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


data_global
_journal_name_full               Chem.Commun.
_journal_coden_cambridge         0182
#TrackingRef '- mper13.cif'

_publ_contact_author_name        'Dr. Garry Hanan'
_publ_contact_author_address     
;
D\'epartement de Chimie
Universit\'e de Montr\'eal
C.P. 6128, Succ. Centre-ville
Montr\'eal, Qu\'ebec
Canada H3C 3J7

;

_publ_contact_author_phone       '+1 514 343 7056'
_publ_contact_author_fax         '+1 514 343 2468'
_publ_contact_author_email       garry.hanan@umontreal.ca
_publ_section_title              
;
MPER13
#Lindqvist-(amide-3-Py)2
#
;

# The loop structure below should contain the names and addresses of all
# authors, in the required order of publication. Repeat as necessary.

loop_
_publ_author_name
_publ_author_address

M.-P.Santoni
;
D\'epartement de Chimie
Universit\'e de Montr\'eal
C.P. 6128, Succ. Centre-ville,
Montr\'eal, Qu\'ebec
Canada H3C 3J7
;
B.Hasenknopf
;
Institut Parisien de Chimie Mol\'eculaire
Universit\'e Pierre et Marie Curie
UMR 7201,
Paris, France
;
A.Proust
;
Institut Parisien de Chimie Mol\'eculaire
Universit\'e Pierre et Marie Curie
UMR 7201,
Paris, France
;
G.HananM.-P.Santoni
;
D\'epartement de Chimie
Universit\'e de Montr\'eal
C.P. 6128, Succ. Centre-ville,
Montr\'eal, Qu\'ebec
Canada H3C 3J7
;
A.Pal ''
G.Hanan ''
M.-C.Tang ''
K.Venne ''
A.Furtos ''
P.Menard-Tremblay ''
C.Malveau ''
B.Hasenknopf ''

#==============================================================================
# 4. TEXT
#==============================================================================

_publ_section_abstract           
;
Here should be written a short abstract
;

_publ_section_comment            
;
Here should be written the text of the article
;

_publ_section_exptl_prep         
;
Small details about the preparation of the compound.
;

_publ_section_exptl_refinement   
;

All non-H atoms were refined by full-matrix least-squares
with anisotropic displacement parameters. The H atoms were
generated geometrically (C-H 0.95 to 0.99, N-H 0.88\%A)
and were included in the refinement in the riding model approximation;
their temperature factors were set to 1.5 times those of the
equivalent isotropic temperature factors of the parent site (methyl)
and 1.2 times for others.

;

# start Validation Reply Form
_vrf_PUBL006_GLOBAL              
;
PROBLEM: _publ_requested_journal is missing
RESPONSE: Will be communicated in due time.
;
_vrf_PLAT220_mper13              
;
PROBLEM: Large Non-Solvent O Ueq(max)/Ueq(min)
RESPONSE: Caused by slight thermal motion of the organic counterpart of the
structure. Checked and found to be acceptable.
;
_vrf_PLAT222_mper13              
;
PROBLEM: Large Non-Solvent H Ueq(max)/Ueq(min)
RESPONSE: Same than for PLAT220 alert.
;
_vrf_PLAT230_mper13              
;
PROBLEM: Hirshfeld Test Diff for N1 -- C5
RESPONSE: Checked. However, no errors could be found as atoms assignation
is unambiguous due to chemistry and no particular thermal motion involving these atoms
is noticeable.
;
_vrf_PLAT242_mper13              
;
PROBLEM: Check Low Ueq as Compared to Neighbors for C202
RESPONSE: Checked and found to be due to thermal motion of the alkyl
chains of the counter-ion. Acceptable.
;

_vrf_PLAT318_mper13              
;
PROBLEM: Check Hybridisation of N1 in Main Residue
RESPONSE: Checked. Comes from
calculation of H atom position using the "Riding Model" approach.
;
# end Validation Reply Form

_publ_section_figure_captions    
;
Fig 1 Ortep view of the title compound.
Thermal ellipsoids are shown at 50% probability levels.
;

_publ_section_table_legends      
;
Table 1. Selected geometric parameters (\%A, \%) for the title compound.
;

_publ_section_acknowledgements   
;
We are grateful to the Natural Sciences and Engineering Research Council of
Canada, the Minist\`ere de l'Education du Qu\'ebec, the Centre for
Self-Assembled Chemical Structures and the Universit\'e de Montr\'eal for
financial support.
;

_publ_section_references         
;

APEX2 (2007) version 2.4-0; Bruker Molecular Analysis Research Tool.
Bruker AXS Inc., Madison, WI 53719-1173.

Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122.

Sheldrick, G.M. (2004). SADABS, Bruker Area Detector Absorption Corrections.
Bruker AXS Inc., Madison, WI 53719-1173.

SHELXTL (2001) version 6.12; Bruker Analytical X-ray Systems Inc.,
Madison, WI 53719-1173.

Spek, A.L. (2008). PLATON, A Multipurpose Crystallographic Tool,
Utrecht University, Utrecht, The Netherlands.

Maris, T. (2004). UdMX, University of Montr\'eal, Montr\'eal, QC, Canada.

XPREP (2005) Version 2005/2; X-ray data Preparation and Reciprocal space
Exploration Program. Bruker AXS Inc., Madison, WI 53719-1173.
;

# ========================================================
# STRUCTURAL DATA
# ========================================================

data_mper13
_database_code_depnum_ccdc_archive 'CCDC 766600'
#TrackingRef '- mper13.cif'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C20 H22 N4 O21 V6, 2(C16 H36 N), 2(C3 H7 N O)'
_chemical_formula_sum            'C58 H108 N8 O23 V6'
_chemical_formula_weight         1591.16
_chemical_compound_source        'Synthesized by the authors. See text'

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   P21/c
_symmetry_space_group_name_hall  '-P 2ybc'

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                   13.5535(17)
_cell_length_b                   13.2675(17)
_cell_length_c                   20.489(3)
_cell_angle_alpha                90
_cell_angle_beta                 103.456(2)
_cell_angle_gamma                90
_cell_volume                     3583.2(8)
_cell_formula_units_Z            2
_cell_measurement_temperature    150
_cell_measurement_reflns_used    8487
_cell_measurement_theta_min      2.25
_cell_measurement_theta_max      24.24

_exptl_crystal_description       hexagon
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.475
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1668
_exptl_absorpt_coefficient_mu    0.828
_exptl_absorpt_correction_Type   multi-scan
_exptl_absorpt_correction_T_min  0.8517
_exptl_absorpt_correction_T_max  0.9359
_exptl_absorpt_process_details   'Sadabs (Sheldrick, 2004)'

_exptl_special_details           
;
X-ray crystallographic data for I were collected from a single crystal
sample, which was mounted on a loop fiber. Data were collected using
a Bruker smart diffractometer equiped with an APEX II CCD Detector,
a graphite monochromator. The crystal-to-detector distance was
5.0 cm, and the data collection was carried out in 512 x 512 pixel mode.
The initial unit cell parameters were determined by a least-squares fit
of the angular setting of strong reflections, collected by a 10.0 degree
scan in 33 frames over four different parts of the reciprocal space
(132 frames total).

