# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2015

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_mn7
_database_code_depnum_ccdc_archive 'CCDC 970132'
_audit_update_record             
;
2013-11-04 deposited with the CCDC.
2015-02-12 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C20 H16 Cu Mo8 N4 O26, 2(H4 N)'
_chemical_formula_sum            'C20 H24 Cu Mo8 N6 O26'
_chemical_formula_weight         1595.51

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'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_Hall  '-P 1'

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

_cell_length_a                   7.7964(5)
_cell_length_b                   10.4432(5)
_cell_length_c                   13.0463(10)
_cell_angle_alpha                100.635(5)
_cell_angle_beta                 100.924(6)
_cell_angle_gamma                108.981(5)
_cell_volume                     950.96(11)
_cell_formula_units_Z            1
_cell_measurement_temperature    295(2)
_cell_measurement_reflns_used    3432
_cell_measurement_theta_min      2.87
_cell_measurement_theta_max      29.60

_exptl_crystal_description       parallelepiped
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      2.785
_exptl_crystal_density_diffrn    2.786
_exptl_crystal_density_method    piknometric
_exptl_crystal_F_000             759
_exptl_absorpt_coefficient_mu    3.195
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.6078
_exptl_absorpt_correction_T_max  0.7167
_exptl_absorpt_process_details   
;
Oxford Diffraction Poland (2008). CrysAlis Red, Version 171.32.6
;

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      295(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  'KUMA KM-4 with CCD detector'
_diffrn_measurement_method       ω-scan
_diffrn_detector_area_resol_mean '1024x1024 with blocks 2x2'
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            11049
_diffrn_reflns_av_R_equivalents  0.0241
_diffrn_reflns_av_sigmaI/netI    0.0327
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.87
_diffrn_reflns_theta_max         29.60
_reflns_number_total             4702
_reflns_number_gt                3432
_reflns_threshold_expression     I>2σ(I)

_computing_data_collection       
;
Oxford Diffraction Poland (2008). CrysAlis CCD, Version 171.32.6
;
_computing_cell_refinement       
;
Oxford Diffraction Poland (2008). CrysAlis Red, Version 171.32.6
;
_computing_data_reduction        
;
Oxford Diffraction Poland (2008). CrysAlis Red, Version 171.32.6
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    
;
Brandenburg & Putz (2006). Diamond 3.0. Crystal and Molecular
Structure Visualisation, University of Bonn, Germany
;
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'

