# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2017

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_6
_database_code_depnum_ccdc_archive 'CCDC 1536783'
_audit_update_record             
;
2017-06-28 deposited with the CCDC.
2017-06-30 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         'C37 H58 Cl N2 O3 V'
_chemical_formula_sum            'C37 H58 Cl N2 O3 V'
_exptl_crystal_recrystallization_method pentane
_chemical_melting_point          ?

_exptl_crystal_description       plate
_exptl_crystal_colour            blue
_diffrn_ambient_temperature      150(2)
_chemical_formula_weight         665.24

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'
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           19
_space_group_name_H-M_alt        'P 21 21 21'
_space_group_name_Hall           'P 2ac 2ab'
_chemical_absolute_configuration syn

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

_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.
;

_cell_length_a                   9.997(2)
_cell_length_b                   12.560(3)
_cell_length_c                   28.755(6)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3610.5(13)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    1373
_cell_measurement_theta_min      2.60
_cell_measurement_theta_max      18.75
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.224
_exptl_crystal_F_000             1432
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.080
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.040
_exptl_absorpt_coefficient_mu    0.385
_shelx_estimated_absorpt_T_min   0.970
_shelx_estimated_absorpt_T_max   0.985
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9698
_exptl_absorpt_correction_T_max  0.9848
_exptl_absorpt_process_details   'SADABS,  G. M. Sheldrick, 1996'
_exptl_absorpt_special_details   ?
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            39525
_diffrn_reflns_av_unetI/netI     0.1487
_diffrn_reflns_av_R_equivalents  0.1644
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_theta_min         2.153
_diffrn_reflns_theta_max         25.048
_diffrn_reflns_theta_full        25.048
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 0.996
_reflns_number_total             6353
_reflns_number_gt                3895
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.770
_reflns_Friedel_fraction_max     0.996
_reflns_Friedel_fraction_full    0.996

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Sir2004 (M.C. Burla et al, 2005)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    
'Ortep3 for Windows v2.0 (L.J. Farrugia, J. Appl. Cryst. (1997) 30, 565)'
_computing_publication_material  'enCIFer v1.6'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0340P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 1270 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.02(3)
_refine_ls_number_reflns         6353
_refine_ls_number_parameters     397
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1292
_refine_ls_R_factor_gt           0.0546
_refine_ls_wR_factor_ref         0.0978
_refine_ls_wR_factor_gt          0.0848
_refine_ls_goodness_of_fit_ref   0.934
_refine_ls_restrained_S_all      0.934
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
V1 V 0.67632(9) 0.97090(7) 0.49369(3) 0.0129(2) Uani 1 1 d . . . . .
Cl1 Cl 0.89177(13) 1.04385(12) 0.49158(5) 0.0221(4) Uani 1 1 d . . . . .
O1 O 0.6828(4) 0.9926(3) 0.55705(11) 0.0136(10) Uani 1 1 d . . . . .
O2 O 0.6685(4) 0.9927(3) 0.43055(11) 0.0133(10) Uani 1 1 d . . . . .
O3 O 0.7012(3) 0.8453(3) 0.49240(13) 0.0179(9) Uani 1 1 d . . . . .
C24 C 0.7569(6) 1.2530(5) 0.34729(19) 0.0127(16) Uani 1 1 d . . . . .
N2 N 0.4541(4) 0.9328(3) 0.49458(16) 0.0136(11) Uani 1 1 d . . . . .
N1 N 0.5730(4) 1.1359(3) 0.49808(15) 0.0098(10) Uani 1 1 d . . . . .
C61 C 0.7920(6) 1.3478(5) 0.31626(19) 0.0155(16) Uani 1 1 d . . . . .
C11 C 0.7177(6) 1.0735(5) 0.58589(18) 0.0118(16) Uani 1 1 d . . . . .
C21 C 0.6990(6) 1.0756(5) 0.40304(19) 0.0125(15) Uani 1 1 d . . . . .
C12 C 0.7690(6) 1.0482(5) 0.63076(18) 0.0136(16) Uani 1 1 d . . . . .
C41 C 0.8001(6) 1.3283(5) 0.68433(19) 0.0172(16) Uani 1 1 d . . . . .
C23 C 0.8060(7) 1.1514(5) 0.33705(19) 0.0199(17) Uani 1 1 d . . . . .
H23 H 0.861504 1.144166 0.311291 0.024 Uiso 1 1 calc R U . . .
C31 C 0.7965(6) 0.9330(5) 0.64511(19) 0.0159(16) Uani 1 1 d . . . . .
C51 C 0.8233(7) 0.9489(5) 0.34775(19) 0.0183(15) Uani 1 1 d . . . . .
C16 C 0.6988(6) 1.1789(5) 0.57232(18) 0.0134(15) Uani 1 1 d . . . . .
C17 C 0.6588(6) 1.2129(4) 0.52362(17) 0.0146(14) Uani 1 1 d . . . . .
H17A H 0.611742 1.280274 0.525678 0.018 Uiso 1 1 calc R U . . .
H17B H 0.739510 1.224888 0.505624 0.018 Uiso 1 1 calc R U . . .
C2 C 0.3655(4) 1.0277(4) 0.5049(2) 0.0144(12) Uani 1 1 d . . . . .
H2 H 0.320967 1.051224 0.476331 0.017 Uiso 1 1 calc R U . . .
C26 C 0.6468(6) 1.1761(5) 0.41439(18) 0.0149(15) Uani 1 1 d . . . . .
C13 C 0.7969(6) 1.1329(5) 0.66014(19) 0.0148(16) Uani 1 1 d . . . . .
H13 H 0.831346 1.117823 0.689446 0.018 Uiso 1 1 calc R U . . .
C14 C 0.7762(6) 1.2396(5) 0.64834(19) 0.0131(15) Uani 1 1 d . . . . .
C15 C 0.7262(6) 1.2605(5) 0.6041(2) 0.0152(16) Uani 1 1 d . . . . .
H15 H 0.710509 1.330738 0.595378 0.018 Uiso 1 1 calc R U . . .
C7 C 0.2708(6) 0.8627(5) 0.4388(2) 0.0247(18) Uani 1 1 d . . . . .
H7A H 0.260384 0.834546 0.407950 0.037 Uiso 1 1 calc R U . . .
H7B H 0.240247 0.811247 0.461051 0.037 Uiso 1 1 calc R U . . .
H7C H 0.219097 0.926771 0.441765 0.037 Uiso 1 1 calc R U . . .
C1 C 0.4481(6) 1.1177(4) 0.52483(19) 0.0154(14) Uani 1 1 d . . . . .
H1A H 0.395221 1.182492 0.524740 0.018 Uiso 1 1 calc R U . . .
H1B H 0.470723 1.101393 0.556848 0.018 Uiso 1 1 calc R U . . .
C32 C 0.6685(6) 0.8646(5) 0.64422(19) 0.0202(15) Uani 1 1 d . . . . .
H32A H 0.689679 0.793111 0.653394 0.030 Uiso 1 1 calc R U . . .
H32B H 0.603954 0.893963 0.665371 0.030 Uiso 1 1 calc R U . . .
H32C H 0.632019 0.864236 0.613328 0.030 Uiso 1 1 calc R U . . .
C250 C 0.6758(6) 1.2618(5) 0.38628(18) 0.0150(14) Uani 1 1 d . . . . .
H250 H 0.639707 1.327964 0.393674 0.018 Uiso 1 1 calc R U . . .
C22 C 0.7772(6) 1.0601(5) 0.36293(19) 0.0139(16) Uani 1 1 d . . . . .
C34 C 0.8553(6) 0.9242(5) 0.69434(18) 0.0221(17) Uani 1 1 d . . . . .
H34A H 0.870719 0.850647 0.701684 0.033 Uiso 1 1 calc R U . . .
H34B H 0.938335 0.962439 0.695745 0.033 Uiso 1 1 calc R U . . .
H34C H 0.793550 0.953978 0.716358 0.033 Uiso 1 1 calc R U . . .
C6 C 0.4177(6) 0.8875(5) 0.44758(19) 0.0180(16) Uani 1 1 d . . . . .
H6A H 0.468216 0.822308 0.443189 0.022 Uiso 1 1 calc R U . . .
H6B H 0.447144 0.937404 0.423975 0.022 Uiso 1 1 calc R U . . .
C33 C 0.9014(6) 0.8859(5) 0.6120(2) 0.0232(17) Uani 1 1 d . . . . .
H33A H 0.919572 0.813533 0.620678 0.035 Uiso 1 1 calc R U . . .
H33B H 0.868020 0.887893 0.580727 0.035 Uiso 1 1 calc R U . . .
H33C H 0.982307 0.926881 0.613947 0.035 Uiso 1 1 calc R U . . .
C52 C 0.9026(6) 0.9522(5) 0.30216(19) 0.0302(18) Uani 1 1 d . . . . .
H52A H 0.929546 0.881387 0.293852 0.045 Uiso 1 1 calc R U . . .
H52B H 0.847449 0.981311 0.277959 0.045 Uiso 1 1 calc R U . . .
H52C H 0.980422 0.996056 0.306129 0.045 Uiso 1 1 calc R U . . .
C5 C 0.4269(6) 0.8514(5) 0.53221(19) 0.0199(16) Uani 1 1 d . . . . .
H5A H 0.385514 0.788444 0.518970 0.024 Uiso 1 1 calc R U . . .
H5B H 0.509722 0.830521 0.547210 0.024 Uiso 1 1 calc R U . . .
C64 C 0.6934(7) 1.4390(5) 0.3230(2) 0.0327(18) Uani 1 1 d . . . . .
H64A H 0.604657 1.414990 0.315690 0.049 Uiso 1 1 calc R U . . .
H64B H 0.696342 1.462706 0.354700 0.049 Uiso 1 1 calc R U . . .
H64C H 0.717006 1.496879 0.302759 0.049 Uiso 1 1 calc R U . . .
C27 C 0.5399(6) 1.1836(5) 0.45164(18) 0.0167(15) Uani 1 1 d . . . . .
H27A H 0.518826 1.258227 0.456296 0.020 Uiso 1 1 calc R U . . .
H27B H 0.459739 1.149252 0.440004 0.020 Uiso 1 1 calc R U . . .
C54 C 0.6981(7) 0.8790(6) 0.3392(2) 0.037(2) Uani 1 1 d . . . . .
H54A H 0.645994 0.875235 0.367212 0.055 Uiso 1 1 calc R U . . .
H54B H 0.645154 0.909676 0.314811 0.055 Uiso 1 1 calc R U . . .
H54C H 0.725603 0.808611 0.330342 0.055 Uiso 1 1 calc R U . . .
C4 C 0.3352(8) 0.9022(5) 0.5665(2) 0.045(2) Uani 1 1 d . . . . .
H4A H 0.385677 0.932599 0.592047 0.055 Uiso 1 1 calc R U . . .
H4B H 0.272763 0.850389 0.578827 0.055 Uiso 1 1 calc R U . . .
C62 C 0.9325(6) 1.3869(5) 0.3279(2) 0.0256(17) Uani 1 1 d . . . . .
H62A H 0.995214 1.329867 0.323785 0.038 Uiso 1 1 calc R U . . .
H62B H 0.955627 1.444895 0.307708 0.038 Uiso 1 1 calc R U . . .
H62C H 0.934964 1.410721 0.359649 0.038 Uiso 1 1 calc R U . . .
C53 C 0.9125(7) 0.8951(6) 0.3843(2) 0.033(2) Uani 1 1 d . . . . .
H53A H 0.865657 0.891749 0.413451 0.049 Uiso 1 1 calc R U . . .
H53B H 0.934401 0.824364 0.374275 0.049 Uiso 1 1 calc R U . . .
H53C H 0.993190 0.935619 0.388169 0.049 Uiso 1 1 calc R U . . .
C3 C 0.2612(6) 0.9889(5) 0.5401(2) 0.0252(17) Uani 1 1 d . . . . .
H3A H 0.233910 1.045971 0.560699 0.030 Uiso 1 1 calc R U . . .
H3B H 0.182938 0.960519 0.524462 0.030 Uiso 1 1 calc R U . . .
C63 C 0.7886(7) 1.3161(5) 0.26427(19) 0.0333(19) Uani 1 1 d . . . . .
H63A H 0.849917 1.258601 0.258944 0.050 Uiso 1 1 calc R U . . .
H63B H 0.699778 1.294004 0.256023 0.050 Uiso 1 1 calc R U . . .
H63C H 0.813936 1.376171 0.245582 0.050 Uiso 1 1 calc R U . . .
C43 C 0.8011(8) 1.4383(5) 0.6620(2) 0.047(2) Uani 1 1 d . . . . .
H43A H 0.717938 1.449998 0.646150 0.071 Uiso 1 1 calc R U . . .
H43B H 0.812454 1.491474 0.685701 0.071 Uiso 1 1 calc R U . . .
H43C H 0.873559 1.442820 0.640211 0.071 Uiso 1 1 calc R U . . .
C42 C 0.6872(7) 1.3244(5) 0.7203(2) 0.0375(18) Uani 1 1 d . . . . .
H42A H 0.685400 1.255362 0.734616 0.056 Uiso 1 1 calc R U . . .
H42B H 0.702228 1.377752 0.743569 0.056 Uiso 1 1 calc R U . . .
H42C H 0.603235 1.337473 0.705121 0.056 Uiso 1 1 calc R U . . .
C44 C 0.9332(6) 1.3121(6) 0.7092(2) 0.045(2) Uani 1 1 d . . . . .
H44A H 0.934435 1.243041 0.723532 0.068 Uiso 1 1 calc R U . . .
H44B H 1.004980 1.317206 0.687182 0.068 Uiso 1 1 calc R U . . .
H44C H 0.943876 1.365860 0.732671 0.068 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
V1 O3 1.597(3) . ?
V1 O2 1.838(4) . ?
V1 O1 1.843(3) . ?
V1 N2 2.273(4) . ?
V1 N1 2.319(4) . ?
V1 Cl1 2.3414(16) . ?
O1 C11 1.357(6) . ?
O2 C21 1.344(6) . ?
C24 C250 1.388(8) . ?
C24 C23 1.398(8) . ?
C24 C61 1.529(8) . ?
N2 C6 1.511(7) . ?
N2 C2 1.514(6) . ?
N2 C5 1.513(6) . ?
N1 C1 1.484(6) . ?
N1 C17 1.488(6) . ?
N1 C27 1.501(6) . ?
C61 C64 1.524(8) . ?
C61 C62 1.526(8) . ?
C61 C63 1.547(7) . ?
C11 C16 1.393(8) . ?
C11 C12 1.424(7) . ?
C21 C26 1.404(8) . ?
C21 C22 1.407(8) . ?
C12 C13 1.387(8) . ?
C12 C31 1.530(8) . ?
C41 C43 1.523(9) . ?
C41 C44 1.524(9) . ?
C41 C42 1.531(8) . ?
C41 C14 1.539(8) . ?
C23 C22 1.397(8) . ?
C23 H23 0.9300 . ?
C31 C33 1.535(8) . ?
C31 C34 1.537(7) . ?
C31 C32 1.542(8) . ?
C51 C52 1.533(8) . ?
C51 C22 1.534(8) . ?
C51 C53 1.536(8) . ?
C51 C54 1.548(9) . ?
C16 C15 1.401(8) . ?
C16 C17 1.518(7) . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C2 C1 1.513(7) . ?
C2 C3 1.532(7) . ?
C2 H2 0.9800 . ?
C26 C250 1.378(8) . ?
C26 C27 1.516(8) . ?
C13 C14 1.398(8) . ?
C13 H13 0.9300 . ?
C14 C15 1.392(8) . ?
C15 H15 0.9300 . ?
C7 C6 1.522(8) . ?
C7 H7A 0.9600 . ?
C7 H7B 0.9600 . ?
C7 H7C 0.9600 . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C32 H32A 0.9600 . ?
C32 H32B 0.9600 . ?
C32 H32C 0.9600 . ?
C250 H250 0.9300 . ?
C34 H34A 0.9600 . ?
C34 H34B 0.9600 . ?
C34 H34C 0.9600 . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C33 H33A 0.9600 . ?
C33 H33B 0.9600 . ?
C33 H33C 0.9600 . ?
C52 H52A 0.9600 . ?
C52 H52B 0.9600 . ?
C52 H52C 0.9600 . ?
C5 C4 1.489(8) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C64 H64A 0.9600 . ?
C64 H64B 0.9600 . ?
C64 H64C 0.9600 . ?
C27 H27A 0.9700 . ?
C27 H27B 0.9700 . ?
C54 H54A 0.9600 . ?
C54 H54B 0.9600 . ?
C54 H54C 0.9600 . ?
C4 C3 1.519(8) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C62 H62A 0.9600 . ?
C62 H62B 0.9600 . ?
C62 H62C 0.9600 . ?
C53 H53A 0.9600 . ?
C53 H53B 0.9600 . ?
C53 H53C 0.9600 . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C63 H63A 0.9600 . ?
C63 H63B 0.9600 . ?
C63 H63C 0.9600 . ?
C43 H43A 0.9600 . ?
C43 H43B 0.9600 . ?
C43 H43C 0.9600 . ?
C42 H42A 0.9600 . ?
C42 H42B 0.9600 . ?
C42 H42C 0.9600 . ?
C44 H44A 0.9600 . ?
C44 H44B 0.9600 . ?
C44 H44C 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
O3 V1 O2 97.50(18) . . ?
O3 V1 O1 99.40(18) . . ?
O2 V1 O1 162.96(14) . . ?
O3 V1 N2 86.83(16) . . ?
O2 V1 N2 90.04(17) . . ?
O1 V1 N2 93.13(17) . . ?
O3 V1 N1 162.39(16) . . ?
O2 V1 N1 84.37(16) . . ?
O1 V1 N1 80.21(16) . . ?
N2 V1 N1 75.63(14) . . ?
O3 V1 Cl1 104.03(13) . . ?
O2 V1 Cl1 87.45(14) . . ?
O1 V1 Cl1 86.29(13) . . ?
N2 V1 Cl1 169.08(11) . . ?
N1 V1 Cl1 93.54(11) . . ?
C11 O1 V1 136.4(3) . . ?
C21 O2 V1 133.4(3) . . ?
C250 C24 C23 116.6(6) . . ?
C250 C24 C61 122.9(6) . . ?
C23 C24 C61 120.5(5) . . ?
C6 N2 C2 109.3(4) . . ?
C6 N2 C5 110.0(4) . . ?
C2 N2 C5 106.6(4) . . ?
C6 N2 V1 107.8(3) . . ?
C2 N2 V1 114.1(3) . . ?
C5 N2 V1 109.0(3) . . ?
C1 N1 C17 109.2(4) . . ?
C1 N1 C27 109.7(4) . . ?
C17 N1 C27 107.8(4) . . ?
C1 N1 V1 105.4(3) . . ?
C17 N1 V1 110.5(3) . . ?
C27 N1 V1 114.0(3) . . ?
C64 C61 C62 109.0(5) . . ?
C64 C61 C24 111.3(5) . . ?
C62 C61 C24 109.5(5) . . ?
C64 C61 C63 107.5(5) . . ?
C62 C61 C63 108.4(5) . . ?
C24 C61 C63 111.0(5) . . ?
O1 C11 C16 120.4(5) . . ?
O1 C11 C12 118.6(5) . . ?
C16 C11 C12 120.9(5) . . ?
O2 C21 C26 118.4(5) . . ?
O2 C21 C22 120.1(5) . . ?
C26 C21 C22 121.4(5) . . ?
C13 C12 C11 117.0(6) . . ?
C13 C12 C31 121.7(5) . . ?
C11 C12 C31 121.3(5) . . ?
C43 C41 C44 108.3(6) . . ?
C43 C41 C42 108.5(6) . . ?
C44 C41 C42 108.8(5) . . ?
C43 C41 C14 112.0(5) . . ?
C44 C41 C14 110.8(5) . . ?
C42 C41 C14 108.4(5) . . ?
C22 C23 C24 124.4(6) . . ?
C22 C23 H23 117.8 . . ?
C24 C23 H23 117.8 . . ?
C12 C31 C33 108.7(5) . . ?
C12 C31 C34 112.7(5) . . ?
C33 C31 C34 106.4(5) . . ?
C12 C31 C32 111.9(5) . . ?
C33 C31 C32 110.0(5) . . ?
C34 C31 C32 107.0(5) . . ?
C52 C51 C22 112.0(5) . . ?
C52 C51 C53 107.3(5) . . ?
C22 C51 C53 112.3(5) . . ?
C52 C51 C54 107.3(5) . . ?
C22 C51 C54 108.6(5) . . ?
C53 C51 C54 109.1(5) . . ?
C11 C16 C15 119.1(5) . . ?
C11 C16 C17 124.2(5) . . ?
C15 C16 C17 116.6(5) . . ?
N1 C17 C16 115.1(4) . . ?
N1 C17 H17A 108.5 . . ?
C16 C17 H17A 108.5 . . ?
N1 C17 H17B 108.5 . . ?
C16 C17 H17B 108.5 . . ?
H17A C17 H17B 107.5 . . ?
N2 C2 C1 110.1(4) . . ?
N2 C2 C3 106.1(4) . . ?
C1 C2 C3 111.0(5) . . ?
N2 C2 H2 109.9 . . ?
C1 C2 H2 109.9 . . ?
C3 C2 H2 109.9 . . ?
C250 C26 C21 119.2(5) . . ?
C250 C26 C27 120.9(5) . . ?
C21 C26 C27 118.8(5) . . ?
C12 C13 C14 123.9(6) . . ?
C12 C13 H13 118.0 . . ?
C14 C13 H13 118.0 . . ?
C15 C14 C13 117.1(5) . . ?
C15 C14 C41 122.3(6) . . ?
C13 C14 C41 120.5(5) . . ?
C14 C15 C16 121.9(6) . . ?
C14 C15 H15 119.1 . . ?
C16 C15 H15 119.1 . . ?
C6 C7 H7A 109.5 . . ?
C6 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C6 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
N1 C1 C2 112.2(4) . . ?
N1 C1 H1A 109.2 . . ?
C2 C1 H1A 109.2 . . ?
N1 C1 H1B 109.2 . . ?
C2 C1 H1B 109.2 . . ?
H1A C1 H1B 107.9 . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C26 C250 C24 122.3(6) . . ?
C26 C250 H250 118.9 . . ?
C24 C250 H250 118.9 . . ?
C23 C22 C21 116.0(6) . . ?
C23 C22 C51 122.3(5) . . ?
C21 C22 C51 121.7(5) . . ?
C31 C34 H34A 109.5 . . ?
C31 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
C31 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
N2 C6 C7 117.3(5) . . ?
N2 C6 H6A 108.0 . . ?
C7 C6 H6A 108.0 . . ?
N2 C6 H6B 108.0 . . ?
C7 C6 H6B 108.0 . . ?
H6A C6 H6B 107.2 . . ?
C31 C33 H33A 109.5 . . ?
C31 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
C31 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C51 C52 H52A 109.5 . . ?
C51 C52 H52B 109.5 . . ?
H52A C52 H52B 109.5 . . ?
C51 C52 H52C 109.5 . . ?
H52A C52 H52C 109.5 . . ?
H52B C52 H52C 109.5 . . ?
C4 C5 N2 107.1(5) . . ?
C4 C5 H5A 110.3 . . ?
N2 C5 H5A 110.3 . . ?
C4 C5 H5B 110.3 . . ?
N2 C5 H5B 110.3 . . ?
H5A C5 H5B 108.6 . . ?
C61 C64 H64A 109.5 . . ?
C61 C64 H64B 109.5 . . ?
H64A C64 H64B 109.5 . . ?
C61 C64 H64C 109.5 . . ?
H64A C64 H64C 109.5 . . ?
H64B C64 H64C 109.5 . . ?
N1 C27 C26 116.7(5) . . ?
N1 C27 H27A 108.1 . . ?
C26 C27 H27A 108.1 . . ?
N1 C27 H27B 108.1 . . ?
C26 C27 H27B 108.1 . . ?
H27A C27 H27B 107.3 . . ?
C51 C54 H54A 109.5 . . ?
C51 C54 H54B 109.5 . . ?
H54A C54 H54B 109.5 . . ?
C51 C54 H54C 109.5 . . ?
H54A C54 H54C 109.5 . . ?
H54B C54 H54C 109.5 . . ?
C5 C4 C3 106.0(5) . . ?
C5 C4 H4A 110.5 . . ?
C3 C4 H4A 110.5 . . ?
C5 C4 H4B 110.5 . . ?
C3 C4 H4B 110.5 . . ?
H4A C4 H4B 108.7 . . ?
C61 C62 H62A 109.5 . . ?
C61 C62 H62B 109.5 . . ?
H62A C62 H62B 109.5 . . ?
C61 C62 H62C 109.5 . . ?
H62A C62 H62C 109.5 . . ?
H62B C62 H62C 109.5 . . ?
C51 C53 H53A 109.5 . . ?
C51 C53 H53B 109.5 . . ?
H53A C53 H53B 109.5 . . ?
C51 C53 H53C 109.5 . . ?
H53A C53 H53C 109.5 . . ?
H53B C53 H53C 109.5 . . ?
C4 C3 C2 103.1(5) . . ?
C4 C3 H3A 111.2 . . ?
C2 C3 H3A 111.2 . . ?
C4 C3 H3B 111.2 . . ?
C2 C3 H3B 111.2 . . ?
H3A C3 H3B 109.1 . . ?
C61 C63 H63A 109.5 . . ?
C61 C63 H63B 109.5 . . ?
H63A C63 H63B 109.5 . . ?
C61 C63 H63C 109.5 . . ?
H63A C63 H63C 109.5 . . ?
H63B C63 H63C 109.5 . . ?
C41 C43 H43A 109.5 . . ?
C41 C43 H43B 109.5 . . ?
H43A C43 H43B 109.5 . . ?
C41 C43 H43C 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
C41 C42 H42A 109.5 . . ?
C41 C42 H42B 109.5 . . ?
H42A C42 H42B 109.5 . . ?
C41 C42 H42C 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
C41 C44 H44A 109.5 . . ?
C41 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
C41 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O3 V1 O1 C11 151.0(5) . . . . ?
O2 V1 O1 C11 -21.3(9) . . . . ?
N2 V1 O1 C11 -121.7(5) . . . . ?
N1 V1 O1 C11 -46.9(5) . . . . ?
Cl1 V1 O1 C11 47.4(5) . . . . ?
O3 V1 O2 C21 -150.5(5) . . . . ?
O1 V1 O2 C21 21.8(9) . . . . ?
N2 V1 O2 C21 122.6(5) . . . . ?
N1 V1 O2 C21 47.1(5) . . . . ?
Cl1 V1 O2 C21 -46.7(5) . . . . ?
C250 C24 C61 C64 -19.4(8) . . . . ?
C23 C24 C61 C64 160.2(6) . . . . ?
C250 C24 C61 C62 101.1(7) . . . . ?
C23 C24 C61 C62 -79.2(7) . . . . ?
C250 C24 C61 C63 -139.2(6) . . . . ?
C23 C24 C61 C63 40.5(8) . . . . ?
V1 O1 C11 C16 31.6(8) . . . . ?
V1 O1 C11 C12 -150.8(4) . . . . ?
V1 O2 C21 C26 -50.4(8) . . . . ?
V1 O2 C21 C22 132.1(5) . . . . ?
O1 C11 C12 C13 -176.7(5) . . . . ?
C16 C11 C12 C13 0.9(9) . . . . ?
O1 C11 C12 C31 5.4(8) . . . . ?
C16 C11 C12 C31 -177.0(5) . . . . ?
C250 C24 C23 C22 0.9(9) . . . . ?
C61 C24 C23 C22 -178.8(6) . . . . ?
C13 C12 C31 C33 -117.1(6) . . . . ?
C11 C12 C31 C33 60.7(7) . . . . ?
C13 C12 C31 C34 0.5(8) . . . . ?
C11 C12 C31 C34 178.3(5) . . . . ?
C13 C12 C31 C32 121.2(6) . . . . ?
C11 C12 C31 C32 -61.0(7) . . . . ?
O1 C11 C16 C15 175.2(5) . . . . ?
C12 C11 C16 C15 -2.3(9) . . . . ?
O1 C11 C16 C17 -9.2(9) . . . . ?
C12 C11 C16 C17 173.2(5) . . . . ?
C1 N1 C17 C16 59.0(6) . . . . ?
C27 N1 C17 C16 178.2(5) . . . . ?
V1 N1 C17 C16 -56.5(5) . . . . ?
C11 C16 C17 N1 31.3(8) . . . . ?
C15 C16 C17 N1 -153.0(5) . . . . ?
C6 N2 C2 C1 -136.1(5) . . . . ?
C5 N2 C2 C1 105.1(5) . . . . ?
V1 N2 C2 C1 -15.4(5) . . . . ?
C6 N2 C2 C3 103.7(5) . . . . ?
C5 N2 C2 C3 -15.1(5) . . . . ?
V1 N2 C2 C3 -135.6(3) . . . . ?
O2 C21 C26 C250 -179.2(5) . . . . ?
C22 C21 C26 C250 -1.7(9) . . . . ?
O2 C21 C26 C27 -10.6(8) . . . . ?
C22 C21 C26 C27 166.9(5) . . . . ?
C11 C12 C13 C14 0.7(9) . . . . ?
C31 C12 C13 C14 178.6(6) . . . . ?
C12 C13 C14 C15 -0.8(9) . . . . ?
C12 C13 C14 C41 175.5(6) . . . . ?
C43 C41 C14 C15 -16.1(9) . . . . ?
C44 C41 C14 C15 -137.0(6) . . . . ?
C42 C41 C14 C15 103.7(7) . . . . ?
C43 C41 C14 C13 167.8(6) . . . . ?
C44 C41 C14 C13 46.8(8) . . . . ?
C42 C41 C14 C13 -72.5(7) . . . . ?
C13 C14 C15 C16 -0.7(9) . . . . ?
C41 C14 C15 C16 -176.9(6) . . . . ?
C11 C16 C15 C14 2.3(9) . . . . ?
C17 C16 C15 C14 -173.7(5) . . . . ?
C17 N1 C1 C2 -171.1(4) . . . . ?
C27 N1 C1 C2 70.9(5) . . . . ?
V1 N1 C1 C2 -52.3(5) . . . . ?
N2 C2 C1 N1 46.2(6) . . . . ?
C3 C2 C1 N1 163.3(4) . . . . ?
C21 C26 C250 C24 -1.1(9) . . . . ?
C27 C26 C250 C24 -169.4(5) . . . . ?
C23 C24 C250 C26 1.5(9) . . . . ?
C61 C24 C250 C26 -178.8(5) . . . . ?
C24 C23 C22 C21 -3.4(9) . . . . ?
C24 C23 C22 C51 174.4(6) . . . . ?
O2 C21 C22 C23 -178.8(5) . . . . ?
C26 C21 C22 C23 3.8(9) . . . . ?
O2 C21 C22 C51 3.4(9) . . . . ?
C26 C21 C22 C51 -174.0(5) . . . . ?
C52 C51 C22 C23 0.2(8) . . . . ?
C53 C51 C22 C23 121.1(6) . . . . ?
C54 C51 C22 C23 -118.1(6) . . . . ?
C52 C51 C22 C21 177.9(5) . . . . ?
C53 C51 C22 C21 -61.3(8) . . . . ?
C54 C51 C22 C21 59.6(7) . . . . ?
C2 N2 C6 C7 -51.5(6) . . . . ?
C5 N2 C6 C7 65.3(7) . . . . ?
V1 N2 C6 C7 -176.0(4) . . . . ?
C6 N2 C5 C4 -124.2(6) . . . . ?
C2 N2 C5 C4 -5.8(6) . . . . ?
V1 N2 C5 C4 117.9(5) . . . . ?
C1 N1 C27 C26 -161.6(5) . . . . ?
C17 N1 C27 C26 79.5(6) . . . . ?
V1 N1 C27 C26 -43.6(6) . . . . ?
C250 C26 C27 N1 -136.7(5) . . . . ?
C21 C26 C27 N1 54.9(7) . . . . ?
N2 C5 C4 C3 24.7(7) . . . . ?
C5 C4 C3 C2 -33.4(7) . . . . ?
N2 C2 C3 C4 29.6(6) . . . . ?
C1 C2 C3 C4 -90.0(6) . . . . ?

_refine_diff_density_max         0.371
_refine_diff_density_min         -0.371
_refine_diff_density_rms         0.073

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_3
_database_code_depnum_ccdc_archive 'CCDC 1536785'
_audit_update_record             
;
2017-06-28 deposited with the CCDC.
2017-06-30 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         'C45 H69 N2 O3 V, C4 H10 O'
_chemical_formula_sum            'C49 H79 N2 O4 V'
_chemical_properties_physical    
'air-sensitive, moisture-sensitive, paramagnetic'
_exptl_crystal_recrystallization_method Et2O
_chemical_melting_point          ?

_exptl_crystal_description       plate
_exptl_crystal_colour            green
_diffrn_ambient_temperature      150(2)
_chemical_formula_weight         811.08

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

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'
_chemical_absolute_configuration .

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

_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.
;

_cell_length_a                   10.4460(4)
_cell_length_b                   22.8520(9)
_cell_length_c                   19.6630(7)
_cell_angle_alpha                90
_cell_angle_beta                 101.824(2)
_cell_angle_gamma                90
_cell_volume                     4594.2(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    10777
_cell_measurement_theta_min      2.88
_cell_measurement_theta_max      27.90
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.173
_exptl_crystal_F_000             1768
_exptl_transmission_factor_min   2.88
_exptl_transmission_factor_max   27.90
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.050
_exptl_absorpt_coefficient_mu    0.260
_shelx_estimated_absorpt_T_min   0.903
_shelx_estimated_absorpt_T_max   0.987
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9033
_exptl_absorpt_correction_T_max  0.9871
_exptl_absorpt_process_details   'SADABS,  G. M. Sheldrick, 1996'
_exptl_absorpt_special_details   ?
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            47432
_diffrn_reflns_av_unetI/netI     0.0451
_diffrn_reflns_av_R_equivalents  0.0624
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         2.876
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_full        25.027
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             8110
_reflns_number_gt                6308
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Sir2004 (M.C. Burla et al, 2005)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    
'Ortep3 for Windows v2.0 (L.J. Farrugia, J. Appl. Cryst. (1997) 30, 565)'
_computing_publication_material  'enCIFer v1.6'

