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

#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_1


_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C19 H17 N2 O6 V'
_chemical_formula_sum            'C19 H17 N2 O6 V'
_chemical_formula_weight         420.29

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

_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                   11.41(3)
_cell_length_b                   11.09(3)
_cell_length_c                   14.77(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 92.95(4)
_cell_angle_gamma                90.00
_cell_volume                     1866(8)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    3169
_cell_measurement_theta_min      2.30
_cell_measurement_theta_max      23.94

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.18
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.496
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             864
_exptl_absorpt_coefficient_mu    0.571
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.851
_exptl_absorpt_correction_T_max  0.904
_exptl_absorpt_process_details   'SADABS; BRUKER, 2008'

_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  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            21335
_diffrn_reflns_av_R_equivalents  0.0614
_diffrn_reflns_av_sigmaI/netI    0.0396
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         1.79
_diffrn_reflns_theta_max         25.90
_reflns_number_total             3518
_reflns_number_gt                2394
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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)+(0.0728P)²+1.4480P] 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         3518
_refine_ls_number_parameters     256
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0736
_refine_ls_R_factor_gt           0.0466
_refine_ls_wR_factor_ref         0.1469
_refine_ls_wR_factor_gt          0.1240
_refine_ls_goodness_of_fit_ref   1.032
_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
V V 0.22200(5) 0.20686(5) 0.95363(3) 0.0425(2) Uani 1 1 d . . .
O4 O 0.1278(2) 0.2117(2) 0.85039(14) 0.0438(5) Uani 1 1 d . . .
O5 O 0.0637(2) 0.3080(2) 1.01085(15) 0.0517(6) Uani 1 1 d . . .
O3 O 0.2639(2) 0.3717(2) 0.92988(14) 0.0498(6) Uani 1 1 d . . .
O2 O 0.1559(2) 0.0894(2) 1.02375(16) 0.0529(6) Uani 1 1 d . . .
O1 O 0.3268(2) 0.1285(2) 0.92140(15) 0.0538(6) Uani 1 1 d . . .
O6 O 0.4248(3) 0.5842(3) 1.1333(2) 0.0901(10) Uani 1 1 d . . .
H6 H 0.4181 0.5106 1.1320 0.135 Uiso 1 1 calc R . .
N2 N 0.3335(2) 0.3843(3) 1.07582(18) 0.0479(7) Uani 1 1 d . . .
N1 N 0.3022(2) 0.2636(3) 1.07163(18) 0.0452(7) Uani 1 1 d . . .
C11 C 0.0470(3) 0.2878(3) 0.8144(2) 0.0403(7) Uani 1 1 d . . .
C16 C 0.0291(3) 0.2905(4) 0.7219(2) 0.0525(9) Uani 1 1 d . . .
H16 H 0.0738 0.2413 0.6861 0.063 Uiso 1 1 calc R . .
C15 C -0.0526(4) 0.3637(4) 0.6824(2) 0.0654(11) Uani 1 1 d . . .
H15 H -0.0626 0.3651 0.6195 0.078 Uiso 1 1 calc R . .
C14 C -0.1221(4) 0.4370(4) 0.7331(3) 0.0673(11) Uani 1 1 d . . .
H14 H -0.1781 0.4874 0.7050 0.081 Uiso 1 1 calc R . .
C13 C -0.1068(3) 0.4337(3) 0.8256(3) 0.0581(10) Uani 1 1 d . . .
H13 H -0.1541 0.4809 0.8609 0.070 Uiso 1 1 calc R . .
C12 C -0.0213(3) 0.3607(3) 0.8671(2) 0.0416(8) Uani 1 1 d . . .
C17 C -0.0112(3) 0.3578(3) 0.9639(2) 0.0495(8) Uani 1 1 d . . .
H17 H -0.0686 0.3988 0.9940 0.059 Uiso 1 1 calc R . .
C10 C 0.3080(4) 0.6126(4) 0.9006(3) 0.0712(12) Uani 1 1 d . . .
H10 H 0.2705 0.5671 0.8548 0.085 Uiso 1 1 calc R . .
C9 C 0.3326(5) 0.7330(5) 0.8859(5) 0.0934(17) Uani 1 1 d . . .
H9 H 0.3126 0.7687 0.8303 0.112 Uiso 1 1 calc R . .
C8 C 0.3876(5) 0.7996(5) 0.9553(6) 0.099(2) Uani 1 1 d . . .
H8 H 0.4044 0.8806 0.9459 0.119 Uiso 1 1 calc R . .
C7 C 0.4171(4) 0.7489(5) 1.0361(5) 0.0923(17) Uani 1 1 d . . .
H7 H 0.4534 0.7954 1.0818 0.111 Uiso 1 1 calc R . .
C6 C 0.3943(4) 0.6293(4) 1.0520(4) 0.0699(12) Uani 1 1 d . . .
C5 C 0.3388(3) 0.5595(3) 0.9834(3) 0.0538(9) Uani 1 1 d . . .
C4 C 0.3121(3) 0.4330(3) 0.9969(2) 0.0457(8) Uani 1 1 d . . .
C18 C 0.3943(4) 0.2509(5) 1.2227(3) 0.0760(13) Uani 1 1 d . . .
H18A H 0.4686 0.2810 1.2049 0.114 Uiso 1 1 calc R . .
H18C H 0.4070 0.1903 1.2686 0.114 Uiso 1 1 calc R . .
H18B H 0.3494 0.3160 1.2462 0.114 Uiso 1 1 calc R . .
C3 C 0.3294(3) 0.1976(4) 1.1429(2) 0.0491(9) Uani 1 1 d . . .
C2 C 0.2914(4) 0.0759(4) 1.1452(3) 0.0615(10) Uani 1 1 d . . .
H2 H 0.3281 0.0254 1.1881 0.074 Uiso 1 1 calc R . .
C1 C 0.2061(3) 0.0279(4) 1.0898(3) 0.0565(10) Uani 1 1 d . . .
C19 C 0.1547(4) -0.0931(4) 1.1046(3) 0.0772(13) Uani 1 1 d . . .
H19B H 0.0724 -0.0851 1.1136 0.116 Uiso 1 1 calc R . .
H19C H 0.1929 -0.1296 1.1572 0.116 Uiso 1 1 calc R . .
H19A H 0.1657 -0.1429 1.0525 0.116 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
V O1 1.572(3) . ?
V O4 1.820(4) . ?
V O2 1.849(4) . ?
V O3 1.925(5) . ?
V N1 2.026(5) . ?
V O5 2.322(4) . ?
O4 C11 1.339(4) . ?
O5 C17 1.206(4) . ?
O3 C4 1.299(4) . ?
O2 C1 1.299(5) . ?
O6 C6 1.330(6) . ?
O6 H6 0.8200 . ?
N2 C4 1.296(5) . ?
N2 N1 1.386(5) . ?
N1 C3 1.307(5) . ?
C11 C16 1.373(6) . ?
C11 C12 1.389(5) . ?
C16 C15 1.346(6) . ?
C16 H16 0.9300 . ?
C15 C14 1.382(6) . ?
C15 H15 0.9300 . ?
C14 C13 1.368(6) . ?
C14 H14 0.9300 . ?
C13 C12 1.386(5) . ?
C13 H13 0.9300 . ?
C12 C17 1.428(6) . ?
C17 H17 0.9300 . ?
C10 C9 1.383(7) . ?
C10 C5 1.386(6) . ?
C10 H10 0.9300 . ?
C9 C8 1.387(9) . ?
C9 H9 0.9300 . ?
C8 C7 1.346(8) . ?
C8 H8 0.9300 . ?
C7 C6 1.374(7) . ?
C7 H7 0.9300 . ?
C6 C5 1.400(6) . ?
C5 C4 1.452(6) . ?
C18 C3 1.482(6) . ?
C18 H18A 0.9600 . ?
C18 H18C 0.9600 . ?
C18 H18B 0.9600 . ?
C3 C2 1.418(6) . ?
C2 C1 1.348(6) . ?
C2 H2 0.9300 . ?
C1 C19 1.485(6) . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?
C19 H19A 0.9600 . ?

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 V O4 100.85(18) . . ?
O1 V O2 96.8(2) . . ?
O4 V O2 104.46(17) . . ?
O1 V O3 105.66(18) . . ?
O4 V O3 87.74(11) . . ?
O2 V O3 151.98(11) . . ?
O1 V N1 96.62(18) . . ?
O4 V N1 158.77(13) . . ?
O2 V N1 85.19(18) . . ?
O3 V N1 75.93(14) . . ?
O1 V O5 174.54(11) . . ?
O4 V O5 81.60(17) . . ?
O2 V O5 77.81(18) . . ?
O3 V O5 79.22(16) . . ?
N1 V O5 82.08(17) . . ?
C11 O4 V 135.7(2) . . ?
C17 O5 V 123.6(3) . . ?
C4 O3 V 117.2(2) . . ?
C1 O2 V 127.8(3) . . ?
C6 O6 H6 109.5 . . ?
C4 N2 N1 109.0(3) . . ?
C3 N1 N2 117.0(3) . . ?
C3 N1 V 126.7(3) . . ?
N2 N1 V 116.2(2) . . ?
O4 C11 C16 118.2(3) . . ?
O4 C11 C12 122.6(3) . . ?
C16 C11 C12 119.1(3) . . ?
C15 C16 C11 120.6(4) . . ?
C15 C16 H16 119.7 . . ?
C11 C16 H16 119.7 . . ?
C16 C15 C14 121.6(4) . . ?
C16 C15 H15 119.2 . . ?
C14 C15 H15 119.2 . . ?
C13 C14 C15 118.6(4) . . ?
C13 C14 H14 120.7 . . ?
C15 C14 H14 120.7 . . ?
C14 C13 C12 120.5(4) . . ?
C14 C13 H13 119.7 . . ?
C12 C13 H13 119.7 . . ?
C13 C12 C11 119.6(3) . . ?
C13 C12 C17 118.4(3) . . ?
C11 C12 C17 121.9(3) . . ?
O5 C17 C12 127.2(3) . . ?
O5 C17 H17 116.4 . . ?
C12 C17 H17 116.4 . . ?
C9 C10 C5 120.2(5) . . ?
C9 C10 H10 119.9 . . ?
C5 C10 H10 119.9 . . ?
C10 C9 C8 119.1(6) . . ?
C10 C9 H9 120.5 . . ?
C8 C9 H9 120.5 . . ?
C7 C8 C9 121.0(5) . . ?
C7 C8 H8 119.5 . . ?
C9 C8 H8 119.5 . . ?
C8 C7 C6 121.0(6) . . ?
C8 C7 H7 119.5 . . ?
C6 C7 H7 119.5 . . ?
O6 C6 C7 118.3(5) . . ?
O6 C6 C5 122.3(4) . . ?
C7 C6 C5 119.4(5) . . ?
C10 C5 C6 119.3(4) . . ?
C10 C5 C4 119.1(4) . . ?
C6 C5 C4 121.6(4) . . ?
N2 C4 O3 121.3(4) . . ?
N2 C4 C5 119.7(3) . . ?
O3 C4 C5 119.0(3) . . ?
C3 C18 H18A 109.5 . . ?
C3 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
C3 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18C C18 H18B 109.5 . . ?
N1 C3 C2 119.4(3) . . ?
N1 C3 C18 120.4(4) . . ?
C2 C3 C18 120.2(4) . . ?
C1 C2 C3 125.0(4) . . ?
C1 C2 H2 117.5 . . ?
C3 C2 H2 117.5 . . ?
O2 C1 C2 121.7(4) . . ?
O2 C1 C19 114.9(4) . . ?
C2 C1 C19 123.1(4) . . ?
C1 C19 H19B 109.5 . . ?
C1 C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C1 C19 H19A 109.5 . . ?
H19B C19 H19A 109.5 . . ?
H19C C19 H19A 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.982
_diffrn_reflns_theta_full        25.90
_diffrn_measured_fraction_theta_full 0.982
_refine_diff_density_max         1.025
_refine_diff_density_min         -0.675
_refine_diff_density_rms         0.060
_database_code_depnum_ccdc_archive 'CCDC 939296'
#######################################################################
#
#                 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         ?
_chemical_formula_sum            'C24 H19 N2 O6 V'
_chemical_formula_weight         482.35

