# Electronic Supplementary Material (ESI) for Materials Advances.
# This journal is © The Royal Society of Chemistry 2022

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_No3_Ins_296K
_database_code_depnum_ccdc_archive 'CCDC 2001310'
loop_
_audit_author_name
_audit_author_address
'Toshio Naito'
;Ehime University
Japan
;
_audit_update_record             
;
2020-05-06 deposited with the CCDC.	2021-12-14 downloaded from the CCDC.
;

#==============================================================================
# CHEMICAL DATA

_chemical_formula_sum            'C22 H16 Cu I N3 S16'
_chemical_formula_moiety         'C22 H16 Cu I N3 S16'
_chemical_formula_weight         1025.80
_chemical_melting_point          ?

#==============================================================================
# CRYSTAL DATA
_space_group_crystal_system      orthorhombic
_space_group_name_H-M_alt        'P n m a'
_space_group_name_Hall           '-P 2ac 2n'
_space_group_IT_number           62
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 +X,+Y,+Z
2 1/2+X,1/2-Y,1/2-Z
3 -X,1/2+Y,-Z
4 1/2-X,-Y,1/2+Z
5 -X,-Y,-Z
6 -1/2-X,-1/2+Y,-1/2+Z
7 +X,-1/2-Y,+Z
8 -1/2+X,+Y,-1/2-Z
#------------------------------------------------------------------------------
_cell_length_a                   12.9208(3)
_cell_length_b                   30.2576(7)
_cell_length_c                   8.6412(2)
_cell_angle_alpha                90.0000
_cell_angle_beta                 90.0000
_cell_angle_gamma                90.0000
_cell_volume                     3378.31(13)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    22696
_cell_measurement_theta_min      3.42
_cell_measurement_theta_max      68.30
_cell_measurement_temperature    296
#------------------------------------------------------------------------------
_exptl_crystal_description       plate
_exptl_crystal_colour            black
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_exptl_crystal_density_diffrn    2.017
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2028.00
_exptl_absorpt_coefficient_mu    17.538
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Rigaku, 1995)'
_exptl_absorpt_correction_T_min  0.116
_exptl_absorpt_correction_T_max  0.173

#==============================================================================
# EXPERIMENTAL DATA

_diffrn_ambient_temperature      296
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54187
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean 10.000
_diffrn_reflns_number            36393
_diffrn_reflns_av_unetI/netI     0.0376
_diffrn_reflns_av_R_equivalents  0.0843
_diffrn_reflns_theta_max         68.250
_diffrn_reflns_theta_min         5.324
_diffrn_reflns_theta_full        67.687
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       10
_diffrn_standards_number         0
_diffrn_standards_interval_count .
_diffrn_standards_decay_%        ?
_reflns_number_total             3149
_reflns_number_gt                2587
_reflns_threshold_expression     F²>2.0σ(F²)
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

#==============================================================================
# REFINEMENT DATA

_refine_special_details          
;
    Refinement was performed using all reflections. The weighted 
    R-factor (wR) and goodness of fit (S) are based on F².
    R-factor (gt) are based on F. The threshold expression of
    F² > 2.0 sigma(F²) is used only for calculating R-factor (gt).
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_R_factor_all          0.0667
_refine_ls_R_factor_gt           0.0549
_refine_ls_wR_factor_ref         0.1639
_refine_ls_wR_factor_gt          0.1554
_refine_ls_number_restraints     0
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_reflns         3149
_refine_ls_number_parameters     224
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w = 1/[σ²(Fo²)+(0.0890P)²+8.0836P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_refine_ls_shift/su_max          0.001
_refine_diff_density_max         0.62
_refine_diff_density_min         -1.41
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
H H 0.0000 0.0000
;
International Tables for Crystallography
(Vol. C, Table 6.1.1.4)
;
Cu Cu -1.9646 0.5888
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
I I -0.3257 6.8362
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
N N 0.0311 0.0180
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
S S 0.3331 0.5567
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;

#==============================================================================
# ATOMIC COORDINATES AND THERMAL PARAMETERS

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C9 C 0.6114(15) 0.6713(6) 0.387(4) 0.060(7) Uani 0.53(5) 1 d . . P A 1
C10 C 0.630(3) 0.6618(7) 0.219(3) 0.063(9) Uani 0.53(5) 1 d . . P A 1
C13 C 0.5844(17) 0.6754(6) 0.300(4) 0.052(7) Uani 0.47(5) 1 d . . P A 2
C14 C 0.683(2) 0.6497(7) 0.263(3) 0.056(7) Uani 0.47(5) 1 d . . P A 2
I1 I 0.36375(7) 0.750000 0.16264(8) 0.0761(3) Uani 1 2 d S T P . .
Cu1 Cu 0.36778(11) 0.750000 0.44562(19) 0.0648(4) Uani 1 2 d S T P . .
S1 S 0.11539(14) 0.39775(7) 0.5007(2) 0.0713(6) Uani 1 1 d . . . . .
S2 S 0.26589(14) 0.35608(5) 0.19418(19) 0.0556(4) Uani 1 1 d . . . . .
S3 S 0.25389(11) 0.47414(5) 0.48175(18) 0.0471(4) Uani 1 1 d . . . . .
S4 S 0.38142(12) 0.43880(5) 0.22999(19) 0.0473(4) Uani 1 1 d . . . . .
S5 S 0.39897(11) 0.56389(5) 0.47716(18) 0.0458(4) Uani 1 1 d . . . . .
S6 S 0.52520(12) 0.52283(5) 0.23444(19) 0.0483(4) Uani 1 1 d . . . . .
S7 S 0.49725(16) 0.65106(5) 0.4574(2) 0.0646(5) Uani 1 1 d . . . . .
S8 S 0.65016(15) 0.60086(7) 0.1678(2) 0.0622(5) Uani 1 1 d . . . . .
N1 N 0.4812(6) 0.750000 0.5930(11) 0.060(2) Uani 1 2 d S T P . .
N2 N 0.2313(7) 0.750000 0.5473(11) 0.067(2) Uani 1 2 d S T P . .
N3 N 0.0619(8) 0.750000 0.6532(14) 0.106(4) Uani 1 2 d S T P . .
C1 C 0.0857(5) 0.3536(2) 0.3697(8) 0.0579(17) Uani 1 1 d . . . . .
H1A H 0.036812 0.333822 0.419584 0.070 Uiso 1 1 calc R U . . .
H1B H 0.051836 0.365887 0.279290 0.070 Uiso 1 1 calc R U . . .
C2 C 0.1771(5) 0.3270(2) 0.3173(7) 0.0541(16) Uani 1 1 d . . . . .
H2A H 0.152172 0.301172 0.262537 0.065 Uiso 1 1 calc R U . . .
H2B H 0.214332 0.316821 0.407972 0.065 Uiso 1 1 calc R U . . .
C3 C 0.2217(4) 0.4220(2) 0.4096(7) 0.0467(14) Uani 1 1 d . . . . .
C4 C 0.2794(5) 0.40634(19) 0.2926(7) 0.0438(13) Uani 1 1 d . . . . .
C5 C 0.3591(4) 0.4818(2) 0.3585(7) 0.0401(13) Uani 1 1 d . . . . .
C6 C 0.4196(4) 0.51860(19) 0.3586(7) 0.0408(13) Uani 1 1 d . . . . .
C7 C 0.4937(5) 0.59680(19) 0.3900(7) 0.0435(13) Uani 1 1 d . . . . .
C8 C 0.5513(5) 0.57786(19) 0.2790(7) 0.0423(13) Uani 1 1 d . . . . .
C11 C 0.5293(8) 0.750000 0.7050(13) 0.055(2) Uani 1 2 d S T P . .
C12 C 0.1555(8) 0.750000 0.6085(13) 0.058(2) Uani 1 2 d S T P . .


#==============================================================================
_computing_data_collection       'RAPID AUTO (Rigaku, ????)'
_computing_cell_refinement       'RAPID AUTO'
_computing_data_reduction        'RAPID AUTO'
_computing_structure_solution    'SHELXT Version 2018/2 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL Version 2018/3 (Sheldrick, 2008)'
_computing_publication_material  'CrystalStructure 4.3 (Rigaku, 2019)'
_computing_molecular_graphics    'CrystalStructure 4.3'

#==============================================================================
# MOLECULAR GEOMETRY

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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C9 C10 1.50(4) . ?
C9 S7 1.711(14) . ?
C10 S8 1.91(2) . ?
C13 C14 1.53(4) . ?
C13 S7 1.91(2) . ?
C14 S8 1.746(16) . ?
I1 Cu1 2.4459(17) . ?
Cu1 N1 1.941(9) . ?
Cu1 N2 1.971(9) . ?
S1 C3 1.744(6) . ?
S1 C1 1.793(7) . ?
S2 C4 1.751(6) . ?
S2 C2 1.794(6) . ?
S3 C5 1.742(6) . ?
S3 C3 1.748(6) . ?
S4 C4 1.731(6) . ?
S4 C5 1.735(6) . ?
S5 C6 1.731(6) . ?
S5 C7 1.749(6) . ?
S6 C6 1.741(6) . ?
S6 C8 1.742(6) . ?
S7 C7 1.742(6) . ?
S8 C8 1.743(6) . ?
N1 C11 1.150(13) . ?
N2 C12 1.113(13) . ?
N3 C12 1.269(15) . ?
N3 C11 1.296(14) 2_466 ?
C1 C2 1.498(10) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 C4 1.342(8) . ?
C5 C6 1.360(8) . ?
C7 C8 1.342(8) . ?

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
C10 C9 S7 114(2) . . ?
C9 C10 S8 116(2) . . ?
C14 C13 S7 116(2) . . ?
C13 C14 S8 109(2) . . ?
N1 Cu1 N2 112.5(4) . . ?
N1 Cu1 I1 132.2(3) . . ?
N2 Cu1 I1 115.3(3) . . ?
C3 S1 C1 101.4(3) . . ?
C4 S2 C2 101.6(3) . . ?
C5 S3 C3 95.0(3) . . ?
C4 S4 C5 95.7(3) . . ?
C6 S5 C7 95.1(3) . . ?
C6 S6 C8 94.9(3) . . ?
C9 S7 C7 103.9(6) . . ?
C7 S7 C13 98.2(7) . . ?
C8 S8 C14 105.0(7) . . ?
C8 S8 C10 99.0(7) . . ?
C11 N1 Cu1 163.7(9) . . ?
C12 N2 Cu1 178.1(9) . . ?
C12 N3 C11 126.7(11) . 2_466 ?
C2 C1 S1 114.9(5) . . ?
C2 C1 H1A 108.5 . . ?
S1 C1 H1A 108.5 . . ?
C2 C1 H1B 108.5 . . ?
S1 C1 H1B 108.5 . . ?
H1A C1 H1B 107.5 . . ?
C1 C2 S2 114.9(5) . . ?
C1 C2 H2A 108.5 . . ?
S2 C2 H2A 108.5 . . ?
C1 C2 H2B 108.5 . . ?
S2 C2 H2B 108.5 . . ?
H2A C2 H2B 107.5 . . ?
C4 C3 S1 129.0(5) . . ?
C4 C3 S3 117.0(5) . . ?
S1 C3 S3 113.9(3) . . ?
C3 C4 S4 117.3(5) . . ?
C3 C4 S2 128.1(5) . . ?
S4 C4 S2 114.6(3) . . ?
C6 C5 S4 121.2(4) . . ?
C6 C5 S3 123.8(5) . . ?
S4 C5 S3 114.9(3) . . ?
C5 C6 S5 124.0(5) . . ?
C5 C6 S6 120.7(5) . . ?
S5 C6 S6 115.3(3) . . ?
C8 C7 S7 128.8(5) . . ?
C8 C7 S5 116.9(4) . . ?
S7 C7 S5 114.3(3) . . ?
C7 C8 S6 117.3(4) . . ?
C7 C8 S8 129.0(5) . . ?
S6 C8 S8 113.7(3) . . ?
N1 C11 N3 166.3(11) . 2_566 ?
N2 C12 N3 169.3(12) . . ?

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
S7 C9 C10 S8 -67(4) . . . . ?
S7 C13 C14 S8 71(3) . . . . ?
C10 C9 S7 C7 47(3) . . . . ?
C13 C14 S8 C8 -48(3) . . . . ?
C3 S1 C1 C2 46.2(6) . . . . ?
S1 C1 C2 S2 -68.2(6) . . . . ?
C4 S2 C2 C1 45.9(6) . . . . ?
C1 S1 C3 C4 -12.8(7) . . . . ?
C1 S1 C3 S3 166.1(4) . . . . ?
C5 S3 C3 C4 -1.6(5) . . . . ?
C5 S3 C3 S1 179.4(4) . . . . ?
S1 C3 C4 S4 -179.3(4) . . . . ?
S3 C3 C4 S4 1.8(7) . . . . ?
S1 C3 C4 S2 -0.2(10) . . . . ?
S3 C3 C4 S2 -179.0(4) . . . . ?
C5 S4 C4 C3 -1.0(5) . . . . ?
C5 S4 C4 S2 179.7(4) . . . . ?
C2 S2 C4 C3 -12.5(7) . . . . ?
C2 S2 C4 S4 166.7(4) . . . . ?
C4 S4 C5 C6 -179.1(5) . . . . ?
C4 S4 C5 S3 -0.1(4) . . . . ?
C3 S3 C5 C6 179.9(5) . . . . ?
C3 S3 C5 S4 0.9(4) . . . . ?
S4 C5 C6 S5 177.1(3) . . . . ?
S3 C5 C6 S5 -1.9(8) . . . . ?
S4 C5 C6 S6 -2.7(7) . . . . ?
S3 C5 C6 S6 178.4(3) . . . . ?
C7 S5 C6 C5 -172.7(5) . . . . ?
C7 S5 C6 S6 7.0(4) . . . . ?
C8 S6 C6 C5 172.7(5) . . . . ?
C8 S6 C6 S5 -7.0(4) . . . . ?
C9 S7 C7 C8 -14.9(15) . . . . ?
C13 S7 C7 C8 10.8(11) . . . . ?
C9 S7 C7 S5 167.2(14) . . . . ?
C13 S7 C7 S5 -167.1(10) . . . . ?
C6 S5 C7 C8 -4.2(5) . . . . ?
C6 S5 C7 S7 173.9(3) . . . . ?
S7 C7 C8 S6 -177.9(4) . . . . ?
S5 C7 C8 S6 0.0(7) . . . . ?
S7 C7 C8 S8 1.3(9) . . . . ?
S5 C7 C8 S8 179.2(4) . . . . ?
C6 S6 C8 C7 4.2(5) . . . . ?
C6 S6 C8 S8 -175.1(3) . . . . ?
C14 S8 C8 C7 15.0(14) . . . . ?
C10 S8 C8 C7 -12.0(12) . . . . ?
C14 S8 C8 S6 -165.8(13) . . . . ?
C10 S8 C8 S6 167.2(11) . . . . ?
Cu1 N1 C11 N3 0.000(15) . . . 2_566 ?
C11 N3 C12 N2 180.000(11) 2_466 . . . ?


#==============================================================================
# Additional structures and associated data_? identifiers
# should be added at this point if there is more than one 
# structure analysis in the CIF.



#==============================================================================
#     End of CIF
#==============================================================================
_chemical_name_systematic        kappa-ET2Cu[N(CN)2]I
_exptl_crystal_recrystallization_method Electrocrystallization
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_100k_slow_autored
_database_code_depnum_ccdc_archive 'CCDC 2114422'
_audit_update_record             
;
2021-10-07 deposited with the CCDC.	2021-12-14 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        
'kappa-ET2Cu[N(CN)2]I, 100 K, slow cooling (-1 K/min)'
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C22 H17.07 Cu I N3 S16'
_chemical_formula_weight         1026.86

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 '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'

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

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   12.6749(3)
_cell_length_b                   30.0135(6)
_cell_length_c                   8.7173(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3316.22(13)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            black
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    2.057
_exptl_crystal_F_000             2032
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.07
_exptl_absorpt_coefficient_mu    2.623
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_measurement_device_type  
'dtrek-CrysAlisPro-abstract goniometer imported rigaku-d*trek images'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            55006
_diffrn_reflns_av_unetI/netI     0.0305
_diffrn_reflns_av_R_equivalents  0.0594
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -41
_diffrn_reflns_limit_k_max       41
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         2.433
_diffrn_reflns_theta_max         31.072
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.936
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.936
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.936
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             5074
_reflns_number_gt                4372
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1000P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5074
_refine_ls_number_parameters     248
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0469
_refine_ls_R_factor_gt           0.0362
_refine_ls_wR_factor_ref         0.1292
_refine_ls_wR_factor_gt          0.1203
_refine_ls_goodness_of_fit_ref   0.966
_refine_ls_restrained_S_all      0.966
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
I1 I 0.12280(3) 0.750000 0.84379(3) 0.02704(11) Uani 1 2 d S T P . .
Cu1 Cu 0.11712(4) 0.750000 0.56035(6) 0.01980(13) Uani 1 2 d S T P . .
S5 S 0.62273(5) 0.43893(2) -0.27052(8) 0.01513(15) Uani 1 1 d . . . . .
S3 S 0.60136(5) 0.56390(2) -0.01661(8) 0.01455(14) Uani 1 1 d . . . . .
S4 S 0.47528(5) 0.52305(2) -0.26312(8) 0.01630(15) Uani 1 1 d . . . . .
S6 S 0.75026(5) 0.47298(2) -0.01392(8) 0.01526(15) Uani 1 1 d . . . . .
S7 S 0.73827(6) 0.35478(2) -0.30681(8) 0.01838(16) Uani 1 1 d . . . . .
S1 S 0.50055(6) 0.65206(2) -0.03506(8) 0.02226(17) Uani 1 1 d . . . . .
S2 S 0.34719(6) 0.60202(3) -0.32821(9) 0.02284(17) Uani 1 1 d . . . . .
S8 S 0.88693(7) 0.39383(3) 0.00869(10) 0.0311(2) Uani 1 1 d . . . . .
N3 N 0.5018(3) 0.750000 0.0884(4) 0.0195(7) Uani 1 2 d S T P . .
N1 N 0.2534(3) 0.750000 0.4573(4) 0.0239(7) Uani 1 2 d S T P . .
N2 N 0.4320(3) 0.750000 0.3489(4) 0.0331(9) Uani 1 2 d S T P . .
C13 C 0.3352(3) 0.750000 0.3975(5) 0.0170(7) Uani 1 2 d S T P . .
C8 C 0.6446(2) 0.48143(9) -0.1380(3) 0.0134(5) Uani 1 1 d . . . . .
C7 C 0.5818(2) 0.51870(9) -0.1381(3) 0.0143(5) Uani 1 1 d . . . . .
C14 C 0.4608(3) 0.750000 0.2067(5) 0.0180(8) Uani 1 2 d S T P . .
C5 C 0.4474(2) 0.57859(8) -0.2174(3) 0.0148(5) Uani 1 1 d . . . . .
C6 C 0.5055(2) 0.59748(8) -0.1042(3) 0.0144(5) Uani 1 1 d . . . . .
C9 C 0.7248(2) 0.40462(9) -0.2053(3) 0.0156(5) Uani 1 1 d . . . . .
C10 C 0.7828(2) 0.42019(8) -0.0863(3) 0.0173(5) Uani 1 1 d . . . . .
C12 C 0.9229(2) 0.35239(10) -0.1303(3) 0.0185(5) Uani 1 1 d . . . . .
C11 C 0.8318(3) 0.32489(10) -0.1875(4) 0.0211(6) Uani 1 1 d . . . . .
C4 C 0.3670(4) 0.66226(14) -0.2791(5) 0.0183(11) Uani 0.732(10) 1 d . . P A 2
H4A H 0.428682 0.673160 -0.333149 0.022 Uiso 0.732(10) 1 calc R U P A 2
H4B H 0.306532 0.679080 -0.315220 0.022 Uiso 0.732(10) 1 calc R U P A 2
C3 C 0.3810(3) 0.67082(13) -0.1101(6) 0.0190(11) Uani 0.732(10) 1 d . . P A 2
C2 C 0.4076(9) 0.6756(3) -0.2013(12) 0.015(3) Uani 0.268(10) 1 d . . P A 1
H2A H 0.385235 0.705281 -0.171434 0.018 Uiso 0.268(10) 1 calc R U P A 1
H2B H 0.450370 0.678816 -0.292895 0.018 Uiso 0.268(10) 1 calc R U P A 1
C1 C 0.3098(9) 0.6495(3) -0.2448(13) 0.015(3) Uani 0.268(10) 1 d . . P A 1
H1A H 0.266716 0.666792 -0.314932 0.018 Uiso 0.268(10) 1 calc R U P A 1
H1B H 0.268245 0.643142 -0.153913 0.018 Uiso 0.268(10) 1 calc R U P A 1
H11A H 0.854(3) 0.3031(14) -0.255(5) 0.035(11) Uiso 1 1 d . . . . .
H12A H 0.957(3) 0.3657(11) -0.210(4) 0.026(9) Uiso 1 1 d . . . . .
H12B H 0.973(2) 0.3335(10) -0.072(4) 0.013(7) Uiso 1 1 d . . . . .
H11B H 0.796(2) 0.3131(9) -0.117(4) 0.006(7) Uiso 1 1 d . . . . .
H3A H 0.381(3) 0.7028(19) -0.098(6) 0.074(17) Uiso 1 1 d . . . B 2
H3B H 0.328(6) 0.658(2) 0.008(8) 0.15(3) Uiso 1 1 d . . . C 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
I1 Cu1 2.4719(6) . ?
Cu1 N1 1.947(4) . ?
Cu1 N3 1.954(3) 6_556 ?
S5 C8 1.743(3) . ?
S5 C9 1.748(3) . ?
S3 C7 1.739(3) . ?
S3 C6 1.753(3) . ?
S4 C7 1.739(3) . ?
S4 C5 1.750(3) . ?
S6 C8 1.740(3) . ?
S6 C10 1.755(3) . ?
S7 C9 1.746(3) . ?
S7 C11 1.814(3) . ?
S1 C3 1.744(4) . ?
S1 C6 1.746(3) . ?
S1 C2 1.997(11) . ?
S2 C1 1.669(9) . ?
S2 C5 1.744(3) . ?
S2 C4 1.875(4) . ?
S8 C10 1.747(3) . ?
S8 C12 1.795(3) . ?
N3 C14 1.154(5) . ?
N1 C13 1.160(5) . ?
N2 C14 1.293(5) . ?
N2 C13 1.298(6) . ?
C8 C7 1.373(4) . ?
C5 C6 1.356(4) . ?
C9 C10 1.355(4) . ?
C12 C11 1.505(4) . ?
C12 H12A 0.91(3) . ?
C12 H12B 0.99(3) . ?
C11 H11A 0.92(4) . ?
C11 H11B 0.84(3) . ?
C4 C3 1.506(6) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C3 H3A 0.97(6) . ?
C3 H3B 1.28(7) . ?
C2 C1 1.515(16) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Cu1 N3 110.92(15) . 6_556 ?
N1 Cu1 I1 115.82(11) . . ?
N3 Cu1 I1 133.26(10) 6_556 . ?
C8 S5 C9 95.62(12) . . ?
C7 S3 C6 94.83(12) . . ?
C7 S4 C5 94.91(12) . . ?
C8 S6 C10 95.10(13) . . ?
C9 S7 C11 101.36(14) . . ?
C3 S1 C6 101.82(16) . . ?
C6 S1 C2 95.9(3) . . ?
C1 S2 C5 108.1(4) . . ?
C5 S2 C4 99.50(15) . . ?
C10 S8 C12 100.68(13) . . ?
C14 N3 Cu1 158.3(3) . 6_656 ?
C13 N1 Cu1 179.2(3) . . ?
C14 N2 C13 125.5(4) . . ?
N1 C13 N2 172.4(4) . . ?
C7 C8 S6 124.4(2) . . ?
C7 C8 S5 120.2(2) . . ?
S6 C8 S5 115.33(15) . . ?
C8 C7 S3 123.5(2) . . ?
C8 C7 S4 120.8(2) . . ?
S3 C7 S4 115.72(15) . . ?
N3 C14 N2 169.7(4) . . ?
C6 C5 S2 129.1(2) . . ?
C6 C5 S4 117.0(2) . . ?
S2 C5 S4 113.91(15) . . ?
C5 C6 S1 128.6(2) . . ?
C5 C6 S3 116.93(19) . . ?
S1 C6 S3 114.45(15) . . ?
C10 C9 S7 129.1(2) . . ?
C10 C9 S5 116.6(2) . . ?
S7 C9 S5 114.34(15) . . ?
C9 C10 S8 128.1(2) . . ?
C9 C10 S6 117.3(2) . . ?
S8 C10 S6 114.58(15) . . ?
C11 C12 S8 114.1(2) . . ?
C11 C12 H12A 111(2) . . ?
S8 C12 H12A 109(2) . . ?
C11 C12 H12B 110.1(17) . . ?
S8 C12 H12B 102.4(18) . . ?
H12A C12 H12B 110(3) . . ?
C12 C11 S7 114.8(2) . . ?
C12 C11 H11A 111(2) . . ?
S7 C11 H11A 101(3) . . ?
C12 C11 H11B 113(2) . . ?
S7 C11 H11B 106(2) . . ?
H11A C11 H11B 109(3) . . ?
C3 C4 S2 113.8(3) . . ?
C3 C4 H4A 108.8 . . ?
S2 C4 H4A 108.8 . . ?
C3 C4 H4B 108.8 . . ?
S2 C4 H4B 108.8 . . ?
H4A C4 H4B 107.7 . . ?
C4 C3 S1 114.5(3) . . ?
C4 C3 H3A 106(3) . . ?
S1 C3 H3A 106(3) . . ?
C4 C3 H3B 132(3) . . ?
S1 C3 H3B 93(3) . . ?
H3A C3 H3B 102(4) . . ?
C1 C2 S1 118.8(7) . . ?
C1 C2 H2A 107.6 . . ?
S1 C2 H2A 107.6 . . ?
C1 C2 H2B 107.6 . . ?
S1 C2 H2B 107.6 . . ?
H2A C2 H2B 107.1 . . ?
C2 C1 S2 108.5(8) . . ?
C2 C1 H1A 110.0 . . ?
S2 C1 H1A 110.0 . . ?
C2 C1 H1B 110.0 . . ?
S2 C1 H1B 110.0 . . ?
H1A C1 H1B 108.4 . . ?

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
C10 S6 C8 C7 179.2(2) . . . . ?
C10 S6 C8 S5 -1.93(18) . . . . ?
C9 S5 C8 C7 -179.5(2) . . . . ?
C9 S5 C8 S6 1.58(17) . . . . ?
S6 C8 C7 S3 1.9(4) . . . . ?
S5 C8 C7 S3 -176.86(15) . . . . ?
S6 C8 C7 S4 -177.89(15) . . . . ?
S5 C8 C7 S4 3.3(3) . . . . ?
C6 S3 C7 C8 172.6(2) . . . . ?
C6 S3 C7 S4 -7.56(17) . . . . ?
C5 S4 C7 C8 -172.7(2) . . . . ?
C5 S4 C7 S3 7.47(17) . . . . ?
Cu1 N3 C14 N2 0.000(3) 6_656 . . . ?
C13 N2 C14 N3 180.000(1) . . . . ?
C1 S2 C5 C6 -14.2(5) . . . . ?
C4 S2 C5 C6 13.0(3) . . . . ?
C1 S2 C5 S4 166.3(5) . . . . ?
C4 S2 C5 S4 -166.49(19) . . . . ?
C7 S4 C5 C6 -4.3(2) . . . . ?
C7 S4 C5 S2 175.21(16) . . . . ?
S2 C5 C6 S1 -1.5(4) . . . . ?
S4 C5 C6 S1 177.98(15) . . . . ?
S2 C5 C6 S3 -179.67(16) . . . . ?
S4 C5 C6 S3 -0.2(3) . . . . ?
C3 S1 C6 C5 15.3(3) . . . . ?
C2 S1 C6 C5 -10.3(4) . . . . ?
C3 S1 C6 S3 -166.4(2) . . . . ?
C2 S1 C6 S3 168.0(3) . . . . ?
C7 S3 C6 C5 4.6(2) . . . . ?
C7 S3 C6 S1 -173.82(15) . . . . ?
C11 S7 C9 C10 11.0(3) . . . . ?
C11 S7 C9 S5 -170.05(16) . . . . ?
C8 S5 C9 C10 -0.4(2) . . . . ?
C8 S5 C9 S7 -179.49(16) . . . . ?
S7 C9 C10 S8 -3.0(4) . . . . ?
S5 C9 C10 S8 178.06(17) . . . . ?
S7 C9 C10 S6 178.03(17) . . . . ?
S5 C9 C10 S6 -0.9(3) . . . . ?
C12 S8 C10 C9 18.8(3) . . . . ?
C12 S8 C10 S6 -162.21(16) . . . . ?
C8 S6 C10 C9 1.7(3) . . . . ?
C8 S6 C10 S8 -177.39(17) . . . . ?
C10 S8 C12 C11 -51.0(2) . . . . ?
S8 C12 C11 S7 69.3(3) . . . . ?
C9 S7 C11 C12 -43.5(3) . . . . ?
C5 S2 C4 C3 -46.1(3) . . . . ?
S2 C4 C3 S1 70.6(4) . . . . ?
C6 S1 C3 C4 -49.5(3) . . . . ?
S1 C2 C1 S2 -68.3(10) . . . . ?
C5 S2 C1 C2 46.1(9) . . . . ?

