# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2016

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_1
_database_code_depnum_ccdc_archive 'CCDC 1438075'
_audit_update_record             
;
2016-04-04 deposited with the CCDC.
2016-08-11 downloaded from the CCDC.
;

_exptl_special_details           
; 
 The crystal was 
placed in the cold stream of an Oxford 
Cryosystems open-flow nitrogen cryostat (Cosier & 
Glazer, 1986) with a nominal stability of 0.1K. 
 
Cosier, J. & Glazer, A.M., 1986. J. Appl. Cryst. 105-107. 
;
_refine_special_details          
; 
? 
;
#--------------------------------------------------------------- 
# _oxford_ data items, April 2010: 
# There is some uncertainty about the correct way of forming local data 
# names, e.g. 

# _atom_site_special_shape_oxford 
# or 
# _oxford_atom_site_special_shape 

# see: 
# http://www.iucr.org/resources/cif/spec/version1.1/semantics#namespace 

# A reserved prefix, e.g. foo, must be used in the following way 
# " If the data file contains items defined in a DDL1 dictionary, the 
# local data names assigned under the reserved prefix must contain it as 
# their first component, e.g. _foo_atom_site_my_item. " 

# However, this seems to say the opposite: 
# http://www.iucr.org/__data/iucr/cif/standard/cifstd8.html 

# According to advice from the IUCr, CRYSTALS is correct 
#--------------------------------------------------------------- 
# End of 'script/refcif.dat' 
#end of refcif 
_cell_length_a                   5.1039(1)
_cell_length_b                   16.8784(1)
_cell_length_c                   6.6915(1)
_cell_angle_alpha                90
_cell_angle_beta                 105.28(1)
_cell_angle_gamma                90
_cell_volume                     556.066(14)

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/m '
_symmetry_space_group_name_Hall  '-P 2yb'
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
x,-y+1/2,z
-x,y+1/2,-z

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
Hg -0.8800 6.2990 20.6809 0.5450 19.0417 8.4484 21.6575 1.5729 5.9676 38.3246
12.6089 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
C 0.0020 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
O 0.0060 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089
0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
S 0.0830 0.1234 6.9053 1.4679 5.2034 22.2151 1.4379 0.2536 1.5863 56.1720
0.0760 'International Tables Vol C 4.2.6.8 and 6.1.1.4'


_cell_formula_units_Z            2

# Given Formula = C16 H16 Hg4 O8 S2 
# Dc =      7.18 Fooo =    528.00 Mu =    303.61 M =    601.40
# Found Formula = C8 H8 Hg2 O4 S1 
# Dc =      3.59 FOOO =    528.00 Mu =    151.80 M =    300.70

_chemical_formula_sum            'C8 H8 Hg2 O4 S1'
_chemical_formula_moiety         'C8 H8 Hg2 O4 S1'
_chemical_compound_source        ?
_chemical_formula_weight         601.40


_cell_measurement_reflns_used    6388
_cell_measurement_theta_min      3
_cell_measurement_theta_max      21
_cell_measurement_temperature    293

_exptl_crystal_description       plate
_exptl_crystal_colour            colorless
_exptl_crystal_size_min          0.034
_exptl_crystal_size_mid          0.113
_exptl_crystal_size_max          0.135

_exptl_crystal_density_diffrn    3.592
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             528
_exptl_absorpt_coefficient_mu    15.180

# Sheldrick geometric approximatio 0.04 0.39 
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_absorpt_correction_T_min  0.04
_exptl_absorpt_correction_T_max  0.39
# For a Kappa CCD, set Tmin to 1.0 and 
# Tmax to the ratio of max:min frame scales in scale_all.log 
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_device       Area
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Ag K\a'
_diffrn_radiation_wavelength     0.56087
_diffrn_measurement_method       ω

# If a reference occurs more than once, delete the author 
# and date from subsequent references. 
_computing_data_collection       'COLLECT (Nonius, 2001).'
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_structure_solution    'Superflip (Palatinus & Chapuis, 2007)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'

_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_number         0
_diffrn_standards_decay_%        ?

