Platinum-based metal complexes as chloride transporters that trigger apoptosis.
Wang, Patrick; Fares, Mohamed; Eladwy, Radwa A.; Bhuyan, Deep J.; Wu, Xin; Lewis, William; Loeb, Stephen J.; Macreadie, Lauren K.; Gale, Philip A.; Chemical science 15 (2024) 11584–11593; doi:10.1039/d4sc02115k

data_1572004
_publ_section_title
;
 Platinum-based metal complexes as chloride transporters that trigger
 apoptosis.
;
_journal_issue                   29
_journal_name_full               'Chemical science'
_journal_page_first              11584
_journal_page_last               11593
_journal_paper_doi               10.1039/d4sc02115k
_journal_volume                  15
_journal_year                    2024
_chemical_formula_moiety         'C48 H52 N12 O4 Pt, 2(B F4)'
_chemical_formula_sum            'C48 H52 B2 F8 N12 O4 Pt'
_chemical_formula_weight         1229.72
_chemical_name_systematic        'Ethyl platinum complex'
_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   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2024-02-07
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2024-02-16 deposited with the CCDC.	2024-06-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.529(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.4301(13)
_cell_length_b                   19.8030(14)
_cell_length_c                   11.2570(9)
_cell_measurement_reflns_used    5395
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.7060
_cell_measurement_theta_min      2.0520
_cell_volume                     2477.3(4)
_computing_cell_refinement       'CrysAlisPro 1.171.42.67a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.67a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.67a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2930
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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    -26.00  71.00   1.00   45.00    --  -11.94  19.00  90.00   97
  2  \w    -15.00  30.00   1.00   45.00    --  -11.94 -99.00 -90.00   45
  3  \w    -15.00  57.00   1.00   45.00    --   14.91 -99.00 -30.00   72
  4  \w     37.00 105.00   1.00   45.00    --   14.91-178.00 -60.00   68
  5  \w    -14.00  92.00   1.00   45.00    --   14.91  38.00  90.00  106
  6  \w    -89.00  17.00   1.00   45.00    --  -11.94 -38.00  90.00  106
  7  \w    -52.00   3.00   1.00   45.00    --  -11.94  91.00  31.00   55
  8  \w    -15.00  30.00   1.00   45.00    --  -11.94 -99.00-180.00   45
  9  \w    -15.00  24.00   1.00   45.00    --   14.91 -99.00 120.00   39
 10  \w    -68.00  26.00   1.00   45.00    --   14.91 -19.00  90.00   94
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0281019000
_diffrn_orient_matrix_UB_12      0.0298633000
_diffrn_orient_matrix_UB_13      0.0143295000
_diffrn_orient_matrix_UB_21      -0.0572154000
_diffrn_orient_matrix_UB_22      -0.0136881000
_diffrn_orient_matrix_UB_23      -0.0278469000
_diffrn_orient_matrix_UB_31      -0.0038922000
_diffrn_orient_matrix_UB_32      -0.0142569000
_diffrn_orient_matrix_UB_33      0.0567209000
_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  0.2077
_diffrn_reflns_av_unetI/netI     0.1094
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            37769
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.024
_diffrn_reflns_theta_max         25.024
_diffrn_reflns_theta_min         1.832
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.920
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.568
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.67a (Rigaku Oxford Diffraction, 2022)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear yellowish yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.649
_exptl_crystal_description       block
_exptl_crystal_F_000             1232
_exptl_crystal_preparation
'Heating platinum complex with isoquinoline urea derivative in acetonitrile'
_exptl_crystal_recrystallization_method 'From DMF/ether'
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.656
_refine_diff_density_min         -2.608
_refine_diff_density_rms         0.180
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.003
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     354
_refine_ls_number_reflns         4374
_refine_ls_number_restraints     144
_refine_ls_restrained_S_all      0.988
_refine_ls_R_factor_all          0.0970
_refine_ls_R_factor_gt           0.0540
_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^)+(0.0557P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1139
_refine_ls_wR_factor_ref         0.1342
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2787
_reflns_number_total             4374
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc02115k2.cif
_cod_data_source_block           pag22_s2618_sn994-2_auto
_cod_depositor_comments
'Adding full bibliography for 1572002--1572006.cif.'
_cod_database_code               1572004
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C48H52B2F8N12O4Pt
_shelx_estimated_absorpt_t_max   0.971
_shelx_estimated_absorpt_t_min   0.868
_olex2_refinement_description
;
1. Uiso/Uaniso restraints and constraints
N31 \\sim C32 \\sim C33 \\sim C38 \\sim C39 \\sim C40: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.2 within 2A
N1 \\sim C2 \\sim C3 \\sim C8 \\sim C9 \\sim C10: within 2A with sigma of 0.01
and sigma for terminal atoms of 0.02 within 2A
2. Rigid body (RIGU) restrains
 N31, C32, C33, C38, C39, C40
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N1, C2, C3, C8, C9, C10
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3.a Secondary CH2 refined with riding coordinates:
 C15(H15A,H15B), C45(H45A,H45B)
3.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C5(H5), C6(H6), C7(H7), C9(H9), C10(H10), C32(H32), C35(H35),
 C36(H36), C37(H37), C39(H39), C40(H40)
3.c Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C46(H46A,H46B,H46C)
;
_shelx_res_checksum              11318
_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 3.079
_oxdiff_exptl_absorpt_empirical_full_min 0.218