# Electronic Supplementary Material (ESI) for Journal of Materials Chemistry A.
# This journal is © The Royal Society of Chemistry 2024

####################################################################### 
# 
# 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_cs_ca_nds_dmso_3_150323
_database_code_depnum_ccdc_archive 'CCDC 2336802'
loop_
_audit_author_name
_audit_author_address
'Christopher Pask'
;University of Leeds
United Kingdom
;
_audit_update_record             
;
2024-03-01 deposited with the CCDC.	2024-06-18 downloaded from the CCDC.
;
_audit_creation_date             2024-03-01
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C14 H18 Ca O8 S4'
_chemical_formula_sum            'C14 H18 Ca O8 S4'
_chemical_formula_weight         482.60
_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 0.0181 0.0091 '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'
Ca Ca 0.3641 1.2855 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 '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           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   5.4131(2)
_cell_length_b                   16.6724(6)
_cell_length_c                   10.7173(3)
_cell_angle_alpha                90
_cell_angle_beta                 103.282(3)
_cell_angle_gamma                90
_cell_volume                     941.36(6)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    4217
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      72.5830
_cell_measurement_theta_min      4.9590
_shelx_estimated_absorpt_T_max   0.808
_shelx_estimated_absorpt_T_min   0.625
_exptl_absorpt_coefficient_mu    7.411
_exptl_absorpt_correction_T_max  0.834
_exptl_absorpt_correction_T_min  0.713
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.81a (Rigaku Oxford Diffraction, 2023)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.703
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             500
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
1 -11 -1 0.0179
-1 11 1 0.0179
-1 0 -6 0.0273
1 0 6 0.0273
0 -10 2 0.0171
0 10 -2 0.0171
3 1 -2 0.0187
-3 -1 2 0.0187

_exptl_crystal_size_max          0.07
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0524
_diffrn_reflns_av_unetI/netI     0.0361
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            8897
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.705
_diffrn_reflns_theta_min         5.001
_diffrn_ambient_temperature      100.15
_diffrn_detector_area_resol_mean 5.3095
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -108.00 -16.00   1.00    8.00    --  -38.50 -44.00 -44.00   92
  2  ω    -61.00  31.00   1.00    8.00    --  -38.50  44.00 105.00   92
  3  ω    -28.00  64.00   1.00    8.00    --   41.96 -44.00 -44.00   92
  4  ω     20.00 112.00   1.00    8.00    --   41.96  44.00 105.00   92
  5  ω     81.00 173.00   1.00   32.00    --  103.10  44.00 105.00   92
  6  ω     33.00 125.00   1.00   32.00    --  103.10 -44.00 -44.00   92
  7  ω    -26.00  67.00   1.00    8.00    --   41.96 -57.00-150.00   93
  8  ω     77.00 172.00   1.00   32.00    --  103.10  61.00  30.00   95
  9  ω     81.00 173.00   1.00   32.00    --  103.10  45.00 150.00   92
 10  ω     81.00 173.00   1.00   32.00    --  103.10  45.00   0.00   92
 11  ω     35.00 129.00   1.00   32.00    --  103.10 -61.00-180.00   94
 12  ω     34.00 126.00   1.00   32.00    --  103.10 -45.00 120.00   92
 13  ω     17.00 110.00   1.00    8.00    --   41.96  57.00-120.00   93
 14  ω     17.00 110.00   1.00    8.00    --   41.96  57.00 150.00   93
 15  ω    -26.00  67.00   1.00    8.00    --   41.96 -57.00  90.00   93
 16  ω     77.00 172.00   1.00   32.00    --  103.10  61.00-150.00   95
 17  ω     77.00 172.00   1.00   32.00    --  103.10  61.00 -90.00   95
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1656
_reflns_number_total             1855
_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 1.171.42.81a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.81a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.81a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_refine_diff_density_max         0.915
_refine_diff_density_min         -0.358
_refine_diff_density_rms         0.110
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.218
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     126
_refine_ls_number_reflns         1855
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0570
_refine_ls_R_factor_gt           0.0505
_refine_ls_restrained_S_all      1.218
_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)+(0.0556P)²+1.6044P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1245
_refine_ls_wR_factor_ref         0.1276
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4)
2.b Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C7(H7A,H7B,H7C)
;
_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
Ca1 Ca 0.5000 0.5000 0.0000 0.0146(3) Uani 1 2 d S . P . .
S1 S 0.08250(16) 0.43039(5) 0.20967(8) 0.0156(2) Uani 1 1 d . . . . .
S2 S 0.70564(17) 0.69926(6) 0.12981(8) 0.0198(2) Uani 1 1 d . . . . .
O1 O 0.2325(5) 0.46961(17) 0.1310(2) 0.0218(6) Uani 1 1 d . . . . .
O2 O 0.1732(5) 0.35135(16) 0.2523(2) 0.0212(6) Uani 1 1 d . . . . .
O3 O -0.1874(5) 0.43054(16) 0.1468(2) 0.0190(6) Uani 1 1 d . . . . .
O4 O 0.6014(5) 0.61487(17) 0.1209(3) 0.0239(6) Uani 1 1 d . . . . .
C1 C 0.1185(7) 0.4913(2) 0.3490(3) 0.0165(7) Uani 1 1 d . . . . .
C2 C 0.2998(7) 0.5501(2) 0.3668(3) 0.0172(7) Uani 1 1 d . . . . .
H2 H 0.3927 0.5596 0.3030 0.021 Uiso 1 1 calc R U . . .
C3 C 0.3488(7) 0.5968(2) 0.4801(3) 0.0177(7) Uani 1 1 d . . . . .
H3 H 0.4759 0.6371 0.4923 0.021 Uiso 1 1 calc R U . . .
C4 C 0.2157(7) 0.5844(2) 0.5721(3) 0.0178(7) Uani 1 1 d . . . . .
H4 H 0.2505 0.6167 0.6471 0.021 Uiso 1 1 calc R U . . .
C5 C 0.0259(7) 0.5241(2) 0.5573(3) 0.0170(7) Uani 1 1 d . . . . .
C6 C 0.7948(8) 0.7202(3) 0.2982(4) 0.0257(9) Uani 1 1 d . . . . .
H6A H 0.6418 0.7268 0.3315 0.039 Uiso 1 1 calc R U . . .
H6B H 0.8953 0.7696 0.3126 0.039 Uiso 1 1 calc R U . . .
H6C H 0.8961 0.6756 0.3427 0.039 Uiso 1 1 calc R U . . .
C7 C 1.0169(8) 0.6913(3) 0.1012(4) 0.0256(9) Uani 1 1 d . . . . .
H7A H 1.1065 0.6463 0.1506 0.038 Uiso 1 1 calc R U . . .
H7B H 1.1105 0.7411 0.1276 0.038 Uiso 1 1 calc R U . . .
H7C H 1.0046 0.6821 0.0097 0.038 Uiso 1 1 calc R 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
Ca1 O1 2.293(3) . ?
Ca1 O1 2.293(3) 3_665 ?
Ca1 O3 2.336(3) 3_565 ?
Ca1 O3 2.336(3) 1_655 ?
Ca1 O4 2.307(3) 3_665 ?
Ca1 O4 2.307(3) . ?
S1 O1 1.453(3) . ?
S1 O2 1.443(3) . ?
S1 O3 1.462(3) . ?
S1 C1 1.779(4) . ?
S2 O4 1.511(3) . ?
S2 C6 1.792(4) . ?
S2 C7 1.785(4) . ?
O3 Ca1 2.336(3) 1_455 ?
C1 C2 1.369(5) . ?
C1 C5 1.430(5) 3_566 ?
C2 H2 0.9500 . ?
C2 C3 1.415(5) . ?
C3 H3 0.9500 . ?
C3 C4 1.364(5) . ?
C4 H4 0.9500 . ?
C4 C5 1.421(5) . ?
C5 C1 1.430(5) 3_566 ?
C5 C5 1.441(7) 3_566 ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?