_refine_special_details          
;
The THF ligands present disorder in atoms C72 and C73. A disorder model was applied giving 26/74% occupancies. SADI restraints and EADP constraints were applied on the disordered atoms.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0635P)²+3.1005P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         8110
_refine_ls_number_parameters     514
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0675
_refine_ls_R_factor_gt           0.0485
_refine_ls_wR_factor_ref         0.1328
_refine_ls_wR_factor_gt          0.1255
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_restrained_S_all      1.059
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
V1 V 0.62549(4) 0.17494(2) 0.13103(2) 0.01481(12) Uani 1 1 d . . . . .
O1 O 0.66204(15) 0.10553(7) 0.18824(8) 0.0176(4) Uani 1 1 d . . . . .
O2 O 0.61962(15) 0.25313(7) 0.09357(8) 0.0180(4) Uani 1 1 d . . . . .
O3 O 0.64722(16) 0.22052(7) 0.23017(8) 0.0203(4) Uani 1 1 d . . . . .
N1 N 0.84322(18) 0.17650(8) 0.13528(10) 0.0167(4) Uani 1 1 d . . . . .
N2 N 0.63466(19) 0.13272(9) 0.02986(10) 0.0192(4) Uani 1 1 d . . . . .
C81 C 0.41268(19) 0.16488(9) 0.11449(11) 0.0107(4) Uani 1 1 d . . . . .
H81A H 0.374560 0.184463 0.071317 0.013 Uiso 1 1 calc R U . . .
H81B H 0.392922 0.123545 0.107850 0.013 Uiso 1 1 calc R U . . .
C13 C 0.8522(2) -0.02520(10) 0.25159(12) 0.0207(5) Uani 1 1 d . . . . .
H13 H 0.839240 -0.063553 0.264506 0.025 Uiso 1 1 calc R U . . .
C12 C 0.7417(2) 0.00994(10) 0.23017(12) 0.0181(5) Uani 1 1 d . . . . .
C22 C 0.6437(2) 0.33299(10) 0.01597(12) 0.0174(5) Uani 1 1 d . . . . .
C11 C 0.7606(2) 0.06814(10) 0.20932(12) 0.0160(5) Uani 1 1 d . . . . .
C31 C 0.6054(2) -0.01340(10) 0.23493(13) 0.0207(5) Uani 1 1 d . . . . .
C51 C 0.4997(2) 0.35283(11) 0.00546(13) 0.0220(5) Uani 1 1 d . . . . .
C21 C 0.6944(2) 0.28646(10) 0.06107(12) 0.0161(5) Uani 1 1 d . . . . .
C3 C 0.6239(3) 0.06846(11) 0.03399(13) 0.0255(6) Uani 1 1 d . . . . .
H3A H 0.689715 0.054035 0.071668 0.038 Uiso 1 1 calc R U . . .
H3B H 0.538886 0.058278 0.041791 0.038 Uiso 1 1 calc R U . . .
H3C H 0.636015 0.051273 -0.008786 0.038 Uiso 1 1 calc R U . . .
C15 C 0.9959(2) 0.05080(11) 0.23554(13) 0.0218(5) Uani 1 1 d . . . . .
H15 H 1.079902 0.064920 0.237091 0.026 Uiso 1 1 calc R U . . .
C4 C 0.5319(3) 0.15302(12) -0.02859(13) 0.0259(6) Uani 1 1 d . . . . .
H4A H 0.536658 0.194801 -0.032502 0.039 Uiso 1 1 calc R U . . .
H4B H 0.544716 0.135220 -0.070921 0.039 Uiso 1 1 calc R U . . .
H4C H 0.447587 0.142224 -0.020343 0.039 Uiso 1 1 calc R U . . .
C25 C 0.9114(2) 0.30694(10) 0.03989(12) 0.0191(5) Uani 1 1 d . . . . .
H25 H 1.000068 0.297895 0.048288 0.023 Uiso 1 1 calc R U . . .
C16 C 0.8903(2) 0.08786(10) 0.21397(12) 0.0186(5) Uani 1 1 d . . . . .
C26 C 0.8304(2) 0.27624(10) 0.07471(12) 0.0179(5) Uani 1 1 d . . . . .
C14 C 0.9800(2) -0.00673(11) 0.25488(13) 0.0218(5) Uani 1 1 d . . . . .
C23 C 0.7310(2) 0.36333(10) -0.01665(12) 0.0194(5) Uani 1 1 d . . . . .
H23 H 0.697878 0.393767 -0.046511 0.023 Uiso 1 1 calc R U . . .
C54 C 0.4682(3) 0.40383(13) -0.04571(15) 0.0344(7) Uani 1 1 d . . . . .
H54A H 0.484620 0.392275 -0.090068 0.052 Uiso 1 1 calc R U . . .
H54B H 0.377807 0.414430 -0.050621 0.052 Uiso 1 1 calc R U . . .
H54C H 0.522267 0.436757 -0.028519 0.052 Uiso 1 1 calc R U . . .
C27 C 0.8910(2) 0.23779(10) 0.13497(13) 0.0200(5) Uani 1 1 d . . . . .
H27A H 0.984481 0.236497 0.136969 0.024 Uiso 1 1 calc R U . . .
H27B H 0.877988 0.256559 0.177288 0.024 Uiso 1 1 calc R U . . .
C24 C 0.8636(2) 0.35103(10) -0.00739(12) 0.0185(5) Uani 1 1 d . . . . .
C61 C 0.9567(2) 0.38484(11) -0.04426(13) 0.0228(6) Uani 1 1 d . . . . .
C1 C 0.8724(2) 0.14255(11) 0.07597(13) 0.0223(5) Uani 1 1 d . . . . .
H1A H 0.883785 0.101606 0.088794 0.027 Uiso 1 1 calc R U . . .
H1B H 0.953409 0.156530 0.064873 0.027 Uiso 1 1 calc R U . . .
C33 C 0.5550(3) 0.02153(12) 0.29085(14) 0.0271(6) Uani 1 1 d . . . . .
H33A H 0.552773 0.062410 0.279429 0.041 Uiso 1 1 calc R U . . .
H33B H 0.468444 0.008534 0.292901 0.041 Uiso 1 1 calc R U . . .
H33C H 0.612151 0.015463 0.335149 0.041 Uiso 1 1 calc R U . . .
C53 C 0.4060(2) 0.30258(12) -0.02271(14) 0.0292(6) Uani 1 1 d . . . . .
H53A H 0.423122 0.269730 0.008249 0.044 Uiso 1 1 calc R U . . .
H53B H 0.317296 0.315311 -0.026123 0.044 Uiso 1 1 calc R U . . .
H53C H 0.418919 0.291323 -0.067852 0.044 Uiso 1 1 calc R U . . .
C82 C 0.3464(2) 0.18610(12) 0.16735(14) 0.0283(6) Uani 1 1 d . . . . .
C17 C 0.9163(2) 0.15130(11) 0.20221(12) 0.0197(5) Uani 1 1 d . . . . .
H17A H 0.894654 0.173805 0.240148 0.024 Uiso 1 1 calc R U . . .
H17B H 1.009184 0.156131 0.204055 0.024 Uiso 1 1 calc R U . . .
C2 C 0.7634(2) 0.14863(11) 0.01326(13) 0.0220(5) Uani 1 1 d . . . . .
H2A H 0.760068 0.188690 -0.003325 0.026 Uiso 1 1 calc R U . . .
H2B H 0.780614 0.123428 -0.023540 0.026 Uiso 1 1 calc R U . . .
C34 C 0.6073(3) -0.07817(11) 0.25514(15) 0.0314(6) Uani 1 1 d . . . . .
H34A H 0.638570 -0.101066 0.220971 0.047 Uiso 1 1 calc R U . . .
H34B H 0.664159 -0.083550 0.299684 0.047 Uiso 1 1 calc R U . . .
H34C H 0.520452 -0.090479 0.257436 0.047 Uiso 1 1 calc R U . . .
C41 C 1.1002(3) -0.04553(11) 0.28120(14) 0.0283(6) Uani 1 1 d . . . . .
C43 C 1.1848(3) -0.01833(14) 0.34649(16) 0.0428(8) Uani 1 1 d . . . . .
H43A H 1.209506 0.020636 0.336213 0.064 Uiso 1 1 calc R U . . .
H43B H 1.135961 -0.016962 0.382839 0.064 Uiso 1 1 calc R U . . .
H43C H 1.261961 -0.041629 0.361313 0.064 Uiso 1 1 calc R U . . .
C52 C 0.4720(3) 0.37329(12) 0.07541(14) 0.0300(6) Uani 1 1 d . . . . .
H52A H 0.491034 0.342096 0.108657 0.045 Uiso 1 1 calc R U . . .
H52B H 0.526111 0.406444 0.091712 0.045 Uiso 1 1 calc R U . . .
H52C H 0.381651 0.384117 0.069610 0.045 Uiso 1 1 calc R U . . .
C62 C 0.8855(3) 0.43336(12) -0.09090(15) 0.0311(6) Uani 1 1 d . . . . .
H62A H 0.846324 0.460035 -0.063429 0.047 Uiso 1 1 calc R U . . .
H62B H 0.946870 0.454057 -0.112273 0.047 Uiso 1 1 calc R U . . .
H62C H 0.818694 0.416409 -0.126264 0.047 Uiso 1 1 calc R U . . .
C63 C 1.0662(3) 0.41289(13) 0.01017(15) 0.0331(7) Uani 1 1 d . . . . .
H63A H 1.028588 0.439110 0.038839 0.050 Uiso 1 1 calc R U . . .
H63B H 1.114345 0.382844 0.038586 0.050 Uiso 1 1 calc R U . . .
H63C H 1.124012 0.434244 -0.012922 0.050 Uiso 1 1 calc R U . . .
C42 C 1.0627(3) -0.10736(12) 0.29938(18) 0.0402(8) Uani 1 1 d . . . . .
H42A H 1.011473 -0.105406 0.334634 0.060 Uiso 1 1 calc R U . . .
H42B H 1.012639 -0.125829 0.258651 0.060 Uiso 1 1 calc R U . . .
H42C H 1.140601 -0.129700 0.316272 0.060 Uiso 1 1 calc R U . . .
C64 C 1.0177(3) 0.34325(13) -0.08950(14) 0.0318(6) Uani 1 1 d . . . . .
H64A H 1.062946 0.312416 -0.061192 0.048 Uiso 1 1 calc R U . . .
H64B H 0.950230 0.326772 -0.124871 0.048 Uiso 1 1 calc R U . . .
H64C H 1.078405 0.364420 -0.110880 0.048 Uiso 1 1 calc R U . . .
C44 C 1.1818(3) -0.05009(13) 0.22494(17) 0.0384(7) Uani 1 1 d . . . . .
H44A H 1.206274 -0.011591 0.212807 0.058 Uiso 1 1 calc R U . . .
H44B H 1.259039 -0.072704 0.242196 0.058 Uiso 1 1 calc R U . . .
H44C H 1.131076 -0.068833 0.184576 0.058 Uiso 1 1 calc R U . . .
C32 C 0.5093(2) -0.00755(12) 0.16471(13) 0.0270(6) Uani 1 1 d . . . . .
H32A H 0.505149 0.032606 0.150072 0.040 Uiso 1 1 calc R U . . .
H32B H 0.538664 -0.031333 0.130678 0.040 Uiso 1 1 calc R U . . .
H32C H 0.424011 -0.020262 0.169546 0.040 Uiso 1 1 calc R U . . .
C84 C 0.2759(3) 0.17012(19) 0.27658(17) 0.0520(9) Uani 1 1 d . . . . .
H84 H 0.266858 0.144873 0.312390 0.062 Uiso 1 1 calc R U . . .
C83 C 0.3291(3) 0.14989(15) 0.22235(15) 0.0373(7) Uani 1 1 d . . . . .
H83 H 0.354446 0.110880 0.222262 0.045 Uiso 1 1 calc R U . . .
C86 C 0.2473(3) 0.26401(16) 0.2239(2) 0.0553(10) Uani 1 1 d . . . . .
H86 H 0.218748 0.302562 0.223983 0.066 Uiso 1 1 calc R U . . .
C87 C 0.3012(3) 0.24349(14) 0.16872(18) 0.0416(8) Uani 1 1 d . . . . .
H87 H 0.307022 0.268620 0.132275 0.050 Uiso 1 1 calc R U . . .
C85 C 0.2363(3) 0.2272(2) 0.27801(19) 0.0597(11) Uani 1 1 d . . . . .
H85 H 0.202315 0.241008 0.315146 0.072 Uiso 1 1 calc R U . . .
C71 C 0.6488(3) 0.19311(11) 0.29687(12) 0.0255(6) Uani 1 1 d . . . . .
H71A H 0.713119 0.161923 0.305386 0.031 Uiso 1 1 calc R U . A 1
H71B H 0.563639 0.176951 0.298460 0.031 Uiso 1 1 calc R U . A 1
C74 C 0.6264(3) 0.28270(11) 0.23686(14) 0.0313(6) Uani 1 1 d . . . . .
H74A H 0.547971 0.295067 0.204539 0.038 Uiso 1 1 calc R U . B 1
H74B H 0.700138 0.304634 0.227236 0.038 Uiso 1 1 calc R U . B 1
C72A C 0.6846(5) 0.2415(2) 0.3502(3) 0.0296(11) Uani 0.742(6) 1 d . . P C 1
H72A H 0.778208 0.248296 0.361527 0.036 Uiso 0.742(6) 1 calc R U P C 1
H72B H 0.653558 0.233128 0.392394 0.036 Uiso 0.742(6) 1 calc R U P C 1
C73A C 0.6119(5) 0.29281(17) 0.31081(19) 0.0312(10) Uani 0.742(6) 1 d . . P C 1
H73A H 0.520567 0.292709 0.314178 0.037 Uiso 0.742(6) 1 calc R U P C 1
H73B H 0.651034 0.329732 0.328430 0.037 Uiso 0.742(6) 1 calc R U P C 1
C73B C 0.6937(15) 0.2945(5) 0.3125(6) 0.0312(10) Uani 0.258(6) 1 d . . P C 2
H73C H 0.788060 0.290774 0.320229 0.037 Uiso 0.258(6) 1 calc R U P C 2
H73D H 0.670154 0.332156 0.329159 0.037 Uiso 0.258(6) 1 calc R U P C 2
C72B C 0.6293(16) 0.2432(8) 0.3428(9) 0.0296(11) Uani 0.258(6) 1 d . . P C 2
H72C H 0.671613 0.235873 0.390672 0.036 Uiso 0.258(6) 1 calc R U P C 2
H72D H 0.536995 0.250590 0.340424 0.036 Uiso 0.258(6) 1 calc R U P C 2
O4 O 0.0836(3) 0.10287(12) 0.97125(14) 0.0704(8) Uani 1 1 d . . . . .
C91 C 0.1519(4) 0.0336(2) 1.0615(2) 0.0733(12) Uani 1 1 d . . . . .
H91A H 0.163471 0.064843 1.094910 0.110 Uiso 1 1 calc R U . . .
H91B H 0.214312 0.003233 1.077411 0.110 Uiso 1 1 calc R U . . .
H91C H 0.064966 0.018147 1.056121 0.110 Uiso 1 1 calc R U . . .
C93 C 0.1126(4) 0.1321(2) 0.9128(2) 0.0772(13) Uani 1 1 d . . . . .
H93A H 0.108269 0.105094 0.874369 0.093 Uiso 1 1 calc R U . . .
H93B H 0.199650 0.148874 0.924018 0.093 Uiso 1 1 calc R U . . .
C92 C 0.1723(4) 0.0567(2) 0.9925(2) 0.0712(12) Uani 1 1 d . . . . .
H92A H 0.261343 0.070711 0.997031 0.085 Uiso 1 1 calc R U . . .
H92B H 0.157841 0.025723 0.958059 0.085 Uiso 1 1 calc R U . . .
C94 C 0.0108(6) 0.1798(2) 0.8940(3) 0.0972(17) Uani 1 1 d . . . . .
H94A H -0.074901 0.162702 0.884483 0.146 Uiso 1 1 calc R U . . .
H94B H 0.024983 0.200256 0.853475 0.146 Uiso 1 1 calc R U . . .
H94C H 0.017918 0.206817 0.931982 0.146 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
V1 O2 1.9287(16) . ?
V1 O1 1.9368(16) . ?
V1 O3 2.1806(16) . ?
V1 C81 2.192(2) . ?
V1 N2 2.2307(19) . ?
V1 N1 2.2590(19) . ?
O1 C11 1.337(3) . ?
O2 C21 1.343(3) . ?
O3 C74 1.448(3) . ?
O3 C71 1.450(3) . ?
N1 C1 1.484(3) . ?
N1 C27 1.487(3) . ?
N1 C17 1.495(3) . ?
N2 C3 1.476(3) . ?
N2 C4 1.477(3) . ?
N2 C2 1.492(3) . ?
C81 C82 1.445(3) . ?
C81 H81A 0.9700 . ?
C81 H81B 0.9700 . ?
C13 C14 1.389(3) . ?
C13 C12 1.398(3) . ?
C13 H13 0.9300 . ?
C12 C11 1.418(3) . ?
C12 C31 1.541(3) . ?
C22 C23 1.401(3) . ?
C22 C21 1.416(3) . ?
C22 C51 1.544(3) . ?
C11 C16 1.412(3) . ?
C31 C34 1.532(3) . ?
C31 C33 1.537(3) . ?
C31 C32 1.538(4) . ?
C51 C54 1.531(4) . ?
C51 C52 1.535(4) . ?
C51 C53 1.537(4) . ?
C21 C26 1.410(3) . ?
C3 H3A 0.9600 . ?
C3 H3B 0.9600 . ?
C3 H3C 0.9600 . ?
C15 C16 1.386(3) . ?
C15 C14 1.388(3) . ?
C15 H15 0.9300 . ?
C4 H4A 0.9600 . ?
C4 H4B 0.9600 . ?
C4 H4C 0.9600 . ?
C25 C26 1.384(3) . ?
C25 C24 1.392(3) . ?
C25 H25 0.9300 . ?
C16 C17 1.502(3) . ?
C26 C27 1.506(3) . ?
C14 C41 1.538(3) . ?
C23 C24 1.388(3) . ?
C23 H23 0.9300 . ?
C54 H54A 0.9600 . ?
C54 H54B 0.9600 . ?
C54 H54C 0.9600 . ?
C27 H27A 0.9700 . ?
C27 H27B 0.9700 . ?
C24 C61 1.535(3) . ?
C61 C64 1.528(4) . ?
C61 C62 1.531(4) . ?
C61 C63 1.537(4) . ?
C1 C2 1.504(3) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C33 H33A 0.9600 . ?
C33 H33B 0.9600 . ?
C33 H33C 0.9600 . ?
C53 H53A 0.9600 . ?
C53 H53B 0.9600 . ?
C53 H53C 0.9600 . ?
C82 C87 1.396(4) . ?
C82 C83 1.402(4) . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C34 H34A 0.9600 . ?
C34 H34B 0.9600 . ?
C34 H34C 0.9600 . ?
C41 C42 1.528(4) . ?
C41 C44 1.532(4) . ?
C41 C43 1.533(4) . ?
C43 H43A 0.9600 . ?
C43 H43B 0.9600 . ?
C43 H43C 0.9600 . ?
C52 H52A 0.9600 . ?
C52 H52B 0.9600 . ?
C52 H52C 0.9600 . ?
C62 H62A 0.9600 . ?
C62 H62B 0.9600 . ?
C62 H62C 0.9600 . ?
C63 H63A 0.9600 . ?
C63 H63B 0.9600 . ?
C63 H63C 0.9600 . ?
C42 H42A 0.9600 . ?
C42 H42B 0.9600 . ?
C42 H42C 0.9600 . ?
C64 H64A 0.9600 . ?
C64 H64B 0.9600 . ?
C64 H64C 0.9600 . ?
C44 H44A 0.9600 . ?
C44 H44B 0.9600 . ?
C44 H44C 0.9600 . ?
C32 H32A 0.9600 . ?
C32 H32B 0.9600 . ?
C32 H32C 0.9600 . ?
C84 C85 1.371(5) . ?
C84 C83 1.379(4) . ?
C84 H84 0.9300 . ?
C83 H83 0.9300 . ?
C86 C85 1.380(5) . ?
C86 C87 1.402(5) . ?
C86 H86 0.9300 . ?
C87 H87 0.9300 . ?
C85 H85 0.9300 . ?
C71 C72B 1.498(19) . ?
C71 C72A 1.517(6) . ?
C71 H71A 0.9700 . ?
C71 H71B 0.9700 . ?
C74 C73A 1.510(4) . ?
C74 C73B 1.533(12) . ?
C74 H74A 0.9700 . ?
C74 H74B 0.9700 . ?
C72A C73A 1.519(7) . ?
C72A H72A 0.9700 . ?
C72A H72B 0.9700 . ?
C73A H73A 0.9700 . ?
C73A H73B 0.9700 . ?
C73B C72B 1.53(2) . ?
C73B H73C 0.9700 . ?
C73B H73D 0.9700 . ?
C72B H72C 0.9700 . ?
C72B H72D 0.9700 . ?
O4 C92 1.410(5) . ?
O4 C93 1.414(5) . ?
C91 C92 1.512(6) . ?
C91 H91A 0.9600 . ?
C91 H91B 0.9600 . ?
C91 H91C 0.9600 . ?
C93 C94 1.515(6) . ?
C93 H93A 0.9700 . ?
C93 H93B 0.9700 . ?
C92 H92A 0.9700 . ?
C92 H92B 0.9700 . ?
C94 H94A 0.9600 . ?
C94 H94B 0.9600 . ?
C94 H94C 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
O2 V1 O1 165.36(7) . . ?
O2 V1 O3 83.59(6) . . ?
O1 V1 O3 84.25(6) . . ?
O2 V1 C81 95.08(7) . . ?
O1 V1 C81 94.22(7) . . ?
O3 V1 C81 95.70(7) . . ?
O2 V1 N2 93.66(7) . . ?
O1 V1 N2 97.14(7) . . ?
O3 V1 N2 171.21(7) . . ?
C81 V1 N2 92.86(8) . . ?
O2 V1 N1 87.28(7) . . ?
O1 V1 N1 85.08(7) . . ?
O3 V1 N1 92.28(7) . . ?
C81 V1 N1 171.87(8) . . ?
N2 V1 N1 79.22(7) . . ?
C11 O1 V1 138.68(14) . . ?
C21 O2 V1 136.97(14) . . ?
C74 O3 C71 108.41(18) . . ?
C74 O3 V1 124.05(14) . . ?
C71 O3 V1 125.59(14) . . ?
C1 N1 C27 111.47(18) . . ?
C1 N1 C17 109.91(18) . . ?
C27 N1 C17 104.79(17) . . ?
C1 N1 V1 109.29(14) . . ?
C27 N1 V1 110.53(14) . . ?
C17 N1 V1 110.80(13) . . ?
C3 N2 C4 107.68(19) . . ?
C3 N2 C2 109.68(19) . . ?
C4 N2 C2 107.27(18) . . ?
C3 N2 V1 111.31(14) . . ?
C4 N2 V1 113.63(15) . . ?
C2 N2 V1 107.16(14) . . ?
C82 C81 V1 118.59(15) . . ?
C82 C81 H81A 107.7 . . ?
V1 C81 H81A 107.7 . . ?
C82 C81 H81B 107.7 . . ?
V1 C81 H81B 107.7 . . ?
H81A C81 H81B 107.1 . . ?
C14 C13 C12 124.4(2) . . ?
C14 C13 H13 117.8 . . ?
C12 C13 H13 117.8 . . ?
C13 C12 C11 118.1(2) . . ?
C13 C12 C31 119.9(2) . . ?
C11 C12 C31 121.8(2) . . ?
C23 C22 C21 117.6(2) . . ?
C23 C22 C51 120.1(2) . . ?
C21 C22 C51 122.2(2) . . ?
O1 C11 C16 118.9(2) . . ?
O1 C11 C12 123.0(2) . . ?
C16 C11 C12 118.0(2) . . ?
C34 C31 C33 107.7(2) . . ?
C34 C31 C32 106.8(2) . . ?
C33 C31 C32 109.9(2) . . ?
C34 C31 C12 112.8(2) . . ?
C33 C31 C12 108.68(19) . . ?
C32 C31 C12 110.92(19) . . ?
C54 C51 C52 107.6(2) . . ?
C54 C51 C53 107.2(2) . . ?
C52 C51 C53 109.1(2) . . ?
C54 C51 C22 112.6(2) . . ?
C52 C51 C22 109.1(2) . . ?
C53 C51 C22 111.1(2) . . ?
O2 C21 C26 118.5(2) . . ?
O2 C21 C22 123.0(2) . . ?
C26 C21 C22 118.5(2) . . ?
N2 C3 H3A 109.5 . . ?
N2 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
N2 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
C16 C15 C14 122.0(2) . . ?
C16 C15 H15 119.0 . . ?
C14 C15 H15 119.0 . . ?
N2 C4 H4A 109.5 . . ?
N2 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
N2 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C26 C25 C24 121.7(2) . . ?
C26 C25 H25 119.2 . . ?
C24 C25 H25 119.2 . . ?
C15 C16 C11 121.2(2) . . ?
C15 C16 C17 118.6(2) . . ?
C11 C16 C17 120.0(2) . . ?
C25 C26 C21 121.1(2) . . ?
C25 C26 C27 118.9(2) . . ?
C21 C26 C27 119.4(2) . . ?
C15 C14 C13 116.3(2) . . ?
C15 C14 C41 120.2(2) . . ?
C13 C14 C41 123.5(2) . . ?
C24 C23 C22 124.4(2) . . ?
C24 C23 H23 117.8 . . ?
C22 C23 H23 117.8 . . ?
C51 C54 H54A 109.5 . . ?
C51 C54 H54B 109.5 . . ?
H54A C54 H54B 109.5 . . ?
C51 C54 H54C 109.5 . . ?
H54A C54 H54C 109.5 . . ?
H54B C54 H54C 109.5 . . ?
N1 C27 C26 117.73(19) . . ?
N1 C27 H27A 107.9 . . ?
C26 C27 H27A 107.9 . . ?
N1 C27 H27B 107.9 . . ?
C26 C27 H27B 107.9 . . ?
H27A C27 H27B 107.2 . . ?
C23 C24 C25 116.5(2) . . ?
C23 C24 C61 123.2(2) . . ?
C25 C24 C61 120.3(2) . . ?
C64 C61 C62 108.1(2) . . ?
C64 C61 C24 110.0(2) . . ?
C62 C61 C24 111.8(2) . . ?
C64 C61 C63 108.9(2) . . ?
C62 C61 C63 108.4(2) . . ?
C24 C61 C63 109.5(2) . . ?
N1 C1 C2 110.68(19) . . ?
N1 C1 H1A 109.5 . . ?
C2 C1 H1A 109.5 . . ?
N1 C1 H1B 109.5 . . ?
C2 C1 H1B 109.5 . . ?
H1A C1 H1B 108.1 . . ?
C31 C33 H33A 109.5 . . ?
C31 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
C31 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C51 C53 H53A 109.5 . . ?
C51 C53 H53B 109.5 . . ?
H53A C53 H53B 109.5 . . ?
C51 C53 H53C 109.5 . . ?
H53A C53 H53C 109.5 . . ?
H53B C53 H53C 109.5 . . ?
C87 C82 C83 116.2(3) . . ?
C87 C82 C81 122.9(3) . . ?
C83 C82 C81 120.9(3) . . ?
N1 C17 C16 115.57(19) . . ?
N1 C17 H17A 108.4 . . ?
C16 C17 H17A 108.4 . . ?
N1 C17 H17B 108.4 . . ?
C16 C17 H17B 108.4 . . ?
H17A C17 H17B 107.4 . . ?
N2 C2 C1 111.29(19) . . ?
N2 C2 H2A 109.4 . . ?
C1 C2 H2A 109.4 . . ?
N2 C2 H2B 109.4 . . ?
C1 C2 H2B 109.4 . . ?
H2A C2 H2B 108.0 . . ?
C31 C34 H34A 109.5 . . ?
C31 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
C31 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C42 C41 C44 108.2(2) . . ?
C42 C41 C43 108.1(2) . . ?
C44 C41 C43 108.8(2) . . ?
C42 C41 C14 112.4(2) . . ?
C44 C41 C14 109.4(2) . . ?
C43 C41 C14 109.8(2) . . ?
C41 C43 H43A 109.5 . . ?
C41 C43 H43B 109.5 . . ?
H43A C43 H43B 109.5 . . ?
C41 C43 H43C 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
C51 C52 H52A 109.5 . . ?
C51 C52 H52B 109.5 . . ?
H52A C52 H52B 109.5 . . ?
C51 C52 H52C 109.5 . . ?
H52A C52 H52C 109.5 . . ?
H52B C52 H52C 109.5 . . ?
C61 C62 H62A 109.5 . . ?
C61 C62 H62B 109.5 . . ?
H62A C62 H62B 109.5 . . ?
C61 C62 H62C 109.5 . . ?
H62A C62 H62C 109.5 . . ?
H62B C62 H62C 109.5 . . ?
C61 C63 H63A 109.5 . . ?
C61 C63 H63B 109.5 . . ?
H63A C63 H63B 109.5 . . ?
C61 C63 H63C 109.5 . . ?
H63A C63 H63C 109.5 . . ?
H63B C63 H63C 109.5 . . ?
C41 C42 H42A 109.5 . . ?
C41 C42 H42B 109.5 . . ?
H42A C42 H42B 109.5 . . ?
C41 C42 H42C 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
C61 C64 H64A 109.5 . . ?
C61 C64 H64B 109.5 . . ?
H64A C64 H64B 109.5 . . ?
C61 C64 H64C 109.5 . . ?
H64A C64 H64C 109.5 . . ?
H64B C64 H64C 109.5 . . ?
C41 C44 H44A 109.5 . . ?
C41 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
C41 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C85 C84 C83 120.4(3) . . ?
C85 C84 H84 119.8 . . ?
C83 C84 H84 119.8 . . ?
C84 C83 C82 122.3(3) . . ?
C84 C83 H83 118.8 . . ?
C82 C83 H83 118.8 . . ?
C85 C86 C87 120.2(3) . . ?
C85 C86 H86 119.9 . . ?
C87 C86 H86 119.9 . . ?
C82 C87 C86 121.4(3) . . ?
C82 C87 H87 119.3 . . ?
C86 C87 H87 119.3 . . ?
C84 C85 C86 119.4(3) . . ?
C84 C85 H85 120.3 . . ?
C86 C85 H85 120.3 . . ?
O3 C71 C72B 103.7(7) . . ?
O3 C71 C72A 105.4(3) . . ?
O3 C71 H71A 110.7 . . ?
C72A C71 H71A 110.7 . . ?
O3 C71 H71B 110.7 . . ?
C72A C71 H71B 110.7 . . ?
H71A C71 H71B 108.8 . . ?
O3 C74 C73A 106.5(2) . . ?
O3 C74 C73B 102.3(5) . . ?
O3 C74 H74A 110.4 . . ?
C73A C74 H74A 110.4 . . ?
O3 C74 H74B 110.4 . . ?
C73A C74 H74B 110.4 . . ?
H74A C74 H74B 108.6 . . ?
C71 C72A C73A 100.6(3) . . ?
C71 C72A H72A 111.7 . . ?
C73A C72A H72A 111.7 . . ?
C71 C72A H72B 111.7 . . ?
C73A C72A H72B 111.7 . . ?
H72A C72A H72B 109.4 . . ?
C74 C73A C72A 103.6(3) . . ?
C74 C73A H73A 111.0 . . ?
C72A C73A H73A 111.0 . . ?
C74 C73A H73B 111.0 . . ?
C72A C73A H73B 111.0 . . ?
H73A C73A H73B 109.0 . . ?
C72B C73B C74 95.3(10) . . ?
C72B C73B H73C 112.7 . . ?
C74 C73B H73C 112.7 . . ?
C72B C73B H73D 112.7 . . ?
C74 C73B H73D 112.7 . . ?
H73C C73B H73D 110.2 . . ?
C71 C72B C73B 103.1(12) . . ?
C71 C72B H72C 111.2 . . ?
C73B C72B H72C 111.2 . . ?
C71 C72B H72D 111.2 . . ?
C73B C72B H72D 111.2 . . ?
H72C C72B H72D 109.1 . . ?
C92 O4 C93 110.9(3) . . ?
C92 C91 H91A 109.5 . . ?
C92 C91 H91B 109.5 . . ?
H91A C91 H91B 109.5 . . ?
C92 C91 H91C 109.5 . . ?
H91A C91 H91C 109.5 . . ?
H91B C91 H91C 109.5 . . ?
O4 C93 C94 106.4(3) . . ?
O4 C93 H93A 110.4 . . ?
C94 C93 H93A 110.4 . . ?
O4 C93 H93B 110.4 . . ?
C94 C93 H93B 110.4 . . ?
H93A C93 H93B 108.6 . . ?
O4 C92 C91 108.8(3) . . ?
O4 C92 H92A 109.9 . . ?
C91 C92 H92A 109.9 . . ?
O4 C92 H92B 109.9 . . ?
C91 C92 H92B 109.9 . . ?
H92A C92 H92B 108.3 . . ?
C93 C94 H94A 109.5 . . ?
C93 C94 H94B 109.5 . . ?
H94A C94 H94B 109.5 . . ?
C93 C94 H94C 109.5 . . ?
H94A C94 H94C 109.5 . . ?
H94B C94 H94C 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
C14 C13 C12 C11 1.0(4) . . . . ?
C14 C13 C12 C31 -174.4(2) . . . . ?
V1 O1 C11 C16 27.1(3) . . . . ?
V1 O1 C11 C12 -155.70(17) . . . . ?
C13 C12 C11 O1 -179.7(2) . . . . ?
C31 C12 C11 O1 -4.3(3) . . . . ?
C13 C12 C11 C16 -2.4(3) . . . . ?
C31 C12 C11 C16 172.9(2) . . . . ?
C13 C12 C31 C34 -7.5(3) . . . . ?
C11 C12 C31 C34 177.3(2) . . . . ?
C13 C12 C31 C33 111.9(2) . . . . ?
C11 C12 C31 C33 -63.4(3) . . . . ?
C13 C12 C31 C32 -127.2(2) . . . . ?
C11 C12 C31 C32 57.6(3) . . . . ?
C23 C22 C51 C54 3.6(3) . . . . ?
C21 C22 C51 C54 -180.0(2) . . . . ?
C23 C22 C51 C52 -115.8(2) . . . . ?
C21 C22 C51 C52 60.6(3) . . . . ?
C23 C22 C51 C53 123.9(2) . . . . ?
C21 C22 C51 C53 -59.7(3) . . . . ?
V1 O2 C21 C26 -28.5(3) . . . . ?
V1 O2 C21 C22 154.21(18) . . . . ?
C23 C22 C21 O2 -177.9(2) . . . . ?
C51 C22 C21 O2 5.6(3) . . . . ?
C23 C22 C21 C26 4.8(3) . . . . ?
C51 C22 C21 C26 -171.7(2) . . . . ?
C14 C15 C16 C11 -1.4(4) . . . . ?
C14 C15 C16 C17 172.7(2) . . . . ?
O1 C11 C16 C15 180.0(2) . . . . ?
C12 C11 C16 C15 2.6(3) . . . . ?
O1 C11 C16 C17 6.0(3) . . . . ?
C12 C11 C16 C17 -171.4(2) . . . . ?
C24 C25 C26 C21 3.2(4) . . . . ?
C24 C25 C26 C27 -168.0(2) . . . . ?
O2 C21 C26 C25 176.3(2) . . . . ?
C22 C21 C26 C25 -6.2(3) . . . . ?
O2 C21 C26 C27 -12.5(3) . . . . ?
C22 C21 C26 C27 164.9(2) . . . . ?
C16 C15 C14 C13 -0.1(4) . . . . ?
C16 C15 C14 C41 -177.6(2) . . . . ?
C12 C13 C14 C15 0.3(4) . . . . ?
C12 C13 C14 C41 177.6(2) . . . . ?
C21 C22 C23 C24 -0.4(4) . . . . ?
C51 C22 C23 C24 176.2(2) . . . . ?
C1 N1 C27 C26 63.9(3) . . . . ?
C17 N1 C27 C26 -177.3(2) . . . . ?
V1 N1 C27 C26 -57.9(2) . . . . ?
C25 C26 C27 N1 -129.6(2) . . . . ?
C21 C26 C27 N1 59.0(3) . . . . ?
C22 C23 C24 C25 -2.7(4) . . . . ?
C22 C23 C24 C61 179.6(2) . . . . ?
C26 C25 C24 C23 1.3(3) . . . . ?
C26 C25 C24 C61 179.1(2) . . . . ?
C23 C24 C61 C64 -119.5(3) . . . . ?
C25 C24 C61 C64 62.9(3) . . . . ?
C23 C24 C61 C62 0.7(3) . . . . ?
C25 C24 C61 C62 -177.0(2) . . . . ?
C23 C24 C61 C63 120.8(3) . . . . ?
C25 C24 C61 C63 -56.8(3) . . . . ?
C27 N1 C1 C2 -88.6(2) . . . . ?
C17 N1 C1 C2 155.67(19) . . . . ?
V1 N1 C1 C2 33.9(2) . . . . ?
V1 C81 C82 C87 88.1(3) . . . . ?
V1 C81 C82 C83 -89.2(3) . . . . ?
C1 N1 C17 C16 -57.3(3) . . . . ?
C27 N1 C17 C16 -177.21(19) . . . . ?
V1 N1 C17 C16 63.6(2) . . . . ?
C15 C16 C17 N1 131.9(2) . . . . ?
C11 C16 C17 N1 -54.0(3) . . . . ?
C3 N2 C2 C1 -76.4(2) . . . . ?
C4 N2 C2 C1 166.9(2) . . . . ?
V1 N2 C2 C1 44.5(2) . . . . ?
N1 C1 C2 N2 -54.0(3) . . . . ?
C15 C14 C41 C42 -179.6(2) . . . . ?
C13 C14 C41 C42 3.1(4) . . . . ?
C15 C14 C41 C44 -59.3(3) . . . . ?
C13 C14 C41 C44 123.4(3) . . . . ?
C15 C14 C41 C43 60.1(3) . . . . ?
C13 C14 C41 C43 -117.2(3) . . . . ?
C85 C84 C83 C82 0.7(5) . . . . ?
C87 C82 C83 C84 -2.8(4) . . . . ?
C81 C82 C83 C84 174.6(3) . . . . ?
C83 C82 C87 C86 2.8(4) . . . . ?
C81 C82 C87 C86 -174.6(3) . . . . ?
C85 C86 C87 C82 -0.8(5) . . . . ?
C83 C84 C85 C86 1.5(5) . . . . ?
C87 C86 C85 C84 -1.4(5) . . . . ?
C74 O3 C71 C72B -0.6(7) . . . . ?
V1 O3 C71 C72B -165.2(6) . . . . ?
C74 O3 C71 C72A -23.0(3) . . . . ?
V1 O3 C71 C72A 172.4(2) . . . . ?
C71 O3 C74 C73A -1.2(3) . . . . ?
V1 O3 C74 C73A 163.6(2) . . . . ?
C71 O3 C74 C73B 32.0(6) . . . . ?
V1 O3 C74 C73B -163.2(6) . . . . ?
O3 C71 C72A C73A 37.2(4) . . . . ?
O3 C74 C73A C72A 24.7(4) . . . . ?
C71 C72A C73A C74 -37.2(5) . . . . ?
O3 C74 C73B C72B -48.2(10) . . . . ?
O3 C71 C72B C73B -31.1(11) . . . . ?
C74 C73B C72B C71 48.1(12) . . . . ?
C92 O4 C93 C94 179.2(4) . . . . ?
C93 O4 C92 C91 170.6(4) . . . . ?

_refine_diff_density_max         0.491
_refine_diff_density_min         -0.514
_refine_diff_density_rms         0.058

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_2
_database_code_depnum_ccdc_archive 'CCDC 1536781'
_audit_update_record             
;
2017-06-28 deposited with the CCDC.
2017-06-30 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         'C37 H58 Cl N2 O2 V, C4 H10 O'
_chemical_formula_sum            'C41 H68 Cl N2 O3 V'
_chemical_properties_physical    
'air-sensitive, moisture-sensitive, paramagnetic'
_exptl_crystal_recrystallization_method EtO2
_chemical_melting_point          ?

_exptl_crystal_description       plate
_exptl_crystal_colour            green
_diffrn_ambient_temperature      150(2)
_chemical_formula_weight         723.36

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'
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      monoclinic
_space_group_IT_number           4
_space_group_name_H-M_alt        'P 21'
_space_group_name_Hall           'P 2yb'
_chemical_absolute_configuration .

