# Electronic Supplementary Material (ESI) for Journal of Materials Chemistry A.
# This journal is © The Royal Society of Chemistry 2017

####################################################################### 
# 
# 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_45K
_database_code_depnum_ccdc_archive 'CCDC 1558088'
_audit_update_record             
;
2017-06-23 deposited with the CCDC.
2017-08-04 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C24 H42 Cu4 N4 O17 S4'
_chemical_formula_weight         1041.01

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0026 0.0014 '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 0.0053 0.0029 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0095 0.0054 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3356 1.1486 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1139 0.1106 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      tetragonal
_space_group_IT_number           77
_space_group_name_H-M_alt        'P 42'
_space_group_name_Hall           'P 4c'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   13.6593(2)
_cell_length_b                   13.6593(2)
_cell_length_c                   12.0051(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2239.88(10)
_cell_formula_units_Z            2
_cell_measurement_temperature    45(2)
_cell_measurement_reflns_used    1684
_cell_measurement_theta_min      2.1100
_cell_measurement_theta_max      29.5850

_exptl_crystal_description       hexagonal
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.544
_exptl_crystal_F_000             1060
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.16
_exptl_absorpt_coefficient_mu    1.751
_exptl_absorpt_correction_T_min  0.67082
_exptl_absorpt_correction_T_max  0.67867
_exptl_absorpt_correction_type   sphere
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Spherical absorption correction
 using equivalent radius and absorption coefficient.
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_oxdiff_exptl_absorpt_empirical_full_min 0.919
_oxdiff_exptl_absorpt_empirical_full_max 1.087
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;

_diffrn_ambient_temperature      45(2)
_diffrn_source                   synchrotron
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.67165
_diffrn_radiation_monochromator  synchrotron
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Atlas'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Atlas
_diffrn_detector_area_resol_mean 10.2930
_diffrn_reflns_number            7323
_diffrn_reflns_av_unetI/netI     0.0773
_diffrn_reflns_av_R_equivalents  0.0516
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         1.4908
_diffrn_reflns_theta_max         24.6939
_diffrn_measured_fraction_theta_max 0.9484
_diffrn_reflns_theta_full        24.6602
_diffrn_measured_fraction_theta_full 0.9891
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_Laue_measured_fraction_full 0.929
_diffrn_reflns_point_group_measured_fraction_max 0.950
_diffrn_reflns_point_group_measured_fraction_full 0.892
_reflns_number_total             3630
_reflns_number_gt                2936
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.825
_reflns_Friedel_fraction_max     0.907
_reflns_Friedel_fraction_full    0.851

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'CRYSTAL MAKER'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0682P)²+3.5913P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    riding
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 1137 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.02(4)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         3630
_refine_ls_number_parameters     226
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0696
_refine_ls_R_factor_gt           0.0516
_refine_ls_wR_factor_ref         0.1329
_refine_ls_wR_factor_gt          0.1215
_refine_ls_goodness_of_fit_ref   0.957
_refine_ls_restrained_S_all      0.957
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
O5 O 0.3236(5) 0.0162(5) 0.5690(6) 0.0261(18) Uani 1 1 d . . . . .
O3 O 0.1981(5) 0.4799(5) 0.1034(6) 0.0218(17) Uani 1 1 d . . . . .
C4 C 0.2183(8) 0.5357(8) 0.1930(10) 0.020(3) Uani 1 1 d . . . . .
C6 C 0.2903(7) -0.0398(8) 0.4845(9) 0.016(2) Uani 1 1 d . . . . .
O4 O 0.2158(5) 0.6342(5) 0.1904(6) 0.0186(17) Uani 1 1 d . . . . .
O6 O 0.2846(6) -0.1349(5) 0.4890(6) 0.0226(18) Uani 1 1 d . . . . .
C8 C 0.3553(8) 0.6213(8) 0.4173(9) 0.027(2) Uani 1 1 d . . . . .
H8A H 0.3346 0.6741 0.3660 0.032 Uiso 1 1 calc R U . . .
H8B H 0.4231 0.6356 0.4414 0.032 Uiso 1 1 calc R U . . .
C7 C 0.3544(7) 0.5199(7) 0.3515(8) 0.019(2) Uani 1 1 d . . . . .
H7A H 0.3819 0.4687 0.4008 0.023 Uiso 1 1 calc R U . . .
H7B H 0.3984 0.5259 0.2863 0.023 Uiso 1 1 calc R U . . .
S1 S 0.2717(2) 0.62188(19) 0.5446(3) 0.0266(6) Uani 1 1 d . . . . .
S2 S 0.1679(2) -0.1185(2) 0.1446(3) 0.0382(7) Uani 1 1 d . . . . .
C9 C 0.3308(10) 0.5268(8) 0.6373(12) 0.044(3) Uani 1 1 d . . . . .
H9A H 0.4008 0.5413 0.6450 0.066 Uiso 1 1 calc R U . . .
H9B H 0.3226 0.4618 0.6040 0.066 Uiso 1 1 calc R U . . .
H9C H 0.2997 0.5280 0.7108 0.066 Uiso 1 1 calc R U . . .
C12 C 0.1877(14) -0.0274(12) 0.0241(15) 0.082(6) Uani 1 1 d . . . . .
H12A H 0.2040 0.0372 0.0545 0.124 Uiso 1 1 calc R U . . .
H12B H 0.1276 -0.0226 -0.0203 0.124 Uiso 1 1 calc R U . . .
H12C H 0.2415 -0.0503 -0.0232 0.124 Uiso 1 1 calc R U . . .
C10 C 0.3289(8) -0.0199(8) 0.2672(9) 0.027(2) Uani 1 1 d . . . . .
H10A H 0.3295 0.0327 0.2104 0.033 Uiso 1 1 calc R U . . .
H10B H 0.3964 -0.0270 0.2959 0.033 Uiso 1 1 calc R U . . .
C11 C 0.2974(9) -0.1205(8) 0.2083(9) 0.032(3) Uani 1 1 d . . . . .
H11A H 0.3008 -0.1738 0.2639 0.039 Uiso 1 1 calc R U . . .
H11B H 0.3451 -0.1356 0.1487 0.039 Uiso 1 1 calc R U . . .
Cu1 Cu 0.19703(8) 0.32728(8) 0.13720(8) 0.0179(3) Uani 1 1 d . . . . .
Cu2 Cu 0.30524(8) 0.16932(8) 0.54419(8) 0.0169(3) Uani 1 1 d . . . . .
O1 O 0.1984(5) 0.1864(5) 0.2141(6) 0.0207(17) Uani 1 1 d . . . . .
O2 O 0.2877(5) 0.3109(5) 0.4728(6) 0.0222(17) Uani 1 1 d . . . . .
N1 N 0.2386(6) 0.3740(6) 0.2887(7) 0.0172(19) Uani 1 1 d . . . . .
N2 N 0.2634(6) 0.1230(6) 0.3910(7) 0.018(2) Uani 1 1 d . . . . .
C2 C 0.2366(7) 0.1948(7) 0.3171(9) 0.016(2) Uani 1 1 d . . . . .
C5 C 0.2581(8) 0.0135(7) 0.3691(9) 0.019(2) Uani 1 1 d . . . . .
H5 H 0.1891 -0.0048 0.3510 0.022 Uiso 1 1 calc R U . . .
C3 C 0.2482(8) 0.4838(7) 0.3084(9) 0.019(2) Uani 1 1 d . . . . .
H3 H 0.1987 0.5030 0.3657 0.023 Uiso 1 1 calc R U . . .
C1 C 0.2555(7) 0.3021(8) 0.3672(9) 0.018(2) Uani 1 1 d . . . . .
O1W O 0.0000 0.5000 0.2478(13) 0.070(4) Uani 1 2 d S T P . .
O2W O 0.0000 0.5000 0.502(4) 0.31(3) Uiso 1 2 d S . P . .


