# Electronic Supplementary Material (ESI) for RSC Advances.
# 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_njy1
_database_code_depnum_ccdc_archive 'CCDC 1057225'
_audit_update_record             
;
2015-03-31 deposited with the CCDC.
2015-07-31 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C12 H23 Mo3 N5 O29.50 P Re4'
_chemical_formula_weight         1772.94

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mn Mn 0.3368 0.7283 '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'
Re Re -1.0185 7.2310 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   C2/m

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                   15.6576(19)
_cell_length_b                   19.748(2)
_cell_length_c                   18.942(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 96.895(2)
_cell_angle_gamma                90.00
_cell_volume                     5814.7(12)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    2062
_cell_measurement_theta_min      2.33
_cell_measurement_theta_max      22.25

_exptl_crystal_description       bar
_exptl_crystal_colour            'light yellow'
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.06
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.025
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3228
_exptl_absorpt_coefficient_mu    9.013
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.1160
_exptl_absorpt_correction_T_max  0.6139
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            14238
_diffrn_reflns_av_R_equivalents  0.0479
_diffrn_reflns_av_sigmaI/netI    0.0553
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         1.90
_diffrn_reflns_theta_max         25.00
_reflns_number_total             5256
_reflns_number_gt                4145
_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)+(0.0936P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   notdet
_refine_ls_hydrogen_treatment    noref
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5256
_refine_ls_number_parameters     282
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0667
_refine_ls_R_factor_gt           0.0497
_refine_ls_wR_factor_ref         0.1433
_refine_ls_wR_factor_gt          0.1363
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_restrained_S_all      1.034
_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
Re1 Re 0.37397(3) 0.0000 0.37684(3) 0.04193(19) Uani 1 2 d S . .
Re2 Re 0.24248(2) 0.14506(2) 0.10406(2) 0.04322(17) Uani 1 1 d . . .
Re3 Re 0.00639(3) 0.0000 0.26363(4) 0.0483(2) Uani 1 2 d S . .
Mo1 Mo 0.35895(6) 0.0000 0.20119(6) 0.0326(3) Uani 1 2 d S . .
Mo2 Mo 0.21700(5) 0.09317(4) 0.28923(5) 0.0373(2) Uani 1 1 d . . .
P1 P 0.14246(19) 0.0000 0.14065(19) 0.0309(7) Uani 1 2 d S . .
O1 O 0.4693(5) 0.0000 0.2134(6) 0.048(3) Uani 1 2 d S . .
O2 O 0.3391(4) 0.0634(3) 0.2861(3) 0.0365(14) Uani 1 1 d . . .
O3 O 0.2104(5) 0.0000 0.2095(5) 0.0319(19) Uani 1 2 d S . .
O4 O 0.3332(4) 0.0704(3) 0.1429(3) 0.0387(15) Uani 1 1 d . . .
O5 O 0.2352(5) 0.1473(4) 0.3597(4) 0.060(2) Uani 1 1 d . . .
O6 O 0.2356(6) 0.0000 0.3554(5) 0.046(2) Uani 1 2 d S . .
O7 O 0.2187(4) 0.1457(3) 0.2125(4) 0.0469(18) Uani 1 1 d . . .
O8 O 0.1050(4) 0.0725(4) 0.2870(4) 0.0471(17) Uani 1 1 d . . .
O9 O 0.1548(5) 0.0611(4) 0.0962(4) 0.071(3) Uani 1 1 d . . .
O10 O 0.0512(6) 0.0000 0.1619(6) 0.071(4) Uani 1 2 d S . .
O11 O 0.3945(7) 0.1086(6) 0.4926(5) 0.092(3) Uani 1 1 d . . .
O12 O 0.5712(7) 0.0000 0.3816(8) 0.089(5) Uani 1 2 d S . .
O13 O 0.3747(6) 0.2591(4) 0.1178(5) 0.080(3) Uani 1 1 d . . .
O14 O 0.2722(8) 0.1349(5) -0.0519(6) 0.087(3) Uani 1 1 d . . .
O15 O 0.1015(6) 0.2467(5) 0.0565(6) 0.092(3) Uani 1 1 d . . .
O16 O -0.1312(7) 0.1054(6) 0.2192(7) 0.114(4) Uani 1 1 d . . .
O17 O -0.0501(12) 0.0000 0.4150(10) 0.146(8) Uani 1 2 d S . .
N1 N 0.1444(8) 0.0000 0.9507(7) 0.052(3) Uani 1 2 d S . .
N2 N 0.9692(5) 0.1118(5) 0.0690(5) 0.055(2) Uani 1 1 d . . .
N3 N 0.1600(13) 0.0000 0.4741(11) 0.151(11) Uani 1 2 d S . .
N4 N 0.2836(16) 0.0000 0.8540(14) 0.144(9) Uani 1 2 d S . .
O1W O 0.011(2) 0.2821(19) 0.305(2) 0.082(11) Uani 0.25 1 d PU . .
O2W O 0.5000 0.0498(17) 0.0000 0.097(9) Uani 0.50 2 d SP . .
O3W O 0.4222(15) 0.0000 0.0060(16) 0.089(9) Uani 0.50 2 d SP . .
C1 C 0.3870(7) 0.0668(7) 0.4489(7) 0.064(3) Uani 1 1 d . . .
C2 C 0.4937(10) 0.0000 0.3830(9) 0.052(4) Uani 1 2 d S . .
C3 C 0.3217(7) 0.2152(6) 0.1137(6) 0.053(3) Uani 1 1 d . . .
C4 C 0.2611(8) 0.1387(5) 0.0075(8) 0.054(3) Uani 1 1 d . . .
C5 C 0.1524(7) 0.2100(6) 0.0747(7) 0.059(3) Uani 1 1 d . . .
C6 C -0.0794(8) 0.0660(8) 0.2369(8) 0.071(4) Uani 1 1 d . . .
C7 C -0.0301(12) 0.0000 0.3509(13) 0.078(6) Uani 1 2 d S . .


