# Electronic Supplementary Material (ESI) for New Journal of Chemistry.
# This journal is © The Royal Society of Chemistry and the Centre National de la Recherche Scientifique 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_shelx
_database_code_depnum_ccdc_archive 'CCDC 1431341'
_audit_update_record             
;
2016-01-13 deposited with the CCDC.
2016-06-06 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C30 H92 Mo12 N10 Ni O73 P8'
_chemical_formula_weight         3218.89

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'
Ni Ni 0.3393 1.1124 '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'

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

_cell_length_a                   13.244(5)
_cell_length_b                   13.546(5)
_cell_length_c                   14.691(5)
_cell_angle_alpha                74.100(5)
_cell_angle_beta                 69.748(5)
_cell_angle_gamma                65.588(5)
_cell_volume                     2225.0(14)
_cell_formula_units_Z            1
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    300
_cell_measurement_theta_min      1.67
_cell_measurement_theta_max      27.18

_exptl_crystal_description       Block
_exptl_crystal_colour            Brown
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.10
_exptl_crystal_density_diffrn    2.402
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1578
_exptl_absorpt_coefficient_mu    2.104
_exptl_absorpt_correction_type   EMPIRICAL
_exptl_absorpt_correction_T_min  0.674
_exptl_absorpt_correction_T_max  0.810
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      293(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 SMART APEX-II CCD'
_diffrn_standards_number         n/a
_diffrn_standards_interval_count n/a
_diffrn_standards_interval_time  n/a
_diffrn_standards_decay_%        n/a
_diffrn_reflns_number            35849
_diffrn_reflns_av_R_equivalents  0.0280
_diffrn_reflns_av_sigmaI/netI    0.0267
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         1.50
_diffrn_reflns_theta_max         27.18
_reflns_number_total             9812
_reflns_number_gt                9188
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'BRUKER SMART APEX II CCD'
_computing_cell_refinement       'BRUKER SMART APEX II CCD'
_computing_data_reduction        'BRUKER SAINT'
_computing_structure_solution    SHELXS-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Diamond 3.0'
_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)+(0.0436P)²+10.3929P] 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         9812
_refine_ls_number_parameters     630
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0341
_refine_ls_R_factor_gt           0.0318
_refine_ls_wR_factor_ref         0.0912
_refine_ls_wR_factor_gt          0.0896
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_restrained_S_all      1.049
_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
Mo2 Mo 0.40552(3) 0.31035(3) 0.92676(2) 0.01381(8) Uani 1 1 d . . .
Mo1 Mo 0.44708(3) 0.22840(3) 1.09579(2) 0.01451(8) Uani 1 1 d . . .
Mo3 Mo 0.36442(3) 0.40060(3) 1.26736(2) 0.01561(8) Uani 1 1 d . . .
Mo4 Mo 0.26426(3) 0.60994(3) 1.22438(2) 0.01574(8) Uani 1 1 d . . .
Mo5 Mo 0.20850(3) 0.71994(3) 0.99521(2) 0.01541(8) Uani 1 1 d . . .
Mo6 Mo 0.26569(3) 0.59232(3) 0.86855(2) 0.01508(8) Uani 1 1 d . . .
Ni1 Ni 0.5000 0.5000 1.0000 0.01917(15) Uani 1 2 d S . .
P1 P 0.20674(8) 0.46304(8) 1.10516(7) 0.01400(19) Uani 1 1 d . . .
P2 P 0.32272(9) 0.16232(8) 1.33275(8) 0.0179(2) Uani 1 1 d . . .
P4 P 0.20480(9) 0.41108(8) 0.80598(8) 0.0168(2) Uani 1 1 d . . .
P3 P 0.00984(9) 0.79727(8) 1.20177(8) 0.0197(2) Uani 1 1 d . . .
O2 O 0.2529(2) 0.4530(2) 0.9955(2) 0.0163(5) Uani 1 1 d . A .
O4 O 0.2926(2) 0.3736(2) 1.1594(2) 0.0158(5) Uani 1 1 d . A .
O3 O 0.1941(2) 0.5769(2) 1.1184(2) 0.0162(5) Uani 1 1 d . A .
O1 O 0.0906(2) 0.4472(2) 1.1471(3) 0.0259(7) Uani 1 1 d . A 1
O12 O 0.4342(3) 0.3991(3) 1.3440(2) 0.0278(7) Uani 1 1 d . . .
O20 O 0.0328(3) 0.0902(3) 1.7722(3) 0.0320(8) Uani 1 1 d . . .
O23 O 0.7810(3) 0.1649(2) 1.0799(2) 0.0261(7) Uani 1 1 d . . .
O8 O 0.3712(3) 0.1482(2) 1.2241(2) 0.0255(7) Uani 1 1 d . . .
O30 O 0.2785(3) 0.3210(2) 0.8715(2) 0.0216(6) Uani 1 1 d . D .
O25 O 0.2900(3) 0.6779(3) 0.7642(2) 0.0278(7) Uani 1 1 d . . .
O17 O 0.0979(3) 0.7160(3) 1.2574(2) 0.0265(7) Uani 1 1 d . . .
O31 O 0.5179(3) 0.2209(3) 0.8592(2) 0.0243(6) Uani 1 1 d . . .
O21 O 0.0575(3) 0.7967(2) 1.0910(2) 0.0254(6) Uani 1 1 d . . .
O6 O 0.5675(3) 0.1211(2) 1.0645(2) 0.0256(7) Uani 1 1 d . . .
O11 O 0.3052(3) 0.2768(2) 1.3483(2) 0.0234(6) Uani 1 1 d . . .
O16 O 0.3127(3) 0.6540(3) 1.2914(2) 0.0279(7) Uani 1 1 d . . .
O10 O 0.3926(3) 0.0724(3) 1.3954(2) 0.0339(8) Uani 1 1 d . . .
O9 O 0.1968(3) 0.1618(3) 1.3642(3) 0.0378(8) Uani 1 1 d . . .
