Structure, conformational properties and matrix photochemistry of S-(tert-butyl)trifluorothioacetate CF3C(O)SC(CH3)3
Cayón, Vanina M.; Erben, Mauricio F.; Romano, Rosana M.; Stammler, Hans-Georg; Mitzel, Norbert W.; Della Védova, Carlos O.; New Journal of Chemistry 44 (2020) 14568–14577; doi:10.1039/D0NJ03173A

data_7059891
_publ_section_title
;
 Structure, conformational properties and matrix photochemistry of
 S-(tert-butyl)trifluorothioacetate CF3C(O)SC(CH3)3
;
_journal_issue                   34
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              14568
_journal_page_last               14577
_journal_paper_doi               10.1039/D0NJ03173A
_journal_volume                  44
_journal_year                    2020
_chemical_formula_moiety         'C6 H9 F3 O S'
_chemical_formula_sum            'C6 H9 F3 O S'
_chemical_formula_weight         186.19
_chemical_melting_point          199.7(10)
_chemical_name_common            S-(tert-Butyl)trifluorothioacetate
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   difmap
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.3
_audit_creation_date             2020-05-05
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)

XD routine XDCIF
;
_audit_update_record
;
2020-05-18 deposited with the CCDC.	2020-08-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.4183(6)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   12.34413(7)
_cell_length_b                   11.69960(6)
_cell_length_c                   11.73975(9)
_cell_measurement_reflns_used    96946
_cell_measurement_temperature    94.0(2)
_cell_measurement_theta_max      50.7430
_cell_measurement_theta_min      2.3960
_cell_volume                     1687.895(18)
_computing_cell_refinement       'CrysAlisPro 1.171.39.45i (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.45i (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.45i (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'Volkov et al, (2006)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      94.0(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0951
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -22.00  71.00   1.00    4.00    --    0.00  38.00 -90.00   93
  2  \w    -22.00  71.00   1.00    4.00    --    0.00  38.00 120.00   93
  3  \w    -22.00  71.00   1.00    4.00    --    0.00  38.00   0.00   93
  4  \w    -71.00  22.00   1.00    4.00    --    0.00 -38.00-180.00   93
  5  \w     39.00 137.00   1.00   16.00    --   67.67  77.00-120.00   98
  6  \w      0.00  88.00   1.00   16.00    --   67.67 -61.00 -30.00   88
  7  \w      2.00 117.00   1.00   16.00    --   67.67-125.00-180.00  115
  8  \w     39.00 137.00   1.00   16.00    --   67.67  77.00 -90.00   98
  9  \w     39.00 137.00   1.00   16.00    --   67.67  77.00 -30.00   98
 10  \w     39.00 137.00   1.00   16.00    --   67.67  77.00  30.00   98
 11  \w     39.00 137.00   1.00   16.00    --   67.67  77.00 120.00   98
 12  \w     39.00 137.00   1.00   16.00    --   67.67  77.00 -60.00   98
 13  \w     39.00 137.00   1.00   16.00    --   67.67  77.00   0.00   98
 14  \w     -3.00 105.00   1.00   16.00    --   67.67 -94.00   0.00  108
 15  \w     39.00 137.00   1.00   16.00    --   67.67  77.00  60.00   98
 16  \w     39.00 137.00   1.00   16.00    --   67.67  77.00 150.00   98
 17  \w     -2.00  96.00   1.00   16.00    --   67.67 -77.00-180.00   98
 18  \w     39.00 137.00   1.00   16.00    --   67.67  77.00-180.00   98
 19  \w     39.00 137.00   1.00   16.00    --   67.67  77.00-150.00   98
 20  \w     39.00 137.00   1.00   16.00    --   67.67  77.00  90.00   98
 21  \w     -2.00  88.00   1.00   16.00    --   67.67 -45.00  30.00   90
 22  \w     73.00 139.00   1.00   16.00    --   67.67 125.00  60.00   66
 23  \w     -2.00  96.00   1.00   16.00    --   67.67 -77.00-120.00   98
 24  \w     40.00 136.00   1.00   16.00    --   67.67  75.00 171.31   96
 25  \w    -53.00   1.00   1.00    4.00    --    0.00 122.00  -9.00   54
 26  \w    -19.00  68.00   1.00    4.00    --    0.00  57.00  30.00   87
 27  \w    -72.00  38.00   1.00    4.00    --    0.00 -19.00-150.00  110
 28  \w    -22.00  71.00   1.00    4.00    --    0.00  38.00  60.00   93
