# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2019

####################################################################### 
# 
# 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_GL49150K
_audit_block_doi                 10.5517/ccdc.csd.cc236jgb
_database_code_depnum_ccdc_archive 'CCDC 1942691'
loop_
_citation_id
_citation_doi
_citation_year
1 10.1016/j.jinorgbio.2019.110865 2019
loop_
_audit_author_name
_audit_author_address
'Isabel Cordeiro Santos'
;CCTN, Instituto Superior Tecnico, Universidade de Lisboa
Portugal
;
_audit_update_record             
;
2019-10-02 deposited with the CCDC.	2019-11-01 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C13 H7 N S6, B F4'
_chemical_formula_sum            'C13 H7 B F4 N S6'
_chemical_formula_weight         456.37

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'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 '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      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   8.3695(3)
_cell_length_b                   9.5289(4)
_cell_length_c                   10.7213(4)
_cell_angle_alpha                92.400(2)
_cell_angle_beta                 94.961(2)
_cell_angle_gamma                91.395(2)
_cell_volume                     850.76(6)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    4182
_cell_measurement_theta_min      2.93
_cell_measurement_theta_max      27.11

_exptl_crystal_description       prism
_exptl_crystal_colour            black
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.781
_exptl_crystal_F_000             458
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.140
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.040
_exptl_absorpt_coefficient_mu    0.841
_shelx_estimated_absorpt_T_min   0.891
_shelx_estimated_absorpt_T_max   0.967
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.891
_exptl_absorpt_correction_T_max  0.967
_exptl_absorpt_process_details   sadabs
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            8699
_diffrn_reflns_av_unetI/netI     0.0387
_diffrn_reflns_av_R_equivalents  0.0319
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         2.930
_diffrn_reflns_theta_max         25.343
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 0.996
_reflns_number_total             3097
_reflns_number_gt                2628
_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       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick 2015)'
_computing_molecular_graphics    'Mercury Macrae et al,2008)'
_computing_publication_material  'WinGX (Farrugia, 2012)'
_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)+(0.0291P)²+0.2398P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         3097
_refine_ls_number_parameters     226
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0359
_refine_ls_R_factor_gt           0.0281
_refine_ls_wR_factor_ref         0.0686
_refine_ls_wR_factor_gt          0.0661
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_restrained_S_all      1.045
_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
S6 S 0.32771(6) 0.62018(5) 0.64100(5) 0.01500(13) Uani 1 1 d . . . . .
S4 S 0.53175(6) 0.81640(5) 0.47048(5) 0.01328(13) Uani 1 1 d . . . . .
S2 S 0.73319(6) 1.00878(5) 0.33793(5) 0.01624(13) Uani 1 1 d . . . . .
S5 S 0.23097(6) 0.43826(5) 0.41596(5) 0.01378(13) Uani 1 1 d . . . . .
S1 S 0.58578(7) 0.80126(6) 0.07066(5) 0.02109(14) Uani 1 1 d . . . . .
S3 S 0.41659(6) 0.64446(5) 0.24963(5) 0.01618(13) Uani 1 1 d . . . . .
F1 F 0.11609(18) -0.00100(14) 0.16783(12) 0.0365(4) Uani 1 1 d . . . . .
F2 F 0.06237(18) 0.20466(15) 0.26774(15) 0.0429(4) Uani 1 1 d . . . . .
F3 F 0.21094(18) 0.04451(14) 0.37039(13) 0.0402(4) Uani 1 1 d . . . . .
F4 F 0.31593(17) 0.16440(14) 0.21630(14) 0.0387(4) Uani 1 1 d . . . . .
N1 N 0.2238(3) 0.6126(2) 0.96896(19) 0.0366(5) Uani 1 1 d . . . . .
C13 C 0.1821(3) 0.5418(2) 0.8835(2) 0.0227(5) Uani 1 1 d . . . . .
C10 C 0.1313(3) 0.4539(2) 0.77324(19) 0.0164(4) Uani 1 1 d . . . . .
C8 C 0.1928(2) 0.48151(19) 0.65945(19) 0.0140(4) Uani 1 1 d . . . . .
C6 C 0.3363(2) 0.5852(2) 0.48221(18) 0.0125(4) Uani 1 1 d . . . . .
C5 C 0.4189(2) 0.6733(2) 0.40898(19) 0.0133(4) Uani 1 1 d . . . . .
C4 C 0.6013(2) 0.86370(19) 0.33081(19) 0.0134(4) Uani 1 1 d . . . . .
C2 C 0.7028(3) 1.0596(2) 0.17721(19) 0.0196(5) Uani 1 1 d . . . . .
H2B H 0.5908 1.0896 0.1604 0.023 Uiso 1 1 calc R U . . .
H2A H 0.7746 1.1413 0.1656 0.023 Uiso 1 1 calc R U . . .
C12 C 0.0239(3) 0.3414(2) 0.7793(2) 0.0202(5) Uani 1 1 d . . . . .
H12 H -0.0192 0.3225 0.8562 0.024 Uiso 1 1 calc R U . . .
C7 C 0.1457(2) 0.39589(19) 0.55326(19) 0.0128(4) Uani 1 1 d . . . . .
C9 C 0.0399(2) 0.2820(2) 0.5605(2) 0.0167(5) Uani 1 1 d . . . . .
H9 H 0.0096 0.2224 0.4887 0.020 Uiso 1 1 calc R U . . .
C11 C -0.0203(2) 0.2570(2) 0.6734(2) 0.0186(5) Uani 1 1 d . . . . .
H11 H -0.0935 0.1801 0.6785 0.022 Uiso 1 1 calc R U . . .
C1 C 0.7345(3) 0.9434(2) 0.0836(2) 0.0219(5) Uani 1 1 d . . . . .
H1B H 0.8409 0.9047 0.1078 0.026 Uiso 1 1 calc R U . . .
H1A H 0.7392 0.9837 0.0003 0.026 Uiso 1 1 calc R U . . .
C3 C 0.5458(2) 0.7835(2) 0.22567(19) 0.0140(4) Uani 1 1 d . . . . .
B1 B 0.1773(3) 0.1027(3) 0.2541(2) 0.0242(6) Uani 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
S6 C6 1.729(2) . ?
S6 C8 1.7457(19) . ?
S4 C5 1.7148(19) . ?
S4 C4 1.726(2) . ?
S2 C4 1.7432(19) . ?
S2 C2 1.808(2) . ?
S5 C6 1.7289(19) . ?
S5 C7 1.7482(19) . ?
S1 C3 1.738(2) . ?
S1 C1 1.810(2) . ?
S3 C5 1.717(2) . ?
S3 C3 1.7311(18) . ?
F1 B1 1.383(3) . ?
F2 B1 1.396(3) . ?
F3 B1 1.395(3) . ?
F4 B1 1.387(3) . ?
N1 C13 1.139(3) . ?
C13 C10 1.447(3) . ?
C10 C12 1.389(3) . ?
C10 C8 1.397(3) . ?
C8 C7 1.395(3) . ?
C6 C5 1.386(3) . ?
C4 C3 1.375(3) . ?
C2 C1 1.507(3) . ?
C2 H2B 0.9900 . ?
C2 H2A 0.9900 . ?
C12 C11 1.382(3) . ?
C12 H12 0.9500 . ?
C7 C9 1.393(3) . ?
C9 C11 1.378(3) . ?
C9 H9 0.9500 . ?
C11 H11 0.9500 . ?
C1 H1B 0.9900 . ?
C1 H1A 0.9900 . ?

