Twisted Tethered Tolanes: Unanticipated Long-Lived Phosphorescence at 77 K
Sebastian Menning; Maximilian Krämer; Benjamin A. Coombs; Frank Rominger; Andrew Beeby; Andreas Dreuw; Uwe H. F. Bunz; Journal of the American Chemical Society 135 (2013) 2160–2163; doi:10.1021/ja400416r

data_4119346
_publ_section_title
;
 Twisted Tethered Tolanes: Unanticipated Long-Lived Phosphorescence at 77
 K
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              2160
_journal_page_last               2163
_journal_paper_doi               10.1021/ja400416r
_journal_volume                  135
_journal_year                    2013
_chemical_formula_sum            'C19 H14 O4'
_chemical_formula_weight         306.30
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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-97
_cell_angle_alpha                83.591(5)
_cell_angle_beta                 83.761(5)
_cell_angle_gamma                69.162(5)
_cell_formula_units_Z            2
_cell_length_a                   8.048(2)
_cell_length_b                   8.856(2)
_cell_length_c                   11.420(3)
_cell_measurement_reflns_used    2446
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      27.90
_cell_measurement_theta_min      2.47
_cell_volume                     753.9(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'Bruker APEX'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0588
_diffrn_reflns_av_sigmaI/netI    0.0791
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            7816
_diffrn_reflns_theta_full        28.35
_diffrn_reflns_theta_max         28.35
_diffrn_reflns_theta_min         1.80
_exptl_absorpt_coefficient_mu    0.095
_exptl_absorpt_correction_T_max  0.9925
_exptl_absorpt_correction_T_min  0.9480
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.349
_exptl_crystal_description       polyhedron
_exptl_crystal_F_000             320
_exptl_crystal_size_max          0.57
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.389
_refine_diff_density_min         -0.293
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     208
_refine_ls_number_reflns         3698
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0816
_refine_ls_R_factor_gt           0.0646
_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^)+(0.1089P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1765
_refine_ls_wR_factor_ref         0.1890
_reflns_number_gt                2869
_reflns_number_total             3698
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja400416r_si_002.cif
_cod_data_source_block           sme9
_cod_database_code               4119346