# 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 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_3
_database_code_depnum_ccdc_archive 'CCDC 1054804'
_audit_update_record             
;
2015-08-24 deposited with the CCDC.
2015-08-26 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C42 H32 Br2 Cl6 Mo2 N8 O6 S4'
_chemical_formula_weight         1437.38

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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 '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'
Cl Cl 0.1484 0.1585 '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                   11.1658(5)
_cell_length_b                   11.1797(5)
_cell_length_c                   13.1399(6)
_cell_angle_alpha                67.8630(10)
_cell_angle_beta                 65.7240(10)
_cell_angle_gamma                67.0800(10)
_cell_volume                     1330.51(10)
_cell_formula_units_Z            1
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    3254
_cell_measurement_theta_min      2.48
_cell_measurement_theta_max      22.93

_exptl_crystal_description       rectangular
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.16
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.794
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             708
_exptl_absorpt_coefficient_mu    2.484
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.636
_exptl_absorpt_correction_T_max  0.692
_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  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            15685
_diffrn_reflns_av_R_equivalents  0.0425
_diffrn_reflns_av_sigmaI/netI    0.0467
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         1.76
_diffrn_reflns_theta_max         25.50
_reflns_number_total             4959
_reflns_number_gt                3683
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_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. 

 distance constraints were applied to the disordered solvent molecules
;


_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)+(0.0687P)²+2.9000P] 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         4875
_refine_ls_number_parameters     343
_refine_ls_number_restraints     12
_refine_ls_R_factor_all          0.0634
_refine_ls_R_factor_gt           0.0416
_refine_ls_wR_factor_ref         0.1219
_refine_ls_wR_factor_gt          0.1037
_refine_ls_goodness_of_fit_ref   0.882
_refine_ls_restrained_S_all      0.885
_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
Br1 Br 0.53878(6) 0.25350(7) 1.32917(5) 0.0661(2) Uani 1 1 d . . .
C1 C 0.6720(5) 0.0456(5) 1.0367(4) 0.0380(11) Uani 1 1 d . . .
C2 C 0.5535(5) 0.0362(6) 1.1274(4) 0.0500(13) Uani 1 1 d . . .
H2 H 0.4995 -0.0107 1.1293 0.060 Uiso 1 1 calc R . .
C3 C 0.5138(5) 0.0956(6) 1.2159(5) 0.0507(13) Uani 1 1 d . . .
H3 H 0.4326 0.0906 1.2758 0.061 Uiso 1 1 calc R . .
C4 C 0.5969(5) 0.1627(5) 1.2140(4) 0.0459(12) Uani 1 1 d . . .
C5 C 0.7164(5) 0.1707(5) 1.1273(4) 0.0451(12) Uani 1 1 d . . .
H5 H 0.7713 0.2147 1.1282 0.054 Uiso 1 1 calc R . .
C6 C 0.7567(5) 0.1120(5) 1.0360(4) 0.0370(10) Uani 1 1 d . . .
C7 C 0.8797(5) 0.1340(5) 0.9419(4) 0.0378(11) Uani 1 1 d . . .
H7 H 0.9252 0.1841 0.9478 0.045 Uiso 1 1 calc R . .
C8 C 1.1010(5) 0.0881(5) 0.6830(4) 0.0415(11) Uani 1 1 d . . .
C9 C 1.2866(6) 0.2249(6) 0.6369(5) 0.0602(15) Uani 1 1 d . . .
H9A H 1.2729 0.1810 0.7185 0.072 Uiso 1 1 calc R . .
H9B H 1.3829 0.2204 0.6010 0.072 Uiso 1 1 calc R . .
C10 C 1.2068(6) 0.3707(6) 0.6254(5) 0.0596(15) Uani 1 1 d . . .
C11 C 1.1757(8) 0.4300(9) 0.7116(7) 0.088(2) Uani 1 1 d . . .
H11 H 1.2001 0.3789 0.7782 0.105 Uiso 1 1 calc R . .
C12 C 1.1079(10) 0.5660(11) 0.6989(9) 0.114(3) Uani 1 1 d . . .
H12 H 1.0905 0.6062 0.7558 0.136 Uiso 1 1 calc R . .
C13 C 1.0663(9) 0.6418(9) 0.6034(10) 0.107(3) Uani 1 1 d . . .
H13 H 1.0177 0.7320 0.5966 0.128 Uiso 1 1 calc R . .
C14 C 1.0970(7) 0.5833(7) 0.5195(8) 0.084(2) Uani 1 1 d . . .
H14 H 1.0699 0.6343 0.4541 0.100 Uiso 1 1 calc R . .
C15 C 1.1678(6) 0.4492(7) 0.5289(6) 0.0704(18) Uani 1 1 d . . .
H15 H 1.1892 0.4115 0.4692 0.085 Uiso 1 1 calc R . .
C16 C 0.7288(6) 0.1456(6) 0.6191(4) 0.0496(13) Uani 1 1 d . . .
H16 H 0.7780 0.0703 0.5902 0.060 Uiso 1 1 calc R . .
C17 C 0.6545(6) 0.2590(7) 0.5547(5) 0.0628(16) Uani 1 1 d . . .
H17 H 0.6545 0.2594 0.4838 0.075 Uiso 1 1 calc R . .
C18 C 0.5815(6) 0.3702(6) 0.5983(6) 0.0625(17) Uani 1 1 d . . .
C19 C 0.5814(6) 0.3655(6) 0.7025(6) 0.0689(17) Uani 1 1 d . . .
H19 H 0.5308 0.4384 0.7345 0.083 Uiso 1 1 calc R . .
C20 C 0.6571(6) 0.2517(5) 0.7600(5) 0.0562(14) Uani 1 1 d . . .
H20 H 0.6570 0.2506 0.8312 0.067 Uiso 1 1 calc R . .
Mo1 Mo 0.86309(4) -0.06330(4) 0.82738(4) 0.03756(15) Uani 1 1 d . . .
N1 N 0.9308(4) 0.0902(4) 0.8511(3) 0.0361(9) Uani 1 1 d . . .
N2 N 1.0456(4) 0.1335(4) 0.7730(3) 0.0414(9) Uani 1 1 d . . .
N3 N 0.7309(4) 0.1425(4) 0.7215(3) 0.0420(9) Uani 1 1 d . . .
N4 N 0.5018(6) 0.5115(6) 0.5374(5) 0.0753(16) Uani 1 1 d . . .
O1 O 0.7021(3) -0.0061(3) 0.9495(3) 0.0448(8) Uani 1 1 d . . .
O2 O 0.8131(4) -0.1383(3) 0.7662(3) 0.0521(9) Uani 1 1 d . . .
O3 O 0.9581(4) -0.1900(4) 0.9076(4) 0.0657(11) Uani 1 1 d . . .
S1 S 1.04781(14) -0.01654(15) 0.64994(13) 0.0546(4) Uani 1 1 d . . .
S2 S 1.24746(15) 0.12811(15) 0.57590(13) 0.0568(4) Uani 1 1 d . . .
C21A C 0.7781(15) 0.5802(15) 0.9084(13) 0.090(5) Uiso 0.539(10) 1 d PD A 1
H21A H 0.8281 0.6470 0.8572 0.108 Uiso 0.539(10) 1 calc PR A 1
Cl1A Cl 0.8804(7) 0.4516(5) 0.9809(7) 0.0826(15) Uani 0.539(10) 1 d PD A 1
Cl2A Cl 0.7348(15) 0.5267(15) 0.8251(12) 0.189(6) Uani 0.539(10) 1 d PD A 1
Cl3A Cl 0.6354(8) 0.6543(7) 1.0090(6) 0.181(5) Uani 0.539(10) 1 d PD A 1
C21B C 0.7282(15) 0.5741(17) 0.9083(13) 0.083(5) Uiso 0.461(10) 1 d PD A 2
H21B H 0.7274 0.6679 0.8677 0.099 Uiso 0.461(10) 1 calc PR A 2
Cl1B Cl 0.5631(7) 0.5643(10) 0.9927(7) 0.161(4) Uani 0.461(10) 1 d PD . 2
Cl2B Cl 0.8344(15) 0.5076(17) 0.9907(12) 0.187(6) Uani 0.461(10) 1 d PD A 2
Cl3B Cl 0.7778(14) 0.4819(11) 0.8086(9) 0.123(4) Uani 0.461(10) 1 d PD A 2


