Competing forces in the self-assembly of amide-functionalized discotic mesogens
Yoshida, Jun; Bozek, Kevin J. A.; Thompson, John R.; Williams, Vance E.; Soft Matter  (2019) –; doi:10.1039/C9SM01435G

data_1556416
_publ_section_title
;
 Competing forces in the self-assembly of amide-functionalized discotic
 mesogens
;
_journal_name_full               'Soft Matter'
_journal_paper_doi               10.1039/C9SM01435G
_journal_year                    2019
_chemical_formula_moiety         'C49 H69 N3 O5'
_chemical_formula_sum            'C49 H69 N3 O5'
_chemical_formula_weight         780.07
_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     dual
_audit_creation_date             2019-07-16
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-07-16 deposited with the CCDC.	2019-11-25 downloaded from the CCDC.
;
_cell_angle_alpha                108.5467(18)
_cell_angle_beta                 98.9702(17)
_cell_angle_gamma                95.1342(17)
_cell_formula_units_Z            2
_cell_length_a                   11.0971(2)
_cell_length_b                   12.3679(3)
_cell_length_c                   17.5421(3)
_cell_measurement_reflns_used    6451
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      73.3870
_cell_measurement_theta_min      3.8160
_cell_volume                     2229.65(8)
_computing_cell_refinement       'CrysAlisPro 1.171.39.45i (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.45i (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.45i (Rigaku OD, 2018)'
_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_temperature      173
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.947
_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    -63.00  36.00   0.50   12.00    --  -39.20  57.00 -90.00  198
  2  \w    -43.00 -17.00   0.50   27.00    --  -94.50 125.00  90.00   52
  3  \w    -32.00  -5.00   0.50   12.00    --  -39.20 109.00 159.00   54
  4  \w    -71.00  41.00   0.50   12.00    --  -39.20  37.00  30.00  224
  5  \w    -44.00 -14.00   0.50   27.00    --  -94.50  30.00 150.00   60
  6  \w    -66.00 -17.00   0.50   27.00    --  -94.50  45.00 120.00   98
  7  \w    -73.00 -48.00   0.50   27.00    --  -94.50 109.00 159.00   50
  8  \w    -90.00 -64.00   0.50   27.00    --  -94.50 125.00  90.00   52
  9  \w    -69.00 -12.00   0.50   27.00    --  -94.50  30.00   0.00  114
 10  \w    -62.00 -19.00   0.50   27.00    --  -94.50  30.00-150.00   86
 11  \w   -126.00-100.00   0.50   27.00    --  -94.50-109.00  62.00   52
 12  \w   -114.00 -71.00   0.50   12.00    --  -39.20-125.00   0.00   86
 13  \w   -117.00 -92.00   0.50   12.00    --  -39.20-125.00 -30.00   50
 14  \w   -115.00 -70.00   0.50   12.00    --  -39.20-125.00-120.00   90
 15  \w   -106.00 -80.00   0.50   12.00    --  -39.20-125.00-150.00   52
 16  \w      1.00  26.00   0.50   12.00    --   39.20 -99.00  30.00   50
 17  \w     37.00  75.00   0.50   12.00    --   39.20-109.00  62.00   76
 18  \w     80.00 111.00   0.50   27.00    --  109.49-109.00  62.00   62
 19  \w     64.00  90.00   0.50   27.00    --  109.49 -94.00 150.00   52
 20  \w     47.00  85.00   0.50   27.00    --  109.49-125.00 150.00   76
 21  \w     31.00  77.00   0.50   27.00    --  109.49 -45.00 150.00   92
 22  \w     34.00  60.00   0.50   27.00    --  109.49 -30.00  90.00   52
 23  \w     31.00  75.00   0.50   27.00    --  109.49 -45.00  60.00   88
 24  \w     28.00  66.00   0.50   27.00    --  109.49 -30.00   0.00   76
 25  \w     34.00  69.00   0.50   27.00    --  109.49 -30.00 -60.00   70
 26  \w     27.00  68.00   0.50   27.00    --  109.49 -30.00 -90.00   82
 27  \w     37.00  62.00   0.50   27.00    --  109.49 -61.00-150.00   50
 28  \w     50.00  75.00   0.50   27.00    --  109.49 -45.00-150.00   50
 29  \w    107.00 133.00   0.50   27.00    --  109.49 -61.00-150.00   52
 30  \w     81.00 117.00   0.50   27.00    --  109.49-125.00-150.00   72
 31  \w     77.00 113.00   0.50   27.00    --  109.49-125.00 -90.00   72
 32  \w     81.00 117.00   0.50   27.00    --  109.49-125.00 -60.00   72
 33  \w     47.00  79.00   0.50   27.00    --  109.49 -94.00 -30.00   64