_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)+(0.0304P)²+3.0681P] 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         4702
_refine_ls_number_parameters     292
_refine_ls_number_restraints     4
_refine_ls_R_factor_all          0.0593
_refine_ls_R_factor_gt           0.0350
_refine_ls_wR_factor_ref         0.0784
_refine_ls_wR_factor_gt          0.0675
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_restrained_S_all      1.000
_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 0.04417(6) 0.24177(4) 0.32908(3) 0.02821(11) Uani 1 1 d . . .
Mo2 Mo -0.22505(5) -0.03354(4) 0.41222(3) 0.02198(10) Uani 1 1 d . . .
Mo3 Mo 0.08866(6) 0.29418(4) 0.58996(3) 0.02657(10) Uani 1 1 d . . .
Mo4 Mo -0.18650(5) 0.02013(4) 0.66754(3) 0.02461(10) Uani 1 1 d . . .
O1 O 0.0990(4) 0.1091(3) 0.4627(2) 0.0256(7) Uani 1 1 d . . .
O2 O -0.2022(4) 0.1046(3) 0.5421(2) 0.0254(7) Uani 1 1 d . . .
O3 O -0.2316(4) 0.0713(3) 0.3225(2) 0.0285(7) Uani 1 1 d . . .
O4 O -0.0170(4) 0.3240(3) 0.4560(3) 0.0299(7) Uani 1 1 d . . .
O5 O 0.2768(5) 0.3521(4) 0.3629(3) 0.0413(9) Uani 1 1 d . . .
O6 O 0.0643(5) 0.0763(3) 0.2516(2) 0.0291(7) Uani 1 1 d . . .
O7 O -0.0682(6) 0.2906(4) 0.2275(3) 0.0448(10) Uani 1 1 d . . .
O8 O -0.4496(4) -0.1487(3) 0.3868(3) 0.0316(8) Uani 1 1 d . . .
O9 O -0.1215(4) -0.1547(3) 0.3312(2) 0.0254(7) Uani 1 1 d . . .
O10 O 0.3205(5) 0.3992(4) 0.6141(3) 0.0404(9) Uani 1 1 d . . .
O11 O 0.0026(5) 0.3849(4) 0.6749(3) 0.0414(9) Uani 1 1 d . . .
O12 O -0.4125(4) -0.0965(4) 0.6302(3) 0.0355(8) Uani 1 1 d . . .
O13 O -0.1751(5) 0.1512(4) 0.7711(3) 0.0369(8) Uani 1 1 d . . .
Cu Cu 0.2989(2) -0.16891(16) 0.06509(11) 0.0442(3) Uani 0.50 1 d P . .
N1 N 0.3251(8) -0.0022(8) 0.0546(4) 0.078(2) Uani 1 1 d . . .
C1 C 0.2152(12) 0.0156(11) -0.0268(6) 0.085(3) Uani 1 1 d . . .
H1 H 0.1409 -0.0629 -0.0839 0.102 Uiso 1 1 calc R . .
C2 C 0.2025(11) 0.1392(12) -0.0334(6) 0.086(3) Uani 1 1 d . . .
H2 H 0.1234 0.1447 -0.0940 0.103 Uiso 1 1 calc R . .
C3 C 0.3104(9) 0.2613(10) 0.0527(5) 0.068(2) Uani 1 1 d . . .
C4 C 0.4306(10) 0.2439(11) 0.1383(5) 0.072(2) Uani 1 1 d . . .
H4 H 0.5078 0.3204 0.1963 0.087 Uiso 1 1 calc R . .
C5 C 0.4334(10) 0.1142(12) 0.1358(5) 0.077(3) Uani 1 1 d . . .
H5 H 0.5147 0.1047 0.1935 0.093 Uiso 1 1 calc R . .
C6 C 0.2960(8) 0.3964(10) 0.0519(5) 0.067(2) Uani 1 1 d . . .
C7 C 0.2213(10) 0.4278(10) -0.0438(5) 0.070(2) Uani 1 1 d . . .
H7 H 0.1735 0.3590 -0.1094 0.084 Uiso 1 1 calc R . .
C8 C 0.2193(9) 0.5576(10) -0.0401(5) 0.071(2) Uani 1 1 d . . .
H8 H 0.1707 0.5762 -0.1041 0.086 Uiso 1 1 calc R . .
N2 N 0.2847(8) 0.6607(8) 0.0523(5) 0.079(2) Uani 1 1 d . . .
C9 C 0.3463(12) 0.6290(12) 0.1447(6) 0.091(3) Uani 1 1 d . . .
H9 H 0.3834 0.6977 0.2097 0.109 Uiso 1 1 calc R . .
