# Electronic Supplementary Material (ESI) for Inorganic Chemistry Frontiers.
# This journal is © The Royal Society of Chemistry 2014


#####################################


data_6

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C25 H18 Cl2 Co1 N3 O1'
_chemical_formula_weight         506.21

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'
Cl Cl 0.1484 0.1585 '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'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P21/c

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

_cell_length_a                   9.3416(5)
_cell_length_b                   12.8676(7)
_cell_length_c                   19.8225(11)
_cell_angle_alpha                90.00
_cell_angle_beta                 103.333(3)
_cell_angle_gamma                90.00
_cell_volume                     2318.5(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    4206
_cell_measurement_theta_min      2.70
_cell_measurement_theta_max      26.85

_exptl_crystal_description       thin_plate
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.01
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.450
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1032
_exptl_absorpt_coefficient_mu    0.993
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   'SADABS (Bruker AXS, 2008)'
_exptl_absorpt_correction_T_min  0.961
_exptl_absorpt_correction_T_max  0.997

_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  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            9921
_diffrn_reflns_av_R_equivalents  0.0805
_diffrn_reflns_av_sigmaI/netI    0.0591
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         1.90
_diffrn_reflns_theta_max         24.00
_reflns_number_total             3489
_reflns_number_gt                2567
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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)+(0.0684P)²+0.2392P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    riding
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3489
_refine_ls_number_parameters     289
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0609
_refine_ls_R_factor_gt           0.0432
_refine_ls_wR_factor_ref         0.1284
_refine_ls_wR_factor_gt          0.1145
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_restrained_S_all      1.051
_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
Co1 Co 0.19896(5) 0.18886(4) 0.77343(2) 0.0395(2) Uani 1 1 d . . .
Cl1 Cl 0.41283(10) 0.21382(8) 0.84971(5) 0.0562(3) Uani 1 1 d . . .
Cl2 Cl -0.01257(9) 0.16373(8) 0.69243(5) 0.0516(3) Uani 1 1 d . . .
O1 O 0.1063(3) 0.1577(2) 0.84523(14) 0.0566(7) Uani 1 1 d . . .
N1 N 0.2522(3) 0.0453(2) 0.76381(15) 0.0424(7) Uani 1 1 d . . .
N2 N 0.2957(3) 0.2111(2) 0.70137(15) 0.0394(7) Uani 1 1 d . . .
N3 N 0.1640(3) 0.3321(2) 0.77038(15) 0.0452(8) Uani 1 1 d . . .
C1 C 0.2204(4) -0.0359(3) 0.7984(2) 0.0519(10) Uani 1 1 d . . .
H1A H 0.1699 -0.0259 0.8331 0.062 Uiso 1 1 calc R . .
C2 C 0.2600(4) -0.1342(3) 0.7843(2) 0.0583(11) Uani 1 1 d . . .
H2A H 0.2350 -0.1905 0.8087 0.070 Uiso 1 1 calc R . .
C3 C 0.3374(4) -0.1493(3) 0.7336(2) 0.0585(11) Uani 1 1 d . . .
H3A H 0.3661 -0.2157 0.7238 0.070 Uiso 1 1 calc R . .
C4 C 0.3715(4) -0.0643(3) 0.69784(19) 0.0488(10) Uani 1 1 d . . .
H4A H 0.4240 -0.0724 0.6636 0.059 Uiso 1 1 calc R . .
C5 C 0.3266(3) 0.0326(3) 0.71370(17) 0.0388(9) Uani 1 1 d . . .
C6 C 0.3489(4) 0.1301(3) 0.67810(17) 0.0425(9) Uani 1 1 d . . .
C7 C 0.4216(4) 0.1284(3) 0.61872(17) 0.0423(9) Uani 1 1 d . . .
C8 C 0.3382(4) 0.1350(3) 0.55152(19) 0.0560(11) Uani 1 1 d . . .
H8A H 0.2362 0.1374 0.5433 0.067 Uiso 1 1 calc R . .
C9 C 0.4051(5) 0.1380(4) 0.4972(2) 0.0669(13) Uani 1 1 d . . .
H9A H 0.3485 0.1419 0.4521 0.080 Uiso 1 1 calc R . .
C10 C 0.5542(5) 0.1354(4) 0.5088(2) 0.0695(13) Uani 1 1 d . . .
H10A H 0.5995 0.1406 0.4718 0.083 Uiso 1 1 calc R . .
C11 C 0.6382(4) 0.1250(4) 0.5751(2) 0.0628(12) Uani 1 1 d . . .
H11A H 0.7400 0.1202 0.5829 0.075 Uiso 1 1 calc R . .