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
O1 Ca1 O1 180.0 . 3_665 ?
O1 Ca1 O3 93.46(9) . 3_565 ?
O1 Ca1 O3 86.54(9) 3_665 3_565 ?
O1 Ca1 O3 86.54(9) . 1_655 ?
O1 Ca1 O3 93.46(9) 3_665 1_655 ?
O1 Ca1 O4 93.34(10) . 3_665 ?
O1 Ca1 O4 86.66(10) . . ?
O1 Ca1 O4 86.65(10) 3_665 3_665 ?
O1 Ca1 O4 93.35(10) 3_665 . ?
O3 Ca1 O3 180.0 1_655 3_565 ?
O4 Ca1 O3 90.50(9) . 3_565 ?
O4 Ca1 O3 90.50(9) 3_665 1_655 ?
O4 Ca1 O3 89.50(9) . 1_655 ?
O4 Ca1 O3 89.50(9) 3_665 3_565 ?
O4 Ca1 O4 180.00(16) 3_665 . ?
O1 S1 O3 111.36(15) . . ?
O1 S1 C1 105.16(17) . . ?
O2 S1 O1 113.56(17) . . ?
O2 S1 O3 112.27(16) . . ?
O2 S1 C1 106.97(16) . . ?
O3 S1 C1 106.94(16) . . ?
O4 S2 C6 104.80(18) . . ?
O4 S2 C7 105.88(19) . . ?
C7 S2 C6 98.1(2) . . ?
S1 O1 Ca1 165.95(19) . . ?
S1 O3 Ca1 143.53(16) . 1_455 ?
S2 O4 Ca1 147.77(17) . . ?
C2 C1 S1 117.6(3) . . ?
C2 C1 C5 121.4(3) . 3_566 ?
C5 C1 S1 120.9(3) 3_566 . ?
C1 C2 H2 120.0 . . ?
C1 C2 C3 120.0(3) . . ?
C3 C2 H2 120.0 . . ?
C2 C3 H3 119.6 . . ?
C4 C3 C2 120.8(3) . . ?
C4 C3 H3 119.6 . . ?
C3 C4 H4 119.5 . . ?
C3 C4 C5 121.0(3) . . ?
C5 C4 H4 119.5 . . ?
C1 C5 C5 117.9(4) 3_566 3_566 ?
C4 C5 C1 123.2(3) . 3_566 ?
C4 C5 C5 118.9(4) . 3_566 ?
S2 C6 H6A 109.5 . . ?
S2 C6 H6B 109.5 . . ?
S2 C6 H6C 109.5 . . ?
H6A C6 H6B 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
S2 C7 H7A 109.5 . . ?
S2 C7 H7B 109.5 . . ?
S2 C7 H7C 109.5 . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
S1 C1 C2 C3 -175.7(3) . . . . ?
O1 S1 O3 Ca1 -27.3(3) . . . 1_455 ?
O1 S1 C1 C2 -10.8(3) . . . . ?
O1 S1 C1 C5 173.1(3) . . . 3_566 ?
O2 S1 O1 Ca1 20.3(7) . . . . ?
O2 S1 O3 Ca1 -155.9(2) . . . 1_455 ?
O2 S1 C1 C2 110.3(3) . . . . ?
O2 S1 C1 C5 -65.9(3) . . . 3_566 ?
O3 S1 O1 Ca1 -107.7(7) . . . . ?
O3 S1 C1 C2 -129.3(3) . . . . ?
O3 S1 C1 C5 54.6(3) . . . 3_566 ?
C1 S1 O1 Ca1 136.9(7) . . . . ?
C1 S1 O3 Ca1 87.0(3) . . . 1_455 ?
C1 C2 C3 C4 -0.6(5) . . . . ?
C2 C3 C4 C5 0.5(6) . . . . ?
C3 C4 C5 C1 179.9(3) . . . 3_566 ?
C3 C4 C5 C5 -0.3(6) . . . 3_566 ?
C5 C1 C2 C3 0.4(5) 3_566 . . . ?
C6 S2 O4 Ca1 -160.4(3) . . . . ?
C7 S2 O4 Ca1 -57.3(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
;
####################################################################### 
# 
# 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_ca-adsmay_twin1_hklf4
_database_code_depnum_ccdc_archive 'CCDC 2336804'
loop_
_audit_author_name
_audit_author_address
'Christopher Pask'
;University of Leeds
United Kingdom
;
_audit_update_record             
;
2024-05-24 deposited with the CCDC.	2024-06-18 downloaded from the CCDC.
;
_audit_creation_date             2024-05-23
_audit_creation_method           
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C14 H12 Ca O11 S2'
_chemical_formula_sum            'C14 H12 Ca O11 S2'
_chemical_formula_weight         460.44
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C56  H48  Ca4  O44  S8  '
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 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'
Ca Ca 0.3641 1.2855 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 '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           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   20.1769(8)
_cell_length_b                   7.6697(3)
_cell_length_c                   10.7097(5)
_cell_angle_alpha                90
_cell_angle_beta                 104.898(4)
_cell_angle_gamma                90
_cell_volume                     1601.62(12)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    4494
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      72.3010
_cell_measurement_theta_min      4.5380
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    6.456
_exptl_absorpt_correction_T_max  0.806
_exptl_absorpt_correction_T_min  0.481
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.81a (Rigaku Oxford Diffraction, 2023)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.909
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             944
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-4 0 7 0.0231
4 0 -7 0.0231
2 -5 0 0.0933
-2 5 0 0.0933
13 0 0 0.0271
-12 0 -1 0.0088

_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.04
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-4.2817 -0.0286 6.9372 -0.0155 -0.4277 -0.9038
4.2817 0.0286 -6.9372 0.0155 0.4277 0.9038
1.7047 -4.9323 -0.0390 -0.9818 0.1810 -0.0580
-1.7047 4.9323 0.0390 0.9818 -0.1810 0.0580
12.6303 -0.1674 0.0359 0.0235 0.9305 -0.3655
-12.2789 0.3757 -0.6042 0.0191 -0.8977 0.4401

