 C2V 0.8(9) . . . . ?
C2P C2N C30 C21 -178.2(7) . . . . ?
C2Q C2V C30 C2N -1.4(10) . . . . ?
C2Q C2V C30 C21 177.6(7) . . . . ?
C2M C21 C30 C2N 1.9(11) . . . . ?
C3Q C21 C30 C2N -119.7(8) . . . . ?
C3O C21 C30 C2N 121.8(8) . . . . ?
C2M C21 C30 C2V -177.1(7) . . . . ?
C3Q C21 C30 C2V 61.3(9) . . . . ?
C3O C21 C30 C2V -57.2(9) . . . . ?
C1V C2Y C32 C2I 1.0(8) . . . . ?
C1V C2Y C32 C2W -179.8(5) . . . . ?
O3 C2I C32 C2Y 173.9(5) . . . . ?
C28 C2I C32 C2Y -4.0(7) . . . . ?
O3 C2I C32 C2W -5.3(8) . . . . ?
C28 C2I C32 C2W 176.8(5) . . . . ?
C3C C2W C32 C2Y 2.7(8) . . . . ?
C1T C2W C32 C2Y -115.9(6) . . . . ?
C3B C2W C32 C2Y 122.6(6) . . . . ?
C3C C2W C32 C2I -178.1(5) . . . . ?
C1T C2W C32 C2I 63.3(7) . . . . ?
C3B C2W C32 C2I -58.3(7) . . . . ?
C37 C1Y C34 C39 -0.9(9) . . . . ?
C37 C1Y C34 C36 177.4(6) . . . . ?
O7 C2J C35 C39 -177.5(5) . . . . ?
C37 C2J C35 C39 0.8(8) . . . . ?
O7 C2J C35 C19 6.7(9) . . . . ?
C37 C2J C35 C19 -175.0(5) . . . . ?
N3 C19 C35 C2J 3.0(10) . . . . ?
N3 C19 C35 C39 -173.0(6) . . . . ?
C39 C34 C36 C3M 123.4(7) . . . . ?
C1Y C34 C36 C3M -54.7(7) . . . . ?
C39 C34 C36 C9 -114.9(7) . . . . ?
C1Y C34 C36 C9 66.9(8) . . . . ?
C39 C34 C36 C2F 6.1(9) . . . . ?
C1Y C34 C36 C2F -172.1(6) . . . . ?
C34 C1Y C37 C2J 0.8(9) . . . . ?
C34 C1Y C37 C1W -178.3(6) . . . . ?
O7 C2J C37 C1Y 177.6(5) . . . . ?
C35 C2J C37 C1Y -0.7(8) . . . . ?
O7 C2J C37 C1W -3.4(8) . . . . ?
C35 C2J C37 C1W 178.4(5) . . . . ?
C1Q C1W C37 C1Y 4.0(8) . . . . ?
C31 C1W C37 C1Y -114.9(6) . . . . ?
C2K C1W C37 C1Y 124.8(6) . . . . ?
C1Q C1W C37 C2J -175.0(5) . . . . ?
C31 C1W C37 C2J 66.1(7) . . . . ?
C2K C1W C37 C2J -54.2(7) . . . . ?
C2 C2H C38 C1N 0.4(12) . . . . ?
C2D C1N C38 C2H 1.9(11) . . . . ?
C1Y C34 C39 C35 0.9(9) . . . . ?
C36 C34 C39 C35 -177.3(5) . . . . ?
C2J C35 C39 C34 -0.9(9) . . . . ?
C19 C35 C39 C34 175.2(5) . . . . ?
C23 O5 C3A F4 -84.4(8) . . . . ?
C23 O5 C3A F6 154.0(6) . . . . ?
C23 O5 C3A F5 37.4(9) . . . . ?
C14 C2O C3D C2Z 2.3(11) . . . . ?
C13 C2Z C3D C2O 0.0(11) . . . . ?
C2D O10 C3H F10 -44.5(9) . . . . ?
C2D O10 C3H F12 -164.0(6) . . . . ?
C2D O10 C3H F11 79.5(8) . . . . ?
C24 C1O C3P C3R 2.2(9) . . . . ?
C1O C3P C3R C10 -1.7(10) . . . . ?
C23 C10 C3R C3P -0.2(9) . . . . ?
C2A C13 O9 C6 137.9(8) . . . . ?
C2Z C13 O9 C6 -45.9(10) . . . . ?
C13 O9 C6 F8 74.8(11) . . . . ?
C13 O9 C6 F7 -44.5(11) . . . . ?
C13 O9 C6 F9 -166.7(7) . . . . ?

_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.995
_refine_diff_density_max         1.095
_refine_diff_density_min         -0.679
_refine_diff_density_rms         0.164
# SQUEEZE RESULTS (APPEND TO CIF)
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
1 0.000 0.000 0.500 567.1 126.0
_platon_squeeze_details          
; ?
;

_database_code_depnum_ccdc_archive 'CCDC 980005'
#######################################################################
#
#                 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_6

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C54 H60 N2 O5 V'
_chemical_formula_sum            'C54 H60 N2 O5 V'
_chemical_formula_weight         867.98

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           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                   11.896(2)
_cell_length_b                   14.224(3)
_cell_length_c                   15.568(3)
_cell_angle_alpha                108.49(3)
_cell_angle_beta                 90.94(3)
_cell_angle_gamma                109.43(3)
_cell_volume                     2334.2(8)
_cell_formula_units_Z            2
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    25233
_cell_measurement_theta_min      1.39
_cell_measurement_theta_max      25.00


_exptl_crystal_description       Plate
_exptl_crystal_colour            brown
_exptl_crystal_size_max          0.397
_exptl_crystal_size_mid          0.169
_exptl_crystal_size_min          0.106
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.235
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             922
_exptl_absorpt_coefficient_mu    0.262
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_absorpt_correction_T_min  .0000
_exptl_absorpt_correction_T_max  .0000

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'MM007-HF CCD(Saturn 724+)'
_diffrn_measurement_method       'ω scans at fixed χ = 45°'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         none
_diffrn_standards_interval_count none
_diffrn_standards_interval_time  none
_diffrn_standards_decay_%        none
_diffrn_reflns_number            25233
_diffrn_reflns_av_R_equivalents  0.0692
_diffrn_reflns_av_unetI/netI     0.0581
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         1.39
_diffrn_reflns_theta_max         25.00
_reflns_number_total             8209
_reflns_number_gt                7447
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrystalClear (Rigaku Inc., 2007)'
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2007)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'CAMERON (Watkin et al, 1993)'
_computing_publication_material  'SHELX97 (Sheldrick, 1997)'


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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1851P)²+0.7904P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         8209
_refine_ls_number_parameters     559
_refine_ls_number_restraints     0
_refine_ls_R_factor_ref          0.0776
_refine_ls_R_factor_gt           0.0590
_refine_ls_wR_factor_ref         0.2345
_refine_ls_wR_factor_gt          0.1911
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_restrained_S_all      1.023
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
V1 V 0.09967(4) 0.87932(3) 0.31451(3) 0.0166(2) Uani 1 1 d . . .
O2 O 0.16972(18) 0.90073(14) 0.20975(13) 0.0218(4) Uani 1 1 d . . .
O3 O 0.18995(18) 0.89368(14) 0.42250(13) 0.0221(4) Uani 1 1 d . . .
O5 O 0.27218(18) 1.22275(15) 0.33667(15) 0.0265(5) Uani 1 1 d . . .
N2 N 0.1303(2) 1.04393(17) 0.37397(15) 0.0179(5) Uani 1 1 d . . .
N1 N 0.0936(2) 0.71951(17) 0.26067(16) 0.0189(5) Uani 1 1 d . . .
O4 O 0.19160(18) 0.56250(15) 0.26946(14) 0.0268(5) Uani 1 1 d . . .
O1 O -0.04326(18) 0.84476(16) 0.30696(16) 0.0316(5) Uani 1 1 d . . .
C8 C 0.2895(2) 1.1528(2) 0.60629(19) 0.0203(6) Uani 1 1 d . . .
H8 H 0.2825 1.2203 0.6186 0.024 Uiso 1 1 calc R . .
C9 C 0.1946(2) 0.8397(2) 0.13397(18) 0.0185(6) Uani 1 1 d . . .
C10 C 0.1497(3) 1.1828(2) 0.30574(19) 0.0210(6) Uani 1 1 d . . .
C11 C 0.2380(2) 1.0732(2) 0.52084(18) 0.0189(6) Uani 1 1 d . . .
C12 C 0.2449(2) 0.9708(2) 0.50078(18) 0.0181(6) Uani 1 1 d . . .
C13 C 0.3120(2) 0.9530(2) 0.56655(19) 0.0204(6) Uani 1 1 d . . .
C14 C 0.1980(2) 0.6663(2) 0.03729(18) 0.0206(6) Uani 1 1 d . . .
H14 H 0.1784 0.5929 0.0272 0.025 Uiso 1 1 calc R . .
C15 C 0.1698(2) 0.7307(2) 0.11710(19) 0.0203(6) Uani 1 1 d . . .
C16 C 0.4042(3) 1.2178(2) 0.76752(19) 0.0234(6) Uani 1 1 d . . .
C17 C 0.0787(3) 1.0937(2) 0.32457(18) 0.0196(6) Uani 1 1 d . . .
C18 C 0.2465(2) 0.8829(2) 0.06664(18) 0.0197(6) Uani 1 1 d . . .
C19 C 0.3610(3) 1.0350(2) 0.64890(19) 0.0213(6) Uani 1 1 d . . .
H19 H 0.4054 1.0227 0.6928 0.026 Uiso 1 1 calc R . .
C20 C 0.1158(2) 0.6779(2) 0.17917(19) 0.0204(6) Uani 1 1 d . . .
H20 H 0.0937 0.6030 0.1575 0.024 Uiso 1 1 calc R . .
C21 C 0.2531(2) 0.7078(2) -0.02592(19) 0.0208(6) Uani 1 1 d . . .
C22 C 0.0887(3) 0.5669(2) 0.30815(19) 0.0244(6) Uani 1 1 d . . .
C23 C 0.3498(2) 1.1352(2) 0.67241(18) 0.0192(6) Uani 1 1 d . . .
C24 C 0.1807(2) 1.1023(2) 0.45732(18) 0.0194(6) Uani 1 1 d . . .
H24 H 0.1791 1.1722 0.4783 0.023 Uiso 1 1 calc R . .
C25 C 0.0432(3) 0.6456(2) 0.30746(18) 0.0219(6) Uani 1 1 d . . .
C26 C 0.1816(3) 0.4751(2) 0.1931(2) 0.0253(6) Uani 1 1 d . . .
C27 C 0.2752(2) 0.8159(2) -0.00911(19) 0.0224(6) Uani 1 1 d . . .
H27 H 0.3126 0.8454 -0.0528 0.027 Uiso 1 1 calc R . .
C28 C 0.0994(3) 1.2251(2) 0.2525(2) 0.0252(6) Uani 1 1 d . . .
H28 H 0.1490 1.2836 0.2371 0.030 Uiso 1 1 calc R . .
C29 C -0.0558(3) 0.6516(2) 0.35332(19) 0.0276(7) Uani 1 1 d . . .
H29 H -0.0873 0.7050 0.3542 0.033 Uiso 1 1 calc R . .
C30 C 0.3350(3) 1.3307(2) 0.35826(19) 0.0215(6) Uani 1 1 d . . .
C31 C -0.0225(3) 1.1820(2) 0.2223(2) 0.0288(7) Uani 1 1 d . . .
H31 H -0.0570 1.2113 0.1866 0.035 Uiso 1 1 calc R . .
C32 C 0.0738(3) 0.4059(2) 0.1405(2) 0.0261(6) Uani 1 1 d . . .
H32 H 0.0005 0.4142 0.1579 0.031 Uiso 1 1 calc R . .
C33 C 0.2885(3) 1.4061(2) 0.4067(2) 0.0273(7) Uani 1 1 d . . .
H33 H 0.2103 1.3850 0.4239 0.033 Uiso 1 1 calc R . .
C34 C 0.2945(3) 0.6422(2) -0.10925(19) 0.0259(6) Uani 1 1 d . . .
C35 C -0.0440(3) 1.0514(2) 0.2942(2) 0.0251(6) Uani 1 1 d . . .
H35 H -0.0934 0.9916 0.3079 0.030 Uiso 1 1 calc R . .
C36 C 0.2062(3) 0.7595(2) 0.5401(2) 0.0317(7) Uani 1 1 d . . .
H36A H 0.1499 0.7565 0.4918 0.048 Uiso 1 1 calc R . .
H36B H 0.1745 0.7763 0.5985 0.048 Uiso 1 1 calc R . .
H36C H 0.2160 0.6906 0.5255 0.048 Uiso 1 1 calc R . .
C37 C 0.4490(3) 1.3609(2) 0.3339(2) 0.0259(6) Uani 1 1 d . . .
H37 H 0.4807 1.3090 0.3009 0.031 Uiso 1 1 calc R . .
C38 C 0.2663(3) 0.9980(2) 0.0762(2) 0.0276(7) Uani 1 1 d . . .
C39 C 0.3771(3) 1.3192(3) 0.7809(2) 0.0365(8) Uani 1 1 d . . .
H39A H 0.2898 1.3017 0.7723 0.055 Uiso 1 1 calc R . .
H39B H 0.4133 1.3513 0.7362 0.055 Uiso 1 1 calc R . .
H39C H 0.4108 1.3693 0.8429 0.055 Uiso 1 1 calc R . .
C40 C 0.3285(3) 0.8455(2) 0.5470(2) 0.0259(6) Uani 1 1 d . . .
C41 C 0.4709(3) 1.5439(2) 0.4059(2) 0.0348(8) Uani 1 1 d . . .
H41 H 0.5176 1.6172 0.4221 0.042 Uiso 1 1 calc R . .
C42 C 0.5166(3) 1.4677(2) 0.3582(2) 0.0318(7) Uani 1 1 d . . .
H42 H 0.5954 1.4891 0.3419 0.038 Uiso 1 1 calc R . .
C43 C -0.0951(3) 1.0957(2) 0.2441(2) 0.0298(7) Uani 1 1 d . . .
H43 H -0.1794 1.0672 0.2247 0.036 Uiso 1 1 calc R . .
C44 C 0.0359(3) 0.4969(3) 0.3532(2) 0.0337(7) Uani 1 1 d . . .
H44 H 0.0678 0.4441 0.3538 0.040 Uiso 1 1 calc R . .
C45 C -0.0632(3) 0.5032(3) 0.3976(2) 0.0384(8) Uani 1 1 d . . .
H45 H -0.0995 0.4545 0.4279 0.046 Uiso 1 1 calc R . .
C46 C 0.2299(3) 0.5230(3) -0.1317(2) 0.0379(8) Uani 1 1 d . . .
H46A H 0.2588 0.4841 -0.1852 0.057 Uiso 1 1 calc R . .
H46B H 0.1431 0.5052 -0.1450 0.057 Uiso 1 1 calc R . .
H46C H 0.2465 0.5032 -0.0793 0.057 Uiso 1 1 calc R . .
C47 C 0.0725(3) 0.3242(2) 0.0622(2) 0.0315(7) Uani 1 1 d . . .
H47 H -0.0017 0.2776 0.0251 0.038 Uiso 1 1 calc R . .
C48 C 0.3202(4) 1.0256(3) -0.0053(2) 0.0385(8) Uani 1 1 d . . .
H48A H 0.2657 0.9786 -0.0618 0.058 Uiso 1 1 calc R . .
H48B H 0.3982 1.0164 -0.0092 0.058 Uiso 1 1 calc R . .
H48C H 0.3311 1.0994 0.0029 0.058 Uiso 1 1 calc R . .
C49 C 0.5405(3) 1.2460(3) 0.7812(2) 0.0383(8) Uani 1 1 d . . .
H49A H 0.5744 1.2988 0.8421 0.057 Uiso 1 1 calc R . .
H49B H 0.5761 1.2752 0.7347 0.057 Uiso 1 1 calc R . .
H49C H 0.5585 1.1820 0.7756 0.057 Uiso 1 1 calc R . .
C50 C 0.3573(3) 1.5121(2) 0.4295(2) 0.0326(7) Uani 1 1 d . . .
H50 H 0.3255 1.5641 0.4622 0.039 Uiso 1 1 calc R . .
C51 C 0.3828(3) 0.8174(3) 0.4576(2) 0.0365(8) Uani 1 1 d . . .
H51A H 0.4608 0.8729 0.4628 0.055 Uiso 1 1 calc R . .
H51B H 0.3283 0.8119 0.4068 0.055 Uiso 1 1 calc R . .
H51C H 0.3938 0.7493 0.4460 0.055 Uiso 1 1 calc R . .
C52 C 0.3485(3) 1.1722(3) 0.8403(2) 0.0392(8) Uani 1 1 d . . .
H52A H 0.2611 1.1541 0.8316 0.059 Uiso 1 1 calc R . .
H52B H 0.3823 1.2250 0.9013 0.059 Uiso 1 1 calc R . .
H52C H 0.3664 1.1082 0.8347 0.059 Uiso 1 1 calc R . .
C53 C -0.1082(3) 0.5805(3) 0.3973(2) 0.0339(8) Uani 1 1 d . . .
H53 H -0.1759 0.5851 0.4275 0.041 Uiso 1 1 calc R . .
C54 C 0.3551(3) 1.0736(2) 0.1617(2) 0.0389(8) Uani 1 1 d . . .
H54A H 0.3673 1.1470 0.1673 0.058 Uiso 1 1 calc R . .
H54B H 0.4321 1.0625 0.1569 0.058 Uiso 1 1 calc R . .
H54C H 0.3228 1.0597 0.2158 0.058 Uiso 1 1 calc R . .
C55 C 0.1772(3) 0.3104(3) 0.0380(3) 0.0464(9) Uani 1 1 d . . .
H55 H 0.1762 0.2538 -0.0151 0.056 Uiso 1 1 calc R . .
C56 C 0.1445(4) 1.0130(3) 0.0785(2) 0.0387(8) Uani 1 1 d . . .
H56A H 0.0904 0.9631 0.0226 0.058 Uiso 1 1 calc R . .
H56B H 0.1560 1.0858 0.0825 0.058 Uiso 1 1 calc R . .
H56C H 0.1093 0.9995 0.1318 0.058 Uiso 1 1 calc R . .
C57 C 0.2728(3) 0.6706(3) -0.1943(2) 0.0352(8) Uani 1 1 d . . .
H57A H 0.3137 0.7469 -0.1808 0.053 Uiso 1 1 calc R . .
H57B H 0.1863 0.6516 -0.2106 0.053 Uiso 1 1 calc R . .
H57C H 0.3047 0.6312 -0.2454 0.053 Uiso 1 1 calc R . .
C58 C 0.2882(3) 0.4616(3) 0.1702(3) 0.0398(8) Uani 1 1 d . . .
H58 H 0.3625 0.5075 0.2075 0.048 Uiso 1 1 calc R . .
C59 C 0.4134(4) 0.8474(3) 0.6232(3) 0.0462(9) Uani 1 1 d . . .
H59A H 0.4925 0.9019 0.6292 0.069 Uiso 1 1 calc R . .
H59B H 0.4217 0.7779 0.6080 0.069 Uiso 1 1 calc R . .
H59C H 0.3803 0.8636 0.6811 0.069 Uiso 1 1 calc R . .
C60 C 0.4297(3) 0.6675(4) -0.0881(3) 0.0456(9) Uani 1 1 d . . .
H60A H 0.4728 0.7437 -0.0736 0.068 Uiso 1 1 calc R . .
H60B H 0.4580 0.6279 -0.1416 0.068 Uiso 1 1 calc R . .
H60C H 0.4448 0.6471 -0.0358 0.068 Uiso 1 1 calc R . .
C61 C 0.2842(4) 0.3793(4) 0.0914(3) 0.0577(12) Uani 1 1 d . . .
H61 H 0.3572 0.3704 0.0740 0.069 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 1.596(2) . ?
V1 O3 1.897(2) . ?
V1 O2 1.907(2) . ?
V1 N2 2.126(2) . ?
V1 N1 2.134(2) . ?
O2 C9 1.329(3) . ?
O3 C12 1.329(3) . ?
O5 C10 1.389(3) . ?
O5 C30 1.389(3) . ?
N2 C24 1.301(4) . ?
N2 C17 1.445(3) . ?
N1 C20 1.292(4) . ?
N1 C25 1.441(3) . ?
O4 C22 1.385(4) . ?
O4 C26 1.390(4) . ?
C8 C23 1.376(4) . ?
C8 C11 1.409(4) . ?
C9 C15 1.412(4) . ?
C9 C18 1.427(4) . ?
C10 C17 1.391(4) . ?
C10 C28 1.396(4) . ?
C11 C12 1.419(4) . ?
C11 C24 1.428(4) . ?
C12 C13 1.423(4) . ?
C13 C19 1.385(4) . ?
C13 C40 1.540(4) . ?
C14 C21 1.371(4) . ?
C14 C15 1.411(4) . ?
C15 C20 1.438(4) . ?
C16 C49 1.529(4) . ?
C16 C39 1.532(4) . ?
C16 C23 1.533(4) . ?
C16 C52 1.534(4) . ?
C17 C35 1.388(4) . ?
C18 C27 1.390(4) . ?
C18 C38 1.532(4) . ?
C19 C23 1.408(4) . ?
C21 C27 1.406(4) . ?
C21 C34 1.534(4) . ?
C22 C44 1.386(4) . ?
C22 C25 1.398(4) . ?
C25 C29 1.400(4) . ?
C26 C32 1.378(4) . ?
C26 C58 1.380(4) . ?
C28 C31 1.380(4) . ?
C29 C53 1.383(4) . ?
C30 C37 1.379(4) . ?
C30 C33 1.385(4) . ?
C31 C43 1.392(4) . ?
C32 C47 1.389(4) . ?
C33 C50 1.379(4) . ?
C34 C46 1.529(4) . ?
C34 C60 1.533(4) . ?
C34 C57 1.542(4) . ?
C35 C43 1.388(4) . ?
C36 C40 1.534(4) . ?
C37 C42 1.382(4) . ?
C38 C54 1.528(4) . ?
C38 C56 1.531(5) . ?
C38 C48 1.533(4) . ?
C40 C59 1.533(5) . ?
C40 C51 1.538(4) . ?
C41 C50 1.371(5) . ?
C41 C42 1.385(5) . ?
C44 C45 1.390(5) . ?
C45 C53 1.376(5) . ?
C47 C55 1.365(5) . ?
C55 C61 1.376(6) . ?
C58 C61 1.389(5) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 V1 O3 120.01(11) . . ?
O1 V1 O2 116.39(11) . . ?
O3 V1 O2 123.58(9) . . ?
O1 V1 N2 94.01(10) . . ?
O3 V1 N2 86.73(9) . . ?
O2 V1 N2 90.86(9) . . ?
O1 V1 N1 93.31(10) . . ?
O3 V1 N1 87.90(9) . . ?
O2 V1 N1 87.65(9) . . ?
N2 V1 N1 172.41(9) . . ?
C9 O2 V1 135.44(17) . . ?
C12 O3 V1 136.72(17) . . ?
C10 O5 C30 118.8(2) . . ?
C24 N2 C17 115.8(2) . . ?
C24 N2 V1 124.64(19) . . ?
C17 N2 V1 119.05(17) . . ?
C20 N1 C25 115.1(2) . . ?
C20 N1 V1 123.07(18) . . ?
C25 N1 V1 120.98(17) . . ?
C22 O4 C26 118.4(2) . . ?
C23 C8 C11 121.6(2) . . ?
O2 C9 C15 121.5(2) . . ?
O2 C9 C18 120.5(2) . . ?
C15 C9 C18 118.1(2) . . ?
O5 C10 C17 117.6(2) . . ?
O5 C10 C28 121.9(2) . . ?
C17 C10 C28 120.3(3) . . ?
C8 C11 C12 120.7(2) . . ?
C8 C11 C24 116.1(2) . . ?
C12 C11 C24 123.2(2) . . ?
O3 C12 C11 120.8(2) . . ?
O3 C12 C13 120.8(2) . . ?
C11 C12 C13 118.4(2) . . ?
C19 C13 C12 117.8(2) . . ?
C19 C13 C40 121.2(2) . . ?
C12 C13 C40 121.0(2) . . ?
C21 C14 C15 121.2(3) . . ?
C14 C15 C9 121.4(2) . . ?
C14 C15 C20 115.5(2) . . ?
C9 C15 C20 123.1(2) . . ?
C49 C16 C39 109.0(3) . . ?
C49 C16 C23 110.1(2) . . ?
C39 C16 C23 111.5(2) . . ?
C49 C16 C52 109.5(3) . . ?
C39 C16 C52 107.5(3) . . ?
C23 C16 C52 109.2(2) . . ?
C35 C17 C10 119.1(3) . . ?
C35 C17 N2 119.6(2) . . ?
C10 C17 N2 121.3(2) . . ?
C27 C18 C9 117.6(2) . . ?
C27 C18 C38 121.3(2) . . ?
C9 C18 C38 121.1(2) . . ?
C13 C19 C23 124.9(3) . . ?
N1 C20 C15 128.3(2) . . ?
C14 C21 C27 116.8(3) . . ?
C14 C21 C34 122.5(3) . . ?
C27 C21 C34 120.7(2) . . ?
O4 C22 C44 119.1(3) . . ?
O4 C22 C25 120.6(2) . . ?
C44 C22 C25 120.2(3) . . ?
C8 C23 C19 116.5(2) . . ?
C8 C23 C16 123.8(2) . . ?
C19 C23 C16 119.7(2) . . ?
N2 C24 C11 127.4(2) . . ?
C22 C25 C29 118.4(3) . . ?
C22 C25 N1 122.5(3) . . ?
C29 C25 N1 119.1(3) . . ?
C32 C26 C58 120.5(3) . . ?
C32 C26 O4 123.6(3) . . ?
C58 C26 O4 115.9(3) . . ?
C18 C27 C21 124.9(3) . . ?
C31 C28 C10 120.0(3) . . ?
C53 C29 C25 120.8(3) . . ?
C37 C30 C33 120.7(3) . . ?
C37 C30 O5 117.4(3) . . ?
C33 C30 O5 121.9(3) . . ?
C28 C31 C43 120.0(3) . . ?
C26 C32 C47 119.9(3) . . ?
C50 C33 C30 119.2(3) . . ?
C46 C34 C60 108.2(3) . . ?
C46 C34 C21 112.1(2) . . ?
C60 C34 C21 108.5(2) . . ?
C46 C34 C57 108.6(3) . . ?
C60 C34 C57 108.3(3) . . ?
C21 C34 C57 111.0(2) . . ?
C43 C35 C17 120.7(3) . . ?
C30 C37 C42 119.1(3) . . ?
C54 C38 C56 112.1(3) . . ?
C54 C38 C18 109.9(3) . . ?
C56 C38 C18 108.9(3) . . ?
C54 C38 C48 106.9(3) . . ?
C56 C38 C48 107.3(3) . . ?
C18 C38 C48 111.7(2) . . ?
C59 C40 C36 107.7(3) . . ?
C59 C40 C51 107.5(3) . . ?
C36 C40 C51 110.2(3) . . ?
C59 C40 C13 112.1(3) . . ?
C36 C40 C13 109.3(2) . . ?
C51 C40 C13 110.0(2) . . ?
C50 C41 C42 119.1(3) . . ?
C37 C42 C41 120.9(3) . . ?
C35 C43 C31 119.8(3) . . ?
C22 C44 C45 120.6(3) . . ?
C53 C45 C44 119.4(3) . . ?
C55 C47 C32 120.4(3) . . ?
C41 C50 C33 121.1(3) . . ?
C45 C53 C29 120.5(3) . . ?
C47 C55 C61 119.3(3) . . ?
C26 C58 C61 118.4(3) . . ?
C55 C61 C58 121.6(3) . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.827
_refine_diff_density_min         -0.801
_refine_diff_density_rms         0.209

_database_code_depnum_ccdc_archive 'CCDC 980006'
#######################################################################
#
#                 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_7.(3/2)MeCN

_audit_creation_method           SHELXL-2012
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C54 H60 N2 O5 V, 1.5(C2 H3 N)'
_chemical_formula_sum            'C57 H64.50 N3.50 O5 V'
_chemical_formula_weight         929.56

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

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

_cell_length_a                   15.3075(16)
_cell_length_b                   18.0329(18)
_cell_length_c                   20.191(2)
_cell_angle_alpha                76.0289(15)
_cell_angle_beta                 81.7168(15)
_cell_angle_gamma                78.9101(15)
_cell_volume                     5279.7(9)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    7132
_cell_measurement_theta_min      2.16
_cell_measurement_theta_max      22.00

_exptl_crystal_description       plate
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.169
_exptl_crystal_F_000             1976
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.620
_exptl_crystal_size_mid          0.380
_exptl_crystal_size_min          0.080
_exptl_absorpt_coefficient_mu    0.237
_shelx_estimated_absorpt_T_min   0.867
_shelx_estimated_absorpt_T_max   0.981
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.867
_exptl_absorpt_correction_T_max  0.981
_exptl_absorpt_process_details   'SADABS v2009/1, Sheldrick, G.M., (2009)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX 2 CCD diffractometer'
_diffrn_measurement_method       'ω rotation with narrow frames'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        0
_diffrn_reflns_number            44050
_diffrn_reflns_sigmaI/netI       0.0702
_diffrn_reflns_av_R_equivalents  0.0659
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         1.393
_diffrn_reflns_theta_max         22.499
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 0.722
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 0.722
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 0.722
_reflns_number_total             13810
_reflns_number_gt                8609
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
; 
 The reflections were merged according to the crystal class 
 for structure refinement and the calculation of statistics. 
 _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. 

 One tBu group at C(65) was modelled as having the methyl groups
 disordered over two sets of positions. Restraints were applied to
 anisotropic displacement and geometrical parameters for this group.
;

