# Electronic Supplementary Material (ESI) for Chemical Science.
# This journal is © The Royal Society of Chemistry 2023

####################################################################### 
# 
# 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_mo_dcys_chcl3_0ma_b
_database_code_depnum_ccdc_archive 'CCDC 2235371'
loop_
_audit_author_name
_audit_author_address
'Jatish Kumar'
;Indian Institute of Science Education and Research (IISER) Tirupati
India
;
_audit_update_record             
;
2023-01-10 deposited with the CCDC.	2023-04-24 downloaded from the CCDC.
;
_audit_creation_date             2023-01-10
_audit_creation_method           
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_shelx_SHELXL_version_number     2019/1
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C11 H24 Cu10 I8 N4 O4.333 S4'
_chemical_formula_sum            'C11 H24 Cu10 I8 N4 O4.33 S4'
_chemical_formula_weight         2060.46
_chemical_absolute_configuration .
_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'
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'

_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      monoclinic
_space_group_IT_number           5
_space_group_name_H-M_alt        'C 1 2 1'
_space_group_name_Hall           'C 2y'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'

_cell_length_a                   7.373(3)
_cell_length_b                   12.555(4)
_cell_length_c                   12.999(5)
_cell_angle_alpha                90
_cell_angle_beta                 95.859(12)
_cell_angle_gamma                90
_cell_volume                     1197.0(7)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    1205
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      24.61
_cell_measurement_theta_min      3.15
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    9.702
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.4594
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1192 before and 0.0760 after correction.
The Ratio of minimum to maximum transmission is 0.6165.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            ?
_exptl_crystal_density_diffrn    2.858
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             931
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0805
_diffrn_reflns_av_unetI/netI     0.0822
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            6218
_diffrn_reflns_point_group_measured_fraction_full 0.906
_diffrn_reflns_point_group_measured_fraction_max 0.905
_diffrn_reflns_theta_full        25.065
_diffrn_reflns_theta_max         25.065
_diffrn_reflns_theta_min         3.151
_diffrn_ambient_temperature      100.00
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.734
_reflns_Friedel_fraction_full    0.808
_reflns_Friedel_fraction_max     0.807
_reflns_number_gt                1402
_reflns_number_total             1939
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _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. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         2.801
_refine_diff_density_min         -1.910
_refine_diff_density_rms         0.401
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.56(15)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     101
_refine_ls_number_reflns         1939
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0968
_refine_ls_R_factor_gt           0.0685
_refine_ls_restrained_S_all      1.045
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1185P)²+13.2650P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1756
_refine_ls_wR_factor_ref         0.2021
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.44(15)
 0.56(15)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H,H) groups
3. Restrained distances
 O1-C7
 1.3 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(N1) = Uanis(O3)
5. Others
 Fixed Sof: O1(0.75) C7(0.75) O3(0.33333)
6.a Ternary CH refined with riding coordinates:
 C00D(H00D)
6.b Secondary CH2 refined with riding coordinates:
 C009(H00A,H00B)
6.c Idealised Me refined as rotating group:
 N1(H1A,H1B,H1C)
;
_atom_sites_solution_hydrogens   geom
_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
I001 I 0.2098(4) 0.58929(16) 0.6424(2) 0.0330(11) Uani 1 1 d . . . . .
Cu1 Cu 0.1389(9) 0.2558(6) 0.4364(6) 0.040(2) Uani 1 1 d . . . . .
I02 I 0.2910(4) 0.74647(15) 0.3578(3) 0.0324(12) Uani 1 1 d . . . . .
Cu03 Cu 0.1399(9) 0.5786(5) 0.4370(6) 0.0350(19) Uani 1 1 d . . . . .
Cu04 Cu 0.500000 0.4153(11) 0.500000 0.0410(12) Uani 1 2 d S T P . .
S006 S 0.2586(8) 0.4191(14) 0.3921(5) 0.0304(15) Uani 1 1 d . . . . .
O1 O 0.215(5) 0.396(5) 0.007(2) 0.07(2) Uani 0.75 1 d D . P . .
C009 C 0.342(4) 0.415(6) 0.266(2) 0.038(7) Uani 1 1 d . . . . .
H00A H 0.461325 0.451736 0.269043 0.045 Uiso 1 1 calc R U . . .
H00B H 0.360701 0.339919 0.246061 0.045 Uiso 1 1 calc R U . . .
N1 N 0.025(4) 0.407(5) 0.171(2) 0.063(12) Uani 1 1 d . . . . .
H1A H -0.023280 0.407236 0.104151 0.075 Uiso 1 1 calc R U . . .
H1B H -0.054656 0.437369 0.211458 0.075 Uiso 1 1 calc R U . . .
H1C H 0.046122 0.338023 0.192230 0.075 Uiso 1 1 calc R U . . .
C00D C 0.206(5) 0.469(4) 0.182(3) 0.055(12) Uani 1 1 d . . . . .
H00D H 0.183451 0.544224 0.203212 0.066 Uiso 1 1 calc R U . . .
C7 C 0.281(6) 0.468(4) 0.074(3) 0.046(15) Uani 0.75 1 d D . P . .
O3 O 0.447(12) 0.540(9) 0.077(6) 0.063(12) Uani 0.3333 1 d . . P . .


