# Supplementary Material (ESI) for PCCP
# This journal is (c) the Owner Societies 2010

data_global

_journal_coden_Cambridge         1326
_journal_volume                  ?
_journal_page_first              ?
_journal_year                    ?

loop_
_publ_author_name
'Alexandre Vimont'
'Jean-Claude Lavalley'
'Arnaud Travert'
'Claude Binet'
'Pierre Mialane'
'Jerome Marrot'
'Celine Pinchon'

_publ_contact_author_name        'Alexandre Vimont'
_publ_contact_author_email       alexandre.vimont@ensicaen.fr

_publ_section_title              
;
Combined XRD and Infrared Studies of pyridinium
species in (PyH)3[PW12O40] Single Crystals
;

# Attachment '- pw12py.cif'

#====================================================================
data_1
_database_code_depnum_ccdc_archive 'CCDC 776230'
#TrackingRef '- pw12py.cif'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C19 H24 N5 O40 P W12'
_chemical_formula_weight         3199.60

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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   C2/c

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

_cell_length_a                   23.5058(4)
_cell_length_b                   14.3158(4)
_cell_length_c                   16.6984(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 119.933(2)
_cell_angle_gamma                90.00
_cell_volume                     4869.5(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    8788
_cell_measurement_theta_min      2.53
_cell_measurement_theta_max      30.13