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
C6 S6 C8 94.61(9) . . ?
C5 S4 C4 95.99(9) . . ?
C4 S2 C2 99.45(10) . . ?
C6 S5 C7 94.90(9) . . ?
C3 S1 C1 102.26(10) . . ?
C5 S3 C3 96.04(9) . . ?
N1 C13 C10 178.7(2) . . ?
C12 C10 C8 119.62(19) . . ?
C12 C10 C13 120.93(19) . . ?
C8 C10 C13 119.45(18) . . ?
C7 C8 C10 119.64(17) . . ?
C7 C8 S6 116.90(15) . . ?
C10 C8 S6 123.46(15) . . ?
C5 C6 S5 120.73(15) . . ?
C5 C6 S6 121.88(15) . . ?
S5 C6 S6 117.35(11) . . ?
C6 C5 S4 122.72(16) . . ?
C6 C5 S3 121.79(15) . . ?
S4 C5 S3 115.48(11) . . ?
C3 C4 S4 116.51(14) . . ?
C3 C4 S2 126.96(15) . . ?
S4 C4 S2 116.53(11) . . ?
C1 C2 S2 113.20(15) . . ?
C1 C2 H2B 108.9 . . ?
S2 C2 H2B 108.9 . . ?
C1 C2 H2A 108.9 . . ?
S2 C2 H2A 108.9 . . ?
H2B C2 H2A 107.8 . . ?
C11 C12 C10 119.91(19) . . ?
C11 C12 H12 120.0 . . ?
C10 C12 H12 120.0 . . ?
C9 C7 C8 120.43(18) . . ?
C9 C7 S5 123.46(16) . . ?
C8 C7 S5 116.09(14) . . ?
C11 C9 C7 119.0(2) . . ?
C11 C9 H9 120.5 . . ?
C7 C9 H9 120.5 . . ?
C9 C11 C12 121.34(19) . . ?
C9 C11 H11 119.3 . . ?
C12 C11 H11 119.3 . . ?
C2 C1 S1 114.14(14) . . ?
C2 C1 H1B 108.7 . . ?
S1 C1 H1B 108.7 . . ?
C2 C1 H1A 108.7 . . ?
S1 C1 H1A 108.7 . . ?
H1B C1 H1A 107.6 . . ?
C4 C3 S3 115.93(15) . . ?
C4 C3 S1 129.42(15) . . ?
S3 C3 S1 114.65(11) . . ?
F1 B1 F4 110.88(19) . . ?
F1 B1 F3 109.42(19) . . ?
F4 B1 F3 109.6(2) . . ?
F1 B1 F2 109.4(2) . . ?
F4 B1 F2 109.73(19) . . ?
F3 B1 F2 107.8(2) . . ?

_refine_diff_density_max         0.351
_refine_diff_density_min         -0.267
_refine_diff_density_rms         0.064

####################################################################### 
# 
# 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_(4-CNB-EDT-TTF)2[Ni(mnt)2]
_audit_block_doi                 10.5517/ccdc.csd.cc236jhc
_database_code_depnum_ccdc_archive 'CCDC 1942692'
loop_
_citation_id
_citation_doi
_citation_year
1 10.1016/j.jinorgbio.2019.110865 2019
loop_
_audit_author_name
_audit_author_address
'Isabel Cordeiro Santos'
;CCTN, Instituto Superior Tecnico, Universidade de Lisboa
Portugal
;
_audit_update_record             
;
2019-10-02 deposited with the CCDC.	2019-11-01 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C34 H14 N6 Ni S16'
_chemical_formula_weight         1078.18

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'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   7.1297(3)
_cell_length_b                   11.6789(4)
_cell_length_c                   12.4910(4)
_cell_angle_alpha                98.5220(10)
_cell_angle_beta                 92.3060(10)
_cell_angle_gamma                100.265(2)
_cell_volume                     1009.76(6)
_cell_formula_units_Z            1
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    3546
_cell_measurement_theta_min      2.62
_cell_measurement_theta_max      27.15