_refine_diff_density_max         0.669
_refine_diff_density_min         -1.107
_refine_diff_density_rms         0.118


_exptl_crystal_recrystallization_method Electrocrystallization
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_296k__autored
_database_code_depnum_ccdc_archive 'CCDC 2114421'
_audit_update_record             
;
2021-10-07 deposited with the CCDC.	2021-12-14 downloaded from the CCDC.
;
_audit_creation_date             2021-07-11
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        'kappa-ET2Cu[N(CN)2]I, 296 K'
_chemical_formula_moiety         '0.5(C4 Cu2 I2 N6), 2(C10 H8.951 S8)'
_chemical_formula_sum            'C22 H17.90 Cu I N3 S16'
_chemical_formula_weight         1027.69
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 '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'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_H-M_alt        'P n m a'
_space_group_name_Hall           '-P 2ac 2n'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z'
'-x-1/2, y-1/2, z-1/2'

_cell_length_a                   12.8915(4)
_cell_length_b                   30.2499(8)
_cell_length_c                   8.6831(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3386.12(16)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    25816
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      30.7200
_cell_measurement_theta_min      2.4280
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    2.569
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.76954
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.93a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    2.016
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2036
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.07
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0730
_diffrn_reflns_av_unetI/netI     0.0421
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.936
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       41
_diffrn_reflns_limit_k_min       -41
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            56376
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.936
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.166
_diffrn_reflns_theta_min         2.440
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.936
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -110.00  70.00   0.50    1.00    --  -20.00  45.00   0.00  360
  2  ω   -110.00  70.00   0.50    1.00    --  -20.00  45.00  90.00  360
  3  ω   -110.00  70.00   0.50    1.00    --  -20.00  45.00 180.00  360
  4  ω   -110.00  70.00   0.50    1.00    --  -20.00  45.00 270.00  360
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  
'dtrek-CrysAlisPro-abstract goniometer imported rigaku-d*trek images'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0375024000
_diffrn_orient_matrix_UB_12      0.0126555000
_diffrn_orient_matrix_UB_13      -0.0403212000
_diffrn_orient_matrix_UB_21      -0.0021299000
_diffrn_orient_matrix_UB_22      0.0151662000
_diffrn_orient_matrix_UB_23      0.0622112000
_diffrn_orient_matrix_UB_31      0.0402160000
_diffrn_orient_matrix_UB_32      0.0126281000
_diffrn_orient_matrix_UB_33      -0.0342980000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3742
_reflns_number_total             5224
_reflns_odcompleteness_completeness 93.68
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     31.10
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.742
_refine_diff_density_min         -0.779
_refine_diff_density_rms         0.099
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     244
_refine_ls_number_reflns         5224
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0839
_refine_ls_R_factor_gt           0.0499
_refine_ls_restrained_S_all      1.028
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1000P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1462
_refine_ls_wR_factor_ref         0.1667
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
2. Others
 Sof(C2)=Sof(H2A)=Sof(H2B)=Sof(C1)=Sof(H1A)=Sof(H1B)=1-FVAR(1)
 Sof(C4)=Sof(H4A)=Sof(H4B)=Sof(C3)=FVAR(1)
3.a Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C2(H2A,H2B), C1(H1A,H1B)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
I1 I 0.63432(4) 0.250000 0.83943(5) 0.05225(17) Uani 1 2 d S T P . .
Cu1 Cu 0.62918(6) 0.250000 0.55468(9) 0.0458(2) Uani 1 2 d S T P . .
S6 S 0.74670(7) 0.52595(3) 0.51754(11) 0.0349(2) Uani 1 1 d . . . . .
S5 S 0.61972(7) 0.56100(3) 0.77016(12) 0.0354(2) Uani 1 1 d . . . . .
S4 S 0.60077(8) 0.43609(3) 0.52192(11) 0.0345(2) Uani 1 1 d . . . . .
S3 S 0.47472(8) 0.47708(3) 0.76495(12) 0.0363(2) Uani 1 1 d . . . . .
S7 S 0.73538(9) 0.64383(3) 0.80624(12) 0.0430(3) Uani 1 1 d . . . . .
S1 S 0.34965(9) 0.39893(4) 0.83098(13) 0.0497(3) Uani 1 1 d . . . . .
S2 S 0.50139(10) 0.34890(3) 0.54103(13) 0.0505(3) Uani 1 1 d . . . . .
S8 S 0.88528(10) 0.60272(4) 0.49866(15) 0.0600(4) Uani 1 1 d . . . . .
N1 N 0.5147(4) 0.250000 0.4080(6) 0.0426(11) Uani 1 2 d S T P . .
C7 C 0.5802(3) 0.48153(11) 0.6403(4) 0.0301(7) Uani 1 1 d . . . . .
N3 N 0.2642(4) 0.250000 0.0483(6) 0.0515(13) Uani 1 2 d S T P . .
C8 C 0.6419(3) 0.51785(12) 0.6405(4) 0.0300(7) Uani 1 1 d . . . . .
C9 C 0.7217(3) 0.59391(11) 0.7063(4) 0.0317(8) Uani 1 1 d . . . . .
C6 C 0.5060(3) 0.40312(11) 0.6096(4) 0.0312(7) Uani 1 1 d . . . . .
C10 C 0.7804(3) 0.57805(12) 0.5908(4) 0.0345(8) Uani 1 1 d . . . . .
C5 C 0.4484(3) 0.42229(12) 0.7204(4) 0.0312(8) Uani 1 1 d . . . . .
C13 C 0.4693(4) 0.250000 0.2942(7) 0.0406(13) Uani 1 2 d S T P . .
C14 C 0.3413(5) 0.250000 0.1084(7) 0.0445(13) Uani 1 2 d S T P . .
C12 C 0.9166(3) 0.64645(15) 0.6306(5) 0.0436(10) Uani 1 1 d . . . . .
H12A H 0.948(3) 0.6345(15) 0.715(5) 0.052 Uiso 1 1 d . U . . .
H12B H 0.966(3) 0.6642(15) 0.571(5) 0.052 Uiso 1 1 d . U . . .
C11 C 0.8252(4) 0.67294(14) 0.6839(5) 0.0424(10) Uani 1 1 d . . . . .
H11A H 0.783(3) 0.6834(14) 0.607(5) 0.051 Uiso 1 1 d . U . . .
H11B H 0.848(4) 0.6929(16) 0.740(6) 0.051 Uiso 1 1 d . U . . .
N2 N 0.4367(5) 0.250000 0.1530(7) 0.086(3) Uani 1 2 d S T P . .
C4 C 0.3715(10) 0.3391(3) 0.7848(13) 0.040(3) Uani 0.52(2) 1 d . . P A 2
H4A H 0.431229 0.328766 0.842465 0.047 Uiso 0.52(2) 1 calc R U P A 2
H4B H 0.311751 0.322313 0.819087 0.047 Uiso 0.52(2) 1 calc R U P A 2
C2 C 0.4130(10) 0.3256(3) 0.701(2) 0.049(3) Uani 0.48(2) 1 d . . P A 1
H2A H 0.391594 0.296237 0.669436 0.058 Uiso 0.48(2) 1 calc R U P A 1
H2B H 0.454868 0.322284 0.792725 0.058 Uiso 0.48(2) 1 calc R U P A 1
C3 C 0.3893(8) 0.3298(4) 0.6153(16) 0.042(3) Uani 0.52(2) 1 d . . P A 2
C1 C 0.3185(10) 0.3503(4) 0.7442(14) 0.043(3) Uani 0.48(2) 1 d . . P A 1
H1A H 0.277090 0.332539 0.813886 0.052 Uiso 0.48(2) 1 calc R U P A 1
H1B H 0.277432 0.356173 0.652908 0.052 Uiso 0.48(2) 1 calc R U P A 1
H3A H 0.343(5) 0.348(2) 0.547(8) 0.11(3) Uiso 1 1 d . . . B 2
H3B H 0.390(5) 0.308(3) 0.604(10) 0.13(4) Uiso 1 1 d . . . C 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
I1 Cu1 2.4734(9) . ?
Cu1 N1 1.950(5) . ?
Cu1 N3 1.957(5) 6_656 ?
S6 C8 1.740(4) . ?
S6 C10 1.754(4) . ?
S5 C8 1.747(4) . ?
S5 C9 1.740(4) . ?
S4 C7 1.737(3) . ?
S4 C6 1.751(4) . ?
S3 C7 1.743(4) . ?
S3 C5 1.735(4) . ?
S7 C9 1.750(3) . ?
S7 C11 1.801(4) . ?
S1 C5 1.744(4) . ?
S1 C4 1.874(10) . ?
S1 C1 1.700(9) . ?
S2 C6 1.746(3) . ?
S2 C2 1.928(13) . ?
S2 C3 1.684(9) . ?
S8 C10 1.739(4) . ?
S8 C12 1.796(4) . ?
N1 C13 1.147(8) . ?
C7 C8 1.356(5) . ?
N3 C14 1.122(8) . ?
C9 C10 1.345(5) . ?
C6 C5 1.347(5) . ?
C13 N2 1.296(8) . ?
C14 N2 1.290(9) . ?
C12 H12A 0.91(4) . ?
C12 H12B 0.98(5) . ?
C12 C11 1.499(6) . ?
C11 H11A 0.92(4) . ?
C11 H11B 0.83(5) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C4 C3 1.516(16) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C2 C1 1.477(19) . ?
C3 H3A 1.00(7) . ?
C3 H3B 0.68(9) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Cu1 I1 132.33(15) . . ?
N1 Cu1 N3 112.0(2) . 6_656 ?
N3 Cu1 I1 115.64(17) 6_656 . ?
C8 S6 C10 95.54(17) . . ?
C9 S5 C8 95.67(17) . . ?
C7 S4 C6 94.99(17) . . ?
C5 S3 C7 95.03(17) . . ?
C9 S7 C11 101.19(19) . . ?
C5 S1 C4 99.4(3) . . ?
C1 S1 C5 106.2(4) . . ?
C6 S2 C2 96.8(4) . . ?
C3 S2 C6 102.7(4) . . ?
C10 S8 C12 101.40(19) . . ?
C13 N1 Cu1 161.4(5) . . ?
S4 C7 S3 115.2(2) . . ?
C8 C7 S4 123.5(3) . . ?
C8 C7 S3 121.3(3) . . ?
C14 N3 Cu1 179.5(6) . 6_556 ?
S6 C8 S5 114.7(2) . . ?
C7 C8 S6 124.7(3) . . ?
C7 C8 S5 120.7(3) . . ?
S5 C9 S7 114.3(2) . . ?
C10 C9 S5 117.3(3) . . ?
C10 C9 S7 128.4(3) . . ?
S2 C6 S4 114.2(2) . . ?
C5 C6 S4 116.7(3) . . ?
C5 C6 S2 129.0(3) . . ?
S8 C10 S6 114.3(2) . . ?
C9 C10 S6 116.8(3) . . ?
C9 C10 S8 128.8(3) . . ?
S3 C5 S1 114.0(2) . . ?
C6 C5 S3 117.6(3) . . ?
C6 C5 S1 128.4(3) . . ?
N1 C13 N2 168.3(7) . . ?
N3 C14 N2 169.8(7) . . ?
S8 C12 H12A 109(3) . . ?
S8 C12 H12B 102(3) . . ?
H12A C12 H12B 111(4) . . ?
C11 C12 S8 114.4(3) . . ?
C11 C12 H12A 108(3) . . ?
C11 C12 H12B 113(3) . . ?
S7 C11 H11A 103(3) . . ?
S7 C11 H11B 104(4) . . ?
C12 C11 S7 115.2(3) . . ?
C12 C11 H11A 115(3) . . ?
C12 C11 H11B 107(3) . . ?
H11A C11 H11B 113(4) . . ?
C14 N2 C13 126.4(6) . . ?
S1 C4 H4A 108.7 . . ?
S1 C4 H4B 108.7 . . ?
H4A C4 H4B 107.6 . . ?
C3 C4 S1 114.2(8) . . ?
C3 C4 H4A 108.7 . . ?
C3 C4 H4B 108.7 . . ?
S2 C2 H2A 107.5 . . ?
S2 C2 H2B 107.5 . . ?
H2A C2 H2B 107.0 . . ?
C1 C2 S2 119.1(9) . . ?
C1 C2 H2A 107.5 . . ?
C1 C2 H2B 107.5 . . ?
S2 C3 H3A 96(4) . . ?
S2 C3 H3B 106(6) . . ?
C4 C3 S2 116.0(9) . . ?
C4 C3 H3A 113(4) . . ?
C4 C3 H3B 109(8) . . ?
H3A C3 H3B 117(8) . . ?
S1 C1 H1A 109.5 . . ?
S1 C1 H1B 109.5 . . ?
C2 C1 S1 110.9(10) . . ?
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
H1A C1 H1B 108.1 . . ?

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
Cu1 N1 C13 N2 0.000(4) . . . . ?
S5 C9 C10 S6 0.2(4) . . . . ?
S5 C9 C10 S8 178.6(2) . . . . ?
S4 C7 C8 S6 3.2(5) . . . . ?
S4 C7 C8 S5 -176.7(2) . . . . ?
S4 C6 C5 S3 -0.4(4) . . . . ?
S4 C6 C5 S1 -179.2(2) . . . . ?
S3 C7 C8 S6 -178.3(2) . . . . ?
S3 C7 C8 S5 1.8(5) . . . . ?
S7 C9 C10 S6 178.9(2) . . . . ?
S7 C9 C10 S8 -2.7(6) . . . . ?
S1 C4 C3 S2 68.6(14) . . . . ?
S2 C6 C5 S3 178.5(2) . . . . ?
S2 C6 C5 S1 -0.3(6) . . . . ?
S2 C2 C1 S1 -67.7(16) . . . . ?
S8 C12 C11 S7 68.3(4) . . . . ?
N1 C13 N2 C14 180.000(3) . . . . ?
C7 S4 C6 S2 -174.7(2) . . . . ?
C7 S4 C6 C5 4.4(3) . . . . ?
C7 S3 C5 S1 175.2(2) . . . . ?
C7 S3 C5 C6 -3.7(3) . . . . ?
N3 C14 N2 C13 180.000(1) . . . . ?
C8 S6 C10 S8 -178.6(2) . . . . ?
C8 S6 C10 C9 0.1(4) . . . . ?
C8 S5 C9 S7 -179.3(2) . . . . ?
C8 S5 C9 C10 -0.3(3) . . . . ?
C9 S5 C8 S6 0.4(2) . . . . ?
C9 S5 C8 C7 -179.7(3) . . . . ?
C9 S7 C11 C12 -45.9(4) . . . . ?
C6 S4 C7 S3 -6.9(2) . . . . ?
C6 S4 C7 C8 171.7(3) . . . . ?
C6 S2 C3 C4 -47.1(11) . . . . ?
C10 S6 C8 S5 -0.3(2) . . . . ?
C10 S6 C8 C7 179.8(3) . . . . ?
C10 S8 C12 C11 -47.2(4) . . . . ?
C5 S3 C7 S4 6.7(2) . . . . ?
C5 S3 C7 C8 -171.9(3) . . . . ?
C5 S1 C4 C3 -45.0(10) . . . . ?
C5 S1 C1 C2 44.8(13) . . . . ?
C12 S8 C10 S6 -166.1(2) . . . . ?
C12 S8 C10 C9 15.4(5) . . . . ?
C11 S7 C9 S5 -167.7(2) . . . . ?
C11 S7 C9 C10 13.5(4) . . . . ?
C4 S1 C5 S3 -165.8(5) . . . . ?
C4 S1 C5 C6 13.1(6) . . . . ?
C2 S2 C6 S4 167.7(5) . . . . ?
C2 S2 C6 C5 -11.3(6) . . . . ?
C3 S2 C6 S4 -167.9(6) . . . . ?
C3 S2 C6 C5 13.2(7) . . . . ?
C1 S1 C5 S3 167.8(6) . . . . ?
C1 S1 C5 C6 -13.4(7) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.294
_oxdiff_exptl_absorpt_empirical_full_min 0.761
_exptl_crystal_recrystallization_method Electrocrystallization
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_No2_IM_296K
_database_code_depnum_ccdc_archive 'CCDC 2001305'
loop_
_audit_author_name
_audit_author_address
'Toshio Naito'
;Ehime University
Japan
;
_audit_update_record             
;
2020-05-06 deposited with the CCDC.	2021-12-14 downloaded from the CCDC.
;

#==============================================================================
# CHEMICAL DATA

_chemical_formula_sum            'C22 H16 Cu I N3 S16'
_chemical_formula_moiety         'C22 H16 Cu I N3 S16'
_chemical_formula_weight         1025.80
_chemical_melting_point          ?

#==============================================================================
# CRYSTAL DATA
_space_group_crystal_system      orthorhombic
_space_group_name_H-M_alt        'P n m a'
_space_group_name_Hall           '-P 2ac 2n'
_space_group_IT_number           62
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 +X,+Y,+Z
2 1/2+X,1/2-Y,1/2-Z
3 -X,1/2+Y,-Z
4 1/2-X,-Y,1/2+Z
5 -X,-Y,-Z
6 -1/2-X,-1/2+Y,-1/2+Z
7 +X,-1/2-Y,+Z
8 -1/2+X,+Y,-1/2-Z
#------------------------------------------------------------------------------
_cell_length_a                   12.9118(5)
_cell_length_b                   30.3410(11)
_cell_length_c                   8.6516(3)
_cell_angle_alpha                90.0000
_cell_angle_beta                 90.0000
_cell_angle_gamma                90.0000
_cell_volume                     3389.3(2)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    21937
_cell_measurement_theta_min      3.42
_cell_measurement_theta_max      68.61
_cell_measurement_temperature    296
#------------------------------------------------------------------------------
_exptl_crystal_description       plate
_exptl_crystal_colour            black
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_exptl_crystal_density_diffrn    2.010
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2028.00
_exptl_absorpt_coefficient_mu    17.481
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Rigaku, 1995)'
_exptl_absorpt_correction_T_min  0.108
_exptl_absorpt_correction_T_max  0.174

#==============================================================================
# EXPERIMENTAL DATA

_diffrn_ambient_temperature      296
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54187
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean 10.000
_diffrn_reflns_number            35119
_diffrn_reflns_av_unetI/netI     0.0427
_diffrn_reflns_av_R_equivalents  0.0995
_diffrn_reflns_theta_max         68.248
_diffrn_reflns_theta_min         5.317
_diffrn_reflns_theta_full        67.687
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measured_fraction_theta_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_limit_l_max       10
_diffrn_standards_number         0
_diffrn_standards_interval_count .
_diffrn_standards_decay_%        ?
_reflns_number_total             3144
_reflns_number_gt                2754
_reflns_threshold_expression     F²>2.0σ(F²)
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

#==============================================================================
# REFINEMENT DATA

_refine_special_details          
;
    Refinement was performed using all reflections. The weighted 
    R-factor (wR) and goodness of fit (S) are based on F².
    R-factor (gt) are based on F. The threshold expression of
    F² > 2.0 sigma(F²) is used only for calculating R-factor (gt).
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_R_factor_all          0.0926
_refine_ls_R_factor_gt           0.0853
_refine_ls_wR_factor_ref         0.2241
_refine_ls_wR_factor_gt          0.2194
_refine_ls_number_restraints     0
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_reflns         3144
_refine_ls_number_parameters     224
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w = 1/[σ²(Fo²)+(0.0810P)²+62.2840P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_refine_ls_shift/su_max          0.000
_refine_diff_density_max         2.59
_refine_diff_density_min         -0.75
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
H H 0.0000 0.0000
;
International Tables for Crystallography
(Vol. C, Table 6.1.1.4)
;
Cu Cu -1.9646 0.5888
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
I I -0.3257 6.8362
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
N N 0.0311 0.0180
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
S S 0.3331 0.5567
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;

#==============================================================================
# ATOMIC COORDINATES AND THERMAL PARAMETERS

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C9 C 0.377(6) 0.3372(15) 1.279(4) 0.09(2) Uani 0.58(9) 1 d . . P A 1
C10 C 0.391(2) 0.3284(9) 1.120(7) 0.053(12) Uani 0.58(9) 1 d . . P A 1
C13 C 0.316(3) 0.3507(10) 1.237(6) 0.051(12) Uani 0.42(9) 1 d . . P A 2
C14 C 0.418(3) 0.3256(10) 1.203(6) 0.038(10) Uani 0.42(9) 1 d . . P A 2
I1 I 0.13819(11) 0.250000 0.16109(14) 0.0637(4) Uani 1 2 d S T P . .
Cu1 Cu 0.1340(2) 0.250000 0.4453(3) 0.0587(7) Uani 1 2 d S T P . .
S1 S 0.7344(2) 0.64367(9) 1.3059(3) 0.0518(7) Uani 1 1 d . . . . .
S2 S 0.8849(3) 0.60230(12) 0.9996(4) 0.0676(10) Uani 1 1 d . . . . .
S3 S 0.6178(2) 0.56104(8) 1.2693(3) 0.0424(6) Uani 1 1 d . . . . .
S4 S 0.74623(19) 0.52576(8) 1.0177(3) 0.0417(6) Uani 1 1 d . . . . .
S5 S 0.4748(2) 0.47714(8) 1.2652(3) 0.0437(6) Uani 1 1 d . . . . .
S6 S 0.60142(19) 0.43618(8) 1.0226(3) 0.0409(6) Uani 1 1 d . . . . .
S7 S 0.3495(2) 0.39912(11) 1.3315(4) 0.0559(8) Uani 1 1 d . . . . .
S8 S 0.5026(3) 0.34913(9) 1.0421(4) 0.0613(9) Uani 1 1 d . . . . .
N1 N 0.0192(12) 0.250000 0.5902(19) 0.056(4) Uani 1 2 d S T P . .
N2 N 0.2703(10) 0.250000 0.5441(19) 0.056(4) Uani 1 2 d S T P . .
N3 N 0.4355(14) 0.250000 0.656(3) 0.105(7) Uani 1 2 d S T P . .
C1 C 0.8256(10) 0.6721(4) 1.1857(13) 0.050(3) Uani 1 1 d . . . . .
H21A H 0.789268 0.683125 1.095479 0.060 Uiso 1 1 calc R U . . .
H21B H 0.851528 0.697416 1.242228 0.060 Uiso 1 1 calc R U . . .
C2 C 0.9153(9) 0.6456(4) 1.1327(15) 0.053(3) Uani 1 1 d . . . . .
H20A H 0.948592 0.632722 1.222478 0.064 Uiso 1 1 calc R U . . .
H20B H 0.964922 0.665213 1.084193 0.064 Uiso 1 1 calc R U . . .
C3 C 0.7221(8) 0.5939(3) 1.2074(12) 0.038(2) Uani 1 1 d . . . . .
C4 C 0.7790(7) 0.5776(3) 1.0911(13) 0.040(2) Uani 1 1 d . . . . .
C5 C 0.6415(7) 0.5185(3) 1.1385(12) 0.035(2) Uani 1 1 d . . . . .
C6 C 0.5797(8) 0.4811(3) 1.1431(12) 0.036(2) Uani 1 1 d . . . . .
C7 C 0.4491(8) 0.4220(3) 1.2190(12) 0.039(2) Uani 1 1 d . . . . .
C8 C 0.5062(8) 0.4034(3) 1.1104(12) 0.038(2) Uani 1 1 d . . . . .
C11 C -0.0340(14) 0.250000 0.703(2) 0.051(4) Uani 1 2 d S T P . .
C12 C 0.3412(14) 0.250000 0.608(3) 0.058(5) Uani 1 2 d S T P . .


#==============================================================================
_computing_data_collection       'RAPID AUTO (Rigaku, ????)'
_computing_cell_refinement       'RAPID AUTO'
_computing_data_reduction        'RAPID AUTO'
_computing_structure_solution    'SHELXT Version 2018/2 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL Version 2018/3 (Sheldrick, 2008)'
_computing_publication_material  'CrystalStructure 4.3 (Rigaku, 2019)'
_computing_molecular_graphics    'CrystalStructure 4.3'

#==============================================================================
# MOLECULAR GEOMETRY

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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C9 C10 1.41(6) . ?
C9 S7 1.96(5) . ?
C10 S8 1.71(2) . ?
C13 C14 1.54(6) . ?
C13 S7 1.74(3) . ?
C14 S8 1.91(3) . ?
I1 Cu1 2.460(3) . ?
Cu1 N1 1.941(17) . ?
Cu1 N2 1.956(13) . ?
S1 C3 1.742(10) . ?
S1 C1 1.792(11) . ?
S2 C4 1.749(10) . ?
S2 C2 1.791(12) . ?
S3 C5 1.743(10) . ?
S3 C3 1.758(10) . ?
S4 C5 1.723(10) . ?
S4 C4 1.748(10) . ?
S5 C6 1.722(10) . ?
S5 C7 1.750(11) . ?
S6 C6 1.739(10) . ?
S6 C8 1.754(11) . ?
S7 C7 1.757(10) . ?
S8 C8 1.750(10) . ?
N1 C11 1.20(2) . ?
N2 C12 1.07(2) . ?
N3 C11 1.28(3) 2_556 ?
N3 C12 1.29(3) . ?
C1 C2 1.483(17) . ?
C1 H21A 0.9700 . ?
C1 H21B 0.9700 . ?
C2 H20A 0.9700 . ?
C2 H20B 0.9700 . ?
C3 C4 1.340(14) . ?
C5 C6 1.388(14) . ?
C7 C8 1.321(15) . ?

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
C10 C9 S7 115(4) . . ?
C9 C10 S8 115(4) . . ?
C14 C13 S7 107(4) . . ?
C13 C14 S8 116(3) . . ?
N1 Cu1 N2 113.9(7) . . ?
N1 Cu1 I1 131.5(5) . . ?
N2 Cu1 I1 114.6(5) . . ?
C3 S1 C1 101.2(5) . . ?
C4 S2 C2 101.2(5) . . ?
C5 S3 C3 95.0(5) . . ?
C5 S4 C4 94.8(5) . . ?
C6 S5 C7 94.3(5) . . ?
C6 S6 C8 94.1(5) . . ?
C13 S7 C7 104.8(14) . . ?
C7 S7 C9 96.7(12) . . ?
C10 S8 C8 103.6(9) . . ?
C8 S8 C14 96.9(12) . . ?
C11 N1 Cu1 165.2(14) . . ?
C12 N2 Cu1 174.7(17) . . ?
C11 N3 C12 127(2) 2_556 . ?
C2 C1 S1 115.5(8) . . ?
C2 C1 H21A 108.4 . . ?
S1 C1 H21A 108.4 . . ?
C2 C1 H21B 108.4 . . ?
S1 C1 H21B 108.4 . . ?
H21A C1 H21B 107.5 . . ?
C1 C2 S2 115.2(9) . . ?
C1 C2 H20A 108.5 . . ?
S2 C2 H20A 108.5 . . ?
C1 C2 H20B 108.5 . . ?
S2 C2 H20B 108.5 . . ?
H20A C2 H20B 107.5 . . ?
C4 C3 S1 129.5(8) . . ?
C4 C3 S3 116.1(8) . . ?
S1 C3 S3 114.4(6) . . ?
C3 C4 S4 118.2(8) . . ?
C3 C4 S2 127.6(8) . . ?
S4 C4 S2 114.2(6) . . ?
C6 C5 S4 124.9(8) . . ?
C6 C5 S3 119.1(8) . . ?
S4 C5 S3 115.9(5) . . ?
C5 C6 S5 121.8(8) . . ?
C5 C6 S6 122.1(8) . . ?
S5 C6 S6 116.1(6) . . ?
C8 C7 S5 117.7(8) . . ?
C8 C7 S7 129.3(8) . . ?
S5 C7 S7 113.0(6) . . ?
C7 C8 S8 128.9(8) . . ?
C7 C8 S6 117.2(8) . . ?
S8 C8 S6 114.0(6) . . ?
N1 C11 N3 163(2) . 2_456 ?
N2 C12 N3 168(2) . . ?

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
S7 C9 C10 S8 69(7) . . . . ?
S7 C13 C14 S8 -73(5) . . . . ?
C14 C13 S7 C7 49(4) . . . . ?
C9 C10 S8 C8 -47(6) . . . . ?
C3 S1 C1 C2 -44.2(10) . . . . ?
S1 C1 C2 S2 67.9(12) . . . . ?
C4 S2 C2 C1 -47.4(10) . . . . ?
C1 S1 C3 C4 11.3(12) . . . . ?
C1 S1 C3 S3 -167.5(6) . . . . ?
C5 S3 C3 C4 0.8(9) . . . . ?
C5 S3 C3 S1 179.7(6) . . . . ?
S1 C3 C4 S4 179.7(7) . . . . ?
S3 C3 C4 S4 -1.6(12) . . . . ?
S1 C3 C4 S2 -0.6(17) . . . . ?
S3 C3 C4 S2 178.1(7) . . . . ?
C5 S4 C4 C3 1.5(10) . . . . ?
C5 S4 C4 S2 -178.3(6) . . . . ?
C2 S2 C4 C3 14.5(12) . . . . ?
C2 S2 C4 S4 -165.7(7) . . . . ?
C4 S4 C5 C6 -177.8(9) . . . . ?
C4 S4 C5 S3 -0.9(7) . . . . ?
C3 S3 C5 C6 177.3(9) . . . . ?
C3 S3 C5 S4 0.3(7) . . . . ?
S4 C5 C6 S5 -178.7(6) . . . . ?
S3 C5 C6 S5 4.5(12) . . . . ?
S4 C5 C6 S6 -0.4(13) . . . . ?
S3 C5 C6 S6 -177.2(5) . . . . ?
C7 S5 C6 C5 -174.4(9) . . . . ?
C7 S5 C6 S6 7.3(6) . . . . ?
C8 S6 C6 C5 174.2(9) . . . . ?
C8 S6 C6 S5 -7.5(7) . . . . ?
C6 S5 C7 C8 -4.1(9) . . . . ?
C6 S5 C7 S7 174.7(6) . . . . ?
C13 S7 C7 C8 -16(2) . . . . ?
C9 S7 C7 C8 13(2) . . . . ?
C13 S7 C7 S5 165.8(18) . . . . ?
C9 S7 C7 S5 -165(2) . . . . ?
S5 C7 C8 S8 178.0(6) . . . . ?
S7 C7 C8 S8 -0.4(16) . . . . ?
S5 C7 C8 S6 -0.5(11) . . . . ?
S7 C7 C8 S6 -179.0(6) . . . . ?
C10 S8 C8 C7 12(2) . . . . ?
C14 S8 C8 C7 -12.5(19) . . . . ?
C10 S8 C8 S6 -170(2) . . . . ?
C14 S8 C8 S6 166.0(17) . . . . ?
C6 S6 C8 C7 4.7(9) . . . . ?
C6 S6 C8 S8 -174.0(6) . . . . ?
Cu1 N1 C11 N3 0.000(18) . . . 2_456 ?
C11 N3 C12 N2 180.000(13) 2_556 . . . ?


#==============================================================================
# Additional structures and associated data_? identifiers
# should be added at this point if there is more than one 
# structure analysis in the CIF.



#==============================================================================
#     End of CIF
#==============================================================================
_chemical_name_systematic        kappa-ET2Cu[N(CN)2]I
_exptl_crystal_recrystallization_method Electrocrystallization
_exptl_crystal_preparation       Superconducting
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_No5_SC_296K
_database_code_depnum_ccdc_archive 'CCDC 2001312'
loop_
_audit_author_name
_audit_author_address
'Toshio Naito'
;Ehime University
Japan
;
_audit_update_record             
;
2020-05-06 deposited with the CCDC.	2021-12-14 downloaded from the CCDC.
;

#==============================================================================
# CHEMICAL DATA

_chemical_formula_sum            'C22 H16 Cu I N3 S16'
_chemical_formula_moiety         'C22 H16 Cu I N3 S16'
_chemical_formula_weight         1025.80
_chemical_melting_point          ?

#==============================================================================
# CRYSTAL DATA
_space_group_crystal_system      orthorhombic
_space_group_name_H-M_alt        'P n m a'
_space_group_name_Hall           '-P 2ac 2n'
_space_group_IT_number           62
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 +X,+Y,+Z
2 1/2+X,1/2-Y,1/2-Z
3 -X,1/2+Y,-Z
4 1/2-X,-Y,1/2+Z
5 -X,-Y,-Z
6 -1/2-X,-1/2+Y,-1/2+Z
7 +X,-1/2-Y,+Z
8 -1/2+X,+Y,-1/2-Z
#------------------------------------------------------------------------------
_cell_length_a                   12.9101(4)
_cell_length_b                   30.2796(10)
_cell_length_c                   8.6523(3)
_cell_angle_alpha                90.0000
_cell_angle_beta                 90.0000
_cell_angle_gamma                90.0000
_cell_volume                     3382.29(19)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    13853
_cell_measurement_theta_min      2.44
_cell_measurement_theta_max      30.27
_cell_measurement_temperature    296
#------------------------------------------------------------------------------
_exptl_crystal_description       block
_exptl_crystal_colour            black
_exptl_crystal_size_max          0.230
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.070
_exptl_crystal_density_diffrn    2.014
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2028.00
_exptl_absorpt_coefficient_mu    2.572
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_correction_T_min  0.579
_exptl_absorpt_correction_T_max  0.835

#==============================================================================
# EXPERIMENTAL DATA

_diffrn_ambient_temperature      296
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_measurement_device_type  'Rigaku Saturn724'
_diffrn_reflns_number            60985
_diffrn_reflns_av_unetI/netI     0.0483
_diffrn_reflns_av_R_equivalents  0.0879
_diffrn_reflns_theta_max         31.248
_diffrn_reflns_theta_min         2.448
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.955
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.955
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.955
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -41
_diffrn_reflns_limit_k_max       44
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_standards_number         0
_diffrn_standards_interval_count .
_diffrn_standards_decay_%        ?
_reflns_number_total             5355
_reflns_number_gt                3578
_reflns_threshold_expression     F²>2.0σ(F²)
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

#==============================================================================
# REFINEMENT DATA

_refine_special_details          
;
    Refinement was performed using all reflections. The weighted 
    R-factor (wR) and goodness of fit (S) are based on F².
    R-factor (gt) are based on F. The threshold expression of
    F² > 2.0 sigma(F²) is used only for calculating R-factor (gt).
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_R_factor_all          0.1196
_refine_ls_R_factor_gt           0.0712
_refine_ls_wR_factor_ref         0.1714
_refine_ls_wR_factor_gt          0.1525
_refine_ls_number_restraints     0
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_reflns         5355
_refine_ls_number_parameters     224
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w = 1/[σ²(Fo²)+(0.0615P)²+11.1738P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_refine_ls_shift/su_max          0.000
_refine_diff_density_max         1.48
_refine_diff_density_min         -1.15
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?