 29  \w    -19.00  68.00   1.00    4.00    --    0.00  57.00-150.00   87
 30  \w    -20.00  40.00   1.00    4.00    --    0.00 -99.00 -90.00   60
 31  \w     46.00 135.00   1.00   16.00    --   67.67  65.00  60.73   89
 32  \w     73.00 139.00   1.00   16.00    --   67.67 125.00-180.00   66
 33  \w     47.00 137.00   1.00   16.00    --   67.67  45.00 -90.00   90
 34  \w     47.00 137.00   1.00   16.00    --   67.67  45.00-180.00   90
 35  \w     48.00 136.00   1.00   16.00    --   67.67  61.00-150.00   88
 36  \w     43.00 136.00   1.00   16.00    --   67.67  70.00 170.11   93
 37  \w     48.00 136.00   1.00   16.00    --   67.67  61.00  30.00   88
 38  \w     73.00 139.00   1.00   16.00    --   67.67 125.00  30.00   66
 39  \w     47.00 138.00   1.00   16.00    --   67.67  43.00  77.58   91
 40  \w     48.00 137.00   1.00   16.00    --   67.67  50.00  25.85   89
 41  \w     47.00 137.00   1.00   16.00    --   67.67  45.00 150.00   90
 42  \w     47.00 137.00   1.00   16.00    --   67.67  45.00 120.00   90
 43  \w     48.00 136.00   1.00   16.00    --   67.67  61.00 -90.00   88
 44  \w     49.00 136.00   1.00   16.00    --   67.67  54.00 142.86   87
 45  \w     47.00 137.00   1.00   16.00    --   67.67  45.00  90.00   90
 46  \w     41.00 136.00   1.00   16.00    --   67.67  74.00  89.92   95
 47  \w     47.00 137.00   1.00   16.00    --   67.67  45.00 -30.00   90
 48  \w     48.00 136.00   1.00   16.00    --   67.67  61.00 -30.00   88
 49  \w     48.00 104.00   1.00   16.00    --   67.67  61.00-120.00   56
 50  \w     44.00 135.00   1.00   16.00    --   67.67  67.00-146.00   91
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset/far, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0367649000
_diffrn_orient_matrix_UB_12      0.0465864000
_diffrn_orient_matrix_UB_13      0.0072443000
_diffrn_orient_matrix_UB_21      -0.0440848000
_diffrn_orient_matrix_UB_22      0.0387893000
_diffrn_orient_matrix_UB_23      -0.0095084000
_diffrn_orient_matrix_UB_31      -0.0059572000
_diffrn_orient_matrix_UB_32      0.0005193000
_diffrn_orient_matrix_UB_33      0.0595116000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0420
_diffrn_reflns_av_unetI/netI     0.0143
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            350214
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         51.391
_diffrn_reflns_theta_min         1.657
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.376
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.399
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.45i (Rigaku Oxford Diffraction, 2018)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.465
_exptl_crystal_description       cylindrically
_exptl_crystal_F_000             768
_exptl_crystal_recrystallization_method 'From the Melt'
_exptl_crystal_size_max          0.619
_exptl_crystal_size_mid          0.305
_exptl_crystal_size_min          0.269
_refine_diff_density_max         0.229
_refine_diff_density_min         -0.294
_refine_diff_density_rms         0.033
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.506
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     810
_refine_ls_number_reflns         14460
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.037
_refine_ls_R_factor_gt           0.019
_refine_ls_shift/su_max          0.00004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
        calc w2 = 1/[s^2^(Fo^2^)]
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.022
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14460
_reflns_number_total             18678
_reflns_threshold_expression     'I > 3\s(I)'
_cod_data_source_file            d0nj03173a2.cif
_cod_data_source_block           x
_cod_depositor_comments
;Adding full bibliography for 7059891.cif.

 Adding full bibliography for 7059891.cif.
;
_cod_database_code               7059891
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         C6H9F3OS
_chemical_oxdiff_usercomment
'In situ grown at 199.7 K by manually growing a crystal seed, chilled to 198 K witk 3 K/h and to 94 K with 360 K/h'
_reflns_odcompleteness_completeness 99.98
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     49.99
_olex2_refinement_description
;

;