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           Monoclinic
_symmetry_space_group_name_H-M   'P2(1)/n  '

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                   13.105(7)
_cell_length_b                   8.486(4)
_cell_length_c                   19.710(10)
_cell_angle_alpha                90.00
_cell_angle_beta                 93.973(15)
_cell_angle_gamma                90.00
_cell_volume                     2186.8(19)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    903
_cell_measurement_theta_min      .994
_cell_measurement_theta_max      21.09

_exptl_crystal_description       ?
_exptl_crystal_colour            black
_exptl_crystal_size_max          .18
_exptl_crystal_size_mid          .16
_exptl_crystal_size_min          .10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.465
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             992
_exptl_absorpt_coefficient_mu    0.498
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  .914
_exptl_absorpt_correction_T_max  .951
_exptl_absorpt_process_details   SADABS

_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  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            13796
_diffrn_reflns_av_R_equivalents  0.1533
_diffrn_reflns_av_sigmaI/netI    0.0961
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         1.93
_diffrn_reflns_theta_max         21.09
_reflns_number_total             2367
_reflns_number_gt                1433
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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)+(0.0709P)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     SHELXL
_refine_ls_extinction_coef       0.0049(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         2367
_refine_ls_number_parameters     301
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1101
_refine_ls_R_factor_gt           0.0560
_refine_ls_wR_factor_ref         0.1489
_refine_ls_wR_factor_gt          0.1218
_refine_ls_goodness_of_fit_ref   0.995
_refine_ls_restrained_S_all      0.995
_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
V V 0.22779(8) 0.19401(14) 0.47901(6) 0.0413(5) Uani 1 1 d . . .
C2 C 0.0105(5) 0.3567(8) 0.4171(3) 0.0459(19) Uani 1 1 d . . .
H2 H -0.0504 0.3867 0.3935 0.055 Uiso 1 1 calc R . .
O6 O -0.0234(4) 0.0154(7) 0.6757(3) 0.0745(17) Uani 1 1 d . . .
H6 H -0.0186 0.0653 0.6405 0.112 Uiso 1 1 calc R . .
C6 C 0.0652(6) -0.0591(9) 0.6923(4) 0.051(2) Uani 1 1 d . . .
O4 O 0.3679(3) 0.2000(5) 0.4787(2) 0.0449(12) Uani 1 1 d . . .
C4 C 0.1507(6) 0.0662(8) 0.5961(3) 0.0455(19) Uani 1 1 d . . .
O5 O 0.2569(4) 0.4065(6) 0.5513(2) 0.0523(14) Uani 1 1 d . . .
C18 C -0.1008(4) 0.2719(8) 0.5087(3) 0.0472(19) Uani 1 1 d . . .
H18A H -0.1224 0.1640 0.5106 0.071 Uiso 1 1 calc R . .
H18B H -0.1491 0.3307 0.4800 0.071 Uiso 1 1 calc R . .
H18C H -0.0969 0.3160 0.5537 0.071 Uiso 1 1 calc R . .
O2 O 0.1871(3) 0.3570(5) 0.4206(2) 0.0465(13) Uani 1 1 d . . .
C21 C 0.1897(7) 0.4833(11) 0.2179(4) 0.080(3) Uani 1 1 d . . .
H21 H 0.2443 0.4564 0.1925 0.096 Uiso 1 1 calc R . .
C1 C 0.0979(5) 0.3903(8) 0.3880(3) 0.0422(18) Uani 1 1 d . . .
C19 C 0.1037(5) 0.4615(8) 0.3212(3) 0.0447(19) Uani 1 1 d . . .
C20 C 0.1850(6) 0.4244(9) 0.2818(4) 0.062(2) Uani 1 1 d . . .
H20 H 0.2367 0.3583 0.2996 0.074 Uiso 1 1 calc R . .
C23 C 0.0340(6) 0.6232(10) 0.2293(4) 0.079(3) Uani 1 1 d . . .
H23 H -0.0169 0.6911 0.2118 0.095 Uiso 1 1 calc R . .
C24 C 0.0305(6) 0.5625(10) 0.2940(4) 0.066(2) Uani 1 1 d . . .
H24A H -0.0233 0.5911 0.3199 0.079 Uiso 1 1 calc R . .
C22 C 0.1147(7) 0.5820(11) 0.1905(4) 0.082(3) Uani 1 1 d . . .
H22 H 0.1177 0.6208 0.1465 0.098 Uiso 1 1 calc R . .
C3 C 0.0028(5) 0.2800(8) 0.4804(3) 0.0397(17) Uani 1 1 d . . .
N1 N 0.0819(4) 0.2142(6) 0.5119(3) 0.0375(14) Uani 1 1 d . . .
N2 N 0.0670(4) 0.1377(6) 0.5729(3) 0.0452(15) Uani 1 1 d . . .
C5 C 0.1517(5) -0.0376(8) 0.6551(3) 0.0424(18) Uani 1 1 d . . .
C7 C 0.0679(6) -0.1641(9) 0.7454(3) 0.058(2) Uani 1 1 d . . .
H7 H 0.0093 -0.1809 0.7684 0.070 Uiso 1 1 calc R . .
C9 C 0.2412(7) -0.2242(10) 0.7286(4) 0.077(3) Uani 1 1 d . . .
H9 H 0.3005 -0.2805 0.7408 0.092 Uiso 1 1 calc R . .
C10 C 0.2391(6) -0.1215(9) 0.6747(4) 0.062(2) Uani 1 1 d . . .
H10 H 0.2975 -0.1082 0.6511 0.075 Uiso 1 1 calc R . .
C8 C 0.1556(7) -0.2440(10) 0.7648(4) 0.073(3) Uani 1 1 d . . .
H8 H 0.1576 -0.3114 0.8021 0.087 Uiso 1 1 calc R . .
O1 O 0.2020(3) 0.0517(5) 0.4290(2) 0.0508(13) Uani 1 1 d . . .
C17 C 0.3396(6) 0.4497(9) 0.5760(3) 0.053(2) Uani 1 1 d . . .
H17 H 0.3400 0.5345 0.6059 0.064 Uiso 1 1 calc R . .
C11 C 0.4480(5) 0.2598(9) 0.5162(4) 0.046(2) Uani 1 1 d . . .
C12 C 0.4388(5) 0.3805(9) 0.5631(4) 0.0471(19) Uani 1 1 d . . .
C16 C 0.5435(6) 0.1955(9) 0.5053(4) 0.064(2) Uani 1 1 d . . .
H16 H 0.5501 0.1153 0.4737 0.077 Uiso 1 1 calc R . .
C13 C 0.5273(7) 0.4383(10) 0.5986(4) 0.070(2) Uani 1 1 d . . .
H13 H 0.5224 0.5208 0.6293 0.084 Uiso 1 1 calc R . .
C15 C 0.6272(7) 0.2542(12) 0.5424(6) 0.086(3) Uani 1 1 d . . .
H15 H 0.6910 0.2108 0.5360 0.103 Uiso 1 1 calc R . .
C14 C 0.6209(7) 0.3741(13) 0.5884(5) 0.087(3) Uani 1 1 d . . .
H14 H 0.6795 0.4115 0.6124 0.105 Uiso 1 1 calc R . .
O3 O 0.2354(3) 0.0851(5) 0.5643(2) 0.0453(13) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
V O1 1.580(4) . ?
V O4 1.838(4) . ?
V O2 1.855(4) . ?
V O3 1.916(4) . ?
V N1 2.069(5) . ?
V O5 2.314(5) . ?
C2 C1 1.348(8) . ?
C2 C3 1.417(8) . ?
O6 C6 1.342(8) . ?
C6 C7 1.372(9) . ?
C6 C5 1.404(9) . ?
O4 C11 1.341(7) . ?
C4 N2 1.309(8) . ?
C4 O3 1.321(7) . ?
C4 C5 1.459(9) . ?
O5 C17 1.214(7) . ?
C18 C3 1.504(8) . ?
O2 C1 1.324(7) . ?
C21 C20 1.361(9) . ?
C21 C22 1.374(11) . ?
C1 C19 1.455(8) . ?
C19 C24 1.368(9) . ?
C19 C20 1.397(9) . ?
C23 C24 1.378(9) . ?
C23 C22 1.392(10) . ?
C3 N1 1.297(7) . ?
N1 N2 1.392(6) . ?
C5 C10 1.381(9) . ?
C7 C8 1.366(10) . ?
C9 C10 1.373(9) . ?
C9 C8 1.380(10) . ?
C17 C12 1.465(9) . ?
C11 C12 1.391(9) . ?
C11 C16 1.395(9) . ?
C12 C13 1.401(9) . ?
C16 C15 1.369(11) . ?
C13 C14 1.371(11) . ?
C15 C14 1.370(11) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 V O4 100.9(2) . . ?
O1 V O2 98.2(2) . . ?
O4 V O2 102.79(19) . . ?
O1 V O3 100.0(2) . . ?
O4 V O3 91.45(18) . . ?
O2 V O3 154.22(19) . . ?
O1 V N1 95.5(2) . . ?
O4 V N1 160.9(2) . . ?
O2 V N1 84.3(2) . . ?
O3 V N1 76.0(2) . . ?
O1 V O5 177.0(2) . . ?
O4 V O5 81.88(18) . . ?
O2 V O5 80.17(18) . . ?
O3 V O5 80.74(18) . . ?
N1 V O5 81.87(18) . . ?
C1 C2 C3 125.9(7) . . ?
O6 C6 C7 117.8(7) . . ?
O6 C6 C5 121.8(7) . . ?
C7 C6 C5 120.3(7) . . ?
C11 O4 V 138.8(4) . . ?
N2 C4 O3 119.4(6) . . ?
N2 C4 C5 121.3(7) . . ?
O3 C4 C5 119.3(7) . . ?
C17 O5 V 125.9(5) . . ?
C1 O2 V 131.8(4) . . ?
C20 C21 C22 120.7(8) . . ?
O2 C1 C2 119.8(6) . . ?
O2 C1 C19 115.3(6) . . ?
C2 C1 C19 124.9(7) . . ?
C24 C19 C20 117.7(7) . . ?
C24 C19 C1 122.4(7) . . ?
C20 C19 C1 119.9(7) . . ?
C21 C20 C19 121.2(8) . . ?
C24 C23 C22 119.4(8) . . ?
C19 C24 C23 121.9(8) . . ?
C21 C22 C23 119.1(8) . . ?
N1 C3 C2 121.1(6) . . ?
N1 C3 C18 121.0(6) . . ?
C2 C3 C18 117.9(6) . . ?
C3 N1 N2 117.3(5) . . ?
C3 N1 V 127.7(4) . . ?
N2 N1 V 114.8(4) . . ?
C4 N2 N1 110.7(5) . . ?
C10 C5 C6 118.0(7) . . ?
C10 C5 C4 119.7(7) . . ?
C6 C5 C4 122.2(7) . . ?
C8 C7 C6 120.8(7) . . ?
C10 C9 C8 120.2(8) . . ?
C9 C10 C5 121.1(7) . . ?
C7 C8 C9 119.5(7) . . ?
O5 C17 C12 126.0(7) . . ?
O4 C11 C12 123.0(6) . . ?
O4 C11 C16 116.3(7) . . ?
C12 C11 C16 120.7(7) . . ?
C11 C12 C13 118.9(7) . . ?
C11 C12 C17 122.0(7) . . ?
C13 C12 C17 119.1(8) . . ?
C15 C16 C11 118.0(8) . . ?
C14 C13 C12 120.4(9) . . ?
C16 C15 C14 122.8(9) . . ?
C15 C14 C13 119.3(9) . . ?
C4 O3 V 118.7(4) . . ?

