# Electronic Supplementary Material (ESI) for New Journal of Chemistry.
# This journal is © The Royal Society of Chemistry and the Centre National de la Recherche Scientifique 2022

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

data_RB21092_auto
_database_code_depnum_ccdc_archive 'CCDC 2119282'
loop_
_audit_author_name
_audit_author_address
'Rene Boere'
;University of Lethbridge
Canada
;
_audit_update_record             
;
2022-01-10 deposited with the CCDC.	2022-02-02 downloaded from the CCDC.
;
_audit_creation_date             2022-01-08
_audit_creation_method           
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_chemical_formula_moiety         'Cu H6 O7 S'
_chemical_formula_sum            'Cu H6 O7 S'
_chemical_formula_weight         213.655
_chemical_absolute_configuration ad
_chemical_oxdiff_formula         'Cu S O7 H6'
_chemical_oxdiff_usercomment     
'Smaller Xtal - small block cut from larger crystals'
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
_atom_type_scat_dispersion_source
Cu 0.34125 1.28947 'NoSpherA2: Chem.Sci. 2021, DOI:10.1039/D0SC05526C'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
H 0.00000 0.00000 'NoSpherA2: Chem.Sci. 2021, DOI:10.1039/D0SC05526C'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
O 0.01158 0.00611 'NoSpherA2: Chem.Sci. 2021, DOI:10.1039/D0SC05526C'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
S 0.12424 0.12443 'NoSpherA2: Chem.Sci. 2021, DOI:10.1039/D0SC05526C'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'

_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_H-M_alt        'C 1 c 1'
_space_group_name_Hall           ' C -2yc'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 x,y,z
2 x,-y,z+1/2
3 x+1/2,y+1/2,z
4 x+1/2,-y+1/2,z+1/2

_symmetry_Int_Tables_number      9
_cell_length_a                   5.5708(2)
_cell_length_b                   12.9751(4)
_cell_length_c                   7.3754(2)
_cell_angle_alpha                90
_cell_angle_beta                 96.450(3)
_cell_angle_gamma                90
_cell_volume                     529.73(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    10841
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      38.3700
_cell_measurement_theta_min      3.0270
_exptl_absorpt_coefficient_mu    4.488
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.95627
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.110a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear grayish blue'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   grayish
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    2.679
_exptl_crystal_description       prism
_exptl_crystal_F_000             430.301
_exptl_crystal_recrystallization_method 
'The material was recrystallised from --- by'
_exptl_crystal_size_max          0.101
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.057
_diffrn_reflns_av_R_equivalents  0.0375
_diffrn_reflns_av_unetI/netI     0.0284
_diffrn_reflns_Laue_measured_fraction_full 1.0000
_diffrn_reflns_Laue_measured_fraction_max 0.9639
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            13522
_diffrn_reflns_point_group_measured_fraction_full 1.0000
_diffrn_reflns_point_group_measured_fraction_max 0.9446
_diffrn_reflns_theta_full        25.2417
_diffrn_reflns_theta_max         38.16
_diffrn_reflns_theta_min         3.14
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 5.8140
_diffrn_detector_type            'Pilatus 200K'
_diffrn_measured_fraction_theta_full 1.0000
_diffrn_measured_fraction_theta_max 0.9639
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     37.00  91.00   0.50    3.59    --   22.41-178.00-150.00  108
  2  ω     37.00  91.00   0.50    3.59    --   22.41-178.00 -30.00  108
  3  ω    -15.00  58.00   0.50    3.59    --   22.41 -99.00 120.00  146
  4  ω    -37.00  38.00   0.50    3.59    --  -25.54  57.00 -60.00  150
  5  ω    -80.00 -30.00   0.50    3.59    --  -25.54 130.00 113.16  100
  6  ω    -87.00 -36.00   0.50    3.59    --  -25.54 142.00-147.35  102
  7  ω    -14.00  13.00   0.50    3.59    --  -25.54-103.00  42.04   54
  8  ω    -29.00  41.00   0.50    3.59    --  -25.54  38.00  60.00  140
  9  ω    -19.00   9.00   0.50    3.59    --  -25.54 -96.00-108.75   56
 10  ω    -95.00 -20.00   0.50    3.59    --  -25.54 -19.00 -60.00  150
 11  ω    -22.00   7.00   0.50    3.59    --  -25.54 -93.00 -21.65   58
 12  ω    -36.00  -6.00   0.50    3.59    --  -25.54 -73.00 161.82   60
 13  ω    -82.00 -33.00   0.50    3.59    --  -25.54 133.00 -54.40   98
 14  ω    -29.00  41.00   0.50    3.59    --  -25.54  38.00-180.00  140
 15  ω    -92.00 -22.00   0.50    3.59    --  -25.54 -38.00  30.00  140
 16  ω     11.00  85.00   0.50    3.59    --   22.41  57.00 -90.00  148
 17  ω     37.00  91.00   0.50    3.59    --   22.41-178.00  90.00  108
 18  ω     11.00  85.00   0.50    3.59    --   22.41  57.00-150.00  148
 19  ω    -22.00   7.00   0.50    3.59    --  -25.54 -93.00  67.26   58
 20  ω    -89.00 -14.00   0.50    3.59    --  -25.54 -57.00   0.00  150
 21  ω    -14.00  12.00   0.50    3.59    --  -25.54-102.00 -66.73   52
 22  ω    -93.00 -49.00   0.50    3.59    --  -25.54 150.00 129.03   88
 23  ω    -89.00 -14.00   0.50    3.59    --  -25.54 -57.00-120.00  150
 24  ω    -92.00 -22.00   0.50    3.59    --  -25.54 -38.00 120.00  140
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  
'SuperNova, Dual, Cu at home/near, Pilatus 200K'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0781743000
_diffrn_orient_matrix_UB_12      -0.0114271000
_diffrn_orient_matrix_UB_13      -0.0668453000
_diffrn_orient_matrix_UB_21      0.0414769000
_diffrn_orient_matrix_UB_22      -0.0445329000
_diffrn_orient_matrix_UB_23      0.0497496000
_diffrn_orient_matrix_UB_31      -0.0927301000
_diffrn_orient_matrix_UB_32      -0.0295665000
_diffrn_orient_matrix_UB_33      -0.0491910000
_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         0.925
_reflns_limit_h_max              9
_reflns_limit_h_min              -9
_reflns_limit_k_max              22
_reflns_limit_k_min              -22
_reflns_limit_l_max              12
_reflns_limit_l_min              -12
_reflns_number_gt                2715
_reflns_number_total             2761
_reflns_threshold_expression     I>=2u(I)
_computing_cell_refinement       'CrysAlisPro 1.171.41.110a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.110a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.110a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.5 (Bourhis et al., 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.3868
_refine_diff_density_min         -0.8111
_refine_diff_density_rms         0.1105
_refine_ls_abs_structure_details 
'Hooft, R.W.W., Straver, L.H., Spek, A.L. (2010). J. Appl. Cryst., 43, 665-668.'
_refine_ls_abs_structure_Flack   0.001(4)
_refine_ls_d_res_high            0.5752
_refine_ls_d_res_low             6.4875
_refine_ls_goodness_of_fit_ref   1.0125
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     136
_refine_ls_number_reflns         2761
_refine_ls_number_restraints     128
_refine_ls_R_factor_all          0.0194
_refine_ls_R_factor_gt           0.0188
_refine_ls_restrained_S_all      0.9891
_refine_ls_shift/su_max          -0.0009
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0228P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0424
_refine_ls_wR_factor_ref         0.0429
_refine_special_details          
;Refinement using NoSpherA2, an implementation of
NOn-SPHERical Atom-form-factors in Olex2.
Please cite:
F. Kleemiss et al. Chem. Sci. DOI 10.1039/D0SC05526C - 2021
NoSpherA2 implementation of HAR makes use of
tailor-made aspherical atomic form factors calculated
on-the-fly from a Hirshfeld-partitioned electron density (ED) - not from
spherical-atom form factors.