_exptl_crystal_description       needle
_exptl_crystal_colour            black
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.773
_exptl_crystal_F_000             544
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.020
_exptl_absorpt_coefficient_mu    1.347
_shelx_estimated_absorpt_T_min   0.552
_shelx_estimated_absorpt_T_max   0.974
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5524
_exptl_absorpt_correction_T_max  0.9736
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            9243
_diffrn_reflns_av_unetI/netI     0.0429
_diffrn_reflns_av_R_equivalents  0.0316
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         2.910
_diffrn_reflns_theta_max         25.679
_diffrn_reflns_theta_full        25.242
_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
_reflns_number_total             3821
_reflns_number_gt                3187
_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       'Bruker SMART'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2015)'
_computing_molecular_graphics    'Mercury Macrae et al,2008)'
_computing_publication_material  'WinGX (Farrugia, 2012)'
_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)+(0.0325P)²+0.0312P] 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         3821
_refine_ls_number_parameters     278
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0383
_refine_ls_R_factor_gt           0.0298
_refine_ls_wR_factor_ref         0.0725
_refine_ls_wR_factor_gt          0.0695
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_restrained_S_all      1.026
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.001

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.5000 0.0000 0.0000 0.01746(12) Uani 1 2 d S . P . .
S1 S 0.55098(9) 0.57741(5) 0.37565(5) 0.02609(16) Uani 1 1 d . . . . .
S2 S 1.00198(9) 0.58439(6) 0.26910(5) 0.02955(16) Uani 1 1 d . . . . .
S3 S 0.40906(8) 0.42741(5) 0.16926(5) 0.02028(14) Uani 1 1 d . . . . .
S4 S 0.78336(8) 0.43587(5) 0.07780(5) 0.02056(14) Uani 1 1 d . . . . .
S5 S 0.20314(8) 0.26448(5) -0.03944(5) 0.02134(15) Uani 1 1 d . . . . .
S6 S 0.57048(8) 0.26879(5) -0.14223(5) 0.02016(14) Uani 1 1 d . . . . .
S7 S 0.78629(8) 0.08588(5) 0.05632(5) 0.02189(14) Uani 1 1 d . . . . .
S8 S 0.38268(8) 0.07925(5) 0.14201(5) 0.02170(14) Uani 1 1 d . . . . .
N1 N 0.6913(3) 0.1257(2) -0.40770(18) 0.0375(6) Uani 1 1 d . . . . .
N2 N 1.0554(3) 0.2815(2) 0.29733(18) 0.0402(6) Uani 1 1 d . . . . .
N3 N 0.5350(4) 0.2703(2) 0.40701(18) 0.0421(6) Uani 1 1 d . . . . .
C1 C 0.7743(5) 0.5857(5) 0.4495(3) 0.0299(12) Uani 0.768(10) 1 d . . P A 1
H1A H 0.7673 0.6235 0.5253 0.036 Uiso 0.768(10) 1 calc R U P A 1
H1B H 0.7975 0.5049 0.4514 0.036 Uiso 0.768(10) 1 calc R U P A 1
C2 C 0.9406(6) 0.6550(5) 0.4000(3) 0.0306(12) Uani 0.768(10) 1 d . . P A 1
H2A H 1.0545 0.6696 0.4517 0.037 Uiso 0.768(10) 1 calc R U P A 1
H2B H 0.9097 0.7326 0.3912 0.037 Uiso 0.768(10) 1 calc R U P A 1
C2A C 0.9558(18) 0.5893(16) 0.4053(9) 0.030(4) Uani 0.232(10) 1 d . . P A 2
H2A1 H 0.9201 0.5079 0.4211 0.036 Uiso 0.232(10) 1 calc R U P A 2
H2A2 H 1.0732 0.6280 0.4509 0.036 Uiso 0.232(10) 1 calc R U P A 2
C1A C 0.7949(19) 0.6564(16) 0.4341(10) 0.030(4) Uani 0.232(10) 1 d . . P A 2
H1A1 H 0.8232 0.7333 0.4081 0.036 Uiso 0.232(10) 1 calc R U P A 2
H1A2 H 0.7929 0.6725 0.5141 0.036 Uiso 0.232(10) 1 calc R U P A 2
C3 C 0.6068(3) 0.50910(19) 0.25050(18) 0.0200(5) Uani 1 1 d . . . . .
C4 C 0.7786(3) 0.51244(19) 0.20897(18) 0.0204(5) Uani 1 1 d . . . . .
C5 C 0.5374(3) 0.38663(19) 0.05940(18) 0.0174(5) Uani 1 1 d . . . . .
C6 C 0.4488(3) 0.31624(19) -0.03114(18) 0.0173(5) Uani 1 1 d . . . . .
C7 C 0.1954(3) 0.17698(19) -0.16524(18) 0.0196(5) Uani 1 1 d . . . . .
C8 C 0.3692(3) 0.17958(19) -0.21368(18) 0.0199(5) Uani 1 1 d . . . . .
C9 C 0.0292(3) 0.10615(19) -0.2164(2) 0.0237(5) Uani 1 1 d . . . . .
H9 H -0.0892 0.1067 -0.1842 0.028 Uiso 1 1 calc R U . . .
C10 C 0.3734(3) 0.1110(2) -0.31482(19) 0.0233(5) Uani 1 1 d . . . . .
C11 C 0.0370(4) 0.0352(2) -0.3137(2) 0.0280(6) Uani 1 1 d . . . . .
H11 H -0.0754 -0.0160 -0.3470 0.034 Uiso 1 1 calc R U . . .
C12 C 0.2074(4) 0.0379(2) -0.3636(2) 0.0280(6) Uani 1 1 d . . . . .
H12 H 0.2106 -0.0104 -0.4315 0.034 Uiso 1 1 calc R U . . .
C13 C 0.5499(4) 0.1177(2) -0.3667(2) 0.0276(6) Uani 1 1 d . . . . .
C14 C 0.7576(3) 0.16312(19) 0.18108(18) 0.0202(5) Uani 1 1 d . . . . .
C15 C 0.5804(3) 0.15968(19) 0.21867(18) 0.0209(5) Uani 1 1 d . . . . .
C16 C 0.9245(4) 0.2289(2) 0.2448(2) 0.0255(5) Uani 1 1 d . . . . .
C17 C 0.5526(4) 0.2208(2) 0.3234(2) 0.0257(6) Uani 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
Ni1 S8 2.1475(6) . ?
Ni1 S8 2.1475(6) 2_655 ?
Ni1 S7 2.1478(6) . ?
Ni1 S7 2.1478(6) 2_655 ?
S1 C3 1.741(2) . ?
S1 C1 1.788(4) . ?
S1 C1A 1.880(13) . ?
S2 C2A 1.740(12) . ?
S2 C4 1.745(2) . ?
S2 C2 1.826(4) . ?
S3 C5 1.735(2) . ?
S3 C3 1.745(2) . ?
S4 C5 1.740(2) . ?
S4 C4 1.751(2) . ?
S5 C7 1.736(2) . ?
S5 C6 1.741(2) . ?
S6 C6 1.740(2) . ?
S6 C8 1.741(2) . ?
S7 C14 1.720(2) . ?
S8 C15 1.714(2) . ?
N1 C13 1.144(3) . ?
N2 C16 1.142(3) . ?
N3 C17 1.140(3) . ?
C1 C2 1.520(7) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C2A C1A 1.53(2) . ?
C2A H2A1 0.9900 . ?
C2A H2A2 0.9900 . ?
C1A H1A1 0.9900 . ?
C1A H1A2 0.9900 . ?
C3 C4 1.346(3) . ?
C5 C6 1.355(3) . ?
C7 C9 1.389(3) . ?
C7 C8 1.398(3) . ?
C8 C10 1.397(3) . ?
C9 C11 1.375(3) . ?
C9 H9 0.9500 . ?
C10 C12 1.389(3) . ?
C10 C13 1.434(3) . ?
C11 C12 1.385(3) . ?
C11 H11 0.9500 . ?
C12 H12 0.9500 . ?
C14 C15 1.361(3) . ?
C14 C16 1.434(3) . ?
C15 C17 1.433(3) . ?

