# Supplementary Material (ESI) for Chemical Communications
# This journal is (c) The Royal Society of Chemistry 2011

data_global
_journal_name_full               Chem.Commun.

_journal_coden_Cambridge         0182

_publ_contact_author_name        'Wei, Yongge'
_publ_contact_author_email       yonggewei@mail.tsinghua.edu.cn

_publ_section_title              
;
DMAP-catalyzed esterification of pentaerythritol-derivatized POMs:
a new route for the functionalization of polyoxometalates
;
_publ_contact_author_address     
;
Department of Chemistry
Tsinghua University
Beijing 100084
P. R. China
;
_publ_author_name                'Yongge Wei'

# Attachment '- c18.cif'

data_c18
_database_code_depnum_ccdc_archive 'CCDC 805404'
#TrackingRef '- c18.cif'

_database_code_CSD               ?

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C78 H158 N2 O23 V6'
_chemical_formula_weight         1797.70

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'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   P-1

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.528(2)
_cell_length_b                   12.074(2)
_cell_length_c                   19.371(4)
_cell_angle_alpha                94.67(3)
_cell_angle_beta                 99.95(3)
_cell_angle_gamma                115.39(3)
_cell_volume                     2362.1(8)
_cell_formula_units_Z            1
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       platelet
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.1
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.264
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             962
_exptl_absorpt_coefficient_mu    0.634
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.827
_exptl_absorpt_correction_T_max  0.939
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      293(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  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            23324
_diffrn_reflns_av_R_equivalents  0.1004
_diffrn_reflns_av_sigmaI/netI    0.1545
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         3.08
_diffrn_reflns_theta_max         27.48
_reflns_number_total             10660
_reflns_number_gt                3676
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0076P)^2^+2.8000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         10660
_refine_ls_number_parameters     493
_refine_ls_number_restraints     32
_refine_ls_R_factor_all          0.2273
_refine_ls_R_factor_gt           0.0709
_refine_ls_wR_factor_ref         0.1345
_refine_ls_wR_factor_gt          0.0917
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_restrained_S_all      1.017
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
V2 V 0.99617(9) -1.32215(8) -0.46219(5) 0.0607(3) Uani 1 1 d . . .
V3 V 0.83250(8) -1.62013(8) -0.45296(5) 0.0595(3) Uani 1 1 d . . .
O7 O 0.8681(3) -1.3727(3) -0.54340(17) 0.0580(9) Uani 1 1 d . . .
O1 O 1.0000 -1.5000 -0.5000 0.0512(12) Uani 1 2 d S . .
O10 O 0.9961(3) -1.1984(3) -0.42408(19) 0.0701(11) Uani 1 1 d . . .
O6 O 0.7366(3) -1.6146(3) -0.53610(17) 0.0589(9) Uani 1 1 d . . .
O5 O 1.1313(3) -1.2591(3) -0.50747(18) 0.0628(10) Uani 1 1 d . . .
O4 O 0.8614(3) -1.4471(3) -0.4175(2) 0.0581(9) Uani 1 1 d . . .
O3 O 0.9943(3) -1.5722(3) -0.37397(19) 0.0576(9) Uani 1 1 d . . .
O2 O 1.1256(3) -1.3321(3) -0.38147(19) 0.0580(9) Uani 1 1 d . . .
O9 O 0.7240(3) -1.6939(3) -0.40967(19) 0.0688(10) Uani 1 1 d . . .
O8 O 1.2628(3) -1.4583(3) -0.33492(19) 0.0760(11) Uani 1 1 d . . .
N1 N 0.6721(4) 0.8574(4) 0.4616(2) 0.0551(11) Uani 1 1 d . . .
C101 C 0.5910(5) 0.7676(4) 0.5050(3) 0.0585(14) Uani 1 1 d . . .
H10D H 0.5056 0.7116 0.4744 0.070 Uiso 1 1 calc R . .
H10E H 0.5763 0.8148 0.5425 0.070 Uiso 1 1 calc R . .
C4 C 0.9898(5) -1.5323(5) -0.3034(3) 0.0690(16) Uani 1 1 d . . .
H4A H 1.0656 -1.5278 -0.2701 0.083 Uiso 1 1 calc R . .
H4B H 0.9110 -1.5937 -0.2921 0.083 Uiso 1 1 calc R . .
C122 C 0.5595(5) 0.7028(5) 0.3443(3) 0.0721(17) Uani 1 1 d . . .
H12D H 0.5066 0.6332 0.3651 0.087 Uiso 1 1 calc R . .
H12E H 0.5098 0.7489 0.3325 0.087 Uiso 1 1 calc R . .
C102 C 0.6531(5) 0.6900(4) 0.5386(3) 0.0619(15) Uani 1 1 d . . .
H10F H 0.6579 0.6341 0.5016 0.074 Uiso 1 1 calc R . .
H10G H 0.7422 0.7445 0.5657 0.074 Uiso 1 1 calc R . .
C103 C 0.5717(5) 0.6151(5) 0.5873(3) 0.0724(17) Uani 1 1 d . . .
H10H H 0.4792 0.5766 0.5630 0.087 Uiso 1 1 calc R . .
H10I H 0.5957 0.5489 0.5964 0.087 Uiso 1 1 calc R . .
C3 C 1.1138(5) -1.3067(5) -0.3105(3) 0.0703(16) Uani 1 1 d . . .
H3A H 1.1131 -1.2266 -0.3031 0.084 Uiso 1 1 calc R . .
H3B H 1.1905 -1.3010 -0.2776 0.084 Uiso 1 1 calc R . .
C1 C 0.9894(5) -1.4055(5) -0.2937(3) 0.0670(16) Uani 1 1 d . . .
C2 C 0.8677(5) -1.4134(5) -0.3442(3) 0.0672(16) Uani 1 1 d . . .
H2A H 0.7894 -1.4741 -0.3321 0.081 Uiso 1 1 calc R . .
H2B H 0.8669 -1.3333 -0.3370 0.081 Uiso 1 1 calc R . .
C131 C 0.5978(5) 0.9313(4) 0.4381(3) 0.0587(14) Uani 1 1 d . . .
H13D H 0.5057 0.8732 0.4189 0.070 Uiso 1 1 calc R . .
H13E H 0.6024 0.9845 0.4798 0.070 Uiso 1 1 calc R . .
C121 C 0.6873(5) 0.7870(5) 0.3984(3) 0.0657(16) Uani 1 1 d . . .
H12F H 0.7290 0.7367 0.4157 0.079 Uiso 1 1 calc R . .
H12G H 0.7463 0.8468 0.3745 0.079 Uiso 1 1 calc R . .
C111 C 0.8100(5) 0.9448(4) 0.5053(3) 0.0592(15) Uani 1 1 d . . .
H11D H 0.8596 0.8973 0.5125 0.071 Uiso 1 1 calc R . .
H11E H 0.8529 1.0073 0.4776 0.071 Uiso 1 1 calc R . .
C104 C 0.5896(6) 0.6913(6) 0.6575(3) 0.091(2) Uani 1 1 d . . .
H10A H 0.5352 0.6387 0.6854 0.136 Uiso 1 1 calc R . .
H10B H 0.5645 0.7562 0.6490 0.136 Uiso 1 1 calc R . .
H10C H 0.6804 0.7277 0.6827 0.136 Uiso 1 1 calc R . .
C123 C 0.5854(7) 0.6541(6) 0.2772(3) 0.096(2) Uani 1 1 d . . .
H12H H 0.6285 0.6021 0.2884 0.116 Uiso 1 1 calc R . .
H12I H 0.6443 0.7236 0.2585 0.116 Uiso 1 1 calc R . .
C112 C 0.8188(5) 1.0109(5) 0.5774(3) 0.0645(15) Uani 1 1 d . . .
H11F H 0.7727 0.9502 0.6053 0.077 Uiso 1 1 calc R . .
H11G H 0.7769 1.0652 0.5712 0.077 Uiso 1 1 calc R . .
V1 V 1.16038(8) -1.47817(8) -0.40773(5) 0.0617(3) Uani 1 1 d . . .
C133 C 0.5536(6) 1.0672(5) 0.3579(3) 0.0756(17) Uani 1 1 d . . .
H13F H 0.5378 1.1044 0.3994 0.091 Uiso 1 1 calc R . .
H13G H 0.5964 1.1331 0.3321 0.091 Uiso 1 1 calc R . .
C113 C 0.9626(5) 1.0871(5) 0.6162(3) 0.0730(16) Uani 1 1 d . . .
H11H H 1.0045 1.0325 0.6206 0.088 Uiso 1 1 calc R . .
H11I H 1.0075 1.1484 0.5883 0.088 Uiso 1 1 calc R . .
C132 C 0.6471(5) 1.0119(5) 0.3829(3) 0.0664(16) Uani 1 1 d . . .
H13H H 0.6517 0.9620 0.3427 0.080 Uiso 1 1 calc R . .
H13I H 0.7350 1.0784 0.4035 0.080 Uiso 1 1 calc R . .
C134 C 0.4231(6) 0.9746(6) 0.3112(3) 0.097(2) Uani 1 1 d . . .
H13A H 0.3687 1.0152 0.2989 0.145 Uiso 1 1 calc R . .
H13B H 0.3800 0.9086 0.3361 0.145 Uiso 1 1 calc R . .
H13C H 0.4372 0.9408 0.2686 0.145 Uiso 1 1 calc R . .
C114 C 0.9778(6) 1.1527(6) 0.6895(3) 0.103(2) Uani 1 1 d . . .
H11A H 1.0699 1.2006 0.7117 0.154 Uiso 1 1 calc R . .
H11B H 0.9363 1.0922 0.7178 0.154 Uiso 1 1 calc R . .