C12 C 0.5720(4) 0.1218(3) 0.62971(18) 0.0493(10) Uani 1 1 d . . .
H12A H 0.6290 0.1151 0.6746 0.059 Uiso 1 1 calc R . .
C13 C 0.2953(4) 0.3165(3) 0.68108(18) 0.0422(9) Uani 1 1 d . . .
C14 C 0.3622(4) 0.3602(3) 0.6321(2) 0.0565(11) Uani 1 1 d . . .
H14A H 0.4120 0.3180 0.6070 0.068 Uiso 1 1 calc R . .
C15 C 0.3548(5) 0.4650(4) 0.6207(2) 0.0696(12) Uani 1 1 d . . .
H15A H 0.4035 0.4942 0.5893 0.084 Uiso 1 1 calc R . .
C16 C 0.2774(5) 0.5268(4) 0.6547(2) 0.0691(12) Uani 1 1 d . . .
H16A H 0.2705 0.5976 0.6449 0.083 Uiso 1 1 calc R . .
C17 C 0.2086(4) 0.4871(3) 0.7034(2) 0.0582(11) Uani 1 1 d . . .
H17A H 0.1548 0.5304 0.7259 0.070 Uiso 1 1 calc R . .
C18 C 0.2204(4) 0.3812(3) 0.71863(19) 0.0448(9) Uani 1 1 d . . .
C19 C 0.1000(4) 0.3814(3) 0.81240(19) 0.0492(10) Uani 1 1 d . . .
H19A H 0.0875 0.4527 0.8063 0.059 Uiso 1 1 calc R . .
C20 C 0.0478(4) 0.3350(3) 0.8668(2) 0.0484(10) Uani 1 1 d . . .
C21 C -0.0148(4) 0.4028(4) 0.9082(2) 0.0604(11) Uani 1 1 d . . .
H21A H -0.0202 0.4736 0.8985 0.072 Uiso 1 1 calc R . .
C22 C -0.0673(5) 0.3659(4) 0.9623(3) 0.0737(14) Uani 1 1 d . . .
H22A H -0.1106 0.4111 0.9885 0.088 Uiso 1 1 calc R . .
C23 C -0.0562(5) 0.2614(4) 0.9782(2) 0.0738(14) Uani 1 1 d . . .
H23A H -0.0896 0.2368 1.0160 0.089 Uiso 1 1 calc R . .
C24 C 0.0038(5) 0.1929(4) 0.9389(2) 0.0699(13) Uani 1 1 d . . .
H24A H 0.0108 0.1229 0.9507 0.084 Uiso 1 1 calc R . .
C25 C 0.0548(4) 0.2272(3) 0.88110(19) 0.0484(10) Uani 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
Co1 N3 1.870(3) . ?
Co1 O1 1.872(2) . ?
Co1 N2 1.880(3) . ?
Co1 N1 1.933(3) . ?
Co1 Cl1 2.2333(10) . ?
Co1 Cl2 2.2637(10) . ?
O1 C25 1.301(4) . ?
N1 C1 1.321(5) . ?
N1 C5 1.347(4) . ?
N2 C6 1.285(4) . ?
N2 C13 1.415(4) . ?
N3 C19 1.297(4) . ?
N3 C18 1.407(4) . ?
C1 C2 1.363(5) . ?
C2 C3 1.380(5) . ?
C3 C4 1.381(5) . ?
C4 C5 1.374(5) . ?
C5 C6 1.478(5) . ?
C6 C7 1.489(4) . ?
C7 C12 1.374(5) . ?
C7 C8 1.382(5) . ?
C8 C9 1.364(5) . ?
C9 C10 1.359(5) . ?
C10 C11 1.373(5) . ?
C11 C12 1.365(5) . ?
C13 C14 1.389(5) . ?
C13 C18 1.406(5) . ?
C14 C15 1.367(6) . ?
C15 C16 1.355(6) . ?
C16 C17 1.375(6) . ?
C17 C18 1.395(5) . ?
C19 C20 1.414(5) . ?
C20 C25 1.414(6) . ?
C20 C21 1.415(5) . ?
C21 C22 1.363(6) . ?
C22 C23 1.380(7) . ?
C23 C24 1.378(6) . ?
C24 C25 1.409(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
N3 Co1 O1 97.34(12) . . ?
N3 Co1 N2 86.35(13) . . ?
O1 Co1 N2 176.30(12) . . ?
N3 Co1 N1 170.08(13) . . ?
O1 Co1 N1 92.59(12) . . ?
N2 Co1 N1 83.72(13) . . ?
N3 Co1 Cl1 90.14(9) . . ?
O1 Co1 Cl1 90.82(9) . . ?
N2 Co1 Cl1 88.90(9) . . ?
N1 Co1 Cl1 89.64(9) . . ?
N3 Co1 Cl2 90.03(9) . . ?
O1 Co1 Cl2 91.58(9) . . ?
N2 Co1 Cl2 88.66(9) . . ?
N1 Co1 Cl2 89.77(9) . . ?
Cl1 Co1 Cl2 177.55(4) . . ?
C25 O1 Co1 124.2(3) . . ?
C1 N1 C5 120.1(3) . . ?
C1 N1 Co1 127.7(3) . . ?
C5 N1 Co1 112.2(2) . . ?
C6 N2 C13 130.6(3) . . ?
C6 N2 Co1 116.3(3) . . ?
C13 N2 Co1 113.1(2) . . ?
C19 N3 C18 123.6(4) . . ?
C19 N3 Co1 124.3(3) . . ?
C18 N3 Co1 112.0(2) . . ?
N1 C1 C2 121.6(4) . . ?
C1 C2 C3 119.5(4) . . ?
C2 C3 C4 118.9(4) . . ?
C5 C4 C3 118.8(4) . . ?
N1 C5 C4 121.0(3) . . ?
N1 C5 C6 113.7(3) . . ?
C4 C5 C6 125.2(3) . . ?
N2 C6 C5 114.1(3) . . ?
N2 C6 C7 125.5(3) . . ?
C5 C6 C7 120.4(3) . . ?
C12 C7 C8 119.0(3) . . ?
C12 C7 C6 120.8(3) . . ?
C8 C7 C6 120.2(3) . . ?
C9 C8 C7 120.2(4) . . ?
C10 C9 C8 120.3(4) . . ?
C9 C10 C11 120.1(4) . . ?
C12 C11 C10 119.9(4) . . ?
C11 C12 C7 120.4(3) . . ?
C14 C13 C18 119.3(3) . . ?
C14 C13 N2 127.9(3) . . ?
C18 C13 N2 112.7(3) . . ?
C15 C14 C13 120.1(4) . . ?
C16 C15 C14 120.6(4) . . ?
C15 C16 C17 121.4(4) . . ?
C16 C17 C18 119.2(4) . . ?
C17 C18 N3 125.0(4) . . ?
C17 C18 C13 119.2(4) . . ?
N3 C18 C13 115.8(3) . . ?
N3 C19 C20 125.0(4) . . ?
C19 C20 C25 124.0(3) . . ?
C19 C20 C21 116.4(4) . . ?
C25 C20 C21 119.6(4) . . ?
C22 C21 C20 121.0(5) . . ?
C21 C22 C23 119.8(4) . . ?
C24 C23 C22 120.9(4) . . ?
C23 C24 C25 121.2(5) . . ?
O1 C25 C24 117.8(4) . . ?
O1 C25 C20 124.7(4) . . ?
C24 C25 C20 117.5(4) . . ?