_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
O5 C6 1.349(12) . ?
O5 Cu2 2.128(7) . ?
O3 C4 1.347(13) . ?
O3 Cu1 2.123(7) . ?
C4 O4 1.346(13) . ?
C4 C3 1.609(15) . ?
C6 O6 1.303(13) . ?
C6 C5 1.626(14) . ?
O4 Cu2 2.042(7) 4_564 ?
O6 Cu1 2.055(7) 4 ?
C8 C7 1.593(14) . ?
C8 S1 1.907(11) . ?
C7 C3 1.618(14) . ?
S1 C9 1.891(12) . ?
S2 C11 1.926(12) . ?
S2 C12 1.928(18) . ?
C10 C11 1.604(15) . ?
C10 C5 1.624(15) . ?
Cu1 N1 2.009(9) . ?
Cu1 O6 2.055(7) 3_554 ?
Cu1 O1 2.135(7) . ?
Cu2 N2 2.027(8) . ?
Cu2 O4 2.042(7) 3_655 ?
Cu2 O2 2.129(7) . ?
O1 C2 1.347(12) . ?
O2 C1 1.347(12) . ?
N1 C1 1.381(13) . ?
N1 C3 1.524(13) . ?
N2 C2 1.373(13) . ?
N2 C5 1.519(13) . ?
C2 C1 1.606(11) . ?

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
C6 O5 Cu2 114.3(6) . . ?
C4 O3 Cu1 113.9(6) . . ?
O4 C4 O3 122.9(9) . . ?
O4 C4 C3 117.8(9) . . ?
O3 C4 C3 119.3(8) . . ?
O6 C6 O5 123.7(9) . . ?
O6 C6 C5 117.8(8) . . ?
O5 C6 C5 118.6(9) . . ?
C4 O4 Cu2 115.6(6) . 4_564 ?
C6 O6 Cu1 115.5(6) . 4 ?
C7 C8 S1 113.3(7) . . ?
C8 C7 C3 115.5(8) . . ?
C9 S1 C8 102.3(6) . . ?
C11 S2 C12 100.3(6) . . ?
C11 C10 C5 114.4(8) . . ?
C10 C11 S2 114.2(8) . . ?
N1 Cu1 O6 172.0(3) . 3_554 ?
N1 Cu1 O3 81.9(3) . . ?
O6 Cu1 O3 96.7(3) 3_554 . ?
N1 Cu1 O1 83.8(3) . . ?
O6 Cu1 O1 97.0(3) 3_554 . ?
O3 Cu1 O1 165.4(3) . . ?
N2 Cu2 O4 172.4(3) . 3_655 ?
N2 Cu2 O5 81.6(3) . . ?
O4 Cu2 O5 97.9(3) 3_655 . ?
N2 Cu2 O2 83.5(3) . . ?
O4 Cu2 O2 96.3(3) 3_655 . ?
O5 Cu2 O2 164.3(3) . . ?
C2 O1 Cu1 108.9(6) . . ?
C1 O2 Cu2 109.6(6) . . ?
C1 N1 C3 125.4(8) . . ?
C1 N1 Cu1 116.0(7) . . ?
C3 N1 Cu1 118.5(6) . . ?
C2 N2 C5 125.3(8) . . ?
C2 N2 Cu2 116.0(7) . . ?
C5 N2 Cu2 118.5(6) . . ?
O1 C2 N2 129.5(9) . . ?
O1 C2 C1 119.0(7) . . ?
N2 C2 C1 111.6(7) . . ?
N2 C5 C10 112.3(8) . . ?
N2 C5 C6 106.3(8) . . ?
C10 C5 C6 110.8(8) . . ?
N1 C3 C4 106.2(8) . . ?
N1 C3 C7 115.2(8) . . ?
C4 C3 C7 111.7(8) . . ?
O2 C1 N1 129.3(9) . . ?
O2 C1 C2 119.1(8) . . ?
N1 C1 C2 111.5(7) . . ?

