From energy transfer to electron transfer photocatalysis (PenT→ PET): oxidative cyclobutane cleavage alters the product composition
Lefarth, Jens; Haseloer, Alexander; Kletsch, Lukas; Klein, Axel; Neudörfl, Jörg-Martin; Griesbeck, Axel; Chemical Communications  (2022) –; doi:10.1039/D2CC04693H

data_7130932
_publ_section_title
;
 From energy transfer to electron transfer photocatalysis
 (PenT\\rightarrow PET): oxidative cyclobutane cleavage alters the product
 composition
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D2CC04693H
_journal_year                    2022
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C17 H20 O3'
_chemical_formula_sum            'C17 H20 O3'
_chemical_formula_weight         272.33
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2022-10-14 deposited with the CCDC.	2022-10-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.0000(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   10.5051(4)
_cell_length_b                   20.1564(8)
_cell_length_c                   13.1906(5)
_cell_measurement_reflns_used    9027
_cell_measurement_temperature    171(2)
_cell_measurement_theta_max      72.08
_cell_measurement_theta_min      4.01
_cell_volume                     2793.04(19)
_computing_cell_refinement       'Bruker APEX 3'
_computing_data_collection       'Bruker APEX 3'
_computing_data_reduction
;
Bruker APEX 3
SADABS Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10.
;
_computing_molecular_graphics    'SCHAKAL99 (E. Keller 1999)'
_computing_publication_material  'PLATON (A. L. Spek 1980-2015)'
_computing_structure_refinement
;
SHELXL-2014/7 (Sheldrick, 2014)
SHELXLE (C. B. Huebschle 2016)'
;
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      171(2)
_diffrn_detector_type            'Bruker PhotonIII M14'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0767
_diffrn_reflns_av_unetI/netI     0.0553
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            42493
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         72.070
_diffrn_reflns_theta_min         3.350
_diffrn_source                   'micro focus'
_exptl_absorpt_coefficient_mu    0.703
_exptl_absorpt_correction_T_max  0.7536
_exptl_absorpt_correction_T_min  0.6253
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.295
_exptl_crystal_description       prism
_exptl_crystal_F_000             1168
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.070
_refine_diff_density_max         0.184
_refine_diff_density_min         -0.197
_refine_diff_density_rms         0.037
_refine_ls_abs_structure_details
;
 Flack x determined using 4044 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.11(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     725
_refine_ls_number_reflns         10780
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.087
_refine_ls_R_factor_all          0.0435
_refine_ls_R_factor_gt           0.0356
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0470P)^2^+0.1023P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0904
_refine_ls_wR_factor_ref         0.0923
_reflns_Friedel_coverage         0.909
_reflns_Friedel_fraction_full    0.982
_reflns_Friedel_fraction_max     0.962
_reflns_number_gt                9716
_reflns_number_total             10780
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc04693h2.cif
_cod_data_source_block           jel646b_1
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               7130932
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.872
_shelx_estimated_absorpt_t_max   0.952
_shelx_res_checksum              21088
_shelx_hkl_checksum              68723