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 for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
H H 0.0000 0.0000
;
International Tables for Crystallography
(Vol. C, Table 6.1.1.4)
;
Cu Cu 0.3201 1.2651
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
I I -0.4742 1.8119
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
N N 0.0061 0.0033
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
S S 0.1246 0.1234
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;

#==============================================================================
# ATOMIC COORDINATES AND THERMAL PARAMETERS

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C9 C 0.3892(11) 0.6717(5) 0.384(3) 0.056(5) Uani 0.57(4) 1 d . . P A 1
C10 C 0.371(2) 0.6616(6) 0.2214(18) 0.065(8) Uani 0.57(4) 1 d . . P A 1
C13 C 0.4127(13) 0.6738(4) 0.300(3) 0.039(5) Uani 0.43(4) 1 d . . P A 2
C14 C 0.3149(15) 0.6485(6) 0.263(3) 0.050(6) Uani 0.43(4) 1 d . . P A 2
I1 I 0.63569(6) 0.750000 0.16116(7) 0.0625(2) Uani 1 2 d S T P . .
Cu1 Cu 0.63169(9) 0.750000 0.44631(13) 0.0565(3) Uani 1 2 d S T P . .
S1 S 0.88491(13) 0.39771(6) 0.5003(2) 0.0651(5) Uani 1 1 d . . . . .
S2 S 0.73478(12) 0.35648(5) 0.19367(17) 0.0480(4) Uani 1 1 d . . . . .
S3 S 0.74630(10) 0.47418(4) 0.48169(16) 0.0388(3) Uani 1 1 d . . . . .
S4 S 0.61906(10) 0.43898(4) 0.22968(16) 0.0396(3) Uani 1 1 d . . . . .
S5 S 0.60098(10) 0.56370(4) 0.47721(16) 0.0383(3) Uani 1 1 d . . . . .
S6 S 0.47481(11) 0.52276(4) 0.23460(16) 0.0407(3) Uani 1 1 d . . . . .
S7 S 0.50245(15) 0.65072(5) 0.45767(19) 0.0575(4) Uani 1 1 d . . . . .
S8 S 0.34990(13) 0.60079(6) 0.16881(18) 0.0552(4) Uani 1 1 d . . . . .
N1 N 0.7684(6) 0.750000 0.5477(10) 0.061(2) Uani 1 2 d S T P . .
N2 N 0.5167(6) 0.750000 0.5921(9) 0.0542(18) Uani 1 2 d S T P . .
N3 N 0.4365(7) 0.750000 0.8452(12) 0.103(4) Uani 1 2 d S T P . .
C1 C 0.9143(4) 0.3542(2) 0.3685(7) 0.0493(14) Uani 1 1 d . . . . .
H1A H 0.947826 0.366875 0.278548 0.059 Uiso 1 1 calc R U . . .
H1B H 0.963763 0.334512 0.417405 0.059 Uiso 1 1 calc R U . . .
C2 C 0.8243(5) 0.32752(19) 0.3155(7) 0.0479(14) Uani 1 1 d . . . . .
H2A H 0.787245 0.316811 0.405524 0.057 Uiso 1 1 calc R U . . .
H2B H 0.849987 0.301984 0.259722 0.057 Uiso 1 1 calc R U . . .
C3 C 0.7792(4) 0.42228(17) 0.4086(6) 0.0386(11) Uani 1 1 d . . . . .
C4 C 0.7217(4) 0.40620(16) 0.2923(6) 0.0361(11) Uani 1 1 d . . . . .
C5 C 0.6413(4) 0.48190(16) 0.3588(6) 0.0332(10) Uani 1 1 d . . . . .
C6 C 0.5805(4) 0.51857(16) 0.3581(6) 0.0342(10) Uani 1 1 d . . . . .
C7 C 0.5066(4) 0.59638(16) 0.3894(6) 0.0360(11) Uani 1 1 d . . . . .
C8 C 0.4484(4) 0.57772(16) 0.2795(6) 0.0357(11) Uani 1 1 d . . . . .
C11 C 0.8436(7) 0.750000 0.6090(11) 0.050(2) Uani 1 2 d S T P . .
C12 C 0.4694(7) 0.750000 0.7002(12) 0.049(2) Uani 1 2 d S T P . .


#==============================================================================
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_structure_solution    'SHELXT Version 2018/2 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL Version 2018/3 (Sheldrick, 2008)'
_computing_publication_material  'CrystalStructure 4.3 (Rigaku, 2019)'
_computing_molecular_graphics    'CrystalStructure 4.3'

#==============================================================================
# MOLECULAR GEOMETRY

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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C9 C10 1.46(2) . ?
C9 S7 1.718(11) . ?
C10 S8 1.916(18) . ?
C13 C14 1.51(3) . ?
C13 S7 1.920(17) . ?
C14 S8 1.722(15) . ?
I1 Cu1 2.4677(13) . ?
Cu1 N2 1.948(8) . ?
Cu1 N1 1.971(8) . ?
S1 C3 1.745(5) . ?
S1 C1 1.784(6) . ?
S2 C4 1.739(5) . ?
S2 C2 1.793(6) . ?
S3 C5 1.738(5) . ?
S3 C3 1.746(5) . ?
S4 C5 1.738(5) . ?
S4 C4 1.742(5) . ?
S5 C6 1.732(5) . ?
S5 C7 1.745(5) . ?
S6 C6 1.737(5) . ?
S6 C8 1.743(5) . ?
S7 C7 1.749(5) . ?
S8 C8 1.738(5) . ?
N1 C11 1.106(11) . ?
N2 C12 1.117(11) . ?
N3 C11 1.263(13) 2_466 ?
N3 C12 1.324(13) . ?
C1 C2 1.488(9) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 C4 1.342(7) . ?
C5 C6 1.360(7) . ?
C7 C8 1.337(7) . ?

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
C10 C9 S7 114.9(15) . . ?
C9 C10 S8 117.0(15) . . ?
C14 C13 S7 118.0(14) . . ?
C13 C14 S8 107.8(16) . . ?
N2 Cu1 N1 113.2(3) . . ?
N2 Cu1 I1 131.6(2) . . ?
N1 Cu1 I1 115.2(3) . . ?
C3 S1 C1 101.0(3) . . ?
C4 S2 C2 101.4(3) . . ?
C5 S3 C3 95.1(2) . . ?
C5 S4 C4 95.8(2) . . ?
C6 S5 C7 94.7(2) . . ?
C6 S6 C8 95.0(2) . . ?
C9 S7 C7 104.4(5) . . ?
C7 S7 C13 97.0(6) . . ?
C14 S8 C8 105.5(7) . . ?
C8 S8 C10 98.9(5) . . ?
C11 N1 Cu1 177.8(9) . . ?
C12 N2 Cu1 163.5(8) . . ?
C11 N3 C12 127.0(10) 2_466 . ?
C2 C1 S1 115.6(4) . . ?
C2 C1 H1A 108.4 . . ?
S1 C1 H1A 108.4 . . ?
C2 C1 H1B 108.4 . . ?
S1 C1 H1B 108.4 . . ?
H1A C1 H1B 107.4 . . ?
C1 C2 S2 114.8(4) . . ?
C1 C2 H2A 108.6 . . ?
S2 C2 H2A 108.6 . . ?
C1 C2 H2B 108.6 . . ?
S2 C2 H2B 108.6 . . ?
H2A C2 H2B 107.5 . . ?
C4 C3 S1 128.3(4) . . ?
C4 C3 S3 117.6(4) . . ?
S1 C3 S3 114.1(3) . . ?
C3 C4 S2 128.9(4) . . ?
C3 C4 S4 116.6(4) . . ?
S2 C4 S4 114.5(3) . . ?
C6 C5 S4 120.8(4) . . ?
C6 C5 S3 124.3(4) . . ?
S4 C5 S3 114.9(3) . . ?
C5 C6 S5 123.6(4) . . ?
C5 C6 S6 121.1(4) . . ?
S5 C6 S6 115.4(3) . . ?
C8 C7 S5 117.6(4) . . ?
C8 C7 S7 128.4(4) . . ?
S5 C7 S7 114.1(3) . . ?
C7 C8 S8 129.3(4) . . ?
C7 C8 S6 116.9(4) . . ?
S8 C8 S6 113.8(3) . . ?
N1 C11 N3 169.6(11) . 2_566 ?
N2 C12 N3 165.6(10) . . ?

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
S7 C9 C10 S8 65(3) . . . . ?
S7 C13 C14 S8 -71(3) . . . . ?
C10 C9 S7 C7 -45(2) . . . . ?
C13 C14 S8 C8 49(2) . . . . ?
C3 S1 C1 C2 -47.1(5) . . . . ?
S1 C1 C2 S2 68.2(6) . . . . ?
C4 S2 C2 C1 -45.1(5) . . . . ?
C1 S1 C3 C4 14.1(6) . . . . ?
C1 S1 C3 S3 -166.3(3) . . . . ?
C5 S3 C3 C4 0.9(5) . . . . ?
C5 S3 C3 S1 -178.8(3) . . . . ?
S1 C3 C4 S2 -1.2(8) . . . . ?
S3 C3 C4 S2 179.2(3) . . . . ?
S1 C3 C4 S4 178.7(3) . . . . ?
S3 C3 C4 S4 -0.9(6) . . . . ?
C2 S2 C4 C3 12.7(6) . . . . ?
C2 S2 C4 S4 -167.2(3) . . . . ?
C5 S4 C4 C3 0.4(5) . . . . ?
C5 S4 C4 S2 -179.7(3) . . . . ?
C4 S4 C5 C6 179.1(4) . . . . ?
C4 S4 C5 S3 0.2(3) . . . . ?
C3 S3 C5 C6 -179.4(5) . . . . ?
C3 S3 C5 S4 -0.6(3) . . . . ?
S4 C5 C6 S5 -177.1(3) . . . . ?
S3 C5 C6 S5 1.6(7) . . . . ?
S4 C5 C6 S6 3.0(6) . . . . ?
S3 C5 C6 S6 -178.2(3) . . . . ?
C7 S5 C6 C5 172.7(5) . . . . ?
C7 S5 C6 S6 -7.5(3) . . . . ?
C8 S6 C6 C5 -173.0(4) . . . . ?
C8 S6 C6 S5 7.2(3) . . . . ?
C6 S5 C7 C8 5.0(5) . . . . ?
C6 S5 C7 S7 -174.2(3) . . . . ?
C9 S7 C7 C8 12.8(10) . . . . ?
C13 S7 C7 C8 -10.6(8) . . . . ?
C9 S7 C7 S5 -168.2(9) . . . . ?
C13 S7 C7 S5 168.4(7) . . . . ?
S5 C7 C8 S8 -179.2(3) . . . . ?
S7 C7 C8 S8 -0.2(8) . . . . ?
S5 C7 C8 S6 -0.8(6) . . . . ?
S7 C7 C8 S6 178.2(3) . . . . ?
C14 S8 C8 C7 -16.6(11) . . . . ?
C10 S8 C8 C7 11.1(9) . . . . ?
C14 S8 C8 S6 164.9(10) . . . . ?
C10 S8 C8 S6 -167.3(8) . . . . ?
C6 S6 C8 C7 -3.8(5) . . . . ?
C6 S6 C8 S8 174.8(3) . . . . ?
Cu1 N2 C12 N3 0.000(14) . . . . ?
C11 N3 C12 N2 180.000(7) 2_466 . . . ?


#==============================================================================
# Additional structures and associated data_? identifiers
# should be added at this point if there is more than one 
# structure analysis in the CIF.



#==============================================================================
#     End of CIF
#==============================================================================
_chemical_name_systematic        kappa-ET2Cu[N(CN)2]I
_exptl_crystal_recrystallization_method Electrocrystallization
_exptl_crystal_preparation       Superconducting
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_296k
_database_code_depnum_ccdc_archive 'CCDC 2110351'
loop_
_audit_author_name
_audit_author_address
'Toshio Naito'
;Ehime University
Japan
;
_audit_update_record             
;
2021-10-05 deposited with the CCDC.	2021-12-14 downloaded from the CCDC.
;
_audit_creation_date             2021-09-13
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        'kappa-ET2Cu[N(CN)2]I, 296 K'
_chemical_formula_moiety         '0.5(C4 Cu2 I2 N6), 2(C10 H8 S8)'
_chemical_formula_sum            'C22 H16 Cu I N3 S16'
_chemical_formula_weight         1025.78
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 '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'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_H-M_alt        'P n m a'
_space_group_name_Hall           '-P 2ac 2n'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z'
'-x-1/2, y-1/2, z-1/2'

_cell_length_a                   12.8892(4)
_cell_length_b                   30.2507(8)
_cell_length_c                   8.6770(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3383.23(16)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    ?
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      ?
_cell_measurement_theta_min      ?
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    2.571
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_type   ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    2.014
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2028
_exptl_crystal_size_max          0.092
_exptl_crystal_size_mid          0.089
_exptl_crystal_size_min          0.018
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0609
_diffrn_reflns_av_unetI/netI     0.0327
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.966
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       43
_diffrn_reflns_limit_k_min       -44
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            60871
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.966
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.321
_diffrn_reflns_theta_min         2.442
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.966
_diffrn_measurement_device_type  'abstract diffractometer'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3753
_reflns_number_total             5446
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.899
_refine_diff_density_min         -0.987
_refine_diff_density_rms         0.095
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     240
_refine_ls_number_reflns         5446
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0754
_refine_ls_R_factor_gt           0.0420
_refine_ls_restrained_S_all      1.031
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0383P)²+4.0371P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0871
_refine_ls_wR_factor_ref         0.0998
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
2. Others
 Sof(C11)=Sof(H11A)=Sof(H11B)=Sof(C12)=Sof(H12A)=Sof(H12B)=1-FVAR(1)
 Sof(C13)=Sof(H13A)=Sof(H13B)=Sof(C14)=Sof(H14A)=Sof(H14B)=FVAR(1)
3.a Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B), C14(H14A,H14B), C11(H11A,H11B), C12(H12A,H12B)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
I1 I 0.36554(3) 0.250000 0.83947(4) 0.05448(11) Uani 1 2 d S T P . .
Cu1 Cu 0.37061(5) 0.250000 0.55452(7) 0.04768(16) Uani 1 2 d S T P . .
S3 S 0.25337(6) 0.52587(2) 0.51753(9) 0.03705(17) Uani 1 1 d . . . . .
S4 S 0.38035(6) 0.56100(2) 0.77021(9) 0.03710(17) Uani 1 1 d . . . . .
S6 S 0.39926(6) 0.43616(2) 0.52164(9) 0.03630(17) Uani 1 1 d . . . . .
S5 S 0.52516(6) 0.47709(2) 0.76521(9) 0.03860(18) Uani 1 1 d . . . . .
S2 S 0.26460(7) 0.64378(3) 0.80615(10) 0.0453(2) Uani 1 1 d . . . . .
S8 S 0.49846(8) 0.34890(3) 0.54098(11) 0.0527(2) Uani 1 1 d . . . . .
S7 S 0.65031(8) 0.39898(3) 0.83110(10) 0.0519(2) Uani 1 1 d . . . . .
S1 S 0.11481(8) 0.60264(4) 0.49847(12) 0.0619(3) Uani 1 1 d . . . . .
N1 N 0.4852(3) 0.250000 0.4079(5) 0.0454(9) Uani 1 2 d S T P . .
C3 C 0.2777(2) 0.59375(9) 0.7068(3) 0.0336(6) Uani 1 1 d . . . . .
N3 N 0.7363(3) 0.250000 0.0498(5) 0.0551(11) Uani 1 2 d S T P . .
C6 C 0.4194(2) 0.48148(9) 0.6410(3) 0.0315(6) Uani 1 1 d . . . . .
C5 C 0.3580(2) 0.51805(9) 0.6409(3) 0.0317(6) Uani 1 1 d . . . . .
C7 C 0.4938(2) 0.40325(9) 0.6092(3) 0.0330(6) Uani 1 1 d . . . . .
C4 C 0.2198(2) 0.57782(10) 0.5903(4) 0.0373(7) Uani 1 1 d . . . . .
C10 C 0.6581(4) 0.250000 0.1086(6) 0.0449(11) Uani 1 2 d S T P . .
C8 C 0.5516(2) 0.42195(9) 0.7205(3) 0.0342(6) Uani 1 1 d . . . . .
C9 C 0.5303(4) 0.250000 0.2948(6) 0.0435(10) Uani 1 2 d S T P . .
C1 C 0.1754(3) 0.67280(11) 0.6835(4) 0.0451(8) Uani 1 1 d . . . . .
C2 C 0.0847(3) 0.64640(13) 0.6304(4) 0.0454(8) Uani 1 1 d . . . . .
N2 N 0.5634(4) 0.250000 0.1539(6) 0.089(2) Uani 1 2 d S T P . .
C13 C 0.6109(6) 0.3292(3) 0.6138(13) 0.046(2) Uani 0.552(15) 1 d . . P A 2
H13A H 0.612847 0.297481 0.598098 0.055 Uiso 0.552(15) 1 calc R U P A 2
H13B H 0.668039 0.341960 0.556122 0.055 Uiso 0.552(15) 1 calc R U P A 2
C14 C 0.6274(9) 0.3385(3) 0.7810(9) 0.050(2) Uani 0.552(15) 1 d . . P A 2
H14A H 0.686653 0.321449 0.816090 0.060 Uiso 0.552(15) 1 calc R U P A 2
H14B H 0.567174 0.328190 0.837579 0.060 Uiso 0.552(15) 1 calc R U P A 2
H1A H 0.154(3) 0.6941(14) 0.736(5) 0.061(12) Uiso 1 1 d . . . . .
H2A H 0.049(3) 0.6346(12) 0.710(4) 0.054(11) Uiso 1 1 d . . . . .
H1B H 0.215(3) 0.6846(12) 0.604(4) 0.054(11) Uiso 1 1 d . . . . .
H2B H 0.037(3) 0.6624(12) 0.578(4) 0.053(11) Uiso 1 1 d . . . . .
C11 C 0.6828(8) 0.3508(3) 0.7409(12) 0.044(3) Uani 0.448(15) 1 d . . P A 1
H11A H 0.722757 0.357300 0.648923 0.053 Uiso 0.448(15) 1 calc R U P A 1
H11B H 0.725528 0.333004 0.808820 0.053 Uiso 0.448(15) 1 calc R U P A 1
C12 C 0.5866(8) 0.3253(3) 0.6974(15) 0.044(2) Uani 0.448(15) 1 d . . P A 1
H12A H 0.545271 0.321572 0.789919 0.053 Uiso 0.448(15) 1 calc R U P A 1
H12B H 0.608242 0.296035 0.664755 0.053 Uiso 0.448(15) 1 calc R U P A 1


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
I1 Cu1 2.4733(7) . ?
Cu1 N1 1.950(4) . ?
Cu1 N3 1.954(4) 6_556 ?
S3 C5 1.738(3) . ?
S3 C4 1.748(3) . ?
S4 C3 1.742(3) . ?
S4 C5 1.741(3) . ?
S6 C6 1.738(3) . ?
S6 C7 1.747(3) . ?
S5 C6 1.743(3) . ?
S5 C8 1.746(3) . ?
S2 C3 1.750(3) . ?
S2 C1 1.796(4) . ?
S8 C7 1.748(3) . ?
S8 C13 1.690(7) . ?
S8 C12 1.909(10) . ?
S7 C8 1.738(3) . ?
S7 C14 1.904(9) . ?
S7 C11 1.706(7) . ?
S1 C4 1.740(3) . ?
S1 C2 1.793(4) . ?
N1 C9 1.140(6) . ?
C3 C4 1.346(4) . ?
N3 C10 1.130(6) . ?
C6 C5 1.360(4) . ?
C7 C8 1.345(4) . ?
C10 N2 1.282(7) . ?
C9 N2 1.295(7) . ?
C1 C2 1.489(5) . ?
C1 H1A 0.83(4) . ?
C1 H1B 0.93(4) . ?
C2 H2A 0.90(4) . ?
C2 H2B 0.91(4) . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C13 C14 1.493(12) . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C11 C12 1.508(15) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Cu1 I1 132.25(13) . . ?
N1 Cu1 N3 111.67(18) . 6_556 ?
N3 Cu1 I1 116.08(13) 6_556 . ?
C5 S3 C4 95.29(14) . . ?
C5 S4 C3 95.47(14) . . ?
C6 S6 C7 94.95(14) . . ?
C6 S5 C8 95.06(14) . . ?
C3 S2 C1 101.11(15) . . ?
C7 S8 C12 97.6(3) . . ?
C13 S8 C7 103.5(3) . . ?
C8 S7 C14 98.3(3) . . ?
C11 S7 C8 105.5(3) . . ?
C4 S1 C2 101.22(16) . . ?
C9 N1 Cu1 161.4(4) . . ?
S4 C3 S2 114.19(16) . . ?
C4 C3 S4 117.1(2) . . ?
C4 C3 S2 128.7(2) . . ?
C10 N3 Cu1 179.3(4) . 6_656 ?
S6 C6 S5 115.16(16) . . ?
C5 C6 S6 123.7(2) . . ?
C5 C6 S5 121.1(2) . . ?
S3 C5 S4 115.07(16) . . ?
C6 C5 S3 124.2(2) . . ?
C6 C5 S4 120.7(2) . . ?
S6 C7 S8 114.36(17) . . ?
C8 C7 S6 117.3(2) . . ?
C8 C7 S8 128.3(2) . . ?
S1 C4 S3 114.52(17) . . ?
C3 C4 S3 117.1(2) . . ?
C3 C4 S1 128.4(2) . . ?
N3 C10 N2 171.0(6) . . ?
S7 C8 S5 113.73(17) . . ?
C7 C8 S5 116.9(2) . . ?
C7 C8 S7 129.3(2) . . ?
N1 C9 N2 168.6(5) . . ?
S2 C1 H1A 105(3) . . ?
S2 C1 H1B 106(2) . . ?
C2 C1 S2 115.1(3) . . ?
C2 C1 H1A 109(3) . . ?
C2 C1 H1B 114(2) . . ?
H1A C1 H1B 107(4) . . ?
S1 C2 H2A 108(2) . . ?
S1 C2 H2B 103(2) . . ?
C1 C2 S1 115.0(3) . . ?
C1 C2 H2A 112(2) . . ?
C1 C2 H2B 114(2) . . ?
H2A C2 H2B 105(3) . . ?
C10 N2 C9 127.1(5) . . ?
S8 C13 H13A 108.6 . . ?
S8 C13 H13B 108.6 . . ?
H13A C13 H13B 107.5 . . ?
C14 C13 S8 114.8(7) . . ?
C14 C13 H13A 108.6 . . ?
C14 C13 H13B 108.6 . . ?
S7 C14 H14A 108.5 . . ?
S7 C14 H14B 108.5 . . ?
C13 C14 S7 115.1(7) . . ?
C13 C14 H14A 108.5 . . ?
C13 C14 H14B 108.5 . . ?
H14A C14 H14B 107.5 . . ?
S7 C11 H11A 109.5 . . ?
S7 C11 H11B 109.5 . . ?
H11A C11 H11B 108.1 . . ?
C12 C11 S7 110.5(8) . . ?
C12 C11 H11A 109.5 . . ?
C12 C11 H11B 109.5 . . ?
S8 C12 H12A 107.7 . . ?
S8 C12 H12B 107.7 . . ?
C11 C12 S8 118.4(8) . . ?
C11 C12 H12A 107.7 . . ?
C11 C12 H12B 107.7 . . ?
H12A C12 H12B 107.1 . . ?

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
Cu1 N1 C9 N2 0.000(3) . . . . ?
S4 C3 C4 S3 0.6(4) . . . . ?
S4 C3 C4 S1 -178.4(2) . . . . ?
S6 C6 C5 S3 -2.3(4) . . . . ?
S6 C6 C5 S4 177.19(16) . . . . ?
S6 C7 C8 S5 0.2(3) . . . . ?
S6 C7 C8 S7 179.44(19) . . . . ?
S5 C6 C5 S3 178.13(16) . . . . ?
S5 C6 C5 S4 -2.4(4) . . . . ?
S2 C3 C4 S3 -179.33(19) . . . . ?
S2 C3 C4 S1 1.6(5) . . . . ?
S2 C1 C2 S1 -68.5(4) . . . . ?
S8 C7 C8 S5 -178.35(18) . . . . ?
S8 C7 C8 S7 0.9(5) . . . . ?
S8 C13 C14 S7 -68.7(11) . . . . ?
S7 C11 C12 S8 68.2(13) . . . . ?
N1 C9 N2 C10 180.000(2) . . . . ?
C3 S4 C5 S3 -0.09(19) . . . . ?
C3 S4 C5 C6 -179.6(3) . . . . ?
C3 S2 C1 C2 45.6(3) . . . . ?
C6 S6 C7 S8 174.22(17) . . . . ?
C6 S6 C7 C8 -4.5(3) . . . . ?
C6 S5 C8 S7 -175.13(18) . . . . ?
C6 S5 C8 C7 4.2(3) . . . . ?
C5 S3 C4 S1 178.59(19) . . . . ?
C5 S3 C4 C3 -0.6(3) . . . . ?
C5 S4 C3 S2 179.64(17) . . . . ?
C5 S4 C3 C4 -0.3(3) . . . . ?
C7 S6 C6 S5 7.31(19) . . . . ?
C7 S6 C6 C5 -172.3(3) . . . . ?
C7 S8 C13 C14 47.3(9) . . . . ?
C4 S3 C5 S4 0.35(19) . . . . ?
C4 S3 C5 C6 179.8(3) . . . . ?
C4 S1 C2 C1 47.3(3) . . . . ?
C8 S5 C6 S6 -7.25(19) . . . . ?
C8 S5 C6 C5 172.4(3) . . . . ?
C8 S7 C11 C12 -45.9(10) . . . . ?
C1 S2 C3 S4 167.1(2) . . . . ?
C1 S2 C3 C4 -12.9(4) . . . . ?
C2 S1 C4 S3 166.4(2) . . . . ?
C2 S1 C4 C3 -14.5(4) . . . . ?
C13 S8 C7 S6 167.6(4) . . . . ?
C13 S8 C7 C8 -13.8(5) . . . . ?
C14 S7 C8 S5 166.4(4) . . . . ?
C14 S7 C8 C7 -12.9(4) . . . . ?
C11 S7 C8 S5 -166.6(5) . . . . ?
C11 S7 C8 C7 14.2(6) . . . . ?
C12 S8 C7 S6 -168.0(4) . . . . ?
C12 S8 C7 C8 10.6(5) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_191119
_database_code_depnum_ccdc_archive 'CCDC 2126206'
loop_
_audit_author_name
_audit_author_address
'Toshio Naito'
;Ehime University
Japan
;
_audit_update_record             
;
2021-12-04 deposited with the CCDC.	2021-12-14 downloaded from the CCDC.
;

#==============================================================================
# CHEMICAL DATA

_chemical_formula_sum            'C22 H16 Cu I N3 S16'
_chemical_formula_moiety         'C22 H16 Cu I N3 S16'
_chemical_formula_weight         1025.80
_chemical_melting_point          ?

#==============================================================================
# CRYSTAL DATA
_space_group_crystal_system      orthorhombic
_space_group_name_H-M_alt        'P n m a'
_space_group_name_Hall           '-P 2ac 2n'
_space_group_IT_number           62
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 +X,+Y,+Z
2 1/2+X,1/2-Y,1/2-Z
3 -X,1/2+Y,-Z
4 1/2-X,-Y,1/2+Z
5 -X,-Y,-Z
6 -1/2-X,-1/2+Y,-1/2+Z
7 +X,-1/2-Y,+Z
8 -1/2+X,+Y,-1/2-Z
#------------------------------------------------------------------------------
_cell_length_a                   12.6628(2)
_cell_length_b                   30.0177(5)
_cell_length_c                   8.68694(16)
_cell_angle_alpha                90.0000
_cell_angle_beta                 90.0000
_cell_angle_gamma                90.0000
_cell_volume                     3301.98(10)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    24015
_cell_measurement_theta_min      2.94
_cell_measurement_theta_max      68.26
_cell_measurement_temperature    89
#------------------------------------------------------------------------------
_exptl_crystal_description       plate
_exptl_crystal_colour            black
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_exptl_crystal_density_diffrn    2.063
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2028.00
_exptl_absorpt_coefficient_mu    17.944
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Rigaku, 1995)'
_exptl_absorpt_correction_T_min  0.084
_exptl_absorpt_correction_T_max  0.166

#==============================================================================
# EXPERIMENTAL DATA

_diffrn_ambient_temperature      89
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54187
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean 10.000
_diffrn_reflns_number            34534
_diffrn_reflns_av_unetI/netI     0.0474
_diffrn_reflns_av_R_equivalents  0.1100
_diffrn_reflns_theta_max         68.223
_diffrn_reflns_theta_min         2.944
_diffrn_reflns_theta_full        67.687
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       10
_diffrn_standards_number         0
_diffrn_standards_interval_count .
_diffrn_standards_decay_%        ?
_reflns_number_total             3089
_reflns_number_gt                2788
_reflns_threshold_expression     F²>2.0σ(F²)
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

#==============================================================================
# REFINEMENT DATA

_refine_special_details          
;Refinement was performed using all reflections. The weighted 
    R-factor (wR) and goodness of fit (S) are based on F².
    R-factor (gt) are based on F. The threshold expression of
    F² > 2.0 sigma(F²) is used only for calculating R-factor (gt).,One of the ethylene groups is disordered
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_R_factor_all          0.0525
_refine_ls_R_factor_gt           0.0484
_refine_ls_wR_factor_ref         0.1263
_refine_ls_wR_factor_gt          0.1227
_refine_ls_number_restraints     0
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_reflns         3089
_refine_ls_number_parameters     224
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w = 1/[σ²(Fo²)+(0.0633P)²+10.8073P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_refine_ls_shift/su_max          0.000
_refine_diff_density_max         1.20
_refine_diff_density_min         -0.71
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
H H 0.0000 0.0000
;
International Tables for Crystallography
(Vol. C, Table 6.1.1.4)
;
Cu Cu -1.9646 0.5888
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
I I -0.3257 6.8362
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
N N 0.0311 0.0180
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
S S 0.3331 0.5567
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;

#==============================================================================
# ATOMIC COORDINATES AND THERMAL PARAMETERS

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C9 C 0.6209(7) 0.6710(3) 0.3908(14) 0.026(3) Uani 0.73(3) 1 d . . P A 1
C10 C 0.6339(10) 0.6626(3) 0.2216(11) 0.026(3) Uani 0.73(3) 1 d . . P A 1
C13 C 0.5937(15) 0.6756(6) 0.298(3) 0.015(7) Uani 0.27(3) 1 d . . P A 2
C14 C 0.691(2) 0.6492(7) 0.252(3) 0.021(6) Uani 0.27(3) 1 d . . P A 2
I1 I 0.37712(5) 0.750000 0.15633(6) 0.03593(19) Uani 1 2 d S T P . .
Cu1 Cu 0.38294(9) 0.750000 0.44005(14) 0.0293(3) Uani 1 2 d S T P . .
S1 S 0.11284(12) 0.39388(5) 0.50874(18) 0.0369(4) Uani 1 1 d . . . . .
S2 S 0.26159(11) 0.35473(4) 0.19297(15) 0.0238(3) Uani 1 1 d . . . . .
S3 S 0.24975(10) 0.47301(4) 0.48611(14) 0.0211(3) Uani 1 1 d . . . . .
S4 S 0.37725(10) 0.43894(4) 0.22915(15) 0.0208(3) Uani 1 1 d . . . . .
S5 S 0.39893(10) 0.56389(4) 0.48348(14) 0.0204(3) Uani 1 1 d . . . . .
S6 S 0.52488(10) 0.52295(4) 0.23658(15) 0.0220(3) Uani 1 1 d . . . . .
S7 S 0.49978(12) 0.65198(4) 0.46490(15) 0.0281(3) Uani 1 1 d . . . . .
S8 S 0.65319(11) 0.60179(5) 0.17114(16) 0.0283(3) Uani 1 1 d . . . . .
N1 N 0.5680(6) 0.750000 0.8495(9) 0.0420(19) Uani 1 2 d S T P . .
N2 N 0.4980(5) 0.750000 0.5864(9) 0.0295(15) Uani 1 2 d S T P . .
N3 N 0.2451(5) 0.750000 0.5424(8) 0.0296(15) Uani 1 2 d S T P . .
C1 C 0.0774(4) 0.35216(17) 0.3696(6) 0.0260(12) Uani 1 1 d . . . . .
H1A H 0.024911 0.331831 0.416466 0.031 Uiso 1 1 calc R U . . .
H1B H 0.043091 0.366967 0.280864 0.031 Uiso 1 1 calc R U . . .
C2 C 0.1690(5) 0.32487(17) 0.3112(6) 0.0264(12) Uani 1 1 d . . . . .
H2A H 0.140813 0.299491 0.251157 0.032 Uiso 1 1 calc R U . . .
H2B H 0.207322 0.312436 0.400809 0.032 Uiso 1 1 calc R U . . .
C3 C 0.2170(4) 0.42016(16) 0.4127(6) 0.0230(11) Uani 1 1 d . . . . .
C4 C 0.2745(4) 0.40475(16) 0.2947(6) 0.0205(10) Uani 1 1 d . . . . .
C5 C 0.3555(4) 0.48161(17) 0.3628(6) 0.0198(10) Uani 1 1 d . . . . .
C6 C 0.4184(4) 0.51841(16) 0.3628(6) 0.0181(10) Uani 1 1 d . . . . .
C7 C 0.4948(4) 0.59745(16) 0.3952(6) 0.0205(10) Uani 1 1 d . . . . .
C8 C 0.5529(4) 0.57854(16) 0.2832(6) 0.0206(10) Uani 1 1 d . . . . .
C11 C 0.5412(6) 0.750000 0.7069(10) 0.0288(18) Uani 1 2 d S T P . .
C12 C 0.1655(6) 0.750000 0.6018(9) 0.0258(16) Uani 1 2 d S T P . .