_computing_data_collection       'Bruker APEX 2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2012 (Sheldrick, 2012)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 ? 
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
; 
 w=1/[σ²(Fo²)+(0.0455P)²+3.3864P] 
 where P=(Fo²+2Fc²)/3 
;
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         13810
_refine_ls_number_parameters     1250
_refine_ls_number_restraints     92
_refine_ls_R_factor_all          0.0973
_refine_ls_R_factor_gt           0.0486
_refine_ls_wR_factor_ref         0.1304
_refine_ls_wR_factor_gt          0.1048
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_restrained_S_all      1.042
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
V1 V 0.43667(4) 0.20015(4) 0.30017(3) 0.03344(18) Uani 1 1 d D . .
O1 O 0.30864(16) 0.21927(14) 0.31552(12) 0.0386(7) Uani 1 1 d D . .
N1 N 0.4222(2) 0.25563(17) 0.19612(14) 0.0340(8) Uani 1 1 d D . .
C1 C 0.2412(3) 0.2560(2) 0.27815(18) 0.0370(10) Uani 1 1 d D . .
O2 O 0.44942(18) 0.40020(15) 0.11219(12) 0.0450(7) Uani 1 1 d D . .
N2 N 0.4385(2) 0.15974(18) 0.40781(15) 0.0362(8) Uani 1 1 d D . .
C2 C 0.1519(3) 0.2655(2) 0.30912(19) 0.0405(10) Uani 1 1 d D . .
O3 O 0.50830(16) 0.27334(14) 0.30574(11) 0.0361(6) Uani 1 1 d D . .
C3 C 0.0854(3) 0.3053(2) 0.2672(2) 0.0469(11) Uani 1 1 d D . .
H3 H 0.0257 0.3123 0.2883 0.056 Uiso 1 1 calc R . .
O4 O 0.32637(17) 0.17043(18) 0.53047(13) 0.0506(8) Uani 1 1 d D . .
C4 C 0.0994(3) 0.3359(2) 0.1966(2) 0.0431(10) Uani 1 1 d D . .
O5 O 0.48890(16) 0.11967(14) 0.28460(12) 0.0384(6) Uani 1 1 d D . .
C5 C 0.1875(3) 0.3247(2) 0.16805(19) 0.0414(10) Uani 1 1 d D . .
H5 H 0.2007 0.3440 0.1203 0.050 Uiso 1 1 calc R . .
C6 C 0.2581(2) 0.2856(2) 0.20747(18) 0.0335(9) Uani 1 1 d D . .
C7 C 0.1285(3) 0.2328(3) 0.3863(2) 0.0519(12) Uani 1 1 d D . .
C8 C 0.1780(3) 0.2689(3) 0.4285(2) 0.0607(13) Uani 1 1 d D . .
H8A H 0.2424 0.2592 0.4145 0.091 Uiso 1 1 calc R . .
H8B H 0.1663 0.2456 0.4773 0.091 Uiso 1 1 calc R . .
H8C H 0.1568 0.3249 0.4204 0.091 Uiso 1 1 calc R . .
C9 C 0.1543(3) 0.1446(3) 0.4019(2) 0.0584(13) Uani 1 1 d D . .
H9A H 0.1188 0.1227 0.3770 0.088 Uiso 1 1 calc R . .
H9B H 0.1426 0.1239 0.4513 0.088 Uiso 1 1 calc R . .
H9C H 0.2181 0.1305 0.3874 0.088 Uiso 1 1 calc R . .
C10 C 0.0274(3) 0.2524(3) 0.4087(2) 0.0684(15) Uani 1 1 d D . .
H10A H 0.0090 0.3088 0.3989 0.103 Uiso 1 1 calc R . .
H10B H 0.0157 0.2314 0.4580 0.103 Uiso 1 1 calc R . .
H10C H -0.0065 0.2296 0.3834 0.103 Uiso 1 1 calc R . .
C11 C 0.0241(3) 0.3814(3) 0.1526(2) 0.0506(12) Uani 1 1 d D . .
C12 C -0.0669(3) 0.3877(4) 0.1932(3) 0.101(2) Uani 1 1 d D . .
H12A H -0.0656 0.4124 0.2313 0.151 Uiso 1 1 calc R . .
H12B H -0.0824 0.3359 0.2115 0.151 Uiso 1 1 calc R . .
H12C H -0.1117 0.4191 0.1633 0.151 Uiso 1 1 calc R . .
C13 C 0.0231(4) 0.3420(4) 0.0949(3) 0.113(2) Uani 1 1 d D . .
H13A H 0.0110 0.2892 0.1139 0.170 Uiso 1 1 calc R . .
H13B H 0.0813 0.3402 0.0673 0.170 Uiso 1 1 calc R . .
H13C H -0.0238 0.3711 0.0659 0.170 Uiso 1 1 calc R . .
C14 C 0.0422(3) 0.4632(3) 0.1230(3) 0.0897(18) Uani 1 1 d D . .
H14A H -0.0068 0.4929 0.0964 0.135 Uiso 1 1 calc R . .
H14B H 0.0986 0.4617 0.0930 0.135 Uiso 1 1 calc R . .
H14C H 0.0465 0.4878 0.1604 0.135 Uiso 1 1 calc R . .
C15 C 0.3462(2) 0.2808(2) 0.17091(18) 0.0332(9) Uani 1 1 d D . .
H15 H 0.3489 0.2982 0.1225 0.040 Uiso 1 1 calc R . .
C16 C 0.4999(2) 0.2627(2) 0.14551(17) 0.0362(10) Uani 1 1 d D . .
C17 C 0.5640(2) 0.1984(2) 0.14038(18) 0.0393(10) Uani 1 1 d D . .
H17 H 0.5579 0.1497 0.1702 0.047 Uiso 1 1 calc R . .
C18 C 0.6375(3) 0.2053(3) 0.0912(2) 0.0528(12) Uani 1 1 d D . .
H18 H 0.6814 0.1611 0.0871 0.063 Uiso 1 1 calc R . .
C19 C 0.6466(3) 0.2767(3) 0.0482(2) 0.0575(13) Uani 1 1 d D . .
H19 H 0.6969 0.2811 0.0147 0.069 Uiso 1 1 calc R . .
C20 C 0.5839(3) 0.3408(3) 0.0535(2) 0.0505(12) Uani 1 1 d D . .
H20 H 0.5910 0.3896 0.0242 0.061 Uiso 1 1 calc R . .
C21 C 0.5094(3) 0.3342(2) 0.10208(18) 0.0391(10) Uani 1 1 d D . .
C22 C 0.3911(3) 0.4384(2) 0.0631(2) 0.0428(11) Uani 1 1 d D . .
C23 C 0.3290(3) 0.4983(3) 0.0813(2) 0.0512(12) Uani 1 1 d D . .
H23 H 0.3303 0.5128 0.1233 0.061 Uiso 1 1 calc R . .
C24 C 0.2641(3) 0.5375(3) 0.0375(3) 0.0602(13) Uani 1 1 d D . .
H24 H 0.2197 0.5776 0.0504 0.072 Uiso 1 1 calc R . .
C25 C 0.2645(3) 0.5179(3) -0.0244(3) 0.0649(14) Uani 1 1 d D . .
H25 H 0.2203 0.5443 -0.0543 0.078 Uiso 1 1 calc R . .
C26 C 0.3290(3) 0.4603(3) -0.0429(2) 0.0586(13) Uani 1 1 d D . .
H26 H 0.3302 0.4484 -0.0864 0.070 Uiso 1 1 calc R . .
C27 C 0.3932(3) 0.4186(2) 0.0009(2) 0.0505(11) Uani 1 1 d D . .
H27 H 0.4368 0.3780 -0.0118 0.061 Uiso 1 1 calc R . .
C28 C 0.5535(2) 0.2845(2) 0.35366(18) 0.0336(9) Uani 1 1 d D . .
C29 C 0.6086(3) 0.3430(2) 0.33794(18) 0.0387(10) Uani 1 1 d D . .
C30 C 0.6560(3) 0.3487(2) 0.38973(19) 0.0403(10) Uani 1 1 d D . .
H30 H 0.6935 0.3872 0.3791 0.048 Uiso 1 1 calc R . .
C31 C 0.6532(3) 0.3021(2) 0.45677(19) 0.0402(10) Uani 1 1 d D . .
C32 C 0.5970(3) 0.2479(2) 0.47087(19) 0.0389(10) Uani 1 1 d D . .
H32 H 0.5915 0.2162 0.5158 0.047 Uiso 1 1 calc R . .
C33 C 0.5471(2) 0.2378(2) 0.42096(18) 0.0340(9) Uani 1 1 d D . .
C34 C 0.6166(3) 0.3967(2) 0.26648(19) 0.0447(11) Uani 1 1 d D . .
C35 C 0.5229(3) 0.4378(2) 0.2473(2) 0.0538(12) Uani 1 1 d D . .
H35A H 0.4865 0.3992 0.2458 0.081 Uiso 1 1 calc R . .
H35B H 0.5283 0.4731 0.2022 0.081 Uiso 1 1 calc R . .
H35C H 0.4942 0.4674 0.2817 0.081 Uiso 1 1 calc R . .
C36 C 0.6628(3) 0.3490(3) 0.21395(19) 0.0531(12) Uani 1 1 d D . .
H36A H 0.7229 0.3245 0.2263 0.080 Uiso 1 1 calc R . .
H36B H 0.6673 0.3831 0.1682 0.080 Uiso 1 1 calc R . .
H36C H 0.6277 0.3090 0.2138 0.080 Uiso 1 1 calc R . .
C37 C 0.6722(3) 0.4598(3) 0.2641(2) 0.0645(14) Uani 1 1 d D . .
H37A H 0.6460 0.4890 0.2993 0.097 Uiso 1 1 calc R . .
H37B H 0.6723 0.4950 0.2188 0.097 Uiso 1 1 calc R . .
H37C H 0.7337 0.4357 0.2727 0.097 Uiso 1 1 calc R . .
C38 C 0.7109(3) 0.3128(2) 0.5088(2) 0.0469(11) Uani 1 1 d D . .
C39 C 0.8097(3) 0.2916(3) 0.4829(2) 0.0630(13) Uani 1 1 d D . .
H39A H 0.8235 0.3267 0.4389 0.094 Uiso 1 1 calc R . .
H39B H 0.8213 0.2381 0.4768 0.094 Uiso 1 1 calc R . .
H39C H 0.8475 0.2962 0.5165 0.094 Uiso 1 1 calc R . .
C40 C 0.6918(3) 0.3964(3) 0.5162(2) 0.0640(14) Uani 1 1 d D . .
H40A H 0.7279 0.4024 0.5504 0.096 Uiso 1 1 calc R . .
H40B H 0.6282 0.4103 0.5311 0.096 Uiso 1 1 calc R . .
H40C H 0.7071 0.4304 0.4720 0.096 Uiso 1 1 calc R . .
C41 C 0.6924(3) 0.2609(3) 0.5798(2) 0.0610(13) Uani 1 1 d D . .
H41A H 0.7307 0.2691 0.6115 0.092 Uiso 1 1 calc R . .
H41B H 0.7052 0.2065 0.5764 0.092 Uiso 1 1 calc R . .
H41C H 0.6294 0.2740 0.5970 0.092 Uiso 1 1 calc R . .
C42 C 0.4916(2) 0.1790(2) 0.44293(19) 0.0374(10) Uani 1 1 d D . .
H42 H 0.4940 0.1507 0.4890 0.045 Uiso 1 1 calc R . .
C43 C 0.3903(2) 0.0984(2) 0.44465(19) 0.0388(10) Uani 1 1 d D . .
C44 C 0.3951(3) 0.0335(2) 0.4185(2) 0.0434(11) Uani 1 1 d D . .
H44 H 0.4282 0.0307 0.3754 0.052 Uiso 1 1 calc R . .
C45 C 0.3525(3) -0.0276(3) 0.4543(2) 0.0521(12) Uani 1 1 d D . .
H45 H 0.3558 -0.0716 0.4354 0.063 Uiso 1 1 calc R . .
C46 C 0.3049(3) -0.0244(3) 0.5177(2) 0.0609(14) Uani 1 1 d D . .
H46 H 0.2775 -0.0670 0.5433 0.073 Uiso 1 1 calc R . .
C47 C 0.2977(3) 0.0407(3) 0.5433(2) 0.0573(13) Uani 1 1 d D . .
H47 H 0.2634 0.0436 0.5860 0.069 Uiso 1 1 calc R . .
C48 C 0.3394(3) 0.1019(3) 0.5078(2) 0.0460(11) Uani 1 1 d D . .
C49 C 0.3652(3) 0.1722(3) 0.5882(2) 0.0479(11) Uani 1 1 d D . .
C50 C 0.3507(3) 0.2431(3) 0.6051(2) 0.0592(13) Uani 1 1 d D . .
H50 H 0.3154 0.2862 0.5787 0.071 Uiso 1 1 calc R . .
C51 C 0.3884(3) 0.2514(3) 0.6614(2) 0.0725(15) Uani 1 1 d D . .
H51 H 0.3781 0.3000 0.6741 0.087 Uiso 1 1 calc R . .
C52 C 0.4405(4) 0.1884(4) 0.6983(3) 0.0790(17) Uani 1 1 d D . .
H52 H 0.4673 0.1940 0.7360 0.095 Uiso 1 1 calc R . .
C53 C 0.4539(3) 0.1184(4) 0.6814(2) 0.0717(15) Uani 1 1 d D . .
H53 H 0.4893 0.0755 0.7079 0.086 Uiso 1 1 calc R . .
C54 C 0.4164(3) 0.1086(3) 0.6257(2) 0.0561(13) Uani 1 1 d D . .
H54 H 0.4258 0.0595 0.6139 0.067 Uiso 1 1 calc R . .
V2 V 0.27432(4) 0.04644(4) 0.84106(3) 0.03330(18) Uani 1 1 d D . .
N3 N 0.21021(19) 0.05356(18) 0.75178(14) 0.0338(8) Uani 1 1 d D . .
N4 N 0.3187(2) 0.04737(17) 0.93574(15) 0.0350(8) Uani 1 1 d D . .
O6 O 0.24387(16) 0.15606(14) 0.82432(12) 0.0378(6) Uani 1 1 d D . .
O7 O 0.05196(17) 0.01996(16) 0.71685(13) 0.0448(7) Uani 1 1 d D . .
O8 O 0.19443(16) -0.01951(14) 0.89268(11) 0.0359(6) Uani 1 1 d D . .
O9 O 0.29814(19) 0.14328(15) 1.03088(14) 0.0497(7) Uani 1 1 d D . .
O10 O 0.37061(16) 0.00622(15) 0.81278(12) 0.0406(7) Uani 1 1 d D . .
C55 C 0.1988(2) 0.2125(2) 0.77919(18) 0.0347(10) Uani 1 1 d D . .
C56 C 0.1821(2) 0.2898(2) 0.78699(19) 0.0373(10) Uani 1 1 d D . .
C57 C 0.1384(3) 0.3459(2) 0.7369(2) 0.0441(11) Uani 1 1 d D . .
H57 H 0.1280 0.3981 0.7418 0.053 Uiso 1 1 calc R . .
C58 C 0.1086(3) 0.3309(3) 0.6792(2) 0.0463(11) Uani 1 1 d D A .
C59 C 0.1238(3) 0.2555(2) 0.67388(19) 0.0432(11) Uani 1 1 d D . .
H59 H 0.1044 0.2430 0.6359 0.052 Uiso 1 1 calc R . .
C60 C 0.1676(2) 0.1951(2) 0.72290(18) 0.0362(10) Uani 1 1 d D . .
C61 C 0.2102(3) 0.3120(2) 0.84910(19) 0.0399(10) Uani 1 1 d D . .
C62 C 0.1715(3) 0.2632(2) 0.9165(2) 0.0513(12) Uani 1 1 d D . .
H62A H 0.1061 0.2716 0.9181 0.077 Uiso 1 1 calc R . .
H62B H 0.1885 0.2788 0.9555 0.077 Uiso 1 1 calc R . .
H62C H 0.1951 0.2083 0.9188 0.077 Uiso 1 1 calc R . .
C63 C 0.3135(3) 0.2989(2) 0.8447(2) 0.0497(11) Uani 1 1 d D . .
H63A H 0.3373 0.2447 0.8435 0.075 Uiso 1 1 calc R . .
H63B H 0.3319 0.3111 0.8848 0.075 Uiso 1 1 calc R . .
H63C H 0.3369 0.3327 0.8028 0.075 Uiso 1 1 calc R . .
C64 C 0.1754(3) 0.3966(2) 0.8510(2) 0.0540(12) Uani 1 1 d D . .
H64A H 0.2029 0.4300 0.8109 0.081 Uiso 1 1 calc R . .
H64B H 0.1907 0.4071 0.8930 0.081 Uiso 1 1 calc R . .
H64C H 0.1102 0.4070 0.8504 0.081 Uiso 1 1 calc R . .
C65 C 0.0631(3) 0.3980(3) 0.6258(2) 0.0639(13) Uani 1 1 d DU . .
C66 C -0.0125(8) 0.4442(9) 0.6657(6) 0.076(4) Uani 0.67(3) 1 d PDU A 1
H66A H 0.0117 0.4586 0.7023 0.113 Uiso 0.67(3) 1 calc PR A 1
H66B H -0.0588 0.4122 0.6858 0.113 Uiso 0.67(3) 1 calc PR A 1
H66C H -0.0386 0.4911 0.6344 0.113 Uiso 0.67(3) 1 calc PR A 1
C67 C 0.1310(9) 0.4549(11) 0.5942(11) 0.122(6) Uani 0.67(3) 1 d PDU A 1
H67A H 0.1501 0.4733 0.6308 0.184 Uiso 0.67(3) 1 calc PR A 1
H67B H 0.1022 0.4991 0.5615 0.184 Uiso 0.67(3) 1 calc PR A 1
H67C H 0.1833 0.4279 0.5704 0.184 Uiso 0.67(3) 1 calc PR A 1
C68 C 0.0262(14) 0.3739(11) 0.5716(9) 0.108(6) Uani 0.67(3) 1 d PDU A 1
H68A H -0.0021 0.4199 0.5404 0.162 Uiso 0.67(3) 1 calc PR A 1
H68B H -0.0184 0.3405 0.5929 0.162 Uiso 0.67(3) 1 calc PR A 1
H68C H 0.0747 0.3453 0.5458 0.162 Uiso 0.67(3) 1 calc PR A 1
C66X C 0.018(3) 0.4712(13) 0.6473(15) 0.113(10) Uani 0.33(3) 1 d PDU A 2
H66D H -0.0072 0.5084 0.6078 0.170 Uiso 0.33(3) 1 calc PR A 2
H66E H 0.0612 0.4934 0.6644 0.170 Uiso 0.33(3) 1 calc PR A 2
H66F H -0.0307 0.4596 0.6837 0.170 Uiso 0.33(3) 1 calc PR A 2
C67X C 0.1375(13) 0.414(2) 0.5646(12) 0.097(9) Uani 0.33(3) 1 d PDU A 2
H67D H 0.1642 0.3653 0.5508 0.145 Uiso 0.33(3) 1 calc PR A 2
H67E H 0.1840 0.4355 0.5789 0.145 Uiso 0.33(3) 1 calc PR A 2
H67F H 0.1110 0.4509 0.5257 0.145 Uiso 0.33(3) 1 calc PR A 2
C68X C -0.003(2) 0.3652(18) 0.5947(16) 0.082(8) Uani 0.33(3) 1 d PDU A 2
H68D H 0.0291 0.3218 0.5749 0.122 Uiso 0.33(3) 1 calc PR A 2
H68E H -0.0312 0.4058 0.5588 0.122 Uiso 0.33(3) 1 calc PR A 2
H68F H -0.0492 0.3470 0.6307 0.122 Uiso 0.33(3) 1 calc PR A 2
C69 C 0.1768(2) 0.1187(2) 0.71255(18) 0.0348(10) Uani 1 1 d D . .
H69 H 0.1560 0.1145 0.6717 0.042 Uiso 1 1 calc R . .
C70 C 0.2090(3) -0.0155(2) 0.72843(17) 0.0332(9) Uani 1 1 d D . .
C71 C 0.2867(3) -0.0698(2) 0.72505(17) 0.0373(10) Uani 1 1 d D . .
H71 H 0.3399 -0.0605 0.7384 0.045 Uiso 1 1 calc R . .
C72 C 0.2883(3) -0.1366(2) 0.70276(19) 0.0464(11) Uani 1 1 d D . .
H72 H 0.3422 -0.1725 0.7003 0.056 Uiso 1 1 calc R . .
C73 C 0.2101(3) -0.1509(3) 0.6839(2) 0.0500(11) Uani 1 1 d D . .
H73 H 0.2104 -0.1971 0.6691 0.060 Uiso 1 1 calc R . .
C74 C 0.1325(3) -0.0982(3) 0.68687(19) 0.0456(11) Uani 1 1 d D . .
H74 H 0.0793 -0.1078 0.6737 0.055 Uiso 1 1 calc R . .
C75 C 0.1316(3) -0.0312(2) 0.70890(18) 0.0378(10) Uani 1 1 d D . .
C76 C -0.0060(3) 0.0370(2) 0.6662(2) 0.0403(10) Uani 1 1 d D . .
C77 C 0.0245(3) 0.0514(2) 0.5968(2) 0.0491(11) Uani 1 1 d D . .
H77 H 0.0868 0.0476 0.5825 0.059 Uiso 1 1 calc R . .
C78 C -0.0364(3) 0.0713(2) 0.5489(2) 0.0528(12) Uani 1 1 d D . .
H78 H -0.0160 0.0818 0.5014 0.063 Uiso 1 1 calc R . .
C79 C -0.1270(3) 0.0761(3) 0.5695(2) 0.0612(13) Uani 1 1 d D . .
H79 H -0.1689 0.0891 0.5364 0.073 Uiso 1 1 calc R . .
C80 C -0.1558(3) 0.0618(3) 0.6384(2) 0.0639(14) Uani 1 1 d D . .
H80 H -0.2181 0.0657 0.6527 0.077 Uiso 1 1 calc R . .
C81 C -0.0956(3) 0.0419(2) 0.6873(2) 0.0491(11) Uani 1 1 d D . .
H81 H -0.1161 0.0318 0.7348 0.059 Uiso 1 1 calc R . .
C82 C 0.1827(2) -0.0586(2) 0.95794(18) 0.0325(9) Uani 1 1 d D . .
C83 C 0.1173(2) -0.1073(2) 0.97835(18) 0.0373(10) Uani 1 1 d D . .
C84 C 0.1142(3) -0.1517(2) 1.04462(19) 0.0436(11) Uani 1 1 d D . .
H84 H 0.0710 -0.1854 1.0577 0.052 Uiso 1 1 calc R . .
C85 C 0.1698(3) -0.1511(2) 1.09426(18) 0.0389(10) Uani 1 1 d D . .
C86 C 0.2292(3) -0.1002(2) 1.07453(18) 0.0384(10) Uani 1 1 d D . .
H86 H 0.2665 -0.0962 1.1068 0.046 Uiso 1 1 calc R . .
C87 C 0.2367(2) -0.0530(2) 1.00719(18) 0.0345(9) Uani 1 1 d D . .
C88 C 0.0528(3) -0.1124(3) 0.9284(2) 0.0477(11) Uani 1 1 d D . .
C89 C 0.0053(3) -0.0313(3) 0.8952(2) 0.0609(13) Uani 1 1 d D . .
H89A H -0.0283 -0.0059 0.9311 0.091 Uiso 1 1 calc R . .
H89B H -0.0360 -0.0362 0.8642 0.091 Uiso 1 1 calc R . .
H89C H 0.0499 -0.0001 0.8692 0.091 Uiso 1 1 calc R . .
C90 C 0.1056(3) -0.1533(3) 0.8733(2) 0.0604(13) Uani 1 1 d D . .
H90A H 0.1547 -0.1257 0.8503 0.091 Uiso 1 1 calc R . .
H90B H 0.0658 -0.1538 0.8395 0.091 Uiso 1 1 calc R . .
H90C H 0.1301 -0.2067 0.8947 0.091 Uiso 1 1 calc R . .
C91 C -0.0207(3) -0.1593(3) 0.9659(2) 0.0848(18) Uani 1 1 d D . .
H91A H 0.0069 -0.2115 0.9877 0.127 Uiso 1 1 calc R . .
H91B H -0.0601 -0.1626 0.9329 0.127 Uiso 1 1 calc R . .
H91C H -0.0557 -0.1336 1.0011 0.127 Uiso 1 1 calc R . .
C92 C 0.1608(3) -0.2057(3) 1.16495(19) 0.0482(11) Uani 1 1 d D . .
C93 C 0.0658(3) -0.1863(3) 1.2012(2) 0.0661(14) Uani 1 1 d D . .
H93A H 0.0613 -0.2197 1.2473 0.099 Uiso 1 1 calc R . .
H93B H 0.0215 -0.1951 1.1746 0.099 Uiso 1 1 calc R . .
H93C H 0.0545 -0.1320 1.2047 0.099 Uiso 1 1 calc R . .
C94 C 0.1763(3) -0.2902(3) 1.1565(2) 0.0684(14) Uani 1 1 d D . .
H94A H 0.2358 -0.3024 1.1326 0.103 Uiso 1 1 calc R . .
H94B H 0.1307 -0.2966 1.1298 0.103 Uiso 1 1 calc R . .
H94C H 0.1721 -0.3252 1.2019 0.103 Uiso 1 1 calc R . .
C95 C 0.2289(3) -0.1983(3) 1.2106(2) 0.0593(13) Uani 1 1 d D . .
H95A H 0.2897 -0.2125 1.1893 0.089 Uiso 1 1 calc R . .
H95B H 0.2204 -0.2330 1.2557 0.089 Uiso 1 1 calc R . .
H95C H 0.2204 -0.1447 1.2160 0.089 Uiso 1 1 calc R . .
C96 C 0.3002(2) -0.0006(2) 0.99326(19) 0.0383(10) Uani 1 1 d D . .
H96 H 0.3324 -0.0011 1.0303 0.046 Uiso 1 1 calc R . .
C97 C 0.3840(3) 0.0952(2) 0.9375(2) 0.0400(10) Uani 1 1 d D . .
C98 C 0.4584(3) 0.0972(2) 0.8884(2) 0.0461(11) Uani 1 1 d D . .
H98 H 0.4646 0.0681 0.8541 0.055 Uiso 1 1 calc R . .
C99 C 0.5231(3) 0.1411(3) 0.8892(2) 0.0568(13) Uani 1 1 d D . .
H99 H 0.5734 0.1419 0.8555 0.068 Uiso 1 1 calc R . .
C100 C 0.5147(3) 0.1836(3) 0.9388(3) 0.0637(14) Uani 1 1 d D . .
H100 H 0.5598 0.2126 0.9402 0.076 Uiso 1 1 calc R . .
C101 C 0.4406(3) 0.1838(3) 0.9863(2) 0.0570(13) Uani 1 1 d D . .
H101 H 0.4335 0.2145 1.0195 0.068 Uiso 1 1 calc R . .
C102 C 0.3761(3) 0.1394(2) 0.9861(2) 0.0450(11) Uani 1 1 d D . .
C103 C 0.3046(3) 0.1164(2) 1.1012(2) 0.0459(11) Uani 1 1 d D . .
C104 C 0.2265(3) 0.1303(3) 1.1427(2) 0.0557(12) Uani 1 1 d D . .
H104 H 0.1735 0.1578 1.1233 0.067 Uiso 1 1 calc R . .
C105 C 0.2260(3) 0.1036(3) 1.2133(2) 0.0630(13) Uani 1 1 d D . .
H105 H 0.1722 0.1125 1.2423 0.076 Uiso 1 1 calc R . .
C106 C 0.3030(4) 0.0644(3) 1.2414(2) 0.0636(14) Uani 1 1 d D . .
H106 H 0.3026 0.0468 1.2897 0.076 Uiso 1 1 calc R . .
C107 C 0.3807(3) 0.0508(3) 1.1994(2) 0.0593(13) Uani 1 1 d D . .
H107 H 0.4337 0.0237 1.2191 0.071 Uiso 1 1 calc R . .
C108 C 0.3827(3) 0.0761(2) 1.1285(2) 0.0513(12) Uani 1 1 d D . .
H108 H 0.4362 0.0659 1.0995 0.062 Uiso 1 1 calc R . .
N5 N 0.4350(4) 0.6320(3) 0.1402(3) 0.113(2) Uani 1 1 d D . .
C109 C 0.4398(4) 0.6407(3) 0.1937(3) 0.0792(17) Uani 1 1 d D . .
C110 C 0.4459(4) 0.6527(3) 0.2611(3) 0.0842(17) Uani 1 1 d D . .
H11A H 0.4517 0.7068 0.2574 0.126 Uiso 1 1 calc R . .
H11B H 0.4984 0.6185 0.2803 0.126 Uiso 1 1 calc R . .
H11C H 0.3918 0.6410 0.2912 0.126 Uiso 1 1 calc R . .
N6 N 0.4423(4) 0.4345(3) 0.5891(3) 0.120(2) Uani 1 1 d D . .
C111 C 0.4317(4) 0.4253(3) 0.5349(4) 0.0871(19) Uani 1 1 d D . .
C112 C 0.4199(4) 0.4166(3) 0.4644(3) 0.0852(17) Uani 1 1 d D . .
H11D H 0.3583 0.4382 0.4541 0.128 Uiso 1 1 calc R . .
H11E H 0.4322 0.3615 0.4631 0.128 Uiso 1 1 calc R . .
H11F H 0.4614 0.4443 0.4303 0.128 Uiso 1 1 calc R . .
N7 N 0.7336(4) 0.4451(4) 0.6741(3) 0.128(2) Uani 1 1 d D . .
C113 C 0.7363(4) 0.4970(4) 0.6944(3) 0.0816(17) Uani 1 1 d D . .
C114 C 0.7389(5) 0.5613(4) 0.7219(4) 0.136(3) Uani 1 1 d D . .
H11G H 0.6836 0.5718 0.7516 0.204 Uiso 1 1 calc R . .
H11H H 0.7447 0.6067 0.6844 0.204 Uiso 1 1 calc R . .
H11I H 0.7903 0.5500 0.7487 0.204 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 O5 1.596(2) . ?
V1 O3 1.903(2) . ?
V1 O1 1.916(2) . ?
V1 N1 2.121(3) . ?
V1 N2 2.121(3) . ?
O1 C1 1.339(4) . ?
N1 C15 1.293(4) . ?
N1 C16 1.456(4) . ?
C1 C6 1.403(5) . ?
C1 C2 1.416(5) . ?
O2 C22 1.394(4) . ?
O2 C21 1.394(5) . ?
N2 C42 1.296(5) . ?
N2 C43 1.442(5) . ?
C2 C3 1.393(5) . ?
C2 C7 1.543(5) . ?
O3 C28 1.340(4) . ?
C3 C4 1.399(5) . ?
O4 C48 1.389(5) . ?
O4 C49 1.392(5) . ?
C4 C5 1.386(5) . ?
C4 C11 1.540(5) . ?
C5 C6 1.407(5) . ?
C6 C15 1.439(5) . ?
C7 C9 1.530(6) . ?
C7 C8 1.538(6) . ?
C7 C10 1.545(5) . ?
C11 C13 1.507(6) . ?
C11 C12 1.511(6) . ?
C11 C14 1.514(6) . ?
C16 C17 1.383(5) . ?
C16 C21 1.393(5) . ?
C17 C18 1.393(5) . ?
C18 C19 1.388(6) . ?
C19 C20 1.368(6) . ?
C20 C21 1.396(5) . ?
C22 C23 1.380(6) . ?
C22 C27 1.380(5) . ?
C23 C24 1.396(6) . ?
C24 C25 1.378(6) . ?
C25 C26 1.372(6) . ?
C26 C27 1.398(6) . ?
C28 C33 1.416(5) . ?
C28 C29 1.424(5) . ?
C29 C30 1.389(5) . ?
C29 C34 1.535(5) . ?
C30 C31 1.410(5) . ?
C31 C32 1.376(5) . ?
C31 C38 1.534(5) . ?
C32 C33 1.412(5) . ?
C33 C42 1.434(5) . ?
C34 C36 1.534(6) . ?
C34 C37 1.535(5) . ?
C34 C35 1.540(5) . ?
C38 C40 1.518(6) . ?
C38 C41 1.533(5) . ?
C38 C39 1.534(6) . ?
C43 C44 1.381(5) . ?
C43 C48 1.404(5) . ?
C44 C45 1.385(5) . ?
C45 C46 1.387(6) . ?
C46 C47 1.373(6) . ?
C47 C48 1.377(6) . ?
C49 C50 1.370(6) . ?
C49 C54 1.382(6) . ?
C50 C51 1.398(6) . ?
C51 C52 1.376(7) . ?
C52 C53 1.355(7) . ?
C53 C54 1.397(6) . ?
V2 O10 1.603(2) . ?
V2 O8 1.895(2) . ?
V2 O6 1.899(3) . ?
V2 N4 2.124(3) . ?
V2 N3 2.140(3) . ?
N3 C69 1.306(4) . ?
N3 C70 1.438(5) . ?
N4 C96 1.301(4) . ?
N4 C97 1.450(5) . ?
O6 C55 1.343(4) . ?
O7 C76 1.391(4) . ?
O7 C75 1.395(4) . ?
O8 C82 1.341(4) . ?
O9 C102 1.391(5) . ?
O9 C103 1.396(5) . ?
C55 C56 1.412(5) . ?
C55 C60 1.416(5) . ?
C56 C57 1.391(5) . ?
C56 C61 1.543(5) . ?
C57 C58 1.412(5) . ?
C58 C59 1.362(5) . ?
C58 C65 1.540(6) . ?
C59 C60 1.417(5) . ?
C60 C69 1.419(5) . ?
C61 C64 1.524(5) . ?
C61 C62 1.538(5) . ?
C61 C63 1.546(5) . ?
C65 C68 1.487(10) . ?
C65 C66X 1.499(13) . ?
C65 C68X 1.538(13) . ?
C65 C66 1.538(9) . ?
C65 C67 1.562(10) . ?
C65 C67X 1.568(14) . ?
C70 C71 1.392(5) . ?
C70 C75 1.400(5) . ?
C71 C72 1.380(5) . ?
C72 C73 1.393(6) . ?
C73 C74 1.376(5) . ?
C74 C75 1.381(5) . ?
C76 C81 1.368(5) . ?
C76 C77 1.390(5) . ?
C77 C78 1.378(5) . ?
C78 C79 1.380(6) . ?
C79 C80 1.376(6) . ?
C80 C81 1.384(6) . ?
C82 C83 1.410(5) . ?
C82 C87 1.414(5) . ?
C83 C84 1.383(5) . ?
C83 C88 1.538(5) . ?
C84 C85 1.408(5) . ?
C85 C86 1.368(5) . ?
C85 C92 1.530(5) . ?
C86 C87 1.421(5) . ?
C87 C96 1.436(5) . ?
C88 C90 1.531(6) . ?
C88 C91 1.538(6) . ?
C88 C89 1.541(6) . ?
C92 C95 1.531(6) . ?
C92 C94 1.543(6) . ?
C92 C93 1.547(6) . ?
C97 C102 1.384(5) . ?
C97 C98 1.398(5) . ?
C98 C99 1.386(6) . ?
C99 C100 1.380(6) . ?
C100 C101 1.376(6) . ?
C101 C102 1.386(6) . ?
C103 C104 1.375(6) . ?
C103 C108 1.387(6) . ?
C104 C105 1.389(6) . ?
C105 C106 1.375(6) . ?
C106 C107 1.374(6) . ?
C107 C108 1.391(6) . ?
N5 C109 1.144(7) . ?
C109 C110 1.447(8) . ?
N6 C111 1.184(8) . ?
C111 C112 1.508(8) . ?
N7 C113 1.120(7) . ?
C113 C114 1.409(8) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O5 V1 O3 116.47(12) . . ?
O5 V1 O1 121.00(12) . . ?
O3 V1 O1 122.49(11) . . ?
O5 V1 N1 95.51(12) . . ?
O3 V1 N1 89.75(11) . . ?
O1 V1 N1 86.89(11) . . ?
O5 V1 N2 93.06(12) . . ?
O3 V1 N2 87.40(11) . . ?
O1 V1 N2 87.76(11) . . ?
N1 V1 N2 171.36(12) . . ?
C1 O1 V1 136.2(2) . . ?
C15 N1 C16 114.2(3) . . ?
C15 N1 V1 124.5(2) . . ?
C16 N1 V1 121.1(2) . . ?
O1 C1 C6 120.4(3) . . ?
O1 C1 C2 120.7(3) . . ?
C6 C1 C2 118.9(3) . . ?
C22 O2 C21 119.8(3) . . ?
C42 N2 C43 115.2(3) . . ?
C42 N2 V1 123.4(2) . . ?
C43 N2 V1 120.7(2) . . ?
C3 C2 C1 117.5(3) . . ?
C3 C2 C7 121.0(3) . . ?
C1 C2 C7 121.5(3) . . ?
C28 O3 V1 135.8(2) . . ?
C2 C3 C4 125.4(4) . . ?
C48 O4 C49 119.5(3) . . ?
C5 C4 C3 115.4(4) . . ?
C5 C4 C11 120.9(4) . . ?
C3 C4 C11 123.6(4) . . ?
C4 C5 C6 122.2(4) . . ?
C1 C6 C5 120.6(3) . . ?
C1 C6 C15 123.7(3) . . ?
C5 C6 C15 115.7(3) . . ?
C9 C7 C8 111.0(4) . . ?
C9 C7 C2 109.3(3) . . ?
C8 C7 C2 109.5(4) . . ?
C9 C7 C10 107.8(4) . . ?
C8 C7 C10 107.0(4) . . ?
C2 C7 C10 112.2(3) . . ?
C13 C11 C12 109.7(4) . . ?
C13 C11 C14 109.3(5) . . ?
C12 C11 C14 107.0(4) . . ?
C13 C11 C4 108.7(4) . . ?
C12 C11 C4 112.9(4) . . ?
C14 C11 C4 109.2(4) . . ?
N1 C15 C6 127.8(3) . . ?
C17 C16 C21 120.0(4) . . ?
C17 C16 N1 119.9(3) . . ?
C21 C16 N1 120.1(3) . . ?
C16 C17 C18 119.7(4) . . ?
C19 C18 C17 120.0(4) . . ?
C20 C19 C18 120.6(4) . . ?
C19 C20 C21 119.8(4) . . ?
C16 C21 O2 119.5(3) . . ?
C16 C21 C20 119.9(4) . . ?
O2 C21 C20 120.2(4) . . ?
C23 C22 C27 121.4(4) . . ?
C23 C22 O2 114.8(4) . . ?
C27 C22 O2 123.8(4) . . ?
C22 C23 C24 119.4(4) . . ?
C25 C24 C23 119.9(5) . . ?
C26 C25 C24 119.7(4) . . ?
C25 C26 C27 121.5(4) . . ?
C22 C27 C26 118.0(4) . . ?
O3 C28 C33 120.2(3) . . ?
O3 C28 C29 120.9(3) . . ?
C33 C28 C29 119.0(3) . . ?
C30 C29 C28 117.3(3) . . ?
C30 C29 C34 121.3(3) . . ?
C28 C29 C34 121.5(3) . . ?
C29 C30 C31 125.4(4) . . ?
C32 C31 C30 115.8(4) . . ?
C32 C31 C38 123.9(4) . . ?
C30 C31 C38 120.3(4) . . ?
C31 C32 C33 122.3(4) . . ?
C32 C33 C28 120.2(4) . . ?
C32 C33 C42 116.2(3) . . ?
C28 C33 C42 123.6(3) . . ?
C36 C34 C29 109.4(3) . . ?
C36 C34 C37 108.0(4) . . ?
C29 C34 C37 111.8(3) . . ?
C36 C34 C35 110.7(3) . . ?
C29 C34 C35 109.7(3) . . ?
C37 C34 C35 107.3(3) . . ?
C40 C38 C41 108.0(4) . . ?
C40 C38 C39 109.8(4) . . ?
C41 C38 C39 108.6(3) . . ?
C40 C38 C31 110.1(3) . . ?
C41 C38 C31 111.8(3) . . ?
C39 C38 C31 108.5(3) . . ?
N2 C42 C33 128.2(3) . . ?
C44 C43 C48 118.4(4) . . ?
C44 C43 N2 119.9(3) . . ?
C48 C43 N2 121.7(4) . . ?
C43 C44 C45 121.0(4) . . ?
C44 C45 C46 119.9(5) . . ?
C47 C46 C45 119.6(4) . . ?
C46 C47 C48 120.8(4) . . ?
C47 C48 O4 121.1(4) . . ?
C47 C48 C43 120.3(4) . . ?
O4 C48 C43 118.4(4) . . ?
C50 C49 C54 121.4(4) . . ?
C50 C49 O4 115.0(4) . . ?
C54 C49 O4 123.6(4) . . ?
C49 C50 C51 119.4(5) . . ?
C52 C51 C50 119.3(5) . . ?
C53 C52 C51 120.7(5) . . ?
C52 C53 C54 121.0(5) . . ?
C49 C54 C53 118.1(5) . . ?
O10 V2 O8 117.40(12) . . ?
O10 V2 O6 120.58(12) . . ?
O8 V2 O6 122.01(11) . . ?
O10 V2 N4 93.01(12) . . ?
O8 V2 N4 87.11(11) . . ?
O6 V2 N4 88.91(11) . . ?
O10 V2 N3 95.71(12) . . ?
O8 V2 N3 88.83(11) . . ?
O6 V2 N3 86.70(11) . . ?
N4 V2 N3 171.28(12) . . ?
C69 N3 C70 115.9(3) . . ?
C69 N3 V2 123.8(3) . . ?
C70 N3 V2 120.1(2) . . ?
C96 N4 C97 115.1(3) . . ?
C96 N4 V2 123.9(3) . . ?
C97 N4 V2 120.4(2) . . ?
C55 O6 V2 136.9(2) . . ?
C76 O7 C75 118.1(3) . . ?
C82 O8 V2 135.9(2) . . ?
C102 O9 C103 118.7(3) . . ?
O6 C55 C56 120.6(3) . . ?
O6 C55 C60 120.3(3) . . ?
C56 C55 C60 119.1(3) . . ?
C57 C56 C55 117.7(4) . . ?
C57 C56 C61 120.6(4) . . ?
C55 C56 C61 121.6(3) . . ?
C56 C57 C58 124.6(4) . . ?
C59 C58 C57 116.3(4) . . ?
C59 C58 C65 123.6(4) . . ?
C57 C58 C65 120.2(4) . . ?
C58 C59 C60 122.4(4) . . ?
C55 C60 C59 119.8(4) . . ?
C55 C60 C69 123.4(3) . . ?
C59 C60 C69 116.8(4) . . ?
C64 C61 C62 106.6(3) . . ?
C64 C61 C56 112.2(3) . . ?
C62 C61 C56 110.3(3) . . ?
C64 C61 C63 108.2(3) . . ?
C62 C61 C63 110.5(3) . . ?
C56 C61 C63 109.0(3) . . ?
C66X C65 C68X 110.0(16) . . ?
C68 C65 C66 109.7(8) . . ?
C68 C65 C58 114.8(8) . . ?
C66X C65 C58 119.1(12) . . ?
C68X C65 C58 107.1(12) . . ?
C66 C65 C58 106.7(6) . . ?
C68 C65 C67 111.4(8) . . ?
C66 C65 C67 105.2(7) . . ?
C58 C65 C67 108.4(6) . . ?
C66X C65 C67X 111.7(11) . . ?
C68X C65 C67X 102.5(12) . . ?
C58 C65 C67X 105.0(9) . . ?
N3 C69 C60 128.5(4) . . ?
C71 C70 C75 117.7(4) . . ?
C71 C70 N3 120.0(3) . . ?
C75 C70 N3 122.4(3) . . ?
C72 C71 C70 121.7(4) . . ?
C71 C72 C73 119.4(4) . . ?
C74 C73 C72 120.0(4) . . ?
C73 C74 C75 120.2(4) . . ?
C74 C75 O7 120.7(4) . . ?
C74 C75 C70 121.0(4) . . ?
O7 C75 C70 118.1(4) . . ?
C81 C76 C77 120.8(4) . . ?
C81 C76 O7 117.2(3) . . ?
C77 C76 O7 122.0(4) . . ?
C78 C77 C76 119.3(4) . . ?
C77 C78 C79 120.5(4) . . ?
C80 C79 C78 119.2(4) . . ?
C79 C80 C81 121.2(4) . . ?
C76 C81 C80 119.0(4) . . ?
O8 C82 C83 120.4(3) . . ?
O8 C82 C87 120.7(3) . . ?
C83 C82 C87 118.8(3) . . ?
C84 C83 C82 117.6(4) . . ?
C84 C83 C88 121.0(3) . . ?
C82 C83 C88 121.4(3) . . ?
C83 C84 C85 125.4(4) . . ?
C86 C85 C84 115.8(3) . . ?
C86 C85 C92 124.5(4) . . ?
C84 C85 C92 119.6(4) . . ?
C85 C86 C87 122.0(4) . . ?
C82 C87 C86 120.1(4) . . ?
C82 C87 C96 123.3(3) . . ?
C86 C87 C96 116.7(3) . . ?
C90 C88 C91 108.3(4) . . ?
C90 C88 C83 108.9(3) . . ?
C91 C88 C83 111.0(3) . . ?
C90 C88 C89 110.5(3) . . ?
C91 C88 C89 106.9(4) . . ?
C83 C88 C89 111.1(3) . . ?
C85 C92 C95 111.7(3) . . ?
C85 C92 C94 109.4(3) . . ?
C95 C92 C94 108.5(4) . . ?
C85 C92 C93 109.8(3) . . ?
C95 C92 C93 108.4(3) . . ?
C94 C92 C93 109.1(4) . . ?
N4 C96 C87 127.4(3) . . ?
C102 C97 C98 118.1(4) . . ?
C102 C97 N4 122.8(4) . . ?
C98 C97 N4 119.1(4) . . ?
C99 C98 C97 120.8(4) . . ?
C100 C99 C98 120.0(5) . . ?
C101 C100 C99 119.7(4) . . ?
C100 C101 C102 120.4(4) . . ?
C97 C102 C101 120.9(4) . . ?
C97 C102 O9 118.2(4) . . ?
C101 C102 O9 120.7(4) . . ?
C104 C103 C108 121.2(4) . . ?
C104 C103 O9 115.3(4) . . ?
C108 C103 O9 123.4(4) . . ?
C103 C104 C105 119.4(4) . . ?
C106 C105 C104 120.3(5) . . ?
C107 C106 C105 119.9(4) . . ?
C106 C107 C108 121.0(4) . . ?
C103 C108 C107 118.3(4) . . ?
N5 C109 C110 179.4(7) . . ?
N6 C111 C112 177.6(7) . . ?
N7 C113 C114 178.3(7) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
V1 O1 C1 C6 6.8(6) . . . . ?
V1 O1 C1 C2 -173.5(3) . . . . ?
O1 C1 C2 C3 179.1(4) . . . . ?
C6 C1 C2 C3 -1.1(6) . . . . ?
O1 C1 C2 C7 -1.1(6) . . . . ?
C6 C1 C2 C7 178.7(4) . . . . ?
C1 C2 C3 C4 1.0(6) . . . . ?
C7 C2 C3 C4 -178.8(4) . . . . ?
C2 C3 C4 C5 -0.3(6) . . . . ?
C2 C3 C4 C11 -178.3(4) . . . . ?
C3 C4 C5 C6 -0.3(6) . . . . ?
C11 C4 C5 C6 177.8(4) . . . . ?
O1 C1 C6 C5 -179.6(3) . . . . ?
C2 C1 C6 C5 0.6(6) . . . . ?
O1 C1 C6 C15 -1.6(6) . . . . ?
C2 C1 C6 C15 178.6(4) . . . . ?
C4 C5 C6 C1 0.2(6) . . . . ?
C4 C5 C6 C15 -178.0(4) . . . . ?
C3 C2 C7 C9 117.5(4) . . . . ?
C1 C2 C7 C9 -62.2(5) . . . . ?
C3 C2 C7 C8 -120.6(4) . . . . ?
C1 C2 C7 C8 59.6(5) . . . . ?
C3 C2 C7 C10 -2.0(6) . . . . ?
C1 C2 C7 C10 178.3(4) . . . . ?
C5 C4 C11 C13 58.6(6) . . . . ?
C3 C4 C11 C13 -123.5(5) . . . . ?
C5 C4 C11 C12 -179.5(4) . . . . ?
C3 C4 C11 C12 -1.6(6) . . . . ?
C5 C4 C11 C14 -60.6(5) . . . . ?
C3 C4 C11 C14 117.3(5) . . . . ?
C16 N1 C15 C6 -176.5(3) . . . . ?
V1 N1 C15 C6 8.2(5) . . . . ?
C1 C6 C15 N1 -6.1(6) . . . . ?
C5 C6 C15 N1 172.1(4) . . . . ?
C15 N1 C16 C17 -125.8(4) . . . . ?
V1 N1 C16 C17 49.7(4) . . . . ?
C15 N1 C16 C21 53.9(5) . . . . ?
V1 N1 C16 C21 -130.6(3) . . . . ?
C21 C16 C17 C18 -0.6(6) . . . . ?
N1 C16 C17 C18 179.1(3) . . . . ?
C16 C17 C18 C19 0.7(6) . . . . ?
C17 C18 C19 C20 0.0(6) . . . . ?
C18 C19 C20 C21 -0.8(6) . . . . ?
C17 C16 C21 O2 -173.5(3) . . . . ?
N1 C16 C21 O2 6.8(5) . . . . ?
C17 C16 C21 C20 -0.1(6) . . . . ?
N1 C16 C21 C20 -179.8(3) . . . . ?
C22 O2 C21 C16 -113.6(4) . . . . ?
C22 O2 C21 C20 73.0(5) . . . . ?
C19 C20 C21 C16 0.8(6) . . . . ?
C19 C20 C21 O2 174.2(4) . . . . ?
C21 O2 C22 C23 174.0(3) . . . . ?
C21 O2 C22 C27 -5.4(5) . . . . ?
C27 C22 C23 C24 3.1(6) . . . . ?
O2 C22 C23 C24 -176.3(3) . . . . ?
C22 C23 C24 C25 -2.3(6) . . . . ?
C23 C24 C25 C26 -0.3(7) . . . . ?
C24 C25 C26 C27 2.2(7) . . . . ?
C23 C22 C27 C26 -1.2(6) . . . . ?
O2 C22 C27 C26 178.1(4) . . . . ?
C25 C26 C27 C22 -1.5(6) . . . . ?
V1 O3 C28 C33 -5.9(5) . . . . ?
V1 O3 C28 C29 173.9(3) . . . . ?
O3 C28 C29 C30 -177.5(3) . . . . ?
C33 C28 C29 C30 2.4(5) . . . . ?
O3 C28 C29 C34 1.6(6) . . . . ?
C33 C28 C29 C34 -178.6(3) . . . . ?
C28 C29 C30 C31 -0.8(6) . . . . ?
C34 C29 C30 C31 -179.9(4) . . . . ?
C29 C30 C31 C32 -1.2(6) . . . . ?
C29 C30 C31 C38 178.3(4) . . . . ?
C30 C31 C32 C33 1.8(6) . . . . ?
C38 C31 C32 C33 -177.7(4) . . . . ?
C31 C32 C33 C28 -0.3(6) . . . . ?
C31 C32 C33 C42 179.8(4) . . . . ?
O3 C28 C33 C32 178.0(3) . . . . ?
C29 C28 C33 C32 -1.8(5) . . . . ?
O3 C28 C33 C42 -2.2(5) . . . . ?
C29 C28 C33 C42 178.0(3) . . . . ?
C30 C29 C34 C36 113.0(4) . . . . ?
C28 C29 C34 C36 -66.1(5) . . . . ?
C30 C29 C34 C37 -6.6(5) . . . . ?
C28 C29 C34 C37 174.3(4) . . . . ?
C30 C29 C34 C35 -125.5(4) . . . . ?
C28 C29 C34 C35 55.5(5) . . . . ?
C32 C31 C38 C40 -125.0(4) . . . . ?
C30 C31 C38 C40 55.5(5) . . . . ?
C32 C31 C38 C41 -4.9(6) . . . . ?
C30 C31 C38 C41 175.6(4) . . . . ?
C32 C31 C38 C39 114.9(4) . . . . ?
C30 C31 C38 C39 -64.6(5) . . . . ?
C43 N2 C42 C33 -179.3(4) . . . . ?
V1 N2 C42 C33 10.6(6) . . . . ?
C32 C33 C42 N2 178.4(4) . . . . ?
C28 C33 C42 N2 -1.5(6) . . . . ?
C42 N2 C43 C44 -125.7(4) . . . . ?
V1 N2 C43 C44 44.7(4) . . . . ?
C42 N2 C43 C48 53.0(5) . . . . ?
V1 N2 C43 C48 -136.7(3) . . . . ?
C48 C43 C44 C45 -1.4(6) . . . . ?
N2 C43 C44 C45 177.3(3) . . . . ?
C43 C44 C45 C46 -0.7(6) . . . . ?
C44 C45 C46 C47 2.5(6) . . . . ?
C45 C46 C47 C48 -2.1(7) . . . . ?
C46 C47 C48 O4 174.6(4) . . . . ?
C46 C47 C48 C43 -0.1(6) . . . . ?
C49 O4 C48 C47 72.6(5) . . . . ?
C49 O4 C48 C43 -112.6(4) . . . . ?
C44 C43 C48 C47 1.8(6) . . . . ?
N2 C43 C48 C47 -176.9(3) . . . . ?
C44 C43 C48 O4 -173.0(3) . . . . ?
N2 C43 C48 O4 8.3(5) . . . . ?
C48 O4 C49 C50 178.1(3) . . . . ?
C48 O4 C49 C54 -0.7(5) . . . . ?
C54 C49 C50 C51 0.0(6) . . . . ?
O4 C49 C50 C51 -178.8(4) . . . . ?
C49 C50 C51 C52 0.9(7) . . . . ?
C50 C51 C52 C53 -1.4(8) . . . . ?
C51 C52 C53 C54 0.9(8) . . . . ?
C50 C49 C54 C53 -0.5(6) . . . . ?
O4 C49 C54 C53 178.2(4) . . . . ?
C52 C53 C54 C49 0.0(7) . . . . ?
O10 V2 O6 C55 97.6(3) . . . . ?
O8 V2 O6 C55 -83.7(3) . . . . ?
N4 V2 O6 C55 -169.6(3) . . . . ?
N3 V2 O6 C55 2.9(3) . . . . ?
O10 V2 O8 C82 81.7(3) . . . . ?
O6 V2 O8 C82 -97.1(3) . . . . ?
N4 V2 O8 C82 -10.2(3) . . . . ?
N3 V2 O8 C82 177.5(3) . . . . ?
V2 O6 C55 C56 173.7(2) . . . . ?
V2 O6 C55 C60 -6.5(5) . . . . ?
O6 C55 C56 C57 177.3(3) . . . . ?
C60 C55 C56 C57 -2.5(5) . . . . ?
O6 C55 C56 C61 -3.3(5) . . . . ?
C60 C55 C56 C61 176.9(3) . . . . ?
C55 C56 C57 C58 0.9(6) . . . . ?
C61 C56 C57 C58 -178.6(4) . . . . ?
C56 C57 C58 C59 0.6(6) . . . . ?
C56 C57 C58 C65 -178.3(4) . . . . ?
C57 C58 C59 C60 -0.4(6) . . . . ?
C65 C58 C59 C60 178.5(4) . . . . ?
O6 C55 C60 C59 -177.1(3) . . . . ?
C56 C55 C60 C59 2.7(5) . . . . ?
O6 C55 C60 C69 3.6(5) . . . . ?
C56 C55 C60 C69 -176.6(3) . . . . ?
C58 C59 C60 C55 -1.3(6) . . . . ?
C58 C59 C60 C69 178.1(4) . . . . ?
C57 C56 C61 C64 6.4(5) . . . . ?
C55 C56 C61 C64 -173.0(3) . . . . ?
C57 C56 C61 C62 125.0(4) . . . . ?
C55 C56 C61 C62 -54.4(5) . . . . ?
C57 C56 C61 C63 -113.5(4) . . . . ?
C55 C56 C61 C63 67.1(4) . . . . ?
C59 C58 C65 C68 7.4(11) . . . . ?
C57 C58 C65 C68 -173.8(10) . . . . ?
C59 C58 C65 C66X 156(2) . . . . ?
C57 C58 C65 C66X -25(2) . . . . ?
C59 C58 C65 C68X 30.9(16) . . . . ?
C57 C58 C65 C68X -150.3(16) . . . . ?
C59 C58 C65 C66 129.1(8) . . . . ?
C57 C58 C65 C66 -52.0(9) . . . . ?
C59 C58 C65 C67 -118.0(12) . . . . ?
C57 C58 C65 C67 60.8(12) . . . . ?
C59 C58 C65 C67X -77.6(18) . . . . ?
C57 C58 C65 C67X 101.2(17) . . . . ?
C70 N3 C69 C60 178.8(3) . . . . ?
V2 N3 C69 C60 -6.6(5) . . . . ?
C55 C60 C69 N3 3.0(6) . . . . ?
C59 C60 C69 N3 -176.3(4) . . . . ?
C69 N3 C70 C71 129.7(3) . . . . ?
V2 N3 C70 C71 -45.1(4) . . . . ?
C69 N3 C70 C75 -50.7(5) . . . . ?
V2 N3 C70 C75 134.5(3) . . . . ?
C75 C70 C71 C72 0.6(5) . . . . ?
N3 C70 C71 C72 -179.8(3) . . . . ?
C70 C71 C72 C73 -0.9(6) . . . . ?
C71 C72 C73 C74 0.8(6) . . . . ?
C72 C73 C74 C75 -0.5(6) . . . . ?
C73 C74 C75 O7 -175.3(3) . . . . ?
C73 C74 C75 C70 0.2(6) . . . . ?
C76 O7 C75 C74 -43.1(5) . . . . ?
C76 O7 C75 C70 141.2(3) . . . . ?
C71 C70 C75 C74 -0.2(5) . . . . ?
N3 C70 C75 C74 -179.8(3) . . . . ?
C71 C70 C75 O7 175.4(3) . . . . ?
N3 C70 C75 O7 -4.2(5) . . . . ?
C75 O7 C76 C81 139.5(4) . . . . ?
C75 O7 C76 C77 -42.9(5) . . . . ?
C81 C76 C77 C78 0.3(6) . . . . ?
O7 C76 C77 C78 -177.2(4) . . . . ?
C76 C77 C78 C79 -0.7(7) . . . . ?
C77 C78 C79 C80 0.9(7) . . . . ?
C78 C79 C80 C81 -0.7(7) . . . . ?
C77 C76 C81 C80 -0.2(6) . . . . ?
O7 C76 C81 C80 177.4(4) . . . . ?
C79 C80 C81 C76 0.4(7) . . . . ?
V2 O8 C82 C83 -176.2(3) . . . . ?
V2 O8 C82 C87 2.6(5) . . . . ?
O8 C82 C83 C84 174.0(3) . . . . ?
C87 C82 C83 C84 -4.9(5) . . . . ?
O8 C82 C83 C88 -4.7(6) . . . . ?
C87 C82 C83 C88 176.4(4) . . . . ?
C82 C83 C84 C85 1.6(6) . . . . ?
C88 C83 C84 C85 -179.7(4) . . . . ?
C83 C84 C85 C86 2.1(6) . . . . ?
C83 C84 C85 C92 -177.9(4) . . . . ?
C84 C85 C86 C87 -2.5(6) . . . . ?
C92 C85 C86 C87 177.6(4) . . . . ?
O8 C82 C87 C86 -174.2(3) . . . . ?
C83 C82 C87 C86 4.6(5) . . . . ?
O8 C82 C87 C96 6.3(6) . . . . ?
C83 C82 C87 C96 -174.9(3) . . . . ?
C85 C86 C87 C82 -0.8(6) . . . . ?
C85 C86 C87 C96 178.7(4) . . . . ?
C84 C83 C88 C90 -109.1(4) . . . . ?
C82 C83 C88 C90 69.6(5) . . . . ?
C84 C83 C88 C91 10.1(6) . . . . ?
C82 C83 C88 C91 -171.2(4) . . . . ?
C84 C83 C88 C89 129.0(4) . . . . ?
C82 C83 C88 C89 -52.3(5) . . . . ?
C86 C85 C92 C95 -1.9(6) . . . . ?
C84 C85 C92 C95 178.1(4) . . . . ?
C86 C85 C92 C94 -122.1(4) . . . . ?
C84 C85 C92 C94 57.9(5) . . . . ?
C86 C85 C92 C93 118.2(4) . . . . ?
C84 C85 C92 C93 -61.8(5) . . . . ?
C97 N4 C96 C87 177.9(4) . . . . ?
V2 N4 C96 C87 -11.2(5) . . . . ?
C82 C87 C96 N4 -0.9(6) . . . . ?
C86 C87 C96 N4 179.6(4) . . . . ?
C96 N4 C97 C102 -52.6(5) . . . . ?
V2 N4 C97 C102 136.2(3) . . . . ?
C96 N4 C97 C98 127.3(4) . . . . ?
V2 N4 C97 C98 -43.9(4) . . . . ?
C102 C97 C98 C99 1.2(6) . . . . ?
N4 C97 C98 C99 -178.8(3) . . . . ?
C97 C98 C99 C100 0.0(6) . . . . ?
C98 C99 C100 C101 -1.7(6) . . . . ?
C99 C100 C101 C102 2.3(6) . . . . ?
C98 C97 C102 C101 -0.6(6) . . . . ?
N4 C97 C102 C101 179.4(4) . . . . ?
C98 C97 C102 O9 174.0(3) . . . . ?
N4 C97 C102 O9 -6.0(5) . . . . ?
C100 C101 C102 C97 -1.1(6) . . . . ?
C100 C101 C102 O9 -175.6(4) . . . . ?
C103 O9 C102 C97 119.2(4) . . . . ?
C103 O9 C102 C101 -66.2(5) . . . . ?
C102 O9 C103 C104 172.7(4) . . . . ?
C102 O9 C103 C108 -9.4(6) . . . . ?
C108 C103 C104 C105 0.2(7) . . . . ?
O9 C103 C104 C105 178.2(4) . . . . ?
C103 C104 C105 C106 0.6(7) . . . . ?
C104 C105 C106 C107 -0.7(7) . . . . ?
C105 C106 C107 C108 -0.1(7) . . . . ?
C104 C103 C108 C107 -1.0(6) . . . . ?
O9 C103 C108 C107 -178.7(4) . . . . ?
C106 C107 C108 C103 0.9(7) . . . . ?

