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_7250325
_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, 2(C2 H3 N)'
_chemical_formula_sum            'C16 H18 Ag F6 N6 O2 P'
_chemical_formula_weight         579.20
_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                115.091(2)
_cell_angle_beta                 103.4530(10)
_cell_angle_gamma                90.1780(10)
_cell_formula_units_Z            2
_cell_length_a                   7.51700(10)
_cell_length_b                   12.2366(2)
_cell_length_c                   13.2587(2)
_cell_measurement_reflns_used    13454
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      76.1520
_cell_measurement_theta_min      4.0310
_cell_volume                     1066.99(3)
_computing_cell_refinement       'CrysAlisPro 1.171.42.89a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.89a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.89a (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_temperature      120.0
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            'HyPix-Arc 100'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.997
_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     82.00 116.00   0.50    0.25    --  101.94-131.00-122.00   68
  2  \w     56.00  97.00   0.50    0.10    --   52.65-131.00-122.00   82
  3  \w     44.00 111.00   0.50    0.25    --  101.94-125.00   0.00  134
  4  \w     89.00 122.00   0.50    0.25    --  101.94-139.00  62.00   66
  5  \w     36.00  88.00   0.50    0.25    --  101.94-125.00  30.00  104
  6  \w     36.00  69.00   0.50    0.25    --  101.94-125.00 120.00   66
  7  \w     39.00  64.00   0.50    0.25    --  101.94-125.00 150.00   50
  8  \w     47.00  72.00   0.50    0.10    --   52.65-139.00  62.00   50
  9  \w     48.00  79.00   0.50    0.25    --  101.94 -99.00 -60.00   62
 10  \w     46.00 104.00   0.50    0.25    --  101.94 -99.00 -90.00  116
 11  \w     47.00 106.00   0.50    0.25    --  101.94 -99.00-180.00  118
 12  \w     35.00  84.00   0.50    0.25    --  101.94 -99.00-120.00   98
 13  \w     60.00 105.00   0.50    0.25    --  101.94 -99.00  30.00   90
 14  \w     59.00 106.00   0.50    0.25    --  101.94 -99.00  90.00   94
 15  \w     37.00  79.00   0.50    0.25    --  101.94 -77.00  30.00   84
 16  \w     53.00  78.00   0.50    0.25    --  101.94 -57.00 120.00   50
 17  \w     46.00  79.00   0.50    0.25    --  101.94 -57.00  90.00   66
 18  \w     90.00 116.00   0.50    0.25    --  101.94 -77.00  30.00   52
 19  \w     26.00  51.00   0.50    0.25    --  101.94 -38.00  60.00   50
 20  \w     25.00  50.00   0.50    0.25    --  101.94 -38.00  90.00   50
 21  \w     25.00  50.00   0.50    0.25    --  101.94 -38.00   0.00   50
 22  \w     25.00  50.00   0.50    0.25    --  101.94 -38.00  30.00   50
 23  \w     26.00  51.00   0.50    0.25    --  101.94 -38.00 -60.00   50
 24  \w     30.00  55.00   0.50    0.25    --  101.94 -57.00 -90.00   50
 25  \w     25.00  50.00   0.50    0.25    --  101.94 -38.00 -90.00   50
 26  \w     72.00 172.00   0.50    0.25    --  101.94  19.00-150.00  200
 27  \w     72.00 172.00   0.50    0.25    --  101.94  19.00 -60.00  200
 28  \w    106.00 132.00   0.50    0.25    --  101.94 131.00 -51.00   52
 29  \w     73.00  98.00   0.50    0.10    --   52.65 139.00 122.00   50
 30  \w    107.00 140.00   0.50    0.25    --  101.94 139.00 122.00   66
 31  \w    123.00 164.00   0.50    0.25    --  101.94 125.00 -30.00   82
 32  \w     28.00 109.00   0.50    0.10    --   52.65  77.00 120.00  162
 33  \w    -54.00 -19.00   0.50    0.25    --  -87.73  57.00  90.00   70
 34  \w    -96.00 -71.00   0.50    0.25    --  -87.73 139.00 122.00   50
