# Electronic Supplementary Material (ESI) for Journal of Materials Chemistry C.
# This journal is © The Royal Society of Chemistry 2014

####################################################################### 
# 
# 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/. 
# 
# Audit and citation data items have may 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_kappa-(ET)2Cu[N(CN)2]Br-100K
_database_code_depnum_ccdc_archive 'CCDC 1016180'
_audit_update_record             
;
2014-07-26 deposited with the CCDC.
2014-11-27 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            (ET)2Cu[N(CN)2]Br
_chemical_formula_moiety         '2(C10 H8 S8), (C2 Br1 Cu1 N3)'
_chemical_formula_sum            'C22 H16 Br1 Cu1 N3 S16'
_chemical_formula_weight         978.90

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'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   'Pnma '
_symmetry_space_group_name_Hall  '-P 2ac 2n'

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

_cell_length_a                   12.8965(12)
_cell_length_b                   29.651(3)
_cell_length_c                   8.4826(8)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     3243.7(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9908
_cell_measurement_theta_min      2.75
_cell_measurement_theta_max      28.08

_exptl_crystal_description       'rhombic plate'
_exptl_crystal_colour            black
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.03
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.004
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1956
_exptl_absorpt_coefficient_mu    2.961
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.4153
_exptl_absorpt_correction_T_max  0.9164
_exptl_absorpt_process_details   
;
APEX2 Software
;
_exptl_special_details           
; 
 kappa polymorph
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEXII CCD area detector'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean 8.333
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            16668
_diffrn_reflns_av_R_equivalents  0.0224
_diffrn_reflns_av_sigmaI/netI    0.0194
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_theta_min         1.37
_diffrn_reflns_theta_max         27.50
_reflns_number_total             3744
_reflns_number_gt                3549
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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)+(0.0173P)²+22.9659P] 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         3744
_refine_ls_number_parameters     214
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0437
_refine_ls_R_factor_gt           0.0418
_refine_ls_wR_factor_ref         0.0984
_refine_ls_wR_factor_gt          0.0975
_refine_ls_goodness_of_fit_ref   1.179
_refine_ls_restrained_S_all      1.179
_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
C1 C 0.6411(3) -0.01832(12) 0.3606(4) 0.0125(7) Uani 1 1 d . . .
C2 C 0.5779(3) 0.01883(13) 0.3592(5) 0.0130(7) Uani 1 1 d . . .
C3 C 0.7832(3) -0.07791(13) 0.4082(5) 0.0141(7) Uani 1 1 d . . .
C4 C 0.7235(3) -0.09508(12) 0.2918(4) 0.0130(7) Uani 1 1 d . . .
C5 C 0.4996(3) 0.09818(13) 0.3878(5) 0.0147(8) Uani 1 1 d . A .
C6 C 0.4430(3) 0.07807(12) 0.2754(5) 0.0141(7) Uani 1 1 d . A .
C7 C 0.9171(3) -0.14981(15) 0.3760(5) 0.0213(9) Uani 1 1 d . . .
H7A H 0.9534 -0.1395 0.2783 0.026 Uiso 1 1 calc R . .
H7B H 0.9652 -0.1705 0.4335 0.026 Uiso 1 1 calc R . .
C8 C 0.8213(3) -0.17613(13) 0.3285(5) 0.0194(8) Uani 1 1 d . . .
H8A H 0.7806 -0.1835 0.4255 0.023 Uiso 1 1 calc R . .
H8B H 0.8434 -0.2052 0.2793 0.023 Uiso 1 1 calc R . .
C9A C 0.4118(4) 0.17897(15) 0.2999(6) 0.0190(13) Uani 0.878(12) 1 d P A 1
H9A H 0.3901 0.2098 0.3340 0.023 Uiso 0.878(12) 1 calc PR A 1
H9B H 0.4554 0.1824 0.2031 0.023 Uiso 0.878(12) 1 calc PR A 1
C10A C 0.3159(4) 0.15227(15) 0.2579(6) 0.0192(12) Uani 0.878(12) 1 d P A 1
H10A H 0.2706 0.1711 0.1886 0.023 Uiso 0.878(12) 1 calc PR A 1
H10B H 0.2764 0.1456 0.3566 0.023 Uiso 0.878(12) 1 calc PR A 1
C9B C 0.385(3) 0.1730(12) 0.392(5) 0.017(9) Uiso 0.122(12) 1 d P A 2
H9C H 0.3261 0.1583 0.4501 0.021 Uiso 0.122(12) 1 calc PR A 2
H9D H 0.3813 0.2061 0.4133 0.021 Uiso 0.122(12) 1 calc PR A 2
C10B C 0.371(3) 0.1652(11) 0.221(4) 0.012(8) Uiso 0.122(12) 1 d P A 2
H10C H 0.4343 0.1759 0.1646 0.014 Uiso 0.122(12) 1 calc PR A 2
H10D H 0.3112 0.1841 0.1831 0.014 Uiso 0.122(12) 1 calc PR A 2
S1 S 0.74739(7) -0.02501(3) 0.48431(11) 0.01420(19) Uani 1 1 d . . .
S2 S 0.61684(7) -0.06304(3) 0.23254(11) 0.01464(19) Uani 1 1 d . . .
S3 S 0.59656(7) 0.06576(3) 0.47911(11) 0.01458(19) Uani 1 1 d . . .
S4 S 0.47142(8) 0.02157(3) 0.23303(12) 0.01452(19) Uani 1 1 d . . .
S5 S 0.89219(8) -0.10130(4) 0.49882(13) 0.0212(2) Uani 1 1 d . . .
S6 S 0.73823(8) -0.14636(3) 0.19205(12) 0.0168(2) Uani 1 1 d . . .
S7 S 0.49169(9) 0.15366(3) 0.45685(13) 0.0227(2) Uani 1 1 d . . .
S8 S 0.34368(8) 0.10031(4) 0.15946(13) 0.0197(2) Uani 1 1 d . . .
C11 C 0.8430(5) 0.2500 0.5980(7) 0.0165(11) Uani 1 2 d S . .
C12 C 0.9709(4) 0.2500 0.7899(7) 0.0173(12) Uani 1 2 d S . .
N1 N 0.7616(4) 0.2500 0.5415(6) 0.0210(10) Uani 1 2 d S . .
N2 N 0.9391(4) 0.2500 0.6426(6) 0.0249(12) Uani 1 2 d S . .
N3 N 1.0118(4) 0.2500 0.9087(6) 0.0192(10) Uani 1 2 d S . .
Cu1 Cu 0.62496(6) 0.2500 0.43823(8) 0.01772(16) Uani 1 2 d S . .
Br1 Br 0.63894(5) 0.2500 0.16373(7) 0.02085(14) Uani 1 2 d S . .


_geom_special_details            
; 
 The positional parameters of the hydrogen atoms were calculated under a 
 fixed C-H bond length of 1.00 A with sp2 configuration of the 
 bonding carbon atoms. In the refinement procedures, isotropic temperature
 factors with the magnitude of 1.2 fold to those of the equivalent
 temperature factors of the bonding carbon atoms were applied for hydrogen
 atoms.

 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 1.371(5) . ?
C1 S1 1.737(4) . ?
C1 S2 1.743(4) . ?
C2 S3 1.740(4) . ?
C2 S4 1.743(4) . ?
C3 C4 1.352(5) . ?
C3 S5 1.746(4) . ?
C3 S1 1.758(4) . ?
C4 S2 1.745(4) . ?
C4 S6 1.750(4) . ?
C5 C6 1.340(6) . ?
C5 S7 1.749(4) . ?
C5 S3 1.758(4) . ?
C6 S8 1.744(4) . ?
C6 S4 1.752(4) . ?
C7 C8 1.515(6) . ?
C7 S5 1.805(4) . ?
C7 H7A 1.0000 . ?
C7 H7B 1.0000 . ?
C8 S6 1.808(4) . ?
C8 H8A 1.0000 . ?
C8 H8B 1.0000 . ?
C9A C10A 1.510(7) . ?
C9A S7 1.843(5) . ?
C9A H9A 1.0000 . ?
C9A H9B 1.0000 . ?
C10A S8 1.789(5) . ?
C10A H10A 1.0000 . ?
C10A H10B 1.0000 . ?
C9B C10B 1.48(5) . ?
C9B S7 1.59(3) . ?
C9B H9C 1.0000 . ?
C9B H9D 1.0000 . ?
C10B S8 2.02(3) . ?
C10B H10C 1.0000 . ?
C10B H10D 1.0000 . ?
C11 N1 1.154(8) . ?
C11 N2 1.295(8) . ?
C12 N3 1.137(8) . ?
C12 N2 1.315(8) . ?
N1 Cu1 1.967(5) . ?
N3 Cu1 1.954(5) 6_657 ?
Cu1 N3 1.954(5) 6_557 ?
Cu1 Br1 2.3354(9) . ?

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 S1 124.5(3) . . ?
C2 C1 S2 119.9(3) . . ?
S1 C1 S2 115.6(2) . . ?
C1 C2 S3 123.7(3) . . ?
C1 C2 S4 120.8(3) . . ?
S3 C2 S4 115.5(2) . . ?
C4 C3 S5 129.1(3) . . ?
C4 C3 S1 117.1(3) . . ?
S5 C3 S1 113.8(2) . . ?
C3 C4 S2 117.0(3) . . ?
C3 C4 S6 128.2(3) . . ?
S2 C4 S6 114.8(2) . . ?
C6 C5 S7 128.7(3) . . ?
C6 C5 S3 117.2(3) . . ?
S7 C5 S3 114.1(2) . . ?
C5 C6 S8 129.3(3) . . ?
C5 C6 S4 117.2(3) . . ?
S8 C6 S4 113.5(2) . . ?
C8 C7 S5 114.8(3) . . ?
C8 C7 H7A 108.6 . . ?
S5 C7 H7A 108.6 . . ?
C8 C7 H7B 108.6 . . ?
S5 C7 H7B 108.6 . . ?
H7A C7 H7B 107.6 . . ?
C7 C8 S6 113.7(3) . . ?
C7 C8 H8A 108.8 . . ?
S6 C8 H8A 108.8 . . ?
C7 C8 H8B 108.8 . . ?
S6 C8 H8B 108.8 . . ?
H8A C8 H8B 107.7 . . ?
C10A C9A S7 114.5(3) . . ?
C10A C9A H9A 108.6 . . ?
S7 C9A H9A 108.6 . . ?
C10A C9A H9B 108.6 . . ?
S7 C9A H9B 108.6 . . ?
H9A C9A H9B 107.6 . . ?
C9A C10A S8 113.4(3) . . ?
C9A C10A H10A 108.9 . . ?
S8 C10A H10A 108.9 . . ?
C9A C10A H10B 108.9 . . ?
S8 C10A H10B 108.9 . . ?
H10A C10A H10B 107.7 . . ?
C10B C9B S7 113(3) . . ?
C10B C9B H9C 109.0 . . ?
S7 C9B H9C 109.0 . . ?
C10B C9B H9D 109.0 . . ?
S7 C9B H9D 109.0 . . ?
H9C C9B H9D 107.8 . . ?
C9B C10B S8 115(2) . . ?
C9B C10B H10C 108.6 . . ?
S8 C10B H10C 108.6 . . ?
C9B C10B H10D 108.6 . . ?
S8 C10B H10D 108.6 . . ?
H10C C10B H10D 107.5 . . ?
C1 S1 C3 95.00(18) . . ?
C1 S2 C4 95.33(18) . . ?
C2 S3 C5 94.66(19) . . ?
C2 S4 C6 94.79(18) . . ?
C3 S5 C7 101.87(19) . . ?
C4 S6 C8 100.32(19) . . ?
C9B S7 C5 105.8(12) . . ?
C9B S7 C9A 28.3(14) . . ?
C5 S7 C9A 100.0(2) . . ?
C6 S8 C10A 102.1(2) . . ?
C6 S8 C10B 95.1(9) . . ?
C10A S8 C10B 25.2(10) . . ?
N1 C11 N2 172.4(6) . . ?
N3 C12 N2 170.6(6) . . ?
C11 N1 Cu1 178.1(5) . . ?
C11 N2 C12 125.1(5) . . ?
C12 N3 Cu1 159.3(5) . 6_657 ?
N3 Cu1 N1 111.9(2) 6_557 . ?
N3 Cu1 Br1 136.08(16) 6_557 . ?
N1 Cu1 Br1 112.01(16) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
S1 C1 C2 S3 1.5(5) . . . . ?
S2 C1 C2 S3 -178.7(2) . . . . ?
S1 C1 C2 S4 -178.6(2) . . . . ?
S2 C1 C2 S4 1.2(5) . . . . ?
S5 C3 C4 S2 178.1(2) . . . . ?
S1 C3 C4 S2 -0.8(4) . . . . ?
S5 C3 C4 S6 -1.2(6) . . . . ?
S1 C3 C4 S6 179.9(2) . . . . ?
S7 C5 C6 S8 0.6(6) . . . . ?
S3 C5 C6 S8 -178.5(2) . . . . ?
S7 C5 C6 S4 179.6(2) . . . . ?
S3 C5 C6 S4 0.4(4) . . . . ?
S5 C7 C8 S6 69.4(4) . . . . ?
S7 C9A C10A S8 -69.7(4) . . . . ?
S7 C9B C10B S8 71(3) . . . . ?
C2 C1 S1 C3 -178.6(4) . . . . ?
S2 C1 S1 C3 1.6(3) . . . . ?
C4 C3 S1 C1 -0.5(3) . . . . ?
S5 C3 S1 C1 -179.6(2) . . . . ?
C2 C1 S2 C4 178.2(3) . . . . ?
S1 C1 S2 C4 -2.0(3) . . . . ?
C3 C4 S2 C1 1.7(3) . . . . ?
S6 C4 S2 C1 -179.0(2) . . . . ?
C1 C2 S3 C5 172.4(4) . . . . ?
S4 C2 S3 C5 -7.5(3) . . . . ?
C6 C5 S3 C2 4.2(3) . . . . ?
S7 C5 S3 C2 -175.1(2) . . . . ?
C1 C2 S4 C6 -172.3(3) . . . . ?
S3 C2 S4 C6 7.6(3) . . . . ?
C5 C6 S4 C2 -4.8(3) . . . . ?
S8 C6 S4 C2 174.3(2) . . . . ?
C4 C3 S5 C7 8.9(4) . . . . ?
S1 C3 S5 C7 -172.1(2) . . . . ?
C8 C7 S5 C3 -42.5(4) . . . . ?
C3 C4 S6 C8 18.7(4) . . . . ?
S2 C4 S6 C8 -160.5(2) . . . . ?
C7 C8 S6 C4 -51.6(3) . . . . ?
C10B C9B S7 C5 -50(3) . . . . ?
C10B C9B S7 C9A 32(2) . . . . ?
C6 C5 S7 C9B 14.2(15) . . . . ?
S3 C5 S7 C9B -166.7(15) . . . . ?
C6 C5 S7 C9A -14.3(4) . . . . ?
S3 C5 S7 C9A 164.9(2) . . . . ?
C10A C9A S7 C9B -57(3) . . . . ?
C10A C9A S7 C5 48.3(4) . . . . ?
C5 C6 S8 C10A -12.8(4) . . . . ?
S4 C6 S8 C10A 168.2(2) . . . . ?
C5 C6 S8 C10B 11.7(11) . . . . ?
S4 C6 S8 C10B -167.2(10) . . . . ?
C9A C10A S8 C6 46.4(4) . . . . ?
C9A C10A S8 C10B -30(2) . . . . ?
C9B C10B S8 C6 -47(3) . . . . ?
C9B C10B S8 C10A 61(3) . . . . ?
N2 C11 N1 Cu1 0.00(3) . . . . ?
N1 C11 N2 C12 180.000(7) . . . . ?
N3 C12 N2 C11 180.000(8) . . . . ?
N2 C12 N3 Cu1 -0.003(9) . . . 6_657 ?
C11 N1 Cu1 N3 180.00(2) . . . 6_557 ?
C11 N1 Cu1 Br1 0.00(2) . . . . ?

_diffrn_measured_fraction_theta_max 0.988
_diffrn_reflns_theta_full        27.50
_diffrn_measured_fraction_theta_full 0.988
_refine_diff_density_max         1.629
_refine_diff_density_min         -0.573
_refine_diff_density_rms         0.133

_exptl_crystal_recrystallization_method electrocrystallization
_exptl_crystal_preparation       'Magnetic properties, electronic property'

####################################################################### 
# 
# 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/. 
# 
# Audit and citation data items have may 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_kappa-(ET)2Cu[N(CN)2]Br-150K
_database_code_depnum_ccdc_archive 'CCDC 1016181'
_audit_update_record             
;
2014-07-26 deposited with the CCDC.
2014-11-27 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            (ET)2Cu[N(CN)2]Br
_chemical_formula_moiety         '2(C10 H8 S8), (C2 Br1 Cu1 N3)'
_chemical_formula_sum            'C22 H16 Br1 Cu1 N3 S16'
_chemical_formula_weight         978.90

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'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   'Pnma '
_symmetry_space_group_name_Hall  '-P 2ac 2n'

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

_cell_length_a                   12.8991(12)
_cell_length_b                   29.754(3)
_cell_length_c                   8.5025(8)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     3263.3(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    9928
_cell_measurement_theta_min      2.49
_cell_measurement_theta_max      28.01

