Synthesis of 2-trifluoromethylpyrazolo[5,1-a]isoquinolines via silver triflate-catalyzed or electrophile-mediated one-pot tandem reaction.
Zhou, Xiaoli; Liu, Meiling; Luo, Puying; Lai, Yingjun; Yang, Tangtao; Ding, Qiuping; Beilstein journal of organic chemistry 10 (2014) 2286–2292; doi:10.3762/bjoc.10.238

data_4029994
_publ_section_title
;
 Synthesis of 2-trifluoromethylpyrazolo[5,1-a]isoquinolines via silver
 triflate-catalyzed or electrophile-mediated one-pot tandem reaction.
;
_journal_name_full               'Beilstein journal of organic chemistry'
_journal_page_first              2286
_journal_page_last               2292
_journal_paper_doi               10.3762/bjoc.10.238
_journal_volume                  10
_journal_year                    2014
_chemical_formula_sum            'C22 H17 F3 N2 O2'
_chemical_formula_weight         398.38
_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                74.933(5)
_cell_angle_beta                 73.640(5)
_cell_angle_gamma                78.131(5)
_cell_formula_units_Z            2
_cell_length_a                   7.4466(8)
_cell_length_b                   11.1033(12)
_cell_length_c                   12.5493(13)
_cell_measurement_reflns_used    7742
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.65
_cell_measurement_theta_min      2.29
_cell_volume                     951.49(18)
_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 0.977
_diffrn_measured_fraction_theta_max 0.977
_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  0.0439
_diffrn_reflns_av_sigmaI/netI    0.0327
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            13438
_diffrn_reflns_theta_full        27.76
_diffrn_reflns_theta_max         27.75
_diffrn_reflns_theta_min         1.92
_exptl_absorpt_coefficient_mu    0.110
_exptl_absorpt_correction_T_max  0.9741
_exptl_absorpt_correction_T_min  0.9678
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            COLORLESS
_exptl_crystal_density_diffrn    1.390
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             412
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.24
_refine_diff_density_max         0.385
_refine_diff_density_min         -0.380
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     264
_refine_ls_number_reflns         4390
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.1102
_refine_ls_R_factor_gt           0.0792
_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^)+(0.1111P)^2^+0.5281P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2240
_refine_ls_wR_factor_ref         0.2589
_reflns_number_gt                2829
_reflns_number_total             4390
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            1860-5397-10-238-S2.cif
_cod_data_source_block           130914cbp_0m
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to
/usr/data/users/saulius/crontab/automatic-downloads/current/Beilstein/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2827 2014-09-09 07:05:25Z andrius 

 Adding full bibliography for 4029994--4029995.cif.
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4029994