# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2018

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_1
_database_code_depnum_ccdc_archive 'CCDC 1573268'
_audit_update_record             
;
2017-09-07 deposited with the CCDC.
2018-01-09 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
'C16 H16 O36 V8, 2(C16 H36 N), 3(C2 H3 N), 2(Cl)'
_chemical_formula_sum            'C54 H97 Cl2 N5 O36 V8'
_chemical_formula_weight         1870.78

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   16.3158(6)
_cell_length_b                   16.3786(6)
_cell_length_c                   16.7821(6)
_cell_angle_alpha                90.9530(10)
_cell_angle_beta                 117.9780(10)
_cell_angle_gamma                93.3520(10)
_cell_volume                     3948.8(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    193(2)
_cell_measurement_reflns_used    8178
_cell_measurement_theta_min      2.43
_cell_measurement_theta_max      28.99

_exptl_crystal_description       prism
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.573
_exptl_crystal_F_000             1924
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.150
_exptl_absorpt_coefficient_mu    1.059
_shelx_estimated_absorpt_T_min   0.677
_shelx_estimated_absorpt_T_max   0.857
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6767
_exptl_absorpt_correction_T_max  0.8573
_exptl_absorpt_process_details   
;
program SADABS, Bruker (2001).
;
_diffrn_ambient_temperature      193(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  
;
 Bruker-Nonius X8kappa APEX II CCD area detector
;
_diffrn_measurement_method       'phi and omega scans with narrow frames'
_diffrn_detector_area_resol_mean 8.26
_diffrn_reflns_number            71065
_diffrn_reflns_av_unetI/netI     0.0235
_diffrn_reflns_av_R_equivalents  0.0303
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         1.957
_diffrn_reflns_theta_max         25.249
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measured_fraction_theta_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_point_group_measured_fraction_full 0.992
_reflns_number_total             14200
_reflns_number_gt                11860
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'APEX2 Software Suite (Bruker, 2007)'
_computing_cell_refinement       'APEX2 Software Suite (Bruker, 2007)'
_computing_data_reduction        'APEX2 Software Suite (Bruker, 2007)'
_computing_structure_solution    'SIR2002 (Burla et al., 2003)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL and publCIF (Westrip, 2010)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0745P)²+5.2245P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         14200
_refine_ls_number_parameters     957
_refine_ls_number_restraints     281
_refine_ls_R_factor_all          0.0549
_refine_ls_R_factor_gt           0.0450
_refine_ls_wR_factor_ref         0.1375
_refine_ls_wR_factor_gt          0.1315
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_restrained_S_all      1.159
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
V1 V 0.29162(4) 0.53558(3) 0.04159(4) 0.03194(14) Uani 1 1 d . . . . .
V2 V 0.23340(4) 0.72252(3) 0.04131(4) 0.03193(14) Uani 1 1 d . . . . .
V3 V 0.24245(4) 0.70008(3) 0.23745(4) 0.02908(13) Uani 1 1 d . . . . .
V4 V 0.30178(4) 0.51248(3) 0.23869(4) 0.02972(14) Uani 1 1 d . . . . .
V5 V 0.75491(4) 0.79413(3) 0.49274(4) 0.03007(14) Uani 1 1 d . . . . .
V6 V 0.72215(4) 0.89851(3) 0.31752(4) 0.02986(14) Uani 1 1 d . . . . .
V7 V 0.77072(4) 0.74005(4) 0.23064(4) 0.03113(14) Uani 1 1 d . . . . .
V8 V 0.80429(4) 0.63618(3) 0.40643(4) 0.03107(14) Uani 1 1 d . . . . .
Cl1 Cl 0.37906(5) 0.65175(5) 0.19018(5) 0.02835(17) Uani 1 1 d . . . . .
Cl2 Cl 0.65153(5) 0.73269(5) 0.31121(5) 0.02813(16) Uani 1 1 d . . . . .
O1 O 0.35427(15) 0.70031(13) 0.35738(15) 0.0313(5) Uani 1 1 d . . . . .
O2 O 0.38930(15) 0.56881(13) 0.36298(15) 0.0301(5) Uani 1 1 d . . . . .
O3 O 0.54773(16) 0.60282(14) 0.52645(15) 0.0342(5) Uani 1 1 d . . . . .
O4 O 0.68484(16) 0.69318(14) 0.50863(15) 0.0324(5) Uani 1 1 d . . . . .
O5 O 0.71148(16) 0.58589(13) 0.44079(16) 0.0331(5) Uani 1 1 d . . . . .
O6 O 0.41171(16) 0.48137(14) 0.12114(16) 0.0334(5) Uani 1 1 d . . . . .
O7 O 0.42240(16) 0.47328(13) 0.25982(16) 0.0333(5) Uani 1 1 d . . . . .
O8 O 0.59004(17) 0.44161(14) 0.18308(17) 0.0382(6) Uani 1 1 d . . . . .
O9 O 0.69351(16) 0.63740(14) 0.17308(16) 0.0348(5) Uani 1 1 d . . . . .
O10 O 0.72335(16) 0.56172(14) 0.29342(16) 0.0349(5) Uani 1 1 d . . . . .
O11 O 0.38121(16) 0.59790(15) 0.01166(16) 0.0353(5) Uani 1 1 d . . . . .
O12 O 0.33617(16) 0.72600(15) 0.00402(15) 0.0346(5) Uani 1 1 d . . . . .
O13 O 0.48242(17) 0.78550(15) -0.02410(16) 0.0400(6) Uani 1 1 d . . . . .
O14 O 0.61660(16) 0.88961(14) 0.19334(15) 0.0334(5) Uani 1 1 d . . . . .
O15 O 0.65232(16) 0.78427(14) 0.13054(15) 0.0334(5) Uani 1 1 d . . . . .
O16 O 0.31105(16) 0.82210(14) 0.11062(16) 0.0339(5) Uani 1 1 d . . . . .
O17 O 0.30881(16) 0.81275(13) 0.24344(16) 0.0334(5) Uani 1 1 d . . . . .
O18 O 0.43650(17) 0.94745(14) 0.31575(18) 0.0409(6) Uani 1 1 d . . . . .
O19 O 0.63132(16) 0.83602(14) 0.45751(15) 0.0330(5) Uani 1 1 d . . . . .
O20 O 0.61153(16) 0.91416(13) 0.34135(15) 0.0320(5) Uani 1 1 d . . . . .
O21 O 0.25141(18) 0.46781(16) -0.03862(17) 0.0428(6) Uani 1 1 d . . . . .
O22 O 0.15753(17) 0.76221(16) -0.04545(17) 0.0435(6) Uani 1 1 d . . . . .
O23 O 0.17008(17) 0.73251(15) 0.26689(17) 0.0383(6) Uani 1 1 d . . . . .
O24 O 0.26248(17) 0.43873(14) 0.27475(18) 0.0410(6) Uani 1 1 d . . . . .
O25 O 0.21357(16) 0.61051(15) 0.00042(16) 0.0357(5) Uani 1 1 d . . . . .
O26 O 0.18284(15) 0.71386(14) 0.11183(16) 0.0333(5) Uani 1 1 d . . . . .
O27 O 0.22257(15) 0.59492(13) 0.23421(16) 0.0314(5) Uani 1 1 d . . . . .
O28 O 0.25231(16) 0.49051(14) 0.12325(16) 0.0340(5) Uani 1 1 d . . . . .
O29 O 0.80802(18) 0.82452(15) 0.59620(16) 0.0419(6) Uani 1 1 d . . . . .
O30 O 0.75720(18) 0.99192(15) 0.32424(17) 0.0407(6) Uani 1 1 d . . . . .
O31 O 0.83186(18) 0.74736(17) 0.18004(17) 0.0436(6) Uani 1 1 d . . . . .
O32 O 0.88562(17) 0.57701(16) 0.45410(17) 0.0424(6) Uani 1 1 d . . . . .
O33 O 0.78362(16) 0.87344(14) 0.44056(15) 0.0324(5) Uani 1 1 d . . . . .
O34 O 0.79199(15) 0.84765(14) 0.28399(15) 0.0323(5) Uani 1 1 d . . . . .
O35 O 0.84048(15) 0.69114(14) 0.32816(16) 0.0342(5) Uani 1 1 d . . . . .
O36 O 0.83377(15) 0.71640(14) 0.48685(15) 0.0338(5) Uani 1 1 d . . . . .
C1 C 0.4044(2) 0.64108(19) 0.3933(2) 0.0284(7) Uani 1 1 d . . . . .
C2 C 0.4914(2) 0.6663(2) 0.4810(2) 0.0339(7) Uani 1 1 d . . . . .
H2A H 0.529655 0.707603 0.467905 0.041 Uiso 1 1 calc R U . . .
H2B H 0.472392 0.693146 0.522344 0.041 Uiso 1 1 calc R U . . .
C3 C 0.6699(2) 0.6203(2) 0.4784(2) 0.0294(7) Uani 1 1 d . . . . .
C4 C 0.5946(2) 0.5662(2) 0.4835(2) 0.0330(7) Uani 1 1 d . . . . .
H4A H 0.547948 0.547451 0.421334 0.040 Uiso 1 1 calc R U . . .
H4B H 0.622734 0.517093 0.516265 0.040 Uiso 1 1 calc R U . . .
C5 C 0.4542(2) 0.46915(18) 0.2033(2) 0.0306(7) Uani 1 1 d . . . . .
C6 C 0.5549(2) 0.4479(2) 0.2456(2) 0.0357(8) Uani 1 1 d . . . . .
H6A H 0.593856 0.490446 0.293190 0.043 Uiso 1 1 calc R U . . .
H6B H 0.560316 0.395166 0.275069 0.043 Uiso 1 1 calc R U . . .
C7 C 0.6808(2) 0.5752(2) 0.2116(2) 0.0314(7) Uani 1 1 d . . . . .
C8 C 0.6020(2) 0.5155(2) 0.1466(2) 0.0372(8) Uani 1 1 d . . . . .
H8A H 0.543301 0.543127 0.123040 0.045 Uiso 1 1 calc R U . . .
H8B H 0.612909 0.502203 0.094780 0.045 Uiso 1 1 calc R U . . .
C9 C 0.3888(2) 0.6747(2) 0.0022(2) 0.0323(7) Uani 1 1 d . . . . .
C10 C 0.4725(2) 0.7011(2) -0.0106(2) 0.0374(8) Uani 1 1 d . . . . .
H10A H 0.529399 0.686797 0.043310 0.045 Uiso 1 1 calc R U . . .
H10B H 0.468232 0.669262 -0.063190 0.045 Uiso 1 1 calc R U . . .
C11 C 0.5997(2) 0.8368(2) 0.1301(2) 0.0316(7) Uani 1 1 d . . . . .
C12 C 0.5032(2) 0.8398(2) 0.0502(2) 0.0382(8) Uani 1 1 d . . . . .
H12A H 0.456558 0.827836 0.071292 0.046 Uiso 1 1 calc R U . . .
H12B H 0.496117 0.896330 0.029074 0.046 Uiso 1 1 calc R U . . .
C13 C 0.3350(2) 0.84531(19) 0.1915(2) 0.0317(7) Uani 1 1 d . . . . .
C14 C 0.4040(3) 0.9200(2) 0.2246(2) 0.0385(8) Uani 1 1 d . . . . .
H14A H 0.458472 0.907623 0.216668 0.046 Uiso 1 1 calc R U . . .
H14B H 0.374564 0.965583 0.185538 0.046 Uiso 1 1 calc R U . . .
C15 C 0.5851(2) 0.88149(19) 0.3930(2) 0.0299(7) Uani 1 1 d . . . . .
C16 C 0.4893(2) 0.8935(2) 0.3814(2) 0.0370(8) Uani 1 1 d . . . . .
H16A H 0.453751 0.839360 0.366178 0.044 Uiso 1 1 calc R U . . .
H16B H 0.495854 0.913545 0.440239 0.044 Uiso 1 1 calc R U . . .
N1 N 0.0556(2) 0.94244(17) 0.2958(2) 0.0356(6) Uani 1 1 d . . . . .
C17 C -0.0040(3) 1.0150(2) 0.2695(3) 0.0421(9) Uani 1 1 d . . . . .
H17A H 0.023815 1.056249 0.245022 0.050 Uiso 1 1 calc R U . . .
H17B H -0.000802 1.040086 0.325108 0.050 Uiso 1 1 calc R U . . .
C18 C -0.1059(3) 0.9975(3) 0.2010(3) 0.0509(10) Uani 1 1 d . . . . .
H18A H -0.135113 0.955898 0.223933 0.061 Uiso 1 1 calc R U . . .
H18B H -0.110901 0.975105 0.143647 0.061 Uiso 1 1 calc R U . . .
C19 C -0.1571(3) 1.0755(3) 0.1840(3) 0.0596(12) Uani 1 1 d . . . . .
H19A H -0.152966 1.096656 0.241459 0.072 Uiso 1 1 calc R U . . .
H19B H -0.125646 1.117496 0.163776 0.072 Uiso 1 1 calc R U . . .
C20 C -0.2580(4) 1.0633(4) 0.1143(4) 0.0800(17) Uani 1 1 d . . . . .
H20A H -0.262865 1.041359 0.057431 0.120 Uiso 1 1 calc R U . . .
H20B H -0.286211 1.115896 0.104406 0.120 Uiso 1 1 calc R U . . .
H20C H -0.290711 1.024692 0.135650 0.120 Uiso 1 1 calc R U . . .
C21 C 0.0520(3) 0.9001(2) 0.2130(3) 0.0409(8) Uani 1 1 d . . . . .
H21A H 0.086786 0.850341 0.231983 0.049 Uiso 1 1 calc R U . . .
H21B H -0.013687 0.882034 0.170895 0.049 Uiso 1 1 calc R U . . .
C22 C 0.0907(3) 0.9509(3) 0.1626(3) 0.0480(9) Uani 1 1 d . . . . .
H22A H 0.157288 0.967162 0.202902 0.058 Uiso 1 1 calc R U . . .
H22B H 0.057267 1.001405 0.143930 0.058 Uiso 1 1 calc R U . . .
C23 C 0.0805(3) 0.9034(3) 0.0795(3) 0.0526(10) Uani 1 1 d . . . . .
H23A H 0.013637 0.890325 0.037436 0.063 Uiso 1 1 calc R U . . .
H23B H 0.110190 0.851058 0.097836 0.063 Uiso 1 1 calc R U . . .
C24 C 0.1251(4) 0.9518(3) 0.0313(3) 0.0630(12) Uani 1 1 d . . . . .
H24A H 0.095918 1.003627 0.013234 0.094 Uiso 1 1 calc R U . . .
H24B H 0.116271 0.919892 -0.022398 0.094 Uiso 1 1 calc R U . . .
H24C H 0.191808 0.962975 0.072160 0.094 Uiso 1 1 calc R U . . .
C25 C 0.1545(3) 0.9747(2) 0.3613(3) 0.0402(8) Uani 1 1 d . . . . .
H25A H 0.177937 1.011552 0.329104 0.048 Uiso 1 1 calc R U . . .
H25B H 0.153196 1.007761 0.410504 0.048 Uiso 1 1 calc R U . . .
C26 C 0.2224(3) 0.9096(2) 0.4029(3) 0.0473(9) Uani 1 1 d . . . . .
H26A H 0.198380 0.870730 0.432990 0.057 Uiso 1 1 calc R U . . .
H26B H 0.227890 0.878569 0.354704 0.057 Uiso 1 1 calc R U . . .
C27 C 0.3170(3) 0.9470(3) 0.4708(3) 0.0556(11) Uani 1 1 d . . . . .
H27A H 0.309504 0.986947 0.511406 0.067 Uiso 1 1 calc R U . . .
H27B H 0.345906 0.977010 0.438555 0.067 Uiso 1 1 calc R U . . .
C28 C 0.3813(3) 0.8835(3) 0.5272(3) 0.0615(12) Uani 1 1 d . . . . .
H28A H 0.356420 0.857821 0.564530 0.092 Uiso 1 1 calc R U . . .
H28B H 0.443252 0.910199 0.566322 0.092 Uiso 1 1 calc R U . . .
H28C H 0.385600 0.841675 0.487254 0.092 Uiso 1 1 calc R U . . .
C29 C 0.0192(3) 0.8784(2) 0.3389(3) 0.0431(9) Uani 1 1 d . . . . .
H29A H -0.045448 0.859492 0.294614 0.052 Uiso 1 1 calc R U . . .
H29B H 0.057258 0.830698 0.351777 0.052 Uiso 1 1 calc R U . . .
C30 C 0.0200(3) 0.9073(3) 0.4246(3) 0.0597(12) Uani 1 1 d . . . . .
H30A H -0.032815 0.941470 0.410155 0.072 Uiso 1 1 calc R U . . .
H30B H 0.078429 0.941198 0.462585 0.072 Uiso 1 1 calc R U . . .
C31 C 0.0123(4) 0.8338(4) 0.4764(3) 0.086(2) Uani 1 1 d . . . . .
H31A H -0.049213 0.803933 0.439589 0.103 Uiso 1 1 calc R U . . .
H31B H 0.060195 0.796471 0.482191 0.103 Uiso 1 1 calc R U . . .
C32 C 0.0223(5) 0.8505(4) 0.5610(4) 0.098(2) Uani 1 1 d . . . . .
H32A H 0.082566 0.880682 0.598434 0.147 Uiso 1 1 calc R U . . .
H32B H 0.019116 0.798993 0.588742 0.147 Uiso 1 1 calc R U . . .
H32C H -0.027798 0.883602 0.556263 0.147 Uiso 1 1 calc R U . . .
N2 N -0.0035(2) 0.5417(2) 0.7304(2) 0.0450(8) Uani 1 1 d . . . . .
C33 C -0.0635(3) 0.6148(3) 0.6956(4) 0.0646(12) Uani 1 1 d . U . . .
H33A H -0.065667 0.628540 0.637471 0.078 Uiso 1 1 calc R U . . .
H33B H -0.127700 0.595824 0.681997 0.078 Uiso 1 1 calc R U . . .
C34 C -0.0379(4) 0.6937(4) 0.7532(5) 0.0874(14) Uani 1 1 d . U . . .
H34A H 0.027330 0.691679 0.800968 0.105 Uiso 1 1 calc R U . . .
H34B H -0.038460 0.738891 0.714539 0.105 Uiso 1 1 calc R U . . .
C35 C -0.0879(5) 0.7149(4) 0.7940(5) 0.0941(15) Uani 1 1 d . U . . .
H35A H -0.077414 0.674594 0.840493 0.113 Uiso 1 1 calc R U . . .
H35B H -0.154146 0.705943 0.748071 0.113 Uiso 1 1 calc R U . . .
C36 C -0.0772(4) 0.7955(3) 0.8376(3) 0.0599(11) Uani 1 1 d . U . . .
H36A H -0.010870 0.811931 0.875006 0.090 Uiso 1 1 calc R U . . .
H36B H -0.107901 0.793248 0.875708 0.090 Uiso 1 1 calc R U . . .
H36C H -0.105642 0.835503 0.791392 0.090 Uiso 1 1 calc R U . . .
C37 C -0.0337(3) 0.4792(2) 0.6525(3) 0.0446(8) Uani 1 1 d . U . . .
H37A H -0.023840 0.504964 0.604417 0.053 Uiso 1 1 calc R U . . .
H37B H 0.007347 0.433429 0.673815 0.053 Uiso 1 1 calc R U . . .
C38 C -0.1336(3) 0.4440(3) 0.6114(3) 0.0488(9) Uani 1 1 d . U . . .
H38A H -0.146341 0.422187 0.659454 0.059 Uiso 1 1 calc R U . . .
H38B H -0.175859 0.487872 0.582827 0.059 Uiso 1 1 calc R U . . .
C39 C -0.1520(4) 0.3770(3) 0.5421(3) 0.0675(11) Uani 1 1 d . U . . .
H39A H -0.110266 0.332999 0.571457 0.081 Uiso 1 1 calc R U . . .
H39B H -0.136953 0.398867 0.495491 0.081 Uiso 1 1 calc R U . . .
C40 C -0.2517(4) 0.3410(4) 0.4969(4) 0.0804(15) Uani 1 1 d . U . . .
H40A H -0.267020 0.318951 0.542628 0.121 Uiso 1 1 calc R U . . .
H40B H -0.259406 0.296887 0.453190 0.121 Uiso 1 1 calc R U . . .
H40C H -0.293289 0.383721 0.465547 0.121 Uiso 1 1 calc R U . . .
C41 C 0.0982(3) 0.5699(3) 0.7652(3) 0.0614(11) Uani 1 1 d . U . . .
H41A H 0.117613 0.607375 0.818929 0.074 Uiso 1 1 calc R U . . .
H41B H 0.135062 0.521468 0.785624 0.074 Uiso 1 1 calc R U . . .
C42 C 0.1233(4) 0.6124(4) 0.7005(4) 0.0802(13) Uani 1 1 d . U . . .
H42A H 0.114977 0.572646 0.651717 0.096 Uiso 1 1 calc R U . . .
H42B H 0.080585 0.656089 0.672519 0.096 Uiso 1 1 calc R U . . .
C43 C 0.2192(4) 0.6484(4) 0.7447(6) 0.1049(17) Uani 1 1 d D U . . .
H43A H 0.252599 0.622768 0.803316 0.126 Uiso 1 1 calc R U . . .
H43B H 0.248426 0.632344 0.707265 0.126 Uiso 1 1 calc R U . . .
C44 C 0.2356(6) 0.7340(4) 0.7614(7) 0.165(3) Uani 1 1 d D U . . .
H44A H 0.176084 0.759170 0.735613 0.248 Uiso 1 1 calc R U . . .
H44B H 0.272868 0.755591 0.733519 0.248 Uiso 1 1 calc R U . . .
H44C H 0.269396 0.746593 0.826717 0.248 Uiso 1 1 calc R U . . .
C45 C -0.0154(3) 0.5081(3) 0.8078(3) 0.0606(10) Uani 1 1 d . U . . .
H45A H 0.016438 0.547664 0.860439 0.073 Uiso 1 1 calc R U . . .
H45B H -0.082537 0.504348 0.790475 0.073 Uiso 1 1 calc R U . . .
C46 C 0.0208(3) 0.4264(4) 0.8362(3) 0.0682(11) Uani 1 1 d . U . . .
H46A H 0.084323 0.425839 0.842843 0.082 Uiso 1 1 calc R U . . .
H46B H -0.019677 0.383673 0.789677 0.082 Uiso 1 1 calc R U . . .
C47 C 0.0228(4) 0.4085(4) 0.9268(4) 0.0847(14) Uani 1 1 d . U . . .
H47A H 0.066143 0.449598 0.973858 0.102 Uiso 1 1 calc R U . . .
H47B H -0.040027 0.412941 0.920910 0.102 Uiso 1 1 calc R U . . .
C48 C 0.0533(5) 0.3242(5) 0.9550(5) 0.115(2) Uani 1 1 d . U . . .
H48A H 0.010400 0.283485 0.908456 0.173 Uiso 1 1 calc R U . . .
H48B H 0.053134 0.313920 1.012279 0.173 Uiso 1 1 calc R U . . .
H48C H 0.116281 0.320309 0.962661 0.173 Uiso 1 1 calc R U . . .
N3 N 0.5250(6) 0.2419(4) 0.2598(6) 0.155(3) Uani 1 1 d D . . . .
C49 C 0.5403(5) 0.1753(4) 0.2349(5) 0.0956(18) Uani 1 1 d D U . . .
C50 C 0.5554(5) 0.0967(3) 0.2107(5) 0.0994(19) Uani 1 1 d D U . . .
H50A H 0.556665 0.057921 0.255094 0.149 Uiso 1 1 calc R U . . .
H50B H 0.614941 0.098833 0.209565 0.149 Uiso 1 1 calc R U . . .
H50C H 0.504946 0.078776 0.150777 0.149 Uiso 1 1 calc R U . . .
N4 N 0.2941(6) 0.0843(4) 0.2656(7) 0.172(3) Uani 1 1 d D U . . .
C51 C 0.3205(5) 0.1574(4) 0.2879(6) 0.111(2) Uani 1 1 d D U . . .
C52 C 0.3461(5) 0.2415(4) 0.3062(5) 0.105(2) Uani 1 1 d D U . . .
H52A H 0.406527 0.253427 0.307915 0.158 Uiso 1 1 calc R U . . .
H52B H 0.350721 0.257619 0.364697 0.158 Uiso 1 1 calc R U . . .
H52C H 0.299095 0.272112 0.258714 0.158 Uiso 1 1 calc R U . . .
N5 N 0.6774(6) 0.7233(5) 0.9453(6) 0.155(3) Uani 1 1 d D U . . .
C53 C 0.7000(8) 0.7991(6) 0.9524(8) 0.167(3) Uani 1 1 d D U . . .
C54 C 0.6877(10) 0.8840(5) 0.9520(9) 0.204(4) Uani 1 1 d D U . . .
H54A H 0.683664 0.905884 0.896326 0.307 Uiso 1 1 calc R U . . .
H54B H 0.740786 0.912146 1.004309 0.307 Uiso 1 1 calc R U . . .
H54C H 0.630290 0.892644 0.954926 0.307 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
V1 O21 1.585(2) . ?
V1 O25 1.729(2) . ?
V1 O28 1.907(2) . ?
V1 O11 1.991(2) . ?
V1 O6 2.049(2) . ?
V2 O22 1.584(2) . ?
V2 O26 1.735(2) . ?
V2 O25 1.903(2) . ?
V2 O16 1.983(2) . ?
V2 O12 2.045(2) . ?
V3 O23 1.591(2) . ?
V3 O27 1.729(2) . ?
V3 O26 1.887(2) . ?
V3 O1 1.983(2) . ?
V3 O17 2.061(2) . ?
V4 O24 1.592(2) . ?
V4 O28 1.735(2) . ?
V4 O27 1.901(2) . ?
V4 O7 1.978(2) . ?
V4 O2 2.056(2) . ?
V5 O29 1.588(2) . ?
V5 O33 1.739(2) . ?
V5 O36 1.896(2) . ?
V5 O19 1.986(2) . ?
V5 O4 2.047(2) . ?
V6 O30 1.585(2) . ?
V6 O34 1.734(2) . ?
V6 O33 1.890(2) . ?
V6 O14 1.981(2) . ?
V6 O20 2.052(2) . ?
V7 O31 1.586(2) . ?
V7 O35 1.737(2) . ?
V7 O34 1.901(2) . ?
V7 O9 1.976(2) . ?
V7 O15 2.059(2) . ?
V8 O32 1.588(2) . ?
V8 O36 1.743(2) . ?
V8 O35 1.895(2) . ?
V8 O5 1.998(2) . ?
V8 O10 2.053(2) . ?
O1 C1 1.274(4) . ?
O2 C1 1.244(4) . ?
O3 C2 1.409(4) . ?
O3 C4 1.422(4) . ?
O4 C3 1.253(4) . ?
O5 C3 1.269(4) . ?
O6 C5 1.245(4) . ?
O7 C5 1.279(4) . ?
O8 C8 1.409(4) . ?
O8 C6 1.418(4) . ?
O9 C7 1.273(4) . ?
O10 C7 1.245(4) . ?
O11 C9 1.277(4) . ?
O12 C9 1.246(4) . ?
O13 C12 1.411(4) . ?
O13 C10 1.417(4) . ?
O14 C11 1.272(4) . ?
O15 C11 1.248(4) . ?
O16 C13 1.268(4) . ?
O17 C13 1.251(4) . ?
O18 C16 1.403(4) . ?
O18 C14 1.418(4) . ?
O19 C15 1.273(4) . ?
O20 C15 1.250(4) . ?
C1 C2 1.517(5) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 C4 1.509(4) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 C6 1.518(5) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 C8 1.516(5) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 C10 1.518(5) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 C12 1.521(5) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C13 C14 1.518(5) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C15 C16 1.508(5) . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
N1 C21 1.516(5) . ?
N1 C17 1.518(4) . ?
N1 C25 1.519(5) . ?
N1 C29 1.528(4) . ?
C17 C18 1.519(6) . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C18 C19 1.526(6) . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C19 C20 1.505(7) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 C22 1.508(5) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C22 C23 1.519(6) . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C23 C24 1.522(6) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 C26 1.512(5) . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C26 C27 1.508(5) . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C27 C28 1.518(7) . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 C30 1.500(6) . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C30 C31 1.529(6) . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C31 C32 1.372(8) . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
N2 C45 1.509(5) . ?
N2 C37 1.515(5) . ?
N2 C41 1.517(5) . ?
N2 C33 1.535(6) . ?
C33 C34 1.514(7) . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
C34 C35 1.344(8) . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
C35 C36 1.459(7) . ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C37 C38 1.512(6) . ?
C37 H37A 0.9900 . ?
C37 H37B 0.9900 . ?
C38 C39 1.496(6) . ?
C38 H38A 0.9900 . ?
C38 H38B 0.9900 . ?
C39 C40 1.512(7) . ?
C39 H39A 0.9900 . ?
C39 H39B 0.9900 . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C40 H40C 0.9800 . ?
C41 C42 1.498(7) . ?
C41 H41A 0.9900 . ?
C41 H41B 0.9900 . ?
C42 C43 1.462(8) . ?
C42 H42A 0.9900 . ?
C42 H42B 0.9900 . ?
C43 C44 1.409(5) . ?
C43 H43A 0.9900 . ?
C43 H43B 0.9900 . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 0.9800 . ?
C45 C46 1.489(8) . ?
C45 H45A 0.9900 . ?
C45 H45B 0.9900 . ?
C46 C47 1.539(7) . ?
C46 H46A 0.9900 . ?
C46 H46B 0.9900 . ?
C47 C48 1.502(10) . ?
C47 H47A 0.9900 . ?
C47 H47B 0.9900 . ?
C48 H48A 0.9800 . ?
C48 H48B 0.9800 . ?
C48 H48C 0.9800 . ?
N3 C49 1.242(7) . ?
C49 C50 1.413(6) . ?
C50 H50A 0.9800 . ?
C50 H50B 0.9800 . ?
C50 H50C 0.9800 . ?
N4 C51 1.237(7) . ?
C51 C52 1.402(7) . ?
C52 H52A 0.9800 . ?
C52 H52B 0.9800 . ?
C52 H52C 0.9800 . ?
N5 C53 1.262(7) . ?
C53 C54 1.416(7) . ?
C54 H54A 0.9800 . ?
C54 H54B 0.9800 . ?
C54 H54C 0.9800 . ?