_refine_diff_density_max         0.396
_refine_diff_density_min         -0.483
_refine_diff_density_rms         0.094

_shelxl_version_number           2013-4


_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: water'
####################################################################### 
# 
# 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_MARMON87_SQ
_database_code_depnum_ccdc_archive 'CCDC 1558089'
_audit_update_record             
;
2017-08-02 deposited with the CCDC.
2017-08-04 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C24 H38 Cl Cu4 Hg0.50 N4 O15 S4'
_chemical_formula_weight         1140.73

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'
Cu Cu 0.3201 1.2651 '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'
Hg Hg -2.3894 9.2266 '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'

_space_group_crystal_system      tetragonal
_space_group_IT_number           77
_space_group_name_H-M_alt        'P 42'
_space_group_name_Hall           'P 4c'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   13.0954(15)
_cell_length_b                   13.0954(15)
_cell_length_c                   11.5653(13)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1983.3(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    90(2)
_cell_measurement_reflns_used    5341
_cell_measurement_theta_min      2.35
_cell_measurement_theta_max      25.7

_exptl_crystal_description       hexagonal
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.910
_exptl_crystal_F_000             1134
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.20
_exptl_absorpt_coefficient_mu    4.386
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.267
_exptl_absorpt_correction_T_max  0.290
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      90(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            25429
_diffrn_reflns_av_unetI/netI     0.0696
_diffrn_reflns_av_R_equivalents  0.1064
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         1.555
_diffrn_reflns_theta_max         24.986
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.972
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.972
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.972
_reflns_number_total             3494
_reflns_number_gt                2914
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.897
_reflns_Friedel_fraction_max     0.999
_reflns_Friedel_fraction_full    0.971

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker APEX'
_computing_cell_refinement       'Bruker APEX'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
'Refined as a 2-component inversion twin.,SQUEEZE'
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0975P)²+72.4588P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    riding
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.18(7)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         3494
_refine_ls_number_parameters     220
_refine_ls_number_restraints     7
_refine_ls_R_factor_all          0.1177
_refine_ls_R_factor_gt           0.1045
_refine_ls_wR_factor_ref         0.2708
_refine_ls_wR_factor_gt          0.2617
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_restrained_S_all      1.043
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.001

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
Cu1 Cu 1.19999(16) 0.32495(17) 0.13741(16) 0.0243(6) Uani 1 1 d . . .
Cu2 Cu 1.30967(16) 0.17215(14) 0.54175(17) 0.0212(5) Uani 1 1 d . . .
N1 N 1.2457(14) 0.3752(13) 0.2891(12) 0.034(3) Uani 1 1 d . . .
N2 N 1.2663(10) 0.1270(10) 0.3951(12) 0.017(3) Uani 1 1 d . . .
O1 O 1.2096(11) 0.1837(9) 0.2167(14) 0.032(3) Uani 1 1 d . . .
O2 O 1.2984(10) 0.3102(9) 0.4706(8) 0.021(2) Uani 1 1 d . . .
O3 O 1.2030(10) 0.4736(10) 0.1025(12) 0.030(3) Uani 1 1 d . . .
O4 O 1.2187(9) 0.6309(8) 0.1806(8) 0.015(2) Uani 1 1 d . . .
O5 O 1.3232(9) 0.0174(8) 0.5714(8) 0.017(2) Uani 1 1 d . . .
O6 O 1.2804(11) -0.1331(11) 0.4861(12) 0.036(3) Uani 1 1 d . . .
C1 C 1.2645(16) 0.3061(16) 0.3594(18) 0.031(5) Uani 1 1 d . . .
C2 C 1.2431(15) 0.1998(12) 0.3147(13) 0.018(3) Uani 1 1 d . . .
C3 C 1.2491(18) 0.4842(12) 0.3022(13) 0.031(3) Uani 1 1 d . . .
H3 H 1.1958 0.5052 0.3594 0.037 Uiso 1 1 calc R . .
C4 C 1.2217(15) 0.5350(15) 0.1768(16) 0.027(4) Uani 1 1 d . . .
C5 C 1.2573(12) 0.0150(13) 0.3685(14) 0.016(3) Uani 1 1 d . . .
H5 H 1.1849 -0.0015 0.3485 0.019 Uiso 1 1 calc R . .
C6 C 1.2857(12) -0.0376(11) 0.4790(12) 0.011(3) Uani 1 1 d . . .
C7 C 1.3600(12) 0.5189(12) 0.3503(15) 0.021(4) Uani 1 1 d . . .
H7A H 1.3862 0.4655 0.4031 0.026 Uiso 1 1 calc R . .
H7B H 1.4080 0.5242 0.2844 0.026 Uiso 1 1 calc R . .
C8 C 1.3576(11) 0.6192(13) 0.4132(10) 0.022(3) Uani 1 1 d D . .
H8A H 1.3356 0.6730 0.3586 0.026 Uiso 1 1 calc R . .
H8B H 1.4278 0.6360 0.4387 0.026 Uiso 1 1 calc R . .
C9 C 1.3412(16) 0.5270(14) 0.6293(18) 0.047(5) Uani 1 1 d D . .
H9A H 1.3279 0.4583 0.5992 0.070 Uiso 1 1 calc R . .
H9B H 1.3177 0.5313 0.7096 0.070 Uiso 1 1 calc R . .
H9C H 1.4147 0.5411 0.6260 0.070 Uiso 1 1 calc R . .
C10 C 1.3305(19) -0.0230(18) 0.2673(16) 0.049(5) Uani 1 1 d . . .
H10A H 1.3292 0.0275 0.2036 0.058 Uiso 1 1 calc R . .
H10B H 1.4014 -0.0269 0.2967 0.058 Uiso 1 1 calc R . .
C11 C 1.2998(10) -0.1263(13) 0.2205(14) 0.031(4) Uani 1 1 d D . .
H11A H 1.2961 -0.1757 0.2852 0.037 Uiso 1 1 calc R . .
H11B H 1.3529 -0.1505 0.1660 0.037 Uiso 1 1 calc R . .
C12 C 1.215(3) -0.043(8) 0.020(6) 0.450 Uiso 1 1 d D . .
H12A H 1.2777 -0.0711 -0.0133 0.675 Uiso 1 1 calc R . .
H12B H 1.2268 0.0268 0.0460 0.675 Uiso 1 1 calc R . .
H12C H 1.1607 -0.0439 -0.0384 0.675 Uiso 1 1 calc R . .
S1 S 1.2722(3) 0.6216(4) 0.5408(4) 0.0314(10) Uani 1 1 d D . .
S2 S 1.1753(7) -0.1231(5) 0.1454(8) 0.081(3) Uani 1 1 d D . .
Hg1 Hg 1.0000 0.0000 0.1906(5) 0.272(7) Uani 0.50 2 d SPD . .
O1W O 1.0000 0.5000 0.237(3) 0.121(15) Uani 1 2 d S . .
O2W O 1.342(2) 0.019(2) -0.058(3) 0.045(7) Uiso 0.50 1 d P . .
Cl1 Cl 0.973(7) 0.1310(14) 0.3198(15) 0.409 Uiso 0.50 1 d PD . .
O3W O 1.0000 0.0000 -0.008(3) 0.109(11) Uiso 1 2 d S . .


