Bis-pyrene probes of foldamer conformation in solution and in phospholipid bilayers.
Lister, Francis G. A.; Eccles, Natasha; Pike, Sarah J.; Brown, Robert A.; Whitehead, George F. S.; Raftery, James; Webb, Simon J.; Clayden, Jonathan; Chemical science 9 (2018) 6860–6870; doi:10.1039/c8sc02532k

data_1549683
_publ_section_title
;
 Bis-pyrene probes of foldamer conformation in solution and in
 phospholipid bilayers.
;
_journal_issue                   33
_journal_name_full               'Chemical science'
_journal_page_first              6860
_journal_page_last               6870
_journal_paper_doi               10.1039/c8sc02532k
_journal_volume                  9
_journal_year                    2018
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C H Cl3, C52 H52 N8 O5'
_chemical_formula_sum            'C53 H53 Cl3 N8 O5'
_chemical_formula_weight         988.38
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2018-02-05
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2018-05-16 deposited with the CCDC.
2018-07-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.161(7)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.7198(6)
_cell_length_b                   18.6592(11)
_cell_length_c                   14.0802(12)
_cell_measurement_reflns_used    3793
_cell_measurement_temperature    149.99(10)
_cell_measurement_theta_max      65.7350
_cell_measurement_theta_min      3.1390
_cell_volume                     2553.6(3)
_computing_cell_refinement       'CrysAlisPro 1.171.39.30c (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.30c (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.30c (Rigaku OD, 2017)'
_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      149.99(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.995
_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    -25.00   2.00   1.00    2.00    --    5.00  57.00-180.00   27
  2  \w      4.00  32.00   1.00    2.00    --  -45.10  57.00 -30.00   28
  3  \w   -125.00 -12.00   1.00    2.00    --  -45.10 -57.00 -60.00  113
  4  \w   -131.00  -8.00   1.00    2.00    --  -45.10 -44.00  34.22  123
  5  \w   -116.00 -15.00   1.00    2.00    --  -45.10 -57.00 120.00  101
  6  \w   -134.00  -6.00   1.00    2.00    --  -45.10 -73.00 -83.03  128
  7  \w   -103.00 -75.00   1.00    8.00    -- -110.00 -76.00 -30.00   28
  8  \w   -197.00 -76.00   1.00    8.00    -- -110.00 -38.00 120.00  121
  9  \w   -193.00 -70.00   1.00    8.00    -- -110.00 -76.00-180.00  123
 10  \w   -105.00 -78.00   1.00    8.00    -- -110.00 -57.00 -30.00   27
 11  \w   -106.00 -79.00   1.00    8.00    -- -110.00  57.00  30.00   27
 12  \w   -149.00 -21.00   1.00    8.00    -- -110.00  76.00 -30.00  128
 13  \w   -194.00-106.00   1.00    8.00    -- -110.00 -57.00-120.00   88
 14  \w   -113.00 -88.00   1.00    8.00    -- -110.00  57.00  60.00   25
 15  \w   -193.00-166.00   1.00    8.00    -- -110.00 -57.00 -30.00   27
 16  \w   -192.00 -72.00   1.00    8.00    -- -110.00 -76.00 -60.00  120
 17  \w   -128.00-101.00   1.00    8.00    -- -110.00 -19.00-150.00   27
 18  \w   -189.00-160.00   1.00    8.00    -- -110.00 -19.00-150.00   29
 19  \w    -64.00 -22.00   1.00    8.00    -- -110.00 -19.00-150.00   42
 20  \w   -159.00 -78.00   1.00    8.00    -- -110.00 -57.00-150.00   81
 21  \w   -181.00-122.00   1.00    8.00    -- -110.00 -38.00 -30.00   59
 22  \w   -111.00 -70.00   1.00    8.00    -- -110.00 -38.00 -30.00   41
 23  \w   -179.00 -84.00   1.00    8.00    -- -110.00 -38.00  90.00   95
 24  \w    -54.00 -25.00   1.00    8.00    -- -110.00 -19.00  60.00   29
 25  \w   -141.00 -92.00   1.00    8.00    -- -110.00  57.00  90.00   49
 26  \w    -69.00 -44.00   1.00    8.00    -- -110.00  57.00  90.00   25
 27  \w    -65.00 -21.00   1.00    8.00    -- -110.00  57.00  60.00   44
 28  \w   -111.00 -86.00   1.00    8.00    -- -110.00  38.00-150.00   25
 29  \w    -74.00 -30.00   1.00    8.00    -- -110.00  38.00-150.00   44