_exptl_crystal_description       platelet
_exptl_crystal_colour            white
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.04
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    4.364
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             5584
_exptl_absorpt_coefficient_mu    28.359
_exptl_absorpt_correction_type   multi-scans
_exptl_absorpt_correction_T_min  0.0701
_exptl_absorpt_correction_T_max  0.3967
_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  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            128879
_diffrn_reflns_av_R_equivalents  0.0795
_diffrn_reflns_av_sigmaI/netI    0.0279
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         1.74
_diffrn_reflns_theta_max         30.15
_reflns_number_total             7200
_reflns_number_gt                6592
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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^)+(0.0580P)^2^+162.9977P] 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         7200
_refine_ls_number_parameters     350
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0434
_refine_ls_R_factor_gt           0.0377
_refine_ls_wR_factor_ref         0.1141
_refine_ls_wR_factor_gt          0.1027
_refine_ls_goodness_of_fit_ref   1.165
_refine_ls_restrained_S_all      1.166
_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
W1 W -0.044166(15) 0.41589(2) 0.36298(2) 0.01389(8) Uani 1 1 d . . .
W2 W 0.110409(15) 0.42185(2) 0.38972(2) 0.01377(8) Uani 1 1 d . . .
W3 W 0.068678(16) 0.24908(2) 0.49435(2) 0.01229(8) Uani 1 1 d . . .
W4 W 0.114047(15) 0.06452(2) 0.38259(2) 0.01434(8) Uani 1 1 d . . .
W5 W 0.053204(16) 0.07058(2) 0.14783(2) 0.01410(8) Uani 1 1 d . . .
W6 W 0.162819(16) 0.23678(2) 0.28756(2) 0.01559(9) Uani 1 1 d . . .
P P 0.0000 0.24314(17) 0.2500 0.0076(5) Uani 1 2 d S . .
O1 O -0.0790(3) 0.4982(5) 0.3976(5) 0.0266(14) Uani 1 1 d . . .
O2 O 0.0037(3) 0.3434(4) 0.4718(4) 0.0180(11) Uani 1 1 d . . .
O3 O -0.0736(3) 0.4510(4) 0.2366(4) 0.0176(11) Uani 1 1 d . . .
O4 O -0.1094(3) 0.3220(4) 0.3100(4) 0.0192(12) Uani 1 1 d . . .
O5 O 0.0372(3) 0.4759(4) 0.3912(4) 0.0170(11) Uani 1 1 d . . .
O6 O 0.0237(3) 0.3051(4) 0.3362(4) 0.0138(10) Uani 1 1 d . . .
O7 O 0.1688(3) 0.5054(5) 0.4453(5) 0.0245(13) Uani 1 1 d . . .
O8 O 0.1561(3) 0.3230(4) 0.3674(4) 0.0190(11) Uani 1 1 d . . .
O9 O 0.1238(3) 0.3472(4) 0.4958(4) 0.0159(11) Uani 1 1 d . . .
O10 O 0.1010(4) 0.2300(5) 0.6104(5) 0.0248(13) Uani 1 1 d . . .
O11 O 0.1131(3) 0.1614(4) 0.4619(4) 0.0186(12) Uani 1 1 d . . .
O12 O -0.0044(3) 0.1636(4) 0.4392(4) 0.0189(12) Uani 1 1 d . . .
O13 O 0.1616(3) -0.0193(5) 0.4579(5) 0.0241(13) Uani 1 1 d . . .
O14 O 0.0938(3) 0.0089(4) 0.2674(4) 0.0179(11) Uani 1 1 d . . .
O15 O 0.0289(3) 0.0340(4) 0.3608(4) 0.0189(12) Uani 1 1 d . . .
O16 O 0.1793(3) 0.1383(4) 0.3735(4) 0.0184(11) Uani 1 1 d . . .
O17 O 0.0570(3) 0.1811(4) 0.2615(4) 0.0151(10) Uani 1 1 d . . .
O18 O 0.0646(3) -0.0125(5) 0.0848(5) 0.0267(14) Uani 1 1 d . . .
O19 O 0.1316(3) 0.1410(4) 0.1930(4) 0.0200(12) Uani 1 1 d . . .
O20 O 0.2389(4) 0.2558(5) 0.3042(6) 0.0263(15) Uani 1 1 d . . .
C1A C 0.2812(6) 0.4571(8) 0.3259(7) 0.036(2) Uani 1 1 d . . .
H1A H 0.3052 0.4238 0.3806 0.044 Uiso 1 1 calc R . .
C2A C 0.2824(6) 0.4297(8) 0.2477(9) 0.036(3) Uani 1 1 d . . .
H2A H 0.3067 0.3781 0.2485 0.043 Uiso 1 1 calc R . .
C3A C 0.2459(6) 0.4821(9) 0.1671(8) 0.040(3) Uani 1 1 d D . .
H3A H 0.2458 0.4658 0.1131 0.048 Uiso 1 1 calc R . .
N4A N 0.2114(5) 0.5554(7) 0.1683(7) 0.040(2) Uani 1 1 d D . .
