# 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_460
_database_code_depnum_ccdc_archive 'CCDC 1560286'
_audit_update_record             
;
2017-07-05 deposited with the CCDC.
2017-11-27 downloaded from the CCDC.
;
_audit_creation_date             2017-07-05
_audit_creation_method           
;
Olex2 1.2-beta
(compiled 2016.11.07 svn.r3352 for OlexSys, GUI svn.r5261)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C20 H28 N6 O23 V6, 2(C16 H36 N), 2(C2 H3 N)'
_chemical_formula_sum            'C56 H106 N10 O23 V6'
_chemical_formula_weight         1593.14
_chemical_melting_point          ?
_chemical_oxdiff_formula         'V O N C H'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
V V 0.0687 2.1097 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_cell_length_a                   10.4326(3)
_cell_length_b                   11.8963(3)
_cell_length_c                   16.2638(5)
_cell_angle_alpha                109.899(3)
_cell_angle_beta                 108.196(3)
_cell_angle_gamma                91.399(2)
_cell_volume                     1783.67(9)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    7451
_cell_measurement_temperature    173.00(10)
_cell_measurement_theta_max      76.5580
_cell_measurement_theta_min      5.5560
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    6.998
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.39340
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43f (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.483
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             834
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.13
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0341
_diffrn_reflns_av_unetI/netI     0.0459
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.967
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            12780
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.967
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.930
_diffrn_reflns_theta_min         3.995
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      173.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2137
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.967
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -67.00  28.00   1.00    1.00    --  -40.81  57.00  30.00   95
  2  ω     17.00 111.00   1.00    1.00    --   40.81  38.00-180.00   94
  3  ω     85.00 158.00   1.00    8.00    --  112.00  30.00-150.00   73
  4  ω    116.00 165.00   1.00    8.00    --  112.00  45.00-120.00   49
  5  ω    135.00 162.00   1.00    8.00    --  112.00  61.00 -60.00   27
  6  ω    114.00 169.00   1.00    8.00    --  112.00 125.00  60.00   55
  7  ω    102.00 129.00   1.00    8.00    --  112.00  45.00 -30.00   27
  8  ω     98.00 178.00   1.00    8.00    --  112.00  30.00 120.00   80
  9  ω     73.00 106.00   1.00    8.00    --  112.00 -95.00 120.00   33
 10  ω     71.00 121.00   1.00    8.00    --  112.00-125.00  60.00   50
 11  ω     40.00 132.00   1.00    8.00    --  112.00 -45.00 150.00   92
 12  ω     40.00 141.00   1.00    8.00    --  112.00 -61.00  30.00  101
 13  ω     64.00 108.00   1.00    8.00    --  112.00 -95.00-120.00   44
 14  ω     75.00 111.00   1.00    8.00    --  112.00-125.00-150.00   36
 15  ω     49.00  96.00   1.00    1.00    --   40.81-125.00-150.00   47
 16  ω     36.00 117.00   1.00    8.00    --  112.00 -30.00 -60.00   81
 17  ω     31.00  87.00   1.00    8.00    --  112.00 -95.00   0.00   56
 18  ω      8.00  60.00   1.00    1.00    --   40.81 -99.00  90.00   52
 19  ω   -113.00 -18.00   1.00    1.00    --  -40.81 -57.00-120.00   95
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0499487000
_diffrn_orient_matrix_UB_12      -0.1179321000
_diffrn_orient_matrix_UB_13      -0.0861540000
_diffrn_orient_matrix_UB_21      -0.0899335000
_diffrn_orient_matrix_UB_22      0.0681023000
_diffrn_orient_matrix_UB_23      -0.0560495000
_diffrn_orient_matrix_UB_31      0.1187748000
_diffrn_orient_matrix_UB_32      0.0289171000
_diffrn_orient_matrix_UB_33      -0.0303234000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6398
_reflns_number_total             7279
_reflns_odcompleteness_completeness 99.92
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     68.13
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_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    'olex2.solve (Bourhis et al., 2015)'
_refine_diff_density_max         0.870
_refine_diff_density_min         -0.662
_refine_diff_density_rms         0.097
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     436
_refine_ls_number_reflns         7279
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0643
_refine_ls_R_factor_gt           0.0580
_refine_ls_restrained_S_all      1.050
_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)+(0.1060P)²+1.3080P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1654
_refine_ls_wR_factor_ref         0.1729
_refine_special_details          ?
_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.a Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C2(H2A,H2B), C7(H7A,H7B), C6(H6A,H6B), C10(H10A,H10B), C21(H21A,
 H21B), C16(H16A,H16B), C17(H17A,H17B), C25(H25A,H25B), C22(H22A,H22B),
 C23(H23A,H23B), C15(H15A,H15B), C24(H24A,H24B), C14(H14A,H14B), C12(H12A,H12B),
  C20(H20A,H20B), C13(H13A,H13B)
2.b Aromatic/amide H refined with riding coordinates:
 C5(H5)
2.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C11(H11A,H11B,H11C), C19(H19A,H19B,H19C), C26(H26A,H26B,
 H26C), C18(H18A,H18B,H18C), C27(H27A,H27B,H27C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_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 0.44918(5) 0.30757(4) 0.48182(4) 0.03317(15) Uani 1 1 d . . . . .
V3 V 0.32273(5) 0.56196(5) 0.54386(4) 0.03276(15) Uani 1 1 d . . . . .
V2 V 0.39447(5) 0.47084(5) 0.34947(4) 0.03366(15) Uani 1 1 d . . . . .
O7 O 0.2444(2) 0.5147(2) 0.40526(15) 0.0346(4) Uani 1 1 d . . . . .
O10 O 0.1837(2) 0.5887(2) 0.56430(18) 0.0435(5) Uani 1 1 d . . . . .
O1 O -0.4672(4) 0.3719(4) 0.1082(2) 0.0736(9) Uani 1 1 d . . . . .
O2 O -0.4188(5) 0.3069(5) -0.0226(3) 0.1002(15) Uani 1 1 d . . . . .
O6 O 0.5000 0.5000 0.5000 0.0291(6) Uani 1 2 d S T P . .
O11 O 0.2897(2) 0.38089(19) 0.51018(15) 0.0338(4) Uani 1 1 d . . . . .
O5 O 0.3465(2) 0.30929(19) 0.35386(15) 0.0336(4) Uani 1 1 d . . . . .
O8 O 0.3991(2) 0.7052(2) 0.55318(18) 0.0398(5) Uani 1 1 d . . . . .
O4 O 0.4546(2) 0.6346(2) 0.39520(17) 0.0409(5) Uani 1 1 d . . . . .
O3 O 0.3005(3) 0.4420(2) 0.24338(17) 0.0463(6) Uani 1 1 d . . . . .
O9 O 0.4420(2) 0.5704(2) 0.65697(16) 0.0395(5) Uani 1 1 d . . . . .
O12 O 0.3923(2) 0.1697(2) 0.45979(18) 0.0423(5) Uani 1 1 d . . . . .
N3 N -0.1132(3) 0.2540(3) 0.2221(2) 0.0527(8) Uani 1 1 d . . . . .
N2 N -0.0809(4) 0.2108(4) 0.1441(3) 0.0666(10) Uani 1 1 d . . . . .
N1 N -0.1743(4) 0.2326(4) 0.0781(3) 0.0685(10) Uani 1 1 d . . . . .
C9 C 0.1117(3) 0.4444(3) 0.3559(2) 0.0383(6) Uani 1 1 d . . . . .
H9A H 0.0815 0.4413 0.2922 0.046 Uiso 1 1 calc R . . . .
H9B H 0.0477 0.4832 0.3847 0.046 Uiso 1 1 calc R . . . .
C4 C -0.2693(5) 0.2882(4) 0.1135(3) 0.0571(10) Uani 1 1 d . . . . .
C3 C -0.3910(5) 0.3232(4) 0.0573(3) 0.0630(11) Uani 1 1 d . . . . .
C8 C 0.1118(3) 0.3153(3) 0.3556(2) 0.0388(7) Uani 1 1 d . . . . .
C2 C -0.5876(7) 0.4197(5) 0.0662(5) 0.0826(15) Uani 1 1 d . . . . .
H2A H -0.6076 0.4833 0.1146 0.099 Uiso 1 1 calc R . . . .
H2B H -0.5689 0.4547 0.0245 0.099 Uiso 1 1 calc R . . . .
C1 C -0.7021(8) 0.3289(7) 0.0162(5) 0.103(2) Uani 1 1 d . . . . .
H1A H -0.6831 0.2664 -0.0324 0.155 Uiso 1 1 calc GR . . . .
H1B H -0.7792 0.3632 -0.0106 0.155 Uiso 1 1 calc GR . . . .
H1C H -0.7220 0.2953 0.0575 0.155 Uiso 1 1 calc GR . . . .
C5 C -0.2295(4) 0.3026(4) 0.2060(3) 0.0518(9) Uani 1 1 d . . . . .
H5 H -0.2733 0.3381 0.2481 0.062 Uiso 1 1 calc R . . . .
C7 C 0.2087(3) 0.2505(3) 0.3076(2) 0.0400(7) Uani 1 1 d . . . . .
H7A H 0.2045 0.1682 0.3058 0.048 Uiso 1 1 calc R . . . .
H7B H 0.1788 0.2472 0.2439 0.048 Uiso 1 1 calc R . . . .
C6 C -0.0328(3) 0.2420(4) 0.3074(3) 0.0466(8) Uani 1 1 d . . . . .
H6A H -0.0245 0.1572 0.2948 0.056 Uiso 1 1 calc R . . . .
H6B H -0.0822 0.2659 0.3508 0.056 Uiso 1 1 calc R . . . .
C10 C 0.1550(3) 0.3180(3) 0.4555(2) 0.0373(6) Uani 1 1 d . . . . .
H10A H 0.0913 0.3570 0.4845 0.045 Uiso 1 1 calc R . . . .
H10B H 0.1509 0.2358 0.4540 0.045 Uiso 1 1 calc R . . . .
N4 N 0.4432(3) 1.0992(3) 0.7029(2) 0.0405(6) Uani 1 1 d . . . . .
C11 C 0.1208(5) 0.9427(4) 0.4274(3) 0.0579(10) Uani 1 1 d . . . . .
H11A H 0.0627 0.8926 0.3659 0.087 Uiso 1 1 calc GR . . . .
H11B H 0.2018 0.9784 0.4242 0.087 Uiso 1 1 calc GR . . . .
H11C H 0.0734 1.0053 0.4542 0.087 Uiso 1 1 calc GR . . . .
C21 C 0.6630(4) 1.2522(4) 0.7874(3) 0.0535(9) Uani 1 1 d . . . . .
H21A H 0.6762 1.2262 0.8395 0.064 Uiso 1 1 calc R . . . .
H21B H 0.6172 1.3230 0.7982 0.064 Uiso 1 1 calc R . . . .
C16 C 0.5620(5) 0.9450(4) 0.7653(3) 0.0618(11) Uani 1 1 d . . . . .
H16A H 0.6540 0.9818 0.7791 0.074 Uiso 1 1 calc R . . . .
H16B H 0.5300 0.8871 0.7018 0.074 Uiso 1 1 calc R . . . .
C17 C 0.5625(5) 0.8795(4) 0.8329(3) 0.0629(11) Uani 1 1 d . . . . .
H17A H 0.4696 0.8457 0.8200 0.075 Uiso 1 1 calc R . . . .
H17B H 0.6146 0.8129 0.8214 0.075 Uiso 1 1 calc R . . . .
C19 C 0.8901(5) 1.3862(5) 0.8706(4) 0.0734(13) Uani 1 1 d . . . . .
H19A H 0.9761 1.4041 0.8645 0.110 Uiso 1 1 calc GR . . . .
H19B H 0.9049 1.3611 0.9226 0.110 Uiso 1 1 calc GR . . . .
H19C H 0.8460 1.4571 0.8803 0.110 Uiso 1 1 calc GR . . . .
C26 C 0.1420(6) 1.3626(5) 0.7486(5) 0.0805(16) Uani 1 1 d . . . . .
H26A H 0.0655 1.3076 0.6998 0.121 Uiso 1 1 calc GR . . . .
H26B H 0.1140 1.4397 0.7732 0.121 Uiso 1 1 calc GR . . . .
H26C H 0.1757 1.3313 0.7973 0.121 Uiso 1 1 calc GR . . . .
C25 C 0.2481(5) 1.3766(4) 0.7121(3) 0.0566(10) Uani 1 1 d . . . . .
H25A H 0.3248 1.4316 0.7626 0.068 Uiso 1 1 calc R . . . .
H25B H 0.2146 1.4144 0.6668 0.068 Uiso 1 1 calc R . . . .
C22 C 0.5745(4) 1.1529(3) 0.6994(3) 0.0429(7) Uani 1 1 d . . . . .
H22A H 0.6277 1.0883 0.6834 0.051 Uiso 1 1 calc R . . . .
H22B H 0.5509 1.1842 0.6496 0.051 Uiso 1 1 calc R . . . .
C23 C 0.3569(4) 1.1973(3) 0.7330(3) 0.0437(7) Uani 1 1 d . . . . .
H23A H 0.2814 1.1609 0.7427 0.052 Uiso 1 1 calc R . . . .
H23B H 0.4124 1.2576 0.7923 0.052 Uiso 1 1 calc R . . . .
C15 C 0.4703(4) 1.0407(3) 0.7753(3) 0.0463(8) Uani 1 1 d . . . . .
H15A H 0.5108 1.1034 0.8365 0.056 Uiso 1 1 calc R . . . .
H15B H 0.3836 1.0049 0.7724 0.056 Uiso 1 1 calc R . . . .
C24 C 0.3003(4) 1.2602(4) 0.6660(3) 0.0519(9) Uani 1 1 d . . . . .
H24A H 0.2260 1.2061 0.6128 0.062 Uiso 1 1 calc R . . . .
H24B H 0.3708 1.2797 0.6438 0.062 Uiso 1 1 calc R . . . .
C14 C 0.3686(4) 1.0079(3) 0.6051(2) 0.0426(7) Uani 1 1 d . . . . .
H14A H 0.3521 1.0503 0.5621 0.051 Uiso 1 1 calc R . . . .
H14B H 0.4285 0.9496 0.5889 0.051 Uiso 1 1 calc R . . . .
C18 C 0.6199(12) 0.9576(7) 0.9307(5) 0.147(4) Uani 1 1 d . . . . .
H18A H 0.7051 1.0027 0.9417 0.220 Uiso 1 1 calc GR . . . .
H18B H 0.6348 0.9091 0.9685 0.220 Uiso 1 1 calc GR . . . .
H18C H 0.5577 1.0124 0.9462 0.220 Uiso 1 1 calc GR . . . .
C12 C 0.1596(5) 0.8667(4) 0.4871(3) 0.0566(10) Uani 1 1 d . . . . .
H12A H 0.2171 0.8104 0.4639 0.068 Uiso 1 1 calc R . . . .
H12B H 0.0773 0.8197 0.4807 0.068 Uiso 1 1 calc R . . . .
C20 C 0.8003(4) 1.2853(4) 0.7824(3) 0.0587(10) Uani 1 1 d . . . . .
H20A H 0.7870 1.3105 0.7299 0.070 Uiso 1 1 calc R . . . .
H20B H 0.8463 1.2145 0.7720 0.070 Uiso 1 1 calc R . . . .
C13 C 0.2344(4) 0.9396(4) 0.5903(3) 0.0503(8) Uani 1 1 d . . . . .
H13A H 0.1777 0.9962 0.6144 0.060 Uiso 1 1 calc R . . . .
H13B H 0.2508 0.8854 0.6243 0.060 Uiso 1 1 calc R . . . .
N5 N -0.1187(7) -0.0713(5) 0.1924(5) 0.1004(18) Uani 1 1 d . . . . .
C28 C -0.0665(7) -0.0829(6) 0.1379(5) 0.0841(16) Uani 1 1 d . . . . .
C27 C -0.0031(10) -0.0980(9) 0.0686(7) 0.129(3) Uani 1 1 d . . . . .
H27A H -0.0645 -0.1509 0.0091 0.194 Uiso 1 1 calc GR . . . .
H27B H 0.0791 -0.1324 0.0849 0.194 Uiso 1 1 calc GR . . . .
H27C H 0.0184 -0.0209 0.0657 0.194 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 V3 3.0211(7) 2_666 ?
V1 V2 3.0347(8) 2_666 ?
V1 O6 2.2340(5) . ?
V1 O11 2.005(2) . ?
V1 O5 2.029(2) . ?
V1 O8 1.835(2) 2_666 ?
V1 O4 1.805(2) 2_666 ?
V1 O12 1.609(2) . ?
V3 V1 3.0211(7) 2_666 ?
V3 V2 3.0310(7) 2_666 ?
V3 O7 2.007(2) . ?
V3 O10 1.602(2) . ?
V3 O6 2.2372(5) . ?
V3 O11 2.025(2) . ?
V3 O8 1.801(2) . ?
V3 O9 1.839(2) . ?
V2 V1 3.0347(8) 2_666 ?
V2 V3 3.0310(7) 2_666 ?
V2 O7 2.037(2) . ?
V2 O6 2.2463(5) . ?
V2 O5 2.004(2) . ?
V2 O4 1.845(2) . ?
V2 O3 1.606(2) . ?
V2 O9 1.811(2) 2_666 ?
O7 C9 1.433(4) . ?
O1 C3 1.327(6) . ?
O1 C2 1.460(7) . ?
O2 C3 1.183(6) . ?
O6 V1 2.2340(5) 2_666 ?
O6 V3 2.2372(5) 2_666 ?
O6 V2 2.2463(5) 2_666 ?
O11 C10 1.428(4) . ?
O5 C7 1.428(4) . ?
O8 V1 1.835(2) 2_666 ?
O4 V1 1.805(2) 2_666 ?
O9 V2 1.811(2) 2_666 ?
N3 N2 1.349(5) . ?
N3 C5 1.346(6) . ?
N3 C6 1.437(5) . ?
N2 N1 1.310(6) . ?
N1 C4 1.371(6) . ?
C9 C8 1.534(5) . ?
C4 C3 1.477(7) . ?
C4 C5 1.376(6) . ?
C8 C7 1.531(4) . ?
C8 C6 1.544(4) . ?
C8 C10 1.533(5) . ?
C2 C1 1.409(9) . ?
N4 C22 1.522(4) . ?
N4 C23 1.533(4) . ?
N4 C15 1.521(5) . ?
N4 C14 1.525(4) . ?
C11 C12 1.515(6) . ?
C21 C22 1.506(5) . ?
C21 C20 1.510(5) . ?
C16 C17 1.548(6) . ?
C16 C15 1.504(6) . ?
C17 C18 1.456(8) . ?
C19 C20 1.520(7) . ?
C26 C25 1.441(7) . ?
C25 C24 1.537(5) . ?
C23 C24 1.507(5) . ?
C14 C13 1.510(5) . ?
C12 C13 1.528(6) . ?
N5 C28 1.150(8) . ?
C28 C27 1.439(10) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
V3 V1 V2 66.123(17) 2_666 2_666 ?
O6 V1 V3 47.537(13) . 2_666 ?
O6 V1 V2 47.534(14) . 2_666 ?
O11 V1 V3 124.90(6) . 2_666 ?
O11 V1 V2 81.63(6) . 2_666 ?
O11 V1 O6 77.59(6) . . ?
O11 V1 O5 82.21(9) . . ?
O5 V1 V3 81.55(6) . 2_666 ?
O5 V1 V2 124.75(6) . 2_666 ?
O5 V1 O6 77.43(6) . . ?
O8 V1 V3 33.46(7) 2_666 2_666 ?
O8 V1 V2 88.87(8) 2_666 2_666 ?
O8 V1 O6 80.97(7) 2_666 . ?
O8 V1 O11 157.53(10) 2_666 . ?
O8 V1 O5 86.67(10) 2_666 . ?
O4 V1 V3 87.59(8) 2_666 2_666 ?
O4 V1 V2 34.17(7) 2_666 2_666 ?
O4 V1 O6 81.69(8) 2_666 . ?
O4 V1 O11 89.18(10) 2_666 . ?
O4 V1 O5 158.68(10) 2_666 . ?
O4 V1 O8 94.34(11) 2_666 2_666 ?
O12 V1 V3 136.80(9) . 2_666 ?
O12 V1 V2 137.95(10) . 2_666 ?
O12 V1 O6 172.23(10) . . ?
O12 V1 O11 97.12(11) . . ?
O12 V1 O5 96.33(12) . . ?
O12 V1 O8 103.49(11) . 2_666 ?
O12 V1 O4 104.10(13) . 2_666 ?
V1 V3 V2 65.995(17) 2_666 2_666 ?
O7 V3 V1 81.78(6) . 2_666 ?
O7 V3 V2 125.30(6) . 2_666 ?
O7 V3 O6 77.91(6) . . ?
O7 V3 O11 82.35(9) . . ?
O10 V3 V1 138.51(10) . 2_666 ?
O10 V3 V2 136.59(10) . 2_666 ?
O10 V3 O7 96.89(12) . . ?
O10 V3 O6 171.94(9) . . ?
O10 V3 O11 96.21(11) . . ?
O10 V3 O8 104.69(12) . . ?
O10 V3 O9 103.23(12) . . ?
O6 V3 V1 47.449(13) . 2_666 ?
O6 V3 V2 47.592(14) . 2_666 ?
O11 V3 V1 124.34(6) . 2_666 ?
O11 V3 V2 81.42(6) . 2_666 ?
O11 V3 O6 77.11(6) . . ?
O8 V3 V1 34.18(7) . 2_666 ?
O8 V3 V2 87.10(8) . 2_666 ?
O8 V3 O7 89.53(11) . . ?
O8 V3 O6 81.60(7) . . ?
O8 V3 O11 158.36(10) . . ?
O8 V3 O9 93.47(11) . . ?
O9 V3 V1 88.62(7) . 2_666 ?
O9 V3 V2 33.56(7) . 2_666 ?
O9 V3 O7 158.16(10) . . ?
O9 V3 O6 81.14(7) . . ?
O9 V3 O11 87.06(10) . . ?
V3 V2 V1 65.831(17) 2_666 2_666 ?
O7 V2 V1 80.98(6) . 2_666 ?
O7 V2 V3 124.25(6) . 2_666 ?
O7 V2 O6 77.10(6) . . ?
O6 V2 V1 47.193(14) . 2_666 ?
O6 V2 V3 47.338(14) . 2_666 ?
O5 V2 V1 124.60(7) . 2_666 ?
O5 V2 V3 81.66(6) . 2_666 ?
O5 V2 O7 82.46(9) . . ?
O5 V2 O6 77.64(6) . . ?
