Amidoxime platinum(ii) complexes: pH-dependent highly selective generation and cytotoxic activity
Bolotin, Dmitrii S.; Demakova, Marina Ya.; Legin, Anton A.; Suslonov, Vitaliy V.; Nazarov, Alexey A.; Jakupec, Michael A.; Keppler, Bernhard K.; Kukushkin, Vadim Yu.; New Journal of Chemistry 41 (2017) 6840–; doi:10.1039/C7NJ00982H

data_7059101
_publ_section_title
;
 Amidoxime platinum(ii) complexes: pH-dependent highly selective
 generation and cytotoxic activity
;
_journal_issue                   14
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              6840
_journal_paper_doi               10.1039/C7NJ00982H
_journal_volume                  41
_journal_year                    2017
_chemical_formula_moiety         'C5 H14 Cl2 N2 O2 Pt S'
_chemical_formula_sum            'C5 H14 Cl2 N2 O2 Pt S'
_chemical_formula_weight         432.23
_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   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2016-03-29
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2016-04-20 deposited with the CCDC.
2017-06-01 downloaded from the CCDC.
;
_cell_angle_alpha                99.166(8)
_cell_angle_beta                 91.628(8)
_cell_angle_gamma                114.355(9)
_cell_formula_units_Z            2
_cell_length_a                   7.7950(7)
_cell_length_b                   8.6094(9)
_cell_length_c                   9.4837(9)
_cell_measurement_reflns_used    2215
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.6990
_cell_measurement_theta_min      3.4170
_cell_volume                     569.27(11)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_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
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 16.2096
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details
;
  1 omega  -44.00   38.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -22.4081   57.0000  150.0000 82

  2 omega  -80.00  -38.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -22.4081  131.0000  -36.0000 42

  3 omega  -88.00  -19.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -22.4081  138.0000  138.0000 69

  4 omega  -90.00  -13.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -22.4081  -57.0000  -90.0000 77

  5 omega  -95.00   14.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -22.4081  -19.0000  -30.0000 109

  6 omega  -67.00  -42.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -22.4081  -77.0000   90.0000 25
;
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0481661000
_diffrn_orient_matrix_UB_12      0.0468355000
_diffrn_orient_matrix_UB_13      -0.0237167000
_diffrn_orient_matrix_UB_21      -0.0066840000
_diffrn_orient_matrix_UB_22      0.0319287000
_diffrn_orient_matrix_UB_23      0.0723726000
_diffrn_orient_matrix_UB_31      0.0878782000
_diffrn_orient_matrix_UB_32      0.0725568000
_diffrn_orient_matrix_UB_33      0.0016146000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0265
_diffrn_reflns_av_unetI/netI     0.0456
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            4656
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.500
_diffrn_reflns_theta_min         2.644
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    12.950
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.46761
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.522
_exptl_crystal_description       prism
_exptl_crystal_F_000             404
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.930
_refine_diff_density_min         -2.495
_refine_diff_density_rms         0.230
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     139
_refine_ls_number_reflns         2607
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0342
_refine_ls_R_factor_gt           0.0311
_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^)+(0.0232P)^2^+3.1833P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0657
_refine_ls_wR_factor_ref         0.0679
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2440
_reflns_number_total             2607
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7nj00982h2.cif
_cod_data_source_block           3b
_cod_original_cell_volume        569.26(10)
_cod_database_code               7059101
_chemical_oxdiff_formula         'Pt Cl2 S O2 N2 C5 H8'
_reflns_odcompleteness_completeness 99.93
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     28.51
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 N1-O1 \\sim N1-O1A
 with sigma of 0.0001
 N1-C1A \\sim N1-C1
 with sigma of 0.0001
 S1-O2 \\sim S1-O2A
 with sigma of 0.0001
 S1-C3 \\sim S1-C3A
 with sigma of 0.0001
 S1-C4 \\sim S1-C4A
 with sigma of 0.0001
 C1A-C2A \\sim C2-C1
 with sigma of 0.0001
3. Uiso/Uaniso restraints and constraints
Uanis(C3A) = Uanis(C4A)
Uanis(O1A) = Uanis(O1)
Uanis(N2A) = Uanis(N2)
Uanis(C1A) = Uanis(C1)
Uanis(O2) = Uanis(S1) = Uanis(O2A)
Uanis(C3) = Uanis(C4) = Uanis(S1)
Uanis(C2) = Uanis(C2A)
Uanis(C5) = Uanis(C5A)
4. Others
 Sof(O1A)=Sof(H1A)=Sof(O2A)=Sof(N2A)=Sof(H2AA)=Sof(H2AB)=Sof(C1A)=Sof(C2A)=
 Sof(H2AC)=Sof(H2AD)=Sof(C3A)=Sof(H3AA)=Sof(H3AB)=Sof(H3AC)=Sof(C4A)=Sof(H4AA)=
 Sof(H4AB)=Sof(H4AC)=Sof(C5A)=Sof(H5AA)=Sof(H5AB)=Sof(H5AC)=1-FVAR(1)
 Sof(O2)=Sof(O1)=Sof(H1)=Sof(N2)=Sof(H2A)=Sof(H2B)=Sof(C1)=Sof(C3)=Sof(H3A)=
 Sof(H3B)=Sof(H3C)=Sof(C4)=Sof(H4A)=Sof(H4B)=Sof(H4C)=Sof(C2)=Sof(H2C)=Sof(H2D)=
 Sof(C5)=Sof(H5A)=Sof(H5B)=Sof(H5C)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C2A(H2AC,H2AD), C2(H2C,H2D)
5.b X=CH2 refined with riding coordinates:
 N2A(H2AA,H2AB), N2(H2A,H2B)
5.c Idealised Me refined as rotating group:
 C3A(H3AA,H3AB,H3AC), C4A(H4AA,H4AB,H4AC), C5A(H5AA,H5AB,H5AC), C3(H3A,H3B,
 H3C), C4(H4A,H4B,H4C), C5(H5A,H5B,H5C)
5.d Idealised tetrahedral OH refined as rotating group:
 O1A(H1A), O1(H1)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'