# Electronic Supplementary Material (ESI) for Inorganic Chemistry Frontiers.
# This journal is © the Partner Organisations 2022

####################################################################### 
# 
# 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_1s_153K
_database_code_depnum_ccdc_archive 'CCDC 2177817'
loop_
_audit_author_name
_audit_author_address
'Yoji Horii'
;Nara Womens University
Japan
;
_audit_update_record             
;
2022-06-08 deposited with the CCDC.	2022-10-04 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C48 H62 N2 O4.50 V0.50'
_chemical_formula_weight         764.46

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                   34.154(4)
_cell_length_b                   10.8740(4)
_cell_length_c                   29.147(3)
_cell_angle_alpha                90
_cell_angle_beta                 128.799(18)
_cell_angle_gamma                90
_cell_volume                     8437(2)
_cell_formula_units_Z            8
_cell_measurement_temperature    153

_cell_measurement_reflns_used    12170

_cell_measurement_theta_min      1.6120

_cell_measurement_theta_max      31.7770


_exptl_crystal_description       prism

_exptl_crystal_colour            red

_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.204
_exptl_crystal_F_000             3292
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.132

_exptl_crystal_size_mid          0.079

_exptl_crystal_size_min          0.010

_exptl_absorpt_coefficient_mu    0.178
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan

_exptl_absorpt_correction_T_min  0.51551

_exptl_absorpt_correction_T_max  1.00000

_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      153

_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_measurement_device_type  
'dtrek-CrysAlisPro-abstract goniometer imported rigaku-d*trek images'

_diffrn_measurement_method       'ω scans'

_diffrn_detector_area_resol_mean ?

_diffrn_reflns_number            45870
_diffrn_reflns_av_unetI/netI     0.0682
_diffrn_reflns_av_R_equivalents  0.0795
_diffrn_reflns_limit_h_min       -44
_diffrn_reflns_limit_h_max       44
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_theta_min         1.793
_diffrn_reflns_theta_max         27.500
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             9696
_reflns_number_gt                6683
_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       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_structure_solution    ?

_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Yadokari-XG 2009 (Wakita Nemoto et al., 2009)'

_computing_publication_material  
;Yadokari-XG 2009 (Wakita,Nemoto et al., 2009)
;

_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)+(0.0150P)²+26.3738P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    ?

_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         9696
_refine_ls_number_parameters     530
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1206
_refine_ls_R_factor_gt           0.0805
_refine_ls_wR_factor_ref         0.1592
_refine_ls_wR_factor_gt          0.1459
_refine_ls_goodness_of_fit_ref   1.161
_refine_ls_restrained_S_all      1.161
_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 0.49260(3) 0.52176(8) 0.01034(4) 0.0186(2) Uani 0.5 1 d . . P . .
O002 O 0.81808(8) 0.7180(2) 0.38811(9) 0.0342(5) Uani 1 1 d . . . . .
O003 O 0.84994(8) 0.5569(2) 0.37324(10) 0.0395(6) Uani 1 1 d . . . . .
O004 O 0.52844(8) -0.31650(19) 0.16430(10) 0.0364(6) Uani 1 1 d . . . . .
N9 N 0.55061(8) 0.6374(2) 0.03486(10) 0.0218(5) Uani 1 1 d . . . . .
N10 N 0.54661(8) 0.4033(2) 0.07486(10) 0.0218(5) Uani 1 1 d . . . . .
O007 O 0.45297(10) -0.2768(2) 0.13886(13) 0.0534(7) Uani 1 1 d . . . . .
C20 C 0.62104(11) 0.7574(3) 0.09776(12) 0.0235(6) Uani 1 1 d . . . . .
H1 H 0.652433 0.782768 0.131131 0.028 Uiso 1 1 calc R U . . .
C009 C 0.59673(10) 0.6430(2) 0.09068(12) 0.0210(6) Uani 1 1 d . . . . .
C00A C 0.61714(10) 0.5508(2) 0.13342(12) 0.0210(6) Uani 1 1 d . . . . .
C00B C 0.59006(10) 0.8213(3) 0.04721(13) 0.0237(6) Uani 1 1 d . . . . .
H2 H 0.596060 0.898943 0.039412 0.028 Uiso 1 1 calc R U . . .
C00C C 0.54620(10) 0.7474(2) 0.00772(13) 0.0216(6) Uani 1 1 d . . . . .
C00D C 0.66838(10) 0.5718(3) 0.19093(12) 0.0217(6) Uani 1 1 d . . . . .
C00E C 0.59303(10) 0.4398(3) 0.12580(12) 0.0233(6) Uani 1 1 d . . . . .
C00F C 0.81546(11) 0.6238(3) 0.35672(13) 0.0278(7) Uani 1 1 d . . . . .
C00G C 0.49225(10) 0.0947(3) 0.07073(12) 0.0227(6) Uani 1 1 d . . . . .
C00H C 0.76398(11) 0.6101(3) 0.29867(12) 0.0232(6) Uani 1 1 d . . . . .
C00I C 0.67737(11) 0.6697(3) 0.22742(13) 0.0249(6) Uani 1 1 d . . . . .
H3 H 0.651301 0.722882 0.215826 0.030 Uiso 1 1 calc R U . . .
C00J C 0.61247(12) 0.3474(3) 0.17047(13) 0.0286(7) Uani 1 1 d . . . . .
H4 H 0.642863 0.350505 0.208481 0.034 Uiso 1 1 calc R U . . .
C00K C 0.48895(11) -0.1321(3) 0.11331(13) 0.0253(6) Uani 1 1 d . . . . .
C00L C 0.72466(11) 0.6885(3) 0.28067(12) 0.0244(6) Uani 1 1 d . . . . .
H5 H 0.730073 0.754096 0.304506 0.029 Uiso 1 1 calc R U . . .
C00M C 0.48753(12) -0.2485(3) 0.13967(14) 0.0295(7) Uani 1 1 d . . . . .
C00N C 0.57857(11) 0.2554(3) 0.14718(13) 0.0290(7) Uani 1 1 d . . . . .
H6 H 0.581341 0.183294 0.166198 0.035 Uiso 1 1 calc R U . . .
C00O C 0.70807(10) 0.4940(3) 0.20889(13) 0.0256(6) Uani 1 1 d . . . . .
H7 H 0.702829 0.429131 0.184809 0.031 Uiso 1 1 calc R U . . .
C00P C 0.53734(11) 0.2890(3) 0.08759(13) 0.0248(6) Uani 1 1 d . . . . .
C00Q C 0.49459(11) 0.2179(2) 0.04928(13) 0.0227(6) Uani 1 1 d . . . . .
C00R C 0.45682(11) 0.0722(3) 0.07902(13) 0.0289(7) Uani 1 1 d . . . . .
H8 H 0.433971 0.133223 0.070253 0.035 Uiso 1 1 calc R U . . .
C00S C 0.75545(11) 0.5124(3) 0.26250(13) 0.0258(6) Uani 1 1 d . . . . .
H9 H 0.781586 0.459282 0.274264 0.031 Uiso 1 1 calc R U . . .
C00T C 0.52505(11) 0.0008(2) 0.08256(13) 0.0257(6) Uani 1 1 d . . . . .
H10 H 0.548125 0.013608 0.076019 0.031 Uiso 1 1 calc R U . . .
C00U C 0.45543(11) -0.0403(3) 0.10019(14) 0.0303(7) Uani 1 1 d . . . . .
H11 H 0.431712 -0.054126 0.105623 0.036 Uiso 1 1 calc R U . . .
C00V C 0.52382(11) -0.1123(3) 0.10406(13) 0.0269(7) Uani 1 1 d . . . . .
H12 H 0.546148 -0.174255 0.112195 0.032 Uiso 1 1 calc R U . . .
C00W C 0.58525(13) -0.4483(3) 0.24646(15) 0.0382(8) Uani 1 1 d . . . . .
H13 H 0.605517 -0.455176 0.233808 0.046 Uiso 1 1 calc R U . . .
H14 H 0.587884 -0.525606 0.264820 0.046 Uiso 1 1 calc R U . . .
C00X C 0.60711(13) -0.3467(3) 0.29248(15) 0.0400(8) Uani 1 1 d . . . . .
H15 H 0.606576 -0.269860 0.275196 0.048 Uiso 1 1 calc R U . . .
H16 H 0.586226 -0.336675 0.304161 0.048 Uiso 1 1 calc R U . . .
C00Y C 0.72977(13) 0.0727(3) 0.52777(16) 0.0434(9) Uani 1 1 d . . . . .
H17 H 0.725378 0.141643 0.503799 0.052 Uiso 1 1 calc R U . . .
H18 H 0.763823 0.042631 0.548994 0.052 Uiso 1 1 calc R U . . .
C00Z C 0.66068(14) -0.3741(3) 0.34671(16) 0.0456(9) Uani 1 1 d . . . . .
H19 H 0.659583 -0.431869 0.371256 0.055 Uiso 1 1 calc R U . . .
H20 H 0.677946 -0.414232 0.334182 0.055 Uiso 1 1 calc R U . . .
C010 C 0.53157(14) -0.4299(3) 0.19319(17) 0.0446(9) Uani 1 1 d . . . . .
H21 H 0.520173 -0.498918 0.166494 0.054 Uiso 1 1 calc R U . . .
H22 H 0.510418 -0.424100 0.204679 0.054 Uiso 1 1 calc R U . . .
C011 C 0.86552(13) 0.7332(4) 0.44715(14) 0.0433(9) Uani 1 1 d . . . . .
H23 H 0.891013 0.764318 0.445110 0.052 Uiso 1 1 calc R U . . .
H24 H 0.876786 0.654835 0.467507 0.052 Uiso 1 1 calc R U . . .
C012 C 0.88916(14) 1.0639(3) 0.55587(16) 0.0478(9) Uani 1 1 d . . . . .
H25 H 0.915213 1.092947 0.554412 0.057 Uiso 1 1 calc R U . . .
H26 H 0.900137 0.985894 0.576565 0.057 Uiso 1 1 calc R U . . .
C013 C 0.69129(14) -0.2631(4) 0.38384(16) 0.0478(10) Uani 1 1 d . . . . .
H27 H 0.691897 -0.204996 0.359044 0.057 Uiso 1 1 calc R U . . .
H28 H 0.725590 -0.289620 0.414334 0.057 Uiso 1 1 calc R U . . .
C014 C 0.72343(13) 0.1183(3) 0.57210(16) 0.0444(9) Uani 1 1 d . . . . .
H29 H 0.690404 0.155084 0.550920 0.053 Uiso 1 1 calc R U . . .
H30 H 0.724918 0.048360 0.593804 0.053 Uiso 1 1 calc R U . . .
C015 C 0.70714(14) -0.0906(4) 0.45251(16) 0.0461(9) Uani 1 1 d . . . . .
H31 H 0.741194 -0.121678 0.479902 0.055 Uiso 1 1 calc R U . . .
H32 H 0.706827 -0.029076 0.428184 0.055 Uiso 1 1 calc R U . . .
C016 C 0.69352(13) -0.0284(4) 0.48751(16) 0.0446(9) Uani 1 1 d . . . . .
H33 H 0.660052 0.006184 0.460313 0.054 Uiso 1 1 calc R U . . .
H34 H 0.692726 -0.089892 0.511028 0.054 Uiso 1 1 calc R U . . .
C017 C 0.86041(15) 1.5221(3) 0.74886(17) 0.0489(10) Uani 1 1 d . . . . .
H57 H 0.885751 1.507973 0.790303 0.073 Uiso 1 1 calc R U . . .
H58 H 0.827878 1.505998 0.737859 0.073 Uiso 1 1 calc R U . . .
H59 H 0.862010 1.606075 0.739959 0.073 Uiso 1 1 calc R U . . .
C018 C 0.85703(15) 0.8239(3) 0.47989(16) 0.0506(10) Uani 1 1 d . . . . .
H35 H 0.828988 0.795200 0.477676 0.061 Uiso 1 1 calc R U . . .
H36 H 0.886573 0.824095 0.521065 0.061 Uiso 1 1 calc R U . . .
C019 C 0.88315(14) 1.1564(3) 0.59066(17) 0.0462(9) Uani 1 1 d . . . . .
H37 H 0.875037 1.236342 0.571936 0.055 Uiso 1 1 calc R U . . .
H38 H 0.855268 1.131131 0.589438 0.055 Uiso 1 1 calc R U . . .
C01A C 0.76268(14) 0.2118(4) 0.61565(18) 0.0488(10) Uani 1 1 d . . . . .
H39 H 0.795654 0.174205 0.637735 0.059 Uiso 1 1 calc R U . . .
H40 H 0.761908 0.280650 0.593955 0.059 Uiso 1 1 calc R U . . .
C01B C 0.67298(14) -0.1960(4) 0.41312(16) 0.0454(9) Uani 1 1 d . . . . .
H41 H 0.639560 -0.163868 0.382843 0.054 Uiso 1 1 calc R U . . .
H42 H 0.670580 -0.254223 0.436468 0.054 Uiso 1 1 calc R U . . .
C01C C 0.86931(14) 1.4367(4) 0.71460(17) 0.0490(10) Uani 1 1 d . . . . .
H43 H 0.867565 1.352161 0.723844 0.059 Uiso 1 1 calc R U . . .
H44 H 0.842582 1.448745 0.672804 0.059 Uiso 1 1 calc R U . . .
C01D C 0.92990(14) 1.1679(4) 0.65430(17) 0.0473(9) Uani 1 1 d . . . . .
H71 H 0.956207 1.203617 0.654854 0.057 Uiso 0.771(12) 1 calc R U P A 1
H72 H 0.940696 1.085613 0.670516 0.057 Uiso 0.771(12) 1 calc R U P A 1
H73 H 0.960198 1.186621 0.659442 0.057 Uiso 0.229(12) 1 calc R U P A 2
H74 H 0.935134 1.099754 0.679100 0.057 Uiso 0.229(12) 1 calc R U P A 2
C01E C 0.91902(15) 1.4567(4) 0.7276(2) 0.0494(10) Uani 1 1 d . . . . .
H75 H 0.945792 1.432867 0.768055 0.033(13) Uiso 0.771(12) 1 calc R . P A 1
H76 H 0.922907 1.543612 0.723944 0.043(13) Uiso 0.771(12) 1 calc R . P A 1
H77 H 0.943991 1.484186 0.767932 0.12(9) Uiso 0.229(12) 1 calc R . P A 2
H78 H 0.915799 1.518550 0.701485 0.8(8) Uiso 0.229(12) 1 calc R . P A 2
C01F C 0.92585(19) 1.2445(4) 0.6959(2) 0.0308(14) Uani 0.771(12) 1 d . . P A 1
H63 H 0.895554 1.220766 0.689915 0.037 Uiso 0.771(12) 1 calc R U P A 1
H64 H 0.954279 1.225432 0.736361 0.037 Uiso 0.771(12) 1 calc R U P A 1
C01G C 0.84123(16) 1.0433(4) 0.49330(18) 0.0608(12) Uani 1 1 d . . . . .
H51 H 0.830052 1.121674 0.472910 0.073 Uiso 1 1 calc R U . . .
H52 H 0.815346 1.013512 0.494912 0.073 Uiso 1 1 calc R U . . .
C01H C 0.75523(16) 0.2595(4) 0.65843(19) 0.0605(12) Uani 1 1 d . . . . .
H60 H 0.723554 0.301358 0.637129 0.091 Uiso 1 1 calc R U . . .
H61 H 0.781847 0.315574 0.685476 0.091 Uiso 1 1 calc R U . . .
H62 H 0.755572 0.191849 0.679840 0.091 Uiso 1 1 calc R U . . .
O8 O 0.46806(14) 0.5830(3) 0.03633(17) 0.0248(9) Uani 0.5 1 d . . P . .
C01J C 0.84662(19) 0.9522(4) 0.45744(17) 0.0666(13) Uani 1 1 d . . . . .
H53 H 0.815901 0.952999 0.416991 0.080 Uiso 1 1 calc R U . . .
H54 H 0.873698 0.979493 0.457516 0.080 Uiso 1 1 calc R U . . .
C01K C 0.9246(2) 1.3832(5) 0.6864(3) 0.0370(15) Uani 0.771(12) 1 d . . P A 1
H65 H 0.896673 1.402554 0.645737 0.044 Uiso 0.771(12) 1 calc R U P A 1
H66 H 0.955340 1.407881 0.693624 0.044 Uiso 0.771(12) 1 calc R U P A 1
C21 C 0.9014(9) 1.295(3) 0.6580(11) 0.091(13) Uani 0.229(12) 1 d . . P A 2
H67 H 0.897773 1.361726 0.633628 0.110 Uiso 0.229(12) 1 calc R U P A 2
H68 H 0.868784 1.274464 0.646898 0.110 Uiso 0.229(12) 1 calc R U P A 2
C22 C 0.9361(11) 1.322(3) 0.7173(17) 0.100(11) Uani 0.229(12) 1 d . . P A 2
H69 H 0.969506 1.327841 0.728855 0.120 Uiso 0.229(12) 1 calc R U P A 2
H70 H 0.936132 1.258307 0.740665 0.120 Uiso 0.229(12) 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 V1 1.1065(18) 5_665 ?
V1 O8 1.586(4) . ?
V1 N9 2.060(2) . ?
V1 N10 2.062(2) . ?
V1 N10 2.111(3) 5_665 ?
V1 N9 2.115(2) 5_665 ?
O002 C00F 1.338(4) . ?
O002 C011 1.456(4) . ?
O003 C00F 1.199(4) . ?
O004 C00M 1.326(4) . ?
O004 C010 1.459(4) . ?
N9 C009 1.386(4) . ?
N9 C00C 1.389(3) . ?
N10 C00E 1.388(4) . ?
N10 C00P 1.389(4) . ?
O007 C00M 1.206(4) . ?
C20 C00B 1.349(4) . ?
C20 C009 1.437(4) . ?
C009 C00A 1.399(4) . ?
C00A C00E 1.398(4) . ?
C00A C00D 1.500(4) . ?
C00B C00C 1.433(4) . ?
C00C C00Q 1.394(4) 5_665 ?
C00D C00O 1.392(4) . ?
C00D C00I 1.396(4) . ?
C00E C00J 1.436(4) . ?
C00F C00H 1.499(4) . ?
C00G C00T 1.390(4) . ?
C00G C00R 1.396(4) . ?
C00G C00Q 1.502(4) . ?
C00H C00L 1.387(4) . ?
C00H C00S 1.393(4) . ?
C00I C00L 1.385(4) . ?
C00J C00N 1.348(4) . ?
C00K C00U 1.380(4) . ?
C00K C00V 1.393(4) . ?
C00K C00M 1.497(4) . ?
C00N C00P 1.438(4) . ?
C00O C00S 1.390(4) . ?
C00P C00Q 1.390(4) . ?
C00R C00U 1.384(4) . ?
C00T C00V 1.393(4) . ?
C00W C010 1.498(5) . ?
C00W C00X 1.524(5) . ?
C00X C00Z 1.520(5) . ?
C00Y C016 1.516(5) . ?
C00Y C014 1.521(5) . ?
C00Z C013 1.518(5) . ?
C011 C018 1.521(5) . ?
C012 C01G 1.521(5) . ?
C012 C019 1.530(5) . ?
C013 C01B 1.524(5) . ?
C014 C01A 1.519(5) . ?
C015 C016 1.519(5) . ?
C015 C01B 1.521(5) . ?
C017 C01C 1.528(5) . ?
C018 C01J 1.486(5) . ?
C019 C01D 1.515(5) . ?
C01A C01H 1.512(5) . ?
C01C C01E 1.505(5) . ?
C01D C01F 1.548(6) . ?
C01D C21 1.73(3) . ?
C01E C01K 1.552(6) . ?
C01E C22 1.67(3) . ?
C01F C01K 1.529(7) . ?
C01G C01J 1.533(6) . ?
C21 C22 1.38(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
V1 V1 O8 176.54(19) 5_665 . ?
V1 V1 N9 77.39(11) 5_665 . ?
O8 V1 N9 105.02(16) . . ?
V1 V1 N10 77.09(12) 5_665 . ?
O8 V1 N10 105.38(16) . . ?
N9 V1 N10 87.05(10) . . ?
V1 V1 N10 72.19(11) 5_665 5_665 ?
O8 V1 N10 105.32(16) . 5_665 ?
N9 V1 N10 86.32(10) . 5_665 ?
N10 V1 N10 149.28(6) . 5_665 ?
V1 V1 N9 71.91(11) 5_665 5_665 ?
O8 V1 N9 105.65(16) . 5_665 ?
N9 V1 N9 149.29(6) . 5_665 ?
N10 V1 N9 86.17(10) . 5_665 ?
N10 V1 N9 84.40(9) 5_665 5_665 ?
C00F O002 C011 116.3(3) . . ?
C00M O004 C010 117.1(3) . . ?
C009 N9 C00C 105.6(2) . . ?
C009 N9 V1 124.97(19) . . ?
C00C N9 V1 126.19(19) . . ?
C009 N9 V1 127.15(18) . 5_665 ?
C00C N9 V1 124.43(19) . 5_665 ?
V1 N9 V1 30.71(6) . 5_665 ?
C00E N10 C00P 105.6(2) . . ?
C00E N10 V1 124.53(18) . . ?
C00P N10 V1 125.39(19) . . ?
C00E N10 V1 127.29(19) . 5_665 ?
C00P N10 V1 125.23(19) . 5_665 ?
V1 N10 V1 30.72(6) . 5_665 ?
C00B C20 C009 107.6(2) . . ?
N9 C009 C00A 125.4(2) . . ?
N9 C009 C20 109.7(2) . . ?
C00A C009 C20 124.9(3) . . ?
C00E C00A C009 124.2(2) . . ?
C00E C00A C00D 117.9(2) . . ?
C009 C00A C00D 117.9(2) . . ?
C20 C00B C00C 107.3(2) . . ?
N9 C00C C00Q 125.6(3) . 5_665 ?
N9 C00C C00B 109.9(2) . . ?
C00Q C00C C00B 124.5(3) 5_665 . ?
C00O C00D C00I 118.6(3) . . ?
C00O C00D C00A 120.5(2) . . ?
C00I C00D C00A 120.9(3) . . ?
N10 C00E C00A 125.5(3) . . ?
N10 C00E C00J 109.9(2) . . ?
C00A C00E C00J 124.6(3) . . ?
O003 C00F O002 124.2(3) . . ?
O003 C00F C00H 123.7(3) . . ?
O002 C00F C00H 112.1(3) . . ?
C00T C00G C00R 118.7(3) . . ?
C00T C00G C00Q 120.9(3) . . ?
C00R C00G C00Q 120.4(3) . . ?
C00L C00H C00S 119.3(3) . . ?
C00L C00H C00F 122.6(3) . . ?
C00S C00H C00F 118.1(3) . . ?
C00L C00I C00D 120.8(3) . . ?
C00N C00J C00E 107.4(3) . . ?
C00U C00K C00V 119.7(3) . . ?
C00U C00K C00M 117.8(3) . . ?
C00V C00K C00M 122.5(3) . . ?
C00I C00L C00H 120.4(3) . . ?
O007 C00M O004 123.7(3) . . ?
O007 C00M C00K 123.5(3) . . ?
O004 C00M C00K 112.8(3) . . ?
C00J C00N C00P 107.5(3) . . ?
C00S C00O C00D 120.6(3) . . ?
N10 C00P C00Q 125.7(3) . . ?
N10 C00P C00N 109.6(2) . . ?
C00Q C00P C00N 124.7(3) . . ?
C00P C00Q C00C 124.7(3) . 5_665 ?
C00P C00Q C00G 117.7(3) . . ?
C00C C00Q C00G 117.6(2) 5_665 . ?
C00U C00R C00G 120.5(3) . . ?
C00O C00S C00H 120.3(3) . . ?
C00G C00T C00V 120.9(3) . . ?
C00K C00U C00R 120.6(3) . . ?
C00T C00V C00K 119.6(3) . . ?
C010 C00W C00X 115.0(3) . . ?
C00Z C00X C00W 112.3(3) . . ?
C016 C00Y C014 114.3(3) . . ?
C013 C00Z C00X 115.3(3) . . ?
O004 C010 C00W 108.1(3) . . ?
O002 C011 C018 107.9(3) . . ?
C01G C012 C019 113.6(3) . . ?
C00Z C013 C01B 116.1(3) . . ?
C01A C014 C00Y 114.0(3) . . ?
C016 C015 C01B 115.4(3) . . ?
C00Y C016 C015 113.4(3) . . ?
C01J C018 C011 114.8(3) . . ?
C01D C019 C012 112.9(3) . . ?
C01H C01A C014 113.7(3) . . ?
C015 C01B C013 113.2(3) . . ?
C01E C01C C017 113.7(3) . . ?
C019 C01D C01F 117.4(3) . . ?
C019 C01D C21 86.5(9) . . ?
C01C C01E C01K 113.4(4) . . ?
C01C C01E C22 107.0(10) . . ?
C01K C01F C01D 113.2(4) . . ?
C012 C01G C01J 114.5(4) . . ?
C018 C01J C01G 113.9(3) . . ?
C01F C01K C01E 111.7(4) . . ?
C22 C21 C01D 100(2) . . ?
C21 C22 C01E 107(3) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C00C N9 C009 C00A -179.2(3) . . . . ?
V1 N9 C009 C00A 20.2(4) . . . . ?
V1 N9 C009 C00A -17.9(4) 5_665 . . . ?
C00C N9 C009 C20 -0.4(3) . . . . ?
V1 N9 C009 C20 -160.88(19) . . . . ?
V1 N9 C009 C20 160.97(19) 5_665 . . . ?
C00B C20 C009 N9 0.5(3) . . . . ?
C00B C20 C009 C00A 179.4(3) . . . . ?
N9 C009 C00A C00E -1.2(5) . . . . ?
C20 C009 C00A C00E -179.9(3) . . . . ?
N9 C009 C00A C00D 178.3(3) . . . . ?
C20 C009 C00A C00D -0.4(4) . . . . ?
C009 C20 C00B C00C -0.5(3) . . . . ?
C009 N9 C00C C00Q -179.8(3) . . . 5_665 ?
V1 N9 C00C C00Q -19.6(4) . . . 5_665 ?
V1 N9 C00C C00Q 18.2(4) 5_665 . . 5_665 ?
C009 N9 C00C C00B 0.1(3) . . . . ?
V1 N9 C00C C00B 160.29(19) . . . . ?
V1 N9 C00C C00B -161.91(18) 5_665 . . . ?
C20 C00B C00C N9 0.3(3) . . . . ?
C20 C00B C00C C00Q -179.9(3) . . . 5_665 ?
C00E C00A C00D C00O 61.4(4) . . . . ?
C009 C00A C00D C00O -118.0(3) . . . . ?
C00E C00A C00D C00I -118.8(3) . . . . ?
C009 C00A C00D C00I 61.7(4) . . . . ?
C00P N10 C00E C00A -179.0(3) . . . . ?
V1 N10 C00E C00A -21.8(4) . . . . ?
V1 N10 C00E C00A 16.2(4) 5_665 . . . ?
C00P N10 C00E C00J -0.3(3) . . . . ?
V1 N10 C00E C00J 156.9(2) . . . . ?
V1 N10 C00E C00J -165.1(2) 5_665 . . . ?
C009 C00A C00E N10 2.1(5) . . . . ?
C00D C00A C00E N10 -177.4(3) . . . . ?
C009 C00A C00E C00J -176.5(3) . . . . ?
C00D C00A C00E C00J 4.1(4) . . . . ?
C011 O002 C00F O003 -3.6(4) . . . . ?
C011 O002 C00F C00H 175.4(3) . . . . ?
O003 C00F C00H C00L 179.8(3) . . . . ?
O002 C00F C00H C00L 0.8(4) . . . . ?
O003 C00F C00H C00S 1.5(4) . . . . ?
O002 C00F C00H C00S -177.5(3) . . . . ?
C00O C00D C00I C00L -0.6(4) . . . . ?
C00A C00D C00I C00L 179.6(3) . . . . ?
N10 C00E C00J C00N 0.3(4) . . . . ?
C00A C00E C00J C00N 179.0(3) . . . . ?
C00D C00I C00L C00H 0.0(4) . . . . ?
C00S C00H C00L C00I 0.2(4) . . . . ?
C00F C00H C00L C00I -178.0(3) . . . . ?
C010 O004 C00M O007 -1.8(5) . . . . ?
C010 O004 C00M C00K 177.8(3) . . . . ?
C00U C00K C00M O007 15.9(5) . . . . ?
C00V C00K C00M O007 -166.7(3) . . . . ?
C00U C00K C00M O004 -163.7(3) . . . . ?
C00V C00K C00M O004 13.7(4) . . . . ?
C00E C00J C00N C00P -0.1(4) . . . . ?
C00I C00D C00O C00S 1.0(4) . . . . ?
C00A C00D C00O C00S -179.2(3) . . . . ?
C00E N10 C00P C00Q 179.3(3) . . . . ?
V1 N10 C00P C00Q 22.4(4) . . . . ?
V1 N10 C00P C00Q -15.5(4) 5_665 . . . ?
C00E N10 C00P C00N 0.2(3) . . . . ?
V1 N10 C00P C00N -156.7(2) . . . . ?
V1 N10 C00P C00N 165.4(2) 5_665 . . . ?
C00J C00N C00P N10 -0.1(4) . . . . ?
C00J C00N C00P C00Q -179.2(3) . . . . ?
N10 C00P C00Q C00C -1.5(5) . . . 5_665 ?
C00N C00P C00Q C00C 177.5(3) . . . 5_665 ?
N10 C00P C00Q C00G 178.2(3) . . . . ?
C00N C00P C00Q C00G -2.9(4) . . . . ?
C00T C00G C00Q C00P -66.1(4) . . . . ?
C00R C00G C00Q C00P 114.1(3) . . . . ?
C00T C00G C00Q C00C 113.6(3) . . . 5_665 ?
C00R C00G C00Q C00C -66.2(4) . . . 5_665 ?
C00T C00G C00R C00U 1.8(4) . . . . ?
C00Q C00G C00R C00U -178.4(3) . . . . ?
C00D C00O C00S C00H -0.8(4) . . . . ?
C00L C00H C00S C00O 0.1(4) . . . . ?
C00F C00H C00S C00O 178.5(3) . . . . ?
C00R C00G C00T C00V -2.1(4) . . . . ?
C00Q C00G C00T C00V 178.1(3) . . . . ?
C00V C00K C00U C00R -1.3(5) . . . . ?
C00M C00K C00U C00R 176.1(3) . . . . ?
C00G C00R C00U C00K -0.2(5) . . . . ?
C00G C00T C00V C00K 0.6(5) . . . . ?
C00U C00K C00V C00T 1.1(5) . . . . ?
C00M C00K C00V C00T -176.3(3) . . . . ?
C010 C00W C00X C00Z 177.0(3) . . . . ?
C00W C00X C00Z C013 159.0(3) . . . . ?
C00M O004 C010 C00W -144.0(3) . . . . ?
C00X C00W C010 O004 61.0(4) . . . . ?
C00F O002 C011 C018 -167.0(3) . . . . ?
C00X C00Z C013 C01B 64.6(4) . . . . ?
C016 C00Y C014 C01A 175.1(3) . . . . ?
C014 C00Y C016 C015 -168.1(3) . . . . ?
C01B C015 C016 C00Y 177.8(3) . . . . ?
O002 C011 C018 C01J -68.0(4) . . . . ?
C01G C012 C019 C01D 175.2(3) . . . . ?
C00Y C014 C01A C01H 178.3(3) . . . . ?
C016 C015 C01B C013 -174.2(3) . . . . ?
C00Z C013 C01B C015 176.5(3) . . . . ?
C012 C019 C01D C01F -171.6(3) . . . . ?
C012 C019 C01D C21 169.2(9) . . . . ?
C017 C01C C01E C01K -171.7(4) . . . . ?
C017 C01C C01E C22 151.2(14) . . . . ?
C019 C01D C01F C01K -75.0(5) . . . . ?
C019 C012 C01G C01J 179.3(3) . . . . ?
C011 C018 C01J C01G -176.6(3) . . . . ?
C012 C01G C01J C018 66.1(5) . . . . ?
C01D C01F C01K C01E 178.4(4) . . . . ?
C01C C01E C01K C01F -66.2(6) . . . . ?
C019 C01D C21 C22 175(2) . . . . ?
C01D C21 C22 C01E 171.6(12) . . . . ?
C01C C01E C22 C21 66(2) . . . . ?