O19 O 0.0965(3) 0.2406(3) 0.7640(3) 0.0295(7) Uani 1 1 d . . .
O26 O 0.1794(3) 0.5264(2) 0.8248(2) 0.0227(6) Uani 1 1 d . D .
O27 O 0.4089(2) 0.4539(2) 0.8267(2) 0.0175(5) Uani 1 1 d . . .
O28 O 0.2609(3) 0.4008(3) 0.6993(2) 0.0356(8) Uani 1 1 d . D .
O18 O 0.2842(2) 0.7244(2) 1.0968(2) 0.0171(5) Uani 1 1 d . . .
O22 O 0.1171(2) 0.6744(2) 0.9476(2) 0.0204(6) Uani 1 1 d . . .
O5 O 0.3387(2) 0.2222(2) 1.0390(2) 0.0186(6) Uani 1 1 d . . .
O7 O 0.4987(2) 0.2796(2) 1.1892(2) 0.0176(6) Uani 1 1 d . . .
N3 N 0.1021(3) 0.0271(3) 1.1609(3) 0.0258(8) Uani 1 1 d . . .
N4 N 0.1111(4) 0.2364(3) 1.0452(4) 0.0337(10) Uani 1 1 d . . .
N1 N 0.3961(4) 0.0584(3) 1.6769(3) 0.0314(9) Uani 1 1 d D . .
O13 O 0.5922(2) 0.4931(2) 0.8467(2) 0.0175(6) Uani 1 1 d . . .
O14 O 0.4822(2) 0.3508(2) 0.99742(19) 0.0159(5) Uani 1 1 d . . .
C2 C 0.3227(5) -0.0070(5) 1.7419(4) 0.0429(13) Uani 1 1 d . B .
H2A H 0.3608 -0.0577 1.7910 0.052 Uiso 1 1 calc R . .
H2B H 0.2502 0.0425 1.7760 0.052 Uiso 1 1 calc R . .
N2 N 0.4471(4) 0.2578(4) 1.5981(3) 0.0406(10) Uani 1 1 d D . .
H2C H 0.4948 0.2934 1.5590 0.049 Uiso 1 1 calc R . .
H2D H 0.3827 0.3070 1.6294 0.049 Uiso 1 1 calc RD . .
C10 C 0.1744(5) 0.1336(5) 1.0016(4) 0.0370(12) Uani 1 1 d . . .
H10A H 0.2526 0.1033 1.0076 0.044 Uiso 1 1 calc R . .
H10B H 0.1777 0.1497 0.9323 0.044 Uiso 1 1 calc R . .
C3 C 0.4251(5) 0.1114(5) 1.7369(4) 0.0416(13) Uani 1 1 d . . .
H3A H 0.4630 0.0556 1.7840 0.050 Uiso 1 1 calc R . .
H3B H 0.3550 0.1616 1.7730 0.050 Uiso 1 1 calc R . .
C1 C 0.2983(6) -0.0705(5) 1.6884(5) 0.0512(15) Uani 1 1 d . . .
O32A O 0.2135(6) -0.0085(6) 1.6379(5) 0.0560(17) Uani 0.70 1 d P B 1
C9 C 0.1161(5) 0.0501(4) 1.0525(4) 0.0357(11) Uani 1 1 d . . .
H9A H 0.0411 0.0774 1.0402 0.043 Uiso 1 1 calc R . .
H9B H 0.1614 -0.0175 1.0252 0.043 Uiso 1 1 calc R . .
C7 C 0.1995(6) -0.0867(5) 1.2940(5) 0.0524(16) Uani 1 1 d . . .
C6 C 0.3421(5) 0.1435(4) 1.6009(4) 0.0334(11) Uani 1 1 d . . .
H6A H 0.2686 0.1933 1.6333 0.040 Uiso 1 1 calc R . .
H6B H 0.3280 0.1079 1.5599 0.040 Uiso 1 1 calc R . .
C12 C 0.0346(4) 0.1324(4) 1.2019(4) 0.0300(10) Uani 1 1 d . . .
H12A H 0.0259 0.1182 1.2721 0.036 Uiso 1 1 calc R . .
H12B H -0.0415 0.1619 1.1914 0.036 Uiso 1 1 calc R . .
C11 C 0.0932(5) 0.2160(4) 1.1540(4) 0.0338(11) Uani 1 1 d . . .
H11A H 0.0463 0.2841 1.1802 0.041 Uiso 1 1 calc R . .
H11B H 0.1669 0.1892 1.1688 0.041 Uiso 1 1 calc R . .
C4 C 0.5031(5) 0.1729(5) 1.6710(4) 0.0445(14) Uani 1 1 d . . .
H4A H 0.5210 0.2072 1.7104 0.053 Uiso 1 1 calc R . .
H4B H 0.5746 0.1220 1.6372 0.053 Uiso 1 1 calc R . .
C5 C 0.4177(5) 0.2076(5) 1.5376(4) 0.0410(13) Uani 1 1 d . . .
H5A H 0.4878 0.1594 1.4995 0.049 Uiso 1 1 calc R . .
H5B H 0.3783 0.2648 1.4922 0.049 Uiso 1 1 calc R . .
O33A O 0.1615(7) -0.0136(5) 1.3587(5) 0.0569(17) Uani 0.70 1 d P C 2
C8 C 0.2146(5) -0.0386(4) 1.1873(4) 0.0397(12) Uani 1 1 d . C .
H8A H 0.2578 -0.0976 1.1482 0.048 Uiso 1 1 calc R . .
H8B H 0.2592 0.0084 1.1707 0.048 Uiso 1 1 calc R . .
O33B O 0.1153(14) -0.1128(12) 1.3438(10) 0.052(4) Uani 0.30 1 d P C 1
O24 O 0.3567(2) 0.6082(2) 0.9424(2) 0.0168(5) Uani 1 1 d . . .
O15 O 0.2071(3) 0.4976(2) 1.3140(2) 0.0203(6) Uani 1 1 d . . .
