# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2015

####################################################################### 
# 
# 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_SCD2
_database_code_depnum_ccdc_archive 'CCDC 1061483'
_audit_update_record             
;
2015-04-23 deposited with the CCDC.
2015-07-28 downloaded from the CCDC.
;

#####################################################################
#                     CHEMICAL INFORMATION                          #
#####################################################################
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         'C14 H10 Cd N6 S2'
_chemical_formula_sum            'C14 H10 Cd N6 S2'
_chemical_formula_weight         438.83
_chemical_melting_point          ?
_chemical_compound_source        ?

#####################################################################
#                    UNIT CELL INFORMATION                          #
#####################################################################
_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_Hall  '-P 1'

loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z

_cell_length_a                   6.0349(13)
_cell_length_b                   8.2409(19)
_cell_length_c                   8.7848(19)
_cell_angle_alpha                110.302(4)
_cell_angle_beta                 100.984(4)
_cell_angle_gamma                93.003(3)
_cell_volume                     398.90(15)
_cell_formula_units_Z            1
_cell_measurement_temperature    294(2)
_cell_measurement_reflns_used    226
_cell_measurement_theta_min      ?7.48
_cell_measurement_theta_max      20.51

#####################################################################
#                      CRYSTAL INFORMATION                          #
#####################################################################
_exptl_crystal_description       needle
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.04
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.827
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             216
_exptl_special_details           ?

#####################################################################
#                      ABSORPTION CORRECTION                        #
#####################################################################
_exptl_absorpt_coefficient_mu    1.637
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2008)'
_exptl_absorpt_correction_T_min  0.834
_exptl_absorpt_correction_T_max  0.940

#####################################################################
#                         DATA COLLECTION                           #
#####################################################################
_diffrn_ambient_temperature      294(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       'Bruker APEX-II CCD'
_diffrn_measurement_method       'ω scans'
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            2411
_diffrn_reflns_av_R_equivalents  0.0178
_diffrn_reflns_av_sigmaI/netI    0.0340
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       9
_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        25.25
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_theta_min         2.54
_diffrn_reflns_theta_max         25.25
_reflns_number_total             1444
_reflns_number_gt                1350
_reflns_threshold_expression     I>2σ(I)

#####################################################################
#                       COMPUTING PROGRAMS                          #
#####################################################################
_computing_data_collection       'APEX2 (Bruker, 2008)'
_computing_cell_refinement       'SAINT (Bruker, 2008)'
_computing_data_reduction        SAINT
_computing_structure_solution    'SIR97 (Altomare et al., 1999)'
_computing_structure_refinement  'SHELX97-L (Sheldrick, 2008)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

#####################################################################
#                     REFINEMENT INFORMATION                        #
#####################################################################
_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)+(0.0430P)²+0.1008P] where P=(Fo²+2Fc²)/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         1444
_refine_ls_number_parameters     106
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0356
_refine_ls_R_factor_gt           0.0321
_refine_ls_wR_factor_ref         0.0764
_refine_ls_wR_factor_gt          0.0744
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_restrained_S_all      1.071
_refine_ls_abs_structure_Flack   ?
_refine_ls_abs_structure_details ?
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         0.390
_refine_diff_density_min         -0.434
_refine_diff_density_rms         0.092

#####################################################################
#      ATOMIC TYPES, COORDINATES AND DISPLACEMENT PARAMETERS        #
#####################################################################
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Cd Cd -0.8075 1.2024 '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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'

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
Cd1 Cd 0.0000 0.0000 0.0000 0.03274(16) Uani 1 2 d S . .
S1 S 0.75593(16) 0.26581(13) -0.03917(13) 0.0385(3) Uani 1 1 d . . .
N1 N 0.0442(5) 0.1245(4) 0.2924(4) 0.0307(7) Uani 1 1 d . . .
N2 N -0.4243(5) 0.4438(4) 0.4647(4) 0.0358(7) Uani 1 1 d . . .
N3 N 0.3264(6) 0.1634(5) 0.0027(4) 0.0437(8) Uani 1 1 d . . .
C1 C 0.2180(6) 0.1069(5) 0.4040(5) 0.0343(9) Uani 1 1 d . . .
H1 H 0.3288 0.0399 0.3648 0.041 Uiso 1 1 calc R . .
C2 C 0.2402(7) 0.1832(5) 0.5737(5) 0.0382(9) Uani 1 1 d . . .
H2 H 0.3612 0.1654 0.6467 0.046 Uiso 1 1 calc R . .
C3 C 0.0801(6) 0.2865(5) 0.6334(4) 0.0329(8) Uani 1 1 d . . .
H3 H 0.0933 0.3413 0.7473 0.039 Uiso 1 1 calc R . .
C4 C -0.1001(6) 0.3071(5) 0.5214(4) 0.0290(8) Uani 1 1 d . . .
C5 C -0.1116(6) 0.2228(5) 0.3535(4) 0.0317(8) Uani 1 1 d . . .
H5 H -0.2347 0.2349 0.2783 0.038 Uiso 1 1 calc R . .
C6 C -0.2711(6) 0.4207(5) 0.5749(5) 0.0328(8) Uani 1 1 d . . .
H6 H -0.2683 0.4753 0.6874 0.039 Uiso 1 1 calc R . .
C7 C 0.5031(7) 0.2050(5) -0.0143(4) 0.0333(8) Uani 1 1 d . . .


