# Electronic Supplementary Material (ESI) for RSC Advances.
# This journal is © The Royal Society of Chemistry 2014

#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_sad

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C8 H54 Mo10 N10 O46'
_chemical_formula_weight         1986.01

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'
Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           ?
_symmetry_space_group_name_H-M   ?

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                   10.5418(5)
_cell_length_b                   16.8661(8)
_cell_length_c                   14.0774(7)
_cell_angle_alpha                90.00
_cell_angle_beta                 92.5250(10)
_cell_angle_gamma                90.00
_cell_volume                     2500.5(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       ?
_exptl_crystal_colour            ?
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.638
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1920
_exptl_absorpt_coefficient_mu    2.545
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  0.7014
_exptl_absorpt_correction_T_max  0.7849
_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  ?
_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            14825
_diffrn_reflns_av_R_equivalents  0.0656
_diffrn_reflns_av_sigmaI/netI    0.0610
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         1.89
_diffrn_reflns_theta_max         27.00
_reflns_number_total             5437
_reflns_number_gt                4791
_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 F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² 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/[σ²(Fo²)+(0.0358P)²+7.4251P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5437
_refine_ls_number_parameters     400
_refine_ls_number_restraints     49
_refine_ls_R_factor_all          0.0561
_refine_ls_R_factor_gt           0.0472
_refine_ls_wR_factor_ref         0.1035
_refine_ls_wR_factor_gt          0.0991
_refine_ls_goodness_of_fit_ref   1.106
_refine_ls_restrained_S_all      1.101
_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
Mo1 Mo 0.25531(5) 0.20374(3) 0.89955(4) 0.02382(14) Uani 1 1 d . . .
Mo2 Mo 0.02947(5) 0.27615(3) 1.07960(4) 0.02175(13) Uani 1 1 d . . .
Mo3 Mo -0.23640(5) 0.36656(3) 1.01081(4) 0.02207(13) Uani 1 1 d . . .
Mo4 Mo -0.23256(5) 0.53327(3) 0.89242(4) 0.02131(13) Uani 1 1 d . . .
Mo5 Mo 0.04851(5) 0.42809(3) 0.92124(4) 0.01735(12) Uani 1 1 d . . .
O1 O 0.3864(5) 0.1401(3) 0.9996(3) 0.0376(12) Uani 1 1 d . . .
O2 O 0.5748(5) 0.0849(3) 1.0216(4) 0.0477(14) Uani 1 1 d . . .
O3 O 0.1688(4) 0.0849(3) 0.9107(3) 0.0333(11) Uani 1 1 d . . .
O4 O 0.1345(5) -0.0303(3) 0.8371(4) 0.0455(13) Uani 1 1 d . . .
O5 O 0.3719(5) 0.2717(3) 0.8805(4) 0.0456(14) Uani 1 1 d . . .
O6 O 0.1515(5) 0.2156(3) 0.8052(4) 0.0416(12) Uani 1 1 d . . .
O7 O -0.0495(4) 0.1894(3) 1.0526(4) 0.0413(13) Uani 1 1 d . . .
O8 O 0.0963(4) 0.2611(3) 1.1906(4) 0.0390(12) Uani 1 1 d . . .
O9 O -0.2973(4) 0.2766(3) 0.9793(4) 0.0341(11) Uani 1 1 d . . .
O10 O -0.3476(4) 0.4085(3) 1.0818(3) 0.0325(11) Uani 1 1 d . . .
O11 O -0.2657(5) 0.5606(4) 0.7753(4) 0.065(2) Uani 1 1 d . . .
O12 O -0.3635(4) 0.5633(3) 0.9512(4) 0.0317(11) Uani 1 1 d . . .
O13 O -0.1149(4) 0.6125(2) 0.9408(3) 0.0208(9) Uani 1 1 d . . .
O14 O 0.1710(4) 0.3955(3) 0.8568(3) 0.0271(10) Uani 1 1 d . . .
O15 O 0.1749(4) 0.2399(3) 1.0027(3) 0.0333(11) Uani 1 1 d . . .
O16 O -0.1187(4) 0.3335(2) 1.1146(3) 0.0240(9) Uani 1 1 d . . .
O17 O -0.2765(4) 0.4207(2) 0.8910(3) 0.0249(9) Uani 1 1 d . . .
O18 O -0.0480(4) 0.4789(3) 0.8357(3) 0.0239(9) Uani 1 1 d . . .
O19 O -0.0506(4) 0.3372(2) 0.9417(3) 0.0236(9) Uani 1 1 d . . .
O20 O -0.1219(4) 0.4794(2) 1.0133(3) 0.0198(9) Uani 1 1 d . . .
C1 C 0.4871(6) 0.1101(4) 0.9707(5) 0.0297(15) Uani 1 1 d . . .
C2 C 0.4999(6) 0.1091(5) 0.8636(5) 0.0380(17) Uani 1 1 d . . .
H2A H 0.5564 0.1514 0.8456 0.046 Uiso 1 1 calc R . .
H2B H 0.5369 0.0592 0.8449 0.046 Uiso 1 1 calc R . .
C3 C 0.1957(7) 0.0323(4) 0.8512(5) 0.0310(15) Uani 1 1 d . . .
C4 C 0.3074(7) 0.0456(4) 0.7915(5) 0.0366(17) Uani 1 1 d . . .
H4A H 0.3659 0.0016 0.8006 0.044 Uiso 1 1 calc R . .
H4B H 0.2787 0.0461 0.7251 0.044 Uiso 1 1 calc R . .
N1 N 0.3750(5) 0.1195(3) 0.8132(4) 0.0242(11) Uani 1 1 d . . .
H1A H 0.3889 0.1437 0.7568 0.029 Uiso 1 1 calc R . .
N2 N 0.4539(5) 0.4293(4) 0.8595(5) 0.0413(16) Uani 1 1 d D . .
N3 N 0.2042(6) 0.3202(4) 0.6599(5) 0.0476(17) Uani 1 1 d D . .
O2W O 0.8083(7) 0.0938(5) 0.9365(5) 0.076(2) Uani 1 1 d D . .
N5 N 0.4698(6) 0.2838(3) 1.1238(4) 0.0387(14) Uani 1 1 d D . .
O1W O 0.3509(7) 0.2750(5) 0.3002(6) 0.076(2) Uani 1 1 d D . .
N4 N -0.1163(7) -0.0529(5) 0.8931(6) 0.073(3) Uani 1 1 d D . .
O3W O 0.3303(8) 0.1259(5) 1.1935(5) 0.085(2) Uani 1 1 d D . .
H9 H -0.118(8) -0.075(4) 0.947(3) 0.102 Uiso 1 1 d D . .
H3W1 H 0.342(9) 0.092(5) 1.237(5) 0.102 Uiso 1 1 d D . .
H3W2 H 0.394(7) 0.126(6) 1.159(6) 0.102 Uiso 1 1 d D . .
H1 H 0.436(7) 0.451(4) 0.806(3) 0.102 Uiso 1 1 d D . .
H2 H 0.431(7) 0.3807(15) 0.857(6) 0.102 Uiso 1 1 d D . .
H3 H 0.5339(16) 0.431(5) 0.871(6) 0.102 Uiso 1 1 d D . .
H4 H 0.415(7) 0.453(4) 0.903(4) 0.102 Uiso 1 1 d D . .
H5 H 0.222(7) 0.275(2) 0.636(5) 0.102 Uiso 1 1 d D . .
H6 H 0.146(5) 0.342(4) 0.625(5) 0.102 Uiso 1 1 d D . .
H7 H 0.270(4) 0.349(4) 0.663(6) 0.102 Uiso 1 1 d D . .
H8 H 0.177(7) 0.313(5) 0.716(2) 0.102 Uiso 1 1 d D . .
H2W1 H 0.863(7) 0.128(5) 0.955(8) 0.102 Uiso 1 1 d D . .
H2W2 H 0.742(6) 0.099(6) 0.968(7) 0.102 Uiso 1 1 d D . .
H13 H 0.514(6) 0.325(3) 1.113(6) 0.102 Uiso 1 1 d D . .
H14 H 0.406(5) 0.283(5) 1.084(5) 0.102 Uiso 1 1 d D . .
H15 H 0.514(6) 0.242(3) 1.118(6) 0.102 Uiso 1 1 d D . .
H16 H 0.443(8) 0.287(5) 1.180(2) 0.102 Uiso 1 1 d D . .
H1W2 H 0.371(8) 0.314(5) 0.336(7) 0.102 Uiso 1 1 d D . .
H11 H -0.127(8) -0.0028(10) 0.899(6) 0.102 Uiso 1 1 d D . .
H1W1 H 0.273(3) 0.278(6) 0.283(8) 0.102 Uiso 1 1 d D . .
H10 H -0.175(5) -0.071(4) 0.856(5) 0.102 Uiso 1 1 d D . .
H12 H -0.045(4) -0.061(5) 0.869(5) 0.102 Uiso 1 1 d D . .


_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
Mo1 O6 1.695(5) . ?
Mo1 O5 1.711(5) . ?
Mo1 O15 1.818(4) . ?
Mo1 O1 2.208(5) . ?
Mo1 O3 2.210(4) . ?
Mo1 N1 2.286(5) . ?
Mo2 O8 1.705(5) . ?
Mo2 O7 1.718(5) . ?
Mo2 O16 1.920(4) . ?
Mo2 O15 2.011(4) . ?
Mo2 O13 2.108(4) 3_567 ?
Mo2 O19 2.324(4) . ?
Mo3 O9 1.698(4) . ?
Mo3 O10 1.725(4) . ?
Mo3 O17 1.948(4) . ?
Mo3 O16 1.956(4) . ?
Mo3 O20 2.253(4) . ?
Mo3 O19 2.279(4) . ?
Mo4 O12 1.717(4) . ?
Mo4 O11 1.732(5) . ?
Mo4 O13 1.927(4) . ?
Mo4 O17 1.953(4) . ?
Mo4 O20 2.215(4) . ?
Mo4 O18 2.324(4) . ?
Mo5 O14 1.702(4) . ?
Mo5 O18 1.763(4) . ?
Mo5 O19 1.884(4) . ?
Mo5 O20 1.954(4) 3_567 ?
Mo5 O13 2.147(4) 3_567 ?
Mo5 O20 2.421(4) . ?
O1 C1 1.259(8) . ?
O2 C1 1.221(8) . ?
O3 C3 1.262(8) . ?
O4 C3 1.249(8) . ?
O13 Mo2 2.108(4) 3_567 ?
O13 Mo5 2.147(4) 3_567 ?
O20 Mo5 1.954(4) 3_567 ?
C1 C2 1.521(10) . ?
C2 N1 1.478(8) . ?
C3 C4 1.493(10) . ?
C4 N1 1.461(8) . ?

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
O6 Mo1 O5 104.0(3) . . ?
O6 Mo1 O15 106.2(2) . . ?
O5 Mo1 O15 105.3(2) . . ?
O6 Mo1 O1 157.1(2) . . ?
O5 Mo1 O1 89.5(2) . . ?
O15 Mo1 O1 87.38(19) . . ?
O6 Mo1 O3 84.7(2) . . ?
O5 Mo1 O3 157.0(2) . . ?
O15 Mo1 O3 92.21(19) . . ?
O1 Mo1 O3 76.26(19) . . ?
O6 Mo1 N1 90.5(2) . . ?
O5 Mo1 N1 85.2(2) . . ?
O15 Mo1 N1 157.0(2) . . ?
O1 Mo1 N1 72.08(18) . . ?
O3 Mo1 N1 73.34(17) . . ?
O8 Mo2 O7 104.6(3) . . ?
O8 Mo2 O16 98.5(2) . . ?
O7 Mo2 O16 95.4(2) . . ?
O8 Mo2 O15 98.9(2) . . ?
O7 Mo2 O15 89.7(2) . . ?
O16 Mo2 O15 160.00(19) . . ?
O8 Mo2 O13 95.5(2) . 3_567 ?
O7 Mo2 O13 159.2(2) . 3_567 ?
O16 Mo2 O13 86.75(17) . 3_567 ?
O15 Mo2 O13 81.80(17) . 3_567 ?
O8 Mo2 O19 162.2(2) . . ?
O7 Mo2 O19 92.2(2) . . ?
O16 Mo2 O19 73.82(16) . . ?
O15 Mo2 O19 86.70(17) . . ?
O13 Mo2 O19 68.45(15) 3_567 . ?
O9 Mo3 O10 105.0(2) . . ?
O9 Mo3 O17 97.3(2) . . ?
O10 Mo3 O17 100.5(2) . . ?
O9 Mo3 O16 99.2(2) . . ?
O10 Mo3 O16 96.3(2) . . ?
O17 Mo3 O16 152.46(17) . . ?
O9 Mo3 O20 162.66(19) . . ?
O10 Mo3 O20 91.22(18) . . ?
O17 Mo3 O20 73.31(16) . . ?
O16 Mo3 O20 84.69(17) . . ?
O9 Mo3 O19 90.95(18) . . ?
O10 Mo3 O19 162.70(19) . . ?
O17 Mo3 O19 83.67(17) . . ?
O16 Mo3 O19 74.25(16) . . ?
O20 Mo3 O19 73.76(14) . . ?
O12 Mo4 O11 104.3(2) . . ?
O12 Mo4 O13 98.25(19) . . ?
O11 Mo4 O13 104.6(3) . . ?
O12 Mo4 O17 95.5(2) . . ?
O11 Mo4 O17 102.2(3) . . ?
O13 Mo4 O17 145.66(18) . . ?
O12 Mo4 O20 99.09(19) . . ?
O11 Mo4 O20 156.6(2) . . ?
O13 Mo4 O20 72.77(16) . . ?
O17 Mo4 O20 74.08(16) . . ?
O12 Mo4 O18 170.10(19) . . ?
O11 Mo4 O18 85.1(2) . . ?
O13 Mo4 O18 81.91(16) . . ?
O17 Mo4 O18 79.33(16) . . ?
O20 Mo4 O18 71.43(14) . . ?
O14 Mo5 O18 102.8(2) . . ?
O14 Mo5 O19 104.94(19) . . ?
O18 Mo5 O19 101.09(19) . . ?
O14 Mo5 O20 102.43(19) . 3_567 ?
O18 Mo5 O20 97.94(18) . 3_567 ?
O19 Mo5 O20 142.02(18) . 3_567 ?
O14 Mo5 O13 98.91(18) . 3_567 ?
O18 Mo5 O13 158.04(17) . 3_567 ?
O19 Mo5 O13 76.31(17) . 3_567 ?
O20 Mo5 O13 73.84(16) 3_567 3_567 ?
O14 Mo5 O20 177.80(18) . . ?
O18 Mo5 O20 76.85(16) . . ?
O19 Mo5 O20 77.25(15) . . ?
O20 Mo5 O20 75.53(16) 3_567 . ?
O13 Mo5 O20 81.35(14) 3_567 . ?
C1 O1 Mo1 120.2(4) . . ?
C3 O3 Mo1 119.0(4) . . ?
Mo4 O13 Mo2 147.3(2) . 3_567 ?
Mo4 O13 Mo5 106.13(18) . 3_567 ?
Mo2 O13 Mo5 106.46(18) 3_567 3_567 ?
Mo1 O15 Mo2 157.7(3) . . ?
Mo2 O16 Mo3 116.6(2) . . ?
Mo3 O17 Mo4 113.9(2) . . ?
Mo5 O18 Mo4 115.1(2) . . ?
Mo5 O19 Mo3 112.42(19) . . ?
Mo5 O19 Mo2 107.74(19) . . ?
Mo3 O19 Mo2 91.53(15) . . ?
Mo5 O20 Mo4 102.64(17) 3_567 . ?
Mo5 O20 Mo3 152.0(2) 3_567 . ?
Mo4 O20 Mo3 94.06(15) . . ?
Mo5 O20 Mo5 104.47(16) 3_567 . ?
Mo4 O20 Mo5 96.50(15) . . ?
Mo3 O20 Mo5 95.70(14) . . ?
O2 C1 O1 125.4(7) . . ?
O2 C1 C2 118.7(6) . . ?
O1 C1 C2 115.9(6) . . ?
N1 C2 C1 111.0(5) . . ?
O4 C3 O3 124.8(7) . . ?
O4 C3 C4 116.9(6) . . ?
O3 C3 C4 118.3(6) . . ?
N1 C4 C3 113.6(5) . . ?
C4 N1 C2 114.6(6) . . ?
C4 N1 Mo1 111.5(4) . . ?
C2 N1 Mo1 108.6(4) . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        27.00
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         1.027
_refine_diff_density_min         -0.677
_refine_diff_density_rms         0.188
_database_code_depnum_ccdc_archive 'CCDC 987093'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_sad

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C4 H17 K4 Mo5 N O25'
_chemical_formula_weight         1115.29

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'
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           ?
_symmetry_space_group_name_H-M   ?

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

_cell_length_a                   10.3517(4)
_cell_length_b                   11.2044(3)
_cell_length_c                   11.3559(3)
_cell_angle_alpha                95.776(2)
_cell_angle_beta                 95.670(3)
_cell_angle_gamma                92.794(3)
_cell_volume                     1301.72(7)
_cell_formula_units_Z            2
_cell_measurement_temperature    446(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       ?
_exptl_crystal_colour            ?
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.845
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1068
_exptl_absorpt_coefficient_mu    3.086
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  0.5125
_exptl_absorpt_correction_T_max  0.7477
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      446(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            12411
_diffrn_reflns_av_R_equivalents  0.0229
_diffrn_reflns_av_sigmaI/netI    0.0302
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         2.71
_diffrn_reflns_theta_max         27.00
_reflns_number_total             5685
_reflns_number_gt                4917
_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 F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² 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/[σ²(Fo²)+(0.0480P)²+2.1251P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5685
_refine_ls_number_parameters     397
_refine_ls_number_restraints     18
_refine_ls_R_factor_all          0.0281
_refine_ls_R_factor_gt           0.0216
_refine_ls_wR_factor_ref         0.0625
_refine_ls_wR_factor_gt          0.0586
_refine_ls_goodness_of_fit_ref   0.813
_refine_ls_restrained_S_all      0.813
_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
Mo1 Mo 0.71240(3) -0.31657(2) -0.13245(2) 0.01133(7) Uani 1 1 d . . .
Mo2 Mo 0.60651(3) -0.27868(2) -0.33889(2) 0.01007(7) Uani 1 1 d . . .
Mo4 Mo 0.59847(3) 0.01679(2) -0.36597(2) 0.00875(7) Uani 1 1 d . . .
Mo3 Mo 0.32111(3) -0.15703(2) -0.33549(2) 0.01105(7) Uani 1 1 d . . .
Mo5 Mo 0.28472(3) 0.11803(2) -0.40047(2) 0.01025(7) Uani 1 1 d . . .
K1 K 0.96191(10) -0.47562(9) -0.32693(8) 0.0321(2) Uani 1 1 d . . .
K2 K 0.97576(7) -0.06414(7) -0.30926(7) 0.01932(16) Uani 1 1 d . . .
K3 K 0.46196(9) -0.38495(8) 0.34183(8) 0.02713(19) Uani 1 1 d . . .
K4 K 1.29236(11) -0.42791(9) -0.09323(10) 0.0414(3) Uani 1 1 d . . .
N1 N 0.6471(3) -0.1350(3) -0.0430(2) 0.0134(6) Uani 1 1 d . . .
H1C H 0.6069 -0.0967 -0.1021 0.016 Uiso 1 1 calc R . .
O1 O 0.8727(2) -0.2393(2) -0.0135(2) 0.0178(5) Uani 1 1 d . . .
O2 O 0.9712(3) -0.0878(3) 0.1071(2) 0.0277(6) Uani 1 1 d . . .
O3 O 0.6306(2) -0.3557(2) 0.0227(2) 0.0192(5) Uani 1 1 d . . .
O4 O 0.4535(3) -0.3289(3) 0.1160(2) 0.0270(6) Uani 1 1 d . . .
O5 O 0.7663(2) -0.2120(2) -0.2452(2) 0.0129(5) Uani 1 1 d . . .
O6 O 0.5352(2) -0.3391(2) -0.2031(2) 0.0139(5) Uani 1 1 d . . .
O7 O 0.4155(2) -0.2763(2) -0.40686(19) 0.0127(5) Uani 1 1 d . . .
O8 O 0.6428(2) -0.1526(2) -0.45448(19) 0.0120(4) Uani 1 1 d . . .
O9 O 0.5286(2) -0.0948(2) -0.27317(19) 0.0114(4) Uani 1 1 d . . .
O10 O 0.3836(2) -0.0419(2) -0.46918(19) 0.0108(4) Uani 1 1 d . . .
O11 O 0.2892(2) 0.0137(2) -0.28111(19) 0.0131(5) Uani 1 1 d . . .
O12 O 0.5090(2) 0.1411(2) -0.3313(2) 0.0133(5) Uani 1 1 d . . .
O13 O 0.7840(3) -0.4490(2) -0.1520(2) 0.0193(5) Uani 1 1 d . . .
O14 O 0.6434(2) -0.4005(2) -0.4279(2) 0.0174(5) Uani 1 1 d . . .
O15 O 0.7502(2) 0.0567(2) -0.2963(2) 0.0158(5) Uani 1 1 d . . .
O16 O 0.3031(2) -0.2023(2) -0.1968(2) 0.0162(5) Uani 1 1 d . . .
O17 O 0.1719(2) -0.1931(2) -0.4164(2) 0.0167(5) Uani 1 1 d . . .
O18 O 0.1267(2) 0.0858(2) -0.4596(2) 0.0185(5) Uani 1 1 d . . .
O19 O 0.2829(2) 0.2610(2) -0.3294(2) 0.0194(5) Uani 1 1 d . . .
C1 C 0.7629(3) -0.0575(3) 0.0087(3) 0.0183(7) Uani 1 1 d . . .
H1A H 0.7423 -0.0100 0.0799 0.022 Uiso 1 1 calc R . .
H1B H 0.7856 -0.0026 -0.0479 0.022 Uiso 1 1 calc R . .
C2 C 0.8782(3) -0.1311(3) 0.0397(3) 0.0177(7) Uani 1 1 d . . .
C3 C 0.5486(4) -0.1597(3) 0.0389(3) 0.0186(7) Uani 1 1 d . . .
H3A H 0.4640 -0.1392 0.0046 0.022 Uiso 1 1 calc R . .
H3B H 0.5700 -0.1094 0.1137 0.022 Uiso 1 1 calc R . .
C4 C 0.5418(3) -0.2904(3) 0.0626(3) 0.0185(7) Uani 1 1 d . . .
O1W O 1.0501(3) -0.2712(3) -0.1866(3) 0.0309(7) Uani 1 1 d D . .
O2W O 0.9556(3) -0.3421(3) -0.5138(3) 0.0335(7) Uani 1 1 d D . .
O3W O 0.7904(3) -0.6728(3) -0.3427(3) 0.0378(7) Uani 1 1 d D . .
O4W O 1.2644(4) -0.4761(3) -0.3400(3) 0.0553(10) Uani 1 1 d D . .
O5W O 1.1833(3) -0.2599(3) 0.0882(3) 0.0446(8) Uani 1 1 d D . .
O6W O 1.0492(6) -0.5601(6) -0.1175(6) 0.0373(15) Uani 0.50 1 d PD . .
O7W O 1.1053(7) -0.6092(6) -0.1804(6) 0.0357(14) Uani 0.50 1 d P . .
H1W1 H 1.017(4) -0.263(4) -0.121(2) 0.043 Uiso 1 1 d D . .
H1W2 H 1.126(2) -0.237(4) -0.179(4) 0.043 Uiso 1 1 d D . .
H2W1 H 0.959(4) -0.356(4) -0.5908(12) 0.043 Uiso 1 1 d D . .
H2W2 H 0.889(3) -0.300(4) -0.506(3) 0.043 Uiso 1 1 d D . .
H3W1 H 0.816(5) -0.690(4) -0.2737(17) 0.043 Uiso 1 1 d D . .
H3W2 H 0.777(5) -0.736(2) -0.391(3) 0.043 Uiso 1 1 d D . .
H4W1 H 1.314(4) -0.422(4) -0.363(4) 0.043 Uiso 1 1 d D . .
H4W2 H 1.207(4) -0.501(4) -0.397(3) 0.043 Uiso 1 1 d D . .
H5W1 H 1.2598(16) -0.231(4) 0.110(4) 0.043 Uiso 1 1 d D . .
H5W2 H 1.128(3) -0.214(3) 0.114(4) 0.043 Uiso 1 1 d D . .
H6W1 H 0.995(4) -0.530(3) -0.074(4) 0.043 Uiso 1 1 d D . .
H6W2 H 1.051(5) -0.6350(13) -0.115(4) 0.043 Uiso 1 1 d D . .