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  ?
_diffrn_reflns_av_unetI/netI     0.0132
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            2341
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.565
_diffrn_reflns_theta_min         4.535
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3095
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     14.00 100.00   1.00    5.74    --   41.04  65.00  48.99   86
  2  ω     14.00  93.00   1.00    5.74    --   41.04  63.00   1.70   79
  3  ω     11.00  60.00   1.00    5.74    --   41.04 -57.00 120.00   49
  4  ω     12.00 101.00   1.00    5.74    --   41.04  64.00 -71.73   89
  5  ω     12.00  72.00   1.00    5.74    --   41.04  65.00 168.96   60
  6  ω     20.00  97.00   1.00    5.74    --   41.04  65.00-152.38   77
  7  ω     15.00  53.00   1.00    5.74    --   41.04  65.00 136.40   38
  8  ω     31.00 113.00   1.00   22.96    --  104.14 -65.00  57.12   82
  9  ω     67.00  94.00   1.00   22.96    --  104.14 -65.00  87.24   27
 10  ω     31.00 101.00   1.00   22.96    --  104.14 -65.00  17.23   70
 11  ω     85.00 134.00   1.00   22.96    --  104.14  45.00 120.00   49
 12  ω    151.00 177.00   1.00   22.96    --  104.14  45.00 120.00   26
 13  ω     87.00 114.00   1.00   22.96    --  104.14  61.00 150.00   27
 14  ω    136.00 176.00   1.00   22.96    --  104.14  61.00 150.00   40
 15  ω     83.00 110.00   1.00   22.96    --  104.14 -65.00-147.89   27
 16  ω     90.00 118.00   1.00   22.96    --  104.14  45.00-120.00   28
 17  ω     69.00 114.00   1.00   22.96    --  104.14 -65.00 -77.60   45
 18  ω     47.00 114.00   1.00   22.96    --  104.14 -65.00-125.31   67
 19  ω     77.00 178.00   1.00   22.96    --  104.14  30.00-150.00  101
 20  ω    144.00 170.00   1.00   22.96    --  104.14  45.00-120.00   26
 21  ω     54.00 106.00   1.00   22.96    --  104.14 -65.00 166.05   52
 22  ω     51.00 148.00   1.00   22.96    --  104.14  15.00 -30.00   97
 23  ω     76.00 101.00   1.00   22.96    --  104.14 -65.00  31.60   25
 24  ω     33.00  62.00   1.00   22.96    --  104.14 -65.00 -77.60   29
 25  ω     66.00  95.00   1.00   22.96    --  104.14 -65.00-169.38   29
 26  ω     67.00 106.00   1.00   22.96    --  104.14 -65.00 112.95   39
 27  ω     73.00 100.00   1.00   22.96    --  104.14 -65.00 -26.94   27
 28  ω     70.00  97.00   1.00   22.96    --  104.14 -65.00  64.55   27
 29  ω     50.00  77.00   1.00   22.96    --  104.14 -65.00 -46.58   27
 30  ω     68.00  95.00   1.00   22.96    --  104.14 -65.00  -7.71   27
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0045130000
_diffrn_orient_matrix_UB_12      0.2005984000
_diffrn_orient_matrix_UB_13      0.0013766000
_diffrn_orient_matrix_UB_21      0.0735735000
_diffrn_orient_matrix_UB_22      -0.0111366000
_diffrn_orient_matrix_UB_23      -0.0162930000
_diffrn_orient_matrix_UB_31      -0.0284746000
_diffrn_orient_matrix_UB_32      0.0030776000
_diffrn_orient_matrix_UB_33      -0.1478418000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2107
_reflns_number_total             2341
_reflns_special_details          
;
 _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 1.171.42.81a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.81a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.81a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_refine_diff_density_max         0.381
_refine_diff_density_min         -0.458
_refine_diff_density_rms         0.071
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     141
_refine_ls_number_reflns         2341
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0309
_refine_ls_R_factor_gt           0.0283
_refine_ls_restrained_S_all      1.058
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0584P)²+0.2098P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0761
_refine_ls_wR_factor_ref         0.0770
_refine_special_details          
;
 Refined as a 2-component twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.7438(9)
 0.2562(9)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
3.a Aromatic/amide H refined with riding coordinates:
 C00D(H00D), C00E(H00E), C00F(H00F)
;
_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
Ca01 Ca 0.5000 0.68938(7) 0.2500 0.00794(15) Uani 1 2 d S T P . .
S002 S 0.60813(2) 0.39438(6) 0.27263(4) 0.00717(15) Uani 1 1 d . . . . .
O003 O 0.56796(7) 0.42325(19) 0.36668(14) 0.0112(3) Uani 1 1 d . . . . .
O004 O 0.49393(9) 0.7721(2) 0.46640(18) 0.0182(3) Uani 1 1 d . . . . .
O005 O 0.61870(7) 0.75909(19) 0.36647(14) 0.0128(3) Uani 1 1 d . . . . .
O006 O 0.58772(9) 0.51547(18) 0.16506(17) 0.0114(3) Uani 1 1 d . . . . .
O007 O 0.60815(8) 0.21363(18) 0.23121(15) 0.0139(3) Uani 1 1 d . . . . .
O008 O 0.5000 0.9978(2) 0.2500 0.0159(5) Uani 1 2 d S T P . .
C009 C 0.72111(10) 0.5925(3) 0.42284(19) 0.0079(4) Uani 1 1 d . . . . .
C00A C 0.79131(10) 0.6026(2) 0.48515(19) 0.0085(4) Uani 1 1 d . . . . .
C00B C 0.69647(10) 0.4399(3) 0.35159(18) 0.0084(4) Uani 1 1 d . . . . .
C00C C 0.67770(10) 0.7470(3) 0.43029(18) 0.0087(4) Uani 1 1 d . . . . .
C00D C 0.83660(11) 0.4698(3) 0.4725(2) 0.0099(4) Uani 1 1 d . . . . .
H00D H 0.8840 0.4790 0.5151 0.012 Uiso 1 1 calc R U . . .
C00E C 0.74269(11) 0.3091(2) 0.33996(19) 0.0096(4) Uani 1 1 d . . . . .
H00E H 0.7261 0.2071 0.2916 0.012 Uiso 1 1 calc R U . . .
C00F C 0.81233(10) 0.3251(3) 0.3977(2) 0.0110(4) Uani 1 1 d . . . . .
H00F H 0.8432 0.2370 0.3858 0.013 Uiso 1 1 calc R U . . .
H008 H 0.4664(16) 1.063(4) 0.257(3) 0.022(7) Uiso 1 1 d . . . . .
H00A H 0.475(2) 0.706(5) 0.502(4) 0.051(12) Uiso 1 1 d . . . . .
H00B H 0.531(2) 0.805(5) 0.514(4) 0.052(12) 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
Ca01 O003 2.5936(15) . ?
Ca01 O003 2.5936(15) 2_655 ?
Ca01 O004 2.4362(17) . ?
Ca01 O004 2.4362(17) 2_655 ?
Ca01 O005 2.4579(14) 2_655 ?
Ca01 O005 2.4579(14) . ?
Ca01 O006 2.5626(17) . ?
Ca01 O006 2.5626(17) 2_655 ?
Ca01 O008 2.3655(19) . ?
S002 O003 1.4630(14) . ?
S002 O006 1.4544(16) . ?
S002 O007 1.4556(15) . ?
S002 C00B 1.800(2) . ?
O004 H00A 0.79(5) . ?
O004 H00B 0.83(5) . ?
O005 C00C 1.214(3) . ?
O008 H008 0.86(3) . ?
C009 C00A 1.404(3) . ?
C009 C00B 1.416(3) . ?
C009 C00C 1.488(3) . ?
C00A C00C 1.500(3) 7_666 ?
C00A C00D 1.398(3) . ?
C00B C00E 1.397(3) . ?
C00C C00A 1.500(3) 7_666 ?
C00D H00D 0.9500 . ?
C00D C00F 1.383(3) . ?
C00E H00E 0.9500 . ?
C00E C00F 1.387(3) . ?
C00F H00F 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
O003 Ca01 O003 76.19(6) . 2_655 ?
O004 Ca01 O003 120.91(5) . 2_655 ?
O004 Ca01 O003 84.05(5) 2_655 2_655 ?
O004 Ca01 O003 120.91(5) 2_655 . ?
O004 Ca01 O003 84.05(5) . . ?
O004 Ca01 O004 149.81(9) . 2_655 ?
O004 Ca01 O005 98.36(6) 2_655 . ?
O004 Ca01 O005 75.01(6) 2_655 2_655 ?
O004 Ca01 O005 98.36(6) . 2_655 ?
O004 Ca01 O005 75.01(6) . . ?
O004 Ca01 O006 132.96(6) 2_655 2_655 ?
O004 Ca01 O006 132.96(6) . . ?
O004 Ca01 O006 65.77(6) 2_655 . ?
O004 Ca01 O006 65.77(6) . 2_655 ?
O005 Ca01 O003 137.83(5) . 2_655 ?
O005 Ca01 O003 66.50(5) 2_655 2_655 ?
O005 Ca01 O003 137.83(5) 2_655 . ?
O005 Ca01 O003 66.50(5) . . ?
O005 Ca01 O005 154.87(7) 2_655 . ?
O005 Ca01 O006 67.77(5) 2_655 2_655 ?
O005 Ca01 O006 127.22(5) 2_655 . ?
O005 Ca01 O006 127.22(5) . 2_655 ?
O005 Ca01 O006 67.77(5) . . ?
O006 Ca01 O003 75.36(5) 2_655 . ?
O006 Ca01 O003 55.50(5) . . ?
O006 Ca01 O003 75.36(5) . 2_655 ?
O006 Ca01 O003 55.50(5) 2_655 2_655 ?
O006 Ca01 O006 117.27(7) . 2_655 ?
O008 Ca01 O003 141.90(3) . 2_655 ?
O008 Ca01 O003 141.90(3) . . ?
O008 Ca01 O004 74.90(4) . 2_655 ?
O008 Ca01 O004 74.90(4) . . ?
O008 Ca01 O005 77.44(4) . 2_655 ?
O008 Ca01 O005 77.44(4) . . ?
O008 Ca01 O006 121.37(3) . 2_655 ?
O008 Ca01 O006 121.37(3) . . ?
O003 S002 C00B 107.71(9) . . ?
O006 S002 O003 110.76(9) . . ?
O006 S002 O007 112.89(9) . . ?
O006 S002 C00B 107.04(9) . . ?
O007 S002 O003 113.43(9) . . ?
O007 S002 C00B 104.49(9) . . ?
S002 O003 Ca01 96.04(7) . . ?
Ca01 O004 H00A 116(3) . . ?
Ca01 O004 H00B 114(3) . . ?
H00A O004 H00B 112(4) . . ?
C00C O005 Ca01 162.82(14) . . ?
S002 O006 Ca01 97.59(9) . . ?
Ca01 O008 H008 126(2) . . ?
C00A C009 C00B 118.25(18) . . ?
C00A C009 C00C 117.80(17) . . ?
C00B C009 C00C 123.87(18) . . ?
C009 C00A C00C 122.83(18) . 7_666 ?
C00D C00A C009 121.22(18) . . ?
C00D C00A C00C 115.94(18) . 7_666 ?
C009 C00B S002 125.58(15) . . ?
C00E C00B S002 114.96(15) . . ?
C00E C00B C009 119.46(18) . . ?
O005 C00C C009 122.41(18) . . ?
O005 C00C C00A 118.50(18) . 7_666 ?
C009 C00C C00A 119.02(17) . 7_666 ?
C00A C00D H00D 120.1 . . ?
C00F C00D C00A 119.87(19) . . ?
C00F C00D H00D 120.1 . . ?
C00B C00E H00E 119.4 . . ?
C00F C00E C00B 121.30(18) . . ?
C00F C00E H00E 119.4 . . ?
C00D C00F C00E 119.77(18) . . ?
C00D C00F H00F 120.1 . . ?
C00E C00F H00F 120.1 . . ?

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
Ca01 O005 C00C C009 35.8(6) . . . . ?
Ca01 O005 C00C C00A -147.2(4) . . . 7_666 ?
S002 C00B C00E C00F -178.96(16) . . . . ?
O003 S002 O006 Ca01 3.22(9) . . . . ?
O003 S002 C00B C009 -50.46(19) . . . . ?
O003 S002 C00B C00E 128.91(15) . . . . ?
O006 S002 O003 Ca01 -3.17(9) . . . . ?
O006 S002 C00B C009 68.68(19) . . . . ?
O006 S002 C00B C00E -111.95(16) . . . . ?
O007 S002 O003 Ca01 -131.31(8) . . . . ?
O007 S002 O006 Ca01 131.65(8) . . . . ?
O007 S002 C00B C009 -171.36(17) . . . . ?
O007 S002 C00B C00E 8.01(17) . . . . ?
C009 C00A C00D C00F -0.2(3) . . . . ?
C009 C00B C00E C00F 0.4(3) . . . . ?
C00A C009 C00B S002 176.13(14) . . . . ?
C00A C009 C00B C00E -3.2(3) . . . . ?
C00A C009 C00C O005 170.49(19) . . . . ?
C00A C009 C00C C00A -6.6(3) . . . 7_666 ?
C00A C00D C00F C00E -2.7(3) . . . . ?
C00B S002 O003 Ca01 113.57(8) . . . . ?
C00B S002 O006 Ca01 -113.93(8) . . . . ?
C00B C009 C00A C00C -176.21(17) . . . 7_666 ?
C00B C009 C00A C00D 3.1(3) . . . . ?
C00B C009 C00C O005 -6.3(3) . . . . ?
C00B C009 C00C C00A 176.67(17) . . . 7_666 ?
C00B C00E C00F C00D 2.5(3) . . . . ?
C00C C009 C00A C00C 6.8(3) . . . 7_666 ?
C00C C009 C00A C00D -173.86(18) . . . . ?
C00C C009 C00B S002 -7.1(3) . . . . ?
C00C C009 C00B C00E 173.56(17) . . . . ?
C00C C00A C00D C00F 179.19(18) 7_666 . . . ?

