On the activation of PhICl<sub>2</sub> with pyridine.
Poynder, Tiffany B.; Chamorro Orué, Analia I; Tania, ?; Sharp-Bucknall, Lachlan; Flynn, Matthew T.; Wilson, David J. D.; Athukorala Arachchige, Kasun S.; Clegg, Jack K.; Dutton, Jason L.; Chemical communications (Cambridge, England) 57 (2021) 4970–4973; doi:10.1039/d1cc01567b

data_7128178
_publ_section_title
;
 On the activation of PhICl<sub>2</sub> with pyridine.
;
_journal_issue                   40
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              4970
_journal_page_last               4973
_journal_paper_doi               10.1039/d1cc01567b
_journal_volume                  57
_journal_year                    2021
_chemical_formula_moiety         'C F3 O3 S, C7 H10 Cl N2'
_chemical_formula_sum            'C8 H10 Cl F3 N2 O3 S'
_chemical_formula_weight         306.69
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2021-02-18
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6226)
;
_audit_update_record
;
2021-03-18 deposited with the CCDC.	2021-04-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.923(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.7784(2)
_cell_length_b                   9.3743(2)
_cell_length_c                   16.8499(5)
_cell_measurement_reflns_used    5234
_cell_measurement_temperature    149.99(10)
_cell_measurement_theta_max      71.0360
_cell_measurement_theta_min      5.2470
_cell_volume                     1222.09(6)
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      149.99(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix3000
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_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    -21.00   8.00   0.50    1.14    --  -38.50  91.00 109.00   58
  2  \w    -62.00 -27.00   0.50    1.14    --  -38.50  91.00 109.00   70
  3  \w     45.00  70.00   0.50    4.54    --  100.00 -91.00  -4.00   50
  4  \w    108.00 161.00   0.50    4.54    --  100.00  91.00 109.00  106
  5  \w    -64.00 -18.00   0.50    1.14    --  -38.50  77.00   0.00   92
  6  \w    -22.00  25.00   0.50    1.14    --  -38.50  77.00 -60.00   94
  7  \w    -81.00 -23.00   0.50    1.14    --  -38.50 -65.00-180.00  116
  8  \w    -13.00  14.00   0.50    1.14    --  -38.50  77.00   0.00   54
  9  \w    -52.00 -15.00   0.50    1.14    --  -38.50 138.00  90.00   74
 10  \w    -63.00 -32.00   0.50    1.14    --  -38.50  77.00 -60.00   62
 11  \w    -95.00 -64.00   0.50    1.14    --  -38.50 -32.00-150.00   62
 12  \w    -92.00 -57.00   0.50    1.14    --  -38.50 138.00  90.00   70
 13  \w    -95.00 -70.00   0.50    1.14    --  -38.50 -43.00 -30.00   50
 14  \w    -41.00  13.00   0.50    1.14    --  -38.50  32.00 -30.00  108
 15  \w    -96.00 -32.00   0.50    1.14    --  -38.50 -32.00  90.00  128
 16  \w    -56.00 -30.00   0.50    1.14    --  -38.50 -32.00-150.00   52
 17  \w    -96.00 -21.00   0.50    1.14    --  -38.50 -54.00   0.00  150
 18  \w     32.00  58.00   0.50    1.14    --   42.60-104.00-150.00   52
 19  \w    -19.00   9.00   0.50    1.14    --   42.60 -43.00-150.00   56
 20  \w     79.00 106.00   0.50    1.14    --   42.60  65.00  90.00   54
 21  \w     29.00  71.00   0.50    1.14    --   42.60  65.00  90.00   84
 22  \w     14.00  39.00   0.50    1.14    --   42.60 -91.00  -4.00   50
 23  \w     38.00  98.00   0.50    1.14    --   42.60  32.00  60.00  120
 24  \w     90.00 115.00   0.50    4.54    --  100.00 -77.00 150.00   50
 25  \w     78.00 104.00   0.50    4.54    --  100.00 -50.00-150.00   52
 26  \w    103.00 129.00   0.50    4.54    --  100.00 117.00  60.00   52
 27  \w     88.00 161.00   0.50    4.54    --  100.00  42.00 -30.00  146
 28  \w     77.00 103.00   0.50    4.54    --  100.00-117.00 -60.00   52
 29  \w    102.00 154.00   0.50    4.54    --  100.00 117.00 150.00  104
 30  \w     62.00 104.00   0.50    4.54    --  100.00 -96.00 120.00   84
 31  \w     87.00 118.00   0.50    4.54    --  100.00 -68.00 -30.00   62
 32  \w     42.00  67.00   0.50    4.54    --  100.00 -77.00 150.00   50
 33  \w     44.00  70.00   0.50    4.54    --  100.00-117.00 -60.00   52
 34  \w     84.00 109.00   0.50    4.54    --  100.00-117.00-150.00   50
 35  \w     84.00 150.00   0.50    4.54    --  100.00  50.00  60.00  132