_exptl_crystal_description       'rhombic plate'
_exptl_crystal_colour            black
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.03
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.992
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1956
_exptl_absorpt_coefficient_mu    2.943
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.4171
_exptl_absorpt_correction_T_max  0.9169
_exptl_absorpt_process_details   
;
APEX2 Software
;
_exptl_special_details           
; 
 kappa polymorph
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEXII CCD area detector'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean 8.333
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            16763
_diffrn_reflns_av_R_equivalents  0.0233
_diffrn_reflns_av_sigmaI/netI    0.0200
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_theta_min         1.37
_diffrn_reflns_theta_max         27.50
_reflns_number_total             3761
_reflns_number_gt                3490
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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)+(0.0224P)²+19.1784P] 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         3761
_refine_ls_number_parameters     214
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0458
_refine_ls_R_factor_gt           0.0427
_refine_ls_wR_factor_ref         0.1034
_refine_ls_wR_factor_gt          0.1021
_refine_ls_goodness_of_fit_ref   1.174
_refine_ls_restrained_S_all      1.174
_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
C1 C 0.6414(3) -0.01828(12) 0.3604(5) 0.0169(7) Uani 1 1 d . . .
C2 C 0.5784(3) 0.01887(12) 0.3592(5) 0.0174(7) Uani 1 1 d . . .
C3 C 0.7817(3) -0.07818(13) 0.4092(5) 0.0194(8) Uani 1 1 d . . .
C4 C 0.7224(3) -0.09506(12) 0.2927(4) 0.0174(7) Uani 1 1 d . . .
C5 C 0.5013(3) 0.09810(13) 0.3880(5) 0.0191(8) Uani 1 1 d . A .
C6 C 0.4443(3) 0.07831(13) 0.2762(5) 0.0182(7) Uani 1 1 d . A .
C7 C 0.9153(3) -0.14954(15) 0.3761(5) 0.0281(10) Uani 1 1 d . . .
H7A H 0.9515 -0.1388 0.2790 0.034 Uiso 1 1 calc R . .
H7B H 0.9637 -0.1702 0.4325 0.034 Uiso 1 1 calc R . .
C8 C 0.8205(4) -0.17589(14) 0.3275(5) 0.0268(9) Uani 1 1 d . . .
H8A H 0.7801 -0.1839 0.4239 0.032 Uiso 1 1 calc R . .
H8B H 0.8433 -0.2046 0.2768 0.032 Uiso 1 1 calc R . .
C9A C 0.4140(5) 0.17860(17) 0.2992(7) 0.0273(15) Uani 0.825(12) 1 d P A 1
H9A H 0.3927 0.2095 0.3329 0.033 Uiso 0.825(12) 1 calc PR A 1
H9B H 0.4577 0.1819 0.2027 0.033 Uiso 0.825(12) 1 calc PR A 1
C10A C 0.3183(5) 0.15251(17) 0.2571(7) 0.0266(14) Uani 0.825(12) 1 d P A 1
H10A H 0.2739 0.1714 0.1868 0.032 Uiso 0.825(12) 1 calc PR A 1
H10B H 0.2780 0.1463 0.3552 0.032 Uiso 0.825(12) 1 calc PR A 1
C9B C 0.3857(18) 0.1727(8) 0.392(3) 0.019(6) Uiso 0.175(12) 1 d P A 2
H9C H 0.3275 0.1577 0.4489 0.023 Uiso 0.175(12) 1 calc PR A 2
H9D H 0.3818 0.2056 0.4145 0.023 Uiso 0.175(12) 1 calc PR A 2
C10B C 0.3723(18) 0.1654(7) 0.218(3) 0.014(5) Uiso 0.175(12) 1 d P A 2
H10C H 0.4364 0.1757 0.1625 0.017 Uiso 0.175(12) 1 calc PR A 2
H10D H 0.3132 0.1842 0.1800 0.017 Uiso 0.175(12) 1 calc PR A 2
S1 S 0.74697(7) -0.02528(3) 0.48426(12) 0.0194(2) Uani 1 1 d . . .
S2 S 0.61681(8) -0.06275(3) 0.23194(12) 0.0198(2) Uani 1 1 d . . .
S3 S 0.59773(8) 0.06547(3) 0.47895(12) 0.0197(2) Uani 1 1 d . . .
S4 S 0.47211(8) 0.02202(3) 0.23292(12) 0.0198(2) Uani 1 1 d . . .
S5 S 0.89005(9) -0.10185(4) 0.50013(14) 0.0301(3) Uani 1 1 d . . .
S6 S 0.73651(8) -0.14625(3) 0.19340(12) 0.0234(2) Uani 1 1 d . . .
S7 S 0.49450(10) 0.15339(3) 0.45716(13) 0.0311(3) Uani 1 1 d . . .
S8 S 0.34513(9) 0.10076(4) 0.16114(13) 0.0273(2) Uani 1 1 d . . .
C11 C 0.8445(5) 0.2500 0.5997(7) 0.0223(12) Uani 1 2 d S . .
C12 C 0.9724(4) 0.2500 0.7903(8) 0.0226(12) Uani 1 2 d S . .
N1 N 0.7635(4) 0.2500 0.5427(6) 0.0284(11) Uani 1 2 d S . .
N2 N 0.9404(4) 0.2500 0.6439(7) 0.0353(13) Uani 1 2 d S . .
N3 N 1.0140(4) 0.2500 0.9085(6) 0.0248(11) Uani 1 2 d S . .
Cu1 Cu 0.62733(6) 0.2500 0.43860(9) 0.02440(17) Uani 1 2 d S . .
Br1 Br 0.64027(6) 0.2500 0.16490(7) 0.02981(16) Uani 1 2 d S . .


_geom_special_details            
; 
 The positional parameters of the hydrogen atoms were calculated under a 
 fixed C-H bond length of 1.00 A with sp2 configuration of the 
 bonding carbon atoms. In the refinement procedures, isotropic temperature
 factors with the magnitude of 1.2 fold to those of the equivalent
 temperature factors of the bonding carbon atoms were applied for hydrogen
 atoms.

 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 1.372(5) . ?
C1 S1 1.734(4) . ?
C1 S2 1.745(4) . ?
C2 S3 1.738(4) . ?
C2 S4 1.744(4) . ?
C3 C4 1.349(5) . ?
C3 S5 1.745(4) . ?
C3 S1 1.757(4) . ?
C4 S2 1.745(4) . ?
C4 S6 1.751(4) . ?
C5 C6 1.338(6) . ?
C5 S7 1.750(4) . ?
C5 S3 1.757(4) . ?
C6 S8 1.743(4) . ?
C6 S4 1.752(4) . ?
C7 C8 1.511(6) . ?
C7 S5 1.798(4) . ?
C7 H7A 1.0000 . ?
C7 H7B 1.0000 . ?
C8 S6 1.803(4) . ?
C8 H8A 1.0000 . ?
C8 H8B 1.0000 . ?
C9A C10A 1.501(8) . ?
C9A S7 1.856(6) . ?
C9A H9A 1.0000 . ?
C9A H9B 1.0000 . ?
C10A S8 1.776(5) . ?
C10A H10A 1.0000 . ?
C10A H10B 1.0000 . ?
C9B C10B 1.50(3) . ?
C9B S7 1.61(2) . ?
C9B H9C 1.0000 . ?
C9B H9D 1.0000 . ?
C10B S8 2.01(2) . ?
C10B H10C 1.0000 . ?
C10B H10D 1.0000 . ?
C11 N1 1.151(8) . ?
C11 N2 1.294(8) . ?
C12 N3 1.139(8) . ?
C12 N2 1.311(9) . ?
N1 Cu1 1.967(5) . ?
N3 Cu1 1.956(5) 6_657 ?
Cu1 N3 1.956(5) 6_557 ?
Cu1 Br1 2.3332(10) . ?

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 S1 124.5(3) . . ?
C2 C1 S2 119.9(3) . . ?
S1 C1 S2 115.6(2) . . ?
C1 C2 S3 123.6(3) . . ?
C1 C2 S4 120.9(3) . . ?
S3 C2 S4 115.5(2) . . ?
C4 C3 S5 129.0(3) . . ?
C4 C3 S1 117.1(3) . . ?
S5 C3 S1 113.9(2) . . ?
C3 C4 S2 117.1(3) . . ?
C3 C4 S6 128.2(3) . . ?
S2 C4 S6 114.7(2) . . ?
C6 C5 S7 128.7(3) . . ?
C6 C5 S3 117.3(3) . . ?
S7 C5 S3 114.0(2) . . ?
C5 C6 S8 129.3(3) . . ?
C5 C6 S4 117.2(3) . . ?
S8 C6 S4 113.5(2) . . ?
C8 C7 S5 115.0(3) . . ?
C8 C7 H7A 108.5 . . ?
S5 C7 H7A 108.5 . . ?
C8 C7 H7B 108.5 . . ?
S5 C7 H7B 108.5 . . ?
H7A C7 H7B 107.5 . . ?
C7 C8 S6 113.9(3) . . ?
C7 C8 H8A 108.8 . . ?
S6 C8 H8A 108.8 . . ?
C7 C8 H8B 108.8 . . ?
S6 C8 H8B 108.8 . . ?
H8A C8 H8B 107.7 . . ?
C10A C9A S7 115.1(4) . . ?
C10A C9A H9A 108.5 . . ?
S7 C9A H9A 108.5 . . ?
C10A C9A H9B 108.5 . . ?
S7 C9A H9B 108.5 . . ?
H9A C9A H9B 107.5 . . ?
C9A C10A S8 113.4(4) . . ?
C9A C10A H10A 108.9 . . ?
S8 C10A H10A 108.9 . . ?
C9A C10A H10B 108.9 . . ?
S8 C10A H10B 108.9 . . ?
H10A C10A H10B 107.7 . . ?
C10B C9B S7 112.8(18) . . ?
C10B C9B H9C 109.0 . . ?
S7 C9B H9C 109.0 . . ?
C10B C9B H9D 109.0 . . ?
S7 C9B H9D 109.0 . . ?
H9C C9B H9D 107.8 . . ?
C9B C10B S8 113.2(16) . . ?
C9B C10B H10C 108.9 . . ?
S8 C10B H10C 108.9 . . ?
C9B C10B H10D 108.9 . . ?
S8 C10B H10D 108.9 . . ?
H10C C10B H10D 107.7 . . ?
C1 S1 C3 95.02(18) . . ?
C1 S2 C4 95.21(18) . . ?
C2 S3 C5 94.66(19) . . ?
C2 S4 C6 94.77(18) . . ?
C3 S5 C7 101.8(2) . . ?
C4 S6 C8 100.56(19) . . ?
C9B S7 C5 105.2(8) . . ?
C9B S7 C9A 28.5(9) . . ?
C5 S7 C9A 99.5(2) . . ?
C6 S8 C10A 102.6(2) . . ?
C6 S8 C10B 95.9(6) . . ?
C10A S8 C10B 25.3(6) . . ?
N1 C11 N2 172.0(7) . . ?
N3 C12 N2 170.2(6) . . ?
C11 N1 Cu1 178.2(5) . . ?
C11 N2 C12 125.2(6) . . ?
C12 N3 Cu1 159.8(5) . 6_657 ?
N3 Cu1 N1 111.6(2) 6_557 . ?
N3 Cu1 Br1 135.76(16) 6_557 . ?
N1 Cu1 Br1 112.63(16) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
S1 C1 C2 S3 1.9(5) . . . . ?
S2 C1 C2 S3 -178.5(2) . . . . ?
S1 C1 C2 S4 -178.5(2) . . . . ?
S2 C1 C2 S4 1.1(5) . . . . ?
S5 C3 C4 S2 178.5(3) . . . . ?
S1 C3 C4 S2 -0.9(5) . . . . ?
S5 C3 C4 S6 -0.9(6) . . . . ?
S1 C3 C4 S6 179.7(2) . . . . ?
S7 C5 C6 S8 0.5(6) . . . . ?
S3 C5 C6 S8 -178.8(2) . . . . ?
S7 C5 C6 S4 179.3(2) . . . . ?
S3 C5 C6 S4 0.0(4) . . . . ?
S5 C7 C8 S6 69.1(4) . . . . ?
S7 C9A C10A S8 -69.2(5) . . . . ?
S7 C9B C10B S8 72(2) . . . . ?
C2 C1 S1 C3 -179.2(4) . . . . ?
S2 C1 S1 C3 1.2(3) . . . . ?
C4 C3 S1 C1 -0.2(4) . . . . ?
S5 C3 S1 C1 -179.7(2) . . . . ?
C2 C1 S2 C4 178.8(3) . . . . ?
S1 C1 S2 C4 -1.6(3) . . . . ?
C3 C4 S2 C1 1.5(4) . . . . ?
S6 C4 S2 C1 -179.1(2) . . . . ?
C1 C2 S3 C5 172.3(4) . . . . ?
S4 C2 S3 C5 -7.4(3) . . . . ?
C6 C5 S3 C2 4.4(3) . . . . ?
S7 C5 S3 C2 -175.0(2) . . . . ?
C1 C2 S4 C6 -172.3(3) . . . . ?
S3 C2 S4 C6 7.4(3) . . . . ?
C5 C6 S4 C2 -4.4(3) . . . . ?
S8 C6 S4 C2 174.6(2) . . . . ?
C4 C3 S5 C7 9.6(5) . . . . ?
S1 C3 S5 C7 -171.0(2) . . . . ?
C8 C7 S5 C3 -43.2(4) . . . . ?
C3 C4 S6 C8 17.5(4) . . . . ?
S2 C4 S6 C8 -161.9(2) . . . . ?
C7 C8 S6 C4 -50.4(4) . . . . ?
C10B C9B S7 C5 -50.8(19) . . . . ?
C10B C9B S7 C9A 31.0(14) . . . . ?
C6 C5 S7 C9B 14.4(11) . . . . ?
S3 C5 S7 C9B -166.3(10) . . . . ?
C6 C5 S7 C9A -14.2(4) . . . . ?
S3 C5 S7 C9A 165.2(3) . . . . ?
C10A C9A S7 C9B -56.2(18) . . . . ?
C10A C9A S7 C5 48.2(4) . . . . ?
C5 C6 S8 C10A -12.4(5) . . . . ?
S4 C6 S8 C10A 168.8(3) . . . . ?
C5 C6 S8 C10B 12.4(8) . . . . ?
S4 C6 S8 C10B -166.4(7) . . . . ?
C9A C10A S8 C6 45.7(5) . . . . ?
C9A C10A S8 C10B -31.4(15) . . . . ?
C9B C10B S8 C6 -47.2(17) . . . . ?
C9B C10B S8 C10A 59.8(17) . . . . ?
N2 C11 N1 Cu1 0.00(3) . . . . ?
N1 C11 N2 C12 180.000(7) . . . . ?
N3 C12 N2 C11 180.000(8) . . . . ?
N2 C12 N3 Cu1 0.007(10) . . . 6_657 ?
C11 N1 Cu1 N3 180.00(2) . . . 6_557 ?
C11 N1 Cu1 Br1 0.00(2) . . . . ?

_diffrn_measured_fraction_theta_max 0.986
_diffrn_reflns_theta_full        27.50
_diffrn_measured_fraction_theta_full 0.986
_refine_diff_density_max         1.517
_refine_diff_density_min         -0.630
_refine_diff_density_rms         0.121

_exptl_crystal_recrystallization_method electrocrystallization
_exptl_crystal_preparation       'Magnetic properties, electronic property'
####################################################################### 
# 
# 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/. 
# 
# Audit and citation data items have may 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_kappa-(ET)2Cu[N(CN)2]Br-200K
_database_code_depnum_ccdc_archive 'CCDC 1016182'
_audit_update_record             
;
2014-07-26 deposited with the CCDC.
2014-11-27 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            (ET)2Cu[N(CN)2]Br
_chemical_formula_moiety         '2(C10 H8 S8), (C2 Br1 Cu1 N3)'
_chemical_formula_sum            'C22 H16 Br1 Cu1 N3 S16'
_chemical_formula_weight         978.90

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'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   'Pnma '
_symmetry_space_group_name_Hall  '-P 2ac 2n'

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

_cell_length_a                   12.9117(12)
_cell_length_b                   29.845(3)
_cell_length_c                   8.5178(8)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     3282.3(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    200(2)
_cell_measurement_reflns_used    9950
_cell_measurement_theta_min      2.49
_cell_measurement_theta_max      27.95

_exptl_crystal_description       'rhombic plate'
_exptl_crystal_colour            black
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.03
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.981
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1956
_exptl_absorpt_coefficient_mu    2.926
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.4189
_exptl_absorpt_correction_T_max  0.9173
_exptl_absorpt_process_details   
;
APEX2 Software
;
_exptl_special_details           
; 
 kappa polymorph
;

_diffrn_ambient_temperature      200(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEXII CCD area detector'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean 8.333
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            16907
_diffrn_reflns_av_R_equivalents  0.0247
_diffrn_reflns_av_sigmaI/netI    0.0210
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_theta_min         1.36
_diffrn_reflns_theta_max         27.50
_reflns_number_total             3787
_reflns_number_gt                3419
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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)+(0.0252P)²+17.1393P] 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         3787
_refine_ls_number_parameters     214
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0477
_refine_ls_R_factor_gt           0.0430
_refine_ls_wR_factor_ref         0.1066
_refine_ls_wR_factor_gt          0.1045
_refine_ls_goodness_of_fit_ref   1.140
_refine_ls_restrained_S_all      1.140
_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
C1 C 0.6413(3) -0.01828(12) 0.3600(5) 0.0213(7) Uani 1 1 d . . .
C2 C 0.5787(3) 0.01873(12) 0.3588(5) 0.0220(7) Uani 1 1 d . . .
C3 C 0.7805(3) -0.07829(13) 0.4098(5) 0.0243(8) Uani 1 1 d . . .
C4 C 0.7213(3) -0.09501(12) 0.2933(5) 0.0222(8) Uani 1 1 d . . .
C5 C 0.5027(3) 0.09800(12) 0.3880(5) 0.0236(8) Uani 1 1 d . A .
C6 C 0.4454(3) 0.07835(12) 0.2766(5) 0.0229(8) Uani 1 1 d . A .
C7 C 0.9140(4) -0.14923(16) 0.3757(6) 0.0361(11) Uani 1 1 d . . .
H7A H 0.9498 -0.1382 0.2790 0.043 Uiso 1 1 calc R . .
H7B H 0.9628 -0.1698 0.4313 0.043 Uiso 1 1 calc R . .
C8 C 0.8199(4) -0.17565(14) 0.3268(5) 0.0338(10) Uani 1 1 d . . .
H8A H 0.7800 -0.1841 0.4230 0.041 Uiso 1 1 calc R . .
H8B H 0.8433 -0.2040 0.2750 0.041 Uiso 1 1 calc R . .
C9A C 0.4159(5) 0.17837(18) 0.2995(8) 0.0355(17) Uani 0.794(12) 1 d P A 1
H9A H 0.3947 0.2091 0.3337 0.043 Uiso 0.794(12) 1 calc PR A 1
H9B H 0.4596 0.1818 0.2032 0.043 Uiso 0.794(12) 1 calc PR A 1
C10A C 0.3206(5) 0.15274(19) 0.2564(8) 0.0349(16) Uani 0.794(12) 1 d P A 1
H10A H 0.2771 0.1716 0.1854 0.042 Uiso 0.794(12) 1 calc PR A 1
H10B H 0.2796 0.1468 0.3538 0.042 Uiso 0.794(12) 1 calc PR A 1
C9B C 0.3871(15) 0.1726(6) 0.392(3) 0.022(5) Uiso 0.206(12) 1 d P A 2
H9C H 0.3289 0.1574 0.4487 0.026 Uiso 0.206(12) 1 calc PR A 2
H9D H 0.3828 0.2054 0.4153 0.026 Uiso 0.206(12) 1 calc PR A 2
C10B C 0.3753(16) 0.1651(6) 0.217(2) 0.019(5) Uiso 0.206(12) 1 d P A 2
H10C H 0.4404 0.1749 0.1631 0.022 Uiso 0.206(12) 1 calc PR A 2
H10D H 0.3174 0.1843 0.1771 0.022 Uiso 0.206(12) 1 calc PR A 2
S1 S 0.74645(7) -0.02544(3) 0.48390(12) 0.0246(2) Uani 1 1 d . . .
S2 S 0.61655(8) -0.06252(3) 0.23168(12) 0.0252(2) Uani 1 1 d . . .
S3 S 0.59877(8) 0.06521(3) 0.47844(12) 0.0248(2) Uani 1 1 d . . .
S4 S 0.47265(8) 0.02234(3) 0.23287(12) 0.0253(2) Uani 1 1 d . . .
S5 S 0.88812(9) -0.10214(4) 0.50085(15) 0.0387(3) Uani 1 1 d . . .
S6 S 0.73490(9) -0.14609(3) 0.19462(13) 0.0303(2) Uani 1 1 d . . .
S7 S 0.49700(11) 0.15312(4) 0.45686(14) 0.0391(3) Uani 1 1 d . . .
S8 S 0.34650(9) 0.10110(4) 0.16226(14) 0.0351(3) Uani 1 1 d . . .
C11 C 0.8459(5) 0.2500 0.6014(7) 0.0282(12) Uani 1 2 d S . .
C12 C 0.9741(4) 0.2500 0.7917(8) 0.0282(13) Uani 1 2 d S . .
N1 N 0.7661(4) 0.2500 0.5438(7) 0.0353(12) Uani 1 2 d S . .
N2 N 0.9415(4) 0.2500 0.6455(7) 0.0468(16) Uani 1 2 d S . .
N3 N 1.0166(4) 0.2500 0.9082(6) 0.0304(11) Uani 1 2 d S . .
Cu1 Cu 0.63001(6) 0.2500 0.43919(9) 0.03126(19) Uani 1 2 d S . .
Br1 Br 0.64186(6) 0.2500 0.16621(7) 0.03851(18) Uani 1 2 d S . .


_geom_special_details            
; 
 The positional parameters of the hydrogen atoms were calculated under a 
 fixed C-H bond length of 1.00 A with sp2 configuration of the 
 bonding carbon atoms. In the refinement procedures, isotropic temperature
 factors with the magnitude of 1.2 fold to those of the equivalent
 temperature factors of the bonding carbon atoms were applied for hydrogen
 atoms.

