# Electronic Supplementary Material (ESI) for Chemical Communications.
# 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_mo_160422a
_database_code_depnum_ccdc_archive 'CCDC 1511671'
_audit_update_record             
;
2017-01-23 deposited with the CCDC.
2017-06-09 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        '[Cu4(OH)6][O3S(CH2)4SO3]'
_chemical_name_common            TJU-1
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C2 H0 Cu2 O6 S'
_chemical_formula_weight         279.16

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'
Cu Cu 0.3201 1.2651 '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'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/m'

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

_cell_length_a                   5.6115(15)
_cell_length_b                   6.0587(12)
_cell_length_c                   10.068(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 93.612(7)
_cell_angle_gamma                90.00
_cell_volume                     341.62(13)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    8205
_cell_measurement_theta_min      3.638
_cell_measurement_theta_max      27.436

_exptl_crystal_description       plate
_exptl_crystal_colour            blue
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.714
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             268
_exptl_absorpt_coefficient_mu    6.504
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.5008
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(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            4382
_diffrn_reflns_av_R_equivalents  0.0198
_diffrn_reflns_av_sigmaI/netI    0.0161
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         3.64
_diffrn_reflns_theta_max         27.47
_reflns_number_total             842
_reflns_number_gt                798
_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)+(0.0494P)²+0.9641P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   .
_refine_ls_hydrogen_treatment    .
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         842
_refine_ls_number_parameters     68
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0317
_refine_ls_R_factor_gt           0.0303
_refine_ls_wR_factor_ref         0.0902
_refine_ls_wR_factor_gt          0.0891
_refine_ls_goodness_of_fit_ref   1.096
_refine_ls_restrained_S_all      1.121
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 1.0000 1.0000 1.0000 0.0092(2) Uani 1 2 d S . 4
Cu2 Cu 0.51007(8) 0.7500 0.99550(5) 0.0079(2) Uani 1 2 d S . 4
S1 S 0.07005(17) 0.7500 0.30429(10) 0.0156(3) Uani 1 2 d SD . 4
O2 O 0.1781(5) 0.7500 0.1747(3) 0.0163(6) Uani 1 2 d SD . 4
O3 O 0.8744(5) 0.7500 0.9008(3) 0.0086(6) Uani 1 2 d S . 4
O4 O 0.6824(4) 1.0051(3) 1.0823(2) 0.0082(4) Uani 1 1 d . . 4
C1 C 0.3028(8) 0.7500 0.4314(4) 0.0182(9) Uani 1 2 d S . 4
C2 C 0.4065(11) 0.9933(10) 0.4407(6) 0.0168(13) Uani 0.50 1 d P . 4
O1 O -0.0266(13) 0.5154(13) 0.3170(8) 0.0248(12) Uani 0.501(9) 1 d PD A 1
O1A O -0.1068(12) 0.5866(14) 0.3237(7) 0.0248(12) Uani 0.499(9) 1 d PD A 2

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
Cu1 0.0047(3) 0.0052(3) 0.0176(3) -0.00189(16) 0.0008(2) -0.00113(15)
Cu2 0.0050(3) 0.0034(3) 0.0148(3) 0.000 -0.0021(2) 0.000
S1 0.0119(5) 0.0266(6) 0.0079(4) 0.000 -0.0027(3) 0.000
O2 0.0183(14) 0.0196(16) 0.0110(14) 0.000 0.0015(11) 0.000
O3 0.0069(12) 0.0068(13) 0.0119(13) 0.000 -0.0003(10) 0.000
O4 0.0062(9) 0.0057(10) 0.0126(10) 0.0001(6) -0.0005(7) 0.0008(6)
C1 0.019(2) 0.022(2) 0.0133(19) 0.000 -0.0083(16) 0.000
C2 0.013(3) 0.022(3) 0.014(3) -0.001(2) -0.005(2) -0.007(2)
O1 0.014(3) 0.044(4) 0.0154(14) 0.003(2) 0.000(2) -0.015(2)
O1A 0.014(3) 0.044(4) 0.0154(14) 0.003(2) 0.000(2) -0.015(2)

