# Electronic Supplementary Material (ESI) for CrystEngComm
# This journal is © The Royal Society of Chemistry 2013

#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_1
#TrackingRef '1.cif'


_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C24 H24 Cu4 I2 N4 S4 W'
_chemical_formula_sum            'C24 H24 Cu4 I2 N4 S4 W'
_chemical_formula_weight         1188.52

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'
S S 0.1246 0.1234 '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'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_H-M   P4(2)/n
_symmetry_space_group_name_Hall  '-P 4bc'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y+1/2, z'
'-y, x+1/2, z+1/2'
'y+1/2, -x, z+1/2'
'-x, -y, -z'
'x-1/2, y-1/2, -z'
'y, -x-1/2, -z-1/2'
'-y-1/2, x, -z-1/2'

_cell_length_a                   9.3967(3)
_cell_length_b                   9.3967(3)
_cell_length_c                   32.3703(18)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     2858.2(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    9956
_cell_measurement_theta_min      2.258
_cell_measurement_theta_max      28.374

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.22
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.381
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1112
_exptl_absorpt_coefficient_mu    4.708
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.242
_exptl_absorpt_correction_T_max  0.355
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      296(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  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            15761
_diffrn_reflns_av_R_equivalents  0.0244
_diffrn_reflns_av_sigmaI/netI    0.0158
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_theta_min         1.26
_diffrn_reflns_theta_max         25.00
_reflns_number_total             2510
_reflns_number_gt                2322
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_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 F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ 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/[\s^2^(Fo^2^)+(0.0856P)^2^+6.9900P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         2510
_refine_ls_number_parameters     83
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0345
_refine_ls_R_factor_gt           0.0323
_refine_ls_wR_factor_ref         0.1217
_refine_ls_wR_factor_gt          0.1202
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_restrained_S_all      1.010
_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
W1 W 0.2500 0.2500 0.2500 0.02754(15) Uani 1 4 d S . .
I2 I 0.7500 0.2500 0.296725(16) 0.04658(19) Uani 1 2 d S . .
Cu1 Cu 0.53281(8) 0.31733(8) 0.24869(2) 0.0418(2) Uani 1 1 d U . .
S1 S 0.41415(14) 0.14309(13) 0.21129(4) 0.035 Uani 1 1 d U . .
N1 N 0.6165(5) 0.4411(5) 0.20235(15) 0.0451(11) Uani 1 1 d U . .
C3 C 0.7283(6) 0.5919(6) 0.13439(18) 0.0429(12) Uani 1 1 d . . .
C4 C 0.8019(6) 0.5796(6) 0.17182(18) 0.0424(12) Uani 1 1 d . . .
H4 H 0.8911 0.6214 0.1745 0.051 Uiso 1 1 calc R . .
C6 C 0.7835(7) 0.6743(7) 0.09844(19) 0.0506(14) Uani 1 1 d . . .
H6A H 0.7597 0.6256 0.0729 0.061 Uiso 1 1 calc R . .
H6B H 0.8863 0.6817 0.1002 0.061 Uiso 1 1 calc R . .
C5 C 0.7446(5) 0.5069(6) 0.20461(18) 0.0406(13) Uani 1 1 d . . .
H5 H 0.7954 0.5026 0.2292 0.049 Uiso 1 1 calc R . .
C2 C 0.5957(7) 0.5226(8) 0.1330(2) 0.0614(18) Uani 1 1 d . . .
H2 H 0.5431 0.5218 0.1086 0.074 Uiso 1 1 calc R . .
C1 C 0.5452(7) 0.4575(8) 0.1670(2) 0.065(2) Uani 1 1 d U . .
H1 H 0.4533 0.4210 0.1657 0.078 Uiso 1 1 calc 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
W1 0.02252(18) 0.02252(18) 0.0376(3) 0.000 0.000 0.000
I2 0.0272(3) 0.0672(4) 0.0453(3) 0.000 0.000 0.0081(2)
Cu1 0.0278(4) 0.0403(4) 0.0575(5) 0.0001(3) 0.0023(3) -0.0027(3)
S1 0.032 0.033 0.041 -0.004 0.010 -0.002
N1 0.034(2) 0.045(3) 0.056(3) 0.007(2) -0.0023(18) -0.007(2)
C3 0.043(3) 0.039(3) 0.047(3) -0.001(2) 0.004(2) -0.007(2)
C4 0.031(3) 0.041(3) 0.055(3) 0.003(2) 0.002(2) -0.011(2)
C6 0.061(4) 0.047(3) 0.044(3) -0.003(3) 0.005(3) -0.004(3)
C5 0.022(2) 0.041(3) 0.059(4) 0.007(2) -0.009(2) -0.003(2)
C2 0.062(4) 0.065(4) 0.057(4) 0.005(3) -0.019(3) -0.023(3)
C1 0.048(4) 0.073(5) 0.074(4) 0.024(4) -0.021(3) -0.036(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
W1 S1 2.2268(12) 8_656 ?
W1 S1 2.2268(12) 7_566 ?
W1 S1 2.2268(12) . ?
W1 S1 2.2268(12) 2 ?
W1 Cu1 2.7321(7) . ?
W1 Cu1 2.7321(7) 8_656 ?
W1 Cu1 2.7321(7) 2 ?
W1 Cu1 2.7321(7) 7_566 ?
I2 Cu1 2.6427(8) . ?
I2 Cu1 2.6427(8) 2_655 ?
Cu1 N1 2.054(5) . ?
Cu1 S1 2.2888(15) 8_656 ?
Cu1 S1 2.3214(14) . ?
S1 Cu1 2.2888(15) 7_566 ?
N1 C1 1.336(8) . ?
N1 C5 1.355(7) . ?
C3 C4 1.400(8) . ?
C3 C2 1.407(9) . ?
C3 C6 1.491(8) . ?
C4 C5 1.373(8) . ?
C4 H4 0.9300 . ?
C6 C6 1.555(13) 2_665 ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C5 H5 0.9300 . ?
C2 C1 1.345(10) . ?
C2 H2 0.9300 . ?
C1 H1 0.9300 . ?

