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

#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
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#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
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data_1a2a

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C6 H12 Cl12 Mo4 O10'
_chemical_formula_weight         1053.32

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

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   Cmcm

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

_cell_length_a                   9.8719(15)
_cell_length_b                   7.9597(12)
_cell_length_c                   34.729(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     2728.9(7)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9928
_cell_measurement_theta_min      2.346
_cell_measurement_theta_max      28.521

_exptl_crystal_description       prism
_exptl_crystal_colour            dark-green
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.14
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.564
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2000
_exptl_absorpt_coefficient_mu    3.010
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.5319
_exptl_absorpt_correction_T_max  0.6779
_exptl_absorpt_process_details   
;
 Data were corrected for Lorentz polarization and absorption
 effects (empirical absorption corrections SADABS).
 R(int) = 0.1599 (selected reflections only, before parameter refinement)
 R(int) = 0.0582 (selected reflections only, after parameter refinement)
;

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            12125
_diffrn_reflns_av_R_equivalents  0.0400
_diffrn_reflns_av_sigmaI/netI    0.0188
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_theta_min         2.35
_diffrn_reflns_theta_max         25.03
_reflns_number_total             1281
_reflns_number_gt                1275
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX2 (Bruker AXS, 2006)'
_computing_cell_refinement       'APEX2 (Bruker AXS, 2006)'
_computing_data_reduction        'SAINT (Bruker AXS, 2004)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'ORTEPII (Johnson, 1996)'
_computing_publication_material  'XCIF (Bruker AXS, 2001)'

_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. The following restraints
 were applied (given as SHELXL lines):  
 simu .01 $c $o
 dfix 1.51 .01 c1 c2
 dfix 1.35 .01 c1 o3  
 eadp o3 c2
 dfix 0.87 .02 o6 h6
;