;

_diffrn_ambient_temperature      150
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'X-ray sealed tube'
_diffrn_radiation_monochromator  Graphite
_diffrn_measurement_device_type  'Bruker APEX II'
_diffrn_measurement_method       \w
_diffrn_detector_area_resol_mean 8.3
_diffrn_standards_number         950
_diffrn_standards_interval_time  900
_diffrn_standards_decay_%        5.40
_diffrn_reflns_number            72395
_diffrn_reflns_av_R_equivalents  0.073
_diffrn_reflns_av_sigmaI/netI    0.0403
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         1.54
_diffrn_reflns_theta_max         27.61
_reflns_number_total             8192
_reflns_number_gt                6277
_reflns_threshold_expression     I>2\s(I)

_computing_data_collection       'APEX2 v2.4-0 (Bruker AXS, 2007)'
_computing_cell_refinement       'SAINT V7.34A (Bruker AXS, 2006)'
_computing_data_reduction        'SAINT V7.34A (Bruker AXS, 2006)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_molecular_graphics    'SHELXTL v6.12 (Bruker AXS, 2001)'
_computing_publication_material  'UdMX (Maris, 2004)'

_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^)+(0.0510P)^2^+3.2783P] 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         8192
_refine_ls_number_parameters     436
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0605
_refine_ls_R_factor_gt           0.0413
_refine_ls_wR_factor_ref         0.1160
_refine_ls_wR_factor_gt          0.1055
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_restrained_S_all      1.037
_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 0.43532(3) 0.52441(3) 0.39022(2) 0.01869(10) Uani 1 1 d . . .
V2 V 0.49709(3) 0.66868(3) 0.50739(2) 0.01974(11) Uani 1 1 d . . .
V3 V 0.64974(3) 0.49343(3) 0.47189(2) 0.01964(11) Uani 1 1 d . . .
O1 O 0.38083(13) 0.52777(13) 0.31183(9) 0.0240(4) Uani 1 1 d . . .
O2 O 0.51204(14) 0.78800(13) 0.51698(9) 0.0259(4) Uani 1 1 d . . .
O3 O 0.76307(13) 0.49807(14) 0.46098(9) 0.0259(4) Uani 1 1 d . . .
O4 O 0.44739(13) 0.65424(13) 0.41545(8) 0.0218(4) Uani 1 1 d . . .
O5 O 0.57031(13) 0.51091(13) 0.38911(8) 0.0217(4) Uani 1 1 d . . .
O6 O 0.37684(13) 0.64276(13) 0.52647(9) 0.0224(4) Uani 1 1 d . . .
O7 O 0.5000 0.5000 0.5000 0.0169(5) Uani 1 2 d S . .
O8 O 0.31058(12) 0.51452(12) 0.42654(8) 0.0189(3) Uani 1 1 d . . .
O9 O 0.43249(12) 0.37134(12) 0.39941(8) 0.0185(3) Uani 1 1 d . . .
O10 O 0.63664(12) 0.64108(12) 0.49011(8) 0.0191(3) Uani 1 1 d . . .
O11 O 0.14749(17) 0.35497(18) 0.25879(11) 0.0424(5) Uani 1 1 d . . .
N1 N 0.16369(17) 0.28404(17) 0.36262(11) 0.0279(5) Uani 1 1 d . . .
H1 H 0.1407 0.2364 0.3851 0.034 Uiso 1 1 calc R . .
N2 N -0.1503(2) 0.2635(2) 0.20099(16) 0.0515(8) Uani 1 1 d . . .
C1 C 0.25383(18) 0.34148(19) 0.39724(12) 0.0221(5) Uani 1 1 d . . .
C2 C 0.22816(18) 0.45402(19) 0.39225(12) 0.0221(5) Uani 1 1 d . . .
H2A H 0.2096 0.4740 0.3444 0.026 Uiso 1 1 calc R . .
H2B H 0.1687 0.4664 0.4115 0.026 Uiso 1 1 calc R . .
C3 C 0.34351(19) 0.31803(19) 0.36594(13) 0.0233(5) Uani 1 1 d . . .
H3A H 0.3573 0.2447 0.3688 0.028 Uiso 1 1 calc R . .
H3B H 0.3259 0.3372 0.3179 0.028 Uiso 1 1 calc R . .
C4 C 0.72208(19) 0.69303(19) 0.52923(12) 0.0219(5) Uani 1 1 d . . .
H4A H 0.7083 0.7664 0.5271 0.026 Uiso 1 1 calc R . .
H4B H 0.7818 0.6807 0.5102 0.026 Uiso 1 1 calc R . .
C5 C 0.1146(2) 0.3007(2) 0.29830(15) 0.0333(6) Uani 1 1 d . . .
C6 C 0.0141(2) 0.2490(2) 0.27427(15) 0.0345(6) Uani 1 1 d . . .
C7 C -0.0084(3) 0.1529(3) 0.29398(17) 0.0417(7) Uani 1 1 d . . .
H7 H 0.0392 0.1160 0.3267 0.050 Uiso 1 1 calc R . .
C8 C -0.1023(3) 0.1131(3) 0.26432(18) 0.0456(8) Uani 1 1 d . . .
H8 H -0.1199 0.0470 0.2754 0.055 Uiso 1 1 calc R . .
C9 C -0.1700(3) 0.1697(3) 0.21873(19) 0.0469(8) Uani 1 1 d . . .
H9 H -0.2340 0.1410 0.1987 0.056 Uiso 1 1 calc R . .
C10 C -0.0598(2) 0.3008(3) 0.22856(17) 0.0407(7) Uani 1 1 d . . .
H10 H -0.0445 0.3670 0.2163 0.049 Uiso 1 1 calc R . .
N200 N 0.57054(16) 0.39217(15) 0.19802(10) 0.0228(4) Uani 1 1 d . . .
C200 C 0.6143(2) 0.38829(19) 0.13590(12) 0.0244(5) Uani 1 1 d . . .
H20A H 0.6881 0.3754 0.1506 0.029 Uiso 1 1 calc R . .
H20B H 0.5837 0.3302 0.1082 0.029 Uiso 1 1 calc R . .
C201 C 0.5988(2) 0.4813(2) 0.09206(15) 0.0343(7) Uani 1 1 d . . .
H20C H 0.6162 0.5421 0.1205 0.041 Uiso 1 1 calc R . .
H20D H 0.5265 0.4864 0.0681 0.041 Uiso 1 1 calc R . .
C202 C 0.6644(2) 0.4773(2) 0.04140(15) 0.0369(7) Uani 1 1 d . . .
H20E H 0.6428 0.5311 0.0076 0.044 Uiso 1 1 calc R . .
H20F H 0.6542 0.4116 0.0178 0.044 Uiso 1 1 calc R . .
C203 C 0.7763(3) 0.4904(4) 0.0742(2) 0.0736(14) Uani 1 1 d . . .
H20G H 0.7866 0.5549 0.0980 0.110 Uiso 1 1 calc R . .
H20H H 0.8155 0.4895 0.0396 0.110 Uiso 1 1 calc R . .
H20I H 0.7988 0.4353 0.1060 0.110 Uiso 1 1 calc R . .
C204 C 0.4560(2) 0.4041(2) 0.17950(14) 0.0264(6) Uani 1 1 d . . .
H20J H 0.4397 0.4698 0.1566 0.032 Uiso 1 1 calc R . .
H20K H 0.4318 0.4069 0.2215 0.032 Uiso 1 1 calc R . .
C205 C 0.3965(2) 0.3226(2) 0.13487(14) 0.0301(6) Uani 1 1 d . . .
H20L H 0.4236 0.2555 0.1512 0.036 Uiso 1 1 calc R . .
H20M H 0.4049 0.3310 0.0885 0.036 Uiso 1 1 calc R . .
C206 C 0.2842(2) 0.3280(2) 0.13497(17) 0.0401(7) Uani 1 1 d . . .
H20N H 0.2477 0.2771 0.1030 0.048 Uiso 1 1 calc R . .
H20O H 0.2765 0.3086 0.1802 0.048 Uiso 1 1 calc R . .
C207 C 0.2333(3) 0.4270(3) 0.1175(2) 0.0581(10) Uani 1 1 d . . .
H20P H 0.2649 0.4775 0.1507 0.087 Uiso 1 1 calc R . .
H20Q H 0.1612 0.4208 0.1173 0.087 Uiso 1 1 calc R . .
H20R H 0.2403 0.4478 0.0729 0.087 Uiso 1 1 calc R . .
C208 C 0.6021(2) 0.29376(18) 0.23533(13) 0.0236(5) Uani 1 1 d . . .
