Backbone conformation affects duplex initiation and duplex propagation in hybridisation of synthetic H-bonding oligomers.
Iadevaia, Giulia; Núñez-Villanueva, Diego; Stross, Alexander E.; Hunter, Christopher A.; Organic & biomolecular chemistry 16 (2018) 4183–4190; doi:10.1039/c8ob00819a

data_7156266
_publ_section_title
;
 Backbone conformation affects duplex initiation and duplex propagation in
 hybridisation of synthetic H-bonding oligomers.
;
_journal_issue                   22
_journal_name_full               'Organic &amp; biomolecular chemistry'
_journal_page_first              4183
_journal_page_last               4190
_journal_paper_doi               10.1039/c8ob00819a
_journal_volume                  16
_journal_year                    2018
_chemical_formula_moiety         'C72 H112 N2 O8 P2'
_chemical_formula_sum            'C72 H112 N2 O8 P2'
_chemical_formula_weight         1195.57
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2018-04-06
_audit_creation_method
;
Olex2 1.2
(compiled Nov 22 2016 11:51:51 for OlexSys, GUI svn.r5269)
;
_audit_update_record
;
2018-04-06 deposited with the CCDC.
2018-04-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 109.030(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   21.0973(5)
_cell_length_b                   11.5790(3)
_cell_length_c                   14.9601(4)
_cell_measurement_reflns_used    4868
_cell_measurement_temperature    150
_cell_measurement_theta_max      24.456
_cell_measurement_theta_min      2.273
_cell_volume                     3454.81(16)
_computing_cell_refinement       'SAINT v7.60A (Bruker, 2009)'
_computing_data_reduction        'SAINT v7.60A (Bruker, 2009)'
_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, 2018)"
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0508
_diffrn_reflns_av_unetI/netI     0.0449
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            32750
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.588
_diffrn_reflns_theta_min         1.021
_exptl_absorpt_coefficient_mu    0.117
_exptl_absorpt_correction_T_max  0.9764
_exptl_absorpt_correction_T_min  0.9536
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 TWINABS-2008/2 (Bruker,2010) was used for absorption correction.
 
For component 1:
 wR2(int) was 0.1338 before and 0.0538 after correction.
 The Ratio of minimum to maximum transmission is 0.77.
 The \l/2 correction factor is Not present