_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 Cu1 2.626(8) 4_556 ?
I001 Cu03 2.671(8) . ?
I001 Cu03 2.681(7) 2_556 ?
Cu1 Cu1 2.760(14) 2_556 ?
Cu1 I02 2.665(7) 3_445 ?
Cu1 I02 2.676(9) 4_546 ?
Cu1 S006 2.328(17) . ?
I02 Cu03 2.642(8) . ?
Cu03 Cu03 2.762(13) 2_556 ?
Cu03 S006 2.286(16) . ?
Cu04 S006 2.151(6) . ?
Cu04 S006 2.151(6) 2_656 ?
S006 C009 1.81(3) . ?
O1 C7 1.32(3) . ?
C009 H00A 0.9900 . ?
C009 H00B 0.9900 . ?
C009 C00D 1.56(5) . ?
N1 H1A 0.9100 . ?
N1 H1B 0.9100 . ?
N1 H1C 0.9100 . ?
N1 C00D 1.54(6) . ?
C00D H00D 1.0000 . ?
C00D C7 1.57(6) . ?
C7 O3 1.52(12) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Cu1 I001 Cu03 72.3(2) 4_556 . ?
Cu1 I001 Cu03 108.7(2) 4_556 2_556 ?
Cu03 I001 Cu03 62.1(3) . 2_556 ?
I001 Cu1 Cu1 127.19(18) 4_546 2_556 ?
I001 Cu1 I02 108.0(3) 4_546 4_546 ?
I001 Cu1 I02 104.3(3) 4_546 3_445 ?
I02 Cu1 Cu1 59.1(3) 3_445 2_556 ?
I02 Cu1 Cu1 58.7(3) 4_546 2_556 ?
I02 Cu1 I02 117.5(3) 3_445 4_546 ?
S006 Cu1 I001 114.7(4) . 4_546 ?
S006 Cu1 Cu1 118.1(3) . 2_556 ?
S006 Cu1 I02 108.6(3) . 3_445 ?
S006 Cu1 I02 104.3(3) . 4_546 ?
Cu1 I02 Cu1 62.2(3) 3 4_556 ?
Cu03 I02 Cu1 72.0(2) . 4_556 ?
Cu03 I02 Cu1 108.2(2) . 3 ?
I001 Cu03 I001 117.5(3) . 2_556 ?
I001 Cu03 Cu03 59.1(3) . 2_556 ?
I001 Cu03 Cu03 58.8(2) 2_556 2_556 ?
I02 Cu03 I001 103.7(3) . 2_556 ?
I02 Cu03 I001 107.7(3) . . ?
I02 Cu03 Cu03 126.97(16) . 2_556 ?
S006 Cu03 I001 105.1(3) . . ?
S006 Cu03 I001 108.9(3) . 2_556 ?
S006 Cu03 I02 114.3(4) . . ?
S006 Cu03 Cu03 118.7(3) . 2_556 ?
S006 Cu04 S006 177.5(12) . 2_656 ?
Cu03 S006 Cu1 122.9(3) . . ?
Cu04 S006 Cu1 97.4(6) . . ?
Cu04 S006 Cu03 99.5(7) . . ?
C009 S006 Cu1 112(2) . . ?
C009 S006 Cu03 116(2) . . ?
C009 S006 Cu04 104.8(9) . . ?
S006 C009 H00A 109.3 . . ?
S006 C009 H00B 109.3 . . ?
H00A C009 H00B 108.0 . . ?
C00D C009 S006 111(3) . . ?
C00D C009 H00A 109.3 . . ?
C00D C009 H00B 109.3 . . ?
H1A N1 H1B 109.5 . . ?
H1A N1 H1C 109.5 . . ?
H1B N1 H1C 109.5 . . ?
C00D N1 H1A 109.5 . . ?
C00D N1 H1B 109.5 . . ?
C00D N1 H1C 109.5 . . ?
C009 C00D H00D 109.7 . . ?
N1 C00D C009 109(4) . . ?
N1 C00D H00D 109.7 . . ?
N1 C00D C7 107(3) . . ?
C7 C00D C009 111(3) . . ?
C7 C00D H00D 109.7 . . ?
O1 C7 C00D 117(4) . . ?
O1 C7 O3 132(5) . . ?
O3 C7 C00D 109(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
Cu1 S006 C009 C00D 103(4) . . . . ?
Cu03 S006 C009 C00D -45(4) . . . . ?
Cu04 S006 C009 C00D -153(3) . . . . ?
S006 C009 C00D N1 -63(5) . . . . ?
S006 C009 C00D C7 179(4) . . . . ?
C009 C00D C7 O1 101(5) . . . . ?
C009 C00D C7 O3 -68(6) . . . . ?
N1 C00D C7 O1 -18(6) . . . . ?
N1 C00D C7 O3 173(5) . . . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.000 0.707 0.000 113.4 152.7 ?
2 0.500 0.207 0.000 113.4 152.7 ?