_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
Mo1 O13 1.695(2) . ?
Mo1 O5 1.925(2) . ?
Mo1 O6 1.923(2) . ?
Mo1 O3 2.104(2) . ?
Mo1 O1 2.124(2) . ?
Mo1 N1 2.341(3) . ?
Mo1 Mo2 2.5721(4) . ?
Mo1 K1 3.9380(10) . ?
Mo1 K4 4.0316(10) 2_745 ?
Mo2 O14 1.698(2) . ?
Mo2 O6 1.941(2) . ?
Mo2 O5 1.949(2) . ?
Mo2 O7 2.053(2) . ?
Mo2 O8 2.068(2) . ?
Mo2 O9 2.329(2) . ?
Mo2 K3 3.7970(9) 2_645 ?
Mo2 K3 3.8325(9) 1_554 ?
Mo4 O15 1.705(2) . ?
Mo4 O12 1.744(2) . ?
Mo4 O9 1.877(2) . ?
Mo4 O10 1.946(2) 2_654 ?
Mo4 O8 2.148(2) . ?
Mo4 O10 2.437(2) . ?
Mo4 K2 4.0567(8) . ?
Mo3 O16 1.727(2) . ?
Mo3 O17 1.726(2) . ?
Mo3 O7 1.861(2) . ?
Mo3 O11 2.003(2) . ?
Mo3 O10 2.213(2) . ?
Mo3 O9 2.249(2) . ?
Mo3 K2 3.8030(8) 1_455 ?
Mo5 O18 1.713(2) . ?
Mo5 O19 1.722(2) . ?
Mo5 O11 1.876(2) . ?
Mo5 O8 1.942(2) 2_654 ?
Mo5 O10 2.219(2) . ?
Mo5 O12 2.370(2) . ?
Mo5 K3 3.8411(9) 2_655 ?
Mo5 K2 3.9889(9) 1_455 ?
Mo5 K2 4.0231(8) 2_654 ?
K1 O2W 2.714(3) . ?
K1 O1W 2.720(3) . ?
K1 O3W 2.746(3) . ?
K1 O6W 2.735(6) . ?
K1 O7W 2.728(6) . ?
K1 O2W 2.811(3) 2_744 ?
K1 O13 2.843(3) . ?
K1 O4W 3.150(5) . ?
K1 K1 4.0735(18) 2_744 ?
K1 K4 4.0955(14) . ?
K1 K3 4.5666(13) 2_645 ?
K1 H1W1 3.15(4) . ?
K1 H2W2 3.04(4) . ?
K1 H3W1 2.93(4) . ?
K1 H4W2 2.75(5) . ?
K1 H6W2 3.23(4) . ?
K2 O2 2.710(3) 2_755 ?
K2 O18 2.715(2) 2_654 ?
K2 O15 2.765(3) . ?
K2 O17 2.848(3) 1_655 ?
K2 O5 2.860(2) . ?
K2 O1W 2.920(3) . ?
K2 O18 3.005(3) 1_655 ?
K2 O11 3.295(2) 1_655 ?
K2 Mo3 3.8030(8) 1_655 ?
K2 Mo5 3.9889(8) 1_655 ?
K2 Mo5 4.0231(8) 2_654 ?
K2 H1W2 2.97(5) . ?
K3 O4 2.695(3) . ?
K3 O3W 2.723(4) 2_645 ?
K3 O12 2.750(2) 2_655 ?
K3 O14 2.890(3) 2_645 ?
K3 O19 2.946(3) 2_655 ?
K3 O7 3.080(2) 1_556 ?
K3 O14 3.090(3) 1_556 ?
K3 O4W 3.299(5) 2_745 ?
K3 O6 3.328(3) 2_645 ?
K3 Mo2 3.7970(9) 2_645 ?
K3 Mo2 3.8325(9) 1_556 ?
K3 Mo5 3.8411(9) 2_655 ?
K4 O3 2.759(3) 2_745 ?
K4 O4W 2.784(4) . ?
K4 O7W 2.773(7) . ?
K4 O6W 2.833(7) . ?
K4 O4 2.857(3) 1_655 ?
K4 O16 2.895(3) 1_655 ?
K4 O5W 2.992(4) . ?
K4 O6 3.080(3) 1_655 ?
K4 C4 3.214(4) 1_655 ?
K4 O1W 3.283(3) . ?
K4 O13 3.374(3) 2_745 ?
K4 Mo1 4.0316(10) 2_745 ?
K4 H1W2 2.98(5) . ?
K4 H4W1 3.10(4) . ?
K4 H5W1 3.08(4) . ?
K4 H6W1 3.26(4) . ?
N1 C3 1.482(4) . ?
N1 C1 1.480(4) . ?
N1 H1C 0.9100 . ?
O1 C2 1.296(4) . ?
O2 C2 1.217(4) . ?
O2 K2 2.710(3) 2_755 ?
O3 C4 1.292(4) . ?
O3 K4 2.759(3) 2_745 ?
O4 C4 1.230(4) . ?
O4 K4 2.857(3) 1_455 ?
O6 K4 3.080(3) 1_455 ?
O6 K3 3.328(3) 2_645 ?
O7 K3 3.080(2) 1_554 ?
O8 Mo5 1.942(2) 2_654 ?
O10 Mo4 1.946(2) 2_654 ?
O11 K2 3.295(2) 1_455 ?
O12 K3 2.750(2) 2_655 ?
O13 K4 3.374(3) 2_745 ?
O14 K3 2.890(3) 2_645 ?
O14 K3 3.090(3) 1_554 ?
O16 K4 2.895(3) 1_455 ?
O17 K2 2.848(3) 1_455 ?
O18 K2 2.715(2) 2_654 ?
O18 K2 3.005(3) 1_455 ?
O19 K3 2.946(3) 2_655 ?
C1 C2 1.517(5) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C3 C4 1.515(5) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 K4 3.214(4) 1_455 ?
O1W H1W1 0.843(10) . ?
O1W H1W2 0.847(10) . ?
O2W K1 2.811(3) 2_744 ?
O2W H2W1 0.877(10) . ?
O2W H2W2 0.860(10) . ?
O3W K3 2.723(4) 2_645 ?
O3W H3W1 0.846(10) . ?
O3W H3W2 0.843(10) . ?
O4W K3 3.299(5) 2_745 ?
O4W H4W1 0.854(10) . ?
O4W H4W2 0.852(10) . ?
O5W H5W1 0.843(10) . ?
O5W H5W2 0.845(10) . ?
O6W O7W 1.088(9) . ?
O6W H6W1 0.837(10) . ?
O6W H6W2 0.844(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
O13 Mo1 O5 109.75(11) . . ?
O13 Mo1 O6 108.57(11) . . ?
O5 Mo1 O6 94.75(9) . . ?
O13 Mo1 O3 94.95(11) . . ?
O5 Mo1 O3 154.34(10) . . ?
O6 Mo1 O3 83.43(10) . . ?
O13 Mo1 O1 91.68(11) . . ?
O5 Mo1 O1 87.48(9) . . ?
O6 Mo1 O1 157.37(10) . . ?
O3 Mo1 O1 84.90(10) . . ?
O13 Mo1 N1 161.30(11) . . ?
O5 Mo1 N1 81.18(10) . . ?
O6 Mo1 N1 84.83(10) . . ?
O3 Mo1 N1 73.16(10) . . ?
O1 Mo1 N1 73.24(10) . . ?
O13 Mo1 Mo2 106.12(9) . . ?
O5 Mo1 Mo2 48.79(7) . . ?
O6 Mo1 Mo2 48.58(7) . . ?
O3 Mo1 Mo2 131.39(7) . . ?
O1 Mo1 Mo2 136.00(7) . . ?
N1 Mo1 Mo2 92.51(7) . . ?
O13 Mo1 K1 39.54(9) . . ?
O5 Mo1 K1 70.26(7) . . ?
O6 Mo1 K1 113.67(7) . . ?
O3 Mo1 K1 133.77(7) . . ?
O1 Mo1 K1 88.30(7) . . ?
N1 Mo1 K1 146.65(7) . . ?
Mo2 Mo1 K1 81.632(17) . . ?
O13 Mo1 K4 55.48(9) . 2_745 ?
O5 Mo1 K4 162.56(7) . 2_745 ?
O6 Mo1 K4 98.93(7) . 2_745 ?
O3 Mo1 K4 39.61(7) . 2_745 ?
O1 Mo1 K4 84.04(7) . 2_745 ?
N1 Mo1 K4 110.68(7) . 2_745 ?
Mo2 Mo1 K4 139.119(18) . 2_745 ?
K1 Mo1 K4 94.23(2) . 2_745 ?
O14 Mo2 O6 106.61(11) . . ?
O14 Mo2 O5 107.97(11) . . ?
O6 Mo2 O5 93.39(10) . . ?
O14 Mo2 O7 96.84(11) . . ?
O6 Mo2 O7 84.58(9) . . ?
O5 Mo2 O7 154.57(10) . . ?
O14 Mo2 O8 96.69(10) . . ?
O6 Mo2 O8 155.59(10) . . ?
O5 Mo2 O8 86.08(9) . . ?
O7 Mo2 O8 85.56(9) . . ?
O14 Mo2 O9 162.21(10) . . ?
O6 Mo2 O9 86.10(9) . . ?
O5 Mo2 O9 83.04(9) . . ?
O7 Mo2 O9 71.53(8) . . ?
O8 Mo2 O9 69.59(8) . . ?
O14 Mo2 Mo1 103.12(8) . . ?
O6 Mo2 Mo1 47.96(7) . . ?
O5 Mo2 Mo1 47.99(7) . . ?
O7 Mo2 Mo1 131.93(6) . . ?
O8 Mo2 Mo1 133.58(6) . . ?
O9 Mo2 Mo1 94.63(5) . . ?
O14 Mo2 K3 46.04(8) . 2_645 ?
O6 Mo2 K3 61.18(7) . 2_645 ?
O5 Mo2 K3 115.70(7) . 2_645 ?
O7 Mo2 K3 85.49(7) . 2_645 ?
O8 Mo2 K3 139.95(6) . 2_645 ?
O9 Mo2 K3 141.87(6) . 2_645 ?
Mo1 Mo2 K3 78.259(16) . 2_645 ?
O14 Mo2 K3 51.95(8) . 1_554 ?
O6 Mo2 K3 121.35(7) . 1_554 ?
O5 Mo2 K3 142.45(7) . 1_554 ?
O7 Mo2 K3 53.25(6) . 1_554 ?
O8 Mo2 K3 68.24(6) . 1_554 ?
O9 Mo2 K3 110.92(5) . 1_554 ?
Mo1 Mo2 K3 152.411(18) . 1_554 ?
K3 Mo2 K3 75.21(2) 2_645 1_554 ?
O15 Mo4 O12 104.07(11) . . ?
O15 Mo4 O9 104.57(11) . . ?
O12 Mo4 O9 101.25(10) . . ?
O15 Mo4 O10 103.08(10) . 2_654 ?
O12 Mo4 O10 97.53(10) . 2_654 ?
O9 Mo4 O10 141.40(10) . 2_654 ?
O15 Mo4 O8 97.41(10) . . ?
O12 Mo4 O8 158.09(10) . . ?
O9 Mo4 O8 77.12(9) . . ?
O10 Mo4 O8 73.06(9) 2_654 . ?
O15 Mo4 O10 178.81(10) . . ?
O12 Mo4 O10 76.78(9) . . ?
O9 Mo4 O10 76.01(8) . . ?
O10 Mo4 O10 75.93(9) 2_654 . ?
O8 Mo4 O10 81.69(8) . . ?
O15 Mo4 K2 32.09(8) . . ?
O12 Mo4 K2 135.89(8) . . ?
O9 Mo4 K2 97.45(7) . . ?
O10 Mo4 K2 91.89(7) 2_654 . ?
O8 Mo4 K2 65.33(6) . . ?
O10 Mo4 K2 146.97(5) . . ?
O16 Mo3 O17 104.68(11) . . ?
O16 Mo3 O7 103.77(11) . . ?
O17 Mo3 O7 98.91(11) . . ?
O16 Mo3 O11 92.25(10) . . ?
O17 Mo3 O11 97.09(11) . . ?
O7 Mo3 O11 153.59(10) . . ?
O16 Mo3 O10 158.27(10) . . ?
O17 Mo3 O10 91.97(10) . . ?
O7 Mo3 O10 86.96(9) . . ?
O11 Mo3 O10 71.58(9) . . ?
O16 Mo3 O9 89.65(10) . . ?
O17 Mo3 O9 165.66(10) . . ?
O7 Mo3 O9 76.80(9) . . ?
O11 Mo3 O9 82.54(9) . . ?
O10 Mo3 O9 74.26(8) . . ?
O16 Mo3 K2 81.76(8) . 1_455 ?
O17 Mo3 K2 44.69(8) . 1_455 ?
O7 Mo3 K2 142.26(7) . 1_455 ?
O11 Mo3 K2 60.00(7) . 1_455 ?
O10 Mo3 K2 101.42(6) . 1_455 ?
O9 Mo3 K2 140.93(6) . 1_455 ?
O18 Mo5 O19 103.67(12) . . ?
O18 Mo5 O11 98.32(11) . . ?
O19 Mo5 O11 106.36(11) . . ?
O18 Mo5 O8 98.07(10) . 2_654 ?
O19 Mo5 O8 100.50(11) . 2_654 ?
O11 Mo5 O8 144.04(10) . 2_654 ?
O18 Mo5 O10 102.70(10) . . ?
O19 Mo5 O10 153.30(10) . . ?
O11 Mo5 O10 73.72(9) . . ?
O8 Mo5 O10 71.55(9) 2_654 . ?
O18 Mo5 O12 173.22(10) . . ?
O19 Mo5 O12 83.06(10) . . ?
O11 Mo5 O12 80.34(9) . . ?
O8 Mo5 O12 79.65(9) 2_654 . ?
O10 Mo5 O12 70.54(8) . . ?
O18 Mo5 K3 139.80(9) . 2_655 ?
O19 Mo5 K3 46.88(9) . 2_655 ?
O11 Mo5 K3 114.71(7) . 2_655 ?
O8 Mo5 K3 68.63(7) 2_654 2_655 ?
O10 Mo5 K3 107.93(6) . 2_655 ?
O12 Mo5 K3 45.28(6) . 2_655 ?
O18 Mo5 K2 44.07(8) . 1_455 ?
O19 Mo5 K2 105.82(9) . 1_455 ?
O11 Mo5 K2 55.05(7) . 1_455 ?
O8 Mo5 K2 137.80(7) 2_654 1_455 ?
O10 Mo5 K2 96.02(6) . 1_455 ?
O12 Mo5 K2 135.34(6) . 1_455 ?
K3 Mo5 K2 150.287(19) 2_655 1_455 ?
O18 Mo5 K2 31.50(8) . 2_654 ?
O19 Mo5 K2 111.85(9) . 2_654 ?
O11 Mo5 K2 121.74(7) . 2_654 ?
O8 Mo5 K2 66.79(7) 2_654 2_654 ?
O10 Mo5 K2 88.90(6) . 2_654 ?
O12 Mo5 K2 144.96(6) . 2_654 ?
K3 Mo5 K2 123.536(18) 2_655 2_654 ?
K2 Mo5 K2 72.970(19) 1_455 2_654 ?
O2W K1 O1W 87.09(10) . . ?
O2W K1 O3W 118.04(10) . . ?
O1W K1 O3W 143.21(10) . . ?
O2W K1 O6W 159.36(16) . . ?
O1W K1 O6W 77.30(17) . . ?
O3W K1 O6W 82.18(16) . . ?
O2W K1 O7W 147.28(16) . . ?
O1W K1 O7W 90.37(16) . . ?
O3W K1 O7W 81.82(16) . . ?
O6W K1 O7W 22.98(19) . . ?
O2W K1 O2W 85.02(10) . 2_744 ?
O1W K1 O2W 141.84(10) . 2_744 ?
O3W K1 O2W 71.15(10) . 2_744 ?
O6W K1 O2W 98.90(18) . 2_744 ?
O7W K1 O2W 77.04(16) . 2_744 ?
O2W K1 O13 122.30(9) . . ?
O1W K1 O13 75.27(8) . . ?
O3W K1 O13 68.64(9) . . ?
O6W K1 O13 66.87(16) . . ?
O7W K1 O13 88.29(16) . . ?
O2W K1 O13 138.71(9) 2_744 . ?
O2W K1 O4W 86.32(10) . . ?
O1W K1 O4W 77.76(9) . . ?
O3W K1 O4W 126.84(10) . . ?
O6W K1 O4W 77.32(16) . . ?
O7W K1 O4W 61.32(16) . . ?
O2W K1 O4W 64.52(9) 2_744 . ?
O13 K1 O4W 138.86(9) . . ?
O2W K1 Mo1 101.54(7) . . ?
O1W K1 Mo1 62.98(6) . . ?
O3W K1 Mo1 84.74(7) . . ?
O6W K1 Mo1 83.45(16) . . ?
O7W K1 Mo1 106.26(15) . . ?
O2W K1 Mo1 155.10(7) 2_744 . ?
O13 K1 Mo1 22.30(5) . . ?
O4W K1 Mo1 139.22(7) . . ?
O2W K1 K1 43.43(7) . 2_744 ?
O1W K1 K1 120.58(7) . 2_744 ?
O3W K1 K1 95.18(8) . 2_744 ?
O6W K1 K1 136.92(17) . 2_744 ?
O7W K1 K1 113.94(15) . 2_744 ?
O2W K1 K1 41.59(7) 2_744 2_744 ?
O13 K1 K1 150.98(7) . 2_744 ?
O4W K1 K1 70.15(8) . 2_744 ?
Mo1 K1 K1 139.39(4) . 2_744 ?
O2W K1 K4 115.91(7) . . ?
O1W K1 K4 53.04(7) . . ?
O3W K1 K4 123.38(8) . . ?
O6W K1 K4 43.57(14) . . ?
O7W K1 K4 42.31(14) . . ?
O2W K1 K4 98.09(7) 2_744 . ?
O13 K1 K4 96.13(6) . . ?
O4W K1 K4 42.75(7) . . ?
Mo1 K1 K4 100.41(3) . . ?
K1 K1 K4 112.84(4) 2_744 . ?
O2W K1 K3 102.12(7) . 2_645 ?
O1W K1 K3 120.49(7) . 2_645 ?
O3W K1 K3 33.23(7) . 2_645 ?
O6W K1 K3 97.44(14) . 2_645 ?
O7W K1 K3 107.18(14) . 2_645 ?
O2W K1 K3 97.67(7) 2_744 2_645 ?
O13 K1 K3 49.98(5) . 2_645 ?
O4W K1 K3 159.86(7) . 2_645 ?
Mo1 K1 K3 57.541(18) . 2_645 ?
K1 K1 K3 103.42(3) 2_744 2_645 ?
K4 K1 K3 139.80(3) . 2_645 ?
O2W K1 H1W1 97.9(8) . . ?
O1W K1 H1W1 14.2(5) . . ?
O3W K1 H1W1 129.0(5) . . ?
O6W K1 H1W1 69.3(9) . . ?
O7W K1 H1W1 86.3(9) . . ?
O2W K1 H1W1 152.0(7) 2_744 . ?
O13 K1 H1W1 61.6(5) . . ?
O4W K1 H1W1 87.7(6) . . ?
Mo1 K1 H1W1 51.7(6) . . ?
K1 K1 H1W1 134.5(6) 2_744 . ?
K4 K1 H1W1 55.5(9) . . ?
K3 K1 H1W1 108.8(5) 2_645 . ?
O2W K1 H2W2 16.0(4) . . ?
O1W K1 H2W2 82.9(9) . . ?
O3W K1 H2W2 113.6(9) . . ?
O6W K1 H2W2 160.1(9) . . ?
O7W K1 H2W2 161.6(7) . . ?
O2W K1 H2W2 97.8(6) 2_744 . ?
O13 K1 H2W2 106.4(4) . . ?
O4W K1 H2W2 100.4(7) . . ?
Mo1 K1 H2W2 85.9(4) . . ?
K1 K1 H2W2 56.8(5) 2_744 . ?
K4 K1 H2W2 123.0(9) . . ?
K3 K1 H2W2 90.9(8) 2_645 . ?
H1W1 K1 H2W2 91.0(12) . . ?
O2W K1 H3W1 134.8(4) . . ?
O1W K1 H3W1 131.0(6) . . ?
O3W K1 H3W1 16.8(4) . . ?
O6W K1 H3W1 65.5(4) . . ?
O7W K1 H3W1 67.4(7) . . ?
O2W K1 H3W1 77.1(8) 2_744 . ?
O13 K1 H3W1 61.6(9) . . ?
O4W K1 H3W1 120.7(9) . . ?
Mo1 K1 H3W1 81.5(9) . . ?
K1 K1 H3W1 108.4(6) 2_744 . ?
K4 K1 H3W1 107.6(5) . . ?
K3 K1 H3W1 41.8(8) 2_645 . ?
H1W1 K1 H3W1 117.1(8) . . ?
H2W2 K1 H3W1 129.3(11) . . ?
O2W K1 H4W2 78.5(8) . . ?
O1W K1 H4W2 89.9(7) . . ?
O3W K1 H4W2 119.8(9) . . ?
O6W K1 H4W2 88.0(7) . . ?
O7W K1 H4W2 68.9(8) . . ?
O2W K1 H4W2 52.0(7) 2_744 . ?
O13 K1 H4W2 152.9(5) . . ?
O4W K1 H4W2 14.7(4) . . ?
Mo1 K1 H4W2 152.7(7) . . ?
K1 K1 H4W2 56.1(5) 2_744 . ?
K4 K1 H4W2 57.2(4) . . ?
K3 K1 H4W2 149.6(7) 2_645 . ?
H1W1 K1 H4W2 101.1(9) . . ?
H2W2 K1 H4W2 93.9(10) . . ?
H3W1 K1 H4W2 118.2(14) . . ?
O2W K1 H6W2 164.6(8) . . ?
O1W K1 H6W2 90.4(6) . . ?
O3W K1 H6W2 71.9(8) . . ?
O6W K1 H6W2 13.2(6) . . ?
O7W K1 H6W2 17.4(8) . . ?
O2W K1 H6W2 87.6(6) 2_744 . ?
O13 K1 H6W2 71.5(7) . . ?
O4W K1 H6W2 78.3(8) . . ?
Mo1 K1 H6W2 90.8(7) . . ?
K1 K1 H6W2 127.8(6) 2_744 . ?
K4 K1 H6W2 51.9(8) . . ?
K3 K1 H6W2 92.3(8) 2_645 . ?
H1W1 K1 H6W2 82.5(11) . . ?
H2W2 K1 H6W2 173.3(11) . . ?
H3W1 K1 H6W2 55.7(9) . . ?
H4W2 K1 H6W2 86.3(11) . . ?
O2 K2 O18 145.16(9) 2_755 2_654 ?
O2 K2 O15 76.87(8) 2_755 . ?
O18 K2 O15 77.87(7) 2_654 . ?
O2 K2 O17 122.28(8) 2_755 1_655 ?
O18 K2 O17 80.12(7) 2_654 1_655 ?
O15 K2 O17 157.94(7) . 1_655 ?
O2 K2 O5 100.45(8) 2_755 . ?
O18 K2 O5 91.65(7) 2_654 . ?
O15 K2 O5 67.65(7) . . ?
O17 K2 O5 114.57(7) 1_655 . ?