_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)+(0.0169P)²+19.6807P] 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         1281
_refine_ls_number_parameters     96
_refine_ls_number_restraints     39
_refine_ls_R_factor_all          0.0277
_refine_ls_R_factor_gt           0.0275
_refine_ls_wR_factor_ref         0.0635
_refine_ls_wR_factor_gt          0.0635
_refine_ls_goodness_of_fit_ref   1.337
_refine_ls_restrained_S_all      1.324
_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 0.0000 1.20902(6) 0.699621(13) 0.01226(14) Uani 1 2 d S . .
Cl1 Cl 0.17080(10) 1.05449(13) 0.67221(3) 0.0202(2) Uani 1 1 d . . .
Cl2 Cl 0.16132(13) 1.30144(17) 0.7500 0.0160(3) Uani 1 2 d S . .
O1 O 0.0000 1.3814(5) 0.67352(11) 0.0202(9) Uani 1 2 d S . .
O2 O 0.0000 0.9950(7) 0.7500 0.0144(11) Uani 1 4 d SU . .
C1 C 0.0000 0.8391(10) 0.7500 0.0193(16) Uani 1 4 d SDU . .
O3 O -0.007(6) 0.7562(15) 0.7159(3) 0.015(2) Uiso 0.25 1 d PDU A -1
H3 H -0.0287 0.8237 0.6984 0.023 Uiso 0.25 1 calc PR A -1
C2 C 0.021(3) 0.724(2) 0.7832(4) 0.015(2) Uiso 0.25 1 d PDU A -1
H2A H 0.0051 0.6076 0.7749 0.023 Uiso 0.25 1 calc PR A -1
H2B H -0.0424 0.7526 0.8038 0.023 Uiso 0.25 1 calc PR A -1
H2C H 0.1141 0.7348 0.7926 0.023 Uiso 0.25 1 calc PR A -1
Mo2 Mo 0.5000 1.10710(6) 0.462303(13) 0.01231(14) Uani 1 2 d S . .
Cl3 Cl 0.31118(13) 1.0000 0.5000 0.0161(3) Uani 1 2 d S . .
Cl4 Cl 0.33938(10) 1.15999(12) 0.41396(3) 0.0189(2) Uani 1 1 d . . .
O4 O 0.5000 1.2917(5) 0.48437(11) 0.0175(9) Uani 1 2 d S . .
O5 O 0.5000 0.8458(5) 0.44123(11) 0.0172(8) Uani 1 2 d SU . .
O6 O 0.5000 0.8114(5) 0.37739(13) 0.0342(12) Uani 1 2 d SDU . .
H6 H 0.5000 0.919(3) 0.375(2) 0.051 Uiso 1 2 d SD . .
C3 C 0.5000 0.7531(7) 0.41336(17) 0.0177(12) Uani 1 2 d SU . .
C4 C 0.5000 0.5679(7) 0.41682(16) 0.0174(12) Uani 1 2 d SU . .
H4A H 0.5000 0.5176 0.3911 0.026 Uiso 1 2 calc SR . .
H4B H 0.4189 0.5317 0.4308 0.026 Uiso 0.50 1 calc PR . .
H4C H 0.5811 0.5317 0.4308 0.026 Uiso 0.50 1 calc PR . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Mo1 0.0125(3) 0.0136(2) 0.0107(2) 0.00140(18) 0.000 0.000
Cl1 0.0205(5) 0.0239(5) 0.0163(5) 0.0002(4) 0.0042(4) 0.0048(4)
Cl2 0.0136(7) 0.0178(6) 0.0164(6) 0.000 0.000 -0.0038(5)
O1 0.021(2) 0.022(2) 0.018(2) 0.0046(17) 0.000 0.000
O2 0.014(3) 0.010(3) 0.019(3) 0.000 0.000 0.000
C1 0.013(4) 0.019(4) 0.026(4) 0.000 0.000 0.000
Mo2 0.0122(3) 0.0105(2) 0.0142(3) -0.00017(18) 0.000 0.000
Cl3 0.0119(6) 0.0189(7) 0.0175(6) 0.0023(5) 0.000 0.000
Cl4 0.0165(5) 0.0211(5) 0.0191(5) 0.0039(4) -0.0040(4) -0.0001(4)
O4 0.022(2) 0.014(2) 0.0163(19) -0.0001(16) 0.000 0.000
O5 0.020(2) 0.0128(19) 0.019(2) -0.0020(16) 0.000 0.000
O6 0.073(4) 0.013(2) 0.017(2) 0.0022(18) 0.000 0.000
C3 0.016(3) 0.017(3) 0.020(3) -0.004(2) 0.000 0.000
C4 0.021(3) 0.017(3) 0.015(3) 0.001(2) 0.000 0.000

_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 O1 1.644(4) . ?
Mo1 Cl1 2.2939(10) 12 ?
Mo1 Cl1 2.2939(10) . ?
Mo1 O2 2.442(4) . ?
Mo1 Cl2 2.4776(10) 3_556 ?
Mo1 Cl2 2.4776(10) . ?
Cl2 Mo1 2.4776(10) 10_557 ?
O2 C1 1.241(10) . ?
O2 Mo1 2.442(4) 10_557 ?
C1 O3 1.356(8) 10_557 ?
C1 O3 1.356(8) 3_556 ?
C1 O3 1.356(8) . ?
C1 O3 1.356(8) 12 ?
C1 C2 1.488(9) 12 ?
C1 C2 1.488(9) . ?
C1 C2 1.488(9) 3_556 ?
C1 C2 1.488(9) 10_557 ?
O3 H3 0.8400 . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
Mo2 O4 1.657(4) . ?
Mo2 O5 2.205(4) . ?
Mo2 Cl4 2.3475(10) . ?
Mo2 Cl4 2.3475(10) 12_655 ?
Mo2 Cl3 2.4321(11) 9_676 ?
Mo2 Cl3 2.4321(11) . ?
Mo2 Mo2 3.1246(10) 9_676 ?
Cl3 Mo2 2.4321(11) 9_676 ?
O5 C3 1.217(7) . ?
O6 C3 1.332(7) . ?
O6 H6 0.86(2) . ?
C3 C4 1.479(8) . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?

