Tailor-made synthesis of various backbone-substituted imidazolinium salts by triflic anhydride mediated intramolecular cyclisation
Jun Zhang; Xiaolong Su; Jun Fu; Xinke Qin; Meixin Zhao; Min Shi; Chem.Commun. 48 (2012) 9192–; doi:10.1039/c2cc34952c

data_7108281
_publ_section_title
;
 Tailor-made synthesis of various backbone-substituted imidazolinium salts
 by triflic anhydride mediated intramolecular cyclisation
;
_journal_name_full               Chem.Commun.
_journal_page_first              9192
_journal_paper_doi               10.1039/c2cc34952c
_journal_volume                  48
_journal_year                    2012
_chemical_formula_sum            'C34 H35 F3 N2 O3 S'
_chemical_formula_weight         608.70
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 101.758(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.301(4)
_cell_length_b                   16.385(8)
_cell_length_c                   20.954(10)
_cell_measurement_reflns_used    750
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.512
_cell_measurement_theta_min      2.342
_cell_volume                     3126(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_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      293(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0661
_diffrn_reflns_av_sigmaI/netI    0.0871
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            12757
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         1.59
_diffrn_standards_decay_%        3.09
_exptl_absorpt_coefficient_mu    0.158
_exptl_absorpt_correction_T_max  0.9767
_exptl_absorpt_correction_T_min  0.9615
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.293
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             1280
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.284
_refine_diff_density_min         -0.191
_refine_diff_density_rms         0.041
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.908
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     398
_refine_ls_number_reflns         5482
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.908
_refine_ls_R_factor_all          0.1247
_refine_ls_R_factor_gt           0.0591
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0659P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1237
_refine_ls_wR_factor_ref         0.1472
_reflns_number_gt                2851
_reflns_number_total             5482
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2cc34952c.txt
_cod_data_source_block           a11230a
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               7108281