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_1549682
_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         'C69 H69 N7 O8, 3(C H Cl3)'
_chemical_formula_sum            'C72 H72 Cl9 N7 O8'
_chemical_formula_weight         1482.41
_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   geom
_audit_creation_date             2018-05-04
_audit_creation_method
;
Olex2 1.2
(compiled 2018.04.26 svn.r3504 for OlexSys, GUI svn.r5492)
;
_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
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.2969(4)
_cell_length_b                   22.3943(5)
_cell_length_c                   25.1034(6)
_cell_measurement_reflns_used    9868
_cell_measurement_temperature    100.15
_cell_measurement_theta_max      70.15
_cell_measurement_theta_min      3.87
_cell_volume                     7475.2(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_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    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.15
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0414
_diffrn_reflns_av_unetI/netI     0.0542
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            35359
_diffrn_reflns_point_group_measured_fraction_full 0.981
_diffrn_reflns_point_group_measured_fraction_max 0.972
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         70.141
_diffrn_reflns_theta_min         3.866
_exptl_absorpt_coefficient_mu    3.549
_exptl_absorpt_correction_T_max  0.7533
_exptl_absorpt_correction_T_min  0.4766
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0976 before and 0.0590 after correction.
The Ratio of minimum to maximum transmission is 0.6327.
The \l/2 correction factor is 0.0000.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.317
_exptl_crystal_description       block
_exptl_crystal_F_000             3080
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.17
_refine_diff_density_max         1.119
_refine_diff_density_min         -0.817
_refine_diff_density_rms         0.075
_refine_ls_abs_structure_details
;
 Flack x determined using 4623 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.016(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     873
_refine_ls_number_reflns         13829
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0733
_refine_ls_R_factor_gt           0.0620
_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^)+(0.0821P)^2^+10.4853P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1603
_refine_ls_wR_factor_ref         0.1709
_reflns_Friedel_coverage         0.787
_reflns_Friedel_fraction_full    0.960
_reflns_Friedel_fraction_max     0.946
_reflns_number_gt                12057
_reflns_number_total             13829
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8sc02532k2.cif
_cod_data_source_block           s3812ma
_cod_depositor_comments
'Adding full bibliography for 1549682--1549686.cif.'
_cod_database_code               1549682
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_max   0.584
_shelx_estimated_absorpt_t_min   0.387
_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.a Ternary CH refined with riding coordinates:
 C19(H19), C54(H54), C70(H70), C71(H71), C72(H72)
2.b Secondary CH2 refined with riding coordinates:
 C17(H17A,H17B), C20(H20A,H20B), C55(H55A,H55B), C63(H63A,H63B)
2.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C6(H6), C7(H7), C8(H8), C10(H10), C11(H11), C13(H13),
 C14(H14), C23(H23), C24(H24), C26(H26), C27(H27), C28(H28), C30(H30), C31(H31),
  C33(H33), C34(H34), C57(H57), C58(H58), C59(H59), C60(H60), C61(H61),
 C65(H65), C66(H66), C67(H67), C68(H68), C69(H69), N1(H1), N2(H2), N3(H3A),
 N4(H4A), N5(H5), N6(H6A), N7(H7A)
2.d Idealised Me refined as rotating group:
 C39(H39A,H39B,H39C), C40(H40A,H40B,H40C), C43(H43A,H43B,H43C), C44(H44A,H44B,
 H44C), C47(H47A,H47B,H47C), C48(H48A,H48B,H48C), C51(H51A,H51B,H51C), C52(H52A,
 H52B,H52C)
;
_shelx_res_checksum              94037
_olex2_diffrn_ambient_temperature_device 'Cryostream 700'
_olex2_submission_special_instructions 'No special instructions were received'