_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
Br1 C4 1.892(5) . ?
C1 O1 1.338(5) . ?
C1 C2 1.378(7) . ?
C1 C6 1.408(6) . ?
C2 C3 1.384(7) . ?
C2 H2 0.9300 . ?
C3 C4 1.390(7) . ?
C3 H3 0.9300 . ?
C4 C5 1.361(7) . ?
C5 C6 1.410(6) . ?
C5 H5 0.9300 . ?
C6 C7 1.454(7) . ?
C7 N1 1.285(6) . ?
C7 H7 0.9300 . ?
C8 N2 1.282(6) . ?
C8 S1 1.745(5) . ?
C8 S2 1.749(5) . ?
C9 C10 1.506(8) . ?
C9 S2 1.821(6) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 C15 1.374(9) . ?
C10 C11 1.380(9) . ?
C11 C12 1.389(12) . ?
C11 H11 0.9300 . ?
C12 C13 1.370(13) . ?
C12 H12 0.9300 . ?
C13 C14 1.349(11) . ?
C13 H13 0.9300 . ?
C14 C15 1.381(9) . ?
C14 H14 0.9300 . ?
C15 H15 0.9300 . ?
C16 N3 1.341(6) . ?
C16 C17 1.401(8) . ?
C16 H16 0.9300 . ?
C17 C18 1.379(9) . ?
C17 H17 0.9300 . ?
C18 C19 1.349(9) . ?
C18 N4 1.570(8) . ?
C19 C20 1.367(8) . ?
C19 H19 0.9300 . ?
C20 N3 1.328(6) . ?
C20 H20 0.9300 . ?
Mo1 O3 1.693(4) . ?
Mo1 O2 1.703(3) . ?
Mo1 O1 1.929(3) . ?
Mo1 N1 2.285(4) . ?
Mo1 S1 2.4352(15) . ?
Mo1 N3 2.458(4) . ?
N1 N2 1.400(5) . ?
N4 N4 1.124(9) 2_666 ?
C21A Cl1A 1.693(14) . ?
C21A Cl2A 1.714(14) . ?
C21A Cl3A 1.742(13) . ?
C21A H21A 0.9800 . ?
C21B Cl2B 1.702(15) . ?
C21B Cl1B 1.740(14) . ?
C21B Cl3B 1.749(15) . ?
C21B H21B 0.9800 . ?
Cl1B Cl1B 2.29(2) 2_667 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 C1 C2 118.9(4) . . ?
O1 C1 C6 121.4(4) . . ?
C2 C1 C6 119.6(4) . . ?
C1 C2 C3 121.0(5) . . ?
C1 C2 H2 119.5 . . ?
C3 C2 H2 119.5 . . ?
C2 C3 C4 119.2(5) . . ?
C2 C3 H3 120.4 . . ?
C4 C3 H3 120.4 . . ?
C5 C4 C3 121.3(5) . . ?
C5 C4 Br1 118.9(4) . . ?
C3 C4 Br1 119.7(4) . . ?
C4 C5 C6 119.9(4) . . ?
C4 C5 H5 120.1 . . ?
C6 C5 H5 120.1 . . ?
C1 C6 C5 119.0(4) . . ?
C1 C6 C7 124.1(4) . . ?
C5 C6 C7 116.7(4) . . ?
N1 C7 C6 125.5(4) . . ?
N1 C7 H7 117.2 . . ?
C6 C7 H7 117.2 . . ?
N2 C8 S1 127.4(4) . . ?
N2 C8 S2 120.8(4) . . ?
S1 C8 S2 111.8(3) . . ?
C10 C9 S2 117.5(4) . . ?
C10 C9 H9A 107.9 . . ?
S2 C9 H9A 107.9 . . ?
C10 C9 H9B 107.9 . . ?
S2 C9 H9B 107.9 . . ?
H9A C9 H9B 107.2 . . ?
C15 C10 C11 118.3(7) . . ?
C15 C10 C9 121.8(6) . . ?
C11 C10 C9 119.8(7) . . ?
C10 C11 C12 120.1(8) . . ?
C10 C11 H11 120.0 . . ?
C12 C11 H11 120.0 . . ?
C13 C12 C11 120.8(8) . . ?
C13 C12 H12 119.6 . . ?
C11 C12 H12 119.6 . . ?
C14 C13 C12 118.8(8) . . ?
C14 C13 H13 120.6 . . ?
C12 C13 H13 120.6 . . ?
C13 C14 C15 121.2(8) . . ?
C13 C14 H14 119.4 . . ?
C15 C14 H14 119.4 . . ?
C10 C15 C14 120.7(7) . . ?
C10 C15 H15 119.6 . . ?
C14 C15 H15 119.6 . . ?
N3 C16 C17 121.9(5) . . ?
N3 C16 H16 119.1 . . ?
C17 C16 H16 119.1 . . ?
C18 C17 C16 118.7(5) . . ?
C18 C17 H17 120.6 . . ?
C16 C17 H17 120.6 . . ?
C19 C18 C17 119.2(5) . . ?
C19 C18 N4 113.0(6) . . ?
C17 C18 N4 127.7(6) . . ?
C18 C19 C20 118.8(6) . . ?
C18 C19 H19 120.6 . . ?
C20 C19 H19 120.6 . . ?
N3 C20 C19 124.6(6) . . ?
N3 C20 H20 117.7 . . ?
C19 C20 H20 117.7 . . ?
O3 Mo1 O2 105.84(18) . . ?
O3 Mo1 O1 99.64(18) . . ?
O2 Mo1 O1 104.97(15) . . ?
O3 Mo1 N1 90.41(16) . . ?
O2 Mo1 N1 160.59(16) . . ?
O1 Mo1 N1 82.10(13) . . ?
O3 Mo1 S1 98.41(15) . . ?
O2 Mo1 S1 90.98(13) . . ?
O1 Mo1 S1 151.52(11) . . ?
N1 Mo1 S1 75.91(10) . . ?
O3 Mo1 N3 171.63(16) . . ?
O2 Mo1 N3 82.53(15) . . ?
O1 Mo1 N3 77.53(14) . . ?
N1 Mo1 N3 81.43(13) . . ?
S1 Mo1 N3 81.45(10) . . ?
C7 N1 N2 112.4(4) . . ?
C7 N1 Mo1 124.7(3) . . ?
N2 N1 Mo1 122.5(3) . . ?
C8 N2 N1 113.6(4) . . ?
C20 N3 C16 116.8(4) . . ?
C20 N3 Mo1 124.3(3) . . ?
C16 N3 Mo1 118.8(3) . . ?
N4 N4 C18 101.3(8) 2_666 . ?
C1 O1 Mo1 136.8(3) . . ?
C8 S1 Mo1 100.04(17) . . ?
C8 S2 C9 102.4(2) . . ?
Cl1A C21A Cl2A 111.3(9) . . ?
Cl1A C21A Cl3A 108.0(8) . . ?
Cl2A C21A Cl3A 112.5(10) . . ?
Cl1A C21A H21A 108.3 . . ?
Cl2A C21A H21A 108.3 . . ?
Cl3A C21A H21A 108.3 . . ?
Cl2B C21B Cl1B 110.9(10) . . ?
Cl2B C21B Cl3B 111.2(10) . . ?
Cl1B C21B Cl3B 104.8(10) . . ?
Cl2B C21B H21B 109.9 . . ?
Cl1B C21B H21B 109.9 . . ?
Cl3B C21B H21B 109.9 . . ?
C21B Cl1B Cl1B 132.0(9) . 2_667 ?

