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

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

data_1
_database_code_depnum_ccdc_archive 'CCDC 1558507'
_audit_update_record             
;
2017-06-26 deposited with the CCDC.
2017-09-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C16 H22 O21 V6 2(C16 H36 N)'
_chemical_formula_sum            'C48 H94 N2 O21 V6'
_chemical_formula_weight         1340.89

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

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

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

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

_cell_length_a                   17.244(2)
_cell_length_b                   22.208(3)
_cell_length_c                   15.317(2)
_cell_angle_alpha                90
_cell_angle_beta                 94.834(3)
_cell_angle_gamma                90
_cell_volume                     5844.9(13)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    1445
_cell_measurement_theta_min      2.37
_cell_measurement_theta_max      19.53

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.524
_exptl_crystal_F_000             2808
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.21
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_coefficient_mu    0.995
_exptl_absorpt_correction_T_max  0.7450
_exptl_absorpt_correction_T_min  0.6081
_exptl_absorpt_process_details   
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.1703 before and 0.0780 after correction.
The Ratio of minimum to maximum transmission is 0.8162.
The λ/2 correction factor is 0.0015.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_measurement_device_type  'Bruker SMART APEX2 area detector'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            29328
_diffrn_reflns_av_unetI/netI     0.1097
_diffrn_reflns_av_R_equivalents  0.0888
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         1.185
_diffrn_reflns_theta_max         24.163
_diffrn_reflns_theta_full        24.163
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             9334
_reflns_number_gt                6652
_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_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2014)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+0.0396P] 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         9334
_refine_ls_number_parameters     705
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0804
_refine_ls_R_factor_gt           0.0510
_refine_ls_wR_factor_ref         0.1276
_refine_ls_wR_factor_gt          0.1151
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_restrained_S_all      1.049
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
V1 V 0.50217(4) 0.53476(3) 0.13774(5) 0.01499(19) Uani 1 1 d . . . . .
V2 V 0.38219(4) 0.54070(3) -0.01806(5) 0.01414(19) Uani 1 1 d . . . . .
V3 V 0.56407(4) 0.58593(3) -0.02760(5) 0.01561(19) Uani 1 1 d . . . . .
V4 V 0.11030(4) 0.55295(3) 0.50791(5) 0.01286(19) Uani 1 1 d . . . . .
V5 V 0.07176(4) 0.42568(3) 0.44708(5) 0.01378(19) Uani 1 1 d . . . . .
V6 V -0.02673(4) 0.54547(3) 0.37067(5) 0.01346(19) Uani 1 1 d . . . . .
O1 O 0.5000 0.5000 0.0000 0.0118(9) Uani 1 2 d S . P . .
O2 O 0.41125(16) 0.56524(11) 0.09968(18) 0.0158(7) Uani 1 1 d . . . . .
O3 O 0.35191(16) 0.46906(11) 0.01408(18) 0.0143(7) Uani 1 1 d . . . . .
O4 O 0.30335(16) 0.57783(12) -0.04079(19) 0.0182(7) Uani 1 1 d . . . . .
O5 O 0.55896(16) 0.59601(11) 0.08623(18) 0.0169(7) Uani 1 1 d . . . . .
O6 O 0.60388(16) 0.64628(12) -0.06050(19) 0.0190(7) Uani 1 1 d . . . . .
O7 O 0.45627(16) 0.45292(11) 0.14937(18) 0.0142(7) Uani 1 1 d . . . . .
O8 O 0.60352(16) 0.48610(11) 0.13771(17) 0.0128(6) Uani 1 1 d . . . . .
O9 O 0.54618(15) 0.38918(11) 0.05062(17) 0.0125(6) Uani 1 1 d . . . . .
O10 O 0.66823(16) 0.33119(12) 0.28499(19) 0.0183(7) Uani 1 1 d . . . . .
O11 O 0.51331(17) 0.55056(11) 0.24085(19) 0.0199(7) Uani 1 1 d . . . . .
O12 O 0.0000 0.5000 0.5000 0.0106(9) Uani 1 2 d S . P . .
O13 O 0.14670(16) 0.48800(11) 0.45862(18) 0.0167(7) Uani 1 1 d . . . . .
O14 O 0.08560(16) 0.40574(11) 0.55875(18) 0.0150(7) Uani 1 1 d . . . . .
O15 O 0.11648(16) 0.37465(11) 0.39764(19) 0.0185(7) Uani 1 1 d . . . . .
O16 O 0.06103(16) 0.58300(11) 0.40158(18) 0.0142(7) Uani 1 1 d . . . . .
O17 O -0.05266(16) 0.56857(12) 0.27301(18) 0.0181(7) Uani 1 1 d . . . . .
O18 O 0.03358(15) 0.60944(11) 0.56509(18) 0.0122(6) Uani 1 1 d . . . . .
O19 O 0.11726(15) 0.51417(11) 0.62458(17) 0.0124(6) Uani 1 1 d . . . . .
O20 O -0.03060(16) 0.52764(11) 0.66399(18) 0.0139(7) Uani 1 1 d . . . . .
O21 O 0.16876(16) 0.66300(12) 0.79212(19) 0.0201(7) Uani 1 1 d . . . . .
O22 O 0.18415(16) 0.59681(12) 0.52368(18) 0.0174(7) Uani 1 1 d . . . . .
C1 C 0.4852(2) 0.41557(17) 0.2211(3) 0.0162(10) Uani 1 1 d . . . . .
H1A H 0.4507 0.3813 0.2251 0.019 Uiso 1 1 calc R U . . .
H1B H 0.4848 0.4383 0.2752 0.019 Uiso 1 1 calc R U . . .
C2 C 0.5679(2) 0.39284(17) 0.2114(3) 0.0125(9) Uani 1 1 d . . . . .
C3 C 0.6241(2) 0.44613(17) 0.2092(3) 0.0154(10) Uani 1 1 d . . . . .
H3A H 0.6243 0.4683 0.2638 0.018 Uiso 1 1 calc R U . . .
H3B H 0.6763 0.4310 0.2043 0.018 Uiso 1 1 calc R U . . .
C4 C 0.5691(3) 0.35502(17) 0.1280(3) 0.0167(10) Uani 1 1 d . . . . .
H4A H 0.6212 0.3394 0.1240 0.020 Uiso 1 1 calc R U . . .
H4B H 0.5342 0.3210 0.1315 0.020 Uiso 1 1 calc R U . . .
C5 C 0.5919(2) 0.35400(18) 0.2916(3) 0.0169(10) Uani 1 1 d . . . . .
H5A H 0.5908 0.3779 0.3445 0.020 Uiso 1 1 calc R U . . .
H5B H 0.5556 0.3209 0.2950 0.020 Uiso 1 1 calc R U . . .
C6 C 0.7041(3) 0.30889(18) 0.3662(3) 0.0216(11) Uani 1 1 d . . . . .
H6A H 0.7054 0.3409 0.4093 0.026 Uiso 1 1 calc R U . . .
H6B H 0.7574 0.2978 0.3581 0.026 Uiso 1 1 calc R U . . .
C7 C 0.6642(3) 0.25654(19) 0.4004(3) 0.0189(10) Uani 1 1 d . . . . .
C8 C 0.6330(3) 0.2141(2) 0.4279(3) 0.0240(11) Uani 1 1 d . . . . .
H8 H 0.6085 0.1806 0.4496 0.029 Uiso 1 1 calc R U . . .
C9 C 0.0603(3) 0.63895(17) 0.6449(3) 0.0144(10) Uani 1 1 d . . . . .
H9A H 0.0216 0.6681 0.6597 0.017 Uiso 1 1 calc R U . . .
H9B H 0.1079 0.6606 0.6363 0.017 Uiso 1 1 calc R U . . .
C10 C 0.0757(3) 0.59455(17) 0.7217(3) 0.0158(10) Uani 1 1 d . . . . .
C11 C 0.1392(2) 0.54966(17) 0.7005(3) 0.0154(10) Uani 1 1 d . . . . .
H11A H 0.1864 0.5716 0.6912 0.019 Uiso 1 1 calc R U . . .
H11B H 0.1504 0.5231 0.7502 0.019 Uiso 1 1 calc R U . . .
C12 C 0.0005(2) 0.56135(18) 0.7382(3) 0.0161(10) Uani 1 1 d . . . . .
H12A H 0.0107 0.5343 0.7875 0.019 Uiso 1 1 calc R U . . .
H12B H -0.0380 0.5905 0.7538 0.019 Uiso 1 1 calc R U . . .
C13 C 0.1018(3) 0.62902(18) 0.8047(3) 0.0185(10) Uani 1 1 d . . . . .
H13A H 0.0604 0.6556 0.8200 0.022 Uiso 1 1 calc R U . . .
H13B H 0.1130 0.6010 0.8527 0.022 Uiso 1 1 calc R U . . .
C14 C 0.2014(3) 0.69036(19) 0.8710(3) 0.0228(11) Uani 1 1 d . . . . .
H14A H 0.2524 0.7062 0.8614 0.027 Uiso 1 1 calc R U . . .
H14B H 0.2082 0.6599 0.9163 0.027 Uiso 1 1 calc R U . . .
C15 C 0.1534(3) 0.73910(18) 0.9016(3) 0.0204(11) Uani 1 1 d . . . . .
C16 C 0.1152(3) 0.7791(2) 0.9253(3) 0.0287(12) Uani 1 1 d . . . . .
H16 H 0.0851 0.8106 0.9439 0.034 Uiso 1 1 calc R U . . .
N1 N 0.3005(2) 0.14975(14) 0.1051(2) 0.0158(8) Uani 1 1 d . . . . .
C17 C 0.2894(2) 0.09054(17) 0.0558(3) 0.0181(10) Uani 1 1 d . . . . .
H17A H 0.2503 0.0671 0.0825 0.022 Uiso 1 1 calc R U . . .
H17B H 0.2695 0.0992 -0.0040 0.022 Uiso 1 1 calc R U . . .
C18 C 0.3623(2) 0.05232(17) 0.0534(3) 0.0171(10) Uani 1 1 d . . . . .
H18A H 0.3907 0.0523 0.1107 0.021 Uiso 1 1 calc R U . . .
H18B H 0.3956 0.0694 0.0119 0.021 Uiso 1 1 calc R U . . .
C19 C 0.3410(3) -0.01239(18) 0.0266(3) 0.0223(11) Uani 1 1 d . . . . .
