The Solid-state Hierarchy and Iodination Potential of [bis(3-acetaminopyridine)iodine(I)]PF6
Ward, Jas S.; CrystEngComm  (2022) –; doi:10.1039/D2CE01225A

data_7245595
_publ_section_title
;
 The Solid-state Hierarchy and Iodination Potential of
 [bis(3-acetaminopyridine)iodine(I)]PF6
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D2CE01225A
_journal_year                    2022
_chemical_formula_moiety         'C14 H16 I N4 O2, F6 P'
_chemical_formula_sum            'C14 H16 F6 I N4 O2 P'
_chemical_formula_weight         544.18
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-07-29
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2022-08-01 deposited with the CCDC.	2022-09-30 downloaded from the CCDC.
;
_cell_angle_alpha                103.504(3)
_cell_angle_beta                 99.401(2)
_cell_angle_gamma                90.172(2)
_cell_formula_units_Z            4
_cell_length_a                   9.9264(3)
_cell_length_b                   13.3351(4)
_cell_length_c                   14.6878(5)
_cell_measurement_reflns_used    12874
_cell_measurement_temperature    119.97(10)
_cell_measurement_theta_max      76.5810
_cell_measurement_theta_min      3.0770
_cell_volume                     1863.36(11)
_computing_cell_refinement       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      119.97(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3895
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.995
_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    -87.00  -6.00   1.00    1.00    --  -42.04 125.00-180.00   81
  2  \w   -117.00 -18.00   1.00    1.00    --  -42.04 -37.00  30.00   99
  3  \w    -75.00  34.00   1.00    1.00    --  -42.04  77.00 -60.00  109
  4  \w    -66.00  32.00   1.00    1.00    --  -42.04  37.00-150.00   98
  5  \w      9.00  42.00   1.00    1.00    --   42.04  80.00  41.77   33
  6  \w    103.00 178.00   1.00    3.00    --  112.00  77.00 -90.00   75
  7  \w     40.00 141.00   1.00    3.00    --  112.00 -61.00 -30.00  101
  8  \w     85.00 178.00   1.00    3.00    --  112.00  53.00  22.46   93
  9  \w     36.00 109.00   1.00    3.00    --  112.00-111.00  90.00   73
 10  \w     84.00 178.00   1.00    3.00    --  112.00  30.00-150.00   94
 11  \w     29.00 107.00   1.00    3.00    --  112.00 -94.00-120.00   78
 12  \w    103.00 178.00   1.00    3.00    --  112.00  77.00 -30.00   75
 13  \w     36.00 140.00   1.00    3.00    --  112.00 -30.00-150.00  104
 14  \w     29.00 107.00   1.00    3.00    --  112.00 -94.00 -60.00   78
 15  \w     36.00 109.00   1.00    3.00    --  112.00-111.00 150.00   73
 16  \w     59.00 178.00   1.00    3.00    --  112.00  15.00 150.00  119
 17  \w     36.00 109.00   1.00    3.00    --  112.00-111.00   0.00   73
 18  \w     29.00 107.00   1.00    3.00    --  112.00 -94.00-180.00   78
 19  \w    -87.00  -6.00   1.00    1.00    --  -42.04 125.00   0.00   81
 20  \w   -114.00 -14.00   1.00    1.00    --  -42.04 -57.00 150.00  100
 21  \w   -114.00 -14.00   1.00    1.00    --  -42.04 -57.00-120.00  100
 22  \w      7.00  33.00   1.00    1.00    --   42.04  84.00 176.97   26
 23  \w      8.00  42.00   1.00    1.00    --   42.04  82.00-139.48   34
 24  \w      8.00  34.00   1.00    1.00    --   42.04  83.00   4.59   26
 25  \w     59.00 178.00   1.00    3.00    --  112.00  15.00 -30.00  119
 26  \w     83.00 178.00   1.00    3.00    --  112.00  61.00-150.00   95
 27  \w     83.00 178.00   1.00    3.00    --  112.00  61.00 120.00   95
 28  \w     83.00 178.00   1.00    3.00    --  112.00  61.00 -30.00   95
 29  \w     83.00 178.00   1.00    3.00    --  112.00  61.00  60.00   95
 30  \w     83.00 178.00   1.00    3.00    --  112.00  61.00 150.00   95
 31  \w     83.00 178.00   1.00    3.00    --  112.00  61.00 -60.00   95