_diffrn_measured_fraction_theta_max 0.960
_diffrn_reflns_theta_full        24.00
_diffrn_measured_fraction_theta_full 0.960
_refine_diff_density_max         0.432
_refine_diff_density_min         -0.549
_refine_diff_density_rms         0.066
_database_code_depnum_ccdc_archive 'CCDC 842402'

data_4

_audit_creation_method           SHELXL-97
_audit_creation_date             2011-03-09
_audit_block_code                WGT-PG-500-06
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_compound_source        methanole
_chemical_formula_moiety         'C33 H35 N3 O2 V, 0.5(C H4 O)'
_chemical_formula_sum            'C33.50 H37 N3 O2.50 V'
_chemical_formula_weight         572.60

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'
V V 0.3005 0.5294 '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                   9.340(3)
_cell_length_b                   11.616(7)
_cell_length_c                   13.836(4)
_cell_angle_alpha                76.22(5)
_cell_angle_beta                 83.19(5)
_cell_angle_gamma                88.86(5)
_cell_volume                     1447.6(11)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    21602
_cell_measurement_theta_min      2.6297
_cell_measurement_theta_max      31.8945

loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0.00 -1.00 1.00 0.0350
0.00 1.00 -1.00 0.0350
1.00 0.00 0.00 0.0500
-1.00 0.00 0.00 0.0700
0.00 -1.00 -1.00 0.0800
0.00 1.00 1.00 0.0800
-2.00 -1.00 -1.00 0.0700
-1.00 -3.00 -3.00 0.0700
0.00 0.00 -1.00 0.0400
0.00 0.00 1.00 0.0700
0.00 1.00 0.00 0.0500


_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.07
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.314
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             604
_exptl_absorpt_coefficient_mu    0.380
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   'SADABS (Bruker AXS, 2008)'
_exptl_absorpt_correction_T_min  0.95674
_exptl_absorpt_correction_T_max  0.97759

_exptl_special_details           
; 
 The minimum and maximum estimated transmissions from the multi-scan
 scaling are 0.6684 and 1.0000 (SADABS).