H19A H 0.3177 -0.0322 0.0744 0.027 Uiso 1 1 calc R U . . .
H19B H 0.3028 -0.0117 -0.0235 0.027 Uiso 1 1 calc R U . . .
C20 C 0.4117(3) -0.04843(19) 0.0035(3) 0.0247(11) Uani 1 1 d . . . . .
H20A H 0.4310 -0.0321 -0.0486 0.037 Uiso 1 1 calc R U . . .
H20B H 0.3971 -0.0897 -0.0065 0.037 Uiso 1 1 calc R U . . .
H20C H 0.4517 -0.0462 0.0510 0.037 Uiso 1 1 calc R U . . .
C21 C 0.2264(2) 0.18643(18) 0.0839(3) 0.0183(10) Uani 1 1 d . . . . .
H21A H 0.2174 0.1899 0.0207 0.022 Uiso 1 1 calc R U . . .
H21B H 0.1830 0.1642 0.1043 0.022 Uiso 1 1 calc R U . . .
C22 C 0.2263(3) 0.24898(18) 0.1227(3) 0.0252(11) Uani 1 1 d . . . . .
H22A H 0.2655 0.2734 0.0978 0.030 Uiso 1 1 calc R U . . .
H22B H 0.2390 0.2468 0.1855 0.030 Uiso 1 1 calc R U . . .
C23 C 0.1466(3) 0.2779(2) 0.1036(3) 0.0337(13) Uani 1 1 d . . . . .
H23A H 0.1514 0.3210 0.1132 0.040 Uiso 1 1 calc R U . . .
H23B H 0.1293 0.2716 0.0424 0.040 Uiso 1 1 calc R U . . .
C24 C 0.0861(3) 0.2535(2) 0.1593(5) 0.066(2) Uani 1 1 d . . . . .
H24A H 0.0366 0.2716 0.1418 0.099 Uiso 1 1 calc R U . . .
H24B H 0.1006 0.2627 0.2198 0.099 Uiso 1 1 calc R U . . .
H24C H 0.0823 0.2107 0.1520 0.099 Uiso 1 1 calc R U . . .
C25 C 0.3140(3) 0.13776(18) 0.2028(3) 0.0205(11) Uani 1 1 d . . . . .
H25A H 0.3649 0.1196 0.2145 0.025 Uiso 1 1 calc R U . . .
H25B H 0.3149 0.1761 0.2333 0.025 Uiso 1 1 calc R U . . .
C26 C 0.2545(3) 0.0975(2) 0.2411(3) 0.0281(12) Uani 1 1 d . . . . .
H26A H 0.2031 0.1073 0.2142 0.034 Uiso 1 1 calc R U . . .
H26B H 0.2653 0.0559 0.2270 0.034 Uiso 1 1 calc R U . . .
C27 C 0.2545(3) 0.1037(2) 0.3388(3) 0.0322(13) Uani 1 1 d . . . . .
H27A H 0.3078 0.1017 0.3647 0.039 Uiso 1 1 calc R U . . .
H27B H 0.2264 0.0700 0.3612 0.039 Uiso 1 1 calc R U . . .
C28 C 0.2182(3) 0.1616(2) 0.3673(3) 0.0440(15) Uani 1 1 d . . . . .
H28A H 0.2456 0.1953 0.3453 0.066 Uiso 1 1 calc R U . . .
H28B H 0.2214 0.1633 0.4302 0.066 Uiso 1 1 calc R U . . .
H28C H 0.1646 0.1631 0.3446 0.066 Uiso 1 1 calc R U . . .
C29 C 0.3702(2) 0.18400(18) 0.0766(3) 0.0198(11) Uani 1 1 d . . . . .
H29A H 0.3786 0.2191 0.1138 0.024 Uiso 1 1 calc R U . . .
H29B H 0.4158 0.1586 0.0860 0.024 Uiso 1 1 calc R U . . .
C30 C 0.3630(3) 0.20436(19) -0.0177(3) 0.0215(11) Uani 1 1 d . . . . .
H30A H 0.3257 0.2371 -0.0245 0.026 Uiso 1 1 calc R U . . .
H30B H 0.3433 0.1713 -0.0546 0.026 Uiso 1 1 calc R U . . .
C31 C 0.4407(3) 0.2254(2) -0.0477(3) 0.0246(11) Uani 1 1 d . . . . .
H31A H 0.4638 0.2545 -0.0060 0.030 Uiso 1 1 calc R U . . .
H31B H 0.4757 0.1913 -0.0488 0.030 Uiso 1 1 calc R U . . .
C32 C 0.4314(3) 0.25376(19) -0.1373(3) 0.0249(11) Uani 1 1 d . . . . .
H32A H 0.4049 0.2263 -0.1779 0.037 Uiso 1 1 calc R U . . .
H32B H 0.4818 0.2629 -0.1561 0.037 Uiso 1 1 calc R U . . .
H32C H 0.4017 0.2902 -0.1349 0.037 Uiso 1 1 calc R U . . .
N2 N 0.20837(19) 0.57720(15) 0.2100(2) 0.0154(8) Uani 1 1 d . . . . .
C33 C 0.2097(3) 0.55402(18) 0.1169(3) 0.0180(10) Uani 1 1 d . . . . .
H33A H 0.2032 0.5879 0.0770 0.022 Uiso 1 1 calc R U . . .
H33B H 0.2604 0.5365 0.1102 0.022 Uiso 1 1 calc R U . . .
C34 C 0.1477(3) 0.5075(2) 0.0906(3) 0.0288(12) Uani 1 1 d . . . . .
H34A H 0.1602 0.4703 0.1219 0.035 Uiso 1 1 calc R U . . .
H34B H 0.0980 0.5216 0.1077 0.035 Uiso 1 1 calc R U . . .
C35 C 0.1408(3) 0.4952(2) -0.0044(3) 0.0315(13) Uani 1 1 d . . . . .
H35A H 0.1920 0.4851 -0.0219 0.038 Uiso 1 1 calc R U . . .
H35B H 0.1242 0.5319 -0.0349 0.038 Uiso 1 1 calc R U . . .
C36 C 0.0852(3) 0.4452(2) -0.0344(3) 0.0351(13) Uani 1 1 d . . . . .
H36A H 0.0795 0.4440 -0.0973 0.053 Uiso 1 1 calc R U . . .
H36B H 0.0354 0.4525 -0.0128 0.053 Uiso 1 1 calc R U . . .
H36C H 0.1053 0.4074 -0.0123 0.053 Uiso 1 1 calc R U . . .
C37 C 0.2189(3) 0.52513(18) 0.2732(3) 0.0176(10) Uani 1 1 d . . . . .
H37A H 0.1778 0.4961 0.2589 0.021 Uiso 1 1 calc R U . . .
H37B H 0.2129 0.5399 0.3318 0.021 Uiso 1 1 calc R U . . .
C38 C 0.2971(3) 0.49280(18) 0.2738(3) 0.0226(11) Uani 1 1 d . . . . .
H38A H 0.3370 0.5163 0.3068 0.027 Uiso 1 1 calc R U . . .
H38B H 0.3117 0.4887 0.2143 0.027 Uiso 1 1 calc R U . . .
C39 C 0.2916(3) 0.43013(19) 0.3156(3) 0.0241(11) Uani 1 1 d . . . . .
H39A H 0.3434 0.4174 0.3377 0.029 Uiso 1 1 calc R U . . .
H39B H 0.2603 0.4331 0.3652 0.029 Uiso 1 1 calc R U . . .
C40 C 0.2568(3) 0.3827(2) 0.2538(3) 0.0341(13) Uani 1 1 d . . . . .
H40A H 0.2856 0.3809 0.2029 0.051 Uiso 1 1 calc R U . . .
H40B H 0.2036 0.3928 0.2364 0.051 Uiso 1 1 calc R U . . .
H40C H 0.2589 0.3443 0.2826 0.051 Uiso 1 1 calc R U . . .
C41 C 0.1321(2) 0.60809(19) 0.2229(3) 0.0182(10) Uani 1 1 d . . . . .
H41A H 0.1376 0.6296 0.2782 0.022 Uiso 1 1 calc R U . . .
H41B H 0.0926 0.5774 0.2275 0.022 Uiso 1 1 calc R U . . .
C42 C 0.1033(3) 0.6521(2) 0.1513(3) 0.0320(13) Uani 1 1 d . . . . .
H42A H 0.0896 0.6301 0.0975 0.038 Uiso 1 1 calc R U . . .
H42B H 0.1450 0.6799 0.1406 0.038 Uiso 1 1 calc R U . . .
C43 C 0.0327(3) 0.68779(19) 0.1760(3) 0.0267(12) Uani 1 1 d . . . . .
H43A H -0.0025 0.6610 0.2033 0.032 Uiso 1 1 calc R U . . .
H43B H 0.0496 0.7186 0.2183 0.032 Uiso 1 1 calc R U . . .
C44 C -0.0093(3) 0.7167(2) 0.0976(3) 0.0382(14) Uani 1 1 d . . . . .
H44A H -0.0300 0.6861 0.0579 0.057 Uiso 1 1 calc R U . . .
H44B H 0.0262 0.7416 0.0687 0.057 Uiso 1 1 calc R U . . .
H44C H -0.0511 0.7410 0.1158 0.057 Uiso 1 1 calc R U . . .
C45 C 0.2754(3) 0.62186(18) 0.2261(3) 0.0182(10) Uani 1 1 d . . . . .
H45A H 0.3226 0.6031 0.2089 0.022 Uiso 1 1 calc R U . . .
H45B H 0.2648 0.6566 0.1886 0.022 Uiso 1 1 calc R U . . .
C46 C 0.2897(3) 0.64332(18) 0.3201(3) 0.0190(10) Uani 1 1 d . . . . .
H46A H 0.3062 0.6095 0.3573 0.023 Uiso 1 1 calc R U . . .
H46B H 0.2416 0.6588 0.3398 0.023 Uiso 1 1 calc R U . . .
C47 C 0.3516(3) 0.69229(18) 0.3293(3) 0.0217(11) Uani 1 1 d . . . . .
H47A H 0.3350 0.7255 0.2910 0.026 Uiso 1 1 calc R U . . .
H47B H 0.3551 0.7072 0.3890 0.026 Uiso 1 1 calc R U . . .
C48 C 0.4319(3) 0.6722(2) 0.3077(3) 0.0271(12) Uani 1 1 d . . . . .
H48A H 0.4301 0.6607 0.2472 0.041 Uiso 1 1 calc R U . . .
H48B H 0.4482 0.6384 0.3439 0.041 Uiso 1 1 calc R U . . .
H48C H 0.4681 0.7047 0.3185 0.041 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 O11 1.613(3) . ?
V1 O2 1.761(3) . ?
V1 O5 1.887(3) . ?
V1 O7 1.996(3) . ?
V1 O8 2.055(3) . ?
V1 O1 2.2439(8) . ?
V1 V2 3.0265(11) . ?
V1 V3 3.0496(11) . ?
V2 O4 1.603(3) . ?
V2 O3 1.758(3) . ?
V2 O2 1.910(3) . ?
V2 O8 1.962(3) 3_665 ?
V2 O9 2.074(3) 3_665 ?
V2 O1 2.2194(7) . ?
V2 V3 3.0244(10) 3_665 ?
V3 O6 1.606(3) . ?
V3 O5 1.767(3) . ?
V3 O3 1.893(3) 3_665 ?
V3 O9 1.983(3) 3_665 ?
V3 O7 2.058(3) 3_665 ?
V3 O1 2.2628(7) . ?
V3 V2 3.0245(10) 3_665 ?
O1 V2 2.2194(7) 3_665 ?
O1 V1 2.2439(8) 3_665 ?
O1 V3 2.2628(7) 3_665 ?
O3 V3 1.893(3) 3_665 ?
O7 C1 1.432(5) . ?
O7 V3 2.058(3) 3_665 ?
O8 C3 1.431(5) . ?
O8 V2 1.962(3) 3_665 ?
O9 C4 1.435(5) . ?
O9 V3 1.983(3) 3_665 ?
O9 V2 2.074(3) 3_665 ?
O10 C5 1.422(5) . ?
O10 C6 1.430(5) . ?
C1 C2 1.532(6) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C2 C5 1.529(5) . ?
C2 C4 1.531(6) . ?
C2 C3 1.532(5) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C6 C7 1.470(6) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C7 C8 1.180(6) . ?
C8 H8 0.9300 . ?
V4 O22 1.605(3) . ?
V4 O13 1.768(3) . ?
V4 O16 1.894(3) . ?
V4 O19 1.978(3) . ?
V4 O18 2.070(3) . ?
V4 O12 2.2308(7) . ?
V4 V6 3.0319(10) . ?
V4 V5 3.0322(10) . ?
V5 O15 1.597(3) . ?
V5 O14 1.764(3) . ?
V5 O13 1.891(3) . ?
V5 O18 1.971(3) 3_566 ?
V5 O20 2.066(3) 3_566 ?
V5 O12 2.2542(7) . ?
V5 V6 3.0284(11) 3_566 ?
V6 O17 1.609(3) . ?
V6 O16 1.757(3) . ?
V6 O14 1.886(3) 3_566 ?
V6 O20 1.996(3) 3_566 ?
V6 O19 2.053(3) 3_566 ?
V6 O12 2.2365(7) . ?