O4 V2 V1 33.33(8) . 2_666 ?
O4 V2 V3 88.25(8) . 2_666 ?
O4 V2 O7 86.54(10) . . ?
O4 V2 O6 80.51(8) . . ?
O4 V2 O5 157.23(10) . . ?
O3 V2 V1 137.15(10) . 2_666 ?
O3 V2 V3 138.42(10) . 2_666 ?
O3 V2 O7 96.40(11) . . ?
O3 V2 O6 171.97(10) . . ?
O3 V2 O5 96.99(12) . . ?
O3 V2 O4 104.02(13) . . ?
O3 V2 O9 104.62(12) . 2_666 ?
O9 V2 V1 87.34(8) 2_666 2_666 ?
O9 V2 V3 34.14(7) 2_666 2_666 ?
O9 V2 O7 158.22(10) 2_666 . ?
O9 V2 O6 81.47(7) 2_666 . ?
O9 V2 O5 89.27(10) 2_666 . ?
O9 V2 O4 93.76(11) 2_666 . ?
V3 O7 V2 109.55(10) . . ?
C9 O7 V3 119.17(19) . . ?
C9 O7 V2 118.42(19) . . ?
C3 O1 C2 118.4(4) . . ?
V1 O6 V1 180.0 2_666 . ?
V1 O6 V3 85.014(19) 2_666 . ?
V1 O6 V3 94.986(19) 2_666 2_666 ?
V1 O6 V3 85.015(19) . 2_666 ?
V1 O6 V3 94.986(19) . . ?
V1 O6 V2 94.73(2) . . ?
V1 O6 V2 85.27(2) . 2_666 ?
V1 O6 V2 85.27(2) 2_666 . ?
V1 O6 V2 94.73(2) 2_666 2_666 ?
V3 O6 V3 180.0 2_666 . ?
V3 O6 V2 85.069(19) 2_666 . ?
V3 O6 V2 94.930(19) . . ?
V3 O6 V2 94.930(19) 2_666 2_666 ?
V3 O6 V2 85.070(19) . 2_666 ?
V2 O6 V2 180.0 2_666 . ?
V1 O11 V3 109.75(10) . . ?
C10 O11 V1 119.20(18) . . ?
C10 O11 V3 118.37(19) . . ?
V2 O5 V1 109.62(10) . . ?
C7 O5 V1 118.8(2) . . ?
C7 O5 V2 118.6(2) . . ?
V3 O8 V1 112.37(12) . 2_666 ?
V1 O4 V2 112.50(12) 2_666 . ?
V2 O9 V3 112.29(11) 2_666 . ?
N2 N3 C6 122.0(4) . . ?
C5 N3 N2 110.7(4) . . ?
C5 N3 C6 127.3(3) . . ?
N1 N2 N3 107.7(4) . . ?
N2 N1 C4 108.6(4) . . ?
O7 C9 C8 111.6(3) . . ?
N1 C4 C3 123.1(4) . . ?
N1 C4 C5 108.0(4) . . ?
C5 C4 C3 128.9(4) . . ?
O1 C3 C4 110.4(4) . . ?
O2 C3 O1 124.7(5) . . ?
O2 C3 C4 124.8(5) . . ?
C9 C8 C6 111.6(3) . . ?
C7 C8 C9 110.4(3) . . ?
C7 C8 C6 109.9(3) . . ?
C7 C8 C10 109.9(3) . . ?
C10 C8 C9 110.1(3) . . ?
C10 C8 C6 104.7(3) . . ?
C1 C2 O1 111.6(5) . . ?
N3 C5 C4 104.9(4) . . ?
O5 C7 C8 112.4(3) . . ?
N3 C6 C8 116.3(3) . . ?
O11 C10 C8 112.3(2) . . ?
C22 N4 C23 111.3(3) . . ?
C22 N4 C14 105.7(3) . . ?
C15 N4 C22 112.2(3) . . ?
C15 N4 C23 104.3(3) . . ?
C15 N4 C14 111.8(3) . . ?
C14 N4 C23 111.7(3) . . ?
C22 C21 C20 111.8(3) . . ?
C15 C16 C17 109.7(4) . . ?
C18 C17 C16 113.6(5) . . ?
C26 C25 C24 116.2(4) . . ?
C21 C22 N4 115.9(3) . . ?
C24 C23 N4 115.6(3) . . ?
C16 C15 N4 115.2(3) . . ?
C23 C24 C25 111.4(3) . . ?
C13 C14 N4 116.3(3) . . ?
C11 C12 C13 114.3(3) . . ?
C21 C20 C19 112.3(4) . . ?
C14 C13 C12 111.0(3) . . ?
N5 C28 C27 179.1(9) . . ?

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 O9 V2 -45.60(11) 2_666 . . 2_666 ?
V1 O11 C10 C8 -69.2(3) . . . . ?
V1 O5 C7 C8 68.3(3) . . . . ?
V3 V2 O4 V1 -45.64(12) 2_666 . . 2_666 ?
V3 O7 C9 C8 -69.2(3) . . . . ?
V3 O11 C10 C8 68.7(3) . . . . ?
V2 V3 O8 V1 49.42(12) 2_666 . . 2_666 ?
V2 O7 C9 C8 68.4(3) . . . . ?
V2 O5 C7 C8 -69.3(3) . . . . ?
O7 V3 O8 V1 -75.96(14) . . . 2_666 ?
O7 V3 O9 V2 18.0(3) . . . 2_666 ?
O7 V2 O4 V1 78.82(13) . . . 2_666 ?
O7 C9 C8 C7 -60.8(4) . . . . ?
O7 C9 C8 C6 176.6(3) . . . . ?
O7 C9 C8 C10 60.7(3) . . . . ?
O10 V3 O8 V1 -172.96(14) . . . 2_666 ?
O10 V3 O9 V2 174.58(13) . . . 2_666 ?
O6 V3 O8 V1 1.89(11) . . . 2_666 ?
O6 V3 O9 V2 1.49(10) . . . 2_666 ?
O6 V2 O4 V1 1.34(11) . . . 2_666 ?
O11 V3 O8 V1 -8.4(4) . . . 2_666 ?
O11 V3 O9 V2 78.89(13) . . . 2_666 ?
O5 V2 O4 V1 17.8(3) . . . 2_666 ?
O8 V3 O9 V2 -79.44(14) . . . 2_666 ?
O3 V2 O4 V1 174.56(13) . . . 2_666 ?
O9 V3 O8 V1 82.39(14) . . . 2_666 ?
O9 V2 O4 V1 -79.35(14) 2_666 . . 2_666 ?
N3 N2 N1 C4 -1.3(5) . . . . ?
N2 N3 C5 C4 -0.1(5) . . . . ?
N2 N3 C6 C8 67.9(5) . . . . ?
N2 N1 C4 C3 -178.5(4) . . . . ?
N2 N1 C4 C5 1.2(5) . . . . ?
N1 C4 C3 O1 178.2(4) . . . . ?
N1 C4 C3 O2 0.2(8) . . . . ?
N1 C4 C5 N3 -0.6(5) . . . . ?
C9 C8 C7 O5 61.2(4) . . . . ?
C9 C8 C6 N3 43.6(4) . . . . ?
C9 C8 C10 O11 -61.2(3) . . . . ?
C3 O1 C2 C1 85.9(7) . . . . ?
C3 C4 C5 N3 179.1(4) . . . . ?
C2 O1 C3 O2 -6.1(8) . . . . ?
C2 O1 C3 C4 175.9(4) . . . . ?
C5 N3 N2 N1 0.9(5) . . . . ?
C5 N3 C6 C8 -115.0(4) . . . . ?
C5 C4 C3 O1 -1.5(7) . . . . ?
C5 C4 C3 O2 -179.5(5) . . . . ?
C7 C8 C6 N3 -79.3(4) . . . . ?
C7 C8 C10 O11 60.6(3) . . . . ?
C6 N3 N2 N1 178.4(4) . . . . ?
C6 N3 C5 C4 -177.5(4) . . . . ?
C6 C8 C7 O5 -175.3(3) . . . . ?
C6 C8 C10 O11 178.7(3) . . . . ?
C10 C8 C7 O5 -60.5(4) . . . . ?
C10 C8 C6 N3 162.7(3) . . . . ?
N4 C23 C24 C25 -165.3(3) . . . . ?
N4 C14 C13 C12 170.9(3) . . . . ?
C11 C12 C13 C14 -62.5(5) . . . . ?
C17 C16 C15 N4 -171.1(4) . . . . ?
C26 C25 C24 C23 -59.2(6) . . . . ?
C22 N4 C23 C24 66.1(4) . . . . ?
C22 N4 C15 C16 -55.6(4) . . . . ?
C22 N4 C14 C13 179.0(3) . . . . ?
C22 C21 C20 C19 179.5(4) . . . . ?
C23 N4 C22 C21 55.0(4) . . . . ?
C23 N4 C15 C16 -176.2(4) . . . . ?
C23 N4 C14 C13 -59.8(4) . . . . ?
C15 N4 C22 C21 -61.5(4) . . . . ?
C15 N4 C23 C24 -172.7(3) . . . . ?
C15 N4 C14 C13 56.7(4) . . . . ?
C15 C16 C17 C18 -64.2(7) . . . . ?
C14 N4 C22 C21 176.4(3) . . . . ?
C14 N4 C23 C24 -51.8(4) . . . . ?
C14 N4 C15 C16 63.0(4) . . . . ?
C20 C21 C22 N4 170.7(3) . . . . ?

_shelx_SHELXL_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.018
_oxdiff_exptl_absorpt_empirical_full_min 0.695
####################################################################### 
# 
# 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_1543
_database_code_depnum_ccdc_archive 'CCDC 1571480'
_audit_update_record             
;
2017-08-30 deposited with the CCDC.
2017-11-27 downloaded from the CCDC.
;
_audit_creation_date             2017-08-18
_audit_creation_method           
;
Olex2 1.2-beta
(compiled 2016.11.07 svn.r3352 for OlexSys, GUI svn.r5261)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C26 H26 Cl2 N6 O19 V6, 2(C16 H36 N)'
_chemical_formula_sum            'C58 H98 Cl2 N8 O19 V6'
_chemical_formula_weight         1587.98
_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 0.0181 0.0091 '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'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
V V 0.0687 2.1097 '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 1 21/c 1'
_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                   10.2078(4)
_cell_length_b                   20.8402(10)
_cell_length_c                   16.9703(9)
_cell_angle_alpha                90
_cell_angle_beta                 91.971(4)
_cell_angle_gamma                90
_cell_volume                     3608.0(3)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    3509
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      72.8900
_cell_measurement_theta_min      4.8140
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    7.534
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.41614
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.27b (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.462
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1652
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.1
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0334
_diffrn_reflns_av_unetI/netI     0.0550
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.966
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            14858
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.966
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.631
_diffrn_reflns_theta_min         4.243
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2137
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.966
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -82.00  21.00   1.00    2.00    --  -40.81  19.00   0.00  103
  2  ω    -65.00   3.00   1.00    2.00    --  -40.81  38.00 -90.00   68
  3  ω    -30.00  72.00   1.00    2.00    --   40.81 -77.00  90.00  102
  4  ω     38.00 111.00   1.00   30.00    --  111.52 -45.00 -90.00   73
  5  ω     94.00 178.00   1.00   30.00    --  111.52  77.00-150.00   84
  6  ω     89.00 165.00   1.00   30.00    --  111.52  61.00  90.00   76
  7  ω     39.00 141.00   1.00   30.00    --  111.52 -61.00  90.00  102
  8  ω     53.00 102.00   1.00   30.00    --  111.52 -95.00-120.00   49
  9  ω     61.00 123.00   1.00   30.00    --  111.52 -30.00  30.00   62
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0334702000
_diffrn_orient_matrix_UB_12      -0.0344853000
_diffrn_orient_matrix_UB_13      -0.0771697000
_diffrn_orient_matrix_UB_21      0.1126107000
_diffrn_orient_matrix_UB_22      0.0478188000
_diffrn_orient_matrix_UB_23      -0.0120983000
_diffrn_orient_matrix_UB_31      0.0947173000
_diffrn_orient_matrix_UB_32      -0.0445824000
_diffrn_orient_matrix_UB_33      0.0464926000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4861
_reflns_number_total             7330
_reflns_odcompleteness_completeness 99.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     61.08
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.27b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.27b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.27b (Rigaku OD, 2015)'
_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         0.599
_refine_diff_density_min         -0.349
_refine_diff_density_rms         0.077
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     425
_refine_ls_number_reflns         7330
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0920
_refine_ls_R_factor_gt           0.0642
_refine_ls_restrained_S_all      1.014
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1273P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1821
_refine_ls_wR_factor_ref         0.2066
_refine_special_details          ?
_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
 C16, C17
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3.a Secondary CH2 refined with riding coordinates:
 C13(H13a,H13b), C12(H12a,H12b), C11(H11a,H11b), C9(H9a,H9b), C26(H26a,H26b),
 C25(H25a,H25b), C18(H18a,H18b), C17(H17a,H17b), C28(H28a,H28b), C24(H24a,H24b),
  C27(H27a,H27b), C23(H23a,H23b), C16(H16a,H16b), C15(H15a,H15b), C19(H19a,
 H19b), C20(H20a,H20b)
3.b Aromatic/amide H refined with riding coordinates:
 C8(H8), C5(H5), C6(H6), C2(H2), C3(H3)
3.c Idealised Me refined as rotating group:
 C29(H29a,H29b,H29c), C22(H22a,H22b,H22c), C14(H14a,H14b,H14c), C21(H21a,H21b,
 H21c)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_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 0.20234(6) 0.51584(4) 0.45954(5) 0.0665(2) Uani 1 1 d . . . . .
V2 V -0.03822(7) 0.45689(4) 0.38023(5) 0.0694(2) Uani 1 1 d . . . . .
V3 V 0.03694(7) 0.39863(4) 0.54023(5) 0.0673(2) Uani 1 1 d . . . . .
O7 O 0.0000 0.5000 0.5000 0.0570(8) Uani 1 2 d S T P . .
O2 O 0.0835(3) 0.45046(16) 0.63874(18) 0.0661(7) Uani 1 1 d . . . . .
O3 O 0.2163(2) 0.42805(15) 0.50930(18) 0.0634(7) Uani 1 1 d . . . . .
O1 O 0.2175(3) 0.54440(15) 0.57195(19) 0.0666(7) Uani 1 1 d . . . . .
O8 O 0.1332(3) 0.47692(18) 0.37103(18) 0.0745(8) Uani 1 1 d . . . . .
O5 O -0.0028(3) 0.38346(16) 0.4379(2) 0.0752(8) Uani 1 1 d . . . . .
O10 O 0.1371(3) 0.59379(16) 0.4332(2) 0.0752(8) Uani 1 1 d . . . . .
O4 O 0.0778(3) 0.32979(17) 0.5747(3) 0.0862(10) Uani 1 1 d . . . . .
O9 O 0.3543(3) 0.52263(19) 0.4421(2) 0.0837(10) Uani 1 1 d . . . . .
O6 O -0.0839(4) 0.4305(2) 0.2957(2) 0.0929(11) Uani 1 1 d . . . . .
N3 N 0.4916(4) 0.3732(2) 0.6907(3) 0.0806(11) Uani 1 1 d . . . . .
N4 N 0.0156(5) 0.2042(3) 0.3543(3) 0.0964(14) Uani 1 1 d . . . . .
C10 C 0.3251(4) 0.4526(2) 0.6363(3) 0.0694(11) Uani 1 1 d . . . . .
C13 C 0.3267(4) 0.4132(2) 0.5603(3) 0.0686(10) Uani 1 1 d . . . . .
H13A H 0.4068 0.4221 0.5331 0.082 Uiso 1 1 calc R . . . .
H13B H 0.3256 0.3679 0.5731 0.082 Uiso 1 1 calc R . . . .
N2 N 0.4275(5) 0.3299(3) 0.7318(3) 0.1052(17) Uani 1 1 d . . . . .
C12 C 0.2012(4) 0.4357(3) 0.6816(3) 0.0714(11) Uani 1 1 d . . . . .
H12A H 0.2023 0.3902 0.6939 0.086 Uiso 1 1 calc R . . . .
H12B H 0.2030 0.4591 0.7311 0.086 Uiso 1 1 calc R . . . .
C11 C 0.3280(4) 0.5239(2) 0.6196(3) 0.0722(11) Uani 1 1 d . . . . .
H11A H 0.3294 0.5471 0.6691 0.087 Uiso 1 1 calc R . . . .
H11B H 0.4077 0.5342 0.5928 0.087 Uiso 1 1 calc R . . . .
C9 C 0.4487(4) 0.4383(3) 0.6897(3) 0.0774(12) Uani 1 1 d . . . . .
H9A H 0.5200 0.4649 0.6724 0.093 Uiso 1 1 calc R . . . .
H9B H 0.4304 0.4509 0.7432 0.093 Uiso 1 1 calc R . . . .
N1 N 0.4876(5) 0.2739(3) 0.7211(4) 0.1056(17) Uani 1 1 d . . . . .
C7 C 0.5896(5) 0.2830(3) 0.6732(3) 0.0841(14) Uani 1 1 d . . . . .
C8 C 0.5927(4) 0.3467(3) 0.6539(3) 0.0806(13) Uani 1 1 d . . . . .
H8 H 0.6521 0.3672 0.6221 0.097 Uiso 1 1 calc R . . . .
C4 C 0.6766(5) 0.2306(3) 0.6517(3) 0.0868(14) Uani 1 1 d . . . . .
C5 C 0.7989(5) 0.2424(3) 0.6246(3) 0.0894(15) Uani 1 1 d . . . . .
H5 H 0.8258 0.2847 0.6184 0.107 Uiso 1 1 calc R . . . .
C1 C 0.8410(8) 0.1317(4) 0.6139(4) 0.111(2) Uani 1 1 d . . . . .
C6 C 0.8844(7) 0.1929(4) 0.6059(4) 0.109(2) Uani 1 1 d . . . . .
H6 H 0.9681 0.2015 0.5885 0.131 Uiso 1 1 calc R . . . .
C26 C -0.0867(7) 0.2404(3) 0.3985(4) 0.1055(19) Uani 1 1 d . . . . .
H26A H -0.1246 0.2111 0.4357 0.127 Uiso 1 1 calc R . . . .
H26B H -0.0425 0.2739 0.4289 0.127 Uiso 1 1 calc R . . . .
C2 C 0.7231(9) 0.1172(4) 0.6397(5) 0.123(2) Uani 1 1 d . . . . .
H2 H 0.6971 0.0747 0.6443 0.147 Uiso 1 1 calc R . . . .
C25 C -0.0413(9) 0.1499(4) 0.3101(5) 0.126(3) Uani 1 1 d . . . . .
H25A H 0.0306 0.1253 0.2895 0.151 Uiso 1 1 calc R . . . .
H25B H -0.0907 0.1672 0.2651 0.151 Uiso 1 1 calc R . . . .
C3 C 0.6377(7) 0.1678(3) 0.6600(5) 0.1057(19) Uani 1 1 d . . . . .
H3 H 0.5554 0.1585 0.6789 0.127 Uiso 1 1 calc R . . . .
C18 C 0.1114(8) 0.1787(4) 0.4192(5) 0.118(2) Uani 1 1 d . . . . .
H18A H 0.1494 0.2157 0.4460 0.142 Uiso 1 1 calc R . . . .
H18B H 0.0594 0.1563 0.4573 0.142 Uiso 1 1 calc R . . . .
C17 C 0.0953(8) 0.2422(5) 0.2964(5) 0.129(3) Uani 1 1 d . U . . .
H17A H 0.1459 0.2121 0.2662 0.155 Uiso 1 1 calc R . . . .
H17B H 0.0349 0.2637 0.2598 0.155 Uiso 1 1 calc R . . . .
C28 C -0.2987(8) 0.2988(4) 0.3994(7) 0.146(4) Uani 1 1 d . . . . .
H28A H -0.2578 0.3216 0.4436 0.176 Uiso 1 1 calc R . . . .
H28B H -0.3428 0.3306 0.3662 0.176 Uiso 1 1 calc R . . . .
C24 C -0.1295(10) 0.1038(5) 0.3516(6) 0.140(3) Uani 1 1 d . . . . .
H24A H -0.0804 0.0841 0.3952 0.168 Uiso 1 1 calc R . . . .
H24B H -0.2015 0.1276 0.3734 0.168 Uiso 1 1 calc R . . . .
C27 C -0.1923(9) 0.2696(5) 0.3532(6) 0.150(4) Uani 1 1 d . . . . .
H27A H -0.2311 0.2373 0.3185 0.180 Uiso 1 1 calc R . . . .
H27B H -0.1559 0.3027 0.3202 0.180 Uiso 1 1 calc R . . . .
C23 C -0.1828(15) 0.0533(5) 0.3000(7) 0.182(5) Uani 1 1 d . . . . .
H23A H -0.1116 0.0277 0.2804 0.218 Uiso 1 1 calc R . . . .
H23B H -0.2292 0.0726 0.2551 0.218 Uiso 1 1 calc R . . . .
C16 C 0.1876(9) 0.2916(5) 0.3313(7) 0.153(4) Uani 1 1 d . U . . .
H16A H 0.2613 0.2707 0.3582 0.183 Uiso 1 1 calc R . . . .
H16B H 0.1428 0.3178 0.3691 0.183 Uiso 1 1 calc R . . . .
C15 C 0.2364(10) 0.3340(5) 0.2632(9) 0.204(7) Uani 1 1 d . . . . .
H15A H 0.2689 0.3075 0.2211 0.245 Uiso 1 1 calc R . . . .
H15B H 0.1660 0.3608 0.2419 0.245 Uiso 1 1 calc R . . . .
C19 C 0.2207(10) 0.1358(6) 0.3994(6) 0.156(4) Uani 1 1 d . . . . .
H19A H 0.2682 0.1543 0.3564 0.187 Uiso 1 1 calc R . . . .
H19B H 0.1858 0.0947 0.3820 0.187 Uiso 1 1 calc R . . . .
C29 C -0.3928(13) 0.2590(9) 0.4285(8) 0.231(7) Uani 1 1 d . . . . .
H29A H -0.4102 0.2246 0.3919 0.346 Uiso 1 1 calc GR . . . .
H29B H -0.4718 0.2829 0.4358 0.346 Uiso 1 1 calc GR . . . .
H29C H -0.3621 0.2416 0.4782 0.346 Uiso 1 1 calc GR . . . .
C22 C -0.2756(13) 0.0104(6) 0.3437(10) 0.218(7) Uani 1 1 d . . . . .
H22A H -0.3002 -0.0255 0.3111 0.327 Uiso 1 1 calc GR . . . .
