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

#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
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#  data retrieval see:
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data_1
_audit_creation_date             2014-04-05
_audit_creation_method           
;
Olex2 1.2
(compiled 2013.11.15 svn.r2834 for OlexSys, GUI svn.r4720)
;
_chemical_name_common            ?
_chemical_name_systematic        
;
 ? 
;
_chemical_formula_moiety         'C32 H40 N4 O10 P2 V2, 2(Cl)'
_chemical_formula_sum            'C32 H40 Cl2 N4 O10 P2 V2'
_chemical_formula_weight         875.40
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 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'
P P 0.1023 0.0942 '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'
V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_H-M_alt        'P n m a'
_space_group_name_Hall           '-P 2ac 2n'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x+1/2, -y, z+1/2'
3 'x+1/2, -y+1/2, -z+1/2'
4 '-x, y+1/2, -z'
5 '-x, -y, -z'
6 'x-1/2, y, -z-1/2'
7 '-x-1/2, y-1/2, z-1/2'
8 'x, -y-1/2, z'

_cell_length_a                   19.079(5)
_cell_length_b                   18.583(5)
_cell_length_c                   10.924(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     3873(2)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    2632
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24.94
_cell_measurement_theta_min      2.19
_exptl_absorpt_coefficient_mu    0.761
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.078127
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS v.2.10 (Bruker,2003) was used for absorption correction. R(int) was 0.1488 before and 0.0496 after correction. The Ratio of minimum to maximum transmission is 0.0781. The λ/2 correction factor is 0.0015.'
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.501
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1800
_exptl_crystal_size_max          0.084
_exptl_crystal_size_mid          0.082
_exptl_crystal_size_min          0.08
_exptl_special_details           
;
 ? 
;
_diffrn_reflns_av_R_equivalents  0.1282
_diffrn_reflns_av_unetI/netI     0.0818
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            19242
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         2.19
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_source                   'fine-focus sealed tube'
_reflns_number_gt                2816
_reflns_number_total             3652
_reflns_threshold_expression     >2sigma(I)
_computing_cell_refinement       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'SIR97 (Burla et al., 2007)'
_refine_diff_density_max         1.080
_refine_diff_density_min         -1.516
_refine_diff_density_rms         0.111
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     253
_refine_ls_number_reflns         3652
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0898
_refine_ls_R_factor_gt           0.0673
_refine_ls_restrained_S_all      1.055
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0727P)²+7.0044P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1543
_refine_ls_wR_factor_ref         0.1670
_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. 
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(O6) = Uanis(O2)
Uanis(C9) = Uanis(C8)
3. Others
 Fixed Sof: H14B(0.5) H14C(0.5) H17A(0.5) H17B(0.5) H17C(0.5)
4.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C6(H6A), C7(H7), C10(H10), C11(H11), C12(H12)
4.b Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C17(H17A,H17B,H17C), C18(H18A,H18B,
 H18C)
4.c Idealised tetrahedral OH refined as rotating group:
 O2(H2A), O6(H6)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
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_disorder_assembly
_atom_site_disorder_group
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
H4 H 0.578(5) 0.2500 0.136(8) 0.05(3) Uiso 1 2 d . . S T
V1 V 0.56902(4) 0.11339(4) 0.45577(7) 0.0217(2) Uani 1 1 d . . . .
Cl1 Cl 0.69204(8) 0.2500 0.15677(14) 0.0245(4) Uani 1 2 d . . S T
Cl2 Cl 0.77854(8) 0.2500 0.54735(14) 0.0265(4) Uani 1 2 d . . S T
P1 P 0.59248(8) 0.2500 0.66107(14) 0.0183(4) Uani 1 2 d . . S T
P2 P 0.51371(8) 0.2500 0.27251(14) 0.0185(4) Uani 1 2 d . . S T
O1 O 0.49575(16) 0.08070(19) 0.4977(3) 0.0325(8) Uani 1 1 d . . . .
O2 O 0.68012(15) 0.14692(19) 0.3891(3) 0.0235(6) Uani 1 1 d . . . .
H2A H 0.6967 0.1765 0.4366 0.035 Uiso 1 1 calc . . GR .
O3 O 0.53944(16) 0.18208(19) 0.3313(3) 0.0346(9) Uani 1 1 d . . . .
O4 O 0.5363(3) 0.2500 0.1349(4) 0.0371(14) Uani 1 2 d . . S T
O5 O 0.58743(18) 0.18221(19) 0.5876(3) 0.0334(8) Uani 1 1 d . . . .
O6 O 0.6638(2) 0.2500 0.7340(4) 0.0235(6) Uani 1 2 d . . S T
H6 H 0.6966 0.2500 0.6855 0.035 Uiso 1 2 calc . . GRS T
N1 N 0.59003(18) 0.0381(2) 0.3124(3) 0.0236(9) Uani 1 1 d . . . .
N2 N 0.63393(18) 0.0369(2) 0.5448(3) 0.0214(8) Uani 1 1 d . . . .
C1 C 0.5692(2) 0.0407(3) 0.1960(5) 0.0333(12) Uani 1 1 d . . . .
H1 H 0.5411 0.0788 0.1708 0.040 Uiso 1 1 calc . . R .
C2 C 0.5880(3) -0.0115(3) 0.1107(5) 0.0394(14) Uani 1 1 d . . . .
H2 H 0.5726 -0.0077 0.0302 0.047 Uiso 1 1 calc . . R .
C3 C 0.6289(2) -0.0683(3) 0.1453(5) 0.0349(12) Uani 1 1 d . . . .
H3 H 0.6414 -0.1035 0.0890 0.042 Uiso 1 1 calc . . R .
C4 C 0.6519(2) -0.0726(3) 0.2670(4) 0.0265(11) Uani 1 1 d . . . .
C5 C 0.6315(2) -0.0177(2) 0.3469(4) 0.0203(10) Uani 1 1 d . . . .
C6 C 0.6967(2) -0.1290(3) 0.3110(5) 0.0305(11) Uani 1 1 d . . . .
H6A H 0.7096 -0.1660 0.2583 0.037 Uiso 1 1 calc . . R .
C7 C 0.7204(2) -0.1293(3) 0.4277(5) 0.0283(11) Uani 1 1 d . . . .
H7 H 0.7503 -0.1657 0.4536 0.034 Uiso 1 1 calc . . R .
C8 C 0.6998(2) -0.0736(2) 0.5125(4) 0.0238(7) Uani 1 1 d . . . .
C9 C 0.6557(2) -0.0180(2) 0.4716(4) 0.0238(7) Uani 1 1 d . . . .
C10 C 0.7214(2) -0.0709(3) 0.6361(4) 0.0287(11) Uani 1 1 d . . . .
H10 H 0.7511 -0.1061 0.6673 0.034 Uiso 1 1 calc . . R .
C11 C 0.6986(2) -0.0167(3) 0.7089(4) 0.0287(11) Uani 1 1 d . . . .
H11 H 0.7116 -0.0152 0.7910 0.034 Uiso 1 1 calc . . R .
C12 C 0.6556(2) 0.0370(3) 0.6604(4) 0.0258(11) Uani 1 1 d . . . .
H12 H 0.6414 0.0744 0.7112 0.031 Uiso 1 1 calc . . R .
C13 C 0.4192(3) 0.2500 0.2639(6) 0.0216(14) Uani 1 2 d . . S T
C14 C 0.3918(3) 0.2500 0.3954(6) 0.0297(17) Uani 1 2 d . . S T
H14A H 0.3414 0.2501 0.3946 0.045 Uiso 1 2 calc . . GRS T
H14B H 0.4084 0.2921 0.4372 0.045 Uiso 0.50 1 calc . . GR .
H14C H 0.4082 0.2077 0.4371 0.045 Uiso 0.50 1 calc . . GR .
C15 C 0.3949(2) 0.1820(3) 0.1973(5) 0.0325(12) Uani 1 1 d . . . .
H15A H 0.3446 0.1797 0.1984 0.049 Uiso 1 1 calc . . GR .
H15B H 0.4138 0.1404 0.2375 0.049 Uiso 1 1 calc . . GR .
H15C H 0.4110 0.1833 0.1140 0.049 Uiso 1 1 calc . . GR .
C16 C 0.5279(3) 0.2500 0.7820(6) 0.0232(14) Uani 1 2 d . . S T
C17 C 0.4549(3) 0.2500 0.7226(7) 0.0344(18) Uani 1 2 d . . S T
H17A H 0.4468 0.2045 0.6835 0.052 Uiso 0.50 1 calc . . GR .
H17B H 0.4523 0.2878 0.6628 0.052 Uiso 0.50 1 calc . . GR .
H17C H 0.4199 0.2577 0.7844 0.052 Uiso 0.50 1 calc . . GR .
C18 C 0.5372(3) 0.3184(3) 0.8600(4) 0.0344(12) Uani 1 1 d . . . .
H18A H 0.5281 0.3601 0.8105 0.052 Uiso 1 1 calc . . GR .
H18B H 0.5843 0.3205 0.8906 0.052 Uiso 1 1 calc . . GR .
H18C H 0.5050 0.3173 0.9275 0.052 Uiso 1 1 calc . . GR .
H2B H 0.682(3) 0.185(3) 0.327(6) 0.07(2) Uiso 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
V1 O1 1.592(3) . ?
V1 O2 2.326(3) . ?
V1 O3 1.948(3) . ?
V1 O5 1.958(4) . ?
V1 N1 2.138(4) . ?
V1 N2 2.122(4) . ?
P1 O5 1.497(3) 8_565 ?
P1 O5 1.497(3) . ?
P1 O6 1.576(4) . ?
P1 C16 1.806(6) . ?
P2 O3 1.499(3) 8_565 ?
P2 O3 1.499(3) . ?
P2 O4 1.564(5) . ?
P2 C13 1.806(6) . ?
O2 H2A 0.8200 . ?
O2 H2B 0.98(7) . ?
O4 H4 0.80(9) . ?
O6 H6 0.8200 . ?
N1 C1 1.333(6) . ?
N1 C5 1.357(6) . ?
N2 C9 1.361(6) . ?
N2 C12 1.329(6) . ?
C1 H1 0.9300 . ?
C1 C2 1.391(7) . ?
C2 H2 0.9300 . ?
C2 C3 1.366(8) . ?
C3 H3 0.9300 . ?
C3 C4 1.402(7) . ?
C4 C5 1.398(6) . ?
C4 C6 1.435(7) . ?
C5 C9 1.438(6) . ?
C6 H6A 0.9300 . ?
C6 C7 1.354(7) . ?
C7 H7 0.9300 . ?
C7 C8 1.443(7) . ?
C8 C9 1.405(6) . ?
C8 C10 1.412(7) . ?
C10 H10 0.9300 . ?
C10 C11 1.357(7) . ?
C11 H11 0.9300 . ?
C11 C12 1.396(7) . ?
C12 H12 0.9300 . ?
C13 C14 1.529(9) . ?
C13 C15 1.530(6) . ?
C13 C15 1.530(6) 8_565 ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C16 C17 1.537(9) . ?
C16 C18 1.541(6) . ?
C16 C18 1.541(6) 8_565 ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 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 O2 173.06(16) . . ?
O1 V1 O3 101.34(16) . . ?
O1 V1 O5 101.24(16) . . ?
O1 V1 N1 97.23(16) . . ?
O1 V1 N2 97.17(16) . . ?
O3 V1 O2 82.52(13) . . ?
O3 V1 O5 97.89(16) . . ?
O3 V1 N1 88.40(15) . . ?
O3 V1 N2 158.12(14) . . ?
O5 V1 O2 83.81(12) . . ?
O5 V1 N1 158.86(14) . . ?
O5 V1 N2 89.77(15) . . ?
N1 V1 O2 76.99(13) . . ?
N2 V1 O2 77.95(13) . . ?
N2 V1 N1 77.74(14) . . ?
O5 P1 O5 114.7(3) 8_565 . ?
O5 P1 O6 109.04(17) 8_565 . ?
O5 P1 O6 109.04(17) . . ?
O5 P1 C16 110.38(16) 8_565 . ?
O5 P1 C16 110.38(16) . . ?
O6 P1 C16 102.6(3) . . ?
O3 P2 O3 114.7(3) 8_565 . ?
O3 P2 O4 108.79(17) 8_565 . ?
O3 P2 O4 108.79(17) . . ?
O3 P2 C13 110.45(16) 8_565 . ?
O3 P2 C13 110.45(16) . . ?
O4 P2 C13 103.0(3) . . ?
V1 O2 H2A 109.5 . . ?
V1 O2 H2B 116(4) . . ?
H2A O2 H2B 86.7 . . ?
P2 O3 V1 161.0(3) . . ?
P2 O4 H4 105(6) . . ?
P1 O5 V1 162.9(2) . . ?
P1 O6 H6 109.5 . . ?
C1 N1 V1 128.3(4) . . ?
C1 N1 C5 117.8(4) . . ?
C5 N1 V1 113.9(3) . . ?
C9 N2 V1 114.3(3) . . ?
C12 N2 V1 128.0(3) . . ?
C12 N2 C9 117.7(4) . . ?
N1 C1 H1 118.8 . . ?
N1 C1 C2 122.5(5) . . ?
C2 C1 H1 118.8 . . ?
C1 C2 H2 120.0 . . ?
C3 C2 C1 120.0(5) . . ?
C3 C2 H2 120.0 . . ?
C2 C3 H3 120.5 . . ?
C2 C3 C4 119.0(5) . . ?
C4 C3 H3 120.5 . . ?
C3 C4 C6 123.0(5) . . ?
C5 C4 C3 117.6(5) . . ?
C5 C4 C6 119.3(4) . . ?
N1 C5 C4 123.1(4) . . ?
N1 C5 C9 117.0(4) . . ?
C4 C5 C9 119.9(4) . . ?
C4 C6 H6A 119.4 . . ?
C7 C6 C4 121.1(5) . . ?
C7 C6 H6A 119.4 . . ?
C6 C7 H7 119.6 . . ?
C6 C7 C8 120.8(5) . . ?
C8 C7 H7 119.6 . . ?
C9 C8 C7 119.1(4) . . ?
C9 C8 C10 116.9(4) . . ?
C10 C8 C7 124.0(4) . . ?
N2 C9 C5 117.0(4) . . ?
N2 C9 C8 123.2(4) . . ?
C8 C9 C5 119.8(4) . . ?
C8 C10 H10 120.2 . . ?
C11 C10 C8 119.5(4) . . ?
C11 C10 H10 120.2 . . ?
C10 C11 H11 120.1 . . ?
C10 C11 C12 119.8(4) . . ?
C12 C11 H11 120.1 . . ?
N2 C12 C11 122.9(5) . . ?
N2 C12 H12 118.6 . . ?
C11 C12 H12 118.6 . . ?
C14 C13 P2 107.0(4) . . ?
C14 C13 C15 110.1(3) . 8_565 ?
C14 C13 C15 110.1(3) . . ?
C15 C13 P2 109.1(3) . . ?
C15 C13 P2 109.1(3) 8_565 . ?
C15 C13 C15 111.3(5) . 8_565 ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C13 C15 H15A 109.5 . . ?
C13 C15 H15B 109.5 . . ?
C13 C15 H15C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C17 C16 P1 108.0(4) . . ?
C17 C16 C18 109.7(3) . . ?
C17 C16 C18 109.7(3) . 8_565 ?
C18 C16 P1 109.0(3) . . ?
C18 C16 P1 109.0(3) 8_565 . ?
C18 C16 C18 111.2(5) . 8_565 ?
C16 C17 H17A 109.5 . . ?
C16 C17 H17B 109.5 . . ?
C16 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C16 C18 H18A 109.5 . . ?
C16 C18 H18B 109.5 . . ?
C16 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
V1 N1 C1 C2 178.6(4) . . . . ?
V1 N1 C5 C4 -179.6(3) . . . . ?
V1 N1 C5 C9 -0.7(5) . . . . ?
V1 N2 C9 C5 -1.0(5) . . . . ?
V1 N2 C9 C8 179.1(3) . . . . ?
V1 N2 C12 C11 -179.9(3) . . . . ?
O1 V1 O3 P2 84.8(7) . . . . ?
O1 V1 O5 P1 -97.4(8) . . . . ?
O1 V1 N1 C1 86.3(4) . . . . ?
O1 V1 N1 C5 -95.7(3) . . . . ?
O1 V1 N2 C9 96.4(3) . . . . ?
O1 V1 N2 C12 -84.3(4) . . . . ?
O2 V1 O3 P2 -101.0(7) . . . . ?
O2 V1 O5 P1 87.4(7) . . . . ?
O2 V1 N1 C1 -97.7(4) . . . . ?
O2 V1 N1 C5 80.4(3) . . . . ?
O2 V1 N2 C9 -78.6(3) . . . . ?
O2 V1 N2 C12 100.7(4) . . . . ?
O3 V1 O5 P1 5.9(8) . . . . ?
O3 V1 N1 C1 -15.0(4) . . . . ?
O3 V1 N1 C5 163.1(3) . . . . ?
O3 V1 N2 C9 -51.4(5) . . . . ?
O3 V1 N2 C12 128.0(4) . . . . ?
O3 P2 O3 V1 36.5(8) 8_565 . . . ?
O3 P2 C13 C14 63.97(18) . . . . ?
O3 P2 C13 C14 -63.97(18) 8_565 . . . ?
O3 P2 C13 C15 55.1(4) 8_565 . . 8_565 ?
O3 P2 C13 C15 -176.9(3) . . . 8_565 ?
O3 P2 C13 C15 -55.1(4) . . . . ?
O3 P2 C13 C15 176.9(3) 8_565 . . . ?
O4 P2 O3 V1 158.6(6) . . . . ?
O4 P2 C13 C14 180.0 . . . . ?
O4 P2 C13 C15 60.9(3) . . . . ?
O4 P2 C13 C15 -60.9(3) . . . 8_565 ?
O5 V1 O3 P2 -18.4(7) . . . . ?
O5 V1 N1 C1 -122.9(5) . . . . ?
O5 V1 N1 C5 55.1(6) . . . . ?
O5 V1 N2 C9 -162.3(3) . . . . ?
O5 V1 N2 C12 17.0(4) . . . . ?
O5 P1 O5 V1 -17.9(9) 8_565 . . . ?
O5 P1 C16 C17 63.89(18) 8_565 . . . ?
O5 P1 C16 C17 -63.89(18) . . . . ?
O5 P1 C16 C18 55.3(4) . . . 8_565 ?
O5 P1 C16 C18 -176.9(3) 8_565 . . 8_565 ?
O5 P1 C16 C18 176.9(3) . . . . ?
O5 P1 C16 C18 -55.3(4) 8_565 . . . ?
O6 P1 O5 V1 -140.4(7) . . . . ?
O6 P1 C16 C17 180.0 . . . . ?
O6 P1 C16 C18 60.8(3) . . . . ?
O6 P1 C16 C18 -60.8(3) . . . 8_565 ?
N1 V1 O3 P2 -178.1(7) . . . . ?
N1 V1 O5 P1 112.2(8) . . . . ?
N1 V1 N2 C9 0.5(3) . . . . ?
N1 V1 N2 C12 179.8(4) . . . . ?
N1 C1 C2 C3 0.3(8) . . . . ?
N1 C5 C9 N2 1.1(6) . . . . ?
N1 C5 C9 C8 -178.9(4) . . . . ?
N2 V1 O3 P2 -127.9(6) . . . . ?
N2 V1 O5 P1 165.3(7) . . . . ?
N2 V1 N1 C1 -177.9(4) . . . . ?
N2 V1 N1 C5 0.1(3) . . . . ?
C1 N1 C5 C4 -1.3(6) . . . . ?
C1 N1 C5 C9 177.6(4) . . . . ?
C1 C2 C3 C4 -0.5(7) . . . . ?
C2 C3 C4 C5 -0.2(7) . . . . ?
C2 C3 C4 C6 -178.2(5) . . . . ?
C3 C4 C5 N1 1.2(6) . . . . ?
C3 C4 C5 C9 -177.7(4) . . . . ?
C3 C4 C6 C7 176.8(5) . . . . ?
C4 C5 C9 N2 -179.9(4) . . . . ?
C4 C5 C9 C8 0.1(6) . . . . ?
C4 C6 C7 C8 1.6(7) . . . . ?
C5 N1 C1 C2 0.6(7) . . . . ?
C5 C4 C6 C7 -1.1(7) . . . . ?
C6 C4 C5 N1 179.2(4) . . . . ?
C6 C4 C5 C9 0.3(6) . . . . ?
C6 C7 C8 C9 -1.2(7) . . . . ?
C6 C7 C8 C10 178.9(4) . . . . ?
C7 C8 C9 N2 -179.7(4) . . . . ?
C7 C8 C9 C5 0.4(6) . . . . ?
C7 C8 C10 C11 -179.3(4) . . . . ?
C8 C10 C11 C12 -1.7(7) . . . . ?
C9 N2 C12 C11 -0.6(6) . . . . ?
C9 C8 C10 C11 0.8(6) . . . . ?
C10 C8 C9 N2 0.2(6) . . . . ?
C10 C8 C9 C5 -179.7(4) . . . . ?
C10 C11 C12 N2 1.7(7) . . . . ?
C12 N2 C9 C5 179.6(4) . . . . ?
C12 N2 C9 C8 -0.3(6) . . . . ?
C13 P2 O3 V1 -89.1(7) . . . . ?
C16 P1 O5 V1 107.5(7) . . . . ?
_database_code_depnum_ccdc_archive 'CCDC 990482'
#######################################################################
#
#                 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.
# 
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#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
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#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_2
_audit_creation_date             2014-05-10
_audit_creation_method           
;
Olex2 1.2
(compiled 2014.03.20 svn.r2914 for OlexSys, GUI svn.r4816)
;
_shelxl_version_number           2013-3
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C28 H41 N4 O11 P2 V2, 2(Cl)'
_chemical_formula_sum            'C28 H41 Cl2 N4 O11 P2 V2'
_chemical_formula_weight         844.37
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 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'
P P 0.1023 0.0942 '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'
V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_H-M_alt        'P n m a'
_space_group_name_Hall           '-P 2ac 2n'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-x, y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'-x-1/2, y-1/2, z-1/2'
'x, -y-1/2, z'

_cell_length_a                   23.066(5)
_cell_length_b                   14.961(5)
_cell_length_c                   10.893(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3759(2)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    3565
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.61
_cell_measurement_theta_min      2.23
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.783
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.503776
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS v.2.10 (Bruker,2003) was used for absorption correction.
R(int) was 0.0440 before and 0.0268 after correction.
The Ratio of minimum to maximum transmission is 0.5038.
The λ/2 correction factor is 0.0015.
;
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.492
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1740
_exptl_crystal_size_max          0.092
_exptl_crystal_size_mid          0.086
_exptl_crystal_size_min          0.082
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0585
_diffrn_reflns_av_unetI/netI     0.0413
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            19194
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.240
_diffrn_reflns_theta_max         25.345
_diffrn_reflns_theta_min         4.078
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2939
_reflns_number_total             3570
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v6.45A (Bruker, 2003)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT v6.45A (Bruker, 2003)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         2.288
_refine_diff_density_min         -1.255
_refine_diff_density_rms         0.164
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     252
_refine_ls_number_reflns         3570
_refine_ls_number_restraints     95
_refine_ls_R_factor_all          0.1351
_refine_ls_R_factor_gt           0.1182
_refine_ls_restrained_S_all      1.128
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1054P)²+64.1964P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2723
_refine_ls_wR_factor_ref         0.2865
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All C(H,H,H,H) groups, All O(H) groups, All O(H,H) groups
2. Restrained distances
 C16-C14
 1.54 with sigma of 0.02
 C15-C14
 1.54 with sigma of 0.02
 C14-C17
 1.54 with sigma of 0.02
 H6A-O6
 0.83 with sigma of 0.02
 C17-C16
 2.5 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
Uanis(C13) \\sim Ueq, Uanis(C12) \\sim Ueq, Uanis(C11) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.002
Uanis(C3) \\sim Ueq, Uanis(C1) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.002
Uanis(O6) \\sim Ueq, Uanis(O5) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.002
Uanis(O2) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.002
Uanis(C14) \\sim Ueq, Uanis(C15) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.002
Uanis(C16) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.002
Uanis(C17) \\sim Ueq: with sigma of 0.007 and sigma for terminal atoms of 0.002
Uanis(O2) \\sim Ueq, Uanis(O5) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.002
Uanis(Cl1) \\sim Ueq, Uanis(Cl2) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.002
Uanis(O5) \\sim Ueq, Uanis(O2) \\sim Ueq: with sigma of 0.003 and sigma for
terminal atoms of 0.002
Uanis(O4) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.002
4. Others
 Fixed Sof: H15A(0.5) H15B(0.5) H15C(0.5) H3C(0.5) H3D(0.5) H3E(0.5) C16(0.5)
 H16A(0.5) H16B(0.5) H16C(0.5) C17(0.5) H17A(0.5) H17B(0.5) H17C(0.5)
5.a Riding coordinates:
 C3(H3C,H3D,H3E)
5.b Rotating group:
 O3(H3A,H3B)
5.c Aromatic/amide H refined with riding coordinates:
 C4(H4), C7(H7), C10(H10), C6(H6), C5(H5), C13(H13), C11(H11), C12(H12)
5.d Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), C1(H1A,H1B,H1C), C16(H16A,H16B,H16C), C17(H17A,H17B,H17C)
5.e Idealised tetrahedral OH refined as rotating group:
 O1(H1)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
V1 V 0.16621(6) 0.08138(9) 0.78619(14) 0.0383(5) Uani 1 1 d . . . . .
P2 P 0.15431(11) 0.2500 0.5799(2) 0.0189(6) Uani 1 2 d S T P . .
Cl2 Cl -0.00594(11) 0.2500 0.6787(2) 0.0317(6) Uani 1 2 d S TU P . .
P1 P 0.21539(11) 0.2500 0.9637(2) 0.0305(7) Uani 1 2 d S T P . .
Cl1 Cl 0.06225(13) 0.2500 1.0845(3) 0.0434(8) Uani 1 2 d S TU P . .
N1 N 0.1411(3) -0.0024(4) 0.9332(6) 0.0263(14) Uani 1 1 d . . . . .
O3 O 0.0781(2) 0.1365(4) 0.8460(5) 0.0384(14) Uani 1 1 d . . . . .
H3A H 0.0686 0.1493 0.9195 0.058 Uiso 1 1 d GR . . . .
H3B H 0.0497 0.1473 0.7983 0.058 Uiso 1 1 d GR . . . .
O2 O 0.1965(3) 0.1678(4) 0.9029(7) 0.0529(17) Uani 1 1 d . U . . .
O4 O 0.2221(3) 0.0275(4) 0.7455(7) 0.0509(16) Uani 1 1 d . U . . .
N2 N 0.1060(4) -0.0063(5) 0.7026(7) 0.0441(19) Uani 1 1 d . . . . .
C2 C 0.2072(5) 0.2500 0.4562(10) 0.027(2) Uani 1 2 d S T P . .
C4 C 0.1610(3) 0.0015(5) 1.0479(8) 0.0314(18) Uani 1 1 d . . . . .
H4 H 0.1914 0.0405 1.0643 0.038 Uiso 1 1 calc R . . . .
C9 C 0.0783(4) -0.0633(6) 0.7789(8) 0.039(2) Uani 1 1 d . . . . .
C7 C 0.0728(3) -0.1116(6) 1.0008(8) 0.0347(18) Uani 1 1 d . . . . .
H7 H 0.0424 -0.1505 0.9829 0.042 Uiso 1 1 calc R . . . .
C15 C 0.3211(6) 0.2500 0.8605(12) 0.048(3) Uani 1 2 d DS TU P . .
H15A H 0.3610 0.2668 0.8701 0.072 Uiso 0.5 1 calc GR . . A -1
H15B H 0.3021 0.2919 0.8073 0.072 Uiso 0.5 1 calc GR . . A -1
H15C H 0.3190 0.1913 0.8253 0.072 Uiso 0.5 1 calc GR . . A -1
C10 C 0.0358(5) -0.1190(7) 0.7358(9) 0.052(2) Uani 1 1 d . . . . .
H10 H 0.0157 -0.1561 0.7896 0.062 Uiso 1 1 calc R . . . .
C6 C 0.0939(4) -0.1055(6) 1.1190(8) 0.0365(19) Uani 1 1 d . . . . .
H6 H 0.0776 -0.1395 1.1817 0.044 Uiso 1 1 calc R . . . .
C5 C 0.1396(4) -0.0481(6) 1.1432(8) 0.0372(19) Uani 1 1 d . . . . .
H5 H 0.1552 -0.0435 1.2216 0.045 Uiso 1 1 calc R . . . .
C8 C 0.0969(3) -0.0597(5) 0.9092(7) 0.0277(16) Uani 1 1 d . . . . .
C13 C 0.0928(6) -0.0069(9) 0.5823(11) 0.074(3) Uani 1 1 d . U . . .
H13 H 0.1113 0.0333 0.5303 0.089 Uiso 1 1 calc R . . . .
C1 C 0.1991(5) 0.1667(7) 0.3791(10) 0.056(3) Uani 1 1 d . U . . .
H1A H 0.2023 0.1147 0.4304 0.084 Uiso 1 1 calc GR . . . .
H1B H 0.2284 0.1646 0.3165 0.084 Uiso 1 1 calc GR . . . .
H1C H 0.1615 0.1679 0.3414 0.084 Uiso 1 1 calc GR . . . .
C11 C 0.0227(6) -0.1196(10) 0.6107(11) 0.079(4) Uani 1 1 d . U . . .
H11 H -0.0062 -0.1568 0.5801 0.095 Uiso 1 1 calc R . . . .
C12 C 0.0529(7) -0.0650(11) 0.5341(12) 0.088(4) Uani 1 1 d . U . . .
H12 H 0.0466 -0.0670 0.4498 0.106 Uiso 1 1 calc R . . . .
C14 C 0.2922(6) 0.2500 0.9823(11) 0.055(4) Uani 1 2 d DS TU P C .
C3 C 0.2670(8) 0.2500 0.5152(16) 0.068(4) Uani 1 2 d S TU P . .
H3C H 0.2859 0.1942 0.4980 0.102 Uiso 0.5 1 d R . . B -1
H3D H 0.2634 0.2576 0.6023 0.102 Uiso 0.5 1 d R . . B -1
H3E H 0.2894 0.2982 0.4817 0.102 Uiso 0.5 1 d R . . B -1
O5 O 0.1587(4) 0.1683(5) 0.6516(7) 0.069(2) Uani 1 1 d . U . . .
O6 O 0.0962(6) 0.2500 0.5114(12) 0.077(3) Uani 1 2 d DS TU P . .
O1 O 0.1922(5) 0.2137(7) 1.0953(10) 0.096(3) Uani 1 1 d . . . C -1
H1 H 0.1586 0.1967 1.0882 0.144 Uiso 1 1 calc GR . . C -1
C16 C 0.3124(8) 0.2891(11) 1.0957(14) 0.043(4) Uani 0.5 1 d D U . C -1
H16A H 0.3524 0.2738 1.1081 0.065 Uiso 0.5 1 calc GR . . C -1
H16B H 0.2897 0.2665 1.1627 0.065 Uiso 0.5 1 calc GR . . C -1
H16C H 0.3085 0.3529 1.0916 0.065 Uiso 0.5 1 calc GR . . C -1
C17 C 0.3076(11) 0.1420(11) 1.002(2) 0.071(6) Uani 0.5 1 d D U . . .
H17A H 0.3488 0.1342 1.0052 0.107 Uiso 0.5 1 calc GR . . C .
H17B H 0.2921 0.1083 0.9342 0.107 Uiso 0.5 1 calc GR . . . .
H17C H 0.2905 0.1214 1.0770 0.107 Uiso 0.5 1 calc GR . . . .
H6A H 0.065(5) 0.2500 0.550(17) 0.107 Uiso 1 2 d DRS T P . .