V6 V5 3.0283(11) 3_566 ?
O12 V4 2.2307(7) 3_566 ?
O12 V6 2.2366(7) 3_566 ?
O12 V5 2.2541(7) 3_566 ?
O14 V6 1.886(3) 3_566 ?
O18 C9 1.429(5) . ?
O18 V5 1.971(3) 3_566 ?
O19 C11 1.429(4) . ?
O19 V6 2.053(3) 3_566 ?
O20 C12 1.428(5) . ?
O20 V6 1.996(3) 3_566 ?
O20 V5 2.066(3) 3_566 ?
O21 C13 1.406(5) . ?
O21 C14 1.425(5) . ?
C9 C10 1.541(5) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 C13 1.520(6) . ?
C10 C12 1.532(6) . ?
C10 C11 1.535(6) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C14 C15 1.463(6) . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C15 C16 1.182(6) . ?
C16 H16 0.9300 . ?
N1 C29 1.517(5) . ?
N1 C25 1.519(5) . ?
N1 C17 1.521(5) . ?
N1 C21 1.527(5) . ?
C17 C18 1.519(6) . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C18 C19 1.530(5) . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
C19 C20 1.525(6) . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
C21 C22 1.511(6) . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C22 C23 1.523(6) . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
C23 C24 1.504(7) . ?
C23 H23A 0.9700 . ?
C23 H23B 0.9700 . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
C25 C26 1.516(6) . ?
C25 H25A 0.9700 . ?
C25 H25B 0.9700 . ?
C26 C27 1.503(6) . ?
C26 H26A 0.9700 . ?
C26 H26B 0.9700 . ?
C27 C28 1.511(7) . ?
C27 H27A 0.9700 . ?
C27 H27B 0.9700 . ?
C28 H28A 0.9600 . ?
C28 H28B 0.9600 . ?
C28 H28C 0.9600 . ?
C29 C30 1.508(6) . ?
C29 H29A 0.9700 . ?
C29 H29B 0.9700 . ?
C30 C31 1.526(6) . ?
C30 H30A 0.9700 . ?
C30 H30B 0.9700 . ?
C31 C32 1.505(6) . ?
C31 H31A 0.9700 . ?
C31 H31B 0.9700 . ?
C32 H32A 0.9600 . ?
C32 H32B 0.9600 . ?
C32 H32C 0.9600 . ?
N2 C37 1.509(5) . ?
N2 C41 1.511(5) . ?
N2 C33 1.518(5) . ?
N2 C45 1.527(5) . ?
C33 C34 1.517(6) . ?
C33 H33A 0.9700 . ?
C33 H33B 0.9700 . ?
C34 C35 1.476(6) . ?
C34 H34A 0.9700 . ?
C34 H34B 0.9700 . ?
C35 C36 1.513(6) . ?
C35 H35A 0.9700 . ?
C35 H35B 0.9700 . ?
C36 H36A 0.9600 . ?
C36 H36B 0.9600 . ?
C36 H36C 0.9600 . ?
C37 C38 1.527(6) . ?
C37 H37A 0.9700 . ?
C37 H37B 0.9700 . ?
C38 C39 1.538(6) . ?
C38 H38A 0.9700 . ?
C38 H38B 0.9700 . ?
C39 C40 1.507(6) . ?
C39 H39A 0.9700 . ?
C39 H39B 0.9700 . ?
C40 H40A 0.9600 . ?
C40 H40B 0.9600 . ?
C40 H40C 0.9600 . ?
C41 C42 1.522(6) . ?
C41 H41A 0.9700 . ?
C41 H41B 0.9700 . ?
C42 C43 1.527(6) . ?
C42 H42A 0.9700 . ?
C42 H42B 0.9700 . ?
C43 C44 1.495(6) . ?
C43 H43A 0.9700 . ?
C43 H43B 0.9700 . ?
C44 H44A 0.9600 . ?
C44 H44B 0.9600 . ?
C44 H44C 0.9600 . ?
C45 C46 1.518(6) . ?
C45 H45A 0.9700 . ?
C45 H45B 0.9700 . ?
C46 C47 1.521(6) . ?
C46 H46A 0.9700 . ?
C46 H46B 0.9700 . ?
C47 C48 1.518(6) . ?
C47 H47A 0.9700 . ?
C47 H47B 0.9700 . ?
C48 H48A 0.9600 . ?
C48 H48B 0.9600 . ?
C48 H48C 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O11 V1 O2 105.65(14) . . ?
O11 V1 O5 103.26(13) . . ?
O2 V1 O5 93.64(12) . . ?
O11 V1 O7 97.24(13) . . ?
O2 V1 O7 91.77(12) . . ?
O5 V1 O7 156.49(12) . . ?
O11 V1 O8 94.78(13) . . ?
O2 V1 O8 159.30(12) . . ?
O5 V1 O8 84.70(11) . . ?
O7 V1 O8 82.23(11) . . ?
O11 V1 O1 170.51(10) . . ?
O2 V1 O1 82.95(9) . . ?
O5 V1 O1 79.80(9) . . ?
O7 V1 O1 78.19(8) . . ?
O8 V1 O1 76.44(8) . . ?
O11 V1 V2 141.21(11) . . ?
O2 V1 V2 36.10(9) . . ?
O5 V1 V2 89.04(9) . . ?
O7 V1 V2 81.96(8) . . ?
O8 V1 V2 123.20(8) . . ?
O1 V1 V2 46.96(2) . . ?
O11 V1 V3 135.29(11) . . ?
O2 V1 V3 86.91(9) . . ?
O5 V1 V3 32.22(8) . . ?
O7 V1 V3 125.63(8) . . ?
O8 V1 V3 80.71(8) . . ?
O1 V1 V3 47.68(2) . . ?
V2 V1 V3 65.98(3) . . ?
O4 V2 O3 105.07(14) . . ?
O4 V2 O2 102.04(13) . . ?
O3 V2 O2 93.11(12) . . ?
O4 V2 O8 97.12(13) . 3_665 ?
O3 V2 O8 92.91(12) . 3_665 ?
O2 V2 O8 157.65(12) . 3_665 ?
O4 V2 O9 94.18(12) . 3_665 ?
O3 V2 O9 160.69(12) . 3_665 ?
O2 V2 O9 84.18(11) . 3_665 ?
O8 V2 O9 83.05(11) 3_665 3_665 ?
O4 V2 O1 170.82(11) . . ?
O3 V2 O1 83.50(9) . . ?
O2 V2 O1 80.45(8) . . ?
O8 V2 O1 78.89(8) 3_665 . ?
O9 V2 O1 77.19(8) 3_665 . ?
O4 V2 V3 140.02(10) . 3_665 ?
O3 V2 V3 35.52(9) . 3_665 ?
O2 V2 V3 89.78(8) . 3_665 ?
O8 V2 V3 82.75(8) 3_665 3_665 ?
O9 V2 V3 125.21(8) 3_665 3_665 ?
O1 V2 V3 48.175(19) . 3_665 ?
O4 V2 V1 134.79(11) . . ?
O3 V2 V1 86.51(9) . . ?
O2 V2 V1 32.91(8) . . ?
O8 V2 V1 126.30(9) 3_665 . ?
O9 V2 V1 80.85(8) 3_665 . ?
O1 V2 V1 47.65(2) . . ?
V3 V2 V1 66.51(2) 3_665 . ?
O6 V3 O5 105.20(14) . . ?
O6 V3 O3 103.25(13) . 3_665 ?
O5 V3 O3 94.31(12) . 3_665 ?
O6 V3 O9 98.08(13) . 3_665 ?
O5 V3 O9 90.77(12) . 3_665 ?
O3 V3 O9 155.91(11) 3_665 3_665 ?
O6 V3 O7 96.32(13) . 3_665 ?
O5 V3 O7 158.15(12) . 3_665 ?
O3 V3 O7 84.20(11) 3_665 3_665 ?
O9 V3 O7 82.42(11) 3_665 3_665 ?
O6 V3 O1 172.18(11) . . ?
O5 V3 O1 81.76(9) . . ?
O3 V3 O1 79.43(8) 3_665 . ?
O9 V3 O1 78.01(8) 3_665 . ?
O7 V3 O1 76.53(8) 3_665 . ?
O6 V3 V2 135.86(11) . 3_665 ?
O5 V3 V2 85.95(9) . 3_665 ?
O3 V3 V2 32.64(8) 3_665 3_665 ?
O9 V3 V2 124.81(8) 3_665 3_665 ?
O7 V3 V2 81.09(7) 3_665 3_665 ?
O1 V3 V2 46.96(2) . 3_665 ?
O6 V3 V1 139.49(11) . . ?
O5 V3 V1 34.70(9) . . ?
O3 V3 V1 89.26(9) 3_665 . ?
O9 V3 V1 81.61(8) 3_665 . ?
O7 V3 V1 123.47(8) 3_665 . ?
O1 V3 V1 47.155(19) . . ?
V2 V3 V1 65.38(2) 3_665 . ?
V2 O1 V2 180.0 . 3_665 ?
V2 O1 V1 85.39(3) . . ?
V2 O1 V1 94.61(3) 3_665 . ?
V2 O1 V1 94.61(3) . 3_665 ?
V2 O1 V1 85.39(3) 3_665 3_665 ?
V1 O1 V1 180.0 . 3_665 ?
V2 O1 V3 95.13(3) . . ?
V2 O1 V3 84.87(3) 3_665 . ?
V1 O1 V3 85.17(3) . . ?
V1 O1 V3 94.83(3) 3_665 . ?
V2 O1 V3 84.87(3) . 3_665 ?
V2 O1 V3 95.13(3) 3_665 3_665 ?
V1 O1 V3 94.83(3) . 3_665 ?
V1 O1 V3 85.17(3) 3_665 3_665 ?
V3 O1 V3 180.0 . 3_665 ?
V1 O2 V2 110.99(14) . . ?
V2 O3 V3 111.84(15) . 3_665 ?
V3 O5 V1 113.08(14) . . ?
C1 O7 V1 118.7(2) . . ?
C1 O7 V3 118.3(2) . 3_665 ?
V1 O7 V3 109.84(13) . 3_665 ?
C3 O8 V2 118.9(2) . 3_665 ?
C3 O8 V1 118.8(2) . . ?
V2 O8 V1 109.48(13) 3_665 . ?
C4 O9 V3 119.2(2) . 3_665 ?
C4 O9 V2 117.9(2) . 3_665 ?
V3 O9 V2 109.24(12) 3_665 3_665 ?
C5 O10 C6 113.3(3) . . ?
O7 C1 C2 112.5(3) . . ?
O7 C1 H1A 109.1 . . ?
C2 C1 H1A 109.1 . . ?
O7 C1 H1B 109.1 . . ?
C2 C1 H1B 109.1 . . ?
H1A C1 H1B 107.8 . . ?
C5 C2 C4 109.8(3) . . ?
C5 C2 C1 107.4(3) . . ?
C4 C2 C1 109.9(3) . . ?
C5 C2 C3 108.9(3) . . ?
C4 C2 C3 110.6(3) . . ?
C1 C2 C3 110.1(3) . . ?
O8 C3 C2 112.3(3) . . ?
O8 C3 H3A 109.1 . . ?
C2 C3 H3A 109.1 . . ?
O8 C3 H3B 109.1 . . ?
C2 C3 H3B 109.1 . . ?
H3A C3 H3B 107.9 . . ?
O9 C4 C2 112.2(3) . . ?
O9 C4 H4A 109.2 . . ?
C2 C4 H4A 109.2 . . ?
O9 C4 H4B 109.2 . . ?
C2 C4 H4B 109.2 . . ?
H4A C4 H4B 107.9 . . ?
O10 C5 C2 109.5(3) . . ?
O10 C5 H5A 109.8 . . ?
C2 C5 H5A 109.8 . . ?
O10 C5 H5B 109.8 . . ?
C2 C5 H5B 109.8 . . ?
H5A C5 H5B 108.2 . . ?
O10 C6 C7 113.8(3) . . ?
O10 C6 H6A 108.8 . . ?
C7 C6 H6A 108.8 . . ?
O10 C6 H6B 108.8 . . ?
C7 C6 H6B 108.8 . . ?
H6A C6 H6B 107.7 . . ?
C8 C7 C6 179.1(5) . . ?
C7 C8 H8 180.0 . . ?
O22 V4 O13 104.69(14) . . ?
O22 V4 O16 102.03(13) . . ?
O13 V4 O16 94.01(12) . . ?
O22 V4 O19 98.12(13) . . ?
O13 V4 O19 91.94(12) . . ?
O16 V4 O19 156.77(12) . . ?
O22 V4 O18 95.50(12) . . ?
O13 V4 O18 159.67(12) . . ?
O16 V4 O18 83.91(11) . . ?
O19 V4 O18 82.76(11) . . ?
O22 V4 O12 171.88(11) . . ?
O13 V4 O12 83.02(9) . . ?
O16 V4 O12 79.65(8) . . ?
O19 V4 O12 78.82(8) . . ?
O18 V4 O12 76.71(7) . . ?
O22 V4 V6 134.40(11) . . ?
O13 V4 V6 86.74(9) . . ?
O16 V4 V6 32.45(8) . . ?
O19 V4 V6 125.93(8) . . ?
O18 V4 V6 80.68(8) . . ?
O12 V4 V6 47.338(19) . . ?
O22 V4 V5 139.67(10) . . ?
O13 V4 V5 35.37(9) . . ?
O16 V4 V5 89.62(8) . . ?
O19 V4 V5 82.35(8) . . ?
O18 V4 V5 124.30(8) . . ?
O12 V4 V5 47.789(19) . . ?
V6 V4 V5 66.30(2) . . ?
O15 V5 O14 104.50(14) . . ?
O15 V5 O13 102.13(13) . . ?
O14 V5 O13 93.30(12) . . ?
O15 V5 O18 98.76(13) . 3_566 ?
O14 V5 O18 92.33(12) . 3_566 ?