_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
Cu1 N1 1.967(15) . ?
Cu1 O3 1.988(13) . ?
Cu1 O6 2.042(14) 3_644 ?
Cu1 O1 2.069(12) . ?
Cu1 S1 2.680(5) 3_744 ?
Cu2 O4 1.885(10) 3_745 ?
Cu2 N2 1.884(14) . ?
Cu2 O2 1.991(12) . ?
Cu2 O5 2.063(11) . ?
Cu2 S2 2.722(6) 3_645 ?
N1 C1 1.24(3) . ?
N1 C3 1.44(2) . ?
N2 C2 1.37(2) . ?
N2 C5 1.50(2) . ?
O1 C2 1.23(2) . ?
O2 C1 1.36(2) . ?
O3 C4 1.20(2) . ?
O4 C4 1.26(2) . ?
O4 Cu2 1.885(10) 4_674 ?
O5 C6 1.379(17) . ?
O6 C6 1.25(2) . ?
O6 Cu1 2.042(14) 4_665 ?
C1 C2 1.51(2) . ?
C3 C4 1.64(2) . ?
C3 C7 1.62(3) . ?
C5 C6 1.50(2) . ?
C5 C10 1.59(2) . ?
C7 C8 1.50(2) . ?
C8 S1 1.852(9) . ?
C9 S1 1.843(9) . ?
C10 C11 1.51(3) . ?
C11 S2 1.848(9) . ?
C12 S2 1.859(10) . ?
S1 Cu1 2.680(5) 4_675 ?
S2 Cl1 2.81(6) 2_755 ?
S2 Cu2 2.722(6) 4_664 ?
S2 Hg1 2.853(8) . ?
Hg1 O3W 2.30(4) . ?
Hg1 Cl1 2.301(10) . ?
Hg1 Cl1 2.301(10) 2_755 ?
Hg1 S2 2.853(8) 2_755 ?
Cl1 S2 2.81(6) 2_755 ?