_refine_diff_density_max         0.419
_refine_diff_density_min         -0.291
_refine_diff_density_rms         0.056


_symmetry_cell_setting           ?
_symmetry_space_group_name_H-M   ?
_diffrn_radiation_source         ?
_diffrn_radiation_monochromator  graphite
_chemical_absolute_configuration ?
####################################################################### 
# 
# 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_1s_200K
_database_code_depnum_ccdc_archive 'CCDC 2177828'
loop_
_audit_author_name
_audit_author_address
'Yoji Horii'
;Nara Womens University
Japan
;
_audit_update_record             
;
2022-06-08 deposited with the CCDC.	2022-10-04 downloaded from the CCDC.
;

_vrf_PLAT149_1s_200K             
;
PROBLEM:  s.u. on the beta Angle is Too Large ....... 0.06 Degree
RESPONSE: This alert originates from the low crystallinity of the sample. 
;
_vrf_PLAT220_1s_200K             
;
PROBLEM:  NonSolvent Resd 1 C Ueq(max)/Ueq(min) Range 9.6 Ratio
RESPONSE: This alert originates from the heavy disorders on alkyl chains. 
;
_vrf_PLAT234_1s_200K             
;
PROBLEM:  Large Hirshfeld Difference C26 --C27 . 0.27 Ang.
PROBLEM:   Large Hirshfeld Difference C68 --C69 . 0.26 Ang.
RESPONSE: This alert originates from the heavy disorders on alkyl chains. 
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C48 H62 N2 O4.50 V0.50'
_chemical_formula_weight         764.46

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                   47.983(15)
_cell_length_b                   10.7203(7)
_cell_length_c                   27.091(8)
_cell_angle_alpha                90
_cell_angle_beta                 141.08(6)
_cell_angle_gamma                90
_cell_volume                     8754(8)
_cell_formula_units_Z            8
_cell_measurement_temperature    200

_cell_measurement_reflns_used    8342

_cell_measurement_theta_min      1.9970

_cell_measurement_theta_max      31.8830


_exptl_crystal_description       prism

_exptl_crystal_colour            red

_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.160
_exptl_crystal_F_000             3292
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.07

_exptl_crystal_size_mid          0.07

_exptl_crystal_size_min          0.03

_exptl_absorpt_coefficient_mu    0.171
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan

_exptl_absorpt_correction_T_min  0.95138

_exptl_absorpt_correction_T_max  1.00000

_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      200

_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_measurement_device_type  
'dtrek-CrysAlisPro-abstract goniometer imported rigaku-d*trek images'

_diffrn_measurement_method       'ω scans'

_diffrn_detector_area_resol_mean ?

_diffrn_reflns_number            47412
_diffrn_reflns_av_unetI/netI     0.1303
_diffrn_reflns_av_R_equivalents  0.1212
_diffrn_reflns_limit_h_min       -62
_diffrn_reflns_limit_h_max       61
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_theta_min         2.016
_diffrn_reflns_theta_max         27.499
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             10051
_reflns_number_gt                4334
_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       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_structure_solution    ?

_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Yadokari-XG 2009 (Wakita Nemoto et al., 2009)'

_computing_publication_material  
;Yadokari-XG 2009 (Wakita,Nemoto et al., 2009)
;

_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)+(0.0708P)²+13.6283P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    ?

_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         10051
_refine_ls_number_parameters     650
_refine_ls_number_restraints     275
_refine_ls_R_factor_all          0.2122
_refine_ls_R_factor_gt           0.0940
_refine_ls_wR_factor_ref         0.2543
_refine_ls_wR_factor_gt          0.1935
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_restrained_S_all      1.037
_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 0.23424(4) 0.27098(11) 0.47737(8) 0.0429(4) Uani 0.5 1 d . . P . .
O1 O 0.18733(17) 0.3344(4) 0.4060(3) 0.0491(13) Uani 0.5 1 d . . P . .
N1 N 0.26821(11) 0.3876(3) 0.57101(18) 0.0447(8) Uani 1 1 d . . . . .
N2 N 0.27380(11) 0.3473(3) 0.47554(19) 0.0464(8) Uani 1 1 d . . . . .
C1 C 0.27939(13) 0.5081(3) 0.6557(2) 0.0482(10) Uani 1 1 d . . . . .
H1 H 0.279176 0.533653 0.688226 0.058 Uiso 1 1 calc R U . . .
C2 C 0.29654(13) 0.5717(3) 0.6412(2) 0.0488(10) Uani 1 1 d . . . . .
H2 H 0.310444 0.649096 0.661890 0.059 Uiso 1 1 calc R U . . .
C3 C 0.28940(13) 0.4982(3) 0.5881(2) 0.0433(9) Uani 1 1 d . . . . .
C4 C 0.29440(13) 0.4632(3) 0.5051(2) 0.0470(10) Uani 1 1 d . . . . .
C5 C 0.26145(13) 0.3938(3) 0.6123(2) 0.0431(9) Uani 1 1 d . . . . .
C6 C 0.30810(15) 0.4969(4) 0.4751(3) 0.0575(11) Uani 1 1 d . . . . .
H6 H 0.322161 0.570640 0.485401 0.069 Uiso 1 1 calc R U . . .
C7 C 0.29706(15) 0.4034(3) 0.4297(3) 0.0581(12) Uani 1 1 d . . . . .
H7 H 0.302628 0.399725 0.403630 0.070 Uiso 1 1 calc R U . . .
C8 C 0.27526(14) 0.3103(3) 0.4282(2) 0.0472(10) Uani 1 1 d . . . . .
C9 C 0.30141(13) 0.5350(3) 0.5568(2) 0.0444(9) Uani 1 1 d . . . . .
C10 C 0.25915(13) 0.1974(3) 0.3878(2) 0.0443(9) Uani 1 1 d . . . . .
C11 C 0.32245(14) 0.6595(3) 0.5793(2) 0.0460(10) Uani 1 1 d . . . . .
C12 C 0.36434(15) 0.6835(4) 0.6549(3) 0.0633(12) Uani 1 1 d . . . . .
H12 H 0.379407 0.621249 0.692653 0.076 Uiso 1 1 calc R U . . .
C13 C 0.38471(15) 0.7990(4) 0.6761(3) 0.0643(12) Uani 1 1 d . . . . .
H13 H 0.412900 0.813882 0.727595 0.077 Uiso 1 1 calc R U . . .
C14 C 0.36261(14) 0.8907(4) 0.6199(3) 0.0524(10) Uani 1 1 d . . . . .
C15 C 0.32048(14) 0.8691(4) 0.5444(3) 0.0539(11) Uani 1 1 d . . . . .
H15 H 0.305297 0.931536 0.506659 0.065 Uiso 1 1 calc R U . . .
C16 C 0.30073(14) 0.7539(3) 0.5247(2) 0.0492(10) Uani 1 1 d . . . . .
H16 H 0.272172 0.740106 0.473596 0.059 Uiso 1 1 calc R U . . .
C17 C 0.26561(13) 0.1723(3) 0.3429(2) 0.0460(10) Uani 1 1 d . . . . .
C18 C 0.29548(14) 0.0813(3) 0.3691(2) 0.0490(10) Uani 1 1 d . . . . .
H18 H 0.310239 0.033940 0.413073 0.059 Uiso 1 1 calc R U . . .
C19 C 0.30360(14) 0.0601(3) 0.3308(2) 0.0500(10) Uani 1 1 d . . . . .
H19 H 0.323714 -0.001123 0.348954 0.060 Uiso 1 1 calc R U . . .
C20 C 0.28159(14) 0.1307(4) 0.2648(2) 0.0479(10) Uani 1 1 d . . . . .
C21 C 0.25125(15) 0.2198(4) 0.2378(2) 0.0575(11) Uani 1 1 d . . . . .
H21 H 0.235923 0.265767 0.193104 0.069 Uiso 1 1 calc R U . . .
C22 C 0.24342(15) 0.2414(4) 0.2766(3) 0.0580(11) Uani 1 1 d . . . . .
H22 H 0.223216 0.302427 0.258231 0.070 Uiso 1 1 calc R U . . .
C23 C 0.38541(17) 1.0125(4) 0.6427(3) 0.0697(13) Uani 1 1 d . . . . .
O2 O 0.41848(14) 1.0423(3) 0.7103(2) 0.1031(13) Uani 1 1 d . . . . .
O3 O 0.36712(12) 1.0802(3) 0.5825(2) 0.0921(12) Uani 1 1 d . . . . .
C24 C 0.29118(16) 0.1178(4) 0.2244(3) 0.0599(12) Uani 1 1 d . . . . .
O4 O 0.27516(12) 0.1849(3) 0.1712(2) 0.0754(10) Uani 1 1 d . . . . .
O5 O 0.31863(11) 0.0237(3) 0.25265(18) 0.0702(9) Uani 1 1 d . . . . .
C25 C 0.3877(2) 1.2004(5) 0.6001(4) 0.125(3) Uani 1 1 d D . . . .
H25 H 0.396890 1.241390 0.642985 0.151 Uiso 0.564(10) 1 calc R U P A 1
H25A H 0.367163 1.254447 0.554389 0.151 Uiso 0.564(10) 1 calc R U P A 1
H25B H 0.365699 1.265320 0.574522 0.151 Uiso 0.436(10) 1 calc R U P A 2
H25C H 0.411250 1.214502 0.656293 0.151 Uiso 0.436(10) 1 calc R U P A 2
C26 C 0.4301(5) 1.1688(15) 0.6244(9) 0.112(6) Uani 0.564(10) 1 d D . P A 1
H26 H 0.444581 1.246700 0.635756 0.134 Uiso 0.564(10) 1 calc R U P A 1
H26A H 0.450965 1.120630 0.672648 0.134 Uiso 0.564(10) 1 calc R U P A 1
C27 C 0.4205(5) 1.0944(18) 0.5615(8) 0.115(6) Uani 0.564(10) 1 d D . P A 1
H27 H 0.402386 1.144148 0.514480 0.138 Uiso 0.564(10) 1 calc R U P A 1
H27A H 0.404906 1.017240 0.547179 0.138 Uiso 0.564(10) 1 calc R U P A 1
C28 C 0.4677(6) 1.066(2) 0.6022(13) 0.145(9) Uani 0.564(10) 1 d D . P A 1
H28 H 0.480375 1.141528 0.605968 0.174 Uiso 0.564(10) 1 calc R U P A 1
H28A H 0.488015 1.032726 0.654697 0.174 Uiso 0.564(10) 1 calc R U P A 1
C29 C 0.4589(5) 0.9659(18) 0.5477(9) 0.151(8) Uani 0.564(10) 1 d D . P A 1
H29 H 0.443042 0.894245 0.538745 0.181 Uiso 0.564(10) 1 calc R U P A 1
H29A H 0.441657 1.002270 0.497317 0.181 Uiso 0.564(10) 1 calc R U P A 1
C30 C 0.5070(5) 0.926(2) 0.5949(9) 0.131(7) Uani 0.564(10) 1 d D . P A 1
H30 H 0.520761 0.996959 0.597585 0.158 Uiso 0.564(10) 1 calc R U P A 1
H30A H 0.525267 0.903927 0.648230 0.158 Uiso 0.564(10) 1 calc R U P A 1
C31 C 0.5045(5) 0.8118(17) 0.5543(9) 0.139(7) Uani 0.564(10) 1 d D . P A 1
H31 H 0.490200 0.742042 0.550874 0.167 Uiso 0.564(10) 1 calc R U P A 1
H31A H 0.486439 0.835029 0.501217 0.167 Uiso 0.564(10) 1 calc R U P A 1
C32 C 0.5488(6) 0.7724(19) 0.5978(12) 0.133(6) Uani 0.564(10) 1 d D . P A 1
H32 H 0.564024 0.845300 0.605997 0.159 Uiso 0.564(10) 1 calc R U P A 1
H32A H 0.565591 0.742804 0.649128 0.159 Uiso 0.564(10) 1 calc R U P A 1
C33 C 0.5499(5) 0.6748(16) 0.5610(8) 0.134(6) Uani 0.564(10) 1 d D . P A 1
H33 H 0.532160 0.701691 0.508658 0.161 Uiso 0.564(10) 1 calc R U P A 1
H33A H 0.536619 0.599346 0.555815 0.161 Uiso 0.564(10) 1 calc R U P A 1
C34 C 0.5953(7) 0.646(2) 0.6063(13) 0.158(8) Uani 0.564(10) 1 d D . P A 1
H34 H 0.608881 0.723642 0.614295 0.189 Uiso 0.564(10) 1 calc R U P A 1
H34A H 0.612227 0.616104 0.657641 0.189 Uiso 0.564(10) 1 calc R U P A 1
C35 C 0.5995(5) 0.556(2) 0.5724(9) 0.162(7) Uani 0.564(10) 1 d D . P A 1
H35 H 0.584287 0.589000 0.522698 0.195 Uiso 0.564(10) 1 calc R U P A 1
H35A H 0.583931 0.480693 0.560724 0.195 Uiso 0.564(10) 1 calc R U P A 1
C36 C 0.6451(8) 0.519(3) 0.6195(15) 0.213(13) Uani 0.564(10) 1 d D . P A 1
H36 H 0.643224 0.459445 0.590653 0.319 Uiso 0.564(10) 1 calc R U P A 1
H36A H 0.660854 0.591615 0.630059 0.319 Uiso 0.564(10) 1 calc R U P A 1
H36B H 0.660496 0.482854 0.668246 0.319 Uiso 0.564(10) 1 calc R U P A 1
C37 C 0.4043(8) 1.2119(13) 0.5784(14) 0.116(6) Uani 0.436(10) 1 d D . P A 2
H37 H 0.418454 1.293034 0.595724 0.139 Uiso 0.436(10) 1 calc R U P A 2
H37A H 0.379876 1.211800 0.521458 0.139 Uiso 0.436(10) 1 calc R U P A 2
C38 C 0.4346(9) 1.124(2) 0.6048(18) 0.132(9) Uani 0.436(10) 1 d D . P A 2
H38 H 0.424505 1.043388 0.602896 0.159 Uiso 0.436(10) 1 calc R U P A 2
H38A H 0.462471 1.141480 0.659677 0.159 Uiso 0.436(10) 1 calc R U P A 2
C39 C 0.4437(8) 1.110(2) 0.5674(14) 0.125(7) Uani 0.436(10) 1 d D . P A 2
H39 H 0.415693 1.092271 0.512683 0.150 Uiso 0.436(10) 1 calc R U P A 2
H39A H 0.453099 1.191642 0.568511 0.150 Uiso 0.436(10) 1 calc R U P A 2
C40 C 0.4740(8) 1.025(2) 0.5914(17) 0.105(6) Uani 0.436(10) 1 d D . P A 2
H40 H 0.501733 1.048338 0.645318 0.126 Uiso 0.436(10) 1 calc R U P A 2
H40A H 0.465310 0.946806 0.594566 0.126 Uiso 0.436(10) 1 calc R U P A 2
C41 C 0.4855(8) 0.994(2) 0.5598(12) 0.127(7) Uani 0.436(10) 1 d D . P A 2
H41 H 0.497424 1.069459 0.561480 0.152 Uiso 0.436(10) 1 calc R U P A 2
H41A H 0.457944 0.976495 0.504722 0.152 Uiso 0.436(10) 1 calc R U P A 2
C42 C 0.5155(11) 0.895(2) 0.589(2) 0.159(12) Uani 0.436(10) 1 d D . P A 2
H42 H 0.539697 0.904023 0.645318 0.191 Uiso 0.436(10) 1 calc R U P A 2
H42A H 0.499990 0.819889 0.576758 0.191 Uiso 0.436(10) 1 calc R U P A 2
C43 C 0.5369(6) 0.8631(19) 0.5728(11) 0.119(6) Uani 0.436(10) 1 d D . P A 2
H43 H 0.550774 0.939296 0.580140 0.143 Uiso 0.436(10) 1 calc R U P A 2
H43A H 0.513239 0.844615 0.517017 0.143 Uiso 0.436(10) 1 calc R U P A 2
C44 C 0.5694(8) 0.767(2) 0.6107(18) 0.129(9) Uani 0.436(10) 1 d D . P A 2
H44 H 0.592924 0.783486 0.666587 0.155 Uiso 0.436(10) 1 calc R U P A 2
H44A H 0.555445 0.689636 0.602033 0.155 Uiso 0.436(10) 1 calc R U P A 2
C45 C 0.5910(5) 0.7386(16) 0.5946(10) 0.104(5) Uani 0.436(10) 1 d D . P A 2
H45 H 0.606416 0.814115 0.605968 0.125 Uiso 0.436(10) 1 calc R U P A 2
H45A H 0.567620 0.725726 0.538312 0.125 Uiso 0.436(10) 1 calc R U P A 2
C46 C 0.6220(7) 0.638(2) 0.6305(15) 0.120(7) Uani 0.436(10) 1 d D . P A 2
H46 H 0.607389 0.562681 0.621605 0.145 Uiso 0.436(10) 1 calc R U P A 2
H46A H 0.646488 0.653091 0.686706 0.145 Uiso 0.436(10) 1 calc R U P A 2
C47 C 0.6413(9) 0.610(2) 0.6095(17) 0.128(8) Uani 0.436(10) 1 d D . P A 2
H47 H 0.661031 0.539895 0.639860 0.192 Uiso 0.436(10) 1 calc R U P A 2
H47A H 0.618175 0.589788 0.554628 0.192 Uiso 0.436(10) 1 calc R U P A 2
H47B H 0.657570 0.680885 0.620223 0.192 Uiso 0.436(10) 1 calc R U P A 2
C48 C 0.33092(19) 0.0070(5) 0.2178(3) 0.0894(17) Uani 1 1 d D . . . .
H48 H 0.304823 -0.011914 0.162263 0.107 Uiso 0.644(5) 1 calc R U P B 3
H48A H 0.344250 0.082821 0.223402 0.107 Uiso 0.644(5) 1 calc R U P B 3
H48B H 0.336692 0.087352 0.210553 0.107 Uiso 0.356(5) 1 calc R U P B -4
H48C H 0.306967 -0.033169 0.166931 0.107 Uiso 0.356(5) 1 calc R U P B -4
C49 C 0.3722(5) -0.0732(12) 0.2730(11) 0.058(4) Uiso 0.356(5) 1 d D . P B -4
H49 H 0.385023 -0.071996 0.257835 0.070 Uiso 0.356(5) 1 calc R U P B -4
H49A H 0.394120 -0.042495 0.326427 0.070 Uiso 0.356(5) 1 calc R U P B -4
C50 C 0.3586(5) -0.2001(11) 0.2674(9) 0.045(3) Uiso 0.356(5) 1 d D . P B -4
H50 H 0.331684 -0.221695 0.212692 0.054 Uiso 0.356(5) 1 calc R U P B -4
H50A H 0.352407 -0.204235 0.294004 0.054 Uiso 0.356(5) 1 calc R U P B -4
C51 C 0.3950(16) -0.292(4) 0.305(3) 0.31(3) Uiso 0.356(5) 1 d D . P B -4
H51 H 0.421083 -0.261330 0.357690 0.368 Uiso 0.356(5) 1 calc R U P B -4
H51A H 0.386713 -0.368552 0.309937 0.368 Uiso 0.356(5) 1 calc R U P B -4
C52 C 0.4113(5) -0.3323(17) 0.2778(9) 0.068(5) Uiso 0.356(5) 1 d D . P B -4
H52 H 0.386302 -0.375316 0.228632 0.082 Uiso 0.356(5) 1 calc R U P B -4
H52A H 0.414477 -0.255276 0.263665 0.082 Uiso 0.356(5) 1 calc R U P B -4
C53 C 0.4505(7) -0.408(3) 0.3170(13) 0.102(7) Uiso 0.356(5) 1 d D . P B -4
H53 H 0.475689 -0.376124 0.370139 0.123 Uiso 0.356(5) 1 calc R U P B -4
H53A H 0.445274 -0.492207 0.321490 0.123 Uiso 0.356(5) 1 calc R U P B -4
C54 C 0.4648(8) -0.418(2) 0.2843(14) 0.127(9) Uiso 0.356(5) 1 d D . P B -4
H54 H 0.471002 -0.335166 0.280337 0.152 Uiso 0.356(5) 1 calc R U P B -4
H54A H 0.440554 -0.452416 0.231665 0.152 Uiso 0.356(5) 1 calc R U P B -4
C55 C 0.5054(7) -0.4989(19) 0.3333(12) 0.113(6) Uiso 0.356(5) 1 d D . P B -4
H55 H 0.530649 -0.459873 0.384055 0.135 Uiso 0.356(5) 1 calc R U P B -4
H55A H 0.500516 -0.579327 0.342118 0.135 Uiso 0.356(5) 1 calc R U P B -4
C56 C 0.5148(9) -0.517(3) 0.2945(14) 0.204(13) Uiso 0.356(5) 1 d D . P B -4
H56 H 0.518374 -0.436067 0.283596 0.244 Uiso 0.356(5) 1 calc R U P B -4
H56A H 0.490142 -0.559171 0.244904 0.244 Uiso 0.356(5) 1 calc R U P B -4
C57 C 0.5562(9) -0.592(2) 0.3449(17) 0.210(13) Uiso 0.356(5) 1 d D . P B -4
H57 H 0.563467 -0.592474 0.319998 0.252 Uiso 0.356(5) 1 calc R U P B -4
H57A H 0.580184 -0.549056 0.394842 0.252 Uiso 0.356(5) 1 calc R U P B -4
C58 C 0.5553(7) -0.7203(18) 0.3608(13) 0.138(8) Uiso 0.356(5) 1 d D . P B -4
H58 H 0.548756 -0.721604 0.386921 0.166 Uiso 0.356(5) 1 calc R U P B -4
H58A H 0.584218 -0.757895 0.395868 0.166 Uiso 0.356(5) 1 calc R U P B -4
C59 C 0.5212(6) -0.7944(18) 0.2870(11) 0.160(9) Uiso 0.356(5) 1 d D . P B -4
H59 H 0.521264 -0.878600 0.299108 0.240 Uiso 0.356(5) 1 calc R U P B -4
H59A H 0.492470 -0.758052 0.252596 0.240 Uiso 0.356(5) 1 calc R U P B -4
H59B H 0.527889 -0.794299 0.261533 0.240 Uiso 0.356(5) 1 calc R U P B -4
C60 C 0.3616(6) -0.0927(14) 0.2575(13) 0.194(10) Uani 0.644(5) 1 d D . P B 3
H60 H 0.359287 -0.119757 0.220253 0.232 Uiso 0.644(5) 1 calc R U P B 3
H60A H 0.390059 -0.050902 0.298961 0.232 Uiso 0.644(5) 1 calc R U P B 3
C61 C 0.3685(8) -0.1990(18) 0.2913(14) 0.262(14) Uani 0.644(5) 1 d D . P B 3
H61 H 0.340140 -0.241774 0.251285 0.315 Uiso 0.644(5) 1 calc R U P B 3
H61A H 0.372613 -0.173845 0.331108 0.315 Uiso 0.644(5) 1 calc R U P B 3
C62 C 0.4004(5) -0.2943(10) 0.3276(11) 0.134(5) Uani 0.644(5) 1 d D . P B 3
H62 H 0.424753 -0.280839 0.383970 0.161 Uiso 0.644(5) 1 calc R U P B 3
H62A H 0.386877 -0.373667 0.317419 0.161 Uiso 0.644(5) 1 calc R U P B 3
C63 C 0.4177(8) -0.3029(16) 0.3037(15) 0.271(12) Uani 0.644(5) 1 d D . P B 3
H63 H 0.393616 -0.312541 0.247093 0.325 Uiso 0.644(5) 1 calc R U P B 3
H63A H 0.433548 -0.226909 0.317604 0.325 Uiso 0.644(5) 1 calc R U P B 3
C64 C 0.4463(7) -0.4044(18) 0.3397(16) 0.317(14) Uani 0.644(5) 1 d D . P B 3
H64 H 0.429829 -0.477192 0.327840 0.380 Uiso 0.644(5) 1 calc R U P B 3
H64A H 0.469718 -0.391135 0.395926 0.380 Uiso 0.644(5) 1 calc R U P B 3
C65 C 0.4669(6) -0.4364(16) 0.3233(15) 0.289(13) Uani 0.644(5) 1 d D . P B 3
H65 H 0.480579 -0.362843 0.327834 0.346 Uiso 0.644(5) 1 calc R U P B 3
H65A H 0.444795 -0.466933 0.269760 0.346 Uiso 0.644(5) 1 calc R U P B 3
C66 C 0.5000(7) -0.530(2) 0.3763(17) 0.415(19) Uani 0.644(5) 1 d D . P B 3
H66 H 0.518408 -0.500540 0.428644 0.498 Uiso 0.644(5) 1 calc R U P B 3
H66A H 0.484324 -0.602785 0.367283 0.498 Uiso 0.644(5) 1 calc R U P B 3
C67 C 0.5290(7) -0.5746(16) 0.3806(15) 0.325(15) Uani 0.644(5) 1 d D . P B 3
H67 H 0.542265 -0.502828 0.382859 0.390 Uiso 0.644(5) 1 calc R U P B 3
H67A H 0.511429 -0.617551 0.331658 0.390 Uiso 0.644(5) 1 calc R U P B 3
C68 C 0.5648(6) -0.6578(14) 0.4446(13) 0.275(11) Uani 0.644(5) 1 d D . P B 3
H68 H 0.578033 -0.623115 0.492402 0.330 Uiso 0.644(5) 1 calc R U P B 3
H68A H 0.551370 -0.736555 0.435417 0.330 Uiso 0.644(5) 1 calc R U P B 3
C69 C 0.5985(4) -0.6845(14) 0.4595(10) 0.186(7) Uani 0.644(5) 1 d D . P B 3
H69 H 0.613322 -0.606017 0.473157 0.223 Uiso 0.644(5) 1 calc R U P B 3
H69A H 0.584750 -0.710256 0.409796 0.223 Uiso 0.644(5) 1 calc R U P B 3
C70 C 0.6330(4) -0.7737(11) 0.5168(7) 0.140(4) Uani 0.644(5) 1 d D . P B 3
H70 H 0.653024 -0.776714 0.516954 0.210 Uiso 0.644(5) 1 calc R U P B 3
H70A H 0.648881 -0.749365 0.567904 0.210 Uiso 0.644(5) 1 calc R U P B 3
H70B H 0.620045 -0.854569 0.503956 0.210 Uiso 0.644(5) 1 calc R U P B 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 V1 1.052(3) 7_556 ?
V1 O1 1.579(5) . ?
V1 N2 2.037(3) 7_556 ?
V1 N1 2.054(4) . ?
V1 N1 2.094(3) 7_556 ?
V1 N2 2.103(3) . ?
N1 C3 1.387(4) . ?
N1 C5 1.387(4) . ?
N2 C4 1.389(5) . ?
N2 C8 1.394(4) . ?
C1 C2 1.341(5) . ?
C1 C5 1.432(5) . ?
C2 C3 1.430(5) . ?
C3 C9 1.401(5) . ?
C4 C9 1.392(5) . ?
C4 C6 1.433(5) . ?
C5 C10 1.389(5) 7_556 ?
C6 C7 1.336(5) . ?
C7 C8 1.424(5) . ?
C8 C10 1.394(5) . ?
C9 C11 1.488(5) . ?
C10 C17 1.496(5) . ?
C11 C12 1.377(6) . ?
C11 C16 1.377(5) . ?
C12 C13 1.394(6) . ?
C13 C14 1.377(6) . ?
C14 C15 1.375(6) . ?
C14 C23 1.494(6) . ?
C15 C16 1.386(5) . ?
C17 C18 1.388(5) . ?
C17 C22 1.391(5) . ?
C18 C19 1.383(5) . ?
C19 C20 1.395(5) . ?
C20 C21 1.383(5) . ?
C20 C24 1.486(5) . ?
C21 C22 1.383(5) . ?
C23 O2 1.205(6) . ?
C23 O3 1.316(6) . ?
O3 C25 1.460(5) . ?
C24 O4 1.210(5) . ?
C24 O5 1.330(5) . ?
O5 C48 1.462(5) . ?
C25 C37 1.314(12) . ?
C25 C26 1.614(13) . ?
C26 C27 1.589(14) . ?
C27 C28 1.599(15) . ?
C28 C29 1.595(16) . ?
C29 C30 1.594(14) . ?
C30 C31 1.592(14) . ?
C31 C32 1.479(15) . ?
C32 C33 1.473(15) . ?
C33 C34 1.477(14) . ?
C34 C35 1.456(15) . ?
C35 C36 1.489(15) . ?
C37 C38 1.378(17) . ?
C38 C39 1.387(17) . ?
C39 C40 1.376(17) . ?
C40 C41 1.373(17) . ?
C41 C42 1.437(16) . ?
C42 C43 1.430(15) . ?
C43 C44 1.437(16) . ?
C44 C45 1.434(15) . ?
C45 C46 1.438(16) . ?
C46 C47 1.446(16) . ?
C48 C60 1.415(12) . ?
C48 C49 1.513(13) . ?
C49 C50 1.464(13) . ?
C50 C51 1.515(16) . ?
C51 C52 1.490(16) . ?
C52 C53 1.487(14) . ?
C53 C54 1.486(14) . ?
C54 C55 1.512(14) . ?
C55 C56 1.445(14) . ?
C56 C57 1.496(15) . ?
C57 C58 1.455(14) . ?
C58 C59 1.489(14) . ?
C60 C61 1.333(13) . ?
C61 C62 1.417(12) . ?
C62 C63 1.398(14) . ?
C63 C64 1.392(14) . ?
C64 C65 1.407(14) . ?
C65 C66 1.430(15) . ?
C66 C67 1.389(14) . ?
C67 C68 1.456(14) . ?
C68 C69 1.358(13) . ?
C69 C70 1.437(12) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
V1 V1 O1 176.1(3) 7_556 . ?
V1 V1 N2 78.76(17) 7_556 7_556 ?
O1 V1 N2 104.5(2) . 7_556 ?
V1 V1 N1 77.37(19) 7_556 . ?
O1 V1 N1 104.8(2) . . ?
N2 V1 N1 87.74(13) 7_556 . ?
V1 V1 N1 73.26(17) 7_556 7_556 ?
O1 V1 N1 104.5(2) . 7_556 ?
N2 V1 N1 86.61(12) 7_556 7_556 ?
N1 V1 N1 150.62(8) . 7_556 ?
V1 V1 N2 71.83(17) 7_556 . ?
O1 V1 N2 104.9(2) . . ?
N2 V1 N2 150.59(8) 7_556 . ?
N1 V1 N2 85.92(13) . . ?
N1 V1 N2 85.02(12) 7_556 . ?
C3 N1 C5 105.1(3) . . ?
C3 N1 V1 127.1(2) . . ?
C5 N1 V1 124.5(3) . . ?
C3 N1 V1 124.9(2) . 7_556 ?
C5 N1 V1 127.5(2) . 7_556 ?
V1 N1 V1 29.38(8) . 7_556 ?
C4 N2 C8 105.1(3) . . ?
C4 N2 V1 126.3(2) . 7_556 ?
C8 N2 V1 124.6(2) . 7_556 ?
C4 N2 V1 125.8(2) . . ?
C8 N2 V1 127.1(3) . . ?
V1 N2 V1 29.40(8) 7_556 . ?
C2 C1 C5 107.9(3) . . ?
C1 C2 C3 107.1(3) . . ?
N1 C3 C9 125.4(3) . . ?
N1 C3 C2 110.2(3) . . ?
C9 C3 C2 124.4(3) . . ?
N2 C4 C9 125.5(3) . . ?
N2 C4 C6 109.5(3) . . ?
C9 C4 C6 125.0(3) . . ?
N1 C5 C10 125.3(3) . 7_556 ?
N1 C5 C1 109.6(3) . . ?
C10 C5 C1 125.1(3) 7_556 . ?
C7 C6 C4 107.7(4) . . ?
C6 C7 C8 107.9(3) . . ?
N2 C8 C10 125.1(3) . . ?
N2 C8 C7 109.7(3) . . ?
C10 C8 C7 125.2(3) . . ?
C4 C9 C3 124.2(3) . . ?
C4 C9 C11 117.6(3) . . ?
C3 C9 C11 118.2(3) . . ?
C5 C10 C8 124.9(3) 7_556 . ?
C5 C10 C17 118.0(3) 7_556 . ?
C8 C10 C17 117.1(3) . . ?
C12 C11 C16 117.9(4) . . ?
C12 C11 C9 121.1(4) . . ?
C16 C11 C9 120.9(4) . . ?
C11 C12 C13 121.6(4) . . ?
C14 C13 C12 119.2(4) . . ?
C15 C14 C13 120.1(4) . . ?
C15 C14 C23 121.2(4) . . ?
C13 C14 C23 118.7(4) . . ?
C14 C15 C16 119.7(4) . . ?
C11 C16 C15 121.5(4) . . ?
C18 C17 C22 118.9(3) . . ?
C18 C17 C10 119.7(3) . . ?
C22 C17 C10 121.3(3) . . ?
C19 C18 C17 120.9(4) . . ?
C18 C19 C20 119.9(4) . . ?
C21 C20 C19 119.2(3) . . ?
C21 C20 C24 118.5(4) . . ?
C19 C20 C24 122.2(4) . . ?
C22 C21 C20 120.8(4) . . ?
C21 C22 C17 120.3(4) . . ?
O2 C23 O3 123.9(5) . . ?
O2 C23 C14 122.3(5) . . ?
O3 C23 C14 113.7(5) . . ?
C23 O3 C25 116.9(5) . . ?
O4 C24 O5 124.3(4) . . ?
O4 C24 C20 123.3(4) . . ?
O5 C24 C20 112.5(4) . . ?
C24 O5 C48 115.9(4) . . ?
C37 C25 O3 115.4(10) . . ?
O3 C25 C26 105.4(7) . . ?
C27 C26 C25 116.4(12) . . ?
C26 C27 C28 106.3(14) . . ?
C29 C28 C27 106.1(16) . . ?
C30 C29 C28 105.0(13) . . ?
C31 C30 C29 111.5(13) . . ?
C32 C31 C30 112.5(14) . . ?
C33 C32 C31 116.7(17) . . ?
C32 C33 C34 113.0(16) . . ?
C35 C34 C33 117.0(19) . . ?
C34 C35 C36 118(2) . . ?
C25 C37 C38 117.8(19) . . ?
C37 C38 C39 120(3) . . ?
C40 C39 C38 122(3) . . ?
C41 C40 C39 131(2) . . ?
C40 C41 C42 124(2) . . ?
C43 C42 C41 132(2) . . ?
C42 C43 C44 126(2) . . ?
C45 C44 C43 125(2) . . ?
C44 C45 C46 124.2(18) . . ?
C45 C46 C47 122(2) . . ?
C60 C48 O5 107.8(9) . . ?
O5 C48 C49 107.9(11) . . ?
C50 C49 C48 106.9(12) . . ?
C49 C50 C51 110(2) . . ?
C52 C51 C50 130(3) . . ?
C53 C52 C51 131.5(19) . . ?
C54 C53 C52 121.7(16) . . ?
C53 C54 C55 113.2(17) . . ?
C56 C55 C54 110.9(18) . . ?
C55 C56 C57 111(2) . . ?
C58 C57 C56 117(2) . . ?
C57 C58 C59 111(2) . . ?
C61 C60 C48 136.4(17) . . ?
C60 C61 C62 130.5(17) . . ?
C63 C62 C61 115.8(14) . . ?
C64 C63 C62 110.3(17) . . ?
C63 C64 C65 122(2) . . ?
C64 C65 C66 111(2) . . ?
C67 C66 C65 125(2) . . ?
C66 C67 C68 119(2) . . ?
C69 C68 C67 120.9(19) . . ?
C68 C69 C70 124.3(16) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C5 C1 C2 C3 0.2(5) . . . . ?
C5 N1 C3 C9 -177.6(4) . . . . ?
V1 N1 C3 C9 -17.5(5) . . . . ?
V1 N1 C3 C9 19.0(5) 7_556 . . . ?
C5 N1 C3 C2 1.2(4) . . . . ?
V1 N1 C3 C2 161.2(3) . . . . ?
V1 N1 C3 C2 -162.3(3) 7_556 . . . ?
C1 C2 C3 N1 -0.9(5) . . . . ?
C1 C2 C3 C9 177.8(4) . . . . ?
C8 N2 C4 C9 -178.6(4) . . . . ?
V1 N2 C4 C9 -20.2(6) 7_556 . . . ?
V1 N2 C4 C9 16.4(6) . . . . ?
C8 N2 C4 C6 0.4(4) . . . . ?
V1 N2 C4 C6 158.8(3) 7_556 . . . ?
V1 N2 C4 C6 -164.6(3) . . . . ?
C3 N1 C5 C10 179.6(4) . . . 7_556 ?
V1 N1 C5 C10 18.8(5) . . . 7_556 ?
V1 N1 C5 C10 -17.5(6) 7_556 . . 7_556 ?
C3 N1 C5 C1 -1.0(4) . . . . ?
V1 N1 C5 C1 -161.8(3) . . . . ?
V1 N1 C5 C1 161.9(3) 7_556 . . . ?
C2 C1 C5 N1 0.5(5) . . . . ?
C2 C1 C5 C10 179.9(4) . . . 7_556 ?
N2 C4 C6 C7 -1.2(5) . . . . ?
C9 C4 C6 C7 177.9(4) . . . . ?
C4 C6 C7 C8 1.4(5) . . . . ?
C4 N2 C8 C10 178.5(4) . . . . ?
V1 N2 C8 C10 19.6(6) 7_556 . . . ?
V1 N2 C8 C10 -16.8(6) . . . . ?
C4 N2 C8 C7 0.5(4) . . . . ?
V1 N2 C8 C7 -158.4(3) 7_556 . . . ?
V1 N2 C8 C7 165.2(3) . . . . ?
C6 C7 C8 N2 -1.2(5) . . . . ?
C6 C7 C8 C10 -179.2(4) . . . . ?
N2 C4 C9 C3 1.6(7) . . . . ?
C6 C4 C9 C3 -177.3(4) . . . . ?
N2 C4 C9 C11 -177.5(4) . . . . ?
C6 C4 C9 C11 3.6(6) . . . . ?
N1 C3 C9 C4 -1.5(6) . . . . ?
C2 C3 C9 C4 180.0(4) . . . . ?
N1 C3 C9 C11 177.7(3) . . . . ?
C2 C3 C9 C11 -0.9(6) . . . . ?
N2 C8 C10 C5 1.2(7) . . . 7_556 ?
C7 C8 C10 C5 178.9(4) . . . 7_556 ?
N2 C8 C10 C17 -177.3(4) . . . . ?
C7 C8 C10 C17 0.4(6) . . . . ?
C4 C9 C11 C12 -112.6(5) . . . . ?
C3 C9 C11 C12 68.2(5) . . . . ?
C4 C9 C11 C16 66.8(5) . . . . ?
C3 C9 C11 C16 -112.4(4) . . . . ?
C16 C11 C12 C13 -0.7(6) . . . . ?
C9 C11 C12 C13 178.6(4) . . . . ?
C11 C12 C13 C14 -0.7(7) . . . . ?
C12 C13 C14 C15 1.7(7) . . . . ?
C12 C13 C14 C23 -177.8(4) . . . . ?
C13 C14 C15 C16 -1.2(6) . . . . ?
C23 C14 C15 C16 178.3(4) . . . . ?
C12 C11 C16 C15 1.2(6) . . . . ?
C9 C11 C16 C15 -178.1(3) . . . . ?
C14 C15 C16 C11 -0.3(6) . . . . ?
C5 C10 C17 C18 -68.9(5) 7_556 . . . ?
C8 C10 C17 C18 109.7(4) . . . . ?
C5 C10 C17 C22 113.5(4) 7_556 . . . ?
C8 C10 C17 C22 -67.9(5) . . . . ?
C22 C17 C18 C19 0.7(6) . . . . ?
C10 C17 C18 C19 -177.0(4) . . . . ?
C17 C18 C19 C20 0.0(6) . . . . ?
C18 C19 C20 C21 -1.1(6) . . . . ?
C18 C19 C20 C24 175.9(4) . . . . ?
C19 C20 C21 C22 1.6(6) . . . . ?
C24 C20 C21 C22 -175.5(4) . . . . ?
C20 C21 C22 C17 -0.9(6) . . . . ?
C18 C17 C22 C21 -0.3(6) . . . . ?
C10 C17 C22 C21 177.4(4) . . . . ?
C15 C14 C23 O2 166.3(5) . . . . ?
C13 C14 C23 O2 -14.1(7) . . . . ?
C15 C14 C23 O3 -16.5(6) . . . . ?
C13 C14 C23 O3 163.1(4) . . . . ?
O2 C23 O3 C25 -2.6(8) . . . . ?
C14 C23 O3 C25 -179.7(5) . . . . ?
C21 C20 C24 O4 3.2(7) . . . . ?
C19 C20 C24 O4 -173.8(4) . . . . ?
C21 C20 C24 O5 -175.9(4) . . . . ?
C19 C20 C24 O5 7.1(6) . . . . ?
O4 C24 O5 C48 2.8(7) . . . . ?
C20 C24 O5 C48 -178.1(4) . . . . ?
C23 O3 C25 C37 116.6(14) . . . . ?
C23 O3 C25 C26 79.6(8) . . . . ?
O3 C25 C26 C27 57.0(14) . . . . ?
C25 C26 C27 C28 -175.6(12) . . . . ?
C26 C27 C28 C29 167.3(15) . . . . ?
C27 C28 C29 C30 -173.0(15) . . . . ?
C28 C29 C30 C31 171.7(15) . . . . ?
C29 C30 C31 C32 -179.2(15) . . . . ?
C30 C31 C32 C33 -174.4(14) . . . . ?
C31 C32 C33 C34 176.8(15) . . . . ?
C32 C33 C34 C35 -176.7(16) . . . . ?
C33 C34 C35 C36 -175.9(18) . . . . ?
O3 C25 C37 C38 -55(3) . . . . ?
C25 C37 C38 C39 162(2) . . . . ?
C37 C38 C39 C40 179(2) . . . . ?
C38 C39 C40 C41 176(3) . . . . ?
C39 C40 C41 C42 -175(3) . . . . ?
C40 C41 C42 C43 -168(3) . . . . ?
C41 C42 C43 C44 175(3) . . . . ?
C42 C43 C44 C45 -178(3) . . . . ?
C43 C44 C45 C46 -177(2) . . . . ?
C44 C45 C46 C47 177(2) . . . . ?
C24 O5 C48 C60 177.3(10) . . . . ?
C24 O5 C48 C49 162.0(7) . . . . ?
O5 C48 C49 C50 72.1(16) . . . . ?
C48 C49 C50 C51 166(2) . . . . ?
C49 C50 C51 C52 -69(5) . . . . ?
C50 C51 C52 C53 170(3) . . . . ?
C51 C52 C53 C54 -169(4) . . . . ?
C52 C53 C54 C55 180(2) . . . . ?
C53 C54 C55 C56 174(2) . . . . ?
C54 C55 C56 C57 177(2) . . . . ?
C55 C56 C57 C58 65(3) . . . . ?
C56 C57 C58 C59 62(3) . . . . ?
O5 C48 C60 C61 33(4) . . . . ?
C48 C60 C61 C62 178(2) . . . . ?
C60 C61 C62 C63 -24(4) . . . . ?
C61 C62 C63 C64 -176(2) . . . . ?
C62 C63 C64 C65 177.7(19) . . . . ?
C63 C64 C65 C66 171(2) . . . . ?
C64 C65 C66 C67 -174(2) . . . . ?
C65 C66 C67 C68 172(2) . . . . ?
C66 C67 C68 C69 -168(2) . . . . ?
C67 C68 C69 C70 -174.4(17) . . . . ?

