Multicenter interactions and ligand field effects in platinum(ii) tripyrrindione radicals
Tomat, Elisa; Curtis, Clayton J.; Astashkin, Andrei V.; Conradie, Jeanet; Ghosh, Abhik; Dalton Transactions  (2023) –; doi:10.1039/D3DT00894K

data_7712886
_publ_section_title
;
 Multicenter interactions and ligand field effects in platinum(ii)
 tripyrrindione radicals
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT00894K
_journal_year                    2023
_chemical_formula_moiety         'C24 H30 N3 O3 Pt, B F4'
_chemical_formula_sum            'C24 H30 B F4 N3 O3 Pt'
_chemical_formula_weight         690.41
_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     iterative
_audit_creation_date             2022-06-14
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2022-06-27 deposited with the CCDC.	2023-04-20 downloaded from the CCDC.
;
_cell_angle_alpha                118.240(9)
_cell_angle_beta                 110.211(10)
_cell_angle_gamma                92.715(10)
_cell_formula_units_Z            4
_cell_length_a                   12.453(4)
_cell_length_b                   15.634(5)
_cell_length_c                   16.230(5)
_cell_measurement_reflns_used    9268
_cell_measurement_temperature    102.25
_cell_measurement_theta_max      26.40
_cell_measurement_theta_min      2.55
_cell_volume                     2525.9(14)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_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    'olex2.solve 1.3 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      102.25
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.996
_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  0.0331
_diffrn_reflns_av_unetI/netI     0.0295
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            50027
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.512
_diffrn_reflns_theta_min         1.514
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.616
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.5678
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0902 before and 0.0417 after correction.
The Ratio of minimum to maximum transmission is 0.7617.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            'metallic red'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.815
_exptl_crystal_description       plate
_exptl_crystal_F_000             1352
_exptl_crystal_size_max          0.249
_exptl_crystal_size_mid          0.075
_exptl_crystal_size_min          0.073
_refine_diff_density_max         1.566
_refine_diff_density_min         -1.064
_refine_diff_density_rms         0.116
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     719
_refine_ls_number_reflns         10465
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0350
_refine_ls_R_factor_gt           0.0273
_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^)+(0.0267P)^2^+6.2732P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0610
_refine_ls_wR_factor_ref         0.0639
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8973
_reflns_number_total             10465
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00894k2.cif
_cod_data_source_block           mo_pttd2bf4_0m
_cod_original_cell_volume        2526.0(14)
_cod_database_code               7712886
_shelx_shelxl_version_number     2018/3
_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, All O(H,H) groups
2. Restrained distances
 C9B-C8B \\sim C9B-C8BB
 with sigma of 0.02
 C6B-C8B \\sim C6B-C8BB
 with sigma of 0.04
 C6B-C7B \\sim C6B-C7BB
 with sigma of 0.02
 C7B-C8B \\sim C7BB-C8BB
 with sigma of 0.02
 C9B-C7B \\sim C9B-C7BB
 with sigma of 0.04
3. Others
 Fixed Sof: C7B(0.5) C8B(0.5) C8BB(0.5) C7BB(0.5) C20B(0.5) H20A(0.5)
 H20B(0.5) C1(0.5) H1A(0.5) H1B(0.5) C21B(0.5) H21A(0.5) H21B(0.5) H21C(0.5)
 C2(0.5) H2A(0.5) H2B(0.5) H2C(0.5) C18B(0.5) H18A(0.5) H18B(0.5) C3(0.5)
 H3A(0.5) H3B(0.5) C19B(0.5) H19A(0.5) H19B(0.5) H19C(0.5) C4(0.5) H4A(0.5)
 H4B(0.5) H4C(0.5)
4.a Rotating group:
 O3A(H3AA,H3AB), O3B(H3BA,H3BB)
4.b Secondary CH2 refined with riding coordinates:
 C18A(H18C,H18D), C20A(H20C,H20D), C23A(H23C,H23D), C15A(H15C,H15D), C23B(H23A,
 H23B), C15B(H15A,H15B), C20B(H20A,H20B), C1(H1A,H1B), C18B(H18A,H18B), C3(H3A,
 H3B)
4.c Aromatic/amide H refined with riding coordinates:
 C5A(H5A), C10A(H10A), C5B(H5B), C10B(H10B)
4.d Idealised Me refined as rotating group:
 C17B(H17A,H17B,H17C), C19A(H19D,H19E,H19F), C24A(H24D,H24E,H24F), C17A(H17D,
 H17E,H17F), C22A(H22D,H22E,H22F), C22B(H22A,H22B,H22C), C21A(H21D,H21E,H21F),
 C16B(H16A,H16B,H16C), C16A(H16D,H16E,H16F), C24B(H24A,H24B,H24C), C21B(H21A,
 H21B,H21C), C2(H2A,H2B,H2C), C19B(H19A,H19B,H19C), C4(H4A,H4B,H4C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              97993
_shelx_fab_checksum              41301
_olex2_submission_special_instructions 'No special instructions were received'