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_7059342
_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         'C30 H34 N6 Pt, 2(Cl), H2 O'
_chemical_formula_sum            'C30 H36 Cl2 N6 O Pt'
_chemical_formula_weight         762.64
_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
_audit_creation_date             2016-09-01
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2016-09-01 deposited with the CCDC.	2020-02-27 downloaded from the CCDC.
;
_cell_angle_alpha                66.866(3)
_cell_angle_beta                 84.414(3)
_cell_angle_gamma                75.822(3)
_cell_formula_units_Z            2
_cell_length_a                   12.1790(6)
_cell_length_b                   12.3643(3)
_cell_length_c                   12.9592(4)
_cell_measurement_reflns_used    8336
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      75.8780
_cell_measurement_theta_min      3.9000
_cell_volume                     1739.88(12)
_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, 2008)'
_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 0.998
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details
;
  1 omega -124.00  -34.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.3104  178.0000  -90.0000 90

  2 omega -113.00  -13.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.3104  -57.0000 -180.0000 100

  3 omega  -48.00   33.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.3104   38.0000  -30.0000 81

  4 omega -116.00  -86.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.3104  -38.0000   60.0000 30

  5 omega  -83.00  -33.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.3104  -38.0000   60.0000 50

  6 omega   79.00  128.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       41.3104 -178.0000  -90.0000 49

  7 omega   87.00  171.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   61.0000 -120.0000 84

  8 omega   39.00   94.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -45.0000 -120.0000 55

  9 omega  150.00  176.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   61.0000 -180.0000 26

 10 omega   34.00   76.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -95.0000 -120.0000 42

 11 omega   91.00  178.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   30.0000  -30.0000 87

 12 omega   70.00   98.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -45.0000    0.0000 28

 13 omega   63.00   97.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -45.0000  120.0000 34

 14 omega   47.00   73.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -45.0000 -150.0000 26

 15 omega   71.00   97.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -95.0000    0.0000 26

 16 omega   84.00  120.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000 -125.0000 -180.0000 36

 17 omega   77.00  103.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -95.0000  -60.0000 26

 18 omega  145.00  171.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  125.0000 -120.0000 26

 19 omega   35.00   62.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -95.0000    0.0000 27

 20 omega   39.00   65.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000 -125.0000  -30.0000 26

 21 omega   74.00  119.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000 -125.0000  -30.0000 45

 22 omega   96.00  164.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  125.0000 -180.0000 68

 23 omega  103.00  128.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  125.0000 -120.0000 25

 24 omega   37.00   65.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -30.0000   30.0000 28

 25 omega   38.00   85.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -30.0000  -60.0000 47

 26 omega   58.00   83.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -77.0000 -120.0000 25

 27 omega   65.00  105.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -95.0000 -150.0000 40

 28 omega   63.00  100.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -95.0000   90.0000 37

 29 omega  127.00  174.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   45.0000    0.0000 47

 30 omega   83.00  141.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   61.0000  120.0000 58

 31 omega   96.00  121.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000 -125.0000   30.0000 25

 32 omega   74.00  109.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -95.0000   30.0000 35

 33 omega   40.00  121.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000 -125.0000 -150.0000 81

 34 omega  125.00  158.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  125.0000  -90.0000 33

 35 omega   97.00  140.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -61.0000 -120.0000 43

 36 omega   59.00   89.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -45.0000  -30.0000 30
;
_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      0.1303528000
_diffrn_orient_matrix_UB_12      -0.0293138000
_diffrn_orient_matrix_UB_13      0.0037042000
_diffrn_orient_matrix_UB_21      -0.0054664000
_diffrn_orient_matrix_UB_22      0.0546816000
_diffrn_orient_matrix_UB_23      0.0891587000
_diffrn_orient_matrix_UB_31      -0.0001770000
_diffrn_orient_matrix_UB_32      -0.1244804000
_diffrn_orient_matrix_UB_33      0.0935336000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0684
_diffrn_reflns_av_unetI/netI     0.0683
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            16339
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.493
_diffrn_reflns_theta_min         3.709
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    9.189
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.14145
_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            'translucent colorless'
_exptl_crystal_density_diffrn    1.456
_exptl_crystal_description       prism
_exptl_crystal_F_000             756
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.15
_refine_diff_density_max         2.534
_refine_diff_density_min         -1.510
_refine_diff_density_rms         0.282
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     326
_refine_ls_number_reflns         6868
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0706
_refine_ls_R_factor_gt           0.0643
_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^)+(0.1286P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1723
_refine_ls_wR_factor_ref         0.1763
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6041
_reflns_number_total             6868
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0nj00060d2.cif
_cod_data_source_block           km-1002
_cod_depositor_comments
;Adding full bibliography for 7059342--7059343.cif.

 Adding full bibliography for 7059342--7059343.cif.
;
_cod_database_code               7059342
_chemical_oxdiff_formula         'Pt C20 Cl N5'
_reflns_odcompleteness_completeness 99.25
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     75.12
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(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(C1) = Uanis(C25) = Uanis(C16)
Uanis(C7) = Uanis(C6)
Uanis(C25) = Uanis(C28) = Uanis(C30) = Uanis(C29)
Uanis(N2) = Uanis(N1)
3.a Free rotating group:
 O7(H7A,H7B)
3.b Secondary CH2 refined with riding coordinates:
 N6(H6A,H6B), N3(H3A,H3B)
3.c Aromatic/amide H refined with riding coordinates:
 N1(H1), N2(H2), C28(H28), C6(H6), N4(H4), C14(H14), N5(H5), C27(H27),
 C11(H11), C13(H13), C21(H21), C7(H7), C12(H12), C26(H26), C20(H20), C22(H22),
 C29(H29), C5(H5A)
3.d Idealised Me refined as rotating group:
 C24(H24A,H24B,H24C), C19(H19A,H19B,H19C), C9(H9A,H9B,H9C), C4(H4A,H4B,H4C)
;
_platon_squeeze_void_probe_radius 1.20
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'