 Crystal mounted on a MiTeGen loop using Perfluoropolyether PFO-XR75
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         '0.2 x 2mm^2^ focus rotating anode'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker AXS Enraf-Nonius KappaCCD'
_diffrn_measurement_method       'CCD φ- and ω-scans'
_diffrn_detector_area_resol_mean 18.02
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            18275
_diffrn_reflns_av_R_equivalents  0.0620
_diffrn_reflns_av_sigmaI/netI    0.0929
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         2.63
_diffrn_reflns_theta_max         30.00
_reflns_number_total             8372
_reflns_number_gt                5603
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'DATCOL (Bruker AXS, 2006)'
_computing_cell_refinement       'DENZO (Bruker AXS, 2006)'
_computing_data_reduction        'DENZO (Bruker AXS, 2006)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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)+(0.0661P)²+1.0490P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         8372
_refine_ls_number_parameters     378
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1118
_refine_ls_R_factor_gt           0.0682
_refine_ls_wR_factor_ref         0.1707
_refine_ls_wR_factor_gt          0.1469
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_restrained_S_all      1.036
_refine_ls_shift/su_max          0.000
_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
V1 V -0.16252(5) 0.78375(4) 0.50714(3) 0.02150(13) Uani 1 1 d . . .
O1 O -0.10844(19) 0.79128(16) 0.36708(13) 0.0223(4) Uani 1 1 d . . .
C2 C -0.0249(3) 0.7218(2) 0.32063(18) 0.0203(5) Uani 1 1 d . . .
C3 C -0.0334(3) 0.7285(2) 0.21653(18) 0.0217(5) Uani 1 1 d . . .
C4 C 0.0701(3) 0.6684(2) 0.16791(18) 0.0228(5) Uani 1 1 d . . .
H4 H 0.0661 0.6743 0.0986 0.027 Uiso 1 1 calc R . .
C5 C 0.1807(3) 0.5991(2) 0.21292(19) 0.0209(5) Uani 1 1 d . . .
C6 C 0.1800(3) 0.5855(2) 0.31481(18) 0.0217(5) Uani 1 1 d . . .
H6 H 0.2493 0.5356 0.3488 0.026 Uiso 1 1 calc R . .
C7 C 0.0774(3) 0.6448(2) 0.37004(18) 0.0201(5) Uani 1 1 d . . .
C8 C 0.0957(3) 0.6323(2) 0.47350(18) 0.0211(5) Uani 1 1 d . . .
H8 H 0.1736 0.5850 0.4982 0.025 Uiso 1 1 calc R . .
N9 N 0.0148(2) 0.68000(19) 0.53669(15) 0.0205(4) Uani 1 1 d . . .
C10 C 0.0562(3) 0.6798(2) 0.63278(18) 0.0210(5) Uani 1 1 d . . .
C11 C 0.1436(3) 0.5964(2) 0.68738(19) 0.0230(5) Uani 1 1 d . . .
H11 H 0.1765 0.5292 0.6635 0.028 Uiso 1 1 calc R . .
C12 C 0.1823(3) 0.6129(3) 0.7775(2) 0.0268(6) Uani 1 1 d . . .
H12 H 0.2412 0.5564 0.8157 0.032 Uiso 1 1 calc R . .
C13 C 0.1347(3) 0.7117(3) 0.8113(2) 0.0274(6) Uani 1 1 d . . .
H13 H 0.1635 0.7230 0.8720 0.033 Uiso 1 1 calc R . .
C14 C 0.0454(3) 0.7948(3) 0.75805(19) 0.0251(6) Uani 1 1 d . . .
H14 H 0.0137 0.8619 0.7825 0.030 Uiso 1 1 calc R . .
C15 C 0.0026(3) 0.7790(2) 0.66824(19) 0.0218(5) Uani 1 1 d . . .
N16 N -0.0865(2) 0.8512(2) 0.60719(16) 0.0235(5) Uani 1 1 d . . .
C17 C -0.1411(3) 0.9609(2) 0.62911(19) 0.0230(5) Uani 1 1 d . . .
H17 H -0.0577 1.0135 0.6293 0.028 Uiso 1 1 calc R . .
C18 C -0.2279(3) 1.0198(2) 0.54454(19) 0.0253(6) Uani 1 1 d . . .
C19 C -0.2927(3) 1.1297(3) 0.5389(2) 0.0287(6) Uani 1 1 d . . .
H19 H -0.2827 1.1722 0.5885 0.034 Uiso 1 1 calc R . .
C20 C -0.3716(3) 1.1763(3) 0.4608(2) 0.0328(7) Uani 1 1 d . . .
H20 H -0.4151 1.2518 0.4553 0.039 Uiso 1 1 calc R . .
C21 C -0.3868(3) 1.1116(3) 0.3901(2) 0.0334(7) Uani 1 1 d . . .
H21 H -0.4409 1.1421 0.3358 0.040 Uiso 1 1 calc R . .
C22 C -0.3221(3) 1.0027(3) 0.4001(2) 0.0290(6) Uani 1 1 d . . .
H22 H -0.3328 0.9582 0.3519 0.035 Uiso 1 1 calc R . .
N23 N -0.2440(2) 0.9568(2) 0.47625(16) 0.0248(5) Uani 1 1 d . . .
C24 C -0.1522(3) 0.8000(2) 0.1616(2) 0.0264(6) Uani 1 1 d . . .
C25 C -0.1321(3) 0.9327(2) 0.1547(2) 0.0292(6) Uani 1 1 d . . .
H25A H -0.1317 0.9455 0.2222 0.044 Uiso 1 1 calc R . .
H25B H -0.2115 0.9771 0.1231 0.044 Uiso 1 1 calc R . .
H25C H -0.0403 0.9603 0.1145 0.044 Uiso 1 1 calc R . .
C26 C -0.3015(3) 0.7568(3) 0.2170(2) 0.0344(7) Uani 1 1 d . . .
H26A H -0.3151 0.6734 0.2171 0.052 Uiso 1 1 calc R . .
H26B H -0.3767 0.8045 0.1830 0.052 Uiso 1 1 calc R . .
H26C H -0.3077 0.7651 0.2862 0.052 Uiso 1 1 calc R . .
C27 C -0.1474(4) 0.7843(3) 0.0537(2) 0.0414(8) Uani 1 1 d . . .
H27A H -0.0558 0.8155 0.0152 0.062 Uiso 1 1 calc R . .
H27B H -0.2275 0.8274 0.0220 0.062 Uiso 1 1 calc R . .
H27C H -0.1560 0.6999 0.0553 0.062 Uiso 1 1 calc R . .
C28 C 0.2934(3) 0.5426(2) 0.14886(18) 0.0232(5) Uani 1 1 d . . .
C29 C 0.4073(3) 0.4747(3) 0.2101(2) 0.0274(6) Uani 1 1 d . . .
H29A H 0.4586 0.5294 0.2384 0.041 Uiso 1 1 calc R . .
H29B H 0.4760 0.4391 0.1667 0.041 Uiso 1 1 calc R . .
H29C H 0.3604 0.4122 0.2645 0.041 Uiso 1 1 calc R . .
C30 C 0.2179(3) 0.4567(3) 0.1010(2) 0.0305(6) Uani 1 1 d . . .
H30A H 0.1678 0.3943 0.1539 0.046 Uiso 1 1 calc R . .
H30B H 0.2900 0.4210 0.0599 0.046 Uiso 1 1 calc R . .
H30C H 0.1480 0.5004 0.0589 0.046 Uiso 1 1 calc R . .
C31 C 0.3708(3) 0.6406(3) 0.0652(2) 0.0301(6) Uani 1 1 d . . .
H31A H 0.2998 0.6854 0.0246 0.045 Uiso 1 1 calc R . .
H31B H 0.4406 0.6047 0.0226 0.045 Uiso 1 1 calc R . .
H31C H 0.4213 0.6942 0.0950 0.045 Uiso 1 1 calc R . .
C32 C -0.2398(3) 0.9483(2) 0.72735(19) 0.0233(5) Uani 1 1 d . . .
C33 C -0.2470(3) 1.0373(3) 0.7789(2) 0.0282(6) Uani 1 1 d . . .
H33 H -0.1825 1.1030 0.7570 0.034 Uiso 1 1 calc R . .
C34 C -0.3482(3) 1.0311(3) 0.8624(2) 0.0329(7) Uani 1 1 d . . .
H34 H -0.3534 1.0929 0.8970 0.039 Uiso 1 1 calc R . .
C35 C -0.4409(3) 0.9349(3) 0.8949(2) 0.0320(7) Uani 1 1 d . . .
H35 H -0.5113 0.9314 0.9511 0.038 Uiso 1 1 calc R . .
C36 C -0.4318(3) 0.8441(3) 0.8463(2) 0.0278(6) Uani 1 1 d . . .
H36 H -0.4944 0.7773 0.8699 0.033 Uiso 1 1 calc R . .
C37 C -0.3309(3) 0.8497(3) 0.7625(2) 0.0260(6) Uani 1 1 d . . .
H37 H -0.3241 0.7866 0.7295 0.031 Uiso 1 1 calc R . .
O40 O -0.3018(2) 0.69976(18) 0.55151(14) 0.0289(4) Uani 1 1 d . . .
O50 O -0.4000(10) 0.5231(8) 0.4702(6) 0.086(2) Uani 0.50 1 d P . .
H50 H -0.3673 0.5792 0.4901 0.128 Uiso 0.50 1 calc PR . .
C51 C -0.5009(14) 0.4635(9) 0.5407(9) 0.069(3) Uani 0.50 1 d P . .
H51A H -0.4543 0.4045 0.5901 0.103 Uiso 0.50 1 calc PR . .
H51B H -0.5672 0.4234 0.5093 0.103 Uiso 0.50 1 calc PR . .
H51C H -0.5549 0.5191 0.5743 0.103 Uiso 0.50 1 calc PR . .