_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.44(15)
2 0.56(15)

# start Validation Reply Form
_vrf_PLAT430_mo_dcys_chcl3_0ma_b 
;
PROBLEM: Short Inter D...A Contact  O3       ..O3       .       2.22 Ang.  
RESPONSE: This alert is generated because crystal structure ishighly
disordered, especially the side chains.
;
_vrf_PLAT342_mo_dcys_chcl3_0ma_b 
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............       0.06 Ang.  
RESPONSE: There is large amount of disorder in the crystal structure.
;
_vrf_PLAT971_mo_dcys_chcl3_0ma_b 
;
PROBLEM: Check Calcd Resid. Dens.  0.13Ang From I02             2.90 eA-3  
RESPONSE: This alert is generated because of the insufficient absorption
correction which is common for heavy atoms.
;
_vrf_PLAT973_mo_dcys_chcl3_0ma_b 
;
PROBLEM: Check Calcd Positive Resid. Density on      Cu03       1.75 eA-3  
RESPONSE: This atert is generated because the heavy atoms are present in 
the crystal structure.
;
# end Validation Reply Form
####################################################################### 
# 
# 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_mo_lcys_0ma_sq
_database_code_depnum_ccdc_archive 'CCDC 2235372'
loop_
_audit_author_name
_audit_author_address
'Jatish Kumar'
;Indian Institute of Science Education and Research (IISER) Tirupati
India
;
_audit_update_record             
;
2023-01-10 deposited with the CCDC.	2023-04-24 downloaded from the CCDC.
;
_audit_creation_date             2023-01-10
_audit_creation_method           
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_shelx_SHELXL_version_number     2019/1
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C2.5 H4 Cu2.5 I2 N0.5 O1.5 S'
_chemical_formula_sum            'C2.50 H4 Cu2.50 I2 N0.50 O1.50 S'
_chemical_formula_weight         509.77
_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'
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'