H22B H -0.3526 0.0343 0.3563 0.327 Uiso 1 1 calc GR . . . .
H22C H -0.2329 -0.0046 0.3915 0.327 Uiso 1 1 calc GR . . . .
C20 C 0.3199(13) 0.1251(9) 0.4744(8) 0.219(7) Uani 1 1 d . . . . .
H20A H 0.3612 0.1654 0.4894 0.262 Uiso 1 1 calc R . . . .
H20B H 0.2720 0.1094 0.5189 0.262 Uiso 1 1 calc R . . . .
C14 C 0.3478(11) 0.3756(6) 0.3001(9) 0.207(7) Uani 1 1 d . . . . .
H14A H 0.3752 0.4066 0.2623 0.310 Uiso 1 1 calc GR . . . .
H14B H 0.4207 0.3487 0.3154 0.310 Uiso 1 1 calc GR . . . .
H14C H 0.3167 0.3974 0.3457 0.310 Uiso 1 1 calc GR . . . .
C21 C 0.4245(18) 0.0761(11) 0.4522(13) 0.334(14) Uani 1 1 d . . . . .
H21A H 0.4721 0.0922 0.4085 0.501 Uiso 1 1 calc GR . . . .
H21B H 0.3830 0.0364 0.4376 0.501 Uiso 1 1 calc GR . . . .
H21C H 0.4839 0.0692 0.4964 0.501 Uiso 1 1 calc GR . . . .
Cl1 Cl 0.9446(3) 0.06856(14) 0.58816(16) 0.1634(11) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
V1 V2 3.0205(11) . ?
V1 V3 3.0238(10) 3_566 ?
V1 O7 2.2236(6) . ?
V1 O3 2.018(3) . ?
V1 O1 1.999(3) . ?
V1 O8 1.827(4) . ?
V1 O10 1.806(3) . ?
V1 O9 1.596(3) . ?
V2 V3 3.0482(12) . ?
V2 O7 2.2441(8) . ?
V2 O2 2.009(3) 3_566 ?
V2 O1 2.027(3) 3_566 ?
V2 O8 1.811(3) . ?
V2 O5 1.845(4) . ?
V2 O6 1.592(4) . ?
V3 V1 3.0238(10) 3_566 ?
V3 O7 2.2480(8) . ?
V3 O2 2.033(3) . ?
V3 O3 2.017(3) . ?
V3 O5 1.798(4) . ?
V3 O10 1.855(3) 3_566 ?
V3 O4 1.599(4) . ?
O7 V1 2.2235(6) 3_566 ?
O7 V2 2.2440(8) 3_566 ?
O7 V3 2.2480(8) 3_566 ?
O2 V2 2.009(3) 3_566 ?
O2 C12 1.417(5) . ?
O3 C13 1.431(5) . ?
O1 V2 2.027(3) 3_566 ?
O1 C11 1.430(5) . ?
O10 V3 1.855(3) 3_566 ?
N3 N2 1.326(6) . ?
N3 C9 1.425(7) . ?
N3 C8 1.344(6) . ?
N4 C26 1.507(7) . ?
N4 C25 1.467(9) . ?
N4 C18 1.541(9) . ?
N4 C17 1.520(9) . ?
C10 C13 1.529(7) . ?
C10 C12 1.543(5) . ?
C10 C11 1.513(7) . ?
C10 C9 1.556(6) . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
N2 N1 1.335(8) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
N1 C7 1.356(7) . ?
C7 C8 1.367(8) . ?
C7 C4 1.462(8) . ?
C8 H8 0.9300 . ?
C4 C5 1.368(8) . ?
C4 C3 1.377(9) . ?
C5 H5 0.9300 . ?
C5 C6 1.395(9) . ?
C1 C6 1.360(11) . ?
C1 C2 1.329(11) . ?
C1 Cl1 1.753(7) . ?
C6 H6 0.9300 . ?
C26 H26A 0.9700 . ?
C26 H26B 0.9700 . ?
C26 C27 1.438(10) . ?
C2 H2 0.9300 . ?
C2 C3 1.417(10) . ?
C25 H25A 0.9700 . ?
C25 H25B 0.9700 . ?
C25 C24 1.509(12) . ?
C3 H3 0.9300 . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
C18 C19 1.477(11) . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C17 C16 1.502(13) . ?
C28 H28A 0.9700 . ?
C28 H28B 0.9700 . ?
C28 C27 1.491(12) . ?
C28 C29 1.374(14) . ?
C24 H24A 0.9700 . ?
C24 H24B 0.9700 . ?
C24 C23 1.462(12) . ?
C27 H27A 0.9700 . ?
C27 H27B 0.9700 . ?
C23 H23A 0.9700 . ?
C23 H23B 0.9700 . ?
C23 C22 1.515(18) . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C16 C15 1.550(14) . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C15 C14 1.547(18) . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C19 C20 1.615(14) . ?
C29 H29A 0.9600 . ?
C29 H29B 0.9600 . ?
C29 H29C 0.9600 . ?
C22 H22A 0.9600 . ?
C22 H22B 0.9600 . ?
C22 H22C 0.9600 . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C20 C21 1.533(19) . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C21 H21A 0.9600 . ?
C21 H21B 0.9600 . ?
C21 H21C 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 66.17(3) . 3_566 ?
O7 V1 V2 47.751(19) . . ?
O7 V1 V3 47.792(19) . 3_566 ?
O3 V1 V2 82.08(9) . . ?
O3 V1 V3 125.38(7) . 3_566 ?
O3 V1 O7 77.81(7) . . ?
O1 V1 V2 125.53(8) . . ?
O1 V1 V3 81.90(9) . 3_566 ?
O1 V1 O7 77.97(8) . . ?
O1 V1 O3 82.45(13) . . ?
O8 V1 V2 33.71(9) . . ?
O8 V1 V3 88.49(10) . 3_566 ?
O8 V1 O7 81.45(9) . . ?
O8 V1 O3 87.77(15) . . ?
O8 V1 O1 158.66(12) . . ?
O10 V1 V2 88.20(11) . . ?
O10 V1 V3 34.85(9) . 3_566 ?
O10 V1 O7 82.63(9) . . ?
O10 V1 O3 159.92(12) . . ?
O10 V1 O1 89.10(16) . . ?
O10 V1 O8 93.85(17) . . ?
O9 V1 V2 137.22(15) . . ?
O9 V1 V3 137.60(14) . 3_566 ?
O9 V1 O7 171.85(14) . . ?
O9 V1 O3 95.93(15) . . ?
O9 V1 O1 96.16(17) . . ?
O9 V1 O8 103.71(17) . . ?
O9 V1 O10 103.09(17) . . ?
V1 V2 V3 65.75(3) . . ?
O7 V2 V1 47.18(2) . . ?
O7 V2 V3 47.32(2) . . ?
O2 V2 V1 81.92(9) 3_566 . ?
O2 V2 V3 125.10(10) 3_566 . ?
O2 V2 O7 78.00(9) 3_566 . ?
O2 V2 O1 82.60(12) 3_566 3_566 ?
O1 V2 V1 123.93(9) 3_566 . ?
O1 V2 V3 80.86(9) 3_566 . ?
O1 V2 O7 76.94(9) 3_566 . ?
O8 V2 V1 34.05(10) . . ?
O8 V2 V3 87.38(11) . . ?
O8 V2 O7 81.22(11) . . ?
O8 V2 O2 88.98(14) . 3_566 ?
O8 V2 O1 157.78(15) . 3_566 ?
O8 V2 O5 93.72(15) . . ?
O5 V2 V1 87.70(11) . . ?
O5 V2 V3 32.73(11) . . ?
O5 V2 O7 80.04(11) . . ?
O5 V2 O2 157.19(15) . 3_566 ?
O5 V2 O1 86.53(14) . 3_566 ?
O6 V2 V1 138.65(15) . . ?
O6 V2 V3 136.24(18) . . ?
O6 V2 O7 172.48(14) . . ?
O6 V2 O2 97.4(2) . 3_566 ?
O6 V2 O1 96.66(17) . 3_566 ?
O6 V2 O8 104.82(18) . . ?
O6 V2 O5 103.7(2) . . ?
V1 V3 V2 65.66(3) 3_566 . ?
O7 V3 V1 47.109(19) . 3_566 ?
O7 V3 V2 47.21(2) . . ?
O2 V3 V1 81.47(8) . 3_566 ?
O2 V3 V2 124.43(9) . . ?
O2 V3 O7 77.43(9) . . ?
O3 V3 V1 124.16(9) . 3_566 ?
O3 V3 V2 81.37(9) . . ?
O3 V3 O7 77.26(9) . . ?
O3 V3 O2 82.18(11) . . ?
O5 V3 V1 87.09(10) . 3_566 ?
O5 V3 V2 33.70(11) . . ?
O5 V3 O7 80.91(11) . . ?
O5 V3 O2 157.89(15) . . ?
O5 V3 O3 88.80(14) . . ?
O5 V3 O10 93.65(16) . 3_566 ?
O10 V3 V1 33.80(10) 3_566 3_566 ?
O10 V3 V2 88.23(11) 3_566 . ?
O10 V3 O7 80.90(10) 3_566 . ?
O10 V3 O2 87.33(14) 3_566 . ?
O10 V3 O3 157.36(14) 3_566 . ?
O4 V3 V1 136.80(13) . 3_566 ?
O4 V3 V2 137.51(17) . . ?
O4 V3 O7 173.24(15) . . ?
O4 V3 O2 97.21(19) . . ?
O4 V3 O3 98.06(15) . . ?
O4 V3 O5 104.0(2) . . ?
O4 V3 O10 103.15(16) . 3_566 ?
V1 O7 V1 180.0 3_566 . ?
V1 O7 V2 85.07(3) . . ?
V1 O7 V2 94.93(3) . 3_566 ?
V1 O7 V2 85.07(3) 3_566 3_566 ?
V1 O7 V2 94.93(3) 3_566 . ?
V1 O7 V3 85.10(3) 3_566 . ?
V1 O7 V3 85.10(3) . 3_566 ?
V1 O7 V3 94.90(3) 3_566 3_566 ?
V1 O7 V3 94.90(3) . . ?
V2 O7 V2 180.0 3_566 . ?
V2 O7 V3 94.53(3) 3_566 . ?
V2 O7 V3 94.53(3) . 3_566 ?
V2 O7 V3 85.47(3) 3_566 3_566 ?
V2 O7 V3 85.47(3) . . ?
V3 O7 V3 180.0 . 3_566 ?
V2 O2 V3 109.45(15) 3_566 . ?
C12 O2 V2 118.5(3) . 3_566 ?
C12 O2 V3 118.5(3) . . ?
V3 O3 V1 109.46(13) . . ?
C13 O3 V1 119.4(3) . . ?
C13 O3 V3 118.7(2) . . ?
V1 O1 V2 109.68(14) . 3_566 ?
C11 O1 V1 118.9(3) . . ?
C11 O1 V2 118.4(3) . 3_566 ?
V2 O8 V1 112.24(15) . . ?
V3 O5 V2 113.57(18) . . ?
V1 O10 V3 111.36(15) . 3_566 ?
N2 N3 C9 119.8(4) . . ?
N2 N3 C8 111.5(5) . . ?
C8 N3 C9 128.8(4) . . ?
C26 N4 C18 104.6(5) . . ?
C26 N4 C17 117.1(6) . . ?
C25 N4 C26 111.8(6) . . ?
C25 N4 C18 109.2(6) . . ?
C25 N4 C17 106.4(6) . . ?
C17 N4 C18 107.5(6) . . ?
C13 C10 C12 109.3(4) . . ?
C13 C10 C9 110.9(4) . . ?
C12 C10 C9 109.1(4) . . ?
C11 C10 C13 111.5(4) . . ?
C11 C10 C12 109.8(4) . . ?
C11 C10 C9 106.1(4) . . ?
O3 C13 C10 111.3(3) . . ?
O3 C13 H13A 109.4 . . ?
O3 C13 H13B 109.4 . . ?
C10 C13 H13A 109.4 . . ?
C10 C13 H13B 109.4 . . ?
H13A C13 H13B 108.0 . . ?
N3 N2 N1 106.6(4) . . ?
O2 C12 C10 113.0(3) . . ?
O2 C12 H12A 109.0 . . ?
O2 C12 H12B 109.0 . . ?
C10 C12 H12A 109.0 . . ?
C10 C12 H12B 109.0 . . ?
H12A C12 H12B 107.8 . . ?
O1 C11 C10 112.4(4) . . ?
O1 C11 H11A 109.1 . . ?
O1 C11 H11B 109.1 . . ?
C10 C11 H11A 109.1 . . ?
C10 C11 H11B 109.1 . . ?
H11A C11 H11B 107.9 . . ?
N3 C9 C10 115.6(4) . . ?
N3 C9 H9A 108.4 . . ?
N3 C9 H9B 108.4 . . ?
C10 C9 H9A 108.4 . . ?
C10 C9 H9B 108.4 . . ?
H9A C9 H9B 107.5 . . ?
N2 N1 C7 108.9(5) . . ?
N1 C7 C8 107.7(5) . . ?
N1 C7 C4 122.0(5) . . ?
C8 C7 C4 130.2(5) . . ?
N3 C8 C7 105.2(4) . . ?
N3 C8 H8 127.4 . . ?
C7 C8 H8 127.4 . . ?
C5 C4 C7 121.2(6) . . ?
C5 C4 C3 118.4(6) . . ?
C3 C4 C7 120.4(5) . . ?
C4 C5 H5 119.0 . . ?
C4 C5 C6 121.9(7) . . ?
C6 C5 H5 119.0 . . ?
C6 C1 Cl1 118.5(6) . . ?
C2 C1 C6 123.2(7) . . ?
C2 C1 Cl1 118.2(7) . . ?
C5 C6 H6 121.2 . . ?
C1 C6 C5 117.6(7) . . ?
C1 C6 H6 121.2 . . ?
N4 C26 H26A 107.9 . . ?
N4 C26 H26B 107.9 . . ?
H26A C26 H26B 107.2 . . ?
C27 C26 N4 117.8(7) . . ?
C27 C26 H26A 107.9 . . ?
C27 C26 H26B 107.9 . . ?
C1 C2 H2 120.6 . . ?
C1 C2 C3 118.9(8) . . ?
C3 C2 H2 120.6 . . ?
N4 C25 H25A 107.6 . . ?
N4 C25 H25B 107.6 . . ?
N4 C25 C24 119.0(7) . . ?
H25A C25 H25B 107.0 . . ?
C24 C25 H25A 107.6 . . ?
C24 C25 H25B 107.6 . . ?
C4 C3 C2 120.0(7) . . ?
C4 C3 H3 120.0 . . ?
C2 C3 H3 120.0 . . ?
N4 C18 H18A 107.1 . . ?
N4 C18 H18B 107.1 . . ?
H18A C18 H18B 106.8 . . ?
C19 C18 N4 120.9(7) . . ?
C19 C18 H18A 107.1 . . ?
C19 C18 H18B 107.1 . . ?
N4 C17 H17A 108.2 . . ?
N4 C17 H17B 108.2 . . ?
H17A C17 H17B 107.3 . . ?
C16 C17 N4 116.4(7) . . ?
C16 C17 H17A 108.2 . . ?
C16 C17 H17B 108.2 . . ?
H28A C28 H28B 107.1 . . ?
C27 C28 H28A 107.7 . . ?
C27 C28 H28B 107.7 . . ?
C29 C28 H28A 107.7 . . ?
C29 C28 H28B 107.7 . . ?
C29 C28 C27 118.3(11) . . ?
C25 C24 H24A 108.9 . . ?
C25 C24 H24B 108.9 . . ?
H24A C24 H24B 107.7 . . ?
C23 C24 C25 113.2(9) . . ?
C23 C24 H24A 108.9 . . ?
C23 C24 H24B 108.9 . . ?
C26 C27 C28 116.0(9) . . ?
C26 C27 H27A 108.3 . . ?
C26 C27 H27B 108.3 . . ?
C28 C27 H27A 108.3 . . ?
C28 C27 H27B 108.3 . . ?
H27A C27 H27B 107.4 . . ?
C24 C23 H23A 109.5 . . ?
C24 C23 H23B 109.5 . . ?
C24 C23 C22 110.9(11) . . ?
H23A C23 H23B 108.1 . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
C17 C16 H16A 110.1 . . ?
C17 C16 H16B 110.1 . . ?
C17 C16 C15 108.1(11) . . ?
H16A C16 H16B 108.4 . . ?
C15 C16 H16A 110.1 . . ?
C15 C16 H16B 110.1 . . ?
C16 C15 H15A 110.6 . . ?
C16 C15 H15B 110.6 . . ?
H15A C15 H15B 108.8 . . ?
C14 C15 C16 105.6(12) . . ?
C14 C15 H15A 110.6 . . ?
C14 C15 H15B 110.6 . . ?
C18 C19 H19A 109.4 . . ?
C18 C19 H19B 109.4 . . ?
C18 C19 C20 111.3(9) . . ?
H19A C19 H19B 108.0 . . ?
C20 C19 H19A 109.4 . . ?
C20 C19 H19B 109.4 . . ?
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 . . ?
C23 C22 H22A 109.5 . . ?
C23 C22 H22B 109.5 . . ?
C23 C22 H22C 109.5 . . ?
H22A C22 H22B 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C19 C20 H20A 109.9 . . ?
C19 C20 H20B 109.9 . . ?
H20A C20 H20B 108.3 . . ?
C21 C20 C19 108.7(14) . . ?
C21 C20 H20A 109.9 . . ?
C21 C20 H20B 109.9 . . ?
C15 C14 H14A 109.5 . . ?
C15 C14 H14B 109.5 . . ?
C15 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 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 . . ?

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 V3 45.75(15) . . . . ?
V1 V3 O5 V2 48.11(15) 3_566 . . . ?
V1 O3 C13 C10 67.2(4) . . . . ?
V1 O1 C11 C10 -68.4(4) . . . . ?
V2 V1 O10 V3 48.54(17) . . . 3_566 ?
V2 O2 C12 C10 -68.5(5) 3_566 . . . ?
V2 O1 C11 C10 69.0(4) 3_566 . . . ?
V3 V1 O8 V2 -46.47(17) 3_566 . . . ?
V3 V2 O8 V1 -48.20(17) . . . . ?
V3 O2 C12 C10 68.0(5) . . . . ?
V3 O3 C13 C10 -70.9(4) . . . . ?
O7 V1 O8 V2 1.02(16) . . . . ?
O7 V1 O10 V3 0.93(16) . . . 3_566 ?
O7 V2 O8 V1 -1.01(15) . . . . ?
O7 V2 O5 V3 -1.12(13) . . . . ?
O7 V3 O5 V2 1.12(13) . . . . ?
O2 V2 O8 V1 77.00(19) 3_566 . . . ?
O2 V2 O5 V3 -17.0(4) 3_566 . . . ?
O2 V3 O5 V2 -10.6(4) . . . . ?
O3 V1 O8 V2 79.03(18) . . . . ?
O3 V1 O10 V3 -12.3(6) . . . 3_566 ?
O3 V3 O5 V2 -76.18(17) . . . . ?
O1 V1 O8 V2 16.5(5) . . . . ?
O1 V1 O10 V3 -77.05(19) . . . 3_566 ?
O1 V2 O8 V1 9.6(5) 3_566 . . . ?
O1 V2 O5 V3 -78.45(17) 3_566 . . . ?
O8 V1 O10 V3 81.8(2) . . . 3_566 ?
O8 V2 O5 V3 79.28(19) . . . . ?
O5 V2 O8 V1 -80.3(2) . . . . ?
O10 V1 O8 V2 -80.93(19) . . . . ?
O10 V3 O5 V2 81.29(18) 3_566 . . . ?
O4 V3 O5 V2 -174.18(17) . . . . ?
O9 V1 O8 V2 174.6(2) . . . . ?
O9 V1 O10 V3 -173.2(2) . . . 3_566 ?
O6 V2 O8 V1 174.4(2) . . . . ?
O6 V2 O5 V3 -174.47(19) . . . . ?
N3 N2 N1 C7 0.2(8) . . . . ?
N4 C26 C27 C28 173.7(7) . . . . ?
N4 C25 C24 C23 178.0(9) . . . . ?
N4 C18 C19 C20 170.8(9) . . . . ?
N4 C17 C16 C15 -168.3(7) . . . . ?
C13 C10 C12 O2 -61.6(5) . . . . ?
C13 C10 C11 O1 60.4(5) . . . . ?
C13 C10 C9 N3 -37.8(5) . . . . ?
N2 N3 C9 C10 -76.6(6) . . . . ?
N2 N3 C8 C7 0.6(7) . . . . ?
N2 N1 C7 C8 0.1(8) . . . . ?
N2 N1 C7 C4 178.6(6) . . . . ?
C12 C10 C13 O3 62.0(5) . . . . ?
C12 C10 C11 O1 -60.9(5) . . . . ?
C12 C10 C9 N3 82.8(5) . . . . ?
C11 C10 C13 O3 -59.6(4) . . . . ?
C11 C10 C12 O2 61.0(5) . . . . ?
C11 C10 C9 N3 -159.0(4) . . . . ?
C9 N3 N2 N1 179.1(5) . . . . ?
C9 N3 C8 C7 -179.0(5) . . . . ?
C9 C10 C13 O3 -177.6(3) . . . . ?
C9 C10 C12 O2 176.9(4) . . . . ?
C9 C10 C11 O1 -178.7(4) . . . . ?
N1 C7 C8 N3 -0.4(7) . . . . ?
N1 C7 C4 C5 -159.8(6) . . . . ?
N1 C7 C4 C3 18.9(9) . . . . ?
C7 C4 C5 C6 178.2(6) . . . . ?
C7 C4 C3 C2 -179.4(7) . . . . ?
C8 N3 N2 N1 -0.5(7) . . . . ?
C8 N3 C9 C10 102.9(6) . . . . ?
C8 C7 C4 C5 18.3(10) . . . . ?
C8 C7 C4 C3 -163.0(7) . . . . ?
C4 C7 C8 N3 -178.7(6) . . . . ?
C4 C5 C6 C1 1.4(10) . . . . ?
C5 C4 C3 C2 -0.7(11) . . . . ?
C1 C2 C3 C4 1.0(12) . . . . ?
C6 C1 C2 C3 -0.1(13) . . . . ?
C26 N4 C25 C24 -49.4(11) . . . . ?
C26 N4 C18 C19 175.0(9) . . . . ?
C26 N4 C17 C16 67.5(10) . . . . ?
C2 C1 C6 C5 -1.1(12) . . . . ?
C25 N4 C26 C27 -61.2(10) . . . . ?
