Azaylide-based gemini amphiphiles displaying unique self-assembling behavior <i>via</i> an even-odd effect of alkyl linker chain length.
Akiyama, Yoshimori; Yamashina, Masahiro; Toyota, Shinji; Soft matter 20 (2024) 6539–6543; doi:10.1039/d4sm00789a

data_1572248
_publ_section_title
;
 Azaylide-based gemini amphiphiles displaying unique self-assembling
 behavior <i>via</i> an even-odd effect of alkyl linker chain length.
;
_journal_issue                   33
_journal_name_full               'Soft matter'
_journal_page_first              6539
_journal_page_last               6543
_journal_paper_doi               10.1039/d4sm00789a
_journal_volume                  20
_journal_year                    2024
_chemical_formula_moiety         'C50 H54 Cl4 N4 O4 P2, 2(Cl)'
_chemical_formula_sum            'C50 H54 Cl6 N4 O4 P2'
_chemical_formula_weight         1049.61
_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             2023-12-01
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2024-03-24 deposited with the CCDC.	2024-07-30 downloaded from the CCDC.
;
_cell_angle_alpha                78.146(5)
_cell_angle_beta                 78.602(4)
_cell_angle_gamma                81.396(4)
_cell_formula_units_Z            2
_cell_length_a                   9.4418(3)
_cell_length_b                   17.2643(12)
_cell_length_c                   17.5420(10)
_cell_measurement_reflns_used    5451
_cell_measurement_temperature    123
_cell_measurement_theta_max      70.5530
_cell_measurement_theta_min      2.6270
_cell_volume                     2725.5(3)
_computing_cell_refinement       'CrysAlisPro 1.171.43.95a (Rigaku OD, 2023)'
_computing_data_collection
'CrysAlisPro system (CCD 43.95a 64-bit (release 03-11-2023))'
_computing_data_reduction        'CrysAlisPro 1.171.43.95a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2016/6 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      123
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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    -80.00  -2.00   0.50    7.70    --  -38.95 109.00-157.00  156
  2  \w     24.00  77.00   0.50    7.70    --   38.95-109.00 105.00  106
  3  \w   -120.00 -83.00   0.50   25.40    -- -102.00-109.00 105.00   74
  4  \w   -108.00 -60.00   0.50   25.40    -- -102.00 109.00-157.00   96
  5  \w     96.00 128.00   0.50   25.40    --  107.86 109.00-157.00   64
  6  \w     30.00 107.00   0.50   25.40    --  107.86-109.00 105.00  154
  7  \w   -115.00 -83.00   0.50    7.70    --  -38.95-178.00  60.00   64
  8  \w    -79.00 -42.00   0.50    7.70    --  -38.95-178.00  60.00   74
  9  \w      4.00  42.00   0.50    7.70    --  -38.95  19.00 -60.00   76
 10  \w    -33.00  41.00   0.50    7.70    --  -38.95  37.00   0.00  148
 11  \w    -30.00  11.00   0.50    7.70    --   38.95 -19.00 -60.00   82
 12  \w     96.00 121.00   0.50    7.70    --   38.95 178.00-120.00   50
 13  \w    -45.00 -19.00   0.50    7.70    --   38.95 -19.00   0.00   52
 14  \w      7.00 120.00   0.50    7.70    --   38.95  37.00 -90.00  226
 15  \w    -45.00   8.00   0.50    7.70    --   38.95 -19.00  30.00  106
 16  \w   -105.00 -76.00   0.50   25.40    -- -102.00 125.00 120.00   58
 17  \w   -171.00-141.00   0.50   25.40    -- -102.00 -77.00 150.00   60
 18  \w   -174.00 -68.00   0.50   25.40    -- -102.00 -77.00 120.00  212
 19  \w   -135.00 -69.00   0.50   25.40    -- -102.00 -77.00 150.00  132
 20  \w    -70.00 -44.00   0.50   25.40    -- -102.00  61.00  30.00   52
 21  \w    -89.00 -27.00   0.50   25.40    -- -102.00 125.00   0.00  124
 22  \w   -102.00 -75.00   0.50   25.40    -- -102.00 -30.00  60.00   54
 23  \w    -61.00 -26.00   0.50   25.40    -- -102.00 147.00  98.53   70
 24  \w   -120.00 -93.00   0.50   25.40    -- -102.00 137.00  69.31   54
 25  \w   -128.00 -91.00   0.50   25.40    -- -102.00 147.00  98.53   74
 26  \w   -159.00 -73.00   0.50   25.40    -- -102.00 -45.00   0.00  172
 27  \w    -61.00 -28.00   0.50   25.40    -- -102.00 125.00 120.00   66
 28  \w    -73.00 -30.00   0.50   25.40    -- -102.00  61.00   0.00   86
