# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2018

####################################################################### 
# 
# 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_mo_160906b_5
_database_code_depnum_ccdc_archive 'CCDC 1546785'
_audit_update_record             
;
2018-02-07 deposited with the CCDC.
2018-02-28 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C2 H5 O6 S Sb2'
_chemical_formula_weight         400.62

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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P2(1)/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                   12.330(3)
_cell_length_b                   10.154(3)
_cell_length_c                   6.0161(15)
_cell_angle_alpha                90.00
_cell_angle_beta                 102.499(9)
_cell_angle_gamma                90.00
_cell_volume                     735.4(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    273(2)
_cell_measurement_reflns_used    4281
_cell_measurement_theta_min      6.770
_cell_measurement_theta_max      54.917

_exptl_crystal_description       plate
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.01
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    3.619
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             732
_exptl_absorpt_coefficient_mu    7.612
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.06185
_exptl_absorpt_correction_T_max  0.09491
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      273(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'
_diffrn_measurement_method       ω/2θ-scans
_diffrn_detector_area_resol_mean 83.33
_diffrn_standards_number         .
_diffrn_standards_interval_count .
_diffrn_standards_interval_time  .
_diffrn_standards_decay_%        .
_diffrn_reflns_number            1620
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0379
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_theta_min         3.38
_diffrn_reflns_theta_max         27.50
_reflns_number_total             1620
_reflns_number_gt                1462
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX-II v2.1-4'
_computing_cell_refinement       'Bruker SAINT v7.34'
_computing_data_reduction        'Bruker SAINT v7.34'
_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)+(0.0673P)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    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         1620
_refine_ls_number_parameters     105
_refine_ls_number_restraints     7
_refine_ls_R_factor_all          0.0413
_refine_ls_R_factor_gt           0.0354
_refine_ls_wR_factor_ref         0.0962
_refine_ls_wR_factor_gt          0.0939
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_restrained_S_all      1.055
_refine_ls_shift/su_max          0.035
_refine_ls_shift/su_mean         0.004

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
Sb1 Sb 0.72727(5) 0.65289(5) 0.52446(12) 0.01406(17) Uani 1 1 d . . .
C1 C 0.9240(8) 0.3870(9) 0.244(2) 0.027(2) Uani 1 1 d . . .
H1A H 0.9027 0.2951 0.2468 0.032 Uiso 1 1 calc R . .
H1B H 0.9833 0.3928 0.1620 0.032 Uiso 1 1 calc R . .
S1 S 0.80830(19) 0.4779(2) 0.0931(5) 0.0210(5) Uani 1 1 d . . .
O1 O 0.7227(5) 0.4715(6) 0.2297(12) 0.0225(15) Uani 1 1 d . . .
C2 C 0.9687(8) 0.4326(9) 0.489(2) 0.024(2) Uani 1 1 d . . .
H2A H 1.0189 0.3659 0.5682 0.029 Uiso 1 1 calc R . .
H2B H 0.9071 0.4396 0.5652 0.029 Uiso 1 1 calc R . .
Sb2 Sb 0.49653(5) 0.59920(5) 0.73010(10) 0.01627(18) Uani 1 1 d . . .
O2 O 0.8476(6) 0.6140(7) 0.0793(16) 0.0309(19) Uani 1 1 d . . .
O3 O 0.7693(6) 0.4148(9) -0.1261(15) 0.0375(19) Uani 1 1 d . . .
O4 O 0.6512(4) 0.7615(6) 0.2610(12) 0.0148(12) Uani 1 1 d U . .
O5 O 0.5864(5) 0.5536(5) 0.4923(13) 0.0154(13) Uani 1 1 d . . .
O6 O 0.4137(6) 0.7329(6) 0.5332(14) 0.0240(15) Uani 1 1 d D . .
H6 H 0.439(13) 0.774(18) 0.656(19) 0.10(7) Uiso 1 1 d 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
Sb1 0.0148(3) 0.0146(3) 0.0126(3) 0.0013(3) 0.0026(3) 0.0006(2)
C1 0.019(4) 0.026(4) 0.036(7) -0.006(5) 0.007(5) 0.003(4)
S1 0.0217(11) 0.0241(11) 0.0156(13) -0.0008(11) 0.0007(11) 0.0021(8)
O1 0.014(3) 0.031(3) 0.022(4) -0.010(3) 0.003(4) 0.001(2)
C2 0.030(5) 0.026(4) 0.018(5) 0.004(5) 0.006(5) 0.003(4)
Sb2 0.0235(3) 0.0150(3) 0.0112(3) 0.0017(3) 0.0058(4) 0.0013(2)
O2 0.027(3) 0.028(3) 0.035(5) 0.016(4) 0.000(4) 0.000(3)
O3 0.034(4) 0.057(5) 0.019(4) -0.007(5) -0.002(4) 0.004(3)
O4 0.0151(14) 0.0152(14) 0.0140(16) 0.0009(10) 0.0030(10) 0.0004(9)
O5 0.012(3) 0.018(3) 0.017(3) -0.005(3) 0.005(3) -0.007(2)
O6 0.035(3) 0.019(3) 0.019(4) 0.007(3) 0.007(4) 0.006(3)

