# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2020

####################################################################### 
# 
# 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_35-wo
_database_code_depnum_ccdc_archive 'CCDC 1974736'
loop_
_audit_author_name
_audit_author_address
'Zicheng Xiao'
;Hubei University of Technology
China
;
_audit_update_record             
;
2019-12-30 deposited with the CCDC.	2020-03-13 downloaded from the CCDC.
;
_audit_creation_date             2017-12-04
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C35 H60 N O12.5 V3, C4 H9 N O, C8 H20 N'
_chemical_formula_sum            'C47 H89 N3 O13.50 V3'
_chemical_formula_weight         1065.03
_chemical_melting_point          ?
_chemical_oxdiff_formula         'V O C N'
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'

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

_cell_length_a                   10.1207(4)
_cell_length_b                   10.7427(5)
_cell_length_c                   27.9069(12)
_cell_angle_alpha                99.871(4)
_cell_angle_beta                 90.774(4)
_cell_angle_gamma                117.159(5)
_cell_volume                     2645.0(2)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    5429
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      28.2670
_cell_measurement_theta_min      3.7390
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.582
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.75280
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.33c (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear orange'
_exptl_crystal_density_diffrn    1.337
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1138
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.01
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0447
_diffrn_reflns_av_unetI/netI     0.0733
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            24023
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.658
_diffrn_reflns_theta_min         3.342
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2137
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     39.00  66.00   1.00   30.00    --    9.97  57.00  90.00   27
  2  ω    -20.00  84.00   1.00   30.00    --    9.97  77.00  60.00  104
  3  ω     49.00  76.00   1.00   30.00    --    9.97 178.00 150.00   27
  4  ω    -38.00  61.00   1.00   30.00    --  -11.85  57.00 -60.00   99
  5  ω    -88.00  10.00   1.00   30.00    --  -11.85 -77.00-180.00   98
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0186840000
_diffrn_orient_matrix_UB_12      -0.0540776000
_diffrn_orient_matrix_UB_13      0.0035982000
_diffrn_orient_matrix_UB_21      0.0607156000
_diffrn_orient_matrix_UB_22      0.0271858000
_diffrn_orient_matrix_UB_23      -0.0142300000
_diffrn_orient_matrix_UB_31      0.0473060000
_diffrn_orient_matrix_UB_32      0.0455187000
_diffrn_orient_matrix_UB_33      0.0213893000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                8402
_reflns_number_total             11088
_reflns_odcompleteness_completeness 96.38
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.42
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         0.463
_refine_diff_density_min         -0.549
_refine_diff_density_rms         0.076
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     631
_refine_ls_number_reflns         11088
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0768
_refine_ls_R_factor_gt           0.0511
_refine_ls_restrained_S_all      1.036
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0289P)²+1.8102P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0900
_refine_ls_wR_factor_ref         0.0995
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(O14A) = Uanis(O14)
Uanis(C44A) = Uanis(C44)
Uanis(C56) = Uanis(C5A)
Uanis(C63) = Uanis(C63A)
Uanis(C5) = Uanis(C56A)
Uanis(N43A) = Uanis(N43)
3. Others
 Sof(C5A)=Sof(H5AA)=Sof(H5AB)=Sof(H5AC)=Sof(C44A)=Sof(O14A)=Sof(N43A)=
 Sof(C63A)=Sof(H63D)=Sof(H63E)=Sof(H63F)=Sof(C56A)=Sof(H56D)=Sof(H56E)=
 Sof(H56F)=1-FVAR(1)
 Sof(O14)=Sof(N43)=Sof(C44)=Sof(C56)=Sof(H56A)=Sof(H56B)=Sof(H56C)=Sof(C63)=
 Sof(H63A)=Sof(H63B)=Sof(H63C)=Sof(C5)=Sof(H5A)=Sof(H5B)=Sof(H5C)=FVAR(1)
4.a Ternary CH refined with riding coordinates:
 N1(H1), C2(H2), C9(H9)
4.b Secondary CH2 refined with riding coordinates:
 C17(H17A,H17B), C20(H20A,H20B), C30(H30A,H30B), C32(H32A,H32B), C33(H33A,
 H33B), C34(H34A,H34B), C35(H35A,H35B), C36(H36A,H36B), C37(H37A,H37B),
 C38(H38A,H38B), C40(H40A,H40B), C41(H41A,H41B), C42(H42A,H42B), C45(H45A,H45B),
  C46(H46A,H46B), C47(H47A,H47B), C49(H49A,H49B), C50(H50A,H50B), C51(H51A,
 H51B), C52(H52A,H52B), C53(H53A,H53B), C57(H57A,H57B), C58(H58A,H58B),
 C59(H59A,H59B), C65(H65A,H65B), C4(H4A,H4B)
4.c Aromatic/amide H refined with riding coordinates:
 N15(H15), C24(H24), C27(H27), C31(H31)
4.d Idealised Me refined with riding coordinates:
 C56(H56A,H56B,H56C), C5A(H5AA,H5AB,H5AC)
4.e Idealised Me refined as rotating group:
 C62(H62A,H62B,H62C), C64(H64A,H64B,H64C), C63(H63A,H63B,H63C), C3(H3A,H3B,
 H3C), C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C),
 C10(H10A,H10B,H10C), C63A(H63D,H63E,H63F), C56A(H56D,H56E,H56F)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
V1 V 0.64306(4) 0.11384(4) 0.44493(2) 0.00902(10) Uani 1 1 d . . . . .
V2 V 0.58716(4) 0.21639(4) 0.54724(2) 0.00868(10) Uani 1 1 d . . . . .
V3 V 0.69460(4) -0.03139(4) 0.52140(2) 0.00875(10) Uani 1 1 d . . . . .
O1 O 0.76991(16) 0.05598(17) 0.47250(6) 0.0095(4) Uani 1 1 d . . . . .
O2 O 0.42185(16) 0.21104(17) 0.52025(6) 0.0091(4) Uani 1 1 d . . . . .
O3 O 0.5000 0.0000 0.5000 0.0066(5) Uani 1 2 d S T P . .
O4 O 0.73935(16) 0.15168(16) 0.56469(6) 0.0072(4) Uani 1 1 d . . . . .
O5 O 0.69318(17) 0.26469(17) 0.49342(6) 0.0097(4) Uani 1 1 d . . . . .
O6 O 0.52933(16) -0.09211(17) 0.40747(6) 0.0079(4) Uani 1 1 d . . . . .
O0AA O 0.45137(16) 0.11309(17) 0.42823(6) 0.0074(4) Uani 1 1 d . . . . .
O8 O 0.82722(17) -0.05014(18) 0.54553(7) 0.0125(4) Uani 1 1 d . . . . .
O9 O 0.66128(17) 0.36302(17) 0.58685(6) 0.0116(4) Uani 1 1 d . . . . .
O10 O 0.72648(17) 0.17999(18) 0.40009(7) 0.0131(4) Uani 1 1 d . . . . .
O11 O 0.20735(19) -0.34191(19) 0.28655(7) 0.0182(4) Uani 1 1 d . . . . .
O12 O -0.15251(19) -0.55889(18) 0.14161(7) 0.0164(4) Uani 1 1 d . . . . .
O13 O -0.00361(19) -0.06556(18) 0.15369(7) 0.0170(4) Uani 1 1 d . . . . .
N15 N 0.2720(2) -0.1066(2) 0.30649(8) 0.0108(5) Uani 1 1 d . . . . .
H15 H 0.2802 -0.0340 0.2953 0.013 Uiso 1 1 calc R . . . .
C17 C 0.3925(3) 0.0760(3) 0.37823(9) 0.0102(5) Uani 1 1 d . . . . .
H17A H 0.4694 0.1326 0.3594 0.012 Uiso 1 1 calc R . . . .
H17B H 0.3107 0.0987 0.3755 0.012 Uiso 1 1 calc R . . . .
C18 C 0.1998(3) -0.2380(3) 0.27679(10) 0.0129(6) Uani 1 1 d . . . . .
C19 C 0.1067(3) -0.2533(3) 0.23148(10) 0.0124(5) Uani 1 1 d . . . . .
C20 C 0.0849(3) 0.0812(3) 0.17722(10) 0.0159(6) Uani 1 1 d . . . . .
H20A H 0.1905 0.1084 0.1775 0.019 Uiso 1 1 calc R . . . .
H20B H 0.0621 0.0970 0.2107 0.019 Uiso 1 1 calc R . . . .
C21 C -0.0743(3) -0.4184(3) 0.16442(10) 0.0140(6) Uani 1 1 d . . . . .
C22 C 0.3365(2) -0.0828(2) 0.35673(9) 0.0086(5) Uani 1 1 d . . . . .
C24 C -0.0813(3) -0.3068(3) 0.14842(10) 0.0133(6) Uani 1 1 d . . . . .
H24 H -0.1455 -0.3242 0.1211 0.016 Uiso 1 1 calc R . . . .
C27 C 0.1034(3) -0.1385(3) 0.21533(10) 0.0136(6) Uani 1 1 d . . . . .
H27 H 0.1627 -0.0452 0.2320 0.016 Uiso 1 1 calc R . . . .
C29 C 0.0097(3) -0.1671(3) 0.17382(10) 0.0133(6) Uani 1 1 d . . . . .
C30 C 0.1277(3) 0.3268(3) 0.16677(11) 0.0178(6) Uani 1 1 d . . . . .
H30A H 0.0813 0.3713 0.1501 0.021 Uiso 1 1 calc R . . . .
H30B H 0.1165 0.3459 0.2013 0.021 Uiso 1 1 calc R . . . .
C31 C 0.0186(3) -0.3920(3) 0.20634(10) 0.0139(6) Uani 1 1 d . . . . .
H31 H 0.0213 -0.4677 0.2174 0.017 Uiso 1 1 calc R . . . .
C32 C 0.2934(3) 0.3959(3) 0.16024(11) 0.0198(6) Uani 1 1 d . . . . .
H32A H 0.3057 0.3697 0.1262 0.024 Uiso 1 1 calc R . . . .
H32B H 0.3424 0.3592 0.1797 0.024 Uiso 1 1 calc R . . . .
C33 C -0.3007(3) -0.9752(3) 0.04949(11) 0.0230(7) Uani 1 1 d . . . . .
H33A H -0.3907 -1.0093 0.0276 0.028 Uiso 1 1 calc R . . . .
H33B H -0.3308 -1.0077 0.0798 0.028 Uiso 1 1 calc R . . . .
C34 C -0.2235(3) -0.8128(3) 0.06030(11) 0.0200(6) Uani 1 1 d . . . . .
H34A H -0.1908 -0.7790 0.0304 0.024 Uiso 1 1 calc R . . . .
H34B H -0.1356 -0.7774 0.0834 0.024 Uiso 1 1 calc R . . . .
C35 C 0.0445(3) 0.1660(3) 0.14758(11) 0.0180(6) Uani 1 1 d . . . . .
H35A H -0.0619 0.1345 0.1471 0.022 Uiso 1 1 calc R . . . .
H35B H 0.0655 0.1457 0.1141 0.022 Uiso 1 1 calc R . . . .
C36 C -0.2002(3) -1.2785(3) -0.00490(11) 0.0220(6) Uani 1 1 d . . . . .
H36A H -0.1605 -1.2431 -0.0340 0.026 Uiso 1 1 calc R . . . .
H36B H -0.1164 -1.2535 0.0187 0.026 Uiso 1 1 calc R . . . .
C37 C -0.2506(3) -0.5932(3) 0.09839(10) 0.0177(6) Uani 1 1 d . . . . .
H37A H -0.1944 -0.5468 0.0731 0.021 Uiso 1 1 calc R . . . .
H37B H -0.3247 -0.5609 0.1056 0.021 Uiso 1 1 calc R . . . .
C38 C 0.2121(3) -0.1747(3) 0.38506(9) 0.0102(5) Uani 1 1 d . . . . .
H38A H 0.1294 -0.1532 0.3824 0.012 Uiso 1 1 calc R . . . .
H38B H 0.1763 -0.2746 0.3704 0.012 Uiso 1 1 calc R . . . .
C40 C -0.3257(3) -0.7532(3) 0.08138(10) 0.0189(6) Uani 1 1 d . . . . .
H40A H -0.4075 -0.7803 0.0567 0.023 Uiso 1 1 calc R . . . .
H40B H -0.3681 -0.7972 0.1088 0.023 Uiso 1 1 calc R . . . .
C41 C 0.4669(3) -0.1192(3) 0.35796(9) 0.0103(5) Uani 1 1 d . . . . .
H41A H 0.4315 -0.2190 0.3432 0.012 Uiso 1 1 calc R . . . .
H41B H 0.5434 -0.0619 0.3392 0.012 Uiso 1 1 calc R . . . .
C42 C -0.2125(3) -1.7513(3) -0.07852(12) 0.0255(7) Uani 1 1 d . . . . .
H42A H -0.1788 -1.7166 -0.1082 0.031 Uiso 1 1 calc R . . . .
H42B H -0.1247 -1.7261 -0.0568 0.031 Uiso 1 1 calc R . . . .
C45 C 0.3687(3) 0.5580(3) 0.17523(11) 0.0188(6) Uani 1 1 d . . . . .
H45A H 0.3625 0.5840 0.2099 0.023 Uiso 1 1 calc R . . . .
H45B H 0.3147 0.5939 0.1576 0.023 Uiso 1 1 calc R . . . .
C46 C 0.6127(3) 1.0838(3) 0.22612(12) 0.0265(7) Uani 1 1 d . . . . .
H46A H 0.5900 1.0525 0.1909 0.032 Uiso 1 1 calc R . . . .
H46B H 0.5187 1.0476 0.2405 0.032 Uiso 1 1 calc R . . . .
C47 C -0.2975(3) -1.6764(3) -0.05435(11) 0.0190(6) Uani 1 1 d . . . . .
H47A H -0.3344 -1.7134 -0.0252 0.023 Uiso 1 1 calc R . . . .
H47B H -0.3833 -1.6985 -0.0766 0.023 Uiso 1 1 calc R . . . .
C49 C -0.2071(3) -1.0433(3) 0.02668(11) 0.0226(7) Uani 1 1 d . . . . .
H49A H -0.1765 -1.0115 -0.0037 0.027 Uiso 1 1 calc R . . . .
H49B H -0.1175 -1.0111 0.0486 0.027 Uiso 1 1 calc R . . . .
C50 C -0.2039(3) -1.5152(3) -0.04021(11) 0.0209(6) Uani 1 1 d . . . . .
H50A H -0.1634 -1.4788 -0.0691 0.025 Uiso 1 1 calc R . . . .
H50B H -0.1206 -1.4931 -0.0169 0.025 Uiso 1 1 calc R . . . .
C51 C -0.2906(3) -1.2052(3) 0.01644(12) 0.0241(7) Uani 1 1 d . . . . .
H51A H -0.3786 -1.2367 -0.0061 0.029 Uiso 1 1 calc R . . . .
H51B H -0.3242 -1.2360 0.0467 0.029 Uiso 1 1 calc R . . . .
C52 C -0.2906(3) -1.4391(3) -0.01797(11) 0.0201(6) Uani 1 1 d . . . . .
H52A H -0.3755 -1.4636 -0.0410 0.024 Uiso 1 1 calc R . . . .
H52B H -0.3290 -1.4741 0.0113 0.024 Uiso 1 1 calc R . . . .
C53 C 0.5319(3) 0.6297(3) 0.16545(12) 0.0226(7) Uani 1 1 d . . . . .
H53A H 0.5385 0.5991 0.1312 0.027 Uiso 1 1 calc R . . . .
H53B H 0.5868 0.5976 0.1845 0.027 Uiso 1 1 calc R . . . .
C57 C 0.6876(3) 1.2447(3) 0.23825(13) 0.0311(8) Uani 1 1 d . . . . .
H57A H 0.7786 1.2813 0.2223 0.037 Uiso 1 1 calc R . . . .
H57B H 0.7153 1.2765 0.2733 0.037 Uiso 1 1 calc R . . . .
C58 C 0.6063(3) 0.7931(3) 0.17774(11) 0.0227(7) Uani 1 1 d . . . . .
H58A H 0.7024 0.8301 0.1648 0.027 Uiso 1 1 calc R . . . .
H58B H 0.5452 0.8246 0.1614 0.027 Uiso 1 1 calc R . . . .
C59 C 0.7048(3) 1.0193(3) 0.24390(12) 0.0248(7) Uani 1 1 d . . . . .
H59A H 0.7278 1.0512 0.2791 0.030 Uiso 1 1 calc R . . . .
H59B H 0.7985 1.0554 0.2295 0.030 Uiso 1 1 calc R . . . .