O13 V5 O18 156.23(11) . 3_566 ?
O15 V5 O20 96.41(13) . 3_566 ?
O14 V5 O20 159.01(12) . 3_566 ?
O13 V5 O20 83.94(11) . 3_566 ?
O18 V5 O20 82.58(11) 3_566 3_566 ?
O15 V5 O12 172.58(11) . . ?
O14 V5 O12 82.45(9) . . ?
O13 V5 O12 79.75(9) . . ?
O18 V5 O12 78.13(8) 3_566 . ?
O20 V5 O12 76.57(8) 3_566 . ?
O15 V5 V6 139.35(11) . 3_566 ?
O14 V5 V6 35.25(9) . 3_566 ?
O13 V5 V6 89.16(9) . 3_566 ?
O18 V5 V6 82.24(8) 3_566 3_566 ?
O20 V5 V6 123.77(8) 3_566 3_566 ?
O12 V5 V6 47.351(19) . 3_566 ?
O15 V5 V4 134.83(10) . . ?
O14 V5 V4 85.86(9) . . ?
O13 V5 V4 32.75(8) . . ?
O18 V5 V4 125.05(8) 3_566 . ?
O20 V5 V4 80.59(7) 3_566 . ?
O12 V5 V4 47.137(19) . . ?
V6 V5 V4 65.55(2) 3_566 . ?
O17 V6 O16 105.35(14) . . ?
O17 V6 O14 103.23(13) . 3_566 ?
O16 V6 O14 93.78(12) . 3_566 ?
O17 V6 O20 96.73(13) . 3_566 ?
O16 V6 O20 91.31(12) . 3_566 ?
O14 V6 O20 157.26(12) 3_566 3_566 ?
O17 V6 O19 94.94(12) . 3_566 ?
O16 V6 O19 159.47(12) . 3_566 ?
O14 V6 O19 84.42(11) 3_566 3_566 ?
O20 V6 O19 83.10(11) 3_566 3_566 ?
O17 V6 O12 171.09(10) . . ?
O16 V6 O12 82.36(9) . . ?
O14 V6 O12 80.36(9) 3_566 . ?
O20 V6 O12 78.38(8) 3_566 . ?
O19 V6 O12 77.17(8) 3_566 . ?
O17 V6 V5 135.80(11) . 3_566 ?
O16 V6 V5 86.17(9) . 3_566 ?
O14 V6 V5 32.65(8) 3_566 3_566 ?
O20 V6 V5 126.05(8) 3_566 3_566 ?
O19 V6 V5 81.32(8) 3_566 3_566 ?
O12 V6 V5 47.84(2) . 3_566 ?
O17 V6 V4 140.04(10) . . ?
O16 V6 V4 35.32(9) . . ?
O14 V6 V4 89.82(9) 3_566 . ?
O20 V6 V4 81.63(8) 3_566 . ?
O19 V6 V4 124.14(8) 3_566 . ?
O12 V6 V4 47.178(19) . . ?
V5 V6 V4 66.09(3) 3_566 . ?
V4 O12 V4 180.0 3_566 . ?
V4 O12 V6 94.52(3) 3_566 . ?
V4 O12 V6 85.48(3) . . ?
V4 O12 V6 85.49(3) 3_566 3_566 ?
V4 O12 V6 94.52(3) . 3_566 ?
V6 O12 V6 180.0 . 3_566 ?
V4 O12 V5 85.07(3) 3_566 3_566 ?
V4 O12 V5 94.93(3) . 3_566 ?
V6 O12 V5 84.81(3) . 3_566 ?
V6 O12 V5 95.19(3) 3_566 3_566 ?
V4 O12 V5 94.93(3) 3_566 . ?
V4 O12 V5 85.07(3) . . ?
V6 O12 V5 95.19(3) . . ?
V6 O12 V5 84.81(3) 3_566 . ?
V5 O12 V5 180.00(2) 3_566 . ?
V4 O13 V5 111.88(15) . . ?
V5 O14 V6 112.10(14) . 3_566 ?
V6 O16 V4 112.23(14) . . ?
C9 O18 V5 119.4(2) . 3_566 ?
C9 O18 V4 117.9(2) . . ?
V5 O18 V4 109.68(12) 3_566 . ?
C11 O19 V4 119.1(2) . . ?
C11 O19 V6 118.5(2) . 3_566 ?
V4 O19 V6 108.93(12) . 3_566 ?
C12 O20 V6 118.5(2) . 3_566 ?
C12 O20 V5 118.2(2) . 3_566 ?
V6 O20 V5 109.42(13) 3_566 3_566 ?
C13 O21 C14 112.5(3) . . ?
O18 C9 C10 112.5(3) . . ?
O18 C9 H9A 109.1 . . ?
C10 C9 H9A 109.1 . . ?
O18 C9 H9B 109.1 . . ?
C10 C9 H9B 109.1 . . ?
H9A C9 H9B 107.8 . . ?
C13 C10 C12 107.4(3) . . ?
C13 C10 C11 109.8(3) . . ?
C12 C10 C11 110.6(3) . . ?
C13 C10 C9 109.6(3) . . ?
C12 C10 C9 109.9(3) . . ?
C11 C10 C9 109.5(3) . . ?
O19 C11 C10 112.7(3) . . ?
O19 C11 H11A 109.1 . . ?
C10 C11 H11A 109.1 . . ?
O19 C11 H11B 109.1 . . ?
C10 C11 H11B 109.1 . . ?
H11A C11 H11B 107.8 . . ?
O20 C12 C10 112.8(3) . . ?
O20 C12 H12A 109.0 . . ?
C10 C12 H12A 109.0 . . ?
O20 C12 H12B 109.0 . . ?
C10 C12 H12B 109.0 . . ?
H12A C12 H12B 107.8 . . ?
O21 C13 C10 110.2(3) . . ?
O21 C13 H13A 109.6 . . ?
C10 C13 H13A 109.6 . . ?
O21 C13 H13B 109.6 . . ?
C10 C13 H13B 109.6 . . ?
H13A C13 H13B 108.1 . . ?
O21 C14 C15 113.2(3) . . ?
O21 C14 H14A 108.9 . . ?
C15 C14 H14A 108.9 . . ?
O21 C14 H14B 108.9 . . ?
C15 C14 H14B 108.9 . . ?
H14A C14 H14B 107.8 . . ?
C16 C15 C14 178.8(5) . . ?
C15 C16 H16 180.0 . . ?
C29 N1 C25 108.2(3) . . ?
C29 N1 C17 111.1(3) . . ?
C25 N1 C17 109.9(3) . . ?
C29 N1 C21 109.9(3) . . ?
C25 N1 C21 111.0(3) . . ?
C17 N1 C21 106.7(3) . . ?
C18 C17 N1 115.2(3) . . ?
C18 C17 H17A 108.5 . . ?
N1 C17 H17A 108.5 . . ?
C18 C17 H17B 108.5 . . ?
N1 C17 H17B 108.5 . . ?
H17A C17 H17B 107.5 . . ?
C17 C18 C19 110.6(3) . . ?
C17 C18 H18A 109.5 . . ?
C19 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
C19 C18 H18B 109.5 . . ?
H18A C18 H18B 108.1 . . ?
C20 C19 C18 112.2(4) . . ?
C20 C19 H19A 109.2 . . ?
C18 C19 H19A 109.2 . . ?
C20 C19 H19B 109.2 . . ?
C18 C19 H19B 109.2 . . ?
H19A C19 H19B 107.9 . . ?
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 115.8(3) . . ?
C22 C21 H21A 108.3 . . ?
N1 C21 H21A 108.3 . . ?
C22 C21 H21B 108.3 . . ?
N1 C21 H21B 108.3 . . ?
H21A C21 H21B 107.4 . . ?
C21 C22 C23 110.1(4) . . ?
C21 C22 H22A 109.6 . . ?
C23 C22 H22A 109.6 . . ?
C21 C22 H22B 109.6 . . ?
C23 C22 H22B 109.6 . . ?
H22A C22 H22B 108.2 . . ?
C24 C23 C22 113.4(4) . . ?
C24 C23 H23A 108.9 . . ?
C22 C23 H23A 108.9 . . ?
C24 C23 H23B 108.9 . . ?
C22 C23 H23B 108.9 . . ?
H23A C23 H23B 107.7 . . ?
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 115.6(3) . . ?
C26 C25 H25A 108.4 . . ?
N1 C25 H25A 108.4 . . ?
C26 C25 H25B 108.4 . . ?
N1 C25 H25B 108.4 . . ?
H25A C25 H25B 107.4 . . ?
C27 C26 C25 112.8(4) . . ?
C27 C26 H26A 109.0 . . ?
C25 C26 H26A 109.0 . . ?
C27 C26 H26B 109.0 . . ?
C25 C26 H26B 109.0 . . ?
H26A C26 H26B 107.8 . . ?
C26 C27 C28 113.6(4) . . ?
C26 C27 H27A 108.8 . . ?
C28 C27 H27A 108.8 . . ?
C26 C27 H27B 108.8 . . ?
C28 C27 H27B 108.8 . . ?
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 115.0(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 112.1(4) . . ?
C29 C30 H30A 109.2 . . ?
C31 C30 H30A 109.2 . . ?
C29 C30 H30B 109.2 . . ?
C31 C30 H30B 109.2 . . ?
H30A C30 H30B 107.9 . . ?
C32 C31 C30 112.0(4) . . ?
C32 C31 H31A 109.2 . . ?
C30 C31 H31A 109.2 . . ?
C32 C31 H31B 109.2 . . ?
C30 C31 H31B 109.2 . . ?
H31A C31 H31B 107.9 . . ?
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 . . ?
C37 N2 C41 108.8(3) . . ?
C37 N2 C33 109.4(3) . . ?
C41 N2 C33 111.0(3) . . ?
C37 N2 C45 110.2(3) . . ?
C41 N2 C45 109.8(3) . . ?
C33 N2 C45 107.5(3) . . ?
C34 C33 N2 114.5(3) . . ?
C34 C33 H33A 108.6 . . ?
N2 C33 H33A 108.6 . . ?
C34 C33 H33B 108.6 . . ?
N2 C33 H33B 108.6 . . ?
H33A C33 H33B 107.6 . . ?
C35 C34 C33 112.6(4) . . ?
C35 C34 H34A 109.1 . . ?
C33 C34 H34A 109.1 . . ?
C35 C34 H34B 109.1 . . ?
C33 C34 H34B 109.1 . . ?
H34A C34 H34B 107.8 . . ?
C34 C35 C36 115.5(4) . . ?
C34 C35 H35A 108.4 . . ?
C36 C35 H35A 108.4 . . ?
C34 C35 H35B 108.4 . . ?
C36 C35 H35B 108.4 . . ?
H35A C35 H35B 107.5 . . ?
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 . . ?
N2 C37 C38 115.0(4) . . ?
N2 C37 H37A 108.5 . . ?
C38 C37 H37A 108.5 . . ?
N2 C37 H37B 108.5 . . ?
C38 C37 H37B 108.5 . . ?
H37A C37 H37B 107.5 . . ?
C37 C38 C39 110.0(4) . . ?
C37 C38 H38A 109.7 . . ?
C39 C38 H38A 109.7 . . ?
C37 C38 H38B 109.7 . . ?
C39 C38 H38B 109.7 . . ?
H38A C38 H38B 108.2 . . ?
C40 C39 C38 113.9(4) . . ?
C40 C39 H39A 108.8 . . ?
C38 C39 H39A 108.8 . . ?
C40 C39 H39B 108.8 . . ?
C38 C39 H39B 108.8 . . ?
H39A C39 H39B 107.7 . . ?
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 . . ?
N2 C41 C42 115.6(4) . . ?
N2 C41 H41A 108.4 . . ?
C42 C41 H41A 108.4 . . ?
N2 C41 H41B 108.4 . . ?
C42 C41 H41B 108.4 . . ?
H41A C41 H41B 107.5 . . ?
C41 C42 C43 111.9(4) . . ?
C41 C42 H42A 109.2 . . ?
C43 C42 H42A 109.2 . . ?
C41 C42 H42B 109.2 . . ?
C43 C42 H42B 109.2 . . ?
H42A C42 H42B 107.9 . . ?
C44 C43 C42 111.5(4) . . ?
C44 C43 H43A 109.3 . . ?
C42 C43 H43A 109.3 . . ?
C44 C43 H43B 109.3 . . ?
C42 C43 H43B 109.3 . . ?
H43A C43 H43B 108.0 . . ?
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 114.7(3) . . ?
C46 C45 H45A 108.6 . . ?
N2 C45 H45A 108.6 . . ?
C46 C45 H45B 108.6 . . ?
N2 C45 H45B 108.6 . . ?
H45A C45 H45B 107.6 . . ?
C45 C46 C47 111.6(4) . . ?
C45 C46 H46A 109.3 . . ?
C47 C46 H46A 109.3 . . ?
C45 C46 H46B 109.3 . . ?
C47 C46 H46B 109.3 . . ?
H46A C46 H46B 108.0 . . ?
C48 C47 C46 114.5(4) . . ?
C48 C47 H47A 108.6 . . ?
C46 C47 H47A 108.6 . . ?
C48 C47 H47B 108.6 . . ?
C46 C47 H47B 108.6 . . ?
H47A C47 H47B 107.6 . . ?
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 . . ?

