Copper(I) and silver(I) complexes of anthraldehyde thiosemicarbazone: synthesis, structure elucidation, <i>in vitro</i> anti-tuberculosis/cytotoxic activity and interactions with DNA/HSA.
Khan, Ashiq; Paul, Kamaldeep; Singh, Iqubal; Jasinski, Jerry P.; Smolenski, Victoria A.; Hotchkiss, Ethan P.; Kelley, Patrick T.; Shalit, Zachary A.; Kaur, Manpreet; Banerjee, Somesh; Roy, Partha; Sharma, Rekha; Dalton transactions (Cambridge, England : 2003) 49 (2020) 17350–17367; doi:10.1039/d0dt03104f

data_7706093
_publ_section_title
;
 Copper(I) and silver(I) complexes of anthraldehyde thiosemicarbazone:
 synthesis, structure elucidation, <i>in vitro</i>
 anti-tuberculosis/cytotoxic activity and interactions with DNA/HSA.
;
_journal_issue                   47
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              17350
_journal_page_last               17367
_journal_paper_doi               10.1039/d0dt03104f
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C70 H60 Ag2 Cl2 N6 P2 S2'
_chemical_formula_sum            'C70 H60 Ag2 Cl2 N6 P2 S2'
_chemical_formula_weight         1397.94
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-10-08
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-10-08 deposited with the CCDC.	2020-10-20 downloaded from the CCDC.
;
_cell_angle_alpha                82.287(5)
_cell_angle_beta                 79.882(6)
_cell_angle_gamma                75.133(5)
_cell_formula_units_Z            1
_cell_length_a                   10.4921(7)
_cell_length_b                   12.0020(6)
_cell_length_c                   13.8200(10)
_cell_measurement_reflns_used    5886
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      71.6210
_cell_measurement_theta_min      4.3960
_cell_volume                     1648.60(19)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 16.0416
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_details
;
  1 omega  -16.00   18.00   1.0000    1.6800
omega____ theta____ kappa____ phi______ frames
    -      -33.5000   37.0000   30.0000 34

  2 omega   60.00  102.00   1.0000    1.6800
omega____ theta____ kappa____ phi______ frames
    -       35.3572   77.0000  -90.0000 42

  3 omega   60.00  101.00   1.0000    1.6800
omega____ theta____ kappa____ phi______ frames
    -       35.3572   77.0000  -60.0000 41

  4 omega   49.00   75.00   1.0000    1.6800
omega____ theta____ kappa____ phi______ frames
    -       35.3572   77.0000 -150.0000 26

  5 omega   10.00   48.00   1.0000    1.6800
omega____ theta____ kappa____ phi______ frames
    -       35.3572   77.0000 -150.0000 38

  6 omega   11.00   36.00   1.0000    1.6800
omega____ theta____ kappa____ phi______ frames
    -       35.3572   77.0000  -90.0000 25

  7 omega   14.00   47.00   1.0000    1.6800
omega____ theta____ kappa____ phi______ frames
    -       35.3572   77.0000  -60.0000 33

  8 omega  -12.00   34.00   1.0000    1.6800
omega____ theta____ kappa____ phi______ frames
    -      -33.5000   57.0000 -150.0000 46

  9 omega   63.00   90.00   1.0000    1.6800
omega____ theta____ kappa____ phi______ frames
    -       35.3572  178.0000   60.0000 27

 10 omega  111.00  154.00   1.0000    6.7200
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000   60.0000 43

 11 omega  140.00  176.00   1.0000    6.7200
omega____ theta____ kappa____ phi______ frames
    -      108.0000   45.0000  120.0000 36

 12 omega  110.00  167.00   1.0000    6.7200
omega____ theta____ kappa____ phi______ frames
    -      108.0000   61.0000   30.0000 57

 13 omega  106.00  172.00   1.0000    6.7200
omega____ theta____ kappa____ phi______ frames
    -      108.0000    0.0000   30.0000 66

 14 omega   91.00  166.00   1.0000    6.7200
omega____ theta____ kappa____ phi______ frames
    -      108.0000   61.0000  -60.0000 75