_refine_diff_density_max         0.422
_refine_diff_density_min         -0.281
_refine_diff_density_rms         0.045


_symmetry_cell_setting           ?
_symmetry_space_group_name_H-M   ?
_diffrn_radiation_source         ?
_diffrn_radiation_monochromator  graphite
_chemical_absolute_configuration ?
####################################################################### 
# 
# 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_1m_283K
_database_code_depnum_ccdc_archive 'CCDC 2177816'
loop_
_audit_author_name
_audit_author_address
'Yoji Horii'
;Nara Womens University
Japan
;
_audit_update_record             
;
2022-06-08 deposited with the CCDC.	2022-10-04 downloaded from the CCDC.
;

_vrf_PLAT084_1m_283K             
;
PROBLEM: High wR2 Value (i.e. > 0.25) ...................       0.37 Report
RESPONSE: This alert originates from low crystallinity of the sample. 
;
_vrf_PLAT213_1m_283K             
;
PROBLEM: Atom C69             has ADP max/min Ratio .....        4.4 prolat
RESPONSE: This alert originates from thermal motion of dodecyl chains. 
;
_vrf_PLAT220_1m_283K             
;
PROBLEM: NonSolvent   Resd 1  C   Ueq(max)/Ueq(min) Range       10.0 Ratio
RESPONSE: This alert originates from thermal motion of dodecyl chains. 
;
_vrf_PLAT430_1m_283K             
;
PROBLEM: Short Inter D...A Contact  O1       ..O3       .       2.61 Ang.  
                                                   x,-1+y,z  =      1_545 Check
RESPONSE: This alert originates from thermal motion of dodecyl chains. 
;

_audit_creation_method           SHELXL-2016/4
_shelx_SHELXL_version_number     2016/4
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C48 H62 N2 O4.50 V0.50'
_chemical_formula_weight         764.46

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                   16.4545(13)
_cell_length_b                   10.8002(6)
_cell_length_c                   26.018(3)
_cell_angle_alpha                90
_cell_angle_beta                 103.803(10)
_cell_angle_gamma                90
_cell_volume                     4490.2(7)
_cell_formula_units_Z            4
_cell_measurement_temperature    283

_cell_measurement_reflns_used    8759

_cell_measurement_theta_min      2.0530

_cell_measurement_theta_max      33.3070


_exptl_crystal_description       plate

_exptl_crystal_colour            red

_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.131
_exptl_crystal_F_000             1646
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.385

_exptl_crystal_size_mid          0.169

_exptl_crystal_size_min          0.058

_exptl_absorpt_coefficient_mu    0.167
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan

_exptl_absorpt_correction_T_min  0.53215

_exptl_absorpt_correction_T_max  1.00000

_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.67a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      283

_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_measurement_device_type  
'dtrek-CrysAlisPro-abstract goniometer imported rigaku-d*trek images'

_diffrn_measurement_method       'ω scans'

_diffrn_detector_area_resol_mean ?

_diffrn_reflns_number            50119
_diffrn_reflns_av_unetI/netI     0.0808
_diffrn_reflns_av_R_equivalents  0.1261
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_theta_min         2.051
_diffrn_reflns_theta_max         27.498
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             10293
_reflns_number_gt                4418
_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       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_structure_solution    ?

_computing_structure_refinement  'SHELXL-2016/4 (Sheldrick, 2016)'
_computing_molecular_graphics    'Yadokari-XG 2009 (Wakita Nemoto et al., 2009)'

_computing_publication_material  
;Yadokari-XG 2009 (Wakita,Nemoto et al., 2009)
;

_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)+(0.1502P)²+1.6996P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    ?