_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
V1 O40 1.612(2) . ?
V1 O1 1.9254(18) . ?
V1 N16 1.950(2) . ?
V1 N9 2.052(2) . ?
V1 N23 2.099(3) . ?
O1 C2 1.332(3) . ?
C2 C7 1.418(4) . ?
C2 C3 1.435(3) . ?
C3 C4 1.384(4) . ?
C3 C24 1.537(4) . ?
C4 C5 1.409(4) . ?
C5 C6 1.380(3) . ?
C5 C28 1.533(3) . ?
C6 C7 1.424(3) . ?
C7 C8 1.434(3) . ?
C8 N9 1.303(3) . ?
N9 C10 1.427(3) . ?
C10 C11 1.394(4) . ?
C10 C15 1.416(4) . ?
C11 C12 1.395(4) . ?
C12 C13 1.385(4) . ?
C13 C14 1.395(4) . ?
C14 C15 1.403(4) . ?
C15 N16 1.382(3) . ?
N16 C17 1.448(3) . ?
C17 C18 1.522(4) . ?
C17 C32 1.528(3) . ?
C18 N23 1.349(4) . ?
C18 C19 1.390(4) . ?
C19 C20 1.378(4) . ?
C20 C21 1.388(5) . ?
C21 C22 1.375(4) . ?
C22 N23 1.352(4) . ?
C24 C25 1.536(4) . ?
C24 C26 1.541(4) . ?
C24 C27 1.542(4) . ?
C28 C29 1.528(4) . ?
C28 C31 1.538(4) . ?
C28 C30 1.544(4) . ?
C32 C33 1.385(4) . ?
C32 C37 1.395(4) . ?
C33 C34 1.392(4) . ?
C34 C35 1.382(4) . ?
C35 C36 1.376(4) . ?
C36 C37 1.394(4) . ?
O50 C51 1.344(12) . ?