#####################################################################
#                       MOLECULAR GEOMETRY                          #
#####################################################################
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
Cd1 N3 2.318(3) . ?
Cd1 N3 2.318(3) 2 ?
Cd1 N1 2.367(3) . ?
Cd1 N1 2.367(3) 2 ?
Cd1 S1 2.7846(11) 2_655 ?
Cd1 S1 2.7846(11) 1_455 ?
S1 C7 1.659(4) . ?
S1 Cd1 2.7846(11) 1_655 ?
N1 C5 1.340(4) . ?
N1 C1 1.344(4) . ?
N2 C6 1.278(5) . ?
N2 N2 1.409(6) 2_466 ?
N3 C7 1.155(5) . ?
C1 C2 1.378(6) . ?
C1 H1 0.9300 . ?
C2 C3 1.379(5) . ?
C2 H2 0.9300 . ?
C3 C4 1.381(5) . ?
C3 H3 0.9300 . ?
C4 C5 1.381(5) . ?
C4 C6 1.464(5) . ?
C5 H5 0.9300 . ?
C6 H6 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
N3 Cd1 N3 180.00(19) . 2 ?
N3 Cd1 N1 93.45(11) . . ?
N3 Cd1 N1 86.55(11) 2 . ?
N3 Cd1 N1 86.55(11) . 2 ?
N3 Cd1 N1 93.45(11) 2 2 ?
N1 Cd1 N1 180.00(15) . 2 ?
N3 Cd1 S1 91.75(9) . 2_655 ?
N3 Cd1 S1 88.25(9) 2 2_655 ?
N1 Cd1 S1 89.38(7) . 2_655 ?
N1 Cd1 S1 90.62(7) 2 2_655 ?
N3 Cd1 S1 88.25(9) . 1_455 ?
N3 Cd1 S1 91.75(9) 2 1_455 ?
N1 Cd1 S1 90.62(7) . 1_455 ?
N1 Cd1 S1 89.38(7) 2 1_455 ?
S1 Cd1 S1 180.0 2_655 1_455 ?
C7 S1 Cd1 101.83(13) . 1_655 ?
C5 N1 C1 116.7(3) . . ?
C5 N1 Cd1 118.6(2) . . ?
C1 N1 Cd1 124.7(2) . . ?
C6 N2 N2 112.4(4) . 2_466 ?
C7 N3 Cd1 163.3(3) . . ?
N1 C1 C2 123.2(3) . . ?
N1 C1 H1 118.4 . . ?
C2 C1 H1 118.4 . . ?
C1 C2 C3 118.9(3) . . ?
C1 C2 H2 120.5 . . ?
C3 C2 H2 120.5 . . ?
C2 C3 C4 119.0(3) . . ?
C2 C3 H3 120.5 . . ?
C4 C3 H3 120.5 . . ?
C3 C4 C5 118.1(3) . . ?
C3 C4 C6 122.2(3) . . ?
C5 C4 C6 119.6(3) . . ?
N1 C5 C4 123.9(3) . . ?
N1 C5 H5 118.0 . . ?
C4 C5 H5 118.0 . . ?
N2 C6 C4 119.1(3) . . ?
N2 C6 H6 120.5 . . ?
C4 C6 H6 120.5 . . ?
N3 C7 S1 179.6(4) . . ?