_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
Sb1 O5 1.981(5) . ?
Sb1 O4 1.991(6) . ?
Sb1 O4 2.059(7) 4_576 ?
Sb1 O1 2.549(7) . ?
C1 C2 1.529(17) . ?
C1 S1 1.775(10) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
S1 O3 1.452(9) . ?
S1 O2 1.473(7) . ?
S1 O1 1.472(7) . ?
C2 C2 1.563(17) 3_766 ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
Sb2 O6 1.941(7) . ?
Sb2 O5 2.044(7) . ?
Sb2 O5 2.156(6) 3_666 ?
Sb2 O4 2.349(5) 4_576 ?
Sb2 H6 1.93(19) . ?
O4 Sb1 2.059(7) 4_575 ?
O4 Sb2 2.349(5) 4_575 ?
O5 Sb2 2.156(6) 3_666 ?
O6 H6 0.849(10) . ?

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
O5 Sb1 O4 87.3(2) . . ?
O5 Sb1 O4 76.2(2) . 4_576 ?
O4 Sb1 O4 96.29(14) . 4_576 ?
O5 Sb1 O1 71.2(2) . . ?
O4 Sb1 O1 84.9(2) . . ?
O4 Sb1 O1 147.3(2) 4_576 . ?
C2 C1 S1 114.8(7) . . ?
C2 C1 H1A 108.6 . . ?
S1 C1 H1A 108.6 . . ?
C2 C1 H1B 108.6 . . ?
S1 C1 H1B 108.6 . . ?
H1A C1 H1B 107.6 . . ?
O3 S1 O2 114.3(5) . . ?
O3 S1 O1 110.5(4) . . ?
O2 S1 O1 110.9(5) . . ?
O3 S1 C1 107.9(5) . . ?
O2 S1 C1 106.2(4) . . ?
O1 S1 C1 106.5(5) . . ?
S1 O1 Sb1 116.5(3) . . ?
C1 C2 C2 114.4(12) . 3_766 ?
C1 C2 H2A 108.7 . . ?
C2 C2 H2A 108.7 3_766 . ?
C1 C2 H2B 108.7 . . ?
C2 C2 H2B 108.6 3_766 . ?
H2A C2 H2B 107.6 . . ?
O6 Sb2 O5 91.4(3) . . ?
O6 Sb2 O5 90.5(3) . 3_666 ?
O5 Sb2 O5 70.0(2) . 3_666 ?
O6 Sb2 O4 86.5(3) . 4_576 ?
O5 Sb2 O4 68.8(2) . 4_576 ?
O5 Sb2 O4 138.6(3) 3_666 4_576 ?
O6 Sb2 H6 25.3(13) . . ?
O5 Sb2 H6 106(5) . . ?
O5 Sb2 H6 114.7(19) 3_666 . ?
O4 Sb2 H6 73(5) 4_576 . ?
Sb1 O4 Sb1 125.3(2) . 4_575 ?
Sb1 O4 Sb2 129.1(3) . 4_575 ?
Sb1 O4 Sb2 100.0(2) 4_575 4_575 ?
Sb1 O5 Sb2 114.4(3) . . ?
Sb1 O5 Sb2 135.6(4) . 3_666 ?
Sb2 O5 Sb2 110.0(2) . 3_666 ?
Sb2 O6 H6 77(10) . . ?

_diffrn_measured_fraction_theta_max 0.958
_diffrn_reflns_theta_full        27.50
_diffrn_measured_fraction_theta_full 0.958
_refine_diff_density_max         1.512
_refine_diff_density_min         -1.303
_refine_diff_density_rms         0.295