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
N1 Cu1 O3 81.2(6) . . ?
N1 Cu1 O6 172.1(7) . 3_644 ?
O3 Cu1 O6 96.5(6) . 3_644 ?
N1 Cu1 O1 83.4(6) . . ?
O3 Cu1 O1 164.6(6) . . ?
O6 Cu1 O1 98.7(6) 3_644 . ?
N1 Cu1 S1 101.1(6) . 3_744 ?
O3 Cu1 S1 98.6(4) . 3_744 ?
O6 Cu1 S1 86.8(5) 3_644 3_744 ?
O1 Cu1 S1 84.3(5) . 3_744 ?
O4 Cu2 N2 173.0(6) 3_745 . ?
O4 Cu2 O2 95.1(4) 3_745 . ?
N2 Cu2 O2 83.7(5) . . ?
O4 Cu2 O5 98.1(4) 3_745 . ?
N2 Cu2 O5 82.4(5) . . ?
O2 Cu2 O5 165.2(4) . . ?
O4 Cu2 S2 89.5(4) 3_745 3_645 ?
N2 Cu2 S2 97.5(5) . 3_645 ?
O2 Cu2 S2 95.8(4) . 3_645 ?
O5 Cu2 S2 91.1(4) . 3_645 ?
C1 N1 C3 130.5(17) . . ?
C1 N1 Cu1 113.6(15) . . ?
C3 N1 Cu1 115.8(11) . . ?
C2 N2 C5 121.7(13) . . ?
C2 N2 Cu2 117.4(11) . . ?
C5 N2 Cu2 120.9(9) . . ?
C2 O1 Cu1 106.0(11) . . ?
C1 O2 Cu2 112.3(11) . . ?
C4 O3 Cu1 120.9(12) . . ?
C4 O4 Cu2 113.1(10) . 4_674 ?
C6 O5 Cu2 110.7(9) . . ?
C6 O6 Cu1 117.9(12) . 4_665 ?
N1 C1 O2 131(2) . . ?
N1 C1 C2 114.2(17) . . ?
O2 C1 C2 114.8(14) . . ?
O1 C2 N2 125.8(15) . . ?
O1 C2 C1 122.6(13) . . ?
N2 C2 C1 111.7(12) . . ?
N1 C3 C4 107.7(14) . . ?
N1 C3 C7 110.0(15) . . ?
C4 C3 C7 112.7(15) . . ?
O3 C4 O4 133.4(17) . . ?
O3 C4 C3 114.0(16) . . ?
O4 C4 C3 112.5(14) . . ?
N2 C5 C6 104.8(12) . . ?
N2 C5 C10 114.1(14) . . ?
C6 C5 C10 109.5(15) . . ?
O6 C6 O5 119.3(15) . . ?
O6 C6 C5 120.0(14) . . ?
O5 C6 C5 120.6(13) . . ?
C8 C7 C3 113.1(13) . . ?
C7 C8 S1 114.4(10) . . ?
C11 C10 C5 112.5(16) . . ?
C10 C11 S2 112.5(14) . . ?
C9 S1 C8 97.8(9) . . ?
C9 S1 Cu1 103.2(7) . 4_675 ?
C8 S1 Cu1 101.0(5) . 4_675 ?
C11 S2 C12 97.7(7) . . ?
C11 S2 Cl1 105.9(15) . 2_755 ?
C12 S2 Cl1 141(3) . 2_755 ?
C11 S2 Cu2 101.5(6) . 4_664 ?
C12 S2 Cu2 99(4) . 4_664 ?
Cl1 S2 Cu2 105.8(8) 2_755 4_664 ?
C11 S2 Hg1 129.5(6) . . ?
C12 S2 Hg1 93(3) . . ?
Cl1 S2 Hg1 48.0(6) 2_755 . ?
Cu2 S2 Hg1 125.1(3) 4_664 . ?
O3W Hg1 Cl1 130.5(4) . . ?
O3W Hg1 Cl1 130.5(4) . 2_755 ?
Cl1 Hg1 Cl1 99.1(7) . 2_755 ?
O3W Hg1 S2 79.4(2) . 2_755 ?
Cl1 Hg1 S2 64.9(17) . 2_755 ?
Cl1 Hg1 S2 131(2) 2_755 2_755 ?
O3W Hg1 S2 79.4(2) . . ?
Cl1 Hg1 S2 131(2) . . ?
Cl1 Hg1 S2 64.9(17) 2_755 . ?
S2 Hg1 S2 158.9(4) 2_755 . ?
Hg1 Cl1 S2 67.1(12) . 2_755 ?


_refine_diff_density_max         1.095
_refine_diff_density_min         -3.322
_refine_diff_density_rms         0.268


loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.500 0.000 0.083 19 5 ' '
2 0.488 0.184 0.356 13 2 ' '
3 0.512 0.816 0.356 13 2 ' '
4 0.000 0.500 0.583 19 5 ' '
5 0.184 0.512 0.856 13 2 ' '
6 0.816 0.488 0.856 13 2 ' '
_platon_squeeze_details          
; 
;

_shelxl_version_number           2013-4

####################################################################### 
# 
# 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_MARMON87_45K
_database_code_depnum_ccdc_archive 'CCDC 1558090'
_audit_update_record             
;
2017-06-23 deposited with the CCDC.
2017-08-04 downloaded from the CCDC.
;

_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C24 H34 Cl2 Cu4 Hg N4 O14 S4'
_chemical_formula_weight         1256.44

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0029 0.0015 '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 0.0057 0.0031 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0101 0.0057 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3319 1.2017 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1188 0.1164 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1424 0.1495 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Hg Hg -1.9504 8.8008 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      tetragonal
_space_group_IT_number           77
_space_group_name_H-M_alt        'P 42'
_space_group_name_Hall           'P 4c'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   12.9735(2)
_cell_length_b                   12.9735(2)
_cell_length_c                   11.5283(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1940.35(8)
_cell_formula_units_Z            2
_cell_measurement_temperature    45(2)
_cell_measurement_reflns_used    12343
_cell_measurement_theta_max      33.0684776087
_cell_measurement_theta_min      1.51201120452

_exptl_crystal_description       hexagonal
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.151
_exptl_crystal_F_000             1224
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_exptl_absorpt_coefficient_mu    5.805
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_T_min  0.988145696935
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   
;
CCP4 7.0.035: AIMLESS, version 0.5.31 : 12/12/16
Scaling & analysis of unmerged intensities, absorption correction using spherical harmonics
;

_diffrn_ambient_temperature      45(2)
_diffrn_radiation_wavelength     0.6889
_diffrn_detector                 'Photon counting pixel array'
_diffrn_radiation_type           Synchrotron
_diffrn_measurement_device       'Fixed χ 3-circle diffractometer'
_diffrn_measurement_device_type  'Fluid Film Devices'
_diffrn_measurement_method       'shutterless scans'
_diffrn_measurement_specimen_support 'MiTeGen MicroMount'
_diffrn_radiation_source         'Diamond Light Source Beamline I19-1'
_diffrn_radiation_monochromator  'Silicon 111'
_diffrn_reflns_number            29039
_diffrn_reflns_av_unetI/netI     0.0624
_diffrn_reflns_av_R_equivalents  0.0940
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         1.521
_diffrn_reflns_theta_max         28.000
_diffrn_reflns_theta_full        24.415
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             5164
_reflns_number_gt                4754
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.909
_reflns_Friedel_fraction_max     0.999
_reflns_Friedel_fraction_full    1.000

