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

data_7709563
_publ_section_title
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 Ligand Exchange Among Iodine(I) Complexes
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D1DT04309A
_journal_year                    2022
_chemical_formula_moiety         'C10 H15 I N5, F6 P'
_chemical_formula_sum            'C10 H15 F6 I N5 P'
_chemical_formula_weight         477.14
_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_Hall           'P 2c -2ac'
_space_group_name_H-M_alt        'P c a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-03-28
_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                   10.7960(3)
_cell_length_b                   20.9622(5)
_cell_length_c                   14.3983(3)
_cell_measurement_reflns_used    5945
_cell_measurement_temperature    120.01(10)
_cell_measurement_theta_max      74.7910
_cell_measurement_theta_min      4.1890
_cell_volume                     3258.45(14)
_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      120.01(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 0.996
_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    -68.00  -8.00   1.00    1.00    --  -41.65 125.00   0.00   60
  2  \w   -119.00  -6.00   1.00    1.00    --  -41.65 -19.00 -90.00  113
  3  \w     60.00  95.00   1.00    1.00    --   41.65-125.00-120.00   35
  4  \w    105.00 163.00   1.00    5.00    --  112.00  77.00-120.00   58
  5  \w    117.00 178.00   1.00    5.00    --  112.00  77.00  30.00   61
  6  \w     56.00  98.00   1.00    5.00    --  112.00-111.00  90.00   42
  7  \w     29.00 104.00   1.00    5.00    --  112.00 -94.00   0.00   75
  8  \w     55.00 108.00   1.00    5.00    --  112.00-111.00 -30.00   53
  9  \w     40.00 138.00   1.00    5.00    --  112.00 -45.00  60.00   98
 10  \w    117.00 177.00   1.00    5.00    --  112.00  77.00   0.00   60
 11  \w      8.00  60.00   1.00    1.00    --   42.15 -77.00 -60.00   52
 12  \w    107.00 144.00   1.00    5.00    --  112.00 178.00 -30.00   37
;
_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      -0.1415870000
_diffrn_orient_matrix_UB_12      -0.0013367000
_diffrn_orient_matrix_UB_13      0.0135050000
_diffrn_orient_matrix_UB_21      0.0040766000
_diffrn_orient_matrix_UB_22      -0.0733169000
_diffrn_orient_matrix_UB_23      0.0071678000
_diffrn_orient_matrix_UB_31      0.0178379000
_diffrn_orient_matrix_UB_32      0.0051802000
_diffrn_orient_matrix_UB_33      0.1058196000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0491
_diffrn_reflns_av_unetI/netI     0.0509
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            13192
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.124
_diffrn_reflns_theta_min         4.218
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    17.024
_exptl_absorpt_correction_T_max  0.750
_exptl_absorpt_correction_T_min  0.172
_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    1.945
_exptl_crystal_description       plate
_exptl_crystal_F_000             1856
_exptl_crystal_size_max          0.182
_exptl_crystal_size_mid          0.157
_exptl_crystal_size_min          0.017
_refine_diff_density_max         4.230
_refine_diff_density_min         -0.798
_refine_diff_density_rms         0.177
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.182(17)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     422
_refine_ls_number_reflns         4634
_refine_ls_number_restraints     56
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0606
_refine_ls_R_factor_gt           0.0545
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0982P)^2^+2.0706P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1361
_refine_ls_wR_factor_ref         0.1434
_reflns_Friedel_coverage         0.917
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                4184
_reflns_number_total             4634
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt04309a2.cif
_cod_data_source_block           I_18_16_PF6
_cod_database_code               7709563
_shelxl_version_number           2014/6
_reflns_odcompleteness_completeness 99.61
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     71.98
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.818(17)
 0.182(17)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 N33-C36
 1.45 with sigma of 0.01
4. Rigid body (RIGU) restrains
 N31, N32, N33, C34, C35, C36
 with sigma for 1-2 distances of 0.003 and sigma for 1-3 distances of 0.003
5.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C6(H6), C14(H14), C15(H15), C22(H22), C23(H23),
 C25(H25), C26(H26), C34(H34), C35(H35)
5.b Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C16(H16A,H16B,H16C), C28(H28A,H28B,H28C),
 C29(H29A,H29B,H29C), C36(H36A,H36B,H36C)
;
_shelx_res_checksum              2111
_ins_header
;
TITL OHA311-1_numabs_ana in Pca2(1) 
REM Pca2(1) (#29, found as Pb2(1)a in a-cb setting)
CELL 1.54184  10.796005  20.962167  14.398289  90.0000  90.0000  90.0000
ZERR    8.00   0.000260   0.000512   0.000348   0.0000   0.0000   0.0000
LATT -1
SYMM -x,-y, z+1/2 
SYMM  x+1/2,-y, z 
SYMM -x+1/2, y, z+1/2 
SFAC C H N F P I
UNIT 80.00 120.00 40.00 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 1.371
_oxdiff_exptl_absorpt_empirical_full_min 0.765