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

_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.
;

_cell_length_a                   14.3330(8)
_cell_length_b                   8.3560(4)
_cell_length_c                   17.3390(9)
_cell_angle_alpha                90
_cell_angle_beta                 100.892(3)
_cell_angle_gamma                90
_cell_volume                     2039.22(18)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    10777
_cell_measurement_theta_min      2.88
_cell_measurement_theta_max      27.90
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.178
_exptl_crystal_F_000             784
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.040
_exptl_absorpt_coefficient_mu    0.346
_shelx_estimated_absorpt_T_min   0.874
_shelx_estimated_absorpt_T_max   0.986
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9033
_exptl_absorpt_correction_T_max  0.9871
_exptl_absorpt_process_details   'SADABS,  G. M. Sheldrick, 1996'
_exptl_absorpt_special_details   ?
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            22024
_diffrn_reflns_av_unetI/netI     0.0715
_diffrn_reflns_av_R_equivalents  0.0417
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         2.392
_diffrn_reflns_theta_max         29.075
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.966
_diffrn_reflns_point_group_measured_fraction_full 0.991
_reflns_number_total             10555
_reflns_number_gt                8284
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.819
_reflns_Friedel_fraction_max     0.931
_reflns_Friedel_fraction_full    0.983

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Sir2004 (M.C. Burla et al, 2005)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    
'Ortep3 for Windows v2.0 (L.J. Farrugia, J. Appl. Cryst. (1997) 30, 565)'
_computing_publication_material  'enCIFer v1.6'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0499P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 3067 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.011(11)
_refine_ls_number_reflns         10555
_refine_ls_number_parameters     433
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0680
_refine_ls_R_factor_gt           0.0441
_refine_ls_wR_factor_ref         0.1011
_refine_ls_wR_factor_gt          0.0949
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_restrained_S_all      1.001
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
V1 V 0.63191(3) 0.44040(6) 0.32615(3) 0.01562(11) Uani 1 1 d . . . . .
Cl1 Cl 0.62883(6) 0.19670(10) 0.39462(5) 0.02790(19) Uani 1 1 d . . . . .
O1 O 0.50594(13) 0.4300(3) 0.27405(11) 0.0211(4) Uani 1 1 d . . . . .
O2 O 0.73728(15) 0.3794(2) 0.28505(13) 0.0204(5) Uani 1 1 d . . . . .
N1 N 0.64333(16) 0.6749(3) 0.27389(14) 0.0166(5) Uani 1 1 d . . . . .
N2 N 0.66627(18) 0.5782(3) 0.43141(16) 0.0213(6) Uani 1 1 d . . . . .
O3 O 0.84708(17) 0.2585(3) 0.63687(15) 0.0318(6) Uani 1 1 d . . . . .
C22 C 0.8931(2) 0.3789(4) 0.25324(17) 0.0177(6) Uani 1 1 d . . . . .
C21 C 0.80318(19) 0.4515(4) 0.25036(16) 0.0181(6) Uani 1 1 d . . . . .
C23 C 0.9553(2) 0.4549(4) 0.21210(16) 0.0203(6) Uani 1 1 d . . . . .
H23 H 1.014078 0.407379 0.212759 0.024 Uiso 1 1 calc R U . . .
C17 C 0.5477(2) 0.7508(4) 0.25137(18) 0.0185(6) Uani 1 1 d . . . . .
H17A H 0.555243 0.857393 0.231304 0.022 Uiso 1 1 calc R U . . .
H17B H 0.519782 0.761526 0.297900 0.022 Uiso 1 1 calc R U . . .
C16 C 0.4809(2) 0.6575(4) 0.19050(18) 0.0178(6) Uani 1 1 d . . . . .
C11 C 0.4574(2) 0.5012(4) 0.20860(18) 0.0180(6) Uani 1 1 d . . . . .
C27 C 0.6843(2) 0.6699(4) 0.20140(17) 0.0197(6) Uani 1 1 d . . . . .
H27A H 0.687660 0.778415 0.182297 0.024 Uiso 1 1 calc R U . . .
H27B H 0.641158 0.610721 0.161629 0.024 Uiso 1 1 calc R U . . .
C12 C 0.3839(2) 0.4196(4) 0.15817(18) 0.0211(7) Uani 1 1 d . . . . .
C26 C 0.7819(2) 0.5953(4) 0.21022(18) 0.0184(6) Uani 1 1 d . . . . .
C54 C 1.0217(2) 0.1681(4) 0.2908(2) 0.0264(7) Uani 1 1 d . . . . .
H54A H 1.065370 0.249473 0.314065 0.040 Uiso 1 1 calc R U . . .
H54B H 1.036608 0.069195 0.318591 0.040 Uiso 1 1 calc R U . . .
H54C H 1.026857 0.153936 0.236793 0.040 Uiso 1 1 calc R U . . .
C13 C 0.3465(2) 0.4934(4) 0.08732(19) 0.0239(7) Uani 1 1 d . . . . .
H13 H 0.298578 0.440222 0.053239 0.029 Uiso 1 1 calc R U . . .
C31 C 0.3470(2) 0.2574(4) 0.1825(2) 0.0251(7) Uani 1 1 d . . . . .
C41 C 0.3363(2) 0.7058(4) -0.01865(19) 0.0286(7) Uani 1 1 d . . . . .
C25 C 0.8475(2) 0.6671(4) 0.17098(17) 0.0200(6) Uani 1 1 d . . . . .
H25 H 0.832352 0.763595 0.144913 0.024 Uiso 1 1 calc R U . . .
C24 C 0.9355(2) 0.5964(4) 0.17025(19) 0.0201(6) Uani 1 1 d . . . . .
C61 C 1.0047(2) 0.6714(4) 0.12279(19) 0.0247(7) Uani 1 1 d . . . . .
C33 C 0.4262(2) 0.1314(4) 0.1941(2) 0.0317(8) Uani 1 1 d . . . . .
H33A H 0.449340 0.118290 0.146047 0.048 Uiso 1 1 calc R U . . .
H33B H 0.477170 0.165669 0.234910 0.048 Uiso 1 1 calc R U . . .
H33C H 0.401536 0.031249 0.208646 0.048 Uiso 1 1 calc R U . . .
C1 C 0.7033(2) 0.7733(4) 0.33542(18) 0.0205(6) Uani 1 1 d . . . . .
H1A H 0.698220 0.885011 0.319939 0.025 Uiso 1 1 calc R U . . .
H1B H 0.769164 0.741402 0.340222 0.025 Uiso 1 1 calc R U . . .
C15 C 0.4418(2) 0.7245(4) 0.11807(18) 0.0198(6) Uani 1 1 d . . . . .
H15 H 0.460233 0.826688 0.105890 0.024 Uiso 1 1 calc R U . . .
C2 C 0.6732(2) 0.7543(4) 0.41444(19) 0.0221(7) Uani 1 1 d . . . . .
H2 H 0.611802 0.806553 0.413526 0.027 Uiso 1 1 calc R U . . .
C14 C 0.3758(2) 0.6416(4) 0.06375(19) 0.0229(7) Uani 1 1 d . . . . .
C51 C 0.9195(2) 0.2188(4) 0.29543(19) 0.0215(7) Uani 1 1 d . . . . .
C3 C 0.7492(3) 0.8242(5) 0.4817(2) 0.0341(9) Uani 1 1 d . . . . .
H3A H 0.793310 0.892159 0.460725 0.041 Uiso 1 1 calc R U . . .
H3B H 0.719491 0.886519 0.517597 0.041 Uiso 1 1 calc R U . . .
C5 C 0.7660(2) 0.5358(4) 0.4713(2) 0.0274(8) Uani 1 1 d . . . . .
H5A H 0.806190 0.519212 0.432823 0.033 Uiso 1 1 calc R U . . .
H5B H 0.766205 0.439096 0.502261 0.033 Uiso 1 1 calc R U . . .
C53 C 0.8519(2) 0.0874(4) 0.2581(2) 0.0274(8) Uani 1 1 d . . . . .
H53A H 0.869051 -0.011922 0.284841 0.041 Uiso 1 1 calc R U . . .
H53B H 0.788042 0.115139 0.262145 0.041 Uiso 1 1 calc R U . . .
H53C H 0.856163 0.076357 0.203739 0.041 Uiso 1 1 calc R U . . .
C4 C 0.8009(2) 0.6774(5) 0.5237(2) 0.0333(8) Uani 1 1 d . . . . .
H4A H 0.869196 0.689218 0.529528 0.040 Uiso 1 1 calc R U . . .
H4B H 0.785117 0.663865 0.575294 0.040 Uiso 1 1 calc R U . . .
C7 C 0.4975(3) 0.5681(6) 0.4530(2) 0.0434(10) Uani 1 1 d . . . . .
H7A H 0.460010 0.548385 0.492427 0.065 Uiso 1 1 calc R U . . .
H7B H 0.485958 0.674916 0.433135 0.065 Uiso 1 1 calc R U . . .
H7C H 0.480553 0.492860 0.410898 0.065 Uiso 1 1 calc R U . . .
C73 C 0.9014(2) 0.1555(4) 0.5979(2) 0.0308(8) Uani 1 1 d . . . . .
H73A H 0.871040 0.144494 0.543257 0.037 Uiso 1 1 calc R U . . .
H73B H 0.905283 0.050272 0.621964 0.037 Uiso 1 1 calc R U . . .
C34 C 0.2652(3) 0.1917(5) 0.1193(2) 0.0370(9) Uani 1 1 d . . . . .
H34A H 0.287273 0.177538 0.070787 0.056 Uiso 1 1 calc R U . . .
H34B H 0.244288 0.090722 0.136229 0.056 Uiso 1 1 calc R U . . .
H34C H 0.213207 0.266116 0.111540 0.056 Uiso 1 1 calc R U . . .
C72 C 0.7565(3) 0.1955(5) 0.6403(2) 0.0359(8) Uani 1 1 d . . . . .
H72A H 0.763172 0.089007 0.662933 0.043 Uiso 1 1 calc R U . . .
H72B H 0.718856 0.187747 0.587756 0.043 Uiso 1 1 calc R U . . .
C6 C 0.6008(3) 0.5496(5) 0.4885(2) 0.0313(8) Uani 1 1 d . . . . .
H6A H 0.611431 0.442314 0.509636 0.038 Uiso 1 1 calc R U . . .
H6B H 0.616830 0.624202 0.531852 0.038 Uiso 1 1 calc R U . . .
C52 C 0.9146(3) 0.2342(4) 0.38317(19) 0.0309(8) Uani 1 1 d . . . . .
H52A H 0.957207 0.316943 0.406564 0.046 Uiso 1 1 calc R U . . .
H52B H 0.850944 0.260819 0.388371 0.046 Uiso 1 1 calc R U . . .
H52C H 0.932660 0.134442 0.409224 0.046 Uiso 1 1 calc R U . . .
C32 C 0.3097(3) 0.2788(5) 0.2591(2) 0.0342(9) Uani 1 1 d . . . . .
H32A H 0.260174 0.357750 0.251585 0.051 Uiso 1 1 calc R U . . .
H32B H 0.284992 0.178789 0.273643 0.051 Uiso 1 1 calc R U . . .
H32C H 0.360626 0.313209 0.299907 0.051 Uiso 1 1 calc R U . . .
C74 C 0.9993(3) 0.2229(5) 0.6032(2) 0.0413(10) Uani 1 1 d . . . . .
H74A H 1.036027 0.152813 0.576762 0.062 Uiso 1 1 calc R U . . .
H74B H 0.995199 0.326471 0.578887 0.062 Uiso 1 1 calc R U . . .
H74C H 1.029355 0.232487 0.657396 0.062 Uiso 1 1 calc R U . . .
C43 C 0.2319(3) 0.7460(6) -0.0277(2) 0.0482(11) Uani 1 1 d . . . . .
H43A H 0.208789 0.785892 -0.079758 0.072 Uiso 1 1 calc R U . . .
H43B H 0.197108 0.651461 -0.019233 0.072 Uiso 1 1 calc R U . . .
H43C H 0.223442 0.826119 0.010036 0.072 Uiso 1 1 calc R U . . .
C63 C 1.0280(3) 0.8439(5) 0.1506(3) 0.0455(11) Uani 1 1 d . . . . .
H63A H 1.055156 0.843702 0.205617 0.068 Uiso 1 1 calc R U . . .
H63B H 1.072478 0.889323 0.121758 0.068 Uiso 1 1 calc R U . . .
H63C H 0.970768 0.906504 0.141780 0.068 Uiso 1 1 calc R U . . .
C42 C 0.3505(3) 0.5780(5) -0.0799(2) 0.0406(10) Uani 1 1 d . . . . .
H42A H 0.416797 0.552872 -0.073916 0.061 Uiso 1 1 calc R U . . .
H42B H 0.315748 0.483089 -0.071945 0.061 Uiso 1 1 calc R U . . .
H42C H 0.327661 0.618738 -0.131790 0.061 Uiso 1 1 calc R U . . .
C64 C 1.1001(3) 0.5810(6) 0.1361(3) 0.0521(12) Uani 1 1 d . . . . .
H64A H 1.127809 0.582149 0.191064 0.078 Uiso 1 1 calc R U . . .
H64B H 1.089521 0.472375 0.118676 0.078 Uiso 1 1 calc R U . . .
H64C H 1.142420 0.632220 0.107024 0.078 Uiso 1 1 calc R U . . .
C62 C 0.9622(3) 0.6689(7) 0.0369(2) 0.0559(13) Uani 1 1 d . . . . .
H62A H 0.948021 0.560503 0.020398 0.084 Uiso 1 1 calc R U . . .
H62B H 0.904726 0.730870 0.027723 0.084 Uiso 1 1 calc R U . . .
H62C H 1.006437 0.713689 0.007702 0.084 Uiso 1 1 calc R U . . .
C44 C 0.3915(4) 0.8559(6) -0.0373(3) 0.0587(14) Uani 1 1 d . . . . .
H44A H 0.457750 0.830511 -0.031515 0.088 Uiso 1 1 calc R U . . .
H44B H 0.367483 0.889849 -0.090199 0.088 Uiso 1 1 calc R U . . .
H44C H 0.383401 0.940492 -0.001620 0.088 Uiso 1 1 calc R U . . .
C71 C 0.7078(3) 0.3023(7) 0.6894(3) 0.0524(12) Uani 1 1 d . . . . .
H71A H 0.646249 0.259388 0.691741 0.079 Uiso 1 1 calc R U . . .
H71B H 0.745017 0.308742 0.741533 0.079 Uiso 1 1 calc R U . . .
H71C H 0.700816 0.407226 0.666551 0.079 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
V1 O2 1.859(2) . ?
V1 O1 1.8620(19) . ?
V1 N2 2.135(3) . ?
V1 N1 2.178(3) . ?
V1 Cl1 2.3618(9) . ?
O1 C11 1.352(4) . ?
O2 C21 1.354(4) . ?
N1 C1 1.485(4) . ?
N1 C27 1.485(4) . ?
N1 C17 1.494(4) . ?
N2 C6 1.506(4) . ?
N2 C2 1.508(4) . ?
N2 C5 1.508(4) . ?
O3 C72 1.412(4) . ?
O3 C73 1.415(4) . ?
C22 C23 1.395(4) . ?
C22 C21 1.417(4) . ?
C22 C51 1.538(4) . ?
C21 C26 1.393(4) . ?
C23 C24 1.388(5) . ?
C23 H23 0.9300 . ?
C17 C16 1.502(4) . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C16 C15 1.392(4) . ?
C16 C11 1.399(4) . ?
C11 C12 1.411(4) . ?
C27 C26 1.512(4) . ?
C27 H27A 0.9700 . ?
C27 H27B 0.9700 . ?
C12 C13 1.389(4) . ?
C12 C31 1.542(5) . ?
C26 C25 1.396(4) . ?
C54 C51 1.542(4) . ?
C54 H54A 0.9600 . ?
C54 H54B 0.9600 . ?
C54 H54C 0.9600 . ?
C13 C14 1.394(5) . ?
C13 H13 0.9300 . ?
C31 C32 1.532(5) . ?
C31 C33 1.533(4) . ?
C31 C34 1.547(5) . ?
C41 C43 1.513(5) . ?
C41 C14 1.531(5) . ?
C41 C42 1.546(5) . ?
C41 C44 1.549(5) . ?
C25 C24 1.394(4) . ?
C25 H25 0.9300 . ?
C24 C61 1.538(4) . ?
C61 C62 1.498(5) . ?
C61 C63 1.536(5) . ?
C61 C64 1.540(5) . ?
C33 H33A 0.9600 . ?
C33 H33B 0.9600 . ?
C33 H33C 0.9600 . ?
C1 C2 1.520(4) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C15 C14 1.387(4) . ?
C15 H15 0.9300 . ?
C2 C3 1.551(4) . ?
C2 H2 0.9800 . ?
C51 C53 1.525(4) . ?
C51 C52 1.542(4) . ?
C3 C4 1.543(5) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C5 C4 1.517(5) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C53 H53A 0.9600 . ?
C53 H53B 0.9600 . ?
C53 H53C 0.9600 . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C7 C6 1.500(5) . ?
C7 H7A 0.9600 . ?
C7 H7B 0.9600 . ?
C7 H7C 0.9600 . ?
C73 C74 1.498(5) . ?
C73 H73A 0.9700 . ?
C73 H73B 0.9700 . ?
C34 H34A 0.9600 . ?
C34 H34B 0.9600 . ?
C34 H34C 0.9600 . ?
C72 C71 1.494(6) . ?
C72 H72A 0.9700 . ?
C72 H72B 0.9700 . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C52 H52A 0.9600 . ?
C52 H52B 0.9600 . ?
C52 H52C 0.9600 . ?
C32 H32A 0.9600 . ?
C32 H32B 0.9600 . ?
C32 H32C 0.9600 . ?
C74 H74A 0.9600 . ?
C74 H74B 0.9600 . ?
C74 H74C 0.9600 . ?
C43 H43A 0.9600 . ?
C43 H43B 0.9600 . ?
C43 H43C 0.9600 . ?
C63 H63A 0.9600 . ?
C63 H63B 0.9600 . ?
C63 H63C 0.9600 . ?
C42 H42A 0.9600 . ?
C42 H42B 0.9600 . ?
C42 H42C 0.9600 . ?
C64 H64A 0.9600 . ?
C64 H64B 0.9600 . ?
C64 H64C 0.9600 . ?
C62 H62A 0.9600 . ?
C62 H62B 0.9600 . ?
C62 H62C 0.9600 . ?
C44 H44A 0.9600 . ?
C44 H44B 0.9600 . ?
C44 H44C 0.9600 . ?
C71 H71A 0.9600 . ?
C71 H71B 0.9600 . ?
C71 H71C 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
O2 V1 O1 125.79(10) . . ?
O2 V1 N2 113.75(10) . . ?
O1 V1 N2 119.06(10) . . ?
O2 V1 N1 87.54(9) . . ?
O1 V1 N1 88.98(9) . . ?
N2 V1 N1 81.21(10) . . ?
O2 V1 Cl1 92.86(7) . . ?
O1 V1 Cl1 95.46(8) . . ?
N2 V1 Cl1 93.35(8) . . ?
N1 V1 Cl1 174.20(7) . . ?
C11 O1 V1 133.25(19) . . ?
C21 O2 V1 137.2(2) . . ?
C1 N1 C27 110.9(2) . . ?
C1 N1 C17 109.3(2) . . ?
C27 N1 C17 106.3(2) . . ?
C1 N1 V1 106.13(18) . . ?
C27 N1 V1 113.52(18) . . ?
C17 N1 V1 110.67(18) . . ?
C6 N2 C2 110.8(3) . . ?
C6 N2 C5 108.4(3) . . ?
C2 N2 C5 103.1(2) . . ?
C6 N2 V1 113.9(2) . . ?
C2 N2 V1 111.87(19) . . ?
C5 N2 V1 108.1(2) . . ?
C72 O3 C73 112.8(3) . . ?
C23 C22 C21 116.9(3) . . ?
C23 C22 C51 121.0(3) . . ?
C21 C22 C51 122.0(3) . . ?
O2 C21 C26 120.0(3) . . ?
O2 C21 C22 120.0(3) . . ?
C26 C21 C22 119.9(3) . . ?
C24 C23 C22 124.6(3) . . ?
C24 C23 H23 117.7 . . ?
C22 C23 H23 117.7 . . ?
N1 C17 C16 113.3(2) . . ?
N1 C17 H17A 108.9 . . ?
C16 C17 H17A 108.9 . . ?
N1 C17 H17B 108.9 . . ?
C16 C17 H17B 108.9 . . ?
H17A C17 H17B 107.7 . . ?
C15 C16 C11 120.3(3) . . ?
C15 C16 C17 121.3(3) . . ?
C11 C16 C17 118.4(3) . . ?
O1 C11 C16 119.4(3) . . ?
O1 C11 C12 120.9(3) . . ?
C16 C11 C12 119.7(3) . . ?
N1 C27 C26 115.6(2) . . ?
N1 C27 H27A 108.4 . . ?
C26 C27 H27A 108.4 . . ?
N1 C27 H27B 108.4 . . ?
C26 C27 H27B 108.4 . . ?
H27A C27 H27B 107.4 . . ?
C13 C12 C11 116.9(3) . . ?
C13 C12 C31 122.5(3) . . ?
C11 C12 C31 120.6(3) . . ?
C21 C26 C25 120.6(3) . . ?
C21 C26 C27 121.1(3) . . ?
C25 C26 C27 118.0(3) . . ?
C51 C54 H54A 109.5 . . ?
C51 C54 H54B 109.5 . . ?
H54A C54 H54B 109.5 . . ?
C51 C54 H54C 109.5 . . ?
H54A C54 H54C 109.5 . . ?
H54B C54 H54C 109.5 . . ?
C12 C13 C14 124.5(3) . . ?
C12 C13 H13 117.7 . . ?
C14 C13 H13 117.7 . . ?
C32 C31 C33 109.7(3) . . ?
C32 C31 C12 109.2(3) . . ?
C33 C31 C12 110.8(3) . . ?
C32 C31 C34 108.3(3) . . ?
C33 C31 C34 107.0(3) . . ?
C12 C31 C34 111.8(3) . . ?
C43 C41 C14 111.0(3) . . ?
C43 C41 C42 109.7(3) . . ?
C14 C41 C42 109.0(3) . . ?
C43 C41 C44 109.4(4) . . ?
C14 C41 C44 111.4(3) . . ?
C42 C41 C44 106.1(3) . . ?
C24 C25 C26 121.1(3) . . ?
C24 C25 H25 119.5 . . ?
C26 C25 H25 119.5 . . ?
C23 C24 C25 116.9(3) . . ?
C23 C24 C61 122.6(3) . . ?
C25 C24 C61 120.6(3) . . ?
C62 C61 C63 110.4(4) . . ?
C62 C61 C24 110.1(3) . . ?
C63 C61 C24 109.8(3) . . ?
C62 C61 C64 109.0(3) . . ?
C63 C61 C64 106.2(3) . . ?
C24 C61 C64 111.3(3) . . ?
C31 C33 H33A 109.5 . . ?
C31 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
C31 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
N1 C1 C2 111.5(2) . . ?
N1 C1 H1A 109.3 . . ?
C2 C1 H1A 109.3 . . ?
N1 C1 H1B 109.3 . . ?
C2 C1 H1B 109.3 . . ?
H1A C1 H1B 108.0 . . ?
C14 C15 C16 121.2(3) . . ?
C14 C15 H15 119.4 . . ?
C16 C15 H15 119.4 . . ?
N2 C2 C1 108.6(2) . . ?
N2 C2 C3 106.5(3) . . ?
C1 C2 C3 111.1(3) . . ?
N2 C2 H2 110.2 . . ?
C1 C2 H2 110.2 . . ?
C3 C2 H2 110.2 . . ?
C15 C14 C13 116.7(3) . . ?
C15 C14 C41 122.9(3) . . ?
C13 C14 C41 120.4(3) . . ?
C53 C51 C22 110.2(3) . . ?
C53 C51 C52 109.6(3) . . ?
C22 C51 C52 110.1(3) . . ?
C53 C51 C54 108.3(3) . . ?
C22 C51 C54 111.4(3) . . ?
C52 C51 C54 107.2(3) . . ?
C4 C3 C2 105.2(3) . . ?
C4 C3 H3A 110.7 . . ?
C2 C3 H3A 110.7 . . ?
C4 C3 H3B 110.7 . . ?
C2 C3 H3B 110.7 . . ?
H3A C3 H3B 108.8 . . ?
N2 C5 C4 105.5(3) . . ?
N2 C5 H5A 110.6 . . ?
C4 C5 H5A 110.6 . . ?
N2 C5 H5B 110.6 . . ?
C4 C5 H5B 110.6 . . ?
H5A C5 H5B 108.8 . . ?
C51 C53 H53A 109.5 . . ?
C51 C53 H53B 109.5 . . ?
H53A C53 H53B 109.5 . . ?
C51 C53 H53C 109.5 . . ?
H53A C53 H53C 109.5 . . ?
H53B C53 H53C 109.5 . . ?
C5 C4 C3 105.2(3) . . ?
C5 C4 H4A 110.7 . . ?
C3 C4 H4A 110.7 . . ?
C5 C4 H4B 110.7 . . ?
C3 C4 H4B 110.7 . . ?
H4A C4 H4B 108.8 . . ?
C6 C7 H7A 109.5 . . ?
C6 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C6 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
O3 C73 C74 109.6(3) . . ?
O3 C73 H73A 109.7 . . ?
C74 C73 H73A 109.7 . . ?
O3 C73 H73B 109.7 . . ?
C74 C73 H73B 109.7 . . ?
H73A C73 H73B 108.2 . . ?
C31 C34 H34A 109.5 . . ?
C31 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
C31 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
O3 C72 C71 109.5(3) . . ?
O3 C72 H72A 109.8 . . ?
C71 C72 H72A 109.8 . . ?
O3 C72 H72B 109.8 . . ?
C71 C72 H72B 109.8 . . ?
H72A C72 H72B 108.2 . . ?
C7 C6 N2 113.8(3) . . ?
C7 C6 H6A 108.8 . . ?
N2 C6 H6A 108.8 . . ?
C7 C6 H6B 108.8 . . ?
N2 C6 H6B 108.8 . . ?
H6A C6 H6B 107.7 . . ?
C51 C52 H52A 109.5 . . ?
C51 C52 H52B 109.5 . . ?
H52A C52 H52B 109.5 . . ?
C51 C52 H52C 109.5 . . ?
H52A C52 H52C 109.5 . . ?
H52B C52 H52C 109.5 . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C73 C74 H74A 109.5 . . ?
C73 C74 H74B 109.5 . . ?
H74A C74 H74B 109.5 . . ?
C73 C74 H74C 109.5 . . ?
H74A C74 H74C 109.5 . . ?
H74B C74 H74C 109.5 . . ?
C41 C43 H43A 109.5 . . ?
C41 C43 H43B 109.5 . . ?
H43A C43 H43B 109.5 . . ?
C41 C43 H43C 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
C61 C63 H63A 109.5 . . ?
C61 C63 H63B 109.5 . . ?
H63A C63 H63B 109.5 . . ?
C61 C63 H63C 109.5 . . ?
H63A C63 H63C 109.5 . . ?
H63B C63 H63C 109.5 . . ?
C41 C42 H42A 109.5 . . ?
C41 C42 H42B 109.5 . . ?
H42A C42 H42B 109.5 . . ?
C41 C42 H42C 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
C61 C64 H64A 109.5 . . ?
C61 C64 H64B 109.5 . . ?
H64A C64 H64B 109.5 . . ?
C61 C64 H64C 109.5 . . ?
H64A C64 H64C 109.5 . . ?
H64B C64 H64C 109.5 . . ?
C61 C62 H62A 109.5 . . ?
C61 C62 H62B 109.5 . . ?
H62A C62 H62B 109.5 . . ?
C61 C62 H62C 109.5 . . ?
H62A C62 H62C 109.5 . . ?
H62B C62 H62C 109.5 . . ?
C41 C44 H44A 109.5 . . ?
C41 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
C41 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
C72 C71 H71A 109.5 . . ?
C72 C71 H71B 109.5 . . ?
H71A C71 H71B 109.5 . . ?
C72 C71 H71C 109.5 . . ?
H71A C71 H71C 109.5 . . ?
H71B C71 H71C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O2 V1 O1 C11 -62.3(3) . . . . ?
N2 V1 O1 C11 103.3(3) . . . . ?
N1 V1 O1 C11 23.9(3) . . . . ?
Cl1 V1 O1 C11 -159.8(3) . . . . ?
O1 V1 O2 C21 97.3(3) . . . . ?
N2 V1 O2 C21 -68.9(3) . . . . ?
N1 V1 O2 C21 10.3(3) . . . . ?
Cl1 V1 O2 C21 -163.9(3) . . . . ?
V1 O2 C21 C26 -25.7(4) . . . . ?
V1 O2 C21 C22 155.8(2) . . . . ?
C23 C22 C21 O2 176.1(3) . . . . ?
C51 C22 C21 O2 -0.4(4) . . . . ?
C23 C22 C21 C26 -2.4(4) . . . . ?
C51 C22 C21 C26 -178.8(3) . . . . ?
C21 C22 C23 C24 1.1(5) . . . . ?
C51 C22 C23 C24 177.6(3) . . . . ?
C1 N1 C17 C16 -178.6(2) . . . . ?
C27 N1 C17 C16 61.6(3) . . . . ?
V1 N1 C17 C16 -62.1(3) . . . . ?
N1 C17 C16 C15 -120.1(3) . . . . ?
N1 C17 C16 C11 60.8(4) . . . . ?
V1 O1 C11 C16 -34.3(4) . . . . ?
V1 O1 C11 C12 145.2(2) . . . . ?
C15 C16 C11 O1 170.5(3) . . . . ?
C17 C16 C11 O1 -10.4(4) . . . . ?
C15 C16 C11 C12 -9.0(4) . . . . ?
C17 C16 C11 C12 170.1(3) . . . . ?
C1 N1 C27 C26 61.9(3) . . . . ?
C17 N1 C27 C26 -179.4(2) . . . . ?
V1 N1 C27 C26 -57.5(3) . . . . ?
O1 C11 C12 C13 -171.7(3) . . . . ?
C16 C11 C12 C13 7.8(4) . . . . ?
O1 C11 C12 C31 9.3(4) . . . . ?
C16 C11 C12 C31 -171.2(3) . . . . ?
O2 C21 C26 C25 -176.9(3) . . . . ?
C22 C21 C26 C25 1.6(4) . . . . ?
O2 C21 C26 C27 -2.7(4) . . . . ?
C22 C21 C26 C27 175.8(3) . . . . ?
N1 C27 C26 C21 45.9(4) . . . . ?
N1 C27 C26 C25 -139.8(3) . . . . ?
C11 C12 C13 C14 -0.8(5) . . . . ?
C31 C12 C13 C14 178.2(3) . . . . ?
C13 C12 C31 C32 -120.0(3) . . . . ?
C11 C12 C31 C32 58.9(4) . . . . ?
C13 C12 C31 C33 119.1(3) . . . . ?
C11 C12 C31 C33 -62.0(4) . . . . ?
C13 C12 C31 C34 -0.2(4) . . . . ?
C11 C12 C31 C34 178.7(3) . . . . ?
C21 C26 C25 C24 0.6(5) . . . . ?
C27 C26 C25 C24 -173.8(3) . . . . ?
C22 C23 C24 C25 1.0(5) . . . . ?
C22 C23 C24 C61 -177.2(3) . . . . ?
C26 C25 C24 C23 -1.8(4) . . . . ?
C26 C25 C24 C61 176.3(3) . . . . ?
C23 C24 C61 C62 114.4(4) . . . . ?
C25 C24 C61 C62 -63.7(4) . . . . ?
C23 C24 C61 C63 -123.9(3) . . . . ?
C25 C24 C61 C63 58.0(4) . . . . ?
C23 C24 C61 C64 -6.6(5) . . . . ?
C25 C24 C61 C64 175.3(3) . . . . ?
C27 N1 C1 C2 -169.2(2) . . . . ?
C17 N1 C1 C2 73.9(3) . . . . ?
V1 N1 C1 C2 -45.5(3) . . . . ?
C11 C16 C15 C14 2.9(5) . . . . ?
C17 C16 C15 C14 -176.1(3) . . . . ?
C6 N2 C2 C1 -156.7(2) . . . . ?
C5 N2 C2 C1 87.5(3) . . . . ?
V1 N2 C2 C1 -28.4(3) . . . . ?
C6 N2 C2 C3 83.7(3) . . . . ?
C5 N2 C2 C3 -32.1(3) . . . . ?
V1 N2 C2 C3 -148.1(2) . . . . ?
N1 C1 C2 N2 50.0(3) . . . . ?
N1 C1 C2 C3 166.7(3) . . . . ?
C16 C15 C14 C13 3.9(5) . . . . ?
C16 C15 C14 C41 -175.6(3) . . . . ?
C12 C13 C14 C15 -5.1(5) . . . . ?
C12 C13 C14 C41 174.5(3) . . . . ?
C43 C41 C14 C15 -112.4(4) . . . . ?
C42 C41 C14 C15 126.6(3) . . . . ?
C44 C41 C14 C15 9.8(5) . . . . ?
C43 C41 C14 C13 68.1(4) . . . . ?
C42 C41 C14 C13 -52.9(4) . . . . ?
C44 C41 C14 C13 -169.7(3) . . . . ?
C23 C22 C51 C53 -115.7(3) . . . . ?
C21 C22 C51 C53 60.7(4) . . . . ?
C23 C22 C51 C52 123.3(3) . . . . ?
C21 C22 C51 C52 -60.3(4) . . . . ?
C23 C22 C51 C54 4.5(4) . . . . ?
C21 C22 C51 C54 -179.1(3) . . . . ?
N2 C2 C3 C4 13.8(4) . . . . ?
C1 C2 C3 C4 -104.3(3) . . . . ?
C6 N2 C5 C4 -78.7(3) . . . . ?
C2 N2 C5 C4 38.8(3) . . . . ?
V1 N2 C5 C4 157.4(2) . . . . ?
N2 C5 C4 C3 -30.3(4) . . . . ?
C2 C3 C4 C5 10.0(4) . . . . ?
C72 O3 C73 C74 -174.7(3) . . . . ?
C73 O3 C72 C71 174.0(3) . . . . ?
C2 N2 C6 C7 74.6(4) . . . . ?
C5 N2 C6 C7 -173.0(3) . . . . ?
V1 N2 C6 C7 -52.6(4) . . . . ?

_refine_diff_density_max         0.474
_refine_diff_density_min         -0.259
_refine_diff_density_rms         0.057

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_7
_database_code_depnum_ccdc_archive 'CCDC 1536786'
_audit_update_record             
;
2017-06-28 deposited with the CCDC.
2017-06-30 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         'C37 H58 Cl N2 O4 V'
_chemical_formula_sum            'C37 H58 Cl N2 O4 V'
_chemical_melting_point          ?

_exptl_crystal_description       prism
_exptl_crystal_colour            blue
_diffrn_ambient_temperature      150(2)
_chemical_formula_weight         681.24

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'
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      monoclinic
_space_group_IT_number           4
_space_group_name_H-M_alt        'P 21'
_space_group_name_Hall           'P 2yb'
_chemical_absolute_configuration syn

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

_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.
;

_cell_length_a                   14.468(11)
_cell_length_b                   7.746(5)
_cell_length_c                   17.587(13)
_cell_angle_alpha                90
_cell_angle_beta                 112.27(2)
_cell_angle_gamma                90
_cell_volume                     1824(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    733
_cell_measurement_theta_min      2.77
_cell_measurement_theta_max      16.92
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.240
_exptl_crystal_F_000             732
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.040
_exptl_absorpt_coefficient_mu    0.385
_shelx_estimated_absorpt_T_min   0.893
_shelx_estimated_absorpt_T_max   0.985
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.893
_exptl_absorpt_correction_T_max  0.985
_exptl_absorpt_process_details   'SADABS,  G. M. Sheldrick, 1996'
_exptl_absorpt_special_details   ?
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'sealed tube'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            16581
_diffrn_reflns_av_unetI/netI     0.3340
_diffrn_reflns_av_R_equivalents  0.1784
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.912
_diffrn_reflns_theta_max         24.057
_diffrn_reflns_theta_full        24.057
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measured_fraction_theta_full 0.980
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_Laue_measured_fraction_full 0.980
_diffrn_reflns_point_group_measured_fraction_max 0.916
_diffrn_reflns_point_group_measured_fraction_full 0.916
_reflns_number_total             5273
_reflns_number_gt                1924
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.724
_reflns_Friedel_fraction_max     0.840
_reflns_Friedel_fraction_full    0.840

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Sir2004 (M.C. Burla et al, 2005)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    
'Ortep3 for Windows v2.0 (L.J. Farrugia, J. Appl. Cryst. (1997) 30, 565)'
_computing_publication_material  'enCIFer v1.6'