_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 1.504
_oxdiff_exptl_absorpt_empirical_full_min 0.647
_oxdiff_twin_integration_method  simultaneous
_oxdiff_twin_items               2
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
_oxdiff_twin_reflns_isolated
_oxdiff_twin_reflns_overlapped
_twin_individual_twin_lattice_type
_twin_individual_twin_matrix_11
_twin_individual_twin_matrix_12
_twin_individual_twin_matrix_13
_twin_individual_twin_matrix_21
_twin_individual_twin_matrix_22
_twin_individual_twin_matrix_23
_twin_individual_twin_matrix_31
_twin_individual_twin_matrix_32
_twin_individual_twin_matrix_33
1 0.7438(9) 3089 3614 ref 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000
0.0000 1.0000
2 0.2562(9) 3094 3614 nmt -1.0003 0.0011 -0.9679 -0.0004 -0.9994 0.0002 -0.0001
0.0009 0.9991

_twin_special_details            
;
Component 2 rotated by -179.9481° 
around [-0.43 0.00 0.90] (reciprocal) or [-0.00 0.00 1.00] (direct)
;
####################################################################### 
# 
# 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_cu-satetoh1
_database_code_depnum_ccdc_archive 'CCDC 2336805'
loop_
_audit_author_name
_audit_author_address
'Christopher Pask'
;University of Leeds
United Kingdom
;
_audit_update_record             
;
2024-03-01 deposited with the CCDC.	2024-06-18 downloaded from the CCDC.
;
_audit_creation_date             2024-03-01
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C4 H10 Cu2 N8 O2, C10 H6 O6 S2'
_chemical_formula_sum            'C14 H16 Cu2 N8 O8 S2'
_chemical_formula_weight         615.55
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C28  H32  Cu4  N16  O16  S4  '
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 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 -1.9646 0.5888 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 '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           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   6.7128(5)
_cell_length_b                   10.0239(7)
_cell_length_c                   14.5560(10)
_cell_angle_alpha                90
_cell_angle_beta                 93.268(6)
_cell_angle_gamma                90
_cell_volume                     977.86(12)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    1517
_cell_measurement_temperature    99.99(10)
_cell_measurement_theta_max      72.2050
_cell_measurement_theta_min      5.3200
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    5.311
_exptl_absorpt_correction_T_max  0.898
_exptl_absorpt_correction_T_min  0.784
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.81a (Rigaku Oxford Diffraction, 2023)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    2.091
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             620
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-4 0 0 0.0162
4 0 0 0.0162
0 6 2 0.0325
0 -6 -2 0.0171
-4 2 4 0.0402
4 -2 -4 0.0043
1 -1 9 0.0417
-2 1 -8 0.0103

_exptl_crystal_size_max          0.07
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-4.3302 -0.1004 -0.3902 0.2486 -0.3420 0.9062
4.3315 -0.2370 0.3081 -0.2057 0.3724 -0.9050
-0.3665 6.4029 1.5292 -0.7948 -0.6049 0.0477
-0.0773 -6.4140 -1.5694 0.8204 0.5700 0.0451
-3.7076 2.1746 4.2695 -0.3666 -0.2139 0.9055
3.7730 -2.2164 -3.9069 0.3419 0.2485 -0.9063
0.7369 -0.5119 9.1857 -0.6407 0.7494 0.1671
-1.7654 1.1173 -8.2590 0.5574 -0.8269 0.0752

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0427
_diffrn_reflns_av_unetI/netI     0.0549
_diffrn_reflns_Laue_measured_fraction_full 0.972
_diffrn_reflns_Laue_measured_fraction_max 0.942
_diffrn_reflns_limit_h_max       4
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            3711
_diffrn_reflns_point_group_measured_fraction_full 0.972
_diffrn_reflns_point_group_measured_fraction_max 0.942
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.476
_diffrn_reflns_theta_min         5.361
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.99(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3095
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.972
_diffrn_measured_fraction_theta_max 0.942
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -113.00 -79.00   1.00    2.58    --  -40.54 -57.00-120.00   34
  2  ω    -69.00  26.00   1.00    2.58    --  -40.54  57.00 -60.00   95
  3  ω    -55.00  14.00   1.00    2.58    --  -40.54  37.00-150.00   69
  4  ω     43.00  68.00   1.00    2.58    --   40.54 -62.00  97.26   25
  5  ω     40.00  80.00   1.00   10.30    --  104.14 -65.00 144.42   40
  6  ω    141.00 177.00   1.00   10.30    --  104.14  45.00 -90.00   36
  7  ω     40.00  97.00   1.00   10.30    --  104.14 -65.00 107.45   57
  8  ω     67.00 126.00   1.00   10.30    --  104.14 -45.00 -90.00   59
  9  ω     76.00 172.00   1.00   10.30    --  104.14  30.00  90.00   96
 10  ω     34.00  60.00   1.00   10.30    --  104.14 -45.00 -90.00   26
 11  ω     35.00  97.00   1.00   10.30    --  104.14 -65.00-143.54   62
 12  ω     38.00  99.00   1.00   10.30    --  104.14 -65.00 157.65   61
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0483790000
_diffrn_orient_matrix_UB_12      -0.1097144000
_diffrn_orient_matrix_UB_13      -0.0719862000
_diffrn_orient_matrix_UB_21      0.0751849000
_diffrn_orient_matrix_UB_22      -0.1067989000
_diffrn_orient_matrix_UB_23      0.0695971000
_diffrn_orient_matrix_UB_31      -0.2120877000
_diffrn_orient_matrix_UB_32      -0.0129206000
_diffrn_orient_matrix_UB_33      0.0344842000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1519
_reflns_number_total             1822
_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 1.171.42.81a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.81a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.81a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_refine_diff_density_max         0.838
_refine_diff_density_min         -0.471
_refine_diff_density_rms         0.124
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.114
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     162
_refine_ls_number_reflns         1822
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0560
_refine_ls_R_factor_gt           0.0461
_refine_ls_restrained_S_all      1.114
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0565P)²+0.7848P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1149
_refine_ls_wR_factor_ref         0.1212
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H) groups
2. Restrained distances
 O1-H1
 0.9 with sigma of 0.02
3.a Rotating group:
 N4(H4A,H4B)
3.b Aromatic/amide H refined with riding coordinates:
 C1(H1A), C2(H2), C4(H4), C5(H5), C6(H6)
;
_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
Cu1 Cu 0.0000 0.0000 0.5000 0.0132(2) Uani 1 2 d S . P . .
Cu2 Cu 0.5000 0.0000 0.5000 0.0122(2) Uani 1 2 d S . P . .
O1 O 0.2395(4) 0.0305(3) 0.43599(19) 0.0139(6) Uani 1 1 d D . . . .
N1 N 0.6355(5) 0.1282(3) 0.4185(2) 0.0137(7) Uani 1 1 d . . . . .
N2 N 0.8340(5) 0.1099(3) 0.4043(2) 0.0141(7) Uani 1 1 d . . . . .
N3 N 0.7201(5) 0.2712(3) 0.3165(2) 0.0154(7) Uani 1 1 d . . . . .
N4 N 0.7193(5) 0.3778(3) 0.2536(2) 0.0176(7) Uani 1 1 d . . . . .
H4A H 0.6164 0.3706 0.2127 0.021 Uiso 1 1 d R U . . .
H4B H 0.7097 0.4549 0.2830 0.021 Uiso 1 1 d R U . . .
C1 C 0.8813(6) 0.1955(4) 0.3410(3) 0.0130(8) Uani 1 1 d . . . . .
H1A H 1.0087 0.2032 0.3163 0.016 Uiso 1 1 calc R U . . .
C2 C 0.5690(6) 0.2252(4) 0.3657(3) 0.0147(8) Uani 1 1 d . . . . .
H2 H 0.4362 0.2583 0.3622 0.018 Uiso 1 1 calc R U . . .
S1 S 0.24580(14) 0.26106(9) 0.61797(6) 0.0134(2) Uani 1 1 d . . . . .
O2 O 0.4079(4) 0.1635(3) 0.61572(19) 0.0149(6) Uani 1 1 d . . . . .
O3 O 0.2504(4) 0.3326(3) 0.7054(2) 0.0186(6) Uani 1 1 d . . . . .
O4 O 0.0518(4) 0.2061(3) 0.5907(2) 0.0177(6) Uani 1 1 d . . . . .
C3 C 0.5159(6) 0.5466(4) 0.4633(3) 0.0137(8) Uani 1 1 d . . . . .
C4 C 0.3671(6) 0.5629(4) 0.3914(3) 0.0167(8) Uani 1 1 d . . . . .
H4 H 0.3885 0.6240 0.3431 0.020 Uiso 1 1 calc R U . . .
C5 C 0.1921(6) 0.4918(4) 0.3906(3) 0.0162(8) Uani 1 1 d . . . . .
H5 H 0.0944 0.5029 0.3413 0.019 Uiso 1 1 calc R U . . .
C6 C 0.1574(6) 0.4022(4) 0.4628(3) 0.0150(8) Uani 1 1 d . . . . .
H6 H 0.0342 0.3555 0.4629 0.018 Uiso 1 1 calc R U . . .
C7 C 0.2992(6) 0.3819(4) 0.5327(3) 0.0148(8) Uani 1 1 d . . . . .
H1 H 0.224(8) -0.020(5) 0.387(2) 0.022(14) Uiso 1 1 d 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
Cu1 O1 1.928(3) 3_556 ?
Cu1 O1 1.928(3) . ?
Cu1 N2 2.054(3) 3_656 ?
Cu1 N2 2.054(3) 1_455 ?
Cu2 O1 1.958(3) . ?
Cu2 O1 1.958(3) 3_656 ?
Cu2 N1 2.002(3) . ?
Cu2 N1 2.002(3) 3_656 ?
O1 H1 0.87(2) . ?
N1 N2 1.372(5) . ?
N1 C2 1.303(5) . ?
N2 Cu1 2.054(3) 1_655 ?
N2 C1 1.311(5) . ?
N3 N4 1.407(5) . ?
N3 C1 1.352(5) . ?
N3 C2 1.355(5) . ?
N4 H4A 0.8883 . ?
N4 H4B 0.8881 . ?
C1 H1A 0.9500 . ?
C2 H2 0.9500 . ?
S1 O2 1.465(3) . ?
S1 O3 1.459(3) . ?
S1 O4 1.448(3) . ?
S1 C7 1.785(4) . ?
C3 C3 1.444(8) 3_666 ?
C3 C4 1.414(6) . ?
C3 C7 1.432(6) 3_666 ?
C4 H4 0.9500 . ?
C4 C5 1.373(6) . ?
C5 H5 0.9500 . ?
C5 C6 1.413(6) . ?
C6 H6 0.9500 . ?
C6 C7 1.368(6) . ?
C7 C3 1.432(6) 3_666 ?

