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

data_7245593
_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         'C18 H22 Ag N6 O2, F6 P'
_chemical_formula_sum            'C18 H22 Ag F6 N6 O2 P'
_chemical_formula_weight         607.25
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2022-07-26
_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                108.995(4)
_cell_angle_beta                 101.944(4)
_cell_angle_gamma                92.083(4)
_cell_formula_units_Z            2
_cell_length_a                   7.2685(3)
_cell_length_b                   12.4304(6)
_cell_length_c                   14.1913(6)
_cell_measurement_reflns_used    5325
_cell_measurement_temperature    120.00(10)
_cell_measurement_theta_max      76.4660
_cell_measurement_theta_min      3.3560
_cell_volume                     1178.65(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)'
_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 10.3895
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.988
_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   -114.00 -23.00   1.00    1.00    --  -42.29 -42.00 -93.00   91
  2  \w    -49.00  -6.00   1.00    1.00    --  -42.29 125.00  60.00   43
  3  \w   -114.00 -28.00   1.00    1.00    --  -42.29 -37.00   0.00   86
  4  \w    -87.00 -12.00   1.00    1.00    --  -42.29 125.00 150.00   75
  5  \w     42.00  84.00   1.00    1.00    --   42.29-125.00  60.00   42
  6  \w    106.00 162.00   1.00    1.00    --  112.00  77.00  30.00   56
  7  \w    115.00 172.00   1.00    1.00    --  112.00  77.00 150.00   57
  8  \w    125.00 167.00   1.00    1.00    --  112.00  61.00   0.00   42
  9  \w     39.00 134.00   1.00    1.00    --  112.00 -45.00   0.00   95
 10  \w     36.00 109.00   1.00    1.00    --  112.00-111.00 -60.00   73
 11  \w     30.00 106.00   1.00    1.00    --  112.00 -94.00-150.00   76
 12  \w     71.00 108.00   1.00    1.00    --  112.00-111.00 120.00   37
 13  \w     38.00 109.00   1.00    1.00    --  112.00-111.00-180.00   71
 14  \w    123.00 174.00   1.00    1.00    --  112.00 111.00   0.00   51
 15  \w     30.00 107.00   1.00    1.00    --  112.00 -94.00  30.00   77
 16  \w    104.00 173.00   1.00    1.00    --  112.00  77.00 -60.00   69
 17  \w     36.00 107.00   1.00    1.00    --  112.00 -94.00 -30.00   71
 18  \w    101.00 177.00   1.00    1.00    --  112.00  45.00  90.00   76
 19  \w     84.00 110.00   1.00    1.00    --  112.00  61.00   0.00   26
;
_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      0.1938059000
_diffrn_orient_matrix_UB_12      -0.0155244000
_diffrn_orient_matrix_UB_13      0.0597967000
_diffrn_orient_matrix_UB_21      -0.0712060000
_diffrn_orient_matrix_UB_22      -0.1252426000
_diffrn_orient_matrix_UB_23      -0.0191354000
_diffrn_orient_matrix_UB_31      0.0699933000
_diffrn_orient_matrix_UB_32      -0.0383665000
_diffrn_orient_matrix_UB_33      -0.0999293000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0271
_diffrn_reflns_av_unetI/netI     0.0286
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            8783
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.495
_diffrn_reflns_theta_min         3.386
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    8.204
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.154
_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    1.711
_exptl_crystal_description       block
_exptl_crystal_F_000             608
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: DCM/pentane'
_exptl_crystal_size_max          0.378
_exptl_crystal_size_mid          0.255
_exptl_crystal_size_min          0.101
_refine_diff_density_max         0.536
_refine_diff_density_min         -0.547
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     317
_refine_ls_number_reflns         4755
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0300
_refine_ls_R_factor_gt           0.0281
_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^)+(0.0493P)^2^+0.3808P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0755
_refine_ls_wR_factor_ref         0.0775
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4505
_reflns_number_total             4755
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ce01225a2.cif
_cod_data_source_block           2_2MeCN
_cod_original_cell_volume        1178.64(10)
_cod_database_code               7245593
_shelxl_version_number           2014/6
_reflns_odcompleteness_completeness 98.79
_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:
 N17(H17), C2(H2), C4(H4), C5(H5), C6(H6), C12(H12), C14(H14), C15(H15),
 C16(H16)
2.b Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C20(H20A,H20B,H20C), C213(H21A,H21B,H21C), C203(H20D,
 H20E,H20F)
;
_shelx_res_checksum              63505
_ins_header
;
TITL OHD385_numabs in P-1 
REM P-1 (#2 in standard setting)
CELL 1.54184   7.268526  12.430411  14.191306 108.9955 101.9436  92.0831
ZERR    2.00   0.000332   0.000591   0.000571   0.0040   0.0037   0.0038
LATT  1
SFAC C H N O F P Ag
UNIT 36.00 44.00 12.00 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 1.496
_oxdiff_exptl_absorpt_empirical_full_min 0.786