 32  \w     80.00 178.00   1.00    3.00    --  112.00  74.00-105.87   98
 33  \w     83.00 178.00   1.00    3.00    --  112.00  61.00   0.00   95
 34  \w     83.00 178.00   1.00    3.00    --  112.00  61.00  90.00   95
 35  \w     83.00 178.00   1.00    3.00    --  112.00  61.00  30.00   95
 36  \w     81.00 178.00   1.00    3.00    --  112.00  69.00-133.29   97
 37  \w   -117.00 -56.00   1.00    1.00    --  -42.04-156.00-109.00   61
 38  \w   -117.00 -18.00   1.00    1.00    --  -42.04 -37.00 -90.00   99
 39  \w      7.00  33.00   1.00    1.00    --   42.04  84.00 -45.14   26
 40  \w      9.00  42.00   1.00    1.00    --   42.04  81.00  81.06   33
 41  \w      9.00  42.00   1.00    1.00    --   42.04  81.00 -80.80   33
 42  \w      9.00  42.00   1.00    1.00    --   42.04  80.00 105.41   33
 43  \w     83.00 134.00   1.00    3.00    --  112.00  61.00-180.00   51
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1231079000
_diffrn_orient_matrix_UB_12      -0.0700443000
_diffrn_orient_matrix_UB_13      0.0009525000
_diffrn_orient_matrix_UB_21      0.0134750000
_diffrn_orient_matrix_UB_22      0.0171621000
_diffrn_orient_matrix_UB_23      0.1085798000
_diffrn_orient_matrix_UB_31      -0.0972369000
_diffrn_orient_matrix_UB_32      -0.0945592000
_diffrn_orient_matrix_UB_33      -0.0136429000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0543
_diffrn_reflns_av_unetI/netI     0.0350
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            37453
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.491
_diffrn_reflns_theta_min         3.139
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    15.056
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.165
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
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            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.940
_exptl_crystal_description       plate
_exptl_crystal_F_000             1064
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: MeCN'
_exptl_crystal_size_max          0.168
_exptl_crystal_size_mid          0.164
_exptl_crystal_size_min          0.014
_refine_diff_density_max         6.174
_refine_diff_density_min         -1.350
_refine_diff_density_rms         0.189
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     509
_refine_ls_number_reflns         7610
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.0630
_refine_ls_R_factor_gt           0.0555
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0876P)^2^+7.4916P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1436
_refine_ls_wR_factor_ref         0.1512
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6527
_reflns_number_total             7610
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ce01225a2.cif
_cod_data_source_block           3_2
_cod_original_cell_volume        1863.36(10)
_cod_database_code               7245595
_shelxl_version_number           2014/6
_reflns_odcompleteness_completeness 99.53
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 N7(H7), N17(H17), C2(H2), C4(H4), C5(H5), C6(H6), C12(H12), C14(H14),
 C15(H15), C16(H16), N27(H27), N37(H37), C22(H22), C24(H24), C25(H25), C26(H26),
  C32(H32), C34(H34), C35(H35), C36(H36)
2.b Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C20(H20A,H20B,H20C), C30(H30A,H30B,H30C), C40(H40A,H40B,
 H40C)
;
_shelx_res_checksum              60611
_ins_header
;
TITL OHD383_numabs in P-1 
REM P-1 (#2 in standard setting)
CELL 1.54184   9.926442  13.335083  14.687814 103.5037  99.4007  90.1715
ZERR    4.00   0.000255   0.000429   0.000523   0.0029   0.0025   0.0023
LATT  1
SFAC C H N O F P I
UNIT 56.00 64.00 16.00 8.00 24.00 4.00 4.00
TREF
HKLF 4
END
;
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 1.320
_oxdiff_exptl_absorpt_empirical_full_min 0.794