_diffrn_ambient_temperature      293
_diffrn_reflns_number            6526
_reflns_number_total             1325
_diffrn_reflns_av_R_equivalents  0.091
# Number of reflections without Friedels Law is 2460 
# Number of reflections with Friedels Law is 1325 
# Theoretical number of reflections is about 1284 


_diffrn_reflns_theta_min         2.666
_diffrn_reflns_theta_max         21.410
_diffrn_measured_fraction_theta_max 0.997

_diffrn_reflns_theta_full        21.410
_diffrn_measured_fraction_theta_full 0.997


_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_limit_l_max       8
_reflns_limit_h_min              -6
_reflns_limit_h_max              6
_reflns_limit_k_min              0
_reflns_limit_k_max              21
_reflns_limit_l_min              0
_reflns_limit_l_max              8

_oxford_diffrn_Wilson_B_factor   2.49
_oxford_diffrn_Wilson_scale      34.31

_atom_sites_solution_primary     Other #heavy,direct,difmap,geom
# _atom_sites_solution_secondary  difmap
_atom_sites_solution_hydrogens   difmap

_refine_diff_density_min         -4.75
_refine_diff_density_max         4.18


# The current dictionary definitions do not cover the 
# situation where the reflections used for refinement were 
# selected by a user-defined sigma threshold 


# The values actually used during refinement 
_oxford_reflns_threshold_expression_ref I>3.0\s(I)
_refine_ls_number_reflns         931
_refine_ls_number_restraints     12
_refine_ls_number_parameters     70
_oxford_refine_ls_R_factor_ref   0.0778
_refine_ls_wR_factor_ref         0.0854
_refine_ls_goodness_of_fit_ref   1.0766
_refine_ls_shift/su_max          0.0001482
_refine_ls_shift/su_mean         0.0000050


# The values computed with all filters except I/sigma 
_oxford_reflns_number_all        1323
_refine_ls_R_factor_all          0.1126
_refine_ls_wR_factor_all         0.1087

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                1046
_refine_ls_R_factor_gt           0.0915
_refine_ls_wR_factor_gt          0.0935

# choose from: rm (reference molecule of known chirality), 
# ad (anomolous dispersion - Flack), rmad (rm and ad), 
# syn (from synthesis), unk (unknown) or . (not applicable). 
_chemical_absolute_configuration .


_refine_ls_structure_factor_coef F
_refine_ls_matrix_type           full
_refine_ls_hydrogen_treatment    constr #undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A₀*T₀(x)+A₁*T₁(x) ... +Aₙ₋₁]*Tₙ₋₁(x)] 
 where Ai are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)²]² 
 Ai are: 
 2.70 1.46 1.96 0.361 
;

# Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3

# Replace last . with number of unfound hydrogen atoms attached to an atom.

# ..._refinement_flags_... 
# . no refinement constraints           S special position constraint on site
# G rigid group refinement of site      R riding atom
# D distance or angle restraint on site T thermal displacement constraints
# U Uiso or Uij restraint (rigid bond)  P partial occupancy constraint


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_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_attached_hydrogens
Hg1 Hg 0.10409(15) 0.43746(5) 0.26392(12) 0.0348 1.0000 Uani . . . . . .
S1 S 0.153(2) 0.2500 0.2020(15) 0.0434 1.0000 Uani S TU . . . .
C1 C 0.019(5) 0.3268(14) 0.312(4) 0.0393 1.0000 Uani . U . . . .
C3 C -0.133(5) 0.2945(10) 0.433(4) 0.0425 1.0000 Uani . U . . . .
O1 O 0.206(3) 0.5486(9) 0.185(3) 0.0385 1.0000 Uani . . . . . .
O2 O 0.626(3) 0.5065(13) 0.298(3) 0.0524 1.0000 Uani . . . . . .
C2 C 0.459(6) 0.5565(14) 0.212(4) 0.0407 1.0000 Uani . U . . . .
C5 C 0.550(6) 0.6348(16) 0.146(5) 0.0522 1.0000 Uani . . . . . .
H31 H -0.2268 0.3250 0.5079 0.0500 1.0000 Uiso R . . . . .
H52 H 0.7445 0.6385 0.1932 0.0741 1.0000 Uiso R . . . . .
H53 H 0.4704 0.6769 0.2064 0.0740 1.0000 Uiso R . . . . .
H51 H 0.4945 0.6392 -0.0018 0.0740 1.0000 Uiso R . . . . .
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
Hg1 0.0314(5) 0.0338(5) 0.0381(5) 0.0021(4) 0.0074(3) 0.0007(4)
S1 0.058(5) 0.032(4) 0.048(4) 0.0000 0.028(4) 0.0000
C1 0.047(8) 0.031(8) 0.038(7) -0.006(7) 0.009(7) 0.000(7)
C3 0.046(12) 0.012(11) 0.080(17) -0.002(10) 0.035(12) -0.004(8)
O1 0.029(7) 0.037(9) 0.052(9) 0.007(7) 0.016(7) 0.011(6)
O2 0.027(8) 0.065(14) 0.068(13) 0.005(9) 0.017(9) 0.005(7)
C2 0.052(8) 0.030(8) 0.042(8) 0.002(7) 0.016(7) -0.003(7)
C5 0.061(16) 0.031(12) 0.061(16) 0.000(11) 0.011(13) -0.018(12)