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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 O3 1.9237(18) 3_777 ?
Cu1 O3 1.9237(18) . ?
Cu1 O4 2.012(2) . ?
Cu1 O4 2.012(2) 3_777 ?
Cu1 Cu1 3.0293(6) 2_757 ?
Cu1 Cu1 3.0293(6) 2_747 ?
Cu2 O4 1.9685(19) 2_647 ?
Cu2 O4 1.9685(19) 3_677 ?
Cu2 O4 1.9949(19) 4_575 ?
Cu2 O4 1.995(2) . ?
Cu2 O3 2.310(3) . ?
Cu2 Cu2 3.0330(6) 3_667 ?
Cu2 Cu2 3.0330(6) 3_677 ?
S1 O2 1.473(3) . ?
S1 C1 1.770(4) . ?
O3 Cu1 1.9237(18) 2_747 ?
O4 Cu2 1.9684(19) 3_677 ?
C1 C2 1.585(6) 4_575 ?
C1 C2 1.585(6) . ?
C2 C2 1.541(11) 3_676 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O3 Cu1 O3 179.999(1) 3_777 . ?
O3 Cu1 O4 94.55(10) 3_777 . ?
O3 Cu1 O4 85.45(10) . . ?
O3 Cu1 O4 85.45(10) 3_777 3_777 ?
O3 Cu1 O4 94.55(10) . 3_777 ?
O4 Cu1 O4 179.999(1) . 3_777 ?
O3 Cu1 Cu1 38.06(7) 3_777 2_757 ?
O3 Cu1 Cu1 141.94(7) . 2_757 ?
O4 Cu1 Cu1 89.13(5) . 2_757 ?
O4 Cu1 Cu1 90.87(5) 3_777 2_757 ?
O3 Cu1 Cu1 141.94(7) 3_777 2_747 ?
O3 Cu1 Cu1 38.06(7) . 2_747 ?
O4 Cu1 Cu1 90.87(5) . 2_747 ?
O4 Cu1 Cu1 89.13(5) 3_777 2_747 ?
Cu1 Cu1 Cu1 180.0 2_757 2_747 ?
O4 Cu2 O4 97.86(12) 2_647 3_677 ?
O4 Cu2 O4 80.14(9) 2_647 4_575 ?
O4 Cu2 O4 175.40(4) 3_677 4_575 ?
O4 Cu2 O4 175.40(4) 2_647 . ?
O4 Cu2 O4 80.14(9) 3_677 . ?
O4 Cu2 O4 101.55(12) 4_575 . ?
O4 Cu2 O3 108.27(8) 2_647 . ?
O4 Cu2 O3 108.27(8) 3_677 . ?
O4 Cu2 O3 76.32(8) 4_575 . ?
O4 Cu2 O3 76.32(8) . . ?
O4 Cu2 Cu2 40.39(6) 2_647 3_667 ?
O4 Cu2 Cu2 138.10(6) 3_677 3_667 ?
O4 Cu2 Cu2 39.75(6) 4_575 3_667 ?
O4 Cu2 Cu2 141.13(6) . 3_667 ?
O3 Cu2 Cu2 92.748(17) . 3_667 ?
O4 Cu2 Cu2 138.10(6) 2_647 3_677 ?
O4 Cu2 Cu2 40.39(6) 3_677 3_677 ?
O4 Cu2 Cu2 141.13(6) 4_575 3_677 ?
O4 Cu2 Cu2 39.75(6) . 3_677 ?
O3 Cu2 Cu2 92.748(17) . 3_677 ?
Cu2 Cu2 Cu2 174.36(3) 3_667 3_677 ?
O2 S1 C1 108.3(2) . . ?
Cu1 O3 Cu1 103.88(13) . 2_747 ?
Cu1 O3 Cu2 95.19(10) . . ?
Cu1 O3 Cu2 95.19(10) 2_747 . ?
Cu2 O4 Cu2 99.86(9) 3_677 . ?
Cu2 O4 Cu1 109.02(10) 3_677 . ?
Cu2 O4 Cu1 103.03(9) . . ?
C2 C1 C2 136.8(5) 4_575 . ?
C2 C1 S1 107.1(2) 4_575 . ?
C2 C1 S1 107.1(2) . . ?
C2 C2 C1 108.9(6) 3_676 . ?