 36  \w    111.00 155.00   0.50    4.54    --  100.00  33.00  30.00   88
 37  \w     29.00 114.00   0.50    4.54    --  100.00 -17.00 150.00  170
 38  \w     93.00 154.00   0.50    4.54    --  100.00  33.00 120.00  122
 39  \w     91.00 120.00   0.50    4.54    --  100.00  33.00-150.00   58
 40  \w     38.00 124.00   0.50    4.54    --  100.00-141.00 150.64  172
 41  \w     38.00 121.00   0.50    4.54    --  100.00 -68.00  90.00  166
 42  \w     35.00  62.00   0.50    4.54    --  100.00-117.00-150.00   54
 43  \w     39.00  65.00   0.50    4.54    --  100.00 -96.00  90.00   52
 44  \w     95.00 145.00   0.50    4.54    --  100.00 145.00 -90.00  100
 45  \w     32.00  81.00   0.50    4.54    --  100.00 -96.00 -60.00   98
 46  \w     37.00 107.00   0.50    4.54    --  100.00-117.00-120.00  140
 47  \w     45.00 105.00   0.50    4.54    --  100.00-117.00   0.00  120
 48  \w     55.00 111.00   0.50    4.54    --  100.00 -68.00 -60.00  112
 49  \w     79.00 111.00   0.50    4.54    --  100.00 -50.00 -30.00   64
 50  \w     84.00 109.00   0.50    4.54    --  100.00-117.00 -30.00   50
 51  \w     44.00  73.00   0.50    4.54    --  100.00 -59.00-180.00   58
 52  \w     80.00 107.00   0.50    4.54    --  100.00 -59.00-180.00   54
 53  \w     97.00 122.00   0.50    4.54    --  100.00-145.00 120.00   50
 54  \w     39.00  65.00   0.50    4.54    --  100.00-145.00 120.00   52
 55  \w    121.00 147.00   0.50    4.54    --  100.00  77.00 -90.00   52
 56  \w     84.00 109.00   0.50    4.54    --  100.00-117.00  30.00   50
 57  \w     89.00 133.00   0.50    4.54    --  100.00  50.00   0.00   88
 58  \w     39.00  65.00   0.50    4.54    --  100.00 -50.00-150.00   52
 59  \w     39.00  73.00   0.50    4.54    --  100.00 -50.00 -30.00   68
 60  \w     39.00 108.00   0.50    4.54    --  100.00 -33.00  30.00  138
 61  \w     72.00  97.00   0.50    4.54    --  100.00 -71.00-139.47   50
 62  \w    114.00 139.00   0.50    4.54    --  100.00 117.00   0.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, HyPix3000'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1499471000
_diffrn_orient_matrix_UB_12      -0.0731907000
_diffrn_orient_matrix_UB_13      -0.0514580000
_diffrn_orient_matrix_UB_21      0.1182644000
_diffrn_orient_matrix_UB_22      -0.0234344000
_diffrn_orient_matrix_UB_23      -0.0667194000
_diffrn_orient_matrix_UB_31      0.0564278000
_diffrn_orient_matrix_UB_32      -0.1452933000
_diffrn_orient_matrix_UB_33      0.0366910000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0324
_diffrn_reflns_av_unetI/netI     0.0253
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            11583
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.295
_diffrn_reflns_theta_min         5.278
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.807
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.74472
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.667
_exptl_crystal_description       plate
_exptl_crystal_F_000             624
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.869
_refine_diff_density_min         -0.531
_refine_diff_density_rms         0.131
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     169
_refine_ls_number_reflns         2360
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0857
_refine_ls_R_factor_gt           0.0788
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1546P)^2^+1.3136P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2045
_refine_ls_wR_factor_ref         0.2133
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2099
_reflns_number_total             2360
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc01567b2.cif
_cod_data_source_block           3
_cod_depositor_comments
'Adding full bibliography for 7128176--7128179.cif.'
_cod_database_code               7128178
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C7H10SF3O3ClN2
_chemical_oxdiff_usercomment     'tania t40 attempt 4'
_shelx_estimated_absorpt_t_max   0.761
_shelx_estimated_absorpt_t_min   0.478
_reflns_odcompleteness_completeness 94.63
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C2(H2A), C1(H1), C5(H5)
2.b Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C7(H7A,H7B,H7C)
;
_shelx_res_checksum              185
_shelx_hkl_checksum              98622