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
O1 Cu1 O1 180.0 3_556 . ?
O1 Cu1 N2 91.27(13) . 1_455 ?
O1 Cu1 N2 88.73(13) 3_556 1_455 ?
O1 Cu1 N2 91.27(13) 3_556 3_656 ?
O1 Cu1 N2 88.73(13) . 3_656 ?
N2 Cu1 N2 180.00(14) 3_656 1_455 ?
O1 Cu2 O1 180.00(15) . 3_656 ?
O1 Cu2 N1 87.63(13) . 3_656 ?
O1 Cu2 N1 92.37(13) 3_656 3_656 ?
O1 Cu2 N1 92.37(13) . . ?
O1 Cu2 N1 87.63(13) 3_656 . ?
N1 Cu2 N1 180.0 . 3_656 ?
Cu1 O1 Cu2 119.47(14) . . ?
Cu1 O1 H1 104(4) . . ?
Cu2 O1 H1 111(4) . . ?
N2 N1 Cu2 118.8(2) . . ?
C2 N1 Cu2 132.6(3) . . ?
C2 N1 N2 108.3(3) . . ?
N1 N2 Cu1 117.6(2) . 1_655 ?
C1 N2 Cu1 133.2(3) . 1_655 ?
C1 N2 N1 107.1(3) . . ?
C1 N3 N4 124.8(3) . . ?
C1 N3 C2 106.3(3) . . ?
C2 N3 N4 128.8(3) . . ?
N3 N4 H4A 110.4 . . ?
N3 N4 H4B 110.2 . . ?
H4A N4 H4B 108.6 . . ?
N2 C1 N3 109.3(3) . . ?
N2 C1 H1A 125.3 . . ?
N3 C1 H1A 125.3 . . ?
N1 C2 N3 108.9(4) . . ?
N1 C2 H2 125.5 . . ?
N3 C2 H2 125.5 . . ?
O2 S1 C7 104.98(17) . . ?
O3 S1 O2 111.66(17) . . ?
O3 S1 C7 106.12(18) . . ?
O4 S1 O2 113.41(17) . . ?
O4 S1 O3 113.56(18) . . ?
O4 S1 C7 106.29(19) . . ?
C4 C3 C3 119.7(5) . 3_666 ?
C4 C3 C7 123.1(4) . 3_666 ?
C7 C3 C3 117.2(5) 3_666 3_666 ?
C3 C4 H4 119.5 . . ?
C5 C4 C3 121.0(4) . . ?
C5 C4 H4 119.5 . . ?
C4 C5 H5 120.0 . . ?
C4 C5 C6 120.0(4) . . ?
C6 C5 H5 120.0 . . ?
C5 C6 H6 119.6 . . ?
C7 C6 C5 120.7(4) . . ?
C7 C6 H6 119.6 . . ?
C3 C7 S1 121.3(3) 3_666 . ?
C6 C7 S1 117.3(3) . . ?
C6 C7 C3 121.4(4) . 3_666 ?

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 N2 C1 N3 -160.4(3) 1_655 . . . ?
Cu2 N1 N2 Cu1 -21.7(4) . . . 1_655 ?
Cu2 N1 N2 C1 172.8(2) . . . . ?
Cu2 N1 C2 N3 -172.8(3) . . . . ?
N1 N2 C1 N3 2.0(4) . . . . ?
N2 N1 C2 N3 0.2(4) . . . . ?
N4 N3 C1 N2 176.7(3) . . . . ?
N4 N3 C2 N1 -177.5(4) . . . . ?
C1 N3 C2 N1 1.0(4) . . . . ?
C2 N1 N2 Cu1 164.2(3) . . . 1_655 ?
C2 N1 N2 C1 -1.3(4) . . . . ?
C2 N3 C1 N2 -1.9(4) . . . . ?
O2 S1 C7 C3 -57.6(4) . . . 3_666 ?
O2 S1 C7 C6 121.7(3) . . . . ?
O3 S1 C7 C3 60.7(4) . . . 3_666 ?
O3 S1 C7 C6 -120.0(3) . . . . ?
O4 S1 C7 C3 -178.1(3) . . . 3_666 ?
O4 S1 C7 C6 1.2(4) . . . . ?
C3 C3 C4 C5 0.3(7) 3_666 . . . ?
C3 C4 C5 C6 0.9(6) . . . . ?
C4 C5 C6 C7 -2.1(6) . . . . ?
C5 C6 C7 S1 -177.2(3) . . . . ?
C5 C6 C7 C3 2.1(6) . . . 3_666 ?
C7 C3 C4 C5 179.9(4) 3_666 . . . ?

_olex2_date_sample_data_collection 2023-02-13
_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 1.406
_oxdiff_exptl_absorpt_empirical_full_min 0.675
####################################################################### 
# 
# 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_cu-sqat1
_database_code_depnum_ccdc_archive 'CCDC 2336803'
loop_
_audit_author_name
_audit_author_address
'Christopher Pask'
;University of Leeds
United Kingdom
;
_audit_update_record             
;
2024-03-01 deposited with the CCDC.	2024-06-18 downloaded from the CCDC.
;
_audit_creation_date             2024-03-01
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C4 H10 Cu2 N8 O2, C14 H6 O8 S2'
_chemical_formula_sum            'C18 H16 Cu2 N8 O10 S2'
_chemical_formula_weight         695.59
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C36  H32  Cu4  N16  O20  S4  '
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 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 -1.9646 0.5888 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 '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           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   13.7271(3)
_cell_length_b                   6.7154(2)
_cell_length_c                   12.1309(3)
_cell_angle_alpha                90
_cell_angle_beta                 91.407(2)
_cell_angle_gamma                90
_cell_volume                     1117.93(5)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    2347
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      72.4310
_cell_measurement_theta_min      3.1710
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    4.818
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.748
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.81a (Rigaku Oxford Diffraction, 2023)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    2.066
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             700
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
2 -4 0 0.0466
-2 4 0 0.0115
0 0 8 0.0558
0 0 -8 0.0260
-8 -1 -1 0.0092
8 1 1 0.0092

_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.02
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
2.1695 -4.2302 0.0012 -0.5006 0.3381 0.7969
-2.1692 4.2288 0.2567 0.4977 -0.3085 -0.8106
0.1629 -0.3421 7.8419 -0.1237 0.9246 -0.3603
-0.0123 0.0487 -7.8706 0.0893 -0.9044 0.4172
-8.4902 -1.0537 -1.2402 -0.8346 -0.4362 -0.3365
8.4902 1.0537 1.2402 0.8346 0.4362 0.3365

