Ligand Exchange Among Iodine(I) Complexes
Yu, Shilin; Ward, Jas S.; Dalton Transactions  (2022) –; doi:10.1039/D1DT04309A

data_7709564
_publ_section_title
;
 Ligand Exchange Among Iodine(I) Complexes
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D1DT04309A
_journal_year                    2022
_chemical_formula_moiety         'C12 H24 I N4, F6 P'
_chemical_formula_sum            'C12 H24 F6 I N4 P'
_chemical_formula_weight         496.22
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-01-20
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-12-08 deposited with the CCDC.	2022-02-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   10.34070(10)
_cell_length_b                   17.5114(3)
_cell_length_c                   20.2383(3)
_cell_measurement_reflns_used    10325
_cell_measurement_temperature    119.97(10)
_cell_measurement_theta_max      76.5100
_cell_measurement_theta_min      2.5130
_cell_volume                     3664.75(9)
_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 5.1977
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_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    -86.00  -7.00   1.00    1.00    --  -41.90 125.00  90.00   79
  2  \w    -55.00 -17.00   1.00    1.00    --  -41.90 -57.00 -60.00   38
  3  \w   -114.00 -64.00   1.00    1.00    --  -41.90 -57.00 -60.00   50
  4  \w     56.00 138.00   1.00    2.00    --  112.00 -45.00 120.00   82
  5  \w    105.00 178.00   1.00    2.00    --  112.00 111.00  30.00   73
  6  \w     51.00 103.00   1.00    2.00    --  112.00-111.00   0.00   52
  7  \w     86.00 135.00   1.00    2.00    --  112.00  45.00   0.00   49
  8  \w      7.00  83.00   1.00    1.00    --   42.15 -99.00-150.00   76
  9  \w     45.00 141.00   1.00    2.00    --  112.00 -61.00   0.00   96
 10  \w     36.00 107.00   1.00    2.00    --  112.00-111.00-180.00   71
;
_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      -0.1389921000
_diffrn_orient_matrix_UB_12      0.0000501000
_diffrn_orient_matrix_UB_13      0.0274326000
_diffrn_orient_matrix_UB_21      0.0014181000
_diffrn_orient_matrix_UB_22      -0.0879402000
_diffrn_orient_matrix_UB_23      0.0017072000
_diffrn_orient_matrix_UB_31      0.0535776000
_diffrn_orient_matrix_UB_32      0.0020607000
_diffrn_orient_matrix_UB_33      0.0710041000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0344
_diffrn_reflns_av_unetI/netI     0.0444
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            14602
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.102
_diffrn_reflns_theta_min         3.337
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    15.140
_exptl_absorpt_correction_T_max  0.37192
_exptl_absorpt_correction_T_min  0.29631
_exptl_absorpt_correction_type   sphere
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
Spherical absorption correction
using equivalent radius and absorption coefficient.
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    1.799
_exptl_crystal_description       plate
_exptl_crystal_F_000             1968
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: MeCN/TBME'
_exptl_crystal_size_max          0.255
_exptl_crystal_size_mid          0.095
_exptl_crystal_size_min          0.054
_exptl_crystal_size_rad          0.056
_refine_diff_density_max         0.435
_refine_diff_density_min         -0.748
_refine_diff_density_rms         0.116
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.398(6)
_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     434
_refine_ls_number_reflns         7153
_refine_ls_number_restraints     21
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0287
_refine_ls_R_factor_gt           0.0266
_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^)+(0.0271P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0641
_refine_ls_wR_factor_ref         0.0659
_reflns_Friedel_coverage         0.789
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                6777
_reflns_number_total             7153
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt04309a2.cif
_cod_data_source_block           I_23-2_PF6
_cod_database_code               7709564
_shelxl_version_number           2014/6
_reflns_odcompleteness_completeness 99.66
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     71.98
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.602(6)
 0.398(6)
2. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
3. Rigid body (RIGU) restrains
 C24, C25, N28, C23, C22
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
4.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B), C7(H7A,H7B),
 C12(H12A,H12B), C13(H13A,H13B), C14(H14A,H14B), C15(H15A,H15B), C16(H16A,H16B),
  C17(H17A,H17B), C22(H22A,H22B), C23(H23A,H23B), C24(H24A,H24B), C25(H25A,
 H25B), C26(H26A,H26B), C27(H27A,H27B), C32(H32A,H32B), C33(H33A,H33B),
 C34(H34A,H34B), C35(H35A,H35B), C36(H36A,H36B), C37(H37A,H37B)
;
_shelx_res_checksum              90270
_ins_header
;
TITL OHA-264-1_scale in P2(1)2(1)2(1) 
REM P2(1)2(1)2(1) (#19 in standard setting)
CELL 1.54184  10.340727  17.511351  20.238315  90.0000  90.0000  90.0000
ZERR    8.00   0.000145   0.000250   0.000275   0.0000   0.0000   0.0000
LATT -1
SYMM -x+1/2,-y, z+1/2 
SYMM -x, y+1/2,-z+1/2 
SYMM  x+1/2,-y+1/2,-z 
SFAC C H N F P I
UNIT 96.00 192.00 32.00 48.00 8.00 8.00
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 3.415
_oxdiff_exptl_absorpt_empirical_full_min 0.764