C10 C 0.3570(11) 0.5030(13) 0.1479(6) 0.089(3) Uani 1 1 d . . .
H10 H 0.4046 0.4876 0.2135 0.107 Uiso 1 1 calc R . .
N3 N 0.6413(7) 0.3628(5) 0.5088(4) 0.0425(11) Uani 1 1 d D . .
H31 H 0.564(7) 0.314(6) 0.540(5) 0.064 Uiso 1 1 d D . .
H32 H 0.554(7) 0.374(7) 0.463(4) 0.064 Uiso 1 1 d D . .
H33 H 0.694(9) 0.4535(12) 0.535(5) 0.064 Uiso 1 1 d D . .
H34 H 0.719(7) 0.330(7) 0.484(5) 0.064 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 1.699(4) . ?
Mo1 O5 1.721(4) . ?
Mo1 O6 1.904(3) . ?
Mo1 O4 1.936(3) . ?
Mo1 O3 2.276(3) . ?
Mo1 O1 2.477(3) . ?
Mo2 O8 1.699(3) . ?
Mo2 O3 1.749(3) . ?
Mo2 O2 1.949(3) . ?
Mo2 O9 1.966(3) . ?
Mo2 O1 2.150(3) 2_556 ?
Mo2 O1 2.366(3) . ?
Mo2 Mo4 3.2126(6) . ?
Mo3 O11 1.699(4) . ?
Mo3 O10 1.713(4) . ?
Mo3 O4 1.911(3) . ?
Mo3 O9 1.985(3) 2_556 ?
Mo3 O1 2.338(3) . ?
Mo3 O2 2.354(3) . ?
Mo4 O12 1.699(3) . ?
Mo4 O13 1.703(4) . ?
Mo4 O6 1.916(3) 2_556 ?
Mo4 O2 1.999(3) . ?
Mo4 O1 2.316(3) 2_556 ?
Mo4 O9 2.350(3) 2_556 ?
O1 Mo2 2.150(3) 2_556 ?
O1 Mo4 2.316(3) 2_556 ?
O6 Mo4 1.916(3) 2_556 ?
O9 Mo3 1.985(3) 2_556 ?
O9 Mo4 2.350(3) 2_556 ?
Cu N1 1.720(8) . ?
Cu N2 1.721(8) 1_545 ?
N1 C1 1.315(9) . ?
N1 C5 1.354(11) . ?
C1 C2 1.343(12) . ?
C1 H1 0.9300 . ?
C2 C3 1.418(11) . ?
C2 H2 0.9300 . ?
C3 C4 1.395(10) . ?
C3 C6 1.453(12) . ?
C4 C5 1.356(12) . ?
C4 H4 0.9300 . ?
C5 H5 0.9300 . ?
C6 C10 1.397(11) . ?
C6 C7 1.416(10) . ?
C7 C8 1.353(12) . ?
C7 H7 0.9300 . ?
C8 N2 1.343(9) . ?
C8 H8 0.9300 . ?
N2 C9 1.350(10) . ?
N2 Cu 1.721(8) 1_565 ?
C9 C10 1.353(13) . ?
C9 H9 0.9300 . ?
C10 H10 0.9300 . ?
N3 H31 0.870(5) . ?
N3 H32 0.870(5) . ?
N3 H33 0.870(5) . ?
N3 H34 0.870(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 105.68(19) . . ?
O7 Mo1 O6 101.66(17) . . ?
O5 Mo1 O6 98.82(16) . . ?
O7 Mo1 O4 104.17(17) . . ?
O5 Mo1 O4 97.31(16) . . ?
O6 Mo1 O4 144.42(13) . . ?
O7 Mo1 O3 90.62(15) . . ?
O5 Mo1 O3 163.70(15) . . ?
O6 Mo1 O3 77.49(13) . . ?
O4 Mo1 O3 78.17(13) . . ?
O7 Mo1 O1 160.42(15) . . ?
O5 Mo1 O1 93.86(15) . . ?
O6 Mo1 O1 73.54(12) . . ?
O4 Mo1 O1 73.91(12) . . ?
O3 Mo1 O1 69.84(10) . . ?
O8 Mo2 O3 106.04(15) . . ?
O8 Mo2 O2 101.86(15) . . ?
O3 Mo2 O2 97.21(14) . . ?
O8 Mo2 O9 99.62(15) . . ?
O3 Mo2 O9 96.48(14) . . ?
O2 Mo2 O9 150.16(13) . . ?
O8 Mo2 O1 97.23(14) . 2_556 ?
O3 Mo2 O1 156.70(13) . 2_556 ?
O2 Mo2 O1 78.60(12) . 2_556 ?
O9 Mo2 O1 78.36(12) . 2_556 ?
O8 Mo2 O1 172.40(14) . . ?
O3 Mo2 O1 81.48(13) . . ?
O2 Mo2 O1 77.87(12) . . ?
O9 Mo2 O1 78.12(12) . . ?
O1 Mo2 O1 75.23(12) 2_556 . ?
O8 Mo2 Mo4 89.69(11) . . ?
O3 Mo2 Mo4 133.28(11) . . ?
O2 Mo2 Mo4 36.07(9) . . ?
O9 Mo2 Mo4 124.46(9) . . ?
O1 Mo2 Mo4 46.11(9) 2_556 . ?
O1 Mo2 Mo4 85.73(8) . . ?
O11 Mo3 O10 105.16(19) . . ?
O11 Mo3 O4 100.20(16) . . ?
O10 Mo3 O4 100.64(16) . . ?
O11 Mo3 O9 100.49(16) . 2_556 ?
O10 Mo3 O9 99.08(15) . 2_556 ?