O2 K2 O1W 92.04(9) 2_755 . ?
O18 K2 O1W 122.47(8) 2_654 . ?
O15 K2 O1W 127.32(8) . . ?
O17 K2 O1W 67.11(8) 1_655 . ?
O5 K2 O1W 64.10(7) . . ?
O2 K2 O18 95.18(8) 2_755 1_655 ?
O18 K2 O18 67.28(8) 2_654 1_655 ?
O15 K2 O18 102.13(7) . 1_655 ?
O17 K2 O18 67.64(7) 1_655 1_655 ?
O5 K2 O18 158.50(7) . 1_655 ?
O1W K2 O18 130.32(8) . 1_655 ?
O2 K2 O11 72.42(7) 2_755 1_655 ?
O18 K2 O11 111.63(7) 2_654 1_655 ?
O15 K2 O11 135.47(7) . 1_655 ?
O17 K2 O11 53.66(6) 1_655 1_655 ?
O5 K2 O11 148.92(7) . 1_655 ?
O1W K2 O11 85.61(7) . 1_655 ?
O18 K2 O11 50.84(6) 1_655 1_655 ?
O2 K2 Mo3 97.05(6) 2_755 1_655 ?
O18 K2 Mo3 102.06(6) 2_654 1_655 ?
O15 K2 Mo3 166.40(6) . 1_655 ?
O17 K2 Mo3 25.23(5) 1_655 1_655 ?
O5 K2 Mo3 125.79(5) . 1_655 ?
O1W K2 Mo3 64.38(6) . 1_655 ?
O18 K2 Mo3 65.96(5) 1_655 1_655 ?
O11 K2 Mo3 31.77(4) 1_655 1_655 ?
O2 K2 Mo5 81.66(6) 2_755 1_655 ?
O18 K2 Mo5 88.90(6) 2_654 1_655 ?
O15 K2 Mo5 117.01(6) . 1_655 ?
O17 K2 Mo5 60.93(5) 1_655 1_655 ?
O5 K2 Mo5 175.30(5) . 1_655 ?
O1W K2 Mo5 111.77(6) . 1_655 ?
O18 K2 Mo5 23.36(5) 1_655 1_655 ?
O11 K2 Mo5 27.81(4) 1_655 1_655 ?
Mo3 K2 Mo5 49.574(11) 1_655 1_655 ?
O2 K2 Mo5 139.92(7) 2_755 2_654 ?
O18 K2 Mo5 19.25(5) 2_654 2_654 ?
O15 K2 Mo5 64.20(5) . 2_654 ?
O17 K2 Mo5 94.69(5) 1_655 2_654 ?
O5 K2 Mo5 74.11(5) . 2_654 ?
O1W K2 Mo5 118.54(6) . 2_654 ?
O18 K2 Mo5 84.42(5) 1_655 2_654 ?
O11 K2 Mo5 130.85(4) 1_655 2_654 ?
Mo3 K2 Mo5 118.67(2) 1_655 2_654 ?
Mo5 K2 Mo5 107.030(18) 1_655 2_654 ?
O2 K2 Mo4 95.00(6) 2_755 . ?
O18 K2 Mo4 64.40(5) 2_654 . ?
O15 K2 Mo4 19.13(5) . . ?
O17 K2 Mo4 142.32(5) 1_655 . ?
O5 K2 Mo4 57.41(5) . . ?
O1W K2 Mo4 121.41(6) . . ?
O18 K2 Mo4 106.81(5) 1_655 . ?
O11 K2 Mo4 151.17(5) 1_655 . ?
Mo3 K2 Mo4 166.45(2) 1_655 . ?
Mo5 K2 Mo4 126.81(2) 1_655 . ?
Mo5 K2 Mo4 47.961(10) 2_654 . ?
O2 K2 H1W2 85.4(8) 2_755 . ?
O18 K2 H1W2 129.0(8) 2_654 . ?
O15 K2 H1W2 139.3(6) . . ?
O17 K2 H1W2 59.2(7) 1_655 . ?
O5 K2 H1W2 80.2(3) . . ?
O1W K2 H1W2 16.5(3) . . ?
O18 K2 H1W2 115.9(4) 1_655 . ?
O11 K2 H1W2 69.2(3) 1_655 . ?
Mo3 K2 H1W2 50.5(5) 1_655 . ?
Mo5 K2 H1W2 95.8(3) 1_655 . ?
Mo5 K2 H1W2 130.6(7) 2_654 . ?
Mo4 K2 H1W2 137.1(3) . . ?
O4 K3 O3W 88.45(10) . 2_645 ?
O4 K3 O12 67.90(8) . 2_655 ?
O3W K3 O12 80.04(9) 2_645 2_655 ?
O4 K3 O14 128.49(8) . 2_645 ?
O3W K3 O14 81.05(9) 2_645 2_645 ?
O12 K3 O14 154.47(8) 2_655 2_645 ?
O4 K3 O19 75.69(8) . 2_655 ?
O3W K3 O19 137.77(9) 2_645 2_655 ?
O12 K3 O19 57.75(7) 2_655 2_655 ?
O14 K3 O19 138.89(8) 2_645 2_655 ?
O4 K3 O7 141.04(8) . 1_556 ?
O3W K3 O7 70.54(9) 2_645 1_556 ?
O12 K3 O7 76.17(7) 2_655 1_556 ?
O14 K3 O7 81.45(7) 2_645 1_556 ?
O19 K3 O7 97.85(7) 2_655 1_556 ?
O4 K3 O14 144.15(8) . 1_556 ?
O3W K3 O14 122.92(9) 2_645 1_556 ?
O12 K3 O14 98.47(7) 2_655 1_556 ?
O14 K3 O14 77.80(8) 2_645 1_556 ?
O19 K3 O14 69.28(7) 2_655 1_556 ?
O7 K3 O14 54.30(6) 1_556 1_556 ?
O4 K3 O4W 96.14(10) . 2_745 ?
O3W K3 O4W 165.64(10) 2_645 2_745 ?
O12 K3 O4W 114.30(8) 2_655 2_745 ?
O14 K3 O4W 85.48(8) 2_645 2_745 ?
O19 K3 O4W 56.55(8) 2_655 2_745 ?
O7 K3 O4W 112.40(8) 1_556 2_745 ?
O14 K3 O4W 58.10(8) 1_556 2_745 ?
O4 K3 O6 81.17(8) . 2_645 ?
O3W K3 O6 107.94(8) 2_645 2_645 ?
O12 K3 O6 148.02(7) 2_655 2_645 ?
O14 K3 O6 55.51(6) 2_645 2_645 ?
O19 K3 O6 107.87(7) 2_655 2_645 ?
O7 K3 O6 135.80(6) 1_556 2_645 ?
O14 K3 O6 102.18(6) 1_556 2_645 ?
O4W K3 O6 59.66(7) 2_745 2_645 ?
O4 K3 Mo2 109.19(7) . 2_645 ?
O3W K3 Mo2 95.82(7) 2_645 2_645 ?
O12 K3 Mo2 174.88(6) 2_655 2_645 ?
O14 K3 Mo2 25.02(5) 2_645 2_645 ?
O19 K3 Mo2 126.27(6) 2_655 2_645 ?
O7 K3 Mo2 105.38(5) 1_556 2_645 ?
O14 K3 Mo2 86.29(5) 1_556 2_645 ?
O4W K3 Mo2 69.82(6) 2_745 2_645 ?
O6 K3 Mo2 30.73(4) 2_645 2_645 ?
O4 K3 Mo2 142.86(6) . 1_556 ?
O3W K3 Mo2 102.74(8) 2_645 1_556 ?
O12 K3 Mo2 79.18(5) 2_655 1_556 ?
O14 K3 Mo2 88.47(5) 2_645 1_556 ?
O19 K3 Mo2 72.34(5) 2_655 1_556 ?
O7 K3 Mo2 32.28(4) 1_556 1_556 ?
O14 K3 Mo2 25.63(4) 1_556 1_556 ?
O4W K3 Mo2 81.73(7) 2_745 1_556 ?
O6 K3 Mo2 126.49(5) 2_645 1_556 ?
Mo2 K3 Mo2 104.79(2) 2_645 1_556 ?
O4 K3 Mo5 82.94(6) . 2_655 ?
O3W K3 Mo5 115.41(7) 2_645 2_655 ?
O12 K3 Mo5 37.77(5) 2_655 2_655 ?
O14 K3 Mo5 146.41(6) 2_645 2_655 ?
O19 K3 Mo5 25.25(5) 2_655 2_655 ?
O7 K3 Mo5 77.58(5) 1_556 2_655 ?
O14 K3 Mo5 68.67(5) 1_556 2_655 ?
O4W K3 Mo5 78.74(6) 2_745 2_655 ?
O6 K3 Mo5 133.12(5) 2_645 2_655 ?
Mo2 K3 Mo5 147.13(3) 2_645 2_655 ?
Mo2 K3 Mo5 60.181(14) 1_556 2_655 ?
O3 K4 O4W 101.84(10) 2_745 . ?
O3 K4 O7W 70.19(14) 2_745 . ?
O4W K4 O7W 65.82(15) . . ?
O3 K4 O6W 79.70(14) 2_745 . ?
O4W K4 O6W 82.15(17) . . ?
O7W K4 O6W 22.36(19) . . ?
O3 K4 O4 83.68(8) 2_745 1_655 ?
O4W K4 O4 147.52(11) . 1_655 ?
O7W K4 O4 143.29(14) . 1_655 ?
O6W K4 O4 130.15(16) . 1_655 ?
O3 K4 O16 159.38(9) 2_745 1_655 ?
O4W K4 O16 71.31(9) . 1_655 ?
O7W K4 O16 121.03(14) . 1_655 ?
O6W K4 O16 117.41(13) . 1_655 ?
O4 K4 O16 92.23(8) 1_655 1_655 ?
O3 K4 O5W 116.98(10) 2_745 . ?
O4W K4 O5W 136.88(12) . . ?
O7W K4 O5W 109.14(17) . . ?
O6W K4 O5W 86.78(18) . . ?
O4 K4 O5W 60.14(9) 1_655 . ?
O16 K4 O5W 77.43(9) 1_655 . ?
O3 K4 O6 101.09(8) 2_745 1_655 ?
O4W K4 O6 68.20(10) . 1_655 ?
O7W K4 O6 129.73(15) . 1_655 ?
O6W K4 O6 149.96(17) . 1_655 ?
O4 K4 O6 79.32(7) 1_655 1_655 ?
O16 K4 O6 58.30(7) 1_655 1_655 ?
O5W K4 O6 118.03(9) . 1_655 ?
O3 K4 C4 90.34(9) 2_745 1_655 ?
O4W K4 C4 125.17(11) . 1_655 ?
O7W K4 C4 159.97(15) . 1_655 ?
O6W K4 C4 152.50(16) . 1_655 ?
O4 K4 C4 22.39(8) 1_655 1_655 ?
O16 K4 C4 78.93(9) 1_655 1_655 ?
O5W K4 C4 74.94(10) . 1_655 ?
O6 K4 C4 56.99(8) 1_655 1_655 ?
O3 K4 O1W 146.95(8) 2_745 . ?
O4W K4 O1W 74.65(11) . . ?
O7W K4 O1W 78.81(15) . . ?
O6W K4 O1W 67.24(14) . . ?
O4 K4 O1W 117.27(9) 1_655 . ?
O16 K4 O1W 51.58(7) 1_655 . ?
O5W K4 O1W 62.67(9) . . ?
O6 K4 O1W 107.53(7) 1_655 . ?
C4 K4 O1W 119.00(9) 1_655 . ?
O3 K4 O13 53.48(7) 2_745 2_745 ?
O4W K4 O13 140.50(9) . 2_745 ?
O7W K4 O13 76.05(14) . 2_745 ?
O6W K4 O13 64.68(14) . 2_745 ?
O4 K4 O13 67.64(7) 1_655 2_745 ?
O16 K4 O13 142.39(8) 1_655 2_745 ?
O5W K4 O13 65.04(9) . 2_745 ?
O6 K4 O13 139.20(7) 1_655 2_745 ?
C4 K4 O13 88.75(8) 1_655 2_745 ?
O1W K4 O13 108.56(7) . 2_745 ?
O3 K4 Mo1 29.09(5) 2_745 2_745 ?
O4W K4 Mo1 123.97(8) . 2_745 ?
O7W K4 Mo1 70.01(13) . 2_745 ?
O6W K4 Mo1 68.20(12) . 2_745 ?
O4 K4 Mo1 74.63(6) 1_655 2_745 ?
O16 K4 Mo1 164.71(6) 1_655 2_745 ?
O5W K4 Mo1 89.07(8) . 2_745 ?
O6 K4 Mo1 124.73(5) 1_655 2_745 ?
C4 K4 Mo1 90.76(7) 1_655 2_745 ?
O1W K4 Mo1 127.72(6) . 2_745 ?
O13 K4 Mo1 24.46(4) 2_745 2_745 ?
O3 K4 H1W2 161.5(3) 2_745 . ?
O4W K4 H1W2 75.4(8) . . ?
O7W K4 H1W2 92.4(5) . . ?
O6W K4 H1W2 81.8(3) . . ?
O4 K4 H1W2 108.6(7) 1_655 . ?
O16 K4 H1W2 37.5(3) 1_655 . ?
O5W K4 H1W2 61.8(8) . . ?
O6 K4 H1W2 94.9(4) 1_655 . ?
C4 K4 H1W2 106.3(5) 1_655 . ?
O1W K4 H1W2 14.5(3) . . ?
O13 K4 H1W2 117.5(6) 2_745 . ?
Mo1 K4 H1W2 139.4(5) 2_745 . ?
O3 K4 H4W1 110.1(9) 2_745 . ?
O4W K4 H4W1 15.5(4) . . ?
O7W K4 H4W1 81.2(4) . . ?
O6W K4 H4W1 96.6(5) . . ?
O4 K4 H4W1 133.2(4) 1_655 . ?
O16 K4 H4W1 59.1(8) 1_655 . ?
O5W K4 H4W1 132.6(10) . . ?
O6 K4 H4W1 54.6(5) 1_655 . ?
C4 K4 H4W1 110.9(5) 1_655 . ?
O1W K4 H4W1 75.2(10) . . ?
O13 K4 H4W1 155.6(5) 2_745 . ?
Mo1 K4 H4W1 136.0(8) 2_745 . ?
H1W2 K4 H4W1 72.0(12) . . ?
O3 K4 H5W1 115.4(10) 2_745 . ?
O4W K4 H5W1 142.7(9) . . ?
O7W K4 H5W1 124.4(4) . . ?
O6W K4 H5W1 102.1(4) . . ?
O4 K4 H5W1 46.0(5) 1_655 . ?
O16 K4 H5W1 74.1(10) 1_655 . ?
O5W K4 H5W1 15.9(2) . . ?
O6 K4 H5W1 104.4(5) 1_655 . ?
C4 K4 H5W1 59.2(3) 1_655 . ?
O1W K4 H5W1 73.2(7) . . ?
O13 K4 H5W1 69.2(9) 2_745 . ?
Mo1 K4 H5W1 91.0(10) 2_745 . ?
H1W2 K4 H5W1 68.7(11) . . ?
H4W1 K4 H5W1 133.0(13) . . ?
O3 K4 H6W1 86.5(7) 2_745 . ?
O4W K4 H6W1 92.2(8) . . ?
O7W K4 H6W1 35.9(5) . . ?
O6W K4 H6W1 13.6(5) . . ?
O4 K4 H6W1 120.2(8) 1_655 . ?
O16 K4 H6W1 112.7(7) 1_655 . ?
O5W K4 H6W1 73.2(5) . . ?
O6 K4 H6W1 159.9(8) 1_655 . ?
C4 K4 H6W1 142.3(7) 1_655 . ?
O1W K4 H6W1 61.1(7) . . ?
O13 K4 H6W1 59.6(9) 2_745 . ?
Mo1 K4 H6W1 69.2(8) 2_745 . ?
H1W2 K4 H6W1 75.4(8) . . ?
H4W1 K4 H6W1 105.4(10) . . ?
H5W1 K4 H6W1 88.6(6) . . ?
C3 N1 C1 116.3(3) . . ?
C3 N1 Mo1 109.7(2) . . ?
C1 N1 Mo1 109.8(2) . . ?
C3 N1 H1C 106.9 . . ?
C1 N1 H1C 106.9 . . ?
Mo1 N1 H1C 106.9 . . ?
C2 O1 Mo1 123.9(2) . . ?
C2 O2 K2 139.7(3) . 2_755 ?
C4 O3 Mo1 119.9(2) . . ?
C4 O3 K4 128.0(2) . 2_745 ?
Mo1 O3 K4 111.31(10) . 2_745 ?
C4 O4 K3 129.2(2) . . ?
C4 O4 K4 95.4(2) . 1_455 ?
K3 O4 K4 130.58(10) . 1_455 ?
Mo1 O5 Mo2 83.22(9) . . ?
Mo1 O5 K2 145.33(11) . . ?
Mo2 O5 K2 130.33(10) . . ?
Mo1 O6 Mo2 83.46(9) . . ?
Mo1 O6 K4 128.92(10) . 1_455 ?
Mo2 O6 K4 147.59(11) . 1_455 ?
Mo1 O6 K3 100.27(9) . 2_645 ?
Mo2 O6 K3 88.09(8) . 2_645 ?
K4 O6 K3 87.24(6) 1_455 2_645 ?
Mo3 O7 Mo2 115.70(11) . . ?
Mo3 O7 K3 139.06(11) . 1_554 ?
Mo2 O7 K3 94.47(8) . 1_554 ?
Mo5 O8 Mo2 147.20(12) 2_654 . ?
Mo5 O8 Mo4 106.71(10) 2_654 . ?
Mo2 O8 Mo4 105.63(10) . . ?
Mo4 O9 Mo3 113.47(10) . . ?
Mo4 O9 Mo2 105.53(10) . . ?
Mo3 O9 Mo2 92.81(8) . . ?
Mo4 O10 Mo3 150.24(12) 2_654 . ?
Mo4 O10 Mo5 103.90(10) 2_654 . ?
Mo3 O10 Mo5 95.16(8) . . ?
Mo4 O10 Mo4 104.07(9) 2_654 . ?
Mo3 O10 Mo4 95.90(8) . . ?
Mo5 O10 Mo4 97.03(8) . . ?
Mo5 O11 Mo3 114.95(11) . . ?
Mo5 O11 K2 97.14(9) . 1_455 ?
Mo3 O11 K2 88.24(8) . 1_455 ?
Mo4 O12 Mo5 115.27(11) . . ?
Mo4 O12 K3 136.35(12) . 2_655 ?
Mo5 O12 K3 96.95(8) . 2_655 ?
Mo1 O13 K1 118.16(12) . . ?
Mo1 O13 K4 100.06(10) . 2_745 ?
K1 O13 K4 139.72(9) . 2_745 ?
Mo2 O14 K3 108.94(11) . 2_645 ?
Mo2 O14 K3 102.42(10) . 1_554 ?
K3 O14 K3 102.20(8) 2_645 1_554 ?
Mo4 O15 K2 128.78(12) . . ?
Mo3 O16 K4 136.54(12) . 1_455 ?
Mo3 O17 K2 110.08(11) . 1_455 ?
Mo5 O18 K2 129.25(12) . 2_654 ?
Mo5 O18 K2 112.57(11) . 1_455 ?
K2 O18 K2 112.72(8) 2_654 1_455 ?
Mo5 O19 K3 107.87(11) . 2_655 ?
N1 C1 C2 111.6(3) . . ?
N1 C1 H1A 109.3 . . ?
C2 C1 H1A 109.3 . . ?
N1 C1 H1B 109.3 . . ?
C2 C1 H1B 109.3 . . ?
H1A C1 H1B 108.0 . . ?
O2 C2 O1 123.2(4) . . ?
O2 C2 C1 121.0(3) . . ?
O1 C2 C1 115.8(3) . . ?
N1 C3 C4 111.7(3) . . ?
N1 C3 H3A 109.3 . . ?
C4 C3 H3A 109.3 . . ?
N1 C3 H3B 109.3 . . ?
C4 C3 H3B 109.3 . . ?
H3A C3 H3B 107.9 . . ?
O4 C4 O3 123.8(4) . . ?
O4 C4 C3 119.7(3) . . ?
O3 C4 C3 116.5(3) . . ?
O4 C4 K4 62.25(19) . 1_455 ?
O3 C4 K4 98.6(2) . 1_455 ?
C3 C4 K4 109.3(2) . 1_455 ?
K1 O1W K2 108.88(10) . . ?
K1 O1W K4 85.51(9) . . ?
K2 O1W K4 145.49(10) . . ?
K1 O1W H1W1 113(3) . . ?
K2 O1W H1W1 106(4) . . ?
K4 O1W H1W1 96(3) . . ?
K1 O1W H1W2 128(3) . . ?
K2 O1W H1W2 85(4) . . ?
K4 O1W H1W2 62(4) . . ?
H1W1 O1W H1W2 110.3(17) . . ?
K1 O2W K1 94.98(10) . 2_744 ?
K1 O2W H2W1 136(3) . . ?
K1 O2W H2W1 43(3) 2_744 . ?
K1 O2W H2W2 104(3) . . ?
K1 O2W H2W2 139(3) 2_744 . ?
H2W1 O2W H2W2 105.4(16) . . ?
K3 O3W K1 113.23(12) 2_645 . ?
K3 O3W H3W1 107(4) 2_645 . ?
K1 O3W H3W1 94(3) . . ?
K3 O3W H3W2 97(4) 2_645 . ?
K1 O3W H3W2 133(4) . . ?
H3W1 O3W H3W2 110.6(18) . . ?
K4 O4W K1 87.07(12) . . ?
K4 O4W K3 92.97(12) . 2_745 ?
K1 O4W K3 151.66(13) . 2_745 ?
K4 O4W H4W1 104(3) . . ?
K1 O4W H4W1 128(4) . . ?
K3 O4W H4W1 79(4) 2_745 . ?
K4 O4W H4W2 140(3) . . ?
K1 O4W H4W2 55(4) . . ?
K3 O4W H4W2 115(4) 2_745 . ?
H4W1 O4W H4W2 108.8(17) . . ?
K4 O5W H5W1 88(3) . . ?
K4 O5W H5W2 155(3) . . ?
H5W1 O5W H5W2 111.0(18) . . ?
O7W O6W K1 78.1(5) . . ?
O7W O6W K4 75.7(5) . . ?
K1 O6W K4 94.70(19) . . ?
O7W O6W H6W1 170(4) . . ?
K1 O6W H6W1 99(3) . . ?
K4 O6W H6W1 114(3) . . ?
O7W O6W H6W2 63(3) . . ?
K1 O6W H6W2 119(4) . . ?
K4 O6W H6W2 117(3) . . ?
H6W1 O6W H6W2 111.8(18) . . ?
O6W O7W K1 78.9(5) . . ?
O6W O7W K4 81.9(5) . . ?
K1 O7W K4 96.2(2) . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        27.00
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         1.070
_refine_diff_density_min         -0.994
_refine_diff_density_rms         0.162
_database_code_depnum_ccdc_archive 'CCDC 987094'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_sad

