Spectroscopic and computational study of the interaction of Pt(II) pyrrole-imine chelates with human serum albumin
Sookai, Sheldon; Munro, Orde Q.; Dalton Transactions  (2023) –; doi:10.1039/D3DT02039H

data_7713898
_publ_section_title
;
 Spectroscopic and computational study of the interaction of Pt(II)
 pyrrole-imine chelates with human serum albumin
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT02039H
_journal_year                    2023
_chemical_formula_moiety         'C15 H18 N4 Pt'
_chemical_formula_sum            'C15 H18 N4 Pt'
_chemical_formula_weight         449.42
_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             2021-09-10
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2023-08-30 deposited with the CCDC.	2023-09-04 downloaded from the CCDC.
;
_cell_angle_alpha                103.788(2)
_cell_angle_beta                 104.926(2)
_cell_angle_gamma                107.795(2)
_cell_formula_units_Z            8
_cell_length_a                   13.7803(5)
_cell_length_b                   15.2877(5)
_cell_length_c                   16.8165(6)
_cell_measurement_reflns_used    9856
_cell_measurement_temperature    173.15
_cell_measurement_theta_max      24.75
_cell_measurement_theta_min      2.25
_cell_volume                     3059.8(2)
_computing_cell_refinement       'SAINT V8.34A (Bruker AXS)'
_computing_data_collection       'APEX 2 (Bruker AXS)'
_computing_data_reduction        'SAINT V8.34A (Bruker AXS)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      173.15
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0665
_diffrn_reflns_av_unetI/netI     0.0536
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            113600
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        30.500
_diffrn_reflns_theta_max         30.565
_diffrn_reflns_theta_min         1.490
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    9.167
_exptl_absorpt_correction_T_max  0.568
_exptl_absorpt_correction_T_min  0.222
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.951
_exptl_crystal_description       blocky
_exptl_crystal_F_000             1712
_exptl_crystal_size_max          0.227
_exptl_crystal_size_mid          0.161
_exptl_crystal_size_min          0.076
_refine_diff_density_max         0.961
_refine_diff_density_min         -1.099
_refine_diff_density_rms         0.173
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.004
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     729
_refine_ls_number_reflns         18723
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.004
_refine_ls_R_factor_all          0.0586
_refine_ls_R_factor_gt           0.0327
_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^)+(0.0192P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0527
_refine_ls_wR_factor_ref         0.0590
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13600
_reflns_number_total             18723
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt02039h2.cif
_cod_data_source_block           21ma_SS_PtMe2PrPyrr
_cod_original_cell_volume        3059.76(19)
_cod_database_code               7713898
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.543
_shelx_estimated_absorpt_t_min   0.230
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C6A(H6AA,H6AB), C8A(H8AA,H8AB), C6B(H6BA,H6BB), C8B(H8BA,H8BB), C6C(H6CA,
 H6CB), C8C(H8CA,H8CB), C6D(H6DA,H6DB), C8D(H8DA,H8DB)
2.b Aromatic/amide H refined with riding coordinates:
 C1A(H1A), C2A(H2A), C3A(H3A), C5A(H5A), C9A(H9A), C11A(H11A), C12A(H12A),
 C13A(H13A), C1B(H1B), C2B(H2B), C3B(H3B), C5B(H5B), C9B(H9B), C11B(H11B),
 C12B(H12B), C13B(H13B), C1C(H1C), C2C(H2C), C3C(H3C), C5C(H5C), C9C(H9C),
 C11C(H11C), C12C(H12C), C13C(H13C), C1D(H1D), C2D(H2D), C3D(H3D), C5D(H5D),
 C9D(H9D), C11D(H11D), C12D(H12D), C13D(H13D)
2.c Idealised Me refined as rotating group:
 C14A(H14A,H14B,H14C), C15A(H15A,H15B,H15C), C14B(H14D,H14E,H14F), C15B(H15D,
 H15E,H15F), C14C(H14G,H14H,H14I), C15C(H15G,H15H,H15I), C14D(H14J,H14K,H14L),
 C15D(H15J,H15K,H15L)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 27 electrons were 
found in a volume of 229\%A^3^ in 3 voids per unit cell. 
This is consistent with the presence of 
1.2[H2O] per Asymmetric Unit 
which account for 24 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              83382
_shelx_fab_checksum              85594
_olex2_submission_special_instructions 'No special instructions were received'