H20S H 0.5809 0.2372 0.2036 0.028 Uiso 1 1 calc R . .
H20T H 0.6771 0.2922 0.2496 0.028 Uiso 1 1 calc R . .
C209 C 0.5595(2) 0.2760(2) 0.29640(14) 0.0298(6) Uani 1 1 d . . .
H20U H 0.4861 0.2609 0.2820 0.036 Uiso 1 1 calc R . .
H20V H 0.5679 0.3376 0.3244 0.036 Uiso 1 1 calc R . .
C210 C 0.6147(3) 0.1877(2) 0.33773(15) 0.0375(7) Uani 1 1 d . . .
H21A H 0.5758 0.1669 0.3708 0.045 Uiso 1 1 calc R . .
H21B H 0.6159 0.1298 0.3074 0.045 Uiso 1 1 calc R . .
C211 C 0.7225(3) 0.2119(3) 0.37459(16) 0.0439(8) Uani 1 1 d . . .
H21C H 0.7640 0.2233 0.3420 0.066 Uiso 1 1 calc R . .
H21D H 0.7505 0.1553 0.4038 0.066 Uiso 1 1 calc R . .
H21E H 0.7228 0.2727 0.4018 0.066 Uiso 1 1 calc R . .
C212 C 0.6116(2) 0.48146(19) 0.24226(13) 0.0266(6) Uani 1 1 d . . .
H21F H 0.5930 0.5438 0.2157 0.032 Uiso 1 1 calc R . .
H21G H 0.5772 0.4835 0.2799 0.032 Uiso 1 1 calc R . .
C213 C 0.7252(2) 0.4828(2) 0.27134(15) 0.0325(6) Uani 1 1 d . . .
H21H H 0.7613 0.4651 0.2361 0.039 Uiso 1 1 calc R . .
H21I H 0.7432 0.4325 0.3078 0.039 Uiso 1 1 calc R . .
C214 C 0.7569(2) 0.5877(2) 0.29867(15) 0.0360(7) Uani 1 1 d . . .
H21J H 0.7441 0.6363 0.2610 0.043 Uiso 1 1 calc R . .
H21K H 0.7144 0.6077 0.3298 0.043 Uiso 1 1 calc R . .
C215 C 0.8679(3) 0.5937(3) 0.33534(17) 0.0449(8) Uani 1 1 d . . .
H21L H 0.8787 0.5551 0.3772 0.067 Uiso 1 1 calc R . .
H21M H 0.8867 0.6642 0.3456 0.067 Uiso 1 1 calc R . .
H21N H 0.9101 0.5655 0.3069 0.067 Uiso 1 1 calc R . .
N300 N 0.9542(2) 0.2762(2) 0.49812(15) 0.0483(7) Uani 1 1 d . . .
O300 O 1.0605(2) 0.1798(2) 0.45384(14) 0.0571(7) Uani 1 1 d . . .
C300 C 0.8913(3) 0.2885(4) 0.5464(2) 0.0629(11) Uani 1 1 d . . .
H30A H 0.8936 0.2266 0.5729 0.094 Uiso 1 1 calc R . .
H30B H 0.8212 0.3022 0.5225 0.094 Uiso 1 1 calc R . .
H30C H 0.9170 0.3450 0.5764 0.094 Uiso 1 1 calc R . .
C301 C 0.9656(3) 0.3602(3) 0.4560(3) 0.0751(14) Uani 1 1 d . . .
H30D H 1.0187 0.4053 0.4806 0.113 Uiso 1 1 calc R . .
H30E H 0.9013 0.3971 0.4433 0.113 Uiso 1 1 calc R . .
H30F H 0.9846 0.3355 0.4156 0.113 Uiso 1 1 calc R . .
C302 C 1.0038(3) 0.1925(3) 0.4929(2) 0.0536(9) Uani 1 1 d . . .
H302 H 0.9957 0.1378 0.5211 0.064 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 0.0198(2) 0.0208(2) 0.0151(2) 0.00264(15) 0.00350(16) -0.00122(16)
V2 0.0206(2) 0.0156(2) 0.0221(2) 0.00103(16) 0.00312(16) 0.00180(16)
V3 0.0174(2) 0.0238(2) 0.0187(2) -0.00188(16) 0.00612(16) 0.00052(16)
O1 0.0259(9) 0.0266(9) 0.0186(9) 0.0021(7) 0.0036(7) -0.0006(7)
O2 0.0287(10) 0.0196(9) 0.0284(10) 0.0006(7) 0.0047(8) 0.0000(7)
O3 0.0192(9) 0.0339(10) 0.0258(10) 0.0004(8) 0.0078(7) -0.0001(7)
O4 0.0232(9) 0.0190(8) 0.0222(9) 0.0057(7) 0.0031(7) -0.0010(7)
O5 0.0227(9) 0.0273(9) 0.0166(8) -0.0012(7) 0.0079(7) -0.0035(7)
O6 0.0207(9) 0.0216(9) 0.0258(9) -0.0038(7) 0.0070(7) 0.0022(7)
O7 0.0167(11) 0.0169(11) 0.0174(11) 0.0007(9) 0.0044(9) -0.0007(9)
O8 0.0163(8) 0.0212(8) 0.0186(8) 0.0006(6) 0.0026(7) -0.0005(6)
O9 0.0186(8) 0.0198(8) 0.0169(8) -0.0016(6) 0.0040(7) -0.0027(7)
O10 0.0186(8) 0.0197(8) 0.0184(8) 0.0010(7) 0.0034(7) -0.0026(7)
O11 0.0408(12) 0.0514(14) 0.0344(12) 0.0034(10) 0.0073(10) -0.0108(10)
N1 0.0261(12) 0.0311(12) 0.0246(11) 0.0020(9) 0.0018(9) -0.0106(9)
N2 0.0369(15) 0.0545(19) 0.0582(19) -0.0137(15) 0.0010(14) -0.0034(13)
C1 0.0194(12) 0.0260(13) 0.0204(12) 0.0007(10) 0.0036(10) -0.0062(10)
C2 0.0169(12) 0.0267(13) 0.0213(12) 0.0009(10) 0.0017(10) -0.0025(10)
C3 0.0253(13) 0.0229(12) 0.0209(12) -0.0025(10) 0.0041(10) -0.0045(10)
C4 0.0214(12) 0.0215(12) 0.0230(12) 0.0010(10) 0.0054(10) -0.0052(10)
C5 0.0325(15) 0.0335(15) 0.0346(16) -0.0022(12) 0.0090(13) -0.0041(12)
C6 0.0336(16) 0.0366(16) 0.0329(15) -0.0087(12) 0.0070(12) -0.0040(12)
C7 0.0418(18) 0.0399(18) 0.0426(18) -0.0053(14) 0.0078(14) -0.0042(14)
C8 0.0435(19) 0.0429(19) 0.053(2) -0.0107(16) 0.0173(16) -0.0125(15)
C9 0.0331(17) 0.048(2) 0.059(2) -0.0204(17) 0.0105(16) -0.0087(15)
C10 0.0335(16) 0.0400(17) 0.0449(18) -0.0077(14) 0.0018(14) -0.0025(13)
N200 0.0279(11) 0.0195(10) 0.0219(11) -0.0034(8) 0.0073(9) 0.0009(8)
C200 0.0296(14) 0.0240(13) 0.0205(12) -0.0017(10) 0.0077(10) -0.0017(10)
C201 0.0432(17) 0.0318(15) 0.0280(15) 0.0052(12) 0.0085(13) 0.0050(13)
C202 0.0399(17) 0.0409(17) 0.0301(15) 0.0080(13) 0.0082(13) -0.0081(13)
C203 0.042(2) 0.102(4) 0.074(3) 0.048(3) 0.010(2) -0.016(2)
C204 0.0276(14) 0.0246(13) 0.0281(14) -0.0035(11) 0.0088(11) 0.0032(11)
C205 0.0310(15) 0.0288(14) 0.0317(15) -0.0054(11) 0.0098(12) 0.0007(11)
C206 0.0313(16) 0.0397(17) 0.0487(19) -0.0099(14) 0.0078(14) -0.0016(13)
C207 0.044(2) 0.059(2) 0.070(3) 0.004(2) 0.0115(19) 0.0068(18)
C208 0.0322(14) 0.0160(11) 0.0242(13) -0.0010(9) 0.0098(11) 0.0012(10)
C209 0.0375(16) 0.0281(14) 0.0276(14) -0.0005(11) 0.0152(12) -0.0004(12)
C210 0.058(2) 0.0290(15) 0.0297(15) 0.0023(12) 0.0195(14) 0.0006(14)
C211 0.059(2) 0.0424(18) 0.0312(16) 0.0003(14) 0.0111(15) 0.0144(16)
C212 0.0382(15) 0.0181(12) 0.0230(13) -0.0060(10) 0.0060(11) -0.0018(11)
C213 0.0349(16) 0.0284(14) 0.0324(15) -0.0058(12) 0.0041(12) -0.0007(12)
C214 0.0444(18) 0.0298(15) 0.0326(15) -0.0039(12) 0.0065(13) -0.0104(13)
C215 0.0451(19) 0.0442(19) 0.0450(19) -0.0015(15) 0.0099(15) -0.0141(15)
N300 0.0401(16) 0.0546(18) 0.0504(18) 0.0010(14) 0.0110(13) 0.0088(13)
O300 0.0559(16) 0.0535(16) 0.0686(18) 0.0076(13) 0.0280(14) 0.0020(12)
C300 0.056(2) 0.088(3) 0.047(2) 0.006(2) 0.0183(19) 0.014(2)
C301 0.069(3) 0.060(3) 0.110(4) 0.025(3) 0.048(3) 0.026(2)
C302 0.047(2) 0.056(2) 0.062(2) 0.0132(18) 0.0215(18) 0.0063(17)

