# Electronic Supplementary Material (ESI) for New Journal of Chemistry.
# This journal is © The Royal Society of Chemistry and the Centre National de la Recherche Scientifique 2016

####################################################################### 
# 
# 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 1489208'
_audit_update_record             
;
2016-10-05 deposited with the CCDC.
2016-10-19 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C26 H18 N4 O3 V'
_chemical_formula_weight         485.38

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           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

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

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

_cell_length_a                   21.5463(13)
_cell_length_b                   8.3435(5)
_cell_length_c                   25.3092(15)
_cell_angle_alpha                90
_cell_angle_beta                 107.290(2)
_cell_angle_gamma                90
_cell_volume                     4344.3(5)
_cell_formula_units_Z            8
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    9865
_cell_measurement_theta_min      2.53
_cell_measurement_theta_max      31.73

_exptl_crystal_description       rectengular
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.484
_exptl_crystal_F_000             1992
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.05
_exptl_absorpt_coefficient_mu    0.495
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.909
_exptl_absorpt_correction_T_max  0.986
_exptl_absorpt_process_details   'APEX2 (Bruker AXS Inc. 2007)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   Mo
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            30617
_diffrn_reflns_av_unetI/netI     0.0394
_diffrn_reflns_av_R_equivalents  0.0428
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_theta_min         2.634
_diffrn_reflns_theta_max         31.952
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.888
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.888
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.888
_diffrn_reflns_point_group_measured_fraction_full 0.996
_reflns_number_total             6679
_reflns_number_gt                5386
_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 APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0001P)²+28.9755P] 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     SHELXL
_refine_ls_extinction_coef       0.00062(17)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         6679
_refine_ls_number_parameters     308
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1071
_refine_ls_R_factor_gt           0.0857
_refine_ls_wR_factor_ref         0.1845
_refine_ls_wR_factor_gt          0.1745
_refine_ls_goodness_of_fit_ref   1.242
_refine_ls_restrained_S_all      1.242
_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
C1 C 0.11609(18) 0.3134(4) 0.51728(15) 0.0318(7) Uani 1 1 d . . . . .
N1 N 0.24435(14) 0.4648(3) 0.54049(11) 0.0272(6) Uani 1 1 d . . . . .
O1 O 0.13884(13) 0.3549(3) 0.56983(11) 0.0367(6) Uani 1 1 d . . . . .
V1 V 0.22738(3) 0.40192(7) 0.61315(2) 0.02842(17) Uani 1 1 d . . . . .
C2 C 0.0560(2) 0.2315(6) 0.49915(19) 0.0460(10) Uani 1 1 d . . . . .
H2 H 0.0342 0.2049 0.5246 0.055 Uiso 1 1 calc R U . . .
N2 N 0.30134(14) 0.5534(4) 0.54520(12) 0.0309(6) Uani 1 1 d . . . . .
O2 O 0.31127(13) 0.5256(3) 0.63847(10) 0.0333(6) Uani 1 1 d . . . . .
C3 C 0.0292(2) 0.1907(6) 0.4446(2) 0.0557(13) Uani 1 1 d . . . . .
H3 H -0.0104 0.1373 0.4338 0.067 Uiso 1 1 calc R U . . .
N3 N 0.19730(14) 0.4259(4) 0.68671(12) 0.0288(6) Uani 1 1 d . . . . .
O3 O 0.25622(14) 0.2253(3) 0.62882(12) 0.0397(6) Uani 1 1 d . . . . .
C4 C 0.0600(2) 0.2275(6) 0.4054(2) 0.0545(12) Uani 1 1 d . . . . .
H4 H 0.0410 0.2007 0.3684 0.065 Uiso 1 1 calc R U . . .
N4 N 0.18756(15) 0.6638(3) 0.61433(12) 0.0285(6) Uani 1 1 d . . . . .
C5 C 0.1190(2) 0.3039(5) 0.42167(17) 0.0428(9) Uani 1 1 d . . . . .
H5 H 0.1401 0.3279 0.3955 0.051 Uiso 1 1 calc R U . . .
C6 C 0.14811(17) 0.3470(4) 0.47751(15) 0.0312(7) Uani 1 1 d . . . . .
C7 C 0.20963(18) 0.4292(4) 0.49088(14) 0.0318(7) Uani 1 1 d . . . . .
H7 H 0.2254 0.4587 0.4618 0.038 Uiso 1 1 calc R U . . .
C8 C 0.33143(16) 0.5759(4) 0.59781(14) 0.0278(7) Uani 1 1 d . . . . .
C9 C 0.39358(17) 0.6679(4) 0.61186(15) 0.0304(7) Uani 1 1 d . . . . .
C10 C 0.4088(2) 0.7663(5) 0.57325(18) 0.0422(9) Uani 1 1 d . . . . .
H10 H 0.3800 0.7747 0.5378 0.051 Uiso 1 1 calc R U . . .
C11 C 0.4662(2) 0.8518(6) 0.5870(2) 0.0511(11) Uani 1 1 d . . . . .
H11 H 0.4755 0.9186 0.5609 0.061 Uiso 1 1 calc R U . . .
C12 C 0.5095(2) 0.8387(6) 0.6386(2) 0.0559(12) Uani 1 1 d . . . . .
H12 H 0.5483 0.8957 0.6476 0.067 Uiso 1 1 calc R U . . .
C13 C 0.4953(2) 0.7406(7) 0.6775(2) 0.0580(13) Uani 1 1 d . . . . .
H13 H 0.5248 0.7312 0.7126 0.070 Uiso 1 1 calc R U . . .
C14 C 0.4372(2) 0.6561(6) 0.66442(17) 0.0440(10) Uani 1 1 d . . . . .
H14 H 0.4276 0.5915 0.6909 0.053 Uiso 1 1 calc R U . . .
C15 C 0.20178(18) 0.3059(5) 0.72243(16) 0.0361(8) Uani 1 1 d . . . . .
H15 H 0.2204 0.2100 0.7161 0.043 Uiso 1 1 calc R U . . .
C16 C 0.1798(2) 0.3175(6) 0.76879(17) 0.0443(10) Uani 1 1 d . . . . .
H16 H 0.1831 0.2301 0.7923 0.053 Uiso 1 1 calc R U . . .
C17 C 0.1535(2) 0.4578(6) 0.77944(17) 0.0462(10) Uani 1 1 d . . . . .
H17 H 0.1395 0.4675 0.8107 0.055 Uiso 1 1 calc R U . . .
C18 C 0.1477(2) 0.5876(5) 0.74305(15) 0.0394(9) Uani 1 1 d . . . . .
C19 C 0.1218(3) 0.7419(6) 0.75104(19) 0.0536(12) Uani 1 1 d . . . . .
H19 H 0.1079 0.7591 0.7820 0.064 Uiso 1 1 calc R U . . .
C20 C 0.1173(3) 0.8618(6) 0.7144(2) 0.0548(12) Uani 1 1 d . . . . .
H20 H 0.0995 0.9593 0.7203 0.066 Uiso 1 1 calc R U . . .
C21 C 0.13937(19) 0.8425(5) 0.66656(16) 0.0371(8) Uani 1 1 d . . . . .
C22 C 0.1365(2) 0.9626(5) 0.62729(19) 0.0435(10) Uani 1 1 d . . . . .
H22 H 0.1188 1.0622 0.6310 0.052 Uiso 1 1 calc R U . . .
C23 C 0.1596(2) 0.9329(5) 0.58369(18) 0.0407(9) Uani 1 1 d . . . . .
H23 H 0.1585 1.0122 0.5576 0.049 Uiso 1 1 calc R U . . .
C24 C 0.18503(19) 0.7814(4) 0.57868(16) 0.0350(8) Uani 1 1 d . . . . .
H24 H 0.2009 0.7624 0.5489 0.042 Uiso 1 1 calc R U . . .
C25 C 0.16533(16) 0.6934(4) 0.65799(14) 0.0283(7) Uani 1 1 d . . . . .
C26 C 0.17005(16) 0.5659(4) 0.69668(14) 0.0277(7) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 O1 1.320(4) . ?
C1 C6 1.407(5) . ?
C1 C2 1.415(5) . ?
N1 C7 1.291(4) . ?
N1 N2 1.408(4) . ?
N1 V1 2.047(3) . ?
O1 V1 1.937(3) . ?
V1 O3 1.602(3) . ?
V1 O2 2.014(3) . ?
V1 N3 2.155(3) . ?
V1 N4 2.351(3) . ?
C2 C3 1.372(6) . ?
C2 H2 0.9300 . ?
N2 C8 1.310(4) . ?
O2 C8 1.300(4) . ?
C3 C4 1.383(7) . ?
C3 H3 0.9300 . ?
N3 C15 1.333(4) . ?
N3 C26 1.364(4) . ?
C4 C5 1.371(6) . ?
C4 H4 0.9300 . ?
N4 C24 1.323(4) . ?
N4 C25 1.351(4) . ?
C5 C6 1.412(5) . ?
C5 H5 0.9300 . ?
C6 C7 1.441(5) . ?
C7 H7 0.9300 . ?
C8 C9 1.492(5) . ?
C9 C14 1.385(5) . ?
C9 C10 1.388(5) . ?
C10 C11 1.381(6) . ?
C10 H10 0.9300 . ?
C11 C12 1.366(7) . ?
C11 H11 0.9300 . ?
C12 C13 1.382(7) . ?
C12 H12 0.9300 . ?
C13 C14 1.389(6) . ?
C13 H13 0.9300 . ?
C14 H14 0.9300 . ?
C15 C16 1.393(5) . ?
C15 H15 0.9300 . ?
C16 C17 1.362(7) . ?
C16 H16 0.9300 . ?
C17 C18 1.403(6) . ?
C17 H17 0.9300 . ?
C18 C26 1.406(5) . ?
C18 C19 1.441(6) . ?
C19 C20 1.347(7) . ?
C19 H19 0.9300 . ?
C20 C21 1.435(6) . ?
C20 H20 0.9300 . ?
C21 C22 1.400(6) . ?
C21 C25 1.407(5) . ?
C22 C23 1.362(6) . ?
C22 H22 0.9300 . ?
C23 C24 1.399(5) . ?
C23 H23 0.9300 . ?
C24 H24 0.9300 . ?
C25 C26 1.429(5) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 C1 C6 123.7(3) . . ?
O1 C1 C2 118.9(4) . . ?
C6 C1 C2 117.4(4) . . ?
C7 N1 N2 116.2(3) . . ?
C7 N1 V1 127.5(2) . . ?
N2 N1 V1 116.3(2) . . ?
C1 O1 V1 129.2(2) . . ?
O3 V1 O1 101.43(14) . . ?
O3 V1 O2 98.45(13) . . ?
O1 V1 O2 157.50(12) . . ?
O3 V1 N1 107.35(13) . . ?
O1 V1 N1 87.26(11) . . ?
O2 V1 N1 76.79(11) . . ?
O3 V1 N3 93.76(13) . . ?
O1 V1 N3 90.54(11) . . ?
O2 V1 N3 98.60(11) . . ?
N1 V1 N3 158.80(12) . . ?
O3 V1 N4 165.38(13) . . ?
O1 V1 N4 83.90(11) . . ?
O2 V1 N4 79.40(11) . . ?
N1 V1 N4 86.36(11) . . ?
N3 V1 N4 72.43(11) . . ?
C3 C2 C1 121.1(4) . . ?
C3 C2 H2 119.5 . . ?
C1 C2 H2 119.5 . . ?
C8 N2 N1 108.5(3) . . ?
C8 O2 V1 113.1(2) . . ?
C2 C3 C4 121.4(4) . . ?
C2 C3 H3 119.3 . . ?
C4 C3 H3 119.3 . . ?
C15 N3 C26 117.8(3) . . ?
C15 N3 V1 122.4(3) . . ?
C26 N3 V1 119.7(2) . . ?
C5 C4 C3 119.1(4) . . ?
C5 C4 H4 120.5 . . ?
C3 C4 H4 120.5 . . ?
C24 N4 C25 118.0(3) . . ?
C24 N4 V1 128.4(2) . . ?
C25 N4 V1 113.5(2) . . ?
C4 C5 C6 121.1(4) . . ?
C4 C5 H5 119.5 . . ?
C6 C5 H5 119.5 . . ?
C1 C6 C5 119.9(4) . . ?
C1 C6 C7 122.6(3) . . ?
C5 C6 C7 117.4(3) . . ?
N1 C7 C6 124.4(3) . . ?
N1 C7 H7 117.8 . . ?
C6 C7 H7 117.8 . . ?
O2 C8 N2 125.3(3) . . ?
O2 C8 C9 117.7(3) . . ?
N2 C8 C9 117.0(3) . . ?
C14 C9 C10 118.9(4) . . ?
C14 C9 C8 119.8(3) . . ?
C10 C9 C8 121.3(3) . . ?
C11 C10 C9 120.7(4) . . ?
C11 C10 H10 119.7 . . ?
C9 C10 H10 119.7 . . ?
C12 C11 C10 120.3(4) . . ?
C12 C11 H11 119.8 . . ?
C10 C11 H11 119.8 . . ?
C11 C12 C13 119.8(4) . . ?
C11 C12 H12 120.1 . . ?
C13 C12 H12 120.1 . . ?
C12 C13 C14 120.4(4) . . ?
C12 C13 H13 119.8 . . ?
C14 C13 H13 119.8 . . ?
C9 C14 C13 119.9(4) . . ?
C9 C14 H14 120.0 . . ?
C13 C14 H14 120.0 . . ?
N3 C15 C16 123.0(4) . . ?
N3 C15 H15 118.5 . . ?
C16 C15 H15 118.5 . . ?
C17 C16 C15 119.5(4) . . ?
C17 C16 H16 120.3 . . ?
C15 C16 H16 120.3 . . ?
C16 C17 C18 119.7(4) . . ?
C16 C17 H17 120.2 . . ?
C18 C17 H17 120.2 . . ?
C17 C18 C26 117.5(4) . . ?
C17 C18 C19 124.1(4) . . ?
C26 C18 C19 118.4(4) . . ?
C20 C19 C18 121.2(4) . . ?
C20 C19 H19 119.4 . . ?
C18 C19 H19 119.4 . . ?
C19 C20 C21 121.6(4) . . ?
C19 C20 H20 119.2 . . ?
C21 C20 H20 119.2 . . ?
C22 C21 C25 117.4(4) . . ?
C22 C21 C20 124.2(4) . . ?
C25 C21 C20 118.4(4) . . ?
C23 C22 C21 119.7(4) . . ?
C23 C22 H22 120.2 . . ?
C21 C22 H22 120.2 . . ?
C22 C23 C24 119.0(4) . . ?
C22 C23 H23 120.5 . . ?
C24 C23 H23 120.5 . . ?
N4 C24 C23 123.1(4) . . ?
N4 C24 H24 118.4 . . ?
C23 C24 H24 118.4 . . ?
N4 C25 C21 122.8(3) . . ?
N4 C25 C26 117.0(3) . . ?
C21 C25 C26 120.2(3) . . ?
N3 C26 C18 122.5(3) . . ?
N3 C26 C25 117.2(3) . . ?
C18 C26 C25 120.3(3) . . ?