_refine_diff_density_max         0.439
_refine_diff_density_min         -0.300
_refine_diff_density_rms         0.047

_shelxl_version_number           2012-4

_iucr_refine_instruction_details 
; 
TITL cr485 in P-1 
CELL 0.71073  15.3075  18.0329  20.191  76.0289  81.7168  78.9101 
ZERR    4.00   0.0016   0.0018   0.002   0.0015   0.0015   0.0015 
LATT  1 
SFAC C H N O V 
UNIT 228 258 14 20 4 
TEMP -123 
SIZE 0.08 0.38 0.62 
  
ACTA 
CONF 
WPDB -1 
  
OMIT -3 45 
OMIT 0 1 0 
OMIT 0 0 1 
L.S. 8 
BOND 
FMAP 2 
PLAN 10 
  
SIMU C65 > C68X 
DELU C65 > C68X 
  
REM   EXTI    0.0002(2)  insig. 
WGHT    0.045500    3.386400 
FVAR       0.08197   0.66550 
V1    5    0.436668    0.200154    0.300167    11.00000    0.03186    0.04239 = 
         0.02250   -0.00139   -0.00132   -0.00582 
O1    4    0.308637    0.219268    0.315523    11.00000    0.03117    0.05284 = 
         0.02586   -0.00112    0.00006   -0.00410 
N1    3    0.422159    0.255628    0.196120    11.00000    0.03039    0.04303 = 
         0.02581   -0.00435    0.00073   -0.00634 
C1    1    0.241230    0.256035    0.278150    11.00000    0.03345    0.04587 = 
         0.03015   -0.00637   -0.00394   -0.00453 
O2    4    0.449416    0.400200    0.112191    11.00000    0.05413    0.04627 = 
         0.03216   -0.00088   -0.00798   -0.00922 
N2    3    0.438470    0.159744    0.407815    11.00000    0.03161    0.04760 = 
         0.02688   -0.00226   -0.00233   -0.00822 
C2    1    0.151890    0.265495    0.309123    11.00000    0.03520    0.05038 = 
         0.03074   -0.00267   -0.00244   -0.00275 
O3    4    0.508301    0.273336    0.305735    11.00000    0.04207    0.04405 = 
         0.02148   -0.00286   -0.00463   -0.01020 
C3    1    0.085403    0.305313    0.267198    11.00000    0.03169    0.05844 = 
         0.04510   -0.00689    0.00414   -0.00562 
AFIX  43 
H3    2    0.025661    0.312292    0.288260    11.00000   -1.20000 
AFIX   0 
O4    4    0.326366    0.170434    0.530468    11.00000    0.04537    0.07405 = 
         0.02732   -0.00651   -0.00235   -0.00454 
C4    1    0.099382    0.335865    0.196636    11.00000    0.03513    0.05283 = 
         0.03818   -0.00569   -0.00463   -0.00448 
O5    4    0.488901    0.119668    0.284596    11.00000    0.03923    0.04166 = 
         0.02969   -0.00317   -0.00175   -0.00289 
C5    1    0.187526    0.324683    0.168053    11.00000    0.04621    0.04658 = 
         0.02919   -0.00193   -0.00602   -0.00890 
AFIX  43 
H5    2    0.200746    0.344034    0.120253    11.00000   -1.20000 
AFIX   0 
C6    1    0.258082    0.285628    0.207466    11.00000    0.02844    0.04091 = 
         0.02959   -0.00421   -0.00160   -0.00763 
C7    1    0.128485    0.232825    0.386303    11.00000    0.03693    0.07286 = 
         0.03377   -0.00125    0.00536    0.00015 
C8    1    0.177995    0.268901    0.428464    11.00000    0.05260    0.09246 = 
         0.03051   -0.01468    0.00368   -0.00034 
AFIX 137 
H8A   2    0.242441    0.259205    0.414525    11.00000   -1.50000 
H8B   2    0.166307    0.245617    0.477347    11.00000   -1.50000 
H8C   2    0.156785    0.324871    0.420385    11.00000   -1.50000 
AFIX   0 
C9    1    0.154322    0.144552    0.401909    11.00000    0.03952    0.07824 = 
         0.04245    0.00721    0.00468   -0.00555 
AFIX 137 
H9A   2    0.118820    0.122717    0.376986    11.00000   -1.50000 
H9B   2    0.142623    0.123900    0.451307    11.00000   -1.50000 
H9C   2    0.218072    0.130501    0.387430    11.00000   -1.50000 
AFIX   0 
C10   1    0.027430    0.252420    0.408683    11.00000    0.04115    0.09760 = 
         0.04756   -0.00201    0.01460    0.00257 
AFIX 137 
H10A  2    0.008971    0.308779    0.398856    11.00000   -1.50000 
H10B  2    0.015679    0.231359    0.458006    11.00000   -1.50000 
H10C  2   -0.006454    0.229552    0.383383    11.00000   -1.50000 
AFIX   0 
C11   1    0.024095    0.381404    0.152579    11.00000    0.03817    0.06171 = 
         0.04829   -0.00724   -0.01183    0.00008 
C12   1   -0.066906    0.387746    0.193247    11.00000    0.03973    0.15230 = 
         0.08137    0.01778   -0.01429    0.00391 
AFIX 137 
H12A  2   -0.065631    0.412351    0.231315    11.00000   -1.50000 
H12B  2   -0.082392    0.335877    0.211460    11.00000   -1.50000 
H12C  2   -0.111727    0.419123    0.163347    11.00000   -1.50000 
AFIX   0 
C13   1    0.023064    0.342030    0.094877    11.00000    0.09120    0.14684 = 
         0.11334   -0.06732   -0.06951    0.04455 
AFIX 137 
H13A  2    0.011047    0.289168    0.113910    11.00000   -1.50000 
H13B  2    0.081301    0.340232    0.067298    11.00000   -1.50000 
H13C  2   -0.023826    0.371082    0.065896    11.00000   -1.50000 
AFIX   0 
C14   1    0.042211    0.463179    0.122989    11.00000    0.06186    0.08044 = 
         0.10539    0.00978   -0.02346    0.01306 
AFIX 137 
H14A  2   -0.006771    0.492936    0.096402    11.00000   -1.50000 
H14B  2    0.098600    0.461687    0.093019    11.00000   -1.50000 
H14C  2    0.046529    0.487841    0.160393    11.00000   -1.50000 
AFIX   0 
C15   1    0.346204    0.280823    0.170910    11.00000    0.03858    0.03723 = 
         0.02367   -0.00449   -0.00510   -0.00702 
AFIX  43 
H15   2    0.348915    0.298245    0.122455    11.00000   -1.20000 
AFIX   0 
C16   1    0.499876    0.262735    0.145507    11.00000    0.03229    0.05568 = 
         0.01904   -0.00309   -0.00321   -0.00913 
C17   1    0.563996    0.198379    0.140378    11.00000    0.03769    0.05149 = 
         0.02512   -0.00485   -0.00354   -0.00252 
AFIX  43 
H17   2    0.557945    0.149691    0.170236    11.00000   -1.20000 
AFIX   0 
C18   1    0.637506    0.205304    0.091210    11.00000    0.03893    0.08043 = 
         0.03433   -0.01373    0.00066   -0.00042 
AFIX  43 
H18   2    0.681421    0.161147    0.087135    11.00000   -1.20000 
AFIX   0 
C19   1    0.646619    0.276695    0.048166    11.00000    0.04312    0.09111 = 
         0.03323   -0.00545    0.00778   -0.01798 
AFIX  43 
H19   2    0.696872    0.281108    0.014699    11.00000   -1.20000 
AFIX   0 
C20   1    0.583909    0.340780    0.053478    11.00000    0.04640    0.07045 = 
         0.02818    0.00517   -0.00131   -0.01605 
AFIX  43 
H20   2    0.591005    0.389573    0.024204    11.00000   -1.20000 
AFIX   0 
C21   1    0.509436    0.334219    0.102079    11.00000    0.03988    0.05521 = 
         0.02105   -0.00185   -0.00566   -0.01123 
C22   1    0.391075    0.438411    0.063073    11.00000    0.04967    0.04213 = 
         0.03450    0.00511   -0.00738   -0.01767 
C23   1    0.328962    0.498329    0.081328    11.00000    0.05519    0.04918 = 
         0.04412   -0.00090    0.00191   -0.01341 
AFIX  43 
H23   2    0.330323    0.512809    0.123346    11.00000   -1.20000 
AFIX   0 
C24   1    0.264106    0.537486    0.037526    11.00000    0.04555    0.05748 = 
         0.06542    0.00762   -0.00251   -0.00806 
AFIX  43 
H24   2    0.219729    0.577563    0.050415    11.00000   -1.20000 
AFIX   0 
C25   1    0.264513    0.517949   -0.024444    11.00000    0.05363    0.06638 = 
         0.06864    0.01576   -0.02713   -0.01860 
AFIX  43 
H25   2    0.220281    0.544308   -0.054270    11.00000   -1.20000 
AFIX   0 
C26   1    0.329048    0.460290   -0.042870    11.00000    0.06737    0.06502 = 
         0.04580    0.00004   -0.02033   -0.02128 
AFIX  43 
H26   2    0.330201    0.448387   -0.086360    11.00000   -1.20000 
AFIX   0 
C27   1    0.393154    0.418647    0.000891    11.00000    0.06266    0.04577 = 
         0.04147    0.00176   -0.01291   -0.01360 
AFIX  43 
H27   2    0.436815    0.377989   -0.011780    11.00000   -1.20000 
AFIX   0 
C28   1    0.553498    0.284512    0.353657    11.00000    0.03075    0.03712 = 
         0.02949   -0.00621   -0.00042   -0.00073 
C29   1    0.608631    0.342960    0.337943    11.00000    0.04072    0.04636 = 
         0.02852   -0.00480   -0.00305   -0.01058 
C30   1    0.656040    0.348699    0.389726    11.00000    0.03865    0.04394 = 
         0.03958   -0.00958   -0.00099   -0.01134 
AFIX  43 
H30   2    0.693476    0.387213    0.379090    11.00000   -1.20000 
AFIX   0 
C31   1    0.653184    0.302076    0.456769    11.00000    0.04035    0.04552 = 
         0.03494   -0.00878   -0.00714   -0.00544 
C32   1    0.596993    0.247928    0.470874    11.00000    0.04112    0.04345 = 
         0.02724   -0.00549    0.00000   -0.00073 
AFIX  43 
H32   2    0.591525    0.216205    0.515782    11.00000   -1.20000 
AFIX   0 
C33   1    0.547144    0.237827    0.420957    11.00000    0.03179    0.04272 = 
         0.02547   -0.00414   -0.00299   -0.00540 
C34   1    0.616584    0.396667    0.266478    11.00000    0.05320    0.04607 = 
         0.03380    0.00461   -0.01001   -0.01830 
C35   1    0.522864    0.437824    0.247291    11.00000    0.06704    0.04754 = 
         0.04508    0.00084   -0.01642   -0.01098 
AFIX 137 
H35A  2    0.486493    0.399185    0.245816    11.00000   -1.50000 
H35B  2    0.528299    0.473092    0.202161    11.00000   -1.50000 
H35C  2    0.494150    0.467392    0.281684    11.00000   -1.50000 
AFIX   0 
C36   1    0.662792    0.349003    0.213952    11.00000    0.05088    0.07349 = 
         0.03202    0.00187   -0.00081   -0.02305 
AFIX 137 
H36A  2    0.722901    0.324478    0.226274    11.00000   -1.50000 
H36B  2    0.667279    0.383134    0.168198    11.00000   -1.50000 
H36C  2    0.627710    0.308953    0.213833    11.00000   -1.50000 
AFIX   0 
C37   1    0.672175    0.459808    0.264114    11.00000    0.08116    0.06250 = 
         0.05195    0.00758   -0.01750   -0.03452 
AFIX 137 
H37A  2    0.645999    0.488971    0.299340    11.00000   -1.50000 
H37B  2    0.672261    0.495049    0.218793    11.00000   -1.50000 
H37C  2    0.733747    0.435705    0.272702    11.00000   -1.50000 
AFIX   0 
C38   1    0.710940    0.312833    0.508775    11.00000    0.04601    0.05443 = 
         0.04218   -0.01391   -0.00989   -0.00457 
C39   1    0.809732    0.291562    0.482904    11.00000    0.04277    0.08701 = 
         0.05725   -0.01153   -0.01192   -0.00653 
AFIX 137 
H39A  2    0.823500    0.326729    0.438935    11.00000   -1.50000 
H39B  2    0.821289    0.238138    0.476777    11.00000   -1.50000 
H39C  2    0.847525    0.296230    0.516473    11.00000   -1.50000 
AFIX   0 
C40   1    0.691811    0.396380    0.516221    11.00000    0.07096    0.07163 = 
         0.05822   -0.02678   -0.02404   -0.00443 
AFIX 137 
H40A  2    0.727851    0.402353    0.550393    11.00000   -1.50000 
H40B  2    0.628164    0.410267    0.531109    11.00000   -1.50000 
H40C  2    0.707072    0.430448    0.471967    11.00000   -1.50000 
AFIX   0 
C41   1    0.692413    0.260936    0.579808    11.00000    0.06040    0.08921 = 
         0.03555   -0.00949   -0.01330   -0.01647 
AFIX 137 
H41A  2    0.730698    0.269104    0.611468    11.00000   -1.50000 
H41B  2    0.705248    0.206535    0.576387    11.00000   -1.50000 
H41C  2    0.629449    0.273991    0.596978    11.00000   -1.50000 
AFIX   0 
C42   1    0.491587    0.179039    0.442930    11.00000    0.03656    0.04655 = 
         0.02343   -0.00027   -0.00004   -0.00492 
AFIX  43 
H42   2    0.494018    0.150657    0.489035    11.00000   -1.20000 
AFIX   0 
C43   1    0.390295    0.098430    0.444648    11.00000    0.03500    0.05073 = 
         0.02771    0.00286   -0.00465   -0.01320 
C44   1    0.395125    0.033522    0.418530    11.00000    0.04440    0.05129 = 
         0.03110    0.00342   -0.00690   -0.01328 
AFIX  43 
H44   2    0.428190    0.030747    0.375365    11.00000   -1.20000 
AFIX   0 
C45   1    0.352490   -0.027613    0.454312    11.00000    0.05571    0.05580 = 
         0.04337    0.00820   -0.01896   -0.01957 
AFIX  43 
H45   2    0.355838   -0.071632    0.435450    11.00000   -1.20000 
AFIX   0 
C46   1    0.304923   -0.024425    0.517711    11.00000    0.05851    0.07643 = 
         0.04159    0.02162   -0.01303   -0.03441 
AFIX  43 
H46   2    0.277540   -0.067033    0.543273    11.00000   -1.20000 
AFIX   0 
C47   1    0.297661    0.040689    0.543292    11.00000    0.04324    0.08829 = 
         0.03312    0.00956   -0.00127   -0.02454 
AFIX  43 
H47   2    0.263423    0.043581    0.586016    11.00000   -1.20000 
AFIX   0 
C48   1    0.339388    0.101881    0.507797    11.00000    0.03957    0.06731 = 
         0.02851   -0.00242   -0.00742   -0.01008 
C49   1    0.365245    0.172227    0.588155    11.00000    0.03743    0.07731 = 
         0.02508   -0.00413    0.00567   -0.01571 
C50   1    0.350723    0.243074    0.605053    11.00000    0.05492    0.08300 = 
         0.03797   -0.00821    0.00235   -0.01881 
AFIX  43 
H50   2    0.315352    0.286201    0.578690    11.00000   -1.20000 
AFIX   0 
C51   1    0.388393    0.251358    0.661411    11.00000    0.07901    0.09450 = 
         0.04902   -0.01820    0.00476   -0.03207 
AFIX  43 
H51   2    0.378149    0.299956    0.674115    11.00000   -1.20000 
AFIX   0 
C52   1    0.440476    0.188396    0.698312    11.00000    0.08346    0.11132 = 
         0.04623    0.00058   -0.01689   -0.04068 
AFIX  43 
H52   2    0.467316    0.194029    0.736025    11.00000   -1.20000 
AFIX   0 
C53   1    0.453896    0.118444    0.681441    11.00000    0.06641    0.10346 = 
         0.03950    0.01025   -0.01216   -0.02773 
AFIX  43 
H53   2    0.489337    0.075485    0.707939    11.00000   -1.20000 
AFIX   0 
C54   1    0.416407    0.108570    0.625690    11.00000    0.04778    0.08365 = 
         0.03120    0.00141   -0.00304   -0.01567 
AFIX  43 
H54   2    0.425798    0.059521    0.613904    11.00000   -1.20000 
AFIX   0 
V2    5    0.274323    0.046439    0.841058    11.00000    0.03414    0.03919 = 
         0.02487   -0.00134   -0.00513   -0.00757 
N3    3    0.210210    0.053557    0.751783    11.00000    0.02959    0.03954 = 
         0.02805   -0.00176    0.00158   -0.00626 
N4    3    0.318717    0.047370    0.935740    11.00000    0.03979    0.03552 = 
         0.03019   -0.00224   -0.00631   -0.01161 
O6    4    0.243871    0.156056    0.824321    11.00000    0.03952    0.04310 = 
         0.02866   -0.00144   -0.00825   -0.00655 
O7    4    0.051956    0.019957    0.716848    11.00000    0.03541    0.06534 = 
         0.03601   -0.01814   -0.00871   -0.00157 
O8    4    0.194430   -0.019515    0.892683    11.00000    0.03810    0.04495 = 
         0.02378   -0.00039   -0.00501   -0.01259 
O9    4    0.298139    0.143282    1.030879    11.00000    0.05871    0.05397 = 
         0.03868   -0.01006   -0.01987   -0.00355 
O10   4    0.370609    0.006216    0.812783    11.00000    0.03409    0.05181 = 
         0.03479   -0.00822   -0.00564   -0.00464 
C55   1    0.198809    0.212464    0.779186    11.00000    0.02801    0.04038 = 
         0.03003    0.00204   -0.00077   -0.00571 
C56   1    0.182130    0.289816    0.786987    11.00000    0.03392    0.03990 = 
         0.03415   -0.00120    0.00101   -0.00857 
C57   1    0.138445    0.345945    0.736868    11.00000    0.04158    0.03778 = 
         0.04620    0.00143   -0.00194   -0.00555 
AFIX  43 
H57   2    0.127987    0.398086    0.741811    11.00000   -1.20000 
AFIX   0 
C58   1    0.108559    0.330909    0.679192    11.00000    0.04809    0.04523 = 
         0.03788    0.00403   -0.00809   -0.00274 
C59   1    0.123819    0.255528    0.673877    11.00000    0.04049    0.05069 = 
         0.03300    0.00201   -0.00889   -0.00452 
AFIX  43 
H59   2    0.104372    0.243036    0.635894    11.00000   -1.20000 
AFIX   0 
C60   1    0.167621    0.195056    0.722897    11.00000    0.03408    0.04171 = 
         0.02977   -0.00234    0.00098   -0.00927 
C61   1    0.210218    0.311991    0.849098    11.00000    0.04075    0.03825 = 
         0.03949   -0.00410   -0.00588   -0.00785 
C62   1    0.171461    0.263233    0.916484    11.00000    0.05591    0.05452 = 
         0.04216   -0.00954   -0.00073   -0.01027 
AFIX 137 
H62A  2    0.106075    0.271567    0.918142    11.00000   -1.50000 
H62B  2    0.188479    0.278800    0.955475    11.00000   -1.50000 
H62C  2    0.195139    0.208271    0.918761    11.00000   -1.50000 
AFIX   0 
C63   1    0.313547    0.298911    0.844674    11.00000    0.04724    0.04696 = 
         0.05486   -0.00682   -0.01259   -0.00771 
AFIX 137 
H63A  2    0.337251    0.244681    0.843545    11.00000   -1.50000 
H63B  2    0.331930    0.311103    0.884827    11.00000   -1.50000 
H63C  2    0.336942    0.332661    0.802847    11.00000   -1.50000 
AFIX   0 
C64   1    0.175399    0.396563    0.851047    11.00000    0.05125    0.04949 = 
         0.06166   -0.01310   -0.01223   -0.00360 
AFIX 137 
H64A  2    0.202900    0.430022    0.810948    11.00000   -1.50000 
H64B  2    0.190655    0.407100    0.893012    11.00000   -1.50000 
H64C  2    0.110249    0.406960    0.850435    11.00000   -1.50000 
AFIX   0 
SAME 0.02 C65 C68 < C66 
SAME 0.02 C65 C66X > C68X 
C65   1    0.063140    0.398045    0.625822    11.00000    0.07580    0.05353 = 
         0.04956    0.00800   -0.01846    0.00519 
PART   1 
C66   1   -0.012512    0.444192    0.665705    21.00000    0.09723    0.05075 = 
         0.06215    0.00773   -0.03974    0.02610 
AFIX  33 
H66A  2    0.011708    0.458602    0.702323    21.00000   -1.50000 
H66B  2   -0.058810    0.412235    0.685807    21.00000   -1.50000 
H66C  2   -0.038629    0.491140    0.634395    21.00000   -1.50000 
AFIX   0 
C67   1    0.131005    0.454860    0.594162    21.00000    0.11455    0.08191 = 
         0.12595    0.06632   -0.01784   -0.01571 
AFIX  33 
H67A  2    0.150087    0.473269    0.630785    21.00000   -1.50000 
H67B  2    0.102248    0.499110    0.561473    21.00000   -1.50000 
H67C  2    0.183262    0.427851    0.570362    21.00000   -1.50000 
AFIX   0 
C68   1    0.026188    0.373873    0.571630    21.00000    0.19670    0.07590 = 
         0.04146    0.00011   -0.05056    0.01593 
AFIX  33 
H68A  2   -0.002105    0.419862    0.540429    21.00000   -1.50000 
H68B  2   -0.018393    0.340543    0.592945    21.00000   -1.50000 
H68C  2    0.074706    0.345279    0.545799    21.00000   -1.50000 
AFIX   0 
PART   2 
C66X  1    0.017696    0.471173    0.647300   -21.00000    0.20143    0.03094 = 
         0.07863    0.02067   -0.02810    0.02115 
AFIX  33 
H66D  2   -0.007160    0.508355    0.607838   -21.00000   -1.50000 
H66E  2    0.061221    0.493412    0.664425   -21.00000   -1.50000 
H66F  2   -0.030681    0.459559    0.683677   -21.00000   -1.50000 
AFIX   0 
C67X  1    0.137541    0.413931    0.564570   -21.00000    0.11125    0.08136 = 
         0.06016    0.04995   -0.01642   -0.00369 
AFIX  33 
H67D  2    0.164212    0.365293    0.550808   -21.00000   -1.50000 
H67E  2    0.183954    0.435538    0.578897   -21.00000   -1.50000 
H67F  2    0.110970    0.450893    0.525713   -21.00000   -1.50000 
AFIX   0 
C68X  1   -0.003041    0.365197    0.594717   -21.00000    0.10431    0.07740 = 
         0.04847    0.02762   -0.05759    0.00455 
AFIX  33 
H68D  2    0.029100    0.321833    0.574882   -21.00000   -1.50000 
H68E  2   -0.031177    0.405800    0.558775   -21.00000   -1.50000 
H68F  2   -0.049216    0.347028    0.630673   -21.00000   -1.50000 
AFIX   0 
PART   0 
C69   1    0.176831    0.118720    0.712553    11.00000    0.02921    0.05067 = 
         0.02295   -0.00327   -0.00020   -0.01047 
AFIX  43 
H69   2    0.155982    0.114465    0.671741    11.00000   -1.20000 
AFIX   0 
C70   1    0.209023   -0.015474    0.728433    11.00000    0.03942    0.04113 = 
         0.01696   -0.00376   -0.00209   -0.00522 
C71   1    0.286671   -0.069752    0.725052    11.00000    0.03903    0.04718 = 
         0.02404   -0.00566   -0.00258   -0.00616 
AFIX  43 
H71   2    0.339929   -0.060542    0.738438    11.00000   -1.20000 
AFIX   0 
C72   1    0.288278   -0.136597    0.702758    11.00000    0.05031    0.05291 = 
         0.03318   -0.01023   -0.00794    0.00234 
AFIX  43 
H72   2    0.342231   -0.172536    0.700261    11.00000   -1.20000 
AFIX   0 
C73   1    0.210118   -0.150931    0.683943    11.00000    0.06504    0.04707 = 
         0.04002   -0.01131   -0.00956   -0.00898 
AFIX  43 
H73   2    0.210415   -0.197123    0.669094    11.00000   -1.20000 
AFIX   0 
C74   1    0.132460   -0.098160    0.686871    11.00000    0.04645    0.05593 = 
         0.03882   -0.01401   -0.01042   -0.00975 
AFIX  43 
H74   2    0.079305   -0.107823    0.673696    11.00000   -1.20000 
AFIX   0 
C75   1    0.131560   -0.031214    0.708900    11.00000    0.04019    0.04481 = 
         0.02608   -0.00511   -0.00414   -0.00428 
C76   1   -0.006042    0.036984    0.666185    11.00000    0.03825    0.04809 = 
         0.03491   -0.00777   -0.00434   -0.00912 
C77   1    0.024529    0.051431    0.596791    11.00000    0.03610    0.06828 = 
         0.04426   -0.01390   -0.00068   -0.01236 
AFIX  43 
H77   2    0.086833    0.047628    0.582522    11.00000   -1.20000 
AFIX   0 
C78   1   -0.036429    0.071320    0.548915    11.00000    0.05569    0.06064 = 
         0.04353   -0.00719   -0.01141   -0.01382 
AFIX  43 
H78   2   -0.016019    0.081811    0.501401    11.00000   -1.20000 
AFIX   0 
C79   1   -0.126954    0.076116    0.569473    11.00000    0.05734    0.07075 = 
         0.05575    0.00027   -0.02653   -0.01371 
AFIX  43 
H79   2   -0.168867    0.089140    0.536399    11.00000   -1.20000 
AFIX   0 
C80   1   -0.155758    0.061815    0.638416    11.00000    0.03631    0.08273 = 
         0.06581    0.00047   -0.00978   -0.01074 
AFIX  43 
H80   2   -0.218056    0.065676    0.652724    11.00000   -1.20000 
AFIX   0 
C81   1   -0.095568    0.041897    0.687314    11.00000    0.03931    0.06458 = 
         0.03968   -0.00380   -0.00053   -0.01191 
AFIX  43 
H81   2   -0.116120    0.031797    0.734807    11.00000   -1.20000 
AFIX   0 
C82   1    0.182737   -0.058646    0.957944    11.00000    0.03530    0.03543 = 
         0.02318   -0.00494   -0.00002   -0.00096 
C83   1    0.117317   -0.107328    0.978347    11.00000    0.03590    0.04768 = 
         0.02566   -0.00274    0.00259   -0.01159 
C84   1    0.114213   -0.151719    1.044620    11.00000    0.04140    0.05315 = 
         0.03319   -0.00266    0.00207   -0.01322 
AFIX  43 
H84   2    0.071010   -0.185389    1.057730    11.00000   -1.20000 
AFIX   0 
C85   1    0.169752   -0.151148    1.094256    11.00000    0.03595    0.04738 = 
         0.02805   -0.00257    0.00037   -0.00409 
C86   1    0.229151   -0.100164    1.074525    11.00000    0.04407    0.04414 = 
         0.02409   -0.00448   -0.00546   -0.00226 
AFIX  43 
H86   2    0.266463   -0.096158    1.106819    11.00000   -1.20000 
AFIX   0 
C87   1    0.236739   -0.053010    1.007191    11.00000    0.03556    0.03829 = 
         0.02826   -0.00326   -0.00567   -0.00588 
C88   1    0.052833   -0.112387    0.928382    11.00000    0.04119    0.06890 = 
         0.03420    0.00063   -0.00406   -0.02661 
C89   1    0.005297   -0.031276    0.895203    11.00000    0.03978    0.09134 = 
         0.04748   -0.00213   -0.01231   -0.01142 
AFIX 137 
H89A  2   -0.028259   -0.005945    0.931108    11.00000   -1.50000 
H89B  2   -0.035992   -0.036204    0.864243    11.00000   -1.50000 
H89C  2    0.049916   -0.000106    0.869162    11.00000   -1.50000 
AFIX   0 
C90   1    0.105611   -0.153308    0.873258    11.00000    0.08609    0.06459 = 
         0.04019   -0.00349   -0.02035   -0.03570 
AFIX 137 
H90A  2    0.154732   -0.125682    0.850323    11.00000   -1.50000 
H90B  2    0.065822   -0.153761    0.839482    11.00000   -1.50000 
H90C  2    0.130061   -0.206673    0.894686    11.00000   -1.50000 
AFIX   0 
C91   1   -0.020675   -0.159268    0.965927    11.00000    0.06518    0.13842 = 
         0.05446    0.01352   -0.01749   -0.06120 
AFIX 137 
H91A  2    0.006930   -0.211546    0.987671    11.00000   -1.50000 
H91B  2   -0.060095   -0.162572    0.932929    11.00000   -1.50000 
H91C  2   -0.055690   -0.133553    1.001100    11.00000   -1.50000 
AFIX   0 
C92   1    0.160810   -0.205655    1.164952    11.00000    0.05067    0.05772 = 
         0.02946    0.00497   -0.00329   -0.01134 
C93   1    0.065816   -0.186342    1.201191    11.00000    0.05511    0.09824 = 
         0.03181    0.00924    0.00455   -0.01697 
AFIX 137 
H93A  2    0.061293   -0.219736    1.247283    11.00000   -1.50000 
H93B  2    0.021497   -0.195083    1.174596    11.00000   -1.50000 
H93C  2    0.054475   -0.131973    1.204653    11.00000   -1.50000 
AFIX   0 
C94   1    0.176250   -0.290169    1.156539    11.00000    0.08339    0.05989 = 
         0.05132    0.00885   -0.01043   -0.01024 
AFIX 137 
H94A  2    0.235788   -0.302375    1.132574    11.00000   -1.50000 
H94B  2    0.130677   -0.296586    1.129833    11.00000   -1.50000 
H94C  2    0.172088   -0.325205    1.201869    11.00000   -1.50000 
AFIX   0 
C95   1    0.228948   -0.198305    1.210593    11.00000    0.06074    0.07425 = 
         0.02932    0.01369   -0.00562   -0.00931 
AFIX 137 
H95A  2    0.289664   -0.212453    1.189296    11.00000   -1.50000 
H95B  2    0.220394   -0.233022    1.255699    11.00000   -1.50000 
H95C  2    0.220403   -0.144735    1.215998    11.00000   -1.50000 
AFIX   0 
C96   1    0.300248   -0.000632    0.993259    11.00000    0.03916    0.04206 = 
         0.03242   -0.00565   -0.01119   -0.00153 
AFIX  43 
H96   2    0.332435   -0.001094    1.030262    11.00000   -1.20000 
AFIX   0 
C97   1    0.384014    0.095243    0.937544    11.00000    0.04115    0.04415 = 
         0.03290    0.00370   -0.01631   -0.00873 
C98   1    0.458387    0.097197    0.888410    11.00000    0.04706    0.05256 = 
         0.03911    0.00110   -0.01830   -0.01308 
AFIX  43 
H98   2    0.464619    0.068088    0.854079    11.00000   -1.20000 
AFIX   0 
C99   1    0.523123    0.141075    0.889176    11.00000    0.05009    0.07051 = 
         0.04837    0.00992   -0.02054   -0.02398 
AFIX  43 
H99   2    0.573363    0.141887    0.855515    11.00000   -1.20000 
AFIX   0 
C100  1    0.514651    0.183593    0.938812    11.00000    0.06877    0.06300 = 
         0.06227    0.01253   -0.03527   -0.03018 
AFIX  43 
H100  2    0.559759    0.212601    0.940170    11.00000   -1.20000 
AFIX   0 
C101  1    0.440552    0.183773    0.986333    11.00000    0.07768    0.04834 = 
         0.05329   -0.00328   -0.02956   -0.02353 
AFIX  43 
H101  2    0.433531    0.214491    1.019506    11.00000   -1.20000 
AFIX   0 
C102  1    0.376120    0.139399    0.986070    11.00000    0.05440    0.04222 = 
         0.03738    0.00026   -0.01967   -0.00598 
C103  1    0.304611    0.116392    1.101194    11.00000    0.05942    0.04272 = 
         0.04010   -0.00868   -0.01780   -0.01060 
C104  1    0.226550    0.130273    1.142709    11.00000    0.05600    0.06650 = 
         0.05291   -0.01872   -0.02161   -0.01126 
AFIX  43 
H104  2    0.173493    0.157829    1.123302    11.00000   -1.20000 
AFIX   0 
C105  1    0.226008    0.103617    1.213309    11.00000    0.06632    0.07618 = 
         0.05341   -0.01821   -0.00447   -0.02442 
AFIX  43 
H105  2    0.172189    0.112521    1.242291    11.00000   -1.20000 
AFIX   0 
C106  1    0.303036    0.064405    1.241402    11.00000    0.07835    0.07210 = 
         0.04164   -0.00093   -0.01550   -0.02315 
AFIX  43 
H106  2    0.302609    0.046774    1.289732    11.00000   -1.20000 
AFIX   0 
C107  1    0.380660    0.050772    1.199410    11.00000    0.06839    0.06293 = 
         0.04806   -0.00633   -0.02080   -0.01093 
AFIX  43 
H107  2    0.433711    0.023690    1.219084    11.00000   -1.20000 
AFIX   0 
C108  1    0.382669    0.076058    1.128509    11.00000    0.06037    0.05276 = 
         0.04078   -0.00730   -0.01558   -0.00502 
AFIX  43 
H108  2    0.436182    0.065942    1.099535    11.00000   -1.20000 
AFIX   0 
N5    3    0.434965    0.631954    0.140193    11.00000    0.17240    0.08150 = 
         0.07903   -0.00730   -0.02731   -0.00719 
C109  1    0.439761    0.640727    0.193708    11.00000    0.08924    0.05187 = 
         0.09003   -0.00374   -0.02025   -0.00261 
C110  1    0.445896    0.652725    0.261076    11.00000    0.09740    0.07965 = 
         0.08302   -0.02434   -0.03087   -0.00830 
AFIX 137 
H11A  2    0.451721    0.706784    0.257405    11.00000   -1.50000 
H11B  2    0.498365    0.618489    0.280310    11.00000   -1.50000 
H11C  2    0.391758    0.641031    0.291152    11.00000   -1.50000 
AFIX   0 
N6    3    0.442291    0.434472    0.589132    11.00000    0.13071    0.12750 = 
         0.07271    0.00356    0.00106    0.00628 
C111  1    0.431687    0.425288    0.534903    11.00000    0.07341    0.06139 = 
         0.10331    0.00577    0.01065    0.00034 
C112  1    0.419872    0.416558    0.464436    11.00000    0.09391    0.08280 = 
         0.07953   -0.03365   -0.01011    0.00503 
AFIX 137 
H11D  2    0.358262    0.438158    0.454145    11.00000   -1.50000 
H11E  2    0.432246    0.361529    0.463107    11.00000   -1.50000 
H11F  2    0.461433    0.444314    0.430274    11.00000   -1.50000 
AFIX   0 
N7    3    0.733606    0.445050    0.674130    11.00000    0.13872    0.15030 = 
         0.12198   -0.07141   -0.01862   -0.03044 
C113  1    0.736334    0.497037    0.694437    11.00000    0.09428    0.09549 = 
         0.06564   -0.03301   -0.01267   -0.01892 
C114  1    0.738931    0.561291    0.721895    11.00000    0.17535    0.13680 = 
         0.12656   -0.07918    0.04644   -0.08189 
AFIX 137 
H11G  2    0.683587    0.571806    0.751614    11.00000   -1.50000 
H11H  2    0.744749    0.606715    0.684438    11.00000   -1.50000 
H11I  2    0.790264    0.550038    0.748729    11.00000   -1.50000 
  