_refine_special_details          
;
ISOR restraints were used on atoms C22, C13, N2, O3, N1, C11, C1, C6, C52, C2, C33, C34 and C32 to prevent them from turning non-positive definite.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1656P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 411 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.02(6)
_refine_ls_number_reflns         5273
_refine_ls_number_parameters     419
_refine_ls_number_restraints     79
_refine_ls_R_factor_all          0.2538
_refine_ls_R_factor_gt           0.1199
_refine_ls_wR_factor_ref         0.3221
_refine_ls_wR_factor_gt          0.2684
_refine_ls_goodness_of_fit_ref   0.905
_refine_ls_restrained_S_all      0.908
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
V1 V 0.2230(2) 0.4604(4) 0.3149(2) 0.0467(12) Uani 1 1 d . . . . .
Cl1 Cl 0.3171(4) 0.6886(6) 0.3931(4) 0.0512(17) Uani 1 1 d . . . . .
O2 O 0.1356(9) 0.4594(17) 0.3623(8) 0.041(3) Uani 1 1 d . . . . .
O1 O 0.3064(8) 0.4204(15) 0.2608(9) 0.041(4) Uani 1 1 d . . . . .
O3 O 0.1251(10) 0.4871(18) 0.2168(9) 0.057(4) Uani 1 1 d . U . . .
O4 O 0.1621(9) 0.6473(16) 0.2494(9) 0.053(4) Uani 1 1 d . . . . .
C11 C 0.2796(15) 0.366(3) 0.1865(14) 0.036(5) Uani 1 1 d . U . . .
N2 N 0.3302(12) 0.312(2) 0.4268(12) 0.042(5) Uani 1 1 d . U . . .
C61 C -0.2662(15) 0.224(3) 0.2598(15) 0.048(6) Uani 1 1 d . . . . .
N1 N 0.1707(11) 0.186(2) 0.2872(11) 0.044(4) Uani 1 1 d . U . . .
C15 C 0.1856(16) 0.150(3) 0.0938(15) 0.048(6) Uani 1 1 d . . . . .
H15 H 0.146966 0.050320 0.083838 0.058 Uiso 1 1 calc R U . . .
C24 C -0.1586(17) 0.289(3) 0.2857(13) 0.044(6) Uani 1 1 d . . . . .
C3 C 0.3160(14) 0.066(2) 0.5076(13) 0.035(6) Uani 1 1 d . . . . .
H3A H 0.364875 -0.026698 0.524274 0.042 Uiso 1 1 calc R U . . .
H3B H 0.254634 0.023781 0.511388 0.042 Uiso 1 1 calc R U . . .
C51 C 0.0002(16) 0.656(2) 0.4165(13) 0.044(6) Uani 1 1 d . . . . .
C23 C -0.1245(17) 0.426(3) 0.3391(13) 0.054(6) Uani 1 1 d . . . . .
H23 H -0.167170 0.480762 0.359947 0.064 Uiso 1 1 calc R U . . .
C12 C 0.2952(15) 0.444(3) 0.1204(18) 0.055(6) Uani 1 1 d . . . . .
C17 C 0.2237(16) 0.108(3) 0.2379(15) 0.050(6) Uani 1 1 d . . . . .
H17A H 0.292711 0.089772 0.274155 0.060 Uiso 1 1 calc R U . . .
H17B H 0.194742 -0.004701 0.219441 0.060 Uiso 1 1 calc R U . . .
C64 C -0.3262(16) 0.297(3) 0.3078(15) 0.069(8) Uani 1 1 d . . . . .
H64A H -0.332809 0.419410 0.300061 0.103 Uiso 1 1 calc R U . . .
H64B H -0.292128 0.271665 0.365201 0.103 Uiso 1 1 calc R U . . .
H64C H -0.391276 0.244698 0.288394 0.103 Uiso 1 1 calc R U . . .
C27 C 0.0653(12) 0.183(3) 0.2390(13) 0.046(6) Uani 1 1 d . . . . .
H27A H 0.044080 0.064113 0.227345 0.056 Uiso 1 1 calc R U . . .
H27B H 0.053722 0.239569 0.186939 0.056 Uiso 1 1 calc R U . . .
C6 C 0.4340(13) 0.322(3) 0.4415(13) 0.041(5) Uani 1 1 d . U . . .
H6A H 0.470301 0.283734 0.497563 0.049 Uiso 1 1 calc R U . . .
H6B H 0.450050 0.442521 0.439106 0.049 Uiso 1 1 calc R U . . .
C5 C 0.3177(18) 0.367(3) 0.4992(13) 0.053(7) Uani 1 1 d . . . . .
H5A H 0.247958 0.392168 0.487462 0.063 Uiso 1 1 calc R U . . .
H5B H 0.356436 0.470549 0.520592 0.063 Uiso 1 1 calc R U . . .
C21 C 0.043(2) 0.407(3) 0.3347(14) 0.054(7) Uani 1 1 d . . . . .
C1 C 0.1970(14) 0.100(3) 0.3677(13) 0.048(6) Uani 1 1 d . U . . .
H1A H 0.153523 0.145790 0.393393 0.057 Uiso 1 1 calc R U . . .
H1B H 0.182197 -0.021628 0.357947 0.057 Uiso 1 1 calc R U . . .
C25 C -0.0944(16) 0.214(3) 0.2546(14) 0.051(6) Uani 1 1 d . . . . .
H25 H -0.116570 0.124782 0.216840 0.062 Uiso 1 1 calc R U . . .
C14 C 0.1945(16) 0.225(3) 0.0265(15) 0.056(6) Uani 1 1 d . . . . .
C7 C 0.4781(16) 0.219(3) 0.3848(16) 0.073(8) Uani 1 1 d . . . . .
H7A H 0.484767 0.099225 0.399830 0.109 Uiso 1 1 calc R U . . .
H7B H 0.542354 0.265269 0.391795 0.109 Uiso 1 1 calc R U . . .
H7C H 0.433738 0.230614 0.328358 0.109 Uiso 1 1 calc R U . . .
C53 C -0.0038(18) 0.796(3) 0.3520(15) 0.071(8) Uani 1 1 d . . . . .
H53A H 0.016878 0.905139 0.379045 0.107 Uiso 1 1 calc R U . . .
H53B H -0.070870 0.805519 0.312225 0.107 Uiso 1 1 calc R U . . .
H53C H 0.040044 0.764004 0.324862 0.107 Uiso 1 1 calc R U . . .
C22 C -0.0242(18) 0.484(3) 0.3624(14) 0.059(7) Uani 1 1 d . U . . .
C2 C 0.2979(14) 0.117(2) 0.4251(13) 0.039(5) Uani 1 1 d . U . . .
H2 H 0.340651 0.046780 0.405192 0.046 Uiso 1 1 calc R U . . .
C26 C 0.0001(17) 0.270(3) 0.2783(13) 0.046(6) Uani 1 1 d . . . . .
C62 C -0.319(2) 0.253(3) 0.1721(14) 0.078(8) Uani 1 1 d . . . . .
H62A H -0.281574 0.202082 0.142673 0.117 Uiso 1 1 calc R U . . .
H62B H -0.325655 0.374561 0.161313 0.117 Uiso 1 1 calc R U . . .
H62C H -0.383763 0.200684 0.154326 0.117 Uiso 1 1 calc R U . . .
C52 C 0.0972(16) 0.657(3) 0.4826(13) 0.063(7) Uani 1 1 d . U . . .
H52A H 0.106269 0.763841 0.512362 0.095 Uiso 1 1 calc R U . . .
H52B H 0.148158 0.645696 0.460450 0.095 Uiso 1 1 calc R U . . .
H52C H 0.101662 0.562465 0.519092 0.095 Uiso 1 1 calc R U . . .
C54 C -0.0765(13) 0.693(3) 0.4546(14) 0.054(6) Uani 1 1 d . . . . .
H54A H -0.081517 0.594902 0.486130 0.081 Uiso 1 1 calc R U . . .
H54B H -0.140301 0.715184 0.411804 0.081 Uiso 1 1 calc R U . . .
H54C H -0.055918 0.792146 0.489776 0.081 Uiso 1 1 calc R U . . .
C16 C 0.2235(14) 0.200(3) 0.1689(15) 0.047(6) Uani 1 1 d . . . . .
C4 C 0.3540(17) 0.219(3) 0.5628(12) 0.061(7) Uani 1 1 d . . . . .
H4A H 0.426214 0.217551 0.589701 0.073 Uiso 1 1 calc R U . . .
H4B H 0.324494 0.226312 0.603821 0.073 Uiso 1 1 calc R U . . .
C13 C 0.2554(13) 0.384(3) 0.0445(16) 0.048(6) Uani 1 1 d . U . . .
H13 H 0.265761 0.442591 0.002226 0.057 Uiso 1 1 calc R U . . .
C41 C 0.1485(19) 0.180(3) -0.0605(13) 0.067(7) Uani 1 1 d . . . . .
C44 C 0.107(2) -0.010(4) -0.0718(18) 0.097(10) Uani 1 1 d . . . . .
H44A H 0.159797 -0.088605 -0.043705 0.145 Uiso 1 1 calc R U . . .
H44B H 0.078587 -0.037831 -0.129211 0.145 Uiso 1 1 calc R U . . .
H44C H 0.055764 -0.018499 -0.049313 0.145 Uiso 1 1 calc R U . . .
C43 C 0.066(2) 0.300(4) -0.1058(17) 0.093(10) Uani 1 1 d . . . . .
H43A H 0.010267 0.280539 -0.089845 0.140 Uiso 1 1 calc R U . . .
H43B H 0.045516 0.281537 -0.163860 0.140 Uiso 1 1 calc R U . . .
H43C H 0.088568 0.417333 -0.093045 0.140 Uiso 1 1 calc R U . . .
C42 C 0.227(2) 0.174(4) -0.102(2) 0.123(13) Uani 1 1 d . . . . .
H42A H 0.259765 0.284285 -0.095300 0.185 Uiso 1 1 calc R U . . .
H42B H 0.193712 0.149544 -0.159421 0.185 Uiso 1 1 calc R U . . .
H42C H 0.275476 0.086212 -0.076552 0.185 Uiso 1 1 calc R U . . .
C63 C -0.261(2) 0.028(3) 0.271(2) 0.108(12) Uani 1 1 d . . . . .
H63A H -0.326550 -0.020045 0.245688 0.162 Uiso 1 1 calc R U . . .
H63B H -0.234890 0.001661 0.328891 0.162 Uiso 1 1 calc R U . . .
H63C H -0.217810 -0.019699 0.246534 0.162 Uiso 1 1 calc R U . . .
C33 C 0.3875(19) 0.666(3) 0.0705(16) 0.084(8) Uani 1 1 d . U . . .
H33A H 0.429847 0.766120 0.086801 0.126 Uiso 1 1 calc R U . . .
H33B H 0.325986 0.696901 0.026784 0.126 Uiso 1 1 calc R U . . .
H33C H 0.420502 0.577844 0.051973 0.126 Uiso 1 1 calc R U . . .
C31 C 0.3671(18) 0.604(2) 0.1388(15) 0.051(7) Uani 1 1 d . . . . .
C32 C 0.4659(18) 0.564(3) 0.2090(19) 0.090(9) Uani 1 1 d . U . . .
H32A H 0.502322 0.480581 0.191068 0.135 Uiso 1 1 calc R U . . .
H32B H 0.452916 0.518198 0.254765 0.135 Uiso 1 1 calc R U . . .
H32C H 0.504537 0.667858 0.225510 0.135 Uiso 1 1 calc R U . . .
C34 C 0.315(2) 0.758(3) 0.1701(18) 0.093(9) Uani 1 1 d . U . . .
H34A H 0.358793 0.855953 0.185465 0.140 Uiso 1 1 calc R U . . .
H34B H 0.301280 0.719427 0.216658 0.140 Uiso 1 1 calc R U . . .
H34C H 0.253406 0.790404 0.126636 0.140 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
V1 O2 1.757(13) . ?
V1 O3 1.782(15) . ?
V1 O1 1.826(15) . ?
V1 O4 1.852(13) . ?
V1 N1 2.250(17) . ?
V1 N2 2.299(19) . ?
V1 Cl1 2.334(6) . ?
O2 C21 1.31(3) . ?
O1 C11 1.29(2) . ?
O3 O4 1.386(18) . ?
C11 C12 1.40(3) . ?
C11 C16 1.49(3) . ?
N2 C5 1.42(3) . ?
N2 C6 1.43(2) . ?
N2 C2 1.58(2) . ?
C61 C62 1.46(3) . ?
C61 C63 1.53(3) . ?
C61 C24 1.53(3) . ?
C61 C64 1.53(3) . ?
N1 C27 1.44(2) . ?
N1 C1 1.47(2) . ?
N1 C17 1.49(2) . ?
C15 C16 1.28(3) . ?
C15 C14 1.37(3) . ?
C15 H15 0.9300 . ?
C24 C25 1.37(3) . ?
C24 C23 1.38(3) . ?
C3 C2 1.43(3) . ?
C3 C4 1.50(3) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C51 C52 1.44(3) . ?
C51 C54 1.52(3) . ?
C51 C53 1.55(3) . ?
C51 C22 1.60(3) . ?
C23 C22 1.42(3) . ?
C23 H23 0.9300 . ?
C12 C13 1.32(3) . ?
C12 C31 1.57(3) . ?
C17 C16 1.40(3) . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C64 H64A 0.9600 . ?
C64 H64B 0.9600 . ?
C64 H64C 0.9600 . ?
C27 C26 1.52(3) . ?
C27 H27A 0.9700 . ?
C27 H27B 0.9700 . ?
C6 C7 1.59(3) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C5 C4 1.55(3) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C21 C22 1.38(3) . ?
C21 C26 1.42(3) . ?
C1 C2 1.43(3) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C25 C26 1.34(3) . ?
C25 H25 0.9300 . ?
C14 C41 1.46(3) . ?
C14 C13 1.48(3) . ?
C7 H7A 0.9600 . ?
C7 H7B 0.9600 . ?
C7 H7C 0.9600 . ?
C53 H53A 0.9600 . ?
C53 H53B 0.9600 . ?
C53 H53C 0.9600 . ?
C2 H2 0.9800 . ?
C62 H62A 0.9600 . ?
C62 H62B 0.9600 . ?
C62 H62C 0.9600 . ?
C52 H52A 0.9600 . ?
C52 H52B 0.9600 . ?
C52 H52C 0.9600 . ?
C54 H54A 0.9600 . ?
C54 H54B 0.9600 . ?
C54 H54C 0.9600 . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C13 H13 0.9300 . ?
C41 C43 1.49(3) . ?
C41 C42 1.56(3) . ?
C41 C44 1.57(4) . ?
C44 H44A 0.9600 . ?
C44 H44B 0.9600 . ?
C44 H44C 0.9600 . ?
C43 H43A 0.9600 . ?
C43 H43B 0.9600 . ?
C43 H43C 0.9600 . ?
C42 H42A 0.9600 . ?
C42 H42B 0.9600 . ?
C42 H42C 0.9600 . ?
C63 H63A 0.9600 . ?
C63 H63B 0.9600 . ?
C63 H63C 0.9600 . ?
C33 C31 1.42(3) . ?
C33 H33A 0.9600 . ?
C33 H33B 0.9600 . ?
C33 H33C 0.9600 . ?
C31 C32 1.53(3) . ?
C31 C34 1.62(3) . ?
C32 H32A 0.9600 . ?
C32 H32B 0.9600 . ?
C32 H32C 0.9600 . ?
C34 H34A 0.9600 . ?
C34 H34B 0.9600 . ?
C34 H34C 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
O2 V1 O3 90.6(6) . . ?
O2 V1 O1 169.4(6) . . ?
O3 V1 O1 87.4(6) . . ?
O2 V1 O4 92.3(6) . . ?
O3 V1 O4 44.8(6) . . ?
O1 V1 O4 93.5(6) . . ?
O2 V1 N1 81.7(6) . . ?
O3 V1 N1 79.7(6) . . ?
O1 V1 N1 87.8(5) . . ?
O4 V1 N1 124.3(7) . . ?
O2 V1 N2 88.0(6) . . ?
O3 V1 N2 156.6(6) . . ?
O1 V1 N2 89.8(6) . . ?
O4 V1 N2 158.6(6) . . ?
N1 V1 N2 77.0(6) . . ?
O2 V1 Cl1 95.1(5) . . ?
O3 V1 Cl1 123.7(5) . . ?
O1 V1 Cl1 94.7(4) . . ?
O4 V1 Cl1 79.0(5) . . ?
N1 V1 Cl1 156.5(5) . . ?
N2 V1 Cl1 79.7(4) . . ?
C21 O2 V1 130.3(13) . . ?
C11 O1 V1 125.5(12) . . ?
O4 O3 V1 70.3(8) . . ?
O3 O4 V1 64.9(8) . . ?
O1 C11 C12 128(2) . . ?
O1 C11 C16 115(2) . . ?
C12 C11 C16 116(2) . . ?
C5 N2 C6 107.8(17) . . ?
C5 N2 C2 99.7(17) . . ?
C6 N2 C2 109.7(15) . . ?
C5 N2 V1 110.1(13) . . ?
C6 N2 V1 116.8(13) . . ?
C2 N2 V1 111.4(12) . . ?
C62 C61 C63 106(2) . . ?
C62 C61 C24 109.2(19) . . ?
C63 C61 C24 106.9(18) . . ?
C62 C61 C64 110.6(19) . . ?
C63 C61 C64 108(2) . . ?
C24 C61 C64 116.1(19) . . ?
C27 N1 C1 113.1(15) . . ?
C27 N1 C17 108.6(17) . . ?
C1 N1 C17 112.1(16) . . ?
C27 N1 V1 109.5(13) . . ?
C1 N1 V1 105.8(12) . . ?
C17 N1 V1 107.7(12) . . ?
C16 C15 C14 128(2) . . ?
C16 C15 H15 115.8 . . ?
C14 C15 H15 115.8 . . ?
C25 C24 C23 118(2) . . ?
C25 C24 C61 120.6(19) . . ?
C23 C24 C61 121(2) . . ?
C2 C3 C4 108.6(16) . . ?
C2 C3 H3A 110.0 . . ?
C4 C3 H3A 110.0 . . ?
C2 C3 H3B 110.0 . . ?
C4 C3 H3B 110.0 . . ?
H3A C3 H3B 108.4 . . ?
C52 C51 C54 107.0(18) . . ?
C52 C51 C53 110.0(18) . . ?
C54 C51 C53 111.0(18) . . ?
C52 C51 C22 114.4(17) . . ?
C54 C51 C22 112.6(18) . . ?
C53 C51 C22 102.0(16) . . ?
C24 C23 C22 120(2) . . ?
C24 C23 H23 119.9 . . ?
C22 C23 H23 119.9 . . ?
C13 C12 C11 123(2) . . ?
C13 C12 C31 119(2) . . ?
C11 C12 C31 118(2) . . ?
C16 C17 N1 117.9(17) . . ?
C16 C17 H17A 107.8 . . ?
N1 C17 H17A 107.8 . . ?
C16 C17 H17B 107.8 . . ?
N1 C17 H17B 107.8 . . ?
H17A C17 H17B 107.2 . . ?
C61 C64 H64A 109.5 . . ?
C61 C64 H64B 109.5 . . ?
H64A C64 H64B 109.5 . . ?
C61 C64 H64C 109.5 . . ?
H64A C64 H64C 109.5 . . ?
H64B C64 H64C 109.5 . . ?
N1 C27 C26 115.4(18) . . ?
N1 C27 H27A 108.4 . . ?
C26 C27 H27A 108.4 . . ?
N1 C27 H27B 108.4 . . ?
C26 C27 H27B 108.4 . . ?
H27A C27 H27B 107.5 . . ?
N2 C6 C7 120.4(17) . . ?
N2 C6 H6A 107.2 . . ?
C7 C6 H6A 107.2 . . ?
N2 C6 H6B 107.2 . . ?
C7 C6 H6B 107.2 . . ?
H6A C6 H6B 106.9 . . ?
N2 C5 C4 107.6(18) . . ?
N2 C5 H5A 110.2 . . ?
C4 C5 H5A 110.2 . . ?
N2 C5 H5B 110.2 . . ?
C4 C5 H5B 110.2 . . ?
H5A C5 H5B 108.5 . . ?
O2 C21 C22 120(2) . . ?
O2 C21 C26 127(2) . . ?
C22 C21 C26 113(2) . . ?
C2 C1 N1 117.5(18) . . ?
C2 C1 H1A 107.9 . . ?
N1 C1 H1A 107.9 . . ?
C2 C1 H1B 107.9 . . ?
N1 C1 H1B 107.9 . . ?
H1A C1 H1B 107.2 . . ?
C26 C25 C24 120(2) . . ?
C26 C25 H25 119.8 . . ?
C24 C25 H25 119.8 . . ?
C15 C14 C41 131(2) . . ?
C15 C14 C13 114(2) . . ?
C41 C14 C13 115(2) . . ?
C6 C7 H7A 109.5 . . ?
C6 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C6 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C51 C53 H53A 109.5 . . ?
C51 C53 H53B 109.5 . . ?
H53A C53 H53B 109.5 . . ?
C51 C53 H53C 109.5 . . ?
H53A C53 H53C 109.5 . . ?
H53B C53 H53C 109.5 . . ?
C21 C22 C23 123(2) . . ?
C21 C22 C51 123(2) . . ?
C23 C22 C51 114(2) . . ?
C3 C2 C1 115.9(19) . . ?
C3 C2 N2 107.8(18) . . ?
C1 C2 N2 108.2(16) . . ?
C3 C2 H2 108.2 . . ?
C1 C2 H2 108.2 . . ?
N2 C2 H2 108.2 . . ?
C25 C26 C21 125(2) . . ?
C25 C26 C27 117(2) . . ?
C21 C26 C27 117.6(19) . . ?
C61 C62 H62A 109.5 . . ?
C61 C62 H62B 109.5 . . ?
H62A C62 H62B 109.5 . . ?
C61 C62 H62C 109.5 . . ?
H62A C62 H62C 109.5 . . ?
H62B C62 H62C 109.5 . . ?
C51 C52 H52A 109.5 . . ?
C51 C52 H52B 109.5 . . ?
H52A C52 H52B 109.5 . . ?
C51 C52 H52C 109.5 . . ?
H52A C52 H52C 109.5 . . ?
H52B C52 H52C 109.5 . . ?
C51 C54 H54A 109.5 . . ?
C51 C54 H54B 109.5 . . ?
H54A C54 H54B 109.5 . . ?
C51 C54 H54C 109.5 . . ?
H54A C54 H54C 109.5 . . ?
H54B C54 H54C 109.5 . . ?
C15 C16 C17 127(2) . . ?
C15 C16 C11 117(2) . . ?
C17 C16 C11 116(2) . . ?
C3 C4 C5 100.3(14) . . ?
C3 C4 H4A 111.7 . . ?
C5 C4 H4A 111.7 . . ?
C3 C4 H4B 111.7 . . ?
C5 C4 H4B 111.7 . . ?
H4A C4 H4B 109.5 . . ?
C12 C13 C14 120(2) . . ?
C12 C13 H13 119.9 . . ?
C14 C13 H13 119.9 . . ?
C14 C41 C43 111(2) . . ?
C14 C41 C42 112(2) . . ?
C43 C41 C42 110(2) . . ?
C14 C41 C44 111(2) . . ?
C43 C41 C44 109(2) . . ?
C42 C41 C44 103(2) . . ?
C41 C44 H44A 109.5 . . ?
C41 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
C41 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
C41 C43 H43A 109.5 . . ?
C41 C43 H43B 109.5 . . ?
H43A C43 H43B 109.5 . . ?
C41 C43 H43C 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
C41 C42 H42A 109.5 . . ?
C41 C42 H42B 109.5 . . ?
H42A C42 H42B 109.5 . . ?
C41 C42 H42C 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
C61 C63 H63A 109.5 . . ?
C61 C63 H63B 109.5 . . ?
H63A C63 H63B 109.5 . . ?
C61 C63 H63C 109.5 . . ?
H63A C63 H63C 109.5 . . ?
H63B C63 H63C 109.5 . . ?
C31 C33 H33A 109.5 . . ?
C31 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
C31 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C33 C31 C32 109(2) . . ?
C33 C31 C12 115(2) . . ?
C32 C31 C12 110.4(19) . . ?
C33 C31 C34 108(2) . . ?
C32 C31 C34 107(2) . . ?
C12 C31 C34 107.1(18) . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C31 C34 H34A 109.5 . . ?
C31 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
C31 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?

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
O3 V1 O2 C21 30.6(17) . . . . ?
O1 V1 O2 C21 -48(4) . . . . ?
O4 V1 O2 C21 75.3(17) . . . . ?
N1 V1 O2 C21 -49.0(16) . . . . ?
N2 V1 O2 C21 -126.1(17) . . . . ?
Cl1 V1 O2 C21 154.4(16) . . . . ?
O2 V1 O1 C11 55(4) . . . . ?
O3 V1 O1 C11 -23.9(15) . . . . ?
O4 V1 O1 C11 -68.3(15) . . . . ?
N1 V1 O1 C11 55.9(15) . . . . ?
N2 V1 O1 C11 132.9(15) . . . . ?
Cl1 V1 O1 C11 -147.5(14) . . . . ?
O2 V1 O3 O4 92.7(9) . . . . ?
O1 V1 O3 O4 -97.6(8) . . . . ?
N1 V1 O3 O4 174.2(9) . . . . ?
N2 V1 O3 O4 179.1(14) . . . . ?
Cl1 V1 O3 O4 -3.7(10) . . . . ?
O2 V1 O4 O3 -88.5(9) . . . . ?
O1 V1 O4 O3 82.7(9) . . . . ?
N1 V1 O4 O3 -7.0(11) . . . . ?
N2 V1 O4 O3 -179.0(15) . . . . ?
Cl1 V1 O4 O3 176.8(9) . . . . ?
V1 O1 C11 C12 123(2) . . . . ?
V1 O1 C11 C16 -56(2) . . . . ?
C62 C61 C24 C25 -63(3) . . . . ?
C63 C61 C24 C25 51(3) . . . . ?
C64 C61 C24 C25 171(2) . . . . ?
C62 C61 C24 C23 115(2) . . . . ?
C63 C61 C24 C23 -131(2) . . . . ?
C64 C61 C24 C23 -11(3) . . . . ?
C25 C24 C23 C22 -2(3) . . . . ?
C61 C24 C23 C22 -180.0(19) . . . . ?
O1 C11 C12 C13 -173.1(19) . . . . ?
C16 C11 C12 C13 6(3) . . . . ?
O1 C11 C12 C31 10(3) . . . . ?
C16 C11 C12 C31 -171.2(17) . . . . ?
C27 N1 C17 C16 69(2) . . . . ?
C1 N1 C17 C16 -165.9(18) . . . . ?
V1 N1 C17 C16 -50(2) . . . . ?
C1 N1 C27 C26 59(2) . . . . ?
C17 N1 C27 C26 -175.8(17) . . . . ?
V1 N1 C27 C26 -59(2) . . . . ?
C5 N2 C6 C7 161.7(18) . . . . ?
C2 N2 C6 C7 54(2) . . . . ?
V1 N2 C6 C7 -74(2) . . . . ?
C6 N2 C5 C4 -75(2) . . . . ?
C2 N2 C5 C4 39(2) . . . . ?
V1 N2 C5 C4 156.2(14) . . . . ?
V1 O2 C21 C22 -150.2(17) . . . . ?
V1 O2 C21 C26 32(3) . . . . ?
C27 N1 C1 C2 -171.4(18) . . . . ?
C17 N1 C1 C2 65(2) . . . . ?
V1 N1 C1 C2 -51.6(19) . . . . ?
C23 C24 C25 C26 3(3) . . . . ?
C61 C24 C25 C26 -179(2) . . . . ?
C16 C15 C14 C41 -176(2) . . . . ?
C16 C15 C14 C13 -1(3) . . . . ?
O2 C21 C22 C23 -175.7(18) . . . . ?
C26 C21 C22 C23 3(3) . . . . ?
O2 C21 C22 C51 10(3) . . . . ?
C26 C21 C22 C51 -171.7(18) . . . . ?
C24 C23 C22 C21 -1(3) . . . . ?
C24 C23 C22 C51 173.8(19) . . . . ?
C52 C51 C22 C21 -45(3) . . . . ?
C54 C51 C22 C21 -167(2) . . . . ?
C53 C51 C22 C21 74(2) . . . . ?
C52 C51 C22 C23 140(2) . . . . ?
C54 C51 C22 C23 18(2) . . . . ?
C53 C51 C22 C23 -101(2) . . . . ?
C4 C3 C2 C1 -119(2) . . . . ?
C4 C3 C2 N2 2(2) . . . . ?
N1 C1 C2 C3 167.0(16) . . . . ?
N1 C1 C2 N2 46(2) . . . . ?
C5 N2 C2 C3 -26(2) . . . . ?
C6 N2 C2 C3 87(2) . . . . ?
V1 N2 C2 C3 -142.1(13) . . . . ?
C5 N2 C2 C1 100(2) . . . . ?
C6 N2 C2 C1 -146.9(18) . . . . ?
V1 N2 C2 C1 -16(2) . . . . ?
C24 C25 C26 C21 -1(3) . . . . ?
C24 C25 C26 C27 -178.5(18) . . . . ?
O2 C21 C26 C25 176(2) . . . . ?
C22 C21 C26 C25 -2(3) . . . . ?
O2 C21 C26 C27 -6(3) . . . . ?
C22 C21 C26 C27 175.8(18) . . . . ?
N1 C27 C26 C25 -154(2) . . . . ?
N1 C27 C26 C21 28(3) . . . . ?
C14 C15 C16 C17 -171(2) . . . . ?
C14 C15 C16 C11 4(3) . . . . ?
N1 C17 C16 C15 -118(2) . . . . ?
N1 C17 C16 C11 67(3) . . . . ?
O1 C11 C16 C15 172.4(17) . . . . ?
C12 C11 C16 C15 -7(3) . . . . ?
O1 C11 C16 C17 -12(3) . . . . ?
C12 C11 C16 C17 169.1(18) . . . . ?
C2 C3 C4 C5 20(2) . . . . ?
N2 C5 C4 C3 -39(2) . . . . ?
C11 C12 C13 C14 -3(3) . . . . ?
C31 C12 C13 C14 174.8(19) . . . . ?
C15 C14 C13 C12 -1(3) . . . . ?
C41 C14 C13 C12 176(2) . . . . ?
C15 C14 C41 C43 104(3) . . . . ?
C13 C14 C41 C43 -71(3) . . . . ?
C15 C14 C41 C42 -132(3) . . . . ?
C13 C14 C41 C42 52(3) . . . . ?
C15 C14 C41 C44 -18(4) . . . . ?
C13 C14 C41 C44 167(2) . . . . ?
C13 C12 C31 C33 -3(3) . . . . ?
C11 C12 C31 C33 174(2) . . . . ?
C13 C12 C31 C32 -127(2) . . . . ?
C11 C12 C31 C32 50(3) . . . . ?
C13 C12 C31 C34 117(2) . . . . ?
C11 C12 C31 C34 -66(2) . . . . ?

_refine_diff_density_max         0.742
_refine_diff_density_min         -0.867
_refine_diff_density_rms         0.130

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_4
_database_code_depnum_ccdc_archive 'CCDC 1536782'
_audit_update_record             
;
2017-06-28 deposited with the CCDC.
2017-06-30 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         'C34 H54 Cl2 N2 O2 V'
_chemical_formula_sum            'C34 H54 Cl2 N2 O2 V'
_exptl_crystal_recrystallization_method toluene
_chemical_melting_point          ?

_exptl_crystal_description       prism
_exptl_crystal_colour            blue
_diffrn_ambient_temperature      150(2)
_chemical_formula_weight         644.63

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'
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      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'
_chemical_absolute_configuration .

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

_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.
;

_cell_length_a                   16.783(6)
_cell_length_b                   15.451(7)
_cell_length_c                   15.217(7)
_cell_angle_alpha                90
_cell_angle_beta                 116.088(10)
_cell_angle_gamma                90
_cell_volume                     3544(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    6724
_cell_measurement_theta_min      3.01
_cell_measurement_theta_max      25.72
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.208
_exptl_crystal_F_000             1380
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    0.461
_shelx_estimated_absorpt_T_min   0.874
_shelx_estimated_absorpt_T_max   0.955
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8741
_exptl_absorpt_correction_T_max  0.9553
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            23383
_diffrn_reflns_av_unetI/netI     0.1136
_diffrn_reflns_av_R_equivalents  0.1028
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         3.007
_diffrn_reflns_theta_max         25.681
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             6714
_reflns_number_gt                3848
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Sir2004 (M.C. Burla et al, 2005)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    
'Ortep3 for Windows v2.0 (L.J. Farrugia, J. Appl. Cryst. (1997) 30, 565)'
_computing_publication_material  'enCIFer v1.6'

