Reversible Photoredox Switching of Porphyrin-Bridged Bis-2,6-di-tert-butylphenols
Shinsuke Ishihara; Jonathan P. Hill; Atsuomi Shundo; Gary J. Richards; Jan Labuta; Kei Ohkubo; Shunichi Fukuzumi; Akira Sato; Mark R. J. Elsegood; Simon J. Teat; Katsuhiko Ariga; Journal of the American Chemical Society 133 (2011) 16119–16126; doi:10.1021/ja2056165

data_4106916
_publ_contact_author
; 
'Jonathan P. Hill'
;
_publ_contact_author_email       jonathan.hill@nims.go.jp
_publ_contact_author_phone       '+81 29 860 4399'
_publ_section_title
;
 Reversible Photoredox Switching of Porphyrin-Bridged
 Bis-2,6-di-tert-butylphenols
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              16119
_journal_page_last               16126
_journal_paper_doi               10.1021/ja2056165
_journal_volume                  133
_journal_year                    2011
_chemical_absolute_configuration unk
_chemical_formula_moiety
'C60 H58 N4 O2, 2(N C16 H36 1+), 3.5(O C4 H8)'
_chemical_formula_sum            'C106 H160 N6 O5.5'
_chemical_formula_weight         1606.40
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           29
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2ac'
_symmetry_space_group_name_H-M   'P c a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.3034(8)
_cell_length_b                   11.7118(4)
_cell_length_c                   43.8395(17)
_cell_measurement_reflns_used    16713
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      33.58
_cell_measurement_theta_min      2.51
_cell_volume                     9911.1(7)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX 2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL and local programs'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX 2 CCD diffractometer'
_diffrn_measurement_method       '\w rotation with narrow frames'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_radiation_source         'ALS Station 11.3.1'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.7749
_diffrn_reflns_av_R_equivalents  0.0734
_diffrn_reflns_av_sigmaI/netI    0.0468
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       54
_diffrn_reflns_limit_l_min       -54
_diffrn_reflns_number            85273
_diffrn_reflns_theta_full        29.12
_diffrn_reflns_theta_max         29.12
_diffrn_reflns_theta_min         2.22
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.065
_exptl_absorpt_correction_T_max  0.996
_exptl_absorpt_correction_T_min  0.984
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS v2008/1, Sheldrick, G.M., (2008)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.077
_exptl_crystal_description       plate
_exptl_crystal_F_000             3528
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.011
_refine_diff_density_min         -0.429
_refine_diff_density_rms         0.077
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_extinction_coef       0.0053(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1069
_refine_ls_number_reflns         10377
_refine_ls_number_restraints     688
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.1165
_refine_ls_R_factor_gt           0.0978
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1895P)^2^+4.0959P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2651
_refine_ls_wR_factor_ref         0.2806
_reflns_number_gt                7872
_reflns_number_total             10377
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ja2056165_si_004.cif
_cod_data_source_block           jph6
_cod_original_formula_sum        'C106 H160 N6 O5.50'
_cod_database_code               4106916