_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      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   7.155(7)
_cell_length_b                   7.155(7)
_cell_length_c                   12.562(18)
_cell_angle_alpha                92.42(3)
_cell_angle_beta                 92.42(3)
_cell_angle_gamma                118.10
_cell_volume                     565.4(11)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    1873
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      25.555
_cell_measurement_theta_min      3.236
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    10.269
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.2064
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1729 before and 0.1100 after correction.
The Ratio of minimum to maximum transmission is 0.2769.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'metallic yellowish'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_density_diffrn    2.994
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             458
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.03
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.2326
_diffrn_reflns_av_unetI/netI     0.3267
_diffrn_reflns_Laue_measured_fraction_full 0.924
_diffrn_reflns_Laue_measured_fraction_max 0.924
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            4597
_diffrn_reflns_point_group_measured_fraction_full 0.924
_diffrn_reflns_point_group_measured_fraction_max 0.924
_diffrn_reflns_theta_full        24.389
_diffrn_reflns_theta_max         24.389
_diffrn_reflns_theta_min         3.236
_diffrn_ambient_temperature      100.00
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.924
_diffrn_measured_fraction_theta_max 0.924
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and 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                663
_reflns_number_total             1734
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _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. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    ?
_refine_diff_density_max         2.464
_refine_diff_density_min         -1.775
_refine_diff_density_rms         0.454
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.140
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     95
_refine_ls_number_reflns         1734
_refine_ls_number_restraints     98
_refine_ls_R_factor_all          0.2766
_refine_ls_R_factor_gt           0.1417
_refine_ls_restrained_S_all      2.441
_refine_ls_shift/su_max          0.019
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.2000P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3482
_refine_ls_wR_factor_ref         0.4197
_refine_special_details          
;
 Refined as a 2-component twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.551(11)
 0.449(11)
2. Fixed Uiso
 At 1.2 times of:
  All N(H,H) groups
3. Restrained distances
 C34-C4
 1.5 with sigma of 0.02
 C61-C34
 1.5 with sigma of 0.02
 C61-O1
 1.4 with sigma of 0.0001
 C34-S3
 2.4 with sigma of 0.02
 C61-C4
 2.2 with sigma of 0.02
 C4-C61
 2.5 with sigma of 0.02
 C34-O1
 2.3 with sigma of 0.02
 C34-C61
 1.3 with sigma of 0.02
 S3-C34
 2.6 with sigma of 0.02
 N12-O53
 4 with sigma of 0.02
 S3-N12
 3 with sigma of 0.02
 O53-N12
 3 with sigma of 0.02
 C34-N12
 1.3 with sigma of 0.02
 Cu5_$1-C4
 2 with sigma of 0.02
 C4-Cu5_$1