_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 N1 2.115(6) . ?
V1 O3 2.288(6) . ?
V1 O2 1.944(7) . ?
V1 O4 1.584(7) . ?
V1 N2 2.115(8) . ?
V1 O5 1.967(8) . ?
P2 C2 1.818(11) . ?
P2 O5 1.455(8) . ?
P2 O5 1.455(8) 8_565 ?
P2 O6 1.533(14) . ?
P1 O2 1.463(7) . ?
P1 O2 1.463(7) 8_565 ?
P1 C14 1.784(14) . ?
P1 O1 1.623(10) . ?
N1 C4 1.331(10) . ?
N1 C8 1.357(10) . ?
O3 H3A 0.8520 . ?
O3 H3B 0.8508 . ?
N2 C9 1.352(11) . ?
N2 C13 1.346(14) . ?
C2 C1 1.515(12) . ?
C2 C1 1.515(12) 8_565 ?
C2 C3 1.52(2) . ?
C4 H4 0.9300 . ?
C4 C5 1.368(11) . ?
C9 C10 1.369(13) . ?
C9 C8 1.485(12) . ?
C7 H7 0.9300 . ?
C7 C6 1.379(12) . ?
C7 C8 1.382(11) . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C15 C14 1.484(14) . ?
C10 H10 0.9300 . ?
C10 C11 1.397(15) . ?
C6 H6 0.9300 . ?
C6 C5 1.385(12) . ?
C5 H5 0.9300 . ?
C13 H13 0.9300 . ?
C13 C12 1.370(19) . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C11 H11 0.9300 . ?
C11 C12 1.360(19) . ?
C12 H12 0.9300 . ?
C14 C16 1.443(14) . ?
C14 C17 1.667(16) 8_565 ?
C14 C17 1.667(16) . ?
C3 H3C 0.9600 . ?
C3 H3D 0.9598 . ?
C3 H3E 0.9596 . ?
O6 H6A 0.83(2) . ?
O1 H1 0.8200 . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C16 C17 1.46(3) 8_565 ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 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
N1 V1 O3 75.8(2) . . ?
N1 V1 N2 77.2(3) . . ?
O2 V1 N1 89.9(3) . . ?
O2 V1 O3 83.9(3) . . ?
O2 V1 N2 158.4(3) . . ?
O2 V1 O5 94.5(3) . . ?
O4 V1 N1 97.6(3) . . ?
O4 V1 O3 170.5(3) . . ?
O4 V1 O2 103.2(3) . . ?
O4 V1 N2 95.6(3) . . ?
O4 V1 O5 101.5(3) . . ?
N2 V1 O3 76.3(3) . . ?
O5 V1 N1 158.8(3) . . ?
O5 V1 O3 84.0(3) . . ?
O5 V1 N2 91.8(3) . . ?
O5 P2 C2 110.6(4) 8_565 . ?
O5 P2 C2 110.6(4) . . ?
O5 P2 O5 114.4(7) . 8_565 ?
O5 P2 O6 108.8(4) . . ?
O5 P2 O6 108.8(4) 8_565 . ?
O6 P2 C2 103.1(6) . . ?
O2 P1 O2 114.4(6) . 8_565 ?
O2 P1 C14 110.3(3) . . ?
O2 P1 C14 110.3(3) 8_565 . ?
O2 P1 O1 125.7(5) 8_565 . ?
O2 P1 O1 91.2(5) . . ?
O1 P1 C14 103.2(5) . . ?
C4 N1 V1 126.2(5) . . ?
C4 N1 C8 117.8(6) . . ?
C8 N1 V1 115.7(5) . . ?
V1 O3 H3A 125.3 . . ?
V1 O3 H3B 125.2 . . ?
H3A O3 H3B 109.5 . . ?
P1 O2 V1 164.3(5) . . ?
C9 N2 V1 115.9(6) . . ?
C13 N2 V1 124.9(8) . . ?
C13 N2 C9 119.1(9) . . ?
C1 C2 P2 109.1(6) 8_565 . ?
C1 C2 P2 109.1(6) . . ?
C1 C2 C1 110.7(11) 8_565 . ?
C1 C2 C3 110.3(7) 8_565 . ?
C1 C2 C3 110.3(7) . . ?
C3 C2 P2 107.2(9) . . ?
N1 C4 H4 117.8 . . ?
N1 C4 C5 124.4(7) . . ?
C5 C4 H4 117.8 . . ?
N2 C9 C10 120.8(9) . . ?
N2 C9 C8 115.3(8) . . ?
C10 C9 C8 123.8(8) . . ?
C6 C7 H7 120.2 . . ?
C6 C7 C8 119.6(7) . . ?
C8 C7 H7 120.2 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C14 C15 H15A 109.5 . . ?
C14 C15 H15B 109.5 . . ?
C14 C15 H15C 109.5 . . ?
C9 C10 H10 120.2 . . ?
C9 C10 C11 119.5(10) . . ?
C11 C10 H10 120.2 . . ?
C7 C6 H6 120.4 . . ?
C7 C6 C5 119.1(7) . . ?
C5 C6 H6 120.4 . . ?
C4 C5 C6 117.8(8) . . ?
C4 C5 H5 121.1 . . ?
C6 C5 H5 121.1 . . ?
N1 C8 C9 115.1(7) . . ?
N1 C8 C7 121.2(7) . . ?
C7 C8 C9 123.6(7) . . ?
N2 C13 H13 119.0 . . ?
N2 C13 C12 122.0(12) . . ?
C12 C13 H13 119.0 . . ?
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
C2 C1 H1C 109.5 . . ?
H1A C1 H1B 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C10 C11 H11 120.5 . . ?
C12 C11 C10 119.0(12) . . ?
C12 C11 H11 120.5 . . ?
C13 C12 H12 120.3 . . ?
C11 C12 C13 119.3(12) . . ?
C11 C12 H12 120.3 . . ?
C15 C14 P1 110.2(9) . . ?
C15 C14 C17 91.0(10) . 8_565 ?
C15 C14 C17 91.0(10) . . ?
C16 C14 P1 114.6(10) . . ?
C16 C14 C15 128.3(12) . . ?
C16 C14 C17 55.3(11) . 8_565 ?
C16 C14 C17 102.4(12) . . ?
C17 C14 P1 103.0(10) 8_565 . ?
C17 C14 P1 103.0(10) . . ?
C17 C14 C17 151.4(19) 8_565 . ?
C2 C3 H3C 109.3 . . ?
C2 C3 H3D 109.9 . . ?
C2 C3 H3E 109.2 . . ?
H3C C3 H3D 109.5 . . ?
H3C C3 H3E 109.5 . . ?
H3D C3 H3E 109.5 . . ?
P2 O5 V1 164.2(6) . . ?
P2 O6 H6A 120(10) . . ?
P1 O1 H1 109.5 . . ?
C14 C16 H16A 109.5 . . ?
C14 C16 H16B 109.5 . . ?
C14 C16 H16C 109.5 . . ?
C14 C16 C17 70.2(10) . 8_565 ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C17 C16 H16A 109.9 8_565 . ?
C17 C16 H16B 137.9 8_565 . ?
C17 C16 H16C 42.0 8_565 . ?
C14 C17 H17A 109.5 . . ?
C14 C17 H17B 109.5 . . ?
C14 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
V1 N1 C4 C5 173.3(6) . . . . ?
V1 N1 C8 C9 8.0(8) . . . . ?
V1 N1 C8 C7 -173.6(6) . . . . ?
V1 N2 C9 C10 175.8(7) . . . . ?
V1 N2 C9 C8 -3.5(10) . . . . ?
V1 N2 C13 C12 -179.4(11) . . . . ?
P1 C14 C16 C17 -89.1(13) . . . 8_565 ?
N1 C4 C5 C6 -0.7(13) . . . . ?
O2 P1 O2 V1 12(2) 8_565 . . . ?
O2 P1 C14 C15 63.6(4) . . . . ?
O2 P1 C14 C15 -63.6(4) 8_565 . . . ?
O2 P1 C14 C16 89.9(10) 8_565 . . . ?
O2 P1 C14 C16 -142.8(9) . . . . ?
O2 P1 C14 C17 -32.4(11) . . . . ?
O2 P1 C14 C17 32.4(11) 8_565 . . 8_565 ?
O2 P1 C14 C17 159.6(10) . . . 8_565 ?
O2 P1 C14 C17 -159.6(10) 8_565 . . . ?
N2 C9 C10 C11 2.9(16) . . . . ?
N2 C9 C8 N1 -2.9(11) . . . . ?
N2 C9 C8 C7 178.7(8) . . . . ?
N2 C13 C12 C11 5(2) . . . . ?
C2 P2 O5 V1 127(2) . . . . ?
C4 N1 C8 C9 -177.8(7) . . . . ?
C4 N1 C8 C7 0.6(11) . . . . ?
C9 N2 C13 C12 -1.4(19) . . . . ?
C9 C10 C11 C12 0(2) . . . . ?
C7 C6 C5 C4 1.3(13) . . . . ?
C15 C14 C16 C17 58.7(16) . . . 8_565 ?
C10 C9 C8 N1 177.8(8) . . . . ?
C10 C9 C8 C7 -0.6(14) . . . . ?
C10 C11 C12 C13 -4(2) . . . . ?
C6 C7 C8 N1 -0.1(12) . . . . ?
C6 C7 C8 C9 178.2(8) . . . . ?
C8 N1 C4 C5 -0.2(11) . . . . ?
C8 C9 C10 C11 -177.9(10) . . . . ?
C8 C7 C6 C5 -0.9(13) . . . . ?
C13 N2 C9 C10 -2.3(15) . . . . ?
C13 N2 C9 C8 178.3(9) . . . . ?
C14 P1 O2 V1 -112.7(17) . . . . ?
O5 P2 C2 C1 55.6(9) . . . . ?
O5 P2 C2 C1 176.7(7) . . . 8_565 ?
O5 P2 C2 C1 -55.6(9) 8_565 . . 8_565 ?
O5 P2 C2 C1 -176.7(7) 8_565 . . . ?
O5 P2 C2 C3 -63.9(4) . . . . ?
O5 P2 C2 C3 63.9(4) 8_565 . . . ?
O5 P2 O5 V1 2(3) 8_565 . . . ?
O6 P2 C2 C1 -60.6(7) . . . . ?
O6 P2 C2 C1 60.6(7) . . . 8_565 ?
O6 P2 C2 C3 180.000(1) . . . . ?
O6 P2 O5 V1 -120(2) . . . . ?
O1 P1 O2 V1 142.8(17) . . . . ?
O1 P1 C14 C15 159.9(4) . . . . ?
O1 P1 C14 C16 -46.6(9) . . . . ?
O1 P1 C14 C17 63.9(11) . . . . ?
O1 P1 C14 C17 -104.1(11) . . . 8_565 ?
C17 C14 C16 C17 160(2) . . . 8_565 ?
_database_code_depnum_ccdc_archive 'CCDC 990483'
#######################################################################
#
#                 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
_audit_creation_date             2014-05-10
_audit_creation_method           
;
Olex2 1.2
(compiled 2014.03.20 svn.r2914 for OlexSys, GUI svn.r4816)
;
_shelxl_version_number           2013-3
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         '2(C24 H25 N4 O7 P V2), 3(C H4 O)'
_chemical_formula_sum            'C51 H62 N8 O17 P2 V4'
_chemical_formula_weight         1324.78
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 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'
P P 0.1023 0.0942 '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'

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

_cell_length_a                   9.765(3)
_cell_length_b                   12.448(4)
_cell_length_c                   14.734(4)
_cell_angle_alpha                66.947(5)
_cell_angle_beta                 84.914(6)
_cell_angle_gamma                80.991(5)
_cell_volume                     1626.9(8)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    2000
_cell_measurement_temperature    100
_cell_measurement_theta_max      26.28
_cell_measurement_theta_min      2.58
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.673
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.400757
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS v.2.10 (Bruker,2003) was used for absorption correction.
R(int) was 0.0848 before and 0.0338 after correction.
The Ratio of minimum to maximum transmission is 0.4008.
The λ/2 correction factor is 0.0015.
;
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.352
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             682
_exptl_crystal_size_max          0.068
_exptl_crystal_size_mid          0.062
_exptl_crystal_size_min          0.06
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0402
_diffrn_reflns_av_unetI/netI     0.0937
_diffrn_reflns_Laue_measured_fraction_full 0.978
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            10470
_diffrn_reflns_point_group_measured_fraction_full 0.978
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.025
_diffrn_reflns_theta_min         4.205
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3588
_reflns_number_total             5608
_reflns_special_details          
;
 Data were apparently pre-merged, so _diffrn_reflns_number
 etc. will have to be added later.
 
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v6.45A (Bruker, 2003)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT v6.45A (Bruker, 2003)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'SIR97 (Burla et al., 2007)'
_refine_diff_density_max         1.477
_refine_diff_density_min         -0.802
_refine_diff_density_rms         0.183
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     385
_refine_ls_number_reflns         5608
_refine_ls_number_restraints     121
_refine_ls_R_factor_all          0.1292
_refine_ls_R_factor_gt           0.0967
_refine_ls_restrained_S_all      1.284
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.2000P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2693
_refine_ls_wR_factor_ref         0.3054
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 O9-C27
 1.4 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(V2) \\sim Ueq, Uanis(V1) \\sim Ueq, Uanis(P1) \\sim Ueq: with sigma of
0.002 and sigma for terminal atoms of 0.002
Uanis(O9) \\sim Ueq, Uanis(C27) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.002
Uanis(C10) \\sim Ueq, Uanis(C9) \\sim Ueq, Uanis(C8) \\sim Ueq, Uanis(C7) \\sim
Ueq, Uanis(C6) \\sim Ueq, Uanis(N2) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.002
Uanis(C16) \\sim Ueq, Uanis(C15) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.002
Uanis(O8) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.002
Uanis(O4) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.002
Uanis(O7) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.002
Uanis(C22) \\sim Ueq, Uanis(C23) \\sim Ueq, Uanis(C21) \\sim Ueq, Uanis(C24)
\\sim Ueq: with sigma of 0.007 and sigma for terminal atoms of 0.002
4. Others
 Fixed Sof: C27(0.5) H27A(0.5) H27B(0.5) H27C(0.5) O9(0.5) H9A(0.5)
5.a Riding coordinates:
 O9(H9A)
5.b Aromatic/amide H refined with riding coordinates:
 C9(H9), C1(H1), C2(H2), C14(H14), C10(H10), C17(H17), C4(H4), C3(H3), C8(H8),
 C13(H13), C19(H19), C7(H7), C11(H11), C12(H12), C18(H18), C20(H20)
5.c Idealised Me refined as rotating group:
 C22(H22A,H22B,H22C), C24(H24A,H24B,H24C), C23(H23A,H23B,H23C), C25(H25A,H25B,
 H25C), C27(H27A,H27B,H27C)
5.d Idealised tetrahedral OH refined as rotating group:
 O8(H8A)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
V1 V 0.23699(10) 0.21760(8) 0.42677(9) 0.0370(4) Uani 1 1 d . U . . .
V2 V 0.47106(11) 0.37639(9) 0.36370(10) 0.0491(4) Uani 1 1 d . U . . .
P1 P 0.23639(18) 0.42394(15) 0.21709(16) 0.0517(6) Uani 1 1 d . U . . .
O1 O 0.1567(4) 0.1086(3) 0.4365(3) 0.0394(11) Uani 1 1 d . . . . .
O3 O 0.4016(4) 0.1857(3) 0.3941(3) 0.0381(10) Uani 1 1 d . . . . .
O4 O 0.3291(4) 0.3763(4) 0.4336(4) 0.0509(13) Uani 1 1 d . U . . .
C9 C -0.1399(7) 0.4211(5) 0.5086(7) 0.053(2) Uani 1 1 d . U . . .
H9 H -0.2170 0.4749 0.4757 0.063 Uiso 1 1 calc R . . . .
O2 O 0.5343(5) 0.4961(4) 0.3462(5) 0.0682(17) Uani 1 1 d . . . . .
O5 O 0.1641(4) 0.3365(4) 0.3081(4) 0.0490(13) Uani 1 1 d . . . . .
O6 O 0.1640(5) 0.5473(4) 0.1897(5) 0.0688(17) Uani 1 1 d . . . . .
O7 O 0.3928(5) 0.4133(4) 0.2376(4) 0.0575(14) Uani 1 1 d . U . . .
N1 N 0.2867(5) 0.1426(4) 0.5788(4) 0.0377(13) Uani 1 1 d . . . . .
C1 C 0.3937(6) 0.0588(5) 0.6129(5) 0.0352(14) Uani 1 1 d . . . . .
H1 H 0.4492 0.0323 0.5675 0.042 Uiso 1 1 calc R . . . .
N2 N 0.0718(5) 0.2960(4) 0.5033(5) 0.0457(15) Uani 1 1 d . U . . .
N4 N 0.6513(5) 0.2784(4) 0.3143(5) 0.0467(15) Uani 1 1 d . . . . .
O8 O 0.9042(6) 0.6536(5) 0.1454(4) 0.0713(16) Uani 1 1 d . U . . .
H8A H 0.9207 0.6314 0.0981 0.107 Uiso 1 1 calc GR . . . .
C5 C 0.2055(6) 0.1790(5) 0.6443(6) 0.0429(17) Uani 1 1 d . . . . .
C2 C 0.4276(7) 0.0088(6) 0.7108(5) 0.0433(16) Uani 1 1 d . . . . .
H2 H 0.5038 -0.0517 0.7329 0.052 Uiso 1 1 calc R . . . .
N3 N 0.5922(5) 0.2752(4) 0.4910(5) 0.0480(16) Uani 1 1 d . . . . .
C16 C 0.7037(6) 0.2005(5) 0.4855(6) 0.0413(16) Uani 1 1 d . U . . .
C14 C 0.8455(7) 0.1296(6) 0.3616(6) 0.0474(18) Uani 1 1 d . . . . .
H14 H 0.9045 0.0743 0.4116 0.057 Uiso 1 1 calc R . . . .
C10 C -0.0400(7) 0.3722(6) 0.4548(6) 0.0510(19) Uani 1 1 d . U . . .
H10 H -0.0502 0.3917 0.3864 0.061 Uiso 1 1 calc R . . . .
C21 C 0.2291(7) 0.3748(6) 0.1165(5) 0.0540(19) Uani 1 1 d . U . . .
C6 C 0.0847(6) 0.2662(6) 0.6013(6) 0.0424(16) Uani 1 1 d . U . . .
C17 C 0.7808(7) 0.1319(6) 0.5685(6) 0.053(2) Uani 1 1 d . . . . .
H17 H 0.8586 0.0776 0.5642 0.063 Uiso 1 1 calc R . . . .
C15 C 0.7369(6) 0.2001(5) 0.3851(5) 0.0418(16) Uani 1 1 d . U . . .
C22 C 0.0741(8) 0.3708(7) 0.1017(6) 0.058(2) Uani 1 1 d . U . . .
H22A H 0.0348 0.3161 0.1627 0.087 Uiso 1 1 calc GR . . . .
H22B H 0.0680 0.3441 0.0480 0.087 Uiso 1 1 calc GR . . . .
H22C H 0.0220 0.4497 0.0850 0.087 Uiso 1 1 calc GR . . . .
C4 C 0.2369(7) 0.1354(7) 0.7415(6) 0.0532(19) Uani 1 1 d . . . . .
H4 H 0.1820 0.1645 0.7855 0.064 Uiso 1 1 calc R . . . .
C3 C 0.3479(7) 0.0492(7) 0.7758(6) 0.0521(18) Uani 1 1 d . . . . .
H3 H 0.3693 0.0178 0.8437 0.062 Uiso 1 1 calc R . . . .
C8 C -0.1273(7) 0.3930(6) 0.6038(8) 0.059(2) Uani 1 1 d . U . . .
H8 H -0.1960 0.4263 0.6386 0.071 Uiso 1 1 calc R . . . .
C13 C 0.8675(6) 0.1395(6) 0.2676(6) 0.0504(19) Uani 1 1 d . . . . .
H13 H 0.9436 0.0923 0.2508 0.060 Uiso 1 1 calc R . . . .
C19 C 0.6272(8) 0.2237(7) 0.6612(7) 0.055(2) Uani 1 1 d . . . . .
H19 H 0.5984 0.2328 0.7214 0.065 Uiso 1 1 calc R . . . .
C7 C -0.0131(7) 0.3141(6) 0.6551(6) 0.0522(19) Uani 1 1 d . U . . .
H7 H -0.0033 0.2945 0.7235 0.063 Uiso 1 1 calc R . . . .
C24 C 0.3135(9) 0.2523(7) 0.1397(6) 0.064(2) Uani 1 1 d . U . . .
H24A H 0.4121 0.2577 0.1418 0.095 Uiso 1 1 calc GR . . . .
H24B H 0.2998 0.2239 0.0883 0.095 Uiso 1 1 calc GR . . . .
H24C H 0.2822 0.1974 0.2038 0.095 Uiso 1 1 calc GR . . . .
C11 C 0.6723(7) 0.2868(6) 0.2222(6) 0.053(2) Uani 1 1 d . . . . .
H11 H 0.6120 0.3415 0.1727 0.064 Uiso 1 1 calc R . . . .
C12 C 0.7815(8) 0.2167(7) 0.1963(6) 0.062(2) Uani 1 1 d . . . . .
H12 H 0.7956 0.2228 0.1299 0.075 Uiso 1 1 calc R . . . .
C18 C 0.7436(7) 0.1434(6) 0.6571(6) 0.054(2) Uani 1 1 d . . . . .
H18 H 0.7957 0.0978 0.7143 0.065 Uiso 1 1 calc R . . . .
C20 C 0.5575(7) 0.2871(6) 0.5784(7) 0.055(2) Uani 1 1 d . . . . .
H20 H 0.4803 0.3429 0.5809 0.066 Uiso 1 1 calc R . . . .
C23 C 0.2905(11) 0.4615(9) 0.0225(7) 0.080(3) Uani 1 1 d . U . . .
H23A H 0.2417 0.5409 0.0089 0.121 Uiso 1 1 calc GR . . . .
H23B H 0.2802 0.4387 -0.0328 0.121 Uiso 1 1 calc GR . . . .
H23C H 0.3892 0.4604 0.0311 0.121 Uiso 1 1 calc GR . . . .
C25 C 0.8026(8) 0.5867(7) 0.2129(7) 0.067(2) Uani 1 1 d . . . . .
H25A H 0.8188 0.5784 0.2802 0.101 Uiso 1 1 calc GR . . . .
H25B H 0.8111 0.5085 0.2102 0.101 Uiso 1 1 calc GR . . . .
H25C H 0.7092 0.6280 0.1939 0.101 Uiso 1 1 calc GR . . . .
C27 C 0.4138(15) 0.7222(14) 0.0852(12) 0.061(4) Uani 0.5 1 d D U P . .
H27A H 0.4780 0.6640 0.1337 0.092 Uiso 0.5 1 calc GR . P . .
H27B H 0.4551 0.7952 0.0521 0.092 Uiso 0.5 1 calc GR . P . .
H27C H 0.3957 0.6913 0.0362 0.092 Uiso 0.5 1 calc GR . P . .
O9 O 0.2879(10) 0.7452(8) 0.1335(7) 0.055(2) Uani 0.5 1 d D U P . .
H9A H 0.2256 0.7217 0.1155 0.082 Uiso 0.5 1 d R . P . .


_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 V2 3.0976(16) . ?
V1 O1 1.624(4) . ?
V1 O3 1.670(4) . ?
V1 O4 2.335(4) . ?
V1 O5 1.902(5) . ?
V1 N1 2.130(6) . ?
V1 N2 2.207(6) . ?
V2 O3 2.432(4) . ?
V2 O4 1.652(5) . ?
V2 O2 1.621(5) . ?
V2 O7 1.929(5) . ?
V2 N4 2.217(6) . ?
V2 N3 2.141(6) . ?
P1 O5 1.553(5) . ?
P1 O6 1.498(5) . ?
P1 O7 1.558(5) . ?
P1 C21 1.821(9) . ?
C9 H9 0.9500 . ?
C9 C10 1.417(10) . ?
C9 C8 1.318(12) . ?
N1 C1 1.331(7) . ?
N1 C5 1.364(8) . ?
C1 H1 0.9500 . ?
C1 C2 1.377(9) . ?
N2 C10 1.373(8) . ?
N2 C6 1.355(9) . ?
N4 C15 1.357(8) . ?
N4 C11 1.319(10) . ?
O8 H8A 0.8400 . ?
O8 C25 1.450(9) . ?
C5 C6 1.471(9) . ?
C5 C4 1.362(10) . ?
C2 H2 0.9500 . ?
C2 C3 1.377(9) . ?
N3 C16 1.335(8) . ?
N3 C20 1.360(10) . ?
C16 C17 1.391(9) . ?
C16 C15 1.488(10) . ?
C14 H14 0.9500 . ?
C14 C15 1.377(9) . ?
C14 C13 1.343(11) . ?
C10 H10 0.9500 . ?
C21 C22 1.560(10) . ?
C21 C24 1.539(10) . ?
C21 C23 1.525(11) . ?
C6 C7 1.398(9) . ?
C17 H17 0.9500 . ?
C17 C18 1.379(11) . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C4 H4 0.9500 . ?
C4 C3 1.374(10) . ?
C3 H3 0.9500 . ?
C8 H8 0.9500 . ?
C8 C7 1.416(11) . ?
C13 H13 0.9500 . ?
C13 C12 1.359(10) . ?
C19 H19 0.9500 . ?
C19 C18 1.405(10) . ?
C19 C20 1.342(11) . ?
C7 H7 0.9500 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C11 H11 0.9500 . ?
C11 C12 1.394(11) . ?
C12 H12 0.9500 . ?
C18 H18 0.9500 . ?
C20 H20 0.9500 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C27 O9 1.412(13) . ?
O9 H9A 0.8200 . ?

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 V2 157.20(17) . . ?
O1 V1 O3 107.1(2) . . ?
O1 V1 O4 170.9(2) . . ?
O1 V1 O5 101.3(2) . . ?
O1 V1 N1 92.9(2) . . ?
O1 V1 N2 95.1(2) . . ?
O3 V1 V2 51.30(14) . . ?
O3 V1 O4 80.54(18) . . ?
O3 V1 O5 102.7(2) . . ?
O3 V1 N1 91.1(2) . . ?
O3 V1 N2 153.9(2) . . ?
O4 V1 V2 31.63(12) . . ?
O5 V1 V2 79.79(13) . . ?
O5 V1 O4 81.51(18) . . ?
O5 V1 N1 156.2(2) . . ?
O5 V1 N2 85.9(2) . . ?
N1 V1 V2 94.47(13) . . ?
N1 V1 O4 81.74(18) . . ?
N1 V1 N2 73.8(2) . . ?
N2 V1 V2 107.69(14) . . ?
N2 V1 O4 76.36(17) . . ?
O3 V2 V1 32.39(9) . . ?
O4 V2 V1 47.81(15) . . ?
O4 V2 O3 77.87(18) . . ?
O4 V2 O7 101.0(2) . . ?
O4 V2 N4 149.8(2) . . ?
O4 V2 N3 91.1(2) . . ?
O2 V2 V1 153.1(2) . . ?
O2 V2 O3 173.76(19) . . ?
O2 V2 O4 106.4(3) . . ?
O2 V2 O7 102.1(3) . . ?
O2 V2 N4 100.1(2) . . ?
O2 V2 N3 93.0(2) . . ?
O7 V2 V1 79.35(13) . . ?
O7 V2 O3 81.16(17) . . ?
O7 V2 N4 86.8(2) . . ?
O7 V2 N3 157.0(2) . . ?
N4 V2 V1 106.80(14) . . ?
N4 V2 O3 74.62(16) . . ?
N3 V2 V1 95.01(14) . . ?
N3 V2 O3 82.36(17) . . ?
N3 V2 N4 73.4(2) . . ?
O5 P1 O7 109.6(3) . . ?
O5 P1 C21 106.4(3) . . ?
O6 P1 O5 111.2(3) . . ?
O6 P1 O7 112.5(3) . . ?
O6 P1 C21 110.2(3) . . ?
O7 P1 C21 106.8(3) . . ?
V1 O3 V2 96.31(17) . . ?
V2 O4 V1 100.6(2) . . ?
C10 C9 H9 119.6 . . ?
C8 C9 H9 119.6 . . ?
C8 C9 C10 120.9(7) . . ?
P1 O5 V1 131.2(3) . . ?
P1 O7 V2 126.5(3) . . ?
C1 N1 V1 122.0(4) . . ?
C1 N1 C5 118.4(6) . . ?
C5 N1 V1 119.5(4) . . ?
N1 C1 H1 118.5 . . ?
N1 C1 C2 123.1(6) . . ?
C2 C1 H1 118.5 . . ?
C10 N2 V1 122.2(5) . . ?
C6 N2 V1 117.3(4) . . ?
C6 N2 C10 120.6(6) . . ?
C15 N4 V2 116.9(5) . . ?
C11 N4 V2 123.3(4) . . ?
C11 N4 C15 119.7(6) . . ?
C25 O8 H8A 109.5 . . ?
N1 C5 C6 114.7(6) . . ?
C4 C5 N1 121.0(6) . . ?
C4 C5 C6 124.3(6) . . ?
C1 C2 H2 121.0 . . ?
C1 C2 C3 118.0(6) . . ?
C3 C2 H2 121.0 . . ?
C16 N3 V2 120.5(5) . . ?
C16 N3 C20 119.1(6) . . ?
C20 N3 V2 120.4(4) . . ?
N3 C16 C17 120.9(7) . . ?
N3 C16 C15 114.5(6) . . ?
C17 C16 C15 124.6(6) . . ?
C15 C14 H14 120.2 . . ?
C13 C14 H14 120.2 . . ?
C13 C14 C15 119.6(7) . . ?
C9 C10 H10 120.6 . . ?
N2 C10 C9 118.8(7) . . ?
N2 C10 H10 120.6 . . ?
C22 C21 P1 108.2(5) . . ?
C24 C21 P1 110.9(5) . . ?
C24 C21 C22 110.2(6) . . ?
C23 C21 P1 109.3(6) . . ?
C23 C21 C22 109.9(6) . . ?
C23 C21 C24 108.4(7) . . ?
N2 C6 C5 114.6(6) . . ?
N2 C6 C7 121.1(6) . . ?
C7 C6 C5 124.3(7) . . ?
C16 C17 H17 120.2 . . ?
C18 C17 C16 119.6(7) . . ?
C18 C17 H17 120.2 . . ?
N4 C15 C16 114.4(6) . . ?
N4 C15 C14 120.6(7) . . ?
C14 C15 C16 125.0(6) . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22B 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C5 C4 H4 120.0 . . ?
C5 C4 C3 120.1(7) . . ?
C3 C4 H4 120.0 . . ?
C2 C3 H3 120.3 . . ?
C4 C3 C2 119.4(7) . . ?
C4 C3 H3 120.3 . . ?
C9 C8 H8 119.4 . . ?
C9 C8 C7 121.1(7) . . ?
C7 C8 H8 119.4 . . ?
C14 C13 H13 119.8 . . ?
C14 C13 C12 120.3(7) . . ?
C12 C13 H13 119.8 . . ?
C18 C19 H19 120.7 . . ?
C20 C19 H19 120.7 . . ?
C20 C19 C18 118.6(8) . . ?
C6 C7 C8 117.6(8) . . ?
C6 C7 H7 121.2 . . ?
C8 C7 H7 121.2 . . ?
C21 C24 H24A 109.5 . . ?
C21 C24 H24B 109.5 . . ?
C21 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
N4 C11 H11 119.5 . . ?
N4 C11 C12 121.0(7) . . ?
C12 C11 H11 119.5 . . ?
C13 C12 C11 118.9(8) . . ?
C13 C12 H12 120.6 . . ?
C11 C12 H12 120.6 . . ?
C17 C18 C19 118.8(7) . . ?
C17 C18 H18 120.6 . . ?
C19 C18 H18 120.6 . . ?
N3 C20 H20 118.5 . . ?
C19 C20 N3 123.0(7) . . ?
C19 C20 H20 118.5 . . ?
C21 C23 H23A 109.5 . . ?
C21 C23 H23B 109.5 . . ?
C21 C23 H23C 109.5 . . ?
H23A C23 H23B 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
O8 C25 H25A 109.5 . . ?
O8 C25 H25B 109.5 . . ?
O8 C25 H25C 109.5 . . ?
H25A C25 H25B 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
O9 C27 H27A 109.5 . . ?
O9 C27 H27B 109.5 . . ?
O9 C27 H27C 109.5 . . ?
C27 O9 H9A 109.3 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O9 H9A O6 0.82 2.17 2.716(10) 124.3 .

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
V1 N1 C1 C2 -179.9(5) . . . . ?
V1 N1 C5 C6 2.5(7) . . . . ?
V1 N1 C5 C4 -178.0(5) . . . . ?
V1 N2 C10 C9 -178.4(4) . . . . ?
V1 N2 C6 C5 -3.3(7) . . . . ?
V1 N2 C6 C7 178.2(5) . . . . ?
V2 N4 C15 C16 -5.7(6) . . . . ?
V2 N4 C15 C14 175.4(4) . . . . ?
V2 N4 C11 C12 -175.1(5) . . . . ?
V2 N3 C16 C17 -178.2(4) . . . . ?
V2 N3 C16 C15 2.9(6) . . . . ?
V2 N3 C20 C19 178.1(5) . . . . ?
O1 V1 O3 V2 171.81(19) . . . . ?
O3 V2 O4 V1 -13.85(16) . . . . ?
O4 V1 O3 V2 -13.43(17) . . . . ?
C9 C8 C7 C6 -0.7(10) . . . . ?
O2 V2 O4 V1 170.8(2) . . . . ?
O5 V1 O3 V2 65.6(2) . . . . ?
O5 P1 O7 V2 -32.8(4) . . . . ?
O5 P1 C21 C22 56.8(5) . . . . ?
O5 P1 C21 C24 -64.1(5) . . . . ?
O5 P1 C21 C23 176.5(5) . . . . ?
O6 P1 O5 V1 -131.2(4) . . . . ?
O6 P1 O7 V2 91.5(4) . . . . ?
O6 P1 C21 C22 -63.8(5) . . . . ?
O6 P1 C21 C24 175.2(5) . . . . ?
O6 P1 C21 C23 55.8(6) . . . . ?
O7 V2 O4 V1 64.5(2) . . . . ?
O7 P1 O5 V1 -6.2(5) . . . . ?
O7 P1 C21 C22 173.8(4) . . . . ?
O7 P1 C21 C24 52.8(5) . . . . ?
O7 P1 C21 C23 -66.6(6) . . . . ?
N1 V1 O3 V2 -94.87(18) . . . . ?
N1 C1 C2 C3 -1.0(10) . . . . ?
N1 C5 C6 N2 0.6(8) . . . . ?
N1 C5 C6 C7 179.1(6) . . . . ?
N1 C5 C4 C3 -3.1(10) . . . . ?
C1 N1 C5 C6 -176.3(5) . . . . ?
C1 N1 C5 C4 3.3(9) . . . . ?
C1 C2 C3 C4 1.2(10) . . . . ?
N2 V1 O3 V2 -41.5(5) . . . . ?
N2 C6 C7 C8 1.2(9) . . . . ?
N4 V2 O4 V1 -38.4(5) . . . . ?
N4 C11 C12 C13 -0.5(10) . . . . ?
C5 N1 C1 C2 -1.2(9) . . . . ?
C5 C6 C7 C8 -177.1(6) . . . . ?
C5 C4 C3 C2 0.8(11) . . . . ?
N3 V2 O4 V1 -95.8(2) . . . . ?
N3 C16 C17 C18 -1.5(9) . . . . ?
N3 C16 C15 N4 2.0(7) . . . . ?
N3 C16 C15 C14 -179.2(5) . . . . ?
C16 N3 C20 C19 -2.6(9) . . . . ?
C16 C17 C18 C19 0.6(10) . . . . ?
C14 C13 C12 C11 1.3(10) . . . . ?
C10 C9 C8 C7 0.6(10) . . . . ?
C10 N2 C6 C5 176.9(5) . . . . ?
C10 N2 C6 C7 -1.6(9) . . . . ?
C21 P1 O5 V1 108.9(4) . . . . ?
C21 P1 O7 V2 -147.5(3) . . . . ?
C6 N2 C10 C9 1.4(8) . . . . ?
C6 C5 C4 C3 176.4(7) . . . . ?
C17 C16 C15 N4 -176.8(5) . . . . ?
C17 C16 C15 C14 2.0(9) . . . . ?
C15 N4 C11 C12 -0.2(9) . . . . ?
C15 C16 C17 C18 177.2(6) . . . . ?
C15 C14 C13 C12 -1.4(10) . . . . ?
C4 C5 C6 N2 -178.9(6) . . . . ?
C4 C5 C6 C7 -0.4(10) . . . . ?
C8 C9 C10 N2 -1.0(9) . . . . ?
C13 C14 C15 N4 0.7(9) . . . . ?
C13 C14 C15 C16 -178.1(6) . . . . ?
C11 N4 C15 C16 179.1(5) . . . . ?
C11 N4 C15 C14 0.1(8) . . . . ?
C18 C19 C20 N3 1.7(10) . . . . ?
C20 N3 C16 C17 2.5(8) . . . . ?
C20 N3 C16 C15 -176.4(5) . . . . ?
C20 C19 C18 C17 -0.7(10) . . . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.232 0.000 0.000 210.4 38.1 ?
_database_code_depnum_ccdc_archive 'CCDC 990484'
#######################################################################
#
#                 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
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# 
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#  data retrieval see:
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data_4
_vrf_PLAT602_4                   
;
PROBLEM: VERY LARGE Solvent Accessible VOID(S) in Structure
RESPONSE: Disordered solvent molecules were omitted by using OLEX-2/Mask
;
_audit_creation_date             2014-04-07
_audit_creation_method           
;
Olex2 1.2
(compiled 2013.11.15 svn.r2834 for OlexSys, GUI svn.r4720)
;
_shelxl_version_number           2013-3
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C74 H60 N6 O12 P2 V3'
_chemical_formula_sum            'C74 H60 N6 O12 P2 V3'
_chemical_formula_weight         1440.04
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 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'
P P 0.1023 0.0942 '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'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_H-M_alt        'C 1 2/m 1'
_space_group_name_Hall           '-C 2y'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z'

_cell_length_a                   26.464(5)
_cell_length_b                   27.628(5)
_cell_length_c                   14.057(5)
_cell_angle_alpha                90
_cell_angle_beta                 91.213(5)
_cell_angle_gamma                90
_cell_volume                     10275(5)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    3505
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      19.14
_cell_measurement_theta_min      2.34
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.343
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.378173
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS v.2.10 (Bruker,2003) was used for absorption correction.
R(int) was 0.0634 before and 0.0316 after correction.
The Ratio of minimum to maximum transmission is 0.3782.
The λ/2 correction factor is 0.0015.
;
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    0.931
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             2964
_exptl_crystal_size_max          0.088
_exptl_crystal_size_mid          0.082
_exptl_crystal_size_min          0.078
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0793
_diffrn_reflns_av_unetI/netI     0.0936
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            27622
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.240
_diffrn_reflns_theta_max         25.499
_diffrn_reflns_theta_min         2.067
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4928
_reflns_number_total             9723
_reflns_special_details          
;
 Data were apparently pre-merged, so _diffrn_reflns_number
 etc. will have to be added later.
 