 15 omega   92.00  132.00   1.0000    6.7200
omega____ theta____ kappa____ phi______ frames
    -      108.0000   45.0000  120.0000 40

 16 omega   58.00   99.00   1.0000    6.7200
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -45.0000   60.0000 41

 17 omega   83.00  109.00   1.0000    6.7200
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -94.0000   30.0000 26

 18 omega   65.00  116.00   1.0000    6.7200
omega____ theta____ kappa____ phi______ frames
    -      108.0000 -111.0000  150.0000 51

 19 omega   49.00   75.00   1.0000    6.7200
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -77.0000  150.0000 26

 20 omega   47.00   90.00   1.0000    6.7200
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000  150.0000 43

 21 omega   39.00   75.00   1.0000    6.7200
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000  120.0000 36

 22 omega   39.00   72.00   1.0000    6.7200
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -94.0000   30.0000 33

 23 omega   44.00  115.00   1.0000    6.7200
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -61.0000    0.0000 71

 24 omega   43.00   89.00   1.0000    1.6800
omega____ theta____ kappa____ phi______ frames
    -       35.3572 -127.0000  103.0000 46

 25 omega   38.00   83.00   1.0000    6.7200
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000    0.0000 45

 26 omega   39.00   79.00   1.0000    6.7200
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000  -60.0000 40

 27 omega   38.00  110.00   1.0000    6.7200
omega____ theta____ kappa____ phi______ frames
    -      108.0000 -111.0000  -60.0000 72

 28 omega   51.00  134.00   1.0000    6.7200
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -77.0000 -180.0000 83

 29 omega   40.00  115.00   1.0000    6.7200
omega____ theta____ kappa____ phi______ frames
    -      108.0000 -111.0000    0.0000 75

 30 omega  -65.00  -40.00   1.0000    1.6800
omega____ theta____ kappa____ phi______ frames
    -      -33.5000 -178.0000  150.0000 25

 31 omega -104.00  -36.00   1.0000    1.6800
omega____ theta____ kappa____ phi______ frames
    -      -33.5000 -178.0000   60.0000 68

 32 omega -101.00  -24.00   1.0000    1.6800
omega____ theta____ kappa____ phi______ frames
    -      -33.5000  -57.0000   60.0000 77

 33 omega  -98.00  -72.00   1.0000    1.6800
omega____ theta____ kappa____ phi______ frames
    -      -33.5000  178.0000 -120.0000 26

 34 omega   57.00   82.00   1.0000    1.6800
omega____ theta____ kappa____ phi______ frames
    -       35.3572  178.0000 -150.0000 25
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Agilent, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0303
_diffrn_reflns_av_unetI/netI     0.0411
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            11739
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        67.500
_diffrn_reflns_theta_max         71.250
_diffrn_reflns_theta_min         3.263
_exptl_absorpt_coefficient_mu    6.912
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.40882
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.408
_exptl_crystal_description       prism
_exptl_crystal_F_000             712
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.452
_refine_diff_density_min         -0.483
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     380
_refine_ls_number_reflns         6262
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.011
_refine_ls_R_factor_all          0.0437
_refine_ls_R_factor_gt           0.0383
_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^)+(0.0650P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0959
_refine_ls_wR_factor_ref         0.0994
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5656
_reflns_number_total             6262
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt03104f2.cif
_cod_data_source_block           far-1
_cod_database_code               7706093
_shelx_shelxl_version_number     2018/1
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 N2(H2), N3(H3), C2(H2A), C3(H3A), C4(H4), C5(H5), C7(H7), C9(H9), C10(H10),
 C11(H11), C12(H12), C15(H15), C19(H19), C20(H20), C21(H21), C22(H22), C23(H23),
  C25(H25), C26(H26), C27(H27), C28(H28), C29(H29), C31(H31), C32(H32),
 C33(H33), C34(H34), C35(H35)
2.b Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C)
;
_shelx_res_checksum              58846
_shelx_fab_checksum              40682
_olex2_exptl_crystal_mounting_method 'Polymer Loop'
_olex2_submission_special_instructions 'No special instructions were received'