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C8 H32 Mo2 N6 O17'
_chemical_formula_weight         676.28

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'
Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           ?
_symmetry_space_group_name_H-M   P-1

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

_cell_length_a                   6.7791(3)
_cell_length_b                   12.8945(6)
_cell_length_c                   14.1217(7)
_cell_angle_alpha                109.5420(10)
_cell_angle_beta                 90.9030(10)
_cell_angle_gamma                103.5270(10)
_cell_volume                     1125.08(9)
_cell_formula_units_Z            2
_cell_measurement_temperature    446(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       ?
_exptl_crystal_colour            ?
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.17
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.996
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             684
_exptl_absorpt_coefficient_mu    1.206
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  0.6846
_exptl_absorpt_correction_T_max  0.8213
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      446(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            11808
_diffrn_reflns_av_R_equivalents  0.0794
_diffrn_reflns_av_sigmaI/netI    0.0562
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         1.54
_diffrn_reflns_theta_max         26.00
_reflns_number_total             4415
_reflns_number_gt                4249
_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 F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² 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/[σ²(Fo²)+(0.0283P)²+1.1882P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.0413(14)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         4415
_refine_ls_number_parameters     353
_refine_ls_number_restraints     31
_refine_ls_R_factor_all          0.0325
_refine_ls_R_factor_gt           0.0311
_refine_ls_wR_factor_ref         0.0788
_refine_ls_wR_factor_gt          0.0777
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_restrained_S_all      1.051
_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
Mo1 Mo 0.19775(3) -0.29095(2) 0.061592(16) 0.02150(10) Uani 1 1 d . . .
Mo2 Mo 0.37726(3) 0.19185(2) 0.433364(16) 0.02228(11) Uani 1 1 d . . .
N1 N -0.1457(3) -0.3627(2) 0.06622(17) 0.0227(5) Uani 1 1 d . . .
H1C H -0.1639 -0.4329 0.0710 0.027 Uiso 1 1 calc R . .
N2 N 0.0306(3) 0.1269(2) 0.39870(17) 0.0232(5) Uani 1 1 d . . .
H2A H 0.0007 0.0507 0.3639 0.028 Uiso 1 1 calc R . .
N3 N 0.3256(4) -0.4467(3) 0.3039(2) 0.0398(6) Uani 1 1 d D . .
N4 N -0.6402(4) -0.2277(3) -0.1773(2) 0.0478(8) Uani 1 1 d D . .
N5 N 0.1911(6) 0.5113(3) 0.5453(3) 0.0650(11) Uani 1 1 d D . .
N6 N -0.1433(6) -0.0287(3) -0.1076(3) 0.0579(9) Uani 1 1 d D . .
O1 O 0.0951(3) -0.15892(18) 0.17920(15) 0.0300(4) Uani 1 1 d . . .
O2 O -0.1449(3) -0.1054(2) 0.27327(18) 0.0419(5) Uani 1 1 d . . .
O3 O 0.0203(3) -0.22281(18) -0.02670(15) 0.0306(4) Uani 1 1 d . . .
O4 O -0.2653(3) -0.2516(2) -0.11981(18) 0.0425(6) Uani 1 1 d . . .
O5 O 0.2569(3) -0.3415(2) 0.15523(16) 0.0324(5) Uani 1 1 d . . .
O6 O 0.1897(3) -0.40415(19) -0.04993(16) 0.0331(5) Uani 1 1 d . . .
O7 O 0.4102(3) -0.1851(2) 0.06296(18) 0.0377(5) Uani 1 1 d . . .
O11 O 0.2735(3) 0.3132(2) 0.37766(18) 0.0375(5) Uani 1 1 d . . .
O12 O 0.0286(3) 0.3508(2) 0.29944(17) 0.0386(5) Uani 1 1 d . . .
O13 O 0.2393(3) 0.2900(2) 0.56094(16) 0.0372(5) Uani 1 1 d . . .
O14 O -0.0287(4) 0.3001(3) 0.64705(17) 0.0512(7) Uani 1 1 d . . .
O15 O 0.6035(3) 0.2959(2) 0.48452(17) 0.0363(5) Uani 1 1 d . . .
O16 O 0.4110(3) 0.1189(2) 0.30921(16) 0.0361(5) Uani 1 1 d . . .
O17 O 0.3709(3) 0.0907(2) 0.48911(16) 0.0344(5) Uani 1 1 d . . .
C1 C -0.2256(4) -0.2909(3) 0.1541(2) 0.0319(6) Uani 1 1 d . . .
H1A H -0.2535 -0.3302 0.2021 0.038 Uiso 1 1 calc R . .
H1B H -0.3537 -0.2808 0.1319 0.038 Uiso 1 1 calc R . .
C2 C -0.0837(4) -0.1765(3) 0.2064(2) 0.0273(6) Uani 1 1 d . . .
C3 C -0.2519(4) -0.3760(3) -0.0302(2) 0.0302(6) Uani 1 1 d . . .
H3A H -0.3957 -0.3815 -0.0230 0.036 Uiso 1 1 calc R . .
H3B H -0.2395 -0.4455 -0.0816 0.036 Uiso 1 1 calc R . .
C4 C -0.1618(4) -0.2758(3) -0.0619(2) 0.0290(6) Uani 1 1 d . . .
C11 C -0.0494(4) 0.1810(3) 0.3350(2) 0.0306(6) Uani 1 1 d . . .
H11A H -0.1772 0.1965 0.3578 0.037 Uiso 1 1 calc R . .
H11B H -0.0777 0.1281 0.2660 0.037 Uiso 1 1 calc R . .
C12 C 0.0940(4) 0.2900(3) 0.3367(2) 0.0274(6) Uani 1 1 d . . .
C13 C -0.0616(4) 0.1443(3) 0.4949(2) 0.0310(6) Uani 1 1 d . . .
H13A H -0.0612 0.0811 0.5174 0.037 Uiso 1 1 calc R . .
H13B H -0.2021 0.1467 0.4848 0.037 Uiso 1 1 calc R . .
C14 C 0.0550(5) 0.2538(3) 0.5746(2) 0.0329(7) Uani 1 1 d . . .
O1W O 0.2898(5) -0.4945(3) -0.2460(2) 0.0610(8) Uani 1 1 d D . .
O2W O -0.5481(4) -0.1073(3) 0.3224(2) 0.0561(7) Uani 1 1 d D . .
O3W O 0.7099(5) 0.0089(3) 0.0868(2) 0.0570(7) Uani 1 1 d D . .
H1 H 0.354(6) -0.400(2) 0.3639(12) 0.068 Uiso 1 1 d D . .
H3 H 0.280(6) -0.417(3) 0.266(2) 0.068 Uiso 1 1 d D . .
H4 H 0.237(5) -0.506(2) 0.302(3) 0.068 Uiso 1 1 d D . .
H6 H -0.746(3) -0.280(2) -0.207(2) 0.068 Uiso 1 1 d D . .
H7 H -0.674(5) -0.172(2) -0.134(2) 0.068 Uiso 1 1 d D . .
H8 H -0.579(4) -0.203(3) -0.2215(19) 0.068 Uiso 1 1 d D . .
H9 H 0.261(6) 0.5746(16) 0.546(3) 0.068 Uiso 1 1 d D . .
H12 H 0.243(6) 0.459(2) 0.513(3) 0.068 Uiso 1 1 d D . .
H13 H -0.175(6) -0.0983(10) -0.121(3) 0.068 Uiso 1 1 d D . .
H14 H -0.029(3) 0.006(3) -0.080(3) 0.068 Uiso 1 1 d D . .
H16 H -0.181(6) -0.009(3) -0.154(2) 0.068 Uiso 1 1 d D . .
H1W1 H 0.267(7) -0.462(4) -0.1860(14) 0.068 Uiso 1 1 d D . .
H2W1 H -0.423(3) -0.102(4) 0.308(3) 0.068 Uiso 1 1 d D . .
H2W2 H -0.603(7) -0.065(4) 0.300(3) 0.068 Uiso 1 1 d D . .
H5 H -0.561(4) -0.253(3) -0.149(2) 0.068 Uiso 1 1 d D . .
H3W2 H 0.612(5) -0.048(3) 0.082(4) 0.068 Uiso 1 1 d D . .
H3W1 H 0.727(7) -0.015(4) 0.0244(12) 0.068 Uiso 1 1 d D . .
H1W2 H 0.317(7) -0.471(4) -0.295(3) 0.068 Uiso 1 1 d D . .


_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
Mo1 O7 1.732(2) . ?
Mo1 O5 1.736(2) . ?
Mo1 O6 1.742(2) . ?
Mo1 O1 2.200(2) . ?
Mo1 O3 2.2255(19) . ?
Mo1 N1 2.306(2) . ?
Mo2 O17 1.728(2) . ?
Mo2 O16 1.738(2) . ?
Mo2 O15 1.741(2) . ?
Mo2 O13 2.192(2) . ?
Mo2 O11 2.210(2) . ?
Mo2 N2 2.288(2) . ?
N1 C3 1.468(3) . ?
N1 C1 1.476(4) . ?
N2 C11 1.473(3) . ?
N2 C13 1.475(3) . ?
O1 C2 1.270(3) . ?
O2 C2 1.231(4) . ?
O3 C4 1.264(4) . ?
O4 C4 1.230(3) . ?
O11 C12 1.264(3) . ?
O12 C12 1.232(4) . ?
O13 C14 1.269(4) . ?
O14 C14 1.222(4) . ?
C1 C2 1.493(4) . ?
C3 C4 1.506(4) . ?
C11 C12 1.503(4) . ?
C13 C14 1.507(5) . ?