O32B O 0.3909(12) -0.1445(12) 1.6521(11) 0.048(3) Uani 0.30 1 d P B 2
O29 O 0.0889(3) 0.3932(3) 0.8387(3) 0.0309(8) Uani 1 1 d . D 2
O37 O 0.1601(7) -0.1276(7) 1.5399(5) 0.1125(14) Uani 1 1 d . . .
O36 O 0.3593(9) -0.3018(8) 1.5456(6) 0.143(2) Uani 1 1 d . . .
O35 O 0.5351(10) -0.4640(10) 1.3926(7) 0.1733(16) Uani 1 1 d . . .
N5 N 0.0151 0.4473 1.4221 0.101(3) Uani 1 1 d . . .
C13 C -0.0781(6) 0.5607(6) 1.4426(5) 0.0697(16) Uani 1 1 d . . .
H13A H -0.0953 0.6035 1.3815 0.084 Uiso 1 1 calc R . .
H13B H -0.1479 0.5501 1.4868 0.084 Uiso 1 1 calc R . .
C14 C 0.0434(6) 0.3793(6) 1.5152(5) 0.0648(15) Uani 1 1 d . . .
H14A H -0.0234 0.3637 1.5605 0.078 Uiso 1 1 calc R . .
H14B H 0.1051 0.3102 1.5015 0.078 Uiso 1 1 calc R . .
C15 C -0.0162(12) 0.4026(11) 1.3807(10) 0.0497(15) Uani 0.50 1 d P . .
H15A H 0.0499 0.3402 1.3569 0.060 Uiso 0.50 1 calc PR . .
H15B H -0.0361 0.4536 1.3234 0.060 Uiso 0.50 1 calc PR . .
O34B O -0.2238(17) 0.4411(16) 1.4553(14) 0.0413(15) Uani 0.20 1 d P . .
C16 C -0.1150(12) 0.3621(11) 1.4354(10) 0.0514(16) Uani 0.50 1 d P . .
O34A O -0.0965(12) 0.3294(11) 1.3526(10) 0.0423(11) Uani 0.30 1 d P . .
H3 H 0.059(6) -0.014(6) 1.182(5) 0.06(2) Uiso 1 1 d . . .
H4 H 0.050(6) 0.271(5) 1.024(5) 0.046(18) Uiso 1 1 d . . .
H4D H 0.151(6) 0.280(6) 1.012(5) 0.056 Uiso 1 1 d . . .
H1 H 0.460(4) 0.011(4) 1.642(4) 0.056 Uiso 1 1 d D . .
H5 H 0.0797 0.4564 1.3822 0.056 Uiso 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
Mo2 O31 1.677(3) . ?
Mo2 O5 1.927(3) . ?
Mo2 O14 1.977(3) . ?
Mo2 O30 2.047(3) . ?
Mo2 O27 2.099(3) . ?
Mo2 O2 2.295(3) . ?
Mo2 Mo1 2.5753(9) . ?
Mo1 O6 1.676(3) . ?
Mo1 O5 1.932(3) . ?
Mo1 O14 1.978(3) . ?
Mo1 O8 2.052(3) . ?
Mo1 O7 2.097(3) . ?
Mo1 O4 2.299(3) . ?
Mo3 O12 1.678(3) . ?
Mo3 O15 1.944(3) . ?
Mo3 O13 1.976(3) 2_667 ?
Mo3 O11 2.047(3) . ?
Mo3 O7 2.091(3) . ?
Mo3 O4 2.281(3) . ?
Mo3 Mo4 2.5864(10) . ?
Mo4 O16 1.678(3) . ?
Mo4 O15 1.946(3) . ?
Mo4 O13 1.971(3) 2_667 ?
Mo4 O17 2.044(3) . ?
Mo4 O18 2.095(3) . ?
Mo4 O3 2.284(3) . ?
Mo5 O23 1.673(3) 2_667 ?
Mo5 O22 1.943(3) . ?
Mo5 O24 1.970(3) . ?
Mo5 O21 2.049(3) . ?
Mo5 O18 2.091(3) . ?
Mo5 O3 2.283(3) . ?
Mo5 Mo6 2.5940(8) . ?
Mo6 O25 1.671(3) . ?
Mo6 O22 1.943(3) . ?
Mo6 O24 1.980(3) . ?
Mo6 O26 2.044(3) . ?
Mo6 O27 2.092(3) . ?
Mo6 O2 2.277(3) . ?
Ni1 O14 2.141(3) . ?
Ni1 O14 2.141(3) 2_667 ?
Ni1 O24 2.145(3) 2_667 ?
Ni1 O24 2.145(3) . ?
Ni1 O13 2.166(3) 2_667 ?
Ni1 O13 2.166(3) . ?
P1 O1 1.528(3) . ?
P1 O4 1.535(3) . ?
P1 O2 1.535(3) . ?
P1 O3 1.540(3) . ?
P2 O10 1.494(3) . ?
P2 O8 1.534(3) . ?
P2 O11 1.540(3) . ?
P2 O9 1.571(4) . ?
P4 O28 1.502(3) . ?
P4 O26 1.539(3) . ?
P4 O29 1.542(3) . ?
P4 O30 1.546(3) . ?
P3 O20 1.500(3) 2_568 ?
P3 O21 1.529(3) . ?
P3 O17 1.531(3) . ?
P3 O19 1.570(3) 2_567 ?
O20 P3 1.500(3) 2_568 ?
O23 Mo5 1.673(3) 2_667 ?
O19 P3 1.570(3) 2_567 ?
N3 C12 1.497(6) . ?
N3 C9 1.497(6) . ?
N3 C8 1.509(6) . ?
N4 C10 1.485(7) . ?
N4 C11 1.497(7) . ?
N1 C2 1.499(7) . ?
N1 C3 1.500(7) . ?
N1 C6 1.500(6) . ?
O13 Mo4 1.971(3) 2_667 ?
O13 Mo3 1.976(3) 2_667 ?
C2 C1 1.496(9) . ?
N2 C4 1.479(8) . ?
N2 C5 1.481(7) . ?
C10 C9 1.513(7) . ?
C3 C4 1.509(9) . ?