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
S8 Ni1 S8 180.0 . 2_655 ?
S8 Ni1 S7 92.49(2) . . ?
S8 Ni1 S7 87.51(2) 2_655 . ?
S8 Ni1 S7 87.51(2) . 2_655 ?
S8 Ni1 S7 92.49(2) 2_655 2_655 ?
S7 Ni1 S7 180.0 . 2_655 ?
C3 S1 C1 98.31(15) . . ?
C3 S1 C1A 100.7(4) . . ?
C2A S2 C4 99.8(5) . . ?
C4 S2 C2 102.13(14) . . ?
C5 S3 C3 95.43(11) . . ?
C5 S4 C4 95.09(11) . . ?
C7 S5 C6 95.41(11) . . ?
C6 S6 C8 94.80(11) . . ?
C14 S7 Ni1 103.20(8) . . ?
C15 S8 Ni1 103.34(9) . . ?
C2 C1 S1 112.5(4) . . ?
C2 C1 H1A 109.1 . . ?
S1 C1 H1A 109.1 . . ?
C2 C1 H1B 109.1 . . ?
S1 C1 H1B 109.1 . . ?
H1A C1 H1B 107.8 . . ?
C1 C2 S2 115.2(3) . . ?
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 . . ?
C1A C2A S2 111.5(10) . . ?
C1A C2A H2A1 109.3 . . ?
S2 C2A H2A1 109.3 . . ?
C1A C2A H2A2 109.3 . . ?
S2 C2A H2A2 109.3 . . ?
H2A1 C2A H2A2 108.0 . . ?
C2A C1A S1 114.4(12) . . ?
C2A C1A H1A1 108.7 . . ?
S1 C1A H1A1 108.7 . . ?
C2A C1A H1A2 108.7 . . ?
S1 C1A H1A2 108.6 . . ?
H1A1 C1A H1A2 107.6 . . ?
C4 C3 S1 128.91(19) . . ?
C4 C3 S3 117.00(19) . . ?
S1 C3 S3 114.08(13) . . ?
C3 C4 S2 128.30(19) . . ?
C3 C4 S4 117.11(18) . . ?
S2 C4 S4 114.59(13) . . ?
C6 C5 S3 120.85(17) . . ?
C6 C5 S4 123.73(18) . . ?
S3 C5 S4 115.33(13) . . ?
C5 C6 S6 122.99(17) . . ?
C5 C6 S5 120.56(17) . . ?
S6 C6 S5 116.41(13) . . ?
C9 C7 C8 120.5(2) . . ?
C9 C7 S5 123.33(19) . . ?
C8 C7 S5 116.14(18) . . ?
C10 C8 C7 119.2(2) . . ?
C10 C8 S6 123.66(19) . . ?
C7 C8 S6 117.19(18) . . ?
C11 C9 C7 119.7(2) . . ?
C11 C9 H9 120.2 . . ?
C7 C9 H9 120.2 . . ?
C12 C10 C8 119.7(2) . . ?
C12 C10 C13 121.1(2) . . ?
C8 C10 C13 119.1(2) . . ?
C9 C11 C12 120.6(2) . . ?
C9 C11 H11 119.7 . . ?
C12 C11 H11 119.7 . . ?
C11 C12 C10 120.3(2) . . ?
C11 C12 H12 119.9 . . ?
C10 C12 H12 119.9 . . ?
N1 C13 C10 178.5(3) . . ?
C15 C14 C16 121.2(2) . . ?
C15 C14 S7 120.41(18) . . ?
C16 C14 S7 118.42(18) . . ?
C14 C15 C17 121.6(2) . . ?
C14 C15 S8 120.51(18) . . ?
C17 C15 S8 117.83(19) . . ?
N2 C16 C14 178.6(3) . . ?
N3 C17 C15 178.4(3) . . ?