_diffrn_measured_fraction_theta_max 0.983
_diffrn_reflns_theta_full        25.50
_diffrn_measured_fraction_theta_full 0.983
_refine_diff_density_max         1.072
_refine_diff_density_min         -0.660
_refine_diff_density_rms         0.087





####################################################################### 
# 
# 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_1
_database_code_depnum_ccdc_archive 'CCDC 1054805'
_audit_update_record             
;
2015-08-24 deposited with the CCDC.
2015-08-26 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C42 H34 Cl6 Mo2 N8 O6 S4'
_chemical_formula_weight         1279.59

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'
S S 0.1246 0.1234 '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'
Cl Cl 0.1484 0.1585 '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                   10.827(18)
_cell_length_b                   11.070(18)
_cell_length_c                   12.58(2)
_cell_angle_alpha                65.780(17)
_cell_angle_beta                 73.533(17)
_cell_angle_gamma                65.932(17)
_cell_volume                     1243(4)
_cell_formula_units_Z            1
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    7866
_cell_measurement_theta_min      1.79
_cell_measurement_theta_max      25.00

_exptl_crystal_description       rectangular
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.14
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.709
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             640
_exptl_absorpt_coefficient_mu    1.050
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.757
_exptl_absorpt_correction_T_max  0.805
_exptl_absorpt_process_details   'SADABS(Sheldrick, 2008)'

_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  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         7902
_diffrn_standards_interval_count n/a
_diffrn_standards_interval_time  n/a
_diffrn_standards_decay_%        n/a
_diffrn_reflns_number            7866
_diffrn_reflns_av_R_equivalents  0.1828
_diffrn_reflns_av_sigmaI/netI    0.1805
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         1.79
_diffrn_reflns_theta_max         25.00
_reflns_number_total             4379
_reflns_number_gt                2429
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_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.