C25 N4 C18 C19 55.2(10) . . . . ?
C25 N4 C17 C16 -166.6(8) . . . . ?
C25 C24 C23 C22 -177.2(10) . . . . ?
C3 C4 C5 C6 -0.5(10) . . . . ?
C18 N4 C26 C27 -179.2(7) . . . . ?
C18 N4 C25 C24 65.8(9) . . . . ?
C18 N4 C17 C16 -49.8(10) . . . . ?
C18 C19 C20 C21 175.5(13) . . . . ?
C17 N4 C26 C27 62.0(10) . . . . ?
C17 N4 C25 C24 -178.5(8) . . . . ?
C17 N4 C18 C19 -59.8(11) . . . . ?
C17 C16 C15 C14 -170.5(8) . . . . ?
C29 C28 C27 C26 -80.2(14) . . . . ?
Cl1 C1 C6 C5 178.2(5) . . . . ?
Cl1 C1 C2 C3 -179.3(6) . . . . ?

_shelx_SHELXL_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.873
_oxdiff_exptl_absorpt_empirical_full_min 0.603
####################################################################### 
# 
# 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_1529
_database_code_depnum_ccdc_archive 'CCDC 1571479'
_audit_update_record             
;
2017-08-31 deposited with the CCDC.
2017-11-27 downloaded from the CCDC.
;
_audit_creation_date             2017-08-30
_audit_creation_method           
;
Olex2 1.2-beta
(compiled 2016.11.07 svn.r3352 for OlexSys, GUI svn.r5261)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C28 H32 N6 O19 V6, 2(C16 H36 N)'
_chemical_formula_sum            'C60 H104 N8 O19 V6'
_chemical_formula_weight         1547.15
_chemical_melting_point          ?
_chemical_oxdiff_formula         V6CHNO
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
V V 0.0687 2.1097 '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 1 21/c 1'
_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                   10.2063(5)
_cell_length_b                   21.4566(18)
_cell_length_c                   16.8058(12)
_cell_angle_alpha                90
_cell_angle_beta                 91.666(5)
_cell_angle_gamma                90
_cell_volume                     3678.8(4)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    3924
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      74.9290
_cell_measurement_theta_min      4.7820
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    6.721
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.56099
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43f (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.397
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1620
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.25
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0316
_diffrn_reflns_av_unetI/netI     0.0571
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.971
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            14987
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.549
_diffrn_reflns_theta_min         4.121
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2137
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -115.00 -18.00   1.00    1.00    --  -40.81 -38.00  90.00   97
  2  ω      6.00  33.00   1.00    1.00    --  -40.81  38.00 150.00   27
  3  ω    -96.00  -8.00   1.00    1.00    --  -40.81 125.00  30.00   88
  4  ω     24.00  80.00   1.00    1.00    --   40.81-125.00 -30.00   56
  5  ω     88.00 114.00   1.00   15.00    --  110.27  45.00 -60.00   26
  6  ω     37.00 137.00   1.00   15.00    --  110.27 -30.00 120.00  100
  7  ω     37.00 131.00   1.00   15.00    --  110.27 -45.00 -90.00   94
  8  ω     98.00 143.00   1.00   15.00    --  110.27 125.00-180.00   45
  9  ω    113.00 174.00   1.00   15.00    --  110.27  45.00  90.00   61
 10  ω    127.00 178.00   1.00   15.00    --  110.27  45.00 -60.00   51
 11  ω     97.00 161.00   1.00   15.00    --  110.27  45.00   0.00   64
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0708099000
_diffrn_orient_matrix_UB_12      0.0551405000
_diffrn_orient_matrix_UB_13      0.0414040000
_diffrn_orient_matrix_UB_21      -0.0775739000
_diffrn_orient_matrix_UB_22      -0.0119380000
_diffrn_orient_matrix_UB_23      0.0758045000
_diffrn_orient_matrix_UB_31      0.1086439000
_diffrn_orient_matrix_UB_32      -0.0443649000
_diffrn_orient_matrix_UB_33      0.0307186000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5029
_reflns_number_total             7404
_reflns_odcompleteness_completeness 99.90
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_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    ?
_refine_diff_density_max         0.691
_refine_diff_density_min         -0.364
_refine_diff_density_rms         0.096
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.998
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     439
_refine_ls_number_reflns         7404
_refine_ls_number_restraints     42
_refine_ls_R_factor_all          0.1006
_refine_ls_R_factor_gt           0.0774
_refine_ls_restrained_S_all      1.009
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1750P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2241
_refine_ls_wR_factor_ref         0.2525
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, 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
 C30A-C29 = C29-C30B = C28-C29
 1.54 with sigma of 0.02
 C29-C30B = C30A-C29 = C28-C29 = C28-C27
 1.54 with sigma of 0.02
 C26-C25B = C25B-C24B = C24B-C23B = C24A-C23A
 1.54 with sigma of 0.02
 C26-C25A = C24A-C25A
 1.54 with sigma of 0.02
 C26-C25B = C26-C25A = C24A-C25A = C25B-C24B = C24A-C23A = C24B-C23B
 1.54 with sigma of 0.02
 C30B-C28
 2.34 with sigma of 0.04
 C30A-C28
 2.34 with sigma of 0.04
 C29-C27
 2.34 with sigma of 0.04
 C25B-C23B
 2.34 with sigma of 0.04
 C23B-C25B
 2.34 with sigma of 0.04
 C24B-C26
 2.34 with sigma of 0.04
 C23A-C25A
 2.34 with sigma of 0.04
 C24A-C26
 2.34 with sigma of 0.04
3. Rigid bond restraints
 C28, C29, C30A, C30B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C25B, C25A, C24A, C24B, C23B, C23A, C26
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
Uanis(C30B) = Uanis(C30A)
Uanis(C25A) = Uanis(C25B)
Uanis(C24B) = Uanis(C24A)
Uanis(C23B) = Uanis(C23A)
5. Others
 Fixed Sof: H29A(0.75) H29B(0.75) H29C(0.25) H29D(0.25) H26A(0.75) H26B(0.75)
 H26C(0.25) H26D(0.25) C24B(0.75) H24A(0.75) H24B(0.75) C25B(0.75) H25A(0.75)
 H25B(0.75) C23B(0.75) H23A(0.75) H23B(0.75) H23C(0.75) C30A(0.75) H30A(0.75)
 H30B(0.75) H30C(0.75) C30B(0.25) H30D(0.25) H30E(0.25) H30F(0.25) C24A(0.25)
 H24C(0.25) H24D(0.25) C23A(0.25) H23D(0.25) H23E(0.25) H23F(0.25) C25A(0.25)
 H25C(0.25) H25D(0.25)
6.a Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C13(H13A,H13B), C10(H10A,H10B), C14(H14A,H14B), C19(H19A,
 H19B), C18(H18A,H18B), C27(H27A,H27B), C29(H29A,H29B), C29(H29C,H29D),
 C26(H26A,H26B), C26(H26C,H26D), C28(H28A,H28B), C20(H20A,H20B), C17(H17A,H17B),
  C24B(H24A,H24B), C21(H21A,H21B), C25B(H25A,H25B), C16(H16A,H16B), C24A(H24C,
 H24D), C25A(H25C,H25D)
6.b Me refined with riding coordinates:
 C30B(H30D,H30E,H30F)
6.c Aromatic/amide H refined with riding coordinates:
 C9(H9), C6(H6), C7(H7), C3(H3), C4(H4)
6.d Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C22(H22A,H22B,H22C), C23B(H23A,H23B,H23C), C15(H15A,H15B,
 H15C), C30A(H30A,H30B,H30C), C23A(H23D,H23E,H23F)
;
_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 1.20295(6) 0.51685(5) 0.46003(5) 0.0730(3) Uani 1 1 d . . . . .
V1 V 0.96328(7) 0.59953(4) 0.46451(5) 0.0741(3) Uani 1 1 d . . . . .
V3 V 0.96316(7) 0.46176(5) 0.37725(5) 0.0760(3) Uani 1 1 d . . . . .
O6 O 1.0000 0.5000 0.5000 0.0617(9) Uani 1 2 d S T P . .
O4 O 0.7837(3) 0.57018(16) 0.49412(18) 0.0691(7) Uani 1 1 d . . . . .
O2 O 0.9174(3) 0.55229(18) 0.36284(19) 0.0740(8) Uani 1 1 d . . . . .
O1 O 0.7831(3) 0.45909(17) 0.4246(2) 0.0736(8) Uani 1 1 d . . . . .
O8 O 1.1370(3) 0.59339(18) 0.4376(2) 0.0800(9) Uani 1 1 d . . . . .
O9 O 1.1343(3) 0.48224(19) 0.36856(19) 0.0798(9) Uani 1 1 d . . . . .
O7 O 1.0020(3) 0.61155(19) 0.5692(2) 0.0830(9) Uani 1 1 d . . . . .
O5 O 0.9223(4) 0.66754(19) 0.4336(3) 0.0946(11) Uani 1 1 d . . . . .
O3 O 0.9181(4) 0.4395(2) 0.2892(2) 0.0985(12) Uani 1 1 d . . . . .
O10 O 1.3556(3) 0.5243(2) 0.4428(2) 0.0903(11) Uani 1 1 d . . . . .
N3 N 0.5131(4) 0.6291(3) 0.3134(3) 0.0878(12) Uani 1 1 d . . . . .
C12 C 0.6767(4) 0.5500(3) 0.3651(3) 0.0741(12) Uani 1 1 d . . . . .
N4 N 0.9778(7) 0.7855(3) 0.6501(4) 0.118(2) Uani 1 1 d . . . . .
C11 C 0.6728(4) 0.5854(3) 0.4433(3) 0.0739(12) Uani 1 1 d . . . . .
H11A H 0.6724 0.6298 0.4326 0.089 Uiso 1 1 calc R . . . .
H11B H 0.5927 0.5752 0.4701 0.089 Uiso 1 1 calc R . . . .
N2 N 0.5773(5) 0.6718(3) 0.2739(4) 0.1107(19) Uani 1 1 d . . . . .
C13 C 0.6729(4) 0.4804(3) 0.3788(3) 0.0794(13) Uani 1 1 d . . . . .
H13A H 0.5934 0.4698 0.4061 0.095 Uiso 1 1 calc R . . . .
H13B H 0.6703 0.4592 0.3278 0.095 Uiso 1 1 calc R . . . .
C10 C 0.5528(4) 0.5654(3) 0.3123(3) 0.0851(15) Uani 1 1 d . . . . .
H10A H 0.5697 0.5538 0.2578 0.102 Uiso 1 1 calc R . . . .
H10B H 0.4806 0.5400 0.3299 0.102 Uiso 1 1 calc R . . . .
C14 C 0.7994(4) 0.5680(3) 0.3201(3) 0.0778(13) Uani 1 1 d . . . . .
H14A H 0.7979 0.5469 0.2690 0.093 Uiso 1 1 calc R . . . .
H14B H 0.7981 0.6125 0.3102 0.093 Uiso 1 1 calc R . . . .
N1 N 0.5189(5) 0.7255(3) 0.2849(4) 0.116(2) Uani 1 1 d . . . . .
C8 C 0.4152(5) 0.7168(3) 0.3327(4) 0.0888(15) Uani 1 1 d . . . . .
C9 C 0.4095(5) 0.6553(3) 0.3507(4) 0.0887(15) Uani 1 1 d . . . . .
H9 H 0.3483 0.6353 0.3816 0.106 Uiso 1 1 calc R . . . .
C6 C 0.2012(7) 0.7557(4) 0.3817(4) 0.1047(19) Uani 1 1 d . . . . .
H6 H 0.1740 0.7148 0.3895 0.126 Uiso 1 1 calc R . . . .
C5 C 0.3256(6) 0.7671(4) 0.3546(4) 0.0984(18) Uani 1 1 d . . . . .
C7 C 0.1168(8) 0.8042(5) 0.3975(4) 0.118(3) Uani 1 1 d . . . . .
H7 H 0.0330 0.7953 0.4146 0.142 Uiso 1 1 calc R . . . .
C19 C 1.0348(11) 0.8406(5) 0.6941(6) 0.144(3) Uani 1 1 d . . . . .
H19A H 0.9626 0.8645 0.7147 0.172 Uiso 1 1 calc R . . . .
H19B H 1.0852 0.8248 0.7397 0.172 Uiso 1 1 calc R . . . .
C2 C 0.1538(10) 0.8651(5) 0.3885(5) 0.137(3) Uani 1 1 d . . . . .
C18 C 0.8775(10) 0.8093(5) 0.5807(5) 0.139(3) Uani 1 1 d . . . . .
H18A H 0.9285 0.8306 0.5413 0.167 Uiso 1 1 calc R . . . .
H18B H 0.8397 0.7727 0.5551 0.167 Uiso 1 1 calc R . . . .
C27 C 1.0796(9) 0.7503(4) 0.6056(5) 0.125(3) Uani 1 1 d D . . . .
H27A H 1.0373 0.7165 0.5764 0.150 Uiso 1 1 calc R . . . .
H27B H 1.1181 0.7780 0.5672 0.150 Uiso 1 1 calc R . . . .
C29 C 1.2947(10) 0.6926(5) 0.6100(8) 0.156(4) Uani 1 1 d D U . . .
H29A H 1.3377 0.6623 0.6447 0.187 Uiso 0.75 1 calc R . . A 1
H29B H 1.2538 0.6697 0.5661 0.187 Uiso 0.75 1 calc R . . A 1
H29C H 1.2768 0.6485 0.6031 0.187 Uiso 0.25 1 calc R . . B 2
H29D H 1.3022 0.7116 0.5579 0.187 Uiso 0.25 1 calc R . . B 2
C3 C 0.2743(12) 0.8773(5) 0.3627(7) 0.151(4) Uani 1 1 d . . . . .
H3 H 0.3005 0.9185 0.3572 0.181 Uiso 1 1 calc R . . . .
C26 C 0.8960(10) 0.7497(5) 0.7096(6) 0.144(3) Uani 1 1 d D U . . .
H26A H 0.8439 0.7791 0.7390 0.173 Uiso 0.75 1 calc R . . C 1
H26B H 0.9546 0.7287 0.7474 0.173 Uiso 0.75 1 calc R . . C 1
H26C H 0.9433 0.7571 0.7596 0.173 Uiso 0.25 1 calc R . . D 2
H26D H 0.8176 0.7750 0.7123 0.173 Uiso 0.25 1 calc R . . D 2
C4 C 0.3635(9) 0.8283(4) 0.3434(6) 0.126(3) Uani 1 1 d . . . . .
H4 H 0.4455 0.8376 0.3237 0.151 Uiso 1 1 calc R . . . .
C28 C 1.1842(11) 0.7245(6) 0.6572(8) 0.180(5) Uani 1 1 d D U . . .
H28A H 1.1467 0.6942 0.6929 0.216 Uiso 1 1 calc R . . . .
H28B H 1.2222 0.7578 0.6895 0.216 Uiso 1 1 calc R . . . .
C20 C 1.1193(13) 0.8839(6) 0.6508(7) 0.159(4) Uani 1 1 d . . . . .
H20A H 1.0695 0.9018 0.6064 0.191 Uiso 1 1 calc R . . . .
H20B H 1.1923 0.8610 0.6295 0.191 Uiso 1 1 calc R . . . .
C17 C 0.7710(12) 0.8499(8) 0.6010(7) 0.189(6) Uani 1 1 d . . . . .
H17A H 0.8068 0.8883 0.6227 0.227 Uiso 1 1 calc R . . . .
H17B H 0.7206 0.8302 0.6422 0.227 Uiso 1 1 calc R . . . .
C1 C 0.0674(15) 0.9203(6) 0.4046(6) 0.201(7) Uani 1 1 d . . . . .
H1A H -0.0181 0.9133 0.3809 0.301 Uiso 1 1 calc GR . . . .
H1B H 0.1050 0.9571 0.3821 0.301 Uiso 1 1 calc GR . . . .
H1C H 0.0602 0.9257 0.4610 0.301 Uiso 1 1 calc GR . . . .
C24B C 0.7525(13) 0.6573(6) 0.7359(8) 0.156(5) Uani 0.75 1 d D U . E 1
H24A H 0.8240 0.6318 0.7570 0.187 Uiso 0.75 1 calc R . . E 1
H24B H 0.7194 0.6822 0.7790 0.187 Uiso 0.75 1 calc R . . E 1
C21 C 1.1706(18) 0.9347(6) 0.7023(9) 0.196(7) Uani 1 1 d . . . . .
H21A H 1.0977 0.9593 0.7208 0.235 Uiso 1 1 calc R . . . .
H21B H 1.2151 0.9167 0.7486 0.235 Uiso 1 1 calc R . . . .
C25B C 0.8020(11) 0.7000(5) 0.6696(7) 0.139(3) Uani 0.75 1 d D U . E 1
H25A H 0.7287 0.7205 0.6426 0.167 Uiso 0.75 1 calc R . . E 1
H25B H 0.8488 0.6757 0.6309 0.167 Uiso 0.75 1 calc R . . E 1
C16 C 0.6781(16) 0.8654(9) 0.5293(8) 0.226(8) Uani 1 1 d . . . . .
H16A H 0.6313 0.8282 0.5123 0.271 Uiso 1 1 calc R . . . .
H16B H 0.7290 0.8800 0.4851 0.271 Uiso 1 1 calc R . . . .
C22 C 1.2576(17) 0.9738(9) 0.6632(13) 0.250(10) Uani 1 1 d . . . . .
H22A H 1.3243 0.9492 0.6392 0.375 Uiso 1 1 calc GR . . . .
H22B H 1.2976 1.0022 0.7008 0.375 Uiso 1 1 calc GR . . . .
H22C H 1.2107 0.9970 0.6226 0.375 Uiso 1 1 calc GR . . . .
C23B C 0.6437(12) 0.6158(7) 0.7014(11) 0.176(6) Uani 0.75 1 d D U . E 1
H23A H 0.5709 0.6411 0.6841 0.265 Uiso 0.75 1 calc GR . . E 1
H23B H 0.6159 0.5872 0.7415 0.265 Uiso 0.75 1 calc GR . . E 1
H23C H 0.6759 0.5929 0.6570 0.265 Uiso 0.75 1 calc GR . . E 1
C15 C 0.576(2) 0.9178(13) 0.5531(13) 0.351(17) Uani 1 1 d . . . . .
H15A H 0.4992 0.8984 0.5736 0.527 Uiso 1 1 calc GR . . . .
H15B H 0.5521 0.9421 0.5070 0.527 Uiso 1 1 calc GR . . . .
H15C H 0.6152 0.9444 0.5931 0.527 Uiso 1 1 calc GR . . . .
C30A C 1.3956(16) 0.7330(11) 0.5776(11) 0.235(10) Uani 0.75 1 d D U . F 1
H30A H 1.3569 0.7718 0.5611 0.352 Uiso 0.75 1 calc GR . . F 1
H30B H 1.4336 0.7130 0.5326 0.352 Uiso 0.75 1 calc GR . . F 1
H30C H 1.4625 0.7405 0.6177 0.352 Uiso 0.75 1 calc GR . . F 1
C30B C 1.419(3) 0.703(3) 0.660(3) 0.235(10) Uani 0.25 1 d D U . F 2
H30D H 1.4917 0.6838 0.6339 0.352 Uiso 0.25 1 calc R . . F 2
H30E H 1.4347 0.7464 0.6663 0.352 Uiso 0.25 1 calc R . . F 2
H30F H 1.4095 0.6837 0.7113 0.352 Uiso 0.25 1 calc R . . F 2
C24A C 0.787(4) 0.6807(16) 0.8040(19) 0.156(5) Uani 0.25 1 d D U . E 2
H24C H 0.7355 0.7171 0.8174 0.187 Uiso 0.25 1 calc R . . E 2
H24D H 0.8528 0.6725 0.8452 0.187 Uiso 0.25 1 calc R . . E 2
C23A C 0.701(3) 0.6234(18) 0.784(3) 0.176(6) Uani 0.25 1 d D U . E 2
H23D H 0.6105 0.6355 0.7816 0.265 Uiso 0.25 1 calc GR . . E 2
H23E H 0.7141 0.5924 0.8251 0.265 Uiso 0.25 1 calc GR . . E 2
H23F H 0.7254 0.6064 0.7339 0.265 Uiso 0.25 1 calc GR . . E 2
C25A C 0.843(4) 0.6845(9) 0.7209(19) 0.139(3) Uani 0.25 1 d D U . E 2
H25C H 0.9126 0.6541 0.7157 0.167 Uiso 0.25 1 calc R . . E 2
H25D H 0.7752 0.6756 0.6809 0.167 Uiso 0.25 1 calc R . . E 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
V2 V1 3.0243(11) . ?
V2 V3 3.0207(12) . ?
V2 O6 2.2256(6) . ?
V2 O4 2.023(3) 3_766 ?
V2 O1 2.007(3) 3_766 ?
V2 O8 1.811(4) . ?
V2 O9 1.829(4) . ?
V2 O10 1.601(3) . ?
V1 V3 3.0412(13) 3_766 ?
V1 O6 2.2458(9) . ?
V1 O4 2.014(3) . ?
V1 O2 2.030(4) . ?
V1 O8 1.847(3) . ?
V1 O7 1.810(4) . ?
V1 O5 1.601(4) . ?
V3 V1 3.0413(13) 3_766 ?
V3 O6 2.2417(8) . ?
V3 O2 2.011(4) . ?
V3 O1 2.025(3) . ?
V3 O9 1.811(3) . ?
V3 O7 1.842(4) 3_766 ?
V3 O3 1.609(4) . ?
O6 V2 2.2256(6) 3_766 ?
O6 V1 2.2458(9) 3_766 ?
O6 V3 2.2417(8) 3_766 ?
O4 V2 2.023(3) 3_766 ?
O4 C11 1.436(5) . ?
O2 C14 1.424(6) . ?
O1 V2 2.007(3) 3_766 ?
O1 C13 1.419(6) . ?
O7 V3 1.842(4) 3_766 ?
N3 N2 1.317(7) . ?
N3 C10 1.426(8) . ?
N3 C9 1.365(7) . ?
C12 C11 1.520(7) . ?
C12 C13 1.512(8) . ?
C12 C10 1.559(6) . ?
C12 C14 1.531(6) . ?
N4 C19 1.502(12) . ?
N4 C18 1.612(12) . ?
N4 C27 1.501(9) . ?
N4 C26 1.529(11) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
N2 N1 1.312(9) . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
N1 C8 1.360(7) . ?
C8 C9 1.355(9) . ?
C8 C5 1.469(9) . ?
C9 H9 0.9300 . ?
C6 H6 0.9300 . ?
C6 C5 1.383(9) . ?
C6 C7 1.381(10) . ?
