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

data_7245596
_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             2022-07-25
_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                98.710(5)
_cell_angle_beta                 92.055(4)
_cell_angle_gamma                105.936(5)
_cell_formula_units_Z            2
_cell_length_a                   8.1008(4)
_cell_length_b                   10.1196(7)
_cell_length_c                   12.4667(6)
_cell_measurement_reflns_used    3550
_cell_measurement_temperature    200.01(10)
_cell_measurement_theta_max      76.7460
_cell_measurement_theta_min      3.5780
_cell_volume                     968.14(10)
_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)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      200.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3895
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.987
_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    -53.00 -12.00   1.00    1.00    --  -42.42 125.00 -30.00   41
  2  \w    -86.00 -60.00   1.00    1.00    --  -42.42 125.00 -30.00   26
  3  \w    -67.00  32.00   1.00    1.00    --  -42.42  37.00-120.00   99
  4  \w   -105.00 -18.00   1.00    1.00    --  -42.42 -37.00  60.00   87
  5  \w      6.00  77.00   1.00    1.00    --   42.42 -99.00 -60.00   71
  6  \w    106.00 178.00   1.00    1.00    --  112.00  61.00  60.00   72
  7  \w     38.00 109.00   1.00    1.00    --  112.00-111.00 -90.00   71
  8  \w     45.00 110.00   1.00    1.00    --  112.00 -77.00 -90.00   65
  9  \w     36.00  67.00   1.00    1.00    --  112.00-111.00-180.00   31
 10  \w     70.00 109.00   1.00    1.00    --  112.00-111.00  60.00   39
 11  \w     70.00 105.00   1.00    1.00    --  112.00-111.00-180.00   35
 12  \w     41.00  66.00   1.00    1.00    --  112.00-111.00  60.00   25
 13  \w     44.00  72.00   1.00    1.00    --  112.00-111.00-150.00   28
 14  \w     77.00 102.00   1.00    1.00    --  112.00-111.00-150.00   25
 15  \w    132.00 178.00   1.00    1.00    --  112.00  45.00 -30.00   46
 16  \w     87.00 173.00   1.00    1.00    --  112.00  30.00  30.00   86
 17  \w     88.00 114.00   1.00    1.00    --  112.00  45.00 -30.00   26
 18  \w     50.00 122.00   1.00    1.00    --  112.00 -61.00 -60.00   72
 19  \w     40.00 122.00   1.00    1.00    --  112.00 -61.00  30.00   82
 20  \w     78.00 120.00   1.00    1.00    --  112.00 178.00 -60.00   42
 21  \w     86.00 178.00   1.00    1.00    --  112.00  45.00 120.00   92
;
_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      0.0839657000
_diffrn_orient_matrix_UB_12      -0.0009251000
_diffrn_orient_matrix_UB_13      0.1126310000
_diffrn_orient_matrix_UB_21      0.0640289000
_diffrn_orient_matrix_UB_22      0.1604468000
_diffrn_orient_matrix_UB_23      0.0194935000
_diffrn_orient_matrix_UB_31      -0.1680078000
_diffrn_orient_matrix_UB_32      0.0069200000
_diffrn_orient_matrix_UB_33      0.0516484000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0546
_diffrn_reflns_av_unetI/netI     0.0517
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            6849
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.479
_diffrn_reflns_theta_min         3.599
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    14.489
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.042
_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    1.867
_exptl_crystal_description       plate
_exptl_crystal_F_000             532
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: DCM/pentane'
_exptl_crystal_size_max          0.377
_exptl_crystal_size_mid          0.311
_exptl_crystal_size_min          0.025
_refine_diff_density_max         2.326
_refine_diff_density_min         -1.451
_refine_diff_density_rms         0.203
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     289
_refine_ls_number_reflns         3914
_refine_ls_number_restraints     126
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0660
_refine_ls_R_factor_gt           0.0611
_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^)+(0.1403P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1642
_refine_ls_wR_factor_ref         0.1735
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3523
_reflns_number_total             3914
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ce01225a2.cif
_cod_data_source_block           3_1
_cod_database_code               7245596
_shelxl_version_number           2014/6
_reflns_odcompleteness_completeness 99.57
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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. Rigid body (RIGU) restrains
 P101, F102, F103, F104, F105, F106, F107
 with sigma for 1-2 distances of 0.003 and sigma for 1-3 distances of 0.003
 P111, F112, F113, F114, F115, F116, F117
 with sigma for 1-2 distances of 0.003 and sigma for 1-3 distances of 0.003
3. Others
 Sof(P101)=Sof(F102)=Sof(F103)=Sof(F104)=Sof(F105)=Sof(F106)=Sof(F107)=1-FVAR(1)
 Sof(P111)=Sof(F112)=Sof(F113)=Sof(F114)=Sof(F115)=Sof(F116)=Sof(F117)=FVAR(1)
4.a Free rotating group:
 P101(F102,F103,F104,F105,F106,F107), P111(F112,F113,F114,F115,F116,F117)
4.b 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)
4.c Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C20(H20A,H20B,H20C)
;
_shelx_res_checksum              94790
_ins_header
;
TITL OHD384-200K_numabs in P-1 
REM P-1 (#2 in standard setting)
CELL 1.54184   8.100771  10.119558  12.466745  98.7100  92.0552 105.9361
ZERR    2.00   0.000447   0.000721   0.000643   0.0050   0.0043   0.0055
LATT  1
SFAC C H N O F P I
UNIT 28.00 32.00 8.00 4.00 12.00 2.00 2.00
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 1.909
_oxdiff_exptl_absorpt_empirical_full_min 0.755