_refine_diff_density_max         0.398
_refine_diff_density_min         -0.279
_refine_diff_density_rms         0.071

####################################################################### 
# 
# 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_GL39ClO4
_database_code_depnum_ccdc_archive 'CCDC 1942690'
loop_
_audit_author_name
_audit_author_address
'Isabel Cordeiro Santos'
;CCTN, Instituto Superior Tecnico, Universidade de Lisboa
Portugal
;
_audit_update_record             
;
2019-10-02 deposited with the CCDC.	2019-11-01 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         'C13 H7 N S6, Cl O4'
_chemical_formula_sum            'C13 H7 Cl N O4 S6'
_chemical_formula_weight         469.01

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'
O O 0.0106 0.0060 '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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   8.5243(4)
_cell_length_b                   9.5290(5)
_cell_length_c                   10.5733(5)
_cell_angle_alpha                84.939(2)
_cell_angle_beta                 82.003(2)
_cell_angle_gamma                84.714(2)
_cell_volume                     844.40(7)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    2695
_cell_measurement_theta_min      2.79
_cell_measurement_theta_max      27.04

_exptl_crystal_description       prism
_exptl_crystal_colour            black
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.845
_exptl_crystal_F_000             474
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.040
_exptl_absorpt_coefficient_mu    0.989
_shelx_estimated_absorpt_T_min   0.908
_shelx_estimated_absorpt_T_max   0.962
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9076
_exptl_absorpt_correction_T_max  0.9615
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            6264
_diffrn_reflns_av_unetI/netI     0.0571
_diffrn_reflns_av_R_equivalents  0.0402
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         3.014
_diffrn_reflns_theta_max         25.677
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measured_fraction_theta_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_point_group_measured_fraction_full 0.987
_reflns_number_total             3176
_reflns_number_gt                2556
_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       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick 2015)'
_computing_molecular_graphics    'Mercury Macrae et al,2008)'
_computing_publication_material  'WinGX (Farrugia, 2012)'
_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)+(0.0432P)²] 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         3176
_refine_ls_number_parameters     226
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0472
_refine_ls_R_factor_gt           0.0354
_refine_ls_wR_factor_ref         0.0930
_refine_ls_wR_factor_gt          0.0874
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_restrained_S_all      1.013
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_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
Cl1 Cl 0.29668(8) 0.66500(7) 0.21225(6) 0.02187(18) Uani 1 1 d . . . . .
S1 S -0.09846(9) 0.34268(7) 0.08218(6) 0.02076(18) Uani 1 1 d . . . . .
S2 S -0.24848(9) 0.52488(7) 0.35533(7) 0.01924(18) Uani 1 1 d . . . . .
S3 S 0.08218(8) 0.16371(7) 0.25995(6) 0.01649(17) Uani 1 1 d . . . . .
S4 S -0.03794(8) 0.31458(7) 0.48511(6) 0.01553(17) Uani 1 1 d . . . . .
S5 S 0.28424(8) -0.06145(7) 0.43210(6) 0.01523(17) Uani 1 1 d . . . . .
S6 S 0.17019(9) 0.09989(7) 0.65728(6) 0.01700(17) Uani 1 1 d . . . . .
O1 O 0.3790(3) 0.6598(2) 0.3231(2) 0.0367(6) Uani 1 1 d . . . . .
O2 O 0.4090(3) 0.6645(3) 0.0994(2) 0.0432(6) Uani 1 1 d . . . . .
O3 O 0.1870(3) 0.7882(2) 0.2086(2) 0.0416(6) Uani 1 1 d . . . . .
O4 O 0.2074(3) 0.5420(3) 0.2211(2) 0.0443(6) Uani 1 1 d . . . . .
N1 N 0.2732(4) 0.0813(3) 0.9806(3) 0.0379(7) Uani 1 1 d . . . . .
C1 C -0.2474(4) 0.4904(3) 0.0975(3) 0.0219(7) Uani 1 1 d . . . . .
H1B H -0.2517 0.5408 0.0120 0.026 Uiso 1 1 calc R U . . .
H1A H -0.3522 0.4532 0.1259 0.026 Uiso 1 1 calc R U . . .
C2 C -0.2203(4) 0.5959(3) 0.1899(3) 0.0211(6) Uani 1 1 d . . . . .
H2B H -0.2946 0.6810 0.1795 0.025 Uiso 1 1 calc R U . . .
H2A H -0.1107 0.6252 0.1683 0.025 Uiso 1 1 calc R U . . .
C3 C -0.0546(3) 0.3089(3) 0.2387(3) 0.0158(6) Uani 1 1 d . . . . .
C4 C -0.1106(3) 0.3785(3) 0.3449(2) 0.0150(6) Uani 1 1 d . . . . .
C5 C 0.0817(3) 0.1769(3) 0.4211(2) 0.0132(5) Uani 1 1 d . . . . .
C6 C 0.1705(3) 0.0814(3) 0.4959(2) 0.0129(6) Uani 1 1 d . . . . .
C7 C 0.3672(3) -0.1178(3) 0.5726(3) 0.0160(6) Uani 1 1 d . . . . .
C8 C 0.3138(3) -0.0392(3) 0.6783(3) 0.0153(6) Uani 1 1 d . . . . .
C9 C 0.4782(3) -0.2336(3) 0.5820(3) 0.0190(6) Uani 1 1 d . . . . .
H9 H 0.5125 -0.2882 0.5108 0.023 Uiso 1 1 calc R U . . .
C10 C 0.3753(3) -0.0754(3) 0.7942(3) 0.0193(6) Uani 1 1 d . . . . .
C11 C 0.5377(3) -0.2679(3) 0.6973(3) 0.0209(6) Uani 1 1 d . . . . .
H11 H 0.6137 -0.3466 0.7046 0.025 Uiso 1 1 calc R U . . .
C12 C 0.4888(3) -0.1898(3) 0.8019(3) 0.0216(7) Uani 1 1 d . . . . .
H12 H 0.5326 -0.2143 0.8795 0.026 Uiso 1 1 calc R U . . .
C13 C 0.3193(4) 0.0087(3) 0.9012(3) 0.0260(7) Uani 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
Cl1 O2 1.422(2) . ?
Cl1 O3 1.433(2) . ?
Cl1 O1 1.443(2) . ?
Cl1 O4 1.444(2) . ?
S1 C3 1.743(3) . ?
S1 C1 1.809(3) . ?
S2 C4 1.740(3) . ?
S2 C2 1.811(3) . ?
S3 C5 1.719(3) . ?
S3 C3 1.745(3) . ?
S4 C5 1.714(3) . ?
S4 C4 1.726(2) . ?
S5 C6 1.727(3) . ?
S5 C7 1.754(3) . ?
S6 C6 1.730(3) . ?
S6 C8 1.741(3) . ?
N1 C13 1.140(4) . ?
C1 C2 1.515(4) . ?
C1 H1B 0.9900 . ?
C1 H1A 0.9900 . ?
C2 H2B 0.9900 . ?
C2 H2A 0.9900 . ?
C3 C4 1.361(4) . ?
C5 C6 1.393(4) . ?
C7 C9 1.392(4) . ?
C7 C8 1.400(4) . ?
C8 C10 1.402(4) . ?
C9 C11 1.387(4) . ?
C9 H9 0.9500 . ?
C10 C12 1.394(4) . ?
C10 C13 1.446(4) . ?
C11 C12 1.382(4) . ?
C11 H11 0.9500 . ?
C12 H12 0.9500 . ?

