Synthesis, crystal structure, cytotoxicity and action mechanism of Zn(ii) and Mn(ii) complexes with 4-([2,2′:6′,2′′-terpyridin]-4′-yl)-N,N-diethylaniline as a ligand
Zou, Hua-Hong; Wei, Jun-Guang; Qin, Xiao-Huan; Mo, Shun-Gui; Qin, Qi-Pin; Liu, Yan-Cheng; Liang, Fu-Pei; Zhang, Yun-Liang; Chen, Zhen-Feng; Med. Chem. Commun. 7 (2016) 1132–; doi:10.1039/C6MD00098C

data_7118954
_publ_section_title
;
 Synthesis, crystal structure, cytotoxicity and action mechanism of Zn(ii)
 and Mn(ii) complexes with
 4-([2,2&#x2032;:6&#x2032;,2&#x2032;&#x2032;-terpyridin]-4&#x2032;-yl)-N,N-diethylaniline
 as a ligand
;
_journal_issue                   6
_journal_name_full               'Med. Chem. Commun.'
_journal_page_first              1132
_journal_paper_doi               10.1039/C6MD00098C
_journal_volume                  7
_journal_year                    2016
_chemical_formula_moiety         'C50 H48 Mn N8, 2(Cl O4)'
_chemical_formula_sum            'C50 H48 Cl2 Mn N8 O8'
_chemical_formula_weight         1014.83
_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
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_audit_creation_date             2015-11-07
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2015-12-15 deposited with the CCDC.
2016-04-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 108.185(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.0394(4)
_cell_length_b                   15.1400(4)
_cell_length_c                   17.3328(5)
_cell_measurement_reflns_used    8456
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.3390
_cell_measurement_theta_min      3.5100
_cell_volume                     4746.7(2)
_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  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_temperature      296.15
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0233
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.9984
_diffrn_measured_fraction_theta_max 0.9984
_diffrn_measurement_details
;
  1 omega  -44.00   54.00   1.0000   34.3150
omega____ theta____ kappa____ phi______ frames
    -      -18.6266   38.0000   30.0000 98

  2 omega  -16.00   46.00   1.0000   34.3150
omega____ theta____ kappa____ phi______ frames
    -       18.7048  -99.0000  -60.0000 62

  3 omega   31.00   61.00   1.0000   34.3150
omega____ theta____ kappa____ phi______ frames
    -       18.7048  -99.0000   30.0000 30

  4 omega  -43.00    4.00   1.0000   34.3150
omega____ theta____ kappa____ phi______ frames
    -      -18.6266  -77.0000 -180.0000 47

  5 omega  -74.00  -49.00   1.0000   34.3150
omega____ theta____ kappa____ phi______ frames
    -      -18.6266 -178.0000    0.0000 25
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0329017000
_diffrn_orient_matrix_UB_12      -0.0238733000
_diffrn_orient_matrix_UB_13      -0.0033270000
_diffrn_orient_matrix_UB_21      -0.0198512000
_diffrn_orient_matrix_UB_22      0.0402346000
_diffrn_orient_matrix_UB_23      -0.0040196000
_diffrn_orient_matrix_UB_31      -0.0079427000
_diffrn_orient_matrix_UB_32      -0.0018699000
_diffrn_orient_matrix_UB_33      -0.0427659000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0302
_diffrn_reflns_av_unetI/netI     0.0407
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            24898
_diffrn_reflns_theta_full        26.3715
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         2.92
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.455
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.67443
_exptl_absorpt_correction_type   multi-scan
_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)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.4200
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2111.4713
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.0016
_refine_diff_density_min         -0.7871
_refine_diff_density_rms         0.0872
_refine_ls_d_res_high            0.8000
_refine_ls_d_res_low             6.9831
_refine_ls_goodness_of_fit_ref   1.0801
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    84
_refine_ls_number_parameters     625
_refine_ls_number_reflns         9698
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0801
_refine_ls_R_factor_all          0.0924
_refine_ls_R_factor_gt           0.0672
_refine_ls_shift/su_max          0.0006
_refine_ls_shift/su_mean         0.0001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1084P)^2^+4.7477P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1939
_refine_ls_wR_factor_ref         0.2230
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              22
_reflns_limit_h_min              -23
_reflns_limit_k_max              18
_reflns_limit_k_min              0
_reflns_limit_l_max              21
_reflns_limit_l_min              0
_reflns_number_gt                6918
_reflns_number_total             9698
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            c6md00098c2.cif
_cod_data_source_block           47
_cod_depositor_comments
'Adding full bibliography for 7118953--7118954.cif.'
_cod_database_code               7118954
_reflns_odcompleteness_completeness 99.79
_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
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C24(H24a,H24b), C47(H47a,H47b), C22(H22a,H22b), C51(H51a,H51b)
2.b Aromatic/amide H refined with riding coordinates:
 C34(H34), C21(H21), C32(H32), C9(H9), C46(H46), C20(H20), C7(H7), C43(H43),
 C45(H45), C17(H17), C29(H29), C37(H37), C42(H42), C18(H18), C40(H40), C26(H26),
  C39(H39), C28(H28), C4(H4), C27(H27), C38(H38), C14(H14), C2(H2), C15(H15),
 C12(H12), C13(H13), C1(H1), C3(H3)
2.c Idealised Me refined as rotating group:
 C23(H23a,H23b,H23c), C50(H50a,H50b,H50c), C52(H52a,H52b,H52c), C25(H25a,H25b,
 H25c)
;
_olex2_submission_special_instructions 'No special instructions were received'