# Electronic Supplementary Material (ESI) for RSC Advances.
# This journal is © The Royal Society of Chemistry 2018

####################################################################### 
# 
# 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_Zn1MeImz2SCN2
_database_code_depnum_ccdc_archive 'CCDC 1588816'
_audit_update_record             
;
2017-12-03 deposited with the CCDC.
2018-06-25 downloaded from the CCDC.
;
_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        dithiocianato-bis(1-methylimidazole)zinc(II)
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C10 H12 N6 S2 Zn'
_chemical_formula_weight         345.75

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'
Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'
_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+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   11.9876(6)
_cell_length_b                   11.6755(4)
_cell_length_c                   11.8909(5)
_cell_angle_alpha                90
_cell_angle_beta                 109.447(5)
_cell_angle_gamma                90
_cell_volume                     1569.32(12)
_cell_formula_units_Z            4
_cell_measurement_temperature    297(2)
_cell_measurement_reflns_used    1757
_cell_measurement_theta_min      3.8850
_cell_measurement_theta_max      24.2510
_exptl_crystal_description       fragment
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.463
_exptl_crystal_F_000             704
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.282
_exptl_crystal_size_mid          0.134
_exptl_crystal_size_min          0.098
_exptl_absorpt_coefficient_mu    1.826
_shelx_estimated_absorpt_T_min   0.627
_shelx_estimated_absorpt_T_max   0.841
_exptl_absorpt_correction_T_min  0.94186
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_oxdiff_exptl_absorpt_empirical_full_min 0.957
_oxdiff_exptl_absorpt_empirical_full_max 1.084
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      297(2)
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Eos
_diffrn_detector_area_resol_mean 16.0604
_diffrn_reflns_number            7733
_diffrn_reflns_av_unetI/netI     0.0387
_diffrn_reflns_av_R_equivalents  0.0272
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         3.432
_diffrn_reflns_theta_max         28.820
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.827
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.827
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.827
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             3397
_reflns_number_gt                2153
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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    'SHELXT (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_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)+(0.0381P)²+0.3380P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         3397
_refine_ls_number_parameters     198
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0771
_refine_ls_R_factor_gt           0.0393
_refine_ls_wR_factor_ref         0.0985
_refine_ls_wR_factor_gt          0.0803
_refine_ls_goodness_of_fit_ref   1.006
_refine_ls_restrained_S_all      1.006
_refine_ls_shift/su_max          0.008
_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
C1 C 0.4626(3) 0.7391(3) 0.4000(3) 0.0691(8) Uani 1 1 d . . . . .
C2 C 0.8747(3) 0.8526(3) 0.6507(3) 0.0658(8) Uani 1 1 d . . . . .
C11 C 0.7973(3) 0.4314(3) 0.5544(3) 0.0724(9) Uani 1 1 d . . . . .
C12 C 0.8154(3) 0.5476(4) 0.4240(3) 0.0802(10) Uani 1 1 d . . . . .
C13 C 0.8661(4) 0.4504(5) 0.4100(4) 0.0918(13) Uani 1 1 d . . . . .
C14 C 0.8981(4) 0.2586(3) 0.5143(5) 0.1299(17) Uani 1 1 d . . . . .
H14A H 0.8791 0.2272 0.5803 0.195 Uiso 1 1 calc R U . . .
H14B H 0.9823 0.2581 0.5323 0.195 Uiso 1 1 calc R U . . .
H14C H 0.8614 0.2133 0.4444 0.195 Uiso 1 1 calc R U . . .
C21 C 0.5591(3) 0.5341(3) 0.7152(3) 0.0663(8) Uani 1 1 d . . . . .
C22 C 0.7328(4) 0.5634(4) 0.8371(3) 0.0796(10) Uani 1 1 d . . . . .
C23 C 0.6756(4) 0.5021(3) 0.8933(3) 0.0798(10) Uani 1 1 d . . . . .
C24 C 0.4719(4) 0.4157(3) 0.8384(3) 0.0994(12) Uani 1 1 d . . . . .
H24A H 0.3961 0.4453 0.7909 0.149 Uiso 1 1 calc R U . . .
H24B H 0.4798 0.4205 0.9213 0.149 Uiso 1 1 calc R U . . .
H24C H 0.4783 0.3372 0.8173 0.149 Uiso 1 1 calc R U . . .
N1 N 0.5479(3) 0.7022(3) 0.4661(3) 0.0838(8) Uani 1 1 d . . . . .
N2 N 0.8067(3) 0.7823(3) 0.6436(3) 0.0891(9) Uani 1 1 d . . . . .
N11 N 0.7718(2) 0.5366(2) 0.5165(2) 0.0656(6) Uani 1 1 d . . . . .
N12 N 0.8544(2) 0.3764(3) 0.4929(3) 0.0786(8) Uani 1 1 d . . . . .
N21 N 0.6584(2) 0.5849(2) 0.7214(2) 0.0654(7) Uani 1 1 d . . . . .
N22 N 0.5654(2) 0.4829(2) 0.8163(2) 0.0675(7) Uani 1 1 d . . . . .
S1 S 0.34352(9) 0.79023(10) 0.30812(10) 0.1028(4) Uani 1 1 d . . . . .
S2 S 0.96811(10) 0.95304(10) 0.66011(10) 0.1057(4) Uani 1 1 d . . . . .
Zn Zn 0.69634(3) 0.65632(3) 0.58696(3) 0.06862(16) Uani 1 1 d . . . . .
H11 H 0.776(2) 0.398(3) 0.615(3) 0.067(9) Uiso 1 1 d . . . . .
H12 H 0.805(3) 0.611(3) 0.382(3) 0.087(12) Uiso 1 1 d . . . . .
H13 H 0.904(3) 0.434(3) 0.361(3) 0.109(14) Uiso 1 1 d . . . . .
H21 H 0.494(3) 0.533(2) 0.651(3) 0.063(9) Uiso 1 1 d . . . . .
H22 H 0.802(3) 0.591(3) 0.850(3) 0.090(13) Uiso 1 1 d . . . . .
H23 H 0.696(3) 0.474(3) 0.969(3) 0.091(11) Uiso 1 1 d . . . . .

