Influence of the Linking Bridge on the Photoreactivity of Benzophenone-Thymine Conjugates.
Blasco-Brusola, Alejandro; Vayá, Ignacio; Miranda, Miguel A.; The Journal of organic chemistry  (2020) –; doi:10.1021/acs.joc.0c02088

data_4038928
_publ_section_title
;
 Influence of the Linking Bridge on the Photoreactivity of
 Benzophenone-Thymine Conjugates.
;
_journal_name_full               'The Journal of organic chemistry'
_journal_paper_doi               10.1021/acs.joc.0c02088
_journal_year                    2020
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C28 H33 N3 O4, C H2 Cl2'
_chemical_formula_sum            'C29 H35 Cl2 N3 O4'
_chemical_formula_weight         560.5
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      33
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   dual
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
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_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.4467(2)
_cell_length_b                   28.7768(6)
_cell_length_c                   10.3242(2)
_cell_measurement_reflns_used    8103
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      74.45
_cell_measurement_theta_min      3.07
_cell_measurement_wavelength     1.54178
_cell_volume                     2806.59(10)
_computing_cell_refinement       'APPEX3v2018.7-2 (BRUKER AXS, 2005)'
_computing_data_collection       'APPEX3v2018.7-2 (BRUKER AXS, 2005)'
_computing_data_reduction        'APPEX3v2018.7-2 (BRUKER AXS, 2005)'
_computing_molecular_graphics    'Ortep for Windows (Farrugia, 2012)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT-2018/2 (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 7.3910
_diffrn_measured_fraction_theta_full 1
_diffrn_measured_fraction_theta_max 1
_diffrn_measurement_device_type  'Bruker D8 VENTURE PHOTON III-14'
_diffrn_measurement_method       'omega and phi'
_diffrn_radiation_monochromator  'Incoatec multilayer mirror'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0818
_diffrn_reflns_av_unetI/netI     0.0504
_diffrn_reflns_Laue_measured_fraction_full 1
_diffrn_reflns_Laue_measured_fraction_max 1
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            32650
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         74.439
_diffrn_reflns_theta_min         3.071
_diffrn_source                   'INCOATEC microfocus sealed tube'
_diffrn_source_type              'Incoatec I\mS 3.0'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.401
_exptl_absorpt_correction_T_max  0.9288
_exptl_absorpt_correction_T_min  0.7986
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'BRUKER SADABS-2016/2'
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.326
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1184
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.369
_refine_diff_density_min         -0.659
_refine_diff_density_rms         0.059
_refine_ls_abs_structure_details
;
 Flack x determined using 1921 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.009(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     349
_refine_ls_number_reflns         5676
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0605
_refine_ls_R_factor_gt           0.0492
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0763P)^2^+1.0782P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1261
_refine_ls_wR_factor_ref         0.1332
_reflns_Friedel_coverage         0.874
_reflns_Friedel_fraction_full    0.983
_reflns_Friedel_fraction_max     0.98
_reflns_number_gt                4896
_reflns_number_total             5676
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jo0c02088_si_002.cif
_cod_data_source_block           RXNV2020-1
_cod_database_code               4038928
_shelx_estimated_absorpt_t_min   0.563
_shelx_estimated_absorpt_t_max   0.91
_shelx_shelxl_version_number     2018/3
_shelx_res_checksum              19961
_shelx_hkl_checksum              20189