 29  \w   -170.00-126.00   0.50   25.40    -- -102.00 -30.00  60.00   88
 30  \w     40.00 105.00   0.50   25.40    --  107.86 -94.00  30.00  130
 31  \w     32.00  58.00   0.50   25.40    --  107.86-125.00   0.00   52
 32  \w     37.00  78.00   0.50   25.40    --  107.86 -61.00-180.00   82
 33  \w     74.00 178.00   0.50   25.40    --  107.86  77.00 -90.00  208
 34  \w     40.00  74.00   0.50   25.40    --  107.86 -61.00  90.00   68
 35  \w     37.00 101.00   0.50   25.40    --  107.86 -94.00 -30.00  128
 36  \w    141.00 166.00   0.50   25.40    --  107.86  61.00-180.00   50
 37  \w    116.00 177.00   0.50   25.40    --  107.86  45.00   0.00  122
 38  \w     80.00 133.00   0.50   25.40    --  107.86  61.00-180.00  106
 39  \w     36.00 105.00   0.50   25.40    --  107.86 -94.00-120.00  138
 40  \w     33.00  58.00   0.50   25.40    --  107.86 -61.00  60.00   50
 41  \w     68.00 107.00   0.50   25.40    --  107.86-125.00   0.00   78
 42  \w     38.00  67.00   0.50   25.40    --  107.86 -61.00 150.00   58
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0183328000
_diffrn_orient_matrix_UB_12      0.0533687000
_diffrn_orient_matrix_UB_13      -0.0801809000
_diffrn_orient_matrix_UB_21      -0.0193929000
_diffrn_orient_matrix_UB_22      0.0745469000
_diffrn_orient_matrix_UB_23      0.0381714000
_diffrn_orient_matrix_UB_31      0.1653919000
_diffrn_orient_matrix_UB_32      0.0040945000
_diffrn_orient_matrix_UB_33      -0.0203268000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0974
_diffrn_reflns_av_unetI/netI     0.0964
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            27888
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        67.075
_diffrn_reflns_theta_max         67.075
_diffrn_reflns_theta_min         2.613
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.789
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.84686
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.95a (Rigaku Oxford Diffraction, 2023)
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    1.279
_exptl_crystal_description       plate
_exptl_crystal_F_000             1092
_exptl_crystal_size_max          0.251
_exptl_crystal_size_mid          0.133
_exptl_crystal_size_min          0.082
_refine_diff_density_max         0.855
_refine_diff_density_min         -0.787
_refine_diff_density_rms         0.136
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     601
_refine_ls_number_reflns         9693
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.1725
_refine_ls_R_factor_gt           0.1280
_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^)+(0.1707P)^2^+26.6498P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3646
_refine_ls_wR_factor_ref         0.3917
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5909
_reflns_number_total             9693
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sm00789a2.cif
_cod_data_source_block           NdpP2
_cod_depositor_comments
'Adding full bibliography for 1572247--1572248.cif.'
_cod_database_code               1572248
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'C11 H10 N O'
_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:
 C00S(H00A,H00B), C011(H01A,H01B), C01A(H01C,H01D), C01C(H01F,H01G), C01F(H01J,
 H01K), C01P(H01T,H01U)
2.b Aromatic/amide H refined with riding coordinates:
 C00F(H00F), C00H(H00H), C00P(H00P), C00X(H00X), C012(H012), C013(H013),
 C014(H014), C015(H015), C016(H016), C017(H017), C018(H018), C019(H019),
 C01B(H01E), C01D(H01H), C01E(H01I), C01G(H01L), C01H(H01M), C01J(H01N),
 C01K(H01O), C01L(H01P), C01M(H01Q), C01N(H01R), C01O(H01S), C01Q(H01V)
2.c Idealised Me refined as rotating group:
 C01R(H01W,H01X,H01Y), C01S(H01Z,H,HA), C01T(H01,HB,HC), C01U(H1,HD,HE),
 C01V(H2,HF,HG), C01W(H3,HH,HI)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              34165
_shelx_hkl_checksum              75839
_shelx_fab_checksum              82168
_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 2.174
_oxdiff_exptl_absorpt_empirical_full_min 0.543