Hierarchical iodine(i) complexes of nicotinamide
Mohan, Sharath; Valkonen, Arto; Rissanen, Kari; Ward, Jas S.; CrystEngComm 27 (2025) 3295–3301; doi:10.1039/D5CE00339C

data_7250326
_publ_section_title
;
 Hierarchical iodine(i) complexes of nicotinamide
;
_journal_issue                   20
_journal_name_full               CrystEngComm
_journal_page_first              3295
_journal_page_last               3301
_journal_paper_doi               10.1039/D5CE00339C
_journal_volume                  27
_journal_year                    2025
_chemical_formula_moiety         'C12 H12 Ag N4 O2, F6 P, 3(C2 H3 N)'
_chemical_formula_sum            'C18 H21 Ag F6 N7 O2 P'
_chemical_formula_weight         620.26
_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             2023-04-14
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2025-03-21 deposited with the CCDC.	2025-04-24 downloaded from the CCDC.
;
_cell_angle_alpha                83.660(2)
_cell_angle_beta                 72.550(2)
_cell_angle_gamma                84.305(2)
_cell_formula_units_Z            2
_cell_length_a                   8.8771(2)
_cell_length_b                   10.4273(3)
_cell_length_c                   13.5713(4)
_cell_measurement_reflns_used    11453
_cell_measurement_temperature    120.00(10)
_cell_measurement_theta_max      76.6940
_cell_measurement_theta_min      3.4140
_cell_volume                     1188.18(6)
_computing_cell_refinement       'CrysAlisPro 1.171.42.80a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.80a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.80a (Rigaku OD, 2023)'
_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                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            'HyPix-Arc 100'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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      2.00  27.00   0.50    0.20    --   52.72 -21.00-105.00   50
  2  \w     -8.00  40.00   0.50    0.20    --   53.07 -21.00-105.00   96
  3  \w     41.00  67.00   0.50    0.20    --   53.07 -21.00-105.00   52
  4  \w     65.00 123.00   0.50    0.20    --   53.07  21.00  60.00  116
  5  \w     85.00 172.00   0.50    0.40    --  101.90  21.00  60.00  174
  6  \w     41.00  99.00   0.50    0.40    --  101.90 -21.00-105.00  116
  7  \w     55.00  80.00   0.50    0.20    --   52.72  21.00  60.00   50
  8  \w      5.00  69.00   0.50    0.20    --   52.72 -77.00 -90.00  128
  9  \w     73.00  98.00   0.50    0.20    --   53.07-125.00 -60.00   50
 10  \w    -15.00  54.00   0.50    0.20    --   53.07 -57.00  60.00  138
 11  \w    -17.00  48.00   0.50    0.20    --   53.07 -37.00-180.00  130
 12  \w     49.00  89.00   0.50    0.20    --   53.07-125.00-120.00   80
 13  \w     37.00  75.00   0.50    0.20    --   53.07-125.00  30.00   76
 14  \w     35.00  80.00   0.50    0.20    --   53.07-125.00 150.00   90
 15  \w     44.00 101.00   0.50    0.20    --   53.07  57.00-180.00  114
 16  \w      9.00  34.00   0.50    0.20    --   53.07 -37.00-150.00   50
 17  \w     45.00 100.00   0.50    0.40    --  101.90 -99.00  60.00  110
 18  \w     75.00 115.00   0.50    0.40    --  101.90 -19.00  90.00   80
 19  \w     65.00 100.00   0.50    0.40    --  101.90 -57.00  30.00   70
 20  \w     42.00  77.00   0.50    0.40    --  101.90 -57.00-120.00   70
 21  \w     44.00 105.00   0.50    0.40    --  101.90 -99.00-180.00  122
 22  \w     32.00  65.00   0.50    0.40    --  101.90 -19.00  90.00   66
 23  \w     96.00 152.00   0.50    0.40    --  101.90 125.00  60.00  112
 24  \w     99.00 124.00   0.50    0.40    --  101.90  37.00 -90.00   50
 25  \w     50.00  81.00   0.50    0.40    --  101.90 -99.00  30.00   62
 26  \w     38.00 103.00   0.50    0.40    --  101.90 -37.00  30.00  130
 27  \w     81.00 106.00   0.50    0.40    --  101.90 -99.00  90.00   50
 28  \w    127.00 174.00   0.50    0.40    --  101.90  37.00 -90.00   94
 29  \w    107.00 132.00   0.50    0.40    --  101.90 125.00-150.00   50
 30  \w     57.00 106.00   0.50    0.40    --  101.90 -99.00 -90.00   98
 31  \w     39.00 109.00   0.50    0.40    --  101.90-125.00 -90.00  140
 32  \w     37.00  63.00   0.50    0.40    --  101.90 -57.00  30.00   52
