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_7712884
_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         'C29 H37 N4 O2 Pt, B F4'
_chemical_formula_sum            'C29 H37 B F4 N4 O2 Pt'
_chemical_formula_weight         755.52
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_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                90
_cell_angle_beta                 95.9540(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.0550(4)
_cell_length_b                   9.2569(3)
_cell_length_c                   24.1295(7)
_cell_measurement_reflns_used    9019
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      26.40
_cell_measurement_theta_min      2.70
_cell_volume                     2900.29(15)
_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    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_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  0.0270
_diffrn_reflns_av_unetI/netI     0.0182
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            33463
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.401
_diffrn_reflns_theta_min         1.697
_diffrn_source_current           30.0
_diffrn_source_power             1.26
_diffrn_source_voltage           42.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.898
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.5275
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0844 before and 0.0377 after correction.
The Ratio of minimum to maximum transmission is 0.7077.
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    1.730
_exptl_crystal_description       plate
_exptl_crystal_F_000             1496
_exptl_crystal_size_max          0.285
_exptl_crystal_size_mid          0.119
_exptl_crystal_size_min          0.089
_refine_diff_density_max         1.308
_refine_diff_density_min         -0.587
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     379
_refine_ls_number_reflns         5947
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0242
_refine_ls_R_factor_gt           0.0218
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0228P)^2^+5.4715P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0488
_refine_ls_wR_factor_ref         0.0498
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5621
_reflns_number_total             5947
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00894k2.cif
_cod_data_source_block           mo_pttd2tbuncbf4_2_0m
_cod_database_code               7712884
_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
2.a Secondary CH2 refined with riding coordinates:
 C20(H20A,H20B), C18(H18A,H18B), C23(H23A,H23B), C15(H15A,H15B)
2.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C10(H10)
2.c Idealised Me refined as rotating group:
 C29(H29A,H29B,H29C), C24(H24A,H24B,H24C), C17(H17A,H17B,H17C), C22(H22A,H22B,
 H22C), C16(H16A,H16B,H16C), C19(H19A,H19B,H19C), C21(H21A,H21B,H21C), C27(H27A,
 H27B,H27C), C28(H28A,H28B,H28C)
;
_shelx_res_checksum              80407
_olex2_submission_special_instructions 'No special instructions were received'