_refine_diff_density_max         0.554
_refine_diff_density_min         -0.787
_refine_diff_density_rms         0.092

_shelxl_version_number           2014/6

####################################################################### 
# 
# 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_SQ
_database_code_depnum_ccdc_archive 'CCDC 1489210'
_audit_update_record             
;
2016-10-18 deposited with the CCDC.
2016-10-19 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C25 H18 N5 O5 V'
_chemical_formula_sum            'C25 H18 N5 O5 V'
_chemical_formula_weight         519.38

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      orthorhombic
_space_group_IT_number           19
_space_group_name_H-M_alt        'P 21 21 21'
_space_group_name_Hall           'P 2ac 2ab'

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

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

_cell_length_a                   13.8584(5)
_cell_length_b                   16.1145(6)
_cell_length_c                   22.9607(9)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     5127.6(3)
_cell_formula_units_Z            8
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    9688
_cell_measurement_theta_min      2.63
_cell_measurement_theta_max      27.34

_exptl_crystal_description       prism
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.346
_exptl_crystal_F_000             2128
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.620
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.170
_exptl_absorpt_coefficient_mu    0.430
_shelx_estimated_absorpt_T_min   0.776
_shelx_estimated_absorpt_T_max   0.930
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.902
_exptl_absorpt_correction_T_max  0.950
_exptl_absorpt_process_details   'APEX2 (Bruker AXS Inc. 2007)'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   Mo
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            78927
_diffrn_reflns_av_unetI/netI     0.0409
_diffrn_reflns_av_R_equivalents  0.0602
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_theta_min         2.924
_diffrn_reflns_theta_max         27.000
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             11180
_reflns_number_gt                8993
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.818
_reflns_Friedel_fraction_max     1.000
_reflns_Friedel_fraction_full    1.000