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0326
_diffrn_reflns_av_unetI/netI     0.0404
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.972
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       2
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            4603
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.972
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.522
_diffrn_reflns_theta_min         3.220
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3095
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -63.00 -35.00   1.00    2.95    --  -41.04  64.00  48.00   28
  2  ω   -110.00 -19.00   1.00    2.95    --  -41.04 -64.00 -88.00   91
  3  ω     39.00 122.00   1.00   11.81    --  104.14 -64.00 -88.00   83
  4  ω     77.00 177.00   1.00   11.81    --  104.14  64.00  48.00  100
  5  ω     -6.00  28.00   1.00    2.95    --  -41.04  37.00-150.00   34
  6  ω    -61.00  -8.00   1.00    2.95    --  -41.04  37.00-150.00   53
  7  ω    -32.00  29.00   1.00    2.95    --  -41.04  64.00  48.00   61
  8  ω     79.00 125.00   1.00   11.81    --  104.14  45.00 -30.00   46
  9  ω     34.00  66.00   1.00   11.81    --  104.14 -61.00 150.00   32
 10  ω     95.00 164.00   1.00   11.81    --  104.14  45.00   0.00   69
 11  ω    138.00 165.00   1.00   11.81    --  104.14  45.00 -30.00   27
 12  ω     89.00 114.00   1.00   11.81    --  104.14 -61.00 150.00   25
 13  ω     41.00 128.00   1.00   11.81    --  104.14 -30.00  30.00   87
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0800472000
_diffrn_orient_matrix_UB_12      0.1593887000
_diffrn_orient_matrix_UB_13      -0.0104882000
_diffrn_orient_matrix_UB_21      0.0419055000
_diffrn_orient_matrix_UB_22      -0.0584032000
_diffrn_orient_matrix_UB_23      0.1144860000
_diffrn_orient_matrix_UB_31      0.0666672000
_diffrn_orient_matrix_UB_32      -0.1542160000
_diffrn_orient_matrix_UB_33      -0.0540592000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1848
_reflns_number_total             2152
_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 1.171.42.81a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.81a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.81a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_refine_diff_density_max         0.444
_refine_diff_density_min         -0.571
_refine_diff_density_rms         0.107
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     193
_refine_ls_number_reflns         2152
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0434
_refine_ls_R_factor_gt           0.0364
_refine_ls_restrained_S_all      1.034
_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)+(0.0656P)²+0.2213P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0987
_refine_ls_wR_factor_ref         0.1042
_refine_special_details          'N-H bond lengths restrained to 0.90(2)A'
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 O1-H1
 0.9 with sigma of 0.02
 N1-H1B = N1-H1A
 0.9 with sigma of 0.02
3.a Aromatic/amide H refined with riding coordinates:
 C1(H1C), C2(H2), C6(H6), C7(H7), C8(H8)
;
_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
Cu1 Cu 0.00319(3) 0.60769(6) 0.75071(3) 0.00899(16) Uani 1 1 d . . . . .
O1 O 0.03849(14) 0.3569(3) 0.68645(15) 0.0095(4) Uani 1 1 d D . . . .
N1 N 0.15591(18) 0.8713(3) 0.36621(19) 0.0106(5) Uani 1 1 d D . . . .
N2 N 0.12840(16) 0.8636(3) 0.47774(19) 0.0093(5) Uani 1 1 d . . . . .
N3 N 0.06648(16) 0.9588(3) 0.63177(17) 0.0088(4) Uani 1 1 d . . . . .
N4 N 0.06187(16) 0.7554(3) 0.62639(17) 0.0090(4) Uani 1 1 d . . . . .
C1 C 0.10780(18) 1.0217(4) 0.5409(2) 0.0098(5) Uani 1 1 d . . . . .
H1C H 0.1208 1.1567 0.5231 0.012 Uiso 1 1 calc R U . . .
C2 C 0.09956(19) 0.6999(4) 0.5318(2) 0.0101(5) Uani 1 1 d . . . . .
H2 H 0.1053 0.5667 0.5063 0.012 Uiso 1 1 calc R U . . .
S1 S 0.25527(5) 0.13670(10) 0.79691(5) 0.01147(18) Uani 1 1 d . . . . .
O2 O 0.23831(14) 0.2732(3) 0.70444(16) 0.0182(4) Uani 1 1 d . . . . .
O3 O 0.17969(14) 0.1586(3) 0.87930(17) 0.0158(4) Uani 1 1 d . . . . .
O4 O 0.27152(14) -0.0666(3) 0.76253(16) 0.0152(4) Uani 1 1 d . . . . .
O5 O 0.31466(16) -0.1212(3) 0.98439(19) 0.0202(5) Uani 1 1 d . . . . .
C3 C 0.3990(2) -0.0680(5) 0.9857(2) 0.0139(6) Uani 1 1 d . . . . .
C4 C 0.4310(2) 0.1152(4) 0.9278(2) 0.0125(6) Uani 1 1 d . . . . .
C5 C 0.36894(19) 0.2254(4) 0.8560(2) 0.0122(5) Uani 1 1 d . . . . .
C6 C 0.4005(2) 0.4080(4) 0.8147(2) 0.0143(6) Uani 1 1 d . . . . .
H6 H 0.3580 0.4844 0.7684 0.017 Uiso 1 1 calc R U . . .
C7 C 0.4939(2) 0.4793(5) 0.8408(2) 0.0154(6) Uani 1 1 d . . . . .
H7 H 0.5135 0.6066 0.8153 0.018 Uiso 1 1 calc R U . . .
C8 C 0.5578(2) 0.3649(4) 0.9036(2) 0.0141(6) Uani 1 1 d . . . . .
H8 H 0.6229 0.4086 0.9166 0.017 Uiso 1 1 calc R U . . .
C9 C 0.5264(2) 0.1849(5) 0.9480(2) 0.0123(5) Uani 1 1 d . . . . .
H1A H 0.198(2) 0.777(4) 0.347(3) 0.016(9) Uiso 1 1 d D . . . .
H1 H 0.1010(15) 0.348(6) 0.681(4) 0.027(11) Uiso 1 1 d D . . . .
H1B H 0.181(3) 0.989(4) 0.355(3) 0.021(9) Uiso 1 1 d 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
Cu1 O1 1.9228(19) . ?
Cu1 O1 1.9316(19) 2_556 ?
Cu1 N3 2.003(2) 2_546 ?
Cu1 N4 1.992(2) . ?
O1 Cu1 1.9316(19) 2_546 ?
O1 H1 0.865(19) . ?
N1 N2 1.414(3) . ?
N1 H1A 0.893(19) . ?
N1 H1B 0.874(19) . ?
N2 C1 1.344(4) . ?
N2 C2 1.344(4) . ?
N3 Cu1 2.003(2) 2_556 ?
N3 N4 1.369(3) . ?
N3 C1 1.321(3) . ?
N4 C2 1.324(3) . ?
C1 H1C 0.9500 . ?
C2 H2 0.9500 . ?
S1 O2 1.463(2) . ?
S1 O3 1.466(2) . ?
S1 O4 1.447(2) . ?
S1 C5 1.802(3) . ?
O5 C3 1.212(4) . ?
C3 C4 1.487(4) . ?
C3 C9 1.507(4) 3_657 ?
C4 C5 1.413(4) . ?
C4 C9 1.408(4) . ?
C5 C6 1.397(4) . ?
C6 H6 0.9500 . ?
C6 C7 1.398(4) . ?
C7 H7 0.9500 . ?
C7 C8 1.381(4) . ?
C8 H8 0.9500 . ?
C8 C9 1.395(4) . ?
C9 C3 1.507(4) 3_657 ?

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
O1 Cu1 O1 177.35(3) . 2_556 ?
O1 Cu1 N3 90.02(9) 2_556 2_546 ?
O1 Cu1 N3 88.91(9) . 2_546 ?
O1 Cu1 N4 91.06(9) . . ?
O1 Cu1 N4 89.80(9) 2_556 . ?
N4 Cu1 N3 175.13(9) . 2_546 ?
Cu1 O1 Cu1 121.26(9) . 2_546 ?
Cu1 O1 H1 111(3) . . ?
Cu1 O1 H1 106(3) 2_546 . ?
N2 N1 H1A 115(2) . . ?
N2 N1 H1B 107(3) . . ?
H1A N1 H1B 110(4) . . ?
C1 N2 N1 125.5(2) . . ?
C1 N2 C2 107.4(2) . . ?
C2 N2 N1 125.8(2) . . ?
N4 N3 Cu1 120.63(16) . 2_556 ?
C1 N3 Cu1 131.03(19) . 2_556 ?
C1 N3 N4 107.4(2) . . ?
N3 N4 Cu1 118.68(15) . . ?
C2 N4 Cu1 133.7(2) . . ?
C2 N4 N3 107.7(2) . . ?
N2 C1 H1C 125.6 . . ?
N3 C1 N2 108.9(2) . . ?
N3 C1 H1C 125.6 . . ?
N2 C2 H2 125.7 . . ?
N4 C2 N2 108.6(2) . . ?
N4 C2 H2 125.7 . . ?
O2 S1 O3 110.98(12) . . ?
O2 S1 C5 102.57(12) . . ?
O3 S1 C5 108.43(12) . . ?
O4 S1 O2 113.15(13) . . ?
O4 S1 O3 114.09(12) . . ?
O4 S1 C5 106.78(12) . . ?
O5 C3 C4 122.0(3) . . ?
O5 C3 C9 119.3(3) . 3_657 ?
C4 C3 C9 118.6(2) . 3_657 ?
C5 C4 C3 123.0(3) . . ?
C9 C4 C3 118.5(3) . . ?
C9 C4 C5 118.5(3) . . ?
C4 C5 S1 125.1(2) . . ?
C6 C5 S1 114.9(2) . . ?
C6 C5 C4 119.6(3) . . ?
C5 C6 H6 119.7 . . ?
C5 C6 C7 120.7(3) . . ?
C7 C6 H6 119.7 . . ?
C6 C7 H7 120.0 . . ?
C8 C7 C6 120.1(3) . . ?
C8 C7 H7 120.0 . . ?
C7 C8 H8 120.1 . . ?
C7 C8 C9 119.8(3) . . ?
C9 C8 H8 120.1 . . ?
C4 C9 C3 122.4(3) . 3_657 ?
C8 C9 C3 116.5(3) . 3_657 ?
C8 C9 C4 121.1(3) . . ?

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 N4 Cu1 -9.8(2) 2_556 . . . ?
Cu1 N3 N4 C2 169.53(17) 2_556 . . . ?
Cu1 N3 C1 N2 -168.12(18) 2_556 . . . ?
Cu1 N4 C2 N2 179.56(18) . . . . ?
N1 N2 C1 N3 167.5(2) . . . . ?
N1 N2 C2 N4 -167.9(2) . . . . ?
N3 N4 C2 N2 0.4(3) . . . . ?
N4 N3 C1 N2 0.7(3) . . . . ?
C1 N2 C2 N4 0.0(3) . . . . ?
C1 N3 N4 Cu1 -179.98(17) . . . . ?
C1 N3 N4 C2 -0.7(3) . . . . ?
C2 N2 C1 N3 -0.4(3) . . . . ?
S1 C5 C6 C7 -170.3(2) . . . . ?
O2 S1 C5 C4 -161.7(2) . . . . ?
O2 S1 C5 C6 10.3(2) . . . . ?
O3 S1 C5 C4 80.8(3) . . . . ?
O3 S1 C5 C6 -107.2(2) . . . . ?
O4 S1 C5 C4 -42.5(3) . . . . ?
O4 S1 C5 C6 129.5(2) . . . . ?
O5 C3 C4 C5 -8.5(4) . . . . ?
O5 C3 C4 C9 169.6(3) . . . . ?
C3 C4 C5 S1 -15.8(4) . . . . ?
C3 C4 C5 C6 172.6(3) . . . . ?
C3 C4 C9 C3 7.8(4) . . . 3_657 ?
C3 C4 C9 C8 -174.4(2) . . . . ?
C4 C5 C6 C7 2.1(4) . . . . ?
C5 C4 C9 C3 -174.0(3) . . . 3_657 ?
C5 C4 C9 C8 3.8(4) . . . . ?
C5 C6 C7 C8 3.2(4) . . . . ?
C6 C7 C8 C9 -4.9(4) . . . . ?
C7 C8 C9 C3 179.3(3) . . . 3_657 ?
C7 C8 C9 C4 1.4(4) . . . . ?
C9 C3 C4 C5 174.4(3) 3_657 . . . ?
C9 C3 C4 C9 -7.5(4) 3_657 . . . ?
C9 C4 C5 S1 166.1(2) . . . . ?
C9 C4 C5 C6 -5.5(4) . . . . ?

