Dihypoiodites Stabilised by 4-ethylpyridine through O-I-N Halogen Bonds
Kramer, Eric; Yu, Shilin; Ward, Jas S.; Rissanen, Kari; Dalton Transactions  (2021) –; doi:10.1039/D1DT03324G

data_7708565
_publ_section_title
;
 Dihypoiodites Stabilised by 4-ethylpyridine through O-I-N Halogen Bonds
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D1DT03324G
_journal_year                    2021
_chemical_formula_moiety         'C22 H22 I2 N2 O4'
_chemical_formula_sum            'C22 H22 I2 N2 O4'
_chemical_formula_weight         632.21
_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             2021-03-06
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-08-24 deposited with the CCDC.	2021-10-14 downloaded from the CCDC.
;
_cell_angle_alpha                94.664(4)
_cell_angle_beta                 95.181(4)
_cell_angle_gamma                107.477(4)
_cell_formula_units_Z            2
_cell_length_a                   8.1534(3)
_cell_length_b                   9.6858(4)
_cell_length_c                   15.4795(8)
_cell_measurement_reflns_used    3812
_cell_measurement_temperature    120.01(10)
_cell_measurement_theta_max      76.6000
_cell_measurement_theta_min      2.8580
_cell_volume                     1153.67(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      120.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1977
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.993
_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    -65.00  33.00   1.00    1.00    --  -41.65  37.00  30.00   98
  2  \w   -107.00 -18.00   1.00    1.00    --  -41.65 -57.00  90.00   89
  3  \w    -65.00  31.00   1.00    1.00    --  -41.65  57.00-120.00   96
  4  \w     46.00  98.00   1.00    1.00    --   41.65-125.00  60.00   52
  5  \w     89.00 134.00   1.00    1.00    --  112.00 -45.00  30.00   45
  6  \w     30.00  77.00   1.00    1.00    --  112.00 -94.00 -60.00   47
  7  \w    104.00 175.00   1.00    1.00    --  112.00  77.00  30.00   71
  8  \w     39.00  69.00   1.00    1.00    --  112.00 -45.00  30.00   30
  9  \w     61.00 116.00   1.00    1.00    --  112.00 178.00 -60.00   55
 10  \w     78.00 107.00   1.00    1.00    --  112.00 -94.00 -60.00   29
 11  \w     39.00 138.00   1.00    1.00    --  112.00 -45.00 -90.00   99
 12  \w     29.00  72.00   1.00    1.00    --  112.00 -94.00 120.00   43
 13  \w     75.00 106.00   1.00    1.00    --  112.00 -94.00 120.00   31
 14  \w     37.00 101.00   1.00    1.00    --  112.00 -94.00  60.00   64
 15  \w     40.00  83.00   1.00    1.00    --  112.00-111.00-150.00   43
 16  \w     38.00 109.00   1.00    1.00    --  112.00-111.00 -90.00   71
 17  \w     37.00 178.00   1.00    1.00    --  112.00   0.00-180.00  141
;
_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      0.1898950000
_diffrn_orient_matrix_UB_12      0.0019810000
_diffrn_orient_matrix_UB_13      0.0015977000
_diffrn_orient_matrix_UB_21      -0.0253731000
_diffrn_orient_matrix_UB_22      -0.0317180000
_diffrn_orient_matrix_UB_23      -0.1002864000
_diffrn_orient_matrix_UB_31      0.0558244000
_diffrn_orient_matrix_UB_32      0.1648126000
_diffrn_orient_matrix_UB_33      -0.0076262000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0443
_diffrn_reflns_av_unetI/netI     0.0507
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            7530
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.128
_diffrn_reflns_theta_min         2.885
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    21.662
_exptl_absorpt_correction_T_max  0.718
_exptl_absorpt_correction_T_min  0.091
_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    1.820
_exptl_crystal_description       plate
_exptl_crystal_F_000             612
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: DCM/TBME'
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.153
_exptl_crystal_size_min          0.016
_refine_diff_density_max         1.348
_refine_diff_density_min         -1.286
_refine_diff_density_rms         0.169
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     273
_refine_ls_number_reflns         4475
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0500
_refine_ls_R_factor_gt           0.0431
_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^)+(0.0795P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1167
_refine_ls_wR_factor_ref         0.1270
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3833
_reflns_number_total             4475
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt03324g2.cif
_cod_data_source_block           1
_cod_original_cell_volume        1153.66(9)
_cod_database_code               7708565
_shelxl_version_number           2014/6
_reflns_odcompleteness_completeness 98.85
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     71.98
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C17(H17A,H17B)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C6(H6), C12(H12), C13(H13), C15(H15), C16(H16),
 C23(H23), C24(H24), C25(H25), C26(H26)
2.c Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C18(H18A,H18B,H18C)
;
_shelx_res_checksum              42090
_shelx_hkl_checksum              34862
_ins_header
;
TITL OIE020_numabs_ana in P-1 
REM P-1 (#2 in standard setting)
CELL 1.54184   8.153375   9.685768  15.479468  94.6638  95.1811 107.4768
ZERR    2.00   0.000314   0.000437   0.000755   0.0038   0.0035   0.0037
LATT  1
SFAC C H N O I
UNIT 44.00 44.00 4.00 8.00 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 1.473
_oxdiff_exptl_absorpt_empirical_full_min 0.569