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
O7 Mo1 O5 105.91(10) . . ?
O7 Mo1 O6 105.93(11) . . ?
O5 Mo1 O6 103.61(11) . . ?
O7 Mo1 O1 87.06(9) . . ?
O5 Mo1 O1 87.67(9) . . ?
O6 Mo1 O1 159.33(9) . . ?
O7 Mo1 O3 88.16(9) . . ?
O5 Mo1 O3 158.52(9) . . ?
O6 Mo1 O3 87.48(9) . . ?
O1 Mo1 O3 76.73(8) . . ?
O7 Mo1 N1 153.81(10) . . ?
O5 Mo1 N1 90.59(9) . . ?
O6 Mo1 N1 89.23(9) . . ?
O1 Mo1 N1 73.17(8) . . ?
O3 Mo1 N1 70.95(7) . . ?
O17 Mo2 O16 101.98(11) . . ?
O17 Mo2 O15 105.89(10) . . ?
O16 Mo2 O15 106.49(10) . . ?
O17 Mo2 O13 89.98(10) . . ?
O16 Mo2 O13 159.15(10) . . ?
O15 Mo2 O13 86.14(10) . . ?
O17 Mo2 O11 159.50(9) . . ?
O16 Mo2 O11 87.61(10) . . ?
O15 Mo2 O11 88.30(9) . . ?
O13 Mo2 O11 76.02(9) . . ?
O17 Mo2 N2 88.28(9) . . ?
O16 Mo2 N2 91.04(9) . . ?
O15 Mo2 N2 154.17(10) . . ?
O13 Mo2 N2 72.10(8) . . ?
O11 Mo2 N2 73.31(8) . . ?
C3 N1 C1 112.5(2) . . ?
C3 N1 Mo1 107.72(16) . . ?
C1 N1 Mo1 112.14(16) . . ?
C11 N2 C13 112.8(2) . . ?
C11 N2 Mo2 111.44(16) . . ?
C13 N2 Mo2 108.65(17) . . ?
C2 O1 Mo1 122.10(19) . . ?
C4 O3 Mo1 119.69(18) . . ?
C12 O11 Mo2 121.05(19) . . ?
C14 O13 Mo2 121.0(2) . . ?
N1 C1 C2 113.7(2) . . ?
O2 C2 O1 123.8(3) . . ?
O2 C2 C1 118.8(3) . . ?
O1 C2 C1 117.4(3) . . ?
N1 C3 C4 110.1(2) . . ?
O4 C4 O3 124.5(3) . . ?
O4 C4 C3 119.5(3) . . ?
O3 C4 C3 116.0(2) . . ?
N2 C11 C12 113.5(2) . . ?
O12 C12 O11 124.7(3) . . ?
O12 C12 C11 118.2(3) . . ?
O11 C12 C11 117.1(2) . . ?
N2 C13 C14 110.7(2) . . ?
O14 C14 O13 124.7(3) . . ?
O14 C14 C13 119.7(3) . . ?
O13 C14 C13 115.6(3) . . ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         0.707
_refine_diff_density_min         -0.659
_refine_diff_density_rms         0.110
_database_code_depnum_ccdc_archive 'CCDC 987095'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_sad

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          'not measured'
_chemical_formula_moiety         ?
_chemical_formula_sum            'C11 H38 Cl Mo2 N7 O16'
_chemical_formula_weight         751.81

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mo Mo -1.6832 0.6857 '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

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                   7.10460(10)
_cell_length_b                   15.0877(4)
_cell_length_c                   25.2185(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 91.879(2)
_cell_angle_gamma                90.00
_cell_volume                     2701.77(10)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    8089
_cell_measurement_theta_min      2.8128
_cell_measurement_theta_max      32.4828

_exptl_crystal_description       acerose
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_diffrn    1.848
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1528
_exptl_absorpt_coefficient_mu    1.108
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7691
_exptl_absorpt_correction_T_max  0.8973
_exptl_absorpt_process_details   
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      173(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            15724
_diffrn_reflns_av_R_equivalents  0.0307
_diffrn_reflns_av_sigmaI/netI    0.0396
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       3
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_theta_min         2.82
_diffrn_reflns_theta_max         27.50
_reflns_number_total             6195
_reflns_number_gt                5406
_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 F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² 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/[σ²(Fo²)+(0.0590P)²+7.4527P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6195
_refine_ls_number_parameters     424
_refine_ls_number_restraints     56
_refine_ls_R_factor_all          0.0525
_refine_ls_R_factor_gt           0.0436
_refine_ls_wR_factor_ref         0.1155
_refine_ls_wR_factor_gt          0.1093
_refine_ls_goodness_of_fit_ref   1.005
_refine_ls_restrained_S_all      1.005
_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
Mo1 Mo 1.17167(4) 0.39414(2) 0.434488(12) 0.01499(10) Uani 1 1 d . . .
Mo2 Mo 0.40363(4) 0.34912(3) 0.156038(13) 0.02424(11) Uani 1 1 d . . .
C1 C 1.2483(6) 0.4640(3) 0.32168(16) 0.0269(9) Uani 1 1 d . . .
H1A H 1.1516 0.5112 0.3190 0.032 Uiso 1 1 calc R . .
H1B H 1.2940 0.4530 0.2856 0.032 Uiso 1 1 calc R . .
C2 C 1.4103(6) 0.4954(3) 0.35703(16) 0.0277(9) Uani 1 1 d . . .
C3 C 1.2705(6) 0.3025(3) 0.32630(16) 0.0272(9) Uani 1 1 d . . .
H3A H 1.3352 0.3157 0.2930 0.033 Uiso 1 1 calc R . .
H3B H 1.1814 0.2532 0.3189 0.033 Uiso 1 1 calc R . .
C4 C 1.4149(6) 0.2725(3) 0.36762(17) 0.0273(9) Uani 1 1 d . . .
C5 C 0.8137(6) 0.4324(3) 0.15384(17) 0.0270(9) Uani 1 1 d . . .
H5A H 0.9419 0.4150 0.1436 0.032 Uiso 1 1 calc R . .
H5B H 0.8265 0.4823 0.1792 0.032 Uiso 1 1 calc R . .
C6 C 0.7048(7) 0.4638(3) 0.10500(18) 0.0327(10) Uani 1 1 d . . .
C7 C 0.8101(6) 0.2709(3) 0.16416(16) 0.0234(8) Uani 1 1 d . . .
H7A H 0.7986 0.2270 0.1931 0.028 Uiso 1 1 calc R . .
H7B H 0.9459 0.2801 0.1585 0.028 Uiso 1 1 calc R . .
C8 C 0.7188(6) 0.2335(3) 0.11396(16) 0.0242(8) Uani 1 1 d . . .
C9 C 0.9638(5) 0.3753(3) 0.32016(14) 0.0182(7) Uani 1 1 d . . .
H9A H 0.8923 0.4280 0.3314 0.022 Uiso 1 1 calc R . .
H9B H 0.9036 0.3223 0.3354 0.022 Uiso 1 1 calc R . .
C10 C 0.9522(5) 0.3688(3) 0.25965(15) 0.0227(8) Uani 1 1 d . . .
H10A H 1.0187 0.3148 0.2481 0.027 Uiso 1 1 calc R . .
H10B H 1.0149 0.4208 0.2441 0.027 Uiso 1 1 calc R . .
C11 C 0.7467(5) 0.3653(3) 0.23970(14) 0.0182(7) Uani 1 1 d . . .
H11A H 0.6839 0.3145 0.2566 0.022 Uiso 1 1 calc R . .
H11B H 0.6822 0.4201 0.2508 0.022 Uiso 1 1 calc R . .
N1 N 1.1617(4) 0.3821(2) 0.34189(12) 0.0150(6) Uani 1 1 d . . .
N2 N 0.7254(4) 0.3562(2) 0.18097(12) 0.0162(6) Uani 1 1 d . . .
O1 O 1.4089(4) 0.4722(2) 0.40527(10) 0.0234(6) Uani 1 1 d . . .
O2 O 1.5321(5) 0.5423(3) 0.33740(13) 0.0525(11) Uani 1 1 d . . .
O3 O 1.3893(4) 0.2968(2) 0.41521(11) 0.0270(6) Uani 1 1 d . . .
O4 O 1.5424(5) 0.2234(3) 0.35434(14) 0.0508(11) Uani 1 1 d . . .
O5 O 0.5365(4) 0.4358(2) 0.09823(12) 0.0349(7) Uani 1 1 d . . .
O6 O 0.7806(6) 0.5153(3) 0.07443(16) 0.0621(13) Uani 1 1 d . . .
O7 O 0.5528(4) 0.2603(2) 0.10166(11) 0.0268(6) Uani 1 1 d . . .
O8 O 0.8063(5) 0.1786(3) 0.08865(15) 0.0453(10) Uani 1 1 d . . .
O9 O 1.2866(4) 0.40413(19) 0.49695(10) 0.0224(6) Uani 1 1 d . . .
O10 O 1.0299(4) 0.4857(2) 0.42781(11) 0.0251(6) Uani 1 1 d . . .
O11 O 1.0101(4) 0.3076(2) 0.43960(12) 0.0269(6) Uani 1 1 d . . .
O12 O 0.2091(4) 0.3369(3) 0.11213(13) 0.0410(9) Uani 1 1 d . . .
O13 O 0.3676(4) 0.4427(2) 0.19441(13) 0.0358(8) Uani 1 1 d . . .
O14 O 0.3869(4) 0.2620(2) 0.20004(12) 0.0341(7) Uani 1 1 d . . .
N3 N 0.7952(5) 0.6370(2) 0.39969(14) 0.0227(7) Uani 1 1 d D . .
H1 H 0.718(6) 0.607(3) 0.3787(17) 0.034 Uiso 1 1 d D . .
H2 H 0.785(7) 0.6945(14) 0.394(2) 0.034 Uiso 1 1 d D . .
H3 H 0.770(7) 0.629(3) 0.4332(9) 0.034 Uiso 1 1 d D . .
H4 H 0.909(4) 0.620(3) 0.391(2) 0.034 Uiso 1 1 d D . .
N4 N 0.6937(5) 0.4019(2) 0.49231(14) 0.0228(7) Uani 1 1 d D . .
H5 H 0.752(6) 0.373(3) 0.4681(15) 0.034 Uiso 1 1 d D . .
H6 H 0.572(3) 0.395(3) 0.488(2) 0.034 Uiso 1 1 d D . .
H7 H 0.713(7) 0.4592(14) 0.490(2) 0.034 Uiso 1 1 d D . .
H8 H 0.731(7) 0.384(3) 0.5241(11) 0.034 Uiso 1 1 d D . .
N6 N 1.0718(12) 0.6369(4) 0.1035(3) 0.078(2) Uani 1 1 d D . .
H13 H 1.056(10) 0.693(2) 0.094(3) 0.094 Uiso 1 1 d D . .
H15 H 1.166(8) 0.601(5) 0.097(4) 0.117 Uiso 1 1 d D . .
H16 H 0.964(7) 0.613(5) 0.093(4) 0.117 Uiso 1 1 d D . .
H14 H 1.086(13) 0.632(6) 0.1386(9) 0.117 Uiso 1 1 d D . .
H17 H 0.474(12) 0.195(5) 0.5291(19) 0.117 Uiso 1 1 d D . .
H18 H 0.459(13) 0.120(3) 0.489(3) 0.117 Uiso 1 1 d D . .
O1W O 1.0286(12) 0.3453(5) 0.0146(3) 0.110(2) Uani 1 1 d D . .
H1W1 H 0.945(13) 0.302(6) 0.015(4) 0.132 Uiso 1 1 d D . .
H1W2 H 1.069(14) 0.346(7) 0.0498(19) 0.132 Uiso 1 1 d D . .
O2W O 0.3095(10) 0.5422(5) 0.0339(2) 0.102(2) Uani 1 1 d D . .
H2W2 H 0.189(8) 0.505(6) 0.032(4) 0.122 Uiso 1 1 d D . .
H2W1 H 0.383(11) 0.499(5) 0.051(4) 0.122 Uiso 1 1 d D . .
Cl1 Cl 1.0018(4) 0.62121(14) 0.22882(9) 0.0661(6) Uani 0.75 1 d P . .
Cl1' Cl 1.1654(19) 0.6070(8) 0.2077(5) 0.070(3) Uani 0.15 1 d P . .
Cl1" Cl 0.855(2) 0.6037(8) 0.2696(6) 0.054(4) Uani 0.10 1 d P . .
N7 N 0.4414(14) 0.1754(4) 0.4971(2) 0.090(3) Uani 1 1 d D . .
H19 H 0.588(6) 0.184(6) 0.490(4) 0.108 Uiso 1 1 d D . .
H20 H 0.422(11) 0.215(4) 0.473(3) 0.108 Uiso 1 1 d D . .
N5 N 0.489(2) 0.1108(4) 0.2664(3) 0.168(6) Uani 1 1 d D . .
H11 H 0.496(17) 0.150(6) 0.292(3) 0.201 Uiso 1 1 d D . .
H12 H 0.501(17) 0.057(3) 0.279(4) 0.201 Uiso 1 1 d D . .
H9 H 0.585(12) 0.120(8) 0.245(4) 0.201 Uiso 1 1 d D . .
H10 H 0.387(10) 0.118(8) 0.246(4) 0.201 Uiso 1 1 d D . .


_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
Mo1 O10 1.715(3) . ?
Mo1 O11 1.746(3) . ?
Mo1 O9 1.757(3) . ?
Mo1 O3 2.199(3) . ?
Mo1 O1 2.203(3) . ?
Mo1 N1 2.341(3) . ?
Mo2 O14 1.727(3) . ?
Mo2 O13 1.736(3) . ?
Mo2 O12 1.752(3) . ?
Mo2 O5 2.194(3) . ?
Mo2 O7 2.212(3) . ?
Mo2 N2 2.353(3) . ?
C1 N1 1.479(5) . ?
C1 C2 1.509(5) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 O2 1.234(5) . ?
C2 O1 1.266(5) . ?
C3 N1 1.488(5) . ?
C3 C4 1.507(5) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 O4 1.225(5) . ?
C4 O3 1.274(5) . ?
C5 N2 1.486(5) . ?
C5 C6 1.509(6) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 O6 1.231(6) . ?
C6 O5 1.275(5) . ?
C7 N2 1.489(5) . ?
C7 C8 1.512(5) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 O8 1.227(5) . ?
C8 O7 1.275(5) . ?
C9 N1 1.495(4) . ?
C9 C10 1.529(5) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 C11 1.529(5) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 N2 1.490(5) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
N3 H1 0.877(19) . ?
N3 H2 0.880(19) . ?
N3 H3 0.878(19) . ?
N3 H4 0.880(19) . ?
N4 H5 0.864(19) . ?
N4 H6 0.874(19) . ?
N4 H7 0.878(19) . ?
N4 H8 0.878(19) . ?
N6 H13 0.88(2) . ?
N6 H15 0.88(2) . ?
N6 H16 0.88(2) . ?
N6 H14 0.89(2) . ?
O1W H1W1 0.88(4) . ?
O1W H1W2 0.92(4) . ?
O2W H2W2 1.02(4) . ?
O2W H2W1 0.93(4) . ?
Cl1 Cl1' 1.312(12) . ?
Cl1 Cl1" 1.509(16) . ?
N7 H17 0.89(4) . ?
N7 H18 0.87(4) . ?
N7 H19 1.07(4) . ?
N7 H20 0.87(4) . ?
N5 H11 0.873(19) . ?
N5 H12 0.874(19) . ?
N5 H9 0.889(19) . ?
N5 H10 0.883(19) . ?

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 Mo1 O11 102.95(14) . . ?
O10 Mo1 O9 105.85(13) . . ?
O11 Mo1 O9 106.59(13) . . ?
O10 Mo1 O3 158.68(13) . . ?
O11 Mo1 O3 89.18(13) . . ?
O9 Mo1 O3 86.91(12) . . ?
O10 Mo1 O1 89.40(13) . . ?
O11 Mo1 O1 159.50(13) . . ?
O9 Mo1 O1 85.17(11) . . ?
O3 Mo1 O1 74.46(12) . . ?
O10 Mo1 N1 88.07(12) . . ?
O11 Mo1 N1 90.97(12) . . ?
O9 Mo1 N1 154.03(11) . . ?
O3 Mo1 N1 74.09(10) . . ?
O1 Mo1 N1 72.93(10) . . ?
O14 Mo2 O13 104.28(16) . . ?
O14 Mo2 O12 104.86(17) . . ?
O13 Mo2 O12 108.10(16) . . ?
O14 Mo2 O5 157.01(14) . . ?
O13 Mo2 O5 87.71(15) . . ?
O12 Mo2 O5 89.45(15) . . ?
O14 Mo2 O7 88.95(14) . . ?
O13 Mo2 O7 157.03(14) . . ?
O12 Mo2 O7 85.89(13) . . ?
O5 Mo2 O7 73.96(13) . . ?
O14 Mo2 N2 87.12(13) . . ?
O13 Mo2 N2 88.48(13) . . ?
O12 Mo2 N2 155.89(13) . . ?
O5 Mo2 N2 73.45(11) . . ?
O7 Mo2 N2 73.28(10) . . ?
N1 C1 C2 112.1(3) . . ?
N1 C1 H1A 109.2 . . ?
C2 C1 H1A 109.2 . . ?
N1 C1 H1B 109.2 . . ?
C2 C1 H1B 109.2 . . ?
H1A C1 H1B 107.9 . . ?
O2 C2 O1 124.9(4) . . ?
O2 C2 C1 118.3(4) . . ?
O1 C2 C1 116.8(4) . . ?
N1 C3 C4 114.0(3) . . ?
N1 C3 H3A 108.7 . . ?
C4 C3 H3A 108.7 . . ?
N1 C3 H3B 108.7 . . ?
C4 C3 H3B 108.7 . . ?
H3A C3 H3B 107.6 . . ?
O4 C4 O3 124.1(4) . . ?
O4 C4 C3 119.0(4) . . ?
O3 C4 C3 116.7(3) . . ?
N2 C5 C6 114.0(3) . . ?
N2 C5 H5A 108.8 . . ?
C6 C5 H5A 108.8 . . ?
N2 C5 H5B 108.8 . . ?
C6 C5 H5B 108.8 . . ?
H5A C5 H5B 107.7 . . ?
O6 C6 O5 123.6(4) . . ?
O6 C6 C5 119.1(4) . . ?
O5 C6 C5 117.3(4) . . ?
N2 C7 C8 113.2(3) . . ?
N2 C7 H7A 108.9 . . ?
C8 C7 H7A 108.9 . . ?
N2 C7 H7B 108.9 . . ?
C8 C7 H7B 108.9 . . ?
H7A C7 H7B 107.7 . . ?
O8 C8 O7 124.6(4) . . ?
O8 C8 C7 118.5(4) . . ?
O7 C8 C7 116.9(3) . . ?
N1 C9 C10 112.9(3) . . ?
N1 C9 H9A 109.0 . . ?
C10 C9 H9A 109.0 . . ?
N1 C9 H9B 109.0 . . ?
C10 C9 H9B 109.0 . . ?
H9A C9 H9B 107.8 . . ?
C9 C10 C11 110.5(3) . . ?
C9 C10 H10A 109.6 . . ?
C11 C10 H10A 109.6 . . ?
C9 C10 H10B 109.6 . . ?
C11 C10 H10B 109.6 . . ?
H10A C10 H10B 108.1 . . ?
N2 C11 C10 113.3(3) . . ?
N2 C11 H11A 108.9 . . ?
C10 C11 H11A 108.9 . . ?
N2 C11 H11B 108.9 . . ?
C10 C11 H11B 108.9 . . ?
H11A C11 H11B 107.7 . . ?
C1 N1 C3 111.0(3) . . ?
C1 N1 C9 109.1(3) . . ?
C3 N1 C9 109.8(3) . . ?
C1 N1 Mo1 106.2(2) . . ?
C3 N1 Mo1 109.1(2) . . ?
C9 N1 Mo1 111.6(2) . . ?
C5 N2 C7 110.9(3) . . ?
C5 N2 C11 110.9(3) . . ?
C7 N2 C11 109.5(3) . . ?
C5 N2 Mo2 109.5(2) . . ?
C7 N2 Mo2 106.4(2) . . ?
C11 N2 Mo2 109.6(2) . . ?
C2 O1 Mo1 120.0(2) . . ?
C4 O3 Mo1 121.6(2) . . ?
C6 O5 Mo2 122.1(3) . . ?
C8 O7 Mo2 119.9(2) . . ?
H1 N3 H2 112(4) . . ?
H1 N3 H3 112(4) . . ?
H2 N3 H3 105(4) . . ?
H1 N3 H4 106(4) . . ?
H2 N3 H4 109(4) . . ?
H3 N3 H4 114(4) . . ?
H5 N4 H6 110(4) . . ?
H5 N4 H7 111(4) . . ?
H6 N4 H7 105(4) . . ?
H5 N4 H8 111(4) . . ?
H6 N4 H8 111(4) . . ?
H7 N4 H8 109(4) . . ?
H13 N6 H15 129(7) . . ?
H13 N6 H16 103(6) . . ?
H15 N6 H16 110(7) . . ?
H13 N6 H14 111(7) . . ?
H15 N6 H14 95(6) . . ?
H16 N6 H14 109(7) . . ?
H1W1 O1W H1W2 101(7) . . ?
H2W2 O2W H2W1 96(6) . . ?
Cl1' Cl1 Cl1" 152.5(8) . . ?
H17 N7 H18 121(7) . . ?
H17 N7 H19 83(6) . . ?
H18 N7 H19 86(6) . . ?
H17 N7 H20 116(7) . . ?
H18 N7 H20 121(7) . . ?
H19 N7 H20 86(6) . . ?
H11 N5 H12 112(4) . . ?
H11 N5 H9 108(4) . . ?
H12 N5 H9 108(4) . . ?
H11 N5 H10 111(4) . . ?
H12 N5 H10 113(4) . . ?
H9 N5 H10 105(4) . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        27.50
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         1.207
_refine_diff_density_min         -1.043
_refine_diff_density_rms         0.117
_database_code_depnum_ccdc_archive 'CCDC 987096'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_p

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C11 H20 K4 Mo2 N2 O17'
_chemical_formula_weight         800.57

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'
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           ?
_symmetry_space_group_name_H-M   ?

