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_7127750
_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 H16 Ca N2 O12 S2'
_chemical_formula_sum            'C18 H16 Ca N2 O12 S2'
_chemical_formula_weight         556.53
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2019-12-18
_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                90
_cell_angle_beta                 108.766(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.8177(3)
_cell_length_b                   28.7454(7)
_cell_length_c                   8.9688(3)
_cell_measurement_reflns_used    6370
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      74.4790
_cell_measurement_theta_min      5.4270
_cell_volume                     2152.46(12)
_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    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'Image Plate'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            'Rigaku IP'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.961
_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     25.00 117.00   0.50    0.14    --   47.20  77.00-150.00  184
  2  \w     36.00 114.00   0.50    0.14    --   47.20  37.00-180.00  156
  3  \w     34.00 115.00   0.50    0.54    --  103.25 -45.00 -90.00  162
  4  \w     71.00 103.00   0.50    0.54    --  103.25 -94.00-180.00   64
  5  \w     58.00  83.00   0.50    0.54    --  103.25 -94.00-150.00   50
  6  \w     33.00 108.00   0.50    0.54    --  103.25 -30.00 -90.00  150
  7  \w     57.00  88.00   0.50    0.14    --   47.20-128.00 -32.00   62
  8  \w     40.00  65.00   0.50    0.14    --   47.20-141.00 156.00   50
  9  \w     70.00 127.00   0.50    0.54    --  103.25-141.00 156.00  114
 10  \w     36.00  68.00   0.50    0.54    --  103.25-141.00 156.00   64
 11  \w     92.00 146.00   0.50    0.54    --  103.25  45.00 120.00  108
 12  \w     92.00 175.00   0.50    0.54    --  103.25 125.00 150.00  166
 13  \w    -75.00 -50.00   0.50    0.14    --  -47.20 128.00  42.00   50
 14  \w   -129.00 -37.00   0.50    0.54    -- -101.00 141.00-146.00  184
 15  \w   -170.00-145.00   0.50    0.54    -- -101.00 -61.00  60.00   50
 16  \w   -128.00 -87.00   0.50    0.54    -- -101.00 -61.00  60.00   82
 17  \w   -110.00 -69.00   0.50    0.14    --  -47.20-128.00 -32.00   82
 18  \w   -119.00 -62.00   0.50    0.14    --  -47.20-141.00 156.00  114
 19  \w   -119.00 -94.00   0.50    0.54    -- -101.00-128.00 -32.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Rigaku R-AXIS SPIDER IP'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0105984000
_diffrn_orient_matrix_UB_12      -0.0533312000
_diffrn_orient_matrix_UB_13      -0.0167674000
_diffrn_orient_matrix_UB_21      0.0187121000
_diffrn_orient_matrix_UB_22      -0.0044481000
_diffrn_orient_matrix_UB_23      0.1761873000
_diffrn_orient_matrix_UB_31      -0.1833088000
_diffrn_orient_matrix_UB_32      0.0026488000
_diffrn_orient_matrix_UB_33      -0.0397686000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0526
_diffrn_reflns_av_unetI/netI     0.0465
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.961
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            14444
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.961
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.173
_diffrn_reflns_theta_min         3.075
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_target            Mo
_diffrn_source_type              'PhotonJet R (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.992
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.52326
_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            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.717
_exptl_crystal_description       plate
_exptl_crystal_F_000             1144
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.767
_refine_diff_density_min         -0.587
_refine_diff_density_rms         0.110
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     328
_refine_ls_number_reflns         4269
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0680
_refine_ls_R_factor_gt           0.0583
_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/[\s^2^(Fo^2^)+(0.0939P)^2^+2.7242P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1550
_refine_ls_wR_factor_ref         0.1681
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3708
_reflns_number_total             4269
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc06379g2.cif
_cod_data_source_block           Compound-2
_cod_original_cell_volume        2152.46(11)
_cod_database_code               7127750
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H N O S Ca'
_shelx_estimated_absorpt_t_max   0.635
_shelx_estimated_absorpt_t_min   0.521
_diffrn_oxdiff_digest_frames
;
014f5038d5fee4f352013a4eceee72670900047456d
;
_diffrn_oxdiff_digest_hkl
;
011589064a3bff358061f43697dade13caaf20
;
_reflns_odcompleteness_completeness 99.92
_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,H) groups
2. Restrained distances
 O12-H12A = O12-H12B
 0.85 with sigma of 0.02
 O11-H11A = O11-H11B
 0.85 with sigma of 0.02
 H12A-H12B
 1.34 with sigma of 0.04
 H11A-H11B
 1.34 with sigma of 0.04
 Ca1-H12A \\sim Ca1-H12B
 with sigma of 0.02
 Ca1-H11A \\sim Ca1-H11B
 with sigma of 0.02
3.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C10(H10A,H10B), C1(H1A,H1B), C11(H11C,H11D)
3.b Aromatic/amide H refined with riding coordinates:
 C17(H17), C8(H8), C18(H18), C9(H9)
;
_shelx_res_checksum              1699
_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 1.712
_oxdiff_exptl_absorpt_empirical_full_min 0.618