_refine_ls_extinction_method     None
_oxford_refine_ls_scale          0.2710(18)
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Hg1 . O1 2_565 3.014(17) yes
Hg1 . C1 . 1.96(2) yes
Hg1 . O1 . 2.052(16) yes
S1 . C1 3_555 1.72(2) yes
S1 . C1 . 1.72(2) yes
C1 . C3 . 1.37(3) yes
C3 . C3 3_555 1.50(4) yes
C3 . H31 . 0.931 no
O1 . C2 . 1.26(3) yes
O2 . C2 . 1.23(3) yes
C2 . C5 . 1.50(3) yes
C5 . H52 . 0.960 no
C5 . H53 . 0.958 no
C5 . H51 . 0.960 no
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O1 2_565 Hg1 . C1 . 99.0(7) yes
O1 2_565 Hg1 . O1 . 77.0(6) yes
C1 . Hg1 . O1 . 173.6(8) yes
C1 3_555 S1 . C1 . 97.7(18) yes
S1 . C1 . Hg1 . 121.0(14) yes
S1 . C1 . C3 . 107.8(17) yes
Hg1 . C1 . C3 . 131.1(17) yes
C3 3_555 C3 . C1 . 113.3(12) yes
C3 3_555 C3 . H31 . 123.6 no
C1 . C3 . H31 . 123.1 no
Hg1 2_565 O1 . Hg1 . 103.0(6) yes
Hg1 2_565 O1 . C2 . 112.4(15) yes
Hg1 . O1 . C2 . 112.2(14) yes
O1 . C2 . O2 . 123(2) yes
O1 . C2 . C5 . 116(2) yes
O2 . C2 . C5 . 121(2) yes
C2 . C5 . H52 . 109.5 no
C2 . C5 . H53 . 109.4 no
H52 . C5 . H53 . 109.4 no
C2 . C5 . H51 . 109.8 no
H52 . C5 . H51 . 109.3 no
H53 . C5 . H51 . 109.4 no


_iucr_refine_instruction_details_constraints 
;
#
# Punched on 24/04/15 at 18:28:59
#
#LIST     12                                                                    
BLOCK SCALE X'S, U'S 
RIDE C   (   4,X'S) H   (  41,X'S) 
RIDE C   (   2,X'S) H   (  23,X'S) H   (  22,X'S) H   (  21,X'S) 
END                                                                             
;


_iucr_refine_instruction_details_restraints 
;
#
# Punched on 24/04/15 at 18:28:59
#
#LIST     16                                                                    
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
U(IJ)'S  0.0, 0.010000 = C(3) TO S(4) 
U(IJ)'S  0.0, 0.010000 = S(4) TO C(5) 
U(IJ)'S  0.0, 0.010000 = S(2) TO C(3) 
U(IJ)'S  0.0, 0.010000 = S(2) TO C(4) 
U(IJ)'S  0.0, 0.010000 = S(1) TO C(1) 
U(IJ)'S  0.0, 0.010000 = S(1) TO C(2) 
END                                                                             
;
_chemical_properties_physical    'highly Toxic'
####################################################################### 
# 
# 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 1438076'
_audit_update_record             
;
2016-04-04 deposited with the CCDC.
2016-08-11 downloaded from the CCDC.
;

_exptl_special_details           
; 
 The crystal was 
placed in the cold stream of an Oxford 
Cryosystems open-flow nitrogen cryostat (Cosier & 
Glazer, 1986) with a nominal stability of 0.1K. 
 
