# Electronic Supplementary Material (ESI) for Green Chemistry.
# 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_t

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C40 H0 Mo8 N8 O26'
_chemical_formula_weight         1776.00

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           Monoclinic
_symmetry_space_group_name_H-M   P21/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                   16.4264(14)
_cell_length_b                   10.8002(9)
_cell_length_c                   17.5844(15)
_cell_angle_alpha                90.00
_cell_angle_beta                 96.3970(10)
_cell_angle_gamma                90.00
_cell_volume                     3100.2(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    273(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.17
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.903
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1680
_exptl_absorpt_coefficient_mu    1.643
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      273(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  'Bruker APEX CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            19087
_diffrn_reflns_av_R_equivalents  0.0362
_diffrn_reflns_av_sigmaI/netI    0.0402
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         1.61
_diffrn_reflns_theta_max         26.04
_reflns_number_total             6096
_reflns_number_gt                4663
_reflns_threshold_expression     >2sigma(I)

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

_refine_special_details          
; 
 Refinement of 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)+(0.0751P)²+11.9572P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   ?
_refine_ls_hydrogen_treatment    ?
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6096
_refine_ls_number_parameters     370
_refine_ls_number_restraints     24
_refine_ls_R_factor_all          0.0701
_refine_ls_R_factor_gt           0.0520
_refine_ls_wR_factor_ref         0.1489
_refine_ls_wR_factor_gt          0.1348
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_restrained_S_all      1.046
_refine_ls_shift/su_max          0.004
_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
C20 C 0.4092(19) -0.057(3) 0.5235(18) 0.269(14) Uani 1 1 d U . .
C11 C 0.3732(9) 0.7789(12) 0.6668(10) 0.118(5) Uani 1 1 d . . .
C7 C 0.6192(9) 0.6047(11) 0.6616(8) 0.109(5) Uani 1 1 d . . .
C1 C 0.8980(10) 1.0337(10) 0.5445(10) 0.144(8) Uani 1 1 d . . .
C14 C 0.3165(8) 0.5720(10) 0.6694(7) 0.082(3) Uani 1 1 d . . .
C2 C 0.7745(7) 1.0775(8) 0.6155(6) 0.077(3) Uani 1 1 d . . .
C6 C 0.6485(6) 0.7280(9) 0.6317(6) 0.066(3) Uani 1 1 d . . .
C9 C 0.5405(12) 0.4121(15) 0.6225(12) 0.151(7) Uani 1 1 d . . .
C8 C 0.5705(11) 0.5335(14) 0.6006(10) 0.143(7) Uani 1 1 d . . .
C10 C 0.6031(11) 0.3165(14) 0.6352(10) 0.135(6) Uani 1 1 d . . .
C12 C 0.4118(9) 0.5990(10) 0.7710(6) 0.102(5) Uani 1 1 d . . .
C3 C 0.7257(6) 1.0100(8) 0.6567(6) 0.069(3) Uani 1 1 d . . .
C4 C 0.8193(6) 0.8830(7) 0.6149(6) 0.072(3) Uani 1 1 d . . .
C13 C 0.3738(6) 0.4914(8) 0.7775(5) 0.062(2) Uani 1 1 d . . .
C5 C 0.7159(5) 0.7797(7) 0.6895(6) 0.058(2) Uani 1 1 d . . .
C15 C 0.2716(8) 0.3577(13) 0.6939(8) 0.113(5) Uani 1 1 d . . .
C16 C 0.3270(12) 0.2729(13) 0.6425(8) 0.145(7) Uani 1 1 d . . .
Mo1 Mo 0.54714(3) 0.12995(5) 1.04846(3) 0.03179(17) Uani 1 1 d . . .
Mo2 Mo 0.66270(3) -0.05231(5) 0.96316(3) 0.03487(17) Uani 1 1 d . . .
Mo3 Mo 0.43136(4) 0.17826(5) 0.89110(4) 0.03591(18) Uani 1 1 d . . .
Mo4 Mo 0.54760(4) -0.00428(7) 0.80350(4) 0.0453(2) Uani 1 1 d . . .
N1 N 0.3663(7) 0.6529(8) 0.7025(6) 0.094(3) Uani 1 1 d . . .
N2 N 0.3193(4) 0.4774(7) 0.7132(4) 0.0595(19) Uani 1 1 d . . .
N3 N 0.8330(6) 0.9968(6) 0.5922(6) 0.089(3) Uani 1 1 d . . .
