Cu(ii) complexes of a tridentate N,N,O-donor Schiff base of pyridoxal: synthesis, X-ray structures, DNA-binding properties and catecholase activity
Mondal, Satyajit; Chakraborty, Moumita; Mondal, Antu; Pakhira, Bholanath; Blake, Alexander J.; Sinn, Ekkehard; Chattopadhyay, Shyamal Kumar; New Journal of Chemistry 42 (2018) 9588–; doi:10.1039/C8NJ00418H

data_7057293
_publ_section_title
;
 Cu(ii) complexes of a tridentate N,N,O-donor Schiff base of pyridoxal:
 synthesis, X-ray structures, DNA-binding properties and catecholase
 activity
;
_journal_issue                   12
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              9588
_journal_paper_doi               10.1039/C8NJ00418H
_journal_volume                  42
_journal_year                    2018
_chemical_formula_moiety         'C12 H18 Cu N6 O2'
_chemical_formula_sum            'C12 H18 Cu N6 O2'
_chemical_formula_weight         341.86
_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_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2014-07-11
_audit_creation_method
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Olex2 1.2
(compiled 2014.06.27 svn.r2953 for OlexSys, GUI svn.r4855)
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_audit_update_record
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2018-01-17 deposited with the CCDC.
2018-04-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.172(11)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   6.7641(8)
_cell_length_b                   11.5087(12)
_cell_length_c                   17.8781(19)
_cell_measurement_reflns_used    2801
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      74.409
_cell_measurement_theta_min      2.518
_cell_volume                     1388.1(3)
_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
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_reduction
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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    'ShelXS (Sheldrick, 2008)'
_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 0.992
_diffrn_measured_fraction_theta_max 0.951
_diffrn_measurement_details
;
  1 omega   51.00   77.00   2.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000  -30.0000  -60.0000 13

  2 omega   39.00   67.00   2.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000  -45.0000  -30.0000 14

  3 omega   41.00   97.00   2.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000  -45.0000  -90.0000 28

  4 omega   51.00   77.00   2.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000  -30.0000 -180.0000 13

  5 omega   40.00  108.00   2.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000  -94.0000  -60.0000 34

  6 omega   50.00   76.00   2.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000 -125.0000 -150.0000 13

  7 omega   31.00   91.00   2.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000  -30.0000   60.0000 30

  8 omega   37.00   97.00   2.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000  -45.0000  150.0000 30

  9 omega  -65.00   31.00   2.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000   77.0000   90.0000 48

 10 omega  -97.00  -17.00   2.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000  -57.0000  -60.0000 40

 11 omega   80.00  170.00   2.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000  125.0000 -180.0000 45
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'GV1000, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0999361000
_diffrn_orient_matrix_UB_12      0.1196469000
_diffrn_orient_matrix_UB_13      -0.0111625000
_diffrn_orient_matrix_UB_21      -0.1098502000
_diffrn_orient_matrix_UB_22      -0.0433857000
_diffrn_orient_matrix_UB_23      -0.0731428000
_diffrn_orient_matrix_UB_31      -0.1734363000
_diffrn_orient_matrix_UB_32      -0.0415029000
_diffrn_orient_matrix_UB_33      0.0446146000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.024
_diffrn_reflns_av_unetI/netI     0.027
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.951
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            5363
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.951
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.825
_diffrn_reflns_theta_min         4.573
_diffrn_source                   'rotating-anode X-ray tube'
_diffrn_source_type              'GV1000 (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.365
_exptl_absorpt_correction_T_max  0.871
_exptl_absorpt_correction_T_min  0.729
_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
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear black'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.636
_exptl_crystal_description       block
_exptl_crystal_F_000             708
_exptl_crystal_size_max          0.393
_exptl_crystal_size_mid          0.194
_exptl_crystal_size_min          0.151
_refine_diff_density_max         0.41
_refine_diff_density_min         -0.38
_refine_diff_density_rms         0.06
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.08
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     196
_refine_ls_number_reflns         2722
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.08
_refine_ls_R_factor_all          0.0318
_refine_ls_R_factor_gt           0.0292
_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^)+(0.045P)^2^+0.659P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0820
_refine_ls_wR_factor_ref         0.0842
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2528
_reflns_number_total             2722
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8nj00418h2.cif
_cod_data_source_block           skcabf
_cod_depositor_comments
'Adding full bibliography for 7057293--7057294.cif.'
_cod_database_code               7057293
_nottingham_internal_coll_name   SKCABF
_nottingham_internal_coll_number 13787
_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   07/07/2014
_nottingham_internal_coll_location NOTTS
_nottingham_internal_process_date 08/07/2014
_nottingham_internal_process_user pcxaeoc
_nottingham_internal_solution_date 08/07/2014
_nottingham_internal_solution_user pcxaeoc
_nottingham_internal_refinement_date 08/07/2014
_nottingham_internal_refinement_user pcxaoec
_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 16/07/2014
_nottingham_internal_validation_user AJB
_nottingham_internal_archive_date 16/07/2014
_shelxl_version_number           2014-3
_chemical_oxdiff_formula         'C25 H38 Cu2 N12 O4'
_reflns_odcompleteness_completeness 99.20
_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
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2.a Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C10(H10A,H10B), C9(H9A,H9B)
2.b Aromatic/amide H refined with riding coordinates:
 C8(H8), C5(H5)
2.c Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C11(H11A,H11B,H11C), C7(H7A,H7B,H7C)
;
_shelx_res_checksum              28893
_olex2_exptl_crystal_mounting_method 'in fomblin film on a micromount'
_olex2_submission_special_instructions 'No special instructions were received'