 34  \w     40.00  66.00   0.50   27.00    --  109.49-125.00 -90.00   52
 35  \w     34.00  59.00   0.50   27.00    --  109.49-125.00-150.00   50
 36  \w     34.00  99.00   0.50   12.00    --   39.20-125.00-120.00  130
 37  \w     32.00  67.00   0.50   27.00    --  109.49 -30.00-150.00   70
 38  \w     28.00  67.00   0.50   27.00    --  109.49 -30.00-180.00   78
 39  \w     94.00 177.00   0.50   27.00    --  109.49 125.00  60.00  166
 40  \w    145.00 177.00   0.50   27.00    --  109.49 109.00 159.00   64
 41  \w    101.00 134.00   0.50   27.00    --  109.49 109.00 159.00   66
 42  \w     82.00 178.00   0.50   27.00    --  109.49  45.00  60.00  192
 43  \w    149.00 175.00   0.50   27.00    --  109.49 125.00-150.00   52
 44  \w     94.00 131.00   0.50   27.00    --  109.49 125.00-150.00   74
 45  \w     27.00  60.00   0.50   27.00    --  109.49 -30.00 120.00   66
 46  \w     27.00  53.00   0.50   27.00    --  109.49 -30.00 150.00   52
 47  \w     34.00  60.00   0.50   27.00    --  109.49 -94.00 150.00   52
 48  \w     32.00 109.00   0.50   27.00    --  109.49-125.00  60.00  154
 49  \w   -115.00 -70.00   0.50   12.00    --  -39.20-125.00  90.00   90
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0566759000
_diffrn_orient_matrix_UB_12      -0.0905214000
_diffrn_orient_matrix_UB_13      0.0327076000
_diffrn_orient_matrix_UB_21      -0.0203549000
_diffrn_orient_matrix_UB_22      -0.0916356000
_diffrn_orient_matrix_UB_23      -0.0860430000
_diffrn_orient_matrix_UB_31      0.1287316000
_diffrn_orient_matrix_UB_32      -0.0325583000
_diffrn_orient_matrix_UB_33      0.0211563000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0347
_diffrn_reflns_av_unetI/netI     0.0440
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.947
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            22133
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.947
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.741
_diffrn_reflns_theta_min         2.709
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.582
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.85533
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.45i (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_density_diffrn    1.162
_exptl_crystal_description       needle
_exptl_crystal_F_000             848
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.717
_refine_diff_density_min         -0.323
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     520
_refine_ls_number_reflns         8667
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0918
_refine_ls_R_factor_gt           0.0699
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0997P)^2^+1.4568P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1888
_refine_ls_wR_factor_ref         0.2062
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6607
_reflns_number_total             8667
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9sm01435g2.cif
_cod_data_source_block           exp_65
_cod_original_cell_volume        2229.66(8)
_cod_database_code               1556416
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         'C38 H34 O4 N2'
_chemical_oxdiff_usercomment     JY25
_shelx_estimated_absorpt_t_max   0.971
_shelx_estimated_absorpt_t_min   0.845
_reflns_odcompleteness_completeness 98.56
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C27(H27A,H27B), C28(H28A,H28B), C29(H29A,H29B), C38(H38A,H38B), C45(H45A,
 H45B), C46(H46A,H46B), C20(H20A,H20B), C30(H30A,H30B), C47(H47A,H47B),
 C55(H55A,H55B), C39(H39A,H39B), C53(H53A,H53B), C40(H40A,H40B), C48(H48A,H48B),
  C31(H31A,H31B), C49(H49A,H49B), C21(H21A,H21B), C41(H41A,H41B), C22(H22A,
 H22B), C42(H42A,H42B), C0AA(H0AA,H0AB), C1AA(H1AA,H1AB)
2.b Aromatic/amide H refined with riding coordinates:
 C33(H33), C6(H6), C18(H18), C36(H36), C8(H8), C9(H9), C15(H15)
2.c Idealised Me refined as rotating group:
 C56(H56A,H56B,H56C), C54(H54A,H54B,H54C), C32(H32A,H32B,H32C), C50(H50A,H50B,
 H50C), C43(H43A,H43B,H43C), C2AA(H2AA,H2AB,H2AC)
;
_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 1.723
_oxdiff_exptl_absorpt_empirical_full_min 0.693