C1 O32B 1.273(14) . ?
C1 O32A 1.404(10) . ?
C7 O33B 1.234(16) . ?
C7 O33A 1.382(9) . ?
C7 C8 1.501(9) . ?
C6 C5 1.502(8) . ?
C12 C11 1.514(6) . ?
N5 C15 1.222(13) . ?
N5 C14 1.496(7) . ?
N5 C13 1.550(7) . ?
C13 C14 1.427(12) 2_568 ?
C14 C13 1.427(12) 2_568 ?
C15 C16 1.511(17) . ?
C15 O34A 1.919(17) . ?
O34B C16 1.38(2) . ?
C16 O34A 1.316(18) . ?

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
O31 Mo2 O5 105.57(14) . . ?
O31 Mo2 O14 101.51(14) . . ?
O5 Mo2 O14 95.65(12) . . ?
O31 Mo2 O30 99.24(14) . . ?
O5 Mo2 O30 84.54(12) . . ?
O14 Mo2 O30 158.38(12) . . ?
O31 Mo2 O27 97.68(14) . . ?
O5 Mo2 O27 155.63(12) . . ?
O14 Mo2 O27 86.64(11) . . ?
O30 Mo2 O27 84.63(11) . . ?
O31 Mo2 O2 170.52(13) . . ?
O5 Mo2 O2 83.28(11) . . ?
O14 Mo2 O2 80.64(11) . . ?
O30 Mo2 O2 77.90(11) . . ?
O27 Mo2 O2 73.13(11) . . ?
O31 Mo2 Mo1 99.21(11) . . ?
O5 Mo2 Mo1 48.23(9) . . ?
O14 Mo2 Mo1 49.39(8) . . ?
O30 Mo2 Mo1 132.39(9) . . ?
O27 Mo2 Mo1 135.18(8) . . ?
O2 Mo2 Mo1 89.22(7) . . ?
O6 Mo1 O5 105.52(14) . . ?
O6 Mo1 O14 102.12(14) . . ?
O5 Mo1 O14 95.44(12) . . ?
O6 Mo1 O8 96.91(15) . . ?
O5 Mo1 O8 87.12(13) . . ?
O14 Mo1 O8 159.32(12) . . ?
O6 Mo1 O7 97.96(14) . . ?
O5 Mo1 O7 155.66(12) . . ?
O14 Mo1 O7 85.66(11) . . ?
O8 Mo1 O7 83.74(12) . . ?
O6 Mo1 O4 170.80(13) . . ?
O5 Mo1 O4 82.86(11) . . ?
O14 Mo1 O4 80.46(11) . . ?
O8 Mo1 O4 79.50(11) . . ?
O7 Mo1 O4 73.31(11) . . ?
O6 Mo1 Mo2 99.64(11) . . ?
O5 Mo1 Mo2 48.04(8) . . ?
O14 Mo1 Mo2 49.37(8) . . ?
O8 Mo1 Mo2 134.89(10) . . ?
O7 Mo1 Mo2 134.17(8) . . ?
O4 Mo1 Mo2 88.75(7) . . ?
O12 Mo3 O15 105.17(15) . . ?
O12 Mo3 O13 102.14(14) . 2_667 ?
O15 Mo3 O13 95.51(12) . 2_667 ?
O12 Mo3 O11 97.28(14) . . ?
O15 Mo3 O11 85.18(13) . . ?
O13 Mo3 O11 159.64(12) 2_667 . ?
O12 Mo3 O7 97.03(14) . . ?
O15 Mo3 O7 156.87(12) . . ?
O13 Mo3 O7 85.93(11) 2_667 . ?
O11 Mo3 O7 85.67(12) . . ?
O12 Mo3 O4 170.21(13) . . ?
O15 Mo3 O4 83.61(11) . . ?
O13 Mo3 O4 80.97(11) 2_667 . ?
O11 Mo3 O4 78.89(11) . . ?
O7 Mo3 O4 73.80(10) . . ?
O12 Mo3 Mo4 99.83(11) . . ?
O15 Mo3 Mo4 48.36(8) . . ?
O13 Mo3 Mo4 48.96(8) 2_667 . ?
O11 Mo3 Mo4 133.22(9) . . ?
O7 Mo3 Mo4 134.16(8) . . ?
O4 Mo3 Mo4 89.23(7) . . ?
O16 Mo4 O15 105.09(14) . . ?
O16 Mo4 O13 101.76(15) . 2_667 ?
O15 Mo4 O13 95.63(12) . 2_667 ?
O16 Mo4 O17 97.01(15) . . ?
O15 Mo4 O17 86.52(13) . . ?
O13 Mo4 O17 159.81(12) 2_667 . ?
O16 Mo4 O18 98.01(14) . . ?
O15 Mo4 O18 156.02(12) . . ?
O13 Mo4 O18 85.77(11) 2_667 . ?
O17 Mo4 O18 84.31(12) . . ?
O16 Mo4 O3 170.90(13) . . ?
O15 Mo4 O3 83.11(11) . . ?
O13 Mo4 O3 81.03(11) 2_667 . ?
O17 Mo4 O3 79.30(12) . . ?
O18 Mo4 O3 73.44(10) . . ?
O16 Mo4 Mo3 99.48(12) . . ?
O15 Mo4 Mo3 48.29(9) . . ?
O13 Mo4 Mo3 49.15(8) 2_667 . ?
O17 Mo4 Mo3 134.52(9) . . ?
O18 Mo4 Mo3 134.05(8) . . ?
O3 Mo4 Mo3 88.92(7) . . ?
O23 Mo5 O22 105.31(14) 2_667 . ?
O23 Mo5 O24 102.52(14) 2_667 . ?
O22 Mo5 O24 95.57(12) . . ?
O23 Mo5 O21 95.35(14) 2_667 . ?
O22 Mo5 O21 86.52(13) . . ?
O24 Mo5 O21 160.72(12) . . ?
O23 Mo5 O18 97.48(14) 2_667 . ?
O22 Mo5 O18 156.03(12) . . ?