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
C1 0.082(2) 0.0523(17) 0.074(2) -0.0029(16) 0.0273(19) -0.0036(17)
C2 0.072(2) 0.069(2) 0.0551(18) -0.0047(15) 0.0200(16) 0.0000(18)
C11 0.077(2) 0.070(2) 0.073(2) 0.0016(18) 0.0281(19) 0.0009(19)
C12 0.074(2) 0.097(3) 0.068(2) 0.002(2) 0.0217(19) -0.013(2)
C13 0.076(3) 0.126(4) 0.080(3) -0.031(3) 0.035(2) -0.019(3)
C14 0.113(4) 0.080(3) 0.192(5) -0.037(3) 0.044(3) 0.015(3)
C21 0.070(2) 0.068(2) 0.0544(19) 0.0004(16) 0.0115(18) -0.0052(18)
C22 0.062(2) 0.100(3) 0.068(2) -0.014(2) 0.0097(19) 0.006(2)
C23 0.089(3) 0.091(3) 0.056(2) 0.0071(19) 0.019(2) 0.019(2)
C24 0.125(3) 0.093(3) 0.089(2) 0.007(2) 0.047(2) -0.018(3)
N1 0.082(2) 0.0787(18) 0.0789(19) -0.0067(15) 0.0108(16) 0.0101(17)
N2 0.096(2) 0.0732(18) 0.093(2) -0.0049(16) 0.0239(18) -0.0191(18)
N11 0.0658(16) 0.0658(16) 0.0643(15) 0.0007(13) 0.0206(13) -0.0004(14)
N12 0.0664(18) 0.0753(18) 0.091(2) -0.0240(17) 0.0217(16) -0.0046(15)
N21 0.0656(17) 0.0663(16) 0.0616(16) -0.0060(12) 0.0175(13) 0.0009(14)
N22 0.0803(19) 0.0617(15) 0.0599(16) 0.0017(12) 0.0225(15) 0.0008(14)
S1 0.0821(7) 0.0969(7) 0.1115(8) 0.0285(6) 0.0083(6) 0.0109(6)
S2 0.0930(7) 0.1124(8) 0.1145(8) -0.0100(6) 0.0382(6) -0.0378(7)
Zn 0.0719(3) 0.0597(2) 0.0705(3) -0.00243(17) 0.01879(19) -0.00286(18)

_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
C1 N1 1.147(4) . ?
C1 S1 1.596(4) . ?
C2 N2 1.140(4) . ?
C2 S2 1.600(4) . ?
C11 N11 1.309(4) . ?
C11 N12 1.323(4) . ?
C12 C13 1.323(6) . ?
C12 N11 1.373(4) . ?
C13 N12 1.353(5) . ?
C14 N12 1.463(5) . ?
C21 N21 1.309(4) . ?
C21 N22 1.322(4) . ?
C22 C23 1.317(5) . ?
C22 N21 1.390(4) . ?
C23 N22 1.352(4) . ?
C24 N22 1.461(4) . ?
N1 Zn 1.953(3) . ?
N2 Zn 1.943(3) . ?
N11 Zn 1.994(2) . ?
N21 Zn 1.986(2) . ?

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 C1 S1 179.7(4) . . ?
N2 C2 S2 178.8(3) . . ?
N11 C11 N12 111.7(3) . . ?
C13 C12 N11 109.5(4) . . ?
C12 C13 N12 107.1(4) . . ?
N21 C21 N22 112.2(3) . . ?
C23 C22 N21 109.2(4) . . ?
C22 C23 N22 107.7(3) . . ?
C1 N1 Zn 173.5(3) . . ?
C2 N2 Zn 163.4(3) . . ?
C11 N11 C12 104.8(3) . . ?
C11 N11 Zn 126.9(2) . . ?
C12 N11 Zn 128.2(3) . . ?
C11 N12 C13 106.9(3) . . ?
C11 N12 C14 125.5(4) . . ?
C13 N12 C14 127.6(4) . . ?
C21 N21 C22 104.3(3) . . ?
C21 N21 Zn 126.3(2) . . ?
C22 N21 Zn 128.9(3) . . ?
C21 N22 C23 106.7(3) . . ?
C21 N22 C24 126.2(3) . . ?
C23 N22 C24 127.0(3) . . ?
N2 Zn N1 113.33(13) . . ?
N2 Zn N21 110.52(12) . . ?
N1 Zn N21 108.09(12) . . ?
N2 Zn N11 108.97(12) . . ?
N1 Zn N11 108.20(11) . . ?
N21 Zn N11 107.54(10) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
C11 H11 S1 0.93(3) 2.93(3) 3.749(4) 148(2) 3_666

_refine_diff_density_max         0.326
_refine_diff_density_min         -0.277
_refine_diff_density_rms         0.045

_shelx_res_file                  
;

    shelx.res created by SHELXL-2014/7


TITL shelxt_a.res in P2(1)/c
CELL  0.71073  11.9876  11.6755  11.8909   90.000  109.447   90.000
ZERR     4.00   0.0006   0.0004   0.0005    0.000    0.005    0.000
LATT   1
SYMM  - X, 1/2 + Y, 1/2 - Z
SFAC  C   H   N   S  ZN
UNIT  40  48  24  8  4
MERG   2
SIZE  0.098 0.134 0.282
TEMP 24
REM  Crystal shape/color: fragment/colourless
FMAP   2
PLAN  -3
EQIV $1 -x+1, -y+1, -z+1
HTAB C11 S1_$1
ACTA
L.S.   15
WGHT    0.038100    0.338000
FVAR       2.80153
C1    1    0.462578    0.739143    0.399968    11.00000    0.08164    0.05228 =
         0.07426   -0.00294    0.02725   -0.00364
C2    1    0.874729    0.852553    0.650708    11.00000    0.07217    0.06922 =
         0.05509   -0.00472    0.02001   -0.00002
C11   1    0.797256    0.431407    0.554368    11.00000    0.07661    0.06951 =
         0.07342    0.00158    0.02810    0.00086
C12   1    0.815420    0.547628    0.423952    11.00000    0.07430    0.09682 =
         0.06807    0.00242    0.02167   -0.01341
C13   1    0.866069    0.450429    0.409976    11.00000    0.07599    0.12617 =
         0.07978   -0.03051    0.03463   -0.01884
C14   1    0.898068    0.258592    0.514313    11.00000    0.11303    0.07990 =
         0.19201   -0.03695    0.04445    0.01492
AFIX 137
H14A  2    0.879114    0.227162    0.580345    11.00000   -1.50000
H14B  2    0.982299    0.258058    0.532278    11.00000   -1.50000
H14C  2    0.861411    0.213275    0.444357    11.00000   -1.50000
AFIX   0
C21   1    0.559128    0.534073    0.715184    11.00000    0.06950    0.06815 =
         0.05437    0.00040    0.01146   -0.00517
C22   1    0.732821    0.563378    0.837055    11.00000    0.06152    0.10020 =
         0.06829   -0.01359    0.00974    0.00584
C23   1    0.675556    0.502130    0.893292    11.00000    0.08923    0.09082 =
         0.05568    0.00710    0.01927    0.01902
C24   1    0.471883    0.415713    0.838356    11.00000    0.12474    0.09301 =
         0.08862    0.00717    0.04652   -0.01828
AFIX 137
H24A  2    0.396116    0.445349    0.790936    11.00000   -1.50000
H24B  2    0.479829    0.420470    0.921267    11.00000   -1.50000
H24C  2    0.478286    0.337189    0.817344    11.00000   -1.50000
AFIX   0
N1    3    0.547874    0.702160    0.466109    11.00000    0.08184    0.07870 =
         0.07894   -0.00668    0.01081    0.01013
N2    3    0.806652    0.782330    0.643631    11.00000    0.09579    0.07318 =
         0.09284   -0.00486    0.02389   -0.01911
N11   3    0.771757    0.536593    0.516494    11.00000    0.06582    0.06577 =
         0.06432    0.00068    0.02057   -0.00038
N12   3    0.854441    0.376390    0.492909    11.00000    0.06640    0.07528 =
         0.09065   -0.02399    0.02166   -0.00459
N21   3    0.658379    0.584909    0.721442    11.00000    0.06557    0.06635 =
         0.06159   -0.00596    0.01754    0.00088
N22   3    0.565379    0.482890    0.816316    11.00000    0.08027    0.06166 =
         0.05989    0.00170    0.02251    0.00078
S1    4    0.343518    0.790232    0.308117    11.00000    0.08209    0.09687 =
         0.11150    0.02853    0.00834    0.01091
S2    4    0.968109    0.953040    0.660109    11.00000    0.09296    0.11235 =
         0.11449   -0.00999    0.03820   -0.03778
ZN    5    0.696338    0.656325    0.586956    11.00000    0.07194    0.05970 =
         0.07054   -0.00243    0.01879   -0.00286
H11   2    0.775778    0.397811    0.615417    11.00000    0.06680
H12   2    0.805465    0.610922    0.381842    11.00000    0.08656
H13   2    0.903681    0.433768    0.361251    11.00000    0.10931
H21   2    0.494290    0.533387    0.650775    11.00000    0.06339
H22   2    0.801586    0.590511    0.850256    11.00000    0.08990
H23   2    0.695777    0.474302    0.969177    11.00000    0.09115
HKLF    4