 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 1.369(5) . ?
C1 S1 1.732(4) . ?
C1 S2 1.744(4) . ?
C2 S3 1.741(4) . ?
C2 S4 1.743(4) . ?
C3 C4 1.349(5) . ?
C3 S5 1.743(4) . ?
C3 S1 1.755(4) . ?
C4 S2 1.745(4) . ?
C4 S6 1.749(4) . ?
C5 C6 1.339(6) . ?
C5 S7 1.748(4) . ?
C5 S3 1.757(4) . ?
C6 S8 1.743(4) . ?
C6 S4 1.748(4) . ?
C7 C8 1.507(7) . ?
C7 S5 1.795(4) . ?
C7 H7A 1.0000 . ?
C7 H7B 1.0000 . ?
C8 S6 1.803(4) . ?
C8 H8A 1.0000 . ?
C8 H8B 1.0000 . ?
C9A C10A 1.495(9) . ?
C9A S7 1.860(6) . ?
C9A H9A 1.0000 . ?
C9A H9B 1.0000 . ?
C10A S8 1.769(5) . ?
C10A H10A 1.0000 . ?
C10A H10B 1.0000 . ?
C9B C10B 1.52(3) . ?
C9B S7 1.629(19) . ?
C9B H9C 1.0000 . ?
C9B H9D 1.0000 . ?
C10B S8 2.003(19) . ?
C10B H10C 1.0000 . ?
C10B H10D 1.0000 . ?
C11 N1 1.141(8) . ?
C11 N2 1.289(8) . ?
C12 N3 1.134(8) . ?
C12 N2 1.314(9) . ?
N1 Cu1 1.970(6) . ?
N3 Cu1 1.957(5) 6_657 ?
Cu1 N3 1.957(5) 6_557 ?
Cu1 Br1 2.3302(10) . ?

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 S1 124.5(3) . . ?
C2 C1 S2 119.9(3) . . ?
S1 C1 S2 115.6(2) . . ?
C1 C2 S3 123.4(3) . . ?
C1 C2 S4 121.2(3) . . ?
S3 C2 S4 115.3(2) . . ?
C4 C3 S5 128.9(3) . . ?
C4 C3 S1 117.1(3) . . ?
S5 C3 S1 114.0(2) . . ?
C3 C4 S2 117.1(3) . . ?
C3 C4 S6 128.2(3) . . ?
S2 C4 S6 114.7(2) . . ?
C6 C5 S7 128.8(3) . . ?
C6 C5 S3 117.2(3) . . ?
S7 C5 S3 114.0(2) . . ?
C5 C6 S8 129.1(3) . . ?
C5 C6 S4 117.3(3) . . ?
S8 C6 S4 113.6(2) . . ?
C8 C7 S5 115.1(3) . . ?
C8 C7 H7A 108.5 . . ?
S5 C7 H7A 108.5 . . ?
C8 C7 H7B 108.5 . . ?
S5 C7 H7B 108.5 . . ?
H7A C7 H7B 107.5 . . ?
C7 C8 S6 114.0(3) . . ?
C7 C8 H8A 108.7 . . ?
S6 C8 H8A 108.7 . . ?
C7 C8 H8B 108.7 . . ?
S6 C8 H8B 108.7 . . ?
H8A C8 H8B 107.6 . . ?
C10A C9A S7 115.6(4) . . ?
C10A C9A H9A 108.4 . . ?
S7 C9A H9A 108.4 . . ?
C10A C9A H9B 108.4 . . ?
S7 C9A H9B 108.4 . . ?
H9A C9A H9B 107.4 . . ?
C9A C10A S8 113.7(4) . . ?
C9A C10A H10A 108.8 . . ?
S8 C10A H10A 108.8 . . ?
C9A C10A H10B 108.8 . . ?
S8 C10A H10B 108.8 . . ?
H10A C10A H10B 107.7 . . ?
C10B C9B S7 111.5(15) . . ?
C10B C9B H9C 109.3 . . ?
S7 C9B H9C 109.3 . . ?
C10B C9B H9D 109.3 . . ?
S7 C9B H9D 109.3 . . ?
H9C C9B H9D 108.0 . . ?
C9B C10B S8 112.8(13) . . ?
C9B C10B H10C 109.0 . . ?
S8 C10B H10C 109.0 . . ?
C9B C10B H10D 109.0 . . ?
S8 C10B H10D 109.0 . . ?
H10C C10B H10D 107.8 . . ?
C1 S1 C3 95.05(18) . . ?
C1 S2 C4 95.17(18) . . ?
C2 S3 C5 94.71(19) . . ?
C2 S4 C6 94.94(19) . . ?
C3 S5 C7 101.8(2) . . ?
C4 S6 C8 100.80(19) . . ?
C9B S7 C5 105.0(7) . . ?
C9B S7 C9A 28.6(8) . . ?
C5 S7 C9A 99.4(2) . . ?
C6 S8 C10A 103.0(2) . . ?
C6 S8 C10B 96.0(6) . . ?
C10A S8 C10B 25.6(6) . . ?
N1 C11 N2 171.5(7) . . ?
N3 C12 N2 169.8(7) . . ?
C11 N1 Cu1 178.6(5) . . ?
C11 N2 C12 125.7(6) . . ?
C12 N3 Cu1 160.5(5) . 6_657 ?
N3 Cu1 N1 111.5(2) 6_557 . ?
N3 Cu1 Br1 135.36(16) 6_557 . ?
N1 Cu1 Br1 113.11(17) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
S1 C1 C2 S3 2.3(5) . . . . ?
S2 C1 C2 S3 -178.3(2) . . . . ?
S1 C1 C2 S4 -178.4(2) . . . . ?
S2 C1 C2 S4 1.0(5) . . . . ?
S5 C3 C4 S2 178.6(3) . . . . ?
S1 C3 C4 S2 -0.9(5) . . . . ?
S5 C3 C4 S6 -0.8(6) . . . . ?
S1 C3 C4 S6 179.7(2) . . . . ?
S7 C5 C6 S8 0.4(6) . . . . ?
S3 C5 C6 S8 -178.7(2) . . . . ?
S7 C5 C6 S4 178.9(2) . . . . ?
S3 C5 C6 S4 -0.2(4) . . . . ?
S5 C7 C8 S6 68.9(4) . . . . ?
S7 C9A C10A S8 -68.2(6) . . . . ?
S7 C9B C10B S8 73.6(17) . . . . ?
C2 C1 S1 C3 -179.6(4) . . . . ?
S2 C1 S1 C3 1.0(3) . . . . ?
C4 C3 S1 C1 0.0(4) . . . . ?
S5 C3 S1 C1 -179.7(2) . . . . ?
C2 C1 S2 C4 179.2(3) . . . . ?
S1 C1 S2 C4 -1.4(3) . . . . ?
C3 C4 S2 C1 1.4(4) . . . . ?
S6 C4 S2 C1 -179.2(2) . . . . ?
C1 C2 S3 C5 172.2(4) . . . . ?
S4 C2 S3 C5 -7.2(3) . . . . ?
C6 C5 S3 C2 4.4(3) . . . . ?
S7 C5 S3 C2 -174.8(2) . . . . ?
C1 C2 S4 C6 -172.3(3) . . . . ?
S3 C2 S4 C6 7.1(3) . . . . ?
C5 C6 S4 C2 -4.1(3) . . . . ?
S8 C6 S4 C2 174.6(2) . . . . ?
C4 C3 S5 C7 10.4(5) . . . . ?
S1 C3 S5 C7 -170.0(3) . . . . ?
C8 C7 S5 C3 -44.0(4) . . . . ?
C3 C4 S6 C8 16.5(4) . . . . ?
S2 C4 S6 C8 -162.9(2) . . . . ?
C7 C8 S6 C4 -49.4(4) . . . . ?
C10B C9B S7 C5 -51.5(16) . . . . ?
C10B C9B S7 C9A 30.5(12) . . . . ?
C6 C5 S7 C9B 15.0(9) . . . . ?
S3 C5 S7 C9B -165.9(8) . . . . ?
C6 C5 S7 C9A -13.8(5) . . . . ?
S3 C5 S7 C9A 165.4(3) . . . . ?
C10A C9A S7 C9B -56.6(15) . . . . ?
C10A C9A S7 C5 47.6(5) . . . . ?
C5 C6 S8 C10A -12.1(5) . . . . ?
S4 C6 S8 C10A 169.4(3) . . . . ?
C5 C6 S8 C10B 12.9(7) . . . . ?
S4 C6 S8 C10B -165.6(6) . . . . ?
C9A C10A S8 C6 45.0(5) . . . . ?
C9A C10A S8 C10B -31.6(13) . . . . ?
C9B C10B S8 C6 -48.6(14) . . . . ?
C9B C10B S8 C10A 59.0(15) . . . . ?
N2 C11 N1 Cu1 0.00(4) . . . . ?
N1 C11 N2 C12 180.000(7) . . . . ?
N3 C12 N2 C11 180.000(8) . . . . ?
N2 C12 N3 Cu1 0.006(9) . . . 6_657 ?
C11 N1 Cu1 N3 180.00(3) . . . 6_557 ?
C11 N1 Cu1 Br1 0.00(3) . . . . ?

_diffrn_measured_fraction_theta_max 0.987
_diffrn_reflns_theta_full        27.50
_diffrn_measured_fraction_theta_full 0.987
_refine_diff_density_max         1.227
_refine_diff_density_min         -0.655
_refine_diff_density_rms         0.114

_exptl_crystal_recrystallization_method electrocrystallization
_exptl_crystal_preparation       'Magnetic properties, electronic property'
####################################################################### 
# 
# 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/. 
# 
# Audit and citation data items have may 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_kappa-(ET)2Cu[N(CN)2]Br-250K
_database_code_depnum_ccdc_archive 'CCDC 1016183'
_audit_update_record             
;
2014-07-26 deposited with the CCDC.
2014-11-27 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            (ET)2Cu[N(CN)2]Br
_chemical_formula_moiety         '2(C10 H8 S8), (C2 Br1 Cu1 N3)'
_chemical_formula_sum            'C22 H16 Br1 Cu1 N3 S16'
_chemical_formula_weight         978.90

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'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   'Pnma '
_symmetry_space_group_name_Hall  '-P 2ac 2n'

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

_cell_length_a                   12.9342(13)
_cell_length_b                   29.937(3)
_cell_length_c                   8.5325(8)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     3303.9(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    250(2)
_cell_measurement_reflns_used    9151
_cell_measurement_theta_min      2.48
_cell_measurement_theta_max      27.91

_exptl_crystal_description       'rhombic plate'
_exptl_crystal_colour            black
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.03
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.968
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1956
_exptl_absorpt_coefficient_mu    2.907
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.4209
_exptl_absorpt_correction_T_max  0.9178
_exptl_absorpt_process_details   
;
APEX2 Software
;
_exptl_special_details           
; 
 kappa polymorph
;

_diffrn_ambient_temperature      250(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEXII CCD area detector'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean 8.333
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            17013
_diffrn_reflns_av_R_equivalents  0.0258
_diffrn_reflns_av_sigmaI/netI    0.0226
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_theta_min         1.36
_diffrn_reflns_theta_max         27.50
_reflns_number_total             3816
_reflns_number_gt                3353
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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)+(0.0261P)²+15.2927P] 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         3816
_refine_ls_number_parameters     224
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0510
_refine_ls_R_factor_gt           0.0446
_refine_ls_wR_factor_ref         0.1089
_refine_ls_wR_factor_gt          0.1061
_refine_ls_goodness_of_fit_ref   1.117
_refine_ls_restrained_S_all      1.117
_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
C1 C 0.6409(3) -0.01823(12) 0.3597(5) 0.0258(8) Uani 1 1 d . . .
C2 C 0.5789(3) 0.01877(12) 0.3582(5) 0.0264(8) Uani 1 1 d . . .
C3 C 0.7793(3) -0.07834(13) 0.4101(5) 0.0292(8) Uani 1 1 d . . .
C4 C 0.7204(3) -0.09488(12) 0.2936(5) 0.0274(8) Uani 1 1 d . . .
C5 C 0.5041(3) 0.09791(12) 0.3875(5) 0.0283(8) Uani 1 1 d . A .
C6 C 0.4466(3) 0.07845(13) 0.2766(5) 0.0276(8) Uani 1 1 d . A .
C7 C 0.9122(4) -0.14909(17) 0.3758(6) 0.0442(12) Uani 1 1 d . . .
H7A H 0.9481 -0.1380 0.2795 0.053 Uiso 1 1 calc R . .
H7B H 0.9609 -0.1697 0.4313 0.053 Uiso 1 1 calc R . .
C8 C 0.8188(4) -0.17527(14) 0.3267(5) 0.0407(11) Uani 1 1 d . . .
H8A H 0.7792 -0.1840 0.4226 0.049 Uiso 1 1 calc R . .
H8B H 0.8423 -0.2034 0.2743 0.049 Uiso 1 1 calc R . .
C9A C 0.4184(6) 0.1780(2) 0.2994(12) 0.041(2) Uani 0.744(19) 1 d P A 1
H9A H 0.3980 0.2088 0.3332 0.049 Uiso 0.744(19) 1 calc PR A 1
H9B H 0.4619 0.1812 0.2031 0.049 Uiso 0.744(19) 1 calc PR A 1
C10A C 0.3216(8) 0.1528(2) 0.2562(10) 0.0408(19) Uani 0.744(19) 1 d P A 1
H10A H 0.2786 0.1717 0.1849 0.049 Uiso 0.744(19) 1 calc PR A 1
H10B H 0.2804 0.1470 0.3534 0.049 Uiso 0.744(19) 1 calc PR A 1
C9B C 0.3902(15) 0.1728(7) 0.390(3) 0.035(5) Uani 0.256(19) 1 d P A 2
H9C H 0.3318 0.1589 0.4486 0.042 Uiso 0.256(19) 1 calc PR A 2
H9D H 0.3882 0.2057 0.4095 0.042 Uiso 0.256(19) 1 calc PR A 2
C10B C 0.375(2) 0.1646(7) 0.217(2) 0.034(6) Uani 0.256(19) 1 d P A 2
H10C H 0.4379 0.1748 0.1599 0.041 Uiso 0.256(19) 1 calc PR A 2
H10D H 0.3153 0.1832 0.1803 0.041 Uiso 0.256(19) 1 calc PR A 2
S1 S 0.74590(8) -0.02552(3) 0.48333(12) 0.0303(2) Uani 1 1 d . . .
S2 S 0.61617(8) -0.06236(3) 0.23154(12) 0.0308(2) Uani 1 1 d . . .
S3 S 0.59964(8) 0.06501(3) 0.47765(12) 0.0302(2) Uani 1 1 d . . .
S4 S 0.47310(8) 0.02261(3) 0.23274(13) 0.0309(2) Uani 1 1 d . . .
S5 S 0.88641(10) -0.10225(4) 0.50104(16) 0.0472(3) Uani 1 1 d . . .
S6 S 0.73344(9) -0.14589(4) 0.19571(13) 0.0377(3) Uani 1 1 d . . .
S7 S 0.49923(12) 0.15283(4) 0.45629(15) 0.0474(3) Uani 1 1 d . . .
S8 S 0.34787(10) 0.10136(4) 0.16314(15) 0.0431(3) Uani 1 1 d . . .
C11 C 0.8479(5) 0.2500 0.6028(8) 0.0350(13) Uani 1 2 d S . .
C12 C 0.9764(5) 0.2500 0.7927(8) 0.0342(13) Uani 1 2 d S . .
N1 N 0.7686(4) 0.2500 0.5456(7) 0.0431(13) Uani 1 2 d S . .
N2 N 0.9434(5) 0.2500 0.6474(8) 0.0607(19) Uani 1 2 d S . .
N3 N 1.0197(4) 0.2500 0.9081(7) 0.0373(12) Uani 1 2 d S . .
Cu1 Cu 0.63309(7) 0.2500 0.44002(9) 0.0385(2) Uani 1 2 d S . .
Br1 Br 0.64360(7) 0.2500 0.16764(8) 0.0475(2) Uani 1 2 d S . .


_geom_special_details            
; 
 The positional parameters of the hydrogen atoms were calculated under a 
 fixed C-H bond length of 1.00 A with sp2 configuration of the 
 bonding carbon atoms. In the refinement procedures, isotropic temperature
 factors with the magnitude of 1.2 fold to those of the equivalent
 temperature factors of the bonding carbon atoms were applied for hydrogen
 atoms.