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
O11 V1 O2 V2 -171.78(14) . . . . ?
O5 V1 O2 V2 83.36(15) . . . . ?
O7 V1 O2 V2 -73.76(15) . . . . ?
O8 V1 O2 V2 -1.3(4) . . . . ?
O1 V1 O2 V2 4.11(11) . . . . ?
V3 V1 O2 V2 51.83(12) . . . . ?
O4 V2 O3 V3 171.40(15) . . . 3_665 ?
O2 V2 O3 V3 -85.25(15) . . . 3_665 ?
O8 V2 O3 V3 73.23(15) 3_665 . . 3_665 ?
O9 V2 O3 V3 -4.0(5) 3_665 . . 3_665 ?
O1 V2 O3 V3 -5.24(12) . . . 3_665 ?
V1 V2 O3 V3 -52.99(12) . . . 3_665 ?
O6 V3 O5 V1 172.58(15) . . . . ?
O3 V3 O5 V1 -82.43(15) 3_665 . . . ?
O9 V3 O5 V1 74.00(15) 3_665 . . . ?
O7 V3 O5 V1 2.7(4) 3_665 . . . ?
O1 V3 O5 V1 -3.78(12) . . . . ?
V2 V3 O5 V1 -50.85(13) 3_665 . . . ?
O11 V1 O5 V3 174.65(15) . . . . ?
O2 V1 O5 V3 -78.33(16) . . . . ?
O7 V1 O5 V3 24.6(4) . . . . ?
O8 V1 O5 V3 80.98(15) . . . . ?
O1 V1 O5 V3 3.83(12) . . . . ?
V2 V1 O5 V3 -42.50(13) . . . . ?
V1 O7 C1 C2 -70.4(4) . . . . ?
V3 O7 C1 C2 66.9(4) 3_665 . . . ?
O7 C1 C2 C5 179.8(3) . . . . ?
O7 C1 C2 C4 -60.7(4) . . . . ?
O7 C1 C2 C3 61.3(4) . . . . ?
V2 O8 C3 C2 -70.7(4) 3_665 . . . ?
V1 O8 C3 C2 67.0(4) . . . . ?
C5 C2 C3 O8 -177.6(3) . . . . ?
C4 C2 C3 O8 61.6(4) . . . . ?
C1 C2 C3 O8 -60.0(4) . . . . ?
V3 O9 C4 C2 -70.6(4) 3_665 . . . ?
V2 O9 C4 C2 65.7(4) 3_665 . . . ?
C5 C2 C4 O9 179.4(3) . . . . ?
C1 C2 C4 O9 61.4(4) . . . . ?
C3 C2 C4 O9 -60.3(4) . . . . ?
C6 O10 C5 C2 163.5(3) . . . . ?
C4 C2 C5 O10 59.8(4) . . . . ?
C1 C2 C5 O10 179.3(3) . . . . ?
C3 C2 C5 O10 -61.4(4) . . . . ?
C5 O10 C6 C7 64.1(5) . . . . ?
O22 V4 O13 V5 172.78(15) . . . . ?
O16 V4 O13 V5 -83.67(15) . . . . ?
O19 V4 O13 V5 73.86(15) . . . . ?
O18 V4 O13 V5 -0.4(4) . . . . ?
O12 V4 O13 V5 -4.62(12) . . . . ?
V6 V4 O13 V5 -52.02(13) . . . . ?
O15 V5 O13 V4 177.30(16) . . . . ?
O14 V5 O13 V4 -77.10(16) . . . . ?
O18 V5 O13 V4 26.3(4) 3_566 . . . ?
O20 V5 O13 V4 82.02(15) 3_566 . . . ?
O12 V5 O13 V4 4.61(12) . . . . ?
V6 V5 O13 V4 -42.08(13) 3_566 . . . ?
O15 V5 O14 V6 -172.72(14) . . . 3_566 ?
O13 V5 O14 V6 83.85(15) . . . 3_566 ?
O18 V5 O14 V6 -73.04(14) 3_566 . . 3_566 ?
O20 V5 O14 V6 2.2(4) 3_566 . . 3_566 ?
O12 V5 O14 V6 4.65(11) . . . 3_566 ?
V4 V5 O14 V6 51.93(12) . . . 3_566 ?
O17 V6 O16 V4 -170.84(14) . . . . ?
O14 V6 O16 V4 84.32(15) 3_566 . . . ?
O20 V6 O16 V4 -73.50(15) 3_566 . . . ?
O19 V6 O16 V4 0.1(4) 3_566 . . . ?
O12 V6 O16 V4 4.59(11) . . . . ?
V5 V6 O16 V4 52.55(12) 3_566 . . . ?
O22 V4 O16 V6 -176.54(15) . . . . ?
O13 V4 O16 V6 77.50(16) . . . . ?
O19 V4 O16 V6 -26.9(4) . . . . ?
O18 V4 O16 V6 -82.20(15) . . . . ?
O12 V4 O16 V6 -4.64(12) . . . . ?
V5 V4 O16 V6 42.38(13) . . . . ?
V5 O18 C9 C10 70.4(4) 3_566 . . . ?
V4 O18 C9 C10 -67.0(4) . . . . ?
O18 C9 C10 C13 -178.5(3) . . . . ?
O18 C9 C10 C12 -60.7(4) . . . . ?
O18 C9 C10 C11 61.0(4) . . . . ?
V4 O19 C11 C10 70.5(4) . . . . ?
V6 O19 C11 C10 -66.0(4) 3_566 . . . ?
C13 C10 C11 O19 178.0(3) . . . . ?
C12 C10 C11 O19 59.7(4) . . . . ?
C9 C10 C11 O19 -61.6(4) . . . . ?
V6 O20 C12 C10 69.6(4) 3_566 . . . ?
V5 O20 C12 C10 -66.6(4) 3_566 . . . ?
C13 C10 C12 O20 179.3(3) . . . . ?
C11 C10 C12 O20 -61.0(4) . . . . ?
C9 C10 C12 O20 60.0(4) . . . . ?
C14 O21 C13 C10 -172.7(3) . . . . ?
C12 C10 C13 O21 -177.0(3) . . . . ?
C11 C10 C13 O21 62.7(4) . . . . ?
C9 C10 C13 O21 -57.6(4) . . . . ?
C13 O21 C14 C15 -70.0(5) . . . . ?
C29 N1 C17 C18 48.7(5) . . . . ?
C25 N1 C17 C18 -71.0(4) . . . . ?
C21 N1 C17 C18 168.5(3) . . . . ?
N1 C17 C18 C19 163.6(4) . . . . ?
C17 C18 C19 C20 167.1(4) . . . . ?
C29 N1 C21 C22 -56.4(5) . . . . ?
C25 N1 C21 C22 63.3(5) . . . . ?
C17 N1 C21 C22 -176.9(4) . . . . ?
N1 C21 C22 C23 -174.6(4) . . . . ?
C21 C22 C23 C24 75.2(6) . . . . ?
C29 N1 C25 C26 -173.1(3) . . . . ?
C17 N1 C25 C26 -51.7(5) . . . . ?
C21 N1 C25 C26 66.2(4) . . . . ?
N1 C25 C26 C27 -160.8(4) . . . . ?
C25 C26 C27 C28 73.8(5) . . . . ?
C25 N1 C29 C30 -174.9(3) . . . . ?
C17 N1 C29 C30 64.4(4) . . . . ?
C21 N1 C29 C30 -53.5(4) . . . . ?
N1 C29 C30 C31 -167.0(3) . . . . ?
C29 C30 C31 C32 -172.0(4) . . . . ?
C37 N2 C33 C34 58.7(5) . . . . ?
C41 N2 C33 C34 -61.4(4) . . . . ?
C45 N2 C33 C34 178.4(4) . . . . ?
N2 C33 C34 C35 168.6(4) . . . . ?
C33 C34 C35 C36 174.8(4) . . . . ?
C41 N2 C37 C38 -174.7(3) . . . . ?
C33 N2 C37 C38 63.8(4) . . . . ?
C45 N2 C37 C38 -54.2(5) . . . . ?
N2 C37 C38 C39 -161.4(4) . . . . ?
C37 C38 C39 C40 82.0(5) . . . . ?
C37 N2 C41 C42 -166.5(4) . . . . ?
C33 N2 C41 C42 -46.0(5) . . . . ?
C45 N2 C41 C42 72.8(5) . . . . ?
N2 C41 C42 C43 -171.7(4) . . . . ?
C41 C42 C43 C44 -163.0(4) . . . . ?
C37 N2 C45 C46 -53.0(5) . . . . ?
C41 N2 C45 C46 66.9(4) . . . . ?
C33 N2 C45 C46 -172.1(3) . . . . ?
N2 C45 C46 C47 -174.2(3) . . . . ?
C45 C46 C47 C48 -63.8(5) . . . . ?