C62 C -0.3032(3) -1.9128(3) -0.09117(12) 0.0306(7) Uani 1 1 d . . . . .
H62A H -0.3872 -1.9391 -0.1143 0.046 Uiso 1 1 calc GR . . . .
H62B H -0.3379 -1.9483 -0.0620 0.046 Uiso 1 1 calc GR . . . .
H62C H -0.2417 -1.9531 -0.1052 0.046 Uiso 1 1 calc GR . . . .
C64 C 0.5896(4) 1.3065(4) 0.22256(13) 0.0364(8) Uani 1 1 d . . . . .
H64A H 0.5601 1.2739 0.1880 0.055 Uiso 1 1 calc GR . . . .
H64B H 0.6445 1.4089 0.2299 0.055 Uiso 1 1 calc GR . . . .
H64C H 0.5024 1.2760 0.2399 0.055 Uiso 1 1 calc GR . . . .
C65 C 0.6297(3) 0.8565(3) 0.23202(11) 0.0263(7) Uani 1 1 d . . . . .
H65A H 0.6904 0.8247 0.2484 0.032 Uiso 1 1 calc R . . . .
H65B H 0.5336 0.8201 0.2450 0.032 Uiso 1 1 calc R . . . .
O14 O 0.2655(16) 0.1680(19) 0.2972(6) 0.0167(14) Uani 0.780(4) 1 d . . . A 1
N43 N 0.0979(3) 0.2391(3) 0.32903(11) 0.0169(7) Uani 0.780(4) 1 d . . . A 1
C44 C 0.2231(4) 0.2652(4) 0.30767(13) 0.0144(8) Uani 0.780(4) 1 d . . . A 1
C56 C 0.0121(7) 0.1013(7) 0.3423(3) 0.0224(12) Uani 0.780(4) 1 d . . . A 1
H56A H 0.0101 0.0274 0.3170 0.034 Uiso 0.780(4) 1 calc R . . A 1
H56B H -0.0881 0.0855 0.3463 0.034 Uiso 0.780(4) 1 calc R . . A 1
H56C H 0.0575 0.0997 0.3725 0.034 Uiso 0.780(4) 1 calc R . . A 1
C63 C 0.0491(10) 0.3436(7) 0.3442(4) 0.0224(14) Uani 0.780(4) 1 d . . . A 1
H63A H 0.0801 0.3835 0.3784 0.034 Uiso 0.780(4) 1 calc GR . . A 1
H63B H -0.0578 0.2996 0.3387 0.034 Uiso 0.780(4) 1 calc GR . . A 1
H63C H 0.0921 0.4179 0.3258 0.034 Uiso 0.780(4) 1 calc GR . . A 1
N1 N -0.2772(2) -0.3876(2) 0.43559(8) 0.0122(5) Uani 1 1 d . . . . .
H1 H -0.3113 -0.3321 0.4590 0.015 Uiso 1 1 calc R . . . .
C2 C -0.1182(3) -0.3439(3) 0.45650(11) 0.0177(6) Uani 1 1 d . . . . .
H2 H -0.0521 -0.2510 0.4487 0.021 Uiso 1 1 calc R . . . .
C3 C -0.5440(3) -0.5792(3) 0.43053(11) 0.0166(6) Uani 1 1 d . . . . .
H3A H -0.5719 -0.5830 0.3971 0.025 Uiso 1 1 calc GR . . . .
H3B H -0.5601 -0.5077 0.4515 0.025 Uiso 1 1 calc GR . . . .
H3C H -0.6034 -0.6705 0.4389 0.025 Uiso 1 1 calc GR . . . .
C4 C -0.3824(3) -0.5424(3) 0.43697(11) 0.0151(6) Uani 1 1 d . . . . .
H4A H -0.3631 -0.6036 0.4113 0.018 Uiso 1 1 calc R . . . .
H4B H -0.3612 -0.5620 0.4681 0.018 Uiso 1 1 calc R . . . .
C5 C 0.3110(12) 0.4101(8) 0.2968(4) 0.0147(15) Uani 0.780(4) 1 d . . . A 1
H5A H 0.3560 0.4782 0.3269 0.022 Uiso 0.780(4) 1 calc GR . . A 1
H5B H 0.2462 0.4348 0.2798 0.022 Uiso 0.780(4) 1 calc GR . . A 1
H5C H 0.3877 0.4107 0.2768 0.022 Uiso 0.780(4) 1 calc GR . . A 1
C6 C -0.1116(3) -0.3257(3) 0.51199(11) 0.0198(6) Uani 1 1 d . . . . .
H6A H -0.1571 -0.2673 0.5246 0.030 Uiso 1 1 calc GR . . . .
H6B H -0.0093 -0.2808 0.5257 0.030 Uiso 1 1 calc GR . . . .
H6C H -0.1642 -0.4176 0.5206 0.030 Uiso 1 1 calc GR . . . .
C7 C -0.2053(3) -0.1934(3) 0.38755(11) 0.0196(6) Uani 1 1 d . . . . .
H7A H -0.2175 -0.1401 0.4169 0.029 Uiso 1 1 calc GR . . . .
H7B H -0.2371 -0.1688 0.3596 0.029 Uiso 1 1 calc GR . . . .
H7C H -0.1021 -0.1710 0.3870 0.029 Uiso 1 1 calc GR . . . .
C8 C -0.0615(3) -0.4483(3) 0.43511(12) 0.0224(7) Uani 1 1 d . . . . .
H8A H -0.1186 -0.5378 0.4449 0.034 Uiso 1 1 calc GR . . . .
H8B H 0.0418 -0.4103 0.4468 0.034 Uiso 1 1 calc GR . . . .
H8C H -0.0717 -0.4626 0.4001 0.034 Uiso 1 1 calc GR . . . .
C9 C -0.2987(3) -0.3515(3) 0.38611(11) 0.0197(6) Uani 1 1 d . . . . .
H9 H -0.4033 -0.3720 0.3814 0.024 Uiso 1 1 calc R . . . .
C10 C -0.2734(4) -0.4407(4) 0.34254(12) 0.0386(8) Uani 1 1 d . . . . .
H10A H -0.1692 -0.4150 0.3434 0.058 Uiso 1 1 calc GR . . . .
H10B H -0.3053 -0.4236 0.3129 0.058 Uiso 1 1 calc GR . . . .
H10C H -0.3298 -0.5400 0.3437 0.058 Uiso 1 1 calc GR . . . .
C5A C 0.031(3) 0.072(3) 0.3369(11) 0.0224(12) Uani 0.220(4) 1 d . . . A 2
H5AA H -0.0625 0.0464 0.3193 0.034 Uiso 0.220(4) 1 calc R . . A 2
H5AB H 0.0321 0.1116 0.3706 0.034 Uiso 0.220(4) 1 calc R . . A 2
H5AC H 0.0455 -0.0110 0.3350 0.034 Uiso 0.220(4) 1 calc R . . A 2
C44A C 0.1589(14) 0.1842(15) 0.3142(5) 0.0144(8) Uani 0.220(4) 1 d . . . A 2
O14A O 0.246(6) 0.169(7) 0.293(2) 0.0167(14) Uani 0.220(4) 1 d . . . A 2
N43A N 0.1708(12) 0.3111(13) 0.3161(4) 0.0169(7) Uani 0.220(4) 1 d . . . A 2
C63A C 0.068(4) 0.376(4) 0.3420(17) 0.0224(14) Uani 0.220(4) 1 d . . . A 2
H63D H 0.0086 0.3863 0.3174 0.034 Uiso 0.220(4) 1 calc GR . . A 2
H63E H 0.1301 0.4670 0.3625 0.034 Uiso 0.220(4) 1 calc GR . . A 2
H63F H 0.0032 0.3118 0.3615 0.034 Uiso 0.220(4) 1 calc GR . . A 2
C56A C 0.310(5) 0.438(4) 0.3019(16) 0.0147(15) Uani 0.220(4) 1 d . . . A 2
H56D H 0.3412 0.5213 0.3271 0.022 Uiso 0.220(4) 1 calc GR . . A 2
H56E H 0.2840 0.4564 0.2716 0.022 Uiso 0.220(4) 1 calc GR . . A 2
H56F H 0.3895 0.4129 0.2981 0.022 Uiso 0.220(4) 1 calc GR . . 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 V2 3.0364(6) . ?
V1 V3 3.0190(6) . ?
V1 O1 1.8688(17) . ?
V1 O3 2.2454(4) . ?
V1 O5 1.7870(17) . ?
V1 O6 2.0402(16) . ?
V1 O0AA 1.9851(15) . ?
V1 O10 1.6030(18) . ?
V2 V3 3.0206(6) 2_656 ?
V2 O2 1.7981(16) . ?
V2 O3 2.2284(4) . ?
V2 O4 2.0411(16) . ?
V2 O5 1.8652(17) . ?
V2 O6 1.9879(17) 2_656 ?
V2 O9 1.6024(17) . ?
V3 V2 3.0206(6) 2_656 ?
V3 O1 1.7715(17) . ?
V3 O2 1.8925(17) 2_656 ?
V3 O3 2.2345(4) . ?
V3 O4 1.9723(16) . ?
V3 O0AA 2.0553(17) 2_656 ?
V3 O8 1.6013(17) . ?
O2 V3 1.8926(16) 2_656 ?
O3 V1 2.2453(4) 2_656 ?
O3 V2 2.2284(4) 2_656 ?
O3 V3 2.2345(4) 2_656 ?
O4 C38 1.421(3) 2_656 ?
O6 V2 1.9879(17) 2_656 ?
O6 C41 1.436(3) . ?
O0AA V3 2.0553(17) 2_656 ?
O0AA C17 1.425(3) . ?
O11 C18 1.228(3) . ?
O12 C21 1.370(3) . ?
O12 C37 1.435(3) . ?
O13 C20 1.435(3) . ?
O13 C29 1.366(3) . ?
N15 H15 0.8600 . ?
N15 C18 1.361(3) . ?
N15 C22 1.469(3) . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C17 C22 1.532(3) . ?
C18 C19 1.506(4) . ?
C19 C27 1.398(4) . ?
C19 C31 1.385(3) . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C20 C35 1.506(4) . ?
C21 C24 1.379(4) . ?
C21 C31 1.395(4) . ?
C22 C38 1.531(3) . ?
C22 C41 1.540(3) . ?
C24 H24 0.9300 . ?
C24 C29 1.400(4) . ?
C27 H27 0.9300 . ?
C27 C29 1.385(4) . ?
C30 H30A 0.9700 . ?
C30 H30B 0.9700 . ?
C30 C32 1.521(4) . ?
C30 C35 1.524(4) . ?
C31 H31 0.9300 . ?
C32 H32A 0.9700 . ?
C32 H32B 0.9700 . ?
C32 C45 1.522(4) . ?
C33 H33A 0.9700 . ?
C33 H33B 0.9700 . ?
C33 C34 1.521(4) . ?
C33 C49 1.526(4) . ?
C34 H34A 0.9700 . ?
C34 H34B 0.9700 . ?
C34 C40 1.522(4) . ?
C35 H35A 0.9700 . ?
C35 H35B 0.9700 . ?
C36 H36A 0.9700 . ?
C36 H36B 0.9700 . ?
C36 C51 1.524(4) . ?
C36 C52 1.510(4) . ?
C37 H37A 0.9700 . ?
C37 H37B 0.9700 . ?
C37 C40 1.509(4) . ?
C38 O4 1.421(3) 2_656 ?
C38 H38A 0.9700 . ?
C38 H38B 0.9700 . ?
C40 H40A 0.9700 . ?
C40 H40B 0.9700 . ?
C41 H41A 0.9700 . ?
C41 H41B 0.9700 . ?
C42 H42A 0.9700 . ?
C42 H42B 0.9700 . ?
C42 C47 1.518(4) . ?
C42 C62 1.518(4) . ?
C45 H45A 0.9700 . ?
C45 H45B 0.9700 . ?
C45 C53 1.523(4) . ?
C46 H46A 0.9700 . ?
C46 H46B 0.9700 . ?
C46 C57 1.507(4) . ?
C46 C59 1.513(4) . ?
C47 H47A 0.9700 . ?
C47 H47B 0.9700 . ?
C47 C50 1.520(4) . ?
C49 H49A 0.9700 . ?
C49 H49B 0.9700 . ?
C49 C51 1.517(4) . ?
C50 H50A 0.9700 . ?
C50 H50B 0.9700 . ?
C50 C52 1.523(4) . ?
C51 H51A 0.9700 . ?
C51 H51B 0.9700 . ?
C52 H52A 0.9700 . ?
C52 H52B 0.9700 . ?
C53 H53A 0.9700 . ?
C53 H53B 0.9700 . ?
C53 C58 1.532(4) . ?
C57 H57A 0.9700 . ?
C57 H57B 0.9700 . ?
C57 C64 1.519(4) . ?
C58 H58A 0.9700 . ?
C58 H58B 0.9700 . ?
C58 C65 1.518(4) . ?
C59 H59A 0.9700 . ?
C59 H59B 0.9700 . ?
C59 C65 1.525(4) . ?
C62 H62A 0.9600 . ?
C62 H62B 0.9600 . ?
C62 H62C 0.9600 . ?
C64 H64A 0.9600 . ?
C64 H64B 0.9600 . ?
C64 H64C 0.9600 . ?
C65 H65A 0.9700 . ?
C65 H65B 0.9700 . ?
O14 C44 1.291(16) . ?
N43 C44 1.339(5) . ?
N43 C56 1.452(7) . ?
N43 C63 1.425(10) . ?
C44 C5 1.487(10) . ?
C56 H56A 0.9600 . ?
C56 H56B 0.9600 . ?
C56 H56C 0.9600 . ?
C63 H63A 0.9600 . ?
C63 H63B 0.9600 . ?
C63 H63C 0.9600 . ?
N1 H1 0.9800 . ?
N1 C2 1.530(3) . ?
N1 C4 1.519(3) . ?
N1 C9 1.535(3) . ?
C2 H2 0.9800 . ?
C2 C6 1.524(4) . ?
C2 C8 1.520(4) . ?
C3 H3A 0.9600 . ?
C3 H3B 0.9600 . ?
C3 H3C 0.9600 . ?
C3 C4 1.497(3) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C5 H5A 0.9600 . ?
C5 H5B 0.9600 . ?
C5 H5C 0.9600 . ?
C6 H6A 0.9600 . ?
C6 H6B 0.9600 . ?
C6 H6C 0.9600 . ?
C7 H7A 0.9600 . ?
C7 H7B 0.9600 . ?
C7 H7C 0.9600 . ?
C7 C9 1.514(4) . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C9 H9 0.9800 . ?
C9 C10 1.515(4) . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C5A H5AA 0.9600 . ?
C5A H5AB 0.9600 . ?
C5A H5AC 0.9600 . ?
C5A C44A 1.54(3) . ?
C44A O14A 1.13(7) . ?
C44A N43A 1.305(19) . ?
N43A C63A 1.61(5) . ?
N43A C56A 1.56(4) . ?
C63A H63D 0.9600 . ?
C63A H63E 0.9600 . ?
C63A H63F 0.9600 . ?
C56A H56D 0.9600 . ?
C56A H56E 0.9600 . ?
C56A H56F 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
V3 V1 V2 65.713(15) . . ?
O1 V1 V2 89.04(5) . . ?
O1 V1 V3 32.95(5) . . ?
O1 V1 O3 80.35(5) . . ?
O1 V1 O6 85.88(7) . . ?
O1 V1 O0AA 156.82(7) . . ?
O3 V1 V2 47.022(12) . . ?
O3 V1 V3 47.478(11) . . ?
O5 V1 V2 34.59(5) . . ?
O5 V1 V3 86.34(6) . . ?
O5 V1 O1 93.76(7) . . ?
O5 V1 O3 81.54(6) . . ?
O5 V1 O6 158.33(7) . . ?
O5 V1 O0AA 90.34(7) . . ?
O6 V1 V2 123.81(5) . . ?
O6 V1 V3 81.62(5) . . ?
O6 V1 O3 77.03(5) . . ?
O0AA V1 V2 81.47(5) . . ?
O0AA V1 V3 124.98(5) . . ?
O0AA V1 O3 77.70(5) . . ?
O0AA V1 O6 82.03(6) . . ?
O10 V1 V2 138.80(6) . . ?
O10 V1 V3 136.61(6) . . ?
O10 V1 O1 103.74(8) . . ?
O10 V1 O3 172.12(6) . . ?
O10 V1 O5 104.69(8) . . ?
O10 V1 O6 96.40(8) . . ?
O10 V1 O0AA 97.23(8) . . ?
V3 V2 V1 66.246(15) 2_656 . ?
O2 V2 V1 87.77(6) . . ?