 35  \w    -93.00 -68.00   0.50    0.10    --  -54.15 139.00 122.00   50
 36  \w   -106.00 -56.00   0.50    0.25    --  -87.73 131.00 -51.00  100
 37  \w    -83.00 -55.00   0.50    0.10    --  -54.15 131.00 -51.00   56
 38  \w    -53.00 -27.00   0.50    0.25    --  -87.73  57.00 -60.00   52
 39  \w   -164.00 -66.00   0.50    0.25    --  -87.73 -19.00  60.00  196
 40  \w   -136.00-111.00   0.50    0.25    --  -87.73-139.00  62.00   50
 41  \w   -124.00 -72.00   0.50    0.10    --  -54.15-139.00  62.00  104
 42  \w   -125.00 -70.00   0.50    0.10    --  -54.15-131.00-122.00  110
 43  \w   -156.00 -91.00   0.50    0.25    --  -87.73-125.00-180.00  130
 44  \w   -103.00 -38.00   0.50    0.10    --  -54.15 -57.00-150.00  130
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, HyPix-Arc 100'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1015757000
_diffrn_orient_matrix_UB_12      0.1131941000
_diffrn_orient_matrix_UB_13      0.0063456000
_diffrn_orient_matrix_UB_21      -0.0442028000
_diffrn_orient_matrix_UB_22      -0.0577021000
_diffrn_orient_matrix_UB_23      -0.1325865000
_diffrn_orient_matrix_UB_31      -0.1809281000
_diffrn_orient_matrix_UB_32      0.0586881000
_diffrn_orient_matrix_UB_33      -0.0042743000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0221
_diffrn_reflns_av_unetI/netI     0.0211
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            15797
_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         74.499
_diffrn_reflns_theta_min         4.016
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet R (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    9.028
_exptl_absorpt_correction_T_max  0.664
_exptl_absorpt_correction_T_min  0.412
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.89a (Rigaku Oxford Diffraction, 2023)
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    1.803
_exptl_crystal_description       block
_exptl_crystal_F_000             576
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: acetonitrile/diethylether'
_exptl_crystal_size_max          0.143
_exptl_crystal_size_mid          0.087
_exptl_crystal_size_min          0.068
_refine_diff_density_max         0.564
_refine_diff_density_min         -0.432
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     311
_refine_ls_number_reflns         4349
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0231
_refine_ls_R_factor_gt           0.0226
_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^)+(0.0314P)^2^+0.6009P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0584
_refine_ls_wR_factor_ref         0.0587
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4236
_reflns_number_total             4349
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5ce00339c2.cif
_cod_data_source_block           2_2MeCN
_cod_depositor_comments
'Adding full bibliography for 7250325--7250334.cif.'
_cod_original_cell_volume        1066.98(3)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7250325
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.571
_shelx_estimated_absorpt_t_min   0.365
_diffrn_oxdiff_digest_frames
;
01ea38f49157bd3936107fb66ff7902bde03710535c
;
_diffrn_oxdiff_digest_hkl
;
01d99e57b775230b879b807f5012e3896445bb
;
_reflns_odcompleteness_completeness 99.72
_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. Uiso/Uaniso restraints and constraints
Uanis(N211) = Uanis(C212) = Uanis(C214)
3. Others
 Sof(C214)=Sof(C215)=Sof(H21D)=Sof(H21E)=Sof(H21F)=1-FVAR(1)
 Sof(C212)=Sof(C213)=Sof(H21A)=Sof(H21B)=Sof(H21C)=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), C215(H21D,H21E,H21F)
;
_shelx_res_checksum              60003
_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 1.118
_oxdiff_exptl_absorpt_empirical_full_min 0.936