_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         10293
_refine_ls_number_parameters     793
_refine_ls_number_restraints     747
_refine_ls_R_factor_all          0.2060
_refine_ls_R_factor_gt           0.1104
_refine_ls_wR_factor_ref         0.3682
_refine_ls_wR_factor_gt          0.2918
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_restrained_S_all      1.018
_refine_ls_shift/su_max          0.002
_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 0.96924(8) 0.48272(11) 0.49873(6) 0.0669(4) Uani 0.5 1 d . . P . .
O1 O 0.8809(3) 0.4207(5) 0.4772(2) 0.0770(15) Uani 0.5 1 d . . P A .
N1 N 0.9457(16) 0.591(2) 0.5585(8) 0.063(3) Uani 0.5 1 d . . P A 1
C1 C 0.946(3) 0.554(3) 0.6092(9) 0.076(5) Uani 0.5 1 d . . P A 1
C2 C 0.9100(18) 0.648(2) 0.6354(7) 0.073(4) Uani 0.5 1 d . . P A 1
H20 H 0.904336 0.646549 0.670141 0.088 Uiso 0.5 1 calc R U P A 1
C3 C 0.887(2) 0.738(2) 0.6009(7) 0.073(4) Uani 0.5 1 d . . P A 1
H21 H 0.859381 0.809895 0.607026 0.06(2) Uiso 0.5 1 calc R . P A 1
C4 C 0.9089(16) 0.7089(17) 0.5536(7) 0.060(3) Uani 0.5 1 d . . P A 1
C5 C 0.8964(17) 0.7809(19) 0.5089(7) 0.062(3) Uani 0.5 1 d . . P A 1
C6 C 0.9193(10) 0.7506(15) 0.4624(6) 0.052(3) Uani 0.5 1 d . . P A 1
N2 N 0.9588(8) 0.6406(13) 0.4543(5) 0.054(3) Uani 0.5 1 d . . P A 1
C7 C 0.9793(14) 0.6542(14) 0.4054(8) 0.056(3) Uani 0.5 1 d . . P A 1
C8 C 0.9418(13) 0.7678(17) 0.3811(7) 0.062(4) Uani 0.5 1 d . . P A 1
H22 H 0.940055 0.794297 0.346822 0.075 Uiso 0.5 1 calc R U P A 1
C9 C 0.9102(14) 0.8274(15) 0.4169(7) 0.062(3) Uani 0.5 1 d . . P A 1
H23 H 0.886267 0.905850 0.412802 0.074 Uiso 0.5 1 calc R U P A 1
C10 C 1.019(2) 0.569(2) 0.3815(10) 0.072(5) Uani 0.5 1 d . . P A 1
C11 C 0.8519(14) 0.9035(19) 0.5081(9) 0.064(4) Uani 0.5 1 d . . P A 1
C12 C 0.769(2) 0.914(4) 0.479(2) 0.130(15) Uani 0.5 1 d . . P A 1
H48 H 0.740879 0.851660 0.457643 0.156 Uiso 0.5 1 calc R U P A 1
C13 C 0.737(2) 1.014(2) 0.4851(11) 0.125(10) Uani 0.5 1 d . . P A 1
H49 H 0.679292 1.020251 0.472281 0.150 Uiso 0.5 1 calc R U P A 1
C14 C 0.778(2) 1.131(3) 0.4967(17) 0.076(7) Uani 0.5 1 d . . P A 2
C15 C 0.861(2) 1.121(2) 0.5337(14) 0.080(5) Uani 0.5 1 d . . P A 2
H50 H 0.884761 1.181075 0.558357 0.096 Uiso 0.5 1 calc R U P A 2
C16 C 0.902(3) 0.996(3) 0.5256(18) 0.083(7) Uani 0.5 1 d . . P A 2
H51 H 0.957255 0.984537 0.543830 0.099 Uiso 0.5 1 calc R U P A 2
C17 C 0.7317(4) 1.2469(5) 0.5028(3) 0.1045(16) Uani 1 1 d . . . . .
O2 O 0.660(2) 1.248(3) 0.4798(14) 0.188(15) Uani 0.5 1 d . . P A 1
O3 O 0.773(2) 1.333(3) 0.5268(13) 0.124(9) Uani 0.5 1 d . . P A 1
C18 C 0.727(2) 1.452(3) 0.5243(14) 0.157(11) Uani 0.5 1 d . . P A 1
H28 H 0.685421 1.457216 0.491116 0.189 Uiso 0.5 1 calc R U P A 1
H29 H 0.765945 1.520109 0.526100 0.189 Uiso 0.5 1 calc R U P A 1
C19 C 0.6845(6) 1.4595(7) 0.5711(4) 0.157(3) Uani 0.5 1 d . . P A 1
H36 H 0.642972 1.394432 0.568063 0.188 Uiso 0.5 1 calc R U P A 1
H37 H 0.725704 1.448809 0.604269 0.188 Uiso 0.5 1 calc R U P A 1
C19A C 0.6845(6) 1.4595(7) 0.5711(4) 0.157(3) Uani 0.5 1 d . . P A 2
H38 H 0.712660 1.440984 0.607415 0.188 Uiso 0.5 1 calc R U P A 2
H39 H 0.641055 1.397753 0.559822 0.188 Uiso 0.5 1 calc R U P A 2
C20 C 0.6430(5) 1.5847(7) 0.5699(4) 0.161(3) Uani 1 1 d . . . . .
H30 H 0.605631 1.596070 0.535251 0.193 Uiso 0.5 1 calc R U P A 1
H31 H 0.685939 1.647972 0.574133 0.193 Uiso 0.5 1 calc R U P A 1
H32 H 0.605631 1.596070 0.535251 0.193 Uiso 0.5 1 calc R U P A 2
H33 H 0.685939 1.647972 0.574133 0.193 Uiso 0.5 1 calc R U P A 2
C21 C 0.5938(6) 1.6051(8) 0.6113(4) 0.188(4) Uani 1 1 d . . . . .
H1 H 0.552994 1.538944 0.607595 0.226 Uiso 1 1 calc R U . . .
H2 H 0.632261 1.594831 0.645637 0.226 Uiso 1 1 calc R U . . .
C22 C 0.5511(5) 1.7171(7) 0.6125(4) 0.170(3) Uani 1 1 d . . . . .
H3 H 0.511154 1.725393 0.578619 0.204 Uiso 1 1 calc R U . . .
H4 H 0.591619 1.783208 0.614512 0.204 Uiso 1 1 calc R U . . .
C23 C 0.5052(6) 1.7415(8) 0.6540(4) 0.182(3) Uani 1 1 d . . . . .
H5 H 0.468318 1.671401 0.653845 0.218 Uiso 1 1 calc R U . . .
H6 H 0.546302 1.739377 0.687594 0.218 Uiso 1 1 calc R U . . .
C24 C 0.4575(6) 1.8471(8) 0.6543(5) 0.194(4) Uani 1 1 d . . . . .
H7 H 0.415087 1.846866 0.621277 0.232 Uiso 1 1 calc R U . . .
H8 H 0.493952 1.916772 0.652618 0.232 Uiso 1 1 calc R U . . .
C25 C 0.4154(6) 1.8756(9) 0.6948(4) 0.194(4) Uani 1 1 d . . . . .
H9 H 0.458026 1.884549 0.727487 0.233 Uiso 1 1 calc R U . . .
H10 H 0.382491 1.803390 0.698960 0.233 Uiso 1 1 calc R U . . .
C26 C 0.3607(7) 1.9820(9) 0.6907(5) 0.202(4) Uani 1 1 d . . . . .
H11 H 0.395298 2.053952 0.689146 0.243 Uiso 1 1 calc R U . . .
H12 H 0.321705 1.976022 0.656303 0.243 Uiso 1 1 calc R U . . .
C27 C 0.3118(6) 2.0117(10) 0.7273(4) 0.190(4) Uani 1 1 d . . . . .
H13 H 0.280190 1.937626 0.730637 0.228 Uiso 1 1 calc R U . . .
H14 H 0.351283 2.023140 0.761174 0.228 Uiso 1 1 calc R U . . .
C28 C 0.2549(7) 2.1106(12) 0.7222(5) 0.211(4) Uani 1 1 d . . . . .
H15 H 0.285479 2.183807 0.716086 0.253 Uiso 1 1 calc R U . . .
H16 H 0.213042 2.095730 0.689592 0.253 Uiso 1 1 calc R U . . .
C29 C 0.2115(7) 2.1442(11) 0.7590(4) 0.216(4) Uani 1 1 d . . . . .
H17 H 0.176813 2.214453 0.746263 0.325 Uiso 1 1 calc R U . . .
H18 H 0.177168 2.076365 0.764882 0.325 Uiso 1 1 calc R U . . .
H19 H 0.250337 2.165332 0.791644 0.325 Uiso 1 1 calc R U . . .
N3 N 0.9586(17) 0.5947(19) 0.5463(7) 0.062(3) Uani 0.5 1 d . . P A 2
C30 C 0.950(2) 0.554(3) 0.5952(9) 0.065(4) Uani 0.5 1 d . . P A 2
C31 C 0.9008(19) 0.640(2) 0.6168(6) 0.077(6) Uani 0.5 1 d . . P A 2
H24 H 0.883551 0.631827 0.648130 0.092 Uiso 0.5 1 calc R U P A 2
C32 C 0.8845(19) 0.737(2) 0.5824(7) 0.072(5) Uani 0.5 1 d . . P A 2
H25 H 0.856499 0.809276 0.586774 0.086 Uiso 0.5 1 calc R U P A 2
C33 C 0.9179(19) 0.706(2) 0.5383(8) 0.067(4) Uani 0.5 1 d . . P A 2
C34 C 0.9056(16) 0.7772(17) 0.4929(7) 0.060(3) Uani 0.5 1 d . . P A 2
C35 C 0.9358(13) 0.7459(16) 0.4498(7) 0.061(4) Uani 0.5 1 d . . P A 2
N4 N 0.9772(9) 0.6374(12) 0.4425(7) 0.059(3) Uani 0.5 1 d . . P A 2
C36 C 0.9883(17) 0.6365(19) 0.3920(7) 0.068(4) Uani 0.5 1 d . . P A 2
C37 C 0.9581(14) 0.7553(19) 0.3689(8) 0.069(4) Uani 0.5 1 d . . P A 2
H26 H 0.961980 0.784603 0.335962 0.083 Uiso 0.5 1 calc R U P A 2
C38 C 0.9248(13) 0.8134(16) 0.4025(7) 0.067(4) Uani 0.5 1 d . . P A 2
H27 H 0.897343 0.889119 0.396079 0.081 Uiso 0.5 1 calc R U P A 2
C39 C 1.0259(17) 0.5489(17) 0.3712(9) 0.058(3) Uani 0.5 1 d . . P A 2
C40 C 0.8646(14) 0.899(2) 0.4942(9) 0.063(4) Uani 0.5 1 d . . P A 2
C41 C 0.897(3) 1.005(3) 0.5318(19) 0.084(6) Uani 0.5 1 d . . P A 1
H52 H 0.951642 0.998677 0.551729 0.101 Uiso 0.5 1 calc R U P A 1
C42 C 0.859(3) 1.103(3) 0.5248(16) 0.097(8) Uani 0.5 1 d . . P A 1
H53 H 0.891463 1.174099 0.531468 0.116 Uiso 0.5 1 calc R U P A 1
C43 C 0.778(3) 1.120(4) 0.5090(17) 0.085(7) Uani 0.5 1 d . . P A 1
C44 C 0.7384(16) 1.0373(18) 0.4675(9) 0.080(4) Uani 0.5 1 d . . P A 2
H54 H 0.684272 1.045975 0.446757 0.096 Uiso 0.5 1 calc R U P A 2
C45 C 0.7847(19) 0.919(3) 0.4698(18) 0.094(5) Uani 0.5 1 d . . P A 2
H55 H 0.754992 0.851925 0.452514 0.113 Uiso 0.5 1 calc R U P A 2
O4 O 0.6693(18) 1.278(3) 0.4711(11) 0.130(5) Uani 0.5 1 d . . P A 2
O5 O 0.774(2) 1.319(3) 0.5431(13) 0.110(5) Uani 0.5 1 d . . P A 2
C46 C 0.7397(14) 1.447(2) 0.5413(13) 0.114(6) Uani 0.5 1 d . . P A 2
H34 H 0.785246 1.505392 0.553482 0.137 Uiso 0.5 1 calc R U P A 2
H35 H 0.712771 1.468292 0.504948 0.137 Uiso 0.5 1 calc R U P A 2
C47 C 1.0378(18) 0.579(2) 0.3162(7) 0.068(4) Uani 0.5 1 d . . P A 2
C48 C 1.0946(3) 0.6729(4) 0.3166(2) 0.0925(14) Uani 1 1 d . . . . .
H40 H 1.131234 0.712676 0.344504 0.13(6) Uiso 0.5 1 calc R . P A 1
H41 H 1.117746 0.718669 0.346864 0.05(2) Uiso 0.5 1 calc R . P A 2
C49 C 1.1047(17) 0.699(2) 0.2642(12) 0.093(7) Uani 0.5 1 d . . P A 1
H42 H 1.140465 0.758830 0.256314 0.112 Uiso 0.5 1 calc R U P A 1
C50 C 1.0546(9) 0.6237(13) 0.2276(5) 0.072(4) Uiso 0.5 1 d . . P A 1
C51 C 1.0073(19) 0.542(2) 0.2233(7) 0.078(4) Uani 0.5 1 d . . P A 2
H43 H 0.978110 0.501200 0.193004 0.094 Uiso 0.5 1 calc R U P A 2
C52 C 0.9932(18) 0.513(2) 0.2737(9) 0.081(4) Uani 0.5 1 d . . P A 2
H44 H 0.955320 0.452264 0.277785 0.097 Uiso 0.5 1 calc R U P A 2
C53 C 1.0810(4) 0.6515(6) 0.1726(3) 0.1069(17) Uani 1 1 d . . . . .
O6 O 1.0528(3) 0.5890(4) 0.13423(17) 0.1374(16) Uani 1 1 d . . . . .
O7 O 1.1324(3) 0.7456(4) 0.17185(15) 0.1205(12) Uani 1 1 d . . . . .
C54 C 1.0327(17) 0.590(2) 0.3306(9) 0.070(4) Uani 0.5 1 d . . P A 1
C55 C 1.002(2) 0.554(3) 0.2394(10) 0.091(5) Uani 0.5 1 d . . P A 1
H45 H 0.968042 0.508658 0.212106 0.109 Uiso 0.5 1 calc R U P A 1
C56 C 1.1135(17) 0.692(2) 0.2717(12) 0.090(7) Uani 0.5 1 d . . P A 2
H46 H 1.158588 0.744809 0.272314 0.108 Uiso 0.5 1 calc R U P A 2
C57 C 1.0720(7) 0.6416(11) 0.2204(6) 0.070(4) Uiso 0.5 1 d . . P A 2
C58 C 0.9891(19) 0.540(2) 0.2845(10) 0.089(5) Uani 0.5 1 d . . P A 1
H47 H 0.944570 0.488920 0.286676 0.106 Uiso 0.5 1 calc R U P A 1
C59 C 1.1538(5) 0.7687(8) 0.1223(3) 0.147(2) Uani 0.470(18) 1 d D . P B 3
H106 H 1.104055 0.763309 0.093533 0.177 Uiso 0.470(18) 1 calc R U P B 3
H107 H 1.193517 0.707110 0.116440 0.177 Uiso 0.470(18) 1 calc R U P B 3
C59A C 1.1538(5) 0.7687(8) 0.1223(3) 0.147(2) Uani 0.530(18) 1 d . . P B 4
H108 H 1.110506 0.817244 0.099095 0.177 Uiso 0.530(18) 1 calc R U P B 4
H109 H 1.160513 0.691466 0.104757 0.177 Uiso 0.530(18) 1 calc R U P B 4
C60 C 1.1902(17) 0.891(2) 0.1235(10) 0.195(10) Uani 0.470(18) 1 d D . P B 3
H60 H 1.208964 0.902436 0.091133 0.234 Uiso 0.470(18) 1 calc R U P B 3
H61 H 1.146245 0.951608 0.122934 0.234 Uiso 0.470(18) 1 calc R U P B 3
C61 C 1.259(3) 0.921(4) 0.1674(15) 0.35(3) Uani 0.470(18) 1 d D . P B 3
H62 H 1.302175 0.859482 0.167003 0.415 Uiso 0.470(18) 1 calc R U P B 3
H63 H 1.239663 0.905227 0.199188 0.415 Uiso 0.470(18) 1 calc R U P B 3
C62 C 1.301(3) 1.039(4) 0.1748(11) 0.29(2) Uani 0.470(18) 1 d D . P B 3
H64 H 1.261451 1.099718 0.182126 0.343 Uiso 0.470(18) 1 calc R U P B 3
H65 H 1.346582 1.033810 0.205976 0.343 Uiso 0.470(18) 1 calc R U P B 3
C63 C 1.3334(9) 1.0854(12) 0.1320(8) 0.298(9) Uani 0.470(18) 1 d D . P B 3
H66 H 1.347867 1.012043 0.114542 0.358 Uiso 0.470(18) 1 calc R U P B 3
H67 H 1.285620 1.121660 0.107365 0.358 Uiso 0.470(18) 1 calc R U P B 3
C64 C 1.4002(9) 1.1695(11) 0.1331(7) 0.270(7) Uani 0.663(16) 1 d D . P B 3
H68 H 1.446935 1.137864 0.159972 0.324 Uiso 0.663(16) 1 calc R U P B 3
H69 H 1.383516 1.246098 0.147093 0.324 Uiso 0.663(16) 1 calc R U P B 3
C63A C 1.3334(9) 1.0854(12) 0.1320(8) 0.298(9) Uani 0.530(18) 1 d . . P B 4
H80 H 1.294980 1.108654 0.098957 0.358 Uiso 0.530(18) 1 calc R U P B 4
H81 H 1.358119 1.008414 0.123918 0.358 Uiso 0.530(18) 1 calc R U P B 4
C64A C 1.4002(9) 1.1695(11) 0.1331(7) 0.270(7) Uani 0.337(16) 1 d D . P B 4
H82 H 1.417311 1.148323 0.100962 0.324 Uiso 0.337(16) 1 calc R U P B 4
H83 H 1.371167 1.247945 0.125297 0.324 Uiso 0.337(16) 1 calc R U P B 4
C65 C 1.4354(12) 1.2060(19) 0.0895(10) 0.308(13) Uani 0.663(16) 1 d D . P B 3
H70 H 1.457265 1.130343 0.077871 0.370 Uiso 0.663(16) 1 calc R U P B 3
H71 H 1.387917 1.229464 0.061311 0.370 Uiso 0.663(16) 1 calc R U P B 3
C66 C 1.4956(15) 1.295(2) 0.0891(15) 0.415(19) Uani 0.663(16) 1 d D . P B 3
H72 H 1.510077 1.282334 0.055476 0.498 Uiso 0.663(16) 1 calc R U P B 3
H73 H 1.464922 1.372212 0.085540 0.498 Uiso 0.663(16) 1 calc R U P B 3
C67 C 1.5702(15) 1.322(2) 0.1234(14) 0.524(19) Uani 0.663(16) 1 d D . P B 3
H74 H 1.598823 1.242896 0.127826 0.629 Uiso 0.663(16) 1 calc R U P B 3
H75 H 1.554320 1.336365 0.156453 0.629 Uiso 0.663(16) 1 calc R U P B 3
C68 C 1.6354(14) 1.406(2) 0.1258(14) 0.472(19) Uani 0.10(2) 1 d D . P B 3
H76 H 1.666516 1.388087 0.161627 0.567 Uiso 0.10(2) 1 calc R U P B 3
H77 H 1.665315 1.360864 0.103920 0.567 Uiso 0.10(2) 1 calc R U P B 3
C67A C 1.5702(15) 1.322(2) 0.1234(14) 0.524(19) Uani 0.337(16) 1 d D . P B 4
H84 H 1.587100 1.246707 0.108503 0.629 Uiso 0.337(16) 1 calc R U P B 4
H85 H 1.522990 1.354558 0.097055 0.629 Uiso 0.337(16) 1 calc R U P B 4
C68A C 1.6354(14) 1.406(2) 0.1258(14) 0.472(19) Uani 0.90(2) 1 d . . P B 4
H86 H 1.658652 1.384632 0.096078 0.567 Uiso 0.90(2) 1 calc R U P B 4
H87 H 1.607789 1.485366 0.116814 0.567 Uiso 0.90(2) 1 calc R U P B 4
C69 C 1.669(5) 1.522(4) 0.121(4) 0.43(11) Uani 0.10(2) 1 d D . P B 3
H78 H 1.654044 1.543310 0.083867 0.514 Uiso 0.10(2) 1 calc R U P B 3
H79 H 1.639784 1.580155 0.138867 0.514 Uiso 0.10(2) 1 calc R U P B 3
C70 C 1.753(5) 1.546(10) 0.139(4) 0.13(3) Uiso 0.10(2) 1 d D . P B 3
H103 H 1.764103 1.631137 0.132368 0.195 Uiso 0.10(2) 1 calc R U P B 3
H104 H 1.770008 1.530487 0.176523 0.195 Uiso 0.10(2) 1 calc R U P B 3
H105 H 1.784374 1.493368 0.121112 0.195 Uiso 0.10(2) 1 calc R U P B 3
C71 C 1.2390(10) 0.8428(13) 0.1366(6) 0.129(4) Uani 0.530(18) 1 d D . P B 4
H88 H 1.279068 0.801906 0.164916 0.155 Uiso 0.530(18) 1 calc R U P B 4
H89 H 1.262859 0.849046 0.105979 0.155 Uiso 0.530(18) 1 calc R U P B 4
C72 C 1.2183(10) 0.9639(14) 0.1531(6) 0.126(5) Uani 0.530(18) 1 d D . P B 4
H90 H 1.205646 0.957964 0.187571 0.151 Uiso 0.530(18) 1 calc R U P B 4
H91 H 1.168963 0.994944 0.128196 0.151 Uiso 0.530(18) 1 calc R U P B 4
C73 C 1.287(2) 1.049(4) 0.156(2) 0.34(2) Uani 0.530(18) 1 d D . P B 4
H92 H 1.263133 1.126113 0.164742 0.410 Uiso 0.530(18) 1 calc R U P B 4
H93 H 1.325383 1.023699 0.188632 0.410 Uiso 0.530(18) 1 calc R U P B 4
C74 C 1.4706(19) 1.202(3) 0.165(2) 0.43(3) Uani 0.337(16) 1 d D . P B 4
H94 H 1.499392 1.123635 0.171641 0.516 Uiso 0.337(16) 1 calc R U P B 4
H95 H 1.452985 1.220736 0.196947 0.516 Uiso 0.337(16) 1 calc R U P B 4
C75 C 1.5363(17) 1.283(4) 0.1686(15) 0.42(3) Uani 0.337(16) 1 d D . P B 4
H96 H 1.582834 1.247304 0.194526 0.507 Uiso 0.337(16) 1 calc R U P B 4
H97 H 1.520792 1.358019 0.184301 0.507 Uiso 0.337(16) 1 calc R U P B 4
C76 C 1.7008(11) 1.432(2) 0.1643(14) 0.413(18) Uani 0.90(2) 1 d D . P B 4
H98 H 1.723966 1.351955 0.177555 0.496 Uiso 0.90(2) 1 calc R U P B 4
H99 H 1.678416 1.467492 0.192263 0.496 Uiso 0.90(2) 1 calc R U P B 4
C77 C 1.7689(10) 1.5044(16) 0.1617(10) 0.270(9) Uani 0.90(2) 1 d D . P B 4
H100 H 1.807425 1.506961 0.195813 0.406 Uiso 0.90(2) 1 calc R U P B 4
H101 H 1.796352 1.469990 0.136274 0.406 Uiso 0.90(2) 1 calc R U P B 4
H102 H 1.750279 1.586854 0.151151 0.406 Uiso 0.90(2) 1 calc R U P B 4