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 Mo1 Cl1 102.63(10) . 12 ?
O1 Mo1 Cl1 102.63(10) . . ?
Cl1 Mo1 Cl1 94.62(6) 12 . ?
O1 Mo1 O2 167.69(17) . . ?
Cl1 Mo1 O2 85.60(7) 12 . ?
Cl1 Mo1 O2 85.60(7) . . ?
O1 Mo1 Cl2 98.14(11) . 3_556 ?
Cl1 Mo1 Cl2 88.84(4) 12 3_556 ?
Cl1 Mo1 Cl2 157.62(4) . 3_556 ?
O2 Mo1 Cl2 72.61(7) . 3_556 ?
O1 Mo1 Cl2 98.14(12) . . ?
Cl1 Mo1 Cl2 157.62(4) 12 . ?
Cl1 Mo1 Cl2 88.84(4) . . ?
O2 Mo1 Cl2 72.61(7) . . ?
Cl2 Mo1 Cl2 80.00(5) 3_556 . ?
Mo1 Cl2 Mo1 89.85(5) . 10_557 ?
C1 O2 Mo1 134.24(9) . 10_557 ?
C1 O2 Mo1 134.24(9) . . ?
Mo1 O2 Mo1 91.52(18) 10_557 . ?
O2 C1 O3 119.1(7) . 10_557 ?
O2 C1 O3 119.1(7) . 3_556 ?
O3 C1 O3 6(5) 10_557 3_556 ?
O2 C1 O3 119.1(7) . . ?
O3 C1 O3 121.5(11) 10_557 . ?
O3 C1 O3 121.8(13) 3_556 . ?
O2 C1 O3 119.1(7) . 12 ?
O3 C1 O3 121.8(13) 10_557 12 ?
O3 C1 O3 121.5(11) 3_556 12 ?
O3 C1 O3 6(5) . 12 ?
O2 C1 C2 128.1(8) . 12 ?
O3 C1 C2 10.7(19) 10_557 12 ?
O3 C1 C2 14.3(19) 3_556 12 ?
O3 C1 C2 111.6(8) . 12 ?
O3 C1 C2 112.4(9) 12 12 ?
O2 C1 C2 128.1(8) . . ?
O3 C1 C2 14.3(19) 10_557 . ?
O3 C1 C2 10.7(18) 3_556 . ?
O3 C1 C2 112.4(9) . . ?
O3 C1 C2 111.6(8) 12 . ?
C2 C1 C2 16(2) 12 . ?
O2 C1 C2 128.1(8) . 3_556 ?
O3 C1 C2 111.6(8) 10_557 3_556 ?
O3 C1 C2 112.4(9) 3_556 3_556 ?
O3 C1 C2 10.7(19) . 3_556 ?
O3 C1 C2 14.3(19) 12 3_556 ?
C2 C1 C2 101.5(17) 12 3_556 ?
C2 C1 C2 103.8(16) . 3_556 ?
O2 C1 C2 128.1(8) . 10_557 ?
O3 C1 C2 112.4(9) 10_557 10_557 ?
O3 C1 C2 111.6(8) 3_556 10_557 ?
O3 C1 C2 14.3(19) . 10_557 ?
O3 C1 C2 10.7(18) 12 10_557 ?
C2 C1 C2 103.8(16) 12 10_557 ?
C2 C1 C2 101.5(17) . 10_557 ?
C2 C1 C2 16(2) 3_556 10_557 ?
C1 O3 H3 109.5 . . ?
C1 C2 H2A 109.5 . . ?
C1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
C1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
O4 Mo2 O5 171.83(17) . . ?
O4 Mo2 Cl4 99.90(10) . . ?
O5 Mo2 Cl4 86.09(8) . . ?
O4 Mo2 Cl4 99.90(10) . 12_655 ?
O5 Mo2 Cl4 86.09(8) . 12_655 ?
Cl4 Mo2 Cl4 84.98(5) . 12_655 ?
O4 Mo2 Cl3 93.54(9) . 9_676 ?
O5 Mo2 Cl3 81.26(7) . 9_676 ?
Cl4 Mo2 Cl3 164.92(3) . 9_676 ?
Cl4 Mo2 Cl3 86.00(3) 12_655 9_676 ?
O4 Mo2 Cl3 93.54(9) . . ?
O5 Mo2 Cl3 81.26(7) . . ?
Cl4 Mo2 Cl3 86.00(3) . . ?
Cl4 Mo2 Cl3 164.92(3) 12_655 . ?