N4 N 0.7536(4) 0.8887(6) 0.6554(4) 0.0557(18) Uani 1 1 d . . .
O1 O 0.4396(3) 0.1870(4) 1.0058(3) 0.0359(11) Uani 1 1 d . . .
O2 O 0.5357(3) 0.0451(4) 0.9381(3) 0.0315(10) Uani 1 1 d . . .
O3 O 0.4443(3) 0.0799(5) 0.8042(3) 0.0448(12) Uani 1 1 d . . .
O4 O 0.6283(3) -0.0009(4) 1.0642(3) 0.0337(10) Uani 1 1 d . . .
O5 O 0.7154(3) 0.0785(5) 0.9489(3) 0.0525(14) Uani 1 1 d . . .
O6 O 0.6057(3) 0.2529(4) 1.0298(3) 0.0486(13) Uani 1 1 d . . .
O7 O 0.7351(3) -0.1592(5) 0.9929(3) 0.0476(13) Uani 1 1 d . . .
O8 O 0.4957(3) 0.2987(4) 0.8792(3) 0.0495(13) Uani 1 1 d . . .
O9 O 0.6289(3) -0.1058(5) 0.8621(3) 0.0426(12) Uani 1 1 d . . .
O10 O 0.5311(3) 0.1485(4) 1.1444(3) 0.0426(12) Uani 1 1 d . . .
O11 O 0.6084(3) 0.1194(6) 0.7915(3) 0.0613(16) Uani 1 1 d . . .
O12 O 0.3361(3) 0.2377(5) 0.8672(3) 0.0471(12) Uani 1 1 d . . .
O13 O 0.5377(4) -0.0778(7) 0.7175(3) 0.0699(18) Uani 1 1 d . . .
C18 C 0.3129(17) 0.068(3) 0.5690(15) 0.197(10) Uani 1 1 d U . .
C17 C 0.2946(12) 0.1443(17) 0.6374(11) 0.148(6) Uani 1 1 d U . .
C19 C 0.3870(14) 0.073(2) 0.5841(12) 0.165(7) Uani 1 1 d U . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C20 C19 1.83(4) . ?
C11 N1 1.509(14) . ?
C7 C8 1.480(19) . ?
C7 C6 1.529(14) . ?
C1 N3 1.483(11) . ?
C14 N2 1.277(12) . ?
C14 N1 1.290(15) . ?
C2 C3 1.352(12) . ?
C2 N3 1.392(11) . ?
C6 C5 1.525(14) . ?
C9 C10 1.46(2) . ?
C9 C8 1.467(19) . ?
C12 C13 1.330(13) . ?
C12 N1 1.466(15) . ?
C3 N4 1.389(10) . ?
C4 N3 1.319(10) . ?
C4 N4 1.359(9) . ?
C13 N2 1.371(11) . ?
C5 N4 1.487(9) . ?
C15 N2 1.530(13) . ?
C15 C16 1.63(2) . ?
C16 C17 1.49(2) . ?
Mo1 O6 1.693(5) . ?
Mo1 O10 1.748(5) . ?
Mo1 O4 1.941(4) . ?
Mo1 O1 1.942(5) . ?
Mo1 O2 2.136(4) . ?
Mo1 O2 2.356(4) 3_657 ?
Mo2 O5 1.690(5) . ?
Mo2 O7 1.698(5) . ?
Mo2 O9 1.892(5) . ?
Mo2 O4 2.002(4) . ?
Mo2 O1 2.332(4) 3_657 ?
Mo2 O2 2.334(4) . ?
Mo3 O12 1.701(5) . ?
Mo3 O8 1.704(5) . ?
Mo3 O3 1.892(5) . ?
Mo3 O1 2.008(5) . ?
Mo3 O2 2.318(4) . ?
Mo3 O4 2.329(4) 3_657 ?
Mo4 O11 1.696(6) . ?
Mo4 O13 1.699(6) . ?
Mo4 O3 1.926(5) . ?
Mo4 O9 1.934(5) . ?
Mo4 O10 2.280(5) 3_657 ?
Mo4 O2 2.455(4) . ?
O1 Mo2 2.332(4) 3_657 ?
O2 Mo1 2.356(4) 3_657 ?
O4 Mo3 2.329(4) 3_657 ?
O10 Mo4 2.280(5) 3_657 ?
C18 C19 1.22(3) . ?