REM  shelxt_a.res in P2(1)/c
REM R1 =  0.0393 for    2153 Fo > 4sig(Fo)  and  0.0771 for all    3397 data
REM    198 parameters refined using      0 restraints

END

WGHT      0.0336      0.3510

REM Highest difference peak  0.326,  deepest hole -0.277,  1-sigma level  0.045
Q1    1   1.0017  0.8799  0.6978  11.00000  0.05    0.33
Q2    1   0.7231  0.6503  0.5172  11.00000  0.05    0.20
Q3    1   0.9185  0.9782  0.6976  11.00000  0.05    0.20
;
_shelx_res_checksum              49833

_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: Ethanol/water mixture'
####################################################################### 
# 
# 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_Zn2MeImz2SCN2
_database_code_depnum_ccdc_archive 'CCDC 1588817'
_audit_update_record             
;
2017-12-03 deposited with the CCDC.
2018-06-25 downloaded from the CCDC.
;
_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        dithiocianato-bis(2-methylimidazole)zinc(II)
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C10 H12 N6 S2 Zn'
_chemical_formula_weight         345.75

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'
Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_H-M_alt        'P n m a'
_space_group_name_Hall           '-P 2ac 2n'

_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+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z'
'-x-1/2, y-1/2, z-1/2'

_cell_length_a                   8.4322(3)
_cell_length_b                   12.5613(5)
_cell_length_c                   13.9647(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1479.13(10)
_cell_formula_units_Z            4
_cell_measurement_temperature    297(2)
_cell_measurement_reflns_used    1117
_cell_measurement_theta_min      4.1130
_cell_measurement_theta_max      27.3590
_exptl_crystal_description       plate
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.553
_exptl_crystal_F_000             704
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.209
_exptl_crystal_size_mid          0.143
_exptl_crystal_size_min          0.048
_exptl_absorpt_coefficient_mu    1.937
_shelx_estimated_absorpt_T_min   0.688
_shelx_estimated_absorpt_T_max   0.913
_exptl_absorpt_correction_T_min  0.82614
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_oxdiff_exptl_absorpt_empirical_full_min 0.863
_oxdiff_exptl_absorpt_empirical_full_max 1.201
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      297(2)
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Eos
_diffrn_detector_area_resol_mean 16.0604
_diffrn_reflns_number            4379
_diffrn_reflns_av_unetI/netI     0.0486
_diffrn_reflns_av_R_equivalents  0.0447
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         2.917
_diffrn_reflns_theta_max         26.998
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.971
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             1634
_reflns_number_gt                1203
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .
_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    'SHELXT (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_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)+(0.0285P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_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         1634
_refine_ls_number_parameters     98
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0603
_refine_ls_R_factor_gt           0.0368
_refine_ls_wR_factor_ref         0.0796
_refine_ls_wR_factor_gt          0.0717
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_restrained_S_all      1.064
_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
C1 C 0.5715(4) 0.4075(3) 0.6742(2) 0.0616(10) Uani 1 1 d . . . . .
H1 H 0.5086 0.3674 0.7154 0.074 Uiso 1 1 calc R U . . .
C2 C 0.6399(5) 0.4997(3) 0.6953(3) 0.0752(12) Uani 1 1 d . . . . .
H2 H 0.6331 0.5362 0.7531 0.090 Uiso 1 1 calc R U . . .
C3 C 0.7007(3) 0.4576(2) 0.5483(2) 0.0456(8) Uani 1 1 d . . . . .
C4 C 0.7713(4) 0.4640(3) 0.4526(2) 0.0642(10) Uani 1 1 d . . . . .
H4A H 0.8112 0.3953 0.4345 0.096 Uiso 1 1 calc R U . . .
H4B H 0.8568 0.5145 0.4532 0.096 Uiso 1 1 calc R U . . .
H4C H 0.6922 0.4864 0.4074 0.096 Uiso 1 1 calc R U . . .
C5 C 0.5540(5) 0.2500 0.2946(3) 0.0387(9) Uani 1 2 d S T P . .
C6 C 0.1697(6) 0.2500 0.5674(3) 0.0426(10) Uani 1 2 d S T P . .
N1 N 0.6096(3) 0.38055(19) 0.58022(15) 0.0406(6) Uani 1 1 d . . . . .
N2 N 0.7221(3) 0.5305(2) 0.6158(2) 0.0629(8) Uani 1 1 d . . . . .
H2A H 0.7781 0.5874 0.6104 0.076 Uiso 1 1 calc R U . . .
N3 N 0.5530(4) 0.2500 0.3775(3) 0.0523(9) Uani 1 2 d S T P . .
N4 N 0.2964(4) 0.2500 0.5469(3) 0.0544(10) Uani 1 2 d S T P . .
S1 S 0.55093(15) 0.2500 0.17881(8) 0.0528(3) Uani 1 2 d S T P . .
S2 S -0.01858(13) 0.2500 0.59368(9) 0.0645(4) Uani 1 2 d S T P . .
Zn Zn 0.52677(5) 0.2500 0.51654(3) 0.03764(17) Uani 1 2 d S T P . .