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
O40 V1 O1 111.66(11) . . ?
O40 V1 N16 113.24(10) . . ?
O1 V1 N16 135.08(9) . . ?
O40 V1 N9 106.57(11) . . ?
O1 V1 N9 87.99(9) . . ?
N16 V1 N9 78.59(10) . . ?
O40 V1 N23 104.85(11) . . ?
O1 V1 N23 92.11(10) . . ?
N16 V1 N23 77.58(11) . . ?
N9 V1 N23 146.09(10) . . ?
C2 O1 V1 131.61(17) . . ?
O1 C2 C7 121.8(2) . . ?
O1 C2 C3 119.5(2) . . ?
C7 C2 C3 118.7(2) . . ?
C4 C3 C2 117.3(2) . . ?
C4 C3 C24 121.6(2) . . ?
C2 C3 C24 121.1(2) . . ?
C3 C4 C5 125.3(2) . . ?
C6 C5 C4 116.7(2) . . ?
C6 C5 C28 123.5(2) . . ?
C4 C5 C28 119.8(2) . . ?
C5 C6 C7 121.3(2) . . ?
C2 C7 C6 120.4(2) . . ?
C2 C7 C8 123.2(2) . . ?
C6 C7 C8 116.0(2) . . ?
N9 C8 C7 125.8(2) . . ?
C8 N9 C10 121.4(2) . . ?
C8 N9 V1 126.38(18) . . ?
C10 N9 V1 111.53(16) . . ?
C11 C10 C15 121.4(2) . . ?
C11 C10 N9 126.1(2) . . ?
C15 C10 N9 112.5(2) . . ?
C10 C11 C12 119.2(3) . . ?
C13 C12 C11 119.9(3) . . ?
C12 C13 C14 121.4(3) . . ?
C13 C14 C15 119.7(3) . . ?
N16 C15 C14 127.3(2) . . ?
N16 C15 C10 114.4(2) . . ?
C14 C15 C10 118.3(2) . . ?
C15 N16 C17 121.0(2) . . ?
C15 N16 V1 116.27(18) . . ?
C17 N16 V1 121.71(18) . . ?
N16 C17 C18 106.9(2) . . ?
N16 C17 C32 115.7(2) . . ?
C18 C17 C32 107.3(2) . . ?
N23 C18 C19 121.1(3) . . ?
N23 C18 C17 115.9(2) . . ?
C19 C18 C17 122.9(3) . . ?
C20 C19 C18 119.4(3) . . ?
C19 C20 C21 119.3(3) . . ?
C22 C21 C20 118.9(3) . . ?
N23 C22 C21 122.1(3) . . ?
C18 N23 C22 119.2(3) . . ?
C18 N23 V1 115.83(19) . . ?
C22 N23 V1 124.7(2) . . ?
C25 C24 C3 110.1(2) . . ?
C25 C24 C26 110.5(2) . . ?
C3 C24 C26 109.8(2) . . ?
C25 C24 C27 107.4(2) . . ?
C3 C24 C27 111.5(2) . . ?
C26 C24 C27 107.5(3) . . ?
C29 C28 C5 112.2(2) . . ?
C29 C28 C31 107.9(2) . . ?
C5 C28 C31 109.2(2) . . ?
C29 C28 C30 108.9(2) . . ?
C5 C28 C30 109.6(2) . . ?
C31 C28 C30 109.0(2) . . ?
C33 C32 C37 119.3(2) . . ?
C33 C32 C17 120.8(2) . . ?
C37 C32 C17 119.8(2) . . ?
C32 C33 C34 120.5(3) . . ?
C35 C34 C33 119.8(3) . . ?
C36 C35 C34 120.3(3) . . ?
C35 C36 C37 120.2(3) . . ?
C36 C37 C32 119.9(3) . . ?

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
O50 H50 O40 0.84 1.94 2.781(9) 173.4 .

_diffrn_measured_fraction_theta_max 0.991
_diffrn_reflns_theta_full        30.00
_diffrn_measured_fraction_theta_full 0.991
_refine_diff_density_max         0.852
_refine_diff_density_min         -0.715
_refine_diff_density_rms         0.085
_database_code_depnum_ccdc_archive 'CCDC 972492'

#############################


data_5

_audit_creation_method           SHELXL-97
_audit_creation_date             2012-08-22
_audit_block_code                FNG-PG-506-88
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_compound_source        'dichloromethane, hexane'
_chemical_formula_moiety         'C25 H19 Mo N3 O3'
_chemical_formula_sum            'C25 H19 Mo N3 O3'
_chemical_formula_weight         505.37

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           Triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_Int_Tables_number      2

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

_cell_length_a                   7.9292(2)
_cell_length_b                   11.4808(6)
_cell_length_c                   11.7269(9)
_cell_angle_alpha                76.524(4)
_cell_angle_beta                 83.276(5)
_cell_angle_gamma                81.837(3)
_cell_volume                     1023.71(10)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    18351
_cell_measurement_theta_min      2.6021
_cell_measurement_theta_max      33.1

loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0.00 0.00 1.00 0.0400
0.00 0.00 -1.00 0.0400
0.00 -1.00 0.00 0.0600
0.00 1.00 0.00 0.0600
-1.00 0.00 0.00 0.1300
1.00 0.00 0.00 0.1400
-2.00 0.00 -1.00 0.1200

_exptl_crystal_description       prism
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.640
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             512
_exptl_absorpt_coefficient_mu    0.675
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   'SADABS (Bruker AXS, 2008)'
_exptl_absorpt_correction_T_min  0.87712
_exptl_absorpt_correction_T_max  0.95069

