Diverse Trifluoromethyl Heterocycles from a Single Precursor
Mark A. Honey; Raffaele Pasceri; William Lewis; Christopher J. Moody; Journal of Organic Chemistry 77 (2012) 1396–1405; doi:10.1021/jo202201w

data_4026915
_publ_section_title
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 Diverse Trifluoromethyl Heterocycles from a Single Precursor
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              1396
_journal_page_last               1405
_journal_paper_doi               10.1021/jo202201w
_journal_volume                  77
_journal_year                    2012
_chemical_formula_sum            'C13 H13 Br F3 N O5'
_chemical_formula_weight         400.15
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_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
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_cell_angle_alpha                98.186(5)
_cell_angle_beta                 100.888(5)
_cell_angle_gamma                96.356(4)
_cell_formula_units_Z            2
_cell_length_a                   7.1571(4)
_cell_length_b                   8.4227(4)
_cell_length_c                   13.3083(8)
_cell_measurement_reflns_used    3028
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      72.6
_cell_measurement_theta_min      3.43
_cell_volume                     771.93(8)
_computing_cell_refinement
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CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.36 (release 02-08-2010 CrysAlis171 .NET)
(compiled Nov  6 2009,16:24:50)
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_computing_data_collection
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CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.36 (release 02-08-2010 CrysAlis171 .NET)
(compiled Nov  6 2009,16:24:50)
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_computing_data_reduction
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CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.36 (release 02-08-2010 CrysAlis171 .NET)
(compiled Nov  6 2009,16:24:50)
;
_computing_molecular_graphics    ' ? '
_computing_publication_material  'enCIFer(Allen et al.,2004);PLATON(Spek,2003)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 10.3613
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.957
_diffrn_measurement_device_type  'SuperNova, Single source at offset), Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'SuperNova (Cu) x-ray Source'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0149
_diffrn_reflns_av_sigmaI/netI    0.0151
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            4463
_diffrn_reflns_theta_full        67.50
_diffrn_reflns_theta_max         72.75
_diffrn_reflns_theta_min         3.43
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.188
_exptl_absorpt_correction_T_max  1.217
_exptl_absorpt_correction_T_min  0.378
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CrysAlisPro, Oxford Diffraction Ltd., 
Version 1.171.34.36 (release 02-08-2010 CrysAlis171 .NET) 
(compiled Jan  5 2010,16:28:46) 
Analytical numeric absorption correction using a multifaceted crystal 
model based on expressions derived by R.C. Clark & J.S. Reid. 
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) 
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.722
_exptl_crystal_description       lath
_exptl_crystal_F_000             400
_exptl_crystal_size_max          0.5881
_exptl_crystal_size_mid          0.1945
_exptl_crystal_size_min          0.0490
_refine_diff_density_max         0.339
_refine_diff_density_min         -0.461
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     214
_refine_ls_number_reflns         2943
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0288
_refine_ls_R_factor_gt           0.0280
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0439P)^2^+0.4133P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0744
_refine_ls_wR_factor_ref         0.0748
_reflns_number_gt                2839
_reflns_number_total             2943
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            jo202201w_si_002_2d.cif
_cod_data_source_block           MHCJMA
_cod_original_cell_volume        771.93(7)
_cod_database_code               4026915
_nottingham_internal_coll_name   MHCJMA
_nottingham_internal_coll_number 9949
_nottingham_internal_coll_client MH/CJM
_nottingham_internal_coll_type   custom
_nottingham_internal_coll_frame_time '2 and 8s'
_nottingham_internal_coll_frame_width '1 degree'
_nottingham_internal_coll_frame_method '\w scans'
_nottingham_internal_coll_user   AJB
_nottingham_internal_coll_date   26/11/2010
_nottingham_internal_process_user WL
_nottingham_internal_process_date 30/11/2010
_nottingham_internal_solution_user wl
_nottingham_internal_solution_date 30/11/2010
_nottingham_internal_refinement_user wl
_nottingham_internal_refinement_date 4/2/2011
_nottingham_internal_validation_user wl
_nottingham_internal_validation_date 24/3/2011
_nottingham_internal_archive_date 24/3/2011