O24 Mo5 O18 86.51(11) . . ?
O21 Mo5 O18 84.03(12) . . ?
O23 Mo5 O3 169.94(13) 2_667 . ?
O22 Mo5 O3 83.12(11) . . ?
O24 Mo5 O3 81.77(11) . . ?
O21 Mo5 O3 79.45(11) . . ?
O18 Mo5 O3 73.53(10) . . ?
O23 Mo5 Mo6 100.63(11) 2_667 . ?
O22 Mo5 Mo6 48.13(9) . . ?
O24 Mo5 Mo6 49.12(8) . . ?
O21 Mo5 Mo6 134.40(10) . . ?
O18 Mo5 Mo6 134.65(8) . . ?
O3 Mo5 Mo6 89.08(7) . . ?
O25 Mo6 O22 105.07(15) . . ?
O25 Mo6 O24 101.93(14) . . ?
O22 Mo6 O24 95.22(12) . . ?
O25 Mo6 O26 96.36(14) . . ?
O22 Mo6 O26 86.98(13) . . ?
O24 Mo6 O26 160.29(12) . . ?
O25 Mo6 O27 97.30(14) . . ?
O22 Mo6 O27 156.88(12) . . ?
O24 Mo6 O27 85.66(11) . . ?
O26 Mo6 O27 84.78(12) . . ?
O25 Mo6 O2 170.42(13) . . ?
O22 Mo6 O2 83.68(11) . . ?
O24 Mo6 O2 80.79(11) . . ?
O26 Mo6 O2 79.99(11) . . ?
O27 Mo6 O2 73.63(10) . . ?
O25 Mo6 Mo5 99.98(11) . . ?
O22 Mo6 Mo5 48.12(9) . . ?
O24 Mo6 Mo5 48.77(8) . . ?
O26 Mo6 Mo5 134.80(9) . . ?
O27 Mo6 Mo5 133.62(8) . . ?
O2 Mo6 Mo5 88.74(7) . . ?
O14 Ni1 O14 180.00(15) . 2_667 ?
O14 Ni1 O24 83.85(10) . 2_667 ?
O14 Ni1 O24 96.15(10) 2_667 2_667 ?
O14 Ni1 O24 96.15(10) . . ?
O14 Ni1 O24 83.85(10) 2_667 . ?
O24 Ni1 O24 180.000(1) 2_667 . ?
O14 Ni1 O13 94.85(10) . 2_667 ?
O14 Ni1 O13 85.15(10) 2_667 2_667 ?
O24 Ni1 O13 83.76(11) 2_667 2_667 ?
O24 Ni1 O13 96.24(11) . 2_667 ?
O14 Ni1 O13 85.15(10) . . ?
O14 Ni1 O13 94.85(10) 2_667 . ?
O24 Ni1 O13 96.24(11) 2_667 . ?
O24 Ni1 O13 83.76(11) . . ?
O13 Ni1 O13 180.000(1) 2_667 . ?
O1 P1 O4 108.92(17) . . ?
O1 P1 O2 110.27(18) . . ?
O4 P1 O2 108.68(16) . . ?
O1 P1 O3 110.08(16) . . ?
O4 P1 O3 109.61(16) . . ?
O2 P1 O3 109.26(16) . . ?
O10 P2 O8 112.07(19) . . ?
O10 P2 O11 112.2(2) . . ?
O8 P2 O11 112.20(17) . . ?
O10 P2 O9 110.2(2) . . ?
O8 P2 O9 106.2(2) . . ?
O11 P2 O9 103.39(19) . . ?
O28 P4 O26 111.04(19) . . ?
O28 P4 O29 110.3(2) . . ?
O26 P4 O29 107.23(17) . . ?
O28 P4 O30 111.15(19) . . ?
O26 P4 O30 111.36(16) . . ?
O29 P4 O30 105.50(18) . . ?
O20 P3 O21 112.3(2) 2_568 . ?
O20 P3 O17 110.7(2) 2_568 . ?
O21 P3 O17 111.67(17) . . ?
O20 P3 O19 107.07(18) 2_568 2_567 ?
O21 P3 O19 107.05(19) . 2_567 ?
O17 P3 O19 107.77(19) . 2_567 ?
P1 O2 Mo6 126.24(15) . . ?
P1 O2 Mo2 126.05(16) . . ?
Mo6 O2 Mo2 99.66(11) . . ?
P1 O4 Mo3 125.60(15) . . ?
P1 O4 Mo1 126.38(16) . . ?
Mo3 O4 Mo1 99.34(11) . . ?
P1 O3 Mo5 125.62(16) . . ?
P1 O3 Mo4 125.70(16) . . ?
Mo5 O3 Mo4 99.58(10) . . ?
P2 O8 Mo1 137.02(18) . . ?
P4 O30 Mo2 134.53(17) . . ?
P3 O17 Mo4 137.63(19) . . ?
P3 O21 Mo5 137.68(19) . . ?
P2 O11 Mo3 135.43(18) . . ?
P4 O26 Mo6 133.85(18) . . ?
Mo6 O27 Mo2 113.00(13) . . ?
Mo5 O18 Mo4 112.87(12) . . ?
Mo5 O22 Mo6 83.74(12) . . ?
Mo2 O5 Mo1 83.73(11) . . ?
Mo3 O7 Mo1 112.97(13) . . ?
C12 N3 C9 108.9(4) . . ?
C12 N3 C8 115.3(4) . . ?
C9 N3 C8 112.7(4) . . ?
C10 N4 C11 112.3(4) . . ?
C2 N1 C3 110.6(4) . . ?
C2 N1 C6 113.1(4) . . ?
C3 N1 C6 110.0(4) . . ?
Mo4 O13 Mo3 81.89(11) 2_667 2_667 ?
Mo4 O13 Ni1 134.47(15) 2_667 . ?
Mo3 O13 Ni1 135.31(14) 2_667 . ?
Mo2 O14 Mo1 81.25(10) . . ?
Mo2 O14 Ni1 134.47(14) . . ?
