Water Soluble Transition metal [Ni(II), Cu(II) and Zn(II)] Complexes of N–Phthaloylglycinate bis(diaminocyclohexane). DNA Binding, pBR322 Cleavage and Cytotoxicity
Khursheed, Salman; Siddique, Hifzur R.; Tabassum, Sartaj; Arjmand, Farukh; Dalton Transactions  (2022) –; doi:10.1039/D2DT01312F

data_7710685
_publ_section_title
;
 Water Soluble Transition metal [Ni(II), Cu(II) and Zn(II)] Complexes of
 N--Phthaloylglycinate bis(diaminocyclohexane). DNA Binding, pBR322
 Cleavage and Cytotoxicity
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT01312F
_journal_year                    2022
_chemical_formula_moiety         'C6 H13 Cu0.5 N2, C10 H6 N O4'
_chemical_formula_sum            'C16 H19 Cu0.5 N3 O4'
_chemical_formula_weight         349.11
_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'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2021-12-04
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2021-12-07 deposited with the CCDC.	2022-07-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.819(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.5779(2)
_cell_length_b                   14.4730(2)
_cell_length_c                   8.74790(10)
_cell_measurement_reflns_used    24846
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.5090
_cell_measurement_theta_min      1.9890
_cell_volume                     1812.88(4)
_computing_cell_refinement       'CrysAlisPro 1.171.40.82a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.82a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.82a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.966
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix3000'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0364
_diffrn_reflns_av_unetI/netI     0.0206
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.966
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            52185
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.966
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.398
_diffrn_reflns_theta_min         2.001
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    0.656
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.81657
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.82a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.279
_exptl_crystal_description       metallic
_exptl_crystal_F_000             730
_refine_diff_density_max         0.397
_refine_diff_density_min         -0.291
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.109
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     255
_refine_ls_number_reflns         3988
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.133
_refine_ls_R_factor_all          0.0564
_refine_ls_R_factor_gt           0.0435
_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^)+(0.0729P)^2^+0.3334P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1262
_refine_ls_wR_factor_ref         0.1328
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3122
_reflns_number_total             3988
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt01312f2.cif
_cod_data_source_block           ov_pthcudch
_cod_original_formula_sum        'C16 H19 Cu0.50 N3 O4'
_cod_database_code               7710685
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H,H,H) groups
2. Restrained distances
 N008-C4 \\sim N008-C4A
 with sigma of 0.02
 N00A-C3 \\sim N00A-C3A
 with sigma of 0.02
 C3-C4 \\sim C3A-C4A
 with sigma of 0.02
 C3-C2 \\sim C3A-C2A
 with sigma of 0.02
 C4-C1 \\sim C4A-C1A
 with sigma of 0.02
 C4-C7 \\sim C4A-C7A
 with sigma of 0.04
 C2-C7 \\sim C2A-C7A
 with sigma of 0.04
 C2-C6 \\sim C2A-C6A
 with sigma of 0.02
 C1-C6 \\sim C1A-C6A
 with sigma of 0.04
 C1-C7 \\sim C1A-C7A
 with sigma of 0.02
 C4-C2 \\sim C4A-C2A
 with sigma of 0.04
 C6-C7 \\sim C6A-C7A
 with sigma of 0.02
 N008-C3 \\sim N008-C3A
 with sigma of 0.04
 N008-C1 \\sim N008-C1A
 with sigma of 0.04
 N00A-C4 \\sim N00A-C4A
 with sigma of 0.04
 N00A-C2 \\sim N00A-C2A
 with sigma of 0.04
 C3-C1 \\sim C3A-C1A
 with sigma of 0.04
 C3-C6 \\sim C3A-C6A
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
Uanis(C7) = Uanis(C7A)
Uanis(C6) = Uanis(C6A)
Uanis(C2A) = Uanis(C2)
4. Others
 Sof(H00C)=Sof(H00D)=Sof(C4A)=Sof(H4A)=Sof(C3A)=Sof(H3A)=Sof(C1A)=Sof(H1AA)=
 Sof(H1AB)=Sof(C7A)=Sof(H7AA)=Sof(H7AB)=Sof(C6A)=Sof(H6AA)=Sof(H6AB)=Sof(C2A)=
 Sof(H2AA)=Sof(H2AB)=1-FVAR(1)
 Sof(H00A)=Sof(H00B)=Sof(C3)=Sof(H3)=Sof(C4)=Sof(H4)=Sof(C2)=Sof(H2A)=Sof(H2B)=
 Sof(C1)=Sof(H1A)=Sof(H1B)=Sof(C6)=Sof(H6A)=Sof(H6B)=Sof(C7)=Sof(H7A)=Sof(H7B)=
 FVAR(1)
5.a Ternary CH refined with riding coordinates:
 C3(H3), C4(H4), C4A(H4A), C3A(H3A)
5.b Secondary CH2 refined with riding coordinates:
 N00A(H00A,H00B), N00A(H00C,H00D), C00E(H00E,H00F), C2(H2A,H2B), C1(H1A,H1B),
 C6(H6A,H6B), C7(H7A,H7B), C1A(H1AA,H1AB), C7A(H7AA,H7AB), C6A(H6AA,H6AB),
 C2A(H2AA,H2AB)
5.c Aromatic/amide H refined with riding coordinates:
 C00H(H00H), C00I(H00I), C00J(H00J), C00K(H00K)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              71682
_shelx_hkl_checksum              90916
_shelx_fab_checksum              67190
_olex2_submission_special_instructions 'No special instructions were received'