# Electronic Supplementary Material (ESI) for RSC Advances.
# This journal is © The Royal Society of Chemistry 2016

####################################################################### 
# 
# 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_mn8
_database_code_depnum_ccdc_archive 'CCDC 970131'
_audit_update_record             
;
2013-11-04 deposited with the CCDC.
2016-03-16 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'Mo4 O13, 2(H4 N)'
_chemical_formula_sum            'H8 Mo4 N2 O13'
_chemical_formula_weight         627.84

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
N N 0.0061 0.0033 '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'
Mo Mo -1.6832 0.6857 '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                   8.2674(4)
_cell_length_b                   8.3564(4)
_cell_length_c                   10.2593(5)
_cell_angle_alpha                104.702(5)
_cell_angle_beta                 106.043(4)
_cell_angle_gamma                109.624(6)
_cell_volume                     592.71(7)
_cell_formula_units_Z            2
_cell_measurement_temperature    295(2)
_cell_measurement_reflns_used    2330
_cell_measurement_theta_min      2.84
_cell_measurement_theta_max      26.0

_exptl_crystal_description       parallelepiped
_exptl_crystal_colour            grey
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      3.515
_exptl_crystal_density_diffrn    3.518
_exptl_crystal_density_method    piknometric
_exptl_crystal_F_000             588
_exptl_absorpt_coefficient_mu    4.207
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.4665
_exptl_absorpt_correction_T_max  0.7317
_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            7192
_diffrn_reflns_av_R_equivalents  0.0222
_diffrn_reflns_av_sigmaI/netI    0.0341
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         2.84
_diffrn_reflns_theta_max         29.59
_reflns_number_total             2945
_reflns_number_gt                2330
_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)+(0.0268P)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         2945
_refine_ls_number_parameters     196
_refine_ls_number_restraints     20
_refine_ls_R_factor_all          0.0421
_refine_ls_R_factor_gt           0.0275
_refine_ls_wR_factor_ref         0.0556
_refine_ls_wR_factor_gt          0.0511
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_restrained_S_all      1.038
_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 0.08189(5) 0.49795(5) 0.29252(4) 0.01290(9) Uani 1 1 d . . .
Mo2 Mo 0.05812(5) 0.87841(5) 0.27193(4) 0.01307(9) Uani 1 1 d . . .
Mo3 Mo -0.22350(5) 0.85031(5) -0.05302(4) 0.01300(9) Uani 1 1 d . . .
Mo4 Mo -0.22674(5) 0.46035(5) -0.03695(4) 0.01153(9) Uani 1 1 d . . .
O1 O 0.3077(4) 0.6196(4) 0.4226(3) 0.0208(7) Uani 1 1 d . . .
O2 O -0.4523(4) 0.3360(4) -0.1622(3) 0.0199(7) Uani 1 1 d . . .
O3 O 0.2906(4) 1.0078(4) 0.3826(3) 0.0237(7) Uani 1 1 d . . .
O4 O -0.2896(4) 0.9869(4) 0.0507(4) 0.0261(7) Uani 1 1 d . . .
O5 O -0.2144(4) 0.3753(4) 0.1012(3) 0.0167(6) Uani 1 1 d . . .
O6 O 0.0986(4) 0.6482(4) 0.1335(3) 0.0140(6) Uani 1 1 d . . .
O7 O 0.0686(4) 0.9797(4) 0.1159(3) 0.0150(6) Uani 1 1 d . . .
O8 O -0.0046(4) 0.6873(4) 0.3440(3) 0.0165(6) Uani 1 1 d . . .
O9 O -0.2205(4) 0.6946(4) 0.0686(3) 0.0133(6) Uani 1 1 d . . .
O10 O 0.1246(4) 0.3588(4) 0.1403(3) 0.0133(6) Uani 1 1 d . . .
O11 O -0.0224(4) 0.3453(4) 0.3603(3) 0.0219(7) Uani 1 1 d . . .
O12 O -0.4194(4) 0.7235(4) -0.2122(4) 0.0252(7) Uani 1 1 d . . .
O13 O -0.0496(4) 0.9908(4) 0.3485(3) 0.0220(7) Uani 1 1 d . . .
N1 N 0.3724(5) 0.9251(5) 0.6893(5) 0.0297(10) Uani 1 1 d D . .
H11 H 0.407(5) 0.905(5) 0.619(3) 0.045 Uiso 1 1 d D . .
H12 H 0.421(5) 0.888(5) 0.752(3) 0.045 Uiso 1 1 d D . .
H13 H 0.406(5) 1.0391(13) 0.729(4) 0.045 Uiso 1 1 d D . .
H14 H 0.2543(9) 0.868(4) 0.657(4) 0.045 Uiso 1 1 d D . .
N2 N 0.3148(5) 0.3563(5) 0.5794(4) 0.0248(9) Uani 1 1 d D . .
H21 H 0.346(5) 0.459(2) 0.571(4) 0.037 Uiso 1 1 d D . .