O2 V2 V3 36.11(5) . 2_656 ?
O2 V2 O3 83.52(5) . . ?
O2 V2 O4 160.17(7) . . ?
O2 V2 O5 94.10(7) . . ?
O2 V2 O6 91.55(7) . 2_656 ?
O3 V2 V1 47.493(12) . . ?
O3 V2 V3 47.489(12) . 2_656 ?
O4 V2 V1 80.64(5) . . ?
O4 V2 V3 124.08(5) . 2_656 ?
O4 V2 O3 76.78(5) . . ?
O5 V2 V1 32.95(5) . . ?
O5 V2 V3 89.36(5) . 2_656 ?
O5 V2 O3 80.38(5) . . ?
O5 V2 O4 84.90(7) . . ?
O5 V2 O6 157.33(7) . 2_656 ?
O6 V2 V1 125.71(5) 2_656 . ?
O6 V2 V3 82.37(5) 2_656 2_656 ?
O6 V2 O3 78.48(5) 2_656 . ?
O6 V2 O4 82.41(7) 2_656 . ?
O9 V2 V1 135.94(6) . . ?
O9 V2 V3 139.86(6) . 2_656 ?
O9 V2 O2 104.24(8) . . ?
O9 V2 O3 171.06(6) . . ?
O9 V2 O4 95.24(7) . . ?
O9 V2 O5 103.16(8) . . ?
O9 V2 O6 96.65(8) . 2_656 ?
V1 V3 V2 65.913(15) . 2_656 ?
O1 V3 V1 35.02(5) . . ?
O1 V3 V2 86.80(5) . 2_656 ?
O1 V3 O2 93.79(8) . 2_656 ?
O1 V3 O3 82.72(5) . . ?
O1 V3 O4 91.22(7) . . ?
O1 V3 O0AA 159.17(7) . 2_656 ?
O2 V3 V1 89.74(5) 2_656 . ?
O2 V3 V2 34.05(5) 2_656 2_656 ?
O2 V3 O3 81.29(5) 2_656 . ?
O2 V3 O4 157.90(7) 2_656 . ?
O2 V3 O0AA 85.32(7) 2_656 2_656 ?
O3 V3 V1 47.783(11) . . ?
O3 V3 V2 47.319(11) . 2_656 ?
O4 V3 V1 82.11(5) . . ?
O4 V3 V2 125.12(5) . 2_656 ?
O4 V3 O3 78.01(5) . . ?
O4 V3 O0AA 82.43(7) . 2_656 ?
O0AA V3 V1 124.17(5) 2_656 . ?
O0AA V3 V2 80.84(5) 2_656 2_656 ?
O0AA V3 O3 76.56(4) 2_656 . ?
O8 V3 V1 139.31(7) . . ?
O8 V3 V2 137.00(6) . 2_656 ?
O8 V3 O1 104.86(8) . . ?
O8 V3 O2 103.11(8) . 2_656 ?
O8 V3 O3 170.78(7) . . ?
O8 V3 O4 96.35(8) . . ?
O8 V3 O0AA 95.58(8) . 2_656 ?
V3 O1 V1 112.03(8) . . ?
V2 O2 V3 109.83(8) . 2_656 ?
V1 O3 V1 180.00(2) 2_656 . ?
V2 O3 V1 85.485(16) . . ?
V2 O3 V1 85.485(16) 2_656 2_656 ?
V2 O3 V1 94.515(16) 2_656 . ?
V2 O3 V1 94.515(16) . 2_656 ?
V2 O3 V2 180.0 . 2_656 ?
V2 O3 V3 94.807(15) 2_656 2_656 ?
V2 O3 V3 85.193(16) . 2_656 ?
V2 O3 V3 85.192(16) 2_656 . ?
V2 O3 V3 94.808(15) . . ?
V3 O3 V1 84.739(16) 2_656 2_656 ?
V3 O3 V1 95.261(16) . 2_656 ?
V3 O3 V1 95.261(16) 2_656 . ?
V3 O3 V1 84.740(16) . . ?
V3 O3 V3 179.999(19) . 2_656 ?
V3 O4 V2 109.88(7) . . ?
C38 O4 V2 118.02(14) 2_656 . ?
C38 O4 V3 119.28(14) 2_656 . ?
V1 O5 V2 112.46(8) . . ?
V2 O6 V1 109.30(8) 2_656 . ?
C41 O6 V1 118.95(14) . . ?
C41 O6 V2 119.79(14) . 2_656 ?
V1 O0AA V3 109.99(8) . 2_656 ?
C17 O0AA V1 119.20(14) . . ?
C17 O0AA V3 117.86(13) . 2_656 ?
C21 O12 C37 117.9(2) . . ?
C29 O13 C20 117.9(2) . . ?
C18 N15 H15 118.3 . . ?
C18 N15 C22 123.3(2) . . ?
C22 N15 H15 118.3 . . ?
O0AA C17 H17A 109.2 . . ?
O0AA C17 H17B 109.2 . . ?
O0AA C17 C22 112.2(2) . . ?
H17A C17 H17B 107.9 . . ?
C22 C17 H17A 109.2 . . ?
C22 C17 H17B 109.2 . . ?
O11 C18 N15 121.8(2) . . ?
O11 C18 C19 120.4(2) . . ?
N15 C18 C19 117.8(2) . . ?
C27 C19 C18 123.9(2) . . ?
C31 C19 C18 115.5(2) . . ?
C31 C19 C27 120.6(2) . . ?
O13 C20 H20A 110.6 . . ?
O13 C20 H20B 110.6 . . ?
O13 C20 C35 105.6(2) . . ?
H20A C20 H20B 108.7 . . ?
C35 C20 H20A 110.6 . . ?
C35 C20 H20B 110.6 . . ?
O12 C21 C24 124.7(2) . . ?
O12 C21 C31 115.2(2) . . ?
C24 C21 C31 120.1(2) . . ?
N15 C22 C17 106.05(19) . . ?
N15 C22 C38 107.99(18) . . ?
N15 C22 C41 111.8(2) . . ?
C17 C22 C41 109.98(19) . . ?
C38 C22 C17 110.3(2) . . ?
C38 C22 C41 110.6(2) . . ?
C21 C24 H24 120.5 . . ?
C21 C24 C29 119.1(2) . . ?
C29 C24 H24 120.5 . . ?
C19 C27 H27 120.8 . . ?
C29 C27 C19 118.4(2) . . ?
C29 C27 H27 120.8 . . ?
O13 C29 C24 113.7(2) . . ?
O13 C29 C27 124.6(2) . . ?
C27 C29 C24 121.6(2) . . ?
H30A C30 H30B 107.6 . . ?
C32 C30 H30A 108.6 . . ?
C32 C30 H30B 108.6 . . ?
C32 C30 C35 114.6(2) . . ?
C35 C30 H30A 108.6 . . ?
C35 C30 H30B 108.6 . . ?
C19 C31 C21 120.2(2) . . ?
C19 C31 H31 119.9 . . ?
C21 C31 H31 119.9 . . ?
C30 C32 H32A 109.0 . . ?
C30 C32 H32B 109.0 . . ?
C30 C32 C45 112.8(2) . . ?
H32A C32 H32B 107.8 . . ?
C45 C32 H32A 109.0 . . ?
C45 C32 H32B 109.0 . . ?
H33A C33 H33B 107.5 . . ?
C34 C33 H33A 108.5 . . ?
C34 C33 H33B 108.5 . . ?
C34 C33 C49 115.3(2) . . ?
C49 C33 H33A 108.5 . . ?
C49 C33 H33B 108.5 . . ?
C33 C34 H34A 109.2 . . ?
C33 C34 H34B 109.2 . . ?
C33 C34 C40 112.0(2) . . ?
H34A C34 H34B 107.9 . . ?
C40 C34 H34A 109.2 . . ?
C40 C34 H34B 109.2 . . ?
C20 C35 C30 113.9(2) . . ?
C20 C35 H35A 108.8 . . ?
C20 C35 H35B 108.8 . . ?
C30 C35 H35A 108.8 . . ?
C30 C35 H35B 108.8 . . ?
H35A C35 H35B 107.7 . . ?
H36A C36 H36B 107.8 . . ?
C51 C36 H36A 109.0 . . ?
C51 C36 H36B 109.0 . . ?
C52 C36 H36A 109.0 . . ?
C52 C36 H36B 109.0 . . ?
C52 C36 C51 113.1(2) . . ?
O12 C37 H37A 110.2 . . ?
O12 C37 H37B 110.2 . . ?
O12 C37 C40 107.5(2) . . ?
H37A C37 H37B 108.5 . . ?
C40 C37 H37A 110.2 . . ?
C40 C37 H37B 110.2 . . ?
O4 C38 C22 112.49(19) 2_656 . ?
O4 C38 H38A 109.1 2_656 . ?
O4 C38 H38B 109.1 2_656 . ?
C22 C38 H38A 109.1 . . ?
C22 C38 H38B 109.1 . . ?
H38A C38 H38B 107.8 . . ?
C34 C40 H40A 108.6 . . ?
C34 C40 H40B 108.6 . . ?
C37 C40 C34 114.6(2) . . ?
C37 C40 H40A 108.6 . . ?
C37 C40 H40B 108.6 . . ?
H40A C40 H40B 107.6 . . ?
O6 C41 C22 110.40(19) . . ?
O6 C41 H41A 109.6 . . ?
O6 C41 H41B 109.6 . . ?
C22 C41 H41A 109.6 . . ?
C22 C41 H41B 109.6 . . ?
H41A C41 H41B 108.1 . . ?
H42A C42 H42B 107.7 . . ?
C47 C42 H42A 108.8 . . ?
C47 C42 H42B 108.8 . . ?
C62 C42 H42A 108.8 . . ?
C62 C42 H42B 108.8 . . ?
C62 C42 C47 114.0(2) . . ?
C32 C45 H45A 108.9 . . ?
C32 C45 H45B 108.9 . . ?
C32 C45 C53 113.5(2) . . ?
H45A C45 H45B 107.7 . . ?
C53 C45 H45A 108.9 . . ?
C53 C45 H45B 108.9 . . ?
H46A C46 H46B 107.6 . . ?
C57 C46 H46A 108.7 . . ?
C57 C46 H46B 108.7 . . ?
C57 C46 C59 114.2(2) . . ?
C59 C46 H46A 108.7 . . ?
C59 C46 H46B 108.7 . . ?
C42 C47 H47A 108.9 . . ?
C42 C47 H47B 108.9 . . ?
C42 C47 C50 113.5(2) . . ?
H47A C47 H47B 107.7 . . ?
C50 C47 H47A 108.9 . . ?
C50 C47 H47B 108.9 . . ?
C33 C49 H49A 109.0 . . ?
C33 C49 H49B 109.0 . . ?
H49A C49 H49B 107.8 . . ?
C51 C49 C33 112.7(2) . . ?
C51 C49 H49A 109.0 . . ?
C51 C49 H49B 109.0 . . ?
C47 C50 H50A 108.8 . . ?
C47 C50 H50B 108.8 . . ?
C47 C50 C52 113.6(2) . . ?
H50A C50 H50B 107.7 . . ?
C52 C50 H50A 108.8 . . ?
C52 C50 H50B 108.8 . . ?
C36 C51 H51A 108.6 . . ?
C36 C51 H51B 108.6 . . ?
C49 C51 C36 114.8(2) . . ?
C49 C51 H51A 108.6 . . ?
C49 C51 H51B 108.6 . . ?
H51A C51 H51B 107.5 . . ?
C36 C52 C50 114.3(2) . . ?
C36 C52 H52A 108.7 . . ?
C36 C52 H52B 108.7 . . ?
C50 C52 H52A 108.7 . . ?
C50 C52 H52B 108.7 . . ?
H52A C52 H52B 107.6 . . ?
C45 C53 H53A 108.8 . . ?
C45 C53 H53B 108.8 . . ?
C45 C53 C58 113.9(2) . . ?
H53A C53 H53B 107.7 . . ?
C58 C53 H53A 108.8 . . ?
C58 C53 H53B 108.8 . . ?
C46 C57 H57A 108.9 . . ?
C46 C57 H57B 108.9 . . ?
C46 C57 C64 113.1(3) . . ?
H57A C57 H57B 107.8 . . ?
C64 C57 H57A 108.9 . . ?
C64 C57 H57B 108.9 . . ?
C53 C58 H58A 108.7 . . ?
C53 C58 H58B 108.7 . . ?
H58A C58 H58B 107.6 . . ?
C65 C58 C53 114.3(3) . . ?
C65 C58 H58A 108.7 . . ?
C65 C58 H58B 108.7 . . ?
C46 C59 H59A 108.6 . . ?
C46 C59 H59B 108.6 . . ?
C46 C59 C65 114.6(2) . . ?
H59A C59 H59B 107.6 . . ?
C65 C59 H59A 108.6 . . ?
C65 C59 H59B 108.6 . . ?
C42 C62 H62A 109.5 . . ?
C42 C62 H62B 109.5 . . ?
C42 C62 H62C 109.5 . . ?
H62A C62 H62B 109.5 . . ?
H62A C62 H62C 109.5 . . ?
H62B C62 H62C 109.5 . . ?
C57 C64 H64A 109.5 . . ?
C57 C64 H64B 109.5 . . ?
C57 C64 H64C 109.5 . . ?
H64A C64 H64B 109.5 . . ?
H64A C64 H64C 109.5 . . ?
H64B C64 H64C 109.5 . . ?
C58 C65 C59 113.9(3) . . ?
C58 C65 H65A 108.8 . . ?
C58 C65 H65B 108.8 . . ?
C59 C65 H65A 108.8 . . ?
C59 C65 H65B 108.8 . . ?
H65A C65 H65B 107.7 . . ?
C44 N43 C56 119.3(3) . . ?
C44 N43 C63 124.0(4) . . ?
C63 N43 C56 116.4(4) . . ?
O14 C44 N43 121.0(9) . . ?
O14 C44 C5 121.6(9) . . ?
N43 C44 C5 117.4(4) . . ?
N43 C56 H56A 109.5 . . ?
N43 C56 H56B 109.5 . . ?
N43 C56 H56C 109.5 . . ?
H56A C56 H56B 109.5 . . ?
H56A C56 H56C 109.5 . . ?
H56B C56 H56C 109.5 . . ?
N43 C63 H63A 109.5 . . ?
N43 C63 H63B 109.5 . . ?
N43 C63 H63C 109.5 . . ?
H63A C63 H63B 109.5 . . ?
H63A C63 H63C 109.5 . . ?
H63B C63 H63C 109.5 . . ?
C2 N1 H1 104.7 . . ?
C2 N1 C9 118.2(2) . . ?
C4 N1 H1 104.7 . . ?
C4 N1 C2 111.43(19) . . ?
C4 N1 C9 111.6(2) . . ?
C9 N1 H1 104.7 . . ?
N1 C2 H2 107.8 . . ?
C6 C2 N1 109.2(2) . . ?
C6 C2 H2 107.8 . . ?
C8 C2 N1 113.3(2) . . ?
C8 C2 H2 107.8 . . ?
C8 C2 C6 110.6(2) . . ?
H3A C3 H3B 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
C4 C3 H3A 109.5 . . ?
C4 C3 H3B 109.5 . . ?
C4 C3 H3C 109.5 . . ?
N1 C4 H4A 108.9 . . ?
N1 C4 H4B 108.9 . . ?
C3 C4 N1 113.5(2) . . ?
C3 C4 H4A 108.9 . . ?
C3 C4 H4B 108.9 . . ?
H4A C4 H4B 107.7 . . ?
C44 C5 H5A 109.5 . . ?
C44 C5 H5B 109.5 . . ?
C44 C5 H5C 109.5 . . ?
H5A C5 H5B 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C2 C6 H6A 109.5 . . ?
C2 C6 H6B 109.5 . . ?
C2 C6 H6C 109.5 . . ?
H6A C6 H6B 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C9 C7 H7A 109.5 . . ?
C9 C7 H7B 109.5 . . ?
C9 C7 H7C 109.5 . . ?
C2 C8 H8A 109.5 . . ?
C2 C8 H8B 109.5 . . ?
C2 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N1 C9 H9 106.5 . . ?
C7 C9 N1 110.5(2) . . ?
C7 C9 H9 106.5 . . ?
C7 C9 C10 111.6(2) . . ?
C10 C9 N1 114.6(2) . . ?
C10 C9 H9 106.5 . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
H5AA C5A H5AB 109.5 . . ?
H5AA C5A H5AC 109.5 . . ?
H5AB C5A H5AC 109.5 . . ?
C44A C5A H5AA 109.5 . . ?
C44A C5A H5AB 109.5 . . ?
C44A C5A H5AC 109.5 . . ?
