In situ modification of nanostructure configuration through the manipulation of hydrogen bonded amphiphile self-association.
Hiscock, Jennifer R.; Bustone, Gianluca P.; Wilson, Ben; Belsey, Kate E.; Blackholly, Laura R.; Soft matter 12 (2016) 4221–; doi:10.1039/c6sm00529b

data_1543057
_publ_section_title
;
 In situ modification of nanostructure configuration through the
 manipulation of hydrogen bonded amphiphile self-association.
;
_journal_issue                   18
_journal_name_full               'Soft matter'
_journal_page_first              4221
_journal_paper_doi               10.1039/c6sm00529b
_journal_volume                  12
_journal_year                    2016
_chemical_formula_moiety         'C8 H8 N3 O6 S, C16 H36 N'
_chemical_formula_sum            'C24 H44 N4 O6 S'
_chemical_formula_weight         516.69
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2016-02-16
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_cell_angle_alpha                90
_cell_angle_beta                 103.701(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   16.9274(4)
_cell_length_b                   16.3647(4)
_cell_length_c                   20.8867(6)
_cell_measurement_reflns_used    9775
_cell_measurement_temperature    150.01(10)
_cell_measurement_theta_max      73.3680
_cell_measurement_theta_min      5.9560
_cell_volume                     5621.2(3)
_computing_cell_refinement       'CrysAlisPro 1.171.38.37f (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.37f (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.37f (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    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2299
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

--------------------------------------------------------------------------
  1  \w    -92.00  -2.00   1.00   10.00    --  -38.50 125.00  60.00   90
  2  \w     18.00 112.00   1.00   10.00    --   43.14  57.00-150.00   94
  3  \w     82.00 174.00   1.00   40.00    --  104.54  45.00-150.00   92
  4  \w     35.00 127.00   1.00   40.00    --  104.54 -45.00  30.00   92
  5  \w     94.00 175.00   1.00   40.00    --  104.54 125.00  30.00   81
  6  \w     35.00 121.00   1.00   40.00    --  104.54-125.00 120.00   86
  7  \w     94.00 175.00   1.00   40.00    --  104.54 125.00 -60.00   81
  8  \w     18.00 112.00   1.00   10.00    --   43.14  57.00  90.00   94
  9  \w     18.00 112.00   1.00   10.00    --   43.14  57.00 -30.00   94
 10  \w     78.00 173.00   1.00   40.00    --  104.54  61.00 120.00   95
 11  \w     78.00 103.00   1.00   40.00    --  104.54  61.00   0.00   25
;
_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      -0.0206830000
_diffrn_orient_matrix_UB_12      -0.0828493000
_diffrn_orient_matrix_UB_13      0.0270422000
_diffrn_orient_matrix_UB_21      -0.0178360000
_diffrn_orient_matrix_UB_22      0.0434543000
_diffrn_orient_matrix_UB_23      0.0604833000
_diffrn_orient_matrix_UB_31      -0.0895935000
_diffrn_orient_matrix_UB_32      0.0104450000
_diffrn_orient_matrix_UB_33      -0.0371040000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_unetI/netI     0.0302
_diffrn_reflns_Laue_measured_fraction_full 0.979
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            13457
_diffrn_reflns_point_group_measured_fraction_full 0.979
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         67.076
_diffrn_reflns_theta_min         3.811
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.377
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.68019
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.37f (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.221
_exptl_crystal_description       plate
_exptl_crystal_F_000             2240
_exptl_crystal_size_max          0.162
_exptl_crystal_size_mid          0.129
_exptl_crystal_size_min          0.068
_refine_diff_density_max         0.291
_refine_diff_density_min         -0.278
_refine_diff_density_rms         0.044
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.967
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     808
_refine_ls_number_reflns         13457
_refine_ls_number_restraints     826
_refine_ls_restrained_S_all      0.961
_refine_ls_R_factor_all          0.0744
_refine_ls_R_factor_gt           0.0510
_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^)+(0.0917P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1338
_refine_ls_wR_factor_ref         0.1429
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9197
_reflns_number_total             13457
_reflns_threshold_expression     'I > 2\s(I)'
_twin_special_details
;
Component 2 rotated by -176.9790\% 
 around [-0.01 1.00 0.01] (reciprocal) or [-0.00 1.00 0.00] (direct)
;
_cod_data_source_file            c6sm00529b3.cif
_cod_data_source_block           jh1_twin1_hklf4
_cod_depositor_comments
'Adding full bibliography for 1543057--1543058.cif.'