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v6.45A (Bruker, 2003)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT v6.45A (Bruker, 2003)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         1.237
_refine_diff_density_min         -0.848
_refine_diff_density_rms         0.157
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     452
_refine_ls_number_reflns         9723
_refine_ls_number_restraints     30
_refine_ls_R_factor_all          0.1673
_refine_ls_R_factor_gt           0.1179
_refine_ls_restrained_S_all      1.062
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.2000P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3111
_refine_ls_wR_factor_ref         0.3460
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C20) \\sim Ueq, Uanis(C1) \\sim Ueq, Uanis(C1Z) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.002
Uanis(C1U) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.002
Uanis(C1S) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.002
3. Others
 Fixed Sof: H5A(0.5) H5B(0.5) H9A(0.5) H9B(0.5) H11A(0.5) H11B(0.5)
4.a Riding coordinates:
 O9(H9A,H9B), O11(H11A,H11B)
4.b Rotating group:
 O5(H5A,H5B)
4.c Aromatic/amide H refined with riding coordinates:
 C13(H13), C14(H14), C16(H16), C17(H17), C1A(H1A), C1F(H1F), C1G(H1G),
 C1H(H1H), C1I(H1I), C1J(H1J), C1K(H1K), C1L(H1L), C1M(H1M), C1N(H1N), C1O(H1O),
  C1P(H1P), C1R(H1R), C1S(H1S), C1T(H1T), C1U(H1U), C1V(H1V), C1W(H1W),
 C1X(H1X), C1Z(H1Z), C1Y(H1Y), C20(H20), C2(H2)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
V1 V 0.84753(5) 0.5000 0.03311(11) 0.0591(4) Uani 1 2 d S T P . .
V2 V 0.71013(6) 0.5000 -0.17800(10) 0.0577(4) Uani 1 2 d S T P . .
V3 V 0.68579(6) 0.5000 0.15212(10) 0.0629(5) Uani 1 2 d S T P . .
P4 P 0.74656(6) 0.56825(5) 0.00374(11) 0.0568(4) Uani 1 1 d . . . . .
O O 0.73770(15) 0.55248(13) -0.0992(3) 0.0597(10) Uani 1 1 d . . . . .
O1 O 0.70350(16) 0.55287(14) 0.0668(3) 0.0627(10) Uani 1 1 d . . . . .
O2 O 0.79773(15) 0.55199(13) 0.0431(3) 0.0612(10) Uani 1 1 d . . . . .
O3 O 0.8574(2) 0.5000 -0.0783(4) 0.0684(15) Uani 1 2 d S T P . .
O4 O 0.7346(2) 0.5000 0.2241(4) 0.0759(17) Uani 1 2 d S T P . .
O5 O 0.7918(2) 0.5000 -0.2341(5) 0.0724(16) Uani 1 2 d S T P . .
H5A H 0.7964 0.4785 -0.2828 0.109 Uiso 0.5 1 d GR . P . .
H5B H 0.8154 0.4919 -0.1881 0.109 Uiso 0.5 1 d GR . P . .
N6 N 0.7040(2) 0.54781(19) -0.2965(4) 0.0723(14) Uani 1 1 d . . . . .
N7 N 0.90696(19) 0.54742(18) 0.0714(4) 0.0654(13) Uani 1 1 d . . . . .
O8 O 0.6531(3) 0.5000 -0.1505(5) 0.0816(18) Uani 1 2 d S T P . .
O9 O 0.8371(2) 0.5000 0.1938(4) 0.0753(17) Uani 1 2 d S T P . .
H9A H 0.8599 0.4819 0.2368 0.113 Uiso 0.5 1 d R . P . .
H9B H 0.8058 0.4880 0.2221 0.113 Uiso 0.5 1 d R . P . .
C10 C 0.9507(2) 0.5259(2) 0.1030(4) 0.0651(16) Uani 1 1 d . . . . .
O11 O 0.6141(3) 0.5000 0.0646(6) 0.093(2) Uani 1 2 d S T P . .
H11A H 0.5886 0.4754 0.0478 0.140 Uiso 0.5 1 d R . P . .
H11B H 0.5954 0.5246 0.0276 0.140 Uiso 0.5 1 d R . P . .
C12 C 0.7096(2) 0.5258(2) -0.3817(4) 0.0645(16) Uani 1 1 d . . . . .
C13 C 0.6560(3) 0.6362(3) -0.0561(6) 0.0794(19) Uani 1 1 d . . . . .
H13 H 0.6486 0.6120 -0.0127 0.095 Uiso 1 1 calc R . . . .
C14 C 0.7012(3) 0.5957(2) -0.2930(5) 0.085(2) Uani 1 1 d . . . . .
H14 H 0.6975 0.6112 -0.2349 0.102 Uiso 1 1 calc R . . . .
N15 N 0.6424(2) 0.5479(2) 0.2363(4) 0.0797(16) Uani 1 1 d . . . . .
C16 C 0.7127(3) 0.6917(2) -0.1253(5) 0.077(2) Uani 1 1 d . . . . .
H16 H 0.7447 0.7052 -0.1291 0.092 Uiso 1 1 calc R . . . .
C17 C 0.7177(3) 0.5243(3) -0.5553(5) 0.093(2) Uani 1 1 d . . . . .
H17 H 0.7206 0.5407 -0.6128 0.112 Uiso 1 1 calc R . . . .
C18 C 0.7132(3) 0.5518(3) -0.4688(5) 0.085(2) Uani 1 1 d . . . . .
C19 C 0.7050(2) 0.6541(2) -0.0619(5) 0.0658(16) Uani 1 1 d . . . . .
C1A C 0.7685(3) 0.6338(2) 0.1826(5) 0.0757(18) Uani 1 1 d . . . . .
H1A H 0.7901 0.6080 0.1711 0.091 Uiso 1 1 calc R . . . .
C1B C 0.9937(3) 0.5499(3) 0.1318(5) 0.0760(18) Uani 1 1 d . . . . .
C1C C 0.7401(3) 0.6543(2) 0.1071(5) 0.0675(16) Uani 1 1 d . . . . .
C1D C 0.7983(2) 0.6526(2) -0.0355(5) 0.0679(17) Uani 1 1 d . . . . .
C1E C 0.7476(3) 0.6357(2) 0.0020(5) 0.0641(16) Uani 1 1 d . . . . .
C1F C 0.8188(3) 0.6333(2) -0.1135(6) 0.0773(19) Uani 1 1 d . . . . .
H1F H 0.8025 0.6074 -0.1433 0.093 Uiso 1 1 calc R . . . .
C1G C 0.7091(3) 0.6920(2) 0.1253(5) 0.079(2) Uani 1 1 d . . . . .
H1G H 0.6915 0.7064 0.0748 0.094 Uiso 1 1 calc R . . . .
C1H C 0.8896(3) 0.6890(3) -0.1050(8) 0.098(3) Uani 1 1 d . . . . .
H1H H 0.9202 0.7004 -0.1274 0.118 Uiso 1 1 calc R . . . .
C1I C 0.8254(3) 0.6918(2) 0.0092(6) 0.079(2) Uani 1 1 d . . . . .
H1I H 0.8127 0.7059 0.0639 0.095 Uiso 1 1 calc R . . . .
C1J C 0.7646(4) 0.6517(3) 0.2729(6) 0.100(3) Uani 1 1 d . . . . .
H1J H 0.7841 0.6383 0.3219 0.120 Uiso 1 1 calc R . . . .
C1K C 0.7072(4) 0.6020(3) -0.4633(6) 0.105(3) Uani 1 1 d . . . . .
H1K H 0.7055 0.6203 -0.5188 0.126 Uiso 1 1 calc R . . . .
C1L C 0.9474(3) 0.6243(3) 0.0963(7) 0.114(3) Uani 1 1 d . . . . .
H1L H 0.9455 0.6579 0.0943 0.136 Uiso 1 1 calc R . . . .
C1M C 0.8692(3) 0.7087(3) -0.0272(7) 0.092(3) Uani 1 1 d . . . . .
H1M H 0.8855 0.7347 0.0025 0.111 Uiso 1 1 calc R . . . .
C1N C 1.0372(3) 0.5236(3) 0.1635(6) 0.085(2) Uani 1 1 d . . . . .
H1N H 1.0659 0.5403 0.1843 0.102 Uiso 1 1 calc R . . . .
C1O C 0.7025(4) 0.7101(3) 0.2172(6) 0.098(3) Uani 1 1 d . . . . .
H1O H 0.6796 0.7348 0.2283 0.118 Uiso 1 1 calc R . . . .
C1P C 0.9066(3) 0.5964(3) 0.0696(6) 0.084(2) Uani 1 1 d . . . . .
H1P H 0.8771 0.6120 0.0492 0.101 Uiso 1 1 calc R . . . .
C1Q C 0.6151(3) 0.5248(3) 0.3050(6) 0.091(2) Uani 1 1 d . . . . .
C1R C 0.6735(4) 0.7099(3) -0.1839(7) 0.097(3) Uani 1 1 d . . . . .
H1R H 0.6799 0.7343 -0.2278 0.116 Uiso 1 1 calc R . . . .
C1S C 0.7040(4) 0.6238(3) -0.3789(7) 0.110(3) Uani 1 1 d . U . . .
H1S H 0.7036 0.6574 -0.3756 0.133 Uiso 1 1 calc R . . . .
C1T C 0.6184(3) 0.6549(3) -0.1159(7) 0.096(2) Uani 1 1 d . . . . .
H1T H 0.5865 0.6410 -0.1139 0.116 Uiso 1 1 calc R . . . .
C1U C 0.6434(3) 0.5958(3) 0.2323(6) 0.097(2) Uani 1 1 d . U . . .
H1U H 0.6614 0.6119 0.1859 0.116 Uiso 1 1 calc R . . . .
C1V C 0.8643(3) 0.6507(3) -0.1521(6) 0.090(2) Uani 1 1 d . . . . .
H1V H 0.8771 0.6373 -0.2073 0.109 Uiso 1 1 calc R . . . .
C1W C 0.6252(4) 0.6912(3) -0.1757(7) 0.101(3) Uani 1 1 d . . . . .
H1W H 0.5983 0.7038 -0.2112 0.121 Uiso 1 1 calc R . . . .
C1X C 0.7315(4) 0.6900(3) 0.2926(6) 0.103(3) Uani 1 1 d . . . . .
H1X H 0.7288 0.7018 0.3542 0.123 Uiso 1 1 calc R . . . .
C1Z C 0.5909(3) 0.5985(5) 0.3728(8) 0.120(3) Uani 1 1 d . U . . .
H1Z H 0.5748 0.6161 0.4197 0.144 Uiso 1 1 calc R . . . .
C1Y C 0.9924(3) 0.6012(3) 0.1265(6) 0.096(2) Uani 1 1 d . . . . .
H1Y H 1.0209 0.6193 0.1429 0.115 Uiso 1 1 calc R . . . .
C20 C 0.5643(3) 0.5226(4) 0.4477(8) 0.130(4) Uani 1 1 d . U . . .
H20 H 0.5477 0.5392 0.4953 0.157 Uiso 1 1 calc R . . . .
C1 C 0.5892(3) 0.5489(4) 0.3760(7) 0.110(3) Uani 1 1 d . U . . .
C2 C 0.6150(4) 0.6223(4) 0.3038(8) 0.121(3) Uani 1 1 d . . . . .
H2 H 0.6137 0.6559 0.3015 0.146 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 O2 1.956(4) . ?
V1 O2 1.956(4) 6_565 ?
V1 O3 1.593(6) . ?
V1 N7 2.108(5) . ?
V1 N7 2.108(5) 6_565 ?
V1 O9 2.281(7) . ?
V2 O 1.956(4) 6_565 ?
V2 O 1.956(4) . ?
V2 O5 2.316(6) . ?
V2 N6 2.129(5) . ?
V2 N6 2.129(5) 6_565 ?
V2 O8 1.567(7) . ?
V3 O1 1.953(4) 6_565 ?
V3 O1 1.953(4) . ?
V3 O4 1.623(7) . ?
V3 O11 2.239(7) . ?
V3 N15 2.127(6) . ?
V3 N15 2.127(6) 6_565 ?
P4 O 1.524(4) . ?
P4 O1 1.519(4) . ?
P4 O2 1.520(4) . ?
P4 C1E 1.863(6) . ?
N6 C12 1.355(8) . ?
N6 C14 1.326(8) . ?
N7 C10 1.367(8) . ?
N7 C1P 1.353(8) . ?
C10 C10 1.429(13) 6_565 ?
C10 C1B 1.372(9) . ?
C12 C12 1.425(13) 6_565 ?
C12 C18 1.424(9) . ?
C13 C19 1.391(9) . ?
C13 C1T 1.388(10) . ?
C14 C1S 1.439(10) . ?
N15 C1Q 1.375(9) . ?
N15 C1U 1.324(10) . ?
C16 C19 1.385(9) . ?
C16 C1R 1.404(10) . ?
C17 C17 1.343(16) 6_565 ?
C17 C18 1.442(10) . ?
C18 C1K 1.397(11) . ?
C19 C1E 1.514(9) . ?
C1A C1C 1.407(9) . ?
C1A C1J 1.368(10) . ?
C1B C1N 1.425(10) . ?
C1B C1Y 1.418(11) . ?
C1C C1E 1.581(9) . ?
C1C C1G 1.354(9) . ?
C1D C1E 1.527(10) . ?
C1D C1F 1.344(10) . ?
C1D C1I 1.436(9) . ?
C1F C1V 1.414(10) . ?
C1G C1O 1.399(10) . ?
C1H C1M 1.346(12) . ?
C1H C1V 1.410(12) . ?
C1I C1M 1.360(10) . ?
C1J C1X 1.403(12) . ?
C1K C1S 1.335(11) . ?
C1L C1P 1.374(10) . ?
C1L C1Y 1.407(11) . ?
C1N C1N 1.305(15) 6_565 ?
C1O C1X 1.410(12) . ?
C1Q C1Q 1.371(17) 6_565 ?
C1Q C1 1.391(11) . ?
C1R C1W 1.387(12) . ?
C1T C1W 1.323(12) . ?
C1U C2 1.463(12) . ?
C1Z C1 1.372(14) . ?
C1Z C2 1.346(14) . ?
C20 C20 1.25(2) 6_565 ?
C20 C1 1.416(13) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 V1 O2 94.5(2) 6_565 . ?
O2 V1 N7 159.7(2) . 6_565 ?
O2 V1 N7 159.7(2) 6_565 . ?
O2 V1 N7 91.46(18) . . ?
O2 V1 N7 91.46(18) 6_565 6_565 ?
O2 V1 O9 80.42(16) 6_565 . ?
O2 V1 O9 80.42(16) . . ?
O3 V1 O2 101.26(19) . 6_565 ?
O3 V1 O2 101.26(19) . . ?
O3 V1 N7 96.6(2) . 6_565 ?
O3 V1 N7 96.6(2) . . ?
O3 V1 O9 177.5(3) . . ?
N7 V1 N7 76.8(3) 6_565 . ?
N7 V1 O9 81.48(19) . . ?
N7 V1 O9 81.48(19) 6_565 . ?
O V2 O 95.6(2) . 6_565 ?
O V2 O5 81.56(17) . . ?
O V2 O5 81.56(17) 6_565 . ?
O V2 N6 157.5(2) . 6_565 ?
O V2 N6 90.26(18) 6_565 6_565 ?
O V2 N6 157.5(2) 6_565 . ?
O V2 N6 90.26(18) . . ?
N6 V2 O5 77.9(2) . . ?
N6 V2 O5 77.9(2) 6_565 . ?
N6 V2 N6 76.7(3) . 6_565 ?
O8 V2 O 102.1(2) . . ?
O8 V2 O 102.1(2) . 6_565 ?
O8 V2 O5 174.4(3) . . ?
O8 V2 N6 97.8(3) . . ?
O8 V2 N6 97.8(3) . 6_565 ?
O1 V3 O1 96.8(2) . 6_565 ?
O1 V3 O11 82.77(19) 6_565 . ?
O1 V3 O11 82.77(19) . . ?
O1 V3 N15 90.9(2) 6_565 6_565 ?
O1 V3 N15 90.9(2) . . ?
O1 V3 N15 161.1(2) . 6_565 ?
O1 V3 N15 161.1(2) 6_565 . ?
O4 V3 O1 100.7(2) . . ?
O4 V3 O1 100.7(2) . 6_565 ?
O4 V3 O11 174.8(3) . . ?
O4 V3 N15 94.8(2) . . ?
O4 V3 N15 94.8(2) . 6_565 ?
N15 V3 O11 81.1(2) . . ?
N15 V3 O11 81.1(2) 6_565 . ?
N15 V3 N15 76.9(4) 6_565 . ?
O P4 C1E 106.0(3) . . ?
O1 P4 O 111.8(2) . . ?
O1 P4 O2 112.2(2) . . ?
O1 P4 C1E 107.4(3) . . ?
O2 P4 O 112.3(2) . . ?
O2 P4 C1E 106.7(3) . . ?
P4 O V2 142.9(2) . . ?
P4 O1 V3 139.5(3) . . ?
P4 O2 V1 142.0(2) . . ?
C12 N6 V2 113.9(4) . . ?
C14 N6 V2 126.4(4) . . ?
C14 N6 C12 119.2(5) . . ?
C10 N7 V1 115.7(4) . . ?
C1P N7 V1 127.7(4) . . ?
C1P N7 C10 116.6(5) . . ?
N7 C10 C10 115.8(3) . 6_565 ?
N7 C10 C1B 125.2(6) . . ?
C1B C10 C10 119.0(4) . 6_565 ?
N6 C12 C12 116.7(3) . 6_565 ?
N6 C12 C18 123.0(6) . . ?
C18 C12 C12 120.3(4) . 6_565 ?
C1T C13 C19 119.3(7) . . ?
N6 C14 C1S 120.3(7) . . ?
C1Q N15 V3 113.6(5) . . ?
C1U N15 V3 125.9(6) . . ?
C1U N15 C1Q 120.3(7) . . ?
C19 C16 C1R 122.1(8) . . ?
C17 C17 C18 121.8(4) 6_565 . ?
C12 C18 C17 117.9(7) . . ?
C1K C18 C12 116.3(7) . . ?
C1K C18 C17 125.5(7) . . ?
C13 C19 C1E 121.9(6) . . ?
C16 C19 C13 116.9(6) . . ?
C16 C19 C1E 121.1(6) . . ?
C1J C1A C1C 120.2(7) . . ?
C10 C1B C1N 120.4(7) . . ?
C10 C1B C1Y 116.6(6) . . ?
C1Y C1B C1N 123.0(6) . . ?
C1A C1C C1E 119.9(6) . . ?
C1G C1C C1A 119.0(6) . . ?
C1G C1C C1E 121.0(6) . . ?
C1F C1D C1E 122.2(6) . . ?
C1F C1D C1I 116.8(7) . . ?
C1I C1D C1E 120.9(6) . . ?
C19 C1E P4 109.5(4) . . ?
C19 C1E C1C 109.8(5) . . ?
C19 C1E C1D 110.0(5) . . ?
C1C C1E P4 108.1(4) . . ?
C1D C1E P4 108.9(4) . . ?
C1D C1E C1C 110.5(5) . . ?
C1D C1F C1V 122.6(7) . . ?
C1C C1G C1O 122.4(8) . . ?
C1M C1H C1V 119.4(7) . . ?
C1M C1I C1D 121.0(8) . . ?
C1A C1J C1X 121.1(8) . . ?
C1S C1K C18 120.5(7) . . ?
C1P C1L C1Y 118.9(7) . . ?
C1H C1M C1I 121.8(8) . . ?
C1N C1N C1B 120.7(4) 6_565 . ?
C1G C1O C1X 118.5(8) . . ?
N7 C1P C1L 123.3(7) . . ?
N15 C1Q C1 123.8(8) . . ?
C1Q C1Q N15 117.6(4) 6_565 . ?
C1Q C1Q C1 118.5(6) 6_565 . ?
C1W C1R C16 119.1(8) . . ?
C1K C1S C14 120.4(8) . . ?
C1W C1T C13 124.1(8) . . ?
N15 C1U C2 117.4(9) . . ?
C1H C1V C1F 118.4(8) . . ?
C1T C1W C1R 118.3(8) . . ?
C1J C1X C1O 118.7(8) . . ?
C2 C1Z C1 121.8(9) . . ?
C1L C1Y C1B 119.3(7) . . ?
C20 C20 C1 120.8(6) 6_565 . ?
C1Q C1 C20 120.6(10) . . ?
C1Z C1 C1Q 115.9(9) . . ?
C1Z C1 C20 123.4(9) . . ?
C1Z C2 C1U 120.6(10) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O5 H5B O3 0.92 1.90 2.766(9) 157.6 .
O9 H9B O4 0.98 1.92 2.757(9) 141.7 .

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 N7 C10 C10 1.8(4) . . . 6_565 ?
V1 N7 C10 C1B -179.7(5) . . . . ?
V1 N7 C1P C1L 179.9(7) . . . . ?
V2 N6 C12 C12 10.8(5) . . . 6_565 ?
V2 N6 C12 C18 -171.9(5) . . . . ?
V2 N6 C14 C1S 171.6(6) . . . . ?
V3 N15 C1Q C1Q -6.1(5) . . . 6_565 ?
V3 N15 C1Q C1 171.5(7) . . . . ?
V3 N15 C1U C2 -173.2(6) . . . . ?
O P4 O1 V3 95.0(4) . . . . ?
O P4 O2 V1 -31.6(5) . . . . ?
O P4 C1E C19 43.6(5) . . . . ?
O P4 C1E C1C 163.2(4) . . . . ?
O P4 C1E C1D -76.6(5) . . . . ?
O1 P4 O V2 -36.8(5) . . . . ?
O1 P4 O2 V1 95.3(4) . . . . ?
O1 P4 C1E C19 -76.0(5) . . . . ?
O1 P4 C1E C1C 43.6(5) . . . . ?
O1 P4 C1E C1D 163.7(4) . . . . ?
O2 P4 O V2 90.4(5) . . . . ?
O2 P4 O1 V3 -32.2(5) . . . . ?
O2 P4 C1E C19 163.5(4) . . . . ?
O2 P4 C1E C1C -77.0(5) . . . . ?
O2 P4 C1E C1D 43.2(5) . . . . ?
N6 C12 C18 C17 -178.3(7) . . . . ?
N6 C12 C18 C1K -4.1(11) . . . . ?
N6 C14 C1S C1K 2.9(14) . . . . ?
N7 C10 C1B C1N -180.0(6) . . . . ?
N7 C10 C1B C1Y -1.0(10) . . . . ?
C10 N7 C1P C1L 0.9(11) . . . . ?
C10 C10 C1B C1N -1.6(8) 6_565 . . . ?
C10 C10 C1B C1Y 177.4(5) 6_565 . . . ?
C10 C1B C1N C1N 1.6(8) . . . 6_565 ?
C10 C1B C1Y C1L 2.4(12) . . . . ?
C12 N6 C14 C1S 0.2(11) . . . . ?
C12 C12 C18 C17 -1.1(8) 6_565 . . . ?
C12 C12 C18 C1K 173.1(6) 6_565 . . . ?
C12 C18 C1K C1S 7.0(14) . . . . ?
C13 C19 C1E P4 46.9(7) . . . . ?
C13 C19 C1E C1C -71.6(7) . . . . ?
C13 C19 C1E C1D 166.5(6) . . . . ?
C13 C1T C1W C1R 4.4(14) . . . . ?
C14 N6 C12 C12 -176.7(5) . . . 6_565 ?
C14 N6 C12 C18 0.6(10) . . . . ?
N15 C1Q C1 C1Z 2.0(13) . . . . ?
N15 C1Q C1 C20 -176.3(8) . . . . ?
N15 C1U C2 C1Z 2.7(14) . . . . ?
C16 C19 C1E P4 -136.6(5) . . . . ?
C16 C19 C1E C1C 104.8(7) . . . . ?
C16 C19 C1E C1D -17.0(8) . . . . ?
C16 C1R C1W C1T -3.5(13) . . . . ?
C17 C17 C18 C12 1.1(8) 6_565 . . . ?
C17 C17 C18 C1K -172.5(7) 6_565 . . . ?
C17 C18 C1K C1S -179.3(9) . . . . ?
C18 C1K C1S C14 -6.6(15) . . . . ?
C19 C13 C1T C1W -4.1(13) . . . . ?
C19 C16 C1R C1W 2.6(12) . . . . ?
C1A C1C C1E P4 47.2(7) . . . . ?
C1A C1C C1E C19 166.6(6) . . . . ?
C1A C1C C1E C1D -71.9(7) . . . . ?
C1A C1C C1G C1O -2.8(11) . . . . ?
C1A C1J C1X C1O -0.5(13) . . . . ?
C1C C1A C1J C1X 1.4(12) . . . . ?
C1C C1G C1O C1X 3.7(12) . . . . ?
C1D C1F C1V C1H 1.9(11) . . . . ?
C1D C1I C1M C1H -1.4(12) . . . . ?
C1E P4 O V2 -153.5(4) . . . . ?
C1E P4 O1 V3 -149.2(4) . . . . ?
C1E P4 O2 V1 -147.3(4) . . . . ?
C1E C1C C1G C1O -178.5(7) . . . . ?
C1E C1D C1F C1V 176.0(6) . . . . ?
C1E C1D C1I C1M -176.3(6) . . . . ?
C1F C1D C1E P4 46.3(8) . . . . ?
C1F C1D C1E C19 -73.7(7) . . . . ?
C1F C1D C1E C1C 165.0(6) . . . . ?
C1F C1D C1I C1M 0.9(10) . . . . ?
C1G C1C C1E P4 -137.2(6) . . . . ?
C1G C1C C1E C19 -17.7(8) . . . . ?
C1G C1C C1E C1D 103.7(7) . . . . ?
C1G C1O C1X C1J -1.9(13) . . . . ?
C1I C1D C1E P4 -136.6(5) . . . . ?
C1I C1D C1E C19 103.4(7) . . . . ?
C1I C1D C1E C1C -18.0(8) . . . . ?
C1I C1D C1F C1V -1.2(10) . . . . ?
C1J C1A C1C C1E 176.0(7) . . . . ?
C1J C1A C1C C1G 0.2(11) . . . . ?
C1M C1H C1V C1F -2.3(12) . . . . ?
C1N C1B C1Y C1L -178.7(8) . . . . ?
C1P N7 C10 C10 -179.0(5) . . . 6_565 ?
C1P N7 C10 C1B -0.6(9) . . . . ?
C1P C1L C1Y C1B -2.1(14) . . . . ?
C1Q N15 C1U C2 0.7(11) . . . . ?
C1Q C1Q C1 C1Z 179.5(6) 6_565 . . . ?
C1Q C1Q C1 C20 1.2(11) 6_565 . . . ?
C1R C16 C19 C13 -2.3(10) . . . . ?
C1R C16 C19 C1E -178.9(6) . . . . ?
C1T C13 C19 C16 2.8(10) . . . . ?
C1T C13 C19 C1E 179.4(6) . . . . ?
C1U N15 C1Q C1Q 179.3(5) . . . 6_565 ?
C1U N15 C1Q C1 -3.1(12) . . . . ?
C1V C1H C1M C1I 2.1(13) . . . . ?
C1Y C1B C1N C1N -177.3(6) . . . 6_565 ?
C1Y C1L C1P N7 0.5(14) . . . . ?
C20 C20 C1 C1Q -1.2(11) 6_565 . . . ?
C20 C20 C1 C1Z -179.4(7) 6_565 . . . ?
C1 C1Z C2 C1U -3.9(16) . . . . ?
C2 C1Z C1 C1Q 1.5(15) . . . . ?
C2 C1Z C1 C20 179.8(10) . . . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.357 -0.148 -0.626 2522.3 1124.5 ?
_database_code_depnum_ccdc_archive 'CCDC 990485'
#######################################################################
#
#                 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
_vrf_PLAT601_5                   
;
PROBLEM: Structure Contains Solvent Accessible VOIDS of .       3050 Ang3
RESPONSE: Disordered solvent molecules were omitted by using OLEX-2/Mask
;
_audit_creation_date             2014-04-07
_audit_creation_method           
;
Olex2 1.2
(compiled 2013.11.15 svn.r2834 for OlexSys, GUI svn.r4720)
;
_shelxl_version_number           2013-3
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C71 H66 N6 O12 P2 V3'
_chemical_formula_sum            'C71 H66 N6 O12 P2 V3'
_chemical_formula_weight         1410.05
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 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'
P P 0.1023 0.0942 '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'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_H-M_alt        'R -3'
_space_group_name_Hall           '-R 3'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'

_cell_length_a                   17.454(3)
_cell_length_b                   17.454(3)
_cell_length_c                   45.618(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     12035(4)
_cell_formula_units_Z            6
_cell_measurement_reflns_used    2589
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.53
_cell_measurement_theta_min      2.24
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.438
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.587984
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS v.2.10 (Bruker,2003) was used for absorption correction.
R(int) was 0.0487 before and 0.0383 after correction.
The Ratio of minimum to maximum transmission is 0.5880.
The λ/2 correction factor is 0.0015.
;
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.167
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             4374
_exptl_crystal_size_max          0.078
_exptl_crystal_size_mid          0.074
_exptl_crystal_size_min          0.07
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0952
_diffrn_reflns_av_unetI/netI     0.0846
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       60
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            26835
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.500
_diffrn_reflns_theta_max         25.498
_diffrn_reflns_theta_min         2.237
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3477
_reflns_number_total             4973
_reflns_special_details          
;
 Data were apparently pre-merged, so _diffrn_reflns_number
 etc. will have to be added later.
 
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v6.45A (Bruker, 2003)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT v6.45A (Bruker, 2003)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'SIR97 (Burla et al., 2007)'
_refine_diff_density_max         0.980
_refine_diff_density_min         -0.526
_refine_diff_density_rms         0.091
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     287
_refine_ls_number_reflns         4973
_refine_ls_number_restraints     9
_refine_ls_R_factor_all          0.0900
_refine_ls_R_factor_gt           0.0669
_refine_ls_restrained_S_all      1.065
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1155P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1823
_refine_ls_wR_factor_ref         0.1968
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 O9-H9
 0.85 with sigma of 0.01
 C33-H9
 1.864079 with sigma of 0.02
 V1-H9
 2.754112 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C33) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.002
4.a Aromatic/amide H refined with riding coordinates:
 C16(H16), C17(H17), C20(H20), C21(H21), C22(H22), C23(H23), C24(H24),
 C25(H25), C26(H26), C27(H27), C28(H28), C29(H29), C30(H30), C31(H31), C32(H32),
  C34(H34), C35(H35), C37(H37)
4.b Idealised Me refined as rotating group:
 C33(H33A,H33B,H33C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
V1 V 0.37503(4) -0.15924(4) 0.31620(2) 0.0275(2) Uani 1 1 d D . . . .
P2 P 0.3333 -0.3333 0.27491(4) 0.0252(4) Uani 1 3 d S T P . .
P3 P 0.3333 -0.3333 0.35733(4) 0.0262(4) Uani 1 3 d S T P . .
O5 O 0.36529(16) -0.23883(15) 0.28465(5) 0.0321(6) Uani 1 1 d . . . . .
O6 O 0.36929(16) -0.23803(15) 0.34775(5) 0.0307(6) Uani 1 1 d . . . . .
O8 O 0.27687(16) -0.17419(15) 0.31745(6) 0.0358(6) Uani 1 1 d . . . . .
O9 O 0.51904(16) -0.13086(16) 0.31325(7) 0.0411(7) Uani 1 1 d D . . . .
H9 H 0.5200(12) -0.1799(9) 0.3129(10) 0.062 Uiso 1 1 d DR . . . .
N10 N 0.42852(19) -0.05044(19) 0.28722(8) 0.0342(8) Uani 1 1 d . . . . .
N11 N 0.43682(19) -0.04788(18) 0.34457(7) 0.0303(7) Uani 1 1 d . . . . .
C12 C 0.3333 -0.3333 0.23438(14) 0.0302(14) Uani 1 3 d S T P . .
C13 C 0.2978(3) -0.2734(2) 0.22306(8) 0.0338(9) Uani 1 1 d . . . . .
C14 C 0.4141(2) -0.2465(2) 0.40900(8) 0.0345(9) Uani 1 1 d . . . . .
C15 C 0.3333 -0.3333 0.39856(14) 0.0326(15) Uani 1 3 d S T P . .
C16 C 0.5207(2) 0.1089(2) 0.34845(10) 0.0385(10) Uani 1 1 d . . . . .
H16 H 0.5502 0.1638 0.3393 0.046 Uiso 1 1 calc R . . . .
C17 C 0.5172(2) 0.1066(2) 0.28189(10) 0.0423(11) Uani 1 1 d . . . . .
H17 H 0.5497 0.1623 0.2904 0.051 Uiso 1 1 calc R . . . .
C18 C 0.4765(2) 0.0318(2) 0.29940(10) 0.0349(9) Uani 1 1 d . . . . .
C19 C 0.4791(2) 0.0327(2) 0.33170(9) 0.0328(9) Uani 1 1 d . . . . .
C20 C 0.2206(3) -0.2799(3) 0.23498(9) 0.0435(10) Uani 1 1 d . . . . .
H20 H 0.1914 -0.3196 0.2502 0.052 Uiso 1 1 calc R . . . .
C21 C 0.4354(3) -0.0529(3) 0.37378(10) 0.0389(10) Uani 1 1 d . . . . .
H21 H 0.4073 -0.1084 0.3826 0.047 Uiso 1 1 calc R . . . .
C22 C 0.4969(2) -0.2145(3) 0.39662(9) 0.0370(9) Uani 1 1 d . . . . .
H22 H 0.5042 -0.2452 0.3812 0.044 Uiso 1 1 calc R . . . .
C23 C 0.5185(3) 0.1038(3) 0.37806(11) 0.0450(11) Uani 1 1 d . . . . .
H23 H 0.5465 0.1550 0.3893 0.054 Uiso 1 1 calc R . . . .
C24 C 0.4206(3) -0.0573(3) 0.25820(10) 0.0422(10) Uani 1 1 d . . . . .
H24 H 0.3877 -0.1133 0.2500 0.051 Uiso 1 1 calc R . . . .
C25 C 0.4742(3) 0.0217(3) 0.39154(11) 0.0463(11) Uani 1 1 d . . . . .
H25 H 0.4707 0.0167 0.4119 0.056 Uiso 1 1 calc R . . . .
C26 C 0.5090(3) 0.0980(3) 0.25177(12) 0.0510(12) Uani 1 1 d . . . . .
H26 H 0.5369 0.1477 0.2398 0.061 Uiso 1 1 calc R . . . .
C27 C 0.3394(3) -0.2132(3) 0.20069(9) 0.0450(10) Uani 1 1 d . . . . .
H27 H 0.3911 -0.2071 0.1926 0.054 Uiso 1 1 calc R . . . .
C28 C 0.4590(3) 0.0149(3) 0.23975(11) 0.0529(12) Uani 1 1 d . . . . .
H28 H 0.4512 0.0076 0.2196 0.063 Uiso 1 1 calc R . . . .
C29 C 0.4062(3) -0.2014(3) 0.43313(9) 0.0468(11) Uani 1 1 d . . . . .
H29 H 0.3516 -0.2227 0.4422 0.056 Uiso 1 1 calc R . . . .
C30 C 0.5611(3) -0.0931(3) 0.43057(12) 0.0572(13) Uani 1 1 d . . . . .
H30 H 0.6100 -0.0424 0.4378 0.069 Uiso 1 1 calc R . . . .
C31 C 0.5699(3) -0.1364(3) 0.40691(11) 0.0523(12) Uani 1 1 d . . . . .
H31 H 0.6245 -0.1139 0.3976 0.063 Uiso 1 1 calc R . . . .
C32 C 0.3052(4) -0.1612(3) 0.19000(10) 0.0648(15) Uani 1 1 d . . . . .
H32 H 0.3339 -0.1214 0.1748 0.078 Uiso 1 1 calc R . . . .
C33 C 0.6026(3) -0.0643(3) 0.32056(12) 0.0658(14) Uani 1 1 d D U . . .
H33A H 0.6157 -0.0114 0.3101 0.099 Uiso 1 1 calc GR . . . .
H33B H 0.6450 -0.0818 0.3154 0.099 Uiso 1 1 calc GR . . . .
H33C H 0.6054 -0.0534 0.3413 0.099 Uiso 1 1 calc GR . . . .
C34 C 0.4790(3) -0.1251(3) 0.44363(10) 0.0576(13) Uani 1 1 d . . . . .
H34 H 0.4727 -0.0953 0.4595 0.069 Uiso 1 1 calc R . . . .
C35 C 0.1874(4) -0.2283(4) 0.22449(11) 0.0687(16) Uani 1 1 d . . . . .
H35 H 0.1362 -0.2336 0.2327 0.082 Uiso 1 1 calc R . . . .
C37 C 0.2293(4) -0.1684(4) 0.20181(11) 0.0727(17) Uani 1 1 d . . . . .
H37 H 0.2064 -0.1340 0.1948 0.087 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 1.948(2) . ?
V1 O6 1.958(2) . ?
V1 O8 1.600(2) . ?
V1 O9 2.310(3) . ?
V1 N10 2.110(3) . ?
V1 N11 2.126(3) . ?
P2 O5 1.520(2) . ?
P2 O5 1.520(2) 2_545 ?
P2 O5 1.519(2) 3_655 ?
P2 C12 1.849(7) . ?
P3 O6 1.519(2) . ?
P3 O6 1.519(2) 2_545 ?
P3 O6 1.519(2) 3_655 ?
P3 C15 1.881(7) . ?
O9 H9 0.865(9) . ?
O9 C33 1.376(6) . ?
N10 C18 1.366(5) . ?
N10 C24 1.330(5) . ?
N11 C19 1.353(5) . ?
N11 C21 1.335(5) . ?
C12 C13 1.548(4) . ?
C12 C13 1.548(4) 2_545 ?
C12 C13 1.548(4) 3_655 ?
C13 C20 1.404(5) . ?
C13 C27 1.382(5) . ?
C14 C15 1.540(4) . ?
C14 C22 1.383(5) . ?
C14 C29 1.400(6) . ?
C15 C14 1.540(4) 2_545 ?
C15 C14 1.540(4) 3_655 ?
C16 H16 0.9300 . ?
C16 C19 1.383(5) . ?
C16 C23 1.353(6) . ?
C17 H17 0.9300 . ?
C17 C18 1.386(5) . ?
C17 C26 1.382(6) . ?
C18 C19 1.474(6) . ?
C20 H20 0.9300 . ?
C20 C35 1.376(6) . ?
C21 H21 0.9300 . ?
C21 C25 1.388(5) . ?
C22 H22 0.9300 . ?
C22 C31 1.402(6) . ?
C23 H23 0.9300 . ?
C23 C25 1.386(6) . ?
C24 H24 0.9300 . ?
C24 C28 1.378(6) . ?
C25 H25 0.9300 . ?
C26 H26 0.9300 . ?
C26 C28 1.379(6) . ?
C27 H27 0.9300 . ?
C27 C32 1.401(6) . ?
C28 H28 0.9300 . ?
C29 H29 0.9300 . ?
C29 C34 1.387(6) . ?
C30 H30 0.9300 . ?
C30 C31 1.370(7) . ?
C30 C34 1.385(7) . ?
C31 H31 0.9300 . ?
C32 H32 0.9300 . ?
C32 C37 1.376(8) . ?
C33 H33A 0.9600 . ?
C33 H33B 0.9600 . ?
C33 H33C 0.9600 . ?
C34 H34 0.9300 . ?
C35 H35 0.9300 . ?
C35 C37 1.390(8) . ?
C37 H37 0.9300 . ?