Mo1 O14 Ni1 136.28(14) . . ?
C1 C2 N1 114.0(5) . . ?
C4 N2 C5 110.7(4) . . ?
N4 C10 C9 110.9(4) . . ?
N1 C3 C4 110.1(4) . . ?
O32B C1 O32A 122.5(9) . . ?
O32B C1 C2 110.0(9) . . ?
O32A C1 C2 115.1(5) . . ?
N3 C9 C10 111.8(4) . . ?
O33B C7 O33A 85.4(9) . . ?
O33B C7 C8 122.3(8) . . ?
O33A C7 C8 116.2(6) . . ?
N1 C6 C5 111.6(4) . . ?
N3 C12 C11 111.5(4) . . ?
N4 C11 C12 110.2(4) . . ?
N2 C4 C3 110.5(5) . . ?
N2 C5 C6 111.0(4) . . ?
C7 C8 N3 113.2(5) . . ?
Mo5 O24 Mo6 82.11(11) . . ?
Mo5 O24 Ni1 134.01(14) . . ?
Mo6 O24 Ni1 135.13(14) . . ?
Mo3 O15 Mo4 83.35(11) . . ?
C15 N5 C14 112.9(7) . . ?
C15 N5 C13 109.9(8) . . ?
C14 N5 C13 110.3(4) . . ?
C14 C13 N5 112.7(6) 2_568 . ?
C13 C14 N5 108.2(5) 2_568 . ?
N5 C15 C16 120.1(11) . . ?
N5 C15 O34A 163.2(11) . . ?
C16 C15 O34A 43.1(8) . . ?
O34A C16 O34B 108.3(13) . . ?
O34A C16 C15 85.2(11) . . ?
O34B C16 C15 116.8(12) . . ?
C16 O34A C15 51.7(8) . . ?

_diffrn_measured_fraction_theta_max 0.992
_diffrn_reflns_theta_full        27.18
_diffrn_measured_fraction_theta_full 0.992
_refine_diff_density_max         2.268
_refine_diff_density_min         -1.886
_refine_diff_density_rms         0.157
####################################################################### 
# 
# 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_shelx
_database_code_depnum_ccdc_archive 'CCDC 1431342'
_audit_update_record             
;
2016-01-13 deposited with the CCDC.
2016-06-06 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 H52 Co Mo5 N4 O35 P2'
_chemical_formula_weight         1413.15

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'
Co Co 0.3494 0.9721 '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   C2/c

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

_cell_length_a                   28.086(4)
_cell_length_b                   9.744(2)
_cell_length_c                   18.685(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 126.780(5)
_cell_angle_gamma                90.00
_cell_volume                     4095.6(12)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    630
_cell_measurement_theta_min      1.81
_cell_measurement_theta_max      32.62

_exptl_crystal_description       Block
_exptl_crystal_colour            Pink
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.25
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.292
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2796
_exptl_absorpt_coefficient_mu    2.072
_exptl_absorpt_correction_type   EMPIRICAL
_exptl_absorpt_correction_T_min  0.456
_exptl_absorpt_correction_T_max  0.596
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      293(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 SMART APEX-II CCD'
_diffrn_measurement_method       ?
_diffrn_standards_number         n/a
_diffrn_standards_interval_count n/a
_diffrn_standards_interval_time  n/a
_diffrn_standards_decay_%        n/a
_diffrn_reflns_number            29665
_diffrn_reflns_av_R_equivalents  0.0753
_diffrn_reflns_av_sigmaI/netI    0.0610
_diffrn_reflns_limit_h_min       -42
_diffrn_reflns_limit_h_max       42
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         1.81
_diffrn_reflns_theta_max         32.62
_reflns_number_total             6300
_reflns_number_gt                4412
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'BRUKER SMART APEX II CCD'
_computing_cell_refinement       'BRUKER SMART APEX II CCD'
_computing_data_reduction        'BRUKER SAINT'
_computing_structure_solution    SHELXS-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Diamond 3.0'
_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)+(0.0413P)²+91.2250P] 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         6300
_refine_ls_number_parameters     311
_refine_ls_number_restraints     14
_refine_ls_R_factor_all          0.0998
_refine_ls_R_factor_gt           0.0619
_refine_ls_wR_factor_ref         0.1545
_refine_ls_wR_factor_gt          0.1285
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_restrained_S_all      1.078
_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 0.5000 0.13504(8) 0.2500 0.02237(17) Uani 1 2 d S . .
Mo2 Mo 0.37971(2) 0.33416(6) 0.16666(3) 0.02236(13) Uani 1 1 d . . .
Mo3 Mo 0.58094(2) 0.66088(6) 0.32146(3) 0.02380(14) Uani 1 1 d . . .
Co1 Co 0.5000 0.0000 0.0000 0.0270(3) Uani 1 2 d S . .
P1 P 0.48939(7) 0.42671(16) 0.13976(10) 0.0202(3) Uani 1 1 d . . .
O8 O 0.54743(19) 0.4657(4) 0.2316(3) 0.0236(9) Uani 1 1 d . . .
O10 O 0.5000 0.7133(6) 0.2500 0.0258(13) Uani 1 2 d S . .
O3 O 0.45571(19) 0.3133(4) 0.1521(3) 0.0233(9) Uani 1 1 d . . .
O1 O 0.4332(2) 0.1914(4) 0.2475(3) 0.0243(9) Uani 1 1 d . . .
O7 O 0.5018(2) 0.3729(5) 0.0763(3) 0.0262(9) Uani 1 1 d . . .
O6 O 0.36321(19) 0.5134(5) 0.1149(3) 0.0263(9) Uani 1 1 d . . .
O4 O 0.3392(2) 0.3416(5) 0.2080(3) 0.0331(11) Uani 1 1 d . . .
O11 O 0.5491(2) 0.5568(4) 0.3959(3) 0.0251(9) Uani 1 1 d . . .
O2 O 0.4672(2) 0.0261(5) 0.1607(3) 0.0325(10) Uani 1 1 d . . .