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_audit_creation_method           'XIA2 0.5.277-gc78b72c6-dials-1.5'
_audit_creation_date             2017-05-11
_computing_data_reduction        
;
aimless (Evans, P. R. and Murshudov, G. N., 2013)
ccp4 (Winn, M. D. et al., 2011)
DIALS 1.5.1-gf72becc3-release
pointless (Evans, P., 2006)
XIA2 0.5.277-gc78b72c6-dials-1.5 (Winter, G., 2010)
;

_computing_cell_refinement       
'DIALS 2theta refinement, DIALS 1.5.1-gf72becc3-release'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'CRYSTAL MAKER'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1798P)²+5.7459P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    riding
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 2097 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.030(7)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         5164
_refine_ls_number_parameters     263
_refine_ls_number_restraints     5
_refine_ls_R_factor_all          0.0831
_refine_ls_R_factor_gt           0.0799
_refine_ls_wR_factor_ref         0.2370
_refine_ls_wR_factor_gt          0.2319
_refine_ls_goodness_of_fit_ref   0.996
_refine_ls_restrained_S_all      0.999
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
O5 O 0.9767(6) 0.3028(7) -0.0755(7) 0.0330(15) Uani 1 1 d . . . . .
O3 O 0.5211(6) 0.1804(7) 0.3903(7) 0.0343(16) Uani 1 1 d . . . . .
C4 C 0.4636(7) 0.2104(7) 0.3082(9) 0.0264(17) Uani 1 1 d . . . . .
C8 C 1.0323(8) 0.2795(7) 0.0080(9) 0.0294(18) Uani 1 1 d . . . . .
O4 O 0.3674(6) 0.2177(6) 0.3133(7) 0.0318(15) Uani 1 1 d . . . . .
O6 O 1.1301(5) 0.2795(6) 0.0042(7) 0.0289(13) Uani 1 1 d . . . . .
S1 S 0.3823(4) 0.3071(6) -0.0493(6) 0.097(2) Uani 1 1 d D . . . .
S2 S 1.1235(2) 0.2268(2) 0.3562(3) 0.0361(6) Uani 1 1 d D . . . .
C10 C 1.0203(8) 0.1426(7) 0.1645(9) 0.0287(17) Uani 1 1 d . . . . .
H10A H 0.9665 0.1122 0.2149 0.034 Uiso 1 1 calc R U . . .
H10B H 1.0275 0.0974 0.0958 0.034 Uiso 1 1 calc R U . . .
Cu1 Cu 0.67258(8) 0.18999(9) 0.36010(10) 0.0257(3) Uani 1 1 d . . . . .
Cu2 Cu 0.82491(9) 0.30170(9) -0.04256(10) 0.0258(3) Uani 1 1 d . . . . .
O1 O 0.8134(5) 0.2041(6) 0.2888(6) 0.0281(14) Uani 1 1 d . . . . .
O2 O 0.6847(5) 0.2953(6) 0.0348(7) 0.0314(15) Uani 1 1 d . . . . .
N1 N 0.6239(6) 0.2288(6) 0.2102(7) 0.0268(16) Uani 1 1 d . . . . .
N2 N 0.8724(6) 0.2555(6) 0.1045(7) 0.0259(15) Uani 1 1 d . . . . .
C2 C 0.8021(7) 0.2376(7) 0.1829(8) 0.0245(17) Uani 1 1 d . . . . .
C9 C 0.9834(7) 0.2490(7) 0.1238(8) 0.0242(17) Uani 1 1 d . . . . .
H9A H 1.0031 0.3013 0.1835 0.029 Uiso 1 1 calc R U . . .
C3 C 0.5148(7) 0.2380(8) 0.1918(9) 0.0289(19) Uani 1 1 d . . . . .
H3A H 0.4978 0.3109 0.1712 0.035 Uiso 1 1 calc R U . . .
C1 C 0.6943(7) 0.2570(7) 0.1357(8) 0.0256(17) Uani 1 1 d . . . . .