 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 1.368(5) . ?
C1 S1 1.733(4) . ?
C1 S2 1.745(4) . ?
C2 S3 1.740(4) . ?
C2 S4 1.741(4) . ?
C3 C4 1.347(5) . ?
C3 S5 1.742(4) . ?
C3 S1 1.754(4) . ?
C4 S2 1.745(4) . ?
C4 S6 1.749(4) . ?
C5 C6 1.337(6) . ?
C5 S7 1.747(4) . ?
C5 S3 1.757(4) . ?
C6 S8 1.743(4) . ?
C6 S4 1.747(4) . ?
C7 C8 1.500(7) . ?
C7 S5 1.794(5) . ?
C7 H7A 1.0000 . ?
C7 H7B 1.0000 . ?
C8 S6 1.801(4) . ?
C8 H8A 1.0000 . ?
C8 H8B 1.0000 . ?
C9A C10A 1.508(13) . ?
C9A S7 1.859(8) . ?
C9A H9A 1.0000 . ?
C9A H9B 1.0000 . ?
C10A S8 1.765(7) . ?
C10A H10A 1.0000 . ?
C10A H10B 1.0000 . ?
C9B C10B 1.50(3) . ?
C9B S7 1.634(17) . ?
C9B H9C 1.0000 . ?
C9B H9D 1.0000 . ?
C10B S8 1.98(2) . ?
C10B H10C 1.0000 . ?
C10B H10D 1.0000 . ?
C11 N1 1.136(8) . ?
C11 N2 1.292(9) . ?
C12 N3 1.133(8) . ?
C12 N2 1.311(9) . ?
N1 Cu1 1.971(6) . ?
N3 Cu1 1.957(6) 6_657 ?
Cu1 N3 1.957(6) 6_557 ?
Cu1 Br1 2.3281(11) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 C1 S1 124.6(3) . . ?
C2 C1 S2 120.0(3) . . ?
S1 C1 S2 115.5(2) . . ?
C1 C2 S3 123.2(3) . . ?
C1 C2 S4 121.4(3) . . ?
S3 C2 S4 115.4(2) . . ?
C4 C3 S5 128.9(3) . . ?
C4 C3 S1 117.1(3) . . ?
S5 C3 S1 114.0(2) . . ?
C3 C4 S2 117.1(3) . . ?
C3 C4 S6 128.2(3) . . ?
S2 C4 S6 114.6(2) . . ?
C6 C5 S7 128.9(3) . . ?
C6 C5 S3 117.2(3) . . ?
S7 C5 S3 113.9(2) . . ?
C5 C6 S8 129.0(3) . . ?
C5 C6 S4 117.4(3) . . ?
S8 C6 S4 113.6(2) . . ?
C8 C7 S5 115.2(3) . . ?
C8 C7 H7A 108.5 . . ?
S5 C7 H7A 108.5 . . ?
C8 C7 H7B 108.5 . . ?
S5 C7 H7B 108.5 . . ?
H7A C7 H7B 107.5 . . ?
C7 C8 S6 114.3(3) . . ?
C7 C8 H8A 108.7 . . ?
S6 C8 H8A 108.7 . . ?
C7 C8 H8B 108.7 . . ?
S6 C8 H8B 108.7 . . ?
H8A C8 H8B 107.6 . . ?
C10A C9A S7 116.0(6) . . ?
C10A C9A H9A 108.3 . . ?
S7 C9A H9A 108.3 . . ?
C10A C9A H9B 108.3 . . ?
S7 C9A H9B 108.3 . . ?
H9A C9A H9B 107.4 . . ?
C9A C10A S8 112.8(7) . . ?
C9A C10A H10A 109.0 . . ?
S8 C10A H10A 109.0 . . ?
C9A C10A H10B 109.0 . . ?
S8 C10A H10B 109.0 . . ?
H10A C10A H10B 107.8 . . ?
C10B C9B S7 113.3(16) . . ?
C10B C9B H9C 108.9 . . ?
S7 C9B H9C 108.9 . . ?
C10B C9B H9D 108.9 . . ?
S7 C9B H9D 108.9 . . ?
H9C C9B H9D 107.7 . . ?
C9B C10B S8 114.1(18) . . ?
C9B C10B H10C 108.7 . . ?
S8 C10B H10C 108.7 . . ?
C9B C10B H10D 108.7 . . ?
S8 C10B H10D 108.7 . . ?
H10C C10B H10D 107.6 . . ?
C1 S1 C3 95.14(19) . . ?
C4 S2 C1 95.19(18) . . ?
C2 S3 C5 94.65(19) . . ?
C2 S4 C6 94.89(19) . . ?
C3 S5 C7 101.8(2) . . ?
C4 S6 C8 100.9(2) . . ?
C9B S7 C5 105.0(7) . . ?
C9B S7 C9A 27.7(8) . . ?
C5 S7 C9A 99.2(3) . . ?
C6 S8 C10A 103.5(3) . . ?
C6 S8 C10B 96.7(5) . . ?
C10A S8 C10B 25.1(7) . . ?
N1 C11 N2 171.7(7) . . ?
N3 C12 N2 169.4(7) . . ?
C11 N1 Cu1 178.2(6) . . ?
C11 N2 C12 126.2(6) . . ?
C12 N3 Cu1 161.1(5) . 6_657 ?
N3 Cu1 N1 111.3(2) 6_557 . ?
N3 Cu1 Br1 134.80(17) 6_557 . ?
N1 Cu1 Br1 113.86(18) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
S1 C1 C2 S3 2.1(5) . . . . ?
S2 C1 C2 S3 -178.2(2) . . . . ?
S1 C1 C2 S4 -178.5(2) . . . . ?
S2 C1 C2 S4 1.2(5) . . . . ?
S5 C3 C4 S2 178.8(3) . . . . ?
S1 C3 C4 S2 -1.2(5) . . . . ?
S5 C3 C4 S6 -0.3(7) . . . . ?
S1 C3 C4 S6 179.7(3) . . . . ?
S7 C5 C6 S8 0.2(6) . . . . ?
S3 C5 C6 S8 -178.9(2) . . . . ?
S7 C5 C6 S4 178.8(2) . . . . ?
S3 C5 C6 S4 -0.3(5) . . . . ?
S5 C7 C8 S6 68.5(5) . . . . ?
S7 C9A C10A S8 -68.2(10) . . . . ?
S7 C9B C10B S8 71(3) . . . . ?
C2 C1 S1 C3 -179.6(4) . . . . ?
S2 C1 S1 C3 0.7(3) . . . . ?
C4 C3 S1 C1 0.3(4) . . . . ?
S5 C3 S1 C1 -179.7(3) . . . . ?
C3 C4 S2 C1 1.4(4) . . . . ?
S6 C4 S2 C1 -179.4(2) . . . . ?
C2 C1 S2 C4 179.1(3) . . . . ?
S1 C1 S2 C4 -1.2(3) . . . . ?
C1 C2 S3 C5 172.3(4) . . . . ?
S4 C2 S3 C5 -7.1(3) . . . . ?
C6 C5 S3 C2 4.5(4) . . . . ?
S7 C5 S3 C2 -174.8(2) . . . . ?
C1 C2 S4 C6 -172.4(4) . . . . ?
S3 C2 S4 C6 7.0(3) . . . . ?
C5 C6 S4 C2 -4.0(4) . . . . ?
S8 C6 S4 C2 174.8(2) . . . . ?
C4 C3 S5 C7 10.4(5) . . . . ?
S1 C3 S5 C7 -169.6(3) . . . . ?
C8 C7 S5 C3 -44.0(4) . . . . ?
C3 C4 S6 C8 15.6(5) . . . . ?
S2 C4 S6 C8 -163.5(3) . . . . ?
C7 C8 S6 C4 -48.7(4) . . . . ?
C10B C9B S7 C5 -49(2) . . . . ?
C10B C9B S7 C9A 32.0(17) . . . . ?
C6 C5 S7 C9B 14.1(10) . . . . ?
S3 C5 S7 C9B -166.8(10) . . . . ?
C6 C5 S7 C9A -13.7(5) . . . . ?
S3 C5 S7 C9A 165.4(4) . . . . ?
C10A C9A S7 C9B -56.8(16) . . . . ?
C10A C9A S7 C5 47.9(8) . . . . ?
C5 C6 S8 C10A -12.2(6) . . . . ?
S4 C6 S8 C10A 169.2(4) . . . . ?
C5 C6 S8 C10B 12.4(9) . . . . ?
S4 C6 S8 C10B -166.2(9) . . . . ?
C9A C10A S8 C6 44.7(8) . . . . ?
C9A C10A S8 C10B -32.1(13) . . . . ?
C9B C10B S8 C6 -46.5(19) . . . . ?
C9B C10B S8 C10A 61(2) . . . . ?
N2 C11 N1 Cu1 0.00(3) . . . . ?
N1 C11 N2 C12 180.000(7) . . . . ?
N3 C12 N2 C11 180.000(8) . . . . ?
N2 C12 N3 Cu1 -0.008(10) . . . 6_657 ?
C11 N1 Cu1 N3 180.00(3) . . . 6_557 ?
C11 N1 Cu1 Br1 0.00(3) . . . . ?

_diffrn_measured_fraction_theta_max 0.987
_diffrn_reflns_theta_full        27.50
_diffrn_measured_fraction_theta_full 0.987
_refine_diff_density_max         1.051
_refine_diff_density_min         -0.665
_refine_diff_density_rms         0.106

_exptl_crystal_recrystallization_method electrocrystallization
_exptl_crystal_preparation       'Magnetic properties, electronic property'

####################################################################### 
# 
# 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/. 
# 
# Audit and citation data items have may 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_kappa-(ET)2Cu[N(CN)2]Br-298K
_database_code_depnum_ccdc_archive 'CCDC 1016184'
_audit_update_record             
;
2014-07-26 deposited with the CCDC.
2014-11-27 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            (ET)2Cu[N(CN)2]Br
_chemical_formula_moiety         '2(C10 H8 S8), (C2 Br1 Cu1 N3)'
_chemical_formula_sum            'C22 H16 Br1 Cu1 N3 S16'
_chemical_formula_weight         978.90

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'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'


_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   'Pnma '
_symmetry_space_group_name_Hall  '-P 2ac 2n'

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

_cell_length_a                   12.9653(13)
_cell_length_b                   30.028(3)
_cell_length_c                   8.5444(9)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     3326.5(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    8377
_cell_measurement_theta_min      2.48
_cell_measurement_theta_max      27.82

_exptl_crystal_description       'rhombic plate'
_exptl_crystal_colour            black
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.03
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.954
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1956
_exptl_absorpt_coefficient_mu    2.888
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.4229
_exptl_absorpt_correction_T_max  0.9184
_exptl_absorpt_process_details   
;
APEX2 Software
;
_exptl_special_details           
; 
 kappa polymorph
;

_diffrn_ambient_temperature      298(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEXII CCD area detector'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean 8.333
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            17153
_diffrn_reflns_av_R_equivalents  0.0269
_diffrn_reflns_av_sigmaI/netI    0.0233
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_theta_min         1.36
_diffrn_reflns_theta_max         27.50
_reflns_number_total             3833
_reflns_number_gt                3272
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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)+(0.0316P)²+13.9633P] 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         3833
_refine_ls_number_parameters     224
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0548
_refine_ls_R_factor_gt           0.0463
_refine_ls_wR_factor_ref         0.1148
_refine_ls_wR_factor_gt          0.1108
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_restrained_S_all      1.077
_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
C1 C 0.6402(3) -0.01821(13) 0.3589(5) 0.0313(8) Uani 1 1 d . . .
C2 C 0.5791(3) 0.01874(13) 0.3578(5) 0.0315(8) Uani 1 1 d . . .
C3 C 0.7778(3) -0.07824(13) 0.4102(5) 0.0345(9) Uani 1 1 d . . .
C4 C 0.7194(3) -0.09464(13) 0.2939(5) 0.0326(8) Uani 1 1 d . . .
C5 C 0.5051(3) 0.09771(13) 0.3867(5) 0.0336(9) Uani 1 1 d . A .
C6 C 0.4478(3) 0.07850(13) 0.2764(5) 0.0325(8) Uani 1 1 d . A .
C7 C 0.9103(4) -0.14882(18) 0.3756(6) 0.0533(13) Uani 1 1 d . . .
H7A H 0.9462 -0.1378 0.2795 0.064 Uiso 1 1 calc R . .
H7B H 0.9587 -0.1694 0.4310 0.064 Uiso 1 1 calc R . .
C8 C 0.8176(4) -0.17478(15) 0.3264(6) 0.0473(12) Uani 1 1 d . . .
H8A H 0.7783 -0.1836 0.4222 0.057 Uiso 1 1 calc R . .
H8B H 0.8412 -0.2027 0.2736 0.057 Uiso 1 1 calc R . .
C9A C 0.4199(7) 0.1779(2) 0.2995(15) 0.047(3) Uani 0.71(2) 1 d P A 1
H9A H 0.3995 0.2084 0.3342 0.057 Uiso 0.71(2) 1 calc PR A 1
H9B H 0.4630 0.1813 0.2032 0.057 Uiso 0.71(2) 1 calc PR A 1
C10A C 0.3239(9) 0.1529(3) 0.2563(12) 0.050(2) Uani 0.71(2) 1 d P A 1
H10A H 0.2813 0.1717 0.1848 0.060 Uiso 0.71(2) 1 calc PR A 1
H10B H 0.2826 0.1473 0.3531 0.060 Uiso 0.71(2) 1 calc PR A 1
C9B C 0.3930(15) 0.1725(7) 0.388(3) 0.042(6) Uani 0.29(2) 1 d P A 2
H9C H 0.3346 0.1587 0.4470 0.050 Uiso 0.29(2) 1 calc PR A 2
H9D H 0.3911 0.2053 0.4079 0.050 Uiso 0.29(2) 1 calc PR A 2
C10B C 0.377(2) 0.1644(8) 0.217(3) 0.049(8) Uani 0.29(2) 1 d P A 2
H10C H 0.4405 0.1743 0.1592 0.058 Uiso 0.29(2) 1 calc PR A 2
H10D H 0.3183 0.1831 0.1798 0.058 Uiso 0.29(2) 1 calc PR A 2
S1 S 0.74511(8) -0.02553(3) 0.48248(13) 0.0363(2) Uani 1 1 d . . .
S2 S 0.61564(9) -0.06223(3) 0.23158(13) 0.0369(2) Uani 1 1 d . . .
S3 S 0.60036(8) 0.06483(3) 0.47649(13) 0.0361(2) Uani 1 1 d . . .
S4 S 0.47345(9) 0.02283(3) 0.23259(13) 0.0370(2) Uani 1 1 d . . .
S5 S 0.88480(10) -0.10215(5) 0.50074(17) 0.0560(4) Uani 1 1 d . . .
S6 S 0.73198(10) -0.14564(4) 0.19675(14) 0.0461(3) Uani 1 1 d . . .
S7 S 0.50148(13) 0.15255(4) 0.45533(16) 0.0562(4) Uani 1 1 d . . .
S8 S 0.34933(11) 0.10158(4) 0.16377(16) 0.0519(3) Uani 1 1 d . . .
C11 C 0.8501(5) 0.2500 0.6047(8) 0.0422(15) Uani 1 2 d S . .
C12 C 0.9785(5) 0.2500 0.7938(9) 0.0420(15) Uani 1 2 d S . .
N1 N 0.7715(5) 0.2500 0.5473(7) 0.0513(14) Uani 1 2 d S . .
N2 N 0.9451(5) 0.2500 0.6491(8) 0.076(2) Uani 1 2 d S . .
N3 N 1.0228(4) 0.2500 0.9076(7) 0.0437(13) Uani 1 2 d S . .
Cu1 Cu 0.63661(7) 0.2500 0.44106(10) 0.0465(2) Uani 1 2 d S . .
Br1 Br 0.64566(7) 0.2500 0.16935(8) 0.0570(2) Uani 1 2 d S . .


_geom_special_details            
; 
 The positional parameters of the hydrogen atoms were calculated under a 
 fixed C-H bond length of 1.00 A with sp2 configuration of the 
 bonding carbon atoms. In the refinement procedures, isotropic temperature
 factors with the magnitude of 1.2 fold to those of the equivalent
 temperature factors of the bonding carbon atoms were applied for hydrogen
 atoms.

 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 1.363(5) . ?
C1 S1 1.736(4) . ?
C1 S2 1.742(4) . ?
C2 S3 1.738(4) . ?
C2 S4 1.743(4) . ?
C3 C4 1.343(6) . ?
C3 S5 1.743(4) . ?
C3 S1 1.751(4) . ?
C4 S2 1.744(4) . ?
C4 S6 1.750(4) . ?
C5 C6 1.332(6) . ?
C5 S7 1.748(4) . ?
C5 S3 1.757(4) . ?
C6 S8 1.742(4) . ?
C6 S4 1.745(4) . ?
C7 C8 1.492(7) . ?
C7 S5 1.794(5) . ?
C7 H7A 1.0000 . ?
C7 H7B 1.0000 . ?
C8 S6 1.796(5) . ?
C8 H8A 1.0000 . ?
C8 H8B 1.0000 . ?
C9A C10A 1.500(15) . ?
C9A S7 1.863(9) . ?
C9A H9A 1.0000 . ?
C9A H9B 1.0000 . ?
C10A S8 1.762(8) . ?
C10A H10A 1.0000 . ?
C10A H10B 1.0000 . ?
C9B C10B 1.50(3) . ?
C9B S7 1.634(16) . ?
C9B H9C 1.0000 . ?
C9B H9D 1.0000 . ?
C10B S8 1.97(3) . ?
C10B H10C 1.0000 . ?
C10B H10D 1.0000 . ?
C11 N1 1.130(9) . ?
C11 N2 1.289(10) . ?
C12 N3 1.130(9) . ?
C12 N2 1.310(10) . ?
N1 Cu1 1.971(6) . ?
N3 Cu1 1.962(6) 6_657 ?
Cu1 N3 1.962(6) 6_557 ?
Cu1 Br1 2.3246(12) . ?

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 S1 124.2(3) . . ?
C2 C1 S2 120.5(3) . . ?
S1 C1 S2 115.3(2) . . ?
C1 C2 S3 123.5(3) . . ?
C1 C2 S4 121.2(3) . . ?
S3 C2 S4 115.3(2) . . ?
C4 C3 S5 128.8(3) . . ?
C4 C3 S1 117.1(3) . . ?
S5 C3 S1 114.1(2) . . ?
C3 C4 S2 117.2(3) . . ?
C3 C4 S6 128.3(3) . . ?
S2 C4 S6 114.6(2) . . ?
C6 C5 S7 129.1(3) . . ?
C6 C5 S3 117.2(3) . . ?
S7 C5 S3 113.7(2) . . ?
C5 C6 S8 128.9(3) . . ?
C5 C6 S4 117.4(3) . . ?
S8 C6 S4 113.7(2) . . ?
C8 C7 S5 115.3(4) . . ?
C8 C7 H7A 108.4 . . ?
S5 C7 H7A 108.4 . . ?
C8 C7 H7B 108.4 . . ?
S5 C7 H7B 108.4 . . ?
H7A C7 H7B 107.5 . . ?
C7 C8 S6 114.6(4) . . ?
C7 C8 H8A 108.6 . . ?
S6 C8 H8A 108.6 . . ?
C7 C8 H8B 108.6 . . ?
S6 C8 H8B 108.6 . . ?
H8A C8 H8B 107.6 . . ?
C10A C9A S7 116.3(7) . . ?
C10A C9A H9A 108.2 . . ?
S7 C9A H9A 108.2 . . ?
C10A C9A H9B 108.2 . . ?
S7 C9A H9B 108.2 . . ?
H9A C9A H9B 107.4 . . ?
C9A C10A S8 113.1(8) . . ?
C9A C10A H10A 109.0 . . ?
S8 C10A H10A 109.0 . . ?
C9A C10A H10B 109.0 . . ?
S8 C10A H10B 109.0 . . ?
H10A C10A H10B 107.8 . . ?
C10B C9B S7 113.7(18) . . ?
C10B C9B H9C 108.8 . . ?
S7 C9B H9C 108.8 . . ?
C10B C9B H9D 108.8 . . ?
S7 C9B H9D 108.8 . . ?
H9C C9B H9D 107.7 . . ?
C9B C10B S8 114(2) . . ?
C9B C10B H10C 108.8 . . ?
S8 C10B H10C 108.8 . . ?
C9B C10B H10D 108.8 . . ?
S8 C10B H10D 108.8 . . ?
H10C C10B H10D 107.7 . . ?
C1 S1 C3 95.17(19) . . ?
C1 S2 C4 95.27(19) . . ?
C2 S3 C5 94.67(19) . . ?
C2 S4 C6 94.93(19) . . ?
C3 S5 C7 101.8(2) . . ?
C4 S6 C8 101.0(2) . . ?
C9B S7 C5 104.5(7) . . ?
C9B S7 C9A 27.1(8) . . ?
C5 S7 C9A 99.2(3) . . ?
C6 S8 C10A 103.7(3) . . ?
C6 S8 C10B 96.8(6) . . ?
C10A S8 C10B 25.4(7) . . ?
N1 C11 N2 171.4(8) . . ?
N3 C12 N2 168.7(7) . . ?
C11 N1 Cu1 178.3(6) . . ?
C11 N2 C12 126.4(7) . . ?
C12 N3 Cu1 161.8(6) . 6_657 ?
N3 Cu1 N1 111.3(3) 6_557 . ?
N3 Cu1 Br1 134.13(18) 6_557 . ?
N1 Cu1 Br1 114.54(18) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
S1 C1 C2 S3 2.1(6) . . . . ?
S2 C1 C2 S3 -178.0(2) . . . . ?
S1 C1 C2 S4 -178.6(2) . . . . ?
S2 C1 C2 S4 1.3(5) . . . . ?
S5 C3 C4 S2 179.1(3) . . . . ?
S1 C3 C4 S2 -1.6(5) . . . . ?
S5 C3 C4 S6 0.4(7) . . . . ?
S1 C3 C4 S6 179.7(3) . . . . ?
S7 C5 C6 S8 -0.3(7) . . . . ?
S3 C5 C6 S8 -179.0(3) . . . . ?
S7 C5 C6 S4 178.6(3) . . . . ?
S3 C5 C6 S4 -0.1(5) . . . . ?
S5 C7 C8 S6 68.2(5) . . . . ?
S7 C9A C10A S8 -67.5(12) . . . . ?
S7 C9B C10B S8 71(3) . . . . ?
C2 C1 S1 C3 -179.7(4) . . . . ?
S2 C1 S1 C3 0.4(3) . . . . ?
C4 C3 S1 C1 0.7(4) . . . . ?
S5 C3 S1 C1 -179.9(3) . . . . ?
C2 C1 S2 C4 179.0(4) . . . . ?
S1 C1 S2 C4 -1.1(3) . . . . ?
C3 C4 S2 C1 1.6(4) . . . . ?
S6 C4 S2 C1 -179.5(2) . . . . ?
C1 C2 S3 C5 172.4(4) . . . . ?
S4 C2 S3 C5 -6.9(3) . . . . ?
C6 C5 S3 C2 4.2(4) . . . . ?
S7 C5 S3 C2 -174.6(2) . . . . ?
C1 C2 S4 C6 -172.4(4) . . . . ?
S3 C2 S4 C6 6.9(3) . . . . ?
C5 C6 S4 C2 -4.1(4) . . . . ?
S8 C6 S4 C2 175.0(2) . . . . ?
C4 C3 S5 C7 10.1(5) . . . . ?
S1 C3 S5 C7 -169.2(3) . . . . ?
C8 C7 S5 C3 -43.9(4) . . . . ?
C3 C4 S6 C8 14.8(5) . . . . ?
S2 C4 S6 C8 -163.9(3) . . . . ?
C7 C8 S6 C4 -48.1(4) . . . . ?
C10B C9B S7 C5 -49(3) . . . . ?
C10B C9B S7 C9A 32(2) . . . . ?
C6 C5 S7 C9B 14.2(11) . . . . ?
S3 C5 S7 C9B -167.1(11) . . . . ?
C6 C5 S7 C9A -13.0(6) . . . . ?
S3 C5 S7 C9A 165.7(4) . . . . ?
C10A C9A S7 C9B -56.9(16) . . . . ?
C10A C9A S7 C5 47.1(10) . . . . ?
C5 C6 S8 C10A -11.9(6) . . . . ?
S4 C6 S8 C10A 169.2(5) . . . . ?
C5 C6 S8 C10B 13.0(10) . . . . ?
S4 C6 S8 C10B -166.0(10) . . . . ?
C9A C10A S8 C6 44.5(10) . . . . ?
C9A C10A S8 C10B -32.2(14) . . . . ?
C9B C10B S8 C6 -47(2) . . . . ?
C9B C10B S8 C10A 61(2) . . . . ?
N2 C11 N1 Cu1 0.00(3) . . . . ?
N1 C11 N2 C12 180.000(7) . . . . ?
N3 C12 N2 C11 180.000(8) . . . . ?
N2 C12 N3 Cu1 -0.007(10) . . . 6_657 ?
C11 N1 Cu1 N3 180.00(3) . . . 6_557 ?
C11 N1 Cu1 Br1 0.00(3) . . . . ?

