Phosphonate-substituted porphyrins as efficient, cost-effective and reusable photocatalysts.
Kechiche, Azhar; Al Shehimy, Shaymaa; Khrouz, Lhoussain; Monnereau, Cyrille; Bucher, Christophe; Parola, Stephane; Bessmertnykh-Lemeune, Alla; Rousselin, Yoann; Cheprakov, Andrey V.; Nasri, Habib; Dalton transactions (Cambridge, England : 2003) 53 (2024) 7498–7516; doi:10.1039/d4dt00418c

data_7715560
_publ_section_title
;
 Phosphonate-substituted porphyrins as efficient, cost-effective and
 reusable photocatalysts.
;
_journal_issue                   17
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              7498
_journal_page_last               7516
_journal_paper_doi               10.1039/d4dt00418c
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C44 H29 N4 O12 P4 Pd, 2(C2 H8 N)'
_chemical_formula_sum            'C48 H45 N6 O12 P4 Pd'
_chemical_formula_weight         1128.18
_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     dual
_audit_creation_date             2022-04-01
_audit_creation_method
;FinalCif V123 by Daniel Kratzert, Freiburg 2023, 
https://dkratzert.de/finalcif.html
;
_audit_update_record
;
2023-08-25 deposited with the CCDC.	2024-03-25 downloaded from the CCDC.
;
_cell_angle_alpha                69.419(2)
_cell_angle_beta                 81.680(2)
_cell_angle_gamma                78.062(2)
_cell_formula_units_Z            2
_cell_length_a                   13.0368(4)
_cell_length_b                   13.9158(5)
_cell_length_c                   18.0430(6)
_cell_measurement_reflns_used    9795
_cell_measurement_temperature    110.0(1)
_cell_measurement_theta_max      26.04
_cell_measurement_theta_min      2.29
_cell_volume                     2988.85(18)
_computing_cell_refinement       'SAINT V8.40B (Bruker, 2016)'
_computing_data_collection       'APEX4 (Bruker, 2021)'
_computing_data_reduction        'SAINT V8.40B (Bruker, 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 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      110.0(1)
_diffrn_detector                 'CCD Plate'
_diffrn_detector_area_resol_mean 8.3
_diffrn_detector_type            APEX2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Nonius Kappa Apex II'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_measurement_specimen_support 'MiTeGen micromount'
_diffrn_radiation_collimation    '0.6 mm'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a~1~'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_xray_symbol    K-L~3~
_diffrn_reflns_av_R_equivalents  0.0878
_diffrn_reflns_av_unetI/netI     0.0340
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            175832
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         1.209
_diffrn_source                   'X-ray tube'
_diffrn_source_current           5.0
_diffrn_source_power             0.1
_diffrn_source_target            Mo
_diffrn_source_type              'Siemens KFF Mo 2K-180'
_diffrn_source_voltage           20.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.474
_exptl_absorpt_correction_T_max  0.8014
_exptl_absorpt_correction_T_min  0.6714
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016) was used for absorption correction.
wR2(int) was 0.0780 before and 0.0675 after correction.
The Ratio of minimum to maximum transmission is 0.8378.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear dark violet'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.254
_exptl_crystal_description       needle
_exptl_crystal_F_000             1154
_exptl_crystal_recrystallization_method
'The material was recrystallised from a mixture of water and DMF  by slow evaporation'
_exptl_crystal_size_max          0.427
_exptl_crystal_size_mid          0.176
_exptl_crystal_size_min          0.134
_refine_diff_density_max         0.940
_refine_diff_density_min         -0.742
_refine_diff_density_rms         0.112
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.123
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     666
_refine_ls_number_reflns         10535
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.123
_refine_ls_R_factor_all          0.0767
_refine_ls_R_factor_gt           0.0606
_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^)+(0.0299P)^2^+21.2275P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1437
_refine_ls_wR_factor_ref         0.1521
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8528
_reflns_number_total             10535
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00418c2.cif
_cod_data_source_block           Pd(TPPP-OH)
_cod_depositor_comments          'Adding full bibliography for 7715560.cif.'
_cod_database_code               7715560
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a MITIGEN holder oil'
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Others
 Sof(C40)=Sof(H40)=Sof(C44)=Sof(H44)=Sof(C43)=Sof(H43)=Sof(C41)=Sof(H41)=1-
 FVAR(1)
 Sof(C43A)=Sof(H43A)=Sof(C44A)=Sof(H44A)=Sof(C40A)=Sof(H40A)=Sof(C41A)=
 Sof(H41A)=FVAR(1)
3.a Secondary CH2 refined with riding coordinates:
 N5(H5A,H5B), N6(H6A,H6B)
3.b Aromatic/amide H refined with riding coordinates:
 C37(H37), C38(H38), C2(H2), C26(H26), C12(H12A), C7(H7A), C32(H32), C28(H28),
 C23(H23), C34(H34), C22(H22), C31(H31), C29(H29), C8(H8A), C25(H25), C17(H17),
 C18(H18), C43A(H43A), C44A(H44A), C40A(H40A), C41A(H41A), C3(H3A), C35(H35),
 C13(H13), C40(H40), C44(H44), C43(H43), C41(H41)
3.c Idealised Me refined as rotating group:
 C46(H46A,H46B,H46C), C45(H45A,H45B,H45C), C47(H47A,H47B,H47C), C48(H48A,H48B,
 H48C)
3.d Idealised tetrahedral OH refined as rotating group:
 O3(H3), O8(H8), O7(H7), O6(H6), O12(H12)
;
_olex2_submission_special_instructions 'No special instructions were received'
_shelx_shelxl_version_number     2018/3
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_estimated_absorpt_t_min   0.823
_shelx_estimated_absorpt_t_max   0.939
_diffrn_measurement_ambient_temperature_device_make 'Oxford Cryostream 600'
_shelx_res_checksum              46294
_shelx_fab_checksum              36817