_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 V1 1.066(2) 3_766 ?
V1 O1 1.577(5) . ?
V1 N3 1.769(16) . ?
V1 N2 1.995(14) 3_766 ?
V1 N3 2.036(15) 3_766 ?
V1 N4 2.038(16) 3_766 ?
V1 N2 2.045(14) . ?
V1 N1 2.053(15) . ?
V1 N4 2.244(15) . ?
V1 N1 2.408(15) 3_766 ?
N1a C1 1.376(18) . ?
N1a C4 1.41(2) . ?
N1a V1 2.408(15) 3_766 ?
C1a C2 1.43(3) . ?
C1a C10 1.45(4) 3_766 ?
C2a C3 1.31(2) . ?
C2a H20 0.9300 . ?
C3a C4 1.403(17) . ?
C3a H21 0.9300 . ?
C4a C5 1.373(19) . ?
C5a C6 1.388(15) . ?
C5a C11 1.51(2) . ?
C6a N2 1.394(16) . ?
C6a C9 1.423(17) . ?
N2a C7 1.398(17) . ?
N2a V1 1.995(14) 3_766 ?
C7a C10 1.364(15) . ?
C7a C8 1.45(2) . ?
C8a C9 1.336(13) . ?
C8a H22 0.9300 . ?
C9a H23 0.9300 . ?
C10a C54 1.41(2) . ?
C10a C1 1.45(4) 3_766 ?
C11a C41 1.38(4) . ?
C11a C12 1.39(4) . ?
C12a C13 1.23(4) . ?
C12a H48 0.9300 . ?
C13a C43 1.39(5) . ?
C13a H49 0.9300 . ?
C14b C44 1.34(4) . ?
C14b C15 1.47(4) . ?
C14b C17 1.49(4) . ?
C15b C16 1.55(5) . ?
C15b H50 0.9300 . ?
C16b C40 1.37(4) . ?
C16b H51 0.9300 . ?
C17 O2 1.18(3) . ?
C17 O4 1.20(3) . ?
C17 O3 1.23(3) . ?
C17 O5 1.36(3) . ?
C17 C43 1.55(4) . ?
O3a C18 1.48(4) . ?
C18a C19 1.55(4) . ?
C18a H28 0.9700 . ?
C18a H29 0.9700 . ?
C19a C20 1.511(9) . ?
C19a H36 0.9700 . ?
C19a H37 0.9700 . ?
C19Ab C46 1.33(3) . ?
C19Ab C20 1.511(9) . ?
C19Ab H38 0.9700 . ?
C19Ab H39 0.9700 . ?
C20 C21 1.510(11) . ?
C20 H30 0.9700 . ?
C20 H31 0.9700 . ?
C20 H32 0.9700 . ?
C20 H33 0.9700 . ?
C21 C22 1.403(10) . ?
C21 H1 0.9700 . ?
C21 H2 0.9700 . ?
C22 C23 1.480(11) . ?
C22 H3 0.9700 . ?
C22 H4 0.9700 . ?
C23 C24 1.386(10) . ?
C23 H5 0.9700 . ?
C23 H6 0.9700 . ?
C24 C25 1.425(12) . ?
C24 H7 0.9700 . ?
C24 H8 0.9700 . ?
C25 C26 1.448(12) . ?
C25 H9 0.9700 . ?
C25 H10 0.9700 . ?
C26 C27 1.422(11) . ?
C26 H11 0.9700 . ?
C26 H12 0.9700 . ?
C27 C28 1.406(12) . ?
C27 H13 0.9700 . ?
C27 H14 0.9700 . ?
C28 C29 1.373(12) . ?
C28 H15 0.9700 . ?
C28 H16 0.9700 . ?
C29 H17 0.9600 . ?
C29 H18 0.9600 . ?
C29 H19 0.9600 . ?
N3b C33 1.37(2) . ?
N3b C30 1.39(2) . ?
N3b V1 2.036(15) 3_766 ?
C30b C39 1.41(3) 3_766 ?
C30b C31 1.43(2) . ?
C31b C32 1.36(2) . ?
C31b H24 0.9300 . ?
C32b C33 1.423(17) . ?
C32b H25 0.9300 . ?
C33b C34 1.384(19) . ?
C34b C35 1.371(14) . ?
C34b C40 1.48(2) . ?
C35b N4 1.392(15) . ?
C35b C38 1.405(19) . ?
N4b C36 1.370(16) . ?
N4b V1 2.038(16) 3_766 ?
C36b C39 1.317(16) . ?
C36b C37 1.45(2) . ?
C37b C38 1.298(15) . ?
C37b H26 0.9300 . ?
C38b H27 0.9300 . ?
C39b C30 1.41(3) 3_766 ?
C39b C47 1.52(2) . ?
C40b C45 1.33(3) . ?
C41a C42 1.22(5) . ?
C41a H52 0.9300 . ?
C42a C43 1.31(6) . ?
C42a H53 0.9300 . ?
C44b C45 1.48(3) . ?
C44b H54 0.9300 . ?
C45b H55 0.9300 . ?
O5b C46 1.50(3) . ?
C46b H34 0.9700 . ?
C46b H35 0.9700 . ?
C47b C52 1.37(2) . ?
C47b C48 1.37(3) . ?
C48 C56 1.30(3) . ?
C48 C49 1.44(3) . ?
C48 C54 1.46(3) . ?
C48 H40 0.9300 . ?
C48 H41 0.9300 . ?
C49a C50 1.37(3) . ?
C49a H42 0.9300 . ?
C50a C55 1.24(3) . ?
C50a C53 1.619(15) . ?
C51b C52 1.42(2) . ?
C51b C57 1.53(3) . ?
C51b H43 0.9300 . ?
C52b H44 0.9300 . ?
C53 O6 1.202(7) . ?
C53 C57 1.293(14) . ?
C53 O7 1.325(7) . ?
O7 C59A 1.437(7) . ?
O7 C59 1.437(7) . ?
C54a C58 1.36(2) . ?
C55a C58 1.25(3) . ?
C55a H45 0.9300 . ?
C56b C57 1.45(3) . ?
C56b H46 0.9300 . ?
C58a H47 0.9300 . ?
C59c C60 1.452(15) . ?
C59c H106 0.9700 . ?
C59c H107 0.9700 . ?
C59Ad C71 1.580(19) . ?
C59Ad H108 0.9700 . ?
C59Ad H109 0.9700 . ?
C60c C61 1.440(17) . ?
C60c H60 0.9700 . ?
C60c H61 0.9700 . ?
C61c C62 1.442(16) . ?
C61c H62 0.9700 . ?
C61c H63 0.9700 . ?
C62c C63 1.437(17) . ?
C62c H64 0.9700 . ?
C62c H65 0.9700 . ?
C63c C64 1.421(12) . ?
C63c H66 0.9700 . ?
C63c H67 0.9700 . ?
C64c C65 1.445(14) . ?
C64c H68 0.9700 . ?
C64c H69 0.9700 . ?
C63Ad C73 1.16(3) . ?
C63Ad C64A 1.421(12) . ?
C63Ad H80 0.9700 . ?
C63Ad H81 0.9700 . ?
C64Ad C74 1.30(4) . ?
C64Ad H82 0.9700 . ?
C64Ad H83 0.9700 . ?
C65c C66 1.380(16) . ?
C65c H70 0.9700 . ?
C65c H71 0.9700 . ?
C66c C67 1.366(18) . ?
C66c H72 0.9700 . ?
C66c H73 0.9700 . ?
C67c C68 1.396(16) . ?
C67c H74 0.9700 . ?
C67c H75 0.9700 . ?
C68c C69 1.39(2) . ?
C68c H76 0.9700 . ?
C68c H77 0.9700 . ?
C67Ad C68A 1.396(16) . ?
C67Ad C75 1.48(2) . ?
C67Ad H84 0.9700 . ?
C67Ad H85 0.9700 . ?
C68Ad C76 1.31(4) . ?
C68Ad H86 0.9700 . ?
C68Ad H87 0.9700 . ?
C69c C70 1.38(2) . ?
C69c H78 0.9700 . ?
C69c H79 0.9700 . ?
C70c H103 0.9600 . ?
C70c H104 0.9600 . ?
C70c H105 0.9600 . ?
C71d C72 1.443(14) . ?
C71d H88 0.9700 . ?
C71d H89 0.9700 . ?
C72d C73 1.450(15) . ?
C72d H90 0.9700 . ?
C72d H91 0.9700 . ?
C73d H92 0.9700 . ?
C73d H93 0.9700 . ?
C74d C75 1.371(19) . ?
C74d H94 0.9700 . ?
C74d H95 0.9700 . ?
C75d H96 0.9700 . ?
C75d H97 0.9700 . ?
C76d C77 1.385(15) . ?
C76d H98 0.9700 . ?
C76d H99 0.9700 . ?
C77d H100 0.9600 . ?
C77d H101 0.9600 . ?
C77d H102 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
V1 V1 O1 162.2(3) 3_766 . ?
V1 V1 N3 88.2(8) 3_766 . ?
O1 V1 N3 107.6(9) . . ?
V1 V1 N2 77.3(4) 3_766 3_766 ?
O1 V1 N2 107.2(5) . 3_766 ?
V1 V1 N3 60.3(8) 3_766 3_766 ?
O1 V1 N3 103.7(8) . 3_766 ?
N3b V1 N3 148.4(3) . 3_766 ?
V1 V1 N4 86.7(4) 3_766 3_766 ?
O1 V1 N4 101.1(5) . 3_766 ?
N3b V1 N4 90.5(8) . 3_766 ?
N3b V1 N4 87.9(7) 3_766 3_766 ?
V1 V1 N2 72.2(4) 3_766 . ?
O1 V1 N2 102.0(5) . . ?
N2a V1 N2 149.4(2) 3_766 . ?
V1 V1 N1 95.9(8) 3_766 . ?
O1 V1 N1 100.7(8) . . ?
N2a V1 N1 96.1(7) 3_766 . ?
N2a V1 N1 87.1(7) . . ?
V1 V1 N4 65.0(4) 3_766 . ?
O1 V1 N4 106.1(5) . . ?
N3b V1 N4 88.7(7) . . ?
N3b V1 N4 78.4(6) 3_766 . ?
N4b V1 N4 151.7(2) 3_766 . ?
V1 V1 N1 58.0(6) 3_766 3_766 ?
O1 V1 N1 105.3(7) . 3_766 ?
N2a V1 N1 79.1(6) 3_766 3_766 ?
N2a V1 N1 84.7(6) . 3_766 ?
N1a V1 N1 153.9(2) . 3_766 ?
C1a N1a C4 104.5(14) . . ?
C1a N1a V1 127.2(16) . . ?
C4a N1a V1 127.0(14) . . ?
C1a N1a V1 129.0(16) . 3_766 ?
C4a N1a V1 122.9(12) . 3_766 ?
V1 N1a V1 26.1(2) . 3_766 ?
N1a C1a C2 110.3(18) . . ?
N1a C1a C10 109.6(19) . 3_766 ?
C2a C1a C10 140.1(17) . 3_766 ?
C3a C2a C1 106.6(15) . . ?
C3a C2a H20 126.7 . . ?
C1a C2a H20 126.7 . . ?
C2a C3a C4 109.9(16) . . ?
C2a C3a H21 125.0 . . ?
C4a C3a H21 125.0 . . ?
C5a C4a C3 126.9(16) . . ?
C5a C4a N1 124.4(15) . . ?
C3a C4a N1 108.7(13) . . ?
C4a C5a C6 126.0(15) . . ?
C4a C5a C11 118.8(13) . . ?
C6a C5a C11 115.2(14) . . ?
C5a C6a N2 124.4(12) . . ?
C5a C6a C9 126.2(13) . . ?
N2a C6a C9 109.3(11) . . ?
C6a N2a C7 105.7(11) . . ?
C6a N2a V1 134.9(10) . 3_766 ?
C7a N2a V1 113.0(9) . 3_766 ?
C6a N2a V1 127.2(8) . . ?
C7a N2a V1 126.6(9) . . ?
V1 N2a V1 30.6(2) 3_766 . ?
C10a C7a N2 126.3(15) . . ?
C10a C7a C8 124.8(16) . . ?
N2a C7a C8 108.4(10) . . ?
C9a C8a C7 107.4(12) . . ?
C9a C8a H22 126.3 . . ?
C7a C8a H22 126.3 . . ?
C8a C9a C6 108.6(12) . . ?
C8a C9a H23 125.7 . . ?
C6a C9a H23 125.7 . . ?
C7a C10a C54 121.4(18) . . ?
C7a C10a C1 139.2(19) . 3_766 ?
C54a C10a C1 99.3(16) . 3_766 ?
C41a C11a C12 122(3) . . ?
C41a C11a C5 119(2) . . ?
C12a C11a C5 119(2) . . ?
C13a C12a C11 114(4) . . ?
C13a C12a H48 123.2 . . ?
C11a C12a H48 123.2 . . ?
C12a C13a C43 127(4) . . ?
C12a C13a H49 116.5 . . ?
C43a C13a H49 116.5 . . ?
C44b C14b C15 124(3) . . ?
C44b C14b C17 120(2) . . ?
C15b C14b C17 114(3) . . ?
C14b C15b C16 110(3) . . ?
C14b C15b H50 125.1 . . ?
C16b C15b H50 125.1 . . ?
C40b C16b C15 127(3) . . ?
C40b C16b H51 116.7 . . ?
C15b C16b H51 116.7 . . ?
O2a C17 O3 128(2) . . ?
O4b C17 O5 124.8(18) . . ?
O4b C17 C14 122.3(18) . . ?
O5b C17 C14 112(2) . . ?
O2a C17 C43 117(2) . . ?
O3a C17 C43 115(2) . . ?
C17 O3a C18 115(3) . . ?
O3a C18a C19 110(3) . . ?
O3a C18a H28 109.7 . . ?
C19a C18a H28 109.7 . . ?
O3a C18a H29 109.7 . . ?
C19a C18a H29 109.7 . . ?
H28a C18a H29 108.2 . . ?
C20 C19a C18 108.8(13) . . ?
C20 C19a H36 109.9 . . ?
C18a C19a H36 109.9 . . ?
C20 C19a H37 109.9 . . ?
C18a C19a H37 109.9 . . ?
H36a C19a H37 108.3 . . ?
C46b C19Ab C20 116.3(13) . . ?
C46b C19Ab H38 108.2 . . ?
C20 C19Ab H38 108.2 . . ?
C46b C19Ab H39 108.2 . . ?
C20 C19Ab H39 108.2 . . ?
H38b C19Ab H39 107.4 . . ?
C19Ab C20 C21 115.6(8) . . ?
C19a C20 C21 115.6(8) . . ?
C19a C20 H30 108.4 . . ?
C21 C20 H30 108.4 . . ?
C19a C20 H31 108.4 . . ?
C21 C20 H31 108.4 . . ?
H30a C20 H31 107.4 . . ?
C19Ab C20 H32 108.4 . . ?
C21 C20 H32 108.4 . . ?
C19Ab C20 H33 108.4 . . ?
C21 C20 H33 108.4 . . ?
H32b C20 H33 107.4 . . ?
C22 C21 C20 119.9(9) . . ?
C22 C21 H1 107.3 . . ?
C20 C21 H1 107.3 . . ?
C22 C21 H2 107.3 . . ?
C20 C21 H2 107.3 . . ?
H1 C21 H2 106.9 . . ?
C21 C22 C23 121.0(9) . . ?
C21 C22 H3 107.1 . . ?
C23 C22 H3 107.1 . . ?
C21 C22 H4 107.1 . . ?
C23 C22 H4 107.1 . . ?
H3 C22 H4 106.8 . . ?
C24 C23 C22 122.7(10) . . ?
C24 C23 H5 106.7 . . ?
C22 C23 H5 106.7 . . ?
C24 C23 H6 106.7 . . ?
C22 C23 H6 106.7 . . ?
H5 C23 H6 106.6 . . ?
C23 C24 C25 124.0(10) . . ?
C23 C24 H7 106.3 . . ?
C25 C24 H7 106.3 . . ?
C23 C24 H8 106.3 . . ?
C25 C24 H8 106.3 . . ?
H7 C24 H8 106.4 . . ?
C24 C25 C26 121.4(10) . . ?
C24 C25 H9 107.0 . . ?
C26 C25 H9 107.0 . . ?
C24 C25 H10 107.0 . . ?
C26 C25 H10 107.0 . . ?
H9 C25 H10 106.7 . . ?
C27 C26 C25 124.8(11) . . ?
C27 C26 H11 106.1 . . ?
C25 C26 H11 106.1 . . ?
C27 C26 H12 106.1 . . ?
C25 C26 H12 106.1 . . ?
H11 C26 H12 106.3 . . ?
C28 C27 C26 125.3(11) . . ?
C28 C27 H13 106.0 . . ?
C26 C27 H13 106.0 . . ?
C28 C27 H14 106.0 . . ?
C26 C27 H14 106.0 . . ?
H13 C27 H14 106.3 . . ?
C29 C28 C27 125.5(12) . . ?
C29 C28 H15 106.0 . . ?
C27 C28 H15 106.0 . . ?
C29 C28 H16 106.0 . . ?
C27 C28 H16 106.0 . . ?
H15 C28 H16 106.3 . . ?
C28 C29 H17 109.5 . . ?
C28 C29 H18 109.5 . . ?
H17 C29 H18 109.5 . . ?
C28 C29 H19 109.5 . . ?
H17 C29 H19 109.5 . . ?
H18 C29 H19 109.5 . . ?
C33b N3b C30 105.2(13) . . ?
C33b N3b V1 128.5(16) . . ?
C30b N3b V1 118.5(15) . . ?
C33b N3b V1 127.3(11) . 3_766 ?
C30b N3b V1 126.9(14) . 3_766 ?
V1 N3b V1 31.6(3) . 3_766 ?
N3b C30b C39 137.9(18) . 3_766 ?
N3b C30b C31 110.3(17) . . ?
C39b C30b C31 111.7(17) 3_766 . ?
C32b C31b C30 106.3(15) . . ?
C32b C31b H24 126.8 . . ?
C30b C31b H24 126.8 . . ?
C31b C32b C33 107.4(16) . . ?
C31b C32b H25 126.3 . . ?
C33b C32b H25 126.3 . . ?
N3b C33b C34 125.6(13) . . ?
N3b C33b C32 110.5(13) . . ?
C34b C33b C32 123.7(15) . . ?
C35b C34b C33 123.7(14) . . ?
C35b C34b C40 119.6(13) . . ?
C33b C34b C40 116.5(14) . . ?
C34b C35b N4 127.1(14) . . ?
C34b C35b C38 126.3(14) . . ?
N4b C35b C38 106.4(11) . . ?
C36b N4b C35 108.6(14) . . ?
C36b N4b V1 125.7(10) . 3_766 ?
C35b N4b V1 124.9(11) . 3_766 ?
C36b N4b V1 131.5(11) . . ?
C35b N4b V1 115.5(9) . . ?
V1 N4b V1 28.3(2) 3_766 . ?
C39b C36b N4 125.6(16) . . ?
C39b C36b C37 127.9(14) . . ?
N4b C36b C37 106.3(13) . . ?
C38b C37b C36 107.8(14) . . ?
C38b C37b H26 126.1 . . ?
C36b C37b H26 126.1 . . ?
C37b C38b C35 110.7(14) . . ?
C37b C38b H27 124.7 . . ?
C35b C38b H27 124.7 . . ?
C36b C39b C30 113.8(16) . 3_766 ?
C36b C39b C47 114.1(15) . . ?
C30b C39b C47 132.1(16) 3_766 . ?
C45b C40b C16 114(2) . . ?
C45b C40b C34 122(2) . . ?
C16b C40b C34 123(2) . . ?
C42a C41a C11 115(4) . . ?
C42a C41a H52 122.5 . . ?
C11a C41a H52 122.5 . . ?
C41a C42a C43 128(4) . . ?
C41a C42a H53 116.1 . . ?
C43a C42a H53 116.1 . . ?
C42a C43a C13 112(3) . . ?
C42a C43a C17 126(4) . . ?
C13a C43a C17 120(3) . . ?
C14b C44b C45 117(3) . . ?
C14b C44b H54 121.5 . . ?
C45b C44b H54 121.5 . . ?
C40b C45b C44 127(3) . . ?
C40b C45b H55 116.6 . . ?
C44b C45b H55 116.6 . . ?
C17 O5b C46 113(2) . . ?
C19Ab C46b O5 112(2) . . ?
C19Ab C46b H34 109.1 . . ?
O5b C46b H34 109.1 . . ?
C19Ab C46b H35 109.1 . . ?
O5b C46b H35 109.1 . . ?
H34b C46b H35 107.9 . . ?
C52b C47b C48 128.4(16) . . ?
C52b C47b C39 119(2) . . ?
C48 C47b C39 113.0(17) . . ?
C56b C48 C47 114.9(11) . . ?
C49a C48 C54 126.7(14) . . ?
C49a C48 H40 116.6 . . ?
C54a C48 H40 116.6 . . ?
C56b C48 H41 122.6 . . ?
C47b C48 H41 122.6 . . ?
C50a C49a C48 111(2) . . ?
C50a C49a H42 124.5 . . ?
C48 C49a H42 124.5 . . ?
C55a C50a C49 122(2) . . ?
C55a C50a C53 133.1(16) . . ?
C49a C50a C53 105.1(17) . . ?
C52b C51b C57 117.9(17) . . ?
C52b C51b H43 121.1 . . ?
C57b C51b H43 121.1 . . ?
C47b C52b C51 117(2) . . ?
C47b C52b H44 121.4 . . ?
C51b C52b H44 121.4 . . ?
O6 C53 C57 130.0(9) . . ?
O6 C53 O7 122.7(7) . . ?
C57b C53 O7 107.3(8) . . ?
O6 C53 C50 119.8(8) . . ?
O7 C53 C50 117.5(8) . . ?
C53 O7 C59A 116.1(6) . . ?
C53 O7 C59 116.1(6) . . ?
C58a C54a C10 127(2) . . ?
C58a C54a C48 106.1(19) . . ?
C10a C54a C48 127.2(19) . . ?
C50a C55a C58 126(2) . . ?
C50a C55a H45 116.9 . . ?
C58a C55a H45 116.9 . . ?
C48 C56b C57 127.2(17) . . ?
C48 C56b H46 116.4 . . ?
C57b C56b H46 116.4 . . ?
C53 C57b C56 135.7(14) . . ?
C53 C57b C51 110.3(11) . . ?
C56b C57b C51 113.7(16) . . ?
C55a C58a C54 128(2) . . ?
C55a C58a H47 116.1 . . ?
C54a C58a H47 116.1 . . ?
O7 C59c C60 109.2(11) . . ?
O7 C59c H106 109.8 . . ?
C60c C59c H106 109.8 . . ?
O7 C59c H107 109.8 . . ?
C60c C59c H107 109.8 . . ?
H106c C59c H107 108.3 . . ?
O7 C59Ad C71 105.7(7) . . ?
O7 C59Ad H108 110.6 . . ?
C71d C59Ad H108 110.6 . . ?
O7 C59Ad H109 110.6 . . ?
C71d C59Ad H109 110.6 . . ?
H108d C59Ad H109 108.7 . . ?
C61c C60c C59 117(3) . . ?
C61c C60c H60 108.0 . . ?
C59c C60c H60 108.0 . . ?
C61c C60c H61 108.0 . . ?
C59c C60c H61 108.0 . . ?
H60c C60c H61 107.2 . . ?
C60c C61c C62 124(3) . . ?
C60c C61c H62 106.3 . . ?
C62c C61c H62 106.3 . . ?
C60c C61c H63 106.3 . . ?
C62c C61c H63 106.3 . . ?
H62c C61c H63 106.4 . . ?
C63c C62c C61 117(3) . . ?
C63c C62c H64 108.0 . . ?
C61c C62c H64 108.0 . . ?
C63c C62c H65 108.0 . . ?
C61c C62c H65 108.0 . . ?
H64c C62c H65 107.2 . . ?
C64c C63c C62 130(2) . . ?
C64c C63c H66 104.9 . . ?
C62c C63c H66 104.9 . . ?
C64c C63c H67 104.9 . . ?
C62c C63c H67 104.9 . . ?
H66c C63c H67 105.8 . . ?
C63c C64c C65 127.7(17) . . ?
C63c C64c H68 105.4 . . ?
C65c C64c H68 105.4 . . ?
C63c C64c H69 105.4 . . ?
C65c C64c H69 105.4 . . ?
H68c C64c H69 106.0 . . ?
C73d C63Ad C64A 144(3) . . ?
C73d C63Ad H80 101.0 . . ?
C64Ad C63Ad H80 101.0 . . ?
C73d C63Ad H81 101.0 . . ?
C64Ad C63Ad H81 101.0 . . ?
H80d C63Ad H81 104.4 . . ?
C74d C64Ad C63A 139(2) . . ?
C74d C64Ad H82 102.3 . . ?
C63Ad C64Ad H82 102.3 . . ?
C74d C64Ad H83 102.3 . . ?
C63Ad C64Ad H83 102.3 . . ?
H82d C64Ad H83 104.9 . . ?
C66c C65c C64 128(2) . . ?
C66c C65c H70 105.3 . . ?
C64c C65c H70 105.3 . . ?
C66c C65c H71 105.3 . . ?
C64c C65c H71 105.3 . . ?
H70c C65c H71 106.0 . . ?
C67c C66c C65 133(3) . . ?
C67c C66c H72 104.0 . . ?
C65c C66c H72 104.0 . . ?
C67c C66c H73 104.0 . . ?
C65c C66c H73 104.0 . . ?
H72c C66c H73 105.5 . . ?
C66c C67c C68 137(3) . . ?
C66c C67c H74 102.9 . . ?
C68c C67c H74 102.9 . . ?
C66c C67c H75 102.9 . . ?
C68c C67c H75 102.9 . . ?
H74c C67c H75 105.0 . . ?
C69c C68c C67 154(4) . . ?
C69c C68c H76 97.8 . . ?
C67c C68c H76 97.8 . . ?
C69c C68c H77 97.8 . . ?
C67c C68c H77 97.8 . . ?
H76c C68c H77 103.7 . . ?
C68Ad C67Ad C75 126(3) . . ?
C68Ad C67Ad H84 105.9 . . ?
C75d C67Ad H84 105.9 . . ?
C68Ad C67Ad H85 105.9 . . ?
C75d C67Ad H85 105.9 . . ?
H84d C67Ad H85 106.3 . . ?
C76d C68Ad C67A 131(4) . . ?
C76d C68Ad H86 104.6 . . ?
C67Ad C68Ad H86 104.6 . . ?
C76d C68Ad H87 104.6 . . ?
C67Ad C68Ad H87 104.6 . . ?
H86d C68Ad H87 105.7 . . ?
C70c C69c C68 122(7) . . ?
C70c C69c H78 106.8 . . ?
C68c C69c H78 106.8 . . ?
C70c C69c H79 106.8 . . ?
C68c C69c H79 106.8 . . ?
H78c C69c H79 106.7 . . ?
C69c C70c H103 109.5 . . ?
C69c C70c H104 109.5 . . ?
H103c C70c H104 109.5 . . ?
C69c C70c H105 109.5 . . ?
H103c C70c H105 109.5 . . ?
H104c C70c H105 109.5 . . ?
C72d C71d C59A 105.6(12) . . ?
C72d C71d H88 110.6 . . ?
C59Ad C71d H88 110.6 . . ?
C72d C71d H89 110.6 . . ?
C59Ad C71d H89 110.6 . . ?
H88d C71d H89 108.7 . . ?
C71d C72d C73 111(2) . . ?
C71d C72d H90 109.5 . . ?
C73d C72d H90 109.5 . . ?
C71d C72d H91 109.5 . . ?
C73d C72d H91 109.5 . . ?
H90d C72d H91 108.1 . . ?
C63Ad C73d C72 142(4) . . ?
C63Ad C73d H92 101.4 . . ?
C72d C73d H92 101.4 . . ?
C63Ad C73d H93 101.4 . . ?
C72d C73d H93 101.4 . . ?
H92d C73d H93 104.6 . . ?
C64Ad C74d C75 142(4) . . ?
C64Ad C74d H94 101.5 . . ?
C75d C74d H94 101.5 . . ?
C64Ad C74d H95 101.5 . . ?
C75d C74d H95 101.5 . . ?
H94d C74d H95 104.6 . . ?
C74d C75d C67A 124(3) . . ?
C74d C75d H96 106.3 . . ?
C67Ad C75d H96 106.3 . . ?
C74d C75d H97 106.3 . . ?
C67Ad C75d H97 106.3 . . ?
H96d C75d H97 106.4 . . ?
C68Ad C76d C77 127(3) . . ?
C68Ad C76d H98 105.5 . . ?
C77d C76d H98 105.5 . . ?
C68Ad C76d H99 105.5 . . ?
C77d C76d H99 105.5 . . ?
H98d C76d H99 106.1 . . ?
C76d C77d H100 109.5 . . ?
C76d C77d H101 109.5 . . ?
H100d C77d H101 109.5 . . ?
C76d C77d H102 109.5 . . ?
H100d C77d H102 109.5 . . ?
H101d C77d H102 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
C4a N1a C1a C2a 0(4) . . . . ?
V1 N1a C1a C2a -168(2) . . . . ?
V1 N1a C1a C2a 159(2) 3_766 . . . ?
C4a N1a C1a C10a 179(3) . . . 3_766 ?
V1 N1a C1a C10a 11(4) . . . 3_766 ?
V1 N1a C1a C10a -23(4) 3_766 . . 3_766 ?
N1a C1a C2a C3a 2(4) . . . . ?
C10a C1a C2a C3a -176(5) 3_766 . . . ?
C1a C2a C3a C4a -3(4) . . . . ?
C2a C3a C4a C5a -179(3) . . . . ?
C2a C3a C4a N1a 3(3) . . . . ?
C1a N1a C4a C5a 180(3) . . . . ?
V1 N1a C4a C5a -12(4) . . . . ?
V1 N1a C4a C5a 19(4) 3_766 . . . ?
C1a N1a C4a C3a -1(3) . . . . ?
V1 N1a C4a C3a 167(2) . . . . ?
V1 N1a C4a C3a -161.8(19) 3_766 . . . ?
C3a C4a C5a C6a 180(3) . . . . ?
N1a C4a C5a C6a -1(4) . . . . ?
C3a C4a C5a C11a -2(4) . . . . ?
N1a C4a C5a C11a 177(3) . . . . ?
C4a C5a C6a N2a 0(4) . . . . ?
C11a C5a C6a N2a -178.2(19) . . . . ?
C4a C5a C6a C9a -177(2) . . . . ?
C11a C5a C6a C9a 5(3) . . . . ?
C5a C6a N2a C7a -173(2) . . . . ?
C9a C6a N2a C7a 4(2) . . . . ?
C5a C6a N2a V1 -25(3) . . . 3_766 ?
C9a C6a N2a V1 152.8(14) . . . 3_766 ?
C5a C6a N2a V1 15(3) . . . . ?
C9a C6a N2a V1 -167.6(14) . . . . ?
C6a N2a C7a C10a 180(2) . . . . ?
V1 N2a C7a C10a 23(3) 3_766 . . . ?
V1 N2a C7a C10a -8(3) . . . . ?
C6a N2a C7a C8a -7(2) . . . . ?
V1 N2a C7a C8a -163.6(15) 3_766 . . . ?
V1 N2a C7a C8a 164.5(14) . . . . ?
C10a C7a C8a C9a -179(2) . . . . ?
N2a C7a C8a C9a 8(2) . . . . ?
C7a C8a C9a C6a -5(2) . . . . ?
C5a C6a C9a C8a 178(2) . . . . ?
N2a C6a C9a C8a 1(2) . . . . ?
N2a C7a C10a C54a 176(2) . . . . ?
C8a C7a C10a C54a 5(4) . . . . ?
N2a C7a C10a C1a 0(6) . . . 3_766 ?
C8a C7a C10a C1a -171(4) . . . 3_766 ?
C4a C5a C11a C41a 81(4) . . . . ?
C6a C5a C11a C41a -101(3) . . . . ?
C4a C5a C11a C12a -105(4) . . . . ?
C6a C5a C11a C12a 74(4) . . . . ?
C41a C11a C12a C13a -12(6) . . . . ?
C5a C11a C12a C13a 174(3) . . . . ?
C11a C12a C13a C43a 12(7) . . . . ?
C44b C14b C15b C16b 11(6) . . . . ?
C17 C14b C15b C16b 178(3) . . . . ?
C14b C15b C16b C40b -8(7) . . . . ?
C44b C14b C17 O4b -24(5) . . . . ?
C15b C14b C17 O4b 169(3) . . . . ?
C44b C14b C17 O5b 165(3) . . . . ?
C15b C14b C17 O5b -2(4) . . . . ?
O2a C17 O3a C18a -2(5) . . . . ?
C43a C17 O3a C18a -176(3) . . . . ?
C17 O3a C18a C19a 90(3) . . . . ?
O3a C18a C19a C20 176(2) . . . . ?
C46b C19Ab C20 C21 -168.6(14) . . . . ?
C18a C19a C20 C21 176.7(15) . . . . ?
C19Ab C20 C21 C22 -178.2(8) . . . . ?
C19a C20 C21 C22 -178.2(8) . . . . ?
C20 C21 C22 C23 -177.5(8) . . . . ?
C21 C22 C23 C24 -175.4(10) . . . . ?
C22 C23 C24 C25 -177.4(9) . . . . ?
C23 C24 C25 C26 -174.6(10) . . . . ?
C24 C25 C26 C27 175.3(10) . . . . ?
C25 C26 C27 C28 -176.2(11) . . . . ?
C26 C27 C28 C29 -175.7(11) . . . . ?
V1 V1 N3b C33b 101(2) 3_766 . . . ?
O1 V1 N3b C33b -71(2) . . . . ?
N3b V1 N3b C33b 101(2) 3_766 . . . ?
N4b V1 N3b C33b -173(2) 3_766 . . . ?
N4b V1 N3b C33b 36(2) . . . . ?
V1 V1 N3b C30b -115(2) 3_766 . . . ?
O1 V1 N3b C30b 73(2) . . . . ?
N3b V1 N3b C30b -115(2) 3_766 . . . ?
N4b V1 N3b C30b -28(2) 3_766 . . . ?
N4b V1 N3b C30b 180(2) . . . . ?
O1 V1 N3b V1 -171.5(4) . . . 3_766 ?
N3b V1 N3b V1 -0.002(1) 3_766 . . 3_766 ?
N4b V1 N3b V1 86.7(4) 3_766 . . 3_766 ?
N4b V1 N3b V1 -65.0(4) . . . 3_766 ?
C33b N3b C30b C39b 180(4) . . . 3_766 ?
V1 N3b C30b C39b 28(6) . . . 3_766 ?
V1 N3b C30b C39b -8(6) 3_766 . . 3_766 ?
C33b N3b C30b C31b 2(4) . . . . ?
V1 N3b C30b C31b -150(2) . . . . ?
V1 N3b C30b C31b 174(2) 3_766 . . . ?
N3b C30b C31b C32b -4(4) . . . . ?
C39b C30b C31b C32b 178(3) 3_766 . . . ?
C30b C31b C32b C33b 4(3) . . . . ?
C30b N3b C33b C34b -176(3) . . . . ?
V1 N3b C33b C34b -28(5) . . . . ?
V1 N3b C33b C34b 13(5) 3_766 . . . ?
C30b N3b C33b C32b 1(3) . . . . ?
V1 N3b C33b C32b 149(2) . . . . ?
V1 N3b C33b C32b -171(2) 3_766 . . . ?
C31b C32b C33b N3b -3(3) . . . . ?
C31b C32b C33b C34b 173(3) . . . . ?
N3b C33b C34b C35b -2(5) . . . . ?
C32b C33b C34b C35b -178(3) . . . . ?
N3b C33b C34b C40b -176(3) . . . . ?
C32b C33b C34b C40b 8(4) . . . . ?
C33b C34b C35b N4b 5(4) . . . . ?
C40b C34b C35b N4b 179(2) . . . . ?
C33b C34b C35b C38b 179(3) . . . . ?
C40b C34b C35b C38b -7(4) . . . . ?
C34b C35b N4b C36b 173(2) . . . . ?
C38b C35b N4b C36b -2(2) . . . . ?
C34b C35b N4b V1 -17(3) . . . 3_766 ?
C38b C35b N4b V1 167.6(13) . . . 3_766 ?
C34b C35b N4b V1 14(3) . . . . ?
C38b C35b N4b V1 -161.3(14) . . . . ?
C35b N4b C36b C39b 179(2) . . . . ?
V1 N4b C36b C39b 10(4) 3_766 . . . ?
V1 N4b C36b C39b -26(4) . . . . ?
C35b N4b C36b C37b 5(3) . . . . ?
V1 N4b C36b C37b -164.8(15) 3_766 . . . ?
V1 N4b C36b C37b 159.5(15) . . . . ?
C39b C36b C37b C38b 180(3) . . . . ?
N4b C36b C37b C38b -6(3) . . . . ?
C36b C37b C38b C35b 5(3) . . . . ?
C34b C35b C38b C37b -177(2) . . . . ?
N4b C35b C38b C37b -2(2) . . . . ?
N4b C36b C39b C30b 5(4) . . . 3_766 ?
C37b C36b C39b C30b 178(3) . . . 3_766 ?
N4b C36b C39b C47b -173(2) . . . . ?
C37b C36b C39b C47b 0(4) . . . . ?
C15b C16b C40b C45b -1(6) . . . . ?
C15b C16b C40b C34b -174(4) . . . . ?
C35b C34b C40b C45b 82(4) . . . . ?
C33b C34b C40b C45b -104(4) . . . . ?
C35b C34b C40b C16b -106(4) . . . . ?
C33b C34b C40b C16b 68(4) . . . . ?
C12a C11a C41a C42a -1(7) . . . . ?
C5a C11a C41a C42a 173(4) . . . . ?
C11a C41a C42a C43a 18(9) . . . . ?
C41a C42a C43a C13a -18(8) . . . . ?
C41a C42a C43a C17 177(5) . . . . ?
C12a C13a C43a C42a 1(7) . . . . ?
C12a C13a C43a C17 167(4) . . . . ?
O2a C17 C43a C42a 168(5) . . . . ?
O3a C17 C43a C42a -19(6) . . . . ?
O2a C17 C43a C13a 4(5) . . . . ?
O3a C17 C43a C13a 178(4) . . . . ?
C15b C14b C44b C45b -5(6) . . . . ?
C17 C14b C44b C45b -171(3) . . . . ?
C16b C40b C45b C44b 9(6) . . . . ?
C34b C40b C45b C44b -178(3) . . . . ?
C14b C44b C45b C40b -6(6) . . . . ?
O4b C17 O5b C46b -5(4) . . . . ?
C14b C17 O5b C46b 166(3) . . . . ?
C20 C19Ab C46b O5b -177.4(18) . . . . ?
C17 O5b C46b C19Ab 94(3) . . . . ?
C36b C39b C47b C52b -112(3) . . . . ?
C30b C39b C47b C52b 71(4) 3_766 . . . ?
C36b C39b C47b C48 69(3) . . . . ?
C30b C39b C47b C48 -109(3) 3_766 . . . ?
C52b C47b C48 C56b -7(3) . . . . ?
C39b C47b C48 C56b 172.7(18) . . . . ?
C54a C48 C49a C50a -8(3) . . . . ?
C48 C49a C50a C55a 8(3) . . . . ?
C48 C49a C50a C53 -173.2(13) . . . . ?
C48 C47b C52b C51b 1(4) . . . . ?
C39b C47b C52b C51b -178(2) . . . . ?
C57b C51b C52b C47b 1(3) . . . . ?
C55a C50a C53 O6 -9(2) . . . . ?
C49a C50a C53 O6 172.5(12) . . . . ?
C55a C50a C53 O7 170(2) . . . . ?
C49a C50a C53 O7 -8.8(14) . . . . ?
O6 C53 O7 C59Ad -0.6(8) . . . . ?
O6 C53 O7 C59c -0.6(8) . . . . ?
C7a C10a C54a C58a -103(3) . . . . ?
C1a C10a C54a C58a 75(4) 3_766 . . . ?
C7a C10a C54a C48 75(4) . . . . ?
C1a C10a C54a C48 -107(3) 3_766 . . . ?
C49a C48 C54a C58a 2(3) . . . . ?
C49a C48 C54a C10a -176(2) . . . . ?
C49a C50a C55a C58a -3(4) . . . . ?
C53 C50a C55a C58a 178(2) . . . . ?
C47b C48 C56b C57b 11(3) . . . . ?
O6 C53 C57b C56b 165.3(18) . . . . ?
O7 C53 C57b C56b -12(2) . . . . ?
O6 C53 C57b C51b -7.3(16) . . . . ?
O7 C53 C57b C51b 175.1(12) . . . . ?
C48 C56b C57b C53 178.9(15) . . . . ?
C48 C56b C57b C51b -9(3) . . . . ?
C52b C51b C57b C53 176.3(17) . . . . ?
C52b C51b C57b C56b 2(3) . . . . ?
C50a C55a C58a C54a -4(5) . . . . ?
C10a C54a C58a C55a -177(3) . . . . ?
C48 C54a C58a C55a 4(4) . . . . ?
C53 O7 C59c C60c 164.4(14) . . . . ?
C53 O7 C59Ad C71d -157.7(7) . . . . ?
O7 C59c C60c C61c 53(4) . . . . ?
C59c C60c C61c C62c -179(4) . . . . ?
C60c C61c C62c C63c -55(8) . . . . ?
C61c C62c C63c C64c -154(3) . . . . ?
C62c C63c C64c C65c 175(4) . . . . ?
C73d C63Ad C64Ad C74d 48(6) . . . . ?
C63c C64c C65c C66c 174(2) . . . . ?
C64c C65c C66c C67c 45(4) . . . . ?
C65c C66c C67c C68c 178(3) . . . . ?
C66c C67c C68c C69c 45(14) . . . . ?
C75d C67Ad C68Ad C76d 31(5) . . . . ?
C67c C68c C69c C70c 170(8) . . . . ?
O7 C59Ad C71d C72d -70.6(11) . . . . ?
C59Ad C71d C72d C73d -167(2) . . . . ?
C64Ad C63Ad C73d C72d 179(3) . . . . ?
C71d C72d C73d C63Ad 50(7) . . . . ?
C63Ad C64Ad C74d C75d -179(4) . . . . ?
C64Ad C74d C75d C67Ad -34(8) . . . . ?
C68Ad C67Ad C75d C74d 178(3) . . . . ?
C67Ad C68Ad C76d C77d 171(2) . . . . ?

_refine_diff_density_max         0.421
_refine_diff_density_min         -0.220
_refine_diff_density_rms         0.052


_symmetry_cell_setting           ?
_symmetry_space_group_name_H-M   ?
_diffrn_radiation_source         ?
_diffrn_radiation_monochromator  graphite
_chemical_absolute_configuration ?
####################################################################### 
# 
# 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_1m_153K
_database_code_depnum_ccdc_archive 'CCDC 2177818'
loop_
_audit_author_name
_audit_author_address
'Yoji Horii'
;Nara Womens University
Japan
;
_audit_update_record             
;
2022-06-08 deposited with the CCDC.	2022-10-04 downloaded from the CCDC.
;

_vrf_PLAT220_1m_153K             
;
PROBLEM: NonSolvent   Resd 1  C   Ueq(max)/Ueq(min) Range       10.0 Ratio
RESPONSE: This alert originates from the heavy disorders on alkyl chains. 
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C48 H62 N2 O4.50 V0.50'
_chemical_formula_weight         764.47

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                   15.6779(6)
_cell_length_b                   10.8485(3)
_cell_length_c                   26.9794(11)
_cell_angle_alpha                90
_cell_angle_beta                 104.186(4)
_cell_angle_gamma                90
_cell_volume                     4448.8(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    153

_cell_measurement_reflns_used    23967

_cell_measurement_theta_min      2.5830

_cell_measurement_theta_max      33.9040


_exptl_crystal_description       plate

_exptl_crystal_colour            red

_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.141
_exptl_crystal_F_000             1646
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.385

_exptl_crystal_size_mid          0.169

_exptl_crystal_size_min          0.058

_exptl_absorpt_coefficient_mu    0.169
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan

_exptl_absorpt_correction_T_min  0.82082

_exptl_absorpt_correction_T_max  1.00000

_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.67a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      153

_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_measurement_device_type  
'dtrek-CrysAlisPro-abstract goniometer imported rigaku-d*trek images'

_diffrn_measurement_method       'ω scans'

_diffrn_detector_area_resol_mean ?

_diffrn_reflns_number            50540
_diffrn_reflns_av_unetI/netI     0.0265
_diffrn_reflns_av_R_equivalents  0.0372
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_theta_min         2.290
_diffrn_reflns_theta_max         27.500
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measured_fraction_theta_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_point_group_measured_fraction_full 0.993
_reflns_number_total             10163
_reflns_number_gt                7698
_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       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_structure_solution    ?

_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Yadokari-XG 2009 (Wakita Nemoto et al., 2009)'

_computing_publication_material  
;Yadokari-XG 2009 (Wakita,Nemoto et al., 2009)
;

_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)+(0.2000P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    ?