C18 C17 1.51(3) . ?

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
C8 C7 C6 111.7(12) . . ?
N2 C14 N1 106.9(10) . . ?
C3 C2 N3 106.9(7) . . ?
C5 C6 C7 108.8(9) . . ?
C10 C9 C8 114.9(17) . . ?
C9 C8 C7 116.4(15) . . ?
C13 C12 N1 102.5(9) . . ?
C2 C3 N4 106.4(7) . . ?
N3 C4 N4 106.8(7) . . ?
C12 C13 N2 107.1(8) . . ?
N4 C5 C6 108.9(7) . . ?
N2 C15 C16 107.1(9) . . ?
C17 C16 C15 109.9(14) . . ?
O6 Mo1 O10 104.3(2) . . ?
O6 Mo1 O4 101.6(2) . . ?
O10 Mo1 O4 96.9(2) . . ?
O6 Mo1 O1 100.9(2) . . ?
O10 Mo1 O1 96.2(2) . . ?
O4 Mo1 O1 150.13(18) . . ?
O6 Mo1 O2 98.9(2) . . ?
O10 Mo1 O2 156.8(2) . . ?
O4 Mo1 O2 78.87(18) . . ?
O1 Mo1 O2 78.48(18) . . ?
O6 Mo1 O2 174.6(2) . 3_657 ?
O10 Mo1 O2 81.03(19) . 3_657 ?
O4 Mo1 O2 78.29(17) . 3_657 ?
O1 Mo1 O2 77.45(17) . 3_657 ?
O2 Mo1 O2 75.74(17) . 3_657 ?
O5 Mo2 O7 105.1(3) . . ?
O5 Mo2 O9 102.6(3) . . ?
O7 Mo2 O9 101.8(2) . . ?
O5 Mo2 O4 95.7(2) . . ?
O7 Mo2 O4 99.9(2) . . ?
O9 Mo2 O4 146.72(19) . . ?
O5 Mo2 O1 161.8(2) . 3_657 ?
O7 Mo2 O1 90.1(2) . 3_657 ?
O9 Mo2 O1 83.44(19) . 3_657 ?
O4 Mo2 O1 71.55(16) . 3_657 ?
O5 Mo2 O2 93.3(2) . . ?
O7 Mo2 O2 161.0(2) . . ?
O9 Mo2 O2 78.31(18) . . ?
O4 Mo2 O2 73.04(17) . . ?
O1 Mo2 O2 70.94(15) 3_657 . ?
O12 Mo3 O8 104.3(2) . . ?
O12 Mo3 O3 101.3(2) . . ?
O8 Mo3 O3 101.7(2) . . ?
O12 Mo3 O1 100.8(2) . . ?
O8 Mo3 O1 96.6(2) . . ?
O3 Mo3 O1 146.7(2) . . ?
O12 Mo3 O2 161.1(2) . . ?
O8 Mo3 O2 94.2(2) . . ?
O3 Mo3 O2 78.10(19) . . ?
O1 Mo3 O2 72.97(16) . . ?
O12 Mo3 O4 89.1(2) . 3_657 ?
O8 Mo3 O4 163.8(2) . 3_657 ?
O3 Mo3 O4 84.26(19) . 3_657 ?
O1 Mo3 O4 71.54(16) . 3_657 ?
O2 Mo3 O4 72.03(15) . 3_657 ?
O11 Mo4 O13 104.9(3) . . ?
O11 Mo4 O3 99.3(3) . . ?
O13 Mo4 O3 103.3(3) . . ?
O11 Mo4 O9 97.6(3) . . ?
O13 Mo4 O9 101.6(3) . . ?
O3 Mo4 O9 145.1(2) . . ?
O11 Mo4 O10 163.0(2) . 3_657 ?
O13 Mo4 O10 92.1(3) . 3_657 ?
O3 Mo4 O10 77.3(2) . 3_657 ?
O9 Mo4 O10 77.7(2) . 3_657 ?
O11 Mo4 O2 93.4(2) . . ?
O13 Mo4 O2 161.7(3) . . ?
O3 Mo4 O2 74.09(18) . . ?
O9 Mo4 O2 74.57(17) . . ?
O10 Mo4 O2 69.60(15) 3_657 . ?
C14 N1 C12 110.0(8) . . ?
C14 N1 C11 119.7(11) . . ?
C12 N1 C11 130.2(11) . . ?