C5 C4 1.384(11) . ?
C7 H7 0.9300 . ?
C7 C2 1.369(14) . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C19 C20 1.476(15) . ?
C2 C3 1.341(15) . ?
C2 C1 1.506(12) . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
C18 C17 1.441(13) . ?
C27 H27A 0.9700 . ?
C27 H27B 0.9700 . ?
C27 C28 1.465(11) . ?
C29 H29A 0.9700 . ?
C29 H29B 0.9700 . ?
C29 H29C 0.9700 . ?
C29 H29D 0.9700 . ?
C29 C28 1.557(11) . ?
C29 C30A 1.463(12) . ?
C29 C30B 1.517(14) . ?
C3 H3 0.9300 . ?
C3 C4 1.433(13) . ?
C26 H26A 0.9700 . ?
C26 H26B 0.9700 . ?
C26 H26C 0.9700 . ?
C26 H26D 0.9700 . ?
C26 C25B 1.572(11) . ?
C26 C25A 1.514(14) . ?
C4 H4 0.9300 . ?
C28 H28A 0.9700 . ?
C28 H28B 0.9700 . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C20 C21 1.478(14) . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C17 C16 1.549(16) . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C24B H24A 0.9700 . ?
C24B H24B 0.9700 . ?
C24B C25B 1.539(11) . ?
C24B C23B 1.524(12) . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C21 C22 1.40(2) . ?
C25B H25A 0.9700 . ?
C25B H25B 0.9700 . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C16 C15 1.59(2) . ?
C22 H22A 0.9600 . ?
C22 H22B 0.9600 . ?
C22 H22C 0.9600 . ?
C23B H23A 0.9600 . ?
C23B H23B 0.9600 . ?
C23B H23C 0.9600 . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C30A H30A 0.9600 . ?
C30A H30B 0.9600 . ?
C30A H30C 0.9600 . ?
C30B H30D 0.9600 . ?
C30B H30E 0.9600 . ?
C30B H30F 0.9600 . ?
C24A H24C 0.9700 . ?
C24A H24D 0.9700 . ?
C24A C23A 1.538(14) . ?
C24A C25A 1.527(14) . ?
C23A H23D 0.9600 . ?
C23A H23E 0.9600 . ?
C23A H23F 0.9600 . ?
C25A H25C 0.9700 . ?
C25A H25D 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
V3 V2 V1 66.17(3) . . ?
O6 V2 V1 47.72(2) . . ?
O6 V2 V3 47.68(2) . . ?
O4 V2 V1 125.27(8) 3_766 . ?
O4 V2 V3 81.89(9) 3_766 . ?
O4 V2 O6 77.76(8) 3_766 . ?
O1 V2 V1 81.95(10) 3_766 . ?
O1 V2 V3 125.41(9) 3_766 . ?
O1 V2 O6 77.94(8) 3_766 . ?
O1 V2 O4 82.38(14) 3_766 3_766 ?
O8 V2 V1 34.61(9) . . ?
O8 V2 V3 88.14(12) . . ?
O8 V2 O6 82.33(10) . . ?
O8 V2 O4 159.57(13) . 3_766 ?
O8 V2 O1 89.06(17) . 3_766 ?
O8 V2 O9 93.56(18) . . ?
O9 V2 V1 88.20(11) . . ?
O9 V2 V3 33.71(9) . . ?
O9 V2 O6 81.39(9) . . ?
O9 V2 O4 88.00(16) . 3_766 ?
O9 V2 O1 158.63(13) . 3_766 ?
O10 V2 V1 137.58(16) . . ?
O10 V2 V3 137.32(17) . . ?
O10 V2 O6 171.88(15) . . ?
O10 V2 O4 96.06(17) . 3_766 ?
O10 V2 O1 96.14(18) . 3_766 ?
O10 V2 O8 103.30(18) . . ?
O10 V2 O9 103.85(19) . . ?
V2 V1 V3 65.72(3) . 3_766 ?
O6 V1 V2 47.16(2) . . ?
O6 V1 V3 47.28(2) . 3_766 ?
O4 V1 V2 124.42(10) . . ?
O4 V1 V3 81.49(9) . 3_766 ?
O4 V1 O6 77.47(10) . . ?
O4 V1 O2 82.10(13) . . ?
O2 V1 V2 81.56(9) . . ?
O2 V1 V3 124.42(11) . 3_766 ?
O2 V1 O6 77.37(10) . . ?
O8 V1 V2 33.84(11) . . ?
O8 V1 V3 88.23(11) . 3_766 ?
O8 V1 O6 80.99(12) . . ?
O8 V1 O4 157.68(16) . . ?
O8 V1 O2 87.58(15) . . ?
O7 V1 V2 87.36(11) . . ?
O7 V1 V3 33.95(13) . 3_766 ?
O7 V1 O6 81.22(13) . . ?
O7 V1 O4 88.79(15) . . ?
O7 V1 O2 158.09(17) . . ?
O7 V1 O8 93.69(17) . . ?
O5 V1 V2 136.94(14) . . ?
O5 V1 V3 137.19(19) . 3_766 ?
O5 V1 O6 173.30(16) . . ?
O5 V1 O4 97.70(17) . . ?
O5 V1 O2 97.5(2) . . ?
O5 V1 O8 103.25(18) . . ?
O5 V1 O7 103.5(2) . . ?
V2 V3 V1 65.82(3) . 3_766 ?
O6 V3 V2 47.23(2) . . ?
O6 V3 V1 47.39(2) . 3_766 ?
O2 V3 V2 81.93(10) . . ?
O2 V3 V1 125.00(10) . 3_766 ?
O2 V3 O6 77.84(10) . . ?
O2 V3 O1 82.21(13) . . ?
O1 V3 V2 124.23(10) . . ?
O1 V3 V1 81.25(10) . 3_766 ?
O1 V3 O6 77.20(10) . . ?
O9 V3 V2 34.09(11) . . ?
O9 V3 V1 87.78(11) . 3_766 ?
O9 V3 O6 81.32(12) . . ?
O9 V3 O2 88.68(16) . . ?
O9 V3 O1 157.99(16) . . ?
O9 V3 O7 94.22(17) . 3_766 ?
O7 V3 V2 88.09(12) 3_766 . ?
O7 V3 V1 33.28(12) 3_766 3_766 ?
O7 V3 O6 80.66(12) 3_766 . ?
O7 V3 O2 157.61(16) 3_766 . ?
O7 V3 O1 87.03(15) 3_766 . ?
O3 V3 V2 138.23(16) . . ?
O3 V3 V1 137.1(2) . 3_766 ?
O3 V3 O6 172.17(16) . . ?
O3 V3 O2 96.7(2) . . ?
O3 V3 O1 96.58(18) . . ?
O3 V3 O9 104.4(2) . . ?
O3 V3 O7 104.0(2) . 3_766 ?
V2 O6 V2 180.0 . 3_766 ?
V2 O6 V1 94.88(3) 3_766 . ?
V2 O6 V1 85.12(3) 3_766 3_766 ?
V2 O6 V1 94.88(3) . 3_766 ?
V2 O6 V1 85.12(3) . . ?
V2 O6 V3 94.91(3) . 3_766 ?
V2 O6 V3 85.09(3) . . ?
V2 O6 V3 85.09(3) 3_766 3_766 ?
V2 O6 V3 94.91(3) 3_766 . ?
V1 O6 V1 180.0 . 3_766 ?
V3 O6 V1 94.67(3) . . ?
V3 O6 V1 85.33(3) 3_766 . ?
V3 O6 V1 94.67(3) 3_766 3_766 ?
V3 O6 V1 85.33(3) . 3_766 ?
V3 O6 V3 180.0 3_766 . ?
V1 O4 V2 109.33(13) . 3_766 ?
C11 O4 V2 118.7(3) . 3_766 ?
C11 O4 V1 119.3(3) . . ?
V3 O2 V1 109.50(15) . . ?
C14 O2 V1 118.5(3) . . ?
C14 O2 V3 118.6(3) . . ?
V2 O1 V3 109.42(15) 3_766 . ?
C13 O1 V2 118.3(3) . 3_766 ?
C13 O1 V3 119.4(3) . . ?
V2 O8 V1 111.55(17) . . ?
V3 O9 V2 112.20(16) . . ?
V1 O7 V3 112.8(2) . 3_766 ?
N2 N3 C10 121.0(5) . . ?
N2 N3 C9 110.4(5) . . ?
C9 N3 C10 128.6(5) . . ?
C11 C12 C10 110.1(4) . . ?
C11 C12 C14 110.0(4) . . ?
C13 C12 C11 111.1(4) . . ?
C13 C12 C10 105.9(4) . . ?
C13 C12 C14 110.5(4) . . ?
C14 C12 C10 109.1(4) . . ?
C19 N4 C18 109.6(7) . . ?
C19 N4 C26 106.5(7) . . ?
C27 N4 C19 112.2(7) . . ?
C27 N4 C18 103.5(6) . . ?
C27 N4 C26 118.1(7) . . ?
C26 N4 C18 106.5(7) . . ?
O4 C11 C12 111.2(4) . . ?
O4 C11 H11A 109.4 . . ?
O4 C11 H11B 109.4 . . ?
C12 C11 H11A 109.4 . . ?
C12 C11 H11B 109.4 . . ?
H11A C11 H11B 108.0 . . ?
N1 N2 N3 107.8(5) . . ?
O1 C13 C12 112.2(4) . . ?
O1 C13 H13A 109.2 . . ?
O1 C13 H13B 109.2 . . ?
C12 C13 H13A 109.2 . . ?
C12 C13 H13B 109.2 . . ?
H13A C13 H13B 107.9 . . ?
N3 C10 C12 115.0(5) . . ?
N3 C10 H10A 108.5 . . ?
N3 C10 H10B 108.5 . . ?
C12 C10 H10A 108.5 . . ?
C12 C10 H10B 108.5 . . ?
H10A C10 H10B 107.5 . . ?
O2 C14 C12 112.6(4) . . ?
O2 C14 H14A 109.1 . . ?
O2 C14 H14B 109.1 . . ?
C12 C14 H14A 109.1 . . ?
C12 C14 H14B 109.1 . . ?
H14A C14 H14B 107.8 . . ?
N2 N1 C8 109.1(5) . . ?
N1 C8 C5 123.2(6) . . ?
C9 C8 N1 107.7(6) . . ?
C9 C8 C5 129.0(5) . . ?
N3 C9 H9 127.5 . . ?
C8 C9 N3 105.0(5) . . ?
C8 C9 H9 127.5 . . ?
C5 C6 H6 119.6 . . ?
C7 C6 H6 119.6 . . ?
C7 C6 C5 120.9(8) . . ?
C6 C5 C8 122.5(7) . . ?
C6 C5 C4 118.4(7) . . ?
C4 C5 C8 119.0(6) . . ?
C6 C7 H7 119.3 . . ?
C2 C7 C6 121.5(8) . . ?
C2 C7 H7 119.3 . . ?
N4 C19 H19A 107.7 . . ?
N4 C19 H19B 107.7 . . ?
H19A C19 H19B 107.1 . . ?
C20 C19 N4 118.5(7) . . ?
C20 C19 H19A 107.7 . . ?
C20 C19 H19B 107.7 . . ?
C7 C2 C1 124.5(11) . . ?
C3 C2 C7 118.7(9) . . ?
C3 C2 C1 116.9(11) . . ?
N4 C18 H18A 107.5 . . ?
N4 C18 H18B 107.5 . . ?
H18A C18 H18B 107.0 . . ?
C17 C18 N4 119.2(8) . . ?
C17 C18 H18A 107.5 . . ?
C17 C18 H18B 107.5 . . ?
N4 C27 H27A 108.9 . . ?
N4 C27 H27B 108.9 . . ?
H27A C27 H27B 107.7 . . ?
C28 C27 N4 113.5(7) . . ?
C28 C27 H27A 108.9 . . ?
C28 C27 H27B 108.9 . . ?
H29A C29 H29B 107.2 . . ?
H29C C29 H29D 108.8 . . ?
C28 C29 H29A 108.0 . . ?
C28 C29 H29B 108.0 . . ?
C28 C29 H29C 110.7 . . ?
C28 C29 H29D 110.7 . . ?
C30A C29 H29A 108.0 . . ?
C30A C29 H29B 108.0 . . ?
C30A C29 C28 117.2(13) . . ?
C30B C29 H29C 110.7 . . ?
C30B C29 H29D 110.7 . . ?
C30B C29 C28 105(2) . . ?
C2 C3 H3 119.2 . . ?
C2 C3 C4 121.7(10) . . ?
C4 C3 H3 119.2 . . ?
N4 C26 H26A 108.9 . . ?
N4 C26 H26B 108.9 . . ?
N4 C26 H26C 102.4 . . ?
N4 C26 H26D 102.4 . . ?
N4 C26 C25B 113.6(8) . . ?
H26A C26 H26B 107.7 . . ?
H26C C26 H26D 104.9 . . ?
C25B C26 H26A 108.9 . . ?
C25B C26 H26B 108.9 . . ?
C25A C26 N4 138.7(12) . . ?
C25A C26 H26C 102.4 . . ?
C25A C26 H26D 102.4 . . ?
C5 C4 C3 118.9(9) . . ?
C5 C4 H4 120.6 . . ?
C3 C4 H4 120.6 . . ?
C27 C28 C29 113.0(10) . . ?
C27 C28 H28A 109.0 . . ?
C27 C28 H28B 109.0 . . ?
C29 C28 H28A 109.0 . . ?
C29 C28 H28B 109.0 . . ?
H28A C28 H28B 107.8 . . ?
C19 C20 H20A 109.2 . . ?
C19 C20 H20B 109.2 . . ?
C19 C20 C21 112.2(11) . . ?
H20A C20 H20B 107.9 . . ?
C21 C20 H20A 109.2 . . ?
C21 C20 H20B 109.2 . . ?
C18 C17 H17A 108.9 . . ?
C18 C17 H17B 108.9 . . ?
C18 C17 C16 113.3(11) . . ?
H17A C17 H17B 107.7 . . ?
C16 C17 H17A 108.9 . . ?
C16 C17 H17B 108.9 . . ?
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
C2 C1 H1C 109.5 . . ?
H1A C1 H1B 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
H24A C24B H24B 108.3 . . ?
C25B C24B H24A 109.9 . . ?
C25B C24B H24B 109.9 . . ?
C23B C24B H24A 109.9 . . ?
C23B C24B H24B 109.9 . . ?
C23B C24B C25B 108.8(11) . . ?
C20 C21 H21A 109.1 . . ?
C20 C21 H21B 109.1 . . ?
H21A C21 H21B 107.8 . . ?
C22 C21 C20 112.6(15) . . ?
C22 C21 H21A 109.1 . . ?
C22 C21 H21B 109.1 . . ?
C26 C25B H25A 110.2 . . ?
C26 C25B H25B 110.2 . . ?
C24B C25B C26 107.7(10) . . ?
C24B C25B H25A 110.2 . . ?
C24B C25B H25B 110.2 . . ?
H25A C25B H25B 108.5 . . ?
C17 C16 H16A 109.6 . . ?
C17 C16 H16B 109.6 . . ?
C17 C16 C15 110.3(14) . . ?
H16A C16 H16B 108.1 . . ?
C15 C16 H16A 109.6 . . ?
C15 C16 H16B 109.6 . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22B 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C24B C23B H23A 109.5 . . ?
C24B C23B H23B 109.5 . . ?
C24B C23B H23C 109.5 . . ?
H23A C23B H23B 109.5 . . ?
H23A C23B H23C 109.5 . . ?
H23B C23B H23C 109.5 . . ?
C16 C15 H15A 109.5 . . ?
C16 C15 H15B 109.5 . . ?
C16 C15 H15C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C29 C30A H30A 109.5 . . ?
C29 C30A H30B 109.5 . . ?
C29 C30A H30C 109.5 . . ?
H30A C30A H30B 109.5 . . ?
H30A C30A H30C 109.5 . . ?
H30B C30A H30C 109.5 . . ?
C29 C30B H30D 109.5 . . ?
C29 C30B H30E 109.5 . . ?
C29 C30B H30F 109.5 . . ?
H30D C30B H30E 109.5 . . ?
H30D C30B H30F 109.5 . . ?
H30E C30B H30F 109.5 . . ?
H24C C24A H24D 110.3 . . ?
C23A C24A H24C 112.9 . . ?
C23A C24A H24D 112.9 . . ?
C25A C24A H24C 112.9 . . ?
C25A C24A H24D 112.9 . . ?
C25A C24A C23A 94.2(19) . . ?
C24A C23A H23D 109.5 . . ?
C24A C23A H23E 109.5 . . ?
C24A C23A H23F 109.5 . . ?
H23D C23A H23E 109.5 . . ?
H23D C23A H23F 109.5 . . ?
H23E C23A H23F 109.5 . . ?
C26 C25A C24A 108.0(19) . . ?
C26 C25A H25C 110.1 . . ?
C26 C25A H25D 110.1 . . ?
C24A C25A H25C 110.1 . . ?
C24A C25A H25D 110.1 . . ?
H25C C25A H25D 108.4 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
V2 V1 O7 V3 -48.05(16) . . . 3_766 ?
V2 O4 C11 C12 -67.8(4) 3_766 . . . ?
V2 O1 C13 C12 69.4(4) 3_766 . . . ?
V1 V2 O9 V3 -47.06(19) . . . . ?
V1 V3 O9 V2 -47.61(18) 3_766 . . . ?
V1 O4 C11 C12 69.8(5) . . . . ?
V1 O2 C14 C12 -68.3(5) . . . . ?
V3 V2 O8 V1 48.34(18) . . . . ?
V3 V1 O8 V2 46.15(18) 3_766 . . . ?
V3 O2 C14 C12 68.5(5) . . . . ?
V3 O1 C13 C12 -68.1(5) . . . . ?
O6 V2 O8 V1 0.82(17) . . . . ?
O6 V2 O9 V3 0.41(17) . . . . ?
O6 V1 O8 V2 -0.82(17) . . . . ?
O6 V1 O7 V3 -1.03(14) . . . 3_766 ?
O6 V3 O9 V2 -0.41(17) . . . . ?
O4 V2 O8 V1 -12.2(6) 3_766 . . . ?
O4 V2 O9 V3 78.3(2) 3_766 . . . ?
O4 V1 O8 V2 -16.1(5) . . . . ?
O4 V1 O7 V3 76.49(19) . . . 3_766 ?
O2 V1 O8 V2 -78.4(2) . . . . ?
O2 V1 O7 V3 11.4(5) . . . 3_766 ?
O2 V3 O9 V2 77.5(2) . . . . ?
O1 V2 O8 V1 -77.1(2) 3_766 . . . ?
O1 V2 O9 V3 15.3(6) 3_766 . . . ?
O1 V3 O9 V2 12.2(6) . . . . ?
O8 V2 O9 V3 -81.3(2) . . . . ?
O8 V1 O7 V3 -81.3(2) . . . 3_766 ?
O9 V2 O8 V1 81.6(2) . . . . ?
O7 V1 O8 V2 79.7(2) . . . . ?
O7 V3 O9 V2 -80.3(2) 3_766 . . . ?
O5 V1 O8 V2 -175.5(2) . . . . ?
O5 V1 O7 V3 174.12(19) . . . 3_766 ?
O3 V3 O9 V2 174.1(2) . . . . ?
O10 V2 O8 V1 -173.2(2) . . . . ?
O10 V2 O9 V3 174.1(2) . . . . ?
N3 N2 N1 C8 0.2(8) . . . . ?
N4 C19 C20 C21 -178.5(10) . . . . ?
N4 C18 C17 C16 -176.4(12) . . . . ?
N4 C27 C28 C29 -175.5(9) . . . . ?
N4 C26 C25B C24B 166.3(8) . . . . ?
N4 C26 C25A C24A 171(2) . . . . ?
C11 C12 C13 O1 -62.1(5) . . . . ?
C11 C12 C10 N3 40.1(6) . . . . ?
C11 C12 C14 O2 62.1(6) . . . . ?
N2 N3 C10 C12 75.8(7) . . . . ?
N2 N3 C9 C8 -1.0(7) . . . . ?
N2 N1 C8 C9 -0.8(8) . . . . ?
N2 N1 C8 C5 -177.7(6) . . . . ?
C13 C12 C11 O4 61.0(5) . . . . ?
C13 C12 C10 N3 160.3(4) . . . . ?
C13 C12 C14 O2 -61.0(6) . . . . ?
C10 N3 N2 N1 179.4(6) . . . . ?
C10 N3 C9 C8 -179.7(6) . . . . ?
C10 C12 C11 O4 177.9(4) . . . . ?
C10 C12 C13 O1 178.3(4) . . . . ?
C10 C12 C14 O2 -177.0(5) . . . . ?
C14 C12 C11 O4 -61.8(5) . . . . ?
C14 C12 C13 O1 60.3(5) . . . . ?
C14 C12 C10 N3 -80.7(6) . . . . ?
N1 C8 C9 N3 1.0(7) . . . . ?
N1 C8 C5 C6 159.7(7) . . . . ?
N1 C8 C5 C4 -16.4(11) . . . . ?
C8 C5 C4 C3 178.2(8) . . . . ?
C9 N3 N2 N1 0.5(8) . . . . ?
C9 N3 C10 C12 -105.5(6) . . . . ?
C9 C8 C5 C6 -16.5(11) . . . . ?
C9 C8 C5 C4 167.4(7) . . . . ?
C6 C5 C4 C3 2.0(13) . . . . ?
C6 C7 C2 C3 1.0(14) . . . . ?
C6 C7 C2 C1 -180.0(9) . . . . ?
C5 C8 C9 N3 177.8(6) . . . . ?
C5 C6 C7 C2 -1.4(12) . . . . ?
C7 C6 C5 C8 -176.3(6) . . . . ?
C7 C6 C5 C4 -0.2(11) . . . . ?
C7 C2 C3 C4 0.9(16) . . . . ?
C19 N4 C18 C17 -55.0(13) . . . . ?
C19 N4 C27 C28 61.2(12) . . . . ?
C19 N4 C26 C25B 166.1(8) . . . . ?
C19 N4 C26 C25A -158(3) . . . . ?
C19 C20 C21 C22 176.2(14) . . . . ?
C2 C3 C4 C5 -2.4(16) . . . . ?
C18 N4 C19 C20 -65.1(11) . . . . ?
C18 N4 C27 C28 179.2(9) . . . . ?
C18 N4 C26 C25B 49.1(10) . . . . ?
C18 N4 C26 C25A 85(3) . . . . ?
C18 C17 C16 C15 -171.8(17) . . . . ?
C27 N4 C19 C20 49.3(13) . . . . ?