_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         10163
_refine_ls_number_parameters     580
_refine_ls_number_restraints     114
_refine_ls_R_factor_all          0.1309
_refine_ls_R_factor_gt           0.1096
_refine_ls_wR_factor_ref         0.3485
_refine_ls_wR_factor_gt          0.3282
_refine_ls_goodness_of_fit_ref   1.395
_refine_ls_restrained_S_all      1.411
_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 0.96726(6) 1.02050(8) 0.49438(3) 0.0339(3) Uani 0.5 1 d . . P . .
O1 O 0.8740(3) 1.0821(4) 0.47245(15) 0.0424(9) Uani 0.5 1 d . . P . .
N1 N 0.94976(16) 0.9038(2) 0.54977(9) 0.0393(5) Uani 1 1 d . . . . .
N2 N 1.03215(16) 1.1367(2) 0.55078(9) 0.0392(5) Uani 1 1 d . . . . .
C1 C 0.9101(2) 0.7906(2) 0.54207(11) 0.0414(6) Uani 1 1 d . . . . .
C2 C 0.9451(2) 0.9402(2) 0.59757(11) 0.0417(6) Uani 1 1 d . . . . .
C3 C 1.01665(19) 1.1418(2) 0.59869(10) 0.0400(6) Uani 1 1 d . . . . .
C4 C 1.07322(19) 1.2453(2) 0.54504(10) 0.0398(6) Uani 1 1 d . . . . .
C5 C 0.8805(2) 0.7559(3) 0.58610(12) 0.0498(7) Uani 1 1 d . . . . .
H5 H 0.851734 0.683131 0.590388 0.060 Uiso 1 1 calc R U . . .
C6 C 0.9017(2) 0.8471(3) 0.61986(12) 0.0498(7) Uani 1 1 d . . . . .
H6 H 0.890450 0.849760 0.652109 0.060 Uiso 1 1 calc R U . . .
C7 C 1.0498(2) 1.2554(3) 0.62294(11) 0.0442(6) Uani 1 1 d . . . . .
H7 H 1.047725 1.280579 0.655581 0.053 Uiso 1 1 calc R U . . .
C8 C 1.0843(2) 1.3187(3) 0.58988(11) 0.0437(6) Uani 1 1 d . . . . .
H8 H 1.110458 1.396086 0.595233 0.052 Uiso 1 1 calc R U . . .
C9 C 0.89950(19) 0.7195(2) 0.49822(11) 0.0410(6) Uani 1 1 d . . . . .
C10 C 0.9763(2) 1.0512(3) 0.62103(11) 0.0426(6) Uani 1 1 d . . . . .
C11 C 0.85589(19) 0.5971(2) 0.49759(11) 0.0417(6) Uani 1 1 d . . . . .
C12 C 0.7734(2) 0.5764(3) 0.46665(14) 0.0561(8) Uani 1 1 d . . . . .
H12 H 0.745325 0.638340 0.444848 0.067 Uiso 1 1 calc R U . . .
C13 C 0.7320(2) 0.4646(3) 0.46765(15) 0.0592(9) Uani 1 1 d . . . . .
H13 H 0.675880 0.452069 0.446837 0.071 Uiso 1 1 calc R U . . .
C14 C 0.7733(2) 0.3708(3) 0.49945(13) 0.0475(7) Uani 1 1 d . . . . .
C15 C 0.8567(2) 0.3895(3) 0.52914(12) 0.0470(7) Uani 1 1 d . . . . .
H15 H 0.885621 0.326341 0.549899 0.056 Uiso 1 1 calc R U . . .
C16 C 0.8981(2) 0.5018(2) 0.52840(12) 0.0448(7) Uani 1 1 d . . . . .
H16 H 0.954607 0.513612 0.548726 0.054 Uiso 1 1 calc R U . . .
C17 C 0.9647(2) 1.0739(3) 0.67302(10) 0.0406(6) Uani 1 1 d . . . . .
C18 C 0.9062(2) 1.1615(3) 0.68152(11) 0.0454(7) Uani 1 1 d . . . . .
H18 H 0.873869 1.207557 0.654260 0.054 Uiso 1 1 calc R U . . .
C19 C 0.8951(2) 1.1817(3) 0.73041(11) 0.0472(7) Uani 1 1 d . . . . .
H19 H 0.856102 1.241746 0.735941 0.057 Uiso 1 1 calc R U . . .
C20 C 0.9419(2) 1.1124(3) 0.77048(11) 0.0444(7) Uani 1 1 d . . . . .
C21 C 1.0007(2) 1.0247(3) 0.76249(12) 0.0491(7) Uani 1 1 d . . . . .
H21 H 1.032194 0.978455 0.789939 0.059 Uiso 1 1 calc R U . . .
C22 C 1.0133(2) 1.0048(3) 0.71478(12) 0.0481(7) Uani 1 1 d . . . . .
H22 H 1.053726 0.946106 0.709864 0.058 Uiso 1 1 calc R U . . .
C23 C 0.7247(2) 0.2536(3) 0.49973(14) 0.0541(8) Uani 1 1 d . . . . .
O2 O 0.6549(2) 0.2323(3) 0.47199(12) 0.0862(10) Uani 1 1 d . . . . .
O3 O 0.76755(18) 0.1763(2) 0.53502(14) 0.0837(10) Uani 1 1 d . . . . .
C24 C 0.9294(2) 1.1255(3) 0.82325(11) 0.0468(7) Uani 1 1 d . . . . .
O4 O 0.96233(19) 1.0601(2) 0.85802(8) 0.0610(7) Uani 1 1 d . . . . .
O5 O 0.87499(18) 1.2176(2) 0.82636(9) 0.0634(7) Uani 1 1 d . . . . .
C25 C 0.7282(3) 0.0545(3) 0.5354(2) 0.0800(13) Uani 1 1 d . . . . .
H25A H 0.688385 0.038591 0.502321 0.096 Uiso 1 1 calc R U . . .
H25B H 0.774001 -0.007696 0.541205 0.096 Uiso 1 1 calc R U . . .
C26 C 0.6807(3) 0.0460(4) 0.5746(2) 0.0820(13) Uani 1 1 d . . . . .
H26A H 0.634873 0.108243 0.568379 0.098 Uiso 1 1 calc R U . . .
H26B H 0.720615 0.063703 0.607374 0.098 Uiso 1 1 calc R U . . .
C27 C 0.6391(3) -0.0791(4) 0.5773(2) 0.0753(11) Uani 1 1 d . . . . .
H27A H 0.596581 -0.093521 0.545039 0.090 Uiso 1 1 calc R U . . .
H27B H 0.684625 -0.141198 0.580526 0.090 Uiso 1 1 calc R U . . .
C28 C 0.5948(4) -0.0976(4) 0.6187(2) 0.0899(14) Uani 1 1 d . . . . .
H28A H 0.550300 -0.034147 0.616086 0.108 Uiso 1 1 calc R U . . .
H28B H 0.637638 -0.085791 0.651016 0.108 Uiso 1 1 calc R U . . .
C29 C 0.5519(3) -0.2202(4) 0.61992(18) 0.0755(11) Uani 1 1 d . . . . .
H29A H 0.509273 -0.231055 0.587442 0.091 Uiso 1 1 calc R U . . .
H29B H 0.596684 -0.282953 0.621830 0.091 Uiso 1 1 calc R U . . .
C30 C 0.5071(4) -0.2457(4) 0.6605(2) 0.1001(17) Uani 1 1 d . . . . .
H30A H 0.550868 -0.243986 0.692852 0.120 Uiso 1 1 calc R U . . .
H30B H 0.466470 -0.178528 0.660996 0.120 Uiso 1 1 calc R U . . .
C31 C 0.4588(3) -0.3596(5) 0.6581(2) 0.0896(14) Uani 1 1 d . . . . .
H31A H 0.498821 -0.425640 0.654926 0.107 Uiso 1 1 calc R U . . .
H31B H 0.413105 -0.358222 0.626449 0.107 Uiso 1 1 calc R U . . .
C32 C 0.4170(5) -0.3944(5) 0.6987(3) 0.109(2) Uani 1 1 d . . . . .
H32A H 0.463183 -0.407088 0.729559 0.131 Uiso 1 1 calc R U . . .
H32B H 0.382375 -0.324587 0.705000 0.131 Uiso 1 1 calc R U . . .
C33 C 0.3603(4) -0.5025(6) 0.6916(2) 0.0918(16) Uani 1 1 d . . . . .
H33A H 0.396717 -0.572636 0.688085 0.110 Uiso 1 1 calc R U . . .
H33B H 0.317989 -0.492534 0.658911 0.110 Uiso 1 1 calc R U . . .
C34 C 0.3097(4) -0.5377(4) 0.7293(2) 0.0848(14) Uani 1 1 d . . . . .
H34A H 0.352254 -0.551962 0.761525 0.102 Uiso 1 1 calc R U . . .
H34B H 0.275633 -0.466079 0.734137 0.102 Uiso 1 1 calc R U . . .
C35 C 0.2522(5) -0.6383(7) 0.7213(3) 0.128(3) Uani 1 1 d . . . . .
H35A H 0.285701 -0.709372 0.715177 0.154 Uiso 1 1 calc R U . . .
H35B H 0.208305 -0.622594 0.689694 0.154 Uiso 1 1 calc R U . . .
C36 C 0.2041(3) -0.6757(5) 0.7597(2) 0.0891(14) Uani 1 1 d . . . . .
H36A H 0.164814 -0.742271 0.746363 0.134 Uiso 1 1 calc R U . . .
H36B H 0.170960 -0.607019 0.767402 0.134 Uiso 1 1 calc R U . . .
H36C H 0.245393 -0.702229 0.790338 0.134 Uiso 1 1 calc R U . . .
C37 C 0.8554(3) 1.2339(4) 0.87603(15) 0.0737(11) Uani 0.365(2) 1 d . . P A 1
H37A H 0.906128 1.209136 0.902690 0.088 Uiso 0.365(2) 1 calc R U P A 1
H37B H 0.806569 1.181056 0.878151 0.088 Uiso 0.365(2) 1 calc R U P A 1
C37A C 0.8554(3) 1.2339(4) 0.87603(15) 0.0737(11) Uani 0.220(2) 1 d . . P A 2
H37C H 0.902948 1.277372 0.899263 0.088 Uiso 0.220(2) 1 calc R U P A 2
H37D H 0.847229 1.154754 0.890916 0.088 Uiso 0.220(2) 1 calc R U P A 2
C37B C 0.8554(3) 1.2339(4) 0.87603(15) 0.0737(11) Uani 0.416(2) 1 d . . P A 3
H37E H 0.902948 1.277372 0.899263 0.088 Uiso 0.416(2) 1 calc R U P A 3
H37F H 0.847229 1.154754 0.890916 0.088 Uiso 0.416(2) 1 calc R U P A 3
C38 C 0.8333(9) 1.3614(11) 0.8845(6) 0.078(3) Uani 0.365(2) 1 d . . P A 1
H38A H 0.806324 1.361632 0.913278 0.093 Uiso 0.365(2) 1 calc R U P A 1
H38B H 0.888228 1.406360 0.895248 0.093 Uiso 0.365(2) 1 calc R U P A 1
C39 C 0.7820(5) 1.4251(8) 0.8478(3) 0.126(2) Uani 0.365(2) 1 d . . P A 1
H39A H 0.763722 1.362955 0.821498 0.151 Uiso 0.365(2) 1 calc R U P A 1
H39B H 0.824201 1.475405 0.835996 0.151 Uiso 0.365(2) 1 calc R U P A 1
C39A C 0.7820(5) 1.4251(8) 0.8478(3) 0.126(2) Uani 0.220(2) 1 d . . P A 2
H39C H 0.759064 1.424831 0.810991 0.151 Uiso 0.220(2) 1 calc R U P A 2
H39D H 0.844663 1.441004 0.854588 0.151 Uiso 0.220(2) 1 calc R U P A 2
C39B C 0.7820(5) 1.4251(8) 0.8478(3) 0.126(2) Uani 0.416(2) 1 d . . P A 3
H39E H 0.759064 1.424831 0.810991 0.151 Uiso 0.416(2) 1 calc R U P A 3
H39F H 0.844663 1.441004 0.854588 0.151 Uiso 0.416(2) 1 calc R U P A 3
C40 C 0.7013(8) 1.5099(11) 0.8376(5) 0.061(3) Uani 0.365(2) 1 d . . P A 1
H40A H 0.714190 1.584762 0.821205 0.073 Uiso 0.365(2) 1 calc R U P A 1
H40B H 0.652383 1.469083 0.814397 0.073 Uiso 0.365(2) 1 calc R U P A 1
C41 C 0.6751(7) 1.5429(9) 0.8862(4) 0.049(2) Uani 0.365(2) 1 d . . P A 1
H41A H 0.649141 1.470714 0.897832 0.059 Uiso 0.365(2) 1 calc R U P A 1
H41B H 0.727976 1.563024 0.912156 0.059 Uiso 0.365(2) 1 calc R U P A 1
C42 C 0.6115(9) 1.6485(13) 0.8821(4) 0.057(3) Uani 0.365(2) 1 d . . P A 1
H42A H 0.636768 1.720985 0.870166 0.069 Uiso 0.365(2) 1 calc R U P A 1
H42B H 0.557806 1.628234 0.856819 0.069 Uiso 0.365(2) 1 calc R U P A 1
C43 C 0.5896(6) 1.6778(8) 0.9314(3) 0.0491(19) Uani 0.365(2) 1 d . . P A 1
H43A H 0.643645 1.685141 0.957996 0.059 Uiso 0.365(2) 1 calc R U P A 1
H43B H 0.555822 1.610355 0.940585 0.059 Uiso 0.365(2) 1 calc R U P A 1
C44 C 0.5378(6) 1.7952(8) 0.9291(3) 0.051(2) Uani 0.365(2) 1 d . . P A 1
H44A H 0.562150 1.856295 0.910242 0.062 Uiso 0.365(2) 1 calc R U P A 1
H44B H 0.477544 1.779704 0.910442 0.062 Uiso 0.365(2) 1 calc R U P A 1
C45 C 0.5375(4) 1.8447(6) 0.9785(2) 0.0783(17) Uani 0.365(2) 1 d . . P A 1
H45A H 0.597622 1.852552 0.998739 0.094 Uiso 0.365(2) 1 calc R U P A 1
H45B H 0.507039 1.788082 0.996113 0.094 Uiso 0.365(2) 1 calc R U P A 1
C46 C 0.4934(5) 1.9682(6) 0.9743(2) 0.0787(17) Uani 0.729(4) 1 d . . P . .
H46A H 0.430952 1.957849 0.959416 0.094 Uiso 0.729(4) 1 calc R U P A 1
H46B H 0.516928 2.020095 0.951521 0.094 Uiso 0.729(4) 1 calc R U P A 1
C47 C 0.5375(4) 1.8447(6) 0.9785(2) 0.0783(17) Uani 0.365(2) 1 d . . P A 4
H47A H 0.527526 1.807939 0.945240 0.117 Uiso 0.365(2) 1 calc R U P A 4
H47B H 0.599574 1.854613 0.992602 0.117 Uiso 0.365(2) 1 calc R U P A 4
H47C H 0.513622 1.792384 1.000495 0.117 Uiso 0.365(2) 1 calc R U P A 4
C48 C 0.7705(4) 1.3097(6) 0.8657(2) 0.0642(15) Uani 0.220(2) 1 d . . P A 2
H48A H 0.724878 1.267029 0.840842 0.077 Uiso 0.220(2) 1 calc R U P A 2
H48B H 0.751095 1.316983 0.897111 0.077 Uiso 0.220(2) 1 calc R U P A 2
C48A C 0.7705(4) 1.3097(6) 0.8657(2) 0.0642(15) Uani 0.416(2) 1 d . . P A 3
H48C H 0.724878 1.267029 0.840842 0.077 Uiso 0.416(2) 1 calc R U P A 3
H48D H 0.751095 1.316983 0.897111 0.077 Uiso 0.416(2) 1 calc R U P A 3
C49 C 0.7359(11) 1.5408(16) 0.8715(9) 0.214(9) Uani 0.220(2) 1 d D . P A 2
H49A H 0.734660 1.524106 0.906630 0.256 Uiso 0.220(2) 1 calc R U P A 2
H49B H 0.768238 1.616567 0.870481 0.256 Uiso 0.220(2) 1 calc R U P A 2
C50 C 0.6442(9) 1.5510(13) 0.8383(7) 0.173(6) Uani 0.220(2) 1 d D . P A 2
H50A H 0.612545 1.475000 0.840112 0.208 Uiso 0.220(2) 1 calc R U P A 2
H50B H 0.646561 1.563512 0.803066 0.208 Uiso 0.220(2) 1 calc R U P A 2
C51 C 0.5959(8) 1.6583(13) 0.8556(5) 0.120(4) Uani 0.220(2) 1 d D . P A 2
H51A H 0.587810 1.639862 0.889365 0.144 Uiso 0.220(2) 1 calc R U P A 2
H51B H 0.632612 1.731256 0.858623 0.144 Uiso 0.220(2) 1 calc R U P A 2
C52 C 0.5067(7) 1.6874(12) 0.8203(6) 0.159(5) Uani 0.220(2) 1 d D . P A 2
H52A H 0.471994 1.612622 0.817890 0.191 Uiso 0.220(2) 1 calc R U P A 2
H52B H 0.516713 1.701411 0.786700 0.191 Uiso 0.220(2) 1 calc R U P A 2
C53 C 0.4476(7) 1.7932(12) 0.8300(8) 0.194(8) Uani 0.220(2) 1 d D . P A 2
H53A H 0.481531 1.867178 0.828401 0.233 Uiso 0.220(2) 1 calc R U P A 2
H53B H 0.446578 1.784185 0.865631 0.233 Uiso 0.220(2) 1 calc R U P A 2
C54 C 0.3500(5) 1.8292(8) 0.8019(3) 0.092(2) Uani 0.220(2) 1 d D . P A 2
H54A H 0.340243 1.805667 0.766278 0.110 Uiso 0.220(2) 1 calc R U P A 2
H54B H 0.310494 1.780231 0.816513 0.110 Uiso 0.220(2) 1 calc R U P A 2
C55 C 0.3249(9) 1.9607(12) 0.8039(6) 0.39(2) Uani 0.220(2) 1 d D . P A 2
H55A H 0.324270 1.998176 0.771181 0.468 Uiso 0.220(2) 1 calc R U P A 2
H55B H 0.370192 2.001822 0.829550 0.468 Uiso 0.220(2) 1 calc R U P A 2
C56 C 0.2366(12) 1.985(2) 0.8159(7) 0.088(6) Uiso 0.220(2) 1 d D . P A 2
H56A H 0.191219 1.938443 0.792578 0.106 Uiso 0.220(2) 1 calc R U P A 2
H56B H 0.222268 2.072088 0.810799 0.106 Uiso 0.220(2) 1 calc R U P A 2
C57 C 0.2382(7) 1.9496(12) 0.8708(4) 0.029(2) Uiso 0.220(2) 1 d D . P A 2
H57A H 0.181799 1.966082 0.877313 0.044 Uiso 0.220(2) 1 calc R U P A 2
H57B H 0.251467 1.863425 0.875751 0.044 Uiso 0.220(2) 1 calc R U P A 2
H57C H 0.282480 1.996913 0.893950 0.044 Uiso 0.220(2) 1 calc R U P A 2
C49A C 0.7359(11) 1.5408(16) 0.8715(9) 0.214(9) Uani 0.416(2) 1 d . . P A 3
H49C H 0.734660 1.524106 0.906630 0.256 Uiso 0.416(2) 1 calc R U P A 3
H49D H 0.768238 1.616567 0.870481 0.256 Uiso 0.416(2) 1 calc R U P A 3
C50A C 0.6442(9) 1.5510(13) 0.8383(7) 0.173(6) Uani 0.416(2) 1 d . . P A 3
H50C H 0.612545 1.475000 0.840112 0.208 Uiso 0.416(2) 1 calc R U P A 3
H50D H 0.646561 1.563512 0.803066 0.208 Uiso 0.416(2) 1 calc R U P A 3
C51A C 0.5959(8) 1.6583(13) 0.8556(5) 0.120(4) Uani 0.416(2) 1 d D . P A 3
H51C H 0.587810 1.639862 0.889365 0.144 Uiso 0.416(2) 1 calc R U P A 3
H51D H 0.632612 1.731256 0.858623 0.144 Uiso 0.416(2) 1 calc R U P A 3
C52A C 0.5067(7) 1.6874(12) 0.8203(6) 0.159(5) Uani 0.416(2) 1 d D . P A 3
H52C H 0.471994 1.612622 0.817890 0.191 Uiso 0.416(2) 1 calc R U P A 3
H52D H 0.516713 1.701411 0.786700 0.191 Uiso 0.416(2) 1 calc R U P A 3
C53A C 0.4476(7) 1.7932(12) 0.8300(8) 0.194(8) Uani 0.416(2) 1 d D . P A 3
H53C H 0.481531 1.867178 0.828401 0.233 Uiso 0.416(2) 1 calc R U P A 3
H53D H 0.446578 1.784185 0.865631 0.233 Uiso 0.416(2) 1 calc R U P A 3
C54A C 0.3500(5) 1.8292(8) 0.8019(3) 0.092(2) Uani 0.416(2) 1 d D . P A 3
H54C H 0.340243 1.805667 0.766278 0.110 Uiso 0.416(2) 1 calc R U P A 3
H54D H 0.310494 1.780231 0.816513 0.110 Uiso 0.416(2) 1 calc R U P A 3
C55A C 0.3249(9) 1.9607(12) 0.8039(6) 0.39(2) Uani 0.416(2) 1 d D . P A 3
H55C H 0.266523 1.975477 0.782342 0.468 Uiso 0.416(2) 1 calc R U P A 3
H55D H 0.366488 2.013933 0.792938 0.468 Uiso 0.416(2) 1 calc R U P A 3
C58 C 0.3270(13) 1.984(3) 0.8617(9) 0.49(5) Uiso 0.416(2) 1 d D . P A 3
H58A H 0.355357 1.916617 0.883472 0.593 Uiso 0.416(2) 1 calc R U P A 3
H58B H 0.354947 2.061115 0.874148 0.593 Uiso 0.416(2) 1 calc R U P A 3
C59 C 0.2264(6) 1.9865(11) 0.8562(4) 0.065(3) Uiso 0.416(2) 1 d D . P A 3
H59A H 0.214902 2.000104 0.889141 0.097 Uiso 0.416(2) 1 calc R U P A 3
H59B H 0.200809 2.051912 0.833474 0.097 Uiso 0.416(2) 1 calc R U P A 3
H59C H 0.201213 1.909210 0.842682 0.097 Uiso 0.416(2) 1 calc R U P A 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 V1 1.0913(18) 3_776 ?
V1 O1 1.584(4) . ?
V1 N1 2.028(2) . ?
V1 N2 2.044(2) . ?
V1 N2 2.097(2) 3_776 ?
V1 N1 2.132(2) 3_776 ?
N1 C2 1.367(4) . ?
N1 C1 1.370(3) . ?
N2 C4 1.370(3) . ?
N2 C3 1.374(4) . ?
C1 C9 1.388(4) . ?
C1 C5 1.428(4) . ?
C2 C10 1.392(4) . ?
C2 C6 1.429(4) . ?
C3 C10 1.384(4) . ?
C3 C7 1.432(4) . ?
C4 C9 1.391(4) 3_776 ?
C4 C8 1.423(4) . ?
C5 C6 1.331(4) . ?
C5 H5 0.9300 . ?
C6 H6 0.9300 . ?
C7 C8 1.340(4) . ?
C7 H7 0.9300 . ?
C8 H8 0.9300 . ?
C9 C11 1.492(4) . ?
C10 C17 1.479(4) . ?
C11 C12 1.375(4) . ?
C11 C16 1.388(4) . ?
C12 C13 1.380(5) . ?
C12 H12 0.9300 . ?
C13 C14 1.385(5) . ?
C13 H13 0.9300 . ?
C14 C15 1.370(4) . ?
C14 C23 1.483(4) . ?
C15 C16 1.382(4) . ?
C15 H15 0.9300 . ?
C16 H16 0.9300 . ?
C17 C18 1.378(4) . ?
C17 C22 1.412(4) . ?
C18 C19 1.390(4) . ?
C18 H18 0.9300 . ?
C19 C20 1.372(4) . ?
C19 H19 0.9300 . ?
C20 C21 1.378(4) . ?
C20 C24 1.491(4) . ?
C21 C22 1.367(4) . ?
C21 H21 0.9300 . ?
C22 H22 0.9300 . ?
C23 O2 1.187(4) . ?
C23 O3 1.322(4) . ?
O3 C25 1.460(4) . ?
C24 O4 1.188(4) . ?
C24 O5 1.329(4) . ?
O5 C37B 1.457(4) . ?
O5 C37 1.457(4) . ?
O5 C37A 1.457(4) . ?
C25 C26 1.438(7) . ?
C25 H25A 0.9700 . ?
C25 H25B 0.9700 . ?
C26 C27 1.514(5) . ?
C26 H26A 0.9700 . ?
C26 H26B 0.9700 . ?
C27 C28 1.467(6) . ?
C27 H27A 0.9700 . ?
C27 H27B 0.9700 . ?
C28 C29 1.495(6) . ?
C28 H28A 0.9700 . ?
C28 H28B 0.9700 . ?
C29 C30 1.465(7) . ?
C29 H29A 0.9700 . ?
C29 H29B 0.9700 . ?
C30 C31 1.441(7) . ?
C30 H30A 0.9700 . ?
C30 H30B 0.9700 . ?
C31 C32 1.459(7) . ?
C31 H31A 0.9700 . ?
C31 H31B 0.9700 . ?
C32 C33 1.455(7) . ?
C32 H32A 0.9700 . ?
C32 H32B 0.9700 . ?
C33 C34 1.485(6) . ?
C33 H33A 0.9700 . ?
C33 H33B 0.9700 . ?
C34 C35 1.398(8) . ?
C34 H34A 0.9700 . ?
C34 H34B 0.9700 . ?
C35 C36 1.480(7) . ?
C35 H35A 0.9700 . ?
C35 H35B 0.9700 . ?
C36 H36A 0.9600 . ?
C36 H36B 0.9600 . ?
C36 H36C 0.9600 . ?
C37 C38 1.458(12) . ?
C37 H37A 0.9700 . ?
C37 H37B 0.9700 . ?
C37A C48 1.532(8) . ?
C37A H37C 0.9700 . ?
C37A H37D 0.9700 . ?
C37B C48A 1.532(8) . ?
C37B H37E 0.9700 . ?
C37B H37F 0.9700 . ?
C38 C39 1.310(16) . ?
C38 H38A 0.9700 . ?
C38 H38B 0.9700 . ?
C39 C40 1.533(14) . ?
C39 H39A 0.9700 . ?
C39 H39B 0.9700 . ?
C39A C48 1.370(11) . ?
C39A C49 1.65(2) . ?
C39A H39C 0.9700 . ?
C39A H39D 0.9700 . ?
C39B C48A 1.370(11) . ?
C39B C49A 1.65(2) . ?
C39B H39E 0.9700 . ?
C39B H39F 0.9700 . ?
C40 C41 1.509(13) . ?
C40 H40A 0.9700 . ?
C40 H40B 0.9700 . ?
C41 C42 1.504(14) . ?
C41 H41A 0.9700 . ?
C41 H41B 0.9700 . ?
C42 C43 1.489(13) . ?
C42 H42A 0.9700 . ?
C42 H42B 0.9700 . ?
C43 C44 1.503(12) . ?
C43 H43A 0.9700 . ?
C43 H43B 0.9700 . ?
C44 C45 1.438(10) . ?
C44 H44A 0.9700 . ?
C44 H44B 0.9700 . ?
C45 C46 1.499(8) . ?
C45 H45A 0.9700 . ?
C45 H45B 0.9700 . ?
C46 C47 1.499(8) . ?
C46 C46 1.517(12) 3_697 ?
C46 H46A 0.9700 . ?
C46 H46B 0.9700 . ?
C47 H47A 0.9600 . ?
C47 H47B 0.9600 . ?
C47 H47C 0.9600 . ?
C48 H48A 0.9700 . ?
C48 H48B 0.9700 . ?
C48A H48C 0.9700 . ?
C48A H48D 0.9700 . ?
C49 C50 1.499(14) . ?
C49 H49A 0.9700 . ?
C49 H49B 0.9700 . ?
C50 C51 1.524(12) . ?
C50 H50A 0.9700 . ?
C50 H50B 0.9700 . ?
C51 C52 1.519(10) . ?
C51 H51A 0.9700 . ?
C51 H51B 0.9700 . ?
C52 C53 1.537(10) . ?
C52 H52A 0.9700 . ?
C52 H52B 0.9700 . ?
C53 C54 1.581(10) . ?
C53 H53A 0.9700 . ?
C53 H53B 0.9700 . ?
C54 C55 1.485(11) . ?
C54 H54A 0.9700 . ?
C54 H54B 0.9700 . ?
C55 C56 1.520(14) . ?
C55 H55A 0.9700 . ?
C55 H55B 0.9700 . ?
C56 C57 1.526(14) . ?
C56 H56A 0.9700 . ?
C56 H56B 0.9700 . ?
C57 H57A 0.9600 . ?
C57 H57B 0.9600 . ?
C57 H57C 0.9600 . ?
C49A C50A 1.499(14) . ?
C49A H49C 0.9700 . ?
C49A H49D 0.9700 . ?
C50A C51A 1.524(12) . ?
C50A H50C 0.9700 . ?
C50A H50D 0.9700 . ?
C51A C52A 1.519(10) . ?
C51A H51C 0.9700 . ?
C51A H51D 0.9700 . ?
C52A C53A 1.537(10) . ?
C52A H52C 0.9700 . ?
C52A H52D 0.9700 . ?
C53A C54A 1.581(10) . ?
C53A H53C 0.9700 . ?
C53A H53D 0.9700 . ?
C54A C55A 1.485(11) . ?
C54A H54C 0.9700 . ?
C54A H54D 0.9700 . ?
C55A C58 1.571(16) . ?
C55A H55C 0.9700 . ?
C55A H55D 0.9700 . ?
C58 C59 1.548(16) . ?
C58 H58A 0.9700 . ?
C58 H58B 0.9700 . ?
C59 H59A 0.9600 . ?
C59 H59B 0.9600 . ?
C59 H59C 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
V1 V1 O1 174.11(18) 3_776 . ?
V1 V1 N1 80.15(11) 3_776 . ?
O1 V1 N1 105.04(16) . . ?
V1 V1 N2 77.41(11) 3_776 . ?
O1 V1 N2 105.27(16) . . ?
N1 V1 N2 88.22(10) . . ?
V1 V1 N2 72.07(11) 3_776 3_776 ?
O1 V1 N2 105.13(16) . 3_776 ?
N1 V1 N2 86.64(9) . 3_776 ?
N2 V1 N2 149.47(6) . 3_776 ?
V1 V1 N1 69.56(11) 3_776 3_776 ?
O1 V1 N1 105.22(16) . 3_776 ?
N1 V1 N1 149.71(6) . 3_776 ?
N2 V1 N1 85.29(10) . 3_776 ?
N2 V1 N1 84.16(9) 3_776 3_776 ?
C2 N1 C1 105.9(2) . . ?
C2 N1 V1 124.27(18) . . ?
C1 N1 V1 125.91(19) . . ?
C2 N1 V1 126.65(19) . 3_776 ?
C1 N1 V1 125.26(18) . 3_776 ?
V1 N1 V1 30.29(6) . 3_776 ?
C4 N2 C3 105.6(2) . . ?
C4 N2 V1 127.46(18) . . ?
C3 N2 V1 123.68(19) . . ?
C4 N2 V1 124.38(19) . 3_776 ?
C3 N2 V1 127.33(18) . 3_776 ?
V1 N2 V1 30.52(6) . 3_776 ?
N1 C1 C9 125.6(3) . . ?
N1 C1 C5 109.8(2) . . ?
C9 C1 C5 124.6(3) . . ?
N1 C2 C10 125.7(3) . . ?
N1 C2 C6 109.5(2) . . ?
C10 C2 C6 124.8(3) . . ?
N2 C3 C10 125.9(3) . . ?
N2 C3 C7 109.7(2) . . ?
C10 C3 C7 124.4(3) . . ?
N2 C4 C9 125.5(2) . 3_776 ?
N2 C4 C8 110.4(2) . . ?
C9 C4 C8 124.2(3) 3_776 . ?
C6 C5 C1 107.2(3) . . ?
C6 C5 H5 126.4 . . ?
C1 C5 H5 126.4 . . ?
C5 C6 C2 107.6(3) . . ?
C5 C6 H6 126.2 . . ?
C2 C6 H6 126.2 . . ?
C8 C7 C3 107.3(3) . . ?
C8 C7 H7 126.3 . . ?
C3 C7 H7 126.3 . . ?
C7 C8 C4 107.1(3) . . ?
C7 C8 H8 126.4 . . ?
C4 C8 H8 126.4 . . ?
C1 C9 C4 124.5(3) . 3_776 ?
C1 C9 C11 117.6(3) . . ?
C4 C9 C11 118.0(2) 3_776 . ?
C3 C10 C2 124.3(3) . . ?
C3 C10 C17 118.0(2) . . ?
C2 C10 C17 117.7(3) . . ?
C12 C11 C16 118.8(3) . . ?
C12 C11 C9 120.8(3) . . ?
C16 C11 C9 120.4(3) . . ?
C11 C12 C13 120.6(3) . . ?
C11 C12 H12 119.7 . . ?
C13 C12 H12 119.7 . . ?
C12 C13 C14 120.4(3) . . ?
C12 C13 H13 119.8 . . ?
C14 C13 H13 119.8 . . ?
C15 C14 C13 119.2(3) . . ?
C15 C14 C23 122.8(3) . . ?
C13 C14 C23 118.0(3) . . ?
C14 C15 C16 120.4(3) . . ?
C14 C15 H15 119.8 . . ?
C16 C15 H15 119.8 . . ?
C15 C16 C11 120.6(3) . . ?
C15 C16 H16 119.7 . . ?
C11 C16 H16 119.7 . . ?
C18 C17 C22 119.0(3) . . ?
C18 C17 C10 121.0(3) . . ?
C22 C17 C10 120.0(3) . . ?
C17 C18 C19 120.7(3) . . ?
C17 C18 H18 119.7 . . ?
C19 C18 H18 119.7 . . ?
C20 C19 C18 119.6(3) . . ?
C20 C19 H19 120.2 . . ?
C18 C19 H19 120.2 . . ?
C19 C20 C21 120.3(3) . . ?
C19 C20 C24 122.0(3) . . ?
C21 C20 C24 117.7(3) . . ?
C22 C21 C20 120.9(3) . . ?
C22 C21 H21 119.6 . . ?
C20 C21 H21 119.6 . . ?
C21 C22 C17 119.5(3) . . ?
C21 C22 H22 120.2 . . ?
C17 C22 H22 120.2 . . ?
O2 C23 O3 123.8(3) . . ?
O2 C23 C14 124.0(3) . . ?
O3 C23 C14 112.1(3) . . ?
C23 O3 C25 116.0(3) . . ?
O4 C24 O5 124.1(3) . . ?
O4 C24 C20 124.3(3) . . ?
O5 C24 C20 111.6(3) . . ?
C24 O5 C37B 115.6(3) . . ?
C24 O5 C37 115.6(3) . . ?
C24 O5 C37A 115.6(3) . . ?
C26 C25 O3 111.1(4) . . ?
C26 C25 H25A 109.4 . . ?
O3 C25 H25A 109.4 . . ?
C26 C25 H25B 109.4 . . ?
O3 C25 H25B 109.4 . . ?
H25A C25 H25B 108.0 . . ?
C25 C26 C27 113.5(4) . . ?
C25 C26 H26A 108.9 . . ?
C27 C26 H26A 108.9 . . ?
C25 C26 H26B 108.9 . . ?
C27 C26 H26B 108.9 . . ?
H26A C26 H26B 107.7 . . ?
C28 C27 C26 116.7(4) . . ?
C28 C27 H27A 108.1 . . ?
C26 C27 H27A 108.1 . . ?
C28 C27 H27B 108.1 . . ?
C26 C27 H27B 108.1 . . ?
H27A C27 H27B 107.3 . . ?
C27 C28 C29 116.0(4) . . ?
C27 C28 H28A 108.3 . . ?
C29 C28 H28A 108.3 . . ?
C27 C28 H28B 108.3 . . ?
C29 C28 H28B 108.3 . . ?
H28A C28 H28B 107.4 . . ?
C30 C29 C28 119.0(4) . . ?
C30 C29 H29A 107.6 . . ?
C28 C29 H29A 107.6 . . ?
C30 C29 H29B 107.6 . . ?
C28 C29 H29B 107.6 . . ?
H29A C29 H29B 107.0 . . ?
C31 C30 C29 118.1(5) . . ?
C31 C30 H30A 107.8 . . ?
C29 C30 H30A 107.8 . . ?
C31 C30 H30B 107.8 . . ?
C29 C30 H30B 107.8 . . ?
H30A C30 H30B 107.1 . . ?
C30 C31 C32 121.0(5) . . ?
C30 C31 H31A 107.1 . . ?
C32 C31 H31A 107.1 . . ?
C30 C31 H31B 107.1 . . ?
C32 C31 H31B 107.1 . . ?
H31A C31 H31B 106.8 . . ?
C33 C32 C31 118.8(5) . . ?
C33 C32 H32A 107.6 . . ?
C31 C32 H32A 107.6 . . ?
C33 C32 H32B 107.6 . . ?
C31 C32 H32B 107.6 . . ?
H32A C32 H32B 107.1 . . ?
C32 C33 C34 121.8(5) . . ?
C32 C33 H33A 106.9 . . ?
C34 C33 H33A 106.9 . . ?
C32 C33 H33B 106.9 . . ?
C34 C33 H33B 106.9 . . ?
H33A C33 H33B 106.7 . . ?
C35 C34 C33 121.8(5) . . ?
C35 C34 H34A 106.9 . . ?
C33 C34 H34A 106.9 . . ?
C35 C34 H34B 106.9 . . ?
C33 C34 H34B 106.9 . . ?
H34A C34 H34B 106.7 . . ?
C34 C35 C36 121.7(5) . . ?
C34 C35 H35A 106.9 . . ?
C36 C35 H35A 106.9 . . ?
C34 C35 H35B 106.9 . . ?
C36 C35 H35B 106.9 . . ?
H35A C35 H35B 106.7 . . ?
C35 C36 H36A 109.5 . . ?
C35 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C35 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
O5 C37 C38 111.9(6) . . ?
O5 C37 H37A 109.2 . . ?
C38 C37 H37A 109.2 . . ?
O5 C37 H37B 109.2 . . ?
C38 C37 H37B 109.2 . . ?
H37A C37 H37B 107.9 . . ?
O5 C37A C48 105.6(4) . . ?
O5 C37A H37C 110.6 . . ?
C48 C37A H37C 110.6 . . ?
O5 C37A H37D 110.6 . . ?
C48 C37A H37D 110.6 . . ?
H37C C37A H37D 108.8 . . ?
O5 C37B C48A 105.6(4) . . ?
O5 C37B H37E 110.6 . . ?
C48A C37B H37E 110.6 . . ?
O5 C37B H37F 110.6 . . ?
C48A C37B H37F 110.6 . . ?
H37E C37B H37F 108.8 . . ?
C39 C38 C37 120.5(11) . . ?
C39 C38 H38A 107.2 . . ?
C37 C38 H38A 107.2 . . ?
C39 C38 H38B 107.2 . . ?
C37 C38 H38B 107.2 . . ?
H38A C38 H38B 106.8 . . ?
C38 C39 C40 141.2(8) . . ?
C38 C39 H39A 101.7 . . ?
C40 C39 H39A 101.7 . . ?
C38 C39 H39B 101.7 . . ?
C40 C39 H39B 101.7 . . ?
H39A C39 H39B 104.7 . . ?
C48 C39A C49 116.7(9) . . ?
C48 C39A H39C 108.1 . . ?
C49 C39A H39C 108.1 . . ?
C48 C39A H39D 108.1 . . ?
C49 C39A H39D 108.1 . . ?
H39C C39A H39D 107.3 . . ?
C48A C39B C49A 116.7(9) . . ?
C48A C39B H39E 108.1 . . ?
C49A C39B H39E 108.1 . . ?
C48A C39B H39F 108.1 . . ?
C49A C39B H39F 108.1 . . ?
H39E C39B H39F 107.3 . . ?
C41 C40 C39 112.0(10) . . ?
C41 C40 H40A 109.2 . . ?
C39 C40 H40A 109.2 . . ?
C41 C40 H40B 109.2 . . ?
C39 C40 H40B 109.2 . . ?
H40A C40 H40B 107.9 . . ?
C42 C41 C40 115.7(10) . . ?
C42 C41 H41A 108.4 . . ?
C40 C41 H41A 108.4 . . ?
C42 C41 H41B 108.4 . . ?
C40 C41 H41B 108.4 . . ?
H41A C41 H41B 107.4 . . ?
C43 C42 C41 113.0(9) . . ?
C43 C42 H42A 109.0 . . ?
C41 C42 H42A 109.0 . . ?
C43 C42 H42B 109.0 . . ?
C41 C42 H42B 109.0 . . ?
H42A C42 H42B 107.8 . . ?
C42 C43 C44 112.7(8) . . ?
C42 C43 H43A 109.1 . . ?
C44 C43 H43A 109.1 . . ?
C42 C43 H43B 109.1 . . ?
C44 C43 H43B 109.1 . . ?
H43A C43 H43B 107.8 . . ?
C45 C44 C43 113.7(7) . . ?
C45 C44 H44A 108.8 . . ?
C43 C44 H44A 108.8 . . ?
C45 C44 H44B 108.8 . . ?
C43 C44 H44B 108.8 . . ?
H44A C44 H44B 107.7 . . ?
C44 C45 C46 111.7(6) . . ?
C44 C45 H45A 109.3 . . ?
C46 C45 H45A 109.3 . . ?
C44 C45 H45B 109.3 . . ?
C46 C45 H45B 109.3 . . ?
H45A C45 H45B 107.9 . . ?
C47 C46 C46 112.3(6) . 3_697 ?
C45 C46 C46 112.3(6) . 3_697 ?
C45 C46 H46A 109.1 . . ?
C46 C46 H46A 109.1 3_697 . ?
C45 C46 H46B 109.1 . . ?
C46 C46 H46B 109.1 3_697 . ?
H46A C46 H46B 107.9 . . ?
C46 C47 H47A 109.5 . . ?
C46 C47 H47B 109.5 . . ?
H47A C47 H47B 109.5 . . ?
C46 C47 H47C 109.5 . . ?
H47A C47 H47C 109.5 . . ?
H47B C47 H47C 109.5 . . ?
C39A C48 C37A 111.7(6) . . ?
C39A C48 H48A 109.3 . . ?
C37A C48 H48A 109.3 . . ?
C39A C48 H48B 109.3 . . ?
C37A C48 H48B 109.3 . . ?
H48A C48 H48B 107.9 . . ?
C39B C48A C37B 111.7(6) . . ?
C39B C48A H48C 109.3 . . ?
C37B C48A H48C 109.3 . . ?
C39B C48A H48D 109.3 . . ?
C37B C48A H48D 109.3 . . ?
H48C C48A H48D 107.9 . . ?
C50 C49 C39A 105.7(15) . . ?
C50 C49 H49A 110.6 . . ?
C39A C49 H49A 110.6 . . ?
C50 C49 H49B 110.6 . . ?
C39A C49 H49B 110.6 . . ?
H49A C49 H49B 108.7 . . ?
C49 C50 C51 110.4(13) . . ?
C49 C50 H50A 109.6 . . ?
C51 C50 H50A 109.6 . . ?
C49 C50 H50B 109.6 . . ?
C51 C50 H50B 109.6 . . ?
H50A C50 H50B 108.1 . . ?
C52 C51 C50 114.6(12) . . ?
C52 C51 H51A 108.6 . . ?
C50 C51 H51A 108.6 . . ?
C52 C51 H51B 108.6 . . ?
C50 C51 H51B 108.6 . . ?
H51A C51 H51B 107.6 . . ?
C51 C52 C53 123.3(12) . . ?
C51 C52 H52A 106.5 . . ?
C53 C52 H52A 106.5 . . ?
C51 C52 H52B 106.5 . . ?
C53 C52 H52B 106.5 . . ?
H52A C52 H52B 106.5 . . ?
C52 C53 C54 131.0(12) . . ?
C52 C53 H53A 104.5 . . ?
C54 C53 H53A 104.5 . . ?
C52 C53 H53B 104.5 . . ?
C54 C53 H53B 104.5 . . ?
H53A C53 H53B 105.7 . . ?
C55 C54 C53 117.0(9) . . ?
C55 C54 H54A 108.0 . . ?
C53 C54 H54A 108.0 . . ?
C55 C54 H54B 108.0 . . ?
C53 C54 H54B 108.0 . . ?
H54A C54 H54B 107.3 . . ?
C54 C55 C56 116.1(14) . . ?
C54 C55 H55A 108.3 . . ?
C56 C55 H55A 108.3 . . ?
C54 C55 H55B 108.3 . . ?
C56 C55 H55B 108.3 . . ?
H55A C55 H55B 107.4 . . ?
C55 C56 C57 111.3(13) . . ?
C55 C56 H56A 109.4 . . ?
C57 C56 H56A 109.4 . . ?
C55 C56 H56B 109.4 . . ?
C57 C56 H56B 109.4 . . ?
H56A C56 H56B 108.0 . . ?
C56 C57 H57A 109.5 . . ?
C56 C57 H57B 109.5 . . ?
H57A C57 H57B 109.5 . . ?
C56 C57 H57C 109.5 . . ?
H57A C57 H57C 109.5 . . ?
H57B C57 H57C 109.5 . . ?
C50A C49A C39B 105.7(15) . . ?
C50A C49A H49C 110.6 . . ?
C39B C49A H49C 110.6 . . ?
C50A C49A H49D 110.6 . . ?
C39B C49A H49D 110.6 . . ?
H49C C49A H49D 108.7 . . ?
C49A C50A C51A 110.4(13) . . ?
C49A C50A H50C 109.6 . . ?
C51A C50A H50C 109.6 . . ?
C49A C50A H50D 109.6 . . ?
C51A C50A H50D 109.6 . . ?
H50C C50A H50D 108.1 . . ?
C52A C51A C50A 114.6(12) . . ?
C52A C51A H51C 108.6 . . ?
C50A C51A H51C 108.6 . . ?
C52A C51A H51D 108.6 . . ?
C50A C51A H51D 108.6 . . ?
H51C C51A H51D 107.6 . . ?
C51A C52A C53A 123.3(12) . . ?
C51A C52A H52C 106.5 . . ?
C53A C52A H52C 106.5 . . ?
C51A C52A H52D 106.5 . . ?
C53A C52A H52D 106.5 . . ?
H52C C52A H52D 106.5 . . ?
C52A C53A C54A 131.0(12) . . ?
C52A C53A H53C 104.5 . . ?
C54A C53A H53C 104.5 . . ?
C52A C53A H53D 104.5 . . ?
C54A C53A H53D 104.5 . . ?
H53C C53A H53D 105.7 . . ?
C55A C54A C53A 117.0(9) . . ?
C55A C54A H54C 108.0 . . ?
C53A C54A H54C 108.0 . . ?
C55A C54A H54D 108.0 . . ?
C53A C54A H54D 108.0 . . ?
H54C C54A H54D 107.3 . . ?
C54A C55A C58 104.2(14) . . ?
C54A C55A H55C 110.9 . . ?
C58 C55A H55C 110.9 . . ?
C54A C55A H55D 110.9 . . ?
C58 C55A H55D 110.9 . . ?
H55C C55A H55D 108.9 . . ?
C59 C58 C55A 97.8(13) . . ?
C59 C58 H58A 112.2 . . ?
C55A C58 H58A 112.2 . . ?
C59 C58 H58B 112.2 . . ?
C55A C58 H58B 112.2 . . ?
H58A C58 H58B 109.8 . . ?
C58 C59 H59A 109.5 . . ?
C58 C59 H59B 109.5 . . ?
H59A C59 H59B 109.5 . . ?
C58 C59 H59C 109.5 . . ?
H59A C59 H59C 109.5 . . ?
H59B C59 H59C 109.5 . . ?