C11 C 1.1227(8) 0.1421(7) 0.2310(8) 0.0315(19) Uani 1 1 d D . . . .
H11A H 1.1786 0.1632 0.1776 0.038 Uiso 1 1 calc R U . . .
H11B H 1.1375 0.0709 0.2570 0.038 Uiso 1 1 calc R U . . .
C5 C 0.4755(8) 0.1649(11) 0.0939(11) 0.042(3) Uani 1 1 d . . . . .
H5A H 0.5274 0.1638 0.0310 0.050 Uiso 1 1 calc R U . . .
H5B H 0.4708 0.0942 0.1257 0.050 Uiso 1 1 calc R U . . .
C12 C 1.0282(9) 0.1652(16) 0.4488(13) 0.068(5) Uani 1 1 d D . . . .
H12A H 1.0210 0.2047 0.5209 0.102 Uiso 1 1 calc R U . . .
H12B H 1.0505 0.0949 0.4670 0.102 Uiso 1 1 calc R U . . .
H12C H 0.9617 0.1630 0.4085 0.102 Uiso 1 1 calc R U . . .
C6 C 0.3728(9) 0.1928(10) 0.0421(11) 0.052(3) Uani 1 1 d D . . . .
H6A H 0.3227 0.2058 0.1051 0.062 Uiso 1 1 calc R U . . .
H6B H 0.3471 0.1343 -0.0048 0.062 Uiso 1 1 calc R U . . .
Hg1 Hg 0.4616(2) 0.52041(19) 0.0032(2) 0.0577(6) Uani 0.25 1 d . . P . .
Cl2 Cl 0.5000 0.5000 -0.1923(13) 0.080(4) Uani 0.5 2 d S T P . .
Cl1 Cl 0.4244(14) 0.5053(10) 0.1933(12) 0.055(3) Uani 0.25 1 d . . P . .
Hg2 Hg 0.1589(2) 0.4796(2) 0.2630(3) 0.0669(7) Uani 0.25 1 d . . P . .
O1W O 1.0000 0.5000 0.076(3) 0.164(19) Uani 1 2 d S T P . .
Cl4 Cl 0.2798(16) 0.4507(12) 0.1312(18) 0.076(6) Uani 0.25 1 d . . P . .
Cl3 Cl 0.0000 0.5000 0.3663(15) 0.112(7) Uani 0.5 2 d S T P . .
C7 C 0.459(2) 0.236(2) -0.162(2) 0.110(9) Uiso 1 1 d D . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O5 C8 1.241(13) . ?
O5 Cu2 2.005(8) . ?
O3 C4 1.266(13) . ?
O3 Cu1 1.999(8) . ?
C4 O4 1.253(12) . ?
C4 C3 1.541(13) . ?
C8 O6 1.271(12) . ?
C8 C9 1.530(13) . ?
O4 Cu2 1.948(8) 4_565 ?
O6 Cu1 1.936(7) 4_664 ?
S1 C6 1.823(11) . ?
S1 C7 1.874(14) . ?
S1 Cu1 2.717(4) 4_564 ?
S1 Hg1 3.014(7) . ?
S2 C11 1.814(9) . ?
S2 C12 1.818(11) . ?
S2 Cu2 2.674(3) 4_665 ?
C10 C11 1.533(14) . ?
C10 C9 1.535(13) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
Cu1 N1 1.908(8) . ?
Cu1 O6 1.936(7) 3_645 ?
Cu1 O1 2.012(7) . ?
Cu1 S1 2.717(4) 3_655 ?
Cu2 N2 1.901(8) . ?
Cu2 O4 1.948(8) 3_654 ?
Cu2 O2 2.028(7) . ?
Cu2 S2 2.674(3) 3_644 ?
O1 C2 1.304(11) . ?
O2 C1 1.271(12) . ?
N1 C1 1.305(12) . ?
N1 C3 1.436(12) . ?
N2 C2 1.305(12) . ?
N2 C9 1.459(12) . ?
C2 C1 1.522(12) . ?
C9 H9A 1.0000 . ?
C3 C5 1.560(16) . ?
C3 H3A 1.0000 . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C5 C6 1.504(15) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
Hg1 Hg1 1.128(5) 2_665 ?
Hg1 Cl1 2.253(14) . ?
Hg1 Cl2 2.323(15) . ?
Hg1 Cl1 2.665(15) 2_665 ?
Hg1 Cl4 2.925(15) . ?
Cl2 Cl1 1.65(2) 3_654 ?
Cl2 Cl1 1.65(2) 4_564 ?
Cl2 Hg1 2.323(15) 2_665 ?
Cl1 Cl2 1.65(2) 3_655 ?
Cl1 Cl1 1.97(4) 2_665 ?
Cl1 Cl4 2.13(3) . ?
Cl1 Hg1 2.665(15) 2_665 ?
Hg2 C7 1.548(17) 4_565 ?
Hg2 Cl4 2.217(14) . ?
Hg2 Cl3 2.395(9) . ?
Cl3 Hg2 2.395(9) 2_565 ?
C7 Hg2 1.548(17) 3_654 ?