_refine_special_details          
; 
One of the tBu fragments presents disordered methyl groups. A disorder model was applied to the methyl groups attached to C61 giving 22/78% occupancies. SADI restraints and EADP constraints were applied on the disordered atoms.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0437P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6714
_refine_ls_number_parameters     380
_refine_ls_number_restraints     15
_refine_ls_R_factor_all          0.1192
_refine_ls_R_factor_gt           0.0543
_refine_ls_wR_factor_ref         0.1179
_refine_ls_wR_factor_gt          0.1036
_refine_ls_goodness_of_fit_ref   0.943
_refine_ls_restrained_S_all      0.944
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
V1 V 0.47882(3) 0.25414(4) 0.48057(4) 0.02012(15) Uani 1 1 d . . . . .
Cl2 Cl 0.43455(5) 0.35441(6) 0.35298(6) 0.0323(2) Uani 1 1 d . . . . .
Cl1 Cl 0.51668(5) 0.14420(6) 0.40249(6) 0.0280(2) Uani 1 1 d . . . . .
O1 O 0.36586(13) 0.22034(14) 0.43727(15) 0.0234(5) Uani 1 1 d . . . . .
O2 O 0.58595(13) 0.30304(14) 0.53536(15) 0.0229(5) Uani 1 1 d . . . . .
N1 N 0.44326(15) 0.34261(17) 0.57220(18) 0.0207(6) Uani 1 1 d . . . . .
N2 N 0.52167(16) 0.17260(18) 0.61459(19) 0.0247(7) Uani 1 1 d . . . . .
C27 C 0.50397(19) 0.4185(2) 0.6141(2) 0.0264(8) Uani 1 1 d . . . . .
H27A H 0.492300 0.441934 0.666380 0.032 Uiso 1 1 calc R U . . .
H27B H 0.486324 0.462362 0.563394 0.032 Uiso 1 1 calc R U . . .
C11 C 0.28359(19) 0.2470(2) 0.4215(2) 0.0225(7) Uani 1 1 d . . . . .
C21 C 0.6394(2) 0.3598(2) 0.6030(2) 0.0230(8) Uani 1 1 d . . . . .
C31 C 0.2127(2) 0.1228(2) 0.2986(2) 0.0283(9) Uani 1 1 d . . . . .
C16 C 0.27640(19) 0.3227(2) 0.4665(2) 0.0228(8) Uani 1 1 d . . . . .
C1 C 0.4416(2) 0.2879(2) 0.6526(2) 0.0246(8) Uani 1 1 d . . . . .
H1A H 0.441878 0.324702 0.704368 0.030 Uiso 1 1 calc R U . . .
H1B H 0.387767 0.253470 0.627535 0.030 Uiso 1 1 calc R U . . .
C15 C 0.19346(19) 0.3482(2) 0.4582(2) 0.0243(8) Uani 1 1 d . . . . .
H15 H 0.189240 0.397517 0.490871 0.029 Uiso 1 1 calc R U . . .
C25 C 0.6583(2) 0.4576(2) 0.7329(2) 0.0245(8) Uani 1 1 d . . . . .
H25 H 0.634313 0.486807 0.769168 0.029 Uiso 1 1 calc R U . . .
C2 C 0.52088(19) 0.2295(2) 0.6926(2) 0.0255(8) Uani 1 1 d . . . . .
H2A H 0.574574 0.264105 0.719716 0.031 Uiso 1 1 calc R U . . .
H2B H 0.519625 0.194353 0.744752 0.031 Uiso 1 1 calc R U . . .
C22 C 0.72914(19) 0.3691(2) 0.6222(2) 0.0249(8) Uani 1 1 d . . . . .
C24 C 0.7476(2) 0.4654(2) 0.7592(2) 0.0262(8) Uani 1 1 d . . . . .
C13 C 0.1275(2) 0.2284(2) 0.3543(2) 0.0261(8) Uani 1 1 d . . . . .
H13 H 0.076669 0.197245 0.315538 0.031 Uiso 1 1 calc R U . . .
C23 C 0.7804(2) 0.4213(2) 0.7011(2) 0.0285(9) Uani 1 1 d . . . . .
H23 H 0.840277 0.427495 0.716607 0.034 Uiso 1 1 calc R U . . .
C26 C 0.60289(19) 0.4075(2) 0.6539(2) 0.0226(8) Uani 1 1 d . . . . .
C61 C 0.8099(2) 0.5209(2) 0.8462(2) 0.0301(9) Uani 1 1 d D . . . .
C54 C 0.8628(2) 0.3532(3) 0.5873(3) 0.0454(11) Uani 1 1 d . . . . .
H54A H 0.868026 0.415131 0.587853 0.068 Uiso 1 1 calc R U . . .
H54B H 0.898183 0.331060 0.651816 0.068 Uiso 1 1 calc R U . . .
H54C H 0.883156 0.329140 0.542606 0.068 Uiso 1 1 calc R U . . .
C14 C 0.1177(2) 0.3016(2) 0.4026(2) 0.0249(8) Uani 1 1 d . . . . .
C17 C 0.35358(18) 0.3832(2) 0.5172(2) 0.0247(8) Uani 1 1 d . . . . .
H17A H 0.356369 0.421922 0.468429 0.030 Uiso 1 1 calc R U . . .
H17B H 0.341435 0.418418 0.562727 0.030 Uiso 1 1 calc R U . . .
C41 C 0.0251(2) 0.3269(2) 0.3909(3) 0.0319(9) Uani 1 1 d . . . . .
C32 C 0.2502(2) 0.1540(3) 0.2283(3) 0.0421(10) Uani 1 1 d . . . . .
H32A H 0.253316 0.106107 0.189666 0.063 Uiso 1 1 calc R U . . .
H32B H 0.212228 0.197933 0.185975 0.063 Uiso 1 1 calc R U . . .
H32C H 0.308591 0.177319 0.265335 0.063 Uiso 1 1 calc R U . . .
C51 C 0.7652(2) 0.3282(2) 0.5546(3) 0.0316(9) Uani 1 1 d . . . . .
C33 C 0.2709(2) 0.0501(2) 0.3638(3) 0.0467(11) Uani 1 1 d . . . . .
H33A H 0.273024 0.003126 0.323528 0.070 Uiso 1 1 calc R U . . .
H33B H 0.329866 0.071621 0.402147 0.070 Uiso 1 1 calc R U . . .
H33C H 0.246465 0.029996 0.406443 0.070 Uiso 1 1 calc R U . . .
C12 C 0.2077(2) 0.1989(2) 0.3602(2) 0.0232(8) Uani 1 1 d . . . . .
C34 C 0.1210(2) 0.0835(2) 0.2370(3) 0.0385(10) Uani 1 1 d . . . . .
H34A H 0.126594 0.036029 0.199354 0.058 Uiso 1 1 calc R U . . .
H34B H 0.096266 0.063136 0.279267 0.058 Uiso 1 1 calc R U . . .
H34C H 0.082772 0.126768 0.193602 0.058 Uiso 1 1 calc R U . . .
C52 C 0.7115(2) 0.3621(3) 0.4498(3) 0.0472(11) Uani 1 1 d . . . . .
H52A H 0.715082 0.424145 0.449713 0.071 Uiso 1 1 calc R U . . .
H52B H 0.735273 0.338540 0.407950 0.071 Uiso 1 1 calc R U . . .
H52C H 0.650641 0.344894 0.426434 0.071 Uiso 1 1 calc R U . . .
C53 C 0.7594(2) 0.2293(2) 0.5545(3) 0.0411(11) Uani 1 1 d . . . . .
H53A H 0.698883 0.212198 0.534228 0.062 Uiso 1 1 calc R U . . .
H53B H 0.780345 0.205907 0.510009 0.062 Uiso 1 1 calc R U . . .
H53C H 0.795372 0.207828 0.619219 0.062 Uiso 1 1 calc R U . . .
C4 C 0.6121(2) 0.1369(2) 0.6482(3) 0.0363(10) Uani 1 1 d . . . . .
H4A H 0.653301 0.183415 0.658697 0.054 Uiso 1 1 calc R U . . .
H4B H 0.628332 0.105906 0.708294 0.054 Uiso 1 1 calc R U . . .
H4C H 0.613451 0.098362 0.599404 0.054 Uiso 1 1 calc R U . . .
C3 C 0.4615(2) 0.0980(2) 0.5997(2) 0.0350(9) Uani 1 1 d . . . . .
H3A H 0.401800 0.118526 0.577796 0.052 Uiso 1 1 calc R U . . .
H3B H 0.464434 0.059853 0.551474 0.052 Uiso 1 1 calc R U . . .
H3C H 0.479314 0.067396 0.660364 0.052 Uiso 1 1 calc R U . . .
C42 C -0.0338(2) 0.3500(3) 0.2833(3) 0.0658(15) Uani 1 1 d . . . . .
H42A H -0.036306 0.301624 0.242470 0.099 Uiso 1 1 calc R U . . .
H42B H -0.092501 0.363522 0.274923 0.099 Uiso 1 1 calc R U . . .
H42C H -0.009298 0.399149 0.265152 0.099 Uiso 1 1 calc R U . . .
C44 C 0.0270(2) 0.4049(2) 0.4519(3) 0.0378(10) Uani 1 1 d . . . . .
H44A H 0.052279 0.453259 0.433511 0.057 Uiso 1 1 calc R U . . .
H44B H -0.032408 0.418853 0.440974 0.057 Uiso 1 1 calc R U . . .
H44C H 0.062194 0.392032 0.519880 0.057 Uiso 1 1 calc R U . . .
C43 C -0.0152(3) 0.2508(3) 0.4210(4) 0.0885(19) Uani 1 1 d . . . . .
H43A H -0.016707 0.200936 0.382674 0.133 Uiso 1 1 calc R U . . .
H43B H 0.020137 0.238403 0.489054 0.133 Uiso 1 1 calc R U . . .
H43C H -0.074466 0.265224 0.410149 0.133 Uiso 1 1 calc R U . . .
C64A C 0.7701(14) 0.6054(12) 0.8517(18) 0.059(2) Uani 0.223(8) 1 d D . P A 1
H64A H 0.757653 0.638201 0.793544 0.089 Uiso 0.223(8) 1 calc R U P A 1
H64B H 0.715964 0.595617 0.857220 0.089 Uiso 0.223(8) 1 calc R U P A 1
H64C H 0.810871 0.636868 0.907858 0.089 Uiso 0.223(8) 1 calc R U P A 1
C63A C 0.8309(18) 0.4662(16) 0.9369(14) 0.079(3) Uani 0.223(8) 1 d D . P A 1
H63A H 0.856425 0.412220 0.931099 0.119 Uiso 0.223(8) 1 calc R U P A 1
H63B H 0.872148 0.496612 0.993753 0.119 Uiso 0.223(8) 1 calc R U P A 1
H63C H 0.777241 0.455361 0.943116 0.119 Uiso 0.223(8) 1 calc R U P A 1
C62A C 0.9002(13) 0.5340(19) 0.8439(19) 0.075(3) Uani 0.223(8) 1 d D . P A 1
H62A H 0.924761 0.478746 0.840364 0.112 Uiso 0.223(8) 1 calc R U P A 1
H62B H 0.891982 0.567963 0.787688 0.112 Uiso 0.223(8) 1 calc R U P A 1
H62C H 0.940103 0.563571 0.902249 0.112 Uiso 0.223(8) 1 calc R U P A 1
C64B C 0.7593(4) 0.5720(5) 0.8927(5) 0.059(2) Uani 0.777(8) 1 d D . P A 2
H64D H 0.716290 0.609007 0.844408 0.089 Uiso 0.777(8) 1 calc R U P A 2
H64E H 0.729615 0.532321 0.917023 0.089 Uiso 0.777(8) 1 calc R U P A 2
H64F H 0.800360 0.606491 0.945780 0.089 Uiso 0.777(8) 1 calc R U P A 2
C63B C 0.8769(5) 0.4634(4) 0.9246(5) 0.079(3) Uani 0.777(8) 1 d D . P A 2
H63D H 0.846307 0.422206 0.945981 0.119 Uiso 0.777(8) 1 calc R U P A 2
H63E H 0.911662 0.433282 0.898331 0.119 Uiso 0.777(8) 1 calc R U P A 2
H63F H 0.915118 0.498285 0.979035 0.119 Uiso 0.777(8) 1 calc R U P A 2
C62B C 0.8550(5) 0.5876(5) 0.8096(5) 0.075(3) Uani 0.777(8) 1 d D . P A 2
H62D H 0.810833 0.622817 0.760177 0.112 Uiso 0.777(8) 1 calc R U P A 2
H62E H 0.893077 0.623482 0.863122 0.112 Uiso 0.777(8) 1 calc R U P A 2
H62F H 0.889621 0.558480 0.782418 0.112 Uiso 0.777(8) 1 calc R U P A 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
V1 O2 1.783(2) . ?
V1 O1 1.789(2) . ?
V1 N1 2.214(3) . ?
V1 N2 2.230(3) . ?
V1 Cl1 2.3162(12) . ?
V1 Cl2 2.3352(13) . ?
O1 C11 1.358(3) . ?
O2 C21 1.349(4) . ?
N1 C27 1.499(4) . ?
N1 C1 1.498(4) . ?
N1 C17 1.501(4) . ?
N2 C4 1.479(4) . ?
N2 C3 1.483(4) . ?
N2 C2 1.482(4) . ?
C27 C26 1.506(4) . ?
C27 H27A 0.9700 . ?
C27 H27B 0.9700 . ?
C11 C16 1.386(4) . ?
C11 C12 1.414(4) . ?
C21 C26 1.391(4) . ?
C21 C22 1.411(4) . ?
C31 C12 1.529(4) . ?
C31 C34 1.531(4) . ?
C31 C33 1.532(5) . ?
C31 C32 1.539(5) . ?
C16 C15 1.398(4) . ?
C16 C17 1.507(4) . ?
C1 C2 1.498(4) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C15 C14 1.380(4) . ?
C15 H15 0.9300 . ?
C25 C24 1.377(4) . ?
C25 C26 1.387(4) . ?
C25 H25 0.9300 . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C22 C23 1.388(5) . ?
C22 C51 1.540(5) . ?
C24 C23 1.405(4) . ?
C24 C61 1.537(5) . ?
C13 C12 1.386(4) . ?
C13 C14 1.397(4) . ?
C13 H13 0.9300 . ?
C23 H23 0.9300 . ?
C61 C64A 1.485(14) . ?
C61 C63B 1.515(6) . ?
C61 C63A 1.522(14) . ?
C61 C62B 1.522(6) . ?
C61 C64B 1.542(6) . ?
C61 C62A 1.546(13) . ?
C54 C51 1.537(4) . ?
C54 H54A 0.9600 . ?
C54 H54B 0.9600 . ?
C54 H54C 0.9600 . ?
C14 C41 1.535(4) . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C41 C44 1.513(5) . ?
C41 C43 1.524(5) . ?
C41 C42 1.537(5) . ?
C32 H32A 0.9600 . ?
C32 H32B 0.9600 . ?
C32 H32C 0.9600 . ?
C51 C53 1.532(5) . ?
C51 C52 1.537(5) . ?
C33 H33A 0.9600 . ?
C33 H33B 0.9600 . ?
C33 H33C 0.9600 . ?
C34 H34A 0.9600 . ?
C34 H34B 0.9600 . ?
C34 H34C 0.9600 . ?
C52 H52A 0.9600 . ?
C52 H52B 0.9600 . ?
C52 H52C 0.9600 . ?
C53 H53A 0.9600 . ?
C53 H53B 0.9600 . ?
C53 H53C 0.9600 . ?
C4 H4A 0.9600 . ?
C4 H4B 0.9600 . ?
C4 H4C 0.9600 . ?
C3 H3A 0.9600 . ?
C3 H3B 0.9600 . ?
C3 H3C 0.9600 . ?
C42 H42A 0.9600 . ?
C42 H42B 0.9600 . ?
C42 H42C 0.9600 . ?
C44 H44A 0.9600 . ?
C44 H44B 0.9600 . ?
C44 H44C 0.9600 . ?
C43 H43A 0.9600 . ?
C43 H43B 0.9600 . ?
C43 H43C 0.9600 . ?
C64A H64A 0.9600 . ?
C64A H64B 0.9600 . ?
C64A H64C 0.9600 . ?
C63A H63A 0.9600 . ?
C63A H63B 0.9600 . ?
C63A H63C 0.9600 . ?
C62A H62A 0.9600 . ?
C62A H62B 0.9600 . ?
C62A H62C 0.9600 . ?
C64B H64D 0.9600 . ?
C64B H64E 0.9600 . ?
C64B H64F 0.9600 . ?
C63B H63D 0.9600 . ?
C63B H63E 0.9600 . ?
C63B H63F 0.9600 . ?
C62B H62D 0.9600 . ?
C62B H62E 0.9600 . ?
C62B H62F 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
O2 V1 O1 169.37(10) . . ?
O2 V1 N1 86.53(10) . . ?
O1 V1 N1 82.92(9) . . ?
O2 V1 N2 87.61(10) . . ?
O1 V1 N2 92.02(10) . . ?
N1 V1 N2 80.84(10) . . ?
O2 V1 Cl1 95.91(8) . . ?
O1 V1 Cl1 94.72(8) . . ?
N1 V1 Cl1 170.64(8) . . ?
N2 V1 Cl1 90.22(8) . . ?
O2 V1 Cl2 89.68(8) . . ?
O1 V1 Cl2 89.39(7) . . ?
N1 V1 Cl2 92.22(8) . . ?
N2 V1 Cl2 172.68(8) . . ?
Cl1 V1 Cl2 96.82(5) . . ?
C11 O1 V1 143.8(2) . . ?
C21 O2 V1 145.8(2) . . ?
C27 N1 C1 110.4(2) . . ?
C27 N1 C17 103.7(2) . . ?
C1 N1 C17 108.5(2) . . ?
C27 N1 V1 115.43(18) . . ?
C1 N1 V1 105.85(19) . . ?
C17 N1 V1 112.90(18) . . ?
C4 N2 C3 106.9(3) . . ?
C4 N2 C2 108.3(2) . . ?
C3 N2 C2 109.7(2) . . ?
C4 N2 V1 113.33(19) . . ?
C3 N2 V1 112.06(19) . . ?
C2 N2 V1 106.5(2) . . ?
N1 C27 C26 120.4(3) . . ?
N1 C27 H27A 107.2 . . ?
C26 C27 H27A 107.2 . . ?
N1 C27 H27B 107.2 . . ?
C26 C27 H27B 107.2 . . ?
H27A C27 H27B 106.9 . . ?
O1 C11 C16 118.2(3) . . ?
O1 C11 C12 120.5(3) . . ?
C16 C11 C12 121.3(3) . . ?
O2 C21 C26 117.5(3) . . ?
O2 C21 C22 121.0(3) . . ?
C26 C21 C22 121.5(3) . . ?
C12 C31 C34 111.7(3) . . ?
C12 C31 C33 111.0(3) . . ?
C34 C31 C33 106.8(3) . . ?
C12 C31 C32 109.5(3) . . ?
C34 C31 C32 107.8(3) . . ?
C33 C31 C32 109.8(3) . . ?
C11 C16 C15 119.5(3) . . ?
C11 C16 C17 122.3(3) . . ?
C15 C16 C17 118.0(3) . . ?
C2 C1 N1 109.8(2) . . ?
C2 C1 H1A 109.7 . . ?
N1 C1 H1A 109.7 . . ?
C2 C1 H1B 109.7 . . ?
N1 C1 H1B 109.7 . . ?
H1A C1 H1B 108.2 . . ?
C14 C15 C16 121.4(3) . . ?
C14 C15 H15 119.3 . . ?
C16 C15 H15 119.3 . . ?
C24 C25 C26 122.0(3) . . ?
C24 C25 H25 119.0 . . ?
C26 C25 H25 119.0 . . ?
N2 C2 C1 110.6(2) . . ?
N2 C2 H2A 109.5 . . ?
C1 C2 H2A 109.5 . . ?
N2 C2 H2B 109.5 . . ?
C1 C2 H2B 109.5 . . ?
H2A C2 H2B 108.1 . . ?
C23 C22 C21 116.0(3) . . ?
C23 C22 C51 122.7(3) . . ?
C21 C22 C51 121.2(3) . . ?
C25 C24 C23 116.9(3) . . ?
C25 C24 C61 122.7(3) . . ?
C23 C24 C61 120.4(3) . . ?
C12 C13 C14 124.6(3) . . ?
C12 C13 H13 117.7 . . ?
C14 C13 H13 117.7 . . ?
C22 C23 C24 124.1(3) . . ?
C22 C23 H23 118.0 . . ?
C24 C23 H23 118.0 . . ?
C25 C26 C21 119.1(3) . . ?
C25 C26 C27 119.1(3) . . ?
C21 C26 C27 120.8(3) . . ?
C64A C61 C63A 111.5(14) . . ?
C63B C61 C62B 111.6(5) . . ?
C64A C61 C24 112.7(9) . . ?
C63B C61 C24 109.8(4) . . ?
C63A C61 C24 105.7(11) . . ?
C62B C61 C24 108.7(3) . . ?
C63B C61 C64B 107.9(4) . . ?
C62B C61 C64B 106.5(4) . . ?
C24 C61 C64B 112.2(3) . . ?
C64A C61 C62A 110.8(13) . . ?
C63A C61 C62A 104.8(13) . . ?
C24 C61 C62A 110.8(9) . . ?
C51 C54 H54A 109.5 . . ?
C51 C54 H54B 109.5 . . ?
H54A C54 H54B 109.5 . . ?
C51 C54 H54C 109.5 . . ?
H54A C54 H54C 109.5 . . ?
H54B C54 H54C 109.5 . . ?
C15 C14 C13 117.1(3) . . ?
C15 C14 C41 123.4(3) . . ?
C13 C14 C41 119.5(3) . . ?
N1 C17 C16 116.8(3) . . ?
N1 C17 H17A 108.1 . . ?
C16 C17 H17A 108.1 . . ?
N1 C17 H17B 108.1 . . ?
C16 C17 H17B 108.1 . . ?
H17A C17 H17B 107.3 . . ?
C44 C41 C43 108.8(3) . . ?
C44 C41 C14 112.7(3) . . ?
C43 C41 C14 109.2(3) . . ?
C44 C41 C42 107.4(3) . . ?
C43 C41 C42 109.7(4) . . ?
C14 C41 C42 109.1(3) . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C53 C51 C54 108.0(3) . . ?
C53 C51 C52 109.3(3) . . ?
C54 C51 C52 107.8(3) . . ?
C53 C51 C22 111.4(3) . . ?
C54 C51 C22 110.9(3) . . ?
C52 C51 C22 109.2(3) . . ?
C31 C33 H33A 109.5 . . ?
C31 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
C31 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C13 C12 C11 115.9(3) . . ?
C13 C12 C31 121.7(3) . . ?
C11 C12 C31 122.2(3) . . ?
C31 C34 H34A 109.5 . . ?
C31 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
C31 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C51 C52 H52A 109.5 . . ?
C51 C52 H52B 109.5 . . ?
H52A C52 H52B 109.5 . . ?
C51 C52 H52C 109.5 . . ?
H52A C52 H52C 109.5 . . ?
H52B C52 H52C 109.5 . . ?
C51 C53 H53A 109.5 . . ?
C51 C53 H53B 109.5 . . ?
H53A C53 H53B 109.5 . . ?
C51 C53 H53C 109.5 . . ?
H53A C53 H53C 109.5 . . ?
H53B C53 H53C 109.5 . . ?
N2 C4 H4A 109.5 . . ?
N2 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
N2 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
N2 C3 H3A 109.5 . . ?
N2 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
N2 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
C41 C42 H42A 109.5 . . ?
C41 C42 H42B 109.5 . . ?
H42A C42 H42B 109.5 . . ?
C41 C42 H42C 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
C41 C44 H44A 109.5 . . ?
C41 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
C41 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
C41 C43 H43A 109.5 . . ?
C41 C43 H43B 109.5 . . ?
H43A C43 H43B 109.5 . . ?
C41 C43 H43C 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
C61 C64A H64A 109.5 . . ?
C61 C64A H64B 109.5 . . ?
H64A C64A H64B 109.5 . . ?
C61 C64A H64C 109.5 . . ?
H64A C64A H64C 109.5 . . ?
H64B C64A H64C 109.5 . . ?
C61 C63A H63A 109.5 . . ?
C61 C63A H63B 109.5 . . ?
H63A C63A H63B 109.5 . . ?
C61 C63A H63C 109.5 . . ?
H63A C63A H63C 109.5 . . ?
H63B C63A H63C 109.5 . . ?
C61 C62A H62A 109.5 . . ?
C61 C62A H62B 109.5 . . ?
H62A C62A H62B 109.5 . . ?
C61 C62A H62C 109.5 . . ?
H62A C62A H62C 109.5 . . ?
H62B C62A H62C 109.5 . . ?
C61 C64B H64D 109.5 . . ?
C61 C64B H64E 109.5 . . ?
H64D C64B H64E 109.5 . . ?
C61 C64B H64F 109.5 . . ?
H64D C64B H64F 109.5 . . ?
H64E C64B H64F 109.5 . . ?
C61 C63B H63D 109.5 . . ?
C61 C63B H63E 109.5 . . ?
H63D C63B H63E 109.5 . . ?
C61 C63B H63F 109.5 . . ?
H63D C63B H63F 109.5 . . ?
H63E C63B H63F 109.5 . . ?
C61 C62B H62D 109.5 . . ?
C61 C62B H62E 109.5 . . ?
H62D C62B H62E 109.5 . . ?
C61 C62B H62F 109.5 . . ?
H62D C62B H62F 109.5 . . ?
H62E C62B H62F 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O2 V1 O1 C11 21.8(8) . . . . ?
N1 V1 O1 C11 29.1(3) . . . . ?
N2 V1 O1 C11 109.6(3) . . . . ?
Cl1 V1 O1 C11 -160.0(3) . . . . ?
Cl2 V1 O1 C11 -63.2(3) . . . . ?
O1 V1 O2 C21 12.2(8) . . . . ?
N1 V1 O2 C21 4.9(4) . . . . ?
N2 V1 O2 C21 -76.1(4) . . . . ?
Cl1 V1 O2 C21 -166.0(4) . . . . ?
Cl2 V1 O2 C21 97.1(4) . . . . ?
C1 N1 C27 C26 78.9(3) . . . . ?
C17 N1 C27 C26 -165.0(3) . . . . ?
V1 N1 C27 C26 -41.0(3) . . . . ?
V1 O1 C11 C16 -16.1(5) . . . . ?
V1 O1 C11 C12 163.3(3) . . . . ?
V1 O2 C21 C26 -4.6(5) . . . . ?
V1 O2 C21 C22 174.5(3) . . . . ?
O1 C11 C16 C15 -174.8(3) . . . . ?
C12 C11 C16 C15 5.7(5) . . . . ?
O1 C11 C16 C17 10.6(5) . . . . ?
C12 C11 C16 C17 -168.9(3) . . . . ?
C27 N1 C1 C2 -81.1(3) . . . . ?
C17 N1 C1 C2 165.9(3) . . . . ?
V1 N1 C1 C2 44.4(3) . . . . ?
C11 C16 C15 C14 -2.9(5) . . . . ?
C17 C16 C15 C14 171.9(3) . . . . ?
C4 N2 C2 C1 162.6(3) . . . . ?
C3 N2 C2 C1 -81.1(3) . . . . ?
V1 N2 C2 C1 40.4(3) . . . . ?
N1 C1 C2 N2 -59.4(3) . . . . ?
O2 C21 C22 C23 -172.4(3) . . . . ?
C26 C21 C22 C23 6.6(5) . . . . ?
O2 C21 C22 C51 11.5(5) . . . . ?
C26 C21 C22 C51 -169.5(3) . . . . ?
C26 C25 C24 C23 1.1(5) . . . . ?
C26 C25 C24 C61 179.8(3) . . . . ?
C21 C22 C23 C24 -1.6(5) . . . . ?
C51 C22 C23 C24 174.4(3) . . . . ?
C25 C24 C23 C22 -2.1(5) . . . . ?
C61 C24 C23 C22 179.2(3) . . . . ?
C24 C25 C26 C21 3.7(5) . . . . ?
C24 C25 C26 C27 -165.2(3) . . . . ?
O2 C21 C26 C25 171.3(3) . . . . ?
C22 C21 C26 C25 -7.8(5) . . . . ?
O2 C21 C26 C27 -19.9(5) . . . . ?
C22 C21 C26 C27 161.0(3) . . . . ?
N1 C27 C26 C25 -146.6(3) . . . . ?
N1 C27 C26 C21 44.6(4) . . . . ?
C25 C24 C61 C64A -42.2(13) . . . . ?
C23 C24 C61 C64A 136.4(12) . . . . ?
C25 C24 C61 C63B 114.7(5) . . . . ?
C23 C24 C61 C63B -66.7(6) . . . . ?
C25 C24 C61 C63A 79.8(12) . . . . ?
C23 C24 C61 C63A -101.5(12) . . . . ?
C25 C24 C61 C62B -122.9(5) . . . . ?
C23 C24 C61 C62B 55.7(6) . . . . ?
C25 C24 C61 C64B -5.3(6) . . . . ?
C23 C24 C61 C64B 173.3(4) . . . . ?
C25 C24 C61 C62A -167.1(13) . . . . ?
C23 C24 C61 C62A 11.5(14) . . . . ?
C16 C15 C14 C13 -0.5(5) . . . . ?
C16 C15 C14 C41 -179.8(3) . . . . ?
C12 C13 C14 C15 1.3(5) . . . . ?
C12 C13 C14 C41 -179.4(3) . . . . ?
C27 N1 C17 C16 -179.4(3) . . . . ?
C1 N1 C17 C16 -62.1(3) . . . . ?
V1 N1 C17 C16 54.9(3) . . . . ?
C11 C16 C17 N1 -36.9(4) . . . . ?
C15 C16 C17 N1 148.4(3) . . . . ?
C15 C14 C41 C44 -3.6(5) . . . . ?
C13 C14 C41 C44 177.1(3) . . . . ?
C15 C14 C41 C43 -124.6(4) . . . . ?
C13 C14 C41 C43 56.1(5) . . . . ?
C15 C14 C41 C42 115.5(4) . . . . ?
C13 C14 C41 C42 -63.7(4) . . . . ?
C23 C22 C51 C53 120.6(4) . . . . ?
C21 C22 C51 C53 -63.6(4) . . . . ?
C23 C22 C51 C54 0.2(5) . . . . ?
C21 C22 C51 C54 176.0(3) . . . . ?
C23 C22 C51 C52 -118.5(4) . . . . ?
C21 C22 C51 C52 57.3(4) . . . . ?
C14 C13 C12 C11 1.3(5) . . . . ?
C14 C13 C12 C31 -174.7(3) . . . . ?
O1 C11 C12 C13 175.7(3) . . . . ?
C16 C11 C12 C13 -4.8(5) . . . . ?
O1 C11 C12 C31 -8.3(5) . . . . ?
C16 C11 C12 C31 171.2(3) . . . . ?
C34 C31 C12 C13 -2.7(5) . . . . ?
C33 C31 C12 C13 -121.9(3) . . . . ?
C32 C31 C12 C13 116.7(3) . . . . ?
C34 C31 C12 C11 -178.5(3) . . . . ?
C33 C31 C12 C11 62.4(4) . . . . ?
C32 C31 C12 C11 -59.1(4) . . . . ?

_refine_diff_density_max         0.440
_refine_diff_density_min         -0.334
_refine_diff_density_rms         0.068

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_8
_database_code_depnum_ccdc_archive 'CCDC 1536784'
_audit_update_record             
;
2017-06-28 deposited with the CCDC.
2017-06-30 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         'C40 H65 N2 O4 V'
_chemical_formula_sum            'C40 H65 N2 O4 V'
_chemical_melting_point          ?

_exptl_crystal_description       block
_exptl_crystal_colour            brown
_diffrn_ambient_temperature      293(2)
_chemical_formula_weight         688.88

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

_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_H-M_alt        'P 21'
_space_group_name_Hall           'P 2yb'
_chemical_absolute_configuration syn

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

_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.
;

_cell_length_a                   15.5180(11)
_cell_length_b                   23.5210(10)
_cell_length_c                   21.8270(10)
_cell_angle_alpha                90
_cell_angle_beta                 100.875(2)
_cell_angle_gamma                90
_cell_volume                     7823.8(7)
_cell_formula_units_Z            8
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    8434
_cell_measurement_theta_min      2.19
_cell_measurement_theta_max      24.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.170
_exptl_crystal_F_000             2992
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.040
_exptl_absorpt_coefficient_mu    0.293
_shelx_estimated_absorpt_T_min   0.949
_shelx_estimated_absorpt_T_max   0.988
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9491
_exptl_absorpt_correction_T_max  0.9884
_exptl_absorpt_process_details   'SADABS,  G. M. Sheldrick, 1996'
_exptl_absorpt_special_details   ?
_diffrn_radiation_probe          ?
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            48637
_diffrn_reflns_av_unetI/netI     0.0921
_diffrn_reflns_av_R_equivalents  0.0482
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         1.979
_diffrn_reflns_theta_max         25.108
_diffrn_reflns_theta_full        25.108
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measured_fraction_theta_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.893
_diffrn_reflns_point_group_measured_fraction_full 0.893
_reflns_number_total             24927
_reflns_number_gt                18919
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.756
_reflns_Friedel_fraction_max     0.790
_reflns_Friedel_fraction_full    0.790

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Sir2004 (M.C. Burla et al, 2005)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    
'Ortep3 for Windows v2.0 (L.J. Farrugia, J. Appl. Cryst. (1997) 30, 565)'
_computing_publication_material  'enCIFer v1.6'