 distance constraints were applied to the solvent molecules
;

_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)+(0.1283P)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    constr
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.012(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         4217
_refine_ls_number_parameters     335
_refine_ls_number_restraints     21
_refine_ls_R_factor_all          0.1394
_refine_ls_R_factor_gt           0.0838
_refine_ls_wR_factor_ref         0.2420
_refine_ls_wR_factor_gt          0.2067
_refine_ls_goodness_of_fit_ref   0.943
_refine_ls_restrained_S_all      0.950
_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
Mo1 Mo 0.45021(8) 0.34965(9) 0.32695(7) 0.0469(4) Uani 1 1 d . . .
N1 N 0.6005(7) 0.4239(8) 0.3550(6) 0.0440(18) Uani 1 1 d . . .
N2 N 0.6337(8) 0.5423(8) 0.2754(6) 0.0502(19) Uani 1 1 d . . .
N3 N 0.6571(8) 0.2156(8) 0.2301(6) 0.0458(18) Uani 1 1 d . . .
N4 N 1.0077(8) -0.0004(9) 0.0479(6) 0.057(2) Uani 1 1 d . . .
O1 O 0.5265(7) 0.1870(7) 0.4553(5) 0.0545(17) Uani 1 1 d . . .
O2 O 0.3742(6) 0.2968(7) 0.2616(6) 0.0536(16) Uani 1 1 d . . .
O3 O 0.3227(7) 0.4434(7) 0.4028(6) 0.0635(19) Uani 1 1 d . . .
S1 S 0.4769(3) 0.5370(3) 0.1451(2) 0.0558(7) Uani 1 1 d . . .
S2 S 0.6010(3) 0.7469(3) 0.0697(2) 0.0647(8) Uani 1 1 d . . .
C1 C 0.5771(11) 0.1647(10) 0.5485(7) 0.052(3) Uani 1 1 d . . .
C2 C 0.5731(12) 0.0453(11) 0.6471(9) 0.065(3) Uani 1 1 d . . .
H2 H 0.5318 -0.0143 0.6480 0.079 Uiso 1 1 calc R . .
C3 C 0.6304(14) 0.0174(13) 0.7417(9) 0.084(4) Uani 1 1 d . . .
H3 H 0.6294 -0.0631 0.8064 0.100 Uiso 1 1 calc R . .
C4 C 0.6899(15) 0.1053(14) 0.7445(9) 0.084(4) Uani 1 1 d . . .
H4 H 0.7268 0.0853 0.8106 0.100 Uiso 1 1 calc R . .
C5 C 0.6933(12) 0.2172(11) 0.6522(8) 0.066(3) Uani 1 1 d . . .
H5 H 0.7355 0.2750 0.6532 0.079 Uiso 1 1 calc R . .
C6 C 0.6348(10) 0.2536(10) 0.5506(7) 0.051(2) Uani 1 1 d . . .
C7 C 0.6487(9) 0.3778(10) 0.4523(8) 0.047(2) Uani 1 1 d . . .
H7 H 0.6955 0.4274 0.4600 0.056 Uiso 1 1 calc R . .
C8 C 0.5796(10) 0.5943(10) 0.1803(8) 0.049(2) Uani 1 1 d . . .
C9 C 0.6993(12) 0.7971(12) 0.1296(11) 0.073(3) Uani 1 1 d . . .
H9A H 0.6839 0.8969 0.0907 0.088 Uiso 1 1 calc R . .
H9B H 0.6648 0.7818 0.2125 0.088 Uiso 1 1 calc R . .
C10 C 0.8511(13) 0.7200(12) 0.1176(10) 0.069(3) Uani 1 1 d . . .
C11 C 0.9214(13) 0.6856(13) 0.0203(12) 0.082(4) Uani 1 1 d . . .
H11 H 0.8750 0.7058 -0.0401 0.099 Uiso 1 1 calc R . .
C12 C 1.0609(15) 0.6211(16) 0.0103(14) 0.102(5) Uani 1 1 d . . .
H12 H 1.1077 0.5981 -0.0568 0.122 Uiso 1 1 calc R . .
C13 C 1.1282(17) 0.5918(17) 0.0935(18) 0.115(6) Uani 1 1 d . . .
H13 H 1.2222 0.5462 0.0859 0.137 Uiso 1 1 calc R . .
C14 C 1.062(2) 0.6276(18) 0.1920(16) 0.122(7) Uani 1 1 d . . .
H14 H 1.1103 0.6093 0.2505 0.146 Uiso 1 1 calc R . .
C15 C 0.9233(16) 0.6908(16) 0.2022(12) 0.095(4) Uani 1 1 d . . .
H15 H 0.8772 0.7145 0.2693 0.114 Uiso 1 1 calc R . .
C16 C 0.7776(10) 0.1494(12) 0.2670(8) 0.060(3) Uani 1 1 d . . .
H16 H 0.7854 0.1525 0.3375 0.071 Uiso 1 1 calc R . .
C17 C 0.8895(10) 0.0783(11) 0.2103(8) 0.061(3) Uani 1 1 d . . .
H17 H 0.9713 0.0344 0.2416 0.073 Uiso 1 1 calc R . .
C18 C 0.8837(9) 0.0699(10) 0.1064(7) 0.047(2) Uani 1 1 d . . .
C19 C 0.7598(10) 0.1339(10) 0.0663(8) 0.053(2) Uani 1 1 d . . .
H19 H 0.7509 0.1288 -0.0030 0.064 Uiso 1 1 calc R . .
C20 C 0.6498(10) 0.2049(11) 0.1279(8) 0.056(3) Uani 1 1 d . . .
H20 H 0.5664 0.2478 0.0992 0.067 Uiso 1 1 calc R . .
C21 C 0.087(2) 0.2979(19) 0.4155(17) 0.088(8) Uiso 0.526(7) 1 d PD A 1
H21 H 0.1477 0.3509 0.3633 0.105 Uiso 0.526(7) 1 calc PR A 1
Cl1 Cl 0.0254(17) 0.2568(15) 0.3278(13) 0.141(5) Uani 0.526(7) 1 d PD A 1
Cl2 Cl -0.0411(7) 0.4061(9) 0.4863(7) 0.113(3) Uani 0.526(7) 1 d PD A 1
Cl3 Cl 0.1823(8) 0.1547(9) 0.5163(7) 0.115(3) Uani 0.526(7) 1 d PD A 1
C22 C 0.094(3) 0.2001(19) 0.4044(17) 0.095(9) Uiso 0.474(7) 1 d PD A 2
H22 H 0.1898 0.1727 0.3690 0.114 Uiso 0.474(7) 1 calc PR A 2
Cl4 Cl 0.0392(8) 0.0561(8) 0.4702(7) 0.097(3) Uani 0.474(7) 1 d PD . 2
Cl5 Cl 0.072(2) 0.2741(16) 0.5075(11) 0.208(10) Uani 0.474(7) 1 d PD A 2
Cl6 Cl -0.011(2) 0.3230(14) 0.2966(13) 0.157(7) Uani 0.474(7) 1 d PD A 2