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
C1 0.086(3) 0.055(2) 0.0434(18) -0.0039(17) 0.0005(17) 0.005(2)
C2 0.112(3) 0.061(3) 0.052(2) -0.019(2) -0.021(2) 0.012(2)
C3 0.0450(17) 0.0317(17) 0.060(2) 0.0013(15) -0.0125(15) 0.0057(14)
C4 0.062(2) 0.053(2) 0.078(2) 0.0101(18) 0.017(2) -0.0045(18)
C5 0.041(2) 0.032(2) 0.043(2) 0.000 0.0032(19) 0.000
C6 0.055(3) 0.034(2) 0.040(2) 0.000 -0.008(2) 0.000
N1 0.0472(14) 0.0329(13) 0.0418(14) -0.0013(11) -0.0034(11) 0.0038(12)
N2 0.0741(19) 0.0385(17) 0.076(2) -0.0106(15) -0.0203(17) -0.0042(15)
N3 0.064(2) 0.050(2) 0.043(2) 0.000 -0.0006(19) 0.000
N4 0.041(2) 0.049(3) 0.073(3) 0.000 0.0042(19) 0.000
S1 0.0758(8) 0.0454(7) 0.0372(6) 0.000 0.0033(5) 0.000
S2 0.0395(6) 0.0923(11) 0.0616(8) 0.000 -0.0014(5) 0.000
Zn 0.0418(3) 0.0336(3) 0.0376(3) 0.000 0.0013(2) 0.000

_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
C1 C2 1.327(5) . ?
C1 N1 1.393(4) . ?
C2 N2 1.365(4) . ?
C3 N1 1.313(4) . ?
C3 N2 1.328(4) . ?
C3 C4 1.465(4) . ?
C5 N3 1.159(5) . ?
C5 S1 1.617(4) . ?
C6 N4 1.106(5) . ?
C6 S2 1.629(5) . ?
N1 Zn 1.992(2) . ?
N3 Zn 1.954(4) . ?
N4 Zn 1.988(4) . ?
Zn N1 1.992(2) 7_565 ?

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
C2 C1 N1 108.7(3) . . ?
C1 C2 N2 106.8(3) . . ?
N1 C3 N2 110.3(3) . . ?
N1 C3 C4 126.0(3) . . ?
N2 C3 C4 123.7(3) . . ?
N3 C5 S1 178.7(4) . . ?
N4 C6 S2 178.0(4) . . ?
C3 N1 C1 106.0(3) . . ?
C3 N1 Zn 131.3(2) . . ?
C1 N1 Zn 122.7(2) . . ?
C3 N2 C2 108.2(3) . . ?
C5 N3 Zn 173.9(3) . . ?
C6 N4 Zn 177.3(4) . . ?
N3 Zn N4 108.79(15) . . ?
N3 Zn N1 113.83(8) . 7_565 ?
N4 Zn N1 104.34(9) . 7_565 ?
N3 Zn N1 113.83(8) . . ?
N4 Zn N1 104.34(9) . . ?
N1 Zn N1 110.81(13) 7_565 . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N2 H2A S1 0.86 2.68 3.469(3) 154.0 2_665

_refine_diff_density_max         0.297
_refine_diff_density_min         -0.333
_refine_diff_density_rms         0.064

_shelx_res_file                  
;

    shelx.res created by SHELXL-2014/7


TITL shelxt_a.res in Pnma
CELL  0.71073   8.4322  12.5613  13.9647   90.000   90.000   90.000
ZERR     4.00   0.0003   0.0005   0.0005    0.000    0.000    0.000
LATT   1
SYMM  1/2 - X, - Y, 1/2 + Z
SYMM  - X, 1/2 + Y, - Z
SYMM  1/2 + X, 1/2 - Y, 1/2 - Z
SFAC  C    H    N    S    ZN
UNIT  40   48   24   8    4
MERG   2
OMIT  -3 54
SIZE  0.048 0.143 0.209
TEMP 24
REM  Crystal shape/color: plate/colourless
ACTA
EQIV $1 -x+3/2, -y+1, z+1/2
HTAB N2 S1_$1
FMAP   2
PLAN -3
L.S.  5
WGHT    0.028500
FVAR       0.35742
C1    1    0.571518    0.407466    0.674241    11.00000    0.08608    0.05535 =
         0.04339   -0.00392    0.00054    0.00481
AFIX  43
H1    2    0.508580    0.367441    0.715407    11.00000   -1.20000
AFIX   0
C2    1    0.639898    0.499668    0.695301    11.00000    0.11218    0.06140 =
         0.05216   -0.01893   -0.02071    0.01189
AFIX  43
H2    2    0.633109    0.536211    0.753075    11.00000   -1.20000
AFIX   0
C3    1    0.700725    0.457555    0.548314    11.00000    0.04501    0.03171 =
         0.06017    0.00131   -0.01247    0.00567
C4    1    0.771312    0.463967    0.452608    11.00000    0.06207    0.05281 =
         0.07781    0.01007    0.01681   -0.00450
AFIX 137
H4A   2    0.811183    0.395276    0.434483    11.00000   -1.50000
H4B   2    0.856761    0.514467    0.453200    11.00000   -1.50000
H4C   2    0.692240    0.486360    0.407436    11.00000   -1.50000
AFIX   0
C5    1    0.553954    0.250000    0.294559    10.50000    0.04077    0.03244 =
         0.04297    0.00000    0.00323    0.00000
C6    1    0.169709    0.250000    0.567422    10.50000    0.05451    0.03370 =
         0.03967    0.00000   -0.00822    0.00000
N1    3    0.609637    0.380545    0.580223    11.00000    0.04719    0.03289 =
         0.04176   -0.00126   -0.00342    0.00378
N2    3    0.722116    0.530542    0.615841    11.00000    0.07414    0.03851 =
         0.07610   -0.01056   -0.02027   -0.00422
AFIX  43
H2A   2    0.778111    0.587449    0.610444    11.00000   -1.20000
AFIX   0
N3    3    0.552950    0.250000    0.377520    10.50000    0.06409    0.05000 =
         0.04290    0.00000   -0.00064    0.00000
N4    3    0.296437    0.250000    0.546864    10.50000    0.04094    0.04932 =
         0.07299    0.00000    0.00423    0.00000
S1    4    0.550927    0.250000    0.178807    10.50000    0.07581    0.04541 =
         0.03724    0.00000    0.00325    0.00000
S2    4   -0.018576    0.250000    0.593684    10.50000    0.03951    0.09232 =
         0.06163    0.00000   -0.00135    0.00000
ZN    5    0.526769    0.250000    0.516537    10.50000    0.04177    0.03355 =
         0.03761    0.00000    0.00127    0.00000
HKLF    4

REM  shelxt_a.res in Pnma
REM R1 =  0.0368 for    1203 Fo > 4sig(Fo)  and  0.0603 for all    1634 data
REM     98 parameters refined using      0 restraints

END

WGHT      0.0310      0.0000

REM Highest difference peak  0.297,  deepest hole -0.333,  1-sigma level  0.064
Q1    1   0.5757  0.3285  0.5313  11.00000  0.05    0.30
Q2    1   0.5475  0.3190  0.5541  11.00000  0.05    0.29
Q3    1   0.4994  0.2956  0.2190  11.00000  0.05    0.26
;
_shelx_res_checksum              93057

_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: ethanol/water mixture'
####################################################################### 
# 
# 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_Cd1MeImz4SCN2
_database_code_depnum_ccdc_archive 'CCDC 1588818'
_audit_update_record             
;
2017-12-03 deposited with the CCDC.
2018-06-25 downloaded from the CCDC.
;
_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        
dithiocianato-tetraquis(1-methylimidazole)cadmium(II)
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C18 H24 Cd N10 S2'
_chemical_formula_weight         556.99

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'
Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
_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'