_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 APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 w=1/[σ²(Fo²)+(0.0413P)²+1.4506P]
 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 3537 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.015(7)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         11180
_refine_ls_number_parameters     654
_refine_ls_number_restraints     124
_refine_ls_R_factor_all          0.0594
_refine_ls_R_factor_gt           0.0403
_refine_ls_wR_factor_ref         0.0954
_refine_ls_wR_factor_gt          0.0859
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_restrained_S_all      1.043
_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
O1 O 0.19270(19) 0.36575(16) 0.57421(11) 0.0451(6) Uani 1 1 d . . . . .
V1 V 0.07390(4) 0.33093(3) 0.53299(3) 0.03663(15) Uani 1 1 d . . . . .
C2 C 0.2286(3) 0.4362(2) 0.55905(16) 0.0404(9) Uani 1 1 d . . . . .
V2 V 0.41061(4) 0.45520(3) 0.38748(2) 0.03277(14) Uani 1 1 d . . . . .
C3 C 0.3248(3) 0.4589(3) 0.58320(16) 0.0476(9) Uani 1 1 d . . . . .
C4 C 0.3740(4) 0.4040(3) 0.6183(2) 0.0698(14) Uani 1 1 d . . . . .
H4 H 0.3448 0.3547 0.6299 0.084 Uiso 1 1 calc R U . . .
C5 C 0.4678(5) 0.4224(5) 0.6364(3) 0.095(2) Uani 1 1 d . . . . .
H5 H 0.5014 0.3848 0.6594 0.114 Uiso 1 1 calc R U . . .
C6 C 0.5099(4) 0.4944(6) 0.6207(3) 0.096(2) Uani 1 1 d . . . . .
H6 H 0.5723 0.5061 0.6332 0.115 Uiso 1 1 calc R U . . .
C7 C 0.4625(5) 0.5494(5) 0.5874(2) 0.097(2) Uani 1 1 d . . . . .
H7 H 0.4925 0.5988 0.5767 0.116 Uiso 1 1 calc R U . . .
C8 C 0.3684(4) 0.5331(3) 0.5686(2) 0.0693(14) Uani 1 1 d . . . . .
H8 H 0.3353 0.5720 0.5463 0.083 Uiso 1 1 calc R U . . .
N9 N 0.1873(2) 0.48737(18) 0.52184(14) 0.0445(8) Uani 1 1 d . . . . .
N10 N 0.1042(2) 0.44965(18) 0.50205(12) 0.0379(7) Uani 1 1 d . . . . .
C11 C 0.0498(3) 0.4837(2) 0.46292(17) 0.0395(8) Uani 1 1 d . . . . .
C12 C -0.0307(3) 0.4303(2) 0.44431(16) 0.0402(8) Uani 1 1 d . . . . .
C13 C -0.1046(3) 0.4552(3) 0.40788(19) 0.0552(10) Uani 1 1 d . . . . .
H13 H -0.1064 0.5092 0.3936 0.066 Uiso 1 1 calc R U . . .
C14 C -0.1760(3) 0.3988(3) 0.3929(2) 0.0595(11) Uani 1 1 d . . . . .
H14 H -0.2264 0.4146 0.3686 0.071 Uiso 1 1 calc R U . . .
C15 C -0.1715(3) 0.3194(3) 0.41450(19) 0.0558(11) Uani 1 1 d . . . . .
H15 H -0.2180 0.2803 0.4043 0.067 Uiso 1 1 calc R U . . .
C16 C -0.0974(3) 0.2984(2) 0.45134(17) 0.0467(9) Uani 1 1 d . . . . .
H16 H -0.0953 0.2449 0.4665 0.056 Uiso 1 1 calc R U . . .
N17 N -0.0284(2) 0.35170(17) 0.46624(13) 0.0383(7) Uani 1 1 d . . . . .
C18 C 0.0623(3) 0.5685(2) 0.43886(17) 0.0441(9) Uani 1 1 d . . . . .
C19 C 0.0670(3) 0.5806(2) 0.37895(18) 0.0489(10) Uani 1 1 d . . . . .
H19 H 0.0645 0.5354 0.3538 0.059 Uiso 1 1 calc R U . . .
C20 C 0.0755(3) 0.6605(3) 0.3569(2) 0.0596(11) Uani 1 1 d . . . . .
H20 H 0.0799 0.6686 0.3169 0.072 Uiso 1 1 calc R U . . .
C21 C 0.0775(3) 0.7279(3) 0.3940(2) 0.0651(13) Uani 1 1 d . . . . .
H21 H 0.0814 0.7814 0.3790 0.078 Uiso 1 1 calc R U . . .
C22 C 0.0735(4) 0.7157(3) 0.4527(2) 0.0684(13) Uani 1 1 d . . . . .
H22 H 0.0753 0.7612 0.4776 0.082 Uiso 1 1 calc R U . . .
C23 C 0.0668(3) 0.6364(2) 0.47582(19) 0.0544(11) Uani 1 1 d . . . . .
H23 H 0.0653 0.6288 0.5160 0.065 Uiso 1 1 calc R U . . .
O25 O 0.17308(18) 0.29898(14) 0.46489(11) 0.0414(6) Uani 1 1 d . . . . .
C26 C 0.1893(2) 0.2198(2) 0.46059(16) 0.0378(8) Uani 1 1 d . . . . .
C27 C 0.2580(3) 0.1834(3) 0.42352(19) 0.0524(10) Uani 1 1 d . . . . .
H27 H 0.2946 0.2163 0.3986 0.063 Uiso 1 1 calc R U . . .
C28 C 0.2705(4) 0.0994(3) 0.4244(2) 0.0648(13) Uani 1 1 d . . . . .
H28 H 0.3158 0.0748 0.4000 0.078 Uiso 1 1 calc R U . . .
C29 C 0.2161(3) 0.0507(3) 0.4615(2) 0.0603(11) Uani 1 1 d D . . . .
C30 C 0.1475(3) 0.0826(2) 0.49892(19) 0.0506(10) Uani 1 1 d . . . . .
H30 H 0.1109 0.0483 0.5229 0.061 Uiso 1 1 calc R U . . .
C31 C 0.1354(2) 0.1691(2) 0.49924(16) 0.0367(8) Uani 1 1 d . . . . .
N32 N 0.0769(2) 0.21341(17) 0.53510(13) 0.0390(7) Uani 1 1 d . . . . .
H32 H 0.0403 0.1875 0.5593 0.047 Uiso 1 1 calc R U . . .
N33 N 0.222(2) -0.0407(6) 0.4560(14) 0.089(6) Uani 0.531(18) 1 d D U P A 1
O34 O 0.2715(15) -0.0700(10) 0.4172(9) 0.130(5) Uani 0.531(18) 1 d D U P A 1
O35 O 0.184(4) -0.081(2) 0.495(3) 0.112(6) Uani 0.531(18) 1 d D U P A 1
N33' N 0.239(2) -0.0385(7) 0.4678(17) 0.089(6) Uani 0.469(18) 1 d D U P A 2
O34' O 0.3151(16) -0.0616(11) 0.4456(10) 0.130(5) Uani 0.469(18) 1 d D U P A 2
O35' O 0.177(5) -0.084(3) 0.488(3) 0.112(6) Uani 0.469(18) 1 d D U P A 2
O36 O -0.0032(2) 0.34231(18) 0.58379(11) 0.0507(7) Uani 1 1 d . . . . .
O40 O 0.47671(18) 0.36185(15) 0.34838(11) 0.0410(6) Uani 1 1 d . . . . .
C41 C 0.5585(3) 0.3785(2) 0.32321(16) 0.0392(8) Uani 1 1 d . . . . .
C42 C 0.6072(3) 0.3118(2) 0.29119(16) 0.0431(9) Uani 1 1 d . . . . .
C43 C 0.5726(4) 0.2325(3) 0.29244(19) 0.0640(12) Uani 1 1 d . . . . .
H43 H 0.5179 0.2204 0.3143 0.077 Uiso 1 1 calc R U . . .
C44 C 0.6178(4) 0.1701(3) 0.2617(2) 0.0800(16) Uani 1 1 d . . . . .
H44 H 0.5931 0.1164 0.2629 0.096 Uiso 1 1 calc R U . . .
C45 C 0.6984(4) 0.1865(3) 0.2296(2) 0.0777(16) Uani 1 1 d . . . . .
H45 H 0.7289 0.1442 0.2091 0.093 Uiso 1 1 calc R U . . .
C46 C 0.7339(4) 0.2652(4) 0.2278(3) 0.093(2) Uani 1 1 d . . . . .
H46 H 0.7888 0.2767 0.2060 0.112 Uiso 1 1 calc R U . . .
C47 C 0.6888(3) 0.3283(3) 0.2583(2) 0.0756(15) Uani 1 1 d . . . . .
H47 H 0.7134 0.3819 0.2567 0.091 Uiso 1 1 calc R U . . .
N48 N 0.5994(2) 0.45216(19) 0.32431(13) 0.0437(7) Uani 1 1 d . . . . .
N49 N 0.5376(2) 0.50506(18) 0.35301(13) 0.0377(7) Uani 1 1 d . . . . .
C51 C 0.4794(3) 0.6307(2) 0.38569(19) 0.0450(9) Uani 1 1 d . . . . .
C52 C 0.4819(3) 0.7157(3) 0.3935(2) 0.0654(13) Uani 1 1 d . . . . .
H52 H 0.5346 0.7465 0.3808 0.078 Uiso 1 1 calc R U . . .
C53 C 0.4053(4) 0.7542(3) 0.4203(2) 0.0735(14) Uani 1 1 d . . . . .
H53 H 0.4060 0.8113 0.4261 0.088 Uiso 1 1 calc R U . . .
C54 C 0.3286(4) 0.7083(3) 0.4383(2) 0.0678(14) Uani 1 1 d . . . . .