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
O2 Cl1 O3 110.81(15) . . ?
O2 Cl1 O1 109.56(14) . . ?
O3 Cl1 O1 110.21(13) . . ?
O2 Cl1 O4 109.22(15) . . ?
O3 Cl1 O4 108.09(15) . . ?
O1 Cl1 O4 108.92(14) . . ?
C3 S1 C1 101.99(13) . . ?
C4 S2 C2 99.26(13) . . ?
C5 S3 C3 95.52(13) . . ?
C5 S4 C4 96.08(13) . . ?
C6 S5 C7 95.02(13) . . ?
C6 S6 C8 94.90(13) . . ?
C2 C1 S1 115.07(19) . . ?
C2 C1 H1B 108.5 . . ?
S1 C1 H1B 108.5 . . ?
C2 C1 H1A 108.5 . . ?
S1 C1 H1A 108.5 . . ?
H1B C1 H1A 107.5 . . ?
C1 C2 S2 112.64(19) . . ?
C1 C2 H2B 109.1 . . ?
S2 C2 H2B 109.1 . . ?
C1 C2 H2A 109.1 . . ?
S2 C2 H2A 109.1 . . ?
H2B C2 H2A 107.8 . . ?
C4 C3 S1 129.7(2) . . ?
C4 C3 S3 116.15(19) . . ?
S1 C3 S3 114.10(16) . . ?
C3 C4 S4 116.6(2) . . ?
C3 C4 S2 127.1(2) . . ?
S4 C4 S2 116.20(16) . . ?
C6 C5 S4 121.8(2) . . ?
C6 C5 S3 122.6(2) . . ?
S4 C5 S3 115.59(15) . . ?
C5 C6 S5 121.5(2) . . ?
C5 C6 S6 121.3(2) . . ?
S5 C6 S6 117.13(15) . . ?
C9 C7 C8 120.7(2) . . ?
C9 C7 S5 123.5(2) . . ?
C8 C7 S5 115.8(2) . . ?
C7 C8 C10 119.7(3) . . ?
C7 C8 S6 116.84(19) . . ?
C10 C8 S6 123.4(2) . . ?
C11 C9 C7 118.7(3) . . ?
C11 C9 H9 120.6 . . ?
C7 C9 H9 120.6 . . ?
C12 C10 C8 119.1(3) . . ?
C12 C10 C13 122.4(2) . . ?
C8 C10 C13 118.5(3) . . ?
C12 C11 C9 121.3(3) . . ?
C12 C11 H11 119.3 . . ?
C9 C11 H11 119.3 . . ?
C11 C12 C10 120.4(3) . . ?
C11 C12 H12 119.8 . . ?
C10 C12 H12 119.8 . . ?
N1 C13 C10 176.1(3) . . ?

_refine_diff_density_max         0.401
_refine_diff_density_min         -0.452
_refine_diff_density_rms         0.086

####################################################################### 
# 
# 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_(4-CNB-EDT-TTF)2[Au(mnt)2]
_audit_block_doi                 10.5517/ccdc.csd.cc236jjd
_database_code_depnum_ccdc_archive 'CCDC 1942693'
loop_
_citation_id
_citation_doi
_citation_year
1 10.1016/j.jinorgbio.2019.110865 2019
loop_
_audit_author_name
_audit_author_address
'Isabel Cordeiro Santos'
;CCTN, Instituto Superior Tecnico, Universidade de Lisboa
Portugal
;
_audit_update_record             
;
2019-10-02 deposited with the CCDC.	2019-11-01 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '2(C13 H7 N S6), C8 Au N4 S4'
_chemical_formula_sum            'C34 H14 Au N6 S16'
_chemical_formula_weight         1216.44

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Au Au -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   7.0948(5)
_cell_length_b                   11.7077(8)
_cell_length_c                   12.6897(10)
_cell_angle_alpha                99.134(2)
_cell_angle_beta                 91.941(4)
_cell_angle_gamma                99.753(2)
_cell_volume                     1023.65(13)
_cell_formula_units_Z            1
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    2044
_cell_measurement_theta_min      2.92
_cell_measurement_theta_max      26.66

_exptl_crystal_description       needle
_exptl_crystal_colour            black
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.973
_exptl_crystal_F_000             595
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.240
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.020
_exptl_absorpt_coefficient_mu    4.448
_shelx_estimated_absorpt_T_min   0.415
_shelx_estimated_absorpt_T_max   0.916
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.4149
_exptl_absorpt_correction_T_max  0.9163
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            6762
_diffrn_reflns_av_unetI/netI     0.0641
_diffrn_reflns_av_R_equivalents  0.0385
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         2.919
_diffrn_reflns_theta_max         25.681
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.934
_diffrn_measured_fraction_theta_full 0.934
_diffrn_reflns_Laue_measured_fraction_max 0.934
_diffrn_reflns_Laue_measured_fraction_full 0.934
_diffrn_reflns_point_group_measured_fraction_max 0.934
_diffrn_reflns_point_group_measured_fraction_full 0.934
_reflns_number_total             3641
_reflns_number_gt                3317
_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       'Bruker SMART'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2015)'
_computing_molecular_graphics    'Mercury Macrae et al,2008)'
_computing_publication_material  'WinGX (Farrugia, 2012)'
_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)+(0.0253P)²] 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         3641
_refine_ls_number_parameters     278
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0416
_refine_ls_R_factor_gt           0.0340
_refine_ls_wR_factor_ref         0.0723
_refine_ls_wR_factor_gt          0.0697
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_restrained_S_all      1.035
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.002