#==============================================================================
_computing_data_collection       'RAPID AUTO (Rigaku, ????)'
_computing_cell_refinement       'RAPID AUTO'
_computing_data_reduction        'RAPID AUTO'
_computing_structure_solution    'SHELXT Version 2018/2 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL Version 2018/3 (Sheldrick, 2008)'
_computing_publication_material  'CrystalStructure 4.3 (Rigaku, 2019)'
_computing_molecular_graphics    'CrystalStructure 4.3'

#==============================================================================
# MOLECULAR GEOMETRY

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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C9 C10 1.500(14) . ?
C9 S7 1.758(7) . ?
C10 S8 1.894(10) . ?
C13 C14 1.51(3) . ?
C13 S7 2.00(2) . ?
C14 S8 1.656(17) . ?
I1 Cu1 2.4658(13) . ?
Cu1 N2 1.934(7) . ?
Cu1 N3 1.959(7) . ?
S1 C3 1.749(5) . ?
S1 C1 1.798(5) . ?
S2 C4 1.750(5) . ?
S2 C2 1.798(5) . ?
S3 C5 1.735(5) . ?
S3 C3 1.759(5) . ?
S4 C5 1.750(5) . ?
S4 C4 1.752(5) . ?
S5 C6 1.739(5) . ?
S5 C7 1.754(5) . ?
S6 C6 1.743(5) . ?
S6 C8 1.753(5) . ?
S7 C7 1.746(5) . ?
S8 C8 1.746(5) . ?
N1 C11 1.285(11) . ?
N1 C12 1.305(11) 2_566 ?
N2 C11 1.181(11) . ?
N3 C12 1.132(10) . ?
C1 C2 1.508(7) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 C4 1.339(7) . ?
C5 C6 1.362(7) . ?
C7 C8 1.346(7) . ?

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
C10 C9 S7 113.6(9) . . ?
C9 C10 S8 113.7(7) . . ?
C14 C13 S7 119.2(17) . . ?
C13 C14 S8 109.3(17) . . ?
N2 Cu1 N3 111.9(3) . . ?
N2 Cu1 I1 132.8(2) . . ?
N3 Cu1 I1 115.3(2) . . ?
C3 S1 C1 100.5(2) . . ?
C4 S2 C2 101.5(2) . . ?
C5 S3 C3 95.3(2) . . ?
C5 S4 C4 95.5(2) . . ?
C6 S5 C7 95.1(2) . . ?
C6 S6 C8 94.9(2) . . ?
C7 S7 C9 102.1(3) . . ?
C7 S7 C13 95.9(7) . . ?
C14 S8 C8 108.4(8) . . ?
C8 S8 C10 99.4(3) . . ?
C11 N1 C12 124.3(8) . 2_566 ?
C11 N2 Cu1 158.7(7) . . ?
C12 N3 Cu1 179.9(7) . . ?
C2 C1 S1 114.4(4) . . ?
C2 C1 H1A 108.7 . . ?
S1 C1 H1A 108.7 . . ?
C2 C1 H1B 108.7 . . ?
S1 C1 H1B 108.7 . . ?
H1A C1 H1B 107.6 . . ?
C1 C2 S2 115.0(4) . . ?
C1 C2 H2A 108.5 . . ?
S2 C2 H2A 108.5 . . ?
C1 C2 H2B 108.5 . . ?
S2 C2 H2B 108.5 . . ?
H2A C2 H2B 107.5 . . ?
C4 C3 S1 128.2(4) . . ?
C4 C3 S3 117.4(4) . . ?
S1 C3 S3 114.3(3) . . ?
C3 C4 S2 129.2(4) . . ?
C3 C4 S4 116.7(4) . . ?
S2 C4 S4 114.1(3) . . ?
C6 C5 S3 124.9(4) . . ?
C6 C5 S4 120.1(4) . . ?
S3 C5 S4 115.0(3) . . ?
C5 C6 S5 123.6(4) . . ?
C5 C6 S6 121.0(4) . . ?
S5 C6 S6 115.3(3) . . ?
C8 C7 S7 128.8(4) . . ?
C8 C7 S5 116.9(4) . . ?
S7 C7 S5 114.3(3) . . ?
C7 C8 S8 129.2(4) . . ?
C7 C8 S6 117.2(4) . . ?
S8 C8 S6 113.5(3) . . ?
N2 C11 N1 167.8(9) . . ?
N3 C12 N1 171.8(9) . 2_466 ?

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
S7 C9 C10 S8 -70.7(12) . . . . ?
S7 C13 C14 S8 67(3) . . . . ?
C10 C9 S7 C7 50.0(10) . . . . ?
C13 C14 S8 C8 -45(2) . . . . ?
C9 C10 S8 C8 46.2(9) . . . . ?
C3 S1 C1 C2 50.4(4) . . . . ?
S1 C1 C2 S2 -68.7(5) . . . . ?
C4 S2 C2 C1 43.1(5) . . . . ?
C1 S1 C3 C4 -18.6(6) . . . . ?
C1 S1 C3 S3 162.8(3) . . . . ?
C5 S3 C3 C4 -1.8(5) . . . . ?
C5 S3 C3 S1 177.1(3) . . . . ?
S1 C3 C4 S2 2.8(8) . . . . ?
S3 C3 C4 S2 -178.5(3) . . . . ?
S1 C3 C4 S4 -177.7(3) . . . . ?
S3 C3 C4 S4 0.9(6) . . . . ?
C2 S2 C4 C3 -10.9(6) . . . . ?
C2 S2 C4 S4 169.7(3) . . . . ?
C5 S4 C4 C3 0.4(5) . . . . ?
C5 S4 C4 S2 179.9(3) . . . . ?
C3 S3 C5 C6 -179.1(5) . . . . ?
C3 S3 C5 S4 2.0(3) . . . . ?
C4 S4 C5 C6 179.4(4) . . . . ?
C4 S4 C5 S3 -1.6(3) . . . . ?
S3 C5 C6 S5 -2.5(7) . . . . ?
S4 C5 C6 S5 176.3(3) . . . . ?
S3 C5 C6 S6 178.4(3) . . . . ?
S4 C5 C6 S6 -2.8(6) . . . . ?
C7 S5 C6 C5 -172.0(5) . . . . ?
C7 S5 C6 S6 7.2(3) . . . . ?
C8 S6 C6 C5 172.4(4) . . . . ?
C8 S6 C6 S5 -6.8(3) . . . . ?
C9 S7 C7 C8 -15.2(7) . . . . ?
C13 S7 C7 C8 10.6(8) . . . . ?
C9 S7 C7 S5 165.8(5) . . . . ?
C13 S7 C7 S5 -168.3(7) . . . . ?
C6 S5 C7 C8 -4.9(4) . . . . ?
C6 S5 C7 S7 174.2(3) . . . . ?
S7 C7 C8 S8 0.5(8) . . . . ?
S5 C7 C8 S8 179.5(3) . . . . ?
S7 C7 C8 S6 -178.0(3) . . . . ?
S5 C7 C8 S6 0.9(6) . . . . ?
C14 S8 C8 C7 14.4(12) . . . . ?
C10 S8 C8 C7 -12.0(6) . . . . ?
C14 S8 C8 S6 -167.0(11) . . . . ?
C10 S8 C8 S6 166.6(4) . . . . ?
C6 S6 C8 C7 3.5(4) . . . . ?
C6 S6 C8 S8 -175.2(3) . . . . ?
Cu1 N2 C11 N1 0.000(11) . . . . ?
C12 N1 C11 N2 180.000(7) 2_566 . . . ?


#==============================================================================
# Additional structures and associated data_? identifiers
# should be added at this point if there is more than one 
# structure analysis in the CIF.



#==============================================================================
#     End of CIF
#==============================================================================
_chemical_name_systematic        
'kappa-ET2Cu[N(CN)2]I, 100 K, slow cooling (-1 K/min)'
_exptl_crystal_recrystallization_method Electrocrystallization
_exptl_crystal_preparation       'Conducting properties'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_No3_Ins_100K
_database_code_depnum_ccdc_archive 'CCDC 2001308'
loop_
_audit_author_name
_audit_author_address
'Toshio Naito'
;Ehime University
Japan
;
_audit_update_record             
;
2020-05-06 deposited with the CCDC.	2021-12-14 downloaded from the CCDC.
;

#==============================================================================
# CHEMICAL DATA

_chemical_formula_sum            'C22 H16 Cu I N3 S16'
_chemical_formula_moiety         'C22 H16 Cu I N3 S16'
_chemical_formula_weight         1025.80
_chemical_melting_point          ?

#==============================================================================
# CRYSTAL DATA
_space_group_crystal_system      orthorhombic
_space_group_name_H-M_alt        'P n m a'
_space_group_name_Hall           '-P 2ac 2n'
_space_group_IT_number           62
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 +X,+Y,+Z
2 1/2+X,1/2-Y,1/2-Z
3 -X,1/2+Y,-Z
4 1/2-X,-Y,1/2+Z
5 -X,-Y,-Z
6 -1/2-X,-1/2+Y,-1/2+Z
7 +X,-1/2-Y,+Z
8 -1/2+X,+Y,-1/2-Z
#------------------------------------------------------------------------------
_cell_length_a                   12.6806(3)
_cell_length_b                   29.9198(5)
_cell_length_c                   8.65985(16)
_cell_angle_alpha                90.0000
_cell_angle_beta                 90.0000
_cell_angle_gamma                90.0000
_cell_volume                     3285.56(11)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    44211
_cell_measurement_theta_min      2.43
_cell_measurement_theta_max      31.35
_cell_measurement_temperature    100
#------------------------------------------------------------------------------
_exptl_crystal_description       block
_exptl_crystal_colour            black
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.140
_exptl_crystal_size_min          0.030
_exptl_crystal_density_diffrn    2.074
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2028.00
_exptl_absorpt_coefficient_mu    2.647
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_correction_T_min  0.772
_exptl_absorpt_correction_T_max  0.924

#==============================================================================
# EXPERIMENTAL DATA

_diffrn_ambient_temperature      100
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_measurement_device_type  'Rigaku Saturn724'
_diffrn_reflns_number            94646
_diffrn_reflns_av_unetI/netI     0.0217
_diffrn_reflns_av_R_equivalents  0.0825
_diffrn_reflns_theta_max         26.499
_diffrn_reflns_theta_min         2.448
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       10
_diffrn_standards_number         0
_diffrn_standards_interval_count .
_diffrn_standards_decay_%        ?
_reflns_number_total             3467
_reflns_number_gt                3202
_reflns_threshold_expression     F²>2.0σ(F²)
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

#==============================================================================
# REFINEMENT DATA

_refine_special_details          
;
    Refinement was performed using all reflections. The weighted 
    R-factor (wR) and goodness of fit (S) are based on F².
    R-factor (gt) are based on F. The threshold expression of
    F² > 2.0 sigma(F²) is used only for calculating R-factor (gt).
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_R_factor_all          0.0476
_refine_ls_R_factor_gt           0.0421
_refine_ls_wR_factor_ref         0.1066
_refine_ls_wR_factor_gt          0.1036
_refine_ls_number_restraints     0
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_reflns         3467
_refine_ls_number_parameters     224
_refine_ls_goodness_of_fit_ref   1.101
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w = 1/[σ²(Fo²)+(0.0445P)²+19.6819P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_refine_ls_shift/su_max          0.001
_refine_diff_density_max         0.85
_refine_diff_density_min         -1.84
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?

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 for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
H H 0.0000 0.0000
;
International Tables for Crystallography
(Vol. C, Table 6.1.1.4)
;
Cu Cu 0.3201 1.2651
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
I I -0.4742 1.8119
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
N N 0.0061 0.0033
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
S S 0.1246 0.1234
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;

#==============================================================================
# ATOMIC COORDINATES AND THERMAL PARAMETERS

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C9 C 0.6195(6) 0.6714(3) -0.1079(14) 0.017(3) Uani 0.63(2) 1 d . . P A 1
C10 C 0.6323(9) 0.6632(3) -0.2799(10) 0.017(3) Uani 0.63(2) 1 d . . P A 1
C13 C 0.5910(12) 0.6765(4) -0.201(2) 0.018(5) Uani 0.37(2) 1 d . . P A 2
C14 C 0.6873(15) 0.6503(5) -0.2480(17) 0.017(4) Uani 0.37(2) 1 d . . P A 2
I1 I 0.87581(5) 0.750000 0.84259(6) 0.03224(16) Uani 1 2 d S T P . .
Cu1 Cu 0.88158(6) 0.750000 0.56081(10) 0.0205(2) Uani 1 2 d S T P . .
S1 S 0.11230(10) 0.39454(5) 0.00756(15) 0.0288(3) Uani 1 1 d . . . . .
S2 S 0.26202(9) 0.35457(3) -0.30700(13) 0.0156(2) Uani 1 1 d . . . . .
S3 S 0.25018(8) 0.47327(3) -0.01397(12) 0.0124(2) Uani 1 1 d . . . . .
S4 S 0.37815(8) 0.43869(3) -0.27055(12) 0.0124(2) Uani 1 1 d . . . . .
S5 S 0.39956(8) 0.56416(3) -0.01705(12) 0.0122(2) Uani 1 1 d . . . . .
S6 S 0.52546(8) 0.52286(3) -0.26391(12) 0.0133(2) Uani 1 1 d . . . . .
S7 S 0.50113(10) 0.65223(4) -0.03569(13) 0.0207(3) Uani 1 1 d . . . . .
S8 S 0.65380(9) 0.60168(4) -0.33022(14) 0.0208(3) Uani 1 1 d . . . . .
N1 N 0.9965(4) 0.750000 0.4121(8) 0.0238(13) Uani 1 2 d S T P . .
N2 N 0.7439(4) 0.750000 0.4590(7) 0.0212(12) Uani 1 2 d S T P . .
N3 N 0.5670(5) 0.750000 0.3502(8) 0.0315(15) Uani 1 2 d S T P . .
C1 C 0.0779(3) 0.35201(15) -0.1291(5) 0.0176(9) Uani 1 1 d . . . . .
H1A H 0.025603 0.331756 -0.081036 0.021 Uiso 1 1 calc R U . . .
H1B H 0.043783 0.366297 -0.219231 0.021 Uiso 1 1 calc R U . . .
C2 C 0.1704(4) 0.32441(15) -0.1853(6) 0.0189(10) Uani 1 1 d . . . . .
H2A H 0.143042 0.298420 -0.243525 0.023 Uiso 1 1 calc R U . . .
H2B H 0.209125 0.312781 -0.094469 0.023 Uiso 1 1 calc R U . . .
C3 C 0.2171(3) 0.42023(14) -0.0871(5) 0.0158(9) Uani 1 1 d . . . . .
C4 C 0.2755(3) 0.40472(14) -0.2050(5) 0.0130(8) Uani 1 1 d . . . . .
C5 C 0.3563(3) 0.48155(13) -0.1380(5) 0.0106(8) Uani 1 1 d . . . . .
C6 C 0.4187(3) 0.51838(14) -0.1383(5) 0.0110(8) Uani 1 1 d . . . . .
C7 C 0.4959(3) 0.59751(14) -0.1060(5) 0.0128(8) Uani 1 1 d . . . . .
C8 C 0.5540(3) 0.57849(13) -0.2188(5) 0.0113(8) Uani 1 1 d . . . . .
C11 C 1.0396(5) 0.750000 0.2908(8) 0.0194(14) Uani 1 2 d S T P . .
C12 C 0.6649(5) 0.750000 0.3989(8) 0.0189(14) Uani 1 2 d S T P . .


#==============================================================================
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_structure_solution    'SHELXT Version 2018/2 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL Version 2018/3 (Sheldrick, 2008)'
_computing_publication_material  'CrystalStructure 4.3 (Rigaku, 2019)'
_computing_molecular_graphics    'CrystalStructure 4.3'

#==============================================================================
# MOLECULAR GEOMETRY

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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C9 C10 1.519(13) . ?
C9 S7 1.724(7) . ?
C10 S8 1.911(9) . ?
C13 C14 1.51(2) . ?
C13 S7 1.969(16) . ?
C14 S8 1.673(12) . ?
I1 Cu1 2.4413(10) . ?
Cu1 N1 1.945(6) . ?
Cu1 N2 1.955(6) . ?
S1 C3 1.740(5) . ?
S1 C1 1.791(5) . ?
S2 C4 1.750(4) . ?
S2 C2 1.809(4) . ?
S3 C5 1.739(4) . ?
S3 C3 1.759(4) . ?
S4 C5 1.743(4) . ?
S4 C4 1.747(4) . ?
S5 C6 1.743(4) . ?
S5 C7 1.755(4) . ?
S6 C6 1.742(4) . ?
S6 C8 1.747(4) . ?
S7 C7 1.748(4) . ?
S8 C8 1.737(4) . ?
N1 C11 1.184(9) . ?
N2 C12 1.129(9) . ?
N3 C11 1.270(10) 2_465 ?
N3 C12 1.312(9) . ?
C1 C2 1.515(6) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 C4 1.344(6) . ?
C5 C6 1.357(6) . ?
C7 C8 1.349(6) . ?

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
C10 C9 S7 113.2(8) . . ?
C9 C10 S8 113.3(7) . . ?
C14 C13 S7 118.3(12) . . ?
C13 C14 S8 111.2(13) . . ?
N1 Cu1 N2 111.7(3) . . ?
N1 Cu1 I1 133.17(19) . . ?
N2 Cu1 I1 115.08(18) . . ?
C3 S1 C1 100.9(2) . . ?
C4 S2 C2 101.3(2) . . ?
C5 S3 C3 95.2(2) . . ?
C5 S4 C4 95.5(2) . . ?
C6 S5 C7 94.9(2) . . ?
C6 S6 C8 95.4(2) . . ?
C9 S7 C7 102.6(3) . . ?
C7 S7 C13 96.5(4) . . ?
C14 S8 C8 107.2(5) . . ?
C8 S8 C10 98.9(3) . . ?
C11 N1 Cu1 158.9(6) . . ?
C12 N2 Cu1 179.3(6) . . ?
C11 N3 C12 124.6(7) 2_465 . ?
C2 C1 S1 114.3(3) . . ?
C2 C1 H1A 108.7 . . ?
S1 C1 H1A 108.7 . . ?
C2 C1 H1B 108.7 . . ?
S1 C1 H1B 108.7 . . ?
H1A C1 H1B 107.6 . . ?
C1 C2 S2 114.4(3) . . ?
C1 C2 H2A 108.7 . . ?
S2 C2 H2A 108.7 . . ?
C1 C2 H2B 108.7 . . ?
S2 C2 H2B 108.7 . . ?
H2A C2 H2B 107.6 . . ?
C4 C3 S1 128.8(3) . . ?
C4 C3 S3 117.0(3) . . ?
S1 C3 S3 114.3(2) . . ?
C3 C4 S4 117.2(3) . . ?
C3 C4 S2 128.8(3) . . ?
S4 C4 S2 114.1(2) . . ?
C6 C5 S3 124.6(3) . . ?
C6 C5 S4 120.2(3) . . ?
S3 C5 S4 115.1(2) . . ?
C5 C6 S6 121.1(3) . . ?
C5 C6 S5 123.8(3) . . ?
S6 C6 S5 115.1(2) . . ?
C8 C7 S7 128.8(3) . . ?
C8 C7 S5 117.2(3) . . ?
S7 C7 S5 114.0(2) . . ?
C7 C8 S8 129.2(3) . . ?
C7 C8 S6 116.8(3) . . ?
S8 C8 S6 114.0(2) . . ?
N1 C11 N3 168.4(7) . 2_565 ?
N2 C12 N3 171.3(8) . . ?

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
S7 C9 C10 S8 -71.3(11) . . . . ?
S7 C13 C14 S8 66.4(19) . . . . ?
C10 C9 S7 C7 50.0(9) . . . . ?
C13 C14 S8 C8 -44.1(16) . . . . ?
C3 S1 C1 C2 49.7(4) . . . . ?
S1 C1 C2 S2 -69.2(4) . . . . ?
C4 S2 C2 C1 44.7(4) . . . . ?
C1 S1 C3 C4 -17.3(5) . . . . ?
C1 S1 C3 S3 163.6(3) . . . . ?
C5 S3 C3 C4 -1.5(4) . . . . ?
C5 S3 C3 S1 177.7(3) . . . . ?
S1 C3 C4 S4 -178.3(3) . . . . ?
S3 C3 C4 S4 0.7(5) . . . . ?
S1 C3 C4 S2 2.8(7) . . . . ?
S3 C3 C4 S2 -178.2(3) . . . . ?
C5 S4 C4 C3 0.5(4) . . . . ?
C5 S4 C4 S2 179.6(2) . . . . ?
C2 S2 C4 C3 -12.4(5) . . . . ?
C2 S2 C4 S4 168.7(3) . . . . ?
C3 S3 C5 C6 -179.5(4) . . . . ?
C3 S3 C5 S4 1.8(3) . . . . ?
C4 S4 C5 C6 179.7(4) . . . . ?
C4 S4 C5 S3 -1.5(3) . . . . ?
S3 C5 C6 S6 178.3(2) . . . . ?
S4 C5 C6 S6 -3.0(5) . . . . ?
S3 C5 C6 S5 -1.9(6) . . . . ?
S4 C5 C6 S5 176.8(2) . . . . ?
C8 S6 C6 C5 172.6(4) . . . . ?
C8 S6 C6 S5 -7.2(3) . . . . ?
C7 S5 C6 C5 -172.5(4) . . . . ?
C7 S5 C6 S6 7.4(3) . . . . ?
C9 S7 C7 C8 -15.1(6) . . . . ?
C13 S7 C7 C8 11.6(7) . . . . ?
C9 S7 C7 S5 166.0(5) . . . . ?
C13 S7 C7 S5 -167.2(6) . . . . ?
C6 S5 C7 C8 -4.7(4) . . . . ?
C6 S5 C7 S7 174.2(2) . . . . ?
S7 C7 C8 S8 0.7(6) . . . . ?
S5 C7 C8 S8 179.5(3) . . . . ?
S7 C7 C8 S6 -178.3(2) . . . . ?
S5 C7 C8 S6 0.5(5) . . . . ?
C14 S8 C8 C7 12.6(9) . . . . ?
C10 S8 C8 C7 -12.9(5) . . . . ?
C14 S8 C8 S6 -168.4(8) . . . . ?
C10 S8 C8 S6 166.1(4) . . . . ?
C6 S6 C8 C7 4.0(4) . . . . ?
C6 S6 C8 S8 -175.1(2) . . . . ?
Cu1 N1 C11 N3 0.000(3) . . . 2_565 ?


#==============================================================================
# Additional structures and associated data_? identifiers
# should be added at this point if there is more than one 
# structure analysis in the CIF.



#==============================================================================
#     End of CIF
#==============================================================================
_chemical_name_systematic        kappa-ET2Cu[N(CN)2]I
_exptl_crystal_recrystallization_method Electrocrystallization
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_191210
_database_code_depnum_ccdc_archive 'CCDC 2126205'
loop_
_audit_author_name
_audit_author_address
'Toshio Naito'
;Ehime University
Japan
;
_audit_update_record             
;
2021-12-04 deposited with the CCDC.	2021-12-14 downloaded from the CCDC.
;

#==============================================================================
# CHEMICAL DATA

_chemical_formula_sum            'C22 H16 Cu I N3 S16'
_chemical_formula_moiety         'C22 H16 Cu I N3 S16'
_chemical_formula_weight         1025.80
_chemical_melting_point          ?

#==============================================================================
# CRYSTAL DATA
_space_group_crystal_system      orthorhombic
_space_group_name_H-M_alt        'P n m a'
_space_group_name_Hall           '-P 2ac 2n'
_space_group_IT_number           62
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 +X,+Y,+Z
2 1/2+X,1/2-Y,1/2-Z
3 -X,1/2+Y,-Z
4 1/2-X,-Y,1/2+Z
5 -X,-Y,-Z
6 -1/2-X,-1/2+Y,-1/2+Z
7 +X,-1/2-Y,+Z
8 -1/2+X,+Y,-1/2-Z
#------------------------------------------------------------------------------
_cell_length_a                   12.7066(5)
_cell_length_b                   29.9277(10)
_cell_length_c                   8.6211(3)
_cell_angle_alpha                90.0000
_cell_angle_beta                 90.0000
_cell_angle_gamma                90.0000
_cell_volume                     3278.4(2)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    15446
_cell_measurement_theta_min      2.43
_cell_measurement_theta_max      30.95
_cell_measurement_temperature    100
#------------------------------------------------------------------------------
_exptl_crystal_description       block
_exptl_crystal_colour            black
_exptl_crystal_size_max          0.140
_exptl_crystal_size_mid          0.070
_exptl_crystal_size_min          0.050
_exptl_crystal_density_diffrn    2.078
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2028.00
_exptl_absorpt_coefficient_mu    2.653
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_correction_T_min  0.589
_exptl_absorpt_correction_T_max  0.876

#==============================================================================
# EXPERIMENTAL DATA

_diffrn_ambient_temperature      100
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_measurement_device_type  ?
_diffrn_reflns_number            58803
_diffrn_reflns_av_unetI/netI     0.0915
_diffrn_reflns_av_R_equivalents  0.1478
_diffrn_reflns_theta_max         31.261
_diffrn_reflns_theta_min         2.459
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.965
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.965
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.965
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -41
_diffrn_reflns_limit_k_max       43
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_standards_number         0
_diffrn_standards_interval_count .
_diffrn_standards_decay_%        ?
_reflns_number_total             5260
_reflns_number_gt                3511
_reflns_threshold_expression     F²>2.0σ(F²)
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

#==============================================================================
# REFINEMENT DATA

_refine_special_details          
;Refinement was performed using all reflections. The weighted 
    R-factor (wR) and goodness of fit (S) are based on F².
    R-factor (gt) are based on F. The threshold expression of
    F² > 2.0 sigma(F²) is used only for calculating R-factor (gt).,One of the ethylene groups is disordered
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_R_factor_all          0.1314
_refine_ls_R_factor_gt           0.0782
_refine_ls_wR_factor_ref         0.1974
_refine_ls_wR_factor_gt          0.1756
_refine_ls_number_restraints     0
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_reflns         5260
_refine_ls_number_parameters     224
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w = 1/[σ²(Fo²)+(0.0770P)²+30.8003P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_refine_ls_shift/su_max          0.001
_refine_diff_density_max         2.04
_refine_diff_density_min         -3.06
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?

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 for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
H H 0.0000 0.0000
;
International Tables for Crystallography
(Vol. C, Table 6.1.1.4)
;
Cu Cu 0.3201 1.2651
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
I I -0.4742 1.8119
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
N N 0.0061 0.0033
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
S S 0.1246 0.1234
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;

#==============================================================================
# ATOMIC COORDINATES AND THERMAL PARAMETERS

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C9 C 0.3802(9) 0.3287(4) 0.6054(15) 0.014(3) Uani 0.54(3) 1 d . . P A 1
C10 C 0.3683(11) 0.3368(4) 0.7811(15) 0.014(3) Uani 0.54(3) 1 d . . P A 1
C13 C 0.4090(12) 0.3239(5) 0.701(2) 0.016(4) Uani 0.46(3) 1 d . . P A 2
C14 C 0.3137(15) 0.3487(6) 0.745(2) 0.023(4) Uani 0.46(3) 1 d . . P A 2
I1 I 0.62588(8) 0.250000 0.84169(9) 0.0399(3) Uani 1 2 d S T P . .
Cu1 Cu 0.61971(10) 0.250000 0.56138(16) 0.0244(3) Uani 1 2 d S T P . .
S1 S 0.88792(15) 0.60501(7) 0.4934(2) 0.0306(5) Uani 1 1 d . . . . .
S2 S 0.73751(13) 0.64545(5) 0.80739(19) 0.0167(3) Uani 1 1 d . . . . .
S3 S 0.74926(12) 0.52667(5) 0.51403(18) 0.0134(3) Uani 1 1 d . . . . .
S4 S 0.62108(12) 0.56148(5) 0.77067(18) 0.0135(3) Uani 1 1 d . . . . .
S5 S 0.60002(12) 0.43564(5) 0.51735(18) 0.0135(3) Uani 1 1 d . . . . .
S6 S 0.47413(12) 0.47724(5) 0.76458(19) 0.0147(3) Uani 1 1 d . . . . .
S7 S 0.49861(16) 0.34770(5) 0.5364(2) 0.0223(4) Uani 1 1 d . . . . .
S8 S 0.34597(14) 0.39856(6) 0.8318(2) 0.0221(4) Uani 1 1 d . . . . .
N1 N 0.7614(7) 0.250000 0.4642(10) 0.0230(19) Uani 1 2 d S T P . .
N2 N 0.5048(6) 0.250000 0.4117(12) 0.026(2) Uani 1 2 d S T P . .
N3 N 0.4343(7) 0.250000 0.1486(13) 0.037(2) Uani 1 2 d S T P . .
C1 C 0.9208(5) 0.6485(2) 0.6290(9) 0.0197(14) Uani 1 1 d . . . . .
H1A H 0.954421 0.635082 0.718610 0.024 Uiso 1 1 calc R U . . .
H1B H 0.971388 0.668415 0.580869 0.024 Uiso 1 1 calc R U . . .
C2 C 0.8278(5) 0.6756(2) 0.6832(8) 0.0192(14) Uani 1 1 d . . . . .
H2A H 0.789581 0.686228 0.592995 0.023 Uiso 1 1 calc R U . . .
H2B H 0.853515 0.701571 0.738810 0.023 Uiso 1 1 calc R U . . .
C3 C 0.7824(5) 0.5796(2) 0.5861(8) 0.0175(13) Uani 1 1 d . . . . .
C4 C 0.7243(5) 0.5951(2) 0.7057(7) 0.0139(12) Uani 1 1 d . . . . .
C5 C 0.6430(5) 0.5183(2) 0.6388(7) 0.0122(11) Uani 1 1 d . . . . .
C6 C 0.5811(5) 0.4816(2) 0.6380(7) 0.0120(11) Uani 1 1 d . . . . .
C7 C 0.5034(5) 0.4027(2) 0.6070(7) 0.0132(12) Uani 1 1 d . . . . .
C8 C 0.4459(5) 0.42186(19) 0.7189(7) 0.0121(12) Uani 1 1 d . . . . .
C11 C 0.8364(8) 0.250000 0.4003(12) 0.021(2) Uani 1 2 d S T P . .
C12 C 0.4584(9) 0.250000 0.2879(14) 0.027(2) Uani 1 2 d S T P . .