The ED is calculated from a gaussian basis set single determinant SCF
wavefunction - either Hartree-Fock or DFT using selected funtionals
 - for a fragment of the crystal.
This fragment can be embedded in an electrostatic crystal field by employing cluster charges
or modelled using implicit solvation models, depending on the software used.
The following options were used:
   SOFTWARE:       'Please Select'
   PARTITIONING:   NoSpherA2
   INT ACCURACY:   Normal
   METHOD:         B3LYP
   BASIS SET:      def2-SVP
   CHARGE:         0
   MULTIPLICITY:   0
   DATE:           2022-01-08_12-56-30,NoSpherA2 refinement.
;
_olex2_refinement_description    
;
1. Restrained distances
 O6-H6b = O6-H6a = O5-H5a = O5-H5b = O7-H7b = O7-H7a
 0.989 with sigma of 0.02
2. Uiso/Uaniso restraints and constraints
Uanis(H7b) \\sim Ueq, Uanis(H6a) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
3. Rigid body (RIGU) restrains
 Cu1, O1, O1, O1, O2, O2, O2, O3, O3, O3, O4, O4, O4, O5, H5a, H5b, O6, H6a,
 H6b, O7, H7a, H7b, S1, S1, S1
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 H7b, H6b, H5b, H5a
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
;
_atom_sites_solution_primary     dual
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_refinement_flags_posn
_atom_site_refinement_flags_adp
Cu1 Cu 0.41266(2) 0.635078(10) 0.350672(18) 0.00453(3) Uani 1.000000 . U
O1 O 0.57354(17) 0.66499(8) 0.59472(12) 0.00728(16) Uani 1.000000 . U
O2 O 0.89114(16) 0.55438(8) 0.73194(13) 0.00908(16) Uani 1.000000 . U
O3 O 0.49382(16) 0.54393(7) 0.83293(13) 0.00807(15) Uani 1.000000 . U
O4 O 0.73805(17) 0.69579(8) 0.90100(12) 0.00774(15) Uani 1.000000 . U
O5 O 0.69954(16) 0.69432(8) 0.26051(12) 0.00790(15) Uani 1.000000 D U
H5a H 0.712(5) 0.693(3) 0.127(2) 0.023(6) Uani 1.000000 D U
H5b H 0.850(3) 0.679(2) 0.343(3) 0.012(5) Uani 1.000000 D U
O6 O 0.24629(19) 0.62860(7) 0.09894(15) 0.00758(17) Uani 1.000000 D U
H6a H 0.336(4) 0.603(2) 0.002(3) 0.013(5) Uani 1.000000 D U
H6b H 0.156(5) 0.6920(16) 0.059(4) 0.018(5) Uani 1.000000 D U
O7 O 0.10630(16) 0.59053(8) 0.43301(12) 0.00698(15) Uani 1.000000 D U
H7a H 0.040(4) 0.5273(15) 0.368(3) 0.013(5) Uani 1.000000 D U
H7b H 0.072(6) 0.588(2) 0.557(2) 0.024(5) Uani 1.000000 D U
S1 S 0.67501(5) 0.61297(2) 0.76723(4) 0.00384(5) Uani 1.000000 . U


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 1.9574(9) . ?
Cu1 O3 2.3726(10) 2_564 ?
Cu1 O5 1.9560(9) . ?
Cu1 O6 1.9816(11) . ?
Cu1 O7 1.9618(9) . ?
O1 S1 1.4941(10) . ?
O2 S1 1.4717(10) . ?
O3 S1 1.4717(10) . ?
O4 S1 1.4743(10) . ?
O5 H5a 0.998(15) . ?
O5 H5b 1.001(15) . ?
O6 H6a 0.978(15) . ?
O6 H6b 0.993(16) . ?
O7 H7a 1.000(15) . ?
O7 H7b 0.954(16) . ?

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
O3 Cu1 O1 100.05(4) 2_564 . ?
O5 Cu1 O1 85.84(4) . . ?
O5 Cu1 O3 101.41(4) . 2_564 ?
O6 Cu1 O1 170.99(4) . . ?
O6 Cu1 O3 88.78(4) . 2_564 ?
O6 Cu1 O5 90.70(4) . . ?
O7 Cu1 O1 95.63(4) . . ?
O7 Cu1 O3 84.63(4) . 2_564 ?
O7 Cu1 O5 173.46(4) . . ?
O7 Cu1 O6 86.90(4) . . ?
S1 O1 Cu1 141.61(7) . . ?
S1 O3 Cu1 139.11(6) . 2_565 ?
H5a O5 Cu1 118.8(16) . . ?
H5b O5 Cu1 112.0(15) . . ?
H5b O5 H5a 117(2) . . ?
H6a O6 Cu1 118.6(15) . . ?
H6b O6 Cu1 114.3(16) . . ?
H6b O6 H6a 110(2) . . ?
H7a O7 Cu1 112.5(14) . . ?
H7b O7 Cu1 125.5(18) . . ?
H7b O7 H7a 109(2) . . ?
O2 S1 O1 108.76(6) . . ?
O3 S1 O1 110.34(6) . . ?
O3 S1 O2 110.41(6) . . ?
O4 S1 O1 106.23(6) . . ?
O4 S1 O2 110.90(6) . . ?
O4 S1 O3 110.12(6) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O5 H5a O4 0.998(15) 1.687(16) 2.6841(13) 178(3) 1_554
O5 H5b O7 1.001(15) 1.890(19) 2.8141(13) 152(2) 1_655
O6 H6a O3 0.978(15) 1.776(16) 2.7505(14) 174(2) 1_554
O6 H6b O1 0.993(16) 1.94(2) 2.8448(15) 151(2) 4_464
O6 H6b O4 0.993(16) 2.48(2) 3.1589(15) 125(2) 1_454
O7 H7a O2 1.000(15) 1.621(16) 2.6022(13) 166(2) 2_464
O7 H7b O2 0.954(16) 1.78(2) 2.6667(13) 153(3) 1_455

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 O1 S1 O2 68.25(11) . . . . ?
Cu1 O1 S1 O3 -53.00(11) . . . . ?
Cu1 O1 S1 O4 -172.33(10) . . . . ?
Cu1 O3 S1 O1 106.11(9) 2_565 . . . ?
Cu1 O3 S1 O2 -14.15(10) 2_565 . . . ?
Cu1 O3 S1 O4 -136.94(8) 2_565 . . . ?


_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 1.083
_oxdiff_exptl_absorpt_empirical_full_min 0.947
loop_
_restr_distance_atom_site_label_1
_restr_distance_atom_site_label_2
_restr_distance_site_symmetry_2
_restr_distance_target
_restr_distance_target_weight_param
_restr_distance_diff
O5 H5a 1 0.9890 0.0200 -0.0085
O5 H5b 1 0.9890 0.0200 -0.0122
O6 H6a 1 0.9890 0.0200 0.0114
O6 H6b 1 0.9890 0.0200 -0.0040
O7 H7a 1 0.9890 0.0200 -0.0112
O7 H7b 1 0.9890 0.0200 0.0345

loop_
_restr_RIGU_atom_site_label_1
_restr_RIGU_atom_site_label_2
_restr_RIGU_target_weight_param
_restr_RIGU_U13_diff
_restr_RIGU_U23_diff
_restr_RIGU_U33_diff
Cu1 O1 0.004000 0.000753 -0.000984 -0.001350
Cu1 O5 0.004000 0.000455 0.000651 -0.001892
Cu1 H5a 0.004000 0.006659 0.004419 -0.008309
Cu1 H5b 0.004000 0.002034 -0.002009 -0.004535
Cu1 O6 0.004000 0.000121 -0.000536 -0.002007
Cu1 H6a 0.004000 -0.002665 -0.000852 -0.001673
Cu1 H6b 0.004000 -0.008697 -0.002044 -0.010012
Cu1 O7 0.004000 0.000439 0.000175 -0.002096
Cu1 H7a 0.004000 0.002816 -0.000996 -0.005640
Cu1 H7b 0.004000 0.007683 0.006593 -0.009779
Cu1 S1 0.004000 0.000288 -0.000431 0.000014
O1 O2 0.004000 0.003899 0.000536 0.001040
O1 O3 0.004000 -0.002928 -0.004681 0.000289
O1 O4 0.004000 -0.002828 0.001193 -0.000000
O1 O5 0.004000 0.002486 -0.003190 0.000343
O1 O6 0.004000 0.000886 0.000288 -0.000900
O1 O7 0.004000 0.000592 0.003243 0.001268
O1 S1 0.004000 -0.000041 -0.000869 0.000745
O2 O3 0.004000 0.005500 -0.001750 -0.000560
O2 O4 0.004000 0.007905 0.004754 0.000957
O2 S1 0.004000 0.000139 0.000694 0.000179
O3 O4 0.004000 -0.000594 -0.003777 -0.000110
O3 S1 0.004000 0.000717 0.000069 0.000847
O4 S1 0.004000 0.001010 0.000179 0.000579
O5 H5a 0.004000 -0.000997 -0.000573 -0.003269
O5 H5b 0.004000 0.000995 0.002066 -0.000688
O5 O6 0.004000 0.000767 -0.002386 0.000131
O5 O7 0.004000 0.000794 -0.000536 -0.000189
H5a H5b 0.004000 0.006300 0.001524 -0.000466
O6 H6a 0.004000 -0.000852 0.000561 -0.002385
O6 H6b 0.004000 -0.001540 0.002859 -0.000835
O6 O7 0.004000 -0.000712 -0.001589 0.000065
H6a H6b 0.004000 -0.007205 0.003905 -0.001375
O7 H7a 0.004000 0.000630 0.001409 -0.001713
O7 H7b 0.004000 -0.002300 -0.001076 -0.002883
H7a H7b 0.004000 0.000991 -0.007375 -0.001196