 4 with sigma of 0.02
 N12-I1_$2
 3 with sigma of 0.02
 O53-O53_$3
 2 with sigma of 0.02
 N12-I6_$4
 2.6 with sigma of 0.02
 C61-O53
 1.5 with sigma of 0.02
 O1-O53
 2.2 with sigma of 0.02
 O1-C61
 1.35 with sigma of 0.02
 H4A-N12
 2.3 with sigma of 0.02
 N12-H4A
 2.2 with sigma of 0.02
 H4A-C4
 1.28 with sigma of 0.02
 C4-H4A
 1.11 with sigma of 0.02
 H4A-C34
 1.6 with sigma of 0.02
 C34-H4A
 2 with sigma of 0.02
 C34-H34
 1 with sigma of 0.02
 H34-C34
 1 with sigma of 0.02
 H34-C4
 2 with sigma of 0.02
 H4B-C4
 1.3 with sigma of 0.02
 H4A-H4B
 2 with sigma of 0.02
4. Rigid bond restraints
 Cu2, S3, C4, C34
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 O53
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C34
 with sigma for 1-2 distances of 0.0001 and sigma for 1-3 distances of 0.0001
 I1, I6
 with sigma for 1-2 distances of 0.1 and sigma for 1-3 distances of 0.1
 I1, Cu5
 with sigma for 1-2 distances of 0.1 and sigma for 1-3 distances of 0.1
5. Uiso/Uaniso restraints and constraints
N12 \\sim C4 \\sim C34: within 2A with sigma of 0.0001 and sigma for terminal
atoms of 0.0002 within 2A
C34: within 2A with sigma of 0.001 and sigma for terminal atoms of 0.002 within
2A
Cu2 \\sim C4 \\sim C34: within 2A with sigma of 0.001 and sigma for terminal
atoms of 0.002 within 2A
O53: within 2A with sigma of 0.001 and sigma for terminal atoms of 0.002 within
2A
C34 \\sim H34: within 2A with sigma of 0.001 and sigma for terminal atoms of
0.002 within 2A
C4 \\sim H4B: within 2A with sigma of 0.001 and sigma for terminal atoms of
0.002 within 2A
I1 \\sim Cu5: within 2A with sigma of 0.1 and sigma for terminal atoms of 0.2
within 2A
I1 \\sim I6: within 2A with sigma of 0.1 and sigma for terminal atoms of 0.2
within 2A
Uanis(N12) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(C34) \\sim Ueq, Uanis(Cu2)
\\sim Ueq, Uanis(O1) \\sim Ueq: with sigma of 0.001 and sigma for terminal
atoms of 0.002
Uanis(C61) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O53) = Uanis(C61) = Uanis(O1)
Uanis(N12) = Uanis(O53)
Uanis(Cu1) = Uanis(S3)
6. Others
 Fixed Sof: C34(0.5) N12(0.5) H12A(0.5) H12B(0.5) O1(0.5)
7.a X=CH2 refined with riding coordinates:
 N12(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
S3 S 0.775(3) 0.760(3) 0.3917(14) 0.0546(18) Uani 1 1 d D U . A 1
Cu1 Cu 0.4824(18) 0.8023(18) 0.4397(10) 0.0546(18) Uani 1 1 d . . . A 1
Cu5 Cu 0.1849(19) 0.507(2) 0.555(2) 0.170(11) Uani 1 1 d . U . A 1
I1 I 0.5327(12) 0.8793(11) 0.6547(7) 0.089(3) Uani 1 1 d . U . A 1
I6 I 0.1340(9) 0.4655(8) 0.3581(8) 0.078(3) Uani 1 1 d . . . A 1
Cu2 Cu 1.000000 1.000000 0.500000 0.0746(18) Uani 1 2 d S U P . .
C4 C 0.740(10) 0.712(9) 0.2614(18) 0.0763(13) Uani 1 1 d D U . . .
C34 C 0.882(5) 0.627(7) 0.2276(17) 0.0763(13) Uani 0.5 1 d D U P A .
C61 C 0.8254(6) 0.5473(9) 0.1189(9) 0.0763(13) Uani 1 1 d D U . . .
O53 O 0.8448(19) 0.448(6) 0.009(2) 0.0763(13) Uani 1 1 d D . . . .
N12 N 1.087(4) 0.741(3) 0.2486(17) 0.0763(13) Uani 0.5 1 d D U P . .
H12A H 1.174143 0.761335 0.197667 0.092 Uiso 0.5 1 calc R U P A .
H12B H 1.138274 0.797228 0.313823 0.092 Uiso 0.5 1 calc R U P . .
O1 O 0.6486(6) 0.5693(9) 0.0843(10) 0.0763(13) Uani 0.5 1 d D U P A 1
H4A H 0.852(10) 0.860(13) 0.213(13) 0.01(11) Uiso 1 1 d D . . . .
H34 H 0.86(5) 0.51(5) 0.27(3) 0.0763(14) Uiso 1 1 d D U . . .
H4B H 0.55(2) 0.63(6) 0.21(3) 0.0763(14) Uiso 1 1 d D U . . .