Cosier, J. & Glazer, A.M., 1986. J. Appl. Cryst. 105-107. 
;
_refine_special_details          
; 
? 
;
#--------------------------------------------------------------- 
# _oxford_ data items, April 2010: 
# There is some uncertainty about the correct way of forming local data 
# names, e.g. 

# _atom_site_special_shape_oxford 
# or 
# _oxford_atom_site_special_shape 

# see: 
# http://www.iucr.org/resources/cif/spec/version1.1/semantics#namespace 

# A reserved prefix, e.g. foo, must be used in the following way 
# " If the data file contains items defined in a DDL1 dictionary, the 
# local data names assigned under the reserved prefix must contain it as 
# their first component, e.g. _foo_atom_site_my_item. " 

# However, this seems to say the opposite: 
# http://www.iucr.org/__data/iucr/cif/standard/cifstd8.html 

# According to advice from the IUCr, CRYSTALS is correct 
#--------------------------------------------------------------- 
# End of 'script/refcif.dat' 
#end of refcif 
_cell_length_a                   8.1729(1)
_cell_length_b                   5.2175(1)
_cell_length_c                   17.3973(1)
_cell_angle_alpha                90
_cell_angle_beta                 99.70(3)
_cell_angle_gamma                90
_cell_volume                     731.24(2)

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21/a 1 '
_symmetry_space_group_name_Hall  '-P 2yab'
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
-x+1/2,y+1/2,-z
x+1/2,-y+1/2,z

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
Hg -0.8800 6.2990 20.6809 0.5450 19.0417 8.4484 21.6575 1.5729 5.9676 38.3246
12.6089 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
C 0.0020 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
O 0.0060 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089
0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
S 0.0830 0.0760 6.9053 1.4679 5.2034 22.2151 1.4379 0.2536 1.5863 56.1720
0.8669 'International Tables Vol C 4.2.6.8 and 6.1.1.4'


_cell_formula_units_Z            2

# Given Formula = C12 H10 Hg2 O4 S2 
# Dc =      3.10 Fooo =    612.00 Mu =    116.25 M =    683.50
# Found Formula = C12 H10 Hg2 O4 S2 
# Dc =      3.10 FOOO =    612.00 Mu =    116.25 M =    683.50

_chemical_formula_sum            'C12 H10 Hg2 O4 S2'
_chemical_formula_moiety         'C12 H10 Hg2 O4 S2'
_chemical_compound_source        ?
_chemical_formula_weight         683.50


_cell_measurement_reflns_used    9381
_cell_measurement_theta_min      2
_cell_measurement_theta_max      21
_cell_measurement_temperature    293

_exptl_crystal_description       plate
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_size_min          0.072
_exptl_crystal_size_mid          0.379
_exptl_crystal_size_max          0.388

_exptl_crystal_density_diffrn    3.104
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             612
_exptl_absorpt_coefficient_mu    11.625

# Sheldrick geometric approximatio 0.00 0.22 
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_absorpt_correction_T_min  0.10
_exptl_absorpt_correction_T_max  0.22
# For a Kappa CCD, set Tmin to 1.0 and 
# Tmax to the ratio of max:min frame scales in scale_all.log 
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_device       Area
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Ag K\a'
_diffrn_radiation_wavelength     0.56087
_diffrn_measurement_method       ω

# If a reference occurs more than once, delete the author 
# and date from subsequent references. 
_computing_data_collection       'COLLECT (Nonius, 2001).'
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'

_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_number         0
_diffrn_standards_decay_%        ?

_diffrn_ambient_temperature      293
_diffrn_reflns_number            9384
_reflns_number_total             1661
_diffrn_reflns_av_R_equivalents  0.059
# Number of reflections without Friedels Law is 0 
# Number of reflections with Friedels Law is 1661 
# Theoretical number of reflections is about 3379 


_diffrn_reflns_theta_min         2.81
_diffrn_reflns_theta_max         21.42
_diffrn_measured_fraction_theta_max 0.976

_diffrn_reflns_theta_full        21.186
_diffrn_measured_fraction_theta_full 0.990


_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       22
_reflns_limit_h_min              -10
_reflns_limit_h_max              10
_reflns_limit_k_min              0
_reflns_limit_k_max              6
_reflns_limit_l_min              0
_reflns_limit_l_max              22

