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_7706092
_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         'C68 H56 Br2 Cu2 N6 P2 S2'
_chemical_formula_sum            'C68 H56 Br2 Cu2 N6 P2 S2'
_chemical_formula_weight         1370.14
_chemical_name_systematic        RS-AR-9
_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                72.604(4)
_cell_angle_beta                 70.354(5)
_cell_angle_gamma                75.461(4)
_cell_formula_units_Z            1
_cell_length_a                   10.6202(6)
_cell_length_b                   11.2960(5)
_cell_length_c                   13.7122(7)
_cell_measurement_reflns_used    4667
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      32.1910
_cell_measurement_theta_min      3.7500
_cell_volume                     1457.49(14)
_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_type            Eos
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.883
_diffrn_measurement_details
;
  1 omega   -1.00   94.00   1.0000    2.1150
omega____ theta____ kappa____ phi______ frames
    -       25.9925   77.0000  -60.0000 95

  2 omega  -16.00   62.00   1.0000    2.1150
omega____ theta____ kappa____ phi______ frames
    -       25.9925  -99.0000   30.0000 78

  3 omega   16.00   76.00   1.0000    2.1150
omega____ theta____ kappa____ phi______ frames
    -       25.9925 -118.0000  133.0000 60

  4 omega  -46.00  -20.00   1.0000    2.1150
omega____ theta____ kappa____ phi______ frames
    -      -23.6487  -57.0000 -180.0000 26

  5 omega  -33.00   73.00   1.0000    2.1150
omega____ theta____ kappa____ phi______ frames
    -       25.9925    0.0000 -180.0000 106

  6 omega  -39.00   53.00   1.0000    2.1150
omega____ theta____ kappa____ phi______ frames
    -       25.9925  -77.0000 -180.0000 92
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Rigaku Oxford Diffraction Gemini Eos'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0388
_diffrn_reflns_av_unetI/netI     0.0627
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.883
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            17767
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.883
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         32.832
_diffrn_reflns_theta_min         3.246
_exptl_absorpt_coefficient_mu    2.276
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.67015
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (reslease 22-05-2014 CrysAlis171.NET)
(Compiled May 22 2014, 16:03:01)
Empirical absorption correction using spherical
harmonics,
 Implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.561
_exptl_crystal_description       plate
_exptl_crystal_F_000             696
_exptl_crystal_size_max          0.54
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.818
_refine_diff_density_min         -0.635
_refine_diff_density_rms         0.092
_refine_ls_extinction_coef       0.0016(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/1 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     371
_refine_ls_number_reflns         9580
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0645
_refine_ls_R_factor_gt           0.0412
_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^)+(0.0355P)^2^+0.0488P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0854
_refine_ls_wR_factor_ref         0.0974
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7249
_reflns_number_total             9580
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt03104f2.cif
_cod_data_source_block           rs-ar-9
_cod_database_code               7706092
_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, All N(H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 N1(H1), C2(H2), C5(H5), C6(H6), C7(H7), C8(H8), C10(H10), C12(H12), C13(H13),
 C14(H14), C15(H15), C18(H18), C19(H19), C20(H20), C21(H21), C22(H22), C24(H24),
  C25(H25), C26(H26), C27(H27), C28(H28), C30(H30), C31(H31), C32(H32),
 C33(H33), C34(H34)
2.b X=CH2 refined with riding coordinates:
 N3(H3A,H3B)
;
_shelx_res_checksum              24208
_olex2_exptl_crystal_mounting_method 'Polymer Loop'
_olex2_submission_special_instructions 'No special instructions were received'