AFIX   0 
HKLF 4 
  
REM  cr485 in P-1 
REM R1 =  0.0486 for    8609 Fo > 4sig(Fo)  and  0.0973 for all   13810 data 
REM   1250 parameters refined using     92 restraints 
  
END 
  
WGHT      0.0453      3.3981 
  
REM Highest difference peak  0.439,  deepest hole -0.300,  1-sigma level  0.047 
Q1    1  -0.0487  0.3171  0.1678  11.00000  0.05    0.44 
Q2    1   0.5006  0.4956  0.4196  11.00000  0.05    0.43 
Q3    1  -0.0075  0.4448  0.1893  11.00000  0.05    0.29 
Q4    1   0.3032 -0.0266  0.8423  11.00000  0.05    0.29 
Q5    1   0.0612  0.4017  0.0739  11.00000  0.05    0.28 
Q6    1   0.2445  0.1108  0.8095  11.00000  0.05    0.26 
Q7    1   0.2964  0.1130  0.8212  11.00000  0.05    0.25 
Q8    1   0.4313  0.2746  0.2988  11.00000  0.05    0.25 
Q9    1   0.7405  0.5202  0.6310  11.00000  0.05    0.25 
Q10   1   0.4772  0.2216  0.3421  11.00000  0.05    0.22 
;
_database_code_depnum_ccdc_archive 'CCDC 980007'
#######################################################################
#
#                 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_8

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C72 H68 N2 O5 V'
_chemical_formula_sum            'C72 H68 N2 O5 V'
_chemical_formula_weight         1092.22

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           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                   13.457(3)
_cell_length_b                   15.049(3)
_cell_length_c                   16.071(3)
_cell_angle_alpha                70.73(3)
_cell_angle_beta                 68.07(3)
_cell_angle_gamma                79.53(3)
_cell_volume                     2843.8(10)
_cell_formula_units_Z            2
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    25484
_cell_measurement_theta_min      1.43
_cell_measurement_theta_max      27.50


_exptl_crystal_description       Plate
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.424
_exptl_crystal_size_mid          0.267
_exptl_crystal_size_min          0.226
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.276
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1154
_exptl_absorpt_coefficient_mu    0.230
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_absorpt_correction_T_min  .0000
_exptl_absorpt_correction_T_max  .0000

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'MM007-HF CCD(Saturn 724+)'
_diffrn_measurement_method       'ω scans at fixed χ = 45°'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         none
_diffrn_standards_interval_count none
_diffrn_standards_interval_time  none
_diffrn_standards_decay_%        none
_diffrn_reflns_number            25484
_diffrn_reflns_av_R_equivalents  0.0520
_diffrn_reflns_av_unetI/netI     0.0651
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         1.43
_diffrn_reflns_theta_max         27.50
_reflns_number_total             12955
_reflns_number_gt                11284
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrystalClear (Rigaku Inc., 2007)'
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2007)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'CAMERON (Watkin et al, 1993)'
_computing_publication_material  'SHELX97 (Sheldrick, 1997)'

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1762P)²+2.5503P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         12955
_refine_ls_number_parameters     723
_refine_ls_number_restraints     0
_refine_ls_R_factor_ref          0.0915
_refine_ls_R_factor_gt           0.0731
_refine_ls_wR_factor_ref         0.2590
_refine_ls_wR_factor_gt          0.2180
_refine_ls_goodness_of_fit_ref   0.984
_refine_ls_restrained_S_all      0.984
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
V1 V 0.79507(3) 0.69035(3) 0.31137(3) 0.01981(15) Uani 1 1 d . . .
O2 O 0.70491(16) 0.79890(13) 0.33628(14) 0.0250(4) Uani 1 1 d . . .
O3 O 0.89697(16) 0.71814(15) 0.18792(13) 0.0256(4) Uani 1 1 d . . .
N1 N 0.90739(18) 0.73652(16) 0.34874(15) 0.0207(4) Uani 1 1 d . . .
O4 O 0.81662(16) 0.70319(16) 0.55409(15) 0.0312(5) Uani 1 1 d . . .
O1 O 0.78428(17) 0.59005(14) 0.38810(15) 0.0291(5) Uani 1 1 d . . .
N2 N 0.68539(19) 0.66847(17) 0.25529(17) 0.0243(5) Uani 1 1 d . . .
O5 O 0.71974(19) 0.46186(18) 0.24680(17) 0.0403(6) Uani 1 1 d . . .
C8 C 0.9963(2) 0.7415(2) 0.49445(19) 0.0234(5) Uani 1 1 d . . .
C9 C 0.6524(2) 0.9630(2) 0.31614(19) 0.0237(5) Uani 1 1 d . . .
C10 C 0.9098(2) 0.82358(19) 0.34308(18) 0.0223(5) Uani 1 1 d . . .
H10 H 0.9722 0.8402 0.3474 0.027 Uiso 1 1 calc R . .
C11 C 0.8278(2) 0.8990(2) 0.33083(19) 0.0237(5) Uani 1 1 d . . .
C12 C 0.8498(2) 0.9886(2) 0.3259(2) 0.0275(6) Uani 1 1 d . . .
H12 H 0.9169 0.9970 0.3283 0.033 Uiso 1 1 calc R . .
C13 C 0.7283(2) 0.88447(19) 0.32783(19) 0.0224(5) Uani 1 1 d . . .
C14 C 0.5690(2) 0.9140(2) 0.2217(2) 0.0286(6) Uani 1 1 d . . .
H14A H 0.6142 0.9572 0.1638 0.034 Uiso 1 1 calc R . .
H14B H 0.6094 0.8518 0.2324 0.034 Uiso 1 1 calc R . .
C15 C 0.6959(2) 0.70546(19) 0.1675(2) 0.0242(5) Uani 1 1 d . . .
H15 H 0.6349 0.7057 0.1512 0.029 Uiso 1 1 calc R . .
C16 C 0.5433(2) 0.6397(2) 0.4061(2) 0.0268(6) Uani 1 1 d . . .
H16 H 0.5826 0.6709 0.4252 0.032 Uiso 1 1 calc R . .
C17 C 0.7891(2) 0.7463(2) 0.0918(2) 0.0253(6) Uani 1 1 d . . .
C18 C 0.8873(2) 0.7514(2) 0.10367(19) 0.0240(5) Uani 1 1 d . . .
C19 C 0.5749(3) 0.5484(2) 0.2019(2) 0.0306(6) Uani 1 1 d . . .
C20 C 1.1046(2) 0.5959(2) 0.4657(2) 0.0271(6) Uani 1 1 d . . .
H20 H 1.1324 0.5954 0.5122 0.033 Uiso 1 1 calc R . .
C21 C 0.6783(2) 1.0487(2) 0.3131(2) 0.0275(6) Uani 1 1 d . . .
H21 H 0.6269 1.1007 0.3075 0.033 Uiso 1 1 calc R . .
C22 C 0.5460(2) 0.9532(2) 0.3054(2) 0.0249(6) Uani 1 1 d . . .
C23 C 0.9894(2) 0.66818(19) 0.37364(19) 0.0222(5) Uani 1 1 d . . .
C24 C 0.7760(3) 1.0644(2) 0.3178(2) 0.0289(6) Uani 1 1 d . . .
C25 C 1.0287(2) 0.66830(19) 0.44361(19) 0.0215(5) Uani 1 1 d . . .
C26 C 0.9435(3) 0.8841(2) 0.5823(2) 0.0330(7) Uani 1 1 d . . .
H26 H 0.9250 0.9338 0.6107 0.040 Uiso 1 1 calc R . .
C27 C 1.1400(2) 0.5257(2) 0.4220(2) 0.0279(6) Uani 1 1 d . . .
H27 H 1.1908 0.4770 0.4390 0.033 Uiso 1 1 calc R . .
C28 C 0.4730(2) 0.8867(2) 0.3950(2) 0.0292(6) Uani 1 1 d . . .
H28A H 0.5118 0.8242 0.4099 0.035 Uiso 1 1 calc R . .
H28B H 0.4547 0.9129 0.4483 0.035 Uiso 1 1 calc R . .
C29 C 1.1011(2) 0.5264(2) 0.3531(2) 0.0266(6) Uani 1 1 d . . .
H29 H 1.1266 0.4789 0.3217 0.032 Uiso 1 1 calc R . .
C30 C 0.8906(2) 0.7587(2) 0.54925(19) 0.0247(5) Uani 1 1 d . . .
C31 C 1.0751(2) 0.7951(2) 0.4873(2) 0.0292(6) Uani 1 1 d . . .
H31 H 1.1478 0.7828 0.4519 0.035 Uiso 1 1 calc R . .
C32 C 0.4440(2) 0.6070(2) 0.4678(2) 0.0306(6) Uani 1 1 d . . .
H32 H 0.4152 0.6175 0.5278 0.037 Uiso 1 1 calc R . .
C33 C 0.9752(2) 0.7938(2) 0.0239(2) 0.0282(6) Uani 1 1 d . . .
C34 C 0.5856(2) 0.62745(19) 0.3175(2) 0.0250(6) Uani 1 1 d . . .
C35 C 1.0251(2) 0.5964(2) 0.32993(19) 0.0243(5) Uani 1 1 d . . .
H35 H 0.9971 0.5954 0.2840 0.029 Uiso 1 1 calc R . .
C36 C 0.4822(2) 1.0492(2) 0.2862(2) 0.0285(6) Uani 1 1 d . . .
H36A H 0.5268 1.0937 0.2290 0.034 Uiso 1 1 calc R . .
H36B H 0.4646 1.0755 0.3392 0.034 Uiso 1 1 calc R . .
C37 C 0.7801(3) 0.7790(2) 0.0017(2) 0.0315(6) Uani 1 1 d . . .
H37 H 0.7142 0.7750 -0.0054 0.038 Uiso 1 1 calc R . .
C38 C 0.5306(2) 0.5746(2) 0.2917(2) 0.0284(6) Uani 1 1 d . . .
C39 C 1.1347(2) 0.7125(2) 0.0734(2) 0.0328(7) Uani 1 1 d . . .
H39A H 1.0846 0.6783 0.1344 0.039 Uiso 1 1 calc R . .
H39B H 1.1529 0.6735 0.0301 0.039 Uiso 1 1 calc R . .
C40 C 0.7122(2) 0.7056(2) 0.6168(2) 0.0284(6) Uani 1 1 d . . .
C41 C 0.4315(2) 0.5430(2) 0.3545(2) 0.0340(7) Uani 1 1 d . . .
H41 H 0.3930 0.5093 0.3371 0.041 Uiso 1 1 calc R . .
C42 C 1.0495(3) 0.8658(2) 0.5309(2) 0.0324(7) Uani 1 1 d . . .
H42 H 1.1042 0.9015 0.5256 0.039 Uiso 1 1 calc R . .
C43 C 0.8642(3) 0.8298(2) 0.5922(2) 0.0312(6) Uani 1 1 d . . .
H43 H 0.7918 0.8415 0.6285 0.037 Uiso 1 1 calc R . .
C44 C 0.3072(2) 0.9712(2) 0.3622(3) 0.0358(7) Uani 1 1 d . . .
H44A H 0.2884 0.9969 0.4159 0.043 Uiso 1 1 calc R . .
H44B H 0.2398 0.9642 0.3542 0.043 Uiso 1 1 calc R . .
C45 C 0.5179(3) 0.5762(3) 0.1393(3) 0.0418(8) Uani 1 1 d . . .
H45 H 0.4514 0.6124 0.1540 0.050 Uiso 1 1 calc R . .
C46 C 0.8715(3) 0.3844(2) 0.2848(2) 0.0364(7) Uani 1 1 d . . .
H46 H 0.8246 0.3487 0.3425 0.044 Uiso 1 1 calc R . .
C47 C 0.3775(2) 1.0385(2) 0.2729(2) 0.0326(7) Uani 1 1 d . . .
H47 H 0.3376 1.1017 0.2609 0.039 Uiso 1 1 calc R . .
C48 C 0.9598(3) 0.8240(2) -0.0621(2) 0.0327(7) Uani 1 1 d . . .
H48 H 1.0178 0.8519 -0.1156 0.039 Uiso 1 1 calc R . .
C49 C 0.3693(2) 0.8753(2) 0.3809(2) 0.0335(7) Uani 1 1 d . . .
H49 H 0.3238 0.8310 0.4390 0.040 Uiso 1 1 calc R . .
C50 C 0.8310(3) 0.4517(2) 0.2200(2) 0.0315(6) Uani 1 1 d . . .
C51 C 0.8654(3) 0.8166(2) -0.0760(2) 0.0338(7) Uani 1 1 d . . .
C52 C 0.4038(3) 1.0007(2) 0.1897(3) 0.0370(7) Uani 1 1 d . . .
H52A H 0.4488 1.0444 0.1322 0.044 Uiso 1 1 calc R . .
H52B H 0.3368 0.9952 0.1803 0.044 Uiso 1 1 calc R . .
C53 C 0.6703(3) 0.4930(2) 0.1801(2) 0.0339(7) Uani 1 1 d . . .
C54 C 1.0796(2) 0.8076(2) 0.0338(2) 0.0290(6) Uani 1 1 d . . .
C55 C 1.0560(3) 0.8707(3) 0.0990(2) 0.0367(7) Uani 1 1 d . . .
H55A H 1.0232 0.9328 0.0722 0.044 Uiso 1 1 calc R . .
H55B H 1.0042 0.8409 0.1610 0.044 Uiso 1 1 calc R . .
C56 C 1.1611(3) 0.8574(3) -0.0609(2) 0.0377(7) Uani 1 1 d . . .
H56A H 1.1782 0.8192 -0.1048 0.045 Uiso 1 1 calc R . .
H56B H 1.1287 0.9196 -0.0881 0.045 Uiso 1 1 calc R . .
C57 C 0.8987(3) 0.5053(2) 0.1372(3) 0.0388(7) Uani 1 1 d . . .
H57 H 0.8700 0.5516 0.0939 0.047 Uiso 1 1 calc R . .
C58 C 0.4644(3) 0.9034(2) 0.2089(2) 0.0338(7) Uani 1 1 d . . .
H58 H 0.4816 0.8773 0.1550 0.041 Uiso 1 1 calc R . .
C59 C 0.3946(3) 0.8367(2) 0.2982(3) 0.0386(8) Uani 1 1 d . . .
H59A H 0.3270 0.8300 0.2905 0.046 Uiso 1 1 calc R . .
H59B H 0.4329 0.7736 0.3102 0.046 Uiso 1 1 calc R . .
C60 C 0.6311(3) 0.7305(3) 0.5785(3) 0.0371(7) Uani 1 1 d . . .
H60 H 0.6478 0.7494 0.5125 0.044 Uiso 1 1 calc R . .
C61 C 0.6890(3) 0.6764(3) 0.7118(2) 0.0453(9) Uani 1 1 d . . .
H61 H 0.7450 0.6577 0.7378 0.054 Uiso 1 1 calc R . .
C62 C 0.3872(2) 0.5589(2) 0.4413(2) 0.0339(7) Uani 1 1 d . . .
H62 H 0.3187 0.5374 0.4824 0.041 Uiso 1 1 calc R . .
C63 C 0.7955(3) 1.1615(2) 0.3142(3) 0.0365(7) Uani 1 1 d . . .
H63A H 0.7499 1.1754 0.3728 0.055 Uiso 1 1 calc R . .
H63B H 0.7783 1.2084 0.2615 0.055 Uiso 1 1 calc R . .
H63C H 0.8711 1.1636 0.3058 0.055 Uiso 1 1 calc R . .
C64 C 0.9826(3) 0.3705(3) 0.2630(3) 0.0470(9) Uani 1 1 d . . .
H64 H 1.0117 0.3243 0.3062 0.056 Uiso 1 1 calc R . .
C65 C 1.1601(3) 0.8847(3) 0.1109(3) 0.0471(9) Uani 1 1 d . . .
H65 H 1.1432 0.9250 0.1537 0.057 Uiso 1 1 calc R . .
C66 C 0.5566(4) 0.5519(3) 0.0566(3) 0.0499(10) Uani 1 1 d . . .
H66 H 0.5189 0.5741 0.0133 0.060 Uiso 1 1 calc R . .
C67 C 0.5003(3) 0.6993(3) 0.7319(3) 0.0529(11) Uani 1 1 d . . .
H67 H 0.4274 0.6968 0.7719 0.063 Uiso 1 1 calc R . .
C68 C 1.0085(3) 0.4910(3) 0.1178(3) 0.0438(8) Uani 1 1 d . . .
H68 H 1.0553 0.5284 0.0613 0.053 Uiso 1 1 calc R . .
C69 C 1.2649(3) 0.8714(3) -0.0494(3) 0.0449(9) Uani 1 1 d . . .
H69 H 1.3162 0.9035 -0.1118 0.054 Uiso 1 1 calc R . .
C70 C 1.3161(3) 0.7751(3) -0.0080(3) 0.0487(10) Uani 1 1 d . . .
H70A H 1.3341 0.7354 -0.0506 0.058 Uiso 1 1 calc R . .
H70B H 1.3832 0.7838 -0.0005 0.058 Uiso 1 1 calc R . .
C71 C 1.0506(3) 0.4223(3) 0.1804(3) 0.0491(9) Uani 1 1 d . . .
H71 H 1.1261 0.4114 0.1660 0.059 Uiso 1 1 calc R . .
C72 C 0.5819(4) 0.6744(3) 0.7696(3) 0.0589(12) Uani 1 1 d . . .
H72 H 0.5648 0.6558 0.8356 0.071 Uiso 1 1 calc R . .
C73 C 0.6506(4) 0.4953(3) 0.0369(3) 0.0517(10) Uani 1 1 d . . .
H73 H 0.6761 0.4768 -0.0190 0.062 Uiso 1 1 calc R . .
C74 C 0.8590(3) 0.8493(3) -0.1732(2) 0.0451(9) Uani 1 1 d . . .
H74A H 0.7916 0.8313 -0.1713 0.068 Uiso 1 1 calc R . .
H74B H 0.9197 0.8199 -0.2144 0.068 Uiso 1 1 calc R . .
H74C H 0.8615 0.9181 -0.1972 0.068 Uiso 1 1 calc R . .
C75 C 0.5250(3) 0.7274(3) 0.6375(3) 0.0478(9) Uani 1 1 d . . .
H75 H 0.4690 0.7452 0.6115 0.057 Uiso 1 1 calc R . .
C76 C 1.2373(3) 0.7274(3) 0.0864(3) 0.0434(8) Uani 1 1 d . . .
H76 H 1.2703 0.6647 0.1136 0.052 Uiso 1 1 calc R . .
C77 C 0.7080(3) 0.4651(3) 0.0986(3) 0.0447(8) Uani 1 1 d . . .
H77 H 0.7723 0.4259 0.0852 0.054 Uiso 1 1 calc R . .
C78 C 1.2107(3) 0.7883(3) 0.1528(3) 0.0491(10) Uani 1 1 d . . .
H78A H 1.2770 0.7969 0.1616 0.059 Uiso 1 1 calc R . .
H78B H 1.1600 0.7567 0.2147 0.059 Uiso 1 1 calc R . .
C79 C 1.2388(3) 0.9322(3) 0.0163(3) 0.0519(10) Uani 1 1 d . . .
H79A H 1.3055 0.9415 0.0240 0.062 Uiso 1 1 calc R . .
H79B H 1.2073 0.9948 -0.0107 0.062 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 1.593(2) . ?
V1 O3 1.903(2) . ?
V1 O2 1.911(2) . ?
V1 N1 2.113(2) . ?
V1 N2 2.113(2) . ?
O2 C13 1.333(3) . ?
O3 C18 1.327(3) . ?
N1 C10 1.289(4) . ?
N1 C23 1.443(3) . ?
O4 C30 1.378(4) . ?
O4 C40 1.393(3) . ?
N2 C15 1.296(4) . ?
N2 C34 1.440(4) . ?
O5 C53 1.378(4) . ?
O5 C50 1.390(4) . ?
C8 C30 1.395(4) . ?
C8 C31 1.396(4) . ?
C8 C25 1.491(4) . ?
C9 C21 1.377(4) . ?
C9 C13 1.425(4) . ?
C9 C22 1.543(4) . ?
C10 C11 1.451(4) . ?
C11 C12 1.404(4) . ?
C11 C13 1.415(4) . ?
C12 C24 1.375(4) . ?
C14 C58 1.539(4) . ?
C14 C22 1.549(4) . ?
C15 C17 1.442(4) . ?
C16 C34 1.384(4) . ?
C16 C32 1.391(4) . ?
C17 C37 1.411(4) . ?
C17 C18 1.422(4) . ?
C18 C33 1.433(4) . ?
C19 C53 1.390(5) . ?
C19 C45 1.399(5) . ?
C19 C38 1.497(4) . ?
C20 C27 1.376(4) . ?
C20 C25 1.402(4) . ?
C21 C24 1.410(4) . ?
C22 C36 1.540(4) . ?
C22 C28 1.545(4) . ?
C23 C35 1.397(4) . ?
C23 C25 1.411(4) . ?
C24 C63 1.510(4) . ?
C26 C42 1.385(5) . ?
C26 C43 1.391(5) . ?
C27 C29 1.387(4) . ?
C28 C49 1.542(4) . ?
C29 C35 1.389(4) . ?
C30 C43 1.383(4) . ?
C31 C42 1.387(4) . ?
C32 C62 1.393(5) . ?
C33 C48 1.388(4) . ?
C33 C54 1.529(4) . ?
C34 C38 1.419(4) . ?
C36 C47 1.544(4) . ?
C37 C51 1.377(5) . ?
C38 C41 1.390(4) . ?
C39 C76 1.536(4) . ?
C39 C54 1.539(4) . ?
C40 C61 1.368(5) . ?
C40 C60 1.383(5) . ?
C41 C62 1.380(5) . ?
C44 C49 1.528(4) . ?
C44 C47 1.535(5) . ?
C45 C66 1.381(5) . ?
C46 C50 1.391(5) . ?
C46 C64 1.396(5) . ?
C47 C52 1.521(5) . ?
C48 C51 1.399(5) . ?
C49 C59 1.523(5) . ?
C50 C57 1.379(5) . ?
C51 C74 1.505(4) . ?
C52 C58 1.536(4) . ?
C53 C77 1.392(5) . ?
C54 C56 1.543(4) . ?
C54 C55 1.548(4) . ?
C55 C65 1.542(5) . ?
C56 C69 1.535(5) . ?
C57 C68 1.382(5) . ?
C58 C59 1.528(5) . ?
C60 C75 1.386(5) . ?
C61 C72 1.393(6) . ?
C64 C71 1.370(6) . ?
C65 C79 1.516(5) . ?
C65 C78 1.537(6) . ?
C66 C73 1.384(6) . ?
C67 C75 1.358(6) . ?
C67 C72 1.382(7) . ?
C68 C71 1.389(6) . ?
C69 C79 1.523(6) . ?
C69 C70 1.537(6) . ?
C70 C76 1.516(5) . ?
C73 C77 1.389(6) . ?
C76 C78 1.533(6) . ?

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 125.65(11) . . ?
O1 V1 O2 122.19(11) . . ?
O3 V1 O2 112.15(10) . . ?
O1 V1 N1 95.34(10) . . ?
O3 V1 N1 86.07(9) . . ?
O2 V1 N1 87.07(9) . . ?
O1 V1 N2 95.16(10) . . ?
O3 V1 N2 87.79(9) . . ?
O2 V1 N2 87.37(9) . . ?
N1 V1 N2 169.50(9) . . ?
C13 O2 V1 131.36(18) . . ?
C18 O3 V1 132.92(18) . . ?
C10 N1 C23 119.7(2) . . ?
C10 N1 V1 122.53(18) . . ?
C23 N1 V1 117.59(17) . . ?
C30 O4 C40 120.1(2) . . ?
C15 N2 C34 117.6(2) . . ?
C15 N2 V1 121.69(19) . . ?
C34 N2 V1 119.63(18) . . ?
C53 O5 C50 120.3(3) . . ?
C30 C8 C31 118.3(3) . . ?
C30 C8 C25 123.0(3) . . ?
C31 C8 C25 118.7(3) . . ?
C21 C9 C13 117.5(3) . . ?
C21 C9 C22 120.9(3) . . ?
C13 C9 C22 121.5(2) . . ?
N1 C10 C11 127.1(3) . . ?
C12 C11 C13 120.5(3) . . ?
C12 C11 C10 116.3(3) . . ?
C13 C11 C10 123.2(3) . . ?
C24 C12 C11 121.2(3) . . ?
O2 C13 C11 120.9(2) . . ?
O2 C13 C9 120.0(2) . . ?
C11 C13 C9 119.0(2) . . ?
C58 C14 C22 111.4(2) . . ?
N2 C15 C17 127.7(3) . . ?
C34 C16 C32 121.2(3) . . ?
C37 C17 C18 120.3(3) . . ?
C37 C17 C15 116.1(3) . . ?
C18 C17 C15 123.5(2) . . ?
O3 C18 C17 120.4(2) . . ?
O3 C18 C33 120.3(3) . . ?
C17 C18 C33 119.3(2) . . ?
C53 C19 C45 118.3(3) . . ?
C53 C19 C38 121.6(3) . . ?
C45 C19 C38 120.0(3) . . ?
C27 C20 C25 122.0(3) . . ?
C9 C21 C24 124.4(3) . . ?
C36 C22 C9 111.5(2) . . ?
C36 C22 C28 107.3(2) . . ?
C9 C22 C28 111.4(2) . . ?
C36 C22 C14 107.4(2) . . ?
C9 C22 C14 110.0(2) . . ?
C28 C22 C14 109.0(2) . . ?
C35 C23 C25 119.8(2) . . ?
C35 C23 N1 117.5(2) . . ?
C25 C23 N1 122.5(2) . . ?
C12 C24 C21 117.3(3) . . ?
C12 C24 C63 122.9(3) . . ?
C21 C24 C63 119.8(3) . . ?
C20 C25 C23 117.9(3) . . ?
C20 C25 C8 117.8(2) . . ?
C23 C25 C8 124.2(2) . . ?
C42 C26 C43 120.0(3) . . ?
C20 C27 C29 119.6(3) . . ?
C49 C28 C22 110.3(2) . . ?
C27 C29 C35 120.1(3) . . ?
O4 C30 C43 123.6(3) . . ?
O4 C30 C8 115.6(2) . . ?
C43 C30 C8 120.7(3) . . ?
C42 C31 C8 121.3(3) . . ?
C16 C32 C62 119.7(3) . . ?
C48 C33 C18 116.8(3) . . ?
C48 C33 C54 121.8(3) . . ?
C18 C33 C54 121.4(2) . . ?
C16 C34 C38 119.3(3) . . ?
C16 C34 N2 118.1(3) . . ?
C38 C34 N2 122.6(3) . . ?
C29 C35 C23 120.5(3) . . ?
C22 C36 C47 110.8(2) . . ?
C51 C37 C17 121.0(3) . . ?
C41 C38 C34 118.2(3) . . ?
C41 C38 C19 118.2(3) . . ?
C34 C38 C19 123.6(3) . . ?
C76 C39 C54 110.9(3) . . ?
C61 C40 C60 120.9(3) . . ?
C61 C40 O4 122.5(3) . . ?
C60 C40 O4 116.3(3) . . ?
C62 C41 C38 122.3(3) . . ?
C26 C42 C31 119.4(3) . . ?
C30 C43 C26 120.1(3) . . ?
C49 C44 C47 108.8(3) . . ?
C66 C45 C19 121.1(4) . . ?
C50 C46 C64 118.3(3) . . ?
C52 C47 C44 110.1(3) . . ?
C52 C47 C36 109.9(3) . . ?
C44 C47 C36 109.6(3) . . ?
C33 C48 C51 124.9(3) . . ?
C59 C49 C44 108.7(3) . . ?
C59 C49 C28 111.0(3) . . ?
C44 C49 C28 109.5(3) . . ?
C57 C50 O5 123.9(3) . . ?
C57 C50 C46 121.1(3) . . ?
O5 C50 C46 115.0(3) . . ?
C37 C51 C48 117.7(3) . . ?
C37 C51 C74 122.1(3) . . ?
C48 C51 C74 120.2(3) . . ?
C47 C52 C58 108.8(3) . . ?
O5 C53 C19 116.1(3) . . ?
O5 C53 C77 122.5(3) . . ?
C19 C53 C77 121.1(3) . . ?
C33 C54 C39 111.3(3) . . ?
C33 C54 C56 112.1(3) . . ?
C39 C54 C56 107.1(3) . . ?
C33 C54 C55 109.8(3) . . ?
C39 C54 C55 109.6(3) . . ?
C56 C54 C55 106.9(3) . . ?
C65 C55 C54 110.7(3) . . ?
C69 C56 C54 111.3(3) . . ?
C50 C57 C68 119.5(3) . . ?
C59 C58 C52 109.4(3) . . ?
C59 C58 C14 109.4(3) . . ?
C52 C58 C14 108.9(3) . . ?
C49 C59 C58 109.9(3) . . ?
C40 C60 C75 119.3(3) . . ?
C40 C61 C72 118.8(4) . . ?
C41 C62 C32 119.2(3) . . ?
C71 C64 C46 121.1(4) . . ?
C79 C65 C78 109.1(4) . . ?
C79 C65 C55 109.7(3) . . ?
C78 C65 C55 109.4(3) . . ?
C45 C66 C73 119.8(4) . . ?
C75 C67 C72 119.5(4) . . ?
C57 C68 C71 120.3(4) . . ?
C79 C69 C56 109.3(3) . . ?
C79 C69 C70 109.4(3) . . ?
C56 C69 C70 109.6(3) . . ?
C76 C70 C69 108.9(3) . . ?
C64 C71 C68 119.7(4) . . ?
C67 C72 C61 120.7(4) . . ?
C66 C73 C77 120.4(4) . . ?
C67 C75 C60 120.8(4) . . ?
C70 C76 C78 109.9(3) . . ?
C70 C76 C39 109.3(3) . . ?
C78 C76 C39 110.2(3) . . ?
C73 C77 C53 119.3(4) . . ?
C76 C78 C65 109.2(3) . . ?
C65 C79 C69 109.9(3) . . ?

_diffrn_measured_fraction_theta_max 0.990
_diffrn_reflns_theta_full        27.50
_diffrn_measured_fraction_theta_full 0.990
_refine_diff_density_max         0.729
_refine_diff_density_min         -0.946
_refine_diff_density_rms         0.208

_database_code_depnum_ccdc_archive 'CCDC 980008'
#######################################################################
#
#                 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_9

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C70 H60 N2 O5 V'
_chemical_formula_sum            'C70 H60 N2 O5 V'
_chemical_formula_weight         1060.14

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   'P -1'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   12.286(3)
_cell_length_b                   13.190(3)
_cell_length_c                   19.728(4)
_cell_angle_alpha                70.80(3)
_cell_angle_beta                 74.35(3)
_cell_angle_gamma                87.75(3)
_cell_volume                     2902.9(11)
_cell_formula_units_Z            2
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    30994
_cell_measurement_theta_min      1.14
_cell_measurement_theta_max      25.00

_exptl_crystal_description       Plate
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.536
_exptl_crystal_size_mid          0.422
_exptl_crystal_size_min          0.254
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.213
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1114
_exptl_absorpt_coefficient_mu    0.224
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_absorpt_correction_T_min  0.5983
_exptl_absorpt_correction_T_max  1.0000

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Saturn724+ CCD'
_diffrn_measurement_method       'ω scans at fixed χ = 45°'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         none
_diffrn_standards_interval_count none
_diffrn_standards_interval_time  none
_diffrn_standards_decay_%        none
_diffrn_reflns_number            30994
_diffrn_reflns_av_R_equivalents  0.0465
_diffrn_reflns_av_unetI/netI     0.0404
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         1.14
_diffrn_reflns_theta_max         25.00
_reflns_number_total             10190
_reflns_number_gt                9357
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrystalClear (Rigaku Inc., 2007)'
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2007)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'CAMERON (Watkin et al, 1993)'
_computing_publication_material  'SHELX97 (Sheldrick, 1997)'


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

 Non-hydrogen atoms closer than 1.7 Α were restrainted to have the
 same U(ij) values with an e.s.d. of 0.01 (SIMU 0.01 0.01 1.7). 
 The thermal parameters of non-hydrogen atoms were restrained to
 approximate to isotropic behaviour with an e.s.d. of 0.01
 (ISOR 0.01).

 A number of C-C bonds were restrained in length: full details
 are given in _iucr_refine_instructions_details.
;