H4A H 0.1895 0.5868 0.1181 0.048 Uiso 1 1 calc R . .
C5A C 0.2091(6) 0.5829(9) 0.2433(9) 0.040(3) Uani 1 1 d . . .
H5A H 0.1841 0.6343 0.2408 0.048 Uiso 1 1 calc R . .
C6A C 0.2445(6) 0.5337(10) 0.3238(8) 0.041(3) Uani 1 1 d . . .
H6A H 0.2439 0.5518 0.3769 0.050 Uiso 1 1 calc R . .
C1B C 1.0000 0.6572(10) 0.2500 0.034(3) Uani 1 2 d S . .
H1B H 1.0000 0.5922 0.2500 0.040 Uiso 1 2 calc SR . .
C2B C 0.9890(7) 0.7037(7) 0.3122(10) 0.041(3) Uani 1 1 d D . .
H2B H 0.9814 0.6713 0.3542 0.049 Uiso 1 1 calc R . .
C3B C 0.9894(8) 0.7991(7) 0.3115(11) 0.046(3) Uani 1 1 d D . .
H3B H 0.9824 0.8324 0.3535 0.056 Uiso 1 1 calc R . .
N4B N 1.0000 0.8444(10) 0.2500 0.042(3) Uani 1 2 d S . .
H4B H 1.0000 0.9044 0.2500 0.050 Uiso 1 2 calc SR . .
N1 N 0.1719(13) 0.7507(15) 0.3777(18) 0.106(8) Uani 1 1 d . . .
C2 C 0.1648(12) 0.7478(15) 0.444(3) 0.097(9) Uani 1 1 d . . .
C3 C 0.1589(14) 0.7448(15) 0.5214(19) 0.091(8) Uani 1 1 d . . .
H3C H 0.2017 0.7420 0.5754 0.136 Uiso 1 1 calc R . .
H3D H 0.1342 0.6905 0.5192 0.136 Uiso 1 1 calc R . .
H3E H 0.1366 0.7999 0.5241 0.136 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
W1 0.01947(15) 0.01096(15) 0.01515(15) -0.00273(10) 0.01158(12) 0.00108(10)
W2 0.01807(15) 0.01028(15) 0.01389(15) -0.00331(10) 0.00867(12) -0.00300(10)
W3 0.01809(16) 0.00992(15) 0.01034(15) -0.00026(9) 0.00821(12) -0.00051(9)
W4 0.01784(15) 0.01062(15) 0.01408(15) 0.00237(10) 0.00760(12) 0.00309(10)
W5 0.01952(15) 0.01017(15) 0.01494(15) -0.00291(10) 0.01035(12) 0.00138(10)
W6 0.01471(15) 0.01510(16) 0.01981(17) -0.00137(11) 0.01076(13) 0.00016(10)
P 0.0126(11) 0.0031(11) 0.0076(11) 0.000 0.0055(9) 0.000
O1 0.036(4) 0.024(3) 0.029(3) -0.003(3) 0.023(3) 0.006(3)
O2 0.023(3) 0.010(3) 0.023(3) 0.001(2) 0.012(2) 0.003(2)
O3 0.027(3) 0.014(3) 0.016(3) 0.001(2) 0.013(2) -0.001(2)
O4 0.025(3) 0.018(3) 0.018(3) -0.001(2) 0.013(2) -0.002(2)
O5 0.023(3) 0.008(3) 0.021(3) -0.002(2) 0.013(2) -0.001(2)
O6 0.018(2) 0.009(2) 0.016(2) -0.0009(19) 0.009(2) -0.0004(19)
O7 0.029(3) 0.018(3) 0.026(3) -0.008(2) 0.013(3) -0.012(2)
O8 0.026(3) 0.019(3) 0.015(3) 0.000(2) 0.013(2) 0.004(2)
O9 0.022(3) 0.015(3) 0.016(3) 0.000(2) 0.013(2) -0.003(2)
O10 0.029(3) 0.030(3) 0.017(3) 0.001(3) 0.013(3) -0.003(3)
O11 0.024(3) 0.012(3) 0.025(3) -0.002(2) 0.016(2) 0.002(2)
O12 0.027(3) 0.012(3) 0.024(3) 0.000(2) 0.017(3) -0.004(2)
O13 0.027(3) 0.018(3) 0.024(3) 0.006(2) 0.010(3) 0.004(2)
O14 0.026(3) 0.015(3) 0.014(3) 0.002(2) 0.010(2) 0.005(2)
O15 0.020(3) 0.011(3) 0.026(3) -0.001(2) 0.012(2) 0.000(2)
O16 0.018(3) 0.018(3) 0.018(3) 0.001(2) 0.009(2) -0.001(2)
O17 0.015(2) 0.010(2) 0.020(3) 0.002(2) 0.009(2) 0.0049(19)
O18 0.030(3) 0.019(3) 0.031(3) -0.008(3) 0.016(3) 0.005(3)
O19 0.025(3) 0.014(3) 0.023(3) -0.002(2) 0.013(2) 0.001(2)
O20 0.021(3) 0.025(4) 0.039(4) -0.004(3) 0.020(3) -0.002(2)
C1A 0.045(6) 0.033(6) 0.020(4) 0.007(4) 0.009(4) -0.009(5)
C2A 0.033(5) 0.027(5) 0.046(6) -0.004(4) 0.017(5) -0.012(4)
C3A 0.043(6) 0.048(7) 0.028(5) -0.002(5) 0.018(5) -0.023(5)
N4A 0.030(4) 0.037(5) 0.034(5) 0.013(4) 0.001(4) -0.007(4)
C5A 0.033(5) 0.043(7) 0.041(6) 0.002(5) 0.016(5) -0.011(5)
C6A 0.046(6) 0.052(8) 0.030(5) -0.008(5) 0.022(5) -0.020(6)
C1B 0.057(10) 0.011(6) 0.047(9) 0.000 0.037(8) 0.000
C2B 0.066(8) 0.020(5) 0.061(8) 0.005(5) 0.051(7) -0.003(5)
C3B 0.078(9) 0.020(5) 0.073(9) -0.008(5) 0.061(8) 0.004(5)
N4B 0.063(9) 0.021(6) 0.066(10) 0.000 0.051(9) 0.000
N1 0.102(19) 0.12(2) 0.079(15) -0.001(11) 0.029(14) 0.005(11)
C2 0.058(13) 0.075(16) 0.11(2) -0.002(13) 0.011(14) 0.005(9)
C3 0.096(19) 0.10(2) 0.077(16) 0.015(11) 0.045(14) 0.011(12)