Cl3 Mo2 Cl3 100.06(4) 9_676 . ?
O4 Mo2 Mo2 95.52(14) . 9_676 ?
O5 Mo2 Mo2 76.31(11) . 9_676 ?
Cl4 Mo2 Mo2 134.21(3) . 9_676 ?
Cl4 Mo2 Mo2 134.21(3) 12_655 9_676 ?
Cl3 Mo2 Mo2 50.03(2) 9_676 9_676 ?
Cl3 Mo2 Mo2 50.03(2) . 9_676 ?
Mo2 Cl3 Mo2 79.94(4) 9_676 . ?
C3 O5 Mo2 146.7(4) . . ?
C3 O6 H6 115(6) . . ?
O5 C3 O6 122.3(5) . . ?
O5 C3 C4 122.6(5) . . ?
O6 C3 C4 115.0(5) . . ?
C3 C4 H4A 109.5 . . ?
C3 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
C3 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O1 Mo1 Cl2 Mo1 130.08(10) . . . 10_557 ?
Cl1 Mo1 Cl2 Mo1 -27.98(13) 12 . . 10_557 ?
Cl1 Mo1 Cl2 Mo1 -127.33(4) . . . 10_557 ?
O2 Mo1 Cl2 Mo1 -41.58(7) . . . 10_557 ?
Cl2 Mo1 Cl2 Mo1 33.19(6) 3_556 . . 10_557 ?
O1 Mo1 O2 C1 180.000(10) . . . . ?
Cl1 Mo1 O2 C1 47.49(3) 12 . . . ?
Cl1 Mo1 O2 C1 -47.49(3) . . . . ?
Cl2 Mo1 O2 C1 137.66(4) 3_556 . . . ?
Cl2 Mo1 O2 C1 -137.66(4) . . . . ?
O1 Mo1 O2 Mo1 0.000(8) . . . 10_557 ?
Cl1 Mo1 O2 Mo1 -132.51(3) 12 . . 10_557 ?
Cl1 Mo1 O2 Mo1 132.51(3) . . . 10_557 ?
Cl2 Mo1 O2 Mo1 -42.34(4) 3_556 . . 10_557 ?
Cl2 Mo1 O2 Mo1 42.34(4) . . . 10_557 ?
Mo1 O2 C1 O3 3(3) 10_557 . . 10_557 ?
Mo1 O2 C1 O3 -177(3) . . . 10_557 ?
Mo1 O2 C1 O3 -3(3) 10_557 . . 3_556 ?
Mo1 O2 C1 O3 177(3) . . . 3_556 ?
Mo1 O2 C1 O3 177(3) 10_557 . . . ?
Mo1 O2 C1 O3 -3(3) . . . . ?
Mo1 O2 C1 O3 -177(3) 10_557 . . 12 ?
Mo1 O2 C1 O3 3(3) . . . 12 ?
Mo1 O2 C1 C2 10.2(15) 10_557 . . 12 ?
Mo1 O2 C1 C2 -169.8(15) . . . 12 ?
Mo1 O2 C1 C2 -10.2(15) 10_557 . . . ?
Mo1 O2 C1 C2 169.8(15) . . . . ?
Mo1 O2 C1 C2 169.8(15) 10_557 . . 3_556 ?
Mo1 O2 C1 C2 -10.2(15) . . . 3_556 ?
Mo1 O2 C1 C2 -169.8(15) 10_557 . . 10_557 ?
Mo1 O2 C1 C2 10.2(15) . . . 10_557 ?
O4 Mo2 Cl3 Mo2 -94.24(10) . . . 9_676 ?
O5 Mo2 Cl3 Mo2 79.43(8) . . . 9_676 ?
Cl4 Mo2 Cl3 Mo2 166.08(3) . . . 9_676 ?
Cl4 Mo2 Cl3 Mo2 112.72(14) 12_655 . . 9_676 ?
Cl3 Mo2 Cl3 Mo2 0.0 9_676 . . 9_676 ?
O4 Mo2 O5 C3 180.000(7) . . . . ?
Cl4 Mo2 O5 C3 42.61(3) . . . . ?
Cl4 Mo2 O5 C3 -42.61(3) 12_655 . . . ?
Cl3 Mo2 O5 C3 -129.16(3) 9_676 . . . ?
Cl3 Mo2 O5 C3 129.16(3) . . . . ?
Mo2 Mo2 O5 C3 180.000(5) 9_676 . . . ?
Mo2 O5 C3 O6 0.000(6) . . . . ?
Mo2 O5 C3 C4 180.000(4) . . . . ?