_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 O3 1.670(7) . ?
Mo1 O2 1.692(6) . ?
Mo1 O1 1.920(6) . ?
Mo1 N1 2.259(8) . ?
Mo1 S1 2.416(4) . ?
Mo1 N3 2.435(8) . ?
N1 C7 1.289(11) . ?
N1 N2 1.398(10) . ?
N2 C8 1.289(11) . ?
N3 C16 1.318(11) . ?
N3 C20 1.366(11) . ?
N4 N4 1.259(14) 2_755 ?
N4 C18 1.417(11) . ?
O1 C1 1.324(10) . ?
S1 C8 1.709(10) . ?
S2 C8 1.747(10) . ?
S2 C9 1.813(11) . ?
C1 C6 1.377(14) . ?
C1 C2 1.399(13) . ?
C2 C3 1.363(15) . ?
C2 H2 0.9300 . ?
C3 C4 1.384(18) . ?
C3 H3 0.9300 . ?
C4 C5 1.310(16) . ?
C4 H4 0.9300 . ?
C5 C6 1.423(13) . ?
C5 H5 0.9300 . ?
C6 C7 1.453(13) . ?
C7 H7 0.9300 . ?
C9 C10 1.508(16) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 C15 1.353(16) . ?
C10 C11 1.357(16) . ?
C11 C12 1.376(17) . ?
C11 H11 0.9300 . ?
C12 C13 1.301(19) . ?
C12 H12 0.9300 . ?
C13 C14 1.37(2) . ?
C13 H13 0.9300 . ?
C14 C15 1.37(2) . ?
C14 H14 0.9300 . ?
C15 H15 0.9300 . ?
C16 C17 1.338(13) . ?
C16 H16 0.9300 . ?
C17 C18 1.368(12) . ?
C17 H17 0.9300 . ?
C18 C19 1.367(13) . ?
C19 C20 1.360(13) . ?
C19 H19 0.9300 . ?
C20 H20 0.9300 . ?
C21 Cl3 1.715(16) . ?
C21 Cl1 1.717(17) . ?
C21 Cl2 1.723(16) . ?
C21 H21 0.9800 . ?
C22 Cl5 1.718(18) . ?
C22 Cl4 1.728(18) . ?
C22 Cl6 1.751(18) . ?
C22 H22 0.9800 . ?
Cl4 Cl4 1.599(15) 2_556 ?