_cell_length_a                   8.1914(3)
_cell_length_b                   8.7859(6)
_cell_length_c                   9.4685(6)
_cell_angle_alpha                90.962(6)
_cell_angle_beta                 112.629(5)
_cell_angle_gamma                104.257(5)
_cell_volume                     604.85(7)
_cell_formula_units_Z            1
_cell_measurement_temperature    297(2)
_cell_measurement_reflns_used    2309
_cell_measurement_theta_min      4.3920
_cell_measurement_theta_max      28.2460
_exptl_crystal_description       fragment
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.529
_exptl_crystal_F_000             282
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.441
_exptl_crystal_size_mid          0.337
_exptl_crystal_size_min          0.138
_exptl_absorpt_coefficient_mu    1.101
_shelx_estimated_absorpt_T_min   0.642
_shelx_estimated_absorpt_T_max   0.863
_exptl_absorpt_correction_T_min  0.92428
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_oxdiff_exptl_absorpt_empirical_full_min 0.875
_oxdiff_exptl_absorpt_empirical_full_max 1.237
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_diffrn_ambient_temperature      297(2)
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Eos
_diffrn_detector_area_resol_mean 16.0604
_diffrn_reflns_number            4197
_diffrn_reflns_av_unetI/netI     0.0343
_diffrn_reflns_av_R_equivalents  0.0251
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         3.156
_diffrn_reflns_theta_max         26.996
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.942
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.942
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.942
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             2500
_reflns_number_gt                2416
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .
_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    'SHELXT (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_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)+(0.0341P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_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         2500
_refine_ls_number_parameters     144
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0262
_refine_ls_R_factor_gt           0.0250
_refine_ls_wR_factor_ref         0.0630
_refine_ls_wR_factor_gt          0.0622
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_restrained_S_all      1.062
_refine_ls_shift/su_max          0.026
_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_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
C1 C 0.4744(3) 0.1466(3) 0.8182(2) 0.0404(5) Uani 1 1 d . . . . .
C11 C 0.0663(3) 0.0351(3) 0.3140(3) 0.0474(5) Uani 1 1 d . . . . .
H11 H 0.0253 -0.0202 0.3823 0.057 Uiso 1 1 calc R U . . .
C12 C -0.0372(3) 0.0995(3) 0.1963(3) 0.0488(5) Uani 1 1 d . . . . .
H12 H -0.1600 0.0969 0.1681 0.059 Uiso 1 1 calc R U . . .
C13 C 0.2397(3) 0.1429(3) 0.2038(2) 0.0419(5) Uani 1 1 d . . . . .
H13 H 0.3407 0.1772 0.1785 0.050 Uiso 1 1 calc R U . . .
C14 C 0.0322(4) 0.2630(4) -0.0024(3) 0.0621(7) Uani 1 1 d . . . . .
H14A H 0.0102 0.3579 0.0287 0.093 Uiso 1 1 calc R U . . .
H14B H -0.0757 0.2022 -0.0876 0.093 Uiso 1 1 calc R U . . .
H14C H 0.1336 0.2903 -0.0332 0.093 Uiso 1 1 calc R U . . .
C21 C 0.6901(3) 0.3906(3) 0.6128(3) 0.0542(6) Uani 1 1 d . . . . .
H21 H 0.6688 0.3865 0.7025 0.065 Uiso 1 1 calc R U . . .
C22 C 0.7494(4) 0.5241(3) 0.5586(3) 0.0622(7) Uani 1 1 d . . . . .
H22 H 0.7764 0.6274 0.6028 0.075 Uiso 1 1 calc R U . . .
C23 C 0.7113(3) 0.3204(3) 0.4062(2) 0.0421(5) Uani 1 1 d . . . . .
H23 H 0.7084 0.2589 0.3239 0.051 Uiso 1 1 calc R U . . .
C24 C 0.8174(4) 0.5816(4) 0.3229(4) 0.0710(8) Uani 1 1 d . . . . .
H24A H 0.8370 0.5201 0.2491 0.107 Uiso 1 1 calc R U . . .
H24B H 0.9292 0.6615 0.3824 0.107 Uiso 1 1 calc R U . . .
H24C H 0.7223 0.6311 0.2698 0.107 Uiso 1 1 calc R U . . .
N1 N 0.4261(3) 0.0634(3) 0.7064(2) 0.0551(5) Uani 1 1 d . . . . .
N11 N 0.2406(2) 0.0626(2) 0.3191(2) 0.0425(4) Uani 1 1 d . . . . .
N12 N 0.0759(2) 0.1696(2) 0.1265(2) 0.0429(4) Uani 1 1 d . . . . .
N21 N 0.6658(2) 0.2620(2) 0.5167(2) 0.0401(4) Uani 1 1 d . . . . .
N22 N 0.7622(2) 0.4781(2) 0.4257(2) 0.0463(4) Uani 1 1 d . . . . .
S1 S 0.54310(9) 0.26909(10) 0.97385(7) 0.06204(19) Uani 1 1 d . . . . .
Cd Cd 0.5000 0.0000 0.5000 0.03573(9) Uani 1 2 d S . P . .

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
C1 0.0447(11) 0.0491(13) 0.0387(11) 0.0127(10) 0.0246(9) 0.0189(10)
C11 0.0549(13) 0.0396(13) 0.0528(13) 0.0026(10) 0.0331(11) 0.0033(10)
C12 0.0429(12) 0.0468(14) 0.0576(14) -0.0041(11) 0.0240(10) 0.0083(10)
C13 0.0408(11) 0.0483(13) 0.0406(11) 0.0085(9) 0.0202(9) 0.0125(9)
C14 0.0715(17) 0.0670(18) 0.0484(13) 0.0163(13) 0.0173(12) 0.0307(14)
C21 0.0643(15) 0.0410(14) 0.0542(14) -0.0084(11) 0.0294(12) 0.0006(11)
C22 0.0716(16) 0.0318(13) 0.0783(19) -0.0080(12) 0.0309(14) 0.0050(11)
C23 0.0463(11) 0.0346(12) 0.0364(10) 0.0020(9) 0.0130(9) 0.0014(9)
C24 0.0629(16) 0.0590(18) 0.0704(18) 0.0352(15) 0.0130(13) 0.0014(13)
N1 0.0755(14) 0.0498(13) 0.0496(11) 0.0011(10) 0.0379(10) 0.0130(10)
N11 0.0480(10) 0.0392(10) 0.0416(9) 0.0064(8) 0.0203(8) 0.0106(8)
N12 0.0441(10) 0.0451(11) 0.0384(9) 0.0027(8) 0.0149(8) 0.0135(8)
N21 0.0462(9) 0.0316(10) 0.0370(9) 0.0013(7) 0.0160(7) 0.0024(7)
N22 0.0422(9) 0.0328(10) 0.0497(11) 0.0124(8) 0.0081(8) 0.0023(7)
S1 0.0647(4) 0.0827(5) 0.0367(3) -0.0063(3) 0.0161(3) 0.0246(4)
Cd 0.04597(14) 0.02748(13) 0.03256(12) 0.00243(8) 0.01755(9) 0.00516(8)

_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
C1 N1 1.150(3) . ?
C1 S1 1.630(2) . ?
C11 C12 1.346(3) . ?
C11 N11 1.369(3) . ?
C12 N12 1.371(3) . ?
C13 N11 1.308(3) . ?
C13 N12 1.340(3) . ?
C14 N12 1.460(3) . ?
C21 C22 1.344(4) . ?
C21 N21 1.363(3) . ?
C22 N22 1.365(3) . ?
C23 N21 1.312(3) . ?
C23 N22 1.332(3) . ?
C24 N22 1.465(3) . ?
N1 Cd 2.3529(19) . ?
N11 Cd 2.3578(18) . ?
N21 Cd 2.3343(17) . ?
Cd N21 2.3343(17) 2_656 ?
Cd N1 2.3528(19) 2_656 ?
Cd N11 2.3578(18) 2_656 ?