_diffrn_measured_fraction_theta_max 0.994
_diffrn_reflns_theta_full        21.09
_diffrn_measured_fraction_theta_full 0.994
_refine_diff_density_max         0.343
_refine_diff_density_min         -0.273
_refine_diff_density_rms         0.064
_database_code_depnum_ccdc_archive 'CCDC 939297'
#######################################################################
#
#                 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         'C36 H34 N4 O10 V2'
_chemical_formula_sum            'C36 H34 N4 O10 V2'
_chemical_formula_weight         784.55

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           Orthorhombic
_symmetry_space_group_name_H-M   Pca2(1)
_symmetry_space_group_name_Hall  'P 2c -2ac'

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

_cell_length_a                   18.5154(18)
_cell_length_b                   9.8382(9)
_cell_length_c                   19.301(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     3515.8(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    5504
_cell_measurement_theta_min      2.34
_cell_measurement_theta_max      24.93

_exptl_crystal_description       BLOCK
_exptl_crystal_colour            BLUE
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.21
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.482
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1616
_exptl_absorpt_coefficient_mu    0.596
_exptl_absorpt_correction_type   MULTI-SCAN
_exptl_absorpt_correction_T_min  0.836
_exptl_absorpt_correction_T_max  0.882
_exptl_absorpt_process_details   'SADABS; BRUKER, 2008'