_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_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
V1 O1 . . 1.6049(17) Y
V1 O4 . . 1.7948(18) Y
V1 O5 . . 1.8438(18) Y
V1 O8 . . 2.0037(17) Y
V1 O9 . . 2.0408(17) Y
V1 O7 . . 2.2394(5) Y
V2 O2 . . 1.6023(18) Y
V2 O6 . . 1.7954(17) Y
V2 O4 . . 1.8570(18) Y
V2 O9 . 3_666 1.9978(17) Y
V2 O10 . . 2.0367(17) Y
V2 O7 . . 2.2440(5) Y
V2 V3 . 3_666 3.0264(6) Y
V3 O3 . . 1.6041(18) Y
V3 O5 . . 1.7998(18) Y
V3 O6 . 3_666 1.8444(18) Y
V3 O10 . . 2.0098(17) Y
V3 O8 . 3_666 2.0275(17) Y
V3 O7 . . 2.2366(5) Y
V3 V2 . 3_666 3.0265(6) Y
O6 V3 . 3_666 1.8443(18) Y
O7 V3 . 3_666 2.2365(5) Y
O7 V1 . 3_666 2.2395(5) Y
O7 V2 . 3_666 2.2440(5) Y
O8 C2 . . 1.422(3) Y
O8 V3 . 3_666 2.0274(17) Y
O9 C3 . . 1.428(3) Y
O9 V2 . 3_666 1.9979(17) Y
O10 C4 . . 1.424(3) Y
O11 C5 . . 1.241(4) Y
N1 C5 . . 1.349(4) Y
N1 C1 . . 1.474(3) Y
N1 H1 . . 0.88 ?
N2 C10 . . 1.322(4) Y
N2 C9 . . 1.340(5) Y
C1 C2 . . 1.531(4) Y
C1 C3 . . 1.532(3) Y
C1 C4 . 3_666 1.535(3) Y
C2 H2a . . 0.99 ?
C2 H2b . . 0.99 ?
C3 H3a . . 0.99 ?
C3 H3b . . 0.99 ?
C4 C1 . 3_666 1.535(3) Y
C4 H4a . . 0.99 ?
C4 H4b . . 0.99 ?
C5 C6 . . 1.503(4) Y
C6 C10 . . 1.384(4) Y
C6 C7 . . 1.392(4) Y
C7 C8 . . 1.382(4) Y
C7 H7 . . 0.95 ?
C8 C9 . . 1.371(5) Y
C8 H8 . . 0.95 ?
C9 H9 . . 0.95 ?
C10 H10 . . 0.95 ?
N200 C212 . . 1.517(3) Y
N200 C204 . . 1.518(3) Y
N200 C208 . . 1.523(3) Y
N200 C200 . . 1.525(3) Y
C200 C201 . . 1.512(4) Y
C200 H20a . . 0.99 ?
C200 H20b . . 0.99 ?
C201 C202 . . 1.517(4) Y
C201 H20c . . 0.99 ?
C201 H20d . . 0.99 ?
C202 C203 . . 1.519(5) Y
C202 H20e . . 0.99 ?
C202 H20f . . 0.99 ?
C203 H20g . . 0.98 ?
C203 H20h . . 0.98 ?
C203 H20i . . 0.98 ?
C204 C205 . . 1.521(4) Y
C204 H20j . . 0.99 ?
C204 H20k . . 0.99 ?
C205 C206 . . 1.525(4) Y
C205 H20l . . 0.99 ?
C205 H20m . . 0.99 ?
C206 C207 . . 1.487(5) Y
C206 H20n . . 0.99 ?
C206 H20o . . 0.99 ?
C207 H20p . . 0.98 ?
C207 H20q . . 0.98 ?
C207 H20r . . 0.98 ?
C208 C209 . . 1.514(3) Y
C208 H20s . . 0.99 ?
C208 H20t . . 0.99 ?
C209 C210 . . 1.535(4) Y
C209 H20u . . 0.99 ?
C209 H20v . . 0.99 ?
C210 C211 . . 1.515(5) Y
C210 H21a . . 0.99 ?
C210 H21b . . 0.99 ?
C211 H21c . . 0.98 ?
C211 H21d . . 0.98 ?
C211 H21e . . 0.98 ?
C212 C213 . . 1.515(4) Y
C212 H21f . . 0.99 ?
C212 H21g . . 0.99 ?
C213 C214 . . 1.524(4) Y
C213 H21h . . 0.99 ?
C213 H21i . . 0.99 ?
C214 C215 . . 1.520(4) Y
C214 H21j . . 0.99 ?
C214 H21k . . 0.99 ?
C215 H21l . . 0.98 ?
C215 H21m . . 0.98 ?
C215 H21n . . 0.98 ?
N300 C302 . . 1.315(5) Y
N300 C301 . . 1.440(5) Y
N300 C300 . . 1.457(4) Y
O300 C302 . . 1.243(4) Y
C300 H30a . . 0.98 ?
C300 H30b . . 0.98 ?
C300 H30c . . 0.98 ?
C301 H30d . . 0.98 ?
C301 H30e . . 0.98 ?
C301 H30f . . 0.98 ?
C302 H302 . . 0.95 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_2
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O1 V1 O4 . . . 104.56(9) Y
O1 V1 O5 . . . 102.55(9) Y
O4 V1 O5 . . . 94.17(8) Y
O1 V1 O8 . . . 98.16(8) Y
O4 V1 O8 . . . 89.09(7) Y
O5 V1 O8 . . . 157.47(7) Y
O1 V1 O9 . . . 96.07(8) Y
O4 V1 O9 . . . 158.57(7) Y
O5 V1 O9 . . . 86.82(7) Y
O8 V1 O9 . . . 82.24(7) Y
O1 V1 O7 . . . 172.20(7) Y
O4 V1 O7 . . . 82.03(6) Y
O5 V1 O7 . . . 80.83(5) Y
O8 V1 O7 . . . 77.55(5) Y
O9 V1 O7 . . . 76.99(5) Y
O2 V2 O6 . . . 104.94(9) Y
O2 V2 O4 . . . 103.41(9) Y
O6 V2 O4 . . . 93.88(8) Y
O2 V2 O9 . . 3_666 97.28(8) Y