H11C H 0.9369 1.2071 0.6854 0.154 Uiso 1 1 calc R . .
O11 O 0.9845(5) -1.2529(4) -0.2083(3) 0.1281(16) Uani 1 1 d U . .
C5 C 0.9860(7) -1.3713(6) -0.2168(3) 0.0987(19) Uani 1 1 d U . .
H5A H 0.9078 -1.4342 -0.2058 0.118 Uiso 1 1 calc R . .
H5B H 1.0630 -1.3668 -0.1847 0.118 Uiso 1 1 calc R . .
C124 C 0.4572(7) 0.5785(6) 0.2207(4) 0.125(3) Uani 1 1 d . . .
H12A H 0.4767 0.5494 0.1786 0.187 Uiso 1 1 calc R . .
H12B H 0.4148 0.6300 0.2093 0.187 Uiso 1 1 calc R . .
H12C H 0.3997 0.5085 0.2387 0.187 Uiso 1 1 calc R . .
C6 C 0.9342(9) -1.2186(8) -0.1649(5) 0.123(2) Uani 1 1 d U . .
O12 O 0.8966(9) -1.2820(6) -0.1250(4) 0.231(3) Uani 1 1 d U . .
C9 C 0.8830(8) -0.9282(7) -0.1175(4) 0.124(3) Uani 1 1 d . . .
H9A H 0.9712 -0.8686 -0.1193 0.148 Uiso 1 1 calc R . .
H9B H 0.8262 -0.9397 -0.1635 0.148 Uiso 1 1 calc R . .
C8 C 0.8871(8) -1.0473(7) -0.1124(4) 0.126(3) Uani 1 1 d . . .
H8A H 0.9421 -1.0374 -0.0661 0.151 Uiso 1 1 calc R . .
H8B H 0.7985 -1.1084 -0.1124 0.151 Uiso 1 1 calc R . .
C7 C 0.9321(8) -1.1004(7) -0.1638(4) 0.131(2) Uani 1 1 d U . .
H7A H 1.0218 -1.0397 -0.1618 0.158 Uiso 1 1 calc R . .
H7B H 0.8800 -1.1049 -0.2099 0.158 Uiso 1 1 calc R . .
C13 C 0.7889(9) -0.5739(8) -0.0290(5) 0.145(3) Uani 1 1 d . . .
H13J H 0.8770 -0.5143 -0.0309 0.174 Uiso 1 1 calc R . .
H13K H 0.7323 -0.5860 -0.0751 0.174 Uiso 1 1 calc R . .
C11 C 0.8360(8) -0.7505(8) -0.0746(4) 0.135(3) Uani 1 1 d . . .
H11J H 0.9237 -0.6907 -0.0770 0.162 Uiso 1 1 calc R . .
H11K H 0.7785 -0.7650 -0.1207 0.162 Uiso 1 1 calc R . .
C17 C 0.6958(9) -0.2193(9) 0.0582(5) 0.155(4) Uani 1 1 d . . .
H17A H 0.7857 -0.1605 0.0589 0.185 Uiso 1 1 calc R . .
H17B H 0.6445 -0.2307 0.0106 0.185 Uiso 1 1 calc R . .
C21 C 0.5916(9) 0.1362(9) 0.1286(4) 0.143(3) Uani 1 1 d . . .
H21A H 0.6831 0.1984 0.1385 0.172 Uiso 1 1 calc R . .
H21B H 0.5559 0.1288 0.0784 0.172 Uiso 1 1 calc R . .
C15 C 0.7418(9) -0.3969(9) 0.0156(5) 0.154(3) Uani 1 1 d . . .
H15A H 0.8301 -0.3368 0.0142 0.184 Uiso 1 1 calc R . .
H15B H 0.6864 -0.4096 -0.0311 0.184 Uiso 1 1 calc R . .
C19 C 0.6479(9) -0.0411(9) 0.0968(5) 0.150(4) Uani 1 1 d . . .
H19A H 0.6044 -0.0510 0.0475 0.180 Uiso 1 1 calc R . .
H19B H 0.7392 0.0189 0.1018 0.180 Uiso 1 1 calc R . .
C10 C 0.8418(9) -0.8679(8) -0.0660(5) 0.148(3) Uani 1 1 d . . .
H10J H 0.9003 -0.8532 -0.0201 0.178 Uiso 1 1 calc R . .
H10K H 0.7545 -0.9276 -0.0630 0.178 Uiso 1 1 calc R . .
C22 C 0.5268(10) 0.1898(10) 0.1654(6) 0.180(4) Uani 1 1 d . . .
H22A H 0.5593 0.1942 0.2157 0.216 Uiso 1 1 calc R . .
H22B H 0.4343 0.1298 0.1537 0.216 Uiso 1 1 calc R . .
C20 C 0.5945(10) 0.0211(10) 0.1367(6) 0.168(4) Uani 1 1 d . . .
H20A H 0.6386 0.0322 0.1860 0.202 Uiso 1 1 calc R . .
H20B H 0.5033 -0.0388 0.1322 0.202 Uiso 1 1 calc R . .
C16 C 0.6988(10) -0.3355(9) 0.0640(6) 0.170(4) Uani 1 1 d . . .
H16A H 0.7530 -0.3241 0.1108 0.204 Uiso 1 1 calc R . .
H16B H 0.6097 -0.3946 0.0646 0.204 Uiso 1 1 calc R . .
C14 C 0.7478(10) -0.5121(9) 0.0211(5) 0.169(4) Uani 1 1 d . . .
H14A H 0.6601 -0.5720 0.0235 0.203 Uiso 1 1 calc R . .
H14B H 0.8050 -0.4991 0.0672 0.203 Uiso 1 1 calc R . .
C18 C 0.6510(10) -0.1556(10) 0.1034(6) 0.172(4) Uani 1 1 d . . .
H18A H 0.5613 -0.2144 0.1030 0.207 Uiso 1 1 calc R . .
H18B H 0.7027 -0.1434 0.1510 0.207 Uiso 1 1 calc R . .
C12 C 0.7938(10) -0.6902(9) -0.0240(5) 0.171(4) Uani 1 1 d . . .
H12J H 0.7056 -0.7502 -0.0225 0.205 Uiso 1 1 calc R . .
H12K H 0.8500 -0.6784 0.0222 0.205 Uiso 1 1 calc R . .
C23 C 0.5305(10) 0.3078(9) 0.1580(5) 0.187(4) Uani 1 1 d . . .
H23A H 0.4808 0.3254 0.1884 0.280 Uiso 1 1 calc R . .
H23B H 0.4928 0.3060 0.1094 0.280 Uiso 1 1 calc R . .
H23C H 0.6203 0.3713 0.1711 0.280 Uiso 1 1 calc R . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
V2 0.0495(6) 0.0478(6) 0.0959(8) 0.0207(5) 0.0249(5) 0.0277(5)
V3 0.0365(5) 0.0512(6) 0.0941(8) 0.0200(5) 0.0233(5) 0.0186(5)
O7 0.044(2) 0.056(2) 0.088(3) 0.0233(19) 0.0209(19) 0.0321(18)
O1 0.035(3) 0.046(3) 0.080(3) 0.014(2) 0.016(2) 0.023(2)
O10 0.070(3) 0.042(2) 0.115(3) 0.015(2) 0.035(2) 0.035(2)
O6 0.036(2) 0.055(2) 0.086(3) 0.0177(19) 0.0179(18) 0.0180(18)
O5 0.050(2) 0.045(2) 0.102(3) 0.024(2) 0.031(2) 0.0223(18)
O4 0.048(2) 0.054(2) 0.084(3) 0.014(2) 0.0237(19) 0.0305(19)
O3 0.046(2) 0.055(2) 0.083(3) 0.022(2) 0.0251(19) 0.0276(18)
O2 0.042(2) 0.050(2) 0.081(3) 0.0124(19) 0.0201(19) 0.0180(18)
O9 0.041(2) 0.064(2) 0.106(3) 0.035(2) 0.034(2) 0.0176(19)
O8 0.047(2) 0.093(3) 0.091(3) 0.025(2) 0.003(2) 0.037(2)
N1 0.037(3) 0.052(3) 0.087(3) 0.019(2) 0.023(2) 0.026(2)
C101 0.037(3) 0.055(3) 0.091(4) 0.021(3) 0.024(3) 0.022(3)
C4 0.053(4) 0.066(4) 0.097(5) 0.029(4) 0.023(3) 0.030(3)
C122 0.066(4) 0.055(4) 0.096(5) 0.016(3) 0.021(4) 0.026(3)
C102 0.049(3) 0.052(3) 0.096(4) 0.021(3) 0.027(3) 0.027(3)
C103 0.050(4) 0.058(4) 0.115(5) 0.034(4) 0.023(4) 0.026(3)
C3 0.053(4) 0.064(4) 0.093(5) 0.010(4) 0.014(3) 0.027(3)
C1 0.048(4) 0.057(4) 0.098(5) 0.022(3) 0.023(3) 0.022(3)
C2 0.050(4) 0.047(3) 0.111(5) 0.014(3) 0.029(3) 0.024(3)
C131 0.053(3) 0.056(3) 0.084(4) 0.015(3) 0.022(3) 0.037(3)
C121 0.054(4) 0.066(4) 0.095(5) 0.024(3) 0.032(3) 0.037(3)
C111 0.041(3) 0.051(3) 0.089(4) 0.022(3) 0.023(3) 0.019(3)
C104 0.087(5) 0.096(5) 0.112(6) 0.040(4) 0.042(4) 0.052(4)
C123 0.094(6) 0.091(5) 0.101(6) 0.005(4) 0.014(5) 0.045(5)
C112 0.051(4) 0.055(3) 0.093(5) 0.018(3) 0.030(3) 0.023(3)
V1 0.0396(6) 0.0621(6) 0.0921(8) 0.0197(5) 0.0165(5) 0.0292(5)
C133 0.078(5) 0.070(4) 0.096(5) 0.025(4) 0.021(4) 0.047(4)
C113 0.062(4) 0.067(4) 0.088(5) 0.015(3) 0.015(3) 0.029(3)
C132 0.050(4) 0.060(4) 0.094(4) 0.021(3) 0.020(3) 0.026(3)
C134 0.064(5) 0.111(5) 0.117(6) 0.041(5) 0.013(4) 0.041(4)
C114 0.101(6) 0.088(5) 0.103(6) 0.001(4) 0.017(4) 0.033(4)
O11 0.171(4) 0.093(3) 0.140(4) 0.007(3) 0.087(3) 0.061(3)
C5 0.120(5) 0.093(4) 0.100(5) 0.016(4) 0.051(4) 0.053(4)
C124 0.140(8) 0.112(6) 0.105(6) -0.006(5) 0.006(5) 0.055(6)
C6 0.173(5) 0.119(5) 0.133(5) 0.043(4) 0.095(4) 0.089(4)
O12 0.381(9) 0.169(6) 0.263(8) 0.105(5) 0.236(7) 0.162(6)
C9 0.148(8) 0.102(6) 0.109(6) -0.016(5) 0.046(5) 0.045(6)
C8 0.128(7) 0.109(6) 0.161(8) 0.018(6) 0.060(6) 0.063(6)
C7 0.177(7) 0.109(5) 0.134(6) 0.007(4) 0.076(5) 0.076(5)
C13 0.156(9) 0.130(8) 0.149(8) -0.012(6) 0.051(6) 0.066(7)
C11 0.147(8) 0.114(7) 0.141(8) -0.007(6) 0.039(6) 0.059(6)
C17 0.161(9) 0.146(9) 0.158(9) -0.014(7) 0.052(7) 0.072(8)
C21 0.145(9) 0.161(9) 0.122(7) -0.016(7) 0.026(6) 0.076(8)
C15 0.147(9) 0.134(8) 0.171(9) -0.013(7) 0.055(7) 0.055(7)
C19 0.142(9) 0.145(9) 0.148(8) -0.034(7) 0.029(6) 0.063(7)
C10 0.158(9) 0.141(8) 0.178(9) 0.024(7) 0.070(7) 0.086(7)
C22 0.186(11) 0.164(10) 0.237(13) 0.068(9) 0.071(9) 0.108(9)
C20 0.162(10) 0.155(9) 0.224(12) 0.051(9) 0.071(8) 0.091(8)
C16 0.179(10) 0.157(9) 0.226(12) 0.048(9) 0.103(8) 0.100(9)
C14 0.186(10) 0.149(9) 0.225(12) 0.046(8) 0.112(8) 0.098(9)
C18 0.178(10) 0.154(9) 0.241(12) 0.055(9) 0.106(9) 0.100(9)
C12 0.171(10) 0.150(9) 0.235(12) 0.033(9) 0.096(8) 0.095(8)
C23 0.253(13) 0.178(10) 0.146(9) 0.017(8) 0.037(8) 0.118(10)

