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

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
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data_exp_shiererchun
_database_code_depnum_ccdc_archive 'CCDC 1503807'
_audit_update_record             
;
2016-09-10 deposited with the CCDC.
2017-02-17 downloaded from the CCDC.
;
_audit_creation_date             2016-08-20
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C34 H62 O25 V6, 2(C16 H36 N)'
_chemical_formula_sum            'C66 H134 N2 O25 V6'
_chemical_formula_weight         1661.38
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   18.2750(6)
_cell_length_b                   17.3035(7)
_cell_length_c                   27.3203(11)
_cell_angle_alpha                90
_cell_angle_beta                 99.021(3)
_cell_angle_gamma                90
_cell_volume                     8532.4(6)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    4756
_cell_measurement_temperature    104.3
_cell_measurement_theta_max      29.3110
_cell_measurement_theta_min      3.2554
_shelx_estimated_absorpt_T_max   0.902
_shelx_estimated_absorpt_T_min   0.768
_exptl_absorpt_coefficient_mu    0.698
_exptl_absorpt_correction_T_max  0.901
_exptl_absorpt_correction_T_min  0.778
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.293
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             3528
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.15
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0350
_diffrn_reflns_av_unetI/netI     0.0537
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            19521
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.999
_diffrn_reflns_theta_min         3.262
_diffrn_ambient_temperature      104.3
_diffrn_detector_area_resol_mean 16.0971
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       ?
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5737
_reflns_number_total             8381
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_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    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         1.104
_refine_diff_density_min         -1.006
_refine_diff_density_rms         0.094
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     475
_refine_ls_number_reflns         8381
_refine_ls_number_restraints     46
_refine_ls_R_factor_all          0.1174
_refine_ls_R_factor_gt           0.0843
_refine_ls_restrained_S_all      1.056
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0647P)²+80.2263P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1900
_refine_ls_wR_factor_ref         0.2119
_refine_special_details          ', SQUEEZE'
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, H20 of O20, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, H14 of O14
2. Restrained distances
 C16-C15
 1.53 with sigma of 0.02
 C17-C16
 1.53 with sigma of 0.02
3. Rigid bond restraints
 C20, C0AA
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C10, C11, C12, C13
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C15, C16
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C17, O20
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C20 \\sim C0AA: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08
C10 \\sim C11 \\sim C12 \\sim C13: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08
C15 \\sim C16: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
C17 \\sim O20: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
5. Others
 Sof(H17C)=Sof(H17D)=Sof(O20)=Sof(H20)=1-FVAR(1)
 Sof(O14)=Sof(H14)=Sof(H17A)=Sof(H17B)=FVAR(1)
 Sof(H20C)=Sof(H20D)=Sof(C0AA)=Sof(H0AA)=Sof(H0AB)=Sof(H0AC)=1-FVAR(2)
 Sof(H20A)=Sof(H20B)=Sof(C21)=Sof(H21A)=Sof(H21B)=Sof(H21C)=FVAR(2)
6.a Rotating group:
 O20(H20)
6.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C30(H30A,H30B), C1(H1A,H1B), C27(H27A,H27B), C22(H22A,H22B),
 C3(H3A,H3B), C24(H24A,H24B), C23(H23A,H23B), C26(H26A,H26B), C20(H20A,H20B),
 C20(H20C,H20D), C18(H18A,H18B), C19(H19A,H19B), C32(H32A,H32B), C6(H6A,H6B),
 C28(H28A,H28B), C31(H31A,H31B), C7(H7A,H7B), C8(H8A,H8B), C15(H15A,H15B),
 C9(H9A,H9B), C10(H10A,H10B), C14(H14A,H14B), C11(H11A,H11B), C13(H13A,H13B),
 C12(H12A,H12B), C16(H16A,H16B), C17(H17A,H17B), C17(H17C,H17D)
6.c Idealised Me refined as rotating group:
 C29(H29A,H29B,H29C), C21(H21A,H21B,H21C), C25(H25A,H25B,H25C), C33(H33A,H33B,
 H33C), C0AA(H0AA,H0AB,H0AC)
6.d Idealised tetrahedral OH refined as rotating group:
 O14(H14)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_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 0.10147(4) 0.87241(5) 0.21390(3) 0.0283(2) Uani 1 1 d . . . . .
V2 V -0.05660(5) 0.77718(5) 0.20304(3) 0.0312(2) Uani 1 1 d . . . . .
V3 V -0.05675(5) 0.96835(5) 0.20294(3) 0.0299(2) Uani 1 1 d . . . . .
O1 O 0.0000 0.8724(3) 0.2500 0.0232(9) Uani 1 2 d S T P . .
O10 O 0.03574(18) 0.7952(2) 0.17222(12) 0.0295(8) Uani 1 1 d . . . . .
O2 O 0.0000 1.0275(3) 0.2500 0.0344(12) Uani 1 2 d S T P . .
O11 O 0.03618(19) 0.9495(2) 0.17279(11) 0.0295(8) Uani 1 1 d . . . . .
O4 O 0.12805(19) 0.7952(2) 0.25898(14) 0.0389(9) Uani 1 1 d . . . . .
O3 O 0.1284(2) 0.9498(2) 0.25883(12) 0.0381(9) Uani 1 1 d . . . . .
O5 O 0.0000 0.7178(3) 0.2500 0.0405(13) Uani 1 2 d S T P . .
O9 O -0.09142(18) 0.8724(2) 0.16354(12) 0.0324(8) Uani 1 1 d . . . . .
O6 O 0.16527(19) 0.8724(2) 0.18007(13) 0.0392(9) Uani 1 1 d . . . . .
O8 O -0.0936(2) 1.0296(2) 0.16247(13) 0.0431(10) Uani 1 1 d . . . . .
O7 O -0.0932(2) 0.7147(2) 0.16356(16) 0.0474(10) Uani 1 1 d . . . . .
N1 N 0.2035(2) 1.1288(3) 0.18519(17) 0.0396(11) Uani 1 1 d . . . . .
C2 C 0.0299(3) 0.7993(3) 0.11967(19) 0.0356(12) Uani 1 1 d . . . . .
H2A H 0.0039 0.7541 0.1049 0.043 Uiso 1 1 calc R . . . .
H2B H 0.0791 0.7994 0.1106 0.043 Uiso 1 1 calc R . . . .
O12 O 0.0495(3) 0.8856(3) 0.03014(15) 0.0713(15) Uani 1 1 d . . . . .
C30 C 0.1191(3) 1.1266(3) 0.1809(2) 0.0407(13) Uani 1 1 d . . . . .
H30A H 0.0990 1.1017 0.1499 0.049 Uiso 1 1 calc R . . . .
H30B H 0.1062 1.0949 0.2075 0.049 Uiso 1 1 calc R . . . .
C1 C 0.0304(3) 0.9458(3) 0.12024(18) 0.0360(12) Uani 1 1 d . . . . .
H1A H 0.0796 0.9457 0.1112 0.043 Uiso 1 1 calc R . . . .
H1B H 0.0044 0.9911 0.1056 0.043 Uiso 1 1 calc R . . . .
C5 C -0.0158(4) 0.8726(4) 0.0431(2) 0.0504(15) Uani 1 1 d . . . . .
C27 C 0.1999(4) 1.1318(4) 0.0894(2) 0.0561(17) Uani 1 1 d . . . . .
H27A H 0.2103 1.0768 0.0910 0.067 Uiso 1 1 calc R . . . .
H27B H 0.1468 1.1386 0.0807 0.067 Uiso 1 1 calc R . . . .
C22 C 0.2374(4) 1.1749(4) 0.2299(2) 0.0480(15) Uani 1 1 d . . . . .
H22A H 0.2205 1.2279 0.2253 0.058 Uiso 1 1 calc R . . . .
H22B H 0.2907 1.1751 0.2312 0.058 Uiso 1 1 calc R . . . .
C3 C -0.0909(3) 0.8725(4) 0.11092(18) 0.0384(12) Uani 1 1 d . . . . .
H3A H -0.1167 0.9180 0.0963 0.046 Uiso 1 1 calc R . . . .
H3B H -0.1170 0.8272 0.0962 0.046 Uiso 1 1 calc R . . . .
O13 O -0.0696(3) 0.8626(5) 0.01427(18) 0.112(3) Uani 1 1 d . . . . .
C24 C 0.2546(4) 1.2037(4) 0.3193(2) 0.0629(19) Uani 1 1 d . . . . .
H24A H 0.3073 1.2077 0.3183 0.075 Uiso 1 1 calc R . . . .
H24B H 0.2328 1.2543 0.3117 0.075 Uiso 1 1 calc R . . . .
C23 C 0.2205(4) 1.1467(4) 0.2797(2) 0.0587(19) Uani 1 1 d . . . . .
H23A H 0.2413 1.0956 0.2868 0.070 Uiso 1 1 calc R . . . .
H23B H 0.1673 1.1438 0.2791 0.070 Uiso 1 1 calc R . . . .
C26 C 0.2269(3) 1.1690(4) 0.1402(2) 0.0421(14) Uani 1 1 d . . . . .
H26A H 0.2806 1.1711 0.1450 0.051 Uiso 1 1 calc R . . . .
H26B H 0.2090 1.2218 0.1393 0.051 Uiso 1 1 calc R . . . .
C4 C -0.0115(3) 0.8723(3) 0.0996(2) 0.0356(12) Uani 1 1 d . . . . .
C20 C 0.3330(3) 0.9492(4) 0.1886(2) 0.0490(16) Uani 1 1 d . U . . .
H20A H 0.3851 0.9412 0.2010 0.059 Uiso 0.796(12) 1 calc R . . A 1
H20B H 0.3046 0.9176 0.2082 0.059 Uiso 0.796(12) 1 calc R . . A 1
H20C H 0.2951 0.9245 0.1649 0.059 Uiso 0.204(12) 1 calc R . . A 2
H20D H 0.3799 0.9450 0.1764 0.059 Uiso 0.204(12) 1 calc R . . A 2
C18 C 0.2298(3) 1.0460(3) 0.1892(2) 0.0401(13) Uani 1 1 d . . . . .
H18A H 0.2067 1.0183 0.1600 0.048 Uiso 1 1 calc R . . . .
H18B H 0.2127 1.0226 0.2176 0.048 Uiso 1 1 calc R . . . .
C19 C 0.3135(3) 1.0347(4) 0.1945(3) 0.0544(17) Uani 1 1 d . . . . .
H19A H 0.3367 1.0529 0.2268 0.065 Uiso 1 1 calc R . . . .
H19B H 0.3327 1.0651 0.1695 0.065 Uiso 1 1 calc R . . . .
C32 C -0.0003(4) 1.1972(4) 0.1741(3) 0.066(2) Uani 1 1 d . . . . .
H32A H -0.0153 1.1627 0.1987 0.079 Uiso 1 1 calc R . . . .
H32B H -0.0162 1.1746 0.1417 0.079 Uiso 1 1 calc R . . . .
C29 C 0.3178(5) 1.1485(5) 0.0522(3) 0.078(2) Uani 1 1 d . . . . .
H29A H 0.3367 1.1717 0.0248 0.118 Uiso 1 1 calc GR . . . .
H29B H 0.3228 1.0934 0.0507 0.118 Uiso 1 1 calc GR . . . .
H29C H 0.3453 1.1673 0.0828 0.118 Uiso 1 1 calc GR . . . .
C6 C 0.0544(6) 0.8906(5) -0.0232(2) 0.081(3) Uani 1 1 d . . . . .
H6A H 0.0166 0.9251 -0.0399 0.098 Uiso 1 1 calc R . . . .
H6B H 0.0480 0.8400 -0.0386 0.098 Uiso 1 1 calc R . . . .
C21 C 0.3167(4) 0.9250(5) 0.1357(3) 0.053(3) Uani 0.796(12) 1 d . . . A 1
H21A H 0.2649 0.9321 0.1236 0.079 Uiso 0.796(12) 1 calc GR . . A 1
H21B H 0.3293 0.8715 0.1329 0.079 Uiso 0.796(12) 1 calc GR . . A 1
H21C H 0.3454 0.9557 0.1164 0.079 Uiso 0.796(12) 1 calc GR . . A 1
C28 C 0.2386(4) 1.1689(5) 0.0498(2) 0.064(2) Uani 1 1 d . . . . .
H28A H 0.2125 1.1541 0.0175 0.076 Uiso 1 1 calc R . . . .
H28B H 0.2347 1.2246 0.0525 0.076 Uiso 1 1 calc R . . . .
C25 C 0.2434(6) 1.1809(6) 0.3706(3) 0.096(3) Uani 1 1 d . . . . .
H25A H 0.1916 1.1726 0.3712 0.143 Uiso 1 1 calc GR . . . .
H25B H 0.2613 1.2213 0.3935 0.143 Uiso 1 1 calc GR . . . .
H25C H 0.2703 1.1341 0.3800 0.143 Uiso 1 1 calc GR . . . .
C31 C 0.0827(4) 1.2041(4) 0.1828(3) 0.065(2) Uani 1 1 d . . . . .
H31A H 0.0980 1.2376 0.1578 0.078 Uiso 1 1 calc R . . . .
H31B H 0.0988 1.2275 0.2149 0.078 Uiso 1 1 calc R . . . .
C33 C -0.0391(5) 1.2753(5) 0.1769(4) 0.116(4) Uani 1 1 d . . . . .
H33A H -0.0168 1.3129 0.1580 0.173 Uiso 1 1 calc GR . . . .
H33B H -0.0341 1.2916 0.2108 0.173 Uiso 1 1 calc GR . . . .
H33C H -0.0906 1.2701 0.1635 0.173 Uiso 1 1 calc GR . . . .
C7 C 0.1326(6) 0.9226(7) -0.0259(3) 0.102(4) Uani 1 1 d . . . . .
H7A H 0.1360 0.9314 -0.0605 0.123 Uiso 1 1 calc R . . . .
H7B H 0.1368 0.9725 -0.0096 0.123 Uiso 1 1 calc R . . . .
C8 C 0.1965(7) 0.8767(6) -0.0048(3) 0.104(3) Uani 1 1 d . . . . .
H8A H 0.1945 0.8278 -0.0223 0.125 Uiso 1 1 calc R . . . .
H8B H 0.1924 0.8654 0.0295 0.125 Uiso 1 1 calc R . . . .
C15 C 0.6920(9) 0.8863(7) 0.0820(4) 0.139(5) Uani 1 1 d D U . . .
H15A H 0.7028 0.9110 0.0521 0.167 Uiso 1 1 calc R . . . .
H15B H 0.7254 0.8427 0.0890 0.167 Uiso 1 1 calc R . . . .
C9 C 0.2707(6) 0.9130(7) -0.0062(3) 0.103(4) Uani 1 1 d . . . . .
H9A H 0.2752 0.9583 0.0150 0.124 Uiso 1 1 calc R . . . .
H9B H 0.2723 0.9304 -0.0397 0.124 Uiso 1 1 calc R . . . .
C10 C 0.3381(8) 0.8606(7) 0.0101(4) 0.120(4) Uani 1 1 d . U . . .
H10A H 0.3346 0.8400 0.0427 0.144 Uiso 1 1 calc R . . . .
H10B H 0.3357 0.8172 -0.0126 0.144 Uiso 1 1 calc R . . . .
C14 C 0.6177(6) 0.8582(11) 0.0732(4) 0.160(7) Uani 1 1 d . . . . .
H14A H 0.6073 0.8430 0.1056 0.192 Uiso 1 1 calc R . . . .
H14B H 0.6203 0.8105 0.0549 0.192 Uiso 1 1 calc R . . . .
C11 C 0.4092(8) 0.8973(8) 0.0121(5) 0.137(4) Uani 1 1 d . U . . .
H11A H 0.4112 0.9402 0.0351 0.164 Uiso 1 1 calc R . . . .
H11B H 0.4115 0.9190 -0.0204 0.164 Uiso 1 1 calc R . . . .
C13 C 0.5497(8) 0.8954(7) 0.0493(6) 0.140(4) Uani 1 1 d . U . . .
H13A H 0.5625 0.9271 0.0226 0.168 Uiso 1 1 calc R . . . .
H13B H 0.5338 0.9304 0.0733 0.168 Uiso 1 1 calc R . . . .
C12 C 0.4823(9) 0.8464(8) 0.0277(6) 0.161(5) Uani 1 1 d . U . . .
H12A H 0.4729 0.8085 0.0522 0.193 Uiso 1 1 calc R . . . .
H12B H 0.4934 0.8187 -0.0011 0.193 Uiso 1 1 calc R . . . .
O14 O 0.7308(4) 0.8493(4) 0.1801(5) 0.122(5) Uani 0.758(12) 1 d . . . B 1
H14 H 0.7757 0.8551 0.1877 0.184 Uiso 0.758(12) 1 calc GR . . B 1
C16 C 0.7068(7) 0.9424(5) 0.1240(3) 0.100(3) Uani 1 1 d D U . . .
H16A H 0.7569 0.9617 0.1252 0.120 Uiso 1 1 calc R . . . .
H16B H 0.6736 0.9860 0.1162 0.120 Uiso 1 1 calc R . . . .
C17 C 0.6994(6) 0.9160(6) 0.1722(4) 0.102(3) Uani 1 1 d D U . . .
H17A H 0.7223 0.9527 0.1967 0.123 Uiso 0.758(12) 1 calc R . . B 1
H17B H 0.6473 0.9119 0.1751 0.123 Uiso 0.758(12) 1 calc R . . B 1
H17C H 0.7470 0.8937 0.1856 0.123 Uiso 0.242(12) 1 calc R . . B 2
H17D H 0.6944 0.9622 0.1915 0.123 Uiso 0.242(12) 1 calc R . . B 2
O20 O 0.6494(12) 0.8673(12) 0.1837(8) 0.071(8) Uani 0.242(12) 1 d . U . B 2
H20 H 0.6024 0.8562 0.1804 0.085 Uiso 0.242(12) 1 d GR . . B 2
C0AA C 0.3380(15) 0.911(2) 0.2373(11) 0.050(8) Uani 0.204(12) 1 d . U . A 2
H0AA H 0.3696 0.9406 0.2617 0.075 Uiso 0.204(12) 1 calc GR . . A 2
H0AB H 0.3583 0.8601 0.2354 0.075 Uiso 0.204(12) 1 calc GR . . A 2
H0AC H 0.2895 0.9074 0.2464 0.075 Uiso 0.204(12) 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 3.0200(12) 2 ?
V1 V3 3.0278(12) 2 ?
V1 O1 2.2326(8) . ?
V1 O10 2.024(3) . ?
V1 O11 2.011(3) . ?
V1 O4 1.830(4) . ?
V1 O3 1.831(4) . ?
V1 O6 1.598(4) . ?
V2 V1 3.0201(12) 2 ?
V2 V2 3.0331(17) 2 ?
V2 O1 2.239(4) . ?
V2 O10 2.025(3) . ?
V2 O4 1.818(4) 2 ?
V2 O5 1.832(3) . ?
V2 O9 2.017(4) . ?
V2 O7 1.598(4) . ?
V3 V1 3.0279(12) 2 ?
V3 V3 3.0400(17) 2 ?
V3 O1 2.252(4) . ?
V3 O2 1.832(3) . ?
V3 O11 2.027(4) . ?
V3 O3 1.826(4) 2 ?
V3 O9 2.026(4) . ?
V3 O8 1.602(4) . ?
O1 V1 2.2327(8) 2 ?
O1 V2 2.239(4) 2 ?
O1 V3 2.252(4) 2 ?
O10 C2 1.425(6) . ?
O2 V3 1.832(3) 2 ?
O11 C1 1.425(6) . ?
O4 V2 1.818(4) 2 ?
O3 V3 1.826(4) 2 ?
O5 V2 1.832(3) 2 ?
O9 C3 1.439(6) . ?
N1 C30 1.527(7) . ?
N1 C22 1.508(7) . ?
N1 C26 1.531(7) . ?
N1 C18 1.510(7) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C2 C4 1.530(7) . ?
O12 C5 1.316(8) . ?
O12 C6 1.476(7) . ?
C30 H30A 0.9700 . ?
C30 H30B 0.9700 . ?
C30 C31 1.502(8) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C1 C4 1.545(7) . ?
C5 O13 1.173(8) . ?
C5 C4 1.532(8) . ?
C27 H27A 0.9700 . ?
C27 H27B 0.9700 . ?
C27 C26 1.539(8) . ?
C27 C28 1.524(9) . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
C22 C23 1.521(8) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C3 C4 1.530(7) . ?
C24 H24A 0.9700 . ?
C24 H24B 0.9700 . ?
C24 C23 1.522(9) . ?
C24 C25 1.502(9) . ?
C23 H23A 0.9700 . ?
C23 H23B 0.9700 . ?
C26 H26A 0.9700 . ?
C26 H26B 0.9700 . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C20 H20C 0.9700 . ?
C20 H20D 0.9700 . ?
C20 C19 1.536(9) . ?
C20 C21 1.490(10) . ?
C20 C0AA 1.47(3) . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
C18 C19 1.525(8) . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C32 H32A 0.9700 . ?
C32 H32B 0.9700 . ?
C32 C31 1.504(10) . ?
C32 C33 1.532(10) . ?
C29 H29A 0.9600 . ?
C29 H29B 0.9600 . ?
C29 H29C 0.9600 . ?
C29 C28 1.480(10) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C6 C7 1.546(13) . ?
C21 H21A 0.9600 . ?
C21 H21B 0.9600 . ?
C21 H21C 0.9600 . ?
C28 H28A 0.9700 . ?
C28 H28B 0.9700 . ?
C25 H25A 0.9600 . ?
C25 H25B 0.9600 . ?
C25 H25C 0.9600 . ?
C31 H31A 0.9700 . ?
C31 H31B 0.9700 . ?
C33 H33A 0.9600 . ?
C33 H33B 0.9600 . ?
C33 H33C 0.9600 . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C7 C8 1.454(13) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C8 C9 1.501(14) . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C15 C14 1.427(16) . ?
C15 C16 1.494(11) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C9 C10 1.539(16) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C10 C11 1.440(16) . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C14 C13 1.459(15) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C11 C12 1.600(18) . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C13 C12 1.536(18) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
O14 H14 0.8200 . ?
O14 C17 1.291(12) . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C16 C17 1.420(10) . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C17 H17C 0.9700 . ?
C17 H17D 0.9700 . ?
C17 O20 1.32(2) . ?
O20 H20 0.8703 . ?
C0AA H0AA 0.9600 . ?
C0AA H0AB 0.9600 . ?
C0AA H0AC 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
V2 V1 V3 66.32(3) 2 2 ?
O1 V1 V2 47.60(9) . 2 ?
O1 V1 V3 47.79(9) . 2 ?
O10 V1 V2 81.69(10) . 2 ?
O10 V1 V3 125.30(10) . 2 ?
O10 V1 O1 77.73(13) . . ?
O11 V1 V2 125.05(10) . 2 ?
O11 V1 V3 81.32(10) . 2 ?
O11 V1 O1 77.63(13) . . ?
O11 V1 O10 82.85(14) . . ?
O4 V1 V2 33.99(11) . 2 ?
O4 V1 V3 88.27(12) . 2 ?
O4 V1 O1 81.59(14) . . ?
O4 V1 O10 88.18(16) . . ?
O4 V1 O11 158.68(15) . . ?
O4 V1 O3 93.90(17) . . ?
O3 V1 V2 88.36(11) . 2 ?
O3 V1 V3 34.06(11) . 2 ?
O3 V1 O1 81.86(15) . . ?
O3 V1 O10 158.95(16) . . ?
O3 V1 O11 87.86(16) . . ?
O6 V1 V2 138.03(15) . 2 ?
O6 V1 V3 137.87(15) . 2 ?
O6 V1 O1 171.01(14) . . ?
O6 V1 O10 95.57(17) . . ?
O6 V1 O11 95.74(17) . . ?
O6 V1 O4 104.38(18) . . ?
O6 V1 O3 104.15(18) . . ?
V1 V2 V2 66.04(3) 2 2 ?
O1 V2 V1 47.43(2) . 2 ?
O1 V2 V2 47.36(8) . 2 ?
O10 V2 V1 124.79(10) . 2 ?
O10 V2 V2 81.34(10) . 2 ?
O10 V2 O1 77.56(10) . . ?
O4 V2 V1 34.26(11) 2 2 ?
O4 V2 V2 88.44(12) 2 2 ?
O4 V2 O1 81.69(11) 2 . ?
O4 V2 O10 158.61(16) 2 . ?
O4 V2 O5 94.23(13) 2 . ?
O4 V2 O9 88.32(16) 2 . ?
O5 V2 V1 88.27(10) . 2 ?
O5 V2 V2 34.13(13) . 2 ?
O5 V2 O1 81.49(16) . . ?
O5 V2 O10 87.81(11) . . ?
O5 V2 O9 158.29(17) . . ?
O9 V2 V1 81.74(10) . 2 ?
O9 V2 V2 124.67(10) . 2 ?
O9 V2 O1 77.56(13) . . ?
O9 V2 O10 82.26(14) . . ?
O7 V2 V1 137.92(15) . 2 ?
O7 V2 V2 136.77(16) . 2 ?
O7 V2 O1 172.50(17) . . ?
O7 V2 O10 96.40(18) . . ?
O7 V2 O4 103.85(19) . 2 ?
O7 V2 O5 102.9(2) . . ?
O7 V2 O9 97.36(19) . . ?
V1 V3 V3 66.04(3) 2 2 ?
O1 V3 V1 47.26(2) . 2 ?
O1 V3 V3 47.54(8) . 2 ?
O2 V3 V1 88.24(9) . 2 ?
O2 V3 V3 33.95(12) . 2 ?
O2 V3 O1 81.49(15) . . ?
O2 V3 O11 87.54(10) . . ?
O2 V3 O9 157.82(16) . . ?
O11 V3 V1 123.95(10) . 2 ?
O11 V3 V3 80.77(10) . 2 ?
O11 V3 O1 76.87(10) . . ?
O3 V3 V1 34.17(11) 2 2 ?
O3 V3 V3 88.35(12) 2 2 ?
O3 V3 O1 81.44(11) 2 . ?
O3 V3 O2 94.25(13) 2 . ?
O3 V3 O11 157.73(15) 2 . ?
O3 V3 O9 88.14(16) 2 . ?
O9 V3 V1 81.40(10) . 2 ?
O9 V3 V3 124.36(10) . 2 ?
O9 V3 O1 77.07(13) . . ?
O9 V3 O11 82.19(14) . . ?
O8 V3 V1 138.31(16) . 2 ?
O8 V3 V3 137.84(15) . 2 ?
O8 V3 O1 171.28(15) . . ?
O8 V3 O2 104.2(2) . . ?
O8 V3 O11 96.60(17) . . ?
O8 V3 O3 104.43(19) . 2 ?
O8 V3 O9 96.48(17) . . ?
V1 O1 V1 180.0(2) . 2 ?
V1 O1 V2 95.06(10) 2 2 ?
V1 O1 V2 84.97(9) . 2 ?
V1 O1 V2 95.06(10) . . ?
V1 O1 V2 84.97(9) 2 . ?
V1 O1 V3 95.02(10) . . ?
V1 O1 V3 84.94(9) 2 . ?
V1 O1 V3 84.94(9) . 2 ?
V1 O1 V3 95.02(10) 2 2 ?
V2 O1 V2 85.28(17) 2 . ?
V2 O1 V3 179.82(16) 2 . ?
V2 O1 V3 179.82(16) . 2 ?
V2 O1 V3 94.90(3) 2 2 ?
V2 O1 V3 94.90(3) . . ?
V3 O1 V3 84.92(17) 2 . ?
V1 O10 V2 109.13(16) . . ?
C2 O10 V1 118.6(3) . . ?
C2 O10 V2 119.4(3) . . ?
V3 O2 V3 112.1(2) 2 . ?
V1 O11 V3 109.98(15) . . ?
C1 O11 V1 118.5(3) . . ?
C1 O11 V3 118.8(3) . . ?
V2 O4 V1 111.76(18) 2 . ?
V3 O3 V1 111.76(18) 2 . ?
V2 O5 V2 111.7(3) . 2 ?
V2 O9 V3 109.82(15) . . ?
C3 O9 V2 119.0(3) . . ?
C3 O9 V3 118.6(3) . . ?
C30 N1 C26 110.8(4) . . ?
C22 N1 C30 110.9(5) . . ?
C22 N1 C26 106.2(4) . . ?
C22 N1 C18 110.9(4) . . ?
C18 N1 C30 106.8(4) . . ?
C18 N1 C26 111.3(4) . . ?
O10 C2 H2A 109.5 . . ?
O10 C2 H2B 109.5 . . ?
O10 C2 C4 110.9(4) . . ?
H2A C2 H2B 108.0 . . ?
C4 C2 H2A 109.5 . . ?
C4 C2 H2B 109.5 . . ?
C5 O12 C6 118.3(6) . . ?
N1 C30 H30A 108.5 . . ?
N1 C30 H30B 108.5 . . ?
H30A C30 H30B 107.5 . . ?
C31 C30 N1 115.0(5) . . ?
C31 C30 H30A 108.5 . . ?
C31 C30 H30B 108.5 . . ?
O11 C1 H1A 109.4 . . ?
O11 C1 H1B 109.4 . . ?
O11 C1 C4 111.1(4) . . ?
H1A C1 H1B 108.0 . . ?
C4 C1 H1A 109.4 . . ?
C4 C1 H1B 109.4 . . ?
O12 C5 C4 111.5(5) . . ?
O13 C5 O12 123.0(6) . . ?
O13 C5 C4 125.5(7) . . ?
H27A C27 H27B 108.1 . . ?
C26 C27 H27A 109.6 . . ?
C26 C27 H27B 109.6 . . ?
C28 C27 H27A 109.6 . . ?
C28 C27 H27B 109.6 . . ?
C28 C27 C26 110.2(5) . . ?
N1 C22 H22A 108.3 . . ?
N1 C22 H22B 108.3 . . ?
N1 C22 C23 116.1(5) . . ?
H22A C22 H22B 107.4 . . ?
C23 C22 H22A 108.3 . . ?
C23 C22 H22B 108.3 . . ?
O9 C3 H3A 109.5 . . ?
O9 C3 H3B 109.5 . . ?
O9 C3 C4 110.9(4) . . ?
H3A C3 H3B 108.0 . . ?
C4 C3 H3A 109.5 . . ?
C4 C3 H3B 109.5 . . ?
H24A C24 H24B 107.8 . . ?
C23 C24 H24A 109.0 . . ?
C23 C24 H24B 109.0 . . ?
C25 C24 H24A 109.0 . . ?
C25 C24 H24B 109.0 . . ?
C25 C24 C23 113.1(6) . . ?
C22 C23 C24 108.1(5) . . ?
C22 C23 H23A 110.1 . . ?
C22 C23 H23B 110.1 . . ?
C24 C23 H23A 110.1 . . ?
C24 C23 H23B 110.1 . . ?
H23A C23 H23B 108.4 . . ?
N1 C26 C27 116.4(5) . . ?
N1 C26 H26A 108.2 . . ?
N1 C26 H26B 108.2 . . ?
C27 C26 H26A 108.2 . . ?
C27 C26 H26B 108.2 . . ?
H26A C26 H26B 107.3 . . ?
C2 C4 C1 111.0(4) . . ?
C2 C4 C5 108.0(4) . . ?
C2 C4 C3 111.2(5) . . ?
C5 C4 C1 108.0(5) . . ?
C3 C4 C1 110.8(4) . . ?
C3 C4 C5 107.7(4) . . ?
H20A C20 H20B 108.0 . . ?
H20C C20 H20D 108.3 . . ?
C19 C20 H20A 109.4 . . ?
C19 C20 H20B 109.4 . . ?
C19 C20 H20C 109.9 . . ?
C19 C20 H20D 109.9 . . ?
C21 C20 H20A 109.4 . . ?
C21 C20 H20B 109.4 . . ?
C21 C20 C19 111.0(6) . . ?
C0AA C20 H20C 109.9 . . ?
C0AA C20 H20D 109.9 . . ?
C0AA C20 C19 108.7(14) . . ?
N1 C18 H18A 108.4 . . ?
N1 C18 H18B 108.4 . . ?
N1 C18 C19 115.6(5) . . ?
H18A C18 H18B 107.4 . . ?
C19 C18 H18A 108.4 . . ?
C19 C18 H18B 108.4 . . ?
C20 C19 H19A 109.4 . . ?
C20 C19 H19B 109.4 . . ?
C18 C19 C20 111.0(5) . . ?
C18 C19 H19A 109.4 . . ?
C18 C19 H19B 109.4 . . ?
H19A C19 H19B 108.0 . . ?
H32A C32 H32B 107.8 . . ?
C31 C32 H32A 109.1 . . ?
C31 C32 H32B 109.1 . . ?
C31 C32 C33 112.7(7) . . ?
C33 C32 H32A 109.1 . . ?
C33 C32 H32B 109.1 . . ?
H29A C29 H29B 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C28 C29 H29A 109.5 . . ?
C28 C29 H29B 109.5 . . ?
C28 C29 H29C 109.5 . . ?
O12 C6 H6A 110.6 . . ?
O12 C6 H6B 110.6 . . ?
O12 C6 C7 105.5(6) . . ?
H6A C6 H6B 108.8 . . ?
C7 C6 H6A 110.6 . . ?
C7 C6 H6B 110.6 . . ?
C20 C21 H21A 109.5 . . ?
C20 C21 H21B 109.5 . . ?
C20 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C27 C28 H28A 108.5 . . ?
C27 C28 H28B 108.5 . . ?
C29 C28 C27 115.3(6) . . ?
C29 C28 H28A 108.5 . . ?
C29 C28 H28B 108.5 . . ?
H28A C28 H28B 107.5 . . ?
C24 C25 H25A 109.5 . . ?
C24 C25 H25B 109.5 . . ?
C24 C25 H25C 109.5 . . ?
H25A C25 H25B 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C30 C31 C32 111.5(6) . . ?
C30 C31 H31A 109.3 . . ?
C30 C31 H31B 109.3 . . ?
C32 C31 H31A 109.3 . . ?
C32 C31 H31B 109.3 . . ?
H31A C31 H31B 108.0 . . ?
C32 C33 H33A 109.5 . . ?
C32 C33 H33B 109.5 . . ?
C32 C33 H33C 109.5 . . ?
H33A C33 H33B 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C6 C7 H7A 107.7 . . ?
C6 C7 H7B 107.7 . . ?
H7A C7 H7B 107.1 . . ?
C8 C7 C6 118.4(9) . . ?
C8 C7 H7A 107.7 . . ?
C8 C7 H7B 107.7 . . ?
C7 C8 H8A 108.4 . . ?
C7 C8 H8B 108.4 . . ?
C7 C8 C9 115.6(10) . . ?
H8A C8 H8B 107.4 . . ?
C9 C8 H8A 108.4 . . ?
C9 C8 H8B 108.4 . . ?
H15A C15 H15B 107.7 . . ?
C14 C15 H15A 108.8 . . ?
C14 C15 H15B 108.8 . . ?
C14 C15 C16 113.8(12) . . ?
C16 C15 H15A 108.8 . . ?
C16 C15 H15B 108.8 . . ?
C8 C9 H9A 108.4 . . ?
C8 C9 H9B 108.4 . . ?
C8 C9 C10 115.6(10) . . ?
H9A C9 H9B 107.4 . . ?
C10 C9 H9A 108.4 . . ?
C10 C9 H9B 108.4 . . ?
C9 C10 H10A 108.4 . . ?
C9 C10 H10B 108.4 . . ?
H10A C10 H10B 107.5 . . ?
C11 C10 C9 115.3(10) . . ?
C11 C10 H10A 108.4 . . ?
C11 C10 H10B 108.4 . . ?
C15 C14 H14A 104.7 . . ?
C15 C14 H14B 104.7 . . ?
C15 C14 C13 130.3(15) . . ?
H14A C14 H14B 105.7 . . ?
C13 C14 H14A 104.7 . . ?
C13 C14 H14B 104.7 . . ?
C10 C11 H11A 107.7 . . ?
C10 C11 H11B 107.7 . . ?
C10 C11 C12 118.5(12) . . ?
H11A C11 H11B 107.1 . . ?
C12 C11 H11A 107.7 . . ?
C12 C11 H11B 107.7 . . ?
C14 C13 H13A 107.3 . . ?
C14 C13 H13B 107.3 . . ?
C14 C13 C12 120.2(12) . . ?
H13A C13 H13B 106.9 . . ?
C12 C13 H13A 107.3 . . ?
C12 C13 H13B 107.3 . . ?
C11 C12 H12A 109.1 . . ?
C11 C12 H12B 109.1 . . ?
C13 C12 C11 112.6(12) . . ?
C13 C12 H12A 109.1 . . ?
C13 C12 H12B 109.1 . . ?
H12A C12 H12B 107.8 . . ?
C17 O14 H14 109.5 . . ?
C15 C16 H16A 107.8 . . ?
C15 C16 H16B 107.8 . . ?
H16A C16 H16B 107.1 . . ?
C17 C16 C15 118.0(9) . . ?
C17 C16 H16A 107.8 . . ?
C17 C16 H16B 107.8 . . ?
O14 C17 C16 109.8(11) . . ?
O14 C17 H17A 109.7 . . ?
O14 C17 H17B 109.7 . . ?
C16 C17 H17A 109.7 . . ?
C16 C17 H17B 109.7 . . ?
C16 C17 H17C 105.6 . . ?
C16 C17 H17D 105.6 . . ?
H17A C17 H17B 108.2 . . ?
H17C C17 H17D 106.1 . . ?
O20 C17 C16 126.7(13) . . ?
O20 C17 H17C 105.6 . . ?
O20 C17 H17D 105.6 . . ?
C17 O20 H20 145.8 . . ?
C20 C0AA H0AA 109.5 . . ?
C20 C0AA H0AB 109.5 . . ?
C20 C0AA H0AC 109.5 . . ?
H0AA C0AA H0AB 109.5 . . ?
H0AA C0AA H0AC 109.5 . . ?
H0AB C0AA H0AC 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 O5 V2 -47.17(2) 2 . . 2 ?
V1 V3 O2 V3 47.01(2) 2 . . 2 ?
V1 O10 C2 C4 -68.8(5) . . . . ?
V1 O11 C1 C4 68.8(5) . . . . ?
V2 V1 O3 V3 -47.54(18) 2 . . 2 ?
V2 O10 C2 C4 68.6(5) . . . . ?
V2 O9 C3 C4 -68.7(5) . . . . ?
V3 V1 O4 V2 47.63(19) 2 . . 2 ?
V3 O11 C1 C4 -69.1(5) . . . . ?
V3 O9 C3 C4 69.4(5) . . . . ?
O1 V1 O4 V2 0.08(19) . . . 2 ?
O1 V1 O3 V3 -0.18(19) . . . 2 ?
O1 V2 O5 V2 -0.002(0) . . . 2 ?
O1 V3 O2 V3 0.000(0) . . . 2 ?
O10 V1 O4 V2 -77.8(2) . . . 2 ?
O10 V1 O3 V3 14.0(6) . . . 2 ?
O10 V2 O5 V2 77.75(10) . . . 2 ?
O10 C2 C4 C1 61.9(6) . . . . ?
O10 C2 C4 C5 -179.9(5) . . . . ?
O10 C2 C4 C3 -61.9(5) . . . . ?
O11 V1 O4 V2 -12.9(6) . . . 2 ?
O11 V1 O3 V3 77.6(2) . . . 2 ?
O11 V3 O2 V3 -77.09(10) . . . 2 ?
O11 C1 C4 C2 -62.0(6) . . . . ?
O11 C1 C4 C5 179.8(4) . . . . ?
O11 C1 C4 C3 62.0(6) . . . . ?
O4 V1 O3 V3 -81.1(2) . . . 2 ?
O4 V2 O5 V2 -80.93(12) 2 . . 2 ?
O3 V1 O4 V2 81.2(2) . . . 2 ?
O3 V3 O2 V3 80.67(12) 2 . . 2 ?
O9 V2 O5 V2 15.2(3) . . . 2 ?
O9 V3 O2 V3 -14.9(3) . . . 2 ?
O9 C3 C4 C2 62.0(6) . . . . ?
O9 C3 C4 C1 -62.0(6) . . . . ?
O9 C3 C4 C5 -179.9(5) . . . . ?
O6 V1 O4 V2 -173.1(2) . . . 2 ?
O6 V1 O3 V3 173.0(2) . . . 2 ?
O8 V3 O2 V3 -173.27(16) . . . 2 ?
O7 V2 O5 V2 173.81(16) . . . 2 ?
N1 C30 C31 C32 175.3(5) . . . . ?
N1 C22 C23 C24 -175.9(6) . . . . ?
N1 C18 C19 C20 -169.5(5) . . . . ?
O12 C5 C4 C2 -70.6(7) . . . . ?
O12 C5 C4 C1 49.5(7) . . . . ?
O12 C5 C4 C3 169.2(5) . . . . ?
O12 C6 C7 C8 63.1(10) . . . . ?
C30 N1 C22 C23 58.4(7) . . . . ?
C30 N1 C26 C27 -60.3(7) . . . . ?
C30 N1 C18 C19 -179.3(5) . . . . ?
C5 O12 C6 C7 168.6(7) . . . . ?
C22 N1 C30 C31 51.9(7) . . . . ?
C22 N1 C26 C27 179.1(5) . . . . ?
C22 N1 C18 C19 -58.4(6) . . . . ?
O13 C5 C4 C2 109.4(8) . . . . ?
O13 C5 C4 C1 -130.5(8) . . . . ?
O13 C5 C4 C3 -10.8(10) . . . . ?
C26 N1 C30 C31 -65.9(7) . . . . ?
C26 N1 C22 C23 178.9(6) . . . . ?
C26 N1 C18 C19 59.6(6) . . . . ?
C26 C27 C28 C29 72.1(9) . . . . ?
C18 N1 C30 C31 172.8(5) . . . . ?
C18 N1 C22 C23 -60.1(7) . . . . ?
C18 N1 C26 C27 58.3(6) . . . . ?
C6 O12 C5 O13 2.3(12) . . . . ?
C6 O12 C5 C4 -177.8(6) . . . . ?
C6 C7 C8 C9 -176.8(8) . . . . ?
C21 C20 C19 C18 74.8(7) . . . . ?
C28 C27 C26 N1 -169.7(6) . . . . ?
C25 C24 C23 C22 -178.4(8) . . . . ?
C33 C32 C31 C30 178.8(7) . . . . ?
C7 C8 C9 C10 -172.6(8) . . . . ?
C8 C9 C10 C11 -175.7(9) . . . . ?
C15 C14 C13 C12 158.4(15) . . . . ?
C15 C16 C17 O14 44.8(15) . . . . ?
C15 C16 C17 O20 -37(2) . . . . ?
C9 C10 C11 C12 -178.9(10) . . . . ?
C10 C11 C12 C13 -155.8(12) . . . . ?
C14 C15 C16 C17 62.9(17) . . . . ?
C14 C13 C12 C11 169.7(11) . . . . ?
C16 C15 C14 C13 76.2(18) . . . . ?
C0AA C20 C19 C18 -86.6(13) . . . . ?