loop_
_restr_U_iso_atom_site_label
_restr_U_iso_weight_param
H6a 0.0200
H7b 0.0200
####################################################################### 
# 
# 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_RB21080ai2f
_database_code_depnum_ccdc_archive 'CCDC 2133583'
loop_
_audit_author_name
_audit_author_address
'Rene Boere'
;University of Lethbridge
Canada
;
_audit_update_record             
;
2022-01-28 deposited with the CCDC.	2022-02-02 downloaded from the CCDC.
;
_audit_creation_date             2022-01-28
_audit_creation_method           
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_chemical_formula_moiety         'Cu H2 O5 S'
_chemical_formula_sum            'Cu H2 O5 S'
_chemical_formula_weight         177.625
_chemical_oxdiff_formula         'Cu H2 O5 S'
_chemical_oxdiff_usercomment     'Prism from H2SO4'
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
_atom_type_scat_dispersion_source
Cu -1.96878 0.60861 'NoSpherA2: Chem.Sci. 2021, DOI:10.1039/D0SC05526C'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
H 0.00000 0.00000 'NoSpherA2: Chem.Sci. 2021, DOI:10.1039/D0SC05526C'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
O 0.05239 0.03377 'NoSpherA2: Chem.Sci. 2021, DOI:10.1039/D0SC05526C'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
S 0.33537 0.55136 'NoSpherA2: Chem.Sci. 2021, DOI:10.1039/D0SC05526C'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'

_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_id
_space_group_symop_operation_xyz
1 x,y,z
2 -x,-y,-z

_symmetry_Int_Tables_number      2
_cell_length_a                   5.0281(5)
_cell_length_b                   5.1502(5)
_cell_length_c                   7.5607(9)
_cell_angle_alpha                108.592(12)
_cell_angle_beta                 108.382(12)
_cell_angle_gamma                91.359(10)
_cell_volume                     174.41(4)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    2958
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      79.9930
_cell_measurement_theta_min      9.1490
_exptl_absorpt_coefficient_mu    13.717
_exptl_absorpt_correction_T_max  0.822
_exptl_absorpt_correction_T_min  0.302
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.116a (Rigaku Oxford Diffraction, 2021)
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_crystal_colour            'clear light blue'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    3.382
_exptl_crystal_description       prism
_exptl_crystal_F_000             171.290
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 1 -1 0.0341
0 -1 1 0.0261
-3 0 4 0.0447
1 0 -1 0.0684
-1 0 0 0.0489
1 0 0 0.0653
0 0 -1 0.0154
0 0 1 0.0120
0 1 0 0.0262
0 -1 0 0.0264

_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.027
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
0.0002 0.9989 -0.9993 0.2765 -0.1627 0.0233
-0.0002 -0.9989 0.9993 -0.2765 0.1627 -0.0233
-2.8135 -0.0051 3.5821 -0.6759 -0.7127 0.1876
1.0013 0.0010 -1.0016 0.2043 0.2316 -0.1126
-0.6680 -0.3336 0.3344 -0.1404 -0.0461 0.1793
0.6680 0.3336 -0.3344 0.1404 0.0461 -0.1793
-0.0006 0.0001 -0.9996 0.1321 0.0811 0.1680
0.0006 -0.0001 0.9996 -0.1321 -0.0811 -0.1680
0.0008 0.9988 0.0003 0.1445 -0.2438 -0.1447
-0.0008 -0.9988 -0.0003 -0.1445 0.2438 0.1447

_diffrn_reflns_av_R_equivalents  0.0399
_diffrn_reflns_av_unetI/netI     0.0243
_diffrn_reflns_Laue_measured_fraction_full 0.9857
_diffrn_reflns_Laue_measured_fraction_max 0.9690
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            3078
_diffrn_reflns_point_group_measured_fraction_full 0.9857
_diffrn_reflns_point_group_measured_fraction_max 0.9690
_diffrn_reflns_theta_full        67.6840
_diffrn_reflns_theta_max         80.33
_diffrn_reflns_theta_min         6.57
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 5.8140
_diffrn_detector_type            'Pilatus 200K'
_diffrn_measured_fraction_theta_full 0.9857
_diffrn_measured_fraction_theta_max 0.9690
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -102.00 -20.00   0.50    0.50    --  -38.50 -70.00 -29.11  164
  2  ω    -50.00  25.00   0.50    0.50    --  -38.50  57.00-120.00  150
  3  ω    -50.00  25.00   0.50    0.50    --  -38.50  57.00 120.00  150
  4  ω     27.00  99.00   0.50    0.50    --   47.56-125.00  30.00  144
  5  ω     36.00 111.00   0.50    0.50    --   47.56  57.00   0.00  150
  6  ω     47.00 117.00   0.50    0.50    --  111.00 -50.00  30.00  140
  7  ω     41.00 109.00   0.50    0.50    --  111.00-111.00 120.00  136
  8  ω    107.00 178.00   0.50    0.50    --  111.00  25.00  30.00  142
  9  ω     41.00 109.00   0.50    0.50    --  111.00-111.00-120.00  136
 10  ω    103.00 176.00   0.50    0.50    --  111.00  77.00 -30.00  146
 11  ω    105.00 175.00   0.50    0.50    --  111.00  50.00-120.00  140
 12  ω     41.00 107.00   0.50    0.50    --  111.00 -91.00 -90.00  132
 13  ω    103.00 176.00   0.50    0.50    --  111.00  77.00 -60.00  146
 14  ω     41.00 109.00   0.50    0.50    --  111.00-111.00 -90.00  136
 15  ω     41.00 107.00   0.50    0.50    --  111.00 -91.00 -30.00  132
 16  ω     41.00 107.00   0.50    0.50    --  111.00 -91.00 150.00  132
 17  ω    105.00 175.00   0.50    0.50    --  111.00  50.00   0.00  140
 18  ω    107.00 177.00   0.50    0.50    --  111.00  38.00  30.00  140
 19  ω    107.00 177.00   0.50    0.50    --  111.00  38.00  60.00  140
 20  ω     41.00 107.00   0.50    0.50    --  111.00 -91.00 -60.00  132
 21  ω     41.00 107.00   0.50    0.50    --  111.00 -91.00  30.00  132
 22  ω    107.00 177.00   0.50    0.50    --  111.00  38.00 -90.00  140
 23  ω     61.00 146.00   0.50    0.50    --  111.00 178.00 -90.00  170
 24  ω    107.00 178.00   0.50    0.50    --  111.00  25.00  90.00  142
 25  ω     46.00 134.00   0.50    0.50    --  111.00 -77.00-180.00  176
 26  ω     47.00 117.00   0.50    0.50    --  111.00 -50.00 -60.00  140
 27  ω     46.00 134.00   0.50    0.50    --  111.00 -77.00 -60.00  176
 28  ω     41.00 107.00   0.50    0.50    --  111.00 -91.00  90.00  132
 29  ω     45.00 115.00   0.50    0.50    --  111.00 -38.00-124.90  140
 30  ω   -102.00 -27.00   0.50    0.50    --  -38.50 -57.00-120.00  150
 31  ω   -102.00 -20.00   0.50    0.50    --  -38.50 -71.00-122.76  164
 32  ω     36.00 111.00   0.50    0.50    --   47.56  57.00 120.00  150
 33  ω     36.00 111.00   0.50    0.50    --   47.56  57.00  60.00  150
 34  ω     36.00 111.00   0.50    0.50    --   47.56  57.00-150.00  150
 35  ω     36.00 111.00   0.50    0.50    --   47.56  57.00 150.00  150
 36  ω     42.00 117.00   0.50    0.50    --   47.56  19.00-120.00  150
 37  ω    105.00 175.00   0.50    0.50    --  111.00  50.00 120.00  140
 38  ω     41.00 115.00   0.50    0.50    --  111.00 -25.00 -60.00  148
 39  ω    107.00 177.00   0.50    0.50    --  111.00  38.00 150.00  140
 40  ω    105.00 175.00   0.50    0.50    --  111.00  50.00 -60.00  140
 41  ω    107.00 177.00   0.50    0.50    --  111.00  38.00-150.00  140
 42  ω    107.00 178.00   0.50    0.50    --  111.00  25.00 120.00  142
 43  ω     99.00 174.00   0.50    0.50    --  111.00  57.00 -77.00  150
 44  ω     96.00 174.00   0.50    0.50    --  111.00  63.00 -30.00  156
 45  ω     96.00 174.00   0.50    0.50    --  111.00  63.00-150.00  156
 46  ω     96.00 174.00   0.50    0.50    --  111.00  63.00  30.00  156
 47  ω    107.00 178.00   0.50    0.50    --  111.00  25.00-180.00  142
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  
'SuperNova, Dual, Cu at home/near, Pilatus 200K'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0717360000
_diffrn_orient_matrix_UB_12      0.1446468000
_diffrn_orient_matrix_UB_13      -0.1321430000
_diffrn_orient_matrix_UB_21      0.1502716000
_diffrn_orient_matrix_UB_22      -0.2442468000
_diffrn_orient_matrix_UB_23      -0.0812762000
_diffrn_orient_matrix_UB_31      -0.2802666000
_diffrn_orient_matrix_UB_32      -0.1446397000
_diffrn_orient_matrix_UB_33      -0.1679531000
_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         0.0
_reflns_limit_h_max              6
_reflns_limit_h_min              -6
_reflns_limit_k_max              6
_reflns_limit_k_min              -6
_reflns_limit_l_max              9
_reflns_limit_l_min              0
_reflns_number_gt                736
_reflns_number_total             751
_reflns_threshold_expression     I>=2u(I)
_computing_cell_refinement       'CrysAlisPro 1.171.41.116a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.116a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.116a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.5 (Bourhis et al., 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         2.4945
_refine_diff_density_min         -1.4795
_refine_diff_density_rms         0.4254
_refine_ls_d_res_high            0.7820
_refine_ls_d_res_low             6.7372
_refine_ls_goodness_of_fit_ref   1.0366
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    2
_refine_ls_number_parameters     73
_refine_ls_number_reflns         751
_refine_ls_number_restraints     32
_refine_ls_R_factor_all          0.0759
_refine_ls_R_factor_gt           0.0753
_refine_ls_restrained_S_all      1.0130
_refine_ls_shift/su_max          0.0001
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1207P)²+6.9086P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2174
_refine_ls_wR_factor_ref         0.2178
_refine_special_details          
;Refinement using NoSpherA2, an implementation of
NOn-SPHERical Atom-form-factors in Olex2.
Please cite:
F. Kleemiss et al. Chem. Sci. DOI 10.1039/D0SC05526C - 2021
NoSpherA2 implementation of HAR makes use of
tailor-made aspherical atomic form factors calculated
on-the-fly from a Hirshfeld-partitioned electron density (ED) - not from
spherical-atom form factors.