_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)+(0.1679P)²+2.4072P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         10190
_refine_ls_number_parameters     831
_refine_ls_number_restraints     1338
_refine_ls_R_factor_ref          0.0916
_refine_ls_R_factor_gt           0.0782
_refine_ls_wR_factor_ref         0.2527
_refine_ls_wR_factor_gt          0.2248
_refine_ls_goodness_of_fit_ref   1.092
_refine_ls_restrained_S_all      1.120
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
V1 V 0.82312(4) 0.41116(4) 0.21582(3) 0.0257(2) Uani 1 1 d U . .
O2 O 0.72808(18) 0.28299(17) 0.24996(13) 0.0330(5) Uani 1 1 d U . .
O1 O 0.85797(19) 0.48901(19) 0.13121(12) 0.0358(5) Uani 1 1 d U . .
O3 O 0.87199(18) 0.43513(18) 0.29390(12) 0.0310(5) Uani 1 1 d U . .
N1 N 0.9601(2) 0.3147(2) 0.19799(14) 0.0295(6) Uani 1 1 d U . .
N2 N 0.6818(2) 0.5006(2) 0.24406(14) 0.0275(5) Uani 1 1 d U . .
C1 C 1.0638(3) 0.3680(3) 0.14587(17) 0.0293(6) Uani 1 1 d U . .
C2 C 1.1167(3) 0.4444(3) 0.16156(19) 0.0341(7) Uani 1 1 d U . .
H2 H 1.0858 0.4594 0.2067 0.041 Uiso 1 1 calc R . .
C3 C 1.2151(3) 0.4992(3) 0.1115(2) 0.0375(7) Uani 1 1 d U . .
H3 H 1.2523 0.5511 0.1225 0.045 Uiso 1 1 calc R . .
C4 C 1.2593(3) 0.4786(3) 0.0455(2) 0.0380(7) Uani 1 1 d U . .
H4 H 1.3272 0.5159 0.0114 0.046 Uiso 1 1 calc R . .
C5 C 1.2044(3) 0.4029(3) 0.02876(18) 0.0341(7) Uani 1 1 d U . .
H5 H 1.2350 0.3897 -0.0170 0.041 Uiso 1 1 calc R . .
C6 C 1.1055(3) 0.3465(3) 0.07812(17) 0.0298(6) Uani 1 1 d U . .
C7 C 1.0391(3) 0.2754(3) 0.05685(17) 0.0313(7) Uani 1 1 d U . .
C8 C 0.9514(3) 0.3167(3) 0.0254(2) 0.0432(8) Uani 1 1 d U . .
H8 H 0.9355 0.3903 0.0166 0.052 Uiso 1 1 calc R . .
C9 C 0.8874(4) 0.2519(3) 0.0068(3) 0.0537(10) Uani 1 1 d U . .
H9 H 0.8274 0.2811 -0.0142 0.064 Uiso 1 1 calc R . .
C10 C 0.9095(4) 0.1460(3) 0.0184(3) 0.0534(10) Uani 1 1 d U . .
H10 H 0.8640 0.1016 0.0062 0.064 Uiso 1 1 calc R . .
C11 C 0.9971(4) 0.1041(3) 0.0475(3) 0.0522(10) Uani 1 1 d U . .
C19 C 0.9563(3) 0.2107(3) 0.22688(18) 0.0328(7) Uani 1 1 d U . .
H19 H 1.0247 0.1759 0.2154 0.039 Uiso 1 1 calc R . .
C20 C 0.8574(3) 0.1439(3) 0.27476(19) 0.0355(7) Uani 1 1 d U . .
C21 C 0.8746(4) 0.0355(3) 0.3113(2) 0.0503(9) Uani 1 1 d U . .
H21 H 0.9494 0.0113 0.3044 0.060 Uiso 1 1 calc R . .
C22 C 0.7851(4) -0.0360(3) 0.3569(3) 0.0564(10) Uani 1 1 d U . .
C24 C 0.8028(6) -0.1527(4) 0.3965(4) 0.0891(18) Uani 1 1 d U . .
H24A H 0.7806 -0.1981 0.3714 0.134 Uiso 1 1 calc R . .
H24B H 0.7564 -0.1743 0.4484 0.134 Uiso 1 1 calc R . .
H24C H 0.8828 -0.1611 0.3954 0.134 Uiso 1 1 calc R . .
C25 C 0.6767(4) 0.0022(3) 0.3647(2) 0.0511(9) Uani 1 1 d U . .
H25 H 0.6146 -0.0467 0.3962 0.061 Uiso 1 1 calc R . .
C26 C 0.6537(3) 0.1078(3) 0.32919(19) 0.0384(8) Uani 1 1 d U . .
C27 C 0.7466(3) 0.1810(3) 0.28427(18) 0.0326(7) Uani 1 1 d U . .
C28 C 0.5317(3) 0.1438(3) 0.3393(2) 0.0447(8) Uani 1 1 d U . .
C29 C 0.4465(4) 0.0515(4) 0.3958(3) 0.0623(12) Uani 1 1 d U . .
H29A H 0.4499 -0.0084 0.3763 0.093 Uiso 1 1 calc R . .
H29B H 0.3698 0.0774 0.4033 0.093 Uiso 1 1 calc R . .
H29C H 0.4658 0.0269 0.4434 0.093 Uiso 1 1 calc R . .
C30 C 0.5173(4) 0.2372(4) 0.3716(3) 0.0584(11) Uani 1 1 d U . .
H30A H 0.5430 0.2160 0.4170 0.088 Uiso 1 1 calc R . .
H30B H 0.4374 0.2538 0.3836 0.088 Uiso 1 1 calc R . .
H30C H 0.5625 0.3009 0.3347 0.088 Uiso 1 1 calc R . .
C31 C 0.4980(3) 0.1747(3) 0.2654(2) 0.0420(8) Uani 1 1 d DU . .
C32 C 0.5676(3) 0.1613(3) 0.2003(2) 0.0451(8) Uani 1 1 d DU . .
H32 H 0.6411 0.1359 0.1998 0.054 Uiso 1 1 calc R . .
C33 C 0.5305(4) 0.1845(4) 0.1359(3) 0.0611(11) Uani 1 1 d DU . .
H33 H 0.5791 0.1744 0.0924 0.073 Uiso 1 1 calc R . .
C34 C 0.4247(4) 0.2219(4) 0.1349(3) 0.0685(13) Uani 1 1 d DU . .
H34 H 0.3994 0.2367 0.0914 0.082 Uiso 1 1 calc R . .
C35 C 0.3562(4) 0.2374(4) 0.1981(3) 0.0708(13) Uani 1 1 d DU . .
H35 H 0.2834 0.2643 0.1978 0.085 Uiso 1 1 calc R . .
C36 C 0.3920(4) 0.2144(4) 0.2614(3) 0.0616(11) Uani 1 1 d DU . .
H36 H 0.3427 0.2259 0.3042 0.074 Uiso 1 1 calc R . .
C37 C 0.6187(2) 0.5413(2) 0.19045(16) 0.0268(6) Uani 1 1 d U A .
C38 C 0.5708(3) 0.4698(3) 0.16723(18) 0.0310(7) Uani 1 1 d U . .
H38 H 0.5804 0.3950 0.1867 0.037 Uiso 1 1 calc R . .
C39 C 0.5087(3) 0.5073(3) 0.11565(19) 0.0350(7) Uani 1 1 d U . .
H39 H 0.4743 0.4580 0.1007 0.042 Uiso 1 1 calc R . .
C40 C 0.4967(3) 0.6166(3) 0.0858(2) 0.0403(8) Uani 1 1 d U . .
H40 H 0.4542 0.6425 0.0504 0.048 Uiso 1 1 calc R . .
C41 C 0.5461(3) 0.6869(3) 0.1074(2) 0.0414(8) Uani 1 1 d U A .
H41 H 0.5370 0.7617 0.0866 0.050 Uiso 1 1 calc R . .
C42 C 0.6100(3) 0.6530(3) 0.15933(18) 0.0339(7) Uani 1 1 d U . .
C43 C 0.6567(9) 0.7357(12) 0.1758(8) 0.036(2) Uani 0.513(5) 1 d PU A 1
C44 C 0.7731(10) 0.7572(9) 0.1480(6) 0.053(2) Uani 0.513(5) 1 d PU A 1
H44 H 0.8177 0.7159 0.1205 0.064 Uiso 0.513(5) 1 calc PR A 1
C55 C 0.6537(3) 0.5291(3) 0.30292(18) 0.0308(7) Uani 1 1 d U . .
H55 H 0.5892 0.5709 0.3085 0.037 Uiso 1 1 calc R . .
C56 C 0.7108(3) 0.5036(3) 0.36106(18) 0.0341(7) Uani 1 1 d U . .
C57 C 0.6576(3) 0.5334(3) 0.4245(2) 0.0419(8) Uani 1 1 d U . .
H57 H 0.5880 0.5678 0.4266 0.050 Uiso 1 1 calc R . .
C58 C 0.7050(3) 0.5135(3) 0.4829(2) 0.0404(8) Uani 1 1 d U . .
C59 C 0.6511(4) 0.5467(4) 0.5500(2) 0.0568(11) Uani 1 1 d U . .
H59A H 0.5812 0.5825 0.5439 0.085 Uiso 1 1 calc R . .
H59B H 0.7035 0.5963 0.5549 0.085 Uiso 1 1 calc R . .
H59C H 0.6333 0.4829 0.5949 0.085 Uiso 1 1 calc R . .
C60 C 0.8058(3) 0.4608(3) 0.47810(18) 0.0358(7) Uani 1 1 d U . .
H60 H 0.8373 0.4444 0.5192 0.043 Uiso 1 1 calc R . .
C61 C 0.8160(3) 0.4561(3) 0.35543(17) 0.0303(7) Uani 1 1 d U . .
C62 C 0.8639(3) 0.4305(3) 0.41695(17) 0.0300(6) Uani 1 1 d U . .
C63 C 0.9749(3) 0.3729(3) 0.41503(18) 0.0327(7) Uani 1 1 d U . .
C64 C 0.9642(3) 0.2680(3) 0.3983(2) 0.0449(8) Uani 1 1 d U . .
H64A H 0.8902 0.2313 0.4274 0.067 Uiso 1 1 calc R . .
H64B H 1.0243 0.2211 0.4119 0.067 Uiso 1 1 calc R . .
H64C H 0.9713 0.2849 0.3450 0.067 Uiso 1 1 calc R . .
C65 C 1.0016(3) 0.3400(3) 0.49142(19) 0.0404(8) Uani 1 1 d U . .
H65A H 1.0102 0.4045 0.5042 0.061 Uiso 1 1 calc R . .
H65B H 1.0720 0.3021 0.4887 0.061 Uiso 1 1 calc R . .
H65C H 0.9395 0.2927 0.5298 0.061 Uiso 1 1 calc R . .
C66 C 1.0755(3) 0.4476(3) 0.35936(18) 0.0361(7) Uani 1 1 d DU . .
C67 C 1.0743(4) 0.5576(3) 0.3438(2) 0.0523(10) Uani 1 1 d DU . .
H67 H 1.0068 0.5879 0.3637 0.063 Uiso 1 1 calc R . .
C68 C 1.1685(4) 0.6250(4) 0.2998(3) 0.0711(13) Uani 1 1 d DU . .
H68 H 1.1660 0.7004 0.2901 0.085 Uiso 1 1 calc R . .
C69 C 1.2668(4) 0.5809(5) 0.2702(2) 0.0663(13) Uani 1 1 d DU . .
H69 H 1.3320 0.6262 0.2396 0.080 Uiso 1 1 calc R . .
C70 C 1.2699(3) 0.4735(5) 0.2847(2) 0.0603(11) Uani 1 1 d DU . .
H70 H 1.3374 0.4439 0.2641 0.072 Uiso 1 1 calc R . .
C71 C 1.1754(3) 0.4056(4) 0.3294(2) 0.0499(9) Uani 1 1 d DU . .
H71 H 1.1791 0.3302 0.3395 0.060 Uiso 1 1 calc R . .
C1A C 0.5963(10) 0.7986(8) 0.2142(6) 0.0459(18) Uani 0.513(5) 1 d PU A 1
C1B C 0.8252(10) 0.8405(10) 0.1607(7) 0.067(2) Uani 0.513(5) 1 d PU A 1
H1B H 0.9047 0.8556 0.1422 0.080 Uiso 0.513(5) 1 calc PR A 1
C1C C 0.4122(11) 0.8180(8) 0.2830(6) 0.069(2) Uani 0.513(5) 1 d PDU A 1
O5' O 0.4825(6) 0.7676(7) 0.2450(5) 0.0772(18) Uani 0.513(5) 1 d PU A 1
C1E C 0.6434(9) 0.8809(7) 0.2274(5) 0.0496(18) Uani 0.513(5) 1 d PU A 1
H1E H 0.5984 0.9231 0.2540 0.059 Uiso 0.513(5) 1 calc PR A 1
C1F C 0.3564(7) 0.9071(7) 0.2540(6) 0.063(2) Uani 0.513(5) 1 d PDU A 1
H1F H 0.3775 0.9413 0.2014 0.075 Uiso 0.513(5) 1 calc PR A 1
C1H C 0.3006(14) 0.8115(13) 0.4085(9) 0.084(3) Uani 0.513(5) 1 d PDU A 1
H1H H 0.2865 0.7833 0.4612 0.100 Uiso 0.513(5) 1 calc PR A 1
C1I C 0.2447(10) 0.8975(10) 0.3720(7) 0.085(3) Uani 0.513(5) 1 d PDU A 1
H1I H 0.1824 0.9216 0.4023 0.102 Uiso 0.513(5) 1 calc PR A 1
C1J C 0.2705(9) 0.9506(9) 0.2969(6) 0.076(2) Uani 0.513(5) 1 d PDU A 1
H1J H 0.2330 1.0123 0.2755 0.091 Uiso 0.513(5) 1 calc PR A 1
C1K C 0.7584(11) 0.8988(9) 0.2001(7) 0.055(2) Uani 0.513(5) 1 d PU A 1
H1K H 0.7934 0.9544 0.2091 0.066 Uiso 0.513(5) 1 calc PR A 1
C1L C 0.3762(10) 0.7729(10) 0.3616(7) 0.083(2) Uani 0.513(5) 1 d PDU A 1
H1L H 0.4093 0.7083 0.3835 0.100 Uiso 0.513(5) 1 calc PR A 1
O5 O 0.5296(9) 0.8221(7) 0.2164(5) 0.0690(18) Uani 0.487(5) 1 d PU A 2
C1P C 0.4728(11) 0.8040(10) 0.2983(7) 0.073(2) Uani 0.487(5) 1 d PU A 2
C1G C 0.3678(12) 0.8350(12) 0.3053(9) 0.081(2) Uani 0.487(5) 1 d PU A 2
H1G H 0.3400 0.8662 0.2629 0.098 Uiso 0.487(5) 1 calc PR A 2
C1M C 0.5196(10) 0.7623(8) 0.3538(6) 0.070(2) Uani 0.487(5) 1 d PU A 2
H1M H 0.5964 0.7434 0.3442 0.084 Uiso 0.487(5) 1 calc PR A 2
C1Q C 0.2920(17) 0.8185(16) 0.3852(10) 0.086(3) Uani 0.487(5) 1 d PU A 2
H1Q H 0.2151 0.8366 0.3965 0.103 Uiso 0.487(5) 1 calc PR A 2
C1R C 0.4553(11) 0.7465(9) 0.4260(7) 0.083(3) Uani 0.487(5) 1 d PU A 2
H1R H 0.4864 0.7160 0.4670 0.100 Uiso 0.487(5) 1 calc PR A 2
C1S C 0.3489(12) 0.7752(11) 0.4366(9) 0.089(3) Uani 0.487(5) 1 d PU A 2
H1S H 0.3076 0.7638 0.4870 0.107 Uiso 0.487(5) 1 calc PR A 2
C1T C 0.6476(10) 0.8117(8) 0.2020(6) 0.049(2) Uani 0.487(5) 1 d PU A 2
C1U C 0.7095(14) 0.8854(10) 0.2108(7) 0.059(3) Uani 0.487(5) 1 d PU A 2
H1U H 0.6744 0.9404 0.2290 0.070 Uiso 0.487(5) 1 calc PR A 2
C43A C 0.6902(10) 0.7308(12) 0.1744(9) 0.035(2) Uani 0.487(5) 1 d PU A 2
C1V C 0.8288(11) 0.8792(9) 0.1922(6) 0.062(2) Uani 0.487(5) 1 d PU A 2
H1V H 0.8756 0.9305 0.1971 0.074 Uiso 0.487(5) 1 calc PR A 2
C1W C 0.8762(9) 0.7961(7) 0.1665(5) 0.0518(18) Uani 0.487(5) 1 d PU A 2
H1W H 0.9558 0.7894 0.1553 0.062 Uiso 0.487(5) 1 calc PR A 2
C44A C 0.8079(8) 0.7230(7) 0.1571(5) 0.0379(18) Uani 0.487(5) 1 d PU A 2
H44A H 0.8411 0.6675 0.1388 0.045 Uiso 0.487(5) 1 calc PR A 2
C12 C 1.2057(4) 0.0470(3) 0.0842(2) 0.0518(10) Uani 1 1 d DU . .
C13 C 1.3411(5) 0.0006(5) -0.0104(3) 0.0779(14) Uani 1 1 d DU . .
H13 H 1.3828 0.0171 -0.0613 0.094 Uiso 1 1 calc R . .
C14 C 1.3517(6) -0.0904(5) 0.0403(3) 0.0856(16) Uani 1 1 d DU . .
H14 H 1.4147 -0.1312 0.0277 0.103 Uiso 1 1 calc R . .
C15 C 1.2693(5) 0.0688(5) 0.0124(3) 0.0791(14) Uani 1 1 d DU . .
H15 H 1.2622 0.1359 -0.0232 0.095 Uiso 1 1 calc R . .
C16 C 1.2780(8) -0.1308(7) 0.1104(4) 0.130(3) Uani 1 1 d DU . .
H16 H 1.2807 -0.2026 0.1417 0.156 Uiso 1 1 calc R . .
C17 C 1.1926(8) -0.0557(6) 0.1354(4) 0.121(2) Uani 1 1 d DU . .
H17 H 1.1357 -0.0769 0.1816 0.145 Uiso 1 1 calc R . .
H11 H 1.017(5) 0.030(5) 0.055(3) 0.076(16) Uiso 1 1 d . . .
O4 O 1.1437(3) 0.1268(3) 0.1034(2) 0.0677(9) Uani 1 1 d U . .
C18 C 1.0602(3) 0.1686(3) 0.0672(2) 0.0414(8) Uani 1 1 d U . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
V1 O1 1.595(2) . ?
V1 O2 1.912(2) . ?
V1 O3 1.915(2) . ?
V1 N1 2.093(3) . ?
V1 N2 2.113(3) . ?
O2 C27 1.334(4) . ?
O3 C61 1.333(4) . ?
N1 C19 1.298(4) . ?
N1 C1 1.436(4) . ?
N2 C55 1.292(4) . ?
N2 C37 1.430(4) . ?
C1 C2 1.378(5) . ?
C1 C6 1.414(4) . ?
C2 C3 1.383(5) . ?
C2 H2 0.9500 . ?
C3 C4 1.379(5) . ?
C3 H3 0.9500 . ?
C4 C5 1.398(5) . ?
C4 H4 0.9500 . ?
C5 C6 1.390(5) . ?
C5 H5 0.9500 . ?
C6 C7 1.492(4) . ?
C7 C18 1.381(5) . ?
C7 C8 1.391(5) . ?
C8 C9 1.377(5) . ?
C8 H8 0.9500 . ?
C9 C10 1.368(6) . ?
C9 H9 0.9500 . ?
C10 C11 1.368(6) . ?
C10 H10 0.9500 . ?
C11 C18 1.382(6) . ?
C11 H11 0.96(6) . ?
C19 C20 1.436(5) . ?
C19 H19 0.9500 . ?
C20 C21 1.411(5) . ?
C20 C27 1.413(5) . ?
C21 C22 1.377(6) . ?
C21 H21 0.9500 . ?
C22 C25 1.393(6) . ?
C22 C24 1.517(6) . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 C26 1.394(5) . ?
C25 H25 0.9500 . ?
C26 C27 1.414(5) . ?
C26 C28 1.535(5) . ?
C28 C31 1.543(6) . ?
C28 C30 1.547(6) . ?
C28 C29 1.550(5) . ?
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 C36 1.397(6) . ?
C31 C32 1.399(5) . ?
C32 C33 1.400(6) . ?
C32 H32 0.9500 . ?
C33 C34 1.374(7) . ?
C33 H33 0.9500 . ?
C34 C35 1.375(8) . ?
C34 H34 0.9500 . ?
C35 C36 1.372(7) . ?
C35 H35 0.9500 . ?
C36 H36 0.9500 . ?
C37 C38 1.385(4) . ?
C37 C42 1.409(4) . ?
C38 C39 1.385(5) . ?
C38 H38 0.9500 . ?
C39 C40 1.386(5) . ?
C39 H39 0.9500 . ?
C40 C41 1.362(6) . ?
C40 H40 0.9500 . ?
C41 C42 1.404(5) . ?
C41 H41 0.9500 . ?
C42 C43 1.418(18) . ?
C42 C43A 1.597(16) . ?
C43 C1A 1.368(19) . ?
C43 C44 1.390(14) . ?
C44 C1B 1.415(15) . ?
C44 H44 0.9500 . ?
C55 C56 1.443(5) . ?
C55 H55 0.9500 . ?
C56 C61 1.407(5) . ?
C56 C57 1.418(5) . ?
C57 C58 1.373(5) . ?
C57 H57 0.9500 . ?
C58 C60 1.391(5) . ?
C58 C59 1.506(5) . ?
C59 H59A 0.9800 . ?
C59 H59B 0.9800 . ?
C59 H59C 0.9800 . ?
C60 C62 1.399(4) . ?
C60 H60 0.9500 . ?
C61 C62 1.426(4) . ?
C62 C63 1.532(5) . ?
C63 C66 1.535(5) . ?
C63 C64 1.542(5) . ?
C63 C65 1.547(4) . ?
C64 H64A 0.9800 . ?
C64 H64B 0.9800 . ?
C64 H64C 0.9800 . ?
C65 H65A 0.9800 . ?
C65 H65B 0.9800 . ?
C65 H65C 0.9800 . ?
C66 C67 1.381(5) . ?
C66 C71 1.390(5) . ?
C67 C68 1.384(6) . ?
C67 H67 0.9500 . ?
C68 C69 1.388(7) . ?
C68 H68 0.9500 . ?
C69 C70 1.351(7) . ?
C69 H69 0.9500 . ?
C70 C71 1.392(6) . ?
C70 H70 0.9500 . ?
C71 H71 0.9500 . ?
C1A C1E 1.378(13) . ?
C1A O5' 1.384(13) . ?
C1B C1K 1.368(17) . ?
C1B H1B 0.9500 . ?
C1C O5' 1.296(13) . ?
C1C C1F 1.373(13) . ?
C1C C1L 1.415(14) . ?
C1E C1K 1.368(14) . ?
C1E H1E 0.9500 . ?
C1F C1J 1.396(12) . ?
C1F H1F 0.9500 . ?
C1H C1L 1.337(16) . ?
C1H C1I 1.396(16) . ?
C1H H1H 0.9500 . ?
C1I C1J 1.366(13) . ?
C1I H1I 0.9500 . ?
C1J H1J 0.9500 . ?
C1K H1K 0.9500 . ?
C1L H1L 0.9500 . ?
O5 C1T 1.410(13) . ?
O5 C1P 1.518(15) . ?
C1P C1G 1.323(19) . ?
C1P C1M 1.325(18) . ?
C1G C1Q 1.55(2) . ?
C1G H1G 0.9500 . ?
C1M C1R 1.380(16) . ?
C1M H1M 0.9500 . ?
C1Q C1S 1.35(2) . ?
C1Q H1Q 0.9500 . ?
C1R C1S 1.328(19) . ?
C1R H1R 0.9500 . ?
C1S H1S 0.9500 . ?
C1T C1U 1.338(19) . ?
C1T C43A 1.377(19) . ?
C1U C1V 1.418(18) . ?
C1U H1U 0.9500 . ?
C43A C44A 1.400(15) . ?
C1V C1W 1.398(15) . ?
C1V H1V 0.9500 . ?
C1W C44A 1.390(12) . ?
C1W H1W 0.9500 . ?
C44A H44A 0.9500 . ?
C12 C15 1.361(7) . ?
C12 O4 1.369(5) . ?
C12 C17 1.382(8) . ?
C13 C14 1.315(8) . ?
C13 C15 1.334(7) . ?
C13 H13 0.9500 . ?
C14 C16 1.377(9) . ?
C14 H14 0.9500 . ?
C15 H15 0.9500 . ?
C16 C17 1.512(9) . ?
C16 H16 0.9500 . ?
C17 H17 0.9500 . ?
O4 C18 1.399(5) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 V1 O2 123.33(12) . . ?
O1 V1 O3 123.94(12) . . ?
O2 V1 O3 112.73(10) . . ?
O1 V1 N1 92.93(11) . . ?
O2 V1 N1 86.76(10) . . ?
O3 V1 N1 89.74(10) . . ?
O1 V1 N2 92.14(11) . . ?
O2 V1 N2 90.98(10) . . ?
O3 V1 N2 86.90(10) . . ?
N1 V1 N2 174.89(10) . . ?
C27 O2 V1 130.7(2) . . ?
C61 O3 V1 132.3(2) . . ?
C19 N1 C1 118.0(3) . . ?
C19 N1 V1 125.1(2) . . ?
C1 N1 V1 116.8(2) . . ?
C55 N2 C37 117.3(3) . . ?
C55 N2 V1 125.1(2) . . ?
C37 N2 V1 117.29(19) . . ?
C2 C1 C6 121.5(3) . . ?
C2 C1 N1 118.5(3) . . ?
C6 C1 N1 119.9(3) . . ?
C1 C2 C3 119.8(3) . . ?
C1 C2 H2 120.1 . . ?
C3 C2 H2 120.1 . . ?
C4 C3 C2 120.2(3) . . ?
C4 C3 H3 119.9 . . ?
C2 C3 H3 119.9 . . ?
C3 C4 C5 120.0(3) . . ?
C3 C4 H4 120.0 . . ?
C5 C4 H4 120.0 . . ?
C6 C5 C4 121.0(3) . . ?
C6 C5 H5 119.5 . . ?
C4 C5 H5 119.5 . . ?
C5 C6 C1 117.5(3) . . ?
C5 C6 C7 121.2(3) . . ?
C1 C6 C7 121.0(3) . . ?
C18 C7 C8 117.5(3) . . ?
C18 C7 C6 122.8(3) . . ?
C8 C7 C6 119.6(3) . . ?
C9 C8 C7 120.6(3) . . ?
C9 C8 H8 119.7 . . ?
C7 C8 H8 119.7 . . ?
C10 C9 C8 120.7(4) . . ?
C10 C9 H9 119.7 . . ?
C8 C9 H9 119.7 . . ?
C11 C10 C9 119.9(4) . . ?
C11 C10 H10 120.0 . . ?
C9 C10 H10 120.0 . . ?
C10 C11 C18 119.5(4) . . ?
C10 C11 H11 122(3) . . ?
C18 C11 H11 118(3) . . ?
N1 C19 C20 125.4(3) . . ?
N1 C19 H19 117.3 . . ?
C20 C19 H19 117.3 . . ?
C21 C20 C27 120.0(3) . . ?
C21 C20 C19 116.7(3) . . ?
C27 C20 C19 123.3(3) . . ?
C22 C21 C20 121.3(4) . . ?
C22 C21 H21 119.3 . . ?
C20 C21 H21 119.3 . . ?
C21 C22 C25 117.6(4) . . ?
C21 C22 C24 121.7(4) . . ?
C25 C22 C24 120.7(4) . . ?
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 C26 124.0(4) . . ?
C22 C25 H25 118.0 . . ?
C26 C25 H25 118.0 . . ?
C25 C26 C27 117.7(3) . . ?
C25 C26 C28 121.2(3) . . ?
C27 C26 C28 121.0(3) . . ?
O2 C27 C20 121.2(3) . . ?
O2 C27 C26 119.5(3) . . ?
C20 C27 C26 119.3(3) . . ?
C26 C28 C31 111.2(3) . . ?
C26 C28 C30 110.0(3) . . ?
C31 C28 C30 111.8(3) . . ?
C26 C28 C29 111.0(3) . . ?
C31 C28 C29 106.1(3) . . ?
C30 C28 C29 106.6(3) . . ?
C28 C29 H29A 109.5 . . ?
C28 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C28 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C28 C30 H30A 109.5 . . ?
C28 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C28 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C36 C31 C32 116.1(4) . . ?
C36 C31 C28 120.6(4) . . ?
C32 C31 C28 123.2(3) . . ?
C31 C32 C33 121.1(4) . . ?
C31 C32 H32 119.5 . . ?
C33 C32 H32 119.5 . . ?
C34 C33 C32 120.7(5) . . ?
C34 C33 H33 119.6 . . ?
C32 C33 H33 119.6 . . ?
C33 C34 C35 118.8(4) . . ?
C33 C34 H34 120.6 . . ?
C35 C34 H34 120.6 . . ?
C36 C35 C34 120.7(4) . . ?
C36 C35 H35 119.7 . . ?
C34 C35 H35 119.7 . . ?
C35 C36 C31 122.5(5) . . ?
C35 C36 H36 118.7 . . ?
C31 C36 H36 118.7 . . ?
C38 C37 C42 120.7(3) . . ?
C38 C37 N2 119.0(3) . . ?
C42 C37 N2 120.3(3) . . ?
C39 C38 C37 120.1(3) . . ?
C39 C38 H38 119.9 . . ?
C37 C38 H38 119.9 . . ?
C38 C39 C40 120.1(3) . . ?
C38 C39 H39 120.0 . . ?
C40 C39 H39 120.0 . . ?
C41 C40 C39 119.7(3) . . ?
C41 C40 H40 120.1 . . ?
C39 C40 H40 120.1 . . ?
C40 C41 C42 122.4(3) . . ?
C40 C41 H41 118.8 . . ?
C42 C41 H41 118.8 . . ?
C41 C42 C37 117.0(3) . . ?
C41 C42 C43 115.8(6) . . ?
C37 C42 C43 127.2(6) . . ?
C41 C42 C43A 124.5(6) . . ?
C37 C42 C43A 117.5(6) . . ?
C1A C43 C44 117.6(13) . . ?
C1A C43 C42 125.4(9) . . ?
C44 C43 C42 116.9(12) . . ?
C43 C44 C1B 120.0(12) . . ?
C43 C44 H44 120.0 . . ?
C1B C44 H44 120.0 . . ?
N2 C55 C56 126.3(3) . . ?
N2 C55 H55 116.8 . . ?
C56 C55 H55 116.8 . . ?
C61 C56 C57 120.4(3) . . ?
C61 C56 C55 123.2(3) . . ?
C57 C56 C55 116.4(3) . . ?
C58 C57 C56 121.2(3) . . ?
C58 C57 H57 119.4 . . ?
C56 C57 H57 119.4 . . ?
C57 C58 C60 117.4(3) . . ?
C57 C58 C59 121.9(3) . . ?
C60 C58 C59 120.6(3) . . ?
C58 C59 H59A 109.5 . . ?
C58 C59 H59B 109.5 . . ?
H59A C59 H59B 109.5 . . ?
C58 C59 H59C 109.5 . . ?
H59A C59 H59C 109.5 . . ?
H59B C59 H59C 109.5 . . ?
C58 C60 C62 124.6(3) . . ?
C58 C60 H60 117.7 . . ?
C62 C60 H60 117.7 . . ?
O3 C61 C56 121.6(3) . . ?
O3 C61 C62 119.4(3) . . ?
C56 C61 C62 119.0(3) . . ?
C60 C62 C61 117.2(3) . . ?
C60 C62 C63 122.0(3) . . ?
C61 C62 C63 120.8(3) . . ?
C62 C63 C66 111.0(3) . . ?
C62 C63 C64 109.6(3) . . ?
C66 C63 C64 112.7(3) . . ?
C62 C63 C65 111.5(3) . . ?
C66 C63 C65 105.5(3) . . ?
C64 C63 C65 106.5(3) . . ?
C63 C64 H64A 109.5 . . ?
C63 C64 H64B 109.5 . . ?
H64A C64 H64B 109.5 . . ?
C63 C64 H64C 109.5 . . ?
H64A C64 H64C 109.5 . . ?
H64B C64 H64C 109.5 . . ?
C63 C65 H65A 109.5 . . ?
C63 C65 H65B 109.5 . . ?
H65A C65 H65B 109.5 . . ?
C63 C65 H65C 109.5 . . ?
H65A C65 H65C 109.5 . . ?
H65B C65 H65C 109.5 . . ?
C67 C66 C71 117.8(3) . . ?
C67 C66 C63 121.1(3) . . ?
C71 C66 C63 120.7(3) . . ?
C66 C67 C68 121.8(4) . . ?
C66 C67 H67 119.1 . . ?
C68 C67 H67 119.1 . . ?
C67 C68 C69 119.1(5) . . ?
C67 C68 H68 120.4 . . ?
C69 C68 H68 120.4 . . ?
C70 C69 C68 120.1(4) . . ?
C70 C69 H69 120.0 . . ?
C68 C69 H69 120.0 . . ?
C69 C70 C71 120.8(4) . . ?
C69 C70 H70 119.6 . . ?
C71 C70 H70 119.6 . . ?
C66 C71 C70 120.3(4) . . ?
C66 C71 H71 119.8 . . ?
C70 C71 H71 119.8 . . ?
C43 C1A C1E 124.3(11) . . ?
C43 C1A O5' 114.5(9) . . ?
C1E C1A O5' 121.1(10) . . ?
C1K C1B C44 118.5(10) . . ?
C1K C1B H1B 120.8 . . ?
C44 C1B H1B 120.8 . . ?
O5' C1C C1F 126.0(11) . . ?
O5' C1C C1L 119.4(11) . . ?
C1F C1C C1L 114.2(11) . . ?
C1C O5' C1A 123.0(9) . . ?
C1K C1E C1A 116.6(10) . . ?
C1K C1E H1E 121.7 . . ?
C1A C1E H1E 121.7 . . ?
C1C C1F C1J 124.1(11) . . ?
C1C C1F H1F 117.9 . . ?
C1J C1F H1F 117.9 . . ?
C1L C1H C1I 112.9(14) . . ?
C1L C1H H1H 123.5 . . ?
C1I C1H H1H 123.5 . . ?
C1J C1I C1H 126.5(13) . . ?
C1J C1I H1I 116.8 . . ?
C1H C1I H1I 116.8 . . ?
C1I C1J C1F 114.8(11) . . ?
C1I C1J H1J 122.6 . . ?
C1F C1J H1J 122.6 . . ?
C1B C1K C1E 123.0(10) . . ?
C1B C1K H1K 118.5 . . ?
C1E C1K H1K 118.5 . . ?
C1H C1L C1C 126.9(14) . . ?
C1H C1L H1L 116.5 . . ?
C1C C1L H1L 116.5 . . ?
C1T O5 C1P 112.3(10) . . ?
C1G C1P C1M 125.5(13) . . ?
C1G C1P O5 108.7(13) . . ?
C1M C1P O5 125.8(11) . . ?
C1P C1G C1Q 117.5(15) . . ?
C1P C1G H1G 121.3 . . ?
C1Q C1G H1G 121.3 . . ?
C1P C1M C1R 119.0(12) . . ?
C1P C1M H1M 120.5 . . ?
C1R C1M H1M 120.5 . . ?
C1S C1Q C1G 111.4(16) . . ?
C1S C1Q H1Q 124.3 . . ?
C1G C1Q H1Q 124.3 . . ?
C1S C1R C1M 118.3(14) . . ?
C1S C1R H1R 120.8 . . ?
C1M C1R H1R 120.8 . . ?
C1R C1S C1Q 128.3(16) . . ?
C1R C1S H1S 115.9 . . ?
C1Q C1S H1S 115.9 . . ?
C1U C1T C43A 125.4(12) . . ?
C1U C1T O5 117.9(11) . . ?
C43A C1T O5 116.5(10) . . ?
C1T C1U C1V 118.2(11) . . ?
C1T C1U H1U 120.9 . . ?
C1V C1U H1U 120.9 . . ?
C1T C43A C44A 116.8(12) . . ?
C1T C43A C42 121.6(9) . . ?
C44A C43A C42 121.5(11) . . ?
C1W C1V C1U 118.7(10) . . ?
C1W C1V H1V 120.6 . . ?
C1U C1V H1V 120.6 . . ?
C44A C1W C1V 120.6(10) . . ?
C44A C1W H1W 119.7 . . ?
C1V C1W H1W 119.7 . . ?
C1W C44A C43A 120.3(11) . . ?
C1W C44A H44A 119.9 . . ?
C43A C44A H44A 119.9 . . ?
C15 C12 O4 118.5(4) . . ?
C15 C12 C17 121.7(5) . . ?
O4 C12 C17 119.4(5) . . ?
C14 C13 C15 117.2(6) . . ?
C14 C13 H13 121.4 . . ?
C15 C13 H13 121.4 . . ?
C13 C14 C16 124.7(6) . . ?
C13 C14 H14 117.7 . . ?
C16 C14 H14 117.7 . . ?
C13 C15 C12 123.3(6) . . ?
C13 C15 H15 118.4 . . ?
C12 C15 H15 118.4 . . ?
C14 C16 C17 116.9(6) . . ?
C14 C16 H16 121.5 . . ?
C17 C16 H16 121.5 . . ?
C12 C17 C16 113.2(6) . . ?
C12 C17 H17 123.4 . . ?
C16 C17 H17 123.4 . . ?
C12 O4 C18 117.9(3) . . ?
C7 C18 C11 121.8(3) . . ?
C7 C18 O4 116.7(3) . . ?
C11 C18 O4 121.4(3) . . ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         1.197
_refine_diff_density_min         -0.677
_refine_diff_density_rms         0.182

_database_code_depnum_ccdc_archive 'CCDC 980009'
#######################################################################
#
#                 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_10

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C54 H60 N2 O8 V2'
_chemical_formula_sum            'C54 H60 N2 O8 V2'
_chemical_formula_weight         966.92

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P2(1)/c
_symmetry_space_group_name_Hall  '-P 2ybc'

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

_cell_length_a                   11.9699(5)
_cell_length_b                   15.6408(6)
_cell_length_c                   13.9536(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 99.3405(6)
_cell_angle_gamma                90.00
_cell_volume                     2577.74(17)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    8390
_cell_measurement_theta_min      2.46
_cell_measurement_theta_max      30.35

_exptl_crystal_description       block
_exptl_crystal_colour            'dark red'
_exptl_crystal_size_max          0.58
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.12
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.246
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1016
_exptl_absorpt_coefficient_mu    0.416
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.795
_exptl_absorpt_correction_T_max  0.952
_exptl_absorpt_process_details   'SADABS v2008/1, Sheldrick, G.M., (2008)'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX 2 CCD diffractometer'
_diffrn_measurement_method       'ω rotation with narrow frames'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        0
_diffrn_reflns_number            29752
_diffrn_reflns_av_R_equivalents  0.0315
_diffrn_reflns_av_unetI/netI     0.0301
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         1.97
_diffrn_reflns_theta_max         30.56
_reflns_number_total             7812
_reflns_number_gt                6246
_reflns_threshold_expression     I>2σ(I)

_computing_data_collection       'Bruker APEX 2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL and local programs'

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0543P)²+0.8316P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   'all non-H atoms found by direct methods'
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         7812
_refine_ls_number_parameters     304
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0506
_refine_ls_R_factor_gt           0.0378
_refine_ls_wR_factor_ref         0.1069
_refine_ls_wR_factor_gt          0.0986
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_restrained_S_all      1.024
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
V1 V 0.019540(18) 0.442159(14) 0.432064(15) 0.01816(7) Uani 1 1 d . . .
O1 O 0.12057(8) 0.45317(6) 0.34714(7) 0.02031(18) Uani 1 1 d . . .
O3 O 0.01162(9) 0.44505(6) 0.56152(7) 0.02285(19) Uani 1 1 d . . .
O4 O -0.09073(8) 0.39690(7) 0.37446(7) 0.0263(2) Uani 1 1 d . . .
C1 C 0.23082(10) 0.43967(8) 0.34896(9) 0.0188(2) Uani 1 1 d . . .
C2 C 0.29225(11) 0.49056(8) 0.29149(10) 0.0207(2) Uani 1 1 d . . .
C3 C 0.40745(11) 0.47323(9) 0.29928(10) 0.0245(3) Uani 1 1 d . . .
H3 H 0.4503 0.5072 0.2620 0.029 Uiso 1 1 calc R . .
C4 C 0.46495(11) 0.40899(9) 0.35848(10) 0.0236(3) Uani 1 1 d . . .
C5 C 0.40161(11) 0.35892(9) 0.41054(10) 0.0225(3) Uani 1 1 d . . .
H5 H 0.4372 0.3137 0.4495 0.027 Uiso 1 1 calc R . .
C6 C 0.28481(11) 0.37367(8) 0.40702(9) 0.0201(2) Uani 1 1 d . . .
C7 C 0.23356(12) 0.56130(9) 0.22617(10) 0.0240(3) Uani 1 1 d . . .
C8 C 0.18557(14) 0.62996(10) 0.28771(12) 0.0326(3) Uani 1 1 d . . .
H8A H 0.1324 0.6033 0.3252 0.049 Uiso 1 1 calc R . .
H8B H 0.1461 0.6738 0.2448 0.049 Uiso 1 1 calc R . .
H8C H 0.2477 0.6564 0.3322 0.049 Uiso 1 1 calc R . .
C9 C 0.13771(13) 0.52294(11) 0.15203(11) 0.0299(3) Uani 1 1 d . . .
H9A H 0.1688 0.4791 0.1136 0.045 Uiso 1 1 calc R . .
H9B H 0.1023 0.5682 0.1089 0.045 Uiso 1 1 calc R . .
H9C H 0.0810 0.4971 0.1863 0.045 Uiso 1 1 calc R . .
C10 C 0.31577(13) 0.60621(11) 0.16914(12) 0.0346(3) Uani 1 1 d . . .
H10A H 0.3771 0.6325 0.2146 0.052 Uiso 1 1 calc R . .
H10B H 0.2752 0.6505 0.1276 0.052 Uiso 1 1 calc R . .
H10C H 0.3475 0.5643 0.1288 0.052 Uiso 1 1 calc R . .
C11 C 0.59297(11) 0.39874(10) 0.36354(11) 0.0279(3) Uani 1 1 d . . .
C12 C 0.62018(15) 0.37778(15) 0.26261(14) 0.0478(5) Uani 1 1 d . . .
H12A H 0.7022 0.3712 0.2664 0.072 Uiso 1 1 calc R . .
H12B H 0.5935 0.4243 0.2177 0.072 Uiso 1 1 calc R . .
H12C H 0.5823 0.3244 0.2392 0.072 Uiso 1 1 calc R . .
C13 C 0.65077(13) 0.48283(11) 0.40010(16) 0.0425(4) Uani 1 1 d . . .
H13A H 0.6340 0.4956 0.4650 0.064 Uiso 1 1 calc R . .
H13B H 0.6224 0.5293 0.3556 0.064 Uiso 1 1 calc R . .
H13C H 0.7328 0.4773 0.4031 0.064 Uiso 1 1 calc R . .
C14 C 0.64034(13) 0.32796(12) 0.43336(15) 0.0412(4) Uani 1 1 d . . .
H14A H 0.6259 0.3417 0.4988 0.062 Uiso 1 1 calc R . .
H14B H 0.7221 0.3229 0.4342 0.062 Uiso 1 1 calc R . .
H14C H 0.6035 0.2737 0.4121 0.062 Uiso 1 1 calc R . .
C15 C 0.22350(11) 0.31988(8) 0.46423(9) 0.0207(2) Uani 1 1 d . . .
H15 H 0.2622 0.2718 0.4952 0.025 Uiso 1 1 calc R . .
N1 N 0.11990(9) 0.33182(7) 0.47676(8) 0.0192(2) Uani 1 1 d . . .
C16 C 0.07270(11) 0.27443(8) 0.53959(9) 0.0209(2) Uani 1 1 d . . .
C17 C -0.02833(12) 0.23257(9) 0.50547(10) 0.0253(3) Uani 1 1 d . . .
H17 H -0.0623 0.2387 0.4394 0.030 Uiso 1 1 calc R . .
C18 C -0.07981(13) 0.18194(10) 0.56711(11) 0.0299(3) Uani 1 1 d . . .
H18 H -0.1484 0.1530 0.5432 0.036 Uiso 1 1 calc R . .
C19 C -0.03110(13) 0.17362(9) 0.66379(11) 0.0288(3) Uani 1 1 d . . .
H19 H -0.0669 0.1395 0.7063 0.035 Uiso 1 1 calc R . .
C20 C 0.06942(13) 0.21490(10) 0.69854(10) 0.0281(3) Uani 1 1 d . . .
H20 H 0.1031 0.2086 0.7646 0.034 Uiso 1 1 calc R . .
C21 C 0.12132(11) 0.26567(9) 0.63686(10) 0.0237(3) Uani 1 1 d . . .
O2 O 0.22412(9) 0.30564(8) 0.66692(7) 0.0311(2) Uani 1 1 d . . .
C22 C 0.24364(12) 0.34482(10) 0.75697(10) 0.0271(3) Uani 1 1 d . . .
C23 C 0.35320(13) 0.33999(11) 0.80703(11) 0.0311(3) Uani 1 1 d . . .
H23 H 0.4093 0.3087 0.7809 0.037 Uiso 1 1 calc R . .
C24 C 0.38032(14) 0.38114(12) 0.89561(13) 0.0397(4) Uani 1 1 d . . .
H24 H 0.4555 0.3785 0.9302 0.048 Uiso 1 1 calc R . .
C25 C 0.29833(17) 0.42612(14) 0.93391(14) 0.0491(5) Uani 1 1 d . . .
H25 H 0.3169 0.4538 0.9950 0.059 Uiso 1 1 calc R . .
C26 C 0.18951(17) 0.43075(14) 0.88313(16) 0.0499(5) Uani 1 1 d . . .
H26 H 0.1336 0.4619 0.9096 0.060 Uiso 1 1 calc R . .
C27 C 0.16073(15) 0.39055(12) 0.79390(13) 0.0392(4) Uani 1 1 d . . .
H27 H 0.0859 0.3942 0.7588 0.047 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 O4 1.5952(10) . ?
V1 O3 1.8084(10) 3_566 ?
V1 O3 1.8247(9) . ?
V1 O1 1.8334(9) . ?
V1 N1 2.1371(11) . ?
V1 V1 2.7157(4) 3_566 ?
O1 C1 1.3326(15) . ?
O3 V1 1.8084(10) 3_566 ?
C1 C6 1.4035(18) . ?
C1 C2 1.4174(18) . ?
C2 C3 1.3921(18) . ?
C2 C7 1.5299(19) . ?
C3 C4 1.408(2) . ?
C4 C5 1.3765(19) . ?
C4 C11 1.5309(18) . ?
C5 C6 1.4100(17) . ?
C6 C15 1.4401(18) . ?
C7 C10 1.5328(19) . ?
C7 C9 1.537(2) . ?
C7 C8 1.543(2) . ?
C11 C14 1.522(2) . ?
C11 C12 1.532(2) . ?
C11 C13 1.534(2) . ?
C15 N1 1.2937(16) . ?
N1 C16 1.4332(16) . ?
C16 C17 1.3896(19) . ?
C16 C21 1.3939(18) . ?
C17 C18 1.3852(19) . ?
C18 C19 1.386(2) . ?
C19 C20 1.382(2) . ?
C20 C21 1.3895(19) . ?
C21 O2 1.3833(17) . ?
O2 C22 1.3833(18) . ?
C22 C23 1.384(2) . ?
C22 C27 1.389(2) . ?
C23 C24 1.384(2) . ?
C24 C25 1.383(3) . ?
C25 C26 1.380(3) . ?
C26 C27 1.388(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O4 V1 O3 107.30(5) . 3_566 ?
O4 V1 O3 109.76(5) . . ?
O3 V1 O3 83.25(4) 3_566 . ?
O4 V1 O1 107.13(5) . . ?
O3 V1 O1 95.93(4) 3_566 . ?
O3 V1 O1 141.55(5) . . ?
O4 V1 N1 99.71(5) . . ?
O3 V1 N1 152.13(5) 3_566 . ?
O3 V1 N1 81.27(4) . . ?
O1 V1 N1 82.30(4) . . ?
O4 V1 V1 115.16(4) . 3_566 ?
O3 V1 V1 41.86(3) 3_566 3_566 ?
O3 V1 V1 41.40(3) . 3_566 ?
O1 V1 V1 126.52(3) . 3_566 ?
N1 V1 V1 119.12(3) . 3_566 ?
C1 O1 V1 136.70(8) . . ?
V1 O3 V1 96.75(4) 3_566 . ?
O1 C1 C6 119.30(11) . . ?
O1 C1 C2 120.22(11) . . ?
C6 C1 C2 120.47(12) . . ?
C3 C2 C1 116.41(12) . . ?
C3 C2 C7 122.73(12) . . ?
C1 C2 C7 120.86(11) . . ?
C2 C3 C4 124.66(13) . . ?
C5 C4 C3 117.20(12) . . ?
C5 C4 C11 123.30(13) . . ?
C3 C4 C11 119.49(12) . . ?
C4 C5 C6 121.10(12) . . ?
C1 C6 C5 120.10(12) . . ?
C1 C6 C15 121.42(11) . . ?
C5 C6 C15 118.47(12) . . ?
C2 C7 C10 111.67(12) . . ?
C2 C7 C9 109.83(12) . . ?
C10 C7 C9 107.55(12) . . ?
C2 C7 C8 110.38(11) . . ?
C10 C7 C8 107.36(12) . . ?
C9 C7 C8 109.98(12) . . ?
C14 C11 C4 111.82(12) . . ?
C14 C11 C12 108.67(14) . . ?
C4 C11 C12 109.92(13) . . ?
C14 C11 C13 108.04(14) . . ?
C4 C11 C13 108.63(12) . . ?
C12 C11 C13 109.73(15) . . ?
N1 C15 C6 125.20(12) . . ?
C15 N1 C16 118.29(11) . . ?
C15 N1 V1 125.66(9) . . ?
C16 N1 V1 115.18(8) . . ?
C17 C16 C21 119.33(12) . . ?
C17 C16 N1 119.54(12) . . ?
C21 C16 N1 120.89(12) . . ?
C18 C17 C16 120.45(13) . . ?
C17 C18 C19 119.91(14) . . ?
C20 C19 C18 120.15(13) . . ?
C19 C20 C21 120.06(13) . . ?
O2 C21 C20 122.38(12) . . ?
O2 C21 C16 117.46(12) . . ?
C20 C21 C16 120.09(13) . . ?
C22 O2 C21 119.11(11) . . ?
O2 C22 C23 116.15(13) . . ?
O2 C22 C27 122.67(14) . . ?
C23 C22 C27 121.10(15) . . ?
C22 C23 C24 119.39(15) . . ?
C25 C24 C23 120.20(16) . . ?
C26 C25 C24 119.87(17) . . ?
C25 C26 C27 120.87(18) . . ?
C26 C27 C22 118.56(16) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O4 V1 O1 C1 -134.67(12) . . . . ?
O3 V1 O1 C1 115.15(12) 3_566 . . . ?
O3 V1 O1 C1 28.54(15) . . . . ?
N1 V1 O1 C1 -36.83(12) . . . . ?
V1 V1 O1 C1 83.89(12) 3_566 . . . ?
O4 V1 O3 V1 -106.01(5) . . . 3_566 ?
O3 V1 O3 V1 0.0 3_566 . . 3_566 ?
O1 V1 O3 V1 91.05(7) . . . 3_566 ?
N1 V1 O3 V1 156.75(5) . . . 3_566 ?
V1 O1 C1 C6 31.84(19) . . . . ?
V1 O1 C1 C2 -149.26(10) . . . . ?
O1 C1 C2 C3 178.76(12) . . . . ?
C6 C1 C2 C3 -2.35(18) . . . . ?
O1 C1 C2 C7 -0.32(19) . . . . ?
C6 C1 C2 C7 178.57(12) . . . . ?
C1 C2 C3 C4 0.8(2) . . . . ?
C7 C2 C3 C4 179.88(13) . . . . ?
C2 C3 C4 C5 1.4(2) . . . . ?
C2 C3 C4 C11 -177.64(13) . . . . ?
C3 C4 C5 C6 -2.2(2) . . . . ?
C11 C4 C5 C6 176.84(13) . . . . ?
O1 C1 C6 C5 -179.44(12) . . . . ?
C2 C1 C6 C5 1.66(19) . . . . ?
O1 C1 C6 C15 0.37(19) . . . . ?
C2 C1 C6 C15 -178.53(12) . . . . ?
C4 C5 C6 C1 0.7(2) . . . . ?
C4 C5 C6 C15 -179.10(12) . . . . ?
C3 C2 C7 C10 2.40(19) . . . . ?
C1 C2 C7 C10 -178.58(13) . . . . ?
C3 C2 C7 C9 121.62(14) . . . . ?
C1 C2 C7 C9 -59.36(16) . . . . ?
C3 C2 C7 C8 -116.94(15) . . . . ?
C1 C2 C7 C8 62.08(16) . . . . ?
C5 C4 C11 C14 -0.7(2) . . . . ?
C3 C4 C11 C14 178.30(14) . . . . ?
C5 C4 C11 C12 120.08(17) . . . . ?
C3 C4 C11 C12 -60.91(18) . . . . ?
C5 C4 C11 C13 -119.84(16) . . . . ?
C3 C4 C11 C13 59.16(18) . . . . ?
C1 C6 C15 N1 -8.0(2) . . . . ?
C5 C6 C15 N1 171.79(13) . . . . ?
C6 C15 N1 C16 -177.23(12) . . . . ?
C6 C15 N1 V1 -8.49(19) . . . . ?
O4 V1 N1 C15 128.86(11) . . . . ?
O3 V1 N1 C15 -65.44(15) 3_566 . . . ?
O3 V1 N1 C15 -122.44(11) . . . . ?
O1 V1 N1 C15 22.69(11) . . . . ?
V1 V1 N1 C15 -105.05(10) 3_566 . . . ?
O4 V1 N1 C16 -62.09(9) . . . . ?
O3 V1 N1 C16 103.61(11) 3_566 . . . ?
O3 V1 N1 C16 46.61(9) . . . . ?
O1 V1 N1 C16 -168.26(9) . . . . ?
V1 V1 N1 C16 64.00(9) 3_566 . . . ?
C15 N1 C16 C17 -126.16(14) . . . . ?
V1 N1 C16 C17 63.93(14) . . . . ?
C15 N1 C16 C21 59.48(17) . . . . ?
V1 N1 C16 C21 -110.43(12) . . . . ?
C21 C16 C17 C18 -0.6(2) . . . . ?
N1 C16 C17 C18 -175.08(13) . . . . ?
C16 C17 C18 C19 0.7(2) . . . . ?
C17 C18 C19 C20 -0.8(2) . . . . ?
C18 C19 C20 C21 0.7(2) . . . . ?
C19 C20 C21 O2 -177.40(13) . . . . ?
C19 C20 C21 C16 -0.6(2) . . . . ?
C17 C16 C21 O2 177.50(12) . . . . ?
N1 C16 C21 O2 -8.13(19) . . . . ?
C17 C16 C21 C20 0.6(2) . . . . ?
N1 C16 C21 C20 174.94(12) . . . . ?
C20 C21 O2 C22 -42.58(19) . . . . ?
C16 C21 O2 C22 140.57(13) . . . . ?
C21 O2 C22 C23 144.35(14) . . . . ?
C21 O2 C22 C27 -39.0(2) . . . . ?
O2 C22 C23 C24 177.00(14) . . . . ?
C27 C22 C23 C24 0.3(2) . . . . ?
C22 C23 C24 C25 0.5(3) . . . . ?
C23 C24 C25 C26 -0.7(3) . . . . ?
C24 C25 C26 C27 0.2(3) . . . . ?
C25 C26 C27 C22 0.5(3) . . . . ?
O2 C22 C27 C26 -177.26(17) . . . . ?
C23 C22 C27 C26 -0.8(3) . . . . ?