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         '0.2 x 2mm^2^ focus rotating anode'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker AXS Enraf-Nonius KappaCCD'
_diffrn_measurement_method       'CCD φ- and ω-scans'
_diffrn_detector_area_resol_mean 18.02
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            15702
_diffrn_reflns_av_R_equivalents  0.0232
_diffrn_reflns_av_sigmaI/netI    0.0280
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         3.00
_diffrn_reflns_theta_max         31.00
_reflns_number_total             6499
_reflns_number_gt                6061
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'DATCOL (Bruker AXS, 2006)'
_computing_cell_refinement       'DENZO (Bruker AXS, 2006)'
_computing_data_reduction        'DENZO (Bruker AXS, 2006)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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)+(0.0343P)²+0.7181P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6499
_refine_ls_number_parameters     289
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0293
_refine_ls_R_factor_gt           0.0263
_refine_ls_wR_factor_ref         0.0696
_refine_ls_wR_factor_gt          0.0675
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_restrained_S_all      1.059
_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
Mo Mo 0.118869(14) 0.135244(10) 0.203729(10) 0.01138(4) Uani 1 1 d . . .
O1 O 0.10084(14) -0.03482(10) 0.20692(10) 0.0159(2) Uani 1 1 d . . .
C2 C 0.10983(18) -0.14039(13) 0.28534(14) 0.0153(3) Uani 1 1 d . . .
C3 C 0.0691(2) -0.24034(15) 0.24901(15) 0.0194(3) Uani 1 1 d . . .
H3 H 0.0366 -0.2311 0.1717 0.023 Uiso 1 1 calc R . .
C4 C 0.0762(2) -0.35286(15) 0.32600(17) 0.0241(3) Uani 1 1 d . . .
H4 H 0.0485 -0.4201 0.3008 0.029 Uiso 1 1 calc R . .
C5 C 0.1237(2) -0.36794(15) 0.43996(17) 0.0253(3) Uani 1 1 d . . .
H5 H 0.1271 -0.4449 0.4923 0.030 Uiso 1 1 calc R . .
C6 C 0.1655(2) -0.27047(14) 0.47596(15) 0.0209(3) Uani 1 1 d . . .
H6 H 0.1980 -0.2811 0.5535 0.025 Uiso 1 1 calc R . .
C7 C 0.16100(19) -0.15507(13) 0.39992(14) 0.0158(3) Uani 1 1 d . . .
C8 C 0.21232(19) -0.05937(14) 0.44461(13) 0.0157(3) Uani 1 1 d . . .
H8 H 0.2457 -0.0785 0.5227 0.019 Uiso 1 1 calc R . .
N9 N 0.21569(16) 0.05050(11) 0.38521(11) 0.0136(2) Uani 1 1 d . . .
C10 C 0.27011(18) 0.14099(13) 0.43212(13) 0.0141(3) Uani 1 1 d . . .
C11 C 0.2970(2) 0.13096(15) 0.55042(14) 0.0187(3) Uani 1 1 d . . .
H11 H 0.2769 0.0594 0.6074 0.022 Uiso 1 1 calc R . .
C12 C 0.3531(2) 0.22638(16) 0.58349(14) 0.0214(3) Uani 1 1 d . . .
H12 H 0.3724 0.2199 0.6633 0.026 Uiso 1 1 calc R . .
C13 C 0.3813(2) 0.33185(15) 0.49998(15) 0.0210(3) Uani 1 1 d . . .
H13 H 0.4213 0.3963 0.5232 0.025 Uiso 1 1 calc R . .
C14 C 0.3516(2) 0.34350(14) 0.38339(14) 0.0175(3) Uani 1 1 d . . .
H14 H 0.3698 0.4161 0.3275 0.021 Uiso 1 1 calc R . .
C15 C 0.29493(18) 0.24859(13) 0.34796(13) 0.0133(2) Uani 1 1 d . . .
N16 N 0.26189(16) 0.25735(11) 0.23040(11) 0.0129(2) Uani 1 1 d . . .
C17 C 0.41060(18) 0.28296(13) 0.14379(13) 0.0132(2) Uani 1 1 d . . .
H17 H 0.4876 0.3246 0.1786 0.016 Uiso 1 1 calc R . .
C18 C 0.50651(18) 0.16279(13) 0.12901(13) 0.0133(2) Uani 1 1 d . . .
C19 C 0.67969(19) 0.14592(15) 0.09358(14) 0.0172(3) Uani 1 1 d . . .
H19 H 0.7459 0.2117 0.0755 0.021 Uiso 1 1 calc R . .
C20 C 0.75410(19) 0.03108(15) 0.08513(14) 0.0178(3) Uani 1 1 d . . .
H20 H 0.8720 0.0174 0.0598 0.021 Uiso 1 1 calc R . .
C21 C 0.65486(19) -0.06373(14) 0.11402(13) 0.0160(3) Uani 1 1 d . . .
H21 H 0.7042 -0.1434 0.1108 0.019 Uiso 1 1 calc R . .
C22 C 0.48289(19) -0.03975(13) 0.14747(13) 0.0142(3) Uani 1 1 d . . .
H22 H 0.4142 -0.1042 0.1661 0.017 Uiso 1 1 calc R . .
N23 N 0.40950(16) 0.07130(11) 0.15459(11) 0.0126(2) Uani 1 1 d . . .
C24 C 0.35980(19) 0.36625(13) 0.02807(13) 0.0154(3) Uani 1 1 d . . .
C25 C 0.2383(2) 0.46567(15) 0.03171(16) 0.0208(3) Uani 1 1 d . . .
H25 H 0.1880 0.4797 0.1056 0.025 Uiso 1 1 calc R . .
C26 C 0.1892(2) 0.54498(16) -0.07138(17) 0.0261(4) Uani 1 1 d . . .
H26 H 0.1056 0.6122 -0.0671 0.031 Uiso 1 1 calc R . .
C27 C 0.2614(3) 0.52650(17) -0.18011(17) 0.0289(4) Uani 1 1 d . . .
H27 H 0.2264 0.5799 -0.2504 0.035 Uiso 1 1 calc R . .
C28 C 0.3852(3) 0.42941(17) -0.18510(15) 0.0268(4) Uani 1 1 d . . .
H28 H 0.4361 0.4164 -0.2593 0.032 Uiso 1 1 calc R . .
C29 C 0.4357(2) 0.35028(15) -0.08158(14) 0.0204(3) Uani 1 1 d . . .
H29 H 0.5225 0.2850 -0.0860 0.025 Uiso 1 1 calc R . .
O30 O 0.09654(14) 0.19180(10) 0.05630(10) 0.0152(2) Uani 1 1 d . . .
O40 O -0.06937(14) 0.17707(11) 0.27899(10) 0.0174(2) Uani 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
Mo O40 1.7096(11) . ?
Mo O30 1.7198(11) . ?
Mo O1 1.9692(11) . ?
Mo N16 2.0219(12) . ?
Mo N9 2.2958(13) . ?
Mo N23 2.3637(12) . ?
O1 C2 1.3383(18) . ?
C2 C3 1.403(2) . ?
C2 C7 1.415(2) . ?
C3 C4 1.391(2) . ?
C4 C5 1.396(3) . ?
C5 C6 1.378(2) . ?
C6 C7 1.413(2) . ?
C7 C8 1.447(2) . ?
C8 N9 1.2934(19) . ?
N9 C10 1.4204(19) . ?
C10 C11 1.404(2) . ?
C10 C15 1.412(2) . ?
C11 C12 1.388(2) . ?
C12 C13 1.396(2) . ?
C13 C14 1.387(2) . ?
C14 C15 1.398(2) . ?
C15 N16 1.4112(19) . ?
N16 C17 1.4789(18) . ?
C17 C18 1.515(2) . ?
C17 C24 1.527(2) . ?
C18 N23 1.3467(18) . ?
C18 C19 1.387(2) . ?
C19 C20 1.387(2) . ?
C20 C21 1.388(2) . ?
C21 C22 1.381(2) . ?
C22 N23 1.3412(19) . ?
C24 C25 1.391(2) . ?
C24 C29 1.395(2) . ?
C25 C26 1.392(2) . ?
C26 C27 1.385(3) . ?
C27 C28 1.384(3) . ?
C28 C29 1.399(2) . ?