_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
W1 O1 1.693(6) . ?
W1 O4 1.894(6) . ?
W1 O2 1.899(6) . ?
W1 O5 1.928(6) . ?
W1 O3 1.930(6) . ?
W1 O6 2.443(6) . ?
W2 O7 1.704(6) . ?
W2 O3 1.885(6) 2 ?
W2 O5 1.899(6) . ?
W2 O8 1.922(6) . ?
W2 O9 1.955(6) . ?
W2 O6 2.436(5) . ?
W3 O10 1.713(7) . ?
W3 O11 1.877(6) . ?
W3 O9 1.903(6) . ?
W3 O12 1.928(6) . ?
W3 O2 1.931(6) . ?
W3 O6 2.438(6) . ?
W4 O13 1.694(6) . ?
W4 O15 1.898(6) . ?
W4 O14 1.911(6) . ?
W4 O11 1.925(6) . ?
W4 O16 1.930(6) . ?
W4 O17 2.442(5) . ?
W5 O18 1.696(6) . ?
W5 O12 1.881(6) 2 ?
W5 O19 1.897(6) . ?
W5 O15 1.934(6) 2 ?
W5 O14 1.942(6) . ?
W5 O17 2.439(6) . ?
W6 O20 1.690(7) . ?
W6 O8 1.880(6) . ?
W6 O16 1.909(6) . ?
W6 O4 1.918(6) 2 ?
W6 O19 1.938(6) . ?
W6 O17 2.437(6) . ?
P O17 1.537(5) . ?
P O17 1.537(5) 2 ?
P O6 1.540(6) 2 ?
P O6 1.540(6) . ?
O3 W2 1.885(6) 2 ?
O4 W6 1.918(6) 2 ?
O12 W5 1.881(6) 2 ?
O15 W5 1.934(6) 2 ?
C1A C2A 1.376(17) . ?
C1A C6A 1.385(19) . ?
C1A H1A 0.9300 . ?
C2A C3A 1.399(17) . ?
C2A H2A 0.9300 . ?
C3A N4A 1.332(14) . ?
C3A H3A 0.9300 . ?
N4A C5A 1.340(17) . ?
N4A H4A 0.8600 . ?
C5A C6A 1.371(18) . ?
C5A H5A 0.9300 . ?
C6A H6A 0.9300 . ?
C1B C2B 1.363(13) . ?
C1B C2B 1.363(13) 2_755 ?
C1B H1B 0.9300 . ?
C2B C3B 1.365(13) . ?
C2B H2B 0.9300 . ?
C3B N4B 1.338(14) . ?
C3B H3B 0.9300 . ?
N4B C3B 1.338(14) 2_755 ?
N4B H4B 0.8600 . ?
N1 C2 1.20(4) . ?
C2 C3 1.37(5) . ?
C3 H3C 0.9600 . ?
C3 H3D 0.9600 . ?
C3 H3E 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 W1 O4 103.7(3) . . ?
O1 W1 O2 102.1(3) . . ?
O4 W1 O2 90.8(3) . . ?
O1 W1 O5 101.3(3) . . ?
O4 W1 O5 154.6(3) . . ?
O2 W1 O5 88.1(3) . . ?
O1 W1 O3 102.8(3) . . ?
O4 W1 O3 84.8(3) . . ?
O2 W1 O3 155.1(3) . . ?
O5 W1 O3 85.6(3) . . ?
O1 W1 O6 170.2(3) . . ?
O4 W1 O6 84.5(2) . . ?
O2 W1 O6 72.0(2) . . ?
O5 W1 O6 71.1(2) . . ?
O3 W1 O6 83.1(2) . . ?
O7 W2 O3 104.4(3) . 2 ?
O7 W2 O5 101.2(3) . . ?
O3 W2 O5 90.7(3) 2 . ?
O7 W2 O8 104.3(3) . . ?
O3 W2 O8 86.2(3) 2 . ?
O5 W2 O8 154.2(3) . . ?
O7 W2 O9 99.7(3) . . ?
O3 W2 O9 155.7(3) 2 . ?
O5 W2 O9 87.0(2) . . ?
O8 W2 O9 85.4(2) . . ?
O7 W2 O6 168.7(3) . . ?
O3 W2 O6 84.8(2) 2 . ?
O5 W2 O6 71.7(2) . . ?
O8 W2 O6 82.5(2) . . ?
O9 W2 O6 71.6(2) . . ?
O10 W3 O11 102.9(3) . . ?
O10 W3 O9 100.9(3) . . ?
O11 W3 O9 91.4(3) . . ?
O10 W3 O12 103.0(3) . . ?
O11 W3 O12 86.0(3) . . ?
O9 W3 O12 155.9(3) . . ?
O10 W3 O2 101.1(3) . . ?
O11 W3 O2 155.8(3) . . ?
O9 W3 O2 87.3(3) . . ?
O12 W3 O2 85.5(3) . . ?
O10 W3 O6 169.9(3) . . ?
O11 W3 O6 84.9(2) . . ?
O9 W3 O6 72.3(2) . . ?
O12 W3 O6 83.7(2) . . ?
O2 W3 O6 71.7(2) . . ?
O13 W4 O15 102.8(3) . . ?
O13 W4 O14 101.1(3) . . ?
O15 W4 O14 90.1(3) . . ?
O13 W4 O11 103.3(3) . . ?
O15 W4 O11 85.7(3) . . ?
O14 W4 O11 155.6(3) . . ?
O13 W4 O16 100.9(3) . . ?
O15 W4 O16 156.2(3) . . ?
O14 W4 O16 87.5(3) . . ?
O11 W4 O16 86.7(3) . . ?
