Fluoride-induced redox-switchable behaviour of a palladium(ii)/(iv) couple
Martínez-Vivas, Sebastián; Poyatos, Macarena; Peris, Eduardo; Chemical Science 16 (2025) 6257–6264; doi:10.1039/D4SC08203F

data_1574089
_publ_section_title
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 Fluoride-induced redox-switchable behaviour of a palladium(ii)/(iv)
 couple
;
_journal_issue                   15
_journal_name_full               'Chemical Science'
_journal_page_first              6257
_journal_page_last               6264
_journal_paper_doi               10.1039/D4SC08203F
_journal_volume                  16
_journal_year                    2025
_chemical_formula_moiety         '2(I), C39 H42 N6 O4'
_chemical_formula_sum            'C39 H42 I2 N6 O4'
_chemical_formula_weight         912.58
_chemical_name_systematic        'salt [1](I)2'
_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             2024-09-04
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-09-30 deposited with the CCDC.	2025-03-07 downloaded from the CCDC.
;
_cell_angle_alpha                106.528(3)
_cell_angle_beta                 102.260(3)
_cell_angle_gamma                90.213(3)
_cell_formula_units_Z            4
_cell_length_a                   14.2539(12)
_cell_length_b                   17.2346(16)
_cell_length_c                   17.3593(17)
_cell_measurement_reflns_used    9548
_cell_measurement_temperature    100.00
_cell_measurement_theta_max      54.228
_cell_measurement_theta_min      4.846
_cell_volume                     3985.7(6)
_computing_cell_refinement       'SAINT V8.40B (Bruker AXS LLC, 2019)'
_computing_data_reduction        'SAINT V8.40B (Bruker AXS LLC, 2019)'
_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    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      100.00
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0530
_diffrn_reflns_av_unetI/netI     0.0261
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            138674
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.370
_diffrn_reflns_theta_min         1.942
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.624
_exptl_absorpt_correction_T_max  0.8620
_exptl_absorpt_correction_T_min  0.8009
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0753 before and 0.0600 after correction.
The Ratio of minimum to maximum transmission is 0.9291.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.521
_exptl_crystal_description       plate
_exptl_crystal_F_000             1824
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.02
_refine_diff_density_max         4.185
_refine_diff_density_min         -3.078
_refine_diff_density_rms         0.158
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     863
_refine_ls_number_reflns         16285
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.089
_refine_ls_R_factor_all          0.0799
_refine_ls_R_factor_gt           0.0706
_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^)+(0.0711P)^2^+37.2360P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1776
_refine_ls_wR_factor_ref         0.1843
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14145
_reflns_number_total             16285
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc08203f2.cif
_cod_data_source_block           24pfa002b
_cod_depositor_comments
'Adding full bibliography for 1574089--1574091.cif.'
_cod_database_code               1574089
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.968
_shelx_estimated_absorpt_t_min   0.697
_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. Restrained distances
 C47-C48
 1.54 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C12) = Uanis(C13) = Uanis(C14)
Uanis(C74) = Uanis(C75) = Uanis(C76) = Uanis(C77) = Uanis(C78)
Uanis(C39) = Uanis(C38) = Uanis(C35) = Uanis(C36) = Uanis(C37)
4.a Ternary CH refined with riding coordinates:
 C35(H35), C74(H74)
4.b Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C8(H8A,H8B), C9(H9A,H9B), C11(H11A,H11B), C12(H12A,H12B),
 C13(H13A,H13B), C36(H36A,H36B), C38(H38A,H38B), C46(H46A,H46B), C47(H47A,H47B),
  C48(H48A,H48B), C50(H50A,H50B), C51(H51A,H51B), C52(H52A,H52B), C75(H75A,
 H75B), C77(H77A,H77B)
4.c Me refined with riding coordinates:
 C10(H10A,H10B,H10C), C14(H14A,H14B,H14C), C76(H76A,H76B,H76C), C78(H78A,H78B,
 H78C)
4.d Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C15(H15), C18(H18), C19(H19),
 C25(H25), C27(H27), C28(H28), C30(H30), C40(H40), C41(H41), C42(H42), C43(H43),
  C44(H44), C45(H45), C54(H54), C57(H57), C58(H58), C64(H64), C66(H66),
 C67(H67), C69(H69)
4.e Idealised Me refined as rotating group:
 C37(H37A,H37B,H37C), C39(H39A,H39B,H39C), C49(H49A,H49B,H49C), C53(H53A,H53B,
 H53C)
;
_olex2_submission_special_instructions 'No special instructions were received'