O14A C44A C5A 127(4) . . ?
O14A C44A N43A 112(4) . . ?
N43A C44A C5A 120.8(14) . . ?
C44A N43A C63A 127.9(15) . . ?
C44A N43A C56A 123.7(16) . . ?
C56A N43A C63A 107.4(17) . . ?
N43A C63A H63D 109.5 . . ?
N43A C63A H63E 109.5 . . ?
N43A C63A H63F 109.5 . . ?
H63D C63A H63E 109.5 . . ?
H63D C63A H63F 109.5 . . ?
H63E C63A H63F 109.5 . . ?
N43A C56A H56D 109.5 . . ?
N43A C56A H56E 109.5 . . ?
N43A C56A H56F 109.5 . . ?
H56D C56A H56E 109.5 . . ?
H56D C56A H56F 109.5 . . ?
H56E C56A H56F 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
V1 V2 O2 V3 50.90(7) . . . 2_656 ?
V1 O6 C41 C22 -68.8(2) . . . . ?
V1 O0AA C17 C22 70.1(2) . . . . ?
V2 V1 O1 V3 43.07(8) . . . . ?
V2 V3 O1 V1 50.76(7) 2_656 . . . ?
V2 O6 C41 C22 69.9(2) 2_656 . . . ?
V3 V1 O5 V2 -50.71(7) . . . . ?
V3 V2 O5 V1 -43.67(8) 2_656 . . . ?
V3 O0AA C17 C22 -67.5(2) 2_656 . . . ?
O1 V1 O5 V2 -82.83(9) . . . . ?
O2 V2 O5 V1 -79.50(9) . . . . ?
O2 V3 O1 V1 84.11(9) 2_656 . . . ?
O3 V1 O1 V3 -3.40(7) . . . . ?
O3 V1 O5 V2 -3.18(7) . . . . ?
O3 V2 O2 V3 3.44(7) . . . 2_656 ?
O3 V2 O5 V1 3.21(7) . . . . ?
O3 V3 O1 V1 3.40(7) . . . . ?
O4 V2 O2 V3 -3.1(3) . . . 2_656 ?
O4 V2 O5 V1 80.64(9) . . . . ?
O4 V3 O1 V1 -74.35(9) . . . . ?
O5 V1 O1 V3 77.35(9) . . . . ?
O5 V2 O2 V3 83.25(9) . . . 2_656 ?
O6 V1 O1 V3 -80.93(9) . . . . ?
O6 V1 O5 V2 5.5(2) . . . . ?
O6 V2 O2 V3 -74.78(9) 2_656 . . 2_656 ?
O6 V2 O5 V1 24.5(2) 2_656 . . . ?
O0AA V1 O1 V3 -22.3(2) . . . . ?
O0AA V1 O5 V2 74.33(9) . . . . ?
O0AA V3 O1 V1 -2.7(3) 2_656 . . . ?
O0AA C17 C22 N15 176.86(18) . . . . ?
O0AA C17 C22 C38 60.2(2) . . . . ?
O0AA C17 C22 C41 -62.1(3) . . . . ?
O8 V3 O1 V1 -171.25(9) . . . . ?
O9 V2 O2 V3 -172.05(9) . . . 2_656 ?
O9 V2 O5 V1 174.84(9) . . . . ?
O10 V1 O1 V3 -176.52(9) . . . . ?
O10 V1 O5 V2 171.90(9) . . . . ?
O11 C18 C19 C27 -173.6(2) . . . . ?
O11 C18 C19 C31 7.9(4) . . . . ?
O12 C21 C24 C29 -177.1(2) . . . . ?
O12 C21 C31 C19 177.9(2) . . . . ?
O12 C37 C40 C34 -70.5(3) . . . . ?
O13 C20 C35 C30 -179.9(2) . . . . ?
N15 C18 C19 C27 7.5(4) . . . . ?
N15 C18 C19 C31 -171.0(2) . . . . ?
N15 C22 C38 O4 -175.77(19) . . . 2_656 ?
N15 C22 C41 O6 178.87(18) . . . . ?
C17 C22 C38 O4 -60.3(3) . . . 2_656 ?
C17 C22 C41 O6 61.4(3) . . . . ?
C18 N15 C22 C17 -174.6(2) . . . . ?
C18 N15 C22 C38 -56.4(3) . . . . ?
C18 N15 C22 C41 65.5(3) . . . . ?
C18 C19 C27 C29 -178.1(2) . . . . ?
C18 C19 C31 C21 178.7(2) . . . . ?
C19 C27 C29 O13 -179.3(2) . . . . ?
C19 C27 C29 C24 0.5(4) . . . . ?
C20 O13 C29 C24 179.8(2) . . . . ?
C20 O13 C29 C27 -0.4(4) . . . . ?
C21 O12 C37 C40 -178.5(2) . . . . ?
C21 C24 C29 O13 178.1(2) . . . . ?
C21 C24 C29 C27 -1.7(4) . . . . ?
C22 N15 C18 O11 -13.7(4) . . . . ?
C22 N15 C18 C19 165.1(2) . . . . ?
C24 C21 C31 C19 -1.4(4) . . . . ?
C27 C19 C31 C21 0.2(4) . . . . ?
C29 O13 C20 C35 -179.0(2) . . . . ?
C30 C32 C45 C53 -175.8(2) . . . . ?
C31 C19 C27 C29 0.3(4) . . . . ?
C31 C21 C24 C29 2.2(4) . . . . ?
C32 C30 C35 C20 70.0(3) . . . . ?
C32 C45 C53 C58 176.8(3) . . . . ?
C33 C34 C40 C37 173.2(2) . . . . ?
C33 C49 C51 C36 -178.2(3) . . . . ?
C34 C33 C49 C51 -179.6(3) . . . . ?
C35 C30 C32 C45 174.3(2) . . . . ?
C37 O12 C21 C24 -1.0(4) . . . . ?
C37 O12 C21 C31 179.7(2) . . . . ?
C38 C22 C41 O6 -60.7(2) . . . . ?
C41 C22 C38 O4 61.6(3) . . . 2_656 ?
C42 C47 C50 C52 177.5(3) . . . . ?
C45 C53 C58 C65 69.3(3) . . . . ?
C46 C59 C65 C58 66.0(3) . . . . ?
C47 C50 C52 C36 -178.5(2) . . . . ?
C49 C33 C34 C40 178.1(2) . . . . ?
C51 C36 C52 C50 179.0(3) . . . . ?
C52 C36 C51 C49 -175.8(3) . . . . ?
C53 C58 C65 C59 179.7(2) . . . . ?
C57 C46 C59 C65 179.8(3) . . . . ?
C59 C46 C57 C64 -176.8(3) . . . . ?
C62 C42 C47 C50 177.9(3) . . . . ?
C56 N43 C44 O14 2.5(9) . . . . ?
C56 N43 C44 C5 -177.2(6) . . . . ?
C63 N43 C44 O14 176.2(9) . . . . ?
C63 N43 C44 C5 -3.6(8) . . . . ?
C2 N1 C4 C3 163.7(2) . . . . ?
C2 N1 C9 C7 -55.1(3) . . . . ?
C2 N1 C9 C10 72.0(3) . . . . ?
C4 N1 C2 C6 -74.3(3) . . . . ?
C4 N1 C2 C8 49.5(3) . . . . ?
C4 N1 C9 C7 173.7(2) . . . . ?
C4 N1 C9 C10 -59.2(3) . . . . ?
C9 N1 C2 C6 154.5(2) . . . . ?
C9 N1 C2 C8 -81.8(3) . . . . ?
C9 N1 C4 C3 -61.8(3) . . . . ?
C5A C44A N43A C63A 2(3) . . . . ?
C5A C44A N43A C56A 170(2) . . . . ?
O14A C44A N43A C63A 179(4) . . . . ?
O14A C44A N43A C56A -13(4) . . . . ?

_olex2_date_sample_data_collection 2017-12-03
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.287
_oxdiff_exptl_absorpt_empirical_full_min 0.591
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: acetonitrile/water'
####################################################################### 
# 
# 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_16-1
_database_code_depnum_ccdc_archive 'CCDC 1974737'
loop_
_audit_author_name
_audit_author_address
'Zicheng Xiao'
;Hubei University of Technology
China
;
_audit_update_record             
;
2019-12-30 deposited with the CCDC.	2020-03-13 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C74 H132 N6 O23 V6'
_chemical_formula_weight         1779.49

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                   21.3920(12)
_cell_length_b                   10.9779(7)
_cell_length_c                   19.1098(11)
_cell_angle_alpha                90
_cell_angle_beta                 105.252(2)
_cell_angle_gamma                90
_cell_volume                     4329.7(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    4760
_cell_measurement_theta_min      2.250
_cell_measurement_theta_max      24.614

_exptl_crystal_description       block
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.365
_exptl_crystal_F_000             1880
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.230
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.140
_exptl_absorpt_coefficient_mu    0.693
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5978
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0972 before and 0.0564 after correction.
The Ratio of minimum to maximum transmission is 0.8018.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            33793
_diffrn_reflns_av_unetI/netI     0.1125
_diffrn_reflns_av_R_equivalents  0.0914
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         2.101
_diffrn_reflns_theta_max         27.520
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             9951
_reflns_number_gt                5094
_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       'SAINT v8.37A (Bruker, 2015)'
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_structure_solution    'SHELXS-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_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)+(0.0010P)²+38.8183P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         9951
_refine_ls_number_parameters     500
_refine_ls_number_restraints     137
_refine_ls_R_factor_all          0.2423
_refine_ls_R_factor_gt           0.1347
_refine_ls_wR_factor_ref         0.2445
_refine_ls_wR_factor_gt          0.2015
_refine_ls_goodness_of_fit_ref   1.113
_refine_ls_restrained_S_all      1.111
_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
V2 V 0.42158(6) 0.47701(18) 0.55593(6) 0.0532(5) Uani 1 1 d . . . . .
V3 V 0.53585(6) 0.30679(18) 0.51726(7) 0.0525(5) Uani 1 1 d . . . . .
O1 O 0.4685(2) 0.2949(6) 0.4229(2) 0.0481(16) Uani 1 1 d . . . . .
O2 O 0.4568(2) 0.3085(6) 0.5569(2) 0.0516(17) Uani 1 1 d . . . . .
O3 O 0.3764(2) 0.4331(6) 0.4518(2) 0.0498(17) Uani 1 1 d . . . . .
O4 O 0.5000 0.5000 0.5000 0.044(2) Uani 1 2 d S . P . .
O5 O 0.5795(2) 0.3737(6) 0.6077(2) 0.0488(16) Uani 1 1 d . . . . .
O6 O 0.4861(2) 0.5142(6) 0.6341(2) 0.0517(17) Uani 1 1 d . . . . .
O7 O 0.4067(2) 0.6392(6) 0.5276(2) 0.0520(17) Uani 1 1 d . . . . .
O8 O 0.3614(2) 0.4432(7) 0.5874(3) 0.0608(19) Uani 1 1 d . . . . .
O9 O 0.3879(2) 0.4233(6) 0.3139(3) 0.0546(18) Uani 1 1 d . . . . .
C1 C 0.3751(4) 0.2106(10) 0.4582(4) 0.051(3) Uani 1 1 d . . . . .
N1 N 0.3325(3) 0.1045(8) 0.4486(3) 0.054(2) Uani 1 1 d . . . . .
H1 H 0.3348 0.0608 0.4865 0.065 Uiso 1 1 calc R U . . .
O11 O 0.2808(3) 0.1254(7) 0.3299(3) 0.070(2) Uani 1 1 d . . . . .
C3 C 0.3365(4) 0.3284(10) 0.4395(4) 0.058(3) Uani 1 1 d . . . . .
H3A H 0.3124 0.3262 0.3888 0.069 Uiso 1 1 calc R U . . .
H3B H 0.3056 0.3338 0.4685 0.069 Uiso 1 1 calc R U . . .
C4 C 0.4132(4) 0.2096(11) 0.5393(4) 0.061(3) Uani 1 1 d . . . . .
H4A H 0.3828 0.2133 0.5691 0.073 Uiso 1 1 calc R U . . .
H4B H 0.4371 0.1338 0.5502 0.073 Uiso 1 1 calc R U . . .
C5 C 0.2896(4) 0.0673(10) 0.3864(4) 0.056(3) Uani 1 1 d . . . . .
O10 O 0.5505(2) 0.1636(7) 0.5290(3) 0.0583(18) Uani 1 1 d . . . . .
C6 C 0.2571(4) -0.0498(10) 0.3916(4) 0.055(3) Uani 1 1 d . . . . .
C8 C 0.2557(4) -0.2530(10) 0.4366(4) 0.057(3) Uani 1 1 d . . . . .
H8 H 0.2767 -0.3160 0.4661 0.068 Uiso 1 1 calc R U . . .
C2 C 0.4236(4) 0.1970(10) 0.4120(4) 0.054(3) Uani 1 1 d . . . . .
H2A H 0.4470 0.1210 0.4243 0.064 Uiso 1 1 calc R U . . .
H2B H 0.4001 0.1937 0.3612 0.064 Uiso 1 1 calc R U . . .
O12 O 0.1565(4) -0.3713(10) 0.3932(4) 0.101(3) Uani 1 1 d . . . . .
C7 C 0.2866(4) -0.1449(10) 0.4351(4) 0.053(3) Uani 1 1 d . . . . .
H7 H 0.3286 -0.1350 0.4641 0.064 Uiso 1 1 calc R U . . .
C9 C 0.1929(4) -0.2688(13) 0.3942(5) 0.076(4) Uani 1 1 d . . . . .
C11 C 0.1944(4) -0.0682(12) 0.3473(5) 0.073(4) Uani 1 1 d . . . . .
H11 H 0.1745 -0.0072 0.3153 0.088 Uiso 1 1 calc R U . . .
C10 C 0.1620(4) -0.1739(14) 0.3504(5) 0.086(4) Uani 1 1 d . . . . .
H10 H 0.1193 -0.1826 0.3232 0.103 Uiso 1 1 calc R U . . .
C16 C 0.1364(5) -0.8876(12) 0.4887(9) 0.118(4) Uani 1 1 d D U . . .
H16A H 0.1557 -0.8660 0.5389 0.141 Uiso 1 1 calc R U . . .
H16B H 0.1712 -0.9146 0.4685 0.141 Uiso 1 1 calc R U . . .
C15 C 0.1075(6) -0.7766(13) 0.4495(9) 0.140(5) Uani 1 1 d D U . . .
H15A H 0.0724 -0.7482 0.4686 0.168 Uiso 1 1 calc R U . . .
H15B H 0.0898 -0.7952 0.3985 0.168 Uiso 1 1 calc R U . . .
C17 C 0.0912(5) -0.9934(12) 0.4871(9) 0.124(5) Uani 1 1 d D U . . .
H17A H 0.0551 -0.9663 0.5050 0.149 Uiso 1 1 calc R U . . .
H17B H 0.0739 -1.0194 0.4372 0.149 Uiso 1 1 calc R U . . .
C12 C 0.1856(5) -0.4689(14) 0.4327(7) 0.098(4) Uani 1 1 d D U . . .
H12 H 0.2283 -0.4748 0.4605 0.117 Uiso 1 1 calc R U . . .
C18 C 0.1224(5) -1.0990(11) 0.5309(7) 0.097(4) Uani 1 1 d D U . . .
H18A H 0.1417 -1.0713 0.5800 0.117 Uiso 1 1 calc R U . . .
H18B H 0.1573 -1.1277 0.5114 0.117 Uiso 1 1 calc R U . . .
C20 C 0.1111(5) -1.3077(10) 0.5809(7) 0.092(3) Uani 1 1 d D U . . .
H20A H 0.1459 -1.3378 0.5618 0.110 Uiso 1 1 calc R U . . .
H20B H 0.1306 -1.2760 0.6291 0.110 Uiso 1 1 calc R U . . .
C14 C 0.1594(5) -0.6753(12) 0.4579(7) 0.106(4) Uani 1 1 d D U . . .
H14A H 0.1773 -0.6581 0.5091 0.127 Uiso 1 1 calc R U . . .
H14B H 0.1943 -0.7041 0.4385 0.127 Uiso 1 1 calc R U . . .
C13 C 0.1332(6) -0.5657(13) 0.4214(8) 0.123(5) Uani 1 1 d D U . . .
H13A H 0.0979 -0.5369 0.4400 0.148 Uiso 1 1 calc R U . . .
H13B H 0.1163 -0.5817 0.3699 0.148 Uiso 1 1 calc R U . . .
C19 C 0.0789(5) -1.2046(11) 0.5341(8) 0.112(4) Uani 1 1 d D U . . .