H54 H 0.2765 0.7337 0.4566 0.081 Uiso 1 1 calc R U . . .
C55 C 0.3287(3) 0.6231(3) 0.42911(19) 0.0533(11) Uani 1 1 d . . . . .
H55 H 0.2759 0.5920 0.4413 0.064 Uiso 1 1 calc R U . . .
N56 N 0.4025(2) 0.58473(18) 0.40329(13) 0.0416(7) Uani 1 1 d . . . . .
C50 C 0.5573(3) 0.5832(2) 0.35692(17) 0.0452(9) Uani 0.774(8) 1 d D . P B 1
C57 C 0.6494(3) 0.6198(3) 0.3361(3) 0.0613(15) Uani 0.774(8) 1 d DG U P B 1
C58 C 0.6736(5) 0.6175(5) 0.2774(2) 0.108(3) Uani 0.774(8) 1 d G U P B 1
H58 H 0.6316 0.5935 0.2506 0.130 Uiso 0.774(8) 1 calc R U P B 1
C59 C 0.7606(5) 0.6511(6) 0.2586(3) 0.148(5) Uani 0.774(8) 1 d G U P B 1
H59 H 0.7768 0.6496 0.2193 0.178 Uiso 0.774(8) 1 calc R U P B 1
C60 C 0.8234(4) 0.6870(4) 0.2985(4) 0.153(5) Uani 0.774(8) 1 d G U P B 1
H60 H 0.8816 0.7094 0.2859 0.184 Uiso 0.774(8) 1 calc R U P B 1
C61 C 0.7992(4) 0.6892(4) 0.3572(3) 0.120(4) Uani 0.774(8) 1 d G U P B 1
H61 H 0.8412 0.7132 0.3840 0.144 Uiso 0.774(8) 1 calc R U P B 1
C62 C 0.7122(4) 0.6556(4) 0.3760(2) 0.090(3) Uani 0.774(8) 1 d G U P B 1
H62 H 0.6960 0.6572 0.4153 0.108 Uiso 0.774(8) 1 calc R U P B 1
C50' C 0.5573(3) 0.5832(2) 0.35692(17) 0.0452(9) Uani 0.226(8) 1 d . U P B 2
C57' C 0.6386(13) 0.6284(8) 0.3323(8) 0.0613(15) Uani 0.226(8) 1 d DG U P B 2
C58' C 0.6307(14) 0.6786(15) 0.2833(9) 0.108(3) Uani 0.226(8) 1 d G U P B 2
H58' H 0.5714 0.6846 0.2648 0.130 Uiso 0.226(8) 1 calc R U P B 2
C59' C 0.7114(18) 0.7198(17) 0.2620(10) 0.148(5) Uani 0.226(8) 1 d G U P B 2
H59' H 0.7061 0.7534 0.2292 0.178 Uiso 0.226(8) 1 calc R U P B 2
C60' C 0.8000(14) 0.7109(14) 0.2897(13) 0.153(5) Uani 0.226(8) 1 d G U P B 2
H60' H 0.8540 0.7385 0.2754 0.184 Uiso 0.226(8) 1 calc R U P B 2
C61' C 0.8079(13) 0.6607(16) 0.3387(13) 0.120(4) Uani 0.226(8) 1 d G U P B 2
H61' H 0.8671 0.6547 0.3572 0.144 Uiso 0.226(8) 1 calc R U P B 2
C62' C 0.7272(16) 0.6194(12) 0.3600(10) 0.090(3) Uani 0.226(8) 1 d G U P B 2
H62' H 0.7324 0.5858 0.3928 0.108 Uiso 0.226(8) 1 calc R U P B 2
O63 O 0.35448(19) 0.48877(16) 0.30558(11) 0.0465(6) Uani 1 1 d . . . . .
C64 C 0.2717(3) 0.4563(2) 0.29453(16) 0.0417(8) Uani 1 1 d . . . . .
C65 C 0.2211(4) 0.4644(3) 0.2421(2) 0.0700(14) Uani 1 1 d . . . . .
H65 H 0.2466 0.4961 0.2119 0.084 Uiso 1 1 calc R U . . .
C66 C 0.1332(4) 0.4250(4) 0.2351(2) 0.0748(15) Uani 1 1 d . . . . .
H66 H 0.0993 0.4304 0.2004 0.090 Uiso 1 1 calc R U . . .
C67 C 0.0958(3) 0.3773(3) 0.28035(18) 0.0513(10) Uani 1 1 d . . . . .
C68 C 0.1417(3) 0.3681(2) 0.33272(16) 0.0407(9) Uani 1 1 d . . . . .
H68 H 0.1152 0.3358 0.3622 0.049 Uiso 1 1 calc R U . . .
C69 C 0.2295(3) 0.4086(2) 0.34032(14) 0.0331(7) Uani 1 1 d . . . . .
N70 N 0.2843(2) 0.40901(16) 0.38900(12) 0.0327(6) Uani 1 1 d . . . . .
H70 H 0.2619 0.3883 0.4208 0.039 Uiso 1 1 calc R U . . .
N71 N 0.0054(3) 0.3339(3) 0.2697(2) 0.0709(11) Uani 1 1 d . . . . .
O72 O -0.0221(3) 0.2846(3) 0.3060(2) 0.1005(13) Uani 1 1 d . . . . .
O73 O -0.0379(3) 0.3471(4) 0.2249(2) 0.129(2) Uani 1 1 d . . . . .
O74 O 0.43478(18) 0.43206(16) 0.45349(10) 0.0447(6) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O1 C2 1.287(4) . ?
O1 V1 1.980(3) . ?
V1 O36 1.593(3) . ?
V1 N32 1.895(3) . ?
V1 N10 2.083(3) . ?
V1 N17 2.114(3) . ?
V1 O25 2.144(3) . ?
C2 N9 1.318(5) . ?
C2 C3 1.489(5) . ?
V2 O74 1.596(2) . ?
V2 N70 1.903(3) . ?
V2 O40 1.977(2) . ?
V2 N49 2.091(3) . ?
V2 O63 2.106(3) . ?
V2 N56 2.122(3) . ?
C3 C4 1.377(6) . ?
C3 C8 1.382(6) . ?
C4 C5 1.397(7) . ?
C4 H4 0.9300 . ?
C5 C6 1.348(10) . ?
C5 H5 0.9300 . ?
C6 C7 1.343(9) . ?
C6 H6 0.9300 . ?
C7 C8 1.399(7) . ?
C7 H7 0.9300 . ?
C8 H8 0.9300 . ?
N9 N10 1.380(4) . ?
N10 C11 1.295(5) . ?
C11 C12 1.472(5) . ?
C11 C18 1.483(5) . ?
C12 N17 1.363(5) . ?
C12 C13 1.382(5) . ?
C13 C14 1.387(6) . ?
C13 H13 0.9300 . ?
C14 C15 1.374(6) . ?
C14 H14 0.9300 . ?
C15 C16 1.373(6) . ?
C15 H15 0.9300 . ?
C16 N17 1.330(5) . ?
C16 H16 0.9300 . ?
C18 C23 1.387(6) . ?
C18 C19 1.391(6) . ?
C19 C20 1.388(5) . ?
C19 H19 0.9300 . ?
C20 C21 1.381(7) . ?
C20 H20 0.9300 . ?
C21 C22 1.364(7) . ?
C21 H21 0.9300 . ?
C22 C23 1.387(6) . ?
C22 H22 0.9300 . ?
C23 H23 0.9300 . ?
O25 C26 1.299(4) . ?
C26 C27 1.405(5) . ?
C26 C31 1.419(5) . ?
C27 C28 1.366(6) . ?
C27 H27 0.9300 . ?
C28 C29 1.383(7) . ?
C28 H28 0.9300 . ?
C29 C30 1.380(6) . ?
C29 N33' 1.480(11) . ?
C29 N33 1.480(10) . ?
C30 C31 1.404(5) . ?
C30 H30 0.9300 . ?
C31 N32 1.359(5) . ?
N32 H32 0.8600 . ?
N33 O34 1.224(13) . ?
N33 O35 1.224(15) . ?
N33' O35' 1.224(16) . ?
N33' O34' 1.224(13) . ?
O40 C41 1.300(4) . ?
C41 N48 1.316(5) . ?
C41 C42 1.467(5) . ?
C42 C43 1.366(6) . ?
C42 C47 1.386(6) . ?
C43 C44 1.378(6) . ?
C43 H43 0.9300 . ?
C44 C45 1.365(7) . ?
C44 H44 0.9300 . ?
C45 C46 1.361(8) . ?
C45 H45 0.9300 . ?
C46 C47 1.382(7) . ?
C46 H46 0.9300 . ?
C47 H47 0.9300 . ?
N48 N49 1.376(4) . ?
N49 C50 1.292(5) . ?
C51 N56 1.359(5) . ?
C51 C52 1.382(5) . ?
C51 C50 1.480(5) . ?
C52 C53 1.374(7) . ?
C52 H52 0.9300 . ?
C53 C54 1.360(7) . ?
C53 H53 0.9300 . ?
C54 C55 1.389(6) . ?
C54 H54 0.9300 . ?
C55 N56 1.334(5) . ?
C55 H55 0.9300 . ?
C50 C57 1.485(5) . ?
C57 C58 1.3900 . ?
C57 C62 1.3900 . ?
C58 C59 1.3900 . ?
C58 H58 0.9300 . ?
C59 C60 1.3900 . ?
C59 H59 0.9300 . ?
C60 C61 1.3900 . ?
C60 H60 0.9300 . ?
C61 C62 1.3900 . ?
C61 H61 0.9300 . ?
C62 H62 0.9300 . ?
C57' C58' 1.3900 . ?
C57' C62' 1.3900 . ?
C58' C59' 1.3900 . ?
C58' H58' 0.9300 . ?
C59' C60' 1.3900 . ?
C59' H59' 0.9300 . ?
C60' C61' 1.3900 . ?
C60' H60' 0.9300 . ?
C61' C62' 1.3900 . ?
C61' H61' 0.9300 . ?
C62' H62' 0.9300 . ?
O63 C64 1.286(4) . ?
C64 C65 1.400(5) . ?
C64 C69 1.427(5) . ?
C65 C66 1.382(6) . ?
C65 H65 0.9300 . ?
C66 C67 1.392(6) . ?
C66 H66 0.9300 . ?
C67 C68 1.369(5) . ?
C67 N71 1.455(6) . ?
C68 C69 1.392(5) . ?
C68 H68 0.9300 . ?
C69 N70 1.351(4) . ?
N70 H70 0.8600 . ?
N71 O73 1.210(5) . ?
N71 O72 1.213(6) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 O1 V1 116.2(2) . . ?
O36 V1 N32 96.36(14) . . ?
