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_7250328
_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 I N4 O2, F6 P'
_chemical_formula_sum            'C12 H12 F6 I N4 O2 P'
_chemical_formula_weight         516.13
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-04-21
_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                 90.9350(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.90190(10)
_cell_length_b                   12.7011(2)
_cell_length_c                   12.2951(2)
_cell_measurement_reflns_used    9902
_cell_measurement_temperature    120.01(10)
_cell_measurement_theta_max      75.9350
_cell_measurement_theta_min      3.4700
_cell_volume                     1702.23(4)
_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      120.01(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 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     19.00  47.00   0.50    0.30    --   52.72 -32.00-172.00   56
  2  \w     61.00  86.00   0.50    0.30    --   52.72  32.00 -13.00   50
  3  \w     62.00  87.00   0.50    0.30    --   53.07  32.00 -13.00   50
  4  \w     -4.00  21.00   0.50    0.30    --   53.07 -32.00-172.00   50
  5  \w    120.00 146.00   0.50    0.80    --  101.90  32.00 -13.00   52
  6  \w     44.00  69.00   0.50    0.80    --  101.90 -32.00-172.00   50
  7  \w     50.00 121.00   0.50    0.30    --   52.72  37.00-150.00  142
  8  \w     37.00  95.00   0.50    0.30    --   53.07-125.00-180.00  116
  9  \w     56.00  96.00   0.50    0.30    --   53.07-125.00  60.00   80
 10  \w    -16.00  48.00   0.50    0.30    --   53.07 -37.00  60.00  128
 11  \w    -17.00  57.00   0.50    0.30    --   53.07 -37.00 -90.00  148
 12  \w     41.00  66.00   0.50    0.30    --   53.07-125.00-120.00   50
 13  \w     66.00 104.00   0.50    0.80    --  101.90 -37.00-120.00   76
 14  \w     75.00 101.00   0.50    0.80    --  101.90 -99.00  30.00   52
 15  \w     44.00  95.00   0.50    0.80    --  101.90 -99.00-150.00  102
 16  \w     90.00 167.00   0.50    0.80    --  101.90  19.00 -60.00  154
 17  \w     59.00 101.00   0.50    0.80    --  101.90 -99.00 120.00   84
 18  \w     37.00  62.00   0.50    0.80    --  101.90 -37.00-120.00   50
 19  \w     43.00 101.00   0.50    0.80    --  101.90 -99.00-120.00  116
 20  \w     67.00  93.00   0.50    0.80    --  101.90 -99.00 -90.00   52
 21  \w     95.00 170.00   0.50    0.80    --  101.90  57.00   0.00  150
 22  \w     38.00  99.00   0.50    0.80    --  101.90 -37.00  60.00  122
 23  \w     39.00 106.00   0.50    0.80    --  101.90 -57.00   0.00  134
;
_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      0.1403267000
_diffrn_orient_matrix_UB_12      0.0022544000
_diffrn_orient_matrix_UB_13      -0.0135280000
_diffrn_orient_matrix_UB_21      -0.0171599000
_diffrn_orient_matrix_UB_22      0.0499830000
_diffrn_orient_matrix_UB_23      -0.1133887000
_diffrn_orient_matrix_UB_31      0.0050369000
_diffrn_orient_matrix_UB_32      0.1104052000
_diffrn_orient_matrix_UB_33      0.0515358000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0311
_diffrn_reflns_av_unetI/netI     0.0256
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            12982
_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         74.501
_diffrn_reflns_theta_min         5.007
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    16.438
_exptl_absorpt_correction_T_max  0.470
_exptl_absorpt_correction_T_min  0.158
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.80a (Rigaku Oxford Diffraction, 2023)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
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    2.014
_exptl_crystal_description       block
_exptl_crystal_F_000             1000
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: methanol/diethylether'
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.877
_refine_diff_density_min         -1.242
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     235
_refine_ls_number_reflns         3479
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.091
_refine_ls_R_factor_all          0.0311
_refine_ls_R_factor_gt           0.0305
_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^)+(0.0382P)^2^+3.4736P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0790
_refine_ls_wR_factor_ref         0.0794
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3389
_reflns_number_total             3479
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5ce00339c2.cif
_cod_data_source_block           3_NS
_cod_depositor_comments
'Adding full bibliography for 7250325--7250334.cif.'
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               7250328
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.265
_shelx_estimated_absorpt_t_min   0.146
_diffrn_oxdiff_digest_frames
;
019e216d949873fc7b9082d3e97863fdda020642ebd
;
_diffrn_oxdiff_digest_hkl
;
019b91102c7e702b5d6756b6f96eefcccbb606
;
_reflns_odcompleteness_completeness 99.97
_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
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 X=CH2 refined with riding coordinates:
 N9(H9A,H9B), N19(H19A,H19B)
;
_shelx_res_checksum              43779
_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 1.205
_oxdiff_exptl_absorpt_empirical_full_min 0.860