C27 N4 C18 C17 -174.8(11) . . . . ?
C27 N4 C26 C25B -66.7(11) . . . . ?
C27 N4 C26 C25A -31(3) . . . . ?
C26 N4 C19 C20 180.0(10) . . . . ?
C26 N4 C18 C17 59.9(13) . . . . ?
C26 N4 C27 C28 -63.4(13) . . . . ?
C1 C2 C3 C4 -178.2(10) . . . . ?
C23B C24B C25B C26 170.5(9) . . . . ?
C30A C29 C28 C27 82.0(15) . . . . ?
C30B C29 C28 C27 148(3) . . . . ?
C23A C24A C25A C26 160(3) . . . . ?

_shelx_SHELXL_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.495
_oxdiff_exptl_absorpt_empirical_full_min 0.653
####################################################################### 
# 
# 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_465
_database_code_depnum_ccdc_archive 'CCDC 1560287'
_audit_update_record             
;
2017-07-05 deposited with the CCDC.
2017-11-27 downloaded from the CCDC.
;
_audit_creation_date             2017-05-09
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5335)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C16 H24 N6 O21 V6, 2(C16 H36 N)'
_chemical_formula_sum            'C48 H96 N8 O21 V6'
_chemical_formula_weight         1426.96
_chemical_melting_point          ?
_chemical_oxdiff_formula         V6CHON
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
V V 0.0687 2.1097 '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 1 21/c 1'
_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                   17.1864(7)
_cell_length_b                   15.7148(5)
_cell_length_c                   25.1531(8)
_cell_angle_alpha                90
_cell_angle_beta                 97.715(3)
_cell_angle_gamma                90
_cell_volume                     6731.9(4)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    8664
_cell_measurement_temperature    173.00(10)
_cell_measurement_theta_max      75.8910
_cell_measurement_theta_min      4.0710
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    7.317
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.20209
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43f (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.408
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       irregular
_exptl_crystal_F_000             2984
_exptl_crystal_size_max          0.7
_exptl_crystal_size_mid          0.5
_exptl_crystal_size_min          0.35
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0510
_diffrn_reflns_av_unetI/netI     0.0595
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.970
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            27976
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.915
_diffrn_reflns_theta_min         3.546
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      173.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2137
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -42.00  33.00   1.00    4.68    --  -40.81  38.00 -60.00   75
  2  ω    -46.00 -12.00   1.00    4.68    --  -40.81 125.00 -90.00   34
  3  ω    -55.00  32.00   1.00    4.68    --  -40.81  57.00  60.00   87
  4  ω     31.00  97.00   1.00    4.68    --   40.81-125.00 120.00   66
  5  ω     37.00  97.00   1.00   18.72    --  112.00 -95.00 150.00   60
  6  ω     65.00 121.00   1.00   18.72    --  112.00-125.00  90.00   56
  7  ω     59.00 118.00   1.00   18.72    --  112.00 -30.00-150.00   59
  8  ω     90.00 141.00   1.00   18.72    --  112.00 -61.00-150.00   51
  9  ω     87.00 178.00   1.00   18.72    --  112.00  61.00   0.00   91
 10  ω     96.00 133.00   1.00   18.72    --  112.00 125.00-120.00   37
 11  ω     97.00 171.00   1.00   18.72    --  112.00 125.00-150.00   74
 12  ω     40.00  79.00   1.00   18.72    --  112.00 -61.00-150.00   39
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0758333000
_diffrn_orient_matrix_UB_12      0.0454676000
_diffrn_orient_matrix_UB_13      -0.0107493000
_diffrn_orient_matrix_UB_21      0.0474526000
_diffrn_orient_matrix_UB_22      -0.0526150000
_diffrn_orient_matrix_UB_23      0.0448155000
_diffrn_orient_matrix_UB_31      0.0136561000
_diffrn_orient_matrix_UB_32      -0.0690989000
_diffrn_orient_matrix_UB_33      -0.0411461000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                10418
_reflns_number_total             13792
_reflns_odcompleteness_completeness 99.93
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     68.13
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_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    ?
_refine_diff_density_max         0.781
_refine_diff_density_min         -1.067
_refine_diff_density_rms         0.089
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     815
_refine_ls_number_reflns         13792
_refine_ls_number_restraints     108
_refine_ls_R_factor_all          0.0921
_refine_ls_R_factor_gt           0.0781
_refine_ls_restrained_S_all      1.059
_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)+(0.1378P)²+0.6711P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2203
_refine_ls_wR_factor_ref         0.2381
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 C15-C16C \\sim C15-C16B \\sim C15-C16A
 with sigma of 0.02
 O20C-C16C \\sim O20A-C16B \\sim O20B-C16A
 with sigma of 0.02
3. Rigid bond restraints
 C46, C48A, C47B, C48B, C47A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C31, C32A, C32B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C43, C44A, C44B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C1, O21A, O21B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C46 \\sim C48A \\sim C47B \\sim C48B \\sim C47A: within 1.7A with sigma of 0.04
and sigma for terminal atoms of 0.08
C31 \\sim C32A \\sim C32B: within 1.7A with sigma of 0.04 and sigma for
terminal atoms of 0.08
C43 \\sim C44A \\sim C44B: within 1.7A with sigma of 0.04 and sigma for
terminal atoms of 0.08
C1 \\sim O21A \\sim O21B: within 1.7A with sigma of 0.04 and sigma for terminal
atoms of 0.08
Uanis(C16C) = Uanis(C16B) = Uanis(C16A)
Uanis(C16C) = Uanis(O20C)
Uanis(C16B) = Uanis(O20A)
Uanis(C16A) = Uanis(O20B)
5. Others
 Fixed Sof: O20B(0.5) H20B(0.5) C16B(0.3) H16A(0.3) H16B(0.3) H1AA(0.8)
 H1AB(0.8) H1BC(0.2) H1BD(0.2) H31A(0.6) H31B(0.6) H31C(0.4) H31D(0.4)
 C32A(0.6) H32A(0.6) H32B(0.6) H32C(0.6) H46A(0.5) H46B(0.5) H46C(0.5)
 H46D(0.5) C48A(0.5) H48A(0.5) H48B(0.5) H48C(0.5) H43A(0.5) H43B(0.5)
 H43C(0.5) H43D(0.5) C44A(0.5) H44A(0.5) H44B(0.5) H44C(0.5) O21A(0.8)
 H21A(0.8) C44B(0.5) H44D(0.5) H44E(0.5) H44F(0.5) C32B(0.4) H32D(0.4)
 H32E(0.4) H32F(0.4) C47B(0.5) H47A(0.5) H47B(0.5) C48B(0.5) H48D(0.5)
 H48E(0.5) H48F(0.5) O21B(0.2) H21B(0.2) C47A(0.5) H47C(0.5) H47D(0.5)
 C16A(0.5) H16C(0.5) H16D(0.5) O20A(0.3) H20A(0.3) O20C(0.2) H20C(0.2)
 C16C(0.2) H16E(0.2) H16F(0.2)
6.a Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C9(H9A,H9B), C0AA(H0AA,H0AB), C11(H11A,H11B), C6(H6A,H6B),
 C10(H10A,H10B), C4(H4A,H4B), C20(H20D,H20E), C29(H29A,H29B), C13(H13A,H13B),
 C30(H30A,H30B), C39(H39A,H39B), C38(H38A,H38B), C37(H37A,H37B), C16B(H16A,
 H16B), C18(H18A,H18B), C1(H1AA,H1AB), C1(H1BC,H1BD), C28(H28A,H28B), C8(H8A,
 H8B), C27(H27A,H27B), C36(H36A,H36B), C21(H21C,H21D), C41(H41A,H41B), C26(H26A,
 H26B), C22(H22A,H22B), C42(H42A,H42B), C35(H35A,H35B), C31(H31A,H31B),
 C31(H31C,H31D), C46(H46A,H46B), C46(H46C,H46D), C23(H23A,H23B), C43(H43A,H43B),
  C43(H43C,H43D), C34(H34A,H34B), C19(H19A,H19B), C47B(H47A,H47B), C47A(H47C,
 H47D), C16A(H16C,H16D), C16C(H16E,H16F)
6.b Me refined with riding coordinates:
 C44B(H44D,H44E,H44F), C32B(H32D,H32E,H32F)
6.c Aromatic/amide H refined with riding coordinates:
 C14(H14), C3(H3)
6.d Idealised Me refined with riding coordinates:
 C44A(H44A,H44B,H44C)
6.e Idealised Me refined as rotating group:
 C40(H40A,H40B,H40C), C17(H17A,H17B,H17C), C25(H25A,H25B,H25C), C32A(H32A,H32B,
 H32C), C48A(H48A,H48B,H48C), C24(H24A,H24B,H24C), C33(H33A,H33B,H33C),
 C48B(H48D,H48E,H48F)
6.f Idealised tetrahedral OH refined with riding coordinates:
 O20B(H20B), O21A(H21A), O20A(H20A)
6.g Idealised tetrahedral OH refined as rotating group:
 O21B(H21B), O20C(H20C)
;
_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 0.16262(4) 0.73136(4) 0.67758(2) 0.04810(18) Uani 1 1 d . . . . .
V3 V 0.27685(4) 0.72584(4) 0.79374(3) 0.05244(19) Uani 1 1 d . . . . .
V6 V 0.26591(4) 0.58134(5) 0.71351(3) 0.05240(19) Uani 1 1 d . . . . .
V5 V 0.07376(4) 0.57728(5) 0.70942(3) 0.05245(19) Uani 1 1 d . . . . .
V1 V 0.08395(5) 0.72329(5) 0.78952(3) 0.05348(19) Uani 1 1 d . . . . .
V4 V 0.18706(6) 0.57242(5) 0.82613(3) 0.0584(2) Uani 1 1 d . . . . .
O0AA O 0.17517(15) 0.65231(16) 0.75150(10) 0.0451(5) Uani 1 1 d . . . . .
O4 O 0.23900(19) 0.65893(19) 0.66102(11) 0.0556(7) Uani 1 1 d . . . . .
O15 O 0.25874(19) 0.51318(18) 0.78088(12) 0.0565(7) Uani 1 1 d . . . . .
O14 O 0.01989(19) 0.6495(2) 0.74734(14) 0.0629(7) Uani 1 1 d . . . . .
O18 O 0.1033(2) 0.50920(19) 0.77718(12) 0.0578(7) Uani 1 1 d . . . . .
O12 O 0.16783(17) 0.51654(18) 0.68669(11) 0.0512(6) Uani 1 1 d . . . . .
O5 O 0.08313(18) 0.6560(2) 0.65700(12) 0.0569(7) Uani 1 1 d . . . . .
O10 O 0.33092(17) 0.65379(19) 0.75621(13) 0.0582(7) Uani 1 1 d . . . . .
O16 O 0.2656(2) 0.64807(19) 0.84686(12) 0.0628(8) Uani 1 1 d . . . . .
O17 O 0.1086(2) 0.6451(2) 0.84199(12) 0.0675(9) Uani 1 1 d . . . . .
O11 O 0.32553(19) 0.5191(2) 0.68947(15) 0.0660(8) Uani 1 1 d . . . . .
O13 O 0.0062(2) 0.5139(2) 0.68163(15) 0.0679(8) Uani 1 1 d . . . . .
O2 O 0.24760(16) 0.79327(17) 0.72637(10) 0.0472(6) Uani 1 1 d . . . . .
O6 O 0.1544(2) 0.8005(2) 0.63027(11) 0.0606(7) Uani 1 1 d . . . . .
O8 O 0.18243(19) 0.78727(17) 0.81719(10) 0.0523(6) Uani 1 1 d . . . . .
O7 O 0.0226(2) 0.7846(2) 0.81347(14) 0.0689(9) Uani 1 1 d . . . . .
O9 O 0.3418(2) 0.7909(2) 0.82185(14) 0.0670(9) Uani 1 1 d . . . . .
O19 O 0.1941(3) 0.5048(2) 0.87432(13) 0.0774(11) Uani 1 1 d . . . . .
O3 O 0.09131(17) 0.79230(18) 0.72283(10) 0.0480(6) Uani 1 1 d . . . . .
C7 C 0.1810(3) 0.8782(3) 0.81558(16) 0.0578(10) Uani 1 1 d . . . . .
H7A H 0.2287 0.9000 0.8360 0.069 Uiso 1 1 calc R . . . .
H7B H 0.1369 0.8985 0.8324 0.069 Uiso 1 1 calc R . . . .
C9 C 0.1692(3) 0.4253(3) 0.68829(19) 0.0587(10) Uani 1 1 d . . . . .
H9A H 0.2119 0.4049 0.6702 0.070 Uiso 1 1 calc R . . . .
H9B H 0.1205 0.4036 0.6692 0.070 Uiso 1 1 calc R . . . .
C0AA C 0.2433(3) 0.8838(3) 0.73056(16) 0.0516(8) Uani 1 1 d . . . . .
H0AA H 0.2387 0.9084 0.6949 0.062 Uiso 1 1 calc R . . . .
H0AB H 0.2916 0.9047 0.7508 0.062 Uiso 1 1 calc R . . . .
C11 C 0.2566(3) 0.4218(3) 0.7772(2) 0.0630(11) Uani 1 1 d . . . . .
H11A H 0.2624 0.3976 0.8130 0.076 Uiso 1 1 calc R . . . .
H11B H 0.3002 0.4022 0.7596 0.076 Uiso 1 1 calc R . . . .
C6 C 0.0972(3) 0.8834(3) 0.72671(16) 0.0534(9) Uani 1 1 d . . . . .
H6A H 0.0541 0.9049 0.7441 0.064 Uiso 1 1 calc R . . . .
H6B H 0.0922 0.9073 0.6909 0.064 Uiso 1 1 calc R . . . .
C5 C 0.1741(3) 0.9125(3) 0.75793(16) 0.0532(9) Uani 1 1 d . . . . .
C12 C 0.1795(3) 0.3913(3) 0.7456(2) 0.0610(10) Uani 1 1 d . . . . .
C10 C 0.1105(3) 0.4182(3) 0.7734(2) 0.0654(11) Uani 1 1 d . . . . .
H10A H 0.0625 0.3954 0.7538 0.079 Uiso 1 1 calc R . . . .
H10B H 0.1166 0.3941 0.8092 0.079 Uiso 1 1 calc R . . . .
N3 N 0.1680(2) 1.0566(2) 0.71405(14) 0.0552(8) Uani 1 1 d . . . . .
N2 N 0.2336(3) 1.0804(3) 0.69369(18) 0.0676(10) Uani 1 1 d . . . . .
N7 N 0.2160(3) 0.8071(3) 0.98742(13) 0.0623(9) Uani 1 1 d . . . . .
N4 N 0.1892(4) 0.2460(3) 0.7893(2) 0.0897(16) Uani 1 1 d . . . . .
O20B O 0.1323(11) 0.0425(6) 0.8928(4) 0.086(3) Uani 0.5 1 d D . P A 1
H20B H 0.1608 0.0250 0.8715 0.128 Uiso 0.5 1 calc R . P A 1
C4 C 0.1746(3) 1.0095(3) 0.76426(17) 0.0604(10) Uani 1 1 d . . . . .
H4A H 0.1314 1.0257 0.7833 0.073 Uiso 1 1 calc R . . . .
H4B H 0.2230 1.0260 0.7862 0.073 Uiso 1 1 calc R . . . .
C20 C 0.2015(4) 0.7240(3) 1.01517(18) 0.0735(14) Uani 1 1 d . . . . .
H20D H 0.2461 0.7128 1.0422 0.088 Uiso 1 1 calc R . . . .
H20E H 0.1558 0.7309 1.0335 0.088 Uiso 1 1 calc R . . . .
C29 C 0.2372(4) 0.8740(4) 1.03098(19) 0.0725(13) Uani 1 1 d . . . . .
H29A H 0.1959 0.8752 1.0537 0.087 Uiso 1 1 calc R . . . .
H29B H 0.2851 0.8562 1.0531 0.087 Uiso 1 1 calc R . . . .
C14 C 0.1322(5) 0.2193(4) 0.8171(3) 0.096(2) Uani 1 1 d . . . . .
H14 H 0.0783 0.2273 0.8088 0.115 Uiso 1 1 calc R . . . .
C13 C 0.1794(4) 0.2930(3) 0.7394(2) 0.0720(13) Uani 1 1 d . . . . .
H13A H 0.1301 0.2760 0.7186 0.086 Uiso 1 1 calc R . . . .
H13B H 0.2212 0.2771 0.7190 0.086 Uiso 1 1 calc R . . . .
C30 C 0.2488(5) 0.9626(4) 1.0115(3) 0.0902(18) Uani 1 1 d . . . . .
H30A H 0.1987 0.9857 0.9956 0.108 Uiso 1 1 calc R . . . .
H30B H 0.2833 0.9611 0.9839 0.108 Uiso 1 1 calc R . . . .
C39 C 0.6079(3) 0.3128(3) 0.8602(2) 0.0692(12) Uani 1 1 d . . . . .
H39A H 0.6624 0.3134 0.8539 0.083 Uiso 1 1 calc R . . . .
H39B H 0.6061 0.3315 0.8967 0.083 Uiso 1 1 calc R . . . .
C40 C 0.5769(4) 0.2237(4) 0.8537(2) 0.0799(15) Uani 1 1 d . . . . .
H40A H 0.5812 0.2039 0.8181 0.120 Uiso 1 1 calc GR . . . .
H40B H 0.5228 0.2229 0.8595 0.120 Uiso 1 1 calc GR . . . .
H40C H 0.6069 0.1873 0.8794 0.120 Uiso 1 1 calc GR . . . .
C38 C 0.5616(4) 0.3745(3) 0.8219(3) 0.0783(15) Uani 1 1 d . . . . .
H38A H 0.5679 0.3593 0.7853 0.094 Uiso 1 1 calc R . . . .
H38B H 0.5063 0.3698 0.8256 0.094 Uiso 1 1 calc R . . . .
C37 C 0.5876(3) 0.4653(3) 0.8322(2) 0.0728(13) Uani 1 1 d . . . . .
H37A H 0.6344 0.4748 0.8153 0.087 Uiso 1 1 calc R . . . .
H37B H 0.6020 0.4728 0.8705 0.087 Uiso 1 1 calc R . . . .
N6 N 0.2513(6) 0.1815(4) 0.8566(4) 0.136(3) Uani 1 1 d . . . . .
C16B C 0.124(2) 0.134(2) 0.9008(17) 0.116(6) Uani 0.3 1 d D . P B 2
H16A H 0.1352 0.1595 0.9360 0.140 Uiso 0.3 1 calc R . P B 2
H16B H 0.0681 0.1393 0.8886 0.140 Uiso 0.3 1 calc R . P B 2
C18 C 0.1689(6) 0.5699(5) 1.0106(3) 0.113(3) Uani 1 1 d . . . . .
H18A H 0.1219 0.5818 1.0268 0.135 Uiso 1 1 calc R . . . .
H18B H 0.1571 0.5229 0.9858 0.135 Uiso 1 1 calc R . . . .
C17 C 0.2305(8) 0.5437(5) 1.0525(4) 0.156(5) Uani 1 1 d . . . . .
H17A H 0.2765 0.5286 1.0367 0.233 Uiso 1 1 calc GR . . . .
H17B H 0.2131 0.4953 1.0710 0.233 Uiso 1 1 calc GR . . . .
H17C H 0.2427 0.5896 1.0773 0.233 Uiso 1 1 calc GR . . . .
N1 N 0.2091(3) 1.1232(3) 0.64919(18) 0.0716(11) Uani 1 1 d . . . . .
C3 C 0.1032(3) 1.0839(3) 0.68320(19) 0.0618(11) Uani 1 1 d . . . . .
H3 H 0.0513 1.0760 0.6887 0.074 Uiso 1 1 calc R . . . .
C2 C 0.1299(4) 1.1255(3) 0.6424(2) 0.0697(13) Uani 1 1 d . . . . .
C1 C 0.0825(5) 1.1734(5) 0.5972(3) 0.0942(19) Uani 1 1 d . U . . .
H1AA H 0.0764 1.2320 0.6080 0.113 Uiso 0.8 1 calc R . P C 1
H1AB H 0.1104 1.1734 0.5662 0.113 Uiso 0.8 1 calc R . P C 1
H1BC H 0.0304 1.1830 0.6068 0.113 Uiso 0.2 1 calc R . P D 2
H1BD H 0.1066 1.2286 0.5940 0.113 Uiso 0.2 1 calc R . P D 2
N0AA N 0.5274(2) 0.5330(3) 0.81220(19) 0.0677(10) Uani 1 1 d . . . . .
C28 C 0.1433(3) 0.8343(3) 0.94962(16) 0.0615(11) Uani 1 1 d . . . . .
H28A H 0.1544 0.8881 0.9334 0.074 Uiso 1 1 calc R . . . .
H28B H 0.1337 0.7926 0.9211 0.074 Uiso 1 1 calc R . . . .
C8 C 0.5683(4) 0.6186(4) 0.8244(3) 0.0823(16) Uani 1 1 d . . . . .
H8A H 0.5870 0.6213 0.8625 0.099 Uiso 1 1 calc R . . . .
H8B H 0.6138 0.6214 0.8054 0.099 Uiso 1 1 calc R . . . .
C27 C 0.0692(3) 0.8441(3) 0.97518(19) 0.0682(12) Uani 1 1 d . . . . .
H27A H 0.0498 0.7883 0.9836 0.082 Uiso 1 1 calc R . . . .
H27B H 0.0806 0.8757 1.0084 0.082 Uiso 1 1 calc R . . . .
C36 C 0.5006(3) 0.5235(3) 0.7524(2) 0.0708(13) Uani 1 1 d . . . . .
H36A H 0.4591 0.5645 0.7420 0.085 Uiso 1 1 calc R . . . .
H36B H 0.4784 0.4672 0.7459 0.085 Uiso 1 1 calc R . . . .
C21 C 0.2826(3) 0.7978(4) 0.95334(18) 0.0699(12) Uani 1 1 d . . . . .
H21C H 0.2681 0.7548 0.9262 0.084 Uiso 1 1 calc R . . . .
H21D H 0.2887 0.8512 0.9350 0.084 Uiso 1 1 calc R . . . .
C41 C 0.4537(3) 0.5254(4) 0.8392(3) 0.0807(16) Uani 1 1 d . . . . .
H41A H 0.4187 0.5718 0.8268 0.097 Uiso 1 1 calc R . . . .
H41B H 0.4273 0.4727 0.8276 0.097 Uiso 1 1 calc R . . . .
C26 C 0.0072(4) 0.8902(4) 0.9378(2) 0.0756(14) Uani 1 1 d . . . . .