_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  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            14815
_diffrn_reflns_av_R_equivalents  0.0306
_diffrn_reflns_av_sigmaI/netI    0.0389
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         2.07
_diffrn_reflns_theta_max         25.02
_reflns_number_total             5345
_reflns_number_gt                4829
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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)+(0.0364P)²+0.2196P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.006(16)
_refine_ls_number_reflns         5345
_refine_ls_number_parameters     475
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0353
_refine_ls_R_factor_gt           0.0286
_refine_ls_wR_factor_ref         0.0686
_refine_ls_wR_factor_gt          0.0655
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_restrained_S_all      1.030
_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 0.67043(2) 0.30007(4) 0.75032(2) 0.01680(10) Uani 1 1 d . . .
V2 V 0.60646(2) -0.01646(4) 0.74127(2) 0.02024(11) Uani 1 1 d . . .
O1 O 0.71726(10) 0.39654(17) 0.79824(10) 0.0238(4) Uani 1 1 d . . .
O2 O 0.57934(9) 0.37336(17) 0.76943(10) 0.0248(4) Uani 1 1 d . . .
O3 O 0.74836(10) 0.23648(17) 0.69052(10) 0.0242(4) Uani 1 1 d . . .
O5 O 0.77970(11) 0.4113(2) 0.49407(11) 0.0376(5) Uani 1 1 d . . .
H5A H 0.7488 0.4286 0.5232 0.056 Uiso 1 1 calc R . .
O6 O 0.56113(11) -0.11348(18) 0.69195(11) 0.0343(5) Uani 1 1 d . . .
O7 O 0.69883(10) -0.08156(17) 0.72387(10) 0.0276(5) Uani 1 1 d . . .
O8 O 0.52798(10) 0.04118(17) 0.80076(10) 0.0248(4) Uani 1 1 d . . .
O10 O 0.47501(12) -0.1804(3) 0.98023(12) 0.0464(6) Uani 1 1 d . . .
H10A H 0.5080 -0.1923 0.9526 0.070 Uiso 1 1 calc R . .
O9 O 0.60120(9) 0.14433(16) 0.69316(9) 0.0196(4) Uani 1 1 d . . .
O4 O 0.67079(9) 0.14376(16) 0.80199(9) 0.0178(4) Uani 1 1 d . . .
N1 N 0.66368(12) 0.4220(2) 0.66214(12) 0.0223(5) Uani 1 1 d . . .
N2 N 0.71507(12) 0.3961(2) 0.61100(12) 0.0232(5) Uani 1 1 d . . .
N3 N 0.61146(12) -0.1478(2) 0.82620(12) 0.0202(5) Uani 1 1 d . . .
N4 N 0.55689(12) -0.1311(2) 0.87543(12) 0.0262(5) Uani 1 1 d . . .
C12 C 0.46336(16) 0.4368(3) 0.85052(16) 0.0296(7) Uani 1 1 d . . .
H12 H 0.4891 0.3571 0.8584 0.036 Uiso 1 1 calc R . .
C13 C 0.40546(17) 0.4687(3) 0.89253(17) 0.0393(8) Uani 1 1 d . . .
H13 H 0.3927 0.4105 0.9285 0.047 Uiso 1 1 calc R . .
C14 C 0.36636(16) 0.5862(3) 0.88155(18) 0.0364(7) Uani 1 1 d . . .
H14 H 0.3274 0.6078 0.9099 0.044 Uiso 1 1 calc R . .
C15 C 0.38606(16) 0.6710(3) 0.82787(17) 0.0341(8) Uani 1 1 d . . .
H15 H 0.3597 0.7501 0.8201 0.041 Uiso 1 1 calc R . .
C16 C 0.44321(14) 0.6417(3) 0.78598(15) 0.0266(6) Uani 1 1 d . . .
H16 H 0.4558 0.7004 0.7502 0.032 Uiso 1 1 calc R . .
C11 C 0.48331(14) 0.5211(3) 0.79728(14) 0.0205(6) Uani 1 1 d . . .
C1 C 0.54553(12) 0.4862(2) 0.75245(15) 0.0191(5) Uani 1 1 d . . .
C2 C 0.56541(14) 0.5601(3) 0.69578(15) 0.0236(6) Uani 1 1 d . . .
H2 H 0.5399 0.6397 0.6870 0.028 Uiso 1 1 calc R . .
C3 C 0.62155(15) 0.5259(3) 0.64928(15) 0.0230(6) Uani 1 1 d . . .
C17 C 0.63122(17) 0.6105(3) 0.58555(17) 0.0337(8) Uani 1 1 d . . .
H17B H 0.6796 0.6453 0.5842 0.050 Uiso 1 1 calc R . .
H17A H 0.5976 0.6848 0.5863 0.050 Uiso 1 1 calc R . .
H17C H 0.6226 0.5556 0.5453 0.050 Uiso 1 1 calc R . .
C4 C 0.75835(15) 0.3001(2) 0.63180(14) 0.0200(6) Uani 1 1 d . . .
C5 C 0.82134(14) 0.2682(3) 0.58789(15) 0.0200(6) Uani 1 1 d . . .
C10 C 0.87628(15) 0.1847(3) 0.61317(16) 0.0253(6) Uani 1 1 d . . .
H10 H 0.8719 0.1458 0.6569 0.030 Uiso 1 1 calc R . .
C9 C 0.93705(16) 0.1594(3) 0.57385(16) 0.0301(7) Uani 1 1 d . . .
H9 H 0.9733 0.1036 0.5912 0.036 Uiso 1 1 calc R . .
C8 C 0.94437(17) 0.2168(3) 0.50834(16) 0.0299(7) Uani 1 1 d . . .
H8 H 0.9856 0.1996 0.4822 0.036 Uiso 1 1 calc R . .
C7 C 0.89078(16) 0.2991(3) 0.48215(16) 0.0318(7) Uani 1 1 d . . .
H7 H 0.8955 0.3363 0.4381 0.038 Uiso 1 1 calc R . .
C6 C 0.82950(15) 0.3266(3) 0.52167(16) 0.0256(6) Uani 1 1 d . . .
C34 C 0.80619(15) -0.1470(3) 0.63088(14) 0.0224(6) Uani 1 1 d . . .
H34 H 0.7831 -0.0634 0.6275 0.027 Uiso 1 1 calc R . .
C33 C 0.85748(16) -0.1832(3) 0.58239(15) 0.0267(7) Uani 1 1 d . . .
H33 H 0.8687 -0.1234 0.5466 0.032 Uiso 1 1 calc R . .
C32 C 0.89237(15) -0.3067(3) 0.58629(15) 0.0258(6) Uani 1 1 d . . .
H32 H 0.9262 -0.3308 0.5528 0.031 Uiso 1 1 calc R . .
C31 C 0.87680(15) -0.3950(3) 0.64035(16) 0.0253(6) Uani 1 1 d . . .
H31 H 0.9008 -0.4779 0.6435 0.030 Uiso 1 1 calc R . .
C30 C 0.82562(14) -0.3601(3) 0.68969(15) 0.0242(6) Uani 1 1 d . . .
H30 H 0.8156 -0.4194 0.7260 0.029 Uiso 1 1 calc R . .
C29 C 0.78879(14) -0.2357(2) 0.68521(14) 0.0203(6) Uani 1 1 d . . .
C19 C 0.73121(13) -0.1997(2) 0.73502(14) 0.0206(6) Uani 1 1 d . . .
C20 C 0.71152(14) -0.2790(3) 0.78912(13) 0.0214(6) Uani 1 1 d . . .
H20 H 0.7376 -0.3585 0.7961 0.026 Uiso 1 1 calc R . .
C21 C 0.65429(15) -0.2511(3) 0.83637(14) 0.0218(6) Uani 1 1 d . . .
C35 C 0.64441(15) -0.3424(3) 0.89763(15) 0.0253(6) Uani 1 1 d . . .
H35B H 0.6523 -0.2916 0.9394 0.038 Uiso 1 1 calc R . .
H35C H 0.6784 -0.4158 0.8952 0.038 Uiso 1 1 calc R . .
H35A H 0.5962 -0.3782 0.8976 0.038 Uiso 1 1 calc R . .
C22 C 0.51430(15) -0.0315(3) 0.85594(15) 0.0239(6) Uani 1 1 d . . .
C23 C 0.44928(15) -0.0031(3) 0.89770(15) 0.0257(6) Uani 1 1 d . . .
C28 C 0.40208(15) 0.1003(3) 0.87711(17) 0.0297(7) Uani 1 1 d . . .
H28 H 0.4115 0.1483 0.8366 0.036 Uiso 1 1 calc R . .
C27 C 0.34180(17) 0.1325(3) 0.91582(19) 0.0372(8) Uani 1 1 d . . .
H27 H 0.3115 0.2029 0.9020 0.045 Uiso 1 1 calc R . .
C26 C 0.32671(17) 0.0593(4) 0.97531(18) 0.0424(9) Uani 1 1 d . . .
H26 H 0.2859 0.0802 1.0012 0.051 Uiso 1 1 calc R . .
C25 C 0.37146(17) -0.0442(4) 0.99646(18) 0.0422(8) Uani 1 1 d . . .
H25 H 0.3608 -0.0924 1.0366 0.051 Uiso 1 1 calc R . .
C24 C 0.43269(17) -0.0772(3) 0.95810(16) 0.0330(7) Uani 1 1 d . . .
C36 C 0.53929(16) 0.1828(3) 0.65318(15) 0.0286(7) Uani 1 1 d . . .
H36A H 0.5269 0.1106 0.6219 0.043 Uiso 1 1 calc R . .
H36C H 0.5501 0.2635 0.6272 0.043 Uiso 1 1 calc R . .
H36B H 0.4994 0.2002 0.6836 0.043 Uiso 1 1 calc R . .
C18 C 0.71685(15) 0.1109(3) 0.85869(15) 0.0273(6) Uani 1 1 d . . .
H18A H 0.7562 0.0557 0.8426 0.041 Uiso 1 1 calc R . .
H18B H 0.6899 0.0618 0.8930 0.041 Uiso 1 1 calc R . .
H18C H 0.7355 0.1931 0.8787 0.041 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 1.5838(18) . ?
V1 O4 1.8330(17) . ?
V1 O2 1.8709(17) . ?
V1 O3 1.9508(19) . ?
V1 N1 2.086(2) . ?
V1 O9 2.2820(17) . ?
V2 O6 1.5879(19) . ?
V2 O9 1.8369(17) . ?
V2 O7 1.8569(18) . ?
V2 O8 1.9370(19) . ?
V2 N3 2.089(2) . ?
V2 O4 2.2972(18) . ?
O2 C1 1.316(3) . ?
O3 C4 1.308(3) . ?
O5 C6 1.352(3) . ?
O5 H5A 0.8200 . ?
O7 C19 1.326(3) . ?
O8 C22 1.308(3) . ?
O10 C24 1.352(4) . ?
O10 H10A 0.8200 . ?
O9 C36 1.433(3) . ?
O4 C18 1.425(3) . ?
N1 C3 1.310(3) . ?
N1 N2 1.394(3) . ?
N2 C4 1.302(3) . ?
N3 C21 1.304(3) . ?
N3 N4 1.397(3) . ?
N4 C22 1.312(3) . ?
C12 C11 1.372(4) . ?
C12 C13 1.380(4) . ?
C12 H12 0.9300 . ?
C13 C14 1.381(4) . ?
C13 H13 0.9300 . ?
C14 C15 1.379(4) . ?
C14 H14 0.9300 . ?
C15 C16 1.363(4) . ?
C15 H15 0.9300 . ?
C16 C11 1.416(3) . ?
C16 H16 0.9300 . ?
C11 C1 1.481(4) . ?
C1 C2 1.364(4) . ?
C2 C3 1.414(4) . ?
C2 H2 0.9300 . ?
C3 C17 1.496(4) . ?
C17 H17B 0.9600 . ?
C17 H17A 0.9600 . ?
C17 H17C 0.9600 . ?
C4 C5 1.475(4) . ?
C5 C10 1.395(4) . ?
C5 C6 1.410(4) . ?
C10 C9 1.380(4) . ?
C10 H10 0.9300 . ?
C9 C8 1.391(4) . ?
C9 H9 0.9300 . ?
C8 C7 1.377(4) . ?
C8 H8 0.9300 . ?
C7 C6 1.394(4) . ?
C7 H7 0.9300 . ?
C34 C33 1.380(4) . ?
C34 C29 1.401(4) . ?
C34 H34 0.9300 . ?
C33 C32 1.379(4) . ?
C33 H33 0.9300 . ?
C32 C31 1.388(4) . ?
C32 H32 0.9300 . ?
C31 C30 1.387(4) . ?
C31 H31 0.9300 . ?
C30 C29 1.404(4) . ?
C30 H30 0.9300 . ?
C29 C19 1.479(4) . ?
C19 C20 1.353(4) . ?
C20 C21 1.425(4) . ?
C20 H20 0.9300 . ?
C21 C35 1.496(4) . ?
C35 H35B 0.9600 . ?
C35 H35C 0.9600 . ?
C35 H35A 0.9600 . ?
C22 C23 1.476(4) . ?
C23 C28 1.399(4) . ?
C23 C24 1.409(4) . ?
C28 C27 1.380(4) . ?
C28 H28 0.9300 . ?
C27 C26 1.384(5) . ?
C27 H27 0.9300 . ?
C26 C25 1.374(5) . ?
C26 H26 0.9300 . ?
C25 C24 1.392(4) . ?
C25 H25 0.9300 . ?
C36 H36A 0.9600 . ?
C36 H36C 0.9600 . ?
C36 H36B 0.9600 . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?