#==============================================================================
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_structure_solution    'SHELXT Version 2018/2 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL Version 2018/3 (Sheldrick, 2008)'
_computing_publication_material  'CrystalStructure 4.3 (Rigaku, 2019)'
_computing_molecular_graphics    'CrystalStructure 4.3'

#==============================================================================
# MOLECULAR GEOMETRY

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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C9 C10 1.541(18) . ?
C9 S7 1.715(11) . ?
C10 S8 1.921(13) . ?
C13 C14 1.47(2) . ?
C13 S7 1.953(15) . ?
C14 S8 1.719(16) . ?
I1 Cu1 2.4179(16) . ?
Cu1 N2 1.948(9) . ?
Cu1 N1 1.986(8) . ?
S1 C3 1.737(7) . ?
S1 C1 1.798(7) . ?
S2 C4 1.752(6) . ?
S2 C2 1.810(6) . ?
S3 C5 1.745(6) . ?
S3 C3 1.753(6) . ?
S4 C5 1.743(6) . ?
S4 C4 1.745(6) . ?
S5 C6 1.742(6) . ?
S5 C7 1.753(6) . ?
S6 C8 1.741(6) . ?
S6 C6 1.748(6) . ?
S7 C7 1.757(6) . ?
S8 C8 1.746(6) . ?
N1 C11 1.100(13) . ?
N2 C12 1.220(15) . ?
N3 C12 1.240(16) . ?
N3 C11 1.313(14) 2_455 ?
C1 C2 1.508(9) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 C4 1.349(9) . ?
C5 C6 1.350(8) . ?
C7 C8 1.338(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
C10 C9 S7 112.0(9) . . ?
C9 C10 S8 112.9(9) . . ?
C14 C13 S7 118.8(12) . . ?
C13 C14 S8 110.8(12) . . ?
N2 Cu1 N1 113.6(4) . . ?
N2 Cu1 I1 133.3(3) . . ?
N1 Cu1 I1 113.1(3) . . ?
C3 S1 C1 101.3(3) . . ?
C4 S2 C2 101.2(3) . . ?
C5 S3 C3 95.6(3) . . ?
C5 S4 C4 95.6(3) . . ?
C6 S5 C7 94.8(3) . . ?
C8 S6 C6 95.2(3) . . ?
C9 S7 C7 102.7(5) . . ?
C7 S7 C13 96.4(5) . . ?
C14 S8 C8 106.0(6) . . ?
C8 S8 C10 98.6(4) . . ?
C11 N1 Cu1 174.9(9) . . ?
C12 N2 Cu1 160.4(9) . . ?
C12 N3 C11 123.0(10) . 2_455 ?
C2 C1 S1 114.1(5) . . ?
C2 C1 H1A 108.7 . . ?
S1 C1 H1A 108.7 . . ?
C2 C1 H1B 108.7 . . ?
S1 C1 H1B 108.7 . . ?
H1A C1 H1B 107.6 . . ?
C1 C2 S2 114.3(5) . . ?
C1 C2 H2A 108.7 . . ?
S2 C2 H2A 108.7 . . ?
C1 C2 H2B 108.7 . . ?
S2 C2 H2B 108.7 . . ?
H2A C2 H2B 107.6 . . ?
C4 C3 S1 128.6(5) . . ?
C4 C3 S3 116.7(5) . . ?
S1 C3 S3 114.7(4) . . ?
C3 C4 S4 117.3(5) . . ?
C3 C4 S2 128.7(5) . . ?
S4 C4 S2 114.0(3) . . ?
C6 C5 S4 120.9(5) . . ?
C6 C5 S3 124.3(5) . . ?
S4 C5 S3 114.8(3) . . ?
C5 C6 S5 124.4(5) . . ?
C5 C6 S6 120.7(5) . . ?
S5 C6 S6 114.9(3) . . ?
C8 C7 S5 117.4(5) . . ?
C8 C7 S7 129.2(5) . . ?
S5 C7 S7 113.5(4) . . ?
C7 C8 S6 117.3(5) . . ?
C7 C8 S8 128.9(5) . . ?
S6 C8 S8 113.8(4) . . ?
N1 C11 N3 168.6(12) . 2 ?
N2 C12 N3 165.4(12) . . ?

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
S7 C9 C10 S8 72.6(12) . . . . ?
S7 C13 C14 S8 -67.8(17) . . . . ?
C10 C9 S7 C7 -51.2(10) . . . . ?
C13 C14 S8 C8 44.8(15) . . . . ?
C3 S1 C1 C2 -48.5(6) . . . . ?
S1 C1 C2 S2 69.5(6) . . . . ?
C4 S2 C2 C1 -45.8(6) . . . . ?
C1 S1 C3 C4 14.9(8) . . . . ?
C1 S1 C3 S3 -164.4(4) . . . . ?
C5 S3 C3 C4 2.0(6) . . . . ?
C5 S3 C3 S1 -178.6(4) . . . . ?
S1 C3 C4 S4 178.9(4) . . . . ?
S3 C3 C4 S4 -1.9(8) . . . . ?
S1 C3 C4 S2 -0.7(10) . . . . ?
S3 C3 C4 S2 178.5(4) . . . . ?
C5 S4 C4 C3 0.7(6) . . . . ?
C5 S4 C4 S2 -179.7(4) . . . . ?
C2 S2 C4 C3 12.2(7) . . . . ?
C2 S2 C4 S4 -167.4(4) . . . . ?
C4 S4 C5 C6 -179.8(5) . . . . ?
C4 S4 C5 S3 0.7(4) . . . . ?
C3 S3 C5 C6 179.0(6) . . . . ?
C3 S3 C5 S4 -1.5(4) . . . . ?
S4 C5 C6 S5 -176.9(3) . . . . ?
S3 C5 C6 S5 2.5(8) . . . . ?
S4 C5 C6 S6 2.4(8) . . . . ?
S3 C5 C6 S6 -178.2(3) . . . . ?
C7 S5 C6 C5 172.3(6) . . . . ?
C7 S5 C6 S6 -7.1(4) . . . . ?
C8 S6 C6 C5 -172.5(5) . . . . ?
C8 S6 C6 S5 6.9(4) . . . . ?
C6 S5 C7 C8 4.6(6) . . . . ?
C6 S5 C7 S7 -174.2(4) . . . . ?
C9 S7 C7 C8 16.1(8) . . . . ?
C13 S7 C7 C8 -11.4(8) . . . . ?
C9 S7 C7 S5 -165.3(5) . . . . ?
C13 S7 C7 S5 167.2(6) . . . . ?
S5 C7 C8 S6 -0.6(7) . . . . ?
S7 C7 C8 S6 178.0(4) . . . . ?
S5 C7 C8 S8 -179.0(4) . . . . ?
S7 C7 C8 S8 -0.5(10) . . . . ?
C6 S6 C8 C7 -3.8(5) . . . . ?
C6 S6 C8 S8 174.9(4) . . . . ?
C14 S8 C8 C7 -12.8(10) . . . . ?
C10 S8 C8 C7 12.7(8) . . . . ?
C14 S8 C8 S6 168.7(8) . . . . ?
C10 S8 C8 S6 -165.8(5) . . . . ?
Cu1 N2 C12 N3 0.000(6) . . . . ?
C11 N3 C12 N2 180.000(3) 2_455 . . . ?


#==============================================================================
# Additional structures and associated data_? identifiers
# should be added at this point if there is more than one 
# structure analysis in the CIF.



#==============================================================================
#     End of CIF
#==============================================================================
_chemical_name_systematic        
'kappa-ET2Cu[N(CN)2]I, 100 K, slow cooling (-1 K/min)'
_exptl_crystal_recrystallization_method Electrocrystallization
_exptl_crystal_preparation       'Conducting properties'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_100k_rapid_autored
_database_code_depnum_ccdc_archive 'CCDC 2110353'
loop_
_audit_author_name
_audit_author_address
'Toshio Naito'
;Ehime University
Japan
;
_audit_update_record             
;
2021-09-17 deposited with the CCDC.	2021-12-14 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        
'kappa-ET2Cu[N(CN)2]I, 100 K, rapid cooling (-10 K/min)'
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C22 H16 Cu I N3 S16'
_chemical_formula_weight         1025.78

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'

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

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   12.6697(3)
_cell_length_b                   29.9957(6)
_cell_length_c                   8.7154(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3312.17(13)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            black
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    2.057
_exptl_crystal_F_000             2028
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.07
_exptl_absorpt_coefficient_mu    2.626
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_measurement_device_type  
'dtrek-CrysAlisPro-abstract goniometer imported rigaku-d*trek images'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            56045
_diffrn_reflns_av_unetI/netI     0.0324
_diffrn_reflns_av_R_equivalents  0.0597
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -42
_diffrn_reflns_limit_k_max       43
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         2.434
_diffrn_reflns_theta_max         31.265
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.938
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.938
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.938
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             5155
_reflns_number_gt                4346
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0208P)²+7.7501P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5155
_refine_ls_number_parameters     224
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0502
_refine_ls_R_factor_gt           0.0367
_refine_ls_wR_factor_ref         0.0732
_refine_ls_wR_factor_gt          0.0688
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_restrained_S_all      1.062
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
I1 I 0.87713(3) 0.250000 0.15618(3) 0.02699(8) Uani 1 2 d S T P . .
Cu1 Cu 0.88287(4) 0.250000 0.43955(5) 0.01977(11) Uani 1 2 d S T P . .
S6 S 0.37724(5) 0.56108(2) 1.27075(7) 0.01515(12) Uani 1 1 d . . . . .
S3 S 0.39871(5) 0.43611(2) 1.01659(7) 0.01470(12) Uani 1 1 d . . . . .
S4 S 0.52490(5) 0.47699(2) 1.26301(7) 0.01617(13) Uani 1 1 d . . . . .
S5 S 0.24971(5) 0.52704(2) 1.01383(7) 0.01512(12) Uani 1 1 d . . . . .
S8 S 0.26164(5) 0.64521(2) 1.30690(8) 0.01833(14) Uani 1 1 d . . . . .
S1 S 0.49956(6) 0.34796(2) 1.03507(8) 0.02225(15) Uani 1 1 d . . . . .
S2 S 0.65297(6) 0.39800(2) 1.32831(8) 0.02282(15) Uani 1 1 d . . . . .
S7 S 0.11311(6) 0.60612(3) 0.99120(9) 0.03113(19) Uani 1 1 d . . . . .
N1 N 0.7463(3) 0.250000 0.5429(4) 0.0230(7) Uani 1 2 d S T P . .
N3 N 0.4982(3) 0.250000 0.9122(4) 0.0201(7) Uani 1 2 d S T P . .
N2 N 0.5680(3) 0.250000 0.6513(4) 0.0323(9) Uani 1 2 d S T P . .
C14 C 0.5393(3) 0.250000 0.7928(5) 0.0189(8) Uani 1 2 d S T P . .
C8 C 0.35562(19) 0.51859(8) 1.1378(3) 0.0134(5) Uani 1 1 d . . . . .
C13 C 0.6653(3) 0.250000 0.6024(4) 0.0184(7) Uani 1 2 d S T P . .
C7 C 0.4182(2) 0.48162(8) 1.1374(3) 0.0136(5) Uani 1 1 d . . . . .
C10 C 0.2748(2) 0.59518(8) 1.2050(3) 0.0155(5) Uani 1 1 d . . . . .
C5 C 0.5524(2) 0.42134(8) 1.2178(3) 0.0152(5) Uani 1 1 d . . . . .
C6 C 0.4945(2) 0.40267(8) 1.1048(3) 0.0147(5) Uani 1 1 d . . . . .
C9 C 0.2174(2) 0.57983(8) 1.0862(3) 0.0174(5) Uani 1 1 d . . . . .
C11 C 0.0777(2) 0.64776(9) 1.1303(3) 0.0187(5) Uani 1 1 d . . . . .
H11A H 0.025796 0.667548 1.084959 0.022 Uiso 1 1 calc R U . . .
H11B H 0.044663 0.633130 1.217161 0.022 Uiso 1 1 calc R U . . .
C12 C 0.1689(2) 0.67531(9) 1.1878(3) 0.0196(5) Uani 1 1 d . . . . .
H12A H 0.141215 0.700257 1.246024 0.024 Uiso 1 1 calc R U . . .
H12B H 0.206502 0.687380 1.100127 0.024 Uiso 1 1 calc R U . . .
C1 C 0.6331(4) 0.33777(13) 1.2795(5) 0.0175(10) Uani 0.708(9) 1 d . . P A 2
H1A H 0.693390 0.320915 1.316057 0.021 Uiso 0.708(9) 1 calc R U P A 2
H1B H 0.571173 0.326934 1.333285 0.021 Uiso 0.708(9) 1 calc R U P A 2
C2 C 0.6193(3) 0.32904(12) 1.1095(5) 0.0163(10) Uani 0.708(9) 1 d . . P A 2
H2A H 0.624779 0.297213 1.091416 0.020 Uiso 0.708(9) 1 calc R U P A 2
H2B H 0.676547 0.343386 1.054469 0.020 Uiso 0.708(9) 1 calc R U P A 2
C3 C 0.5920(8) 0.3248(3) 1.1996(13) 0.019(3) Uani 0.292(9) 1 d . . P A 1
H3A H 0.548692 0.320962 1.290419 0.022 Uiso 0.292(9) 1 calc R U P A 1
H3B H 0.615114 0.295271 1.168616 0.022 Uiso 0.292(9) 1 calc R U P A 1
C4 C 0.6883(10) 0.3504(3) 1.2466(12) 0.020(3) Uani 0.292(9) 1 d . . P A 1
H4A H 0.731625 0.356388 1.157201 0.024 Uiso 0.292(9) 1 calc R U P A 1
H4B H 0.729609 0.332806 1.318168 0.024 Uiso 0.292(9) 1 calc R U P A 1


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
I1 Cu1 2.4708(5) . ?
Cu1 N3 1.950(3) 6_657 ?
Cu1 N1 1.951(3) . ?
S6 C8 1.744(2) . ?
S6 C10 1.749(3) . ?
S3 C7 1.741(2) . ?
S3 C6 1.752(3) . ?
S4 C7 1.745(3) . ?
S4 C5 1.750(3) . ?
S5 C8 1.741(3) . ?
S5 C9 1.753(3) . ?
S8 C10 1.752(2) . ?
S8 C12 1.809(3) . ?
S1 C2 1.745(4) . ?
S1 C6 1.751(2) . ?
S1 C3 1.978(10) . ?
S2 C4 1.658(9) . ?
S2 C5 1.744(3) . ?
S2 C1 1.873(4) . ?
S7 C9 1.747(3) . ?
S7 C11 1.798(3) . ?
N1 C13 1.150(5) . ?
N3 C14 1.164(5) . ?
N2 C14 1.286(5) . ?
N2 C13 1.304(5) . ?
C8 C7 1.363(3) . ?
C10 C9 1.346(4) . ?
C5 C6 1.350(4) . ?
C11 C12 1.507(4) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C1 C2 1.514(6) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 C4 1.498(16) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N3 Cu1 N1 111.00(15) 6_657 . ?
N3 Cu1 I1 133.18(11) 6_657 . ?
N1 Cu1 I1 115.82(10) . . ?
C8 S6 C10 95.33(12) . . ?
C7 S3 C6 94.89(12) . . ?
C7 S4 C5 95.10(12) . . ?
C8 S5 C9 95.06(12) . . ?
C10 S8 C12 101.44(13) . . ?
C2 S1 C6 101.99(15) . . ?
C6 S1 C3 95.7(3) . . ?
C4 S2 C5 107.8(3) . . ?
C5 S2 C1 99.40(16) . . ?
C9 S7 C11 100.52(12) . . ?
C13 N1 Cu1 179.3(3) . . ?
C14 N3 Cu1 158.1(3) . 6_557 ?
C14 N2 C13 125.5(4) . . ?
N3 C14 N2 169.8(4) . . ?
C7 C8 S5 124.41(19) . . ?
C7 C8 S6 120.30(19) . . ?
S5 C8 S6 115.28(14) . . ?
N1 C13 N2 172.3(4) . . ?
C8 C7 S3 123.82(19) . . ?
C8 C7 S4 120.92(19) . . ?
S3 C7 S4 115.27(14) . . ?
C9 C10 S6 116.94(19) . . ?
C9 C10 S8 129.1(2) . . ?
S6 C10 S8 113.92(14) . . ?
C6 C5 S2 129.3(2) . . ?
C6 C5 S4 116.84(19) . . ?
S2 C5 S4 113.83(15) . . ?
C5 C6 S1 128.4(2) . . ?
C5 C6 S3 117.34(19) . . ?
S1 C6 S3 114.19(15) . . ?
C10 C9 S7 128.2(2) . . ?
C10 C9 S5 117.3(2) . . ?
S7 C9 S5 114.44(14) . . ?
C12 C11 S7 114.45(19) . . ?
C12 C11 H11A 108.6 . . ?
S7 C11 H11A 108.6 . . ?
C12 C11 H11B 108.6 . . ?
S7 C11 H11B 108.6 . . ?
H11A C11 H11B 107.6 . . ?
C11 C12 S8 114.52(19) . . ?
C11 C12 H12A 108.6 . . ?
S8 C12 H12A 108.6 . . ?
C11 C12 H12B 108.6 . . ?
S8 C12 H12B 108.6 . . ?
H12A C12 H12B 107.6 . . ?
C2 C1 S2 113.9(3) . . ?
C2 C1 H1A 108.8 . . ?
S2 C1 H1A 108.8 . . ?
C2 C1 H1B 108.8 . . ?
S2 C1 H1B 108.8 . . ?
H1A C1 H1B 107.7 . . ?
C1 C2 S1 114.0(3) . . ?
C1 C2 H2A 108.7 . . ?
S1 C2 H2A 108.7 . . ?
C1 C2 H2B 108.7 . . ?
S1 C2 H2B 108.7 . . ?
H2A C2 H2B 107.6 . . ?
C4 C3 S1 120.0(7) . . ?
C4 C3 H3A 107.3 . . ?
S1 C3 H3A 107.3 . . ?
C4 C3 H3B 107.3 . . ?
S1 C3 H3B 107.3 . . ?
H3A C3 H3B 106.9 . . ?
C3 C4 S2 109.8(8) . . ?
C3 C4 H4A 109.7 . . ?
S2 C4 H4A 109.7 . . ?
C3 C4 H4B 109.7 . . ?
S2 C4 H4B 109.7 . . ?
H4A C4 H4B 108.2 . . ?

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
Cu1 N3 C14 N2 0.000(6) 6_557 . . . ?
C13 N2 C14 N3 180.000(4) . . . . ?
C9 S5 C8 C7 -179.0(2) . . . . ?
C9 S5 C8 S6 2.24(17) . . . . ?
C10 S6 C8 C7 179.5(2) . . . . ?
C10 S6 C8 S5 -1.69(17) . . . . ?
S5 C8 C7 S3 -2.3(3) . . . . ?
S6 C8 C7 S3 176.37(14) . . . . ?
S5 C8 C7 S4 178.21(14) . . . . ?
S6 C8 C7 S4 -3.1(3) . . . . ?
C6 S3 C7 C8 -172.2(2) . . . . ?
C6 S3 C7 S4 7.32(16) . . . . ?
C5 S4 C7 C8 172.2(2) . . . . ?
C5 S4 C7 S3 -7.34(16) . . . . ?
C8 S6 C10 C9 0.2(2) . . . . ?
C8 S6 C10 S8 179.81(15) . . . . ?
C12 S8 C10 C9 -10.8(3) . . . . ?
C12 S8 C10 S6 169.63(15) . . . . ?
C4 S2 C5 C6 12.9(6) . . . . ?
C1 S2 C5 C6 -13.3(3) . . . . ?
C4 S2 C5 S4 -167.1(5) . . . . ?
C1 S2 C5 S4 166.69(19) . . . . ?
C7 S4 C5 C6 4.4(2) . . . . ?
C7 S4 C5 S2 -175.63(15) . . . . ?
S2 C5 C6 S1 1.7(4) . . . . ?
S4 C5 C6 S1 -178.34(15) . . . . ?
S2 C5 C6 S3 -179.97(16) . . . . ?
S4 C5 C6 S3 0.0(3) . . . . ?
C2 S1 C6 C5 -15.4(3) . . . . ?
C3 S1 C6 C5 10.1(4) . . . . ?
C2 S1 C6 S3 166.2(2) . . . . ?
C3 S1 C6 S3 -168.3(3) . . . . ?
C7 S3 C6 C5 -4.4(2) . . . . ?
C7 S3 C6 S1 174.17(15) . . . . ?
S6 C10 C9 S7 -178.13(17) . . . . ?
S8 C10 C9 S7 2.3(4) . . . . ?
S6 C10 C9 S5 1.4(3) . . . . ?
S8 C10 C9 S5 -178.17(16) . . . . ?
C11 S7 C9 C10 -18.1(3) . . . . ?
C11 S7 C9 S5 162.39(16) . . . . ?
C8 S5 C9 C10 -2.2(2) . . . . ?
C8 S5 C9 S7 177.40(16) . . . . ?
C9 S7 C11 C12 50.8(2) . . . . ?
S7 C11 C12 S8 -69.2(2) . . . . ?
C10 S8 C12 C11 43.4(2) . . . . ?
C5 S2 C1 C2 46.5(4) . . . . ?
S2 C1 C2 S1 -70.6(4) . . . . ?
C6 S1 C2 C1 49.3(4) . . . . ?
S1 C3 C4 S2 66.8(11) . . . . ?
C5 S2 C4 C3 -44.0(9) . . . . ?

_refine_diff_density_max         0.643
_refine_diff_density_min         -0.907
_refine_diff_density_rms         0.120


_exptl_crystal_recrystallization_method Electrocrystallization
_exptl_crystal_preparation       'Conducting properties'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_100k
_database_code_depnum_ccdc_archive 'CCDC 2110352'
loop_
_audit_author_name
_audit_author_address
'Toshio Naito'
;Ehime University
Japan
;
_audit_update_record             
;
2021-10-05 deposited with the CCDC.	2021-12-14 downloaded from the CCDC.
;
_audit_creation_date             2021-09-13
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        
'kappa-ET2Cu[N(CN)2]I, 100 K, slow cooling (-1 K/min)'
_chemical_formula_moiety         '0.5(C2 Cu I N3), C10 H8 S8'
_chemical_formula_sum            'C11 H8 Cu0.50 I0.50 N1.50 S8'
_chemical_formula_weight         512.89
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 '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'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_H-M_alt        'P n m a'
_space_group_name_Hall           '-P 2ac 2n'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z'
'-x-1/2, y-1/2, z-1/2'

_cell_length_a                   12.6735(2)
_cell_length_b                   30.0068(5)
_cell_length_c                   8.71810(10)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3315.42(9)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    ?
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      ?
_cell_measurement_theta_min      ?
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    2.623
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_type   ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    2.055
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2028
_exptl_crystal_size_max          0.092
_exptl_crystal_size_mid          0.089
_exptl_crystal_size_min          0.018
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0476
_diffrn_reflns_av_unetI/netI     0.0248
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.970
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       43
_diffrn_reflns_limit_k_min       -43
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            60759
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.208
_diffrn_reflns_theta_min         2.433
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measurement_device_type  'abstract diffractometer'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4317
_reflns_number_total             5316
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.766
_refine_diff_density_min         -0.754
_refine_diff_density_rms         0.106
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     240
_refine_ls_number_reflns         5316
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0466
_refine_ls_R_factor_gt           0.0315
_refine_ls_restrained_S_all      1.063
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0316P)²+3.8541P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0676
_refine_ls_wR_factor_ref         0.0730
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
2. Others
 Sof(C13)=Sof(H13A)=Sof(H13B)=Sof(C14)=Sof(H14A)=Sof(H14B)=1-FVAR(1)
 Sof(C1)=Sof(H1A)=Sof(H1B)=Sof(C2)=Sof(H2A)=Sof(H2B)=FVAR(1)
3.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C13(H13A,H13B), C14(H14A,H14B)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
I1 I 0.37739(2) 0.250000 0.84371(3) 0.02869(7) Uani 1 2 d S T P . .
Cu1 Cu 0.38314(3) 0.250000 0.56037(5) 0.02161(9) Uani 1 2 d S T P . .
N1 N 0.4984(2) 0.250000 0.4118(4) 0.0227(6) Uani 1 2 d S T P . .
N2 N 0.5686(2) 0.250000 0.1503(4) 0.0339(8) Uani 1 2 d S T P . .
N3 N 0.7464(2) 0.250000 0.0434(3) 0.0256(6) Uani 1 2 d S T P . .
C11 C 0.5395(2) 0.250000 0.2936(4) 0.0201(6) Uani 1 2 d S T P . .
C12 C 0.6651(3) 0.250000 0.1026(4) 0.0188(6) Uani 1 2 d S T P . .
S1 S 0.50039(5) 0.65204(2) 0.46481(7) 0.02398(13) Uani 1 1 d . . . . .
S2 S 0.34695(5) 0.60193(2) 0.17175(7) 0.02450(13) Uani 1 1 d . . . . .
S3 S 0.60131(4) 0.56390(2) 0.48341(6) 0.01655(11) Uani 1 1 d . . . . .
S4 S 0.47523(4) 0.52303(2) 0.23690(7) 0.01830(11) Uani 1 1 d . . . . .
S5 S 0.75032(4) 0.47300(2) 0.48612(6) 0.01683(11) Uani 1 1 d . . . . .
S6 S 0.62292(4) 0.43891(2) 0.22925(6) 0.01678(11) Uani 1 1 d . . . . .
S7 S 0.88712(5) 0.39387(2) 0.50862(8) 0.03277(16) Uani 1 1 d . . . . .
S8 S 0.73854(5) 0.35475(2) 0.19315(7) 0.02009(12) Uani 1 1 d . . . . .
C1 C 0.3803(3) 0.67092(11) 0.3912(5) 0.0183(9) Uani 0.707(8) 1 d . . P A 1
H1A H 0.323253 0.656327 0.445767 0.022 Uiso 0.707(8) 1 calc R U P A 1
H1B H 0.374492 0.702683 0.409993 0.022 Uiso 0.707(8) 1 calc R U P A 1
C2 C 0.3672(3) 0.66238(12) 0.2204(4) 0.0189(9) Uani 0.707(8) 1 d . . P A 1
H2A H 0.429435 0.673108 0.167199 0.023 Uiso 0.707(8) 1 calc R U P A 1
H2B H 0.307200 0.679317 0.183346 0.023 Uiso 0.707(8) 1 calc R U P A 1
C3 C 0.50559(17) 0.59734(7) 0.3959(2) 0.0167(4) Uani 1 1 d . . . . .
C4 C 0.44749(17) 0.57868(7) 0.2828(2) 0.0164(4) Uani 1 1 d . . . . .
C5 C 0.58170(16) 0.51846(7) 0.3629(2) 0.0155(4) Uani 1 1 d . . . . .
C6 C 0.64429(16) 0.48148(7) 0.3620(2) 0.0157(4) Uani 1 1 d . . . . .
C7 C 0.78286(17) 0.42018(7) 0.4141(3) 0.0190(4) Uani 1 1 d . . . . .
C8 C 0.72529(17) 0.40479(7) 0.2949(3) 0.0167(4) Uani 1 1 d . . . . .
C9 C 0.92292(18) 0.35220(8) 0.3696(3) 0.0201(4) Uani 1 1 d . . . . .
C10 C 0.8314(2) 0.32469(8) 0.3119(3) 0.0213(5) Uani 1 1 d . . . . .
C13 C 0.4073(7) 0.6752(3) 0.3045(11) 0.019(2) Uani 0.293(8) 1 d . . P A 2
H13A H 0.382893 0.704207 0.338508 0.022 Uiso 0.293(8) 1 calc R U P A 2
H13B H 0.450574 0.680232 0.214392 0.022 Uiso 0.293(8) 1 calc R U P A 2
C14 C 0.3112(8) 0.6495(3) 0.2526(10) 0.022(2) Uani 0.293(8) 1 d . . P A 2
H14A H 0.271535 0.667243 0.179593 0.027 Uiso 0.293(8) 1 calc R U P A 2
H14B H 0.266073 0.643515 0.339988 0.027 Uiso 0.293(8) 1 calc R U P A 2
H10A H 0.857(3) 0.3010(12) 0.244(4) 0.044(9) Uiso 1 1 d . . . . .
H9A H 0.960(2) 0.3652(8) 0.294(3) 0.015(6) Uiso 1 1 d . . . . .
H9B H 0.974(2) 0.3346(9) 0.417(3) 0.024(7) Uiso 1 1 d . . . . .
H10B H 0.796(3) 0.3117(11) 0.390(4) 0.039(9) Uiso 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
I1 Cu1 2.4713(5) . ?
Cu1 N1 1.952(3) . ?
Cu1 N3 1.954(3) 6_556 ?
N1 C11 1.155(4) . ?
N2 C11 1.302(5) . ?
N2 C12 1.292(4) . ?
N3 C12 1.153(4) . ?
S1 C1 1.746(3) . ?
S1 C3 1.749(2) . ?
S1 C13 1.957(8) . ?
S2 C2 1.880(4) . ?
S2 C4 1.746(2) . ?
S2 C14 1.656(8) . ?
S3 C3 1.749(2) . ?
S3 C5 1.739(2) . ?
S4 C4 1.753(2) . ?
S4 C5 1.746(2) . ?
S5 C6 1.744(2) . ?
S5 C7 1.754(2) . ?
S6 C6 1.745(2) . ?
S6 C8 1.749(2) . ?
S7 C7 1.746(2) . ?
S7 C9 1.799(2) . ?
S8 C8 1.752(2) . ?
S8 C10 1.809(2) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C1 C2 1.520(5) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 C4 1.353(3) . ?
C5 C6 1.364(3) . ?
C7 C8 1.351(3) . ?
C9 C10 1.509(3) . ?
C9 H9A 0.90(3) . ?
C9 H9B 0.93(3) . ?
C10 H10A 0.98(4) . ?
C10 H10B 0.91(3) . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C13 C14 1.510(13) . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Cu1 I1 133.25(9) . . ?
N1 Cu1 N3 110.87(13) . 6_556 ?
N3 Cu1 I1 115.88(9) 6_556 . ?
C11 N1 Cu1 158.4(3) . . ?
C12 N2 C11 125.2(3) . . ?
C12 N3 Cu1 179.1(3) . 6_656 ?
N1 C11 N2 169.6(4) . . ?
N3 C12 N2 172.1(4) . . ?
C1 S1 C3 102.19(14) . . ?
C3 S1 C13 96.4(2) . . ?
C4 S2 C2 99.26(13) . . ?
C14 S2 C4 108.0(3) . . ?
C5 S3 C3 95.01(10) . . ?
C5 S4 C4 94.95(10) . . ?
C6 S5 C7 95.21(10) . . ?
C6 S6 C8 95.52(10) . . ?
C7 S7 C9 100.79(11) . . ?
C8 S8 C10 101.53(11) . . ?
S1 C1 H1A 108.8 . . ?
S1 C1 H1B 108.8 . . ?
H1A C1 H1B 107.7 . . ?
C2 C1 S1 113.6(3) . . ?
C2 C1 H1A 108.8 . . ?
C2 C1 H1B 108.8 . . ?
S2 C2 H2A 108.9 . . ?
S2 C2 H2B 108.9 . . ?
C1 C2 S2 113.5(3) . . ?
C1 C2 H2A 108.9 . . ?
C1 C2 H2B 108.9 . . ?
H2A C2 H2B 107.7 . . ?
S1 C3 S3 114.50(12) . . ?
C4 C3 S1 128.20(17) . . ?
C4 C3 S3 117.27(16) . . ?
S2 C4 S4 113.63(13) . . ?
C3 C4 S2 129.52(17) . . ?
C3 C4 S4 116.85(17) . . ?
S3 C5 S4 115.40(12) . . ?
C6 C5 S3 123.94(17) . . ?
C6 C5 S4 120.65(16) . . ?
S5 C6 S6 115.11(12) . . ?
C5 C6 S5 124.26(17) . . ?
C5 C6 S6 120.62(17) . . ?
S7 C7 S5 114.69(12) . . ?
C8 C7 S5 117.21(17) . . ?
C8 C7 S7 128.10(17) . . ?
S6 C8 S8 114.01(12) . . ?
C7 C8 S6 116.89(16) . . ?
C7 C8 S8 129.10(17) . . ?
S7 C9 H9A 109.1(16) . . ?
S7 C9 H9B 105.7(18) . . ?
C10 C9 S7 114.26(17) . . ?
C10 C9 H9A 113.2(16) . . ?
C10 C9 H9B 111.6(17) . . ?
H9A C9 H9B 102(2) . . ?
S8 C10 H10A 103(2) . . ?
S8 C10 H10B 109(2) . . ?
C9 C10 S8 114.71(17) . . ?
C9 C10 H10A 110.3(19) . . ?
C9 C10 H10B 112(2) . . ?
H10A C10 H10B 108(3) . . ?
S1 C13 H13A 107.0 . . ?
S1 C13 H13B 107.0 . . ?
H13A C13 H13B 106.8 . . ?
C14 C13 S1 121.3(6) . . ?
C14 C13 H13A 107.0 . . ?
C14 C13 H13B 107.0 . . ?
S2 C14 H14A 109.6 . . ?
S2 C14 H14B 109.6 . . ?
C13 C14 S2 110.3(7) . . ?
C13 C14 H14A 109.6 . . ?
C13 C14 H14B 109.6 . . ?
H14A C14 H14B 108.1 . . ?

