Synthesis, electronic properties, structural studies, and catalytic activity of peripherally metalated β-η<sup>1</sup>-Pd(II)-thioalkyl porphyrazine.
Belviso, Sandra; Larotonda, Giuseppe; Santoro, Ernesto; Santarsiere, Alessandro; Tuzi, Angela; Dalton transactions (Cambridge, England : 2003) 54 (2025) 11563–11572; doi:10.1039/d5dt01394a

data_7719221
_publ_section_title
;
 Synthesis, electronic properties, structural studies, and catalytic
 activity of peripherally metalated
 &#x3b2;-&#x3b7;<sup>1</sup>-Pd(II)-thioalkyl porphyrazine.
;
_journal_issue                   30
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              11563
_journal_page_last               11572
_journal_paper_doi               10.1039/d5dt01394a
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'C66 H67 Br0.02 Cl0.98 N8 P2 Pd S7, C H2 Cl2'
_chemical_formula_sum            'C67 H69 Br0.02 Cl2.98 N8 P2 Pd S7'
_chemical_formula_weight         1485.85
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2019/2
_audit_update_record
;
2025-05-30 deposited with the CCDC.	2025-07-07 downloaded from the CCDC.
;
_cell_angle_alpha                103.771(8)
_cell_angle_beta                 107.797(13)
_cell_angle_gamma                98.259(10)
_cell_formula_units_Z            2
_cell_length_a                   13.0130(19)
_cell_length_b                   14.2340(12)
_cell_length_c                   20.382(4)
_cell_measurement_reflns_used    233
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      21.282
_cell_measurement_theta_min      3.795
_cell_volume                     3394.4(10)
_computing_cell_refinement       'Dirax/lsq (Duisenberg & Schreurs 1989-2000)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction        'EvalCCD (Duisenberg & Schreurs 1990-2000)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 2012)'
_computing_publication_material  'WinGX (Farrugia, 2012)'
_computing_structure_refinement  'SHELXL-2019/2 (Sheldrick, 2019)'
_computing_structure_solution    'SIR97 (Altomare et al. 1999)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker-Nonius KappaCCD'
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0644
_diffrn_reflns_av_unetI/netI     0.0798
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            41490
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.483
_diffrn_reflns_theta_min         2.899
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    0.707
_exptl_absorpt_correction_T_max  0.940
_exptl_absorpt_correction_T_min  0.837
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS(Bruker 2002)
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.454
_exptl_crystal_description       block
_exptl_crystal_F_000             1532
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.080
_refine_diff_density_max         0.524
_refine_diff_density_min         -0.450
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     884
_refine_ls_number_reflns         15457
_refine_ls_number_restraints     42
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0848
_refine_ls_R_factor_gt           0.0459
_refine_ls_shift/su_max          0.014
_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^+1.9565P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0786
_refine_ls_wR_factor_ref         0.0902
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10813
_reflns_number_total             15457
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt01394a2.cif
_cod_data_source_block           shelx
_cod_database_code               7719221
_shelx_shelxl_version_number     2019/2
_shelx_estimated_absorpt_t_min   0.872
_shelx_estimated_absorpt_t_max   0.946
_shelx_res_checksum              76780
_shelx_hkl_checksum              96772