_cod_database_code               1543057
_shelxl_version_number           2013-4
_chemical_oxdiff_formula         'C148 H264 N40 O56 S8 '
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.7982(17) 0.2018(17)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 C32-C31 = C27-C28 = C26-C27 = C31-C30 = C26-C25 = C30-C29 = C22-C21 = C18-C17
 = C22-C23 = C18-C19 = C20-C19 = C23-C24 = C48-C47 = C43-C44 = C46-C47 = C42-
 C43 = C46-C45 = C42-C41 = C38-C39 = C36-C35 = C40-C39 = C34-C35 = C34-C33 =
 C37-C38
 1.54 with sigma of 0.01
 N7-C25 \\sim N7-C29 \\sim N7-C37 \\sim N7-C33 \\sim N7-C17 \\sim N7-C21 \\sim
N7-C45 \\sim N7-C41
 with sigma of 0.01
4. Uiso/Uaniso restraints and constraints
N7 \\sim C33 \\sim C45 \\sim C29 \\sim C17 \\sim C37 \\sim C41 \\sim C25 \\sim
C21 \\sim C34 \\sim C46 \\sim C30 \\sim C18 \\sim C38 \\sim C42 \\sim C26 \\sim
C22 \\sim C35 \\sim C47 \\sim C31 \\sim C19 \\sim C39 \\sim C43 \\sim C27 \\sim
C23 \\sim C36 \\sim C48 \\sim C32 \\sim C20 \\sim C40 \\sim C44 \\sim C28 \\sim
C24: within 2A with sigma of 0.02 and sigma for terminal atoms of 0.04
Uanis(C27) = Uanis(C31)
5. Rigid body (RIGU) restrains
 C33, C45, C29, C17, C37, C41, C25, C21, C34, C46, C30, C18, C38, C42, C26,
 C22, C35, C47, C31, C19, C39, C43, C27, C23, C36, C48, C32, C20, C40, C44, C28,
  C24
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C21, N8, C63, C58, C49, C54, C64, C59, C50, C55, C65, C60, C51, C56, C66, C67,
  C62, C52, C53, C57
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C48, N7, C33, C45, C29, C17, C37, C41, C25, C21, C34, C46, C30, C18, C38, C42,
  C26, C22, C35, C47, C31, C19, C39, C43, C27, C23, C36, C32, C20, C40, C44,
 C28, C24
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Sof(H60A)=Sof(H60B)=Sof(C62)=Sof(H62D)=Sof(H62E)=Sof(H62F)=1-FVAR(1)
 Sof(H61A)=Sof(H61B)=Sof(C61)=Sof(H62A)=Sof(H62B)=Sof(H62C)=FVAR(1)
 Sof(H51C)=Sof(H51D)=Sof(C53)=Sof(H53A)=Sof(H53B)=Sof(H53C)=1-FVAR(2)
 Sof(H51A)=Sof(H51B)=Sof(C52)=Sof(H52A)=Sof(H52B)=Sof(H52C)=FVAR(2)
 Sof(H65A)=Sof(H65B)=Sof(C66)=Sof(H66C)=Sof(H66D)=Sof(H66E)=1-FVAR(3)
 Sof(H66A)=Sof(H66B)=Sof(C67)=Sof(H68A)=Sof(H68B)=Sof(H68C)=FVAR(3)
 Fixed Sof: C47(0.75) H47A(0.75) H47B(0.75) C33(0.75) H33A(0.75) H33B(0.75)
 C45(0.75) H45A(0.75) H45B(0.75) C35(0.75) H35A(0.75) H35B(0.75) C29(0.75)
 H29A(0.75) H29B(0.75) C30(0.75) H30A(0.75) H30B(0.75) C17(0.75) H17A(0.75)
 H17B(0.75) C19(0.75) H19A(0.75) H19B(0.75) C31(0.75) H31A(0.75) H31B(0.75)