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
O3 H3 Cl1 0.84 2.48 3.25(4) 152.2 12
O6 H6 O1 0.86(2) 2.32(6) 3.018(6) 138(7) 13_576
O6 H6 Cl4 0.86(2) 2.82(5) 3.439(4) 130(5) 12_655
O6 H6 Cl4 0.86(2) 2.82(5) 3.439(4) 130(5) .

_diffrn_measured_fraction_theta_max 0.973
_diffrn_reflns_theta_full        25.03
_diffrn_measured_fraction_theta_full 0.973
_refine_diff_density_max         0.625
_refine_diff_density_min         -0.747
_refine_diff_density_rms         0.121
_database_code_depnum_ccdc_archive 'CCDC 1015025'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_1b

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C4 H2 Cl12 Mo2 O6'
_chemical_formula_weight         763.34

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'
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'
Mo Mo -1.6832 0.6857 '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'

_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                   5.9376(17)
_cell_length_b                   7.406(2)
_cell_length_c                   12.038(4)
_cell_angle_alpha                83.082(3)
_cell_angle_beta                 88.495(3)
_cell_angle_gamma                75.691(3)
_cell_volume                     509.2(3)
_cell_formula_units_Z            1
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    3644
_cell_measurement_theta_min      2.8585
_cell_measurement_theta_max      278.2455

_exptl_crystal_description       plate
_exptl_crystal_colour            yellow-green
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.12
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.489
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             362
_exptl_absorpt_coefficient_mu    2.824
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.5755
_exptl_absorpt_correction_T_max  0.7281
_exptl_absorpt_process_details   
;
 Data were corrected for Lorentz polarization and absorption
 effects (empirical absorption corrections SADABS).
 R(int) = 0.1257 (selected reflections only, before parameter refinement)
 R(int) = 0.0637 (selected reflections only, after parameter refinement)
;

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            5458
_diffrn_reflns_av_R_equivalents  0.0413
_diffrn_reflns_av_sigmaI/netI    0.0486
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         1.70
_diffrn_reflns_theta_max         27.00
_reflns_number_total             2208
_reflns_number_gt                2008
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX2 (Bruker AXS, 2006)'
_computing_cell_refinement       'APEX2 (Bruker AXS, 2006)'
_computing_data_reduction        'SAINT (Bruker AXS, 2004)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'ORTEPII (Johnson, 1996)'
_computing_publication_material  'XCIF (Bruker AXS, 2001)'