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
O21 V1 O25 103.38(13) . . ?
O21 V1 O28 102.40(12) . . ?
O25 V1 O28 98.20(11) . . ?
O21 V1 O11 99.11(12) . . ?
O25 V1 O11 91.58(11) . . ?
O28 V1 O11 153.53(10) . . ?
O21 V1 O6 96.21(12) . . ?
O25 V1 O6 159.49(10) . . ?
O28 V1 O6 83.27(10) . . ?
O11 V1 O6 79.23(10) . . ?
O22 V2 O26 104.02(13) . . ?
O22 V2 O25 100.90(12) . . ?
O26 V2 O25 97.45(11) . . ?
O22 V2 O16 100.34(12) . . ?
O26 V2 O16 91.55(10) . . ?
O25 V2 O16 154.13(10) . . ?
O22 V2 O12 97.03(12) . . ?
O26 V2 O12 158.10(10) . . ?
O25 V2 O12 84.25(10) . . ?
O16 V2 O12 78.65(10) . . ?
O23 V3 O27 102.77(12) . . ?
O23 V3 O26 102.57(12) . . ?
O27 V3 O26 98.07(11) . . ?
O23 V3 O1 99.85(11) . . ?
O27 V3 O1 91.90(10) . . ?
O26 V3 O1 152.72(10) . . ?
O23 V3 O17 96.41(11) . . ?
O27 V3 O17 159.79(10) . . ?
O26 V3 O17 83.75(10) . . ?
O1 V3 O17 78.46(9) . . ?
O24 V4 O28 104.24(12) . . ?
O24 V4 O27 100.65(12) . . ?
O28 V4 O27 97.33(11) . . ?
O24 V4 O7 100.89(11) . . ?
O28 V4 O7 92.15(10) . . ?
O27 V4 O7 153.50(10) . . ?
O24 V4 O2 96.62(12) . . ?
O28 V4 O2 158.63(10) . . ?
O27 V4 O2 83.10(9) . . ?
O7 V4 O2 79.25(9) . . ?
O29 V5 O33 102.62(12) . . ?
O29 V5 O36 102.15(12) . . ?
O33 V5 O36 98.61(11) . . ?
O29 V5 O19 99.87(12) . . ?
O33 V5 O19 91.28(10) . . ?
O36 V5 O19 153.19(10) . . ?
O29 V5 O4 96.45(11) . . ?
O33 V5 O4 159.84(10) . . ?
O36 V5 O4 83.55(10) . . ?
O19 V5 O4 78.94(9) . . ?
O30 V6 O34 103.77(13) . . ?
O30 V6 O33 100.71(12) . . ?
O34 V6 O33 97.28(11) . . ?
O30 V6 O14 100.66(12) . . ?
O34 V6 O14 91.89(10) . . ?
O33 V6 O14 153.98(10) . . ?
O30 V6 O20 98.21(12) . . ?
O34 V6 O20 157.30(10) . . ?
O33 V6 O20 83.99(10) . . ?
O14 V6 O20 78.42(10) . . ?
O31 V7 O35 103.40(13) . . ?
O31 V7 O34 100.82(12) . . ?
O35 V7 O34 97.54(11) . . ?
O31 V7 O9 101.09(12) . . ?
O35 V7 O9 91.65(11) . . ?
O34 V7 O9 153.53(10) . . ?
O31 V7 O15 97.26(12) . . ?
O35 V7 O15 158.56(10) . . ?
O34 V7 O15 83.99(10) . . ?
O9 V7 O15 78.68(10) . . ?
O32 V8 O36 103.51(13) . . ?
O32 V8 O35 101.76(12) . . ?
O36 V8 O35 97.75(11) . . ?
O32 V8 O5 99.84(12) . . ?
O36 V8 O5 90.96(10) . . ?
O35 V8 O5 154.06(10) . . ?
O32 V8 O10 97.16(12) . . ?
O36 V8 O10 158.51(10) . . ?
O35 V8 O10 83.52(10) . . ?
O5 V8 O10 79.68(10) . . ?
C1 O1 V3 127.8(2) . . ?
C1 O2 V4 133.5(2) . . ?
C2 O3 C4 116.3(2) . . ?
C3 O4 V5 133.4(2) . . ?
C3 O5 V8 128.5(2) . . ?
C5 O6 V1 133.6(2) . . ?
C5 O7 V4 127.3(2) . . ?
C8 O8 C6 115.8(3) . . ?
C7 O9 V7 127.9(2) . . ?
C7 O10 V8 132.6(2) . . ?
C9 O11 V1 128.5(2) . . ?
C9 O12 V2 133.7(2) . . ?
C12 O13 C10 116.2(3) . . ?
C11 O14 V6 128.3(2) . . ?
C11 O15 V7 133.5(2) . . ?
C13 O16 V2 128.5(2) . . ?
C13 O17 V3 132.1(2) . . ?
C16 O18 C14 116.0(3) . . ?
C15 O19 V5 128.5(2) . . ?
C15 O20 V6 133.1(2) . . ?
V1 O25 V2 127.44(13) . . ?
V2 O26 V3 127.83(13) . . ?
V3 O27 V4 128.63(12) . . ?
V4 O28 V1 127.17(12) . . ?
V5 O33 V6 128.12(12) . . ?
V6 O34 V7 128.14(12) . . ?
V7 O35 V8 127.97(13) . . ?
V8 O36 V5 127.52(13) . . ?
O2 C1 O1 126.9(3) . . ?
O2 C1 C2 119.9(3) . . ?
O1 C1 C2 113.2(3) . . ?
O3 C2 C1 116.1(3) . . ?
O3 C2 H2A 108.3 . . ?
C1 C2 H2A 108.3 . . ?
O3 C2 H2B 108.3 . . ?
C1 C2 H2B 108.3 . . ?
H2A C2 H2B 107.4 . . ?
O4 C3 O5 126.2(3) . . ?
O4 C3 C4 119.3(3) . . ?
O5 C3 C4 114.4(3) . . ?
O3 C4 C3 115.7(3) . . ?
O3 C4 H4A 108.4 . . ?
C3 C4 H4A 108.4 . . ?
O3 C4 H4B 108.4 . . ?
C3 C4 H4B 108.4 . . ?
H4A C4 H4B 107.4 . . ?
O6 C5 O7 126.8(3) . . ?
O6 C5 C6 119.7(3) . . ?
O7 C5 C6 113.4(3) . . ?
O8 C6 C5 113.8(3) . . ?
O8 C6 H6A 108.8 . . ?
C5 C6 H6A 108.8 . . ?
O8 C6 H6B 108.8 . . ?
C5 C6 H6B 108.8 . . ?
H6A C6 H6B 107.7 . . ?
O10 C7 O9 127.1(3) . . ?
O10 C7 C8 120.2(3) . . ?
O9 C7 C8 112.7(3) . . ?
O8 C8 C7 115.6(3) . . ?
O8 C8 H8A 108.4 . . ?
C7 C8 H8A 108.4 . . ?
O8 C8 H8B 108.4 . . ?
C7 C8 H8B 108.4 . . ?
H8A C8 H8B 107.4 . . ?
O12 C9 O11 126.1(3) . . ?
O12 C9 C10 120.6(3) . . ?
O11 C9 C10 113.2(3) . . ?
O13 C10 C9 115.4(3) . . ?
O13 C10 H10A 108.4 . . ?
C9 C10 H10A 108.4 . . ?
O13 C10 H10B 108.4 . . ?
C9 C10 H10B 108.4 . . ?
H10A C10 H10B 107.5 . . ?
O15 C11 O14 126.5(3) . . ?
O15 C11 C12 120.4(3) . . ?
O14 C11 C12 113.1(3) . . ?
O13 C12 C11 115.6(3) . . ?
O13 C12 H12A 108.4 . . ?
C11 C12 H12A 108.4 . . ?
O13 C12 H12B 108.4 . . ?
C11 C12 H12B 108.4 . . ?
H12A C12 H12B 107.4 . . ?
O17 C13 O16 127.0(3) . . ?
O17 C13 C14 119.9(3) . . ?
O16 C13 C14 113.1(3) . . ?
O18 C14 C13 116.1(3) . . ?
O18 C14 H14A 108.3 . . ?
C13 C14 H14A 108.3 . . ?
O18 C14 H14B 108.3 . . ?
C13 C14 H14B 108.3 . . ?
H14A C14 H14B 107.4 . . ?
O20 C15 O19 126.6(3) . . ?
O20 C15 C16 120.2(3) . . ?
O19 C15 C16 113.2(3) . . ?
O18 C16 C15 116.5(3) . . ?
O18 C16 H16A 108.2 . . ?
C15 C16 H16A 108.2 . . ?
O18 C16 H16B 108.2 . . ?
C15 C16 H16B 108.2 . . ?
H16A C16 H16B 107.3 . . ?
C21 N1 C17 110.7(3) . . ?
C21 N1 C25 110.7(3) . . ?
C17 N1 C25 107.5(3) . . ?
C21 N1 C29 106.4(3) . . ?
C17 N1 C29 110.7(3) . . ?
C25 N1 C29 110.9(3) . . ?
N1 C17 C18 116.6(3) . . ?
N1 C17 H17A 108.1 . . ?
C18 C17 H17A 108.1 . . ?
N1 C17 H17B 108.1 . . ?
C18 C17 H17B 108.1 . . ?
H17A C17 H17B 107.3 . . ?
C17 C18 C19 110.5(4) . . ?
C17 C18 H18A 109.6 . . ?
C19 C18 H18A 109.6 . . ?
C17 C18 H18B 109.6 . . ?
C19 C18 H18B 109.6 . . ?
H18A C18 H18B 108.1 . . ?
C20 C19 C18 113.4(5) . . ?
C20 C19 H19A 108.9 . . ?
C18 C19 H19A 108.9 . . ?
C20 C19 H19B 108.9 . . ?
C18 C19 H19B 108.9 . . ?
H19A C19 H19B 107.7 . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C22 C21 N1 115.5(3) . . ?
C22 C21 H21A 108.4 . . ?
N1 C21 H21A 108.4 . . ?
C22 C21 H21B 108.4 . . ?
N1 C21 H21B 108.4 . . ?
H21A C21 H21B 107.5 . . ?
C21 C22 C23 110.9(3) . . ?
C21 C22 H22A 109.5 . . ?
C23 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
C23 C22 H22B 109.5 . . ?
H22A C22 H22B 108.0 . . ?
C22 C23 C24 111.6(4) . . ?
C22 C23 H23A 109.3 . . ?
C24 C23 H23A 109.3 . . ?
C22 C23 H23B 109.3 . . ?
C24 C23 H23B 109.3 . . ?
H23A C23 H23B 108.0 . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C26 C25 N1 115.0(3) . . ?
C26 C25 H25A 108.5 . . ?
N1 C25 H25A 108.5 . . ?
C26 C25 H25B 108.5 . . ?
N1 C25 H25B 108.5 . . ?
H25A C25 H25B 107.5 . . ?
C27 C26 C25 111.2(3) . . ?
C27 C26 H26A 109.4 . . ?
C25 C26 H26A 109.4 . . ?
C27 C26 H26B 109.4 . . ?
C25 C26 H26B 109.4 . . ?
H26A C26 H26B 108.0 . . ?
C26 C27 C28 112.7(4) . . ?
C26 C27 H27A 109.1 . . ?
C28 C27 H27A 109.1 . . ?
C26 C27 H27B 109.1 . . ?
C28 C27 H27B 109.1 . . ?
H27A C27 H27B 107.8 . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C30 C29 N1 115.1(3) . . ?
C30 C29 H29A 108.5 . . ?
N1 C29 H29A 108.5 . . ?
C30 C29 H29B 108.5 . . ?
N1 C29 H29B 108.5 . . ?
H29A C29 H29B 107.5 . . ?
C29 C30 C31 110.0(4) . . ?
C29 C30 H30A 109.7 . . ?
C31 C30 H30A 109.7 . . ?
C29 C30 H30B 109.7 . . ?
C31 C30 H30B 109.7 . . ?
H30A C30 H30B 108.2 . . ?
C32 C31 C30 116.7(6) . . ?
C32 C31 H31A 108.1 . . ?
C30 C31 H31A 108.1 . . ?
C32 C31 H31B 108.1 . . ?
C30 C31 H31B 108.1 . . ?
H31A C31 H31B 107.3 . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C45 N2 C37 112.5(3) . . ?
C45 N2 C41 108.3(3) . . ?
C37 N2 C41 109.6(3) . . ?
C45 N2 C33 108.4(4) . . ?
C37 N2 C33 108.2(3) . . ?
C41 N2 C33 109.8(3) . . ?
C34 C33 N2 120.2(4) . . ?
C34 C33 H33A 107.3 . . ?
N2 C33 H33A 107.3 . . ?
C34 C33 H33B 107.3 . . ?
N2 C33 H33B 107.3 . . ?
H33A C33 H33B 106.9 . . ?
C35 C34 C33 120.7(6) . . ?
C35 C34 H34A 107.2 . . ?
C33 C34 H34A 107.2 . . ?
C35 C34 H34B 107.2 . . ?
C33 C34 H34B 107.2 . . ?
H34A C34 H34B 106.8 . . ?
C34 C35 C36 123.5(6) . . ?
C34 C35 H35A 106.4 . . ?
C36 C35 H35A 106.4 . . ?
C34 C35 H35B 106.4 . . ?
C36 C35 H35B 106.4 . . ?
H35A C35 H35B 106.5 . . ?
C35 C36 H36A 109.5 . . ?
C35 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C35 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C38 C37 N2 115.8(3) . . ?
C38 C37 H37A 108.3 . . ?
N2 C37 H37A 108.3 . . ?
C38 C37 H37B 108.3 . . ?
N2 C37 H37B 108.3 . . ?
H37A C37 H37B 107.4 . . ?
C39 C38 C37 110.7(4) . . ?
C39 C38 H38A 109.5 . . ?
C37 C38 H38A 109.5 . . ?
C39 C38 H38B 109.5 . . ?
C37 C38 H38B 109.5 . . ?
H38A C38 H38B 108.1 . . ?
C38 C39 C40 113.0(4) . . ?
C38 C39 H39A 109.0 . . ?
C40 C39 H39A 109.0 . . ?
C38 C39 H39B 109.0 . . ?
C40 C39 H39B 109.0 . . ?
H39A C39 H39B 107.8 . . ?
C39 C40 H40A 109.5 . . ?
C39 C40 H40B 109.5 . . ?
H40A C40 H40B 109.5 . . ?
C39 C40 H40C 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
C42 C41 N2 116.7(4) . . ?
C42 C41 H41A 108.1 . . ?
N2 C41 H41A 108.1 . . ?
C42 C41 H41B 108.1 . . ?
N2 C41 H41B 108.1 . . ?
H41A C41 H41B 107.3 . . ?
C43 C42 C41 112.2(5) . . ?
C43 C42 H42A 109.2 . . ?
C41 C42 H42A 109.2 . . ?
C43 C42 H42B 109.2 . . ?
C41 C42 H42B 109.2 . . ?
H42A C42 H42B 107.9 . . ?
C44 C43 C42 119.0(7) . . ?
C44 C43 H43A 107.6 . . ?
C42 C43 H43A 107.6 . . ?
C44 C43 H43B 107.6 . . ?
C42 C43 H43B 107.6 . . ?
H43A C43 H43B 107.0 . . ?
C43 C44 H44A 109.5 . . ?
C43 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
C43 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
C46 C45 N2 115.3(4) . . ?
C46 C45 H45A 108.4 . . ?
N2 C45 H45A 108.4 . . ?
C46 C45 H45B 108.4 . . ?
N2 C45 H45B 108.4 . . ?
H45A C45 H45B 107.5 . . ?
C45 C46 C47 109.3(5) . . ?
C45 C46 H46A 109.8 . . ?
C47 C46 H46A 109.8 . . ?
C45 C46 H46B 109.8 . . ?
C47 C46 H46B 109.8 . . ?
H46A C46 H46B 108.3 . . ?
C48 C47 C46 111.0(6) . . ?
C48 C47 H47A 109.4 . . ?
C46 C47 H47A 109.4 . . ?
C48 C47 H47B 109.4 . . ?
C46 C47 H47B 109.4 . . ?
H47A C47 H47B 108.0 . . ?
C47 C48 H48A 109.5 . . ?
C47 C48 H48B 109.5 . . ?
H48A C48 H48B 109.5 . . ?
C47 C48 H48C 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?
N3 C49 C50 175.7(8) . . ?
C49 C50 H50A 109.5 . . ?
C49 C50 H50B 109.5 . . ?
H50A C50 H50B 109.5 . . ?
C49 C50 H50C 109.5 . . ?
H50A C50 H50C 109.5 . . ?
H50B C50 H50C 109.5 . . ?
N4 C51 C52 175.6(10) . . ?
C51 C52 H52A 109.5 . . ?
C51 C52 H52B 109.5 . . ?
H52A C52 H52B 109.5 . . ?
C51 C52 H52C 109.5 . . ?
H52A C52 H52C 109.5 . . ?
H52B C52 H52C 109.5 . . ?
N5 C53 C54 157.2(12) . . ?
C53 C54 H54A 109.5 . . ?
C53 C54 H54B 109.5 . . ?
H54A C54 H54B 109.5 . . ?
C53 C54 H54C 109.5 . . ?
H54A C54 H54C 109.5 . . ?
H54B C54 H54C 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
O21 V1 O25 V2 -159.88(17) . . . . ?
O28 V1 O25 V2 95.21(17) . . . . ?
O11 V1 O25 V2 -60.13(17) . . . . ?
O6 V1 O25 V2 2.5(4) . . . . ?
O22 V2 O26 V3 -161.30(16) . . . . ?
O25 V2 O26 V3 95.45(16) . . . . ?
O16 V2 O26 V3 -60.24(16) . . . . ?
O12 V2 O26 V3 2.3(4) . . . . ?
O23 V3 O26 V2 157.66(16) . . . . ?
O27 V3 O26 V2 -97.25(17) . . . . ?
O1 V3 O26 V2 13.1(3) . . . . ?
O17 V3 O26 V2 62.46(16) . . . . ?
O23 V3 O27 V4 -160.23(17) . . . . ?
O26 V3 O27 V4 94.85(17) . . . . ?
O1 V3 O27 V4 -59.68(17) . . . . ?
O17 V3 O27 V4 1.0(4) . . . . ?
O24 V4 O28 V1 -162.58(16) . . . . ?
O27 V4 O28 V1 94.43(16) . . . . ?
O7 V4 O28 V1 -60.77(16) . . . . ?
O2 V4 O28 V1 4.6(4) . . . . ?
O29 V5 O33 V6 -160.74(17) . . . . ?
O36 V5 O33 V6 94.67(17) . . . . ?
O19 V5 O33 V6 -60.33(17) . . . . ?
O4 V5 O33 V6 -0.1(4) . . . . ?
O30 V6 O33 V5 158.67(18) . . . . ?
O34 V6 O33 V5 -95.77(18) . . . . ?
O14 V6 O33 V5 13.9(4) . . . . ?
O20 V6 O33 V5 61.42(17) . . . . ?
O30 V6 O34 V7 -161.21(16) . . . . ?
O33 V6 O34 V7 95.84(16) . . . . ?
O14 V6 O34 V7 -59.76(16) . . . . ?
O20 V6 O34 V7 4.0(4) . . . . ?
O31 V7 O35 V8 -162.10(17) . . . . ?
O34 V7 O35 V8 94.82(17) . . . . ?
O9 V7 O35 V8 -60.29(17) . . . . ?
O15 V7 O35 V8 2.1(4) . . . . ?
O32 V8 O35 V7 157.59(17) . . . . ?
O36 V8 O35 V7 -96.79(17) . . . . ?
O5 V8 O35 V7 11.8(3) . . . . ?
O10 V8 O35 V7 61.59(17) . . . . ?
O32 V8 O36 V5 -161.41(16) . . . . ?
O35 V8 O36 V5 94.44(16) . . . . ?
O5 V8 O36 V5 -61.05(16) . . . . ?
O10 V8 O36 V5 2.4(4) . . . . ?
O29 V5 O36 V8 157.94(16) . . . . ?
O33 V5 O36 V8 -97.07(16) . . . . ?
O19 V5 O36 V8 13.4(3) . . . . ?
O4 V5 O36 V8 62.71(16) . . . . ?
V4 O2 C1 O1 14.9(5) . . . . ?
V4 O2 C1 C2 -163.8(2) . . . . ?
V3 O1 C1 O2 -5.9(5) . . . . ?
V3 O1 C1 C2 172.9(2) . . . . ?
C4 O3 C2 C1 68.4(4) . . . . ?
O2 C1 C2 O3 -4.1(4) . . . . ?
O1 C1 C2 O3 177.1(3) . . . . ?
V5 O4 C3 O5 14.5(5) . . . . ?
V5 O4 C3 C4 -164.0(2) . . . . ?
V8 O5 C3 O4 -6.3(5) . . . . ?
V8 O5 C3 C4 172.3(2) . . . . ?
C2 O3 C4 C3 67.6(4) . . . . ?
O4 C3 C4 O3 -2.2(4) . . . . ?
O5 C3 C4 O3 179.2(3) . . . . ?
V1 O6 C5 O7 15.9(5) . . . . ?
V1 O6 C5 C6 -163.3(2) . . . . ?
V4 O7 C5 O6 -7.7(5) . . . . ?
V4 O7 C5 C6 171.5(2) . . . . ?
C8 O8 C6 C5 68.9(4) . . . . ?
O6 C5 C6 O8 -1.9(4) . . . . ?
O7 C5 C6 O8 178.8(3) . . . . ?
V8 O10 C7 O9 17.7(5) . . . . ?
V8 O10 C7 C8 -159.8(2) . . . . ?
V7 O9 C7 O10 -9.6(5) . . . . ?
V7 O9 C7 C8 168.1(2) . . . . ?
C6 O8 C8 C7 70.7(4) . . . . ?
O10 C7 C8 O8 -8.0(4) . . . . ?
O9 C7 C8 O8 174.2(3) . . . . ?
V2 O12 C9 O11 11.9(5) . . . . ?
V2 O12 C9 C10 -166.9(2) . . . . ?
V1 O11 C9 O12 -5.2(5) . . . . ?
V1 O11 C9 C10 173.7(2) . . . . ?
C12 O13 C10 C9 67.2(4) . . . . ?
O12 C9 C10 O13 -2.9(4) . . . . ?
O11 C9 C10 O13 178.2(3) . . . . ?
V7 O15 C11 O14 14.2(5) . . . . ?
V7 O15 C11 C12 -163.2(2) . . . . ?
V6 O14 C11 O15 -8.4(5) . . . . ?
V6 O14 C11 C12 169.2(2) . . . . ?
C10 O13 C12 C11 69.2(4) . . . . ?
O15 C11 C12 O13 -5.6(5) . . . . ?
O14 C11 C12 O13 176.7(3) . . . . ?
V3 O17 C13 O16 14.8(5) . . . . ?
V3 O17 C13 C14 -164.1(2) . . . . ?
V2 O16 C13 O17 -5.6(5) . . . . ?
V2 O16 C13 C14 173.4(2) . . . . ?
C16 O18 C14 C13 64.7(4) . . . . ?
O17 C13 C14 O18 1.4(5) . . . . ?
O16 C13 C14 O18 -177.7(3) . . . . ?
V6 O20 C15 O19 12.1(5) . . . . ?
V6 O20 C15 C16 -167.1(2) . . . . ?
V5 O19 C15 O20 -5.3(5) . . . . ?
V5 O19 C15 C16 174.0(2) . . . . ?
C14 O18 C16 C15 70.2(4) . . . . ?
O20 C15 C16 O18 -5.0(4) . . . . ?
O19 C15 C16 O18 175.7(3) . . . . ?
C21 N1 C17 C18 56.7(4) . . . . ?
C25 N1 C17 C18 177.8(3) . . . . ?
C29 N1 C17 C18 -61.0(4) . . . . ?
N1 C17 C18 C19 178.2(3) . . . . ?
C17 C18 C19 C20 178.1(4) . . . . ?
C17 N1 C21 C22 63.3(4) . . . . ?
C25 N1 C21 C22 -55.8(4) . . . . ?
C29 N1 C21 C22 -176.4(3) . . . . ?
N1 C21 C22 C23 -178.1(3) . . . . ?
C21 C22 C23 C24 -176.2(4) . . . . ?
C21 N1 C25 C26 -65.3(4) . . . . ?
C17 N1 C25 C26 173.7(3) . . . . ?
C29 N1 C25 C26 52.6(4) . . . . ?
N1 C25 C26 C27 -176.7(3) . . . . ?
C25 C26 C27 C28 168.6(4) . . . . ?
C21 N1 C29 C30 178.0(3) . . . . ?
C17 N1 C29 C30 -61.6(4) . . . . ?
C25 N1 C29 C30 57.5(4) . . . . ?
N1 C29 C30 C31 -162.1(4) . . . . ?
C29 C30 C31 C32 173.2(5) . . . . ?
C45 N2 C33 C34 69.1(6) . . . . ?
C37 N2 C33 C34 -168.6(5) . . . . ?
C41 N2 C33 C34 -49.1(6) . . . . ?
N2 C33 C34 C35 -106.9(7) . . . . ?
C33 C34 C35 C36 -169.4(6) . . . . ?
C45 N2 C37 C38 58.4(4) . . . . ?
C41 N2 C37 C38 179.0(3) . . . . ?
C33 N2 C37 C38 -61.4(4) . . . . ?
N2 C37 C38 C39 -174.0(4) . . . . ?
C37 C38 C39 C40 -178.5(4) . . . . ?
C45 N2 C41 C42 -174.6(5) . . . . ?
C37 N2 C41 C42 62.3(5) . . . . ?
C33 N2 C41 C42 -56.4(6) . . . . ?
N2 C41 C42 C43 170.8(5) . . . . ?
C41 C42 C43 C44 -105.4(9) . . . . ?
C37 N2 C45 C46 47.3(5) . . . . ?
C41 N2 C45 C46 -73.9(5) . . . . ?
C33 N2 C45 C46 167.0(4) . . . . ?
N2 C45 C46 C47 168.2(4) . . . . ?
C45 C46 C47 C48 176.4(5) . . . . ?