#####################################################################
#                  SHELXL-97 instruction file (.RES)                #
#              produced by the last cycles of refinement            #
#####################################################################
_iucr_refine_instruction_details 
;
TITL SCD2 - P-1
CELL 0.71073 6.0349 8.2409 8.7848 110.302 100.984 93.003
ZERR   1    0.0013 0.0019 0.0019   0.004   0.004  0.003
LATT  1
SFAC  C   H   CD  N  S
UNIT  14  10  1  6  2
TEMP  21
SIZE  0.18 0.07 0.04
REM  Crystal colour: yellow
MERG  2
OMIT  -2  50.5
L.S.  10
FMAP  2
PLAN  25
BOND  $H
ACTA
WGHT    0.043000    0.100800
FVAR       0.95248
CD1   3    0.000000    0.000000    0.000000    10.50000    0.02417    0.04440 =
         0.02697    0.00810    0.00804    0.00711
S1    5    0.755935    0.265806   -0.039173    11.00000    0.03108    0.04669 =
         0.04303    0.01986    0.01328    0.00812
N1    4    0.044159    0.124544    0.292401    11.00000    0.02805    0.03512 =
         0.02844    0.01033    0.00691    0.00600
N2    4   -0.424258    0.443816    0.464680    11.00000    0.03482    0.03867 =
         0.03363    0.00929    0.01305    0.01040
N3    4    0.326355    0.163429    0.002725    11.00000    0.02708    0.05164 =
         0.05018    0.01717    0.00709    0.00175
C1    1    0.218022    0.106886    0.404019    11.00000    0.02704    0.03733 =
         0.03799    0.01204    0.00778    0.01009
AFIX  43
H1    2    0.328791    0.039852    0.364843    11.00000   -1.20000
AFIX   0
C2    1    0.240215    0.183226    0.573655    11.00000    0.03437    0.04483 =
         0.03444    0.01669   -0.00060    0.01142
AFIX  43
H2    2    0.361235    0.165413    0.646718    11.00000   -1.20000
AFIX   0
C3    1    0.080117    0.286460    0.633356    11.00000    0.03463    0.03825 =
         0.02172    0.00835    0.00226    0.00204
AFIX  43
H3    2    0.093321    0.341347    0.747325    11.00000   -1.20000
AFIX   0
C4    1   -0.100104    0.307127    0.521399    11.00000    0.03047    0.03055 =
         0.02620    0.01019    0.00713    0.00291
C5    1   -0.111562    0.222782    0.353480    11.00000    0.02707    0.03811 =
         0.02688    0.01039    0.00089    0.00829
AFIX  43
H5    2   -0.234710    0.234884    0.278299    11.00000   -1.20000
AFIX   0
C6    1   -0.271069    0.420704    0.574857    11.00000    0.03694    0.03365 =
         0.02738    0.00718    0.01374    0.00496
AFIX  43
H6    2   -0.268267    0.475296    0.687440    11.00000   -1.20000
AFIX   0
C7    1    0.503062    0.205013   -0.014275    11.00000    0.03318    0.03838 =
         0.02566    0.01037    0.00080    0.01065
HKLF      4
 
REM  SCD2 - P-1
REM R1 =  0.0321 for   1350 Fo > 4sig(Fo)  and  0.0356 for all   1444 data
REM    106 parameters refined using      0 restraints
 
END  
     
WGHT      0.0430      0.1026 
REM Highest difference peak  0.390,  deepest hole -0.434,  1-sigma level  0.092
Q1    1   0.7083  0.3229 -0.1373  11.00000  0.05    0.39
Q2    1   0.0952  0.0646  0.3257  11.00000  0.05    0.37
Q3    1   0.0684  0.2733  0.1073  11.00000  0.05    0.36
Q4    1   0.4578  0.3803  0.1203  11.00000  0.05    0.34
Q5    1   0.0454 -0.0600  0.0963  11.00000  0.05    0.33
Q6    1   0.9049  0.2830 -0.1089  11.00000  0.05    0.33
Q7    1   0.7285  0.1431 -0.1033  11.00000  0.05    0.32
Q8    1   0.2123 -0.0415  0.0689  11.00000  0.05    0.32
Q9    1   0.1405  0.0385 -0.0432  11.00000  0.05    0.32
Q10   1   0.0823 -0.1213 -0.0291  11.00000  0.05    0.31
Q11   1  -0.3897  0.3701  0.5197  11.00000  0.05    0.30
Q12   1   0.3203  0.3063  0.1575  11.00000  0.05    0.30
Q13   1   0.2194  0.1934  0.4833  11.00000  0.05    0.30
Q14   1   0.1054  0.2224  0.5805  11.00000  0.05    0.29
Q15   1   0.0995  0.1383  0.0725  11.00000  0.05    0.28
Q16   1   0.8505  0.2408  0.0484  11.00000  0.05    0.27
Q17   1   0.1844  0.3107  0.4362  11.00000  0.05    0.27
Q18   1   0.0588 -0.1386  0.0639  11.00000  0.05    0.27
Q19   1   0.3088  0.0656  0.6438  11.00000  0.05    0.27
Q20   1   0.3357  0.0289  0.1566  11.00000  0.05    0.26
Q21   1   0.2025  0.2228 -0.0950  11.00000  0.05    0.26
Q22   1   0.5071  0.1187 -0.0053  11.00000  0.05    0.25
Q23   1  -0.1565  0.2229  0.1410  11.00000  0.05    0.25
Q24   1  -0.5255  0.3917  0.3389  11.00000  0.05    0.25
Q25   1   0.7516  0.4339  0.1431  11.00000  0.05    0.25
;
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: methanol/water'