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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
V2 O10 1.612(3) . ?
V2 O7 1.815(3) . ?
V2 O5 1.827(3) . ?
V2 O2 2.016(3) . ?
V2 O4 2.027(4) . ?
V2 O1 2.2330(10) . ?
V2 V1 3.021(2) 2_724 ?
V2 V3 3.0339(15) 2_724 ?
V3 O9 1.609(3) . ?
V3 O6 1.813(3) . ?
V3 O5 1.828(3) 2_724 ?
V3 O4 2.009(3) . ?
V3 O3 2.025(4) . ?
V3 O1 2.2547(12) . ?
V3 V2 3.0339(15) 2_724 ?
V3 V1 3.0351(15) 2_724 ?
O7 V1 1.832(3) 2_724 ?
O1 V2 2.2330(10) 2_724 ?
O1 V1 2.2462(12) . ?
O1 V1 2.2462(12) 2_724 ?
O1 V3 2.2547(12) 2_724 ?
O6 V1 1.831(3) 2_724 ?
O5 V3 1.828(3) 2_724 ?
O4 C2 1.426(6) . ?
O3 C4 1.429(6) . ?
O3 V1 2.017(3) . ?
O2 C3 1.426(6) . ?
O2 V1 2.015(3) . ?
O8 V1 1.602(3) . ?
N1 C121 1.511(6) . ?
N1 C101 1.518(6) . ?
N1 C111 1.518(6) . ?
N1 C131 1.524(5) . ?
C101 C102 1.525(5) . ?
C4 C1 1.529(6) . ?
C122 C123 1.512(7) . ?
C122 C121 1.520(7) . ?
C102 C103 1.518(7) . ?
C103 C104 1.508(7) . ?
C3 C1 1.530(7) . ?
C1 C5 1.525(7) . ?
C1 C2 1.526(7) . ?
C131 C132 1.522(6) . ?
C111 C112 1.516(6) . ?
C123 C124 1.528(8) . ?
C112 C113 1.520(7) . ?
V1 O6 1.831(3) 2_724 ?
V1 O7 1.832(3) 2_724 ?
V1 V2 3.021(2) 2_724 ?
V1 V3 3.0351(15) 2_724 ?
C133 C134 1.502(7) . ?
C133 C132 1.527(6) . ?
C113 C114 1.511(7) . ?
O11 C6 1.237(8) . ?
O11 C5 1.434(6) . ?
C6 O12 1.139(8) . ?
C6 C7 1.436(9) . ?
C9 C10 1.447(9) . ?
C9 C8 1.470(8) . ?
C8 C7 1.425(8) . ?
C13 C14 1.437(10) . ?
C13 C12 1.440(9) . ?
C11 C12 1.442(9) . ?
C11 C10 1.468(9) . ?
C17 C18 1.419(10) . ?
C17 C16 1.431(10) . ?
C21 C22 1.417(10) . ?
C21 C20 1.425(10) . ?
C15 C16 1.427(10) . ?
C15 C14 1.435(10) . ?
C19 C18 1.414(10) . ?
C19 C20 1.417(10) . ?
C22 C23 1.426(10) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O10 V2 O7 104.05(16) . . ?
O10 V2 O5 102.66(16) . . ?
O7 V2 O5 94.17(15) . . ?
O10 V2 O2 96.28(17) . . ?
O7 V2 O2 158.64(14) . . ?
O5 V2 O2 87.62(15) . . ?
O10 V2 O4 97.66(16) . . ?
O7 V2 O4 87.83(15) . . ?
O5 V2 O4 158.41(13) . . ?
O2 V2 O4 82.97(13) . . ?
O10 V2 O1 172.12(14) . . ?
O7 V2 O1 82.01(10) . . ?
O5 V2 O1 81.67(10) . . ?
O2 V2 O1 77.18(10) . . ?
O4 V2 O1 77.32(9) . . ?
O10 V2 V1 138.10(14) . 2_724 ?
O7 V2 V1 34.24(9) . 2_724 ?
O5 V2 V1 88.42(12) . 2_724 ?
O2 V2 V1 124.77(10) . 2_724 ?
O4 V2 V1 81.17(11) . 2_724 ?
O1 V2 V1 47.77(3) . 2_724 ?
O10 V2 V3 136.23(14) . 2_724 ?
O7 V2 V3 88.78(11) . 2_724 ?
O5 V2 V3 33.90(9) . 2_724 ?
O2 V2 V3 80.86(11) . 2_724 ?
O4 V2 V3 124.88(10) . 2_724 ?
O1 V2 V3 47.77(3) . 2_724 ?
V1 V2 V3 66.58(4) 2_724 2_724 ?
O9 V3 O6 104.35(16) . . ?
O9 V3 O5 103.18(16) . 2_724 ?
O6 V3 O5 94.26(15) . 2_724 ?
O9 V3 O4 97.93(16) . . ?
O6 V3 O4 87.79(15) . . ?
O5 V3 O4 157.55(15) 2_724 . ?
O9 V3 O3 97.25(16) . . ?
O6 V3 O3 157.37(14) . . ?
O5 V3 O3 87.22(15) 2_724 . ?
O4 V3 O3 82.57(14) . . ?
O9 V3 O1 172.53(14) . . ?
O6 V3 O1 81.26(11) . . ?
O5 V3 O1 81.06(11) 2_724 . ?
O4 V3 O1 77.16(10) . . ?
O3 V3 O1 76.66(10) . . ?
O9 V3 V2 136.82(13) . 2_724 ?
O6 V3 V2 88.10(11) . 2_724 ?
O5 V3 V2 33.89(10) 2_724 2_724 ?
O4 V3 V2 124.12(11) . 2_724 ?
O3 V3 V2 80.58(11) . 2_724 ?
O1 V3 V2 47.16(3) . 2_724 ?
O9 V3 V1 137.95(13) . 2_724 ?
O6 V3 V1 33.78(10) . 2_724 ?
O5 V3 V1 88.25(11) 2_724 2_724 ?
O4 V3 V1 81.06(11) . 2_724 ?
O3 V3 V1 123.94(10) . 2_724 ?
O1 V3 V1 47.48(3) . 2_724 ?
V2 V3 V1 66.04(4) 2_724 2_724 ?
V2 O7 V1 111.87(15) . 2_724 ?
V2 O1 V2 180.000(1) 2_724 . ?
V2 O1 V1 84.83(5) 2_724 . ?
V2 O1 V1 95.17(5) . . ?
V2 O1 V1 95.17(5) 2_724 2_724 ?
V2 O1 V1 84.83(5) . 2_724 ?
V1 O1 V1 180.000(1) . 2_724 ?
V2 O1 V3 85.07(4) 2_724 . ?
V2 O1 V3 94.93(4) . . ?
V1 O1 V3 95.19(4) . . ?
V1 O1 V3 84.81(4) 2_724 . ?
V2 O1 V3 94.93(4) 2_724 2_724 ?
V2 O1 V3 85.07(4) . 2_724 ?
V1 O1 V3 84.81(4) . 2_724 ?
V1 O1 V3 95.19(4) 2_724 2_724 ?
V3 O1 V3 180.00(5) . 2_724 ?
V3 O6 V1 112.81(16) . 2_724 ?
V2 O5 V3 112.21(16) . 2_724 ?
C2 O4 V3 118.6(3) . . ?
C2 O4 V2 117.6(3) . . ?
V3 O4 V2 110.03(17) . . ?
C4 O3 V1 118.5(3) . . ?
C4 O3 V3 117.8(3) . . ?
V1 O3 V3 110.61(17) . . ?
C3 O2 V1 118.0(3) . . ?
C3 O2 V2 118.3(3) . . ?
V1 O2 V2 110.26(17) . . ?
C121 N1 C101 110.5(4) . . ?
C121 N1 C111 107.2(4) . . ?
C101 N1 C111 111.6(4) . . ?
C121 N1 C131 111.4(4) . . ?
C101 N1 C131 106.1(3) . . ?
C111 N1 C131 110.2(4) . . ?
N1 C101 C102 114.9(4) . . ?
O3 C4 C1 113.0(4) . . ?
C123 C122 C121 111.6(5) . . ?
C103 C102 C101 110.2(4) . . ?
C104 C103 C102 113.7(5) . . ?
O2 C3 C1 113.5(5) . . ?
C5 C1 C2 110.0(5) . . ?
C5 C1 C4 108.7(5) . . ?
C2 C1 C4 109.1(5) . . ?
C5 C1 C3 109.8(5) . . ?
C2 C1 C3 109.4(4) . . ?
C4 C1 C3 109.8(4) . . ?
O4 C2 C1 113.9(4) . . ?
C132 C131 N1 115.8(4) . . ?
N1 C121 C122 115.1(4) . . ?
C112 C111 N1 116.3(4) . . ?
C122 C123 C124 111.3(6) . . ?
C111 C112 C113 109.7(4) . . ?
O8 V1 O6 104.36(17) . 2_724 ?
O8 V1 O7 104.00(17) . 2_724 ?
O6 V1 O7 94.13(15) 2_724 2_724 ?
O8 V1 O2 97.19(17) . . ?
O6 V1 O2 87.38(14) 2_724 . ?
O7 V1 O2 157.64(14) 2_724 . ?
O8 V1 O3 96.89(17) . . ?
O6 V1 O3 157.51(14) 2_724 . ?
O7 V1 O3 87.72(15) 2_724 . ?
O2 V1 O3 82.68(13) . . ?
O8 V1 O1 171.89(14) . . ?
O6 V1 O1 81.12(10) 2_724 . ?
O7 V1 O1 81.30(10) 2_724 . ?
O2 V1 O1 76.90(10) . . ?
O3 V1 O1 77.00(10) . . ?
O8 V1 V2 137.62(14) . 2_724 ?
O6 V1 V2 88.06(11) 2_724 2_724 ?
O7 V1 V2 33.89(9) 2_724 2_724 ?
O2 V1 V2 124.11(11) . 2_724 ?
O3 V1 V2 81.02(11) . 2_724 ?
O1 V1 V2 47.40(3) . 2_724 ?
O8 V1 V3 137.52(14) . 2_724 ?
O6 V1 V3 33.41(10) 2_724 2_724 ?
O7 V1 V3 88.17(11) 2_724 2_724 ?
O2 V1 V3 80.85(11) . 2_724 ?
O3 V1 V3 124.52(10) . 2_724 ?
O1 V1 V3 47.72(3) . 2_724 ?
V2 V1 V3 66.19(4) 2_724 2_724 ?
C134 C133 C132 114.1(4) . . ?
C114 C113 C112 112.2(5) . . ?
C131 C132 C133 109.8(4) . . ?
C6 O11 C5 124.9(6) . . ?
O11 C5 C1 108.4(5) . . ?
O12 C6 O11 116.9(9) . . ?
O12 C6 C7 123.0(9) . . ?
O11 C6 C7 120.0(8) . . ?
C10 C9 C8 123.3(7) . . ?
C7 C8 C9 120.7(7) . . ?
C8 C7 C6 124.6(7) . . ?
C14 C13 C12 124.8(9) . . ?
C12 C11 C10 121.7(8) . . ?
C18 C17 C16 127.1(9) . . ?
C22 C21 C20 125.7(10) . . ?
C16 C15 C14 125.3(9) . . ?
C18 C19 C20 128.5(10) . . ?
C9 C10 C11 121.2(8) . . ?
C21 C22 C23 124.1(10) . . ?
C19 C20 C21 127.5(10) . . ?
C15 C16 C17 124.5(9) . . ?
C15 C14 C13 124.5(9) . . ?
C19 C18 C17 126.5(9) . . ?
C13 C12 C11 124.0(9) . . ?