_refine_diff_density_max         0.638
_refine_diff_density_min         -0.423
_refine_diff_density_rms         0.095

####################################################################### 
# 
# 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_2f
_database_code_depnum_ccdc_archive 'CCDC 1558508'
_audit_update_record             
;
2017-06-26 deposited with the CCDC.
2017-09-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C24 H36 N6 O25 V6, 2(C16 H36 N)'
_chemical_formula_sum            'C56 H108 N8 O25 V6'
_chemical_formula_weight         1599.14

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

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

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

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

_cell_length_a                   11.4733(17)
_cell_length_b                   11.9543(17)
_cell_length_c                   14.603(2)
_cell_angle_alpha                73.992(2)
_cell_angle_beta                 71.464(2)
_cell_angle_gamma                78.819(3)
_cell_volume                     1812.9(5)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    1848
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      20.86
_cell_measurement_theta_min      2.44

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.465
_exptl_crystal_F_000             838
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.18
_exptl_absorpt_coefficient_mu    0.821
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6611
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2008/1 (Bruker,2008) was used for absorption correction. wR2(int) was 0.1235 before and 0.0486 after correction. The Ratio of minimum to maximum transmission is 0.8869. The λ/2 correction factor is 0.0015.'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  'multilayer optics'
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX CCD'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            22167
_diffrn_reflns_av_unetI/netI     0.0887
_diffrn_reflns_av_R_equivalents  0.0650
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         1.511
_diffrn_reflns_theta_max         26.342
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             7395
_reflns_number_gt                5373
_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       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0520P)²+1.6840P] 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     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_extinction_coef       0.0022(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         7395
_refine_ls_number_parameters     435
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0819
_refine_ls_R_factor_gt           0.0564
_refine_ls_wR_factor_ref         0.1530
_refine_ls_wR_factor_gt          0.1388
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_restrained_S_all      1.046
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
V1 V 0.96341(6) 0.42039(5) 0.39181(4) 0.02558(17) Uani 1 1 d . . . . .
V2 V 1.04500(6) 0.65497(5) 0.37203(4) 0.02533(17) Uani 1 1 d . . . . .
V3 V 1.18945(6) 0.40024(5) 0.46193(5) 0.02647(18) Uani 1 1 d . . . . .
O1 O 1.0000 0.5000 0.5000 0.0211(7) Uani 1 2 d S . P . .
O2 O 0.9115(2) 0.30024(19) 0.52310(17) 0.0236(5) Uani 1 1 d . . . . .
O3 O 0.7983(2) 0.50417(19) 0.44515(17) 0.0240(5) Uani 1 1 d . . . . .
O4 O 1.1244(2) 0.34795(19) 0.38913(17) 0.0256(5) Uani 1 1 d . . . . .
O5 O 0.8872(2) 0.70248(19) 0.41867(17) 0.0267(5) Uani 1 1 d . . . . .
O6 O 1.2119(2) 0.55066(19) 0.36329(17) 0.0250(5) Uani 1 1 d . . . . .
O7 O 1.0117(2) 0.5519(2) 0.30795(17) 0.0260(5) Uani 1 1 d . . . . .
O8 O 0.9222(2) 0.3541(2) 0.32684(18) 0.0301(6) Uani 1 1 d . . . . .
O9 O 1.0976(2) 0.7604(2) 0.28178(18) 0.0304(6) Uani 1 1 d . . . . .
O10 O 1.3310(2) 0.3431(2) 0.4394(2) 0.0337(6) Uani 1 1 d . . . . .
O11 O 1.4393(2) 0.8111(2) 0.33457(19) 0.0318(6) Uani 1 1 d . . . . .
N1 N 1.1956(3) 1.1140(3) 0.2028(2) 0.0299(7) Uani 1 1 d . . . . .
C1 C 1.3152(3) 0.6553(3) 0.4335(3) 0.0292(8) Uani 1 1 d . . . . .
N2 N 1.7373(3) 0.7264(3) 0.0911(2) 0.0440(9) Uani 1 1 d . . . . .
C2 C 1.3182(3) 0.6069(3) 0.3460(3) 0.0287(8) Uani 1 1 d . . . . .
H2A H 1.3240 0.6707 0.2874 0.034 Uiso 1 1 calc R U . . .
H2B H 1.3917 0.5512 0.3328 0.034 Uiso 1 1 calc R U . . .
C3 C 1.6506(4) 0.7787(3) 0.2309(3) 0.0332(9) Uani 1 1 d . . . . .
N3 N 1.7952(3) 0.6612(3) 0.1595(2) 0.0339(7) Uani 1 1 d . . . . .
C4 C 1.2026(3) 0.7469(3) 0.4539(3) 0.0280(8) Uani 1 1 d . . . . .
H4A H 1.2028 0.7773 0.5090 0.034 Uiso 1 1 calc R U . . .
H4B H 1.2088 0.8117 0.3960 0.034 Uiso 1 1 calc R U . . .
O12 O 1.9087(4) 0.3821(3) 0.0975(2) 0.0615(10) Uani 1 1 d . . . . .
C5 C 1.7423(4) 0.6912(3) 0.2471(3) 0.0314(9) Uani 1 1 d . . . . .
H5 H 1.7638 0.6592 0.3060 0.038 Uiso 1 1 calc R U . . .
C6 C 1.2820(4) 1.2079(3) 0.1481(3) 0.0325(9) Uani 1 1 d . . . . .
H6A H 1.3521 1.1893 0.1754 0.039 Uiso 1 1 calc R U . . .
H6B H 1.3136 1.2029 0.0792 0.039 Uiso 1 1 calc R U . . .
C7 C 1.2533(4) 1.0863(3) 0.3644(3) 0.0348(9) Uani 1 1 d . . . . .
H7A H 1.2961 1.1554 0.3433 0.042 Uiso 1 1 calc R U . . .
H7B H 1.3129 1.0212 0.3455 0.042 Uiso 1 1 calc R U . . .
C8 C 1.3614(4) 0.8615(3) 0.0698(3) 0.0350(9) Uani 1 1 d . . . . .
H8A H 1.4402 0.8572 0.0827 0.042 Uiso 1 1 calc R U . . .
H8B H 1.3169 0.7995 0.1185 0.042 Uiso 1 1 calc R U . . .
C9 C 1.3093(3) 0.5543(3) 0.5261(3) 0.0285(8) Uani 1 1 d . . . . .
H9A H 1.3823 0.4981 0.5130 0.034 Uiso 1 1 calc R U . . .
H9B H 1.3104 0.5851 0.5807 0.034 Uiso 1 1 calc R U . . .
C10 C 1.4344(4) 0.7081(3) 0.4120(3) 0.0320(9) Uani 1 1 d . . . . .
H10A H 1.4380 0.7270 0.4715 0.038 Uiso 1 1 calc R U . . .
H10B H 1.5050 0.6515 0.3927 0.038 Uiso 1 1 calc R U . . .
C11 C 1.2292(4) 1.3329(3) 0.1507(3) 0.0372(9) Uani 1 1 d . . . . .
H11A H 1.1641 1.3561 0.1177 0.045 Uiso 1 1 calc R U . . .
H11B H 1.1933 1.3393 0.2191 0.045 Uiso 1 1 calc R U . . .
O13 O 1.7248(4) 0.4548(3) 0.1878(3) 0.0610(9) Uani 1 1 d . . . . .
C12 C 1.0830(4) 1.1452(3) 0.1631(3) 0.0370(9) Uani 1 1 d . . . . .
H12A H 1.0394 1.2188 0.1785 0.044 Uiso 1 1 calc R U . . .
H12B H 1.1111 1.1572 0.0914 0.044 Uiso 1 1 calc R U . . .
C13 C 1.2640(4) 0.9967(3) 0.1844(3) 0.0333(9) Uani 1 1 d . . . . .
H13A H 1.3431 0.9868 0.1984 0.040 Uiso 1 1 calc R U . . .
H13B H 1.2169 0.9354 0.2315 0.040 Uiso 1 1 calc R U . . .
C14 C 1.3844(4) 0.8424(4) -0.0327(3) 0.0444(11) Uani 1 1 d . . . . .
H14A H 1.4206 0.9077 -0.0815 0.067 Uiso 1 1 calc R U . . .
H14B H 1.3074 0.8352 -0.0423 0.067 Uiso 1 1 calc R U . . .
H14C H 1.4398 0.7719 -0.0396 0.067 Uiso 1 1 calc R U . . .
C15 C 1.5602(4) 0.8488(3) 0.2991(3) 0.0341(9) Uani 1 1 d . . . . .