H19A H 0.0431 -1.1757 0.5520 0.134 Uiso 1 1 calc R U . . .
H19B H 0.0610 -1.2349 0.4853 0.134 Uiso 1 1 calc R U . . .
V1 V 0.43579(6) 0.46446(18) 0.38929(6) 0.0518(5) Uani 1 1 d . . . . .
N2 N 0.3877(3) 0.7653(8) 0.7529(3) 0.059(2) Uani 1 1 d . U . . .
H2 H 0.4029 0.8242 0.7923 0.071 Uiso 1 1 calc R U . . .
C33 C 0.2772(4) 0.8359(12) 0.7543(5) 0.082(4) Uani 1 1 d . . . . .
H33A H 0.2608 0.7611 0.7686 0.123 Uiso 1 1 calc R U . . .
H33B H 0.2420 0.8823 0.7247 0.123 Uiso 1 1 calc R U . . .
H33C H 0.2978 0.8821 0.7968 0.123 Uiso 1 1 calc R U . . .
C36 C 0.5053(4) 0.7279(11) 0.7678(4) 0.074(3) Uani 1 1 d . . . . .
H36A H 0.5137 0.7823 0.8085 0.111 Uiso 1 1 calc R U . . .
H36B H 0.5389 0.7361 0.7433 0.111 Uiso 1 1 calc R U . . .
H36C H 0.5043 0.6456 0.7843 0.111 Uiso 1 1 calc R U . . .
C31 C 0.3241(5) 0.8091(17) 0.7131(6) 0.121(6) Uani 1 1 d . . . . .
H31 H 0.3330 0.8889 0.6949 0.146 Uiso 1 1 calc R U . . .
C34 C 0.4400(5) 0.7594(17) 0.7155(6) 0.124(7) Uani 1 1 d . . . . .
H34 H 0.4291 0.6932 0.6800 0.149 Uiso 1 1 calc R U . . .
C38 C 0.3817(8) 0.5324(13) 0.7494(7) 0.123(5) Uani 1 1 d . U . . .
H38A H 0.3456 0.5396 0.7074 0.184 Uiso 1 1 calc R U . . .
H38B H 0.3764 0.4610 0.7763 0.184 Uiso 1 1 calc R U . . .
H38C H 0.4211 0.5258 0.7345 0.184 Uiso 1 1 calc R U . . .
C37 C 0.3847(9) 0.6357(14) 0.7933(6) 0.150(7) Uani 1 1 d . U . . .
H37A H 0.4227 0.6290 0.8341 0.180 Uiso 1 1 calc R U . . .
H37B H 0.3469 0.6359 0.8125 0.180 Uiso 1 1 calc R U . . .
C35 C 0.4362(8) 0.8842(13) 0.6708(9) 0.157(8) Uani 1 1 d . . . . .
H35A H 0.4035 0.8773 0.6257 0.236 Uiso 1 1 calc R U . . .
H35B H 0.4774 0.8999 0.6613 0.236 Uiso 1 1 calc R U . . .
H35C H 0.4256 0.9500 0.6986 0.236 Uiso 1 1 calc R U . . .
C32 C 0.2942(5) 0.7353(16) 0.6434(6) 0.142(7) Uani 1 1 d . . . . .
H32A H 0.3258 0.7257 0.6162 0.213 Uiso 1 1 calc R U . . .
H32B H 0.2572 0.7777 0.6144 0.213 Uiso 1 1 calc R U . . .
H32C H 0.2812 0.6565 0.6562 0.213 Uiso 1 1 calc R U . . .
N3 N 0.2945(4) 0.0704(10) 0.6016(4) 0.083(3) Uani 1 1 d . . . . .
C41 C 0.2891(4) 0.1455(12) 0.6389(4) 0.063(3) Uani 1 1 d . . . . .
C42 C 0.2861(5) 0.2454(12) 0.6861(5) 0.094(4) Uani 1 1 d . . . . .
H42A H 0.2434 0.2803 0.6725 0.141 Uiso 1 1 calc R U . . .
H42B H 0.3173 0.3060 0.6820 0.141 Uiso 1 1 calc R U . . .
H42C H 0.2955 0.2168 0.7352 0.141 Uiso 1 1 calc R U . . .
C22 C 0.1020(6) -1.5189(11) 0.6295(7) 0.104(4) Uani 1 1 d D U . . .
H22A H 0.1247 -1.4909 0.6777 0.124 Uiso 1 1 calc R U . . .
H22B H 0.1345 -1.5478 0.6064 0.124 Uiso 1 1 calc R U . . .
C24 C 0.0939(8) -1.7354(13) 0.6722(7) 0.127(5) Uani 1 1 d D U . . .
H24A H 0.1211 -1.7134 0.7196 0.153 Uiso 1 1 calc R U . . .
H24B H 0.1223 -1.7637 0.6435 0.153 Uiso 1 1 calc R U . . .
C21 C 0.0689(5) -1.4126(11) 0.5878(8) 0.113(4) Uani 1 1 d D U . . .
H21A H 0.0362 -1.3838 0.6106 0.136 Uiso 1 1 calc R U . . .
H21B H 0.0466 -1.4401 0.5394 0.136 Uiso 1 1 calc R U . . .
C23 C 0.0607(7) -1.6243(12) 0.6377(9) 0.137(6) Uani 1 1 d D U . . .
H23A H 0.0315 -1.5974 0.6657 0.164 Uiso 1 1 calc R U . . .
H23B H 0.0343 -1.6462 0.5898 0.164 Uiso 1 1 calc R U . . .
C26 C 0.0846(10) -1.9552(16) 0.7074(8) 0.194(8) Uani 1 1 d D U . . .
H26A H 0.1164 -1.9400 0.7531 0.233 Uiso 1 1 calc R U . . .
H26B H 0.1080 -1.9815 0.6729 0.233 Uiso 1 1 calc R U . . .
C25 C 0.0514(9) -1.8396(14) 0.6815(9) 0.186(8) Uani 1 1 d D U . . .
H25A H 0.0272 -1.8147 0.7154 0.223 Uiso 1 1 calc R U . . .
H25B H 0.0204 -1.8547 0.6352 0.223 Uiso 1 1 calc R U . . .
C27 C 0.0413(12) -2.0579(18) 0.7183(9) 0.266(14) Uani 1 1 d D U . . .
H27A H 0.0092 -2.0734 0.6736 0.398 Uiso 1 1 calc R U . . .
H27B H 0.0204 -2.0357 0.7551 0.398 Uiso 1 1 calc R U . . .
H27C H 0.0669 -2.1299 0.7330 0.398 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
V2 O8 1.600(5) . ?
V2 O6 1.794(5) . ?
V2 O7 1.863(7) . ?
V2 O2 1.996(7) . ?
V2 O3 2.028(5) . ?
V2 O4 2.2280(12) . ?
V2 V3 3.015(2) 3_666 ?
V2 V1 3.0230(19) 3_666 ?
V3 O10 1.607(7) . ?
V3 O7 1.775(5) 3_666 ?
V3 O5 1.884(5) . ?
V3 O1 1.994(5) . ?
V3 O2 2.027(5) . ?
V3 O4 2.2501(19) . ?
V3 V2 3.015(2) 3_666 ?
V3 V1 3.048(2) 3_666 ?
O1 C2 1.419(10) . ?
O1 V1 2.033(7) . ?
O2 C4 1.413(11) . ?
O3 C3 1.413(11) . ?
O3 V1 1.990(5) . ?
O4 V2 2.2280(12) 3_666 ?
O4 V1 2.2329(12) 3_666 ?
O4 V1 2.2330(12) . ?
O4 V3 2.2501(19) 3_666 ?
O5 V1 1.810(7) 3_666 ?
O6 V1 1.854(5) 3_666 ?
O7 V3 1.775(5) 3_666 ?
O9 V1 1.597(5) . ?
C1 N1 1.460(11) . ?
C1 C3 1.525(13) . ?
C1 C2 1.535(9) . ?
C1 C4 1.550(9) . ?
N1 C5 1.360(9) . ?
O11 C5 1.226(10) . ?
C5 C6 1.477(14) . ?
C6 C7 1.380(13) . ?
C6 C11 1.399(11) . ?
C8 C7 1.363(13) . ?
C8 C9 1.385(11) . ?
O12 C12 1.364(15) . ?
O12 C9 1.364(13) . ?
C9 C10 1.389(16) . ?
C11 C10 1.361(16) . ?
C16 C15 1.478(13) . ?
C16 C17 1.507(13) . ?
C15 C14 1.548(13) . ?
C17 C18 1.484(13) . ?
C12 C13 1.519(13) . ?
C18 C19 1.497(12) . ?
C20 C21 1.491(12) . ?
C20 C19 1.493(12) . ?
C14 C13 1.430(13) . ?
V1 O5 1.810(7) 3_666 ?
V1 O6 1.854(5) 3_666 ?
V1 V2 3.0230(19) 3_666 ?
V1 V3 3.049(2) 3_666 ?
N2 C31 1.455(12) . ?
N2 C34 1.479(12) . ?
N2 C37 1.629(15) . ?
C33 C31 1.459(12) . ?
C36 C34 1.528(14) . ?
C31 C32 1.547(15) . ?
C34 C35 1.61(2) . ?
C38 C37 1.402(17) . ?
N3 C41 1.115(13) . ?
C41 C42 1.431(15) . ?
C22 C21 1.485(13) . ?
C22 C23 1.489(13) . ?
C24 C23 1.477(13) . ?
C24 C25 1.499(15) . ?
C26 C25 1.475(15) . ?
C26 C27 1.507(16) . ?

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
O8 V2 O6 105.0(2) . . ?
O8 V2 O7 103.8(3) . . ?
O6 V2 O7 93.4(3) . . ?
O8 V2 O2 96.9(3) . . ?
O6 V2 O2 89.9(3) . . ?
O7 V2 O2 157.4(2) . . ?
O8 V2 O3 95.2(2) . . ?
O6 V2 O3 159.2(2) . . ?
O7 V2 O3 86.7(2) . . ?
O2 V2 O3 82.5(2) . . ?
O8 V2 O4 171.0(2) . . ?
O6 V2 O4 82.06(15) . . ?
O7 V2 O4 81.07(15) . . ?
O2 V2 O4 77.26(15) . . ?
O3 V2 O4 77.36(14) . . ?
O8 V2 V3 136.7(3) . 3_666 ?
O6 V2 V3 86.9(2) . 3_666 ?
O7 V2 V3 33.11(15) . 3_666 ?
O2 V2 V3 125.08(15) . 3_666 ?
O3 V2 V3 81.74(19) . 3_666 ?
O4 V2 V3 47.99(4) . 3_666 ?
O8 V2 V1 139.2(2) . 3_666 ?
O6 V2 V1 34.69(14) . 3_666 ?
O7 V2 V1 88.67(17) . 3_666 ?
O2 V2 V1 81.37(16) . 3_666 ?
O3 V2 V1 124.58(14) . 3_666 ?
O4 V2 V1 47.41(3) . 3_666 ?
V3 V2 V1 65.97(5) 3_666 3_666 ?
O10 V3 O7 105.1(3) . 3_666 ?
O10 V3 O5 102.9(3) . . ?
O7 V3 O5 94.3(2) 3_666 . ?
O10 V3 O1 97.4(3) . . ?
O7 V3 O1 90.7(2) 3_666 . ?
O5 V3 O1 157.0(3) . . ?
O10 V3 O2 96.2(3) . . ?
O7 V3 O2 158.3(3) 3_666 . ?
O5 V3 O2 85.1(2) . . ?
O1 V3 O2 82.08(18) . . ?
O10 V3 O4 171.5(2) . . ?
O7 V3 O4 82.3(2) 3_666 . ?
O5 V3 O4 80.4(2) . . ?
O1 V3 O4 78.0(2) . . ?
O2 V3 O4 76.1(2) . . ?
O10 V3 V2 139.8(2) . 3_666 ?
O7 V3 V2 35.0(2) 3_666 3_666 ?
O5 V3 V2 88.9(2) . 3_666 ?
O1 V3 V2 82.37(19) . 3_666 ?
O2 V3 V2 123.4(2) . 3_666 ?
O4 V3 V2 47.37(4) . 3_666 ?
O10 V3 V1 136.3(2) . 3_666 ?
O7 V3 V1 87.2(2) 3_666 3_666 ?
O5 V3 V1 33.6(2) . 3_666 ?
O1 V3 V1 124.7(2) . 3_666 ?
O2 V3 V1 80.26(19) . 3_666 ?
O4 V3 V1 46.92(4) . 3_666 ?
V2 V3 V1 65.51(5) 3_666 3_666 ?
C2 O1 V3 118.9(5) . . ?
C2 O1 V1 118.9(5) . . ?
V3 O1 V1 109.4(3) . . ?
C4 O2 V2 119.1(5) . . ?
C4 O2 V3 117.9(5) . . ?
V2 O2 V3 110.8(3) . . ?
C3 O3 V1 119.5(4) . . ?
C3 O3 V2 117.9(4) . . ?
V1 O3 V2 109.5(2) . . ?
V2 O4 V2 180.0 . 3_666 ?
V2 O4 V1 85.32(5) . 3_666 ?
V2 O4 V1 94.68(5) 3_666 3_666 ?
V2 O4 V1 94.68(5) . . ?
V2 O4 V1 85.32(5) 3_666 . ?
V1 O4 V1 180.00(6) 3_666 . ?
V2 O4 V3 84.63(6) . 3_666 ?
V2 O4 V3 95.37(6) 3_666 3_666 ?
V1 O4 V3 94.31(6) 3_666 3_666 ?
V1 O4 V3 85.69(6) . 3_666 ?
V2 O4 V3 95.37(6) . . ?
V2 O4 V3 84.63(6) 3_666 . ?
V1 O4 V3 85.69(6) 3_666 . ?
V1 O4 V3 94.31(6) . . ?
V3 O4 V3 180.0 3_666 . ?
V1 O5 V3 111.2(3) 3_666 . ?
V2 O6 V1 111.9(2) . 3_666 ?
V3 O7 V2 111.9(3) 3_666 . ?
N1 C1 C3 111.4(7) . . ?
N1 C1 C2 110.2(7) . . ?
C3 C1 C2 110.7(7) . . ?
N1 C1 C4 105.4(7) . . ?
C3 C1 C4 110.5(7) . . ?
C2 C1 C4 108.5(6) . . ?
C5 N1 C1 127.2(7) . . ?
O3 C3 C1 112.7(6) . . ?
O2 C4 C1 111.9(7) . . ?
O11 C5 N1 121.7(9) . . ?
O11 C5 C6 123.2(7) . . ?
N1 C5 C6 115.1(8) . . ?
C7 C6 C11 118.0(10) . . ?
C7 C6 C5 123.3(7) . . ?
C11 C6 C5 118.6(9) . . ?
C7 C8 C9 119.9(10) . . ?
O1 C2 C1 112.1(7) . . ?
C12 O12 C9 117.7(9) . . ?
C8 C7 C6 121.5(8) . . ?
O12 C9 C8 124.9(11) . . ?
O12 C9 C10 115.5(9) . . ?
C8 C9 C10 119.5(11) . . ?
C10 C11 C6 121.0(10) . . ?
C11 C10 C9 119.9(9) . . ?
C15 C16 C17 116.4(10) . . ?
C16 C15 C14 110.2(10) . . ?
C18 C17 C16 113.5(10) . . ?
O12 C12 C13 105.0(10) . . ?
C17 C18 C19 115.8(9) . . ?
C21 C20 C19 116.3(9) . . ?
C13 C14 C15 112.1(10) . . ?
C14 C13 C12 109.9(11) . . ?
C20 C19 C18 114.7(9) . . ?
O9 V1 O5 103.2(3) . 3_666 ?
O9 V1 O6 102.9(2) . 3_666 ?
O5 V1 O6 93.7(3) 3_666 3_666 ?
O9 V1 O3 97.7(2) . . ?
O5 V1 O3 90.1(3) 3_666 . ?
O6 V1 O3 157.6(2) 3_666 . ?
O9 V1 O1 96.4(3) . . ?
O5 V1 O1 159.8(2) 3_666 . ?
O6 V1 O1 86.3(2) 3_666 . ?
O3 V1 O1 82.7(2) . . ?
O9 V1 O4 173.0(3) . . ?
O5 V1 O4 82.49(16) 3_666 . ?
O6 V1 O4 80.64(15) 3_666 . ?
O3 V1 O4 78.00(14) . . ?
O1 V1 O4 77.62(14) . . ?
O9 V1 V2 136.18(18) . 3_666 ?
O5 V1 V2 87.38(16) 3_666 3_666 ?
O6 V1 V2 33.40(14) 3_666 3_666 ?
O3 V1 V2 125.07(15) . 3_666 ?