H22 H 0.2005(15) 0.310(4) 0.565(4) 0.037 Uiso 1 1 d D . .
H23 H 0.380(4) 0.371(5) 0.6649(16) 0.037 Uiso 1 1 d D . .
H24 H 0.334(5) 0.285(4) 0.517(3) 0.037 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 O11 1.702(3) . ?
Mo1 O1 1.720(3) . ?
Mo1 O10 1.890(3) . ?
Mo1 O8 1.959(3) . ?
Mo1 O6 2.303(3) . ?
Mo1 O5 2.353(3) . ?
Mo1 Mo4 3.2170(5) 2_565 ?
Mo2 O13 1.693(3) . ?
Mo2 O3 1.711(3) . ?
Mo2 O8 1.903(3) . ?
Mo2 O7 2.001(3) . ?
Mo2 O6 2.266(3) . ?
Mo2 O9 2.315(3) . ?
Mo3 O4 1.690(3) . ?
Mo3 O12 1.709(3) . ?
Mo3 O7 1.942(3) 2_575 ?
Mo3 O9 2.020(2) . ?
Mo3 O7 2.233(3) . ?
Mo3 O10 2.257(3) 2_565 ?
Mo4 O2 1.704(3) . ?
Mo4 O5 1.734(3) . ?
Mo4 O6 1.923(3) 2_565 ?
Mo4 O9 1.957(3) . ?
Mo4 O10 2.138(3) 2_565 ?
Mo4 O6 2.435(3) . ?
Mo4 Mo1 3.2170(5) 2_565 ?
O6 Mo4 1.923(3) 2_565 ?
O7 Mo3 1.942(3) 2_575 ?
O10 Mo4 2.138(3) 2_565 ?
O10 Mo3 2.257(3) 2_565 ?
N1 H11 0.844(5) . ?
N1 H12 0.844(5) . ?
N1 H13 0.845(5) . ?
N1 H14 0.847(5) . ?
N2 H21 0.845(5) . ?
N2 H22 0.844(5) . ?
N2 H23 0.846(5) . ?
N2 H24 0.846(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
O11 Mo1 O1 103.27(14) . . ?
O11 Mo1 O10 105.00(13) . . ?
O1 Mo1 O10 99.30(13) . . ?
O11 Mo1 O8 102.60(13) . . ?
O1 Mo1 O8 97.70(13) . . ?
O10 Mo1 O8 143.08(11) . . ?
O11 Mo1 O6 156.60(13) . . ?
O1 Mo1 O6 100.03(12) . . ?
O10 Mo1 O6 72.96(10) . . ?
O8 Mo1 O6 71.94(10) . . ?
O11 Mo1 O5 86.32(13) . . ?
O1 Mo1 O5 169.92(11) . . ?
O10 Mo1 O5 80.86(11) . . ?
O8 Mo1 O5 76.92(11) . . ?
O6 Mo1 O5 70.29(9) . . ?
O11 Mo1 Mo4 144.39(11) . 2_565 ?
O1 Mo1 Mo4 90.68(10) . 2_565 ?
O10 Mo1 Mo4 39.76(8) . 2_565 ?
O8 Mo1 Mo4 107.83(8) . 2_565 ?
O6 Mo1 Mo4 36.21(7) . 2_565 ?
O5 Mo1 Mo4 83.02(7) . 2_565 ?
O13 Mo2 O3 104.22(15) . . ?
O13 Mo2 O8 95.97(13) . . ?
O3 Mo2 O8 101.29(13) . . ?
O13 Mo2 O7 98.72(12) . . ?
O3 Mo2 O7 94.95(13) . . ?
O8 Mo2 O7 154.69(12) . . ?
O13 Mo2 O6 159.80(13) . . ?
O3 Mo2 O6 94.96(13) . . ?
O8 Mo2 O6 73.76(10) . . ?
O7 Mo2 O6 85.70(10) . . ?
O13 Mo2 O9 89.60(13) . . ?
O3 Mo2 O9 162.78(12) . . ?
O8 Mo2 O9 87.17(11) . . ?
O7 Mo2 O9 72.49(10) . . ?
O6 Mo2 O9 72.84(10) . . ?
O4 Mo3 O12 102.94(16) . . ?
O4 Mo3 O7 101.69(13) . 2_575 ?
O12 Mo3 O7 100.31(13) . 2_575 ?
O4 Mo3 O9 94.19(13) . . ?
O12 Mo3 O9 107.39(13) . . ?
O7 Mo3 O9 143.98(11) 2_575 . ?
O4 Mo3 O7 93.21(13) . . ?
O12 Mo3 O7 163.56(13) . . ?
O7 Mo3 O7 73.05(12) 2_575 . ?
O9 Mo3 O7 73.96(10) . . ?
O4 Mo3 O10 164.30(12) . 2_565 ?
O12 Mo3 O10 85.04(13) . 2_565 ?
O7 Mo3 O10 89.95(10) 2_575 2_565 ?
O9 Mo3 O10 70.38(10) . 2_565 ?
O7 Mo3 O10 80.01(10) . 2_565 ?
O2 Mo4 O5 105.20(13) . . ?
O2 Mo4 O6 101.42(13) . 2_565 ?
O5 Mo4 O6 100.49(12) . 2_565 ?
O2 Mo4 O9 103.48(13) . . ?
O5 Mo4 O9 97.88(12) . . ?
O6 Mo4 O9 143.78(11) 2_565 . ?
O2 Mo4 O10 99.06(12) . 2_565 ?
O5 Mo4 O10 155.65(12) . 2_565 ?
O6 Mo4 O10 76.32(11) 2_565 2_565 ?
O9 Mo4 O10 74.13(10) . 2_565 ?
O2 Mo4 O6 176.75(11) . . ?
O5 Mo4 O6 78.05(11) . . ?
O6 Mo4 O6 77.98(12) 2_565 . ?
O9 Mo4 O6 75.66(10) . . ?
O10 Mo4 O6 77.68(10) 2_565 . ?
O2 Mo4 Mo1 90.97(10) . 2_565 ?
O5 Mo4 Mo1 144.87(9) . 2_565 ?
O6 Mo4 Mo1 45.03(8) 2_565 2_565 ?
O9 Mo4 Mo1 108.55(8) . 2_565 ?
O10 Mo4 Mo1 34.42(7) 2_565 2_565 ?
O6 Mo4 Mo1 86.37(6) . 2_565 ?
Mo4 O5 Mo1 116.55(13) . . ?
Mo4 O6 Mo2 156.29(14) 2_565 . ?
Mo4 O6 Mo1 98.76(11) 2_565 . ?
Mo2 O6 Mo1 92.68(10) . . ?
Mo4 O6 Mo4 102.02(12) 2_565 . ?
Mo2 O6 Mo4 97.58(10) . . ?
Mo1 O6 Mo4 94.90(9) . . ?
Mo3 O7 Mo2 146.43(16) 2_575 . ?
Mo3 O7 Mo3 106.95(12) 2_575 . ?
Mo2 O7 Mo3 106.56(11) . . ?
Mo2 O8 Mo1 117.72(14) . . ?
Mo4 O9 Mo3 111.91(13) . . ?
Mo4 O9 Mo2 111.59(12) . . ?
Mo3 O9 Mo2 102.96(11) . . ?
Mo1 O10 Mo4 105.82(12) . 2_565 ?
Mo1 O10 Mo3 150.92(14) . 2_565 ?
Mo4 O10 Mo3 97.10(10) 2_565 2_565 ?
H11 N1 H12 109.8(8) . . ?
H11 N1 H13 109.6(8) . . ?
H12 N1 H13 109.6(8) . . ?
H11 N1 H14 109.5(8) . . ?
H12 N1 H14 109.2(8) . . ?
H13 N1 H14 109.2(8) . . ?
H21 N2 H22 109.7(8) . . ?
H21 N2 H23 109.3(8) . . ?
H22 N2 H23 109.7(8) . . ?
H21 N2 H24 109.5(8) . . ?
H22 N2 H24 109.6(8) . . ?
H23 N2 H24 109.1(8) . . ?