_oxford_diffrn_Wilson_B_factor   3.23
_oxford_diffrn_Wilson_scale      16.75

_atom_sites_solution_primary     direct #heavy,direct,difmap,geom
# _atom_sites_solution_secondary  difmap
_atom_sites_solution_hydrogens   difmap

_refine_diff_density_min         -3.85
_refine_diff_density_max         2.96


# The current dictionary definitions do not cover the 
# situation where the reflections used for refinement were 
# selected by a user-defined sigma threshold 


# The values actually used during refinement 
_oxford_reflns_threshold_expression_ref I>0.0\s(I)
_refine_ls_number_reflns         1127
_refine_ls_number_restraints     6
_refine_ls_number_parameters     91
_oxford_refine_ls_R_factor_ref   0.0718
_refine_ls_wR_factor_ref         0.0870
_refine_ls_goodness_of_fit_ref   1.0349
_refine_ls_shift/su_max          0.0003473
_refine_ls_shift/su_mean         0.0000123


# The values computed with all filters except I/sigma 
_oxford_reflns_number_all        1660
_refine_ls_R_factor_all          0.0978
_refine_ls_wR_factor_all         0.1216

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                1249
_refine_ls_R_factor_gt           0.0796
_refine_ls_wR_factor_gt          0.0921

# choose from: rm (reference molecule of known chirality), 
# ad (anomolous dispersion - Flack), rmad (rm and ad), 
# syn (from synthesis), unk (unknown) or . (not applicable). 
_chemical_absolute_configuration .


_refine_ls_structure_factor_coef F
_refine_ls_matrix_type           full
_refine_ls_hydrogen_treatment    noref #undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A₀*T₀(x)+A₁*T₁(x) ... +Aₙ₋₁]*Tₙ₋₁(x)] 
 where Ai are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)²]² 
 Ai are: 
 1.88 1.35 1.14 
;

# Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3

# Replace last . with number of unfound hydrogen atoms attached to an atom.

# ..._refinement_flags_... 
# . no refinement constraints           S special position constraint on site
# G rigid group refinement of site      R riding atom
# D distance or angle restraint on site T thermal displacement constraints
# U Uiso or Uij restraint (rigid bond)  P partial occupancy constraint


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_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_attached_hydrogens
Hg1 Hg 0.86218(8) 0.75845(10) 0.76273(4) 0.0456 1.0000 Uani . . . . . .
C1 C 0.704(2) 0.901(3) 0.6723(9) 0.0370 1.0000 Uani . U . . . .
C3 C 0.602(2) 1.117(3) 0.6697(9) 0.0409 1.0000 Uani . U . . . .
C4 C 0.5103(18) 1.168(3) 0.5992(9) 0.0367 1.0000 Uani . . . . . .
C5 C 0.5348(16) 0.999(2) 0.5408(9) 0.0313 1.0000 Uani . . . . . .
S1 S 0.6805(5) 0.7742(6) 0.5799(3) 0.0408 1.0000 Uani . . . . . .
O1 O 1.0214(18) 0.627(2) 0.8578(8) 0.0569 1.0000 Uani . . . . . .
C2 C 1.001(2) 0.383(3) 0.8667(9) 0.0417 1.0000 Uani . . . . . .
O2 O 0.9036(19) 0.258(2) 0.8259(7) 0.0527 1.0000 Uani . . . . . .
C6 C 1.106(3) 0.269(3) 0.9340(13) 0.0634 1.0000 Uani . . . . . .
H31 H 0.5988 1.2180 0.7142 0.0500 1.0000 Uiso . . . . . .
H41 H 0.4363 1.3040 0.5918 0.0452 1.0000 Uiso . . . . . .
H63 H 1.0594 0.1109 0.9481 0.1010 1.0000 Uiso . . . . . .
H62 H 1.1162 0.3854 0.9777 0.1011 1.0000 Uiso . . . . . .
H61 H 1.2163 0.2376 0.9224 0.1010 1.0000 Uiso . . . . . .
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
Hg1 0.0504(5) 0.0307(4) 0.0502(5) 0.0072(3) -0.0075(3) -0.0006(3)
C1 0.040(7) 0.038(6) 0.027(7) 0.011(5) -0.010(6) 0.002(6)
C3 0.049(8) 0.041(6) 0.028(7) 0.000(5) -0.005(6) 0.006(6)
C4 0.033(7) 0.034(6) 0.042(9) -0.003(6) 0.002(7) 0.008(6)
C5 0.028(7) 0.017(5) 0.051(9) 0.006(5) 0.010(6) -0.003(5)
S1 0.0421(19) 0.0280(16) 0.049(2) 0.0009(14) -0.0018(17) 0.0094(15)
O1 0.068(8) 0.033(6) 0.057(8) 0.009(5) -0.025(7) -0.002(6)
C2 0.045(9) 0.049(9) 0.028(8) 0.007(6) -0.002(7) 0.001(7)
O2 0.071(9) 0.058(8) 0.022(6) 0.004(5) -0.010(6) -0.006(6)
C6 0.075(13) 0.055(11) 0.048(11) 0.015(8) -0.025(10) 0.025(9)