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
C2 N1 C1 C9 179.6(3) . . . . ?
V1 N1 C1 C9 21.2(4) . . . . ?
V1 N1 C1 C9 -16.3(4) 3_776 . . . ?
C2 N1 C1 C5 -0.2(3) . . . . ?
V1 N1 C1 C5 -158.6(2) . . . . ?
V1 N1 C1 C5 163.9(2) 3_776 . . . ?
C1 N1 C2 C10 -179.0(3) . . . . ?
V1 N1 C2 C10 -20.1(4) . . . . ?
V1 N1 C2 C10 17.2(4) 3_776 . . . ?
C1 N1 C2 C6 0.2(3) . . . . ?
V1 N1 C2 C6 159.0(2) . . . . ?
V1 N1 C2 C6 -163.7(2) 3_776 . . . ?
C4 N2 C3 C10 -179.9(3) . . . . ?
V1 N2 C3 C10 19.3(4) . . . . ?
V1 N2 C3 C10 -18.1(4) 3_776 . . . ?
C4 N2 C3 C7 -0.6(3) . . . . ?
V1 N2 C3 C7 -161.4(2) . . . . ?
V1 N2 C3 C7 161.1(2) 3_776 . . . ?
C3 N2 C4 C9 -179.4(3) . . . 3_776 ?
V1 N2 C4 C9 -19.5(4) . . . 3_776 ?
V1 N2 C4 C9 18.2(4) 3_776 . . 3_776 ?
C3 N2 C4 C8 0.5(3) . . . . ?
V1 N2 C4 C8 160.3(2) . . . . ?
V1 N2 C4 C8 -161.9(2) 3_776 . . . ?
N1 C1 C5 C6 0.2(4) . . . . ?
C9 C1 C5 C6 -179.6(3) . . . . ?
C1 C5 C6 C2 -0.1(4) . . . . ?
N1 C2 C6 C5 0.0(4) . . . . ?
C10 C2 C6 C5 179.1(3) . . . . ?
N2 C3 C7 C8 0.5(3) . . . . ?
C10 C3 C7 C8 179.8(3) . . . . ?
C3 C7 C8 C4 -0.2(3) . . . . ?
N2 C4 C8 C7 -0.2(3) . . . . ?
C9 C4 C8 C7 179.7(3) 3_776 . . . ?
N1 C1 C9 C4 -1.1(5) . . . 3_776 ?
C5 C1 C9 C4 178.6(3) . . . 3_776 ?
N1 C1 C9 C11 178.8(3) . . . . ?
C5 C1 C9 C11 -1.4(4) . . . . ?
N2 C3 C10 C2 0.0(5) . . . . ?
C7 C3 C10 C2 -179.2(3) . . . . ?
N2 C3 C10 C17 -179.5(3) . . . . ?
C7 C3 C10 C17 1.3(5) . . . . ?
N1 C2 C10 C3 0.3(5) . . . . ?
C6 C2 C10 C3 -178.7(3) . . . . ?
N1 C2 C10 C17 179.7(3) . . . . ?
C6 C2 C10 C17 0.8(5) . . . . ?
C1 C9 C11 C12 110.7(4) . . . . ?
C4 C9 C11 C12 -69.3(4) 3_776 . . . ?
C1 C9 C11 C16 -69.2(4) . . . . ?
C4 C9 C11 C16 110.8(3) 3_776 . . . ?
C16 C11 C12 C13 2.5(5) . . . . ?
C9 C11 C12 C13 -177.5(3) . . . . ?
C11 C12 C13 C14 -0.8(6) . . . . ?
C12 C13 C14 C15 -1.4(6) . . . . ?
C12 C13 C14 C23 178.7(3) . . . . ?
C13 C14 C15 C16 1.8(5) . . . . ?
C23 C14 C15 C16 -178.2(3) . . . . ?
C14 C15 C16 C11 -0.1(5) . . . . ?
C12 C11 C16 C15 -2.0(5) . . . . ?
C9 C11 C16 C15 177.9(3) . . . . ?
C3 C10 C17 C18 69.5(4) . . . . ?
C2 C10 C17 C18 -110.0(3) . . . . ?
C3 C10 C17 C22 -111.0(3) . . . . ?
C2 C10 C17 C22 69.5(4) . . . . ?
C22 C17 C18 C19 0.0(5) . . . . ?
C10 C17 C18 C19 179.4(3) . . . . ?
C17 C18 C19 C20 -0.9(5) . . . . ?
C18 C19 C20 C21 1.0(5) . . . . ?
C18 C19 C20 C24 -176.8(3) . . . . ?
C19 C20 C21 C22 -0.2(5) . . . . ?
C24 C20 C21 C22 177.8(3) . . . . ?
C20 C21 C22 C17 -0.8(5) . . . . ?
C18 C17 C22 C21 0.9(5) . . . . ?
C10 C17 C22 C21 -178.6(3) . . . . ?
C15 C14 C23 O2 -174.9(4) . . . . ?
C13 C14 C23 O2 5.1(6) . . . . ?
C15 C14 C23 O3 6.1(5) . . . . ?
C13 C14 C23 O3 -173.9(3) . . . . ?
O2 C23 O3 C25 5.8(6) . . . . ?
C14 C23 O3 C25 -175.2(3) . . . . ?
C19 C20 C24 O4 172.8(3) . . . . ?
C21 C20 C24 O4 -5.1(5) . . . . ?
C19 C20 C24 O5 -5.7(4) . . . . ?
C21 C20 C24 O5 176.4(3) . . . . ?
O4 C24 O5 C37B -1.2(5) . . . . ?
C20 C24 O5 C37B 177.3(3) . . . . ?
O4 C24 O5 C37 -1.2(5) . . . . ?
C20 C24 O5 C37 177.3(3) . . . . ?
O4 C24 O5 C37A -1.2(5) . . . . ?
C20 C24 O5 C37A 177.3(3) . . . . ?
C23 O3 C25 C26 -100.3(5) . . . . ?
O3 C25 C26 C27 -179.3(4) . . . . ?
C25 C26 C27 C28 175.8(4) . . . . ?
C26 C27 C28 C29 178.3(4) . . . . ?
C27 C28 C29 C30 179.5(5) . . . . ?
C28 C29 C30 C31 174.0(5) . . . . ?
C29 C30 C31 C32 176.3(5) . . . . ?
C30 C31 C32 C33 172.7(6) . . . . ?
C31 C32 C33 C34 -174.9(5) . . . . ?
C32 C33 C34 C35 177.0(6) . . . . ?
C33 C34 C35 C36 177.9(6) . . . . ?
C24 O5 C37 C38 152.6(7) . . . . ?
C24 O5 C37A C48 -160.5(4) . . . . ?
C24 O5 C37B C48A -160.5(4) . . . . ?
O5 C37 C38 C39 42.3(11) . . . . ?
C37 C38 C39 C40 132.3(13) . . . . ?
C38 C39 C40 C41 8(2) . . . . ?
C39 C40 C41 C42 165.8(10) . . . . ?
C40 C41 C42 C43 -179.0(10) . . . . ?
C41 C42 C43 C44 170.9(10) . . . . ?
C42 C43 C44 C45 -162.9(9) . . . . ?
C43 C44 C45 C46 173.8(7) . . . . ?
C44 C45 C46 C46 -169.9(9) . . . 3_697 ?
C49 C39A C48 C37A -137.7(9) . . . . ?
O5 C37A C48 C39A -64.3(6) . . . . ?
C49A C39B C48A C37B -137.7(9) . . . . ?
O5 C37B C48A C39B -64.3(6) . . . . ?
C48 C39A C49 C50 -87.8(16) . . . . ?
C39A C49 C50 C51 -178.2(12) . . . . ?
C49 C50 C51 C52 172.3(16) . . . . ?
C50 C51 C52 C53 -178.9(15) . . . . ?
C51 C52 C53 C54 -172.5(15) . . . . ?
C52 C53 C54 C55 -153.6(17) . . . . ?
C53 C54 C55 C56 -135.1(15) . . . . ?
C54 C55 C56 C57 68(2) . . . . ?
C48A C39B C49A C50A -87.8(16) . . . . ?
C39B C49A C50A C51A -178.2(12) . . . . ?
C49A C50A C51A C52A 172.3(16) . . . . ?
C50A C51A C52A C53A -178.9(15) . . . . ?
C51A C52A C53A C54A -172.5(15) . . . . ?
C52A C53A C54A C55A -153.6(17) . . . . ?
C53A C54A C55A C58 -67.4(15) . . . . ?
C54A C55A C58 C59 -105.5(16) . . . . ?

_refine_diff_density_max         1.347
_refine_diff_density_min         -0.503
_refine_diff_density_rms         0.098


_symmetry_cell_setting           ?
_symmetry_space_group_name_H-M   ?
_diffrn_radiation_source         ?
_diffrn_radiation_monochromator  graphite
_chemical_absolute_configuration ?
####################################################################### 
# 
# 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_1s_283K
_database_code_depnum_ccdc_archive 'CCDC 2177815'
loop_
_audit_author_name
_audit_author_address
'Yoji Horii'
;Nara Womens University
Japan
;
_audit_update_record             
;
2022-06-08 deposited with the CCDC.	2022-10-04 downloaded from the CCDC.
;

_vrf_PLAT026_1s_283K             
;
PROBLEM: Ratio Observed / Unique Reflections (too) Low ..        38% Check 
RESPONSE: This alert originates from low crystallinity of the sample. 
;
_vrf_PLAT084_1s_283K             
;
PROBLEM: High wR2 Value (i.e. > 0.25) ...................       0.36 Report
RESPONSE: This alert originates from thermal motion of dodecyl chains. 
;
_vrf_PLAT149_1s_283K             
;
PROBLEM: s.u. on the   beta    Angle is Too Large .......       0.06 Degree
RESPONSE: This alert originates from low crystallinity of the sample. 
;
_vrf_PLAT220_1s_283K             
;
PROBLEM: NonSolvent   Resd 1  C   Ueq(max)/Ueq(min) Range        9.7 Ratio
RESPONSE: This alert originates from thermal motion of dodecyl chains. 
;
_vrf_PLAT241_1s_283K             
;
PROBLEM: High   'MainMol' Ueq as Compared to Neighbors of        C26 Check
PROBLEM: High   'MainMol' Ueq as Compared to Neighbors of        C46 Check
PROBLEM: High   'MainMol' Ueq as Compared to Neighbors of        C47 Check
RESPONSE: This alert originates from thermal motion of dodecyl chains. 
;
_vrf_PLAT242_1s_283K             
;
PROBLEM: Low    'MainMol' Ueq as Compared to Neighbors of        C34 Check
PROBLEM: Low    'MainMol' Ueq as Compared to Neighbors of        C45 Check
RESPONSE: This alert originates from thermal motion of dodecyl chains. 
;
_vrf_PLAT341_1s_283K             
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............    0.02567 Ang.
RESPONSE: This alert originates from thermal motion of dodecyl chains. 
;
_vrf_PLAT410_1s_283K             
;
PROBLEM: Short Intra H...H Contact  H44      ..H45      .       1.87 Ang.  
                                                      x,y,z  =      1_555 Check
RESPONSE: This alert originates from thermal motion of dodecyl chains. 
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C48 H62 N2 O4.50 V0.50'
_chemical_formula_weight         764.46

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                   47.906(15)
_cell_length_b                   10.8092(7)
_cell_length_c                   27.354(8)
_cell_angle_alpha                90
_cell_angle_beta                 140.90(6)
_cell_angle_gamma                90
_cell_volume                     8933(9)
_cell_formula_units_Z            8
_cell_measurement_temperature    283

_cell_measurement_reflns_used    7792

_cell_measurement_theta_min      1.9010

_cell_measurement_theta_max      31.8860


_exptl_crystal_description       prism

_exptl_crystal_colour            red

_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.137
_exptl_crystal_F_000             3292
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.132

_exptl_crystal_size_mid          0.079

_exptl_crystal_size_min          0.010

_exptl_absorpt_coefficient_mu    0.168
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan

_exptl_absorpt_correction_T_min  0.77961

_exptl_absorpt_correction_T_max  1.00000

_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      283

_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_measurement_device_type  
'dtrek-CrysAlisPro-abstract goniometer imported rigaku-d*trek images'

_diffrn_measurement_method       'ω scans'

_diffrn_detector_area_resol_mean ?

_diffrn_reflns_number            48327
_diffrn_reflns_av_unetI/netI     0.1285
_diffrn_reflns_av_R_equivalents  0.1106
_diffrn_reflns_limit_h_min       -62
_diffrn_reflns_limit_h_max       62
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_theta_min         1.721
_diffrn_reflns_theta_max         27.499
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             10254
_reflns_number_gt                3898
_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       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_structure_solution    ?

_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Yadokari-XG 2009 (Wakita Nemoto et al., 2009)'

_computing_publication_material  
;Yadokari-XG 2009 (Wakita,Nemoto et al., 2009)
;

_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)+(0.1265P)²+13.8881P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    ?