O36 V1 O1 100.09(13) . . ?
N32 V1 O1 104.65(12) . . ?
O36 V1 N10 106.20(13) . . ?
N32 V1 N10 157.24(13) . . ?
O1 V1 N10 74.66(11) . . ?
O36 V1 N17 93.60(13) . . ?
N32 V1 N17 101.03(12) . . ?
O1 V1 N17 149.20(11) . . ?
N10 V1 N17 75.06(11) . . ?
O36 V1 O25 172.63(13) . . ?
N32 V1 O25 76.40(11) . . ?
O1 V1 O25 83.32(11) . . ?
N10 V1 O25 80.96(10) . . ?
N17 V1 O25 86.51(11) . . ?
O1 C2 N9 124.0(3) . . ?
O1 C2 C3 117.5(4) . . ?
N9 C2 C3 118.4(3) . . ?
O74 V2 N70 94.84(13) . . ?
O74 V2 O40 98.98(12) . . ?
N70 V2 O40 97.88(11) . . ?
O74 V2 N49 105.81(13) . . ?
N70 V2 N49 158.76(12) . . ?
O40 V2 N49 74.36(11) . . ?
O74 V2 O63 170.20(12) . . ?
N70 V2 O63 77.11(11) . . ?
O40 V2 O63 87.78(11) . . ?
N49 V2 O63 82.78(11) . . ?
O74 V2 N56 94.50(13) . . ?
N70 V2 N56 109.43(12) . . ?
O40 V2 N56 148.32(12) . . ?
N49 V2 N56 74.42(12) . . ?
O63 V2 N56 83.13(11) . . ?
C4 C3 C8 118.8(4) . . ?
C4 C3 C2 120.2(4) . . ?
C8 C3 C2 120.9(4) . . ?
C3 C4 C5 119.9(6) . . ?
C3 C4 H4 120.1 . . ?
C5 C4 H4 120.1 . . ?
C6 C5 C4 120.5(6) . . ?
C6 C5 H5 119.7 . . ?
C4 C5 H5 119.7 . . ?
C7 C6 C5 120.5(6) . . ?
C7 C6 H6 119.7 . . ?
C5 C6 H6 119.7 . . ?
C6 C7 C8 120.5(6) . . ?
C6 C7 H7 119.7 . . ?
C8 C7 H7 119.7 . . ?
C3 C8 C7 119.7(6) . . ?
C3 C8 H8 120.1 . . ?
C7 C8 H8 120.1 . . ?
C2 N9 N10 107.5(3) . . ?
C11 N10 N9 121.9(3) . . ?
C11 N10 V1 120.6(2) . . ?
N9 N10 V1 117.4(2) . . ?
N10 C11 C12 113.2(3) . . ?
N10 C11 C18 125.5(3) . . ?
C12 C11 C18 121.3(3) . . ?
N17 C12 C13 120.7(4) . . ?
N17 C12 C11 114.8(3) . . ?
C13 C12 C11 124.5(3) . . ?
C12 C13 C14 119.2(4) . . ?
C12 C13 H13 120.4 . . ?
C14 C13 H13 120.4 . . ?
C15 C14 C13 119.3(4) . . ?
C15 C14 H14 120.4 . . ?
C13 C14 H14 120.4 . . ?
C16 C15 C14 119.0(4) . . ?
C16 C15 H15 120.5 . . ?
C14 C15 H15 120.5 . . ?
N17 C16 C15 122.6(4) . . ?
N17 C16 H16 118.7 . . ?
C15 C16 H16 118.7 . . ?
C16 N17 C12 119.2(3) . . ?
C16 N17 V1 124.5(3) . . ?
C12 N17 V1 115.5(2) . . ?
C23 C18 C19 119.5(3) . . ?
C23 C18 C11 120.3(3) . . ?
C19 C18 C11 120.2(3) . . ?
C20 C19 C18 119.6(4) . . ?
C20 C19 H19 120.2 . . ?
C18 C19 H19 120.2 . . ?
C21 C20 C19 120.4(4) . . ?
C21 C20 H20 119.8 . . ?
C19 C20 H20 119.8 . . ?
C22 C21 C20 119.7(4) . . ?
C22 C21 H21 120.1 . . ?
C20 C21 H21 120.1 . . ?
C21 C22 C23 120.9(4) . . ?
C21 C22 H22 119.6 . . ?
C23 C22 H22 119.6 . . ?
C18 C23 C22 119.8(4) . . ?
C18 C23 H23 120.1 . . ?
C22 C23 H23 120.1 . . ?
C26 O25 V1 113.7(2) . . ?
O25 C26 C27 125.0(3) . . ?
O25 C26 C31 115.2(3) . . ?
C27 C26 C31 119.7(3) . . ?
C28 C27 C26 119.4(4) . . ?
C28 C27 H27 120.3 . . ?
C26 C27 H27 120.3 . . ?
C27 C28 C29 120.2(4) . . ?
C27 C28 H28 119.9 . . ?
C29 C28 H28 119.9 . . ?
C30 C29 C28 123.2(4) . . ?
C30 C29 N33' 116.9(10) . . ?
C28 C29 N33' 119.5(10) . . ?
C30 C29 N33 117.4(9) . . ?
C28 C29 N33 119.0(9) . . ?
C29 C30 C31 117.1(4) . . ?
C29 C30 H30 121.4 . . ?
C31 C30 H30 121.4 . . ?
N32 C31 C30 126.6(3) . . ?
N32 C31 C26 113.0(3) . . ?
C30 C31 C26 120.4(4) . . ?
C31 N32 V1 121.5(2) . . ?
C31 N32 H32 119.3 . . ?
V1 N32 H32 119.3 . . ?
O34 N33 O35 125.0(17) . . ?
O34 N33 C29 118.4(15) . . ?
O35 N33 C29 116(2) . . ?
O35' N33' O34' 125.3(19) . . ?
O35' N33' C29 118(2) . . ?
O34' N33' C29 116.2(16) . . ?
C41 O40 V2 116.7(2) . . ?
O40 C41 N48 123.6(3) . . ?
O40 C41 C42 118.2(3) . . ?
N48 C41 C42 118.2(3) . . ?
C43 C42 C47 118.5(4) . . ?
C43 C42 C41 120.9(4) . . ?
C47 C42 C41 120.6(4) . . ?
C42 C43 C44 120.9(5) . . ?
C42 C43 H43 119.6 . . ?
C44 C43 H43 119.6 . . ?
C45 C44 C43 120.4(5) . . ?
C45 C44 H44 119.8 . . ?
C43 C44 H44 119.8 . . ?
C46 C45 C44 119.5(5) . . ?
C46 C45 H45 120.2 . . ?
C44 C45 H45 120.2 . . ?
C45 C46 C47 120.4(5) . . ?
C45 C46 H46 119.8 . . ?
C47 C46 H46 119.8 . . ?
C46 C47 C42 120.3(5) . . ?
C46 C47 H47 119.9 . . ?
C42 C47 H47 119.9 . . ?
C41 N48 N49 107.5(3) . . ?
C50 N49 N48 120.4(3) . . ?
C50 N49 V2 121.8(3) . . ?
N48 N49 V2 117.8(2) . . ?
N56 C51 C52 121.4(4) . . ?
N56 C51 C50 115.0(3) . . ?
C52 C51 C50 123.5(4) . . ?
C53 C52 C51 119.1(4) . . ?
C53 C52 H52 120.5 . . ?
C51 C52 H52 120.5 . . ?
C54 C53 C52 119.6(4) . . ?
C54 C53 H53 120.2 . . ?
C52 C53 H53 120.2 . . ?
C53 C54 C55 119.4(4) . . ?
C53 C54 H54 120.3 . . ?
C55 C54 H54 120.3 . . ?
N56 C55 C54 121.8(4) . . ?
N56 C55 H55 119.1 . . ?
C54 C55 H55 119.1 . . ?
C55 N56 C51 118.7(3) . . ?
C55 N56 V2 124.9(3) . . ?
C51 N56 V2 116.3(2) . . ?
N49 C50 C51 112.4(3) . . ?
N49 C50 C57 123.1(4) . . ?
C51 C50 C57 124.5(4) . . ?
C58 C57 C62 120.0 . . ?
C58 C57 C50 120.6(4) . . ?
C62 C57 C50 119.4(4) . . ?
C57 C58 C59 120.0 . . ?
C57 C58 H58 120.0 . . ?
C59 C58 H58 120.0 . . ?
C58 C59 C60 120.0 . . ?
C58 C59 H59 120.0 . . ?
C60 C59 H59 120.0 . . ?
C61 C60 C59 120.0 . . ?
C61 C60 H60 120.0 . . ?
C59 C60 H60 120.0 . . ?
C60 C61 C62 120.0 . . ?
C60 C61 H61 120.0 . . ?
C62 C61 H61 120.0 . . ?
C61 C62 C57 120.0 . . ?
C61 C62 H62 120.0 . . ?
C57 C62 H62 120.0 . . ?
C58' C57' C62' 120.0 . . ?
C59' C58' C57' 120.0 . . ?
C59' C58' H58' 120.0 . . ?
C57' C58' H58' 120.0 . . ?
C60' C59' C58' 120.0 . . ?
C60' C59' H59' 120.0 . . ?
C58' C59' H59' 120.0 . . ?
C59' C60' C61' 120.0 . . ?
C59' C60' H60' 120.0 . . ?
C61' C60' H60' 120.0 . . ?
C60' C61' C62' 120.0 . . ?
C60' C61' H61' 120.0 . . ?
C62' C61' H61' 120.0 . . ?
C61' C62' C57' 120.0 . . ?
C61' C62' H62' 120.0 . . ?
C57' C62' H62' 120.0 . . ?
C64 O63 V2 113.7(2) . . ?
O63 C64 C65 125.4(4) . . ?
O63 C64 C69 116.0(3) . . ?
C65 C64 C69 118.6(4) . . ?
C66 C65 C64 119.8(4) . . ?
C66 C65 H65 120.1 . . ?
C64 C65 H65 120.1 . . ?
C65 C66 C67 119.8(4) . . ?
C65 C66 H66 120.1 . . ?
C67 C66 H66 120.1 . . ?
C68 C67 C66 122.8(4) . . ?
C68 C67 N71 119.7(4) . . ?
C66 C67 N71 117.5(4) . . ?
C67 C68 C69 117.8(4) . . ?
C67 C68 H68 121.1 . . ?
C69 C68 H68 121.1 . . ?
N70 C69 C68 126.6(3) . . ?
N70 C69 C64 112.2(3) . . ?
C68 C69 C64 121.2(3) . . ?
C69 N70 V2 120.2(2) . . ?
C69 N70 H70 119.9 . . ?
V2 N70 H70 119.9 . . ?
O73 N71 O72 123.0(4) . . ?
O73 N71 C67 119.0(5) . . ?
O72 N71 C67 118.0(4) . . ?

