Average orientation of a fluoroaromatic molecule in lipid bilayers from DFT-informed NMR measurements of <sup>1</sup>H-<sup>19</sup>F dipolar couplings.
Hughes, Eleri; Griffin, John M.; Coogan, Michael P.; Middleton, David A.; Physical chemistry chemical physics : PCCP 20 (2018) 18207–18215; doi:10.1039/c8cp01064a

data_7230818
_publ_section_title
;
 Average orientation of a fluoroaromatic molecule in lipid bilayers from
 DFT-informed NMR measurements of <sup>1</sup>H-<sup>19</sup>F dipolar
 couplings.
;
_journal_issue                   27
_journal_name_full               'Physical chemistry chemical physics : PCCP'
_journal_page_first              18207
_journal_page_last               18215
_journal_paper_doi               10.1039/c8cp01064a
_journal_volume                  20
_journal_year                    2018
_chemical_formula_moiety         'C13 H9 F N2 S, C H4 O'
_chemical_formula_sum            'C14 H13 F N2 O S'
_chemical_formula_weight         276.32
_chemical_name_common            'Fluorobenzathiazole aniline'
_chemical_name_systematic        'Fluorobenzathiazole aniline'
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2017-11-09
_audit_creation_method
;
Olex2 1.2-ac21
(compiled 2015.09.16 svn.r134, GUI svn.r4998)
;
_audit_update_record
;
2017-11-09 deposited with the CCDC.
2018-05-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   9.54533(14)
_cell_length_b                   14.9685(2)
_cell_length_c                   17.9615(3)
_cell_measurement_reflns_used    12277
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      76.4100
_cell_measurement_theta_min      4.9140
_cell_volume                     2566.33(7)
_computing_cell_refinement       'CrysAlisPro 1.171.38.44a (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.44a (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.44a (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2303
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.996
_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   -115.00 -17.00   1.00    1.50    --  -41.22 -38.00  30.00   98
  2  \w    -96.00  -2.00   1.00    1.50    --  -41.22 125.00  90.00   94
  3  \w      1.00  82.00   1.00    1.50    --   41.22 -99.00  60.00   81
  4  \w     30.00 109.00   1.00    6.00    --  112.00 -95.00-180.00   79
  5  \w     30.00 109.00   1.00    6.00    --  112.00 -95.00-150.00   79
  6  \w     30.00 109.00   1.00    6.00    --  112.00 -95.00 -90.00   79
  7  \w     79.00 178.00   1.00    6.00    --  112.00  77.00 -90.00   99
  8  \w     30.00 109.00   1.00    6.00    --  112.00 -95.00 150.00   79
  9  \w     36.00 116.00   1.00    6.00    --  112.00-111.00  60.00   80
 10  \w     59.00 178.00   1.00    6.00    --  112.00  15.00-180.00  119
 11  \w    -66.00  33.00   1.00    1.50    --  -41.22  38.00 -30.00   99
 12  \w   -113.00 -13.00   1.00    1.50    --  -41.22 -57.00-180.00  100
 13  \w   -113.00 -13.00   1.00    1.50    --  -41.22 -57.00 -60.00  100
 14  \w     79.00 178.00   1.00    6.00    --  112.00  77.00  60.00   99
 15  \w     79.00 178.00   1.00    6.00    --  112.00  77.00-150.00   99
 16  \w     86.00 174.00   1.00    6.00    --  112.00  45.00 -30.00   88
 17  \w     84.00 178.00   1.00    6.00    --  112.00  30.00  30.00   94
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0510218000
_diffrn_orient_matrix_UB_12      -0.0112069000
_diffrn_orient_matrix_UB_13      0.0808930000
_diffrn_orient_matrix_UB_21      0.1490410000
_diffrn_orient_matrix_UB_22      -0.0270445000
_diffrn_orient_matrix_UB_23      0.0239643000
_diffrn_orient_matrix_UB_31      0.0348124000
_diffrn_orient_matrix_UB_32      0.0986954000
_diffrn_orient_matrix_UB_33      0.0155119000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0460
_diffrn_reflns_av_unetI/netI     0.0203
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            21876
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.755
_diffrn_reflns_theta_min         4.924
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.302
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.67873
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.44a (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.430
_exptl_crystal_description       Plate
_exptl_crystal_F_000             1152
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Methanol'
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.789
_refine_diff_density_min         -0.711
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     178
_refine_ls_number_reflns         2691
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0396
_refine_ls_R_factor_gt           0.0379
_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^)+(0.0614P)^2^+1.8550P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1072
_refine_ls_wR_factor_ref         0.1089
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2545
_reflns_number_total             2691
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cp01064a2.cif
_cod_data_source_block           mc207
_cod_depositor_comments          'Adding full bibliography for 7230818.cif.'
_cod_database_code               7230818
_shelxl_version_number           2014/6
_chemical_oxdiff_formula         C14H13FN2OS
_chemical_oxdiff_usercomment     'FBTA ex MeOH'
_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.a Rotating group:
 N16(H16A,H16B)
2.b Aromatic/amide H refined with riding coordinates:
 C11(H11), C12(H12), C15(H15), C6(H6), C4(H4), C7(H7), C14(H14)
2.c Idealised Me refined as rotating group:
 C19(H19A,H19B,H19C)
;
_olex2_date_sample_data_collection 2017-11-08
_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 1.815
_oxdiff_exptl_absorpt_empirical_full_min 0.587