_refine_special_details          
;
Two of the tBu fragments present disordered methyl groups. Disorder models were applied to the methyl groups attached to C61 and C141 giving 47/53% and 39/61% occupancies, respectively. SADI restraints and EADP constraints were applied on the disordered atoms. ISOR restraints were used on atoms C143 and C146 to prevent them from turning non-positive definite.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0436P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 6772 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.004(10)
_refine_ls_number_reflns         24927
_refine_ls_number_parameters     1713
_refine_ls_number_restraints     43
_refine_ls_R_factor_all          0.0761
_refine_ls_R_factor_gt           0.0492
_refine_ls_wR_factor_ref         0.1046
_refine_ls_wR_factor_gt          0.0965
_refine_ls_goodness_of_fit_ref   0.976
_refine_ls_restrained_S_all      0.980
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
V2 V 0.31163(5) 0.56920(4) 0.96084(4) 0.0210(2) Uani 1 1 d . . . . .
V1 V 0.74220(5) 0.38125(4) 0.93595(3) 0.0186(2) Uani 1 1 d . . . . .
V4 V 0.12785(6) 0.46995(4) 0.56043(4) 0.0238(2) Uani 1 1 d . . . . .
V3 V 0.24667(6) 0.16720(4) 0.45048(4) 0.0233(2) Uani 1 1 d . . . . .
O1 O 0.7658(2) 0.39410(14) 1.02335(13) 0.0173(8) Uani 1 1 d . . . . .
O202 O 0.2938(2) 0.15619(15) 0.53666(13) 0.0235(8) Uani 1 1 d . . . . .
O2 O 0.7244(2) 0.34292(14) 0.85724(13) 0.0202(8) Uani 1 1 d . . . . .
O101 O 0.4067(2) 0.57438(16) 0.91695(14) 0.0244(8) Uani 1 1 d . . . . .
O3 O 0.8089(2) 0.43643(15) 0.91515(13) 0.0230(8) Uani 1 1 d . . . . .
O201 O 0.2076(2) 0.20440(16) 0.37352(14) 0.0245(9) Uani 1 1 d . . . . .
O303 O 0.2139(2) 0.47332(16) 0.62668(14) 0.0272(9) Uani 1 1 d . . . . .
O103 O 0.2314(2) 0.55981(15) 0.89291(14) 0.0239(8) Uani 1 1 d . . . . .
O102 O 0.2434(2) 0.54532(14) 1.02042(14) 0.0215(8) Uani 1 1 d . . . . .
O301 O 0.1969(2) 0.49718(15) 0.50283(14) 0.0254(9) Uani 1 1 d . . . . .
O304 O 0.1228(2) 0.40626(15) 0.53521(14) 0.0274(9) Uani 1 1 d . . . . .
O302 O 0.0339(2) 0.46314(16) 0.60440(14) 0.0258(8) Uani 1 1 d . . . . .
O104 O 0.3120(2) 0.63493(15) 0.97874(14) 0.0252(8) Uani 1 1 d . . . . .
O4 O 0.6442(2) 0.40422(14) 0.92547(13) 0.0228(8) Uani 1 1 d . . . . .
O203 O 0.3174(2) 0.11994(16) 0.42059(14) 0.0290(9) Uani 1 1 d . . . . .
N301 N 0.0231(3) 0.50124(19) 0.48375(18) 0.0246(10) Uani 1 1 d . . . . .
N1 N 0.7146(3) 0.29496(18) 0.97224(16) 0.0188(10) Uani 1 1 d . . . . .
N201 N 0.1976(3) 0.24883(18) 0.48382(17) 0.0209(10) Uani 1 1 d . . . . .
N102 N 0.3316(3) 0.46538(19) 0.95421(18) 0.0258(10) Uani 1 1 d . . . . .
C14 C 0.4816(3) 0.2644(2) 0.7975(2) 0.0208(12) Uani 1 1 d . . . . .
N2 N 0.8849(3) 0.33207(18) 0.95820(17) 0.0221(10) Uani 1 1 d . . . . .
C11 C 0.6455(3) 0.3182(2) 0.8346(2) 0.0177(12) Uani 1 1 d . . . . .
N101 N 0.4244(3) 0.54831(18) 1.03712(17) 0.0223(10) Uani 1 1 d . . . . .
O204 O 0.1569(2) 0.13392(16) 0.45077(14) 0.0282(9) Uani 1 1 d . . . . .
C211 C 0.1283(3) 0.2267(2) 0.3497(2) 0.0230(12) Uani 1 1 d . . . . .
C213 C 0.0164(3) 0.2521(2) 0.2615(2) 0.0227(13) Uani 1 1 d . . . . .
H213 H -0.003833 0.252011 0.218563 0.027 Uiso 1 1 calc R U . . .
N302 N 0.1154(3) 0.5706(2) 0.58155(18) 0.0297(11) Uani 1 1 d . . . . .
C16 C 0.6213(3) 0.2731(2) 0.86896(19) 0.0165(11) Uani 1 1 d . . . . .
C111 C 0.4772(3) 0.6097(2) 0.9298(2) 0.0244(13) Uani 1 1 d . . . . .
C1 C 0.7930(3) 0.2742(2) 1.0162(2) 0.0234(13) Uani 1 1 d . . . . .
H1A H 0.782815 0.235201 1.027531 0.028 Uiso 1 1 calc R U . . .
H1B H 0.800941 0.296912 1.053865 0.028 Uiso 1 1 calc R U . . .
C215 C -0.0012(3) 0.2796(2) 0.3622(2) 0.0252(13) Uani 1 1 d . . . . .
H215 H -0.033347 0.297692 0.388464 0.030 Uiso 1 1 calc R U . . .
C22 C 0.7066(3) 0.4320(2) 1.1087(2) 0.0226(12) Uani 1 1 d . . . . .
C13 C 0.5107(3) 0.3080(2) 0.7632(2) 0.0220(12) Uani 1 1 d . . . . .
H13 H 0.472776 0.319865 0.727232 0.026 Uiso 1 1 calc R U . . .
C15 C 0.5396(3) 0.2474(2) 0.8506(2) 0.0204(12) Uani 1 1 d . . . . .
H15 H 0.523509 0.218102 0.874743 0.025 Uiso 1 1 calc R U . . .
C216 C 0.0776(3) 0.2531(2) 0.3882(2) 0.0218(12) Uani 1 1 d . . . . .
C2 C 0.8770(3) 0.2765(2) 0.9892(2) 0.0213(12) Uani 1 1 d . . . . .
H2 H 0.876816 0.245618 0.959121 0.026 Uiso 1 1 calc R U . . .
N202 N 0.3730(3) 0.2345(2) 0.46336(17) 0.0262(11) Uani 1 1 d . . . . .
C121 C 0.2478(3) 0.5723(2) 1.0760(2) 0.0218(12) Uani 1 1 d . . . . .
C217 C 0.1018(3) 0.2534(2) 0.4585(2) 0.0250(13) Uani 1 1 d . . . . .
H21A H 0.080103 0.288243 0.473920 0.030 Uiso 1 1 calc R U . . .
H21B H 0.072171 0.221913 0.474518 0.030 Uiso 1 1 calc R U . . .
C31 C 0.6166(3) 0.3818(2) 0.7362(2) 0.0218(12) Uani 1 1 d . . . . .
C314 C 0.1838(3) 0.4472(2) 0.3173(2) 0.0261(13) Uani 1 1 d . . . . .
C322 C -0.0630(3) 0.3871(2) 0.6228(2) 0.0258(13) Uani 1 1 d . . . . .
C311 C 0.1933(3) 0.4800(2) 0.4435(2) 0.0239(13) Uani 1 1 d . . . . .
C124 C 0.2726(3) 0.6287(2) 1.1918(2) 0.0244(13) Uani 1 1 d . . . . .
C27 C 0.6411(3) 0.3001(2) 1.0068(2) 0.0209(12) Uani 1 1 d . . . . .
H27A H 0.632167 0.263253 1.024507 0.025 Uiso 1 1 calc R U . . .
H27B H 0.588252 0.309221 0.977032 0.025 Uiso 1 1 calc R U . . .
C325 C -0.1596(3) 0.4079(2) 0.5027(2) 0.0266(13) Uani 1 1 d . . . . .
H325 H -0.191841 0.415402 0.463168 0.032 Uiso 1 1 calc R U . . .
C21 C 0.7078(3) 0.3899(2) 1.06222(19) 0.0190(12) Uani 1 1 d . . . . .
C122 C 0.1742(3) 0.5955(2) 1.0955(2) 0.0205(12) Uani 1 1 d . . . . .
C312 C 0.2707(3) 0.4778(2) 0.4176(2) 0.0248(13) Uani 1 1 d . . . . .
C61 C 0.5348(3) 0.3680(2) 1.1971(2) 0.0309(15) Uani 1 1 d D . . . .
C26 C 0.6514(3) 0.3433(2) 1.0584(2) 0.0213(12) Uani 1 1 d . . . . .
C321 C -0.0372(3) 0.4297(2) 0.5855(2) 0.0253(13) Uani 1 1 d . . . . .
C41 C 0.3897(3) 0.2388(2) 0.7765(2) 0.0275(13) Uani 1 1 d . . . . .
C225 C 0.1267(3) 0.1975(2) 0.6236(2) 0.0262(13) Uani 1 1 d . . . . .
H225 H 0.092000 0.229166 0.626708 0.031 Uiso 1 1 calc R U . . .
C12 C 0.5910(3) 0.3351(2) 0.7780(2) 0.0184(12) Uani 1 1 d . . . . .
C126 C 0.3307(3) 0.5739(2) 1.1155(2) 0.0221(12) Uani 1 1 d . . . . .
C241 C -0.1228(3) 0.3077(2) 0.2721(2) 0.0263(13) Uani 1 1 d . . . . .
C23 C 0.6495(3) 0.4234(2) 1.1504(2) 0.0253(13) Uani 1 1 d . . . . .
H23 H 0.647495 0.450959 1.180666 0.030 Uiso 1 1 calc R U . . .
C6 C 0.9168(3) 0.3249(2) 0.8985(2) 0.0275(14) Uani 1 1 d . . . . .
H6A H 0.921175 0.362174 0.880391 0.033 Uiso 1 1 calc R U . . .
H6B H 0.873008 0.303610 0.869875 0.033 Uiso 1 1 calc R U . . .
C227 C 0.2093(3) 0.2522(2) 0.5532(2) 0.0259(13) Uani 1 1 d . . . . .
H22A H 0.172740 0.282691 0.563964 0.031 Uiso 1 1 calc R U . . .
H22B H 0.269866 0.262028 0.570036 0.031 Uiso 1 1 calc R U . . .
C323 C -0.1364(3) 0.3546(2) 0.5967(2) 0.0299(14) Uani 1 1 d . . . . .
H323 H -0.153908 0.325760 0.620735 0.036 Uiso 1 1 calc R U . . .
C222 C 0.2358(3) 0.1031(2) 0.6151(2) 0.0235(12) Uani 1 1 d . . . . .
C113 C 0.5879(3) 0.6675(2) 0.8971(2) 0.0305(14) Uani 1 1 d . . . . .
H113 H 0.611766 0.683635 0.865075 0.037 Uiso 1 1 calc R U . . .
C309 C 0.2928(4) 0.3835(3) 0.6378(2) 0.0364(14) Uani 1 1 d . . . . .
H30A H 0.344881 0.365740 0.660513 0.055 Uiso 1 1 calc R U . . .
H30B H 0.242069 0.363627 0.645899 0.055 Uiso 1 1 calc R U . . .
H30C H 0.293586 0.382297 0.593988 0.055 Uiso 1 1 calc R U . . .
C226 C 0.1872(3) 0.1987(2) 0.5839(2) 0.0217(12) Uani 1 1 d . . . . .
C5 C 0.9480(3) 0.3669(2) 1.0033(2) 0.0265(13) Uani 1 1 d . . . . .
H5A H 0.997461 0.378024 0.984649 0.032 Uiso 1 1 calc R U . . .
H5B H 0.919378 0.401153 1.014205 0.032 Uiso 1 1 calc R U . . .
C101 C 0.4728(3) 0.4988(2) 1.0183(2) 0.0256(13) Uani 1 1 d . . . . .
H10A H 0.518329 0.487702 1.053025 0.031 Uiso 1 1 calc R U . . .
H10B H 0.501012 0.509954 0.984091 0.031 Uiso 1 1 calc R U . . .
C123 C 0.1899(3) 0.6232(2) 1.1529(2) 0.0247(13) Uani 1 1 d . . . . .
H123 H 0.142051 0.639215 1.166510 0.030 Uiso 1 1 calc R U . . .
C331 C 0.3607(3) 0.4948(3) 0.4566(2) 0.0306(14) Uani 1 1 d . . . . .
C223 C 0.1739(3) 0.1040(2) 0.6542(2) 0.0269(13) Uani 1 1 d . . . . .
H223 H 0.170030 0.072173 0.678886 0.032 Uiso 1 1 calc R U . . .
C341 C 0.1819(4) 0.4285(2) 0.2496(2) 0.0281(13) Uani 1 1 d . . . . .
C151 C 0.0814(3) 0.5865(2) 1.0582(2) 0.0243(13) Uani 1 1 d . . . . .
C25 C 0.5965(3) 0.3372(2) 1.1019(2) 0.0238(13) Uani 1 1 d . . . . .
H25 H 0.559442 0.305821 1.098883 0.029 Uiso 1 1 calc R U . . .
C24 C 0.5955(3) 0.3759(3) 1.1491(2) 0.0272(13) Uani 1 1 d . . . . .
C114 C 0.6292(4) 0.6791(2) 0.9586(2) 0.0298(14) Uani 1 1 d . . . . .
C129 C 0.4825(3) 0.5981(2) 1.0471(2) 0.0246(13) Uani 1 1 d . . . . .
H12A H 0.532283 0.588755 1.079571 0.030 Uiso 1 1 calc R U . . .
H12B H 0.450959 0.628813 1.062680 0.030 Uiso 1 1 calc R U . . .
C212 C 0.0952(3) 0.2238(2) 0.2847(2) 0.0243(13) Uani 1 1 d . . . . .
C127 C 0.3982(3) 0.5359(2) 1.0981(2) 0.0262(13) Uani 1 1 d . . . . .
H12C H 0.376476 0.497123 1.096966 0.031 Uiso 1 1 calc R U . . .
H12D H 0.450157 0.537802 1.130603 0.031 Uiso 1 1 calc R U . . .
C17 C 0.6873(3) 0.2517(2) 0.9215(2) 0.0225(12) Uani 1 1 d . . . . .
H17A H 0.738832 0.239588 0.905856 0.027 Uiso 1 1 calc R U . . .
H17B H 0.663648 0.218739 0.939253 0.027 Uiso 1 1 calc R U . . .
C51 C 0.7636(3) 0.4857(2) 1.1128(2) 0.0238(13) Uani 1 1 d . . . . .
C152 C 0.0624(4) 0.5225(2) 1.0536(2) 0.0310(14) Uani 1 1 d . . . . .
H15A H 0.105406 0.503963 1.034144 0.047 Uiso 1 1 calc R U . . .
H15B H 0.064971 0.507190 1.094670 0.047 Uiso 1 1 calc R U . . .
H15C H 0.005008 0.516213 1.029084 0.047 Uiso 1 1 calc R U . . .
C301 C 0.0381(3) 0.5623(2) 0.4707(2) 0.0280(13) Uani 1 1 d . . . . .
H30D H -0.012160 0.576855 0.441681 0.034 Uiso 1 1 calc R U . . .
H30E H 0.089094 0.565500 0.451144 0.034 Uiso 1 1 calc R U . . .
C7 C 1.0055(4) 0.2947(3) 0.9029(2) 0.0385(16) Uani 1 1 d . . . . .
H7A H 1.019974 0.292222 0.862164 0.058 Uiso 1 1 calc R U . . .
H7B H 1.050083 0.315845 0.929987 0.058 Uiso 1 1 calc R U . . .
H7C H 1.001783 0.257120 0.919443 0.058 Uiso 1 1 calc R U . . .
C351 C -0.0149(3) 0.3785(3) 0.6911(2) 0.0311(14) Uani 1 1 d . . . . .
C3 C 0.9565(3) 0.2707(2) 1.0416(2) 0.0305(14) Uani 1 1 d . . . . .
H3A H 1.004739 0.252222 1.027015 0.037 Uiso 1 1 calc R U . . .
H3B H 0.942208 0.249313 1.076312 0.037 Uiso 1 1 calc R U . . .
C112 C 0.5144(3) 0.6339(2) 0.8807(2) 0.0227(12) Uani 1 1 d . . . . .
C125 C 0.3423(3) 0.6023(2) 1.1721(2) 0.0243(13) Uani 1 1 d . . . . .
H125 H 0.397775 0.603703 1.197171 0.029 Uiso 1 1 calc R U . . .
C102 C 0.4138(3) 0.4483(2) 0.9983(2) 0.0260(13) Uani 1 1 d . . . . .
H102 H 0.398400 0.430187 1.035145 0.031 Uiso 1 1 calc R U . . .
C214 C -0.0332(3) 0.2800(2) 0.2985(2) 0.0225(12) Uani 1 1 d . . . . .
C116 C 0.5172(3) 0.6199(2) 0.9912(2) 0.0236(13) Uani 1 1 d . . . . .
C317 C 0.0273(3) 0.4667(2) 0.4277(2) 0.0238(12) Uani 1 1 d . . . . .
H31A H -0.017740 0.480223 0.393838 0.029 Uiso 1 1 calc R U . . .
H31B H 0.012778 0.427721 0.436259 0.029 Uiso 1 1 calc R U . . .
C43 C 0.3726(4) 0.2273(3) 0.7062(2) 0.0395(16) Uani 1 1 d . . . . .
H43A H 0.415554 0.201047 0.696706 0.059 Uiso 1 1 calc R U . . .
H43B H 0.315012 0.211449 0.693478 0.059 Uiso 1 1 calc R U . . .
H43C H 0.376524 0.262348 0.684249 0.059 Uiso 1 1 calc R U . . .
C224 C 0.1178(3) 0.1493(2) 0.6585(2) 0.0271(13) Uani 1 1 d . . . . .
C232 C 0.1416(4) 0.1884(3) 0.2415(2) 0.0300(14) Uani 1 1 d . . . . .
C324 C -0.1844(3) 0.3629(2) 0.5372(2) 0.0275(13) Uani 1 1 d . . . . .
C313 C 0.2635(3) 0.4619(2) 0.3560(2) 0.0287(13) Uani 1 1 d . . . . .
H313 H 0.314254 0.460991 0.339245 0.034 Uiso 1 1 calc R U . . .
C326 C -0.0877(3) 0.4418(2) 0.5262(2) 0.0251(13) Uani 1 1 d . . . . .
C316 C 0.1130(3) 0.4663(2) 0.4054(2) 0.0234(12) Uani 1 1 d . . . . .
C361 C -0.2639(4) 0.3269(3) 0.5101(2) 0.0351(15) Uani 1 1 d . . . . .
C315 C 0.1106(3) 0.4506(2) 0.3437(2) 0.0262(13) Uani 1 1 d . . . . .
H315 H 0.056549 0.441916 0.319130 0.031 Uiso 1 1 calc R U . . .
C115 C 0.5919(3) 0.6540(2) 1.0042(2) 0.0306(14) Uani 1 1 d . . . . .
H115 H 0.617853 0.660012 1.045654 0.037 Uiso 1 1 calc R U . . .
C327 C -0.0682(3) 0.4961(2) 0.4965(2) 0.0264(13) Uani 1 1 d . . . . .
H32A H -0.078301 0.527285 0.523370 0.032 Uiso 1 1 calc R U . . .
H32B H -0.109400 0.500275 0.457407 0.032 Uiso 1 1 calc R U . . .
C33 C 0.7105(3) 0.3737(3) 0.7258(2) 0.0331(14) Uani 1 1 d . . . . .
H33A H 0.715379 0.337500 0.706320 0.050 Uiso 1 1 calc R U . . .
H33B H 0.724842 0.403426 0.699351 0.050 Uiso 1 1 calc R U . . .
H33C H 0.750279 0.374921 0.765210 0.050 Uiso 1 1 calc R U . . .
C308 C 0.2895(4) 0.4447(3) 0.6585(2) 0.0347(15) Uani 1 1 d . . . . .
H308 H 0.340637 0.464027 0.647916 0.042 Uiso 1 1 calc R U . . .
C221 C 0.2390(3) 0.1514(2) 0.5779(2) 0.0236(13) Uani 1 1 d . . . . .
C244 C -0.1295(4) 0.3668(2) 0.3004(2) 0.0369(15) Uani 1 1 d . . . . .
H24A H -0.120849 0.363749 0.344993 0.055 Uiso 1 1 calc R U . . .
H24B H -0.085416 0.391204 0.289155 0.055 Uiso 1 1 calc R U . . .
H24C H -0.186559 0.382501 0.284746 0.055 Uiso 1 1 calc R U . . .
C161 C 0.2818(3) 0.6581(2) 1.2553(2) 0.0283(13) Uani 1 1 d . . . . .
C251 C 0.3016(3) 0.0544(2) 0.6172(2) 0.0268(13) Uani 1 1 d . . . . .
C253 C 0.3088(4) 0.0328(2) 0.5522(2) 0.0287(14) Uani 1 1 d . . . . .
H25A H 0.323157 0.063978 0.527480 0.043 Uiso 1 1 calc R U . . .
H25B H 0.353952 0.004472 0.555784 0.043 Uiso 1 1 calc R U . . .
H25C H 0.253793 0.016571 0.532433 0.043 Uiso 1 1 calc R U . . .
C53 C 0.8599(3) 0.4697(3) 1.1320(2) 0.0331(14) Uani 1 1 d . . . . .
H53A H 0.875054 0.442494 1.103070 0.050 Uiso 1 1 calc R U . . .
H53B H 0.895431 0.503129 1.132007 0.050 Uiso 1 1 calc R U . . .
H53C H 0.869932 0.453520 1.173125 0.050 Uiso 1 1 calc R U . . .
C34 C 0.5574(4) 0.3830(3) 0.6713(2) 0.0402(16) Uani 1 1 d . . . . .
H34A H 0.562202 0.347464 0.650513 0.060 Uiso 1 1 calc R U . . .
H34B H 0.497629 0.388818 0.675616 0.060 Uiso 1 1 calc R U . . .
H34C H 0.575399 0.413395 0.647204 0.060 Uiso 1 1 calc R U . . .
C203 C 0.3762(4) 0.3311(3) 0.4244(3) 0.0406(16) Uani 1 1 d . . . . .
H20A H 0.434559 0.345425 0.441047 0.049 Uiso 1 1 calc R U . . .
H20B H 0.337375 0.362964 0.411167 0.049 Uiso 1 1 calc R U . . .
C305 C 0.2027(4) 0.5991(3) 0.5836(3) 0.0366(15) Uani 1 1 d . . . . .
H30F H 0.246930 0.571186 0.578614 0.044 Uiso 1 1 calc R U . . .
H30G H 0.221230 0.618432 0.623098 0.044 Uiso 1 1 calc R U . . .
C333 C 0.3840(3) 0.4589(3) 0.5165(2) 0.0379(16) Uani 1 1 d . . . . .
H33D H 0.385214 0.419434 0.505707 0.057 Uiso 1 1 calc R U . . .
H33E H 0.440586 0.470122 0.539218 0.057 Uiso 1 1 calc R U . . .
H33F H 0.340680 0.464945 0.542000 0.057 Uiso 1 1 calc R U . . .
C54 C 0.7422(4) 0.5290(3) 1.1600(2) 0.0412(16) Uani 1 1 d . . . . .
H54A H 0.681588 0.539776 1.148957 0.062 Uiso 1 1 calc R U . . .
H54B H 0.753033 0.512374 1.200946 0.062 Uiso 1 1 calc R U . . .
H54C H 0.778532 0.561983 1.159829 0.062 Uiso 1 1 calc R U . . .
C202 C 0.3417(4) 0.2945(2) 0.4723(2) 0.0307(14) Uani 1 1 d . . . . .
H202 H 0.365921 0.307765 0.514651 0.037 Uiso 1 1 calc R U . . .
C52 C 0.7489(4) 0.5163(2) 1.0494(2) 0.0368(15) Uani 1 1 d . . . . .
H52A H 0.688050 0.526364 1.037369 0.055 Uiso 1 1 calc R U . . .
H52B H 0.784072 0.550157 1.052835 0.055 Uiso 1 1 calc R U . . .
H52C H 0.765268 0.491630 1.018557 0.055 Uiso 1 1 calc R U . . .
C106 C 0.2572(3) 0.4313(2) 0.9708(3) 0.0328(14) Uani 1 1 d . . . . .
H10C H 0.272228 0.391349 0.970100 0.039 Uiso 1 1 calc R U . . .
H10D H 0.252139 0.440692 1.013305 0.039 Uiso 1 1 calc R U . . .
C243 C -0.1371(4) 0.3146(3) 0.2011(2) 0.0367(15) Uani 1 1 d . . . . .
H24D H -0.133230 0.278081 0.182120 0.055 Uiso 1 1 calc R U . . .
H24E H -0.194045 0.330627 0.186179 0.055 Uiso 1 1 calc R U . . .
H24F H -0.092903 0.339330 0.190589 0.055 Uiso 1 1 calc R U . . .
C332 C 0.4358(4) 0.4878(3) 0.4198(3) 0.0454(18) Uani 1 1 d . . . . .
H33G H 0.439123 0.448762 0.407520 0.068 Uiso 1 1 calc R U . . .
H33H H 0.424713 0.511445 0.383350 0.068 Uiso 1 1 calc R U . . .
H33I H 0.490352 0.498712 0.445726 0.068 Uiso 1 1 calc R U . . .
C264 C 0.0852(4) 0.1857(3) 0.7587(2) 0.0495(18) Uani 1 1 d . . . . .
H26A H 0.095541 0.223428 0.745073 0.074 Uiso 1 1 calc R U . . .
H26B H 0.042655 0.186984 0.785442 0.074 Uiso 1 1 calc R U . . .
H26C H 0.139092 0.170036 0.781304 0.074 Uiso 1 1 calc R U . . .
C201 C 0.2417(3) 0.2981(2) 0.4600(2) 0.0288(13) Uani 1 1 d . . . . .
H20C H 0.224756 0.332496 0.479218 0.035 Uiso 1 1 calc R U . . .
H20D H 0.220618 0.301222 0.415423 0.035 Uiso 1 1 calc R U . . .
C131 C 0.4730(4) 0.6242(3) 0.8115(2) 0.0322(14) Uani 1 1 d . . . . .
C242 C -0.1956(3) 0.2689(3) 0.2876(3) 0.0370(15) Uani 1 1 d . . . . .
H24G H -0.187733 0.264073 0.331988 0.056 Uiso 1 1 calc R U . . .
H24H H -0.251812 0.285898 0.272366 0.056 Uiso 1 1 calc R U . . .
H24I H -0.192721 0.232518 0.268151 0.056 Uiso 1 1 calc R U . . .
C261 C 0.0512(4) 0.1489(3) 0.7029(2) 0.0320(14) Uani 1 1 d . . . . .
C204 C 0.3775(4) 0.2895(3) 0.3706(3) 0.0422(16) Uani 1 1 d . . . . .
H20E H 0.319234 0.284301 0.345766 0.051 Uiso 1 1 calc R U . . .
H20F H 0.416921 0.302251 0.343894 0.051 Uiso 1 1 calc R U . . .
C254 C 0.2787(4) 0.0032(3) 0.6544(2) 0.0424(17) Uani 1 1 d . . . . .
H25D H 0.321697 -0.026131 0.654363 0.064 Uiso 1 1 calc R U . . .
H25E H 0.278142 0.014577 0.696578 0.064 Uiso 1 1 calc R U . . .
H25F H 0.221809 -0.010993 0.635614 0.064 Uiso 1 1 calc R U . . .
C304 C 0.1901(4) 0.6415(3) 0.5300(3) 0.0460(17) Uani 1 1 d . . . . .
H30H H 0.224888 0.675429 0.541534 0.055 Uiso 1 1 calc R U . . .
H30I H 0.206608 0.624891 0.493234 0.055 Uiso 1 1 calc R U . . .
C262 C -0.0382(4) 0.1714(3) 0.6674(3) 0.0442(16) Uani 1 1 d . . . . .
H26D H -0.058885 0.147541 0.632043 0.066 Uiso 1 1 calc R U . . .
H26E H -0.079957 0.171170 0.694743 0.066 Uiso 1 1 calc R U . . .
H26F H -0.031113 0.209568 0.653511 0.066 Uiso 1 1 calc R U . . .
C42 C 0.3806(4) 0.1819(3) 0.8086(2) 0.0413(16) Uani 1 1 d . . . . .
H42A H 0.423484 0.155722 0.798916 0.062 Uiso 1 1 calc R U . . .
H42B H 0.389658 0.187501 0.852928 0.062 Uiso 1 1 calc R U . . .
H42C H 0.322826 0.166865 0.794096 0.062 Uiso 1 1 calc R U . . .
C164 C 0.2452(4) 0.6176(3) 1.2997(2) 0.0387(16) Uani 1 1 d . . . . .
H16A H 0.185065 0.608881 1.282485 0.058 Uiso 1 1 calc R U . . .
H16B H 0.279008 0.583200 1.304607 0.058 Uiso 1 1 calc R U . . .
H16C H 0.248700 0.635603 1.339553 0.058 Uiso 1 1 calc R U . . .
C110 C 0.1664(4) 0.6490(2) 0.8519(2) 0.0326(14) Uani 1 1 d . . . . .
H11A H 0.132054 0.665988 0.815266 0.049 Uiso 1 1 calc R U . . .
H11B H 0.135884 0.652646 0.886097 0.049 Uiso 1 1 calc R U . . .
H11C H 0.222059 0.667922 0.862054 0.049 Uiso 1 1 calc R U . . .
C235 C 0.2376(3) 0.2059(3) 0.2444(2) 0.0370(16) Uani 1 1 d . . . . .
H23A H 0.263151 0.182427 0.216595 0.055 Uiso 1 1 calc R U . . .
H23B H 0.239867 0.245007 0.232084 0.055 Uiso 1 1 calc R U . . .
H23C H 0.269658 0.201334 0.286190 0.055 Uiso 1 1 calc R U . . .
C108 C 0.1807(4) 0.5868(3) 0.8397(2) 0.0342(15) Uani 1 1 d . . . . .
H108 H 0.213178 0.584149 0.805440 0.041 Uiso 1 1 calc R U . . .
C141 C 0.7120(4) 0.7154(3) 0.9746(2) 0.0371(16) Uani 1 1 d D . . . .
C105 C 0.3454(4) 0.4489(3) 0.8901(2) 0.0342(15) Uani 1 1 d . . . . .
H10E H 0.305035 0.418827 0.873225 0.041 Uiso 1 1 calc R U . . .
H10F H 0.335158 0.481303 0.862199 0.041 Uiso 1 1 calc R U . . .
C32 C 0.6067(4) 0.4390(2) 0.7671(2) 0.0348(15) Uani 1 1 d . . . . .
H32C H 0.622463 0.469048 0.741594 0.052 Uiso 1 1 calc R U . . .
H32D H 0.546851 0.443856 0.771882 0.052 Uiso 1 1 calc R U . . .
H32E H 0.644408 0.440092 0.807387 0.052 Uiso 1 1 calc R U . . .
C206 C 0.4438(4) 0.2222(3) 0.5187(3) 0.0420(16) Uani 1 1 d . . . . .
H20G H 0.487058 0.252390 0.522698 0.050 Uiso 1 1 calc R U . . .
H20H H 0.418248 0.222601 0.555969 0.050 Uiso 1 1 calc R U . . .
C162 C 0.2303(4) 0.7143(2) 1.2493(2) 0.0404(16) Uani 1 1 d . . . . .
H16D H 0.169912 0.707073 1.231436 0.061 Uiso 1 1 calc R U . . .
H16E H 0.234082 0.731028 1.289892 0.061 Uiso 1 1 calc R U . . .
H16F H 0.254721 0.739994 1.222965 0.061 Uiso 1 1 calc R U . . .
C302 C 0.0526(4) 0.5985(2) 0.5304(2) 0.0325(14) Uani 1 1 d . . . . .
H302 H -0.003533 0.604898 0.543669 0.039 Uiso 1 1 calc R U . . .
C103 C 0.4587(4) 0.4056(3) 0.9633(2) 0.0372(15) Uani 1 1 d . . . . .
H10G H 0.434504 0.367798 0.965651 0.045 Uiso 1 1 calc R U . . .
H10H H 0.521393 0.404504 0.979200 0.045 Uiso 1 1 calc R U . . .
C263 C 0.0349(4) 0.0887(3) 0.7252(3) 0.0407(16) Uani 1 1 d . . . . .
H26G H 0.013170 0.065066 0.689777 0.061 Uiso 1 1 calc R U . . .
H26H H 0.088840 0.073244 0.747777 0.061 Uiso 1 1 calc R U . . .
H26I H -0.007597 0.090192 0.751915 0.061 Uiso 1 1 calc R U . . .
C354 C -0.0206(4) 0.4333(3) 0.7266(2) 0.0525(19) Uani 1 1 d . . . . .
H35A H -0.081093 0.442714 0.725458 0.079 Uiso 1 1 calc R U . . .
H35B H 0.008700 0.428634 0.769092 0.079 Uiso 1 1 calc R U . . .
H35C H 0.006975 0.463414 0.707605 0.079 Uiso 1 1 calc R U . . .
C306 C 0.0882(4) 0.5762(3) 0.6431(2) 0.0364(15) Uani 1 1 d . . . . .
H30J H 0.132742 0.558470 0.674392 0.044 Uiso 1 1 calc R U . . .
H30K H 0.034242 0.554967 0.641516 0.044 Uiso 1 1 calc R U . . .
C134 C 0.5248(4) 0.6524(3) 0.7674(2) 0.0499(19) Uani 1 1 d . . . . .
H13A H 0.528255 0.692527 0.775365 0.075 Uiso 1 1 calc R U . . .
H13B H 0.582877 0.636636 0.773935 0.075 Uiso 1 1 calc R U . . .
H13C H 0.495994 0.645750 0.725100 0.075 Uiso 1 1 calc R U . . .
C334 C 0.3590(4) 0.5572(3) 0.4745(3) 0.0461(17) Uani 1 1 d . . . . .
H33J H 0.344553 0.579910 0.437506 0.069 Uiso 1 1 calc R U . . .
H33K H 0.315782 0.562886 0.500118 0.069 Uiso 1 1 calc R U . . .
H33L H 0.415688 0.568063 0.497336 0.069 Uiso 1 1 calc R U . . .
C208 C 0.3204(4) 0.0738(3) 0.3794(3) 0.0495(18) Uani 1 1 d . . . . .
H208 H 0.306163 0.089681 0.337201 0.059 Uiso 1 1 calc R U . . .
C353 C -0.0567(4) 0.3308(3) 0.7232(2) 0.0427(17) Uani 1 1 d . . . . .
H35D H -0.053555 0.295757 0.701165 0.064 Uiso 1 1 calc R U . . .
H35E H -0.025756 0.326803 0.765413 0.064 Uiso 1 1 calc R U . . .
H35F H -0.117008 0.339914 0.723177 0.064 Uiso 1 1 calc R U . . .
C107 C 0.1698(4) 0.4397(3) 0.9300(3) 0.0459(17) Uani 1 1 d . . . . .
H10J H 0.127149 0.416286 0.944448 0.069 Uiso 1 1 calc R U . . .
H10K H 0.152919 0.478931 0.931242 0.069 Uiso 1 1 calc R U . . .
H10L H 0.173063 0.429455 0.887921 0.069 Uiso 1 1 calc R U . . .
C9 C 0.7392(4) 0.5278(3) 0.8844(3) 0.0439(17) Uani 1 1 d . . . . .
H9A H 0.739316 0.558383 0.855245 0.066 Uiso 1 1 calc R U . . .
H9B H 0.681681 0.511182 0.878369 0.066 Uiso 1 1 calc R U . . .
H9C H 0.754652 0.542225 0.926154 0.066 Uiso 1 1 calc R U . . .
C44 C 0.3219(4) 0.2804(3) 0.7918(3) 0.0479(18) Uani 1 1 d . . . . .
H44A H 0.327736 0.316066 0.771571 0.072 Uiso 1 1 calc R U . . .
H44B H 0.264117 0.265375 0.777237 0.072 Uiso 1 1 calc R U . . .
H44C H 0.330949 0.286012 0.836068 0.072 Uiso 1 1 calc R U . . .
C344 C 0.2325(4) 0.4697(3) 0.2157(2) 0.0485(17) Uani 1 1 d . . . . .
H34D H 0.206321 0.506749 0.214628 0.073 Uiso 1 1 calc R U . . .
H34E H 0.292386 0.471720 0.237258 0.073 Uiso 1 1 calc R U . . .
H34F H 0.230798 0.456574 0.173833 0.073 Uiso 1 1 calc R U . . .
C154 C 0.0117(3) 0.6143(3) 1.0893(2) 0.0383(16) Uani 1 1 d . . . . .
H15D H -0.045336 0.607618 1.064366 0.057 Uiso 1 1 calc R U . . .
H15E H 0.014321 0.598176 1.129988 0.057 Uiso 1 1 calc R U . . .
H15F H 0.022334 0.654435 1.092961 0.057 Uiso 1 1 calc R U . . .
C163 C 0.3769(4) 0.6712(3) 1.2837(2) 0.0495(18) Uani 1 1 d . . . . .
H16G H 0.379696 0.689549 1.323316 0.074 Uiso 1 1 calc R U . . .
H16H H 0.409862 0.636395 1.289495 0.074 Uiso 1 1 calc R U . . .
H16I H 0.401293 0.695790 1.256314 0.074 Uiso 1 1 calc R U . . .
C10 C 0.8964(4) 0.5060(3) 0.8781(3) 0.062(2) Uani 1 1 d . . . . .
H10M H 0.895341 0.537962 0.850621 0.093 Uiso 1 1 calc R U . . .
H10N H 0.919283 0.517694 0.920181 0.093 Uiso 1 1 calc R U . . .
H10O H 0.933055 0.476726 0.866198 0.093 Uiso 1 1 calc R U . . .
C234 C 0.0940(4) 0.1906(3) 0.1730(2) 0.0454(18) Uani 1 1 d . . . . .
H23D H 0.033783 0.179699 0.170349 0.068 Uiso 1 1 calc R U . . .
H23E H 0.096689 0.228524 0.157309 0.068 Uiso 1 1 calc R U . . .
H23F H 0.121856 0.164869 0.148667 0.068 Uiso 1 1 calc R U . . .
C352 C 0.0802(4) 0.3628(3) 0.6922(3) 0.0482(18) Uani 1 1 d . . . . .
H35G H 0.082840 0.328058 0.669601 0.072 Uiso 1 1 calc R U . . .
H35H H 0.108145 0.392660 0.673136 0.072 Uiso 1 1 calc R U . . .
H35I H 0.109870 0.357880 0.734624 0.072 Uiso 1 1 calc R U . . .
C8 C 0.8046(4) 0.4835(3) 0.8740(3) 0.0471(18) Uani 1 1 d . . . . .
H8 H 0.785492 0.468843 0.831532 0.057 Uiso 1 1 calc R U . . .
C342 C 0.2248(5) 0.3704(3) 0.2505(3) 0.0525(19) Uani 1 1 d . . . . .
H34G H 0.193787 0.343808 0.271721 0.079 Uiso 1 1 calc R U . . .
H34H H 0.223152 0.357736 0.208482 0.079 Uiso 1 1 calc R U . . .
H34I H 0.284740 0.372882 0.271907 0.079 Uiso 1 1 calc R U . . .
C303 C 0.0934(4) 0.6551(2) 0.5185(3) 0.0395(15) Uani 1 1 d . . . . .
H30L H 0.072859 0.667747 0.475953 0.047 Uiso 1 1 calc R U . . .
H30M H 0.080417 0.684040 0.547031 0.047 Uiso 1 1 calc R U . . .
C153 C 0.0736(3) 0.6118(2) 0.9924(2) 0.0299(14) Uani 1 1 d . . . . .
H15G H 0.116914 0.594916 0.971994 0.045 Uiso 1 1 calc R U . . .
H15H H 0.016103 0.604252 0.968635 0.045 Uiso 1 1 calc R U . . .
H15I H 0.082856 0.652178 0.995453 0.045 Uiso 1 1 calc R U . . .
C343 C 0.0878(4) 0.4246(3) 0.2128(2) 0.054(2) Uani 1 1 d . . . . .
H34J H 0.060182 0.461168 0.211952 0.082 Uiso 1 1 calc R U . . .
H34K H 0.088785 0.412588 0.170854 0.082 Uiso 1 1 calc R U . . .
H34L H 0.055452 0.397517 0.232361 0.082 Uiso 1 1 calc R U . . .
C252 C 0.3931(3) 0.0768(3) 0.6492(2) 0.0425(16) Uani 1 1 d . . . . .
H25G H 0.408646 0.109014 0.626543 0.064 Uiso 1 1 calc R U . . .
H25H H 0.391297 0.087990 0.691287 0.064 Uiso 1 1 calc R U . . .
H25I H 0.436054 0.047366 0.649691 0.064 Uiso 1 1 calc R U . . .
C104 C 0.4382(4) 0.4288(3) 0.8961(2) 0.0391(16) Uani 1 1 d . . . . .
H10P H 0.477199 0.459833 0.890675 0.047 Uiso 1 1 calc R U . . .
H10Q H 0.443039 0.399162 0.866020 0.047 Uiso 1 1 calc R U . . .
C109 C 0.0968(4) 0.5544(3) 0.8214(3) 0.0528(19) Uani 1 1 d . . . . .
H10R H 0.061549 0.571953 0.785479 0.079 Uiso 1 1 calc R U . . .
H10S H 0.109673 0.515924 0.811532 0.079 Uiso 1 1 calc R U . . .
H10T H 0.065455 0.554591 0.855292 0.079 Uiso 1 1 calc R U . . .
C133 C 0.3798(4) 0.6492(3) 0.7987(2) 0.0488(18) Uani 1 1 d . . . . .
H13D H 0.345831 0.631934 0.826185 0.073 Uiso 1 1 calc R U . . .
H13E H 0.382756 0.689518 0.805776 0.073 Uiso 1 1 calc R U . . .
H13F H 0.352554 0.641815 0.756213 0.073 Uiso 1 1 calc R U . . .
C205 C 0.4101(4) 0.2361(3) 0.4045(2) 0.0360(15) Uani 1 1 d . . . . .
H20I H 0.473726 0.236029 0.414431 0.043 Uiso 1 1 calc R U . . .
H20J H 0.390802 0.203122 0.378871 0.043 Uiso 1 1 calc R U . . .
C362 C -0.2751(5) 0.2755(3) 0.5512(3) 0.057(2) Uani 1 1 d . . . . .
H36A H -0.325974 0.254240 0.532209 0.085 Uiso 1 1 calc R U . . .
H36B H -0.224096 0.251739 0.555457 0.085 Uiso 1 1 calc R U . . .
H36C H -0.282371 0.288489 0.591627 0.085 Uiso 1 1 calc R U . . .
C310 C 0.2953(4) 0.4506(3) 0.7277(2) 0.0524(19) Uani 1 1 d . . . . .
H31C H 0.346613 0.431166 0.749168 0.079 Uiso 1 1 calc R U . . .
H31D H 0.299077 0.490159 0.738834 0.079 Uiso 1 1 calc R U . . .
H31E H 0.244016 0.434342 0.739369 0.079 Uiso 1 1 calc R U . . .
C364 C -0.2540(5) 0.3039(3) 0.4459(3) 0.058(2) Uani 1 1 d . . . . .
H36D H -0.304249 0.281170 0.428940 0.087 Uiso 1 1 calc R U . . .
H36E H -0.249537 0.335093 0.418311 0.087 Uiso 1 1 calc R U . . .
H36F H -0.201961 0.280984 0.450291 0.087 Uiso 1 1 calc R U . . .
C132 C 0.4695(4) 0.5609(3) 0.7970(3) 0.055(2) Uani 1 1 d . . . . .
H13G H 0.437014 0.541714 0.824131 0.082 Uiso 1 1 calc R U . . .
H13H H 0.441171 0.555047 0.754378 0.082 Uiso 1 1 calc R U . . .
H13I H 0.528054 0.545933 0.803212 0.082 Uiso 1 1 calc R U . . .
C233 C 0.1399(4) 0.1258(3) 0.2625(2) 0.0429(17) Uani 1 1 d . . . . .
H23G H 0.080318 0.114117 0.261035 0.064 Uiso 1 1 calc R U . . .
H23H H 0.166241 0.102253 0.235195 0.064 Uiso 1 1 calc R U . . .
H23I H 0.172244 0.122167 0.304413 0.064 Uiso 1 1 calc R U . . .
C363 C -0.3468(4) 0.3634(3) 0.5042(4) 0.066(2) Uani 1 1 d . . . . .
H36G H -0.397227 0.340796 0.487131 0.099 Uiso 1 1 calc R U . . .
H36H H -0.352564 0.377112 0.544644 0.099 Uiso 1 1 calc R U . . .
H36I H -0.342740 0.394994 0.477113 0.099 Uiso 1 1 calc R U . . .
C207 C 0.4887(4) 0.1672(3) 0.5154(3) 0.0480(17) Uani 1 1 d . . . . .
H20K H 0.532926 0.162325 0.552272 0.072 Uiso 1 1 calc R U . . .
H20L H 0.446801 0.136855 0.512624 0.072 Uiso 1 1 calc R U . . .
H20M H 0.515702 0.166684 0.479309 0.072 Uiso 1 1 calc R U . . .
C209 C 0.4105(5) 0.0534(4) 0.3874(4) 0.081(3) Uani 1 1 d . . . . .
H20N H 0.413201 0.022049 0.359610 0.121 Uiso 1 1 calc R U . . .
H20O H 0.447738 0.083508 0.378058 0.121 Uiso 1 1 calc R U . . .
H20P H 0.429918 0.041116 0.429676 0.121 Uiso 1 1 calc R U . . .
C4 C 0.9787(5) 0.3323(3) 1.0599(3) 0.061(2) Uani 1 1 d . . . . .
H4A H 0.949335 0.343878 1.093362 0.073 Uiso 1 1 calc R U . . .
H4B H 1.041514 0.336721 1.073926 0.073 Uiso 1 1 calc R U . . .