O4 Mo3 O9 146.45(13) . 2_556 ?
O11 Mo3 O1 159.33(15) . . ?
O10 Mo3 O1 95.39(15) . . ?
O4 Mo3 O1 77.77(12) . . ?
O9 Mo3 O1 73.58(11) 2_556 . ?
O11 Mo3 O2 88.13(15) . . ?
O10 Mo3 O2 165.43(15) . . ?
O4 Mo3 O2 82.46(12) . . ?
O9 Mo3 O2 72.14(11) 2_556 . ?
O1 Mo3 O2 71.20(11) . . ?
O12 Mo4 O13 105.55(18) . . ?
O12 Mo4 O6 100.24(15) . 2_556 ?
O13 Mo4 O6 99.53(16) . 2_556 ?
O12 Mo4 O2 97.64(15) . . ?
O13 Mo4 O2 102.44(15) . . ?
O6 Mo4 O2 146.69(14) 2_556 . ?
O12 Mo4 O1 93.53(14) . 2_556 ?
O13 Mo4 O1 160.91(15) . 2_556 ?
O6 Mo4 O1 77.32(12) 2_556 2_556 ?
O2 Mo4 O1 73.72(12) . 2_556 ?
O12 Mo4 O9 164.01(14) . 2_556 ?
O13 Mo4 O9 88.86(14) . 2_556 ?
O6 Mo4 O9 83.79(13) 2_556 2_556 ?
O2 Mo4 O9 72.00(12) . 2_556 ?
O1 Mo4 O9 72.12(11) 2_556 2_556 ?
O12 Mo4 Mo2 85.23(12) . . ?
O13 Mo4 Mo2 137.44(12) . . ?
O6 Mo4 Mo2 119.29(10) 2_556 . ?
O2 Mo4 Mo2 35.03(9) . . ?
O1 Mo4 Mo2 41.99(8) 2_556 . ?
O9 Mo4 Mo2 79.37(7) 2_556 . ?
Mo2 O1 Mo4 91.91(12) 2_556 2_556 ?
Mo2 O1 Mo3 91.81(11) 2_556 . ?
Mo4 O1 Mo3 162.68(14) 2_556 . ?
Mo2 O1 Mo2 104.77(12) 2_556 . ?
Mo4 O1 Mo2 97.67(11) 2_556 . ?
Mo3 O1 Mo2 97.72(12) . . ?
Mo2 O1 Mo1 164.22(14) 2_556 . ?
Mo4 O1 Mo1 86.07(10) 2_556 . ?
Mo3 O1 Mo1 85.77(10) . . ?
Mo2 O1 Mo1 91.01(10) . . ?
Mo2 O2 Mo4 108.90(15) . . ?
Mo2 O2 Mo3 110.48(13) . . ?
Mo4 O2 Mo3 103.39(13) . . ?
Mo2 O3 Mo1 117.66(15) . . ?
Mo3 O4 Mo1 116.87(17) . . ?
Mo1 O6 Mo4 117.93(16) . 2_556 ?
Mo2 O9 Mo3 109.45(14) . 2_556 ?
Mo2 O9 Mo4 109.20(13) . 2_556 ?
Mo3 O9 Mo4 103.97(13) 2_556 2_556 ?
N1 Cu N2 168.9(3) . 1_545 ?
C1 N1 C5 116.4(9) . . ?
C1 N1 Cu 120.1(7) . . ?
C5 N1 Cu 122.6(6) . . ?
N1 C1 C2 124.6(9) . . ?
N1 C1 H1 117.7 . . ?
C2 C1 H1 117.7 . . ?
C1 C2 C3 119.7(8) . . ?
C1 C2 H2 120.2 . . ?
C3 C2 H2 120.2 . . ?
C4 C3 C2 116.0(9) . . ?
C4 C3 C6 122.0(8) . . ?
C2 C3 C6 121.9(7) . . ?
C5 C4 C3 119.3(8) . . ?
C5 C4 H4 120.4 . . ?
C3 C4 H4 120.4 . . ?
N1 C5 C4 124.0(7) . . ?
N1 C5 H5 118.0 . . ?
C4 C5 H5 118.0 . . ?
C10 C6 C7 116.6(9) . . ?
C10 C6 C3 120.5(7) . . ?
C7 C6 C3 122.9(7) . . ?
C8 C7 C6 120.2(7) . . ?
C8 C7 H7 119.9 . . ?
C6 C7 H7 119.9 . . ?
N2 C8 C7 122.6(8) . . ?
N2 C8 H8 118.7 . . ?
C7 C8 H8 118.7 . . ?
C8 N2 C9 117.5(9) . . ?
C8 N2 Cu 126.3(7) . 1_565 ?
C9 N2 Cu 116.2(6) . 1_565 ?
N2 C9 C10 123.7(8) . . ?
N2 C9 H9 118.2 . . ?
C10 C9 H9 118.2 . . ?
C9 C10 C6 119.4(8) . . ?
C9 C10 H10 120.3 . . ?
C6 C10 H10 120.3 . . ?
H31 N3 H32 95(6) . . ?
H31 N3 H33 119(6) . . ?
H32 N3 H33 89(6) . . ?
H31 N3 H34 120(6) . . ?
H32 N3 H34 118(7) . . ?
H33 N3 H34 111(6) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
N3 H31 O8 0.870(5) 2.15(3) 2.967(6) 156(6) 2_556 y
N3 H32 O5 0.870(5) 2.22(2) 3.063(7) 163(6) . y
N3 H33 O5 0.870(5) 2.13(3) 2.931(7) 153(6) 2_666 y
N3 H34 O4 0.870(5) 2.18(3) 3.005(6) 159(6) 1_655 y