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

_cell_length_a                   6.7798(10)
_cell_length_b                   12.993(2)
_cell_length_c                   14.072(2)
_cell_angle_alpha                104.655(13)
_cell_angle_beta                 90.484(12)
_cell_angle_gamma                94.979(12)
_cell_volume                     1194.2(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       ?
_exptl_crystal_colour            ?
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.04
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.226
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             792
_exptl_absorpt_coefficient_mu    1.831
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  0.7110
_exptl_absorpt_correction_T_max  0.9304
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      173(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            10965
_diffrn_reflns_av_R_equivalents  0.0633
_diffrn_reflns_av_sigmaI/netI    0.1439
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         2.99
_diffrn_reflns_theta_max         25.99
_reflns_number_total             4683
_reflns_number_gt                2871
_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 F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² 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/[σ²(Fo²)+(0.0186P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4683
_refine_ls_number_parameters     320
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0790
_refine_ls_R_factor_gt           0.0397
_refine_ls_wR_factor_ref         0.0703
_refine_ls_wR_factor_gt          0.0655
_refine_ls_goodness_of_fit_ref   0.771
_refine_ls_restrained_S_all      0.771
_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
Mo1 Mo -0.16143(7) 1.11668(4) 1.15423(4) 0.00894(13) Uani 1 1 d . . .
Mo2 Mo 0.66171(7) 1.70718(4) 1.29999(4) 0.01115(14) Uani 1 1 d . . .
K1 K 0.16489(17) 1.20320(10) 0.90928(10) 0.0141(3) Uani 1 1 d . . .
K2 K -0.31111(18) 0.98467(10) 0.90363(10) 0.0173(3) Uani 1 1 d . . .
K3 K 0.84441(18) 1.79803(11) 1.55014(10) 0.0212(3) Uani 1 1 d . . .
K4 K -0.3859(2) 0.99707(11) 1.35291(11) 0.0284(4) Uani 1 1 d . . .
C1 C -0.2440(7) 1.3363(4) 1.2970(4) 0.0120(13) Uani 1 1 d . . .
H1A H -0.2999 1.4050 1.3002 0.014 Uiso 1 1 calc R . .
H1B H -0.1475 1.3481 1.3528 0.014 Uiso 1 1 calc R . .
C2 C -0.4081(8) 1.2555(5) 1.3083(4) 0.0168(15) Uani 1 1 d . . .
C3 C -0.2400(8) 1.3402(4) 1.1262(4) 0.0133(14) Uani 1 1 d . . .
H3A H -0.1423 1.3499 1.0765 0.016 Uiso 1 1 calc R . .
H3B H -0.2891 1.4105 1.1554 0.016 Uiso 1 1 calc R . .
C4 C -0.4113(8) 1.2638(5) 1.0754(4) 0.0141(14) Uani 1 1 d . . .
C5 C 0.2402(4) 1.6751(3) 1.3806(2) 0.0096(13) Uani 1 1 d . . .
H5A H 0.2574 1.6226 1.4195 0.012 Uiso 1 1 calc R . .
H5B H 0.0961 1.6778 1.3707 0.012 Uiso 1 1 calc R . .
C6 C 0.3281(4) 1.7841(3) 1.4393(2) 0.0105(13) Uani 1 1 d RU . .
C7 C 0.2334(4) 1.6751(3) 1.2056(2) 0.0104(13) Uani 1 1 d R . .
H7A H 0.0915 1.6809 1.2200 0.013 Uiso 1 1 calc R . .
H7B H 0.2411 1.6216 1.1419 0.013 Uiso 1 1 calc R . .
C8 C 0.3248(8) 1.7815(5) 1.1957(4) 0.0123(13) Uani 1 1 d . . .
C9 C 0.0717(7) 1.3493(4) 1.2173(4) 0.0073(12) Uani 1 1 d . . .
H9A H 0.1403 1.3237 1.1550 0.009 Uiso 1 1 calc R . .
H9B H 0.1368 1.3227 1.2685 0.009 Uiso 1 1 calc R . .
C10 C 0.0940(7) 1.4709(4) 1.2466(4) 0.0108(13) Uani 1 1 d . . .
H10A H 0.0255 1.4974 1.1964 0.013 Uiso 1 1 calc R . .
H10B H 0.0290 1.4965 1.3098 0.013 Uiso 1 1 calc R . .
C11 C 0.3096(7) 1.5168(4) 1.2569(4) 0.0096(13) Uani 1 1 d . . .
H11A H 0.3774 1.4922 1.3086 0.012 Uiso 1 1 calc R . .
H11B H 0.3759 1.4897 1.1943 0.012 Uiso 1 1 calc R . .
N1 N -0.1390(6) 1.3044(3) 1.2043(3) 0.0068(10) Uani 1 1 d . . .
N2 N 0.3285(6) 1.6368(3) 1.2829(3) 0.0107(11) Uani 1 1 d . . .
O1 O -0.5405(6) 1.2842(3) 1.3672(3) 0.0267(11) Uani 1 1 d . . .
O2 O -0.3951(5) 1.1592(3) 1.2598(3) 0.0162(10) Uani 1 1 d . . .
O3 O -0.5415(6) 1.2985(3) 1.0349(3) 0.0300(13) Uani 1 1 d . . .
O4 O -0.4007(5) 1.1663(3) 1.0734(3) 0.0147(10) Uani 1 1 d . . .
O5 O 0.2294(5) 1.8358(3) 1.5051(3) 0.0198(11) Uani 1 1 d . . .
O6 O 0.5037(5) 1.8129(3) 1.4205(3) 0.0132(9) Uani 1 1 d . . .
O7 O 0.2246(6) 1.8343(3) 1.1553(3) 0.0234(11) Uani 1 1 d . . .
O8 O 0.5030(5) 1.8077(3) 1.2273(3) 0.0130(9) Uani 1 1 d . . .
O9 O -0.0002(5) 1.1116(3) 1.2491(3) 0.0203(10) Uani 1 1 d . . .
O10 O -0.2893(5) 0.9905(3) 1.1173(3) 0.0162(10) Uani 1 1 d . . .
O11 O -0.0065(5) 1.1257(3) 1.0584(3) 0.0155(10) Uani 1 1 d . . .
O12 O 0.8518(5) 1.8098(3) 1.3250(3) 0.0227(11) Uani 1 1 d . . .
O13 O 0.7062(5) 1.6259(3) 1.1860(3) 0.0201(10) Uani 1 1 d . . .
O14 O 0.7015(5) 1.6279(3) 1.3793(3) 0.0189(10) Uani 1 1 d . . .
O1W O -0.8256(7) 0.9885(4) 1.3668(4) 0.0381(13) Uani 1 1 d . . .
O2W O 0.1600(12) 1.4376(4) 0.9993(4) 0.095(3) Uani 1 1 d . . .
O3W O 0.8410(13) 1.5642(4) 1.5311(4) 0.102(3) Uani 1 1 d . . .


_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
Mo1 O9 1.736(4) . ?
Mo1 O11 1.737(4) . ?
Mo1 O10 1.739(4) . ?
Mo1 O2 2.191(4) . ?
Mo1 O4 2.205(3) . ?
Mo1 N1 2.352(4) . ?
Mo1 K2 3.5910(14) 2_577 ?
Mo1 K2 3.6034(15) . ?
Mo1 K2 3.7116(14) 2_477 ?
Mo1 K4 3.7959(19) . ?
Mo1 K1 4.0221(15) 2_577 ?
Mo2 O13 1.728(4) . ?
Mo2 O14 1.733(4) . ?
Mo2 O12 1.738(4) . ?
Mo2 O8 2.194(4) . ?
Mo2 O6 2.241(4) . ?
Mo2 N2 2.349(5) . ?
Mo2 K3 3.5902(16) . ?
Mo2 K1 3.6009(16) 2_687 ?
Mo2 K4 3.6935(16) 1_665 ?
K1 O3 2.650(4) 1_655 ?
K1 O10 2.662(4) 2_577 ?
K1 O7 2.747(4) 2_587 ?
K1 O11 2.770(4) . ?
K1 O13 2.947(5) 2_687 ?
K1 O8 2.962(4) 2_687 ?
K1 O2W 2.991(5) . ?
K1 O12 3.259(5) 2_687 ?
K1 Mo2 3.6009(16) 2_687 ?
K1 Mo1 4.0221(15) 2_577 ?
K1 K2 4.0956(19) . ?
K1 K2 4.1834(19) 2_577 ?
K2 O7 2.706(4) 2_587 ?
K2 O4 2.728(4) 2_477 ?
K2 O10 2.778(4) 2_477 ?
K2 O11 2.807(4) 2_577 ?
K2 O10 2.991(4) . ?
K2 O4 3.011(4) . ?
K2 O11 3.101(4) . ?
K2 O9 3.133(4) 2_577 ?
K2 O2 3.139(4) 2_477 ?
K2 Mo1 3.5910(14) 2_577 ?
K2 Mo1 3.7116(14) 2_477 ?
K3 O1 2.651(5) 2_588 ?
K3 O5 2.723(4) 1_655 ?
K3 O1W 2.739(5) 2_588 ?
K3 O14 2.916(4) . ?
K3 O9 2.921(4) 2_688 ?
K3 O3W 2.979(6) . ?
K3 O6 2.981(4) . ?
K3 O12 3.211(5) . ?
K3 K4 4.276(2) 2_588 ?
K3 K4 4.337(2) 2_688 ?
K3 K4 4.592(2) 1_665 ?
K4 O8 2.684(4) 1_445 ?
K4 O5 2.684(4) 2_588 ?
K4 O2 2.752(4) . ?
K4 O6 2.836(4) 1_445 ?
K4 O12 2.980(4) 1_445 ?
K4 O1W 2.983(5) . ?
K4 O10 3.366(4) . ?
K4 O9 3.417(5) . ?
K4 C6 3.517(3) 2_588 ?
K4 C8 3.524(6) 1_445 ?
K4 Mo2 3.6935(16) 1_445 ?
C1 N1 1.475(7) . ?
C1 C2 1.500(8) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 O1 1.243(7) . ?
C2 O2 1.276(7) . ?
C3 N1 1.481(6) . ?
C3 C4 1.507(8) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 O3 1.224(6) . ?
C4 O4 1.267(6) . ?
C5 N2 1.488(6) . ?
C5 C6 1.5148 . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 O5 1.238(5) . ?
C6 O6 1.267(5) . ?
C6 K4 3.517(3) 2_588 ?
C7 N2 1.473(5) . ?
C7 C8 1.505(7) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 O7 1.236(6) . ?
C8 O8 1.271(6) . ?
C8 K4 3.524(6) 1_665 ?
C9 N1 1.488(6) . ?
C9 C10 1.521(7) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 C11 1.521(7) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 N2 1.503(6) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
O1 K3 2.651(5) 2_588 ?
O2 K2 3.139(4) 2_477 ?
O3 K1 2.650(4) 1_455 ?
O4 K2 2.728(4) 2_477 ?
O5 K4 2.684(4) 2_588 ?
O5 K3 2.723(4) 1_455 ?
O6 K4 2.836(4) 1_665 ?
O7 K2 2.706(4) 2_587 ?
O7 K1 2.747(4) 2_587 ?
O8 K4 2.684(4) 1_665 ?
O8 K1 2.962(4) 2_687 ?
O9 K3 2.921(4) 2_688 ?
O9 K2 3.133(4) 2_577 ?
O10 K1 2.662(4) 2_577 ?
O10 K2 2.778(4) 2_477 ?
O11 K2 2.807(4) 2_577 ?
O12 K4 2.980(4) 1_665 ?
O12 K1 3.259(5) 2_687 ?
O13 K1 2.947(5) 2_687 ?
O1W K3 2.739(5) 2_588 ?