_diffrn_measured_fraction_theta_max 0.983
_diffrn_reflns_theta_full        27.48
_diffrn_measured_fraction_theta_full 0.983
_refine_diff_density_max         0.499
_refine_diff_density_min         -0.540
_refine_diff_density_rms         0.071


# Attachment '- c3.cif'

data_c3
_database_code_depnum_ccdc_archive 'CCDC 810985'
#TrackingRef '- c3.cif'

_database_code_CSD               ?
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C48 H98 N2 O23 V6'
_chemical_formula_weight         1376.92

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'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P2(1)/c

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

_cell_length_a                   11.135(2)
_cell_length_b                   14.900(3)
_cell_length_c                   19.855(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 97.63(3)
_cell_angle_gamma                90.00
_cell_volume                     3265.1(11)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.401
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1444
_exptl_absorpt_coefficient_mu    0.894
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.732
_exptl_absorpt_correction_T_max  0.836
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      293(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  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            31068
_diffrn_reflns_av_R_equivalents  0.0647
_diffrn_reflns_av_sigmaI/netI    0.0559
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         3.25
_diffrn_reflns_theta_max         27.48
_reflns_number_total             7439
_reflns_number_gt                4175
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0883P)^2^+1.3293P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.0079(11)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_number_reflns         7439
_refine_ls_number_parameters     359
_refine_ls_number_restraints     23
_refine_ls_R_factor_all          0.1157
_refine_ls_R_factor_gt           0.0576
_refine_ls_wR_factor_ref         0.1995
_refine_ls_wR_factor_gt          0.1409
_refine_ls_goodness_of_fit_ref   1.135
_refine_ls_restrained_S_all      1.135
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
V1 V 0.67572(7) 0.46241(5) -0.03622(4) 0.0505(3) Uani 1 1 d . . .
V2 V 0.52643(7) 0.64837(4) -0.01014(4) 0.0493(2) Uani 1 1 d . . .
V3 V 0.57393(7) 0.49493(5) 0.11072(3) 0.0484(2) Uani 1 1 d . . .
O1 O 0.6851(2) 0.59796(18) -0.03254(14) 0.0500(7) Uani 1 1 d . . .
O2 O 0.6030(2) 0.62499(18) 0.08622(13) 0.0466(7) Uani 1 1 d . . .
O3 O 0.6203(3) 0.35033(18) -0.02103(16) 0.0559(8) Uani 1 1 d . . .
O4 O 0.5000 0.5000 0.0000 0.0402(8) Uani 1 2 d S . .
O5 O 0.7237(3) 0.47522(18) 0.06509(14) 0.0496(7) Uani 1 1 d . . .
O6 O 0.5817(3) 0.47328(19) -0.11851(15) 0.0565(8) Uani 1 1 d . . .
O7 O 0.5386(3) 0.37687(19) 0.09736(14) 0.0545(7) Uani 1 1 d . . .
O8 O 0.5633(3) 0.75168(18) -0.01288(15) 0.0604(8) Uani 1 1 d . . .
O9 O 0.8093(3) 0.4453(2) -0.05486(17) 0.0654(9) Uani 1 1 d . . .
O10 O 0.6420(3) 0.4977(2) 0.18681(15) 0.0615(8) Uani 1 1 d . . .
O11 O 0.9302(3) 0.7626(2) 0.0870(2) 0.0817(11) Uani 1 1 d . . .
O12 O 1.0803(7) 0.7928(4) 0.1655(4) 0.200(4) Uani 1 1 d U . .
N1 N 0.3834(4) 0.8089(3) -0.23027(19) 0.0612(10) Uani 1 1 d . . .
C1 C 0.8199(4) 0.6242(3) 0.0734(2) 0.0498(10) Uani 1 1 d . . .
C2 C 0.8323(4) 0.5232(3) 0.0901(2) 0.0572(11) Uani 1 1 d . . .
H2A H 0.8997 0.4986 0.0698 0.069 Uiso 1 1 calc R . .
H2B H 0.8495 0.5154 0.1389 0.069 Uiso 1 1 calc R . .
C3 C 0.7961(4) 0.6391(3) -0.0032(2) 0.0558(11) Uani 1 1 d . . .
H3A H 0.7924 0.7030 -0.0124 0.067 Uiso 1 1 calc R . .
H3B H 0.8627 0.6143 -0.0241 0.067 Uiso 1 1 calc R . .
C4 C 0.7181(4) 0.6640(3) 0.1091(2) 0.0521(10) Uani 1 1 d . . .
H4A H 0.7371 0.6546 0.1577 0.062 Uiso 1 1 calc R . .
H4B H 0.7138 0.7282 0.1010 0.062 Uiso 1 1 calc R . .
C5 C 0.9405(4) 0.6678(3) 0.1021(3) 0.0619(12) Uani 1 1 d . . .
H5A H 0.9564 0.6585 0.1509 0.074 Uiso 1 1 calc R . .
H5B H 1.0064 0.6417 0.0814 0.074 Uiso 1 1 calc R . .
C6 C 1.0023(7) 0.8184(5) 0.1219(4) 0.103(2) Uani 1 1 d U . .
C7 C 0.9823(8) 0.9142(5) 0.1006(5) 0.136(3) Uani 1 1 d U . .
H7A H 0.9896 0.9506 0.1415 0.163 Uiso 1 1 calc R . .
H7B H 1.0479 0.9315 0.0757 0.163 Uiso 1 1 calc R . .
C8 C 0.8704(11) 0.9378(7) 0.0600(7) 0.213(6) Uani 1 1 d U . .
H8A H 0.8706 1.0008 0.0496 0.320 Uiso 1 1 calc R . .
H8B H 0.8039 0.9247 0.0846 0.320 Uiso 1 1 calc R . .
H8C H 0.8618 0.9039 0.0185 0.320 Uiso 1 1 calc R . .
C11 C 0.2847(5) 0.7594(3) -0.2007(2) 0.0688(14) Uani 1 1 d . . .
H11A H 0.2114 0.7629 -0.2330 0.083 Uiso 1 1 calc R . .
H11B H 0.3075 0.6967 -0.1964 0.083 Uiso 1 1 calc R . .
C12 C 0.2551(5) 0.7908(4) -0.1334(3) 0.0720(14) Uani 1 1 d . . .
H12A H 0.2327 0.8537 -0.1364 0.086 Uiso 1 1 calc R . .
H12B H 0.3262 0.7850 -0.0997 0.086 Uiso 1 1 calc R . .
C13 C 0.1515(5) 0.7368(4) -0.1109(3) 0.0824(16) Uani 1 1 d . . .
H13A H 0.0818 0.7418 -0.1456 0.099 Uiso 1 1 calc R . .
H13B H 0.1751 0.6741 -0.1081 0.099 Uiso 1 1 calc R . .
C14 C 0.1146(6) 0.7639(5) -0.0448(3) 0.102(2) Uani 1 1 d . . .
H14A H 0.0497 0.7260 -0.0345 0.153 Uiso 1 1 calc R . .
H14B H 0.0877 0.8252 -0.0474 0.153 Uiso 1 1 calc R . .
H14C H 0.1823 0.7582 -0.0098 0.153 Uiso 1 1 calc R . .
C21 C 0.3887(5) 0.7747(3) -0.3025(3) 0.0727(14) Uani 1 1 d . . .
H21A H 0.3105 0.7856 -0.3291 0.087 Uiso 1 1 calc R . .
H21B H 0.4481 0.8102 -0.3223 0.087 Uiso 1 1 calc R . .
C22 C 0.4197(7) 0.6772(4) -0.3095(3) 0.0962(19) Uani 1 1 d . . .
H22A H 0.3647 0.6405 -0.2873 0.115 Uiso 1 1 calc R . .
H22B H 0.5015 0.6661 -0.2876 0.115 Uiso 1 1 calc R . .
C23 C 0.4100(10) 0.6511(5) -0.3857(4) 0.151(4) Uani 1 1 d . . .
H23A H 0.3287 0.6656 -0.4067 0.181 Uiso 1 1 calc R . .
H23B H 0.4652 0.6893 -0.4065 0.181 Uiso 1 1 calc R . .
C24 C 0.4335(12) 0.5626(7) -0.4024(6) 0.221(6) Uani 1 1 d . . .
H24A H 0.4251 0.5564 -0.4510 0.331 Uiso 1 1 calc R . .
H24B H 0.3771 0.5234 -0.3845 0.331 Uiso 1 1 calc R . .
H24C H 0.5146 0.5469 -0.3834 0.331 Uiso 1 1 calc R . .
C31 C 0.3604(4) 0.9090(3) -0.2333(3) 0.0646(12) Uani 1 1 d . . .
H31A H 0.3709 0.9318 -0.1871 0.077 Uiso 1 1 calc R . .
H31B H 0.4221 0.9366 -0.2566 0.077 Uiso 1 1 calc R . .
C32 C 0.2385(4) 0.9393(4) -0.2675(3) 0.0707(14) Uani 1 1 d . . .
H32A H 0.1755 0.9154 -0.2433 0.085 Uiso 1 1 calc R . .
H32B H 0.2254 0.9163 -0.3136 0.085 Uiso 1 1 calc R . .
C33 C 0.2311(5) 1.0414(4) -0.2688(3) 0.0872(17) Uani 1 1 d . . .
H33A H 0.2466 1.0637 -0.2226 0.105 Uiso 1 1 calc R . .
H33B H 0.2942 1.0645 -0.2934 0.105 Uiso 1 1 calc R . .
C34 C 0.1116(6) 1.0770(5) -0.3011(4) 0.122(3) Uani 1 1 d . . .
H34A H 0.1122 1.1414 -0.2989 0.183 Uiso 1 1 calc R . .
H34B H 0.0483 1.0542 -0.2775 0.183 Uiso 1 1 calc R . .
H34C H 0.0975 1.0583 -0.3478 0.183 Uiso 1 1 calc R . .
C41 C 0.5041(4) 0.7921(4) -0.1852(3) 0.0739(15) Uani 1 1 d . . .
H41A H 0.4986 0.8177 -0.1408 0.089 Uiso 1 1 calc R . .
H41B H 0.5141 0.7278 -0.1793 0.089 Uiso 1 1 calc R . .
C42 C 0.6161(5) 0.8286(4) -0.2100(3) 0.0832(17) Uani 1 1 d . . .
H42A H 0.6306 0.7964 -0.2506 0.100 Uiso 1 1 calc R . .
H42B H 0.6036 0.8913 -0.2219 0.100 Uiso 1 1 calc R . .
C43 C 0.7250(5) 0.8200(5) -0.1573(4) 0.104(2) Uani 1 1 d . . .
H43A H 0.7080 0.8491 -0.1159 0.124 Uiso 1 1 calc R . .
H43B H 0.7394 0.7569 -0.1472 0.124 Uiso 1 1 calc R . .
C44 C 0.8375(7) 0.8600(7) -0.1781(4) 0.151(4) Uani 1 1 d . . .
H44A H 0.9035 0.8524 -0.1422 0.227 Uiso 1 1 calc R . .
H44B H 0.8249 0.9228 -0.1873 0.227 Uiso 1 1 calc R . .
H44C H 0.8565 0.8304 -0.2184 0.227 Uiso 1 1 calc R . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
V1 0.0553(5) 0.0499(4) 0.0485(5) -0.0059(3) 0.0151(3) 0.0038(3)
V2 0.0616(5) 0.0399(4) 0.0465(4) 0.0031(3) 0.0075(3) 0.0035(3)
V3 0.0611(5) 0.0471(4) 0.0377(4) 0.0028(3) 0.0095(3) 0.0002(3)
O1 0.0594(17) 0.0455(16) 0.0467(17) -0.0019(12) 0.0134(13) -0.0053(13)
O2 0.0530(16) 0.0442(15) 0.0433(16) 0.0002(12) 0.0092(13) -0.0018(13)
O3 0.0597(18) 0.0483(16) 0.061(2) -0.0045(14) 0.0122(15) 0.0081(14)
O4 0.047(2) 0.0356(19) 0.039(2) 0.0032(15) 0.0105(16) -0.0019(16)
O5 0.0550(17) 0.0449(15) 0.0488(17) 0.0000(12) 0.0068(14) 0.0012(13)
O6 0.0646(19) 0.0587(18) 0.0486(18) -0.0034(14) 0.0166(15) -0.0054(15)
O7 0.0669(19) 0.0480(16) 0.0476(17) 0.0105(13) 0.0038(14) -0.0015(14)
O8 0.077(2) 0.0412(16) 0.063(2) 0.0027(14) 0.0068(16) 0.0009(14)
O9 0.0564(19) 0.074(2) 0.069(2) -0.0089(17) 0.0188(16) 0.0054(16)
O10 0.078(2) 0.0614(19) 0.0438(18) 0.0042(14) 0.0051(15) -0.0039(16)
O11 0.081(2) 0.072(2) 0.089(3) -0.005(2) 0.000(2) -0.0203(19)
O12 0.211(7) 0.132(5) 0.217(8) -0.012(5) -0.120(6) -0.032(4)
N1 0.069(2) 0.063(2) 0.053(2) 0.0190(19) 0.0113(19) 0.0003(19)
C1 0.051(2) 0.052(2) 0.048(2) -0.0006(19) 0.0075(19) -0.0048(19)
C2 0.050(3) 0.062(3) 0.058(3) -0.004(2) 0.003(2) 0.005(2)
C3 0.055(3) 0.059(3) 0.056(3) -0.002(2) 0.016(2) -0.009(2)
C4 0.055(3) 0.051(2) 0.051(3) -0.0016(19) 0.006(2) -0.002(2)
C5 0.060(3) 0.058(3) 0.066(3) 0.001(2) 0.006(2) -0.003(2)
C6 0.109(5) 0.090(4) 0.106(5) -0.020(4) -0.006(4) -0.025(4)
C7 0.168(8) 0.078(4) 0.160(8) -0.012(4) 0.022(6) -0.036(5)
C8 0.247(13) 0.115(7) 0.268(16) 0.049(8) -0.002(10) 0.018(8)
C11 0.074(3) 0.068(3) 0.067(3) 0.023(3) 0.017(3) -0.005(3)
C12 0.075(3) 0.075(3) 0.067(3) 0.029(3) 0.013(3) 0.004(3)
C13 0.076(4) 0.082(4) 0.094(4) 0.020(3) 0.032(3) 0.002(3)
C14 0.091(4) 0.126(5) 0.097(5) 0.030(4) 0.046(4) 0.016(4)
C21 0.088(4) 0.071(3) 0.060(3) 0.012(3) 0.013(3) 0.006(3)
C22 0.124(5) 0.078(4) 0.092(5) 0.013(3) 0.035(4) 0.009(4)
C23 0.275(12) 0.073(4) 0.122(7) 0.013(4) 0.091(7) 0.027(6)
C24 0.379(19) 0.115(8) 0.174(11) 0.006(7) 0.056(11) 0.053(10)
C31 0.074(3) 0.062(3) 0.058(3) 0.016(2) 0.011(2) 0.000(2)
C32 0.071(3) 0.078(3) 0.063(3) 0.019(3) 0.010(3) 0.003(3)
C33 0.091(4) 0.076(4) 0.093(5) 0.005(3) 0.007(3) 0.015(3)
C34 0.117(6) 0.120(6) 0.123(6) 0.023(5) -0.003(5) 0.036(5)
C41 0.073(3) 0.087(4) 0.061(3) 0.028(3) 0.008(3) 0.000(3)
C42 0.072(3) 0.103(4) 0.076(4) 0.029(3) 0.016(3) 0.002(3)
C43 0.064(4) 0.138(6) 0.108(5) 0.044(4) 0.007(3) 0.006(4)
C44 0.093(5) 0.206(10) 0.149(8) 0.037(7) -0.007(5) -0.011(6)