_refine_diff_density_max         1.541
_refine_diff_density_min         -0.810
_refine_diff_density_rms         0.081


#==============================================================================0
# start Validation Reply Form



_vrf_PLAT223_1                   
;
PROBLEM:
Alert level C
PLAT223_ALERT_4_C Solv./Anion Resd 3   H   Ueq(max)/Ueq(min) Range        4.7 Ratio 

RESPONSE: 
Even at 193(2) K there are some carbon and nitrogen atoms severely affected by 
thermal disorder. This C alert is likely to be due to some structural disorder 
associated with some carbon atoms of tetrabutyl groups of the tetrabutylammonium 
cations and also with carbon and nitrogen atoms of the acetonitrile molecules of 
crystallization. Attempts to model these molecules over two or more distinct 
crystallographic positions did not lead to reasonable structural models. 
;


_vrf_PLAT241_1                   
;
PROBLEM:
Alert level C
PLAT241_ALERT_2_C High   'MainMol' Ueq as Compared to Neighbors of      C35 Check 

RESPONSE: Please see our response to Alert _vrf_PLAT223
;

_vrf_PLAT242_1                   
;
PROBLEM:
Alert level C
PLAT242_ALERT_2_C Low    'MainMol' Ueq as Compared to Neighbors of       C43Check

RESPONSE: Please see our response to Alert _vrf_PLAT223
;


_vrf_PLAT244_1                   
;
PROBLEM:
Alert level C
PLAT244_ALERT_4_C Low    'MainMol' Ueq as Compared to Neighbors of       C49Check

RESPONSE: Please see our response to Alert _vrf_PLAT223. 
;


_vrf_PLAT341_1                   
;
PROBLEM:
Alert level C
PLAT341_ALERT_3_C Low Bond Precision on  C-C Bonds ...............   0.00749 Ang.
RESPONSE: 
The crystal was not of very good quality despite being the best selected from
the sample supplied. The crystal structure shows distinct thermal displacements 
of outer atoms. So that some shelxl restraints(DELU, SIMU, ..) were used to 
make the structure more plausible.
;


_vrf_PLAT360_1                   
;
PROBLEM:
Alert level C
PLAT360_ALERT_2_C Short  C(sp3)-C(sp3) Bond   C31    -   C32    ..       1.37 Ang. 

RESPONSE: Please see our response to Alert _vrf_PLAT223. 

;
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_3
_database_code_depnum_ccdc_archive 'CCDC 1573270'
_audit_update_record             
;
2017-09-07 deposited with the CCDC.
2018-01-09 downloaded from the CCDC.
;


_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C10 H12 F O16 V4, C16 H36 N'
_chemical_formula_sum            'C26 H48 F N O16 V4'
_chemical_formula_weight         853.41

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

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

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

_cell_length_a                   23.418(12)
_cell_length_b                   13.297(8)
_cell_length_c                   23.133(13)
_cell_angle_alpha                90
_cell_angle_beta                 90.199(13)
_cell_angle_gamma                90
_cell_volume                     7203(7)
_cell_formula_units_Z            8
_cell_measurement_temperature    193(2)
_cell_measurement_reflns_used    9944
_cell_measurement_theta_min      2.33
_cell_measurement_theta_max      28.40

_exptl_crystal_description       prism
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.574
_exptl_crystal_F_000             3520
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.450
_exptl_crystal_size_mid          0.400
_exptl_crystal_size_min          0.300
_exptl_absorpt_coefficient_mu    1.079
_shelx_estimated_absorpt_T_min   0.642
_shelx_estimated_absorpt_T_max   0.738
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6423
_exptl_absorpt_correction_T_max  0.7378
_exptl_absorpt_process_details   
; 
program SADABS, Bruker (2001). 
;

_diffrn_ambient_temperature      193(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  
; 
 Bruker-Nonius X8kappa APEX II CCD area detector 
;
_diffrn_measurement_method       'phi and omega scans with narrow frames'
_diffrn_detector_area_resol_mean 8.26
_diffrn_reflns_number            69352
_diffrn_reflns_av_unetI/netI     0.0339
_diffrn_reflns_av_R_equivalents  0.0448
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         1.961
_diffrn_reflns_theta_max         25.250
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             13007
_reflns_number_gt                9438
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'APEX2 Software Suite (Bruker, 2007)'
_computing_cell_refinement       'APEX2 Software Suite (Bruker, 2007)'
_computing_data_reduction        'APEX2 Software Suite (Bruker, 2007)'
_computing_structure_solution    'SIR2002 (Burla et al., 2003)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL and publCIF (Westrip, 2010)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           fullcycle
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0995P)²+4.3118P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         13007
_refine_ls_number_parameters     873
_refine_ls_number_restraints     100
_refine_ls_R_factor_all          0.0819
_refine_ls_R_factor_gt           0.0556
_refine_ls_wR_factor_ref         0.1759
_refine_ls_wR_factor_gt          0.1584
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_restrained_S_all      1.098
_refine_ls_shift/su_max          0.011
_refine_ls_shift/su_mean         0.002

