Water soluble palladium(ii) and platinum(ii) acyclic diaminocarbene complexes: solution behavior, DNA binding, and antiproliferative activity
Serebryanskaya, Tatiyana V.; Kinzhalov, Mikhail A.; Bakulev, Vladimir; Alekseev, Georgii; Andreeva, Anastasiya; Gushchin, Pavel V.; Protas, Aleksandra V.; Smirnov, Andrey S.; Panikorovskii, Taras L.; Lippmann, Petra; Ott, Ingo; Verbilo, Cyril M.; Zuraev, Alexander V.; Bunev, Alexander S.; Boyarskiy, Vadim P.; Kasyanenko, Nina A.; New Journal of Chemistry 44 (2020) 5762–5773; doi:10.1039/D0NJ00060D

data_7059343
_publ_section_title
;
 Water soluble palladium(ii) and platinum(ii) acyclic diaminocarbene
 complexes: solution behavior, DNA binding, and antiproliferative activity
;
_journal_issue                   15
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              5762
_journal_page_last               5773
_journal_paper_doi               10.1039/D0NJ00060D
_journal_volume                  44
_journal_year                    2020
_chemical_formula_moiety
'2(C30 H34 N6 Pd), 3(C H2 Br2), 4(Cl), 2(H2 O)'
_chemical_formula_sum            'C63 H78 Br6 Cl4 N12 O2 Pd2'
_chemical_formula_weight         1869.43
_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
_audit_creation_date             2020-01-27
_audit_creation_method
;
Olex2 1.3
(compiled Nov 21 2019 18:26:39 for OlexSys, GUI svn.r6003)
;
_audit_update_record
;
2020-01-27 deposited with the CCDC.	2020-02-27 downloaded from the CCDC.
;
_cell_angle_alpha                66.979(5)
_cell_angle_beta                 84.114(5)
_cell_angle_gamma                75.288(5)
_cell_formula_units_Z            1
_cell_length_a                   12.1819(8)
_cell_length_b                   12.3676(7)
_cell_length_c                   12.8999(7)
_cell_measurement_reflns_used    5750
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      76.0160
_cell_measurement_theta_min      3.7950
_cell_volume                     1730.08(19)
_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 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
;
Superflip  (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3829
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details
;
  1 omega  -68.00   32.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -      -41.1854   57.0000 -180.0000 100

  2 omega  -43.00   33.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -      -41.1854   38.0000  -30.0000 76

  3 omega -109.00  -18.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -      -41.1854  -57.0000   30.0000 91

  4 omega    5.00   67.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -       41.1854  -99.0000 -120.0000 62

  5 omega   75.00  130.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -       41.1854  178.0000  120.0000 55

  6 omega   36.00   67.00   1.0000   24.5000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -77.0000   60.0000 31

  7 omega   77.00  117.00   1.0000   24.5000
omega____ theta____ kappa____ phi______ frames
    -      112.0000 -125.0000  150.0000 40

  8 omega   45.00   96.00   1.0000   24.5000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -45.0000  -30.0000 51

  9 omega   42.00   69.00   1.0000   24.5000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -30.0000  -60.0000 27

 10 omega   41.00   83.00   1.0000   24.5000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -61.0000 -150.0000 42

 11 omega   64.00  109.00   1.0000   24.5000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -95.0000  -90.0000 45

 12 omega   97.00  161.00   1.0000   24.5000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   45.0000 -180.0000 64

 13 omega  102.00  168.00   1.0000   24.5000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   42.0000   44.0000 66

 14 omega   40.00  118.00   1.0000   24.5000
omega____ theta____ kappa____ phi______ frames
    -      112.0000 -125.0000   30.0000 78

 15 omega   40.00   81.00   1.0000   24.5000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -30.0000 -150.0000 41

 16 omega   65.00  108.00   1.0000   24.5000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -95.0000   30.0000 43

 17 omega   42.00   88.00   1.0000   24.5000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -30.0000 -120.0000 46

 18 omega   40.00   95.00   1.0000   24.5000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -45.0000   90.0000 55

 19 omega   37.00   88.00   1.0000   24.5000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -30.0000  150.0000 51

 20 omega   96.00  126.00   1.0000   24.5000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -61.0000 -150.0000 30

 21 omega   45.00  109.00   1.0000   24.5000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -95.0000 -150.0000 64

 22 omega   36.00   70.00   1.0000   24.5000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -77.0000   90.0000 34

 23 omega   84.00  126.00   1.0000   24.5000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -77.0000   90.0000 42

 24 omega   59.00  166.00   1.0000   24.5000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   15.0000  150.0000 107
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0701347000
_diffrn_orient_matrix_UB_12      0.1302558000
_diffrn_orient_matrix_UB_13      -0.0578340000
_diffrn_orient_matrix_UB_21      -0.1103489000
_diffrn_orient_matrix_UB_22      -0.0443328000
_diffrn_orient_matrix_UB_23      0.0369347000
_diffrn_orient_matrix_UB_31      -0.0003818000
_diffrn_orient_matrix_UB_32      0.0210489000
_diffrn_orient_matrix_UB_33      0.1101287000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0464
_diffrn_reflns_av_unetI/netI     0.0517
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            13229
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         69.992
_diffrn_reflns_theta_min         3.723
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    10.090
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.28293
_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            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.794
_exptl_crystal_description       prism
_exptl_crystal_F_000             926
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.575
_refine_diff_density_min         -1.241
_refine_diff_density_rms         0.223
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     425
_refine_ls_number_reflns         6529
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0776
_refine_ls_R_factor_gt           0.0707
_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^)+(0.1458P)^2^+4.2213P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1933
_refine_ls_wR_factor_ref         0.2070
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5674
_reflns_number_total             6529
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0nj00060d2.cif
_cod_data_source_block           km994
_cod_depositor_comments
;Adding full bibliography for 7059342--7059343.cif.

 Adding full bibliography for 7059342--7059343.cif.
;
_cod_original_cell_volume        1730.07(19)
_cod_database_code               7059343
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C63 Br6 H76 Cl4 N12 O2 Pd2'
_reflns_odcompleteness_completeness 99.90
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     72.42
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups, All N(H,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(C6) = Uanis(C7)
3. Others
 Fixed Sof: Br2S(0.5) Br3S(0.5) C2S(0.5) H2SA(0.5) H2SB(0.5) C3S(0.5)
 H3SA(0.5) H3SB(0.5) C1S(0.5) H1SA(0.5) H1SB(0.5)
4.a Free rotating group:
 O1S(H1SC,H1SD)
4.b Secondary CH2 refined with riding coordinates:
 N3(H3A,H3B), N6(H6A,H6B), C2S(H2SA,H2SB), C3S(H3SA,H3SB), C1S(H1SA,H1SB)
4.c Aromatic/amide H refined with riding coordinates:
 N1(H1), N2(H2), N4(H4), N5(H5), C5(H5A), C6(H6), C7(H7), C11(H11), C12(H12),
 C13(H13), C14(H14), C20(H20), C21(H21), C22(H22), C26(H26), C27(H27), C28(H28),
  C29(H29)
4.d Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C9(H9A,H9B,H9C), C19(H19A,H19B,H19C), C24(H24A,H24B,H24C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_submission_special_instructions 'No special instructions were received'