The ED is calculated from a gaussian basis set single determinant SCF
wavefunction - either Hartree-Fock or DFT using selected funtionals
 - for a fragment of the crystal.
This fragment can be embedded in an electrostatic crystal field by employing cluster charges
or modelled using implicit solvation models, depending on the software used.
The following options were used:
   SOFTWARE:       ORCA 5.0
   PARTITIONING:   NoSpherA2
   INT ACCURACY:   Normal
   METHOD:         B3LYP
   BASIS SET:      6-31G(d,p)
   CHARGE:         -10
   MULTIPLICITY:   3
   DATE:           2021-12-25_22-16-14,Hirsfeld Atom Refinement
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All O(H,H) groups
2. Restrained distances
 O1-H1a = O1-H1b
 0.989 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O1) \\sim Ueq, Uanis(O2) \\sim Ueq, Uanis(O5) \\sim Ueq, Uanis(O3) \\sim
Ueq, Uanis(O4) \\sim Ueq: with sigma of 0.05 and sigma for terminal atoms of
0.001
4. Rigid body (RIGU) restrains
 S1, Cu2, Cu1
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
;
_atom_sites_solution_primary     dual
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_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
Cu1 Cu 0.5 0.5 0.5 0.0116(6) Uani 1.000000 2 S TU P
Cu2 Cu 0.0 0.0 0.0 0.0110(6) Uani 1.000000 2 S TU P
S1 S 0.3916(4) 1.0745(4) 0.7526(3) 0.0106(6) Uani 1.000000 1 . U .
O1 O 0.1374(14) 0.4397(14) 0.2702(9) 0.0129(13) Uani 1.000000 1 D U .
H1a H 0.21(3) 0.58(2) 0.23(2) 0.0155(16) Uiso 1.000000 1 DR . .
H1b H -0.045(18) 0.43(3) 0.29(2) 0.0155(16) Uiso 1.000000 1 DR . .
O2 O 0.3361(14) 0.7703(13) 0.6711(10) 0.0140(13) Uani 1.000000 1 . U .
O3 O 0.7043(13) 1.1635(13) 0.8517(10) 0.0130(13) Uani 1.000000 1 . U .
O4 O 0.2528(14) 1.1710(14) 0.9026(10) 0.0142(13) Uani 1.000000 1 . U .
O5 O 0.2937(14) 1.1969(14) 0.5993(10) 0.0140(13) Uani 1.000000 1 . U .


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 2.018(6) 2_666 ?
Cu1 O1 2.018(6) . ?
Cu1 O2 1.967(6) . ?
Cu1 O2 1.967(6) 2_666 ?
Cu1 O5 2.289(6) 2_676 ?
Cu1 O5 2.289(6) 1_545 ?
Cu2 O1 2.422(7) 2 ?
Cu2 O1 2.422(7) . ?
Cu2 O3 1.946(6) 2_666 ?
Cu2 O3 1.946(6) 1_444 ?
Cu2 O4 1.971(6) 2_566 ?
Cu2 O4 1.971(6) 1_544 ?
S1 O2 1.472(7) . ?
S1 O3 1.499(7) . ?
S1 O4 1.476(7) . ?
S1 O5 1.450(7) . ?
O1 H1a 0.992(19) . ?
O1 H1b 0.992(19) . ?

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 2_666 . ?
O2 Cu1 O1 89.0(3) . . ?
O2 Cu1 O1 91.0(3) . 2_666 ?
O2 Cu1 O1 91.0(3) 2_666 . ?
O2 Cu1 O1 89.0(3) 2_666 2_666 ?
O2 Cu1 O2 180.0 2_666 . ?
O5 Cu1 O1 89.1(2) 1_545 . ?
O5 Cu1 O1 89.1(2) 2_676 2_666 ?
O5 Cu1 O1 90.9(2) 2_676 . ?
O5 Cu1 O1 90.9(2) 1_545 2_666 ?
O5 Cu1 O2 82.5(3) 1_545 . ?
O5 Cu1 O2 82.5(3) 2_676 2_666 ?
O5 Cu1 O2 97.5(3) 2_676 . ?
O5 Cu1 O2 97.5(3) 1_545 2_666 ?
O5 Cu1 O5 180.0 2_676 1_545 ?
O1 Cu2 O1 180.0 2 . ?
O3 Cu2 O1 91.4(2) 2_666 . ?
O3 Cu2 O1 88.6(2) 2_666 2 ?
O3 Cu2 O1 88.6(2) 1_444 . ?
O3 Cu2 O1 91.4(2) 1_444 2 ?
O3 Cu2 O3 180.0 2_666 1_444 ?
O4 Cu2 O1 83.0(2) 1_544 . ?
O4 Cu2 O1 97.0(2) 1_544 2 ?
O4 Cu2 O1 97.0(2) 2_566 . ?
O4 Cu2 O1 83.0(2) 2_566 2 ?
O4 Cu2 O3 85.5(3) 1_544 1_444 ?
O4 Cu2 O3 85.5(3) 2_566 2_666 ?
O4 Cu2 O3 94.5(3) 1_544 2_666 ?
O4 Cu2 O3 94.5(3) 2_566 1_444 ?
O4 Cu2 O4 180.0 2_566 1_544 ?
O3 S1 O2 109.1(4) . . ?
O4 S1 O2 108.2(4) . . ?
O4 S1 O3 108.8(4) . . ?
O5 S1 O2 112.1(4) . . ?
O5 S1 O3 107.8(4) . . ?
O5 S1 O4 110.9(4) . . ?
Cu2 O1 Cu1 119.4(3) . . ?
H1a O1 Cu1 92(9) . . ?
H1a O1 Cu2 110(9) . . ?
H1b O1 Cu1 119(10) . . ?
H1b O1 Cu2 93(10) . . ?
H1b O1 H1a 125(13) . . ?
S1 O2 Cu1 130.9(4) . . ?
S1 O3 Cu2 131.6(4) . 2_666 ?
S1 O4 Cu2 136.3(4) . 1_566 ?
S1 O5 Cu1 134.7(4) . 1_565 ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1 H1a O3 0.992(19) 1.70(3) 2.692(9) 173(14) 2_676
O1 H1b O2 0.992(19) 1.91(9) 2.808(9) 150(14) 2_566
O1 H1b O5 0.992(19) 2.38(13) 3.088(9) 128(12) 2_576