_refine_diff_density_max         0.229
_refine_diff_density_min         -0.239
_refine_diff_density_rms         0.046

_shelxl_version_number           2013-2



####################################################################### 
# 
# 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_1
_database_code_depnum_ccdc_archive 'CCDC 1508431'
_audit_update_record             
;
2016-10-05 deposited with the CCDC.
2016-10-19 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C32 H33 N2 O5 V'
_chemical_formula_weight         576.54

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'

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

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

_cell_length_a                   11.1788(5)
_cell_length_b                   18.3320(9)
_cell_length_c                   17.6872(8)
_cell_angle_alpha                90
_cell_angle_beta                 107.635(2)
_cell_angle_gamma                90
_cell_volume                     3454.3(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    9889
_cell_measurement_theta_min      2.53
_cell_measurement_theta_max      28.32

_exptl_crystal_description       prism
_exptl_crystal_colour            black
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.109
_exptl_crystal_F_000             1208
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.89
_exptl_crystal_size_mid          0.54
_exptl_crystal_size_min          0.42
_exptl_absorpt_coefficient_mu    0.323
_shelx_estimated_absorpt_T_min   0.897
_shelx_estimated_absorpt_T_max   0.952
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.872
_exptl_absorpt_correction_T_max  0.982
_exptl_absorpt_process_details   'APEX2 (Bruker AXS Inc. 2007)'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   Mo
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            49527
_diffrn_reflns_av_unetI/netI     0.0237
_diffrn_reflns_av_R_equivalents  0.0351
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         2.816
_diffrn_reflns_theta_max         27.499
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measured_fraction_theta_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_point_group_measured_fraction_full 0.993
_reflns_number_total             7878
_reflns_number_gt                6245
_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.
 