 30  \w   -108.00 -72.00   1.00    8.00    -- -110.00 -38.00 -60.00   36
 31  \w    -92.00 -65.00   1.00    8.00    -- -110.00  38.00 -90.00   27
 32  \w   -139.00-114.00   1.00    8.00    -- -110.00  38.00 -90.00   25
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC11 (RINC): Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0363817000
_diffrn_orient_matrix_UB_12      0.0492316000
_diffrn_orient_matrix_UB_13      0.0842207000
_diffrn_orient_matrix_UB_21      -0.0802517000
_diffrn_orient_matrix_UB_22      -0.0497034000
_diffrn_orient_matrix_UB_23      0.0674181000
_diffrn_orient_matrix_UB_31      0.1318017000
_diffrn_orient_matrix_UB_32      -0.0438448000
_diffrn_orient_matrix_UB_33      0.0180743000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0636
_diffrn_reflns_av_unetI/netI     0.0642
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            30504
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.499
_diffrn_reflns_theta_min         3.139
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.069
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.43306
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.30c (Rigaku Oxford Diffraction, 2017)
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    1.285
_exptl_crystal_description       block
_exptl_crystal_F_000             1036
_exptl_crystal_size_max          0.213
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.031
_refine_diff_density_max         0.308
_refine_diff_density_min         -0.444
_refine_diff_density_rms         0.046
_refine_ls_abs_structure_details
;
 Flack x determined using 2544 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.019(14)
_refine_ls_extinction_coef       0.0023(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2017/1 (Sheldrick 2017)'
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     654
_refine_ls_number_reflns         10270
_refine_ls_number_restraints     76
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0884
_refine_ls_R_factor_gt           0.0614
_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^)+(0.0934P)^2^+0.0168P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1542
_refine_ls_wR_factor_ref         0.1719
_reflns_Friedel_coverage         0.913
_reflns_Friedel_fraction_full    0.995
_reflns_Friedel_fraction_max     0.970
_reflns_number_gt                7244
_reflns_number_total             10270
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8sc02532k2.cif
_cod_data_source_block           s5108r
_cod_depositor_comments
'Adding full bibliography for 1549682--1549686.cif.'
_cod_database_code               1549683
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.939
_shelx_estimated_absorpt_t_min   0.667
_reflns_odcompleteness_completeness 99.98
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     68.13
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
C1 \\sim Cl4 \\sim Cl1 \\sim Cl2 \\sim Cl3 \\sim Cl5: within 2A with sigma of
0.04 and sigma for terminal atoms of 0.08
3. Rigid body (RIGU) restrains
 C1, Cl4, Cl1, Cl2, Cl3, Cl5
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(Cl1)=Sof(Cl2)=Sof(H1B)=1-FVAR(1)
 Sof(Cl3)=Sof(Cl5)=Sof(H1A)=FVAR(1)
5.a Riding coordinates:
 N4(H4), N3(H3), N2(H2), N1(H1), N5(H5)
5.b Ternary CH refined with riding coordinates:
 C9(H9), C10(H10), C1(H1B)
5.c Aromatic/amide H refined with riding coordinates:
 C42(H42), C43(H43), C44(H44), C36(H36), C35(H35), C33(H33), C34(H34),
 C41(H41), C40(H40), C18(H18), C17(H17), C19(H19), C20(H20), C28(H28), C27(H27),
  C26(H26), C24(H24), C25(H25)
5.d Idealised Me refined as rotating group:
 C52(H52A,H52B,H52C), C53(H53A,H53B,H53C), C49(H49A,H49B,H49C), C50(H50A,H50B,
 H50C), C47(H47A,H47B,H47C), C48(H48A,H48B,H48C), C12(H12A,H12B,H12C), C45(H45A,
 H45B,H45C), C46(H46A,H46B,H46C)
;
_shelx_res_checksum              66531
_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 2.140
_oxdiff_exptl_absorpt_empirical_full_min 0.568