_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 O9 1.600(3) . ?
V1 O3 1.819(3) . ?
V1 O6 1.827(3) . ?
V1 O5 2.021(3) . ?
V1 O1 2.023(3) . ?
V1 O4 2.2434(8) . ?
V1 V2 3.0312(12) 3_665 ?
V1 V3 3.0378(13) 3_665 ?
V2 O8 1.596(3) . ?
V2 O3 1.822(3) 3_665 ?
V2 O7 1.825(3) 3_665 ?
V2 O2 2.019(3) . ?
V2 O1 2.023(3) . ?
V2 O4 2.2429(8) . ?
V2 V1 3.0312(12) 3_665 ?
V2 V3 3.0338(11) 3_665 ?
V3 O10 1.598(3) . ?
V3 O7 1.814(3) . ?
V3 O6 1.823(3) 3_665 ?
V3 O5 2.023(3) . ?
V3 O2 2.034(3) . ?
V3 O4 2.2441(9) . ?
V3 V2 3.0338(11) 3_665 ?
V3 V1 3.0378(13) 3_665 ?
O1 C3 1.433(5) . ?
O2 C4 1.426(5) . ?
O3 V2 1.822(3) 3_665 ?
O4 V2 2.2429(8) 3_665 ?
O4 V1 2.2434(9) 3_665 ?
O4 V3 2.2441(9) 3_665 ?
O5 C2 1.435(5) . ?
O6 V3 1.823(3) 3_665 ?
O7 V2 1.825(3) 3_665 ?
O11 C6 1.292(7) . ?
O11 C5 1.446(5) . ?
O12 C6 1.204(8) . ?
N1 C11 1.506(6) . ?
N1 C31 1.513(6) . ?
N1 C21 1.530(6) . ?
N1 C41 1.532(6) . ?
C1 C3 1.524(6) . ?
C1 C5 1.532(6) . ?
C1 C4 1.535(6) . ?
C1 C2 1.543(6) . ?
C6 C7 1.497(10) . ?
C7 C8 1.436(12) . ?
C11 C12 1.493(7) . ?
C12 C13 1.521(7) . ?
C13 C14 1.482(8) . ?
C21 C22 1.505(7) . ?
C22 C23 1.550(9) . ?
C23 C24 1.393(10) . ?
C31 C32 1.504(6) . ?
C32 C33 1.524(7) . ?
C33 C34 1.495(8) . ?
C41 C42 1.502(7) . ?
C42 C43 1.499(8) . ?
C43 C44 1.494(9) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O9 V1 O3 103.81(15) . . ?
O9 V1 O6 104.32(16) . . ?
O3 V1 O6 93.60(14) . . ?
O9 V1 O5 96.54(15) . . ?
O3 V1 O5 88.42(13) . . ?
O6 V1 O5 157.87(13) . . ?
O9 V1 O1 97.00(14) . . ?
O3 V1 O1 158.01(12) . . ?
O6 V1 O1 87.96(12) . . ?
O5 V1 O1 82.19(11) . . ?
O9 V1 O4 172.27(13) . . ?
O3 V1 O4 81.16(9) . . ?
O6 V1 O4 81.02(10) . . ?
O5 V1 O4 77.53(9) . . ?
O1 V1 O4 77.42(8) . . ?
O9 V1 V2 137.24(12) . 3_665 ?
O3 V1 V2 33.68(9) . 3_665 ?
O6 V1 V2 87.67(10) . 3_665 ?
O5 V1 V2 81.84(9) . 3_665 ?
O1 V1 V2 124.71(8) . 3_665 ?
O4 V1 V2 47.49(2) . 3_665 ?
O9 V1 V3 137.68(13) . 3_665 ?
O3 V1 V3 87.94(10) . 3_665 ?
O6 V1 V3 33.61(10) . 3_665 ?
O5 V1 V3 124.68(9) . 3_665 ?
O1 V1 V3 81.27(8) . 3_665 ?
O4 V1 V3 47.40(2) . 3_665 ?
V2 V1 V3 66.01(3) 3_665 3_665 ?
O8 V2 O3 104.33(15) . 3_665 ?
O8 V2 O7 103.76(14) . 3_665 ?
O3 V2 O7 93.67(14) 3_665 3_665 ?
O8 V2 O2 96.93(14) . . ?
O3 V2 O2 87.97(13) 3_665 . ?
O7 V2 O2 158.12(13) 3_665 . ?
O8 V2 O1 96.58(14) . . ?
O3 V2 O1 157.99(12) 3_665 . ?
O7 V2 O1 87.87(13) 3_665 . ?
O2 V2 O1 82.71(11) . . ?
O8 V2 O4 172.40(12) . . ?
O3 V2 O4 81.13(9) 3_665 . ?
O7 V2 O4 80.90(9) 3_665 . ?
O2 V2 O4 77.80(8) . . ?
O1 V2 O4 77.44(8) . . ?
O8 V2 V1 137.76(12) . 3_665 ?
O3 V2 V1 33.62(9) 3_665 3_665 ?
O7 V2 V1 87.65(10) 3_665 3_665 ?
O2 V2 V1 81.68(8) . 3_665 ?
O1 V2 V1 124.75(8) . 3_665 ?
O4 V2 V1 47.50(2) . 3_665 ?
O8 V2 V3 136.91(12) . 3_665 ?
O3 V2 V3 87.85(10) 3_665 3_665 ?
O7 V2 V3 33.42(9) 3_665 3_665 ?
O2 V2 V3 125.08(8) . 3_665 ?
O1 V2 V3 81.38(8) . 3_665 ?
O4 V2 V3 47.47(2) . 3_665 ?
V1 V2 V3 65.99(3) 3_665 3_665 ?
O10 V3 O7 103.30(14) . . ?
O10 V3 O6 104.47(16) . 3_665 ?
O7 V3 O6 94.25(14) . 3_665 ?
O10 V3 O5 96.40(15) . . ?
O7 V3 O5 88.25(12) . . ?
O6 V3 O5 157.76(13) 3_665 . ?
O10 V3 O2 97.51(14) . . ?
O7 V3 O2 157.95(12) . . ?
O6 V3 O2 87.46(12) 3_665 . ?
O5 V3 O2 82.22(11) . . ?
O10 V3 O4 172.47(12) . . ?
O7 V3 O4 81.09(9) . . ?
O6 V3 O4 81.09(10) 3_665 . ?
O5 V3 O4 77.47(9) . . ?
O2 V3 O4 77.46(8) . . ?
O10 V3 V2 136.69(11) . 3_665 ?
O7 V3 V2 33.65(9) . 3_665 ?
O6 V3 V2 88.14(10) 3_665 3_665 ?
O5 V3 V2 81.75(8) . 3_665 ?
O2 V3 V2 124.71(8) . 3_665 ?
O4 V3 V2 47.44(2) . 3_665 ?
O10 V3 V1 138.01(12) . 3_665 ?
O7 V3 V1 87.99(10) . 3_665 ?
O6 V3 V1 33.71(10) 3_665 3_665 ?
O5 V3 V1 124.61(9) . 3_665 ?
O2 V3 V1 81.28(8) . 3_665 ?
O4 V3 V1 47.39(3) . 3_665 ?
V2 V3 V1 66.01(3) 3_665 3_665 ?
C3 O1 V2 118.9(2) . . ?
C3 O1 V1 118.7(3) . . ?
V2 O1 V1 109.65(13) . . ?
C4 O2 V2 118.7(2) . . ?
C4 O2 V3 118.5(2) . . ?
V2 O2 V3 109.31(13) . . ?
V1 O3 V2 112.70(14) . 3_665 ?
V2 O4 V2 180.00(4) . 3_665 ?
V2 O4 V1 85.01(3) . 3_665 ?
V2 O4 V1 94.99(3) 3_665 3_665 ?
V2 O4 V1 94.99(3) . . ?
V2 O4 V1 85.01(3) 3_665 . ?
V1 O4 V1 180.00(5) 3_665 . ?
V2 O4 V3 85.09(3) . 3_665 ?
V2 O4 V3 94.91(3) 3_665 3_665 ?
V1 O4 V3 94.79(4) 3_665 3_665 ?
V1 O4 V3 85.21(4) . 3_665 ?
V2 O4 V3 94.91(3) . . ?
V2 O4 V3 85.09(3) 3_665 . ?
V1 O4 V3 85.21(4) 3_665 . ?
V1 O4 V3 94.79(4) . . ?
V3 O4 V3 180.0 3_665 . ?
C2 O5 V1 119.4(3) . . ?
C2 O5 V3 118.7(3) . . ?
V1 O5 V3 109.56(13) . . ?
V3 O6 V1 112.68(16) 3_665 . ?
V3 O7 V2 112.92(14) . 3_665 ?
C6 O11 C5 119.3(5) . . ?
C11 N1 C31 111.6(4) . . ?
C11 N1 C21 108.9(4) . . ?
C31 N1 C21 108.6(3) . . ?
C11 N1 C41 108.7(3) . . ?
C31 N1 C41 108.4(4) . . ?
C21 N1 C41 110.6(4) . . ?
C3 C1 C5 109.7(4) . . ?
C3 C1 C4 111.3(4) . . ?
C5 C1 C4 109.1(4) . . ?
C3 C1 C2 110.8(4) . . ?
C5 C1 C2 106.6(3) . . ?
C4 C1 C2 109.2(4) . . ?
O5 C2 C1 111.4(3) . . ?
O1 C3 C1 111.7(3) . . ?
O2 C4 C1 112.5(3) . . ?
O11 C5 C1 107.2(4) . . ?
O12 C6 O11 121.4(7) . . ?
O12 C6 C7 124.8(7) . . ?
O11 C6 C7 113.8(7) . . ?
C8 C7 C6 118.6(7) . . ?
C12 C11 N1 117.1(4) . . ?
C11 C12 C13 111.3(5) . . ?
C14 C13 C12 115.2(5) . . ?
C22 C21 N1 116.5(4) . . ?
C21 C22 C23 110.2(5) . . ?
C24 C23 C22 118.6(8) . . ?
C32 C31 N1 116.9(4) . . ?
C31 C32 C33 110.6(4) . . ?
C34 C33 C32 113.9(5) . . ?
C42 C41 N1 116.9(4) . . ?
C43 C42 C41 111.8(5) . . ?
C44 C43 C42 113.7(6) . . ?