 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 APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 w=1/[σ²(Fo²)+(0.0906P)²+4.3557P]
 where P=(Fo²+2Fc²)/3
;
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         7878
_refine_ls_number_parameters     423
_refine_ls_number_restraints     431
_refine_ls_R_factor_all          0.0825
_refine_ls_R_factor_gt           0.0637
_refine_ls_wR_factor_ref         0.1984
_refine_ls_wR_factor_gt          0.1727
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_restrained_S_all      1.029
_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 0.27870(4) 0.62213(2) 0.46296(3) 0.04034(16) Uani 1 1 d . . . . .
O50 O 0.2122(2) 0.67198(13) 0.38921(13) 0.0636(6) Uani 1 1 d . . . . .
O1 O 0.45445(19) 0.65375(10) 0.48413(12) 0.0462(4) Uani 1 1 d . . . . .
C2 C 0.5254(2) 0.61638(12) 0.45369(14) 0.0344(5) Uani 1 1 d . . . . .
C3 C 0.6553(3) 0.64089(14) 0.46443(17) 0.0429(6) Uani 1 1 d . . . . .
C4 C 0.7134(3) 0.68615(19) 0.5274(2) 0.0602(8) Uani 1 1 d . . . . .
H4 H 0.6710 0.7008 0.5627 0.072 Uiso 1 1 calc R U . . .
C5 C 0.8358(4) 0.7097(2) 0.5378(3) 0.0831(12) Uani 1 1 d . . . . .
H5 H 0.8757 0.7394 0.5807 0.100 Uiso 1 1 calc R U . . .
C6 C 0.8976(4) 0.6894(2) 0.4852(3) 0.0859(13) Uani 1 1 d . . . . .
H6 H 0.9790 0.7059 0.4923 0.103 Uiso 1 1 calc R U . . .
C7 C 0.8412(4) 0.6454(2) 0.4225(3) 0.0791(12) Uani 1 1 d . . . . .
H7 H 0.8839 0.6318 0.3870 0.095 Uiso 1 1 calc R U . . .
C8 C 0.7199(3) 0.62103(17) 0.4119(2) 0.0577(8) Uani 1 1 d . . . . .
H8 H 0.6814 0.5910 0.3690 0.069 Uiso 1 1 calc R U . . .
N9 N 0.48492(19) 0.55665(11) 0.41330(12) 0.0361(4) Uani 1 1 d . . . . .
N10 N 0.35879(18) 0.54515(11) 0.40736(11) 0.0327(4) Uani 1 1 d . . . . .
C11 C 0.3047(2) 0.49041(14) 0.36445(15) 0.0384(5) Uani 1 1 d . . . . .
H11 H 0.3523 0.4629 0.3399 0.046 Uiso 1 1 calc R U . . .
C12 C 0.1777(2) 0.46904(15) 0.35199(15) 0.0413(6) Uani 1 1 d D . . . .
C15 C -0.0671(3) 0.4220(2) 0.3357(2) 0.0585(8) Uani 1 1 d D . . . .
H15 H -0.1508 0.4094 0.3272 0.070 Uiso 1 1 calc R U . A 1
C16 C -0.0155(3) 0.4740(2) 0.38952(18) 0.0539(7) Uani 1 1 d . . . . .
H16 H -0.0607 0.4931 0.4212 0.065 Uiso 1 1 calc R U . . .
C17 C 0.1077(2) 0.49963(15) 0.39803(15) 0.0408(6) Uani 1 1 d . . . . .
O18 O 0.15524(18) 0.54994(12) 0.45194(11) 0.0499(5) Uani 1 1 d . . . . .
C14X C 0.0029(7) 0.3854(5) 0.2911(5) 0.0494(19) Uani 0.661(14) 1 d D U P B 1
C13X C 0.1271(8) 0.4081(5) 0.2999(5) 0.047(2) Uani 0.661(14) 1 d D U P B 1
C19X C 0.1965(7) 0.3696(4) 0.2574(5) 0.065(2) Uani 0.661(14) 1 d D U P B 1
H19X H 0.2795 0.3825 0.2641 0.078 Uiso 0.661(14) 1 calc R U P B 1
C20X C 0.1431(9) 0.3138(5) 0.2068(6) 0.088(3) Uani 0.661(14) 1 d D U P B 1
H20X H 0.1902 0.2890 0.1798 0.106 Uiso 0.661(14) 1 calc R U P B 1
C21X C 0.0186(9) 0.2941(5) 0.1956(6) 0.092(3) Uani 0.661(14) 1 d D U P B 1
H21X H -0.0180 0.2573 0.1599 0.110 Uiso 0.661(14) 1 calc R U P B 1
C22X C -0.0494(8) 0.3286(5) 0.2370(6) 0.072(3) Uani 0.661(14) 1 d D U P B 1
H22X H -0.1321 0.3146 0.2296 0.087 Uiso 0.661(14) 1 calc R U P B 1
C14Y C -0.0113(15) 0.3991(11) 0.2771(10) 0.0494(19) Uani 0.339(14) 1 d D U P B
2
C13Y C 0.1137(16) 0.4207(13) 0.2872(12) 0.047(2) Uani 0.339(14) 1 d D U P B 2
C19Y C 0.1684(14) 0.3917(9) 0.2306(10) 0.065(2) Uani 0.339(14) 1 d D U P B 2
H19Y H 0.2485 0.4065 0.2318 0.078 Uiso 0.339(14) 1 calc R U P B 2
C20Y C 0.1052(16) 0.3424(10) 0.1743(11) 0.088(3) Uani 0.339(14) 1 d D U P B 2
H20Y H 0.1439 0.3244 0.1384 0.106 Uiso 0.339(14) 1 calc R U P B 2
C21Y C -0.0151(16) 0.3187(11) 0.1693(12) 0.092(3) Uani 0.339(14) 1 d D U P B 2
H21Y H -0.0556 0.2844 0.1316 0.110 Uiso 0.339(14) 1 calc R U P B 2
C22Y C -0.0729(16) 0.3466(12) 0.2206(13) 0.072(3) Uani 0.339(14) 1 d D U P B 2
H22Y H -0.1530 0.3309 0.2183 0.087 Uiso 0.339(14) 1 calc R U P B 2
O25 O 0.36650(18) 0.55558(10) 0.57743(11) 0.0414(4) Uani 1 1 d . . . . .
H25 H 0.413(3) 0.5206(19) 0.583(2) 0.054 Uiso 1 1 d . U . . .
C26 C 0.3826(2) 0.59945(14) 0.64138(15) 0.0354(5) Uani 1 1 d . . . . .
C27 C 0.4367(2) 0.57825(15) 0.71959(15) 0.0399(5) Uani 1 1 d . . . . .
H27 H 0.4667 0.5310 0.7317 0.048 Uiso 1 1 calc R U . . .
C28 C 0.4452(3) 0.62897(16) 0.77983(15) 0.0460(6) Uani 1 1 d D . . . .
C29 C 0.4036(3) 0.70001(16) 0.75865(16) 0.0493(7) Uani 1 1 d . . . . .
H29 H 0.4141 0.7342 0.7990 0.059 Uiso 1 1 calc R U . . .
C30 C 0.3473(3) 0.72302(13) 0.68092(15) 0.0409(6) Uani 1 1 d D . . . .
C31 C 0.3324(2) 0.66939(13) 0.62186(14) 0.0359(5) Uani 1 1 d . . . . .
O32 O 0.26959(18) 0.68075(10) 0.54490(10) 0.0411(4) Uani 1 1 d . . . . .
C33X C 0.4900(9) 0.6073(6) 0.8676(3) 0.0598(11) Uani 0.462(3) 1 d D U P C 1
C34X C 0.5621(15) 0.5350(6) 0.8796(14) 0.093(3) Uani 0.462(3) 1 d D U P C 1
H34A H 0.6326 0.5394 0.8596 0.139 Uiso 0.462(3) 1 calc R U P C 1
H34B H 0.5076 0.4969 0.8516 0.139 Uiso 0.462(3) 1 calc R U P C 1
H34C H 0.5912 0.5235 0.9351 0.139 Uiso 0.462(3) 1 calc R U P C 1
C35X C 0.3756(9) 0.6002(7) 0.8977(6) 0.089(3) Uani 0.462(3) 1 d D U P C 1
H35A H 0.4027 0.5862 0.9526 0.134 Uiso 0.462(3) 1 calc R U P C 1
H35B H 0.3198 0.5637 0.8673 0.134 Uiso 0.462(3) 1 calc R U P C 1
H35C H 0.3326 0.6461 0.8921 0.134 Uiso 0.462(3) 1 calc R U P C 1
C36X C 0.5767(10) 0.6669(6) 0.9156(6) 0.086(3) Uani 0.462(3) 1 d D U P C 1
H36A H 0.6495 0.6712 0.8979 0.129 Uiso 0.462(3) 1 calc R U P C 1
H36B H 0.6021 0.6543 0.9709 0.129 Uiso 0.462(3) 1 calc R U P C 1
H36C H 0.5326 0.7126 0.9081 0.129 Uiso 0.462(3) 1 calc R U P C 1
C37X C 0.2975(11) 0.8012(2) 0.6584(4) 0.0456(14) Uani 0.74(3) 1 d D U P D 1
C38X C 0.3554(16) 0.8328(5) 0.5971(5) 0.073(2) Uani 0.74(3) 1 d D U P D 1
H38A H 0.4451 0.8336 0.6190 0.110 Uiso 0.74(3) 1 calc R U P D 1
H38B H 0.3250 0.8815 0.5836 0.110 Uiso 0.74(3) 1 calc R U P D 1
H38C H 0.3322 0.8029 0.5503 0.110 Uiso 0.74(3) 1 calc R U P D 1
C39X C 0.3346(14) 0.8512(7) 0.7316(5) 0.080(2) Uani 0.74(3) 1 d D U P D 1
H39A H 0.4243 0.8514 0.7542 0.121 Uiso 0.74(3) 1 calc R U P D 1
H39B H 0.2969 0.8336 0.7702 0.121 Uiso 0.74(3) 1 calc R U P D 1
H39C H 0.3058 0.8999 0.7162 0.121 Uiso 0.74(3) 1 calc R U P D 1
C40X C 0.1541(11) 0.8017(6) 0.6230(6) 0.085(2) Uani 0.74(3) 1 d D U P D 1
H40A H 0.1168 0.7819 0.6608 0.127 Uiso 0.74(3) 1 calc R U P D 1
H40B H 0.1302 0.7727 0.5756 0.127 Uiso 0.74(3) 1 calc R U P D 1
H40C H 0.1255 0.8509 0.6104 0.127 Uiso 0.74(3) 1 calc R U P D 1
C33Y C 0.5077(12) 0.6120(8) 0.8681(4) 0.0598(11) Uani 0.346(3) 1 d D U P C 2
C34Y C 0.535(2) 0.5303(7) 0.8800(19) 0.093(3) Uani 0.346(3) 1 d D U P C 2
H34D H 0.4579 0.5034 0.8610 0.139 Uiso 0.346(3) 1 calc R U P C 2
H34E H 0.5729 0.5204 0.9355 0.139 Uiso 0.346(3) 1 calc R U P C 2
H34F H 0.5912 0.5157 0.8512 0.139 Uiso 0.346(3) 1 calc R U P C 2
C35Y C 0.4175(13) 0.6345(9) 0.9144(8) 0.089(3) Uani 0.346(3) 1 d D U P C 2
H35D H 0.3406 0.6076 0.8950 0.134 Uiso 0.346(3) 1 calc R U P C 2
H35E H 0.4001 0.6858 0.9074 0.134 Uiso 0.346(3) 1 calc R U P C 2
H35F H 0.4554 0.6243 0.9697 0.134 Uiso 0.346(3) 1 calc R U P C 2
C36Y C 0.6304(12) 0.6548(9) 0.8999(9) 0.086(3) Uani 0.346(3) 1 d D U P C 2
H36D H 0.6134 0.7061 0.8928 0.129 Uiso 0.346(3) 1 calc R U P C 2
H36E H 0.6876 0.6407 0.8715 0.129 Uiso 0.346(3) 1 calc R U P C 2
H36F H 0.6672 0.6445 0.9553 0.129 Uiso 0.346(3) 1 calc R U P C 2
C37Y C 0.330(2) 0.8046(5) 0.6616(14) 0.0456(14) Uani 0.26(3) 1 d D U P D 2
C38Y C 0.406(3) 0.8240(15) 0.6061(18) 0.073(2) Uani 0.26(3) 1 d D U P D 2
H38D H 0.4940 0.8194 0.6340 0.110 Uiso 0.26(3) 1 calc R U P D 2
H38E H 0.3882 0.8733 0.5879 0.110 Uiso 0.26(3) 1 calc R U P D 2
H38F H 0.3844 0.7915 0.5614 0.110 Uiso 0.26(3) 1 calc R U P D 2
C39Y C 0.369(4) 0.854(2) 0.7345(16) 0.080(2) Uani 0.26(3) 1 d D U P D 2
H39D H 0.4577 0.8507 0.7591 0.121 Uiso 0.26(3) 1 calc R U P D 2
H39E H 0.3259 0.8396 0.7715 0.121 Uiso 0.26(3) 1 calc R U P D 2
H39F H 0.3469 0.9038 0.7185 0.121 Uiso 0.26(3) 1 calc R U P D 2
C40Y C 0.190(2) 0.8140(19) 0.618(2) 0.085(2) Uani 0.26(3) 1 d D U P D 2
H40D H 0.1421 0.8010 0.6533 0.127 Uiso 0.26(3) 1 calc R U P D 2
H40E H 0.1662 0.7830 0.5725 0.127 Uiso 0.26(3) 1 calc R U P D 2
H40F H 0.1732 0.8639 0.6023 0.127 Uiso 0.26(3) 1 calc R U P D 2
C33Z C 0.4944(15) 0.6009(8) 0.8657(5) 0.0598(11) Uani 0.192(3) 1 d D U P C 3
C34Z C 0.4055(18) 0.5410(10) 0.8771(11) 0.093(3) Uani 0.192(3) 1 d D U P C 3
H34G H 0.4007 0.5027 0.8393 0.139 Uiso 0.192(3) 1 calc R U P C 3
H34H H 0.3234 0.5612 0.8692 0.139 Uiso 0.192(3) 1 calc R U P C 3
H34I H 0.4367 0.5216 0.9298 0.139 Uiso 0.192(3) 1 calc R U P C 3
C35Z C 0.498(2) 0.6625(9) 0.9253(11) 0.089(3) Uani 0.192(3) 1 d D U P C 3
H35G H 0.5566 0.6993 0.9205 0.134 Uiso 0.192(3) 1 calc R U P C 3
H35H H 0.5240 0.6431 0.9782 0.134 Uiso 0.192(3) 1 calc R U P C 3
H35I H 0.4161 0.6837 0.9144 0.134 Uiso 0.192(3) 1 calc R U P C 3
C36Z C 0.6267(15) 0.5688(13) 0.8825(12) 0.086(3) Uani 0.192(3) 1 d D U P C 3
H36G H 0.6827 0.6058 0.8749 0.129 Uiso 0.192(3) 1 calc R U P C 3
H36H H 0.6245 0.5290 0.8470 0.129 Uiso 0.192(3) 1 calc R U P C 3
H36I H 0.6556 0.5517 0.9363 0.129 Uiso 0.192(3) 1 calc R U P C 3