_shelx_SHELXL_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_qinshui
_database_code_depnum_ccdc_archive 'CCDC 1503808'
_audit_update_record             
;
2016-09-10 deposited with the CCDC.
2017-02-17 downloaded from the CCDC.
;
_audit_creation_date             2016-09-10
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C24 H42 O29 V6, 2(C16 H36 N)'
_chemical_formula_sum            'C56 H114 N2 O29 V6'
_chemical_formula_weight         1585.13
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_cell_length_a                   13.504(3)
_cell_length_b                   17.740(4)
_cell_length_c                   15.324(3)
_cell_angle_alpha                90
_cell_angle_beta                 108.64(3)
_cell_angle_gamma                90
_cell_volume                     3478.5(13)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    12190
_cell_measurement_temperature    153.1500
_cell_measurement_theta_max      29.1270
_cell_measurement_theta_min      1.9624
_shelx_estimated_absorpt_T_max   0.847
_shelx_estimated_absorpt_T_min   0.679
_exptl_absorpt_coefficient_mu    0.857
_exptl_absorpt_correction_T_max  0.842
_exptl_absorpt_correction_T_min  0.705
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.513
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1668
_exptl_crystal_size_max          0.49
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.2
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0337
_diffrn_reflns_av_unetI/netI     0.0330
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            24997
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.999
_diffrn_reflns_theta_min         1.962
_diffrn_ambient_temperature      153.1500
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  
;
Saturn724+ (2x2 bin mode)
;
_diffrn_measurement_method       dtprofit.ref
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Rotating Anode'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6264
_reflns_number_total             6820
_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       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2008)'
_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    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.766
_refine_diff_density_min         -0.637
_refine_diff_density_rms         0.085
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.114
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     435
_refine_ls_number_reflns         6820
_refine_ls_number_restraints     21
_refine_ls_R_factor_all          0.0646
_refine_ls_R_factor_gt           0.0586
_refine_ls_restrained_S_all      1.113
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0683P)²+3.6987P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1459
_refine_ls_wR_factor_ref         0.1506
_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C1E-C1D
 1.4 with sigma of 0.001
3. Rigid bond restraints
 C1F, C1H, C1I
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4. Uiso/Uaniso restraints and constraints
C1F \\sim C1H \\sim C1I: within 1.7A with sigma of 0.001 and sigma for terminal
atoms of 0.002
5. Others
 Sof(H1FC)=Sof(H1FD)=Sof(C1I)=Sof(H1IA)=Sof(H1IB)=Sof(H1IC)=1-FVAR(1)
 Sof(H1FA)=Sof(H1FB)=Sof(C1H)=Sof(H1HA)=Sof(H1HB)=Sof(H1HC)=FVAR(1)
6.a Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C11(H11A,H11B), C9(H9A,H9B), C7(H7A,H7B), C1(H1A,H1B), C2(H2A,
 H2B), C15(H15A,H15B), C17(H17A,H17B), C20(H20A,H20B), C3(H3A,H3B), C4(H4A,H4B),
  C5(H5A,H5B), C6(H6A,H6B), C10(H10A,H10B), C13(H13A,H13B), C16(H16A,H16B),
 C19(H19A,H19B), C1A(H1AA,H1AB), C1E(H1EA,H1EB), C1F(H1FA,H1FB), C1F(H1FC,H1FD),
  C1G(H1GA,H1GB)
6.b Me refined with riding coordinates:
 C1D(H1DA,H1DB,H1DC), C1I(H1IA,H1IB,H1IC)
6.c Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C), C1B(H1BA,H1BB,H1BC), C1C(H1CA,H1CB,H1CC), C1H(H1HA,H1HB,
 H1HC)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_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 0.45710(4) 0.11516(3) 0.03564(4) 0.03185(16) Uani 1 1 d . . . . .
V2 V 0.41041(4) -0.06187(3) 0.07882(4) 0.03268(16) Uani 1 1 d . . . . .
V3 V 0.37231(4) -0.00544(3) -0.13614(4) 0.03321(16) Uani 1 1 d . . . . .
O1 O 0.34153(16) 0.09302(12) -0.08132(15) 0.0309(5) Uani 1 1 d . . . . .
O2 O 0.53878(17) 0.14340(13) -0.03224(17) 0.0373(5) Uani 1 1 d . . . . .
O4 O 0.56955(17) 0.09630(14) 0.14031(16) 0.0380(5) Uani 1 1 d . . . . .
O5 O 0.5000 0.0000 0.0000 0.0266(6) Uani 1 2 d S T P . .
O6 O 0.37272(16) 0.04619(12) 0.09080(14) 0.0302(5) Uani 1 1 d . . . . .
O7 O 0.47029(18) 0.04758(14) -0.17243(15) 0.0383(5) Uani 1 1 d . . . . .
O8 O 0.40998(18) 0.19283(13) 0.05858(17) 0.0401(6) Uani 1 1 d . . . . .
C8 C 0.2657(2) 0.06485(19) 0.0773(2) 0.0333(7) Uani 1 1 d . . . . .
H8A H 0.2614 0.1164 0.0968 0.040 Uiso 1 1 calc R . . . .
H8B H 0.2387 0.0322 0.1152 0.040 Uiso 1 1 calc R . . . .
C11 C 0.2356(2) 0.10926(19) -0.0858(2) 0.0344(7) Uani 1 1 d . . . . .
H11A H 0.1901 0.1040 -0.1489 0.041 Uiso 1 1 calc R . . . .
H11B H 0.2311 0.1610 -0.0669 0.041 Uiso 1 1 calc R . . . .
C12 C 0.0845(2) 0.07606(18) -0.0305(2) 0.0321(7) Uani 1 1 d . . . . .
C14 C 0.1981(2) 0.05626(19) -0.0237(2) 0.0332(7) Uani 1 1 d . . . . .
O3 O 0.30285(16) -0.04987(12) -0.04921(15) 0.0314(5) Uani 1 1 d . . . . .
O9 O 0.27082(19) -0.00331(15) -0.22621(17) 0.0449(6) Uani 1 1 d . . . . .
O10 O 0.33127(19) -0.09881(14) 0.12561(18) 0.0428(6) Uani 1 1 d . . . . .
O11 O 0.02648(19) 0.09033(17) -0.11482(19) 0.0520(7) Uani 1 1 d . . . . .
O12 O 0.0544(2) 0.07509(18) 0.03572(19) 0.0561(7) Uani 1 1 d . . . . .
C9 C 0.1993(2) -0.02591(19) -0.0566(2) 0.0338(7) Uani 1 1 d . . . . .
H9A H 0.1711 -0.0588 -0.0199 0.041 Uiso 1 1 calc R . . . .
H9B H 0.1550 -0.0300 -0.1203 0.041 Uiso 1 1 calc R . . . .
O13 O -0.0759(2) 0.23553(18) -0.16463(19) 0.0580(8) Uani 1 1 d . . . . .
O14 O -0.1198(2) 0.39863(18) -0.1618(2) 0.0640(8) Uani 1 1 d . . . . .
O15 O -0.1567(3) 0.4962(2) -0.0209(3) 0.0755(10) Uani 1 1 d . . . . .
C7 C -0.1194(3) 0.1652(3) -0.2017(3) 0.0548(10) Uani 1 1 d . . . . .
H7A H -0.0971 0.1524 -0.2540 0.066 Uiso 1 1 calc R . . . .
H7B H -0.1951 0.1684 -0.2226 0.066 Uiso 1 1 calc R . . . .
C1 C -0.0840(3) 0.1064(3) -0.1294(3) 0.0556(11) Uani 1 1 d . . . . .
H1A H -0.0932 0.1239 -0.0725 0.067 Uiso 1 1 calc R . . . .
H1B H -0.1251 0.0609 -0.1487 0.067 Uiso 1 1 calc R . . . .
C2 C -0.1073(4) 0.4766(3) -0.1541(3) 0.0668(13) Uani 1 1 d . . . . .
H2A H -0.1151 0.4982 -0.2141 0.080 Uiso 1 1 calc R . . . .
H2B H -0.0377 0.4885 -0.1135 0.080 Uiso 1 1 calc R . . . .
C15 C -0.1878(4) 0.5100(3) -0.1160(4) 0.0693(13) Uani 1 1 d . . . . .
H15A H -0.1935 0.5639 -0.1276 0.083 Uiso 1 1 calc R . . . .
H15B H -0.2555 0.4873 -0.1459 0.083 Uiso 1 1 calc R . . . .
C17 C -0.0802(4) 0.2894(3) -0.2340(3) 0.0656(13) Uani 1 1 d . . . . .
H17A H -0.1516 0.2938 -0.2747 0.079 Uiso 1 1 calc R . . . .
H17B H -0.0375 0.2722 -0.2703 0.079 Uiso 1 1 calc R . . . .
C20 C -0.0425(4) 0.3649(3) -0.1939(3) 0.0653(12) Uani 1 1 d . . . . .
H20A H 0.0221 0.3594 -0.1432 0.078 Uiso 1 1 calc R . . . .
H20B H -0.0290 0.3967 -0.2403 0.078 Uiso 1 1 calc R . . . .
N1 N 0.7652(3) 0.29883(18) 0.0896(2) 0.0486(8) Uani 1 1 d . . . . .
C3 C 0.6991(3) 0.3585(2) 0.1147(3) 0.0538(10) Uani 1 1 d . . . . .
H3A H 0.6914 0.4007 0.0728 0.065 Uiso 1 1 calc R . . . .
H3B H 0.7359 0.3766 0.1762 0.065 Uiso 1 1 calc R . . . .
C4 C 0.8703(3) 0.3346(2) 0.0970(3) 0.0489(9) Uani 1 1 d . . . . .
H4A H 0.9042 0.3495 0.1605 0.059 Uiso 1 1 calc R . . . .
H4B H 0.8578 0.3800 0.0598 0.059 Uiso 1 1 calc R . . . .
C5 C 0.5904(4) 0.3321(3) 0.1118(4) 0.0679(13) Uani 1 1 d . . . . .
H5A H 0.5648 0.2971 0.0609 0.082 Uiso 1 1 calc R . . . .
H5B H 0.5974 0.3043 0.1680 0.082 Uiso 1 1 calc R . . . .
C6 C 0.7798(4) 0.2318(2) 0.1548(4) 0.0667(13) Uani 1 1 d . . . . .
H6A H 0.7119 0.2097 0.1472 0.080 Uiso 1 1 calc R . . . .
H6B H 0.8218 0.1941 0.1371 0.080 Uiso 1 1 calc R . . . .
C10 C 1.0496(3) 0.3217(3) 0.0862(3) 0.0600(11) Uani 1 1 d . . . . .
H10A H 1.0779 0.3328 0.1515 0.072 Uiso 1 1 calc R . . . .
H10B H 1.0405 0.3691 0.0529 0.072 Uiso 1 1 calc R . . . .
C13 C 0.7126(4) 0.2702(3) -0.0076(3) 0.0596(12) Uani 1 1 d . . . . .
H13A H 0.6495 0.2434 -0.0092 0.071 Uiso 1 1 calc R . . . .
H13B H 0.7589 0.2345 -0.0230 0.071 Uiso 1 1 calc R . . . .
C16 C 0.9450(3) 0.2837(2) 0.0667(3) 0.0564(10) Uani 1 1 d . . . . .
H16A H 0.9536 0.2362 0.0996 0.068 Uiso 1 1 calc R . . . .
H16B H 0.9157 0.2732 0.0013 0.068 Uiso 1 1 calc R . . . .
C18 C 1.1273(4) 0.2719(3) 0.0576(4) 0.0708(13) Uani 1 1 d . . . . .
H18A H 1.1354 0.2246 0.0896 0.106 Uiso 1 1 calc GR . . . .
H18B H 1.1937 0.2969 0.0730 0.106 Uiso 1 1 calc GR . . . .
H18C H 1.1013 0.2631 -0.0076 0.106 Uiso 1 1 calc GR . . . .
C19 C 0.6842(4) 0.3316(3) -0.0806(3) 0.0659(13) Uani 1 1 d . . . . .
H19A H 0.6345 0.3659 -0.0679 0.079 Uiso 1 1 calc R . . . .
H19B H 0.7465 0.3602 -0.0776 0.079 Uiso 1 1 calc R . . . .
C1A C 0.6377(4) 0.2996(4) -0.1760(4) 0.0864(18) Uani 1 1 d . . . . .
H1AA H 0.6896 0.2689 -0.1906 0.104 Uiso 1 1 calc R . . . .
H1AB H 0.5792 0.2673 -0.1773 0.104 Uiso 1 1 calc R . . . .
C1B C -0.2173(5) 0.5370(3) 0.0234(5) 0.0915(18) Uani 1 1 d . . . . .
H1BA H -0.2122 0.5900 0.0127 0.137 Uiso 1 1 calc GR . . . .
H1BB H -0.1917 0.5273 0.0884 0.137 Uiso 1 1 calc GR . . . .
H1BC H -0.2890 0.5215 -0.0008 0.137 Uiso 1 1 calc GR . . . .
C1C C 0.6011(5) 0.3594(4) -0.2469(4) 0.098(2) Uani 1 1 d . . . . .
H1CA H 0.5501 0.3903 -0.2324 0.147 Uiso 1 1 calc GR . . . .
H1CB H 0.5702 0.3366 -0.3062 0.147 Uiso 1 1 calc GR . . . .
H1CC H 0.6593 0.3901 -0.2479 0.147 Uiso 1 1 calc GR . . . .
C1D C 0.5298(5) 0.4626(4) 0.1365(7) 0.157(4) Uani 1 1 d D . . . .
H1DA H 0.4643 0.4889 0.1204 0.235 Uiso 1 1 calc R . . . .
H1DB H 0.5603 0.4613 0.2023 0.235 Uiso 1 1 calc R . . . .
H1DC H 0.5762 0.4882 0.1103 0.235 Uiso 1 1 calc R . . . .
C1E C 0.5132(6) 0.3890(3) 0.1024(7) 0.149(4) Uani 1 1 d D . . . .
H1EA H 0.4781 0.3940 0.0367 0.179 Uiso 1 1 calc R . . . .
H1EB H 0.4623 0.3674 0.1277 0.179 Uiso 1 1 calc R . . . .
C1F C 0.8358(6) 0.1787(4) 0.3120(5) 0.113(2) Uani 1 1 d . U . . .
H1FA H 0.7660 0.1574 0.2926 0.136 Uiso 0.511(8) 1 calc R . . A 1
H1FB H 0.8799 0.1433 0.2933 0.136 Uiso 0.511(8) 1 calc R . . A 1
H1FC H 0.8377 0.1346 0.2753 0.136 Uiso 0.489(8) 1 calc R . . A 2
H1FD H 0.8990 0.1793 0.3648 0.136 Uiso 0.489(8) 1 calc R . . A 2
C1G C 0.8306(6) 0.2501(4) 0.2544(4) 0.100(2) Uani 1 1 d . . . . .
H1GA H 0.7906 0.2886 0.2733 0.120 Uiso 1 1 calc R . . . .
H1GB H 0.9005 0.2693 0.2642 0.120 Uiso 1 1 calc R . . . .
C1H C 0.7496(12) 0.1755(8) 0.3413(10) 0.112(2) Uani 0.511(8) 1 d . U . A 2
H1HA H 0.7106 0.2216 0.3253 0.168 Uiso 0.511(8) 1 calc GR . . A 2
H1HB H 0.7717 0.1690 0.4069 0.168 Uiso 0.511(8) 1 calc GR . . A 2
H1HC H 0.7062 0.1338 0.3122 0.168 Uiso 0.511(8) 1 calc GR . . A 2
C1I C 0.8656(13) 0.1788(8) 0.3957(10) 0.112(2) Uani 0.489(8) 1 d . U . A 1
H1IA H 0.8626 0.1284 0.4177 0.168 Uiso 0.489(8) 1 calc R . . A 1
H1IB H 0.9362 0.1969 0.4181 0.168 Uiso 0.489(8) 1 calc R . . A 1
H1IC H 0.8213 0.2110 0.4174 0.168 Uiso 0.489(8) 1 calc R . . A 1


