Synthesis and DNA cleavage studies of rationally designed metallopeptides from N-salicyl-AA-picolamide (SAP) and Cu(ii) ions
Panda, Subhashree S.; Kumari, Supriya; Dixit, Manjusha; Sharma, Nagendra K.; New Journal of Chemistry 48 (2024) 19188–19194; doi:10.1039/D4NJ03573A

data_7063489
_publ_section_title
;
 Synthesis and DNA cleavage studies of rationally designed metallopeptides
 from N-salicyl-AA-picolamide (SAP) and Cu(ii) ions
;
_journal_issue                   45
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              19188
_journal_page_last               19194
_journal_paper_doi               10.1039/D4NJ03573A
_journal_volume                  48
_journal_year                    2024
_chemical_formula_moiety         'C15 H13 Cu N3 O3'
_chemical_formula_sum            'C15 H13 Cu N3 O3'
_chemical_formula_weight         346.83
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_Int_Tables_number      14
_atom_sites_solution_primary     direct
_audit_creation_date             2022-12-02
_audit_creation_method
;
Olex2 1.2-alpha
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5335)
;
_audit_update_record
;
2024-01-20 deposited with the CCDC.	2024-10-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.164(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.3112(9)
_cell_length_b                   6.6485(5)
_cell_length_c                   18.4942(14)
_cell_measurement_reflns_used    6089
_cell_measurement_temperature    297.3(9)
_cell_measurement_theta_max      30.5290
_cell_measurement_theta_min      3.6820
_cell_volume                     1348.53(19)
_computing_cell_refinement       'CrysAlisPro 1.171.42.52a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.52a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.52a (Rigaku OD, 2022)'
_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    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_temperature      297.15
_diffrn_detector_area_resol_mean 5.8140
_diffrn_detector_type            'Pilatus 200K'
_diffrn_measured_fraction_theta_full 0.9967
_diffrn_measured_fraction_theta_max 0.9967
_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     -1.00  49.00   0.50   36.68    --    3.51-116.00  27.00  100
  2  \w    -60.00   3.00   0.50   36.68    --    3.51 -37.00  60.00  126
  3  \w      7.00  39.00   0.50   36.68    --    3.51  37.00-150.00   64
  4  \w    -42.00   7.00   0.50   36.68    --    3.51 -77.00-120.00   98
  5  \w    -15.00  17.00   0.50   36.68    --   -4.14  77.00  60.00   64
  6  \w    -15.00  17.00   0.50   36.68    --   -4.14 -99.00 -30.00   64
  7  \w    -27.00   9.00   0.50   36.68    --   -4.14  77.00 150.00   72
  8  \w      5.00  31.00   0.50   36.68    --   -4.14 -99.00-150.00   52
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'SuperNova, Dual, Cu at home/near, Pilatus 200K'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0586
_diffrn_reflns_av_unetI/netI     0.0488
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            12828
_diffrn_reflns_theta_full        26.3650
_diffrn_reflns_theta_max         26.36
_diffrn_reflns_theta_min         3.58
_exptl_absorpt_coefficient_mu    1.636
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.64509
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.52a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear orangish red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   orangish
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.7082
_exptl_crystal_description       needle
_exptl_crystal_F_000             709.6318
_exptl_crystal_preparation       'As per the reaction scheme'
_exptl_crystal_recrystallization_method 'Slow evaporation'
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.3668
_refine_diff_density_min         -0.3477
_refine_diff_density_rms         0.0801
_refine_ls_d_res_high            0.8002
_refine_ls_d_res_low             5.6854
_refine_ls_goodness_of_fit_ref   1.0286
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    24
_refine_ls_number_parameters     200
_refine_ls_number_reflns         2748
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0286
_refine_ls_R_factor_all          0.0381
_refine_ls_R_factor_gt           0.0319
_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^)+(0.0301P)^2^+0.8084P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0783
_refine_ls_wR_factor_ref         0.0814
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              13
_reflns_limit_h_min              -14
_reflns_limit_k_max              8
_reflns_limit_k_min              0
_reflns_limit_l_max              22
_reflns_limit_l_min              0
_reflns_number_gt                2378
_reflns_number_total             2748
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d4nj03573a2.cif
_cod_data_source_block           NKS-SSDP-221-Cu_auto
_cod_depositor_comments
'Adding full bibliography for 7063489--7063491.cif.'
_cod_database_code               7063489
_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.a Secondary CH2 refined with riding coordinates:
 C10(H10a,H10b), C8(H8a,H8b)
2.b Aromatic/amide H refined with riding coordinates:
 C15(H15), C5(H5), C2(H2), C12(H12), C14(H14), C3(H3), C4(H4), C13(H13)
2.c Idealised tetrahedral OH refined as rotating group:
 O1(H1)
;
_olex2_exptl_crystal_mounting_method 'mMethod on the loop'
_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
;