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 O4 100.54(9) . . ?
O1 V1 O2 98.48(9) . . ?
O4 V1 O2 102.67(8) . . ?
O1 V1 O3 97.63(9) . . ?
O4 V1 O3 92.87(8) . . ?
O2 V1 O3 155.10(9) . . ?
O1 V1 N1 99.49(9) . . ?
O4 V1 N1 157.91(8) . . ?
O2 V1 N1 83.42(9) . . ?
O3 V1 N1 75.28(8) . . ?
O1 V1 O9 172.85(8) . . ?
O4 V1 O9 72.65(7) . . ?
O2 V1 O9 81.24(7) . . ?
O3 V1 O9 85.07(7) . . ?
N1 V1 O9 87.59(8) . . ?
O6 V2 O9 100.75(9) . . ?
O6 V2 O7 99.85(10) . . ?
O9 V2 O7 104.74(8) . . ?
O6 V2 O8 97.75(10) . . ?
O9 V2 O8 90.45(8) . . ?
O7 V2 O8 154.05(9) . . ?
O6 V2 N3 97.01(9) . . ?
O9 V2 N3 158.67(8) . . ?
O7 V2 N3 83.56(8) . . ?
O8 V2 N3 75.47(8) . . ?
O6 V2 O4 172.91(9) . . ?
O9 V2 O4 72.21(7) . . ?
O7 V2 O4 81.45(7) . . ?
O8 V2 O4 83.44(7) . . ?
N3 V2 O4 90.06(7) . . ?
C1 O2 V1 134.82(17) . . ?
C4 O3 V1 117.63(16) . . ?
C6 O5 H5A 109.5 . . ?
C19 O7 V2 133.60(16) . . ?
C22 O8 V2 117.90(17) . . ?
C24 O10 H10A 109.5 . . ?
C36 O9 V2 122.84(16) . . ?
C36 O9 V1 122.16(14) . . ?
V2 O9 V1 107.70(8) . . ?
C18 O4 V1 127.63(16) . . ?
C18 O4 V2 123.14(15) . . ?
V1 O4 V2 107.23(8) . . ?
C3 N1 N2 114.5(2) . . ?
C3 N1 V1 129.7(2) . . ?
N2 N1 V1 115.58(16) . . ?
C4 N2 N1 109.5(2) . . ?
C21 N3 N4 115.4(2) . . ?
C21 N3 V2 128.84(19) . . ?
N4 N3 V2 115.39(15) . . ?
C22 N4 N3 109.1(2) . . ?
C11 C12 C13 120.8(3) . . ?
C11 C12 H12 119.6 . . ?
C13 C12 H12 119.6 . . ?
C12 C13 C14 120.5(3) . . ?
C12 C13 H13 119.7 . . ?
C14 C13 H13 119.7 . . ?
C15 C14 C13 118.9(3) . . ?
C15 C14 H14 120.6 . . ?
C13 C14 H14 120.6 . . ?
C16 C15 C14 121.5(3) . . ?
C16 C15 H15 119.2 . . ?
C14 C15 H15 119.2 . . ?
C15 C16 C11 119.6(3) . . ?
C15 C16 H16 120.2 . . ?
C11 C16 H16 120.2 . . ?
C12 C11 C16 118.7(3) . . ?
C12 C11 C1 120.4(2) . . ?
C16 C11 C1 120.8(2) . . ?
O2 C1 C2 121.4(2) . . ?
O2 C1 C11 114.9(2) . . ?
C2 C1 C11 123.7(2) . . ?
C1 C2 C3 125.5(2) . . ?
C1 C2 H2 117.3 . . ?
C3 C2 H2 117.3 . . ?
N1 C3 C2 120.2(3) . . ?
N1 C3 C17 121.2(3) . . ?
C2 C3 C17 118.5(2) . . ?
C3 C17 H17B 109.5 . . ?
C3 C17 H17A 109.5 . . ?
H17B C17 H17A 109.5 . . ?
C3 C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
N2 C4 O3 121.8(2) . . ?
N2 C4 C5 117.6(2) . . ?
O3 C4 C5 120.5(2) . . ?
C10 C5 C6 118.6(3) . . ?
C10 C5 C4 120.0(2) . . ?
C6 C5 C4 121.2(2) . . ?
C9 C10 C5 120.6(3) . . ?
C9 C10 H10 119.7 . . ?
C5 C10 H10 119.7 . . ?
C10 C9 C8 120.4(3) . . ?
C10 C9 H9 119.8 . . ?
C8 C9 H9 119.8 . . ?
C7 C8 C9 120.1(3) . . ?
C7 C8 H8 119.9 . . ?
C9 C8 H8 119.9 . . ?
C8 C7 C6 120.0(3) . . ?
C8 C7 H7 120.0 . . ?
C6 C7 H7 120.0 . . ?
O5 C6 C7 117.3(3) . . ?
O5 C6 C5 122.4(3) . . ?
C7 C6 C5 120.3(3) . . ?
C33 C34 C29 120.3(2) . . ?
C33 C34 H34 119.8 . . ?
C29 C34 H34 119.8 . . ?
C32 C33 C34 120.8(3) . . ?
C32 C33 H33 119.6 . . ?
C34 C33 H33 119.6 . . ?
C33 C32 C31 119.7(3) . . ?
C33 C32 H32 120.1 . . ?
C31 C32 H32 120.1 . . ?
C30 C31 C32 120.2(3) . . ?
C30 C31 H31 119.9 . . ?
C32 C31 H31 119.9 . . ?
C31 C30 C29 120.4(3) . . ?
C31 C30 H30 119.8 . . ?
C29 C30 H30 119.8 . . ?
C34 C29 C30 118.5(3) . . ?
C34 C29 C19 120.2(2) . . ?
C30 C29 C19 121.2(2) . . ?
O7 C19 C20 120.6(2) . . ?
O7 C19 C29 115.5(2) . . ?
C20 C19 C29 123.9(2) . . ?
C19 C20 C21 125.7(2) . . ?
C19 C20 H20 117.1 . . ?
C21 C20 H20 117.1 . . ?
N3 C21 C20 120.4(3) . . ?
N3 C21 C35 120.8(3) . . ?
C20 C21 C35 118.8(2) . . ?
C21 C35 H35B 109.5 . . ?
C21 C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C21 C35 H35A 109.5 . . ?
H35B C35 H35A 109.5 . . ?
H35C C35 H35A 109.5 . . ?
O8 C22 N4 121.7(3) . . ?
O8 C22 C23 119.9(2) . . ?
N4 C22 C23 118.4(3) . . ?
C28 C23 C24 118.4(3) . . ?
C28 C23 C22 119.5(3) . . ?
C24 C23 C22 122.1(3) . . ?
C27 C28 C23 121.2(3) . . ?
C27 C28 H28 119.4 . . ?
C23 C28 H28 119.4 . . ?
C28 C27 C26 119.5(3) . . ?
C28 C27 H27 120.2 . . ?
C26 C27 H27 120.2 . . ?
C25 C26 C27 120.7(3) . . ?
C25 C26 H26 119.7 . . ?
C27 C26 H26 119.7 . . ?
C26 C25 C24 120.4(3) . . ?
C26 C25 H25 119.8 . . ?
C24 C25 H25 119.8 . . ?
O10 C24 C25 118.6(3) . . ?
O10 C24 C23 121.6(3) . . ?
C25 C24 C23 119.8(3) . . ?
O9 C36 H36A 109.5 . . ?
O9 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
O9 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
H36C C36 H36B 109.5 . . ?
O4 C18 H18A 109.5 . . ?
O4 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
O4 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        25.02
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.263
_refine_diff_density_min         -0.262
_refine_diff_density_rms         0.042
_database_code_depnum_ccdc_archive 'CCDC 972496'
#######################################################################
#
#                 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         ?
_chemical_formula_sum            'C24.50 H24.50 Cl1.50 N4 O9 V2'
_chemical_formula_weight         674.04

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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 '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                   11.8887(9)
_cell_length_b                   13.9072(11)
_cell_length_c                   18.0799(14)
_cell_angle_alpha                108.122(7)
_cell_angle_beta                 93.759(6)
_cell_angle_gamma                90.318(6)
_cell_volume                     2833.8(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    16810
_cell_measurement_theta_min      3.25
_cell_measurement_theta_max      27.50

_exptl_crystal_description       plate
_exptl_crystal_colour            black
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.580
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1372
_exptl_absorpt_coefficient_mu    0.859
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'ABSPACK, Oxford Diffraction Ltd'

_exptl_absorpt_correction_T_min  0.901
_exptl_absorpt_correction_T_max  1.000

_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_standards_number         ?
_diffrn_measurement_device       'Oxford Diffaction X-Calibur System'
_diffrn_measurement_method       '321 frames, counting time 10 s.'
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            16810
_diffrn_reflns_av_R_equivalents  0.0809
_diffrn_reflns_av_sigmaI/netI    0.1815
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         3.25
_diffrn_reflns_theta_max         27.50
_reflns_number_total             12661
_reflns_number_gt                6611
_reflns_threshold_expression     >2sigma(I)


_computing_data_collection       'Crysalis, Oxford Diffraction'
_computing_cell_refinement       'Crysalis, Oxford Diffraction'
_computing_data_reduction        'Crysalis, Oxford Diffraction'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    PLATON(Spek,2004)