_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 3.0295(10) 3_655 ?
V1 V3 3.0331(11) 3_655 ?
V1 O1 2.004(2) . ?
V1 O2 1.812(2) . ?
V1 O4 1.853(2) . ?
V1 O5 2.2382(7) . ?
V1 O6 2.031(2) . ?
V1 O8 1.603(2) . ?
V2 V1 3.0296(10) 3_655 ?
V2 V3 3.0264(10) 3_655 ?
V2 O2 1.840(2) 3_655 ?
V2 O5 2.2498(7) . ?
V2 O6 2.007(2) . ?
V2 O7 1.800(2) 3_655 ?
V2 O3 2.045(2) . ?
V2 O10 1.605(2) . ?
V3 V1 3.0330(10) 3_655 ?
V3 V2 3.0264(10) 3_655 ?
V3 O1 2.038(2) . ?
V3 O4 1.803(2) 3_655 ?
V3 O5 2.2440(10) . ?
V3 O7 1.848(2) . ?
V3 O3 2.018(2) . ?
V3 O9 1.605(2) . ?
O1 C11 1.440(4) . ?
O2 V2 1.840(2) 3_655 ?
O4 V3 1.803(2) 3_655 ?
O5 V1 2.2382(7) 3_655 ?
O5 V2 2.2497(7) 3_655 ?
O5 V3 2.2441(10) 3_655 ?
O6 C8 1.432(4) . ?
O7 V2 1.800(2) 3_655 ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C8 C14 1.532(4) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C11 C14 1.534(5) . ?
C12 C14 1.544(4) . ?
C12 O11 1.305(4) . ?
C12 O12 1.207(4) . ?
C14 C9 1.544(5) . ?
O3 C9 1.431(4) . ?
O11 C1 1.464(4) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
O13 C7 1.417(5) . ?
O13 C17 1.417(5) . ?
O14 C2 1.394(6) . ?
O14 C20 1.419(5) . ?
O15 C15 1.404(6) . ?
O15 C1B 1.418(6) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C7 C1 1.486(6) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C2 C15 1.509(7) . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C17 C20 1.494(7) . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
N1 C3 1.512(5) . ?
N1 C4 1.524(5) . ?
N1 C6 1.525(5) . ?
N1 C13 1.518(5) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C3 C5 1.528(6) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C4 C16 1.533(6) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C5 C1E 1.425(7) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C6 C1G 1.495(8) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C10 C16 1.507(6) . ?
C10 C18 1.539(6) . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C13 C19 1.520(7) . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C19 C1A 1.506(6) . ?
C1A H1AA 0.9700 . ?
C1A H1AB 0.9700 . ?
C1A C1C 1.487(9) . ?
C1B H1BA 0.9600 . ?
C1B H1BB 0.9600 . ?
C1B H1BC 0.9600 . ?
C1C H1CA 0.9600 . ?
C1C H1CB 0.9600 . ?
C1C H1CC 0.9600 . ?
C1D H1DA 0.9600 . ?
C1D H1DB 0.9600 . ?
C1D H1DC 0.9600 . ?
C1D C1E 1.3981(11) . ?
C1E H1EA 0.9700 . ?
C1E H1EB 0.9700 . ?
C1F H1FA 0.9700 . ?
C1F H1FB 0.9700 . ?
C1F H1FC 0.9700 . ?
C1F H1FD 0.9700 . ?
C1F C1G 1.531(8) . ?
C1F C1H 1.377(13) . ?
C1F C1I 1.216(15) . ?
C1G H1GA 0.9700 . ?
C1G H1GB 0.9700 . ?
C1H H1HA 0.9600 . ?
C1H H1HB 0.9600 . ?
C1H H1HC 0.9600 . ?
C1I H1IA 0.9600 . ?
C1I H1IB 0.9600 . ?
C1I H1IC 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
V2 V1 V3 66.45(2) 3_655 3_655 ?
O1 V1 V2 81.73(6) . 3_655 ?
O1 V1 V3 125.20(7) . 3_655 ?
O1 V1 O5 77.94(6) . . ?
O1 V1 O6 82.76(9) . . ?
O2 V1 V2 34.24(7) . 3_655 ?
O2 V1 V3 88.05(8) . 3_655 ?
O2 V1 O1 89.06(10) . . ?
O2 V1 O4 93.78(11) . . ?
O2 V1 O5 81.93(8) . . ?
O2 V1 O6 158.57(10) . . ?
O4 V1 V2 88.43(7) . 3_655 ?
O4 V1 V3 33.41(7) . 3_655 ?
O4 V1 O1 158.04(10) . . ?
O4 V1 O5 80.91(7) . . ?
O4 V1 O6 86.82(10) . . ?
O5 V1 V2 47.703(15) . 3_655 ?
O5 V1 V3 47.50(2) . 3_655 ?
O6 V1 V2 124.52(7) . 3_655 ?
O6 V1 V3 80.69(6) . 3_655 ?
O6 V1 O5 77.00(6) . . ?
O8 V1 V2 138.11(9) . 3_655 ?
O8 V1 V3 136.93(9) . 3_655 ?
O8 V1 O1 96.57(11) . . ?
O8 V1 O2 104.20(12) . . ?
O8 V1 O4 103.79(12) . . ?
O8 V1 O5 171.83(9) . . ?
O8 V1 O6 96.42(11) . . ?
V3 V2 V1 66.04(2) 3_655 3_655 ?
O2 V2 V1 33.66(7) 3_655 3_655 ?
O2 V2 V3 88.60(7) 3_655 3_655 ?
O2 V2 O5 81.03(7) 3_655 . ?
O2 V2 O6 157.42(10) 3_655 . ?
O2 V2 O3 87.03(10) 3_655 . ?
O5 V2 V1 47.382(19) . 3_655 ?
O5 V2 V3 47.58(2) . 3_655 ?
O6 V2 V1 124.40(6) . 3_655 ?
O6 V2 V3 81.22(6) . 3_655 ?
O6 V2 O5 77.22(6) . . ?
O6 V2 O3 82.25(9) . . ?
O7 V2 V1 87.80(8) 3_655 3_655 ?
O7 V2 V3 34.45(7) 3_655 3_655 ?
O7 V2 O2 94.02(11) 3_655 3_655 ?
O7 V2 O5 82.03(8) 3_655 . ?
O7 V2 O6 88.92(10) 3_655 . ?
O7 V2 O3 158.46(10) 3_655 . ?
O3 V2 V1 81.19(6) . 3_655 ?
O3 V2 V3 124.25(7) . 3_655 ?
O3 V2 O5 76.88(6) . . ?
O10 V2 V1 137.06(10) . 3_655 ?
O10 V2 V3 138.92(10) . 3_655 ?
O10 V2 O2 103.67(12) . 3_655 ?
O10 V2 O5 171.21(9) . . ?
O10 V2 O6 97.16(11) . . ?
O10 V2 O7 104.81(12) . 3_655 ?
O10 V2 O3 95.79(11) . . ?
V2 V3 V1 66.25(3) 3_655 3_655 ?
O1 V3 V1 124.24(7) . 3_655 ?
O1 V3 V2 81.30(6) . 3_655 ?
O1 V3 O5 77.13(6) . . ?
O4 V3 V1 34.47(7) 3_655 3_655 ?
O4 V3 V2 88.29(7) 3_655 3_655 ?
O4 V3 O1 158.34(10) 3_655 . ?
O4 V3 O5 81.80(7) 3_655 . ?
O4 V3 O7 94.74(11) 3_655 . ?
O4 V3 O3 88.50(10) 3_655 . ?
O5 V3 V1 47.34(2) . 3_655 ?
O5 V3 V2 47.74(2) . 3_655 ?
O7 V3 V1 88.78(8) . 3_655 ?
O7 V3 V2 33.44(7) . 3_655 ?
O7 V3 O1 87.01(10) . . ?
O7 V3 O5 81.17(7) . . ?
O7 V3 O3 157.79(10) . . ?
O3 V3 V1 81.49(7) . 3_655 ?
O3 V3 V2 125.06(7) . 3_655 ?
O3 V3 O1 82.16(9) . . ?
O3 V3 O5 77.54(6) . . ?
O9 V3 V1 138.86(10) . 3_655 ?
O9 V3 V2 136.27(10) . 3_655 ?
O9 V3 O1 95.95(11) . . ?
O9 V3 O4 104.62(12) . 3_655 ?
O9 V3 O5 171.80(9) . . ?
O9 V3 O7 103.06(12) . . ?
O9 V3 O3 97.33(12) . . ?
V1 O1 V3 109.49(10) . . ?
C11 O1 V1 118.78(19) . . ?
C11 O1 V3 118.85(19) . . ?
V1 O2 V2 112.10(12) . 3_655 ?
V3 O4 V1 112.11(12) 3_655 . ?
V1 O5 V1 180.0 3_655 . ?
V1 O5 V2 95.09(2) . . ?
V1 O5 V2 84.91(2) 3_655 . ?
V1 O5 V2 84.91(2) . 3_655 ?
V1 O5 V2 95.09(2) 3_655 3_655 ?
V1 O5 V3 94.83(2) . . ?
V1 O5 V3 94.83(2) 3_655 3_655 ?
V1 O5 V3 85.17(2) . 3_655 ?
V1 O5 V3 85.17(2) 3_655 . ?
V2 O5 V2 180.0 3_655 . ?
V3 O5 V2 95.33(3) . . ?
V3 O5 V2 84.67(3) . 3_655 ?
V3 O5 V2 84.67(3) 3_655 . ?
V3 O5 V2 95.33(3) 3_655 3_655 ?
V3 O5 V3 180.0 . 3_655 ?
V2 O6 V1 110.18(10) . . ?
C8 O6 V1 118.37(19) . . ?
C8 O6 V2 118.77(19) . . ?
V2 O7 V3 112.11(12) 3_655 . ?
O6 C8 H8A 109.3 . . ?
O6 C8 H8B 109.3 . . ?
O6 C8 C14 111.8(2) . . ?
H8A C8 H8B 107.9 . . ?
C14 C8 H8A 109.3 . . ?
C14 C8 H8B 109.3 . . ?
O1 C11 H11A 109.3 . . ?
O1 C11 H11B 109.3 . . ?
O1 C11 C14 111.6(3) . . ?
H11A C11 H11B 108.0 . . ?
C14 C11 H11A 109.3 . . ?
C14 C11 H11B 109.3 . . ?
O11 C12 C14 112.3(3) . . ?
O12 C12 C14 122.3(3) . . ?
O12 C12 O11 125.3(3) . . ?
C8 C14 C11 110.9(3) . . ?
C8 C14 C12 107.7(3) . . ?
C8 C14 C9 111.0(3) . . ?
C11 C14 C12 109.7(3) . . ?
C11 C14 C9 109.6(3) . . ?
C12 C14 C9 107.9(3) . . ?
V3 O3 V2 109.66(10) . . ?
C9 O3 V2 118.91(19) . . ?
C9 O3 V3 118.69(19) . . ?
C12 O11 C1 116.7(3) . . ?
C14 C9 H9A 109.3 . . ?
C14 C9 H9B 109.3 . . ?
O3 C9 C14 111.5(2) . . ?
O3 C9 H9A 109.3 . . ?
O3 C9 H9B 109.3 . . ?
H9A C9 H9B 108.0 . . ?
C17 O13 C7 112.3(3) . . ?
C2 O14 C20 111.4(4) . . ?
C15 O15 C1B 112.4(4) . . ?
O13 C7 H7A 109.9 . . ?
O13 C7 H7B 109.9 . . ?
O13 C7 C1 109.1(3) . . ?
H7A C7 H7B 108.3 . . ?
C1 C7 H7A 109.9 . . ?
C1 C7 H7B 109.9 . . ?
O11 C1 C7 108.7(3) . . ?
O11 C1 H1A 110.0 . . ?
O11 C1 H1B 110.0 . . ?
C7 C1 H1A 110.0 . . ?
C7 C1 H1B 110.0 . . ?
H1A C1 H1B 108.3 . . ?
O14 C2 H2A 109.7 . . ?
O14 C2 H2B 109.7 . . ?
O14 C2 C15 109.9(4) . . ?
H2A C2 H2B 108.2 . . ?
C15 C2 H2A 109.7 . . ?
C15 C2 H2B 109.7 . . ?
O15 C15 C2 108.6(4) . . ?
O15 C15 H15A 110.0 . . ?
O15 C15 H15B 110.0 . . ?
C2 C15 H15A 110.0 . . ?
C2 C15 H15B 110.0 . . ?
H15A C15 H15B 108.3 . . ?
O13 C17 H17A 109.3 . . ?
O13 C17 H17B 109.3 . . ?
O13 C17 C20 111.6(4) . . ?
H17A C17 H17B 108.0 . . ?
C20 C17 H17A 109.3 . . ?
C20 C17 H17B 109.3 . . ?
O14 C20 C17 109.2(4) . . ?
O14 C20 H20A 109.8 . . ?
O14 C20 H20B 109.8 . . ?
C17 C20 H20A 109.8 . . ?
C17 C20 H20B 109.8 . . ?
H20A C20 H20B 108.3 . . ?
C3 N1 C4 107.5(3) . . ?
C3 N1 C6 110.0(3) . . ?
C3 N1 C13 110.8(3) . . ?
C4 N1 C6 110.7(3) . . ?
C13 N1 C4 110.2(3) . . ?
C13 N1 C6 107.8(3) . . ?
N1 C3 H3A 108.6 . . ?
N1 C3 H3B 108.6 . . ?
N1 C3 C5 114.7(4) . . ?
H3A C3 H3B 107.6 . . ?
C5 C3 H3A 108.6 . . ?
C5 C3 H3B 108.6 . . ?
N1 C4 H4A 108.6 . . ?
N1 C4 H4B 108.6 . . ?
N1 C4 C16 114.7(3) . . ?
H4A C4 H4B 107.6 . . ?
C16 C4 H4A 108.6 . . ?
C16 C4 H4B 108.6 . . ?
C3 C5 H5A 108.1 . . ?
C3 C5 H5B 108.1 . . ?
H5A C5 H5B 107.3 . . ?
C1E C5 C3 116.8(5) . . ?
C1E C5 H5A 108.1 . . ?
C1E C5 H5B 108.1 . . ?
N1 C6 H6A 108.5 . . ?
N1 C6 H6B 108.5 . . ?
H6A C6 H6B 107.5 . . ?
C1G C6 N1 115.0(4) . . ?
C1G C6 H6A 108.5 . . ?
C1G C6 H6B 108.5 . . ?
H10A C10 H10B 108.0 . . ?
C16 C10 H10A 109.3 . . ?
C16 C10 H10B 109.3 . . ?
C16 C10 C18 111.6(4) . . ?
C18 C10 H10A 109.3 . . ?
C18 C10 H10B 109.3 . . ?
N1 C13 H13A 108.7 . . ?
N1 C13 H13B 108.7 . . ?
N1 C13 C19 114.3(4) . . ?
H13A C13 H13B 107.6 . . ?
C19 C13 H13A 108.7 . . ?
C19 C13 H13B 108.7 . . ?
C4 C16 H16A 109.7 . . ?
C4 C16 H16B 109.7 . . ?
C10 C16 C4 110.0(4) . . ?
C10 C16 H16A 109.7 . . ?
C10 C16 H16B 109.7 . . ?
H16A C16 H16B 108.2 . . ?
C10 C18 H18A 109.5 . . ?
C10 C18 H18B 109.5 . . ?
C10 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C13 C19 H19A 109.2 . . ?
C13 C19 H19B 109.2 . . ?
H19A C19 H19B 107.9 . . ?
C1A C19 C13 111.9(4) . . ?
C1A C19 H19A 109.2 . . ?
C1A C19 H19B 109.2 . . ?
C19 C1A H1AA 109.2 . . ?
C19 C1A H1AB 109.2 . . ?
H1AA C1A H1AB 107.9 . . ?
C1C C1A C19 112.3(5) . . ?
C1C C1A H1AA 109.2 . . ?
C1C C1A H1AB 109.2 . . ?
O15 C1B H1BA 109.5 . . ?
O15 C1B H1BB 109.5 . . ?
O15 C1B H1BC 109.5 . . ?
H1BA C1B H1BB 109.5 . . ?
H1BA C1B H1BC 109.5 . . ?
H1BB C1B H1BC 109.5 . . ?
C1A C1C H1CA 109.5 . . ?
C1A C1C H1CB 109.5 . . ?
C1A C1C H1CC 109.5 . . ?
H1CA C1C H1CB 109.5 . . ?
H1CA C1C H1CC 109.5 . . ?
H1CB C1C H1CC 109.5 . . ?
H1DA C1D H1DB 109.5 . . ?
H1DA C1D H1DC 109.5 . . ?
H1DB C1D H1DC 109.5 . . ?
C1E C1D H1DA 109.5 . . ?
C1E C1D H1DB 109.5 . . ?
C1E C1D H1DC 109.5 . . ?
C5 C1E H1EA 105.6 . . ?
C5 C1E H1EB 105.6 . . ?
C1D C1E C5 126.8(7) . . ?
C1D C1E H1EA 105.6 . . ?
C1D C1E H1EB 105.6 . . ?
H1EA C1E H1EB 106.1 . . ?
H1FA C1F H1FB 106.5 . . ?
H1FC C1F H1FD 108.2 . . ?
C1G C1F H1FA 106.6 . . ?
C1G C1F H1FB 106.6 . . ?
C1G C1F H1FC 109.8 . . ?
C1G C1F H1FD 109.8 . . ?
C1H C1F H1FC 109.8 . . ?
C1H C1F H1FD 109.8 . . ?
C1H C1F C1G 109.5(8) . . ?
C1I C1F H1FA 106.6 . . ?
C1I C1F H1FB 106.6 . . ?
C1I C1F C1G 123.1(10) . . ?
C6 C1G C1F 109.3(6) . . ?
C6 C1G H1GA 109.8 . . ?
C6 C1G H1GB 109.8 . . ?
C1F C1G H1GA 109.8 . . ?
C1F C1G H1GB 109.8 . . ?
H1GA C1G H1GB 108.3 . . ?
C1F C1H H1HA 109.5 . . ?
C1F C1H H1HB 109.5 . . ?
C1F C1H H1HC 109.5 . . ?
H1HA C1H H1HB 109.5 . . ?
H1HA C1H H1HC 109.5 . . ?
H1HB C1H H1HC 109.5 . . ?
C1F C1I H1IA 109.5 . . ?
C1F C1I H1IB 109.5 . . ?
C1F C1I H1IC 109.5 . . ?
H1IA C1I H1IB 109.5 . . ?
H1IA C1I H1IC 109.5 . . ?
H1IB C1I H1IC 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 V3 O7 V2 -45.66(12) 3_655 . . 3_655 ?
V1 O1 C11 C14 -68.8(3) . . . . ?
V1 O6 C8 C14 68.1(3) . . . . ?
V2 V1 O4 V3 -46.83(11) 3_655 . . 3_655 ?
V2 O6 C8 C14 -69.9(3) . . . . ?
V2 O3 C9 C14 67.3(3) . . . . ?
V3 V1 O2 V2 48.66(11) 3_655 . . 3_655 ?
V3 O1 C11 C14 68.7(3) . . . . ?
V3 O3 C9 C14 -70.5(3) . . . . ?
O1 V1 O2 V2 -76.61(13) . . . 3_655 ?
O1 V1 O4 V3 16.2(3) . . . 3_655 ?
O1 V3 O7 V2 78.71(13) . . . 3_655 ?
O1 C11 C14 C8 61.0(3) . . . . ?
O1 C11 C14 C12 179.8(2) . . . . ?
O1 C11 C14 C9 -62.0(3) . . . . ?
O2 V1 O4 V3 -80.67(14) . . . 3_655 ?
O4 V1 O2 V2 81.60(13) . . . 3_655 ?
O4 V3 O7 V2 -79.65(14) 3_655 . . 3_655 ?
O5 V1 O2 V2 1.35(10) . . . 3_655 ?
O5 V1 O4 V3 0.53(10) . . . 3_655 ?
O5 V3 O7 V2 1.29(11) . . . 3_655 ?
O6 V1 O2 V2 -9.3(3) . . . 3_655 ?
O6 V1 O4 V3 77.87(13) . . . 3_655 ?
O6 C8 C14 C11 -61.1(3) . . . . ?
O6 C8 C14 C12 178.9(3) . . . . ?
O6 C8 C14 C9 61.0(3) . . . . ?
O8 V1 O2 V2 -173.14(13) . . . 3_655 ?
O8 V1 O4 V3 173.70(13) . . . 3_655 ?
C8 C14 C9 O3 -60.0(3) . . . . ?
C11 C14 C9 O3 62.9(3) . . . . ?
C12 C14 C9 O3 -177.8(3) . . . . ?
C12 O11 C1 C7 143.4(4) . . . . ?
C14 C12 O11 C1 177.3(3) . . . . ?
O3 V3 O7 V2 18.0(3) . . . 3_655 ?
O9 V3 O7 V2 174.14(14) . . . 3_655 ?
O11 C12 C14 C8 162.7(3) . . . . ?
O11 C12 C14 C11 41.9(4) . . . . ?
O11 C12 C14 C9 -77.4(4) . . . . ?
O12 C12 C14 C8 -20.0(4) . . . . ?
O12 C12 C14 C11 -140.7(3) . . . . ?
O12 C12 C14 C9 99.9(4) . . . . ?
O12 C12 O11 C1 0.0(6) . . . . ?
O13 C7 C1 O11 -72.7(4) . . . . ?
O13 C17 C20 O14 -74.2(5) . . . . ?
O14 C2 C15 O15 76.7(5) . . . . ?
C7 O13 C17 C20 175.1(4) . . . . ?
C2 O14 C20 C17 -159.0(4) . . . . ?
C17 O13 C7 C1 162.9(3) . . . . ?
C20 O14 C2 C15 -177.6(4) . . . . ?
N1 C3 C5 C1E -158.5(6) . . . . ?
N1 C4 C16 C10 -174.2(3) . . . . ?
N1 C6 C1G C1F 177.5(4) . . . . ?
N1 C13 C19 C1A 176.9(4) . . . . ?
C3 N1 C4 C16 -175.5(3) . . . . ?
C3 N1 C6 C1G -58.9(5) . . . . ?
C3 N1 C13 C19 54.9(4) . . . . ?
C3 C5 C1E C1D -32.1(13) . . . . ?
C4 N1 C3 C5 -179.4(4) . . . . ?
C4 N1 C6 C1G 59.7(5) . . . . ?
C4 N1 C13 C19 -63.9(5) . . . . ?
C6 N1 C3 C5 -58.9(5) . . . . ?
C6 N1 C4 C16 64.4(4) . . . . ?
C6 N1 C13 C19 175.2(4) . . . . ?
C13 N1 C3 C5 60.1(5) . . . . ?
C13 N1 C4 C16 -54.7(5) . . . . ?
C13 N1 C6 C1G -179.7(4) . . . . ?
C13 C19 C1A C1C 175.0(5) . . . . ?
C18 C10 C16 C4 179.4(4) . . . . ?
C1B O15 C15 C2 169.3(4) . . . . ?
C1H C1F C1G C6 -93.5(10) . . . . ?
C1I C1F C1G C6 -173.8(10) . . . . ?

_shelx_SHELXL_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_exp_sanfuyichun
_database_code_depnum_ccdc_archive 'CCDC 1503811'
_audit_update_record             
;
2016-09-10 deposited with the CCDC.
2017-02-17 downloaded from the CCDC.
;
_audit_creation_date             2016-08-19
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '2(C7 H8 F3 O11.5 V3), 2(C16 H36 N)'
_chemical_formula_sum            'C46 H88 F6 N2 O23 V6'
_chemical_formula_weight         1456.82
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 '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      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'
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                   22.5215(4)
_cell_length_b                   15.8480(2)
_cell_length_c                   18.2434(3)
_cell_angle_alpha                90
_cell_angle_beta                 102.9704(17)
_cell_angle_gamma                90
_cell_volume                     6345.29(19)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    11294
_cell_measurement_temperature    105.5
_cell_measurement_theta_max      29.1806
_cell_measurement_theta_min      3.0412
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.938
_exptl_absorpt_correction_T_max  0.829
_exptl_absorpt_correction_T_min  0.727
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.525
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             3016
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.20
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0321
_diffrn_reflns_av_unetI/netI     0.0365
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            39135
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_min         3.047
_diffrn_ambient_temperature      105.5
_diffrn_detector_area_resol_mean 16.0971
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega    9.00   35.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.0609   77.0000 -120.0000 26

#__ type_ start__ end____ width___ exp.time_
  2 omega  -46.00  -11.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.0609   77.0000   90.0000 35

#__ type_ start__ end____ width___ exp.time_
  3 omega  -86.00   12.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.0609  -77.0000  -90.0000 98

#__ type_ start__ end____ width___ exp.time_
  4 omega   10.00   36.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       21.1390  -53.0000  -65.0000 26

#__ type_ start__ end____ width___ exp.time_
  5 omega   20.00   46.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       21.1390  -37.0000  -60.0000 26

#__ type_ start__ end____ width___ exp.time_
  6 omega  -38.00   18.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       21.1390  -37.0000   30.0000 56