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 O2 S1 O3 -50.9(6) . . . . ?
Cu1 O2 S1 O3 -50.9(6) 2_666 . . . ?
Cu1 O2 S1 O4 -169.0(5) . . . . ?
Cu1 O2 S1 O4 -169.0(5) 2_666 . . . ?
Cu1 O2 S1 O5 68.4(6) . . . . ?
Cu1 O2 S1 O5 68.4(6) 2_666 . . . ?
Cu1 O5 S1 O2 -124.8(5) 1_565 . . . ?
Cu1 O5 S1 O2 -124.8(5) 2_676 . . . ?
Cu1 O5 S1 O3 -4.8(6) 1_565 . . . ?
Cu1 O5 S1 O3 -4.8(6) 2_676 . . . ?
Cu1 O5 S1 O4 114.2(6) 1_565 . . . ?
Cu1 O5 S1 O4 114.2(6) 2_676 . . . ?
Cu2 O3 S1 O2 -34.5(6) 1_666 . . . ?
Cu2 O3 S1 O2 -34.5(6) 2_666 . . . ?
Cu2 O3 S1 O4 83.2(6) 1_666 . . . ?
Cu2 O3 S1 O4 83.2(6) 2_666 . . . ?
Cu2 O3 S1 O5 -156.4(5) 1_666 . . . ?
Cu2 O3 S1 O5 -156.4(5) 2_666 . . . ?
Cu2 O4 S1 O2 -5.6(7) 1_566 . . . ?
Cu2 O4 S1 O2 -5.6(7) 2_566 . . . ?
Cu2 O4 S1 O3 -123.9(6) 2_566 . . . ?
Cu2 O4 S1 O3 -123.9(6) 1_566 . . . ?
Cu2 O4 S1 O5 117.8(6) 2_566 . . . ?
Cu2 O4 S1 O5 117.8(6) 1_566 . . . ?

_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2

_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 1.403
_oxdiff_exptl_absorpt_empirical_full_min 0.760
loop_
_restr_distance_atom_site_label_1
_restr_distance_atom_site_label_2
_restr_distance_site_symmetry_2
_restr_distance_target
_restr_distance_target_weight_param
_restr_distance_diff
O1 H1a 1 0.9890 0.0200 -0.0029
O1 H1b 1 0.9890 0.0200 -0.0026

loop_
_restr_U_iso_atom_site_label
_restr_U_iso_weight_param
O1 0.0500
O2 0.0500
O3 0.0010
O4 0.0010
O5 0.0010

_vrf_PLAT430_RB21080ai2f         
;
PROBLEM: Short Inter D...A Contact O3 ..O4 . 2.66 Ang.
RESPONSE: Sulfate O3 coordinates to Cu2(1+x,1+y,1+z)
with a short Cu-O distance of 1.946 A, and O4(1+x,y,z)
is the second short Cu-O ligand to this same Cu, at 
1.971 A. The appartent short contact is therefore just
a shared set of equatorial O donors to the same metal. 
;
####################################################################### 
# 
# 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_RB21097if
_database_code_depnum_ccdc_archive 'CCDC 2133582'
loop_
_audit_author_name
_audit_author_address
'Rene Boere'
;University of Lethbridge
Canada
;
_audit_update_record             
;
2022-01-10 deposited with the CCDC.	2022-02-02 downloaded from the CCDC.
;
_audit_creation_date             2022-01-07
_audit_creation_method           
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_chemical_formula_moiety         'Cu O4 S'
_chemical_formula_sum            'Cu O4 S'
_chemical_formula_weight         159.609
_chemical_oxdiff_formula         'Cu S O4'
_chemical_oxdiff_usercomment     
'Small  prism grown from (NH4)2SO4/H2SO4 X = 0.2'
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
_atom_type_scat_dispersion_source
Cu 0.34125 1.28947 'NoSpherA2: Chem.Sci. 2021, DOI:10.1039/D0SC05526C'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
O 0.01158 0.00611 'NoSpherA2: Chem.Sci. 2021, DOI:10.1039/D0SC05526C'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
S 0.12424 0.12443 'NoSpherA2: Chem.Sci. 2021, DOI:10.1039/D0SC05526C'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_H-M_alt        'P n m a'
_space_group_name_Hall           '-P 2ac 2n'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 x,y,z
2 x+1/2,-y+1/2,-z+1/2
3 -x,y+1/2,-z
4 -x+1/2,-y,z+1/2
5 -x,-y,-z
6 -x-1/2,y-1/2,z-1/2
7 x,-y-1/2,z
8 x-1/2,y,-z-1/2

_symmetry_Int_Tables_number      62
_cell_length_a                   8.3958(6)
_cell_length_b                   6.6760(4)
_cell_length_c                   4.8270(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     270.56(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    2493
_cell_measurement_temperature    100.0(3)
_cell_measurement_theta_max      38.1800
_cell_measurement_theta_min      4.8190
_exptl_absorpt_coefficient_mu    8.637
_exptl_absorpt_correction_T_max  0.785
_exptl_absorpt_correction_T_min  0.524
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.116a (Rigaku Oxford Diffraction, 2021)
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_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    3.918
_exptl_crystal_description       prism
_exptl_crystal_F_000             310.162
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 1 0 0.0355
0 -1 0 0.0505
-1 0 -1 0.0169
1 0 1 0.0201
1 0 -1 0.0170
-1 0 1 0.0233
1 0 0 0.0215
-1 0 0 0.0208

_exptl_crystal_size_max          0.09
_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
-0.0019 0.9994 -0.0004 0.0472 0.0804 0.0507
0.0019 -0.9994 0.0004 -0.0472 -0.0804 -0.0507
-0.9984 -0.0013 -0.9991 0.1510 -0.0713 -0.0272
0.9984 0.0013 0.9991 -0.1510 0.0713 0.0272
0.9995 -0.0005 -0.9976 0.0642 -0.1085 0.1128
-0.9995 0.0005 0.9976 -0.0642 0.1085 -0.1128
0.9990 0.0004 0.0007 -0.0434 -0.0186 0.0700
-0.9990 -0.0004 -0.0007 0.0434 0.0186 -0.0700

_diffrn_reflns_av_R_equivalents  0.0344
_diffrn_reflns_av_unetI/netI     0.0251
_diffrn_reflns_Laue_measured_fraction_full 1.0000
_diffrn_reflns_Laue_measured_fraction_max 0.9295
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            3682
_diffrn_reflns_point_group_measured_fraction_full 1.0000
_diffrn_reflns_point_group_measured_fraction_max 0.9295
_diffrn_reflns_theta_full        25.2417
_diffrn_reflns_theta_max         38.09
_diffrn_reflns_theta_min         4.86
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.0(3)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 5.8140
_diffrn_detector_type            'Pilatus 200K'
_diffrn_measured_fraction_theta_full 1.0000
_diffrn_measured_fraction_theta_max 0.9295
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     37.00  91.00   0.50    5.73    --   22.41-178.00   0.00  108
  2  ω    -44.00  26.00   0.50    5.73    --   22.41 -38.00-180.00  140
  3  ω     39.00  91.00   0.50    5.73    --   22.41 178.00 150.00  104
  4  ω    -92.00 -22.00   0.50    5.73    --  -25.54 -38.00-150.00  140
  5  ω    -92.00 -22.00   0.50    5.73    --  -25.54 -38.00 -60.00  140
  6  ω    -89.00 -14.00   0.50    5.73    --  -25.54 -57.00  90.00  150
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  
'SuperNova, Dual, Cu at home/near, Pilatus 200K'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0433904000
_diffrn_orient_matrix_UB_12      0.0470898000
_diffrn_orient_matrix_UB_13      -0.1078525000
_diffrn_orient_matrix_UB_21      -0.0187158000
_diffrn_orient_matrix_UB_22      0.0804924000
_diffrn_orient_matrix_UB_23      0.0899959000
_diffrn_orient_matrix_UB_31      0.0700919000
_diffrn_orient_matrix_UB_32      0.0508926000
_diffrn_orient_matrix_UB_33      -0.0428774000
_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         0.0
_reflns_limit_h_max              14
_reflns_limit_h_min              0
_reflns_limit_k_max              11
_reflns_limit_k_min              0
_reflns_limit_l_max              8
_reflns_limit_l_min              0
_reflns_number_gt                653
_reflns_number_total             738
_reflns_threshold_expression     I>=2u(I)
_computing_cell_refinement       'CrysAlisPro 1.171.41.116a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.116a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.116a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.5 (Bourhis et al., 2015)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_refine_diff_density_max         0.6089
_refine_diff_density_min         -1.0296
_refine_diff_density_rms         0.1972
_refine_ls_d_res_high            0.5760
_refine_ls_d_res_low             4.1979
_refine_ls_goodness_of_fit_ref   1.0215
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     34
_refine_ls_number_reflns         738
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0235
_refine_ls_R_factor_gt           0.0205
_refine_ls_restrained_S_all      1.0215
_refine_ls_shift/su_max          -0.0002
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0296P)²+0.0357P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0520
_refine_ls_wR_factor_ref         0.0535
_refine_special_details          
;Refinement using NoSpherA2, an implementation of
NOn-SPHERical Atom-form-factors in Olex2.
Please cite:
F. Kleemiss et al. Chem. Sci. DOI 10.1039/D0SC05526C - 2021
NoSpherA2 implementation of HAR makes use of
tailor-made aspherical atomic form factors calculated
on-the-fly from a Hirshfeld-partitioned electron density (ED) - not from
spherical-atom form factors.