C14 N2 C13 112.7(9) . . ?
C14 N2 C15 124.0(10) . . ?
C13 N2 C15 123.2(8) . . ?
C4 N3 C2 110.3(7) . . ?
C4 N3 C1 125.4(7) . . ?
C2 N3 C1 124.2(7) . . ?
C4 N4 C3 109.5(7) . . ?
C4 N4 C5 124.5(6) . . ?
C3 N4 C5 126.0(7) . . ?
Mo1 O1 Mo3 109.3(2) . . ?
Mo1 O1 Mo2 111.1(2) . 3_657 ?
Mo3 O1 Mo2 103.68(19) . 3_657 ?
Mo1 O2 Mo3 92.54(15) . . ?
Mo1 O2 Mo2 92.01(17) . . ?
Mo3 O2 Mo2 163.1(2) . . ?
Mo1 O2 Mo1 104.26(17) . 3_657 ?
Mo3 O2 Mo1 96.98(15) . 3_657 ?
Mo2 O2 Mo1 97.67(15) . 3_657 ?
Mo1 O2 Mo4 163.9(2) . . ?
Mo3 O2 Mo4 85.79(15) . . ?
Mo2 O2 Mo4 85.34(13) . . ?
Mo1 O2 Mo4 91.82(14) 3_657 . ?
Mo3 O3 Mo4 116.7(3) . . ?
Mo1 O4 Mo2 109.4(2) . . ?
Mo1 O4 Mo3 109.78(19) . 3_657 ?
Mo2 O4 Mo3 104.02(17) . 3_657 ?
Mo2 O9 Mo4 116.1(2) . . ?
Mo1 O10 Mo4 117.5(2) . 3_657 ?
C19 C18 C17 95(2) . . ?
C16 C17 C18 117.0(18) . . ?
C18 C19 C20 96(2) . . ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        26.04
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         1.974
_refine_diff_density_min         -1.082
_refine_diff_density_rms         0.153
_database_code_depnum_ccdc_archive 'CCDC 997672'
#######################################################################
#
#                 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_x182

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C44 H0 Mo8 N4 O27'
_chemical_formula_weight         1784.00

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           Monoclinic
_symmetry_space_group_name_H-M   P2(1)/n

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

_cell_length_a                   15.6345(9)
_cell_length_b                   12.1211(7)
_cell_length_c                   16.5893(10)
_cell_angle_alpha                90.00
_cell_angle_beta                 94.6030(10)
_cell_angle_gamma                90.00
_cell_volume                     3133.7(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    188(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.891
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1688
_exptl_absorpt_coefficient_mu    1.625
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  0.7063
_exptl_absorpt_correction_T_max  0.8544
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      188(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  'Bruker APEX CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            19651
_diffrn_reflns_av_R_equivalents  0.0390
_diffrn_reflns_av_sigmaI/netI    0.0423
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         1.72
_diffrn_reflns_theta_max         26.01
_reflns_number_total             6162
_reflns_number_gt                5072
_reflns_threshold_expression     >2sigma(I)

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

_refine_special_details          
; 
 Refinement of 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)+(0.0506P)²+10.2145P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   ?
_refine_ls_hydrogen_treatment    ?
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6162
_refine_ls_number_parameters     379
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0530
_refine_ls_R_factor_gt           0.0415
_refine_ls_wR_factor_ref         0.1109
_refine_ls_wR_factor_gt          0.1042
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_restrained_S_all      1.046
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C20 C 0.3629(4) 0.8861(5) 0.1033(4) 0.0371(15) Uani 1 1 d . . .
Mo1 Mo 0.10177(3) 1.04536(4) 1.04099(3) 0.01760(12) Uani 1 1 d . . .
Mo2 Mo -0.02815(3) 0.84861(4) 1.13009(3) 0.02248(13) Uani 1 1 d . . .
Mo3 Mo 0.08861(3) 0.79684(4) 0.97158(3) 0.01981(13) Uani 1 1 d . . .
Mo4 Mo 0.01973(3) 0.90117(4) 0.79892(3) 0.02419(13) Uani 1 1 d . . .
O1 O 0.0971(2) 0.8902(3) 1.0715(2) 0.0202(8) Uani 1 1 d . . .
O2 O -0.0430(2) 1.0250(3) 1.0677(2) 0.0183(8) Uani 1 1 d . . .
O3 O 0.1074(2) 1.0972(3) 1.1398(2) 0.0236(8) Uani 1 1 d . . .