O1 V1 V2 81.57(15) . 3_666 ?
O4 V1 V2 47.27(3) . 3_666 ?
O9 V1 V3 138.0(3) . 3_666 ?
O5 V1 V3 35.16(15) 3_666 3_666 ?
O6 V1 V3 89.1(2) 3_666 3_666 ?
O3 V1 V3 81.42(19) . 3_666 ?
O1 V1 V3 124.77(14) . 3_666 ?
O4 V1 V3 47.39(4) . 3_666 ?
V2 V1 V3 66.10(5) 3_666 3_666 ?
C31 N2 C34 118.9(8) . . ?
C31 N2 C37 112.8(11) . . ?
C34 N2 C37 108.7(11) . . ?
N2 C31 C33 117.8(9) . . ?
N2 C31 C32 113.2(11) . . ?
C33 C31 C32 112.6(9) . . ?
N2 C34 C36 111.8(9) . . ?
N2 C34 C35 106.4(10) . . ?
C36 C34 C35 116.8(13) . . ?
C38 C37 N2 115.1(9) . . ?
N3 C41 C42 176.1(11) . . ?
C21 C22 C23 117.0(11) . . ?
C23 C24 C25 116.6(14) . . ?
C22 C21 C20 116.1(10) . . ?
C24 C23 C22 117.4(13) . . ?
C25 C26 C27 115.5(18) . . ?
C26 C25 C24 116.3(17) . . ?

_refine_diff_density_max         0.963
_refine_diff_density_min         -0.672
_refine_diff_density_rms         0.102


_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: acetonitrile'
####################################################################### 
# 
# 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_wo
_database_code_depnum_ccdc_archive 'CCDC 1978670'
loop_
_audit_author_name
_audit_author_address
'Zicheng Xiao'
;Hubei University of Technology
China
;
_audit_update_record             
;
2020-01-18 deposited with the CCDC.	2020-03-13 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C124 H220 N8 O46 V12'
_chemical_formula_weight         3170.35

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

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_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'

_cell_length_a                   13.709(2)
_cell_length_b                   13.919(2)
_cell_length_c                   19.530(3)
_cell_angle_alpha                97.532(2)
_cell_angle_beta                 93.120(3)
_cell_angle_gamma                99.117(2)
_cell_volume                     3637.0(9)
_cell_formula_units_Z            1
_cell_measurement_temperature    273(2)
_cell_measurement_reflns_used    4305
_cell_measurement_theta_min      2.253
_cell_measurement_theta_max      26.233

_exptl_crystal_description       needle
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.447
_exptl_crystal_F_000             1664
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.11
_exptl_absorpt_coefficient_mu    0.814
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6266
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_process_details   
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.1088 before and 0.0543 after correction.
The Ratio of minimum to maximum transmission is 0.8404.
The λ/2 correction factor is 0.0015.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      273(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            32605
_diffrn_reflns_av_unetI/netI     0.0958
_diffrn_reflns_av_R_equivalents  0.0528
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         1.497
_diffrn_reflns_theta_max         28.094
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measured_fraction_theta_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_point_group_measured_fraction_full 0.991
_reflns_number_total             17407
_reflns_number_gt                11443
_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       'SAINT v7.68A (Bruker, 2009)'
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2009)'
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_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)+(0.0894P)²+3.8551P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         17407
_refine_ls_number_parameters     880
_refine_ls_number_restraints     157
_refine_ls_R_factor_all          0.1008
_refine_ls_R_factor_gt           0.0627
_refine_ls_wR_factor_ref         0.1881
_refine_ls_wR_factor_gt          0.1589
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_restrained_S_all      1.034
_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
C0 C 0.2009(3) 1.1843(3) 0.14059(19) 0.0149(8) Uani 1 1 d . . . . .
O1 O -0.09642(19) 1.14706(19) -0.02002(14) 0.0156(6) Uani 1 1 d . . . . .
N1 N 0.2763(2) 1.2526(2) 0.18702(16) 0.0163(7) Uani 1 1 d . . . . .
H1 H 0.3237 1.2855 0.1684 0.020 Uiso 1 1 calc R U . . .
C1 C 0.2768(3) 1.2678(3) 0.2570(2) 0.0193(8) Uani 1 1 d . . . . .
V1 V 0.15884(5) 0.98210(5) 0.01220(3) 0.01391(15) Uani 1 1 d . . . . .
V2 V -0.01967(5) 1.01628(5) 0.11347(3) 0.01460(15) Uani 1 1 d . . . . .
O2 O 0.0000 1.0000 0.0000 0.0132(7) Uani 1 2 d S . P . .
N2 N -2.1843(2) -0.2918(2) -0.82298(16) 0.0167(7) Uani 1 1 d . . . . .
H2 H -2.1583 -0.2368 -0.8350 0.020 Uiso 1 1 calc R U . . .
C2 C 0.2382(3) 1.1864(3) 0.06823(18) 0.0139(7) Uani 1 1 d . . . . .
H2A H 0.2473 1.2534 0.0580 0.017 Uiso 1 1 calc R U . . .
H2B H 0.3020 1.1648 0.0677 0.017 Uiso 1 1 calc R U . . .
O3 O 0.12287(19) 1.01211(19) 0.11251(13) 0.0148(5) Uani 1 1 d . . . . .
C3 C 0.1009(3) 1.2219(3) 0.1427(2) 0.0174(8) Uani 1 1 d . . . . .
H3A H 0.0792 1.2240 0.1892 0.021 Uiso 1 1 calc R U . . .
H3B H 0.1095 1.2882 0.1310 0.021 Uiso 1 1 calc R U . . .
V3 V -2.44613(5) -0.56104(5) -0.90810(3) 0.01399(15) Uani 1 1 d . . . . .
V4 V -2.50492(5) -0.35018(5) -0.94151(3) 0.01414(15) Uani 1 1 d . . . . .
O4 O -0.05362(19) 0.8886(2) 0.09810(13) 0.0166(6) Uani 1 1 d . . . . .
C4 C 0.1919(3) 1.0807(3) 0.1602(2) 0.0168(8) Uani 1 1 d . . . . .
H4A H 0.2564 1.0603 0.1602 0.020 Uiso 1 1 calc R U . . .
H4B H 0.1700 1.0810 0.2066 0.020 Uiso 1 1 calc R U . . .
V5 V -2.35037(5) -0.45763(5) -1.03589(3) 0.01347(15) Uani 1 1 d . . . . .
O5 O -0.14720(18) 1.03853(19) 0.07917(14) 0.0155(6) Uani 1 1 d . . . . .
C5 C 0.3598(3) 1.3408(3) 0.29505(19) 0.0178(8) Uani 1 1 d . . . . .
V6 V 0.03241(5) 1.16201(5) -0.00474(3) 0.01348(15) Uani 1 1 d . . . . .
O6 O 0.02669(18) 1.15948(19) 0.09484(13) 0.0146(5) Uani 1 1 d . . . . .
C6 C 0.4466(3) 1.3775(3) 0.26728(19) 0.0169(8) Uani 1 1 d . . . . .
H6 H 0.4562 1.3547 0.2216 0.020 Uiso 1 1 calc R U . . .
O7 O 0.17148(18) 1.12519(19) 0.01581(13) 0.0141(5) Uani 1 1 d . . . . .
C7 C 0.5199(3) 1.4475(3) 0.3057(2) 0.0222(9) Uani 1 1 d . . . . .
H7 H 0.5778 1.4709 0.2863 0.027 Uiso 1 1 calc R U . . .
O8 O -0.0223(2) 1.0450(2) 0.19536(14) 0.0225(6) Uani 1 1 d . . . . .
C8 C 0.3479(4) 1.3750(4) 0.3642(2) 0.0352(12) Uani 1 1 d . . . . .
H8 H 0.2912 1.3500 0.3844 0.042 Uiso 1 1 calc R U . . .
O9 O 0.27297(19) 0.9788(2) 0.03201(14) 0.0197(6) Uani 1 1 d . . . . .
C9 C 0.4185(4) 1.4448(5) 0.4026(2) 0.0489(16) Uani 1 1 d . . . . .
H9 H 0.4090 1.4676 0.4482 0.059 Uiso 1 1 calc R U . . .
O10 O 0.0687(2) 1.2770(2) -0.00354(14) 0.0187(6) Uani 1 1 d . . . . .
C10 C 0.5045(4) 1.4815(4) 0.3735(2) 0.0360(13) Uani 1 1 d . . . . .
O11 O 0.2117(2) 1.2249(2) 0.28837(15) 0.0288(7) Uani 1 1 d . . . . .
C11 C 0.6618(4) 1.5919(4) 0.3919(2) 0.0475(16) Uani 1 1 d . U . . .
H11A H 0.6515 1.6196 0.3496 0.057 Uiso 1 1 calc R U . . .
H11B H 0.7029 1.5416 0.3834 0.057 Uiso 1 1 calc R U . . .
O12 O 0.5693(3) 1.5524(3) 0.41608(17) 0.0612(14) Uani 1 1 d . U . . .
C12 C 0.7092(5) 1.6716(5) 0.4508(3) 0.068(2) Uani 1 1 d . U . . .
H12A H 0.7039 1.6452 0.4942 0.081 Uiso 1 1 calc R U . . .
H12B H 0.6723 1.7258 0.4528 0.081 Uiso 1 1 calc R U . . .
C13 C 0.8186(4) 1.7114(5) 0.4434(2) 0.0497(16) Uani 1 1 d . U . . .
H13A H 0.8566 1.6581 0.4422 0.060 Uiso 1 1 calc R U . . .
H13B H 0.8249 1.7384 0.4003 0.060 Uiso 1 1 calc R U . . .
C14 C 0.8596(4) 1.7910(5) 0.5041(3) 0.0518(17) Uani 1 1 d . . . . .
H14A H 0.8455 1.7659 0.5471 0.062 Uiso 1 1 calc R U . . .
H14B H 0.8259 1.8470 0.5019 0.062 Uiso 1 1 calc R U . . .
C15 C 0.9712(4) 1.8252(4) 0.5042(3) 0.0487(16) Uani 1 1 d . . . . .
H15A H 1.0048 1.7694 0.5074 0.058 Uiso 1 1 calc R U . . .
H15B H 0.9853 1.8485 0.4605 0.058 Uiso 1 1 calc R U . . .
C16 C 1.0131(4) 1.9067(5) 0.5633(3) 0.0491(16) Uani 1 1 d . . . . .
H16A H 0.9822 1.9638 0.5586 0.059 Uiso 1 1 calc R U . . .
H16B H 0.9961 1.8847 0.6069 0.059 Uiso 1 1 calc R U . . .
C17 C 1.1249(4) 1.9365(5) 0.5651(3) 0.0495(16) Uani 1 1 d . . . . .
H17A H 1.1422 1.9539 0.5203 0.059 Uiso 1 1 calc R U . . .
H17B H 1.1559 1.8805 0.5731 0.059 Uiso 1 1 calc R U . . .
C18 C 1.1665(4) 2.0234(4) 0.6213(3) 0.0441(14) Uani 1 1 d . . . . .
H18A H 1.1393 2.0807 0.6115 0.053 Uiso 1 1 calc R U . . .
H18B H 1.1451 2.0079 0.6658 0.053 Uiso 1 1 calc R U . . .
C19 C 1.2777(4) 2.0476(5) 0.6262(3) 0.0504(16) Uani 1 1 d . U . . .
H19A H 1.2984 2.0659 0.5823 0.061 Uiso 1 1 calc R U . . .
H19B H 1.3044 1.9888 0.6333 0.061 Uiso 1 1 calc R U . . .
O20 O -2.42530(19) -0.40740(19) -1.10226(13) 0.0148(5) Uani 1 1 d . . . . .
C20 C 1.3225(4) 2.1303(5) 0.6840(3) 0.0514(16) Uani 1 1 d . U . . .
H20A H 1.3010 2.1127 0.7279 0.062 Uiso 1 1 calc R U . . .
H20B H 1.2972 2.1895 0.6764 0.062 Uiso 1 1 calc R U . . .
O21 O -2.4959(2) -0.24774(19) -0.89215(14) 0.0183(6) Uani 1 1 d . . . . .
C21 C 1.4358(4) 2.1522(5) 0.6889(4) 0.0605(19) Uani 1 1 d D U . . .
H21A H 1.4554 2.1636 0.6433 0.073 Uiso 0.472(12) 1 calc R U P A 1
H21B H 1.4559 2.2138 0.7195 0.073 Uiso 0.472(12) 1 calc R U P A 1
H21C H 1.4581 2.2010 0.7292 0.073 Uiso 0.528(12) 1 calc R U P A 2
H21D H 1.4607 2.0927 0.6965 0.073 Uiso 0.528(12) 1 calc R U P A 2
O22 O -2.3921(2) -0.5930(2) -0.84234(13) 0.0174(6) Uani 1 1 d . . . . .
O23 O -2.23962(19) -0.4168(2) -1.05230(13) 0.0171(6) Uani 1 1 d . . . . .
O24 O -2.62780(19) -0.41992(19) -0.91963(13) 0.0156(6) Uani 1 1 d . . . . .
O25 O -2.55436(19) -0.33075(19) -1.02295(13) 0.0156(6) Uani 1 1 d . . . . .
N4 N -0.7848(3) 0.6469(3) 0.15331(17) 0.0212(7) Uani 1 1 d . . . . .
H4 H -0.7246 0.6401 0.1295 0.025 Uiso 1 1 calc R U . . .
O26 O -2.31777(18) -0.50284(19) -0.94733(13) 0.0137(5) Uani 1 1 d . . . . .
O27 O -2.36955(18) -0.33350(19) -0.97124(13) 0.0135(5) Uani 1 1 d . . . . .
O28 O -2.5000 -0.5000 -1.0000 0.0126(7) Uani 1 2 d S . P . .
O29 O -2.44410(19) -0.42228(19) -0.86920(13) 0.0135(5) Uani 1 1 d . . . . .
O30 O -2.1778(2) -0.3934(2) -0.74137(15) 0.0278(7) Uani 1 1 d . . . . .
N3 N -0.6978(3) 0.8634(3) -0.1317(2) 0.0279(9) Uani 1 1 d . . . . .
H3 H -0.7495 0.9027 -0.1202 0.034 Uiso 1 1 calc R U . . .
C30 C -2.1436(3) -0.3187(3) -0.7643(2) 0.0209(9) Uani 1 1 d . . . . .
C31 C -2.2687(3) -0.3497(3) -0.86663(19) 0.0143(7) Uani 1 1 d . . . . .
O31 O -1.7952(3) -0.0847(4) -0.62761(19) 0.0651(14) Uani 1 1 d . . . . .
C32 C -2.3601(3) -0.3700(3) -0.82491(19) 0.0155(8) Uani 1 1 d . . . . .
H32A H -2.3455 -0.4084 -0.7888 0.019 Uiso 1 1 calc R U . . .
H32B H -2.3756 -0.3082 -0.8029 0.019 Uiso 1 1 calc R U . . .
C33 C -2.2898(3) -0.2856(3) -0.92194(18) 0.0136(7) Uani 1 1 d . . . . .
H33A H -2.3063 -0.2244 -0.8996 0.016 Uiso 1 1 calc R U . . .
H33B H -2.2305 -0.2699 -0.9460 0.016 Uiso 1 1 calc R U . . .
C34 C -2.2391(3) -0.4455(3) -0.90066(19) 0.0156(8) Uani 1 1 d . . . . .
H34A H -2.1809 -0.4300 -0.9259 0.019 Uiso 1 1 calc R U . . .
H34B H -2.2221 -0.4837 -0.8650 0.019 Uiso 1 1 calc R U . . .
C35 C -2.0532(3) -0.2523(3) -0.7304(2) 0.0232(9) Uani 1 1 d . . . . .
C36 C -1.9927(3) -0.2888(4) -0.6836(2) 0.0301(10) Uani 1 1 d . . . . .
H36 H -2.0100 -0.3530 -0.6747 0.036 Uiso 1 1 calc R U . . .
C37 C -1.9081(4) -0.2313(5) -0.6507(2) 0.0406(13) Uani 1 1 d . . . . .
H37 H -1.8692 -0.2570 -0.6196 0.049 Uiso 1 1 calc R U . . .
C38 C -2.0248(3) -0.1558(4) -0.7419(2) 0.0301(10) Uani 1 1 d . . . . .
H38 H -2.0638 -0.1300 -0.7729 0.036 Uiso 1 1 calc R U . . .
C39 C -1.9398(4) -0.0966(4) -0.7083(2) 0.0423(14) Uani 1 1 d . . . . .
H39 H -1.9230 -0.0316 -0.7159 0.051 Uiso 1 1 calc R U . . .