_diffrn_measured_fraction_theta_max 0.991
_diffrn_reflns_theta_full        30.56
_diffrn_measured_fraction_theta_full 0.991
_refine_diff_density_max         0.440
_refine_diff_density_min         -0.399
_refine_diff_density_rms         0.056

_database_code_depnum_ccdc_archive 'CCDC 980010'
#######################################################################
#
#                 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_11

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C65 H72 N2 O8 V2, 4(C2 H3 N)'
_chemical_formula_sum            'C73 H84 N6 O8 V2'
_chemical_formula_weight         1275.35

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   P-1

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   13.547(3)
_cell_length_b                   13.980(3)
_cell_length_c                   21.040(4)
_cell_angle_alpha                105.21(3)
_cell_angle_beta                 90.24(3)
_cell_angle_gamma                117.26(3)
_cell_volume                     3381.7(12)
_cell_formula_units_Z            2
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    24375
_cell_measurement_theta_min      1.01
_cell_measurement_theta_max      25.00

_exptl_crystal_description       Prism
_exptl_crystal_colour            Colorless
_exptl_crystal_size_max          0.2000
_exptl_crystal_size_mid          0.2000
_exptl_crystal_size_min          0.2000
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.251
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1348
_exptl_absorpt_coefficient_mu    0.335
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_absorpt_correction_T_min  0.5789
_exptl_absorpt_correction_T_max  1.0000

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Saturn724+ CCD'
_diffrn_measurement_method       'ω scans at fixed χ = 45°'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         none
_diffrn_standards_interval_count none
_diffrn_standards_interval_time  none
_diffrn_standards_decay_%        none
_diffrn_reflns_number            24375
_diffrn_reflns_av_R_equivalents  0.0826
_diffrn_reflns_av_unetI/netI     0.0829
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         1.01
_diffrn_reflns_theta_max         25.00
_reflns_number_total             11669
_reflns_number_gt                10464
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrystalClear (Rigaku Inc., 2007)'
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2007)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'XP in Siemens SHELXTL (Sheldrick, 1994)'
_computing_publication_material  'SHELX97 (Sheldrick, 1997)'

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

 Non-hydrogen atoms closer than 1.7 Α were restrainted to have the
 same U(ij) values with an e.s.d. of 0.02 (SIMU 0.02 0.04 1.7). 
 The thermal parameters of non-hydrogen atoms were restrained to
 approximate to isotropic behaviour with an e.s.d. of 0.01
 (ISOR 0.02).
;

_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)+(0.0725P)²+42.5580P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         11669
_refine_ls_number_parameters     811
_refine_ls_number_restraints     1080
_refine_ls_R_factor_ref          0.1486
_refine_ls_R_factor_gt           0.1386
_refine_ls_wR_factor_ref         0.3335
_refine_ls_wR_factor_gt          0.3266
_refine_ls_goodness_of_fit_ref   1.110
_refine_ls_restrained_S_all      1.069
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
V1 V 0.40294(10) 0.84581(10) 0.13894(6) 0.0246(3) Uani 1 1 d U . .
V2 V 0.64961(10) 1.02942(11) 0.21034(6) 0.0262(3) Uani 1 1 d U . .
O3 O 0.5114(4) 1.0070(4) 0.1624(3) 0.0311(12) Uani 1 1 d U . .
H3A H 0.5010 1.0572 0.1537 0.037 Uiso 1 1 d R . .
O4 O 0.5328(4) 0.8718(4) 0.1992(3) 0.0301(11) Uani 1 1 d U . .
O1 O 0.4098(5) 0.7797(5) 0.0659(3) 0.0343(12) Uani 1 1 d U . .
O6 O 0.7138(5) 1.0418(4) 0.2970(3) 0.0319(12) Uani 1 1 d U . .
O7 O 0.0347(5) 0.9808(6) 0.1199(4) 0.0555(18) Uani 1 1 d U . .
O5 O 0.2983(4) 0.7385(4) 0.1800(3) 0.0286(11) Uani 1 1 d U . .
O8 O 0.5182(5) 1.1357(5) 0.3086(3) 0.0393(13) Uani 1 1 d U . .
C32 C 0.5578(7) 1.3288(7) 0.1384(5) 0.0406(19) Uani 1 1 d U . .
H32 H 0.5230 1.3563 0.1140 0.049 Uiso 1 1 calc R . .
O2 O 0.7361(5) 1.0271(5) 0.1593(3) 0.0392(13) Uani 1 1 d U . .
C20 C 0.6917(8) 0.8399(8) 0.4887(5) 0.045(2) Uani 1 1 d U . .
H20A H 0.6621 0.7659 0.4971 0.054 Uiso 1 1 calc R . .
H20B H 0.6800 0.8917 0.5263 0.054 Uiso 1 1 calc R . .
C26 C 0.5938(7) 1.3290(7) 0.3159(4) 0.0371(18) Uani 1 1 d U . .
C41 C 0.2736(7) 1.1292(7) 0.0784(4) 0.0353(18) Uani 1 1 d U . .
H41 H 0.2456 1.1813 0.0930 0.042 Uiso 1 1 calc R . .
N1 N 0.2779(5) 0.8850(5) 0.1189(3) 0.0274(13) Uani 1 1 d U . .
C73 C 0.2553(10) 0.7274(10) 0.4795(6) 0.059(3) Uani 1 1 d U . .
H73A H 0.1757 0.6918 0.4615 0.089 Uiso 1 1 calc R . .
H73B H 0.2654 0.7606 0.5278 0.089 Uiso 1 1 calc R . .
H73C H 0.2810 0.6707 0.4696 0.089 Uiso 1 1 calc R . .
C40 C 0.3254(7) 1.1288(7) 0.0218(4) 0.0382(19) Uani 1 1 d U . .
H40 H 0.3335 1.1811 -0.0015 0.046 Uiso 1 1 calc R . .
C50 C 0.1726(6) 0.8263(6) 0.1256(4) 0.0289(16) Uani 1 1 d U . .
H50 H 0.1220 0.8478 0.1103 0.035 Uiso 1 1 calc R . .
N2 N 0.7089(5) 1.2031(5) 0.2452(3) 0.0283(13) Uani 1 1 d U . .
C17 C 0.8624(7) 1.0010(7) 0.4711(4) 0.0369(18) Uani 1 1 d U . .
H17A H 0.9438 1.0323 0.4686 0.044 Uiso 1 1 calc R . .
H17B H 0.8521 1.0539 0.5086 0.044 Uiso 1 1 calc R . .
C6 C 0.9421(7) 1.2016(7) 0.4364(4) 0.0367(18) Uani 1 1 d U . .
H6 H 0.9775 1.1891 0.4701 0.044 Uiso 1 1 calc R . .
C48 C 0.1005(7) 1.0311(7) 0.1815(5) 0.0409(19) Uani 1 1 d U . .
C57 C 0.1881(6) 0.6921(7) 0.1802(4) 0.0290(16) Uani 1 1 d U . .
C59 C 0.1838(7) 0.5365(7) 0.2285(4) 0.0344(17) Uani 1 1 d U . .
C28 C 0.6610(6) 1.2514(6) 0.2107(4) 0.0302(16) Uani 1 1 d U . .
C37 C 0.2986(6) 0.9735(6) 0.0884(4) 0.0280(15) Uani 1 1 d U . .
C43 C 0.2166(7) 1.0652(6) 0.1801(4) 0.0303(16) Uani 1 1 d U . .
C14 C 0.8191(7) 0.9081(7) 0.3486(4) 0.0363(18) Uani 1 1 d U . .
H14A H 0.9002 0.9387 0.3454 0.044 Uiso 1 1 calc R . .
H14B H 0.7801 0.8990 0.3058 0.044 Uiso 1 1 calc R . .
C67 C 0.2714(7) 0.6177(7) 0.2910(4) 0.0352(18) Uani 1 1 d U . .
H67A H 0.3291 0.6843 0.2799 0.042 Uiso 1 1 calc R . .
H67B H 0.2340 0.6444 0.3263 0.042 Uiso 1 1 calc R . .
C27 C 0.6026(6) 1.3088(7) 0.2445(4) 0.0331(17) Uani 1 1 d U . .
C65 C 0.3280(8) 0.5602(7) 0.3169(5) 0.042(2) Uani 1 1 d U . .
H65 H 0.3846 0.6148 0.3569 0.051 Uiso 1 1 calc R . .
C38 C 0.3522(6) 0.9764(7) 0.0329(4) 0.0312(16) Uani 1 1 d U . .
H38 H 0.3807 0.9250 0.0175 0.037 Uiso 1 1 calc R . .
C21 C 0.5525(7) 1.2451(7) 0.3487(4) 0.0358(17) Uani 1 1 d U . .
C1 C 0.7871(6) 1.2711(7) 0.2950(4) 0.0315(16) Uani 1 1 d U . .
H1 H 0.8120 1.3493 0.3031 0.038 Uiso 1 1 calc R . .
C52 C 0.0097(7) 0.6914(7) 0.1566(4) 0.0356(18) Uani 1 1 d U . .
H52 H -0.0298 0.7234 0.1403 0.043 Uiso 1 1 calc R . .
C54 C -0.1702(7) 0.5611(9) 0.1901(6) 0.055(3) Uani 1 1 d U . .
H54A H -0.2014 0.5953 0.1665 0.083 Uiso 1 1 calc R . .
H54B H -0.1782 0.5813 0.2373 0.083 Uiso 1 1 calc R . .
H54C H -0.2107 0.4790 0.1709 0.083 Uiso 1 1 calc R . .
C42 C 0.2615(6) 1.0531(6) 0.1150(4) 0.0292(16) Uani 1 1 d U . .
C29 C 0.6662(7) 1.2356(7) 0.1425(4) 0.0349(17) Uani 1 1 d U . .
H29 H 0.7061 1.1985 0.1209 0.042 Uiso 1 1 calc R . .
C62 C 0.2126(9) 0.3335(7) 0.2194(5) 0.046(2) Uani 1 1 d U . .
H62A H 0.2487 0.2951 0.2356 0.056 Uiso 1 1 calc R . .
H62B H 0.1569 0.2792 0.1797 0.056 Uiso 1 1 calc R . .
C53 C -0.0494(7) 0.6033(7) 0.1832(5) 0.0391(19) Uani 1 1 d U . .
C3 C 0.9321(7) 1.3304(7) 0.3852(4) 0.0349(18) Uani 1 1 d U . .
H3 H 0.9571 1.4051 0.3836 0.042 Uiso 1 1 calc R . .
C16 C 0.8010(7) 0.9912(7) 0.4052(4) 0.0316(16) Uani 1 1 d U . .
C4 C 0.7995(6) 1.1274(7) 0.3408(4) 0.0289(15) Uani 1 1 d U . .
C18 C 0.8189(8) 0.8875(8) 0.4845(5) 0.043(2) Uani 1 1 d U . .
H18 H 0.8598 0.8969 0.5272 0.051 Uiso 1 1 calc R . .
C58 C 0.2435(7) 0.4943(7) 0.1744(4) 0.0359(18) Uani 1 1 d U . .
H58A H 0.3012 0.5589 0.1616 0.043 Uiso 1 1 calc R . .
H58B H 0.1883 0.4410 0.1344 0.043 Uiso 1 1 calc R . .
C56 C 0.1279(7) 0.5966(6) 0.2029(4) 0.0306(16) Uani 1 1 d U . .
C12 C 0.6468(8) 0.7452(8) 0.3674(5) 0.045(2) Uani 1 1 d U . .
H12A H 0.6056 0.7355 0.3253 0.054 Uiso 1 1 calc R . .
H12B H 0.6164 0.6707 0.3752 0.054 Uiso 1 1 calc R . .
C5 C 0.8492(7) 1.1086(7) 0.3942(4) 0.0327(17) Uani 1 1 d U . .
C7 C 0.9865(7) 1.3110(8) 0.4327(4) 0.042(2) Uani 1 1 d U . .
C55 C 0.0135(7) 0.5589(7) 0.2039(4) 0.0377(18) Uani 1 1 d U . .
H55 H -0.0255 0.4963 0.2204 0.045 Uiso 1 1 calc R . .
C30 C 0.6132(8) 1.2740(7) 0.1058(5) 0.042(2) Uani 1 1 d U . .
H30 H 0.6156 1.2623 0.0594 0.051 Uiso 1 1 calc R . .
C60 C 0.0976(7) 0.4340(7) 0.2485(4) 0.0373(18) Uani 1 1 d U . .
H60A H 0.0399 0.3799 0.2096 0.045 Uiso 1 1 calc R . .
H60B H 0.0595 0.4592 0.2840 0.045 Uiso 1 1 calc R . .
C63 C 0.1548(9) 0.3745(8) 0.2735(5) 0.046(2) Uani 1 1 d U . .
H63 H 0.0965 0.3083 0.2855 0.055 Uiso 1 1 calc R . .
C8 C 1.0890(9) 1.4074(8) 0.4817(4) 0.050(2) Uani 1 1 d U . .
H8A H 1.0750 1.4076 0.5274 0.075 Uiso 1 1 calc R . .
H8B H 1.1026 1.4795 0.4757 0.075 Uiso 1 1 calc R . .
H8C H 1.1549 1.3968 0.4733 0.075 Uiso 1 1 calc R . .
C39 C 0.3651(7) 1.0540(8) -0.0009(4) 0.042(2) Uani 1 1 d U . .
H39 H 0.4013 1.0548 -0.0395 0.051 Uiso 1 1 calc R . .
C2 C 0.8403(7) 1.2399(7) 0.3395(4) 0.0324(17) Uani 1 1 d U . .
C45 C 0.2438(9) 1.1282(9) 0.2999(5) 0.054(2) Uani 1 1 d U . .
H45 H 0.2938 1.1620 0.3406 0.064 Uiso 1 1 calc R . .
C51 C 0.1246(7) 0.7351(6) 0.1528(4) 0.0304(16) Uani 1 1 d U . .
C10 C 0.6755(7) 0.9432(7) 0.4112(4) 0.0359(18) Uani 1 1 d U . .
H10A H 0.6337 0.9342 0.3695 0.043 Uiso 1 1 calc R . .
H10B H 0.6642 0.9964 0.4481 0.043 Uiso 1 1 calc R . .
C61 C 0.3001(8) 0.4344(7) 0.2013(5) 0.0402(19) Uani 1 1 d U . .
H61 H 0.3392 0.4085 0.1661 0.048 Uiso 1 1 calc R . .
C22 C 0.5395(8) 1.2695(8) 0.4165(5) 0.047(2) Uani 1 1 d U . .
H22 H 0.5102 1.2113 0.4373 0.056 Uiso 1 1 calc R . .
C11 C 0.6292(7) 0.8266(7) 0.4248(5) 0.0396(19) Uani 1 1 d U . .
H11 H 0.5473 0.7961 0.4282 0.047 Uiso 1 1 calc R . .
C15 C 0.7729(8) 0.7905(7) 0.3614(4) 0.0393(19) Uani 1 1 d U . .
H15 H 0.7839 0.7366 0.3241 0.047 Uiso 1 1 calc R . .
C64 C 0.2395(9) 0.4574(8) 0.3356(5) 0.047(2) Uani 1 1 d U . .
H64A H 0.2764 0.4205 0.3529 0.057 Uiso 1 1 calc R . .
H64B H 0.2005 0.4819 0.3708 0.057 Uiso 1 1 calc R . .
C23 C 0.5708(9) 1.3812(9) 0.4528(5) 0.052(2) Uani 1 1 d U . .
H23 H 0.5630 1.3993 0.4986 0.062 Uiso 1 1 calc R . .
C31 C 0.5508(7) 1.3455(7) 0.2056(5) 0.0379(18) Uani 1 1 d U . .
H31 H 0.5101 1.3826 0.2258 0.046 Uiso 1 1 calc R . .
C33 C 0.4710(9) 1.0473(8) 0.3396(5) 0.048(2) Uani 1 1 d U . .
H33A H 0.4496 0.9746 0.3065 0.071 Uiso 1 1 calc R . .
H33B H 0.4045 1.0463 0.3583 0.071 Uiso 1 1 calc R . .
H33C H 0.5267 1.0607 0.3753 0.071 Uiso 1 1 calc R . .
C24 C 0.6129(9) 1.4650(9) 0.4218(5) 0.051(2) Uani 1 1 d U . .
H24 H 0.6332 1.5403 0.4467 0.062 Uiso 1 1 calc R . .
C47 C 0.0609(9) 1.0497(8) 0.2420(6) 0.053(2) Uani 1 1 d U . .
H47 H -0.0167 1.0275 0.2424 0.064 Uiso 1 1 calc R . .
C44 C 0.2823(8) 1.1072(8) 0.2387(5) 0.0414(19) Uani 1 1 d U . .
H44 H 0.3585 1.1236 0.2388 0.050 Uiso 1 1 calc R . .
C25 C 0.6259(8) 1.4414(8) 0.3557(5) 0.047(2) Uani 1 1 d U . .
H25 H 0.6568 1.5010 0.3360 0.056 Uiso 1 1 calc R . .
C46 C 0.1305(10) 1.0984(9) 0.2999(5) 0.054(2) Uani 1 1 d U . .
H46 H 0.1026 1.1126 0.3407 0.065 Uiso 1 1 calc R . .
C19 C 0.8334(8) 0.8044(8) 0.4276(5) 0.043(2) Uani 1 1 d U . .
H19A H 0.8026 0.7304 0.4363 0.052 Uiso 1 1 calc R . .
H19B H 0.9143 0.8315 0.4248 0.052 Uiso 1 1 calc R . .
C34 C 0.5504(8) 0.7826(7) 0.2065(5) 0.0399(19) Uani 1 1 d U . .
H34A H 0.4778 0.7192 0.2088 0.048 Uiso 1 1 calc R . .
H34B H 0.6005 0.8087 0.2488 0.048 Uiso 1 1 calc R . .
C66 C 0.3864(8) 0.5185(8) 0.2625(5) 0.044(2) Uani 1 1 d U . .
H66A H 0.4445 0.5832 0.2501 0.053 Uiso 1 1 calc R . .
H66B H 0.4237 0.4818 0.2796 0.053 Uiso 1 1 calc R . .
C49 C -0.0864(10) 0.9278(15) 0.1203(9) 0.105(5) Uani 1 1 d U . .
H49A H -0.1252 0.8945 0.0744 0.157 Uiso 1 1 calc R . .
H49B H -0.1071 0.9846 0.1445 0.157 Uiso 1 1 calc R . .
H49C H -0.1083 0.8687 0.1422 0.157 Uiso 1 1 calc R . .
C72 C 0.3180(11) 0.8122(10) 0.4503(6) 0.063(3) Uani 1 1 d U . .
N3 N 0.3656(12) 0.8838(10) 0.4293(7) 0.101(4) Uani 1 1 d U . .
C71 C 0.0590(12) 0.7411(13) 0.3546(6) 0.070(3) Uani 1 1 d U . .
N4 N 0.0115(12) 0.6614(13) 0.3720(6) 0.093(4) Uani 1 1 d U . .
C35 C 0.6042(12) 0.7407(11) 0.1471(8) 0.076(3) Uani 1 1 d U . .
H35A H 0.5573 0.7216 0.1049 0.091 Uiso 1 1 calc R . .
H35B H 0.6793 0.8029 0.1474 0.091 Uiso 1 1 calc R . .
C70 C 0.1120(15) 0.8332(12) 0.3320(7) 0.088(4) Uani 1 1 d U . .
H70A H 0.0772 0.8153 0.2866 0.132 Uiso 1 1 calc R . .
H70B H 0.1915 0.8537 0.3322 0.132 Uiso 1 1 calc R . .
H70C H 0.1051 0.8965 0.3612 0.132 Uiso 1 1 calc R . .
C36 C 0.6156(17) 0.6415(15) 0.1492(10) 0.116(6) Uani 1 1 d U . .
H36A H 0.6165 0.5996 0.1040 0.174 Uiso 1 1 calc R . .
H36B H 0.5522 0.5926 0.1677 0.174 Uiso 1 1 calc R . .
H36C H 0.6859 0.6664 0.1773 0.174 Uiso 1 1 calc R . .
C69 C 0.0705(17) 0.7635(18) -0.0477(9) 0.112(5) Uani 1 1 d U . .
N5 N 0.0892(18) 0.6852(15) -0.0439(9) 0.147(7) Uani 1 1 d U . .
C68 C 0.0528(16) 0.8496(16) -0.0510(10) 0.118(6) Uani 1 1 d U . .
H68A H 0.0454 0.8488 -0.0975 0.177 Uiso 1 1 calc R . .
H68B H 0.1164 0.9211 -0.0250 0.177 Uiso 1 1 calc R . .
H68C H -0.0161 0.8415 -0.0328 0.177 Uiso 1 1 calc R . .
C9 C 0.174(2) 0.5105(17) 0.0059(10) 0.144(8) Uani 1 1 d U . .
H9A H 0.1976 0.5415 -0.0314 0.215 Uiso 1 1 calc R . .
H9B H 0.2156 0.5694 0.0478 0.215 Uiso 1 1 calc R . .
H9C H 0.0936 0.4834 0.0060 0.215 Uiso 1 1 calc R . .
C13 C 0.197(2) 0.424(2) -0.0005(12) 0.142(7) Uani 1 1 d U . .
N6 N 0.192(2) 0.334(2) -0.0051(10) 0.181(8) Uani 1 1 d U . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
V1 O1 1.600(6) . ?
V1 O5 1.936(5) . ?
V1 O3 1.964(5) . ?
V1 O4 1.996(5) . ?
V1 N1 2.077(6) . ?
V2 O2 1.599(6) . ?
V2 O6 1.947(5) . ?
V2 O3 1.974(5) . ?
V2 O4 1.986(6) . ?
V2 N2 2.086(7) . ?
O3 H3A 0.8399 . ?
O4 C34 1.419(9) . ?
O6 C4 1.330(9) . ?
O7 C48 1.381(12) . ?
O7 C49 1.460(13) . ?
O5 C57 1.329(9) . ?
O8 C21 1.392(10) . ?
O8 C33 1.438(10) . ?
C32 C30 1.369(13) . ?
C32 C31 1.381(13) . ?
C32 H32 0.9500 . ?
C20 C11 1.508(13) . ?
C20 C18 1.549(13) . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C26 C21 1.411(12) . ?
C26 C25 1.429(12) . ?
C26 C27 1.470(12) . ?
C41 C40 1.385(12) . ?
C41 C42 1.424(11) . ?
C41 H41 0.9500 . ?
N1 C50 1.310(10) . ?
N1 C37 1.456(9) . ?
C73 C72 1.403(16) . ?
C73 H73A 0.9800 . ?
C73 H73B 0.9800 . ?
C73 H73C 0.9800 . ?
C40 C39 1.367(13) . ?
C40 H40 0.9500 . ?
C50 C51 1.415(11) . ?
C50 H50 0.9500 . ?
N2 C1 1.291(10) . ?
N2 C28 1.436(10) . ?
C17 C18 1.525(12) . ?
C17 C16 1.556(10) . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C6 C7 1.389(12) . ?
C6 C5 1.396(12) . ?
C6 H6 0.9500 . ?
C48 C47 1.391(14) . ?
C48 C43 1.423(11) . ?
C57 C56 1.420(11) . ?
C57 C51 1.443(10) . ?
C59 C60 1.543(11) . ?
C59 C56 1.545(11) . ?
C59 C58 1.546(11) . ?
C59 C67 1.548(12) . ?
C28 C29 1.399(12) . ?
C28 C27 1.436(11) . ?
C37 C38 1.378(11) . ?
C37 C42 1.411(11) . ?
C43 C44 1.337(12) . ?
C43 C42 1.502(11) . ?
C14 C16 1.538(11) . ?
C14 C15 1.568(12) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C67 C65 1.524(11) . ?
C67 H67A 0.9900 . ?
C67 H67B 0.9900 . ?
C27 C31 1.405(12) . ?
C65 C66 1.534(13) . ?
C65 C64 1.544(13) . ?
C65 H65 1.0000 . ?
C38 C39 1.394(12) . ?
C38 H38 0.9500 . ?
C21 C22 1.408(13) . ?
C1 C2 1.443(11) . ?
C1 H1 0.9500 . ?
C52 C53 1.391(12) . ?
C52 C51 1.400(11) . ?
C52 H52 0.9500 . ?
C54 C53 1.487(12) . ?
C54 H54A 0.9800 . ?
C54 H54B 0.9800 . ?
C54 H54C 0.9800 . ?
C29 C30 1.403(12) . ?
C29 H29 0.9500 . ?
C62 C61 1.514(13) . ?
C62 C63 1.521(13) . ?
C62 H62A 0.9900 . ?
C62 H62B 0.9900 . ?
C53 C55 1.386(12) . ?
C3 C7 1.390(12) . ?
C3 C2 1.408(11) . ?
C3 H3 0.9500 . ?
C16 C10 1.535(11) . ?
C16 C5 1.548(11) . ?
C4 C2 1.416(11) . ?
C4 C5 1.447(11) . ?
C18 C19 1.516(13) . ?
C18 H18 1.0000 . ?
C58 C61 1.563(11) . ?
C58 H58A 0.9900 . ?
C58 H58B 0.9900 . ?
C56 C55 1.392(11) . ?
C12 C11 1.530(13) . ?
C12 C15 1.545(13) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C7 C8 1.534(12) . ?
C55 H55 0.9500 . ?
C30 H30 0.9500 . ?
C60 C63 1.545(12) . ?
C60 H60A 0.9900 . ?
C60 H60B 0.9900 . ?
C63 C64 1.531(14) . ?
C63 H63 1.0000 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C39 H39 0.9500 . ?
C45 C46 1.393(15) . ?
C45 C44 1.402(13) . ?
C45 H45 0.9500 . ?
C10 C11 1.562(12) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C61 C66 1.530(13) . ?
C61 H61 1.0000 . ?
C22 C23 1.402(14) . ?
C22 H22 0.9500 . ?
C11 H11 1.0000 . ?
C15 C19 1.533(12) . ?
C15 H15 1.0000 . ?
C64 H64A 0.9900 . ?
C64 H64B 0.9900 . ?
C23 C24 1.384(15) . ?
C23 H23 0.9500 . ?
C31 H31 0.9500 . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C24 C25 1.375(14) . ?
C24 H24 0.9500 . ?
C47 C46 1.343(16) . ?
C47 H47 0.9500 . ?
C44 H44 0.9500 . ?
C25 H25 0.9500 . ?
C46 H46 0.9500 . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C34 C35 1.565(15) . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
C66 H66A 0.9900 . ?
C66 H66B 0.9900 . ?
C49 H49A 0.9800 . ?
C49 H49B 0.9800 . ?
C49 H49C 0.9800 . ?
C72 N3 1.121(16) . ?
C71 N4 1.161(18) . ?
C71 C70 1.37(2) . ?
C35 C36 1.476(18) . ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
C70 H70A 0.9800 . ?
C70 H70B 0.9800 . ?
C70 H70C 0.9800 . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C69 N5 1.25(3) . ?
C69 C68 1.35(3) . ?
C68 H68A 0.9800 . ?
C68 H68B 0.9800 . ?
C68 H68C 0.9800 . ?
C9 C13 1.36(3) . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C13 N6 1.20(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 V1 O5 109.1(3) . . ?
O1 V1 O3 111.3(3) . . ?
O5 V1 O3 139.3(2) . . ?
O1 V1 O4 106.8(3) . . ?
O5 V1 O4 91.2(2) . . ?
O3 V1 O4 72.7(2) . . ?
O1 V1 N1 101.3(3) . . ?
O5 V1 N1 88.3(2) . . ?
O3 V1 N1 88.6(2) . . ?
O4 V1 N1 150.4(2) . . ?
O2 V2 O6 108.1(3) . . ?
O2 V2 O3 109.6(3) . . ?
O6 V2 O3 142.1(2) . . ?
O2 V2 O4 108.4(3) . . ?
O6 V2 O4 91.6(2) . . ?
O3 V2 O4 72.7(2) . . ?
O2 V2 N2 99.1(3) . . ?
O6 V2 N2 86.8(2) . . ?
O3 V2 N2 91.3(2) . . ?
O4 V2 N2 151.5(2) . . ?
V1 O3 V2 107.5(2) . . ?
V1 O3 H3A 126.2 . . ?
V2 O3 H3A 126.3 . . ?
C34 O4 V2 126.7(5) . . ?
C34 O4 V1 122.6(5) . . ?
V2 O4 V1 105.8(2) . . ?
C4 O6 V2 131.1(5) . . ?
C48 O7 C49 115.9(9) . . ?
C57 O5 V1 134.3(5) . . ?
C21 O8 C33 117.1(7) . . ?
C30 C32 C31 122.3(8) . . ?
C30 C32 H32 118.8 . . ?
C31 C32 H32 118.8 . . ?
C11 C20 C18 110.6(7) . . ?
C11 C20 H20A 109.5 . . ?
C18 C20 H20A 109.5 . . ?
C11 C20 H20B 109.5 . . ?
C18 C20 H20B 109.5 . . ?
H20A C20 H20B 108.1 . . ?
C21 C26 C25 116.5(8) . . ?
C21 C26 C27 125.2(8) . . ?
C25 C26 C27 118.2(8) . . ?
C40 C41 C42 121.1(8) . . ?
C40 C41 H41 119.5 . . ?
C42 C41 H41 119.5 . . ?
C50 N1 C37 114.2(6) . . ?
C50 N1 V1 123.8(5) . . ?
C37 N1 V1 121.6(5) . . ?
C72 C73 H73A 109.5 . . ?
C72 C73 H73B 109.5 . . ?
H73A C73 H73B 109.5 . . ?
C72 C73 H73C 109.5 . . ?
H73A C73 H73C 109.5 . . ?
H73B C73 H73C 109.5 . . ?
C39 C40 C41 120.8(8) . . ?
C39 C40 H40 119.6 . . ?
C41 C40 H40 119.6 . . ?
N1 C50 C51 128.4(7) . . ?
N1 C50 H50 115.8 . . ?
C51 C50 H50 115.8 . . ?
C1 N2 C28 117.2(7) . . ?
C1 N2 V2 125.0(5) . . ?
C28 N2 V2 117.8(5) . . ?
C18 C17 C16 112.1(7) . . ?
C18 C17 H17A 109.2 . . ?
C16 C17 H17A 109.2 . . ?
C18 C17 H17B 109.2 . . ?
C16 C17 H17B 109.2 . . ?
H17A C17 H17B 107.9 . . ?
C7 C6 C5 124.7(8) . . ?
C7 C6 H6 117.7 . . ?
C5 C6 H6 117.7 . . ?
O7 C48 C47 124.8(8) . . ?
O7 C48 C43 115.1(7) . . ?
C47 C48 C43 120.1(9) . . ?
O5 C57 C56 122.5(7) . . ?
O5 C57 C51 119.6(7) . . ?
C56 C57 C51 117.8(7) . . ?
C60 C59 C56 111.9(7) . . ?
C60 C59 C58 107.9(6) . . ?
C56 C59 C58 110.7(7) . . ?
C60 C59 C67 107.1(7) . . ?
C56 C59 C67 110.5(6) . . ?
C58 C59 C67 108.6(7) . . ?
C29 C28 C27 120.6(7) . . ?
C29 C28 N2 118.7(7) . . ?
C27 C28 N2 120.6(7) . . ?
C38 C37 C42 121.0(7) . . ?
C38 C37 N1 119.1(7) . . ?
C42 C37 N1 119.8(7) . . ?
C44 C43 C48 117.2(8) . . ?
C44 C43 C42 122.3(7) . . ?
C48 C43 C42 120.5(7) . . ?
C16 C14 C15 110.7(7) . . ?
C16 C14 H14A 109.5 . . ?
C15 C14 H14A 109.5 . . ?
C16 C14 H14B 109.5 . . ?
C15 C14 H14B 109.5 . . ?
H14A C14 H14B 108.1 . . ?
C65 C67 C59 111.4(7) . . ?
C65 C67 H67A 109.4 . . ?
C59 C67 H67A 109.4 . . ?
C65 C67 H67B 109.4 . . ?
C59 C67 H67B 109.4 . . ?
H67A C67 H67B 108.0 . . ?
C31 C27 C28 116.6(8) . . ?
C31 C27 C26 119.6(7) . . ?
C28 C27 C26 123.7(7) . . ?
C67 C65 C66 109.8(7) . . ?
C67 C65 C64 110.0(8) . . ?
C66 C65 C64 108.2(7) . . ?
C67 C65 H65 109.6 . . ?
C66 C65 H65 109.6 . . ?
C64 C65 H65 109.6 . . ?
C37 C38 C39 120.7(8) . . ?
C37 C38 H38 119.6 . . ?
C39 C38 H38 119.6 . . ?
O8 C21 C22 122.2(8) . . ?
O8 C21 C26 115.5(7) . . ?
C22 C21 C26 122.1(8) . . ?
N2 C1 C2 126.4(7) . . ?
N2 C1 H1 116.8 . . ?
C2 C1 H1 116.8 . . ?
C53 C52 C51 123.0(7) . . ?
C53 C52 H52 118.5 . . ?
C51 C52 H52 118.5 . . ?
C53 C54 H54A 109.5 . . ?
C53 C54 H54B 109.5 . . ?
H54A C54 H54B 109.5 . . ?
C53 C54 H54C 109.5 . . ?
H54A C54 H54C 109.5 . . ?
H54B C54 H54C 109.5 . . ?
C37 C42 C41 116.6(7) . . ?
C37 C42 C43 124.1(7) . . ?
C41 C42 C43 119.2(7) . . ?
C28 C29 C30 120.6(8) . . ?
C28 C29 H29 119.7 . . ?
C30 C29 H29 119.7 . . ?
C61 C62 C63 108.4(7) . . ?
C61 C62 H62A 110.0 . . ?
C63 C62 H62A 110.0 . . ?
C61 C62 H62B 110.0 . . ?
C63 C62 H62B 110.0 . . ?
H62A C62 H62B 108.4 . . ?
C55 C53 C52 114.9(8) . . ?
C55 C53 C54 122.5(8) . . ?
C52 C53 C54 122.6(8) . . ?
C7 C3 C2 120.4(8) . . ?
C7 C3 H3 119.8 . . ?
C2 C3 H3 119.8 . . ?
C10 C16 C14 109.8(7) . . ?
C10 C16 C5 111.2(6) . . ?
C14 C16 C5 111.2(7) . . ?
C10 C16 C17 107.5(7) . . ?
C14 C16 C17 107.3(7) . . ?
C5 C16 C17 109.7(6) . . ?
O6 C4 C2 121.5(7) . . ?
O6 C4 C5 120.5(7) . . ?
C2 C4 C5 117.9(7) . . ?
C19 C18 C17 110.4(8) . . ?
C19 C18 C20 107.8(8) . . ?
C17 C18 C20 108.5(7) . . ?
C19 C18 H18 110.0 . . ?
C17 C18 H18 110.0 . . ?
C20 C18 H18 110.0 . . ?
C59 C58 C61 110.0(7) . . ?
C59 C58 H58A 109.7 . . ?
C61 C58 H58A 109.7 . . ?
C59 C58 H58B 109.7 . . ?
C61 C58 H58B 109.7 . . ?
H58A C58 H58B 108.2 . . ?
C55 C56 C57 117.4(7) . . ?
C55 C56 C59 119.2(7) . . ?
C57 C56 C59 123.3(7) . . ?
C11 C12 C15 110.6(7) . . ?
C11 C12 H12A 109.5 . . ?
C15 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
C15 C12 H12B 109.5 . . ?
H12A C12 H12B 108.1 . . ?
C6 C5 C4 117.2(7) . . ?
C6 C5 C16 120.9(7) . . ?
C4 C5 C16 121.9(7) . . ?
C6 C7 C3 117.8(8) . . ?
C6 C7 C8 120.6(8) . . ?
C3 C7 C8 121.6(8) . . ?
C53 C55 C56 126.6(8) . . ?
C53 C55 H55 116.7 . . ?
C56 C55 H55 116.7 . . ?
C32 C30 C29 118.5(9) . . ?
C32 C30 H30 120.8 . . ?
C29 C30 H30 120.8 . . ?
C59 C60 C63 111.2(7) . . ?
C59 C60 H60A 109.4 . . ?
C63 C60 H60A 109.4 . . ?
C59 C60 H60B 109.4 . . ?
C63 C60 H60B 109.4 . . ?
H60A C60 H60B 108.0 . . ?
C62 C63 C64 110.8(8) . . ?
C62 C63 C60 110.4(7) . . ?
C64 C63 C60 108.7(7) . . ?
C62 C63 H63 109.0 . . ?
C64 C63 H63 109.0 . . ?
C60 C63 H63 109.0 . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C40 C39 C38 119.6(8) . . ?
C40 C39 H39 120.2 . . ?
C38 C39 H39 120.2 . . ?
C3 C2 C4 121.6(7) . . ?
C3 C2 C1 115.3(7) . . ?
C4 C2 C1 123.0(7) . . ?
C46 C45 C44 118.5(10) . . ?
C46 C45 H45 120.8 . . ?
C44 C45 H45 120.8 . . ?
C52 C51 C50 116.0(7) . . ?
C52 C51 C57 119.8(7) . . ?
C50 C51 C57 124.0(7) . . ?
C16 C10 C11 110.6(7) . . ?
C16 C10 H10A 109.5 . . ?
C11 C10 H10A 109.5 . . ?
C16 C10 H10B 109.5 . . ?
C11 C10 H10B 109.5 . . ?
H10A C10 H10B 108.1 . . ?
C62 C61 C66 110.1(8) . . ?
C62 C61 C58 110.3(8) . . ?
C66 C61 C58 109.0(7) . . ?
C62 C61 H61 109.1 . . ?
C66 C61 H61 109.1 . . ?
C58 C61 H61 109.1 . . ?
C23 C22 C21 118.9(9) . . ?
C23 C22 H22 120.6 . . ?
C21 C22 H22 120.6 . . ?
C20 C11 C12 108.9(7) . . ?
C20 C11 C10 109.8(7) . . ?
C12 C11 C10 109.0(7) . . ?
C20 C11 H11 109.7 . . ?
C12 C11 H11 109.7 . . ?
C10 C11 H11 109.7 . . ?
C19 C15 C12 107.8(7) . . ?
C19 C15 C14 109.6(7) . . ?
C12 C15 C14 108.7(7) . . ?
C19 C15 H15 110.2 . . ?
C12 C15 H15 110.2 . . ?
C14 C15 H15 110.2 . . ?
C63 C64 C65 108.6(7) . . ?
C63 C64 H64A 110.0 . . ?
C65 C64 H64A 110.0 . . ?
C63 C64 H64B 110.0 . . ?
C65 C64 H64B 110.0 . . ?
H64A C64 H64B 108.3 . . ?
C24 C23 C22 120.0(9) . . ?
C24 C23 H23 120.0 . . ?
C22 C23 H23 120.0 . . ?
C32 C31 C27 121.4(8) . . ?
C32 C31 H31 119.3 . . ?
C27 C31 H31 119.3 . . ?
O8 C33 H33A 109.5 . . ?
O8 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
O8 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C25 C24 C23 121.3(9) . . ?
C25 C24 H24 119.4 . . ?
C23 C24 H24 119.4 . . ?
C46 C47 C48 121.0(10) . . ?
C46 C47 H47 119.5 . . ?
C48 C47 H47 119.5 . . ?
C43 C44 C45 123.0(9) . . ?
C43 C44 H44 118.5 . . ?
C45 C44 H44 118.5 . . ?
C24 C25 C26 121.2(9) . . ?
C24 C25 H25 119.4 . . ?
C26 C25 H25 119.4 . . ?
C47 C46 C45 119.9(9) . . ?
C47 C46 H46 120.0 . . ?
C45 C46 H46 120.0 . . ?
C18 C19 C15 110.8(7) . . ?
C18 C19 H19A 109.5 . . ?
C15 C19 H19A 109.5 . . ?
C18 C19 H19B 109.5 . . ?
C15 C19 H19B 109.5 . . ?
H19A C19 H19B 108.1 . . ?
O4 C34 C35 111.3(8) . . ?
O4 C34 H34A 109.4 . . ?
C35 C34 H34A 109.4 . . ?
O4 C34 H34B 109.4 . . ?
C35 C34 H34B 109.4 . . ?
H34A C34 H34B 108.0 . . ?
C61 C66 C65 109.9(8) . . ?
C61 C66 H66A 109.7 . . ?
C65 C66 H66A 109.7 . . ?
C61 C66 H66B 109.7 . . ?
C65 C66 H66B 109.7 . . ?
H66A C66 H66B 108.2 . . ?
O7 C49 H49A 109.5 . . ?
O7 C49 H49B 109.5 . . ?
H49A C49 H49B 109.5 . . ?
O7 C49 H49C 109.5 . . ?
H49A C49 H49C 109.5 . . ?
H49B C49 H49C 109.5 . . ?
N3 C72 C73 175.8(14) . . ?
N4 C71 C70 177.8(16) . . ?
C36 C35 C34 113.7(11) . . ?
C36 C35 H35A 108.8 . . ?
C34 C35 H35A 108.8 . . ?
C36 C35 H35B 108.8 . . ?
C34 C35 H35B 108.8 . . ?
H35A C35 H35B 107.7 . . ?
C71 C70 H70A 109.5 . . ?
C71 C70 H70B 109.5 . . ?
H70A C70 H70B 109.5 . . ?
C71 C70 H70C 109.5 . . ?
H70A C70 H70C 109.5 . . ?
H70B C70 H70C 109.5 . . ?
C35 C36 H36A 109.5 . . ?
C35 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C35 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
N5 C69 C68 179(2) . . ?
C69 C68 H68A 109.5 . . ?
C69 C68 H68B 109.5 . . ?
H68A C68 H68B 109.5 . . ?
C69 C68 H68C 109.5 . . ?
H68A C68 H68C 109.5 . . ?
H68B C68 H68C 109.5 . . ?
C13 C9 H9A 109.5 . . ?
C13 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C13 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
N6 C13 C9 165(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 O3 V2 -93.2(3) . . . . ?
O5 V1 O3 V2 79.5(4) . . . . ?
O4 V1 O3 V2 8.6(2) . . . . ?
N1 V1 O3 V2 165.2(3) . . . . ?
O2 V2 O3 V1 95.2(3) . . . . ?
O6 V2 O3 V1 -78.0(4) . . . . ?
O4 V2 O3 V1 -8.6(2) . . . . ?
N2 V2 O3 V1 -164.6(3) . . . . ?
O2 V2 O4 C34 58.3(7) . . . . ?
O6 V2 O4 C34 -51.3(6) . . . . ?
O3 V2 O4 C34 163.9(7) . . . . ?
N2 V2 O4 C34 -137.6(7) . . . . ?
O2 V2 O4 V1 -97.1(3) . . . . ?
O6 V2 O4 V1 153.3(3) . . . . ?
O3 V2 O4 V1 8.4(2) . . . . ?
N2 V2 O4 V1 67.0(6) . . . . ?
O1 V1 O4 C34 -57.5(6) . . . . ?
O5 V1 O4 C34 52.9(6) . . . . ?
O3 V1 O4 C34 -165.2(6) . . . . ?
N1 V1 O4 C34 141.5(6) . . . . ?
O1 V1 O4 V2 99.2(3) . . . . ?
O5 V1 O4 V2 -150.4(3) . . . . ?
O3 V1 O4 V2 -8.5(2) . . . . ?
N1 V1 O4 V2 -61.7(5) . . . . ?
O2 V2 O6 C4 71.4(7) . . . . ?
O3 V2 O6 C4 -115.3(6) . . . . ?
O4 V2 O6 C4 -178.7(6) . . . . ?
N2 V2 O6 C4 -27.2(6) . . . . ?
O1 V1 O5 C57 -87.4(7) . . . . ?
O3 V1 O5 C57 99.9(7) . . . . ?
O4 V1 O5 C57 164.3(7) . . . . ?
N1 V1 O5 C57 14.0(7) . . . . ?
O1 V1 N1 C50 98.0(6) . . . . ?
O5 V1 N1 C50 -11.1(6) . . . . ?
O3 V1 N1 C50 -150.5(6) . . . . ?
O4 V1 N1 C50 -100.6(7) . . . . ?
O1 V1 N1 C37 -74.5(6) . . . . ?
O5 V1 N1 C37 176.3(6) . . . . ?
O3 V1 N1 C37 36.9(6) . . . . ?
O4 V1 N1 C37 86.9(7) . . . . ?
C42 C41 C40 C39 0.9(13) . . . . ?
C37 N1 C50 C51 179.8(8) . . . . ?
V1 N1 C50 C51 6.7(12) . . . . ?
O2 V2 N2 C1 -88.2(6) . . . . ?
O6 V2 N2 C1 19.6(6) . . . . ?
O3 V2 N2 C1 161.7(6) . . . . ?
O4 V2 N2 C1 107.1(7) . . . . ?
O2 V2 N2 C28 90.7(6) . . . . ?
O6 V2 N2 C28 -161.6(5) . . . . ?
O3 V2 N2 C28 -19.5(5) . . . . ?
O4 V2 N2 C28 -74.1(7) . . . . ?
C49 O7 C48 C47 -10.5(15) . . . . ?
C49 O7 C48 C43 169.7(10) . . . . ?
V1 O5 C57 C56 165.9(6) . . . . ?
V1 O5 C57 C51 -10.4(11) . . . . ?
C1 N2 C28 C29 121.6(8) . . . . ?
V2 N2 C28 C29 -57.3(8) . . . . ?
C1 N2 C28 C27 -62.3(10) . . . . ?
V2 N2 C28 C27 118.8(7) . . . . ?
C50 N1 C37 C38 -125.5(8) . . . . ?
V1 N1 C37 C38 47.8(9) . . . . ?
C50 N1 C37 C42 53.0(9) . . . . ?
V1 N1 C37 C42 -133.8(6) . . . . ?
O7 C48 C43 C44 -175.5(7) . . . . ?
C47 C48 C43 C44 4.7(12) . . . . ?
O7 C48 C43 C42 4.1(11) . . . . ?
C47 C48 C43 C42 -175.7(7) . . . . ?
C60 C59 C67 C65 58.1(9) . . . . ?
C56 C59 C67 C65 -179.7(7) . . . . ?
C58 C59 C67 C65 -58.1(9) . . . . ?
C29 C28 C27 C31 1.0(11) . . . . ?
N2 C28 C27 C31 -175.1(7) . . . . ?
C29 C28 C27 C26 -179.8(8) . . . . ?
N2 C28 C27 C26 4.2(12) . . . . ?
C21 C26 C27 C31 124.6(9) . . . . ?
C25 C26 C27 C31 -53.2(11) . . . . ?
C21 C26 C27 C28 -54.7(12) . . . . ?
C25 C26 C27 C28 127.5(9) . . . . ?
C59 C67 C65 C66 59.0(10) . . . . ?
C59 C67 C65 C64 -60.0(9) . . . . ?
C42 C37 C38 C39 -3.9(11) . . . . ?
N1 C37 C38 C39 174.5(7) . . . . ?
C33 O8 C21 C22 -1.6(12) . . . . ?
C33 O8 C21 C26 -177.3(8) . . . . ?
C25 C26 C21 O8 177.9(7) . . . . ?
C27 C26 C21 O8 0.1(12) . . . . ?
C25 C26 C21 C22 2.1(13) . . . . ?
C27 C26 C21 C22 -175.7(8) . . . . ?
C28 N2 C1 C2 174.9(7) . . . . ?
V2 N2 C1 C2 -6.3(11) . . . . ?
C38 C37 C42 C41 5.2(11) . . . . ?
N1 C37 C42 C41 -173.2(7) . . . . ?
C38 C37 C42 C43 -171.5(7) . . . . ?
N1 C37 C42 C43 10.1(11) . . . . ?
C40 C41 C42 C37 -3.7(11) . . . . ?
C40 C41 C42 C43 173.1(7) . . . . ?
C44 C43 C42 C37 70.7(11) . . . . ?
C48 C43 C42 C37 -108.9(9) . . . . ?
C44 C43 C42 C41 -105.9(9) . . . . ?
C48 C43 C42 C41 74.5(10) . . . . ?
C27 C28 C29 C30 -0.9(12) . . . . ?
N2 C28 C29 C30 175.2(7) . . . . ?
C51 C52 C53 C55 -2.1(13) . . . . ?
C51 C52 C53 C54 177.0(9) . . . . ?
C15 C14 C16 C10 -58.1(8) . . . . ?
C15 C14 C16 C5 178.4(6) . . . . ?
C15 C14 C16 C17 58.4(8) . . . . ?
C18 C17 C16 C10 59.3(9) . . . . ?
C18 C17 C16 C14 -58.7(9) . . . . ?
C18 C17 C16 C5 -179.7(7) . . . . ?
V2 O6 C4 C2 19.6(11) . . . . ?
V2 O6 C4 C5 -164.6(5) . . . . ?
C16 C17 C18 C19 58.7(9) . . . . ?
C16 C17 C18 C20 -59.3(10) . . . . ?
C11 C20 C18 C19 -60.7(9) . . . . ?
C11 C20 C18 C17 58.9(10) . . . . ?
C60 C59 C58 C61 -57.5(9) . . . . ?
C56 C59 C58 C61 179.7(7) . . . . ?
C67 C59 C58 C61 58.1(8) . . . . ?
O5 C57 C56 C55 176.8(7) . . . . ?
C51 C57 C56 C55 -6.8(11) . . . . ?
O5 C57 C56 C59 -1.0(12) . . . . ?
C51 C57 C56 C59 175.4(7) . . . . ?
C60 C59 C56 C55 3.5(11) . . . . ?
C58 C59 C56 C55 123.9(8) . . . . ?
C67 C59 C56 C55 -115.8(8) . . . . ?
C60 C59 C56 C57 -178.8(7) . . . . ?
C58 C59 C56 C57 -58.4(10) . . . . ?
C67 C59 C56 C57 62.0(10) . . . . ?
C7 C6 C5 C4 3.3(13) . . . . ?
C7 C6 C5 C16 -175.9(8) . . . . ?
O6 C4 C5 C6 177.2(7) . . . . ?
C2 C4 C5 C6 -6.9(11) . . . . ?
O6 C4 C5 C16 -3.7(11) . . . . ?
C2 C4 C5 C16 172.2(7) . . . . ?
C10 C16 C5 C6 125.0(8) . . . . ?
C14 C16 C5 C6 -112.3(9) . . . . ?
C17 C16 C5 C6 6.2(11) . . . . ?
C10 C16 C5 C4 -54.1(10) . . . . ?
C14 C16 C5 C4 68.6(9) . . . . ?
C17 C16 C5 C4 -172.9(7) . . . . ?
C5 C6 C7 C3 2.6(14) . . . . ?
C5 C6 C7 C8 179.9(9) . . . . ?
C2 C3 C7 C6 -4.6(13) . . . . ?
C2 C3 C7 C8 178.1(8) . . . . ?
C52 C53 C55 C56 2.8(14) . . . . ?
C54 C53 C55 C56 -176.2(9) . . . . ?
C57 C56 C55 C53 1.7(13) . . . . ?
C59 C56 C55 C53 179.6(8) . . . . ?
C31 C32 C30 C29 -1.2(13) . . . . ?
C28 C29 C30 C32 1.0(12) . . . . ?
C56 C59 C60 C63 179.6(7) . . . . ?
C58 C59 C60 C63 57.6(9) . . . . ?
C67 C59 C60 C63 -59.1(9) . . . . ?
C61 C62 C63 C64 -60.5(9) . . . . ?
C61 C62 C63 C60 60.0(10) . . . . ?
C59 C60 C63 C62 -59.8(10) . . . . ?
C59 C60 C63 C64 61.9(9) . . . . ?
C41 C40 C39 C38 0.7(13) . . . . ?
C37 C38 C39 C40 0.8(12) . . . . ?
C7 C3 C2 C4 0.8(13) . . . . ?
C7 C3 C2 C1 176.8(8) . . . . ?
O6 C4 C2 C3 -179.0(7) . . . . ?
C5 C4 C2 C3 5.1(12) . . . . ?
O6 C4 C2 C1 5.3(12) . . . . ?
C5 C4 C2 C1 -170.6(7) . . . . ?
N2 C1 C2 C3 173.0(8) . . . . ?
N2 C1 C2 C4 -11.0(13) . . . . ?
C53 C52 C51 C50 -178.8(8) . . . . ?
C53 C52 C51 C57 -3.0(13) . . . . ?
N1 C50 C51 C52 177.0(8) . . . . ?
N1 C50 C51 C57 1.5(13) . . . . ?
O5 C57 C51 C52 -176.0(7) . . . . ?
C56 C57 C51 C52 7.6(11) . . . . ?
O5 C57 C51 C50 -0.6(12) . . . . ?
C56 C57 C51 C50 -177.1(7) . . . . ?
C14 C16 C10 C11 58.5(9) . . . . ?
C5 C16 C10 C11 -178.0(7) . . . . ?
C17 C16 C10 C11 -57.9(9) . . . . ?
C63 C62 C61 C66 59.7(10) . . . . ?
C63 C62 C61 C58 -60.7(10) . . . . ?
C59 C58 C61 C62 60.9(9) . . . . ?
C59 C58 C61 C66 -60.2(9) . . . . ?
O8 C21 C22 C23 -176.7(8) . . . . ?
C26 C21 C22 C23 -1.2(14) . . . . ?
C18 C20 C11 C12 60.0(10) . . . . ?
C18 C20 C11 C10 -59.2(10) . . . . ?
C15 C12 C11 C20 -59.6(9) . . . . ?
C15 C12 C11 C10 60.2(9) . . . . ?
C16 C10 C11 C20 59.8(9) . . . . ?
C16 C10 C11 C12 -59.4(9) . . . . ?
C11 C12 C15 C19 59.1(9) . . . . ?
C11 C12 C15 C14 -59.6(9) . . . . ?
C16 C14 C15 C19 -59.3(9) . . . . ?
C16 C14 C15 C12 58.2(9) . . . . ?
C62 C63 C64 C65 61.1(9) . . . . ?
C60 C63 C64 C65 -60.5(10) . . . . ?
C67 C65 C64 C63 60.2(10) . . . . ?
C66 C65 C64 C63 -59.8(9) . . . . ?
C21 C22 C23 C24 0.3(15) . . . . ?
C30 C32 C31 C27 1.3(13) . . . . ?
C28 C27 C31 C32 -1.1(12) . . . . ?
C26 C27 C31 C32 179.5(8) . . . . ?
C22 C23 C24 C25 -0.5(16) . . . . ?
O7 C48 C47 C46 179.5(9) . . . . ?
C43 C48 C47 C46 -0.8(14) . . . . ?
C48 C43 C44 C45 -6.1(13) . . . . ?
C42 C43 C44 C45 174.3(8) . . . . ?
C46 C45 C44 C43 3.5(15) . . . . ?
C23 C24 C25 C26 1.6(16) . . . . ?
C21 C26 C25 C24 -2.3(13) . . . . ?
C27 C26 C25 C24 175.7(9) . . . . ?
C48 C47 C46 C45 -1.9(15) . . . . ?
C44 C45 C46 C47 0.7(15) . . . . ?
C17 C18 C19 C15 -57.4(10) . . . . ?
C20 C18 C19 C15 61.0(9) . . . . ?
C12 C15 C19 C18 -60.6(9) . . . . ?
C14 C15 C19 C18 57.5(10) . . . . ?
V2 O4 C34 C35 -72.5(10) . . . . ?
V1 O4 C34 C35 79.2(9) . . . . ?
C62 C61 C66 C65 -60.9(9) . . . . ?
C58 C61 C66 C65 60.3(9) . . . . ?
C67 C65 C66 C61 -59.9(9) . . . . ?
C64 C65 C66 C61 60.2(9) . . . . ?
O4 C34 C35 C36 -175.1(13) . . . . ?