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
S1 W1 S1 111.51(7) 8_656 7_566 ?
S1 W1 S1 108.46(4) 8_656 . ?
S1 W1 S1 108.46(4) 7_566 . ?
S1 W1 S1 108.46(4) 8_656 2 ?
S1 W1 S1 108.46(4) 7_566 2 ?
S1 W1 S1 111.51(7) . 2 ?
S1 W1 Cu1 53.81(4) 8_656 . ?
S1 W1 Cu1 127.44(4) 7_566 . ?
S1 W1 Cu1 54.69(4) . . ?
S1 W1 Cu1 124.09(4) 2 . ?
S1 W1 Cu1 54.69(4) 8_656 8_656 ?
S1 W1 Cu1 124.09(4) 7_566 8_656 ?
S1 W1 Cu1 127.44(4) . 8_656 ?
S1 W1 Cu1 53.81(4) 2 8_656 ?
Cu1 W1 Cu1 90.0 . 8_656 ?
S1 W1 Cu1 127.44(4) 8_656 2 ?
S1 W1 Cu1 53.81(4) 7_566 2 ?
S1 W1 Cu1 124.09(4) . 2 ?
S1 W1 Cu1 54.69(4) 2 2 ?
Cu1 W1 Cu1 178.21(3) . 2 ?
Cu1 W1 Cu1 90.0 8_656 2 ?
S1 W1 Cu1 124.09(4) 8_656 7_566 ?
S1 W1 Cu1 54.69(4) 7_566 7_566 ?
S1 W1 Cu1 53.81(4) . 7_566 ?
S1 W1 Cu1 127.44(4) 2 7_566 ?
Cu1 W1 Cu1 90.0 . 7_566 ?
Cu1 W1 Cu1 178.21(3) 8_656 7_566 ?
Cu1 W1 Cu1 90.0 2 7_566 ?
Cu1 I2 Cu1 107.91(4) . 2_655 ?
N1 Cu1 S1 117.69(15) . 8_656 ?
N1 Cu1 S1 101.68(15) . . ?
S1 Cu1 S1 103.22(6) 8_656 . ?
N1 Cu1 I2 105.63(14) . . ?
S1 Cu1 I2 108.65(4) 8_656 . ?
S1 Cu1 I2 120.59(5) . . ?
N1 Cu1 W1 120.99(14) . . ?
S1 Cu1 W1 51.74(3) 8_656 . ?
S1 Cu1 W1 51.51(3) . . ?
I2 Cu1 W1 133.36(3) . . ?
W1 S1 Cu1 74.45(4) . 7_566 ?
W1 S1 Cu1 73.81(4) . . ?
Cu1 S1 Cu1 113.90(6) 7_566 . ?
C1 N1 C5 116.0(5) . . ?
C1 N1 Cu1 120.0(4) . . ?
C5 N1 Cu1 124.0(4) . . ?
C4 C3 C2 115.3(5) . . ?
C4 C3 C6 123.1(5) . . ?
C2 C3 C6 121.6(6) . . ?
C5 C4 C3 121.1(5) . . ?
C5 C4 H4 119.5 . . ?
C3 C4 H4 119.5 . . ?
C3 C6 C6 109.5(5) . 2_665 ?
C3 C6 H6A 109.8 . . ?
C6 C6 H6A 109.8 2_665 . ?
C3 C6 H6B 109.8 . . ?
C6 C6 H6B 109.8 2_665 . ?
H6A C6 H6B 108.2 . . ?
N1 C5 C4 122.3(5) . . ?
N1 C5 H5 118.9 . . ?
C4 C5 H5 118.9 . . ?
C1 C2 C3 119.8(6) . . ?
C1 C2 H2 120.1 . . ?
C3 C2 H2 120.1 . . ?
N1 C1 C2 125.2(6) . . ?
N1 C1 H1 117.4 . . ?
C2 C1 H1 117.4 . . ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.566
_refine_diff_density_min         -1.391
_refine_diff_density_rms         0.105

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 -0.021 -0.007 0.000 739 326 ' '
2 -0.023 0.193 0.500 739 324 ' '
_platon_squeeze_details          
;
;


_database_code_depnum_ccdc_archive 'CCDC 926784'