_diffrn_measured_fraction_theta_max 0.993
_diffrn_reflns_theta_full        27.48
_diffrn_measured_fraction_theta_full 0.993
_refine_diff_density_max         0.580
_refine_diff_density_min         -0.738
_refine_diff_density_rms         0.094

# Attachment '- c6.cif'

data_c6
_database_code_depnum_ccdc_archive 'CCDC 810986'
#TrackingRef '- c6.cif'

_database_code_CSD               ?
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C54 H110 N2 O23 V6'
_chemical_formula_weight         1461.08

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'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P2(1)/c

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

_cell_length_a                   11.375(2)
_cell_length_b                   15.453(3)
_cell_length_c                   19.841(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 97.54(3)
_cell_angle_gamma                90.00
_cell_volume                     3457.3(12)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.404
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1540
_exptl_absorpt_coefficient_mu    0.849
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.744
_exptl_absorpt_correction_T_max  0.844
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      293(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  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            32952
_diffrn_reflns_av_R_equivalents  0.0259
_diffrn_reflns_av_sigmaI/netI    0.0224
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         3.20
_diffrn_reflns_theta_max         27.45
_reflns_number_total             7866
_reflns_number_gt                6289
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0707P)^2^+1.0785P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         7866
_refine_ls_number_parameters     404
_refine_ls_number_restraints     103
_refine_ls_R_factor_all          0.0522
_refine_ls_R_factor_gt           0.0413
_refine_ls_wR_factor_ref         0.1281
_refine_ls_wR_factor_gt          0.1188
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_restrained_S_all      1.061
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
V1 V 0.45967(3) 0.35865(2) 0.008602(19) 0.04607(12) Uani 1 1 d . . .
V2 V 0.33144(3) 0.54484(3) 0.035392(19) 0.04741(12) Uani 1 1 d . . .
V3 V 0.43129(3) 0.50913(3) -0.111398(17) 0.04539(12) Uani 1 1 d . . .
O1 O 0.38980(12) 0.38531(10) -0.08815(7) 0.0442(3) Uani 1 1 d . . .
O2 O 0.5000 0.5000 0.0000 0.0384(4) Uani 1 2 d S . .
O3 O 0.30843(12) 0.41565(10) 0.03016(7) 0.0475(3) Uani 1 1 d . . .
O4 O 0.47775(14) 0.62020(10) -0.09756(8) 0.0530(4) Uani 1 1 d . . .
O5 O 0.28615(13) 0.53552(10) -0.06691(8) 0.0473(3) Uani 1 1 d . . .
O6 O 0.41926(14) 0.53098(11) 0.11789(8) 0.0518(4) Uani 1 1 d . . .
O7 O 0.39672(14) 0.65056(10) 0.02052(9) 0.0531(4) Uani 1 1 d . . .
O8 O 0.41393(17) 0.26067(11) 0.01031(9) 0.0614(4) Uani 1 1 d . . .
O9 O 0.20193(15) 0.56830(13) 0.05322(10) 0.0657(5) Uani 1 1 d . . .
O10 O 0.36776(16) 0.50832(12) -0.18844(8) 0.0619(4) Uani 1 1 d . . .
O11 O 0.0502(2) 0.27261(16) -0.09727(13) 0.0943(7) Uani 1 1 d . . .
O12 O -0.0822(6) 0.2584(3) -0.1829(3) 0.279(4) Uani 1 1 d U . .
N1 N 0.5962(2) 0.18145(15) 0.21975(11) 0.0626(5) Uani 1 1 d . . .
C1 C 0.19714(19) 0.38180(18) -0.00080(12) 0.0551(6) Uani 1 1 d . . .
H1A H 0.1335 0.4089 0.0197 0.066 Uiso 1 1 calc R . .
H1B H 0.1945 0.3201 0.0079 0.066 Uiso 1 1 calc R . .
C2 C 0.27348(19) 0.35334(16) -0.11188(12) 0.0521(5) Uani 1 1 d . . .
H2A H 0.2712 0.2916 -0.1034 0.062 Uiso 1 1 calc R . .
H2B H 0.2572 0.3622 -0.1606 0.062 Uiso 1 1 calc R . .
C3 C 0.1764(2) 0.49491(16) -0.09215(13) 0.0565(6) Uani 1 1 d . . .
H3A H 0.1601 0.5043 -0.1408 0.068 Uiso 1 1 calc R . .
H3B H 0.1130 0.5217 -0.0713 0.068 Uiso 1 1 calc R . .
C4 C 0.17720(19) 0.39743(16) -0.07778(12) 0.0532(5) Uani 1 1 d . . .
C5 C 0.0550(2) 0.36385(19) -0.10852(15) 0.0684(7) Uani 1 1 d . . .
H5A H -0.0065 0.3927 -0.0874 0.082 Uiso 1 1 calc R . .
H5B H 0.0420 0.3760 -0.1569 0.082 Uiso 1 1 calc R . .
C6 C -0.0204(4) 0.2267(3) -0.1393(3) 0.1250(17) Uani 1 1 d DU A .
C7 C -0.0200(6) 0.1294(4) -0.1234(4) 0.178(3) Uani 1 1 d DU . .
H7C H -0.0989 0.1141 -0.1139 0.213 Uiso 0.495(13) 1 calc PR A 2
H7D H -0.0067 0.0988 -0.1644 0.213 Uiso 0.495(13) 1 calc PR A 2
H7A H -0.0600 0.1223 -0.0835 0.213 Uiso 0.505(13) 1 calc PR A 1
H7B H -0.0694 0.1016 -0.1607 0.213 Uiso 0.505(13) 1 calc PR A 1
C8A C 0.0830(17) 0.0829(12) -0.1121(9) 0.213(7) Uani 0.505(13) 1 d PDU A 1
H8A H 0.0608 0.0223 -0.1137 0.256 Uiso 0.505(13) 1 calc PR A 1
H8B H 0.1254 0.0932 -0.1507 0.256 Uiso 0.505(13) 1 calc PR A 1
C9A C 0.1583(17) 0.0930(10) -0.0585(11) 0.244(8) Uani 0.505(13) 1 d PDU A 1
H9A H 0.1152 0.1200 -0.0250 0.293 Uiso 0.505(13) 1 calc PR A 1
H9B H 0.2150 0.1355 -0.0701 0.293 Uiso 0.505(13) 1 calc PR A 1
C10 C 0.2273(11) 0.0241(8) -0.0233(8) 0.286(6) Uani 1 1 d DU . .
H10C H 0.2044 0.0612 0.0121 0.343 Uiso 0.495(13) 1 calc PR A 2
H10D H 0.2218 -0.0344 -0.0063 0.343 Uiso 0.495(13) 1 calc PR A 2
H10A H 0.2065 0.0190 0.0224 0.343 Uiso 0.505(13) 1 calc PR A 1
H10B H 0.2072 -0.0302 -0.0467 0.343 Uiso 0.505(13) 1 calc PR A 1
C11 C 0.3423(9) 0.0370(6) -0.0199(6) 0.247(5) Uani 1 1 d DU A .
H11A H 0.3836 -0.0030 0.0119 0.370 Uiso 1 1 calc R . .
H11B H 0.3607 0.0951 -0.0051 0.370 Uiso 1 1 calc R . .
H11C H 0.3666 0.0282 -0.0639 0.370 Uiso 1 1 calc R . .
C8B C 0.0622(18) 0.0970(11) -0.0693(9) 0.206(7) Uani 0.495(13) 1 d PDU A 2
H8C H 0.1145 0.1447 -0.0541 0.248 Uiso 0.495(13) 1 calc PR A 2
H8D H 0.0171 0.0842 -0.0323 0.248 Uiso 0.495(13) 1 calc PR A 2
C9B C 0.1306(17) 0.0298(12) -0.0750(11) 0.246(8) Uani 0.495(13) 1 d PDU A 2
H9C H 0.1603 0.0325 -0.1186 0.296 Uiso 0.495(13) 1 calc PR A 2
H9D H 0.0833 -0.0224 -0.0745 0.296 Uiso 0.495(13) 1 calc PR A 2
C21 C 0.5831(3) 0.2163(2) 0.29055(15) 0.0760(8) Uani 1 1 d . . .
H21A H 0.5304 0.1783 0.3114 0.091 Uiso 1 1 calc R . .