C40 C -1.8802(4) -0.1362(5) -0.6631(2) 0.0408(14) Uani 1 1 d . . . . .
C41 C -1.7608(6) 0.0126(7) -0.6391(3) 0.106(4) Uani 1 1 d D U . . .
H41A H -1.8105 0.0535 -0.6283 0.128 Uiso 1 1 calc R U . . .
H41B H -1.7472 0.0137 -0.6872 0.128 Uiso 1 1 calc R U . . .
C58 C -0.8320(4) 0.7165(3) -0.1264(2) 0.0330(11) Uani 1 1 d . . . . .
H58A H -0.8363 0.6952 -0.1755 0.049 Uiso 1 1 calc R U . . .
H58B H -0.8779 0.7608 -0.1163 0.049 Uiso 1 1 calc R U . . .
H58C H -0.8479 0.6605 -0.1027 0.049 Uiso 1 1 calc R U . . .
C61 C -0.7692(3) 0.6134(3) 0.2244(2) 0.0246(9) Uani 1 1 d . . . . .
H61 H -0.8214 0.6322 0.2531 0.029 Uiso 1 1 calc R U . . .
C66 C -0.8701(4) 0.6095(4) 0.0352(2) 0.0382(13) Uani 1 1 d . . . . .
H66A H -0.8866 0.6740 0.0352 0.057 Uiso 1 1 calc R U . . .
H66B H -0.9177 0.5626 0.0051 0.057 Uiso 1 1 calc R U . . .
H66C H -0.8052 0.6085 0.0193 0.057 Uiso 1 1 calc R U . . .
C64 C -0.8714(3) 0.5838(4) 0.1067(2) 0.0316(11) Uani 1 1 d . . . . .
H64 H -0.8600 0.5157 0.1035 0.038 Uiso 1 1 calc R U . . .
C57 C -0.7278(4) 0.7684(3) -0.1026(2) 0.0302(10) Uani 1 1 d . . . . .
H57A H -0.6818 0.7243 -0.1159 0.036 Uiso 1 1 calc R U . . .
H57B H -0.7222 0.7824 -0.0524 0.036 Uiso 1 1 calc R U . . .
C67 C -0.7934(4) 0.7547(4) 0.1612(3) 0.0366(12) Uani 1 1 d . . . . .
H67A H -0.8536 0.7627 0.1356 0.044 Uiso 1 1 calc R U . . .
H67B H -0.7980 0.7785 0.2096 0.044 Uiso 1 1 calc R U . . .
C56 C -0.5098(4) 0.8808(4) -0.1120(3) 0.0480(15) Uani 1 1 d . . . . .
H56A H -0.5144 0.8144 -0.1025 0.072 Uiso 1 1 calc R U . . .
H56B H -0.4528 0.9207 -0.0860 0.072 Uiso 1 1 calc R U . . .
H56C H -0.5034 0.8823 -0.1606 0.072 Uiso 1 1 calc R U . . .
C65 C -0.9710(4) 0.5864(5) 0.1371(3) 0.0469(15) Uani 1 1 d . . . . .
H65A H -0.9693 0.5634 0.1814 0.070 Uiso 1 1 calc R U . . .
H65B H -1.0222 0.5447 0.1065 0.070 Uiso 1 1 calc R U . . .
H65C H -0.9842 0.6525 0.1428 0.070 Uiso 1 1 calc R U . . .
C53 C -0.7894(5) 0.8759(5) -0.2411(3) 0.0526(17) Uani 1 1 d . . . . .
H53A H -0.8428 0.8255 -0.2339 0.079 Uiso 1 1 calc R U . . .
H53B H -0.7849 0.8768 -0.2899 0.079 Uiso 1 1 calc R U . . .
H53C H -0.8017 0.9385 -0.2197 0.079 Uiso 1 1 calc R U . . .
C51 C -0.6948(4) 0.8556(4) -0.2099(3) 0.0427(14) Uani 1 1 d . . . . .
H51 H -0.6429 0.9085 -0.2187 0.051 Uiso 1 1 calc R U . . .
C54 C -0.6030(4) 0.9207(4) -0.0913(3) 0.0404(13) Uani 1 1 d . . . . .
H54 H -0.6094 0.9144 -0.0423 0.048 Uiso 1 1 calc R U . . .
C68 C -0.7064(4) 0.8146(4) 0.1352(3) 0.0494(15) Uani 1 1 d . . . . .
H68A H -0.7016 0.7913 0.0872 0.074 Uiso 1 1 calc R U . . .
H68B H -0.6469 0.8088 0.1615 0.074 Uiso 1 1 calc R U . . .
H68C H -0.7147 0.8823 0.1402 0.074 Uiso 1 1 calc R U . . .
C63 C -0.7747(5) 0.5030(4) 0.2186(3) 0.0449(14) Uani 1 1 d . . . . .
H63A H -0.8410 0.4710 0.2032 0.067 Uiso 1 1 calc R U . . .
H63B H -0.7569 0.4858 0.2631 0.067 Uiso 1 1 calc R U . . .
H63C H -0.7298 0.4822 0.1859 0.067 Uiso 1 1 calc R U . . .
C55 C -0.5950(4) 1.0284(4) -0.0979(4) 0.0539(17) Uani 1 1 d . . . . .
H55A H -0.5842 1.0378 -0.1449 0.081 Uiso 1 1 calc R U . . .
H55B H -0.5404 1.0652 -0.0677 0.081 Uiso 1 1 calc R U . . .
H55C H -0.6552 1.0507 -0.0853 0.081 Uiso 1 1 calc R U . . .
C52 C -0.6669(5) 0.7603(4) -0.2440(3) 0.0496(16) Uani 1 1 d . . . . .
H52A H -0.6053 0.7508 -0.2223 0.074 Uiso 1 1 calc R U . . .
H52B H -0.6599 0.7635 -0.2923 0.074 Uiso 1 1 calc R U . . .
H52C H -0.7178 0.7063 -0.2390 0.074 Uiso 1 1 calc R U . . .
C62 C -0.6711(4) 0.6667(5) 0.2581(3) 0.0543(17) Uani 1 1 d . . . . .
H62A H -0.6189 0.6477 0.2313 0.081 Uiso 1 1 calc R U . . .
H62B H -0.6623 0.6503 0.3040 0.081 Uiso 1 1 calc R U . . .
H62C H -0.6695 0.7363 0.2605 0.081 Uiso 1 1 calc R U . . .
C42 C -1.6695(5) 0.0496(9) -0.5938(4) 0.147(5) Uani 1 1 d D U . . .
H42 H -1.6653 0.0307 -0.5499 0.177 Uiso 1 1 calc R U . . .
C48 C -1.2169(7) 0.3786(8) -0.4743(5) 0.115(3) Uani 1 1 d D U . . .
H48A H -1.2381 0.3621 -0.4301 0.138 Uiso 1 1 calc R U . . .
H48B H -1.1692 0.3368 -0.4886 0.138 Uiso 1 1 calc R U . . .
C43 C -1.5955(6) 0.1067(11) -0.6120(7) 0.202(6) Uani 1 1 d D U . . .
H43 H -1.5995 0.1308 -0.6541 0.242 Uiso 1 1 calc R U . . .
C29 C -1.0831(9) 0.4977(8) -0.4121(6) 0.175(6) Uani 1 1 d D U . . .
H29A H -1.0981 0.4523 -0.3791 0.210 Uiso 1 1 calc R U . . .
H29B H -1.0278 0.4777 -0.4361 0.210 Uiso 1 1 calc R U . . .
C44 C -1.5048(7) 0.1333(11) -0.5659(9) 0.244(8) Uani 1 1 d D U . . .
H44A H -1.5226 0.1274 -0.5191 0.292 Uiso 1 1 calc R U . . .
H44B H -1.4625 0.0850 -0.5781 0.292 Uiso 1 1 calc R U . . .
C46 C -1.3565(6) 0.2581(9) -0.5255(7) 0.154(5) Uani 1 1 d D U . . .
H46A H -1.3684 0.2500 -0.4779 0.185 Uiso 1 1 calc R U . . .
H46B H -1.3132 0.2122 -0.5409 0.185 Uiso 1 1 calc R U . . .
C27 C -0.9589(8) 0.6132(8) -0.3276(6) 0.150(5) Uani 1 1 d D U . . .
H27A H -0.9071 0.5809 -0.3459 0.225 Uiso 1 1 calc R U . . .
H27B H -0.9727 0.5943 -0.2831 0.225 Uiso 1 1 calc R U . . .
H27C H -0.9384 0.6831 -0.3228 0.225 Uiso 1 1 calc R U . . .
C45 C -1.4485(7) 0.2268(9) -0.5652(6) 0.134(4) Uani 1 1 d D U . . .
H45A H -1.4909 0.2741 -0.5508 0.161 Uiso 1 1 calc R U . . .
H45B H -1.4359 0.2334 -0.6129 0.161 Uiso 1 1 calc R U . . .
C28 C -1.0473(8) 0.5851(9) -0.3743(8) 0.195(7) Uani 1 1 d D U . . .
H28A H -1.1009 0.6009 -0.3467 0.233 Uiso 1 1 calc R U . . .
H28B H -1.0406 0.6315 -0.4074 0.233 Uiso 1 1 calc R U . . .
C47 C -1.3019(8) 0.3540(8) -0.5241(6) 0.133(4) Uani 1 1 d D U . . .
H47A H -1.3459 0.4014 -0.5139 0.159 Uiso 1 1 calc R U . . .
H47B H -1.2796 0.3604 -0.5698 0.159 Uiso 1 1 calc R U . . .
C49 C -1.1672(9) 0.4771(9) -0.4635(7) 0.196(7) Uani 1 1 d D U . . .
H49A H -1.2143 0.5196 -0.4493 0.235 Uiso 1 1 calc R U . . .
H49B H -1.1444 0.4939 -0.5072 0.235 Uiso 1 1 calc R U . . .
C0AA C 1.4950(8) 2.0809(9) 0.7127(6) 0.050(3) Uani 0.472(12) 1 d D U P A 1
H0AA H 1.5643 2.1065 0.7126 0.075 Uiso 0.472(12) 1 calc R U P A 1
H0AB H 1.4798 2.0702 0.7588 0.075 Uiso 0.472(12) 1 calc R U P A 1
H0AC H 1.4794 2.0198 0.6821 0.075 Uiso 0.472(12) 1 calc R U P A 1
C1AA C 1.4792(9) 2.1874(11) 0.6289(7) 0.084(5) Uani 0.528(12) 1 d D U P A 2
H1AA H 1.5501 2.1991 0.6366 0.126 Uiso 0.528(12) 1 calc R U P A 2
H1AB H 1.4594 2.1389 0.5888 0.126 Uiso 0.528(12) 1 calc R U P A 2
H1AC H 1.4569 2.2475 0.6216 0.126 Uiso 0.528(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
C0 N1 1.468(5) . ?
C0 C4 1.528(5) . ?
C0 C2 1.531(5) . ?
C0 C3 1.543(5) . ?
O1 V6 1.750(3) . ?
O1 V1 1.894(3) 2_575 ?
N1 C1 1.354(5) . ?
C1 O11 1.231(5) . ?
C1 C5 1.491(5) . ?
V1 O9 1.600(3) . ?
V1 O5 1.764(3) 2_575 ?
V1 O1 1.894(3) 2_575 ?
V1 O7 1.963(3) . ?
V1 O3 2.052(3) . ?
V1 O2 2.2342(7) . ?
V1 V6 3.0222(10) 2_575 ?
V1 V2 3.0304(10) 2_575 ?
V2 O8 1.601(3) . ?
V2 O4 1.746(3) . ?
V2 O5 1.923(3) . ?
V2 O3 1.965(3) . ?
V2 O6 2.079(3) . ?
V2 O2 2.2333(7) . ?
V2 V6 3.0230(9) 2_575 ?
V2 V1 3.0304(10) 2_575 ?
O2 V2 2.2333(7) 2_575 ?
O2 V1 2.2342(7) 2_575 ?
O2 V6 2.2434(7) 2_575 ?
O2 V6 2.2434(7) . ?
N2 C30 1.369(5) . ?
N2 C31 1.460(5) . ?
C2 O7 1.425(4) . ?
O3 C4 1.436(4) . ?
C3 O6 1.438(4) . ?
V3 O22 1.596(3) . ?
V3 O20 1.777(3) 2_043 ?
V3 O25 1.885(3) 2_043 ?
V3 O29 1.976(3) . ?
V3 O26 2.049(3) . ?
V3 O28 2.2233(7) . ?
V3 V5 3.0032(10) 2_043 ?
V3 V4 3.0292(10) 2_043 ?
V4 O21 1.596(3) . ?
V4 O25 1.765(3) . ?
V4 O24 1.906(3) . ?
V4 O27 1.962(3) . ?
V4 O29 2.051(3) . ?
V4 O28 2.2554(7) . ?
V4 V3 3.0291(10) 2_043 ?
V4 V5 3.0332(10) 2_043 ?
O4 V6 1.921(3) 2_575 ?
V5 O23 1.599(3) . ?
V5 O24 1.781(3) 2_043 ?
V5 O20 1.883(3) . ?
V5 O26 1.969(3) . ?
V5 O27 2.063(3) . ?
V5 O28 2.2199(7) . ?
V5 V3 3.0031(10) 2_043 ?
V5 V4 3.0332(10) 2_043 ?
O5 V1 1.764(3) 2_575 ?
C5 C6 1.386(5) . ?
C5 C8 1.399(6) . ?
V6 O10 1.595(3) . ?
V6 O4 1.921(3) 2_575 ?
V6 O6 1.955(3) . ?
V6 O7 2.083(3) . ?
V6 V1 3.0222(10) 2_575 ?
V6 V2 3.0231(9) 2_575 ?
C6 C7 1.392(5) . ?
C7 C10 1.386(6) . ?
C8 C9 1.369(6) . ?
C9 C10 1.389(6) . ?
C10 O12 1.372(5) . ?
C11 O12 1.429(6) . ?
C11 C12 1.527(7) . ?
C12 C13 1.535(7) . ?
C13 C14 1.528(7) . ?
C14 C15 1.529(7) . ?
C15 C16 1.525(7) . ?
C16 C17 1.520(7) . ?
C17 C18 1.536(7) . ?
C18 C19 1.503(7) . ?
C19 C20 1.529(7) . ?
O20 V3 1.777(3) 2_043 ?
C20 C21 1.529(7) . ?
C21 C1AA 1.450(13) . ?
C21 C0AA 1.481(12) . ?
O24 V5 1.781(3) 2_043 ?
O25 V3 1.885(3) 2_043 ?
N4 C67 1.513(6) . ?
N4 C64 1.534(6) . ?
N4 C61 1.535(5) . ?
O26 C34 1.436(4) . ?
O27 C33 1.433(4) . ?
O28 V5 2.2199(7) 2_043 ?
O28 V3 2.2233(7) 2_043 ?
O28 V4 2.2554(7) 2_043 ?
O29 C32 1.437(4) . ?
O30 C30 1.222(5) . ?
N3 C57 1.514(6) . ?
N3 C51 1.520(6) . ?
N3 C54 1.530(6) . ?
C30 C35 1.489(6) . ?
C31 C33 1.532(5) . ?
C31 C34 1.533(5) . ?
C31 C32 1.540(5) . ?
O31 C40 1.367(6) . ?
O31 C41 1.413(10) . ?
C35 C38 1.388(7) . ?
C35 C36 1.397(6) . ?
C36 C37 1.374(7) . ?
C37 C40 1.375(8) . ?
C38 C39 1.393(6) . ?
C39 C40 1.393(8) . ?
C41 C42 1.473(8) . ?
C58 C57 1.514(7) . ?
C61 C62 1.500(7) . ?
C61 C63 1.516(7) . ?
C66 C64 1.486(7) . ?
C64 C65 1.522(6) . ?
C67 C68 1.496(8) . ?
C56 C54 1.526(6) . ?
C53 C51 1.486(7) . ?
C51 C52 1.519(7) . ?
C54 C55 1.508(7) . ?
C42 C43 1.282(10) . ?
C48 C49 1.414(11) . ?
C48 C47 1.444(9) . ?
C43 C44 1.462(10) . ?
C29 C28 1.343(9) . ?
C29 C49 1.453(9) . ?
C44 C45 1.403(11) . ?
C46 C47 1.419(10) . ?
C46 C45 1.420(10) . ?
C27 C28 1.444(9) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 C0 C4 110.5(3) . . ?
N1 C0 C2 105.0(3) . . ?
C4 C0 C2 110.4(3) . . ?
N1 C0 C3 109.7(3) . . ?
C4 C0 C3 111.5(3) . . ?