 C46(0.75) H46A(0.75) H46B(0.75) C20(0.75) H20A(0.75) H20B(0.75) H20C(0.75)
 C34(0.75) H34A(0.75) H34B(0.75) C36(0.75) H36A(0.75) H36B(0.75) H36C(0.75)
 C48(0.75) H48A(0.75) H48B(0.75) H48C(0.75) C32(0.75) H32A(0.75) H32B(0.75)
 H32C(0.75) C18(0.75) H18A(0.75) H18B(0.75) C38(0.25) H38A(0.25) H38B(0.25)
 C37(0.25) H37A(0.25) H37B(0.25) C41(0.25) H41A(0.25) H41B(0.25) C42(0.25)
 H42A(0.25) H42B(0.25) C25(0.25) H25A(0.25) H25B(0.25) C26(0.25) H26A(0.25)
 H26B(0.25) C22(0.25) H22A(0.25) H22B(0.25) C21(0.25) H21A(0.25) H21B(0.25)
 C40(0.25) H40A(0.25) H40B(0.25) H40C(0.25) C39(0.25) H39A(0.25) H39B(0.25)
 C24(0.25) H24A(0.25) H24B(0.25) H24C(0.25) C23(0.25) H23A(0.25) H23B(0.25)
 C28(0.25) H28A(0.25) H28B(0.25) H28C(0.25) C27(0.25) H27A(0.25) H27B(0.25)
 C44(0.25) H44A(0.25) H44B(0.25) H44C(0.25) C43(0.25) H43A(0.25) H43B(0.25)
7.a Secondary CH2 refined with riding coordinates:
 C63(H63A,H63B), C58(H58A,H58B), C16(H16A,H16B), C55(H55A,H55B), C64(H64A,
 H64B), C8(H8A,H8B), C49(H49A,H49B), C47(H47A,H47B), C33(H33A,H33B), C59(H59A,
 H59B), C56(H56A,H56B), C45(H45A,H45B), C35(H35A,H35B), C29(H29A,H29B),
 C30(H30A,H30B), C17(H17A,H17B), C65(H65A,H65B), C65(H66A,H66B), C50(H50A,H50B),
  C54(H54A,H54B), C19(H19A,H19B), C31(H31A,H31B), C46(H46A,H46B), C60(H61A,
 H61B), C60(H60A,H60B), C34(H34A,H34B), C51(H51A,H51B), C51(H51C,H51D),
 C18(H18A,H18B), C38(H38A,H38B), C37(H37A,H37B), C41(H41A,H41B), C42(H42A,H42B),
  C25(H25A,H25B), C26(H26A,H26B), C22(H22A,H22B), C21(H21A,H21B), C39(H39A,
 H39B), C23(H23A,H23B), C27(H27A,H27B), C43(H43A,H43B)
7.b Me refined with riding coordinates:
 C57(H57A,H57B,H57C), C66(H66C,H66D,H66E), C52(H52A,H52B,H52C), C61(H62A,H62B,
 H62C), C62(H62D,H62E,H62F), C53(H53A,H53B,H53C), C67(H68A,H68B,H68C)
7.c Aromatic/amide H refined with riding coordinates:
 N6(H6A), N5(H5A), N3(H3), N2(H2), C10(H10), C11(H11), C6(H6), C14(H14),
 C5(H5), C13(H13), C2(H2A), C3(H3A)
7.d Idealised Me refined as rotating group:
 C20(H20A,H20B,H20C), C36(H36A,H36B,H36C), C48(H48A,H48B,H48C), C32(H32A,H32B,
 H32C), C40(H40A,H40B,H40C), C24(H24A,H24B,H24C), C28(H28A,H28B,H28C), C44(H44A,
 H44B,H44C)
;
_shelx_res_checksum              62951
_shelx_hkl_checksum              73040
_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 2.070
_oxdiff_exptl_absorpt_empirical_full_min 0.659
_oxdiff_twin_integration_method  simultaneous
_oxdiff_twin_items               2