_olex2_date_sample_data_collection 2023-02-20
_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 3.089
_oxdiff_exptl_absorpt_empirical_full_min 0.770
####################################################################### 
# 
# 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_cs_ca_nds_dmf_a
_database_code_depnum_ccdc_archive 'CCDC 2336806'
loop_
_audit_author_name
_audit_author_address
'Christopher Pask'
;University of Leeds
United Kingdom
;
_audit_update_record             
;
2024-03-01 deposited with the CCDC.	2024-06-18 downloaded from the CCDC.
;
_audit_creation_date             2022-11-15
_audit_creation_method           
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C16 H20 Ca N2 O8 S2'
_chemical_formula_sum            'C16 H20 Ca N2 O8 S2'
_chemical_formula_weight         472.54
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C32  H40  Ca2  N4  O16  S4  '
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'
Ca Ca 0.2262 0.3064 '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                   9.4952(7)
_cell_length_b                   10.2875(7)
_cell_length_c                   11.0657(8)
_cell_angle_alpha                74.765(6)
_cell_angle_beta                 79.328(6)
_cell_angle_gamma                85.839(6)
_cell_volume                     1024.57(13)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    1836
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      29.3540
_cell_measurement_theta_min      2.9640
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.556
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.717
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.93a (Rigaku Oxford Diffraction, 2020)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.532
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             492
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-13 0 1 0.0374
13 0 -1 0.0374
8 -10 -3 0.1021
-1 -14 -3 0.1548
1 14 3 0.1899
12 5 0 0.0921
5 0 15 0.0274
-6 -4 -15 0.0986
-7 -11 -11 0.1262
0 10 -8 0.1772

_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.08
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-12.9553 0.4393 1.0186 -0.8742 0.4786 0.0821
12.9553 -0.4393 -1.0186 0.8742 -0.4786 -0.0821
8.4048 -10.4608 -2.9831 0.4348 -0.5771 -0.6913
-1.2914 -14.4702 -3.2109 -0.2759 -0.3325 -0.9019
0.7069 14.4805 3.2547 0.2363 0.3539 0.9050
12.4377 5.0851 0.2789 0.9109 -0.3152 0.2664
5.1443 -0.3246 14.5814 -0.2738 -0.9010 0.3366
-6.4700 -3.8240 -14.8175 0.1044 0.8111 -0.5756
-7.1531 -11.2154 -10.5673 -0.2808 0.3649 -0.8877
0.3885 10.3422 -7.5252 0.5671 0.7209 0.3983

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0411
_diffrn_reflns_av_unetI/netI     0.0931
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.815
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            8441
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.815
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.831
_diffrn_reflns_theta_min         2.052
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3095
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.815
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -12.00  78.00   1.00    2.50    --    9.30  57.00  90.00   90
  2  ω    -59.00  34.00   1.00    2.50    --    9.30 -57.00 -60.00   93
  3  ω    -41.00   5.00   1.00    2.50    --   -9.92 -37.00 150.00   46
  4  ω    -45.00  -2.00   1.00    2.50    --   -9.92 -57.00 120.00   43
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0649962000
_diffrn_orient_matrix_UB_12      0.0224070000
_diffrn_orient_matrix_UB_13      -0.0412073000
_diffrn_orient_matrix_UB_21      -0.0393913000
_diffrn_orient_matrix_UB_22      0.0369390000
_diffrn_orient_matrix_UB_23      -0.0470699000
_diffrn_orient_matrix_UB_31      -0.0024275000
_diffrn_orient_matrix_UB_32      0.0569483000
_diffrn_orient_matrix_UB_33      0.0252069000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2467
_reflns_number_total             4810
_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 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_refine_diff_density_max         0.558
_refine_diff_density_min         -0.561
_refine_diff_density_rms         0.094
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     266
_refine_ls_number_reflns         4810
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1174
_refine_ls_R_factor_gt           0.0550
_refine_ls_restrained_S_all      1.043
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0348P)²+0.1550P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1037
_refine_ls_wR_factor_ref         0.1406
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C7(H7), C8(H8), C9(H9), C11(H11), C14(H14)
2.b Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C15(H15A,H15B,H15C), C16(H16A,H16B,
 H16C)
;
_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
Ca1 Ca 0.50330(8) 0.99961(7) 0.24881(7) 0.01177(17) Uani 1 1 d . . . . .
S1 S 0.63324(9) 0.78745(9) 0.53690(8) 0.0127(2) Uani 1 1 d . . . . .
S2 S 0.36196(9) 0.21228(9) 0.96562(8) 0.0125(2) Uani 1 1 d . . . . .
O1 O 0.5750(3) 0.8615(2) 0.4253(2) 0.0191(6) Uani 1 1 d . . . . .
O2 O 0.6268(2) 0.8675(2) 0.6291(2) 0.0156(6) Uani 1 1 d . . . . .
O3 O 0.7753(2) 0.7318(2) 0.5056(2) 0.0186(6) Uani 1 1 d . . . . .
O4 O 0.2223(2) 0.2702(2) 1.0005(2) 0.0182(6) Uani 1 1 d . . . . .
O5 O 0.3615(2) 0.1320(2) 0.8743(2) 0.0160(6) Uani 1 1 d . . . . .
O6 O 0.4240(3) 0.1360(2) 1.0746(2) 0.0179(6) Uani 1 1 d . . . . .
O7 O 0.3084(3) 0.8656(3) 0.2704(2) 0.0191(6) Uani 1 1 d . . . . .
O8 O 0.7068(3) 1.1273(3) 0.2166(2) 0.0223(6) Uani 1 1 d . . . . .
N1 N 0.1146(3) 0.7872(3) 0.2229(3) 0.0245(8) Uani 1 1 d . . . . .
N2 N 0.9181(3) 1.1800(4) 0.2583(3) 0.0264(8) Uani 1 1 d . . . . .
C1 C 0.5170(4) 0.6500(3) 0.6103(3) 0.0111(8) Uani 1 1 d . . . . .
C2 C 0.4065(3) 0.6352(4) 0.5530(3) 0.0132(8) Uani 1 1 d . . . . .
H2 H 0.3892 0.7005 0.4784 0.016 Uiso 1 1 calc R U . . .
C3 C 0.3172(4) 0.5228(4) 0.6043(3) 0.0139(8) Uani 1 1 d . . . . .
H3 H 0.2407 0.5124 0.5634 0.017 Uiso 1 1 calc R U . . .
C4 C 0.3400(4) 0.4297(4) 0.7116(3) 0.0140(8) Uani 1 1 d . . . . .
H4 H 0.2796 0.3543 0.7444 0.017 Uiso 1 1 calc R U . . .
C5 C 0.4529(4) 0.4429(4) 0.7759(3) 0.0132(8) Uani 1 1 d . . . . .
C6 C 0.4791(4) 0.3480(3) 0.8903(3) 0.0119(8) Uani 1 1 d . . . . .
C7 C 0.5912(4) 0.3632(4) 0.9478(3) 0.0142(8) Uani 1 1 d . . . . .
H7 H 0.6080 0.2989 1.0231 0.017 Uiso 1 1 calc R U . . .
C8 C 0.6813(4) 0.4743(4) 0.8948(3) 0.0141(8) Uani 1 1 d . . . . .
H8 H 0.7591 0.4839 0.9346 0.017 Uiso 1 1 calc R U . . .
C9 C 0.6585(4) 0.5680(4) 0.7874(3) 0.0132(8) Uani 1 1 d . . . . .
H9 H 0.7193 0.6431 0.7543 0.016 Uiso 1 1 calc R U . . .
C10 C 0.5452(3) 0.5552(3) 0.7240(3) 0.0104(7) Uani 1 1 d . . . . .
C11 C 0.2257(4) 0.8658(4) 0.1962(4) 0.0269(10) Uani 1 1 d . . . . .
H11 H 0.2435 0.9268 0.1143 0.032 Uiso 1 1 calc R U . . .
C12 C 0.0860(4) 0.6848(4) 0.3422(4) 0.0293(10) Uani 1 1 d . . . . .
H12A H 0.1110 0.5957 0.3269 0.044 Uiso 1 1 calc R U . . .
H12B H -0.0160 0.6886 0.3787 0.044 Uiso 1 1 calc R U . . .
H12C H 0.1436 0.7010 0.4015 0.044 Uiso 1 1 calc R U . . .
C13 C 0.0222(5) 0.7910(5) 0.1311(5) 0.0484(14) Uani 1 1 d . . . . .
H13A H -0.0727 0.8273 0.1601 0.073 Uiso 1 1 calc R U . . .
H13B H 0.0129 0.6996 0.1228 0.073 Uiso 1 1 calc R U . . .
H13C H 0.0639 0.8488 0.0485 0.073 Uiso 1 1 calc R U . . .
C14 C 0.8146(4) 1.0982(4) 0.2677(4) 0.0277(10) Uani 1 1 d . . . . .
H14 H 0.8230 1.0087 0.3182 0.033 Uiso 1 1 calc R U . . .
C15 C 0.9155(4) 1.3185(4) 0.1831(4) 0.0290(11) Uani 1 1 d . . . . .
H15A H 0.9941 1.3312 0.1102 0.044 Uiso 1 1 calc R U . . .
H15B H 0.9268 1.3790 0.2357 0.044 Uiso 1 1 calc R U . . .
H15C H 0.8238 1.3389 0.1527 0.044 Uiso 1 1 calc R U . . .
C16 C 1.0443(4) 1.1341(5) 0.3185(4) 0.0404(12) Uani 1 1 d . . . . .
H16A H 1.0334 1.0398 0.3669 0.061 Uiso 1 1 calc R U . . .
H16B H 1.0535 1.1898 0.3761 0.061 Uiso 1 1 calc R U . . .
H16C H 1.1304 1.1422 0.2529 0.061 Uiso 1 1 calc R 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
Ca1 O1 2.278(3) . ?
Ca1 O2 2.307(2) 2_676 ?
Ca1 O5 2.325(2) 2_666 ?
Ca1 O6 2.284(3) 1_564 ?
Ca1 O7 2.327(2) . ?
Ca1 O8 2.335(3) . ?
S1 O1 1.452(3) . ?
S1 O2 1.461(2) . ?
S1 O3 1.444(2) . ?
S1 C1 1.780(3) . ?
S2 O4 1.442(2) . ?
S2 O5 1.464(2) . ?
S2 O6 1.454(3) . ?
S2 C6 1.776(4) . ?
O2 Ca1 2.307(2) 2_676 ?
O5 Ca1 2.325(2) 2_666 ?
O6 Ca1 2.284(3) 1_546 ?
O7 C11 1.236(5) . ?
O8 C14 1.241(5) . ?
N1 C11 1.318(5) . ?
N1 C12 1.450(5) . ?
N1 C13 1.452(5) . ?
N2 C14 1.312(5) . ?
N2 C15 1.450(5) . ?
N2 C16 1.467(5) . ?
C1 C2 1.358(5) . ?
C1 C10 1.432(5) . ?
C2 H2 0.9500 . ?
C2 C3 1.413(5) . ?
C3 H3 0.9500 . ?
C3 C4 1.357(5) . ?
C4 H4 0.9500 . ?
C4 C5 1.425(5) . ?
C5 C6 1.432(5) . ?
C5 C10 1.429(4) . ?
C6 C7 1.375(5) . ?
C7 H7 0.9500 . ?
C7 C8 1.409(5) . ?
C8 H8 0.9500 . ?
C8 C9 1.360(5) . ?
C9 H9 0.9500 . ?
C9 C10 1.419(5) . ?
C11 H11 0.9500 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14 0.9500 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?