C2 C0 C3 109.5(3) . . ?
V6 O1 V1 112.04(13) . 2_575 ?
C1 N1 C0 124.9(3) . . ?
O11 C1 N1 122.3(4) . . ?
O11 C1 C5 120.8(4) . . ?
N1 C1 C5 116.8(3) . . ?
O9 V1 O5 104.30(13) . 2_575 ?
O9 V1 O1 102.58(13) . 2_575 ?
O5 V1 O1 93.44(12) 2_575 2_575 ?
O9 V1 O7 97.25(13) . . ?
O5 V1 O7 92.99(12) 2_575 . ?
O1 V1 O7 156.91(11) 2_575 . ?
O9 V1 O3 95.35(13) . . ?
O5 V1 O3 160.29(11) 2_575 . ?
O1 V1 O3 83.58(11) 2_575 . ?
O7 V1 O3 82.92(11) . . ?
O9 V1 O2 171.49(10) . . ?
O5 V1 O2 83.53(8) 2_575 . ?
O1 V1 O2 79.95(8) 2_575 . ?
O7 V1 O2 78.78(8) . . ?
O3 V1 O2 76.77(7) . . ?
O9 V1 V6 134.99(11) . 2_575 ?
O5 V1 V6 86.20(9) 2_575 2_575 ?
O1 V1 V6 32.46(8) 2_575 2_575 ?
O7 V1 V6 126.26(8) . 2_575 ?
O3 V1 V6 80.86(7) . 2_575 ?
O2 V1 V6 47.678(19) . 2_575 ?
O9 V1 V2 140.12(11) . 2_575 ?
O5 V1 V2 36.49(8) 2_575 2_575 ?
O1 V1 V2 90.00(8) 2_575 2_575 ?
O7 V1 V2 82.13(8) . 2_575 ?
O3 V1 V2 123.85(8) . 2_575 ?
O2 V1 V2 47.277(17) . 2_575 ?
V6 V1 V2 66.12(2) 2_575 2_575 ?
O8 V2 O4 105.08(14) . . ?
O8 V2 O5 102.20(13) . . ?
O4 V2 O5 93.32(12) . . ?
O8 V2 O3 97.40(13) . . ?
O4 V2 O3 93.84(12) . . ?
O5 V2 O3 156.58(12) . . ?
O8 V2 O6 95.01(13) . . ?
O4 V2 O6 159.87(12) . . ?
O5 V2 O6 83.55(11) . . ?
O3 V2 O6 82.08(11) . . ?
O8 V2 O2 170.61(11) . . ?
O4 V2 O2 83.74(9) . . ?
O5 V2 O2 80.14(8) . . ?
O3 V2 O2 78.53(8) . . ?
O6 V2 O2 76.12(7) . . ?
O8 V2 V6 140.68(11) . 2_575 ?
O4 V2 V6 36.40(9) . 2_575 ?
O5 V2 V6 90.59(8) . 2_575 ?
O3 V2 V6 82.14(8) . 2_575 ?
O6 V2 V6 123.55(7) . 2_575 ?
O2 V2 V6 47.666(18) . 2_575 ?
O8 V2 V1 135.18(11) . 2_575 ?
O4 V2 V1 85.82(9) . 2_575 ?
O5 V2 V1 33.06(8) . 2_575 ?
O3 V2 V1 125.61(8) . 2_575 ?
O6 V2 V1 80.73(7) . 2_575 ?
O2 V2 V1 47.300(18) . 2_575 ?
V6 V2 V1 66.16(2) 2_575 2_575 ?
V2 O2 V2 180.0 . 2_575 ?
V2 O2 V1 94.58(2) . . ?
V2 O2 V1 85.42(2) 2_575 . ?
V2 O2 V1 85.43(2) . 2_575 ?
V2 O2 V1 94.57(2) 2_575 2_575 ?
V1 O2 V1 180.0 . 2_575 ?
V2 O2 V6 84.95(2) . 2_575 ?
V2 O2 V6 95.05(2) 2_575 2_575 ?
V1 O2 V6 84.90(2) . 2_575 ?
V1 O2 V6 95.10(2) 2_575 2_575 ?
V2 O2 V6 95.05(2) . . ?
V2 O2 V6 84.95(2) 2_575 . ?
V1 O2 V6 95.10(2) . . ?
V1 O2 V6 84.90(2) 2_575 . ?
V6 O2 V6 180.0 2_575 . ?
C30 N2 C31 124.8(3) . . ?
O7 C2 C0 112.4(3) . . ?
C4 O3 V2 119.8(2) . . ?
C4 O3 V1 118.3(2) . . ?
V2 O3 V1 109.58(12) . . ?
O6 C3 C0 111.1(3) . . ?
O22 V3 O20 104.75(13) . 2_043 ?
O22 V3 O25 102.43(13) . 2_043 ?
O20 V3 O25 93.59(12) 2_043 2_043 ?
O22 V3 O29 97.33(13) . . ?
O20 V3 O29 92.24(11) 2_043 . ?
O25 V3 O29 157.22(12) 2_043 . ?
O22 V3 O26 95.02(12) . . ?
O20 V3 O26 160.05(12) 2_043 . ?
O25 V3 O26 84.60(11) 2_043 . ?
O29 V3 O26 82.46(10) . . ?
O22 V3 O28 171.15(11) . . ?
O20 V3 O28 83.29(9) 2_043 . ?
O25 V3 O28 80.43(8) 2_043 . ?
O29 V3 O28 78.41(8) . . ?
O26 V3 O28 76.81(7) . . ?
O22 V3 V5 140.20(10) . 2_043 ?
O20 V3 V5 36.02(9) 2_043 2_043 ?
O25 V3 V5 89.77(8) 2_043 2_043 ?
O29 V3 V5 82.12(8) . 2_043 ?
O26 V3 V5 124.03(8) . 2_043 ?
O28 V3 V5 47.429(18) . 2_043 ?
O22 V3 V4 135.02(10) . 2_043 ?
O20 V3 V4 86.49(8) 2_043 2_043 ?
O25 V3 V4 32.68(8) 2_043 2_043 ?
O29 V3 V4 126.10(8) . 2_043 ?
O26 V3 V4 81.28(7) . 2_043 ?
O28 V3 V4 47.891(19) . 2_043 ?
V5 V3 V4 66.12(2) 2_043 2_043 ?
O21 V4 O25 105.95(13) . . ?
O21 V4 O24 102.40(13) . . ?
O25 V4 O24 93.07(12) . . ?
O21 V4 O27 98.01(13) . . ?
O25 V4 O27 91.95(12) . . ?
O24 V4 O27 156.73(11) . . ?
O21 V4 O29 95.71(12) . . ?
O25 V4 O29 158.21(11) . . ?
O24 V4 O29 84.43(11) . . ?
O27 V4 O29 82.53(11) . . ?
O21 V4 O28 171.34(10) . . ?
O25 V4 O28 82.06(8) . . ?
O24 V4 O28 80.06(8) . . ?
O27 V4 O28 78.15(8) . . ?
O29 V4 O28 76.18(7) . . ?
O21 V4 V3 140.67(11) . 2_043 ?
O25 V4 V3 35.21(8) . 2_043 ?
O24 V4 V3 89.17(8) . 2_043 ?
O27 V4 V3 81.96(8) . 2_043 ?
O29 V4 V3 123.00(7) . 2_043 ?
O28 V4 V3 46.997(17) . 2_043 ?
O21 V4 V5 135.58(10) . 2_043 ?
O25 V4 V5 85.82(9) . 2_043 ?
O24 V4 V5 33.32(8) . 2_043 ?
O27 V4 V5 124.77(8) . 2_043 ?
O29 V4 V5 80.23(8) . 2_043 ?
O28 V4 V5 46.840(18) . 2_043 ?
V3 V4 V5 65.39(2) 2_043 2_043 ?
V2 O4 V6 110.97(14) . 2_575 ?
O3 C4 C0 111.0(3) . . ?
O23 V5 O24 103.15(13) . 2_043 ?
O23 V5 O20 101.64(13) . . ?
O24 V5 O20 94.83(12) 2_043 . ?
O23 V5 O26 97.52(13) . . ?
O24 V5 O26 91.78(12) 2_043 . ?
O20 V5 O26 157.71(11) . . ?
O23 V5 O27 95.99(12) . . ?
O24 V5 O27 160.59(12) 2_043 . ?
O20 V5 O27 84.36(11) . . ?
O26 V5 O27 82.40(10) . . ?
O23 V5 O28 172.26(10) . . ?
O24 V5 O28 83.73(9) 2_043 . ?
O20 V5 O28 81.09(8) . . ?
O26 V5 O28 78.50(8) . . ?
O27 V5 O28 76.98(7) . . ?
O23 V5 V3 135.31(10) . 2_043 ?
O24 V5 V3 87.46(8) 2_043 2_043 ?
O20 V5 V3 33.71(8) . 2_043 ?
O26 V5 V3 125.80(8) . 2_043 ?
O27 V5 V3 81.12(7) . 2_043 ?
O28 V5 V3 47.525(19) . 2_043 ?
O23 V5 V4 138.73(10) . 2_043 ?
O24 V5 V4 36.00(8) 2_043 2_043 ?
O20 V5 V4 90.55(8) . 2_043 ?
O26 V5 V4 82.38(8) . 2_043 ?
O27 V5 V4 124.60(8) . 2_043 ?
O28 V5 V4 47.827(17) . 2_043 ?
V3 V5 V4 66.26(2) 2_043 2_043 ?
V1 O5 V2 110.45(13) 2_575 . ?
C6 C5 C8 117.9(4) . . ?
C6 C5 C1 125.3(3) . . ?
C8 C5 C1 116.8(4) . . ?
O10 V6 O1 104.13(13) . . ?
O10 V6 O4 101.49(13) . 2_575 ?
O1 V6 O4 94.41(12) . 2_575 ?
O10 V6 O6 98.99(13) . . ?
O1 V6 O6 93.51(12) . . ?
O4 V6 O6 155.50(12) 2_575 . ?
O10 V6 O7 96.92(12) . . ?
O1 V6 O7 158.91(12) . . ?
O4 V6 O7 82.57(11) 2_575 . ?
O6 V6 O7 81.73(10) . . ?
O10 V6 O2 172.85(10) . . ?
O1 V6 O2 82.73(9) . . ?
O4 V6 O2 79.71(8) 2_575 . ?
O6 V6 O2 78.34(8) . . ?
O7 V6 O2 76.19(7) . . ?
O10 V6 V1 139.22(10) . 2_575 ?
O1 V6 V1 35.51(9) . 2_575 ?
O4 V6 V1 90.34(8) 2_575 2_575 ?
O6 V6 V1 82.80(8) . 2_575 ?
O7 V6 V1 123.43(8) . 2_575 ?
O2 V6 V1 47.421(18) . 2_575 ?
O10 V6 V2 134.11(10) . 2_575 ?
O1 V6 V2 85.70(8) . 2_575 ?
O4 V6 V2 32.63(8) 2_575 2_575 ?
O6 V6 V2 125.45(8) . 2_575 ?
O7 V6 V2 80.55(7) . 2_575 ?
O2 V6 V2 47.383(19) . 2_575 ?
V1 V6 V2 65.78(2) 2_575 2_575 ?
C3 O6 V6 119.9(2) . . ?
C3 O6 V2 118.3(2) . . ?
V6 O6 V2 109.81(12) . . ?
C5 C6 C7 122.0(4) . . ?
C2 O7 V1 118.3(2) . . ?
C2 O7 V6 118.8(2) . . ?
V1 O7 V6 109.44(12) . . ?
C10 C7 C6 118.5(4) . . ?
C9 C8 C5 120.9(4) . . ?
C8 C9 C10 120.2(4) . . ?
O12 C10 C7 124.2(4) . . ?
O12 C10 C9 115.4(4) . . ?
C7 C10 C9 120.4(4) . . ?
O12 C11 C12 104.2(4) . . ?
C10 O12 C11 119.6(4) . . ?
C11 C12 C13 114.0(5) . . ?
C14 C13 C12 110.4(5) . . ?
C13 C14 C15 112.8(5) . . ?
C16 C15 C14 113.6(5) . . ?
C17 C16 C15 113.2(5) . . ?
C16 C17 C18 113.4(5) . . ?
C19 C18 C17 113.0(5) . . ?
C18 C19 C20 114.7(5) . . ?
V3 O20 V5 110.27(14) 2_043 . ?
C19 C20 C21 113.8(5) . . ?
C1AA C21 C20 115.3(8) . . ?
C0AA C21 C20 120.8(7) . . ?
V5 O24 V4 110.68(13) 2_043 . ?
V4 O25 V3 112.11(14) . 2_043 ?
C67 N4 C64 111.5(3) . . ?
C67 N4 C61 110.9(3) . . ?
C64 N4 C61 114.1(3) . . ?
C34 O26 V5 119.2(2) . . ?
C34 O26 V3 119.0(2) . . ?
V5 O26 V3 109.16(12) . . ?
C33 O27 V4 118.6(2) . . ?
C33 O27 V5 118.7(2) . . ?
V4 O27 V5 109.64(12) . . ?
V5 O28 V5 180.0 . 2_043 ?
V5 O28 V3 94.95(3) . . ?
V5 O28 V3 85.05(3) 2_043 . ?
V5 O28 V3 85.05(2) . 2_043 ?
V5 O28 V3 94.95(2) 2_043 2_043 ?
V3 O28 V3 180.00(3) . 2_043 ?
V5 O28 V4 94.67(2) . . ?
V5 O28 V4 85.33(2) 2_043 . ?
V3 O28 V4 94.89(2) . . ?
V3 O28 V4 85.11(2) 2_043 . ?
V5 O28 V4 85.33(2) . 2_043 ?
V5 O28 V4 94.67(2) 2_043 2_043 ?
V3 O28 V4 85.11(2) . 2_043 ?
V3 O28 V4 94.89(2) 2_043 2_043 ?
V4 O28 V4 180.0 . 2_043 ?
C32 O29 V3 119.5(2) . . ?
C32 O29 V4 118.1(2) . . ?
V3 O29 V4 110.03(12) . . ?
C57 N3 C51 116.6(4) . . ?
C57 N3 C54 109.2(4) . . ?
C51 N3 C54 114.0(4) . . ?
O30 C30 N2 122.5(4) . . ?
O30 C30 C35 121.6(4) . . ?
N2 C30 C35 116.0(4) . . ?
N2 C31 C33 104.7(3) . . ?
N2 C31 C34 109.2(3) . . ?
C33 C31 C34 110.0(3) . . ?
N2 C31 C32 111.3(3) . . ?
C33 C31 C32 109.8(3) . . ?
C34 C31 C32 111.5(3) . . ?
C40 O31 C41 119.7(5) . . ?
O29 C32 C31 110.8(3) . . ?
O27 C33 C31 112.0(3) . . ?
O26 C34 C31 111.5(3) . . ?
C38 C35 C36 117.5(4) . . ?
C38 C35 C30 124.3(4) . . ?
C36 C35 C30 118.2(4) . . ?
C37 C36 C35 121.1(5) . . ?
C36 C37 C40 120.9(5) . . ?
C35 C38 C39 121.9(5) . . ?
C40 C39 C38 118.9(5) . . ?
O31 C40 C37 116.6(5) . . ?
O31 C40 C39 123.7(6) . . ?
C37 C40 C39 119.6(5) . . ?
O31 C41 C42 107.7(8) . . ?
C62 C61 C63 111.3(5) . . ?
C62 C61 N4 108.3(4) . . ?
C63 C61 N4 111.9(3) . . ?
C66 C64 C65 113.2(4) . . ?
C66 C64 N4 110.5(4) . . ?
C65 C64 N4 112.9(4) . . ?
C58 C57 N3 114.2(4) . . ?
C68 C67 N4 111.7(4) . . ?
C53 C51 C52 112.7(5) . . ?
C53 C51 N3 109.8(4) . . ?
C52 C51 N3 114.3(4) . . ?
C55 C54 C56 111.7(4) . . ?
C55 C54 N3 109.7(4) . . ?
C56 C54 N3 113.3(4) . . ?
C43 C42 C41 123.1(9) . . ?
C49 C48 C47 117.5(9) . . ?
C42 C43 C44 119.3(11) . . ?
C28 C29 C49 126.1(9) . . ?
C45 C44 C43 117.9(12) . . ?
C47 C46 C45 121.6(10) . . ?
C44 C45 C46 122.5(11) . . ?
C29 C28 C27 129.1(10) . . ?
C46 C47 C48 114.7(11) . . ?
C48 C49 C29 115.0(11) . . ?

_refine_diff_density_max         1.426
_refine_diff_density_min         -1.092
_refine_diff_density_rms         0.120