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
Cu1 N1 C11 N2 0.000(2) . . . . ?
C12 N2 C11 N1 180.000(1) . . . . ?
S1 C1 C2 S2 71.2(3) . . . . ?
S1 C3 C4 S2 -1.7(3) . . . . ?
S1 C3 C4 S4 177.99(13) . . . . ?
S1 C13 C14 S2 -64.3(10) . . . . ?
S3 C3 C4 S2 -179.79(13) . . . . ?
S3 C3 C4 S4 -0.1(2) . . . . ?
S3 C5 C6 S5 2.6(3) . . . . ?
S3 C5 C6 S6 -176.29(12) . . . . ?
S4 C5 C6 S5 -178.31(12) . . . . ?
S4 C5 C6 S6 2.8(3) . . . . ?
S5 C7 C8 S6 -1.4(3) . . . . ?
S5 C7 C8 S8 178.17(14) . . . . ?
S7 C7 C8 S6 178.24(14) . . . . ?
S7 C7 C8 S8 -2.2(4) . . . . ?
S7 C9 C10 S8 69.0(2) . . . . ?
C1 S1 C3 S3 -166.05(17) . . . . ?
C1 S1 C3 C4 15.8(3) . . . . ?
C2 S2 C4 S4 -166.33(16) . . . . ?
C2 S2 C4 C3 13.4(3) . . . . ?
C3 S1 C1 C2 -50.1(3) . . . . ?
C3 S3 C5 S4 -7.03(14) . . . . ?
C3 S3 C5 C6 172.1(2) . . . . ?
C4 S2 C2 C1 -46.8(3) . . . . ?
C4 S2 C14 C13 42.5(8) . . . . ?
C4 S4 C5 S3 7.00(14) . . . . ?
C4 S4 C5 C6 -172.12(19) . . . . ?
C5 S3 C3 S1 -174.06(13) . . . . ?
C5 S3 C3 C4 4.27(19) . . . . ?
C5 S4 C4 S2 175.62(13) . . . . ?
C5 S4 C4 C3 -4.14(19) . . . . ?
C6 S5 C7 S7 -177.51(14) . . . . ?
C6 S5 C7 C8 2.2(2) . . . . ?
C6 S6 C8 S8 -179.80(13) . . . . ?
C6 S6 C8 C7 -0.2(2) . . . . ?
C7 S5 C6 S6 -2.23(14) . . . . ?
C7 S5 C6 C5 178.8(2) . . . . ?
C7 S7 C9 C10 -50.6(2) . . . . ?
C8 S6 C6 S5 1.66(14) . . . . ?
C8 S6 C6 C5 -179.31(19) . . . . ?
C8 S8 C10 C9 -43.3(2) . . . . ?
C9 S7 C7 S5 -162.26(14) . . . . ?
C9 S7 C7 C8 18.1(3) . . . . ?
C10 S8 C8 S6 -169.76(13) . . . . ?
C10 S8 C8 C7 10.6(3) . . . . ?
C13 S1 C3 S3 168.9(3) . . . . ?
C13 S1 C3 C4 -9.2(4) . . . . ?
C14 S2 C4 S4 167.3(4) . . . . ?
C14 S2 C4 C3 -13.0(5) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_exptl_crystal_recrystallization_method Electrocrystallization
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_100k_2
_database_code_depnum_ccdc_archive 'CCDC 2110365'
loop_
_audit_author_name
_audit_author_address
'Toshio Naito'
;Ehime University
Japan
;
_audit_update_record             
;
2021-09-17 deposited with the CCDC.	2021-12-14 downloaded from the CCDC.
;
_audit_creation_date             2021-09-14
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        
'kappa-ET2Cu[N(CN)2]I, 100 K, rapid cooling (-10 K/min)'
_chemical_formula_moiety         '0.5(C4 Cu2 I2 N6), 2(C10 H8 S8)'
_chemical_formula_sum            'C22 H16 Cu I N3 S16'
_chemical_formula_weight         1025.78
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C22 H8 N3 S16 Cu I'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_H-M_alt        'P n m a'
_space_group_name_Hall           '-P 2ac 2n'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z'
'-x-1/2, y-1/2, z-1/2'

_cell_length_a                   12.6853(2)
_cell_length_b                   30.0090(5)
_cell_length_c                   8.71030(10)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3315.78(9)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    34883
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.2610
_cell_measurement_theta_min      2.4120
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    2.623
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.86167
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.67a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    2.055
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2028
_exptl_crystal_size_max          0.092
_exptl_crystal_size_mid          0.089
_exptl_crystal_size_min          0.018
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0457
_diffrn_reflns_av_unetI/netI     0.0231
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.963
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       42
_diffrn_reflns_limit_k_min       -42
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            61056
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.963
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.290
_diffrn_reflns_theta_min         2.435
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.963
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -110.00  70.00   0.50    1.00    --  -20.00  45.00   0.00  360
  2  ω   -110.00  70.00   0.50    1.00    --  -20.00  45.00  90.00  360
  3  ω   -110.00  70.00   0.50    1.00    --  -20.00  45.00 180.00  360
  4  ω   -110.00  70.00   0.50    1.00    --  -20.00  45.00 270.00  360
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  
'dtrek-CrysAlisPro-abstract goniometer imported rigaku-d*trek images'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0370164000
_diffrn_orient_matrix_UB_12      0.0002470000
_diffrn_orient_matrix_UB_13      -0.0609979000
_diffrn_orient_matrix_UB_21      0.0374831000
_diffrn_orient_matrix_UB_22      -0.0107499000
_diffrn_orient_matrix_UB_23      0.0477078000
_diffrn_orient_matrix_UB_31      -0.0187055000
_diffrn_orient_matrix_UB_32      -0.0210619000
_diffrn_orient_matrix_UB_33      -0.0251210000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4403
_reflns_number_total             5318
_reflns_odcompleteness_completeness 96.38
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     31.22
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         1.180
_refine_diff_density_min         -1.439
_refine_diff_density_rms         0.116
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.909
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     224
_refine_ls_number_reflns         5318
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0464
_refine_ls_R_factor_gt           0.0333
_refine_ls_restrained_S_all      0.909
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1000P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1073
_refine_ls_wR_factor_ref         0.1190
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
2. Others
 Sof(C8)=Sof(H8A)=Sof(H8B)=Sof(C10)=Sof(H10A)=Sof(H10B)=1-FVAR(1)
 Sof(C3)=Sof(H3A)=Sof(H3B)=Sof(C4)=Sof(H4A)=Sof(H4B)=FVAR(1)
3.a Secondary CH2 refined with riding coordinates:
 C00M(H00A,H00B), C00N(H00C,H00D), C3(H3A,H3B), C4(H4A,H4B), C8(H8A,H8B),
 C10(H10A,H10B)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
I001 I 0.37703(2) 0.250000 0.84368(3) 0.02904(9) Uani 1 2 d S T P . .
Cu02 Cu 0.38290(3) 0.250000 0.56012(5) 0.02167(12) Uani 1 2 d S T P . .
S003 S 0.37723(4) 0.56112(2) 0.77082(7) 0.01706(13) Uani 1 1 d . . . . .
S004 S 0.39884(4) 0.43602(2) 0.51677(7) 0.01652(13) Uani 1 1 d . . . . .
S005 S 0.52487(5) 0.47703(2) 0.76319(7) 0.01832(13) Uani 1 1 d . . . . .
S006 S 0.24987(4) 0.52692(2) 0.51403(7) 0.01719(13) Uani 1 1 d . . . . .
S007 S 0.26144(5) 0.64521(2) 0.80703(7) 0.02038(14) Uani 1 1 d . . . . .
S008 S 0.65302(5) 0.39810(2) 0.82852(8) 0.02476(15) Uani 1 1 d . . . . .
S009 S 0.49978(6) 0.34794(2) 0.53536(7) 0.02434(15) Uani 1 1 d . . . . .
S00A S 0.11303(6) 0.60599(3) 0.49149(9) 0.03342(19) Uani 1 1 d . . . . .
N00B N 0.7465(3) 0.250000 0.0436(4) 0.0255(6) Uani 1 2 d S T P . .
N00C N 0.4982(2) 0.250000 0.4121(4) 0.0229(6) Uani 1 2 d S T P . .
N00D N 0.5684(3) 0.250000 0.1492(4) 0.0360(9) Uani 1 2 d S T P . .
C00E C 0.35569(17) 0.51858(8) 0.6386(3) 0.0154(4) Uani 1 1 d . . . . .
C00F C 0.6654(3) 0.250000 0.1028(4) 0.0180(6) Uani 1 2 d S T P . .
C00G C 0.41886(17) 0.48147(8) 0.6380(3) 0.0164(4) Uani 1 1 d . . . . .
C00H C 0.5397(3) 0.250000 0.2934(4) 0.0201(7) Uani 1 2 d S T P . .
C00I C 0.27527(19) 0.59513(8) 0.7053(3) 0.0170(4) Uani 1 1 d . . . . .
C00J C 0.55279(18) 0.42154(8) 0.7177(3) 0.0171(4) Uani 1 1 d . . . . .
C00K C 0.49468(18) 0.40255(7) 0.6044(3) 0.0173(4) Uani 1 1 d . . . . .
C00L C 0.21715(18) 0.57985(8) 0.5863(3) 0.0188(5) Uani 1 1 d . . . . .
C00M C 0.1684(2) 0.67528(8) 0.6879(3) 0.0219(5) Uani 1 1 d . . . . .
H00A H 0.140791 0.700201 0.746289 0.026 Uiso 1 1 calc R U . . .
H00B H 0.205814 0.687358 0.600132 0.026 Uiso 1 1 calc R U . . .
C00N C 0.07656(18) 0.64760(8) 0.6301(3) 0.0208(5) Uani 1 1 d . . . . .
H00C H 0.024843 0.667335 0.584239 0.025 Uiso 1 1 calc R U . . .
H00D H 0.043386 0.633002 0.716925 0.025 Uiso 1 1 calc R U . . .
C3 C 0.6190(3) 0.32915(12) 0.6083(5) 0.0173(9) Uani 0.692(9) 1 d . . P A 2
H3A H 0.624502 0.297369 0.589692 0.021 Uiso 0.692(9) 1 calc R U P A 2
H3B H 0.675870 0.343617 0.553080 0.021 Uiso 0.692(9) 1 calc R U P A 2
C4 C 0.6332(3) 0.33778(13) 0.7800(4) 0.0192(10) Uani 0.692(9) 1 d . . P A 2
H4A H 0.693565 0.320952 0.816155 0.023 Uiso 0.692(9) 1 calc R U P A 2
H4B H 0.571496 0.326908 0.834057 0.023 Uiso 0.692(9) 1 calc R U P A 2
C8 C 0.6905(8) 0.3508(3) 0.7493(11) 0.022(2) Uani 0.308(9) 1 d . . P A 1
H8A H 0.735725 0.356743 0.661928 0.026 Uiso 0.308(9) 1 calc R U P A 1
H8B H 0.730025 0.333226 0.823012 0.026 Uiso 0.308(9) 1 calc R U P A 1
C10 C 0.5920(8) 0.3246(3) 0.6967(12) 0.024(2) Uani 0.308(9) 1 d . . P A 1
H10A H 0.548530 0.319918 0.786812 0.029 Uiso 0.308(9) 1 calc R U P A 1
H10B H 0.615905 0.295511 0.663261 0.029 Uiso 0.308(9) 1 calc R U P A 1


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
I001 Cu02 2.4710(5) . ?
Cu02 N00B 1.952(3) 6_556 ?
Cu02 N00C 1.950(3) . ?
S003 C00E 1.741(2) . ?
S003 C00I 1.744(2) . ?
S004 C00G 1.743(2) . ?
S004 C00K 1.752(2) . ?
S005 C00G 1.736(2) . ?
S005 C00J 1.748(2) . ?
S006 C00E 1.744(2) . ?
S006 C00L 1.758(2) . ?
S007 C00I 1.754(2) . ?
S007 C00M 1.812(2) . ?
S008 C00J 1.744(2) . ?
S008 C4 1.876(4) . ?
S008 C8 1.649(8) . ?
S009 C00K 1.747(2) . ?
S009 C3 1.734(3) . ?
S009 C10 1.957(10) . ?
S00A C00L 1.744(2) . ?
S00A C00N 1.797(2) . ?
N00B C00F 1.151(5) . ?
N00C C00H 1.160(5) . ?
N00D C00F 1.296(5) . ?
N00D C00H 1.307(5) . ?
C00E C00G 1.372(3) . ?
C00I C00L 1.352(3) . ?
C00J C00K 1.357(3) . ?
C00M H00A 0.9700 . ?
C00M H00B 0.9700 . ?
C00M C00N 1.517(3) . ?
C00N H00C 0.9700 . ?
C00N H00D 0.9700 . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C3 C4 1.528(5) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C8 C10 1.544(13) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?

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
N00B Cu02 I001 115.86(10) 6_556 . ?
N00C Cu02 I001 133.13(10) . . ?
N00C Cu02 N00B 111.01(14) . 6_556 ?
C00E S003 C00I 95.52(11) . . ?
C00G S004 C00K 94.79(11) . . ?
C00G S005 C00J 95.03(11) . . ?
C00E S006 C00L 95.08(11) . . ?
C00I S007 C00M 101.68(12) . . ?
C00J S008 C4 99.59(14) . . ?
C8 S008 C00J 109.0(3) . . ?
C00K S009 C10 96.3(3) . . ?
C3 S009 C00K 102.19(15) . . ?
C00L S00A C00N 100.91(11) . . ?
C00F N00B Cu02 179.0(3) . 6_656 ?
C00H N00C Cu02 158.4(3) . . ?
C00F N00D C00H 124.3(3) . . ?
S003 C00E S006 115.29(13) . . ?
C00G C00E S003 120.41(18) . . ?
C00G C00E S006 124.29(18) . . ?
N00B C00F N00D 171.5(4) . . ?
S005 C00G S004 115.67(13) . . ?
C00E C00G S004 123.52(18) . . ?
C00E C00G S005 120.80(18) . . ?
N00C C00H N00D 169.2(4) . . ?
S003 C00I S007 114.22(13) . . ?
C00L C00I S003 117.20(18) . . ?
C00L C00I S007 128.58(19) . . ?
S008 C00J S005 113.98(13) . . ?
C00K C00J S005 117.05(18) . . ?
C00K C00J S008 128.97(18) . . ?
S009 C00K S004 114.44(13) . . ?
C00J C00K S004 116.92(18) . . ?
C00J C00K S009 128.62(19) . . ?
S00A C00L S006 114.55(13) . . ?
C00I C00L S006 116.88(18) . . ?
C00I C00L S00A 128.57(18) . . ?
S007 C00M H00A 108.6 . . ?
S007 C00M H00B 108.6 . . ?
H00A C00M H00B 107.6 . . ?
C00N C00M S007 114.68(18) . . ?
C00N C00M H00A 108.6 . . ?
C00N C00M H00B 108.6 . . ?
S00A C00N H00C 108.8 . . ?
S00A C00N H00D 108.8 . . ?
C00M C00N S00A 113.93(18) . . ?
C00M C00N H00C 108.8 . . ?
C00M C00N H00D 108.8 . . ?
H00C C00N H00D 107.7 . . ?
S009 C3 H3A 108.8 . . ?
S009 C3 H3B 108.8 . . ?
H3A C3 H3B 107.7 . . ?
C4 C3 S009 114.0(3) . . ?
C4 C3 H3A 108.8 . . ?
C4 C3 H3B 108.8 . . ?
S008 C4 H4A 108.9 . . ?
S008 C4 H4B 108.9 . . ?
C3 C4 S008 113.6(3) . . ?
C3 C4 H4A 108.9 . . ?
C3 C4 H4B 108.9 . . ?
H4A C4 H4B 107.7 . . ?
S008 C8 H8A 109.8 . . ?
S008 C8 H8B 109.8 . . ?
H8A C8 H8B 108.3 . . ?
C10 C8 S008 109.2(7) . . ?
C10 C8 H8A 109.8 . . ?
C10 C8 H8B 109.8 . . ?
S009 C10 H10A 107.1 . . ?
S009 C10 H10B 107.1 . . ?
C8 C10 S009 121.0(6) . . ?
C8 C10 H10A 107.1 . . ?
C8 C10 H10B 107.1 . . ?
H10A C10 H10B 106.8 . . ?

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
Cu02 N00C C00H N00D 0.000(2) . . . . ?
S003 C00E C00G S004 176.51(13) . . . . ?
S003 C00E C00G S005 -2.7(3) . . . . ?
S003 C00I C00L S006 1.1(3) . . . . ?
S003 C00I C00L S00A -178.20(16) . . . . ?
S005 C00J C00K S004 0.2(3) . . . . ?
S005 C00J C00K S009 -178.01(14) . . . . ?
S006 C00E C00G S004 -2.7(3) . . . . ?
S006 C00E C00G S005 178.07(13) . . . . ?
S007 C00I C00L S006 -178.01(15) . . . . ?
S007 C00I C00L S00A 2.7(4) . . . . ?
S007 C00M C00N S00A -69.0(2) . . . . ?
S008 C00J C00K S004 179.65(14) . . . . ?
S008 C00J C00K S009 1.4(4) . . . . ?
S008 C8 C10 S009 64.5(9) . . . . ?
S009 C3 C4 S008 -70.7(4) . . . . ?
C00E S003 C00I S007 179.51(14) . . . . ?
C00E S003 C00I C00L 0.2(2) . . . . ?
C00E S006 C00L S00A 177.56(15) . . . . ?
C00E S006 C00L C00I -1.9(2) . . . . ?
C00F N00D C00H N00C 180.000(1) . . . . ?
C00G S004 C00K S009 174.07(14) . . . . ?
C00G S004 C00K C00J -4.4(2) . . . . ?
C00G S005 C00J S008 -175.40(14) . . . . ?
C00G S005 C00J C00K 4.1(2) . . . . ?
C00I S003 C00E S006 -1.54(16) . . . . ?
C00I S003 C00E C00G 179.2(2) . . . . ?
C00I S007 C00M C00N 43.6(2) . . . . ?
C00J S005 C00G S004 -7.11(15) . . . . ?
C00J S005 C00G C00E 172.2(2) . . . . ?
C00J S008 C4 C3 46.2(3) . . . . ?
C00J S008 C8 C10 -42.7(8) . . . . ?
C00K S004 C00G S005 7.18(15) . . . . ?
C00K S004 C00G C00E -172.1(2) . . . . ?
C00K S009 C3 C4 49.7(3) . . . . ?
C00L S006 C00E S003 2.00(16) . . . . ?
C00L S006 C00E C00G -178.7(2) . . . . ?
C00L S00A C00N C00M 50.6(2) . . . . ?
C00M S007 C00I S003 169.80(14) . . . . ?
C00M S007 C00I C00L -11.0(3) . . . . ?
C00N S00A C00L S006 162.15(14) . . . . ?
C00N S00A C00L C00I -18.5(3) . . . . ?
C3 S009 C00K S004 166.04(18) . . . . ?
C3 S009 C00K C00J -15.7(3) . . . . ?
C4 S008 C00J S005 166.37(17) . . . . ?
C4 S008 C00J C00K -13.1(3) . . . . ?
C8 S008 C00J S005 -166.9(4) . . . . ?
C8 S008 C00J C00K 13.6(5) . . . . ?
C10 S009 C00K S004 -168.5(3) . . . . ?
C10 S009 C00K C00J 9.8(4) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.205
_oxdiff_exptl_absorpt_empirical_full_min 0.878
_exptl_crystal_recrystallization_method Electrocrystallization
_exptl_crystal_preparation       'Conducting properties'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_296k_autored
_database_code_depnum_ccdc_archive 'CCDC 2114420'
_audit_update_record             
;
2021-10-07 deposited with the CCDC.	2021-12-14 downloaded from the CCDC.
;
_audit_creation_date             2021-09-14
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        'kappa-ET2Cu[N(CN)2]I, 296 K'
_chemical_formula_moiety         '0.5(C4 Cu2 I2 N6), 2(C10 H8 S8)'
_chemical_formula_sum            'C22 H16 Cu I N3 S16'
_chemical_formula_weight         1025.78
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 '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'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_H-M_alt        'P n m a'
_space_group_name_Hall           '-P 2ac 2n'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z'
'-x-1/2, y-1/2, z-1/2'

_cell_length_a                   12.8867(4)
_cell_length_b                   30.2590(9)
_cell_length_c                   8.6857(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3386.89(17)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    21950
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      29.7880
_cell_measurement_theta_min      2.4290
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    2.568
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.72916
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.93a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    2.012
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2028
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.12
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0912
_diffrn_reflns_av_unetI/netI     0.0587
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.938
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       42
_diffrn_reflns_limit_k_min       -43
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            57122
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.938
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.223
_diffrn_reflns_theta_min         2.440
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.938
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -110.00  70.00   0.50    1.00    --  -20.00  45.00   0.00  360
  2  ω   -110.00  70.00   0.50    1.00    --  -20.00  45.00  90.00  360
  3  ω   -110.00  70.00   0.50    1.00    --  -20.00  45.00 180.00  360
  4  ω   -110.00  70.00   0.50    1.00    --  -20.00  45.00 270.00  360
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  
'dtrek-CrysAlisPro-abstract goniometer imported rigaku-d*trek images'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0294813000
_diffrn_orient_matrix_UB_12      -0.0194545000
_diffrn_orient_matrix_UB_13      -0.0126990000
_diffrn_orient_matrix_UB_21      -0.0381756000
_diffrn_orient_matrix_UB_22      -0.0126032000
_diffrn_orient_matrix_UB_23      0.0391346000
_diffrn_orient_matrix_UB_31      -0.0264958000
_diffrn_orient_matrix_UB_32      -0.0034921000
_diffrn_orient_matrix_UB_33      -0.0705565000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3469
_reflns_number_total             5252
_reflns_odcompleteness_completeness 93.88
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     31.15
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.843
_refine_diff_density_min         -0.543
_refine_diff_density_rms         0.111
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     224
_refine_ls_number_reflns         5252
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1108
_refine_ls_R_factor_gt           0.0599
_refine_ls_restrained_S_all      1.011
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1000P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1529
_refine_ls_wR_factor_ref         0.1788
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
2. Others
 Sof(C3)=Sof(H3A)=Sof(H3B)=Sof(C4)=Sof(H4A)=Sof(H4B)=1-FVAR(1)
 Sof(C1)=Sof(H1A)=Sof(H1B)=Sof(C2)=Sof(H2A)=Sof(H2B)=FVAR(1)
3.a Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C12(H12A,H12B), C3(H3A,H3B), C1(H1A,H1B), C4(H4A,H4B), C2(H2A,
 H2B)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
I1 I 0.36562(4) 0.250000 0.83950(6) 0.05234(19) Uani 1 2 d S T P . .
Cu1 Cu 0.37081(7) 0.250000 0.55454(11) 0.0459(3) Uani 1 2 d S T P . .
S6 S 0.25323(9) 0.52593(4) 0.51768(14) 0.0347(3) Uani 1 1 d . . . . .
S5 S 0.38028(9) 0.56095(4) 0.77023(14) 0.0351(3) Uani 1 1 d . . . . .
S4 S 0.39930(9) 0.43617(4) 0.52176(13) 0.0340(3) Uani 1 1 d . . . . .
S3 S 0.52517(9) 0.47709(4) 0.76510(14) 0.0364(3) Uani 1 1 d . . . . .
S7 S 0.26463(11) 0.64386(4) 0.80587(14) 0.0433(3) Uani 1 1 d . . . . .
S1 S 0.65038(11) 0.39897(5) 0.83116(15) 0.0494(4) Uani 1 1 d . . . . .
S2 S 0.49878(12) 0.34896(4) 0.54118(15) 0.0507(4) Uani 1 1 d . . . . .
S8 S 0.11483(11) 0.60277(5) 0.49838(17) 0.0594(4) Uani 1 1 d . . . . .
N1 N 0.4858(4) 0.250000 0.4086(7) 0.0428(14) Uani 1 2 d S T P . .
N3 N 0.7366(5) 0.250000 0.0492(7) 0.0501(16) Uani 1 2 d S T P . .
C9 C 0.2783(3) 0.59387(14) 0.7066(5) 0.0304(9) Uani 1 1 d . . . . .
C7 C 0.4194(3) 0.48143(14) 0.6405(5) 0.0312(9) Uani 1 1 d . . . . .
C10 C 0.2204(3) 0.57790(14) 0.5909(5) 0.0320(10) Uani 1 1 d . . . . .
C13 C 0.5307(5) 0.250000 0.2965(8) 0.0395(16) Uani 1 2 d S T P . .
C8 C 0.3578(3) 0.51809(14) 0.6404(5) 0.0307(9) Uani 1 1 d . . . . .
C6 C 0.4939(3) 0.40298(14) 0.6098(5) 0.0306(9) Uani 1 1 d . . . . .
C5 C 0.5517(3) 0.42229(14) 0.7200(5) 0.0307(9) Uani 1 1 d . . . . .
C14 C 0.6590(6) 0.250000 0.1071(9) 0.0453(17) Uani 1 2 d S T P . .
C11 C 0.1757(4) 0.67272(15) 0.6842(5) 0.0417(11) Uani 1 1 d . . . . .
H11A H 0.150141 0.698362 0.739472 0.050 Uiso 1 1 calc R U . . .
H11B H 0.213248 0.683362 0.594774 0.050 Uiso 1 1 calc R U . . .
C12 C 0.0838(4) 0.64605(18) 0.6295(6) 0.0442(12) Uani 1 1 d . . . . .
H12A H 0.034798 0.665874 0.580194 0.053 Uiso 1 1 calc R U . . .
H12B H 0.049509 0.633294 0.718435 0.053 Uiso 1 1 calc R U . . .
N2 N 0.5633(5) 0.250000 0.1542(8) 0.083(3) Uani 1 2 d S T P . .
C3 C 0.6277(12) 0.3392(4) 0.7817(14) 0.041(3) Uani 0.53(2) 1 d . . P A 2
H3A H 0.686674 0.322149 0.817497 0.049 Uiso 0.53(2) 1 calc R U P A 2
H3B H 0.567151 0.329003 0.837831 0.049 Uiso 0.53(2) 1 calc R U P A 2
C1 C 0.5878(10) 0.3258(4) 0.694(2) 0.040(4) Uani 0.47(2) 1 d . . P A 1
H1A H 0.546491 0.321461 0.786391 0.047 Uiso 0.47(2) 1 calc R U P A 1
H1B H 0.609784 0.296762 0.660014 0.047 Uiso 0.47(2) 1 calc R U P A 1
C4 C 0.6113(9) 0.3294(4) 0.6101(19) 0.043(3) Uani 0.53(2) 1 d . . P A 2
H4A H 0.613326 0.297621 0.594498 0.052 Uiso 0.53(2) 1 calc R U P A 2
H4B H 0.668019 0.342225 0.551968 0.052 Uiso 0.53(2) 1 calc R U P A 2
C2 C 0.6815(12) 0.3502(4) 0.7397(17) 0.041(4) Uani 0.47(2) 1 d . . P A 1
H2A H 0.722706 0.356613 0.648874 0.050 Uiso 0.47(2) 1 calc R U P A 1
H2B H 0.722994 0.332035 0.807999 0.050 Uiso 0.47(2) 1 calc R U P A 1


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
I1 Cu1 2.4760(10) . ?
Cu1 N1 1.950(6) . ?
Cu1 N3 1.951(6) 6_556 ?
S6 C10 1.748(4) . ?
S6 C8 1.734(4) . ?
S5 C9 1.740(4) . ?
S5 C8 1.743(4) . ?
S4 C7 1.734(4) . ?
S4 C6 1.755(4) . ?
S3 C7 1.746(4) . ?
S3 C5 1.738(4) . ?
S7 C9 1.750(4) . ?
S7 C11 1.787(5) . ?
S1 C5 1.746(4) . ?
S1 C3 1.882(12) . ?
S1 C2 1.723(11) . ?
S2 C6 1.741(4) . ?
S2 C1 1.891(14) . ?
S2 C4 1.677(10) . ?
S8 C10 1.751(4) . ?
S8 C12 1.781(5) . ?
N1 C13 1.133(9) . ?
N3 C14 1.118(9) . ?
C9 C10 1.341(6) . ?
C7 C8 1.364(6) . ?
C13 N2 1.305(9) . ?
C6 C5 1.346(6) . ?
C14 N2 1.300(10) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C11 C12 1.511(7) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C3 C4 1.535(19) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C1 C2 1.47(2) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Cu1 I1 132.10(18) . . ?
N1 Cu1 N3 111.9(3) . 6_556 ?
N3 Cu1 I1 115.97(18) 6_556 . ?
C8 S6 C10 95.0(2) . . ?
C9 S5 C8 95.4(2) . . ?
C7 S4 C6 95.1(2) . . ?
C5 S3 C7 94.9(2) . . ?
C9 S7 C11 101.3(2) . . ?
C5 S1 C3 98.6(4) . . ?
C2 S1 C5 105.1(4) . . ?
C6 S2 C1 97.4(4) . . ?
C4 S2 C6 104.0(4) . . ?
C10 S8 C12 101.4(2) . . ?
C13 N1 Cu1 161.3(6) . . ?
C14 N3 Cu1 179.2(6) . 6_656 ?
S5 C9 S7 114.5(2) . . ?
C10 C9 S5 116.9(3) . . ?
C10 C9 S7 128.7(3) . . ?
S4 C7 S3 115.2(2) . . ?
C8 C7 S4 123.7(3) . . ?
C8 C7 S3 121.1(3) . . ?
S6 C10 S8 114.0(2) . . ?
C9 C10 S6 117.5(3) . . ?
C9 C10 S8 128.4(3) . . ?
N1 C13 N2 168.1(8) . . ?
S6 C8 S5 115.2(2) . . ?
C7 C8 S6 124.3(3) . . ?
C7 C8 S5 120.6(3) . . ?
S2 C6 S4 114.4(2) . . ?
C5 C6 S4 116.5(3) . . ?
C5 C6 S2 129.1(3) . . ?
S3 C5 S1 113.9(2) . . ?
C6 C5 S3 117.8(3) . . ?
C6 C5 S1 128.4(3) . . ?
N3 C14 N2 171.7(8) . . ?
S7 C11 H11A 108.4 . . ?
S7 C11 H11B 108.4 . . ?
H11A C11 H11B 107.5 . . ?
C12 C11 S7 115.3(4) . . ?
C12 C11 H11A 108.4 . . ?
C12 C11 H11B 108.4 . . ?
S8 C12 H12A 108.6 . . ?
S8 C12 H12B 108.6 . . ?
C11 C12 S8 114.7(3) . . ?
C11 C12 H12A 108.6 . . ?
C11 C12 H12B 108.6 . . ?
H12A C12 H12B 107.6 . . ?
C14 N2 C13 127.2(7) . . ?
S1 C3 H3A 108.4 . . ?
S1 C3 H3B 108.4 . . ?
H3A C3 H3B 107.5 . . ?
C4 C3 S1 115.4(10) . . ?
C4 C3 H3A 108.4 . . ?
C4 C3 H3B 108.4 . . ?
S2 C1 H1A 107.3 . . ?
S2 C1 H1B 107.3 . . ?
H1A C1 H1B 106.9 . . ?
C2 C1 S2 120.1(12) . . ?
C2 C1 H1A 107.3 . . ?
C2 C1 H1B 107.3 . . ?
S2 C4 H4A 108.9 . . ?
S2 C4 H4B 108.9 . . ?
C3 C4 S2 113.4(11) . . ?
C3 C4 H4A 108.9 . . ?
C3 C4 H4B 108.9 . . ?
H4A C4 H4B 107.7 . . ?
S1 C2 H2A 109.4 . . ?
S1 C2 H2B 109.4 . . ?
C1 C2 S1 111.3(12) . . ?
C1 C2 H2A 109.4 . . ?
C1 C2 H2B 109.4 . . ?
H2A C2 H2B 108.0 . . ?

