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

data_7245594
_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         'C11 H16 I N2 O, F6 P'
_chemical_formula_sum            'C11 H16 F6 I N2 O P'
_chemical_formula_weight         464.13
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-07-11
_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                90
_cell_angle_beta                 100.6590(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.47010(10)
_cell_length_b                   14.79040(10)
_cell_length_c                   10.52560(10)
_cell_measurement_reflns_used    9046
_cell_measurement_temperature    120.00(10)
_cell_measurement_theta_max      76.2280
_cell_measurement_theta_min      5.1960
_cell_volume                     1601.84(2)
_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      120.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1947
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.989
_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   -110.00 -23.00   1.00    1.00    --  -42.17 -37.00 -30.00   87
  2  \w    -74.00  30.00   1.00    1.00    --  -42.17  77.00 120.00  104
  3  \w     14.00 114.00   1.00    1.00    --   42.17  57.00-120.00  100
  4  \w     37.00  75.00   1.00    1.00    --   42.17 -77.00-120.00   38
  5  \w     45.00  74.00   1.00    5.00    --  112.00-111.00 -60.00   29
  6  \w     45.00  71.00   1.00    5.00    --  112.00-111.00  90.00   26
  7  \w    130.00 168.00   1.00    5.00    --  112.00  30.00  30.00   38
  8  \w    141.00 173.00   1.00    5.00    --  112.00 111.00 120.00   32
  9  \w    104.00 157.00   1.00    5.00    --  112.00  77.00  90.00   53
 10  \w     58.00 109.00   1.00    5.00    --  112.00-111.00 150.00   51
 11  \w     77.00 103.00   1.00    5.00    --  112.00-111.00 -60.00   26
 12  \w     37.00 109.00   1.00    5.00    --  112.00-111.00   0.00   72
 13  \w    108.00 135.00   1.00    5.00    --  112.00 111.00 120.00   27
 14  \w     76.00 109.00   1.00    5.00    --  112.00-111.00  90.00   33
 15  \w    148.00 177.00   1.00    5.00    --  112.00  30.00 -60.00   29
 16  \w    106.00 132.00   1.00    5.00    --  112.00  30.00 -60.00   26
 17  \w     84.00 109.00   1.00    5.00    --  112.00  30.00  60.00   25
 18  \w    128.00 178.00   1.00    5.00    --  112.00  30.00  60.00   50
 19  \w     45.00 138.00   1.00    5.00    --  112.00 -45.00   0.00   93
 20  \w     36.00  71.00   1.00    5.00    --  112.00 -77.00 -60.00   35
 21  \w     97.00 128.00   1.00    5.00    --  112.00 -77.00 -60.00   31
 22  \w     37.00 107.00   1.00    5.00    --  112.00-111.00 -90.00   70
 23  \w    123.00 178.00   1.00    5.00    --  112.00  77.00 -30.00   55
 24  \w     29.00 107.00   1.00    5.00    --  112.00 -94.00-180.00   78
 25  \w     85.00 114.00   1.00    5.00    --  112.00  30.00  30.00   29
;
_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      -0.0035821000
_diffrn_orient_matrix_UB_12      0.0211796000
_diffrn_orient_matrix_UB_13      0.1426212000
_diffrn_orient_matrix_UB_21      0.1465566000
_diffrn_orient_matrix_UB_22      0.0210458000
_diffrn_orient_matrix_UB_23      0.0242219000
_diffrn_orient_matrix_UB_31      -0.0300094000
_diffrn_orient_matrix_UB_32      0.0998471000
_diffrn_orient_matrix_UB_33      -0.0352839000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0211
_diffrn_reflns_av_unetI/netI     0.0194
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            12018
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.694
_diffrn_reflns_theta_min         4.297
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    17.284
_exptl_absorpt_correction_T_max  0.569
_exptl_absorpt_correction_T_min  0.146
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
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    1.925
_exptl_crystal_description       needle
_exptl_crystal_F_000             904
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: DCM/TBME'
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.081
_exptl_crystal_size_min          0.047
_refine_diff_density_max         1.185
_refine_diff_density_min         -0.661
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     202
_refine_ls_number_reflns         3333
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0235
_refine_ls_R_factor_gt           0.0229
_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^)+(0.0315P)^2^+1.4006P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0580
_refine_ls_wR_factor_ref         0.0584
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3248
_reflns_number_total             3333
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ce01225a2.cif
_cod_data_source_block           4
_cod_database_code               7245594
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.497
_shelx_estimated_absorpt_t_min   0.104
_reflns_odcompleteness_completeness 99.77
_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 C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C12(H12A,H12B)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C5(H5), C6(H6), N7(H7)
2.c Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C)
;
_shelx_res_checksum              49785
_ins_header
;
TITL OHD377_numabs_ana in P2(1)/c 
REM P2(1)/c (#14 in standard setting)
CELL 1.54184  10.470146  14.790379  10.525594  90.0000 100.6589  90.0000
ZERR    4.00   0.000127   0.000145   0.000134   0.0000   0.0012   0.0000
LATT  1
SYMM -x, y+1/2,-z+1/2 
SFAC C H N O F P I
UNIT 44.00 64.00 8.00 4.00 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 1.542
_oxdiff_exptl_absorpt_empirical_full_min 0.663