_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)+(0.0764P)²+0.4225P] 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         2208
_refine_ls_number_parameters     109
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0477
_refine_ls_R_factor_gt           0.0434
_refine_ls_wR_factor_ref         0.1183
_refine_ls_wR_factor_gt          0.1149
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_restrained_S_all      1.060
_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 0.36633(6) 0.65630(5) 0.57460(3) 0.01709(16) Uani 1 1 d . . .
Cl1 Cl 0.28629(17) 0.36452(15) 0.53768(8) 0.0179(2) Uani 1 1 d . . .
Cl2 Cl 0.11361(18) 0.64387(16) 0.72585(9) 0.0216(3) Uani 1 1 d . . .
Cl3 Cl 0.48246(18) 0.89479(15) 0.65563(9) 0.0208(3) Uani 1 1 d . . .
O1 O 0.1880(6) 0.7889(5) 0.4785(3) 0.0247(7) Uani 1 1 d . . .
O2 O 0.6292(5) 0.4562(4) 0.6988(3) 0.0187(6) Uani 1 1 d . . .
O3 O 0.6360(6) 0.5936(5) 0.8549(3) 0.0243(7) Uani 1 1 d . . .
H3 H 0.5757 0.6923 0.8132 0.036 Uiso 1 1 calc R . .
C2 C 0.7881(8) 0.2626(6) 0.8650(4) 0.0196(9) Uani 1 1 d . . .
C1 C 0.6764(7) 0.4526(6) 0.7975(4) 0.0176(9) Uani 1 1 d . . .
Cl4 Cl 0.9932(2) 0.12492(17) 0.78245(10) 0.0294(3) Uani 1 1 d . . .
Cl5 Cl 0.9192(2) 0.28735(18) 0.98918(10) 0.0325(3) Uani 1 1 d . . .
Cl6 Cl 0.5505(2) 0.1597(2) 0.89668(12) 0.0368(3) Uani 1 1 d . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Mo1 0.0136(2) 0.0193(2) 0.0168(2) 0.00586(16) -0.00087(15) -0.00496(15)
Cl1 0.0155(5) 0.0183(5) 0.0183(5) 0.0012(4) 0.0021(4) -0.0031(4)
Cl2 0.0174(5) 0.0251(6) 0.0217(5) -0.0005(4) 0.0050(4) -0.0057(4)
Cl3 0.0214(5) 0.0163(5) 0.0234(5) 0.0011(4) 0.0006(4) -0.0037(4)
O1 0.0192(16) 0.0289(19) 0.0245(17) 0.0054(14) -0.0039(13) -0.0069(13)
O2 0.0163(15) 0.0206(16) 0.0178(15) 0.0021(13) -0.0017(12) -0.0039(12)
O3 0.0281(18) 0.0193(17) 0.0217(16) 0.0000(13) -0.0006(14) 0.0000(13)
C2 0.022(2) 0.020(2) 0.015(2) 0.0016(18) 0.0018(17) -0.0046(17)
C1 0.0123(18) 0.020(2) 0.021(2) 0.0034(17) 0.0033(16) -0.0076(16)
Cl4 0.0318(6) 0.0248(6) 0.0229(6) 0.0014(5) 0.0029(5) 0.0070(5)
Cl5 0.0419(7) 0.0299(7) 0.0220(6) -0.0001(5) -0.0124(5) -0.0015(5)
Cl6 0.0330(7) 0.0374(8) 0.0417(7) 0.0119(6) 0.0037(6) -0.0200(6)