_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
S3 Cu1 2.35(2) . ?
S3 Cu5 2.18(3) 2_666 ?
S3 Cu2 2.099(18) . ?
S3 C4 1.64(3) . ?
Cu1 Cu1 3.05(2) 2_676 ?
Cu1 Cu5 2.720(16) . ?
Cu1 I1 2.708(13) . ?
Cu1 I1 2.656(15) 2_676 ?
Cu1 I6 2.644(11) . ?
Cu5 Cu5 2.90(4) 2_566 ?
Cu5 I1 2.839(17) . ?
Cu5 I6 2.47(3) . ?
Cu5 I6 2.655(18) 2_566 ?
C4 C34 1.48(2) . ?
C4 H4A 1.196(16) . ?
C4 H4B 1.30(2) . ?
C34 C61 1.423(13) . ?
C34 N12 1.31(2) . ?
C34 H34 1.000(16) . ?
C61 O53 1.561(16) . ?
C61 O1 1.4000(12) . ?
N12 H12A 0.8800 . ?
N12 H12B 0.8800 . ?

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
Cu5 S3 Cu1 120.5(8) 2_666 . ?
Cu2 S3 Cu1 96.3(8) . . ?
Cu2 S3 Cu5 98.8(10) . 2_666 ?
C4 S3 Cu1 104.6(18) . . ?
C4 S3 Cu5 102.6(12) . 2_666 ?
C4 S3 Cu2 136(2) . . ?
S3 Cu1 Cu1 124.3(8) . 2_676 ?
S3 Cu1 Cu5 119.2(8) . . ?
S3 Cu1 I1 111.8(7) . 2_676 ?
S3 Cu1 I1 105.6(7) . . ?
S3 Cu1 I6 107.7(6) . . ?
Cu5 Cu1 Cu1 98.0(6) . 2_676 ?
I1 Cu1 Cu1 56.2(4) 2_676 2_676 ?
I1 Cu1 Cu1 54.6(4) . 2_676 ?
I1 Cu1 Cu5 63.1(5) . . ?
I1 Cu1 Cu5 128.4(6) 2_676 . ?
I1 Cu1 I1 110.7(5) 2_676 . ?
I6 Cu1 Cu1 127.8(6) . 2_676 ?
I6 Cu1 Cu5 54.9(6) . . ?
I6 Cu1 I1 103.2(5) . 2_676 ?
I6 Cu1 I1 117.8(4) . . ?
S3 Cu5 Cu1 120.2(8) 2_666 . ?
S3 Cu5 Cu5 127.9(9) 2_666 2_566 ?
S3 Cu5 I1 106.2(9) 2_666 . ?
S3 Cu5 I6 107.6(9) 2_666 . ?
S3 Cu5 I6 112.9(10) 2_666 2_566 ?
Cu1 Cu5 Cu5 97.3(11) . 2_566 ?
Cu1 Cu5 I1 58.3(3) . . ?
I1 Cu5 Cu5 124.8(7) . 2_566 ?
I6 Cu5 Cu1 126.2(7) 2_566 . ?
I6 Cu5 Cu1 61.0(6) . . ?
I6 Cu5 Cu5 58.6(10) . 2_566 ?
I6 Cu5 Cu5 52.7(5) 2_566 2_566 ?
I6 Cu5 I1 119.0(7) . . ?
I6 Cu5 I1 99.8(7) 2_566 . ?
I6 Cu5 I6 111.4(7) . 2_566 ?
Cu1 I1 Cu1 69.3(5) 2_676 . ?
Cu1 I1 Cu5 58.7(5) . . ?
Cu1 I1 Cu5 104.9(6) 2_676 . ?
Cu1 I6 Cu5 105.5(5) . 2_566 ?
Cu5 I6 Cu1 64.1(3) . . ?
Cu5 I6 Cu5 68.6(7) . 2_566 ?
S3 Cu2 S3 180.0(11) 2_776 . ?
S3 C4 H4A 114(10) . . ?
S3 C4 H4B 122(10) . . ?
C34 C4 S3 108(2) . . ?
C34 C4 H4A 83.7(14) . . ?
C34 C4 H4B 116(10) . . ?
H4A C4 H4B 106(2) . . ?
C4 C34 H34 106(2) . . ?
C61 C34 C4 108.7(15) . . ?
C61 C34 H34 110(10) . . ?
N12 C34 C4 119(4) . . ?
N12 C34 C61 113.2(19) . . ?
N12 C34 H34 98(10) . . ?
C34 C61 O53 156.5(13) . . ?
O1 C61 C34 108.3(11) . . ?
O1 C61 O53 95.2(11) . . ?
C34 N12 H12A 120.0 . . ?
C34 N12 H12B 120.0 . . ?
H12A N12 H12B 120.0 . . ?