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 O6 94.97(10) . . ?
O5 V1 O9 78.90(10) . . ?
O5 V1 N10 91.17(12) . . ?
O5 V1 N11 157.72(11) . . ?
O6 V1 O9 82.04(10) . . ?
O6 V1 N10 159.51(11) . . ?
O6 V1 N11 91.10(11) . . ?
O8 V1 O5 101.86(12) . . ?
O8 V1 O6 100.64(12) . . ?
O8 V1 O9 177.10(12) . . ?
O8 V1 N10 97.18(12) . . ?
O8 V1 N11 98.03(12) . . ?
N10 V1 O9 79.99(11) . . ?
N10 V1 N11 76.39(13) . . ?
N11 V1 O9 80.75(10) . . ?
O5 P2 O5 111.82(10) . 2_545 ?
O5 P2 O5 111.82(10) . 3_655 ?
O5 P2 O5 111.83(10) 2_545 3_655 ?
O5 P2 C12 107.00(11) . . ?
O5 P2 C12 107.00(11) 2_545 . ?
O5 P2 C12 107.00(11) 3_655 . ?
O6 P3 O6 112.08(10) . 2_545 ?
O6 P3 O6 112.09(10) . 3_655 ?
O6 P3 O6 112.08(10) 2_545 3_655 ?
O6 P3 C15 106.71(11) . . ?
O6 P3 C15 106.71(11) 2_545 . ?
O6 P3 C15 106.71(11) 3_655 . ?
P2 O5 V1 147.56(17) . . ?
P3 O6 V1 145.93(16) . . ?
V1 O9 H9 110.3(13) . . ?
C33 O9 V1 138.4(3) . . ?
C33 O9 H9 107.6(14) . . ?
C18 N10 V1 117.0(3) . . ?
C24 N10 V1 124.3(2) . . ?
C24 N10 C18 118.7(3) . . ?
C19 N11 V1 116.8(3) . . ?
C21 N11 V1 124.3(2) . . ?
C21 N11 C19 119.0(3) . . ?
C13 C12 P2 109.5(3) 3_655 . ?
C13 C12 P2 109.5(3) 2_545 . ?
C13 C12 P2 109.5(3) . . ?
C13 C12 C13 109.5(3) 2_545 3_655 ?
C13 C12 C13 109.5(3) . 3_655 ?
C13 C12 C13 109.5(3) . 2_545 ?
C20 C13 C12 120.6(3) . . ?
C27 C13 C12 121.6(4) . . ?
C27 C13 C20 117.8(4) . . ?
C22 C14 C15 121.9(4) . . ?
C22 C14 C29 118.0(4) . . ?
C29 C14 C15 119.9(4) . . ?
C14 C15 P3 108.0(3) 3_655 . ?
C14 C15 P3 108.0(3) . . ?
C14 C15 P3 108.0(3) 2_545 . ?
C14 C15 C14 110.9(3) . 3_655 ?
C14 C15 C14 110.9(3) 2_545 3_655 ?
C14 C15 C14 110.9(3) 2_545 . ?
C19 C16 H16 119.9 . . ?
C23 C16 H16 119.9 . . ?
C23 C16 C19 120.3(4) . . ?
C18 C17 H17 120.2 . . ?
C26 C17 H17 120.2 . . ?
C26 C17 C18 119.6(4) . . ?
N10 C18 C17 120.8(4) . . ?
N10 C18 C19 114.7(3) . . ?
C17 C18 C19 124.5(4) . . ?
N11 C19 C16 120.7(4) . . ?
N11 C19 C18 115.1(3) . . ?
C16 C19 C18 124.2(3) . . ?
C13 C20 H20 119.6 . . ?
C35 C20 C13 120.8(4) . . ?
C35 C20 H20 119.6 . . ?
N11 C21 H21 118.8 . . ?
N11 C21 C25 122.4(4) . . ?
C25 C21 H21 118.8 . . ?
C14 C22 H22 119.5 . . ?
C14 C22 C31 121.0(4) . . ?
C31 C22 H22 119.5 . . ?
C16 C23 H23 120.2 . . ?
C16 C23 C25 119.6(4) . . ?
C25 C23 H23 120.2 . . ?
N10 C24 H24 118.5 . . ?
N10 C24 C28 123.0(4) . . ?
C28 C24 H24 118.5 . . ?
C21 C25 H25 121.0 . . ?
C23 C25 C21 118.0(4) . . ?
C23 C25 H25 121.0 . . ?
C17 C26 H26 120.4 . . ?
C28 C26 C17 119.1(4) . . ?
C28 C26 H26 120.4 . . ?
C13 C27 H27 119.4 . . ?
C13 C27 C32 121.1(4) . . ?
C32 C27 H27 119.4 . . ?
C24 C28 C26 118.8(4) . . ?
C24 C28 H28 120.6 . . ?
C26 C28 H28 120.6 . . ?
C14 C29 H29 119.6 . . ?
C34 C29 C14 120.7(4) . . ?
C34 C29 H29 119.6 . . ?
C31 C30 H30 120.2 . . ?
C31 C30 C34 119.7(4) . . ?
C34 C30 H30 120.2 . . ?
C22 C31 H31 119.9 . . ?
C30 C31 C22 120.1(4) . . ?
C30 C31 H31 119.9 . . ?
C27 C32 H32 119.7 . . ?
C37 C32 C27 120.5(5) . . ?
C37 C32 H32 119.7 . . ?
O9 C33 H33A 109.5 . . ?
O9 C33 H33B 109.5 . . ?
O9 C33 H33C 109.5 . . ?
H33A C33 H33B 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C29 C34 H34 119.8 . . ?
C30 C34 C29 120.3(4) . . ?
C30 C34 H34 119.8 . . ?
C20 C35 H35 119.5 . . ?
C20 C35 C37 121.1(5) . . ?
C37 C35 H35 119.5 . . ?
C32 C37 C35 118.7(4) . . ?
C32 C37 H37 120.7 . . ?
C35 C37 H37 120.7 . . ?

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 N10 C18 C17 177.3(3) . . . . ?
V1 N10 C18 C19 -3.8(4) . . . . ?
V1 N10 C24 C28 -177.6(3) . . . . ?
V1 N11 C19 C16 179.6(2) . . . . ?
V1 N11 C19 C18 -0.2(4) . . . . ?
V1 N11 C21 C25 -177.9(3) . . . . ?
P2 C12 C13 C20 -46.7(4) . . . . ?
P2 C12 C13 C27 134.6(3) . . . . ?
O5 P2 O5 V1 -79.5(2) 3_655 . . . ?
O5 P2 O5 V1 46.8(3) 2_545 . . . ?
O5 P2 C12 C13 78.98(18) 3_655 . . 2_545 ?
O5 P2 C12 C13 -41.03(18) . . . . ?
O5 P2 C12 C13 -41.03(18) 2_545 . . 2_545 ?
O5 P2 C12 C13 -161.02(18) . . . 2_545 ?
O5 P2 C12 C13 78.97(18) 2_545 . . . ?
O5 P2 C12 C13 -161.03(18) 2_545 . . 3_655 ?
O5 P2 C12 C13 -41.02(18) 3_655 . . 3_655 ?
O5 P2 C12 C13 -161.03(18) 3_655 . . . ?
O5 P2 C12 C13 78.98(18) . . . 3_655 ?
O6 P3 O6 V1 85.7(2) 3_655 . . . ?
O6 P3 O6 V1 -41.3(3) 2_545 . . . ?
O6 P3 C15 C14 -154.46(18) . . . 3_655 ?
O6 P3 C15 C14 85.54(18) 2_545 . . 3_655 ?
O6 P3 C15 C14 -34.46(18) 2_545 . . 2_545 ?
O6 P3 C15 C14 85.54(18) . . . 2_545 ?
O6 P3 C15 C14 -34.46(18) 3_655 . . 3_655 ?
O6 P3 C15 C14 -154.46(18) 2_545 . . . ?
O6 P3 C15 C14 -34.46(18) . . . . ?
O6 P3 C15 C14 85.54(18) 3_655 . . . ?
O6 P3 C15 C14 -154.46(18) 3_655 . . 2_545 ?
N10 C18 C19 N11 2.6(4) . . . . ?
N10 C18 C19 C16 -177.1(3) . . . . ?
N10 C24 C28 C26 1.0(7) . . . . ?
N11 C21 C25 C23 -2.3(6) . . . . ?
C12 P2 O5 V1 163.6(3) . . . . ?
C12 C13 C20 C35 -178.4(4) . . . . ?
C12 C13 C27 C32 178.0(4) . . . . ?
C13 C12 C13 C20 -166.7(4) 3_655 . . . ?
C13 C12 C13 C20 73.4(6) 2_545 . . . ?
C13 C12 C13 C27 -105.4(3) 2_545 . . . ?
C13 C12 C13 C27 14.6(6) 3_655 . . . ?
C13 C20 C35 C37 0.1(8) . . . . ?
C13 C27 C32 C37 0.6(7) . . . . ?
C14 C22 C31 C30 3.5(6) . . . . ?
C14 C29 C34 C30 -0.9(7) . . . . ?
C15 P3 O6 V1 -157.8(2) . . . . ?
C15 C14 C22 C31 -178.5(4) . . . . ?
C15 C14 C29 C34 177.3(4) . . . . ?
C16 C23 C25 C21 1.6(6) . . . . ?
C17 C18 C19 N11 -178.5(3) . . . . ?
C17 C18 C19 C16 1.7(5) . . . . ?
C17 C26 C28 C24 -1.8(7) . . . . ?
C18 N10 C24 C28 0.2(6) . . . . ?
C18 C17 C26 C28 1.3(6) . . . . ?
C19 N11 C21 C25 1.3(5) . . . . ?
C19 C16 C23 C25 -0.1(5) . . . . ?
C20 C13 C27 C32 -0.8(6) . . . . ?
C20 C35 C37 C32 -0.3(8) . . . . ?
C21 N11 C19 C16 0.3(5) . . . . ?
C21 N11 C19 C18 -179.5(3) . . . . ?
C22 C14 C15 P3 -44.9(4) . . . . ?
C22 C14 C15 C14 -163.0(4) . . . 2_545 ?
C22 C14 C15 C14 73.3(6) . . . 3_655 ?
C22 C14 C29 C34 2.0(6) . . . . ?
C23 C16 C19 N11 -0.9(5) . . . . ?
C23 C16 C19 C18 178.8(3) . . . . ?
C24 N10 C18 C17 -0.7(5) . . . . ?
C24 N10 C18 C19 178.2(3) . . . . ?
C26 C17 C18 N10 0.0(6) . . . . ?
C26 C17 C18 C19 -178.8(3) . . . . ?
C27 C13 C20 C35 0.5(6) . . . . ?
C27 C32 C37 C35 0.0(8) . . . . ?
C29 C14 C15 P3 140.1(3) . . . . ?
C29 C14 C15 C14 -101.8(3) . . . 3_655 ?
C29 C14 C15 C14 21.9(6) . . . 2_545 ?
C29 C14 C22 C31 -3.4(6) . . . . ?
C31 C30 C34 C29 1.0(7) . . . . ?
C34 C30 C31 C22 -2.2(7) . . . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 -0.074 -0.859 -0.492 1250.7 779.6 ?
_database_code_depnum_ccdc_archive 'CCDC 990486'
#######################################################################
#
#                 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
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# 
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#  data retrieval see:
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data_6
_vrf_PLAT601_6                   
;
PROBLEM: Structure Contains Solvent Accessible VOIDS of .       3050 Ang3
RESPONSE: Disordered solvent molecules were omitted by using OLEX-2/Mask
;
_audit_creation_date             2014-04-07
_audit_creation_method           
;
Olex2 1.2
(compiled 2013.11.15 svn.r2834 for OlexSys, GUI svn.r4720)
;
_shelxl_version_number           2013-3
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         
'2(C80 H72 O20 P4 V4), 2(Cl), 2(C5 H9 N2), 6(C7 H8)'
_chemical_formula_sum            'C212 H210 Cl2 N4 O40 P8 V8'
_chemical_formula_weight         4180.01
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 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'
P P 0.1023 0.0942 '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'
V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_cell_length_a                   16.502(5)
_cell_length_b                   32.938(5)
_cell_length_c                   39.238(5)
_cell_angle_alpha                90
_cell_angle_beta                 98.390(5)
_cell_angle_gamma                90
_cell_volume                     21099(8)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    4667
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.22
_cell_measurement_theta_min      2.23
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.496
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.567226
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS v.2.10 (Bruker,2003) was used for absorption correction.
R(int) was 0.0571 before and 0.0444 after correction.
The Ratio of minimum to maximum transmission is 0.5672.
The λ/2 correction factor is 0.0015.
;
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.316
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             8672
_exptl_crystal_size_max          0.088
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.071
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1248
_diffrn_reflns_av_unetI/netI     0.1609
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -40
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -48
_diffrn_reflns_number            121159
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.240
_diffrn_reflns_theta_max         25.500
_diffrn_reflns_theta_min         1.850
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                16890
_reflns_number_total             39165
_reflns_special_details          
;
 Data were apparently pre-merged, so _diffrn_reflns_number
 etc. will have to be added later.
 