#__ type_ start__ end____ width___ exp.time_
  7 omega   -5.00   82.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       21.1390   37.0000 -150.0000 87
;
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      -0.0034430000
_diffrn_orient_matrix_UB_12      -0.0286628000
_diffrn_orient_matrix_UB_13      0.0286251000
_diffrn_orient_matrix_UB_21      0.0321217000
_diffrn_orient_matrix_UB_22      -0.0033836000
_diffrn_orient_matrix_UB_23      0.0118683000
_diffrn_orient_matrix_UB_31      0.0002784000
_diffrn_orient_matrix_UB_32      0.0342248000
_diffrn_orient_matrix_UB_33      0.0251405000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                10379
_reflns_number_total             12449
_reflns_odcompleteness_completeness 99.72
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_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    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         1.656
_refine_diff_density_min         -1.587
_refine_diff_density_rms         0.076
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     835
_refine_ls_number_reflns         12449
_refine_ls_number_restraints     22
_refine_ls_R_factor_all          0.0549
_refine_ls_R_factor_gt           0.0433
_refine_ls_restrained_S_all      1.033
_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)+(0.0375P)²+12.8423P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1002
_refine_ls_wR_factor_ref         0.1071
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid bond restraints
 C7, C12, C13
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C11, C10
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
C7 \\sim C12 \\sim C13: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02
C11 \\sim C10: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
Uanis(C19) = Uanis(C1A)
Uanis(C15) = Uanis(C8) = Uanis(C1D)
Uanis(C1C) = Uanis(C1E)
Uanis(N) = Uanis(C1) = Uanis(C10)
Uanis(C42) = Uanis(O25) = Uanis(O55)
4. Others
 Sof(C1)=Sof(H1A)=Sof(H1B)=Sof(C7)=Sof(H7A)=Sof(H7B)=Sof(C12)=Sof(H12A)=
 Sof(H12B)=Sof(C13)=Sof(H13A)=Sof(H13B)=Sof(H13C)=1-FVAR(1)
 Sof(C0AA)=Sof(H0AA)=Sof(H0AB)=Sof(C1AA)=Sof(H1AA)=Sof(H1AB)=Sof(H1AC)=
 Sof(C11)=Sof(H11A)=Sof(H11B)=Sof(C10)=Sof(H10A)=Sof(H10B)=FVAR(1)
 Sof(C16)=Sof(H16A)=Sof(H16B)=Sof(C17)=Sof(H17A)=Sof(H17B)=Sof(C19)=Sof(H19A)=
 Sof(H19B)=Sof(C1A)=Sof(H1AD)=Sof(H1AE)=Sof(H1AF)=1-FVAR(2)
 Sof(C2)=Sof(H2A)=Sof(H2B)=Sof(C9)=Sof(H9A)=Sof(H9B)=Sof(C18)=Sof(H18A)=
 Sof(H18B)=Sof(H18C)=Sof(C1B)=Sof(H1BA)=Sof(H1BB)=FVAR(2)
 Sof(H3BC)=Sof(H3BD)=Sof(C1C)=Sof(H1CA)=Sof(H1CB)=Sof(H1CC)=Sof(C1E)=Sof(H1EA)=
 Sof(H1EB)=1-FVAR(3)
 Sof(H3AA)=Sof(H3AB)=Sof(C4)=Sof(H4A)=Sof(H4B)=Sof(H4C)=Sof(C5)=Sof(H5A)=
 Sof(H5B)=FVAR(3)
 Sof(H65C)=Sof(H65D)=Sof(C8)=Sof(H8A)=Sof(H8B)=Sof(C15)=Sof(H15A)=Sof(H15B)=
 Sof(C1D)=Sof(H1DA)=Sof(H1DB)=Sof(H1DC)=1-FVAR(4)
 Sof(H65A)=Sof(H65B)=Sof(C77)=Sof(H77A)=Sof(H77B)=Sof(C6)=Sof(H6A)=Sof(H6B)=
 Sof(H6C)=Sof(C14)=Sof(H14A)=Sof(H14B)=FVAR(4)
5.a Secondary CH2 refined with riding coordinates:
 C26(H26A,H26B), C35(H35A,H35B), C38(H38A,H38B), C41(H41A,H41B), C43(H43A,
 H43B), C50(H50A,H50B), C56(H56A,H56B), C61(H61A,H61B), C65(H65A,H65B),
 C65(H65C,H65D), C77(H77A,H77B), C28(H28A,H28B), C30(H30A,H30B), C32(H32A,H32B),
  C33(H33A,H33B), C34(H34A,H34B), C39(H39A,H39B), C40(H40A,H40B), C44(H44A,
 H44B), C46(H46A,H46B), C52(H52A,H52B), C53(H53A,H53B), C57(H57A,H57B), C1(H1A,
 H1B), C3(H3AA,H3AB), C3(H3BC,H3BD), C5(H5A,H5B), C7(H7A,H7B), C0AA(H0AA,H0AB),
 C11(H11A,H11B), C12(H12A,H12B), C10(H10A,H10B), C21(H21A,H21B), C2(H2A,H2B),
 C9(H9A,H9B), C14(H14A,H14B), C16(H16A,H16B), C17(H17A,H17B), C19(H19A,H19B),
 C1B(H1BA,H1BB), C8(H8A,H8B), C15(H15A,H15B), C1E(H1EA,H1EB)
5.b Me refined with riding coordinates:
 C1A(H1AD,H1AE,H1AF)
5.c Idealised Me refined as rotating group:
 C45(H45A,H45B,H45C), C59(H59A,H59B,H59C), C64(H64A,H64B,H64C), C67(H67A,H67B,
 H67C), C4(H4A,H4B,H4C), C1AA(H1AA,H1AB,H1AC), C13(H13A,H13B,H13C), C6(H6A,H6B,
 H6C), C1C(H1CA,H1CB,H1CC), C18(H18A,H18B,H18C), C1D(H1DA,H1DB,H1DC)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_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 0.48278(2) 0.36337(3) 0.47039(3) 0.01505(11) Uani 1 1 d . . . . .
V2 V 0.03974(2) 0.37075(3) 0.50219(3) 0.01725(11) Uani 1 1 d . . . . .
V3 V 0.08846(2) 0.56813(3) 0.50237(3) 0.01848(11) Uani 1 1 d . . . . .
V4 V 0.44498(2) 0.50080(3) 0.58797(2) 0.01529(11) Uani 1 1 d . . . . .
V5 V 0.00802(2) 0.50723(3) 0.62390(3) 0.01725(11) Uani 1 1 d . . . . .
V6 V 0.42416(2) 0.54859(3) 0.40754(3) 0.01580(11) Uani 1 1 d . . . . .
O1 O 0.53031(8) 0.38804(12) 0.40449(10) 0.0160(4) Uani 1 1 d . . . . .
O2 O 0.54712(9) 0.35050(12) 0.55075(10) 0.0167(4) Uani 1 1 d . . . . .
O3 O 0.41279(8) 0.42155(12) 0.39844(10) 0.0150(4) Uani 1 1 d . . . . .
O4 O 0.02586(9) 0.38993(12) 0.39988(10) 0.0186(4) Uani 1 1 d . . . . .
O5 O 0.11410(9) 0.44634(12) 0.51424(11) 0.0181(4) Uani 1 1 d . . . . .
O6 O 0.38283(8) 0.53238(11) 0.49393(10) 0.0144(4) Uani 1 1 d . . . . .
O7 O 0.48346(9) 0.53802(12) 0.35384(10) 0.0166(4) Uani 1 1 d . . . . .
O8 O 0.42929(8) 0.38345(11) 0.54461(10) 0.0149(4) Uani 1 1 d . . . . .
O9 O -0.06489(9) 0.44978(12) 0.59869(11) 0.0199(4) Uani 1 1 d . . . . .
O10 O -0.03875(9) 0.33971(12) 0.49836(11) 0.0199(4) Uani 1 1 d . . . . .
O11 O 0.08896(9) 0.55518(12) 0.61355(11) 0.0182(4) Uani 1 1 d . . . . .
O12 O 0.36457(9) 0.57355(12) 0.34507(11) 0.0204(4) Uani 1 1 d . . . . .
O13 O 0.45988(9) 0.26845(12) 0.44935(11) 0.0196(4) Uani 1 1 d . . . . .
O14 O 0.04934(9) 0.39597(12) 0.61189(10) 0.0184(4) Uani 1 1 d . . . . .
O15 O 0.07751(10) 0.28450(12) 0.51315(11) 0.0227(4) Uani 1 1 d . . . . .
O16 O 0.22308(9) 0.41420(14) 0.40445(12) 0.0262(5) Uani 1 1 d . . . . .
O17 O 0.0000 0.5000 0.5000 0.0152(5) Uani 1 2 d S T P . .
O18 O 0.15551(10) 0.60757(13) 0.51427(12) 0.0253(5) Uani 1 1 d . . . . .
O19 O 0.5000 0.5000 0.5000 0.0129(5) Uani 1 2 d S T P . .
O21 O 0.39826(9) 0.49576(12) 0.64250(11) 0.0197(4) Uani 1 1 d . . . . .
O22 O 0.02457(10) 0.50665(12) 0.71431(11) 0.0225(4) Uani 1 1 d . . . . .
O23 O 0.25351(10) 0.28853(15) 0.45678(14) 0.0343(6) Uani 1 1 d . . . . .
F24 F 0.10255(11) 0.33152(18) 0.26260(13) 0.0622(7) Uani 1 1 d . . . . .
O25 O 0.20784(12) 0.40603(18) 0.77638(14) 0.0439(4) Uani 1 1 d . . . . .
C26 C 0.16771(14) 0.4243(2) 0.56965(16) 0.0230(6) Uani 1 1 d . . . . .
H26A H 0.2011 0.4604 0.5639 0.028 Uiso 1 1 calc R . . . .
H26B H 0.1789 0.3664 0.5618 0.028 Uiso 1 1 calc R . . . .
C27 C 0.32808(13) 0.39957(18) 0.46125(15) 0.0175(6) Uani 1 1 d . . . . .
F29 F 0.16247(12) 0.43369(16) 0.25269(13) 0.0580(7) Uani 1 1 d . . . . .
C31 C 0.26485(13) 0.35871(19) 0.44305(16) 0.0197(6) Uani 1 1 d . . . . .
C35 C 0.36833(12) 0.35161(18) 0.52757(15) 0.0167(6) Uani 1 1 d . . . . .
H35A H 0.3511 0.3571 0.5715 0.020 Uiso 1 1 calc R . . . .
H35B H 0.3689 0.2922 0.5151 0.020 Uiso 1 1 calc R . . . .
C36 C 0.15743(14) 0.43386(19) 0.64982(16) 0.0236(6) Uani 1 1 d . . . . .
F37 F 0.19879(11) 0.30996(16) 0.28046(13) 0.0581(7) Uani 1 1 d . . . . .
C38 C 0.32437(12) 0.49364(17) 0.47978(16) 0.0176(6) Uani 1 1 d . . . . .
H38A H 0.2975 0.5219 0.4380 0.021 Uiso 1 1 calc R . . . .
H38B H 0.3072 0.4998 0.5237 0.021 Uiso 1 1 calc R . . . .
C41 C 0.14315(14) 0.52688(19) 0.66430(16) 0.0226(6) Uani 1 1 d . . . . .
H41A H 0.1383 0.5328 0.7156 0.027 Uiso 1 1 calc R . . . .
H41B H 0.1771 0.5620 0.6587 0.027 Uiso 1 1 calc R . . . .
C42 C 0.21754(18) 0.4082(3) 0.7055(2) 0.0439(4) Uani 1 1 d . . . . .
C43 C 0.35297(13) 0.38840(18) 0.38935(15) 0.0183(6) Uani 1 1 d . . . . .
H43A H 0.3534 0.3289 0.3771 0.022 Uiso 1 1 calc R . . . .
H43B H 0.3261 0.4168 0.3477 0.022 Uiso 1 1 calc R . . . .
N N 0.51724(14) 0.17300(17) 0.69324(14) 0.0304(6) Uani 1 1 d . . . . .
F48 F 0.30574(14) 0.51297(19) 0.83065(17) 0.0761(8) Uani 1 1 d . . . . .
C50 C 0.10575(14) 0.37609(19) 0.66245(16) 0.0228(6) Uani 1 1 d . . . . .
H50A H 0.1162 0.3178 0.6553 0.027 Uiso 1 1 calc R . . . .
H50B H 0.1013 0.3823 0.7138 0.027 Uiso 1 1 calc R . . . .
F51 F 0.33719(13) 0.4337(2) 0.92816(15) 0.0862(10) Uani 1 1 d . . . . .
F54 F 0.25081(14) 0.4971(2) 0.91099(17) 0.0788(9) Uani 1 1 d . . . . .
O55 O 0.26123(12) 0.38664(18) 0.68824(14) 0.0439(4) Uani 1 1 d . . . . .
C56 C 0.16242(14) 0.3826(2) 0.37414(19) 0.0304(7) Uani 1 1 d . . . . .
H56A H 0.1324 0.4243 0.3804 0.036 Uiso 1 1 calc R . . . .
H56B H 0.1555 0.3317 0.4005 0.036 Uiso 1 1 calc R . . . .
C58 C 0.15650(16) 0.3642(2) 0.2929(2) 0.0366(8) Uani 1 1 d . . . . .
C61 C 0.25912(18) 0.3803(3) 0.8342(2) 0.0437(9) Uani 1 1 d . . . . .
H61A H 0.2886 0.3511 0.8119 0.052 Uiso 1 1 calc R . . . .
H61B H 0.2458 0.3418 0.8686 0.052 Uiso 1 1 calc R . . . .
C63 C 0.2879(2) 0.4561(3) 0.8759(2) 0.0517(11) Uani 1 1 d . . . . .
C65 C 0.57690(17) 0.1556(2) 0.74764(18) 0.0351(8) Uani 1 1 d . . . . .
H65A H 0.5861 0.0963 0.7433 0.042 Uiso 0.774(8) 1 calc R . . A 1
H65B H 0.5705 0.1641 0.7980 0.042 Uiso 0.774(8) 1 calc R . . A 1
H65C H 0.5997 0.1110 0.7300 0.042 Uiso 0.226(8) 1 calc R . . A 2
H65D H 0.5713 0.1419 0.7975 0.042 Uiso 0.226(8) 1 calc R . . A 2
C77 C 0.6335(3) 0.2056(6) 0.7417(3) 0.066(2) Uani 0.774(8) 1 d . . . A 1
H77A H 0.6254 0.2650 0.7476 0.079 Uiso 0.774(8) 1 calc R . . A 1
H77B H 0.6403 0.1980 0.6914 0.079 Uiso 0.774(8) 1 calc R . . A 1
N0AA N 0.08065(11) 0.70548(15) 0.22662(13) 0.0202(5) Uani 1 1 d . . . . .
C28 C 0.05873(14) 0.78744(18) 0.25577(16) 0.0208(6) Uani 1 1 d . . . . .
H28A H 0.0928 0.8263 0.2673 0.025 Uiso 1 1 calc R . . . .
H28B H 0.0281 0.8123 0.2157 0.025 Uiso 1 1 calc R . . . .
C30 C 0.10643(14) 0.72824(18) 0.15896(16) 0.0218(6) Uani 1 1 d . . . . .
H30A H 0.1415 0.7645 0.1758 0.026 Uiso 1 1 calc R . . . .
H30B H 0.0760 0.7605 0.1240 0.026 Uiso 1 1 calc R . . . .
C32 C 0.18123(15) 0.7193(2) 0.32639(18) 0.0293(7) Uani 1 1 d . . . . .
H32A H 0.1664 0.7601 0.3578 0.035 Uiso 1 1 calc R . . . .
H32B H 0.1971 0.7501 0.2890 0.035 Uiso 1 1 calc R . . . .
C33 C -0.06988(16) 0.5988(2) 0.12092(18) 0.0289(7) Uani 1 1 d . . . . .
H33A H -0.0498 0.5538 0.0997 0.035 Uiso 1 1 calc R . . . .
H33B H -0.0811 0.5768 0.1656 0.035 Uiso 1 1 calc R . . . .
C34 C 0.02836(14) 0.64267(18) 0.20578(18) 0.0241(7) Uani 1 1 d . . . . .
H34A H 0.0442 0.5904 0.1902 0.029 Uiso 1 1 calc R . . . .
H34B H 0.0133 0.6306 0.2505 0.029 Uiso 1 1 calc R . . . .
C39 C 0.12946(14) 0.66327(19) 0.28772(17) 0.0243(7) Uani 1 1 d . . . . .
H39A H 0.1099 0.6404 0.3256 0.029 Uiso 1 1 calc R . . . .
H39B H 0.1464 0.6162 0.2652 0.029 Uiso 1 1 calc R . . . .
C40 C -0.02494(15) 0.67115(19) 0.14377(19) 0.0285(7) Uani 1 1 d . . . . .
H40A H -0.0100 0.6898 0.1005 0.034 Uiso 1 1 calc R . . . .
H40B H -0.0454 0.7184 0.1614 0.034 Uiso 1 1 calc R . . . .
C44 C 0.02545(16) 0.86724(19) 0.35636(18) 0.0287(7) Uani 1 1 d . . . . .
H44A H 0.0026 0.9025 0.3164 0.034 Uiso 1 1 calc R . . . .
H44B H 0.0656 0.8920 0.3732 0.034 Uiso 1 1 calc R . . . .
C45 C -0.00665(17) 0.8665(2) 0.42173(19) 0.0337(8) Uani 1 1 d . . . . .
H45A H -0.0479 0.8474 0.4042 0.051 Uiso 1 1 calc GR . . . .
H45B H -0.0068 0.9225 0.4418 0.051 Uiso 1 1 calc GR . . . .
H45C H 0.0145 0.8291 0.4603 0.051 Uiso 1 1 calc GR . . . .
C46 C 0.15460(16) 0.6829(2) 0.05378(18) 0.0296(7) Uani 1 1 d . . . . .
H46A H 0.1896 0.7180 0.0745 0.035 Uiso 1 1 calc R . . . .
H46B H 0.1255 0.7168 0.0186 0.035 Uiso 1 1 calc R . . . .
C52 C 0.03202(14) 0.77931(19) 0.32519(17) 0.0237(6) Uani 1 1 d . . . . .
H52A H 0.0586 0.7452 0.3630 0.028 Uiso 1 1 calc R . . . .
H52B H -0.0075 0.7520 0.3119 0.028 Uiso 1 1 calc R . . . .
C53 C 0.23188(15) 0.6666(2) 0.37470(19) 0.0325(8) Uani 1 1 d . . . . .
H53A H 0.2148 0.6322 0.4088 0.039 Uiso 1 1 calc R . . . .
H53B H 0.2485 0.6290 0.3424 0.039 Uiso 1 1 calc R . . . .
C57 C 0.12555(17) 0.6536(2) 0.11701(18) 0.0312(8) Uani 1 1 d . . . . .
H57A H 0.1544 0.6190 0.1519 0.037 Uiso 1 1 calc R . . . .
H57B H 0.0901 0.6192 0.0963 0.037 Uiso 1 1 calc R . . . .
C59 C -0.12721(17) 0.6236(2) 0.0644(2) 0.0436(9) Uani 1 1 d . . . . .
H59A H -0.1167 0.6445 0.0196 0.065 Uiso 1 1 calc GR . . . .
H59B H -0.1481 0.6668 0.0855 0.065 Uiso 1 1 calc GR . . . .
H59C H -0.1532 0.5752 0.0523 0.065 Uiso 1 1 calc GR . . . .
C64 C 0.28278(17) 0.7200(3) 0.4199(2) 0.0452(10) Uani 1 1 d . . . . .
H64A H 0.2987 0.7560 0.3866 0.068 Uiso 1 1 calc GR . . . .
H64B H 0.3146 0.6840 0.4467 0.068 Uiso 1 1 calc GR . . . .
H64C H 0.2673 0.7539 0.4550 0.068 Uiso 1 1 calc GR . . . .
C67 C 0.1748(2) 0.6088(2) 0.0120(2) 0.0446(10) Uani 1 1 d . . . . .
H67A H 0.1929 0.6297 -0.0273 0.067 Uiso 1 1 calc GR . . . .
H67B H 0.1401 0.5745 -0.0094 0.067 Uiso 1 1 calc GR . . . .
H67C H 0.2041 0.5756 0.0465 0.067 Uiso 1 1 calc GR . . . .
C1 C 0.4710(4) 0.1189(6) 0.7120(4) 0.0304(6) Uani 0.546(11) 1 d . . . B 1
H1A H 0.4692 0.1296 0.7638 0.037 Uiso 0.546(11) 1 calc R . . B 1
H1B H 0.4836 0.0607 0.7089 0.037 Uiso 0.546(11) 1 calc R . . B 1
C3 C 0.5498(3) 0.0914(3) 0.5887(2) 0.0736(17) Uani 1 1 d . . . . .
H3AA H 0.5281 0.0435 0.6032 0.088 Uiso 0.731(10) 1 calc R . . C 1
H3AB H 0.5921 0.0870 0.6154 0.088 Uiso 0.731(10) 1 calc R . . C 1
H3BC H 0.5204 0.0456 0.5802 0.088 Uiso 0.269(10) 1 calc R . . C 2
H3BD H 0.5862 0.0739 0.6249 0.088 Uiso 0.269(10) 1 calc R . . C 2
C4 C 0.5947(3) 0.1442(4) 0.4883(3) 0.0462(18) Uani 0.731(10) 1 d . . . C 1
H4A H 0.5966 0.1377 0.4366 0.069 Uiso 0.731(10) 1 calc GR . . C 1
H4B H 0.6333 0.1296 0.5202 0.069 Uiso 0.731(10) 1 calc GR . . C 1
H4C H 0.5851 0.2018 0.4974 0.069 Uiso 0.731(10) 1 calc GR . . C 1
C5 C 0.5462(4) 0.0874(4) 0.5051(3) 0.0453(18) Uani 0.731(10) 1 d . . . C 1
H5A H 0.5527 0.0300 0.4903 0.054 Uiso 0.731(10) 1 calc R . . C 1
H5B H 0.5064 0.1058 0.4776 0.054 Uiso 0.731(10) 1 calc R . . C 1
C7 C 0.4082(5) 0.1289(9) 0.6636(6) 0.059(3) Uani 0.546(11) 1 d . U . B 1
H7A H 0.4094 0.1218 0.6111 0.070 Uiso 0.546(11) 1 calc R . . B 1
H7B H 0.3932 0.1853 0.6698 0.070 Uiso 0.546(11) 1 calc R . . B 1
C0AA C 0.3837(5) 0.0025(10) 0.6816(6) 0.061(4) Uani 0.454(11) 1 d . . . B 2
H0AA H 0.4077 -0.0472 0.6770 0.073 Uiso 0.454(11) 1 calc R . . B 2
H0AB H 0.3837 0.0096 0.7344 0.073 Uiso 0.454(11) 1 calc R . . B 2
C1AA C 0.3188(5) -0.0120(11) 0.6382(7) 0.077(5) Uani 0.454(11) 1 d . . . B 2
H1AA H 0.3180 -0.0155 0.5854 0.115 Uiso 0.454(11) 1 calc GR . . B 2
H1AB H 0.2937 0.0341 0.6470 0.115 Uiso 0.454(11) 1 calc GR . . B 2
H1AC H 0.3038 -0.0637 0.6546 0.115 Uiso 0.454(11) 1 calc GR . . B 2
C11 C 0.4141(6) 0.0802(9) 0.6545(7) 0.052(3) Uani 0.454(11) 1 d . U . B 2
H11A H 0.3905 0.1305 0.6588 0.062 Uiso 0.454(11) 1 calc R . . B 2
H11B H 0.4156 0.0732 0.6022 0.062 Uiso 0.454(11) 1 calc R . . B 2
C12 C 0.3648(6) 0.0635(10) 0.6851(5) 0.080(4) Uani 0.546(11) 1 d . U . B 1
H12A H 0.3783 0.0075 0.6748 0.096 Uiso 0.546(11) 1 calc R . . B 1
H12B H 0.3669 0.0674 0.7387 0.096 Uiso 0.546(11) 1 calc R . . B 1
C13 C 0.2994(6) 0.0752(14) 0.6429(7) 0.130(6) Uani 0.546(11) 1 d . U . B 1
H13A H 0.2966 0.0680 0.5900 0.195 Uiso 0.546(11) 1 calc GR . . B 1
H13B H 0.2860 0.1309 0.6521 0.195 Uiso 0.546(11) 1 calc GR . . B 1
H13C H 0.2741 0.0342 0.6598 0.195 Uiso 0.546(11) 1 calc GR . . B 1
C10 C 0.4793(5) 0.0896(7) 0.7034(5) 0.0304(6) Uani 0.454(11) 1 d . U . B 2
H10A H 0.5027 0.0411 0.6939 0.037 Uiso 0.454(11) 1 calc R . . B 2
H10B H 0.4767 0.0866 0.7557 0.037 Uiso 0.454(11) 1 calc R . . B 2
C21 C 0.52331(17) 0.1711(2) 0.61202(17) 0.0303(8) Uani 1 1 d . . . . .
H21A H 0.4833 0.1796 0.5796 0.036 Uiso 1 1 calc R . . . .
H21B H 0.5488 0.2180 0.6040 0.036 Uiso 1 1 calc R . . . .
C2 C 0.5047(3) 0.2666(3) 0.7087(3) 0.0266(14) Uani 0.665(9) 1 d . . . B 1
H2A H 0.5342 0.3012 0.6912 0.032 Uiso 0.665(9) 1 calc R . . B 1
H2B H 0.4647 0.2814 0.6792 0.032 Uiso 0.665(9) 1 calc R . . B 1
C6 C 0.6886(2) 0.1908(3) 0.8781(3) 0.0432(15) Uani 0.774(8) 1 d . . . A 1
H6A H 0.6803 0.2487 0.8876 0.065 Uiso 0.774(8) 1 calc GR . . A 1
H6B H 0.7261 0.1739 0.9112 0.065 Uiso 0.774(8) 1 calc GR . . A 1
H6C H 0.6560 0.1560 0.8868 0.065 Uiso 0.774(8) 1 calc GR . . A 1
C9 C 0.5074(3) 0.2884(3) 0.7913(3) 0.0356(17) Uani 0.665(9) 1 d . . . B 1
H9A H 0.5495 0.2928 0.8184 0.043 Uiso 0.665(9) 1 calc R . . B 1
H9B H 0.4882 0.2439 0.8142 0.043 Uiso 0.665(9) 1 calc R . . B 1
C14 C 0.6936(6) 0.1815(8) 0.8001(7) 0.110(5) Uani 0.774(8) 1 d . . . A 1
H14A H 0.7041 0.1235 0.7916 0.131 Uiso 0.774(8) 1 calc R . . A 1
H14B H 0.7266 0.2171 0.7917 0.131 Uiso 0.774(8) 1 calc R . . A 1
C16 C 0.4714(7) 0.2445(8) 0.6989(6) 0.031(3) Uani 0.335(9) 1 d . . . B 2
H16A H 0.4900 0.2983 0.6923 0.038 Uiso 0.335(9) 1 calc R . . B 2
H16B H 0.4357 0.2380 0.6583 0.038 Uiso 0.335(9) 1 calc R . . B 2
C17 C 0.4516(7) 0.2457(10) 0.7728(6) 0.056(4) Uani 0.335(9) 1 d . . . B 2
H17A H 0.4876 0.2468 0.8137 0.067 Uiso 0.335(9) 1 calc R . . B 2
H17B H 0.4296 0.1940 0.7773 0.067 Uiso 0.335(9) 1 calc R . . B 2
C1C C 0.6132(7) 0.0785(10) 0.4782(8) 0.044(4) Uani 0.269(10) 1 d . . . C 2
H1CA H 0.6052 0.0813 0.4243 0.065 Uiso 0.269(10) 1 calc GR . . C 2
H1CB H 0.6121 0.0207 0.4936 0.065 Uiso 0.269(10) 1 calc GR . . C 2
H1CC H 0.6528 0.1017 0.4991 0.065 Uiso 0.269(10) 1 calc GR . . C 2
C18 C 0.4048(5) 0.3605(6) 0.7791(6) 0.065(3) Uani 0.665(9) 1 d . . . B 1
H18A H 0.3912 0.3378 0.7294 0.097 Uiso 0.665(9) 1 calc GR . . B 1
H18B H 0.3855 0.4140 0.7821 0.097 Uiso 0.665(9) 1 calc GR . . B 1
H18C H 0.3942 0.3223 0.8151 0.097 Uiso 0.665(9) 1 calc GR . . B 1
C19 C 0.4114(10) 0.3206(12) 0.7809(9) 0.060(4) Uani 0.335(9) 1 d . . . B 2
H19A H 0.3791 0.3262 0.7361 0.072 Uiso 0.335(9) 1 calc R . . B 2
H19B H 0.3930 0.3120 0.8236 0.072 Uiso 0.335(9) 1 calc R . . B 2
C1A C 0.4447(10) 0.3885(13) 0.7908(9) 0.060(4) Uani 0.335(9) 1 d . . . B 2
H1AD H 0.4197 0.4362 0.7960 0.090 Uiso 0.335(9) 1 calc R . . B 2
H1AE H 0.4764 0.3827 0.8355 0.090 Uiso 0.335(9) 1 calc R . . B 2
H1AF H 0.4625 0.3968 0.7483 0.090 Uiso 0.335(9) 1 calc R . . B 2
C1B C 0.4745(4) 0.3724(5) 0.7965(4) 0.0425(18) Uani 0.665(9) 1 d . . . B 1
H1BA H 0.4850 0.4124 0.7611 0.051 Uiso 0.665(9) 1 calc R . . B 1
H1BB H 0.4881 0.3956 0.8467 0.051 Uiso 0.665(9) 1 calc R . . B 1
C8 C 0.6694(6) 0.2358(9) 0.8057(10) 0.025(3) Uani 0.226(8) 1 d . . . A 2
H8A H 0.6989 0.2762 0.7955 0.030 Uiso 0.226(8) 1 calc R . . A 2
H8B H 0.6629 0.2468 0.8556 0.030 Uiso 0.226(8) 1 calc R . . A 2
C15 C 0.6076(7) 0.2446(9) 0.7454(10) 0.025(3) Uani 0.226(8) 1 d . . . A 2
H15A H 0.5825 0.2891 0.7589 0.030 Uiso 0.226(8) 1 calc R . . A 2
H15B H 0.6148 0.2562 0.6959 0.030 Uiso 0.226(8) 1 calc R . . A 2
C1D C 0.6902(10) 0.1560(14) 0.8018(16) 0.025(3) Uani 0.226(8) 1 d . . . A 2
H1DA H 0.6563 0.1182 0.7872 0.038 Uiso 0.226(8) 1 calc GR . . A 2
H1DB H 0.7141 0.1396 0.8501 0.038 Uiso 0.226(8) 1 calc GR . . A 2
H1DC H 0.7149 0.1537 0.7652 0.038 Uiso 0.226(8) 1 calc GR . . A 2
C1E C 0.5660(9) 0.1278(15) 0.5056(10) 0.044(4) Uani 0.269(10) 1 d . . . C 2
H1EA H 0.5286 0.1273 0.4668 0.052 Uiso 0.269(10) 1 calc R . . C 2
H1EB H 0.5795 0.1859 0.5128 0.052 Uiso 0.269(10) 1 calc R . . C 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 V4 3.0320(7) 3_666 ?
V1 V6 3.0337(7) 3_666 ?
V1 O1 1.8227(19) . ?
V1 O2 1.8267(19) . ?
V1 O3 2.0320(19) . ?
V1 O8 2.0294(18) . ?
V1 O13 1.609(2) . ?
V1 O19 2.2443(5) . ?
V2 V3 3.0288(7) 3_566 ?
V2 V5 3.0128(7) 3_566 ?
V2 O4 1.8472(19) . ?
V2 O5 2.030(2) . ?
V2 O10 1.821(2) . ?
V2 O14 2.0043(19) . ?
V2 O15 1.599(2) . ?
V2 O17 2.2321(5) . ?
V3 V2 3.0289(7) 3_566 ?
V3 V5 3.0344(7) 3_566 ?
V3 O5 2.012(2) . ?
V3 O9 1.823(2) 3_566 ?
V3 O10 1.839(2) 3_566 ?
V3 O11 2.0362(19) . ?
V3 O17 2.2580(5) . ?
V3 O18 1.603(2) . ?
V4 V1 3.0319(7) 3_666 ?
V4 V6 3.0327(7) 3_666 ?
V4 O1 1.8434(19) 3_666 ?
V4 O6 2.0187(19) . ?
V4 O7 1.8262(19) 3_666 ?
V4 O8 2.0209(19) . ?
V4 O19 2.2371(4) . ?
V4 O21 1.6039(19) . ?
V5 V2 3.0128(7) 3_566 ?
V5 V3 3.0345(7) 3_566 ?
V5 O4 1.811(2) 3_566 ?
V5 O9 1.843(2) . ?
V5 O11 2.022(2) . ?
V5 O14 2.028(2) . ?
V5 O17 2.2297(5) . ?
V5 O22 1.607(2) . ?
V6 V1 3.0337(7) 3_666 ?
V6 V4 3.0328(7) 3_666 ?
V6 O2 1.8258(19) 3_666 ?
V6 O3 2.0317(19) . ?
V6 O6 2.0185(19) . ?
V6 O7 1.8327(19) . ?
V6 O12 1.6031(19) . ?
V6 O19 2.2500(5) . ?
O1 V4 1.8433(19) 3_666 ?
O2 V6 1.8258(19) 3_666 ?
O3 C43 1.421(3) . ?
O4 V5 1.811(2) 3_566 ?
O5 C26 1.433(3) . ?
O6 C38 1.423(3) . ?
O7 V4 1.8263(19) 3_666 ?
O8 C35 1.430(3) . ?
O9 V3 1.823(2) 3_566 ?
O10 V3 1.838(2) 3_566 ?
O11 C41 1.428(3) . ?
O14 C50 1.428(3) . ?
O16 C31 1.363(4) . ?
O16 C56 1.444(4) . ?
O17 V2 2.2321(5) 3_566 ?
O17 V3 2.2580(5) 3_566 ?
O17 V5 2.2297(5) 3_566 ?
O19 V1 2.2443(5) 3_666 ?
O19 V4 2.2371(4) 3_666 ?
O19 V6 2.2499(5) 3_666 ?
O23 C31 1.181(4) . ?
F24 C58 1.322(4) . ?
O25 C42 1.359(4) . ?
O25 C61 1.438(4) . ?
C26 H26A 0.9700 . ?
C26 H26B 0.9700 . ?
C26 C36 1.539(4) . ?
C27 C31 1.531(4) . ?
C27 C35 1.540(4) . ?
C27 C38 1.535(4) . ?
C27 C43 1.548(4) . ?
F29 C58 1.347(4) . ?
C35 H35A 0.9700 . ?
C35 H35B 0.9700 . ?
C36 C41 1.544(4) . ?
C36 C42 1.553(5) . ?
C36 C50 1.538(4) . ?
F37 C58 1.340(4) . ?
C38 H38A 0.9700 . ?
C38 H38B 0.9700 . ?
C41 H41A 0.9700 . ?
C41 H41B 0.9700 . ?
C42 O55 1.151(4) . ?
C43 H43A 0.9700 . ?
C43 H43B 0.9700 . ?
N C65 1.506(4) . ?
N C1 1.448(8) . ?
N C10 1.608(10) . ?
N C21 1.519(4) . ?
N C2 1.547(6) . ?
N C16 1.552(12) . ?
F48 C63 1.344(5) . ?
C50 H50A 0.9700 . ?
C50 H50B 0.9700 . ?
F51 C63 1.339(5) . ?
F54 C63 1.330(5) . ?
C56 H56A 0.9700 . ?
C56 H56B 0.9700 . ?
C56 C58 1.487(5) . ?
C61 H61A 0.9700 . ?
C61 H61B 0.9700 . ?
C61 C63 1.490(6) . ?
C65 H65A 0.9700 . ?
C65 H65B 0.9700 . ?
C65 H65C 0.9700 . ?
C65 H65D 0.9700 . ?
C65 C77 1.525(7) . ?
C65 C15 1.574(15) . ?
C77 H77A 0.9700 . ?
C77 H77B 0.9700 . ?
C77 C14 1.571(14) . ?
N0AA C28 1.527(4) . ?
N0AA C30 1.521(4) . ?
N0AA C34 1.524(4) . ?
N0AA C39 1.532(4) . ?
C28 H28A 0.9700 . ?
C28 H28B 0.9700 . ?
C28 C52 1.525(4) . ?
C30 H30A 0.9700 . ?
C30 H30B 0.9700 . ?
C30 C57 1.523(4) . ?
C32 H32A 0.9700 . ?
C32 H32B 0.9700 . ?
C32 C39 1.509(5) . ?
C32 C53 1.525(4) . ?
C33 H33A 0.9700 . ?
C33 H33B 0.9700 . ?
C33 C40 1.524(4) . ?
C33 C59 1.512(5) . ?
C34 H34A 0.9700 . ?
C34 H34B 0.9700 . ?
C34 C40 1.521(4) . ?
C39 H39A 0.9700 . ?
C39 H39B 0.9700 . ?
C40 H40A 0.9700 . ?
C40 H40B 0.9700 . ?
C44 H44A 0.9700 . ?
C44 H44B 0.9700 . ?
C44 C45 1.527(4) . ?
C44 C52 1.525(4) . ?
C45 H45A 0.9600 . ?
C45 H45B 0.9600 . ?
C45 H45C 0.9600 . ?
C46 H46A 0.9700 . ?
C46 H46B 0.9700 . ?
C46 C57 1.521(4) . ?
C46 C67 1.523(5) . ?
C52 H52A 0.9700 . ?
C52 H52B 0.9700 . ?
C53 H53A 0.9700 . ?
C53 H53B 0.9700 . ?
C53 C64 1.511(5) . ?
C57 H57A 0.9700 . ?
C57 H57B 0.9700 . ?
C59 H59A 0.9600 . ?
C59 H59B 0.9600 . ?
C59 H59C 0.9600 . ?
C64 H64A 0.9600 . ?
C64 H64B 0.9600 . ?
C64 H64C 0.9600 . ?
C67 H67A 0.9600 . ?
C67 H67B 0.9600 . ?
C67 H67C 0.9600 . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C1 C7 1.500(13) . ?
C3 H3AA 0.9700 . ?
C3 H3AB 0.9700 . ?
C3 H3BC 0.9700 . ?
C3 H3BD 0.9700 . ?
C3 C5 1.511(6) . ?
C3 C21 1.498(5) . ?
C3 C1E 1.74(2) . ?
C4 H4A 0.9600 . ?
C4 H4B 0.9600 . ?
C4 H4C 0.9600 . ?
C4 C5 1.499(10) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C7 C12 1.534(14) . ?
C0AA H0AA 0.9700 . ?
C0AA H0AB 0.9700 . ?
C0AA C1AA 1.514(14) . ?
C0AA C11 1.543(15) . ?
C1AA H1AA 0.9600 . ?
C1AA H1AB 0.9600 . ?
C1AA H1AC 0.9600 . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C11 C10 1.545(16) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C12 C13 1.513(16) . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C2 C9 1.534(7) . ?
C6 H6A 0.9600 . ?
C6 H6B 0.9600 . ?
C6 H6C 0.9600 . ?
C6 C14 1.461(12) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C9 C1B 1.537(8) . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C16 C17 1.512(15) . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C17 C19 1.52(2) . ?
C1C H1CA 0.9600 . ?
C1C H1CB 0.9600 . ?
C1C H1CC 0.9600 . ?
C1C C1E 1.49(3) . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C18 C1B 1.542(13) . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C19 C1A 1.30(3) . ?
C1A H1AD 0.9600 . ?
C1A H1AE 0.9600 . ?
C1A H1AF 0.9600 . ?
C1B H1BA 0.9700 . ?
C1B H1BB 0.9700 . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C8 C15 1.57(2) . ?
C8 C1D 1.36(3) . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C1D H1DA 0.9600 . ?
C1D H1DB 0.9600 . ?
C1D H1DC 0.9600 . ?
C1E H1EA 0.9700 . ?
C1E H1EB 0.9700 . ?