_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 O50 1.582(2) . ?
V1 O32 1.8318(17) . ?
V1 O18 1.879(2) . ?
V1 O1 1.972(2) . ?
V1 N10 2.0721(19) . ?
V1 O25 2.3123(19) . ?
O1 C2 1.284(3) . ?
C2 N9 1.311(3) . ?
C2 C3 1.476(4) . ?
C3 C4 1.383(4) . ?
C3 C8 1.388(4) . ?
C4 C5 1.393(5) . ?
C4 H4 0.9300 . ?
C5 C6 1.368(7) . ?
C5 H5 0.9300 . ?
C6 C7 1.362(6) . ?
C6 H6 0.9300 . ?
C7 C8 1.386(5) . ?
C7 H7 0.9300 . ?
C8 H8 0.9300 . ?
N9 N10 1.398(3) . ?
N10 C11 1.292(3) . ?
C11 C12 1.425(4) . ?
C11 H11 0.9300 . ?
C12 C17 1.406(3) . ?
C12 C13X 1.449(5) . ?
C12 C13Y 1.454(7) . ?
C15 C16 1.347(5) . ?
C15 C14Y 1.425(7) . ?
C15 C14X 1.435(5) . ?
C15 H15 0.9300 . ?
C16 C17 1.419(4) . ?
C16 H16 0.9300 . ?
C17 O18 1.317(3) . ?
C14X C13X 1.412(5) . ?
C14X C22X 1.414(6) . ?
C13X C19X 1.421(6) . ?
C19X C20X 1.371(6) . ?
C19X H19X 0.9300 . ?
C20X C21X 1.392(7) . ?
C20X H20X 0.9300 . ?
C21X C22X 1.362(7) . ?
C21X H21X 0.9300 . ?
C22X H22X 0.9300 . ?
C14Y C22Y 1.408(8) . ?
C14Y C13Y 1.411(8) . ?
C13Y C19Y 1.424(8) . ?
C19Y C20Y 1.371(9) . ?
C19Y H19Y 0.9300 . ?
C20Y C21Y 1.391(10) . ?
C20Y H20Y 0.9300 . ?
C21Y C22Y 1.362(9) . ?
C21Y H21Y 0.9300 . ?
C22Y H22Y 0.9300 . ?
O25 C26 1.355(3) . ?
O25 H25 0.81(4) . ?
C26 C27 1.387(4) . ?
C26 C31 1.400(4) . ?
C27 C28 1.395(4) . ?
C27 H27 0.9300 . ?
C28 C29 1.395(4) . ?
C28 C33X 1.533(6) . ?
C28 C33Y 1.536(7) . ?
C28 C33Z 1.538(7) . ?
C29 C30 1.393(4) . ?
C29 H29 0.9300 . ?
C30 C31 1.407(3) . ?
C30 C37Y 1.533(8) . ?
C30 C37X 1.546(5) . ?
C31 O32 1.346(3) . ?
C33X C34X 1.531(6) . ?
C33X C35X 1.533(7) . ?
C33X C36X 1.535(7) . ?
C34X H34A 0.9600 . ?
C34X H34B 0.9600 . ?
C34X H34C 0.9600 . ?
C35X H35A 0.9600 . ?
C35X H35B 0.9600 . ?
C35X H35C 0.9600 . ?
C36X H36A 0.9600 . ?
C36X H36B 0.9600 . ?
C36X H36C 0.9600 . ?
C37X C40X 1.534(5) . ?
C37X C38X 1.535(5) . ?
C37X C39X 1.538(5) . ?
C38X H38A 0.9600 . ?
C38X H38B 0.9600 . ?
C38X H38C 0.9600 . ?
C39X H39A 0.9600 . ?
C39X H39B 0.9600 . ?
C39X H39C 0.9600 . ?
C40X H40A 0.9600 . ?
C40X H40B 0.9600 . ?
C40X H40C 0.9600 . ?
C33Y C36Y 1.531(7) . ?
C33Y C34Y 1.532(7) . ?
C33Y C35Y 1.537(7) . ?
C34Y H34D 0.9600 . ?
C34Y H34E 0.9600 . ?
C34Y H34F 0.9600 . ?
C35Y H35D 0.9600 . ?
C35Y H35E 0.9600 . ?
C35Y H35F 0.9600 . ?
C36Y H36D 0.9600 . ?
C36Y H36E 0.9600 . ?
C36Y H36F 0.9600 . ?
C37Y C40Y 1.528(7) . ?
C37Y C38Y 1.528(7) . ?
C37Y C39Y 1.530(7) . ?
C38Y H38D 0.9600 . ?
C38Y H38E 0.9600 . ?
C38Y H38F 0.9600 . ?
C39Y H39D 0.9600 . ?
C39Y H39E 0.9600 . ?
C39Y H39F 0.9600 . ?
C40Y H40D 0.9600 . ?
C40Y H40E 0.9600 . ?
C40Y H40F 0.9600 . ?
C33Z C36Z 1.535(7) . ?
C33Z C34Z 1.535(7) . ?
C33Z C35Z 1.537(7) . ?
C34Z H34G 0.9600 . ?
C34Z H34H 0.9600 . ?
C34Z H34I 0.9600 . ?
C35Z H35G 0.9600 . ?
C35Z H35H 0.9600 . ?
C35Z H35I 0.9600 . ?
C36Z H36G 0.9600 . ?
C36Z H36H 0.9600 . ?
C36Z H36I 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
O50 V1 O32 100.87(10) . . ?
O50 V1 O18 100.04(13) . . ?
O32 V1 O18 106.27(9) . . ?
O50 V1 O1 100.33(12) . . ?
O32 V1 O1 88.18(8) . . ?
O18 V1 O1 152.21(9) . . ?
O50 V1 N10 99.49(10) . . ?
O32 V1 N10 155.60(8) . . ?
O18 V1 N10 83.14(8) . . ?
O1 V1 N10 75.02(8) . . ?
O50 V1 O25 174.68(9) . . ?
O32 V1 O25 74.17(7) . . ?
O18 V1 O25 79.80(8) . . ?
O1 V1 O25 81.64(8) . . ?
N10 V1 O25 85.78(7) . . ?
C2 O1 V1 118.06(16) . . ?
O1 C2 N9 121.3(2) . . ?
O1 C2 C3 119.5(2) . . ?
N9 C2 C3 119.2(2) . . ?
C4 C3 C8 119.0(3) . . ?
C4 C3 C2 119.3(3) . . ?
C8 C3 C2 121.7(3) . . ?
C3 C4 C5 119.7(4) . . ?
C3 C4 H4 120.1 . . ?
C5 C4 H4 120.1 . . ?
C6 C5 C4 120.3(4) . . ?
C6 C5 H5 119.9 . . ?
C4 C5 H5 119.9 . . ?
C7 C6 C5 120.7(4) . . ?
C7 C6 H6 119.6 . . ?
C5 C6 H6 119.6 . . ?
C6 C7 C8 119.6(4) . . ?
C6 C7 H7 120.2 . . ?
C8 C7 H7 120.2 . . ?
C7 C8 C3 120.8(4) . . ?
C7 C8 H8 119.6 . . ?
C3 C8 H8 119.6 . . ?
C2 N9 N10 109.95(19) . . ?
C11 N10 N9 116.28(19) . . ?
C11 N10 V1 127.96(17) . . ?
N9 N10 V1 115.64(14) . . ?
N10 C11 C12 124.8(2) . . ?
N10 C11 H11 117.6 . . ?
C12 C11 H11 117.6 . . ?
C17 C12 C11 120.3(2) . . ?
C17 C12 C13X 119.8(4) . . ?
C11 C12 C13X 119.3(4) . . ?
C17 C12 C13Y 118.2(7) . . ?
C11 C12 C13Y 121.2(7) . . ?
C16 C15 C14Y 122.2(7) . . ?
C16 C15 C14X 122.0(4) . . ?
C16 C15 H15 119.0 . . ?
C14X C15 H15 119.0 . . ?
C15 C16 C17 120.3(3) . . ?
C15 C16 H16 119.9 . . ?
C17 C16 H16 119.9 . . ?
O18 C17 C12 121.7(2) . . ?
O18 C17 C16 118.3(2) . . ?
C12 C17 C16 119.9(3) . . ?
C17 O18 V1 133.69(17) . . ?
C13X C14X C22X 118.9(4) . . ?
C13X C14X C15 118.9(6) . . ?
C22X C14X C15 122.2(6) . . ?
C14X C13X C19X 118.1(4) . . ?
C14X C13X C12 118.6(6) . . ?
C19X C13X C12 123.3(6) . . ?
C20X C19X C13X 121.1(5) . . ?
C20X C19X H19X 119.5 . . ?
C13X C19X H19X 119.5 . . ?
C19X C20X C21X 120.4(6) . . ?
C19X C20X H20X 119.8 . . ?
C21X C20X H20X 119.8 . . ?
C22X C21X C20X 120.0(5) . . ?
C22X C21X H21X 120.0 . . ?
C20X C21X H21X 120.0 . . ?
C21X C22X C14X 121.5(5) . . ?
C21X C22X H22X 119.3 . . ?
C14X C22X H22X 119.3 . . ?
C22Y C14Y C13Y 122.2(7) . . ?
C22Y C14Y C15 119.3(12) . . ?
C13Y C14Y C15 117.5(13) . . ?
C14Y C13Y C19Y 115.3(7) . . ?
C14Y C13Y C12 120.1(12) . . ?
C19Y C13Y C12 124.6(11) . . ?
C20Y C19Y C13Y 121.3(9) . . ?
C20Y C19Y H19Y 119.3 . . ?
C13Y C19Y H19Y 119.3 . . ?
C19Y C20Y C21Y 121.8(9) . . ?
C19Y C20Y H20Y 119.1 . . ?
C21Y C20Y H20Y 119.1 . . ?
C22Y C21Y C20Y 119.1(9) . . ?
C22Y C21Y H21Y 120.5 . . ?
C20Y C21Y H21Y 120.5 . . ?
C21Y C22Y C14Y 120.0(9) . . ?
C21Y C22Y H22Y 120.0 . . ?
C14Y C22Y H22Y 120.0 . . ?
C26 O25 V1 109.37(15) . . ?
C26 O25 H25 117(2) . . ?
V1 O25 H25 128(2) . . ?
O25 C26 C27 125.0(2) . . ?
O25 C26 C31 113.3(2) . . ?
C27 C26 C31 121.6(2) . . ?
C26 C27 C28 118.9(2) . . ?
C26 C27 H27 120.6 . . ?
C28 C27 H27 120.6 . . ?
C27 C28 C29 118.5(2) . . ?
C27 C28 C33X 121.8(5) . . ?
C29 C28 C33X 119.6(4) . . ?
C27 C28 C33Y 123.1(6) . . ?
C29 C28 C33Y 118.3(6) . . ?
C27 C28 C33Z 116.9(6) . . ?
C29 C28 C33Z 124.5(6) . . ?
C30 C29 C28 124.2(2) . . ?
C30 C29 H29 117.9 . . ?
C28 C29 H29 117.9 . . ?
C29 C30 C31 115.9(2) . . ?
C29 C30 C37Y 120.3(10) . . ?
C31 C30 C37Y 122.5(9) . . ?
C29 C30 C37X 123.7(4) . . ?
C31 C30 C37X 120.3(4) . . ?
O32 C31 C26 116.0(2) . . ?
O32 C31 C30 123.4(2) . . ?
C26 C31 C30 120.6(2) . . ?
C31 O32 V1 124.93(15) . . ?
C34X C33X C35X 109.7(5) . . ?
C34X C33X C28 111.2(12) . . ?
C35X C33X C28 108.9(7) . . ?
C34X C33X C36X 108.8(6) . . ?
C35X C33X C36X 108.8(5) . . ?
C28 C33X C36X 109.5(7) . . ?
C33X C34X H34A 109.5 . . ?
C33X C34X H34B 109.5 . . ?
H34A C34X H34B 109.5 . . ?
C33X C34X H34C 109.5 . . ?
H34A C34X H34C 109.5 . . ?
H34B C34X H34C 109.5 . . ?
C33X C35X H35A 109.5 . . ?
C33X C35X H35B 109.5 . . ?
H35A C35X H35B 109.5 . . ?
C33X C35X H35C 109.5 . . ?
H35A C35X H35C 109.5 . . ?
H35B C35X H35C 109.5 . . ?
C33X C36X H36A 109.5 . . ?
C33X C36X H36B 109.5 . . ?
H36A C36X H36B 109.5 . . ?
C33X C36X H36C 109.5 . . ?
H36A C36X H36C 109.5 . . ?
H36B C36X H36C 109.5 . . ?
C40X C37X C38X 108.7(4) . . ?
C40X C37X C39X 108.8(4) . . ?
C38X C37X C39X 107.8(4) . . ?
C40X C37X C30 111.2(5) . . ?
C38X C37X C30 109.6(4) . . ?
C39X C37X C30 110.6(7) . . ?
C37X C38X H38A 109.5 . . ?
C37X C38X H38B 109.5 . . ?
H38A C38X H38B 109.5 . . ?
C37X C38X H38C 109.5 . . ?
H38A C38X H38C 109.5 . . ?
H38B C38X H38C 109.5 . . ?
C37X C39X H39A 109.5 . . ?
C37X C39X H39B 109.5 . . ?
H39A C39X H39B 109.5 . . ?
C37X C39X H39C 109.5 . . ?
H39A C39X H39C 109.5 . . ?
H39B C39X H39C 109.5 . . ?
C37X C40X H40A 109.5 . . ?
C37X C40X H40B 109.5 . . ?
H40A C40X H40B 109.5 . . ?
C37X C40X H40C 109.5 . . ?
H40A C40X H40C 109.5 . . ?
H40B C40X H40C 109.5 . . ?
C36Y C33Y C34Y 109.4(6) . . ?
C36Y C33Y C28 110.5(9) . . ?
C34Y C33Y C28 110.4(16) . . ?
C36Y C33Y C35Y 109.0(6) . . ?
C34Y C33Y C35Y 108.9(6) . . ?
C28 C33Y C35Y 108.5(9) . . ?
C33Y C34Y H34D 109.5 . . ?
C33Y C34Y H34E 109.5 . . ?
H34D C34Y H34E 109.5 . . ?
C33Y C34Y H34F 109.5 . . ?
H34D C34Y H34F 109.5 . . ?
H34E C34Y H34F 109.5 . . ?
C33Y C35Y H35D 109.5 . . ?
C33Y C35Y H35E 109.5 . . ?
H35D C35Y H35E 109.5 . . ?
C33Y C35Y H35F 109.5 . . ?
H35D C35Y H35F 109.5 . . ?
H35E C35Y H35F 109.5 . . ?
C33Y C36Y H36D 109.5 . . ?
C33Y C36Y H36E 109.5 . . ?
H36D C36Y H36E 109.5 . . ?
C33Y C36Y H36F 109.5 . . ?
H36D C36Y H36F 109.5 . . ?
H36E C36Y H36F 109.5 . . ?
C40Y C37Y C38Y 109.8(7) . . ?
C40Y C37Y C39Y 110.0(7) . . ?
C38Y C37Y C39Y 109.3(7) . . ?
C40Y C37Y C30 105.4(17) . . ?
C38Y C37Y C30 108.1(15) . . ?
C39Y C37Y C30 114(2) . . ?
C37Y C38Y H38D 109.5 . . ?
C37Y C38Y H38E 109.5 . . ?
H38D C38Y H38E 109.5 . . ?
C37Y C38Y H38F 109.5 . . ?
H38D C38Y H38F 109.5 . . ?
H38E C38Y H38F 109.5 . . ?
C37Y C39Y H39D 109.5 . . ?
C37Y C39Y H39E 109.5 . . ?
H39D C39Y H39E 109.5 . . ?
C37Y C39Y H39F 109.5 . . ?
H39D C39Y H39F 109.5 . . ?
H39E C39Y H39F 109.5 . . ?
C37Y C40Y H40D 109.5 . . ?
C37Y C40Y H40E 109.5 . . ?
H40D C40Y H40E 109.5 . . ?
C37Y C40Y H40F 109.5 . . ?
H40D C40Y H40F 109.5 . . ?
H40E C40Y H40F 109.5 . . ?
C36Z C33Z C34Z 108.9(6) . . ?
C36Z C33Z C35Z 108.9(6) . . ?
C34Z C33Z C35Z 108.7(6) . . ?
C36Z C33Z C28 110.8(12) . . ?
C34Z C33Z C28 108.5(11) . . ?
C35Z C33Z C28 111.0(11) . . ?
C33Z C34Z H34G 109.5 . . ?
C33Z C34Z H34H 109.5 . . ?
H34G C34Z H34H 109.5 . . ?
C33Z C34Z H34I 109.5 . . ?
H34G C34Z H34I 109.5 . . ?
H34H C34Z H34I 109.5 . . ?
C33Z C35Z H35G 109.5 . . ?
C33Z C35Z H35H 109.5 . . ?
H35G C35Z H35H 109.5 . . ?
C33Z C35Z H35I 109.5 . . ?
H35G C35Z H35I 109.5 . . ?
H35H C35Z H35I 109.5 . . ?
C33Z C36Z H36G 109.5 . . ?
C33Z C36Z H36H 109.5 . . ?
H36G C36Z H36H 109.5 . . ?
C33Z C36Z H36I 109.5 . . ?
H36G C36Z H36I 109.5 . . ?
H36H C36Z H36I 109.5 . . ?

_refine_diff_density_max         0.396
_refine_diff_density_min         -0.331
_refine_diff_density_rms         0.068

_shelxl_version_number           2013-2