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
O3 Mo1 O2 105.5(3) . . ?
O3 Mo1 O1 99.5(3) . . ?
O2 Mo1 O1 106.0(3) . . ?
O3 Mo1 N1 90.9(3) . . ?
O2 Mo1 N1 160.2(3) . . ?
O1 Mo1 N1 81.7(3) . . ?
O3 Mo1 S1 99.5(3) . . ?
O2 Mo1 S1 90.3(3) . . ?
O1 Mo1 S1 150.6(2) . . ?
N1 Mo1 S1 75.8(2) . . ?
O3 Mo1 N3 172.0(3) . . ?
O2 Mo1 N3 82.4(3) . . ?
O1 Mo1 N3 76.8(3) . . ?
N1 Mo1 N3 81.7(3) . . ?
S1 Mo1 N3 81.4(2) . . ?
C7 N1 N2 111.4(7) . . ?
C7 N1 Mo1 124.6(7) . . ?
N2 N1 Mo1 123.1(5) . . ?
C8 N2 N1 112.1(7) . . ?
C16 N3 C20 115.5(8) . . ?
C16 N3 Mo1 126.6(5) . . ?
C20 N3 Mo1 117.9(6) . . ?
N4 N4 C18 112.1(9) 2_755 . ?
C1 O1 Mo1 135.1(6) . . ?
C8 S1 Mo1 100.3(3) . . ?
C8 S2 C9 103.8(5) . . ?
O1 C1 C6 122.2(8) . . ?
O1 C1 C2 118.5(9) . . ?
C6 C1 C2 119.3(9) . . ?
C3 C2 C1 119.2(11) . . ?
C3 C2 H2 120.4 . . ?
C1 C2 H2 120.4 . . ?
C2 C3 C4 122.0(11) . . ?
C2 C3 H3 119.0 . . ?
C4 C3 H3 119.0 . . ?
C5 C4 C3 118.7(11) . . ?
C5 C4 H4 120.6 . . ?
C3 C4 H4 120.6 . . ?
C4 C5 C6 122.4(11) . . ?
C4 C5 H5 118.8 . . ?
C6 C5 H5 118.8 . . ?
C1 C6 C5 118.3(9) . . ?
C1 C6 C7 124.1(8) . . ?
C5 C6 C7 117.4(9) . . ?
N1 C7 C6 124.4(9) . . ?
N1 C7 H7 117.8 . . ?
C6 C7 H7 117.8 . . ?
N2 C8 S1 128.3(8) . . ?
N2 C8 S2 120.6(7) . . ?
S1 C8 S2 111.1(5) . . ?
C10 C9 S2 115.4(9) . . ?
C10 C9 H9A 108.4 . . ?
S2 C9 H9A 108.4 . . ?
C10 C9 H9B 108.4 . . ?
S2 C9 H9B 108.4 . . ?
H9A C9 H9B 107.5 . . ?
C15 C10 C11 117.7(13) . . ?
C15 C10 C9 120.0(13) . . ?
C11 C10 C9 122.2(11) . . ?
C10 C11 C12 120.4(14) . . ?
C10 C11 H11 119.8 . . ?
C12 C11 H11 119.8 . . ?
C13 C12 C11 121.0(17) . . ?
C13 C12 H12 119.5 . . ?
C11 C12 H12 119.5 . . ?
C12 C13 C14 120.6(17) . . ?
C12 C13 H13 119.7 . . ?
C14 C13 H13 119.7 . . ?
C15 C14 C13 118.4(15) . . ?
C15 C14 H14 120.8 . . ?
C13 C14 H14 120.8 . . ?
C10 C15 C14 121.9(15) . . ?
C10 C15 H15 119.1 . . ?
C14 C15 H15 119.1 . . ?
N3 C16 C17 124.8(8) . . ?
N3 C16 H16 117.6 . . ?
C17 C16 H16 117.6 . . ?
C16 C17 C18 120.0(9) . . ?
C16 C17 H17 120.0 . . ?
C18 C17 H17 120.0 . . ?
C19 C18 C17 117.2(8) . . ?
C19 C18 N4 125.8(8) . . ?
C17 C18 N4 117.0(8) . . ?
C20 C19 C18 119.9(8) . . ?
C20 C19 H19 120.0 . . ?
C18 C19 H19 120.0 . . ?
C19 C20 N3 122.5(9) . . ?
C19 C20 H20 118.7 . . ?
N3 C20 H20 118.7 . . ?
Cl3 C21 Cl1 114.2(12) . . ?
Cl3 C21 Cl2 109.7(11) . . ?
Cl1 C21 Cl2 112.1(11) . . ?
Cl3 C21 H21 106.8 . . ?
Cl1 C21 H21 106.8 . . ?
Cl2 C21 H21 106.8 . . ?
Cl5 C22 Cl4 109.3(12) . . ?
Cl5 C22 Cl6 108.2(13) . . ?
Cl4 C22 Cl6 107.4(12) . . ?
Cl5 C22 H22 110.6 . . ?
Cl4 C22 H22 110.6 . . ?
Cl6 C22 H22 110.6 . . ?
Cl4 Cl4 C22 169.4(11) 2_556 . ?

_diffrn_measured_fraction_theta_max 0.964
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.964
_refine_diff_density_max         1.204
_refine_diff_density_min         -1.733
_refine_diff_density_rms         0.145
####################################################################### 
# 
# 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_2
_database_code_depnum_ccdc_archive 'CCDC 1054806'
_audit_update_record             
;
2015-08-24 deposited with the CCDC.
2015-08-26 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C42 H32 Cl6 Mo2 N10 O10 S4'
_chemical_formula_weight         1369.60

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'
Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 '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'

_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                   10.9255(7)
_cell_length_b                   10.9637(7)
_cell_length_c                   13.2353(8)
_cell_angle_alpha                67.269(6)
_cell_angle_beta                 69.255(5)
_cell_angle_gamma                67.937(6)
_cell_volume                     1314.00(16)
_cell_formula_units_Z            1
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    9331
_cell_measurement_theta_min      3.33
_cell_measurement_theta_max      30.00


_exptl_crystal_description       cube
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.03
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.731
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             684
_exptl_absorpt_coefficient_mu    1.006

_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'ABSPACK, Oxford Diffraction Ltd'
_exptl_absorpt_correction_T_min  0.912
_exptl_absorpt_correction_T_max  1.000

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_standards_number         n/a
_diffrn_measurement_device_type  'Oxford Diffaction X-Calibur System'
_diffrn_measurement_method       '321 frames, counting time 10 s.'
_diffrn_standards_interval_count n/a
_diffrn_standards_interval_time  n/a
_diffrn_standards_decay_%        n/a
_diffrn_reflns_number            9331
_diffrn_reflns_av_R_equivalents  0.0314
_diffrn_reflns_av_sigmaI/netI    0.0800
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         3.33
_diffrn_reflns_theta_max         30.00
_reflns_number_total             7678
_reflns_number_gt                5698
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Crysalis, Oxford Diffraction'
_computing_cell_refinement       'Crysalis, Oxford Diffraction'
_computing_data_reduction        'Crysalis, Oxford Diffraction'
_computing_structure_solution    'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    PLATON(Spek,2004)
_computing_publication_material  PLATON(Spek,2004)

_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.

 distance constraints were applied to the disordered solvent molecules
;


