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_7116065
_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            'C54 H50 N6 O5'
_chemical_formula_weight         863.00
_chemical_melting_point          484.15
_chemical_name_common            '(bpep)2(res)2 '
_chemical_name_systematic
'1,3-bis(trans-4-pyridylethenyl)pyridine resorcinol tetrahydrofuran solvate'
_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                66.711(3)
_cell_angle_beta                 69.574(4)
_cell_angle_gamma                66.077(3)
_cell_formula_units_Z            2
_cell_length_a                   13.274(5)
_cell_length_b                   13.860(5)
_cell_length_c                   15.867(6)
_cell_measurement_reflns_used    2554
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      21.60
_cell_measurement_theta_min      2.48
_cell_volume                     2388.3(15)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0474
_diffrn_reflns_av_sigmaI/netI    0.0821
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            16593
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.48
_exptl_absorpt_coefficient_mu    0.078
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_correction_T_min  0.460
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS; Bruker, 2000'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.200
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             912
_exptl_crystal_recrystallization_method 'liquid-liquid diffusion'
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.580
_refine_diff_density_min         -0.371
_refine_diff_density_rms         0.039
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     644
_refine_ls_number_reflns         8297
_refine_ls_number_restraints     294
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.1743
_refine_ls_R_factor_gt           0.0676
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+2.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1267
_refine_ls_wR_factor_ref         0.1646
_reflns_number_gt                3321
_reflns_number_total             8297
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4cc06808d2.cif
_cod_data_source_block           x
_cod_original_cell_volume        2388.2(15)
_cod_original_sg_symbol_H-M      'P-1   '
_cod_database_code               7116065