O4 O 0.0477(2) 1.1760(3) 0.9892(2) 0.0198(8) Uani 1 1 d . . .
O5 O 0.2029(2) 1.0575(3) 1.0125(2) 0.0244(8) Uani 1 1 d . . .
O6 O -0.1334(3) 0.8411(4) 1.1488(2) 0.0329(10) Uani 1 1 d . . .
O7 O 0.0151(3) 0.7267(3) 1.1639(3) 0.0344(10) Uani 1 1 d . . .
O8 O 0.0313(2) 0.7731(3) 0.8689(2) 0.0252(9) Uani 1 1 d . . .
O9 O 0.1916(2) 0.8184(3) 0.9484(2) 0.0262(9) Uani 1 1 d . . .
O10 O 0.0886(3) 0.6678(3) 1.0122(3) 0.0313(9) Uani 1 1 d . . .
O11 O -0.0155(2) 1.0530(3) 0.7879(2) 0.0260(9) Uani 1 1 d . . .
O12 O 0.1244(3) 0.9144(4) 0.7791(2) 0.0328(10) Uani 1 1 d . . .
O13 O -0.0301(3) 0.8449(4) 0.7142(3) 0.0399(11) Uani 1 1 d . . .
N1 N 0.3313(3) 0.9191(4) 0.7951(3) 0.0286(11) Uani 1 1 d . . .
N2 N 0.2394(3) 0.5152(4) 0.1593(3) 0.0380(13) Uani 1 1 d . . .
C1 C 0.3854(4) 0.9543(6) 0.7409(4) 0.0402(16) Uani 1 1 d . . .
C2 C 0.4120(4) 1.0646(6) 0.7428(5) 0.0465(18) Uani 1 1 d . . .
C3 C 0.3830(4) 1.1352(6) 0.8001(5) 0.0453(18) Uani 1 1 d . . .
C4 C 0.3268(4) 1.0967(5) 0.8544(4) 0.0369(15) Uani 1 1 d . . .
C5 C 0.3015(4) 0.9869(5) 0.8506(4) 0.0289(13) Uani 1 1 d . . .
C6 C 0.3035(4) 0.8009(5) 0.7950(4) 0.0335(14) Uani 1 1 d . . .
C7 C 0.3635(4) 0.7324(5) 0.8519(4) 0.0363(15) Uani 1 1 d . . .
C8 C 0.3242(5) 0.6170(5) 0.8596(4) 0.0401(16) Uani 1 1 d . . .
C9 C 0.3846(5) 0.5400(5) 0.9119(4) 0.0442(17) Uani 1 1 d . . .
C10 C 0.3418(6) 0.4270(6) 0.9243(5) 0.055(2) Uani 1 1 d . . .
C11 C 0.4062(6) 0.3486(7) 0.9715(5) 0.066(2) Uani 1 1 d . . .
C12 C 0.1709(5) 0.4688(6) 0.1150(5) 0.054(2) Uani 1 1 d . . .
C13 C 0.1753(5) 0.3579(6) 0.0942(5) 0.056(2) Uani 1 1 d . . .
C14 C 0.2467(5) 0.2954(6) 0.1176(5) 0.0513(19) Uani 1 1 d . . .
C15 C 0.3146(5) 0.3440(6) 0.1640(5) 0.0476(18) Uani 1 1 d . . .
C16 C 0.3086(4) 0.4537(6) 0.1840(4) 0.0416(16) Uani 1 1 d . . .
C17 C 0.2391(5) 0.6348(5) 0.1795(4) 0.0420(17) Uani 1 1 d . . .
C18 C 0.2920(4) 0.7001(5) 0.1205(4) 0.0353(15) Uani 1 1 d . . .
C19 C 0.3042(4) 0.8165(5) 0.1534(4) 0.0368(15) Uani 1 1 d . . .
C21 C 0.3796(4) 0.9998(5) 0.1404(4) 0.0427(17) Uani 1 1 d . . .
C22 C 0.4372(5) 1.0716(7) 0.0911(5) 0.059(2) Uani 1 1 d . . .
O1W O 0.0447(9) 0.4705(11) 0.9291(8) 0.093(5) Uani 0.50 1 d P . .


_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
C20 C21 1.523(9) . ?
C20 C19 1.538(9) . ?
Mo1 O5 1.694(4) . ?
Mo1 O3 1.751(4) . ?
