Photocatalytic Radical Trifluoromethylation/Cyclization Cascade: Synthesis of CF3-Containing Pyrazolines and Isoxazolines.
Wei, Qiang; Chen, Jia-Rong; Hu, Xiao-Qiang; Yang, Xiao-Chen; Lu, Bin; Xiao, Wen-Jing; Organic letters 17 (2015) 4464–4467; doi:10.1021/acs.orglett.5b02118

data_1529503
_publ_section_title
;
 Photocatalytic Radical Trifluoromethylation/Cyclization Cascade:
 Synthesis of CF3-Containing Pyrazolines and Isoxazolines.
;
_journal_issue                   18
_journal_name_full               'Organic letters'
_journal_page_first              4464
_journal_page_last               4467
_journal_paper_doi               10.1021/acs.orglett.5b02118
_journal_volume                  17
_journal_year                    2015
_chemical_formula_sum            'C25 H22 Cl3 F3 N2 O2 S'
_chemical_formula_weight         577.86
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_symmetry_space_group_name_Hall  '-P 1'
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_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                99.954(7)
_cell_angle_beta                 98.372(7)
_cell_angle_gamma                101.416(7)
_cell_formula_units_Z            2
_cell_length_a                   8.374(3)
_cell_length_b                   10.228(4)
_cell_length_c                   16.064(7)
_cell_measurement_reflns_used    2171
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      24.75
_cell_measurement_theta_min      2.53
_cell_volume                     1305.1(9)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
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_diffrn_reflns_av_sigmaI/netI    0.0789
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            9894
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         2.08
_exptl_absorpt_coefficient_mu    0.479
_exptl_absorpt_correction_T_max  0.9103
_exptl_absorpt_correction_T_min  0.8696
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.470
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             592
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.502
_refine_diff_density_min         -0.312
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_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     382
_refine_ls_number_reflns         5078
_refine_ls_number_restraints     60
_refine_ls_restrained_S_all      1.125
_refine_ls_R_factor_all          0.0983
_refine_ls_R_factor_gt           0.0618
_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^)+(0.0847P)^2^+0.4893P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1519
_refine_ls_wR_factor_ref         0.1806
_reflns_number_gt                3309
_reflns_number_total             5078
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ol5b02118_si_002.cif
_cod_data_source_block           mo_150504b_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/rss-feeds/ACS/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 3271 2015-04-21 07:52:19Z andrius 

 Adding full bibliography for 1529503.cif.
;
_cod_original_cell_volume        1305.2(9)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               1529503