 33  \w    108.00 142.00   0.50    0.40    --  101.90 125.00 150.00   68
 34  \w     43.00  78.00   0.50    0.40    --  101.90 -99.00-150.00   70
 35  \w     49.00 103.00   0.50    0.40    --  101.90 -99.00 -60.00  108
 36  \w     84.00 109.00   0.50    0.40    --  101.90 -57.00-120.00   50
 37  \w     61.00  86.00   0.50    0.40    --  101.90 -57.00-180.00   50
 38  \w     50.00 106.00   0.50    0.40    --  101.90 -99.00 150.00  112
 39  \w    145.00 172.00   0.50    0.40    --  101.90  37.00 -30.00   54
 40  \w     50.00 107.00   0.50    0.40    --  107.75-104.00  15.17  114
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dualflex, HyPix-Arc 100'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1331797000
_diffrn_orient_matrix_UB_12      0.0938613000
_diffrn_orient_matrix_UB_13      -0.0306889000
_diffrn_orient_matrix_UB_21      -0.1244201000
_diffrn_orient_matrix_UB_22      0.1157368000
_diffrn_orient_matrix_UB_23      0.0126001000
_diffrn_orient_matrix_UB_31      -0.0061662000
_diffrn_orient_matrix_UB_32      -0.0007869000
_diffrn_orient_matrix_UB_33      0.1147246000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0277
_diffrn_reflns_av_unetI/netI     0.0239
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            16097
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.499
_diffrn_reflns_theta_min         3.426
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    8.167
_exptl_absorpt_correction_T_max  0.28098
_exptl_absorpt_correction_T_min  0.18728
_exptl_absorpt_correction_type   sphere
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.80a (Rigaku Oxford Diffraction, 2023)
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    1.734
_exptl_crystal_description       block
_exptl_crystal_F_000             620
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: acetonitrile/diisopropylether'
_exptl_crystal_size_max          0.281
_exptl_crystal_size_mid          0.146
_exptl_crystal_size_min          0.137
_exptl_crystal_size_rad          0.100
_refine_diff_density_max         0.656
_refine_diff_density_min         -0.867
_refine_diff_density_rms         0.104
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.106
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     395
_refine_ls_number_reflns         4842
_refine_ls_number_restraints     126
_refine_ls_restrained_S_all      1.207
_refine_ls_R_factor_all          0.0358
_refine_ls_R_factor_gt           0.0338
_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^)+(0.0656P)^2^+0.4342P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1028
_refine_ls_wR_factor_ref         0.1051
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4370
_reflns_number_total             4842
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5ce00339c2.cif
_cod_data_source_block           2_3MeCN
_cod_depositor_comments
'Adding full bibliography for 7250325--7250334.cif.'
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7250326
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.401
_shelx_estimated_absorpt_t_min   0.207
_diffrn_oxdiff_digest_frames
;
014165e8018131604cdddb8bf19390b95903492c46d
;
_diffrn_oxdiff_digest_hkl
;
01f1ec8754422a989f32b5d2ebc774343bdc19
;
_reflns_odcompleteness_completeness 99.90
_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,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid body (RIGU) restrains
 P101, F102, F103, F104, F105, F106, F107
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.003
 P111, F112, F113, F114, F115, F116, F117
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.003
3. Others
 Sof(P111)=Sof(F112)=Sof(F113)=Sof(F114)=Sof(F115)=Sof(F116)=Sof(F117)=1-FVAR(1)
 Sof(P101)=Sof(F102)=Sof(F103)=Sof(F104)=Sof(F105)=Sof(F106)=Sof(F107)=FVAR(1)
4.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C5(H5), C6(H6), C12(H12), C14(H14), C15(H15), C16(H16)
4.b Idealised Me refined as rotating group:
 C203(H20A,H20B,H20C), C213(H21A,H21B,H21C), C223(H22A,H22B,H22C)
;
_shelx_res_checksum              79837
_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 1.520
_oxdiff_exptl_absorpt_empirical_full_min 0.745