_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     
;
  w=1/[σ²(Fo²)+(0.0317P)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         12661
_refine_ls_number_parameters     751
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1763
_refine_ls_R_factor_gt           0.0924
_refine_ls_wR_factor_ref         0.1696
_refine_ls_wR_factor_gt          0.1376
_refine_ls_goodness_of_fit_ref   0.986
_refine_ls_restrained_S_all      0.986
_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
V1A V 0.71163(9) 0.64743(7) 0.38340(5) 0.0206(2) Uani 1 1 d . . .
V2A V 0.95932(9) 0.62534(8) 0.35406(6) 0.0227(3) Uani 1 1 d . . .
V1B V 0.64895(9) 0.85634(8) 0.62214(5) 0.0212(3) Uani 1 1 d . . .
V2B V 0.89999(9) 0.87801(8) 0.65285(6) 0.0233(3) Uani 1 1 d . . .
C1A C 0.5726(5) 0.8052(4) 0.3571(3) 0.0216(14) Uani 1 1 d . . .
C1B C 0.5018(6) 0.7039(5) 0.6392(3) 0.0279(16) Uani 1 1 d . . .
C2A C 0.4909(5) 0.7421(4) 0.3106(3) 0.0278(15) Uani 1 1 d . . .
H2A H 0.4206 0.7686 0.3041 0.033 Uiso 1 1 calc R . .
C2B C 0.4302(6) 0.7694(4) 0.6835(3) 0.0293(16) Uani 1 1 d . . .
H2B H 0.3570 0.7465 0.6851 0.035 Uiso 1 1 calc R . .
C3A C 0.5071(5) 0.6370(5) 0.2710(3) 0.0258(15) Uani 1 1 d . . .
C3B C 0.4606(5) 0.8710(5) 0.7277(3) 0.0241(14) Uani 1 1 d . . .
C11A C 0.5657(6) 0.9178(4) 0.3865(4) 0.0334(17) Uani 1 1 d . . .
H11A H 0.5853 0.9413 0.4417 0.050 Uiso 1 1 calc R . .
H11B H 0.4902 0.9370 0.3763 0.050 Uiso 1 1 calc R . .
H11C H 0.6170 0.9475 0.3605 0.050 Uiso 1 1 calc R . .
C11B C 0.4748(6) 0.5935(5) 0.6018(4) 0.0391(19) Uani 1 1 d . . .
H11D H 0.5193 0.5552 0.6283 0.059 Uiso 1 1 calc R . .
H11E H 0.4916 0.5739 0.5480 0.059 Uiso 1 1 calc R . .
H11F H 0.3962 0.5806 0.6052 0.059 Uiso 1 1 calc R . .
C12A C 0.4237(6) 0.5814(5) 0.2066(4) 0.0362(18) Uani 1 1 d . . .
H12A H 0.4534 0.5754 0.1573 0.054 Uiso 1 1 calc R . .
H12B H 0.3548 0.6178 0.2108 0.054 Uiso 1 1 calc R . .
H12C H 0.4090 0.5151 0.2102 0.054 Uiso 1 1 calc R . .
C12B C 0.3884(6) 0.9276(5) 0.7918(4) 0.0355(17) Uani 1 1 d . . .
H12D H 0.4249 0.9306 0.8415 0.053 Uiso 1 1 calc R . .
H12E H 0.3164 0.8933 0.7852 0.053 Uiso 1 1 calc R . .
H12F H 0.3780 0.9951 0.7895 0.053 Uiso 1 1 calc R . .
C4A C 0.7071(5) 0.4614(4) 0.2628(3) 0.0209(14) Uani 1 1 d . . .
C4B C 0.6722(5) 1.0425(4) 0.7432(3) 0.0241(15) Uani 1 1 d . . .
C5A C 0.7530(5) 0.3648(4) 0.2169(3) 0.0204(13) Uani 1 1 d . . .
C5B C 0.7282(5) 1.1392(4) 0.7890(3) 0.0203(13) Uani 1 1 d . . .
C10A C 0.8393(5) 0.3214(4) 0.2487(3) 0.0223(14) Uani 1 1 d . . .
H10A H 0.8651 0.3518 0.3006 0.027 Uiso 1 1 calc R . .
C10B C 0.8141(5) 1.1798(4) 0.7584(3) 0.0222(14) Uani 1 1 d . . .
H10B H 0.8341 1.1467 0.7081 0.027 Uiso 1 1 calc R . .
C9A C 0.8885(5) 0.2338(5) 0.2056(3) 0.0286(15) Uani 1 1 d . . .
H9A H 0.9475 0.2059 0.2276 0.034 Uiso 1 1 calc R . .
C9B C 0.8705(5) 1.2691(4) 0.8020(3) 0.0262(15) Uani 1 1 d . . .
H9B H 0.9282 1.2957 0.7813 0.031 Uiso 1 1 calc R . .
C8A C 0.8477(6) 0.1882(5) 0.1281(3) 0.0319(17) Uani 1 1 d . . .
H8A H 0.8804 0.1296 0.0981 0.038 Uiso 1 1 calc R . .
C8B C 0.8392(6) 1.3185(4) 0.8775(3) 0.0283(16) Uani 1 1 d . . .
H8B H 0.8764 1.3785 0.9070 0.034 Uiso 1 1 calc R . .
C7A C 0.7608(6) 0.2283(5) 0.0961(3) 0.0303(16) Uani 1 1 d . . .
H7A H 0.7335 0.1958 0.0449 0.036 Uiso 1 1 calc R . .
C7B C 0.7554(6) 1.2801(4) 0.9081(3) 0.0292(16) Uani 1 1 d . . .
H7B H 0.7357 1.3145 0.9582 0.035 Uiso 1 1 calc R . .
C6A C 0.7121(5) 0.3175(4) 0.1387(3) 0.0231(14) Uani 1 1 d . . .
C6B C 0.6979(5) 1.1898(4) 0.8659(3) 0.0239(14) Uani 1 1 d . . .
C13B C 1.0484(5) 1.0389(4) 0.6405(3) 0.0255(15) Uani 1 1 d . . .
C14B C 1.0913(6) 1.0683(5) 0.7167(4) 0.0315(16) Uani 1 1 d . . .
H14B H 1.1575 1.1075 0.7297 0.038 Uiso 1 1 calc R . .
C15B C 1.0396(6) 1.0419(5) 0.7773(3) 0.0280(15) Uani 1 1 d . . .
C23B C 1.0912(6) 1.0769(5) 0.5803(3) 0.0357(18) Uani 1 1 d . . .
H23D H 1.1147 1.0211 0.5382 0.054 Uiso 1 1 calc R . .
H23E H 1.1542 1.1225 0.6023 0.054 Uiso 1 1 calc R . .
H23F H 1.0326 1.1119 0.5610 0.054 Uiso 1 1 calc R . .
C24B C 1.0761(6) 1.1008(5) 0.8611(3) 0.043(2) Uani 1 1 d . . .
H24D H 1.0202 1.1493 0.8823 0.064 Uiso 1 1 calc R . .
H24E H 1.1468 1.1355 0.8629 0.064 Uiso 1 1 calc R . .
H24F H 1.0846 1.0550 0.8912 0.064 Uiso 1 1 calc R . .
C16B C 0.8288(5) 0.8926(4) 0.8013(3) 0.0246(15) Uani 1 1 d . . .
C13A C 1.1034(6) 0.4671(4) 0.3742(4) 0.0269(15) Uani 1 1 d . . .
C14A C 1.1324(5) 0.4344(5) 0.2995(4) 0.0295(16) Uani 1 1 d . . .
H14A H 1.1955 0.3945 0.2892 0.035 Uiso 1 1 calc R . .
C15A C 1.0754(5) 0.4556(5) 0.2363(3) 0.0261(15) Uani 1 1 d . . .
C23A C 1.1546(6) 0.4342(5) 0.4389(3) 0.0324(16) Uani 1 1 d . . .
H23A H 1.0988 0.3986 0.4571 0.049 Uiso 1 1 calc R . .
H23B H 1.1824 0.4924 0.4808 0.049 Uiso 1 1 calc R . .
H23C H 1.2158 0.3903 0.4207 0.049 Uiso 1 1 calc R . .
C24A C 1.0989(6) 0.3964(5) 0.1538(3) 0.043(2) Uani 1 1 d . . .
H24A H 1.0341 0.3546 0.1288 0.064 Uiso 1 1 calc R . .
H24B H 1.1626 0.3545 0.1546 0.064 Uiso 1 1 calc R . .
H24C H 1.1150 0.4424 0.1256 0.064 Uiso 1 1 calc R . .
C16A C 0.8629(5) 0.6043(4) 0.2025(3) 0.0197(13) Uani 1 1 d . . .
C17A C 0.7842(5) 0.6238(5) 0.1443(3) 0.0251(15) Uani 1 1 d . . .
C17B C 0.7548(6) 0.8721(5) 0.8560(3) 0.0277(15) Uani 1 1 d . . .
C22A C 0.7020(6) 0.6966(5) 0.1671(4) 0.0303(16) Uani 1 1 d . . .
H22A H 0.7019 0.7359 0.2192 0.036 Uiso 1 1 calc R . .
C22B C 0.6687(6) 0.7974(5) 0.8316(3) 0.0310(16) Uani 1 1 d . . .
H22B H 0.6646 0.7552 0.7802 0.037 Uiso 1 1 calc R . .
C21A C 0.6209(6) 0.7110(5) 0.1135(4) 0.0405(19) Uani 1 1 d . . .
H21A H 0.5689 0.7619 0.1290 0.049 Uiso 1 1 calc R . .
C21B C 0.5904(6) 0.7837(6) 0.8796(4) 0.0426(19) Uani 1 1 d . . .
H21B H 0.5340 0.7337 0.8615 0.051 Uiso 1 1 calc R . .
C20A C 0.6174(7) 0.6495(6) 0.0368(4) 0.046(2) Uani 1 1 d . . .
H20A H 0.5607 0.6569 0.0012 0.055 Uiso 1 1 calc R . .
C20B C 0.5976(7) 0.8465(6) 0.9562(4) 0.047(2) Uani 1 1 d . . .
H20B H 0.5443 0.8394 0.9897 0.057 Uiso 1 1 calc R . .
C19A C 0.6970(7) 0.5779(6) 0.0132(4) 0.048(2) Uani 1 1 d . . .
H19A H 0.6947 0.5379 -0.0388 0.058 Uiso 1 1 calc R . .
C19B C 0.6820(8) 0.9190(6) 0.9835(4) 0.055(2) Uani 1 1 d . . .
H19B H 0.6858 0.9591 1.0355 0.066 Uiso 1 1 calc R . .
C18A C 0.7813(6) 0.5639(5) 0.0656(4) 0.0354(18) Uani 1 1 d . . .
