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_7709749
_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         'C14 H18 N8 Pt S4'
_chemical_formula_sum            'C14 H18 N8 Pt S4'
_chemical_formula_weight         621.69
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-01-05
_audit_creation_method
;
Olex2 1.5-beta
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_audit_update_record
;
2022-01-06 deposited with the CCDC.	2022-02-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.532(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.8524(2)
_cell_length_b                   4.00670(10)
_cell_length_c                   27.1392(6)
_cell_measurement_reflns_used    2700
_cell_measurement_temperature    270(2)
_cell_measurement_theta_max      74.0970
_cell_measurement_theta_min      4.9880
_cell_volume                     962.56(4)
_computing_cell_refinement       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.5-beta (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-beta (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      270(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.946
_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    135.00 168.00   0.50    1.78    --  110.12  37.00  16.00   66
  2  \w     98.00 129.00   0.50    1.78    --  110.12  37.00  16.00   62
  3  \w    153.00 178.00   0.50    1.78    --  110.12  61.00 150.00   50
  4  \w     82.00 140.00   0.50    1.78    --  110.12  61.00 150.00  116
  5  \w     69.00 121.00   0.50    0.57    --   39.95 178.00 150.00  104
  6  \w    -36.00  37.00   0.50    0.57    --  -39.95  37.00  16.00  146
  7  \w    -71.00 -27.00   0.50    1.78    --  -94.50  61.00 120.00   88
  8  \w    -44.00 -17.00   0.50    1.78    --  -94.50  45.00 150.00   54
  9  \w    -49.00 -24.00   0.50    1.78    --  -94.50  45.00 120.00   50
 10  \w    -42.00 -17.00   0.50    1.78    --  -94.50  37.00  16.00   50
 11  \w    -44.00 -17.00   0.50    1.78    --  -94.50  45.00-150.00   54
 12  \w    -46.00 -18.00   0.50    1.78    --  -94.50  45.00-180.00   56
 13  \w   -121.00 -11.00   0.50    0.57    --  -39.95 -37.00-139.00  220
 14  \w   -171.00 -74.00   0.50    1.78    --  -94.50 -37.00-139.00  194
 15  \w     80.00 105.00   0.50    1.78    --  110.12 -77.00   0.00   50
 16  \w     38.00  65.00   0.50    1.78    --  110.12 -61.00 -60.00   54
 17  \w     36.00  68.00   0.50    1.78    --  110.12 -61.00 -90.00   64
 18  \w     75.00 106.00   0.50    1.78    --  110.12 -77.00-150.00   62
 19  \w     35.00  69.00   0.50    1.78    --  110.12 -61.00-180.00   68
 20  \w     43.00  71.00   0.50    1.78    --  110.12 -61.00-150.00   56
 21  \w     39.00  64.00   0.50    1.78    --  110.12 -61.00-120.00   50
 22  \w     61.00 106.00   0.50    1.78    --  110.12 -77.00 -90.00   90
 23  \w     35.00  60.00   0.50    1.78    --  110.12 -61.00 150.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0008606000
_diffrn_orient_matrix_UB_12      -0.0915107000
_diffrn_orient_matrix_UB_13      0.0551341000
_diffrn_orient_matrix_UB_21      0.1565133000
_diffrn_orient_matrix_UB_22      0.1624307000
_diffrn_orient_matrix_UB_23      0.0066295000
_diffrn_orient_matrix_UB_31      -0.0759291000
_diffrn_orient_matrix_UB_32      0.3364017000
_diffrn_orient_matrix_UB_33      0.0118224000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0230
_diffrn_reflns_av_unetI/netI     0.0301
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.946
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       4
_diffrn_reflns_limit_k_min       -4
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            4408
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.946
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.258
_diffrn_reflns_theta_min         3.257
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    17.855
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.16743
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
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    2.145
_exptl_crystal_description       plate
_exptl_crystal_F_000             600
_exptl_crystal_preparation       'heated 343 k'
_exptl_crystal_recrystallization_method 'heated 343 k'
_exptl_crystal_size_max          0.65
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.907
_refine_diff_density_min         -1.923
_refine_diff_density_rms         0.132
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.116
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     126
_refine_ls_number_reflns         1836
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.116
_refine_ls_R_factor_all          0.0306
_refine_ls_R_factor_gt           0.0282
_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^)+(0.0480P)^2^+0.3971P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0757
_refine_ls_wR_factor_ref         0.0778
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1670
_reflns_number_total             1836
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt03964d2.cif
_cod_data_source_block           20211230-yf-jm-pt
_cod_database_code               7709749
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C32 H48 N12 Pt2 S8 '
_shelx_estimated_absorpt_t_max   0.189
_shelx_estimated_absorpt_t_min   0.030
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C00A(H00A), C00D(H00H), C00E(H00I)
2.b Idealised Me refined as rotating group:
 C00B(H00B,H00C,H00D), C00C(H00E,H00F,H00G)
;
_shelx_res_checksum              46765
_shelx_hkl_checksum              67300
_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 4.597
_oxdiff_exptl_absorpt_empirical_full_min 0.524