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
V4 V1 V6 66.074(15) 3_666 3_666 ?
O1 V1 V4 34.42(6) . 3_666 ?
O1 V1 V6 88.53(6) . 3_666 ?
O1 V1 O2 94.35(8) . . ?
O1 V1 O3 87.82(8) . . ?
O1 V1 O8 158.59(8) . . ?
O1 V1 O19 81.75(6) . . ?
O2 V1 V4 88.25(6) . 3_666 ?
O2 V1 V6 33.83(6) . 3_666 ?
O2 V1 O3 158.38(8) . . ?
O2 V1 O8 87.98(8) . . ?
O2 V1 O19 81.45(6) . . ?
O3 V1 V4 81.41(5) . 3_666 ?
O3 V1 V6 124.99(6) . 3_666 ?
O3 V1 O19 77.57(5) . . ?
O8 V1 V4 124.66(6) . 3_666 ?
O8 V1 V6 81.60(5) . 3_666 ?
O8 V1 O3 82.48(7) . . ?
O8 V1 O19 77.55(5) . . ?
O13 V1 V4 138.48(7) . 3_666 ?
O13 V1 V6 137.47(8) . 3_666 ?
O13 V1 O1 104.33(9) . . ?
O13 V1 O2 103.96(9) . . ?
O13 V1 O3 96.29(9) . . ?
O13 V1 O8 95.70(9) . . ?
O13 V1 O19 171.33(8) . . ?
O19 V1 V4 47.323(12) . 3_666 ?
O19 V1 V6 47.623(12) . 3_666 ?
V5 V2 V3 66.359(16) 3_566 3_566 ?
O4 V2 V3 88.60(6) . 3_566 ?
O4 V2 V5 34.15(6) . 3_566 ?
O4 V2 O5 87.75(8) . . ?
O4 V2 O14 158.75(8) . . ?
O4 V2 O17 81.64(6) . . ?
O5 V2 V3 124.91(6) . 3_566 ?
O5 V2 V5 81.28(6) . 3_566 ?
O5 V2 O17 77.19(6) . . ?
O10 V2 V3 34.33(6) . 3_566 ?
O10 V2 V5 88.10(6) . 3_566 ?
O10 V2 O4 93.61(9) . . ?
O10 V2 O5 158.99(8) . . ?
O10 V2 O14 88.77(9) . . ?
O10 V2 O17 82.26(6) . . ?
O14 V2 V3 81.50(6) . 3_566 ?
O14 V2 V5 125.06(6) . 3_566 ?
O14 V2 O5 82.69(8) . . ?
O14 V2 O17 77.75(6) . . ?
O15 V2 V3 138.94(8) . 3_566 ?
O15 V2 V5 137.14(8) . 3_566 ?
O15 V2 O4 103.40(10) . . ?
O15 V2 O5 95.05(10) . . ?
O15 V2 O10 104.98(10) . . ?
O15 V2 O14 96.34(9) . . ?
O15 V2 O17 170.70(8) . . ?
O17 V2 V3 47.943(13) . 3_566 ?
O17 V2 V5 47.493(13) . 3_566 ?
V2 V3 V5 65.745(16) 3_566 3_566 ?
O5 V3 V2 123.94(6) . 3_566 ?
O5 V3 V5 80.99(6) . 3_566 ?
O5 V3 O11 81.88(8) . . ?
O5 V3 O17 76.94(6) . . ?
O9 V3 V2 87.85(7) 3_566 3_566 ?
O9 V3 V5 34.35(6) 3_566 3_566 ?
O9 V3 O5 88.33(8) 3_566 . ?
O9 V3 O10 94.46(9) 3_566 3_566 ?
O9 V3 O11 157.99(9) 3_566 . ?
O9 V3 O17 81.41(6) 3_566 . ?
O10 V3 V2 33.96(6) 3_566 3_566 ?
O10 V3 V5 88.63(6) 3_566 3_566 ?
O10 V3 O5 157.26(9) 3_566 . ?
O10 V3 O11 87.39(8) 3_566 . ?
O10 V3 O17 81.17(6) 3_566 . ?
O11 V3 V2 81.47(6) . 3_566 ?
O11 V3 V5 124.01(6) . 3_566 ?
O11 V3 O17 77.20(6) . . ?
O17 V3 V2 47.219(13) . 3_566 ?
O17 V3 V5 47.062(13) . 3_566 ?
O18 V3 V2 137.91(8) . 3_566 ?
O18 V3 V5 138.46(8) . 3_566 ?
O18 V3 O5 96.93(10) . . ?
O18 V3 O9 104.44(10) . 3_566 ?
O18 V3 O10 104.17(10) . 3_566 ?
O18 V3 O11 96.31(10) . . ?
O18 V3 O17 171.54(8) . . ?
V1 V4 V6 66.288(16) 3_666 3_666 ?
O1 V4 V1 33.99(6) 3_666 3_666 ?
O1 V4 V6 88.25(6) 3_666 3_666 ?
O1 V4 O6 88.08(8) 3_666 . ?
O1 V4 O8 158.76(8) 3_666 . ?
O1 V4 O19 81.51(6) 3_666 . ?
O6 V4 V1 81.36(5) . 3_666 ?
O6 V4 V6 124.83(6) . 3_666 ?
O6 V4 O8 82.45(8) . . ?
O6 V4 O19 77.39(5) . . ?
O7 V4 V1 88.29(6) 3_666 3_666 ?
O7 V4 V6 34.09(6) 3_666 3_666 ?
O7 V4 O1 93.80(9) 3_666 3_666 ?
O7 V4 O6 158.53(8) 3_666 . ?
O7 V4 O8 88.37(8) 3_666 . ?
O7 V4 O19 81.74(6) 3_666 . ?
O8 V4 V1 125.20(5) . 3_666 ?
O8 V4 V6 81.75(5) . 3_666 ?
O8 V4 O19 77.89(5) . . ?
O19 V4 V1 47.524(12) . 3_666 ?
O19 V4 V6 47.656(12) . 3_666 ?
O21 V4 V1 137.01(7) . 3_666 ?
O21 V4 V6 137.66(8) . 3_666 ?
O21 V4 O1 103.31(9) . 3_666 ?
O21 V4 O6 96.51(9) . . ?
O21 V4 O7 103.82(9) . 3_666 ?
O21 V4 O8 96.64(9) . . ?
O21 V4 O19 172.21(8) . . ?
V2 V5 V3 66.479(16) 3_566 3_566 ?
O4 V5 V2 34.94(6) 3_566 3_566 ?
O4 V5 V3 88.91(6) 3_566 3_566 ?
O4 V5 O9 94.64(9) 3_566 . ?
O4 V5 O11 88.83(9) 3_566 . ?
O4 V5 O14 159.31(8) 3_566 . ?
O4 V5 O17 82.50(6) 3_566 . ?
O9 V5 V2 88.92(6) . 3_566 ?
O9 V5 V3 33.91(6) . 3_566 ?
O9 V5 O11 158.97(8) . . ?
O9 V5 O14 87.03(8) . . ?
O9 V5 O17 81.76(6) . . ?
O11 V5 V2 82.09(6) . 3_566 ?
O11 V5 V3 125.73(6) . 3_566 ?
O11 V5 O14 82.62(8) . . ?
O11 V5 O17 78.13(6) . . ?
O14 V5 V2 124.70(6) . 3_566 ?
O14 V5 V3 81.00(6) . 3_566 ?
O14 V5 O17 77.33(5) . . ?
O17 V5 V2 47.560(13) . 3_566 ?
O17 V5 V3 47.850(13) . 3_566 ?
O22 V5 V2 138.41(8) . 3_566 ?
O22 V5 V3 137.59(8) . 3_566 ?
O22 V5 O4 103.84(10) . 3_566 ?
O22 V5 O9 103.98(10) . . ?
O22 V5 O11 95.26(10) . . ?
O22 V5 O14 95.71(9) . . ?
O22 V5 O17 170.87(8) . . ?
V4 V6 V1 65.907(15) 3_666 3_666 ?
O2 V6 V1 33.85(6) 3_666 3_666 ?
O2 V6 V4 87.91(6) 3_666 3_666 ?
O2 V6 O3 158.18(8) 3_666 . ?
O2 V6 O6 88.19(8) 3_666 . ?
O2 V6 O7 94.03(9) 3_666 . ?
O2 V6 O19 81.31(6) 3_666 . ?
O3 V6 V1 124.71(6) . 3_666 ?
O3 V6 V4 81.39(5) . 3_666 ?
O3 V6 O19 77.44(5) . . ?
O6 V6 V1 81.32(5) . 3_666 ?
O6 V6 V4 124.17(6) . 3_666 ?
O6 V6 O3 82.30(7) . . ?
O6 V6 O19 77.09(5) . . ?
O7 V6 V1 88.18(6) . 3_666 ?
O7 V6 V4 33.95(6) . 3_666 ?
O7 V6 O3 87.67(8) . . ?
O7 V6 O6 157.63(8) . . ?
O7 V6 O19 81.24(6) . . ?
O12 V6 V1 137.61(8) . 3_666 ?
O12 V6 V4 137.42(7) . 3_666 ?
O12 V6 O2 104.00(10) . 3_666 ?
O12 V6 O3 96.68(9) . . ?
O12 V6 O6 97.31(9) . . ?
O12 V6 O7 103.69(9) . . ?
O12 V6 O19 172.29(8) . . ?
O19 V6 V1 47.465(12) . 3_666 ?
O19 V6 V4 47.296(12) . 3_666 ?
V1 O1 V4 111.59(9) . 3_666 ?
V6 O2 V1 112.32(10) 3_666 . ?
V6 O3 V1 109.37(9) . . ?
C43 O3 V1 119.04(16) . . ?
C43 O3 V6 118.35(16) . . ?
V5 O4 V2 110.91(10) 3_566 . ?
V3 O5 V2 110.15(9) . . ?
C26 O5 V2 118.47(17) . . ?
C26 O5 V3 119.03(17) . . ?
V6 O6 V4 109.99(9) . . ?
C38 O6 V4 118.94(16) . . ?
C38 O6 V6 118.91(16) . . ?
V4 O7 V6 111.97(9) 3_666 . ?
V4 O8 V1 109.13(8) . . ?
C35 O8 V1 118.97(15) . . ?
C35 O8 V4 119.00(16) . . ?
V3 O9 V5 111.73(10) 3_566 . ?
V2 O10 V3 111.72(10) . 3_566 ?
V5 O11 V3 109.11(9) . . ?
C41 O11 V3 119.35(17) . . ?
C41 O11 V5 118.57(17) . . ?
V2 O14 V5 109.38(9) . . ?
C50 O14 V2 118.82(17) . . ?
C50 O14 V5 119.03(17) . . ?
C31 O16 C56 117.3(2) . . ?
V2 O17 V2 180.00(2) . 3_566 ?
V2 O17 V3 84.837(18) . 3_566 ?
V2 O17 V3 84.839(18) 3_566 . ?
V2 O17 V3 95.162(18) . . ?
V2 O17 V3 95.162(18) 3_566 3_566 ?
V3 O17 V3 180.0 . 3_566 ?
V5 O17 V2 95.052(17) . . ?
V5 O17 V2 84.947(17) 3_566 . ?
V5 O17 V2 95.053(17) 3_566 3_566 ?
V5 O17 V2 84.948(17) . 3_566 ?
V5 O17 V3 85.089(18) . 3_566 ?
V5 O17 V3 85.087(18) 3_566 . ?
V5 O17 V3 94.913(18) . . ?
V5 O17 V3 94.912(18) 3_566 3_566 ?
V5 O17 V5 180.0 . 3_566 ?
V1 O19 V1 180.0 3_666 . ?
V1 O19 V6 84.912(17) 3_666 . ?
V1 O19 V6 95.089(17) 3_666 3_666 ?
V1 O19 V6 95.088(17) . . ?
V1 O19 V6 84.911(17) . 3_666 ?
V4 O19 V1 85.152(17) . 3_666 ?
V4 O19 V1 94.847(17) . . ?
V4 O19 V1 94.847(17) 3_666 3_666 ?
V4 O19 V1 85.153(17) 3_666 . ?
V4 O19 V4 180.00(2) . 3_666 ?
V4 O19 V6 85.050(17) 3_666 . ?
V4 O19 V6 94.952(17) 3_666 3_666 ?
V4 O19 V6 94.952(17) . . ?
V4 O19 V6 85.046(17) . 3_666 ?
V6 O19 V6 180.0 3_666 . ?
C42 O25 C61 115.5(3) . . ?
O5 C26 H26A 109.4 . . ?
O5 C26 H26B 109.4 . . ?
O5 C26 C36 111.3(2) . . ?
H26A C26 H26B 108.0 . . ?
C36 C26 H26A 109.4 . . ?
C36 C26 H26B 109.4 . . ?
C31 C27 C35 108.5(2) . . ?
C31 C27 C38 111.4(2) . . ?
C31 C27 C43 105.3(2) . . ?
C35 C27 C43 110.4(2) . . ?
C38 C27 C35 111.0(2) . . ?
C38 C27 C43 110.2(2) . . ?
O16 C31 C27 109.9(2) . . ?
O23 C31 O16 124.1(3) . . ?
O23 C31 C27 126.0(3) . . ?
O8 C35 C27 111.3(2) . . ?
O8 C35 H35A 109.4 . . ?
O8 C35 H35B 109.4 . . ?
C27 C35 H35A 109.4 . . ?
C27 C35 H35B 109.4 . . ?
H35A C35 H35B 108.0 . . ?
C26 C36 C41 109.7(2) . . ?
C26 C36 C42 107.5(3) . . ?
C41 C36 C42 108.8(3) . . ?
C50 C36 C26 111.4(2) . . ?
C50 C36 C41 110.4(2) . . ?
C50 C36 C42 108.9(3) . . ?
O6 C38 C27 111.4(2) . . ?
O6 C38 H38A 109.3 . . ?
O6 C38 H38B 109.3 . . ?
C27 C38 H38A 109.3 . . ?
C27 C38 H38B 109.3 . . ?
H38A C38 H38B 108.0 . . ?
O11 C41 C36 111.7(2) . . ?
O11 C41 H41A 109.3 . . ?
O11 C41 H41B 109.3 . . ?
C36 C41 H41A 109.3 . . ?
C36 C41 H41B 109.3 . . ?
H41A C41 H41B 107.9 . . ?
O25 C42 C36 109.1(3) . . ?
O55 C42 O25 125.7(3) . . ?
O55 C42 C36 124.8(3) . . ?
O3 C43 C27 111.9(2) . . ?
O3 C43 H43A 109.2 . . ?
O3 C43 H43B 109.2 . . ?
C27 C43 H43A 109.2 . . ?
C27 C43 H43B 109.2 . . ?
H43A C43 H43B 107.9 . . ?
C65 N C10 101.1(4) . . ?
C65 N C21 112.1(3) . . ?
C65 N C2 103.1(3) . . ?
C65 N C16 126.7(6) . . ?
C1 N C65 108.6(4) . . ?
C1 N C21 116.5(4) . . ?
C1 N C2 110.8(5) . . ?
C21 N C10 105.3(4) . . ?
C21 N C2 104.9(3) . . ?
C21 N C16 106.7(4) . . ?
C16 N C10 102.3(7) . . ?
O14 C50 C36 111.4(2) . . ?
O14 C50 H50A 109.3 . . ?
O14 C50 H50B 109.3 . . ?
C36 C50 H50A 109.3 . . ?
C36 C50 H50B 109.3 . . ?
H50A C50 H50B 108.0 . . ?
O16 C56 H56A 110.0 . . ?
O16 C56 H56B 110.0 . . ?
O16 C56 C58 108.4(3) . . ?
H56A C56 H56B 108.4 . . ?
C58 C56 H56A 110.0 . . ?
C58 C56 H56B 110.0 . . ?
F24 C58 F29 106.7(3) . . ?
F24 C58 F37 107.4(3) . . ?
F24 C58 C56 111.2(3) . . ?
F29 C58 C56 112.6(3) . . ?
F37 C58 F29 105.7(3) . . ?
F37 C58 C56 112.8(3) . . ?
O25 C61 H61A 109.8 . . ?
O25 C61 H61B 109.8 . . ?
O25 C61 C63 109.3(3) . . ?
H61A C61 H61B 108.3 . . ?
C63 C61 H61A 109.8 . . ?
C63 C61 H61B 109.8 . . ?
F48 C63 C61 112.6(4) . . ?
F51 C63 F48 107.5(4) . . ?
F51 C63 C61 110.2(4) . . ?
F54 C63 F48 105.9(4) . . ?
F54 C63 F51 107.2(4) . . ?
F54 C63 C61 113.1(4) . . ?
N C65 H65A 107.4 . . ?
N C65 H65B 107.4 . . ?
N C65 H65C 112.0 . . ?
N C65 H65D 112.0 . . ?
N C65 C77 119.6(4) . . ?
N C65 C15 98.7(6) . . ?
H65A C65 H65B 106.9 . . ?
H65C C65 H65D 109.7 . . ?
C77 C65 H65A 107.4 . . ?
C77 C65 H65B 107.4 . . ?
C15 C65 H65C 112.0 . . ?
C15 C65 H65D 112.0 . . ?
C65 C77 H77A 108.4 . . ?
C65 C77 H77B 108.4 . . ?
C65 C77 C14 115.6(6) . . ?
H77A C77 H77B 107.4 . . ?
C14 C77 H77A 108.4 . . ?
C14 C77 H77B 108.4 . . ?
C28 N0AA C39 110.7(2) . . ?
C30 N0AA C28 107.0(2) . . ?
C30 N0AA C34 111.5(2) . . ?
C30 N0AA C39 110.6(2) . . ?
C34 N0AA C28 110.5(2) . . ?
C34 N0AA C39 106.5(2) . . ?
N0AA C28 H28A 108.3 . . ?
N0AA C28 H28B 108.3 . . ?
H28A C28 H28B 107.4 . . ?
C52 C28 N0AA 115.9(2) . . ?
C52 C28 H28A 108.3 . . ?
C52 C28 H28B 108.3 . . ?
N0AA C30 H30A 108.5 . . ?
N0AA C30 H30B 108.5 . . ?
N0AA C30 C57 115.2(2) . . ?
H30A C30 H30B 107.5 . . ?
C57 C30 H30A 108.5 . . ?
C57 C30 H30B 108.5 . . ?
H32A C32 H32B 108.1 . . ?
C39 C32 H32A 109.6 . . ?
C39 C32 H32B 109.6 . . ?
C39 C32 C53 110.3(3) . . ?
C53 C32 H32A 109.6 . . ?
C53 C32 H32B 109.6 . . ?
H33A C33 H33B 107.7 . . ?
C40 C33 H33A 108.8 . . ?
C40 C33 H33B 108.8 . . ?
C59 C33 H33A 108.8 . . ?
C59 C33 H33B 108.8 . . ?
C59 C33 C40 113.8(3) . . ?
N0AA C34 H34A 108.4 . . ?
N0AA C34 H34B 108.4 . . ?
H34A C34 H34B 107.5 . . ?
C40 C34 N0AA 115.4(2) . . ?
C40 C34 H34A 108.4 . . ?
C40 C34 H34B 108.4 . . ?
N0AA C39 H39A 108.3 . . ?
N0AA C39 H39B 108.3 . . ?
C32 C39 N0AA 115.8(2) . . ?
C32 C39 H39A 108.3 . . ?
C32 C39 H39B 108.3 . . ?
H39A C39 H39B 107.4 . . ?
C33 C40 H40A 109.6 . . ?
C33 C40 H40B 109.6 . . ?
C34 C40 C33 110.2(2) . . ?
C34 C40 H40A 109.6 . . ?
C34 C40 H40B 109.6 . . ?
H40A C40 H40B 108.1 . . ?
H44A C44 H44B 107.8 . . ?
C45 C44 H44A 109.0 . . ?
C45 C44 H44B 109.0 . . ?
C52 C44 H44A 109.0 . . ?
C52 C44 H44B 109.0 . . ?
C52 C44 C45 112.7(3) . . ?
C44 C45 H45A 109.5 . . ?
C44 C45 H45B 109.5 . . ?
C44 C45 H45C 109.5 . . ?
H45A C45 H45B 109.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?
H46A C46 H46B 107.9 . . ?
C57 C46 H46A 109.3 . . ?
C57 C46 H46B 109.3 . . ?
C57 C46 C67 111.8(3) . . ?
C67 C46 H46A 109.3 . . ?
C67 C46 H46B 109.3 . . ?
C28 C52 C44 108.8(2) . . ?
C28 C52 H52A 109.9 . . ?
C28 C52 H52B 109.9 . . ?
C44 C52 H52A 109.9 . . ?
C44 C52 H52B 109.9 . . ?
H52A C52 H52B 108.3 . . ?
C32 C53 H53A 109.1 . . ?
C32 C53 H53B 109.1 . . ?
H53A C53 H53B 107.8 . . ?
C64 C53 C32 112.7(3) . . ?
C64 C53 H53A 109.1 . . ?
C64 C53 H53B 109.1 . . ?
C30 C57 H57A 109.4 . . ?
C30 C57 H57B 109.4 . . ?
C46 C57 C30 111.2(3) . . ?
C46 C57 H57A 109.4 . . ?
C46 C57 H57B 109.4 . . ?
H57A C57 H57B 108.0 . . ?
C33 C59 H59A 109.5 . . ?
C33 C59 H59B 109.5 . . ?
C33 C59 H59C 109.5 . . ?
H59A C59 H59B 109.5 . . ?
H59A C59 H59C 109.5 . . ?
H59B C59 H59C 109.5 . . ?
C53 C64 H64A 109.5 . . ?
C53 C64 H64B 109.5 . . ?
C53 C64 H64C 109.5 . . ?
H64A C64 H64B 109.5 . . ?
H64A C64 H64C 109.5 . . ?
H64B C64 H64C 109.5 . . ?
C46 C67 H67A 109.5 . . ?
C46 C67 H67B 109.5 . . ?
C46 C67 H67C 109.5 . . ?
H67A C67 H67B 109.5 . . ?
H67A C67 H67C 109.5 . . ?
H67B C67 H67C 109.5 . . ?
N C1 H1A 108.4 . . ?
N C1 H1B 108.4 . . ?
N C1 C7 115.6(6) . . ?
H1A C1 H1B 107.4 . . ?
C7 C1 H1A 108.4 . . ?
C7 C1 H1B 108.4 . . ?
H3AA C3 H3AB 107.8 . . ?
H3BC C3 H3BD 109.8 . . ?
C5 C3 H3AA 109.0 . . ?
C5 C3 H3AB 109.0 . . ?
C21 C3 H3AA 109.0 . . ?
C21 C3 H3AB 109.0 . . ?
C21 C3 H3BC 112.1 . . ?
C21 C3 H3BD 112.1 . . ?
C21 C3 C5 112.8(4) . . ?
C21 C3 C1E 98.2(8) . . ?
C1E C3 H3BC 112.1 . . ?
C1E C3 H3BD 112.1 . . ?
H4A C4 H4B 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C5 C4 H4A 109.5 . . ?
C5 C4 H4B 109.5 . . ?
C5 C4 H4C 109.5 . . ?
C3 C5 H5A 110.1 . . ?
C3 C5 H5B 110.1 . . ?
C4 C5 C3 107.8(6) . . ?
C4 C5 H5A 110.1 . . ?
C4 C5 H5B 110.1 . . ?
H5A C5 H5B 108.5 . . ?
C1 C7 H7A 109.6 . . ?
C1 C7 H7B 109.6 . . ?
C1 C7 C12 110.4(9) . . ?
H7A C7 H7B 108.1 . . ?
C12 C7 H7A 109.6 . . ?
C12 C7 H7B 109.6 . . ?
H0AA C0AA H0AB 107.7 . . ?
C1AA C0AA H0AA 108.9 . . ?
C1AA C0AA H0AB 108.9 . . ?
C1AA C0AA C11 113.5(10) . . ?
C11 C0AA H0AA 108.9 . . ?
C11 C0AA H0AB 108.9 . . ?
C0AA C1AA H1AA 109.5 . . ?
C0AA C1AA H1AB 109.5 . . ?
C0AA C1AA H1AC 109.5 . . ?
H1AA C1AA H1AB 109.5 . . ?
H1AA C1AA H1AC 109.5 . . ?
H1AB C1AA H1AC 109.5 . . ?
C0AA C11 H11A 109.9 . . ?
C0AA C11 H11B 109.9 . . ?
C0AA C11 C10 108.9(8) . . ?
H11A C11 H11B 108.3 . . ?
C10 C11 H11A 109.9 . . ?
C10 C11 H11B 109.9 . . ?
C7 C12 H12A 109.0 . . ?
C7 C12 H12B 109.0 . . ?
H12A C12 H12B 107.8 . . ?
C13 C12 C7 112.9(11) . . ?
C13 C12 H12A 109.0 . . ?
C13 C12 H12B 109.0 . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
N C10 H10A 107.7 . . ?
N C10 H10B 107.7 . . ?
C11 C10 N 118.3(7) . . ?
C11 C10 H10A 107.7 . . ?
C11 C10 H10B 107.7 . . ?
H10A C10 H10B 107.1 . . ?
N C21 H21A 108.5 . . ?
N C21 H21B 108.5 . . ?
C3 C21 N 114.9(3) . . ?
C3 C21 H21A 108.5 . . ?
C3 C21 H21B 108.5 . . ?
H21A C21 H21B 107.5 . . ?
N C2 H2A 108.5 . . ?
N C2 H2B 108.5 . . ?
H2A C2 H2B 107.5 . . ?
C9 C2 N 115.2(4) . . ?
C9 C2 H2A 108.5 . . ?
C9 C2 H2B 108.5 . . ?
H6A C6 H6B 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C14 C6 H6A 109.5 . . ?
C14 C6 H6B 109.5 . . ?
C14 C6 H6C 109.5 . . ?
C2 C9 H9A 109.6 . . ?
C2 C9 H9B 109.6 . . ?
C2 C9 C1B 110.1(4) . . ?
H9A C9 H9B 108.2 . . ?
C1B C9 H9A 109.6 . . ?
C1B C9 H9B 109.6 . . ?
C77 C14 H14A 109.0 . . ?
C77 C14 H14B 109.0 . . ?
C6 C14 C77 113.0(9) . . ?
C6 C14 H14A 109.0 . . ?
C6 C14 H14B 109.0 . . ?
H14A C14 H14B 107.8 . . ?
N C16 H16A 108.8 . . ?
N C16 H16B 108.8 . . ?
H16A C16 H16B 107.7 . . ?
C17 C16 N 113.7(8) . . ?
C17 C16 H16A 108.8 . . ?
C17 C16 H16B 108.8 . . ?
C16 C17 H17A 108.9 . . ?
C16 C17 H17B 108.9 . . ?
C16 C17 C19 113.4(11) . . ?
H17A C17 H17B 107.7 . . ?
C19 C17 H17A 108.9 . . ?
C19 C17 H17B 108.9 . . ?
H1CA C1C H1CB 109.5 . . ?
H1CA C1C H1CC 109.5 . . ?
H1CB C1C H1CC 109.5 . . ?
C1E C1C H1CA 109.5 . . ?
C1E C1C H1CB 109.5 . . ?
C1E C1C H1CC 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C1B C18 H18A 109.5 . . ?
C1B C18 H18B 109.5 . . ?
C1B C18 H18C 109.5 . . ?
C17 C19 H19A 109.9 . . ?
C17 C19 H19B 109.9 . . ?
H19A C19 H19B 108.3 . . ?
C1A C19 C17 109(2) . . ?
C1A C19 H19A 109.9 . . ?
C1A C19 H19B 109.9 . . ?
C19 C1A H1AD 109.5 . . ?
C19 C1A H1AE 109.5 . . ?
C19 C1A H1AF 109.5 . . ?
H1AD C1A H1AE 109.5 . . ?
H1AD C1A H1AF 109.5 . . ?
H1AE C1A H1AF 109.5 . . ?
C9 C1B C18 111.3(6) . . ?
C9 C1B H1BA 109.4 . . ?
C9 C1B H1BB 109.4 . . ?
C18 C1B H1BA 109.4 . . ?
C18 C1B H1BB 109.4 . . ?
H1BA C1B H1BB 108.0 . . ?
H8A C8 H8B 108.5 . . ?
C15 C8 H8A 110.1 . . ?
C15 C8 H8B 110.1 . . ?
C1D C8 H8A 110.1 . . ?
C1D C8 H8B 110.1 . . ?
C1D C8 C15 107.8(15) . . ?
C65 C15 C8 103.2(9) . . ?
C65 C15 H15A 111.1 . . ?
C65 C15 H15B 111.1 . . ?
C8 C15 H15A 111.1 . . ?
C8 C15 H15B 111.1 . . ?
H15A C15 H15B 109.1 . . ?
C8 C1D H1DA 109.5 . . ?
C8 C1D H1DB 109.5 . . ?
C8 C1D H1DC 109.5 . . ?
H1DA C1D H1DB 109.5 . . ?
H1DA C1D H1DC 109.5 . . ?
H1DB C1D H1DC 109.5 . . ?
C3 C1E H1EA 108.5 . . ?
C3 C1E H1EB 108.5 . . ?
C1C C1E C3 115.1(14) . . ?
C1C C1E H1EA 108.5 . . ?
C1C C1E H1EB 108.5 . . ?
H1EA C1E H1EB 107.5 . . ?