The ED is calculated from a gaussian basis set single determinant SCF
wavefunction - either Hartree-Fock or DFT using selected funtionals
 - for a fragment of the crystal.
This fragment can be embedded in an electrostatic crystal field by employing cluster charges
or modelled using implicit solvation models, depending on the software used.
The following options were used:
   SOFTWARE:       ORCA 5.0
   PARTITIONING:   NoSpherA2
   INT ACCURACY:   Normal
   METHOD:         B3LYP
   BASIS SET:      def2-SVP
   CHARGE:         0
   MULTIPLICITY:   2
   DATE:           2021-12-18_23-43-40,Refinement with NoSpherA2
;
_olex2_refinement_description    
;
1. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
;
_atom_sites_solution_primary     heavy
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_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
Cu Cu 0.0 0.0 0.0 0.00364(7) Uani 1.000000 2 S TU P
S S 0.18370(5) 0.25 0.45155(8) 0.00240(8) Uani 1.000000 2 S TU P
O1 O 0.13062(14) 0.25 0.7388(2) 0.0052(2) Uani 1.000000 2 S TU P
O2 O 0.36421(14) 0.25 0.4379(3) 0.0041(2) Uani 1.000000 2 S TU P
O3 O 0.13217(9) 0.06669(12) 0.31105(18) 0.00494(15) Uani 1.000000 1 . U .


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
Cu O1 2.3618(8) 3_546 ?
Cu O1 2.3618(8) 1_554 ?
Cu O2 2.0433(7) 2_455 ?
Cu O2 2.0433(7) 4_554 ?
Cu O3 1.9194(8) 5 ?
Cu O3 1.9194(8) . ?
S O1 1.4563(12) . ?
S O2 1.5170(12) . ?
S O3 1.4645(8) . ?
S O3 1.4645(8) 7_565 ?

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 Cu O1 180.0 3_546 1_554 ?
O2 Cu O1 76.13(3) 2_455 1_554 ?
O2 Cu O1 103.87(3) 2_455 3_546 ?
O2 Cu O1 103.87(3) 4_554 1_554 ?
O2 Cu O1 76.13(3) 4_554 3_546 ?
O2 Cu O2 180.0 4_554 2_455 ?
O3 Cu O1 90.84(4) . 3_546 ?
O3 Cu O1 89.16(4) . 1_554 ?
O3 Cu O1 89.16(4) 5 3_546 ?
O3 Cu O1 90.84(4) 5 1_554 ?
O3 Cu O2 88.95(4) 5 2_455 ?
O3 Cu O2 91.05(4) . 2_455 ?
O3 Cu O2 88.95(4) . 4_554 ?
O3 Cu O2 91.05(4) 5 4_554 ?
O3 Cu O3 180.0 5 . ?
O2 S O1 110.31(7) . . ?
O3 S O1 110.52(4) . . ?
O3 S O1 110.52(4) 7_565 . ?
O3 S O2 105.96(4) 7_565 . ?
O3 S O2 105.96(4) . . ?
O3 S O3 113.36(7) 7_565 . ?
Cu O1 Cu 89.93(4) 3_556 1_556 ?
S O1 Cu 130.57(3) . 1_556 ?
S O1 Cu 130.57(3) . 3_556 ?
Cu O2 Cu 109.53(5) 4 2 ?
S O2 Cu 123.44(3) . 2 ?
S O2 Cu 123.44(3) . 4 ?
S O3 Cu 136.63(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
Cu O1 S O2 -111.52(7) 1_556 . . . ?
Cu O1 S O2 111.52(7) 3_556 . . . ?
Cu O1 S O3 131.63(7) 1_556 . . 7_565 ?
Cu O1 S O3 5.32(9) 1_556 . . . ?
Cu O1 S O3 -131.63(7) 3_556 . . . ?
Cu O1 S O3 -5.32(9) 3_556 . . 7_565 ?
Cu O2 S O1 -78.18(7) 2 . . . ?
Cu O2 S O1 78.18(7) 4 . . . ?
Cu O2 S O3 41.46(9) 2 . . 7_565 ?
Cu O2 S O3 -41.46(9) 4 . . . ?
Cu O2 S O3 162.18(7) 2 . . . ?
Cu O2 S O3 -162.18(7) 4 . . 7_565 ?
Cu O3 S O1 119.13(8) . . . . ?
Cu O3 S O1 119.13(8) 5 . . . ?
Cu O3 S O2 -121.37(8) 5 . . . ?
Cu O3 S O2 -121.37(8) . . . . ?
Cu O3 S O3 -5.57(5) 5 . . 7_565 ?
Cu O3 S O3 -5.57(5) . . . 7_565 ?


_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 1.283
_oxdiff_exptl_absorpt_empirical_full_min 0.853
####################################################################### 
# 
# 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_RB21086i
_database_code_depnum_ccdc_archive 'CCDC 2133584'
loop_
_audit_author_name
_audit_author_address
'Rene Boere'
;University of Lethbridge
Canada
;
_audit_update_record             
;
2022-01-10 deposited with the CCDC.	2022-02-02 downloaded from the CCDC.
;
_audit_creation_date             2022-01-08
_audit_creation_method           
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_chemical_formula_moiety         'Cu H8 O8 S, H2 O'
_chemical_formula_sum            'Cu H10 O9 S'
_chemical_formula_weight         249.686
_chemical_oxdiff_formula         'Cu C O9 H10'
_chemical_oxdiff_usercomment     Mo
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
_atom_type_scat_dispersion_source
Cu 0.34125 1.28947 'NoSpherA2: Chem.Sci. 2021, DOI:10.1039/D0SC05526C'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
H 0.00000 0.00000 'NoSpherA2: Chem.Sci. 2021, DOI:10.1039/D0SC05526C'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
O 0.01158 0.00611 'NoSpherA2: Chem.Sci. 2021, DOI:10.1039/D0SC05526C'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
S 0.12424 0.12443 'NoSpherA2: Chem.Sci. 2021, DOI:10.1039/D0SC05526C'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'

_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_id
_space_group_symop_operation_xyz
1 x,y,z
2 -x,-y,-z

_symmetry_Int_Tables_number      2
_cell_length_a                   5.9676(2)
_cell_length_b                   6.0957(2)
_cell_length_c                   10.6366(3)
_cell_angle_alpha                77.224(3)
_cell_angle_beta                 82.387(2)
_cell_angle_gamma                72.434(3)
_cell_volume                     358.85(2)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    10138
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      38.2480
_cell_measurement_theta_min      3.5350
_exptl_absorpt_coefficient_mu    3.350
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.91744
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.116a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear blue'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    2.311
_exptl_crystal_description       irregular
_exptl_crystal_F_000             255.197
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 -1 -1 0.0866
0 1 0 0.0696
0 -1 0 0.0904
-1 0 1 0.1074
1 0 -1 0.0985
0 -1 1 0.1088
0 1 -1 0.0644
1 0 1 0.0694
-1 0 -1 0.0918
1 1 1 0.0760
0 0 1 0.0794
0 0 -1 0.0638
-1 -1 -1 0.0599
1 1 2 0.0601
1 -1 0 0.0918