_diffrn_measured_fraction_theta_max 0.985
_diffrn_reflns_theta_full        27.50
_diffrn_measured_fraction_theta_full 0.985
_refine_diff_density_max         0.916
_refine_diff_density_min         -0.719
_refine_diff_density_rms         0.100

_exptl_crystal_recrystallization_method electrocrystallization
_exptl_crystal_preparation       'Magnetic properties, electronic property'
####################################################################### 
# 
# 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/. 
# 
# Audit and citation data items have may 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_kappa-(ET)2Cu[N(CN)2]Cl-100K
_database_code_depnum_ccdc_archive 'CCDC 1016185'
_audit_update_record             
;
2014-07-26 deposited with the CCDC.
2014-11-27 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            (ET)2Cu[N(CN)2]Cl
_chemical_formula_moiety         '2(C10 H8 S8), (C2 Cl1 Cu1 N3)'
_chemical_formula_sum            'C22 H16 Cl1 Cu1 N3 S16'
_chemical_formula_weight         934.44

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   'Pnma '
_symmetry_space_group_name_Hall  '-P 2ac 2n'

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

_cell_length_a                   12.8852(7)
_cell_length_b                   29.5759(17)
_cell_length_c                   8.4161(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     3207.3(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9888
_cell_measurement_theta_min      2.52
_cell_measurement_theta_max      28.12

_exptl_crystal_description       'elongate block'
_exptl_crystal_colour            black
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.16
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.935
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1884
_exptl_absorpt_coefficient_mu    1.832
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.5917
_exptl_absorpt_correction_T_max  0.7581
_exptl_absorpt_process_details   
;
APEX2 Software
;
_exptl_special_details           
; 
 kappa polymorph
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean 8.333
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            16834
_diffrn_reflns_av_R_equivalents  0.0103
_diffrn_reflns_av_sigmaI/netI    0.0084
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_theta_min         1.38
_diffrn_reflns_theta_max         27.49
_reflns_number_total             3690
_reflns_number_gt                3517
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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)+(0.0627P)²+15.3777P] 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         3690
_refine_ls_number_parameters     205
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0411
_refine_ls_R_factor_gt           0.0394
_refine_ls_wR_factor_ref         0.1196
_refine_ls_wR_factor_gt          0.1178
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_restrained_S_all      1.059
_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
C1 C 0.6400(2) -0.01844(11) 0.3603(4) 0.0141(6) Uani 1 1 d . . .
C2 C 0.5777(2) 0.01875(10) 0.3590(4) 0.0137(6) Uani 1 1 d . . .
C3 C 0.7821(2) -0.07814(11) 0.4092(4) 0.0147(6) Uani 1 1 d . . .
C4 C 0.7222(2) -0.09579(11) 0.2933(4) 0.0141(6) Uani 1 1 d . . .
C5 C 0.5004(2) 0.09849(10) 0.3883(4) 0.0146(6) Uani 1 1 d . . .
C6 C 0.4428(3) 0.07826(11) 0.2746(4) 0.0143(6) Uani 1 1 d . . .
C7 C 0.9148(3) -0.15117(12) 0.3798(4) 0.0222(7) Uani 1 1 d . . .
H7A H 0.9519 -0.1416 0.2810 0.027 Uiso 1 1 calc R . .
H7B H 0.9620 -0.1719 0.4395 0.027 Uiso 1 1 calc R . .
C8 C 0.8186(3) -0.17724(11) 0.3326(4) 0.0198(7) Uani 1 1 d . . .
H8A H 0.7776 -0.1842 0.4304 0.024 Uiso 1 1 calc R . .
H8B H 0.8402 -0.2066 0.2839 0.024 Uiso 1 1 calc R . .
C9A C 0.4145(3) 0.17993(12) 0.3005(5) 0.0242(7) Uani 1 1 d . . .
H9A H 0.3931 0.2108 0.3358 0.029 Uiso 1 1 calc R . .
H9B H 0.4581 0.1835 0.2029 0.029 Uiso 1 1 calc R . .
C10A C 0.3183(3) 0.15319(12) 0.2581(5) 0.0237(7) Uani 1 1 d . . .
H10A H 0.2730 0.1723 0.1888 0.028 Uiso 1 1 calc R . .
H10B H 0.2788 0.1466 0.3578 0.028 Uiso 1 1 calc R . .
S1 S 0.74700(6) -0.02506(3) 0.48455(10) 0.01471(18) Uani 1 1 d . . .
S2 S 0.61551(6) -0.06355(3) 0.23299(10) 0.01505(18) Uani 1 1 d . . .
S3 S 0.59685(6) 0.06589(3) 0.47889(10) 0.01488(18) Uani 1 1 d . . .
S4 S 0.47103(6) 0.02166(3) 0.23203(10) 0.01499(18) Uani 1 1 d . . .
S5 S 0.89120(7) -0.10167(3) 0.50030(10) 0.0197(2) Uani 1 1 d . . .
S6 S 0.73622(7) -0.14731(3) 0.19371(10) 0.01747(19) Uani 1 1 d . . .
S7 S 0.49327(8) 0.15418(3) 0.45630(11) 0.0217(2) Uani 1 1 d . . .
S8 S 0.34401(7) 0.10082(3) 0.15780(10) 0.0201(2) Uani 1 1 d . . .
C11 C 0.8460(4) 0.2500 0.5966(6) 0.0178(9) Uani 1 2 d S . .
C12 C 0.9736(4) 0.2500 0.7877(6) 0.0179(9) Uani 1 2 d S . .
N1 N 0.7644(3) 0.2500 0.5390(5) 0.0211(9) Uani 1 2 d S . .
N2 N 0.9421(3) 0.2500 0.6414(5) 0.0249(9) Uani 1 2 d S . .
N3 N 1.0165(3) 0.2500 0.9088(5) 0.0190(8) Uani 1 2 d S . .
Cu1 Cu 0.62724(5) 0.2500 0.43438(7) 0.01853(16) Uani 1 2 d S . .
Cl1 Cl 0.64037(7) 0.2500 0.16833(10) 0.00733(19) Uani 1 2 d S . .


_geom_special_details            
; 
 The positional parameters of the hydrogen atoms were calculated under a 
 fixed C-H bond length of 1.00 A with sp2 configuration of the 
 bonding carbon atoms. In the refinement procedures, isotropic temperature
 factors with the magnitude of 1.2 fold to those of the equivalent
 temperature factors of the bonding carbon atoms were applied for hydrogen
 atoms.

 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 1.362(4) . ?
C1 S2 1.740(3) . ?
C1 S1 1.741(3) . ?
C2 S3 1.739(3) . ?
C2 S4 1.743(3) . ?
C3 C4 1.349(4) . ?
C3 S5 1.746(3) . ?
C3 S1 1.753(3) . ?
C4 S2 1.748(3) . ?
C4 S6 1.749(3) . ?
C5 C6 1.350(5) . ?
C5 S7 1.746(3) . ?
C5 S3 1.748(3) . ?
C6 S8 1.741(3) . ?
C6 S4 1.750(3) . ?
C7 C8 1.512(5) . ?
C7 S5 1.807(4) . ?
C7 H7A 1.0000 . ?
C7 H7B 1.0000 . ?
C8 S6 1.810(3) . ?
C8 H8A 1.0000 . ?
C8 H8B 1.0000 . ?
C9A C10A 1.513(5) . ?
C9A S7 1.825(4) . ?
C9A H9A 1.0000 . ?
C9A H9B 1.0000 . ?
C10A S8 1.795(4) . ?
C10A H10A 1.0000 . ?
C10A H10B 1.0000 . ?
C11 N1 1.159(7) . ?
C11 N2 1.294(7) . ?
C12 N3 1.159(7) . ?
C12 N2 1.296(7) . ?
N1 Cu1 1.974(4) . ?
N3 Cu1 1.944(4) 6_657 ?
Cu1 N3 1.944(4) 6_557 ?
Cu1 Cl1 2.2455(11) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 C1 S2 120.5(2) . . ?
C2 C1 S1 124.2(2) . . ?
S2 C1 S1 115.30(18) . . ?
C1 C2 S3 124.0(2) . . ?
C1 C2 S4 120.7(2) . . ?
S3 C2 S4 115.35(18) . . ?
C4 C3 S5 128.6(3) . . ?
C4 C3 S1 117.4(2) . . ?
S5 C3 S1 113.93(18) . . ?
C3 C4 S2 116.7(2) . . ?
C3 C4 S6 128.6(3) . . ?
S2 C4 S6 114.69(18) . . ?
C6 C5 S7 128.4(3) . . ?
C6 C5 S3 117.1(2) . . ?
S7 C5 S3 114.50(19) . . ?
C5 C6 S8 129.2(3) . . ?
C5 C6 S4 117.1(2) . . ?
S8 C6 S4 113.75(18) . . ?
C8 C7 S5 115.0(2) . . ?
C8 C7 H7A 108.5 . . ?
S5 C7 H7A 108.5 . . ?
C8 C7 H7B 108.5 . . ?
S5 C7 H7B 108.5 . . ?
H7A C7 H7B 107.5 . . ?
C7 C8 S6 113.6(2) . . ?
C7 C8 H8A 108.8 . . ?
S6 C8 H8A 108.8 . . ?
C7 C8 H8B 108.8 . . ?
S6 C8 H8B 108.8 . . ?
H8A C8 H8B 107.7 . . ?
C10A C9A S7 114.0(3) . . ?
C10A C9A H9A 108.7 . . ?
S7 C9A H9A 108.7 . . ?
C10A C9A H9B 108.7 . . ?
S7 C9A H9B 108.7 . . ?
H9A C9A H9B 107.6 . . ?
C9A C10A S8 114.2(3) . . ?
C9A C10A H10A 108.7 . . ?
S8 C10A H10A 108.7 . . ?
C9A C10A H10B 108.7 . . ?
S8 C10A H10B 108.7 . . ?
H10A C10A H10B 107.6 . . ?
C1 S1 C3 95.02(15) . . ?
C1 S2 C4 95.55(15) . . ?
C2 S3 C5 95.06(15) . . ?
C2 S4 C6 94.91(15) . . ?
C3 S5 C7 102.22(16) . . ?
C4 S6 C8 100.20(15) . . ?
C5 S7 C9A 100.79(17) . . ?
C6 S8 C10A 101.55(17) . . ?
N1 C11 N2 172.2(5) . . ?
N3 C12 N2 169.8(5) . . ?
C11 N1 Cu1 178.2(4) . . ?
C11 N2 C12 125.2(5) . . ?
C12 N3 Cu1 161.2(4) . 6_657 ?
N3 Cu1 N1 110.73(18) 6_557 . ?
N3 Cu1 Cl1 137.09(13) 6_557 . ?
N1 Cu1 Cl1 112.18(13) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
S2 C1 C2 S3 -178.89(18) . . . . ?
S1 C1 C2 S3 1.3(4) . . . . ?
S2 C1 C2 S4 0.9(4) . . . . ?
S1 C1 C2 S4 -178.92(18) . . . . ?
S5 C3 C4 S2 178.1(2) . . . . ?
S1 C3 C4 S2 -0.4(4) . . . . ?
S5 C3 C4 S6 -1.7(5) . . . . ?
S1 C3 C4 S6 179.74(19) . . . . ?
S7 C5 C6 S8 0.6(5) . . . . ?
S3 C5 C6 S8 -178.1(2) . . . . ?
S7 C5 C6 S4 179.02(19) . . . . ?
S3 C5 C6 S4 0.4(4) . . . . ?
S5 C7 C8 S6 68.7(3) . . . . ?
S7 C9A C10A S8 -69.5(3) . . . . ?
C2 C1 S1 C3 -178.6(3) . . . . ?
S2 C1 S1 C3 1.6(2) . . . . ?
C4 C3 S1 C1 -0.7(3) . . . . ?
S5 C3 S1 C1 -179.45(19) . . . . ?
C2 C1 S2 C4 178.4(3) . . . . ?
S1 C1 S2 C4 -1.8(2) . . . . ?
C3 C4 S2 C1 1.3(3) . . . . ?
S6 C4 S2 C1 -178.82(19) . . . . ?
C1 C2 S3 C5 172.6(3) . . . . ?
S4 C2 S3 C5 -7.2(2) . . . . ?
C6 C5 S3 C2 4.1(3) . . . . ?
S7 C5 S3 C2 -174.72(19) . . . . ?
C1 C2 S4 C6 -172.5(3) . . . . ?
S3 C2 S4 C6 7.4(2) . . . . ?
C5 C6 S4 C2 -4.6(3) . . . . ?
S8 C6 S4 C2 174.04(19) . . . . ?
C4 C3 S5 C7 8.5(4) . . . . ?
S1 C3 S5 C7 -172.96(19) . . . . ?
C8 C7 S5 C3 -41.7(3) . . . . ?
C3 C4 S6 C8 19.6(4) . . . . ?
S2 C4 S6 C8 -160.19(19) . . . . ?
C7 C8 S6 C4 -51.9(3) . . . . ?
C6 C5 S7 C9A -14.2(4) . . . . ?
S3 C5 S7 C9A 164.5(2) . . . . ?
C10A C9A S7 C5 47.7(3) . . . . ?
C5 C6 S8 C10A -12.8(4) . . . . ?
S4 C6 S8 C10A 168.72(19) . . . . ?
C9A C10A S8 C6 46.6(3) . . . . ?
N2 C11 N1 Cu1 0.00(2) . . . . ?
N1 C11 N2 C12 180.000(6) . . . . ?
N3 C12 N2 C11 180.000(6) . . . . ?
N2 C12 N3 Cu1 0.006(7) . . . 6_657 ?
C11 N1 Cu1 N3 180.002(19) . . . 6_557 ?
C11 N1 Cu1 Cl1 0.000(19) . . . . ?

_diffrn_measured_fraction_theta_max 0.985
_diffrn_reflns_theta_full        27.49
_diffrn_measured_fraction_theta_full 0.985
_refine_diff_density_max         3.446
_refine_diff_density_min         -0.748
_refine_diff_density_rms         0.143

_exptl_crystal_recrystallization_method electrocrystallization
_exptl_crystal_preparation       'Magnetic properties, electronic property'
####################################################################### 
# 
# 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/. 
# 
# Audit and citation data items have may 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_kappa-(ET)2Cu[N(CN)2]Cl-150K
_database_code_depnum_ccdc_archive 'CCDC 1016186'
_audit_update_record             
;
2014-07-26 deposited with the CCDC.
2014-11-27 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            (ET)2Cu[N(CN)2]Cl
_chemical_formula_moiety         '2(C10 H8 S8), (C2 Cl1 Cu1 N3)'
_chemical_formula_sum            'C22 H16 Cl1 Cu1 N3 S16'
_chemical_formula_weight         934.44

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   'Pnma '
_symmetry_space_group_name_Hall  '-P 2ac 2n'

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

_cell_length_a                   12.8917(7)
_cell_length_b                   29.6686(17)
_cell_length_c                   8.4335(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     3225.6(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    9976
_cell_measurement_theta_min      2.51
_cell_measurement_theta_max      28.08

_exptl_crystal_description       'elongate block'
_exptl_crystal_colour            black
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.16
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.924
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1884
_exptl_absorpt_coefficient_mu    1.822
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.5933
_exptl_absorpt_correction_T_max  0.7592
_exptl_absorpt_process_details   
;
APEX2 Software
;
_exptl_special_details           
; 
 kappa polymorph
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean 8.333
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            16932
_diffrn_reflns_av_R_equivalents  0.0108
_diffrn_reflns_av_sigmaI/netI    0.0089
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_theta_min         1.37
_diffrn_reflns_theta_max         27.49
_reflns_number_total             3709
_reflns_number_gt                3483
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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)+(0.0712P)²+12.6248P] 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         3709
_refine_ls_number_parameters     205
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0444
_refine_ls_R_factor_gt           0.0422
_refine_ls_wR_factor_ref         0.1307
_refine_ls_wR_factor_gt          0.1280
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_restrained_S_all      1.071
_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
C1 C 0.6398(2) -0.01843(11) 0.3600(4) 0.0184(6) Uani 1 1 d . . .
C2 C 0.5780(2) 0.01874(11) 0.3586(4) 0.0179(6) Uani 1 1 d . . .
C3 C 0.7809(3) -0.07826(11) 0.4098(4) 0.0194(6) Uani 1 1 d . . .
C4 C 0.7210(3) -0.09579(11) 0.2940(4) 0.0184(6) Uani 1 1 d . . .
C5 C 0.5018(3) 0.09842(11) 0.3886(4) 0.0190(6) Uani 1 1 d . A .
C6 C 0.4442(3) 0.07840(11) 0.2752(4) 0.0186(6) Uani 1 1 d . A .
C7 C 0.9130(3) -0.15098(14) 0.3800(5) 0.0297(8) Uani 1 1 d . . .
H7A H 0.9501 -0.1412 0.2817 0.036 Uiso 1 1 calc R . .
H7B H 0.9603 -0.1717 0.4391 0.036 Uiso 1 1 calc R . .
C8 C 0.8176(3) -0.17692(12) 0.3320(4) 0.0270(8) Uani 1 1 d . . .
H8A H 0.7768 -0.1844 0.4294 0.032 Uiso 1 1 calc R . .
H8B H 0.8396 -0.2060 0.2823 0.032 Uiso 1 1 calc R . .
C9A C 0.4165(4) 0.17958(14) 0.3004(5) 0.0354(9) Uani 1 1 d . A 1
H9A H 0.3953 0.2104 0.3358 0.042 Uiso 1 1 calc R A 1
H9B H 0.4603 0.1832 0.2033 0.042 Uiso 1 1 calc R A 1
C10A C 0.3207(3) 0.15354(14) 0.2569(6) 0.0356(9) Uani 1 1 d . A 1
H10A H 0.2767 0.1727 0.1862 0.043 Uiso 1 1 calc R A 1
H10B H 0.2801 0.1474 0.3556 0.043 Uiso 1 1 calc R A 1
S1 S 0.74652(6) -0.02526(3) 0.48434(10) 0.01980(19) Uani 1 1 d . . .
S2 S 0.61543(7) -0.06326(3) 0.23250(10) 0.02031(19) Uani 1 1 d . . .
S3 S 0.59788(6) 0.06563(3) 0.47864(10) 0.01979(19) Uani 1 1 d . . .
S4 S 0.47166(7) 0.02207(3) 0.23201(10) 0.02020(19) Uani 1 1 d . . .
S5 S 0.88923(7) -0.10207(3) 0.50111(12) 0.0280(2) Uani 1 1 d . . .
S6 S 0.73452(7) -0.14717(3) 0.19488(11) 0.0241(2) Uani 1 1 d . . .
S7 S 0.49561(9) 0.15391(3) 0.45623(12) 0.0301(2) Uani 1 1 d . . .
S8 S 0.34543(8) 0.10119(3) 0.15908(11) 0.0278(2) Uani 1 1 d . . .
C11 C 0.8478(4) 0.2500 0.5983(6) 0.0230(10) Uani 1 2 d S . .
C12 C 0.9755(4) 0.2500 0.7884(6) 0.0232(10) Uani 1 2 d S . .
N1 N 0.7666(4) 0.2500 0.5404(6) 0.0278(9) Uani 1 2 d S . .
N2 N 0.9436(4) 0.2500 0.6428(6) 0.0339(11) Uani 1 2 d S . .
N3 N 1.0188(3) 0.2500 0.9086(6) 0.0250(9) Uani 1 2 d S . .
Cu1 Cu 0.62967(5) 0.2500 0.43487(8) 0.02507(18) Uani 1 2 d S . .
Cl1 Cl 0.64210(8) 0.2500 0.16966(11) 0.0157(2) Uani 1 2 d S . .