H21B H 0.6600 0.2142 0.3182 0.091 Uiso 1 1 calc R . .
C22 C 0.5359(5) 0.3074(3) 0.2918(2) 0.1191(15) Uani 1 1 d . . .
H22A H 0.5883 0.3462 0.2714 0.143 Uiso 1 1 calc R . .
H22B H 0.4583 0.3101 0.2650 0.143 Uiso 1 1 calc R . .
C23 C 0.5266(6) 0.3363(3) 0.3622(3) 0.1336(18) Uani 1 1 d . . .
H23A H 0.4802 0.3891 0.3603 0.160 Uiso 1 1 calc R . .
H23B H 0.4842 0.2926 0.3845 0.160 Uiso 1 1 calc R . .
C24 C 0.6283(8) 0.3503(5) 0.3985(5) 0.238(5) Uani 1 1 d . . .
H24A H 0.6157 0.3718 0.4424 0.357 Uiso 1 1 calc R . .
H24B H 0.6720 0.3921 0.3761 0.357 Uiso 1 1 calc R . .
H24C H 0.6723 0.2972 0.4039 0.357 Uiso 1 1 calc R . .
C31 C 0.6932(3) 0.2329(2) 0.19268(15) 0.0726(7) Uani 1 1 d . . .
H31A H 0.6678 0.2928 0.1887 0.087 Uiso 1 1 calc R . .
H31B H 0.7630 0.2309 0.2265 0.087 Uiso 1 1 calc R . .
C32 C 0.7294(3) 0.2060(2) 0.12607(16) 0.0812(9) Uani 1 1 d . . .
H32A H 0.6632 0.2131 0.0903 0.097 Uiso 1 1 calc R . .
H32B H 0.7520 0.1455 0.1279 0.097 Uiso 1 1 calc R . .
C33 C 0.8335(3) 0.2611(3) 0.1104(2) 0.0996(12) Uani 1 1 d . . .
H33A H 0.8100 0.3215 0.1106 0.119 Uiso 1 1 calc R . .
H33B H 0.8983 0.2534 0.1469 0.119 Uiso 1 1 calc R . .
C34 C 0.8781(4) 0.2430(3) 0.0456(2) 0.1220(16) Uani 1 1 d . . .
H34A H 0.9446 0.2799 0.0412 0.183 Uiso 1 1 calc R . .
H34B H 0.8164 0.2538 0.0087 0.183 Uiso 1 1 calc R . .
H34C H 0.9024 0.1836 0.0446 0.183 Uiso 1 1 calc R . .
C41 C 0.6246(2) 0.08637(18) 0.22541(13) 0.0639(6) Uani 1 1 d . . .
H41A H 0.6191 0.0628 0.1798 0.077 Uiso 1 1 calc R . .
H41B H 0.5638 0.0584 0.2477 0.077 Uiso 1 1 calc R . .
C42 C 0.7440(2) 0.06148(18) 0.26307(14) 0.0635(6) Uani 1 1 d . . .
H42A H 0.7538 0.0877 0.3079 0.076 Uiso 1 1 calc R . .
H42B H 0.8064 0.0830 0.2387 0.076 Uiso 1 1 calc R . .
C43 C 0.7539(3) -0.03666(19) 0.26991(16) 0.0736(8) Uani 1 1 d . . .
H43A H 0.6914 -0.0577 0.2945 0.088 Uiso 1 1 calc R . .
H43B H 0.7426 -0.0625 0.2250 0.088 Uiso 1 1 calc R . .
C44 C 0.8727(3) -0.0648(3) 0.3067(2) 0.1032(12) Uani 1 1 d . . .
H44A H 0.8746 -0.1267 0.3104 0.155 Uiso 1 1 calc R . .
H44B H 0.8841 -0.0397 0.3513 0.155 Uiso 1 1 calc R . .
H44C H 0.9348 -0.0458 0.2817 0.155 Uiso 1 1 calc R . .
C51 C 0.4809(2) 0.1933(2) 0.17117(16) 0.0763(8) Uani 1 1 d . . .
H51A H 0.4676 0.2547 0.1635 0.092 Uiso 1 1 calc R . .
H51B H 0.4909 0.1672 0.1278 0.092 Uiso 1 1 calc R . .
C52 C 0.3728(3) 0.1552(3) 0.1953(2) 0.1041(13) Uani 1 1 d . . .
H52A H 0.3811 0.0928 0.1976 0.125 Uiso 1 1 calc R . .
H52B H 0.3666 0.1763 0.2407 0.125 Uiso 1 1 calc R . .
C53 C 0.2624(3) 0.1773(4) 0.1499(2) 0.1200(15) Uani 1 1 d . . .
H53A H 0.2711 0.1593 0.1040 0.144 Uiso 1 1 calc R . .
H53B H 0.2528 0.2397 0.1495 0.144 Uiso 1 1 calc R . .
C54 C 0.1523(4) 0.1369(5) 0.1698(3) 0.174(3) Uani 1 1 d . . .
H54A H 0.0848 0.1556 0.1390 0.261 Uiso 1 1 calc R . .
H54B H 0.1427 0.1541 0.2152 0.261 Uiso 1 1 calc R . .
H54C H 0.1587 0.0750 0.1678 0.261 Uiso 1 1 calc R . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
V1 0.0493(2) 0.0425(2) 0.0465(2) 0.00402(15) 0.00667(16) 0.00023(14)
V2 0.04174(19) 0.0560(2) 0.0466(2) -0.00796(16) 0.01396(15) 0.00358(15)
V3 0.0489(2) 0.0535(2) 0.03450(19) 0.00294(14) 0.00835(15) -0.00188(15)
O1 0.0434(7) 0.0488(8) 0.0414(7) -0.0022(6) 0.0087(6) -0.0011(6)
O2 0.0404(10) 0.0420(10) 0.0341(9) 0.0008(7) 0.0099(8) 0.0029(8)
O3 0.0442(7) 0.0561(9) 0.0442(8) -0.0010(7) 0.0135(6) -0.0054(6)
O4 0.0603(9) 0.0525(9) 0.0456(8) 0.0107(7) 0.0041(7) -0.0049(7)
O5 0.0415(7) 0.0529(8) 0.0472(8) -0.0009(7) 0.0040(6) 0.0034(6)
O6 0.0519(8) 0.0653(10) 0.0415(8) -0.0081(7) 0.0181(7) -0.0051(7)
O7 0.0488(8) 0.0481(8) 0.0627(10) -0.0065(7) 0.0081(7) 0.0070(6)
O8 0.0745(11) 0.0474(9) 0.0617(10) 0.0039(8) 0.0072(8) -0.0080(8)
O9 0.0477(8) 0.0821(12) 0.0705(11) -0.0141(9) 0.0198(8) 0.0063(8)
O10 0.0710(11) 0.0744(12) 0.0391(8) 0.0036(7) 0.0029(7) -0.0061(8)
O11 0.0779(14) 0.0939(17) 0.1071(18) 0.0000(13) -0.0031(13) -0.0274(12)
O12 0.333(7) 0.134(3) 0.299(7) -0.011(4) -0.222(6) -0.033(4)
N1 0.0711(13) 0.0657(13) 0.0533(11) 0.0189(10) 0.0163(10) 0.0073(10)
C1 0.0440(11) 0.0689(15) 0.0544(13) -0.0047(11) 0.0140(10) -0.0112(10)
C2 0.0489(12) 0.0591(13) 0.0482(11) -0.0079(10) 0.0060(9) -0.0076(10)
C3 0.0415(11) 0.0675(15) 0.0592(14) -0.0029(11) 0.0025(10) 0.0034(10)
C4 0.0411(10) 0.0650(14) 0.0534(12) -0.0044(11) 0.0056(9) -0.0063(10)
C5 0.0489(13) 0.0811(19) 0.0745(17) -0.0093(14) 0.0055(12) -0.0096(12)
C6 0.103(3) 0.106(3) 0.151(4) -0.023(3) -0.040(3) -0.010(2)
C7 0.147(5) 0.102(4) 0.274(8) -0.030(4) -0.008(5) -0.019(3)
C8A 0.250(13) 0.153(10) 0.233(15) -0.046(11) 0.019(11) 0.076(9)
C9A 0.258(13) 0.118(10) 0.327(17) -0.020(12) -0.075(12) -0.019(10)
C10 0.226(9) 0.249(11) 0.364(15) 0.022(10) -0.031(11) 0.030(9)
C11 0.234(8) 0.155(7) 0.351(14) 0.057(7) 0.037(10) -0.017(7)
C8B 0.255(14) 0.124(9) 0.241(15) -0.022(10) 0.036(12) 0.076(10)
C9B 0.261(13) 0.175(13) 0.288(17) -0.038(12) -0.020(11) 0.106(10)
C21 0.096(2) 0.0684(17) 0.0658(16) 0.0133(14) 0.0181(15) 0.0155(15)
C22 0.177(4) 0.089(3) 0.099(3) 0.011(2) 0.046(3) 0.046(3)
C23 0.184(5) 0.094(3) 0.126(4) -0.012(3) 0.036(4) 0.020(3)
C24 0.222(9) 0.171(7) 0.296(11) -0.095(7) -0.057(8) 0.016(6)
C31 0.0716(16) 0.0730(18) 0.0754(18) 0.0241(15) 0.0172(14) 0.0021(13)
C32 0.0789(19) 0.095(2) 0.0736(18) 0.0305(17) 0.0238(15) 0.0126(16)
C33 0.083(2) 0.102(3) 0.122(3) 0.037(2) 0.044(2) 0.0159(19)
C34 0.104(3) 0.151(4) 0.122(3) 0.052(3) 0.056(3) 0.026(3)
C41 0.0729(16) 0.0661(16) 0.0540(13) 0.0131(12) 0.0132(12) 0.0050(12)
C42 0.0677(15) 0.0686(16) 0.0555(14) 0.0107(12) 0.0131(12) 0.0064(12)
C43 0.0809(19) 0.0688(17) 0.0724(18) 0.0000(14) 0.0143(15) 0.0147(14)
C44 0.107(3) 0.094(3) 0.103(3) 0.003(2) -0.005(2) 0.037(2)
C51 0.0710(17) 0.089(2) 0.0687(17) 0.0306(15) 0.0086(14) 0.0083(15)
C52 0.0713(19) 0.141(3) 0.102(3) 0.057(2) 0.0182(18) 0.013(2)
C53 0.077(2) 0.178(5) 0.103(3) 0.027(3) 0.003(2) 0.009(3)
C54 0.074(3) 0.284(9) 0.161(5) 0.047(5) 0.003(3) -0.001(4)