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
Cu1 N1 C13 N2 0.000(4) . . . . ?
S5 C9 C10 S6 0.3(5) . . . . ?
S5 C9 C10 S8 -178.7(3) . . . . ?
S4 C7 C8 S6 -2.4(6) . . . . ?
S4 C7 C8 S5 177.0(2) . . . . ?
S4 C6 C5 S3 1.1(5) . . . . ?
S4 C6 C5 S1 179.2(3) . . . . ?
S3 C7 C8 S6 178.3(2) . . . . ?
S3 C7 C8 S5 -2.4(6) . . . . ?
S7 C9 C10 S6 -179.0(3) . . . . ?
S7 C9 C10 S8 2.0(7) . . . . ?
S7 C11 C12 S8 -68.2(5) . . . . ?
S1 C3 C4 S2 -69.2(17) . . . . ?
S2 C6 C5 S3 -178.5(3) . . . . ?
S2 C6 C5 S1 -0.4(7) . . . . ?
S2 C1 C2 S1 67(2) . . . . ?
N1 C13 N2 C14 180.000(3) . . . . ?
C9 S5 C8 S6 -0.5(3) . . . . ?
C9 S5 C8 C7 -179.9(4) . . . . ?
C9 S7 C11 C12 45.4(4) . . . . ?
C7 S4 C6 S2 174.6(2) . . . . ?
C7 S4 C6 C5 -5.1(4) . . . . ?
C7 S3 C5 S1 -174.9(3) . . . . ?
C7 S3 C5 C6 3.5(4) . . . . ?
C10 S6 C8 S5 0.6(3) . . . . ?
C10 S6 C8 C7 180.0(4) . . . . ?
C10 S8 C12 C11 47.0(4) . . . . ?
C8 S6 C10 S8 178.6(3) . . . . ?
C8 S6 C10 C9 -0.5(4) . . . . ?
C8 S5 C9 S7 179.5(3) . . . . ?
C8 S5 C9 C10 0.1(4) . . . . ?
C6 S4 C7 S3 7.3(3) . . . . ?
C6 S4 C7 C8 -172.0(4) . . . . ?
C6 S2 C1 C2 -45.7(16) . . . . ?
C6 S2 C4 C3 47.2(14) . . . . ?
C5 S3 C7 S4 -6.9(3) . . . . ?
C5 S3 C7 C8 172.5(4) . . . . ?
C5 S1 C3 C4 45.8(12) . . . . ?
C5 S1 C2 C1 -44.8(16) . . . . ?
C11 S7 C9 S5 167.5(3) . . . . ?
C11 S7 C9 C10 -13.2(5) . . . . ?
C12 S8 C10 S6 165.8(3) . . . . ?
C12 S8 C10 C9 -15.1(5) . . . . ?
C3 S1 C5 S3 166.1(5) . . . . ?
C3 S1 C5 C6 -12.1(7) . . . . ?
C1 S2 C6 S4 -169.1(6) . . . . ?
C1 S2 C6 C5 10.5(7) . . . . ?
C4 S2 C6 S4 166.4(7) . . . . ?
C4 S2 C6 C5 -14.0(8) . . . . ?
C2 S1 C5 S3 -167.3(7) . . . . ?
C2 S1 C5 C6 14.5(8) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.540
_oxdiff_exptl_absorpt_empirical_full_min 0.748
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_No2_IM_100K
_database_code_depnum_ccdc_archive 'CCDC 2001301'
loop_
_audit_author_name
_audit_author_address
'Toshio Naito'
;Ehime University
Japan
;
_audit_update_record             
;
2020-05-06 deposited with the CCDC.	2021-12-14 downloaded from the CCDC.
;

#==============================================================================
# CHEMICAL DATA

_chemical_formula_sum            'C22 H16 Cu I N3 S16'
_chemical_formula_moiety         'C22 H16 Cu I N3 S16'
_chemical_formula_weight         1025.80
_chemical_melting_point          ?

#==============================================================================
# CRYSTAL DATA
_space_group_crystal_system      orthorhombic
_space_group_name_H-M_alt        'P n m a'
_space_group_name_Hall           '-P 2ac 2n'
_space_group_IT_number           62
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 +X,+Y,+Z
2 1/2+X,1/2-Y,1/2-Z
3 -X,1/2+Y,-Z
4 1/2-X,-Y,1/2+Z
5 -X,-Y,-Z
6 -1/2-X,-1/2+Y,-1/2+Z
7 +X,-1/2-Y,+Z
8 -1/2+X,+Y,-1/2-Z
#------------------------------------------------------------------------------
_cell_length_a                   12.6951(3)
_cell_length_b                   29.9226(5)
_cell_length_c                   8.64092(16)
_cell_angle_alpha                90.0000
_cell_angle_beta                 90.0000
_cell_angle_gamma                90.0000
_cell_volume                     3282.43(11)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    45940
_cell_measurement_theta_min      2.43
_cell_measurement_theta_max      31.24
_cell_measurement_temperature    100
#------------------------------------------------------------------------------
_exptl_crystal_description       block
_exptl_crystal_colour            black
_exptl_crystal_size_max          0.110
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.040
_exptl_crystal_density_diffrn    2.076
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2028.00
_exptl_absorpt_coefficient_mu    2.650
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_correction_T_min  0.718
_exptl_absorpt_correction_T_max  0.899

#==============================================================================
# EXPERIMENTAL DATA

_diffrn_ambient_temperature      100
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_measurement_device_type  'Rigaku Saturn724'
_diffrn_reflns_number            96594
_diffrn_reflns_av_unetI/netI     0.0187
_diffrn_reflns_av_R_equivalents  0.0737
_diffrn_reflns_theta_max         26.494
_diffrn_reflns_theta_min         2.453
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       10
_diffrn_standards_number         0
_diffrn_standards_interval_count .
_diffrn_standards_decay_%        ?
_reflns_number_total             3458
_reflns_number_gt                3155
_reflns_threshold_expression     F²>2.0σ(F²)
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

#==============================================================================
# REFINEMENT DATA

_refine_special_details          
;
    Refinement was performed using all reflections. The weighted 
    R-factor (wR) and goodness of fit (S) are based on F².
    R-factor (gt) are based on F. The threshold expression of
    F² > 2.0 sigma(F²) is used only for calculating R-factor (gt).
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_R_factor_all          0.0487
_refine_ls_R_factor_gt           0.0432
_refine_ls_wR_factor_ref         0.1235
_refine_ls_wR_factor_gt          0.1204
_refine_ls_number_restraints     0
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_reflns         3458
_refine_ls_number_parameters     224
_refine_ls_goodness_of_fit_ref   1.120
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w = 1/[σ²(Fo²)+(0.0592P)²+20.1272P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_refine_ls_shift/su_max          0.001
_refine_diff_density_max         1.08
_refine_diff_density_min         -2.34
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?

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 for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
H H 0.0000 0.0000
;
International Tables for Crystallography
(Vol. C, Table 6.1.1.4)
;
Cu Cu 0.3201 1.2651
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
I I -0.4742 1.8119
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
N N 0.0061 0.0033
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
S S 0.1246 0.1234
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;

#==============================================================================
# ATOMIC COORDINATES AND THERMAL PARAMETERS

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C9 C 0.3814(7) 0.6715(3) 0.3906(14) 0.016(3) Uani 0.60(2) 1 d . . P A 1
C10 C 0.3672(10) 0.6631(3) 0.2193(12) 0.018(3) Uani 0.60(2) 1 d . . P A 1
C13 C 0.4099(11) 0.6766(4) 0.297(2) 0.015(4) Uani 0.40(2) 1 d . . P A 2
C14 C 0.3129(15) 0.6505(5) 0.2541(16) 0.016(4) Uani 0.40(2) 1 d . . P A 2
I1 I 0.62521(5) 0.750000 0.15805(6) 0.03514(18) Uani 1 2 d S T P . .
Cu1 Cu 0.61937(7) 0.750000 0.43892(11) 0.0216(2) Uani 1 2 d S T P . .
S1 S 0.88770(11) 0.39476(5) 0.50703(16) 0.0287(3) Uani 1 1 d . . . . .
S2 S 0.73757(9) 0.35445(4) 0.19288(13) 0.0155(2) Uani 1 1 d . . . . .
S3 S 0.74954(8) 0.47336(4) 0.48597(13) 0.0123(2) Uani 1 1 d . . . . .
S4 S 0.62136(8) 0.43862(4) 0.22956(13) 0.0123(2) Uani 1 1 d . . . . .
S5 S 0.60030(9) 0.56424(4) 0.48285(13) 0.0121(2) Uani 1 1 d . . . . .
S6 S 0.47437(9) 0.52284(4) 0.23579(13) 0.0132(2) Uani 1 1 d . . . . .
S7 S 0.49864(11) 0.65229(4) 0.46387(14) 0.0208(3) Uani 1 1 d . . . . .
S8 S 0.34611(10) 0.60164(4) 0.16891(14) 0.0209(3) Uani 1 1 d . . . . .
N1 N 0.7577(5) 0.750000 0.5399(7) 0.0214(13) Uani 1 2 d S T P . .
N2 N 0.5047(5) 0.750000 0.5878(9) 0.0253(14) Uani 1 2 d S T P . .
N3 N 0.4341(5) 0.750000 0.8519(9) 0.0318(16) Uani 1 2 d S T P . .
C1 C 0.9210(4) 0.35180(16) 0.3709(6) 0.0186(10) Uani 1 1 d . . . . .
H1A H 0.954887 0.365784 0.279852 0.022 Uiso 1 1 calc R U . . .
H1B H 0.973133 0.331527 0.419178 0.022 Uiso 1 1 calc R U . . .
C2 C 0.8285(4) 0.32453(16) 0.3167(6) 0.0202(10) Uani 1 1 d . . . . .
H2A H 0.789632 0.313515 0.408399 0.024 Uiso 1 1 calc R U . . .
H2B H 0.855216 0.298131 0.259850 0.024 Uiso 1 1 calc R U . . .
C3 C 0.7825(4) 0.42044(15) 0.4130(5) 0.0152(9) Uani 1 1 d . . . . .
C4 C 0.7243(3) 0.40477(14) 0.2945(5) 0.0118(9) Uani 1 1 d . . . . .
C5 C 0.6432(3) 0.48164(15) 0.3615(5) 0.0111(8) Uani 1 1 d . . . . .
C6 C 0.5810(3) 0.51840(14) 0.3616(5) 0.0106(8) Uani 1 1 d . . . . .
C7 C 0.5040(4) 0.59760(15) 0.3941(5) 0.0127(9) Uani 1 1 d . . . . .
C8 C 0.4463(4) 0.57848(14) 0.2813(5) 0.0123(9) Uani 1 1 d . . . . .
C11 C 0.8364(6) 0.750000 0.6009(8) 0.0185(14) Uani 1 2 d S T P . .
C12 C 0.4612(6) 0.750000 0.7095(10) 0.0234(16) Uani 1 2 d S T P . .


#==============================================================================
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_structure_solution    'SHELXT Version 2018/2 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL Version 2018/3 (Sheldrick, 2008)'
_computing_publication_material  'CrystalStructure 4.3 (Rigaku, 2019)'
_computing_molecular_graphics    'CrystalStructure 4.3'

#==============================================================================
# MOLECULAR GEOMETRY

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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C9 C10 1.513(14) . ?
C9 S7 1.717(7) . ?
C10 S8 1.909(10) . ?
C13 C14 1.50(2) . ?
C13 S7 1.971(14) . ?
C14 S8 1.691(11) . ?
I1 Cu1 2.4281(11) . ?
Cu1 N2 1.943(7) . ?
Cu1 N1 1.960(6) . ?
S1 C3 1.741(5) . ?
S1 C1 1.793(5) . ?
S2 C4 1.751(4) . ?
S2 C2 1.811(5) . ?
S3 C5 1.744(4) . ?
S3 C3 1.755(5) . ?
S4 C5 1.741(4) . ?
S4 C4 1.746(4) . ?
S5 C6 1.743(4) . ?
S5 C7 1.755(5) . ?
S6 C6 1.741(4) . ?
S6 C8 1.747(4) . ?
S7 C7 1.745(4) . ?
S8 C8 1.744(5) . ?
N1 C11 1.130(10) . ?
N2 C12 1.188(11) . ?
N3 C12 1.277(11) . ?
N3 C11 1.306(10) 2_466 ?
C1 C2 1.505(7) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 C4 1.348(6) . ?
C5 C6 1.354(6) . ?
C7 C8 1.348(7) . ?

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
C10 C9 S7 114.1(8) . . ?
C9 C10 S8 113.6(7) . . ?
C14 C13 S7 117.1(10) . . ?
C13 C14 S8 110.6(12) . . ?
N2 Cu1 N1 112.1(3) . . ?
N2 Cu1 I1 133.2(2) . . ?
N1 Cu1 I1 114.7(2) . . ?
C3 S1 C1 101.0(2) . . ?
C4 S2 C2 101.0(2) . . ?
C5 S3 C3 95.2(2) . . ?
C5 S4 C4 95.7(2) . . ?
C6 S5 C7 95.0(2) . . ?
C6 S6 C8 95.2(2) . . ?
C9 S7 C7 102.8(3) . . ?
C7 S7 C13 96.6(4) . . ?
C14 S8 C8 106.5(5) . . ?
C8 S8 C10 98.8(3) . . ?
C11 N1 Cu1 178.6(6) . . ?
C12 N2 Cu1 159.1(6) . . ?
C12 N3 C11 123.8(7) . 2_466 ?
C2 C1 S1 114.2(4) . . ?
C2 C1 H1A 108.7 . . ?
S1 C1 H1A 108.7 . . ?
C2 C1 H1B 108.7 . . ?
S1 C1 H1B 108.7 . . ?
H1A C1 H1B 107.6 . . ?
C1 C2 S2 114.4(3) . . ?
C1 C2 H2A 108.7 . . ?
S2 C2 H2A 108.7 . . ?
C1 C2 H2B 108.7 . . ?
S2 C2 H2B 108.7 . . ?
H2A C2 H2B 107.6 . . ?
C4 C3 S1 128.5(4) . . ?
C4 C3 S3 117.1(4) . . ?
S1 C3 S3 114.4(3) . . ?
C3 C4 S4 116.9(3) . . ?
C3 C4 S2 128.8(4) . . ?
S4 C4 S2 114.2(2) . . ?
C6 C5 S4 120.6(3) . . ?
C6 C5 S3 124.5(3) . . ?
S4 C5 S3 114.9(2) . . ?
C5 C6 S6 121.0(3) . . ?
C5 C6 S5 123.9(3) . . ?
S6 C6 S5 115.1(2) . . ?
C8 C7 S7 128.8(4) . . ?
C8 C7 S5 117.0(3) . . ?
S7 C7 S5 114.2(3) . . ?
C7 C8 S8 129.1(3) . . ?
C7 C8 S6 117.2(3) . . ?
S8 C8 S6 113.7(3) . . ?
N1 C11 N3 170.4(8) . 2_566 ?
N2 C12 N3 167.9(8) . . ?

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
S7 C9 C10 S8 70.4(12) . . . . ?
S7 C13 C14 S8 -68.7(16) . . . . ?
C10 C9 S7 C7 -49.3(9) . . . . ?
C13 C14 S8 C8 45.7(14) . . . . ?
C3 S1 C1 C2 -49.4(4) . . . . ?
S1 C1 C2 S2 69.8(5) . . . . ?
C4 S2 C2 C1 -45.5(4) . . . . ?
C1 S1 C3 C4 16.3(5) . . . . ?
C1 S1 C3 S3 -164.2(3) . . . . ?
C5 S3 C3 C4 1.6(4) . . . . ?
C5 S3 C3 S1 -178.0(3) . . . . ?
S1 C3 C4 S4 178.4(3) . . . . ?
S3 C3 C4 S4 -1.1(5) . . . . ?
S1 C3 C4 S2 -2.0(7) . . . . ?
S3 C3 C4 S2 178.5(3) . . . . ?
C5 S4 C4 C3 0.0(4) . . . . ?
C5 S4 C4 S2 -179.6(3) . . . . ?
C2 S2 C4 C3 12.5(5) . . . . ?
C2 S2 C4 S4 -168.0(3) . . . . ?
C4 S4 C5 C6 -179.7(4) . . . . ?
C4 S4 C5 S3 1.1(3) . . . . ?
C3 S3 C5 C6 179.3(4) . . . . ?
C3 S3 C5 S4 -1.5(3) . . . . ?
S4 C5 C6 S6 2.6(5) . . . . ?
S3 C5 C6 S6 -178.3(2) . . . . ?
S4 C5 C6 S5 -176.9(2) . . . . ?
S3 C5 C6 S5 2.2(6) . . . . ?
C8 S6 C6 C5 -172.5(4) . . . . ?
C8 S6 C6 S5 7.1(3) . . . . ?
C7 S5 C6 C5 172.4(4) . . . . ?
C7 S5 C6 S6 -7.2(3) . . . . ?
C9 S7 C7 C8 14.8(6) . . . . ?
C13 S7 C7 C8 -12.1(6) . . . . ?
C9 S7 C7 S5 -166.6(5) . . . . ?
C13 S7 C7 S5 166.5(5) . . . . ?
C6 S5 C7 C8 4.5(4) . . . . ?
C6 S5 C7 S7 -174.2(3) . . . . ?
S7 C7 C8 S8 -0.9(7) . . . . ?
S5 C7 C8 S8 -179.4(3) . . . . ?
S7 C7 C8 S6 178.3(3) . . . . ?
S5 C7 C8 S6 -0.3(5) . . . . ?
C14 S8 C8 C7 -12.8(9) . . . . ?
C10 S8 C8 C7 12.9(6) . . . . ?
C14 S8 C8 S6 168.1(8) . . . . ?
C10 S8 C8 S6 -166.3(4) . . . . ?
C6 S6 C8 C7 -4.1(4) . . . . ?
C6 S6 C8 S8 175.1(3) . . . . ?
Cu1 N2 C12 N3 0.000(11) . . . . ?
C11 N3 C12 N2 180.000(7) 2_466 . . . ?


#==============================================================================
# Additional structures and associated data_? identifiers
# should be added at this point if there is more than one 
# structure analysis in the CIF.



#==============================================================================
#     End of CIF
#==============================================================================
_chemical_name_systematic        kappa-ET2Cu[N(CN)2]I
_exptl_crystal_recrystallization_method Electrocrystallization
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_No5_SC_100K
_database_code_depnum_ccdc_archive 'CCDC 2001311'
loop_
_audit_author_name
_audit_author_address
'Toshio Naito'
;Ehime University
Japan
;
_audit_update_record             
;
2020-05-06 deposited with the CCDC.	2021-12-14 downloaded from the CCDC.
;

#==============================================================================
# CHEMICAL DATA

_chemical_formula_sum            'C22 H16 Cu I N3 S16'
_chemical_formula_moiety         'C22 H16 Cu I N3 S16'
_chemical_formula_weight         1025.80
_chemical_melting_point          ?

#==============================================================================
# CRYSTAL DATA
_space_group_crystal_system      orthorhombic
_space_group_name_H-M_alt        'P n m a'
_space_group_name_Hall           '-P 2ac 2n'
_space_group_IT_number           62
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 +X,+Y,+Z
2 1/2+X,1/2-Y,1/2-Z
3 -X,1/2+Y,-Z
4 1/2-X,-Y,1/2+Z
5 -X,-Y,-Z
6 -1/2-X,-1/2+Y,-1/2+Z
7 +X,-1/2-Y,+Z
8 -1/2+X,+Y,-1/2-Z
#------------------------------------------------------------------------------
_cell_length_a                   12.6933(2)
_cell_length_b                   30.0387(5)
_cell_length_c                   8.67757(16)
_cell_angle_alpha                90.0000
_cell_angle_beta                 90.0000
_cell_angle_gamma                90.0000
_cell_volume                     3308.67(10)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    27687
_cell_measurement_theta_min      2.94
_cell_measurement_theta_max      68.32
_cell_measurement_temperature    100
#------------------------------------------------------------------------------
_exptl_crystal_description       plate
_exptl_crystal_colour            black
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_exptl_crystal_density_diffrn    2.059
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2028.00
_exptl_absorpt_coefficient_mu    17.908
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Rigaku, 1995)'
_exptl_absorpt_correction_T_min  0.062
_exptl_absorpt_correction_T_max  0.167

#==============================================================================
# EXPERIMENTAL DATA

_diffrn_ambient_temperature      100
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54187
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean 10.000
_diffrn_reflns_number            34472
_diffrn_reflns_av_unetI/netI     0.0903
_diffrn_reflns_av_R_equivalents  0.1939
_diffrn_reflns_theta_max         68.213
_diffrn_reflns_theta_min         2.942
_diffrn_reflns_theta_full        67.687
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       10
_diffrn_standards_number         0
_diffrn_standards_interval_count .
_diffrn_standards_decay_%        ?
_reflns_number_total             3099
_reflns_number_gt                2684
_reflns_threshold_expression     F²>2.0σ(F²)
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

#==============================================================================
# REFINEMENT DATA

_refine_special_details          
;Refinement was performed using all reflections. The weighted 
    R-factor (wR) and goodness of fit (S) are based on F².
    R-factor (gt) are based on F. The threshold expression of
    F² > 2.0 sigma(F²) is used only for calculating R-factor (gt).,Superconducting
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_R_factor_all          0.0738
_refine_ls_R_factor_gt           0.0693
_refine_ls_wR_factor_ref         0.2046
_refine_ls_wR_factor_gt          0.1952
_refine_ls_number_restraints     0
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_reflns         3099
_refine_ls_number_parameters     224
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w = 1/[σ²(Fo²)+(0.1285P)²+1.1066P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_refine_ls_shift/su_max          0.000
_refine_diff_density_max         2.03
_refine_diff_density_min         -1.10
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
H H 0.0000 0.0000
;
International Tables for Crystallography
(Vol. C, Table 6.1.1.4)
;
Cu Cu -1.9646 0.5888
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
I I -0.3257 6.8362
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
N N 0.0311 0.0180
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
S S 0.3331 0.5567
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;

#==============================================================================
# ATOMIC COORDINATES AND THERMAL PARAMETERS

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C9 C 0.310(2) 0.3509(7) 0.744(3) 0.021(7) Uani 0.24(3) 1 d . . P A 1
C10 C 0.409(2) 0.3252(7) 0.710(3) 0.029(7) Uani 0.24(3) 1 d . . P A 1
C13 C 0.3650(10) 0.3374(4) 0.7795(14) 0.048(4) Uani 0.76(3) 1 d . . P A 2
C14 C 0.3812(7) 0.3293(3) 0.6120(16) 0.045(4) Uani 0.76(3) 1 d . . P A 2
I1 I 0.62366(6) 0.250000 0.84331(7) 0.0557(3) Uani 1 2 d S T P . .
Cu1 Cu 0.61786(10) 0.250000 0.55932(17) 0.0483(4) Uani 1 2 d S T P . .
S1 S 0.73828(13) 0.64512(5) 0.80727(17) 0.0412(4) Uani 1 1 d . . . . .
S2 S 0.88727(15) 0.60563(6) 0.4919(2) 0.0554(5) Uani 1 1 d . . . . .
S3 S 0.62251(11) 0.56114(5) 0.77111(18) 0.0377(4) Uani 1 1 d . . . . .
S4 S 0.74991(12) 0.52679(5) 0.51425(17) 0.0385(4) Uani 1 1 d . . . . .
S5 S 0.47472(12) 0.47714(4) 0.76366(18) 0.0397(4) Uani 1 1 d . . . . .
S6 S 0.60113(12) 0.43612(5) 0.51698(17) 0.0381(4) Uani 1 1 d . . . . .
S7 S 0.34690(14) 0.39846(6) 0.82933(18) 0.0464(4) Uani 1 1 d . . . . .
S8 S 0.50013(14) 0.34814(5) 0.53626(17) 0.0455(4) Uani 1 1 d . . . . .
N1 N 0.7558(7) 0.250000 0.4568(9) 0.0491(19) Uani 1 2 d S T P . .
N2 N 0.5028(6) 0.250000 0.4122(10) 0.0500(19) Uani 1 2 d S T P . .
N3 N 0.4335(8) 0.250000 0.1488(10) 0.062(2) Uani 1 2 d S T P . .
C1 C 0.8296(6) 0.6749(2) 0.6874(7) 0.0469(15) Uani 1 1 d . . . . .
H1A H 0.790984 0.686854 0.597311 0.056 Uiso 1 1 calc R U . . .
H1B H 0.857413 0.700546 0.746300 0.056 Uiso 1 1 calc R U . . .
C2 C 0.9216(5) 0.6474(2) 0.6298(7) 0.0436(14) Uani 1 1 d . . . . .
H2A H 0.955697 0.632827 0.719138 0.052 Uiso 1 1 calc R U . . .
H2B H 0.974062 0.667691 0.582725 0.052 Uiso 1 1 calc R U . . .
C3 C 0.7241(5) 0.59513(18) 0.7057(7) 0.0377(13) Uani 1 1 d . . . . .
C4 C 0.7826(4) 0.57962(19) 0.5864(7) 0.0387(13) Uani 1 1 d . . . . .
C5 C 0.6450(5) 0.5184(2) 0.6373(7) 0.0364(13) Uani 1 1 d . . . . .
C6 C 0.5817(5) 0.48145(19) 0.6384(7) 0.0377(13) Uani 1 1 d . . . . .
C7 C 0.4477(5) 0.42215(18) 0.7179(7) 0.0378(13) Uani 1 1 d . . . . .
C8 C 0.5060(5) 0.40267(18) 0.6052(7) 0.0374(12) Uani 1 1 d . . . . .
C11 C 0.8352(8) 0.250000 0.3988(11) 0.0418(19) Uani 1 2 d S T P . .
C12 C 0.4594(8) 0.250000 0.2951(13) 0.051(2) Uani 1 2 d S T P . .


#==============================================================================
_computing_data_collection       'RAPID AUTO (Rigaku, ????)'
_computing_cell_refinement       'RAPID AUTO'
_computing_data_reduction        'RAPID AUTO'
_computing_structure_solution    'SHELXT Version 2018/2 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL Version 2018/3 (Sheldrick, 2008)'
_computing_publication_material  'CrystalStructure 4.3 (Rigaku, 2019)'
_computing_molecular_graphics    'CrystalStructure 4.3'

#==============================================================================
# MOLECULAR GEOMETRY

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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C9 C10 1.51(4) . ?
C9 S7 1.678(19) . ?
C10 S8 2.02(3) . ?
C13 C14 1.488(17) . ?
C13 S7 1.898(12) . ?
C14 S8 1.741(8) . ?
I1 Cu1 2.4655(15) . ?
Cu1 N2 1.940(9) . ?
Cu1 N1 1.964(8) . ?
S1 C3 1.751(6) . ?
S1 C1 1.796(7) . ?
S2 C4 1.745(6) . ?
S2 C2 1.788(6) . ?
S3 C3 1.740(6) . ?
S3 C5 1.755(6) . ?
S4 C5 1.725(6) . ?
S4 C4 1.756(6) . ?
S5 C7 1.733(6) . ?
S5 C6 1.744(6) . ?
S6 C6 1.740(6) . ?
S6 C8 1.748(6) . ?
S7 C7 1.754(6) . ?
S8 C8 1.745(6) . ?
N1 C11 1.126(12) . ?
N2 C12 1.156(13) . ?
N3 C12 1.311(12) . ?
N3 C11 1.315(14) 2_455 ?
C1 C2 1.515(9) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 C4 1.357(8) . ?
C5 C6 1.370(9) . ?
C7 C8 1.359(8) . ?

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
C10 C9 S7 106.9(18) . . ?
C9 C10 S8 116.7(17) . . ?
C14 C13 S7 113.4(8) . . ?
C13 C14 S8 115.9(9) . . ?
N2 Cu1 N1 111.9(4) . . ?
N2 Cu1 I1 132.9(3) . . ?
N1 Cu1 I1 115.2(2) . . ?
C3 S1 C1 101.6(3) . . ?
C4 S2 C2 100.7(3) . . ?
C3 S3 C5 95.3(3) . . ?
C5 S4 C4 95.4(3) . . ?
C7 S5 C6 94.7(3) . . ?
C6 S6 C8 95.0(3) . . ?
C9 S7 C7 107.7(8) . . ?
C7 S7 C13 100.3(4) . . ?
C14 S8 C8 102.2(4) . . ?
C8 S8 C10 95.2(8) . . ?
C11 N1 Cu1 179.6(8) . . ?
C12 N2 Cu1 159.7(9) . . ?
C12 N3 C11 122.8(9) . 2_455 ?
C2 C1 S1 114.7(4) . . ?
C2 C1 H1A 108.6 . . ?
S1 C1 H1A 108.6 . . ?
C2 C1 H1B 108.6 . . ?
S1 C1 H1B 108.6 . . ?
H1A C1 H1B 107.6 . . ?
C1 C2 S2 114.5(5) . . ?
C1 C2 H2A 108.6 . . ?
S2 C2 H2A 108.6 . . ?
C1 C2 H2B 108.6 . . ?
S2 C2 H2B 108.6 . . ?
H2A C2 H2B 107.6 . . ?
C4 C3 S3 116.9(4) . . ?
C4 C3 S1 128.5(5) . . ?
S3 C3 S1 114.5(3) . . ?
C3 C4 S2 128.4(5) . . ?
C3 C4 S4 116.9(5) . . ?
S2 C4 S4 114.7(3) . . ?
C6 C5 S4 125.1(5) . . ?
C6 C5 S3 119.5(5) . . ?
S4 C5 S3 115.4(3) . . ?
C5 C6 S6 123.1(5) . . ?
C5 C6 S5 121.4(5) . . ?
S6 C6 S5 115.4(3) . . ?
C8 C7 S5 117.9(5) . . ?
C8 C7 S7 128.3(5) . . ?
S5 C7 S7 113.9(3) . . ?
C7 C8 S8 128.9(5) . . ?
C7 C8 S6 116.4(4) . . ?
S8 C8 S6 114.7(3) . . ?
N1 C11 N3 171.8(10) . 2 ?
N2 C12 N3 166.0(11) . . ?

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
S7 C9 C10 S8 -73(2) . . . . ?
S7 C13 C14 S8 69.0(12) . . . . ?
C10 C9 S7 C7 49(2) . . . . ?
C14 C13 S7 C7 -44.5(10) . . . . ?
C13 C14 S8 C8 -49.2(10) . . . . ?
C3 S1 C1 C2 -44.2(6) . . . . ?
S1 C1 C2 S2 69.3(6) . . . . ?
C4 S2 C2 C1 -50.0(5) . . . . ?
C5 S3 C3 C4 -0.4(6) . . . . ?
C5 S3 C3 S1 -179.4(3) . . . . ?
C1 S1 C3 C4 11.9(7) . . . . ?
C1 S1 C3 S3 -169.3(4) . . . . ?
S3 C3 C4 S2 178.5(4) . . . . ?
S1 C3 C4 S2 -2.7(10) . . . . ?
S3 C3 C4 S4 -0.9(7) . . . . ?
S1 C3 C4 S4 177.9(3) . . . . ?
C2 S2 C4 C3 17.7(7) . . . . ?
C2 S2 C4 S4 -162.9(4) . . . . ?
C5 S4 C4 C3 1.7(5) . . . . ?
C5 S4 C4 S2 -177.8(4) . . . . ?
C4 S4 C5 C6 179.2(6) . . . . ?
C4 S4 C5 S3 -2.0(4) . . . . ?
C3 S3 C5 C6 -179.5(6) . . . . ?
C3 S3 C5 S4 1.6(4) . . . . ?
S4 C5 C6 S6 1.9(9) . . . . ?
S3 C5 C6 S6 -176.9(3) . . . . ?
S4 C5 C6 S5 -177.8(3) . . . . ?
S3 C5 C6 S5 3.4(8) . . . . ?
C8 S6 C6 C5 172.3(6) . . . . ?
C8 S6 C6 S5 -7.9(4) . . . . ?
C7 S5 C6 C5 -172.7(6) . . . . ?
C7 S5 C6 S6 7.5(4) . . . . ?
C6 S5 C7 C8 -4.0(5) . . . . ?
C6 S5 C7 S7 175.1(3) . . . . ?
C9 S7 C7 C8 -15.0(13) . . . . ?
C13 S7 C7 C8 11.9(7) . . . . ?
C9 S7 C7 S5 166.0(11) . . . . ?
C13 S7 C7 S5 -167.0(5) . . . . ?
S5 C7 C8 S8 178.4(3) . . . . ?
S7 C7 C8 S8 -0.5(9) . . . . ?
S5 C7 C8 S6 -0.9(7) . . . . ?
S7 C7 C8 S6 -179.8(3) . . . . ?
C14 S8 C8 C7 14.2(8) . . . . ?
C10 S8 C8 C7 -12.4(10) . . . . ?
C14 S8 C8 S6 -166.4(5) . . . . ?
C10 S8 C8 S6 167.0(9) . . . . ?
C6 S6 C8 C7 5.3(5) . . . . ?
C6 S6 C8 S8 -174.2(3) . . . . ?
Cu1 N2 C12 N3 0.000(5) . . . . ?
C11 N3 C12 N2 180.000(3) 2_455 . . . ?


#==============================================================================
# Additional structures and associated data_? identifiers
# should be added at this point if there is more than one 
# structure analysis in the CIF.



