Formation of a long-lived radical pair in a Sn(iv) porphyrin-di(l-tyrosinato) conjugate driven by proton-coupled electron-transfer.
Natali, Mirco; Amati, Agnese; Demitri, Nicola; Iengo, Elisabetta; Chemical communications (Cambridge, England) 54 (2018) 6148–6152; doi:10.1039/c8cc03441a

data_7121768
_publ_section_title
;
 Formation of a long-lived radical pair in a Sn(iv)
 porphyrin-di(l-tyrosinato) conjugate driven by proton-coupled
 electron-transfer.
;
_journal_issue                   48
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              6148
_journal_page_last               6152
_journal_paper_doi               10.1039/c8cc03441a
_journal_volume                  54
_journal_year                    2018
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C66 H46 N6 O8 Sn, 2 (C3 H6 O), 2 (C4 H10 O)'
_chemical_formula_sum            'C80 H84 N6 O12 Sn'
_chemical_formula_weight         1440.22
_chemical_name_systematic
trans-di(N-acetyl-L-tyrosinato)[5,10,15,20-tetraphenylporphyrinato]-tin(IV)
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_space_group_name_Hall           'P 1'
_space_group_name_H-M_alt        'P 1'
_symmetry_space_group_name_Hall  'P 1'
_symmetry_space_group_name_H-M   'P 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2017/1
_audit_update_record
;
2017-12-22 deposited with the CCDC.
2018-05-29 downloaded from the CCDC.
;
_cell_angle_alpha                112.87(3)
_cell_angle_beta                 100.33(3)
_cell_angle_gamma                94.47(3)
_cell_formula_units_Z            1
_cell_length_a                   9.756(2)
_cell_length_b                   13.413(3)
_cell_length_c                   14.922(3)
_cell_measurement_reflns_used    5264
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.972
_cell_measurement_theta_min      1.498
_cell_volume                     1746.4(8)
_computing_cell_refinement       'XDS (Kabsch, 2010)'
_computing_data_collection       'Elettra XRD1 Data Collection SW'
_computing_data_reduction        'XDS (Kabsch, 2010)'
_computing_molecular_graphics    'Ortep3 for Windows - Coot'
_computing_publication_material  'enCIFer - publCIF'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.945
_diffrn_measurement_device_type
;
'Huber 4-circles Kappa Goniometer, Pilatus 2M detector'
;
_diffrn_measurement_method       'Rotating crystal'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.700
_diffrn_reflns_av_R_equivalents  0.0316
_diffrn_reflns_av_unetI/netI     0.0431
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.945
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            37846
_diffrn_reflns_point_group_measured_fraction_full 0.926
_diffrn_reflns_point_group_measured_fraction_max 0.858
_diffrn_reflns_theta_full        24.835
_diffrn_reflns_theta_max         30.972
_diffrn_reflns_theta_min         1.498
_diffrn_source                   'Elettra Synchrotron - XRD1 BL'
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.412
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'Pale yellow'
_exptl_crystal_density_diffrn    1.369
_exptl_crystal_description       'Thick rods'
_exptl_crystal_F_000             752
_exptl_crystal_size_max          0.030
_exptl_crystal_size_mid          0.030
_exptl_crystal_size_min          0.010
_refine_diff_density_max         0.704
_refine_diff_density_min         -1.376
_refine_diff_density_rms         0.097
_refine_ls_abs_structure_details
;
 Flack x determined using 8665 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.025(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     738
_refine_ls_number_reflns         19922
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0406
_refine_ls_R_factor_gt           0.0400
_refine_ls_shift/su_max          0.018
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0678P)^2^+0.6076P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1060
_refine_ls_wR_factor_ref         0.1066
_reflns_Friedel_coverage         0.817
_reflns_Friedel_fraction_full    0.865
_reflns_Friedel_fraction_max     0.771
_reflns_number_gt                19635
_reflns_number_total             19922
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc03441a2.cif
_cod_data_source_block           SnPTyrOH
_cod_depositor_comments          'Adding full bibliography for 7121768.cif.'
_cod_original_cell_volume        1746.5(7)
_cod_database_code               7121768
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_min   0.988
_shelx_estimated_absorpt_t_max   0.996
_shelx_res_checksum              63567
_shelx_hkl_checksum              25158
_shelx_fab_checksum              52798