O6 V2 O9 . . 3_666 89.83(7) Y
O4 V2 O9 . . 3_666 157.23(7) Y
O2 V2 O10 . . . 95.90(8) Y
O6 V2 O10 . . . 158.45(8) Y
O4 V2 O10 . . . 86.41(7) Y
O9 V2 O10 3_666 . . 82.06(7) Y
O2 V2 O7 . . . 171.85(7) Y
O6 V2 O7 . . . 81.65(6) Y
O4 V2 O7 . . . 80.60(5) Y
O9 V2 O7 3_666 . . 77.73(5) Y
O10 V2 O7 . . . 77.13(5) Y
O2 V2 V3 . . 3_666 138.89(7) Y
O6 V2 V3 . . 3_666 34.27(5) Y
O4 V2 V3 . . 3_666 88.50(5) Y
O9 V2 V3 3_666 . 3_666 81.98(5) Y
O10 V2 V3 . . 3_666 124.34(5) Y
O7 V2 V3 . . 3_666 47.406(12) Y
O3 V3 O5 . . . 104.24(9) Y
O3 V3 O6 . . 3_666 103.75(9) Y
O5 V3 O6 . . 3_666 93.84(8) Y
O3 V3 O10 . . . 96.74(8) Y
O5 V3 O10 . . . 89.44(7) Y
O6 V3 O10 3_666 . . 157.73(7) Y
O3 V3 O8 . . 3_666 96.38(8) Y
O5 V3 O8 . . 3_666 158.69(7) Y
O6 V3 O8 3_666 . 3_666 86.36(7) Y
O10 V3 O8 . . 3_666 82.75(7) Y
O3 V3 O7 . . . 171.95(7) Y
O5 V3 O7 . . . 81.84(6) Y
O6 V3 O7 3_666 . . 80.83(5) Y
O10 V3 O7 . . . 77.85(5) Y
O8 V3 O7 3_666 . . 77.14(5) Y
O3 V3 V2 . . 3_666 136.81(7) Y
O5 V3 V2 . . 3_666 87.43(6) Y
O6 V3 V2 3_666 . 3_666 33.24(5) Y
O10 V3 V2 . . 3_666 125.25(5) Y
O8 V3 V2 3_666 . 3_666 81.08(5) Y
O7 V3 V2 . . 3_666 47.614(12) Y
V1 O4 V2 . . . 112.23(9) Y
V3 O5 V1 . . . 112.24(9) Y
V2 O6 V3 . . 3_666 112.50(9) Y
V3 O7 V3 3_666 . . 180 Y
V3 O7 V1 3_666 . . 94.960(17) Y
V3 O7 V1 . . . 85.040(17) Y
V3 O7 V1 3_666 . 3_666 85.039(16) Y
V3 O7 V1 . . 3_666 94.961(17) Y
V1 O7 V1 . . 3_666 180 Y
V3 O7 V2 3_666 . 3_666 95.020(15) Y
V3 O7 V2 . . 3_666 84.981(15) Y
V1 O7 V2 . . 3_666 94.900(15) Y
V1 O7 V2 3_666 . 3_666 85.101(15) Y
V3 O7 V2 3_666 . . 84.979(15) Y
V3 O7 V2 . . . 95.020(15) Y
V1 O7 V2 . . . 85.101(15) Y
V1 O7 V2 3_666 . . 94.898(15) Y
V2 O7 V2 3_666 . . 180.00(2) Y
C2 O8 V1 . . . 119.16(14) Y
C2 O8 V3 . . 3_666 117.93(14) Y
V1 O8 V3 . . 3_666 109.84(8) Y
C3 O9 V2 . . 3_666 119.31(14) Y
C3 O9 V1 . . . 118.71(14) Y
V2 O9 V1 3_666 . . 109.73(8) Y
C4 O10 V3 . . . 118.76(14) Y
C4 O10 V2 . . . 118.80(14) Y
V3 O10 V2 . . . 109.47(7) Y
C5 N1 C1 . . . 123.4(2) Y
C5 N1 H1 . . . 118.3 ?
C1 N1 H1 . . . 118.3 ?
C10 N2 C9 . . . 117.0(3) Y
N1 C1 C2 . . . 108.8(2) Y
N1 C1 C3 . . . 110.1(2) Y
C2 C1 C3 . . . 111.1(2) Y
N1 C1 C4 . . 3_666 106.32(19) Y
C2 C1 C4 . . 3_666 110.5(2) Y
C3 C1 C4 . . 3_666 110.0(2) Y
O8 C2 C1 . . . 112.17(19) Y
O8 C2 H2A . . . 109.2 ?
C1 C2 H2A . . . 109.2 ?
O8 C2 H2B . . . 109.2 ?
C1 C2 H2B . . . 109.2 ?
H2A C2 H2B . . . 107.9 ?
O9 C3 C1 . . . 111.22(19) Y
O9 C3 H3A . . . 109.4 ?
C1 C3 H3A . . . 109.4 ?
O9 C3 H3B . . . 109.4 ?
C1 C3 H3B . . . 109.4 ?
H3A C3 H3B . . . 108 ?
O10 C4 C1 . . 3_666 111.56(19) Y
O10 C4 H4A . . . 109.3 ?
C1 C4 H4A 3_666 . . 109.3 ?
O10 C4 H4B . . . 109.3 ?
C1 C4 H4B 3_666 . . 109.3 ?
H4A C4 H4B . . . 108 ?
O11 C5 N1 . . . 124.2(3) Y
O11 C5 C6 . . . 119.2(3) Y
N1 C5 C6 . . . 116.6(3) Y
C10 C6 C7 . . . 118.6(3) Y
C10 C6 C5 . . . 116.9(3) Y
C7 C6 C5 . . . 124.5(3) Y
C8 C7 C6 . . . 117.6(3) Y
C8 C7 H7 . . . 121.2 ?
C6 C7 H7 . . . 121.2 ?
C9 C8 C7 . . . 119.5(3) Y
C9 C8 H8 . . . 120.3 ?
C7 C8 H8 . . . 120.3 ?
N2 C9 C8 . . . 123.4(3) Y
N2 C9 H9 . . . 118.3 ?
C8 C9 H9 . . . 118.3 ?
N2 C10 C6 . . . 123.8(3) Y
N2 C10 H10 . . . 118.1 ?
C6 C10 H10 . . . 118.1 ?
C212 N200 C204 . . . 106.24(19) Y
C212 N200 C208 . . . 110.39(19) Y
C204 N200 C208 . . . 111.5(2) Y
C212 N200 C200 . . . 111.4(2) Y
C204 N200 C200 . . . 111.6(2) Y
C208 N200 C200 . . . 105.76(18) Y