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 C1 S1 178.3(2) . . ?
C12 C11 N11 110.5(2) . . ?
C11 C12 N12 105.7(2) . . ?
N11 C13 N12 111.99(18) . . ?
C22 C21 N21 109.9(2) . . ?
C21 C22 N22 106.4(2) . . ?
N21 C23 N22 112.1(2) . . ?
C1 N1 Cd 144.66(19) . . ?
C13 N11 C11 104.99(18) . . ?
C13 N11 Cd 125.17(14) . . ?
C11 N11 Cd 129.72(15) . . ?
C13 N12 C12 106.87(19) . . ?
C13 N12 C14 125.7(2) . . ?
C12 N12 C14 127.3(2) . . ?
C23 N21 C21 105.06(19) . . ?
C23 N21 Cd 123.75(14) . . ?
C21 N21 Cd 128.91(15) . . ?
C23 N22 C22 106.6(2) . . ?
C23 N22 C24 126.7(2) . . ?
C22 N22 C24 126.8(2) . . ?
N21 Cd N21 180.0 . 2_656 ?
N21 Cd N1 88.60(7) . 2_656 ?
N21 Cd N1 91.40(7) 2_656 2_656 ?
N21 Cd N1 91.40(7) . . ?
N21 Cd N1 88.60(7) 2_656 . ?
N1 Cd N1 180.00(9) 2_656 . ?
N21 Cd N11 87.72(6) . . ?
N21 Cd N11 92.28(6) 2_656 . ?
N1 Cd N11 88.10(7) 2_656 . ?
N1 Cd N11 91.90(7) . . ?
N21 Cd N11 92.28(6) . 2_656 ?
N21 Cd N11 87.72(6) 2_656 2_656 ?
N1 Cd N11 91.90(7) 2_656 2_656 ?
N1 Cd N11 88.10(7) . 2_656 ?
N11 Cd N11 180.0 . 2_656 ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
C13 H13 S1 0.93 3.00 3.878(2) 157.2 1_554
C24 H24C S1 0.96 2.82 3.740(3) 160.2 2_666

_refine_diff_density_max         0.256
_refine_diff_density_min         -0.614
_refine_diff_density_rms         0.070

_shelx_res_file                  
;

    shelx.res created by SHELXL-2014/7


TITL shelxt_a.res in P-1
CELL  0.71073   8.1914   8.7859   9.4685   90.962  112.629  104.257
ZERR     1.00   0.0003   0.0006   0.0006    0.006    0.005    0.005
LATT   1
SFAC  C    H    N    S    CD
UNIT  18   24   10   2    1
MERG   2
OMIT -3 54
SIZE  0.138 0.337 0.441
TEMP  24
REM   Crystal shape/color: fragment/colorless
ACTA
EQIV $1 x, y, z-1
HTAB C13 S1_$1
EQIV $2 -x+1, -y+1, -z+1
HTAB C24 S1_$2
FMAP   2
PLAN  -3
L.S.  10
WGHT    0.034100
FVAR       8.83913
C1    1    0.474447    0.146625    0.818231    11.00000    0.04468    0.04914 =
         0.03870    0.01270    0.02463    0.01889
C11   1    0.066334    0.035116    0.314014    11.00000    0.05488    0.03963 =
         0.05284    0.00265    0.03310    0.00330
AFIX  43
H11   2    0.025308   -0.020245    0.382305    11.00000   -1.20000
AFIX   0
C12   1   -0.037229    0.099461    0.196278    11.00000    0.04292    0.04677 =
         0.05758   -0.00412    0.02397    0.00826
AFIX  43
H12   2   -0.159983    0.096853    0.168147    11.00000   -1.20000
AFIX   0
C13   1    0.239654    0.142852    0.203827    11.00000    0.04077    0.04829 =
         0.04059    0.00848    0.02021    0.01250
AFIX  43
H13   2    0.340655    0.177238    0.178534    11.00000   -1.20000
AFIX   0
C14   1    0.032245    0.263033   -0.002434    11.00000    0.07155    0.06705 =
         0.04844    0.01632    0.01734    0.03068
AFIX 137
H14A  2    0.010170    0.357914    0.028712    11.00000   -1.50000
H14B  2   -0.075718    0.202230   -0.087576    11.00000   -1.50000
H14C  2    0.133596    0.290345   -0.033163    11.00000   -1.50000
AFIX   0
C21   1    0.690074    0.390585    0.612787    11.00000    0.06427    0.04104 =
         0.05422   -0.00840    0.02945    0.00062
AFIX  43
H21   2    0.668775    0.386541    0.702479    11.00000   -1.20000
AFIX   0
C22   1    0.749398    0.524123    0.558582    11.00000    0.07157    0.03176 =
         0.07829   -0.00805    0.03088    0.00505
AFIX  43
H22   2    0.776378    0.627391    0.602848    11.00000   -1.20000
AFIX   0
C23   1    0.711285    0.320374    0.406199    11.00000    0.04626    0.03460 =
         0.03643    0.00196    0.01298    0.00144
AFIX  43
H23   2    0.708355    0.258883    0.323891    11.00000   -1.20000
AFIX   0
C24   1    0.817449    0.581586    0.322868    11.00000    0.06294    0.05896 =
         0.07040    0.03517    0.01297    0.00142
AFIX 137
H24A  2    0.837022    0.520091    0.249104    11.00000   -1.50000
H24B  2    0.929226    0.661466    0.382381    11.00000   -1.50000
H24C  2    0.722324    0.631057    0.269754    11.00000   -1.50000
AFIX   0
N1    3    0.426092    0.063391    0.706401    11.00000    0.07549    0.04975 =
         0.04958    0.00115    0.03791    0.01303
N11   3    0.240562    0.062623    0.319102    11.00000    0.04801    0.03924 =
         0.04164    0.00640    0.02030    0.01059
N12   3    0.075882    0.169642    0.126457    11.00000    0.04407    0.04514 =
         0.03842    0.00270    0.01486    0.01350
N21   3    0.665772    0.261964    0.516745    11.00000    0.04624    0.03160 =
         0.03698    0.00129    0.01601    0.00237
N22   3    0.762175    0.478050    0.425656    11.00000    0.04220    0.03275 =
         0.04969    0.01243    0.00809    0.00229
S1    4    0.543095    0.269086    0.973850    11.00000    0.06466    0.08273 =
         0.03668   -0.00634    0.01606    0.02458
CD    5    0.500000    0.000000    0.500000    10.50000    0.04597    0.02748 =
         0.03256    0.00243    0.01755    0.00516
HKLF    4