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 V6 O7 V4 46.84(9) 3_666 . . 3_666 ?
V1 O3 C43 C27 68.2(3) . . . . ?
V1 O8 C35 C27 -69.1(2) . . . . ?
V2 V5 O9 V3 46.58(9) 3_566 . . 3_566 ?
V2 O5 C26 C36 -67.8(3) . . . . ?
V2 O14 C50 C36 69.1(3) . . . . ?
V3 V2 O4 V5 47.28(9) 3_566 . . 3_566 ?
V3 O5 C26 C36 70.7(3) . . . . ?
V3 O11 C41 C36 -68.2(3) . . . . ?
V4 V1 O2 V6 46.90(9) 3_666 . . 3_666 ?
V4 O6 C38 C27 -69.0(2) . . . . ?
V4 O8 C35 C27 68.2(2) . . . . ?
V5 V2 O10 V3 -48.47(9) 3_566 . . 3_566 ?
V5 O11 C41 C36 69.0(3) . . . . ?
V5 O14 C50 C36 -68.6(3) . . . . ?
V6 V1 O1 V4 -47.15(9) 3_666 . . 3_666 ?
V6 O3 C43 C27 -68.7(3) . . . . ?
V6 O6 C38 C27 69.7(2) . . . . ?
O1 V1 O2 V6 80.81(11) . . . 3_666 ?
O2 V1 O1 V4 -80.50(11) . . . 3_666 ?
O2 V6 O7 V4 80.20(11) 3_666 . . 3_666 ?
O3 V1 O1 V4 77.95(10) . . . 3_666 ?
O3 V1 O2 V6 -14.2(3) . . . 3_666 ?
O3 V6 O7 V4 -78.01(10) . . . 3_666 ?
O4 V2 O10 V3 -82.19(11) . . . 3_566 ?
O4 V5 O9 V3 81.09(11) 3_566 . . 3_566 ?
O5 V2 O4 V5 -77.74(11) . . . 3_566 ?
O5 V2 O10 V3 10.9(3) . . . 3_566 ?
O5 C26 C36 C41 -62.1(3) . . . . ?
O5 C26 C36 C42 179.7(3) . . . . ?
O5 C26 C36 C50 60.4(3) . . . . ?
O6 V6 O7 V4 -14.9(3) . . . 3_666 ?
O8 V1 O1 V4 15.1(3) . . . 3_666 ?
O8 V1 O2 V6 -77.88(10) . . . 3_666 ?
O10 V2 O4 V5 81.26(11) . . . 3_566 ?
O11 V5 O9 V3 -17.8(3) . . . 3_566 ?
O12 V6 O7 V4 -174.32(11) . . . 3_666 ?
O13 V1 O1 V4 173.88(10) . . . 3_666 ?
O13 V1 O2 V6 -173.25(10) . . . 3_666 ?
O14 V2 O4 V5 -14.6(3) . . . 3_566 ?
O14 V2 O10 V3 76.67(11) . . . 3_566 ?
O14 V5 O9 V3 -78.25(11) . . . 3_566 ?
O15 V2 O4 V5 -172.41(11) . . . 3_566 ?
O15 V2 O10 V3 172.90(10) . . . 3_566 ?
O16 C56 C58 F24 177.3(3) . . . . ?
O16 C56 C58 F29 -63.0(4) . . . . ?
O16 C56 C58 F37 56.5(4) . . . . ?
O17 V2 O4 V5 -0.37(8) . . . 3_566 ?
O17 V2 O10 V3 -1.14(8) . . . 3_566 ?
O17 V5 O9 V3 -0.63(9) . . . 3_566 ?
O19 V1 O1 V4 0.20(8) . . . 3_666 ?
O19 V1 O2 V6 -0.16(8) . . . 3_666 ?
O19 V6 O7 V4 -0.36(8) . . . 3_666 ?
O22 V5 O9 V3 -173.40(11) . . . 3_566 ?
O25 C61 C63 F48 -57.6(5) . . . . ?
O25 C61 C63 F51 -177.6(3) . . . . ?
O25 C61 C63 F54 62.4(5) . . . . ?
C26 C36 C41 O11 61.2(3) . . . . ?
C26 C36 C42 O25 -172.7(3) . . . . ?
C26 C36 C42 O55 0.3(6) . . . . ?
C26 C36 C50 O14 -60.7(3) . . . . ?
C31 O16 C56 C58 -99.6(3) . . . . ?
C31 C27 C35 O8 176.5(2) . . . . ?
C31 C27 C38 O6 -177.8(2) . . . . ?
C31 C27 C43 O3 -178.4(2) . . . . ?
C35 C27 C31 O16 159.1(2) . . . . ?
C35 C27 C31 O23 -24.2(4) . . . . ?
C35 C27 C38 O6 61.3(3) . . . . ?
C35 C27 C43 O3 -61.5(3) . . . . ?
C38 C27 C31 O16 36.7(3) . . . . ?
C38 C27 C31 O23 -146.6(3) . . . . ?
C38 C27 C35 O8 -60.8(3) . . . . ?
C38 C27 C43 O3 61.4(3) . . . . ?
C41 C36 C42 O25 68.5(4) . . . . ?
C41 C36 C42 O55 -118.5(5) . . . . ?
C41 C36 C50 O14 61.5(3) . . . . ?
C42 O25 C61 C63 102.0(4) . . . . ?
C42 C36 C41 O11 178.6(3) . . . . ?
C42 C36 C50 O14 -179.2(2) . . . . ?
C43 C27 C31 O16 -82.8(3) . . . . ?
C43 C27 C31 O23 94.0(3) . . . . ?
C43 C27 C35 O8 61.6(3) . . . . ?
C43 C27 C38 O6 -61.3(3) . . . . ?
N C65 C77 C14 -178.9(6) . . . . ?
N C65 C15 C8 176.0(10) . . . . ?
N C1 C7 C12 175.4(8) . . . . ?
N C2 C9 C1B -161.5(5) . . . . ?
N C16 C17 C19 174.6(13) . . . . ?
C50 C36 C41 O11 -61.9(3) . . . . ?
C50 C36 C42 O25 -51.9(4) . . . . ?
C50 C36 C42 O55 121.1(4) . . . . ?
C56 O16 C31 O23 -4.6(4) . . . . ?
C56 O16 C31 C27 172.2(2) . . . . ?
C61 O25 C42 C36 177.9(3) . . . . ?
C61 O25 C42 O55 5.0(6) . . . . ?
C65 N C1 C7 179.2(6) . . . . ?
C65 N C10 C11 -178.1(7) . . . . ?
C65 N C21 C3 55.2(5) . . . . ?
C65 N C2 C9 -52.6(6) . . . . ?
C65 N C16 C17 -54.3(14) . . . . ?
C65 C77 C14 C6 -58.3(10) . . . . ?
N0AA C28 C52 C44 167.9(3) . . . . ?
N0AA C30 C57 C46 -176.1(3) . . . . ?
N0AA C34 C40 C33 172.3(3) . . . . ?
C28 N0AA C30 C57 -174.6(3) . . . . ?
C28 N0AA C34 C40 61.3(3) . . . . ?
C28 N0AA C39 C32 -50.0(3) . . . . ?
C30 N0AA C28 C52 -178.9(2) . . . . ?
C30 N0AA C34 C40 -57.6(3) . . . . ?
C30 N0AA C39 C32 68.5(3) . . . . ?
C34 N0AA C28 C52 59.5(3) . . . . ?
C34 N0AA C30 C57 -53.6(3) . . . . ?
C34 N0AA C39 C32 -170.2(3) . . . . ?
C39 N0AA C28 C52 -58.3(3) . . . . ?
C39 N0AA C30 C57 64.8(3) . . . . ?
C39 N0AA C34 C40 -178.4(3) . . . . ?
C39 C32 C53 C64 -175.3(3) . . . . ?
C45 C44 C52 C28 174.5(3) . . . . ?
C53 C32 C39 N0AA -169.5(3) . . . . ?
C59 C33 C40 C34 174.8(3) . . . . ?
C67 C46 C57 C30 179.2(3) . . . . ?
C1 N C65 C77 -178.7(6) . . . . ?
C1 N C21 C3 -70.7(6) . . . . ?
C1 N C2 C9 63.4(7) . . . . ?
C1 C7 C12 C13 174.9(10) . . . . ?
C5 C3 C21 N 171.5(5) . . . . ?
C0AA C11 C10 N -172.2(8) . . . . ?
C1AA C0AA C11 C10 179.0(10) . . . . ?
C10 N C65 C15 -171.0(8) . . . . ?
C10 N C21 C3 -53.8(6) . . . . ?
C10 N C16 C17 59.8(12) . . . . ?
C21 N C65 C77 51.1(5) . . . . ?
C21 N C65 C15 77.3(7) . . . . ?
C21 N C1 C7 -53.1(8) . . . . ?
C21 N C10 C11 -61.2(8) . . . . ?
C21 N C2 C9 -170.1(5) . . . . ?
C21 N C16 C17 170.1(10) . . . . ?
C21 C3 C5 C4 76.0(6) . . . . ?
C21 C3 C1E C1C 158.4(14) . . . . ?
C2 N C65 C77 -61.2(5) . . . . ?
C2 N C1 C7 66.7(7) . . . . ?
C2 N C21 C3 166.5(5) . . . . ?
C2 C9 C1B C18 79.0(7) . . . . ?
C16 N C65 C15 -56.3(10) . . . . ?
C16 N C10 C11 50.1(9) . . . . ?
C16 N C21 C3 -162.1(7) . . . . ?
C16 C17 C19 C1A -71.9(18) . . . . ?
C1D C8 C15 C65 36.6(19) . . . . ?
C1E C3 C21 N -165.4(7) . . . . ?

_shelx_SHELXL_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_kuixi
_database_code_depnum_ccdc_archive 'CCDC 1503809'
_audit_update_record             
;
2016-09-10 deposited with the CCDC.
2017-02-17 downloaded from the CCDC.
;
_audit_creation_date             2016-08-19
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C30 H50 O23 V6, 2(C16 H36 N)'
_chemical_formula_sum            'C62 H122 N2 O23 V6'
_chemical_formula_weight         1569.25
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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                   11.562(2)
_cell_length_b                   12.318(3)
_cell_length_c                   15.050(3)
_cell_angle_alpha                78.38(3)
_cell_angle_beta                 89.80(3)
_cell_angle_gamma                62.09(3)
_cell_volume                     1845.0(8)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    6756
_cell_measurement_temperature    173.1500
_cell_measurement_theta_max      31.4970
_cell_measurement_theta_min      2.3161
_shelx_estimated_absorpt_T_max   0.856
_shelx_estimated_absorpt_T_min   0.700
_exptl_absorpt_coefficient_mu    0.801
_exptl_absorpt_correction_T_max  0.852
_exptl_absorpt_correction_T_min  0.743
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    1.412
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       Prism
_exptl_crystal_F_000             830
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.2
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0325
_diffrn_reflns_av_unetI/netI     0.0380
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            18958
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_min         2.556
_diffrn_ambient_temperature      173.15
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  
;
Saturn724+ (2x2 bin mode)
;
_diffrn_measurement_method       dtprofit.ref
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Rotating Anode'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6754
_reflns_number_total             7224
_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       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2008)'
_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    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.959
_refine_diff_density_min         -1.033
_refine_diff_density_rms         0.073
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     425
_refine_ls_number_reflns         7224
_refine_ls_number_restraints     7
_refine_ls_R_factor_all          0.0532
_refine_ls_R_factor_gt           0.0492
_refine_ls_restrained_S_all      1.103
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0576P)²+1.9644P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1229
_refine_ls_wR_factor_ref         0.1263
_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid bond restraints
 C20, O17
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
3. Uiso/Uaniso restraints and constraints
C20 \\sim O17: within 2A with sigma of 0.001 and sigma for terminal atoms of
0.002
4.a Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C8(H8A,H8B), C11(H11A,H11B), C26(H26A,H26B), C16(H16A,H16B),
 C19(H19A,H19B), C1(H1A,H1B), C21(H21A,H21B), C22(H22A,H22B), C24(H24A,H24B),
 C2(H2A,H2B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B), C7(H7A,H7B), C9(H9A,H9B),
 C10(H10A,H10B), C12(H12A,H12B), C14(H14A,H14B), C15(H15A,H15B), C18(H18A,H18B),
  C1A(H1AA,H1AB), C1C(H1CA,H1CB)
4.b Aromatic/amide H refined with riding coordinates:
 C23(H23)
4.c X=CH2 refined with riding coordinates:
 C25(H25A,H25B)
4.d Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C1B(H1BA,H1BB,H1BC), C1D(H1DA,H1DB,H1DC), C1E(H1EA,H1EB,
 H1EC)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_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
V2 V -0.02496(4) -0.17257(4) 0.04272(3) 0.02206(12) Uani 1 1 d . . . . .
V3 V 0.13881(4) -0.04555(4) 0.12244(3) 0.02259(13) Uani 1 1 d . . . . .
V1 V -0.18056(4) 0.12577(4) 0.05741(3) 0.02159(12) Uani 1 1 d . . . . .
O10 O -0.13119(17) -0.10474(17) -0.06370(13) 0.0246(4) Uani 1 1 d . . . . .
O8 O 0.12712(17) -0.24110(17) -0.01144(13) 0.0241(4) Uani 1 1 d . . . . .
O9 O -0.04130(19) -0.29418(17) 0.08747(14) 0.0284(4) Uani 1 1 d . . . . .
O7 O 0.0000 0.0000 0.0000 0.0184(5) Uani 1 2 d S T P . .
O6 O 0.25822(16) -0.13733(17) 0.05173(13) 0.0246(4) Uani 1 1 d . . . . .
O5 O -0.30222(17) 0.19951(18) 0.11258(13) 0.0278(4) Uani 1 1 d . . . . .
O4 O 0.22212(18) -0.08063(19) 0.21799(13) 0.0301(4) Uani 1 1 d . . . . .
O3 O 0.08673(17) -0.18332(16) 0.15102(12) 0.0217(4) Uani 1 1 d . . . . .
O2 O -0.03987(17) 0.05657(17) 0.16212(12) 0.0215(4) Uani 1 1 d . . . . .
O1 O -0.17116(17) -0.04642(17) 0.09908(12) 0.0221(4) Uani 1 1 d . . . . .
C3 C 0.0533(3) -0.2143(3) 0.24050(18) 0.0275(6) Uani 1 1 d . . . . .
H3A H 0.1232 -0.2305 0.2851 0.033 Uiso 1 1 calc R . . . .
H3B H 0.0458 -0.2907 0.2476 0.033 Uiso 1 1 calc R . . . .
O11 O -0.1217(3) -0.0787(3) 0.40621(17) 0.0652(8) Uani 1 1 d . . . . .
C8 C -0.0667(3) 0.0145(3) 0.25125(18) 0.0257(6) Uani 1 1 d . . . . .
H8A H -0.1486 0.0799 0.2651 0.031 Uiso 1 1 calc R . . . .
H8B H 0.0030 -0.0010 0.2957 0.031 Uiso 1 1 calc R . . . .
C11 C -0.1904(3) -0.0840(3) 0.19117(19) 0.0268(6) Uani 1 1 d . . . . .
H11A H -0.1975 -0.1606 0.1986 0.032 Uiso 1 1 calc R . . . .
H11B H -0.2724 -0.0189 0.2051 0.032 Uiso 1 1 calc R . . . .
C13 C -0.0771(3) -0.1073(3) 0.25877(19) 0.0273(6) Uani 1 1 d . . . . .
O17 O -0.1361(3) -0.2361(3) 0.37074(19) 0.0675(7) Uani 1 1 d . U . . .
C20 C -0.1102(4) -0.1512(4) 0.3547(2) 0.0477(7) Uani 1 1 d . U . . .
C26 C -0.1676(5) -0.1034(4) 0.4960(2) 0.0663(12) Uani 1 1 d . . . . .
H26A H -0.2542 -0.0967 0.4886 0.080 Uiso 1 1 calc R . . . .
H26B H -0.1072 -0.1872 0.5311 0.080 Uiso 1 1 calc R . . . .
C16 C -0.1724(4) -0.0069(4) 0.5419(2) 0.0556(10) Uani 1 1 d . . . . .
H16A H -0.0835 -0.0201 0.5523 0.067 Uiso 1 1 calc R . . . .
H16B H -0.2035 -0.0192 0.6011 0.067 Uiso 1 1 calc R . . . .
C19 C -0.2997(5) 0.3497(5) 0.4833(3) 0.0736(13) Uani 1 1 d . . . . .
H19A H -0.3922 0.3839 0.4635 0.088 Uiso 1 1 calc R . . . .
H19B H -0.2533 0.3458 0.4293 0.088 Uiso 1 1 calc R . . . .
C1 C -0.2503(5) 0.2205(4) 0.5391(3) 0.0698(12) Uani 1 1 d . . . . .
H1A H -0.2999 0.2248 0.5916 0.084 Uiso 1 1 calc R . . . .
H1B H -0.1592 0.1888 0.5617 0.084 Uiso 1 1 calc R . . . .
C21 C -0.2574(5) 0.1264(4) 0.4918(3) 0.0694(12) Uani 1 1 d . . . . .
H21A H -0.3478 0.1426 0.4856 0.083 Uiso 1 1 calc R . . . .
H21B H -0.2306 0.1381 0.4310 0.083 Uiso 1 1 calc R . . . .
C22 C -0.2840(6) 0.4397(5) 0.5326(4) 0.0807(14) Uani 1 1 d . . . . .
H22A H -0.3361 0.4481 0.5839 0.097 Uiso 1 1 calc R . . . .
H22B H -0.1926 0.4011 0.5571 0.097 Uiso 1 1 calc R . . . .
C23 C -0.1597(8) 0.5965(6) 0.5638(4) 0.0946(19) Uani 1 1 d . . . . .
H23 H -0.1051 0.5916 0.5176 0.114 Uiso 1 1 calc R . . . .
C24 C -0.3231(7) 0.5715(5) 0.4761(4) 0.0984(19) Uani 1 1 d . . . . .
H24A H -0.4156 0.6136 0.4533 0.118 Uiso 1 1 calc R . . . .
H24B H -0.2723 0.5655 0.4242 0.118 Uiso 1 1 calc R . . . .
C25 C -0.1060(8) 0.5563(6) 0.6434(4) 0.108(2) Uani 1 1 d . . . . .
H25A H -0.1565 0.5591 0.6921 0.129 Uiso 1 1 calc R . . . .
H25B H -0.0155 0.5233 0.6544 0.129 Uiso 1 1 calc R . . . .
C2 C -0.2976(7) 0.6498(5) 0.5360(6) 0.119(3) Uani 1 1 d . . . . .
H2A H -0.3309 0.7359 0.5015 0.142 Uiso 1 1 calc R . . . .
H2B H -0.3447 0.6515 0.5897 0.142 Uiso 1 1 calc R . . . .
N1 N -0.6788(2) 0.3551(2) 0.04452(16) 0.0233(5) Uani 1 1 d . . . . .
C4 C -0.6142(2) 0.4246(3) 0.07860(19) 0.0241(5) Uani 1 1 d . . . . .
H4A H -0.5254 0.3631 0.1052 0.029 Uiso 1 1 calc R . . . .
H4B H -0.6073 0.4812 0.0264 0.029 Uiso 1 1 calc R . . . .
C5 C -0.5821(2) 0.2707(3) -0.01192(19) 0.0248(6) Uani 1 1 d . . . . .
H5A H -0.5008 0.2127 0.0267 0.030 Uiso 1 1 calc R . . . .
H5B H -0.5624 0.3229 -0.0602 0.030 Uiso 1 1 calc R . . . .
C6 C -0.6836(3) 0.5004(3) 0.1482(2) 0.0275(6) Uani 1 1 d . . . . .
H6A H -0.6982 0.4470 0.1987 0.033 Uiso 1 1 calc R . . . .
H6B H -0.7685 0.5694 0.1203 0.033 Uiso 1 1 calc R . . . .
C7 C -0.5368(3) 0.1334(3) -0.1240(2) 0.0331(7) Uani 1 1 d . . . . .
H7A H -0.4467 0.0936 -0.0965 0.040 Uiso 1 1 calc R . . . .
H7B H -0.5533 0.0679 -0.1377 0.040 Uiso 1 1 calc R . . . .
C9 C -0.6007(3) 0.5527(3) 0.1834(2) 0.0317(6) Uani 1 1 d . . . . .
H9A H -0.5764 0.5961 0.1318 0.038 Uiso 1 1 calc R . . . .
H9B H -0.6537 0.6140 0.2181 0.038 Uiso 1 1 calc R . . . .
C10 C -0.8101(2) 0.4495(3) -0.01229(19) 0.0255(6) Uani 1 1 d . . . . .
H10A H -0.8564 0.4043 -0.0231 0.031 Uiso 1 1 calc R . . . .
H10B H -0.8630 0.5096 0.0232 0.031 Uiso 1 1 calc R . . . .
C12 C -0.6294(3) 0.1944(3) -0.0548(2) 0.0291(6) Uani 1 1 d . . . . .
H12A H -0.7178 0.2492 -0.0851 0.035 Uiso 1 1 calc R . . . .
H12B H -0.6319 0.1293 -0.0075 0.035 Uiso 1 1 calc R . . . .
C14 C -0.7093(3) 0.2774(3) 0.1237(2) 0.0277(6) Uani 1 1 d . . . . .
H14A H -0.7788 0.3346 0.1536 0.033 Uiso 1 1 calc R . . . .
H14B H -0.7425 0.2290 0.0994 0.033 Uiso 1 1 calc R . . . .
C15 C -0.5934(3) 0.1873(3) 0.1946(2) 0.0306(6) Uani 1 1 d . . . . .
H15A H -0.5597 0.2345 0.2202 0.037 Uiso 1 1 calc R . . . .
H15B H -0.5235 0.1284 0.1659 0.037 Uiso 1 1 calc R . . . .
C17 C -0.4764(3) 0.4518(3) 0.2434(2) 0.0418(8) Uani 1 1 d . . . . .
H17A H -0.4200 0.3944 0.2081 0.063 Uiso 1 1 calc GR . . . .
H17B H -0.4993 0.4063 0.2936 0.063 Uiso 1 1 calc GR . . . .
H17C H -0.4313 0.4907 0.2662 0.063 Uiso 1 1 calc GR . . . .
C18 C -0.7997(3) 0.5217(3) -0.10325(19) 0.0274(6) Uani 1 1 d . . . . .
H18A H -0.7461 0.4630 -0.1395 0.033 Uiso 1 1 calc R . . . .
H18B H -0.7576 0.5711 -0.0936 0.033 Uiso 1 1 calc R . . . .
C1A C -0.9365(3) 0.6089(3) -0.1541(2) 0.0339(7) Uani 1 1 d . . . . .
H1AA H -0.9782 0.5589 -0.1631 0.041 Uiso 1 1 calc R . . . .
H1AB H -0.9897 0.6667 -0.1172 0.041 Uiso 1 1 calc R . . . .
C1B C -0.5518(3) 0.2255(3) -0.2125(2) 0.0435(8) Uani 1 1 d . . . . .
H1BA H -0.4921 0.1811 -0.2528 0.065 Uiso 1 1 calc GR . . . .
H1BB H -0.5323 0.2890 -0.2000 0.065 Uiso 1 1 calc GR . . . .
H1BC H -0.6405 0.2647 -0.2407 0.065 Uiso 1 1 calc GR . . . .
C1C C -0.6351(3) 0.1151(3) 0.2703(2) 0.0407(7) Uani 1 1 d . . . . .
H1CA H -0.7095 0.1746 0.2955 0.049 Uiso 1 1 calc R . . . .
H1CB H -0.6633 0.0639 0.2449 0.049 Uiso 1 1 calc R . . . .
C1D C -0.5247(4) 0.0307(4) 0.3462(2) 0.0519(9) Uani 1 1 d . . . . .
H1DA H -0.4524 -0.0310 0.3221 0.078 Uiso 1 1 calc GR . . . .
H1DB H -0.5559 -0.0113 0.3931 0.078 Uiso 1 1 calc GR . . . .
H1DC H -0.4961 0.0809 0.3714 0.078 Uiso 1 1 calc GR . . . .
C1E C -0.9317(4) 0.6838(3) -0.2459(3) 0.0508(9) Uani 1 1 d . . . . .
H1EA H -0.8855 0.6272 -0.2845 0.076 Uiso 1 1 calc GR . . . .
H1EB H -0.8869 0.7304 -0.2376 0.076 Uiso 1 1 calc GR . . . .
H1EC H -1.0198 0.7413 -0.2737 0.076 Uiso 1 1 calc GR . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
V2 V3 3.0250(16) 2 ?
V2 V1 3.0260(10) 2 ?
V2 O10 1.813(2) . ?
V2 O8 1.8293(19) . ?
V2 O9 1.6097(19) . ?
V2 O7 2.2445(7) . ?
V2 O3 2.0272(19) . ?
V2 O1 2.0132(19) . ?
V3 V2 3.0251(16) 2 ?
V3 V1 3.0261(10) 2 ?
V3 O10 1.845(2) 2 ?
V3 O7 2.2466(9) . ?
V3 O6 1.825(2) . ?
V3 O4 1.598(2) . ?
V3 O3 2.0220(18) . ?
V3 O2 2.0169(19) . ?
V1 V2 3.0260(10) 2 ?
V1 V3 3.0260(10) 2 ?
V1 O8 1.8170(19) 2 ?
V1 O7 2.2368(10) . ?
V1 O6 1.8222(19) 2 ?
V1 O5 1.6102(19) . ?
V1 O2 2.009(2) . ?
V1 O1 2.0378(19) . ?
O10 V3 1.845(2) 2 ?
O8 V1 1.8170(19) 2 ?
O7 V2 2.2445(7) 2 ?
O7 V3 2.2466(9) 2 ?
O7 V1 2.2368(10) 2 ?
O6 V1 1.8223(19) 2 ?
O3 C3 1.427(3) . ?
O2 C8 1.426(3) . ?
O1 C11 1.421(3) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C3 C13 1.539(4) . ?
O11 C20 1.258(4) . ?
O11 C26 1.476(4) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C8 C13 1.542(4) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C11 C13 1.540(4) . ?
C13 C20 1.548(4) . ?
O17 C20 1.198(4) . ?
C26 H26A 0.9700 . ?
C26 H26B 0.9700 . ?
C26 C16 1.471(5) . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C16 C21 1.492(6) . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C19 C1 1.476(6) . ?
C19 C22 1.527(7) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C1 C21 1.509(6) . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
C22 C24 1.524(7) . ?
C23 H23 0.9300 . ?
C23 C25 1.243(8) . ?
C23 C2 1.436(9) . ?
C24 H24A 0.9700 . ?
C24 H24B 0.9700 . ?
C24 C2 1.565(9) . ?
C25 H25A 0.9300 . ?
C25 H25B 0.9300 . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
N1 C4 1.527(3) . ?
N1 C5 1.521(3) . ?
N1 C10 1.531(3) . ?
N1 C14 1.521(3) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C4 C6 1.516(4) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C5 C12 1.525(4) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C6 C9 1.528(4) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C7 C12 1.533(4) . ?
C7 C1B 1.516(5) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C9 C17 1.519(4) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C10 C18 1.512(4) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C14 C15 1.519(4) . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C15 C1C 1.520(4) . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
C18 C1A 1.525(4) . ?
C1A H1AA 0.9700 . ?
C1A H1AB 0.9700 . ?
C1A C1E 1.516(5) . ?
C1B H1BA 0.9600 . ?
C1B H1BB 0.9600 . ?
C1B H1BC 0.9600 . ?
C1C H1CA 0.9700 . ?
C1C H1CB 0.9700 . ?
C1C C1D 1.518(5) . ?
C1D H1DA 0.9600 . ?
C1D H1DB 0.9600 . ?
C1D H1DC 0.9600 . ?
C1E H1EA 0.9600 . ?
C1E H1EB 0.9600 . ?
C1E H1EC 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 V2 V1 66.28(3) 2 2 ?
O10 V2 V3 34.56(6) . 2 ?
O10 V2 V1 88.66(6) . 2 ?
O10 V2 O8 94.45(9) . . ?
O10 V2 O7 82.24(7) . . ?
O10 V2 O3 158.69(8) . . ?
O10 V2 O1 88.30(9) . . ?
O8 V2 V3 88.50(7) . 2 ?
O8 V2 V1 33.78(6) . 2 ?
O8 V2 O7 81.20(6) . . ?
O8 V2 O3 87.13(8) . . ?
O8 V2 O1 158.13(8) . . ?
O9 V2 V3 138.58(8) . 2 ?
O9 V2 V1 136.02(8) . 2 ?
O9 V2 O10 104.20(10) . . ?
O9 V2 O8 102.53(10) . . ?
O9 V2 O7 172.13(8) . . ?
O9 V2 O3 96.15(9) . . ?
O9 V2 O1 97.79(9) . . ?
O7 V2 V3 47.69(2) . 2 ?
O7 V2 V1 47.42(3) . 2 ?
O3 V2 V3 124.48(6) . 2 ?
O3 V2 V1 80.87(5) . 2 ?
O3 V2 O7 76.99(6) . . ?
O1 V2 V3 81.50(6) . 2 ?
O1 V2 V1 124.88(6) . 2 ?
O1 V2 O7 77.68(6) . . ?
O1 V2 O3 82.69(8) . . ?
V2 V3 V1 66.22(3) 2 2 ?
O10 V3 V2 33.86(6) 2 2 ?
O10 V3 V1 88.51(6) 2 2 ?
O10 V3 O7 81.49(7) 2 . ?
O10 V3 O3 157.88(8) 2 . ?
O10 V3 O2 87.76(8) 2 . ?
O7 V3 V2 47.63(3) . 2 ?
O7 V3 V1 47.41(2) . 2 ?
O6 V3 V2 87.86(7) . 2 ?
O6 V3 V1 33.90(6) . 2 ?
O6 V3 O10 93.93(9) . 2 ?
O6 V3 O7 81.31(6) . . ?
O6 V3 O3 88.11(8) . . ?
O6 V3 O2 157.43(8) . . ?
O4 V3 V2 137.20(8) . 2 ?
O4 V3 V1 138.15(8) . 2 ?
O4 V3 O10 103.61(10) . 2 ?
O4 V3 O7 171.76(8) . . ?
O4 V3 O6 104.55(10) . . ?
O4 V3 O3 97.15(10) . . ?
O4 V3 O2 96.88(9) . . ?
O3 V3 V2 124.47(6) . 2 ?
O3 V3 V1 80.94(6) . 2 ?
O3 V3 O7 77.04(6) . . ?
O2 V3 V2 81.04(6) . 2 ?
O2 V3 V1 123.86(6) . 2 ?
O2 V3 O7 76.68(6) . . ?
O2 V3 O3 82.21(8) . . ?
V2 V1 V3 66.53(3) 2 2 ?
O8 V1 V2 34.04(6) 2 2 ?
O8 V1 V3 88.35(6) 2 2 ?
O8 V1 O7 81.67(6) 2 . ?
O8 V1 O6 94.56(9) 2 2 ?
O8 V1 O2 88.30(8) 2 . ?
O8 V1 O1 158.50(8) 2 . ?
O7 V1 V2 47.63(2) . 2 ?
O7 V1 V3 47.69(3) . 2 ?
O6 V1 V2 89.00(6) 2 2 ?
O6 V1 V3 33.96(6) 2 2 ?
O6 V1 O7 81.64(7) 2 . ?
O6 V1 O2 157.88(8) 2 . ?
O6 V1 O1 87.13(9) 2 . ?
O5 V1 V2 137.70(7) . 2 ?
O5 V1 V3 137.88(7) . 2 ?
O5 V1 O8 104.03(9) . 2 ?
O5 V1 O7 171.30(7) . . ?
O5 V1 O6 104.17(9) . 2 ?
O5 V1 O2 96.35(9) . . ?
O5 V1 O1 96.28(9) . . ?
O2 V1 V2 81.14(6) . 2 ?
O2 V1 V3 124.52(6) . 2 ?
O2 V1 O7 77.07(6) . . ?
O2 V1 O1 82.45(8) . . ?
O1 V1 V2 124.79(6) . 2 ?
O1 V1 V3 81.11(6) . 2 ?
O1 V1 O7 77.37(6) . . ?
V2 O10 V3 111.57(10) . 2 ?
V1 O8 V2 112.17(10) 2 . ?
V2 O7 V2 180.0 . 2 ?
V2 O7 V3 95.31(4) . . ?
V2 O7 V3 95.32(4) 2 2 ?
V2 O7 V3 84.69(4) 2 . ?
V2 O7 V3 84.69(4) . 2 ?
V3 O7 V3 180.0 2 . ?
V1 O7 V2 84.95(3) 2 . ?
V1 O7 V2 95.05(3) 2 2 ?
V1 O7 V2 95.05(3) . . ?
V1 O7 V2 84.95(3) . 2 ?
V1 O7 V3 84.90(3) . 2 ?
V1 O7 V3 95.10(3) 2 2 ?
V1 O7 V3 84.90(3) 2 . ?
V1 O7 V3 95.10(3) . . ?
V1 O7 V1 180.0 2 . ?
V1 O6 V3 112.14(9) 2 . ?
V3 O3 V2 110.13(9) . . ?
C3 O3 V2 118.56(16) . . ?
C3 O3 V3 118.50(16) . . ?
V1 O2 V3 110.53(9) . . ?
C8 O2 V3 118.59(16) . . ?
C8 O2 V1 119.07(15) . . ?
V2 O1 V1 109.35(8) . . ?
C11 O1 V2 118.88(16) . . ?
C11 O1 V1 118.31(16) . . ?
O3 C3 H3A 109.3 . . ?
O3 C3 H3B 109.3 . . ?
O3 C3 C13 111.6(2) . . ?
H3A C3 H3B 108.0 . . ?
C13 C3 H3A 109.3 . . ?
C13 C3 H3B 109.3 . . ?
C20 O11 C26 116.8(3) . . ?
O2 C8 H8A 109.4 . . ?
O2 C8 H8B 109.4 . . ?
O2 C8 C13 111.2(2) . . ?
H8A C8 H8B 108.0 . . ?
C13 C8 H8A 109.4 . . ?
C13 C8 H8B 109.4 . . ?
O1 C11 H11A 109.2 . . ?
O1 C11 H11B 109.2 . . ?
O1 C11 C13 112.2(2) . . ?
H11A C11 H11B 107.9 . . ?
C13 C11 H11A 109.2 . . ?
C13 C11 H11B 109.2 . . ?
C3 C13 C8 110.6(2) . . ?
C3 C13 C11 110.1(2) . . ?
C3 C13 C20 108.4(2) . . ?
C8 C13 C20 111.3(2) . . ?
C11 C13 C8 110.4(2) . . ?
C11 C13 C20 105.9(2) . . ?
O11 C20 C13 112.2(3) . . ?
O17 C20 O11 126.1(3) . . ?
O17 C20 C13 121.2(3) . . ?
O11 C26 H26A 110.6 . . ?
O11 C26 H26B 110.6 . . ?
H26A C26 H26B 108.7 . . ?
C16 C26 O11 105.9(3) . . ?
C16 C26 H26A 110.6 . . ?
C16 C26 H26B 110.6 . . ?
C26 C16 H16A 108.4 . . ?
C26 C16 H16B 108.4 . . ?
C26 C16 C21 115.4(4) . . ?
H16A C16 H16B 107.5 . . ?
C21 C16 H16A 108.4 . . ?
C21 C16 H16B 108.4 . . ?
H19A C19 H19B 107.6 . . ?
C1 C19 H19A 108.7 . . ?
C1 C19 H19B 108.7 . . ?
C1 C19 C22 114.2(4) . . ?
C22 C19 H19A 108.7 . . ?
C22 C19 H19B 108.7 . . ?
C19 C1 H1A 108.2 . . ?
C19 C1 H1B 108.2 . . ?
C19 C1 C21 116.2(4) . . ?
H1A C1 H1B 107.4 . . ?
C21 C1 H1A 108.2 . . ?
C21 C1 H1B 108.2 . . ?
C16 C21 C1 112.8(4) . . ?
C16 C21 H21A 109.0 . . ?
C16 C21 H21B 109.0 . . ?
C1 C21 H21A 109.0 . . ?
C1 C21 H21B 109.0 . . ?
H21A C21 H21B 107.8 . . ?
C19 C22 H22A 108.2 . . ?
C19 C22 H22B 108.2 . . ?
H22A C22 H22B 107.3 . . ?
C24 C22 C19 116.5(5) . . ?
C24 C22 H22A 108.2 . . ?
C24 C22 H22B 108.2 . . ?
C25 C23 H23 116.7 . . ?
C25 C23 C2 126.5(7) . . ?
C2 C23 H23 116.7 . . ?
C22 C24 H24A 109.7 . . ?
C22 C24 H24B 109.7 . . ?
C22 C24 C2 109.9(5) . . ?
H24A C24 H24B 108.2 . . ?
C2 C24 H24A 109.7 . . ?
C2 C24 H24B 109.7 . . ?
C23 C25 H25A 120.0 . . ?
C23 C25 H25B 120.0 . . ?
H25A C25 H25B 120.0 . . ?
C23 C2 C24 111.2(5) . . ?
C23 C2 H2A 109.4 . . ?
C23 C2 H2B 109.4 . . ?
C24 C2 H2A 109.4 . . ?
C24 C2 H2B 109.4 . . ?
H2A C2 H2B 108.0 . . ?
C4 N1 C10 110.3(2) . . ?
C5 N1 C4 106.55(19) . . ?
C5 N1 C10 111.4(2) . . ?
C5 N1 C14 110.7(2) . . ?
C14 N1 C4 111.2(2) . . ?
C14 N1 C10 106.68(19) . . ?
N1 C4 H4A 108.3 . . ?
N1 C4 H4B 108.3 . . ?
H4A C4 H4B 107.4 . . ?
C6 C4 N1 116.1(2) . . ?
C6 C4 H4A 108.3 . . ?
C6 C4 H4B 108.3 . . ?
N1 C5 H5A 108.5 . . ?
N1 C5 H5B 108.5 . . ?
N1 C5 C12 115.1(2) . . ?
H5A C5 H5B 107.5 . . ?
C12 C5 H5A 108.5 . . ?
C12 C5 H5B 108.5 . . ?
C4 C6 H6A 109.6 . . ?
C4 C6 H6B 109.6 . . ?
C4 C6 C9 110.3(2) . . ?
H6A C6 H6B 108.1 . . ?
C9 C6 H6A 109.6 . . ?
C9 C6 H6B 109.6 . . ?
H7A C7 H7B 107.7 . . ?
C12 C7 H7A 108.8 . . ?
C12 C7 H7B 108.8 . . ?
C1B C7 H7A 108.8 . . ?
C1B C7 H7B 108.8 . . ?
C1B C7 C12 113.8(2) . . ?
C6 C9 H9A 108.9 . . ?
C6 C9 H9B 108.9 . . ?
H9A C9 H9B 107.7 . . ?
C17 C9 C6 113.4(2) . . ?
C17 C9 H9A 108.9 . . ?
C17 C9 H9B 108.9 . . ?
N1 C10 H10A 108.5 . . ?
N1 C10 H10B 108.5 . . ?
H10A C10 H10B 107.5 . . ?
C18 C10 N1 115.3(2) . . ?
C18 C10 H10A 108.5 . . ?
C18 C10 H10B 108.5 . . ?
C5 C12 C7 110.2(2) . . ?
C5 C12 H12A 109.6 . . ?
C5 C12 H12B 109.6 . . ?
C7 C12 H12A 109.6 . . ?
C7 C12 H12B 109.6 . . ?
H12A C12 H12B 108.1 . . ?
N1 C14 H14A 108.5 . . ?
N1 C14 H14B 108.5 . . ?
H14A C14 H14B 107.5 . . ?
C15 C14 N1 115.0(2) . . ?
C15 C14 H14A 108.5 . . ?
C15 C14 H14B 108.5 . . ?
C14 C15 H15A 109.6 . . ?
C14 C15 H15B 109.6 . . ?
C14 C15 C1C 110.5(2) . . ?
H15A C15 H15B 108.1 . . ?
C1C C15 H15A 109.6 . . ?
C1C C15 H15B 109.6 . . ?
C9 C17 H17A 109.5 . . ?
C9 C17 H17B 109.5 . . ?
C9 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C10 C18 H18A 109.7 . . ?
C10 C18 H18B 109.7 . . ?
C10 C18 C1A 110.0(2) . . ?
H18A C18 H18B 108.2 . . ?
C1A C18 H18A 109.7 . . ?
C1A C18 H18B 109.7 . . ?
C18 C1A H1AA 109.2 . . ?
C18 C1A H1AB 109.2 . . ?
H1AA C1A H1AB 107.9 . . ?
C1E C1A C18 112.2(3) . . ?
C1E C1A H1AA 109.2 . . ?
C1E C1A H1AB 109.2 . . ?
C7 C1B H1BA 109.5 . . ?
C7 C1B H1BB 109.5 . . ?
C7 C1B H1BC 109.5 . . ?
H1BA C1B H1BB 109.5 . . ?
H1BA C1B H1BC 109.5 . . ?
H1BB C1B H1BC 109.5 . . ?
C15 C1C H1CA 109.1 . . ?
C15 C1C H1CB 109.1 . . ?
H1CA C1C H1CB 107.9 . . ?
C1D C1C C15 112.3(3) . . ?
C1D C1C H1CA 109.1 . . ?
C1D C1C H1CB 109.1 . . ?
C1C C1D H1DA 109.5 . . ?
C1C C1D H1DB 109.5 . . ?
C1C C1D H1DC 109.5 . . ?
H1DA C1D H1DB 109.5 . . ?
H1DA C1D H1DC 109.5 . . ?
H1DB C1D H1DC 109.5 . . ?
C1A C1E H1EA 109.5 . . ?
C1A C1E H1EB 109.5 . . ?
C1A C1E H1EC 109.5 . . ?
H1EA C1E H1EB 109.5 . . ?
H1EA C1E H1EC 109.5 . . ?
H1EB C1E H1EC 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
V2 V3 O6 V1 -48.10(9) 2 . . 2 ?
V2 O3 C3 C13 -68.9(3) . . . . ?
V2 O1 C11 C13 68.6(3) . . . . ?
V3 V2 O8 V1 46.81(9) 2 . . 2 ?
V3 O3 C3 C13 68.9(3) . . . . ?
V3 O2 C8 C13 -69.7(2) . . . . ?
V1 V2 O10 V3 -47.52(9) 2 . . 2 ?
V1 O2 C8 C13 69.7(2) . . . . ?
V1 O1 C11 C13 -68.0(2) . . . . ?
O10 V2 O8 V1 80.88(11) . . . 2 ?
O10 V3 O6 V1 -81.43(11) 2 . . 2 ?
O8 V2 O10 V3 -80.83(11) . . . 2 ?
O9 V2 O10 V3 175.04(10) . . . 2 ?
O9 V2 O8 V1 -173.49(10) . . . 2 ?
O7 V2 O10 V3 -0.35(8) . . . 2 ?
O7 V2 O8 V1 -0.55(8) . . . 2 ?
O7 V3 O6 V1 -0.67(8) . . . 2 ?
O4 V3 O6 V1 173.41(10) . . . 2 ?
O3 V2 O10 V3 12.7(3) . . . 2 ?
O3 V2 O8 V1 -77.82(11) . . . 2 ?
O3 V3 O6 V1 76.51(11) . . . 2 ?
O3 C3 C13 C8 -60.9(3) . . . . ?
O3 C3 C13 C11 61.4(3) . . . . ?
O3 C3 C13 C20 176.8(2) . . . . ?
O2 V3 O6 V1 12.2(3) . . . 2 ?
O2 C8 C13 C3 61.0(3) . . . . ?
O2 C8 C13 C11 -61.0(3) . . . . ?
O2 C8 C13 C20 -178.4(2) . . . . ?
O1 V2 O10 V3 77.44(10) . . . 2 ?
O1 V2 O8 V1 -15.7(3) . . . 2 ?
O1 C11 C13 C3 -61.3(3) . . . . ?
O1 C11 C13 C8 61.1(3) . . . . ?
O1 C11 C13 C20 -178.2(2) . . . . ?
C3 C13 C20 O11 121.9(3) . . . . ?
C3 C13 C20 O17 -66.3(5) . . . . ?
O11 C26 C16 C21 57.3(5) . . . . ?
C8 C13 C20 O11 0.1(4) . . . . ?
C8 C13 C20 O17 171.9(4) . . . . ?
C11 C13 C20 O11 -120.0(3) . . . . ?
C11 C13 C20 O17 51.8(5) . . . . ?
C20 O11 C26 C16 179.9(4) . . . . ?
C26 O11 C20 C13 173.4(3) . . . . ?
C26 O11 C20 O17 2.1(7) . . . . ?
C26 C16 C21 C1 -175.8(4) . . . . ?
C19 C1 C21 C16 163.3(4) . . . . ?
C19 C22 C24 C2 -178.5(5) . . . . ?
C1 C19 C22 C24 175.2(5) . . . . ?
C22 C19 C1 C21 -177.0(5) . . . . ?
C22 C24 C2 C23 64.8(7) . . . . ?
C25 C23 C2 C24 -119.9(7) . . . . ?
N1 C4 C6 C9 173.9(2) . . . . ?
N1 C5 C12 C7 169.1(2) . . . . ?
N1 C10 C18 C1A 178.2(2) . . . . ?
N1 C14 C15 C1C 179.8(2) . . . . ?
C4 N1 C5 C12 -178.6(2) . . . . ?
C4 N1 C10 C18 69.0(3) . . . . ?
C4 N1 C14 C15 -53.1(3) . . . . ?
C4 C6 C9 C17 -69.9(3) . . . . ?
C5 N1 C4 C6 -171.3(2) . . . . ?
C5 N1 C10 C18 -49.2(3) . . . . ?
C5 N1 C14 C15 65.2(3) . . . . ?
C10 N1 C4 C6 67.6(3) . . . . ?
C10 N1 C5 C12 -58.2(3) . . . . ?
C10 N1 C14 C15 -173.5(2) . . . . ?
C10 C18 C1A C1E 179.9(3) . . . . ?
C14 N1 C4 C6 -50.6(3) . . . . ?
C14 N1 C5 C12 60.4(3) . . . . ?
C14 N1 C10 C18 -170.1(2) . . . . ?
C14 C15 C1C C1D -175.9(3) . . . . ?
C1B C7 C12 C5 -74.2(3) . . . . ?

