Contrasting effects of ethylene and propylene linkers on the kinetic stability of water-soluble near-infrared-absorbing diradical-Pt<sup>II</sup> complexes.
Sawamura, Ryota; Horii, Satoshi; Tamura, Kousaku; Tsuchiya, Satoshi; Iki, Nobuhiko; Dalton transactions (Cambridge, England : 2003) 54 (2025) 13598–13608; doi:10.1039/d5dt01798j

data_7719277
_publ_section_title
;
 Contrasting effects of ethylene and propylene linkers on the kinetic
 stability of water-soluble near-infrared-absorbing
 diradical-Pt<sup>II</sup> complexes.
;
_journal_issue                   36
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              13598
_journal_page_last               13608
_journal_paper_doi               10.1039/d5dt01798j
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'C15 H14 N4 O6 Pt S2, 2(C20 H20 P), 3(H2 O)'
_chemical_formula_sum            'C55 H60 N4 O9 P2 Pt S2'
_chemical_formula_weight         1242.22
_chemical_properties_physical    Air-sensitive
_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   mixed
_atom_sites_solution_primary     dual
_audit_block_doi                 10.5517/ccdc.csd.cc2mzchh
_audit_creation_date             2025-04-08
_audit_creation_method
;
Olex2 1.5
(compiled 2025.03.04 svn.red2d20d0 for OlexSys, GUI svn.r7188)
;
_audit_update_record
;
2025-04-09 deposited with the CCDC.	2025-08-18 downloaded from the CCDC.
;
_cell_angle_alpha                70.6470(10)
_cell_angle_beta                 70.0150(10)
_cell_angle_gamma                64.7980(10)
_cell_formula_units_Z            2
_cell_length_a                   12.9759(4)
_cell_length_b                   13.0258(4)
_cell_length_c                   18.4137(6)
_cell_measurement_reflns_used    9983
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.04
_cell_measurement_theta_min      2.38
_cell_volume                     2582.49(14)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 5.6
_diffrn_detector_type            'Bruker SMART CCD 6000 area detector'
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART CCD 6000 area detector'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.0452
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            9106
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.067
_diffrn_reflns_theta_min         1.898
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_target            Mo
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.922
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.5209
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 TWINABS-2012/1 (Bruker,2012) was used for absorption correction.
 
For component 1:
 wR2(int) was 0.0951 before and 0.0374 after correction.
 
For component 2:
 wR2(int) was 0.1175 before and 0.0365 after correction.
 The Ratio of minimum to maximum transmission is 0.70.

Final HKLF 4 output contains 76963 reflections, Rint = 0.1119
 (54151 with I > 3sig(I), Rint = 0.0528)
;
_exptl_crystal_colour            violet
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.597
_exptl_crystal_description       'rect. Prism'
_exptl_crystal_F_000             1260
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: dimethylsulfoxide and pure water'
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.019
_refine_diff_density_min         -2.877
_refine_diff_density_rms         0.193
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.168
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     670
_refine_ls_number_reflns         9106
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.168
_refine_ls_R_factor_all          0.0478
_refine_ls_R_factor_gt           0.0372
_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^)+(0.0555P)^2^+17.8175P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1148
_refine_ls_wR_factor_ref         0.1211
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8729
_reflns_number_total             9106
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt01798j2.cif
_cod_data_source_block           250328ptpabs_re_twin
_cod_depositor_comments
'Adding full bibliography for 7719276--7719277.cif.'
_cod_database_code               7719277
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.668
_shelx_estimated_absorpt_t_min   0.529
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.9138(16)
 0.0862(16)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
3.a Free rotating group:
 O7(H7A,H7B), O8(H8A,H8B), O9(H9A,H9B)
3.b Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B), C15(H15A,H15B), C34(H34A,H34B), C54(H54A,H54B), C14(H14A,H14B)
3.c Aromatic/amide H refined with riding coordinates:
 N4(H4), N2(H2), C23(H23), C41(H41), C11(H11), C9(H9), C44(H44), C33(H33),
 C32(H32), C21(H21), C39(H39), C27(H27), C18(H18), C17(H17), C37(H37), C26(H26),
  C53(H53), C12(H12), C43(H43), C38(H38), C40(H40), C45(H45), C19(H19), C5(H5),
 C3(H3), C29(H29), C46(H46), C31(H31), C49(H49), C25(H25), C24(H24), C20(H20),
 C47(H47), C30(H30), C50(H50), C51(H51), C6(H6), C52(H52)
3.d Idealised Me refined as rotating group:
 C35(H35A,H35B,H35C), C55(H55A,H55B,H55C)
;
_shelx_res_checksum              2779
_olex2_submission_special_instructions 'No special instructions were received'