O13 W4 O17 170.1(3) . . ?
O15 W4 O17 84.7(2) . . ?
O14 W4 O17 72.1(2) . . ?
O11 W4 O17 83.5(2) . . ?
O16 W4 O17 72.0(2) . . ?
O18 W5 O12 104.0(3) . 2 ?
O18 W5 O19 101.3(3) . . ?
O12 W5 O19 91.6(3) 2 . ?
O18 W5 O15 103.0(3) . 2 ?
O12 W5 O15 86.2(3) 2 2 ?
O19 W5 O15 155.4(3) . 2 ?
O18 W5 O14 99.8(3) . . ?
O12 W5 O14 156.0(3) 2 . ?
O19 W5 O14 87.2(3) . . ?
O15 W5 O14 85.1(3) 2 . ?
O18 W5 O17 169.3(3) . . ?
O12 W5 O17 85.0(2) 2 . ?
O19 W5 O17 72.2(2) . . ?
O15 W5 O17 83.2(2) 2 . ?
O14 W5 O17 71.7(2) . . ?
O20 W6 O8 103.6(3) . . ?
O20 W6 O16 101.2(3) . . ?
O8 W6 O16 90.5(3) . . ?
O20 W6 O4 103.2(3) . 2 ?
O8 W6 O4 86.2(3) . 2 ?
O16 W6 O4 155.5(3) . 2 ?
O20 W6 O19 100.8(3) . . ?
O8 W6 O19 155.6(3) . . ?
O16 W6 O19 86.7(3) . . ?
O4 W6 O19 86.4(3) 2 . ?
O20 W6 O17 170.1(3) . . ?
O8 W6 O17 84.3(2) . . ?
O16 W6 O17 72.5(2) . . ?
O4 W6 O17 83.0(2) 2 . ?
O19 W6 O17 71.7(2) . . ?
O17 P O17 109.4(5) . 2 ?
O17 P O6 109.6(3) . 2 ?
O17 P O6 109.3(3) 2 2 ?
O17 P O6 109.3(3) . . ?
O17 P O6 109.6(3) 2 . ?
O6 P O6 109.7(4) 2 . ?
W1 O2 W3 127.0(3) . . ?
W2 O3 W1 151.6(4) 2 . ?
W1 O4 W6 152.0(3) . 2 ?
W2 O5 W1 127.6(3) . . ?
P O6 W2 125.7(3) . . ?
P O6 W3 125.6(3) . . ?
W2 O6 W3 89.84(18) . . ?
P O6 W1 125.5(3) . . ?
W2 O6 W1 89.47(18) . . ?
W3 O6 W1 89.19(18) . . ?
W6 O8 W2 150.9(3) . . ?
W3 O9 W2 126.3(3) . . ?
W3 O11 W4 151.5(4) . . ?
W5 O12 W3 150.8(3) 2 . ?
W4 O14 W5 126.4(3) . . ?
W4 O15 W5 150.4(4) . 2 ?
W6 O16 W4 126.3(3) . . ?
P O17 W6 125.6(3) . . ?
P O17 W5 125.9(3) . . ?
W6 O17 W5 89.32(18) . . ?
P O17 W4 125.7(3) . . ?
W6 O17 W4 89.17(18) . . ?
W5 O17 W4 89.57(18) . . ?
W5 O19 W6 126.7(3) . . ?
C2A C1A C6A 120.6(11) . . ?
C2A C1A H1A 119.7 . . ?
C6A C1A H1A 119.7 . . ?
C1A C2A C3A 117.9(12) . . ?
C1A C2A H2A 121.1 . . ?
C3A C2A H2A 121.1 . . ?
N4A C3A C2A 119.6(11) . . ?
N4A C3A H3A 120.2 . . ?
C2A C3A H3A 120.2 . . ?
C3A N4A C5A 123.6(11) . . ?
C3A N4A H4A 118.2 . . ?
C5A N4A H4A 118.2 . . ?
N4A C5A C6A 118.6(13) . . ?
N4A C5A H5A 120.7 . . ?
C6A C5A H5A 120.7 . . ?
C5A C6A C1A 119.8(11) . . ?
C5A C6A H6A 120.1 . . ?
C1A C6A H6A 120.1 . . ?
C2B C1B C2B 121.5(13) . 2_755 ?
C2B C1B H1B 119.3 . . ?
C2B C1B H1B 119.3 2_755 . ?
C1B C2B C3B 118.4(10) . . ?
C1B C2B H2B 120.8 . . ?
C3B C2B H2B 120.8 . . ?
N4B C3B C2B 119.8(10) . . ?
N4B C3B H3B 120.1 . . ?
C2B C3B H3B 120.1 . . ?
C3B N4B C3B 122.0(14) 2_755 . ?
C3B N4B H4B 119.0 2_755 . ?
C3B N4B H4B 119.0 . . ?
N1 C2 C3 178(3) . . ?
C2 C3 H3C 109.5 . . ?
C2 C3 H3D 109.5 . . ?
H3C C3 H3D 109.5 . . ?
C2 C3 H3E 109.5 . . ?
H3C C3 H3E 109.5 . . ?
H3D C3 H3E 109.5 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N4A H4A O9 0.86 2.07 2.926(11) 171.2 6_565
N4B H4B O15 0.86 2.46 3.162(14) 138.8 1_665
N4B H4B O15 0.86 2.46 3.162(14) 138.8 2_665
N4B H4B O14 0.86 2.56 3.140(12) 125.8 1_665
N4B H4B O14 0.86 2.56 3.140(12) 125.8 2_665