H15A H 1.5907 0.8425 0.3554 0.041 Uiso 1 1 calc R U . . .
H15B H 1.5544 0.9307 0.2644 0.041 Uiso 1 1 calc R U . . .
C16 C 1.1521(4) 1.1068(3) 0.3139(3) 0.0332(9) Uani 1 1 d . . . . .
H16A H 1.1011 1.1793 0.3250 0.040 Uiso 1 1 calc R U . . .
H16B H 1.1002 1.0440 0.3454 0.040 Uiso 1 1 calc R U . . .
N4 N 1.6489(3) 0.7982(3) 0.1350(3) 0.0445(9) Uani 1 1 d . . . . .
C17 C 1.8441(4) 0.4579(4) 0.1370(3) 0.0433(11) Uani 1 1 d . . . . .
C18 C 1.1975(4) 1.0590(3) 0.4774(3) 0.0425(11) Uani 1 1 d . . . . .
H18A H 1.1391 1.1249 0.4960 0.051 Uiso 1 1 calc R U . . .
H18B H 1.1528 0.9911 0.4979 0.051 Uiso 1 1 calc R U . . .
C19 C 1.2875(4) 0.9790(3) 0.0814(3) 0.0366(9) Uani 1 1 d . . . . .
H19A H 1.3324 1.0411 0.0333 0.044 Uiso 1 1 calc R U . . .
H19B H 1.2090 0.9837 0.0679 0.044 Uiso 1 1 calc R U . . .
C20 C 0.9940(5) 1.0550(4) 0.2037(4) 0.0527(12) Uani 1 1 d . . . . .
H20A H 0.9380 1.0667 0.2668 0.063 Uiso 1 1 calc R U . . .
H20B H 1.0393 0.9774 0.2150 0.063 Uiso 1 1 calc R U . . .
C21 C 1.2968(5) 1.0352(4) 0.5303(3) 0.0580(14) Uani 1 1 d . . . . .
H21A H 1.3563 0.9718 0.5102 0.087 Uiso 1 1 calc R U . . .
H21B H 1.2598 1.0145 0.6007 0.087 Uiso 1 1 calc R U . . .
H21C H 1.3374 1.1042 0.5136 0.087 Uiso 1 1 calc R U . . .
C22 C 1.3285(5) 1.4131(4) 0.1000(4) 0.0494(11) Uani 1 1 d . . . . .
H22A H 1.3633 1.4065 0.0316 0.059 Uiso 1 1 calc R U . . .
H22B H 1.3942 1.3878 0.1322 0.059 Uiso 1 1 calc R U . . .
C23 C 1.8912(4) 0.5688(4) 0.1325(3) 0.0391(10) Uani 1 1 d . . . . .
H23A H 1.9437 0.5508 0.1764 0.047 Uiso 1 1 calc R U . . .
H23B H 1.9420 0.5969 0.0655 0.047 Uiso 1 1 calc R U . . .
C24 C 0.9193(6) 1.0635(5) 0.1313(5) 0.0752(18) Uani 1 1 d . . . . .
H24A H 0.8656 1.1371 0.1273 0.090 Uiso 1 1 calc R U . . .
H24B H 0.9756 1.0634 0.0658 0.090 Uiso 1 1 calc R U . . .
C25 C 0.8449(6) 0.9679(5) 0.1612(5) 0.085(2) Uani 1 1 d . . . . .
H25A H 0.7996 0.9769 0.1141 0.127 Uiso 1 1 calc R U . . .
H25B H 0.7880 0.9684 0.2256 0.127 Uiso 1 1 calc R U . . .
H25C H 0.8978 0.8949 0.1639 0.127 Uiso 1 1 calc R U . . .
C26 C 1.6499(9) 0.3663(8) 0.1874(7) 0.042(2) Uiso 0.5 1 d . . P A 2
H26A H 1.6032 0.4021 0.1396 0.050 Uiso 0.5 1 calc R U P A 2
H26B H 1.7066 0.3022 0.1635 0.050 Uiso 0.5 1 calc R U P A 2
C27 C 1.5780(13) 0.3250(12) 0.2654(11) 0.088(4) Uiso 0.5 1 d . . P A 2
H27A H 1.6028 0.3342 0.3195 0.133 Uiso 0.5 1 calc R U P A 2
H27B H 1.5779 0.2432 0.2705 0.133 Uiso 0.5 1 calc R U P A 2
H27C H 1.4963 0.3649 0.2678 0.133 Uiso 0.5 1 calc R U P A 2
C28 C 1.7041(13) 0.3264(12) 0.2097(10) 0.080(4) Uiso 0.5 1 d . . P A 1
H28A H 1.6659 0.3230 0.1602 0.097 Uiso 0.5 1 calc R U P A 1
H28B H 1.7865 0.2847 0.1925 0.097 Uiso 0.5 1 calc R U P A 1
C29 C 1.6516(9) 0.2677(8) 0.2820(7) 0.046(2) Uiso 0.5 1 d . . P A 1
H29A H 1.6058 0.2194 0.2667 0.070 Uiso 0.5 1 calc R U P A 1
H29B H 1.5955 0.3158 0.3240 0.070 Uiso 0.5 1 calc R U P A 1
H29C H 1.7096 0.2189 0.3155 0.070 Uiso 0.5 1 calc R U P A 1
C30 C 1.2816(5) 1.5410(4) 0.1015(4) 0.0549(13) Uani 1 1 d . . . . .
H30A H 1.2250 1.5699 0.0617 0.082 Uiso 1 1 calc R U . . .
H30B H 1.3503 1.5864 0.0752 0.082 Uiso 1 1 calc R U . . .
H30C H 1.2400 1.5474 0.1685 0.082 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 O8 1.611(2) . ?
V1 O7 1.768(2) . ?
V1 O4 1.875(2) . ?
V1 O3 1.988(2) . ?
V1 O2 2.045(2) . ?
V1 O1 2.2324(6) . ?
V1 V3 3.0236(10) . ?
V1 V2 3.0368(9) . ?
V2 O9 1.601(2) . ?
V2 O5 1.760(3) . ?
V2 O7 1.893(2) . ?
V2 O2 1.981(2) 2_766 ?
V2 O6 2.060(2) . ?
V2 O1 2.2447(6) . ?
V2 V3 3.0347(10) 2_766 ?
V3 O10 1.602(3) . ?
V3 O4 1.769(2) . ?
V3 O5 1.893(2) 2_766 ?
V3 O6 1.972(2) . ?
V3 O3 2.051(2) 2_766 ?
V3 O1 2.2468(7) . ?
V3 V2 3.0347(9) 2_766 ?
O1 V1 2.2325(6) 2_766 ?
O1 V2 2.2447(6) 2_766 ?
O1 V3 2.2468(7) 2_766 ?
O2 C4 1.431(4) 2_766 ?
O2 V2 1.981(2) 2_766 ?
O3 C9 1.426(4) 2_766 ?
O3 V3 2.051(2) 2_766 ?
O5 V3 1.893(2) 2_766 ?
O6 C2 1.426(4) . ?
O11 C10 1.420(4) . ?
O11 C15 1.433(5) . ?
N1 C13 1.516(4) . ?
N1 C16 1.521(5) . ?
N1 C12 1.521(5) . ?
N1 C6 1.521(5) . ?
C1 C10 1.523(5) . ?
C1 C2 1.530(5) . ?
C1 C4 1.531(5) . ?
C1 C9 1.538(5) . ?
N2 N4 1.314(5) . ?
N2 N3 1.356(4) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 N4 1.360(5) . ?
C3 C5 1.361(5) . ?
C3 C15 1.496(5) . ?
N3 C5 1.345(5) . ?
N3 C23 1.443(5) . ?
C4 O2 1.431(4) 2_766 ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
O12 C17 1.209(5) . ?
C5 H5 0.9300 . ?
C6 C11 1.506(5) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C7 C16 1.511(5) . ?
C7 C18 1.533(5) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 C14 1.509(5) . ?
C8 C19 1.515(5) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C9 O3 1.426(4) 2_766 ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C11 C22 1.504(6) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
O13 C17 1.335(6) . ?
O13 C26 1.489(9) . ?
O13 C28 1.528(13) . ?
C12 C20 1.500(6) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C13 C19 1.509(5) . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C17 C23 1.503(6) . ?
C18 C21 1.513(6) . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C20 C24 1.530(7) . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C21 H21A 0.9600 . ?
C21 H21B 0.9600 . ?
C21 H21C 0.9600 . ?
C22 C30 1.524(6) . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
C23 H23A 0.9700 . ?
C23 H23B 0.9700 . ?
C24 C25 1.446(7) . ?
C24 H24A 0.9700 . ?
C24 H24B 0.9700 . ?
C25 H25A 0.9600 . ?
C25 H25B 0.9600 . ?
C25 H25C 0.9600 . ?
C26 C27 1.213(15) . ?
C26 H26A 0.9700 . ?
C26 H26B 0.9700 . ?
C27 H27A 0.9600 . ?
C27 H27B 0.9600 . ?
C27 H27C 0.9600 . ?
C28 C29 1.149(15) . ?
C28 H28A 0.9700 . ?
C28 H28B 0.9700 . ?
C29 H29A 0.9600 . ?
C29 H29B 0.9600 . ?
C29 H29C 0.9600 . ?
C30 H30A 0.9600 . ?
C30 H30B 0.9600 . ?
C30 H30C 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O8 V1 O7 104.27(12) . . ?
O8 V1 O4 102.81(12) . . ?
O7 V1 O4 94.68(11) . . ?
O8 V1 O3 97.47(12) . . ?
O7 V1 O3 90.40(10) . . ?
O4 V1 O3 157.14(10) . . ?
O8 V1 O2 95.71(11) . . ?
O7 V1 O2 159.57(10) . . ?
O4 V1 O2 84.83(10) . . ?
O3 V1 O2 82.74(9) . . ?
O8 V1 O1 171.91(10) . . ?
O7 V1 O1 82.67(8) . . ?
O4 V1 O1 80.45(7) . . ?
O3 V1 O1 78.12(7) . . ?
O2 V1 O1 77.09(7) . . ?
O8 V1 V3 135.57(10) . . ?
O7 V1 V3 87.15(8) . . ?
O4 V1 V3 32.83(7) . . ?
O3 V1 V3 125.68(7) . . ?
O2 V1 V3 81.40(7) . . ?
O1 V1 V3 47.744(16) . . ?
O8 V1 V2 139.13(9) . . ?
O7 V1 V2 35.29(8) . . ?
O4 V1 V2 89.83(7) . . ?
O3 V1 V2 81.52(7) . . ?
O2 V1 V2 124.33(7) . . ?
O1 V1 V2 47.461(16) . . ?
V3 V1 V2 66.24(2) . . ?
O9 V2 O5 105.03(12) . . ?
O9 V2 O7 103.05(12) . . ?
O5 V2 O7 93.05(11) . . ?
O9 V2 O2 97.89(11) . 2_766 ?
O5 V2 O2 92.02(10) . 2_766 ?
O7 V2 O2 156.35(10) . 2_766 ?
O9 V2 O6 96.00(12) . . ?
O5 V2 O6 158.82(10) . . ?
O7 V2 O6 84.55(10) . . ?
O2 V2 O6 82.43(10) 2_766 . ?