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 Mo1 O11 103.94(18) . . ?
O9 Mo1 O10 105.82(19) . . ?
O11 Mo1 O10 105.25(18) . . ?
O9 Mo1 O2 90.02(17) . . ?
O11 Mo1 O2 157.83(16) . . ?
O10 Mo1 O2 86.90(17) . . ?
O9 Mo1 O4 160.67(16) . . ?
O11 Mo1 O4 88.37(16) . . ?
O10 Mo1 O4 84.69(16) . . ?
O2 Mo1 O4 74.12(14) . . ?
O9 Mo1 N1 91.46(17) . . ?
O11 Mo1 N1 88.89(17) . . ?
O10 Mo1 N1 153.87(15) . . ?
O2 Mo1 N1 73.39(15) . . ?
O4 Mo1 N1 73.67(14) . . ?
O9 Mo1 K2 60.75(13) . 2_577 ?
O11 Mo1 K2 49.93(12) . 2_577 ?
O10 Mo1 K2 93.15(12) . 2_577 ?
O2 Mo1 K2 149.65(10) . 2_577 ?
O4 Mo1 K2 136.14(11) . 2_577 ?
N1 Mo1 K2 112.56(10) . 2_577 ?
O9 Mo1 K2 142.82(13) . . ?
O11 Mo1 K2 59.33(12) . . ?
O10 Mo1 K2 55.71(14) . . ?
O2 Mo1 K2 117.67(10) . . ?
O4 Mo1 K2 56.45(10) . . ?
N1 Mo1 K2 118.86(11) . . ?
K2 Mo1 K2 86.46(3) 2_577 . ?
O9 Mo1 K2 132.16(15) . 2_477 ?
O11 Mo1 K2 118.90(12) . 2_477 ?
O10 Mo1 K2 45.27(11) . 2_477 ?
O2 Mo1 K2 57.57(10) . 2_477 ?
O4 Mo1 K2 46.83(11) . 2_477 ?
N1 Mo1 K2 108.67(10) . 2_477 ?
K2 Mo1 K2 136.37(4) 2_577 2_477 ?
K2 Mo1 K2 61.07(4) . 2_477 ?
O9 Mo1 K4 64.14(15) . . ?
O11 Mo1 K4 156.53(12) . . ?
O10 Mo1 K4 62.46(14) . . ?
O2 Mo1 K4 45.61(11) . . ?
O4 Mo1 K4 109.03(11) . . ?
N1 Mo1 K4 110.68(12) . . ?
K2 Mo1 K4 108.49(3) 2_577 . ?
K2 Mo1 K4 116.99(4) . . ?
K2 Mo1 K4 68.16(3) 2_477 . ?
O9 Mo1 K1 83.05(13) . 2_577 ?
O11 Mo1 K1 92.55(13) . 2_577 ?
O10 Mo1 K1 29.98(11) . 2_577 ?
O2 Mo1 K1 106.35(11) . 2_577 ?
O4 Mo1 K1 111.65(10) . 2_577 ?
N1 Mo1 K1 174.51(10) . 2_577 ?
K2 Mo1 K1 64.80(3) 2_577 2_577 ?
K2 Mo1 K1 66.28(3) . 2_577 ?
K2 Mo1 K1 75.21(3) 2_477 2_577 ?
K4 Mo1 K1 66.77(3) . 2_577 ?
O13 Mo2 O14 103.28(19) . . ?
O13 Mo2 O12 106.4(2) . . ?
O14 Mo2 O12 106.33(19) . . ?
O13 Mo2 O8 89.26(16) . . ?
O14 Mo2 O8 158.07(17) . . ?
O12 Mo2 O8 86.76(16) . . ?
O13 Mo2 O6 159.98(15) . . ?
O14 Mo2 O6 88.20(16) . . ?
O12 Mo2 O6 85.44(17) . . ?
O8 Mo2 O6 75.12(14) . . ?
O13 Mo2 N2 89.70(17) . . ?
O14 Mo2 N2 88.56(18) . . ?
O12 Mo2 N2 154.36(16) . . ?
O8 Mo2 N2 73.38(15) . . ?
O6 Mo2 N2 74.05(15) . . ?
O13 Mo2 K3 143.85(12) . . ?
O14 Mo2 K3 53.58(13) . . ?
O12 Mo2 K3 63.33(15) . . ?
O8 Mo2 K3 122.56(10) . . ?
O6 Mo2 K3 55.88(9) . . ?
N2 Mo2 K3 114.05(12) . . ?
O13 Mo2 K1 54.26(15) . 2_687 ?
O14 Mo2 K1 146.30(13) . 2_687 ?
O12 Mo2 K1 64.61(15) . 2_687 ?
O8 Mo2 K1 55.25(10) . 2_687 ?
O6 Mo2 K1 121.43(11) . 2_687 ?
N2 Mo2 K1 113.38(12) . 2_687 ?
K3 Mo2 K1 127.91(4) . 2_687 ?
O13 Mo2 K4 125.19(15) . 1_665 ?
O14 Mo2 K4 130.07(13) . 1_665 ?
O12 Mo2 K4 52.68(12) . 1_665 ?
O8 Mo2 K4 46.03(10) . 1_665 ?
O6 Mo2 K4 50.09(11) . 1_665 ?
N2 Mo2 K4 101.75(11) . 1_665 ?
K3 Mo2 K4 78.16(4) . 1_665 ?
K1 Mo2 K4 72.35(4) 2_687 1_665 ?
O3 K1 O10 94.23(12) 1_655 2_577 ?
O3 K1 O7 153.92(14) 1_655 2_587 ?
O10 K1 O7 104.49(12) 2_577 2_587 ?
O3 K1 O11 88.27(14) 1_655 . ?
O10 K1 O11 75.79(12) 2_577 . ?
O7 K1 O11 79.13(12) 2_587 . ?
O3 K1 O13 82.05(13) 1_655 2_687 ?
O10 K1 O13 129.15(12) 2_577 2_687 ?
O7 K1 O13 99.26(12) 2_587 2_687 ?
O11 K1 O13 153.64(11) . 2_687 ?
O3 K1 O8 80.03(13) 1_655 2_687 ?
O10 K1 O8 73.33(12) 2_577 2_687 ?
O7 K1 O8 122.42(12) 2_587 2_687 ?
O11 K1 O8 145.92(11) . 2_687 ?
O13 K1 O8 56.01(10) 2_687 2_687 ?
O3 K1 O2W 62.63(15) 1_655 . ?
O10 K1 O2W 156.69(15) 2_577 . ?
O7 K1 O2W 96.76(17) 2_587 . ?
O11 K1 O2W 99.35(15) . . ?
O13 K1 O2W 54.48(14) 2_687 . ?
O8 K1 O2W 103.27(17) 2_687 . ?
O3 K1 O12 125.81(13) 1_655 2_687 ?
O10 K1 O12 93.56(11) 2_577 2_687 ?
O7 K1 O12 71.67(12) 2_587 2_687 ?
O11 K1 O12 145.32(11) . 2_687 ?
O13 K1 O12 52.85(10) 2_687 2_687 ?
O8 K1 O12 51.60(9) 2_687 2_687 ?
O2W K1 O12 102.23(13) . 2_687 ?
O3 K1 Mo2 97.91(11) 1_655 2_687 ?
O10 K1 Mo2 104.53(10) 2_577 2_687 ?
O7 K1 Mo2 94.81(10) 2_587 2_687 ?
O11 K1 Mo2 173.75(8) . 2_687 ?
O13 K1 Mo2 28.42(7) 2_687 2_687 ?
O8 K1 Mo2 37.48(7) 2_687 2_687 ?
O2W K1 Mo2 82.80(13) . 2_687 ?
O12 K1 Mo2 28.80(7) 2_687 2_687 ?
O3 K1 Mo1 111.46(9) 1_655 2_577 ?
O10 K1 Mo1 19.05(8) 2_577 2_577 ?
O7 K1 Mo1 85.54(9) 2_587 2_577 ?
O11 K1 Mo1 69.59(8) . 2_577 ?
O13 K1 Mo1 136.75(8) 2_687 2_577 ?
O8 K1 Mo1 85.05(8) 2_687 2_577 ?
O2W K1 Mo1 168.14(12) . 2_577 ?
O12 K1 Mo1 89.54(7) 2_687 2_577 ?
Mo2 K1 Mo1 108.66(4) 2_687 2_577 ?
O3 K1 K2 136.71(12) 1_655 . ?
O10 K1 K2 70.56(9) 2_577 . ?
O7 K1 K2 40.94(9) 2_587 . ?
O11 K1 K2 49.18(8) . . ?
O13 K1 K2 139.20(8) 2_687 . ?
O8 K1 K2 128.98(8) 2_687 . ?
O2W K1 K2 123.66(16) . . ?
O12 K1 K2 96.14(8) 2_687 . ?
Mo2 K1 K2 124.82(4) 2_687 . ?
Mo1 K1 K2 52.50(3) 2_577 . ?
O3 K1 K2 68.16(10) 1_655 2_577 ?
O10 K1 K2 45.40(9) 2_577 2_577 ?
O7 K1 K2 113.10(10) 2_587 2_577 ?
O11 K1 K2 41.75(7) . 2_577 ?
O13 K1 K2 147.58(8) 2_687 2_577 ?
O8 K1 K2 104.58(8) 2_687 2_577 ?
O2W K1 K2 116.87(10) . 2_577 ?
O12 K1 K2 138.96(7) 2_687 2_577 ?
Mo2 K1 K2 142.04(4) 2_687 2_577 ?
Mo1 K1 K2 52.05(3) 2_577 2_577 ?
K2 K1 K2 73.04(4) . 2_577 ?
O7 K2 O4 146.46(12) 2_587 2_477 ?
O7 K2 O10 88.66(12) 2_587 2_477 ?
O4 K2 O10 58.23(11) 2_477 2_477 ?
O7 K2 O11 117.66(12) 2_587 2_577 ?
O4 K2 O11 95.33(12) 2_477 2_577 ?
O10 K2 O11 153.56(13) 2_477 2_577 ?
O7 K2 O10 120.03(12) 2_587 . ?
O4 K2 O10 75.01(11) 2_477 . ?
O10 K2 O10 99.84(10) 2_477 . ?
O11 K2 O10 70.20(11) 2_577 . ?
O7 K2 O4 73.77(13) 2_587 . ?
O4 K2 O4 99.40(11) 2_477 . ?
O10 K2 O4 73.99(10) 2_477 . ?
O11 K2 O4 113.91(10) 2_577 . ?
O10 K2 O4 53.02(10) . . ?
O7 K2 O11 74.14(12) 2_587 . ?
O4 K2 O11 128.83(12) 2_477 . ?
O10 K2 O11 127.64(11) 2_477 . ?
O11 K2 O11 67.08(12) 2_577 . ?
O10 K2 O11 53.89(11) . . ?
O4 K2 O11 53.84(10) . . ?
O7 K2 O9 84.91(12) 2_587 2_577 ?
O4 K2 O9 112.17(12) 2_477 2_577 ?
O10 K2 O9 131.81(11) 2_477 2_577 ?
O11 K2 O9 54.51(11) 2_577 2_577 ?
O10 K2 O9 124.47(10) . 2_577 ?
O4 K2 O9 146.67(12) . 2_577 ?
O11 K2 O9 96.15(10) . 2_577 ?
O7 K2 O2 104.88(12) 2_587 2_477 ?
O4 K2 O2 53.13(11) 2_477 2_477 ?
O10 K2 O2 54.37(10) 2_477 2_477 ?
O11 K2 O2 111.76(11) 2_577 2_477 ?
O10 K2 O2 128.13(12) . 2_477 ?
O4 K2 O2 128.28(10) . 2_477 ?
O11 K2 O2 177.49(11) . 2_477 ?
O9 K2 O2 81.43(10) 2_577 2_477 ?
O7 K2 Mo1 95.29(9) 2_587 2_577 ?
O4 K2 Mo1 113.70(8) 2_477 2_577 ?
O10 K2 Mo1 158.88(9) 2_477 2_577 ?
O11 K2 Mo1 28.27(9) 2_577 2_577 ?
O10 K2 Mo1 96.11(7) . 2_577 ?
O4 K2 Mo1 127.02(8) . 2_577 ?
O11 K2 Mo1 73.21(7) . 2_577 ?
O9 K2 Mo1 28.91(7) 2_577 2_577 ?
O2 K2 Mo1 104.69(8) 2_477 2_577 ?
O7 K2 Mo1 91.99(10) 2_587 . ?
O4 K2 Mo1 102.20(9) 2_477 . ?
O10 K2 Mo1 107.08(9) 2_477 . ?
O11 K2 Mo1 76.31(8) 2_577 . ?
O10 K2 Mo1 28.70(7) . . ?
O4 K2 Mo1 37.62(7) . . ?
O11 K2 Mo1 28.81(8) . . ?
O9 K2 Mo1 120.82(7) 2_577 . ?
O2 K2 Mo1 153.62(9) 2_477 . ?
Mo1 K2 Mo1 93.54(3) 2_577 . ?
O7 K2 Mo1 110.62(9) 2_587 2_477 ?
O4 K2 Mo1 36.14(7) 2_477 2_477 ?
O10 K2 Mo1 26.40(8) 2_477 2_477 ?
O11 K2 Mo1 128.81(9) 2_577 2_477 ?
O10 K2 Mo1 99.99(8) . 2_477 ?
O4 K2 Mo1 94.46(8) . 2_477 ?
O11 K2 Mo1 146.39(8) . 2_477 ?
O9 K2 Mo1 117.23(8) 2_577 2_477 ?
O2 K2 Mo1 36.09(7) 2_477 2_477 ?
Mo1 K2 Mo1 136.37(4) 2_577 2_477 ?
Mo1 K2 Mo1 118.93(4) . 2_477 ?
O1 K3 O5 157.32(15) 2_588 1_655 ?
O1 K3 O1W 100.61(14) 2_588 2_588 ?
O5 K3 O1W 90.49(14) 1_655 2_588 ?
O1 K3 O14 82.22(13) 2_588 . ?
O5 K3 O14 101.30(12) 1_655 . ?
O1W K3 O14 141.62(13) 2_588 . ?
O1 K3 O9 85.42(13) 2_588 2_688 ?
O5 K3 O9 82.68(12) 1_655 2_688 ?
O1W K3 O9 61.27(13) 2_588 2_688 ?
O14 K3 O9 155.81(13) . 2_688 ?
O1 K3 O3W 65.66(19) 2_588 . ?
O5 K3 O3W 98.07(19) 1_655 . ?
O1W K3 O3W 160.22(17) 2_588 . ?
O14 K3 O3W 53.89(13) . . ?
O9 K3 O3W 102.02(13) 2_688 . ?
O1 K3 O6 77.63(13) 2_588 . ?
O5 K3 O6 123.14(13) 1_655 . ?
O1W K3 O6 86.48(12) 2_588 . ?
O14 K3 O6 56.45(10) . . ?
O9 K3 O6 140.04(11) 2_688 . ?
O3W K3 O6 103.34(16) . . ?
O1 K3 O12 124.96(13) 2_588 . ?
O5 K3 O12 72.25(11) 1_655 . ?
O1W K3 O12 97.32(13) 2_588 . ?
O14 K3 O12 53.67(11) . . ?
O9 K3 O12 147.14(13) 2_688 . ?
O3W K3 O12 102.25(13) . . ?
O6 K3 O12 52.05(10) . . ?
O1 K3 Mo2 97.61(10) 2_588 . ?
O5 K3 Mo2 95.53(9) 1_655 . ?
O1W K3 Mo2 114.76(11) 2_588 . ?
O14 K3 Mo2 28.57(8) . . ?
O9 K3 Mo2 175.53(10) 2_688 . ?
O3W K3 Mo2 82.27(11) . . ?
O6 K3 Mo2 38.48(7) . . ?
O12 K3 Mo2 28.93(7) . . ?
O1 K3 K4 63.97(10) 2_588 2_588 ?
O5 K3 K4 132.94(10) 1_655 2_588 ?
O1W K3 K4 43.87(10) 2_588 2_588 ?
O14 K3 K4 109.65(8) . 2_588 ?
O9 K3 K4 83.01(8) 2_688 2_588 ?
O3W K3 K4 128.74(18) . 2_588 ?
O6 K3 K4 57.04(8) . 2_588 ?
O12 K3 K4 98.56(7) . 2_588 ?
Mo2 K3 K4 95.33(4) . 2_588 ?
O1 K3 K4 137.19(11) 2_588 2_688 ?
O5 K3 K4 36.37(8) 1_655 2_688 ?
O1W K3 K4 60.34(10) 2_588 2_688 ?
O14 K3 K4 137.51(9) . 2_688 ?
O9 K3 K4 51.81(9) 2_688 2_688 ?
O3W K3 K4 119.32(16) . 2_688 ?
O6 K3 K4 132.52(9) . 2_688 ?
O12 K3 K4 96.64(8) . 2_688 ?
Mo2 K3 K4 124.99(5) . 2_688 ?
K4 K3 K4 103.85(4) 2_588 2_688 ?
O1 K3 K4 109.19(10) 2_588 1_665 ?
O5 K3 K4 93.46(10) 1_655 1_665 ?
O1W K3 K4 62.90(11) 2_588 1_665 ?
O14 K3 K4 79.88(8) . 1_665 ?
O9 K3 K4 123.97(9) 2_688 1_665 ?
O3W K3 K4 133.66(11) . 1_665 ?
O6 K3 K4 36.77(8) . 1_665 ?
O12 K3 K4 40.22(7) . 1_665 ?
Mo2 K3 K4 51.92(3) . 1_665 ?
K4 K3 K4 59.61(4) 2_588 1_665 ?
K4 K3 K4 95.81(4) 2_688 1_665 ?
O8 K4 O5 168.71(13) 1_445 2_588 ?
O8 K4 O2 110.44(12) 1_445 . ?
O5 K4 O2 79.25(13) 2_588 . ?
O8 K4 O6 58.57(12) 1_445 1_445 ?
O5 K4 O6 113.52(13) 2_588 1_445 ?
O2 K4 O6 162.01(12) . 1_445 ?
O8 K4 O12 57.13(11) 1_445 1_445 ?
O5 K4 O12 112.15(12) 2_588 1_445 ?
O2 K4 O12 133.05(13) . 1_445 ?
O6 K4 O12 55.80(11) 1_445 1_445 ?
O8 K4 O1W 78.76(12) 1_445 . ?
O5 K4 O1W 107.79(13) 2_588 . ?
O2 K4 O1W 89.56(13) . . ?
O6 K4 O1W 74.73(12) 1_445 . ?
O12 K4 O1W 125.22(13) 1_445 . ?
O8 K4 O10 66.53(11) 1_445 . ?
O5 K4 O10 118.75(13) 2_588 . ?
O2 K4 O10 51.66(10) . . ?
O6 K4 O10 123.89(11) 1_445 . ?
O12 K4 O10 85.93(11) 1_445 . ?
O1W K4 O10 106.07(12) . . ?
O8 K4 O9 106.53(12) 1_445 . ?
O5 K4 O9 74.32(12) 2_588 . ?
O2 K4 O9 52.56(10) . . ?
O6 K4 O9 141.10(10) 1_445 . ?
O12 K4 O9 85.56(11) 1_445 . ?
O1W K4 O9 141.63(12) . . ?
O10 K4 O9 48.24(9) . . ?
O8 K4 C6 164.05(12) 1_445 2_588 ?
O5 K4 C6 17.13(10) 2_588 2_588 ?
O2 K4 C6 81.27(10) . 2_588 ?
O6 K4 C6 107.18(10) 1_445 2_588 ?
O12 K4 C6 122.98(10) 1_445 2_588 ?
O1W K4 C6 90.87(11) . 2_588 ?
O10 K4 C6 128.66(10) . 2_588 ?
O9 K4 C6 89.14(9) . 2_588 ?
O8 K4 C8 17.82(11) 1_445 1_445 ?
O5 K4 C8 168.58(14) 2_588 1_445 ?
O2 K4 C8 103.77(13) . 1_445 ?
O6 K4 C8 61.23(13) 1_445 1_445 ?
O12 K4 C8 74.07(12) 1_445 1_445 ?
O1W K4 C8 61.56(13) . 1_445 ?
O10 K4 C8 70.33(12) . 1_445 ?
O9 K4 C8 116.39(12) . 1_445 ?
C6 K4 C8 151.59(12) 2_588 1_445 ?
O8 K4 Mo2 36.03(8) 1_445 1_445 ?
O5 K4 Mo2 132.72(10) 2_588 1_445 ?
O2 K4 Mo2 141.06(9) . 1_445 ?
O6 K4 Mo2 37.30(8) 1_445 1_445 ?
O12 K4 Mo2 27.64(8) 1_445 1_445 ?
O1W K4 Mo2 97.89(10) . 1_445 ?
O10 K4 Mo2 89.75(7) . 1_445 ?
O9 K4 Mo2 108.25(7) . 1_445 ?
C6 K4 Mo2 136.33(7) 2_588 1_445 ?
C8 K4 Mo2 50.05(10) 1_445 1_445 ?
O8 K4 Mo1 93.61(10) 1_445 . ?
O5 K4 Mo1 91.55(11) 2_588 . ?
O2 K4 Mo1 34.67(8) . . ?
O6 K4 Mo1 148.69(9) 1_445 . ?
O12 K4 Mo1 98.39(10) 1_445 . ?
O1W K4 Mo1 116.59(10) . . ?
O10 K4 Mo1 27.26(7) . . ?
O9 K4 Mo1 27.21(6) . . ?
C6 K4 Mo1 101.92(7) 2_588 . ?
C8 K4 Mo1 97.07(11) 1_445 . ?
Mo2 K4 Mo1 111.68(4) 1_445 . ?
N1 C1 C2 113.5(5) . . ?
N1 C1 H1A 108.9 . . ?
C2 C1 H1A 108.9 . . ?
N1 C1 H1B 108.9 . . ?
C2 C1 H1B 108.9 . . ?
H1A C1 H1B 107.7 . . ?
O1 C2 O2 124.2(6) . . ?
O1 C2 C1 119.1(5) . . ?
O2 C2 C1 116.6(5) . . ?
N1 C3 C4 113.8(5) . . ?
N1 C3 H3A 108.8 . . ?
C4 C3 H3A 108.8 . . ?
N1 C3 H3B 108.8 . . ?
C4 C3 H3B 108.8 . . ?
H3A C3 H3B 107.7 . . ?
O3 C4 O4 125.4(5) . . ?
O3 C4 C3 118.5(5) . . ?
O4 C4 C3 115.9(5) . . ?
N2 C5 C6 114.4(2) . . ?
N2 C5 H5A 108.7 . . ?
C6 C5 H5A 108.7 . . ?
N2 C5 H5B 108.7 . . ?
C6 C5 H5B 108.7 . . ?
H5A C5 H5B 107.6 . . ?
O5 C6 O6 124.6(4) . . ?
O5 C6 C5 118.4(2) . . ?
O6 C6 C5 116.8(2) . . ?
O5 C6 K4 39.7(2) . 2_588 ?
O6 C6 K4 85.6(2) . 2_588 ?
C5 C6 K4 154.76(6) . 2_588 ?
N2 C7 C8 113.8(3) . . ?
N2 C7 H7A 108.8 . . ?
C8 C7 H7A 108.8 . . ?
N2 C7 H7B 108.8 . . ?
C8 C7 H7B 108.8 . . ?
H7A C7 H7B 107.7 . . ?
O7 C8 O8 125.5(6) . . ?
O7 C8 C7 118.0(5) . . ?
O8 C8 C7 116.4(5) . . ?
O7 C8 K4 97.7(4) . 1_665 ?
O8 C8 K4 40.3(3) . 1_665 ?
C7 C8 K4 134.4(3) . 1_665 ?
N1 C9 C10 112.6(4) . . ?
N1 C9 H9A 109.1 . . ?
C10 C9 H9A 109.1 . . ?
N1 C9 H9B 109.1 . . ?
C10 C9 H9B 109.1 . . ?
H9A C9 H9B 107.8 . . ?
C11 C10 C9 112.6(4) . . ?
C11 C10 H10A 109.1 . . ?
C9 C10 H10A 109.1 . . ?
C11 C10 H10B 109.1 . . ?
C9 C10 H10B 109.1 . . ?
H10A C10 H10B 107.8 . . ?
N2 C11 C10 111.8(4) . . ?
N2 C11 H11A 109.3 . . ?
C10 C11 H11A 109.3 . . ?
N2 C11 H11B 109.3 . . ?
C10 C11 H11B 109.3 . . ?
H11A C11 H11B 107.9 . . ?
C1 N1 C3 109.7(4) . . ?
C1 N1 C9 110.7(4) . . ?
C3 N1 C9 110.6(4) . . ?
C1 N1 Mo1 108.4(3) . . ?
C3 N1 Mo1 106.6(3) . . ?
C9 N1 Mo1 110.7(3) . . ?
C7 N2 C5 112.6(3) . . ?
C7 N2 C11 110.2(4) . . ?
C5 N2 C11 108.0(4) . . ?
C7 N2 Mo2 107.9(3) . . ?
C5 N2 Mo2 106.5(3) . . ?
C11 N2 Mo2 111.7(3) . . ?
C2 O1 K3 140.3(4) . 2_588 ?
C2 O2 Mo1 121.6(4) . . ?
C2 O2 K4 121.2(4) . . ?
Mo1 O2 K4 99.73(13) . . ?
C2 O2 K2 128.1(3) . 2_477 ?
Mo1 O2 K2 86.34(12) . 2_477 ?
K4 O2 K2 90.91(11) . 2_477 ?
C4 O3 K1 132.4(4) . 1_455 ?
C4 O4 Mo1 121.1(4) . . ?
C4 O4 K2 130.0(4) . 2_477 ?
Mo1 O4 K2 97.03(15) . 2_477 ?
C4 O4 K2 129.0(4) . . ?
Mo1 O4 K2 85.92(11) . . ?
K2 O4 K2 80.60(11) 2_477 . ?
C6 O5 K4 123.2(3) . 2_588 ?
C6 O5 K3 129.9(3) . 1_455 ?
K4 O5 K3 106.64(13) 2_588 1_455 ?
C6 O6 Mo2 119.6(3) . . ?
C6 O6 K4 124.4(3) . 1_665 ?
Mo2 O6 K4 92.61(14) . 1_665 ?
C6 O6 K3 121.0(3) . . ?
Mo2 O6 K3 85.64(11) . . ?
K4 O6 K3 104.25(12) 1_665 . ?
C8 O7 K2 132.7(4) . 2_587 ?
C8 O7 K1 129.9(4) . 2_587 ?
K2 O7 K1 97.36(12) 2_587 2_587 ?
C8 O8 Mo2 121.6(4) . . ?
C8 O8 K4 121.9(3) . 1_665 ?
Mo2 O8 K4 97.94(13) . 1_665 ?
C8 O8 K1 121.4(3) . 2_687 ?
Mo2 O8 K1 87.27(11) . 2_687 ?
K4 O8 K1 99.28(12) 1_665 2_687 ?
Mo1 O9 K3 149.24(19) . 2_688 ?
Mo1 O9 K2 90.34(16) . 2_577 ?
K3 O9 K2 115.29(12) 2_688 2_577 ?
Mo1 O9 K4 88.65(15) . . ?
K3 O9 K4 85.99(11) 2_688 . ?
K2 O9 K4 132.47(13) 2_577 . ?
Mo1 O10 K1 130.97(17) . 2_577 ?
Mo1 O10 K2 108.33(15) . 2_477 ?
K1 O10 K2 120.61(14) 2_577 2_477 ?
Mo1 O10 K2 95.59(17) . . ?
K1 O10 K2 95.29(12) 2_577 . ?
K2 O10 K2 80.16(10) 2_477 . ?
Mo1 O10 K4 90.28(15) . . ?
K1 O10 K4 90.41(12) 2_577 . ?
K2 O10 K4 85.88(11) 2_477 . ?
K2 O10 K4 165.95(12) . . ?
Mo1 O11 K1 159.30(19) . . ?
Mo1 O11 K2 101.80(17) . 2_577 ?
K1 O11 K2 97.18(12) . 2_577 ?
Mo1 O11 K2 91.86(15) . . ?
K1 O11 K2 88.28(11) . . ?
K2 O11 K2 112.92(12) 2_577 . ?
Mo2 O12 K4 99.68(14) . 1_665 ?
Mo2 O12 K3 87.74(17) . . ?
K4 O12 K3 95.70(12) 1_665 . ?
Mo2 O12 K1 86.58(15) . 2_687 ?
K4 O12 K1 87.17(11) 1_665 2_687 ?
K3 O12 K1 174.00(14) . 2_687 ?
Mo2 O13 K1 97.32(17) . 2_687 ?
Mo2 O14 K3 97.85(16) . . ?
K3 O1W K4 96.61(15) 2_588 . ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        25.99
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         1.469
_refine_diff_density_min         -0.641
_refine_diff_density_rms         0.139
_database_code_depnum_ccdc_archive 'CCDC 987097'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_sad

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C0 H32 Mo8 N6 O31'
_chemical_formula_weight         1379.84