_geom_special_details            
; 
 The positional parameters of the hydrogen atoms were calculated under a 
 fixed C-H bond length of 1.00 A with sp2 configuration of the 
 bonding carbon atoms. In the refinement procedures, isotropic temperature
 factors with the magnitude of 1.2 fold to those of the equivalent
 temperature factors of the bonding carbon atoms were applied for hydrogen
 atoms.

 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 1.361(5) . ?
C1 S2 1.739(3) . ?
C1 S1 1.741(3) . ?
C2 S3 1.740(3) . ?
C2 S4 1.740(3) . ?
C3 C4 1.350(5) . ?
C3 S5 1.744(3) . ?
C3 S1 1.750(3) . ?
C4 S2 1.747(3) . ?
C4 S6 1.747(3) . ?
C5 C6 1.349(5) . ?
C5 S7 1.744(3) . ?
C5 S3 1.749(3) . ?
C6 S8 1.743(3) . ?
C6 S4 1.747(3) . ?
C7 C8 1.506(6) . ?
C7 S5 1.801(4) . ?
C7 H7A 1.0000 . ?
C7 H7B 1.0000 . ?
C8 S6 1.807(4) . ?
C8 H8A 1.0000 . ?
C8 H8B 1.0000 . ?
C9A C10A 1.502(6) . ?
C9A S7 1.829(4) . ?
C9A H9A 1.0000 . ?
C9A H9B 1.0000 . ?
C10A S8 1.787(4) . ?
C10A H10A 1.0000 . ?
C10A H10B 1.0000 . ?
C11 N1 1.156(7) . ?
C11 N2 1.291(7) . ?
C12 N3 1.158(7) . ?
C12 N2 1.294(7) . ?
N1 Cu1 1.977(5) . ?
N3 Cu1 1.945(4) 6_657 ?
Cu1 N3 1.945(4) 6_557 ?
Cu1 Cl1 2.2423(11) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 C1 S2 120.5(3) . . ?
C2 C1 S1 124.2(3) . . ?
S2 C1 S1 115.24(19) . . ?
C1 C2 S3 123.8(3) . . ?
C1 C2 S4 120.9(3) . . ?
S3 C2 S4 115.32(18) . . ?
C4 C3 S5 128.4(3) . . ?
C4 C3 S1 117.5(3) . . ?
S5 C3 S1 114.09(19) . . ?
C3 C4 S2 116.6(3) . . ?
C3 C4 S6 128.7(3) . . ?
S2 C4 S6 114.70(18) . . ?
C6 C5 S7 128.5(3) . . ?
C6 C5 S3 116.9(2) . . ?
S7 C5 S3 114.55(19) . . ?
C5 C6 S8 129.0(3) . . ?
C5 C6 S4 117.2(3) . . ?
S8 C6 S4 113.72(19) . . ?
C8 C7 S5 115.2(3) . . ?
C8 C7 H7A 108.5 . . ?
S5 C7 H7A 108.5 . . ?
C8 C7 H7B 108.5 . . ?
S5 C7 H7B 108.5 . . ?
H7A C7 H7B 107.5 . . ?
C7 C8 S6 114.0(3) . . ?
C7 C8 H8A 108.8 . . ?
S6 C8 H8A 108.8 . . ?
C7 C8 H8B 108.8 . . ?
S6 C8 H8B 108.8 . . ?
H8A C8 H8B 107.7 . . ?
C10A C9A S7 114.8(3) . . ?
C10A C9A H9A 108.6 . . ?
S7 C9A H9A 108.6 . . ?
C10A C9A H9B 108.6 . . ?
S7 C9A H9B 108.6 . . ?
H9A C9A H9B 107.5 . . ?
C9A C10A S8 114.4(3) . . ?
C9A C10A H10A 108.7 . . ?
S8 C10A H10A 108.7 . . ?
C9A C10A H10B 108.7 . . ?
S8 C10A H10B 108.7 . . ?
H10A C10A H10B 107.6 . . ?
C1 S1 C3 95.06(16) . . ?
C1 S2 C4 95.62(16) . . ?
C2 S3 C5 95.03(16) . . ?
C2 S4 C6 94.95(16) . . ?
C3 S5 C7 102.25(17) . . ?
C4 S6 C8 100.34(16) . . ?
C5 S7 C9A 100.58(18) . . ?
C6 S8 C10A 102.01(19) . . ?
N1 C11 N2 171.9(6) . . ?
N3 C12 N2 169.7(5) . . ?
C11 N1 Cu1 178.3(4) . . ?
C11 N2 C12 125.4(5) . . ?
C12 N3 Cu1 161.6(4) . 6_657 ?
N3 Cu1 N1 110.53(19) 6_557 . ?
N3 Cu1 Cl1 136.82(14) 6_557 . ?
N1 Cu1 Cl1 112.65(14) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
S2 C1 C2 S3 -178.61(19) . . . . ?
S1 C1 C2 S3 1.3(5) . . . . ?
S2 C1 C2 S4 1.1(4) . . . . ?
S1 C1 C2 S4 -178.96(19) . . . . ?
S5 C3 C4 S2 178.4(2) . . . . ?
S1 C3 C4 S2 -0.2(4) . . . . ?
S5 C3 C4 S6 -1.8(5) . . . . ?
S1 C3 C4 S6 179.6(2) . . . . ?
S7 C5 C6 S8 0.2(5) . . . . ?
S3 C5 C6 S8 -178.2(2) . . . . ?
S7 C5 C6 S4 178.7(2) . . . . ?
S3 C5 C6 S4 0.3(4) . . . . ?
S5 C7 C8 S6 68.4(4) . . . . ?
S7 C9A C10A S8 -68.5(4) . . . . ?
C2 C1 S1 C3 -178.8(3) . . . . ?
S2 C1 S1 C3 1.2(2) . . . . ?
C4 C3 S1 C1 -0.6(3) . . . . ?
S5 C3 S1 C1 -179.4(2) . . . . ?
C2 C1 S2 C4 178.7(3) . . . . ?
S1 C1 S2 C4 -1.2(2) . . . . ?
C3 C4 S2 C1 0.8(3) . . . . ?
S6 C4 S2 C1 -179.0(2) . . . . ?
C1 C2 S3 C5 172.7(3) . . . . ?
S4 C2 S3 C5 -7.0(2) . . . . ?
C6 C5 S3 C2 4.0(3) . . . . ?
S7 C5 S3 C2 -174.5(2) . . . . ?
C1 C2 S4 C6 -172.6(3) . . . . ?
S3 C2 S4 C6 7.2(2) . . . . ?
C5 C6 S4 C2 -4.5(3) . . . . ?
S8 C6 S4 C2 174.24(19) . . . . ?
C4 C3 S5 C7 9.2(4) . . . . ?
S1 C3 S5 C7 -172.2(2) . . . . ?
C8 C7 S5 C3 -42.2(3) . . . . ?
C3 C4 S6 C8 18.9(4) . . . . ?
S2 C4 S6 C8 -161.4(2) . . . . ?
C7 C8 S6 C4 -51.0(3) . . . . ?
C6 C5 S7 C9A -13.8(4) . . . . ?
S3 C5 S7 C9A 164.6(2) . . . . ?
C10A C9A S7 C5 47.3(4) . . . . ?
C5 C6 S8 C10A -12.1(4) . . . . ?
S4 C6 S8 C10A 169.4(2) . . . . ?
C9A C10A S8 C6 45.5(4) . . . . ?
N2 C11 N1 Cu1 0.00(3) . . . . ?
N1 C11 N2 C12 180.000(6) . . . . ?
N3 C12 N2 C11 180.000(6) . . . . ?
N2 C12 N3 Cu1 0.011(8) . . . 6_657 ?
C11 N1 Cu1 N3 180.00(2) . . . 6_557 ?
C11 N1 Cu1 Cl1 0.00(2) . . . . ?

_diffrn_measured_fraction_theta_max 0.986
_diffrn_reflns_theta_full        27.49
_diffrn_measured_fraction_theta_full 0.986
_refine_diff_density_max         3.096
_refine_diff_density_min         -0.721
_refine_diff_density_rms         0.137

_exptl_crystal_recrystallization_method electrocrystallization
_exptl_crystal_preparation       'Magnetic properties, electronic property'
####################################################################### 
# 
# 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/. 
# 
# Audit and citation data items have may 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_kappa-(ET)2Cu[N(CN)2]Cl-200K
_database_code_depnum_ccdc_archive 'CCDC 1016187'
_audit_update_record             
;
2014-07-26 deposited with the CCDC.
2014-11-27 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            (ET)2Cu[N(CN)2]Cl
_chemical_formula_moiety         '2(C10 H8 S8), (C2 Cl1 Cu1 N3)'
_chemical_formula_sum            'C22 H16 Cl1 Cu1 N3 S16'
_chemical_formula_weight         934.44

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   'Pnma '
_symmetry_space_group_name_Hall  '-P 2ac 2n'

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

_cell_length_a                   12.9062(7)
_cell_length_b                   29.7595(16)
_cell_length_c                   8.4509(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     3245.8(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    200(2)
_cell_measurement_reflns_used    9910
_cell_measurement_theta_min      2.51
_cell_measurement_theta_max      28.04

_exptl_crystal_description       'elongate block'
_exptl_crystal_colour            black
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.16
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.912
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1884
_exptl_absorpt_coefficient_mu    1.811
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.5950
_exptl_absorpt_correction_T_max  0.7605
_exptl_absorpt_process_details   
;
APEX2 Software
;
_exptl_special_details           
; 
 kappa polymorph
;

_diffrn_ambient_temperature      200(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEXII CCD area detector'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean 8.333
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            17091
_diffrn_reflns_av_R_equivalents  0.0120
_diffrn_reflns_av_sigmaI/netI    0.0097
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_theta_min         1.37
_diffrn_reflns_theta_max         27.50
_reflns_number_total             3734
_reflns_number_gt                3448
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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)+(0.0706P)²+11.0319P] 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         3734
_refine_ls_number_parameters     224
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0452
_refine_ls_R_factor_gt           0.0420
_refine_ls_wR_factor_ref         0.1303
_refine_ls_wR_factor_gt          0.1258
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_restrained_S_all      1.049
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.6397(2) -0.01843(11) 0.3601(4) 0.0225(6) Uani 1 1 d . . .
C2 C 0.5783(2) 0.01871(10) 0.3583(4) 0.0223(6) Uani 1 1 d . . .
C3 C 0.7796(2) -0.07845(11) 0.4103(4) 0.0246(6) Uani 1 1 d . . .
C4 C 0.7199(2) -0.09567(11) 0.2943(4) 0.0230(6) Uani 1 1 d . . .
C5 C 0.5034(3) 0.09831(10) 0.3884(4) 0.0237(6) Uani 1 1 d . A .
C6 C 0.4455(3) 0.07853(11) 0.2754(4) 0.0235(6) Uani 1 1 d . A .
C7 C 0.9112(3) -0.15080(14) 0.3792(5) 0.0382(9) Uani 1 1 d . . .
H7A H 0.9480 -0.1407 0.2813 0.046 Uiso 1 1 calc R . .
H7B H 0.9587 -0.1716 0.4374 0.046 Uiso 1 1 calc R . .
C8 C 0.8164(3) -0.17664(12) 0.3310(4) 0.0341(8) Uani 1 1 d . . .
H8A H 0.7760 -0.1844 0.4282 0.041 Uiso 1 1 calc R . .
H8B H 0.8387 -0.2054 0.2804 0.041 Uiso 1 1 calc R . .
C9A C 0.4187(4) 0.17944(15) 0.2997(8) 0.0365(15) Uani 0.869(15) 1 d P A 1
H9A H 0.3977 0.2102 0.3350 0.044 Uiso 0.869(15) 1 calc PR A 1
H9B H 0.4623 0.1829 0.2027 0.044 Uiso 0.869(15) 1 calc PR A 1
C10A C 0.3225(5) 0.15353(18) 0.2565(7) 0.0367(15) Uani 0.869(15) 1 d P A 1
H10A H 0.2787 0.1726 0.1858 0.044 Uiso 0.869(15) 1 calc PR A 1
H10B H 0.2820 0.1476 0.3551 0.044 Uiso 0.869(15) 1 calc PR A 1
C9B C 0.389(2) 0.1740(9) 0.388(4) 0.023(8) Uani 0.131(15) 1 d P A 2
H9C H 0.3303 0.1602 0.4482 0.028 Uiso 0.131(15) 1 calc PR A 2
H9D H 0.3877 0.2071 0.4081 0.028 Uiso 0.131(15) 1 calc PR A 2
C10B C 0.374(3) 0.1656(9) 0.217(3) 0.022(8) Uani 0.131(15) 1 d P A 2
H10C H 0.4376 0.1759 0.1594 0.027 Uiso 0.131(15) 1 calc PR A 2
H10D H 0.3148 0.1843 0.1793 0.027 Uiso 0.131(15) 1 calc PR A 2
S1 S 0.74598(6) -0.02543(3) 0.48398(10) 0.0252(2) Uani 1 1 d . . .
S2 S 0.61527(7) -0.06304(3) 0.23207(10) 0.0257(2) Uani 1 1 d . . .
S3 S 0.59882(6) 0.06540(3) 0.47809(10) 0.02505(19) Uani 1 1 d . . .
S4 S 0.47224(7) 0.02240(3) 0.23202(10) 0.0257(2) Uani 1 1 d . . .
S5 S 0.88740(8) -0.10235(3) 0.50173(12) 0.0365(2) Uani 1 1 d . . .
S6 S 0.73298(7) -0.14702(3) 0.19602(11) 0.0311(2) Uani 1 1 d . . .
S7 S 0.49789(9) 0.15364(3) 0.45598(12) 0.0384(3) Uani 1 1 d . . .
S8 S 0.34691(8) 0.10154(3) 0.16007(12) 0.0356(2) Uani 1 1 d . . .
C11 C 0.8495(4) 0.2500 0.5999(6) 0.0285(10) Uani 1 2 d S . .
C12 C 0.9774(4) 0.2500 0.7891(7) 0.0286(10) Uani 1 2 d S . .
N1 N 0.7686(4) 0.2500 0.5420(6) 0.0349(10) Uani 1 2 d S . .
N2 N 0.9454(4) 0.2500 0.6440(6) 0.0443(12) Uani 1 2 d S . .
N3 N 1.0209(3) 0.2500 0.9086(6) 0.0313(9) Uani 1 2 d S . .
Cu1 Cu 0.63209(5) 0.2500 0.43551(8) 0.03191(18) Uani 1 2 d S . .
Cl1 Cl 0.64390(9) 0.2500 0.17111(12) 0.0242(2) Uani 1 2 d S . .


_geom_special_details            
; 
 The positional parameters of the hydrogen atoms were calculated under a 
 fixed C-H bond length of 1.00 A with sp2 configuration of the 
 bonding carbon atoms. In the refinement procedures, isotropic temperature
 factors with the magnitude of 1.2 fold to those of the equivalent
 temperature factors of the bonding carbon atoms were applied for hydrogen
 atoms.

 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 1.360(5) . ?
C1 S1 1.738(3) . ?
C1 S2 1.741(3) . ?
C2 S4 1.739(3) . ?
C2 S3 1.739(3) . ?
C3 C4 1.348(5) . ?
C3 S5 1.743(3) . ?
C3 S1 1.751(3) . ?
C4 S2 1.745(3) . ?
C4 S6 1.747(3) . ?
C5 C6 1.348(5) . ?
C5 S7 1.744(3) . ?
C5 S3 1.747(3) . ?
C6 S8 1.743(3) . ?
C6 S4 1.744(3) . ?
C7 C8 1.501(6) . ?
C7 S5 1.801(4) . ?
C7 H7A 1.0000 . ?
C7 H7B 1.0000 . ?
C8 S6 1.800(4) . ?
C8 H8A 1.0000 . ?
C8 H8B 1.0000 . ?
C9A C10A 1.506(9) . ?
C9A S7 1.838(5) . ?
C9A H9A 1.0000 . ?
C9A H9B 1.0000 . ?
C10A S8 1.777(4) . ?
C10A H10A 1.0000 . ?
C10A H10B 1.0000 . ?
C9B C10B 1.48(4) . ?
C9B S7 1.63(2) . ?
C9B H9C 1.0000 . ?
C9B H9D 1.0000 . ?
C10B S8 2.00(3) . ?
C10B H10C 1.0000 . ?
C10B H10D 1.0000 . ?
C11 N1 1.152(7) . ?
C11 N2 1.294(7) . ?
C12 N3 1.156(7) . ?
C12 N2 1.293(7) . ?
N1 Cu1 1.979(5) . ?
N3 Cu1 1.948(4) 6_657 ?
Cu1 N3 1.948(5) 6_557 ?
Cu1 Cl1 2.2396(12) . ?