O15 O 0.4415(2) 0.1436(5) -0.0107(3) 0.0339(11) Uani 1 1 d D . .
O5 O 0.3358(2) 0.2418(5) 0.0697(3) 0.0309(10) Uani 1 1 d . . .
O12 O 0.6137(2) 0.7794(5) 0.4050(3) 0.0324(10) Uani 1 1 d . . .
O9 O 0.5996(2) 0.7187(5) 0.2537(3) 0.0374(12) Uani 1 1 d . . .
O17 O 0.3479(3) 0.0238(6) -0.0117(4) 0.0453(13) Uani 1 1 d D . .
O14 O 0.4287(2) -0.0837(6) -0.1215(3) 0.0344(11) Uani 1 1 d D . .
O16 O 0.1663(2) 0.5826(6) -0.2458(4) 0.0431(13) Uani 1 1 d D . .
O13 O 0.5149(3) 0.1495(6) -0.0679(3) 0.0367(12) Uani 1 1 d D . .
N2 N 0.2854(3) 0.4984(6) -0.1410(4) 0.0312(12) Uani 1 1 d D . .
N1 N 0.4033(3) 0.5918(7) -0.0720(4) 0.0334(13) Uani 1 1 d . . .
C1 C 0.3546(3) 0.6910(8) -0.1056(5) 0.0340(15) Uani 1 1 d . . .
H1A H 0.3357 0.7099 -0.1682 0.041 Uiso 1 1 calc R . .
H1B H 0.3704 0.7765 -0.0728 0.041 Uiso 1 1 calc R . .
C3 C 0.3357(3) 0.4003(8) -0.1067(5) 0.0362(15) Uani 1 1 d . . .
H3A H 0.3204 0.3145 -0.1392 0.043 Uiso 1 1 calc R . .
H3B H 0.3546 0.3815 -0.0440 0.043 Uiso 1 1 calc R . .
C5 C 0.2408(3) 0.4389(9) -0.1296(6) 0.0415(18) Uani 1 1 d . . .
H5B H 0.2248 0.3550 -0.1641 0.050 Uiso 1 1 calc R . .
H5A H 0.2610 0.4155 -0.0672 0.050 Uiso 1 1 calc R . .
C2 C 0.3087(3) 0.6340(8) -0.0949(5) 0.0330(15) Uani 1 1 d . . .
H2B H 0.3267 0.6231 -0.0318 0.040 Uiso 1 1 calc R . .
H2A H 0.2760 0.6984 -0.1198 0.040 Uiso 1 1 calc R . .
C6 C 0.1907(3) 0.5349(9) -0.1584(5) 0.0412(18) Uani 1 1 d . . .
H6B H 0.1604 0.4876 -0.1581 0.049 Uiso 1 1 calc R . .
H6A H 0.2051 0.6118 -0.1174 0.049 Uiso 1 1 calc R . .
C4 C 0.3814(3) 0.4588(8) -0.1172(5) 0.0353(16) Uani 1 1 d . . .
H4A H 0.4144 0.3953 -0.0921 0.042 Uiso 1 1 calc R . .
H4B H 0.3635 0.4700 -0.1802 0.042 Uiso 1 1 calc R . .
O18 O 0.2490(4) 0.4923(12) -0.3139(5) 0.092(3) Uani 1 1 d D . .
H1 H 0.426(6) 0.572(15) -0.013(10) 0.110 Uiso 1 1 d . . .
H16 H 0.149(6) 0.659(8) -0.254(11) 0.138 Uiso 1 1 d D . .
H7 H 0.450(7) 0.223(7) 0.012(10) 0.138 Uiso 1 1 d D . .
H6 H 0.402(5) -0.024(12) -0.155(9) 0.138 Uiso 1 1 d D . .
H8 H 0.418(6) 0.114(16) 0.001(11) 0.138 Uiso 1 1 d D . .
H5 H 0.438(7) -0.139(13) -0.147(10) 0.138 Uiso 1 1 d D . .
H3 H 0.522(7) 0.111(15) -0.101(9) 0.138 Uiso 1 1 d D . .
H4 H 0.490(5) 0.214(11) -0.097(9) 0.138 Uiso 1 1 d D . .
H17A H 0.365(6) -0.052(8) 0.013(10) 0.138 Uiso 1 1 d D . .
H18A H 0.246(8) 0.580(3) -0.317(5) 0.138 Uiso 1 1 d D . .
H17B H 0.338(7) 0.089(11) 0.008(10) 0.138 Uiso 1 1 d D . .
H2N H 0.270(6) 0.515(16) -0.192(3) 0.138 Uiso 1 1 d D . .
H18B H 0.214(3) 0.474(17) -0.360(7) 0.138 Uiso 1 1 d D . .
H1D H 0.430(6) 0.630(14) -0.081(9) 0.110 Uiso 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 O2 1.709(5) . ?
Mo1 O2 1.709(5) 2_655 ?
Mo1 O1 1.929(4) 2_655 ?
Mo1 O1 1.929(4) . ?
Mo1 O3 2.277(4) 2_655 ?
Mo1 O3 2.277(4) . ?
Mo2 O5 1.714(5) . ?
Mo2 O4 1.718(4) . ?
Mo2 O6 1.914(4) . ?
Mo2 O1 1.938(4) . ?
Mo2 O8 2.188(4) 2_655 ?
Mo2 O3 2.316(4) . ?
Mo3 O12 1.703(5) . ?
Mo3 O9 1.729(4) . ?
Mo3 O10 1.8911(18) . ?
Mo3 O6 1.925(5) 2_655 ?
Mo3 O11 2.292(4) . ?
Mo3 O8 2.330(4) . ?
Co1 O15 2.074(5) 5_655 ?
Co1 O15 2.074(5) . ?
Co1 O14 2.094(5) . ?
Co1 O14 2.094(5) 5_655 ?
Co1 O13 2.131(5) . ?
Co1 O13 2.131(5) 5_655 ?
P1 O7 1.515(4) . ?
P1 O11 1.535(5) 2_655 ?
P1 O8 1.548(5) . ?