C307 C 0.0737(4) 0.6363(3) 0.6641(3) 0.0508(18) Uani 1 1 d . . . . .
H30N H 0.056469 0.635188 0.704085 0.076 Uiso 1 1 calc R U . . .
H30O H 0.127100 0.657606 0.667266 0.076 Uiso 1 1 calc R U . . .
H30P H 0.028330 0.654095 0.634300 0.076 Uiso 1 1 calc R U . . .
C210 C 0.2522(5) 0.0290(3) 0.3828(3) 0.0516(19) Uani 1 1 d . . . . .
H21C H 0.257581 -0.000974 0.353958 0.077 Uiso 1 1 calc R U . . .
H21D H 0.260834 0.013829 0.424386 0.077 Uiso 1 1 calc R U . . .
H21E H 0.194777 0.045566 0.372377 0.077 Uiso 1 1 calc R U . . .
C142 C 0.7856(11) 0.6810(8) 1.0126(10) 0.061(3) Uani 0.389(10) 1 d D . P A 1
H14A H 0.765461 0.663631 1.047064 0.091 Uiso 0.389(10) 1 calc R U P A 1
H14B H 0.803860 0.652081 0.986756 0.091 Uiso 0.389(10) 1 calc R U P A 1
H14C H 0.834265 0.705627 1.027960 0.091 Uiso 0.389(10) 1 calc R U P A 1
C143 C 0.6894(17) 0.7640(10) 1.0164(11) 0.085(6) Uani 0.389(10) 1 d D U P A 1
H14D H 0.642688 0.786549 0.993352 0.128 Uiso 0.389(10) 1 calc R U P A 1
H14E H 0.671264 0.748265 1.052489 0.128 Uiso 0.389(10) 1 calc R U P A 1
H14F H 0.740221 0.787469 1.029246 0.128 Uiso 0.389(10) 1 calc R U P A 1
C144 C 0.738(3) 0.7447(12) 0.9186(14) 0.077(6) Uani 0.389(10) 1 d D . P A 1
H14G H 0.688460 0.765705 0.896515 0.116 Uiso 0.389(10) 1 calc R U P A 1
H14H H 0.785619 0.770242 0.932634 0.116 Uiso 0.389(10) 1 calc R U P A 1
H14I H 0.755214 0.716696 0.891430 0.116 Uiso 0.389(10) 1 calc R U P A 1
C145 C 0.7900(7) 0.6780(5) 0.9648(6) 0.061(3) Uani 0.611(10) 1 d D . P A 2
H14J H 0.793479 0.645021 0.991035 0.091 Uiso 0.611(10) 1 calc R U P A 2
H14K H 0.781718 0.666328 0.921901 0.091 Uiso 0.611(10) 1 calc R U P A 2
H14L H 0.843475 0.699396 0.975235 0.091 Uiso 0.611(10) 1 calc R U P A 2
C146 C 0.7326(11) 0.7353(8) 1.0429(5) 0.085(6) Uani 0.611(10) 1 d D U P A 2
H14M H 0.734958 0.703004 1.070020 0.128 Uiso 0.611(10) 1 calc R U P A 2
H14N H 0.788135 0.754543 1.050781 0.128 Uiso 0.611(10) 1 calc R U P A 2
H14O H 0.687482 0.760851 1.050462 0.128 Uiso 0.611(10) 1 calc R U P A 2
C147 C 0.7085(15) 0.7670(7) 0.9324(9) 0.077(6) Uani 0.611(10) 1 d D . P A 2
H14P H 0.761583 0.788634 0.943956 0.116 Uiso 0.611(10) 1 calc R U P A 2
H14Q H 0.702540 0.754850 0.889845 0.116 Uiso 0.611(10) 1 calc R U P A 2
H14R H 0.659175 0.790292 0.936783 0.116 Uiso 0.611(10) 1 calc R U P A 2
C62 C 0.5070(9) 0.4276(5) 1.2217(6) 0.057(3) Uani 0.528(6) 1 d D . P B 1
H62A H 0.475712 0.449252 1.187263 0.086 Uiso 0.528(6) 1 calc R U P B 1
H62B H 0.469971 0.421510 1.251675 0.086 Uiso 0.528(6) 1 calc R U P B 1
H62C H 0.558566 0.448085 1.240927 0.086 Uiso 0.528(6) 1 calc R U P B 1
C64 C 0.5823(8) 0.3373(6) 1.2524(5) 0.052(3) Uani 0.528(6) 1 d D . P B 1
H64A H 0.636101 0.356853 1.268612 0.078 Uiso 0.528(6) 1 calc R U P B 1
H64B H 0.546547 0.335848 1.283742 0.078 Uiso 0.528(6) 1 calc R U P B 1
H64C H 0.595170 0.299368 1.240659 0.078 Uiso 0.528(6) 1 calc R U P B 1
C66 C 0.4482(8) 0.3398(7) 1.1682(6) 0.067(4) Uani 0.528(6) 1 d D . P B 1
H66A H 0.420237 0.361424 1.132609 0.101 Uiso 0.528(6) 1 calc R U P B 1
H66B H 0.459175 0.301895 1.155278 0.101 Uiso 0.528(6) 1 calc R U P B 1
H66C H 0.410551 0.338375 1.198361 0.101 Uiso 0.528(6) 1 calc R U P B 1
C63 C 0.5769(10) 0.3929(7) 1.2610(5) 0.057(3) Uani 0.472(6) 1 d D . P B 2
H63A H 0.635070 0.377809 1.273544 0.086 Uiso 0.472(6) 1 calc R U P B 2
H63B H 0.579889 0.433537 1.257904 0.086 Uiso 0.472(6) 1 calc R U P B 2
H63C H 0.542112 0.382880 1.291347 0.086 Uiso 0.472(6) 1 calc R U P B 2
C65 C 0.5277(9) 0.3020(5) 1.2109(6) 0.052(3) Uani 0.472(6) 1 d D . P B 2
H65A H 0.584511 0.287601 1.229460 0.078 Uiso 0.472(6) 1 calc R U P B 2
H65B H 0.487810 0.296350 1.239102 0.078 Uiso 0.472(6) 1 calc R U P B 2
H65C H 0.506389 0.282205 1.172616 0.078 Uiso 0.472(6) 1 calc R U P B 2
C67 C 0.4445(9) 0.3857(8) 1.1689(7) 0.067(4) Uani 0.472(6) 1 d D . P B 2
H67A H 0.426700 0.367020 1.129474 0.101 Uiso 0.472(6) 1 calc R U P B 2
H67B H 0.405222 0.375490 1.196237 0.101 Uiso 0.472(6) 1 calc R U P B 2
H67C H 0.442998 0.426146 1.162795 0.101 Uiso 0.472(6) 1 calc R U P B 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
V2 O104 1.594(3) . ?
V2 O103 1.761(3) . ?
V2 O101 1.909(3) . ?
V2 O102 1.910(3) . ?
V2 N101 2.231(4) . ?
V2 N102 2.469(5) . ?
V1 O4 1.589(3) . ?
V1 O3 1.772(3) . ?
V1 O1 1.898(3) . ?
V1 O2 1.913(3) . ?
V1 N1 2.249(4) . ?
V1 N2 2.464(4) . ?
V4 O304 1.593(4) . ?
V4 O303 1.775(3) . ?
V4 O302 1.897(3) . ?
V4 O301 1.910(3) . ?
V4 N301 2.227(4) . ?
V4 N302 2.428(5) . ?
V3 O204 1.598(4) . ?
V3 O203 1.771(3) . ?
V3 O201 1.890(3) . ?
V3 O202 1.903(3) . ?
V3 N201 2.237(4) . ?
V3 N202 2.494(4) . ?
O1 C21 1.352(5) . ?
O202 C221 1.354(5) . ?
O2 C11 1.362(6) . ?
O101 C111 1.360(6) . ?
O3 C8 1.419(6) . ?
O201 C211 1.350(6) . ?
O303 C308 1.416(6) . ?
O103 C108 1.423(6) . ?
O102 C121 1.359(5) . ?
O301 C311 1.348(5) . ?
O302 C321 1.356(6) . ?
O203 C208 1.414(7) . ?
N301 C317 1.482(6) . ?
N301 C301 1.491(7) . ?
N301 C327 1.500(6) . ?
N1 C1 1.482(6) . ?
N1 C27 1.486(6) . ?
N1 C17 1.503(6) . ?
N201 C201 1.487(6) . ?
N201 C217 1.490(6) . ?
N201 C227 1.494(6) . ?
N102 C102 1.500(6) . ?
N102 C106 1.505(6) . ?
N102 C105 1.506(6) . ?
C14 C15 1.385(6) . ?
C14 C13 1.395(7) . ?
C14 C41 1.537(7) . ?
N2 C2 1.487(6) . ?
N2 C6 1.489(6) . ?
N2 C5 1.497(6) . ?
C11 C16 1.391(6) . ?
C11 C12 1.416(6) . ?
N101 C129 1.468(6) . ?
N101 C101 1.485(6) . ?
N101 C127 1.492(6) . ?
C211 C216 1.400(6) . ?
C211 C212 1.417(6) . ?
C213 C214 1.382(7) . ?
C213 C212 1.400(7) . ?
C213 H213 0.9300 . ?
N302 C306 1.486(6) . ?
N302 C302 1.487(7) . ?
N302 C305 1.505(7) . ?
C16 C15 1.394(7) . ?
C16 C17 1.475(6) . ?
C111 C116 1.387(7) . ?
C111 C112 1.429(6) . ?
C1 C2 1.529(7) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C215 C214 1.386(6) . ?
C215 C216 1.394(7) . ?
C215 H215 0.9300 . ?
C22 C23 1.399(6) . ?
C22 C21 1.419(7) . ?
C22 C51 1.535(7) . ?
C13 C12 1.383(7) . ?
C13 H13 0.9300 . ?
C15 H15 0.9300 . ?
C216 C217 1.510(6) . ?
C2 C3 1.521(7) . ?
C2 H2 0.9800 . ?
N202 C206 1.500(6) . ?
N202 C205 1.504(6) . ?
N202 C202 1.515(7) . ?
C121 C122 1.404(6) . ?
C121 C126 1.407(7) . ?
C217 H21A 0.9700 . ?
C217 H21B 0.9700 . ?
C31 C32 1.527(7) . ?
C31 C12 1.528(6) . ?
C31 C33 1.528(7) . ?
C31 C34 1.536(6) . ?
C314 C315 1.370(7) . ?
C314 C313 1.403(7) . ?
C314 C341 1.536(6) . ?
C322 C321 1.394(7) . ?
C322 C323 1.401(7) . ?
C322 C351 1.549(7) . ?
C311 C316 1.400(7) . ?
C311 C312 1.421(7) . ?
C124 C125 1.384(7) . ?
C124 C123 1.405(7) . ?
C124 C161 1.531(7) . ?
C27 C26 1.502(7) . ?
C27 H27A 0.9700 . ?
C27 H27B 0.9700 . ?
C325 C326 1.388(7) . ?
C325 C324 1.393(7) . ?
C325 H325 0.9300 . ?
C21 C26 1.395(7) . ?
C122 C123 1.392(6) . ?
C122 C151 1.529(7) . ?
C312 C313 1.378(7) . ?
C312 C331 1.545(7) . ?
C61 C64 1.477(10) . ?
C61 C67 1.480(13) . ?
C61 C66 1.525(13) . ?
C61 C63 1.540(12) . ?
C61 C24 1.547(6) . ?
C61 C65 1.588(13) . ?
C61 C62 1.590(11) . ?
C26 C25 1.397(6) . ?
C321 C326 1.410(7) . ?
C41 C44 1.518(8) . ?
C41 C42 1.529(7) . ?
C41 C43 1.532(7) . ?
C225 C224 1.386(7) . ?
C225 C226 1.392(7) . ?
C225 H225 0.9300 . ?
C126 C125 1.387(7) . ?
C126 C127 1.480(7) . ?
C241 C243 1.531(7) . ?
C241 C244 1.534(8) . ?
C241 C242 1.538(7) . ?
C241 C214 1.545(7) . ?
C23 C24 1.393(7) . ?
C23 H23 0.9300 . ?
C6 C7 1.535(7) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C227 C226 1.495(7) . ?
C227 H22A 0.9700 . ?
C227 H22B 0.9700 . ?
C323 C324 1.384(7) . ?
C323 H323 0.9300 . ?
C222 C223 1.400(6) . ?
C222 C221 1.403(7) . ?
C222 C251 1.530(7) . ?
C113 C112 1.378(7) . ?
C113 C114 1.402(7) . ?
C113 H113 0.9300 . ?
C309 C308 1.512(8) . ?
C309 H30A 0.9600 . ?
C309 H30B 0.9600 . ?
C309 H30C 0.9600 . ?
C226 C221 1.394(7) . ?
C5 C4 1.482(7) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C101 C102 1.512(7) . ?
C101 H10A 0.9700 . ?
C101 H10B 0.9700 . ?
C123 H123 0.9300 . ?
C331 C334 1.519(8) . ?
C331 C333 1.542(7) . ?
C331 C332 1.544(7) . ?
C223 C224 1.392(7) . ?
C223 H223 0.9300 . ?
C341 C342 1.520(8) . ?
C341 C344 1.524(7) . ?
C341 C343 1.531(8) . ?
C151 C154 1.527(7) . ?
C151 C152 1.534(7) . ?
C151 C153 1.538(6) . ?
C25 C24 1.378(7) . ?
C25 H25 0.9300 . ?
C114 C115 1.374(7) . ?
C114 C141 1.527(8) . ?
C129 C116 1.513(6) . ?
C129 H12A 0.9700 . ?
C129 H12B 0.9700 . ?
C212 C232 1.535(7) . ?
C127 H12C 0.9700 . ?
C127 H12D 0.9700 . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C51 C53 1.521(7) . ?
C51 C54 1.529(7) . ?
C51 C52 1.539(7) . ?
C152 H15A 0.9600 . ?
C152 H15B 0.9600 . ?
C152 H15C 0.9600 . ?
C301 C302 1.538(7) . ?
C301 H30D 0.9700 . ?
C301 H30E 0.9700 . ?
C7 H7A 0.9600 . ?
C7 H7B 0.9600 . ?
C7 H7C 0.9600 . ?
C351 C354 1.517(8) . ?
C351 C352 1.517(7) . ?
C351 C353 1.530(7) . ?
C3 C4 1.525(8) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C112 C131 1.543(7) . ?
C125 H125 0.9300 . ?
C102 C103 1.510(7) . ?
C102 H102 0.9800 . ?
C116 C115 1.394(7) . ?
C317 C316 1.499(6) . ?
C317 H31A 0.9700 . ?
C317 H31B 0.9700 . ?
C43 H43A 0.9600 . ?
C43 H43B 0.9600 . ?
C43 H43C 0.9600 . ?
C224 C261 1.543(7) . ?
C232 C235 1.535(7) . ?
C232 C234 1.539(6) . ?
C232 C233 1.543(8) . ?
C324 C361 1.521(8) . ?
C313 H313 0.9300 . ?
C326 C327 1.489(7) . ?
C316 C315 1.389(6) . ?
C361 C363 1.531(9) . ?
C361 C362 1.534(8) . ?
C361 C364 1.537(7) . ?
C315 H315 0.9300 . ?
C115 H115 0.9300 . ?
C327 H32A 0.9700 . ?
C327 H32B 0.9700 . ?
C33 H33A 0.9600 . ?
C33 H33B 0.9600 . ?
C33 H33C 0.9600 . ?
C308 C310 1.502(7) . ?
C308 H308 0.9800 . ?
C244 H24A 0.9600 . ?
C244 H24B 0.9600 . ?
C244 H24C 0.9600 . ?
C161 C163 1.521(7) . ?
C161 C162 1.538(8) . ?
C161 C164 1.541(7) . ?
C251 C254 1.531(8) . ?
C251 C253 1.532(6) . ?
C251 C252 1.553(7) . ?
C253 H25A 0.9600 . ?
C253 H25B 0.9600 . ?
C253 H25C 0.9600 . ?
C53 H53A 0.9600 . ?
C53 H53B 0.9600 . ?
C53 H53C 0.9600 . ?
C34 H34A 0.9600 . ?
C34 H34B 0.9600 . ?
C34 H34C 0.9600 . ?
C203 C202 1.528(7) . ?
C203 C204 1.532(8) . ?
C203 H20A 0.9700 . ?
C203 H20B 0.9700 . ?
C305 C304 1.521(8) . ?
C305 H30F 0.9700 . ?
C305 H30G 0.9700 . ?
C333 H33D 0.9600 . ?
C333 H33E 0.9600 . ?
C333 H33F 0.9600 . ?
C54 H54A 0.9600 . ?
C54 H54B 0.9600 . ?
C54 H54C 0.9600 . ?
C202 C201 1.527(7) . ?
C202 H202 0.9800 . ?
C52 H52A 0.9600 . ?
C52 H52B 0.9600 . ?
C52 H52C 0.9600 . ?
C106 C107 1.489(7) . ?
C106 H10C 0.9700 . ?
C106 H10D 0.9700 . ?
C243 H24D 0.9600 . ?
C243 H24E 0.9600 . ?
C243 H24F 0.9600 . ?
C332 H33G 0.9600 . ?
C332 H33H 0.9600 . ?
C332 H33I 0.9600 . ?
C264 C261 1.508(7) . ?
C264 H26A 0.9600 . ?
C264 H26B 0.9600 . ?
C264 H26C 0.9600 . ?
C201 H20C 0.9700 . ?
C201 H20D 0.9700 . ?
C131 C134 1.517(7) . ?
C131 C132 1.522(9) . ?
C131 C133 1.537(8) . ?
C242 H24G 0.9600 . ?
C242 H24H 0.9600 . ?
C242 H24I 0.9600 . ?
C261 C263 1.532(8) . ?
C261 C262 1.548(8) . ?
C204 C205 1.496(8) . ?
C204 H20E 0.9700 . ?
C204 H20F 0.9700 . ?
C254 H25D 0.9600 . ?
C254 H25E 0.9600 . ?
C254 H25F 0.9600 . ?
C304 C303 1.508(8) . ?
C304 H30H 0.9700 . ?
C304 H30I 0.9700 . ?
C262 H26D 0.9600 . ?
C262 H26E 0.9600 . ?
C262 H26F 0.9600 . ?
C42 H42A 0.9600 . ?
C42 H42B 0.9600 . ?
C42 H42C 0.9600 . ?
C164 H16A 0.9600 . ?
C164 H16B 0.9600 . ?
C164 H16C 0.9600 . ?
C110 C108 1.511(8) . ?
C110 H11A 0.9600 . ?
C110 H11B 0.9600 . ?
C110 H11C 0.9600 . ?
C235 H23A 0.9600 . ?
C235 H23B 0.9600 . ?
C235 H23C 0.9600 . ?
C108 C109 1.496(8) . ?
C108 H108 0.9800 . ?
C141 C142 1.512(15) . ?
C141 C147 1.520(13) . ?
C141 C144 1.520(18) . ?
C141 C146 1.537(11) . ?
C141 C143 1.544(16) . ?
C141 C145 1.544(11) . ?
C105 C104 1.498(7) . ?
C105 H10E 0.9700 . ?
C105 H10F 0.9700 . ?
C32 H32C 0.9600 . ?
C32 H32D 0.9600 . ?
C32 H32E 0.9600 . ?
C206 C207 1.478(8) . ?
C206 H20G 0.9700 . ?
C206 H20H 0.9700 . ?
C162 H16D 0.9600 . ?
C162 H16E 0.9600 . ?
C162 H16F 0.9600 . ?
C302 C303 1.517(8) . ?
C302 H302 0.9800 . ?
C103 C104 1.539(7) . ?
C103 H10G 0.9700 . ?
C103 H10H 0.9700 . ?
C263 H26G 0.9600 . ?
C263 H26H 0.9600 . ?
C263 H26I 0.9600 . ?
C354 H35A 0.9600 . ?
C354 H35B 0.9600 . ?
C354 H35C 0.9600 . ?
C306 C307 1.516(8) . ?
C306 H30J 0.9700 . ?
C306 H30K 0.9700 . ?
C134 H13A 0.9600 . ?
C134 H13B 0.9600 . ?
C134 H13C 0.9600 . ?
C334 H33J 0.9600 . ?
C334 H33K 0.9600 . ?
C334 H33L 0.9600 . ?
C208 C209 1.458(8) . ?
C208 C210 1.505(9) . ?
C208 H208 0.9800 . ?
C353 H35D 0.9600 . ?
C353 H35E 0.9600 . ?
C353 H35F 0.9600 . ?
C107 H10J 0.9600 . ?
C107 H10K 0.9600 . ?
C107 H10L 0.9600 . ?
C9 C8 1.502(8) . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C44 H44A 0.9600 . ?
C44 H44B 0.9600 . ?
C44 H44C 0.9600 . ?
C344 H34D 0.9600 . ?
C344 H34E 0.9600 . ?
C344 H34F 0.9600 . ?
C154 H15D 0.9600 . ?
C154 H15E 0.9600 . ?
C154 H15F 0.9600 . ?
C163 H16G 0.9600 . ?
C163 H16H 0.9600 . ?
C163 H16I 0.9600 . ?
C10 C8 1.507(8) . ?
C10 H10M 0.9600 . ?
C10 H10N 0.9600 . ?
C10 H10O 0.9600 . ?
C234 H23D 0.9600 . ?
C234 H23E 0.9600 . ?
C234 H23F 0.9600 . ?
C352 H35G 0.9600 . ?
C352 H35H 0.9600 . ?
C352 H35I 0.9600 . ?
C8 H8 0.9800 . ?
C342 H34G 0.9600 . ?
C342 H34H 0.9600 . ?
C342 H34I 0.9600 . ?
C303 H30L 0.9700 . ?
C303 H30M 0.9700 . ?
C153 H15G 0.9600 . ?
C153 H15H 0.9600 . ?
C153 H15I 0.9600 . ?
C343 H34J 0.9600 . ?
C343 H34K 0.9600 . ?
C343 H34L 0.9600 . ?
C252 H25G 0.9600 . ?
C252 H25H 0.9600 . ?
C252 H25I 0.9600 . ?
C104 H10P 0.9700 . ?
C104 H10Q 0.9700 . ?
C109 H10R 0.9600 . ?
C109 H10S 0.9600 . ?
C109 H10T 0.9600 . ?
C133 H13D 0.9600 . ?
C133 H13E 0.9600 . ?
C133 H13F 0.9600 . ?
C205 H20I 0.9700 . ?
C205 H20J 0.9700 . ?
C362 H36A 0.9600 . ?
C362 H36B 0.9600 . ?
C362 H36C 0.9600 . ?
C310 H31C 0.9600 . ?
C310 H31D 0.9600 . ?
C310 H31E 0.9600 . ?
C364 H36D 0.9600 . ?
C364 H36E 0.9600 . ?
C364 H36F 0.9600 . ?
C132 H13G 0.9600 . ?
C132 H13H 0.9600 . ?
C132 H13I 0.9600 . ?
C233 H23G 0.9600 . ?
C233 H23H 0.9600 . ?
C233 H23I 0.9600 . ?
C363 H36G 0.9600 . ?
C363 H36H 0.9600 . ?
C363 H36I 0.9600 . ?
C207 H20K 0.9600 . ?
C207 H20L 0.9600 . ?
C207 H20M 0.9600 . ?
C209 H20N 0.9600 . ?
C209 H20O 0.9600 . ?
C209 H20P 0.9600 . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C307 H30N 0.9600 . ?
C307 H30O 0.9600 . ?
C307 H30P 0.9600 . ?
C210 H21C 0.9600 . ?
C210 H21D 0.9600 . ?
C210 H21E 0.9600 . ?
C142 H14A 0.9600 . ?
C142 H14B 0.9600 . ?
C142 H14C 0.9600 . ?
C143 H14D 0.9600 . ?
C143 H14E 0.9600 . ?
C143 H14F 0.9600 . ?
C144 H14G 0.9600 . ?
C144 H14H 0.9600 . ?
C144 H14I 0.9600 . ?
C145 H14J 0.9600 . ?
C145 H14K 0.9600 . ?
C145 H14L 0.9600 . ?
C146 H14M 0.9600 . ?
C146 H14N 0.9600 . ?
C146 H14O 0.9600 . ?
C147 H14P 0.9600 . ?
C147 H14Q 0.9600 . ?
C147 H14R 0.9600 . ?
C62 H62A 0.9600 . ?
C62 H62B 0.9600 . ?
C62 H62C 0.9600 . ?
C64 H64A 0.9600 . ?
C64 H64B 0.9600 . ?
C64 H64C 0.9600 . ?
C66 H66A 0.9600 . ?
C66 H66B 0.9600 . ?
C66 H66C 0.9600 . ?
C63 H63A 0.9600 . ?
C63 H63B 0.9600 . ?
C63 H63C 0.9600 . ?
C65 H65A 0.9600 . ?
C65 H65B 0.9600 . ?
C65 H65C 0.9600 . ?
C67 H67A 0.9600 . ?
C67 H67B 0.9600 . ?
C67 H67C 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
O104 V2 O103 107.28(17) . . ?
O104 V2 O101 95.41(17) . . ?
O103 V2 O101 94.36(14) . . ?
O104 V2 O102 95.44(16) . . ?
O103 V2 O102 98.15(15) . . ?
O101 V2 O102 160.21(15) . . ?
O104 V2 N101 93.72(17) . . ?
O103 V2 N101 158.63(16) . . ?
O101 V2 N101 79.44(14) . . ?
O102 V2 N101 83.38(14) . . ?
O104 V2 N102 168.15(16) . . ?
O103 V2 N102 84.44(15) . . ?
O101 V2 N102 85.19(15) . . ?
O102 V2 N102 80.84(14) . . ?
N101 V2 N102 74.72(15) . . ?
O4 V1 O3 107.66(17) . . ?
O4 V1 O1 95.09(15) . . ?
O3 V1 O1 97.44(14) . . ?
O4 V1 O2 93.38(15) . . ?
O3 V1 O2 96.16(14) . . ?
O1 V1 O2 160.98(14) . . ?
O4 V1 N1 96.71(16) . . ?
O3 V1 N1 155.59(15) . . ?
O1 V1 N1 78.65(14) . . ?
O2 V1 N1 83.47(14) . . ?
O4 V1 N2 171.08(16) . . ?
O3 V1 N2 81.26(15) . . ?
O1 V1 N2 83.14(13) . . ?
O2 V1 N2 85.86(13) . . ?
N1 V1 N2 74.37(14) . . ?
O304 V4 O303 107.70(17) . . ?
O304 V4 O302 95.92(17) . . ?
O303 V4 O302 97.08(15) . . ?
O304 V4 O301 94.88(16) . . ?
O303 V4 O301 95.29(15) . . ?
O302 V4 O301 160.28(16) . . ?
O304 V4 N301 94.00(17) . . ?
O303 V4 N301 158.07(17) . . ?
O302 V4 N301 83.48(14) . . ?
O301 V4 N301 79.34(15) . . ?
O304 V4 N302 169.33(16) . . ?
O303 V4 N302 82.90(15) . . ?
O302 V4 N302 83.67(15) . . ?
O301 V4 N302 82.68(15) . . ?
N301 V4 N302 75.35(15) . . ?
O204 V3 O203 107.17(18) . . ?
O204 V3 O201 95.56(16) . . ?
O203 V3 O201 94.60(15) . . ?
O204 V3 O202 95.85(16) . . ?
O203 V3 O202 97.45(15) . . ?
O201 V3 O202 160.18(16) . . ?
O204 V3 N201 93.95(17) . . ?
O203 V3 N201 158.60(17) . . ?
O201 V3 N201 79.63(14) . . ?
O202 V3 N201 83.45(14) . . ?
O204 V3 N202 167.72(16) . . ?
O203 V3 N202 84.92(16) . . ?
O201 V3 N202 85.38(14) . . ?
O202 V3 N202 80.09(14) . . ?
N201 V3 N202 74.13(15) . . ?
C21 O1 V1 126.5(3) . . ?
C221 O202 V3 119.7(3) . . ?
C11 O2 V1 119.6(3) . . ?
C111 O101 V2 127.1(3) . . ?
C8 O3 V1 140.7(4) . . ?
C211 O201 V3 129.7(3) . . ?
C308 O303 V4 143.6(3) . . ?
C108 O103 V2 145.6(3) . . ?
C121 O102 V2 121.9(3) . . ?
C311 O301 V4 127.3(3) . . ?
C321 O302 V4 123.7(3) . . ?
C208 O203 V3 144.2(4) . . ?
C317 N301 C301 109.8(4) . . ?
C317 N301 C327 107.5(4) . . ?
C301 N301 C327 107.5(4) . . ?
C317 N301 V4 107.4(3) . . ?
C301 N301 V4 110.1(3) . . ?
C327 N301 V4 114.5(3) . . ?
C1 N1 C27 108.2(3) . . ?
C1 N1 C17 109.6(4) . . ?
C27 N1 C17 107.0(4) . . ?
C1 N1 V1 109.8(3) . . ?
C27 N1 V1 108.7(3) . . ?
C17 N1 V1 113.4(3) . . ?
C201 N201 C217 107.9(4) . . ?
C201 N201 C227 109.7(4) . . ?
C217 N201 C227 107.1(4) . . ?
C201 N201 V3 110.4(3) . . ?
C217 N201 V3 108.6(3) . . ?
C227 N201 V3 113.1(3) . . ?
C102 N102 C106 107.6(4) . . ?
C102 N102 C105 105.9(4) . . ?
C106 N102 C105 109.7(4) . . ?
C102 N102 V2 109.1(3) . . ?
C106 N102 V2 113.7(3) . . ?
C105 N102 V2 110.5(3) . . ?
C15 C14 C13 115.9(5) . . ?
C15 C14 C41 123.9(4) . . ?
C13 C14 C41 120.2(4) . . ?
C2 N2 C6 111.6(4) . . ?
C2 N2 C5 106.4(4) . . ?
C6 N2 C5 110.7(4) . . ?
C2 N2 V1 110.8(3) . . ?
C6 N2 V1 108.4(3) . . ?
C5 N2 V1 109.0(3) . . ?
O2 C11 C16 116.4(4) . . ?
O2 C11 C12 123.0(4) . . ?
C16 C11 C12 120.5(5) . . ?
C129 N101 C101 109.8(4) . . ?
C129 N101 C127 106.7(4) . . ?
C101 N101 C127 109.3(4) . . ?
C129 N101 V2 107.9(3) . . ?
C101 N101 V2 109.4(3) . . ?
C127 N101 V2 113.6(3) . . ?
O201 C211 C216 121.1(4) . . ?
O201 C211 C212 119.9(4) . . ?
C216 C211 C212 119.0(5) . . ?
C214 C213 C212 124.0(4) . . ?
C214 C213 H213 118.0 . . ?
C212 C213 H213 118.0 . . ?
C306 N302 C302 112.5(4) . . ?
C306 N302 C305 110.0(4) . . ?
C302 N302 C305 106.5(4) . . ?
C306 N302 V4 107.7(3) . . ?
C302 N302 V4 110.6(3) . . ?
C305 N302 V4 109.6(3) . . ?
C11 C16 C15 119.9(4) . . ?
C11 C16 C17 117.5(4) . . ?
C15 C16 C17 122.5(4) . . ?
O101 C111 C116 120.1(4) . . ?
O101 C111 C112 120.8(4) . . ?
C116 C111 C112 119.0(5) . . ?
N1 C1 C2 113.2(4) . . ?
N1 C1 H1A 108.9 . . ?
C2 C1 H1A 108.9 . . ?
N1 C1 H1B 108.9 . . ?
C2 C1 H1B 108.9 . . ?
H1A C1 H1B 107.7 . . ?
C214 C215 C216 122.1(5) . . ?
C214 C215 H215 118.9 . . ?
C216 C215 H215 118.9 . . ?
C23 C22 C21 117.4(5) . . ?
C23 C22 C51 120.5(4) . . ?
C21 C22 C51 122.0(4) . . ?
C12 C13 C14 125.6(5) . . ?
C12 C13 H13 117.2 . . ?
C14 C13 H13 117.2 . . ?
C14 C15 C16 121.9(5) . . ?
C14 C15 H15 119.1 . . ?
C16 C15 H15 119.1 . . ?
C215 C216 C211 120.2(4) . . ?
C215 C216 C217 116.3(4) . . ?
C211 C216 C217 123.5(4) . . ?
N2 C2 C3 107.2(4) . . ?
N2 C2 C1 110.9(4) . . ?
C3 C2 C1 109.7(4) . . ?
N2 C2 H2 109.6 . . ?
C3 C2 H2 109.6 . . ?
C1 C2 H2 109.6 . . ?
C206 N202 C205 110.6(4) . . ?
C206 N202 C202 106.2(4) . . ?
C205 N202 C202 105.8(4) . . ?
C206 N202 V3 114.1(3) . . ?
C205 N202 V3 109.8(3) . . ?
C202 N202 V3 110.0(3) . . ?
O102 C121 C122 123.1(4) . . ?
O102 C121 C126 116.4(4) . . ?
C122 C121 C126 120.4(4) . . ?
N201 C217 C216 114.6(4) . . ?
N201 C217 H21A 108.6 . . ?
C216 C217 H21A 108.6 . . ?
N201 C217 H21B 108.6 . . ?
C216 C217 H21B 108.6 . . ?
H21A C217 H21B 107.6 . . ?
C32 C31 C12 108.0(4) . . ?
C32 C31 C33 110.8(5) . . ?
C12 C31 C33 111.2(4) . . ?
C32 C31 C34 107.4(4) . . ?
C12 C31 C34 112.7(4) . . ?
C33 C31 C34 106.7(4) . . ?
C315 C314 C313 115.9(4) . . ?
C315 C314 C341 123.7(5) . . ?
C313 C314 C341 120.4(4) . . ?
C321 C322 C323 117.1(5) . . ?
C321 C322 C351 121.1(5) . . ?
C323 C322 C351 121.7(5) . . ?
O301 C311 C316 120.7(4) . . ?
O301 C311 C312 120.6(4) . . ?
C316 C311 C312 118.6(4) . . ?
C125 C124 C123 116.6(4) . . ?
C125 C124 C161 122.7(5) . . ?
C123 C124 C161 120.5(5) . . ?
N1 C27 C26 116.9(4) . . ?
N1 C27 H27A 108.1 . . ?
C26 C27 H27A 108.1 . . ?
N1 C27 H27B 108.1 . . ?
C26 C27 H27B 108.1 . . ?
H27A C27 H27B 107.3 . . ?
C326 C325 C324 121.4(5) . . ?
C326 C325 H325 119.3 . . ?
C324 C325 H325 119.3 . . ?
O1 C21 C26 120.3(4) . . ?
O1 C21 C22 119.9(4) . . ?
C26 C21 C22 119.8(4) . . ?
C123 C122 C121 116.1(5) . . ?
C123 C122 C151 122.1(4) . . ?
C121 C122 C151 121.5(4) . . ?
C313 C312 C311 118.6(5) . . ?
C313 C312 C331 120.4(4) . . ?
C311 C312 C331 121.0(4) . . ?
C64 C61 C66 113.1(9) . . ?
C67 C61 C63 118.4(10) . . ?
C64 C61 C24 109.8(6) . . ?
C67 C61 C24 109.5(7) . . ?
C66 C61 C24 111.9(6) . . ?
C63 C61 C24 111.0(6) . . ?
C67 C61 C65 105.1(10) . . ?
C63 C61 C65 103.5(8) . . ?
C24 C61 C65 108.6(6) . . ?
C64 C61 C62 106.3(8) . . ?
C66 C61 C62 104.4(9) . . ?
C24 C61 C62 111.1(6) . . ?
C21 C26 C25 119.8(5) . . ?
C21 C26 C27 123.5(4) . . ?
C25 C26 C27 116.6(5) . . ?
O302 C321 C322 123.1(5) . . ?
O302 C321 C326 116.2(5) . . ?
C322 C321 C326 120.6(5) . . ?
C44 C41 C42 109.6(5) . . ?
C44 C41 C43 109.7(5) . . ?
C42 C41 C43 106.9(5) . . ?
C44 C41 C14 109.0(5) . . ?
C42 C41 C14 111.5(4) . . ?
C43 C41 C14 110.1(4) . . ?
C224 C225 C226 120.6(5) . . ?
C224 C225 H225 119.7 . . ?
C226 C225 H225 119.7 . . ?
C13 C12 C11 116.0(4) . . ?
C13 C12 C31 121.1(4) . . ?
C11 C12 C31 122.9(4) . . ?
C125 C126 C121 120.5(5) . . ?
C125 C126 C127 122.8(5) . . ?
C121 C126 C127 115.9(4) . . ?
C243 C241 C244 107.7(4) . . ?
C243 C241 C242 108.3(4) . . ?
C244 C241 C242 109.9(4) . . ?
C243 C241 C214 111.7(4) . . ?
C244 C241 C214 110.9(4) . . ?
C242 C241 C214 108.3(4) . . ?
C24 C23 C22 123.6(5) . . ?
C24 C23 H23 118.2 . . ?
C22 C23 H23 118.2 . . ?
N2 C6 C7 116.1(4) . . ?
N2 C6 H6A 108.3 . . ?
C7 C6 H6A 108.3 . . ?
N2 C6 H6B 108.3 . . ?
C7 C6 H6B 108.3 . . ?
H6A C6 H6B 107.4 . . ?
N201 C227 C226 114.6(4) . . ?
N201 C227 H22A 108.6 . . ?
C226 C227 H22A 108.6 . . ?
N201 C227 H22B 108.6 . . ?
C226 C227 H22B 108.6 . . ?
H22A C227 H22B 107.6 . . ?
C324 C323 C322 123.8(5) . . ?
C324 C323 H323 118.1 . . ?
C322 C323 H323 118.1 . . ?
C223 C222 C221 116.4(5) . . ?
C223 C222 C251 121.5(5) . . ?
C221 C222 C251 121.9(4) . . ?
C112 C113 C114 124.5(5) . . ?
C112 C113 H113 117.8 . . ?
C114 C113 H113 117.8 . . ?
C308 C309 H30A 109.5 . . ?
C308 C309 H30B 109.5 . . ?
H30A C309 H30B 109.5 . . ?
C308 C309 H30C 109.5 . . ?
H30A C309 H30C 109.5 . . ?
H30B C309 H30C 109.5 . . ?
C225 C226 C221 120.7(5) . . ?
C225 C226 C227 122.4(5) . . ?
C221 C226 C227 116.3(4) . . ?
C4 C5 N2 108.3(5) . . ?
C4 C5 H5A 110.0 . . ?
N2 C5 H5A 110.0 . . ?
C4 C5 H5B 110.0 . . ?
N2 C5 H5B 110.0 . . ?
H5A C5 H5B 108.4 . . ?
N101 C101 C102 112.7(4) . . ?
N101 C101 H10A 109.0 . . ?
C102 C101 H10A 109.1 . . ?
N101 C101 H10B 109.0 . . ?
C102 C101 H10B 109.0 . . ?
H10A C101 H10B 107.8 . . ?
C122 C123 C124 124.9(5) . . ?
C122 C123 H123 117.5 . . ?
C124 C123 H123 117.5 . . ?
C334 C331 C333 108.8(5) . . ?
C334 C331 C332 106.8(5) . . ?
C333 C331 C332 107.6(5) . . ?
C334 C331 C312 109.6(5) . . ?
C333 C331 C312 111.6(4) . . ?
C332 C331 C312 112.3(4) . . ?
C224 C223 C222 124.2(5) . . ?
C224 C223 H223 117.9 . . ?
C222 C223 H223 117.9 . . ?
C342 C341 C344 108.2(5) . . ?
C342 C341 C343 108.9(5) . . ?
C344 C341 C343 108.2(5) . . ?
C342 C341 C314 108.4(4) . . ?
C344 C341 C314 111.6(4) . . ?
C343 C341 C314 111.5(4) . . ?
C154 C151 C122 112.2(4) . . ?
C154 C151 C152 107.8(4) . . ?
C122 C151 C152 108.7(4) . . ?
C154 C151 C153 108.2(4) . . ?
C122 C151 C153 110.1(4) . . ?
C152 C151 C153 109.8(4) . . ?
C24 C25 C26 122.3(5) . . ?
C24 C25 H25 118.9 . . ?
C26 C25 H25 118.9 . . ?
C25 C24 C23 117.0(4) . . ?
C25 C24 C61 121.4(5) . . ?
C23 C24 C61 121.6(5) . . ?
C115 C114 C113 115.6(5) . . ?
C115 C114 C141 121.7(5) . . ?
C113 C114 C141 122.7(4) . . ?
N101 C129 C116 116.9(4) . . ?
N101 C129 H12A 108.1 . . ?
C116 C129 H12A 108.1 . . ?
N101 C129 H12B 108.1 . . ?
C116 C129 H12B 108.1 . . ?
H12A C129 H12B 107.3 . . ?
C213 C212 C211 117.8(4) . . ?
C213 C212 C232 121.0(4) . . ?
C211 C212 C232 121.2(4) . . ?
C126 C127 N101 115.8(4) . . ?
C126 C127 H12C 108.3 . . ?
N101 C127 H12C 108.3 . . ?
C126 C127 H12D 108.3 . . ?
N101 C127 H12D 108.3 . . ?
H12C C127 H12D 107.4 . . ?
C16 C17 N1 113.6(4) . . ?
C16 C17 H17A 108.8 . . ?
N1 C17 H17A 108.8 . . ?
C16 C17 H17B 108.8 . . ?
N1 C17 H17B 108.8 . . ?
H17A C17 H17B 107.7 . . ?
C53 C51 C54 107.8(4) . . ?
C53 C51 C22 109.8(4) . . ?
C54 C51 C22 113.1(4) . . ?
C53 C51 C52 109.6(4) . . ?
C54 C51 C52 106.2(4) . . ?
C22 C51 C52 110.3(4) . . ?
C151 C152 H15A 109.5 . . ?
C151 C152 H15B 109.5 . . ?
H15A C152 H15B 109.5 . . ?
C151 C152 H15C 109.5 . . ?
H15A C152 H15C 109.5 . . ?
H15B C152 H15C 109.5 . . ?
N301 C301 C302 112.0(4) . . ?
N301 C301 H30D 109.2 . . ?
C302 C301 H30D 109.2 . . ?
N301 C301 H30E 109.2 . . ?
C302 C301 H30E 109.2 . . ?
H30D C301 H30E 107.9 . . ?
C6 C7 H7A 109.5 . . ?
C6 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C6 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C354 C351 C352 110.3(5) . . ?
C354 C351 C353 108.6(4) . . ?
C352 C351 C353 108.1(5) . . ?
C354 C351 C322 108.4(5) . . ?
C352 C351 C322 109.8(4) . . ?
C353 C351 C322 111.7(4) . . ?
C2 C3 C4 102.9(4) . . ?
C2 C3 H3A 111.2 . . ?
C4 C3 H3A 111.2 . . ?
C2 C3 H3B 111.2 . . ?
C4 C3 H3B 111.2 . . ?
H3A C3 H3B 109.1 . . ?
C113 C112 C111 117.8(4) . . ?
C113 C112 C131 120.7(4) . . ?
C111 C112 C131 121.5(5) . . ?
C124 C125 C126 121.1(5) . . ?
C124 C125 H125 119.5 . . ?
C126 C125 H125 119.5 . . ?
N102 C102 C103 105.7(4) . . ?
N102 C102 C101 111.7(4) . . ?
C103 C102 C101 110.9(4) . . ?
N102 C102 H102 109.4 . . ?
C103 C102 H102 109.4 . . ?
C101 C102 H102 109.4 . . ?
C213 C214 C215 116.8(5) . . ?
C213 C214 C241 122.9(4) . . ?
C215 C214 C241 120.2(4) . . ?
C111 C116 C115 119.9(4) . . ?
C111 C116 C129 123.9(5) . . ?
C115 C116 C129 116.1(4) . . ?
N301 C317 C316 116.8(4) . . ?
N301 C317 H31A 108.1 . . ?
C316 C317 H31A 108.1 . . ?
N301 C317 H31B 108.1 . . ?
C316 C317 H31B 108.1 . . ?
H31A C317 H31B 107.3 . . ?
C41 C43 H43A 109.5 . . ?
C41 C43 H43B 109.5 . . ?
H43A C43 H43B 109.5 . . ?
C41 C43 H43C 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
C225 C224 C223 117.4(5) . . ?
C225 C224 C261 119.9(5) . . ?
C223 C224 C261 122.6(5) . . ?
C235 C232 C212 113.1(4) . . ?
C235 C232 C234 108.3(4) . . ?
C212 C232 C234 112.5(4) . . ?
C235 C232 C233 108.4(5) . . ?
C212 C232 C233 107.5(4) . . ?
C234 C232 C233 106.8(5) . . ?
C323 C324 C325 117.3(5) . . ?
C323 C324 C361 122.6(5) . . ?
C325 C324 C361 120.0(5) . . ?
C312 C313 C314 123.7(5) . . ?
C312 C313 H313 118.2 . . ?
C314 C313 H313 118.2 . . ?
C325 C326 C321 119.4(5) . . ?
C325 C326 C327 123.1(5) . . ?
C321 C326 C327 116.8(5) . . ?
C315 C316 C311 119.6(4) . . ?
C315 C316 C317 117.0(4) . . ?
C311 C316 C317 123.4(4) . . ?
C324 C361 C363 109.2(5) . . ?
C324 C361 C362 112.6(5) . . ?
C363 C361 C362 107.7(5) . . ?
C324 C361 C364 109.7(5) . . ?
C363 C361 C364 110.4(5) . . ?
C362 C361 C364 107.3(5) . . ?
C314 C315 C316 123.5(5) . . ?
C314 C315 H315 118.3 . . ?
C316 C315 H315 118.3 . . ?
C114 C115 C116 123.2(5) . . ?
C114 C115 H115 118.4 . . ?
C116 C115 H115 118.4 . . ?
C326 C327 N301 115.3(4) . . ?
C326 C327 H32A 108.5 . . ?
N301 C327 H32A 108.5 . . ?
C326 C327 H32B 108.5 . . ?
N301 C327 H32B 108.5 . . ?
H32A C327 H32B 107.5 . . ?
C31 C33 H33A 109.5 . . ?
C31 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
C31 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
O303 C308 C310 109.7(5) . . ?
O303 C308 C309 112.2(4) . . ?
C310 C308 C309 112.9(5) . . ?
O303 C308 H308 107.2 . . ?
C310 C308 H308 107.2 . . ?
C309 C308 H308 107.2 . . ?
O202 C221 C226 116.3(5) . . ?
O202 C221 C222 123.2(5) . . ?
C226 C221 C222 120.5(4) . . ?
C241 C244 H24A 109.5 . . ?
C241 C244 H24B 109.5 . . ?
H24A C244 H24B 109.5 . . ?
C241 C244 H24C 109.5 . . ?
H24A C244 H24C 109.5 . . ?
H24B C244 H24C 109.5 . . ?
C163 C161 C124 112.2(4) . . ?
C163 C161 C162 108.1(5) . . ?
C124 C161 C162 110.8(4) . . ?
C163 C161 C164 108.2(4) . . ?
C124 C161 C164 107.8(4) . . ?
C162 C161 C164 109.7(4) . . ?
C254 C251 C222 112.7(4) . . ?
C254 C251 C253 107.2(4) . . ?
C222 C251 C253 112.6(4) . . ?
C254 C251 C252 108.3(4) . . ?
C222 C251 C252 107.9(4) . . ?
C253 C251 C252 108.0(4) . . ?
C251 C253 H25A 109.5 . . ?
C251 C253 H25B 109.5 . . ?
H25A C253 H25B 109.5 . . ?
C251 C253 H25C 109.5 . . ?
H25A C253 H25C 109.5 . . ?
H25B C253 H25C 109.5 . . ?
C51 C53 H53A 109.5 . . ?
C51 C53 H53B 109.5 . . ?
H53A C53 H53B 109.5 . . ?
C51 C53 H53C 109.5 . . ?
H53A C53 H53C 109.5 . . ?
H53B C53 H53C 109.5 . . ?
C31 C34 H34A 109.5 . . ?
C31 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
C31 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C202 C203 C204 102.7(5) . . ?
C202 C203 H20A 111.2 . . ?