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
O1 Ca1 O2 90.32(9) . 2_676 ?
O1 Ca1 O5 89.50(9) . 2_666 ?
O1 Ca1 O6 178.16(9) . 1_564 ?
O1 Ca1 O7 91.61(9) . . ?
O1 Ca1 O8 89.13(9) . . ?
O2 Ca1 O5 178.84(9) 2_676 2_666 ?
O2 Ca1 O7 92.73(8) 2_676 . ?
O2 Ca1 O8 91.01(8) 2_676 . ?
O5 Ca1 O7 88.42(8) 2_666 . ?
O5 Ca1 O8 87.84(9) 2_666 . ?
O6 Ca1 O2 88.90(9) 1_564 2_676 ?
O6 Ca1 O5 91.31(9) 1_564 2_666 ?
O6 Ca1 O7 86.76(9) 1_564 . ?
O6 Ca1 O8 92.56(9) 1_564 . ?
O7 Ca1 O8 176.18(9) . . ?
O1 S1 O2 111.82(14) . . ?
O1 S1 C1 105.35(16) . . ?
O2 S1 C1 106.72(14) . . ?
O3 S1 O1 112.80(14) . . ?
O3 S1 O2 112.11(15) . . ?
O3 S1 C1 107.51(15) . . ?
O4 S2 O5 112.00(15) . . ?
O4 S2 O6 113.23(14) . . ?
O4 S2 C6 107.17(15) . . ?
O5 S2 C6 107.45(14) . . ?
O6 S2 O5 111.27(14) . . ?
O6 S2 C6 105.22(16) . . ?
S1 O1 Ca1 172.50(16) . . ?
S1 O2 Ca1 149.67(15) . 2_676 ?
S2 O5 Ca1 146.17(15) . 2_666 ?
S2 O6 Ca1 173.93(16) . 1_546 ?
C11 O7 Ca1 130.7(3) . . ?
C14 O8 Ca1 128.4(3) . . ?
C11 N1 C12 121.2(4) . . ?
C11 N1 C13 121.9(4) . . ?
C12 N1 C13 116.7(4) . . ?
C14 N2 C15 121.3(4) . . ?
C14 N2 C16 121.6(4) . . ?
C15 N2 C16 117.0(4) . . ?
C2 C1 S1 118.5(3) . . ?
C2 C1 C10 121.7(3) . . ?
C10 C1 S1 119.7(3) . . ?
C1 C2 H2 120.0 . . ?
C1 C2 C3 120.1(4) . . ?
C3 C2 H2 120.0 . . ?
C2 C3 H3 119.8 . . ?
C4 C3 C2 120.4(3) . . ?
C4 C3 H3 119.8 . . ?
C3 C4 H4 119.4 . . ?
C3 C4 C5 121.2(3) . . ?
C5 C4 H4 119.4 . . ?
C4 C5 C6 122.9(3) . . ?
C4 C5 C10 118.9(3) . . ?
C10 C5 C6 118.2(3) . . ?
C5 C6 S2 120.6(3) . . ?
C7 C6 S2 118.3(3) . . ?
C7 C6 C5 121.0(3) . . ?
C6 C7 H7 120.0 . . ?
C6 C7 C8 119.9(4) . . ?
C8 C7 H7 120.0 . . ?
C7 C8 H8 119.5 . . ?
C9 C8 C7 120.9(3) . . ?
C9 C8 H8 119.5 . . ?
C8 C9 H9 119.5 . . ?
C8 C9 C10 121.0(3) . . ?
C10 C9 H9 119.5 . . ?
C5 C10 C1 117.6(3) . . ?
C9 C10 C1 123.4(3) . . ?
C9 C10 C5 119.0(3) . . ?
O7 C11 N1 124.4(4) . . ?
O7 C11 H11 117.8 . . ?
N1 C11 H11 117.8 . . ?
N1 C12 H12A 109.5 . . ?
N1 C12 H12B 109.5 . . ?
N1 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
N1 C13 H13A 109.5 . . ?
N1 C13 H13B 109.5 . . ?
N1 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
O8 C14 N2 125.8(4) . . ?
O8 C14 H14 117.1 . . ?
N2 C14 H14 117.1 . . ?
N2 C15 H15A 109.5 . . ?
N2 C15 H15B 109.5 . . ?
N2 C15 H15C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
N2 C16 H16A 109.5 . . ?
N2 C16 H16B 109.5 . . ?
N2 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?

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
Ca1 O7 C11 N1 -177.0(2) . . . . ?
Ca1 O8 C14 N2 -170.9(3) . . . . ?
S1 C1 C2 C3 176.1(2) . . . . ?
S1 C1 C10 C5 -177.0(2) . . . . ?
S1 C1 C10 C9 3.6(4) . . . . ?
S2 C6 C7 C8 -176.2(2) . . . . ?
O1 S1 O2 Ca1 51.5(3) . . . 2_676 ?
O1 S1 C1 C2 2.2(3) . . . . ?
O1 S1 C1 C10 179.5(2) . . . . ?
O2 S1 C1 C2 121.2(3) . . . . ?
O2 S1 C1 C10 -61.5(3) . . . . ?
O3 S1 O2 Ca1 179.3(3) . . . 2_676 ?
O3 S1 C1 C2 -118.3(3) . . . . ?
O3 S1 C1 C10 58.9(3) . . . . ?
O4 S2 O5 Ca1 179.1(2) . . . 2_666 ?
O4 S2 C6 C5 -61.0(3) . . . . ?
O4 S2 C6 C7 115.9(3) . . . . ?
O5 S2 C6 C5 59.6(3) . . . . ?
O5 S2 C6 C7 -123.5(3) . . . . ?
O6 S2 O5 Ca1 -53.0(3) . . . 2_666 ?
O6 S2 C6 C5 178.2(2) . . . . ?
O6 S2 C6 C7 -4.9(3) . . . . ?
C1 S1 O2 Ca1 -63.3(3) . . . 2_676 ?
C1 C2 C3 C4 0.7(5) . . . . ?
C2 C1 C10 C5 0.2(4) . . . . ?
C2 C1 C10 C9 -179.3(3) . . . . ?
C2 C3 C4 C5 0.6(5) . . . . ?
C3 C4 C5 C6 179.1(3) . . . . ?
C3 C4 C5 C10 -1.4(5) . . . . ?
C4 C5 C6 S2 -4.6(4) . . . . ?
C4 C5 C6 C7 178.6(3) . . . . ?
C4 C5 C10 C1 1.1(4) . . . . ?
C4 C5 C10 C9 -179.5(3) . . . . ?
C5 C6 C7 C8 0.7(5) . . . . ?
C6 S2 O5 Ca1 61.7(3) . . . 2_666 ?
C6 C5 C10 C1 -179.4(3) . . . . ?
C6 C5 C10 C9 0.0(4) . . . . ?
C6 C7 C8 C9 0.5(5) . . . . ?
C7 C8 C9 C10 -1.4(5) . . . . ?
C8 C9 C10 C1 -179.5(3) . . . . ?
C8 C9 C10 C5 1.1(4) . . . . ?
C10 C1 C2 C3 -1.1(5) . . . . ?
C10 C5 C6 S2 175.9(2) . . . . ?
C10 C5 C6 C7 -0.9(4) . . . . ?
C12 N1 C11 O7 -4.5(6) . . . . ?
C13 N1 C11 O7 -179.3(4) . . . . ?
C15 N2 C14 O8 -0.2(6) . . . . ?
C16 N2 C14 O8 -177.5(4) . . . . ?

_olex2_date_sample_data_collection 2022-11-15
_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 1.475
_oxdiff_exptl_absorpt_empirical_full_min 0.814