_exptl_crystal_size_max          0.222
_exptl_crystal_size_mid          0.173
_exptl_crystal_size_min          0.135
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
-0.0010 -0.9995 -1.0005 0.1291 0.0066 -0.0127
0.0010 1.0000 0.0014 -0.1084 -0.0468 -0.0387
-0.0010 -1.0000 -0.0014 0.1084 0.0468 0.0387
-0.9992 0.0002 0.9995 -0.0469 -0.0554 0.1274
0.9992 -0.0002 -0.9995 0.0469 0.0554 -0.1274
-0.0010 -1.0004 0.9977 0.0878 0.0870 0.0902
0.0010 1.0004 -0.9977 -0.0878 -0.0870 -0.0902
0.9992 -0.0010 0.9987 0.0055 0.1358 -0.0245
-0.9992 0.0010 -0.9987 -0.0055 -0.1358 0.0245
1.0002 0.9989 1.0001 -0.1029 0.0890 -0.0633
-0.0000 -0.0004 0.9991 -0.0207 0.0402 0.0514
0.0000 0.0004 -0.9991 0.0207 -0.0402 -0.0514
-1.0002 -0.9989 -1.0001 0.1029 -0.0890 0.0633
1.0002 0.9985 1.9992 -0.1236 0.1293 -0.0118
0.9982 -1.0006 -0.0018 0.1346 0.1424 -0.0373

_diffrn_reflns_av_R_equivalents  0.0463
_diffrn_reflns_av_unetI/netI     0.0349
_diffrn_reflns_Laue_measured_fraction_full 0.9992
_diffrn_reflns_Laue_measured_fraction_max 0.9344
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            18712
_diffrn_reflns_point_group_measured_fraction_full 0.9992
_diffrn_reflns_point_group_measured_fraction_max 0.9344
_diffrn_reflns_theta_full        25.2417
_diffrn_reflns_theta_max         38.30
_diffrn_reflns_theta_min         3.57
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 5.8140
_diffrn_detector_type            'Pilatus 200K'
_diffrn_measured_fraction_theta_full 0.9992
_diffrn_measured_fraction_theta_max 0.9344
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     37.00  91.00   0.50    0.66    --   22.41-178.00   0.00  108
  2  ω     39.00  91.00   0.50    0.66    --   22.41 178.00  60.00  104
  3  ω    -29.00  41.00   0.50    0.66    --  -25.54  38.00  90.00  140
  4  ω    -77.00 -27.00   0.50    0.66    --  -25.54 125.00 -92.32  100
  5  ω    -36.00  -6.00   0.50    0.66    --  -25.54 -73.00  21.11   60
  6  ω    -95.00  44.00   0.50    0.66    --  -25.54   0.00 -90.00  278
  7  ω    -89.00 -37.00   0.50    0.66    --  -25.54 145.00  66.26  104
  8  ω    -37.00  38.00   0.50    0.66    --  -25.54  57.00  30.00  150
  9  ω    -23.00   7.00   0.50    0.66    --  -25.54 -92.00 -52.16   60
 10  ω    -14.00  13.00   0.50    0.66    --  -25.54-104.00-178.69   54
 11  ω    -81.00 -30.00   0.50    0.66    --  -25.54 132.00 107.74  102
 12  ω    -24.00   6.00   0.50    0.66    --  -25.54 -91.00-168.86   60
 13  ω    -95.00  44.00   0.50    0.66    --  -25.54   0.00 -90.00  278
 14  ω    -89.00 -14.00   0.50    0.66    --  -25.54 -57.00 120.00  150
 15  ω    -92.00 -22.00   0.50    0.66    --  -25.54 -38.00 -90.00  140
 16  ω    -14.00  13.00   0.50    0.66    --  -25.54-104.00 -16.30   54
 17  ω    -89.00 -14.00   0.50    0.66    --  -25.54 -57.00  60.00  150
 18  ω    -89.00 -14.00   0.50    0.66    --  -25.54 -57.00-180.00  150
 19  ω    -49.00  21.00   0.50    0.66    --  -25.54  77.00-150.00  140
 20  ω    -90.00 -37.00   0.50    0.66    --  -25.54 146.00 -14.46  106
 21  ω    -92.00 -37.00   0.50    0.66    --  -25.54 -38.00-120.00  110
 22  ω    -36.00  -6.00   0.50    0.66    --  -25.54 -72.00-131.33   60
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  
'SuperNova, Dual, Cu at home/near, Pilatus 200K'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0261332000
_diffrn_orient_matrix_UB_12      -0.1084481000
_diffrn_orient_matrix_UB_13      -0.0207348000
_diffrn_orient_matrix_UB_21      0.0956846000
_diffrn_orient_matrix_UB_22      -0.0469526000
_diffrn_orient_matrix_UB_23      0.0402417000
_diffrn_orient_matrix_UB_31      -0.0760451000
_diffrn_orient_matrix_UB_32      -0.0387255000
_diffrn_orient_matrix_UB_33      0.0514748000
_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         0.0
_reflns_limit_h_max              10
_reflns_limit_h_min              -9
_reflns_limit_k_max              10
_reflns_limit_k_min              -10
_reflns_limit_l_max              18
_reflns_limit_l_min              0
_reflns_number_gt                3369
_reflns_number_total             3729
_reflns_threshold_expression     I>=2u(I)
_computing_cell_refinement       'CrysAlisPro 1.171.41.116a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.116a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.116a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.5 (Bourhis et al., 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.5598
_refine_diff_density_min         -0.6281
_refine_diff_density_rms         0.1423
_refine_ls_d_res_high            0.5734
_refine_ls_d_res_low             5.7037
_refine_ls_goodness_of_fit_ref   1.0757
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     193
_refine_ls_number_reflns         3729
_refine_ls_number_restraints     70
_refine_ls_R_factor_all          0.0290
_refine_ls_R_factor_gt           0.0249
_refine_ls_restrained_S_all      1.0652
_refine_ls_shift/su_max          -0.0001
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0178P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0494
_refine_ls_wR_factor_ref         0.0513
_refine_special_details          
;Refinement using NoSpherA2, an implementation of
NOn-SPHERical Atom-form-factors in Olex2.
Please cite:
F. Kleemiss et al. Chem. Sci. DOI 10.1039/D0SC05526C - 2021
NoSpherA2 implementation of HAR makes use of
tailor-made aspherical atomic form factors calculated
on-the-fly from a Hirshfeld-partitioned electron density (ED) - not from
spherical-atom form factors.

The ED is calculated from a gaussian basis set single determinant SCF
wavefunction - either Hartree-Fock or DFT using selected funtionals
 - for a fragment of the crystal.
This fragment can be embedded in an electrostatic crystal field by employing cluster charges
or modelled using implicit solvation models, depending on the software used.
The following options were used:
   SOFTWARE:       'Please Select'
   PARTITIONING:   NoSpherA2
   INT ACCURACY:   Normal
   METHOD:         B3LYP
   BASIS SET:      def2-SVP
   CHARGE:         0
   MULTIPLICITY:   0
   DATE:           2022-01-08_13-25-43,HAR refinement with NoSpherA2
;
_olex2_refinement_description    
;
1. Restrained distances
 O5-H5a = O5-H5b = O2-H2a = O2-H2b = O1-H1b = O1-H1a = O4-H4a = O4-H4b = O3-
 H3b = O3-H3a
 0.989 with sigma of 0.02
2. Uiso/Uaniso restraints and constraints
Uanis(H1a) \\sim Ueq, Uanis(H1b) \\sim Ueq, Uanis(H3a) \\sim Ueq, Uanis(H3b)
\\sim Ueq, Uanis(H4a) \\sim Ueq, Uanis(H4b) \\sim Ueq, Uanis(H5a) \\sim Ueq,
Uanis(H5b) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(H2a) \\sim Ueq, Uanis(H2b) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.005
3. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
;
_atom_sites_solution_primary     dual
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_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
Cu1 Cu 0.5 0.5 0.5 0.00532(4) Uani 1.000000 2 S TU P
S1 S 0.87394(4) 0.51417(4) 0.21429(2) 0.00458(4) Uani 1.000000 1 . U .
O1 O 0.35103(14) 0.31497(13) 0.42559(7) 0.00892(13) Uani 1.000000 1 D U .
H1a H 0.244(3) 0.395(3) 0.3592(16) 0.025(5) Uani 1.000000 1 D U .
H1b H 0.269(3) 0.221(3) 0.4859(17) 0.021(5) Uani 1.000000 1 D U .
Cu2 Cu 0.5 1.0 0.0 0.00507(4) Uani 1.000000 2 S TU P
O2 O 0.65298(13) 0.20875(13) 0.61817(7) 0.00862(13) Uani 1.000000 1 D U .
H2a H 0.574(3) 0.198(3) 0.7042(15) 0.019(5) Uani 1.000000 1 D U .
H2b H 0.818(2) 0.161(3) 0.6241(17) 0.019(4) Uani 1.000000 1 D U .
O3 O 0.79729(14) 1.03431(14) -0.09523(8) 0.01210(15) Uani 1.000000 1 D U .
H3a H 0.935(3) 0.905(3) -0.1040(18) 0.024(5) Uani 1.000000 1 D U .
H3b H 0.845(3) 1.177(3) -0.1221(18) 0.027(5) Uani 1.000000 1 D U .
O4 O 0.52005(14) 0.74121(14) -0.08269(8) 0.01319(15) Uani 1.000000 1 D U .
H4a H 0.389(3) 0.697(3) -0.0984(19) 0.029(5) Uani 1.000000 1 D U .
H4b H 0.666(3) 0.648(3) -0.117(2) 0.029(5) Uani 1.000000 1 D U .
O6 O 0.82533(13) 0.40490(13) 0.34940(7) 0.00821(13) Uani 1.000000 1 . U .
O7 O 0.86238(13) 0.36289(13) 0.12590(7) 0.00864(13) Uani 1.000000 1 . U .
O8 O 1.11579(12) 0.54340(13) 0.19998(7) 0.00753(12) Uani 1.000000 1 . U .
O9 O 0.70303(13) 0.74810(12) 0.18336(7) 0.00852(13) Uani 1.000000 1 . U .
O5 O 0.13125(14) 0.06638(13) 0.62509(8) 0.00982(13) Uani 1.000000 1 D U .
H5a H 0.169(4) -0.100(3) 0.628(2) 0.042(6) Uani 1.000000 1 D U .
H5b H 0.203(4) 0.089(4) 0.6955(17) 0.031(6) Uani 1.000000 1 D U .