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
N1 H11 O3 0.844(5) 2.36(3) 2.986(5) 131(3) 2_676 y
N1 H11 O1 0.844(5) 2.40(3) 3.003(5) 129(3) . y
N1 H12 O12 0.844(5) 2.23(2) 2.945(5) 143(3) 1_656 y
N1 H13 O2 0.845(5) 2.17(2) 2.999(5) 168(3) 1_666 y
N1 H14 O11 0.847(5) 2.06(2) 2.819(5) 149(3) 2_566 y
N1 H14 O13 0.847(5) 2.36(3) 2.931(5) 125(3) 2_576 y
N2 H21 O1 0.845(5) 2.30(2) 3.043(5) 148(3) . y
N2 H21 O12 0.845(5) 2.42(3) 2.891(5) 116(3) 1_656 y
N2 H22 O8 0.844(5) 2.09(2) 2.821(5) 145(3) 2_566 y
N2 H22 O11 0.844(5) 2.53(3) 3.015(5) 117(3) . y
N2 H23 O2 0.846(5) 2.08(2) 2.897(5) 162(3) 1_656 y
N2 H24 O3 0.846(5) 2.22(2) 3.000(5) 153(3) 1_545 y

_diffrn_measured_fraction_theta_max 0.882
_diffrn_reflns_theta_full        26.50
_diffrn_measured_fraction_theta_full 0.983
_refine_diff_density_max         0.848
_refine_diff_density_min         -0.754
_refine_diff_density_rms         0.157