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 0.10446(3) 0.36510(5) 0.28011(3) 0.04507(16) Uani 1 1 d . . . . .
V2 V 0.20073(3) 0.20394(5) 0.30153(3) 0.04201(15) Uani 1 1 d . . . . .
V3 V 0.19164(3) 0.23943(5) 0.43644(3) 0.04440(16) Uani 1 1 d . . . . .
V4 V 0.09074(3) 0.39262(5) 0.41404(3) 0.04715(16) Uani 1 1 d . . . . .
F1 F 0.14639(8) 0.29962(14) 0.35813(7) 0.0354(4) Uani 1 1 d . . . . .
O1 O 0.07331(14) 0.4149(2) 0.22610(12) 0.0683(9) Uani 1 1 d . . . . .
O2 O 0.16204(11) 0.2945(2) 0.24988(10) 0.0466(6) Uani 1 1 d . . . . .
O3 O 0.05904(11) 0.40961(19) 0.34449(11) 0.0467(6) Uani 1 1 d . . . . .
O4 O 0.05953(11) 0.2378(2) 0.28631(11) 0.0469(6) Uani 1 1 d . . . . .
O5 O 0.12870(11) 0.12256(19) 0.29818(11) 0.0476(6) Uani 1 1 d . . . . .
O6 O 0.15766(12) 0.4769(2) 0.30013(13) 0.0562(7) Uani 1 1 d . . . . .
O7 O 0.14891(13) 0.4973(2) 0.39597(13) 0.0597(7) Uani 1 1 d . . . . .
O8 O 0.23809(12) 0.1360(2) 0.25973(12) 0.0605(8) Uani 1 1 d . . . . .
O9 O 0.21691(10) 0.15799(19) 0.37240(10) 0.0445(6) Uani 1 1 d . . . . .
O10 O 0.25602(11) 0.3159(2) 0.31430(11) 0.0505(6) Uani 1 1 d . . . . .
O11 O 0.25053(11) 0.3375(2) 0.41029(11) 0.0509(6) Uani 1 1 d . . . . .
O12 O 0.22532(13) 0.1943(3) 0.49033(11) 0.0652(8) Uani 1 1 d . . . . .
O13 O 0.14819(11) 0.3377(2) 0.46541(10) 0.0483(6) Uani 1 1 d . . . . .
O14 O 0.12394(12) 0.1476(2) 0.43639(11) 0.0505(6) Uani 1 1 d . . . . .
O15 O 0.05248(11) 0.2577(2) 0.42253(11) 0.0502(6) Uani 1 1 d . . . . .
O16 O 0.05089(13) 0.4554(2) 0.45601(13) 0.0681(8) Uani 1 1 d . . . . .
C1 C 0.07751(16) 0.1488(3) 0.29635(15) 0.0443(9) Uani 1 1 d . . . . .
C2 C 0.03268(19) 0.0699(3) 0.30784(19) 0.0617(11) Uani 1 1 d . . . . .
H2A H 0.051680 0.003777 0.312210 0.074 Uiso 1 1 calc R U . . .
H2B H 0.006873 0.065680 0.273941 0.074 Uiso 1 1 calc R U . . .
C3 C -0.00284(19) 0.0904(4) 0.36153(19) 0.0634(12) Uani 1 1 d . . . . .
H3A H -0.034546 0.041224 0.362919 0.076 Uiso 1 1 calc R U . . .
H3B H -0.019883 0.158273 0.358132 0.076 Uiso 1 1 calc R U . . .
C4 C 0.0307(2) 0.0845(4) 0.4185(2) 0.0673(12) Uani 1 1 d . . . . .
H4A H 0.003318 0.084168 0.451001 0.081 Uiso 1 1 calc R U . . .
H4B H 0.051952 0.020169 0.419575 0.081 Uiso 1 1 calc R U . . .
C5 C 0.07217(17) 0.1697(3) 0.42701(16) 0.0487(9) Uani 1 1 d . . . . .
C6 C 0.1726(2) 0.5144(3) 0.3474(2) 0.0588(11) Uani 1 1 d . . . . .
C7 C 0.2225(2) 0.5858(4) 0.3485(3) 0.0842(16) Uani 1 1 d . . . . .
H7A H 0.209895 0.649946 0.366026 0.101 Uiso 1 1 calc R U . . .
H7B H 0.233815 0.600242 0.308122 0.101 Uiso 1 1 calc R U . . .
C8 C 0.2745(2) 0.5485(4) 0.3812(2) 0.0769(14) Uani 1 1 d . . . . .
H8A H 0.302839 0.603638 0.383016 0.092 Uiso 1 1 calc R U . . .
H8B H 0.262958 0.533009 0.421384 0.092 Uiso 1 1 calc R U . . .
C9 C 0.30332(19) 0.4566(4) 0.3562(2) 0.0682(13) Uani 1 1 d . . . . .
H9A H 0.312117 0.469328 0.315028 0.082 Uiso 1 1 calc R U . . .
H9B H 0.339927 0.445390 0.376750 0.082 Uiso 1 1 calc R U . . .
C10 C 0.26744(16) 0.3625(3) 0.36059(18) 0.0508(10) Uani 1 1 d . . . . .
V5 V 0.41290(3) 0.58807(6) 0.09433(3) 0.05151(18) Uani 1 1 d . . . . .
V6 V 0.39884(3) 0.61778(5) 0.22812(3) 0.04610(16) Uani 1 1 d . . . . .
V7 V 0.29733(3) 0.76888(5) 0.20546(3) 0.04630(16) Uani 1 1 d . . . . .
V8 V 0.30808(3) 0.73281(6) 0.07105(3) 0.05106(17) Uani 1 1 d . . . . .
F2 F 0.35482(8) 0.67707(14) 0.14988(7) 0.0371(4) Uani 1 1 d . . . . .
O17 O 0.45450(14) 0.5274(3) 0.05273(14) 0.0766(10) Uani 1 1 d . . . . .
O18 O 0.44529(11) 0.5759(2) 0.16407(12) 0.0515(7) Uani 1 1 d . . . . .
O19 O 0.35423(12) 0.6361(2) 0.04306(10) 0.0551(7) Uani 1 1 d . . . . .
O20 O 0.35850(12) 0.4784(2) 0.11466(13) 0.0595(7) Uani 1 1 d . . . . .
O21 O 0.34995(13) 0.4993(2) 0.21050(12) 0.0573(7) Uani 1 1 d . . . . .
O22 O 0.44799(12) 0.7250(2) 0.08513(12) 0.0575(7) Uani 1 1 d . . . . .
O23 O 0.37341(13) 0.8289(2) 0.07064(12) 0.0595(8) Uani 1 1 d . . . . .
O24 O 0.43165(15) 0.5735(2) 0.28295(13) 0.0695(9) Uani 1 1 d . . . . .
O25 O 0.33858(11) 0.6834(2) 0.25795(10) 0.0468(6) Uani 1 1 d . . . . .
O26 O 0.43919(11) 0.7491(2) 0.22102(11) 0.0479(6) Uani 1 1 d . . . . .
O27 O 0.36655(12) 0.85744(19) 0.20850(11) 0.0501(6) Uani 1 1 d . . . . .
O28 O 0.25721(13) 0.8330(3) 0.24664(13) 0.0707(9) Uani 1 1 d . . . . .
O29 O 0.27967(11) 0.8117(2) 0.13409(11) 0.0493(6) Uani 1 1 d . . . . .
O30 O 0.24617(11) 0.6512(2) 0.19319(11) 0.0535(7) Uani 1 1 d . . . . .
O31 O 0.25268(11) 0.6284(2) 0.09732(12) 0.0559(7) Uani 1 1 d . . . . .
O32 O 0.27402(15) 0.7737(3) 0.01671(13) 0.0779(10) Uani 1 1 d . . . . .
C11 C 0.33584(19) 0.4597(3) 0.1636(2) 0.0570(11) Uani 1 1 d . . . . .
C12 C 0.2882(2) 0.3847(4) 0.1639(2) 0.0774(15) Uani 1 1 d . . . . .
H12A H 0.276366 0.373134 0.204413 0.093 Uiso 1 1 calc R U . . .
H12B H 0.302789 0.320093 0.148642 0.093 Uiso 1 1 calc R U . . .
C13 C 0.2358(2) 0.4148(4) 0.1289(2) 0.0750(14) Uani 1 1 d . . . . .
H13A H 0.247958 0.428995 0.088776 0.090 Uiso 1 1 calc R U . . .
H13B H 0.209359 0.356725 0.127494 0.090 Uiso 1 1 calc R U . . .
C14 C 0.20329(19) 0.5055(4) 0.1515(2) 0.0701(13) Uani 1 1 d . . . . .
H14A H 0.167218 0.512414 0.129377 0.084 Uiso 1 1 calc R U . . .
H14B H 0.193292 0.493767 0.192456 0.084 Uiso 1 1 calc R U . . .
C15 C 0.23639(16) 0.6022(3) 0.14700(18) 0.0533(10) Uani 1 1 d . . . . .
C16 C 0.4253(2) 0.8105(4) 0.08024(16) 0.0560(11) Uani 1 1 d . . . . .
C17 C 0.4647(2) 0.8997(4) 0.0870(2) 0.0715(14) Uani 1 1 d . . . . .
H17A H 0.441961 0.962280 0.084322 0.086 Uiso 1 1 calc R U . . .
H17B H 0.492470 0.899808 0.054864 0.086 Uiso 1 1 calc R U . . .
C18 C 0.4970(2) 0.8991(4) 0.1439(2) 0.0821(16) Uani 1 1 d . . . . .
H18A H 0.527165 0.951157 0.142177 0.099 Uiso 1 1 calc R U . . .
H18B H 0.516173 0.833167 0.148157 0.099 Uiso 1 1 calc R U . . .
C19 C 0.4612(2) 0.9178(3) 0.19769(19) 0.0640(12) Uani 1 1 d . . . . .
H19A H 0.487085 0.925176 0.231363 0.077 Uiso 1 1 calc R U . . .
H19B H 0.440324 0.981965 0.192882 0.077 Uiso 1 1 calc R U . . .
C20 C 0.41877(17) 0.8354(3) 0.21030(15) 0.0445(9) Uani 1 1 d . . . . .
N1 N 0.12308(15) 0.5222(3) 0.61681(14) 0.0556(9) Uani 1 1 d . . . . .
C21 C 0.1327(2) 0.5971(4) 0.5685(2) 0.0753(14) Uani 1 1 d . . . . .
H21A H 0.160785 0.647630 0.581990 0.090 Uiso 1 1 calc R U . . .
H21B H 0.149894 0.561106 0.535414 0.090 Uiso 1 1 calc R U . . .
C22 C 0.0801(2) 0.6518(4) 0.5473(2) 0.0838(16) Uani 1 1 d . . . . .
H22A H 0.059410 0.680369 0.580819 0.101 Uiso 1 1 calc R U . . .
H22B H 0.054296 0.603509 0.527746 0.101 Uiso 1 1 calc R U . . .
C23 C 0.0957(3) 0.7376(5) 0.5048(3) 0.0947(18) Uani 1 1 d . . . . .
H23A H 0.121963 0.710012 0.475336 0.114 Uiso 1 1 calc R U . . .
H23B H 0.060426 0.758849 0.484469 0.114 Uiso 1 1 calc R U . . .
C24 C 0.1225(3) 0.8276(6) 0.5304(3) 0.118(2) Uani 1 1 d . . . . .
H24A H 0.101114 0.848001 0.564816 0.176 Uiso 1 1 calc R U . . .
H24B H 0.122208 0.882428 0.502134 0.176 Uiso 1 1 calc R U . . .
H24C H 0.162000 0.812072 0.541359 0.176 Uiso 1 1 calc R U . . .
C25 C 0.0939(2) 0.5704(4) 0.66756(19) 0.0634(11) Uani 1 1 d . . . . .
H25A H 0.053513 0.582616 0.656800 0.076 Uiso 1 1 calc R U . . .
H25B H 0.093983 0.521621 0.699871 0.076 Uiso 1 1 calc R U . . .
C26 C 0.1184(2) 0.6670(4) 0.6893(2) 0.0661(12) Uani 1 1 d . . . . .
H26A H 0.116900 0.718180 0.658227 0.079 Uiso 1 1 calc R U . . .
H26B H 0.158930 0.656752 0.700128 0.079 Uiso 1 1 calc R U . . .
C27 C 0.0853(2) 0.7044(4) 0.7415(2) 0.0703(13) Uani 1 1 d . . . . .
H27A H 0.044220 0.707868 0.731362 0.084 Uiso 1 1 calc R U . . .
H27B H 0.089599 0.655215 0.773375 0.084 Uiso 1 1 calc R U . . .
C28 C 0.1044(2) 0.8057(4) 0.7625(2) 0.0862(16) Uani 1 1 d . . . . .
H28A H 0.144189 0.801754 0.775528 0.129 Uiso 1 1 calc R U . . .
H28B H 0.080194 0.827114 0.794702 0.129 Uiso 1 1 calc R U . . .
H28C H 0.101297 0.854587 0.730900 0.129 Uiso 1 1 calc R U . . .
C29 C 0.1814(2) 0.4840(4) 0.6354(2) 0.0822(15) Uani 1 1 d D U . . .
H29A H 0.204931 0.542121 0.647597 0.099 Uiso 1 1 calc R U . . .
H29B H 0.176523 0.439815 0.669507 0.099 Uiso 1 1 calc R U . . .
C30 C 0.2129(3) 0.4270(6) 0.5897(3) 0.120(2) Uani 1 1 d D U . . .
H30A H 0.186926 0.375314 0.573597 0.144 Uiso 1 1 calc R U . . .
H30B H 0.222302 0.474176 0.558042 0.144 Uiso 1 1 calc R U . . .
C31 C 0.2659(3) 0.3771(6) 0.6084(3) 0.125(2) Uani 1 1 d D U . . .
H31A H 0.257166 0.334506 0.642321 0.150 Uiso 1 1 calc R U . . .
H31B H 0.278683 0.332028 0.576931 0.150 Uiso 1 1 calc R U . . .
C32 C 0.3115(4) 0.4421(6) 0.6231(4) 0.160(3) Uani 1 1 d D U . . .
H32A H 0.324158 0.478151 0.588490 0.239 Uiso 1 1 calc R U . . .
H32B H 0.343245 0.402544 0.638794 0.239 Uiso 1 1 calc R U . . .
H32C H 0.298604 0.490574 0.652163 0.239 Uiso 1 1 calc R U . . .
C33 C 0.0844(2) 0.4354(4) 0.5947(2) 0.0779(15) Uani 1 1 d . . . . .
H33A H 0.048334 0.464932 0.580148 0.093 Uiso 1 1 calc R U . . .
H33B H 0.103638 0.403011 0.561493 0.093 Uiso 1 1 calc R U . . .
C34 C 0.0700(3) 0.3556(4) 0.6377(3) 0.109(2) Uani 1 1 d . . . . .
H34A H 0.049668 0.387265 0.670502 0.131 Uiso 1 1 calc R U . . .
H34B H 0.105926 0.326690 0.653002 0.131 Uiso 1 1 calc R U . . .
C35 C 0.0327(4) 0.2694(5) 0.6136(3) 0.128(3) Uani 1 1 d . . . . .
H35A H 0.012279 0.237113 0.646154 0.153 Uiso 1 1 calc R U . . .
H35B H 0.003584 0.298219 0.587280 0.153 Uiso 1 1 calc R U . . .
C36 C 0.0628(5) 0.1973(6) 0.5844(4) 0.173(4) Uani 1 1 d . . . . .
H36A H 0.077050 0.225413 0.548103 0.259 Uiso 1 1 calc R U . . .
H36B H 0.037782 0.139943 0.576107 0.259 Uiso 1 1 calc R U . . .
H36C H 0.095069 0.174868 0.608242 0.259 Uiso 1 1 calc R U . . .
N2 N 0.36934(14) 0.0174(3) 0.38528(13) 0.0551(9) Uani 1 1 d . . . . .
C37 C 0.4041(2) 0.0782(4) 0.4297(2) 0.0799(14) Uani 1 1 d D U . . .
H37A H 0.410665 0.034693 0.463849 0.096 Uiso 1 1 calc R U . . .
H37B H 0.441940 0.092512 0.412607 0.096 Uiso 1 1 calc R U . . .
C38 C 0.3800(3) 0.1741(5) 0.4503(3) 0.1056(18) Uani 1 1 d D U . . .
H38A H 0.341533 0.161849 0.466420 0.127 Uiso 1 1 calc R U . . .
H38B H 0.375870 0.220757 0.417183 0.127 Uiso 1 1 calc R U . . .
C39 C 0.4167(3) 0.2214(5) 0.4952(3) 0.123(2) Uani 1 1 d D U . . .
H39A H 0.416002 0.179786 0.530681 0.148 Uiso 1 1 calc R U . . .
H39B H 0.456562 0.224321 0.481260 0.148 Uiso 1 1 calc R U . . .
C40 C 0.3966(4) 0.3241(6) 0.5088(5) 0.197(4) Uani 1 1 d D U . . .
H40A H 0.408765 0.370378 0.478258 0.295 Uiso 1 1 calc R U . . .
H40B H 0.412964 0.345663 0.545845 0.295 Uiso 1 1 calc R U . . .
H40C H 0.354860 0.324336 0.511350 0.295 Uiso 1 1 calc R U . . .
C41 C 0.3552(2) 0.0848(4) 0.3328(2) 0.0770(15) Uani 1 1 d . . . . .
H41A H 0.334898 0.042938 0.303998 0.092 Uiso 1 1 calc R U . . .
H41B H 0.328155 0.137184 0.345910 0.092 Uiso 1 1 calc R U . . .
C42 C 0.4028(2) 0.1358(4) 0.3030(2) 0.0767(14) Uani 1 1 d . . . . .
H42A H 0.430868 0.084637 0.290535 0.092 Uiso 1 1 calc R U . . .
H42B H 0.422179 0.181298 0.330640 0.092 Uiso 1 1 calc R U . . .
C43 C 0.3846(3) 0.1950(7) 0.2518(3) 0.122(3) Uani 1 1 d . . . . .
H43A H 0.360987 0.150396 0.227149 0.146 Uiso 1 1 calc R U . . .
H43B H 0.359347 0.249523 0.265653 0.146 Uiso 1 1 calc R U . . .
C44 C 0.4268(3) 0.2397(6) 0.2157(3) 0.112(2) Uani 1 1 d . . . . .
H44A H 0.438029 0.305049 0.231770 0.168 Uiso 1 1 calc R U . . .
H44B H 0.411180 0.249165 0.176764 0.168 Uiso 1 1 calc R U . . .
H44C H 0.460341 0.195680 0.213868 0.168 Uiso 1 1 calc R U . . .
C45 C 0.4027(2) -0.0713(5) 0.3650(2) 0.0872(18) Uani 1 1 d . . . . .
H45A H 0.382584 -0.101745 0.331637 0.105 Uiso 1 1 calc R U . . .
H45B H 0.440428 -0.047787 0.351332 0.105 Uiso 1 1 calc R U . . .
C46 C 0.4117(3) -0.1499(5) 0.4096(2) 0.0917(19) Uani 1 1 d . . . . .
H46A H 0.374383 -0.168410 0.426498 0.110 Uiso 1 1 calc R U . . .
H46B H 0.435860 -0.122140 0.440969 0.110 Uiso 1 1 calc R U . . .
C47 C 0.4401(4) -0.2444(5) 0.3854(3) 0.134(3) Uani 1 1 d . . . . .
H47A H 0.420657 -0.262892 0.348867 0.161 Uiso 1 1 calc R U . . .
H47B H 0.480285 -0.228132 0.375915 0.161 Uiso 1 1 calc R U . . .
C48 C 0.4397(4) -0.3325(5) 0.4240(3) 0.140(3) Uani 1 1 d . . . . .
H48A H 0.466237 -0.321090 0.456217 0.209 Uiso 1 1 calc R U . . .
H48B H 0.451616 -0.392243 0.402370 0.209 Uiso 1 1 calc R U . . .
H48C H 0.401116 -0.342630 0.439058 0.209 Uiso 1 1 calc R U . . .
C49 C 0.3127(2) -0.0114(4) 0.41389(19) 0.0710(14) Uani 1 1 d . . . . .
H49A H 0.321338 -0.049389 0.449660 0.085 Uiso 1 1 calc R U . . .
H49B H 0.292904 0.051250 0.425453 0.085 Uiso 1 1 calc R U . . .
C50 C 0.2723(2) -0.0727(4) 0.3780(2) 0.0808(15) Uani 1 1 d . . . . .
H50A H 0.262498 -0.034633 0.342535 0.097 Uiso 1 1 calc R U . . .
H50B H 0.291627 -0.135513 0.366076 0.097 Uiso 1 1 calc R U . . .
C51 C 0.2189(3) -0.0986(5) 0.4090(2) 0.100(2) Uani 1 1 d . . . . .
H51A H 0.226236 -0.157562 0.434043 0.120 Uiso 1 1 calc R U . . .
H51B H 0.208270 -0.041613 0.434294 0.120 Uiso 1 1 calc R U . . .
C52 C 0.1704(3) -0.1216(5) 0.3706(3) 0.107(2) Uani 1 1 d . . . . .
H52A H 0.161206 -0.062275 0.347234 0.161 Uiso 1 1 calc R U . . .
H52B H 0.137156 -0.140138 0.393946 0.161 Uiso 1 1 calc R U . . .
H52C H 0.180496 -0.177669 0.345153 0.161 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
V1 O1 1.589(3) . ?
V1 O2 1.788(3) . ?
V1 O3 1.926(3) . ?
V1 O6 1.994(3) . ?
V1 O4 1.999(3) . ?
V1 F1 2.229(2) . ?
V2 O8 1.588(3) . ?
V2 O9 1.789(3) . ?
V2 O2 1.921(3) . ?
V2 O10 1.995(3) . ?
V2 O5 2.005(3) . ?
V2 F1 2.228(2) . ?
V3 O12 1.590(3) . ?
V3 O13 1.788(3) . ?
V3 O9 1.930(3) . ?
V3 O11 1.993(3) . ?
V3 O14 2.001(3) . ?
V3 F1 2.243(2) . ?
V4 O16 1.586(3) . ?
V4 O3 1.784(3) . ?
V4 O13 1.935(3) . ?
V4 O7 1.993(3) . ?
V4 O15 2.015(3) . ?
V4 F1 2.216(2) . ?
O4 C1 1.277(5) . ?
O5 C1 1.249(5) . ?
O6 C6 1.251(5) . ?
O7 C6 1.275(5) . ?
O10 C10 1.265(5) . ?
O11 C10 1.262(5) . ?
O14 C5 1.266(5) . ?
O15 C5 1.262(5) . ?
C1 C2 1.509(5) . ?
C2 C3 1.522(6) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 C4 1.533(7) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 C5 1.506(6) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C6 C7 1.506(6) . ?
C7 C8 1.516(7) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 C9 1.512(7) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 C10 1.511(6) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
V5 O17 1.591(3) . ?
V5 O18 1.788(3) . ?
V5 O19 1.921(3) . ?
V5 O20 1.994(3) . ?
V5 O22 2.009(3) . ?
V5 F2 2.217(2) . ?
V6 O24 1.593(3) . ?
V6 O25 1.799(3) . ?
V6 O18 1.923(3) . ?
V6 O21 1.989(3) . ?
V6 O26 1.992(3) . ?
V6 F2 2.224(2) . ?
V7 O28 1.588(3) . ?
V7 O29 1.793(3) . ?
V7 O25 1.922(3) . ?
V7 O30 1.990(3) . ?
V7 O27 2.005(3) . ?
V7 F2 2.229(2) . ?
V8 O32 1.583(3) . ?
V8 O19 1.801(3) . ?
V8 O29 1.918(3) . ?
V8 O23 1.993(3) . ?
V8 O31 1.996(3) . ?
V8 F2 2.249(2) . ?
O20 C11 1.277(5) . ?
O21 C11 1.249(5) . ?
O22 C16 1.260(6) . ?
O23 C16 1.259(5) . ?
O26 C20 1.268(5) . ?
O27 C20 1.258(5) . ?
O30 C15 1.272(5) . ?
O31 C15 1.261(5) . ?
C11 C12 1.497(6) . ?
C12 C13 1.520(7) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C13 C14 1.520(7) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C14 C15 1.505(6) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C16 C17 1.510(6) . ?
C17 C18 1.516(7) . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C18 C19 1.522(7) . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C19 C20 1.508(6) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
N1 C25 1.504(5) . ?
N1 C21 1.513(6) . ?
N1 C29 1.517(6) . ?
N1 C33 1.553(6) . ?
C21 C22 1.512(7) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C22 C23 1.552(8) . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C23 C24 1.475(9) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 C26 1.493(6) . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C26 C27 1.523(6) . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C27 C28 1.500(7) . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 C30 1.498(6) . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C30 C31 1.470(6) . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C31 C32 1.415(7) . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C33 C34 1.494(8) . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
C34 C35 1.544(8) . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
C35 C36 1.370(11) . ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
N2 C45 1.491(6) . ?
N2 C49 1.534(6) . ?
N2 C37 1.539(6) . ?
N2 C41 1.543(6) . ?
C37 C38 1.474(6) . ?
C37 H37A 0.9900 . ?
C37 H37B 0.9900 . ?
C38 C39 1.485(6) . ?
C38 H38A 0.9900 . ?
C38 H38B 0.9900 . ?
C39 C40 1.479(7) . ?
C39 H39A 0.9900 . ?
C39 H39B 0.9900 . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C40 H40C 0.9800 . ?
C41 C42 1.478(7) . ?
C41 H41A 0.9900 . ?
C41 H41B 0.9900 . ?
C42 C43 1.482(7) . ?
C42 H42A 0.9900 . ?
C42 H42B 0.9900 . ?
C43 C44 1.426(8) . ?
C43 H43A 0.9900 . ?
C43 H43B 0.9900 . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 0.9800 . ?
C45 C46 1.483(7) . ?
C45 H45A 0.9900 . ?
C45 H45B 0.9900 . ?
C46 C47 1.529(8) . ?
C46 H46A 0.9900 . ?
C46 H46B 0.9900 . ?
C47 C48 1.472(9) . ?
C47 H47A 0.9900 . ?
C47 H47B 0.9900 . ?
C48 H48A 0.9800 . ?
C48 H48B 0.9800 . ?
C48 H48C 0.9800 . ?
C49 C50 1.497(7) . ?
C49 H49A 0.9900 . ?
C49 H49B 0.9900 . ?
C50 C51 1.484(7) . ?
C50 H50A 0.9900 . ?
C50 H50B 0.9900 . ?
C51 C52 1.470(8) . ?
C51 H51A 0.9900 . ?
C51 H51B 0.9900 . ?
C52 H52A 0.9800 . ?
C52 H52B 0.9800 . ?
C52 H52C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 V1 O2 104.85(15) . . ?
O1 V1 O3 103.10(15) . . ?
O2 V1 O3 152.02(11) . . ?
O1 V1 O6 99.01(15) . . ?
O2 V1 O6 90.64(13) . . ?
O3 V1 O6 86.42(12) . . ?
O1 V1 O4 99.73(15) . . ?
O2 V1 O4 88.91(12) . . ?
O3 V1 O4 84.99(11) . . ?
O6 V1 O4 160.72(11) . . ?
O1 V1 F1 177.72(14) . . ?
O2 V1 F1 77.33(10) . . ?
O3 V1 F1 74.75(10) . . ?
O6 V1 F1 80.22(10) . . ?
O4 V1 F1 80.89(9) . . ?
O8 V2 O9 104.38(14) . . ?
O8 V2 O2 103.75(14) . . ?
O9 V2 O2 151.87(11) . . ?
O8 V2 O10 98.99(14) . . ?
O9 V2 O10 89.08(12) . . ?
O2 V2 O10 85.92(12) . . ?
O8 V2 O5 97.73(14) . . ?
O9 V2 O5 91.52(12) . . ?
O2 V2 O5 85.36(12) . . ?
O10 V2 O5 162.56(11) . . ?
O8 V2 F1 178.32(12) . . ?
O9 V2 F1 77.06(10) . . ?
O2 V2 F1 74.84(10) . . ?
O10 V2 F1 81.86(10) . . ?
O5 V2 F1 81.30(10) . . ?
O12 V3 O13 105.26(15) . . ?
O12 V3 O9 103.74(15) . . ?
O13 V3 O9 150.96(11) . . ?
O12 V3 O11 98.21(15) . . ?
O13 V3 O11 91.78(13) . . ?
O9 V3 O11 85.40(12) . . ?
O12 V3 O14 99.27(15) . . ?
O13 V3 O14 89.68(13) . . ?
O9 V3 O14 84.38(12) . . ?
O11 V3 O14 161.42(11) . . ?
O12 V3 F1 177.75(13) . . ?
O13 V3 F1 76.94(10) . . ?
O9 V3 F1 74.07(9) . . ?
O11 V3 F1 81.19(10) . . ?
O14 V3 F1 81.10(9) . . ?
O16 V4 O3 103.97(15) . . ?
O16 V4 O13 103.42(15) . . ?
O3 V4 O13 152.61(11) . . ?
O16 V4 O7 99.48(16) . . ?
O3 V4 O7 90.29(13) . . ?
O13 V4 O7 85.30(13) . . ?
O16 V4 O15 98.41(15) . . ?
O3 V4 O15 90.96(12) . . ?
O13 V4 O15 84.98(12) . . ?
O7 V4 O15 161.20(12) . . ?
O16 V4 F1 177.56(14) . . ?
O3 V4 F1 77.76(10) . . ?
O13 V4 F1 74.86(10) . . ?
O7 V4 F1 82.16(11) . . ?
O15 V4 F1 79.78(10) . . ?
V4 F1 V2 178.76(10) . . ?
V4 F1 V1 89.79(8) . . ?
V2 F1 V1 89.90(8) . . ?
V4 F1 V3 90.28(8) . . ?
V2 F1 V3 90.09(8) . . ?
V1 F1 V3 177.33(10) . . ?
V1 O2 V2 116.16(13) . . ?
V4 O3 V1 115.41(14) . . ?
C1 O4 V1 128.6(2) . . ?
C1 O5 V2 131.1(3) . . ?
C6 O6 V1 132.3(3) . . ?
C6 O7 V4 127.5(3) . . ?
V2 O9 V3 116.58(13) . . ?
C10 O10 V2 128.8(2) . . ?
C10 O11 V3 132.0(3) . . ?
V3 O13 V4 116.17(13) . . ?
C5 O14 V3 128.1(3) . . ?
C5 O15 V4 132.1(3) . . ?
O5 C1 O4 125.5(3) . . ?
O5 C1 C2 117.9(4) . . ?
O4 C1 C2 116.6(4) . . ?
C1 C2 C3 113.7(3) . . ?
C1 C2 H2A 108.8 . . ?
C3 C2 H2A 108.8 . . ?
C1 C2 H2B 108.8 . . ?
C3 C2 H2B 108.8 . . ?
H2A C2 H2B 107.7 . . ?
C2 C3 C4 114.4(4) . . ?
C2 C3 H3A 108.7 . . ?
C4 C3 H3A 108.7 . . ?
C2 C3 H3B 108.7 . . ?
C4 C3 H3B 108.7 . . ?
H3A C3 H3B 107.6 . . ?
C5 C4 C3 113.7(4) . . ?
C5 C4 H4A 108.8 . . ?
C3 C4 H4A 108.8 . . ?
C5 C4 H4B 108.8 . . ?
C3 C4 H4B 108.8 . . ?
H4A C4 H4B 107.7 . . ?
O15 C5 O14 125.4(4) . . ?
O15 C5 C4 116.9(4) . . ?
O14 C5 C4 117.7(4) . . ?
O6 C6 O7 125.3(4) . . ?
O6 C6 C7 118.7(4) . . ?
O7 C6 C7 116.0(4) . . ?
C6 C7 C8 115.1(4) . . ?
C6 C7 H7A 108.5 . . ?
C8 C7 H7A 108.5 . . ?
C6 C7 H7B 108.5 . . ?
C8 C7 H7B 108.5 . . ?
H7A C7 H7B 107.5 . . ?
C9 C8 C7 115.6(5) . . ?
C9 C8 H8A 108.4 . . ?
C7 C8 H8A 108.4 . . ?
C9 C8 H8B 108.4 . . ?
C7 C8 H8B 108.4 . . ?
H8A C8 H8B 107.4 . . ?
C10 C9 C8 113.2(4) . . ?
C10 C9 H9A 108.9 . . ?
C8 C9 H9A 108.9 . . ?
C10 C9 H9B 108.9 . . ?
C8 C9 H9B 108.9 . . ?
H9A C9 H9B 107.7 . . ?
O11 C10 O10 125.2(4) . . ?
O11 C10 C9 117.1(4) . . ?
O10 C10 C9 117.7(4) . . ?
O17 V5 O18 103.97(17) . . ?
O17 V5 O19 103.49(16) . . ?
O18 V5 O19 152.54(12) . . ?
O17 V5 O20 99.49(16) . . ?
O18 V5 O20 89.46(13) . . ?
O19 V5 O20 86.14(13) . . ?
O17 V5 O22 98.28(16) . . ?
O18 V5 O22 90.28(12) . . ?
O19 V5 O22 85.70(13) . . ?
O20 V5 O22 161.75(12) . . ?
O17 V5 F2 177.89(16) . . ?
O18 V5 F2 77.54(10) . . ?
O19 V5 F2 75.01(10) . . ?
O20 V5 F2 81.95(11) . . ?
O22 V5 F2 80.18(10) . . ?
O24 V6 O25 104.51(16) . . ?
O24 V6 O18 103.53(16) . . ?
O25 V6 O18 151.93(12) . . ?
O24 V6 O21 98.42(15) . . ?
O25 V6 O21 90.63(13) . . ?
O18 V6 O21 86.54(12) . . ?
O24 V6 O26 99.31(15) . . ?
O25 V6 O26 88.83(12) . . ?
O18 V6 O26 85.42(12) . . ?
O21 V6 O26 161.82(12) . . ?
O24 V6 F2 178.29(14) . . ?
O25 V6 F2 77.19(10) . . ?
O18 V6 F2 74.78(10) . . ?
O21 V6 F2 81.32(10) . . ?
O26 V6 F2 80.84(9) . . ?
O28 V7 O29 104.28(16) . . ?
O28 V7 O25 103.63(15) . . ?
O29 V7 O25 152.07(12) . . ?
O28 V7 O30 98.64(15) . . ?
O29 V7 O30 88.95(12) . . ?
O25 V7 O30 85.76(12) . . ?
O28 V7 O27 98.27(15) . . ?
O29 V7 O27 91.69(12) . . ?
O25 V7 O27 85.45(12) . . ?
O30 V7 O27 162.37(11) . . ?
O28 V7 F2 178.37(14) . . ?
O29 V7 F2 77.34(10) . . ?
O25 V7 F2 74.75(10) . . ?
O30 V7 F2 81.47(10) . . ?
O27 V7 F2 81.48(10) . . ?
O32 V8 O19 105.15(17) . . ?
O32 V8 O29 103.92(17) . . ?
O19 V8 O29 150.93(12) . . ?
O32 V8 O23 99.25(16) . . ?
O19 V8 O23 89.67(14) . . ?
O29 V8 O23 85.48(13) . . ?
O32 V8 O31 98.89(15) . . ?
O19 V8 O31 90.25(13) . . ?
O29 V8 O31 85.50(12) . . ?
O23 V8 O31 161.22(12) . . ?
O32 V8 F2 178.40(16) . . ?
O19 V8 F2 76.42(10) . . ?
O29 V8 F2 74.50(10) . . ?
O23 V8 F2 81.00(10) . . ?
O31 V8 F2 80.73(10) . . ?
V5 F2 V6 89.94(8) . . ?
V5 F2 V7 179.02(10) . . ?
V6 F2 V7 90.23(8) . . ?
V5 F2 V8 90.21(8) . . ?
V6 F2 V8 178.04(10) . . ?
V7 F2 V8 89.65(8) . . ?
V5 O18 V6 115.46(14) . . ?
V8 O19 V5 116.38(13) . . ?
C11 O20 V5 128.3(3) . . ?
C11 O21 V6 131.5(3) . . ?
C16 O22 V5 130.9(3) . . ?
C16 O23 V8 128.0(3) . . ?
V6 O25 V7 115.97(13) . . ?
C20 O26 V6 129.1(2) . . ?
C20 O27 V7 130.6(3) . . ?
V7 O29 V8 116.54(14) . . ?
C15 O30 V7 129.0(2) . . ?
C15 O31 V8 131.9(3) . . ?
O21 C11 O20 125.3(4) . . ?
O21 C11 C12 118.2(4) . . ?
O20 C11 C12 116.5(4) . . ?
C11 C12 C13 115.0(4) . . ?
C11 C12 H12A 108.5 . . ?
C13 C12 H12A 108.5 . . ?
C11 C12 H12B 108.5 . . ?
C13 C12 H12B 108.5 . . ?
H12A C12 H12B 107.5 . . ?
C14 C13 C12 115.5(4) . . ?
C14 C13 H13A 108.4 . . ?
C12 C13 H13A 108.4 . . ?
C14 C13 H13B 108.4 . . ?
C12 C13 H13B 108.4 . . ?
H13A C13 H13B 107.5 . . ?
C15 C14 C13 113.3(4) . . ?
C15 C14 H14A 108.9 . . ?
C13 C14 H14A 108.9 . . ?
C15 C14 H14B 108.9 . . ?
C13 C14 H14B 108.9 . . ?
H14A C14 H14B 107.7 . . ?
O31 C15 O30 124.8(4) . . ?
O31 C15 C14 117.1(4) . . ?
O30 C15 C14 118.1(4) . . ?
O23 C16 O22 126.7(4) . . ?
O23 C16 C17 117.1(5) . . ?
O22 C16 C17 116.3(4) . . ?
C16 C17 C18 112.9(4) . . ?
C16 C17 H17A 109.0 . . ?
C18 C17 H17A 109.0 . . ?
C16 C17 H17B 109.0 . . ?
C18 C17 H17B 109.0 . . ?
H17A C17 H17B 107.8 . . ?
C17 C18 C19 115.7(5) . . ?
C17 C18 H18A 108.3 . . ?
C19 C18 H18A 108.3 . . ?
C17 C18 H18B 108.3 . . ?
C19 C18 H18B 108.3 . . ?
H18A C18 H18B 107.4 . . ?
C20 C19 C18 113.9(4) . . ?
C20 C19 H19A 108.8 . . ?
C18 C19 H19A 108.8 . . ?
C20 C19 H19B 108.8 . . ?
C18 C19 H19B 108.8 . . ?
H19A C19 H19B 107.7 . . ?
O27 C20 O26 125.7(4) . . ?
O27 C20 C19 117.8(4) . . ?
O26 C20 C19 116.5(4) . . ?
C25 N1 C21 111.4(4) . . ?
C25 N1 C29 109.4(3) . . ?
C21 N1 C29 107.1(4) . . ?
C25 N1 C33 107.9(4) . . ?
C21 N1 C33 109.5(3) . . ?
C29 N1 C33 111.6(4) . . ?
C22 C21 N1 115.6(4) . . ?
C22 C21 H21A 108.4 . . ?
N1 C21 H21A 108.4 . . ?
C22 C21 H21B 108.4 . . ?
N1 C21 H21B 108.4 . . ?
H21A C21 H21B 107.4 . . ?
C21 C22 C23 111.5(5) . . ?
C21 C22 H22A 109.3 . . ?
C23 C22 H22A 109.3 . . ?
C21 C22 H22B 109.3 . . ?
C23 C22 H22B 109.3 . . ?
H22A C22 H22B 108.0 . . ?
C24 C23 C22 116.3(5) . . ?
C24 C23 H23A 108.2 . . ?
C22 C23 H23A 108.2 . . ?
C24 C23 H23B 108.2 . . ?
C22 C23 H23B 108.2 . . ?
H23A C23 H23B 107.4 . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C26 C25 N1 117.0(4) . . ?
C26 C25 H25A 108.0 . . ?
N1 C25 H25A 108.0 . . ?
C26 C25 H25B 108.0 . . ?
N1 C25 H25B 108.0 . . ?
H25A C25 H25B 107.3 . . ?
C25 C26 C27 110.6(4) . . ?
C25 C26 H26A 109.5 . . ?
C27 C26 H26A 109.5 . . ?
C25 C26 H26B 109.5 . . ?
C27 C26 H26B 109.5 . . ?
H26A C26 H26B 108.1 . . ?
C28 C27 C26 113.4(5) . . ?
C28 C27 H27A 108.9 . . ?
C26 C27 H27A 108.9 . . ?
C28 C27 H27B 108.9 . . ?
C26 C27 H27B 108.9 . . ?
H27A C27 H27B 107.7 . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C30 C29 N1 114.5(4) . . ?
C30 C29 H29A 108.6 . . ?
N1 C29 H29A 108.6 . . ?
C30 C29 H29B 108.6 . . ?
N1 C29 H29B 108.6 . . ?
H29A C29 H29B 107.6 . . ?
C31 C30 C29 116.0(6) . . ?
C31 C30 H30A 108.3 . . ?
C29 C30 H30A 108.3 . . ?
C31 C30 H30B 108.3 . . ?
C29 C30 H30B 108.3 . . ?
H30A C30 H30B 107.4 . . ?
C32 C31 C30 115.5(7) . . ?
C32 C31 H31A 108.4 . . ?
C30 C31 H31A 108.4 . . ?
C32 C31 H31B 108.4 . . ?
C30 C31 H31B 108.4 . . ?
H31A C31 H31B 107.5 . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C34 C33 N1 116.2(4) . . ?
C34 C33 H33A 108.2 . . ?
N1 C33 H33A 108.2 . . ?
C34 C33 H33B 108.2 . . ?
N1 C33 H33B 108.2 . . ?
H33A C33 H33B 107.4 . . ?
C33 C34 C35 114.6(5) . . ?
C33 C34 H34A 108.6 . . ?
C35 C34 H34A 108.6 . . ?
C33 C34 H34B 108.6 . . ?
C35 C34 H34B 108.6 . . ?
H34A C34 H34B 107.6 . . ?
C36 C35 C34 114.0(8) . . ?
C36 C35 H35A 108.8 . . ?
C34 C35 H35A 108.8 . . ?
C36 C35 H35B 108.8 . . ?
C34 C35 H35B 108.8 . . ?
H35A C35 H35B 107.7 . . ?
C35 C36 H36A 109.5 . . ?
C35 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C35 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C45 N2 C49 113.2(4) . . ?
C45 N2 C37 110.4(4) . . ?
C49 N2 C37 107.4(3) . . ?
C45 N2 C41 108.9(3) . . ?
C49 N2 C41 107.5(3) . . ?
C37 N2 C41 109.4(4) . . ?
C38 C37 N2 117.9(4) . . ?
C38 C37 H37A 107.8 . . ?
N2 C37 H37A 107.8 . . ?
C38 C37 H37B 107.8 . . ?
N2 C37 H37B 107.8 . . ?
H37A C37 H37B 107.2 . . ?
C37 C38 C39 111.8(5) . . ?
C37 C38 H38A 109.3 . . ?
C39 C38 H38A 109.3 . . ?
C37 C38 H38B 109.3 . . ?
C39 C38 H38B 109.3 . . ?
H38A C38 H38B 107.9 . . ?
C40 C39 C38 110.9(7) . . ?
C40 C39 H39A 109.5 . . ?
C38 C39 H39A 109.5 . . ?
C40 C39 H39B 109.5 . . ?
C38 C39 H39B 109.5 . . ?
H39A C39 H39B 108.0 . . ?
C39 C40 H40A 109.5 . . ?
C39 C40 H40B 109.5 . . ?
H40A C40 H40B 109.5 . . ?
C39 C40 H40C 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
C42 C41 N2 118.4(4) . . ?
C42 C41 H41A 107.7 . . ?
N2 C41 H41A 107.7 . . ?
C42 C41 H41B 107.7 . . ?
N2 C41 H41B 107.7 . . ?
H41A C41 H41B 107.1 . . ?
C41 C42 C43 113.7(5) . . ?
C41 C42 H42A 108.8 . . ?
C43 C42 H42A 108.8 . . ?
C41 C42 H42B 108.8 . . ?
C43 C42 H42B 108.8 . . ?
H42A C42 H42B 107.7 . . ?
C44 C43 C42 119.4(5) . . ?
C44 C43 H43A 107.5 . . ?
C42 C43 H43A 107.5 . . ?
C44 C43 H43B 107.5 . . ?
C42 C43 H43B 107.5 . . ?
H43A C43 H43B 107.0 . . ?
C43 C44 H44A 109.5 . . ?
C43 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
C43 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
C46 C45 N2 114.4(4) . . ?
C46 C45 H45A 108.7 . . ?
N2 C45 H45A 108.7 . . ?
C46 C45 H45B 108.7 . . ?
N2 C45 H45B 108.7 . . ?
H45A C45 H45B 107.6 . . ?
C45 C46 C47 112.7(5) . . ?
C45 C46 H46A 109.1 . . ?
C47 C46 H46A 109.1 . . ?
C45 C46 H46B 109.1 . . ?
C47 C46 H46B 109.1 . . ?
H46A C46 H46B 107.8 . . ?
C48 C47 C46 115.3(5) . . ?
C48 C47 H47A 108.4 . . ?
C46 C47 H47A 108.4 . . ?
C48 C47 H47B 108.4 . . ?
C46 C47 H47B 108.4 . . ?
H47A C47 H47B 107.5 . . ?
C47 C48 H48A 109.5 . . ?
C47 C48 H48B 109.5 . . ?
H48A C48 H48B 109.5 . . ?
C47 C48 H48C 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?
C50 C49 N2 116.2(4) . . ?
C50 C49 H49A 108.2 . . ?
N2 C49 H49A 108.2 . . ?
C50 C49 H49B 108.2 . . ?
N2 C49 H49B 108.2 . . ?
H49A C49 H49B 107.4 . . ?
C51 C50 C49 113.0(4) . . ?
C51 C50 H50A 109.0 . . ?
C49 C50 H50A 109.0 . . ?
C51 C50 H50B 109.0 . . ?
C49 C50 H50B 109.0 . . ?
H50A C50 H50B 107.8 . . ?
C52 C51 C50 114.0(5) . . ?
C52 C51 H51A 108.7 . . ?
C50 C51 H51A 108.7 . . ?
C52 C51 H51B 108.7 . . ?
C50 C51 H51B 108.7 . . ?
H51A C51 H51B 107.6 . . ?
C51 C52 H52A 109.5 . . ?
C51 C52 H52B 109.5 . . ?
H52A C52 H52B 109.5 . . ?
C51 C52 H52C 109.5 . . ?
H52A C52 H52C 109.5 . . ?
H52B C52 H52C 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
O1 V1 O2 V2 -168.91(17) . . . . ?
O3 V1 O2 V2 8.0(3) . . . . ?
O6 V1 O2 V2 91.59(16) . . . . ?
O4 V1 O2 V2 -69.13(15) . . . . ?
F1 V1 O2 V2 11.77(13) . . . . ?
O16 V4 O3 V1 168.46(17) . . . . ?
O13 V4 O3 V1 -11.7(4) . . . . ?
O7 V4 O3 V1 68.61(16) . . . . ?
O15 V4 O3 V1 -92.63(15) . . . . ?
F1 V4 O3 V1 -13.30(12) . . . . ?
O8 V2 O9 V3 167.74(16) . . . . ?
O2 V2 O9 V3 -10.9(3) . . . . ?
O10 V2 O9 V3 68.69(16) . . . . ?
O5 V2 O9 V3 -93.88(16) . . . . ?
F1 V2 O9 V3 -13.17(12) . . . . ?
O12 V3 O13 V4 -168.86(16) . . . . ?
O9 V3 O13 V4 8.4(3) . . . . ?
O11 V3 O13 V4 92.13(15) . . . . ?
O14 V3 O13 V4 -69.34(15) . . . . ?
F1 V3 O13 V4 11.59(13) . . . . ?
V2 O5 C1 O4 12.8(6) . . . . ?
V2 O5 C1 C2 -166.2(3) . . . . ?
V1 O4 C1 O5 -8.3(5) . . . . ?
V1 O4 C1 C2 170.7(3) . . . . ?
O5 C1 C2 C3 116.6(4) . . . . ?
O4 C1 C2 C3 -62.5(5) . . . . ?
C1 C2 C3 C4 -66.5(5) . . . . ?
C2 C3 C4 C5 70.5(5) . . . . ?
V4 O15 C5 O14 12.0(6) . . . . ?
V4 O15 C5 C4 -165.8(3) . . . . ?
V3 O14 C5 O15 -9.0(5) . . . . ?
V3 O14 C5 C4 168.8(3) . . . . ?
C3 C4 C5 O15 53.5(5) . . . . ?
C3 C4 C5 O14 -124.5(4) . . . . ?
V1 O6 C6 O7 -11.6(7) . . . . ?
V1 O6 C6 C7 168.3(3) . . . . ?
V4 O7 C6 O6 10.4(6) . . . . ?
V4 O7 C6 C7 -169.5(3) . . . . ?
O6 C6 C7 C8 -114.1(5) . . . . ?
O7 C6 C7 C8 65.8(6) . . . . ?
C6 C7 C8 C9 64.5(7) . . . . ?
C7 C8 C9 C10 -67.9(6) . . . . ?
V3 O11 C10 O10 -12.7(6) . . . . ?
V3 O11 C10 C9 166.2(3) . . . . ?
V2 O10 C10 O11 9.6(6) . . . . ?
V2 O10 C10 C9 -169.3(3) . . . . ?
C8 C9 C10 O11 -56.0(5) . . . . ?
C8 C9 C10 O10 123.0(4) . . . . ?
O17 V5 O18 V6 -168.23(17) . . . . ?
O19 V5 O18 V6 12.0(4) . . . . ?
O20 V5 O18 V6 -68.58(16) . . . . ?
O22 V5 O18 V6 93.17(16) . . . . ?
F2 V5 O18 V6 13.29(13) . . . . ?
O32 V8 O19 V5 167.97(17) . . . . ?
O29 V8 O19 V5 -11.6(3) . . . . ?
O23 V8 O19 V5 68.47(16) . . . . ?
O31 V8 O19 V5 -92.75(16) . . . . ?
F2 V8 O19 V5 -12.35(13) . . . . ?
O24 V6 O25 V7 168.17(17) . . . . ?
O18 V6 O25 V7 -9.1(3) . . . . ?
O21 V6 O25 V7 -92.97(16) . . . . ?
O26 V6 O25 V7 68.86(15) . . . . ?
F2 V6 O25 V7 -12.01(13) . . . . ?
O28 V7 O29 V8 -167.68(17) . . . . ?
O25 V7 O29 V8 9.9(3) . . . . ?
O30 V7 O29 V8 -69.03(16) . . . . ?
O27 V7 O29 V8 93.35(16) . . . . ?
F2 V7 O29 V8 12.47(13) . . . . ?
V6 O21 C11 O20 12.6(7) . . . . ?
V6 O21 C11 C12 -166.8(3) . . . . ?
V5 O20 C11 O21 -10.6(7) . . . . ?
V5 O20 C11 C12 168.8(3) . . . . ?
O21 C11 C12 C13 116.9(5) . . . . ?
O20 C11 C12 C13 -62.5(6) . . . . ?
C11 C12 C13 C14 -65.9(6) . . . . ?
C12 C13 C14 C15 67.0(6) . . . . ?
V8 O31 C15 O30 12.4(7) . . . . ?
V8 O31 C15 C14 -167.2(3) . . . . ?
V7 O30 C15 O31 -9.7(6) . . . . ?
V7 O30 C15 C14 170.0(3) . . . . ?
C13 C14 C15 O31 58.5(6) . . . . ?
C13 C14 C15 O30 -121.2(5) . . . . ?
V8 O23 C16 O22 9.5(6) . . . . ?
V8 O23 C16 C17 -170.0(3) . . . . ?
V5 O22 C16 O23 -12.4(6) . . . . ?
V5 O22 C16 C17 167.2(3) . . . . ?
O23 C16 C17 C18 123.7(5) . . . . ?
O22 C16 C17 C18 -55.9(6) . . . . ?
C16 C17 C18 C19 -69.3(6) . . . . ?
C17 C18 C19 C20 66.3(6) . . . . ?
V7 O27 C20 O26 -13.5(6) . . . . ?
V7 O27 C20 C19 165.3(3) . . . . ?
V6 O26 C20 O27 8.9(6) . . . . ?
V6 O26 C20 C19 -170.0(3) . . . . ?
C18 C19 C20 O27 -116.4(5) . . . . ?
C18 C19 C20 O26 62.6(5) . . . . ?
C25 N1 C21 C22 -54.9(5) . . . . ?
C29 N1 C21 C22 -174.5(4) . . . . ?
C33 N1 C21 C22 64.4(5) . . . . ?
N1 C21 C22 C23 171.4(4) . . . . ?
C21 C22 C23 C24 -72.8(7) . . . . ?
C21 N1 C25 C26 -49.3(5) . . . . ?
C29 N1 C25 C26 68.9(5) . . . . ?
C33 N1 C25 C26 -169.6(4) . . . . ?
N1 C25 C26 C27 -178.4(4) . . . . ?
C25 C26 C27 C28 -175.0(4) . . . . ?
C25 N1 C29 C30 175.4(5) . . . . ?
C21 N1 C29 C30 -63.8(6) . . . . ?
C33 N1 C29 C30 56.1(7) . . . . ?
N1 C29 C30 C31 -172.0(6) . . . . ?
C29 C30 C31 C32 -68.7(10) . . . . ?
C25 N1 C33 C34 -57.5(6) . . . . ?
C21 N1 C33 C34 -179.0(5) . . . . ?
C29 N1 C33 C34 62.7(6) . . . . ?
N1 C33 C34 C35 -178.6(5) . . . . ?
C33 C34 C35 C36 81.8(9) . . . . ?
C45 N2 C37 C38 174.2(5) . . . . ?
C49 N2 C37 C38 -62.0(6) . . . . ?
C41 N2 C37 C38 54.4(6) . . . . ?
N2 C37 C38 C39 176.9(5) . . . . ?
C37 C38 C39 C40 171.4(7) . . . . ?
C45 N2 C41 C42 -66.3(6) . . . . ?
C49 N2 C41 C42 170.7(5) . . . . ?
C37 N2 C41 C42 54.3(6) . . . . ?
N2 C41 C42 C43 177.5(5) . . . . ?
C41 C42 C43 C44 -173.8(7) . . . . ?
C49 N2 C45 C46 -51.9(6) . . . . ?
C37 N2 C45 C46 68.6(6) . . . . ?
C41 N2 C45 C46 -171.4(5) . . . . ?
N2 C45 C46 C47 173.6(6) . . . . ?
C45 C46 C47 C48 -168.1(7) . . . . ?
C45 N2 C49 C50 -57.1(5) . . . . ?
C37 N2 C49 C50 -179.2(4) . . . . ?
C41 N2 C49 C50 63.2(5) . . . . ?
N2 C49 C50 C51 179.2(5) . . . . ?
C49 C50 C51 C52 156.9(6) . . . . ?