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v6.45A (Bruker, 2003)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT v6.45A (Bruker, 2003)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'SIR97 (Burla et al., 2007)'
_refine_diff_density_max         0.991
_refine_diff_density_min         -0.524
_refine_diff_density_rms         0.113
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.952
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2449
_refine_ls_number_reflns         39165
_refine_ls_number_restraints     258
_refine_ls_R_factor_all          0.1959
_refine_ls_R_factor_gt           0.0949
_refine_ls_restrained_S_all      0.951
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1316P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2282
_refine_ls_wR_factor_ref         0.2796
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C50) \\sim Ueq, Uanis(C57) \\sim Ueq, Uanis(C33) \\sim Ueq, Uanis(C5B)
\\sim Ueq, Uanis(C5H) \\sim Ueq, Uanis(C5I) \\sim Ueq, Uanis(C5G) \\sim Ueq:
with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C58) \\sim Ueq, Uanis(C4R) \\sim Ueq, Uanis(C3G) \\sim Ueq, Uanis(C2X)
\\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C4K) \\sim Ueq, Uanis(C3U) \\sim Ueq, Uanis(C4X) \\sim Ueq: with sigma of
0.001 and sigma for terminal atoms of 0.002
Uanis(C54) \\sim Ueq, Uanis(C4V) \\sim Ueq, Uanis(C53) \\sim Ueq, Uanis(C4U)
\\sim Ueq, Uanis(C4M) \\sim Ueq, Uanis(C4P) \\sim Ueq: with sigma of 0.001 and
sigma for terminal atoms of 0.002
Uanis(C3D) \\sim Ueq, Uanis(C4Z) \\sim Ueq, Uanis(C4I) \\sim Ueq, Uanis(C29)
\\sim Ueq, Uanis(C4N) \\sim Ueq, Uanis(C4G) \\sim Ueq: with sigma of 0.001 and
sigma for terminal atoms of 0.002
Uanis(C47) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C1F) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C2M) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.002
Uanis(C48) \\sim Ueq, Uanis(C5E) \\sim Ueq, Uanis(C5O) \\sim Ueq, Uanis(C5K)
\\sim Ueq, Uanis(C51) \\sim Ueq, Uanis(C4W) \\sim Ueq: with sigma of 0.004 and
sigma for terminal atoms of 0.002
Uanis(C3Q) \\sim Ueq, Uanis(C23) \\sim Ueq, Uanis(C3V) \\sim Ueq: with sigma of
0.001 and sigma for terminal atoms of 0.002
Uanis(C4C) \\sim Ueq, Uanis(C4F) \\sim Ueq, Uanis(C4E) \\sim Ueq: with sigma of
0.006 and sigma for terminal atoms of 0.002
Uanis(C23) \\sim Ueq, Uanis(C3Q) \\sim Ueq, Uanis(C4T) \\sim Ueq, Uanis(C3L)
\\sim Ueq: with sigma of 0.006 and sigma for terminal atoms of 0.002
3.a Aromatic/amide H refined with riding coordinates:
 N58(H58), C70(H70), C73(H73), C75(H75), C78(H78), C80(H80), C84(H84),
 C86(H86), C87(H87), N88(H88), C89(H89), C90(H90), C91(H91), C92(H92), C94(H94),
  C95(H95), C96(H96), C97(H97), C98(H98), C99(H99), N10(H10), C1(H1), C4(H4),
 C7(H7), C8(H8), C11(H11), C12(H12), C14(H14), C15(H15), C16(H16), C17(H17),
 C18(H18), C1A(H1A), C1B(H1B), C1C(H1C), C1D(H1D), C1E(H1E), C1I(H1I), C1K(H1K),
  C1L(H1L), C1M(H1M), C1O(H1O), C1P(H1P), C1S(H1S), C1V(H1V), C1W(H1W),
 C1X(H1X), C1Y(H1Y), C1Z(H1Z), C20(H20), C21(H21), C22(H22), C23(H23), C24(H24),
  C25(H25), C26(H26), C27(H27), N29(H29), C2C(H2C), C2D(H2D), C2E(H2E),
 C2F(H2F), C2G(H2G), C2H(H2H), C2I(H2I), C2L(H2L), C2N(H2N), C2O(H2O), C2P(H2P),
  C2Q(H2Q), C2R(H2R), C2S(H2S), C2T(H2T), C2U(H2U), C2W(H2W), C2Y(H2Y),
 C2Z(H2Z), C30(H30), C32(H32), C34(H34), C35(H35), C36(H36), C37(H37), C38(H38),
  C39(H39), C3A(H3AA), C3B(H3B), C3C(H3CA), C3E(H3E), C3F(H3F), C3G(H3G),
 C3H(H3H), C3I(H3I), C3J(H3J), C3K(H3K), C3L(H3L), C3M(H3M), C3N(H3N), C3O(H3O),
  C3P(H3P), C3Q(H3Q), C3R(H3R), C3S(H3S), C3T(H3T), C3U(H3U), C3V(H3V),
 C3W(H3W), C3X(H3X), C3Y(H3Y), C3Z(H3Z), C40(H40), C41(H41), C42(H42), C43(H43),
  C44(H44), C45(H45), C46(H46), C48(H48), C4A(H4A), C4C(H4C), C4D(H4D),
 C4E(H4E), C4F(H4F), C4H(H4H), C4J(H4J), C4K(H4K), C4L(H4L), C4O(H4O), C4Q(H4Q),
  C4R(H4R), C4T(H4T), C4X(H4X), C4Y(H4Y), C51(H51), C58(H58A), C59(H59),
 C5C(H5C), C5D(H5D), C5F(H5F), C5H(H5H), C5I(H5I), C5B(H5B), C33(H33), C57(H57),
  C5K(H5K), C5O(H5O), C4M(H4M), C4V(H4V), C54(H54), C53(H53), C4U(H4U),
 C4N(H4N), C29(H29A), C4I(H4I), C4Z(H4Z), C3D(H3DA)
3.b Fitted hexagon refined as free rotating group:
 C5H(C5I,C5B,C33,C57,C50), C4M(C4V,C54,C53,C4U,C10), C4N(C29,C4I,C4Z,C3D,C4G)
3.c Idealised Me refined as rotating group:
 C83(H83A,H83B,H83C), C3(H3A,H3C,H3D), C1G(H1GA,H1GB,H1GC), C1J(H1JA,H1JB,
 H1JC), C1N(H1NA,H1NB,H1NC), C1U(H1UA,H1UB,H1UC), C2B(H2BA,H2BB,H2BC), C2M(H2MA,
 H2MB,H2MC), C2V(H2VA,H2VB,H2VC), C2X(H2XA,H2XB,H2XC), C47(H47A,H47B,H47C),
 C4B(H4BA,H4BB,H4BC), C4S(H4SA,H4SB,H4SC), C56(H56A,H56B,H56C), C5E(H5EA,H5EB,
 H5EC), C5G(H5GA,H5GB,H5GC), C4P(H4PA,H4PB,H4PC), C52(H52A,H52B,H52C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
V3B V 0.52273(7) 0.30308(3) 0.45006(3) 0.0293(3) Uani 1 1 d . . . . .
V1B V 0.36037(7) 0.20005(4) 0.49370(3) 0.0305(3) Uani 1 1 d . . . . .
V4A V 0.80333(7) 0.20241(4) 0.71701(3) 0.0321(3) Uani 1 1 d . . . . .
V2B V 0.51792(7) 0.20094(4) 0.44754(3) 0.0309(3) Uani 1 1 d . . . . .
V2A V 0.66230(7) 0.30765(4) 0.76809(3) 0.0360(3) Uani 1 1 d . . . . .
V1A V 0.81895(7) 0.30650(4) 0.72150(3) 0.0331(3) Uani 1 1 d . . . . .
V4B V 0.36470(7) 0.30426(4) 0.49654(3) 0.0297(3) Uani 1 1 d . . . . .
V3A V 0.64805(7) 0.20516(4) 0.76446(3) 0.0344(3) Uani 1 1 d . . . . .
Cl9 Cl 0.51574(9) 0.25028(5) 0.51049(4) 0.0278(4) Uani 1 1 d . . . . .
P3B P 0.52554(10) 0.35881(5) 0.51767(5) 0.0260(4) Uani 1 1 d . . . . .
P4B P 0.34510(10) 0.24963(5) 0.56342(5) 0.0268(4) Uani 1 1 d . . . . .
P1A P 0.67385(11) 0.37105(6) 0.70598(5) 0.0325(4) Uani 1 1 d . . . . .
P1B P 0.51531(11) 0.14156(5) 0.51200(5) 0.0290(4) Uani 1 1 d . . . . .
Cl14 Cl 0.65988(10) 0.25945(5) 0.70407(4) 0.0334(4) Uani 1 1 d . . . . .
P4A P 0.82763(10) 0.25661(6) 0.65104(5) 0.0292(4) Uani 1 1 d . . . . .
P3A P 0.64011(11) 0.14739(6) 0.69849(5) 0.0328(5) Uani 1 1 d . . . . .
P2A P 0.48820(12) 0.26377(6) 0.75144(5) 0.0361(5) Uani 1 1 d . . . . .
P2B P 0.68767(11) 0.25019(6) 0.46220(5) 0.0323(4) Uani 1 1 d . . . . .
O19B O 0.4162(3) 0.24971(13) 0.59504(11) 0.0292(11) Uani 1 1 d . . . . .
O1B O 0.2785(3) 0.17575(14) 0.48100(12) 0.0372(12) Uani 1 1 d . . . . .
O11B O 0.5178(3) 0.32918(14) 0.41570(11) 0.0381(12) Uani 1 1 d . . . . .
O1A O 0.9039(3) 0.32776(14) 0.73348(12) 0.0397(12) Uani 1 1 d . . . . .
O19A O 0.7573(3) 0.25994(14) 0.61928(12) 0.0351(12) Uani 1 1 d . . . . .
O15A O 0.7236(3) 0.16281(13) 0.69304(12) 0.0366(12) Uani 1 1 d . . . . .
O14B O 0.5875(3) 0.34653(13) 0.55052(11) 0.0297(11) Uani 1 1 d . . . . .
O14A O 0.5768(3) 0.15745(15) 0.66549(12) 0.0400(13) Uani 1 1 d . . . . .
O9B O 0.7374(3) 0.24814(14) 0.49970(12) 0.0374(12) Uani 1 1 d . . . . .
O10B O 0.6417(3) 0.28977(14) 0.45866(11) 0.0334(11) Uani 1 1 d . . . . .
O20B O 0.3529(3) 0.21142(13) 0.54251(11) 0.0321(11) Uani 1 1 d . . . . .
O10A O 0.5316(3) 0.22327(14) 0.75559(12) 0.0355(12) Uani 1 1 d . . . . .
O16A O 0.8804(3) 0.17390(14) 0.72730(12) 0.0398(12) Uani 1 1 d . . . . .
O15B O 0.4422(3) 0.34258(12) 0.52213(11) 0.0301(11) Uani 1 1 d . . . . .
O16B O 0.2865(3) 0.33087(15) 0.48571(12) 0.0414(13) Uani 1 1 d . . . . .
O5B O 0.5512(3) 0.15949(13) 0.48224(11) 0.0305(11) Uani 1 1 d . . . . .
O7A O 0.5424(3) 0.29996(14) 0.76041(12) 0.0374(12) Uani 1 1 d . . . . .
O17A O 0.8170(3) 0.21740(14) 0.66968(11) 0.0342(12) Uani 1 1 d . . . . .
O5A O 0.6338(3) 0.35244(14) 0.73462(12) 0.0358(12) Uani 1 1 d . . . . .
O11A O 0.6490(3) 0.18022(15) 0.79928(12) 0.0416(13) Uani 1 1 d . . . . .
O17B O 0.3481(2) 0.28904(13) 0.54353(11) 0.0304(11) Uani 1 1 d . . . . .
O2A O 0.7557(3) 0.35257(13) 0.70152(12) 0.0342(11) Uani 1 1 d . . . . .
O12B O 0.5577(3) 0.34460(13) 0.48556(11) 0.0298(11) Uani 1 1 d . . . . .
O12A O 0.6082(3) 0.16490(14) 0.72974(12) 0.0372(12) Uani 1 1 d . . . . .
O6B O 0.5134(3) 0.17627(14) 0.41229(12) 0.0384(12) Uani 1 1 d . . . . .
O18B O 0.3270(3) 0.25215(13) 0.48415(12) 0.0335(11) Uani 1 1 d . . . . .
O3B O 0.4288(3) 0.15486(13) 0.51439(11) 0.0323(11) Uani 1 1 d . . . . .
O7B O 0.6353(3) 0.21258(14) 0.45542(12) 0.0344(12) Uani 1 1 d . . . . .
O4B O 0.5715(3) 0.15302(13) 0.54635(12) 0.0338(12) Uani 1 1 d . . . . .
O6A O 0.6718(3) 0.33130(14) 0.80397(12) 0.0424(13) Uani 1 1 d . . . . .
O20A O 0.8268(3) 0.29426(14) 0.67257(12) 0.0348(12) Uani 1 1 d . . . . .
O9A O 0.4448(3) 0.26796(16) 0.71343(13) 0.0468(14) Uani 1 1 d . . . . .
O13B O 0.4180(3) 0.31032(13) 0.46000(11) 0.0328(11) Uani 1 1 d . . . . .
O4A O 0.6125(3) 0.36676(14) 0.67167(12) 0.0361(12) Uani 1 1 d . . . . .
O3A O 0.7688(3) 0.31139(14) 0.75895(12) 0.0358(12) Uani 1 1 d . . . . .
O8B O 0.5042(3) 0.25274(13) 0.43111(11) 0.0338(11) Uani 1 1 d . . . . .
C55 C 0.5204(4) 0.0859(2) 0.50842(18) 0.0323(17) Uani 1 1 d . . . . .
O13A O 0.7504(3) 0.19671(13) 0.75473(11) 0.0356(12) Uani 1 1 d . . . . .
O8A O 0.6724(3) 0.25596(14) 0.78313(11) 0.0351(12) Uani 1 1 d . . . . .
N58 N 0.4631(4) 0.2316(2) 0.35908(16) 0.0472(17) Uani 1 1 d . . . . .
H58 H 0.4867 0.2171 0.3759 0.057 Uiso 1 1 calc R . . . .
O2B O 0.4130(3) 0.19547(13) 0.45644(11) 0.0329(11) Uani 1 1 d . . . . .
C60 C 0.1807(4) 0.2570(2) 0.55183(17) 0.0286(16) Uani 1 1 d . . . . .
C61 C 0.2487(4) 0.24656(19) 0.58239(17) 0.0254(15) Uani 1 1 d . . . . .
C62 C 0.7181(4) 0.4432(2) 0.68074(17) 0.0311(16) Uani 1 1 d . . . . .
C63 C 0.6052(4) 0.43019(19) 0.51142(18) 0.0314(17) Uani 1 1 d . . . . .
C64 C 0.9258(4) 0.2551(2) 0.63217(19) 0.0331(17) Uani 1 1 d . . . . .
C65 C 0.5203(4) 0.4151(2) 0.51759(18) 0.0294(16) Uani 1 1 d . . . . .
C66 C 0.7660(4) 0.2492(2) 0.4326(2) 0.0404(19) Uani 1 1 d . . . . .
C67 C 0.6425(4) 0.0912(2) 0.70211(19) 0.0349(17) Uani 1 1 d . . . . .
O18A O 0.8468(3) 0.25175(14) 0.72993(12) 0.0401(13) Uani 1 1 d . . . . .
C69 C 0.5010(4) 0.43149(19) 0.55255(18) 0.0302(16) Uani 1 1 d . . . . .
C70 C 0.1326(4) 0.2914(2) 0.5506(2) 0.0376(18) Uani 1 1 d . . . . .
H70 H 0.1370 0.3084 0.5697 0.045 Uiso 1 1 calc R . . . .
C71 C 0.4448(4) 0.2682(2) 0.8157(2) 0.0392(19) Uani 1 1 d . . . . .
C72 C 0.9913(4) 0.2424(2) 0.66253(18) 0.0325(17) Uani 1 1 d . . . . .
C73 C 0.1600(4) 0.1863(2) 0.5934(2) 0.0409(19) Uani 1 1 d . . . . .
H73 H 0.1152 0.2005 0.5821 0.049 Uiso 1 1 calc R . . . .
C74 C 0.2369(4) 0.2030(2) 0.59572(18) 0.0324(17) Uani 1 1 d . . . . .
C75 C 0.2880(5) 0.1432(2) 0.6260(2) 0.053(2) Uani 1 1 d . . . . .
H75 H 0.3323 0.1287 0.6374 0.063 Uiso 1 1 calc R . . . .
C76 C 0.4488(4) 0.4248(2) 0.48879(19) 0.0328(17) Uani 1 1 d . . . . .
C77 C 0.6903(4) 0.4262(2) 0.71362(19) 0.0367(18) Uani 1 1 d . . . . .
C78 C 0.2736(4) 0.3178(2) 0.60713(18) 0.0350(18) Uani 1 1 d . . . . .
H78 H 0.2887 0.3260 0.5863 0.042 Uiso 1 1 calc R . . . .
C79 C 0.4735(5) 0.0696(2) 0.5374(2) 0.044(2) Uani 1 1 d . . . . .
C80 C 0.6785(4) 0.2882(2) 0.3851(2) 0.042(2) Uani 1 1 d . . . . .
H80 H 0.6793 0.3094 0.4009 0.051 Uiso 1 1 calc R . . . .
C81 C 0.8230(4) 0.2872(2) 0.4380(2) 0.0403(19) Uani 1 1 d . . . . .
C82 C 0.6871(4) 0.0823(2) 0.73895(17) 0.0334(17) Uani 1 1 d . . . . .
C83 C 0.4775(4) 0.2817(2) 0.59973(18) 0.0377(18) Uani 1 1 d . . . . .
H83A H 0.5062 0.2824 0.5802 0.057 Uiso 1 1 calc GR . . . .
H83B H 0.5155 0.2764 0.6202 0.057 Uiso 1 1 calc GR . . . .
H83C H 0.4511 0.3073 0.6020 0.057 Uiso 1 1 calc GR . . . .
C84 C 1.0048(4) 0.2674(3) 0.69203(18) 0.0396(19) Uani 1 1 d . . . . .
H84 H 0.9780 0.2922 0.6923 0.047 Uiso 1 1 calc R . . . .
C85 C 0.8143(4) 0.2096(2) 0.44036(19) 0.0390(19) Uani 1 1 d . . . . .
C86 C 0.7375(5) 0.4156(2) 0.77707(19) 0.0421(19) Uani 1 1 d . . . . .
H86 H 0.6867 0.4038 0.7780 0.050 Uiso 1 1 calc R . . . .
C87 C 0.7333(5) 0.0376(2) 0.6819(2) 0.048(2) Uani 1 1 d . . . . .
H87 H 0.7349 0.0258 0.7035 0.058 Uiso 1 1 calc R . . . .
N88 N 0.4553(4) 0.2716(2) 0.35956(17) 0.0501(18) Uani 1 1 d . . . . .
H88 H 0.4719 0.2872 0.3768 0.060 Uiso 1 1 calc R . . . .
C89 C 0.6700(5) 0.4704(2) 0.66005(19) 0.0413(19) Uani 1 1 d . . . . .
H89 H 0.6204 0.4788 0.6662 0.050 Uiso 1 1 calc R . . . .
C90 C 0.5131(4) 0.4722(2) 0.55947(18) 0.0374(18) Uani 1 1 d . . . . .
H90 H 0.5360 0.4881 0.5438 0.045 Uiso 1 1 calc R . . . .
C91 C 0.3773(4) 0.4434(2) 0.4965(2) 0.0399(19) Uani 1 1 d . . . . .
H91 H 0.3742 0.4517 0.5189 0.048 Uiso 1 1 calc R . . . .
C92 C 0.2313(4) 0.2664(2) 0.64310(18) 0.0356(17) Uani 1 1 d . . . . .
H92 H 0.2174 0.2395 0.6467 0.043 Uiso 1 1 calc R . . . .
C93 C 0.2520(4) 0.2779(2) 0.61159(17) 0.0298(16) Uani 1 1 d . . . . .
C94 C 0.8152(5) 0.4453(2) 0.6399(2) 0.052(2) Uani 1 1 d . . . . .
H94 H 0.8644 0.4366 0.6334 0.063 Uiso 1 1 calc R . . . .
C95 C 0.7178(5) 0.2207(3) 0.3708(2) 0.050(2) Uani 1 1 d . . . . .
H95 H 0.7450 0.1963 0.3765 0.060 Uiso 1 1 calc R . . . .
C96 C 1.0361(4) 0.3517(2) 0.6098(2) 0.044(2) Uani 1 1 d . . . . .
H96 H 1.0887 0.3624 0.6141 0.052 Uiso 1 1 calc R . . . .
C97 C 0.6868(4) 0.0893(2) 0.64208(17) 0.0329(17) Uani 1 1 d . . . . .
H97 H 0.6580 0.1133 0.6365 0.040 Uiso 1 1 calc R . . . .
C98 C 0.6726(4) 0.4266(2) 0.5368(2) 0.0403(19) Uani 1 1 d . . . . .
H98 H 0.6651 0.4159 0.5581 0.048 Uiso 1 1 calc R . . . .
C99 C 0.3813(5) 0.3402(2) 0.76581(19) 0.046(2) Uani 1 1 d . . . . .
H99 H 0.4378 0.3436 0.7692 0.056 Uiso 1 1 calc R . . . .
N10 N 0.2306(4) 0.2332(3) 0.35395(18) 0.061(2) Uani 1 1 d . . . . .
H10 H 0.2102 0.2182 0.3368 0.073 Uiso 1 1 calc R . . . .
C1 C 1.0352(4) 0.2069(2) 0.66242(19) 0.0354(17) Uani 1 1 d . . . . .
H1 H 1.0277 0.1904 0.6430 0.042 Uiso 1 1 calc R . . . .
C2 C 0.9176(4) 0.2235(2) 0.60288(18) 0.0322(17) Uani 1 1 d . . . . .
C3 C 0.5081(4) 0.1841(2) 0.66559(19) 0.0391(18) Uani 1 1 d . . . . .
H3A H 0.4875 0.1919 0.6424 0.059 Uiso 1 1 calc GR . . . .
H3C H 0.5250 0.2078 0.6789 0.059 Uiso 1 1 calc GR . . . .
H3D H 0.4659 0.1703 0.6755 0.059 Uiso 1 1 calc GR . . . .
C4 C 0.6203(5) 0.4471(2) 0.4798(2) 0.045(2) Uani 1 1 d . . . . .
H4 H 0.5773 0.4502 0.4618 0.054 Uiso 1 1 calc R . . . .
C5 C 0.6895(4) 0.0734(2) 0.67493(18) 0.0347(17) Uani 1 1 d . . . . .
C6 C 0.4762(5) 0.0748(2) 0.4722(2) 0.042(2) Uani 1 1 d . . . . .
C7 C 1.0187(4) 0.3156(2) 0.62424(19) 0.0391(19) Uani 1 1 d . . . . .
H7 H 1.0603 0.3025 0.6387 0.047 Uiso 1 1 calc R . . . .
C8 C 1.1020(4) 0.2179(2) 0.7198(2) 0.046(2) Uani 1 1 d . . . . .
H8 H 1.1381 0.2096 0.7390 0.055 Uiso 1 1 calc R . . . .
C9 C 0.7180(4) 0.2524(2) 0.39582(19) 0.0379(18) Uani 1 1 d . . . . .
C11 C 0.4928(5) 0.4904(2) 0.58857(19) 0.045(2) Uani 1 1 d . . . . .
H11 H 0.4993 0.5182 0.5918 0.054 Uiso 1 1 calc R . . . .
C12 C 0.7511(5) 0.4385(2) 0.5318(2) 0.049(2) Uani 1 1 d . . . . .
H12 H 0.7948 0.4357 0.5496 0.059 Uiso 1 1 calc R . . . .
C13 C 0.6085(5) 0.0715(2) 0.5137(2) 0.046(2) Uani 1 1 d . . . . .
C14 C 0.8299(4) 0.3129(2) 0.46604(19) 0.0407(19) Uani 1 1 d . . . . .
H14 H 0.7999 0.3079 0.4839 0.049 Uiso 1 1 calc R . . . .
C15 C 0.8295(4) 0.4502(2) 0.7454(2) 0.045(2) Uani 1 1 d . . . . .
H15 H 0.8416 0.4615 0.7250 0.054 Uiso 1 1 calc R . . . .
C16 C 0.8968(5) 0.2094(2) 0.45358(18) 0.0397(19) Uani 1 1 d . . . . .
H16 H 0.9237 0.2340 0.4582 0.048 Uiso 1 1 calc R . . . .
C17 C 0.7686(5) 0.0930(2) 0.7470(2) 0.043(2) Uani 1 1 d . . . . .
H17 H 0.7957 0.1048 0.7304 0.051 Uiso 1 1 calc R . . . .
C18 C 0.7906(5) 0.4295(2) 0.67003(19) 0.0418(19) Uani 1 1 d . . . . .
H18 H 0.8224 0.4100 0.6828 0.050 Uiso 1 1 calc R . . . .
C19 C 0.6105(5) 0.4474(2) 0.72151(19) 0.0379(18) Uani 1 1 d . . . . .
C1A C 0.8832(4) 0.1854(2) 0.60579(18) 0.0365(18) Uani 1 1 d . . . . .
H1A H 0.8607 0.1790 0.6255 0.044 Uiso 1 1 calc R . . . .
C1B C 0.1172(4) 0.2423(3) 0.49373(19) 0.043(2) Uani 1 1 d . . . . .
H1B H 0.1133 0.2257 0.4743 0.051 Uiso 1 1 calc R . . . .
C1C C 0.8198(5) 0.1354(3) 0.4407(2) 0.056(2) Uani 1 1 d . . . . .
H1C H 0.7937 0.1106 0.4356 0.067 Uiso 1 1 calc R . . . .
C1D C 0.4710(4) 0.4087(2) 0.57777(19) 0.0391(18) Uani 1 1 d . . . . .
H1D H 0.4631 0.3810 0.5745 0.047 Uiso 1 1 calc R . . . .
C1E C 0.8704(5) 0.2954(2) 0.4120(2) 0.045(2) Uani 1 1 d . . . . .
H1E H 0.8669 0.2780 0.3932 0.054 Uiso 1 1 calc R . . . .
C1F C 0.2685(5) 0.2194(3) 0.3831(2) 0.049(2) Uani 1 1 d . U . . .
C1G C 0.6638(4) 0.3247(2) 0.54804(19) 0.0379(18) Uani 1 1 d . . . . .
H1GA H 0.6916 0.3375 0.5310 0.057 Uiso 1 1 calc GR . . . .
H1GB H 0.6516 0.2971 0.5415 0.057 Uiso 1 1 calc GR . . . .
H1GC H 0.6983 0.3253 0.5700 0.057 Uiso 1 1 calc GR . . . .
C1H C 0.3486(5) 0.3010(2) 0.76770(18) 0.0386(19) Uani 1 1 d . . . . .
C1I C 0.8817(5) 0.1570(2) 0.5803(2) 0.046(2) Uani 1 1 d . . . . .
H1I H 0.8593 0.1315 0.5831 0.055 Uiso 1 1 calc R . . . .
C1J C 0.6897(4) 0.2314(2) 0.6134(2) 0.0418(19) Uani 1 1 d . . . . .
H1JA H 0.6533 0.2392 0.5931 0.063 Uiso 1 1 calc GR . . . .
H1JB H 0.6605 0.2316 0.6329 0.063 Uiso 1 1 calc GR . . . .
H1JC H 0.7105 0.2047 0.6105 0.063 Uiso 1 1 calc GR . . . .
C1K C 0.2731(4) 0.3462(2) 0.63382(19) 0.0396(19) Uani 1 1 d . . . . .
H1K H 0.2881 0.3729 0.6305 0.048 Uiso 1 1 calc R . . . .
C1L C 0.6749(4) 0.0921(2) 0.5075(2) 0.044(2) Uani 1 1 d . . . . .
H1L H 0.6668 0.1186 0.4996 0.053 Uiso 1 1 calc R . . . .
C1M C 0.7256(5) 0.0708(2) 0.6175(2) 0.044(2) Uani 1 1 d . . . . .
H1M H 0.7213 0.0820 0.5956 0.052 Uiso 1 1 calc R . . . .
C1N C 0.4559(5) 0.3019(3) 0.69098(19) 0.052(2) Uani 1 1 d . . . . .
H1NA H 0.4259 0.2970 0.6685 0.078 Uiso 1 1 calc GR . . . .
H1NB H 0.5131 0.3048 0.6892 0.078 Uiso 1 1 calc GR . . . .
H1NC H 0.4362 0.3263 0.7003 0.078 Uiso 1 1 calc GR . . . .
C1O C 0.4623(5) 0.4665(2) 0.6133(2) 0.047(2) Uani 1 1 d . . . . .
H1O H 0.4489 0.4779 0.6334 0.056 Uiso 1 1 calc R . . . .
C1P C 0.7765(5) 0.1714(2) 0.4349(2) 0.048(2) Uani 1 1 d . . . . .
H1P H 0.7205 0.1703 0.4271 0.058 Uiso 1 1 calc R . . . .
C1Q C 0.3564(4) 0.2237(2) 0.7727(2) 0.044(2) Uani 1 1 d . . . . .
C1R C 0.9429(4) 0.2975(2) 0.61848(19) 0.0360(18) Uani 1 1 d . . . . .
C1S C 0.3019(4) 0.1804(2) 0.6117(2) 0.045(2) Uani 1 1 d . . . . .
H1S H 0.3551 0.1902 0.6128 0.054 Uiso 1 1 calc R . . . .
C1T C 0.2646(5) 0.2875(3) 0.3850(2) 0.052(2) Uani 1 1 d . . . . .
C1U C 0.6414(5) 0.3564(3) 0.63881(18) 0.050(2) Uani 1 1 d . . . . .
H1UA H 0.6041 0.3375 0.6262 0.075 Uiso 1 1 calc GR . . . .
H1UB H 0.6949 0.3444 0.6435 0.075 Uiso 1 1 calc GR . . . .
H1UC H 0.6440 0.3806 0.6254 0.075 Uiso 1 1 calc GR . . . .
C1V C 0.4528(4) 0.4263(2) 0.60725(18) 0.0372(18) Uani 1 1 d . . . . .
H1V H 0.4333 0.4101 0.6237 0.045 Uiso 1 1 calc R . . . .
C1W C 0.1689(4) 0.2320(2) 0.5228(2) 0.0397(19) Uani 1 1 d . . . . .
H1W H 0.1972 0.2076 0.5233 0.048 Uiso 1 1 calc R . . . .
C1X C 0.4532(6) 0.0670(3) 0.5965(2) 0.063(3) Uani 1 1 d . . . . .
H1X H 0.4748 0.0716 0.6194 0.076 Uiso 1 1 calc R . . . .
C1Y C 1.0580(4) 0.2547(2) 0.7205(2) 0.043(2) Uani 1 1 d . . . . .
H1Y H 1.0649 0.2705 0.7404 0.052 Uiso 1 1 calc R . . . .
C1Z C 0.2310(4) 0.2951(2) 0.6700(2) 0.0423(19) Uani 1 1 d . . . . .
H1Z H 0.2175 0.2870 0.6911 0.051 Uiso 1 1 calc R . . . .
C20 C 0.6382(5) 0.2939(3) 0.3522(2) 0.049(2) Uani 1 1 d . . . . .
H20 H 0.6121 0.3184 0.3460 0.058 Uiso 1 1 calc R . . . .
C21 C 0.2127(5) 0.1274(2) 0.6241(2) 0.046(2) Uani 1 1 d . . . . .
H21 H 0.2050 0.1022 0.6339 0.055 Uiso 1 1 calc R . . . .
C22 C 0.9402(5) 0.1738(3) 0.46017(18) 0.045(2) Uani 1 1 d . . . . .
H22 H 0.9957 0.1747 0.4688 0.054 Uiso 1 1 calc R . . . .
C23 C 0.9771(5) 0.3717(3) 0.5893(2) 0.050(2) Uani 1 1 d . U . . .
H23 H 0.9884 0.3967 0.5799 0.059 Uiso 1 1 calc R . . . .
C24 C 0.3259(5) 0.2050(2) 0.8003(2) 0.049(2) Uani 1 1 d . . . . .
H24 H 0.3346 0.2174 0.8219 0.058 Uiso 1 1 calc R . . . .
C25 C 0.9490(4) 0.2322(3) 0.5731(2) 0.044(2) Uani 1 1 d . . . . .
H25 H 0.9716 0.2577 0.5704 0.052 Uiso 1 1 calc R . . . .
C26 C 0.7934(6) 0.4180(2) 0.8067(2) 0.056(2) Uani 1 1 d . . . . .
H26 H 0.7812 0.4070 0.8273 0.068 Uiso 1 1 calc R . . . .
C27 C 0.1476(5) 0.1484(2) 0.6077(2) 0.047(2) Uani 1 1 d . . . . .
H27 H 0.0951 0.1376 0.6059 0.057 Uiso 1 1 calc R . . . .
C28 C 0.4286(5) 0.2170(2) 0.3282(2) 0.046(2) Uani 1 1 d . . . . .
N29 N 0.2277(4) 0.2735(3) 0.35438(18) 0.059(2) Uani 1 1 d . . . . .
H29 H 0.2056 0.2884 0.3376 0.070 Uiso 1 1 calc R . . . .
C2A C 0.7551(5) 0.4304(2) 0.74544(18) 0.0380(18) Uani 1 1 d . . . . .
C2B C 0.5386(5) 0.1720(2) 0.57520(19) 0.046(2) Uani 1 1 d . . . . .
H2BA H 0.5343 0.2008 0.5715 0.069 Uiso 1 1 calc GR . . . .
H2BB H 0.5746 0.1667 0.5962 0.069 Uiso 1 1 calc GR . . . .
H2BC H 0.4854 0.1610 0.5768 0.069 Uiso 1 1 calc GR . . . .
C2C C 0.5324(4) 0.4327(2) 0.7111(2) 0.044(2) Uani 1 1 d . . . . .
H2C H 0.5249 0.4084 0.6990 0.052 Uiso 1 1 calc R . . . .
C2D C 0.2507(4) 0.3349(2) 0.6646(2) 0.043(2) Uani 1 1 d . . . . .
H2D H 0.2488 0.3541 0.6818 0.052 Uiso 1 1 calc R . . . .
C2E C 0.4232(5) 0.2988(2) 0.8374(2) 0.046(2) Uani 1 1 d . . . . .
H2E H 0.3847 0.3181 0.8285 0.056 Uiso 1 1 calc R . . . .
C2F C 0.7744(5) 0.0190(3) 0.6581(2) 0.058(2) Uani 1 1 d . . . . .
H2F H 0.8044 -0.0046 0.6638 0.069 Uiso 1 1 calc R . . . .
C2G C 0.2641(4) 0.2981(2) 0.76195(18) 0.0386(18) Uani 1 1 d . . . . .
H2G H 0.2400 0.2726 0.7625 0.046 Uiso 1 1 calc R . . . .
C2H C 0.5369(5) 0.0366(3) 0.6796(2) 0.052(2) Uani 1 1 d . . . . .
H2H H 0.5796 0.0229 0.6715 0.063 Uiso 1 1 calc R . . . .
C2I C 0.6988(5) 0.4592(2) 0.4753(2) 0.050(2) Uani 1 1 d . . . . .
H2I H 0.7073 0.4709 0.4546 0.060 Uiso 1 1 calc R . . . .
C2J C 0.4032(4) 0.2640(2) 0.77786(18) 0.0375(18) Uani 1 1 d . . . . .
C2K C 0.5516(5) 0.0741(2) 0.6957(2) 0.044(2) Uani 1 1 d . . . . .
C2L C 0.5002(5) 0.2389(3) 0.8299(2) 0.055(2) Uani 1 1 d . . . . .
H2L H 0.5145 0.2178 0.8163 0.066 Uiso 1 1 calc R . . . .
C2M C 0.6065(7) 0.1067(4) 0.3560(3) 0.105(4) Uani 1 1 d . U . . .
H2MA H 0.5804 0.1012 0.3330 0.157 Uiso 1 1 calc GR . . . .
H2MB H 0.6149 0.1355 0.3588 0.157 Uiso 1 1 calc GR . . . .
H2MC H 0.5723 0.0973 0.3722 0.157 Uiso 1 1 calc GR . . . .
C2N C 0.3820(5) 0.4190(2) 0.4301(2) 0.046(2) Uani 1 1 d . . . . .
H2N H 0.3843 0.4105 0.4076 0.055 Uiso 1 1 calc R . . . .
C2O C 0.9267(5) 0.3550(3) 0.4416(2) 0.057(2) Uani 1 1 d . . . . .
H2O H 0.9595 0.3781 0.4427 0.068 Uiso 1 1 calc R . . . .
C2P C 0.4571(5) 0.3013(3) 0.8715(2) 0.058(2) Uani 1 1 d . . . . .
H2P H 0.4422 0.3223 0.8852 0.070 Uiso 1 1 calc R . . . .
C2Q C 0.0775(4) 0.3011(3) 0.5214(2) 0.051(2) Uani 1 1 d . . . . .
H2Q H 0.0452 0.3242 0.5215 0.061 Uiso 1 1 calc R . . . .
C2R C 0.6262(5) 0.0338(3) 0.5311(2) 0.058(2) Uani 1 1 d . . . . .
H2R H 0.5836 0.0190 0.5382 0.069 Uiso 1 1 calc R . . . .
C2S C 0.9219(5) 0.3282(2) 0.4135(2) 0.049(2) Uani 1 1 d . . . . .
H2S H 0.9533 0.3327 0.3960 0.059 Uiso 1 1 calc R . . . .
C2T C 0.7669(5) 0.4739(3) 0.6195(2) 0.052(2) Uani 1 1 d . . . . .
H2T H 0.7835 0.4845 0.5996 0.062 Uiso 1 1 calc R . . . .
C2U C 0.4648(5) 0.4543(3) 0.7187(2) 0.057(2) Uani 1 1 d . . . . .
H2U H 0.4125 0.4440 0.7121 0.068 Uiso 1 1 calc R . . . .
C2V C 0.7316(5) 0.2142(2) 0.52224(19) 0.044(2) Uani 1 1 d . . . . .
H2VA H 0.7549 0.1906 0.5131 0.067 Uiso 1 1 calc GR . . . .
H2VB H 0.6752 0.2091 0.5241 0.067 Uiso 1 1 calc GR . . . .
H2VC H 0.7610 0.2201 0.5446 0.067 Uiso 1 1 calc GR . . . .
C2W C 0.9009(5) 0.1365(2) 0.4538(2) 0.048(2) Uani 1 1 d . . . . .
H2W H 0.9300 0.1125 0.4586 0.058 Uiso 1 1 calc R . . . .
C2X C 0.0430(7) 0.1110(4) 0.7485(3) 0.110(4) Uani 1 1 d . U . . .
H2XA H 0.0932 0.1059 0.7636 0.165 Uiso 1 1 calc GR . . . .
H2XB H -0.0019 0.0994 0.7581 0.165 Uiso 1 1 calc GR . . . .
H2XC H 0.0350 0.1398 0.7459 0.165 Uiso 1 1 calc GR . . . .
C2Y C 0.6188(5) 0.4842(2) 0.7381(2) 0.047(2) Uani 1 1 d . . . . .
H2Y H 0.6708 0.4951 0.7447 0.056 Uiso 1 1 calc R . . . .
C2Z C 0.4498(5) 0.4130(2) 0.4554(2) 0.0424(19) Uani 1 1 d . . . . .
H2Z H 0.4966 0.4008 0.4495 0.051 Uiso 1 1 calc R . . . .
C30 C 0.0702(5) 0.2775(3) 0.4931(2) 0.054(2) Uani 1 1 d . . . . .
H30 H 0.0345 0.2847 0.4734 0.064 Uiso 1 1 calc R . . . .
C31 C 0.4173(5) 0.2837(2) 0.32893(19) 0.044(2) Uani 1 1 d . . . . .
C32 C 0.7529(5) 0.0778(2) 0.5119(2) 0.043(2) Uani 1 1 d . . . . .
H32 H 0.7944 0.0925 0.5040 0.052 Uiso 1 1 calc R . . . .
C34 C 0.3309(5) 0.3741(3) 0.75900(19) 0.049(2) Uani 1 1 d . . . . .
H34 H 0.3539 0.3997 0.7577 0.059 Uiso 1 1 calc R . . . .
C35 C 0.4895(5) 0.0926(3) 0.7102(3) 0.071(3) Uani 1 1 d . . . . .
H35 H 0.4992 0.1159 0.7235 0.086 Uiso 1 1 calc R . . . .
C36 C 0.7637(5) 0.4542(2) 0.5010(2) 0.049(2) Uani 1 1 d . . . . .
H36 H 0.8162 0.4615 0.4974 0.058 Uiso 1 1 calc R . . . .
C37 C 0.9131(5) 0.1659(3) 0.5502(2) 0.048(2) Uani 1 1 d . . . . .
H37 H 0.9110 0.1468 0.5327 0.058 Uiso 1 1 calc R . . . .
C38 C 1.0908(4) 0.1952(2) 0.6910(2) 0.043(2) Uani 1 1 d . . . . .
H38 H 1.1206 0.1713 0.6901 0.052 Uiso 1 1 calc R . . . .
C39 C 0.3979(6) 0.2507(3) 0.3093(2) 0.069(3) Uani 1 1 d . . . . .
H39 H 0.3692 0.2504 0.2870 0.082 Uiso 1 1 calc R . . . .
C3A C 0.8861(5) 0.4533(3) 0.7752(2) 0.061(3) Uani 1 1 d . . . . .
H3AA H 0.9357 0.4664 0.7745 0.073 Uiso 1 1 calc R . . . .
C3B C 0.6759(5) 0.2269(3) 0.3376(2) 0.062(3) Uani 1 1 d . . . . .
H3B H 0.6746 0.2061 0.3215 0.074 Uiso 1 1 calc R . . . .
C3C C 0.7704(5) 0.0362(3) 0.6249(2) 0.055(2) Uani 1 1 d . . . . .
H3CA H 0.7977 0.0242 0.6084 0.066 Uiso 1 1 calc R . . . .
C3E C 0.3123(4) 0.4493(2) 0.4714(2) 0.042(2) Uani 1 1 d . . . . .
H3E H 0.2658 0.4622 0.4769 0.051 Uiso 1 1 calc R . . . .
C3F C 0.8106(5) 0.0860(2) 0.7802(2) 0.050(2) Uani 1 1 d . . . . .
H3F H 0.8652 0.0934 0.7857 0.060 Uiso 1 1 calc R . . . .
C3G C 0.0625(7) 0.0551(4) 0.6536(3) 0.091(3) Uani 1 1 d . U . . .
H3G H 0.0682 0.0424 0.6329 0.109 Uiso 1 1 calc R . . . .
C3H C 0.7059(5) 0.0186(3) 0.5378(2) 0.062(3) Uani 1 1 d . . . . .
H3H H 0.7168 -0.0063 0.5487 0.074 Uiso 1 1 calc R . . . .
C3I C 0.5347(5) 0.2410(3) 0.8645(2) 0.065(3) Uani 1 1 d . . . . .
H3I H 0.5722 0.2213 0.8737 0.078 Uiso 1 1 calc R . . . .
C3J C 0.2136(5) 0.3320(3) 0.7553(2) 0.050(2) Uani 1 1 d . . . . .
H3J H 0.1570 0.3289 0.7516 0.060 Uiso 1 1 calc R . . . .
C3K C 0.6487(5) 0.0640(2) 0.7645(2) 0.046(2) Uani 1 1 d . . . . .
H3K H 0.5938 0.0565 0.7596 0.055 Uiso 1 1 calc R . . . .
C3L C 0.6902(6) 0.0570(3) 0.7961(2) 0.063(2) Uani 1 1 d . U . . .
H3L H 0.6639 0.0444 0.8126 0.075 Uiso 1 1 calc R . . . .
C3M C 0.4742(6) 0.4908(3) 0.7360(2) 0.060(2) Uani 1 1 d . . . . .
H3M H 0.4287 0.5050 0.7412 0.072 Uiso 1 1 calc R . . . .
C3N C 0.8693(5) 0.4372(3) 0.8056(2) 0.058(2) Uani 1 1 d . . . . .
H3N H 0.9078 0.4390 0.8253 0.069 Uiso 1 1 calc R . . . .
C3O C 0.6952(5) 0.4856(2) 0.62956(19) 0.046(2) Uani 1 1 d . . . . .
H3O H 0.6618 0.5040 0.6161 0.056 Uiso 1 1 calc R . . . .
C3P C 0.6372(5) 0.2625(3) 0.3283(2) 0.059(3) Uani 1 1 d . . . . .
H3P H 0.6100 0.2658 0.3060 0.071 Uiso 1 1 calc R . . . .
C3Q C 0.9006(6) 0.3553(3) 0.5823(3) 0.072(3) Uani 1 1 d . U . . .
H3Q H 0.8600 0.3687 0.5675 0.086 Uiso 1 1 calc R . . . .
C3R C 0.3497(6) 0.0415(3) 0.5556(3) 0.068(3) Uani 1 1 d . . . . .
H3R H 0.2997 0.0282 0.5504 0.082 Uiso 1 1 calc R . . . .
C3S C 0.9476(4) 0.2035(3) 0.5469(2) 0.049(2) Uani 1 1 d . . . . .
H3S H 0.9700 0.2098 0.5271 0.059 Uiso 1 1 calc R . . . .
C3T C 0.4823(6) 0.0370(3) 0.4182(2) 0.070(3) Uani 1 1 d . . . . .
H3T H 0.5084 0.0195 0.4047 0.085 Uiso 1 1 calc R . . . .
C3U C 0.8410(8) 0.0503(4) 0.3737(3) 0.112(4) Uani 1 1 d . U . . .
H3U H 0.8928 0.0387 0.3781 0.134 Uiso 1 1 calc R . . . .
C3V C 0.8832(5) 0.3181(3) 0.5973(2) 0.059(2) Uani 1 1 d . U . . .
H3V H 0.8306 0.3074 0.5929 0.071 Uiso 1 1 calc R . . . .
C3W C 0.5494(5) 0.5056(3) 0.7454(2) 0.055(2) Uani 1 1 d . . . . .
H3W H 0.5561 0.5303 0.7568 0.066 Uiso 1 1 calc R . . . .
C3X C 0.4991(5) 0.0774(2) 0.5705(2) 0.055(2) Uani 1 1 d . . . . .
H3X H 0.5494 0.0902 0.5766 0.067 Uiso 1 1 calc R . . . .
C3Y C 0.4596(5) 0.0194(3) 0.6754(2) 0.062(3) Uani 1 1 d . . . . .
H3Y H 0.4502 -0.0058 0.6649 0.075 Uiso 1 1 calc R . . . .
C3Z C 0.7011(6) 0.0530(3) 0.3833(3) 0.077(3) Uani 1 1 d . . . . .
H3Z H 0.6584 0.0428 0.3938 0.093 Uiso 1 1 calc R . . . .
C40 C 0.2838(5) 0.1692(3) 0.7966(3) 0.063(3) Uani 1 1 d . . . . .
H40 H 0.2645 0.1577 0.8155 0.075 Uiso 1 1 calc R . . . .
C41 C 0.5135(5) 0.2724(3) 0.8856(2) 0.058(2) Uani 1 1 d . . . . .
H41 H 0.5368 0.2739 0.9086 0.069 Uiso 1 1 calc R . . . .
C42 C 0.3376(5) 0.2050(3) 0.7412(2) 0.055(2) Uani 1 1 d . . . . .
H42 H 0.3535 0.2174 0.7219 0.065 Uiso 1 1 calc R . . . .
C43 C 0.3959(5) 0.0524(3) 0.5298(3) 0.066(3) Uani 1 1 d . . . . .
H43 H 0.3741 0.0481 0.5068 0.079 Uiso 1 1 calc R . . . .
C44 C 0.8816(5) 0.3460(3) 0.4674(2) 0.053(2) Uani 1 1 d . . . . .
H44 H 0.8860 0.3629 0.4866 0.064 Uiso 1 1 calc R . . . .
C45 C 0.3137(5) 0.4367(2) 0.4377(2) 0.049(2) Uani 1 1 d . . . . .
H45 H 0.2684 0.4404 0.4209 0.059 Uiso 1 1 calc R . . . .
C46 C 0.3985(6) 0.0396(3) 0.6870(2) 0.069(3) Uani 1 1 d . . . . .
H46 H 0.3461 0.0286 0.6828 0.083 Uiso 1 1 calc R . . . .
C47 C 0.4045(6) 0.3278(3) 0.3218(2) 0.066(3) Uani 1 1 d . U . . .
H47A H 0.3477 0.3328 0.3136 0.099 Uiso 1 1 calc GR . . . .
H47B H 0.4369 0.3361 0.3045 0.099 Uiso 1 1 calc GR . . . .
H47C H 0.4207 0.3430 0.3425 0.099 Uiso 1 1 calc GR . . . .
C48 C 0.7569(9) 0.4342(4) 0.3453(4) 0.122(5) Uani 1 1 d . U . . .
H48 H 0.7932 0.4442 0.3313 0.146 Uiso 1 1 calc R . . . .
C49 C 0.0472(7) 0.0930(3) 0.7153(3) 0.079(3) Uani 1 1 d . . . . .
C4A C 0.2465(5) 0.3694(3) 0.75415(19) 0.052(2) Uani 1 1 d . . . . .
H4A H 0.2127 0.3920 0.7501 0.062 Uiso 1 1 calc R . . . .
C4B C 0.2808(6) 0.1758(3) 0.3897(2) 0.076(3) Uani 1 1 d . . . . .
H4BA H 0.2430 0.1606 0.3737 0.114 Uiso 1 1 calc GR . . . .
H4BB H 0.2717 0.1697 0.4128 0.114 Uiso 1 1 calc GR . . . .
H4BC H 0.3359 0.1685 0.3870 0.114 Uiso 1 1 calc GR . . . .
C4C C 0.3630(6) 0.0765(3) 0.4239(2) 0.059(2) Uani 1 1 d . U . . .
H4C H 0.3112 0.0863 0.4152 0.071 Uiso 1 1 calc R . . . .
C4D C 0.4088(5) 0.0743(3) 0.7039(2) 0.057(2) Uani 1 1 d . . . . .
H4D H 0.3646 0.0870 0.7118 0.069 Uiso 1 1 calc R . . . .
C4E C 0.4027(6) 0.0517(3) 0.4056(3) 0.071(3) Uani 1 1 d . U . . .
H4E H 0.3778 0.0437 0.3838 0.086 Uiso 1 1 calc R . . . .
C4F C 0.4024(6) 0.0878(3) 0.4576(2) 0.066(3) Uani 1 1 d . U . . .
H4F H 0.3745 0.1054 0.4703 0.079 Uiso 1 1 calc R . . . .
C4H C 0.5226(6) 0.0487(3) 0.4514(2) 0.061(3) Uani 1 1 d . . . . .
H4H H 0.5756 0.0403 0.4595 0.073 Uiso 1 1 calc R . . . .
C4J C 0.3814(6) 0.0512(3) 0.5892(3) 0.067(3) Uani 1 1 d . . . . .
H4J H 0.3504 0.0463 0.6068 0.081 Uiso 1 1 calc R . . . .
C4K C 0.7750(7) 0.0346(4) 0.3895(3) 0.095(4) Uani 1 1 d . U . . .
H4K H 0.7827 0.0121 0.4039 0.114 Uiso 1 1 calc R . . . .
C4L C 0.7692(5) 0.0423(3) 0.5277(3) 0.066(3) Uani 1 1 d . . . . .
H4L H 0.8230 0.0330 0.5320 0.079 Uiso 1 1 calc R . . . .
C4O C 0.2697(5) 0.1504(3) 0.7656(3) 0.076(3) Uani 1 1 d . . . . .
H4O H 0.2427 0.1255 0.7634 0.091 Uiso 1 1 calc R . . . .
C4Q C 0.2918(6) 0.2530(3) 0.4037(2) 0.060(2) Uani 1 1 d . . . . .
H4Q H 0.3204 0.2525 0.4259 0.072 Uiso 1 1 calc R . . . .
C4R C 0.1232(7) 0.0494(3) 0.6823(3) 0.092(3) Uani 1 1 d . U . . .
H4R H 0.1674 0.0326 0.6800 0.110 Uiso 1 1 calc R . . . .
C4S C 0.4249(6) 0.1725(2) 0.3211(2) 0.067(3) Uani 1 1 d . . . . .
H4SA H 0.4648 0.1655 0.3066 0.100 Uiso 1 1 calc GR . . . .
H4SB H 0.3712 0.1655 0.3097 0.100 Uiso 1 1 calc GR . . . .
H4SC H 0.4361 0.1579 0.3424 0.100 Uiso 1 1 calc GR . . . .
C4T C 0.7700(6) 0.0681(2) 0.8041(2) 0.056(2) Uani 1 1 d . U . . .
H4T H 0.7973 0.0635 0.8263 0.067 Uiso 1 1 calc R . . . .
C4W C 0.6125(7) 0.4248(3) 0.3542(3) 0.083(3) Uani 1 1 d . U . . .
C4X C 0.8270(7) 0.0820(4) 0.3524(3) 0.094(4) Uani 1 1 d . U . . .
H4X H 0.8680 0.0913 0.3404 0.113 Uiso 1 1 calc R . . . .
C4Y C 0.2954(5) 0.1682(3) 0.7372(3) 0.064(3) Uani 1 1 d . . . . .
H4Y H 0.2849 0.1558 0.7157 0.077 Uiso 1 1 calc R . . . .
C51 C 0.7253(7) 0.4001(3) 0.3929(3) 0.079(3) Uani 1 1 d . U . . .
H51 H 0.7442 0.3852 0.4126 0.095 Uiso 1 1 calc R . . . .
C56 C 0.2689(6) 0.3293(3) 0.3933(3) 0.085(3) Uani 1 1 d . . . . .
H56A H 0.2500 0.3450 0.3731 0.127 Uiso 1 1 calc GR . . . .
H56B H 0.3246 0.3365 0.4017 0.127 Uiso 1 1 calc GR . . . .
H56C H 0.2352 0.3349 0.4107 0.127 Uiso 1 1 calc GR . . . .
C58 C 0.1201(7) 0.0667(3) 0.7120(3) 0.094(4) Uani 1 1 d . U . . .
H58A H 0.1616 0.0628 0.7305 0.113 Uiso 1 1 calc R . . . .
C59 C -0.0063(9) 0.0796(4) 0.6554(3) 0.104(4) Uani 1 1 d . . . . .
H59 H -0.0459 0.0840 0.6363 0.124 Uiso 1 1 calc R . . . .
C5A C 0.6868(6) 0.0855(3) 0.3623(3) 0.073(3) Uani 1 1 d . . . . .
C5C C 0.7533(7) 0.1008(4) 0.3482(3) 0.095(4) Uani 1 1 d . . . . .
H5C H 0.7467 0.1247 0.3355 0.114 Uiso 1 1 calc R . . . .
C5D C 0.6725(6) 0.4383(3) 0.3362(3) 0.080(3) Uani 1 1 d . . . . .
H5D H 0.6549 0.4517 0.3156 0.096 Uiso 1 1 calc R . . . .
C5E C 0.5311(6) 0.4293(3) 0.3433(3) 0.094(4) Uani 1 1 d . U . . .
H5EA H 0.5182 0.4577 0.3408 0.141 Uiso 1 1 calc GR . . . .
H5EB H 0.5008 0.4175 0.3599 0.141 Uiso 1 1 calc GR . . . .
H5EC H 0.5168 0.4159 0.3215 0.141 Uiso 1 1 calc GR . . . .
C5F C -0.0120(8) 0.0966(3) 0.6871(3) 0.090(4) Uani 1 1 d . . . . .
H5F H -0.0589 0.1114 0.6894 0.108 Uiso 1 1 calc R . . . .
C5G C -0.0174(8) 0.3930(4) 0.3070(4) 0.144(5) Uani 1 1 d . U . . .
H5GA H -0.0650 0.4059 0.2946 0.217 Uiso 1 1 calc GR . . . .
H5GB H -0.0309 0.3658 0.3129 0.217 Uiso 1 1 calc GR . . . .
H5GC H 0.0253 0.3922 0.2928 0.217 Uiso 1 1 calc GR . . . .
C5H C -0.0070(4) 0.4568(3) 0.3451(2) 0.115(4) Uani 1 1 d . U . . .
H5H H -0.0382 0.4718 0.3279 0.138 Uiso 1 1 calc R . . . .
C5I C 0.0211(5) 0.47455(18) 0.3767(2) 0.111(4) Uani 1 1 d G U . . .
H5I H 0.0087 0.5015 0.3807 0.133 Uiso 1 1 calc R . . . .
C5B C 0.0677(5) 0.4520(3) 0.40244(17) 0.118(4) Uani 1 1 d G U . . .
H5B H 0.0865 0.4639 0.4236 0.141 Uiso 1 1 calc R . . . .
C33 C 0.0862(4) 0.4117(2) 0.39648(19) 0.108(4) Uani 1 1 d G U . . .
H33 H 0.1174 0.3966 0.4137 0.129 Uiso 1 1 calc R . . . .
C57 C 0.0581(5) 0.39391(18) 0.3648(2) 0.099(4) Uani 1 1 d G U . . .
H57 H 0.0705 0.3669 0.3609 0.118 Uiso 1 1 calc R . . . .
C50 C 0.0115(5) 0.4164(3) 0.33915(17) 0.101(4) Uani 1 1 d G U . . .
C5K C 0.6446(7) 0.4041(3) 0.3855(3) 0.086(3) Uani 1 1 d . U . . .
H5K H 0.6100 0.3938 0.4001 0.103 Uiso 1 1 calc R . . . .
C5O C 0.7837(9) 0.4151(4) 0.3752(4) 0.121(5) Uani 1 1 d . U . . .
H5O H 0.8392 0.4123 0.3833 0.146 Uiso 1 1 calc R . . . .
C4M C 0.1391(5) 0.0367(3) 0.5204(2) 0.112(4) Uani 1 1 d . U . . .
H4M H 0.1830 0.0333 0.5083 0.134 Uiso 1 1 calc R . . . .
C4V C 0.0998(7) 0.0030(2) 0.5317(3) 0.166(6) Uani 1 1 d G U . . .
H4V H 0.1174 -0.0230 0.5271 0.199 Uiso 1 1 calc R . . . .
C54 C 0.0342(6) 0.0082(3) 0.5498(3) 0.179(7) Uani 1 1 d G U . . .
H54 H 0.0079 -0.0144 0.5574 0.215 Uiso 1 1 calc R . . . .
C53 C 0.0079(5) 0.0470(4) 0.5567(2) 0.148(6) Uani 1 1 d G U . . .
H53 H -0.0360 0.0505 0.5688 0.177 Uiso 1 1 calc R . . . .
C4U C 0.0472(6) 0.0807(3) 0.5454(2) 0.147(5) Uani 1 1 d G U . . .
H4U H 0.0296 0.1067 0.5500 0.177 Uiso 1 1 calc R . . . .
C10 C 0.1128(5) 0.0756(2) 0.5273(2) 0.101(4) Uani 1 1 d G . . . .
C4N C 0.1754(5) 0.4597(3) 0.6896(3) 0.138(5) Uani 1 1 d . U . . .
H4N H 0.2200 0.4695 0.6801 0.165 Uiso 1 1 calc R . . . .
C29 C 0.1237(6) 0.4310(3) 0.67180(19) 0.115(4) Uani 1 1 d G U . . .
H29A H 0.1337 0.4217 0.6504 0.138 Uiso 1 1 calc R . . . .
C4I C 0.0570(6) 0.4163(3) 0.6860(3) 0.166(6) Uani 1 1 d G U . . .
H4I H 0.0224 0.3971 0.6741 0.199 Uiso 1 1 calc R . . . .
C4Z C 0.0421(5) 0.4303(3) 0.7179(3) 0.155(6) Uani 1 1 d G U . . .
H4Z H -0.0025 0.4204 0.7274 0.186 Uiso 1 1 calc R . . . .
C3D C 0.0938(6) 0.4589(3) 0.73567(19) 0.107(4) Uani 1 1 d G U . . .
H3DA H 0.0838 0.4682 0.7570 0.128 Uiso 1 1 calc R . . . .
C4G C 0.1605(6) 0.4736(3) 0.7215(3) 0.140(5) Uani 1 1 d G U . . .
C4P C 0.1591(9) 0.1089(5) 0.5176(4) 0.165(6) Uani 1 1 d . U . . .
H4PA H 0.2000 0.1162 0.5366 0.248 Uiso 1 1 calc GR . . . .
H4PB H 0.1233 0.1316 0.5116 0.248 Uiso 1 1 calc GR . . . .
H4PC H 0.1851 0.1014 0.4982 0.248 Uiso 1 1 calc GR . . . .
C52 C 0.2154(10) 0.4975(5) 0.7408(4) 0.181(7) Uani 1 1 d . . . . .
H52A H 0.2298 0.4856 0.7632 0.271 Uiso 1 1 calc GR . . . .
H52B H 0.1920 0.5239 0.7431 0.271 Uiso 1 1 calc GR . . . .
H52C H 0.2636 0.5000 0.7299 0.271 Uiso 1 1 calc GR . . . .


