Design of a novel Pt(ii) complex to reverse cisplatin-induced resistance in lung cancer via a multi-mechanism
Jiang, Ming; Yang, Tongfu; Chu, Yong; Zhang, Zhenlei; Sun, Hongbin; Liang, Hong; Yang, Feng; Dalton Transactions  (2022) –; doi:10.1039/D1DT03964D

data_7709753
_publ_section_title
;
 Design of a novel Pt(ii) complex to reverse cisplatin-induced resistance
 in lung cancer via a multi-mechanism
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D1DT03964D
_journal_year                    2022
_chemical_formula_moiety         'C12 H11 N4 Pt0.5 S2, C12 H12 N4 Pt0.5 S2'
_chemical_formula_sum            'C24 H23 N8 Pt S4'
_chemical_formula_weight         746.83
_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     dual
_audit_creation_date             2022-01-06
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2022-01-06 deposited with the CCDC.	2022-02-28 downloaded from the CCDC.
;
_cell_angle_alpha                68.768(8)
_cell_angle_beta                 82.547(6)
_cell_angle_gamma                78.354(6)
_cell_formula_units_Z            2
_cell_length_a                   8.8378(6)
_cell_length_b                   11.4663(9)
_cell_length_c                   14.3741(12)
_cell_measurement_reflns_used    2135
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      21.2180
_cell_measurement_theta_min      3.8570
_cell_volume                     1327.24(19)
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      296.15
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 15.9784
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w     -3.00  87.00   1.00    1.00    --   17.93  57.00 120.00   90
  2  \w    -12.00  88.00   1.00    1.00    --   17.93  77.00-150.00  100
  3  \w    -20.00  60.00   1.00    1.00    --   17.93 -99.00   0.00   80
  4  \w    -51.00  38.00   1.00    1.00    --   17.93 -57.00-120.00   89
  5  \w    -55.00  62.00   1.00    1.00    --   17.93 -19.00 -60.00  117
  6  \w     -3.00  87.00   1.00    1.00    --   17.93  57.00   0.00   90
  7  \w    -96.00 -35.00   1.00    1.00    --  -19.72-178.00  30.00   61
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset/far, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0040231000
_diffrn_orient_matrix_UB_12      0.0035332000
_diffrn_orient_matrix_UB_13      0.0653451000
_diffrn_orient_matrix_UB_21      0.0514855000
_diffrn_orient_matrix_UB_22      0.0474442000
_diffrn_orient_matrix_UB_23      -0.0161139000
_diffrn_orient_matrix_UB_31      -0.0796518000
_diffrn_orient_matrix_UB_32      0.0845771000
_diffrn_orient_matrix_UB_33      -0.0185207000
_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  0.0787
_diffrn_reflns_av_unetI/netI     0.1018
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            14571
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.027
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_min         3.399
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.632
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.66673
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'metallic brownish brown'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   brownish
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.869
_exptl_crystal_description       block
_exptl_crystal_F_000             730
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.19
_refine_diff_density_max         1.387
_refine_diff_density_min         -0.969
_refine_diff_density_rms         0.158
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.997
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     380
_refine_ls_number_reflns         4688
_refine_ls_number_restraints     178
_refine_ls_restrained_S_all      0.983
_refine_ls_R_factor_all          0.0861
_refine_ls_R_factor_gt           0.0463
_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^)+(0.0183P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0773
_refine_ls_wR_factor_ref         0.0957
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2921
_reflns_number_total             4688
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt03964d2.cif
_cod_data_source_block           1
_cod_original_cell_volume        1327.25(19)
_cod_database_code               7709753
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.414
_shelx_estimated_absorpt_t_min   0.357
_reflns_odcompleteness_completeness 99.74
_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 N(H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C5A-C4A
 1.41 with sigma of 0.02
 C5-C4
 1.41 with sigma of 0.02
 N4-C6A = N4-C6
 1.43 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C6 \\sim C5 \\sim C10 \\sim C7 \\sim C4 \\sim C9 \\sim C8: within 2A with sigma
of 0.01 and sigma for terminal atoms of 0.02
C7A \\sim C8A \\sim C9A \\sim C10A \\sim C5A \\sim C4A \\sim C6A: within 2A
with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 C6, C7, C8, C9, C10, C5, C4
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C6A, C7A, C8A, C9A, C10A, C5A, C4A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 C4, C6, C5, C9, C8, C7, C10
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C7A, C6A, C5A, C4A, C10A, C9A, C8A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
5. Others
 Sof(H4b)=Sof(C6A)=Sof(C7A)=Sof(H7A)=Sof(C8A)=Sof(H8A)=Sof(C9A)=Sof(H9A)=
 Sof(C10A)=Sof(H10A)=Sof(C5A)=Sof(C4A)=Sof(H4Aa)=Sof(H4Ab)=Sof(H4Ac)=1-FVAR(1)
 Sof(H4a)=Sof(C6)=Sof(C5)=Sof(C10)=Sof(H10)=Sof(C9)=Sof(H9)=Sof(C8)=Sof(H8)=
 Sof(C7)=Sof(H7)=Sof(C4)=Sof(H4c)=Sof(H4d)=Sof(H4e)=FVAR(1)
6.a Aromatic/amide H refined with riding coordinates:
 N3AA(H3AA), N4(H4a), N4(H4b), N3(H3), C3(H3a), C5AA(H5AA), C1(H1), C2(H2),
 C7AA(H7AA), C8AA(H8AA), C0BA(H0BA), C1AA(H1AA), C3AA(H3Ab), C9AA(H9AA),
 C10(H10), C9(H9), C8(H8), C7(H7), C7A(H7A), C8A(H8A), C9A(H9A), C10A(H10A)
6.b Fitted hexagon refined as free rotating group:
 C6(C5,C10,C9,C8,C7), C6A(C7A,C8A,C9A,C10A,C5A)
6.c Idealised Me refined as rotating group:
 C12(H12a,H12b,H12c), C4(H4c,H4d,H4e), C4A(H4Aa,H4Ab,H4Ac)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.427
_oxdiff_exptl_absorpt_empirical_full_min 0.722