PhICl<sub>2</sub> is activated by chloride ions.
Tania, ?; Poynder, Tiffany B.; Kaur, Aishvaryadeep; Barwise, Lachlan; Houston, Sevan D.; Nair, Akshay J.; Clegg, Jack K.; Wilson, David J. D.; Dutton, Jason L.; Dalton transactions (Cambridge, England : 2003) 50 (2021) 11986–11991; doi:10.1039/d1dt02565a

data_7707951
_publ_section_title
;
 PhICl<sub>2</sub> is activated by chloride ions.
;
_journal_issue                   34
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              11986
_journal_page_last               11991
_journal_paper_doi               10.1039/d1dt02565a
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety         '2(C6 H5 Cl2 I), Cl, C8 H20 N'
_chemical_formula_sum            'C20 H30 Cl5 I2 N'
_chemical_formula_weight         715.50
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-06-18
_audit_creation_method
;
Olex2 1.3-ac4
(compiled 2020.11.27 svn.r5f609507 for Rigaku Oxford Diffraction, GUI svn.r6214)
;
_audit_update_record
;
2021-06-21 deposited with the CCDC.	2021-08-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.359(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.8786(4)
_cell_length_b                   17.2644(6)
_cell_length_c                   15.6853(6)
_cell_measurement_reflns_used    10950
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      32.9130
_cell_measurement_theta_min      2.3860
_cell_volume                     2622.70(18)
_computing_cell_refinement       'CrysAlisPro 1.171.41.103a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.103a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.103a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 5.8140
_diffrn_detector_type            'Pilatus 300K'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_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    -25.00  11.00   0.50    2.50    --    8.20  91.00 145.00   72
  2  \w     16.00  42.00   0.50    2.50    --    8.20  91.00 145.00   52
  3  \w    -16.00  69.00   0.50    2.50    --    8.20  77.00 -90.00  170
  4  \w    -13.00  34.00   0.50    2.50    --    8.20 -91.00  32.00   94
  5  \w     -1.00  45.00   0.50    2.50    --    8.20 -99.00 120.00   92
  6  \w     11.00  45.00   0.50    2.50    --    8.20 -99.00 -30.00   68
  7  \w    -65.00 -11.00   0.50    2.50    --    8.20 -57.00 -30.00  108
  8  \w    -37.00 -12.00   0.50    2.50    --   -9.76 -57.00 -30.00   50
  9  \w    -80.00 -55.00   0.50    2.50    --   -9.76 -57.00 -30.00   50
 10  \w     -1.00  24.00   0.50    2.50    --   -9.76  91.00 145.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, Pilatus 300K'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0347861000
_diffrn_orient_matrix_UB_12      -0.0007783000
_diffrn_orient_matrix_UB_13      0.0441144000
_diffrn_orient_matrix_UB_21      0.0256940000
_diffrn_orient_matrix_UB_22      -0.0374998000
_diffrn_orient_matrix_UB_23      -0.0062858000
_diffrn_orient_matrix_UB_31      0.0591004000
_diffrn_orient_matrix_UB_32      0.0167542000
_diffrn_orient_matrix_UB_33      -0.0119537000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0390
_diffrn_reflns_av_unetI/netI     0.0290
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            16675
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.281
_diffrn_reflns_theta_min         2.411
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.916
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.77196
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.103a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.812
_exptl_crystal_description       block
_exptl_crystal_F_000             1392
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.775
_refine_diff_density_min         -0.568
_refine_diff_density_rms         0.110
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     130
_refine_ls_number_reflns         3242
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0283
_refine_ls_R_factor_gt           0.0239
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0158P)^2^+6.5299P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0493
_refine_ls_wR_factor_ref         0.0506
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2902
_reflns_number_total             3242
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt02565a2.cif
_cod_data_source_block           sjkc21aj08
_cod_depositor_comments          'Adding full bibliography for 7707951.cif.'
_cod_database_code               7707951
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C14 H16 I Cl3 N'
_shelx_estimated_absorpt_t_max   0.868
_shelx_estimated_absorpt_t_min   0.669
_reflns_odcompleteness_completeness 99.76
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     28.22
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C9(H9A,H9B)
2.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C2(H2), C3(H3), C5(H5), C4(H4)
2.c Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C8(H8A,H8B,H8C)
;
_shelx_res_checksum              33086
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.328
_oxdiff_exptl_absorpt_empirical_full_min 0.817