_shelx_SHELXL_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_exp_shiliuchun
_database_code_depnum_ccdc_archive 'CCDC 1503810'
_audit_update_record             
;
2016-09-10 deposited with the CCDC.
2017-02-17 downloaded from the CCDC.
;
_audit_creation_date             2016-08-19
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C42 H78 O23 V6, 2(C16 H36 N)'
_chemical_formula_sum            'C74 H150 N2 O23 V6'
_chemical_formula_weight         1741.59
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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                   11.4081(7)
_cell_length_b                   11.9363(6)
_cell_length_c                   18.8822(11)
_cell_angle_alpha                101.329(4)
_cell_angle_beta                 96.637(5)
_cell_angle_gamma                116.297(5)
_cell_volume                     2199.3(2)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    5270
_cell_measurement_temperature    105.6
_cell_measurement_theta_max      29.1498
_cell_measurement_theta_min      2.9927
_shelx_estimated_absorpt_T_max   0.948
_shelx_estimated_absorpt_T_min   0.759
_exptl_absorpt_coefficient_mu    0.679
_exptl_absorpt_correction_T_max  0.947
_exptl_absorpt_correction_T_min  0.796
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.315
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       'flat stick'
_exptl_crystal_F_000             930
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.08
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0288
_diffrn_reflns_av_unetI/netI     0.0526
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            15055
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_min         2.999
_diffrn_ambient_temperature      105.6
_diffrn_detector_area_resol_mean 16.0971
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -36.00   -3.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -15.9046  -77.0000 -150.0000 33

#__ type_ start__ end____ width___ exp.time_
  2 omega   29.00   54.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       21.1390  -84.0000  139.0000 25

#__ type_ start__ end____ width___ exp.time_
  3 omega   -9.00   84.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       21.1390   77.0000  -60.0000 93

#__ type_ start__ end____ width___ exp.time_
  4 omega    7.00   39.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       21.1390   77.0000   30.0000 32

#__ type_ start__ end____ width___ exp.time_
  5 omega  -45.00   45.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       21.1390  -37.0000   30.0000 90