P1 O3 1.559(4) . ?
O8 Mo2 2.188(4) 2_655 ?
O10 Mo3 1.8911(18) 2_655 ?
O6 Mo3 1.925(5) 2_655 ?
O11 P1 1.535(5) 2_655 ?
O16 C6 1.420(9) . ?
N2 C3 1.494(9) . ?
N2 C2 1.497(9) . ?
N2 C5 1.506(9) . ?
N1 C4 1.466(10) . ?
N1 C1 1.475(10) . ?
C1 C2 1.522(9) . ?
C3 C4 1.522(10) . ?
C5 C6 1.497(11) . ?

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
O2 Mo1 O2 103.2(3) . 2_655 ?
O2 Mo1 O1 98.5(2) . 2_655 ?
O2 Mo1 O1 101.9(2) 2_655 2_655 ?
O2 Mo1 O1 101.9(2) . . ?
O2 Mo1 O1 98.5(2) 2_655 . ?
O1 Mo1 O1 146.9(3) 2_655 . ?
O2 Mo1 O3 166.92(19) . 2_655 ?
O2 Mo1 O3 88.5(2) 2_655 2_655 ?
O1 Mo1 O3 73.00(16) 2_655 2_655 ?
O1 Mo1 O3 81.84(16) . 2_655 ?
O2 Mo1 O3 88.5(2) . . ?
O2 Mo1 O3 166.92(19) 2_655 . ?
O1 Mo1 O3 81.84(16) 2_655 . ?
O1 Mo1 O3 73.00(16) . . ?
O3 Mo1 O3 80.6(2) 2_655 . ?
O5 Mo2 O4 104.3(2) . . ?
O5 Mo2 O6 98.2(2) . . ?
O4 Mo2 O6 99.4(2) . . ?
O5 Mo2 O1 100.2(2) . . ?
O4 Mo2 O1 95.3(2) . . ?
O6 Mo2 O1 152.75(18) . . ?
O5 Mo2 O8 158.85(18) . 2_655 ?
O4 Mo2 O8 96.38(19) . 2_655 ?
O6 Mo2 O8 73.85(18) . 2_655 ?
O1 Mo2 O8 81.85(18) . 2_655 ?
O5 Mo2 O3 87.67(19) . . ?
O4 Mo2 O3 164.1(2) . . ?
O6 Mo2 O3 89.00(16) . . ?
O1 Mo2 O3 71.93(16) . . ?
O8 Mo2 O3 72.87(15) 2_655 . ?
O12 Mo3 O9 102.5(2) . . ?
O12 Mo3 O10 103.0(2) . . ?
O9 Mo3 O10 99.1(2) . . ?
O12 Mo3 O6 98.5(2) . 2_655 ?
O9 Mo3 O6 101.7(2) . 2_655 ?
O10 Mo3 O6 145.9(2) . 2_655 ?
O12 Mo3 O11 86.36(19) . . ?
O9 Mo3 O11 171.1(2) . . ?
O10 Mo3 O11 78.86(15) . . ?
O6 Mo3 O11 76.41(17) 2_655 . ?
O12 Mo3 O8 168.0(2) . . ?
O9 Mo3 O8 84.7(2) . . ?
O10 Mo3 O8 85.14(19) . . ?
O6 Mo3 O8 70.37(17) 2_655 . ?
O11 Mo3 O8 86.58(14) . . ?
O15 Co1 O15 180.0(3) 5_655 . ?
O15 Co1 O14 91.7(2) 5_655 . ?
O15 Co1 O14 88.3(2) . . ?
O15 Co1 O14 88.3(2) 5_655 5_655 ?
O15 Co1 O14 91.7(2) . 5_655 ?
O14 Co1 O14 180.0(6) . 5_655 ?
O15 Co1 O13 95.3(2) 5_655 . ?
O15 Co1 O13 84.7(2) . . ?
O14 Co1 O13 91.3(2) . . ?
O14 Co1 O13 88.7(2) 5_655 . ?
O15 Co1 O13 84.7(2) 5_655 5_655 ?
O15 Co1 O13 95.3(2) . 5_655 ?
O14 Co1 O13 88.7(2) . 5_655 ?
O14 Co1 O13 91.3(2) 5_655 5_655 ?
O13 Co1 O13 180.0(3) . 5_655 ?
O7 P1 O11 112.2(2) . 2_655 ?
O7 P1 O8 111.7(2) . . ?
O11 P1 O8 106.2(2) 2_655 . ?
O7 P1 O3 108.3(2) . . ?
O11 P1 O3 108.6(2) 2_655 . ?
O8 P1 O3 109.9(2) . . ?
P1 O8 Mo2 129.5(3) . 2_655 ?
P1 O8 Mo3 134.6(3) . . ?
Mo2 O8 Mo3 95.04(16) 2_655 . ?
Mo3 O10 Mo3 148.7(4) 2_655 . ?
P1 O3 Mo1 124.9(2) . . ?
P1 O3 Mo2 129.7(2) . . ?
Mo1 O3 Mo2 94.10(14) . . ?
Mo1 O1 Mo2 120.8(2) . . ?
Mo2 O6 Mo3 120.5(2) . 2_655 ?
P1 O11 Mo3 122.1(2) 2_655 . ?
C3 N2 C2 110.0(6) . . ?
C3 N2 C5 110.2(6) . . ?
C2 N2 C5 111.9(6) . . ?
C4 N1 C1 111.8(6) . . ?
N1 C1 C2 110.3(6) . . ?
N2 C3 C4 111.0(6) . . ?
C6 C5 N2 113.1(6) . . ?
N2 C2 C1 111.0(5) . . ?
O16 C6 C5 108.7(6) . . ?
N1 C4 C3 110.6(5) . . ?

_diffrn_measured_fraction_theta_max 0.941
_diffrn_reflns_theta_full        32.62
_diffrn_measured_fraction_theta_full 0.941
_refine_diff_density_max         2.411
_refine_diff_density_min         -1.819
_refine_diff_density_rms         0.232