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'
O O 0.0106 0.0060 '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'
Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           ?
_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                   9.5129(6)
_cell_length_b                   11.3042(6)
_cell_length_c                   14.8647(10)
_cell_angle_alpha                90.00
_cell_angle_beta                 107.488(7)
_cell_angle_gamma                90.00
_cell_volume                     1524.60(16)
_cell_formula_units_Z            2
_cell_measurement_temperature    571(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       ?
_exptl_crystal_colour            ?
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    3.006
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1316
_exptl_absorpt_coefficient_mu    3.299
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6930
_exptl_absorpt_correction_T_max  0.7339
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      571(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            6833
_diffrn_reflns_av_R_equivalents  0.0616
_diffrn_reflns_av_sigmaI/netI    0.0951
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         2.87
_diffrn_reflns_theta_max         26.00
_reflns_number_total             2994
_reflns_number_gt                2139
_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 F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² 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/[σ²(Fo²)+(0.0247P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         2994
_refine_ls_number_parameters     250
_refine_ls_number_restraints     35
_refine_ls_R_factor_all          0.0781
_refine_ls_R_factor_gt           0.0490
_refine_ls_wR_factor_ref         0.1123
_refine_ls_wR_factor_gt          0.0892
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_restrained_S_all      1.061
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Mo1 Mo -0.07351(10) 0.62269(6) 0.14999(6) 0.0126(2) Uani 1 1 d . . .
Mo2 Mo 0.36826(9) 0.62756(6) -0.04053(6) 0.0137(2) Uani 1 1 d . . .
Mo3 Mo 0.13891(9) 0.76897(6) 0.04947(6) 0.0133(2) Uani 1 1 d . . .
Mo4 Mo 0.17610(9) 0.46366(6) 0.06916(5) 0.0110(2) Uani 1 1 d . . .
O1 O 0.0075(7) 0.3848(5) -0.0189(4) 0.0152(14) Uani 1 1 d . . .
O2 O -0.1959(7) 0.5088(5) 0.0689(4) 0.0149(14) Uani 1 1 d . . .
O3 O 0.1076(7) 0.4742(5) 0.1649(5) 0.0190(15) Uani 1 1 d . . .
O4 O 0.0998(7) 0.7188(5) 0.1686(5) 0.0181(15) Uani 1 1 d . . .
O5 O -0.1931(8) 0.7387(5) 0.1303(5) 0.0246(17) Uani 1 1 d . . .
O6 O -0.0628(8) 0.5740(5) 0.2634(5) 0.0229(16) Uani 1 1 d . . .
O8 O 0.2899(7) 0.6019(4) 0.0840(4) 0.0115(14) Uani 1 1 d . . .
O9 O 0.4835(8) 0.7397(5) 0.0129(5) 0.0243(17) Uani 1 1 d . . .
O10 O 0.3552(8) 0.6355(5) -0.1575(5) 0.0252(17) Uani 1 1 d . . .
O11 O -0.0096(7) 0.8601(5) 0.0050(5) 0.0206(16) Uani 1 1 d . . .
O12 O 0.2800(8) 0.8614(5) 0.1067(5) 0.0243(17) Uani 1 1 d . . .
O13 O 0.1878(7) 0.7331(5) -0.0611(4) 0.0148(15) Uani 1 1 d . . .
O14 O 0.2998(8) 0.3511(5) 0.1007(5) 0.0209(16) Uani 1 1 d . . .
O1W O 0.3703(9) 0.6711(7) 0.2964(6) 0.036(2) Uani 1 1 d D . .
O2W O -0.2251(10) -0.4518(7) 0.3850(6) 0.036(2) Uani 1 1 d D . .
O7 O 0.5000 0.5000 0.0000 0.024(2) Uiso 1 2 d S . .
N3 N 0.5662(9) 0.8047(7) 0.2203(6) 0.032(2) Uani 1 1 d D . .
N1 N 0.5075(10) 0.5510(6) 0.7171(6) 0.029(2) Uani 1 1 d D . .
N2 N -0.3244(10) 0.8966(6) -0.0482(6) 0.030(2) Uani 1 1 d D . .
H1 H 0.506(8) 0.567(6) 0.773(2) 0.036 Uiso 1 1 d D . .
H2 H 0.557(6) 0.488(4) 0.718(5) 0.036 Uiso 1 1 d D . .
H3 H 0.420(3) 0.540(6) 0.681(4) 0.036 Uiso 1 1 d D . .
H4 H 0.547(7) 0.608(4) 0.696(5) 0.036 Uiso 1 1 d D . .
H5 H -0.378(6) 0.837(4) -0.047(5) 0.036 Uiso 1 1 d D . .
H6 H -0.337(8) 0.949(5) -0.010(4) 0.036 Uiso 1 1 d D . .
H7 H -0.347(8) 0.926(6) -0.103(2) 0.036 Uiso 1 1 d D . .
H8 H -0.234(2) 0.876(6) -0.031(5) 0.036 Uiso 1 1 d D . .
H9 H 0.528(7) 0.755(4) 0.249(5) 0.036 Uiso 1 1 d D . .
H10 H 0.522(7) 0.802(6) 0.1614(13) 0.036 Uiso 1 1 d D . .
H11 H 0.558(8) 0.874(3) 0.241(5) 0.036 Uiso 1 1 d D . .
H12 H 0.657(2) 0.788(6) 0.230(5) 0.036 Uiso 1 1 d D . .
H1W1 H 0.283(4) 0.673(9) 0.260(5) 0.036 Uiso 1 1 d D . .
H1W2 H 0.371(10) 0.688(8) 0.352(2) 0.036 Uiso 1 1 d D . .
H2W2 H -0.20(3) -0.396(14) 0.355(16) 0.20(13) Uiso 1 1 d D . .
H2W1 H -0.165(15) -0.450(14) 0.353(11) 0.08(6) Uiso 1 1 d D . .


_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
Mo1 O5 1.703(6) . ?
Mo1 O6 1.747(7) . ?
Mo1 O2 1.904(6) . ?
Mo1 O4 1.924(6) . ?
Mo1 O1 2.221(6) 3_565 ?
Mo1 O3 2.368(6) . ?
Mo2 O10 1.707(7) . ?
Mo2 O9 1.708(6) . ?
Mo2 O7 1.8865(8) . ?
Mo2 O13 2.037(6) . ?
Mo2 O2 2.197(6) 3_565 ?
Mo2 O8 2.213(6) . ?
Mo3 O12 1.712(6) . ?
Mo3 O11 1.712(6) . ?
Mo3 O13 1.882(6) . ?
Mo3 O4 1.998(7) . ?
Mo3 O1 2.188(6) 3_565 ?
Mo3 O8 2.335(5) . ?
Mo4 O14 1.700(6) . ?
Mo4 O3 1.738(7) . ?
Mo4 O8 1.876(5) . ?
Mo4 O1 1.954(6) . ?
Mo4 O2 2.139(6) 3_565 ?
Mo4 O1 2.400(6) 3_565 ?
O1 Mo3 2.188(6) 3_565 ?
O1 Mo1 2.221(6) 3_565 ?
O1 Mo4 2.400(6) 3_565 ?
O2 Mo4 2.139(6) 3_565 ?
O2 Mo2 2.197(6) 3_565 ?
O7 Mo2 1.8865(8) 3_665 ?

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
O5 Mo1 O6 104.5(3) . . ?
O5 Mo1 O2 99.3(3) . . ?
O6 Mo1 O2 104.2(3) . . ?
O5 Mo1 O4 95.1(3) . . ?
O6 Mo1 O4 103.9(3) . . ?
O2 Mo1 O4 143.9(3) . . ?
O5 Mo1 O1 103.2(3) . 3_565 ?
O6 Mo1 O1 152.2(3) . 3_565 ?
O2 Mo1 O1 72.5(2) . 3_565 ?
O4 Mo1 O1 72.1(3) . 3_565 ?
O5 Mo1 O3 172.7(3) . . ?
O6 Mo1 O3 81.8(3) . . ?
O2 Mo1 O3 82.5(2) . . ?
O4 Mo1 O3 79.6(2) . . ?
O1 Mo1 O3 70.5(2) 3_565 . ?
O10 Mo2 O9 105.9(3) . . ?
O10 Mo2 O7 101.7(2) . . ?
O9 Mo2 O7 98.5(2) . . ?
O10 Mo2 O13 90.9(3) . . ?
O9 Mo2 O13 91.7(3) . . ?
O7 Mo2 O13 160.86(17) . . ?
O10 Mo2 O2 91.1(3) . 3_565 ?
O9 Mo2 O2 161.4(3) . 3_565 ?
O7 Mo2 O2 84.89(15) . 3_565 ?
O13 Mo2 O2 80.5(2) . 3_565 ?
O10 Mo2 O8 156.8(3) . . ?
O9 Mo2 O8 92.2(3) . . ?
O7 Mo2 O8 89.48(14) . . ?
O13 Mo2 O8 73.9(2) . . ?
O2 Mo2 O8 69.4(2) 3_565 . ?
O12 Mo3 O11 104.9(3) . . ?
O12 Mo3 O13 101.7(3) . . ?
O11 Mo3 O13 100.6(3) . . ?
O12 Mo3 O4 93.4(3) . . ?
O11 Mo3 O4 99.3(3) . . ?
O13 Mo3 O4 150.9(2) . . ?
O12 Mo3 O1 160.6(3) . 3_565 ?
O11 Mo3 O1 89.9(3) . 3_565 ?
O13 Mo3 O1 87.5(2) . 3_565 ?
O4 Mo3 O1 71.5(2) . 3_565 ?
O12 Mo3 O8 92.6(3) . . ?
O11 Mo3 O8 162.4(3) . . ?
O13 Mo3 O8 73.8(2) . . ?
O4 Mo3 O8 80.9(2) . . ?
O1 Mo3 O8 73.4(2) 3_565 . ?
O14 Mo4 O3 102.9(3) . . ?
O14 Mo4 O8 105.3(3) . . ?
O3 Mo4 O8 101.1(3) . . ?
O14 Mo4 O1 101.8(3) . . ?
O3 Mo4 O1 98.4(3) . . ?
O8 Mo4 O1 141.9(2) . . ?
O14 Mo4 O2 96.9(3) . 3_565 ?
O3 Mo4 O2 159.7(3) . 3_565 ?
O8 Mo4 O2 77.1(2) . 3_565 ?
O1 Mo4 O2 73.4(3) . 3_565 ?
O14 Mo4 O1 176.9(3) . 3_565 ?
O3 Mo4 O1 77.8(3) . 3_565 ?
O8 Mo4 O1 77.4(2) . 3_565 ?
O1 Mo4 O1 75.1(2) . 3_565 ?
O2 Mo4 O1 82.1(2) 3_565 3_565 ?
Mo4 O1 Mo3 147.6(3) . 3_565 ?
Mo4 O1 Mo1 102.3(3) . 3_565 ?
Mo3 O1 Mo1 96.8(2) 3_565 3_565 ?
Mo4 O1 Mo4 104.9(2) . 3_565 ?
Mo3 O1 Mo4 98.3(3) 3_565 3_565 ?
Mo1 O1 Mo4 97.2(2) 3_565 3_565 ?
Mo1 O2 Mo4 107.2(3) . 3_565 ?
Mo1 O2 Mo2 151.1(3) . 3_565 ?
Mo4 O2 Mo2 101.2(2) 3_565 3_565 ?
Mo4 O3 Mo1 114.4(3) . . ?
Mo1 O4 Mo3 114.3(3) . . ?
Mo4 O8 Mo2 109.8(3) . . ?
Mo4 O8 Mo3 110.7(3) . . ?
Mo2 O8 Mo3 92.8(2) . . ?
Mo3 O13 Mo2 114.4(3) . . ?
Mo2 O7 Mo2 180.0 3_665 . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         1.112
_refine_diff_density_min         -1.329
_refine_diff_density_rms         0.285
_database_code_depnum_ccdc_archive 'CCDC 987098'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_mop

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'H5 Mo4 N0.50 O15'
_chemical_formula_weight         635.81

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Mo Mo -1.6832 0.6857 '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'
O O 0.0106 0.0060 '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'

_symmetry_cell_setting           ?
_symmetry_space_group_name_H-M   P-1

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

_cell_length_a                   8.2533(9)
_cell_length_b                   8.3054(10)
_cell_length_c                   10.2054(11)
_cell_angle_alpha                104.687(10)
_cell_angle_beta                 105.910(10)
_cell_angle_gamma                109.499(10)
_cell_volume                     586.44(11)
_cell_formula_units_Z            2
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       ?
_exptl_crystal_colour            ?
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    3.601
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             593
_exptl_absorpt_coefficient_mu    4.263
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  0.4827
_exptl_absorpt_correction_T_max  0.8828
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      173(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            3454
_diffrn_reflns_av_R_equivalents  0.0402
_diffrn_reflns_av_sigmaI/netI    0.0666
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_theta_min         3.01
_diffrn_reflns_theta_max         25.00
_reflns_number_total             2065
_reflns_number_gt                1666
_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 F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² 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/[σ²(Fo²)+(0.0268P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         2065
_refine_ls_number_parameters     181
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0495
_refine_ls_R_factor_gt           0.0384
_refine_ls_wR_factor_ref         0.0883
_refine_ls_wR_factor_gt          0.0816
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_restrained_S_all      1.006
_refine_ls_shift/su_max          0.074
_refine_ls_shift/su_mean         0.004

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
Mo1 Mo 0.27689(9) 0.35210(9) 0.94927(7) 0.00677(19) Uani 1 1 d . . .
Mo2 Mo 0.41702(9) 0.00268(9) 0.70679(7) 0.00667(19) Uani 1 1 d . . .
Mo3 Mo 0.27405(8) -0.03897(9) 0.96452(7) 0.00561(18) Uani 1 1 d D . .
Mo4 Mo 0.44094(9) -0.37922(9) 0.72673(7) 0.00690(19) Uani 1 1 d . . .
O5 O 0.5039(7) -0.1861(7) 0.6553(6) 0.0097(12) Uani 1 1 d . . .
O6 O 0.1904(7) -0.1187(7) 0.5767(6) 0.0117(12) Uani 1 1 d . . .
O1 O 0.4305(7) 0.5205(7) 0.8844(6) 0.0089(12) Uani 1 1 d . . .
O2 O 0.0485(7) -0.1625(7) 0.8403(6) 0.0127(12) Uani 1 1 d . . .
O3 O 0.2804(7) 0.1956(7) 1.0698(6) 0.0086(11) Uani 1 1 d . . .
O4 O 0.4028(7) -0.1466(7) 0.8662(6) 0.0098(12) Uani 1 1 d . . .
O7 O 0.5210(7) 0.1566(7) 0.6378(6) 0.0112(12) Uani 1 1 d . . .
O8 O 0.2071(7) -0.5105(8) 0.6139(6) 0.0144(13) Uani 1 1 d . . .
O9 O 0.2137(7) 0.4905(7) 1.0561(6) 0.0136(12) Uani 1 1 d . . .
O10 O 0.0805(7) 0.2270(8) 0.7912(6) 0.0151(13) Uani 1 1 d . . .
O11 O 0.3741(7) 0.1415(7) 0.8593(6) 0.0092(12) Uani 1 1 d . . .
O12 O 0.5502(7) -0.4917(8) 0.6508(6) 0.0116(12) Uani 1 1 d . . .
O13 O 0.2893(7) -0.1244(7) 1.1031(6) 0.0093(12) Uani 1 1 d D . .
H13 H 0.181(4) -0.169(10) 1.109(6) 0.014 Uiso 1 1 d D . .
N14 N -0.1842(9) -0.1421(9) 0.5806(7) 0.0141(16) Uani 1 1 d G . .
H14A H -0.1751 -0.2257 0.5190 0.021 Uiso 1 1 d G . .
H14B H -0.2978 -0.1600 0.5549 0.021 Uiso 1 1 d G . .
N15 N -0.1271(9) 0.4266(10) 0.6865(8) 0.0149(15) Uani 1 1 d G . .
H15A H -0.2434 0.3563 0.6523 0.022 Uiso 1 1 d G . .
H15B H -0.1001 0.3997 0.7622 0.022 Uiso 1 1 d G . .


_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
Mo1 O9 1.691(5) . ?
Mo1 O10 1.703(5) . ?
Mo1 O1 1.936(5) . ?
Mo1 O3 2.005(5) . ?
Mo1 O1 2.229(5) 2_667 ?
Mo1 O11 2.252(5) . ?
Mo2 O7 1.709(5) . ?
Mo2 O6 1.726(5) . ?
Mo2 O11 1.882(5) . ?
Mo2 O5 1.946(5) . ?
Mo2 O4 2.286(5) . ?
Mo2 O13 2.335(5) 2_657 ?
Mo2 Mo3 3.2126(10) . ?
Mo3 O2 1.702(5) . ?
Mo3 O13 1.729(5) . ?
Mo3 O4 1.923(5) . ?
Mo3 O3 1.947(5) . ?
Mo3 O11 2.135(5) . ?
Mo3 O4 2.419(5) 2_657 ?
Mo4 O12 1.693(5) . ?
Mo4 O8 1.726(5) . ?
Mo4 O5 1.902(5) . ?
Mo4 O1 1.999(5) 1_545 ?
Mo4 O4 2.262(5) . ?
Mo4 O3 2.316(5) 2_657 ?
O1 Mo4 1.999(5) 1_565 ?
O1 Mo1 2.229(5) 2_667 ?
O3 Mo4 2.316(5) 2_657 ?
O4 Mo3 2.419(5) 2_657 ?
O13 Mo2 2.335(5) 2_657 ?

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 Mo1 O10 103.1(2) . . ?
O9 Mo1 O1 102.1(2) . . ?
O10 Mo1 O1 100.1(2) . . ?
O9 Mo1 O3 94.0(2) . . ?
O10 Mo1 O3 107.4(3) . . ?
O1 Mo1 O3 143.9(2) . . ?
O9 Mo1 O1 93.1(2) . 2_667 ?
O10 Mo1 O1 163.5(2) . 2_667 ?
O1 Mo1 O1 72.9(2) . 2_667 ?
O3 Mo1 O1 74.1(2) . 2_667 ?
O9 Mo1 O11 164.1(2) . . ?
O10 Mo1 O11 85.2(2) . . ?
O1 Mo1 O11 89.47(19) . . ?
O3 Mo1 O11 70.44(19) . . ?
O1 Mo1 O11 79.81(18) 2_667 . ?
O7 Mo2 O6 103.2(2) . . ?
O7 Mo2 O11 105.1(2) . . ?
O6 Mo2 O11 99.1(2) . . ?
O7 Mo2 O5 102.6(2) . . ?
O6 Mo2 O5 98.0(2) . . ?
O11 Mo2 O5 143.0(2) . . ?
O7 Mo2 O4 156.3(2) . . ?
O6 Mo2 O4 100.4(2) . . ?
O11 Mo2 O4 72.9(2) . . ?
O5 Mo2 O4 71.87(19) . . ?
O7 Mo2 O13 86.5(2) . 2_657 ?
O6 Mo2 O13 170.0(2) . 2_657 ?
O11 Mo2 O13 80.8(2) . 2_657 ?
O5 Mo2 O13 76.9(2) . 2_657 ?
O4 Mo2 O13 69.90(18) . 2_657 ?
O7 Mo2 Mo3 144.39(17) . . ?
O6 Mo2 Mo3 90.78(18) . . ?
O11 Mo2 Mo3 39.68(16) . . ?
O5 Mo2 Mo3 107.77(16) . . ?
O4 Mo2 Mo3 36.23(12) . . ?
O13 Mo2 Mo3 82.75(13) 2_657 . ?
O2 Mo3 O13 105.6(3) . . ?
O2 Mo3 O4 101.8(2) . . ?
O13 Mo3 O4 100.4(2) . . ?
O2 Mo3 O3 103.2(2) . . ?
O13 Mo3 O3 98.3(2) . . ?
O4 Mo3 O3 143.2(2) . . ?
O2 Mo3 O11 98.8(2) . . ?
O13 Mo3 O11 155.5(2) . . ?
O4 Mo3 O11 75.8(2) . . ?
O3 Mo3 O11 74.1(2) . . ?
O2 Mo3 O4 177.0(2) . 2_657 ?
O13 Mo3 O4 77.3(2) . 2_657 ?
O4 Mo3 O4 77.8(2) . 2_657 ?
O3 Mo3 O4 75.83(19) . 2_657 ?
O11 Mo3 O4 78.21(19) . 2_657 ?
O2 Mo3 Mo2 91.08(19) . . ?
O13 Mo3 Mo2 144.39(16) . . ?
O4 Mo3 Mo2 44.64(15) . . ?
O3 Mo3 Mo2 108.35(15) . . ?
O11 Mo3 Mo2 34.26(13) . . ?
O4 Mo3 Mo2 86.60(12) 2_657 . ?
O12 Mo4 O8 104.2(3) . . ?
O12 Mo4 O5 96.3(2) . . ?
O8 Mo4 O5 101.3(2) . . ?
O12 Mo4 O1 98.9(2) . 1_545 ?
O8 Mo4 O1 95.4(2) . 1_545 ?
O5 Mo4 O1 154.0(2) . 1_545 ?
O12 Mo4 O4 159.0(2) . . ?
O8 Mo4 O4 95.8(2) . . ?
O5 Mo4 O4 73.2(2) . . ?
O1 Mo4 O4 85.42(19) 1_545 . ?
O12 Mo4 O3 89.0(2) . 2_657 ?
O8 Mo4 O3 163.4(2) . 2_657 ?
O5 Mo4 O3 87.0(2) . 2_657 ?
O1 Mo4 O3 72.3(2) 1_545 2_657 ?
O4 Mo4 O3 72.56(17) . 2_657 ?
Mo4 O5 Mo2 117.8(3) . . ?
Mo1 O1 Mo4 146.6(3) . 1_565 ?
Mo1 O1 Mo1 107.1(2) . 2_667 ?
Mo4 O1 Mo1 106.2(2) 1_565 2_667 ?
Mo3 O3 Mo1 112.3(2) . . ?
Mo3 O3 Mo4 111.5(2) . 2_657 ?
Mo1 O3 Mo4 102.9(2) . 2_657 ?
Mo3 O4 Mo4 155.4(3) . . ?
Mo3 O4 Mo2 99.1(2) . . ?
Mo4 O4 Mo2 92.89(19) . . ?
Mo3 O4 Mo3 102.2(2) . 2_657 ?
Mo4 O4 Mo3 97.83(17) . 2_657 ?
Mo2 O4 Mo3 95.44(19) . 2_657 ?
Mo2 O11 Mo3 106.1(2) . . ?
Mo2 O11 Mo1 151.3(3) . . ?
Mo3 O11 Mo1 96.88(19) . . ?
Mo3 O13 Mo2 117.1(3) . 2_657 ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         1.254
_refine_diff_density_min         -1.189
_refine_diff_density_rms         0.233
_database_code_depnum_ccdc_archive 'CCDC 987099'