_diffrn_measured_fraction_theta_max 0.880
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 0.987
_refine_diff_density_max         0.748
_refine_diff_density_min         -0.751
_refine_diff_density_rms         0.131
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_mn6
_database_code_depnum_ccdc_archive 'CCDC 975177'
_audit_update_record             
;
2013-12-04 deposited with the CCDC.
2015-02-12 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'Mo8 O26, 2(C10 H10 N2), 2(C5 H4 N), 2(H2 O)'
_chemical_formula_sum            'C30 H30 Mo8 N6 O28'
_chemical_formula_weight         1690.10

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   'C 2/m'
_symmetry_space_group_name_Hall  '-C 2y'

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

_cell_length_a                   18.8599(8)
_cell_length_b                   19.0464(7)
_cell_length_c                   10.2919(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 104.635(4)
_cell_angle_gamma                90.00
_cell_volume                     3577.0(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    295(2)
_cell_measurement_reflns_used    3240
_cell_measurement_theta_min      2.78
_cell_measurement_theta_max      26.0

_exptl_crystal_description       parallelepiped
_exptl_crystal_colour            grey
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      1.565
_exptl_crystal_density_diffrn    1.567
_exptl_crystal_density_method    floatation
_exptl_crystal_F_000             1620
_exptl_absorpt_coefficient_mu    1.419
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.7633
_exptl_absorpt_correction_T_max  0.9078
_exptl_absorpt_process_details   
;
Oxford Diffraction Poland (2006). CrysAlis Red, Version
171.32.6, Wrocław, Poland
;

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      295(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  'KUMA KM-4 with area CCD detector'
_diffrn_measurement_method       ω-scan
_diffrn_detector_area_resol_mean '1024x1024 with blocks 2x2'
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            21141
_diffrn_reflns_av_R_equivalents  0.0247
_diffrn_reflns_av_sigmaI/netI    0.0306
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         2.78
_diffrn_reflns_theta_max         29.62
_reflns_number_total             4795
_reflns_number_gt                3240
_reflns_threshold_expression     I>2σ(I)

_computing_data_collection       
;
Oxford Diffraction Poland (2006). CrysAlis CCD, Version
171.32.6, Wrocław, Poland
;
_computing_cell_refinement       
;
Oxford Diffraction Poland (2006). CrysAlis Red, Version
171.32.6, Wrocław, Poland
;
_computing_data_reduction        
;
Oxford Diffraction Poland (2006). CrysAlis Red, Version
171.32.6, Wrocław, Poland
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    
;
Brandenburg & Putz (2006). Diamond 3.0. Crystal and Molecular
Structure Visualisation, University of Bonn, Germany
;
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'

