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_7713899
_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         'C13 H14 N4 O Pt'
_chemical_formula_sum            'C13 H14 N4 O Pt'
_chemical_formula_weight         437.37
_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     iterative
_audit_creation_date             2023-05-15
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2023-08-30 deposited with the CCDC.	2023-09-04 downloaded from the CCDC.
;
_cell_angle_alpha                108.653(7)
_cell_angle_beta                 90.856(8)
_cell_angle_gamma                96.322(9)
_cell_formula_units_Z            6
_cell_length_a                   9.0752(19)
_cell_length_b                   12.639(3)
_cell_length_c                   18.870(3)
_cell_measurement_reflns_used    9769
_cell_measurement_temperature    173.0
_cell_measurement_theta_max      32.82
_cell_measurement_theta_min      2.59
_cell_volume                     2035.4(7)
_computing_cell_refinement       'SAINT V8.40B (Bruker AXS)'
_computing_data_collection       'APEX 3 (Bruker AXS)'
_computing_data_reduction        'SAINT V8.40B (Bruker AXS)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.5 (Bourhis et al., 2015)'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      173.0
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker Venture Photon 2'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0636
_diffrn_reflns_av_unetI/netI     0.0358
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            139345
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        33.000
_diffrn_reflns_theta_max         33.284
_diffrn_reflns_theta_min         2.346
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    10.338
_exptl_absorpt_correction_T_max  0.5685
_exptl_absorpt_correction_T_min  0.2516
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0884 before and 0.0673 after correction.
The Ratio of minimum to maximum transmission is 0.4426.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    2.141
_exptl_crystal_description       needle
_exptl_crystal_F_000             1236
_exptl_crystal_recrystallization_method 'water-ethanol mixture'
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.902
_refine_diff_density_min         -1.462
_refine_diff_density_rms         0.175
_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     514
_refine_ls_number_reflns         15567
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0444
_refine_ls_R_factor_gt           0.0308
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0245P)^2^+4.8496P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0643
_refine_ls_wR_factor_ref         0.0689
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12755
_reflns_number_total             15567
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt02039h2.cif
_cod_data_source_block           mo_21ov_ss_ptprohpyrr_2_0m
_cod_original_cell_volume        2035.3(7)
_cod_database_code               7713899
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.626
_shelx_estimated_absorpt_t_min   0.258
_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 O(H) groups
2.a Ternary CH refined with riding coordinates:
 C7B(H7B)
2.b Secondary CH2 refined with riding coordinates:
 C8B(H8Ba,H8Bb), C6B(H6Ba,H6Bb)
2.c Aromatic/amide H refined with riding coordinates:
 C2B(H2B), C9B(H9B), C5B(H5B), C3B(H3B), C12B(H12B), C11B(H11B), C1B(H1Ba),
 C13B(H13B)
2.d Idealised tetrahedral OH refined as rotating group:
 O1B(H1B)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 96 electrons were 
found in a volume of 175\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
4.5[H2O] per Asymmetric Unit 
which account for 90 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              63381
_shelx_fab_checksum              41997
_olex2_exptl_crystal_mounting_method
'mounted in Paratone oil with a Hampton nylon loop'
_olex2_submission_special_instructions 'No special instructions were received'