In situ Raman monitoring of [2+2] cycloaddition of pyridine substituted olefins induced by visible laser
Dengtai Chen; Xijiang Han; Wen Jin; Yunchen Du; Ping Xu; Chem.Commun. 50 (2014) 15631–; doi:10.1039/C4cc06808D

data_7116066
_publ_section_title
;
 In situ Raman monitoring of [2+2] cycloaddition of pyridine substituted
 olefins induced by visible laser
;
_journal_name_full               Chem.Commun.
_journal_page_first              15631
_journal_paper_doi               10.1039/C4cc06808D
_journal_volume                  50
_journal_year                    2014
_chemical_formula_sum            'C13.5 H11 Ag0.5 F1.5 N O3'
_chemical_formula_weight         317.67
_chemical_melting_point          339.15
_chemical_name_common
'[Ag2(PEA)4][TFA]2 (PEA = Ethyl-(pyridine-4-yl)prop-2-enotate, TFA =TFA = trifluoroacetate) '
_chemical_name_systematic
'[Ag2(Ethyl-(pyridine-4-yl)prop-2-enotate)4][trifluoroacetate]2 '
_chemical_properties_physical    'Air-sensitive, Light-sensitive'
_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                112.017(5)
_cell_angle_beta                 93.953(5)
_cell_angle_gamma                94.913(6)
_cell_formula_units_Z            4
_cell_length_a                   7.2173(19)
_cell_length_b                   13.875(4)
_cell_length_c                   14.970(4)
_cell_measurement_temperature    296(2)
_cell_volume                     1376.4(7)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0398
_diffrn_reflns_av_sigmaI/netI    0.0779
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            4727
_diffrn_reflns_theta_full        20.93
_diffrn_reflns_theta_max         20.93
_diffrn_reflns_theta_min         1.59
_exptl_absorpt_coefficient_mu    0.795
_exptl_crystal_colour            transparent
_exptl_crystal_density_diffrn    1.533
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             640
_exptl_crystal_recrystallization_method 'liquid-liquid difussion'
_refine_diff_density_max         0.302
_refine_diff_density_min         -0.390
_refine_diff_density_rms         0.054
_refine_ls_extinction_coef       0.0007(3)
_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   1.040
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     399
_refine_ls_number_reflns         2913
_refine_ls_number_restraints     490
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.1071
_refine_ls_R_factor_gt           0.0509
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0200P)^2^+1.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0852
_refine_ls_wR_factor_ref         0.0998
_reflns_number_gt                1535
_reflns_number_total             2913
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4cc06808d2.cif
_cod_data_source_block           x1
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C13.50 H11 Ag0.50 F1.50 N O3'
_cod_database_code               7116066