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
O3 Cu1 O3 Cu1 158(7) 3_777 . . 2_747 ?
O4 Cu1 O3 Cu1 -97.27(12) . . . 2_747 ?
O4 Cu1 O3 Cu1 82.73(12) 3_777 . . 2_747 ?
Cu1 Cu1 O3 Cu1 180.0 2_757 . . 2_747 ?
O3 Cu1 O3 Cu2 -105(7) 3_777 . . . ?
O4 Cu1 O3 Cu2 -0.61(7) . . . . ?
O4 Cu1 O3 Cu2 179.39(7) 3_777 . . . ?
Cu1 Cu1 O3 Cu2 -83.34(13) 2_757 . . . ?
Cu1 Cu1 O3 Cu2 96.66(13) 2_747 . . . ?
O4 Cu2 O3 Cu1 -179.69(7) 2_647 . . . ?
O4 Cu2 O3 Cu1 75.21(12) 3_677 . . . ?
O4 Cu2 O3 Cu1 -105.11(12) 4_575 . . . ?
O4 Cu2 O3 Cu1 0.63(7) . . . . ?
Cu2 Cu2 O3 Cu1 -141.61(7) 3_667 . . . ?
Cu2 Cu2 O3 Cu1 37.13(8) 3_677 . . . ?
O4 Cu2 O3 Cu1 -75.21(12) 2_647 . . 2_747 ?
O4 Cu2 O3 Cu1 179.69(7) 3_677 . . 2_747 ?
O4 Cu2 O3 Cu1 -0.63(7) 4_575 . . 2_747 ?
O4 Cu2 O3 Cu1 105.11(12) . . . 2_747 ?
Cu2 Cu2 O3 Cu1 -37.13(8) 3_667 . . 2_747 ?
Cu2 Cu2 O3 Cu1 141.61(7) 3_677 . . 2_747 ?
O4 Cu2 O4 Cu2 -64.5(8) 2_647 . . 3_677 ?
O4 Cu2 O4 Cu2 0.0 3_677 . . 3_677 ?
O4 Cu2 O4 Cu2 -175.64(3) 4_575 . . 3_677 ?
O3 Cu2 O4 Cu2 111.70(11) . . . 3_677 ?
Cu2 Cu2 O4 Cu2 -171.20(6) 3_667 . . 3_677 ?
O4 Cu2 O4 Cu1 -176.8(7) 2_647 . . . ?
O4 Cu2 O4 Cu1 -112.31(12) 3_677 . . . ?
O4 Cu2 O4 Cu1 72.05(12) 4_575 . . . ?
O3 Cu2 O4 Cu1 -0.61(7) . . . . ?
Cu2 Cu2 O4 Cu1 76.49(13) 3_667 . . . ?
Cu2 Cu2 O4 Cu1 -112.31(13) 3_677 . . . ?
O3 Cu1 O4 Cu2 75.31(12) 3_777 . . 3_677 ?
O3 Cu1 O4 Cu2 -104.69(12) . . . 3_677 ?
O4 Cu1 O4 Cu2 90(12) 3_777 . . 3_677 ?
Cu1 Cu1 O4 Cu2 37.61(8) 2_757 . . 3_677 ?
Cu1 Cu1 O4 Cu2 -142.39(8) 2_747 . . 3_677 ?
O3 Cu1 O4 Cu2 -179.28(8) 3_777 . . . ?
O3 Cu1 O4 Cu2 0.72(8) . . . . ?
O4 Cu1 O4 Cu2 -165(12) 3_777 . . . ?
Cu1 Cu1 O4 Cu2 143.01(7) 2_757 . . . ?
Cu1 Cu1 O4 Cu2 -36.99(7) 2_747 . . . ?
O2 S1 C1 C2 -76.6(3) . . . 4_575 ?
O2 S1 C1 C2 76.6(3) . . . . ?
C2 C1 C2 C2 -44.4(12) 4_575 . . 3_676 ?
S1 C1 C2 C2 174.6(6) . . . 3_676 ?

_diffrn_measured_fraction_theta_max 0.978
_diffrn_reflns_theta_full        27.47
_diffrn_measured_fraction_theta_full 0.978
_refine_diff_density_max         0.868
_refine_diff_density_min         -0.712
_refine_diff_density_rms         0.159