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        30.15
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         3.839
_refine_diff_density_min         -4.651
_refine_diff_density_rms         0.937

#====================================================================

data_2
_database_code_depnum_ccdc_archive 'CCDC 776231'
#TrackingRef '- pw12py.cif'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C15 H18 N3 O40 P W12'
_chemical_formula_weight         3117.49

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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
W W -0.8490 6.8722 '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)/n

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

_cell_length_a                   12.216(3)
_cell_length_b                   14.035(3)
_cell_length_c                   12.988(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 98.045(13)
_cell_angle_gamma                90.00
_cell_volume                     2205.1(8)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    1058
_cell_measurement_theta_min      2.14
_cell_measurement_theta_max      20.47

_exptl_crystal_description       platelet
_exptl_crystal_colour            white
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.03
_exptl_crystal_density_meas      0
_exptl_crystal_density_diffrn    4.695
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2704
_exptl_absorpt_coefficient_mu    31.306
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.1458
_exptl_absorpt_correction_T_max  0.4535
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      296(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  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            24722
_diffrn_reflns_av_R_equivalents  0.3949
_diffrn_reflns_av_sigmaI/netI    0.2922
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         2.14
_diffrn_reflns_theta_max         25.00
_reflns_number_total             3887
_reflns_number_gt                1471
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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^)+(0.1516P)^2^+0.0000P] 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         3887
_refine_ls_number_parameters     265
_refine_ls_number_restraints     170
_refine_ls_R_factor_all          0.2909
_refine_ls_R_factor_gt           0.1145
_refine_ls_wR_factor_ref         0.3095
_refine_ls_wR_factor_gt          0.2535
_refine_ls_goodness_of_fit_ref   0.947
_refine_ls_restrained_S_all      0.932
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.001

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
W1 W 0.89534(9) -0.21907(6) 0.88501(9) 0.0389(3) Uani 1 1 d U . .
W2 W 0.92482(9) -0.01781(7) 0.72539(8) 0.0417(3) Uani 1 1 d U . .
W3 W 0.71729(8) -0.02001(7) 0.89218(9) 0.0428(3) Uani 1 1 d DU . .
W4 W 0.82042(9) 0.19969(7) 1.00540(9) 0.0395(3) Uani 1 1 d U . .
W5 W 1.02976(9) 0.20099(6) 0.84072(9) 0.0418(3) Uani 1 1 d U . .
W6 W 1.20884(9) 0.00163(8) 0.83466(9) 0.0437(3) Uani 1 1 d DU . .
P P 1.0000 0.0000 1.0000 0.030 Uiso 1 2 d SU . .
O1 O 0.8530(18) -0.3241(11) 0.8361(15) 0.078(6) Uani 1 1 d U . .
O2 O 0.7723(13) -0.1432(10) 0.8882(12) 0.0408(10) Uani 1 1 d U . .
O3 O 1.0961(15) 0.2418(10) 0.9697(14) 0.059(2) Uani 1 1 d U . .
O4 O 0.9226(12) -0.1493(11) 0.7650(12) 0.0414(17) Uani 1 1 d U . .
O5 O 0.9202(13) 0.2180(11) 1.0972(12) 0.045(2) Uani 1 1 d U . .
O6 O 0.8652(15) -0.0227(10) 0.6153(13) 0.054(2) Uani 1 1 d U . .
O7 O 0.9560(14) 0.1183(11) 0.7366(12) 0.0498(15) Uani 1 1 d U . .
O8 O 1.0994(14) -0.0215(10) 0.7342(13) 0.0425(17) Uani 1 1 d U . .
O9 O 0.7672(14) -0.0019(11) 0.7731(14) 0.0541(12) Uani 1 1 d U . .
O10 O 0.7099(11) -0.0406(9) 1.0352(5) 0.0445(12) Uani 1 1 d DU . .
O11 O 0.5764(14) -0.0290(11) 0.8450(14) 0.060(3) Uani 1 1 d U . .
O12 O 0.7383(16) 0.1095(11) 0.9195(14) 0.0641(19) Uani 1 1 d U . .
O13 O 0.7285(14) 0.2918(11) 1.0090(13) 0.0541(12) Uani 1 1 d U . .
O14 O 0.8862(14) 0.2257(10) 0.8997(12) 0.0462(12) Uani 1 1 d U . .
O15 O 0.7797(14) 0.1272(10) 1.1318(12) 0.0462(12) Uani 1 1 d U . .
O16 O 1.0528(14) 0.2884(12) 0.7680(15) 0.076(2) Uani 1 1 d U . .
O17 O 1.1673(14) 0.1228(11) 0.8315(14) 0.0560(19) Uani 1 1 d U . .
O18 O 1.2975(15) 0.0033(11) 0.7652(13) 0.048(3) Uani 1 1 d U . .
O19 O 0.926(3) -0.054(2) 0.910(2) 0.0408(10) Uani 0.50 1 d PU . .
O20 O 1.000(3) 0.112(2) 0.991(2) 0.0445(12) Uani 0.50 1 d PU . .
O21 O 1.019(3) 0.0380(19) 0.883(2) 0.0365(10) Uani 0.50 1 d PU . .
O22 O 0.887(3) 0.041(2) 1.010(3) 0.0586(16) Uani 0.50 1 d PU . .
C1A C 0.5024(6) 0.1741(5) 0.9804(5) 0.087(11) Uiso 1 1 d DU . .
H1A H 0.5544 0.1277 1.0038 0.104 Uiso 1 1 calc R . .
C2A C 0.4648(6) 0.1828(5) 0.8751(5) 0.060(8) Uiso 1 1 d DU . .
H2A H 0.4911 0.1425 0.8272 0.072 Uiso 1 1 calc R . .
C3A C 0.3868(6) 0.2529(5) 0.8421(6) 0.17(2) Uiso 1 1 d DU . .
H3A H 0.3624 0.2598 0.7714 0.208 Uiso 1 1 calc R . .
C4A C 0.3446(9) 0.3129(8) 0.9127(5) 0.094(12) Uiso 1 1 d DU . .
H4A H 0.2895 0.3570 0.8903 0.113 Uiso 1 1 calc R . .
C5A C 0.3870(7) 0.3049(6) 1.0173(7) 0.096(12) Uiso 1 1 d DU . .
H5A H 0.3644 0.3473 1.0651 0.116 Uiso 1 1 calc R . .
N6A N 0.4626(8) 0.2345(6) 1.0509(5) 0.23(2) Uiso 1 1 d DU . .
H6A H 0.4852 0.2281 1.1163 0.272 Uiso 1 1 calc R . .
C1B C 0.5805(5) -0.0256(5) 0.5815(5) 0.083(9) Uiso 0.50 1 d P . .
N1B N 0.5805(5) -0.0256(5) 0.5815(5) 0.083(9) Uiso 0.50 1 d PDU . .
H1B H 0.6308 -0.0412 0.6318 0.100 Uiso 1 1 calc R . .
C2B C 0.4724(5) -0.0125(5) 0.5995(6) 0.037(6) Uiso 1 1 d DU . .
H2B H 0.4535 -0.0210 0.6658 0.044 Uiso 1 1 calc R . .
C3B C 0.3929(5) 0.0135(6) 0.5178(4) 0.070(9) Uiso 1 1 d DU . .
H3B H 0.3204 0.0230 0.5298 0.085 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
W1 0.0476(6) 0.0187(4) 0.0453(7) -0.0048(4) -0.0117(5) -0.0055(4)
W2 0.0562(6) 0.0306(5) 0.0319(6) -0.0018(4) -0.0159(5) 0.0040(5)
W3 0.0338(5) 0.0340(5) 0.0532(7) 0.0043(5) -0.0192(5) -0.0023(5)
W4 0.0437(6) 0.0221(4) 0.0490(7) -0.0026(4) -0.0070(5) 0.0038(4)
W5 0.0555(6) 0.0184(4) 0.0467(7) 0.0061(4) -0.0096(6) -0.0064(5)
W6 0.0466(6) 0.0372(5) 0.0492(7) -0.0071(5) 0.0136(5) -0.0053(5)
O1 0.112(13) 0.031(3) 0.093(12) -0.042(4) 0.024(8) -0.026(4)
O2 0.049(2) 0.0295(15) 0.0418(18) -0.0007(15) -0.0005(18) -0.0028(15)
O3 0.071(4) 0.019(3) 0.076(3) -0.017(3) -0.024(4) 0.004(3)
O4 0.044(4) 0.033(2) 0.043(3) -0.0015(19) -0.007(3) 0.007(2)
O5 0.049(4) 0.047(4) 0.035(3) -0.009(4) -0.002(3) 0.029(3)
O6 0.082(4) 0.030(5) 0.041(2) 0.004(3) -0.019(3) -0.014(6)
O7 0.075(3) 0.028(2) 0.040(2) -0.0056(18) -0.013(3) 0.009(2)
O8 0.0639(19) 0.023(4) 0.040(3) 0.000(3) 0.005(2) 0.006(3)
O9 0.0590(18) 0.043(2) 0.055(2) 0.006(2) -0.0106(17) 0.0198(19)
O10 0.066(3) 0.023(2) 0.0425(16) -0.0036(13) -0.0022(18) 0.0107(18)
O11 0.047(3) 0.040(6) 0.082(5) 0.039(7) -0.029(3) -0.007(3)
O12 0.110(4) 0.032(2) 0.042(3) 0.004(2) -0.018(3) -0.016(2)
O13 0.0590(18) 0.043(2) 0.055(2) 0.006(2) -0.0106(17) 0.0198(19)
O14 0.067(2) 0.028(3) 0.038(2) -0.0034(19) -0.0100(17) 0.0097(19)
O15 0.067(2) 0.028(3) 0.038(2) -0.0034(19) -0.0100(17) 0.0097(19)
O16 0.043(5) 0.062(3) 0.112(3) 0.054(3) -0.024(4) -0.028(3)
O17 0.058(2) 0.035(3) 0.074(5) -0.013(3) 0.006(2) -0.0103(19)
O18 0.075(3) 0.037(7) 0.035(6) -0.009(6) 0.019(3) -0.015(4)
O19 0.049(2) 0.0295(15) 0.0418(18) -0.0007(15) -0.0005(18) -0.0028(15)
O20 0.066(3) 0.023(2) 0.0425(16) -0.0036(13) -0.0022(18) 0.0107(18)
O21 0.054(2) 0.0176(17) 0.0356(19) -0.0024(15) -0.0021(15) 0.0014(17)
O22 0.079(3) 0.028(2) 0.074(4) 0.007(2) 0.029(2) 0.012(2)