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
Au1 Au 0.5000 0.0000 0.0000 0.01586(10) Uani 1 2 d S . P . .
S1 S 0.5457(2) 0.57649(11) 0.37254(11) 0.0263(3) Uani 1 1 d . . . . .
S2 S 1.0015(2) 0.58409(12) 0.26828(12) 0.0300(3) Uani 1 1 d . . . . .
S3 S 0.40839(19) 0.42573(10) 0.16750(10) 0.0211(3) Uani 1 1 d . . . . .
S4 S 0.78605(18) 0.43442(10) 0.07810(10) 0.0210(3) Uani 1 1 d . . . . .
S5 S 0.20473(19) 0.26566(11) -0.04109(11) 0.0221(3) Uani 1 1 d . . . . .
S6 S 0.57529(19) 0.26974(11) -0.14223(10) 0.0209(3) Uani 1 1 d . . . . .
S7 S 0.80839(19) 0.09278(11) 0.06039(10) 0.0218(3) Uani 1 1 d . . . . .
S8 S 0.37922(19) 0.08666(11) 0.15376(10) 0.0223(3) Uani 1 1 d . . . . .
N1 N 0.6983(8) 0.1286(5) -0.4085(4) 0.0423(14) Uani 1 1 d . . . . .
N2 N 1.0655(7) 0.2824(4) 0.3024(4) 0.0397(13) Uani 1 1 d . . . . .
N3 N 0.5487(8) 0.2744(4) 0.4119(4) 0.0421(14) Uani 1 1 d . . . . .
C1 C 0.7682(14) 0.5846(13) 0.4467(8) 0.032(3) Uani 0.68(2) 1 d . . P A 1
H1A H 0.7589 0.6220 0.5215 0.038 Uiso 0.68(2) 1 calc R U P A 1
H1B H 0.7933 0.5041 0.4476 0.038 Uiso 0.68(2) 1 calc R U P A 1
C2 C 0.9334(16) 0.6544(13) 0.3988(8) 0.033(3) Uani 0.68(2) 1 d . . P A 1
H2A H 1.0467 0.6701 0.4501 0.040 Uiso 0.68(2) 1 calc R U P A 1
H2B H 0.8995 0.7312 0.3904 0.040 Uiso 0.68(2) 1 calc R U P A 1
C2A C 0.950(3) 0.587(3) 0.4033(14) 0.027(6) Uani 0.32(2) 1 d . . P A 2
H2A1 H 0.9152 0.5050 0.4168 0.032 Uiso 0.32(2) 1 calc R U P A 2
H2A2 H 1.0666 0.6247 0.4493 0.032 Uiso 0.32(2) 1 calc R U P A 2
C1A C 0.787(4) 0.653(3) 0.433(2) 0.044(8) Uani 0.32(2) 1 d . . P A 2
H1A1 H 0.8161 0.7307 0.4096 0.053 Uiso 0.32(2) 1 calc R U P A 2
H1A2 H 0.7826 0.6669 0.5114 0.053 Uiso 0.32(2) 1 calc R U P A 2
C3 C 0.6037(8) 0.5087(4) 0.2485(4) 0.0191(11) Uani 1 1 d . . . . .
C4 C 0.7783(8) 0.5121(4) 0.2076(4) 0.0225(12) Uani 1 1 d . . . . .
C5 C 0.5392(7) 0.3850(4) 0.0586(4) 0.0174(11) Uani 1 1 d . . . . .
C6 C 0.4525(7) 0.3162(4) -0.0315(4) 0.0181(11) Uani 1 1 d . . . . .
C7 C 0.1992(8) 0.1782(4) -0.1665(4) 0.0212(12) Uani 1 1 d . . . . .
C8 C 0.3740(8) 0.1816(4) -0.2132(4) 0.0201(12) Uani 1 1 d . . . . .
C9 C 0.0322(8) 0.1077(4) -0.2177(4) 0.0279(13) Uani 1 1 d . . . . .
H9 H -0.0869 0.1084 -0.1858 0.033 Uiso 1 1 calc R U . . .
C10 C 0.3782(8) 0.1131(4) -0.3158(4) 0.0253(13) Uani 1 1 d . . . . .
C11 C 0.0408(9) 0.0372(4) -0.3143(5) 0.0305(14) Uani 1 1 d . . . . .
H11 H -0.0714 -0.0140 -0.3471 0.037 Uiso 1 1 calc R U . . .
C12 C 0.2105(9) 0.0400(4) -0.3640(5) 0.0330(15) Uani 1 1 d . . . . .
H12 H 0.2139 -0.0079 -0.4315 0.040 Uiso 1 1 calc R U . . .
C13 C 0.5557(9) 0.1203(5) -0.3665(4) 0.0320(15) Uani 1 1 d . . . . .
C14 C 0.7669(8) 0.1673(4) 0.1853(4) 0.0185(11) Uani 1 1 d . . . . .
C15 C 0.5891(8) 0.1637(4) 0.2237(4) 0.0194(11) Uani 1 1 d . . . . .
C16 C 0.9343(8) 0.2326(4) 0.2503(4) 0.0252(13) Uani 1 1 d . . . . .
C17 C 0.5680(8) 0.2265(4) 0.3287(4) 0.0261(13) Uani 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
Au1 S8 2.3130(13) . ?
Au1 S8 2.3130(13) 2_655 ?
Au1 S7 2.3176(13) . ?
Au1 S7 2.3176(13) 2_655 ?
S1 C3 1.742(5) . ?
S1 C1 1.791(10) . ?
S1 C1A 1.87(3) . ?
S2 C4 1.752(5) . ?
S2 C2A 1.759(18) . ?
S2 C2 1.846(10) . ?
S3 C5 1.740(5) . ?
S3 C3 1.746(5) . ?
S4 C5 1.745(5) . ?
S4 C4 1.755(5) . ?
S5 C7 1.745(5) . ?