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
C8 O5 Cu2 114.9(7) . . ?
C4 O3 Cu1 115.5(6) . . ?
O4 C4 O3 125.2(9) . . ?
O4 C4 C3 116.9(9) . . ?
O3 C4 C3 117.9(8) . . ?
O5 C8 O6 123.6(9) . . ?
O5 C8 C9 119.9(9) . . ?
O6 C8 C9 116.4(9) . . ?
C4 O4 Cu2 117.0(7) . 4_565 ?
C8 O6 Cu1 115.5(7) . 4_664 ?
C6 S1 C7 92.2(12) . . ?
C6 S1 Cu1 103.8(4) . 4_564 ?
C7 S1 Cu1 105.4(11) . 4_564 ?
C6 S1 Hg1 130.8(5) . . ?
C7 S1 Hg1 114.2(10) . . ?
Cu1 S1 Hg1 107.5(2) 4_564 . ?
C11 S2 C12 101.4(7) . . ?
C11 S2 Cu2 101.6(3) . 4_665 ?
C12 S2 Cu2 102.8(5) . 4_665 ?
C11 C10 C9 115.3(8) . . ?
C11 C10 H10A 108.5 . . ?
C9 C10 H10A 108.5 . . ?
C11 C10 H10B 108.5 . . ?
C9 C10 H10B 108.5 . . ?
H10A C10 H10B 107.5 . . ?
N1 Cu1 O6 171.7(3) . 3_645 ?
N1 Cu1 O3 81.3(3) . . ?
O6 Cu1 O3 98.1(3) 3_645 . ?
N1 Cu1 O1 84.6(3) . . ?
O6 Cu1 O1 95.5(3) 3_645 . ?
O3 Cu1 O1 165.8(3) . . ?
N1 Cu1 S1 97.9(3) . 3_655 ?
O6 Cu1 S1 90.4(2) 3_645 3_655 ?
O3 Cu1 S1 94.9(3) . 3_655 ?
O1 Cu1 S1 89.2(3) . 3_655 ?
N2 Cu2 O4 172.3(3) . 3_654 ?
N2 Cu2 O5 81.6(3) . . ?
O4 Cu2 O5 96.5(3) 3_654 . ?
N2 Cu2 O2 83.4(3) . . ?
O4 Cu2 O2 98.0(3) 3_654 . ?
O5 Cu2 O2 164.7(3) . . ?
N2 Cu2 S2 101.4(3) . 3_644 ?
O4 Cu2 S2 86.3(2) 3_654 3_644 ?
O5 Cu2 S2 99.8(3) . 3_644 ?
O2 Cu2 S2 86.1(2) . 3_644 ?
C2 O1 Cu1 108.1(6) . . ?
C1 O2 Cu2 109.3(6) . . ?
C1 N1 C3 124.6(8) . . ?
C1 N1 Cu1 116.0(7) . . ?
C3 N1 Cu1 118.8(6) . . ?
C2 N2 C9 125.0(8) . . ?
C2 N2 Cu2 116.6(7) . . ?
C9 N2 Cu2 118.3(6) . . ?
O1 C2 N2 129.0(9) . . ?
O1 C2 C1 119.6(8) . . ?
N2 C2 C1 111.4(7) . . ?
N2 C9 C8 105.2(7) . . ?
N2 C9 C10 114.0(7) . . ?
C8 C9 C10 111.7(8) . . ?
N2 C9 H9A 108.6 . . ?
C8 C9 H9A 108.6 . . ?
C10 C9 H9A 108.6 . . ?
N1 C3 C4 106.1(8) . . ?
N1 C3 C5 112.3(8) . . ?
C4 C3 C5 110.4(9) . . ?
N1 C3 H3A 109.3 . . ?
C4 C3 H3A 109.3 . . ?
C5 C3 H3A 109.3 . . ?
O2 C1 N1 130.0(9) . . ?
O2 C1 C2 118.8(8) . . ?
N1 C1 C2 111.1(8) . . ?
C10 C11 S2 113.6(7) . . ?
C10 C11 H11A 108.8 . . ?
S2 C11 H11A 108.8 . . ?
C10 C11 H11B 108.8 . . ?
S2 C11 H11B 108.8 . . ?
H11A C11 H11B 107.7 . . ?
C6 C5 C3 115.5(11) . . ?
C6 C5 H5A 108.4 . . ?
C3 C5 H5A 108.4 . . ?
C6 C5 H5B 108.4 . . ?
C3 C5 H5B 108.4 . . ?
H5A C5 H5B 107.5 . . ?
S2 C12 H12A 109.5 . . ?
S2 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
S2 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C5 C6 S1 111.5(9) . . ?
C5 C6 H6A 109.3 . . ?
S1 C6 H6A 109.3 . . ?
C5 C6 H6B 109.3 . . ?
S1 C6 H6B 109.3 . . ?
H6A C6 H6B 108.0 . . ?
Hg1 Hg1 Cl1 98.5(4) 2_665 . ?
Hg1 Hg1 Cl2 75.94(12) 2_665 . ?
Cl1 Hg1 Cl2 168.5(4) . . ?
Hg1 Hg1 Cl1 56.7(4) 2_665 2_665 ?
Cl1 Hg1 Cl1 46.2(8) . 2_665 ?
Cl2 Hg1 Cl1 131.6(4) . 2_665 ?
Hg1 Hg1 Cl4 124.5(5) 2_665 . ?
Cl1 Hg1 Cl4 46.3(7) . . ?
Cl2 Hg1 Cl4 128.8(4) . . ?
Cl1 Hg1 Cl4 89.6(6) 2_665 . ?
Hg1 Hg1 S1 82.5(3) 2_665 . ?
Cl1 Hg1 S1 92.4(4) . . ?
Cl2 Hg1 S1 76.92(14) . . ?
Cl1 Hg1 S1 103.9(3) 2_665 . ?
Cl4 Hg1 S1 62.8(3) . . ?
Cl1 Cl2 Cl1 73.4(13) 3_654 4_564 ?
Cl1 Cl2 Hg1 135.9(6) 3_654 2_665 ?
Cl1 Cl2 Hg1 146.8(6) 4_564 2_665 ?
Cl1 Cl2 Hg1 146.8(6) 3_654 . ?
Cl1 Cl2 Hg1 135.9(6) 4_564 . ?
Hg1 Cl2 Hg1 28.1(2) 2_665 . ?
Cl2 Cl1 Cl1 53.3(6) 3_655 2_665 ?
Cl2 Cl1 Cl4 141.4(10) 3_655 . ?
Cl1 Cl1 Cl4 148.8(9) 2_665 . ?
Cl2 Cl1 Hg1 131.0(10) 3_655 . ?
Cl1 Cl1 Hg1 78.0(5) 2_665 . ?
Cl4 Cl1 Hg1 83.7(7) . . ?
Cl2 Cl1 Hg1 108.9(9) 3_655 2_665 ?
Cl1 Cl1 Hg1 55.8(4) 2_665 2_665 ?
Cl4 Cl1 Hg1 99.8(7) . 2_665 ?
Hg1 Cl1 Hg1 24.7(2) . 2_665 ?
C7 Hg2 Cl4 90.6(13) 4_565 . ?
C7 Hg2 Cl3 102.9(12) 4_565 . ?
Cl4 Hg2 Cl3 165.7(8) . . ?
Cl1 Cl4 Hg2 109.7(9) . . ?
Cl1 Cl4 Hg1 50.0(5) . . ?
Hg2 Cl4 Hg1 149.8(7) . . ?
Hg2 Cl3 Hg2 120.4(8) . 2_565 ?
Hg2 C7 S1 168(2) 3_654 . ?

_refine_diff_density_max         2.994
_refine_diff_density_min         -2.431
_refine_diff_density_rms         0.242

_shelxl_version_number           2013-4


_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: water'