REM  shelxt_a.res in P-1
REM R1 =  0.0250 for    2416 Fo > 4sig(Fo)  and  0.0262 for all    2500 data
REM    144 parameters refined using      0 restraints

END

WGHT      0.0356      0.0000

REM Highest difference peak  0.256,  deepest hole -0.614,  1-sigma level  0.070
Q1    1   0.0256  0.2161 -0.1159  11.00000  0.05    0.26
Q2    1   0.1236  0.3793  0.0314  11.00000  0.05    0.25
Q3    1   0.3831  0.1184  0.6578  11.00000  0.05    0.23
;
_shelx_res_checksum              29321

_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: Ethanol/water mixture'
####################################################################### 
# 
# 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_Cd2MeImz2SCN2
_database_code_depnum_ccdc_archive 'CCDC 1588819'
_audit_update_record             
;
2017-12-03 deposited with the CCDC.
2018-06-25 downloaded from the CCDC.
;
_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        
'bis(2-methylimidazole)di(μ-S,N-thiocyanate) cadmium(II)'
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C10 H12 Cd N6 S2'
_chemical_formula_weight         392.78
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'
Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           36
_space_group_name_H-M_alt        'C m c 21'
_space_group_name_Hall           'C 2c -2'
_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+1/2'
'x, -y, z+1/2'
'-x, y, z'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z+1/2'
'x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, z'

_cell_length_a                   13.9249(4)
_cell_length_b                   14.7811(4)
_cell_length_c                   6.9732(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1435.26(7)
_cell_formula_units_Z            4
_cell_measurement_temperature    297(2)
_cell_measurement_reflns_used    1186
_cell_measurement_theta_min      4.0130
_cell_measurement_theta_max      28.2060
_exptl_crystal_description       fragment
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.818
_exptl_crystal_F_000             776
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.377
_exptl_crystal_size_mid          0.260
_exptl_crystal_size_min          0.211
_exptl_absorpt_coefficient_mu    1.807
_shelx_estimated_absorpt_T_min   0.549
_shelx_estimated_absorpt_T_max   0.702
_exptl_absorpt_correction_T_min  0.90625
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_oxdiff_exptl_absorpt_empirical_full_min 0.913
_oxdiff_exptl_absorpt_empirical_full_max 1.074
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      297(2)
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Eos
_diffrn_detector_area_resol_mean 16.0604
_diffrn_reflns_number            1995
_diffrn_reflns_av_unetI/netI     0.0299
_diffrn_reflns_av_R_equivalents  0.0217
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_theta_min         2.926
_diffrn_reflns_theta_max         26.860
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.955
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.955
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.692
_diffrn_reflns_point_group_measured_fraction_full 0.731
_reflns_number_total             1115
_reflns_number_gt                1083
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.334
_reflns_Friedel_fraction_max     0.379
_reflns_Friedel_fraction_full    0.412
_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    'SHELXT (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_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)+(0.0216P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_extinction_coef       0.0068(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_abs_structure_details 
;
Flack x determined using 269 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.01(3)
_chemical_absolute_configuration ad
# start Validation Reply Form
_vrf_PLAT915_Cd2MeImz2SCN2       
;
PROBLEM: No Flack x Check Done: Low Friedel Pair Coverage         38 %     
RESPONSE: The absolute structure determination is reliable, as it 
involves an acceptable number of Friedel pairs (269) and a strong
anomalous dispersion scatterer (cadmium) to produce a small 
Flack's x-value (-0.01) and a reasonable standard deviation (0.03). 
;
# end Validation Reply Form
_refine_ls_number_reflns         1115
_refine_ls_number_parameters     99
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0205
_refine_ls_R_factor_gt           0.0194
_refine_ls_wR_factor_ref         0.0441
_refine_ls_wR_factor_gt          0.0436
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_restrained_S_all      1.031
_refine_ls_shift/su_max          0.002
_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
C1 C 0.5000 0.5808(3) 0.5201(7) 0.0289(13) Uani 1 2 d S T P . .
C2 C 0.5000 0.1354(3) 0.3795(10) 0.0355(14) Uani 1 2 d S T P . .
C3 C 0.2731(2) 0.38677(19) 0.5738(9) 0.0292(7) Uani 1 1 d . . . . .
C4 C 0.2127(3) 0.3314(3) 0.3086(7) 0.0415(10) Uani 1 1 d . . . . .
H4 H 0.1698 0.3148 0.2127 0.050 Uiso 1 1 calc R U . . .
C5 C 0.3084(3) 0.3177(3) 0.3107(6) 0.0380(10) Uani 1 1 d . . . . .
H5 H 0.3435 0.2894 0.2145 0.046 Uiso 1 1 calc R U . . .
C6 C 0.2761(3) 0.4308(3) 0.7643(7) 0.0433(10) Uani 1 1 d . . . . .
H6A H 0.2879 0.3860 0.8612 0.065 Uiso 1 1 calc R U . . .
H6B H 0.2157 0.4599 0.7889 0.065 Uiso 1 1 calc R U . . .
H6C H 0.3265 0.4750 0.7663 0.065 Uiso 1 1 calc R U . . .
N1 N 0.5000 0.5093(3) 0.5799(10) 0.0397(10) Uani 1 2 d S T P . .
N2 N 0.5000 0.1952(3) 0.4821(9) 0.0493(15) Uani 1 2 d S T P . .
N3 N 0.3459(2) 0.35245(16) 0.4776(5) 0.0299(7) Uani 1 1 d . . . . .
N4 N 0.1917(2) 0.3746(2) 0.4766(5) 0.0355(8) Uani 1 1 d . . . . .
H4A H 0.1355 0.3913 0.5135 0.043 Uiso 1 1 calc R U . . .
S1 S 0.5000 0.68680(8) 0.4368(2) 0.0330(3) Uani 1 2 d S T P . .
S2 S 0.5000 0.04842(10) 0.2316(3) 0.0436(4) Uani 1 2 d S T P . .
Cd Cd 0.5000 0.34854(2) 0.57070(2) 0.02952(14) Uani 1 2 d S T P . .