_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)+(0.0380P)²+3.3806P] 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         4795
_refine_ls_number_parameters     260
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0658
_refine_ls_R_factor_gt           0.0334
_refine_ls_wR_factor_ref         0.0788
_refine_ls_wR_factor_gt          0.0660
_refine_ls_goodness_of_fit_ref   1.003
_refine_ls_restrained_S_all      1.003
_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 0.079940(18) 0.5000 -0.06490(4) 0.02938(9) Uani 1 2 d S . .
Mo2 Mo 0.039955(14) 0.379397(13) 0.17084(3) 0.03328(8) Uani 1 1 d . . .
Mo3 Mo 0.16374(2) 0.5000 0.27661(4) 0.03740(11) Uani 1 2 d S . .
O1 O 0.10256(17) 0.5000 -0.2135(3) 0.0435(8) Uani 1 2 d S . .
O2 O 0.01389(13) 0.38570(11) 0.3178(2) 0.0443(5) Uani 1 1 d . . .
O3 O 0.13554(18) 0.5000 0.4220(3) 0.0485(8) Uani 1 2 d S . .
O4 O 0.14034(11) 0.40436(12) 0.2261(2) 0.0417(5) Uani 1 1 d . . .
O5 O 0.16453(16) 0.5000 0.0568(3) 0.0411(7) Uani 1 2 d S . .
O6 O 0.04423(13) 0.29160(12) 0.1437(2) 0.0492(6) Uani 1 1 d . . .
O7 O 0.05774(11) 0.40071(10) -0.0452(2) 0.0368(5) Uani 1 1 d . . .
O8 O 0.25772(18) 0.5000 0.3237(4) 0.0573(9) Uani 1 2 d S . .
O9 O 0.03698(15) 0.5000 0.1354(3) 0.0339(6) Uani 1 2 d S . .
C11 C 0.2268(4) 0.2230(4) -0.0041(7) 0.064(3) Uani 0.50 1 d P . .
C12 C 0.1530(5) 0.2269(5) -0.0137(9) 0.071(3) Uani 0.50 1 d P . .
H12 H 0.1311 0.2710 -0.0231 0.085 Uiso 0.50 1 calc PR . .
C13 C 0.1120(6) 0.1727(8) -0.0104(14) 0.099(5) Uani 0.50 1 d P . .
H13 H 0.0626 0.1795 -0.0154 0.116 Uiso 0.50 1 calc PR . .
N14 N 0.1392(7) 0.1059(6) 0.0003(14) 0.096(6) Uani 0.50 1 d P . .
C15 C 0.2126(7) 0.0975(7) 0.0060(15) 0.096(5) Uani 0.50 1 d P . .
H15 H 0.2326 0.0526 0.0135 0.115 Uiso 0.50 1 calc PR . .
C16 C 0.2558(6) 0.1531(5) 0.0009(11) 0.087(3) Uani 0.50 1 d P . .
H16 H 0.3045 0.1462 0.0006 0.105 Uiso 0.50 1 calc PR . .
N21 N 0.2477(5) 0.3254(5) 0.6415(8) 0.093(3) Uani 0.50 1 d P . .
H21 H 0.2799 0.3583 0.6510 0.111 Uiso 0.50 1 calc PR . .
C22 C 0.1755(12) 0.3412(7) 0.6027(11) 0.121(10) Uani 0.50 1 d P . .
H22 H 0.1615 0.3873 0.5801 0.145 Uiso 0.50 1 calc PR . .
C23 C 0.1249(7) 0.2935(6) 0.5962(11) 0.093(4) Uani 0.50 1 d P . .
H23 H 0.0754 0.3047 0.5657 0.111 Uiso 0.50 1 calc PR . .
C24 C 0.1468(6) 0.2261(5) 0.6357(9) 0.077(3) Uani 0.50 1 d P . .
C25 C 0.2200(6) 0.2138(6) 0.6627(9) 0.086(4) Uani 0.50 1 d P . .
H25 H 0.2362 0.1679 0.6813 0.103 Uiso 0.50 1 calc PR . .
C26 C 0.2682(6) 0.2614(7) 0.6642(8) 0.090(4) Uani 0.50 1 d P . .
H26 H 0.3176 0.2497 0.6815 0.108 Uiso 0.50 1 calc PR . .
C27 C 0.1003(5) 0.1819(5) 0.6581(8) 0.072(3) Uani 0.50 1 d P . .
C28 C 0.0335(6) 0.2011(6) 0.6772(9) 0.086(3) Uani 0.50 1 d P . .
H28 H 0.0212 0.2481 0.6820 0.103 Uiso 0.50 1 calc PR . .
C29 C -0.0164(6) 0.1470(7) 0.6892(11) 0.092(3) Uani 0.50 1 d P . .
H29 H -0.0612 0.1597 0.7045 0.110 Uiso 0.50 1 calc PR . .
N30 N -0.0030(5) 0.0826(6) 0.6803(8) 0.086(2) Uani 0.50 1 d P . .
H30 H -0.0361 0.0519 0.6818 0.104 Uiso 0.50 1 calc PR . .
C31 C 0.0597(7) 0.0632(6) 0.6689(10) 0.088(3) Uani 0.50 1 d P . .
H31 H 0.0695 0.0155 0.6650 0.105 Uiso 0.50 1 calc PR . .
C32 C 0.1098(7) 0.1078(9) 0.6626(12) 0.123(5) Uani 0.50 1 d P . .
H32 H 0.1556 0.0903 0.6608 0.147 Uiso 0.50 1 calc PR . .
O1W O 0.0000 0.5000 0.5000 0.0543(13) Uani 1 4 d S . .
O2W O -0.1000(7) 0.0000 0.6902(16) 0.17(2) Uani 0.50 2 d SP . .