_refine_diff_density_max         0.817
_refine_diff_density_min         -0.589
_refine_diff_density_rms         0.085




#==============================================================================0
# start Validation Reply Form

_vrf_PLAT230_3                   
;
PROBLEM:
Alert level C
PLAT230_ALERT_2_C Hirshfeld Test Diff for    C35    --  C36     ..        6.4 s.u. 
RESPONSE:

Even at 193(2) K there are some carbon atoms severely affected by thermal 
disorder. This C alert is likely to be due to some structural disorder 
associated with some carbon  and nitrogen atoms of tetrabutyl groups of the 
tetrabutylammonium cations. Attempts to model these molecules over two or 
more distinct crystallographic positions did not lead to reasonable structural 
models. 

;

_vrf_PLAT234_3                   
;
PROBLEM:
Alert level C
PLAT234_ALERT_4_C Large Hirshfeld Difference C39    --  C40     ..       0.19 Ang.
RESPONSE: 
Analogous to previous alert and we offer the same explanation. 
;

_vrf_PLAT241_3                   
;
PROBLEM:
Alert level C
PLAT241_ALERT_2_C High   'MainMol' Ueq as Compared to Neighbors of       C7 Check 

RESPONSE:
Analogous to previous alert and we offer the same explanation. 
;

_vrf_PLAT242_3                   
;
PROBLEM:
Alert level C
PLAT242_ALERT_2_C Low    'MainMol' Ueq as Compared to Neighbors of        N1 Check 

RESPONSE:
Analogous to previous alert and we offer the same explanation. 
;

_vrf_PLAT341_3                   
;
PROBLEM:
Alert level C
PLAT341_ALERT_3_C Low Bond Precision on  C-C Bonds ...............   0.008 Ang.
RESPONSE: 
The crystal was not of very good quality despite being the best selected from
the sample supplied. The crystal structure heve two tetrabutylammonium cations 
severely affected by thermal disorder and in general shows distinct thermal 
displacements of some outer atoms. So that some shelxl restraints 
(DELU, SIMU, ..) were used to make the structure more plausible.

;

_vrf_PLAT360_3                   
;
PROBLEM:
Alert level C
PLAT360_ALERT_2_C Short  C(sp3)-C(sp3) Bond   C31    -   C32    ..       1.41 Ang.
 