C18B C 0.7612(7) 0.9335(6) 0.9355(4) 0.0407(19) Uani 1 1 d . . .
O1A O 0.6381(4) 0.6341(3) 0.4491(2) 0.0263(10) Uani 1 1 d . . .
O1B O 0.5634(3) 0.8691(3) 0.5554(2) 0.0262(10) Uani 1 1 d . . .
O6A O 1.0569(4) 0.7071(3) 0.3679(2) 0.0296(11) Uani 1 1 d . . .
O6B O 0.9935(4) 0.7958(3) 0.6373(2) 0.0299(11) Uani 1 1 d . . .
O4A O 0.8546(3) 0.6762(3) 0.4222(2) 0.0205(9) Uani 1 1 d . . .
O4B O 0.7827(3) 0.8283(3) 0.5829(2) 0.0225(10) Uani 1 1 d . . .
O2A O 0.6717(4) 0.7713(3) 0.3736(2) 0.0260(10) Uani 1 1 d . . .
O2B O 0.6034(4) 0.7331(3) 0.6299(2) 0.0239(10) Uani 1 1 d . . .
O3A O 0.7613(3) 0.5115(3) 0.3301(2) 0.0226(10) Uani 1 1 d . . .
O3B O 0.7138(3) 0.9917(3) 0.6768(2) 0.0209(9) Uani 1 1 d . . .
O5A O 0.6295(4) 0.3560(3) 0.1019(2) 0.0306(11) Uani 1 1 d . . .
H5A H 0.6184 0.4144 0.1280 0.046 Uiso 1 1 calc R . .
O5B O 0.6164(4) 1.1545(3) 0.9000(2) 0.0287(11) Uani 1 1 d . . .
H5B H 0.5851 1.1045 0.8682 0.043 Uiso 1 1 calc R . .
O7B O 0.9591(4) 0.9764(3) 0.6189(2) 0.0277(10) Uani 1 1 d . . .
O8B O 0.8082(3) 0.8409(3) 0.7259(2) 0.0238(10) Uani 1 1 d . . .
O7A O 1.0202(4) 0.5292(3) 0.3934(2) 0.0275(10) Uani 1 1 d . . .
O8A O 0.8563(3) 0.6572(3) 0.2769(2) 0.0232(10) Uani 1 1 d . . .
O9A O 0.8584(5) 0.4932(4) 0.0384(2) 0.0485(15) Uani 1 1 d . . .
H9C H 0.9047 0.4930 0.0741 0.073 Uiso 1 1 calc R . .
O9B O 0.8414(5) 1.0064(4) 0.9654(3) 0.0544(16) Uani 1 1 d . . .
H9D H 0.8761 1.0146 0.9300 0.082 Uiso 1 1 calc R . .
N1A N 0.5979(4) 0.5927(3) 0.2881(3) 0.0214(12) Uani 1 1 d . . .
N1B N 0.5529(4) 0.9133(3) 0.7154(3) 0.0217(12) Uani 1 1 d . . .
N2A N 0.6182(4) 0.4964(4) 0.2367(3) 0.0253(12) Uani 1 1 d . . .
N2B N 0.5863(4) 1.0074(4) 0.7677(3) 0.0219(12) Uani 1 1 d . . .
N3B N 0.9596(4) 0.9732(4) 0.7616(3) 0.0230(12) Uani 1 1 d . . .
N4B N 0.9065(5) 0.9619(4) 0.8248(3) 0.0262(12) Uani 1 1 d . . .
N3A N 0.9983(4) 0.5251(3) 0.2482(3) 0.0200(11) Uani 1 1 d . . .
N4A N 0.9371(4) 0.5333(4) 0.1826(3) 0.0240(12) Uani 1 1 d . . .
C25 C 0.3041(7) 0.7865(6) 0.4948(4) 0.051(2) Uani 1 1 d . . .
H25 H 0.3744 0.8060 0.5279 0.061 Uiso 1 1 calc R . .
Cl1 Cl 0.31675(19) 0.66200(17) 0.43076(14) 0.0671(7) Uani 1 1 d . . .
Cl2 Cl 0.19314(19) 0.7880(2) 0.55495(12) 0.0697(7) Uani 1 1 d . . .
Cl3 Cl 0.28166(16) 0.87232(13) 0.44369(10) 0.0413(5) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
V1A O1A 1.575(4) . ?
V1A O4A 1.790(4) . ?
V1A O2A 1.847(4) . ?
V1A O3A 1.951(4) . ?
V1A N1A 2.059(5) . ?
V1A V2A 3.0266(16) . ?
V2A O6A 1.572(4) . ?
V2A O4A 1.799(4) . ?
V2A O7A 1.831(4) . ?
V2A O8A 1.952(4) . ?
V2A N3A 2.070(4) . ?
V1B O1B 1.579(4) . ?
V1B O4B 1.780(4) . ?
V1B O2B 1.844(4) . ?
V1B O3B 1.960(4) . ?
V1B N1B 2.051(5) . ?
V1B V2B 2.9958(15) . ?
V2B O6B 1.574(4) . ?
V2B O4B 1.799(4) . ?
V2B O7B 1.820(4) . ?
V2B O8B 1.952(4) . ?
V2B N3B 2.075(5) . ?
C1A O2A 1.321(7) . ?
C1A C2A 1.358(8) . ?
C1A C11A 1.494(7) . ?
C1B O2B 1.309(7) . ?
C1B C2B 1.358(8) . ?
C1B C11B 1.496(8) . ?
C2A C3A 1.435(8) . ?
C2A H2A 0.9300 . ?
C2B C3B 1.421(8) . ?
C2B H2B 0.9300 . ?
C3A N1A 1.312(7) . ?
C3A C12A 1.489(8) . ?
C3B N1B 1.306(7) . ?
C3B C12B 1.506(8) . ?
C11A H11A 0.9600 . ?
C11A H11B 0.9600 . ?
C11A H11C 0.9600 . ?
C11B H11D 0.9600 . ?
C11B H11E 0.9600 . ?
C11B H11F 0.9600 . ?
C12A H12A 0.9600 . ?
C12A H12B 0.9600 . ?
C12A H12C 0.9600 . ?
C12B H12D 0.9600 . ?
C12B H12E 0.9600 . ?
C12B H12F 0.9600 . ?
C4A N2A 1.288(7) . ?
C4A O3A 1.322(6) . ?
C4A C5A 1.471(8) . ?
C4B N2B 1.290(8) . ?
C4B O3B 1.320(6) . ?
C4B C5B 1.471(8) . ?
C5A C10A 1.375(8) . ?
C5A C6A 1.413(7) . ?
C5B C10B 1.389(8) . ?
C5B C6B 1.421(7) . ?
C10A C9A 1.383(8) . ?
C10A H10A 0.9300 . ?
C10B C9B 1.387(7) . ?
C10B H10B 0.9300 . ?
C9A C8A 1.399(8) . ?
C9A H9A 0.9300 . ?
C9B C8B 1.400(8) . ?
C9B H9B 0.9300 . ?
C8A C7A 1.357(9) . ?
C8A H8A 0.9300 . ?
C8B C7B 1.354(9) . ?
C8B H8B 0.9300 . ?
C7A C6A 1.393(8) . ?
C7A H7A 0.9300 . ?
C7B C6B 1.397(8) . ?
C7B H7B 0.9300 . ?
C6A O5A 1.355(7) . ?
C6B O5B 1.348(7) . ?
C13B O7B 1.326(7) . ?
C13B C14B 1.370(8) . ?
C13B C23B 1.467(8) . ?
C14B C15B 1.431(9) . ?
C14B H14B 0.9300 . ?
C15B N3B 1.298(8) . ?
C15B C24B 1.515(8) . ?
C23B H23D 0.9600 . ?
C23B H23E 0.9600 . ?
C23B H23F 0.9600 . ?
C24B H24D 0.9600 . ?
C24B H24E 0.9600 . ?
C24B H24F 0.9600 . ?
C16B N4B 1.283(7) . ?
C16B O8B 1.333(6) . ?
C16B C17B 1.457(9) . ?
C13A O7A 1.308(7) . ?
C13A C14A 1.353(8) . ?
C13A C23A 1.480(8) . ?
C14A C15A 1.401(8) . ?
C14A H14A 0.9300 . ?
C15A N3A 1.314(7) . ?
C15A C24A 1.508(8) . ?
C23A H23A 0.9600 . ?
C23A H23B 0.9600 . ?
C23A H23C 0.9600 . ?
C24A H24A 0.9600 . ?
C24A H24B 0.9600 . ?
C24A H24C 0.9600 . ?
C16A N4A 1.309(7) . ?
C16A O8A 1.325(6) . ?
C16A C17A 1.452(8) . ?
C17A C22A 1.397(8) . ?
C17A C18A 1.405(8) . ?
C17B C22B 1.403(9) . ?
C17B C18B 1.421(8) . ?
C22A C21A 1.382(8) . ?
C22A H22A 0.9300 . ?
C22B C21B 1.365(9) . ?
C22B H22B 0.9300 . ?
C21A C20A 1.382(9) . ?
C21A H21A 0.9300 . ?
C21B C20B 1.385(9) . ?
C21B H21B 0.9300 . ?
C20A C19A 1.367(10) . ?
C20A H20A 0.9300 . ?
C20B C19B 1.372(11) . ?
C20B H20B 0.9300 . ?
C19A C18A 1.391(9) . ?
C19A H19A 0.9300 . ?
C19B C18B 1.377(10) . ?
C19B H19B 0.9300 . ?
C18A O9A 1.348(8) . ?
C18B O9B 1.345(8) . ?
O5A H5A 0.8200 . ?
O5B H5B 0.8200 . ?
O9A H9C 0.8200 . ?
O9B H9D 0.8200 . ?
N1A N2A 1.405(6) . ?
N1B N2B 1.393(6) . ?
N3B N4B 1.392(7) . ?
N3A N4A 1.387(6) . ?
C25 Cl3 1.734(8) . ?
C25 Cl2 1.761(8) . ?
C25 Cl1 1.772(8) . ?
C25 H25 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
O1A V1A O4A 109.1(2) . . ?
O1A V1A O2A 104.5(2) . . ?
O4A V1A O2A 99.92(18) . . ?
O1A V1A O3A 104.64(19) . . ?
O4A V1A O3A 86.70(17) . . ?
O2A V1A O3A 146.03(17) . . ?
O1A V1A N1A 99.6(2) . . ?
O4A V1A N1A 149.22(19) . . ?
O2A V1A N1A 83.09(18) . . ?
O3A V1A N1A 75.17(17) . . ?
O6A V2A O4A 108.39(19) . . ?
O6A V2A O7A 104.4(2) . . ?
O4A V2A O7A 100.98(18) . . ?
O6A V2A O8A 102.7(2) . . ?
O4A V2A O8A 85.92(17) . . ?
O7A V2A O8A 148.18(18) . . ?
O6A V2A N3A 100.6(2) . . ?
O4A V2A N3A 148.38(19) . . ?
O7A V2A N3A 83.48(18) . . ?
O8A V2A N3A 75.37(17) . . ?
O1B V1B O4B 107.88(19) . . ?
O1B V1B O2B 102.24(19) . . ?
O4B V1B O2B 101.98(18) . . ?
O1B V1B O3B 105.96(19) . . ?
O4B V1B O3B 85.97(17) . . ?
O2B V1B O3B 146.67(16) . . ?
O1B V1B N1B 98.8(2) . . ?
O4B V1B N1B 150.63(18) . . ?
O2B V1B N1B 83.56(18) . . ?