C204 C203 H20A 111.2 . . ?
C202 C203 H20B 111.2 . . ?
C204 C203 H20B 111.2 . . ?
H20A C203 H20B 109.1 . . ?
N302 C305 C304 106.5(4) . . ?
N302 C305 H30F 110.4 . . ?
C304 C305 H30F 110.4 . . ?
N302 C305 H30G 110.4 . . ?
C304 C305 H30G 110.4 . . ?
H30F C305 H30G 108.6 . . ?
C331 C333 H33D 109.5 . . ?
C331 C333 H33E 109.5 . . ?
H33D C333 H33E 109.5 . . ?
C331 C333 H33F 109.5 . . ?
H33D C333 H33F 109.5 . . ?
H33E C333 H33F 109.5 . . ?
C51 C54 H54A 109.5 . . ?
C51 C54 H54B 109.5 . . ?
H54A C54 H54B 109.5 . . ?
C51 C54 H54C 109.5 . . ?
H54A C54 H54C 109.5 . . ?
H54B C54 H54C 109.5 . . ?
N202 C202 C203 105.9(4) . . ?
N202 C202 C201 111.6(4) . . ?
C203 C202 C201 108.9(5) . . ?
N202 C202 H202 110.1 . . ?
C203 C202 H202 110.1 . . ?
C201 C202 H202 110.1 . . ?
C51 C52 H52A 109.5 . . ?
C51 C52 H52B 109.5 . . ?
H52A C52 H52B 109.5 . . ?
C51 C52 H52C 109.5 . . ?
H52A C52 H52C 109.5 . . ?
H52B C52 H52C 109.5 . . ?
C107 C106 N102 116.0(5) . . ?
C107 C106 H10C 108.3 . . ?
N102 C106 H10C 108.3 . . ?
C107 C106 H10D 108.3 . . ?
N102 C106 H10D 108.3 . . ?
H10C C106 H10D 107.4 . . ?
C241 C243 H24D 109.5 . . ?
C241 C243 H24E 109.5 . . ?
H24D C243 H24E 109.5 . . ?
C241 C243 H24F 109.5 . . ?
H24D C243 H24F 109.5 . . ?
H24E C243 H24F 109.5 . . ?
C331 C332 H33G 109.5 . . ?
C331 C332 H33H 109.5 . . ?
H33G C332 H33H 109.5 . . ?
C331 C332 H33I 109.5 . . ?
H33G C332 H33I 109.5 . . ?
H33H C332 H33I 109.5 . . ?
C261 C264 H26A 109.5 . . ?
C261 C264 H26B 109.5 . . ?
H26A C264 H26B 109.5 . . ?
C261 C264 H26C 109.5 . . ?
H26A C264 H26C 109.5 . . ?
H26B C264 H26C 109.5 . . ?
N201 C201 C202 114.5(4) . . ?
N201 C201 H20C 108.6 . . ?
C202 C201 H20C 108.6 . . ?
N201 C201 H20D 108.6 . . ?
C202 C201 H20D 108.6 . . ?
H20C C201 H20D 107.6 . . ?
C134 C131 C132 107.3(5) . . ?
C134 C131 C133 108.1(5) . . ?
C132 C131 C133 109.9(5) . . ?
C134 C131 C112 112.5(5) . . ?
C132 C131 C112 109.9(5) . . ?
C133 C131 C112 109.0(4) . . ?
C241 C242 H24G 109.5 . . ?
C241 C242 H24H 109.5 . . ?
H24G C242 H24H 109.5 . . ?
C241 C242 H24I 109.5 . . ?
H24G C242 H24I 109.5 . . ?
H24H C242 H24I 109.5 . . ?
C264 C261 C263 109.1(4) . . ?
C264 C261 C224 109.2(5) . . ?
C263 C261 C224 112.1(5) . . ?
C264 C261 C262 110.6(5) . . ?
C263 C261 C262 106.8(5) . . ?
C224 C261 C262 109.1(4) . . ?
C205 C204 C203 102.1(5) . . ?
C205 C204 H20E 111.3 . . ?
C203 C204 H20E 111.3 . . ?
C205 C204 H20F 111.3 . . ?
C203 C204 H20F 111.3 . . ?
H20E C204 H20F 109.2 . . ?
C251 C254 H25D 109.5 . . ?
C251 C254 H25E 109.5 . . ?
H25D C254 H25E 109.5 . . ?
C251 C254 H25F 109.5 . . ?
H25D C254 H25F 109.5 . . ?
H25E C254 H25F 109.5 . . ?
C303 C304 C305 104.3(5) . . ?
C303 C304 H30H 110.9 . . ?
C305 C304 H30H 110.9 . . ?
C303 C304 H30I 110.9 . . ?
C305 C304 H30I 110.9 . . ?
H30H C304 H30I 108.9 . . ?
C261 C262 H26D 109.5 . . ?
C261 C262 H26E 109.5 . . ?
H26D C262 H26E 109.5 . . ?
C261 C262 H26F 109.5 . . ?
H26D C262 H26F 109.5 . . ?
H26E C262 H26F 109.5 . . ?
C41 C42 H42A 109.5 . . ?
C41 C42 H42B 109.5 . . ?
H42A C42 H42B 109.5 . . ?
C41 C42 H42C 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
C161 C164 H16A 109.5 . . ?
C161 C164 H16B 109.5 . . ?
H16A C164 H16B 109.5 . . ?
C161 C164 H16C 109.5 . . ?
H16A C164 H16C 109.5 . . ?
H16B C164 H16C 109.5 . . ?
C108 C110 H11A 109.5 . . ?
C108 C110 H11B 109.5 . . ?
H11A C110 H11B 109.5 . . ?
C108 C110 H11C 109.5 . . ?
H11A C110 H11C 109.5 . . ?
H11B C110 H11C 109.5 . . ?
C232 C235 H23A 109.5 . . ?
C232 C235 H23B 109.5 . . ?
H23A C235 H23B 109.5 . . ?
C232 C235 H23C 109.5 . . ?
H23A C235 H23C 109.5 . . ?
H23B C235 H23C 109.5 . . ?
O103 C108 C109 108.1(5) . . ?
O103 C108 C110 111.4(4) . . ?
C109 C108 C110 113.0(5) . . ?
O103 C108 H108 108.0 . . ?
C109 C108 H108 108.0 . . ?
C110 C108 H108 108.0 . . ?
C142 C141 C144 113.4(16) . . ?
C142 C141 C114 110.1(8) . . ?
C147 C141 C114 112.1(10) . . ?
C144 C141 C114 114.0(17) . . ?
C147 C141 C146 108.7(11) . . ?
C114 C141 C146 113.8(7) . . ?
C142 C141 C143 107.7(13) . . ?
C144 C141 C143 105.1(15) . . ?
C114 C141 C143 105.9(10) . . ?
C147 C141 C145 108.1(9) . . ?
C114 C141 C145 107.4(6) . . ?
C146 C141 C145 106.5(9) . . ?
C104 C105 N102 107.6(4) . . ?
C104 C105 H10E 110.2 . . ?
N102 C105 H10E 110.2 . . ?
C104 C105 H10F 110.2 . . ?
N102 C105 H10F 110.2 . . ?
H10E C105 H10F 108.5 . . ?
C31 C32 H32C 109.5 . . ?
C31 C32 H32D 109.5 . . ?
H32C C32 H32D 109.5 . . ?
C31 C32 H32E 109.5 . . ?
H32C C32 H32E 109.5 . . ?
H32D C32 H32E 109.5 . . ?
C207 C206 N202 114.3(5) . . ?
C207 C206 H20G 108.7 . . ?
N202 C206 H20G 108.7 . . ?
C207 C206 H20H 108.7 . . ?
N202 C206 H20H 108.7 . . ?
H20G C206 H20H 107.6 . . ?
C161 C162 H16D 109.5 . . ?
C161 C162 H16E 109.5 . . ?
H16D C162 H16E 109.5 . . ?
C161 C162 H16F 109.5 . . ?
H16D C162 H16F 109.5 . . ?
H16E C162 H16F 109.5 . . ?
N302 C302 C303 106.3(4) . . ?
N302 C302 C301 111.3(4) . . ?
C303 C302 C301 109.8(4) . . ?
N302 C302 H302 109.8 . . ?
C303 C302 H302 109.8 . . ?
C301 C302 H302 109.8 . . ?
C102 C103 C104 102.3(4) . . ?
C102 C103 H10G 111.3 . . ?
C104 C103 H10G 111.3 . . ?
C102 C103 H10H 111.3 . . ?
C104 C103 H10H 111.3 . . ?
H10G C103 H10H 109.2 . . ?
C261 C263 H26G 109.5 . . ?
C261 C263 H26H 109.5 . . ?
H26G C263 H26H 109.5 . . ?
C261 C263 H26I 109.5 . . ?
H26G C263 H26I 109.5 . . ?
H26H C263 H26I 109.5 . . ?
C351 C354 H35A 109.5 . . ?
C351 C354 H35B 109.5 . . ?
H35A C354 H35B 109.5 . . ?
C351 C354 H35C 109.5 . . ?
H35A C354 H35C 109.5 . . ?
H35B C354 H35C 109.5 . . ?
N302 C306 C307 116.0(5) . . ?
N302 C306 H30J 108.3 . . ?
C307 C306 H30J 108.3 . . ?
N302 C306 H30K 108.3 . . ?
C307 C306 H30K 108.3 . . ?
H30J C306 H30K 107.4 . . ?
C131 C134 H13A 109.5 . . ?
C131 C134 H13B 109.5 . . ?
H13A C134 H13B 109.5 . . ?
C131 C134 H13C 109.5 . . ?
H13A C134 H13C 109.5 . . ?
H13B C134 H13C 109.5 . . ?
C331 C334 H33J 109.5 . . ?
C331 C334 H33K 109.5 . . ?
H33J C334 H33K 109.5 . . ?
C331 C334 H33L 109.5 . . ?
H33J C334 H33L 109.5 . . ?
H33K C334 H33L 109.5 . . ?
O203 C208 C209 108.8(5) . . ?
O203 C208 C210 113.5(5) . . ?
C209 C208 C210 115.5(7) . . ?
O203 C208 H208 106.1 . . ?
C209 C208 H208 106.1 . . ?
C210 C208 H208 106.1 . . ?
C351 C353 H35D 109.5 . . ?
C351 C353 H35E 109.5 . . ?
H35D C353 H35E 109.5 . . ?
C351 C353 H35F 109.5 . . ?
H35D C353 H35F 109.5 . . ?
H35E C353 H35F 109.5 . . ?
C106 C107 H10J 109.5 . . ?
C106 C107 H10K 109.5 . . ?
H10J C107 H10K 109.5 . . ?
C106 C107 H10L 109.5 . . ?
H10J C107 H10L 109.5 . . ?
H10K C107 H10L 109.5 . . ?
C8 C9 H9A 109.5 . . ?
C8 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C8 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C41 C44 H44A 109.5 . . ?
C41 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
C41 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
C341 C344 H34D 109.5 . . ?
C341 C344 H34E 109.5 . . ?
H34D C344 H34E 109.5 . . ?
C341 C344 H34F 109.5 . . ?
H34D C344 H34F 109.5 . . ?
H34E C344 H34F 109.5 . . ?
C151 C154 H15D 109.5 . . ?
C151 C154 H15E 109.5 . . ?
H15D C154 H15E 109.5 . . ?
C151 C154 H15F 109.5 . . ?
H15D C154 H15F 109.5 . . ?
H15E C154 H15F 109.5 . . ?
C161 C163 H16G 109.5 . . ?
C161 C163 H16H 109.5 . . ?
H16G C163 H16H 109.5 . . ?
C161 C163 H16I 109.5 . . ?
H16G C163 H16I 109.5 . . ?
H16H C163 H16I 109.5 . . ?
C8 C10 H10M 109.5 . . ?
C8 C10 H10N 109.5 . . ?
H10M C10 H10N 109.5 . . ?
C8 C10 H10O 109.5 . . ?
H10M C10 H10O 109.5 . . ?
H10N C10 H10O 109.5 . . ?
C232 C234 H23D 109.5 . . ?
C232 C234 H23E 109.5 . . ?
H23D C234 H23E 109.5 . . ?
C232 C234 H23F 109.5 . . ?
H23D C234 H23F 109.5 . . ?
H23E C234 H23F 109.5 . . ?
C351 C352 H35G 109.5 . . ?
C351 C352 H35H 109.5 . . ?
H35G C352 H35H 109.5 . . ?
C351 C352 H35I 109.5 . . ?
H35G C352 H35I 109.5 . . ?
H35H C352 H35I 109.5 . . ?
O3 C8 C9 113.4(5) . . ?
O3 C8 C10 107.8(5) . . ?
C9 C8 C10 113.9(6) . . ?
O3 C8 H8 107.1 . . ?
C9 C8 H8 107.1 . . ?
C10 C8 H8 107.1 . . ?
C341 C342 H34G 109.5 . . ?
C341 C342 H34H 109.5 . . ?
H34G C342 H34H 109.5 . . ?
C341 C342 H34I 109.5 . . ?
H34G C342 H34I 109.5 . . ?
H34H C342 H34I 109.5 . . ?
C304 C303 C302 102.7(5) . . ?
C304 C303 H30L 111.2 . . ?
C302 C303 H30L 111.2 . . ?
C304 C303 H30M 111.2 . . ?
C302 C303 H30M 111.2 . . ?
H30L C303 H30M 109.1 . . ?
C151 C153 H15G 109.5 . . ?
C151 C153 H15H 109.5 . . ?
H15G C153 H15H 109.5 . . ?
C151 C153 H15I 109.5 . . ?
H15G C153 H15I 109.5 . . ?
H15H C153 H15I 109.5 . . ?
C341 C343 H34J 109.5 . . ?
C341 C343 H34K 109.5 . . ?
H34J C343 H34K 109.5 . . ?
C341 C343 H34L 109.5 . . ?
H34J C343 H34L 109.5 . . ?
H34K C343 H34L 109.5 . . ?
C251 C252 H25G 109.5 . . ?
C251 C252 H25H 109.5 . . ?
H25G C252 H25H 109.5 . . ?
C251 C252 H25I 109.5 . . ?
H25G C252 H25I 109.5 . . ?
H25H C252 H25I 109.5 . . ?
C105 C104 C103 102.6(4) . . ?
C105 C104 H10P 111.3 . . ?
C103 C104 H10P 111.3 . . ?
C105 C104 H10Q 111.3 . . ?
C103 C104 H10Q 111.3 . . ?
H10P C104 H10Q 109.2 . . ?
C108 C109 H10R 109.5 . . ?
C108 C109 H10S 109.5 . . ?
H10R C109 H10S 109.5 . . ?
C108 C109 H10T 109.5 . . ?
H10R C109 H10T 109.5 . . ?
H10S C109 H10T 109.5 . . ?
C131 C133 H13D 109.5 . . ?
C131 C133 H13E 109.5 . . ?
H13D C133 H13E 109.5 . . ?
C131 C133 H13F 109.5 . . ?
H13D C133 H13F 109.5 . . ?
H13E C133 H13F 109.5 . . ?
C204 C205 N202 107.1(4) . . ?
C204 C205 H20I 110.3 . . ?
N202 C205 H20I 110.3 . . ?
C204 C205 H20J 110.3 . . ?
N202 C205 H20J 110.3 . . ?
H20I C205 H20J 108.6 . . ?
C361 C362 H36A 109.5 . . ?
C361 C362 H36B 109.5 . . ?
H36A C362 H36B 109.5 . . ?
C361 C362 H36C 109.5 . . ?
H36A C362 H36C 109.5 . . ?
H36B C362 H36C 109.5 . . ?
C308 C310 H31C 109.5 . . ?
C308 C310 H31D 109.5 . . ?
H31C C310 H31D 109.5 . . ?
C308 C310 H31E 109.5 . . ?
H31C C310 H31E 109.5 . . ?
H31D C310 H31E 109.5 . . ?
C361 C364 H36D 109.5 . . ?
C361 C364 H36E 109.5 . . ?
H36D C364 H36E 109.5 . . ?
C361 C364 H36F 109.5 . . ?
H36D C364 H36F 109.5 . . ?
H36E C364 H36F 109.5 . . ?
C131 C132 H13G 109.5 . . ?
C131 C132 H13H 109.5 . . ?
H13G C132 H13H 109.5 . . ?
C131 C132 H13I 109.5 . . ?
H13G C132 H13I 109.5 . . ?
H13H C132 H13I 109.5 . . ?
C232 C233 H23G 109.5 . . ?
C232 C233 H23H 109.5 . . ?
H23G C233 H23H 109.5 . . ?
C232 C233 H23I 109.5 . . ?
H23G C233 H23I 109.5 . . ?
H23H C233 H23I 109.5 . . ?
C361 C363 H36G 109.5 . . ?
C361 C363 H36H 109.5 . . ?
H36G C363 H36H 109.5 . . ?
C361 C363 H36I 109.5 . . ?
H36G C363 H36I 109.5 . . ?
H36H C363 H36I 109.5 . . ?
C206 C207 H20K 109.5 . . ?
C206 C207 H20L 109.5 . . ?
H20K C207 H20L 109.5 . . ?
C206 C207 H20M 109.5 . . ?
H20K C207 H20M 109.5 . . ?
H20L C207 H20M 109.5 . . ?
C208 C209 H20N 109.5 . . ?
C208 C209 H20O 109.5 . . ?
H20N C209 H20O 109.5 . . ?
C208 C209 H20P 109.5 . . ?
H20N C209 H20P 109.5 . . ?
H20O C209 H20P 109.5 . . ?
C5 C4 C3 106.4(5) . . ?
C5 C4 H4A 110.5 . . ?
C3 C4 H4A 110.5 . . ?
C5 C4 H4B 110.5 . . ?
C3 C4 H4B 110.5 . . ?
H4A C4 H4B 108.6 . . ?
C306 C307 H30N 109.5 . . ?
C306 C307 H30O 109.5 . . ?
H30N C307 H30O 109.5 . . ?
C306 C307 H30P 109.5 . . ?
H30N C307 H30P 109.5 . . ?
H30O C307 H30P 109.5 . . ?
C208 C210 H21C 109.5 . . ?
C208 C210 H21D 109.5 . . ?
H21C C210 H21D 109.5 . . ?
C208 C210 H21E 109.5 . . ?
H21C C210 H21E 109.5 . . ?
H21D C210 H21E 109.5 . . ?
C141 C142 H14A 109.5 . . ?
C141 C142 H14B 109.5 . . ?
H14A C142 H14B 109.5 . . ?
C141 C142 H14C 109.5 . . ?
H14A C142 H14C 109.5 . . ?
H14B C142 H14C 109.5 . . ?
C141 C143 H14D 109.5 . . ?
C141 C143 H14E 109.5 . . ?
H14D C143 H14E 109.5 . . ?
C141 C143 H14F 109.5 . . ?
H14D C143 H14F 109.5 . . ?
H14E C143 H14F 109.5 . . ?
C141 C144 H14G 109.5 . . ?
C141 C144 H14H 109.5 . . ?
H14G C144 H14H 109.5 . . ?
C141 C144 H14I 109.5 . . ?
H14G C144 H14I 109.5 . . ?
H14H C144 H14I 109.5 . . ?
C141 C145 H14J 109.5 . . ?
C141 C145 H14K 109.5 . . ?
H14J C145 H14K 109.5 . . ?
C141 C145 H14L 109.5 . . ?
H14J C145 H14L 109.5 . . ?
H14K C145 H14L 109.5 . . ?
C141 C146 H14M 109.5 . . ?
C141 C146 H14N 109.5 . . ?
H14M C146 H14N 109.5 . . ?
C141 C146 H14O 109.5 . . ?
H14M C146 H14O 109.5 . . ?
H14N C146 H14O 109.5 . . ?
C141 C147 H14P 109.5 . . ?
C141 C147 H14Q 109.5 . . ?
H14P C147 H14Q 109.5 . . ?
C141 C147 H14R 109.5 . . ?
H14P C147 H14R 109.5 . . ?
H14Q C147 H14R 109.5 . . ?
C61 C62 H62A 109.5 . . ?
C61 C62 H62B 109.5 . . ?
H62A C62 H62B 109.5 . . ?
C61 C62 H62C 109.5 . . ?
H62A C62 H62C 109.5 . . ?
H62B C62 H62C 109.5 . . ?
C61 C64 H64A 109.5 . . ?
C61 C64 H64B 109.5 . . ?
H64A C64 H64B 109.5 . . ?
C61 C64 H64C 109.5 . . ?
H64A C64 H64C 109.5 . . ?
H64B C64 H64C 109.5 . . ?
C61 C66 H66A 109.5 . . ?
C61 C66 H66B 109.5 . . ?
H66A C66 H66B 109.5 . . ?
C61 C66 H66C 109.5 . . ?
H66A C66 H66C 109.5 . . ?
H66B C66 H66C 109.5 . . ?
C61 C63 H63A 109.5 . . ?
C61 C63 H63B 109.5 . . ?
H63A C63 H63B 109.5 . . ?
C61 C63 H63C 109.5 . . ?
H63A C63 H63C 109.5 . . ?
H63B C63 H63C 109.5 . . ?
C61 C65 H65A 109.5 . . ?
C61 C65 H65B 109.5 . . ?
H65A C65 H65B 109.5 . . ?
C61 C65 H65C 109.5 . . ?
H65A C65 H65C 109.5 . . ?
H65B C65 H65C 109.5 . . ?
C61 C67 H67A 109.5 . . ?
C61 C67 H67B 109.5 . . ?
H67A C67 H67B 109.5 . . ?
C61 C67 H67C 109.5 . . ?
H67A C67 H67C 109.5 . . ?
H67B C67 H67C 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
O4 V1 O1 C21 33.3(4) . . . . ?
O3 V1 O1 C21 141.9(4) . . . . ?
O2 V1 O1 C21 -82.8(6) . . . . ?
N1 V1 O1 C21 -62.5(4) . . . . ?
N2 V1 O1 C21 -137.9(4) . . . . ?
O4 V1 O3 C8 -30.5(6) . . . . ?
O1 V1 O3 C8 -128.3(5) . . . . ?
O2 V1 O3 C8 65.0(6) . . . . ?
N1 V1 O3 C8 152.8(5) . . . . ?
N2 V1 O3 C8 149.9(6) . . . . ?
O204 V3 O201 C211 38.2(4) . . . . ?
O203 V3 O201 C211 145.9(4) . . . . ?
O202 V3 O201 C211 -86.7(6) . . . . ?
N201 V3 O201 C211 -54.9(4) . . . . ?
N202 V3 O201 C211 -129.5(4) . . . . ?
O304 V4 O303 C308 17.3(6) . . . . ?
O302 V4 O303 C308 115.8(6) . . . . ?
O301 V4 O303 C308 -79.6(6) . . . . ?
N301 V4 O303 C308 -154.1(5) . . . . ?
N302 V4 O303 C308 -161.5(6) . . . . ?
O104 V2 O103 C108 21.4(6) . . . . ?
O101 V2 O103 C108 -75.6(6) . . . . ?
O102 V2 O103 C108 119.8(5) . . . . ?
N101 V2 O103 C108 -147.6(5) . . . . ?
N102 V2 O103 C108 -160.4(6) . . . . ?
O304 V4 O302 C321 -33.2(4) . . . . ?
O303 V4 O302 C321 -141.9(4) . . . . ?
O301 V4 O302 C321 89.7(6) . . . . ?
N301 V4 O302 C321 60.2(4) . . . . ?
N302 V4 O302 C321 136.1(4) . . . . ?
O204 V3 O203 C208 30.7(7) . . . . ?
O201 V3 O203 C208 -66.6(6) . . . . ?
O202 V3 O203 C208 129.2(6) . . . . ?
N201 V3 O203 C208 -139.8(6) . . . . ?
N202 V3 O203 C208 -151.5(6) . . . . ?
V1 O2 C11 C16 -64.3(5) . . . . ?
V1 O2 C11 C12 118.0(4) . . . . ?
V3 O201 C211 C216 35.5(7) . . . . ?
V3 O201 C211 C212 -144.7(4) . . . . ?
O2 C11 C16 C15 176.7(4) . . . . ?
C12 C11 C16 C15 -5.6(7) . . . . ?
O2 C11 C16 C17 -7.5(6) . . . . ?
C12 C11 C16 C17 170.1(4) . . . . ?
V2 O101 C111 C116 40.0(7) . . . . ?
V2 O101 C111 C112 -143.9(4) . . . . ?
C27 N1 C1 C2 -170.3(4) . . . . ?
C17 N1 C1 C2 73.3(5) . . . . ?
V1 N1 C1 C2 -51.8(5) . . . . ?
C15 C14 C13 C12 -0.3(8) . . . . ?
C41 C14 C13 C12 178.6(5) . . . . ?
C13 C14 C15 C16 0.9(7) . . . . ?
C41 C14 C15 C16 -177.9(5) . . . . ?
C11 C16 C15 C14 2.0(7) . . . . ?
C17 C16 C15 C14 -173.5(4) . . . . ?
C214 C215 C216 C211 1.4(8) . . . . ?
C214 C215 C216 C217 -176.7(5) . . . . ?
O201 C211 C216 C215 175.2(5) . . . . ?
C212 C211 C216 C215 -4.5(8) . . . . ?
O201 C211 C216 C217 -6.8(8) . . . . ?
C212 C211 C216 C217 173.5(5) . . . . ?
C6 N2 C2 C3 101.8(4) . . . . ?
C5 N2 C2 C3 -19.1(5) . . . . ?
V1 N2 C2 C3 -137.3(3) . . . . ?
C6 N2 C2 C1 -138.4(4) . . . . ?
C5 N2 C2 C1 100.7(4) . . . . ?
V1 N2 C2 C1 -17.5(4) . . . . ?
N1 C1 C2 N2 45.9(5) . . . . ?
N1 C1 C2 C3 164.2(4) . . . . ?
V2 O102 C121 C122 123.5(4) . . . . ?
V2 O102 C121 C126 -59.5(6) . . . . ?
C201 N201 C217 C216 59.7(5) . . . . ?
C227 N201 C217 C216 177.7(4) . . . . ?
V3 N201 C217 C216 -60.0(5) . . . . ?
C215 C216 C217 N201 -154.6(5) . . . . ?
C211 C216 C217 N201 27.3(7) . . . . ?
V4 O301 C311 C316 37.6(7) . . . . ?
V4 O301 C311 C312 -145.2(4) . . . . ?
C1 N1 C27 C26 64.8(5) . . . . ?
C17 N1 C27 C26 -177.2(4) . . . . ?
V1 N1 C27 C26 -54.4(5) . . . . ?
V1 O1 C21 C26 45.7(6) . . . . ?
V1 O1 C21 C22 -136.6(4) . . . . ?
C23 C22 C21 O1 -175.6(4) . . . . ?
C51 C22 C21 O1 5.7(7) . . . . ?
C23 C22 C21 C26 2.0(7) . . . . ?
C51 C22 C21 C26 -176.6(4) . . . . ?
O102 C121 C122 C123 -178.3(4) . . . . ?
C126 C121 C122 C123 4.8(7) . . . . ?
O102 C121 C122 C151 6.4(7) . . . . ?
C126 C121 C122 C151 -170.5(5) . . . . ?
O301 C311 C312 C313 -177.6(5) . . . . ?
C316 C311 C312 C313 -0.4(8) . . . . ?
O301 C311 C312 C331 0.2(8) . . . . ?
C316 C311 C312 C331 177.4(5) . . . . ?
O1 C21 C26 C25 175.0(4) . . . . ?
C22 C21 C26 C25 -2.6(7) . . . . ?
O1 C21 C26 C27 -9.1(7) . . . . ?
C22 C21 C26 C27 173.2(5) . . . . ?
N1 C27 C26 C21 22.1(7) . . . . ?
N1 C27 C26 C25 -161.9(4) . . . . ?
V4 O302 C321 C322 123.5(4) . . . . ?
V4 O302 C321 C326 -59.5(6) . . . . ?
C323 C322 C321 O302 -178.2(5) . . . . ?
C351 C322 C321 O302 4.7(7) . . . . ?
C323 C322 C321 C326 5.0(7) . . . . ?
C351 C322 C321 C326 -172.2(5) . . . . ?
C15 C14 C41 C44 103.9(6) . . . . ?
C13 C14 C41 C44 -74.9(6) . . . . ?
C15 C14 C41 C42 -17.3(7) . . . . ?
C13 C14 C41 C42 163.9(5) . . . . ?
C15 C14 C41 C43 -135.8(5) . . . . ?
C13 C14 C41 C43 45.4(7) . . . . ?
C14 C13 C12 C11 -3.1(7) . . . . ?
C14 C13 C12 C31 178.8(5) . . . . ?
O2 C11 C12 C13 -176.5(4) . . . . ?
C16 C11 C12 C13 6.0(7) . . . . ?
O2 C11 C12 C31 1.5(7) . . . . ?
C16 C11 C12 C31 -176.0(4) . . . . ?
C32 C31 C12 C13 103.4(5) . . . . ?
C33 C31 C12 C13 -134.9(5) . . . . ?
C34 C31 C12 C13 -15.1(7) . . . . ?
C32 C31 C12 C11 -74.6(6) . . . . ?
C33 C31 C12 C11 47.2(6) . . . . ?
C34 C31 C12 C11 167.0(5) . . . . ?
O102 C121 C126 C125 177.6(5) . . . . ?
C122 C121 C126 C125 -5.3(8) . . . . ?
O102 C121 C126 C127 -12.5(7) . . . . ?
C122 C121 C126 C127 164.5(5) . . . . ?
C21 C22 C23 C24 0.9(8) . . . . ?
C51 C22 C23 C24 179.6(5) . . . . ?
C2 N2 C6 C7 -57.6(6) . . . . ?
C5 N2 C6 C7 60.7(6) . . . . ?
V1 N2 C6 C7 -179.9(4) . . . . ?
C201 N201 C227 C226 -166.0(4) . . . . ?
C217 N201 C227 C226 77.1(5) . . . . ?
V3 N201 C227 C226 -42.4(5) . . . . ?
C321 C322 C323 C324 -0.9(8) . . . . ?
C351 C322 C323 C324 176.2(5) . . . . ?
C224 C225 C226 C221 0.9(8) . . . . ?
C224 C225 C226 C227 -170.0(5) . . . . ?
N201 C227 C226 C225 -125.0(5) . . . . ?
N201 C227 C226 C221 63.7(6) . . . . ?
C2 N2 C5 C4 1.1(6) . . . . ?
C6 N2 C5 C4 -120.3(5) . . . . ?
V1 N2 C5 C4 120.6(4) . . . . ?
C129 N101 C101 C102 -171.8(4) . . . . ?
C127 N101 C101 C102 71.5(5) . . . . ?
V2 N101 C101 C102 -53.5(4) . . . . ?
C121 C122 C123 C124 -0.8(7) . . . . ?
C151 C122 C123 C124 174.5(5) . . . . ?
C125 C124 C123 C122 -2.8(8) . . . . ?
C161 C124 C123 C122 -177.7(5) . . . . ?
C313 C312 C331 C334 114.8(6) . . . . ?
C311 C312 C331 C334 -63.0(6) . . . . ?
C313 C312 C331 C333 -124.6(5) . . . . ?
C311 C312 C331 C333 57.5(7) . . . . ?
C313 C312 C331 C332 -3.7(8) . . . . ?
C311 C312 C331 C332 178.5(5) . . . . ?
C221 C222 C223 C224 -0.9(8) . . . . ?
C251 C222 C223 C224 174.0(5) . . . . ?
C315 C314 C341 C342 -109.9(6) . . . . ?
C313 C314 C341 C342 70.1(6) . . . . ?
C315 C314 C341 C344 131.0(6) . . . . ?
C313 C314 C341 C344 -48.9(7) . . . . ?
C315 C314 C341 C343 10.0(8) . . . . ?
C313 C314 C341 C343 -170.0(5) . . . . ?
C123 C122 C151 C154 3.5(7) . . . . ?
C121 C122 C151 C154 178.5(5) . . . . ?
C123 C122 C151 C152 -115.6(5) . . . . ?
C121 C122 C151 C152 59.4(6) . . . . ?
C123 C122 C151 C153 124.1(5) . . . . ?
C121 C122 C151 C153 -60.9(6) . . . . ?
C21 C26 C25 C24 0.3(8) . . . . ?
C27 C26 C25 C24 -175.9(5) . . . . ?
C26 C25 C24 C23 2.5(8) . . . . ?
C26 C25 C24 C61 -179.5(5) . . . . ?
C22 C23 C24 C25 -3.2(8) . . . . ?
C22 C23 C24 C61 178.8(5) . . . . ?
C64 C61 C24 C25 92.7(8) . . . . ?
C67 C61 C24 C25 -78.9(10) . . . . ?
C66 C61 C24 C25 -33.7(10) . . . . ?
C63 C61 C24 C25 148.5(8) . . . . ?
C65 C61 C24 C25 35.3(9) . . . . ?
C62 C61 C24 C25 -150.1(7) . . . . ?
C64 C61 C24 C23 -89.4(9) . . . . ?
C67 C61 C24 C23 99.0(10) . . . . ?
C66 C61 C24 C23 144.2(9) . . . . ?
C63 C61 C24 C23 -33.6(9) . . . . ?
C65 C61 C24 C23 -146.7(7) . . . . ?
C62 C61 C24 C23 27.9(8) . . . . ?
C112 C113 C114 C115 0.5(8) . . . . ?
C112 C113 C114 C141 178.4(5) . . . . ?
C101 N101 C129 C116 62.6(5) . . . . ?
C127 N101 C129 C116 -179.1(4) . . . . ?
V2 N101 C129 C116 -56.6(5) . . . . ?
C214 C213 C212 C211 -3.5(8) . . . . ?
C214 C213 C212 C232 173.3(5) . . . . ?
O201 C211 C212 C213 -174.4(5) . . . . ?
C216 C211 C212 C213 5.4(8) . . . . ?
O201 C211 C212 C232 8.8(8) . . . . ?
C216 C211 C212 C232 -171.4(5) . . . . ?
C125 C126 C127 N101 -126.7(5) . . . . ?
C121 C126 C127 N101 63.6(6) . . . . ?
C129 N101 C127 C126 76.5(5) . . . . ?
C101 N101 C127 C126 -164.8(4) . . . . ?
V2 N101 C127 C126 -42.3(5) . . . . ?
C11 C16 C17 N1 62.9(5) . . . . ?
C15 C16 C17 N1 -121.5(5) . . . . ?
C1 N1 C17 C16 -168.5(4) . . . . ?
C27 N1 C17 C16 74.4(5) . . . . ?
V1 N1 C17 C16 -45.5(5) . . . . ?
C23 C22 C51 C53 113.5(5) . . . . ?
C21 C22 C51 C53 -67.9(6) . . . . ?
C23 C22 C51 C54 -7.0(7) . . . . ?
C21 C22 C51 C54 171.7(5) . . . . ?
C23 C22 C51 C52 -125.7(5) . . . . ?
C21 C22 C51 C52 52.9(6) . . . . ?
C317 N301 C301 C302 -168.7(4) . . . . ?
C327 N301 C301 C302 74.7(5) . . . . ?
V4 N301 C301 C302 -50.7(5) . . . . ?
C321 C322 C351 C354 58.5(6) . . . . ?
C323 C322 C351 C354 -118.5(6) . . . . ?
C321 C322 C351 C352 -62.1(7) . . . . ?
C323 C322 C351 C352 120.9(6) . . . . ?
C321 C322 C351 C353 178.1(5) . . . . ?
C323 C322 C351 C353 1.0(7) . . . . ?
N2 C2 C3 C4 28.9(5) . . . . ?
C1 C2 C3 C4 -91.6(5) . . . . ?
C114 C113 C112 C111 0.6(8) . . . . ?
C114 C113 C112 C131 179.3(5) . . . . ?
O101 C111 C112 C113 -177.5(5) . . . . ?
C116 C111 C112 C113 -1.3(7) . . . . ?
O101 C111 C112 C131 3.9(8) . . . . ?
C116 C111 C112 C131 -179.9(5) . . . . ?
C123 C124 C125 C126 2.4(7) . . . . ?
C161 C124 C125 C126 177.1(5) . . . . ?
C121 C126 C125 C124 1.6(8) . . . . ?
C127 C126 C125 C124 -167.6(5) . . . . ?
C106 N102 C102 C103 98.4(5) . . . . ?
C105 N102 C102 C103 -18.9(5) . . . . ?
V2 N102 C102 C103 -137.9(3) . . . . ?
C106 N102 C102 C101 -140.8(4) . . . . ?
C105 N102 C102 C101 101.9(5) . . . . ?
V2 N102 C102 C101 -17.0(4) . . . . ?
N101 C101 C102 N102 46.7(5) . . . . ?
N101 C101 C102 C103 164.4(4) . . . . ?
C212 C213 C214 C215 0.4(8) . . . . ?
C212 C213 C214 C241 -176.2(5) . . . . ?
C216 C215 C214 C213 0.7(8) . . . . ?
C216 C215 C214 C241 177.4(5) . . . . ?
C243 C241 C214 C213 -15.4(7) . . . . ?
C244 C241 C214 C213 -135.6(5) . . . . ?
C242 C241 C214 C213 103.7(6) . . . . ?
C243 C241 C214 C215 168.1(5) . . . . ?
C244 C241 C214 C215 48.0(6) . . . . ?
C242 C241 C214 C215 -72.7(6) . . . . ?
O101 C111 C116 C115 177.0(5) . . . . ?
C112 C111 C116 C115 0.8(8) . . . . ?
O101 C111 C116 C129 -5.8(8) . . . . ?
C112 C111 C116 C129 178.1(5) . . . . ?
N101 C129 C116 C111 22.5(7) . . . . ?
N101 C129 C116 C115 -160.1(5) . . . . ?
C301 N301 C317 C316 62.3(6) . . . . ?
C327 N301 C317 C316 179.0(4) . . . . ?
V4 N301 C317 C316 -57.3(5) . . . . ?
C226 C225 C224 C223 2.7(8) . . . . ?
C226 C225 C224 C261 179.3(5) . . . . ?
C222 C223 C224 C225 -2.7(8) . . . . ?
C222 C223 C224 C261 -179.2(5) . . . . ?
C213 C212 C232 C235 125.7(5) . . . . ?
C211 C212 C232 C235 -57.6(7) . . . . ?
C213 C212 C232 C234 2.5(7) . . . . ?
C211 C212 C232 C234 179.2(5) . . . . ?
C213 C212 C232 C233 -114.8(6) . . . . ?
C211 C212 C232 C233 61.9(6) . . . . ?
C322 C323 C324 C325 -2.7(8) . . . . ?
C322 C323 C324 C361 -180.0(5) . . . . ?
C326 C325 C324 C323 2.2(8) . . . . ?
C326 C325 C324 C361 179.6(5) . . . . ?
C311 C312 C313 C314 -0.7(8) . . . . ?
C331 C312 C313 C314 -178.5(5) . . . . ?
C315 C314 C313 C312 1.5(8) . . . . ?
C341 C314 C313 C312 -178.5(5) . . . . ?
C324 C325 C326 C321 1.7(8) . . . . ?
C324 C325 C326 C327 -168.7(5) . . . . ?
O302 C321 C326 C325 177.5(4) . . . . ?
C322 C321 C326 C325 -5.4(7) . . . . ?
O302 C321 C326 C327 -11.5(6) . . . . ?
C322 C321 C326 C327 165.5(4) . . . . ?
O301 C311 C316 C315 177.8(5) . . . . ?
C312 C311 C316 C315 0.6(8) . . . . ?
O301 C311 C316 C317 -3.3(8) . . . . ?
C312 C311 C316 C317 179.5(5) . . . . ?
N301 C317 C316 C315 -159.4(5) . . . . ?
N301 C317 C316 C311 21.6(8) . . . . ?
C323 C324 C361 C363 110.3(6) . . . . ?
C325 C324 C361 C363 -66.9(6) . . . . ?
C323 C324 C361 C362 -9.2(8) . . . . ?
C325 C324 C361 C362 173.5(5) . . . . ?
C323 C324 C361 C364 -128.7(6) . . . . ?
C325 C324 C361 C364 54.1(7) . . . . ?
C313 C314 C315 C316 -1.4(8) . . . . ?
C341 C314 C315 C316 178.6(5) . . . . ?
C311 C316 C315 C314 0.4(8) . . . . ?
C317 C316 C315 C314 -178.6(5) . . . . ?
C113 C114 C115 C116 -1.1(8) . . . . ?
C141 C114 C115 C116 -178.9(5) . . . . ?
C111 C116 C115 C114 0.4(8) . . . . ?
C129 C116 C115 C114 -177.0(5) . . . . ?
C325 C326 C327 N301 -128.0(5) . . . . ?
C321 C326 C327 N301 61.4(6) . . . . ?
C317 N301 C327 C326 77.0(5) . . . . ?
C301 N301 C327 C326 -165.0(4) . . . . ?
V4 N301 C327 C326 -42.3(5) . . . . ?
V4 O303 C308 C310 -142.8(5) . . . . ?
V4 O303 C308 C309 -16.5(8) . . . . ?
V3 O202 C221 C226 -62.8(5) . . . . ?
V3 O202 C221 C222 119.9(4) . . . . ?
C225 C226 C221 O202 177.9(4) . . . . ?
C227 C226 C221 O202 -10.6(6) . . . . ?
C225 C226 C221 C222 -4.7(8) . . . . ?
C227 C226 C221 C222 166.7(4) . . . . ?
C223 C222 C221 O202 -178.2(4) . . . . ?
C251 C222 C221 O202 6.9(7) . . . . ?
C223 C222 C221 C226 4.6(7) . . . . ?
C251 C222 C221 C226 -170.2(4) . . . . ?
C125 C124 C161 C163 17.9(7) . . . . ?
C123 C124 C161 C163 -167.6(5) . . . . ?
C125 C124 C161 C162 138.7(5) . . . . ?
C123 C124 C161 C162 -46.7(6) . . . . ?
C125 C124 C161 C164 -101.2(6) . . . . ?
C123 C124 C161 C164 73.3(6) . . . . ?
C223 C222 C251 C254 12.6(7) . . . . ?
C221 C222 C251 C254 -172.8(5) . . . . ?
C223 C222 C251 C253 134.0(5) . . . . ?
C221 C222 C251 C253 -51.4(7) . . . . ?
C223 C222 C251 C252 -106.9(5) . . . . ?
C221 C222 C251 C252 67.7(6) . . . . ?
C306 N302 C305 C304 -125.4(5) . . . . ?
C302 N302 C305 C304 -3.2(6) . . . . ?
V4 N302 C305 C304 116.4(4) . . . . ?
C206 N202 C202 C203 108.0(5) . . . . ?
C205 N202 C202 C203 -9.5(5) . . . . ?
V3 N202 C202 C203 -128.0(4) . . . . ?
C206 N202 C202 C201 -133.6(4) . . . . ?
C205 N202 C202 C201 108.8(5) . . . . ?
V3 N202 C202 C201 -9.6(5) . . . . ?
C204 C203 C202 N202 30.8(6) . . . . ?
C204 C203 C202 C201 -89.3(5) . . . . ?
C102 N102 C106 C107 -176.8(4) . . . . ?
C105 N102 C106 C107 -62.0(6) . . . . ?
V2 N102 C106 C107 62.3(5) . . . . ?
C217 N201 C201 C202 -169.9(4) . . . . ?
C227 N201 C201 C202 73.8(5) . . . . ?
V3 N201 C201 C202 -51.5(5) . . . . ?
N202 C202 C201 N201 39.5(6) . . . . ?
C203 C202 C201 N201 156.1(4) . . . . ?
C113 C112 C131 C134 3.2(8) . . . . ?
C111 C112 C131 C134 -178.2(5) . . . . ?
C113 C112 C131 C132 122.7(6) . . . . ?
C111 C112 C131 C132 -58.7(7) . . . . ?
C113 C112 C131 C133 -116.8(6) . . . . ?
C111 C112 C131 C133 61.8(7) . . . . ?
C225 C224 C261 C264 -72.6(6) . . . . ?
C223 C224 C261 C264 103.8(6) . . . . ?
C225 C224 C261 C263 166.4(5) . . . . ?
C223 C224 C261 C263 -17.2(7) . . . . ?
C225 C224 C261 C262 48.3(7) . . . . ?
C223 C224 C261 C262 -135.3(5) . . . . ?
C202 C203 C204 C205 -40.2(6) . . . . ?
N302 C305 C304 C303 24.8(6) . . . . ?
V2 O103 C108 C109 -152.1(5) . . . . ?
V2 O103 C108 C110 -27.3(8) . . . . ?
C115 C114 C141 C142 57.5(11) . . . . ?
C113 C114 C141 C142 -120.2(11) . . . . ?
C115 C114 C141 C147 -141.0(9) . . . . ?
C113 C114 C141 C147 41.2(10) . . . . ?
C115 C114 C141 C144 -173.7(14) . . . . ?
C113 C114 C141 C144 8.5(15) . . . . ?
C115 C114 C141 C146 -17.2(11) . . . . ?
C113 C114 C141 C146 165.1(10) . . . . ?
C115 C114 C141 C143 -58.6(13) . . . . ?
C113 C114 C141 C143 123.6(12) . . . . ?
C115 C114 C141 C145 100.4(7) . . . . ?
C113 C114 C141 C145 -77.3(8) . . . . ?
C102 N102 C105 C104 -6.3(6) . . . . ?
C106 N102 C105 C104 -122.1(5) . . . . ?
V2 N102 C105 C104 111.7(4) . . . . ?
C205 N202 C206 C207 -60.1(6) . . . . ?
C202 N202 C206 C207 -174.4(5) . . . . ?
V3 N202 C206 C207 64.2(5) . . . . ?
C306 N302 C302 C303 101.0(5) . . . . ?
C305 N302 C302 C303 -19.5(5) . . . . ?
V4 N302 C302 C303 -138.6(4) . . . . ?
C306 N302 C302 C301 -139.5(5) . . . . ?
C305 N302 C302 C301 100.0(5) . . . . ?
V4 N302 C302 C301 -19.1(5) . . . . ?
N301 C301 C302 N302 46.1(6) . . . . ?
N301 C301 C302 C303 163.4(4) . . . . ?
N102 C102 C103 C104 36.0(6) . . . . ?
C101 C102 C103 C104 -85.3(5) . . . . ?
C302 N302 C306 C307 -56.0(7) . . . . ?
C305 N302 C306 C307 62.6(6) . . . . ?
V4 N302 C306 C307 -178.1(4) . . . . ?
V3 O203 C208 C209 -173.0(5) . . . . ?
V3 O203 C208 C210 -42.9(9) . . . . ?
V1 O3 C8 C9 61.0(8) . . . . ?
V1 O3 C8 C10 -172.0(4) . . . . ?
C305 C304 C303 C302 -36.0(6) . . . . ?
N302 C302 C303 C304 34.7(6) . . . . ?
C301 C302 C303 C304 -85.7(5) . . . . ?
N102 C105 C104 C103 28.3(6) . . . . ?
C102 C103 C104 C105 -39.1(6) . . . . ?
C203 C204 C205 N202 35.3(6) . . . . ?
C206 N202 C205 C204 -130.9(5) . . . . ?
C202 N202 C205 C204 -16.3(6) . . . . ?
V3 N202 C205 C204 102.3(4) . . . . ?
N2 C5 C4 C3 17.1(7) . . . . ?
C2 C3 C4 C5 -27.9(6) . . . . ?

_refine_diff_density_max         0.428
_refine_diff_density_min         -0.316
_refine_diff_density_rms         0.052