Mo1 O1 1.951(4) . ?
Mo1 O4 1.961(4) . ?
Mo1 O2 2.135(3) 3_577 ?
Mo1 O2 2.353(3) . ?
Mo2 O6 1.701(4) . ?
Mo2 O7 1.702(4) . ?
Mo2 O11 1.895(4) 3_577 ?
Mo2 O4 2.000(4) 3_577 ?
Mo2 O1 2.310(4) . ?
Mo2 O2 2.378(3) . ?
Mo3 O10 1.703(4) . ?
Mo3 O9 1.706(4) . ?
Mo3 O8 1.882(4) . ?
Mo3 O1 2.003(4) . ?
Mo3 O4 2.301(4) 3_577 ?
Mo3 O2 2.350(3) 3_577 ?
Mo4 O13 1.694(4) . ?
Mo4 O12 1.703(4) . ?
Mo4 O11 1.925(4) . ?
Mo4 O8 1.938(4) . ?
Mo4 O3 2.304(4) 3_577 ?
Mo4 O2 2.388(3) 3_577 ?
O2 Mo1 2.135(3) 3_577 ?
O2 Mo3 2.350(3) 3_577 ?
O2 Mo4 2.388(3) 3_577 ?
O3 Mo4 2.304(4) 3_577 ?
O4 Mo2 2.000(4) 3_577 ?
O4 Mo3 2.301(4) 3_577 ?
O11 Mo2 1.895(4) 3_577 ?
N1 C5 1.345(7) . ?
N1 C1 1.350(8) . ?
N1 C6 1.497(8) . ?
N2 C16 1.351(8) . ?
N2 C12 1.369(8) . ?
N2 C17 1.487(8) . ?
C1 C2 1.399(10) . ?
C2 C3 1.383(10) . ?
C3 C4 1.389(9) . ?
C4 C5 1.388(8) . ?
C6 C7 1.523(9) . ?
C7 C8 1.537(9) . ?
C8 C9 1.546(9) . ?
C9 C10 1.544(10) . ?
C10 C11 1.551(11) . ?
C12 C13 1.392(11) . ?
C13 C14 1.378(11) . ?
C14 C15 1.392(10) . ?
C15 C16 1.376(10) . ?
C17 C18 1.548(9) . ?
C18 C19 1.520(8) . ?
C21 C22 1.534(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
C21 C20 C19 111.6(6) . . ?
O5 Mo1 O3 104.62(18) . . ?
O5 Mo1 O1 102.25(16) . . ?
O3 Mo1 O1 95.91(16) . . ?
O5 Mo1 O4 100.77(16) . . ?
O3 Mo1 O4 96.19(16) . . ?
O1 Mo1 O4 150.29(15) . . ?
O5 Mo1 O2 98.47(16) . 3_577 ?
O3 Mo1 O2 156.91(15) . 3_577 ?
O1 Mo1 O2 79.16(14) . 3_577 ?
O4 Mo1 O2 79.10(14) . 3_577 ?
O5 Mo1 O2 174.56(15) . . ?
O3 Mo1 O2 80.70(15) . . ?
O1 Mo1 O2 78.05(13) . . ?
O4 Mo1 O2 77.29(13) . . ?
O2 Mo1 O2 76.20(14) 3_577 . ?
O6 Mo2 O7 104.9(2) . . ?
O6 Mo2 O11 101.57(19) . 3_577 ?
O7 Mo2 O11 101.48(19) . 3_577 ?
O6 Mo2 O4 95.70(17) . 3_577 ?
O7 Mo2 O4 102.81(18) . 3_577 ?
O11 Mo2 O4 145.28(16) 3_577 3_577 ?
O6 Mo2 O1 162.40(16) . . ?
O7 Mo2 O1 90.05(17) . . ?
O11 Mo2 O1 84.03(15) 3_577 . ?
O4 Mo2 O1 71.57(13) 3_577 . ?
O6 Mo2 O2 93.76(16) . . ?
O7 Mo2 O2 161.18(17) . . ?
O11 Mo2 O2 76.34(14) 3_577 . ?
O4 Mo2 O2 72.65(13) 3_577 . ?
O1 Mo2 O2 71.15(12) . . ?
O10 Mo3 O9 105.07(19) . . ?
O10 Mo3 O8 101.67(19) . . ?
O9 Mo3 O8 102.05(17) . . ?
O10 Mo3 O1 101.16(18) . . ?
