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_7250327
_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, C3 H6 O'
_chemical_formula_sum            'C15 H18 Ag F6 N4 O3 P'
_chemical_formula_weight         555.17
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2023-05-18
_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                90
_cell_angle_beta                 98.5790(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.58960(10)
_cell_length_b                   23.3498(2)
_cell_length_c                   9.92860(10)
_cell_measurement_reflns_used    15699
_cell_measurement_temperature    119.95(16)
_cell_measurement_theta_max      78.2830
_cell_measurement_theta_min      3.8010
_cell_volume                     1969.05(4)
_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_environment      N~2~
_diffrn_ambient_temperature      119.95(16)
_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 1.000
_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     34.00  59.00   0.50    0.45    --  102.01-125.00 -60.00   50
  2  \w     75.00 101.00   0.50    0.45    --  102.01-125.00 -60.00   52
  3  \w     47.00 106.00   0.50    0.45    --  102.01 -99.00 -60.00  118
  4  \w     52.00 106.00   0.50    0.45    --  102.01 -99.00-120.00  108
  5  \w     39.00 104.00   0.50    0.45    --  102.01 -99.00 -30.00  130
  6  \w     80.00 106.00   0.50    0.45    --  102.01 -99.00   0.00   52
  7  \w     38.00  81.00   0.50    0.45    --  102.01 -99.00  30.00   86
  8  \w     53.00 106.00   0.50    0.45    --  102.01 -99.00  60.00  106
  9  \w     75.00 106.00   0.50    0.45    --  102.01 -99.00 120.00   62
 10  \w     41.00 106.00   0.50    0.45    --  107.25 -98.00 170.50  130
 11  \w     39.00  65.00   0.50    0.45    --  102.01 -99.00 120.00   52
 12  \w     -4.00  85.00   0.50    0.20    --   52.15 -99.00 -30.00  178
 13  \w     64.00 106.00   0.50    0.45    --  102.01 -99.00-150.00   84
 14  \w     37.00  92.00   0.50    0.45    --  102.01 -77.00  90.00  110
 15  \w     27.00  52.00   0.50    0.45    --  102.01 -38.00 150.00   50
 16  \w     45.00  71.00   0.50    0.45    --  102.01 -57.00  90.00   52
 17  \w     25.00  50.00   0.50    0.45    --  102.01 -38.00  90.00   50
 18  \w     48.00  74.00   0.50    0.45    --  102.01 -57.00  30.00   52
 19  \w     41.00  66.00   0.50    0.45    --  102.01 -57.00-120.00   50
 20  \w     37.00  63.00   0.50    0.45    --  102.01 -57.00-150.00   52
 21  \w     91.00 147.00   0.50    0.45    --  102.01  19.00-180.00  112
 22  \w    138.00 163.00   0.50    0.45    --  102.01  77.00-180.00   50
 23  \w     95.00 174.00   0.50    0.45    --  102.01  57.00-150.00  158
 24  \w     80.00 105.00   0.50    0.45    --  102.01  77.00-180.00   50
 25  \w     88.00 168.00   0.50    0.45    --  102.01  38.00   0.00  160
 26  \w     81.00 151.00   0.50    0.45    --  102.01  19.00 -30.00  140
 27  \w     89.00 125.00   0.50    0.45    --  102.01  38.00  60.00   72
 28  \w    133.00 158.00   0.50    0.45    --  102.01  38.00  60.00   50
 29  \w    101.00 137.00   0.50    0.45    --  102.01  19.00 120.00   72
 30  \w     29.00 119.00   0.50    0.20    --   52.15  77.00  60.00  180
 31  \w     -3.00  25.00   0.50    0.20    --  -51.53  19.00  60.00   56
 32  \w    -26.00  23.00   0.50    0.20    --  -51.53  38.00   0.00   98
 33  \w    -54.00 -26.00   0.50    0.45    --  -87.67  57.00 -60.00   56
 34  \w     -2.00  24.00   0.50    0.20    --  -51.53  19.00-150.00   52
 35  \w    -53.00 -25.00   0.50    0.45    --  -87.67  57.00-120.00   56
 36  \w    -49.00 -16.00   0.50    0.45    --  -87.67  57.00 -90.00   66
 37  \w   -101.00 -24.00   0.50    0.45    --  -87.67  77.00 150.00  154
 38  \w   -163.00-100.00   0.50    0.45    --  -87.67 -38.00 120.00  126
 39  \w   -155.00-129.00   0.50    0.45    --  -87.67 -77.00  30.00   52
 40  \w   -102.00 -73.00   0.50    0.45    --  -87.67 -77.00  30.00   58
;
_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      -0.1201033000
_diffrn_orient_matrix_UB_12      0.0472535000
_diffrn_orient_matrix_UB_13      0.0185907000
_diffrn_orient_matrix_UB_21      0.0339734000
_diffrn_orient_matrix_UB_22      0.0291655000
_diffrn_orient_matrix_UB_23      -0.1317431000
_diffrn_orient_matrix_UB_31      -0.1314332000
_diffrn_orient_matrix_UB_32      -0.0357093000
_diffrn_orient_matrix_UB_33      -0.0831827000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0321
_diffrn_reflns_av_unetI/netI     0.0201
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            26148
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.496
_diffrn_reflns_theta_min         3.786
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet R (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    9.757
_exptl_absorpt_correction_T_max  0.864
_exptl_absorpt_correction_T_min  0.548
_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    1.873
_exptl_crystal_description       plate
_exptl_crystal_F_000             1104
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: acetone/pentane'
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.877
_refine_diff_density_min         -0.594
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     285
_refine_ls_number_reflns         4034
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0293
_refine_ls_R_factor_gt           0.0277
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0468P)^2^+1.5259P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0730
_refine_ls_wR_factor_ref         0.0741
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3815
_reflns_number_total             4034
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5ce00339c2.cif
_cod_data_source_block           2_Acetone
_cod_depositor_comments
'Adding full bibliography for 7250325--7250334.cif.'
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               7250327
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.829
_shelx_estimated_absorpt_t_min   0.413
_diffrn_oxdiff_digest_frames
;
01ee3e7adf6def75cbb5a91a1d14ca4ac003442f00b
;
_diffrn_oxdiff_digest_hkl
;
018dde8c7aaa4c9a1d873cba869e854738d908
;
_reflns_odcompleteness_completeness 99.98
_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.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C5(H5), C6(H6), C12(H12), C14(H14), C15(H15), C16(H16)
2.b Idealised Me refined as rotating group:
 C203(H20A,H20B,H20C), C204(H20D,H20E,H20F)
;
_shelx_res_checksum              6143
_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 1.353
_oxdiff_exptl_absorpt_empirical_full_min 0.812