_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
V3B O11B 1.591(5) . ?
V3B O10B 1.992(5) . ?
V3B O12B 1.977(5) . ?
V3B O13B 1.842(4) . ?
V3B O8B 1.825(5) . ?
V1B O1B 1.587(4) . ?
V1B O20B 1.973(4) . ?
V1B O18B 1.824(4) . ?
V1B O3B 1.971(4) . ?
V1B O2B 1.812(5) . ?
V4A O15A 1.989(5) . ?
V4A O16A 1.585(5) . ?
V4A O17A 1.966(5) . ?
V4A O13A 1.835(5) . ?
V4A O18A 1.818(5) . ?
V2B O5B 1.950(4) . ?
V2B O6B 1.597(5) . ?
V2B O7B 1.955(4) . ?
V2B O8B 1.826(4) . ?
V2B O2B 1.825(5) . ?
V2A O7A 1.974(5) . ?
V2A O5A 1.985(5) . ?
V2A O6A 1.597(5) . ?
V2A O3A 1.848(5) . ?
V2A O8A 1.802(5) . ?
V1A O1A 1.576(5) . ?
V1A O2A 1.941(5) . ?
V1A O20A 1.984(5) . ?
V1A O3A 1.796(5) . ?
V1A O18A 1.878(5) . ?
V4B O15B 1.966(5) . ?
V4B O16B 1.567(5) . ?
V4B O17B 1.968(4) . ?
V4B O18B 1.866(5) . ?
V4B O13B 1.799(5) . ?
V3A O10A 1.993(5) . ?
V3A O11A 1.592(5) . ?
V3A O12A 1.946(5) . ?
V3A O13A 1.806(5) . ?
V3A O8A 1.847(5) . ?
P3B O14B 1.577(5) . ?
P3B O15B 1.509(5) . ?
P3B O12B 1.511(4) . ?
P3B C65 1.855(7) . ?
P4B O19B 1.578(5) . ?
P4B O20B 1.518(4) . ?
P4B O17B 1.519(5) . ?
P4B C61 1.855(6) . ?
P1A O5A 1.514(5) . ?
P1A O2A 1.515(5) . ?
P1A O4A 1.569(5) . ?
P1A C77 1.855(7) . ?
P1B O5B 1.505(5) . ?
P1B O3B 1.509(5) . ?
P1B O4B 1.566(5) . ?
P1B C55 1.842(7) . ?
P4A O19A 1.577(5) . ?
P4A O17A 1.507(5) . ?
P4A O20A 1.502(5) . ?
P4A C64 1.878(7) . ?
P3A O15A 1.513(5) . ?
P3A O14A 1.576(5) . ?
P3A O12A 1.518(5) . ?
P3A C67 1.855(7) . ?
P2A O10A 1.512(5) . ?
P2A O7A 1.501(5) . ?
P2A O9A 1.563(5) . ?
P2A C2J 1.862(7) . ?
P2B O9B 1.578(5) . ?
P2B O10B 1.504(5) . ?
P2B O7B 1.511(5) . ?
P2B C66 1.859(7) . ?
O19B C83 1.453(7) . ?
O19A C1J 1.451(8) . ?
O14B C1G 1.465(7) . ?
O14A C3 1.433(8) . ?
O9B C2V 1.438(8) . ?
O4B C2B 1.465(8) . ?
O9A C1N 1.451(8) . ?
O4A C1U 1.479(8) . ?
C55 C79 1.562(10) . ?
C55 C6 1.545(10) . ?
C55 C13 1.514(10) . ?
N58 H58 0.8600 . ?
N58 N88 1.325(9) . ?
N58 C28 1.351(9) . ?
C60 C61 1.556(9) . ?
C60 C70 1.379(9) . ?
C60 C1W 1.396(10) . ?
C61 C74 1.548(9) . ?
C61 C93 1.537(9) . ?
C62 C77 1.537(9) . ?
C62 C89 1.379(10) . ?
C62 C18 1.399(9) . ?
C63 C65 1.539(9) . ?
C63 C98 1.386(10) . ?
C63 C4 1.416(9) . ?
C64 C72 1.545(9) . ?
C64 C2 1.543(10) . ?
C64 C1R 1.536(9) . ?
C65 C69 1.550(9) . ?
C65 C76 1.543(9) . ?
C66 C81 1.560(10) . ?
C66 C85 1.537(10) . ?
C66 C9 1.547(11) . ?
C67 C82 1.552(9) . ?
C67 C5 1.525(10) . ?
C67 C2K 1.588(10) . ?
C69 C90 1.378(9) . ?
C69 C1D 1.388(9) . ?
C70 H70 0.9300 . ?
C70 C2Q 1.391(10) . ?
C71 C2E 1.401(10) . ?
C71 C2J 1.548(10) . ?
C71 C2L 1.389(11) . ?
C72 C84 1.411(10) . ?
C72 C1 1.376(9) . ?
C73 H73 0.9300 . ?
C73 C74 1.375(9) . ?
C73 C27 1.395(10) . ?
C74 C1S 1.380(10) . ?
C75 H75 0.9300 . ?
C75 C1S 1.381(10) . ?
C75 C21 1.340(10) . ?
C76 C91 1.401(9) . ?
C76 C2Z 1.368(10) . ?
C77 C19 1.561(9) . ?
C77 C2A 1.527(10) . ?
C78 H78 0.9300 . ?
C78 C93 1.381(9) . ?
C78 C1K 1.404(9) . ?
C79 C3X 1.330(11) . ?
C79 C43 1.391(11) . ?
C80 H80 0.9300 . ?
C80 C9 1.383(10) . ?
C80 C20 1.376(10) . ?
C81 C14 1.378(10) . ?
C81 C1E 1.400(9) . ?
C82 C17 1.381(10) . ?
C82 C3K 1.399(10) . ?
C83 H83A 0.9600 . ?
C83 H83B 0.9600 . ?
C83 H83C 0.9600 . ?
C84 H84 0.9300 . ?
C84 C1Y 1.382(10) . ?
C85 C16 1.384(10) . ?
C85 C1P 1.407(10) . ?
C86 H86 0.9300 . ?
C86 C26 1.378(11) . ?
C86 C2A 1.404(10) . ?
C87 H87 0.9300 . ?
C87 C5 1.389(10) . ?
C87 C2F 1.376(10) . ?
N88 H88 0.8600 . ?
N88 C31 1.333(9) . ?
C89 H89 0.9300 . ?
C89 C3O 1.414(10) . ?
C90 H90 0.9300 . ?
C90 C11 1.373(9) . ?
C91 H91 0.9300 . ?
C91 C3E 1.360(10) . ?
C92 H92 0.9300 . ?
C92 C93 1.382(9) . ?
C92 C1Z 1.416(9) . ?
C94 H94 0.9300 . ?
C94 C18 1.404(10) . ?
C94 C2T 1.410(11) . ?
C95 H95 0.9300 . ?
C95 C9 1.435(10) . ?
C95 C3B 1.397(11) . ?
C96 H96 0.9300 . ?
C96 C7 1.368(10) . ?
C96 C23 1.341(10) . ?
C97 H97 0.9300 . ?
C97 C5 1.386(9) . ?
C97 C1M 1.375(9) . ?
C98 H98 0.9300 . ?
C98 C12 1.395(10) . ?
C99 H99 0.9300 . ?
C99 C1H 1.405(10) . ?
C99 C34 1.393(10) . ?
N10 H10 0.8600 . ?
N10 C1F 1.302(10) . ?
N10 N29 1.329(10) . ?
C1 H1 0.9300 . ?
C1 C38 1.396(10) . ?
C2 C1A 1.389(10) . ?
C2 C25 1.377(9) . ?
C3 H3A 0.9600 . ?
C3 H3C 0.9600 . ?
C3 H3D 0.9600 . ?
C4 H4 0.9300 . ?
C4 C2I 1.389(10) . ?
C6 C4F 1.338(11) . ?
C6 C4H 1.473(11) . ?
C7 H7 0.9300 . ?
C7 C1R 1.374(9) . ?
C8 H8 0.9300 . ?
C8 C1Y 1.416(10) . ?
C8 C38 1.347(10) . ?
C11 H11 0.9300 . ?
C11 C1O 1.401(10) . ?
C12 H12 0.9300 . ?
C12 C36 1.358(11) . ?
C13 C1L 1.340(9) . ?
C13 C2R 1.427(11) . ?
C14 H14 0.9300 . ?
C14 C44 1.380(10) . ?
C15 H15 0.9300 . ?
C15 C2A 1.389(10) . ?
C15 C3A 1.392(11) . ?
C16 H16 0.9300 . ?
C16 C22 1.377(10) . ?
C17 H17 0.9300 . ?
C17 C3F 1.400(10) . ?
C18 H18 0.9300 . ?
C19 C2C 1.382(10) . ?
C19 C2Y 1.375(10) . ?
C1A H1A 0.9300 . ?
C1A C1I 1.366(10) . ?
C1B H1B 0.9300 . ?
C1B C1W 1.362(10) . ?
C1B C30 1.395(11) . ?
C1C H1C 0.9300 . ?
C1C C1P 1.388(11) . ?
C1C C2W 1.364(11) . ?
C1D H1D 0.9300 . ?
C1D C1V 1.366(9) . ?
C1E H1E 0.9300 . ?
C1E C2S 1.370(10) . ?
C1F C4B 1.470(12) . ?
C1F C4Q 1.392(11) . ?
C1G H1GA 0.9600 . ?
C1G H1GB 0.9600 . ?
C1G H1GC 0.9600 . ?
C1H C2G 1.384(10) . ?
C1H C2J 1.532(10) . ?
C1I H1I 0.9300 . ?
C1I C37 1.388(10) . ?
C1J H1JA 0.9600 . ?
C1J H1JB 0.9600 . ?
C1J H1JC 0.9600 . ?
C1K H1K 0.9300 . ?
C1K C2D 1.363(10) . ?
C1L H1L 0.9300 . ?
C1L C32 1.359(10) . ?
C1M H1M 0.9300 . ?
C1M C3C 1.367(11) . ?
C1N H1NA 0.9600 . ?
C1N H1NB 0.9600 . ?
C1N H1NC 0.9600 . ?
C1O H1O 0.9300 . ?
C1O C1V 1.348(10) . ?
C1P H1P 0.9300 . ?
C1Q C24 1.401(10) . ?
C1Q C2J 1.536(10) . ?
C1Q C42 1.376(11) . ?
C1R C3V 1.371(10) . ?
C1S H1S 0.9300 . ?
C1T N29 1.347(10) . ?
C1T C4Q 1.392(11) . ?
C1T C56 1.414(12) . ?
C1U H1UA 0.9600 . ?
C1U H1UB 0.9600 . ?
C1U H1UC 0.9600 . ?
C1V H1V 0.9300 . ?
C1W H1W 0.9300 . ?
C1X H1X 0.9300 . ?
C1X C3X 1.400(11) . ?
C1X C4J 1.286(12) . ?
C1Y H1Y 0.9300 . ?
C1Z H1Z 0.9300 . ?
C1Z C2D 1.377(10) . ?
C20 H20 0.9300 . ?
C20 C3P 1.399(11) . ?
C21 H21 0.9300 . ?
C21 C27 1.359(10) . ?
C22 H22 0.9300 . ?
C22 C2W 1.396(11) . ?
C23 H23 0.9300 . ?
C23 C3Q 1.364(11) . ?
C24 H24 0.9300 . ?
C24 C40 1.365(11) . ?
C25 H25 0.9300 . ?
C25 C3S 1.395(10) . ?
C26 H26 0.9300 . ?
C26 C3N 1.412(12) . ?
C27 H27 0.9300 . ?
C28 C39 1.387(11) . ?
C28 C4S 1.492(11) . ?
N29 H29 0.8600 . ?
C2B H2BA 0.9600 . ?
C2B H2BB 0.9600 . ?
C2B H2BC 0.9600 . ?
C2C H2C 0.9300 . ?
C2C C2U 1.393(10) . ?
C2D H2D 0.9300 . ?
C2E H2E 0.9300 . ?
C2E C2P 1.376(11) . ?
C2F H2F 0.9300 . ?
C2F C3C 1.413(11) . ?
C2G H2G 0.9300 . ?
C2G C3J 1.396(10) . ?
C2H H2H 0.9300 . ?
C2H C2K 1.391(11) . ?
C2H C3Y 1.384(11) . ?
C2I H2I 0.9300 . ?
C2I C36 1.370(11) . ?
C2K C35 1.385(11) . ?
C2L H2L 0.9300 . ?
C2L C3I 1.395(12) . ?
C2M H2MA 0.9600 . ?
C2M H2MB 0.9600 . ?
C2M H2MC 0.9600 . ?
C2M C5A 1.488(13) . ?
C2N H2N 0.9300 . ?
C2N C2Z 1.399(10) . ?
C2N C45 1.341(10) . ?
C2O H2O 0.9300 . ?
C2O C2S 1.407(11) . ?
C2O C44 1.374(10) . ?
C2P H2P 0.9300 . ?
C2P C41 1.389(12) . ?
C2Q H2Q 0.9300 . ?
C2Q C30 1.346(11) . ?
C2R H2R 0.9300 . ?
C2R C3H 1.397(11) . ?
C2S H2S 0.9300 . ?
C2T H2T 0.9300 . ?
C2T C3O 1.356(11) . ?
C2U H2U 0.9300 . ?
C2U C3M 1.377(12) . ?
C2V H2VA 0.9600 . ?
C2V H2VB 0.9600 . ?
C2V H2VC 0.9600 . ?
C2W H2W 0.9300 . ?
C2X H2XA 0.9600 . ?
C2X H2XB 0.9600 . ?
C2X H2XC 0.9600 . ?
C2X C49 1.441(14) . ?
C2Y H2Y 0.9300 . ?
C2Y C3W 1.408(10) . ?
C2Z H2Z 0.9300 . ?
C30 H30 0.9300 . ?
C31 C39 1.347(11) . ?
C31 C47 1.488(11) . ?
C32 H32 0.9300 . ?
C32 C4L 1.332(11) . ?
C34 H34 0.9300 . ?
C34 C4A 1.387(11) . ?
C35 H35 0.9300 . ?
C35 C4D 1.448(11) . ?
C36 H36 0.9300 . ?
C37 H37 0.9300 . ?
C37 C3S 1.378(11) . ?
C38 H38 0.9300 . ?
C39 H39 0.9300 . ?
C3A H3AA 0.9300 . ?
C3A C3N 1.368(12) . ?
C3B H3B 0.9300 . ?
C3B C3P 1.359(12) . ?
C3C H3CA 0.9300 . ?
C3E H3E 0.9300 . ?
C3E C45 1.390(11) . ?
C3F H3F 0.9300 . ?
C3F C4T 1.365(11) . ?
C3G H3G 0.9300 . ?
C3G C4R 1.406(14) . ?
C3G C59 1.402(15) . ?
C3H H3H 0.9300 . ?
C3H C4L 1.406(11) . ?
C3I H3I 0.9300 . ?
C3I C41 1.400(12) . ?
C3J H3J 0.9300 . ?
C3J C4A 1.349(11) . ?
C3K H3K 0.9300 . ?
C3K C3L 1.346(11) . ?
C3L H3L 0.9300 . ?
C3L C4T 1.359(12) . ?
C3M H3M 0.9300 . ?
C3M C3W 1.333(11) . ?
C3N H3N 0.9300 . ?
C3O H3O 0.9300 . ?
C3P H3P 0.9300 . ?
C3Q H3Q 0.9300 . ?
C3Q C3V 1.409(11) . ?
C3R H3R 0.9300 . ?
C3R C43 1.402(11) . ?
C3R C4J 1.384(12) . ?
C3S H3S 0.9300 . ?
C3T H3T 0.9300 . ?
C3T C4E 1.419(13) . ?
C3T C4H 1.427(12) . ?
C3U H3U 0.9300 . ?
C3U C4K 1.428(14) . ?
C3U C4X 1.337(15) . ?
C3V H3V 0.9300 . ?
C3W H3W 0.9300 . ?
C3X H3X 0.9300 . ?
C3Y H3Y 0.9300 . ?
C3Y C46 1.341(12) . ?
C3Z H3Z 0.9300 . ?
C3Z C4K 1.352(13) . ?
C3Z C5A 1.350(13) . ?
C40 H40 0.9300 . ?
C40 C4O 1.356(13) . ?
C41 H41 0.9300 . ?
C42 H42 0.9300 . ?
C42 C4Y 1.396(11) . ?
C43 H43 0.9300 . ?
C44 H44 0.9300 . ?
C45 H45 0.9300 . ?
C46 H46 0.9300 . ?
C46 C4D 1.322(12) . ?
C47 H47A 0.9600 . ?
C47 H47B 0.9600 . ?
C47 H47C 0.9600 . ?
C48 H48 0.9300 . ?
C48 C5D 1.392(15) . ?
C48 C5O 1.348(16) . ?
C49 C58 1.505(14) . ?
C49 C5F 1.371(15) . ?
C4A H4A 0.9300 . ?
C4B H4BA 0.9600 . ?
C4B H4BB 0.9600 . ?
C4B H4BC 0.9600 . ?
C4C H4C 0.9300 . ?
C4C C4E 1.324(12) . ?
C4C C4F 1.435(11) . ?
C4D H4D 0.9300 . ?
C4E H4E 0.9300 . ?
C4F H4F 0.9300 . ?
C4H H4H 0.9300 . ?
C4J H4J 0.9300 . ?
C4K H4K 0.9300 . ?
C4L H4L 0.9300 . ?
C4O H4O 0.9300 . ?
C4O C4Y 1.379(13) . ?
C4Q H4Q 0.9300 . ?
C4R H4R 0.9300 . ?
C4R C58 1.305(14) . ?
C4S H4SA 0.9600 . ?
C4S H4SB 0.9600 . ?
C4S H4SC 0.9600 . ?
C4T H4T 0.9300 . ?
C4W C5D 1.371(13) . ?
C4W C5E 1.356(13) . ?
C4W C5K 1.440(14) . ?
C4X H4X 0.9300 . ?
C4X C5C 1.353(14) . ?
C4Y H4Y 0.9300 . ?
C51 H51 0.9300 . ?
C51 C5K 1.327(13) . ?
C51 C5O 1.360(15) . ?
C56 H56A 0.9600 . ?
C56 H56B 0.9600 . ?
C56 H56C 0.9600 . ?
C58 H58A 0.9300 . ?
C59 H59 0.9300 . ?
C59 C5F 1.379(14) . ?
C5A C5C 1.391(13) . ?
C5C H5C 0.9300 . ?
C5D H5D 0.9300 . ?
C5E H5EA 0.9600 . ?
C5E H5EB 0.9600 . ?
C5E H5EC 0.9600 . ?
C5F H5F 0.9300 . ?
C5G H5GA 0.9600 . ?
C5G H5GB 0.9600 . ?
C5G H5GC 0.9600 . ?
C5G C50 1.497(14) . ?
C5H H5H 0.9300 . ?
C5H C5I 1.3900 . ?
C5H C50 1.3900 . ?
C5I H5I 0.9300 . ?
C5I C5B 1.3900 . ?
C5B H5B 0.9300 . ?
C5B C33 1.3900 . ?
C33 H33 0.9300 . ?
C33 C57 1.3900 . ?
C57 H57 0.9300 . ?
C57 C50 1.3900 . ?
C5K H5K 0.9300 . ?
C5O H5O 0.9300 . ?
C4M H4M 0.9300 . ?
C4M C4V 1.3900 . ?
C4M C10 1.3900 . ?
C4V H4V 0.9300 . ?
C4V C54 1.3900 . ?
C54 H54 0.9300 . ?
C54 C53 1.3900 . ?
C53 H53 0.9300 . ?
C53 C4U 1.3900 . ?
C4U H4U 0.9300 . ?
C4U C10 1.3900 . ?
C10 C4P 1.419(15) . ?
C4N H4N 0.9300 . ?
C4N C29 1.3900 . ?
C4N C4G 1.3900 . ?
C29 H29A 0.9300 . ?
C29 C4I 1.3900 . ?
C4I H4I 0.9300 . ?
C4I C4Z 1.3900 . ?
C4Z H4Z 0.9300 . ?
C4Z C3D 1.3900 . ?
C3D H3DA 0.9300 . ?
C3D C4G 1.3900 . ?
C4G C52 1.347(16) . ?
C4P H4PA 0.9600 . ?
C4P H4PB 0.9600 . ?
C4P H4PC 0.9600 . ?
C52 H52A 0.9600 . ?
C52 H52B 0.9600 . ?
C52 H52C 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
O11B V3B O10B 101.0(2) . . ?
O11B V3B O12B 101.4(2) . . ?
O11B V3B O13B 100.1(2) . . ?
O11B V3B O8B 99.2(2) . . ?
O12B V3B O10B 81.60(19) . . ?
O13B V3B O10B 157.6(2) . . ?
O13B V3B O12B 86.99(19) . . ?
O8B V3B O10B 88.4(2) . . ?
O8B V3B O12B 158.4(2) . . ?
O8B V3B O13B 95.6(2) . . ?
O1B V1B O20B 103.3(2) . . ?
O1B V1B O18B 101.1(2) . . ?
O1B V1B O3B 99.2(2) . . ?
O1B V1B O2B 101.0(2) . . ?
O18B V1B O20B 87.8(2) . . ?
O18B V1B O3B 158.9(2) . . ?
O3B V1B O20B 81.78(19) . . ?
O2B V1B O20B 154.7(2) . . ?
O2B V1B O18B 94.5(2) . . ?
O2B V1B O3B 87.48(19) . . ?
O16A V4A O15A 100.5(2) . . ?
O16A V4A O17A 101.0(2) . . ?
O16A V4A O13A 101.1(2) . . ?
O16A V4A O18A 100.9(2) . . ?
O17A V4A O15A 82.94(19) . . ?
O13A V4A O15A 87.4(2) . . ?
O13A V4A O17A 157.1(2) . . ?
O18A V4A O15A 157.6(2) . . ?
O18A V4A O17A 86.8(2) . . ?
O18A V4A O13A 94.7(2) . . ?
O5B V2B O7B 81.68(19) . . ?
O6B V2B O5B 102.8(2) . . ?
O6B V2B O7B 99.0(2) . . ?
O6B V2B O8B 100.5(2) . . ?
O6B V2B O2B 100.9(2) . . ?
O8B V2B O5B 155.3(2) . . ?
O8B V2B O7B 86.7(2) . . ?
O2B V2B O5B 88.59(19) . . ?
O2B V2B O7B 159.3(2) . . ?
O2B V2B O8B 95.0(2) . . ?
O7A V2A O5A 81.88(19) . . ?
O6A V2A O7A 99.5(2) . . ?
O6A V2A O5A 101.8(2) . . ?
O6A V2A O3A 99.5(2) . . ?
O6A V2A O8A 100.3(2) . . ?
O3A V2A O7A 160.0(2) . . ?
O3A V2A O5A 87.86(19) . . ?
O8A V2A O7A 88.4(2) . . ?
O8A V2A O5A 157.0(2) . . ?
O8A V2A O3A 94.7(2) . . ?
O1A V1A O2A 100.1(2) . . ?
O1A V1A O20A 101.4(2) . . ?
O1A V1A O3A 102.3(2) . . ?
O1A V1A O18A 100.9(2) . . ?
O2A V1A O20A 82.82(19) . . ?
O3A V1A O2A 88.6(2) . . ?
O3A V1A O20A 155.9(2) . . ?
O3A V1A O18A 94.1(2) . . ?
O18A V1A O2A 157.7(2) . . ?
O18A V1A O20A 85.8(2) . . ?
O15B V4B O17B 81.63(18) . . ?
O16B V4B O15B 103.2(2) . . ?
O16B V4B O17B 100.0(2) . . ?
O16B V4B O18B 102.3(2) . . ?
O16B V4B O13B 101.6(2) . . ?
O18B V4B O15B 153.0(2) . . ?
O18B V4B O17B 85.59(19) . . ?
O13B V4B O15B 88.7(2) . . ?
O13B V4B O17B 157.8(2) . . ?
O13B V4B O18B 94.5(2) . . ?
O11A V3A O10A 101.1(2) . . ?
O11A V3A O12A 102.1(2) . . ?
O11A V3A O13A 102.1(2) . . ?
O11A V3A O8A 98.8(2) . . ?
O12A V3A O10A 82.1(2) . . ?
O13A V3A O10A 156.4(2) . . ?
O13A V3A O12A 88.7(2) . . ?
O13A V3A O8A 93.9(2) . . ?
O8A V3A O10A 86.9(2) . . ?
O8A V3A O12A 157.9(2) . . ?
O14B P3B C65 106.4(3) . . ?
O15B P3B O14B 107.9(2) . . ?
O15B P3B O12B 115.1(3) . . ?
O15B P3B C65 108.1(3) . . ?
O12B P3B O14B 109.7(2) . . ?
O12B P3B C65 109.3(3) . . ?
O19B P4B C61 105.5(3) . . ?
O20B P4B O19B 108.3(3) . . ?
O20B P4B O17B 114.8(3) . . ?
O20B P4B C61 108.5(3) . . ?
O17B P4B O19B 109.1(2) . . ?
O17B P4B C61 110.3(3) . . ?
O5A P1A O2A 114.6(3) . . ?
O5A P1A O4A 107.6(3) . . ?
O5A P1A C77 110.3(3) . . ?
O2A P1A O4A 109.8(3) . . ?
O2A P1A C77 107.5(3) . . ?
O4A P1A C77 106.7(3) . . ?
O5B P1B O3B 114.6(3) . . ?
O5B P1B O4B 108.8(3) . . ?
O5B P1B C55 107.7(3) . . ?
O3B P1B O4B 108.9(3) . . ?
O3B P1B C55 110.4(3) . . ?
O4B P1B C55 106.1(3) . . ?
O19A P4A C64 105.5(3) . . ?
O17A P4A O19A 108.6(3) . . ?
O17A P4A C64 109.7(3) . . ?
O20A P4A O19A 108.7(3) . . ?
O20A P4A O17A 115.0(3) . . ?
O20A P4A C64 108.8(3) . . ?
O15A P3A O14A 108.8(3) . . ?
O15A P3A O12A 114.7(3) . . ?
O15A P3A C67 109.6(3) . . ?
O14A P3A C67 106.1(3) . . ?
O12A P3A O14A 108.5(3) . . ?
O12A P3A C67 108.9(3) . . ?
O10A P2A O9A 108.9(3) . . ?
O10A P2A C2J 109.2(3) . . ?
O7A P2A O10A 114.8(3) . . ?
O7A P2A O9A 109.1(3) . . ?
O7A P2A C2J 109.7(3) . . ?
O9A P2A C2J 104.7(3) . . ?
O9B P2B C66 105.5(3) . . ?
O10B P2B O9B 108.0(3) . . ?
O10B P2B O7B 115.3(3) . . ?
O10B P2B C66 110.1(3) . . ?
O7B P2B O9B 109.6(3) . . ?
O7B P2B C66 107.9(3) . . ?
C83 O19B P4B 121.6(4) . . ?
C1J O19A P4A 122.7(4) . . ?
P3A O15A V4A 134.9(3) . . ?
C1G O14B P3B 122.2(4) . . ?
C3 O14A P3A 123.8(4) . . ?
C2V O9B P2B 122.3(5) . . ?
P2B O10B V3B 132.6(3) . . ?
P4B O20B V1B 134.8(3) . . ?
P2A O10A V3A 135.4(3) . . ?
P3B O15B V4B 134.8(3) . . ?
P1B O5B V2B 135.6(3) . . ?
P2A O7A V2A 133.4(3) . . ?
P4A O17A V4A 135.3(3) . . ?
P1A O5A V2A 134.8(3) . . ?
P4B O17B V4B 135.9(3) . . ?
P1A O2A V1A 134.7(3) . . ?
P3B O12B V3B 134.4(3) . . ?
P3A O12A V3A 134.7(3) . . ?
V1B O18B V4B 137.1(3) . . ?
P1B O3B V1B 133.2(3) . . ?
P2B O7B V2B 135.7(3) . . ?
C2B O4B P1B 121.9(4) . . ?
P4A O20A V1A 136.0(3) . . ?
C1N O9A P2A 124.5(5) . . ?
V4B O13B V3B 137.5(3) . . ?
C1U O4A P1A 121.3(4) . . ?
V1A O3A V2A 135.8(3) . . ?
V3B O8B V2B 134.4(3) . . ?
C79 C55 P1B 104.6(4) . . ?
C6 C55 P1B 106.6(5) . . ?
C6 C55 C79 111.9(6) . . ?
C13 C55 P1B 110.8(5) . . ?
C13 C55 C79 111.2(6) . . ?
C13 C55 C6 111.5(6) . . ?
V3A O13A V4A 136.4(3) . . ?
V2A O8A V3A 136.2(3) . . ?
N88 N58 H58 125.1 . . ?
N88 N58 C28 109.7(6) . . ?
C28 N58 H58 125.1 . . ?
V1B O2B V2B 136.5(3) . . ?
C70 C60 C61 123.7(6) . . ?
C70 C60 C1W 116.3(7) . . ?
C1W C60 C61 119.9(6) . . ?
C60 C61 P4B 104.0(4) . . ?
C74 C61 P4B 110.1(4) . . ?
C74 C61 C60 110.7(5) . . ?
C93 C61 P4B 108.9(4) . . ?
C93 C61 C60 111.7(5) . . ?
C93 C61 C74 111.2(5) . . ?
C89 C62 C77 120.9(6) . . ?
C89 C62 C18 118.5(7) . . ?
C18 C62 C77 120.5(6) . . ?
C98 C63 C65 120.9(6) . . ?
C98 C63 C4 116.0(7) . . ?
C4 C63 C65 123.1(6) . . ?
C72 C64 P4A 104.4(4) . . ?
C2 C64 P4A 108.9(5) . . ?
C2 C64 C72 111.5(5) . . ?
C1R C64 P4A 109.1(4) . . ?
C1R C64 C72 111.9(6) . . ?
C1R C64 C2 110.7(6) . . ?
C63 C65 P3B 106.3(4) . . ?
C63 C65 C69 109.6(6) . . ?
C63 C65 C76 115.7(5) . . ?
C69 C65 P3B 111.2(4) . . ?
C76 C65 P3B 103.8(4) . . ?
C76 C65 C69 110.0(5) . . ?
C81 C66 P2B 111.2(5) . . ?
C85 C66 P2B 106.2(5) . . ?
C85 C66 C81 111.6(6) . . ?
C85 C66 C9 114.9(6) . . ?
C9 C66 P2B 105.9(5) . . ?
C9 C66 C81 106.8(6) . . ?
C82 C67 P3A 105.2(5) . . ?
C82 C67 C2K 112.9(6) . . ?
C5 C67 P3A 109.7(5) . . ?
C5 C67 C82 111.0(6) . . ?
C5 C67 C2K 108.5(6) . . ?
C2K C67 P3A 109.5(5) . . ?
V4A O18A V1A 137.1(3) . . ?
C90 C69 C65 118.1(6) . . ?
C90 C69 C1D 116.2(7) . . ?
C1D C69 C65 125.7(6) . . ?
C60 C70 H70 119.3 . . ?
C60 C70 C2Q 121.4(8) . . ?
C2Q C70 H70 119.3 . . ?
C2E C71 C2J 122.0(7) . . ?
C2L C71 C2E 117.8(8) . . ?
C2L C71 C2J 119.9(7) . . ?
C84 C72 C64 118.9(6) . . ?
C1 C72 C64 122.5(7) . . ?
C1 C72 C84 118.5(7) . . ?
C74 C73 H73 119.3 . . ?
C74 C73 C27 121.3(7) . . ?
C27 C73 H73 119.3 . . ?
C73 C74 C61 120.6(6) . . ?
C73 C74 C1S 117.6(7) . . ?
C1S C74 C61 121.7(6) . . ?
C1S C75 H75 119.0 . . ?
C21 C75 H75 119.0 . . ?
C21 C75 C1S 122.0(8) . . ?
C91 C76 C65 120.7(6) . . ?
C2Z C76 C65 121.9(6) . . ?
C2Z C76 C91 117.3(7) . . ?
C62 C77 P1A 106.0(5) . . ?
C62 C77 C19 111.6(6) . . ?
C19 C77 P1A 111.2(5) . . ?
C2A C77 P1A 106.8(5) . . ?
C2A C77 C62 113.2(6) . . ?
C2A C77 C19 108.0(6) . . ?
C93 C78 H78 119.7 . . ?
C93 C78 C1K 120.6(7) . . ?
C1K C78 H78 119.7 . . ?
C3X C79 C55 121.6(7) . . ?
C3X C79 C43 116.1(8) . . ?
C43 C79 C55 121.3(7) . . ?
C9 C80 H80 118.6 . . ?
C20 C80 H80 118.6 . . ?
C20 C80 C9 122.9(8) . . ?
C14 C81 C66 125.4(7) . . ?
C14 C81 C1E 118.2(7) . . ?
C1E C81 C66 116.5(7) . . ?
C17 C82 C67 118.7(6) . . ?
C17 C82 C3K 118.3(7) . . ?
C3K C82 C67 123.1(7) . . ?
O19B C83 H83A 109.5 . . ?
O19B C83 H83B 109.5 . . ?
O19B C83 H83C 109.5 . . ?
H83A C83 H83B 109.5 . . ?
H83A C83 H83C 109.5 . . ?
H83B C83 H83C 109.5 . . ?
C72 C84 H84 120.2 . . ?
C1Y C84 C72 119.6(7) . . ?
C1Y C84 H84 120.2 . . ?
C16 C85 C66 122.1(7) . . ?
C16 C85 C1P 116.3(7) . . ?
C1P C85 C66 121.5(7) . . ?
C26 C86 H86 119.1 . . ?
C26 C86 C2A 121.8(8) . . ?
C2A C86 H86 119.1 . . ?
C5 C87 H87 118.7 . . ?
C2F C87 H87 118.7 . . ?
C2F C87 C5 122.6(8) . . ?
N58 N88 H88 125.7 . . ?
N58 N88 C31 108.6(6) . . ?
C31 N88 H88 125.7 . . ?
C62 C89 H89 119.6 . . ?
C62 C89 C3O 120.8(7) . . ?
C3O C89 H89 119.6 . . ?
C69 C90 H90 118.6 . . ?
C11 C90 C69 122.8(7) . . ?
C11 C90 H90 118.6 . . ?
C76 C91 H91 119.8 . . ?
C3E C91 C76 120.5(7) . . ?
C3E C91 H91 119.8 . . ?
C93 C92 H92 119.6 . . ?
C93 C92 C1Z 120.7(7) . . ?
C1Z C92 H92 119.6 . . ?
C78 C93 C61 121.8(6) . . ?
C78 C93 C92 118.5(6) . . ?
C92 C93 C61 119.8(6) . . ?