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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
W1 O1 1.659(16) . ?
W1 O2 1.847(16) . ?
W1 O3 1.902(18) 3_757 ?
W1 O4 1.908(16) . ?
W1 O5 2.233(16) 3_757 ?
W1 O19 2.36(3) . ?
W1 O20 2.43(3) 3_757 ?
W2 O6 1.513(16) . ?
W2 O4 1.918(15) . ?
W2 O7 1.950(15) . ?
W2 O9 2.115(18) . ?
W2 O8 2.121(17) . ?
W2 O21 2.34(3) . ?
W2 O19 2.45(3) . ?
W3 O11 1.748(16) . ?
W3 O9 1.759(19) . ?
W3 O2 1.858(15) . ?
W3 O12 1.863(16) . ?
W3 O10 1.894(7) . ?
W4 O5 1.603(15) . ?
W4 O13 1.717(17) . ?
W4 O14 1.724(18) . ?
W4 O12 1.882(17) . ?
W4 O15 2.051(16) . ?
W4 O22 2.37(3) . ?
W5 O16 1.598(18) . ?
W5 O3 1.847(16) . ?
W5 O7 1.909(15) . ?
W5 O17 2.025(17) . ?
W5 O14 2.039(18) . ?
W5 O21 2.36(3) . ?
W5 O20 2.38(3) . ?
W6 O18 1.503(19) . ?
W6 O8 1.762(16) . ?
W6 O17 1.773(16) . ?
W6 O15 1.861(15) 3_757 ?
W6 O10 1.917(8) 3_757 ?
W6 O21 2.54(3) . ?
P O22 1.52(4) 3_757 ?
P O22 1.52(4) . ?
P O19 1.57(3) . ?
P O19 1.57(3) 3_757 ?
P O20 1.58(3) . ?
P O20 1.58(3) 3_757 ?
P O21 1.65(3) . ?
P O21 1.65(3) 3_757 ?
O3 W1 1.902(18) 3_757 ?
O5 W1 2.233(16) 3_757 ?
O10 W6 1.917(8) 3_757 ?
O15 W6 1.861(15) 3_757 ?
O19 O20 1.68(4) 3_757 ?
O19 O21 1.79(4) . ?
O20 O19 1.68(4) 3_757 ?
O20 O22 1.74(5) . ?
O20 O21 1.78(4) . ?
O20 W1 2.43(3) 3_757 ?
C1A N6A 1.385(9) . ?
C1A C2A 1.386(8) . ?
C1A H1A 0.9300 . ?
C2A C3A 1.395(9) . ?
C2A H2A 0.9300 . ?
C3A C4A 1.396(11) . ?
C3A H3A 0.9300 . ?
C4A C5A 1.390(10) . ?
C4A H4A 0.9300 . ?
C5A N6A 1.381(10) . ?
C5A H5A 0.9300 . ?
N6A H6A 0.8600 . ?
C1B C3B 1.384(7) 3_656 ?
C2B C3B 1.384(8) . ?
C2B H2B 0.9300 . ?
C3B N1B 1.384(7) 3_656 ?
C3B H3B 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 W1 O2 108.1(9) . . ?
O1 W1 O3 101.6(8) . 3_757 ?
O2 W1 O3 90.4(7) . 3_757 ?
O1 W1 O4 102.9(8) . . ?
O2 W1 O4 87.6(7) . . ?
O3 W1 O4 154.7(6) 3_757 . ?
O1 W1 O5 107.5(8) . 3_757 ?
O2 W1 O5 143.7(6) . 3_757 ?
O3 W1 O5 89.1(7) 3_757 3_757 ?
O4 W1 O5 78.0(6) . 3_757 ?
O1 W1 O19 163.6(10) . . ?
O2 W1 O19 62.8(9) . . ?
O3 W1 O19 92.3(9) 3_757 . ?
O4 W1 O19 64.5(9) . . ?
O5 W1 O19 81.0(9) 3_757 . ?
O1 W1 O20 155.4(9) . 3_757 ?
O2 W1 O20 89.1(9) . 3_757 ?
O3 W1 O20 59.6(9) 3_757 3_757 ?
O4 W1 O20 95.1(9) . 3_757 ?
O5 W1 O20 59.8(9) 3_757 3_757 ?
O19 W1 O20 41.0(10) . 3_757 ?
O6 W2 O4 100.8(7) . . ?
O6 W2 O7 100.3(7) . . ?
O4 W2 O7 158.9(6) . . ?
O6 W2 O9 86.8(9) . . ?
O4 W2 O9 88.6(6) . . ?
O7 W2 O9 92.9(7) . . ?
O6 W2 O8 113.4(9) . . ?
O4 W2 O8 90.8(6) . . ?
O7 W2 O8 80.5(6) . . ?
O9 W2 O8 159.5(6) . . ?
O6 W2 O21 162.9(9) . . ?
O4 W2 O21 96.3(8) . . ?
O7 W2 O21 62.6(8) . . ?
O9 W2 O21 93.6(9) . . ?
O8 W2 O21 66.1(9) . . ?
O6 W2 O19 148.3(10) . . ?
O4 W2 O19 62.3(8) . . ?
O7 W2 O19 99.0(8) . . ?
O9 W2 O19 67.3(9) . . ?
O8 W2 O19 94.4(9) . . ?
O21 W2 O19 43.8(10) . . ?
O11 W3 O9 98.5(8) . . ?
O11 W3 O2 105.4(7) . . ?
O9 W3 O2 86.5(7) . . ?
O11 W3 O12 103.9(8) . . ?
O9 W3 O12 88.3(8) . . ?
O2 W3 O12 150.7(8) . . ?
O11 W3 O10 98.8(7) . . ?
O9 W3 O10 162.6(7) . . ?
O2 W3 O10 87.3(6) . . ?
O12 W3 O10 89.2(7) . . ?
O5 W4 O13 106.9(8) . . ?
O5 W4 O14 99.7(8) . . ?
O13 W4 O14 104.0(8) . . ?
O5 W4 O12 146.7(8) . . ?
O13 W4 O12 103.1(8) . . ?
O14 W4 O12 86.6(8) . . ?
O5 W4 O15 74.2(7) . . ?
O13 W4 O15 96.8(8) . . ?
O14 W4 O15 159.2(7) . . ?
O12 W4 O15 88.4(7) . . ?
O5 W4 O22 84.8(10) . . ?
O13 W4 O22 158.5(11) . . ?
O14 W4 O22 91.3(11) . . ?
O12 W4 O22 62.3(10) . . ?
O15 W4 O22 68.6(11) . . ?
O16 W5 O3 101.9(8) . . ?
O16 W5 O7 98.8(8) . . ?
O3 W5 O7 159.2(7) . . ?
O16 W5 O17 99.5(8) . . ?
O3 W5 O17 87.7(7) . . ?
O7 W5 O17 86.7(7) . . ?
O16 W5 O14 108.8(8) . . ?
O3 W5 O14 84.1(7) . . ?
O7 W5 O14 91.4(7) . . ?
O17 W5 O14 151.5(7) . . ?
O16 W5 O21 154.6(11) . . ?
