Water-soluble platinum and palladium porphyrins with peripheral ethyl phosphonic acid substituents: synthesis, aggregation in solution, and photocatalytic properties.
Volostnykh, Marina V.; Kirakosyan, Gayane A.; Sinelshchikova, Anna A.; Ermakova, Elizaveta V.; Gorbunova, Yulia G.; Tsivadze, Aslan Yu; Borisov, Sergey M.; Meyer, Michel; Khrouz, Lhoussain; Monnereau, Cyrille; Parola, Stephane; Bessmertnykh-Lemeune, Alla; Dalton transactions (Cambridge, England : 2003) 54 (2025) 2340–2356; doi:10.1039/d4dt03068k

data_7717780
_publ_section_title
;
 Water-soluble platinum and palladium porphyrins with peripheral ethyl
 phosphonic acid substituents: synthesis, aggregation in solution, and
 photocatalytic properties.
;
_journal_issue                   6
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2340
_journal_page_last               2356
_journal_paper_doi               10.1039/d4dt03068k
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'C44 H42 N4 O10 P2 Pd'
_chemical_formula_sum            'C44 H42 N4 O10 P2 Pd'
_chemical_formula_weight         955.15
_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_Hall           'P 2c -2ac'
_space_group_name_H-M_alt        'P c a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-03-16
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-09-07 deposited with the CCDC.	2025-01-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   23.940(3)
_cell_length_b                   7.2579(9)
_cell_length_c                   23.162(3)
_cell_measurement_reflns_used    9353
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      35.114
_cell_measurement_theta_min      3.062
_cell_volume                     4024.5(9)
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2009)'
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.15
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type
'Bruker KAPPA APEX II area-detector diffractometer'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0646
_diffrn_reflns_av_unetI/netI     0.0411
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            132202
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         34.999
_diffrn_reflns_theta_min         4.184
_exptl_absorpt_coefficient_mu    0.608
_exptl_absorpt_correction_T_max  0.7469
_exptl_absorpt_correction_T_min  0.6892
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2008/1 (Bruker,2008) was used for absorption correction. wR2(int) was 0.0904 before and 0.0774 after correction. The Ratio of minimum to maximum transmission is 0.9227. The \l/2 correction factor is 0.0015.'
_exptl_crystal_colour            'dark red'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.576
_exptl_crystal_description       block
_exptl_crystal_F_000             1960
_exptl_crystal_preparation       Luminescent
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: CHCl3, hexane'
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.465
_refine_diff_density_min         -0.656
_refine_diff_density_rms         0.066
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.070(15)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     551
_refine_ls_number_reflns         17666
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.0337
_refine_ls_R_factor_gt           0.0271
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0231P)^2^+1.1750P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0601
_refine_ls_wR_factor_ref         0.0629
_reflns_Friedel_coverage         0.960
_reflns_Friedel_fraction_full    0.995
_reflns_Friedel_fraction_max     0.997
_reflns_number_gt                15802
_reflns_number_total             17666
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt03068k2.cif
_cod_data_source_block           pd7b
_cod_depositor_comments
'Adding full bibliography for 7717779--7717780.cif.'
_cod_database_code               7717780
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.920
_shelx_estimated_absorpt_t_min   0.820
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.930(15)
 0.070(15)
2. 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
3.a Secondary CH2 refined with riding coordinates:
 C43(H43A,H43B), C39(H39A,H39B), C37(H37A,H37B), C41(H41A,H41B)
3.b Me refined with riding coordinates:
 C38(H38A,H38B,H38C), C44(H44A,H44B,H44C), C30(H30A,H30B,H30C), C42(H42A,H42B,
 H42C), C12(H12A,H12B,H12C), C40(H40A,H40B,H40C)
3.c Aromatic/amide H refined with riding coordinates:
 C13(H13), C34(H34), C22(H22), C4(H4), C27(H27), C31(H31), C35(H35), C16(H16),
 C32(H32), C17(H17), C9(H9), C21(H21), C26(H26), C3(H3), C8(H8), C14(H14)
;
_shelx_res_checksum              957
_olex2_submission_special_instructions 'No special instructions were received'