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
C1 0.026(2) 0.034(2) 0.027(3) -0.002(2) 0.000 0.000
C2 0.022(3) 0.032(2) 0.053(4) 0.005(3) 0.000 0.000
C3 0.0278(15) 0.0250(13) 0.0350(16) 0.003(3) 0.001(3) -0.0025(12)
C4 0.038(2) 0.050(2) 0.036(3) -0.005(2) -0.0043(19) -0.012(2)
C5 0.041(2) 0.0419(19) 0.031(2) -0.012(2) 0.0014(17) -0.0083(19)
C6 0.040(2) 0.049(2) 0.040(2) -0.016(2) 0.004(2) 0.005(2)
N1 0.042(2) 0.032(2) 0.046(2) 0.006(4) 0.000 0.000
N2 0.051(3) 0.037(2) 0.059(4) -0.015(3) 0.000 0.000
N3 0.0272(17) 0.0296(15) 0.0328(17) -0.0042(14) 0.0006(15) 0.0004(11)
N4 0.0247(17) 0.0405(15) 0.0412(19) 0.0031(16) 0.0021(15) -0.0027(14)
S1 0.0406(8) 0.0278(6) 0.0305(7) -0.0002(6) 0.000 0.000
S2 0.0348(7) 0.0436(8) 0.0523(10) -0.0146(8) 0.000 0.000
Cd 0.02544(19) 0.03086(18) 0.0323(2) -0.0027(2) 0.000 0.000

_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
C1 N1 1.136(6) . ?
C1 S1 1.670(5) . ?
C2 N2 1.137(8) . ?
C2 S2 1.648(6) . ?
C3 N3 1.317(5) . ?
C3 N4 1.332(5) . ?
C3 C6 1.480(8) . ?
C4 C5 1.349(6) . ?
C4 N4 1.366(6) . ?
C5 N3 1.375(5) . ?
N1 Cd 2.378(4) . ?
N2 Cd 2.349(5) . ?
N3 Cd 2.242(3) . ?
S1 Cd 2.6054(16) 2_664 ?
Cd N3 2.242(3) 4_655 ?
Cd S1 2.6054(16) 2_665 ?

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 C1 S1 178.8(5) . . ?
N2 C2 S2 179.7(6) . . ?
N3 C3 N4 110.1(5) . . ?
N3 C3 C6 127.2(4) . . ?
N4 C3 C6 122.7(4) . . ?
C5 C4 N4 105.8(4) . . ?
C4 C5 N3 109.2(4) . . ?
C1 N1 Cd 156.9(6) . . ?
C2 N2 Cd 156.3(5) . . ?
C3 N3 C5 106.4(4) . . ?
C3 N3 Cd 126.8(3) . . ?
C5 N3 Cd 126.8(3) . . ?
C3 N4 C4 108.5(4) . . ?
C1 S1 Cd 98.79(18) . 2_664 ?
N3 Cd N3 146.21(17) . 4_655 ?
N3 Cd N2 87.06(8) . . ?
N3 Cd N2 87.06(8) 4_655 . ?
N3 Cd N1 88.97(8) . . ?
N3 Cd N1 88.97(8) 4_655 . ?
N2 Cd N1 166.3(2) . . ?
N3 Cd S1 106.78(8) . 2_665 ?
N3 Cd S1 106.78(8) 4_655 2_665 ?
N2 Cd S1 93.69(16) . 2_665 ?
N1 Cd S1 100.02(17) . 2_665 ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
C5 H5 S1 0.93 2.94 3.731(4) 144.2 2_664
N4 H4A S2 0.86 2.58 3.404(4) 160.0 6

_refine_diff_density_max         0.513
_refine_diff_density_min         -0.380
_refine_diff_density_rms         0.074

_shelx_res_file                  
;

    shelx.res created by SHELXL-2014/7


TITL shelxt_b.res in Cmc2(1) (#36)
CELL  0.71073  13.9249  14.7811   6.9732   90.000   90.000   90.000
ZERR     4.00   0.0004   0.0004   0.0002    0.000    0.000    0.000
LATT  -7
SYMM  - X, - Y, 1/2 + Z
SYMM    X, - Y, 1/2 + Z
SYMM  - X,   Y,   Z
SFAC  C    H    N    S    CD
UNIT  40   48   24   8    4
MERG   2
OMIT  -3 54
SIZE  0.211 0.260 0.377
TEMP  24
REM   Crystal shape/color: fragment/colorless
EQIV $2 -x+1, -y+1, z-1/2
HTAB C5 S1_$2
EQIV $3 -x+1/2, -y+1/2, z+1/2
HTAB N4 S2_$3
EQIV  $1 1-x, y, z
MPLA  4 N1 N2 N3 N3_$1 CD
ACTA
FMAP   2
PLAN -3
L.S.  5
WGHT    0.021600
EXTI    0.006763
FVAR       3.54770
C1    1    0.500000    0.580839    0.520068    10.50000    0.02557    0.03422 =
         0.02692   -0.00239    0.00000    0.00000
C2    1    0.500000    0.135393    0.379484    10.50000    0.02177    0.03205 =
         0.05279    0.00514    0.00000    0.00000
C3    1    0.273092    0.386766    0.573799    11.00000    0.02782    0.02495 =
         0.03498    0.00311    0.00082   -0.00248
C4    1    0.212660    0.331390    0.308608    11.00000    0.03823    0.05002 =
         0.03633   -0.00547   -0.00435   -0.01180
AFIX  43
H4    2    0.169751    0.314790    0.212657    11.00000   -1.20000
AFIX   0
C5    1    0.308422    0.317741    0.310698    11.00000    0.04098    0.04194 =
         0.03111   -0.01229    0.00141   -0.00830
AFIX  43
H5    2    0.343522    0.289356    0.214500    11.00000   -1.20000
AFIX   0
C6    1    0.276062    0.430804    0.764272    11.00000    0.04037    0.04907 =
         0.04046   -0.01626    0.00360    0.00536
AFIX 137
H6A   2    0.287894    0.386033    0.861168    11.00000   -1.50000
H6B   2    0.215683    0.459916    0.788909    11.00000   -1.50000
H6C   2    0.326538    0.475032    0.766312    11.00000   -1.50000
AFIX   0
N1    3    0.500000    0.509339    0.579880    10.50000    0.04150    0.03174 =
         0.04585    0.00562    0.00000    0.00000
N2    3    0.500000    0.195200    0.482080    10.50000    0.05097    0.03746 =
         0.05941   -0.01483    0.00000    0.00000
N3    3    0.345925    0.352450    0.477622    11.00000    0.02721    0.02958 =
         0.03284   -0.00421    0.00062    0.00038
N4    3    0.191746    0.374648    0.476618    11.00000    0.02473    0.04046 =
         0.04123    0.00315    0.00209   -0.00266
AFIX  43
H4A   2    0.135507    0.391265    0.513457    11.00000   -1.20000
AFIX   0
S1    4    0.500000    0.686796    0.436753    10.50000    0.04064    0.02778 =
         0.03051   -0.00023    0.00000    0.00000
S2    4    0.500000    0.048424    0.231642    10.50000    0.03484    0.04359 =
         0.05231   -0.01458    0.00000    0.00000
CD    5    0.500000    0.348538    0.570704    10.50000    0.02544    0.03086 =
         0.03227   -0.00269    0.00000    0.00000
HKLF    4

REM  shelxt_b.res in Cmc2(1) (#36)
REM R1 =  0.0194 for    1083 Fo > 4sig(Fo)  and  0.0205 for all    1115 data
REM     99 parameters refined using      1 restraints

END

WGHT      0.0213      0.0000

REM Highest difference peak  0.513,  deepest hole -0.380,  1-sigma level  0.074
Q1    1   0.5000  0.3497  0.4415  10.50000  0.05    0.51
Q2    1   0.5000  0.6497  0.1998  10.50000  0.05    0.47
Q3    1   0.3955  0.3458  0.6154  11.00000  0.05    0.33
;
_shelx_res_checksum              27166

_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: Water'
