‘Frustrated’ hydrogen bond mediated amphiphile self-assembly – a solid state study
Blackholly, Laura R.; Shepherd, Helena J.; Hiscock, Jennifer R.; CrystEngComm 18 (2016) 7021–; doi:10.1039/C6CE01493C

data_7226475
_publ_section_title
;
 &#x2018;Frustrated&#x2019; hydrogen bond mediated amphiphile
 self-assembly -- a solid state study
;
_journal_issue                   37
_journal_name_full               CrystEngComm
_journal_page_first              7021
_journal_paper_doi               10.1039/C6CE01493C
_journal_volume                  18
_journal_year                    2016
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C9 H10 F3 N2 Na O5 S'
_chemical_formula_sum            'C9 H10 F3 N2 Na O5 S'
_chemical_formula_weight         338.24
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2016-05-31
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2016-07-04 deposited with the CCDC.
2016-08-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   4.8741(3)
_cell_length_b                   6.3672(4)
_cell_length_c                   40.456(3)
_cell_measurement_reflns_used    5289
_cell_measurement_temperature    100(1)
_cell_measurement_theta_max      72.8710
_cell_measurement_theta_min      4.3580
_cell_volume                     1255.53(14)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2887
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  1  \w     23.00  49.00   1.00    1.00    --   40.62  77.00 -30.00   26
  2  \w     59.00 151.00   1.00    1.00    --  105.19  15.00 -30.00   92
  3  \w    103.00 163.00   1.00    1.00    --  105.19 111.00   0.00   60
  4  \w     79.00 143.00   1.00    1.00    --  105.19  45.00  90.00   64
  5  \w     59.00  86.00   1.00    1.00    --  105.19 178.00 -90.00   27
  6  \w    -62.00  30.00   1.00    1.00    --  -40.62  77.00 120.00   92
  7  \w     43.00 126.00   1.00    1.00    --  105.19 -30.00 -90.00   83
  8  \w     83.00 108.00   1.00    1.00    --  105.19 -94.00  30.00   25
  9  \w     87.00 116.00   1.00    1.00    --  105.19-111.00 150.00   29
 10  \w     45.00 131.00   1.00    1.00    --  105.19 -45.00  90.00   86
 11  \w     57.00  88.00   1.00    1.00    --   40.62-125.00 -30.00   31
 12  \w     37.00 101.00   1.00    1.00    --  105.19-111.00 -60.00   64
 13  \w     29.00 137.00   1.00    1.00    --  105.19 -77.00 -60.00  108
 14  \w     33.00  77.00   1.00    1.00    --  105.19 -94.00 120.00   44
 15  \w     31.00  56.00   1.00    1.00    --  105.19-111.00 150.00   25
 16  \w      1.00  78.00   1.00    1.00    --   40.62 -99.00-120.00   77
 17  \w   -112.00 -18.00   1.00    1.00    --  -40.62 -38.00 -30.00   94
 18  \w   -114.00 -87.00   1.00    1.00    --  -40.62 -57.00  90.00   27
;
_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      0.1493123000
_diffrn_orient_matrix_UB_12      0.1008511000
_diffrn_orient_matrix_UB_13      -0.0295605000
_diffrn_orient_matrix_UB_21      0.0840070000
_diffrn_orient_matrix_UB_22      -0.2197321000
_diffrn_orient_matrix_UB_23      -0.0123545000
_diffrn_orient_matrix_UB_31      -0.2653800000
_diffrn_orient_matrix_UB_32      -0.0127913000
_diffrn_orient_matrix_UB_33      -0.0205829000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0288
_diffrn_reflns_av_unetI/netI     0.0262
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       4
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       47
_diffrn_reflns_limit_l_min       -49
_diffrn_reflns_number            7871
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.848
_diffrn_reflns_theta_min         2.184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.277
_exptl_absorpt_correction_T_max  0.811
_exptl_absorpt_correction_T_min  0.433
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (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_density_diffrn    1.789
_exptl_crystal_description       block
_exptl_crystal_F_000             688
_exptl_crystal_size_max          0.596
_exptl_crystal_size_mid          0.103
_exptl_crystal_size_min          0.087
_refine_diff_density_max         0.309
_refine_diff_density_min         -0.396
_refine_diff_density_rms         0.058
_refine_ls_abs_structure_details
;
 Refined as an inversion twin; batch scale factor refined to 0.34(2)
;
_refine_ls_abs_structure_Flack   0.34(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     192
_refine_ls_number_reflns         2439
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0288
_refine_ls_R_factor_gt           0.0279
_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^)+(0.0406P)^2^+0.3662P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0697
_refine_ls_wR_factor_ref         0.0701
_reflns_Friedel_coverage         0.641
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.995
_reflns_number_gt                2402
_reflns_number_total             2439
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6ce01493c2.cif
_cod_data_source_block           Compound_9
_cod_depositor_comments
'Adding full bibliography for 7226468--7226476.cif.'
_cod_original_cell_volume        1255.54(14)
_cod_database_code               7226475
_shelxl_version_number           2013-4
_chemical_oxdiff_formula         'C8 H9 N2 O5 F3 S Na'
_reflns_odcompleteness_completeness 99.93
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H5A(0.033) H5B(0.033) H2(0.016) H1(0.019) H3(0.019) H4(0.018)
 H9A(0.015) H9B(0.015) H6(0.019) H7(0.019)
 Fixed X: H5A(1.1291) H5B(1.0725) H2(0.8152) H1(0.7682) H3(-0.036) H4(0.1578)
 H9A(0.6281) H9B(0.348) H6(0.7101) H7(0.5178)
 Fixed Y: H5A(0.6326) H5B(0.4205) H2(0.1372) H1(0.4059) H3(0.9127) H4(0.6376)
 H9A(-0.1747) H9B(-0.0574) H6(0.5517) H7(0.8277)
 Fixed Z: H5A(0.4452) H5B(0.4347) H2(0.391) H1(0.3598) H3(0.3466) H4(0.3761)
 H9A(0.4076) H9B(0.4122) H6(0.3032) H7(0.2742)
;
_shelx_res_checksum              10881
_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 1.415
_oxdiff_exptl_absorpt_empirical_full_min 0.429