H26A H -0.0030 0.8585 0.9045 0.091 Uiso 1 1 calc R . . . .
H26B H 0.0273 0.9456 0.9295 0.091 Uiso 1 1 calc R . . . .
C25 C -0.0692(4) 0.9021(5) 0.9603(3) 0.099(2) Uani 1 1 d . . . . .
H25A H -0.1053 0.9335 0.9352 0.149 Uiso 1 1 calc GR . . . .
H25B H -0.0597 0.9329 0.9935 0.149 Uiso 1 1 calc GR . . . .
H25C H -0.0913 0.8475 0.9666 0.149 Uiso 1 1 calc GR . . . .
C22 C 0.3606(4) 0.7738(6) 0.9846(2) 0.099(2) Uani 1 1 d . . . . .
H22A H 0.3738 0.8145 1.0134 0.119 Uiso 1 1 calc R . . . .
H22B H 0.3560 0.7182 1.0007 0.119 Uiso 1 1 calc R . . . .
C42 C 0.4674(4) 0.5268(6) 0.8998(3) 0.104(2) Uani 1 1 d . . . . .
H42A H 0.5039 0.4819 0.9126 0.125 Uiso 1 1 calc R . . . .
H42B H 0.4908 0.5808 0.9118 0.125 Uiso 1 1 calc R . . . .
C35 C 0.5645(4) 0.5360(5) 0.7167(3) 0.0915(18) Uani 1 1 d . . . . .
H35A H 0.5821 0.5947 0.7184 0.110 Uiso 1 1 calc R . . . .
H35B H 0.6091 0.4999 0.7288 0.110 Uiso 1 1 calc R . . . .
C31 C 0.2842(6) 1.0199(6) 1.0570(4) 0.122(3) Uani 1 1 d . U . . .
H31A H 0.2489 1.0201 1.0840 0.147 Uiso 0.6 1 calc R . P E 1
H31B H 0.3330 0.9941 1.0732 0.147 Uiso 0.6 1 calc R . P E 1
H31C H 0.2766 0.9969 1.0917 0.147 Uiso 0.4 1 calc R . P F 2
H31D H 0.2629 1.0770 1.0534 0.147 Uiso 0.4 1 calc R . P F 2
C32A C 0.3007(12) 1.1080(10) 1.0444(8) 0.159(8) Uani 0.6 1 d . U P G 1
H32A H 0.3395 1.1095 1.0203 0.239 Uiso 0.6 1 calc GR . P G 1
H32B H 0.3200 1.1377 1.0768 0.239 Uiso 0.6 1 calc GR . P G 1
H32C H 0.2534 1.1347 1.0277 0.239 Uiso 0.6 1 calc GR . P G 1
C46 C 0.5168(4) 0.6953(4) 0.8091(4) 0.099(2) Uani 1 1 d . U . . .
H46A H 0.4850 0.7082 0.8371 0.119 Uiso 0.5 1 calc R . P H 1
H46B H 0.4822 0.6845 0.7760 0.119 Uiso 0.5 1 calc R . P H 1
H46C H 0.5092 0.7006 0.7703 0.119 Uiso 0.5 1 calc R . P I 2
H46D H 0.4657 0.6854 0.8203 0.119 Uiso 0.5 1 calc R . P I 2
C23 C 0.4257(4) 0.7715(7) 0.9501(3) 0.119(3) Uani 1 1 d . . . . .
H23A H 0.4286 0.8262 0.9326 0.143 Uiso 1 1 calc R . . . .
H23B H 0.4139 0.7287 0.9225 0.143 Uiso 1 1 calc R . . . .
C48A C 0.6165(11) 0.7968(10) 0.8031(8) 0.093(4) Uani 0.5 1 d . U P J 2
H48A H 0.6004 0.7921 0.7651 0.139 Uiso 0.5 1 calc GR . P J 2
H48B H 0.6587 0.7578 0.8137 0.139 Uiso 0.5 1 calc GR . P J 2
H48C H 0.6338 0.8538 0.8116 0.139 Uiso 0.5 1 calc GR . P J 2
C43 C 0.3920(6) 0.5146(9) 0.9232(4) 0.148(4) Uani 1 1 d . U . . .
H43A H 0.3572 0.5614 0.9111 0.178 Uiso 0.5 1 calc R . P K 1
H43B H 0.3674 0.4628 0.9083 0.178 Uiso 0.5 1 calc R . P K 1
H43C H 0.3491 0.5421 0.9006 0.178 Uiso 0.5 1 calc R . P L 2
H43D H 0.3965 0.5405 0.9585 0.178 Uiso 0.5 1 calc R . P L 2
C24 C 0.5040(6) 0.7518(10) 0.9826(4) 0.173(6) Uani 1 1 d . . . . .
H24A H 0.5433 0.7464 0.9589 0.259 Uiso 1 1 calc GR . . . .
H24B H 0.5004 0.6994 1.0017 0.259 Uiso 1 1 calc GR . . . .
H24C H 0.5183 0.7970 1.0076 0.259 Uiso 1 1 calc GR . . . .
C44A C 0.3967(13) 0.5097(19) 0.9798(9) 0.160(10) Uani 0.5 1 d . U P M 1
H44A H 0.3623 0.4657 0.9892 0.240 Uiso 0.5 1 calc R . P M 1
H44B H 0.3814 0.5632 0.9936 0.240 Uiso 0.5 1 calc R . P M 1
H44C H 0.4497 0.4967 0.9949 0.240 Uiso 0.5 1 calc R . P M 1
C34 C 0.5314(5) 0.5133(5) 0.6595(3) 0.099(2) Uani 1 1 d . . . . .
H34A H 0.5143 0.4545 0.6584 0.118 Uiso 1 1 calc R . . . .
H34B H 0.4858 0.5485 0.6484 0.118 Uiso 1 1 calc R . . . .
O21A O 0.0048(4) 1.1354(5) 0.5824(2) 0.113(2) Uani 0.8 1 d . U P N 1
H21A H 0.0009 1.1177 0.5515 0.169 Uiso 0.8 1 calc R . P N 1
C33 C 0.5899(6) 0.5251(8) 0.6202(4) 0.141(4) Uani 1 1 d . . . . .
H33A H 0.5654 0.5111 0.5847 0.212 Uiso 1 1 calc GR . . . .
H33B H 0.6342 0.4884 0.6299 0.212 Uiso 1 1 calc GR . . . .
H33C H 0.6072 0.5832 0.6210 0.212 Uiso 1 1 calc GR . . . .
C19 C 0.1889(4) 0.6482(4) 0.9790(2) 0.0834(16) Uani 1 1 d . . . . .
H19A H 0.2361 0.6372 0.9628 0.100 Uiso 1 1 calc R . . . .
H19B H 0.1464 0.6596 0.9505 0.100 Uiso 1 1 calc R . . . .
N5 N 0.2616(5) 0.2242(4) 0.8127(3) 0.123(3) Uani 1 1 d . . . . .
C15 C 0.1722(8) 0.1771(4) 0.8608(3) 0.123(4) Uani 1 1 d D . . . .
C44B C 0.3748(19) 0.419(2) 0.9275(12) 0.221(14) Uani 0.5 1 d . U P M 2
H44D H 0.3268 0.4114 0.9425 0.332 Uiso 0.5 1 calc R . P M 2
H44E H 0.3699 0.3939 0.8925 0.332 Uiso 0.5 1 calc R . P M 2
H44F H 0.4171 0.3923 0.9503 0.332 Uiso 0.5 1 calc R . P M 2
C32B C 0.3701(15) 1.0177(19) 1.0484(13) 0.151(10) Uani 0.4 1 d . U P G 2
H32D H 0.4004 1.0521 1.0752 0.227 Uiso 0.4 1 calc R . P G 2
H32E H 0.3889 0.9601 1.0514 0.227 Uiso 0.4 1 calc R . P G 2
H32F H 0.3754 1.0394 1.0134 0.227 Uiso 0.4 1 calc R . P G 2
C47B C 0.5769(11) 0.7754(9) 0.8012(8) 0.092(4) Uani 0.5 1 d . U P O 1
H47A H 0.6106 0.7599 0.7747 0.110 Uiso 0.5 1 calc R . P O 1
H47B H 0.5463 0.8247 0.7878 0.110 Uiso 0.5 1 calc R . P O 1
C48B C 0.6250(11) 0.7973(10) 0.8508(7) 0.112(5) Uani 0.5 1 d . U P O 1
H48D H 0.6511 0.8504 0.8466 0.168 Uiso 0.5 1 calc GR . P O 1
H48E H 0.6634 0.7535 0.8600 0.168 Uiso 0.5 1 calc GR . P O 1
H48F H 0.5925 0.8025 0.8788 0.168 Uiso 0.5 1 calc GR . P O 1
O21B O 0.075(2) 1.136(2) 0.5499(9) 0.118(9) Uani 0.2 1 d . U P N 2
H21B H 0.1014 1.1619 0.5303 0.178 Uiso 0.2 1 calc GR . P N 2
C47A C 0.5484(7) 0.7760(7) 0.8325(6) 0.074(3) Uani 0.5 1 d . U P J 2
H47C H 0.5656 0.7696 0.8706 0.088 Uiso 0.5 1 calc R . P J 2
H47D H 0.5089 0.8204 0.8273 0.088 Uiso 0.5 1 calc R . P J 2
C16A C 0.1554(11) 0.1264(7) 0.9092(4) 0.086(3) Uani 0.5 1 d D . P A 1
H16C H 0.2020 0.1243 0.9356 0.103 Uiso 0.5 1 calc R . P A 1
H16D H 0.1138 0.1537 0.9255 0.103 Uiso 0.5 1 calc R . P A 1
O20A O 0.146(2) 0.0462(17) 0.9032(11) 0.116(6) Uani 0.3 1 d D . P B 2
H20A H 0.1191 0.0201 0.8790 0.174 Uiso 0.3 1 calc R . P B 2
O20C O 0.0407(17) 0.1724(18) 0.9161(9) 0.116(6) Uani 0.2 1 d D . P B 3
H20C H 0.0049 0.1567 0.8934 0.174 Uiso 0.2 1 calc GR . P B 3
C16C C 0.115(3) 0.147(4) 0.900(2) 0.116(6) Uani 0.2 1 d D . P B 3
H16E H 0.1058 0.0877 0.8901 0.140 Uiso 0.2 1 calc R . P B 3
H16F H 0.1492 0.1445 0.9343 0.140 Uiso 0.2 1 calc R . P B 3


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
V2 V6 3.0159(10) . ?
V2 V5 3.0275(10) . ?
V2 O0AA 2.223(3) . ?
V2 O4 1.827(3) . ?
V2 O5 1.829(3) . ?
V2 O2 2.026(3) . ?
V2 O6 1.604(3) . ?
V2 O3 2.022(3) . ?
V3 V6 3.0270(10) . ?
V3 V4 3.0324(11) . ?
V3 O0AA 2.240(3) . ?
V3 O10 1.809(3) . ?
V3 O16 1.840(3) . ?
V3 O2 2.005(3) . ?
V3 O8 2.042(3) . ?
V3 O9 1.607(3) . ?
V6 O0AA 2.234(3) . ?
V6 O4 1.811(3) . ?
V6 O15 2.023(3) . ?
V6 O12 2.007(3) . ?
V6 O10 1.837(3) . ?
V6 O11 1.594(3) . ?
V5 V1 3.0430(10) . ?
V5 O0AA 2.248(3) . ?
V5 O14 1.814(3) . ?
V5 O18 2.019(3) . ?
V5 O12 2.025(3) . ?
V5 O5 1.831(3) . ?
V5 O13 1.616(3) . ?
V1 V4 3.0284(11) . ?
V1 O0AA 2.240(3) . ?
V1 O14 1.835(3) . ?
V1 O17 1.812(3) . ?
V1 O8 2.011(3) . ?
V1 O7 1.604(3) . ?
V1 O3 2.016(3) . ?
V4 O0AA 2.245(3) . ?
V4 O15 2.014(3) . ?
V4 O18 2.024(3) . ?
V4 O16 1.821(3) . ?
V4 O17 1.851(4) . ?
V4 O19 1.605(3) . ?
O15 C11 1.439(5) . ?
O18 C10 1.439(6) . ?
O12 C9 1.434(5) . ?
O2 C0AA 1.429(5) . ?
O8 C7 1.429(5) . ?
O3 C6 1.437(5) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C7 C5 1.537(5) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C9 C12 1.525(7) . ?
C0AA H0AA 0.9700 . ?
C0AA H0AB 0.9700 . ?
C0AA C5 1.522(6) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C11 C12 1.528(6) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C6 C5 1.514(6) . ?
C5 C4 1.531(6) . ?
C12 C10 1.517(7) . ?
C12 C13 1.553(6) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
N3 N2 1.352(6) . ?
N3 C4 1.455(5) . ?
N3 C3 1.339(6) . ?
N2 N1 1.326(6) . ?
N7 C20 1.517(6) . ?
N7 C29 1.526(6) . ?
N7 C28 1.526(6) . ?
N7 C21 1.527(6) . ?
N4 C14 1.345(10) . ?
N4 C13 1.448(8) . ?
N4 N5 1.347(9) . ?
O20B H20B 0.8200 . ?
O20B C16A 1.422(14) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C20 H20D 0.9700 . ?
C20 H20E 0.9700 . ?
C20 C19 1.497(8) . ?
C29 H29A 0.9700 . ?
C29 H29B 0.9700 . ?
C29 C30 1.500(9) . ?
C14 H14 0.9300 . ?
C14 C15 1.385(10) . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C30 H30A 0.9700 . ?
C30 H30B 0.9700 . ?
C30 C31 1.517(9) . ?
C39 H39A 0.9700 . ?
C39 H39B 0.9700 . ?
C39 C40 1.500(8) . ?
C39 C38 1.515(7) . ?
C40 H40A 0.9600 . ?
C40 H40B 0.9600 . ?
C40 H40C 0.9600 . ?
C38 H38A 0.9700 . ?
C38 H38B 0.9700 . ?
C38 C37 1.507(7) . ?
C37 H37A 0.9700 . ?
C37 H37B 0.9700 . ?
C37 N0AA 1.521(6) . ?
N6 N5 1.325(12) . ?
N6 C15 1.379(14) . ?
C16B H16A 0.9700 . ?
C16B H16B 0.9700 . ?
C16B C15 1.547(18) . ?
C16B O20A 1.42(2) . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
C18 C17 1.448(13) . ?
C18 C19 1.529(9) . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
N1 C2 1.348(8) . ?
C3 H3 0.9300 . ?
C3 C2 1.348(7) . ?
C2 C1 1.509(7) . ?
C1 H1AA 0.9700 . ?
C1 H1AB 0.9700 . ?
C1 H1BC 0.9700 . ?
C1 H1BD 0.9700 . ?
C1 O21A 1.464(11) . ?
C1 O21B 1.31(3) . ?
N0AA C8 1.529(7) . ?
N0AA C36 1.519(7) . ?
N0AA C41 1.519(8) . ?
C28 H28A 0.9700 . ?
C28 H28B 0.9700 . ?
C28 C27 1.509(7) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C8 C46 1.514(8) . ?
C27 H27A 0.9700 . ?
C27 H27B 0.9700 . ?
C27 C26 1.509(8) . ?
C36 H36A 0.9700 . ?
C36 H36B 0.9700 . ?
C36 C35 1.522(9) . ?
C21 H21C 0.9700 . ?
C21 H21D 0.9700 . ?
C21 C22 1.508(8) . ?
C41 H41A 0.9700 . ?
C41 H41B 0.9700 . ?
C41 C42 1.511(9) . ?
C26 H26A 0.9700 . ?
C26 H26B 0.9700 . ?
C26 C25 1.511(9) . ?
C25 H25A 0.9600 . ?
C25 H25B 0.9600 . ?
C25 H25C 0.9600 . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
C22 C23 1.505(10) . ?
C42 H42A 0.9700 . ?
C42 H42B 0.9700 . ?
C42 C43 1.507(12) . ?
C35 H35A 0.9700 . ?
C35 H35B 0.9700 . ?
C35 C34 1.517(9) . ?
C31 H31A 0.9700 . ?
C31 H31B 0.9700 . ?
C31 H31C 0.9700 . ?
C31 H31D 0.9700 . ?
C31 C32A 1.457(19) . ?
C31 C32B 1.52(3) . ?
C32A H32A 0.9600 . ?
C32A H32B 0.9600 . ?
C32A H32C 0.9600 . ?
C46 H46A 0.9700 . ?
C46 H46B 0.9700 . ?
C46 H46C 0.9700 . ?
C46 H46D 0.9700 . ?
C46 C47B 1.658(18) . ?
C46 C47A 1.471(12) . ?
C23 H23A 0.9700 . ?
C23 H23B 0.9700 . ?
C23 C24 1.511(12) . ?
C48A H48A 0.9600 . ?
C48A H48B 0.9600 . ?
C48A H48C 0.9600 . ?
C48A C47A 1.502(18) . ?
C43 H43A 0.9700 . ?
C43 H43B 0.9700 . ?
C43 H43C 0.9700 . ?
C43 H43D 0.9700 . ?
C43 C44A 1.42(2) . ?
C43 C44B 1.54(3) . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
C44A H44A 0.9600 . ?
C44A H44B 0.9600 . ?
C44A H44C 0.9600 . ?
C34 H34A 0.9700 . ?
C34 H34B 0.9700 . ?
C34 C33 1.512(12) . ?
O21A H21A 0.8200 . ?
C33 H33A 0.9600 . ?
C33 H33B 0.9600 . ?
C33 H33C 0.9600 . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C15 C16A 1.515(13) . ?
C15 C16C 1.561(19) . ?
C44B H44D 0.9600 . ?
C44B H44E 0.9600 . ?
C44B H44F 0.9600 . ?
C32B H32D 0.9600 . ?
C32B H32E 0.9600 . ?
C32B H32F 0.9600 . ?
C47B H47A 0.9700 . ?
C47B H47B 0.9700 . ?
C47B C48B 1.44(2) . ?
C48B H48D 0.9600 . ?
C48B H48E 0.9600 . ?
C48B H48F 0.9600 . ?
O21B H21B 0.8200 . ?
C47A H47C 0.9700 . ?
C47A H47D 0.9700 . ?
C16A H16C 0.9700 . ?
C16A H16D 0.9700 . ?
O20A H20A 0.8200 . ?
O20C H20C 0.8200 . ?
O20C C16C 1.45(2) . ?
C16C H16E 0.9700 . ?
C16C H16F 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
V6 V2 V5 65.98(2) . . ?
O0AA V2 V6 47.56(7) . . ?
O0AA V2 V5 47.72(7) . . ?
O4 V2 V6 33.84(9) . . ?
O4 V2 V5 88.02(10) . . ?
O4 V2 O0AA 81.40(12) . . ?
O4 V2 O5 93.69(14) . . ?
O4 V2 O2 87.46(13) . . ?
O4 V2 O3 158.66(12) . . ?
O5 V2 V6 88.05(10) . . ?
O5 V2 V5 34.22(10) . . ?
O5 V2 O0AA 81.94(12) . . ?
O5 V2 O2 158.83(13) . . ?
O5 V2 O3 88.84(13) . . ?
O2 V2 V6 81.17(8) . . ?
O2 V2 V5 124.89(8) . . ?
O2 V2 O0AA 77.32(10) . . ?
O6 V2 V6 137.89(13) . . ?
O6 V2 V5 137.82(13) . . ?
O6 V2 O0AA 171.31(13) . . ?
O6 V2 O4 104.34(16) . . ?
O6 V2 O5 103.93(16) . . ?
O6 V2 O2 96.22(15) . . ?
O6 V2 O3 95.56(14) . . ?
O3 V2 V6 125.33(8) . . ?
O3 V2 V5 82.21(8) . . ?
O3 V2 O0AA 77.99(10) . . ?
O3 V2 O2 82.74(12) . . ?
V6 V3 V4 66.07(2) . . ?
O0AA V3 V6 47.33(7) . . ?
O0AA V3 V4 47.52(7) . . ?
O10 V3 V6 34.19(9) . . ?
O10 V3 V4 87.60(10) . . ?
O10 V3 O0AA 81.51(11) . . ?
O10 V3 O16 94.28(16) . . ?
O10 V3 O2 88.74(13) . . ?
O10 V3 O8 158.51(13) . . ?
O16 V3 V6 89.01(9) . . ?
O16 V3 V4 33.89(10) . . ?
O16 V3 O0AA 81.40(12) . . ?
O16 V3 O2 157.83(14) . . ?
O16 V3 O8 86.50(14) . . ?
O2 V3 V6 81.20(8) . . ?
O2 V3 V4 124.65(8) . . ?
O2 V3 O0AA 77.33(10) . . ?
O2 V3 O8 82.85(11) . . ?
O8 V3 V6 124.51(9) . . ?
O8 V3 V4 81.11(9) . . ?
O8 V3 O0AA 77.37(11) . . ?
O9 V3 V6 138.45(15) . . ?
O9 V3 V4 137.43(14) . . ?
O9 V3 O0AA 171.46(15) . . ?
O9 V3 O10 104.64(17) . . ?
O9 V3 O16 103.75(17) . . ?
O9 V3 O2 96.68(15) . . ?
O9 V3 O8 95.99(17) . . ?
V2 V6 V3 66.09(2) . . ?
O0AA V6 V2 47.25(7) . . ?
O0AA V6 V3 47.52(7) . . ?
O4 V6 V2 34.19(9) . . ?
O4 V6 V3 88.16(9) . . ?
O4 V6 O0AA 81.44(12) . . ?
O4 V6 O15 158.30(14) . . ?
O4 V6 O12 88.62(13) . . ?
O4 V6 O10 94.86(14) . . ?
O15 V6 V2 124.44(10) . . ?
O15 V6 V3 81.03(9) . . ?
O15 V6 O0AA 77.37(12) . . ?
O12 V6 V2 82.06(9) . . ?
O12 V6 V3 125.38(9) . . ?
O12 V6 O0AA 78.11(11) . . ?
O12 V6 O15 82.53(12) . . ?
O10 V6 V2 88.74(10) . . ?
O10 V6 V3 33.59(10) . . ?
O10 V6 O0AA 81.10(12) . . ?
O10 V6 O15 86.50(14) . . ?
O10 V6 O12 158.16(14) . . ?
O11 V6 V2 138.50(15) . . ?
O11 V6 V3 136.72(12) . . ?
O11 V6 O0AA 172.04(15) . . ?
O11 V6 O4 104.54(18) . . ?
O11 V6 O15 96.16(17) . . ?
O11 V6 O12 96.59(15) . . ?
O11 V6 O10 103.34(16) . . ?
V2 V5 V1 65.53(2) . . ?