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 1.9686(8) . ?
Cu1 O1 1.9686(8) 2_666 ?
Cu1 O2 1.9759(7) . ?
Cu1 O2 1.9759(7) 2_666 ?
Cu1 O6 2.3619(7) 2_666 ?
Cu1 O6 2.3619(7) . ?
S1 O6 1.4751(7) . ?
S1 O7 1.4758(8) . ?
S1 O8 1.4910(7) . ?
S1 O9 1.4783(7) . ?
O1 H1a 0.962(14) . ?
O1 H1b 0.950(13) . ?
Cu2 O3 1.9676(7) 2_675 ?
Cu2 O3 1.9676(7) . ?
Cu2 O4 1.9360(8) . ?
Cu2 O4 1.9360(8) 2_675 ?
Cu2 O9 2.4100(7) 2_675 ?
Cu2 O9 2.4100(7) . ?
O2 H2a 0.971(14) . ?
O2 H2b 0.947(13) . ?
O3 H3a 0.964(14) . ?
O3 H3b 0.969(14) . ?
O4 H4a 0.947(14) . ?
O4 H4b 0.961(14) . ?
O5 H5a 0.964(15) . ?
O5 H5b 0.963(15) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Cu1 O1 180.0 2_666 . ?
O2 Cu1 O1 88.30(3) . . ?
O2 Cu1 O1 91.70(3) 2_666 . ?
O2 Cu1 O1 88.30(3) 2_666 2_666 ?
O2 Cu1 O1 91.70(3) . 2_666 ?
O2 Cu1 O2 180.0 . 2_666 ?
O6 Cu1 O1 87.82(3) 2_666 2_666 ?
O6 Cu1 O1 92.18(3) 2_666 . ?
O6 Cu1 O1 92.18(3) . 2_666 ?
O6 Cu1 O1 87.82(3) . . ?
O6 Cu1 O2 92.28(3) . 2_666 ?
O6 Cu1 O2 87.72(3) 2_666 2_666 ?
O6 Cu1 O2 92.28(3) 2_666 . ?
O6 Cu1 O2 87.72(3) . . ?
O6 Cu1 O6 180.0 . 2_666 ?
O7 S1 O6 110.26(4) . . ?
O8 S1 O6 108.62(4) . . ?
O8 S1 O7 108.84(4) . . ?
O9 S1 O6 109.46(4) . . ?
O9 S1 O7 110.96(4) . . ?
O9 S1 O8 108.65(4) . . ?
H1a O1 Cu1 118.7(12) . . ?
H1b O1 Cu1 115.6(12) . . ?
H1b O1 H1a 104.5(16) . . ?
O3 Cu2 O3 180.0 2_675 . ?
O4 Cu2 O3 90.39(3) . 2_675 ?
O4 Cu2 O3 90.39(3) 2_675 . ?
O4 Cu2 O3 89.61(3) . . ?
O4 Cu2 O3 89.61(3) 2_675 2_675 ?
O4 Cu2 O4 180.0 . 2_675 ?
O9 Cu2 O3 91.97(3) 2_675 2_675 ?
O9 Cu2 O3 91.97(3) . . ?
O9 Cu2 O3 88.03(3) . 2_675 ?
O9 Cu2 O3 88.03(3) 2_675 . ?
O9 Cu2 O4 86.65(3) 2_675 . ?
O9 Cu2 O4 93.35(3) . . ?
O9 Cu2 O4 93.35(3) 2_675 2_675 ?
O9 Cu2 O4 86.65(3) . 2_675 ?
O9 Cu2 O9 180.0 2_675 . ?
H2a O2 Cu1 112.1(11) . 2_666 ?
H2b O2 Cu1 120.6(11) . 2_666 ?
H2b O2 H2a 109.8(16) . . ?
H3a O3 Cu2 123.8(11) . 2_675 ?
H3b O3 Cu2 127.0(12) . 2_675 ?
H3b O3 H3a 107.6(15) . . ?
H4a O4 Cu2 124.7(13) . 2_675 ?
H4b O4 Cu2 123.2(13) . 2_675 ?
H4b O4 H4a 112.0(18) . . ?
S1 O6 Cu1 132.10(4) . 2_666 ?
Cu2 O9 S1 138.36(4) 2_675 . ?
H5b O5 H5a 107.5(18) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1 H1a O6 0.962(14) 2.494(17) 3.1997(11) 130.1(14) 1_455
O1 H1a O8 0.962(14) 1.875(15) 2.8113(11) 163.5(17) 1_455
O1 H1b O5 0.950(13) 1.812(14) 2.7494(11) 168.4(18) .
O2 H2a O3 0.971(14) 2.517(18) 3.1423(11) 122.1(14) 1_546
O2 H2a O9 0.971(14) 1.895(16) 2.7855(10) 151.3(17) 2_666
O2 H2b O5 0.947(13) 1.781(13) 2.7271(11) 176.2(17) 1_655
O3 H3a O7 0.964(14) 1.754(14) 2.7017(11) 166.7(17) 2_765
O3 H3b O8 0.969(14) 1.791(14) 2.7424(11) 166.5(18) 2_775
O4 H4a O7 0.947(14) 1.720(15) 2.6653(11) 175.7(19) 2_665
O4 H4b O8 0.961(14) 1.752(15) 2.6930(10) 166(2) 2_765
O5 H5a O6 0.964(15) 1.810(15) 2.7601(11) 167.6(19) 2_656
O5 H5b O9 0.963(15) 2.015(16) 2.9388(11) 160.0(19) 2_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 O6 S1 O7 -108.98(6) 2_666 . . . ?
Cu1 O6 S1 O7 -108.98(6) . . . . ?
Cu1 O6 S1 O8 131.84(6) 2_666 . . . ?
Cu1 O6 S1 O8 131.84(6) . . . . ?
Cu1 O6 S1 O9 13.35(7) 2_666 . . . ?
Cu1 O6 S1 O9 13.35(7) . . . . ?


_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.104
_oxdiff_exptl_absorpt_empirical_full_min 0.938
loop_
_restr_distance_atom_site_label_1
_restr_distance_atom_site_label_2
_restr_distance_site_symmetry_2
_restr_distance_target
_restr_distance_target_weight_param
_restr_distance_diff
O1 H1a 1 0.9890 0.0200 0.0266
O1 H1b 1 0.9890 0.0200 0.0388
O2 H2a 1 0.9890 0.0200 0.0184
O2 H2b 1 0.9890 0.0200 0.0417
O3 H3a 1 0.9890 0.0200 0.0248
O3 H3b 1 0.9890 0.0200 0.0201
O4 H4a 1 0.9890 0.0200 0.0419
O4 H4b 1 0.9890 0.0200 0.0280
O5 H5a 1 0.9890 0.0200 0.0246
O5 H5b 1 0.9890 0.0200 0.0256

loop_
_restr_U_iso_atom_site_label
_restr_U_iso_weight_param
H1a 0.0100
H1b 0.0100
H2a 0.0050
H2b 0.0050
H3a 0.0100
H3b 0.0100
H4a 0.0100
H4b 0.0100
H5a 0.0100
H5b 0.0100