C201 C200 N200 . . . 116.2(2) Y
C201 C200 H20A . . . 108.2 ?
N200 C200 H20A . . . 108.2 ?
C201 C200 H20B . . . 108.2 ?
N200 C200 H20B . . . 108.2 ?
H20A C200 H20B . . . 107.4 ?
C200 C201 C202 . . . 110.8(2) Y
C200 C201 H20C . . . 109.5 ?
C202 C201 H20C . . . 109.5 ?
C200 C201 H20D . . . 109.5 ?
C202 C201 H20D . . . 109.5 ?
H20C C201 H20D . . . 108.1 ?
C201 C202 C203 . . . 112.2(3) Y
C201 C202 H20E . . . 109.2 ?
C203 C202 H20E . . . 109.2 ?
C201 C202 H20F . . . 109.2 ?
C203 C202 H20F . . . 109.2 ?
H20E C202 H20F . . . 107.9 ?
C202 C203 H20G . . . 109.5 ?
C202 C203 H20H . . . 109.5 ?
H20G C203 H20H . . . 109.5 ?
C202 C203 H20I . . . 109.5 ?
H20G C203 H20I . . . 109.5 ?
H20H C203 H20I . . . 109.5 ?
N200 C204 C205 . . . 116.3(2) Y
N200 C204 H20J . . . 108.2 ?
C205 C204 H20J . . . 108.2 ?
N200 C204 H20K . . . 108.2 ?
C205 C204 H20K . . . 108.2 ?
H20J C204 H20K . . . 107.4 ?
C204 C205 C206 . . . 110.8(2) Y
C204 C205 H20L . . . 109.5 ?
C206 C205 H20L . . . 109.5 ?
C204 C205 H20M . . . 109.5 ?
C206 C205 H20M . . . 109.5 ?
H20L C205 H20M . . . 108.1 ?
C207 C206 C205 . . . 116.7(3) Y
C207 C206 H20N . . . 108.1 ?
C205 C206 H20N . . . 108.1 ?
C207 C206 H20O . . . 108.1 ?
C205 C206 H20O . . . 108.1 ?
H20N C206 H20O . . . 107.3 ?
C206 C207 H20P . . . 109.5 ?
C206 C207 H20Q . . . 109.5 ?
H20P C207 H20Q . . . 109.5 ?
C206 C207 H20R . . . 109.5 ?
H20P C207 H20R . . . 109.5 ?
H20Q C207 H20R . . . 109.5 ?
C209 C208 N200 . . . 115.6(2) Y
C209 C208 H20S . . . 108.4 ?
N200 C208 H20S . . . 108.4 ?
C209 C208 H20T . . . 108.4 ?
N200 C208 H20T . . . 108.4 ?
H20S C208 H20T . . . 107.4 ?
C208 C209 C210 . . . 110.1(2) Y
C208 C209 H20U . . . 109.6 ?
C210 C209 H20U . . . 109.6 ?
C208 C209 H20V . . . 109.6 ?
C210 C209 H20V . . . 109.6 ?
H20U C209 H20V . . . 108.1 ?
C211 C210 C209 . . . 113.7(3) Y
C211 C210 H21A . . . 108.8 ?
C209 C210 H21A . . . 108.8 ?
C211 C210 H21B . . . 108.8 ?
C209 C210 H21B . . . 108.8 ?
H21A C210 H21B . . . 107.7 ?
C210 C211 H21C . . . 109.5 ?
C210 C211 H21D . . . 109.5 ?
H21C C211 H21D . . . 109.5 ?
C210 C211 H21E . . . 109.5 ?
H21C C211 H21E . . . 109.5 ?
H21D C211 H21E . . . 109.5 ?
C213 C212 N200 . . . 116.3(2) Y
C213 C212 H21F . . . 108.2 ?
N200 C212 H21F . . . 108.2 ?
C213 C212 H21G . . . 108.2 ?
N200 C212 H21G . . . 108.2 ?
H21F C212 H21G . . . 107.4 ?
C212 C213 C214 . . . 109.2(2) Y
C212 C213 H21H . . . 109.8 ?
C214 C213 H21H . . . 109.8 ?
C212 C213 H21I . . . 109.8 ?
C214 C213 H21I . . . 109.8 ?
H21H C213 H21I . . . 108.3 ?
C215 C214 C213 . . . 113.0(3) Y
C215 C214 H21J . . . 109 ?
C213 C214 H21J . . . 109 ?
C215 C214 H21K . . . 109 ?
C213 C214 H21K . . . 109 ?
H21J C214 H21K . . . 107.8 ?
C214 C215 H21L . . . 109.5 ?
C214 C215 H21M . . . 109.5 ?
H21L C215 H21M . . . 109.5 ?
C214 C215 H21N . . . 109.5 ?
H21L C215 H21N . . . 109.5 ?
H21M C215 H21N . . . 109.5 ?
C302 N300 C301 . . . 118.5(3) Y
C302 N300 C300 . . . 122.7(3) Y
C301 N300 C300 . . . 118.8(3) Y
N300 C300 H30A . . . 109.5 ?
N300 C300 H30B . . . 109.5 ?
H30A C300 H30B . . . 109.5 ?
N300 C300 H30C . . . 109.5 ?
H30A C300 H30C . . . 109.5 ?
H30B C300 H30C . . . 109.5 ?
N300 C301 H30D . . . 109.5 ?
N300 C301 H30E . . . 109.5 ?
H30D C301 H30E . . . 109.5 ?
N300 C301 H30F . . . 109.5 ?
H30D C301 H30F . . . 109.5 ?
H30E C301 H30F . . . 109.5 ?
O300 C302 N300 . . . 124.9(4) Y
O300 C302 H302 . . . 117.6 ?
N300 C302 H302 . . . 117.6 ?