_diffrn_measured_fraction_theta_max 0.980
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.980
_refine_diff_density_max         1.188
_refine_diff_density_min         -0.531
_refine_diff_density_rms         0.123

_database_code_depnum_ccdc_archive 'CCDC 980011'
#######################################################################
#
#                 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_12

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C63 H64 N2 O8 V2 '
_chemical_formula_sum            'C63 H64 N2 O8 V2'
_chemical_formula_weight         1079.05

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   P-1

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.830(2)
_cell_length_b                   13.423(3)
_cell_length_c                   21.429(4)
_cell_angle_alpha                92.36(3)
_cell_angle_beta                 100.78(3)
_cell_angle_gamma                98.46(3)
_cell_volume                     2740.7(10)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    21355
_cell_measurement_theta_min      0.97
_cell_measurement_theta_max      25.00

_exptl_crystal_description       Plate
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.288
_exptl_crystal_size_mid          0.252
_exptl_crystal_size_min          0.159
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.306
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1132
_exptl_absorpt_coefficient_mu    0.399
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_absorpt_correction_T_min  0.5603
_exptl_absorpt_correction_T_max  1.0000

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Saturn724+ CCD'
_diffrn_measurement_method       'ω scans at fixed χ = 45°'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         none
_diffrn_standards_interval_count none
_diffrn_standards_interval_time  none
_diffrn_standards_decay_%        none
_diffrn_reflns_number            21355
_diffrn_reflns_av_R_equivalents  0.0699
_diffrn_reflns_av_unetI/netI     0.0849
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         0.97
_diffrn_reflns_theta_max         25.00
_reflns_number_total             9547
_reflns_number_gt                7741
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrystalClear (Rigaku Inc., 2007)'
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2007)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'XP in Siemens SHELXTL (Sheldrick, 1994)'
_computing_publication_material  'SHELX97 (Sheldrick, 1997)'


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

 Non-hydrogen atoms closer than 1.7 Α were restrainted to have the
 same U(ij) values with an e.s.d. of 0.02 (SIMU 0.02 0.02 1.7). 
;

_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)+(0.1608P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         9547
_refine_ls_number_parameters     685
_refine_ls_number_restraints     462
_refine_ls_R_factor_ref          0.1196
_refine_ls_R_factor_gt           0.0894
_refine_ls_wR_factor_ref         0.2840
_refine_ls_wR_factor_gt          0.2367
_refine_ls_goodness_of_fit_ref   1.228
_refine_ls_restrained_S_all      1.202
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
V2 V 0.26577(8) 0.77559(6) 0.26785(4) 0.0229(3) Uani 1 1 d U . .
V1 V 0.08096(8) 0.57362(6) 0.20609(4) 0.0234(3) Uani 1 1 d U . .
O4 O 0.1527(4) 0.6496(2) 0.28920(15) 0.0264(8) Uani 1 1 d U . .
O2 O 0.4250(4) 0.7582(3) 0.27758(17) 0.0338(8) Uani 1 1 d U . .
O6 O 0.2310(4) 0.8463(2) 0.34174(15) 0.0274(8) Uani 1 1 d U . .
O3 O 0.1571(4) 0.7118(2) 0.18683(16) 0.0273(8) Uani 1 1 d . . .
H3A H 0.1460 0.7371 0.1514 0.033 Uiso 1 1 d R . .
N1 N -0.0583(4) 0.5549(3) 0.11853(19) 0.0240(9) Uani 1 1 d U . .
O1 O 0.1902(4) 0.5016(3) 0.19393(18) 0.0354(9) Uani 1 1 d U . .
C2 C 0.3656(7) 1.0272(4) 0.6400(3) 0.0429(14) Uani 1 1 d U . .
H2 H 0.4515 1.0604 0.6626 0.052 Uiso 1 1 calc R . .
C36 C -0.1619(6) 0.6800(4) 0.0524(2) 0.0307(11) Uani 1 1 d U . .
C38 C -0.4199(6) 0.6267(4) 0.0410(3) 0.0367(12) Uani 1 1 d U . .
H38 H -0.4248 0.6177 -0.0027 0.044 Uiso 1 1 calc R . .
O7 O -0.1582(4) 0.7143(3) 0.18226(18) 0.0374(9) Uani 1 1 d U . .
C34 C -0.0284(7) 0.7675(4) -0.0177(3) 0.0399(13) Uani 1 1 d U . .
H34 H -0.0210 0.8157 -0.0474 0.048 Uiso 1 1 calc R . .
C10 C 0.2461(5) 0.9707(4) 0.4286(2) 0.0246(10) Uani 1 1 d U . .
C19 C 0.0692(6) 1.1074(4) 0.1602(3) 0.0335(12) Uani 1 1 d U . .
C17 C 0.2888(5) 1.0028(3) 0.2578(2) 0.0251(10) Uani 1 1 d U . .
H17 H 0.3029 1.0595 0.2349 0.030 Uiso 1 1 calc R . .
O8 O 0.1909(4) 1.1724(3) 0.16102(19) 0.0414(10) Uani 1 1 d U . .
C45 C -0.2085(5) 0.4062(3) 0.1445(2) 0.0244(10) Uani 1 1 d U . .
C55 C -0.2145(6) 0.4558(4) 0.3488(3) 0.0351(12) Uani 1 1 d U . .
C8 C 0.3338(6) 0.8193(4) 0.4796(2) 0.0315(12) Uani 1 1 d U . .
H8A H 0.3280 0.7857 0.4386 0.047 Uiso 1 1 calc R . .
H8B H 0.3180 0.7700 0.5098 0.047 Uiso 1 1 calc R . .
H8C H 0.4252 0.8587 0.4932 0.047 Uiso 1 1 calc R . .
C11 C 0.2639(5) 1.0730(4) 0.4460(2) 0.0270(11) Uani 1 1 d U . .
H11 H 0.2576 1.0912 0.4875 0.032 Uiso 1 1 calc R . .
C26 C 0.2156(6) 0.9801(4) 0.0575(2) 0.0311(11) Uani 1 1 d U . .
H26 H 0.1551 1.0132 0.0301 0.037 Uiso 1 1 calc R . .
C44 C -0.1621(5) 0.4797(3) 0.1035(2) 0.0236(10) Uani 1 1 d U . .
H44 H -0.2110 0.4734 0.0616 0.028 Uiso 1 1 calc R . .
C37 C -0.2910(5) 0.6625(4) 0.0803(2) 0.0299(11) Uani 1 1 d U . .
N2 N 0.2803(4) 0.9158(3) 0.22705(19) 0.0247(9) Uani 1 1 d U . .
O5 O -0.0641(4) 0.4896(2) 0.24023(16) 0.0275(8) Uani 1 1 d U . .
C30 C 0.2891(5) 0.9226(3) 0.1606(2) 0.0243(10) Uani 1 1 d U . .
C33 C 0.0814(6) 0.7146(4) 0.0014(3) 0.0392(13) Uani 1 1 d U . .
H33 H 0.1623 0.7267 -0.0155 0.047 Uiso 1 1 calc R . .
C14 C 0.2969(6) 1.1234(4) 0.3453(2) 0.0318(12) Uani 1 1 d U . .
H14 H 0.3135 1.1733 0.3176 0.038 Uiso 1 1 calc R . .
C47 C -0.3800(5) 0.2582(4) 0.1491(3) 0.0325(12) Uani 1 1 d U . .
C29 C 0.3946(6) 0.8807(4) 0.1375(3) 0.0334(12) Uani 1 1 d U . .
H29 H 0.4549 0.8467 0.1644 0.040 Uiso 1 1 calc R . .
C15 C 0.2789(5) 1.0209(4) 0.3226(2) 0.0280(11) Uani 1 1 d U . .
C6 C 0.1202(7) 0.9735(5) 0.6330(3) 0.0444(14) Uani 1 1 d U . .
H6 H 0.0408 0.9692 0.6511 0.053 Uiso 1 1 calc R . .
C52 C -0.1927(6) 0.3518(4) 0.3211(3) 0.0348(12) Uani 1 1 d U . .
C54 C -0.0414(6) 0.3308(4) 0.3395(3) 0.0395(13) Uani 1 1 d U . .
H54A H 0.0201 0.3799 0.3223 0.059 Uiso 1 1 calc R . .
H54B H -0.0360 0.2644 0.3227 0.059 Uiso 1 1 calc R . .
H54C H -0.0138 0.3349 0.3851 0.059 Uiso 1 1 calc R . .
C32 C 0.0695(6) 0.6443(4) 0.0455(2) 0.0337(12) Uani 1 1 d U . .
H32 H 0.1425 0.6081 0.0581 0.040 Uiso 1 1 calc R . .
C28 C 0.4089(6) 0.8897(4) 0.0759(3) 0.0386(13) Uani 1 1 d U . .
H28 H 0.4783 0.8611 0.0609 0.046 Uiso 1 1 calc R . .
C60 C -0.1369(7) 0.4983(5) 0.4071(3) 0.0450(14) Uani 1 1 d U . .
H60 H -0.0655 0.4669 0.4286 0.054 Uiso 1 1 calc R . .
C41 C -0.4082(6) 0.6544(4) 0.1708(3) 0.0365(12) Uani 1 1 d U . .
H41 H -0.4048 0.6630 0.2144 0.044 Uiso 1 1 calc R . .
C53 C -0.2857(7) 0.2722(5) 0.3507(3) 0.0471(15) Uani 1 1 d U . .
H53A H -0.2613 0.2822 0.3963 0.071 Uiso 1 1 calc R . .
H53B H -0.2715 0.2059 0.3376 0.071 Uiso 1 1 calc R . .
H53C H -0.3824 0.2789 0.3368 0.071 Uiso 1 1 calc R . .
C50 C -0.1646(5) 0.4161(4) 0.2110(2) 0.0280(11) Uani 1 1 d U . .
C57 C -0.3479(9) 0.5919(6) 0.3457(3) 0.0604(19) Uani 1 1 d U . .
H57 H -0.4212 0.6223 0.3250 0.073 Uiso 1 1 calc R . .
C12 C 0.2905(6) 1.1513(4) 0.4068(2) 0.0309(11) Uani 1 1 d U . .
C35 C -0.1489(6) 0.7489(4) 0.0071(3) 0.0377(13) Uani 1 1 d U . .
H35 H -0.2228 0.7835 -0.0071 0.045 Uiso 1 1 calc R . .
C1 C 0.3555(6) 0.9846(4) 0.5794(3) 0.0345(12) Uani 1 1 d U . .
H1 H 0.4359 0.9881 0.5621 0.041 Uiso 1 1 calc R . .
C42 C -0.2870(5) 0.6772(4) 0.1464(3) 0.0304(11) Uani 1 1 d U . .
C7 C 0.2208(5) 0.8898(4) 0.4752(2) 0.0265(11) Uani 1 1 d U . .
C51 C -0.2334(5) 0.3447(4) 0.2486(2) 0.0277(11) Uani 1 1 d U . .
C4 C 0.2271(5) 0.9359(4) 0.5431(2) 0.0283(11) Uani 1 1 d U . .
C49 C -0.3367(5) 0.2696(4) 0.2164(3) 0.0330(12) Uani 1 1 d U . .
H49 H -0.3807 0.2234 0.2403 0.040 Uiso 1 1 calc R . .
C5 C 0.1106(6) 0.9325(4) 0.5717(2) 0.0332(12) Uani 1 1 d U . .
H5 H 0.0235 0.9017 0.5488 0.040 Uiso 1 1 calc R . .
C9 C 0.0745(6) 0.8261(4) 0.4504(3) 0.0333(12) Uani 1 1 d U . .
H9A H 0.0041 0.8693 0.4471 0.050 Uiso 1 1 calc R . .
H9B H 0.0564 0.7755 0.4794 0.050 Uiso 1 1 calc R . .
H9C H 0.0722 0.7942 0.4092 0.050 Uiso 1 1 calc R . .
C16 C 0.2516(5) 0.9432(3) 0.3637(2) 0.0248(10) Uani 1 1 d U . .
C25 C 0.1974(5) 0.9712(3) 0.1199(2) 0.0261(11) Uani 1 1 d U . .
C24 C 0.0724(6) 1.0060(4) 0.1403(2) 0.0288(11) Uani 1 1 d U . .
C48 C -0.4935(6) 0.1732(4) 0.1168(3) 0.0463(15) Uani 1 1 d U . .
H48A H -0.4743 0.1105 0.1337 0.069 Uiso 1 1 calc R . .
H48B H -0.4954 0.1694 0.0718 0.069 Uiso 1 1 calc R . .
H48C H -0.5828 0.1860 0.1245 0.069 Uiso 1 1 calc R . .
C27 C 0.3200(6) 0.9415(4) 0.0351(3) 0.0359(13) Uani 1 1 d U . .
H27 H 0.3317 0.9496 -0.0066 0.043 Uiso 1 1 calc R . .
C61 C 0.1627(6) 0.6091(4) 0.3505(2) 0.0324(12) Uani 1 1 d U . .
H61A H 0.0856 0.5544 0.3489 0.039 Uiso 1 1 calc R . .
H61B H 0.1544 0.6612 0.3817 0.039 Uiso 1 1 calc R . .
C13 C 0.2488(7) 1.0209(4) 0.6674(3) 0.0436(14) Uani 1 1 d U . .
H13 H 0.2562 1.0483 0.7087 0.052 Uiso 1 1 calc R . .
C43 C -0.1505(6) 0.7397(5) 0.2489(3) 0.0404(13) Uani 1 1 d U . .
H43A H -0.2247 0.7767 0.2539 0.061 Uiso 1 1 calc R . .
H43B H -0.0617 0.7804 0.2663 0.061 Uiso 1 1 calc R . .
H43C H -0.1600 0.6789 0.2708 0.061 Uiso 1 1 calc R . .
C31 C -0.0499(5) 0.6265(4) 0.0716(2) 0.0267(10) Uani 1 1 d U . .
C18 C 0.3093(8) 1.2599(4) 0.4313(3) 0.0454(15) Uani 1 1 d U . .
H18A H 0.2312 1.2709 0.4502 0.068 Uiso 1 1 calc R . .
H18B H 0.3144 1.3025 0.3966 0.068 Uiso 1 1 calc R . .
H18C H 0.3944 1.2756 0.4626 0.068 Uiso 1 1 calc R . .
C20 C -0.0511(7) 1.1337(4) 0.1768(3) 0.0429(14) Uani 1 1 d U . .
H20 H -0.0531 1.2005 0.1895 0.051 Uiso 1 1 calc R . .
C22 C -0.1670(6) 0.9626(5) 0.1569(3) 0.0493(15) Uani 1 1 d U . .
H22 H -0.2451 0.9143 0.1570 0.059 Uiso 1 1 calc R . .
C1A C 0.1933(8) 1.2763(4) 0.1814(3) 0.0573(18) Uani 1 1 d U . .
H1AA H 0.1194 1.3027 0.1545 0.086 Uiso 1 1 calc R . .
H1AB H 0.2821 1.3150 0.1787 0.086 Uiso 1 1 calc R . .
H1AC H 0.1802 1.2807 0.2247 0.086 Uiso 1 1 calc R . .
C59 C -0.1649(8) 0.5867(5) 0.4334(3) 0.0601(19) Uani 1 1 d U . .
H59 H -0.1126 0.6141 0.4727 0.072 Uiso 1 1 calc R . .
C40 C -0.5346(6) 0.6186(5) 0.1298(3) 0.0443(14) Uani 1 1 d U . .
H40 H -0.6160 0.6041 0.1462 0.053 Uiso 1 1 calc R . .
C21 C -0.1662(7) 1.0627(5) 0.1749(3) 0.0495(15) Uani 1 1 d U . .
H21 H -0.2461 1.0821 0.1860 0.059 Uiso 1 1 calc R . .
C46 C -0.3174(5) 0.3281(4) 0.1147(3) 0.0281(11) Uani 1 1 d U . .
H46 H -0.3468 0.3246 0.0708 0.034 Uiso 1 1 calc R . .
C56 C -0.3205(7) 0.5035(5) 0.3183(3) 0.0449(15) Uani 1 1 d U . .
H56 H -0.3739 0.4762 0.2792 0.054 Uiso 1 1 calc R . .
C39 C -0.5413(6) 0.6043(5) 0.0652(3) 0.0472(15) Uani 1 1 d U . .
H39 H -0.6263 0.5798 0.0381 0.057 Uiso 1 1 calc R . .
C58 C -0.2703(9) 0.6352(5) 0.4018(4) 0.063(2) Uani 1 1 d U . .
H58 H -0.2873 0.6960 0.4188 0.076 Uiso 1 1 calc R . .
C23 C -0.0476(6) 0.9358(4) 0.1386(3) 0.0369(12) Uani 1 1 d U . .
H23 H -0.0482 0.8691 0.1248 0.044 Uiso 1 1 calc R . .
C62 C 0.2993(8) 0.5705(6) 0.3711(3) 0.0575(18) Uani 1 1 d U . .
H62A H 0.3764 0.6247 0.3710 0.069 Uiso 1 1 calc R . .
H62B H 0.3059 0.5168 0.3406 0.069 Uiso 1 1 calc R . .
C63 C 0.3137(10) 0.5308(5) 0.4371(3) 0.078(3) Uani 1 1 d U . .
H63A H 0.2381 0.4768 0.4375 0.117 Uiso 1 1 calc R . .
H63B H 0.3104 0.5843 0.4677 0.117 Uiso 1 1 calc R . .
H63C H 0.4015 0.5063 0.4479 0.117 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
V2 O2 1.593(4) . ?
V2 O6 1.924(3) . ?
V2 O3 1.950(4) . ?
V2 O4 2.001(3) . ?
V2 N2 2.105(4) . ?
V1 O1 1.595(4) . ?
V1 O5 1.956(3) . ?
V1 O4 1.970(3) . ?
V1 O3 1.985(3) . ?
V1 N1 2.087(4) . ?
O4 C61 1.433(6) . ?
O6 C16 1.338(6) . ?
N1 C44 1.307(6) . ?
N1 C31 1.425(6) . ?
C2 C13 1.376(8) . ?
C2 C1 1.377(8) . ?
C36 C35 1.379(7) . ?
C36 C31 1.409(7) . ?
C36 C37 1.494(7) . ?
C38 C39 1.387(8) . ?
C38 C37 1.391(7) . ?
O7 C42 1.364(6) . ?
O7 C43 1.439(6) . ?
C34 C35 1.380(8) . ?
C34 C33 1.386(8) . ?
C10 C11 1.384(7) . ?
C10 C16 1.436(7) . ?
C10 C7 1.531(7) . ?
C19 O8 1.370(6) . ?
C19 C20 1.386(8) . ?
C19 C24 1.416(7) . ?
C17 N2 1.300(6) . ?
C17 C15 1.425(7) . ?
O8 C1A 1.441(7) . ?
C45 C50 1.405(7) . ?
C45 C46 1.417(7) . ?
C45 C44 1.430(6) . ?
C55 C56 1.377(8) . ?
C55 C60 1.388(9) . ?
C55 C52 1.554(7) . ?
C8 C7 1.554(7) . ?
C11 C12 1.397(7) . ?
C26 C27 1.368(7) . ?
C26 C25 1.389(7) . ?
C37 C42 1.415(7) . ?
N2 C30 1.448(6) . ?
O5 C50 1.331(6) . ?
C30 C25 1.388(7) . ?
C30 C29 1.407(7) . ?
C33 C32 1.372(7) . ?
C14 C12 1.372(7) . ?
C14 C15 1.414(7) . ?
C47 C46 1.364(7) . ?
C47 C49 1.420(8) . ?
C47 C48 1.515(7) . ?
C29 C28 1.361(8) . ?
C15 C16 1.421(7) . ?
C6 C5 1.386(8) . ?
C6 C13 1.386(9) . ?
C52 C51 1.524(7) . ?
C52 C54 1.537(8) . ?
C52 C53 1.539(7) . ?
C32 C31 1.385(7) . ?
C28 C27 1.398(8) . ?
C60 C59 1.378(9) . ?
C41 C42 1.388(7) . ?
C41 C40 1.389(8) . ?
C50 C51 1.449(6) . ?
C57 C58 1.355(11) . ?
C57 C56 1.387(9) . ?
C12 C18 1.501(7) . ?
C1 C4 1.405(7) . ?
C7 C4 1.543(7) . ?
C7 C9 1.548(7) . ?
C51 C49 1.380(7) . ?
C4 C5 1.393(7) . ?
C25 C24 1.507(7) . ?
C24 C23 1.390(7) . ?
C61 C62 1.506(8) . ?
C20 C21 1.361(9) . ?
C22 C21 1.381(9) . ?
C22 C23 1.395(8) . ?
C59 C58 1.389(11) . ?
C40 C39 1.378(8) . ?
C62 C63 1.522(9) . ?