C18 C94 H94 119.4 . . ?
C18 C94 C2T 121.2(7) . . ?
C2T C94 H94 119.4 . . ?
C9 C95 H95 120.6 . . ?
C3B C95 H95 120.6 . . ?
C3B C95 C9 118.9(8) . . ?
C7 C96 H96 120.0 . . ?
C23 C96 H96 120.0 . . ?
C23 C96 C7 119.9(7) . . ?
C5 C97 H97 119.0 . . ?
C1M C97 H97 119.0 . . ?
C1M C97 C5 121.9(7) . . ?
C63 C98 H98 118.7 . . ?
C63 C98 C12 122.7(7) . . ?
C12 C98 H98 118.7 . . ?
C1H C99 H99 119.2 . . ?
C34 C99 H99 119.2 . . ?
C34 C99 C1H 121.6(7) . . ?
C1F N10 H10 124.8 . . ?
C1F N10 N29 110.5(8) . . ?
N29 N10 H10 124.8 . . ?
C72 C1 H1 119.4 . . ?
C72 C1 C38 121.2(7) . . ?
C38 C1 H1 119.4 . . ?
C1A C2 C64 122.8(6) . . ?
C25 C2 C64 119.1(7) . . ?
C25 C2 C1A 117.9(7) . . ?
O14A C3 H3A 109.5 . . ?
O14A C3 H3C 109.5 . . ?
O14A C3 H3D 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3A C3 H3D 109.5 . . ?
H3C C3 H3D 109.5 . . ?
C63 C4 H4 119.7 . . ?
C2I C4 C63 120.7(8) . . ?
C2I C4 H4 119.7 . . ?
C87 C5 C67 119.5(6) . . ?
C97 C5 C67 123.7(7) . . ?
C97 C5 C87 116.7(7) . . ?
C4F C6 C55 126.6(7) . . ?
C4F C6 C4H 117.6(8) . . ?
C4H C6 C55 115.7(7) . . ?
C96 C7 H7 118.3 . . ?
C96 C7 C1R 123.4(7) . . ?
C1R C7 H7 118.3 . . ?
C1Y C8 H8 120.5 . . ?
C38 C8 H8 120.5 . . ?
C38 C8 C1Y 119.0(7) . . ?
C80 C9 C66 119.7(7) . . ?
C80 C9 C95 117.4(7) . . ?
C95 C9 C66 122.7(7) . . ?
C90 C11 H11 120.4 . . ?
C90 C11 C1O 119.2(7) . . ?
C1O C11 H11 120.4 . . ?
C98 C12 H12 120.1 . . ?
C36 C12 C98 119.8(8) . . ?
C36 C12 H12 120.1 . . ?
C1L C13 C55 127.6(7) . . ?
C1L C13 C2R 114.3(7) . . ?
C2R C13 C55 117.6(7) . . ?
C81 C14 H14 120.1 . . ?
C81 C14 C44 119.7(7) . . ?
C44 C14 H14 120.1 . . ?
C2A C15 H15 119.4 . . ?
C2A C15 C3A 121.2(8) . . ?
C3A C15 H15 119.4 . . ?
C85 C16 H16 119.0 . . ?
C22 C16 C85 122.1(8) . . ?
C22 C16 H16 119.0 . . ?
C82 C17 H17 119.8 . . ?
C82 C17 C3F 120.3(8) . . ?
C3F C17 H17 119.8 . . ?
C62 C18 C94 119.9(7) . . ?
C62 C18 H18 120.0 . . ?
C94 C18 H18 120.0 . . ?
C2C C19 C77 124.2(7) . . ?
C2Y C19 C77 117.3(7) . . ?
C2Y C19 C2C 118.3(7) . . ?
C2 C1A H1A 119.3 . . ?
C1I C1A C2 121.4(7) . . ?
C1I C1A H1A 119.3 . . ?
C1W C1B H1B 120.0 . . ?
C1W C1B C30 120.0(7) . . ?
C30 C1B H1B 120.0 . . ?
C1P C1C H1C 120.2 . . ?
C2W C1C H1C 120.2 . . ?
C2W C1C C1P 119.5(8) . . ?
C69 C1D H1D 119.3 . . ?
C1V C1D C69 121.3(7) . . ?
C1V C1D H1D 119.3 . . ?
C81 C1E H1E 119.0 . . ?
C2S C1E C81 122.1(8) . . ?
C2S C1E H1E 119.0 . . ?
N10 C1F C4B 122.2(9) . . ?
N10 C1F C4Q 106.9(8) . . ?
C4Q C1F C4B 130.9(9) . . ?
O14B C1G H1GA 109.5 . . ?
O14B C1G H1GB 109.5 . . ?
O14B C1G H1GC 109.5 . . ?
H1GA C1G H1GB 109.5 . . ?
H1GA C1G H1GC 109.5 . . ?
H1GB C1G H1GC 109.5 . . ?
C99 C1H C2J 121.9(7) . . ?
C2G C1H C99 116.1(7) . . ?
C2G C1H C2J 121.9(7) . . ?
C1A C1I H1I 119.7 . . ?
C1A C1I C37 120.6(8) . . ?
C37 C1I H1I 119.7 . . ?
O19A C1J H1JA 109.5 . . ?
O19A C1J H1JB 109.5 . . ?
O19A C1J H1JC 109.5 . . ?
H1JA C1J H1JB 109.5 . . ?
H1JA C1J H1JC 109.5 . . ?
H1JB C1J H1JC 109.5 . . ?
C78 C1K H1K 119.6 . . ?
C2D C1K C78 120.7(7) . . ?
C2D C1K H1K 119.6 . . ?
C13 C1L H1L 117.1 . . ?
C13 C1L C32 125.9(7) . . ?
C32 C1L H1L 117.1 . . ?
C97 C1M H1M 119.6 . . ?
C3C C1M C97 120.9(7) . . ?
C3C C1M H1M 119.6 . . ?
O9A C1N H1NA 109.5 . . ?
O9A C1N H1NB 109.5 . . ?
O9A C1N H1NC 109.5 . . ?
H1NA C1N H1NB 109.5 . . ?
H1NA C1N H1NC 109.5 . . ?
H1NB C1N H1NC 109.5 . . ?
C11 C1O H1O 120.9 . . ?
C1V C1O C11 118.2(7) . . ?
C1V C1O H1O 120.9 . . ?
C85 C1P H1P 118.9 . . ?
C1C C1P C85 122.2(8) . . ?
C1C C1P H1P 118.9 . . ?
C24 C1Q C2J 120.6(7) . . ?
C42 C1Q C24 116.1(8) . . ?
C42 C1Q C2J 123.1(7) . . ?
C7 C1R C64 123.0(6) . . ?
C3V C1R C64 120.6(7) . . ?
C3V C1R C7 116.2(7) . . ?
C74 C1S C75 120.0(7) . . ?
C74 C1S H1S 120.0 . . ?
C75 C1S H1S 120.0 . . ?
N29 C1T C4Q 105.0(8) . . ?
N29 C1T C56 122.8(9) . . ?
C4Q C1T C56 132.2(9) . . ?
O4A C1U H1UA 109.5 . . ?
O4A C1U H1UB 109.5 . . ?
O4A C1U H1UC 109.5 . . ?
H1UA C1U H1UB 109.5 . . ?
H1UA C1U H1UC 109.5 . . ?
H1UB C1U H1UC 109.5 . . ?
C1D C1V H1V 118.9 . . ?
C1O C1V C1D 122.2(7) . . ?
C1O C1V H1V 118.9 . . ?
C60 C1W H1W 118.9 . . ?
C1B C1W C60 122.2(7) . . ?
C1B C1W H1W 118.9 . . ?
C3X C1X H1X 119.5 . . ?
C4J C1X H1X 119.5 . . ?
C4J C1X C3X 121.0(10) . . ?
C84 C1Y C8 120.7(7) . . ?
C84 C1Y H1Y 119.7 . . ?
C8 C1Y H1Y 119.7 . . ?
C92 C1Z H1Z 120.2 . . ?
C2D C1Z C92 119.7(7) . . ?
C2D C1Z H1Z 120.2 . . ?
C80 C20 H20 120.4 . . ?
C80 C20 C3P 119.1(8) . . ?
C3P C20 H20 120.4 . . ?
C75 C21 H21 120.3 . . ?
C75 C21 C27 119.3(7) . . ?
C27 C21 H21 120.3 . . ?
C16 C22 H22 120.0 . . ?
C16 C22 C2W 120.0(8) . . ?
C2W C22 H22 120.0 . . ?
C96 C23 H23 120.2 . . ?
C96 C23 C3Q 119.7(8) . . ?
C3Q C23 H23 120.2 . . ?
C1Q C24 H24 119.0 . . ?
C40 C24 C1Q 122.0(8) . . ?
C40 C24 H24 119.0 . . ?
C2 C25 H25 119.5 . . ?
C2 C25 C3S 121.0(8) . . ?
C3S C25 H25 119.5 . . ?
C86 C26 H26 120.5 . . ?
C86 C26 C3N 119.1(8) . . ?
C3N C26 H26 120.5 . . ?
C73 C27 H27 120.1 . . ?
C21 C27 C73 119.7(7) . . ?
C21 C27 H27 120.1 . . ?
N58 C28 C39 105.6(7) . . ?
N58 C28 C4S 121.2(7) . . ?
C39 C28 C4S 133.1(8) . . ?
N10 N29 C1T 110.0(7) . . ?
N10 N29 H29 125.0 . . ?
C1T N29 H29 125.0 . . ?
C86 C2A C77 118.7(7) . . ?
C15 C2A C77 123.6(7) . . ?
C15 C2A C86 117.6(7) . . ?
O4B C2B H2BA 109.5 . . ?
O4B C2B H2BB 109.5 . . ?
O4B C2B H2BC 109.5 . . ?
H2BA C2B H2BB 109.5 . . ?
H2BA C2B H2BC 109.5 . . ?
H2BB C2B H2BC 109.5 . . ?
C19 C2C H2C 120.1 . . ?
C19 C2C C2U 119.9(8) . . ?
C2U C2C H2C 120.1 . . ?
C1K C2D C1Z 119.7(7) . . ?
C1K C2D H2D 120.1 . . ?
C1Z C2D H2D 120.1 . . ?
C71 C2E H2E 118.9 . . ?
C2P C2E C71 122.1(8) . . ?
C2P C2E H2E 118.9 . . ?
C87 C2F H2F 120.5 . . ?
C87 C2F C3C 118.9(8) . . ?
C3C C2F H2F 120.5 . . ?
C1H C2G H2G 118.8 . . ?
C1H C2G C3J 122.3(8) . . ?
C3J C2G H2G 118.8 . . ?
C2K C2H H2H 119.5 . . ?
C3Y C2H H2H 119.5 . . ?
C3Y C2H C2K 120.9(9) . . ?
C4 C2I H2I 119.5 . . ?
C36 C2I C4 121.0(8) . . ?
C36 C2I H2I 119.5 . . ?
C71 C2J P2A 105.6(5) . . ?
C1H C2J P2A 108.7(5) . . ?
C1H C2J C71 109.9(6) . . ?
C1H C2J C1Q 112.9(6) . . ?
C1Q C2J P2A 109.2(5) . . ?
C1Q C2J C71 110.2(6) . . ?
C2H C2K C67 119.1(7) . . ?
C35 C2K C67 121.1(8) . . ?
C35 C2K C2H 119.1(8) . . ?
C71 C2L H2L 119.7 . . ?
C71 C2L C3I 120.6(9) . . ?
C3I C2L H2L 119.7 . . ?
H2MA C2M H2MB 109.5 . . ?
H2MA C2M H2MC 109.5 . . ?
H2MB C2M H2MC 109.5 . . ?
C5A C2M H2MA 109.5 . . ?
C5A C2M H2MB 109.5 . . ?
C5A C2M H2MC 109.5 . . ?
C2Z C2N H2N 119.6 . . ?
C45 C2N H2N 119.6 . . ?
C45 C2N C2Z 120.9(8) . . ?
C2S C2O H2O 121.1 . . ?
C44 C2O H2O 121.1 . . ?
C44 C2O C2S 117.9(8) . . ?
C2E C2P H2P 120.0 . . ?
C2E C2P C41 120.0(9) . . ?
C41 C2P H2P 120.0 . . ?
C70 C2Q H2Q 119.5 . . ?
C30 C2Q C70 121.1(8) . . ?
C30 C2Q H2Q 119.5 . . ?
C13 C2R H2R 119.2 . . ?
C3H C2R C13 121.6(8) . . ?
C3H C2R H2R 119.2 . . ?
C1E C2S C2O 119.5(8) . . ?
C1E C2S H2S 120.3 . . ?
C2O C2S H2S 120.3 . . ?
C94 C2T H2T 121.0 . . ?
C3O C2T C94 117.9(8) . . ?
C3O C2T H2T 121.0 . . ?
C2C C2U H2U 119.4 . . ?
C3M C2U C2C 121.2(8) . . ?
C3M C2U H2U 119.4 . . ?
O9B C2V H2VA 109.5 . . ?
O9B C2V H2VB 109.5 . . ?
O9B C2V H2VC 109.5 . . ?
H2VA C2V H2VB 109.5 . . ?
H2VA C2V H2VC 109.5 . . ?
H2VB C2V H2VC 109.5 . . ?
C1C C2W C22 119.7(8) . . ?
C1C C2W H2W 120.1 . . ?
C22 C2W H2W 120.1 . . ?
H2XA C2X H2XB 109.5 . . ?
H2XA C2X H2XC 109.5 . . ?
H2XB C2X H2XC 109.5 . . ?
C49 C2X H2XA 109.5 . . ?
C49 C2X H2XB 109.5 . . ?
C49 C2X H2XC 109.5 . . ?
C19 C2Y H2Y 119.7 . . ?
C19 C2Y C3W 120.5(8) . . ?
C3W C2Y H2Y 119.7 . . ?
C76 C2Z C2N 121.4(7) . . ?
C76 C2Z H2Z 119.3 . . ?
C2N C2Z H2Z 119.3 . . ?
C1B C30 H30 120.6 . . ?
C2Q C30 C1B 118.8(8) . . ?
C2Q C30 H30 120.6 . . ?
N88 C31 C39 108.4(7) . . ?
N88 C31 C47 119.8(7) . . ?
C39 C31 C47 131.7(8) . . ?
C1L C32 H32 120.4 . . ?
C4L C32 C1L 119.1(8) . . ?
C4L C32 H32 120.4 . . ?
C99 C34 H34 120.1 . . ?
C4A C34 C99 119.7(8) . . ?
C4A C34 H34 120.1 . . ?
C2K C35 H35 121.1 . . ?
C2K C35 C4D 117.7(9) . . ?
C4D C35 H35 121.1 . . ?
C12 C36 C2I 119.8(7) . . ?
C12 C36 H36 120.1 . . ?
C2I C36 H36 120.1 . . ?
C1I C37 H37 120.6 . . ?
C3S C37 C1I 118.7(7) . . ?
C3S C37 H37 120.6 . . ?
C1 C38 H38 119.5 . . ?
C8 C38 C1 120.9(7) . . ?
C8 C38 H38 119.5 . . ?
C28 C39 H39 126.2 . . ?
C31 C39 C28 107.5(8) . . ?
C31 C39 H39 126.2 . . ?
C15 C3A H3AA 119.7 . . ?
C3N C3A C15 120.5(9) . . ?
C3N C3A H3AA 119.7 . . ?
C95 C3B H3B 119.1 . . ?
C3P C3B C95 121.8(9) . . ?
C3P C3B H3B 119.1 . . ?
C1M C3C C2F 118.8(7) . . ?
C1M C3C H3CA 120.6 . . ?
C2F C3C H3CA 120.6 . . ?
C91 C3E H3E 119.2 . . ?
C91 C3E C45 121.7(8) . . ?
C45 C3E H3E 119.2 . . ?
C17 C3F H3F 120.5 . . ?
C4T C3F C17 119.0(8) . . ?
C4T C3F H3F 120.5 . . ?
C4R C3G H3G 119.2 . . ?
C59 C3G H3G 119.2 . . ?
C59 C3G C4R 121.6(12) . . ?
C2R C3H H3H 121.1 . . ?
C2R C3H C4L 117.8(8) . . ?
C4L C3H H3H 121.1 . . ?
C2L C3I H3I 119.7 . . ?
C2L C3I C41 120.6(9) . . ?
C41 C3I H3I 119.7 . . ?
C2G C3J H3J 119.8 . . ?
C4A C3J C2G 120.3(8) . . ?
C4A C3J H3J 119.8 . . ?
C82 C3K H3K 119.7 . . ?
C3L C3K C82 120.6(8) . . ?
C3L C3K H3K 119.7 . . ?
C3K C3L H3L 119.5 . . ?
C3K C3L C4T 121.0(9) . . ?
C4T C3L H3L 119.5 . . ?
C2U C3M H3M 120.5 . . ?
C3W C3M C2U 119.0(8) . . ?
C3W C3M H3M 120.5 . . ?
C26 C3N H3N 120.1 . . ?
C3A C3N C26 119.7(8) . . ?
C3A C3N H3N 120.1 . . ?
C89 C3O H3O 119.2 . . ?
C2T C3O C89 121.6(8) . . ?
C2T C3O H3O 119.2 . . ?
C20 C3P H3P 120.1 . . ?
C3B C3P C20 119.9(9) . . ?
C3B C3P H3P 120.1 . . ?
C23 C3Q H3Q 120.0 . . ?
C23 C3Q C3V 120.0(9) . . ?
C3V C3Q H3Q 120.0 . . ?
C43 C3R H3R 121.3 . . ?
C4J C3R H3R 121.3 . . ?
C4J C3R C43 117.3(9) . . ?
C25 C3S H3S 119.9 . . ?
C37 C3S C25 120.2(8) . . ?
C37 C3S H3S 119.9 . . ?
C4E C3T H3T 119.7 . . ?
C4E C3T C4H 120.7(9) . . ?
C4H C3T H3T 119.7 . . ?
C4K C3U H3U 120.6 . . ?
C4X C3U H3U 120.6 . . ?
C4X C3U C4K 118.8(13) . . ?
C1R C3V C3Q 120.8(9) . . ?
C1R C3V H3V 119.6 . . ?
C3Q C3V H3V 119.6 . . ?
C2Y C3W H3W 119.5 . . ?
C3M C3W C2Y 121.1(8) . . ?
C3M C3W H3W 119.5 . . ?
C79 C3X C1X 122.4(9) . . ?
C79 C3X H3X 118.8 . . ?
C1X C3X H3X 118.8 . . ?
C2H C3Y H3Y 120.6 . . ?
C46 C3Y C2H 118.8(9) . . ?
C46 C3Y H3Y 120.6 . . ?
C4K C3Z H3Z 118.7 . . ?
C5A C3Z H3Z 118.7 . . ?
C5A C3Z C4K 122.6(11) . . ?
C24 C40 H40 119.7 . . ?
C4O C40 C24 120.7(9) . . ?
C4O C40 H40 119.7 . . ?
C2P C41 C3I 118.9(8) . . ?
C2P C41 H41 120.6 . . ?
C3I C41 H41 120.6 . . ?
C1Q C42 H42 119.0 . . ?
C1Q C42 C4Y 122.1(9) . . ?
C4Y C42 H42 119.0 . . ?
C79 C43 C3R 121.9(9) . . ?
C79 C43 H43 119.0 . . ?
C3R C43 H43 119.0 . . ?
C14 C44 H44 118.7 . . ?
C2O C44 C14 122.6(8) . . ?
C2O C44 H44 118.7 . . ?
C2N C45 C3E 118.3(8) . . ?
C2N C45 H45 120.9 . . ?
C3E C45 H45 120.9 . . ?
C3Y C46 H46 118.2 . . ?
C4D C46 C3Y 123.5(10) . . ?
C4D C46 H46 118.2 . . ?
C31 C47 H47A 109.5 . . ?
C31 C47 H47B 109.5 . . ?
C31 C47 H47C 109.5 . . ?
H47A C47 H47B 109.5 . . ?
H47A C47 H47C 109.5 . . ?
H47B C47 H47C 109.5 . . ?
C5D C48 H48 121.4 . . ?
C5O C48 H48 121.4 . . ?
C5O C48 C5D 117.3(14) . . ?
C2X C49 C58 117.3(11) . . ?
C5F C49 C2X 125.0(12) . . ?
C5F C49 C58 117.6(11) . . ?
C34 C4A H4A 120.1 . . ?
C3J C4A C34 119.9(8) . . ?
C3J C4A H4A 120.1 . . ?
C1F C4B H4BA 109.5 . . ?
C1F C4B H4BB 109.5 . . ?
C1F C4B H4BC 109.5 . . ?
H4BA C4B H4BB 109.5 . . ?
H4BA C4B H4BC 109.5 . . ?
H4BB C4B H4BC 109.5 . . ?
C4E C4C H4C 121.1 . . ?
C4E C4C C4F 117.8(9) . . ?
C4F C4C H4C 121.1 . . ?
C35 C4D H4D 120.3 . . ?
C46 C4D C35 119.4(9) . . ?
C46 C4D H4D 120.3 . . ?
C3T C4E H4E 119.1 . . ?
C4C C4E C3T 121.9(10) . . ?
C4C C4E H4E 119.1 . . ?
C6 C4F C4C 125.0(9) . . ?
C6 C4F H4F 117.5 . . ?
C4C C4F H4F 117.5 . . ?
C6 C4H H4H 121.5 . . ?
C3T C4H C6 116.9(8) . . ?
C3T C4H H4H 121.5 . . ?
C1X C4J C3R 121.0(10) . . ?
C1X C4J H4J 119.5 . . ?
C3R C4J H4J 119.5 . . ?
C3U C4K H4K 120.5 . . ?
C3Z C4K C3U 118.9(12) . . ?
C3Z C4K H4K 120.5 . . ?
C32 C4L C3H 120.7(8) . . ?
C32 C4L H4L 119.7 . . ?
C3H C4L H4L 119.7 . . ?
C40 C4O H4O 120.1 . . ?
C40 C4O C4Y 119.8(9) . . ?
C4Y C4O H4O 120.1 . . ?
C1F C4Q C1T 107.6(8) . . ?
C1F C4Q H4Q 126.2 . . ?
C1T C4Q H4Q 126.2 . . ?
C3G C4R H4R 118.6 . . ?
C58 C4R C3G 122.8(12) . . ?
C58 C4R H4R 118.6 . . ?
C28 C4S H4SA 109.5 . . ?
C28 C4S H4SB 109.5 . . ?
C28 C4S H4SC 109.5 . . ?
H4SA C4S H4SB 109.5 . . ?
H4SA C4S H4SC 109.5 . . ?
H4SB C4S H4SC 109.5 . . ?
C3F C4T H4T 119.7 . . ?
C3L C4T C3F 120.7(9) . . ?
C3L C4T H4T 119.7 . . ?
C5D C4W C5K 112.9(11) . . ?
C5E C4W C5D 124.1(11) . . ?
C5E C4W C5K 123.0(11) . . ?
C3U C4X H4X 119.9 . . ?
C3U C4X C5C 120.2(13) . . ?
C5C C4X H4X 119.9 . . ?
C42 C4Y H4Y 120.4 . . ?
C4O C4Y C42 119.2(9) . . ?
C4O C4Y H4Y 120.4 . . ?
C5K C51 H51 116.0 . . ?
C5K C51 C5O 128.0(12) . . ?
C5O C51 H51 116.0 . . ?
C1T C56 H56A 109.5 . . ?
C1T C56 H56B 109.5 . . ?
C1T C56 H56C 109.5 . . ?
H56A C56 H56B 109.5 . . ?
H56A C56 H56C 109.5 . . ?
H56B C56 H56C 109.5 . . ?
C49 C58 H58A 121.2 . . ?
C4R C58 C49 117.7(12) . . ?
C4R C58 H58A 121.2 . . ?
C3G C59 H59 121.9 . . ?
C5F C59 C3G 116.2(13) . . ?
C5F C59 H59 121.9 . . ?
C3Z C5A C2M 123.1(10) . . ?
C3Z C5A C5C 116.8(10) . . ?
C5C C5A C2M 119.9(11) . . ?
C4X C5C C5A 122.3(12) . . ?
C4X C5C H5C 118.9 . . ?
C5A C5C H5C 118.9 . . ?
C48 C5D H5D 116.3 . . ?
C4W C5D C48 127.4(12) . . ?
C4W C5D H5D 116.3 . . ?
C4W C5E H5EA 109.5 . . ?
C4W C5E H5EB 109.5 . . ?
C4W C5E H5EC 109.5 . . ?
H5EA C5E H5EB 109.5 . . ?
H5EA C5E H5EC 109.5 . . ?
H5EB C5E H5EC 109.5 . . ?
C49 C5F C59 124.1(13) . . ?
C49 C5F H5F 118.0 . . ?
C59 C5F H5F 118.0 . . ?
H5GA C5G H5GB 109.5 . . ?
H5GA C5G H5GC 109.5 . . ?
H5GB C5G H5GC 109.5 . . ?
C50 C5G H5GA 109.5 . . ?
C50 C5G H5GB 109.5 . . ?
C50 C5G H5GC 109.5 . . ?
C5I C5H H5H 120.0 . . ?
C5I C5H C50 120.0 . . ?
C50 C5H H5H 120.0 . . ?
C5H C5I H5I 120.0 . . ?
C5H C5I C5B 120.0 . . ?
C5B C5I H5I 120.0 . . ?
C5I C5B H5B 120.0 . . ?
C33 C5B C5I 120.0 . . ?
C33 C5B H5B 120.0 . . ?
C5B C33 H33 120.0 . . ?
C5B C33 C57 120.0 . . ?
C57 C33 H33 120.0 . . ?
C33 C57 H57 120.0 . . ?
C50 C57 C33 120.0 . . ?
C50 C57 H57 120.0 . . ?
C5H C50 C5G 125.7(8) . . ?
C57 C50 C5G 114.2(8) . . ?
C57 C50 C5H 120.0 . . ?
C4W C5K H5K 121.1 . . ?
C51 C5K C4W 117.8(11) . . ?
C51 C5K H5K 121.1 . . ?
C48 C5O C51 116.5(14) . . ?
C48 C5O H5O 121.7 . . ?
C51 C5O H5O 121.7 . . ?
C4V C4M H4M 120.0 . . ?
C4V C4M C10 120.0 . . ?
C10 C4M H4M 120.0 . . ?
C4M C4V H4V 120.0 . . ?
C54 C4V C4M 120.0 . . ?
C54 C4V H4V 120.0 . . ?
C4V C54 H54 120.0 . . ?
C53 C54 C4V 120.0 . . ?
C53 C54 H54 120.0 . . ?
C54 C53 H53 120.0 . . ?
C4U C53 C54 120.0 . . ?
C4U C53 H53 120.0 . . ?
C53 C4U H4U 120.0 . . ?
C53 C4U C10 120.0 . . ?
C10 C4U H4U 120.0 . . ?
C4M C10 C4P 117.7(10) . . ?
C4U C10 C4M 120.0 . . ?
C4U C10 C4P 122.1(10) . . ?
C29 C4N H4N 120.0 . . ?
C29 C4N C4G 120.0 . . ?
C4G C4N H4N 120.0 . . ?
C4N C29 H29A 120.0 . . ?
C4N C29 C4I 120.0 . . ?
C4I C29 H29A 120.0 . . ?
C29 C4I H4I 120.0 . . ?
C4Z C4I C29 120.0 . . ?
C4Z C4I H4I 120.0 . . ?
C4I C4Z H4Z 120.0 . . ?
C4I C4Z C3D 120.0 . . ?
C3D C4Z H4Z 120.0 . . ?
C4Z C3D H3DA 120.0 . . ?
C4G C3D C4Z 120.0 . . ?
C4G C3D H3DA 120.0 . . ?
C3D C4G C4N 120.0 . . ?
C52 C4G C4N 120.4(11) . . ?
C52 C4G C3D 119.1(11) . . ?
C10 C4P H4PA 109.5 . . ?
C10 C4P H4PB 109.5 . . ?
C10 C4P H4PC 109.5 . . ?
H4PA C4P H4PB 109.5 . . ?
H4PA C4P H4PC 109.5 . . ?
H4PB C4P H4PC 109.5 . . ?
C4G C52 H52A 109.5 . . ?
C4G C52 H52B 109.5 . . ?
C4G C52 H52C 109.5 . . ?
H52A C52 H52B 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
P3B C65 C69 C90 165.6(5) . . . . ?
P3B C65 C69 C1D -15.4(9) . . . . ?
P3B C65 C76 C91 115.2(6) . . . . ?
P3B C65 C76 C2Z -59.9(7) . . . . ?
P4B C61 C74 C73 -144.5(6) . . . . ?
P4B C61 C74 C1S 38.5(8) . . . . ?
P4B C61 C93 C78 49.2(7) . . . . ?
P4B C61 C93 C92 -132.1(5) . . . . ?
P1A C77 C19 C2C -24.2(9) . . . . ?
P1A C77 C19 C2Y 159.8(6) . . . . ?
P1A C77 C2A C86 -62.9(7) . . . . ?
P1A C77 C2A C15 120.7(7) . . . . ?
P1B C55 C79 C3X -62.0(9) . . . . ?
P1B C55 C79 C43 106.8(7) . . . . ?
P1B C55 C6 C4F -49.1(10) . . . . ?
P1B C55 C6 C4H 128.1(6) . . . . ?
P1B C55 C13 C1L -27.1(11) . . . . ?
P1B C55 C13 C2R 144.4(6) . . . . ?
P4A C64 C72 C84 -60.5(7) . . . . ?
P4A C64 C72 C1 117.3(6) . . . . ?
P4A C64 C2 C1A -44.1(8) . . . . ?
P4A C64 C2 C25 139.2(6) . . . . ?
P4A C64 C1R C7 135.3(6) . . . . ?
P4A C64 C1R C3V -49.7(9) . . . . ?
P3A C67 C82 C17 -65.4(7) . . . . ?
P3A C67 C82 C3K 114.6(6) . . . . ?
P3A C67 C5 C87 148.7(6) . . . . ?
P3A C67 C5 C97 -36.1(8) . . . . ?
P3A C67 C2K C2H 146.6(6) . . . . ?
P3A C67 C2K C35 -43.2(9) . . . . ?
P2B C66 C81 C14 15.4(10) . . . . ?
P2B C66 C81 C1E -164.4(6) . . . . ?
P2B C66 C85 C16 -115.7(6) . . . . ?
P2B C66 C85 C1P 63.2(8) . . . . ?
P2B C66 C9 C80 68.9(7) . . . . ?
P2B C66 C9 C95 -116.4(6) . . . . ?
O19B P4B O20B V1B -126.1(4) . . . . ?
O19B P4B O17B V4B 118.3(4) . . . . ?
O19B P4B C61 C60 166.8(4) . . . . ?
O19B P4B C61 C74 -74.6(5) . . . . ?
O19B P4B C61 C93 47.6(5) . . . . ?
O1B V1B O18B V4B 163.7(4) . . . . ?
O1B V1B O2B V2B -161.3(4) . . . . ?
O11B V3B O13B V4B -162.7(4) . . . . ?
O11B V3B O8B V2B 164.7(4) . . . . ?
O1A V1A O3A V2A 162.5(4) . . . . ?
O1A V1A O18A V4A -162.8(4) . . . . ?
O19A P4A O17A V4A -123.1(4) . . . . ?
O19A P4A O20A V1A 124.7(4) . . . . ?
O19A P4A C64 C72 -167.9(4) . . . . ?
O19A P4A C64 C2 -48.6(5) . . . . ?
O19A P4A C64 C1R 72.4(5) . . . . ?
O15A V4A O13A V3A -60.4(4) . . . . ?
O15A V4A O18A V1A 0.5(8) . . . . ?
O15A P3A O14A C3 -116.6(5) . . . . ?
O15A P3A O12A V3A 3.0(5) . . . . ?
O15A P3A C67 C82 76.6(5) . . . . ?
O15A P3A C67 C5 -42.8(6) . . . . ?
O15A P3A C67 C2K -161.8(5) . . . . ?
O14B P3B O15B V4B -119.5(4) . . . . ?
O14B P3B O12B V3B 111.8(4) . . . . ?
O14B P3B C65 C63 66.7(5) . . . . ?
O14B P3B C65 C69 -52.5(5) . . . . ?
O14B P3B C65 C76 -170.8(4) . . . . ?
O14A P3A O15A V4A 120.2(4) . . . . ?
O14A P3A O12A V3A -118.8(4) . . . . ?
O14A P3A C67 C82 -166.1(4) . . . . ?
O14A P3A C67 C5 74.4(5) . . . . ?
O14A P3A C67 C2K -44.5(5) . . . . ?
O9B P2B O10B V3B -117.5(4) . . . . ?
O9B P2B O7B V2B 114.0(4) . . . . ?
O9B P2B C66 C81 -62.8(6) . . . . ?
O9B P2B C66 C85 58.8(5) . . . . ?
O9B P2B C66 C9 -178.5(4) . . . . ?
O10B V3B O13B V4B -2.5(8) . . . . ?
O10B V3B O8B V2B 63.9(4) . . . . ?
O10B P2B O9B C2V 127.4(5) . . . . ?
O10B P2B O7B V2B -8.1(5) . . . . ?
O10B P2B C66 C81 53.5(6) . . . . ?
O10B P2B C66 C85 175.2(5) . . . . ?
O10B P2B C66 C9 -62.2(5) . . . . ?
O20B V1B O18B V4B 60.7(4) . . . . ?
O20B V1B O2B V2B 2.2(7) . . . . ?
O20B P4B O19B C83 119.0(5) . . . . ?
O20B P4B O17B V4B -3.4(5) . . . . ?
O20B P4B C61 C60 -77.3(5) . . . . ?
O20B P4B C61 C74 41.3(5) . . . . ?
O20B P4B C61 C93 163.5(4) . . . . ?
O10A V3A O13A V4A -5.2(8) . . . . ?
O10A V3A O8A V2A -60.3(4) . . . . ?
O10A P2A O7A V2A 14.0(5) . . . . ?
O10A P2A O9A C1N -126.3(5) . . . . ?
O10A P2A C2J C71 74.0(5) . . . . ?
O10A P2A C2J C1H -168.0(5) . . . . ?
O10A P2A C2J C1Q -44.5(6) . . . . ?
O16A V4A O13A V3A -160.6(4) . . . . ?
O16A V4A O18A V1A 163.7(4) . . . . ?