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_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag

O1 V1 O4 V2 . . . . 174.08(9) ?
O5 V1 O4 V2 . . . . -81.8(1) ?
O8 V1 O4 V2 . . . . 75.88(9) ?
O9 V1 O4 V2 . . . . 10.1(3) ?
O7 V1 O4 V2 . . . . -1.67(7) ?
O2 V2 O4 V1 . . . . 174.44(10) ?
O6 V2 O4 V1 . . . . -79.19(10) ?
O9 V2 O4 V1 3_666 . . . 19.7(2) ?
O10 V2 O4 V1 . . . . 79.22(9) ?
O7 V2 O4 V1 . . . . 1.68(7) ?
V3 V2 O4 V1 3_666 . . . -45.33(8) ?
O3 V3 O5 V1 . . . . -172.8(1) ?
O6 V3 O5 V1 3_666 . . . 81.97(10) ?
O10 V3 O5 V1 . . . . -75.98(9) ?
O8 V3 O5 V1 3_666 . . . -7.8(3) ?
O7 V3 O5 V1 . . . . 1.82(7) ?
V2 V3 O5 V1 3_666 . . . 49.34(8) ?
O1 V1 O5 V3 . . . . -174.66(10) ?
O4 V1 O5 V3 . . . . 79.41(10) ?
O8 V1 O5 V3 . . . . -18.3(2) ?
O9 V1 O5 V3 . . . . -79.14(9) ?
O7 V1 O5 V3 . . . . -1.82(7) ?
O2 V2 O6 V3 . . . 3_666 -173.4(1) ?
O4 V2 O6 V3 . . . 3_666 81.6(1) ?
O9 V2 O6 V3 3_666 . . 3_666 -75.92(10) ?
O10 V2 O6 V3 . . . 3_666 -8.5(3) ?
O7 V2 O6 V3 . . . 3_666 1.71(8) ?
O5 V3 O7 V1 . . . . -1.39(6) ?
O6 V3 O7 V1 3_666 . . . -96.65(6) ?
O10 V3 O7 V1 . . . . 89.80(5) ?
O8 V3 O7 V1 3_666 . . . 175.02(5) ?
V2 V3 O7 V1 3_666 . . . -95.375(15) ?
O5 V3 O7 V1 . . . 3_666 178.61(6) ?
O6 V3 O7 V1 3_666 . . 3_666 83.35(6) ?
O10 V3 O7 V1 . . . 3_666 -90.20(5) ?
O8 V3 O7 V1 3_666 . . 3_666 -4.98(5) ?
V2 V3 O7 V1 3_666 . . 3_666 84.625(15) ?
O5 V3 O7 V2 . . . 3_666 93.99(6) ?
O6 V3 O7 V2 3_666 . . 3_666 -1.27(6) ?
O10 V3 O7 V2 . . . 3_666 -174.82(5) ?
O8 V3 O7 V2 3_666 . . 3_666 -89.60(5) ?
O5 V3 O7 V2 . . . . -86.01(6) ?
O6 V3 O7 V2 3_666 . . . 178.73(6) ?
O10 V3 O7 V2 . . . . 5.17(5) ?
O8 V3 O7 V2 3_666 . . . 90.40(5) ?
V2 V3 O7 V2 3_666 . . . 180 ?
O4 V1 O7 V3 . . . 3_666 85.80(6) ?
O5 V1 O7 V3 . . . 3_666 -178.64(6) ?
O8 V1 O7 V3 . . . 3_666 -5.03(5) ?
O9 V1 O7 V3 . . . 3_666 -89.81(5) ?
O4 V1 O7 V3 . . . . -94.20(6) ?
O5 V1 O7 V3 . . . . 1.36(6) ?
O8 V1 O7 V3 . . . . 174.97(5) ?
O9 V1 O7 V3 . . . . 90.19(5) ?
O4 V1 O7 V1 . . . 3_666 50(6) ?
O5 V1 O7 V1 . . . 3_666 145(6) ?
O8 V1 O7 V1 . . . 3_666 -41(47) ?
O9 V1 O7 V1 . . . 3_666 -126(6) ?
O4 V1 O7 V2 . . . 3_666 -178.71(6) ?
O5 V1 O7 V2 . . . 3_666 -83.16(6) ?
O8 V1 O7 V2 . . . 3_666 90.46(5) ?
O9 V1 O7 V2 . . . 3_666 5.67(5) ?
O4 V1 O7 V2 . . . . 1.29(6) ?
O5 V1 O7 V2 . . . . 96.85(6) ?
O8 V1 O7 V2 . . . . -89.54(5) ?
O9 V1 O7 V2 . . . . -174.33(5) ?
O6 V2 O7 V3 . . . 3_666 -1.30(6) ?
O4 V2 O7 V3 . . . 3_666 -96.68(6) ?
O9 V2 O7 V3 3_666 . . 3_666 90.35(5) ?
O10 V2 O7 V3 . . . 3_666 174.88(5) ?
O6 V2 O7 V3 . . . . 178.70(6) ?
O4 V2 O7 V3 . . . . 83.32(6) ?
O9 V2 O7 V3 3_666 . . . -89.65(5) ?
O10 V2 O7 V3 . . . . -5.12(5) ?
V3 V2 O7 V3 3_666 . . . 180 ?
O6 V2 O7 V1 . . . . 94.13(6) ?
O4 V2 O7 V1 . . . . -1.25(6) ?
O9 V2 O7 V1 3_666 . . . -174.22(5) ?
O10 V2 O7 V1 . . . . -89.69(5) ?
V3 V2 O7 V1 3_666 . . . 95.431(17) ?
O6 V2 O7 V1 . . . 3_666 -85.87(6) ?
O4 V2 O7 V1 . . . 3_666 178.75(6) ?
O9 V2 O7 V1 3_666 . . 3_666 5.78(5) ?
O10 V2 O7 V1 . . . 3_666 90.31(5) ?
V3 V2 O7 V1 3_666 . . 3_666 -84.568(16) ?
O1 V1 O8 C2 . . . . 38.76(17) ?
O4 V1 O8 C2 . . . . 143.34(16) ?
O5 V1 O8 C2 . . . . -118.0(2) ?
O9 V1 O8 C2 . . . . -56.31(16) ?
O7 V1 O8 C2 . . . . -134.61(16) ?
O1 V1 O8 V3 . . . 3_666 179.25(9) ?
O4 V1 O8 V3 . . . 3_666 -76.16(9) ?
O5 V1 O8 V3 . . . 3_666 22.5(2) ?