_refine_ls_extinction_method     None
_oxford_refine_ls_scale          0.2622(16)
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Hg1 . O2 1_565 2.826(11) yes
Hg1 . C1 . 2.002(13) yes
Hg1 . O1 . 2.043(11) yes
Hg1 . O2 . 2.832(11) yes
C1 . C3 . 1.40(2) yes
C1 . S1 . 1.718(16) yes
C3 . C4 . 1.35(2) yes
C3 . H31 . 0.940 no
C4 . C5 . 1.39(2) yes
C4 . H41 . 0.927 no
C5 . C5 2_676 1.44(3) yes
C5 . S1 . 1.729(13) yes
O1 . C2 . 1.296(19) yes
C2 . O2 . 1.17(2) yes
C2 . C6 . 1.46(2) yes
C6 . H63 . 0.960 no
C6 . H62 . 0.965 no
C6 . H61 . 0.968 no
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O2 1_565 Hg1 . C1 . 89.0(5) yes
O2 1_565 Hg1 . O1 . 88.6(4) yes
C1 . Hg1 . O1 . 177.4(5) yes
O2 1_565 Hg1 . O2 . 134.5(4) yes
C1 . Hg1 . O2 . 131.8(5) yes
O1 . Hg1 . O2 . 50.1(4) yes
Hg1 . C1 . C3 . 128.8(12) yes
Hg1 . C1 . S1 . 123.2(9) yes
C3 . C1 . S1 . 107.9(10) yes
C1 . C3 . C4 . 115.1(14) yes
C1 . C3 . H31 . 121.5 no
C4 . C3 . H31 . 123.4 no
C3 . C4 . C5 . 114.6(13) yes
C3 . C4 . H41 . 121.7 no
C5 . C4 . H41 . 123.7 no
C5 2_676 C5 . C4 . 129.8(16) yes
C5 2_676 C5 . S1 . 121.6(14) yes
C4 . C5 . S1 . 108.5(11) yes
C1 . S1 . C5 . 94.0(7) yes
Hg1 . O1 . C2 . 110.4(10) yes
O1 . C2 . O2 . 124.3(15) yes
O1 . C2 . C6 . 115.3(15) yes
O2 . C2 . C6 . 120.4(16) yes
Hg1 1_545 O2 . Hg1 . 134.5(4) yes
Hg1 1_545 O2 . C2 . 140.7(12) yes
Hg1 . O2 . C2 . 75.2(9) yes
C2 . C6 . H63 . 110.5 no
C2 . C6 . H62 . 109.6 no
H63 . C6 . H62 . 108.9 no
C2 . C6 . H61 . 110.2 no
H63 . C6 . H61 . 109.3 no
H62 . C6 . H61 . 108.2 no
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_site_symmetry_D
_geom_hbond_atom_site_label_H
_geom_hbond_site_symmetry_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_angle_DHA
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_publ_flag
C6 . H61 . O2 4_555 148.0(12) 0.968 2.456 3.32(2) yes


_iucr_refine_instruction_details_constraints 
;
#
# Punched on 21/04/15 at 12:31:58
#
#LIST     12                                                                    
BLOCK SCALE X'S, U'S 
END                                                                             
;


_iucr_refine_instruction_details_restraints 
;
#
# Punched on 21/04/15 at 12:31:58
#
#LIST     16                                                                    
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
U(IJ)'S  0.0, 0.010000 = C(2) TO C(3) 
END                                                                             
;
_chemical_properties_physical    'Highly Toxic'