 
RESPONSE:
We offer the same explanation as for the previous alerts PLAT230 
and PLAT341 

;

# end Validation Reply Form
#==============================================================================0

###END




####################################################################### 
# 
# 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_2
_database_code_depnum_ccdc_archive 'CCDC 1573269'
_audit_update_record             
;
2017-09-07 deposited with the CCDC.
2018-01-09 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C20 H24 O32 V8, 2(C16 H36 N), 2(Cl)'
_chemical_formula_sum            'C52 H96 Cl2 N2 O32 V8'
_chemical_formula_weight         1739.72

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   14.8986(4)
_cell_length_b                   16.7125(5)
_cell_length_c                   17.4333(5)
_cell_angle_alpha                64.2850(10)
_cell_angle_beta                 85.7850(10)
_cell_angle_gamma                86.1320(10)
_cell_volume                     3897.24(19)
_cell_formula_units_Z            2
_cell_measurement_temperature    193(2)
_cell_measurement_reflns_used    9891
_cell_measurement_theta_min      2.62
_cell_measurement_theta_max      30.52

_exptl_crystal_description       prism
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.483
_exptl_crystal_F_000             1792
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_exptl_absorpt_coefficient_mu    1.062
_shelx_estimated_absorpt_T_min   0.741
_shelx_estimated_absorpt_T_max   0.816
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7412
_exptl_absorpt_correction_T_max  0.8157
_exptl_absorpt_process_details   
;
program SADABS, Bruker (2001).
;
_diffrn_ambient_temperature      193(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  
;
 Bruker-Nonius X8kappa APEX II CCD area detector
;
_diffrn_measurement_method       'phi and omega scans with narrow frames'
_diffrn_detector_area_resol_mean 8.26
_diffrn_reflns_number            49714
_diffrn_reflns_av_unetI/netI     0.0259
_diffrn_reflns_av_R_equivalents  0.0251
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         1.298
_diffrn_reflns_theta_max         25.250
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             14080
_reflns_number_gt                11537
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'APEX2 Software Suite (Bruker, 2007)'
_computing_cell_refinement       'APEX2 Software Suite (Bruker, 2007)'
_computing_data_reduction        'APEX2 Software Suite (Bruker, 2007)'
_computing_structure_solution    'SIR2002 (Burla et al., 2003)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL and publCIF (Westrip, 2010)'
_refine_special_details          SQUEEZE
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0891P)²+8.5295P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         14080
_refine_ls_number_parameters     1021
_refine_ls_number_restraints     740
_refine_ls_R_factor_all          0.0703
_refine_ls_R_factor_gt           0.0586
_refine_ls_wR_factor_ref         0.1739
_refine_ls_wR_factor_gt          0.1652
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_restrained_S_all      1.028
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
V1 V 0.07130(4) 0.23708(4) 0.09961(4) 0.02751(16) Uani 1 1 d . . . . .
V2 V -0.12976(4) 0.24354(4) 0.03568(4) 0.02982(17) Uani 1 1 d . . . . .
V3 V -0.15282(4) 0.69096(4) 0.09732(4) 0.02734(16) Uani 1 1 d . . . . .
V4 V 0.05036(4) 0.67542(4) 0.16121(4) 0.02720(16) Uani 1 1 d . . . . .
Cl1 Cl 0.00538(6) 0.61723(6) 0.04144(6) 0.0263(2) Uani 1 1 d . . . . .
O1 O 0.1161(2) 0.15996(18) 0.18010(17) 0.0361(6) Uani 1 1 d . . . . .
O2 O -0.02770(18) 0.18744(16) 0.09122(16) 0.0312(6) Uani 1 1 d . . . . .
O3 O -0.2002(2) 0.16707(19) 0.08020(18) 0.0408(7) Uani 1 1 d . . . . .
O4 O 0.13634(18) 0.22702(16) 0.01019(17) 0.0306(6) Uani 1 1 d . . . . .
O5 O 0.15375(17) 0.33428(17) 0.08270(17) 0.0316(6) Uani 1 1 d . . . . .
O6 O 0.20836(17) 0.38525(17) -0.05277(17) 0.0320(6) Uani 1 1 d . . . . .
O7 O -0.00392(18) 0.29829(17) 0.15914(16) 0.0297(6) Uani 1 1 d . . . . .
O8 O -0.14374(18) 0.30114(18) 0.11698(17) 0.0322(6) Uani 1 1 d . . . . .
O9 O -0.24050(19) 0.72883(19) 0.12982(19) 0.0379(7) Uani 1 1 d . . . . .
O10 O -0.06221(17) 0.72245(16) 0.14421(16) 0.0295(6) Uani 1 1 d . . . . .
O11 O 0.08149(19) 0.70209(18) 0.23242(17) 0.0335(6) Uani 1 1 d . . . . .
O12 O 0.10198(17) 0.76184(17) 0.06333(16) 0.0297(6) Uani 1 1 d . . . . .
O13 O -0.14291(18) 0.57193(17) 0.19868(17) 0.0322(6) Uani 1 1 d . . . . .
O14 O -0.00017(18) 0.55849(17) 0.23826(16) 0.0313(6) Uani 1 1 d . . . . .
O15 O 0.15986(17) 0.59714(18) 0.16064(16) 0.0300(6) Uani 1 1 d . . . . .
O16 O 0.21633(17) 0.65523(18) 0.02513(16) 0.0313(6) Uani 1 1 d . . . . .
C1 C 0.1988(2) 0.3875(2) 0.0192(2) 0.0278(8) Uani 1 1 d . . . . .
C2 C 0.2435(3) 0.4607(3) 0.0280(3) 0.0362(9) Uani 1 1 d . . . . .
H2A H 0.207823 0.516811 -0.001156 0.043 Uiso 1 1 calc R U . . .
H2B H 0.303867 0.468266 -0.001554 0.043 Uiso 1 1 calc R U . . .
C3 C 0.2542(3) 0.4451(3) 0.1196(2) 0.0331(9) Uani 1 1 d . . . . .
H3A H 0.296161 0.393329 0.146927 0.040 Uiso 1 1 calc R U . . .
H3B H 0.195108 0.430645 0.151261 0.040 Uiso 1 1 calc R U . . .
C4 C 0.2898(3) 0.5255(3) 0.1263(3) 0.0329(9) Uani 1 1 d . . . . .
H4A H 0.307557 0.508312 0.185181 0.040 Uiso 1 1 calc R U . . .
H4B H 0.343588 0.546924 0.087275 0.040 Uiso 1 1 calc R U . . .
C5 C 0.2169(3) 0.5990(3) 0.1029(3) 0.0297(8) Uani 1 1 d . . . . .
C6 C -0.0870(3) 0.3206(2) 0.1564(2) 0.0285(8) Uani 1 1 d . . . . .
C7 C -0.1209(3) 0.3775(3) 0.2005(3) 0.0338(9) Uani 1 1 d . . . . .
H7A H -0.182406 0.359880 0.225360 0.041 Uiso 1 1 calc R U . . .
H7B H -0.125234 0.440218 0.157574 0.041 Uiso 1 1 calc R U . . .
C8 C -0.0624(3) 0.3713(3) 0.2705(2) 0.0347(9) Uani 1 1 d . . . . .
H8A H 0.000231 0.384238 0.246785 0.042 Uiso 1 1 calc R U . . .
H8B H -0.062116 0.309619 0.315843 0.042 Uiso 1 1 calc R U . . .
C9 C -0.0936(3) 0.4352(3) 0.3102(3) 0.0352(9) Uani 1 1 d . . . . .
H9A H -0.158244 0.427905 0.328187 0.042 Uiso 1 1 calc R U . . .
H9B H -0.059035 0.421793 0.361027 0.042 Uiso 1 1 calc R U . . .
C10 C -0.0785(3) 0.5299(2) 0.2444(2) 0.0273(8) Uani 1 1 d . . . . .
V5 V 0.43222(4) 0.32577(4) 0.34127(4) 0.02706(16) Uani 1 1 d . . . . .
V6 V 0.64635(4) 0.74762(4) 0.46243(4) 0.02700(16) Uani 1 1 d . . . . .
V7 V 0.44092(4) 0.76717(4) 0.40057(4) 0.02662(16) Uani 1 1 d . . . . .
V8 V 0.36266(4) 0.69258(4) 0.59805(4) 0.02765(16) Uani 1 1 d . . . . .
Cl2 Cl 0.48535(6) 0.38435(6) 0.45870(6) 0.02491(19) Uani 1 1 d . . . . .
O17 O 0.39865(18) 0.29765(19) 0.27223(18) 0.0349(6) Uani 1 1 d . . . . .
O18 O 0.37771(17) 0.24377(16) 0.43900(17) 0.0285(6) Uani 1 1 d . . . . .
O19 O 0.54463(17) 0.27661(16) 0.35764(16) 0.0286(6) Uani 1 1 d . . . . .
O20 O 0.32695(17) 0.40925(17) 0.33936(16) 0.0286(6) Uani 1 1 d . . . . .
O21 O 0.27273(16) 0.35791(16) 0.47509(16) 0.0273(6) Uani 1 1 d . . . . .
O22 O 0.48568(18) 0.44156(17) 0.26096(16) 0.0301(6) Uani 1 1 d . . . . .
O23 O 0.62838(18) 0.42618(17) 0.30115(17) 0.0309(6) Uani 1 1 d . . . . .
O24 O 0.72087(19) 0.81860(18) 0.41521(18) 0.0367(7) Uani 1 1 d . . . . .
O25 O 0.54440(18) 0.80995(16) 0.40925(17) 0.0304(6) Uani 1 1 d . . . . .
O26 O 0.3985(2) 0.84875(18) 0.32139(18) 0.0382(7) Uani 1 1 d . . . . .
O27 O 0.37847(18) 0.77608(17) 0.49110(17) 0.0307(6) Uani 1 1 d . . . . .
O28 O 0.27616(18) 0.7306(2) 0.63234(19) 0.0378(7) Uani 1 1 d . . . . .
O29 O 0.65094(17) 0.68881(17) 0.38284(16) 0.0289(6) Uani 1 1 d . . . . .
O30 O 0.50999(18) 0.70430(17) 0.33895(16) 0.0300(6) Uani 1 1 d . . . . .
O31 O 0.35275(17) 0.67509(17) 0.41484(17) 0.0302(6) Uani 1 1 d . . . . .
O32 O 0.30347(17) 0.62013(17) 0.55244(17) 0.0299(6) Uani 1 1 d . . . . .
C11 C 0.2725(2) 0.4124(2) 0.3973(2) 0.0245(8) Uani 1 1 d . . . . .
C12 C 0.2042(2) 0.4888(3) 0.3721(2) 0.0293(8) Uani 1 1 d . . . . .
H12A H 0.149544 0.470753 0.410474 0.035 Uiso 1 1 calc R U . . .
H12B H 0.186730 0.506048 0.313083 0.035 Uiso 1 1 calc R U . . .
C13 C 0.2450(3) 0.5680(2) 0.3778(2) 0.0305(8) Uani 1 1 d . . . . .
H13A H 0.303849 0.580193 0.345434 0.037 Uiso 1 1 calc R U . . .
H13B H 0.204800 0.621384 0.351010 0.037 Uiso 1 1 calc R U . . .
C14 C 0.2583(3) 0.5513(3) 0.4693(3) 0.0326(9) Uani 1 1 d . . . . .
H14A H 0.198454 0.546204 0.499296 0.039 Uiso 1 1 calc R U . . .
H14B H 0.291632 0.493592 0.497858 0.039 Uiso 1 1 calc R U . . .
C15 C 0.3083(2) 0.6218(2) 0.4788(2) 0.0278(8) Uani 1 1 d . . . . .
C16 C 0.5646(3) 0.4687(3) 0.2550(2) 0.0291(8) Uani 1 1 d . . . . .
C17 C 0.5825(3) 0.5624(3) 0.1887(2) 0.0354(9) Uani 1 1 d . . . . .
H17A H 0.546150 0.577120 0.138662 0.042 Uiso 1 1 calc R U . . .
H17B H 0.646944 0.566829 0.169384 0.042 Uiso 1 1 calc R U . . .
C18 C 0.5577(3) 0.6277(3) 0.2278(2) 0.0331(9) Uani 1 1 d . . . . .
H18A H 0.561801 0.689172 0.182471 0.040 Uiso 1 1 calc R U . . .
H18B H 0.494446 0.619433 0.250636 0.040 Uiso 1 1 calc R U . . .
C19 C 0.6181(3) 0.6162(3) 0.2991(3) 0.0324(9) Uani 1 1 d . . . . .
H19A H 0.617451 0.553440 0.342173 0.039 Uiso 1 1 calc R U . . .
H19B H 0.680666 0.628563 0.275118 0.039 Uiso 1 1 calc R U . . .
C20 C 0.5911(3) 0.6751(2) 0.3426(2) 0.0268(8) Uani 1 1 d . . . . .
N1 N 0.6770(3) 0.0763(3) 0.3071(3) 0.0564(11) Uani 1 1 d . . . . .
C21 C 0.6179(3) 0.0220(4) 0.2875(3) 0.0567(13) Uani 1 1 d . . . . .
H21A H 0.556501 0.050046 0.281174 0.068 Uiso 1 1 calc R U . . .
H21B H 0.614813 -0.036894 0.337180 0.068 Uiso 1 1 calc R U . . .
C22 C 0.6436(4) 0.0072(5) 0.2088(4) 0.0733(19) Uani 1 1 d . . . . .
H22A H 0.649401 0.065552 0.158863 0.088 Uiso 1 1 calc R U . . .
H22B H 0.703018 -0.024811 0.215980 0.088 Uiso 1 1 calc R U . . .
C23 C 0.5770(5) -0.0443(5) 0.1918(4) 0.084(2) Uani 1 1 d . . . . .
H23A H 0.565460 -0.098492 0.245094 0.101 Uiso 1 1 calc R U . . .
H23B H 0.519851 -0.008359 0.178408 0.101 Uiso 1 1 calc R U . . .
C24 C 0.5999(7) -0.0712(5) 0.1245(5) 0.120(3) Uani 1 1 d . . . . .
H24A H 0.599995 -0.018717 0.069451 0.179 Uiso 1 1 calc R U . . .
H24B H 0.555512 -0.112342 0.125592 0.179 Uiso 1 1 calc R U . . .
H24C H 0.659877 -0.100764 0.132779 0.179 Uiso 1 1 calc R U . . .
C25 C 0.6757(4) 0.1730(3) 0.2367(3) 0.0508(12) Uani 1 1 d . . . . .
H25A H 0.701431 0.209947 0.260541 0.061 Uiso 1 1 calc R U . . .
H25B H 0.717918 0.173952 0.189753 0.061 Uiso 1 1 calc R U . . .
C26 C 0.5907(3) 0.2191(3) 0.1976(4) 0.0554(13) Uani 1 1 d . . . . .
H26A H 0.543807 0.213273 0.242765 0.067 Uiso 1 1 calc R U . . .
H26B H 0.569067 0.191558 0.162535 0.067 Uiso 1 1 calc R U . . .
C27 C 0.6074(3) 0.3165(3) 0.1422(3) 0.0478(11) Uani 1 1 d . . . . .
H27A H 0.622797 0.343978 0.179404 0.057 Uiso 1 1 calc R U . . .
H27B H 0.660420 0.320495 0.103172 0.057 Uiso 1 1 calc R U . . .
C28 C 0.5296(4) 0.3704(4) 0.0893(3) 0.0635(15) Uani 1 1 d . . . . .
H28A H 0.518660 0.348964 0.046769 0.095 Uiso 1 1 calc R U . . .
H28B H 0.544590 0.433188 0.060299 0.095 Uiso 1 1 calc R U . . .
H28C H 0.475396 0.363968 0.126534 0.095 Uiso 1 1 calc R U . . .
C29 C 0.6426(4) 0.0796(3) 0.3906(3) 0.0549(13) Uani 1 1 d . . . . .
H29A H 0.678616 0.122479 0.399193 0.066 Uiso 1 1 calc R U . . .
H29B H 0.579603 0.103489 0.383899 0.066 Uiso 1 1 calc R U . . .
C30 C 0.6452(4) -0.0073(4) 0.4707(4) 0.0707(16) Uani 1 1 d . . . . .
H30A H 0.706248 -0.035703 0.475021 0.085 Uiso 1 1 calc R U . . .
H30B H 0.602201 -0.047997 0.466995 0.085 Uiso 1 1 calc R U . . .
C31 C 0.6204(5) 0.0075(5) 0.5525(4) 0.086(2) Uani 1 1 d . . . . .
H31A H 0.656893 0.056299 0.549374 0.103 Uiso 1 1 calc R U . . .
H31B H 0.556529 0.028678 0.550071 0.103 Uiso 1 1 calc R U . . .
C32 C 0.6311(8) -0.0624(5) 0.6308(5) 0.130(4) Uani 1 1 d . . . . .
H32A H 0.642815 -0.117397 0.623967 0.195 Uiso 1 1 calc R U . . .
H32B H 0.576204 -0.067523 0.666917 0.195 Uiso 1 1 calc R U . . .
H32C H 0.682092 -0.052232 0.657554 0.195 Uiso 1 1 calc R U . . .
C33 C 0.7734(3) 0.0384(3) 0.3146(3) 0.0509(12) Uani 1 1 d . . . . .
H33A H 0.795964 0.043931 0.257788 0.061 Uiso 1 1 calc R U . . .
H33B H 0.772182 -0.025858 0.353279 0.061 Uiso 1 1 calc R U . . .
C34 C 0.8413(4) 0.0800(4) 0.3470(4) 0.0625(14) Uani 1 1 d . . . . .
H34A H 0.836077 0.145546 0.315814 0.075 Uiso 1 1 calc R U . . .
H34B H 0.827740 0.063608 0.408353 0.075 Uiso 1 1 calc R U . . .
C35 C 0.9349(3) 0.0484(4) 0.3345(4) 0.0620(14) Uani 1 1 d . . . . .
H35A H 0.948832 0.066980 0.272854 0.074 Uiso 1 1 calc R U . . .
H35B H 0.938821 -0.017362 0.363356 0.074 Uiso 1 1 calc R U . . .
C36 C 1.0046(5) 0.0851(5) 0.3696(5) 0.087(2) Uani 1 1 d . . . . .
H36A H 1.006334 0.149682 0.336256 0.130 Uiso 1 1 calc R U . . .
H36B H 1.064074 0.057882 0.365603 0.130 Uiso 1 1 calc R U . . .
H36C H 0.988145 0.071289 0.429326 0.130 Uiso 1 1 calc R U . . .
N2A N 0.1916(2) 0.9301(2) 0.1791(2) 0.0434(8) Uani 0.5 1 d D . P A 1
C37A C 0.1038(5) 0.9767(6) 0.1481(6) 0.0453(17) Uani 0.5 1 d D U P A 1
H37A H 0.114623 1.023333 0.089393 0.054 Uiso 0.5 1 calc R U P A 1
H37B H 0.082709 1.007211 0.184081 0.054 Uiso 0.5 1 calc R U P A 1
C38A C 0.0289(6) 0.9219(6) 0.1467(7) 0.0518(17) Uani 0.5 1 d D U P A 1
H38A H 0.045839 0.896407 0.105678 0.062 Uiso 0.5 1 calc R U P A 1
H38B H 0.020017 0.872056 0.203855 0.062 Uiso 0.5 1 calc R U P A 1
C39A C -0.0576(8) 0.9755(9) 0.1221(12) 0.061(2) Uani 0.5 1 d D U P A 1
H39A H -0.044871 1.030835 0.070318 0.073 Uiso 0.5 1 calc R U P A 1
H39B H -0.078236 0.992818 0.168246 0.073 Uiso 0.5 1 calc R U P A 1
C40A C -0.1335(6) 0.9324(7) 0.1049(7) 0.052(2) Uani 0.5 1 d D U P A 1
H40A H -0.109374 0.885651 0.088604 0.078 Uiso 0.5 1 calc R U P A 1
H40B H -0.167991 0.977002 0.058488 0.078 Uiso 0.5 1 calc R U P A 1
H40C H -0.173053 0.906232 0.156441 0.078 Uiso 0.5 1 calc R U P A 1
C41A C 0.2565(6) 0.9936(5) 0.1833(5) 0.0446(16) Uani 0.5 1 d D U P A 1
H41A H 0.226554 1.023470 0.216975 0.053 Uiso 0.5 1 calc R U P A 1
H41B H 0.309052 0.958358 0.214784 0.053 Uiso 0.5 1 calc R U P A 1
C42A C 0.2905(7) 1.0634(6) 0.0999(6) 0.057(2) Uani 0.5 1 d D U P A 1
H42A H 0.238889 1.095460 0.064806 0.068 Uiso 0.5 1 calc R U P A 1
H42B H 0.328363 1.035187 0.068648 0.068 Uiso 0.5 1 calc R U P A 1
C43A C 0.3446(8) 1.1280(8) 0.1137(7) 0.064(2) Uani 0.5 1 d D U P A 1
H43A H 0.304731 1.158004 0.142075 0.077 Uiso 0.5 1 calc R U P A 1
H43B H 0.392339 1.094189 0.153244 0.077 Uiso 0.5 1 calc R U P A 1
C44A C 0.3876(9) 1.1972(9) 0.0355(8) 0.088(4) Uani 0.5 1 d D U P A 1
H44A H 0.428220 1.168599 0.007219 0.132 Uiso 0.5 1 calc R U P A 1
H44B H 0.421939 1.235516 0.051068 0.132 Uiso 0.5 1 calc R U P A 1
H44C H 0.340954 1.233106 -0.003232 0.132 Uiso 0.5 1 calc R U P A 1
C45A C 0.1786(7) 0.8584(6) 0.2694(5) 0.0540(18) Uani 0.5 1 d D U P A 1
H45A H 0.142053 0.812131 0.267321 0.065 Uiso 0.5 1 calc R U P A 1
H45B H 0.238474 0.830499 0.288827 0.065 Uiso 0.5 1 calc R U P A 1
C46A C 0.1353(12) 0.8847(8) 0.3357(7) 0.069(2) Uani 0.5 1 d D U P A 1
H46A H 0.163244 0.938596 0.331467 0.083 Uiso 0.5 1 calc R U P A 1
H46B H 0.070471 0.899043 0.325251 0.083 Uiso 0.5 1 calc R U P A 1
C47A C 0.1456(10) 0.8120(9) 0.4227(7) 0.076(3) Uani 0.5 1 d D U P A 1
H47A H 0.117426 0.758397 0.426275 0.091 Uiso 0.5 1 calc R U P A 1
H47B H 0.210522 0.797258 0.432079 0.091 Uiso 0.5 1 calc R U P A 1
C48A C 0.1050(12) 0.8340(12) 0.4914(9) 0.105(4) Uani 0.5 1 d D U P A 1
H48A H 0.127472 0.890503 0.484676 0.158 Uiso 0.5 1 calc R U P A 1
H48B H 0.121258 0.786845 0.546769 0.158 Uiso 0.5 1 calc R U P A 1
H48C H 0.039317 0.839105 0.488206 0.158 Uiso 0.5 1 calc R U P A 1
C49A C 0.2280(6) 0.8834(7) 0.1263(7) 0.0545(18) Uani 0.5 1 d D U P A 1
H49A H 0.181702 0.843363 0.126919 0.065 Uiso 0.5 1 calc R U P A 1
H49B H 0.237042 0.928583 0.066731 0.065 Uiso 0.5 1 calc R U P A 1
C50A C 0.3142(7) 0.8301(8) 0.1526(9) 0.073(2) Uani 0.5 1 d D U P A 1
H50A H 0.361050 0.870793 0.149610 0.088 Uiso 0.5 1 calc R U P A 1
H50B H 0.305901 0.786865 0.213074 0.088 Uiso 0.5 1 calc R U P A 1
C51A C 0.3489(13) 0.7806(10) 0.1031(8) 0.072(2) Uani 0.5 1 d D U P A 1
H51A H 0.404124 0.745373 0.128205 0.087 Uiso 0.5 1 calc R U P A 1
H51B H 0.303317 0.739153 0.105172 0.087 Uiso 0.5 1 calc R U P A 1
C52A C 0.3685(11) 0.8420(10) 0.0166(9) 0.102(4) Uani 0.5 1 d D U P A 1
H52A H 0.400624 0.891802 0.015451 0.152 Uiso 0.5 1 calc R U P A 1
H52B H 0.312186 0.864282 -0.012696 0.152 Uiso 0.5 1 calc R U P A 1
H52C H 0.406253 0.811854 -0.012162 0.152 Uiso 0.5 1 calc R U P A 1
N2B N 0.1916(2) 0.9301(2) 0.1791(2) 0.0434(8) Uani 0.5 1 d D U P B 2
C37B C 0.1042(5) 0.9224(6) 0.1442(7) 0.0476(16) Uani 0.5 1 d D U P B 2
H37C H 0.119230 0.918973 0.089423 0.057 Uiso 0.5 1 calc R U P B 2
H37D H 0.078712 0.864943 0.183980 0.057 Uiso 0.5 1 calc R U P B 2
C38B C 0.0307(6) 0.9935(7) 0.1289(8) 0.0604(19) Uani 0.5 1 d D U P B 2
H38C H 0.022584 1.005024 0.180120 0.073 Uiso 0.5 1 calc R U P B 2
H38D H 0.051244 1.048910 0.080886 0.073 Uiso 0.5 1 calc R U P B 2
C39B C -0.0591(8) 0.9735(11) 0.1093(11) 0.069(3) Uani 0.5 1 d D U P B 2
H39C H -0.097226 1.028967 0.088722 0.083 Uiso 0.5 1 calc R U P B 2
H39D H -0.050080 0.955473 0.062106 0.083 Uiso 0.5 1 calc R U P B 2
C40B C -0.1092(10) 0.9028(9) 0.1819(10) 0.092(3) Uani 0.5 1 d D U P B 2
H40D H -0.154120 0.879266 0.159595 0.139 Uiso 0.5 1 calc R U P B 2
H40E H -0.139516 0.928183 0.218613 0.139 Uiso 0.5 1 calc R U P B 2
H40F H -0.066830 0.854743 0.214988 0.139 Uiso 0.5 1 calc R U P B 2
C41B C 0.2311(6) 1.0172(5) 0.1162(6) 0.0518(18) Uani 0.5 1 d D U P B 2
H41C H 0.229337 1.020261 0.058290 0.062 Uiso 0.5 1 calc R U P B 2
H41D H 0.191032 1.066207 0.117856 0.062 Uiso 0.5 1 calc R U P B 2
C42B C 0.3252(7) 1.0345(7) 0.1282(8) 0.067(2) Uani 0.5 1 d D U P B 2
H42C H 0.328486 1.027075 0.187446 0.080 Uiso 0.5 1 calc R U P B 2
H42D H 0.366266 0.988593 0.121592 0.080 Uiso 0.5 1 calc R U P B 2
C43B C 0.3592(9) 1.1234(7) 0.0695(8) 0.070(2) Uani 0.5 1 d D U P B 2
H43C H 0.423453 1.116656 0.053500 0.084 Uiso 0.5 1 calc R U P B 2
H43D H 0.325360 1.147738 0.016795 0.084 Uiso 0.5 1 calc R U P B 2
C44B C 0.3500(10) 1.1865(9) 0.1082(9) 0.081(3) Uani 0.5 1 d D U P B 2
H44D H 0.286362 1.194561 0.122866 0.122 Uiso 0.5 1 calc R U P B 2
H44E H 0.373429 1.243828 0.067588 0.122 Uiso 0.5 1 calc R U P B 2
H44F H 0.384250 1.163153 0.159941 0.122 Uiso 0.5 1 calc R U P B 2
C45B C 0.1793(7) 0.9319(6) 0.2634(5) 0.0529(17) Uani 0.5 1 d D U P B 2
H45C H 0.145468 0.987735 0.255570 0.063 Uiso 0.5 1 calc R U P B 2
H45D H 0.239621 0.934786 0.282219 0.063 Uiso 0.5 1 calc R U P B 2
C46B C 0.1326(11) 0.8573(8) 0.3336(6) 0.067(2) Uani 0.5 1 d D U P B 2
H46C H 0.155198 0.800317 0.333372 0.080 Uiso 0.5 1 calc R U P B 2
H46D H 0.067167 0.863741 0.324551 0.080 Uiso 0.5 1 calc R U P B 2
C47B C 0.1480(10) 0.8559(9) 0.4179(7) 0.071(3) Uani 0.5 1 d D U P B 2
H47C H 0.213341 0.850313 0.427214 0.086 Uiso 0.5 1 calc R U P B 2
H47D H 0.123751 0.911863 0.419463 0.086 Uiso 0.5 1 calc R U P B 2
C48B C 0.1017(11) 0.7790(9) 0.4855(9) 0.092(4) Uani 0.5 1 d D U P B 2
H48D H 0.036969 0.785508 0.476262 0.138 Uiso 0.5 1 calc R U P B 2
H48E H 0.111476 0.776716 0.541382 0.138 Uiso 0.5 1 calc R U P B 2
H48F H 0.125973 0.723958 0.483408 0.138 Uiso 0.5 1 calc R U P B 2
C49B C 0.2536(6) 0.8537(6) 0.1838(6) 0.0526(17) Uani 0.5 1 d D U P B 2
H49C H 0.305060 0.852399 0.217241 0.063 Uiso 0.5 1 calc R U P B 2
H49D H 0.220912 0.798543 0.217674 0.063 Uiso 0.5 1 calc R U P B 2
C50B C 0.2920(7) 0.8480(7) 0.1043(6) 0.0578(18) Uani 0.5 1 d D U P B 2
H50C H 0.242806 0.848033 0.069104 0.069 Uiso 0.5 1 calc R U P B 2
H50D H 0.329381 0.899679 0.070371 0.069 Uiso 0.5 1 calc R U P B 2
C51B C 0.3481(12) 0.7638(9) 0.1302(8) 0.071(2) Uani 0.5 1 d D U P B 2
H51C H 0.391265 0.760560 0.172094 0.085 Uiso 0.5 1 calc R U P B 2
H51D H 0.308762 0.712487 0.158040 0.085 Uiso 0.5 1 calc R U P B 2
C52B C 0.3986(8) 0.7584(8) 0.0557(8) 0.069(3) Uani 0.5 1 d D U P B 2
H52D H 0.356808 0.769240 0.011028 0.103 Uiso 0.5 1 calc R U P B 2
H52E H 0.427533 0.699080 0.073324 0.103 Uiso 0.5 1 calc R U P B 2
H52F H 0.444598 0.803209 0.033736 0.103 Uiso 0.5 1 calc R U P B 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
V1 O1 1.590(3) . ?
V1 O2 1.785(3) . ?
V1 O4 1.839(3) . ?
V1 O7 1.994(3) . ?
V1 O5 2.009(3) . ?
V2 O3 1.593(3) . ?
V2 O12 1.784(3) 2_565 ?
V2 O2 1.834(3) . ?
V2 O16 2.000(3) 2_565 ?
V2 O8 2.023(3) . ?
V3 O9 1.587(3) . ?
V3 O4 1.789(3) 2_565 ?
V3 O10 1.844(3) . ?
V3 O6 2.001(3) 2_565 ?
V3 O13 2.012(3) . ?
V4 O11 1.596(3) . ?
V4 O10 1.792(3) . ?
V4 O12 1.846(3) . ?
V4 O14 1.990(3) . ?
V4 O15 2.023(3) . ?
V4 Cl1 2.7947(11) . ?
O5 C1 1.258(5) . ?
O6 C1 1.269(5) . ?
O7 C6 1.267(5) . ?
O8 C6 1.268(5) . ?
O13 C10 1.260(5) . ?
O14 C10 1.270(5) . ?
O15 C5 1.260(5) . ?
O16 C5 1.271(5) . ?
C1 C2 1.501(5) . ?
C2 C3 1.521(6) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 C4 1.530(5) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 C5 1.518(5) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C6 C7 1.505(5) . ?
C7 C8 1.514(5) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 C9 1.538(6) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 C10 1.518(5) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
V5 O17 1.591(3) . ?
V5 O19 1.801(3) . ?
V5 O18 1.833(3) . ?
V5 O22 2.008(3) . ?
V5 O20 2.020(3) . ?
V6 O24 1.585(3) . ?
V6 O18 1.794(3) 2_666 ?
V6 O25 1.846(3) . ?
V6 O21 1.997(3) 2_666 ?
V6 O29 2.014(3) . ?
V7 O26 1.595(3) . ?
V7 O25 1.785(3) . ?
V7 O27 1.830(3) . ?
V7 O30 1.997(3) . ?
V7 O31 2.012(3) . ?
V8 O28 1.590(3) . ?
V8 O27 1.789(3) . ?
V8 O19 1.835(3) 2_666 ?
V8 O32 1.989(3) . ?
V8 O23 2.004(3) 2_666 ?
O20 C11 1.266(4) . ?
O21 C11 1.264(4) . ?
O22 C16 1.270(5) . ?
O23 C16 1.256(5) . ?
O29 C20 1.264(5) . ?
O30 C20 1.268(5) . ?
O31 C15 1.258(5) . ?
O32 C15 1.269(5) . ?
C11 C12 1.503(5) . ?
C12 C13 1.538(5) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C13 C14 1.520(5) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C14 C15 1.509(5) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C16 C17 1.517(5) . ?
C17 C18 1.532(5) . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C18 C19 1.525(5) . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C19 C20 1.503(5) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
N1 C21 1.462(6) . ?
N1 C33 1.521(6) . ?
N1 C29 1.530(6) . ?
N1 C25 1.548(6) . ?