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
O40 Mo O30 107.32(5) . . ?
O40 Mo O1 102.10(5) . . ?
O30 Mo O1 97.65(5) . . ?
O40 Mo N16 99.62(5) . . ?
O30 Mo N16 98.53(5) . . ?
O1 Mo N16 147.57(5) . . ?
O40 Mo N9 86.07(5) . . ?
O30 Mo N9 166.38(5) . . ?
O1 Mo N9 81.51(5) . . ?
N16 Mo N9 76.25(5) . . ?
O40 Mo N23 163.00(5) . . ?
O30 Mo N23 88.64(5) . . ?
O1 Mo N23 80.93(4) . . ?
N16 Mo N23 71.57(5) . . ?
N9 Mo N23 77.79(4) . . ?
C2 O1 Mo 137.77(10) . . ?
O1 C2 C3 117.12(14) . . ?
O1 C2 C7 123.20(14) . . ?
C3 C2 C7 119.66(14) . . ?
C4 C3 C2 120.13(16) . . ?
C3 C4 C5 120.67(16) . . ?
C6 C5 C4 119.56(16) . . ?
C5 C6 C7 121.35(16) . . ?
C6 C7 C2 118.61(14) . . ?
C6 C7 C8 117.19(14) . . ?
C2 C7 C8 124.20(14) . . ?
N9 C8 C7 124.24(14) . . ?
C8 N9 C10 122.22(13) . . ?
C8 N9 Mo 128.00(11) . . ?
C10 N9 Mo 109.57(9) . . ?
C11 C10 C15 120.37(14) . . ?
C11 C10 N9 125.74(14) . . ?
C15 C10 N9 113.89(13) . . ?
C12 C11 C10 119.46(15) . . ?
C11 C12 C13 120.27(15) . . ?
C14 C13 C12 120.64(15) . . ?
C13 C14 C15 120.13(15) . . ?
C14 C15 N16 121.82(13) . . ?
C14 C15 C10 119.10(14) . . ?
N16 C15 C10 119.08(13) . . ?
C15 N16 C17 114.01(11) . . ?
C15 N16 Mo 116.18(9) . . ?
C17 N16 Mo 116.02(9) . . ?
N16 C17 C18 107.35(11) . . ?
N16 C17 C24 112.63(12) . . ?
C18 C17 C24 113.52(12) . . ?
N23 C18 C19 121.91(14) . . ?
N23 C18 C17 114.24(12) . . ?
C19 C18 C17 123.84(13) . . ?
C20 C19 C18 118.61(14) . . ?
C19 C20 C21 119.47(14) . . ?
C22 C21 C20 118.61(14) . . ?
N23 C22 C21 122.29(14) . . ?
C22 N23 C18 119.09(13) . . ?
C22 N23 Mo 128.44(10) . . ?
C18 N23 Mo 112.45(9) . . ?
C25 C24 C29 118.20(15) . . ?
C25 C24 C17 118.87(14) . . ?
C29 C24 C17 122.86(14) . . ?
C24 C25 C26 121.00(17) . . ?
C27 C26 C25 120.44(17) . . ?
C28 C27 C26 119.24(16) . . ?
C27 C28 C29 120.37(17) . . ?
C24 C29 C28 120.70(17) . . ?

_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_theta_full        31.00
_diffrn_measured_fraction_theta_full 0.995
_refine_diff_density_max         0.729
_refine_diff_density_min         -1.406
_refine_diff_density_rms         0.081
_database_code_depnum_ccdc_archive 'CCDC 972493'
