Synthesis of tetra-substituted olefins via annulation by Pd-catalyzed carbopalladation/C-H activation and solid state fluorescence properties
Naveen, Kanagaraj; Avanashiappan, Nandakumar; Paramasivan Thirumalai, Perumal; RSC Adv.  (2015) –; doi:10.1039/C5RA14621F

data_7221870
_publ_section_title
;
 Synthesis of tetra-substituted olefins via annulation by Pd-catalyzed
 carbopalladation/C-H activation and solid state fluorescence properties
;
_journal_name_full               'RSC Adv.'
_journal_paper_doi               10.1039/C5RA14621F
_journal_year                    2015
_chemical_formula_moiety         'C39 H39 N O2'
_chemical_formula_sum            'C39 H39 N O2'
_chemical_formula_weight         553.71
_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
_audit_update_record
;
2014-04-20 deposited with the CCDC.
2015-08-24 downloaded from the CCDC.
;
_cell_angle_alpha                97.221(4)
_cell_angle_beta                 111.326(4)
_cell_angle_gamma                102.377(4)
_cell_formula_units_Z            2
_cell_length_a                   10.6305(6)
_cell_length_b                   11.4052(7)
_cell_length_c                   14.0678(9)
_cell_measurement_temperature    293(2)
_cell_volume                     1512.53(17)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.971
_diffrn_measured_fraction_theta_max 0.971
_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  0.0598
_diffrn_reflns_av_sigmaI/netI    0.0587
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            21810
_diffrn_reflns_theta_full        26.82
_diffrn_reflns_theta_max         26.82
_diffrn_reflns_theta_min         1.59
_exptl_absorpt_coefficient_mu    0.074
_exptl_absorpt_correction_T_max  0.9854
_exptl_absorpt_correction_T_min  0.9782
_exptl_crystal_density_diffrn    1.216
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             592
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.238
_refine_diff_density_min         -0.173
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.987
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     382
_refine_ls_number_reflns         6299
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.987
_refine_ls_R_factor_all          0.1180
_refine_ls_R_factor_gt           0.0554
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0949P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1380
_refine_ls_wR_factor_ref         0.1787
_reflns_number_gt                3247
_reflns_number_total             6299
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5ra14621f2.cif
_cod_data_source_block           fin
_cod_original_cell_volume        1512.53(16)
_cod_database_code               7221870