_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)+(0.0495P)²+2.0871P] 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         7348
_refine_ls_number_parameters     343
_refine_ls_number_restraints     21
_refine_ls_R_factor_all          0.0822
_refine_ls_R_factor_gt           0.0590
_refine_ls_wR_factor_ref         0.1387
_refine_ls_wR_factor_gt          0.1243
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_restrained_S_all      1.283
_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
Mo1 Mo 0.43474(4) 0.35831(4) 0.82155(3) 0.01647(12) Uani 1 1 d . . .
O2 O 0.3584(4) 0.3011(4) 0.7625(3) 0.0227(7) Uani 1 1 d . . .
O3 O 0.3064(4) 0.4559(4) 0.9000(3) 0.0267(8) Uani 1 1 d . . .
S1 S 0.48144(13) 0.53705(13) 0.64591(10) 0.0217(3) Uani 1 1 d . . .
N5 N 0.7193(5) 0.0862(5) 1.2986(4) 0.0276(10) Uani 1 1 d . . .
O4 O 0.7139(5) -0.0207(4) 1.3757(3) 0.0420(11) Uani 1 1 d . . .
O5 O 0.7747(5) 0.1675(4) 1.2940(3) 0.0406(11) Uani 1 1 d . . .
C8 C 0.5837(5) 0.6001(5) 0.6783(4) 0.0183(9) Uani 1 1 d . . .
N2 N 0.6310(4) 0.5502(4) 0.7672(3) 0.0186(8) Uani 1 1 d . . .
N1 N 0.5888(4) 0.4339(4) 0.8446(3) 0.0155(8) Uani 1 1 d . . .
C7 C 0.6320(5) 0.3890(5) 0.9351(4) 0.0173(9) Uani 1 1 d . . .
H7 H 0.6821 0.4379 0.9401 0.021 Uiso 1 1 calc R . .
C6 C 0.6095(5) 0.2696(5) 1.0292(4) 0.0163(9) Uani 1 1 d . . .
C5 C 0.6663(5) 0.2368(5) 1.1195(4) 0.0199(10) Uani 1 1 d . . .
H5 H 0.7112 0.2938 1.1198 0.024 Uiso 1 1 calc R . .
C4 C 0.6547(5) 0.1191(5) 1.2076(4) 0.0193(10) Uani 1 1 d . . .
C3 C 0.5912(6) 0.0300(5) 1.2113(4) 0.0236(11) Uani 1 1 d . . .
H3 H 0.5866 -0.0494 1.2716 0.028 Uiso 1 1 calc R . .
C2 C 0.5343(6) 0.0613(5) 1.1231(4) 0.0232(10) Uani 1 1 d . . .
H2 H 0.4897 0.0027 1.1250 0.028 Uiso 1 1 calc R . .
C1 C 0.5426(5) 0.1795(5) 1.0310(4) 0.0172(9) Uani 1 1 d . . .
O1 O 0.4943(4) 0.1999(3) 0.9458(3) 0.0189(7) Uani 1 1 d . . .
N3 N 0.6415(4) 0.2219(4) 0.7249(3) 0.0170(8) Uani 1 1 d . . .
C16 C 0.7528(5) 0.1515(5) 0.7658(4) 0.0219(10) Uani 1 1 d . . .
H16 H 0.7504 0.1544 0.8358 0.026 Uiso 1 1 calc R . .
C17 C 0.8697(5) 0.0756(6) 0.7097(4) 0.0259(11) Uani 1 1 d . . .
H17 H 0.9444 0.0276 0.7412 0.031 Uiso 1 1 calc R . .
C18 C 0.8735(5) 0.0727(5) 0.6045(4) 0.0208(10) Uani 1 1 d . . .
C19 C 0.7593(5) 0.1423(5) 0.5615(4) 0.0194(10) Uani 1 1 d . . .
H19 H 0.7590 0.1402 0.4920 0.023 Uiso 1 1 calc R . .
C20 C 0.6466(5) 0.2142(5) 0.6241(4) 0.0196(9) Uani 1 1 d . . .
H20 H 0.5695 0.2603 0.5956 0.024 Uiso 1 1 calc R . .
N4 N 1.0014(5) -0.0002(5) 0.5455(4) 0.0280(10) Uani 1 1 d . . .
S2 S 0.62006(13) 0.74686(13) 0.57280(10) 0.0216(3) Uani 1 1 d . . .
C9 C 0.7223(6) 0.7920(5) 0.6291(4) 0.0245(11) Uani 1 1 d . . .
H9B H 0.7192 0.8881 0.5914 0.029 Uiso 1 1 calc R . .
H9A H 0.6795 0.7829 0.7086 0.029 Uiso 1 1 calc R . .
C10 C 0.8688(6) 0.7098(5) 0.6181(4) 0.0263(11) Uani 1 1 d . . .
C15 C 0.9484(6) 0.6739(6) 0.5197(5) 0.0325(13) Uani 1 1 d . . .
H15 H 0.9092 0.6983 0.4602 0.039 Uiso 1 1 calc R . .
C14 C 1.0855(7) 0.6022(7) 0.5092(6) 0.0398(15) Uani 1 1 d . . .
H14 H 1.1366 0.5769 0.4437 0.048 Uiso 1 1 calc R . .
C13 C 1.1460(7) 0.5684(7) 0.5956(6) 0.0449(16) Uani 1 1 d . . .
H13 H 1.2378 0.5208 0.5885 0.054 Uiso 1 1 calc R . .
C12 C 1.0694(7) 0.6058(7) 0.6927(6) 0.0469(18) Uani 1 1 d . . .
H12 H 1.1102 0.5852 0.7504 0.056 Uiso 1 1 calc R . .
C11 C 0.9306(7) 0.6747(6) 0.7043(5) 0.0375(14) Uani 1 1 d . . .
H11 H 0.8792 0.6973 0.7708 0.045 Uiso 1 1 calc R . .
C1A C 0.9254(14) 0.7185(15) 0.1032(11) 0.046(3) Uiso 0.526(6) 1 d PD A 1
H1A H 0.8583 0.6680 0.1535 0.055 Uiso 0.526(6) 1 calc PR A 1
Cl1A Cl 0.8438(4) 0.8628(4) 0.0040(3) 0.0714(18) Uani 0.526(6) 1 d PD A 1
Cl2A Cl 1.0041(3) 0.7430(3) 0.1906(2) 0.0954(10) Uani 0.526(6) 1 d PD A 1
Cl3A Cl 1.0363(3) 0.6261(3) 0.02310(17) 0.0809(8) Uani 0.526(6) 1 d PD A 1
Cl1B Cl 0.9327(6) 0.9376(5) 0.0131(5) 0.089(2) Uani 0.474(6) 1 d PD . 2
Cl2B Cl 1.0041(3) 0.7430(3) 0.1906(2) 0.0954(10) Uani 0.474(6) 1 d PD A 2
Cl3B Cl 1.0363(3) 0.6261(3) 0.02310(17) 0.0809(8) Uani 0.474(6) 1 d PD A 2
C1B C 0.9284(17) 0.7668(15) 0.0947(12) 0.049(4) Uiso 0.474(6) 1 d PD A 2
H1B H 0.8346 0.7606 0.1289 0.058 Uiso 0.474(6) 1 calc PR A 2