O0AA V5 V2 47.02(7) . . ?
O0AA V5 V1 47.21(7) . . ?
O14 V5 V2 87.12(10) . . ?
O14 V5 V1 33.73(11) . . ?
O14 V5 O0AA 80.94(13) . . ?
O14 V5 O18 88.64(15) . . ?
O14 V5 O12 157.88(14) . . ?
O14 V5 O5 93.22(15) . . ?
O18 V5 V2 124.65(9) . . ?
O18 V5 V1 81.67(9) . . ?
O18 V5 O0AA 77.82(11) . . ?
O18 V5 O12 82.45(13) . . ?
O12 V5 V2 81.49(9) . . ?
O12 V5 V1 124.42(8) . . ?
O12 V5 O0AA 77.42(10) . . ?
O5 V5 V2 34.18(9) . . ?
O5 V5 V1 87.96(10) . . ?
O5 V5 O0AA 81.20(12) . . ?
O5 V5 O18 158.38(14) . . ?
O5 V5 O12 87.96(14) . . ?
O13 V5 V2 137.50(14) . . ?
O13 V5 V1 136.52(14) . . ?
O13 V5 O0AA 173.56(16) . . ?
O13 V5 O14 103.05(18) . . ?
O13 V5 O18 97.08(17) . . ?
O13 V5 O12 98.13(16) . . ?
O13 V5 O5 103.45(17) . . ?
V4 V1 V5 65.81(2) . . ?
O0AA V1 V5 47.41(7) . . ?
O0AA V1 V4 47.59(7) . . ?
O14 V1 V5 33.30(10) . . ?
O14 V1 V4 87.84(11) . . ?
O14 V1 O0AA 80.71(12) . . ?
O14 V1 O8 158.07(13) . . ?
O14 V1 O3 87.62(14) . . ?
O17 V1 V5 87.58(10) . . ?
O17 V1 V4 34.65(11) . . ?
O17 V1 O0AA 82.22(13) . . ?
O17 V1 O14 93.21(16) . . ?
O17 V1 O8 89.06(15) . . ?
O17 V1 O3 159.50(15) . . ?
O8 V1 V5 125.25(9) . . ?
O8 V1 V4 81.67(9) . . ?
O8 V1 O0AA 78.00(11) . . ?
O8 V1 O3 82.83(12) . . ?
O7 V1 V5 135.98(15) . . ?
O7 V1 V4 138.00(13) . . ?
O7 V1 O0AA 172.86(14) . . ?
O7 V1 O14 102.87(18) . . ?
O7 V1 O17 103.58(17) . . ?
O7 V1 O8 97.76(17) . . ?
O7 V1 O3 96.17(15) . . ?
O3 V1 V5 81.90(8) . . ?
O3 V1 V4 125.08(8) . . ?
O3 V1 O0AA 77.70(10) . . ?
V1 V4 V3 66.04(2) . . ?
O0AA V4 V3 47.40(7) . . ?
O0AA V4 V1 47.47(7) . . ?
O15 V4 V3 81.01(9) . . ?
O15 V4 V1 124.57(9) . . ?
O15 V4 O0AA 77.28(11) . . ?
O15 V4 O18 82.43(13) . . ?
O18 V4 V3 124.93(9) . . ?
O18 V4 V1 81.96(10) . . ?
O18 V4 O0AA 77.78(11) . . ?
O16 V4 V3 34.29(9) . . ?
O16 V4 V1 87.53(11) . . ?
O16 V4 O0AA 81.68(12) . . ?
O16 V4 O15 88.72(15) . . ?
O16 V4 O18 158.96(13) . . ?
O16 V4 O17 93.95(17) . . ?
O17 V4 V3 88.81(11) . . ?
O17 V4 V1 33.81(9) . . ?
O17 V4 O0AA 81.26(11) . . ?
O17 V4 O15 157.76(13) . . ?
O17 V4 O18 87.41(16) . . ?
O19 V4 V3 137.76(16) . . ?
O19 V4 V1 136.88(17) . . ?
O19 V4 O0AA 172.50(14) . . ?
O19 V4 O15 97.52(18) . . ?
O19 V4 O18 96.29(17) . . ?
O19 V4 O16 103.79(18) . . ?
O19 V4 O17 103.23(19) . . ?
V2 O0AA V3 95.18(10) . . ?
V2 O0AA V6 85.19(9) . . ?
V2 O0AA V5 85.26(9) . . ?
V2 O0AA V1 94.81(10) . . ?
V2 O0AA V4 179.66(14) . . ?
V3 O0AA V5 179.41(15) . . ?
V3 O0AA V1 94.97(10) . . ?
V3 O0AA V4 85.08(9) . . ?
V6 O0AA V3 85.15(9) . . ?
V6 O0AA V5 94.50(10) . . ?
V6 O0AA V1 179.87(16) . . ?
V6 O0AA V4 95.06(10) . . ?
V1 O0AA V5 85.38(9) . . ?
V1 O0AA V4 84.94(9) . . ?
V4 O0AA V5 94.49(10) . . ?
V6 O4 V2 111.98(15) . . ?
V4 O15 V6 109.84(14) . . ?
C11 O15 V6 118.6(3) . . ?
C11 O15 V4 119.1(3) . . ?
V5 O14 V1 112.97(17) . . ?
V5 O18 V4 109.34(14) . . ?
C10 O18 V5 119.0(3) . . ?
C10 O18 V4 117.9(3) . . ?
V6 O12 V5 109.41(13) . . ?
C9 O12 V6 119.2(3) . . ?
C9 O12 V5 118.3(3) . . ?
V2 O5 V5 111.60(15) . . ?
V3 O10 V6 112.22(16) . . ?
V4 O16 V3 111.82(15) . . ?
V1 O17 V4 111.55(16) . . ?
V3 O2 V2 109.68(13) . . ?
C0AA O2 V2 118.9(3) . . ?
C0AA O2 V3 118.2(2) . . ?
V1 O8 V3 109.16(13) . . ?
C7 O8 V3 118.4(3) . . ?
C7 O8 V1 118.6(3) . . ?
V1 O3 V2 108.91(13) . . ?
C6 O3 V2 117.8(2) . . ?
C6 O3 V1 119.4(2) . . ?
O8 C7 H7A 109.2 . . ?
O8 C7 H7B 109.2 . . ?
O8 C7 C5 112.1(3) . . ?
H7A C7 H7B 107.9 . . ?
C5 C7 H7A 109.2 . . ?
C5 C7 H7B 109.2 . . ?
O12 C9 H9A 109.2 . . ?
O12 C9 H9B 109.2 . . ?
O12 C9 C12 112.1(3) . . ?
H9A C9 H9B 107.9 . . ?
C12 C9 H9A 109.2 . . ?
C12 C9 H9B 109.2 . . ?
O2 C0AA H0AA 109.1 . . ?
O2 C0AA H0AB 109.1 . . ?
O2 C0AA C5 112.3(3) . . ?
H0AA C0AA H0AB 107.9 . . ?
C5 C0AA H0AA 109.1 . . ?
C5 C0AA H0AB 109.1 . . ?
O15 C11 H11A 109.4 . . ?
O15 C11 H11B 109.4 . . ?
O15 C11 C12 111.1(4) . . ?
H11A C11 H11B 108.0 . . ?
C12 C11 H11A 109.4 . . ?
C12 C11 H11B 109.4 . . ?
O3 C6 H6A 109.1 . . ?
O3 C6 H6B 109.1 . . ?
O3 C6 C5 112.7(4) . . ?
H6A C6 H6B 107.8 . . ?
C5 C6 H6A 109.1 . . ?
C5 C6 H6B 109.1 . . ?
C0AA C5 C7 110.9(4) . . ?
C0AA C5 C4 110.4(4) . . ?
C6 C5 C7 109.6(4) . . ?
C6 C5 C0AA 110.9(3) . . ?
C6 C5 C4 110.3(4) . . ?
C4 C5 C7 104.7(3) . . ?
C9 C12 C11 111.3(4) . . ?
C9 C12 C13 104.8(4) . . ?
C11 C12 C13 110.7(4) . . ?
C10 C12 C9 109.8(4) . . ?
C10 C12 C11 110.5(4) . . ?
C10 C12 C13 109.5(4) . . ?
O18 C10 C12 112.7(4) . . ?
O18 C10 H10A 109.0 . . ?
O18 C10 H10B 109.0 . . ?
C12 C10 H10A 109.0 . . ?
C12 C10 H10B 109.0 . . ?
H10A C10 H10B 107.8 . . ?
N2 N3 C4 119.8(4) . . ?
C3 N3 N2 111.2(4) . . ?
C3 N3 C4 128.9(4) . . ?
N1 N2 N3 105.9(4) . . ?
C20 N7 C29 107.5(4) . . ?
C20 N7 C28 110.9(4) . . ?
C20 N7 C21 110.9(4) . . ?
C29 N7 C21 110.1(4) . . ?
C28 N7 C29 110.6(4) . . ?
C28 N7 C21 106.9(3) . . ?
C14 N4 C13 126.9(6) . . ?
C14 N4 N5 112.9(7) . . ?
N5 N4 C13 120.2(7) . . ?
C16A O20B H20B 109.5 . . ?
C5 C4 H4A 108.6 . . ?
C5 C4 H4B 108.6 . . ?
N3 C4 C5 114.6(3) . . ?
N3 C4 H4A 108.6 . . ?
N3 C4 H4B 108.6 . . ?
H4A C4 H4B 107.6 . . ?
N7 C20 H20D 108.5 . . ?
N7 C20 H20E 108.5 . . ?
H20D C20 H20E 107.5 . . ?
C19 C20 N7 115.2(4) . . ?
C19 C20 H20D 108.5 . . ?
C19 C20 H20E 108.5 . . ?
N7 C29 H29A 108.4 . . ?
N7 C29 H29B 108.4 . . ?
H29A C29 H29B 107.4 . . ?
C30 C29 N7 115.7(4) . . ?
C30 C29 H29A 108.4 . . ?
C30 C29 H29B 108.4 . . ?
N4 C14 H14 128.0 . . ?
N4 C14 C15 104.1(9) . . ?
C15 C14 H14 128.0 . . ?
C12 C13 H13A 108.5 . . ?
C12 C13 H13B 108.5 . . ?
N4 C13 C12 114.9(4) . . ?
N4 C13 H13A 108.5 . . ?
N4 C13 H13B 108.5 . . ?
H13A C13 H13B 107.5 . . ?
C29 C30 H30A 109.4 . . ?
C29 C30 H30B 109.4 . . ?
C29 C30 C31 111.2(6) . . ?
H30A C30 H30B 108.0 . . ?
C31 C30 H30A 109.4 . . ?
C31 C30 H30B 109.4 . . ?
H39A C39 H39B 107.9 . . ?
C40 C39 H39A 109.1 . . ?
C40 C39 H39B 109.1 . . ?
C40 C39 C38 112.3(5) . . ?
C38 C39 H39A 109.1 . . ?
C38 C39 H39B 109.1 . . ?
C39 C40 H40A 109.5 . . ?
C39 C40 H40B 109.5 . . ?
C39 C40 H40C 109.5 . . ?
H40A C40 H40B 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
C39 C38 H38A 109.2 . . ?
C39 C38 H38B 109.2 . . ?
H38A C38 H38B 107.9 . . ?
C37 C38 C39 112.2(4) . . ?
C37 C38 H38A 109.2 . . ?
C37 C38 H38B 109.2 . . ?
C38 C37 H37A 108.4 . . ?
C38 C37 H37B 108.4 . . ?
C38 C37 N0AA 115.6(4) . . ?
H37A C37 H37B 107.4 . . ?
N0AA C37 H37A 108.4 . . ?
N0AA C37 H37B 108.4 . . ?
N5 N6 C15 109.4(7) . . ?
H16A C16B H16B 108.6 . . ?
C15 C16B H16A 110.3 . . ?
C15 C16B H16B 110.3 . . ?
O20A C16B H16A 110.3 . . ?
O20A C16B H16B 110.3 . . ?
O20A C16B C15 107(3) . . ?
H18A C18 H18B 107.6 . . ?
C17 C18 H18A 108.7 . . ?
C17 C18 H18B 108.7 . . ?
C17 C18 C19 114.4(8) . . ?
C19 C18 H18A 108.7 . . ?
C19 C18 H18B 108.7 . . ?
C18 C17 H17A 109.5 . . ?
C18 C17 H17B 109.5 . . ?
C18 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
N2 N1 C2 108.7(4) . . ?
N3 C3 H3 127.6 . . ?
N3 C3 C2 104.8(5) . . ?
C2 C3 H3 127.6 . . ?
N1 C2 C3 109.4(4) . . ?
N1 C2 C1 122.9(5) . . ?
C3 C2 C1 127.6(6) . . ?
C2 C1 H1AA 109.3 . . ?
C2 C1 H1AB 109.3 . . ?
C2 C1 H1BC 108.3 . . ?
C2 C1 H1BD 108.3 . . ?
H1AA C1 H1AB 107.9 . . ?
H1BC C1 H1BD 107.4 . . ?
O21A C1 C2 111.7(6) . . ?
O21A C1 H1AA 109.3 . . ?
O21A C1 H1AB 109.3 . . ?
O21B C1 C2 116.0(14) . . ?
O21B C1 H1BC 108.3 . . ?
O21B C1 H1BD 108.3 . . ?
C37 N0AA C8 105.9(4) . . ?
C36 N0AA C37 111.1(4) . . ?
C36 N0AA C8 110.8(4) . . ?
C36 N0AA C41 105.9(4) . . ?
C41 N0AA C37 111.6(5) . . ?
C41 N0AA C8 111.6(5) . . ?
N7 C28 H28A 108.4 . . ?
N7 C28 H28B 108.4 . . ?
H28A C28 H28B 107.5 . . ?
C27 C28 N7 115.5(4) . . ?
C27 C28 H28A 108.4 . . ?
C27 C28 H28B 108.4 . . ?
N0AA C8 H8A 108.7 . . ?
N0AA C8 H8B 108.7 . . ?
H8A C8 H8B 107.6 . . ?
C46 C8 N0AA 114.3(5) . . ?
C46 C8 H8A 108.7 . . ?
C46 C8 H8B 108.7 . . ?
C28 C27 H27A 109.6 . . ?
C28 C27 H27B 109.6 . . ?
H27A C27 H27B 108.1 . . ?
C26 C27 C28 110.4(4) . . ?
C26 C27 H27A 109.6 . . ?
C26 C27 H27B 109.6 . . ?
N0AA C36 H36A 108.5 . . ?
N0AA C36 H36B 108.5 . . ?
N0AA C36 C35 115.2(4) . . ?
H36A C36 H36B 107.5 . . ?
C35 C36 H36A 108.5 . . ?
C35 C36 H36B 108.5 . . ?
N7 C21 H21C 108.7 . . ?
N7 C21 H21D 108.7 . . ?
H21C C21 H21D 107.6 . . ?
C22 C21 N7 114.3(4) . . ?
C22 C21 H21C 108.7 . . ?
C22 C21 H21D 108.7 . . ?
N0AA C41 H41A 108.5 . . ?
N0AA C41 H41B 108.5 . . ?
H41A C41 H41B 107.5 . . ?
C42 C41 N0AA 115.0(5) . . ?
C42 C41 H41A 108.5 . . ?
C42 C41 H41B 108.5 . . ?
C27 C26 H26A 108.8 . . ?
C27 C26 H26B 108.8 . . ?
C27 C26 C25 113.7(5) . . ?
H26A C26 H26B 107.7 . . ?
C25 C26 H26A 108.8 . . ?
C25 C26 H26B 108.8 . . ?
C26 C25 H25A 109.5 . . ?
C26 C25 H25B 109.5 . . ?
C26 C25 H25C 109.5 . . ?
H25A C25 H25B 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C21 C22 H22A 109.1 . . ?
C21 C22 H22B 109.1 . . ?
H22A C22 H22B 107.8 . . ?
C23 C22 C21 112.5(5) . . ?
C23 C22 H22A 109.1 . . ?
C23 C22 H22B 109.1 . . ?
C41 C42 H42A 109.3 . . ?
C41 C42 H42B 109.3 . . ?
H42A C42 H42B 108.0 . . ?
C43 C42 C41 111.6(7) . . ?
C43 C42 H42A 109.3 . . ?
C43 C42 H42B 109.3 . . ?
C36 C35 H35A 109.9 . . ?
C36 C35 H35B 109.9 . . ?
H35A C35 H35B 108.3 . . ?
C34 C35 C36 108.8(6) . . ?
C34 C35 H35A 109.9 . . ?
C34 C35 H35B 109.9 . . ?
C30 C31 H31A 107.8 . . ?
C30 C31 H31B 107.8 . . ?
C30 C31 H31C 111.7 . . ?
C30 C31 H31D 111.7 . . ?
C30 C31 C32B 100.3(12) . . ?
H31A C31 H31B 107.2 . . ?
H31C C31 H31D 109.5 . . ?
C32A C31 C30 118.0(10) . . ?
C32A C31 H31A 107.8 . . ?
C32A C31 H31B 107.8 . . ?
C32B C31 H31C 111.7 . . ?
C32B C31 H31D 111.7 . . ?
C31 C32A H32A 109.5 . . ?
C31 C32A H32B 109.5 . . ?
C31 C32A H32C 109.5 . . ?
H32A C32A H32B 109.5 . . ?
H32A C32A H32C 109.5 . . ?
H32B C32A H32C 109.5 . . ?
C8 C46 H46A 110.4 . . ?
C8 C46 H46B 110.4 . . ?
C8 C46 H46C 108.7 . . ?
C8 C46 H46D 108.7 . . ?
C8 C46 C47B 106.4(8) . . ?
H46A C46 H46B 108.6 . . ?
H46C C46 H46D 107.6 . . ?
C47B C46 H46A 110.4 . . ?
C47B C46 H46B 110.4 . . ?
C47A C46 C8 114.4(7) . . ?
C47A C46 H46C 108.7 . . ?
C47A C46 H46D 108.7 . . ?
C22 C23 H23A 109.3 . . ?
C22 C23 H23B 109.3 . . ?
C22 C23 C24 111.8(7) . . ?
H23A C23 H23B 107.9 . . ?
C24 C23 H23A 109.3 . . ?
C24 C23 H23B 109.3 . . ?
H48A C48A H48B 109.5 . . ?
H48A C48A H48C 109.5 . . ?
H48B C48A H48C 109.5 . . ?
C47A C48A H48A 109.5 . . ?
C47A C48A H48B 109.5 . . ?
C47A C48A H48C 109.5 . . ?
C42 C43 H43A 107.9 . . ?
C42 C43 H43B 107.9 . . ?
C42 C43 H43C 109.8 . . ?
C42 C43 H43D 109.8 . . ?
C42 C43 C44B 109.5(16) . . ?
H43A C43 H43B 107.2 . . ?
H43C C43 H43D 108.2 . . ?
C44A C43 C42 117.7(13) . . ?
C44A C43 H43A 107.9 . . ?
C44A C43 H43B 107.9 . . ?
C44B C43 H43C 109.8 . . ?
C44B C43 H43D 109.8 . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C43 C44A H44A 109.5 . . ?
C43 C44A H44B 109.5 . . ?
C43 C44A H44C 109.5 . . ?
H44A C44A H44B 109.5 . . ?
H44A C44A H44C 109.5 . . ?
H44B C44A H44C 109.5 . . ?
C35 C34 H34A 108.9 . . ?
C35 C34 H34B 108.9 . . ?
H34A C34 H34B 107.8 . . ?
C33 C34 C35 113.2(7) . . ?
C33 C34 H34A 108.9 . . ?
C33 C34 H34B 108.9 . . ?
C1 O21A H21A 109.5 . . ?
C34 C33 H33A 109.5 . . ?
C34 C33 H33B 109.5 . . ?
C34 C33 H33C 109.5 . . ?
H33A C33 H33B 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C20 C19 C18 110.5(5) . . ?
C20 C19 H19A 109.6 . . ?
C20 C19 H19B 109.6 . . ?
C18 C19 H19A 109.6 . . ?
C18 C19 H19B 109.6 . . ?
H19A C19 H19B 108.1 . . ?
N6 N5 N4 105.9(9) . . ?
C14 C15 C16B 118(2) . . ?
C14 C15 C16A 139.7(14) . . ?
C14 C15 C16C 111(2) . . ?
N6 C15 C14 107.8(8) . . ?
N6 C15 C16B 133.8(18) . . ?
N6 C15 C16A 112.5(11) . . ?
N6 C15 C16C 141(2) . . ?
C43 C44B H44D 109.5 . . ?
C43 C44B H44E 109.5 . . ?
C43 C44B H44F 109.5 . . ?
H44D C44B H44E 109.5 . . ?
H44D C44B H44F 109.5 . . ?
H44E C44B H44F 109.5 . . ?
C31 C32B H32D 109.5 . . ?
C31 C32B H32E 109.5 . . ?
C31 C32B H32F 109.5 . . ?
H32D C32B H32E 109.5 . . ?
H32D C32B H32F 109.5 . . ?
H32E C32B H32F 109.5 . . ?
C46 C47B H47A 109.3 . . ?
C46 C47B H47B 109.3 . . ?
H47A C47B H47B 107.9 . . ?
C48B C47B C46 111.7(15) . . ?
C48B C47B H47A 109.3 . . ?
C48B C47B H47B 109.3 . . ?
C47B C48B H48D 109.5 . . ?
C47B C48B H48E 109.5 . . ?
C47B C48B H48F 109.5 . . ?
H48D C48B H48E 109.5 . . ?
H48D C48B H48F 109.5 . . ?
H48E C48B H48F 109.5 . . ?
C1 O21B H21B 109.5 . . ?
C46 C47A C48A 105.1(11) . . ?
C46 C47A H47C 110.7 . . ?
C46 C47A H47D 110.7 . . ?
C48A C47A H47C 110.7 . . ?
C48A C47A H47D 110.7 . . ?
H47C C47A H47D 108.8 . . ?
O20B C16A C15 109.2(10) . . ?
O20B C16A H16C 109.8 . . ?
O20B C16A H16D 109.8 . . ?
C15 C16A H16C 109.8 . . ?
C15 C16A H16D 109.8 . . ?
H16C C16A H16D 108.3 . . ?
C16B O20A H20A 109.5 . . ?
C16C O20C H20C 109.5 . . ?
C15 C16C H16E 102.6 . . ?
C15 C16C H16F 102.6 . . ?
O20C C16C C15 138(4) . . ?
O20C C16C H16E 102.6 . . ?
O20C C16C H16F 102.6 . . ?
H16E C16C H16F 105.0 . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.064
_oxdiff_exptl_absorpt_empirical_full_min 0.462