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 S1 124.3(3) . . ?
C2 C1 S2 120.5(3) . . ?
S1 C1 S2 115.20(18) . . ?
C1 C2 S4 121.1(2) . . ?
C1 C2 S3 123.6(3) . . ?
S4 C2 S3 115.26(18) . . ?
C4 C3 S5 128.6(3) . . ?
C4 C3 S1 117.3(3) . . ?
S5 C3 S1 114.08(19) . . ?
C3 C4 S2 116.8(2) . . ?
C3 C4 S6 128.5(3) . . ?
S2 C4 S6 114.72(18) . . ?
C6 C5 S7 128.4(3) . . ?
C6 C5 S3 117.0(2) . . ?
S7 C5 S3 114.58(19) . . ?
C5 C6 S8 129.0(3) . . ?
C5 C6 S4 117.2(3) . . ?
S8 C6 S4 113.77(19) . . ?
C8 C7 S5 115.3(3) . . ?
C8 C7 H7A 108.5 . . ?
S5 C7 H7A 108.5 . . ?
C8 C7 H7B 108.5 . . ?
S5 C7 H7B 108.5 . . ?
H7A C7 H7B 107.5 . . ?
C7 C8 S6 114.1(3) . . ?
C7 C8 H8A 108.7 . . ?
S6 C8 H8A 108.7 . . ?
C7 C8 H8B 108.7 . . ?
S6 C8 H8B 108.7 . . ?
H8A C8 H8B 107.6 . . ?
C10A C9A S7 114.7(4) . . ?
C10A C9A H9A 108.6 . . ?
S7 C9A H9A 108.6 . . ?
C10A C9A H9B 108.6 . . ?
S7 C9A H9B 108.6 . . ?
H9A C9A H9B 107.6 . . ?
C9A C10A S8 114.3(4) . . ?
C9A C10A H10A 108.7 . . ?
S8 C10A H10A 108.7 . . ?
C9A C10A H10B 108.7 . . ?
S8 C10A H10B 108.7 . . ?
H10A C10A H10B 107.6 . . ?
C10B C9B S7 113(2) . . ?
C10B C9B H9C 109.0 . . ?
S7 C9B H9C 109.0 . . ?
C10B C9B H9D 109.0 . . ?
S7 C9B H9D 109.0 . . ?
H9C C9B H9D 107.8 . . ?
C9B C10B S8 115(2) . . ?
C9B C10B H10C 108.6 . . ?
S8 C10B H10C 108.6 . . ?
C9B C10B H10D 108.6 . . ?
S8 C10B H10D 108.6 . . ?
H10C C10B H10D 107.5 . . ?
C1 S1 C3 95.14(16) . . ?
C1 S2 C4 95.56(15) . . ?
C2 S3 C5 95.04(16) . . ?
C2 S4 C6 95.00(16) . . ?
C3 S5 C7 101.99(17) . . ?
C4 S6 C8 100.65(16) . . ?
C9B S7 C5 105.7(9) . . ?
C9B S7 C9A 27.8(12) . . ?
C5 S7 C9A 100.5(2) . . ?
C6 S8 C10A 102.4(2) . . ?
C6 S8 C10B 96.4(8) . . ?
C10A S8 C10B 24.4(9) . . ?
N1 C11 N2 171.6(6) . . ?
N3 C12 N2 169.6(5) . . ?
C11 N1 Cu1 178.1(5) . . ?
C12 N2 C11 125.4(5) . . ?
C12 N3 Cu1 161.6(4) . 6_657 ?
N3 Cu1 N1 110.4(2) 6_557 . ?
N3 Cu1 Cl1 136.47(15) 6_557 . ?
N1 Cu1 Cl1 113.16(15) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
S1 C1 C2 S4 -179.03(18) . . . . ?
S2 C1 C2 S4 1.4(4) . . . . ?
S1 C1 C2 S3 1.3(5) . . . . ?
S2 C1 C2 S3 -178.28(18) . . . . ?
S5 C3 C4 S2 178.6(2) . . . . ?
S1 C3 C4 S2 -0.4(4) . . . . ?
S5 C3 C4 S6 -1.3(5) . . . . ?
S1 C3 C4 S6 179.6(2) . . . . ?
S7 C5 C6 S8 0.1(5) . . . . ?
S3 C5 C6 S8 -178.4(2) . . . . ?
S7 C5 C6 S4 178.6(2) . . . . ?
S3 C5 C6 S4 0.1(4) . . . . ?
S5 C7 C8 S6 68.4(4) . . . . ?
S7 C9A C10A S8 -68.4(7) . . . . ?
S7 C9B C10B S8 70(3) . . . . ?
C2 C1 S1 C3 -178.9(3) . . . . ?
S2 C1 S1 C3 0.7(2) . . . . ?
C4 C3 S1 C1 -0.2(3) . . . . ?
S5 C3 S1 C1 -179.3(2) . . . . ?
C2 C1 S2 C4 178.8(3) . . . . ?
S1 C1 S2 C4 -0.8(2) . . . . ?
C3 C4 S2 C1 0.7(3) . . . . ?
S6 C4 S2 C1 -179.3(2) . . . . ?
C1 C2 S3 C5 172.7(3) . . . . ?
S4 C2 S3 C5 -7.0(2) . . . . ?
C6 C5 S3 C2 4.1(3) . . . . ?
S7 C5 S3 C2 -174.6(2) . . . . ?
C1 C2 S4 C6 -172.7(3) . . . . ?
S3 C2 S4 C6 7.1(2) . . . . ?
C5 C6 S4 C2 -4.3(3) . . . . ?
S8 C6 S4 C2 174.44(19) . . . . ?
C4 C3 S5 C7 9.5(4) . . . . ?
S1 C3 S5 C7 -171.5(2) . . . . ?
C8 C7 S5 C3 -42.7(4) . . . . ?
C3 C4 S6 C8 17.8(4) . . . . ?
S2 C4 S6 C8 -162.2(2) . . . . ?
C7 C8 S6 C4 -50.2(3) . . . . ?
C10B C9B S7 C5 -49(3) . . . . ?
C10B C9B S7 C9A 33(2) . . . . ?
C6 C5 S7 C9B 14.2(14) . . . . ?
S3 C5 S7 C9B -167.3(14) . . . . ?
C6 C5 S7 C9A -13.8(4) . . . . ?
S3 C5 S7 C9A 164.7(3) . . . . ?
C10A C9A S7 C9B -57(2) . . . . ?
C10A C9A S7 C5 47.3(5) . . . . ?
C5 C6 S8 C10A -12.0(4) . . . . ?
S4 C6 S8 C10A 169.4(3) . . . . ?
C5 C6 S8 C10B 12.0(10) . . . . ?
S4 C6 S8 C10B -166.6(10) . . . . ?
C9A C10A S8 C6 45.5(6) . . . . ?
C9A C10A S8 C10B -32.5(18) . . . . ?
C9B C10B S8 C6 -46(3) . . . . ?
C9B C10B S8 C10A 60(2) . . . . ?
N2 C11 N1 Cu1 0.00(2) . . . . ?
N3 C12 N2 C11 180.000(6) . . . . ?
N1 C11 N2 C12 180.000(5) . . . . ?
N2 C12 N3 Cu1 -0.009(8) . . . 6_657 ?
C11 N1 Cu1 N3 179.997(19) . . . 6_557 ?
C11 N1 Cu1 Cl1 0.000(19) . . . . ?

_diffrn_measured_fraction_theta_max 0.984
_diffrn_reflns_theta_full        27.50
_diffrn_measured_fraction_theta_full 0.984
_refine_diff_density_max         2.765
_refine_diff_density_min         -0.733
_refine_diff_density_rms         0.125

_exptl_crystal_recrystallization_method electrocrystallization
_exptl_crystal_preparation       'Magnetic properties, electronic property'

####################################################################### 
# 
# 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/. 
# 
# Audit and citation data items have may 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_kappa-(ET)2Cu[N(CN)2]Cl-250K
_database_code_depnum_ccdc_archive 'CCDC 1016188'
_audit_update_record             
;
2014-07-26 deposited with the CCDC.
2014-11-27 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            (ET)2Cu[N(CN)2]Cl
_chemical_formula_moiety         '2(C10 H8 S8), (C2 Cl1 Cu1 N3)'
_chemical_formula_sum            'C22 H16 Cl1 Cu1 N3 S16'
_chemical_formula_weight         934.44

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   'Pnma '
_symmetry_space_group_name_Hall  '-P 2ac 2n'

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

_cell_length_a                   12.9262(8)
_cell_length_b                   29.8480(18)
_cell_length_c                   8.4661(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     3266.4(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    250(2)
_cell_measurement_reflns_used    9947
_cell_measurement_theta_min      2.50
_cell_measurement_theta_max      27.97

_exptl_crystal_description       'elongate block'
_exptl_crystal_colour            black
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.16
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.900
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1884
_exptl_absorpt_coefficient_mu    1.799
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.5967
_exptl_absorpt_correction_T_max  0.7617
_exptl_absorpt_process_details   
;
APEX2 Software
;
_exptl_special_details           
; 
 kappa polymorph
;

_diffrn_ambient_temperature      250(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEXII CCD area detector'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean 8.333
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            17201
_diffrn_reflns_av_R_equivalents  0.0122
_diffrn_reflns_av_sigmaI/netI    0.0100
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_theta_min         1.36
_diffrn_reflns_theta_max         27.50
_reflns_number_total             3752
_reflns_number_gt                3386
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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)+(0.0723P)²+10.1073P] 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         3752
_refine_ls_number_parameters     224
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0481
_refine_ls_R_factor_gt           0.0436
_refine_ls_wR_factor_ref         0.1359
_refine_ls_wR_factor_gt          0.1297
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_restrained_S_all      1.042
_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
C1 C 0.6394(3) -0.01842(11) 0.3595(4) 0.0270(7) Uani 1 1 d . . .
C2 C 0.5786(3) 0.01871(11) 0.3579(4) 0.0269(6) Uani 1 1 d . . .
C3 C 0.7783(3) -0.07843(11) 0.4104(4) 0.0300(7) Uani 1 1 d . . .
C4 C 0.7189(3) -0.09553(11) 0.2947(4) 0.0283(7) Uani 1 1 d . . .
C5 C 0.5048(3) 0.09825(11) 0.3882(4) 0.0288(7) Uani 1 1 d . A .
C6 C 0.4465(3) 0.07865(11) 0.2755(4) 0.0284(7) Uani 1 1 d . A .
C7 C 0.9095(3) -0.15050(16) 0.3792(5) 0.0468(10) Uani 1 1 d . . .
H7A H 0.9462 -0.1403 0.2817 0.056 Uiso 1 1 calc R . .
H7B H 0.9571 -0.1712 0.4370 0.056 Uiso 1 1 calc R . .
C8 C 0.8155(4) -0.17630(13) 0.3307(5) 0.0418(9) Uani 1 1 d . . .
H8A H 0.7754 -0.1844 0.4276 0.050 Uiso 1 1 calc R . .
H8B H 0.8381 -0.2049 0.2795 0.050 Uiso 1 1 calc R . .
C9A C 0.4207(5) 0.17923(17) 0.2994(10) 0.0454(18) Uani 0.839(17) 1 d P A 1
H9A H 0.4002 0.2099 0.3348 0.054 Uiso 0.839(17) 1 calc PR A 1
H9B H 0.4643 0.1827 0.2025 0.054 Uiso 0.839(17) 1 calc PR A 1
C10A C 0.3243(6) 0.1537(2) 0.2560(8) 0.0450(17) Uani 0.839(17) 1 d P A 1
H10A H 0.2811 0.1728 0.1848 0.054 Uiso 0.839(17) 1 calc PR A 1
H10B H 0.2834 0.1480 0.3542 0.054 Uiso 0.839(17) 1 calc PR A 1
C9B C 0.392(2) 0.1735(8) 0.387(4) 0.029(7) Uani 0.161(17) 1 d P A 2
H9C H 0.3335 0.1602 0.4480 0.035 Uiso 0.161(17) 1 calc PR A 2
H9D H 0.3912 0.2066 0.4057 0.035 Uiso 0.161(17) 1 calc PR A 2
C10B C 0.375(3) 0.1649(9) 0.216(3) 0.033(7) Uani 0.161(17) 1 d P A 2
H10C H 0.4379 0.1752 0.1568 0.040 Uiso 0.161(17) 1 calc PR A 2
H10D H 0.3155 0.1834 0.1797 0.040 Uiso 0.161(17) 1 calc PR A 2
S1 S 0.74531(7) -0.02553(3) 0.48342(11) 0.0309(2) Uani 1 1 d . . .
S2 S 0.61497(7) -0.06287(3) 0.23195(11) 0.0315(2) Uani 1 1 d . . .
S3 S 0.59966(7) 0.06517(3) 0.47735(11) 0.0307(2) Uani 1 1 d . . .
S4 S 0.47270(7) 0.02266(3) 0.23193(11) 0.0313(2) Uani 1 1 d . . .
S5 S 0.88561(8) -0.10247(4) 0.50191(14) 0.0454(3) Uani 1 1 d . . .
S6 S 0.73153(8) -0.14682(3) 0.19706(12) 0.0386(2) Uani 1 1 d . . .
S7 S 0.50016(10) 0.15339(3) 0.45538(13) 0.0472(3) Uani 1 1 d . . .
S8 S 0.34835(9) 0.10184(4) 0.16098(13) 0.0438(3) Uani 1 1 d . . .
C11 C 0.8515(4) 0.2500 0.6016(7) 0.0348(11) Uani 1 2 d S . .
C12 C 0.9793(4) 0.2500 0.7899(7) 0.0350(11) Uani 1 2 d S . .
N1 N 0.7710(4) 0.2500 0.5436(6) 0.0427(11) Uani 1 2 d S . .
N2 N 0.9467(4) 0.2500 0.6456(7) 0.0558(15) Uani 1 2 d S . .
N3 N 1.0236(4) 0.2500 0.9082(6) 0.0383(10) Uani 1 2 d S . .
Cu1 Cu 0.63482(5) 0.2500 0.43627(9) 0.0394(2) Uani 1 2 d S . .
Cl1 Cl 0.64583(10) 0.2500 0.17268(13) 0.0330(3) Uani 1 2 d S . .


_geom_special_details            
; 
 The positional parameters of the hydrogen atoms were calculated under a 
 fixed C-H bond length of 1.00 A with sp2 configuration of the 
 bonding carbon atoms. In the refinement procedures, isotropic temperature
 factors with the magnitude of 1.2 fold to those of the equivalent
 temperature factors of the bonding carbon atoms were applied for hydrogen
 atoms.

 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 1.359(5) . ?
C1 S1 1.738(3) . ?
C1 S2 1.740(3) . ?
C2 S3 1.738(3) . ?
C2 S4 1.740(3) . ?
C3 C4 1.346(5) . ?
C3 S5 1.743(4) . ?
C3 S1 1.749(3) . ?
C4 S2 1.743(3) . ?
C4 S6 1.747(3) . ?
C5 C6 1.349(5) . ?
C5 S7 1.742(3) . ?
C5 S3 1.746(4) . ?
C6 S8 1.741(4) . ?
C6 S4 1.745(3) . ?
C7 C8 1.496(6) . ?
C7 S5 1.797(4) . ?
C7 H7A 1.0000 . ?
C7 H7B 1.0000 . ?
C8 S6 1.798(4) . ?
C8 H8A 1.0000 . ?
C8 H8B 1.0000 . ?
C9A C10A 1.507(10) . ?
C9A S7 1.842(6) . ?
C9A H9A 1.0000 . ?
C9A H9B 1.0000 . ?
C10A S8 1.772(5) . ?
C10A H10A 1.0000 . ?
C10A H10B 1.0000 . ?
C9B C10B 1.49(4) . ?
C9B S7 1.63(2) . ?
C9B H9C 1.0000 . ?
C9B H9D 1.0000 . ?
C10B S8 1.97(3) . ?
C10B H10C 1.0000 . ?
C10B H10D 1.0000 . ?
C11 N1 1.150(7) . ?
C11 N2 1.287(7) . ?
C12 N3 1.153(7) . ?
C12 N2 1.293(8) . ?
N1 Cu1 1.981(5) . ?
N3 Cu1 1.949(5) 6_657 ?
Cu1 N3 1.949(5) 6_557 ?
Cu1 Cl1 2.2361(13) . ?

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 S1 124.1(3) . . ?
C2 C1 S2 120.7(3) . . ?
S1 C1 S2 115.13(19) . . ?
C1 C2 S3 123.7(3) . . ?
C1 C2 S4 121.1(3) . . ?
S3 C2 S4 115.21(19) . . ?
C4 C3 S5 128.4(3) . . ?
C4 C3 S1 117.4(3) . . ?
S5 C3 S1 114.13(19) . . ?
C3 C4 S2 116.7(3) . . ?
C3 C4 S6 128.6(3) . . ?
S2 C4 S6 114.71(19) . . ?
C6 C5 S7 128.4(3) . . ?
C6 C5 S3 116.9(3) . . ?
S7 C5 S3 114.7(2) . . ?
C5 C6 S8 128.9(3) . . ?
C5 C6 S4 117.2(3) . . ?
S8 C6 S4 113.8(2) . . ?
C8 C7 S5 115.5(3) . . ?
C8 C7 H7A 108.4 . . ?
S5 C7 H7A 108.4 . . ?
C8 C7 H7B 108.4 . . ?
S5 C7 H7B 108.4 . . ?
H7A C7 H7B 107.5 . . ?
C7 C8 S6 114.3(3) . . ?
C7 C8 H8A 108.7 . . ?
S6 C8 H8A 108.7 . . ?
C7 C8 H8B 108.7 . . ?
S6 C8 H8B 108.7 . . ?
H8A C8 H8B 107.6 . . ?
C10A C9A S7 115.1(5) . . ?
C10A C9A H9A 108.5 . . ?
S7 C9A H9A 108.5 . . ?
C10A C9A H9B 108.5 . . ?
S7 C9A H9B 108.5 . . ?
H9A C9A H9B 107.5 . . ?
C9A C10A S8 114.1(5) . . ?
C9A C10A H10A 108.7 . . ?
S8 C10A H10A 108.7 . . ?
C9A C10A H10B 108.7 . . ?
S8 C10A H10B 108.7 . . ?
H10A C10A H10B 107.6 . . ?
C10B C9B S7 114(2) . . ?
C10B C9B H9C 108.7 . . ?
S7 C9B H9C 108.7 . . ?
C10B C9B H9D 108.7 . . ?
S7 C9B H9D 108.7 . . ?
H9C C9B H9D 107.6 . . ?
C9B C10B S8 115(2) . . ?
C9B C10B H10C 108.5 . . ?
S8 C10B H10C 108.5 . . ?
C9B C10B H10D 108.5 . . ?
S8 C10B H10D 108.5 . . ?
H10C C10B H10D 107.5 . . ?
C1 S1 C3 95.11(16) . . ?
C1 S2 C4 95.60(16) . . ?
C2 S3 C5 95.15(16) . . ?
C2 S4 C6 95.03(16) . . ?
C3 S5 C7 102.01(18) . . ?
C4 S6 C8 100.81(17) . . ?
C9B S7 C5 105.2(8) . . ?
C9B S7 C9A 27.4(11) . . ?
C5 S7 C9A 100.4(2) . . ?
C6 S8 C10A 102.8(2) . . ?
C6 S8 C10B 96.8(8) . . ?
C10A S8 C10B 24.4(9) . . ?
N1 C11 N2 171.5(6) . . ?
N3 C12 N2 169.3(6) . . ?
C11 N1 Cu1 178.0(5) . . ?
C11 N2 C12 125.8(6) . . ?
C12 N3 Cu1 162.2(5) . 6_657 ?
N3 Cu1 N1 110.2(2) 6_557 . ?
N3 Cu1 Cl1 136.14(16) 6_557 . ?
N1 Cu1 Cl1 113.64(16) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
S1 C1 C2 S3 1.3(5) . . . . ?
S2 C1 C2 S3 -178.19(19) . . . . ?
S1 C1 C2 S4 -178.96(19) . . . . ?
S2 C1 C2 S4 1.5(4) . . . . ?
S5 C3 C4 S2 178.8(2) . . . . ?
S1 C3 C4 S2 -0.4(4) . . . . ?
S5 C3 C4 S6 -1.2(6) . . . . ?
S1 C3 C4 S6 179.6(2) . . . . ?
S7 C5 C6 S8 0.1(5) . . . . ?
S3 C5 C6 S8 -178.4(2) . . . . ?
S7 C5 C6 S4 178.4(2) . . . . ?
S3 C5 C6 S4 0.0(4) . . . . ?
S5 C7 C8 S6 68.1(4) . . . . ?
S7 C9A C10A S8 -67.9(8) . . . . ?
S7 C9B C10B S8 70(3) . . . . ?
C2 C1 S1 C3 -179.0(3) . . . . ?
S2 C1 S1 C3 0.5(2) . . . . ?
C4 C3 S1 C1 -0.1(3) . . . . ?
S5 C3 S1 C1 -179.4(2) . . . . ?
C2 C1 S2 C4 178.9(3) . . . . ?
S1 C1 S2 C4 -0.7(2) . . . . ?
C3 C4 S2 C1 0.7(3) . . . . ?
S6 C4 S2 C1 -179.4(2) . . . . ?
C1 C2 S3 C5 172.7(3) . . . . ?
S4 C2 S3 C5 -7.0(2) . . . . ?
C6 C5 S3 C2 4.2(3) . . . . ?
S7 C5 S3 C2 -174.5(2) . . . . ?
C1 C2 S4 C6 -172.8(3) . . . . ?
S3 C2 S4 C6 7.0(2) . . . . ?
C5 C6 S4 C2 -4.2(3) . . . . ?
S8 C6 S4 C2 174.5(2) . . . . ?
C4 C3 S5 C7 9.9(4) . . . . ?
S1 C3 S5 C7 -171.0(2) . . . . ?
C8 C7 S5 C3 -43.0(4) . . . . ?
C3 C4 S6 C8 17.1(4) . . . . ?
S2 C4 S6 C8 -162.8(2) . . . . ?
C7 C8 S6 C4 -49.5(3) . . . . ?
C10B C9B S7 C5 -49(3) . . . . ?
C10B C9B S7 C9A 35(2) . . . . ?
C6 C5 S7 C9B 14.0(13) . . . . ?
S3 C5 S7 C9B -167.5(13) . . . . ?
C6 C5 S7 C9A -13.7(4) . . . . ?
S3 C5 S7 C9A 164.9(3) . . . . ?
C10A C9A S7 C9B -56.0(18) . . . . ?
C10A C9A S7 C5 47.1(6) . . . . ?
C5 C6 S8 C10A -12.0(5) . . . . ?
S4 C6 S8 C10A 169.6(4) . . . . ?
C5 C6 S8 C10B 12.0(11) . . . . ?
S4 C6 S8 C10B -166.4(10) . . . . ?
C9A C10A S8 C6 45.1(7) . . . . ?
C9A C10A S8 C10B -32.9(18) . . . . ?
C9B C10B S8 C6 -46(3) . . . . ?
C9B C10B S8 C10A 61(2) . . . . ?
N2 C11 N1 Cu1 0.00(2) . . . . ?
N1 C11 N2 C12 180.000(6) . . . . ?
N3 C12 N2 C11 180.000(7) . . . . ?
N2 C12 N3 Cu1 -0.003(9) . . . 6_657 ?
C11 N1 Cu1 N3 179.999(19) . . . 6_557 ?
C11 N1 Cu1 Cl1 0.000(19) . . . . ?

