Platinum(ii) and palladium(ii) complexes with electron-deficient meso-diethoxyphosphorylporphyrins: synthesis, structure and tuning of photophysical properties by varying peripheral substituents.
Volostnykh, Marina V.; Borisov, Sergey M.; Konovalov, Mikhail A.; Sinelshchikova, Anna A.; Gorbunova, Yulia G.; Tsivadze, Aslan Yu; Meyer, Michel; Stern, Christine; Bessmertnykh-Lemeune, Alla; Dalton transactions (Cambridge, England : 2003) 48 (2019) 8882–8898; doi:10.1039/c9dt01577a

data_7701574
_publ_section_title
;
 Platinum(ii) and palladium(ii) complexes with electron-deficient
 meso-diethoxyphosphorylporphyrins: synthesis, structure and tuning of
 photophysical properties by varying peripheral substituents.
;
_journal_issue                   24
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              8882
_journal_page_last               8898
_journal_paper_doi               10.1039/c9dt01577a
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C40 H33 N4 O7 P Pd, C H Cl3'
_chemical_formula_sum            'C41 H34 Cl3 N4 O7 P Pd'
_chemical_formula_weight         938.44
_chemical_name_common            PdD(CMP)PP
_chemical_name_systematic
'[10-(Diethoxyphosphoryl)-5,15-bis{p-(methoxycarbonyl)phenyl}porphyrinato(2-)] palladium(II) chloroform solvate'
_chemical_properties_physical
Oxygen-sensitive,Light-sensitive,Photo-sensitive
_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             2019-01-25
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-03-20 deposited with the CCDC.	2019-05-14 downloaded from the CCDC.
;
_cell_angle_alpha                72.119(2)
_cell_angle_beta                 75.384(2)
_cell_angle_gamma                85.933(2)
_cell_formula_units_Z            2
_cell_length_a                   10.7842(3)
_cell_length_b                   11.5565(4)
_cell_length_c                   17.0314(6)
_cell_measurement_reflns_used    5329
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.968
_cell_measurement_theta_min      2.945
_cell_volume                     1954.63(11)
_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 0.998
_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  0.0393
_diffrn_reflns_av_unetI/netI     0.0638
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            24057
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.999
_diffrn_reflns_theta_min         3.013
_exptl_absorpt_coefficient_mu    0.778
_exptl_absorpt_correction_T_max  0.985
_exptl_absorpt_correction_T_min  0.908
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2008/1 (Bruker,2008) was used for absorption correction. wR2(int) was 0.0456 before and 0.0416 after correction. The Ratio of minimum to maximum transmission is 0.9223. The \l/2 correction factor is 0.0015.'
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.594
_exptl_crystal_description       prism
_exptl_crystal_F_000             952
_exptl_crystal_preparation       Luminescent
_exptl_crystal_recrystallization_method CHCl3-hexane
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.799
_refine_diff_density_min         -0.766
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     518
_refine_ls_number_reflns         11378
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.0615
_refine_ls_R_factor_gt           0.0388
_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^)+(0.0339P)^2^+0.2672P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0766
_refine_ls_wR_factor_ref         0.0844
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8738
_reflns_number_total             11378
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt01577a2.cif
_cod_data_source_block           PdD(CMP)PP
_cod_database_code               7701574
_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 Ternary CH refined with riding coordinates:
 C1S(H1S)
2.b Secondary CH2 refined with riding coordinates:
 C39(H39A,H39B), C37(H37A,H37B)
2.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C8(H8), C9(H9), C13(H13), C14(H14), C16(H16), C17(H17),
 C19(H19), C21(H21), C22(H22), C26(H26), C27(H27), C31(H31), C32(H32), C34(H34),
  C35(H35)
2.d Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C30(H30A,H30B,H30C), C40(H40A,H40B,H40C), C38(H38A,H38B,
 H38C)
;
_shelx_res_checksum              51144
_olex2_submission_special_instructions 'No special instructions were received'