Ni(ii)/Cu(ii)/Zn(ii) 5,5-diethylbarbiturate complexes with 1,10-phenanthroline and 2,2'-dipyridylamine: synthesis, structures, DNA/BSA binding, nuclease activity, molecular docking, cellular uptake, cytotoxicity and the mode of cell death.
Yilmaz, Veysel T.; Icsel, Ceyda; Suyunova, Feruza; Aygun, Muhittin; Aztopal, Nazlihan; Ulukaya, Engin; Dalton transactions (Cambridge, England : 2003) 45 (2016) 10466–10479; doi:10.1039/c6dt01726f

data_7040189
_publ_section_title
;
 Ni(ii)/Cu(ii)/Zn(ii) 5,5-diethylbarbiturate complexes with
 1,10-phenanthroline and 2,2'-dipyridylamine: synthesis, structures,
 DNA/BSA binding, nuclease activity, molecular docking, cellular uptake,
 cytotoxicity and the mode of cell death.
;
_journal_issue                   25
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              10466
_journal_page_last               10479
_journal_paper_doi               10.1039/c6dt01726f
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety         'C36 H24 N6 Ni, C8 H11 N2 O3, Cl, 7(H2 O)'
_chemical_formula_sum            'C44 H49 Cl N8 Ni O10'
_chemical_formula_weight         944.05
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2016-04-14
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2016-05-01 deposited with the CCDC.
2016-05-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 109.180(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.4665(8)
_cell_length_b                   29.0250(16)
_cell_length_c                   14.1163(9)
_cell_measurement_reflns_used    4469
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.2070
_cell_measurement_theta_min      3.7010
_cell_volume                     4437.3(5)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0667
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_details
;
  1 omega   -3.00   91.00   1.0000   30.0600
omega____ theta____ kappa____ phi______ frames
    -       20.2271   57.0000   60.0000 94

  2 omega  -79.00   25.00   1.0000   30.0600
omega____ theta____ kappa____ phi______ frames
    -      -22.1802  -19.0000   90.0000 104
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0024434000
_diffrn_orient_matrix_UB_12      -0.0143415000
_diffrn_orient_matrix_UB_13      -0.0399954000
_diffrn_orient_matrix_UB_21      0.0633891000
_diffrn_orient_matrix_UB_22      0.0054409000
_diffrn_orient_matrix_UB_23      0.0110331000
_diffrn_orient_matrix_UB_31      0.0163317000
_diffrn_orient_matrix_UB_32      -0.0190159000
_diffrn_orient_matrix_UB_33      0.0333133000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0253
_diffrn_reflns_av_unetI/netI     0.0499
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            15302
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.371
_diffrn_reflns_theta_min         3.097
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.565
_exptl_absorpt_correction_T_max  0.882
_exptl_absorpt_correction_T_min  0.812
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Analytical numeric absorption correction using a multifaceted crystal
            model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.413
_exptl_crystal_description       block
_exptl_crystal_F_000             1976
_exptl_crystal_size_max          0.4877
_exptl_crystal_size_mid          0.4166
_exptl_crystal_size_min          0.2884
_refine_diff_density_max         0.330
_refine_diff_density_min         -0.355
_refine_diff_density_rms         0.047
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     620
_refine_ls_number_reflns         8977
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0757
_refine_ls_R_factor_gt           0.0477
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0482P)^2^+1.0155P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1058
_refine_ls_wR_factor_ref         0.1198
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6489
_reflns_number_total             8977
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt01726f2.cif
_cod_data_source_block           Compound_I
_cod_database_code               7040189
_chemical_oxdiff_formula         'C44 H46 Cl N8 Ni O10'
_reflns_odcompleteness_completeness 98.68
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C37) \\sim Ueq, Uanis(C38) \\sim Ueq: with sigma of 0.1 and sigma for
terminal atoms of 0.2
3. Others
 Sof(C39A)=Sof(H39A)=Sof(H39B)=Sof(C40A)=Sof(H40D)=Sof(H40E)=Sof(H40F)=1-FVAR(1)
 Sof(C40B)=Sof(H40A)=Sof(H40B)=Sof(H40C)=Sof(C39B)=Sof(H39C)=Sof(H39D)=FVAR(1)
4.a Free rotating group:
 O7W(H7WA,H7WB), O5W(H5WA,H5WB), O4W(H4WA,H4WB), O1W(H1WA,H1WB), O6W(H6WA,
 H6WB), O2W(H2WA,H2WB), O3W(H3WA,H3WB)
4.b Secondary CH2 refined with riding coordinates:
 C39A(H39A,H39B), C38(H38A,H38B), C39B(H39C,H39D)
4.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C5(H5), C6(H6), C8(H8), C9(H9), C10(H10), C13(H13),
 C14(H14), C15(H15), C17(H17), C18(H18), C20(H20), C21(H21), C22(H22), C25(H25),
  C26(H26), C27(H27), C29(H29), C30(H30), C32(H32), C33(H33), C34(H34), N7(H7)
4.d Idealised Me refined as rotating group:
 C40B(H40A,H40B,H40C), C37(H37A,H37B,H37C), C40A(H40D,H40E,H40F)
;
_shelx_shelxl_version_number     2014/7
_olex2_date_sample_data_collection 2015-09-30
_olex2_submission_special_instructions 'No special instructions were received'