_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
Re1 C2 1.864(16) . ?
Re1 C1 1.891(13) . ?
Re1 C1 1.891(13) 6 ?
Re1 O2 2.144(6) 6 ?
Re1 O2 2.144(6) . ?
Re1 O6 2.156(9) . ?
Re2 C3 1.854(11) . ?
Re2 C4 1.891(15) . ?
Re2 C5 1.938(12) . ?
Re2 O4 2.118(6) . ?
Re2 O7 2.131(8) . ?
Re2 O9 2.146(7) . ?
Re3 C7 1.81(2) . ?
Re3 C6 1.896(14) 6 ?
Re3 C6 1.896(14) . ?
Re3 O8 2.114(7) . ?
Re3 O8 2.114(7) 6 ?
Re3 O10 2.128(11) . ?
Mo1 O1 1.716(8) . ?
Mo1 O4 1.790(6) 6 ?
Mo1 O4 1.790(6) . ?
Mo1 O2 2.090(6) . ?
Mo1 O2 2.090(6) 6 ?
Mo1 O3 2.350(7) . ?
Mo2 O5 1.706(7) . ?
Mo2 O7 1.788(7) . ?
Mo2 O8 1.795(6) . ?
Mo2 O2 2.008(6) . ?
Mo2 O6 2.226(6) . ?
Mo2 O3 2.375(5) . ?
P1 O9 1.498(8) 6 ?
P1 O9 1.498(8) . ?
P1 O10 1.530(10) . ?
P1 O3 1.581(9) . ?
O3 Mo2 2.375(5) 6 ?
O6 Mo2 2.226(6) 6 ?
O11 C1 1.165(15) . ?
O12 C2 1.218(19) . ?
O13 C3 1.196(13) . ?
O14 C4 1.161(15) . ?
O15 C5 1.101(14) . ?
O16 C6 1.144(16) . ?
O17 C7 1.29(3) . ?
O2W O3W 1.58(3) . ?
O2W O3W 1.58(3) 5_655 ?
O3W O2W 1.58(3) 5_655 ?

