Heterogeneous h-bonding in a foldamer helix.
Fisher, Brian F.; Guo, Li; Dolinar, Brian S.; Guzei, Ilia A.; Gellman, Samuel H.; Journal of the American Chemical Society 137 (2015) 6484–6487; doi:10.1021/jacs.5b03382

data_4123641
_publ_section_title
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 Heterogeneous h-bonding in a foldamer helix.
;
_journal_issue                   20
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              6484
_journal_page_last               6487
_journal_paper_doi               10.1021/jacs.5b03382
_journal_volume                  137
_journal_year                    2015
_chemical_formula_moiety         'C50 H68 N4 O7, 0.82(C H Cl3), 0.18(C7 H16)'
_chemical_formula_sum            'C52.11 H71.78 Cl2.44 N4 O7'
_chemical_formula_weight         952.90
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2014-03-26
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2014.03.20 svn.r2914 for OlexSys, GUI svn.r4813)
;
_cell_angle_alpha                96.227(2)
_cell_angle_beta                 108.4600(18)
_cell_angle_gamma                105.9040(18)
_cell_formula_units_Z            2
_cell_length_a                   11.5447(4)
_cell_length_b                   14.2478(5)
_cell_length_c                   17.4006(6)
_cell_measurement_reflns_used    9493
_cell_measurement_temperature    100
_cell_measurement_theta_max      30.099
_cell_measurement_theta_min      2.201
_cell_volume                     2550.47(16)
_computing_cell_refinement       'SAINT+ Ver. 8.34A (Bruker-AXS, 2014)'
_computing_data_collection       'APEX2 Ver. 2014.1-1 (Bruker-AXS, 2014)'
_computing_data_reduction        'SAINT+ Ver. 8.34A (Bruker-AXS, 2014)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.0
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX2 area detector'
_diffrn_measurement_method       '0.5\ \w and 0.5\ \f scans'
_diffrn_radiation_collimation    'focusing mirrors'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0557
_diffrn_reflns_av_unetI/netI     0.0599
_diffrn_reflns_laue_measured_fraction_full 0.999
_diffrn_reflns_laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            62220
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         30.615
_diffrn_reflns_theta_min         1.263
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    0.204
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6833
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0566 before and 0.0484 after correction.
The Ratio of minimum to maximum transmission is 0.9158.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.241
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1020
_exptl_crystal_size_max          0.162
_exptl_crystal_size_mid          0.119
_exptl_crystal_size_min          0.091
_refine_diff_density_max         0.539
_refine_diff_density_min         -0.439
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     640
_refine_ls_number_reflns         15641
_refine_ls_number_restraints     19
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0937
_refine_ls_R_factor_gt           0.0546
_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^)+(0.0615P)^2^+1.0029P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1260
_refine_ls_wR_factor_ref         0.1433
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10392
_reflns_number_total             15641
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            gellman155.cif
_cod_data_source_block           gellman155
_cod_depositor_comments
'Adding full bibliography for 4123639--4123645.cif.'
_cod_database_code               4123641
_shelxl_version_number           2014-3
_shelx_estimated_absorpt_t_max   0.982
_shelx_estimated_absorpt_t_min   0.968
_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, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C58-C57 = C57-C56 = C56-C55 = C55-C54 = C54-C53 = C53-C52
 1.529 with sigma of 0.003
 C52-C54 = C53-C55 = C54-C56 = C55-C57 = C56-C58
 2.555 with sigma of 0.004
 N1-H1 = N2-H2 = N3-H3 = N4-H4
 0.88 with sigma of 0.01
 C8-C7 \\sim C8A-C7
 with sigma of 0.004
3. Others
 Sof(H7BC)=Sof(H7BD)=Sof(C8A)=Sof(C9A)=Sof(H9A)=Sof(C10A)=Sof(H10A)=Sof(C11A)=
 Sof(H11A)=Sof(C12A)=Sof(H12A)=Sof(C13A)=Sof(H13A)=1-FVAR(1)
 Sof(H7AA)=Sof(H7AB)=Sof(C8)=Sof(C9)=Sof(H9)=Sof(C10)=Sof(H10)=Sof(C11)=
 Sof(H11)=Sof(C12)=Sof(H12)=Sof(C13)=Sof(H13)=FVAR(1)
 Sof(C52)=Sof(H52A)=Sof(H52B)=Sof(H52C)=Sof(C53)=Sof(H53A)=Sof(H53B)=Sof(C54)=
 Sof(H54A)=Sof(H54B)=Sof(C55)=Sof(H55A)=Sof(H55B)=Sof(C56)=Sof(H56A)=Sof(H56B)=
 Sof(C57)=Sof(H57A)=Sof(H57B)=Sof(C58)=Sof(H58A)=Sof(H58B)=Sof(H58C)=1-FVAR(2)
 Sof(Cl1)=Sof(Cl2)=Sof(Cl3)=Sof(C51)=Sof(H51)=FVAR(2)
 Fixed Uiso: C52(0.08) C53(0.08) C54(0.08) C55(0.08) C56(0.08) C57(0.08)
 C58(0.08)
4.a Ternary CH refined with riding coordinates:
 C6(H6), C15(H15), C20(H20), C21(H21), C25(H25), C34(H34), C39(H39), C40(H40),
 C51(H51)
4.b Secondary CH2 refined with riding coordinates:
 C7(H7AA,H7AB), C7(H7BC,H7BD), C16(H16A,H16B), C17(H17A,H17B), C18(H18A,H18B),
 C19(H19A,H19B), C22(H22A,H22B), C26(H26A,H26B), C35(H35A,H35B), C36(H36A,H36B),
  C37(H37A,H37B), C38(H38A,H38B), C41(H41A,H41B), C44(H44A,H44B), C53(H53A,
 H53B), C54(H54A,H54B), C55(H55A,H55B), C56(H56A,H56B), C57(H57A,H57B)
4.c Aromatic/amide H refined with riding coordinates:
 C9(H9), C10(H10), C11(H11), C12(H12), C13(H13), C9A(H9A), C10A(H10A),
 C11A(H11A), C12A(H12A), C13A(H13A), C28(H28), C29(H29), C30(H30), C31(H31),
 C32(H32), C46(H46), C47(H47), C48(H48), C49(H49), C50(H50)
4.d Fitted hexagon refined as free rotating group:
 C8A(C9A,C10A,C11A,C12A,C13A)
4.e Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C23(H23A,H23B,H23C),
 C42(H42A,H42B,H42C), C52(H52A,H52B,H52C), C58(H58A,H58B,H58C)
;
_shelx_res_checksum              43359
_shelx_hkl_checksum              5658