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
S3 C4 C34 C61 169(3) . . . . ?
S3 C4 C34 N12 -59(5) . . . . ?
Cu1 S3 C4 C34 -165(4) . . . . ?
Cu5 S3 C4 C34 -38(4) 2_666 . . . ?
Cu2 S3 C4 C34 79(4) . . . . ?
C4 C34 C61 O53 175(5) . . . . ?
C4 C34 C61 O1 -3(4) . . . . ?
N12 C34 C61 O53 40(8) . . . . ?
N12 C34 C61 O1 -138(2) . . . . ?

_platon_squeeze_details          ?
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 -0.042 -0.030 0.000 289 364 ' '

_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.551(11)
2 0.449(11)

# start Validation Reply Form
_vrf_RINTA01_mo_lcys_0ma_sq      
;
PROBLEM: The value of Rint is greater than 0.18
RESPONSE: The crystals were poorly diffracting in nature.
;
_vrf_SYMMS02_mo_lcys_0ma_sq      
;
PROBLEM: The unit-cell lengths a and b should not be equal for a
RESPONSE: Even though the unit cell was checked for higher symmetry
using multiple methods (cellnow, reciprocal lattice, xprep, platon)
the programme could not find it. This alert is believed to be
generated due to the merohedral twinning, which was further complicated
by absorption correction.
;
_vrf_PLAT029_mo_lcys_0ma_sq      
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.924 Why?  
RESPONSE: The poor diffraction results in poor overall data completeness
although the 2 theta value was maintained close to 50 degrees.
;
_vrf_PLAT213_mo_lcys_0ma_sq      
;
PROBLEM: Atom I6              has ADP max/min Ratio .....       29.7 prolat
RESPONSE: A large amount of disorder in the structure dissipated 
and modelling was not converging.
;
_vrf_PLAT351_mo_lcys_0ma_sq      
;
PROBLEM: Long   C-H (X0.96,N1.08A)  C4       - H4B      .       1.30 Ang.  
RESPONSE: A large amount of disorder in the structure dissipated 
and modelling was not converging.
;
_vrf_PLAT430_mo_lcys_0ma_sq      
;
PROBLEM: Short Inter D...A Contact  O53      ..O53      .       2.01 Ang.  
RESPONSE: A large amount of disorder in the structure dissipated 
and modelling was not converging.
;
_vrf_PLAT020_mo_lcys_0ma_sq      
;
PROBLEM: The Value of Rint is Greater Than 0.12 .........      0.233 Report
RESPONSE: The crystals were poorly diffracting in nature.
;
_vrf_PLAT026_mo_lcys_0ma_sq      
;
PROBLEM: Ratio Observed / Unique Reflections (too) Low ..        38% Check 
RESPONSE: The crystals were poorly diffracting in nature.
;
_vrf_PLAT084_mo_lcys_0ma_sq      
;
PROBLEM: High wR2 Value (i.e. > 0.25) ...................       0.42 Report
RESPONSE: The crystals were poorly diffracting in nature.
;
_vrf_PLAT241_mo_lcys_0ma_sq      
;
PROBLEM: High   'MainMol' Ueq as Compared to Neighbors of        Cu5 Check 
RESPONSE: A large amount of disorder in the structure dissipated 
and modelling was not converging.
;
_vrf_PLAT245_mo_lcys_0ma_sq      
;
PROBLEM: U(iso) H4A       Smaller than U(eq) C4        by      0.066 Ang**2
RESPONSE: A large amount of disorder in the structure dissipated 
and modelling was not converging.
;
_vrf_PLAT911_mo_lcys_0ma_sq      
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.581        142 Report
RESPONSE: Probaly due to beam stopper.
;
_vrf_PLAT722_mo_lcys_0ma_sq      
;
PROBLEM: Angle   Calc      109.00, Rep      106(2) Dev...       3.00 Degree
RESPONSE: A large amount of disorder in the structure dissipated 
and modelling was not converging.
;
# end Validation Reply Form
