Monitoring dynamic pre-crystallization aggregation processes in solution by VT-DOSY NMR spectroscopy
Mix, Andreas; Lamm, Jan-Hendrik; Schwabedissen, Jan; Gebel, Erich; Stammler, Georg; Mitzel, Norbert Werner; Chemical Communications  (2022) –; doi:10.1039/D1CC05925D

data_7129479
_publ_section_title
;
 Monitoring dynamic pre-crystallization aggregation processes in solution
 by VT-DOSY NMR spectroscopy
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D1CC05925D
_journal_year                    2022
_chemical_formula_moiety         'C5 F4 I N, C7 H8'
_chemical_formula_sum            'C12 H8 F4 I N'
_chemical_formula_weight         369.09
_chemical_melting_point          287
_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     direct
_audit_creation_date             2017-10-09
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2021-05-06 deposited with the CCDC.	2021-12-24 downloaded from the CCDC.
;
_cell_angle_alpha                92.9070(14)
_cell_angle_beta                 94.961(2)
_cell_angle_gamma                94.097(2)
_cell_formula_units_Z            2
_cell_length_a                   7.4116(3)
_cell_length_b                   7.88224(9)
_cell_length_c                   10.6922(2)
_cell_measurement_reflns_used    32146
_cell_measurement_temperature    100.0(1)
_cell_measurement_theta_max      36.6110
_cell_measurement_theta_min      3.1250
_cell_volume                     619.69(3)
_computing_cell_refinement       'CrysAlisPro 1.171.39.15e (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.15e (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.15e (Rigaku OD, 2015)'
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.0(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0951
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.972
_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      7.00 105.00   1.00   16.00    --   35.84  77.00-120.00   98
  2  \w     17.00 104.00   1.00   16.00    --   35.84  57.00  30.00   87
  3  \w     35.00 110.00   1.00   16.00    --   35.84 178.00-120.00   75
  4  \w     -4.00  22.00   1.00   16.00    --   35.84  97.00 -50.16   26
  5  \w     17.00 104.00   1.00   16.00    --   35.84  57.00 -30.00   87
  6  \w     35.00 110.00   1.00   16.00    --   35.84 178.00 -60.00   75
  7  \w     -2.00  25.00   1.00   16.00    --   35.84  95.00-175.00   27
  8  \w     14.00 106.00   1.00   16.00    --   35.84  38.00-120.00   92
  9  \w     35.00 110.00   1.00   16.00    --   35.84 178.00  60.00   75
 10  \w    -20.00  76.00   1.00   16.00    --   35.84 -99.00 120.00   96
 11  \w      7.00 105.00   1.00   16.00    --   35.84  77.00  60.00   98
 12  \w      7.00 105.00   1.00   16.00    --   35.84  77.00 120.00   98
 13  \w     34.00 111.00   1.00   16.00    --   35.84-178.00 120.00   77
 14  \w    -20.00  76.00   1.00   16.00    --   35.84 -99.00 -60.00   96
 15  \w    -33.00  54.00   1.00   16.00    --   35.84 -57.00   0.00   87
 16  \w     34.00 111.00   1.00   16.00    --   35.84-178.00 -30.00   77
 17  \w     17.00 104.00   1.00   16.00    --   35.84  57.00  60.00   87
 18  \w     17.00 104.00   1.00   16.00    --   35.84  57.00 150.00   87
 19  \w     -2.00 108.00   1.00   16.00    --   35.84  19.00  30.00  110
 20  \w     17.00 104.00   1.00   16.00    --   35.84  57.00-120.00   87
 21  \w     17.00 104.00   1.00   16.00    --   35.84  57.00 120.00   87
 22  \w     17.00 104.00   1.00   16.00    --   35.84  57.00 -90.00   87
 23  \w    -35.00 107.00   1.00   16.00    --   35.84   0.00-180.00  142
 24  \w    -35.00 107.00   1.00   16.00    --   35.84   0.00-150.00  142
 25  \w    -35.00 107.00   1.00   16.00    --   35.84   0.00-120.00  142
 26  \w    -35.00 107.00   1.00   16.00    --   35.84   0.00 -90.00  142
 27  \w     14.00 106.00   1.00   16.00    --   35.84  38.00  30.00   92
 28  \w    -35.00 107.00   1.00   16.00    --   35.84   0.00 -30.00  142
 29  \w    -35.00 107.00   1.00   16.00    --   35.84   0.00 -60.00  142
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset/far, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0111710000
_diffrn_orient_matrix_UB_12      0.0028910000
_diffrn_orient_matrix_UB_13      0.0652728000
_diffrn_orient_matrix_UB_21      0.0955384000
_diffrn_orient_matrix_UB_22      0.0021664000
_diffrn_orient_matrix_UB_23      0.0136364000
_diffrn_orient_matrix_UB_31      0.0054139000
_diffrn_orient_matrix_UB_32      0.0902937000
_diffrn_orient_matrix_UB_33      0.0014047000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0125
_diffrn_reflns_av_unetI/netI     0.0083
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.972
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            68657
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.972
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         36.838
_diffrn_reflns_theta_min         2.595
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.614
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.107
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.15e (Rigaku Oxford Diffraction, 2015)
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            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.978
_exptl_crystal_description       cylindrically
_exptl_crystal_F_000             352
_exptl_crystal_size_max          0.624
_exptl_crystal_size_mid          0.39
_exptl_crystal_size_min          0.354
_refine_diff_density_max         1.798
_refine_diff_density_min         -0.657
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     165
_refine_ls_number_reflns         10787
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0177
_refine_ls_R_factor_gt           0.0173
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0316P)^2^+0.1180P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0476
_refine_ls_wR_factor_ref         0.0477
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10641
_reflns_number_total             10787
_reflns_threshold_expression     'I > 2\s(I)'
_twin_special_details
;
Component 2 rotated by -179.9950\% 
 around [-0.07 1.00 -0.07] (reciprocal) or [0.00 1.00 0.00] (direct)
;
_cod_data_source_file            d1cc05925d2.cif
_cod_data_source_block           2_100K
_cod_database_code               7129479
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'C11 H5 F5 I N'
_cell_oxdiff_angle_alpha         92.9070(14)
_cell_oxdiff_angle_beta          94.961(2)
_cell_oxdiff_angle_gamma         94.097(2)
_cell_oxdiff_length_a            7.4116(2)
_cell_oxdiff_length_b            7.88224(9)
_cell_oxdiff_length_c            10.6922(2)
_cell_oxdiff_measurement_reflns_used 32146
_cell_oxdiff_volume              619.69(3)
_shelx_estimated_absorpt_t_max   0.458
_shelx_estimated_absorpt_t_min   0.292
_diffrn_oxdiff_ac3_digest_frames
;
0148f493577466de9410b867f057a371d90276453df
;
_diffrn_oxdiff_ac3_digest_hkl
;
01c8878af9b9efdb0197887cfc9e152964e7cc
;
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H,H,H,H,H) groups
2. Others
 Sof(H12D)=Sof(H12E)=Sof(H12F)=1-FVAR(1)
 Sof(H12A)=Sof(H12B)=Sof(H12C)=FVAR(1)
3.a Aromatic/amide H refined with riding coordinates:
 C7(H7), C8(H8), C9(H9), C10(H10), C11(H11)
3.b Disordered Me refined as rotating group:
 C12(H12A,H12B,H12C,H12D,H12E,H12F)
;
_shelx_res_checksum              45339
_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 8.650
_oxdiff_exptl_absorpt_empirical_full_min 0.656
_oxdiff_twin_integration_method  simultaneous
_oxdiff_twin_items               2