C21 C22 1.516(7) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C22 C23 1.479(8) . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C23 C24 1.439(9) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 C26 1.483(7) . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C26 C27 1.517(7) . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C27 C28 1.517(7) . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 C30 1.518(7) . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C30 C31 1.564(8) . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C31 C32 1.370(9) . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C33 C34 1.531(7) . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
C34 C35 1.493(8) . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
C35 C36 1.528(8) . ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
N2A C37A 1.487(7) . ?
N2A C49A 1.496(7) . ?
N2A C41A 1.512(6) . ?
N2A C45A 1.516(7) . ?
C37A C38A 1.499(7) . ?
C37A H37A 0.9900 . ?
C37A H37B 0.9900 . ?
C38A C39A 1.496(9) . ?
C38A H38A 0.9900 . ?
C38A H38B 0.9900 . ?
C39A C40A 1.495(8) . ?
C39A H39A 0.9900 . ?
C39A H39B 0.9900 . ?
C40A H40A 0.9800 . ?
C40A H40B 0.9800 . ?
C40A H40C 0.9800 . ?
C41A C42A 1.494(8) . ?
C41A H41A 0.9900 . ?
C41A H41B 0.9900 . ?
C42A C43A 1.498(8) . ?
C42A H42A 0.9900 . ?
C42A H42B 0.9900 . ?
C43A C44A 1.486(8) . ?
C43A H43A 0.9900 . ?
C43A H43B 0.9900 . ?
C44A H44A 0.9800 . ?
C44A H44B 0.9800 . ?
C44A H44C 0.9800 . ?
C45A C46A 1.495(8) . ?
C45A H45A 0.9900 . ?
C45A H45B 0.9900 . ?
C46A C47A 1.487(8) . ?
C46A H46A 0.9900 . ?
C46A H46B 0.9900 . ?
C47A C48A 1.475(9) . ?
C47A H47A 0.9900 . ?
C47A H47B 0.9900 . ?
C48A H48A 0.9800 . ?
C48A H48B 0.9800 . ?
C48A H48C 0.9800 . ?
C49A C50A 1.493(8) . ?
C49A H49A 0.9900 . ?
C49A H49B 0.9900 . ?
C50A C51A 1.481(8) . ?
C50A H50A 0.9900 . ?
C50A H50B 0.9900 . ?
C51A C52A 1.430(8) . ?
C51A H51A 0.9900 . ?
C51A H51B 0.9900 . ?
C52A H52A 0.9800 . ?
C52A H52B 0.9800 . ?
C52A H52C 0.9800 . ?
N2B C45B 1.481(7) . ?
N2B C49B 1.500(7) . ?
N2B C37B 1.512(7) . ?
N2B C41B 1.518(7) . ?
C37B C38B 1.508(8) . ?
C37B H37C 0.9900 . ?
C37B H37D 0.9900 . ?
C38B C39B 1.498(8) . ?
C38B H38C 0.9900 . ?
C38B H38D 0.9900 . ?
C39B C40B 1.496(9) . ?
C39B H39C 0.9900 . ?
C39B H39D 0.9900 . ?
C40B H40D 0.9800 . ?
C40B H40E 0.9800 . ?
C40B H40F 0.9800 . ?
C41B C42B 1.498(8) . ?
C41B H41C 0.9900 . ?
C41B H41D 0.9900 . ?
C42B C43B 1.488(8) . ?
C42B H42C 0.9900 . ?
C42B H42D 0.9900 . ?
C43B C44B 1.474(8) . ?
C43B H43C 0.9900 . ?
C43B H43D 0.9900 . ?
C44B H44D 0.9800 . ?
C44B H44E 0.9800 . ?
C44B H44F 0.9800 . ?
C45B C46B 1.485(8) . ?
C45B H45C 0.9900 . ?
C45B H45D 0.9900 . ?
C46B C47B 1.495(8) . ?
C46B H46C 0.9900 . ?
C46B H46D 0.9900 . ?
C47B C48B 1.484(8) . ?
C47B H47C 0.9900 . ?
C47B H47D 0.9900 . ?
C48B H48D 0.9800 . ?
C48B H48E 0.9800 . ?
C48B H48F 0.9800 . ?
C49B C50B 1.499(8) . ?
C49B H49C 0.9900 . ?
C49B H49D 0.9900 . ?
C50B C51B 1.492(8) . ?
C50B H50C 0.9900 . ?
C50B H50D 0.9900 . ?
C51B C52B 1.486(8) . ?
C51B H51C 0.9900 . ?
C51B H51D 0.9900 . ?
C52B H52D 0.9800 . ?
C52B H52E 0.9800 . ?
C52B H52F 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 V1 O2 102.47(13) . . ?
O1 V1 O4 102.29(14) . . ?
O2 V1 O4 96.45(12) . . ?
O1 V1 O7 98.88(13) . . ?
O2 V1 O7 88.80(12) . . ?
O4 V1 O7 156.49(11) . . ?
O1 V1 O5 98.17(13) . . ?
O2 V1 O5 158.00(12) . . ?
O4 V1 O5 86.43(11) . . ?
O7 V1 O5 80.52(11) . . ?
O3 V2 O12 102.28(14) . 2_565 ?
O3 V2 O2 100.87(14) . . ?
O12 V2 O2 98.65(12) 2_565 . ?
O3 V2 O16 98.56(14) . 2_565 ?
O12 V2 O16 88.32(12) 2_565 2_565 ?
O2 V2 O16 157.40(11) . 2_565 ?
O3 V2 O8 99.74(14) . . ?
O12 V2 O8 156.02(11) 2_565 . ?
O2 V2 O8 86.35(12) . . ?
O16 V2 O8 79.07(11) 2_565 . ?
O9 V3 O4 102.47(14) . 2_565 ?
O9 V3 O10 102.33(14) . . ?
O4 V3 O10 98.00(12) 2_565 . ?
O9 V3 O6 100.42(13) . 2_565 ?
O4 V3 O6 88.67(12) 2_565 2_565 ?
O10 V3 O6 154.25(12) . 2_565 ?
O9 V3 O13 97.85(13) . . ?
O4 V3 O13 158.14(12) 2_565 . ?
O10 V3 O13 85.31(11) . . ?
O6 V3 O13 79.77(11) 2_565 . ?
O11 V4 O10 102.48(14) . . ?
O11 V4 O12 101.54(13) . . ?
O10 V4 O12 96.00(12) . . ?
O11 V4 O14 98.18(13) . . ?
O10 V4 O14 88.88(11) . . ?
O12 V4 O14 158.11(12) . . ?
O11 V4 O15 96.92(13) . . ?
O10 V4 O15 159.50(12) . . ?
O12 V4 O15 86.47(11) . . ?
O14 V4 O15 81.81(11) . . ?
O11 V4 Cl1 175.50(11) . . ?
O10 V4 Cl1 81.53(9) . . ?
O12 V4 Cl1 79.90(8) . . ?
O14 V4 Cl1 79.74(8) . . ?
O15 V4 Cl1 78.87(8) . . ?
V1 O2 V2 127.83(14) . . ?
V3 O4 V1 128.87(14) 2_565 . ?
C1 O5 V1 133.3(3) . . ?
C1 O6 V3 131.1(2) . 2_565 ?
C6 O7 V1 131.2(2) . . ?
C6 O8 V2 132.3(3) . . ?
V4 O10 V3 127.25(15) . . ?
V2 O12 V4 127.49(14) 2_565 . ?
C10 O13 V3 132.7(2) . . ?
C10 O14 V4 130.5(2) . . ?
C5 O15 V4 132.9(3) . . ?
C5 O16 V2 130.7(3) . 2_565 ?
O5 C1 O6 125.1(3) . . ?
O5 C1 C2 118.0(4) . . ?
O6 C1 C2 116.9(3) . . ?
C1 C2 C3 114.5(3) . . ?
C1 C2 H2A 108.6 . . ?
C3 C2 H2A 108.6 . . ?
C1 C2 H2B 108.6 . . ?
C3 C2 H2B 108.6 . . ?
H2A C2 H2B 107.6 . . ?
C2 C3 C4 113.0(3) . . ?
C2 C3 H3A 109.0 . . ?
C4 C3 H3A 109.0 . . ?
C2 C3 H3B 109.0 . . ?
C4 C3 H3B 109.0 . . ?
H3A C3 H3B 107.8 . . ?
C5 C4 C3 109.4(3) . . ?
C5 C4 H4A 109.8 . . ?
C3 C4 H4A 109.8 . . ?
C5 C4 H4B 109.8 . . ?
C3 C4 H4B 109.8 . . ?
H4A C4 H4B 108.2 . . ?
O15 C5 O16 125.4(4) . . ?
O15 C5 C4 117.8(3) . . ?
O16 C5 C4 116.7(4) . . ?
O7 C6 O8 125.1(4) . . ?
O7 C6 C7 117.8(3) . . ?
O8 C6 C7 117.1(3) . . ?
C6 C7 C8 114.1(3) . . ?
C6 C7 H7A 108.7 . . ?
C8 C7 H7A 108.7 . . ?
C6 C7 H7B 108.7 . . ?
C8 C7 H7B 108.7 . . ?
H7A C7 H7B 107.6 . . ?
C7 C8 C9 113.5(3) . . ?
C7 C8 H8A 108.9 . . ?
C9 C8 H8A 108.9 . . ?
C7 C8 H8B 108.9 . . ?
C9 C8 H8B 108.9 . . ?
H8A C8 H8B 107.7 . . ?
C10 C9 C8 108.9(3) . . ?
C10 C9 H9A 109.9 . . ?
C8 C9 H9A 109.9 . . ?
C10 C9 H9B 109.9 . . ?
C8 C9 H9B 109.9 . . ?
H9A C9 H9B 108.3 . . ?
O13 C10 O14 125.7(3) . . ?
O13 C10 C9 117.7(3) . . ?
O14 C10 C9 116.6(3) . . ?
O17 V5 O19 102.25(13) . . ?
O17 V5 O18 100.89(13) . . ?
O19 V5 O18 97.69(12) . . ?
O17 V5 O22 98.23(13) . . ?
O19 V5 O22 88.39(11) . . ?
O18 V5 O22 158.18(11) . . ?
O17 V5 O20 97.34(13) . . ?
O19 V5 O20 158.78(11) . . ?
O18 V5 O20 86.44(11) . . ?
O22 V5 O20 80.76(11) . . ?
O24 V6 O18 103.51(14) . 2_666 ?
O24 V6 O25 101.11(13) . . ?
O18 V6 O25 96.71(12) 2_666 . ?
O24 V6 O21 98.72(13) . 2_666 ?
O18 V6 O21 88.14(11) 2_666 2_666 ?
O25 V6 O21 157.84(11) . 2_666 ?
O24 V6 O29 98.95(13) . . ?
O18 V6 O29 155.96(11) 2_666 . ?
O25 V6 O29 87.18(11) . . ?
O21 V6 O29 80.03(11) 2_666 . ?
O26 V7 O25 102.15(14) . . ?
O26 V7 O27 102.15(14) . . ?
O25 V7 O27 97.93(12) . . ?
O26 V7 O30 99.42(13) . . ?
O25 V7 O30 88.38(12) . . ?
O27 V7 O30 155.65(11) . . ?
O26 V7 O31 98.53(13) . . ?
O25 V7 O31 157.61(11) . . ?
O27 V7 O31 85.92(11) . . ?
O30 V7 O31 79.81(11) . . ?
O28 V8 O27 102.33(14) . . ?
O28 V8 O19 102.71(13) . 2_666 ?
O27 V8 O19 96.69(12) . 2_666 ?
O28 V8 O32 99.80(13) . . ?
O27 V8 O32 88.59(12) . . ?
O19 V8 O32 155.16(11) 2_666 . ?
O28 V8 O23 97.14(14) . 2_666 ?
O27 V8 O23 159.18(12) . 2_666 ?
O19 V8 O23 86.06(11) 2_666 2_666 ?
O32 V8 O23 80.84(11) . 2_666 ?
V6 O18 V5 127.09(14) 2_666 . ?
V5 O19 V8 127.35(14) . 2_666 ?
C11 O20 V5 132.5(2) . . ?
C11 O21 V6 131.3(2) . 2_666 ?
C16 O22 V5 130.2(3) . . ?
C16 O23 V8 132.9(3) . 2_666 ?
V7 O25 V6 128.32(14) . . ?
V8 O27 V7 128.75(15) . . ?
C20 O29 V6 132.5(2) . . ?
C20 O30 V7 131.4(2) . . ?
C15 O31 V7 132.3(3) . . ?
C15 O32 V8 131.1(2) . . ?
O21 C11 O20 125.1(3) . . ?
O21 C11 C12 117.5(3) . . ?
O20 C11 C12 117.4(3) . . ?
C11 C12 C13 109.3(3) . . ?
C11 C12 H12A 109.8 . . ?
C13 C12 H12A 109.8 . . ?
C11 C12 H12B 109.8 . . ?
C13 C12 H12B 109.8 . . ?
H12A C12 H12B 108.3 . . ?
C14 C13 C12 112.5(3) . . ?
C14 C13 H13A 109.1 . . ?
C12 C13 H13A 109.1 . . ?
C14 C13 H13B 109.1 . . ?
C12 C13 H13B 109.1 . . ?
H13A C13 H13B 107.8 . . ?
C15 C14 C13 115.0(3) . . ?
C15 C14 H14A 108.5 . . ?
C13 C14 H14A 108.5 . . ?
C15 C14 H14B 108.5 . . ?
C13 C14 H14B 108.5 . . ?
H14A C14 H14B 107.5 . . ?
O31 C15 O32 125.7(4) . . ?
O31 C15 C14 118.2(3) . . ?
O32 C15 C14 116.1(3) . . ?
O23 C16 O22 125.9(4) . . ?
O23 C16 C17 117.0(4) . . ?
O22 C16 C17 117.0(4) . . ?
C16 C17 C18 109.2(3) . . ?
C16 C17 H17A 109.8 . . ?
C18 C17 H17A 109.8 . . ?
C16 C17 H17B 109.8 . . ?
C18 C17 H17B 109.8 . . ?
H17A C17 H17B 108.3 . . ?
C19 C18 C17 113.1(3) . . ?
C19 C18 H18A 109.0 . . ?
C17 C18 H18A 109.0 . . ?
C19 C18 H18B 109.0 . . ?
C17 C18 H18B 109.0 . . ?
H18A C18 H18B 107.8 . . ?
C20 C19 C18 114.1(3) . . ?
C20 C19 H19A 108.7 . . ?
C18 C19 H19A 108.7 . . ?
C20 C19 H19B 108.7 . . ?
C18 C19 H19B 108.7 . . ?
H19A C19 H19B 107.6 . . ?
O29 C20 O30 125.3(3) . . ?
O29 C20 C19 116.8(3) . . ?
O30 C20 C19 117.9(3) . . ?
C21 N1 C33 110.7(4) . . ?
C21 N1 C29 109.1(4) . . ?
C33 N1 C29 110.1(4) . . ?
C21 N1 C25 110.8(4) . . ?
C33 N1 C25 108.8(4) . . ?
C29 N1 C25 107.4(4) . . ?
N1 C21 C22 116.9(4) . . ?
N1 C21 H21A 108.1 . . ?
C22 C21 H21A 108.1 . . ?
N1 C21 H21B 108.1 . . ?
C22 C21 H21B 108.1 . . ?
H21A C21 H21B 107.3 . . ?
C23 C22 C21 112.8(5) . . ?
C23 C22 H22A 109.0 . . ?
C21 C22 H22A 109.0 . . ?
C23 C22 H22B 109.0 . . ?
C21 C22 H22B 109.0 . . ?
H22A C22 H22B 107.8 . . ?
C24 C23 C22 117.4(6) . . ?
C24 C23 H23A 108.0 . . ?
C22 C23 H23A 108.0 . . ?
C24 C23 H23B 108.0 . . ?
C22 C23 H23B 108.0 . . ?
H23A C23 H23B 107.2 . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C26 C25 N1 121.3(4) . . ?
C26 C25 H25A 107.0 . . ?
N1 C25 H25A 107.0 . . ?
C26 C25 H25B 107.0 . . ?
N1 C25 H25B 107.0 . . ?
H25A C25 H25B 106.7 . . ?
C25 C26 C27 109.3(4) . . ?
C25 C26 H26A 109.8 . . ?
C27 C26 H26A 109.8 . . ?
C25 C26 H26B 109.8 . . ?
C27 C26 H26B 109.8 . . ?
H26A C26 H26B 108.3 . . ?
C28 C27 C26 115.6(4) . . ?
C28 C27 H27A 108.4 . . ?
C26 C27 H27A 108.4 . . ?
C28 C27 H27B 108.4 . . ?
C26 C27 H27B 108.4 . . ?
H27A C27 H27B 107.4 . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C30 C29 N1 117.0(4) . . ?
C30 C29 H29A 108.1 . . ?
N1 C29 H29A 108.1 . . ?
C30 C29 H29B 108.1 . . ?
N1 C29 H29B 108.1 . . ?
H29A C29 H29B 107.3 . . ?
C29 C30 C31 111.6(5) . . ?
C29 C30 H30A 109.3 . . ?
C31 C30 H30A 109.3 . . ?
C29 C30 H30B 109.3 . . ?
C31 C30 H30B 109.3 . . ?
H30A C30 H30B 108.0 . . ?
C32 C31 C30 118.8(6) . . ?
C32 C31 H31A 107.6 . . ?
C30 C31 H31A 107.6 . . ?
C32 C31 H31B 107.6 . . ?
C30 C31 H31B 107.6 . . ?
H31A C31 H31B 107.0 . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
N1 C33 C34 117.2(4) . . ?
N1 C33 H33A 108.0 . . ?
C34 C33 H33A 108.0 . . ?
N1 C33 H33B 108.0 . . ?
C34 C33 H33B 108.0 . . ?
H33A C33 H33B 107.2 . . ?
C35 C34 C33 110.4(4) . . ?
C35 C34 H34A 109.6 . . ?
C33 C34 H34A 109.6 . . ?
C35 C34 H34B 109.6 . . ?
C33 C34 H34B 109.6 . . ?
H34A C34 H34B 108.1 . . ?
C34 C35 C36 112.1(5) . . ?
C34 C35 H35A 109.2 . . ?
C36 C35 H35A 109.2 . . ?
C34 C35 H35B 109.2 . . ?
C36 C35 H35B 109.2 . . ?
H35A C35 H35B 107.9 . . ?
C35 C36 H36A 109.5 . . ?
C35 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C35 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C37A N2A C49A 110.6(6) . . ?
C37A N2A C41A 110.6(5) . . ?
C49A N2A C41A 113.3(6) . . ?
C37A N2A C45A 109.8(6) . . ?
C49A N2A C45A 106.2(6) . . ?
C41A N2A C45A 106.1(5) . . ?
N2A C37A C38A 117.7(7) . . ?
N2A C37A H37A 107.9 . . ?
C38A C37A H37A 107.9 . . ?
N2A C37A H37B 107.9 . . ?
C38A C37A H37B 107.9 . . ?
H37A C37A H37B 107.2 . . ?
C39A C38A C37A 112.0(7) . . ?
C39A C38A H38A 109.2 . . ?
C37A C38A H38A 109.2 . . ?
C39A C38A H38B 109.2 . . ?
C37A C38A H38B 109.2 . . ?
H38A C38A H38B 107.9 . . ?
C38A C39A C40A 117.1(11) . . ?
C38A C39A H39A 108.0 . . ?
C40A C39A H39A 108.0 . . ?
C38A C39A H39B 108.0 . . ?
C40A C39A H39B 108.0 . . ?
H39A C39A H39B 107.3 . . ?
C39A C40A H40A 109.5 . . ?
C39A C40A H40B 109.5 . . ?
H40A C40A H40B 109.5 . . ?
C39A C40A H40C 109.5 . . ?
H40A C40A H40C 109.5 . . ?
H40B C40A H40C 109.5 . . ?
C42A C41A N2A 116.3(6) . . ?
C42A C41A H41A 108.2 . . ?
N2A C41A H41A 108.2 . . ?
C42A C41A H41B 108.2 . . ?
N2A C41A H41B 108.2 . . ?
H41A C41A H41B 107.4 . . ?
C41A C42A C43A 110.4(8) . . ?
C41A C42A H42A 109.6 . . ?
C43A C42A H42A 109.6 . . ?
C41A C42A H42B 109.6 . . ?
C43A C42A H42B 109.6 . . ?
H42A C42A H42B 108.1 . . ?
C44A C43A C42A 115.5(10) . . ?
C44A C43A H43A 108.4 . . ?
C42A C43A H43A 108.4 . . ?
C44A C43A H43B 108.4 . . ?
C42A C43A H43B 108.4 . . ?
H43A C43A H43B 107.5 . . ?
C43A C44A H44A 109.5 . . ?
C43A C44A H44B 109.5 . . ?
H44A C44A H44B 109.5 . . ?
C43A C44A H44C 109.5 . . ?
H44A C44A H44C 109.5 . . ?
H44B C44A H44C 109.5 . . ?
C46A C45A N2A 118.3(7) . . ?
C46A C45A H45A 107.7 . . ?
N2A C45A H45A 107.7 . . ?
C46A C45A H45B 107.7 . . ?
N2A C45A H45B 107.7 . . ?
H45A C45A H45B 107.1 . . ?
C47A C46A C45A 111.1(9) . . ?
C47A C46A H46A 109.4 . . ?
C45A C46A H46A 109.4 . . ?
C47A C46A H46B 109.4 . . ?
C45A C46A H46B 109.4 . . ?
H46A C46A H46B 108.0 . . ?
C48A C47A C46A 113.9(12) . . ?
C48A C47A H47A 108.8 . . ?
C46A C47A H47A 108.8 . . ?
C48A C47A H47B 108.8 . . ?
C46A C47A H47B 108.8 . . ?
H47A C47A H47B 107.7 . . ?
C47A C48A H48A 109.5 . . ?
C47A C48A H48B 109.5 . . ?
H48A C48A H48B 109.5 . . ?
C47A C48A H48C 109.5 . . ?
H48A C48A H48C 109.5 . . ?
H48B C48A H48C 109.5 . . ?
C50A C49A N2A 116.6(7) . . ?
C50A C49A H49A 108.1 . . ?
N2A C49A H49A 108.1 . . ?
C50A C49A H49B 108.1 . . ?
N2A C49A H49B 108.1 . . ?
H49A C49A H49B 107.3 . . ?
C51A C50A C49A 117.1(11) . . ?
C51A C50A H50A 108.0 . . ?
C49A C50A H50A 108.0 . . ?
C51A C50A H50B 108.0 . . ?
C49A C50A H50B 108.0 . . ?
H50A C50A H50B 107.3 . . ?
C52A C51A C50A 109.5(13) . . ?
C52A C51A H51A 109.8 . . ?
C50A C51A H51A 109.8 . . ?
C52A C51A H51B 109.8 . . ?
C50A C51A H51B 109.8 . . ?
H51A C51A H51B 108.2 . . ?
C51A C52A H52A 109.5 . . ?
C51A C52A H52B 109.5 . . ?
H52A C52A H52B 109.5 . . ?
C51A C52A H52C 109.5 . . ?
H52A C52A H52C 109.5 . . ?
H52B C52A H52C 109.5 . . ?
C45B N2B C49B 110.6(6) . . ?
C45B N2B C37B 113.2(6) . . ?
C49B N2B C37B 108.0(5) . . ?
C45B N2B C41B 108.1(6) . . ?
C49B N2B C41B 110.0(6) . . ?
C37B N2B C41B 106.8(6) . . ?
C38B C37B N2B 119.4(7) . . ?
C38B C37B H37C 107.5 . . ?
N2B C37B H37C 107.5 . . ?
C38B C37B H37D 107.5 . . ?
N2B C37B H37D 107.5 . . ?
H37C C37B H37D 107.0 . . ?
C39B C38B C37B 116.1(10) . . ?
C39B C38B H38C 108.3 . . ?
C37B C38B H38C 108.3 . . ?
C39B C38B H38D 108.3 . . ?
C37B C38B H38D 108.3 . . ?
H38C C38B H38D 107.4 . . ?
C40B C39B C38B 115.7(13) . . ?
C40B C39B H39C 108.4 . . ?
C38B C39B H39C 108.4 . . ?
C40B C39B H39D 108.4 . . ?
C38B C39B H39D 108.4 . . ?
H39C C39B H39D 107.4 . . ?
C39B C40B H40D 109.5 . . ?
C39B C40B H40E 109.5 . . ?
H40D C40B H40E 109.5 . . ?
C39B C40B H40F 109.5 . . ?
H40D C40B H40F 109.5 . . ?
H40E C40B H40F 109.5 . . ?
C42B C41B N2B 117.7(7) . . ?
C42B C41B H41C 107.9 . . ?
N2B C41B H41C 107.9 . . ?
C42B C41B H41D 107.9 . . ?
N2B C41B H41D 107.9 . . ?
H41C C41B H41D 107.2 . . ?
C43B C42B C41B 116.2(10) . . ?
C43B C42B H42C 108.2 . . ?
C41B C42B H42C 108.2 . . ?
C43B C42B H42D 108.2 . . ?
C41B C42B H42D 108.2 . . ?
H42C C42B H42D 107.4 . . ?
C44B C43B C42B 112.3(11) . . ?
C44B C43B H43C 109.2 . . ?
C42B C43B H43C 109.2 . . ?
C44B C43B H43D 109.2 . . ?
C42B C43B H43D 109.2 . . ?
H43C C43B H43D 107.9 . . ?
C43B C44B H44D 109.5 . . ?
C43B C44B H44E 109.5 . . ?
H44D C44B H44E 109.5 . . ?
C43B C44B H44F 109.5 . . ?
H44D C44B H44F 109.5 . . ?
H44E C44B H44F 109.5 . . ?
N2B C45B C46B 118.0(8) . . ?
N2B C45B H45C 107.8 . . ?
C46B C45B H45C 107.8 . . ?
N2B C45B H45D 107.8 . . ?
C46B C45B H45D 107.8 . . ?
H45C C45B H45D 107.1 . . ?
C45B C46B C47B 110.8(9) . . ?
C45B C46B H46C 109.5 . . ?
C47B C46B H46C 109.5 . . ?
C45B C46B H46D 109.5 . . ?
C47B C46B H46D 109.5 . . ?
H46C C46B H46D 108.1 . . ?
C48B C47B C46B 108.3(11) . . ?
C48B C47B H47C 110.0 . . ?
C46B C47B H47C 110.0 . . ?
C48B C47B H47D 110.0 . . ?
C46B C47B H47D 110.0 . . ?
H47C C47B H47D 108.4 . . ?
C47B C48B H48D 109.5 . . ?
C47B C48B H48E 109.5 . . ?
H48D C48B H48E 109.5 . . ?
C47B C48B H48F 109.5 . . ?
H48D C48B H48F 109.5 . . ?
H48E C48B H48F 109.5 . . ?
C50B C49B N2B 120.8(7) . . ?
C50B C49B H49C 107.1 . . ?
N2B C49B H49C 107.1 . . ?
C50B C49B H49D 107.1 . . ?
N2B C49B H49D 107.1 . . ?
H49C C49B H49D 106.8 . . ?
C51B C50B C49B 107.9(8) . . ?
C51B C50B H50C 110.1 . . ?
C49B C50B H50C 110.1 . . ?
C51B C50B H50D 110.1 . . ?
C49B C50B H50D 110.1 . . ?
H50C C50B H50D 108.4 . . ?
C52B C51B C50B 111.6(10) . . ?
C52B C51B H51C 109.3 . . ?
C50B C51B H51C 109.3 . . ?
C52B C51B H51D 109.3 . . ?
C50B C51B H51D 109.3 . . ?
H51C C51B H51D 108.0 . . ?
C51B C52B H52D 109.5 . . ?
C51B C52B H52E 109.5 . . ?
H52D C52B H52E 109.5 . . ?
C51B C52B H52F 109.5 . . ?
H52D C52B H52F 109.5 . . ?
H52E C52B H52F 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
O1 V1 O2 V2 160.02(19) . . . . ?
O4 V1 O2 V2 -95.83(19) . . . . ?
O7 V1 O2 V2 61.19(19) . . . . ?
O5 V1 O2 V2 0.6(5) . . . . ?
O3 V2 O2 V1 -160.6(2) . . . . ?
O12 V2 O2 V1 95.0(2) 2_565 . . . ?
O16 V2 O2 V1 -11.7(4) 2_565 . . . ?
O8 V2 O2 V1 -61.36(19) . . . . ?
O1 V1 O4 V3 -157.27(19) . . . 2_565 ?
O2 V1 O4 V3 98.42(19) . . . 2_565 ?
O7 V1 O4 V3 -3.5(4) . . . 2_565 ?
O5 V1 O4 V3 -59.68(19) . . . 2_565 ?
O11 V4 O10 V3 -159.35(18) . . . . ?
O12 V4 O10 V3 97.40(18) . . . . ?
O14 V4 O10 V3 -61.22(18) . . . . ?
O15 V4 O10 V3 1.4(4) . . . . ?
Cl1 V4 O10 V3 18.57(16) . . . . ?
O9 V3 O10 V4 160.31(18) . . . . ?
O4 V3 O10 V4 -94.98(19) 2_565 . . . ?
O6 V3 O10 V4 8.8(4) 2_565 . . . ?
O13 V3 O10 V4 63.28(18) . . . . ?
O11 V4 O12 V2 157.01(19) . . . 2_565 ?
O10 V4 O12 V2 -98.92(19) . . . 2_565 ?
O14 V4 O12 V2 3.1(4) . . . 2_565 ?
O15 V4 O12 V2 60.66(19) . . . 2_565 ?
Cl1 V4 O12 V2 -18.66(16) . . . 2_565 ?
V1 O5 C1 O6 -7.2(6) . . . . ?
V1 O5 C1 C2 171.6(3) . . . . ?
V3 O6 C1 O5 5.3(6) 2_565 . . . ?
V3 O6 C1 C2 -173.4(3) 2_565 . . . ?
O5 C1 C2 C3 18.6(5) . . . . ?
O6 C1 C2 C3 -162.6(3) . . . . ?
C1 C2 C3 C4 -173.2(3) . . . . ?
C2 C3 C4 C5 71.2(4) . . . . ?
V4 O15 C5 O16 -1.3(6) . . . . ?
V4 O15 C5 C4 -177.9(2) . . . . ?
V2 O16 C5 O15 -1.3(6) 2_565 . . . ?
V2 O16 C5 C4 175.3(2) 2_565 . . . ?
C3 C4 C5 O15 85.2(4) . . . . ?
C3 C4 C5 O16 -91.7(4) . . . . ?
V1 O7 C6 O8 5.7(5) . . . . ?
V1 O7 C6 C7 -171.8(2) . . . . ?
V2 O8 C6 O7 -7.6(5) . . . . ?
V2 O8 C6 C7 169.9(2) . . . . ?
O7 C6 C7 C8 -23.1(5) . . . . ?
O8 C6 C7 C8 159.2(3) . . . . ?
C6 C7 C8 C9 175.4(3) . . . . ?
C7 C8 C9 C10 -68.4(4) . . . . ?
V3 O13 C10 O14 4.2(6) . . . . ?
V3 O13 C10 C9 -172.8(2) . . . . ?
V4 O14 C10 O13 1.9(6) . . . . ?
V4 O14 C10 C9 178.9(2) . . . . ?
C8 C9 C10 O13 92.9(4) . . . . ?
C8 C9 C10 O14 -84.3(4) . . . . ?
O17 V5 O18 V6 -158.63(18) . . . 2_666 ?
O19 V5 O18 V6 97.24(18) . . . 2_666 ?
O22 V5 O18 V6 -7.9(4) . . . 2_666 ?
O20 V5 O18 V6 -61.83(18) . . . 2_666 ?
O17 V5 O19 V8 159.53(18) . . . 2_666 ?
O18 V5 O19 V8 -97.50(18) . . . 2_666 ?
O22 V5 O19 V8 61.46(18) . . . 2_666 ?
O20 V5 O19 V8 2.6(4) . . . 2_666 ?
O26 V7 O25 V6 -159.64(19) . . . . ?
O27 V7 O25 V6 96.04(19) . . . . ?
O30 V7 O25 V6 -60.35(19) . . . . ?
O31 V7 O25 V6 -2.6(4) . . . . ?
O24 V6 O25 V7 157.7(2) . . . . ?
O18 V6 O25 V7 -97.1(2) 2_666 . . . ?
O21 V6 O25 V7 4.6(4) 2_666 . . . ?
O29 V6 O25 V7 59.08(19) . . . . ?
O28 V8 O27 V7 -159.71(19) . . . . ?
O19 V8 O27 V7 95.67(19) 2_666 . . . ?
O32 V8 O27 V7 -59.98(19) . . . . ?
O23 V8 O27 V7 -0.9(5) 2_666 . . . ?
O26 V7 O27 V8 159.53(19) . . . . ?
O25 V7 O27 V8 -96.15(19) . . . . ?
O30 V7 O27 V8 7.7(4) . . . . ?
O31 V7 O27 V8 61.67(19) . . . . ?
V6 O21 C11 O20 1.4(5) 2_666 . . . ?
V6 O21 C11 C12 -176.4(2) 2_666 . . . ?
V5 O20 C11 O21 -1.0(5) . . . . ?
V5 O20 C11 C12 176.7(2) . . . . ?
O21 C11 C12 C13 90.3(4) . . . . ?
O20 C11 C12 C13 -87.7(4) . . . . ?
C11 C12 C13 C14 -69.4(4) . . . . ?
C12 C13 C14 C15 172.9(3) . . . . ?
V7 O31 C15 O32 7.1(6) . . . . ?
V7 O31 C15 C14 -170.8(2) . . . . ?
V8 O32 C15 O31 -2.3(6) . . . . ?
V8 O32 C15 C14 175.7(2) . . . . ?
C13 C14 C15 O31 -16.7(5) . . . . ?
C13 C14 C15 O32 165.2(3) . . . . ?
V8 O23 C16 O22 -3.1(6) 2_666 . . . ?
V8 O23 C16 C17 174.2(2) 2_666 . . . ?
V5 O22 C16 O23 -0.4(6) . . . . ?
V5 O22 C16 C17 -177.7(2) . . . . ?
O23 C16 C17 C18 -90.3(4) . . . . ?
O22 C16 C17 C18 87.3(4) . . . . ?
C16 C17 C18 C19 66.0(4) . . . . ?
C17 C18 C19 C20 -175.9(3) . . . . ?
V6 O29 C20 O30 6.3(5) . . . . ?
V6 O29 C20 C19 -171.0(2) . . . . ?
V7 O30 C20 O29 -8.0(5) . . . . ?
V7 O30 C20 C19 169.3(2) . . . . ?
C18 C19 C20 O29 -159.4(3) . . . . ?
C18 C19 C20 O30 23.2(5) . . . . ?
C33 N1 C21 C22 -55.9(7) . . . . ?
C29 N1 C21 C22 -177.2(5) . . . . ?
C25 N1 C21 C22 64.8(6) . . . . ?
N1 C21 C22 C23 -176.8(6) . . . . ?
C21 C22 C23 C24 -172.9(7) . . . . ?
C21 N1 C25 C26 40.8(6) . . . . ?
C33 N1 C25 C26 162.7(4) . . . . ?
C29 N1 C25 C26 -78.2(6) . . . . ?
N1 C25 C26 C27 170.6(4) . . . . ?
C25 C26 C27 C28 172.9(4) . . . . ?
C21 N1 C29 C30 64.8(6) . . . . ?
C33 N1 C29 C30 -56.9(6) . . . . ?
C25 N1 C29 C30 -175.1(5) . . . . ?
N1 C29 C30 C31 172.5(5) . . . . ?
C29 C30 C31 C32 -171.4(8) . . . . ?
C21 N1 C33 C34 -171.8(5) . . . . ?
C29 N1 C33 C34 -51.1(6) . . . . ?
C25 N1 C33 C34 66.3(6) . . . . ?
N1 C33 C34 C35 -168.8(5) . . . . ?
C33 C34 C35 C36 -177.5(5) . . . . ?
C49A N2A C37A C38A 58.5(10) . . . . ?
C41A N2A C37A C38A -175.2(8) . . . . ?
C45A N2A C37A C38A -58.4(10) . . . . ?
N2A C37A C38A C39A 174.6(11) . . . . ?
C37A C38A C39A C40A 170.6(12) . . . . ?
C37A N2A C41A C42A -69.3(10) . . . . ?
C49A N2A C41A C42A 55.5(10) . . . . ?
C45A N2A C41A C42A 171.6(8) . . . . ?
N2A C41A C42A C43A 173.0(9) . . . . ?
C41A C42A C43A C44A 175.8(11) . . . . ?
C37A N2A C45A C46A -55.3(12) . . . . ?
C49A N2A C45A C46A -175.0(10) . . . . ?
C41A N2A C45A C46A 64.2(12) . . . . ?
N2A C45A C46A C47A -167.7(11) . . . . ?
C45A C46A C47A C48A 179.4(14) . . . . ?
C37A N2A C49A C50A -177.3(9) . . . . ?
C41A N2A C49A C50A 57.9(11) . . . . ?
C45A N2A C49A C50A -58.2(11) . . . . ?
N2A C49A C50A C51A 177.5(11) . . . . ?
C49A C50A C51A C52A 63(2) . . . . ?
C45B N2B C37B C38B 59.9(11) . . . . ?
C49B N2B C37B C38B -177.2(9) . . . . ?
C41B N2B C37B C38B -59.0(11) . . . . ?
N2B C37B C38B C39B -169.5(10) . . . . ?
C37B C38B C39B C40B 70.0(19) . . . . ?
C45B N2B C41B C42B 67.4(11) . . . . ?
C49B N2B C41B C42B -53.4(11) . . . . ?
C37B N2B C41B C42B -170.4(9) . . . . ?
N2B C41B C42B C43B -175.5(9) . . . . ?
C41B C42B C43B C44B 97.3(15) . . . . ?
C49B N2B C45B C46B -65.7(12) . . . . ?
C37B N2B C45B C46B 55.7(12) . . . . ?
C41B N2B C45B C46B 173.8(10) . . . . ?
N2B C45B C46B C47B 164.4(11) . . . . ?
C45B C46B C47B C48B -178.7(12) . . . . ?
C45B N2B C49B C50B -167.2(9) . . . . ?
C37B N2B C49B C50B 68.4(11) . . . . ?
C41B N2B C49B C50B -47.8(11) . . . . ?
N2B C49B C50B C51B -178.3(11) . . . . ?
C49B C50B C51B C52B -172.5(12) . . . . ?