_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 O1 1.643(3) . ?
Mo1 O2 2.306(3) . ?
Mo1 Cl2 2.3366(12) . ?
Mo1 Cl3 2.3662(12) . ?
Mo1 Cl1 2.4173(13) . ?
Mo1 Cl1 2.4190(12) 2_666 ?
Mo1 Mo1 3.1845(9) 2_666 ?
Cl1 Mo1 2.4190(12) 2_666 ?
O2 C1 1.224(5) . ?
O3 C1 1.291(5) . ?
O3 H3 0.8400 . ?
C2 C1 1.540(6) . ?
C2 Cl5 1.753(4) . ?
C2 Cl4 1.754(4) . ?
C2 Cl6 1.775(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
O1 Mo1 O2 175.57(14) . . ?
O1 Mo1 Cl2 100.88(12) . . ?
O2 Mo1 Cl2 82.48(8) . . ?
O1 Mo1 Cl3 98.85(12) . . ?
O2 Mo1 Cl3 84.14(8) . . ?
Cl2 Mo1 Cl3 87.10(4) . . ?
O1 Mo1 Cl1 95.47(12) . . ?
O2 Mo1 Cl1 81.85(8) . . ?
Cl2 Mo1 Cl1 85.53(4) . . ?
Cl3 Mo1 Cl1 164.90(4) . . ?
O1 Mo1 Cl1 95.70(12) . 2_666 ?
O2 Mo1 Cl1 81.22(8) . 2_666 ?
Cl2 Mo1 Cl1 162.76(4) . 2_666 ?
Cl3 Mo1 Cl1 85.71(4) . 2_666 ?
Cl1 Mo1 Cl1 97.64(4) . 2_666 ?
O1 Mo1 Mo1 98.50(12) . 2_666 ?
O2 Mo1 Mo1 77.08(8) . 2_666 ?
Cl2 Mo1 Mo1 131.78(4) . 2_666 ?
Cl3 Mo1 Mo1 132.53(4) . 2_666 ?
Cl1 Mo1 Mo1 48.84(3) . 2_666 ?
Cl1 Mo1 Mo1 48.79(3) 2_666 2_666 ?
Mo1 Cl1 Mo1 82.36(4) . 2_666 ?
C1 O2 Mo1 134.7(3) . . ?
C1 O3 H3 109.5 . . ?
C1 C2 Cl5 112.6(3) . . ?
C1 C2 Cl4 110.0(3) . . ?
Cl5 C2 Cl4 109.8(2) . . ?
C1 C2 Cl6 103.7(3) . . ?
Cl5 C2 Cl6 109.8(2) . . ?
Cl4 C2 Cl6 110.7(2) . . ?
O2 C1 O3 126.7(4) . . ?
O2 C1 C2 118.8(4) . . ?
O3 C1 C2 114.4(4) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O1 Mo1 Cl1 Mo1 96.51(12) . . . 2_666 ?
O2 Mo1 Cl1 Mo1 -79.93(8) . . . 2_666 ?
Cl2 Mo1 Cl1 Mo1 -162.96(4) . . . 2_666 ?
Cl3 Mo1 Cl1 Mo1 -101.95(14) . . . 2_666 ?
Cl1 Mo1 Cl1 Mo1 0.0 2_666 . . 2_666 ?
O1 Mo1 O2 C1 175.8(17) . . . . ?
Cl2 Mo1 O2 C1 -44.7(4) . . . . ?
Cl3 Mo1 O2 C1 43.2(4) . . . . ?
Cl1 Mo1 O2 C1 -131.2(4) . . . . ?
Cl1 Mo1 O2 C1 129.7(4) 2_666 . . . ?
Mo1 Mo1 O2 C1 179.3(4) 2_666 . . . ?
Mo1 O2 C1 O3 -22.6(7) . . . . ?
Mo1 O2 C1 C2 155.1(3) . . . . ?
Cl5 C2 C1 O2 162.7(3) . . . . ?
Cl4 C2 C1 O2 39.8(5) . . . . ?
Cl6 C2 C1 O2 -78.6(4) . . . . ?
Cl5 C2 C1 O3 -19.3(5) . . . . ?
Cl4 C2 C1 O3 -142.1(3) . . . . ?
Cl6 C2 C1 O3 99.4(4) . . . . ?

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
O3 H3 Cl3 0.84 2.26 3.063(4) 159.6 .

_diffrn_measured_fraction_theta_max 0.988
_diffrn_reflns_theta_full        27.00
_diffrn_measured_fraction_theta_full 0.988
_refine_diff_density_max         2.306
_refine_diff_density_min         -1.474
_refine_diff_density_rms         0.208
_database_code_depnum_ccdc_archive 'CCDC 1015026'