O9 V1 O8 V3 . . . 3_666 84.19(8) ?
O7 V1 O8 V3 . . . 3_666 5.88(6) ?
O1 V1 O9 C3 . . . . -41.01(17) ?
O4 V1 O9 C3 . . . . 123.4(2) ?
O5 V1 O9 C3 . . . . -143.30(16) ?
O8 V1 O9 C3 . . . . 56.44(16) ?
O7 V1 O9 C3 . . . . 135.38(16) ?
O1 V1 O9 V2 . . . 3_666 176.86(9) ?
O4 V1 O9 V2 . . . 3_666 -18.7(2) ?
O5 V1 O9 V2 . . . 3_666 74.57(8) ?
O8 V1 O9 V2 . . . 3_666 -85.69(8) ?
O7 V1 O9 V2 . . . 3_666 -6.75(6) ?
O3 V3 O10 C4 . . . . -39.01(17) ?
O5 V3 O10 C4 . . . . -143.28(16) ?
O6 V3 O10 C4 3_666 . . . 117.9(2) ?
O8 V3 O10 C4 3_666 . . . 56.60(16) ?
O7 V3 O10 C4 . . . . 134.95(16) ?
V2 V3 O10 C4 3_666 . . . 130.27(14) ?
O3 V3 O10 V2 . . . . -179.98(9) ?
O5 V3 O10 V2 . . . . 75.75(8) ?
O6 V3 O10 V2 3_666 . . . -23.0(2) ?
O8 V3 O10 V2 3_666 . . . -84.37(8) ?
O7 V3 O10 V2 . . . . -6.03(6) ?
V2 V3 O10 V2 3_666 . . . -10.71(10) ?
O2 V2 O10 C4 . . . . 40.77(17) ?
O6 V2 O10 C4 . . . . -124.6(2) ?
O4 V2 O10 C4 . . . . 143.91(16) ?
O9 V2 O10 C4 3_666 . . . -55.78(16) ?
O7 V2 O10 C4 . . . . -134.93(16) ?
V3 V2 O10 C4 3_666 . . . -130.37(14) ?
O2 V2 O10 V3 . . . . -178.27(9) ?
O6 V2 O10 V3 . . . . 16.4(2) ?
O4 V2 O10 V3 . . . . -75.14(8) ?
O9 V2 O10 V3 3_666 . . . 85.17(8) ?
O7 V2 O10 V3 . . . . 6.02(6) ?
V3 V2 O10 V3 3_666 . . . 10.59(10) ?
C5 N1 C1 C2 . . . . 54.8(3) ?
C5 N1 C1 C3 . . . . -67.1(3) ?
C5 N1 C1 C4 . . . 3_666 173.8(2) ?
V1 O8 C2 C1 . . . . 68.7(2) ?
V3 O8 C2 C1 3_666 . . . -68.6(2) ?
N1 C1 C2 O8 . . . . 178.01(19) ?
C3 C1 C2 O8 . . . . -60.7(3) ?
C4 C1 C2 O8 3_666 . . . 61.7(3) ?
V2 O9 C3 C1 3_666 . . . 70.3(2) ?
V1 O9 C3 C1 . . . . -68.2(2) ?
N1 C1 C3 O9 . . . . -178.90(19) ?
C2 C1 C3 O9 . . . . 60.5(3) ?
C4 C1 C3 O9 3_666 . . . -62.1(3) ?
V3 O10 C4 C1 . . . 3_666 -68.9(2) ?
V2 O10 C4 C1 . . . 3_666 68.4(2) ?
C1 N1 C5 O11 . . . . 10.8(5) ?
C1 N1 C5 C6 . . . . -169.5(2) ?
O11 C5 C6 C10 . . . . -35.1(4) ?
N1 C5 C6 C10 . . . . 145.2(3) ?
O11 C5 C6 C7 . . . . 143.7(3) ?
N1 C5 C6 C7 . . . . -36.0(4) ?
C10 C6 C7 C8 . . . . 2.7(5) ?
C5 C6 C7 C8 . . . . -176.2(3) ?
C6 C7 C8 C9 . . . . -1.8(5) ?
C10 N2 C9 C8 . . . . 1.4(5) ?
C7 C8 C9 N2 . . . . -0.3(5) ?
C9 N2 C10 C6 . . . . -0.4(5) ?
C7 C6 C10 N2 . . . . -1.7(5) ?
C5 C6 C10 N2 . . . . 177.3(3) ?
C212 N200 C200 C201 . . . . -56.4(3) ?
C204 N200 C200 C201 . . . . 62.2(3) ?
C208 N200 C200 C201 . . . . -176.3(2) ?
N200 C200 C201 C202 . . . . 167.6(2) ?
C200 C201 C202 C203 . . . . -70.5(4) ?
C212 N200 C204 C205 . . . . -179.8(2) ?
C208 N200 C204 C205 . . . . -59.5(3) ?
C200 N200 C204 C205 . . . . 58.5(3) ?
N200 C204 C205 C206 . . . . 165.3(2) ?
C204 C205 C206 C207 . . . . 54.0(4) ?
C212 N200 C208 C209 . . . . 64.4(3) ?
C204 N200 C208 C209 . . . . -53.4(3) ?
C200 N200 C208 C209 . . . . -174.9(2) ?
N200 C208 C209 C210 . . . . -167.5(2) ?
C208 C209 C210 C211 . . . . 71.8(3) ?
C204 N200 C212 C213 . . . . 176.0(2) ?
C208 N200 C212 C213 . . . . 55.0(3) ?
C200 N200 C212 C213 . . . . -62.2(3) ?
N200 C212 C213 C214 . . . . 165.6(2) ?
C212 C213 C214 C215 . . . . 174.1(3) ?
C301 N300 C302 O300 . . . . -0.2(6) ?
C300 N300 C302 O300 . . . . -177.8(4) ?

_diffrn_measured_fraction_theta_max 0.984
_diffrn_reflns_theta_full        27.61
_diffrn_measured_fraction_theta_full 0.984
_refine_diff_density_max         0.871
_refine_diff_density_min         -0.451
_refine_diff_density_rms         0.075