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 V2 O6 111.05(18) . . ?
O2 V2 O3 111.39(17) . . ?
O6 V2 O3 137.40(15) . . ?
O2 V2 O4 107.73(16) . . ?
O6 V2 O4 89.69(14) . . ?
O3 V2 O4 74.22(14) . . ?
O2 V2 N2 100.32(17) . . ?
O6 V2 N2 86.58(15) . . ?
O3 V2 N2 89.41(15) . . ?
O4 V2 N2 151.11(15) . . ?
O1 V1 O5 105.90(16) . . ?
O1 V1 O4 108.47(18) . . ?
O5 V1 O4 91.36(14) . . ?
O1 V1 O3 107.36(16) . . ?
O5 V1 O3 146.46(15) . . ?
O4 V1 O3 74.17(14) . . ?
O1 V1 N1 101.45(18) . . ?
O5 V1 N1 87.32(15) . . ?
O4 V1 N1 149.20(15) . . ?
O3 V1 N1 90.28(15) . . ?
C61 O4 V1 126.4(3) . . ?
C61 O4 V2 126.6(3) . . ?
V1 O4 V2 103.75(15) . . ?
C16 O6 V2 134.9(3) . . ?
V2 O3 V1 105.08(15) . . ?
C44 N1 C31 115.1(4) . . ?
C44 N1 V1 123.1(3) . . ?
C31 N1 V1 121.7(3) . . ?
C13 C2 C1 120.3(6) . . ?
C35 C36 C31 118.0(5) . . ?
C35 C36 C37 121.0(5) . . ?
C31 C36 C37 121.0(4) . . ?
C39 C38 C37 121.7(5) . . ?
C42 O7 C43 117.4(4) . . ?
C35 C34 C33 120.2(5) . . ?
C11 C10 C16 116.6(4) . . ?
C11 C10 C7 122.6(4) . . ?
C16 C10 C7 120.8(4) . . ?
O8 C19 C20 125.4(5) . . ?
O8 C19 C24 114.7(5) . . ?
C20 C19 C24 119.9(5) . . ?
N2 C17 C15 127.3(4) . . ?
C19 O8 C1A 116.8(5) . . ?
C50 C45 C46 120.8(4) . . ?
C50 C45 C44 123.2(4) . . ?
C46 C45 C44 115.4(4) . . ?
C56 C55 C60 118.5(6) . . ?
C56 C55 C52 120.1(5) . . ?
C60 C55 C52 121.2(5) . . ?
C10 C11 C12 126.1(5) . . ?
C27 C26 C25 121.9(5) . . ?
N1 C44 C45 127.1(5) . . ?
C38 C37 C42 118.0(5) . . ?
C38 C37 C36 119.7(5) . . ?
C42 C37 C36 122.3(5) . . ?
C17 N2 C30 113.9(4) . . ?
C17 N2 V2 125.1(3) . . ?
C30 N2 V2 121.0(3) . . ?
C50 O5 V1 129.7(3) . . ?
C25 C30 C29 119.6(4) . . ?
C25 C30 N2 121.3(4) . . ?
C29 C30 N2 119.1(4) . . ?
C32 C33 C34 119.3(5) . . ?
C12 C14 C15 122.0(4) . . ?
C46 C47 C49 117.2(5) . . ?
C46 C47 C48 121.3(5) . . ?
C49 C47 C48 121.5(5) . . ?
C28 C29 C30 120.3(5) . . ?
C14 C15 C16 120.1(4) . . ?
C14 C15 C17 116.0(4) . . ?
C16 C15 C17 123.9(4) . . ?
C5 C6 C13 119.7(5) . . ?
C51 C52 C54 108.2(4) . . ?
C51 C52 C53 112.0(5) . . ?
C54 C52 C53 107.1(4) . . ?
C51 C52 C55 110.2(4) . . ?
C54 C52 C55 113.6(5) . . ?
C53 C52 C55 105.7(4) . . ?
C33 C32 C31 120.8(5) . . ?
C29 C28 C27 120.5(5) . . ?
C59 C60 C55 120.5(7) . . ?
C42 C41 C40 119.6(5) . . ?
O5 C50 C45 122.1(4) . . ?
O5 C50 C51 119.5(5) . . ?
C45 C50 C51 118.5(5) . . ?
C58 C57 C56 121.6(7) . . ?
C14 C12 C11 116.4(5) . . ?
C14 C12 C18 122.4(5) . . ?
C11 C12 C18 121.2(5) . . ?
C36 C35 C34 121.4(5) . . ?
C2 C1 C4 121.8(5) . . ?
O7 C42 C41 124.4(5) . . ?
O7 C42 C37 115.1(4) . . ?
C41 C42 C37 120.5(5) . . ?
C10 C7 C4 112.2(4) . . ?
C10 C7 C9 108.4(4) . . ?
C4 C7 C9 109.4(4) . . ?
C10 C7 C8 110.4(4) . . ?
C4 C7 C8 107.5(4) . . ?
C9 C7 C8 109.0(4) . . ?
C49 C51 C50 117.5(5) . . ?
C49 C51 C52 121.1(4) . . ?
C50 C51 C52 121.4(5) . . ?
C5 C4 C1 116.4(5) . . ?
C5 C4 C7 123.5(5) . . ?
C1 C4 C7 120.0(4) . . ?
C51 C49 C47 124.3(5) . . ?
C6 C5 C4 122.1(5) . . ?
O6 C16 C15 120.0(4) . . ?
O6 C16 C10 121.2(4) . . ?
C15 C16 C10 118.8(4) . . ?
C30 C25 C26 118.8(5) . . ?
C30 C25 C24 121.3(4) . . ?
C26 C25 C24 119.7(5) . . ?
C23 C24 C19 117.7(5) . . ?
C23 C24 C25 118.8(5) . . ?
C19 C24 C25 123.5(5) . . ?
C26 C27 C28 118.9(5) . . ?
O4 C61 C62 112.0(5) . . ?
C2 C13 C6 119.6(6) . . ?
C32 C31 C36 120.2(5) . . ?
C32 C31 N1 119.8(5) . . ?
C36 C31 N1 120.0(4) . . ?
C21 C20 C19 120.6(5) . . ?
C21 C22 C23 118.3(6) . . ?
C60 C59 C58 120.6(7) . . ?
C39 C40 C41 121.0(5) . . ?
C20 C21 C22 121.4(6) . . ?
C47 C46 C45 121.6(5) . . ?
C55 C56 C57 120.2(7) . . ?
C40 C39 C38 119.3(6) . . ?
C57 C58 C59 118.5(7) . . ?
C24 C23 C22 121.9(5) . . ?
C61 C62 C63 112.6(6) . . ?

_diffrn_measured_fraction_theta_max 0.991
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.991
_refine_diff_density_max         0.703
_refine_diff_density_min         -1.326
_refine_diff_density_rms         0.248

_database_code_depnum_ccdc_archive 'CCDC 980012'
#######################################################################
#
#                 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_13

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C51 H56 N2 O8 V2'
_chemical_formula_sum            'C51 H56 N2 O8 V2'
_chemical_formula_weight         926.86

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           ?
_symmetry_space_group_name_H-M   'P -1'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.169(2)
_cell_length_b                   12.960(3)
_cell_length_c                   20.218(4)
_cell_angle_alpha                71.25(3)
_cell_angle_beta                 71.42(3)
_cell_angle_gamma                74.94(3)
_cell_volume                     2354.6(10)
_cell_formula_units_Z            2
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    17326
_cell_measurement_theta_min      1.69
_cell_measurement_theta_max      25.00

_exptl_crystal_description       Plate
_exptl_crystal_colour            brown
_exptl_crystal_size_max          0.443
_exptl_crystal_size_mid          0.282
_exptl_crystal_size_min          0.254
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.307
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             972
_exptl_absorpt_coefficient_mu    0.452
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_absorpt_correction_T_min  0.6363
_exptl_absorpt_correction_T_max  1.0000

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'MM007-HF CCD(Saturn 724+)'
_diffrn_measurement_method       'ω scans at fixed χ = 45°'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         none
_diffrn_standards_interval_count none
_diffrn_standards_interval_time  none
_diffrn_standards_decay_%        none
_diffrn_reflns_number            17326
_diffrn_reflns_av_R_equivalents  0.0574
_diffrn_reflns_av_unetI/netI     0.0599
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         1.69
_diffrn_reflns_theta_max         25.00
_reflns_number_total             8194
_reflns_number_gt                7318
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrystalClear (Rigaku Inc., 2007)'
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2007)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'XP in Siemens SHELXTL (Sheldrick, 1994)'
_computing_publication_material  'SHELX97 (Sheldrick, 1997)'


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

 Non-hydrogen atoms closer than 1.7 Α were restrainted to have the
 same U(ij) values with an e.s.d. of 0.02 (SIMU 0.01 0.02 1.7). 
 The thermal parameters of non-hydrogen atoms were restrained to
 approximate to isotropic behaviour with an e.s.d. of 0.02
 (ISOR 0.02).
;

_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)+(0.0440P)²+0.9953P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         8194
_refine_ls_number_parameters     577
_refine_ls_number_restraints     756
_refine_ls_R_factor_ref          0.0536
_refine_ls_R_factor_gt           0.0464
_refine_ls_wR_factor_ref         0.1164
_refine_ls_wR_factor_gt          0.1112
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_restrained_S_all      1.032
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
V1 V 0.62987(4) 0.09923(3) 0.286474(19) 0.02253(11) Uani 1 1 d U . .
V2 V 0.49046(4) 0.32952(3) 0.204796(19) 0.02236(11) Uani 1 1 d U . .
O2 O 0.34423(16) 0.32477(13) 0.19383(9) 0.0317(4) Uani 1 1 d U . .
O6 O 0.60890(15) 0.40664(12) 0.11990(8) 0.0248(3) Uani 1 1 d U . .
O4 O 0.61267(16) 0.18865(12) 0.18903(8) 0.0273(3) Uani 1 1 d U . .
O3 O 0.52571(16) 0.24610(12) 0.29840(8) 0.0268(3) Uani 1 1 d U . .
H3A H 0.5014 0.2681 0.3361 0.032 Uiso 1 1 d R . .
O1 O 0.52211(17) 0.01571(13) 0.31703(9) 0.0341(4) Uani 1 1 d U . .
O5 O 0.81034(16) 0.02104(13) 0.24437(8) 0.0305(4) Uani 1 1 d U . .
O7 O 0.83895(16) 0.24875(14) 0.28983(8) 0.0346(4) Uani 1 1 d U . .
O8 O 0.3909(2) 0.72732(14) 0.31680(11) 0.0485(5) Uani 1 1 d U . .
N2 N 0.43609(18) 0.47528(15) 0.23856(10) 0.0251(4) Uani 1 1 d U . .
N1 N 0.70379(18) 0.06463(14) 0.37749(9) 0.0236(4) Uani 1 1 d U . .
C1 C 0.8775(2) 0.3474(2) 0.01925(13) 0.0341(5) Uani 1 1 d U . .
H1A H 0.8152 0.3150 0.0655 0.051 Uiso 1 1 calc R . .
H1B H 0.9543 0.3693 0.0281 0.051 Uiso 1 1 calc R . .
H1C H 0.9168 0.2927 -0.0091 0.051 Uiso 1 1 calc R . .
C2 C 0.6745(2) 0.4192(2) -0.04047(12) 0.0312(5) Uani 1 1 d U . .
H2A H 0.6039 0.3940 0.0044 0.047 Uiso 1 1 calc R . .
H2B H 0.7137 0.3598 -0.0651 0.047 Uiso 1 1 calc R . .
H2C H 0.6300 0.4843 -0.0720 0.047 Uiso 1 1 calc R . .
C3 C 0.8959(3) 0.4952(2) -0.09495(13) 0.0394(6) Uani 1 1 d U . .
H111 H 0.9353 0.4378 -0.1213 0.059 Uiso 1 1 calc R . .
H3B H 0.9723 0.5168 -0.0856 0.059 Uiso 1 1 calc R . .
H3C H 0.8456 0.5598 -0.1240 0.059 Uiso 1 1 calc R . .
C4 C 0.7930(2) 0.44981(19) -0.02277(12) 0.0278(5) Uani 1 1 d U . .
C5 C 0.7261(2) 0.53653(18) 0.02084(12) 0.0259(5) Uani 1 1 d U . .
C6 C 0.7475(2) 0.6454(2) -0.00696(13) 0.0342(5) Uani 1 1 d U . .
H6 H 0.8080 0.6657 -0.0540 0.041 Uiso 1 1 calc R . .
C7 C 0.6850(3) 0.7266(2) 0.03052(14) 0.0392(6) Uani 1 1 d U . .
H7 H 0.7045 0.7997 0.0095 0.047 Uiso 1 1 calc R . .
C8 C 0.5960(3) 0.70043(19) 0.09740(13) 0.0349(5) Uani 1 1 d U . .
H8 H 0.5525 0.7554 0.1231 0.042 Uiso 1 1 calc R . .
C9 C 0.5681(2) 0.59174(18) 0.12856(12) 0.0265(5) Uani 1 1 d U . .
C10 C 0.6335(2) 0.50909(17) 0.09067(11) 0.0234(4) Uani 1 1 d U . .
C11 C 0.4738(2) 0.56921(18) 0.19940(12) 0.0265(5) Uani 1 1 d U . .
H11 H 0.4343 0.6302 0.2201 0.032 Uiso 1 1 calc R . .
C12 C 0.3518(2) 0.47122(17) 0.31112(12) 0.0273(5) Uani 1 1 d U . .
C13 C 0.2291(3) 0.4257(2) 0.33499(14) 0.0362(6) Uani 1 1 d U . .
H13 H 0.2009 0.4019 0.3026 0.043 Uiso 1 1 calc R . .
C14 C 0.1485(3) 0.4151(2) 0.40573(15) 0.0422(6) Uani 1 1 d U . .
H14 H 0.0649 0.3845 0.4216 0.051 Uiso 1 1 calc R . .
C15 C 0.1896(3) 0.4489(2) 0.45291(14) 0.0398(6) Uani 1 1 d U . .
H15 H 0.1342 0.4418 0.5014 0.048 Uiso 1 1 calc R . .
C16 C 0.3116(3) 0.49320(19) 0.42985(13) 0.0363(6) Uani 1 1 d U . .
H16 H 0.3392 0.5158 0.4630 0.044 Uiso 1 1 calc R . .
C17 C 0.3949(2) 0.50541(18) 0.35891(12) 0.0297(5) Uani 1 1 d U . .
C18 C 0.5270(3) 0.5514(2) 0.33703(12) 0.0346(5) Uani 1 1 d U . .
C19 C 0.5218(3) 0.6662(2) 0.31733(13) 0.0411(6) Uani 1 1 d U . .
C21 C 0.3746(5) 0.8460(2) 0.2967(2) 0.0791(12) Uani 1 1 d U . .
H21A H 0.4248 0.8716 0.2459 0.119 Uiso 1 1 calc R . .
H21B H 0.4134 0.8691 0.3272 0.119 Uiso 1 1 calc R . .
H21C H 0.2743 0.8783 0.3032 0.119 Uiso 1 1 calc R . .
C22 C 0.6412(4) 0.7102(3) 0.29977(16) 0.0579(8) Uani 1 1 d U . .
H22 H 0.6363 0.7881 0.2865 0.070 Uiso 1 1 calc R . .
C23 C 0.7683(4) 0.6401(4) 0.3017(2) 0.0757(11) Uani 1 1 d U . .
H23 H 0.8509 0.6704 0.2902 0.091 Uiso 1 1 calc R . .
C24 C 0.7779(4) 0.5267(4) 0.3199(2) 0.0745(10) Uani 1 1 d U . .
H24 H 0.8665 0.4793 0.3202 0.089 Uiso 1 1 calc R . .
C25 C 0.6560(3) 0.4822(3) 0.33799(16) 0.0512(7) Uani 1 1 d U . .
H25 H 0.6615 0.4042 0.3510 0.061 Uiso 1 1 calc R . .
C26 C 0.6315(3) 0.15173(19) 0.12621(12) 0.0333(5) Uani 1 1 d U . .
H26A H 0.7272 0.1075 0.1147 0.040 Uiso 1 1 calc R . .
H26B H 0.6240 0.2169 0.0845 0.040 Uiso 1 1 calc R . .
C27 C 0.5249(4) 0.0832(3) 0.13708(15) 0.0550(8) Uani 1 1 d U . .
H27A H 0.4296 0.1285 0.1468 0.066 Uiso 1 1 calc R . .
H27B H 0.5299 0.0199 0.1801 0.066 Uiso 1 1 calc R . .
C28 C 0.5466(4) 0.0396(3) 0.07235(17) 0.0623(9) Uani 1 1 d U . .
H28A H 0.5470 0.1017 0.0290 0.093 Uiso 1 1 calc R . .
H28B H 0.4699 0.0004 0.0808 0.093 Uiso 1 1 calc R . .
H28C H 0.6368 -0.0113 0.0654 0.093 Uiso 1 1 calc R . .
C29 C 1.0533(3) 0.0263(3) 0.11786(17) 0.0617(9) Uani 1 1 d U . .
H29A H 0.9670 0.0755 0.1355 0.093 Uiso 1 1 calc R . .
H29B H 1.0770 0.0449 0.0650 0.093 Uiso 1 1 calc R . .
H29C H 1.1307 0.0354 0.1334 0.093 Uiso 1 1 calc R . .
C30 C 0.9067(4) -0.1124(3) 0.12862(16) 0.0617(9) Uani 1 1 d U . .
H30A H 0.9026 -0.1915 0.1435 0.093 Uiso 1 1 calc R . .
H30B H 0.9197 -0.0847 0.0762 0.093 Uiso 1 1 calc R . .
H30C H 0.8186 -0.0722 0.1532 0.093 Uiso 1 1 calc R . .
C31 C 1.1639(4) -0.1667(3) 0.1137(2) 0.0858(13) Uani 1 1 d U . .
H31A H 1.2447 -0.1603 0.1277 0.129 Uiso 1 1 calc R . .
H31B H 1.1809 -0.1413 0.0610 0.129 Uiso 1 1 calc R . .
H31C H 1.1512 -0.2441 0.1300 0.129 Uiso 1 1 calc R . .
C32 C 1.0300(3) -0.0947(2) 0.14890(15) 0.0513(7) Uani 1 1 d U . .
C33 C 1.0025(3) -0.1287(2) 0.23120(14) 0.0377(6) Uani 1 1 d U . .
C34 C 1.0792(3) -0.2232(2) 0.26761(16) 0.0443(7) Uani 1 1 d U . .
H34 H 1.1501 -0.2675 0.2397 0.053 Uiso 1 1 calc R . .
C35 C 1.0584(3) -0.2567(2) 0.34220(17) 0.0464(7) Uani 1 1 d U . .
H35 H 1.1099 -0.3244 0.3644 0.056 Uiso 1 1 calc R . .
C36 C 0.9630(3) -0.1910(2) 0.38320(14) 0.0379(6) Uani 1 1 d U . .
H36 H 0.9520 -0.2104 0.4339 0.045 Uiso 1 1 calc R . .
C37 C 0.8937(2) -0.06531(18) 0.27491(13) 0.0294(5) Uani 1 1 d U . .
C38 C 0.8809(2) -0.09427(19) 0.35011(12) 0.0290(5) Uani 1 1 d U . .
C39 C 0.7970(2) -0.02192(18) 0.39411(12) 0.0272(5) Uani 1 1 d U . .
H39 H 0.8111 -0.0392 0.4410 0.033 Uiso 1 1 calc R . .
C40 C 0.6511(2) 0.13312(18) 0.42690(11) 0.0253(5) Uani 1 1 d U . .
C41 C 0.5077(2) 0.1483(2) 0.46152(12) 0.0328(5) Uani 1 1 d U . .
H41 H 0.4464 0.1134 0.4523 0.039 Uiso 1 1 calc R . .
C42 C 0.4549(3) 0.2140(2) 0.50920(13) 0.0423(6) Uani 1 1 d U . .
H42 H 0.3574 0.2241 0.5330 0.051 Uiso 1 1 calc R . .
C43 C 0.5439(3) 0.2649(2) 0.52220(14) 0.0484(7) Uani 1 1 d U . .
H43 H 0.5071 0.3108 0.5547 0.058 Uiso 1 1 calc R . .
C44 C 0.6854(3) 0.2498(2) 0.48853(13) 0.0424(6) Uani 1 1 d U . .
H44 H 0.7458 0.2842 0.4989 0.051 Uiso 1 1 calc R . .
C45 C 0.7421(2) 0.18486(19) 0.43934(11) 0.0289(5) Uani 1 1 d U . .
C46 C 0.8960(2) 0.17281(19) 0.40143(12) 0.0302(5) Uani 1 1 d U . .
C47 C 0.9422(2) 0.20392(19) 0.32603(12) 0.0296(5) Uani 1 1 d U . .
C48 C 0.9964(3) 0.1288(2) 0.44088(14) 0.0414(6) Uani 1 1 d U . .
H48 H 0.9668 0.1091 0.4922 0.050 Uiso 1 1 calc R . .
C49 C 1.0852(3) 0.1906(2) 0.29162(14) 0.0398(6) Uani 1 1 d U . .
H49 H 1.1162 0.2131 0.2404 0.048 Uiso 1 1 calc R . .
C50 C 1.1819(3) 0.1444(2) 0.33263(16) 0.0490(7) Uani 1 1 d U . .
H50 H 1.2797 0.1340 0.3092 0.059 Uiso 1 1 calc R . .
C51 C 1.1391(3) 0.1133(3) 0.40658(16) 0.0534(8) Uani 1 1 d U . .
H51 H 1.2066 0.0814 0.4342 0.064 Uiso 1 1 calc R . .
C52 C 0.8816(3) 0.2992(3) 0.21409(13) 0.0504(7) Uani 1 1 d U . .
H52A H 0.9417 0.3527 0.2055 0.076 Uiso 1 1 calc R . .
H52B H 0.7980 0.3372 0.1961 0.076 Uiso 1 1 calc R . .
H52C H 0.9342 0.2421 0.1887 0.076 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 1.5841(17) . ?
V1 O5 1.9267(17) . ?
V1 O3 1.9717(16) . ?
V1 O4 1.9751(16) . ?
V1 N1 2.0803(18) . ?
V2 O2 1.5909(16) . ?
V2 O6 1.8977(17) . ?
V2 O3 1.9479(16) . ?
V2 O4 1.9803(16) . ?
V2 N2 2.0943(19) . ?
O6 C10 1.322(3) . ?
O4 C26 1.438(3) . ?
O3 H3A 0.8401 . ?
O5 C37 1.322(3) . ?
O7 C47 1.369(3) . ?
O7 C52 1.428(3) . ?
O8 C19 1.362(3) . ?
O8 C21 1.438(3) . ?
N2 C11 1.298(3) . ?
N2 C12 1.436(3) . ?
N1 C39 1.295(3) . ?
N1 C40 1.433(3) . ?
C1 C4 1.539(3) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 C4 1.534(3) . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C3 C4 1.538(3) . ?
C3 H111 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C4 C5 1.536(3) . ?
C5 C6 1.388(3) . ?
C5 C10 1.418(3) . ?
C6 C7 1.394(3) . ?
C6 H6 0.9500 . ?
C7 C8 1.359(4) . ?
C7 H7 0.9500 . ?
C8 C9 1.409(3) . ?
C8 H8 0.9500 . ?
C9 C10 1.417(3) . ?
C9 C11 1.434(3) . ?
C11 H11 0.9500 . ?
C12 C13 1.398(3) . ?
C12 C17 1.403(3) . ?
C13 C14 1.386(4) . ?
C13 H13 0.9500 . ?
C14 C15 1.377(4) . ?
C14 H14 0.9500 . ?
C15 C16 1.384(4) . ?
C15 H15 0.9500 . ?
C16 C17 1.396(3) . ?
C16 H16 0.9500 . ?
C17 C18 1.492(3) . ?
C18 C25 1.385(4) . ?
C18 C19 1.402(4) . ?
C19 C22 1.371(4) . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 C23 1.377(5) . ?
C22 H22 0.9500 . ?
C23 C24 1.381(5) . ?
C23 H23 0.9500 . ?
C24 C25 1.396(5) . ?
C24 H24 0.9500 . ?
C25 H25 0.9500 . ?
C26 C27 1.495(4) . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C27 C28 1.519(4) . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 C32 1.541(4) . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C30 C32 1.526(5) . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C31 C32 1.543(4) . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C32 C33 1.529(4) . ?
C33 C34 1.393(4) . ?
C33 C37 1.433(3) . ?
C34 C35 1.390(4) . ?
C34 H34 0.9500 . ?
C35 C36 1.366(4) . ?
C35 H35 0.9500 . ?
C36 C38 1.410(3) . ?
C36 H36 0.9500 . ?
C37 C38 1.415(3) . ?
C38 C39 1.427(3) . ?
C39 H39 0.9500 . ?
C40 C41 1.394(3) . ?
C40 C45 1.396(3) . ?
C41 C42 1.379(3) . ?
C41 H41 0.9500 . ?
C42 C43 1.377(4) . ?
C42 H42 0.9500 . ?
C43 C44 1.374(4) . ?
C43 H43 0.9500 . ?
C44 C45 1.397(3) . ?
C44 H44 0.9500 . ?
C45 C46 1.499(3) . ?
C46 C48 1.389(3) . ?
C46 C47 1.398(3) . ?
C47 C49 1.390(3) . ?
C48 C51 1.387(4) . ?
C48 H48 0.9500 . ?
C49 C50 1.381(4) . ?
C49 H49 0.9500 . ?
C50 C51 1.370(4) . ?
C50 H50 0.9500 . ?
C51 H51 0.9500 . ?
C52 H52A 0.9800 . ?
C52 H52B 0.9800 . ?
C52 H52C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 V1 O5 107.44(8) . . ?
O1 V1 O3 108.54(8) . . ?
O5 V1 O3 143.72(7) . . ?
O1 V1 O4 108.48(8) . . ?
O5 V1 O4 89.99(7) . . ?
O3 V1 O4 74.41(7) . . ?
O1 V1 N1 98.89(8) . . ?
O5 V1 N1 86.40(7) . . ?
O3 V1 N1 92.56(7) . . ?
O4 V1 N1 152.19(7) . . ?
O2 V2 O6 113.14(8) . . ?
O2 V2 O3 115.96(8) . . ?
O6 V2 O3 130.65(7) . . ?
O2 V2 O4 104.33(8) . . ?
O6 V2 O4 88.88(7) . . ?
O3 V2 O4 74.82(7) . . ?
O2 V2 N2 100.36(8) . . ?
O6 V2 N2 86.55(7) . . ?
O3 V2 N2 89.45(7) . . ?
O4 V2 N2 154.68(7) . . ?
C10 O6 V2 137.07(14) . . ?
C26 O4 V1 128.66(13) . . ?
C26 O4 V2 122.82(13) . . ?
V1 O4 V2 104.41(7) . . ?
V2 O3 V1 105.77(7) . . ?
V2 O3 H3A 127.1 . . ?
V1 O3 H3A 127.1 . . ?
C37 O5 V1 130.17(14) . . ?
C47 O7 C52 117.52(18) . . ?
C19 O8 C21 118.7(2) . . ?
C11 N2 C12 117.06(18) . . ?
C11 N2 V2 125.26(15) . . ?
C12 N2 V2 117.68(14) . . ?
C39 N1 C40 115.98(18) . . ?
C39 N1 V1 122.02(15) . . ?
C40 N1 V1 121.96(13) . . ?
C4 C1 H1A 109.5 . . ?
C4 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
C4 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C4 C2 H2A 109.5 . . ?
C4 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
C4 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
C4 C3 H111 109.5 . . ?
C4 C3 H3B 109.5 . . ?
H111 C3 H3B 109.5 . . ?
C4 C3 H3C 109.5 . . ?
H111 C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
C2 C4 C5 107.96(18) . . ?
C2 C4 C3 107.38(19) . . ?
C5 C4 C3 112.0(2) . . ?
C2 C4 C1 111.5(2) . . ?
C5 C4 C1 111.14(18) . . ?
C3 C4 C1 106.79(19) . . ?
C6 C5 C10 117.0(2) . . ?
C6 C5 C4 122.2(2) . . ?
C10 C5 C4 120.7(2) . . ?
C5 C6 C7 123.5(2) . . ?
C5 C6 H6 118.3 . . ?
C7 C6 H6 118.3 . . ?
C8 C7 C6 119.5(2) . . ?
C8 C7 H7 120.2 . . ?
C6 C7 H7 120.2 . . ?
C7 C8 C9 120.0(2) . . ?
C7 C8 H8 120.0 . . ?
C9 C8 H8 120.0 . . ?
C8 C9 C10 120.2(2) . . ?
C8 C9 C11 117.4(2) . . ?
C10 C9 C11 122.4(2) . . ?
O6 C10 C9 120.55(19) . . ?
O6 C10 C5 119.74(19) . . ?
C9 C10 C5 119.7(2) . . ?
N2 C11 C9 127.7(2) . . ?
N2 C11 H11 116.2 . . ?
C9 C11 H11 116.2 . . ?
C13 C12 C17 120.1(2) . . ?
C13 C12 N2 118.4(2) . . ?
C17 C12 N2 121.3(2) . . ?
C14 C13 C12 120.3(2) . . ?
C14 C13 H13 119.8 . . ?
C12 C13 H13 119.8 . . ?
C15 C14 C13 120.0(2) . . ?
C15 C14 H14 120.0 . . ?
C13 C14 H14 120.0 . . ?
C14 C15 C16 120.1(2) . . ?
C14 C15 H15 120.0 . . ?
C16 C15 H15 120.0 . . ?
C15 C16 C17 121.4(2) . . ?
C15 C16 H16 119.3 . . ?
C17 C16 H16 119.3 . . ?
C16 C17 C12 118.2(2) . . ?
C16 C17 C18 119.4(2) . . ?
C12 C17 C18 122.4(2) . . ?
C25 C18 C19 118.8(3) . . ?
C25 C18 C17 121.0(2) . . ?
C19 C18 C17 120.2(2) . . ?
O8 C19 C22 124.4(3) . . ?
O8 C19 C18 114.4(2) . . ?
C22 C19 C18 121.2(3) . . ?
O8 C21 H21A 109.5 . . ?
O8 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
O8 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C19 C22 C23 119.3(3) . . ?
C19 C22 H22 120.4 . . ?
C23 C22 H22 120.4 . . ?
C22 C23 C24 121.3(3) . . ?
C22 C23 H23 119.4 . . ?
C24 C23 H23 119.4 . . ?
C23 C24 C25 119.3(3) . . ?
C23 C24 H24 120.3 . . ?
C25 C24 H24 120.3 . . ?
C18 C25 C24 120.2(3) . . ?
C18 C25 H25 119.9 . . ?
C24 C25 H25 119.9 . . ?
O4 C26 C27 112.1(2) . . ?
O4 C26 H26A 109.2 . . ?
C27 C26 H26A 109.2 . . ?
O4 C26 H26B 109.2 . . ?
C27 C26 H26B 109.2 . . ?
H26A C26 H26B 107.9 . . ?
C26 C27 C28 112.9(3) . . ?
C26 C27 H27A 109.0 . . ?
C28 C27 H27A 109.0 . . ?
C26 C27 H27B 109.0 . . ?
C28 C27 H27B 109.0 . . ?
H27A C27 H27B 107.8 . . ?
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 . . ?
C32 C29 H29A 109.5 . . ?
C32 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C32 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C32 C30 H30A 109.5 . . ?
C32 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C32 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C32 C31 H31A 109.5 . . ?
C32 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C32 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C30 C32 C33 109.1(2) . . ?
C30 C32 C29 111.6(3) . . ?
C33 C32 C29 110.7(2) . . ?
C30 C32 C31 107.2(3) . . ?
C33 C32 C31 111.3(3) . . ?
C29 C32 C31 106.9(3) . . ?
C34 C33 C37 116.6(2) . . ?
C34 C33 C32 122.2(2) . . ?
C37 C33 C32 121.2(2) . . ?
C35 C34 C33 124.1(2) . . ?
C35 C34 H34 117.9 . . ?
C33 C34 H34 117.9 . . ?
C36 C35 C34 119.1(2) . . ?
C36 C35 H35 120.4 . . ?
C34 C35 H35 120.4 . . ?
C35 C36 C38 119.9(2) . . ?
C35 C36 H36 120.1 . . ?
C38 C36 H36 120.1 . . ?
O5 C37 C38 121.1(2) . . ?
O5 C37 C33 119.9(2) . . ?
C38 C37 C33 119.0(2) . . ?
C36 C38 C37 120.9(2) . . ?
C36 C38 C39 117.0(2) . . ?
C37 C38 C39 121.8(2) . . ?
N1 C39 C38 127.5(2) . . ?
N1 C39 H39 116.3 . . ?
C38 C39 H39 116.3 . . ?
C41 C40 C45 120.6(2) . . ?
C41 C40 N1 119.1(2) . . ?
C45 C40 N1 120.27(19) . . ?
C42 C41 C40 119.9(2) . . ?
C42 C41 H41 120.0 . . ?
C40 C41 H41 120.0 . . ?
C43 C42 C41 119.9(2) . . ?
C43 C42 H42 120.0 . . ?
C41 C42 H42 120.0 . . ?
C44 C43 C42 120.4(2) . . ?
C44 C43 H43 119.8 . . ?
C42 C43 H43 119.8 . . ?
C43 C44 C45 121.1(3) . . ?
C43 C44 H44 119.4 . . ?
C45 C44 H44 119.4 . . ?
C40 C45 C44 117.9(2) . . ?
C40 C45 C46 122.0(2) . . ?
C44 C45 C46 120.1(2) . . ?
C48 C46 C47 118.4(2) . . ?
C48 C46 C45 120.3(2) . . ?
C47 C46 C45 121.3(2) . . ?
O7 C47 C49 123.4(2) . . ?
O7 C47 C46 115.9(2) . . ?
C49 C47 C46 120.6(2) . . ?
C51 C48 C46 121.1(2) . . ?
C51 C48 H48 119.5 . . ?
C46 C48 H48 119.5 . . ?
C50 C49 C47 119.3(2) . . ?
C50 C49 H49 120.3 . . ?
C47 C49 H49 120.3 . . ?
C51 C50 C49 121.1(3) . . ?
C51 C50 H50 119.5 . . ?
C49 C50 H50 119.5 . . ?
C50 C51 C48 119.5(2) . . ?
C50 C51 H51 120.2 . . ?
C48 C51 H51 120.2 . . ?
O7 C52 H52A 109.5 . . ?
O7 C52 H52B 109.5 . . ?
H52A C52 H52B 109.5 . . ?
O7 C52 H52C 109.5 . . ?
H52A C52 H52C 109.5 . . ?
H52B C52 H52C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O2 V2 O6 C10 92.4(2) . . . . ?
O3 V2 O6 C10 -93.7(2) . . . . ?
O4 V2 O6 C10 -162.5(2) . . . . ?
N2 V2 O6 C10 -7.4(2) . . . . ?
O1 V1 O4 C26 -58.4(2) . . . . ?
O5 V1 O4 C26 50.03(19) . . . . ?
O3 V1 O4 C26 -163.15(19) . . . . ?
N1 V1 O4 C26 132.29(19) . . . . ?
O1 V1 O4 V2 98.87(9) . . . . ?
O5 V1 O4 V2 -152.71(8) . . . . ?
O3 V1 O4 V2 -5.89(7) . . . . ?
N1 V1 O4 V2 -70.45(16) . . . . ?
O2 V2 O4 C26 51.40(18) . . . . ?
O6 V2 O4 C26 -62.23(17) . . . . ?
O3 V2 O4 C26 164.90(18) . . . . ?
N2 V2 O4 C26 -141.73(18) . . . . ?
O2 V2 O4 V1 -107.55(9) . . . . ?
O6 V2 O4 V1 138.82(8) . . . . ?
O3 V2 O4 V1 5.95(7) . . . . ?
N2 V2 O4 V1 59.32(19) . . . . ?
O2 V2 O3 V1 92.81(9) . . . . ?
O6 V2 O3 V1 -80.95(10) . . . . ?
O4 V2 O3 V1 -6.00(7) . . . . ?
N2 V2 O3 V1 -165.93(8) . . . . ?
O1 V1 O3 V2 -98.66(9) . . . . ?
O5 V1 O3 V2 73.68(13) . . . . ?
O4 V1 O3 V2 6.03(7) . . . . ?
N1 V1 O3 V2 161.08(8) . . . . ?
O1 V1 O5 C37 -64.3(2) . . . . ?
O3 V1 O5 C37 123.37(19) . . . . ?
O4 V1 O5 C37 -173.7(2) . . . . ?
N1 V1 O5 C37 33.9(2) . . . . ?
O2 V2 N2 C11 -105.91(19) . . . . ?
O6 V2 N2 C11 7.00(18) . . . . ?
O3 V2 N2 C11 137.78(18) . . . . ?
O4 V2 N2 C11 87.0(2) . . . . ?
O2 V2 N2 C12 74.91(16) . . . . ?
O6 V2 N2 C12 -172.18(15) . . . . ?
O3 V2 N2 C12 -41.40(15) . . . . ?
O4 V2 N2 C12 -92.2(2) . . . . ?
O1 V1 N1 C39 78.81(19) . . . . ?
O5 V1 N1 C39 -28.29(18) . . . . ?
O3 V1 N1 C39 -171.97(18) . . . . ?
O4 V1 N1 C39 -111.4(2) . . . . ?
O1 V1 N1 C40 -99.00(17) . . . . ?
O5 V1 N1 C40 153.90(17) . . . . ?
O3 V1 N1 C40 10.22(16) . . . . ?
O4 V1 N1 C40 70.8(2) . . . . ?
C2 C4 C5 C6 -111.7(2) . . . . ?
C3 C4 C5 C6 6.3(3) . . . . ?
C1 C4 C5 C6 125.6(2) . . . . ?
C2 C4 C5 C10 65.2(2) . . . . ?
C3 C4 C5 C10 -176.8(2) . . . . ?
C1 C4 C5 C10 -57.5(3) . . . . ?
C10 C5 C6 C7 1.1(3) . . . . ?
C4 C5 C6 C7 178.1(2) . . . . ?
C5 C6 C7 C8 -1.2(4) . . . . ?
C6 C7 C8 C9 0.4(4) . . . . ?
C7 C8 C9 C10 0.5(4) . . . . ?
C7 C8 C9 C11 179.7(2) . . . . ?
V2 O6 C10 C9 5.1(3) . . . . ?
V2 O6 C10 C5 -174.84(14) . . . . ?
C8 C9 C10 O6 179.3(2) . . . . ?
C11 C9 C10 O6 0.2(3) . . . . ?
C8 C9 C10 C5 -0.7(3) . . . . ?
C11 C9 C10 C5 -179.8(2) . . . . ?
C6 C5 C10 O6 179.88(19) . . . . ?
C4 C5 C10 O6 2.8(3) . . . . ?
C6 C5 C10 C9 -0.1(3) . . . . ?
C4 C5 C10 C9 -177.13(19) . . . . ?
C12 N2 C11 C9 173.5(2) . . . . ?
V2 N2 C11 C9 -5.7(3) . . . . ?
C8 C9 C11 N2 -178.4(2) . . . . ?
C10 C9 C11 N2 0.8(4) . . . . ?
C11 N2 C12 C13 130.7(2) . . . . ?
V2 N2 C12 C13 -50.0(2) . . . . ?
C11 N2 C12 C17 -53.3(3) . . . . ?
V2 N2 C12 C17 125.97(18) . . . . ?
C17 C12 C13 C14 0.7(3) . . . . ?
N2 C12 C13 C14 176.8(2) . . . . ?
C12 C13 C14 C15 -0.4(4) . . . . ?
C13 C14 C15 C16 -0.2(4) . . . . ?
C14 C15 C16 C17 0.4(4) . . . . ?
C15 C16 C17 C12 -0.1(3) . . . . ?
C15 C16 C17 C18 -178.7(2) . . . . ?
C13 C12 C17 C16 -0.4(3) . . . . ?
N2 C12 C17 C16 -176.39(19) . . . . ?
C13 C12 C17 C18 178.1(2) . . . . ?
N2 C12 C17 C18 2.2(3) . . . . ?
C16 C17 C18 C25 95.1(3) . . . . ?
C12 C17 C18 C25 -83.4(3) . . . . ?
C16 C17 C18 C19 -82.7(3) . . . . ?
C12 C17 C18 C19 98.7(3) . . . . ?
C21 O8 C19 C22 0.0(4) . . . . ?
C21 O8 C19 C18 -179.4(3) . . . . ?
C25 C18 C19 O8 178.9(2) . . . . ?
C17 C18 C19 O8 -3.2(3) . . . . ?
C25 C18 C19 C22 -0.5(4) . . . . ?
C17 C18 C19 C22 177.4(2) . . . . ?
O8 C19 C22 C23 -179.4(3) . . . . ?
C18 C19 C22 C23 -0.1(4) . . . . ?
C19 C22 C23 C24 0.9(5) . . . . ?
C22 C23 C24 C25 -1.1(6) . . . . ?
C19 C18 C25 C24 0.3(4) . . . . ?
C17 C18 C25 C24 -177.6(3) . . . . ?
C23 C24 C25 C18 0.5(5) . . . . ?
V1 O4 C26 C27 63.9(3) . . . . ?
V2 O4 C26 C27 -89.7(2) . . . . ?
O4 C26 C27 C28 -177.7(2) . . . . ?
C30 C32 C33 C34 109.4(3) . . . . ?
C29 C32 C33 C34 -127.4(3) . . . . ?
C31 C32 C33 C34 -8.7(4) . . . . ?
C30 C32 C33 C37 -69.3(3) . . . . ?
C29 C32 C33 C37 53.8(3) . . . . ?
C31 C32 C33 C37 172.5(3) . . . . ?
C37 C33 C34 C35 -1.7(4) . . . . ?
C32 C33 C34 C35 179.5(3) . . . . ?
C33 C34 C35 C36 -3.9(4) . . . . ?
C34 C35 C36 C38 4.0(4) . . . . ?
V1 O5 C37 C38 -20.1(3) . . . . ?
V1 O5 C37 C33 162.25(17) . . . . ?
C34 C33 C37 O5 -175.3(2) . . . . ?
C32 C33 C37 O5 3.5(4) . . . . ?
C34 C33 C37 C38 6.9(4) . . . . ?
C32 C33 C37 C38 -174.2(2) . . . . ?
C35 C36 C38 C37 1.4(4) . . . . ?
C35 C36 C38 C39 -172.0(2) . . . . ?
O5 C37 C38 C36 175.3(2) . . . . ?
C33 C37 C38 C36 -7.0(4) . . . . ?
O5 C37 C38 C39 -11.6(3) . . . . ?
C33 C37 C38 C39 166.1(2) . . . . ?
C40 N1 C39 C38 -170.1(2) . . . . ?
V1 N1 C39 C38 12.0(3) . . . . ?
C36 C38 C39 N1 -172.4(2) . . . . ?
C37 C38 C39 N1 14.2(4) . . . . ?
C39 N1 C40 C41 -118.9(2) . . . . ?
V1 N1 C40 C41 59.1(2) . . . . ?
C39 N1 C40 C45 61.9(3) . . . . ?
V1 N1 C40 C45 -120.17(19) . . . . ?
C45 C40 C41 C42 -0.7(3) . . . . ?
N1 C40 C41 C42 -179.9(2) . . . . ?
C40 C41 C42 C43 0.3(4) . . . . ?
C41 C42 C43 C44 -0.7(4) . . . . ?
C42 C43 C44 C45 1.4(4) . . . . ?
C41 C40 C45 C44 1.4(3) . . . . ?
N1 C40 C45 C44 -179.4(2) . . . . ?
C41 C40 C45 C46 -178.3(2) . . . . ?
N1 C40 C45 C46 0.9(3) . . . . ?
C43 C44 C45 C40 -1.7(4) . . . . ?
C43 C44 C45 C46 177.9(2) . . . . ?
C40 C45 C46 C48 -120.9(3) . . . . ?
C44 C45 C46 C48 59.4(3) . . . . ?
C40 C45 C46 C47 58.3(3) . . . . ?
C44 C45 C46 C47 -121.4(3) . . . . ?
C52 O7 C47 C49 -9.7(4) . . . . ?
C52 O7 C47 C46 169.3(2) . . . . ?
C48 C46 C47 O7 -178.8(2) . . . . ?
C45 C46 C47 O7 2.0(3) . . . . ?
C48 C46 C47 C49 0.2(4) . . . . ?
C45 C46 C47 C49 -179.0(2) . . . . ?
C47 C46 C48 C51 -1.6(4) . . . . ?
C45 C46 C48 C51 177.6(3) . . . . ?
O7 C47 C49 C50 -179.9(2) . . . . ?
C46 C47 C49 C50 1.1(4) . . . . ?
C47 C49 C50 C51 -1.2(4) . . . . ?
C49 C50 C51 C48 -0.2(5) . . . . ?
C46 C48 C51 C50 1.7(5) . . . . ?

_diffrn_measured_fraction_theta_max 0.990
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.990
_refine_diff_density_max         0.324
_refine_diff_density_min         -0.303
_refine_diff_density_rms         0.057




_database_code_depnum_ccdc_archive 'CCDC 980013'