O9 Mo3 O1 95.70(17) . . ?
O8 Mo3 O1 146.17(15) . . ?
O10 Mo3 O4 89.44(16) . 3_577 ?
O9 Mo3 O4 162.63(16) . 3_577 ?
O8 Mo3 O4 83.89(14) . 3_577 ?
O1 Mo3 O4 71.71(13) . 3_577 ?
O10 Mo3 O2 160.75(16) . 3_577 ?
O9 Mo3 O2 93.88(15) . 3_577 ?
O8 Mo3 O2 77.17(14) . 3_577 ?
O1 Mo3 O2 73.06(13) . 3_577 ?
O4 Mo3 O2 71.31(12) 3_577 3_577 ?
O13 Mo4 O12 105.2(2) . . ?
O13 Mo4 O11 101.36(19) . . ?
O12 Mo4 O11 99.41(19) . . ?
O13 Mo4 O8 100.9(2) . . ?
O12 Mo4 O8 98.41(18) . . ?
O11 Mo4 O8 146.61(16) . . ?
O13 Mo4 O3 90.81(18) . 3_577 ?
O12 Mo4 O3 163.94(17) . 3_577 ?
O11 Mo4 O3 77.50(15) . 3_577 ?
O8 Mo4 O3 77.58(15) . 3_577 ?
O13 Mo4 O2 160.95(18) . 3_577 ?
O12 Mo4 O2 93.80(16) . 3_577 ?
O11 Mo4 O2 75.58(14) . 3_577 ?
O8 Mo4 O2 75.26(14) . 3_577 ?
O3 Mo4 O2 70.15(12) 3_577 3_577 ?
Mo1 O1 Mo3 109.32(16) . . ?
Mo1 O1 Mo2 111.76(16) . . ?
Mo3 O1 Mo2 102.88(15) . . ?
Mo1 O2 Mo3 91.84(12) 3_577 3_577 ?
Mo1 O2 Mo1 103.80(14) 3_577 . ?
Mo3 O2 Mo1 97.27(13) 3_577 . ?
Mo1 O2 Mo2 91.66(12) 3_577 . ?
Mo3 O2 Mo2 164.45(16) 3_577 . ?
Mo1 O2 Mo2 96.59(12) . . ?
Mo1 O2 Mo4 162.88(17) 3_577 3_577 ?
Mo3 O2 Mo4 86.13(11) 3_577 3_577 ?
Mo1 O2 Mo4 93.32(12) . 3_577 ?
Mo2 O2 Mo4 86.07(11) . 3_577 ?
Mo1 O3 Mo4 115.83(18) . 3_577 ?
Mo1 O4 Mo2 109.82(16) . 3_577 ?
Mo1 O4 Mo3 111.60(16) . 3_577 ?
Mo2 O4 Mo3 103.29(15) 3_577 3_577 ?
Mo3 O8 Mo4 115.73(19) . . ?
Mo2 O11 Mo4 116.69(18) 3_577 . ?
C5 N1 C1 122.2(6) . . ?
C5 N1 C6 117.9(5) . . ?
C1 N1 C6 119.9(5) . . ?
C16 N2 C12 120.6(6) . . ?
C16 N2 C17 119.1(5) . . ?
C12 N2 C17 120.3(6) . . ?
N1 C1 C2 119.2(6) . . ?
C3 C2 C1 119.6(6) . . ?
C2 C3 C4 119.8(7) . . ?
C5 C4 C3 119.1(6) . . ?
N1 C5 C4 120.2(6) . . ?
N1 C6 C7 110.9(5) . . ?
C6 C7 C8 108.5(5) . . ?
C7 C8 C9 111.5(6) . . ?
C10 C9 C8 111.0(6) . . ?
C9 C10 C11 109.8(7) . . ?
N2 C12 C13 118.6(7) . . ?
C14 C13 C12 121.0(7) . . ?
C13 C14 C15 119.3(7) . . ?
C16 C15 C14 118.5(7) . . ?
N2 C16 C15 121.9(6) . . ?
N2 C17 C18 110.2(6) . . ?
C19 C18 C17 107.8(5) . . ?
C18 C19 C20 112.2(6) . . ?
C20 C21 C22 112.8(6) . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        26.01
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.861
_refine_diff_density_min         -0.494
_refine_diff_density_rms         0.139
_database_code_depnum_ccdc_archive 'CCDC 997673'