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
C2 Re1 C1 86.2(5) . . ?
C2 Re1 C1 86.2(5) . 6 ?
C1 Re1 C1 88.4(9) . 6 ?
C2 Re1 O2 102.0(4) . 6 ?
C1 Re1 O2 168.8(4) . 6 ?
C1 Re1 O2 99.6(4) 6 6 ?
C2 Re1 O2 102.0(4) . . ?
C1 Re1 O2 99.6(4) . . ?
C1 Re1 O2 168.8(4) 6 . ?
O2 Re1 O2 71.5(3) 6 . ?
C2 Re1 O6 172.8(6) . . ?
C1 Re1 O6 98.9(4) . . ?
C1 Re1 O6 98.9(4) 6 . ?
O2 Re1 O6 72.3(3) 6 . ?
O2 Re1 O6 72.3(3) . . ?
C3 Re2 C4 88.0(5) . . ?
C3 Re2 C5 89.4(5) . . ?
C4 Re2 C5 87.6(5) . . ?
C3 Re2 O4 94.2(4) . . ?
C4 Re2 O4 96.6(4) . . ?
C5 Re2 O4 174.6(4) . . ?
C3 Re2 O7 95.4(4) . . ?
C4 Re2 O7 176.3(3) . . ?
C5 Re2 O7 93.9(4) . . ?
O4 Re2 O7 81.8(2) . . ?
C3 Re2 O9 177.4(4) . . ?
C4 Re2 O9 93.1(4) . . ?
C5 Re2 O9 93.1(4) . . ?
O4 Re2 O9 83.3(3) . . ?
O7 Re2 O9 83.5(3) . . ?
C7 Re3 C6 87.3(6) . 6 ?
C7 Re3 C6 87.3(6) . . ?
C6 Re3 C6 86.8(8) 6 . ?
C7 Re3 O8 96.4(5) . . ?
C6 Re3 O8 176.3(5) 6 . ?
C6 Re3 O8 93.9(5) . . ?
C7 Re3 O8 96.4(5) . 6 ?
C6 Re3 O8 93.9(5) 6 6 ?
C6 Re3 O8 176.3(5) . 6 ?
O8 Re3 O8 85.3(4) . 6 ?
C7 Re3 O10 179.1(7) . . ?
C6 Re3 O10 93.4(5) 6 . ?
C6 Re3 O10 93.4(5) . . ?
O8 Re3 O10 83.0(3) . . ?
O8 Re3 O10 83.0(3) 6 . ?
O1 Mo1 O4 103.4(3) . 6 ?
O1 Mo1 O4 103.4(3) . . ?
O4 Mo1 O4 101.8(4) 6 . ?
O1 Mo1 O2 97.9(3) . . ?
O4 Mo1 O2 153.6(3) 6 . ?
O4 Mo1 O2 88.1(3) . . ?
O1 Mo1 O2 97.9(3) . 6 ?
O4 Mo1 O2 88.1(3) 6 6 ?
O4 Mo1 O2 153.6(3) . 6 ?
O2 Mo1 O2 73.6(4) . 6 ?
O1 Mo1 O3 168.5(4) . . ?
O4 Mo1 O3 83.7(2) 6 . ?
O4 Mo1 O3 83.7(2) . . ?
O2 Mo1 O3 73.1(2) . . ?
O2 Mo1 O3 73.1(2) 6 . ?
O5 Mo2 O7 104.8(4) . . ?
O5 Mo2 O8 103.4(4) . . ?
O7 Mo2 O8 102.8(3) . . ?
O5 Mo2 O2 97.8(3) . . ?
O7 Mo2 O2 92.2(3) . . ?
O8 Mo2 O2 149.7(3) . . ?
O5 Mo2 O6 94.5(4) . . ?
O7 Mo2 O6 157.4(3) . . ?
O8 Mo2 O6 83.5(3) . . ?
O2 Mo2 O6 73.4(3) . . ?
O5 Mo2 O3 166.6(3) . . ?
O7 Mo2 O3 86.3(3) . . ?
O8 Mo2 O3 80.9(3) . . ?
O2 Mo2 O3 73.9(3) . . ?
O6 Mo2 O3 73.2(3) . . ?
O9 P1 O9 107.4(8) 6 . ?
O9 P1 O10 109.6(5) 6 . ?
O9 P1 O10 109.6(5) . . ?
O9 P1 O3 110.2(3) 6 . ?
O9 P1 O3 110.2(3) . . ?
O10 P1 O3 109.9(6) . . ?
Mo2 O2 Mo1 115.4(3) . . ?
Mo2 O2 Re1 107.4(3) . . ?
Mo1 O2 Re1 102.7(3) . . ?
P1 O3 Mo1 121.2(5) . . ?
P1 O3 Mo2 119.9(2) . . ?
Mo1 O3 Mo2 94.3(2) . . ?
P1 O3 Mo2 119.9(2) . 6 ?
Mo1 O3 Mo2 94.3(2) . 6 ?
Mo2 O3 Mo2 101.6(3) . 6 ?
Mo1 O4 Re2 147.9(3) . . ?
Re1 O6 Mo2 99.6(3) . 6 ?
Re1 O6 Mo2 99.6(3) . . ?
Mo2 O6 Mo2 111.5(4) 6 . ?
Mo2 O7 Re2 143.3(4) . . ?
Mo2 O8 Re3 147.7(4) . . ?
P1 O9 Re2 135.1(4) . . ?
P1 O10 Re3 131.1(7) . . ?
O3W O2W O3W 103(2) . 5_655 ?
O2W O3W O2W 77(2) . 5_655 ?
O11 C1 Re1 179.1(13) . . ?
O12 C2 Re1 175.1(14) . . ?
O13 C3 Re2 177.1(11) . . ?
O14 C4 Re2 179.7(13) . . ?
O15 C5 Re2 178.5(13) . . ?
O16 C6 Re3 178.5(14) . . ?
O17 C7 Re3 175.7(17) . . ?

_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.995
_refine_diff_density_max         1.910
_refine_diff_density_min         -1.658
_refine_diff_density_rms         0.276