O15B V4B O18B V1B -2.4(7) . . . . ?
O15B V4B O13B V3B 58.4(4) . . . . ?
O15B P3B O14B C1G 126.3(5) . . . . ?
O15B P3B O12B V3B -10.1(5) . . . . ?
O15B P3B C65 C63 -177.6(4) . . . . ?
O15B P3B C65 C69 63.2(5) . . . . ?
O15B P3B C65 C76 -55.1(5) . . . . ?
O16B V4B O18B V1B -163.4(4) . . . . ?
O16B V4B O13B V3B 161.7(4) . . . . ?
O5B V2B O8B V3B -2.9(7) . . . . ?
O5B V2B O2B V1B 57.6(4) . . . . ?
O5B P1B O3B V1B -16.7(5) . . . . ?
O5B P1B O4B C2B 127.9(5) . . . . ?
O5B P1B C55 C79 -173.8(4) . . . . ?
O5B P1B C55 C6 -55.1(5) . . . . ?
O5B P1B C55 C13 66.4(6) . . . . ?
O7A V2A O3A V1A -0.3(9) . . . . ?
O7A V2A O8A V3A 63.3(4) . . . . ?
O7A P2A O10A V3A -9.8(5) . . . . ?
O7A P2A O9A C1N -0.3(6) . . . . ?
O7A P2A C2J C71 -52.5(5) . . . . ?
O7A P2A C2J C1H 65.4(6) . . . . ?
O7A P2A C2J C1Q -171.1(5) . . . . ?
O17A V4A O13A V3A 4.5(8) . . . . ?
O17A V4A O18A V1A 63.1(4) . . . . ?
O17A P4A O19A C1J 7.4(6) . . . . ?
O17A P4A O20A V1A 2.8(5) . . . . ?
O17A P4A C64 C72 -51.1(5) . . . . ?
O17A P4A C64 C2 68.2(5) . . . . ?
O17A P4A C64 C1R -170.8(5) . . . . ?
O5A V2A O3A V1A -59.4(4) . . . . ?
O5A V2A O8A V3A -1.3(8) . . . . ?
O5A P1A O2A V1A 6.6(5) . . . . ?
O5A P1A O4A C1U -140.4(5) . . . . ?
O5A P1A C77 C62 -171.3(4) . . . . ?
O5A P1A C77 C19 -49.8(6) . . . . ?
O5A P1A C77 C2A 67.7(5) . . . . ?
O11A V3A O13A V4A 163.8(4) . . . . ?
O11A V3A O8A V2A -161.1(4) . . . . ?
O17B V4B O18B V1B -64.1(4) . . . . ?
O17B V4B O13B V3B -5.5(8) . . . . ?
O17B P4B O19B C83 -6.6(5) . . . . ?
O17B P4B O20B V1B -4.0(5) . . . . ?
O17B P4B C61 C60 49.1(5) . . . . ?
O17B P4B C61 C74 167.8(4) . . . . ?
O17B P4B C61 C93 -70.0(5) . . . . ?
O2A V1A O3A V2A 62.4(4) . . . . ?
O2A V1A O18A V4A -2.6(8) . . . . ?
O2A P1A O5A V2A -1.5(5) . . . . ?
O2A P1A O4A C1U -15.0(6) . . . . ?
O2A P1A C77 C62 63.2(5) . . . . ?
O2A P1A C77 C19 -175.4(5) . . . . ?
O2A P1A C77 C2A -57.9(5) . . . . ?
O12B V3B O13B V4B -61.7(4) . . . . ?
O12B V3B O8B V2B 1.8(8) . . . . ?
O12B P3B O14B C1G 0.3(5) . . . . ?
O12B P3B O15B V4B 3.4(5) . . . . ?
O12B P3B C65 C63 -51.7(5) . . . . ?
O12B P3B C65 C69 -170.9(4) . . . . ?
O12B P3B C65 C76 70.8(5) . . . . ?
O12A V3A O13A V4A 61.7(4) . . . . ?
O12A V3A O8A V2A -0.2(8) . . . . ?
O12A P3A O15A V4A -1.5(5) . . . . ?
O12A P3A O14A C3 8.7(6) . . . . ?
O12A P3A C67 C82 -49.6(5) . . . . ?
O12A P3A C67 C5 -169.0(4) . . . . ?
O12A P3A C67 C2K 72.0(5) . . . . ?
O6B V2B O8B V3B -163.2(4) . . . . ?
O6B V2B O2B V1B 160.4(4) . . . . ?
O18B V1B O2B V2B 96.5(4) . . . . ?
O18B V4B O13B V3B -94.8(4) . . . . ?
O3B V1B O18B V4B 0.5(8) . . . . ?
O3B V1B O2B V2B -62.5(4) . . . . ?
O3B P1B O5B V2B 7.8(5) . . . . ?
O3B P1B O4B C2B 2.3(6) . . . . ?
O3B P1B C55 C79 -47.9(5) . . . . ?
O3B P1B C55 C6 70.7(5) . . . . ?
O3B P1B C55 C13 -167.8(5) . . . . ?
O7B V2B O8B V3B -64.6(4) . . . . ?
O7B V2B O2B V1B -4.0(8) . . . . ?
O7B P2B O9B C2V 1.1(6) . . . . ?
O7B P2B O10B V3B 5.4(5) . . . . ?
O7B P2B C66 C81 -179.9(5) . . . . ?
O7B P2B C66 C85 -58.2(6) . . . . ?
O7B P2B C66 C9 64.4(5) . . . . ?
O4B P1B O5B V2B -114.3(4) . . . . ?
O4B P1B O3B V1B 105.4(4) . . . . ?
O4B P1B C55 C79 69.8(5) . . . . ?
O4B P1B C55 C6 -171.5(4) . . . . ?
O4B P1B C55 C13 -50.0(6) . . . . ?
O6A V2A O3A V1A -161.0(4) . . . . ?
O6A V2A O8A V3A 162.6(4) . . . . ?
O20A V1A O3A V2A -6.5(8) . . . . ?
O20A V1A O18A V4A -62.0(4) . . . . ?
O20A P4A O19A C1J -118.4(5) . . . . ?
O20A P4A O17A V4A -1.1(5) . . . . ?
O20A P4A C64 C72 75.6(5) . . . . ?
O20A P4A C64 C2 -165.1(4) . . . . ?
O20A P4A C64 C1R -44.2(6) . . . . ?
O9A P2A O10A V3A 112.8(4) . . . . ?
O9A P2A O7A V2A -108.5(4) . . . . ?
O9A P2A C2J C71 -169.5(5) . . . . ?
O9A P2A C2J C1H -51.6(6) . . . . ?
O9A P2A C2J C1Q 72.0(6) . . . . ?
O13B V3B O8B V2B -94.1(4) . . . . ?
O13B V4B O18B V1B 93.7(4) . . . . ?
O4A P1A O5A V2A 121.0(4) . . . . ?
O4A P1A O2A V1A -114.7(4) . . . . ?
O4A P1A C77 C62 -54.6(5) . . . . ?
O4A P1A C77 C19 66.8(5) . . . . ?
O4A P1A C77 C2A -175.6(4) . . . . ?
O3A V2A O8A V3A -96.9(4) . . . . ?
O3A V1A O18A V4A 93.8(4) . . . . ?
O8B V3B O13B V4B 96.8(4) . . . . ?
O8B V2B O2B V1B -97.9(4) . . . . ?
C55 P1B O5B V2B 131.1(4) . . . . ?
C55 P1B O3B V1B -138.5(4) . . . . ?
C55 P1B O4B C2B -116.5(5) . . . . ?
C55 C79 C3X C1X 172.7(7) . . . . ?
C55 C79 C43 C3R -173.4(7) . . . . ?
C55 C6 C4F C4C -179.5(8) . . . . ?
C55 C6 C4H C3T 178.2(7) . . . . ?
C55 C13 C1L C32 -178.4(8) . . . . ?
C55 C13 C2R C3H -178.5(8) . . . . ?
O13A V4A O18A V1A -94.0(4) . . . . ?
O13A V3A O8A V2A 96.0(4) . . . . ?
O8A V2A O3A V1A 97.7(4) . . . . ?
O8A V3A O13A V4A -96.4(4) . . . . ?
N58 N88 C31 C39 2.5(9) . . . . ?
N58 N88 C31 C47 -176.7(7) . . . . ?
N58 C28 C39 C31 1.9(10) . . . . ?
O2B V1B O18B V4B -94.1(4) . . . . ?
O2B V2B O8B V3B 94.7(4) . . . . ?
C60 C61 C74 C73 -30.0(8) . . . . ?
C60 C61 C74 C1S 153.0(7) . . . . ?
C60 C61 C93 C78 -65.1(8) . . . . ?
C60 C61 C93 C92 113.5(7) . . . . ?
C60 C70 C2Q C30 -1.1(11) . . . . ?
C61 P4B O19B C83 -125.0(5) . . . . ?
C61 P4B O20B V1B 119.8(4) . . . . ?
C61 P4B O17B V4B -126.2(4) . . . . ?
C61 C60 C70 C2Q 174.4(6) . . . . ?
C61 C60 C1W C1B -172.0(6) . . . . ?
C61 C74 C1S C75 174.0(7) . . . . ?
C62 C77 C19 C2C 93.9(8) . . . . ?
C62 C77 C19 C2Y -82.1(8) . . . . ?
C62 C77 C2A C86 -179.2(6) . . . . ?
C62 C77 C2A C15 4.4(10) . . . . ?
C62 C89 C3O C2T 0.4(12) . . . . ?
C63 C65 C69 C90 48.4(8) . . . . ?
C63 C65 C69 C1D -132.6(7) . . . . ?
C63 C65 C76 C91 -128.8(7) . . . . ?
C63 C65 C76 C2Z 56.1(9) . . . . ?
C63 C98 C12 C36 -0.2(12) . . . . ?
C63 C4 C2I C36 1.6(12) . . . . ?
C64 P4A O19A C1J 124.9(5) . . . . ?
C64 P4A O17A V4A 122.0(4) . . . . ?
C64 P4A O20A V1A -120.8(4) . . . . ?
C64 C72 C84 C1Y 174.5(6) . . . . ?
C64 C72 C1 C38 -176.5(6) . . . . ?
C64 C2 C1A C1I -175.6(6) . . . . ?
C64 C2 C25 C3S 175.8(6) . . . . ?
C64 C1R C3V C3Q -174.3(7) . . . . ?
C65 P3B O14B C1G -117.8(5) . . . . ?
C65 P3B O15B V4B 125.8(4) . . . . ?
C65 P3B O12B V3B -131.9(4) . . . . ?
C65 C63 C98 C12 177.5(7) . . . . ?
C65 C63 C4 C2I -178.1(7) . . . . ?
C65 C69 C90 C11 175.5(7) . . . . ?
C65 C69 C1D C1V -177.4(7) . . . . ?
C65 C76 C91 C3E -175.5(6) . . . . ?
C65 C76 C2Z C2N 174.6(6) . . . . ?
C66 P2B O9B C2V -114.8(5) . . . . ?
C66 P2B O10B V3B 127.8(4) . . . . ?
C66 P2B O7B V2B -131.6(4) . . . . ?
C66 C81 C14 C44 -178.7(7) . . . . ?
C66 C81 C1E C2S 178.9(7) . . . . ?
C66 C85 C16 C22 -179.3(6) . . . . ?
C66 C85 C1P C1C 177.9(7) . . . . ?
C67 P3A O15A V4A -124.3(4) . . . . ?
C67 P3A O14A C3 125.5(5) . . . . ?
C67 P3A O12A V3A 126.2(4) . . . . ?
C67 C82 C17 C3F 179.0(6) . . . . ?
C67 C82 C3K C3L -179.9(7) . . . . ?
C67 C2K C35 C4D -178.2(7) . . . . ?
O18A V4A O13A V3A 97.3(4) . . . . ?
O18A V1A O3A V2A -95.4(4) . . . . ?
C69 C65 C76 C91 -3.9(8) . . . . ?
C69 C65 C76 C2Z -179.0(6) . . . . ?
C69 C90 C11 C1O 3.3(12) . . . . ?
C69 C1D C1V C1O 0.6(12) . . . . ?
C70 C60 C61 P4B -114.1(6) . . . . ?
C70 C60 C61 C74 127.7(6) . . . . ?
C70 C60 C61 C93 3.2(8) . . . . ?
C70 C60 C1W C1B 4.7(10) . . . . ?
C70 C2Q C30 C1B 2.0(12) . . . . ?
C71 C2E C2P C41 -1.2(12) . . . . ?
C71 C2L C3I C41 0.6(13) . . . . ?
C72 C64 C2 C1A 70.6(8) . . . . ?
C72 C64 C2 C25 -106.1(7) . . . . ?
C72 C64 C1R C7 20.2(9) . . . . ?
C72 C64 C1R C3V -164.7(7) . . . . ?
C72 C84 C1Y C8 3.0(11) . . . . ?
C72 C1 C38 C8 1.3(11) . . . . ?
C73 C74 C1S C75 -3.0(11) . . . . ?
C74 C61 C93 C78 170.7(6) . . . . ?
C74 C61 C93 C92 -10.6(8) . . . . ?
C74 C73 C27 C21 -0.2(12) . . . . ?
C75 C21 C27 C73 -0.7(12) . . . . ?
C76 C65 C69 C90 -79.9(7) . . . . ?
C76 C65 C69 C1D 99.0(8) . . . . ?
C76 C91 C3E C45 1.3(11) . . . . ?
C77 P1A O5A V2A -122.9(4) . . . . ?
C77 P1A O2A V1A 129.5(4) . . . . ?
C77 P1A O4A C1U 101.2(5) . . . . ?
C77 C62 C89 C3O -179.1(7) . . . . ?
C77 C62 C18 C94 179.9(7) . . . . ?
C77 C19 C2C C2U -178.5(7) . . . . ?
C77 C19 C2Y C3W 178.5(7) . . . . ?
C78 C1K C2D C1Z 2.1(11) . . . . ?
C79 C55 C6 C4F 64.7(10) . . . . ?
C79 C55 C6 C4H -118.1(7) . . . . ?
C79 C55 C13 C1L -143.0(8) . . . . ?
C79 C55 C13 C2R 28.5(9) . . . . ?
C80 C20 C3P C3B -0.3(12) . . . . ?
C81 C66 C85 C16 5.7(10) . . . . ?
C81 C66 C85 C1P -175.4(7) . . . . ?
C81 C66 C9 C80 -49.7(8) . . . . ?
C81 C66 C9 C95 125.0(7) . . . . ?
C81 C14 C44 C2O 0.6(12) . . . . ?
C81 C1E C2S C2O -1.0(12) . . . . ?
C82 C67 C5 C87 32.9(9) . . . . ?
C82 C67 C5 C97 -151.9(6) . . . . ?
C82 C67 C2K C2H -96.6(8) . . . . ?
C82 C67 C2K C35 73.6(9) . . . . ?
C82 C17 C3F C4T 0.8(11) . . . . ?
C82 C3K C3L C4T 1.0(13) . . . . ?
C84 C72 C1 C38 1.2(10) . . . . ?
C85 C66 C81 C14 -103.0(8) . . . . ?
C85 C66 C81 C1E 77.1(8) . . . . ?
C85 C66 C9 C80 -174.1(6) . . . . ?
C85 C66 C9 C95 0.6(9) . . . . ?
C85 C16 C22 C2W -0.7(11) . . . . ?
C86 C26 C3N C3A 0.3(12) . . . . ?
C87 C2F C3C C1M -0.1(13) . . . . ?
N88 N58 C28 C39 -0.4(9) . . . . ?
N88 N58 C28 C4S -176.9(7) . . . . ?
N88 C31 C39 C28 -2.7(11) . . . . ?
C89 C62 C77 P1A 114.4(6) . . . . ?
C89 C62 C77 C19 -6.8(10) . . . . ?
C89 C62 C77 C2A -128.8(7) . . . . ?
C89 C62 C18 C94 3.9(11) . . . . ?
C90 C69 C1D C1V 1.6(10) . . . . ?
C90 C11 C1O C1V -1.0(12) . . . . ?
C91 C76 C2Z C2N -0.6(10) . . . . ?
C91 C3E C45 C2N -1.4(11) . . . . ?
C92 C1Z C2D C1K -2.2(11) . . . . ?
C93 C61 C74 C73 94.7(8) . . . . ?
C93 C61 C74 C1S -82.3(8) . . . . ?
C93 C78 C1K C2D -0.4(11) . . . . ?
C93 C92 C1Z C2D 0.6(11) . . . . ?
C94 C2T C3O C89 1.5(12) . . . . ?
C95 C3B C3P C20 -0.3(13) . . . . ?
C96 C7 C1R C64 174.3(7) . . . . ?
C96 C7 C1R C3V -0.9(11) . . . . ?
C96 C23 C3Q C3V 1.9(13) . . . . ?
C97 C1M C3C C2F 1.8(12) . . . . ?
C98 C63 C65 P3B -71.5(7) . . . . ?
C98 C63 C65 C69 48.8(8) . . . . ?
C98 C63 C65 C76 173.9(6) . . . . ?
C98 C63 C4 C2I -0.1(10) . . . . ?
C98 C12 C36 C2I 1.7(12) . . . . ?
C99 C1H C2G C3J -1.2(10) . . . . ?
C99 C1H C2J P2A -49.6(8) . . . . ?
C99 C1H C2J C71 65.6(8) . . . . ?
C99 C1H C2J C1Q -170.9(6) . . . . ?
C99 C34 C4A C3J -1.5(12) . . . . ?
N10 C1F C4Q C1T 0.6(10) . . . . ?
C1 C72 C84 C1Y -3.4(10) . . . . ?
C2 C64 C72 C84 -177.9(6) . . . . ?
C2 C64 C72 C1 -0.2(9) . . . . ?
C2 C64 C1R C7 -104.9(8) . . . . ?
C2 C64 C1R C3V 70.1(8) . . . . ?
C2 C1A C1I C37 -1.4(11) . . . . ?
C2 C25 C3S C37 1.2(11) . . . . ?
C4 C63 C65 P3B 106.5(6) . . . . ?
C4 C63 C65 C69 -133.2(7) . . . . ?
C4 C63 C65 C76 -8.1(9) . . . . ?
C4 C63 C98 C12 -0.6(11) . . . . ?
C4 C2I C36 C12 -2.4(12) . . . . ?
C5 C67 C82 C17 53.1(8) . . . . ?
C5 C67 C82 C3K -126.9(7) . . . . ?
C5 C67 C2K C2H 26.9(9) . . . . ?
C5 C67 C2K C35 -162.9(7) . . . . ?
C5 C87 C2F C3C -1.7(13) . . . . ?
C5 C97 C1M C3C -1.7(11) . . . . ?
C6 C55 C79 C3X -177.0(7) . . . . ?
C6 C55 C79 C43 -8.2(10) . . . . ?
C6 C55 C13 C1L 91.4(10) . . . . ?
C6 C55 C13 C2R -97.1(8) . . . . ?
C7 C96 C23 C3Q -1.7(12) . . . . ?
C7 C1R C3V C3Q 1.1(12) . . . . ?
C9 C66 C81 C14 130.5(8) . . . . ?
C9 C66 C81 C1E -49.3(8) . . . . ?
C9 C66 C85 C16 127.5(7) . . . . ?
C9 C66 C85 C1P -53.5(9) . . . . ?
C9 C80 C20 C3P -0.4(11) . . . . ?
C9 C95 C3B C3P 1.5(12) . . . . ?
C11 C1O C1V C1D -0.8(12) . . . . ?
C13 C55 C79 C3X 57.6(9) . . . . ?
C13 C55 C79 C43 -133.6(8) . . . . ?
C13 C55 C6 C4F -170.1(8) . . . . ?
C13 C55 C6 C4H 7.1(9) . . . . ?
C13 C1L C32 C4L -9.2(14) . . . . ?
C13 C2R C3H C4L 1.7(13) . . . . ?
C14 C81 C1E C2S -0.9(11) . . . . ?
C15 C3A C3N C26 -1.2(13) . . . . ?
C16 C85 C1P C1C -3.1(11) . . . . ?
C16 C22 C2W C1C 1.0(11) . . . . ?
C17 C82 C3K C3L 0.1(11) . . . . ?
C17 C3F C4T C3L 0.4(12) . . . . ?
C18 C62 C77 P1A -61.6(8) . . . . ?
C18 C62 C77 C19 177.2(6) . . . . ?
C18 C62 C77 C2A 55.2(9) . . . . ?
C18 C62 C89 C3O -3.0(11) . . . . ?
C18 C94 C2T C3O -0.6(12) . . . . ?
C19 C77 C2A C86 56.7(8) . . . . ?
C19 C77 C2A C15 -119.7(7) . . . . ?
C19 C2C C2U C3M 1.2(12) . . . . ?
C19 C2Y C3W C3M -0.6(13) . . . . ?
C1A C2 C25 C3S -1.0(10) . . . . ?
C1A C1I C37 C3S 1.4(12) . . . . ?
C1D C69 C90 C11 -3.5(11) . . . . ?
C1E C81 C14 C44 1.1(11) . . . . ?
C1F N10 N29 C1T -0.4(9) . . . . ?
C1H C99 C34 C4A 0.4(11) . . . . ?
C1H C2G C3J C4A 0.1(12) . . . . ?
C1I C37 C3S C25 -1.3(11) . . . . ?
C1K C78 C93 C61 177.5(6) . . . . ?
C1K C78 C93 C92 -1.2(10) . . . . ?
C1L C13 C2R C3H -5.9(12) . . . . ?
C1L C32 C4L C3H 3.9(14) . . . . ?
C1M C97 C5 C67 -175.4(7) . . . . ?
C1M C97 C5 C87 -0.1(10) . . . . ?
C1P C85 C16 C22 1.7(10) . . . . ?
C1P C1C C2W C22 -2.4(12) . . . . ?
C1Q C24 C40 C4O -0.2(13) . . . . ?
C1Q C42 C4Y C4O 1.9(12) . . . . ?
C1R C64 C72 C84 57.4(8) . . . . ?
C1R C64 C72 C1 -124.8(7) . . . . ?
C1R C64 C2 C1A -164.1(6) . . . . ?
C1R C64 C2 C25 19.2(8) . . . . ?
C1S C75 C21 C27 -0.2(13) . . . . ?
C1W C60 C61 P4B 62.4(7) . . . . ?
C1W C60 C61 C74 -55.9(7) . . . . ?
C1W C60 C61 C93 179.7(6) . . . . ?
C1W C60 C70 C2Q -2.2(10) . . . . ?
C1W C1B C30 C2Q 0.5(11) . . . . ?
C1Y C8 C38 C1 -1.7(11) . . . . ?
C1Z C92 C93 C61 -177.7(6) . . . . ?
C1Z C92 C93 C78 1.0(10) . . . . ?
C20 C80 C9 C66 176.6(7) . . . . ?
C20 C80 C9 C95 1.6(10) . . . . ?
C21 C75 C1S C74 2.2(13) . . . . ?
C23 C96 C7 C1R 1.3(12) . . . . ?
C23 C3Q C3V C1R -1.6(14) . . . . ?
C24 C1Q C2J P2A 142.6(6) . . . . ?
C24 C1Q C2J C71 27.0(9) . . . . ?
C24 C1Q C2J C1H -96.3(8) . . . . ?
C24 C1Q C42 C4Y -4.3(12) . . . . ?
C24 C40 C4O C4Y -2.4(14) . . . . ?
C25 C2 C1A C1I 1.1(10) . . . . ?
C26 C86 C2A C77 179.4(7) . . . . ?
C26 C86 C2A C15 -4.0(11) . . . . ?
C27 C73 C74 C61 -175.0(6) . . . . ?
C27 C73 C74 C1S 2.1(11) . . . . ?
C28 N58 N88 C31 -1.3(8) . . . . ?
N29 N10 C1F C4B -179.8(8) . . . . ?
N29 N10 C1F C4Q -0.1(9) . . . . ?
N29 C1T C4Q C1F -0.8(10) . . . . ?
C2A C77 C19 C2C -141.0(7) . . . . ?
C2A C77 C19 C2Y 42.9(9) . . . . ?
C2A C86 C26 C3N 2.4(11) . . . . ?
C2A C15 C3A C3N -0.6(13) . . . . ?
C2C C19 C2Y C3W 2.2(11) . . . . ?
C2C C2U C3M C3W 0.4(13) . . . . ?
C2E C71 C2J P2A 125.9(6) . . . . ?
C2E C71 C2J C1H 8.7(9) . . . . ?
C2E C71 C2J C1Q -116.3(7) . . . . ?
C2E C71 C2L C3I -1.9(11) . . . . ?
C2E C2P C41 C3I -0.1(12) . . . . ?
C2F C87 C5 C67 177.3(7) . . . . ?
C2F C87 C5 C97 1.8(11) . . . . ?
C2G C1H C2J P2A 134.4(6) . . . . ?
C2G C1H C2J C71 -110.4(7) . . . . ?
C2G C1H C2J C1Q 13.1(9) . . . . ?
C2G C3J C4A C34 1.2(12) . . . . ?
C2H C2K C35 C4D -8.0(12) . . . . ?
C2H C3Y C46 C4D -4.0(15) . . . . ?
C2J P2A O10A V3A -133.4(4) . . . . ?
C2J P2A O7A V2A 137.3(4) . . . . ?
C2J P2A O9A C1N 117.1(6) . . . . ?
C2J C71 C2E C2P 176.6(7) . . . . ?
C2J C71 C2L C3I -176.4(7) . . . . ?
C2J C1H C2G C3J 175.0(7) . . . . ?
C2J C1Q C24 C40 179.7(7) . . . . ?
C2J C1Q C42 C4Y 179.6(7) . . . . ?
C2K C67 C82 C17 175.2(6) . . . . ?
C2K C67 C82 C3K -4.8(9) . . . . ?
C2K C67 C5 C87 -91.8(8) . . . . ?
C2K C67 C5 C97 83.4(8) . . . . ?
C2K C2H C3Y C46 0.5(13) . . . . ?
C2K C35 C4D C46 4.8(13) . . . . ?
C2L C71 C2E C2P 2.2(11) . . . . ?
C2L C71 C2J P2A -59.8(8) . . . . ?
C2L C71 C2J C1H -177.0(6) . . . . ?
C2L C71 C2J C1Q 58.0(8) . . . . ?
C2L C3I C41 C2P 0.4(13) . . . . ?
C2M C5A C5C C4X -178.2(11) . . . . ?
C2R C13 C1L C32 9.9(13) . . . . ?
C2R C3H C4L C32 -0.6(14) . . . . ?
C2S C2O C44 C14 -2.6(13) . . . . ?
C2T C94 C18 C62 -2.1(12) . . . . ?
C2U C3M C3W C2Y -0.7(14) . . . . ?
C2W C1C C1P C85 3.5(12) . . . . ?
C2X C49 C58 C4R 178.2(10) . . . . ?
C2X C49 C5F C59 179.1(10) . . . . ?
C2Y C19 C2C C2U -2.5(11) . . . . ?
C2Z C76 C91 C3E -0.2(10) . . . . ?
C2Z C2N C45 C3E 0.6(11) . . . . ?
C30 C1B C1W C60 -4.0(11) . . . . ?
C34 C99 C1H C2G 0.9(10) . . . . ?
C34 C99 C1H C2J -175.3(7) . . . . ?
C38 C8 C1Y C84 -0.5(11) . . . . ?
C3A C15 C2A C77 179.6(7) . . . . ?
C3A C15 C2A C86 3.1(11) . . . . ?
C3B C95 C9 C66 -176.9(7) . . . . ?
C3B C95 C9 C80 -2.1(10) . . . . ?
C3G C4R C58 C49 1.2(17) . . . . ?
C3G C59 C5F C49 4.4(15) . . . . ?
C3K C82 C17 C3F -1.0(10) . . . . ?
C3K C3L C4T C3F -1.2(14) . . . . ?
C3U C4X C5C C5A -7.6(19) . . . . ?
C3X C79 C43 C3R -4.0(13) . . . . ?
C3X C1X C4J C3R 4.4(15) . . . . ?
C3Y C2H C2K C67 175.9(7) . . . . ?
C3Y C2H C2K C35 5.5(12) . . . . ?
C3Y C46 C4D C35 1.2(15) . . . . ?
C3Z C5A C5C C4X 6.2(17) . . . . ?
C40 C4O C4Y C42 1.6(13) . . . . ?
C42 C1Q C24 C40 3.5(12) . . . . ?
C42 C1Q C2J P2A -41.4(9) . . . . ?
C42 C1Q C2J C71 -157.0(7) . . . . ?
C42 C1Q C2J C1H 79.6(9) . . . . ?
C43 C79 C3X C1X 3.3(13) . . . . ?
C43 C3R C4J C1X -4.9(15) . . . . ?
C44 C2O C2S C1E 2.7(12) . . . . ?
C45 C2N C2Z C76 0.4(12) . . . . ?
C47 C31 C39 C28 176.4(9) . . . . ?
C4B C1F C4Q C1T -179.8(9) . . . . ?
C4E C3T C4H C6 2.9(13) . . . . ?
C4E C4C C4F C6 -0.6(15) . . . . ?
C4F C6 C4H C3T -4.4(12) . . . . ?
C4F C4C C4E C3T -1.1(14) . . . . ?
C4H C6 C4F C4C 3.4(13) . . . . ?
C4H C3T C4E C4C -0.2(15) . . . . ?
C4J C1X C3X C79 -3.7(14) . . . . ?
C4J C3R C43 C79 4.8(13) . . . . ?
C4K C3U C4X C5C 5.2(19) . . . . ?
C4K C3Z C5A C2M -178.1(11) . . . . ?
C4K C3Z C5A C5C -2.7(17) . . . . ?
C4Q C1T N29 N10 0.7(9) . . . . ?
C4R C3G C59 C5F -1.8(16) . . . . ?
C4S C28 C39 C31 177.8(9) . . . . ?
C4X C3U C4K C3Z -1.8(19) . . . . ?
C56 C1T N29 N10 -178.2(8) . . . . ?
C56 C1T C4Q C1F 178.0(10) . . . . ?
C58 C49 C5F C59 -4.1(15) . . . . ?
C59 C3G C4R C58 -0.9(19) . . . . ?
C5A C3Z C4K C3U 0.6(18) . . . . ?
C5D C48 C5O C51 2.8(19) . . . . ?
C5D C4W C5K C51 -0.8(15) . . . . ?
C5E C4W C5D C48 -178.7(12) . . . . ?
C5E C4W C5K C51 177.3(11) . . . . ?
C5F C49 C58 C4R 1.2(15) . . . . ?
C5H C5I C5B C33 0.0 . . . . ?
C5I C5H C50 C5G 177.4(10) . . . . ?
C5I C5H C50 C57 0.0 . . . . ?
C5I C5B C33 C57 0.0 . . . . ?
C5B C33 C57 C50 0.0 . . . . ?
C33 C57 C50 C5G -177.7(9) . . . . ?
C33 C57 C50 C5H 0.0 . . . . ?
C50 C5H C5I C5B 0.0 . . . . ?
C5K C4W C5D C48 -0.7(17) . . . . ?
C5K C51 C5O C48 -5(2) . . . . ?
C5O C48 C5D C4W 0(2) . . . . ?
C5O C51 C5K C4W 3.7(18) . . . . ?
C4M C4V C54 C53 0.0 . . . . ?
C4V C4M C10 C4U 0.0 . . . . ?
C4V C4M C10 C4P 175.0(11) . . . . ?
C4V C54 C53 C4U 0.0 . . . . ?
C54 C53 C4U C10 0.0 . . . . ?
C53 C4U C10 C4M 0.0 . . . . ?
C53 C4U C10 C4P -174.8(11) . . . . ?
C10 C4M C4V C54 0.0 . . . . ?
C4N C29 C4I C4Z 0.0 . . . . ?
C29 C4N C4G C3D 0.0 . . . . ?
C29 C4N C4G C52 171.8(12) . . . . ?
C29 C4I C4Z C3D 0.0 . . . . ?
C4I C4Z C3D C4G 0.0 . . . . ?
C4Z C3D C4G C4N 0.0 . . . . ?
C4Z C3D C4G C52 -172.0(12) . . . . ?
C4G C4N C29 C4I 0.0 . . . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.079 0.080 0.375 59.7 41.9 ?
2 0.000 0.500 0.500 171.7 90.7 ?
3 -0.079 0.920 0.625 59.7 42.1 ?
4 0.056 0.369 0.775 0.2 0.0 ?
5 0.109 0.327 0.431 0.4 0.0 ?
6 0.128 0.383 0.935 0.1 0.0 ?
7 0.500 0.000 0.000 171.7 90.7 ?
8 0.421 0.580 0.125 59.7 42.1 ?
9 0.579 0.420 0.875 59.7 41.9 ?
10 0.391 0.827 0.069 0.4 0.0 ?
11 0.372 0.883 0.565 0.1 0.0 ?
12 0.444 0.869 0.725 0.2 0.0 ?
13 0.556 0.131 0.275 0.2 0.0 ?
14 0.609 0.173 0.931 0.4 0.0 ?
15 0.628 0.117 0.435 0.1 0.0 ?
16 0.872 0.617 0.065 0.1 0.0 ?
17 0.891 0.673 0.569 0.4 0.0 ?
18 0.944 0.631 0.225 0.2 0.0 ?


#------------------------------------------------------------------#
_database_code_depnum_ccdc_archive 'CCDC 990487'