S5 C6 1.751(5) . ?
S6 C6 1.741(5) . ?
S6 C8 1.742(5) . ?
S7 C14 1.744(5) . ?
S8 C15 1.738(5) . ?
N1 C13 1.156(8) . ?
N2 C16 1.139(6) . ?
N3 C17 1.138(7) . ?
C1 C2 1.514(19) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C2A C1A 1.52(4) . ?
C2A H2A1 0.9900 . ?
C2A H2A2 0.9900 . ?
C1A H1A1 0.9900 . ?
C1A H1A2 0.9900 . ?
C3 C4 1.356(7) . ?
C5 C6 1.351(7) . ?
C7 C8 1.390(8) . ?
C7 C9 1.398(7) . ?
C8 C10 1.419(7) . ?
C9 C11 1.374(8) . ?
C9 H9 0.9500 . ?
C10 C12 1.401(7) . ?
C10 C13 1.430(9) . ?
C11 C12 1.375(8) . ?
C11 H11 0.9500 . ?
C12 H12 0.9500 . ?
C14 C15 1.364(7) . ?
C14 C16 1.449(7) . ?
C15 C17 1.442(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
S8 Au1 S8 180.0 . 2_655 ?
S8 Au1 S7 90.83(5) . . ?
S8 Au1 S7 89.17(5) 2_655 . ?
S8 Au1 S7 89.17(5) . 2_655 ?
S8 Au1 S7 90.83(5) 2_655 2_655 ?
S7 Au1 S7 180.0 . 2_655 ?
C3 S1 C1 99.0(4) . . ?
C3 S1 C1A 101.3(9) . . ?
C4 S2 C2A 99.3(7) . . ?
C4 S2 C2 101.7(4) . . ?
C5 S3 C3 96.0(2) . . ?
C5 S4 C4 95.4(2) . . ?
C7 S5 C6 95.6(2) . . ?
C6 S6 C8 94.8(2) . . ?
C14 S7 Au1 100.84(18) . . ?
C15 S8 Au1 100.77(18) . . ?
C2 C1 S1 111.7(10) . . ?
C2 C1 H1A 109.3 . . ?
S1 C1 H1A 109.3 . . ?
C2 C1 H1B 109.3 . . ?
S1 C1 H1B 109.3 . . ?
H1A C1 H1B 107.9 . . ?
C1 C2 S2 115.6(9) . . ?
C1 C2 H2A 108.4 . . ?
S2 C2 H2A 108.4 . . ?
C1 C2 H2B 108.4 . . ?
S2 C2 H2B 108.4 . . ?
H2A C2 H2B 107.5 . . ?
C1A C2A S2 112(2) . . ?
C1A C2A H2A1 109.3 . . ?
S2 C2A H2A1 109.3 . . ?
C1A C2A H2A2 109.2 . . ?
S2 C2A H2A2 109.2 . . ?
H2A1 C2A H2A2 107.9 . . ?
C2A C1A S1 115(2) . . ?
C2A C1A H1A1 108.6 . . ?
S1 C1A H1A1 108.6 . . ?
C2A C1A H1A2 108.6 . . ?
S1 C1A H1A2 108.6 . . ?
H1A1 C1A H1A2 107.5 . . ?
C4 C3 S1 128.7(4) . . ?
C4 C3 S3 116.7(4) . . ?
S1 C3 S3 114.6(3) . . ?
C3 C4 S2 128.2(4) . . ?
C3 C4 S4 117.0(4) . . ?
S2 C4 S4 114.8(3) . . ?
C6 C5 S3 121.1(4) . . ?
C6 C5 S4 124.0(4) . . ?
S3 C5 S4 114.9(3) . . ?
C5 C6 S6 123.5(4) . . ?
C5 C6 S5 120.5(4) . . ?
S6 C6 S5 116.0(3) . . ?
C8 C7 C9 121.1(5) . . ?
C8 C7 S5 115.6(4) . . ?
C9 C7 S5 123.2(4) . . ?
C7 C8 C10 118.3(5) . . ?
C7 C8 S6 117.9(4) . . ?
C10 C8 S6 123.9(5) . . ?
C11 C9 C7 119.8(6) . . ?
C11 C9 H9 120.1 . . ?
C7 C9 H9 120.1 . . ?
C12 C10 C8 119.6(5) . . ?
C12 C10 C13 121.8(5) . . ?
C8 C10 C13 118.6(5) . . ?
C12 C11 C9 120.6(5) . . ?
C12 C11 H11 119.7 . . ?
C9 C11 H11 119.7 . . ?
C11 C12 C10 120.5(5) . . ?
C11 C12 H12 119.8 . . ?
C10 C12 H12 119.8 . . ?
N1 C13 C10 178.2(6) . . ?
C15 C14 C16 120.2(5) . . ?
C15 C14 S7 123.3(4) . . ?
C16 C14 S7 116.4(4) . . ?
C14 C15 C17 119.7(5) . . ?
C14 C15 S8 124.2(4) . . ?
C17 C15 S8 116.1(4) . . ?
N2 C16 C14 178.9(5) . . ?
N3 C17 C15 178.7(7) . . ?

_refine_diff_density_max         0.919
_refine_diff_density_min         -1.094
_refine_diff_density_rms         0.140

# start Validation Reply Form
_vrf_PLAT029_4-CNB-EDT-TTF2Aumnt2 
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.934 Why?  
RESPONSE:the crystal was small with poor quality  
and the diffraction was weak. 
;
_vrf_PLAT911_4-CNB-EDT-TTF2Aumnt2 
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600        240 Report
RESPONSE: the crystal was small with poor quality  
and the diffraction was weak. 
;

# end Validation Reply Form


_exptl_crystal_preparation       'Magnetic properties,Transport properties'