O3B V1B N1B 74.96(17) . . ?
O6B V2B O4B 107.53(19) . . ?
O6B V2B O7B 103.3(2) . . ?
O4B V2B O7B 102.81(19) . . ?
O6B V2B O8B 102.9(2) . . ?
O4B V2B O8B 84.94(17) . . ?
O7B V2B O8B 148.84(18) . . ?
O6B V2B N3B 100.5(2) . . ?
O4B V2B N3B 148.85(19) . . ?
O7B V2B N3B 83.22(19) . . ?
O8B V2B N3B 75.70(18) . . ?
O2A C1A C2A 121.5(5) . . ?
O2A C1A C11A 113.7(5) . . ?
C2A C1A C11A 124.5(6) . . ?
O2B C1B C2B 121.3(6) . . ?
O2B C1B C11B 115.2(6) . . ?
C2B C1B C11B 123.4(6) . . ?
C1A C2A C3A 123.6(6) . . ?
C1A C2A H2A 118.2 . . ?
C3A C2A H2A 118.2 . . ?
C1B C2B C3B 123.7(6) . . ?
C1B C2B H2B 118.1 . . ?
C3B C2B H2B 118.1 . . ?
N1A C3A C2A 120.1(5) . . ?
N1A C3A C12A 120.8(5) . . ?
C2A C3A C12A 118.9(5) . . ?
N1B C3B C2B 120.5(6) . . ?
N1B C3B C12B 120.3(5) . . ?
C2B C3B C12B 119.2(6) . . ?
C1A C11A H11A 109.5 . . ?
C1A C11A H11B 109.5 . . ?
H11A C11A H11B 109.5 . . ?
C1A C11A H11C 109.5 . . ?
H11A C11A H11C 109.5 . . ?
H11B C11A H11C 109.5 . . ?
C1B C11B H11D 109.5 . . ?
C1B C11B H11E 109.5 . . ?
H11D C11B H11E 109.5 . . ?
C1B C11B H11F 109.5 . . ?
H11D C11B H11F 109.5 . . ?
H11E C11B H11F 109.5 . . ?
C3A C12A H12A 109.5 . . ?
C3A C12A H12B 109.5 . . ?
H12A C12A H12B 109.5 . . ?
C3A C12A H12C 109.5 . . ?
H12A C12A H12C 109.5 . . ?
H12B C12A H12C 109.5 . . ?
C3B C12B H12D 109.5 . . ?
C3B C12B H12E 109.5 . . ?
H12D C12B H12E 109.5 . . ?
C3B C12B H12F 109.5 . . ?
H12D C12B H12F 109.5 . . ?
H12E C12B H12F 109.5 . . ?
N2A C4A O3A 121.6(5) . . ?
N2A C4A C5A 120.5(5) . . ?
O3A C4A C5A 117.9(5) . . ?
N2B C4B O3B 120.9(5) . . ?
N2B C4B C5B 121.3(5) . . ?
O3B C4B C5B 117.8(6) . . ?
C10A C5A C6A 119.1(5) . . ?
C10A C5A C4A 120.4(5) . . ?
C6A C5A C4A 120.4(5) . . ?
C10B C5B C6B 119.5(5) . . ?
C10B C5B C4B 120.2(5) . . ?
C6B C5B C4B 120.3(6) . . ?
C5A C10A C9A 121.7(5) . . ?
C5A C10A H10A 119.2 . . ?
C9A C10A H10A 119.2 . . ?
C9B C10B C5B 120.8(5) . . ?
C9B C10B H10B 119.6 . . ?
C5B C10B H10B 119.6 . . ?
C10A C9A C8A 118.6(6) . . ?
C10A C9A H9A 120.7 . . ?
C8A C9A H9A 120.7 . . ?
C10B C9B C8B 119.0(6) . . ?
C10B C9B H9B 120.5 . . ?
C8B C9B H9B 120.5 . . ?
C7A C8A C9A 120.8(6) . . ?
C7A C8A H8A 119.6 . . ?
C9A C8A H8A 119.6 . . ?
C7B C8B C9B 120.9(6) . . ?
C7B C8B H8B 119.6 . . ?
C9B C8B H8B 119.6 . . ?
C8A C7A C6A 121.0(6) . . ?
C8A C7A H7A 119.5 . . ?
C6A C7A H7A 119.5 . . ?
C8B C7B C6B 121.4(6) . . ?
C8B C7B H7B 119.3 . . ?
C6B C7B H7B 119.3 . . ?
O5A C6A C7A 117.8(5) . . ?
O5A C6A C5A 123.3(5) . . ?
C7A C6A C5A 118.8(6) . . ?
O5B C6B C7B 118.7(5) . . ?
O5B C6B C5B 123.0(5) . . ?
C7B C6B C5B 118.3(6) . . ?
O7B C13B C14B 119.7(6) . . ?
O7B C13B C23B 116.2(5) . . ?
C14B C13B C23B 124.0(6) . . ?
C13B C14B C15B 123.6(6) . . ?
C13B C14B H14B 118.2 . . ?
C15B C14B H14B 118.2 . . ?
N3B C15B C14B 121.4(6) . . ?
N3B C15B C24B 120.4(6) . . ?
C14B C15B C24B 118.1(6) . . ?
C13B C23B H23D 109.5 . . ?
C13B C23B H23E 109.5 . . ?
H23D C23B H23E 109.5 . . ?
C13B C23B H23F 109.5 . . ?
H23D C23B H23F 109.5 . . ?
H23E C23B H23F 109.5 . . ?
C15B C24B H24D 109.5 . . ?
C15B C24B H24E 109.5 . . ?
H24D C24B H24E 109.5 . . ?
C15B C24B H24F 109.5 . . ?
H24D C24B H24F 109.5 . . ?
H24E C24B H24F 109.5 . . ?
N4B C16B O8B 121.8(6) . . ?
N4B C16B C17B 120.6(5) . . ?
O8B C16B C17B 117.5(6) . . ?
O7A C13A C14A 120.1(6) . . ?
O7A C13A C23A 114.4(5) . . ?
C14A C13A C23A 125.4(6) . . ?
C13A C14A C15A 125.6(6) . . ?
C13A C14A H14A 117.2 . . ?
C15A C14A H14A 117.2 . . ?
N3A C15A C14A 120.3(5) . . ?
N3A C15A C24A 119.3(6) . . ?
C14A C15A C24A 120.3(6) . . ?
C13A C23A H23A 109.5 . . ?
C13A C23A H23B 109.5 . . ?
H23A C23A H23B 109.5 . . ?
C13A C23A H23C 109.5 . . ?
H23A C23A H23C 109.5 . . ?
H23B C23A H23C 109.5 . . ?
C15A C24A H24A 109.5 . . ?
C24A C24A H24B 109.5 . . ?
H24A C24A H24B 109.5 . . ?
C15A C24A H24C 109.5 . . ?
H24A C24A H24C 109.5 . . ?
H24B C24A H24C 109.5 . . ?
N4A C16A O8A 120.1(5) . . ?
N4A C16A C17A 120.8(5) . . ?
O8A C16A C17A 119.1(5) . . ?
C22A C17A C18A 118.5(6) . . ?
C22A C17A C16A 120.0(5) . . ?
C18A C17A C16A 121.2(6) . . ?
C22B C17B C18B 117.3(6) . . ?
C22B C17B C16B 121.7(5) . . ?
C18B C17B C16B 120.8(6) . . ?
C21A C22A C17A 121.0(6) . . ?
C21A C22A H22A 119.5 . . ?
C17A C22A H22A 119.5 . . ?
C21B C22B C17B 123.2(6) . . ?
C21B C22B H22B 118.4 . . ?
C17B C22B H22B 118.4 . . ?
C20A C21A C22A 119.7(7) . . ?
C20A C21A H21A 120.1 . . ?
C22A C21A H21A 120.1 . . ?
C22B C21B C20B 117.9(7) . . ?
C22B C21B H21B 121.0 . . ?
C20B C21B H21B 121.0 . . ?
C19A C20A C21A 120.2(7) . . ?
C19A C20A H20A 119.9 . . ?
C21A C20A H20A 119.9 . . ?
C19B C20B C21B 121.1(7) . . ?
C19B C20B H20B 119.4 . . ?
C21B C20B H20B 119.4 . . ?
C20A C19A C18A 121.1(6) . . ?
C20A C19A H19A 119.5 . . ?
C18A C19A H19A 119.5 . . ?
C20B C19B C18B 121.4(7) . . ?
C20B C19B H19B 119.3 . . ?
C18B C19B H19B 119.3 . . ?
O9A C18A C19A 118.2(6) . . ?
O9A C18A C17A 122.3(6) . . ?
C19A C18A C17A 119.4(7) . . ?
O9B C18B C19B 118.6(7) . . ?
O9B C18B C17B 122.3(7) . . ?
C19B C18B C17B 119.1(7) . . ?
V1A O4A V2A 114.97(19) . . ?
V1B O4B V2B 113.68(19) . . ?
C1A O2A V1A 130.9(4) . . ?
C1B O2B V1B 128.0(4) . . ?
C4A O3A V1A 117.4(4) . . ?
C4B O3B V1B 117.4(4) . . ?
C6A O5A H5A 109.5 . . ?
C6B O5B H5B 109.5 . . ?
C13B O7B V2B 135.0(4) . . ?
C16B O8B V2B 116.6(4) . . ?
C13A O7A V2A 133.6(4) . . ?
C16A O8A V2A 118.0(4) . . ?
C18A O9A H9C 109.5 . . ?
C18B O9B H9D 109.5 . . ?
C3A N1A N2A 116.3(5) . . ?
C3A N1A V1A 127.2(4) . . ?
N2A N1A V1A 116.5(4) . . ?
C3B N1B N2B 117.5(5) . . ?
C3B N1B V1B 125.5(4) . . ?
N2B N1B V1B 116.9(4) . . ?
C4A N2A N1A 109.0(5) . . ?
C4B N2B N1B 109.6(5) . . ?
C15B N3B N4B 116.6(5) . . ?
C15B N3B V2B 127.8(4) . . ?
N4B N3B V2B 115.7(4) . . ?
C16B N4B N3B 110.2(5) . . ?
C15A N3A N4A 116.5(5) . . ?
C15A N3A V2A 127.3(4) . . ?
N4A N3A V2A 116.2(3) . . ?
C16A N4A N3A 110.4(4) . . ?
Cl3 C25 Cl2 110.7(4) . . ?
Cl3 C25 Cl1 111.4(4) . . ?
Cl2 C25 Cl1 109.1(4) . . ?
Cl3 C25 H25 108.5 . . ?
Cl2 C25 H25 108.5 . . ?
Cl1 C25 H25 108.5 . . ?

_diffrn_measured_fraction_theta_max 0.972
_diffrn_reflns_theta_full        27.50
_diffrn_measured_fraction_theta_full 0.972
_refine_diff_density_max         0.668
_refine_diff_density_min         -0.755
_refine_diff_density_rms         0.113
_database_code_depnum_ccdc_archive 'CCDC 972497'