#==============================================================================
#     End of CIF
#==============================================================================
_chemical_name_systematic        kappa-ET2Cu[N(CN)2]I
_exptl_crystal_recrystallization_method Electrocrystallization
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_100k_rapid_autored_CCDC1
_database_code_depnum_ccdc_archive 'CCDC 2110364'
loop_
_audit_author_name
_audit_author_address
'Toshio Naito'
;Ehime University
Japan
;
_audit_update_record             
;
2021-09-17 deposited with the CCDC.	2021-12-14 downloaded from the CCDC.
;
_audit_creation_date             2021-09-14
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        
'kappa-ET2Cu[N(CN)2]I, 100 K, rapid cooling (-10 K/min)'
_chemical_formula_moiety         '0.5(C4 Cu2 I2 N6), 2(C10 H8 S8)'
_chemical_formula_sum            'C22 H16 Cu I N3 S16'
_chemical_formula_weight         1025.78
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 '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'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_H-M_alt        'P n m a'
_space_group_name_Hall           '-P 2ac 2n'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z'
'-x-1/2, y-1/2, z-1/2'

_cell_length_a                   12.6524(3)
_cell_length_b                   29.9686(7)
_cell_length_c                   8.6953(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3297.04(13)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    28503
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.0880
_cell_measurement_theta_min      2.4250
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    2.638
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.69028
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.93a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    2.067
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2028
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.12
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0795
_diffrn_reflns_av_unetI/netI     0.0481
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.941
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       42
_diffrn_reflns_limit_k_min       -42
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            56082
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.941
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.266
_diffrn_reflns_theta_min         2.439
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.941
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -110.00  70.00   0.50    1.00    --  -20.00  45.00   0.00  360
  2  ω   -110.00  70.00   0.50    1.00    --  -20.00  45.00  90.00  360
  3  ω   -110.00  70.00   0.50    1.00    --  -20.00  45.00 180.00  360
  4  ω   -110.00  70.00   0.50    1.00    --  -20.00  45.00 270.00  360
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  
'dtrek-CrysAlisPro-abstract goniometer imported rigaku-d*trek images'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0473696000
_diffrn_orient_matrix_UB_12      0.0039903000
_diffrn_orient_matrix_UB_13      -0.0413783000
_diffrn_orient_matrix_UB_21      0.0117234000
_diffrn_orient_matrix_UB_22      -0.0231341000
_diffrn_orient_matrix_UB_23      0.0019891000
_diffrn_orient_matrix_UB_31      -0.0275471000
_diffrn_orient_matrix_UB_32      -0.0030040000
_diffrn_orient_matrix_UB_33      -0.0703151000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4109
_reflns_number_total             5150
_reflns_odcompleteness_completeness 94.10
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     31.20
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.747
_refine_diff_density_min         -0.630
_refine_diff_density_rms         0.141
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     224
_refine_ls_number_reflns         5150
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0742
_refine_ls_R_factor_gt           0.0490
_refine_ls_restrained_S_all      1.078
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0185P)²+10.6973P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0768
_refine_ls_wR_factor_ref         0.0837
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
2. Others
 Sof(C3)=Sof(H3A)=Sof(H3B)=Sof(C4)=Sof(H4A)=Sof(H4B)=1-FVAR(1)
 Sof(C1)=Sof(H1A)=Sof(H1B)=Sof(C2)=Sof(H2A)=Sof(H2B)=FVAR(1)
3.a Secondary CH2 refined with riding coordinates:
 C12(H12A,H12B), C11(H11A,H11B), C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C4(H4A,
 H4B)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
I1 I 0.37666(3) 0.250000 0.84437(4) 0.02788(10) Uani 1 2 d S T P . .
Cu1 Cu 0.38276(5) 0.250000 0.56069(7) 0.02030(14) Uani 1 2 d S T P . .
S4 S 0.39876(6) 0.43609(3) 0.51670(9) 0.01482(16) Uani 1 1 d . . . . .
S5 S 0.37740(6) 0.56105(3) 0.77104(9) 0.01533(16) Uani 1 1 d . . . . .
S6 S 0.24990(6) 0.52695(3) 0.51372(9) 0.01523(16) Uani 1 1 d . . . . .
S3 S 0.52500(6) 0.47701(3) 0.76330(10) 0.01632(17) Uani 1 1 d . . . . .
S7 S 0.26184(7) 0.64520(3) 0.80732(10) 0.01867(18) Uani 1 1 d . . . . .
S2 S 0.49956(8) 0.34799(3) 0.53526(10) 0.02261(19) Uani 1 1 d . . . . .
S1 S 0.65302(7) 0.39810(3) 0.82872(11) 0.02287(19) Uani 1 1 d . . . . .
S8 S 0.11323(8) 0.60602(4) 0.49127(12) 0.0315(2) Uani 1 1 d . . . . .
N3 N 0.7457(3) 0.250000 0.0430(5) 0.0235(9) Uani 1 2 d S T P . .
N1 N 0.4983(3) 0.250000 0.4127(5) 0.0220(9) Uani 1 2 d S T P . .
N2 N 0.5684(3) 0.250000 0.1511(6) 0.0321(11) Uani 1 2 d S T P . .
C14 C 0.6646(4) 0.250000 0.1020(5) 0.0173(10) Uani 1 2 d S T P . .
C8 C 0.3561(2) 0.51846(10) 0.6383(4) 0.0136(6) Uani 1 1 d . . . . .
C7 C 0.4179(3) 0.48166(10) 0.6370(4) 0.0145(6) Uani 1 1 d . . . . .
C13 C 0.5396(4) 0.250000 0.2929(6) 0.0185(10) Uani 1 2 d S T P . .
C9 C 0.2751(2) 0.59511(10) 0.7057(4) 0.0145(6) Uani 1 1 d . . . . .
C5 C 0.5525(2) 0.42120(10) 0.7178(4) 0.0146(6) Uani 1 1 d . . . . .
C6 C 0.4948(3) 0.40254(10) 0.6054(4) 0.0152(6) Uani 1 1 d . . . . .
C10 C 0.2171(3) 0.57989(11) 0.5864(4) 0.0177(7) Uani 1 1 d . . . . .
C12 C 0.0778(3) 0.64758(11) 0.6309(4) 0.0189(7) Uani 1 1 d . . . . .
H12A H 0.025507 0.667293 0.585860 0.023 Uiso 1 1 calc R U . . .
H12B H 0.045146 0.632852 0.718141 0.023 Uiso 1 1 calc R U . . .
C11 C 0.1689(3) 0.67533(11) 0.6881(4) 0.0208(7) Uani 1 1 d . . . . .
H11A H 0.141000 0.700253 0.746605 0.025 Uiso 1 1 calc R U . . .
H11B H 0.206346 0.687441 0.600219 0.025 Uiso 1 1 calc R U . . .
C1 C 0.6330(5) 0.33768(17) 0.7796(6) 0.0174(13) Uani 0.718(11) 1 d . . P A 2
H1A H 0.693521 0.320806 0.815850 0.021 Uiso 0.718(11) 1 calc R U P A 2
H1B H 0.571149 0.326798 0.833706 0.021 Uiso 0.718(11) 1 calc R U P A 2
C2 C 0.6190(4) 0.32914(16) 0.6093(7) 0.0186(14) Uani 0.718(11) 1 d . . P A 2
H2A H 0.624446 0.297305 0.590807 0.022 Uiso 0.718(11) 1 calc R U P A 2
H2B H 0.676161 0.343564 0.554174 0.022 Uiso 0.718(11) 1 calc R U P A 2
C3 C 0.5904(10) 0.3243(4) 0.6989(16) 0.015(3) Uani 0.282(11) 1 d . . P A 1
H3A H 0.546909 0.320495 0.789829 0.018 Uiso 0.282(11) 1 calc R U P A 1
H3B H 0.613426 0.294812 0.667510 0.018 Uiso 0.282(11) 1 calc R U P A 1
C4 C 0.6885(11) 0.3505(4) 0.7466(15) 0.015(3) Uani 0.282(11) 1 d . . P A 1
H4A H 0.731730 0.356544 0.656916 0.018 Uiso 0.282(11) 1 calc R U P A 1
H4B H 0.730046 0.332916 0.818222 0.018 Uiso 0.282(11) 1 calc R U P A 1


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
I1 Cu1 2.4678(7) . ?
Cu1 N3 1.955(4) 6_556 ?
Cu1 N1 1.947(4) . ?
S4 C7 1.737(3) . ?
S4 C6 1.755(3) . ?
S5 C8 1.742(3) . ?
S5 C9 1.744(3) . ?
S6 C8 1.745(3) . ?
S6 C10 1.758(3) . ?
S3 C7 1.750(3) . ?
S3 C5 1.754(3) . ?
S7 C9 1.750(3) . ?
S7 C11 1.809(3) . ?
S2 C6 1.746(3) . ?
S2 C2 1.737(5) . ?
S2 C3 1.962(12) . ?
S1 C5 1.740(3) . ?
S1 C1 1.878(5) . ?
S1 C4 1.658(11) . ?
S8 C10 1.740(3) . ?
S8 C12 1.796(3) . ?
N3 C14 1.147(6) . ?
N1 C13 1.165(7) . ?
N2 C14 1.290(7) . ?
N2 C13 1.286(7) . ?
C8 C7 1.352(4) . ?
C9 C10 1.349(5) . ?
C5 C6 1.342(5) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C12 C11 1.505(5) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C1 C2 1.513(8) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C3 C4 1.525(19) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N3 Cu1 I1 115.68(13) 6_556 . ?
N1 Cu1 I1 133.15(13) . . ?
N1 Cu1 N3 111.17(18) . 6_556 ?
C7 S4 C6 95.12(16) . . ?
C8 S5 C9 95.64(15) . . ?
C8 S6 C10 95.16(15) . . ?
C7 S3 C5 95.05(15) . . ?
C9 S7 C11 101.60(16) . . ?
C6 S2 C3 96.1(4) . . ?
C2 S2 C6 101.8(2) . . ?
C5 S1 C1 99.2(2) . . ?
C4 S1 C5 107.6(4) . . ?
C10 S8 C12 100.32(16) . . ?
C14 N3 Cu1 179.1(4) . 6_656 ?
C13 N1 Cu1 158.0(4) . . ?
C13 N2 C14 125.7(5) . . ?
N3 C14 N2 172.8(5) . . ?
S5 C8 S6 115.06(18) . . ?
C7 C8 S5 120.9(2) . . ?
C7 C8 S6 124.0(2) . . ?
S4 C7 S3 115.04(18) . . ?
C8 C7 S4 124.5(3) . . ?
C8 C7 S3 120.5(2) . . ?
N1 C13 N2 169.8(5) . . ?
S5 C9 S7 114.12(18) . . ?
C10 C9 S5 117.1(2) . . ?
C10 C9 S7 128.8(3) . . ?
S1 C5 S3 113.54(19) . . ?
C6 C5 S3 117.0(2) . . ?
C6 C5 S1 129.5(3) . . ?
S2 C6 S4 114.01(19) . . ?
C5 C6 S4 117.2(2) . . ?
C5 C6 S2 128.7(3) . . ?
S8 C10 S6 114.43(19) . . ?
C9 C10 S6 117.0(3) . . ?
C9 C10 S8 128.6(3) . . ?
S8 C12 H12A 108.6 . . ?
S8 C12 H12B 108.6 . . ?
H12A C12 H12B 107.6 . . ?
C11 C12 S8 114.6(2) . . ?
C11 C12 H12A 108.6 . . ?
C11 C12 H12B 108.6 . . ?
S7 C11 H11A 108.7 . . ?
S7 C11 H11B 108.7 . . ?
C12 C11 S7 114.3(2) . . ?
C12 C11 H11A 108.7 . . ?
C12 C11 H11B 108.7 . . ?
H11A C11 H11B 107.6 . . ?
S1 C1 H1A 108.8 . . ?
S1 C1 H1B 108.8 . . ?
H1A C1 H1B 107.7 . . ?
C2 C1 S1 113.7(4) . . ?
C2 C1 H1A 108.8 . . ?
C2 C1 H1B 108.8 . . ?
S2 C2 H2A 108.7 . . ?
S2 C2 H2B 108.7 . . ?
C1 C2 S2 114.2(4) . . ?
C1 C2 H2A 108.7 . . ?
C1 C2 H2B 108.7 . . ?
H2A C2 H2B 107.6 . . ?
S2 C3 H3A 107.5 . . ?
S2 C3 H3B 107.5 . . ?
H3A C3 H3B 107.0 . . ?
C4 C3 S2 119.2(9) . . ?
C4 C3 H3A 107.5 . . ?
C4 C3 H3B 107.5 . . ?
S1 C4 H4A 109.7 . . ?
S1 C4 H4B 109.7 . . ?
C3 C4 S1 109.8(10) . . ?
C3 C4 H4A 109.7 . . ?
C3 C4 H4B 109.7 . . ?
H4A C4 H4B 108.2 . . ?

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
Cu1 N1 C13 N2 0.000(3) . . . . ?
S5 C8 C7 S4 176.29(18) . . . . ?
S5 C8 C7 S3 -3.0(4) . . . . ?
S5 C9 C10 S6 1.3(4) . . . . ?
S5 C9 C10 S8 -178.0(2) . . . . ?
S6 C8 C7 S4 -2.5(4) . . . . ?
S6 C8 C7 S3 178.20(18) . . . . ?
S3 C5 C6 S4 0.2(4) . . . . ?
S3 C5 C6 S2 -178.40(19) . . . . ?
S7 C9 C10 S6 -178.4(2) . . . . ?
S7 C9 C10 S8 2.3(5) . . . . ?
S2 C3 C4 S1 66.8(13) . . . . ?
S1 C5 C6 S4 -180.0(2) . . . . ?
S1 C5 C6 S2 1.5(5) . . . . ?
S1 C1 C2 S2 -70.6(5) . . . . ?
S8 C12 C11 S7 -69.4(3) . . . . ?
C14 N2 C13 N1 180.000(2) . . . . ?
C8 S5 C9 S7 179.89(19) . . . . ?
C8 S5 C9 C10 0.2(3) . . . . ?
C8 S6 C10 S8 177.4(2) . . . . ?
C8 S6 C10 C9 -2.1(3) . . . . ?
C7 S4 C6 S2 174.25(19) . . . . ?
C7 S4 C6 C5 -4.5(3) . . . . ?
C7 S3 C5 S1 -175.64(19) . . . . ?
C7 S3 C5 C6 4.3(3) . . . . ?
C9 S5 C8 S6 -1.6(2) . . . . ?
C9 S5 C8 C7 179.5(3) . . . . ?
C9 S7 C11 C12 43.3(3) . . . . ?
C5 S3 C7 S4 -7.3(2) . . . . ?
C5 S3 C7 C8 172.1(3) . . . . ?
C5 S1 C1 C2 46.2(5) . . . . ?
C5 S1 C4 C3 -44.2(11) . . . . ?
C6 S4 C7 S3 7.3(2) . . . . ?
C6 S4 C7 C8 -172.0(3) . . . . ?
C6 S2 C2 C1 49.4(5) . . . . ?
C10 S6 C8 S5 2.1(2) . . . . ?
C10 S6 C8 C7 -179.0(3) . . . . ?
C10 S8 C12 C11 51.2(3) . . . . ?
C12 S8 C10 S6 162.4(2) . . . . ?
C12 S8 C10 C9 -18.3(4) . . . . ?
C11 S7 C9 S5 169.61(19) . . . . ?
C11 S7 C9 C10 -10.7(4) . . . . ?
C1 S1 C5 S3 166.7(2) . . . . ?
C1 S1 C5 C6 -13.2(4) . . . . ?
C2 S2 C6 S4 166.1(3) . . . . ?
C2 S2 C6 C5 -15.3(4) . . . . ?
C3 S2 C6 S4 -167.9(4) . . . . ?
C3 S2 C6 C5 10.7(5) . . . . ?
C4 S1 C5 S3 -167.0(6) . . . . ?
C4 S1 C5 C6 13.1(7) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.402
_oxdiff_exptl_absorpt_empirical_full_min 0.755
_exptl_crystal_recrystallization_method Electrocrystallization
_exptl_crystal_preparation       'Conducting properties'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_slow_autored
_database_code_depnum_ccdc_archive 'CCDC 2110354'
loop_
_audit_author_name
_audit_author_address
'Toshio Naito'
;Ehime University
Japan
;
_audit_update_record             
;
2021-09-17 deposited with the CCDC.	2021-12-14 downloaded from the CCDC.
;
_audit_creation_date             2021-09-14
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        
'kappa-ET2Cu[N(CN)2]I, 100 K, slow cooling (-1 K/min)'
_chemical_formula_moiety         '0.5(C4 Cu2 I2 N6), 2(C10 H8 S8)'
_chemical_formula_sum            'C22 H16 Cu I N3 S16'
_chemical_formula_weight         1025.78
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C22 H16 Cu I N3 S16'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_H-M_alt        'P n m a'
_space_group_name_Hall           '-P 2ac 2n'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z'
'-x-1/2, y-1/2, z-1/2'

_cell_length_a                   12.6844(5)
_cell_length_b                   29.9858(9)
_cell_length_c                   8.7084(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3312.3(2)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    16737
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.9810
_cell_measurement_theta_min      2.4020
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    2.626
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.78277
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.93a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    2.057
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2028
_exptl_crystal_size_max          0.131
_exptl_crystal_size_mid          0.081
_exptl_crystal_size_min          0.051
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1220
_diffrn_reflns_av_unetI/netI     0.0792
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.947
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       42
_diffrn_reflns_limit_k_min       -42
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            57353
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.947
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.162
_diffrn_reflns_theta_min         2.435
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.947
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -110.00  70.00   0.50    1.00    --  -20.00  45.00   0.00  360
  2  ω   -110.00  70.00   0.50    1.00    --  -20.00  45.00  90.00  360
  3  ω   -110.00  70.00   0.50    1.00    --  -20.00  45.00 180.00  360
  4  ω   -110.00  70.00   0.50    1.00    --  -20.00  45.00 270.00  360
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  
'dtrek-CrysAlisPro-abstract goniometer imported rigaku-d*trek images'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0092943000
_diffrn_orient_matrix_UB_12      -0.0795196000
_diffrn_orient_matrix_UB_13      -0.0033220000
_diffrn_orient_matrix_UB_21      -0.0058249000
_diffrn_orient_matrix_UB_22      -0.0129359000
_diffrn_orient_matrix_UB_23      0.0232220000
_diffrn_orient_matrix_UB_31      -0.0548343000
_diffrn_orient_matrix_UB_32      -0.0119900000
_diffrn_orient_matrix_UB_33      -0.0030427000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3870
_reflns_number_total             5163
_reflns_odcompleteness_completeness 94.59
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     31.09
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         1.069
_refine_diff_density_min         -1.221
_refine_diff_density_rms         0.185
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.201
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     224
_refine_ls_number_reflns         5163
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1201
_refine_ls_R_factor_gt           0.0779
_refine_ls_restrained_S_all      1.201
_refine_ls_shift/su_max          0.021
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0159P)²+21.6806P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1056
_refine_ls_wR_factor_ref         0.1146
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
2. Others
 Sof(C4)=Sof(H4A)=Sof(H4B)=Sof(C3)=Sof(H3A)=Sof(H3B)=1-FVAR(1)
 Sof(C1)=Sof(H1A)=Sof(H1B)=Sof(C2)=Sof(H2A)=Sof(H2B)=FVAR(1)
3.a Secondary CH2 refined with riding coordinates:
 C00K(H00A,H00B), C00M(H00C,H00D), C1(H1A,H1B), C2(H2A,H2B), C4(H4A,H4B),
 C3(H3A,H3B)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
I001 I 0.62279(5) 0.250000 0.84413(6) 0.02493(15) Uani 1 2 d S T P . .
Cu02 Cu 0.61626(8) 0.250000 0.56023(11) 0.0182(2) Uani 1 2 d S T P . .
S003 S 0.60079(10) 0.43597(4) 0.51675(15) 0.0132(3) Uani 1 1 d . . . . .
S004 S 0.47495(10) 0.47715(4) 0.76312(15) 0.0144(3) Uani 1 1 d . . . . .
S005 S 0.62287(11) 0.56112(4) 0.77084(14) 0.0140(3) Uani 1 1 d . . . . .
S006 S 0.75031(10) 0.52691(4) 0.51389(15) 0.0134(3) Uani 1 1 d . . . . .
S007 S 0.73873(11) 0.64522(4) 0.80726(16) 0.0165(3) Uani 1 1 d . . . . .
S008 S 0.34669(11) 0.39817(5) 0.82859(16) 0.0210(3) Uani 1 1 d . . . . .
S009 S 0.49969(13) 0.34793(4) 0.53516(16) 0.0208(3) Uani 1 1 d . . . . .
S00A S 0.88728(12) 0.60591(5) 0.49159(18) 0.0297(4) Uani 1 1 d . . . . .
N00B N 0.2534(5) 0.250000 0.0443(7) 0.0199(14) Uani 1 2 d S T P . .
N00C N 0.5009(5) 0.250000 0.4122(8) 0.0187(14) Uani 1 2 d S T P . .
N00D N 0.4309(5) 0.250000 0.1513(9) 0.0297(18) Uani 1 2 d S T P . .
C00E C 0.7255(4) 0.59515(16) 0.7054(6) 0.0118(10) Uani 1 1 d . . . . .
C00F C 0.7828(4) 0.57978(17) 0.5874(6) 0.0156(11) Uani 1 1 d . . . . .
C00G C 0.4598(6) 0.250000 0.2934(10) 0.0163(16) Uani 1 2 d S T P . .
C00H C 0.5820(4) 0.48168(16) 0.6375(6) 0.0118(10) Uani 1 1 d . . . . .
C00I C 0.5053(4) 0.40240(16) 0.6057(6) 0.0124(10) Uani 1 1 d . . . . .
C00J C 0.6436(4) 0.51867(16) 0.6384(6) 0.0120(10) Uani 1 1 d . . . . .
C00K C 0.9229(4) 0.64757(18) 0.6306(6) 0.0173(12) Uani 1 1 d . . . . .
H00A H 0.955437 0.632915 0.717907 0.021 Uiso 1 1 calc R U . . .
H00B H 0.975146 0.667199 0.585413 0.021 Uiso 1 1 calc R U . . .
C00L C 0.4471(4) 0.42141(16) 0.7179(6) 0.0123(10) Uani 1 1 d . . . . .
C00M C 0.8319(4) 0.67542(18) 0.6874(6) 0.0190(12) Uani 1 1 d . . . . .
H00C H 0.794605 0.687438 0.599433 0.023 Uiso 1 1 calc R U . . .
H00D H 0.859719 0.700384 0.745530 0.023 Uiso 1 1 calc R U . . .
C00N C 0.3343(6) 0.250000 0.1032(9) 0.0150(16) Uani 1 2 d S T P . .
C1 C 0.3795(6) 0.3290(2) 0.6097(10) 0.010(2) Uani 0.702(17) 1 d . . P A 2
H1A H 0.322357 0.343414 0.554672 0.013 Uiso 0.702(17) 1 calc R U P A 2
H1B H 0.373858 0.297178 0.591795 0.013 Uiso 0.702(17) 1 calc R U P A 2
C2 C 0.3663(8) 0.3378(3) 0.7787(9) 0.015(2) Uani 0.702(17) 1 d . . P A 2
H2A H 0.428259 0.326955 0.832202 0.018 Uiso 0.702(17) 1 calc R U P A 2
H2B H 0.306152 0.321002 0.815732 0.018 Uiso 0.702(17) 1 calc R U P A 2
C4 C 0.4087(15) 0.3249(6) 0.699(2) 0.016(5) Uani 0.298(17) 1 d . . P A 1
H4A H 0.385947 0.295315 0.668404 0.019 Uiso 0.298(17) 1 calc R U P A 1
H4B H 0.452067 0.321341 0.789785 0.019 Uiso 0.298(17) 1 calc R U P A 1
C3 C 0.3116(18) 0.3506(7) 0.746(2) 0.020(5) Uani 0.298(17) 1 d . . P A 1
H3A H 0.269960 0.333000 0.816582 0.024 Uiso 0.298(17) 1 calc R U P A 1
H3B H 0.268760 0.356820 0.655856 0.024 Uiso 0.298(17) 1 calc R U P A 1


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
I001 Cu02 2.4737(11) . ?
Cu02 N00B 1.963(7) 6_656 ?
Cu02 N00C 1.950(7) . ?
S003 C00H 1.744(5) . ?
S003 C00I 1.755(5) . ?
S004 C00H 1.749(5) . ?
S004 C00L 1.753(5) . ?
S005 C00E 1.749(5) . ?
S005 C00J 1.738(5) . ?
S006 C00F 1.759(5) . ?
S006 C00J 1.751(5) . ?
S007 C00E 1.752(5) . ?
S007 C00M 1.819(5) . ?
S008 C00L 1.743(5) . ?
S008 C2 1.877(8) . ?
S008 C3 1.66(2) . ?
S009 C00I 1.747(5) . ?
S009 C1 1.752(7) . ?
S009 C4 1.96(2) . ?
S00A C00F 1.751(5) . ?
S00A C00K 1.798(5) . ?
N00B C00N 1.148(10) . ?
N00C C00G 1.159(10) . ?
N00D C00G 1.291(11) . ?
N00D C00N 1.294(10) . ?
C00E C00F 1.341(7) . ?
C00H C00J 1.357(7) . ?
C00I C00L 1.350(7) . ?
C00K H00A 0.9700 . ?
C00K H00B 0.9700 . ?
C00K C00M 1.507(7) . ?
C00M H00C 0.9700 . ?
C00M H00D 0.9700 . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C1 C2 1.504(11) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C4 C3 1.51(3) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?

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
N00B Cu02 I001 115.7(2) 6_656 . ?
N00C Cu02 I001 133.3(2) . . ?
N00C Cu02 N00B 111.0(3) . 6_656 ?
C00H S003 C00I 95.2(2) . . ?
C00H S004 C00L 95.2(2) . . ?
C00J S005 C00E 95.6(2) . . ?
C00J S006 C00F 94.8(2) . . ?
C00E S007 C00M 101.4(2) . . ?
C00L S008 C2 99.2(3) . . ?
C3 S008 C00L 107.4(7) . . ?
C00I S009 C1 102.0(3) . . ?
C00I S009 C4 95.6(6) . . ?
C00F S00A C00K 100.4(2) . . ?
C00N N00B Cu02 178.9(6) . 6_556 ?
C00G N00C Cu02 158.1(7) . . ?
C00G N00D C00N 125.4(7) . . ?
S005 C00E S007 114.0(3) . . ?
C00F C00E S005 116.9(4) . . ?
C00F C00E S007 129.1(4) . . ?
S00A C00F S006 114.0(3) . . ?
C00E C00F S006 117.5(4) . . ?
C00E C00F S00A 128.5(4) . . ?
N00C C00G N00D 169.8(8) . . ?
S003 C00H S004 115.0(3) . . ?
C00J C00H S003 124.5(4) . . ?
C00J C00H S004 120.5(4) . . ?
S009 C00I S003 114.1(3) . . ?
C00L C00I S003 117.0(4) . . ?
C00L C00I S009 128.8(4) . . ?
S005 C00J S006 115.1(3) . . ?
C00H C00J S005 121.0(4) . . ?
C00H C00J S006 123.8(4) . . ?
S00A C00K H00A 108.7 . . ?
S00A C00K H00B 108.7 . . ?
H00A C00K H00B 107.6 . . ?
C00M C00K S00A 114.4(4) . . ?
C00M C00K H00A 108.7 . . ?
C00M C00K H00B 108.7 . . ?
S008 C00L S004 113.8(3) . . ?
C00I C00L S004 117.1(4) . . ?
C00I C00L S008 129.1(4) . . ?
S007 C00M H00C 108.7 . . ?
S007 C00M H00D 108.7 . . ?
C00K C00M S007 114.2(4) . . ?
C00K C00M H00C 108.7 . . ?
C00K C00M H00D 108.7 . . ?
H00C C00M H00D 107.6 . . ?
N00B C00N N00D 172.3(8) . . ?
S009 C1 H1A 108.8 . . ?
S009 C1 H1B 108.8 . . ?
H1A C1 H1B 107.7 . . ?
C2 C1 S009 113.7(6) . . ?
C2 C1 H1A 108.8 . . ?
C2 C1 H1B 108.8 . . ?
S008 C2 H2A 108.7 . . ?
S008 C2 H2B 108.7 . . ?
C1 C2 S008 114.2(6) . . ?
C1 C2 H2A 108.7 . . ?
C1 C2 H2B 108.7 . . ?
H2A C2 H2B 107.6 . . ?
S009 C4 H4A 107.4 . . ?
S009 C4 H4B 107.4 . . ?
H4A C4 H4B 106.9 . . ?
C3 C4 S009 119.8(15) . . ?
C3 C4 H4A 107.4 . . ?
C3 C4 H4B 107.4 . . ?
S008 C3 H3A 109.7 . . ?
S008 C3 H3B 109.7 . . ?
C4 C3 S008 109.8(16) . . ?
C4 C3 H3A 109.7 . . ?
C4 C3 H3B 109.7 . . ?
H3A C3 H3B 108.2 . . ?

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
Cu02 N00C C00G N00D 0.000(5) . . . . ?
S003 C00H C00J S005 -176.3(3) . . . . ?
S003 C00H C00J S006 1.8(7) . . . . ?
S003 C00I C00L S004 -0.8(6) . . . . ?
S003 C00I C00L S008 179.8(3) . . . . ?
S004 C00H C00J S005 3.6(6) . . . . ?
S004 C00H C00J S006 -178.3(3) . . . . ?
S005 C00E C00F S006 -1.1(6) . . . . ?
S005 C00E C00F S00A 177.9(3) . . . . ?
S007 C00E C00F S006 178.4(3) . . . . ?
S007 C00E C00F S00A -2.6(8) . . . . ?
S009 C00I C00L S004 178.9(3) . . . . ?
S009 C00I C00L S008 -0.5(8) . . . . ?
S009 C1 C2 S008 70.7(9) . . . . ?
S009 C4 C3 S008 -68(2) . . . . ?
S00A C00K C00M S007 69.4(5) . . . . ?
C00E S005 C00J S006 1.8(3) . . . . ?
C00E S005 C00J C00H -179.9(4) . . . . ?
C00E S007 C00M C00K -43.5(5) . . . . ?
C00F S006 C00J S005 -2.3(3) . . . . ?
C00F S006 C00J C00H 179.5(5) . . . . ?
C00F S00A C00K C00M -51.1(5) . . . . ?
C00H S003 C00I S009 -174.6(3) . . . . ?
C00H S003 C00I C00L 5.1(4) . . . . ?
C00H S004 C00L S008 175.5(3) . . . . ?
C00H S004 C00L C00I -4.0(4) . . . . ?
C00I S003 C00H S004 -7.7(3) . . . . ?
C00I S003 C00H C00J 172.1(5) . . . . ?
C00I S009 C1 C2 -49.0(7) . . . . ?
C00J S005 C00E S007 -180.0(3) . . . . ?
C00J S005 C00E C00F -0.5(5) . . . . ?
C00J S006 C00F S00A -177.1(3) . . . . ?
C00J S006 C00F C00E 2.0(5) . . . . ?
C00K S00A C00F S006 -162.6(3) . . . . ?
C00K S00A C00F C00E 18.4(6) . . . . ?
C00L S004 C00H S003 7.4(3) . . . . ?
C00L S004 C00H C00J -172.4(4) . . . . ?
C00L S008 C2 C1 -46.7(8) . . . . ?
C00L S008 C3 C4 44.4(18) . . . . ?
C00M S007 C00E S005 -169.5(3) . . . . ?
C00M S007 C00E C00F 11.0(6) . . . . ?
C00N N00D C00G N00C 180.000(3) . . . . ?
C1 S009 C00I S003 -165.7(4) . . . . ?
C1 S009 C00I C00L 14.6(6) . . . . ?
C2 S008 C00L S004 -166.9(4) . . . . ?
C2 S008 C00L C00I 12.5(6) . . . . ?
C4 S009 C00I S003 168.4(6) . . . . ?
C4 S009 C00I C00L -11.2(8) . . . . ?
C3 S008 C00L S004 166.9(9) . . . . ?
C3 S008 C00L C00I -13.7(10) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.347
_oxdiff_exptl_absorpt_empirical_full_min 0.786
_exptl_crystal_recrystallization_method Electrocrystallization
_exptl_crystal_preparation       'Conducting properties'