#__ type_ start__ end____ width___ exp.time_
  6 omega   -5.00   94.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       21.1390   37.0000 -150.0000 99
;
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      -0.0238049000
_diffrn_orient_matrix_UB_12      -0.0064105000
_diffrn_orient_matrix_UB_13      0.0328334000
_diffrn_orient_matrix_UB_21      0.0464902000
_diffrn_orient_matrix_UB_22      -0.0209505000
_diffrn_orient_matrix_UB_23      0.0114880000
_diffrn_orient_matrix_UB_31      0.0484932000
_diffrn_orient_matrix_UB_32      0.0654348000
_diffrn_orient_matrix_UB_33      0.0184407000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                7165
_reflns_number_total             8630
_reflns_odcompleteness_completeness 99.82
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_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    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.337
_refine_diff_density_min         -0.337
_refine_diff_density_rms         0.061
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     480
_refine_ls_number_reflns         8630
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0489
_refine_ls_R_factor_gt           0.0375
_refine_ls_restrained_S_all      1.053
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0206P)²+0.9031P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0745
_refine_ls_wR_factor_ref         0.0809
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C26(H26A,H26B), C22(H22A,H22B), C32(H32A,H32B), C30(H30A,H30B), C34(H34A,
 H34B), C2(H2A,H2B), C24(H24A,H24B), C35(H35A,H35B), C31(H31A,H31B), C1(H1A,
 H1B), C3(H3A,H3B), C23(H23A,H23B), C28(H28A,H28B), C27(H27A,H27B), C6(H6A,H6B),
  C36(H36A,H36B), C7(H7A,H7B), C9(H9A,H9B), C10(H10A,H10B), C13(H13A,H13B),
 C19(H19A,H19B), C15(H15A,H15B), C16(H16A,H16B), C8(H8A,H8B), C17(H17A,H17B),
 C20(H20A,H20B), C12(H12A,H12B), C14(H14A,H14B), C11(H11A,H11B), C18(H18A,H18B)
2.b Idealised Me refined as rotating group:
 C33(H33A,H33B,H33C), C25(H25A,H25B,H25C), C37(H37A,H37B,H37C), C21(H21A,H21B,
 H21C), C29(H29A,H29B,H29C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_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 0.16099(3) 0.04614(3) 0.09922(2) 0.01311(9) Uani 1 1 d . . . . .
V2 V -0.00987(3) 0.18428(3) 0.03707(2) 0.01226(9) Uani 1 1 d . . . . .
V3 V -0.17181(3) -0.11789(3) 0.04715(2) 0.01253(9) Uani 1 1 d . . . . .
O5 O 0.14213(13) -0.10924(13) 0.04970(7) 0.0137(3) Uani 1 1 d . . . . .
O1 O 0.0000 0.0000 0.0000 0.0101(4) Uani 1 2 d S T P . .
O6 O -0.12630(14) -0.24421(12) 0.00878(8) 0.0135(3) Uani 1 1 d . . . . .
O7 O 0.26815(13) 0.13600(13) 0.04061(8) 0.0137(3) Uani 1 1 d . . . . .
O10 O -0.00817(13) -0.04613(12) 0.13319(7) 0.0121(3) Uani 1 1 d . . . . .
O9 O -0.14912(13) 0.06195(12) 0.08262(7) 0.0110(3) Uani 1 1 d . . . . .
O8 O 0.11934(13) 0.19669(12) 0.12424(7) 0.0114(3) Uani 1 1 d . . . . .
O4 O -0.28201(13) -0.18712(13) 0.09259(8) 0.0154(3) Uani 1 1 d . . . . .
O2 O 0.26452(14) 0.08732(13) 0.17632(8) 0.0166(3) Uani 1 1 d . . . . .
O3 O -0.01684(14) 0.31373(13) 0.07570(8) 0.0150(3) Uani 1 1 d . . . . .
N1 N 0.32685(16) 0.64451(15) 0.03973(9) 0.0126(4) Uani 1 1 d . . . . .
O12 O -0.05427(17) 0.28864(15) 0.29486(8) 0.0273(4) Uani 1 1 d . . . . .
C26 C 0.18658(19) 0.54677(18) -0.00754(11) 0.0140(4) Uani 1 1 d . . . . .
H26A H 0.1420 0.4846 0.0194 0.017 Uiso 1 1 calc R . . . .
H26B H 0.1359 0.5929 -0.0135 0.017 Uiso 1 1 calc R . . . .
C22 C 0.3995(2) 0.57351(19) 0.06555(11) 0.0136(4) Uani 1 1 d . . . . .
H22A H 0.3911 0.5079 0.0228 0.016 Uiso 1 1 calc R . . . .
H22B H 0.4943 0.6355 0.0840 0.016 Uiso 1 1 calc R . . . .
O11 O -0.0314(2) 0.13895(17) 0.34099(9) 0.0376(5) Uani 1 1 d . . . . .
C5 C -0.0348(2) 0.1849(2) 0.29149(12) 0.0162(5) Uani 1 1 d . . . . .
C32 C 0.4373(2) 0.87263(19) -0.08859(12) 0.0176(5) Uani 1 1 d . . . . .
H32A H 0.4165 0.9407 -0.0957 0.021 Uiso 1 1 calc R . . . .
H32B H 0.5312 0.9140 -0.0632 0.021 Uiso 1 1 calc R . . . .
C30 C 0.4119(2) 0.72907(19) -0.00428(12) 0.0143(4) Uani 1 1 d . . . . .
H30A H 0.4271 0.6746 -0.0435 0.017 Uiso 1 1 calc R . . . .
H30B H 0.4987 0.7919 0.0283 0.017 Uiso 1 1 calc R . . . .
C34 C 0.3099(2) 0.72761(19) 0.10578(11) 0.0152(4) Uani 1 1 d . . . . .
H34A H 0.2486 0.6705 0.1302 0.018 Uiso 1 1 calc R . . . .
H34B H 0.2687 0.7754 0.0876 0.018 Uiso 1 1 calc R . . . .
C2 C -0.1489(2) 0.10976(19) 0.15816(11) 0.0135(4) Uani 1 1 d . . . . .
H2A H -0.2285 0.0474 0.1699 0.016 Uiso 1 1 calc R . . . .
H2B H -0.1528 0.1906 0.1645 0.016 Uiso 1 1 calc R . . . .
C24 C 0.4421(2) 0.4542(2) 0.15163(12) 0.0189(5) Uani 1 1 d . . . . .
H24A H 0.3975 0.3933 0.1792 0.023 Uiso 1 1 calc R . . . .
H24B H 0.4563 0.4068 0.1085 0.023 Uiso 1 1 calc R . . . .
C35 C 0.4401(2) 0.82428(19) 0.16308(11) 0.0180(5) Uani 1 1 d . . . . .
H35A H 0.4945 0.8929 0.1424 0.022 Uiso 1 1 calc R . . . .
H35B H 0.4905 0.7803 0.1749 0.022 Uiso 1 1 calc R . . . .
C31 C 0.3513(2) 0.80191(19) -0.03895(12) 0.0152(5) Uani 1 1 d . . . . .
H31A H 0.3455 0.8645 -0.0001 0.018 Uiso 1 1 calc R . . . .
H31B H 0.2610 0.7410 -0.0682 0.018 Uiso 1 1 calc R . . . .
C1 C 0.1052(2) 0.23804(19) 0.19762(11) 0.0144(4) Uani 1 1 d . . . . .
H1A H 0.1008 0.3186 0.2038 0.017 Uiso 1 1 calc R . . . .
H1B H 0.1833 0.2546 0.2334 0.017 Uiso 1 1 calc R . . . .
C4 C -0.0231(2) 0.13365(19) 0.21262(11) 0.0137(4) Uani 1 1 d . . . . .
C33 C 0.4170(2) 0.7848(2) -0.16430(12) 0.0241(5) Uani 1 1 d . . . . .
H33A H 0.4707 0.8361 -0.1931 0.036 Uiso 1 1 calc GR . . . .
H33B H 0.3240 0.7420 -0.1895 0.036 Uiso 1 1 calc GR . . . .
H33C H 0.4437 0.7208 -0.1580 0.036 Uiso 1 1 calc GR . . . .
C3 C -0.0161(2) 0.00662(19) 0.20658(11) 0.0148(4) Uani 1 1 d . . . . .
H3A H 0.0621 0.0233 0.2423 0.018 Uiso 1 1 calc R . . . .
H3B H -0.0954 -0.0563 0.2184 0.018 Uiso 1 1 calc R . . . .
C25 C 0.5786(2) 0.5598(2) 0.20047(13) 0.0235(5) Uani 1 1 d . . . . .
H25A H 0.6241 0.6199 0.1734 0.035 Uiso 1 1 calc GR . . . .
H25B H 0.6317 0.5205 0.2146 0.035 Uiso 1 1 calc GR . . . .
H25C H 0.5657 0.6054 0.2442 0.035 Uiso 1 1 calc GR . . . .
C23 C 0.3501(2) 0.50766(19) 0.12563(12) 0.0154(5) Uani 1 1 d . . . . .
H23A H 0.2589 0.4372 0.1061 0.019 Uiso 1 1 calc R . . . .
H23B H 0.3502 0.5700 0.1673 0.019 Uiso 1 1 calc R . . . .
C28 C 0.0339(2) 0.3828(2) -0.12665(12) 0.0190(5) Uani 1 1 d . . . . .
H28A H -0.0114 0.3215 -0.0994 0.023 Uiso 1 1 calc R . . . .
H28B H -0.0108 0.4350 -0.1297 0.023 Uiso 1 1 calc R . . . .
C27 C 0.1806(2) 0.47163(19) -0.08433(11) 0.0156(5) Uani 1 1 d . . . . .
H27A H 0.2251 0.4197 -0.0795 0.019 Uiso 1 1 calc R . . . .
H27B H 0.2270 0.5321 -0.1117 0.019 Uiso 1 1 calc R . . . .
C6 C -0.0790(2) 0.3453(2) 0.36327(12) 0.0246(5) Uani 1 1 d . . . . .
H6A H -0.0054 0.3714 0.4050 0.030 Uiso 1 1 calc R . . . .
H6B H -0.1615 0.2833 0.3728 0.030 Uiso 1 1 calc R . . . .
C36 C 0.4116(2) 0.8837(2) 0.23395(12) 0.0267(6) Uani 1 1 d . . . . .
H36A H 0.3497 0.8147 0.2519 0.032 Uiso 1 1 calc R . . . .
H36B H 0.3694 0.9352 0.2231 0.032 Uiso 1 1 calc R . . . .
C7 C -0.0900(3) 0.4626(2) 0.35153(12) 0.0261(6) Uani 1 1 d . . . . .
H7A H -0.1588 0.4348 0.3069 0.031 Uiso 1 1 calc R . . . .
H7B H -0.0054 0.5239 0.3436 0.031 Uiso 1 1 calc R . . . .
C9 C -0.1342(3) 0.6497(2) 0.40136(13) 0.0266(6) Uani 1 1 d . . . . .
H9A H -0.0476 0.7118 0.3959 0.032 Uiso 1 1 calc R . . . .
H9B H -0.1986 0.6212 0.3548 0.032 Uiso 1 1 calc R . . . .
C10 C -0.1765(3) 0.7185(2) 0.46244(13) 0.0297(6) Uani 1 1 d . . . . .
H10A H -0.1128 0.7466 0.5092 0.036 Uiso 1 1 calc R . . . .
H10B H -0.2639 0.6572 0.4675 0.036 Uiso 1 1 calc R . . . .
C13 C -0.2310(3) 1.0254(2) 0.49212(14) 0.0316(6) Uani 1 1 d . . . . .
H13A H -0.1402 1.0880 0.4924 0.038 Uiso 1 1 calc R . . . .
H13B H -0.2864 1.0019 0.4431 0.038 Uiso 1 1 calc R . . . .
C19 C -0.3881(2) 1.5859(2) 0.61350(13) 0.0272(6) Uani 1 1 d . . . . .
H19A H -0.2945 1.6522 0.6265 0.033 Uiso 1 1 calc R . . . .
H19B H -0.4222 1.5700 0.5610 0.033 Uiso 1 1 calc R . . . .
C15 C -0.2801(3) 1.2137(2) 0.53556(14) 0.0313(6) Uani 1 1 d . . . . .
H15A H -0.1878 1.2762 0.5387 0.038 Uiso 1 1 calc R . . . .
H15B H -0.3308 1.1925 0.4855 0.038 Uiso 1 1 calc R . . . .
C16 C -0.3368(3) 1.2777(2) 0.58977(15) 0.0336(6) Uani 1 1 d . . . . .
H16A H -0.4302 1.2165 0.5852 0.040 Uiso 1 1 calc R . . . .
H16B H -0.2884 1.2960 0.6400 0.040 Uiso 1 1 calc R . . . .
C8 C -0.1243(3) 0.5320(2) 0.41602(13) 0.0271(6) Uani 1 1 d . . . . .
H8A H -0.0556 0.5607 0.4608 0.032 Uiso 1 1 calc R . . . .
H8B H -0.2092 0.4715 0.4241 0.032 Uiso 1 1 calc R . . . .
C17 C -0.3282(3) 1.4032(2) 0.57785(14) 0.0304(6) Uani 1 1 d . . . . .
H17A H -0.3689 1.3867 0.5263 0.036 Uiso 1 1 calc R . . . .
H17B H -0.2343 1.4671 0.5871 0.036 Uiso 1 1 calc R . . . .
C20 C -0.4666(3) 1.6376(2) 0.65767(14) 0.0318(6) Uani 1 1 d . . . . .
H20A H -0.5604 1.5719 0.6441 0.038 Uiso 1 1 calc R . . . .
H20B H -0.4334 1.6524 0.7101 0.038 Uiso 1 1 calc R . . . .
C12 C -0.2299(3) 0.9042(2) 0.50596(14) 0.0333(6) Uani 1 1 d . . . . .
H12A H -0.3197 0.8431 0.5080 0.040 Uiso 1 1 calc R . . . .
H12B H -0.1708 0.9284 0.5539 0.040 Uiso 1 1 calc R . . . .
C14 C -0.2831(3) 1.0902(2) 0.54874(15) 0.0347(6) Uani 1 1 d . . . . .
H14A H -0.2292 1.1117 0.5979 0.042 Uiso 1 1 calc R . . . .
H14B H -0.3747 1.0285 0.5474 0.042 Uiso 1 1 calc R . . . .
C11 C -0.1838(3) 0.8367(2) 0.44659(13) 0.0301(6) Uani 1 1 d . . . . .
H11A H -0.0957 0.8990 0.4429 0.036 Uiso 1 1 calc R . . . .
H11B H -0.2453 0.8089 0.3990 0.036 Uiso 1 1 calc R . . . .
C18 C -0.3964(3) 1.4606(2) 0.62694(14) 0.0295(6) Uani 1 1 d . . . . .
H18A H -0.3550 1.4784 0.6785 0.035 Uiso 1 1 calc R . . . .
H18B H -0.4902 1.3966 0.6182 0.035 Uiso 1 1 calc R . . . .
C37 C 0.5410(3) 0.9697(2) 0.29416(14) 0.0363(7) Uani 1 1 d . . . . .
H37A H 0.6004 1.0407 0.2775 0.054 Uiso 1 1 calc GR . . . .
H37B H 0.5838 0.9193 0.3042 0.054 Uiso 1 1 calc GR . . . .
H37C H 0.5200 1.0032 0.3386 0.054 Uiso 1 1 calc GR . . . .
C21 C -0.4563(3) 1.7632(3) 0.64492(14) 0.0409(7) Uani 1 1 d . . . . .
H21A H -0.4862 1.7503 0.5929 0.061 Uiso 1 1 calc GR . . . .
H21B H -0.3646 1.8308 0.6620 0.061 Uiso 1 1 calc GR . . . .
H21C H -0.5116 1.7878 0.6719 0.061 Uiso 1 1 calc GR . . . .
C29 C 0.0222(2) 0.3081(2) -0.20469(13) 0.0284(6) Uani 1 1 d . . . . .
H29A H 0.0622 0.3683 -0.2328 0.043 Uiso 1 1 calc GR . . . .
H29B H -0.0708 0.2511 -0.2285 0.043 Uiso 1 1 calc GR . . . .
H29C H 0.0680 0.2577 -0.2020 0.043 Uiso 1 1 calc GR . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
V1 V2 3.0253(5) 2 ?
V1 V3 3.0500(5) 2 ?
V1 O5 1.8108(13) . ?
V1 O1 2.2560(4) . ?
V1 O7 1.8673(14) . ?
V1 O10 2.0073(14) . ?
V1 O8 2.0379(13) . ?
V1 O2 1.6010(14) . ?
V2 V1 3.0253(5) 2 ?
V2 V3 3.0292(5) 2 ?
V2 O5 1.8487(14) 2 ?
V2 O1 2.2303(3) . ?
V2 O6 1.8012(14) 2 ?
V2 O9 2.0370(14) . ?
V2 O8 2.0134(14) . ?
V2 O3 1.6141(13) . ?
V3 V1 3.0500(5) 2 ?
V3 V2 3.0292(5) 2 ?
V3 O1 2.2509(4) . ?
V3 O6 1.8493(13) . ?
V3 O7 1.7968(14) 2 ?
V3 O10 2.0478(13) . ?
V3 O9 2.0065(13) . ?
V3 O4 1.6145(14) . ?
O5 V2 1.8488(14) 2 ?
O1 V1 2.2559(4) 2 ?
O1 V2 2.2303(3) 2 ?
O1 V3 2.2509(4) 2 ?
O6 V2 1.8012(14) 2 ?
O7 V3 1.7968(14) 2 ?
O10 C3 1.436(2) . ?
O9 C2 1.428(2) . ?
O8 C1 1.429(2) . ?
N1 C26 1.525(2) . ?
N1 C22 1.528(2) . ?
N1 C30 1.516(3) . ?
N1 C34 1.522(2) . ?
O12 C5 1.343(2) . ?
O12 C6 1.454(2) . ?
C26 H26A 0.9700 . ?
C26 H26B 0.9700 . ?
C26 C27 1.524(3) . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
C22 C23 1.526(3) . ?
O11 C5 1.178(3) . ?
C5 C4 1.539(3) . ?
C32 H32A 0.9700 . ?
C32 H32B 0.9700 . ?
C32 C31 1.531(3) . ?
C32 C33 1.522(3) . ?
C30 H30A 0.9700 . ?
C30 H30B 0.9700 . ?
C30 C31 1.522(3) . ?
C34 H34A 0.9700 . ?
C34 H34B 0.9700 . ?
C34 C35 1.526(3) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C2 C4 1.543(3) . ?
C24 H24A 0.9700 . ?
C24 H24B 0.9700 . ?
C24 C25 1.528(3) . ?
C24 C23 1.532(3) . ?
C35 H35A 0.9700 . ?
C35 H35B 0.9700 . ?
C35 C36 1.527(3) . ?
C31 H31A 0.9700 . ?
C31 H31B 0.9700 . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C1 C4 1.547(3) . ?
C4 C3 1.536(3) . ?
C33 H33A 0.9600 . ?
C33 H33B 0.9600 . ?
C33 H33C 0.9600 . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C25 H25A 0.9600 . ?
C25 H25B 0.9600 . ?
C25 H25C 0.9600 . ?
C23 H23A 0.9700 . ?
C23 H23B 0.9700 . ?
C28 H28A 0.9700 . ?
C28 H28B 0.9700 . ?
C28 C27 1.533(3) . ?
C28 C29 1.522(3) . ?
C27 H27A 0.9700 . ?
C27 H27B 0.9700 . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C6 C7 1.516(3) . ?
C36 H36A 0.9700 . ?
C36 H36B 0.9700 . ?
C36 C37 1.528(3) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C7 C8 1.524(3) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C9 C10 1.531(3) . ?
C9 C8 1.533(3) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C10 C11 1.533(3) . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C13 C12 1.525(3) . ?
C13 C14 1.524(3) . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C19 C20 1.529(3) . ?
C19 C18 1.530(3) . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C15 C16 1.528(3) . ?
C15 C14 1.529(3) . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C16 C17 1.521(3) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C17 C18 1.524(3) . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C20 C21 1.520(3) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C12 C11 1.529(3) . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
C37 H37A 0.9600 . ?
C37 H37B 0.9600 . ?
C37 H37C 0.9600 . ?
C21 H21A 0.9600 . ?
C21 H21B 0.9600 . ?
C21 H21C 0.9600 . ?
C29 H29A 0.9600 . ?
C29 H29B 0.9600 . ?
C29 H29C 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
V2 V1 V3 65.852(12) 2 2 ?
O5 V1 V2 34.65(4) . 2 ?
O5 V1 V3 87.43(5) . 2 ?
O5 V1 O1 81.86(4) . . ?
O5 V1 O7 93.60(6) . . ?
O5 V1 O10 89.90(6) . . ?
O5 V1 O8 158.31(6) . . ?
O1 V1 V2 47.239(10) . 2 ?
O1 V1 V3 47.341(10) . 2 ?
O7 V1 V2 88.11(4) . 2 ?
O7 V1 V3 32.93(4) . 2 ?
O7 V1 O1 80.25(4) . . ?
O7 V1 O10 156.95(6) . . ?
O7 V1 O8 86.39(6) . . ?
O10 V1 V2 81.90(4) . 2 ?
O10 V1 V3 124.79(4) . 2 ?
O10 V1 O1 77.70(4) . . ?
O10 V1 O8 82.11(5) . . ?
O8 V1 V2 123.79(4) . 2 ?
O8 V1 V3 80.80(4) . 2 ?
O8 V1 O1 76.75(4) . . ?
O2 V1 V2 138.79(5) . 2 ?
O2 V1 V3 136.70(6) . 2 ?
O2 V1 O5 104.49(7) . . ?
O2 V1 O1 171.95(5) . . ?
O2 V1 O7 103.98(7) . . ?
O2 V1 O10 97.15(7) . . ?
O2 V1 O8 96.53(6) . . ?
V1 V2 V3 66.464(13) 2 2 ?
O5 V2 V1 33.84(4) 2 2 ?
O5 V2 V3 89.37(4) 2 2 ?
O5 V2 O1 81.77(4) 2 . ?
O5 V2 O9 86.65(6) 2 . ?
O5 V2 O8 158.62(6) 2 . ?
O1 V2 V1 47.957(10) . 2 ?
O1 V2 V3 47.758(10) . 2 ?
O6 V2 V1 87.84(4) 2 2 ?
O6 V2 V3 34.43(4) 2 2 ?
O6 V2 O5 94.31(6) 2 2 ?
O6 V2 O1 82.18(4) 2 . ?
O6 V2 O9 159.26(6) 2 . ?
O6 V2 O8 89.25(6) 2 . ?
O9 V2 V1 81.45(4) . 2 ?
O9 V2 V3 125.01(4) . 2 ?
O9 V2 O1 77.45(4) . . ?
O8 V2 V1 125.59(4) . 2 ?
O8 V2 V3 81.69(4) . 2 ?
O8 V2 O1 77.83(4) . . ?
O8 V2 O9 82.74(5) . . ?
O3 V2 V1 137.66(5) . 2 ?
O3 V2 V3 137.23(5) . 2 ?
O3 V2 O5 103.96(7) . 2 ?
O3 V2 O1 171.61(6) . . ?
O3 V2 O6 103.25(7) . 2 ?
O3 V2 O9 96.58(6) . . ?
O3 V2 O8 95.68(6) . . ?
V2 V3 V1 66.040(12) 2 2 ?
O1 V3 V1 47.480(10) . 2 ?
O1 V3 V2 47.183(10) . 2 ?
O6 V3 V1 88.58(5) . 2 ?
O6 V3 V2 33.42(4) . 2 ?
O6 V3 O1 80.59(4) . . ?
O6 V3 O10 86.78(6) . . ?
O6 V3 O9 157.30(6) . . ?
O7 V3 V1 34.40(4) 2 2 ?
O7 V3 V2 87.78(5) 2 2 ?
O7 V3 O1 81.86(5) 2 . ?
O7 V3 O6 94.19(6) 2 . ?
O7 V3 O10 158.42(6) 2 . ?
O7 V3 O9 88.83(6) 2 . ?
O10 V3 V1 124.26(4) . 2 ?
O10 V3 V2 81.19(4) . 2 ?
O10 V3 O1 77.02(4) . . ?
O9 V3 V1 81.26(4) . 2 ?
O9 V3 V2 124.56(4) . 2 ?
O9 V3 O1 77.58(4) . . ?
O9 V3 O10 82.37(5) . . ?
O4 V3 V1 139.04(5) . 2 ?
O4 V3 V2 136.70(5) . 2 ?
O4 V3 O1 171.57(5) . . ?
O4 V3 O6 103.52(7) . . ?
O4 V3 O7 104.95(7) . 2 ?
O4 V3 O10 95.73(6) . . ?
O4 V3 O9 97.38(6) . . ?
V1 O5 V2 111.51(7) . 2 ?
V1 O1 V1 180.0 2 . ?
V2 O1 V1 95.195(14) 2 2 ?
V2 O1 V1 95.196(14) . . ?
V2 O1 V1 84.804(13) 2 . ?
V2 O1 V1 84.805(14) . 2 ?
V2 O1 V2 180.0 . 2 ?
V2 O1 V3 85.060(14) . 2 ?
V2 O1 V3 85.061(13) 2 . ?
V2 O1 V3 94.939(13) 2 2 ?
V2 O1 V3 94.940(13) . . ?
V3 O1 V1 94.821(14) . . ?
V3 O1 V1 85.180(14) . 2 ?
V3 O1 V1 94.821(14) 2 2 ?
V3 O1 V1 85.179(14) 2 . ?
V3 O1 V3 180.0 . 2 ?
V2 O6 V3 112.15(7) 2 . ?
V3 O7 V1 112.68(7) 2 . ?
V1 O10 V3 109.81(6) . . ?
C3 O10 V1 119.08(11) . . ?
C3 O10 V3 118.85(12) . . ?
V3 O9 V2 109.51(6) . . ?
C2 O9 V2 118.03(11) . . ?
C2 O9 V3 119.11(12) . . ?
V2 O8 V1 109.71(6) . . ?
C1 O8 V1 118.73(12) . . ?
C1 O8 V2 119.10(12) . . ?
C26 N1 C22 110.25(14) . . ?
C30 N1 C26 111.27(15) . . ?
C30 N1 C22 106.87(15) . . ?
C30 N1 C34 110.46(15) . . ?
C34 N1 C26 107.23(15) . . ?
C34 N1 C22 110.80(15) . . ?
C5 O12 C6 117.97(18) . . ?
N1 C26 H26A 108.3 . . ?
N1 C26 H26B 108.3 . . ?
H26A C26 H26B 107.4 . . ?
C27 C26 N1 115.88(17) . . ?
C27 C26 H26A 108.3 . . ?
C27 C26 H26B 108.3 . . ?
N1 C22 H22A 108.3 . . ?
N1 C22 H22B 108.3 . . ?
H22A C22 H22B 107.4 . . ?
C23 C22 N1 115.86(16) . . ?
C23 C22 H22A 108.3 . . ?
C23 C22 H22B 108.3 . . ?
O12 C5 C4 109.33(18) . . ?
O11 C5 O12 124.7(2) . . ?
O11 C5 C4 125.96(19) . . ?
H32A C32 H32B 107.6 . . ?
C31 C32 H32A 108.7 . . ?
C31 C32 H32B 108.7 . . ?
C33 C32 H32A 108.7 . . ?
C33 C32 H32B 108.7 . . ?
C33 C32 C31 114.10(17) . . ?
N1 C30 H30A 108.6 . . ?
N1 C30 H30B 108.6 . . ?
N1 C30 C31 114.70(16) . . ?
H30A C30 H30B 107.6 . . ?
C31 C30 H30A 108.6 . . ?
C31 C30 H30B 108.6 . . ?
N1 C34 H34A 108.6 . . ?
N1 C34 H34B 108.6 . . ?
N1 C34 C35 114.69(16) . . ?
H34A C34 H34B 107.6 . . ?
C35 C34 H34A 108.6 . . ?
C35 C34 H34B 108.6 . . ?
O9 C2 H2A 109.1 . . ?
O9 C2 H2B 109.1 . . ?
O9 C2 C4 112.36(16) . . ?
H2A C2 H2B 107.9 . . ?
C4 C2 H2A 109.1 . . ?
C4 C2 H2B 109.1 . . ?
H24A C24 H24B 107.7 . . ?
C25 C24 H24A 108.9 . . ?
C25 C24 H24B 108.9 . . ?
C25 C24 C23 113.42(17) . . ?
C23 C24 H24A 108.9 . . ?
C23 C24 H24B 108.9 . . ?
C34 C35 H35A 109.4 . . ?
C34 C35 H35B 109.4 . . ?
C34 C35 C36 111.15(18) . . ?
H35A C35 H35B 108.0 . . ?
C36 C35 H35A 109.4 . . ?
C36 C35 H35B 109.4 . . ?
C32 C31 H31A 109.5 . . ?
C32 C31 H31B 109.5 . . ?
C30 C31 C32 110.55(17) . . ?
C30 C31 H31A 109.5 . . ?
C30 C31 H31B 109.5 . . ?
H31A C31 H31B 108.1 . . ?
O8 C1 H1A 109.4 . . ?
O8 C1 H1B 109.4 . . ?
O8 C1 C4 111.09(15) . . ?
H1A C1 H1B 108.0 . . ?
C4 C1 H1A 109.4 . . ?
C4 C1 H1B 109.4 . . ?
C5 C4 C2 107.24(16) . . ?
C5 C4 C1 108.73(16) . . ?
C2 C4 C1 110.22(17) . . ?
C3 C4 C5 109.17(17) . . ?
C3 C4 C2 110.78(16) . . ?
C3 C4 C1 110.61(16) . . ?
C32 C33 H33A 109.5 . . ?
C32 C33 H33B 109.5 . . ?
C32 C33 H33C 109.5 . . ?
H33A C33 H33B 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
O10 C3 C4 110.99(16) . . ?
O10 C3 H3A 109.4 . . ?
O10 C3 H3B 109.4 . . ?
C4 C3 H3A 109.4 . . ?
C4 C3 H3B 109.4 . . ?
H3A C3 H3B 108.0 . . ?
C24 C25 H25A 109.5 . . ?
C24 C25 H25B 109.5 . . ?
C24 C25 H25C 109.5 . . ?
H25A C25 H25B 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C22 C23 C24 109.64(17) . . ?
C22 C23 H23A 109.7 . . ?
C22 C23 H23B 109.7 . . ?
C24 C23 H23A 109.7 . . ?
C24 C23 H23B 109.7 . . ?
H23A C23 H23B 108.2 . . ?
H28A C28 H28B 107.9 . . ?
C27 C28 H28A 109.2 . . ?
C27 C28 H28B 109.2 . . ?
C29 C28 H28A 109.2 . . ?
C29 C28 H28B 109.2 . . ?
C29 C28 C27 112.08(19) . . ?
C26 C27 C28 109.97(17) . . ?
C26 C27 H27A 109.7 . . ?
C26 C27 H27B 109.7 . . ?
C28 C27 H27A 109.7 . . ?
C28 C27 H27B 109.7 . . ?
H27A C27 H27B 108.2 . . ?
O12 C6 H6A 110.6 . . ?
O12 C6 H6B 110.6 . . ?
O12 C6 C7 105.65(18) . . ?
H6A C6 H6B 108.7 . . ?
C7 C6 H6A 110.6 . . ?
C7 C6 H6B 110.6 . . ?
C35 C36 H36A 109.4 . . ?
C35 C36 H36B 109.4 . . ?
C35 C36 C37 111.1(2) . . ?
H36A C36 H36B 108.0 . . ?
C37 C36 H36A 109.4 . . ?
C37 C36 H36B 109.4 . . ?
C6 C7 H7A 108.8 . . ?
C6 C7 H7B 108.8 . . ?
C6 C7 C8 113.9(2) . . ?
H7A C7 H7B 107.7 . . ?
C8 C7 H7A 108.8 . . ?
C8 C7 H7B 108.8 . . ?
H9A C9 H9B 107.6 . . ?
C10 C9 H9A 108.7 . . ?
C10 C9 H9B 108.7 . . ?
C10 C9 C8 114.0(2) . . ?
C8 C9 H9A 108.7 . . ?
C8 C9 H9B 108.7 . . ?
C9 C10 H10A 109.0 . . ?
C9 C10 H10B 109.0 . . ?
C9 C10 C11 112.7(2) . . ?
H10A C10 H10B 107.8 . . ?
C11 C10 H10A 109.0 . . ?
C11 C10 H10B 109.0 . . ?
H13A C13 H13B 107.6 . . ?
C12 C13 H13A 108.7 . . ?
C12 C13 H13B 108.7 . . ?
C14 C13 H13A 108.7 . . ?
C14 C13 H13B 108.7 . . ?
C14 C13 C12 114.1(2) . . ?
H19A C19 H19B 107.7 . . ?
C20 C19 H19A 108.8 . . ?
C20 C19 H19B 108.8 . . ?
C20 C19 C18 113.8(2) . . ?
C18 C19 H19A 108.8 . . ?
C18 C19 H19B 108.8 . . ?
H15A C15 H15B 107.6 . . ?
C16 C15 H15A 108.6 . . ?
C16 C15 H15B 108.6 . . ?
C16 C15 C14 114.8(2) . . ?
C14 C15 H15A 108.6 . . ?
C14 C15 H15B 108.6 . . ?
C15 C16 H16A 108.7 . . ?
C15 C16 H16B 108.7 . . ?
H16A C16 H16B 107.6 . . ?
C17 C16 C15 114.2(2) . . ?
C17 C16 H16A 108.7 . . ?
C17 C16 H16B 108.7 . . ?
C7 C8 C9 111.8(2) . . ?
C7 C8 H8A 109.3 . . ?
C7 C8 H8B 109.3 . . ?
C9 C8 H8A 109.3 . . ?
C9 C8 H8B 109.3 . . ?
H8A C8 H8B 107.9 . . ?
C16 C17 H17A 108.7 . . ?
C16 C17 H17B 108.7 . . ?
C16 C17 C18 114.3(2) . . ?
H17A C17 H17B 107.6 . . ?
C18 C17 H17A 108.7 . . ?
C18 C17 H17B 108.7 . . ?
C19 C20 H20A 108.9 . . ?
C19 C20 H20B 108.9 . . ?
H20A C20 H20B 107.7 . . ?
C21 C20 C19 113.6(2) . . ?
C21 C20 H20A 108.9 . . ?
C21 C20 H20B 108.9 . . ?
C13 C12 H12A 108.9 . . ?
C13 C12 H12B 108.9 . . ?
C13 C12 C11 113.5(2) . . ?
H12A C12 H12B 107.7 . . ?
C11 C12 H12A 108.9 . . ?
C11 C12 H12B 108.9 . . ?
C13 C14 C15 113.7(2) . . ?
C13 C14 H14A 108.8 . . ?
C13 C14 H14B 108.8 . . ?
C15 C14 H14A 108.8 . . ?
C15 C14 H14B 108.8 . . ?
H14A C14 H14B 107.7 . . ?
C10 C11 H11A 108.9 . . ?
C10 C11 H11B 108.9 . . ?
C12 C11 C10 113.4(2) . . ?
C12 C11 H11A 108.9 . . ?
C12 C11 H11B 108.9 . . ?
H11A C11 H11B 107.7 . . ?
C19 C18 H18A 108.9 . . ?
C19 C18 H18B 108.9 . . ?
C17 C18 C19 113.6(2) . . ?
C17 C18 H18A 108.9 . . ?
C17 C18 H18B 108.9 . . ?
H18A C18 H18B 107.7 . . ?
C36 C37 H37A 109.5 . . ?
C36 C37 H37B 109.5 . . ?
C36 C37 H37C 109.5 . . ?
H37A C37 H37B 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
C20 C21 H21A 109.5 . . ?
C20 C21 H21B 109.5 . . ?
C20 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C28 C29 H29A 109.5 . . ?
C28 C29 H29B 109.5 . . ?
C28 C29 H29C 109.5 . . ?
H29A C29 H29B 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 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 V3 O6 V2 45.58(6) 2 . . 2 ?
V1 O10 C3 C4 70.05(18) . . . . ?
V1 O8 C1 C4 -68.60(18) . . . . ?
V2 V1 O7 V3 45.42(6) 2 . . 2 ?
V2 O9 C2 C4 -68.22(18) . . . . ?
V2 O8 C1 C4 69.58(18) . . . . ?
V3 V1 O5 V2 -49.05(7) 2 . . 2 ?
V3 O10 C3 C4 -68.47(18) . . . . ?
V3 O9 C2 C4 68.63(19) . . . . ?
O5 V1 O7 V3 79.64(8) . . . 2 ?
O1 V1 O5 V2 -1.80(6) . . . 2 ?
O1 V1 O7 V3 -1.46(6) . . . 2 ?
O1 V3 O6 V2 -1.49(6) . . . 2 ?
O7 V1 O5 V2 -81.41(8) . . . 2 ?
O7 V3 O6 V2 79.54(8) 2 . . 2 ?
O10 V1 O5 V2 75.79(8) . . . 2 ?
O10 V1 O7 V3 -18.61(18) . . . 2 ?
O10 V3 O6 V2 -78.85(8) . . . 2 ?
O9 V3 O6 V2 -17.5(2) . . . 2 ?
O9 C2 C4 C5 179.88(16) . . . . ?
O9 C2 C4 C1 61.7(2) . . . . ?
O9 C2 C4 C3 -61.1(2) . . . . ?
O8 V1 O5 V2 7.9(2) . . . 2 ?
O8 V1 O7 V3 -78.62(7) . . . 2 ?
O8 C1 C4 C5 -178.59(16) . . . . ?
O8 C1 C4 C2 -61.3(2) . . . . ?
O8 C1 C4 C3 61.5(2) . . . . ?
O4 V3 O6 V2 -173.98(7) . . . 2 ?
O2 V1 O5 V2 173.14(8) . . . 2 ?
O2 V1 O7 V3 -174.46(7) . . . 2 ?
N1 C26 C27 C28 -177.10(16) . . . . ?
N1 C22 C23 C24 -173.73(16) . . . . ?
N1 C30 C31 C32 -174.06(16) . . . . ?
N1 C34 C35 C36 -168.68(17) . . . . ?
O12 C5 C4 C2 -53.9(2) . . . . ?
O12 C5 C4 C1 65.3(2) . . . . ?
O12 C5 C4 C3 -173.93(16) . . . . ?
O12 C6 C7 C8 176.65(19) . . . . ?
C26 N1 C22 C23 -72.8(2) . . . . ?
C26 N1 C30 C31 56.0(2) . . . . ?
C26 N1 C34 C35 175.12(17) . . . . ?
C22 N1 C26 C27 -71.0(2) . . . . ?
C22 N1 C30 C31 176.44(16) . . . . ?
C22 N1 C34 C35 54.8(2) . . . . ?
O11 C5 C4 C2 124.0(2) . . . . ?
O11 C5 C4 C1 -116.8(2) . . . . ?
O11 C5 C4 C3 4.0(3) . . . . ?
C5 O12 C6 C7 177.34(18) . . . . ?
C5 C4 C3 O10 178.70(16) . . . . ?
C30 N1 C26 C27 47.4(2) . . . . ?
C30 N1 C22 C23 166.19(16) . . . . ?
C30 N1 C34 C35 -63.5(2) . . . . ?
C34 N1 C26 C27 168.26(17) . . . . ?
C34 N1 C22 C23 45.8(2) . . . . ?
C34 N1 C30 C31 -63.0(2) . . . . ?
C34 C35 C36 C37 174.17(19) . . . . ?
C2 C4 C3 O10 60.8(2) . . . . ?
C1 C4 C3 O10 -61.7(2) . . . . ?
C33 C32 C31 C30 78.2(2) . . . . ?
C25 C24 C23 C22 73.9(2) . . . . ?
C6 O12 C5 O11 -2.9(3) . . . . ?
C6 O12 C5 C4 175.06(18) . . . . ?
C6 C7 C8 C9 180.0(2) . . . . ?
C9 C10 C11 C12 178.3(2) . . . . ?
C10 C9 C8 C7 176.6(2) . . . . ?
C13 C12 C11 C10 177.3(2) . . . . ?
C15 C16 C17 C18 174.5(2) . . . . ?
C16 C15 C14 C13 177.8(2) . . . . ?
C16 C17 C18 C19 -179.3(2) . . . . ?
C8 C9 C10 C11 179.3(2) . . . . ?
C20 C19 C18 C17 175.0(2) . . . . ?
C12 C13 C14 C15 178.4(2) . . . . ?
C14 C13 C12 C11 177.2(2) . . . . ?
C14 C15 C16 C17 177.8(2) . . . . ?
C18 C19 C20 C21 179.2(2) . . . . ?
C29 C28 C27 C26 178.45(18) . . . . ?

_shelx_SHELXL_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