_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 O3 1.700(3) . ?
Mo1 O2 1.713(3) . ?
Mo1 O1 1.961(3) . ?
Mo1 N1 2.285(4) . ?
Mo1 N3 2.423(4) . ?
Mo1 S1 2.4280(13) . ?
S1 C8 1.748(5) . ?
N5 O5 1.226(6) . ?
N5 O4 1.226(6) . ?
N5 C4 1.468(6) . ?
C8 N2 1.293(6) . ?
C8 S2 1.746(5) . ?
N2 N1 1.409(5) . ?
N1 C7 1.292(6) . ?
C7 C6 1.445(6) . ?
C6 C5 1.403(6) . ?
C6 C1 1.423(7) . ?
C5 C4 1.377(7) . ?
C4 C3 1.373(7) . ?
C3 C2 1.382(7) . ?
C2 C1 1.401(7) . ?
C1 O1 1.318(5) . ?
N3 C16 1.343(6) . ?
N3 C20 1.350(6) . ?
C16 C17 1.372(7) . ?
C17 C18 1.391(7) . ?
C18 C19 1.385(7) . ?
C18 N4 1.439(6) . ?
C19 C20 1.370(6) . ?
N4 N4 1.214(8) 2_756 ?
S2 C9 1.826(5) . ?
C9 C10 1.499(8) . ?
C10 C11 1.384(8) . ?
C10 C15 1.395(8) . ?
C15 C14 1.390(9) . ?
C14 C13 1.381(9) . ?
C13 C12 1.381(10) . ?
C12 C11 1.399(9) . ?
C1A Cl3A 1.618(13) . ?
C1A Cl1A 1.785(13) . ?
C1A Cl2A 1.808(13) . ?
Cl1B C1B 1.773(15) . ?
Cl2B C1B 1.639(14) . ?
Cl3B C1B 1.908(14) . ?

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
O3 Mo1 O2 106.18(17) . . ?
O3 Mo1 O1 98.31(16) . . ?
O2 Mo1 O1 105.31(15) . . ?
O3 Mo1 N1 89.86(16) . . ?
O2 Mo1 N1 160.95(15) . . ?
O1 Mo1 N1 81.87(14) . . ?
O3 Mo1 N3 170.63(16) . . ?
O2 Mo1 N3 83.03(15) . . ?
O1 Mo1 N3 77.17(13) . . ?
N1 Mo1 N3 81.42(13) . . ?
O3 Mo1 S1 99.66(14) . . ?
O2 Mo1 S1 90.76(12) . . ?
O1 Mo1 S1 151.43(11) . . ?
N1 Mo1 S1 76.16(10) . . ?
N3 Mo1 S1 81.65(10) . . ?
C8 S1 Mo1 100.10(16) . . ?
O5 N5 O4 123.5(5) . . ?
O5 N5 C4 118.3(4) . . ?
O4 N5 C4 118.2(4) . . ?
N2 C8 S2 120.6(4) . . ?
N2 C8 S1 127.5(4) . . ?
S2 C8 S1 111.9(3) . . ?
C8 N2 N1 113.0(4) . . ?
C7 N1 N2 112.2(4) . . ?
C7 N1 Mo1 124.6(3) . . ?
N2 N1 Mo1 122.5(3) . . ?
N1 C7 C6 125.9(4) . . ?
C5 C6 C1 118.9(4) . . ?
C5 C6 C7 117.2(4) . . ?
C1 C6 C7 123.7(4) . . ?
C4 C5 C6 119.1(4) . . ?
C3 C4 C5 123.2(4) . . ?
C3 C4 N5 119.4(4) . . ?
C5 C4 N5 117.4(4) . . ?
C4 C3 C2 118.4(5) . . ?
C3 C2 C1 121.2(5) . . ?
O1 C1 C2 118.8(4) . . ?
O1 C1 C6 121.9(4) . . ?
C2 C1 C6 119.2(4) . . ?
C1 O1 Mo1 135.9(3) . . ?
C16 N3 C20 117.1(4) . . ?
C16 N3 Mo1 124.1(3) . . ?
C20 N3 Mo1 118.8(3) . . ?
N3 C16 C17 123.5(4) . . ?
C16 C17 C18 118.1(5) . . ?
C19 C18 C17 119.5(4) . . ?
C19 C18 N4 124.4(4) . . ?
C17 C18 N4 116.1(4) . . ?
C20 C19 C18 118.2(4) . . ?
N3 C20 C19 123.5(5) . . ?
N4 N4 C18 113.2(6) 2_756 . ?
C8 S2 C9 102.6(2) . . ?
C10 C9 S2 116.8(4) . . ?
C11 C10 C15 118.2(6) . . ?
C11 C10 C9 120.1(5) . . ?
C15 C10 C9 121.6(5) . . ?
C14 C15 C10 121.0(6) . . ?
C13 C14 C15 120.2(6) . . ?
C12 C13 C14 119.6(6) . . ?
C13 C12 C11 120.1(6) . . ?
C10 C11 C12 120.9(6) . . ?
Cl3A C1A Cl1A 101.9(7) . . ?
Cl3A C1A Cl2A 111.0(8) . . ?
Cl1A C1A Cl2A 120.4(8) . . ?
Cl2B C1B Cl1B 100.1(8) . . ?
Cl2B C1B Cl3B 105.4(8) . . ?
Cl1B C1B Cl3B 116.7(8) . . ?

_diffrn_measured_fraction_theta_max 0.957
_diffrn_reflns_theta_full        30.00
_diffrn_measured_fraction_theta_full 0.957
_refine_diff_density_max         2.214
_refine_diff_density_min         -2.235
_refine_diff_density_rms         0.147