_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         10254
_refine_ls_number_parameters     544
_refine_ls_number_restraints     226
_refine_ls_R_factor_all          0.2515
_refine_ls_R_factor_gt           0.1117
_refine_ls_wR_factor_ref         0.3569
_refine_ls_wR_factor_gt          0.2700
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_restrained_S_all      1.022
_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 0.26597(5) 0.22834(15) 0.52309(10) 0.0610(5) Uani 0.5 1 d . . P . .
N1 N 0.27502(14) 0.3452(3) 0.4773(2) 0.0661(11) Uani 1 1 d . . . . .
N2 N 0.23242(14) 0.1122(3) 0.4308(2) 0.0664(11) Uani 1 1 d . . . . .
C1 C 0.29519(18) 0.4600(4) 0.5062(3) 0.0678(13) Uani 1 1 d . . . . .
C2 C 0.3103(2) 0.4921(5) 0.4785(3) 0.0846(17) Uani 1 1 d . . . . .
H2 H 0.325318 0.563847 0.490244 0.101 Uiso 1 1 calc R U . . .
C3 C 0.2987(2) 0.3994(4) 0.4326(3) 0.0805(16) Uani 1 1 d . . . . .
H3 H 0.304063 0.395902 0.406437 0.097 Uiso 1 1 calc R U . . .
C4 C 0.27675(18) 0.3077(4) 0.4312(3) 0.0679(13) Uani 1 1 d . . . . .
C5 C 0.23962(17) 0.1047(4) 0.3902(3) 0.0637(13) Uani 1 1 d . . . . .
O1 O 0.3131(2) 0.1642(6) 0.5952(4) 0.0708(18) Uani 0.5 1 d . . P . .
C6 C 0.22257(18) -0.0085(4) 0.3489(3) 0.0712(14) Uani 1 1 d . . . . .
H6 H 0.223196 -0.034771 0.317376 0.085 Uiso 1 1 calc R U . . .
C7 C 0.20535(17) -0.0711(5) 0.3633(3) 0.0711(14) Uani 1 1 d . . . . .
H7 H 0.192025 -0.148617 0.343851 0.085 Uiso 1 1 calc R U . . .
C8 C 0.21120(16) 0.0025(4) 0.4138(3) 0.0637(13) Uani 1 1 d . . . . .
C9 C 0.30180(17) 0.5324(4) 0.5565(3) 0.0652(13) Uani 1 1 d . . . . .
C10 C 0.26052(17) 0.1963(4) 0.3907(3) 0.0652(13) Uani 1 1 d . . . . .
C11 C 0.32301(18) 0.6555(4) 0.5790(3) 0.0646(13) Uani 1 1 d . . . . .
C12 C 0.3644(2) 0.6788(5) 0.6545(4) 0.0939(18) Uani 1 1 d . . . . .
H12 H 0.378820 0.617887 0.692032 0.113 Uiso 1 1 calc R U . . .
C13 C 0.3850(2) 0.7938(6) 0.6750(4) 0.102(2) Uani 1 1 d . . . . .
H13 H 0.413217 0.808086 0.725710 0.122 Uiso 1 1 calc R U . . .
C14 C 0.3639(2) 0.8836(5) 0.6212(4) 0.0850(16) Uani 1 1 d . . . . .
C15 C 0.3224(2) 0.8625(5) 0.5454(3) 0.0829(16) Uani 1 1 d . . . . .
H15 H 0.308182 0.923553 0.508013 0.099 Uiso 1 1 calc R U . . .
C16 C 0.30217(18) 0.7500(4) 0.5259(3) 0.0751(15) Uani 1 1 d . . . . .
H16 H 0.273619 0.737471 0.475411 0.090 Uiso 1 1 calc R U . . .
C17 C 0.26661(17) 0.1719(4) 0.3456(3) 0.0661(13) Uani 1 1 d . . . . .
C18 C 0.29567(18) 0.0811(5) 0.3690(3) 0.0713(14) Uani 1 1 d . . . . .
H18 H 0.310618 0.032790 0.412073 0.086 Uiso 1 1 calc R U . . .
C19 C 0.30268(18) 0.0616(4) 0.3297(3) 0.0725(14) Uani 1 1 d . . . . .
H19 H 0.322423 0.000380 0.346813 0.087 Uiso 1 1 calc R U . . .
C20 C 0.28107(18) 0.1309(5) 0.2652(3) 0.0696(14) Uani 1 1 d . . . . .
C21 C 0.2508(2) 0.2219(5) 0.2408(3) 0.0854(16) Uani 1 1 d . . . . .
H21 H 0.235253 0.269093 0.196957 0.103 Uiso 1 1 calc R U . . .
C22 C 0.24435(19) 0.2410(5) 0.2809(3) 0.0814(16) Uani 1 1 d . . . . .
H22 H 0.224567 0.301645 0.264157 0.098 Uiso 1 1 calc R U . . .
C23 C 0.3876(3) 1.0037(6) 0.6450(5) 0.107(2) Uani 1 1 d . . . . .
O2 O 0.4200(2) 1.0336(5) 0.7116(3) 0.161(2) Uani 1 1 d . . . . .
O3 O 0.37039(16) 1.0722(4) 0.5861(3) 0.1222(16) Uani 1 1 d . . . . .
C24 C 0.2899(2) 0.1184(5) 0.2243(3) 0.0798(16) Uani 1 1 d . . . . .
O4 O 0.27326(16) 0.1857(4) 0.1715(3) 0.1027(13) Uani 1 1 d . . . . .
O5 O 0.31612(15) 0.0261(4) 0.2495(2) 0.0946(12) Uani 1 1 d . . . . .
C25 C 0.3909(3) 1.1912(7) 0.6029(6) 0.169(4) Uani 1 1 d D . . . .
H25 H 0.368440 1.248646 0.561035 0.203 Uiso 1 1 calc R U . . .
H25A H 0.403982 1.225096 0.650190 0.203 Uiso 1 1 calc R U . . .
C26 C 0.4229(6) 1.1778(12) 0.6112(12) 0.298(10) Uani 1 1 d D . . . .
H26 H 0.425972 1.260295 0.601828 0.358 Uiso 1 1 calc R U . . .
H26A H 0.449775 1.163725 0.666339 0.358 Uiso 1 1 calc R U . . .
C27 C 0.4275(5) 1.1019(12) 0.5777(10) 0.245(7) Uani 1 1 d D . . . .
H27 H 0.420009 1.021587 0.581039 0.294 Uiso 1 1 calc R U . . .
H27A H 0.402133 1.124713 0.523458 0.294 Uiso 1 1 calc R U . . .
C28 C 0.4583(7) 1.0722(17) 0.5850(12) 0.292(9) Uani 1 1 d D . . . .
H28 H 0.462541 1.150311 0.574019 0.351 Uiso 1 1 calc R U . . .
H28A H 0.484835 1.061110 0.640531 0.351 Uiso 1 1 calc R U . . .
C29 C 0.4641(6) 0.9885(17) 0.5564(12) 0.277(9) Uani 1 1 d D . . . .
H29 H 0.445790 1.022027 0.505544 0.333 Uiso 1 1 calc R U . . .
H29A H 0.448007 0.917102 0.546461 0.333 Uiso 1 1 calc R U . . .
C30 C 0.4983(7) 0.935(2) 0.5774(13) 0.302(10) Uani 1 1 d D . . . .
H30 H 0.507310 1.002294 0.568231 0.362 Uiso 1 1 calc R U . . .
H30A H 0.521293 0.931254 0.633346 0.362 Uiso 1 1 calc R U . . .
C31 C 0.5077(8) 0.8343(18) 0.5624(12) 0.292(10) Uani 1 1 d D . . . .
H31 H 0.486055 0.838098 0.506803 0.351 Uiso 1 1 calc R U . . .
H31A H 0.498588 0.765301 0.570348 0.351 Uiso 1 1 calc R U . . .
C32 C 0.5458(8) 0.792(2) 0.5913(14) 0.340(12) Uani 1 1 d D . . . .
H32 H 0.554425 0.862793 0.583456 0.408 Uiso 1 1 calc R U . . .
H32A H 0.566867 0.790072 0.646676 0.408 Uiso 1 1 calc R U . . .
C33 C 0.5594(9) 0.695(2) 0.5815(16) 0.358(13) Uani 1 1 d D . . . .
H33 H 0.538538 0.693040 0.526223 0.430 Uiso 1 1 calc R U . . .
H33A H 0.552893 0.622165 0.592177 0.430 Uiso 1 1 calc R U . . .
C34 C 0.5998(8) 0.669(2) 0.6151(12) 0.304(10) Uani 1 1 d D . . . .
H34 H 0.609928 0.744199 0.612867 0.364 Uiso 1 1 calc R U . . .
H34A H 0.620604 0.651340 0.669427 0.364 Uiso 1 1 calc R U . . .
C35 C 0.6022(8) 0.576(3) 0.5856(17) 0.418(18) Uani 1 1 d D . . . .
H35 H 0.583273 0.594189 0.532084 0.502 Uiso 1 1 calc R U . . .
H35A H 0.592275 0.499734 0.586926 0.502 Uiso 1 1 calc R U . . .
C36 C 0.6452(6) 0.565(2) 0.6291(10) 0.318(10) Uani 1 1 d D . . . .
H36 H 0.652112 0.630156 0.615756 0.477 Uiso 1 1 calc R U . . .
H36A H 0.649279 0.486428 0.618905 0.477 Uiso 1 1 calc R U . . .
H36B H 0.664538 0.570805 0.683104 0.477 Uiso 1 1 calc R U . . .
C37 C 0.3281(3) 0.0086(7) 0.2148(4) 0.112(2) Uani 1 1 d D . . . .
H37 H 0.334829 0.087625 0.208962 0.135 Uiso 0.809(10) 1 calc R U P A 1
H37A H 0.303628 -0.028771 0.163906 0.135 Uiso 0.809(10) 1 calc R U P A 1
H37B H 0.352736 0.061310 0.239380 0.135 Uiso 0.191(10) 1 calc R U P A 2
H37C H 0.303194 0.026981 0.159752 0.135 Uiso 0.191(10) 1 calc R U P A 2
C38 C 0.3670(4) -0.0728(10) 0.2660(8) 0.136(4) Uani 0.809(10) 1 d D . P A 1
H38 H 0.376793 -0.077308 0.245488 0.164 Uiso 0.809(10) 1 calc R U P A 1
H38A H 0.390525 -0.033261 0.316329 0.164 Uiso 0.809(10) 1 calc R U P A 1
C39 C 0.3627(4) -0.1933(10) 0.2773(8) 0.155(5) Uani 0.809(10) 1 d D . P A 1
H39 H 0.337887 -0.230341 0.226474 0.185 Uiso 0.809(10) 1 calc R U P A 1
H39A H 0.354265 -0.187835 0.300050 0.185 Uiso 0.809(10) 1 calc R U P A 1
C40 C 0.3998(5) -0.2809(12) 0.3247(9) 0.184(6) Uani 0.809(10) 1 d D . P A 1
H40 H 0.424690 -0.247477 0.376586 0.221 Uiso 0.809(10) 1 calc R U P A 1
H40A H 0.391194 -0.357849 0.328541 0.221 Uiso 0.809(10) 1 calc R U P A 1
C41 C 0.4141(5) -0.3076(12) 0.2942(10) 0.189(7) Uani 0.809(10) 1 d D . P A 1
H41 H 0.387708 -0.331568 0.240480 0.226 Uiso 0.809(10) 1 calc R U P A 1
H41A H 0.423562 -0.229181 0.293219 0.226 Uiso 0.809(10) 1 calc R U P A 1
C42 C 0.4478(5) -0.3962(13) 0.3266(10) 0.264(8) Uani 1 1 d D . . . .
H42 H 0.472947 -0.376349 0.381359 0.317 Uiso 0.809(10) 1 calc R U P A 1
H42A H 0.436734 -0.475161 0.323289 0.317 Uiso 0.809(10) 1 calc R U P A 1
H42B H 0.469558 -0.364127 0.378949 0.317 Uiso 0.191(10) 1 calc R U P A 2
H42C H 0.432950 -0.467446 0.320538 0.317 Uiso 0.191(10) 1 calc R U P A 2
C43 C 0.4657(6) -0.4212(14) 0.3051(11) 0.268(8) Uani 1 1 d D . . . .
H43 H 0.475075 -0.343304 0.303674 0.322 Uiso 1 1 calc R U . . .
H43A H 0.442158 -0.453468 0.252621 0.322 Uiso 1 1 calc R U . . .
C44 C 0.5029(6) -0.5072(19) 0.3530(13) 0.352(12) Uani 1 1 d D . . . .
H44 H 0.524259 -0.468236 0.403566 0.422 Uiso 1 1 calc R U . . .
H44A H 0.491827 -0.577388 0.356292 0.422 Uiso 1 1 calc R U . . .
C45 C 0.5294(8) -0.562(2) 0.3559(15) 0.429(15) Uani 1 1 d D . . . .
H45 H 0.550396 -0.496436 0.378194 0.515 Uiso 1 1 calc R U . . .
H45A H 0.510201 -0.562156 0.301425 0.515 Uiso 1 1 calc R U . . .
C46 C 0.5564(9) -0.668(3) 0.3820(16) 0.62(2) Uani 1 1 d D U . . .
H46 H 0.539371 -0.743526 0.363774 0.741 Uiso 1 1 calc R U . . .
H46A H 0.565844 -0.665935 0.360945 0.741 Uiso 1 1 calc R U . . .
C47 C 0.5939(8) -0.6690(18) 0.4640(15) 0.53(2) Uani 1 1 d D . . . .
H47 H 0.582334 -0.670212 0.481366 0.633 Uiso 1 1 calc R U . . .
H47A H 0.607766 -0.588725 0.478666 0.633 Uiso 1 1 calc R U . . .
C48 C 0.6296(6) -0.7575(15) 0.5119(11) 0.323(9) Uani 1 1 d D . . . .
H48 H 0.621226 -0.827464 0.480998 0.485 Uiso 1 1 calc R U . . .
H48A H 0.635617 -0.784385 0.552923 0.485 Uiso 1 1 calc R U . . .
H48B H 0.655557 -0.719787 0.533679 0.485 Uiso 1 1 calc R U . . .
C49 C 0.3407(9) -0.126(3) 0.228(2) 0.086(9) Uani 0.191(10) 1 d D . P A 2
H49 H 0.358101 -0.146704 0.280767 0.103 Uiso 0.191(10) 1 calc R U P A 2
H49A H 0.313744 -0.174723 0.193456 0.103 Uiso 0.191(10) 1 calc R U P A 2
C50 C 0.3661(13) -0.169(4) 0.219(2) 0.144(15) Uani 0.191(10) 1 d D . P A 2
H50 H 0.395083 -0.130423 0.257904 0.173 Uiso 0.191(10) 1 calc R U P A 2
H50A H 0.350520 -0.145813 0.168249 0.173 Uiso 0.191(10) 1 calc R U P A 2
C51 C 0.3710(17) -0.308(5) 0.228(6) 0.38(6) Uani 0.191(10) 1 d D . P A 2
H51 H 0.371295 -0.339915 0.261512 0.460 Uiso 0.191(10) 1 calc R U P A 2
H51A H 0.349660 -0.351619 0.179036 0.460 Uiso 0.191(10) 1 calc R U P A 2
C52 C 0.4159(13) -0.299(5) 0.266(3) 0.27(3) Uani 0.191(10) 1 d D . P A 2
H52 H 0.428306 -0.218356 0.290566 0.324 Uiso 0.191(10) 1 calc R U P A 2
H52A H 0.412847 -0.305190 0.227052 0.324 Uiso 0.191(10) 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 V1 1.075(3) 7_556 ?
V1 O1 1.599(7) . ?
V1 N1 2.048(4) . ?
V1 N2 2.057(4) . ?
V1 N2 2.101(4) 7_556 ?
V1 N1 2.111(4) 7_556 ?
N1 C1 1.383(6) . ?
N1 C4 1.387(5) . ?
N2 C8 1.386(6) . ?
N2 C5 1.399(6) . ?
C1 C9 1.390(6) . ?
C1 C2 1.436(6) . ?
C2 C3 1.344(7) . ?
C3 C4 1.425(7) . ?
C4 C10 1.395(6) . ?
C5 C10 1.400(6) . ?
C5 C6 1.417(6) . ?
C6 C7 1.341(6) . ?
C7 C8 1.420(6) . ?
C8 C9 1.407(6) 7_556 ?
C9 C11 1.487(6) . ?
C10 C17 1.496(6) . ?
C11 C16 1.378(6) . ?
C11 C12 1.380(8) . ?
C12 C13 1.405(8) . ?
C13 C14 1.350(8) . ?
C14 C15 1.380(8) . ?
C14 C23 1.498(8) . ?
C15 C16 1.378(7) . ?
C17 C22 1.378(7) . ?
C17 C18 1.388(6) . ?
C18 C19 1.367(6) . ?
C19 C20 1.382(6) . ?
C20 C21 1.417(7) . ?
C20 C24 1.477(7) . ?
C21 C22 1.369(7) . ?
C23 O2 1.201(8) . ?
C23 O3 1.329(8) . ?
O3 C25 1.459(8) . ?
C24 O4 1.211(6) . ?
C24 O5 1.306(7) . ?
O5 C37 1.453(6) . ?
C25 C26 1.374(12) . ?
C26 C27 1.368(12) . ?
C27 C28 1.365(12) . ?
C28 C29 1.360(13) . ?
C29 C30 1.372(13) . ?
C30 C31 1.359(15) . ?
C31 C32 1.388(15) . ?
C32 C33 1.368(16) . ?
C33 C34 1.379(17) . ?
C34 C35 1.349(17) . ?
C35 C36 1.370(16) . ?
C37 C38 1.471(10) . ?
C37 C49 1.51(3) . ?
C38 C39 1.392(11) . ?
C39 C40 1.471(11) . ?
C40 C41 1.463(12) . ?
C41 C42 1.442(12) . ?
C42 C43 1.392(14) . ?
C42 C52 1.50(3) . ?
C43 C44 1.461(14) . ?
C44 C45 1.348(16) . ?
C45 C46 1.436(17) . ?
C46 C47 1.417(18) . ?
C47 C48 1.441(15) . ?
C49 C50 1.50(3) . ?
C50 C51 1.51(3) . ?
C51 C52 1.50(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
V1 V1 O1 176.2(3) 7_556 . ?
V1 V1 N1 78.3(2) 7_556 . ?
O1 V1 N1 104.8(3) . . ?
V1 V1 N2 77.3(2) 7_556 . ?
O1 V1 N2 105.0(3) . . ?
N1 V1 N2 87.74(16) . . ?
V1 V1 N2 72.8(2) 7_556 7_556 ?
O1 V1 N2 104.9(3) . 7_556 ?
N1 V1 N2 86.25(16) . 7_556 ?
N2 V1 N2 150.06(10) . 7_556 ?
V1 V1 N1 71.8(2) 7_556 7_556 ?
O1 V1 N1 105.1(3) . 7_556 ?
N1 V1 N1 150.09(10) . 7_556 ?
N2 V1 N1 85.76(17) . 7_556 ?
N2 V1 N1 84.99(16) 7_556 7_556 ?
C1 N1 C4 105.9(4) . . ?
C1 N1 V1 126.1(3) . . ?
C4 N1 V1 124.5(3) . . ?
C1 N1 V1 125.1(3) . 7_556 ?
C4 N1 V1 126.7(3) . 7_556 ?
V1 N1 V1 29.91(10) . 7_556 ?
C8 N2 C5 104.6(4) . . ?
C8 N2 V1 127.3(3) . . ?
C5 N2 V1 124.8(3) . . ?
C8 N2 V1 125.4(3) . 7_556 ?
C5 N2 V1 127.4(3) . 7_556 ?
V1 N2 V1 29.94(10) . 7_556 ?
N1 C1 C9 126.3(4) . . ?
N1 C1 C2 109.3(4) . . ?
C9 C1 C2 124.4(5) . . ?
C3 C2 C1 107.5(5) . . ?
C2 C3 C4 107.7(4) . . ?
N1 C4 C10 125.8(4) . . ?
N1 C4 C3 109.6(4) . . ?
C10 C4 C3 124.6(4) . . ?
N2 C5 C10 124.5(4) . . ?
N2 C5 C6 109.8(4) . . ?
C10 C5 C6 125.8(4) . . ?
C7 C6 C5 107.9(4) . . ?
C6 C7 C8 107.5(4) . . ?
N2 C8 C9 125.0(4) . 7_556 ?
N2 C8 C7 110.3(4) . . ?
C9 C8 C7 124.7(4) 7_556 . ?
C1 C9 C8 124.0(4) . 7_556 ?
C1 C9 C11 118.1(4) . . ?
C8 C9 C11 117.9(4) 7_556 . ?
C4 C10 C5 124.9(4) . . ?
C4 C10 C17 117.5(4) . . ?
C5 C10 C17 117.5(4) . . ?
C16 C11 C12 117.8(5) . . ?
C16 C11 C9 121.6(5) . . ?
C12 C11 C9 120.7(5) . . ?
C11 C12 C13 120.5(5) . . ?
C14 C13 C12 120.1(6) . . ?
C13 C14 C15 120.3(5) . . ?
C13 C14 C23 118.4(6) . . ?
C15 C14 C23 121.3(6) . . ?
C16 C15 C14 119.3(5) . . ?
C11 C16 C15 122.0(5) . . ?
C22 C17 C18 118.4(4) . . ?
C22 C17 C10 120.8(4) . . ?
C18 C17 C10 120.8(4) . . ?
C19 C18 C17 121.1(5) . . ?
C18 C19 C20 121.4(5) . . ?
C19 C20 C21 117.2(4) . . ?
C19 C20 C24 123.1(5) . . ?
C21 C20 C24 119.6(5) . . ?
C22 C21 C20 120.7(5) . . ?
C21 C22 C17 121.1(5) . . ?
O2 C23 O3 122.9(6) . . ?
O2 C23 C14 123.0(7) . . ?
O3 C23 C14 114.0(7) . . ?
C23 O3 C25 118.5(6) . . ?
O4 C24 O5 124.1(5) . . ?
O4 C24 C20 122.7(6) . . ?
O5 C24 C20 113.2(5) . . ?
C24 O5 C37 117.4(5) . . ?
C26 C25 O3 110.5(9) . . ?
C27 C26 C25 133.7(15) . . ?
C28 C27 C26 139.5(18) . . ?
C29 C28 C27 139(2) . . ?
C28 C29 C30 139(2) . . ?
C31 C30 C29 141(2) . . ?
C30 C31 C32 134(3) . . ?
C33 C32 C31 139(3) . . ?
C32 C33 C34 131(3) . . ?
C35 C34 C33 119(3) . . ?
C34 C35 C36 108(3) . . ?
O5 C37 C38 108.0(6) . . ?
O5 C37 C49 104.5(14) . . ?
C39 C38 C37 118.2(11) . . ?
C38 C39 C40 120.7(12) . . ?
C41 C40 C39 114.0(12) . . ?
C42 C41 C40 125.1(15) . . ?
C43 C42 C41 129.0(18) . . ?
C43 C42 C52 96(3) . . ?
C42 C43 C44 117.9(19) . . ?
C45 C44 C43 141(3) . . ?
C44 C45 C46 146(3) . . ?
C47 C46 C45 110(2) . . ?
C46 C47 C48 126(2) . . ?
C50 C49 C37 119(3) . . ?
C49 C50 C51 109(5) . . ?
C52 C51 C50 91(5) . . ?
C51 C52 C42 114(4) . . ?

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
C4 N1 C1 C9 -178.7(5) . . . . ?
V1 N1 C1 C9 -19.3(8) . . . . ?
V1 N1 C1 C9 17.7(7) 7_556 . . . ?
C4 N1 C1 C2 -1.2(6) . . . . ?
V1 N1 C1 C2 158.2(4) . . . . ?
V1 N1 C1 C2 -164.7(4) 7_556 . . . ?
N1 C1 C2 C3 1.1(7) . . . . ?
C9 C1 C2 C3 178.8(5) . . . . ?
C1 C2 C3 C4 -0.6(7) . . . . ?
C1 N1 C4 C10 179.5(5) . . . . ?
V1 N1 C4 C10 19.6(7) . . . . ?
V1 N1 C4 C10 -17.3(7) 7_556 . . . ?
C1 N1 C4 C3 0.8(6) . . . . ?
V1 N1 C4 C3 -159.1(4) . . . . ?
V1 N1 C4 C3 164.0(4) 7_556 . . . ?
C2 C3 C4 N1 -0.1(7) . . . . ?
C2 C3 C4 C10 -178.8(5) . . . . ?
C8 N2 C5 C10 -179.8(5) . . . . ?
V1 N2 C5 C10 -19.3(7) . . . . ?
V1 N2 C5 C10 17.8(7) 7_556 . . . ?
C8 N2 C5 C6 0.3(5) . . . . ?
V1 N2 C5 C6 160.8(3) . . . . ?
V1 N2 C5 C6 -162.0(3) 7_556 . . . ?
N2 C5 C6 C7 -0.4(6) . . . . ?
C10 C5 C6 C7 179.8(5) . . . . ?
C5 C6 C7 C8 0.3(6) . . . . ?
C5 N2 C8 C9 178.5(5) . . . 7_556 ?
V1 N2 C8 C9 18.6(7) . . . 7_556 ?
V1 N2 C8 C9 -18.7(7) 7_556 . . 7_556 ?
C5 N2 C8 C7 -0.1(5) . . . . ?
V1 N2 C8 C7 -160.0(3) . . . . ?
V1 N2 C8 C7 162.7(3) 7_556 . . . ?
C6 C7 C8 N2 -0.1(6) . . . . ?
C6 C7 C8 C9 -178.7(5) . . . 7_556 ?
N1 C1 C9 C8 0.5(9) . . . 7_556 ?
C2 C1 C9 C8 -176.8(5) . . . 7_556 ?
N1 C1 C9 C11 -178.1(5) . . . . ?
C2 C1 C9 C11 4.6(8) . . . . ?
N1 C4 C10 C5 0.3(9) . . . . ?
C3 C4 C10 C5 178.8(5) . . . . ?
N1 C4 C10 C17 -178.6(5) . . . . ?
C3 C4 C10 C17 -0.1(8) . . . . ?
N2 C5 C10 C4 -0.4(8) . . . . ?
C6 C5 C10 C4 179.4(5) . . . . ?
N2 C5 C10 C17 178.4(4) . . . . ?
C6 C5 C10 C17 -1.8(8) . . . . ?
C1 C9 C11 C16 66.8(7) . . . . ?
C8 C9 C11 C16 -111.8(6) 7_556 . . . ?
C1 C9 C11 C12 -113.4(6) . . . . ?
C8 C9 C11 C12 67.9(7) 7_556 . . . ?
C16 C11 C12 C13 -2.5(9) . . . . ?
C9 C11 C12 C13 177.8(5) . . . . ?
C11 C12 C13 C14 1.5(10) . . . . ?
C12 C13 C14 C15 -1.1(10) . . . . ?
C12 C13 C14 C23 -178.4(6) . . . . ?
C13 C14 C15 C16 1.8(9) . . . . ?
C23 C14 C15 C16 179.1(6) . . . . ?
C12 C11 C16 C15 3.3(8) . . . . ?
C9 C11 C16 C15 -177.0(5) . . . . ?
C14 C15 C16 C11 -3.0(9) . . . . ?
C4 C10 C17 C22 -68.0(7) . . . . ?
C5 C10 C17 C22 113.1(6) . . . . ?
C4 C10 C17 C18 110.4(6) . . . . ?
C5 C10 C17 C18 -68.5(7) . . . . ?
C22 C17 C18 C19 1.0(8) . . . . ?
C10 C17 C18 C19 -177.4(5) . . . . ?
C17 C18 C19 C20 -0.2(8) . . . . ?
C18 C19 C20 C21 -0.9(8) . . . . ?
C18 C19 C20 C24 175.8(5) . . . . ?
C19 C20 C21 C22 1.3(8) . . . . ?
C24 C20 C21 C22 -175.5(5) . . . . ?
C20 C21 C22 C17 -0.6(9) . . . . ?
C18 C17 C22 C21 -0.6(8) . . . . ?
C10 C17 C22 C21 177.9(5) . . . . ?
C13 C14 C23 O2 -15.5(11) . . . . ?
C15 C14 C23 O2 167.2(7) . . . . ?
C13 C14 C23 O3 162.3(6) . . . . ?
C15 C14 C23 O3 -15.0(9) . . . . ?
O2 C23 O3 C25 -2.4(12) . . . . ?
C14 C23 O3 C25 179.9(7) . . . . ?
C19 C20 C24 O4 -174.4(5) . . . . ?
C21 C20 C24 O4 2.2(8) . . . . ?
C19 C20 C24 O5 7.5(8) . . . . ?
C21 C20 C24 O5 -175.8(5) . . . . ?
O4 C24 O5 C37 4.0(9) . . . . ?
C20 C24 O5 C37 -178.0(5) . . . . ?
C23 O3 C25 C26 90.8(14) . . . . ?
O3 C25 C26 C27 33(3) . . . . ?
C25 C26 C27 C28 -173(2) . . . . ?
C26 C27 C28 C29 172(3) . . . . ?
C27 C28 C29 C30 -156(3) . . . . ?
C28 C29 C30 C31 159(3) . . . . ?
C29 C30 C31 C32 -178(3) . . . . ?
C30 C31 C32 C33 -180(3) . . . . ?
C31 C32 C33 C34 178(3) . . . . ?
C32 C33 C34 C35 -169(3) . . . . ?
C33 C34 C35 C36 -178(2) . . . . ?
C24 O5 C37 C38 163.1(7) . . . . ?
C24 O5 C37 C49 -156.8(13) . . . . ?
O5 C37 C38 C39 63.6(13) . . . . ?
C37 C38 C39 C40 176.9(10) . . . . ?
C38 C39 C40 C41 -62(2) . . . . ?
C39 C40 C41 C42 -175.7(14) . . . . ?
C40 C41 C42 C43 -174.9(18) . . . . ?
C41 C42 C43 C44 173.7(16) . . . . ?
C52 C42 C43 C44 175(3) . . . . ?
C42 C43 C44 C45 177(3) . . . . ?
C43 C44 C45 C46 -152(4) . . . . ?
C44 C45 C46 C47 -67(6) . . . . ?
C45 C46 C47 C48 -178(2) . . . . ?
O5 C37 C49 C50 -164(2) . . . . ?
C37 C49 C50 C51 -175(4) . . . . ?
C49 C50 C51 C52 -145(4) . . . . ?
C50 C51 C52 C42 148(5) . . . . ?
C43 C42 C52 C51 138(5) . . . . ?

_refine_diff_density_max         0.430
_refine_diff_density_min         -0.289
_refine_diff_density_rms         0.049


_symmetry_cell_setting           ?
_symmetry_space_group_name_H-M   ?
_diffrn_radiation_source         ?
_diffrn_radiation_monochromator  graphite
_chemical_absolute_configuration ?