O9 V2 O1 171.57(10) . . ?
O5 V2 O1 82.64(8) . . ?
O7 V2 O1 79.69(7) . . ?
O2 V2 O1 78.08(7) 2_766 . ?
O6 V2 O1 76.23(7) . . ?
O9 V2 V3 139.78(10) . 2_766 ?
O5 V2 V3 35.25(8) . 2_766 ?
O7 V2 V3 88.86(8) . 2_766 ?
O2 V2 V3 82.07(7) 2_766 2_766 ?
O6 V2 V3 123.57(7) . 2_766 ?
O1 V2 V3 47.524(16) . 2_766 ?
O9 V2 V1 135.54(9) . . ?
O5 V2 V1 86.46(8) . . ?
O7 V2 V1 32.64(7) . . ?
O2 V2 V1 124.96(7) 2_766 . ?
O6 V2 V1 80.19(7) . . ?
O1 V2 V1 47.120(17) . . ?
V3 V2 V1 65.95(2) 2_766 . ?
O10 V3 O4 105.28(13) . . ?
O10 V3 O5 102.54(12) . 2_766 ?
O4 V3 O5 93.48(11) . 2_766 ?
O10 V3 O6 98.47(12) . . ?
O4 V3 O6 91.65(10) . . ?
O5 V3 O6 156.19(10) 2_766 . ?
O10 V3 O3 95.80(12) . 2_766 ?
O4 V3 O3 158.79(11) . 2_766 ?
O5 V3 O3 84.09(10) 2_766 2_766 ?
O6 V3 O3 82.78(9) . 2_766 ?
O10 V3 O1 171.82(10) . . ?
O4 V3 O1 82.28(8) . . ?
O5 V3 O1 79.78(7) 2_766 . ?
O6 V3 O1 77.90(7) . . ?
O3 V3 O1 76.55(7) 2_766 . ?
O10 V3 V1 139.91(10) . . ?
O4 V3 V1 35.06(8) . . ?
O5 V3 V1 89.14(8) 2_766 . ?
O6 V3 V1 81.82(7) . . ?
O3 V3 V1 123.73(7) 2_766 . ?
O1 V3 V1 47.343(18) . . ?
O10 V3 V2 134.91(10) . 2_766 ?
O4 V3 V2 86.01(8) . 2_766 ?
O5 V3 V2 32.44(7) 2_766 2_766 ?
O6 V3 V2 125.17(7) . 2_766 ?
O3 V3 V2 80.66(7) 2_766 2_766 ?
O1 V3 V2 47.466(17) . 2_766 ?
V1 V3 V2 65.78(2) . 2_766 ?
V1 O1 V1 180.0 . 2_766 ?
V1 O1 V2 94.58(2) . 2_766 ?
V1 O1 V2 85.42(2) 2_766 2_766 ?
V1 O1 V2 85.42(2) . . ?
V1 O1 V2 94.58(2) 2_766 . ?
V2 O1 V2 180.00(2) 2_766 . ?
V1 O1 V3 84.91(2) . . ?
V1 O1 V3 95.09(2) 2_766 . ?
V2 O1 V3 85.01(2) 2_766 . ?
V2 O1 V3 94.99(2) . . ?
V1 O1 V3 95.09(2) . 2_766 ?
V1 O1 V3 84.91(2) 2_766 2_766 ?
V2 O1 V3 94.99(2) 2_766 2_766 ?
V2 O1 V3 85.01(2) . 2_766 ?
V3 O1 V3 180.0 . 2_766 ?
C4 O2 V2 119.7(2) 2_766 2_766 ?
C4 O2 V1 117.94(19) 2_766 . ?
V2 O2 V1 109.62(11) 2_766 . ?
C9 O3 V1 119.3(2) 2_766 . ?
C9 O3 V3 117.3(2) 2_766 2_766 ?
V1 O3 V3 109.80(11) . 2_766 ?
V3 O4 V1 112.11(12) . . ?
V2 O5 V3 112.31(12) . 2_766 ?
C2 O6 V3 119.3(2) . . ?
C2 O6 V2 117.2(2) . . ?
V3 O6 V2 110.39(11) . . ?
V1 O7 V2 112.07(12) . . ?
C10 O11 C15 111.1(3) . . ?
C13 N1 C16 109.2(3) . . ?
C13 N1 C12 110.6(3) . . ?
C16 N1 C12 108.5(3) . . ?
C13 N1 C6 108.7(3) . . ?
C16 N1 C6 111.6(3) . . ?
C12 N1 C6 108.2(3) . . ?
C10 C1 C2 110.0(3) . . ?
C10 C1 C4 110.6(3) . . ?
C2 C1 C4 110.3(3) . . ?
C10 C1 C9 106.7(3) . . ?
C2 C1 C9 109.4(3) . . ?
C4 C1 C9 109.8(3) . . ?
N4 N2 N3 107.1(3) . . ?
O6 C2 C1 113.0(3) . . ?
O6 C2 H2A 109.0 . . ?
C1 C2 H2A 109.0 . . ?
O6 C2 H2B 109.0 . . ?
C1 C2 H2B 109.0 . . ?
H2A C2 H2B 107.8 . . ?
N4 C3 C5 108.7(3) . . ?
N4 C3 C15 120.6(3) . . ?
C5 C3 C15 130.7(4) . . ?
C5 N3 N2 110.4(3) . . ?
C5 N3 C23 130.8(3) . . ?
N2 N3 C23 118.6(3) . . ?
O2 C4 C1 112.3(3) 2_766 . ?
O2 C4 H4A 109.2 2_766 . ?
C1 C4 H4A 109.2 . . ?
O2 C4 H4B 109.2 2_766 . ?
C1 C4 H4B 109.2 . . ?
H4A C4 H4B 107.9 . . ?
N3 C5 C3 105.1(3) . . ?
N3 C5 H5 127.4 . . ?
C3 C5 H5 127.4 . . ?
C11 C6 N1 117.3(3) . . ?
C11 C6 H6A 108.0 . . ?
N1 C6 H6A 108.0 . . ?
C11 C6 H6B 108.0 . . ?
N1 C6 H6B 108.0 . . ?
H6A C6 H6B 107.2 . . ?
C16 C7 C18 110.0(3) . . ?
C16 C7 H7A 109.7 . . ?
C18 C7 H7A 109.7 . . ?
C16 C7 H7B 109.7 . . ?
C18 C7 H7B 109.7 . . ?
H7A C7 H7B 108.2 . . ?
C14 C8 C19 112.2(3) . . ?
C14 C8 H8A 109.2 . . ?
C19 C8 H8A 109.2 . . ?
C14 C8 H8B 109.2 . . ?
C19 C8 H8B 109.2 . . ?
H8A C8 H8B 107.9 . . ?
O3 C9 C1 112.9(3) 2_766 . ?
O3 C9 H9A 109.0 2_766 . ?
C1 C9 H9A 109.0 . . ?
O3 C9 H9B 109.0 2_766 . ?
C1 C9 H9B 109.0 . . ?
H9A C9 H9B 107.8 . . ?
O11 C10 C1 110.1(3) . . ?
O11 C10 H10A 109.6 . . ?
C1 C10 H10A 109.6 . . ?
O11 C10 H10B 109.6 . . ?
C1 C10 H10B 109.6 . . ?
H10A C10 H10B 108.2 . . ?
C22 C11 C6 110.5(4) . . ?
C22 C11 H11A 109.5 . . ?
C6 C11 H11A 109.5 . . ?
C22 C11 H11B 109.5 . . ?
C6 C11 H11B 109.5 . . ?
H11A C11 H11B 108.1 . . ?
C17 O13 C26 123.0(5) . . ?
C17 O13 C28 104.7(6) . . ?
C20 C12 N1 114.6(3) . . ?
C20 C12 H12A 108.6 . . ?
N1 C12 H12A 108.6 . . ?
C20 C12 H12B 108.6 . . ?
N1 C12 H12B 108.6 . . ?
H12A C12 H12B 107.6 . . ?
C19 C13 N1 116.1(3) . . ?
C19 C13 H13A 108.3 . . ?
N1 C13 H13A 108.3 . . ?
C19 C13 H13B 108.3 . . ?
N1 C13 H13B 108.3 . . ?
H13A C13 H13B 107.4 . . ?
C8 C14 H14A 109.5 . . ?
C8 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C8 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
O11 C15 C3 112.7(3) . . ?
O11 C15 H15A 109.1 . . ?
C3 C15 H15A 109.1 . . ?
O11 C15 H15B 109.1 . . ?
C3 C15 H15B 109.1 . . ?
H15A C15 H15B 107.8 . . ?
C7 C16 N1 115.7(3) . . ?
C7 C16 H16A 108.4 . . ?
N1 C16 H16A 108.4 . . ?
C7 C16 H16B 108.4 . . ?
N1 C16 H16B 108.4 . . ?
H16A C16 H16B 107.4 . . ?
N2 N4 C3 108.6(3) . . ?
O12 C17 O13 125.1(5) . . ?
O12 C17 C23 122.5(4) . . ?
O13 C17 C23 112.5(4) . . ?
C21 C18 C7 111.3(4) . . ?
C21 C18 H18A 109.4 . . ?
C7 C18 H18A 109.4 . . ?
C21 C18 H18B 109.4 . . ?
C7 C18 H18B 109.4 . . ?
H18A C18 H18B 108.0 . . ?
C13 C19 C8 111.7(3) . . ?
C13 C19 H19A 109.3 . . ?
C8 C19 H19A 109.3 . . ?
C13 C19 H19B 109.3 . . ?
C8 C19 H19B 109.3 . . ?
H19A C19 H19B 107.9 . . ?
C12 C20 C24 110.7(4) . . ?
C12 C20 H20A 109.5 . . ?
C24 C20 H20A 109.5 . . ?
C12 C20 H20B 109.5 . . ?
C24 C20 H20B 109.5 . . ?
H20A C20 H20B 108.1 . . ?
C18 C21 H21A 109.5 . . ?
C18 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C18 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C11 C22 C30 113.2(4) . . ?
C11 C22 H22A 108.9 . . ?
C30 C22 H22A 108.9 . . ?
C11 C22 H22B 108.9 . . ?
C30 C22 H22B 108.9 . . ?
H22A C22 H22B 107.7 . . ?
N3 C23 C17 114.3(4) . . ?
N3 C23 H23A 108.7 . . ?
C17 C23 H23A 108.7 . . ?
N3 C23 H23B 108.7 . . ?
C17 C23 H23B 108.7 . . ?
H23A C23 H23B 107.6 . . ?
C25 C24 C20 112.3(5) . . ?
C25 C24 H24A 109.2 . . ?
C20 C24 H24A 109.2 . . ?
C25 C24 H24B 109.2 . . ?
C20 C24 H24B 109.2 . . ?
H24A C24 H24B 107.9 . . ?
C24 C25 H25A 109.5 . . ?
C24 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C24 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C27 C26 O13 117.5(10) . . ?
C27 C26 H26A 107.9 . . ?
O13 C26 H26A 107.9 . . ?
C27 C26 H26B 107.9 . . ?
O13 C26 H26B 107.9 . . ?
H26A C26 H26B 107.2 . . ?
C26 C27 H27A 109.5 . . ?
C26 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C26 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C29 C28 O13 129.7(12) . . ?
C29 C28 H28A 104.9 . . ?
O13 C28 H28A 104.9 . . ?
C29 C28 H28B 104.9 . . ?
O13 C28 H28B 104.9 . . ?
H28A C28 H28B 105.8 . . ?
C28 C29 H29A 109.5 . . ?
C28 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C28 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C22 C30 H30A 109.5 . . ?
C22 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C22 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?

_refine_diff_density_max         0.811
_refine_diff_density_min         -0.544
_refine_diff_density_rms         0.100