_diffrn_measured_fraction_theta_max 0.982
_diffrn_reflns_theta_full        27.50
_diffrn_measured_fraction_theta_full 0.982
_refine_diff_density_max         2.500
_refine_diff_density_min         -0.723
_refine_diff_density_rms         0.118

_exptl_crystal_recrystallization_method electrocrystallization
_exptl_crystal_preparation       'Magnetic properties, electronic property'
####################################################################### 
# 
# 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/. 
# 
# Audit and citation data items have may 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_kappa-(ET)2Cu[N(CN)2]Cl-298K
_database_code_depnum_ccdc_archive 'CCDC 1016189'
_audit_update_record             
;
2014-07-26 deposited with the CCDC.
2014-11-27 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            (ET)2Cu[N(CN)2]Cl
_chemical_formula_moiety         '2(C10 H8 S8), (C2 Cl1 Cu1 N3)'
_chemical_formula_sum            'C22 H16 Cl1 Cu1 N3 S16'
_chemical_formula_weight         934.33

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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   'Pnma '
_symmetry_space_group_name_Hall  '-P 2ac 2n'

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

_cell_length_a                   12.9550(8)
_cell_length_b                   29.9368(18)
_cell_length_c                   8.4811(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     3289.2(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    9957
_cell_measurement_theta_min      2.50
_cell_measurement_theta_max      27.91

_exptl_crystal_description       'elongate block'
_exptl_crystal_colour            black
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.16
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.887
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1884
_exptl_absorpt_coefficient_mu    1.787
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.5987
_exptl_absorpt_correction_T_max  0.7631
_exptl_absorpt_process_details   
;
APEX2 Software
;
_exptl_special_details           
; 
 kappa polymorph
;

_diffrn_ambient_temperature      298(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEXII CCD area detector'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean 8.333
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            17329
_diffrn_reflns_av_R_equivalents  0.0136
_diffrn_reflns_av_sigmaI/netI    0.0109
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_theta_min         1.36
_diffrn_reflns_theta_max         27.50
_reflns_number_total             3778
_reflns_number_gt                3298
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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)+(0.0771P)²+8.1667P] 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         3778
_refine_ls_number_parameters     214
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0523
_refine_ls_R_factor_gt           0.0458
_refine_ls_wR_factor_ref         0.1461
_refine_ls_wR_factor_gt          0.1380
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_restrained_S_all      1.067
_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
C1 C 0.6391(3) -0.01841(11) 0.3589(4) 0.0323(7) Uani 1 1 d . . .
C2 C 0.5788(3) 0.01873(11) 0.3574(4) 0.0319(7) Uani 1 1 d . . .
C3 C 0.7772(3) -0.07834(12) 0.4103(4) 0.0353(7) Uani 1 1 d . . .
C4 C 0.7180(3) -0.09538(11) 0.2950(4) 0.0339(7) Uani 1 1 d . . .
C5 C 0.5061(3) 0.09813(11) 0.3874(4) 0.0341(7) Uani 1 1 d . A .
C6 C 0.4478(3) 0.07872(11) 0.2754(4) 0.0333(7) Uani 1 1 d . A .
C7 C 0.9076(4) -0.15027(17) 0.3795(6) 0.0563(12) Uani 1 1 d . . .
H7A H 0.9446 -0.1401 0.2824 0.068 Uiso 1 1 calc R . .
H7B H 0.9549 -0.1709 0.4374 0.068 Uiso 1 1 calc R . .
C8 C 0.8145(4) -0.17589(13) 0.3305(5) 0.0498(10) Uani 1 1 d . . .
H8A H 0.7745 -0.1842 0.4271 0.060 Uiso 1 1 calc R . .
H8B H 0.8373 -0.2042 0.2787 0.060 Uiso 1 1 calc R . .
C9A C 0.4226(5) 0.17889(18) 0.2993(8) 0.0555(18) Uani 0.831(14) 1 d P A 1
H9A H 0.4021 0.2094 0.3352 0.067 Uiso 0.831(14) 1 calc PR A 1
H9B H 0.4661 0.1825 0.2028 0.067 Uiso 0.831(14) 1 calc PR A 1
C10A C 0.3270(5) 0.1538(2) 0.2550(8) 0.0547(18) Uani 0.831(14) 1 d P A 1
H10A H 0.2847 0.1729 0.1829 0.066 Uiso 0.831(14) 1 calc PR A 1
H10B H 0.2853 0.1484 0.3524 0.066 Uiso 0.831(14) 1 calc PR A 1
C9B C 0.3945(16) 0.1737(7) 0.387(3) 0.030(6) Uiso 0.169(14) 1 d P A 2
H9C H 0.3356 0.1603 0.4471 0.036 Uiso 0.169(14) 1 calc PR A 2
H9D H 0.3936 0.2067 0.4065 0.036 Uiso 0.169(14) 1 calc PR A 2
C10B C 0.379(2) 0.1652(8) 0.216(3) 0.034(6) Uiso 0.169(14) 1 d P A 2
H10C H 0.4428 0.1749 0.1581 0.041 Uiso 0.169(14) 1 calc PR A 2
H10D H 0.3207 0.1841 0.1777 0.041 Uiso 0.169(14) 1 calc PR A 2
S1 S 0.74458(7) -0.02560(3) 0.48276(11) 0.0370(2) Uani 1 1 d . . .
S2 S 0.61454(8) -0.06272(3) 0.23189(11) 0.0376(2) Uani 1 1 d . . .
S3 S 0.60042(7) 0.06496(3) 0.47638(11) 0.0366(2) Uani 1 1 d . . .
S4 S 0.47303(8) 0.02290(3) 0.23177(11) 0.0374(2) Uani 1 1 d . . .
S5 S 0.88393(9) -0.10245(4) 0.50167(15) 0.0547(3) Uani 1 1 d . . .
S6 S 0.73010(9) -0.14660(3) 0.19810(13) 0.0470(3) Uani 1 1 d . . .
S7 S 0.50232(11) 0.15313(3) 0.45448(14) 0.0566(3) Uani 1 1 d . . .
S8 S 0.34985(10) 0.10208(4) 0.16165(14) 0.0527(3) Uani 1 1 d . . .
C11 C 0.8531(4) 0.2500 0.6033(7) 0.0421(12) Uani 1 2 d S . .
C12 C 0.9814(4) 0.2500 0.7908(8) 0.0427(13) Uani 1 2 d S . .
N1 N 0.7736(4) 0.2500 0.5458(6) 0.0505(12) Uani 1 2 d S . .
N2 N 0.9481(5) 0.2500 0.6469(7) 0.0698(18) Uani 1 2 d S . .
N3 N 1.0266(4) 0.2500 0.9080(6) 0.0454(11) Uani 1 2 d S . .
Cu1 Cu 0.63788(6) 0.2500 0.43724(9) 0.0478(2) Uani 1 2 d S . .
Cl1 Cl 0.64796(12) 0.2500 0.17425(14) 0.0423(3) Uani 1 2 d S . .


_geom_special_details            
; 
 The positional parameters of the hydrogen atoms were calculated under a 
 fixed C-H bond length of 1.00 A with sp2 configuration of the 
 bonding carbon atoms. In the refinement procedures, isotropic temperature
 factors with the magnitude of 1.2 fold to those of the equivalent
 temperature factors of the bonding carbon atoms were applied for hydrogen
 atoms.

 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 1.359(5) . ?
C1 S1 1.737(4) . ?
C1 S2 1.738(3) . ?
C2 S3 1.736(3) . ?
C2 S4 1.740(4) . ?
C3 C4 1.343(5) . ?
C3 S5 1.742(4) . ?
C3 S1 1.746(4) . ?
C4 S2 1.743(4) . ?
C4 S6 1.747(3) . ?
C5 C6 1.346(5) . ?
C5 S7 1.743(3) . ?
C5 S3 1.746(4) . ?
C6 S8 1.740(4) . ?
C6 S4 1.743(4) . ?
C7 C8 1.489(7) . ?
C7 S5 1.794(5) . ?
C7 H7A 1.0000 . ?
C7 H7B 1.0000 . ?
C8 S6 1.796(4) . ?
C8 H8A 1.0000 . ?
C8 H8B 1.0000 . ?
C9A C10A 1.497(10) . ?
C9A S7 1.842(6) . ?
C9A H9A 1.0000 . ?
C9A H9B 1.0000 . ?
C10A S8 1.765(5) . ?
C10A H10A 1.0000 . ?
C10A H10B 1.0000 . ?
C9B C10B 1.49(3) . ?
C9B S7 1.63(2) . ?
C9B H9C 1.0000 . ?
C9B H9D 1.0000 . ?
C10B S8 1.98(2) . ?
C10B H10C 1.0000 . ?
C10B H10D 1.0000 . ?
C11 N1 1.140(8) . ?
C11 N2 1.286(8) . ?
C12 N3 1.154(8) . ?
C12 N2 1.294(9) . ?
N1 Cu1 1.985(5) . ?
N3 Cu1 1.950(5) 6_657 ?
Cu1 N3 1.950(5) 6_557 ?
Cu1 Cl1 2.2342(14) . ?

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 S1 124.0(3) . . ?
C2 C1 S2 120.9(3) . . ?
S1 C1 S2 115.1(2) . . ?
C1 C2 S3 123.7(3) . . ?
C1 C2 S4 121.1(3) . . ?
S3 C2 S4 115.19(19) . . ?
C4 C3 S5 128.3(3) . . ?
C4 C3 S1 117.5(3) . . ?
S5 C3 S1 114.2(2) . . ?
C3 C4 S2 116.7(3) . . ?
C3 C4 S6 128.6(3) . . ?
S2 C4 S6 114.6(2) . . ?
C6 C5 S7 128.5(3) . . ?
C6 C5 S3 116.9(3) . . ?
S7 C5 S3 114.6(2) . . ?
C5 C6 S8 128.8(3) . . ?
C5 C6 S4 117.3(3) . . ?
S8 C6 S4 113.9(2) . . ?
C8 C7 S5 115.7(3) . . ?
C8 C7 H7A 108.4 . . ?
S5 C7 H7A 108.4 . . ?
C8 C7 H7B 108.4 . . ?
S5 C7 H7B 108.4 . . ?
H7A C7 H7B 107.4 . . ?
C7 C8 S6 114.6(3) . . ?
C7 C8 H8A 108.6 . . ?
S6 C8 H8A 108.6 . . ?
C7 C8 H8B 108.6 . . ?
S6 C8 H8B 108.6 . . ?
H8A C8 H8B 107.6 . . ?
C10A C9A S7 115.7(5) . . ?
C10A C9A H9A 108.4 . . ?
S7 C9A H9A 108.4 . . ?
C10A C9A H9B 108.4 . . ?
S7 C9A H9B 108.4 . . ?
H9A C9A H9B 107.4 . . ?
C9A C10A S8 114.4(5) . . ?
C9A C10A H10A 108.7 . . ?
S8 C10A H10A 108.7 . . ?
C9A C10A H10B 108.7 . . ?
S8 C10A H10B 108.7 . . ?
H10A C10A H10B 107.6 . . ?
C10B C9B S7 113.0(18) . . ?
C10B C9B H9C 109.0 . . ?
S7 C9B H9C 109.0 . . ?
C10B C9B H9D 109.0 . . ?
S7 C9B H9D 109.0 . . ?
H9C C9B H9D 107.8 . . ?
C9B C10B S8 114.5(17) . . ?
C9B C10B H10C 108.6 . . ?
S8 C10B H10C 108.6 . . ?
C9B C10B H10D 108.6 . . ?
S8 C10B H10D 108.6 . . ?
H10C C10B H10D 107.6 . . ?
C1 S1 C3 95.13(17) . . ?
C1 S2 C4 95.57(17) . . ?
C2 S3 C5 95.12(17) . . ?
C2 S4 C6 94.97(17) . . ?
C3 S5 C7 102.10(19) . . ?
C4 S6 C8 100.90(18) . . ?
C9B S7 C5 105.5(7) . . ?
C9B S7 C9A 27.3(8) . . ?
C5 S7 C9A 100.3(2) . . ?
C6 S8 C10A 103.1(2) . . ?
C6 S8 C10B 96.6(7) . . ?
C10A S8 C10B 24.7(7) . . ?
N1 C11 N2 171.4(7) . . ?
N3 C12 N2 168.9(6) . . ?
C11 N1 Cu1 177.7(5) . . ?
C11 N2 C12 126.2(6) . . ?
C12 N3 Cu1 162.8(5) . 6_657 ?
N3 Cu1 N1 110.0(2) 6_557 . ?
N3 Cu1 Cl1 135.67(17) 6_557 . ?
N1 Cu1 Cl1 114.30(17) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
S1 C1 C2 S3 1.4(5) . . . . ?
S2 C1 C2 S3 -178.1(2) . . . . ?
S1 C1 C2 S4 -178.9(2) . . . . ?
S2 C1 C2 S4 1.5(5) . . . . ?
S5 C3 C4 S2 178.8(2) . . . . ?
S1 C3 C4 S2 -0.4(4) . . . . ?
S5 C3 C4 S6 -1.0(6) . . . . ?
S1 C3 C4 S6 179.8(2) . . . . ?
S7 C5 C6 S8 -0.1(6) . . . . ?
S3 C5 C6 S8 -178.6(2) . . . . ?
S7 C5 C6 S4 178.4(2) . . . . ?
S3 C5 C6 S4 -0.1(4) . . . . ?
S5 C7 C8 S6 67.5(5) . . . . ?
S7 C9A C10A S8 -67.0(7) . . . . ?
S7 C9B C10B S8 71(2) . . . . ?
C2 C1 S1 C3 -179.0(3) . . . . ?
S2 C1 S1 C3 0.5(2) . . . . ?
C4 C3 S1 C1 -0.1(3) . . . . ?
S5 C3 S1 C1 -179.4(2) . . . . ?
C2 C1 S2 C4 178.9(3) . . . . ?
S1 C1 S2 C4 -0.7(2) . . . . ?
C3 C4 S2 C1 0.7(3) . . . . ?
S6 C4 S2 C1 -179.5(2) . . . . ?
C1 C2 S3 C5 172.7(3) . . . . ?
S4 C2 S3 C5 -7.0(2) . . . . ?
C6 C5 S3 C2 4.3(3) . . . . ?
S7 C5 S3 C2 -174.4(2) . . . . ?
C1 C2 S4 C6 -172.7(3) . . . . ?
S3 C2 S4 C6 7.0(2) . . . . ?
C5 C6 S4 C2 -4.1(3) . . . . ?
S8 C6 S4 C2 174.6(2) . . . . ?
C4 C3 S5 C7 10.0(4) . . . . ?
S1 C3 S5 C7 -170.9(3) . . . . ?
C8 C7 S5 C3 -42.9(4) . . . . ?
C3 C4 S6 C8 16.5(4) . . . . ?
S2 C4 S6 C8 -163.3(2) . . . . ?
C7 C8 S6 C4 -48.7(4) . . . . ?
C10B C9B S7 C5 -49(2) . . . . ?
C10B C9B S7 C9A 33.2(16) . . . . ?
C6 C5 S7 C9B 14.2(10) . . . . ?
S3 C5 S7 C9B -167.3(10) . . . . ?
C6 C5 S7 C9A -13.3(4) . . . . ?
S3 C5 S7 C9A 165.2(3) . . . . ?
C10A C9A S7 C9B -57.4(16) . . . . ?
C10A C9A S7 C5 46.5(5) . . . . ?
C5 C6 S8 C10A -11.5(5) . . . . ?
S4 C6 S8 C10A 169.9(3) . . . . ?
C5 C6 S8 C10B 12.6(9) . . . . ?
S4 C6 S8 C10B -165.9(8) . . . . ?
C9A C10A S8 C6 44.3(6) . . . . ?
C9A C10A S8 C10B -32.8(17) . . . . ?
C9B C10B S8 C6 -47.0(19) . . . . ?
C9B C10B S8 C10A 60(2) . . . . ?
N2 C11 N1 Cu1 0.00(2) . . . . ?
N1 C11 N2 C12 180.000(6) . . . . ?
N3 C12 N2 C11 180.000(7) . . . . ?
N2 C12 N3 Cu1 -0.010(9) . . . 6_657 ?
C11 N1 Cu1 N3 179.997(18) . . . 6_557 ?
C11 N1 Cu1 Cl1 0.000(18) . . . . ?

_diffrn_measured_fraction_theta_max 0.982
_diffrn_reflns_theta_full        27.50
_diffrn_measured_fraction_theta_full 0.982
_refine_diff_density_max         2.265
_refine_diff_density_min         -0.721
_refine_diff_density_rms         0.113

_exptl_crystal_recrystallization_method electrocrystallization
_exptl_crystal_preparation       'Magnetic properties, electronic property'

