Platinum(ii) complexes of aryl guanidine-like derivatives as potential anticancer agents: between coordination and cyclometallation.
O'Sullivan, Patrick; Previtali, Viola; Twamley, Brendan; Marmion, Celine J.; McDonald, Aidan R.; Rozas, Isabel; RSC advances 15 (2025) 3427–3438; doi:10.1039/d5ra00310e

data_7249909
_publ_section_title
;
 Platinum(ii) complexes of aryl guanidine-like derivatives as potential
 anticancer agents: between coordination and cyclometallation.
;
_journal_issue                   5
_journal_name_full               'RSC advances'
_journal_page_first              3427
_journal_page_last               3438
_journal_paper_doi               10.1039/d5ra00310e
_journal_volume                  15
_journal_year                    2025
_chemical_formula_moiety         'C24 H30 I3 N9 O3 Pt2, C4 H10 O, 2(H2 O)'
_chemical_formula_sum            'C28 H44 I3 N9 O6 Pt2'
_chemical_formula_weight         1373.60
_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     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2024-11-26
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-12-19 deposited with the CCDC.	2025-01-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.2679(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.3526(11)
_cell_length_b                   15.6010(11)
_cell_length_c                   16.0353(12)
_cell_measurement_reflns_used    9967
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.095
_cell_measurement_theta_min      2.312
_cell_volume                     3830.1(5)
_computing_cell_refinement       'SAINT (Bruker, 2016)'
_computing_data_collection       'APEX 4 (Bruker, 2021) '
_computing_data_reduction        'SAINT (Bruker, 2015)'
_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    'SHELXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 8.33
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'Kappa diffractometer'
_diffrn_measurement_device_type  'Bruker Apex Kappa Duo Mo'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0676
_diffrn_reflns_av_unetI/netI     0.0390
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            71636
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.142
_diffrn_reflns_theta_min         1.824
_diffrn_source                   'standard sealed X-ray tube'
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_type              'Siemens, KFF Mo 2K -90 C'
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    9.766
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.4960
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS (Krause, 2015) was used for absorption correction.
wR2(int) was 0.0949 before and 0.0543 after correction.
The Ratio of minimum to maximum transmission is 0.6653.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            bronze
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    2.382
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       fragment
_exptl_crystal_F_000             2552
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.013
_refine_diff_density_max         1.951
_refine_diff_density_min         -2.060
_refine_diff_density_rms         0.200
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     448
_refine_ls_number_reflns         8483
_refine_ls_number_restraints     48
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0412
_refine_ls_R_factor_gt           0.0261
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0325P)^2^+4.8081P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0599
_refine_ls_wR_factor_ref         0.0668
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6996
_reflns_number_total             8483
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5ra00310e2.cif
_cod_data_source_block           tcd230
_cod_database_code               7249909
_shelx_shelxl_version_number     2019/1
_shelx_estimated_absorpt_t_max   0.884
_shelx_estimated_absorpt_t_min   0.322
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,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. Shared sites
{O23A, O23B}
3. Restrained distances
 C41B-C40 \\sim C41A-C40
 with sigma of 0.02
 O23A-C20 \\sim O23B-C20
 with sigma of 0.02
 O23B-C24B \\sim O23A-C24A
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(C41B) = Uanis(C41A)
Uanis(C24A) = Uanis(C24B)
Uanis(O23A) = Uanis(O23B)
5. Rigid body (RIGU) restrains
 C20, C24A, O23A, C24B, O23B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C37, C38, C40, O39, C41A, C41B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Sof(H40C)=Sof(H40D)=Sof(C41B)=Sof(H41D)=Sof(H41E)=Sof(H41F)=1-FVAR(1)
 Sof(H40A)=Sof(H40B)=Sof(C41A)=Sof(H41A)=Sof(H41B)=Sof(H41C)=FVAR(1)
 Sof(C24B)=Sof(H24D)=Sof(H24E)=Sof(H24F)=Sof(O23B)=1-FVAR(2)
 Sof(C24A)=Sof(H24A)=Sof(H24B)=Sof(H24C)=Sof(O23A)=FVAR(2)
7.a Riding coordinates:
 O1S(H1SA,H1SB), O2S(H2SA,H2SB)
7.b Secondary CH2 refined with riding coordinates:
 C38(H38A,H38B), C40(H40C,H40D), C40(H40A,H40B)
7.c Aromatic/amide H refined with riding coordinates:
 C7(H7), C9(H9), C10(H10), C19(H19), C21(H21), C22(H22), C30(H30), C31(H31),
 C33(H33), C34(H34), N1(H1), N4(H4), N13(H13), N16(H16), N25(H25), N26(H26),
 N28(H28)
7.d X=CH2 refined with riding coordinates:
 N2(H2A,H2B), N14(H14A,H14B)
7.e Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C36(H36A,H36B,H36C), C24A(H24A,H24B,H24C), C24B(H24D,
 H24E,H24F), C37(H37A,H37B,H37C), C41A(H41A,H41B,H41C), C41B(H41D,H41E,H41F)
;
_shelx_res_checksum              85148
_shelx_hkl_checksum              68279
_olex2_exptl_crystal_mounting_method 'mounted in oil on a MiTeGen microloop'
_olex2_submission_original_sample_id POS616
_olex2_submission_special_instructions 'No special instructions were received'