Ultrastable radical-doped coordination compounds with antimicrobial activity against antibiotic-resistant bacteria.
Ke, Hua; Hu, Fen; Meng, Lingyi; Chen, Qi-Hua; Lai, Qian-Sheng; Li, Ze-Chen; Huang, Ze-Long; Liao, Jian-Zhen; Qiu, Jian-Ding; Lu, Can-Zhong; Chemical communications (Cambridge, England) 56 (2020) 14353–14356; doi:10.1039/d0cc06379g

data_7127749
_publ_section_title
;
 Ultrastable radical-doped coordination compounds with antimicrobial
 activity against antibiotic-resistant bacteria.
;
_journal_issue                   92
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              14353
_journal_page_last               14356
_journal_paper_doi               10.1039/d0cc06379g
_journal_volume                  56
_journal_year                    2020
_chemical_formula_moiety         'C18 H14 K2 N2 O11 S2'
_chemical_formula_sum            'C18 H14 K2 N2 O11 S2'
_chemical_formula_weight         576.63
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2019-12-12
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-09-18 deposited with the CCDC.	2020-10-23 downloaded from the CCDC.
;
_cell_angle_alpha                89.883(2)
_cell_angle_beta                 81.215(2)
_cell_angle_gamma                76.999(2)
_cell_formula_units_Z            1
_cell_length_a                   5.62440(10)
_cell_length_b                   6.10970(10)
_cell_length_c                   15.9088(3)
_cell_measurement_reflns_used    4227
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      75.1790
_cell_measurement_theta_min      2.8390
_cell_volume                     526.121(17)
_computing_cell_refinement       'CrysAlisPro 1.171.40.54a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.54a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.54a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.954
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -26.00  60.00   0.50    0.05    --   47.20 -37.00 -60.00  172
  2  \w    106.00 132.00   0.50    0.05    --  103.25  30.00 -60.00   52
  3  \w    150.00 176.00   0.50    0.05    --  103.25  30.00 -60.00   52
  4  \w    124.00 152.00   0.50    0.05    --  103.25 109.00-152.00   56
  5  \w     86.00 120.00   0.50    0.05    --  103.25 109.00-152.00   68
  6  \w     86.00 119.00   0.50    0.05    --  103.25  77.00   0.00   66
  7  \w    127.00 168.00   0.50    0.05    --  103.25  77.00   0.00   82
  8  \w     53.00  78.00   0.50    0.05    --  103.25-109.00 112.00   50
  9  \w     77.00 105.00   0.50    0.05    --  103.25 -94.00 120.00   56
 10  \w     35.00  70.00   0.50    0.05    --  103.25 -94.00 120.00   70
 11  \w     34.00 116.00   0.50    0.05    --  103.25-125.00  30.00  164
 12  \w      8.00  68.00   0.50    0.05    --   47.20-109.00 112.00  120
 13  \w    -24.00  22.00   0.50    0.05    --  -47.20  37.00 150.00   92
 14  \w    -58.00 -29.00   0.50    0.05    --  -47.20  37.00 150.00   58
 15  \w    -80.00 -30.00   0.50    0.05    -- -101.00  77.00 150.00  100
 16  \w    -93.00 -28.00   0.50    0.05    -- -101.00 125.00   0.00  130
 17  \w    -66.00 -41.00   0.50    0.05    --  -47.20 109.00-152.00   50
 18  \w     18.00  43.00   0.50    0.05    --   47.20-125.00-180.00   50
 19  \w     63.00  94.00   0.50    0.05    --   47.20-125.00-180.00   62
 20  \w    -95.00 -66.00   0.50    0.05    -- -101.00 109.00-152.00   58
 21  \w   -100.00 -35.00   0.50    0.05    -- -101.00  77.00 -90.00  130
 22  \w   -109.00 -29.00   0.50    0.05    -- -101.00  45.00 -90.00  160
 23  \w   -122.00 -96.00   0.50    0.05    -- -101.00  77.00  30.00   52
 24  \w   -112.00 -32.00   0.50    0.05    -- -101.00  15.00  90.00  160
 25  \w   -107.00 -82.00   0.50    0.05    -- -101.00-109.00 112.00   50
 26  \w   -115.00 -72.00   0.50    0.05    --  -47.20-125.00 120.00   86
 27  \w   -112.00 -72.00   0.50    0.05    --  -47.20-125.00 150.00   80
 28  \w   -168.00 -79.00   0.50    0.05    -- -101.00 -77.00 150.00  178
 29  \w   -104.00 -78.00   0.50    0.05    --  -47.20-125.00 -90.00   52
 30  \w   -121.00 -95.00   0.50    0.05    -- -101.00  77.00 150.00   52
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0220885000
_diffrn_orient_matrix_UB_12      -0.1027961000
_diffrn_orient_matrix_UB_13      -0.0899815000
_diffrn_orient_matrix_UB_21      -0.2017869000
_diffrn_orient_matrix_UB_22      -0.1268847000
_diffrn_orient_matrix_UB_23      0.0326771000
_diffrn_orient_matrix_UB_31      -0.1994906000
_diffrn_orient_matrix_UB_32      0.2009399000
_diffrn_orient_matrix_UB_33      -0.0211592000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0214
_diffrn_reflns_av_unetI/netI     0.0222
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.954
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            5054
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.954
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.872
_diffrn_reflns_theta_min         2.812
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_target            Mo
_diffrn_source_type              'PhotonJet R (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.473
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.59178
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.54a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            gray
_exptl_crystal_colour_primary    gray
_exptl_crystal_density_diffrn    1.820
_exptl_crystal_description       plate
_exptl_crystal_F_000             294
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.287
_refine_diff_density_min         -0.568
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.153
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     163
_refine_ls_number_reflns         2063
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.214
_refine_ls_R_factor_all          0.0449
_refine_ls_R_factor_gt           0.0389
_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/[\s^2^(Fo^2^)+(0.0577P)^2^+0.4129P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1035
_refine_ls_wR_factor_ref         0.1166
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1895
_reflns_number_total             2063
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc06379g2.cif
_cod_data_source_block           Compound-1
_cod_database_code               7127749
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H O N S K'
_shelx_estimated_absorpt_t_max   0.881
_shelx_estimated_absorpt_t_min   0.247
_diffrn_oxdiff_digest_frames
;
01c0b4ee1f4d838808d31793b6054af70902608ee35
;
_diffrn_oxdiff_digest_hkl
;
01a8dc1bea4d9dc9843c933dda47da1f08c233
;
_reflns_odcompleteness_completeness 99.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All O(H) groups
2. Restrained distances
 O1-H1
 0.85 with sigma of 0.01
 S1-H1
 1.899989 with sigma of 0.02
 K1-H1
 3.59028 with sigma of 0.02
3.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C1(H1A,H1B)
3.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C5(H5)
;
_shelx_res_checksum              98489
_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 1.424
_oxdiff_exptl_absorpt_empirical_full_min 0.779