O3 W5 O21 96.9(9) . . ?
O7 W5 O21 62.7(9) . . ?
O17 W5 O21 64.1(9) . . ?
O14 W5 O21 89.9(9) . . ?
O16 W5 O20 160.9(10) . . ?
O3 W5 O20 61.3(9) . . ?
O7 W5 O20 98.6(9) . . ?
O17 W5 O20 89.4(9) . . ?
O14 W5 O20 62.8(9) . . ?
O21 W5 O20 44.1(10) . . ?
O18 W6 O8 95.4(8) . . ?
O18 W6 O17 101.5(8) . . ?
O8 W6 O17 88.5(7) . . ?
O18 W6 O15 96.8(8) . 3_757 ?
O8 W6 O15 91.1(6) . 3_757 ?
O17 W6 O15 161.7(8) . 3_757 ?
O18 W6 O10 101.4(7) . 3_757 ?
O8 W6 O10 162.0(7) . 3_757 ?
O17 W6 O10 81.8(7) . 3_757 ?
O15 W6 O10 93.3(6) 3_757 3_757 ?
O18 W6 O21 154.9(9) . . ?
O8 W6 O21 66.2(9) . . ?
O17 W6 O21 62.9(8) . . ?
O15 W6 O21 100.3(8) 3_757 . ?
O10 W6 O21 95.8(8) 3_757 . ?
O22 P O22 179.998(10) 3_757 . ?
O22 P O19 101.0(18) 3_757 . ?
O22 P O19 79.0(18) . . ?
O22 P O19 79.0(18) 3_757 3_757 ?
O22 P O19 101.0(18) . 3_757 ?
O19 P O19 179.999(7) . 3_757 ?
O22 P O20 111.4(18) 3_757 . ?
O22 P O20 68.6(18) . . ?
O19 P O20 115.5(15) . . ?
O19 P O20 64.5(15) 3_757 . ?
O22 P O20 68.6(18) 3_757 3_757 ?
O22 P O20 111.4(18) . 3_757 ?
O19 P O20 64.5(15) . 3_757 ?
O19 P O20 115.5(15) 3_757 3_757 ?
O20 P O20 179.999(4) . 3_757 ?
O22 P O21 78.4(18) 3_757 . ?
O22 P O21 101.6(18) . . ?
O19 P O21 67.4(15) . . ?
O19 P O21 112.6(15) 3_757 . ?
O20 P O21 66.8(15) . . ?
O20 P O21 113.2(15) 3_757 . ?
O22 P O21 101.6(18) 3_757 3_757 ?
O22 P O21 78.4(18) . 3_757 ?
O19 P O21 112.6(15) . 3_757 ?
O19 P O21 67.4(15) 3_757 3_757 ?
O20 P O21 113.2(15) . 3_757 ?
O20 P O21 66.8(15) 3_757 3_757 ?
O21 P O21 179.998(8) . 3_757 ?
W1 O2 W3 146.7(9) . . ?
W5 O3 W1 143.5(10) . 3_757 ?
W1 O4 W2 136.4(9) . . ?
W4 O5 W1 136.9(10) . 3_757 ?
W5 O7 W2 135.7(8) . . ?
W6 O8 W2 133.5(9) . . ?
W3 O9 W2 133.2(9) . . ?
W3 O10 W6 137.0(7) . 3_757 ?
W3 O12 W4 144.8(10) . . ?
W4 O14 W5 141.6(9) . . ?
W6 O15 W4 130.6(9) 3_757 . ?
W6 O17 W5 139.1(10) . . ?
P O19 O20 58.0(14) . 3_757 ?
P O19 O21 58.5(14) . . ?
O20 O19 O21 102(2) 3_757 . ?
P O19 W1 129.9(16) . . ?
O20 O19 W1 71.9(14) 3_757 . ?
O21 O19 W1 141(2) . . ?
P O19 W2 123.3(17) . . ?
O20 O19 W2 141(2) 3_757 . ?
O21 O19 W2 64.8(14) . . ?
W1 O19 W2 95.1(11) . . ?
P O20 O19 57.5(14) . 3_757 ?
P O20 O22 54.1(15) . . ?
O19 O20 O22 88(2) 3_757 . ?
P O20 O21 58.6(13) . . ?
O19 O20 O21 102(2) 3_757 . ?
O22 O20 O21 88(2) . . ?
P O20 W5 125.9(17) . . ?
O19 O20 W5 139(2) 3_757 . ?
O22 O20 W5 129(2) . . ?
O21 O20 W5 67.3(14) . . ?
P O20 W1 124.6(16) . 3_757 ?
O19 O20 W1 67.1(14) 3_757 3_757 ?
O22 O20 W1 128(2) . 3_757 ?
O21 O20 W1 140(2) . 3_757 ?
W5 O20 W1 95.3(11) . 3_757 ?
P O21 O20 54.6(14) . . ?
P O21 O19 54.0(14) . . ?
O20 O21 O19 96(2) . . ?
P O21 W2 125.5(15) . . ?
O20 O21 W2 141(2) . . ?
O19 O21 W2 71.5(14) . . ?
P O21 W5 123.2(15) . . ?
O20 O21 W5 68.6(13) . . ?
O19 O21 W5 143.5(19) . . ?
W2 O21 W5 99.0(11) . . ?
P O21 W6 114.4(14) . . ?
O20 O21 W6 122.5(18) . . ?
O19 O21 W6 122.1(17) . . ?
W2 O21 W6 93.9(11) . . ?
W5 O21 W6 93.0(11) . . ?
P O22 O20 57.3(17) . . ?
P O22 W4 132(2) . . ?
O20 O22 W4 74.6(15) . . ?
N6A C1A C2A 120.0(6) . . ?
N6A C1A H1A 120.0 . . ?
C2A C1A H1A 120.0 . . ?
C1A C2A C3A 118.9(7) . . ?
C1A C2A H2A 120.5 . . ?
C3A C2A H2A 120.5 . . ?
C2A C3A C4A 121.5(7) . . ?
C2A C3A H3A 119.2 . . ?
C4A C3A H3A 119.2 . . ?
C5A C4A C3A 118.1(8) . . ?
C5A C4A H4A 120.9 . . ?
C3A C4A H4A 120.9 . . ?
N6A C5A C4A 120.6(8) . . ?
N6A C5A H5A 119.7 . . ?
C4A C5A H5A 119.7 . . ?
C5A N6A C1A 120.7(6) . . ?
C5A N6A H6A 119.6 . . ?
C1A N6A H6A 119.6 . . ?
C3B C2B H2B 120.4 . . ?
C2B C3B N1B 121.0(6) . 3_656 ?
C2B C3B H3B 119.5 . . ?
N1B C3B H3B 119.5 3_656 . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         6.687
_refine_diff_density_min         -4.095
_refine_diff_density_rms         0.861

#===========END