Final HKLF 4 output contains 58563 reflections, Rint = 0.0874
 (10951 with I > 3sig(I), Rint = 0.0335)
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.149
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1304
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: acetonitrile'
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.21
_refine_diff_density_max         1.390
_refine_diff_density_min         -1.366
_refine_diff_density_rms         0.135
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.904
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     327
_refine_ls_number_reflns         7942
_refine_ls_number_restraints     207
_refine_ls_restrained_S_all      1.951
_refine_ls_R_factor_all          0.1938
_refine_ls_R_factor_gt           0.1540
_refine_ls_shift/su_max          0.014
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.4485
_refine_ls_wR_factor_ref         0.4875
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5179
_reflns_number_total             7942
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8ob00819a2.cif
_cod_data_source_block           och544p21c
_cod_depositor_comments          'Adding full bibliography for 7156266.cif.'
_cod_database_code               7156266
_shelx_estimated_absorpt_t_max   0.976
_shelx_estimated_absorpt_t_min   0.953
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 P1-C16
 2.6 with sigma of 0.02
 C15-C16 \\sim C15-C18 \\sim C15-C17 \\sim C15-C18
 with sigma of 0.003
 C19-C20 \\sim C19-C21 \\sim C19-C22 \\sim C19-C20
 with sigma of 0.003
3. Rigid bond restraints
 C1, C2, C3, C4, C5, C6, C7, C8, C9, C10, C11, C12, C13, C14, C15, C15', C16,
 C16', C17, C17', C18, C18', C19, C19', C20, C20', C21, C21', C22, C22', C23,
 C24, C25, C26, C27, C28, C29, C30, C31, C32, C33, C34, C35, C28', C29', C32',
 C34', C30', C31', C33'
 with sigma for 1-2 distances of 0.003 and sigma for 1-3 distances of 0.006
4. Uiso/Uaniso restraints and constraints
C1 \\sim C2 \\sim C3 \\sim C4 \\sim C5 \\sim C6 \\sim C7 \\sim C8 \\sim C9
\\sim C10 \\sim C11 \\sim C12 \\sim C13 \\sim C14 \\sim C15 \\sim C15' \\sim
C16 \\sim C16' \\sim C17 \\sim C17' \\sim C18 \\sim C18' \\sim C19 \\sim C19'
\\sim C20 \\sim C20' \\sim C21 \\sim C21' \\sim C22 \\sim C22' \\sim C23 \\sim
C24 \\sim C25 \\sim C26 \\sim C27 \\sim C28 \\sim C29 \\sim C30 \\sim C31 \\sim
C32 \\sim C33 \\sim C34 \\sim C35 \\sim C28' \\sim C29' \\sim C32' \\sim C34'
\\sim C30' \\sim C31' \\sim C33': within 2A with sigma of 0.003 and sigma for
terminal atoms of 0.006
5. Others
 Sof(C15')=Sof(C17')=Sof(H17D)=Sof(H17E)=Sof(H17F)=Sof(C18')=Sof(H18D)=
 Sof(H18E)=Sof(H18F)=Sof(C19')=Sof(C20')=Sof(H20D)=Sof(H20E)=Sof(H20F)=
 Sof(C21')=Sof(H21D)=Sof(H21E)=Sof(H21F)=Sof(C22')=Sof(H22D)=Sof(H22E)=
 Sof(H22F)=Sof(H27C)=Sof(H27D)=Sof(O4')=Sof(C28')=Sof(H28')=Sof(C29')=Sof(H29C)=
 Sof(H29D)=Sof(C32')=Sof(H32D)=Sof(H32E)=Sof(H32F)=Sof(C34')=Sof(H34D)=
 Sof(H34E)=Sof(H34F)=Sof(C30')=Sof(H30C)=Sof(H30D)=Sof(C31')=Sof(H31C)=
 Sof(H31D)=Sof(C33')=Sof(H33C)=Sof(H33D)=1-FVAR(1)
 Sof(C15)=Sof(C17)=Sof(H17A)=Sof(H17B)=Sof(H17C)=Sof(C18)=Sof(H18A)=Sof(H18B)=
 Sof(H18C)=Sof(C19)=Sof(C20)=Sof(H20A)=Sof(H20B)=Sof(H20C)=Sof(C21)=Sof(H21A)=
 Sof(H21B)=Sof(H21C)=Sof(C22)=Sof(H22A)=Sof(H22B)=Sof(H22C)=Sof(H27A)=Sof(H27B)=
 Sof(O4)=Sof(C28)=Sof(H28)=Sof(C29)=Sof(H29A)=Sof(H29B)=Sof(C30)=Sof(H30A)=
 Sof(H30B)=Sof(C31)=Sof(H31A)=Sof(H31B)=Sof(C32)=Sof(H32A)=Sof(H32B)=Sof(H32C)=
 Sof(C33)=Sof(H33A)=Sof(H33B)=Sof(C34)=Sof(H34A)=Sof(H34B)=Sof(H34C)=FVAR(1)
6.a Free rotating group:
 O4(C28,C29,C30,C31,C32,C33,C34,C35,O4',C28',C29',C32',C34',C30',C31',C33')
6.b Ternary CH refined with riding coordinates:
 C28(H28), C28'(H28')
6.c Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C14(H14A,H14B), C23(H23A,H23B), C27(H27C,H27D), C27(H27A,H27B),
 C29(H29A,H29B), C30(H30A,H30B), C31(H31A,H31B), C33(H33A,H33B), C29'(H29C,
 H29D), C30'(H30C,H30D), C31'(H31C,H31D), C33'(H33C,H33D)
6.d Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C9(H9), C10(H10), C12(H12), C13(H13), C25(H25)
6.e Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C16'(H16D,H16E,H16F), C17(H17A,H17B,H17C), C17'(H17D,
 H17E,H17F), C18(H18A,H18B,H18C), C18'(H18D,H18E,H18F), C20(H20A,H20B,H20C),
 C20'(H20D,H20E,H20F), C21(H21A,H21B,H21C), C21'(H21D,H21E,H21F), C22(H22A,H22B,
 H22C), C22'(H22D,H22E,H22F), C32(H32A,H32B,H32C), C34(H34A,H34B,H34C),
 C35(H35A,H35B,H35C), C32'(H32D,H32E,H32F), C34'(H34D,H34E,H34F)
;
_shelx_res_checksum              62775
_shelx_shelxl_version_number     2018/3
_olex2_submission_special_instructions 'No special instructions were received'