Catecholase activity, DNA binding and cytotoxicity studies of a Cu(ii) complex of a pyridoxal schiff base: synthesis, X-ray crystal structure, spectroscopic, electrochemical and theoretical studies
Adak, Piyali; Ghosh, Bipinbihari; Bauzá, Antonio; Frontera, Antonio; Blake, Alexander J.; Corbella, Montserrat; Das Mukhopadhyay, Chitrangada; Chattopadhyay, Shyamal Kumar; RSC Advances 6 (2016) 86851–; doi:10.1039/C6RA14059A

data_7236244
_publ_section_title
;
 Catecholase activity, DNA binding and cytotoxicity studies of a Cu(ii)
 complex of a pyridoxal schiff base: synthesis, X-ray crystal structure,
 spectroscopic, electrochemical and theoretical studies
;
_journal_issue                   90
_journal_name_full               'RSC Advances'
_journal_page_first              86851
_journal_paper_doi               10.1039/C6RA14059A
_journal_volume                  6
_journal_year                    2016
_chemical_formula_moiety         'C28 H30 Cl2 Cu2 N6 O4, 2(Cl O4)'
_chemical_formula_sum            'C28 H30 Cl4 Cu2 N6 O12'
_chemical_formula_weight         911.46
_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   mixed
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_date             2014-07-11
_audit_creation_method
;
Olex2 1.2
(compiled 2014.06.27 svn.r2953 for OlexSys, GUI svn.r4855)
;
_audit_update_record
;
2016-03-14 deposited with the CCDC.
2016-08-31 downloaded from the CCDC.
;
_cell_angle_alpha                75.507(10)
_cell_angle_beta                 83.103(10)
_cell_angle_gamma                65.615(15)
_cell_formula_units_Z            1
_cell_length_a                   7.7545(13)
_cell_length_b                   8.7537(13)
_cell_length_c                   13.9700(11)
_cell_measurement_reflns_used    3075
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      72.1140
_cell_measurement_theta_min      3.2660
_cell_volume                     836.1(2)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies, Version 1.171.37.33 
(release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies, Version 1.171.37.33
(release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies, Version 1.171.37.33
(release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2013)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3271
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.953
_diffrn_measurement_details
;
  1 omega  -26.00   66.00   2.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       42.7573  -57.0000    0.0000 46

  2 omega   24.00   50.00   2.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       42.7573 -125.0000  -30.0000 13

  3 omega   72.00   96.00   2.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       42.7573 -125.0000  -30.0000 12

  4 omega   33.00  107.00   2.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000  -94.0000   60.0000 37

  5 omega   64.00  118.00   2.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000 -125.0000   30.0000 27

  6 omega   58.00   86.00   2.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000  -30.0000   30.0000 14

  7 omega   40.00   86.00   2.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000  -45.0000   30.0000 23

  8 omega   36.00   84.00   2.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000  -30.0000  -60.0000 24

  9 omega   65.00  131.00   2.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000  -61.0000 -150.0000 33

 10 omega   85.00  177.00   2.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000   15.0000 -150.0000 46

 11 omega   42.00  144.00   2.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000  -15.0000 -180.0000 51

 12 omega   27.00  105.00   2.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000  -94.0000 -120.0000 39

 13 omega  -15.00   67.00   2.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       42.7573  -57.0000 -150.0000 41

 14 omega   19.00  111.00   2.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       42.7573   57.0000  150.0000 46

 15 omega   39.00   77.00   2.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000  -61.0000  150.0000 19

 16 omega   25.00  109.00   2.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000  -94.0000  150.0000 42
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'GV1000, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.2087384000
_diffrn_orient_matrix_UB_12      -0.0237853000
_diffrn_orient_matrix_UB_13      -0.0167695000
_diffrn_orient_matrix_UB_21      0.0623700000
_diffrn_orient_matrix_UB_22      -0.1967333000
_diffrn_orient_matrix_UB_23      0.0282513000
_diffrn_orient_matrix_UB_31      -0.0116056000
_diffrn_orient_matrix_UB_32      -0.0013621000
_diffrn_orient_matrix_UB_33      -0.1090812000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0716
_diffrn_reflns_av_unetI/netI     0.0622
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.953
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            5562
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.953
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.262
_diffrn_reflns_theta_min         5.691
_diffrn_source                   'rotating-anode X-ray tube'
_diffrn_source_type              'GV1000 (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.158
_exptl_absorpt_correction_T_max  0.771
_exptl_absorpt_correction_T_min  0.624
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies, Version 1.171.37.33 (release 27-03-2014
CrysAlis171 .NET) (compiled Mar 27 2014,17:12:48) Numerical absorption 
correction based on gaussian integration over a multifaceted crystal model
;
_exptl_crystal_colour            'clear green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.810
_exptl_crystal_description       block
_exptl_crystal_F_000             462
_exptl_crystal_size_max          0.2632
_exptl_crystal_size_mid          0.1953
_exptl_crystal_size_min          0.1253
_refine_diff_density_max         1.147
_refine_diff_density_min         -0.997
_refine_diff_density_rms         0.133
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     243
_refine_ls_number_reflns         3245
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.04
_refine_ls_R_factor_all          0.0610
_refine_ls_R_factor_gt           0.0572
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.100P)^2^+0.595P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.154
_refine_ls_wR_factor_ref         0.159
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2926
_reflns_number_total             3245
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6ra14059a2.cif
_cod_data_source_block           skcaba
_cod_database_code               7236244
_nottingham_internal_coll_name   SKCABA
_nottingham_internal_coll_number 13782
_nottingham_internal_coll_client SKC/AJB
_nottingham_internal_coll_type   custom
_nottingham_internal_coll_frame_method 'omega scans'
_nottingham_internal_coll_frame_time 2.0000
_nottingham_internal_coll_frame_width 2.0000
_nottingham_internal_coll_user   pcxaeoc
_nottingham_internal_coll_date   04/07/2014
_nottingham_internal_coll_location NOTTS
_nottingham_internal_process_date 07/07/2014
_nottingham_internal_process_user pcxaeoc
_nottingham_internal_solution_date 7/7/2014
_nottingham_internal_solution_user pcxaeoc
_nottingham_internal_refinement_date 8/7/2014
_nottingham_internal_refinement_user pcxaeoc
_nottingham_internal_self_archive_date 11/07/2014
_nottingham_internal_self_validation_date 11/07/2014
_nottingham_internal_self_validation_user pcxaeoc
_nottingham_internal_validation_date 16/7/2014
_nottingham_internal_validation_user AEOC/AJB
_nottingham_internal_archive_date 16/7/2014
_shelxl_version_number           2014-3
_chemical_oxdiff_formula         'C11 H10 N3 O10 Cl2 Cu'
_chemical_oxdiff_usercomment     '#13782 for SKCABA for AJB'
_reflns_odcompleteness_completeness 99.06
_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, All O(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B), C6(H6A,H6B)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2A), C11(H11), C3(H3A), C4(H4), C1(H1), C7(H7)
2.c Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C)
;
_shelx_res_checksum              83013
_olex2_exptl_crystal_mounting_method 'in fomblin film on a micromount'
_olex2_submission_special_instructions 'No special instructions were received'