Single X-ray crystal structure, DFT studies and topoisomerase I inhibition activity of a tailored ionic Ag(i) nalidixic acid‒piperazinium drug entity specific for pancreatic cancer cells
Yousuf, Imtiyaz; Usman, Mohammad; Ahmad, Musheer; Tabassum, Sartaj; Arjmand, Farukh; New Journal of Chemistry 42 (2018) 506–; doi:10.1039/C7NJ03602G

data_7056786
_publ_section_title
;
 Single X-ray crystal structure, DFT studies and topoisomerase I
 inhibition activity of a tailored ionic Ag(i) nalidixic
 acid--piperazinium drug entity specific for pancreatic cancer cells
;
_journal_issue                   1
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              506
_journal_paper_doi               10.1039/C7NJ03602G
_journal_volume                  42
_journal_year                    2018
_chemical_formula_moiety
'C8 H22 Ag N4, 2(C12 H11 N2 O3), N O3, 8(H2 O)'
_chemical_formula_sum            'C32 H60 Ag N9 O17'
_chemical_formula_weight         950.75
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_primary     direct
_audit_creation_date             2017-11-21
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2017-11-21 deposited with the CCDC.
2017-11-23 downloaded from the CCDC.
;
_cell_angle_alpha                85.314(5)
_cell_angle_beta                 76.322(5)
_cell_angle_gamma                84.973(5)
_cell_formula_units_Z            1
_cell_length_a                   7.607(5)
_cell_length_b                   11.845(5)
_cell_length_c                   12.098(5)
_cell_measurement_reflns_used    9866
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.33
_cell_measurement_theta_min      2.37
_cell_volume                     1053.0(9)
_computing_cell_refinement       'SAINT v6.45A (Bruker, 2003)'
_computing_data_collection       'Bruker Smart'
_computing_data_reduction        'SAINT v6.45A (Bruker, 2003)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution    'SIR97 (Burla et al., 2007)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.9986
_diffrn_measured_fraction_theta_max 0.9987
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0368
_diffrn_reflns_av_unetI/netI     0.0424
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            16077
_diffrn_reflns_theta_full        25.0000
_diffrn_reflns_theta_max         25.60
_diffrn_reflns_theta_min         2.53
_exptl_absorpt_coefficient_mu    0.560
_exptl_absorpt_correction_T_max  25.599
_exptl_absorpt_correction_T_min  2.527
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.4992
_exptl_crystal_description       block
_exptl_crystal_F_000             497.4027
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.4547
_refine_diff_density_min         -0.3907
_refine_diff_density_rms         0.0757
_refine_ls_d_res_high            0.8225
_refine_ls_d_res_low             8.0611
_refine_ls_goodness_of_fit_ref   1.0704
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    58
_refine_ls_number_parameters     348
_refine_ls_number_reflns         3971
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0704
_refine_ls_R_factor_all          0.0319
_refine_ls_R_factor_gt           0.0294
_refine_ls_shift/su_max          0.0000
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0303P)^2^+0.8106P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0701
_refine_ls_wR_factor_ref         0.0713
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              9
_reflns_limit_h_min              -8
_reflns_limit_k_max              14
_reflns_limit_k_min              -14
_reflns_limit_l_max              14
_reflns_limit_l_min              0
_reflns_number_gt                3787
_reflns_number_total             3971
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            c7nj03602g2.cif
_cod_data_source_block           Complex1
_cod_depositor_comments          'Adding full bibliography for 7056786.cif.'
_cod_database_code               7056786
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Others
 Fixed Sof: O4(0.5) O5(0.5) O7A(0.5) H7Aa(0.5) H7Ab(0.5) O7B(0.5) H7Ba(0.5)
 H7Bb(0.5) O8A(0.5) H8Aa(0.5) H8Ab(0.5) O8B(0.5) H8Ba(0.5) H8Bb(0.5) O9A(0.5)
 H9Aa(0.5) H9Ab(0.5) O9B(0.5) H9Ba(0.5) H9Bb(0.5) O10A(0.5) H10a(0.5) H10b(0.5)
 O10B(0.5) H10c(0.5) H10d(0.5) O6(0.5) N5(0.5)
3.a Free rotating group:
 O7A(H7Aa,H7Ab), O7B(H7Ba,H7Bb), O8A(H8Aa,H8Ab), O8B(H8Ba,H8Bb), O9A(H9Aa,
 H9Ab), O9B(H9Ba,H9Bb), O10A(H10a,H10b), O10B(H10c,H10d)
3.b Ternary CH refined with riding coordinates:
 N3(H3)
3.c Secondary CH2 refined with riding coordinates:
 N4(H4a,H4b), C11(H11a,H11b), C13(H13a,H13b), C14(H14a,H14b), C15(H15a,H15b),
 C16(H16a,H16b)
3.d Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C10(H10)
3.e Idealised Me refined as rotating group:
 C8(H8a,H8b,H8c), C12(H12a,H12b,H12c)
;
_olex2_submission_special_instructions 'No special instructions were received'