_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 1.6028(17) . ?
V1 O7 1.8085(17) 3_665 ?
V1 O4 1.8435(16) 3_665 ?
V1 O1 2.0213(15) . ?
V1 O3 2.0276(16) . ?
V1 O2 2.2430(6) . ?
V1 V2 3.0292(8) 3_665 ?
V1 V3 3.0345(8) 3_665 ?
V2 O9 1.6011(16) . ?
V2 O6 1.8147(17) . ?
V2 O7 1.8344(17) . ?
V2 O3 2.0144(16) . ?
V2 O5 2.0326(16) . ?
V2 O2 2.2367(6) . ?
V2 V1 3.0292(8) 3_665 ?
V2 V3 3.0306(10) 3_665 ?
V3 O10 1.6028(17) . ?
V3 O4 1.8062(16) . ?
V3 O6 1.8297(17) 3_665 ?
V3 O5 2.0134(16) . ?
V3 O1 2.0382(16) . ?
V3 O2 2.2499(7) . ?
V3 V2 3.0306(10) 3_665 ?
V3 V1 3.0345(8) 3_665 ?
O1 C2 1.433(2) . ?
O2 V2 2.2367(6) 3_665 ?
O2 V1 2.2430(6) 3_665 ?
O2 V3 2.2499(7) 3_665 ?
O3 C1 1.432(3) . ?
O4 V1 1.8435(16) 3_665 ?
O5 C3 1.428(3) . ?
O6 V3 1.8297(17) 3_665 ?
O7 V1 1.8085(17) 3_665 ?
O11 C6 1.292(4) . ?
O11 C5 1.430(4) . ?
O12 C6 1.149(5) . ?
N1 C41 1.505(3) . ?
N1 C31 1.514(3) . ?
N1 C21 1.530(4) . ?
N1 C51 1.534(3) . ?
C1 C4 1.533(3) . ?
C2 C4 1.522(3) . ?
C3 C4 1.533(3) . ?
C4 C5 1.533(3) . ?
C6 C7 1.536(7) . ?
C7 C8A 1.368(12) . ?
C7 C8B 1.419(13) . ?
C8A C9A 1.283(16) . ?
C9A C10 1.447(15) . ?
C10 C11 1.316(11) . ?
C10 C9B 1.405(15) . ?
C8B C9B 1.311(15) . ?
C21 C22 1.507(4) . ?
C22 C23 1.484(6) . ?
C23 C24 1.298(7) . ?
C31 C32 1.494(4) . ?
C32 C33 1.523(5) . ?
C33 C34 1.469(6) . ?
C41 C42 1.511(3) . ?
C42 C43 1.526(4) . ?
C43 C44 1.513(4) . ?
C51 C52 1.497(4) . ?
C52 C53 1.485(5) . ?
C53 C54 1.498(6) . ?

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 103.99(9) . 3_665 ?
O8 V1 O4 103.46(8) . 3_665 ?
O7 V1 O4 93.92(8) 3_665 3_665 ?
O8 V1 O1 97.14(8) . . ?
O7 V1 O1 88.37(7) 3_665 . ?
O4 V1 O1 158.02(7) 3_665 . ?
O8 V1 O3 96.84(9) . . ?
O7 V1 O3 158.21(7) 3_665 . ?
O4 V1 O3 87.29(7) 3_665 . ?
O1 V1 O3 82.71(6) . . ?
O8 V1 O2 172.62(7) . . ?
O7 V1 O2 81.37(5) 3_665 . ?
O4 V1 O2 80.97(5) 3_665 . ?
O1 V1 O2 77.77(4) . . ?
O3 V1 O2 77.33(5) . . ?
O8 V1 V2 137.75(7) . 3_665 ?
O7 V1 V2 34.02(5) 3_665 3_665 ?
O4 V1 V2 88.27(6) 3_665 3_665 ?
O1 V1 V2 81.46(5) . 3_665 ?
O3 V1 V2 124.49(5) . 3_665 ?
O2 V1 V2 47.364(11) . 3_665 ?
O8 V1 V3 136.63(7) . 3_665 ?
O7 V1 V3 87.77(5) 3_665 3_665 ?
O4 V1 V3 33.36(5) 3_665 3_665 ?
O1 V1 V3 125.18(5) . 3_665 ?
O3 V1 V3 81.31(5) . 3_665 ?
O2 V1 V3 47.612(13) . 3_665 ?
V2 V1 V3 66.13(2) 3_665 3_665 ?
O9 V2 O6 103.94(9) . . ?
O9 V2 O7 103.74(9) . . ?
O6 V2 O7 93.65(8) . . ?
O9 V2 O3 96.82(8) . . ?
O6 V2 O3 88.96(7) . . ?
O7 V2 O3 157.97(7) . . ?
O9 V2 O5 96.70(9) . . ?
O6 V2 O5 158.38(7) . . ?
O7 V2 O5 87.56(7) . . ?
O3 V2 O5 82.19(6) . . ?
O9 V2 O2 172.30(7) . . ?
O6 V2 O2 81.58(5) . . ?
O7 V2 O2 81.01(5) . . ?
O3 V2 O2 77.74(4) . . ?
O5 V2 O2 77.28(5) . . ?
O9 V2 V1 137.01(8) . 3_665 ?
O6 V2 V1 87.61(5) . 3_665 ?
O7 V2 V1 33.47(5) . 3_665 ?
O3 V2 V1 125.07(4) . 3_665 ?
O5 V2 V1 81.53(5) . 3_665 ?
O2 V2 V1 47.540(16) . 3_665 ?
O9 V2 V3 137.52(7) . 3_665 ?
O6 V2 V3 33.90(5) . 3_665 ?
O7 V2 V3 88.42(5) . 3_665 ?
O3 V2 V3 81.61(4) . 3_665 ?
O5 V2 V3 124.74(5) . 3_665 ?
O2 V2 V3 47.694(15) . 3_665 ?
V1 V2 V3 66.293(18) 3_665 3_665 ?
O10 V3 O4 103.81(8) . . ?
O10 V3 O6 103.71(9) . 3_665 ?
O4 V3 O6 94.39(8) . 3_665 ?
O10 V3 O5 97.28(9) . . ?
O4 V3 O5 88.93(7) . . ?
O6 V3 O5 157.27(7) 3_665 . ?
O10 V3 O1 96.87(8) . . ?
O4 V3 O1 158.36(7) . . ?
O6 V3 O1 86.72(7) 3_665 . ?
O5 V3 O1 82.14(6) . . ?
O10 V3 O2 172.46(7) . . ?
O4 V3 O2 81.56(5) . . ?
O6 V3 O2 80.90(6) 3_665 . ?
O5 V3 O2 77.35(5) . . ?
O1 V3 O2 77.27(4) . . ?
O10 V3 V2 137.14(7) . 3_665 ?
O4 V3 V2 87.83(5) . 3_665 ?
O6 V3 V2 33.58(5) 3_665 3_665 ?
O5 V3 V2 124.44(5) . 3_665 ?
O1 V3 V2 81.17(4) . 3_665 ?
O2 V3 V2 47.32(2) . 3_665 ?
O10 V3 V1 137.70(7) . 3_665 ?
O4 V3 V1 34.15(5) . 3_665 ?
O6 V3 V1 88.50(5) 3_665 3_665 ?
O5 V3 V1 81.68(5) . 3_665 ?
O1 V3 V1 124.50(4) . 3_665 ?
O2 V3 V1 47.420(15) . 3_665 ?
V2 V3 V1 65.93(2) 3_665 3_665 ?
C2 O1 V1 118.22(13) . . ?
C2 O1 V3 118.73(13) . . ?
V1 O1 V3 109.41(7) . . ?
V2 O2 V2 180.00(3) . 3_665 ?
V2 O2 V1 85.096(17) . 3_665 ?
V2 O2 V1 94.904(17) 3_665 3_665 ?
V2 O2 V1 94.904(17) . . ?
V2 O2 V1 85.096(17) 3_665 . ?
V1 O2 V1 180.000(19) 3_665 . ?
V2 O2 V3 95.02(3) . . ?
V2 O2 V3 84.98(3) 3_665 . ?
V1 O2 V3 84.968(15) 3_665 . ?
V1 O2 V3 95.032(15) . . ?
V2 O2 V3 84.98(3) . 3_665 ?
V2 O2 V3 95.02(3) 3_665 3_665 ?
V1 O2 V3 95.032(15) 3_665 3_665 ?
V1 O2 V3 84.968(15) . 3_665 ?
V3 O2 V3 180.000(6) . 3_665 ?
C1 O3 V2 119.07(14) . . ?
C1 O3 V1 118.53(14) . . ?
V2 O3 V1 109.47(7) . . ?
V3 O4 V1 112.49(8) . 3_665 ?
C3 O5 V3 119.13(14) . . ?
C3 O5 V2 118.46(15) . . ?
V3 O5 V2 109.71(7) . . ?
V2 O6 V3 112.52(8) . 3_665 ?
V1 O7 V2 112.52(8) 3_665 . ?
C6 O11 C5 118.3(3) . . ?
C41 N1 C31 112.3(2) . . ?
C41 N1 C21 108.72(19) . . ?
C31 N1 C21 107.7(2) . . ?
C41 N1 C51 108.7(2) . . ?
C31 N1 C51 108.5(2) . . ?
C21 N1 C51 110.9(2) . . ?
O3 C1 C4 112.12(18) . . ?
O1 C2 C4 112.76(18) . . ?
O5 C3 C4 112.50(18) . . ?
C2 C4 C3 110.2(2) . . ?
C2 C4 C5 109.8(2) . . ?
C3 C4 C5 106.0(2) . . ?
C2 C4 C1 110.6(2) . . ?
C3 C4 C1 109.7(2) . . ?
C5 C4 C1 110.5(2) . . ?
O11 C5 C4 108.8(2) . . ?
O12 C6 O11 121.2(5) . . ?
O12 C6 C7 123.9(5) . . ?
O11 C6 C7 114.8(5) . . ?
C8A C7 C8B 39.2(10) . . ?
C8A C7 C6 121.8(11) . . ?
C8B C7 C6 119.1(9) . . ?
C9A C8A C7 122.4(15) . . ?
C8A C9A C10 124.8(15) . . ?
C11 C10 C9B 135.0(19) . . ?
C11 C10 C9A 112.7(14) . . ?
C9B C10 C9A 43.8(9) . . ?
C9B C8B C7 123.7(14) . . ?
C8B C9B C10 113.8(14) . . ?
C22 C21 N1 114.9(3) . . ?
C23 C22 C21 111.5(3) . . ?
C24 C23 C22 113.8(7) . . ?
C32 C31 N1 117.8(3) . . ?
C31 C32 C33 109.7(3) . . ?
C34 C33 C32 116.0(4) . . ?
N1 C41 C42 117.1(2) . . ?
C41 C42 C43 110.4(2) . . ?
C44 C43 C42 112.3(3) . . ?
C52 C51 N1 115.1(2) . . ?
C53 C52 C51 112.4(3) . . ?
C52 C53 C54 114.5(4) . . ?

_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_theta_full        27.45
_diffrn_measured_fraction_theta_full 0.995
_refine_diff_density_max         0.398
_refine_diff_density_min         -0.460
_refine_diff_density_rms         0.056