_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 O1 1.689(3) . ?
Mo1 O5 1.762(3) . ?
Mo1 O7 1.958(2) 6_565 ?
Mo1 O7 1.958(2) . ?
Mo1 O9 2.140(3) 5_565 ?
Mo1 O9 2.398(3) . ?
Mo1 Mo2 3.2144(4) 2 ?
Mo1 Mo2 3.2144(4) 5_565 ?
Mo2 O6 1.701(2) . ?
Mo2 O2 1.709(2) . ?
Mo2 O4 1.895(2) . ?
Mo2 O7 2.007(2) 2 ?
Mo2 O9 2.3242(5) . ?
Mo2 O7 2.366(2) . ?
Mo2 Mo1 3.2144(4) 5_565 ?
Mo3 O3 1.710(3) . ?
Mo3 O8 1.715(3) . ?
Mo3 O4 1.915(2) 6_565 ?
Mo3 O4 1.915(2) . ?
Mo3 O5 2.266(3) . ?
Mo3 O9 2.464(3) . ?
O7 Mo2 2.007(2) 2 ?
O9 Mo1 2.140(3) 5_565 ?
O9 Mo2 2.3242(5) 6_565 ?
C11 C11 1.340(18) 7 ?
C11 C12 1.373(11) . ?
C11 C16 1.435(10) . ?
C12 C13 1.294(15) . ?
C12 H12 0.9300 . ?
C13 N14 1.365(16) . ?
C13 H13 0.9300 . ?
N14 C15 1.381(14) . ?
C15 C16 1.344(15) . ?
C15 H15 0.9300 . ?
C16 H16 0.9300 . ?
N21 C26 1.282(13) . ?
N21 C22 1.353(19) . ?
N21 H21 0.8600 . ?
C22 C23 1.31(2) . ?
C22 H22 0.9300 . ?
C23 C24 1.379(13) . ?
C23 H23 0.9300 . ?
C24 C27 1.277(13) . ?
C24 C25 1.359(13) . ?
C25 C26 1.282(14) . ?
C25 H25 0.9300 . ?
C26 H26 0.9300 . ?
C27 C28 1.374(12) . ?
C27 C32 1.422(17) . ?
C28 C29 1.422(14) . ?
C28 H28 0.9300 . ?
C29 N30 1.260(13) . ?
C29 H29 0.9300 . ?
N30 C31 1.272(13) . ?
N30 H30 0.8600 . ?
C31 C32 1.284(17) . ?
C31 H31 0.9300 . ?
C32 H32 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Mo1 O5 104.68(14) . . ?
O1 Mo1 O7 101.73(6) . 6_565 ?
O5 Mo1 O7 96.04(7) . 6_565 ?
O1 Mo1 O7 101.73(6) . . ?
O5 Mo1 O7 96.04(7) . . ?
O7 Mo1 O7 149.86(11) 6_565 . ?
O1 Mo1 O9 99.62(13) . 5_565 ?
O5 Mo1 O9 155.70(12) . 5_565 ?
O7 Mo1 O9 78.83(6) 6_565 5_565 ?
O7 Mo1 O9 78.83(6) . 5_565 ?
O1 Mo1 O9 175.07(12) . . ?
O5 Mo1 O9 80.25(11) . . ?
O7 Mo1 O9 77.49(6) 6_565 . ?
O7 Mo1 O9 77.49(6) . . ?
O9 Mo1 O9 75.44(11) 5_565 . ?
O1 Mo1 Mo2 90.56(7) . 2 ?
O5 Mo1 Mo2 132.39(2) . 2 ?
O7 Mo1 Mo2 125.08(6) 6_565 2 ?
O7 Mo1 Mo2 36.35(6) . 2 ?
O9 Mo1 Mo2 46.271(13) 5_565 2 ?
O9 Mo1 Mo2 85.99(5) . 2 ?
O1 Mo1 Mo2 90.56(7) . 5_565 ?
O5 Mo1 Mo2 132.39(2) . 5_565 ?
O7 Mo1 Mo2 36.35(6) 6_565 5_565 ?
O7 Mo1 Mo2 125.08(6) . 5_565 ?
O9 Mo1 Mo2 46.271(13) 5_565 5_565 ?
O9 Mo1 Mo2 85.99(5) . 5_565 ?
Mo2 Mo1 Mo2 91.222(14) 2 5_565 ?
O6 Mo2 O2 104.53(11) . . ?
O6 Mo2 O4 102.17(11) . . ?
O2 Mo2 O4 101.89(10) . . ?
O6 Mo2 O7 99.60(10) . 2 ?
O2 Mo2 O7 97.68(10) . 2 ?
O4 Mo2 O7 145.86(9) . 2 ?
O6 Mo2 O9 161.12(10) . . ?
O2 Mo2 O9 93.92(10) . . ?
O4 Mo2 O9 77.39(9) . . ?
O7 Mo2 O9 73.57(9) 2 . ?
O6 Mo2 O7 89.44(9) . . ?
O2 Mo2 O7 163.87(9) . . ?
O4 Mo2 O7 82.57(8) . . ?
O7 Mo2 O7 71.63(8) 2 . ?
O9 Mo2 O7 71.74(8) . . ?
O6 Mo2 Mo1 134.86(8) . 5_565 ?