_refine_diff_density_max         0.944
_refine_diff_density_min         -0.579
_refine_diff_density_rms         0.096



#==============================================================================0
# start Validation Reply Form


_vrf_PLAT413_2                   
;
PROBLEM:
Alert level B
PLAT413_ALERT_2_B Short Inter XH3 .. XHn     H24A   ..  H52A    ..       1.99 Ang.  
RESPONSE:
intermolecular contact of a hydrogen belonging to a disordered (non-real) part 
of a butyl group of a tetrabutylammonium cation with the hydrogen belonging to 
another tetrabutylammonium in a symmetry equivalent position. 

;

_vrf_PLAT112_2                   
;
PROBLEM:
Alert level C
PLAT112_ALERT_2_C ADDSYM Detects New (Pseudo) Symm. Elem.        B         81 %Fit  

RESPONSE: 
Close examination of the possible higher (pseudo) symmetry in the structural 
model in combination with the reflction data using PLATON/ADDSYM disprove this 
issue 

;

_vrf_PLAT230_2                   
;
PROBLEM:
Alert level C
PLAT230_ALERT_2_C Hirshfeld Test Diff for    O15    --  C5      ..        5.5 s.u. 
RESPONSE:

C-level alerts for this structure are a technical issue due either to disorder 
modeling or uncorrected absorption effects. As discussed in detail in the 
article, the complicated asymmetric unit of compound 2 contains two independent 
half polyoxovanadates (POV) molecular cages (which are generated to their 
completeness by symmetry through an inversion center) each containing a chloride 
anion and two tetrabutylammonium cations. One of tetrabutylammonium cations is 
disordered while the second appears to be unaffected. This disordered 
tetrabutylammonium cation was modeled at two sites and refined both with equal 
fixed occupancy. This required a number of least-squares constraints/restraints. 
However, the alert affect to a POV cage which does not appear clearly 
disordered. As shown in the refinement instruction details, no Uij restraints 
were applied to this non-disordered POV cage. The authors believe that the best 
disorder model has been applied to the tetrabutylammonium cation refinement 
which results in acceptable geometries for both components of disorder. 
Other causes for these alerts could be related to the presence of one type 
of heavy V atoms attached to lighter O atom with weaker scattering and 
absorption.In view of the complexity of the partial disorder problem, the 
refinement results were judged satisfactory.


;


_vrf_PLAT341_2                   
;
PROBLEM:
Alert level C
PLAT341_ALERT_3_C Low Bond Precision on  C-C Bonds ...............   0.00743 Ang.
RESPONSE: 
The crystal was not of very good quality despite being the best selected from
the sample supplied. The crystal structure has one tetrabutylammonium cation 
disordered and in general shows distinct thermal displacements of some outer 
atoms. So that some shelxl restraints(DELU, SIMU, ..) were used to make 
the structure more plausible.

;


_vrf_PLAT360_2                   
;
PROBLEM:
Alert level C
PLAT360_ALERT_2_C Short  C(sp3)-C(sp3) Bond   C31    -   C32    ..       1.37 Ang. 
RESPONSE: We offer the same explanation as for the previous alerts PLAT230 
and PLAT341 
;