O2 Mo2 Mo1 85.13(8) . 5_565 ?
O4 Mo2 Mo1 119.10(7) . 5_565 ?
O7 Mo2 Mo1 35.34(6) 2 5_565 ?
O9 Mo2 Mo1 41.71(7) . 5_565 ?
O7 Mo2 Mo1 79.24(5) . 5_565 ?
O3 Mo3 O8 106.27(17) . . ?
O3 Mo3 O4 97.84(7) . 6_565 ?
O8 Mo3 O4 103.15(7) . 6_565 ?
O3 Mo3 O4 97.84(7) . . ?
O8 Mo3 O4 103.15(7) . . ?
O4 Mo3 O4 144.04(13) 6_565 . ?
O3 Mo3 O5 162.85(13) . . ?
O8 Mo3 O5 90.88(14) . . ?
O4 Mo3 O5 77.76(7) 6_565 . ?
O4 Mo3 O5 77.76(7) . . ?
O3 Mo3 O9 92.64(13) . . ?
O8 Mo3 O9 161.09(14) . . ?
O4 Mo3 O9 73.57(6) 6_565 . ?
O4 Mo3 O9 73.57(6) . . ?
O5 Mo3 O9 70.21(10) . . ?
Mo2 O4 Mo3 117.67(11) . . ?
Mo1 O5 Mo3 118.46(14) . . ?
Mo1 O7 Mo2 108.30(10) . 2 ?
Mo1 O7 Mo2 110.35(9) . . ?
Mo2 O7 Mo2 104.23(8) 2 . ?
Mo1 O9 Mo2 92.02(7) 5_565 . ?
Mo1 O9 Mo2 92.02(7) 5_565 6_565 ?
Mo2 O9 Mo2 162.46(13) . 6_565 ?
Mo1 O9 Mo1 104.56(11) 5_565 . ?
Mo2 O9 Mo1 97.75(6) . . ?
Mo2 O9 Mo1 97.75(6) 6_565 . ?
Mo1 O9 Mo3 164.37(13) 5_565 . ?
Mo2 O9 Mo3 85.77(7) . . ?
Mo2 O9 Mo3 85.76(7) 6_565 . ?
Mo1 O9 Mo3 91.07(9) . . ?
C11 C11 C12 126.7(9) 7 . ?
C11 C11 C16 118.3(9) 7 . ?
C12 C11 C16 115.0(9) . . ?
C13 C12 C11 123.8(9) . . ?
C13 C12 H12 118.1 . . ?
C11 C12 H12 118.1 . . ?
C12 C13 N14 122.1(10) . . ?
C12 C13 H13 119.0 . . ?
N14 C13 H13 119.0 . . ?
C13 N14 C15 117.6(12) . . ?
C16 C15 N14 121.2(11) . . ?
C16 C15 H15 119.4 . . ?
N14 C15 H15 119.4 . . ?
C15 C16 C11 120.2(9) . . ?
C15 C16 H16 119.9 . . ?
C11 C16 H16 119.9 . . ?
C26 N21 C22 119.9(12) . . ?
C26 N21 H21 120.0 . . ?
C22 N21 H21 120.0 . . ?
C23 C22 N21 122.0(11) . . ?
C23 C22 H22 119.0 . . ?
N21 C22 H22 119.0 . . ?
C22 C23 C24 118.1(12) . . ?
C22 C23 H23 121.0 . . ?
C24 C23 H23 121.0 . . ?
C27 C24 C25 123.9(9) . . ?
C27 C24 C23 119.9(10) . . ?
C25 C24 C23 115.7(11) . . ?
C26 C25 C24 124.2(10) . . ?
C26 C25 H25 117.9 . . ?
C24 C25 H25 117.9 . . ?
C25 C26 N21 119.4(10) . . ?
C25 C26 H26 120.3 . . ?
N21 C26 H26 120.3 . . ?
C24 C27 C28 123.2(10) . . ?
C24 C27 C32 125.0(10) . . ?
C28 C27 C32 111.8(11) . . ?
C27 C28 C29 118.2(10) . . ?
C27 C28 H28 120.9 . . ?
C29 C28 H28 120.9 . . ?
N30 C29 C28 123.3(10) . . ?
N30 C29 H29 118.4 . . ?
C28 C29 H29 118.4 . . ?
C29 N30 C31 119.9(11) . . ?
C29 N30 H30 120.0 . . ?
C31 N30 H30 120.0 . . ?
N30 C31 C32 121.6(12) . . ?
N30 C31 H31 119.2 . . ?
C32 C31 H31 119.2 . . ?
C31 C32 C27 124.8(11) . . ?
C31 C32 H32 117.6 . . ?
C27 C32 H32 117.6 . . ?

_diffrn_measured_fraction_theta_max 0.922
_diffrn_reflns_theta_full        28.00
_diffrn_measured_fraction_theta_full 0.982
_refine_diff_density_max         0.768
_refine_diff_density_min         -0.402
_refine_diff_density_rms         0.085
