Hydrogen-Bonding-Driven 3D Supramolecular Assembly of Peptidomimetic Zipper.
Teng, Peng; Niu, Zheng; She, Fengyu; Zhou, Mi; Sang, Peng; Gray, Geoffrey M.; Verma, Gaurav; Wojtas, Lukasz; van der Vaart, Arjan; Ma, Shengqian; Cai, Jianfeng; Journal of the American Chemical Society 140 (2018) 5661–5665; doi:10.1021/jacs.7b11997

data_4131881
_publ_section_title
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 Hydrogen-Bonding-Driven 3D Supramolecular Assembly of Peptidomimetic
 Zipper.
;
_journal_issue                   17
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              5661
_journal_page_last               5665
_journal_paper_doi               10.1021/jacs.7b11997
_journal_volume                  140
_journal_year                    2018
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C103 H136 Cl7 N23 O30 S7, 10(C2 H3 N)'
_chemical_formula_sum            'C123 H166 Cl7 N33 O30 S7'
_chemical_formula_weight         3059.45
_space_group_crystal_system      tetragonal
_space_group_IT_number           92
_space_group_name_Hall           'P 4abw 2nw'
_space_group_name_H-M_alt        'P 41 21 2'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2018-02-15
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   17.0979(5)
_cell_length_b                   17.0979(5)
_cell_length_c                   28.8128(11)
_cell_measurement_reflns_used    9887
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      56.34
_cell_measurement_theta_min      2.58
_cell_volume                     8423.1(5)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_diffrn_ambient_temperature      99.99
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker D8 Venture PHOTON 100 CMOS'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  mirrors
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1135
_diffrn_reflns_av_unetI/netI     0.0501
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            44152
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        58.904
_diffrn_reflns_theta_max         58.904
_diffrn_reflns_theta_min         3.656
_diffrn_source                   'INCOATEC Imus micro-focus source'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.480
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7183
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1178 before and 0.0802 after correction.
The Ratio of minimum to maximum transmission is 0.7183.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.206
_exptl_crystal_description       block
_exptl_crystal_F_000             3212
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.391
_refine_diff_density_min         -0.465
_refine_diff_density_rms         0.079
_refine_ls_abs_structure_details
;
 Flack x determined using 1162 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.072(15)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     491
_refine_ls_number_reflns         6020
_refine_ls_number_restraints     257
_refine_ls_restrained_S_all      1.182
_refine_ls_R_factor_all          0.1558
_refine_ls_R_factor_gt           0.1106
_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^)+(0.1933P)^2^+7.6425P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3013
_refine_ls_wR_factor_ref         0.3544
_reflns_Friedel_coverage         0.738
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                3865
_reflns_number_total             6020
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b11997_si_002.cif
_cod_data_source_block           tp_g48_3_0213
_cod_original_cell_volume        8423.1(6)
_cod_database_code               4131881
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.790
_shelx_estimated_absorpt_t_min   0.755
_olex2_refinement_description
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1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups, All N(H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C202-C203
 1.45 with sigma of 0.001
 N201-C202
 1.15 with sigma of 0.001
 C302-C303
 1.45 with sigma of 0.001
 N301-C302
 1.15 with sigma of 0.001
 C402-C403
 1.45 with sigma of 0.001
 N401-C402
 1.15 with sigma of 0.001
 C602-C603
 1.45 with sigma of 0.001
 N601-C602
 1.15 with sigma of 0.001
 C702-C703
 1.45 with sigma of 0.001
 N701-C702
 1.15 with sigma of 0.001
 C802-C803
 1.45 with sigma of 0.001
 N801-C802
 1.15 with sigma of 0.001
 C902-C903
 1.45 with sigma of 0.001
 N901-C902
 1.15 with sigma of 0.001
 H90A-H43
 -2.2 with sigma of 0.005
 C502-C503
 1.45 with sigma of 0.001
 N501-C502
 1.15 with sigma of 0.001
 N201-C203
 2.6 with sigma of 0.005
 N301-C303
 2.6 with sigma of 0.005
 N401-C403
 2.6 with sigma of 0.005
 N601-C603
 2.6 with sigma of 0.005
 N701-C703
 2.6 with sigma of 0.005
 N801-C803
 2.6 with sigma of 0.005
 N901-C903
 2.6 with sigma of 0.005
 C902-H90A = C902-H90B = C902-H90C
 1.99 with sigma of 0.001
 C802-H80A = C802-H80B = C802-H80C
 1.99 with sigma of 0.001
 C702-H70A = C702-H70B = C702-H70C
 1.99 with sigma of 0.001
 C602-H60A = C602-H60B = C602-H60C
 1.99 with sigma of 0.001
 C402-H40A = C402-H40B = C402-H40C
 1.99 with sigma of 0.001
 C302-H30A = C302-H30B = C302-H30C
 1.99 with sigma of 0.001
 C202-H20A = C202-H20B = C202-H20C
 1.99 with sigma of 0.001
 C502-H50A = C502-H50B = C502-H50C
 1.99 with sigma of 0.001
 N501-C503
 2.6 with sigma of 0.005
3. Uiso/Uaniso restraints and constraints
C12 \\sim C13 \\sim C14 \\sim C15 \\sim C16 \\sim C17 \\sim Cl18: within 2A
with sigma of 0.04 and sigma for terminal atoms of 0.08
C42 \\sim C43 \\sim C44 \\sim C45 \\sim C46 \\sim C47 \\sim Cl48: within 2A
with sigma of 0.04 and sigma for terminal atoms of 0.08
C302 \\sim C303 \\sim N401 \\sim C402 \\sim C403 \\sim N501 \\sim C502 \\sim
C503 \\sim N601 \\sim C602 \\sim C603 \\sim N701 \\sim C702 \\sim N301 \\sim
C203 \\sim C202 \\sim N201 \\sim C803 \\sim C802 \\sim N801 \\sim C703 \\sim
N901 \\sim C902 \\sim C903: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08
4. Rigid body (RIGU) restrains
 C12, C13, C14, C15, C16, C17, Cl18
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C42, C43, C44, C45, C46, C47, Cl48
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: H3AA(0.75) H3AB(0.75) H3BC(0.25) H3BD(0.25) H3BE(0.25) N4(0.75)
 C5(0.75) H5A(0.75) H5B(0.75) C6(0.75) H6A(0.75) H7A(0.75) H6B(0.25) H7B(0.25)
 C8(0.75) H8A(0.75) H8B(0.75) H8C(0.75) S9(0.75) O10(0.75) O11(0.75) C12(0.75)
 C13(0.75) H13(0.75) C14(0.75) H14(0.75) C15(0.75) C16(0.75) H16(0.75)
 C17(0.75) H17(0.75) Cl18(0.75) N201(0.5) C202(0.5) C203(0.5) H20A(0.5)
 H20B(0.5) H20C(0.5) N301(0.25) C302(0.25) C303(0.25) H30A(0.25) H30B(0.25)
 H30C(0.25) N401(0.5) C402(0.5) C403(0.5) H40A(0.5) H40B(0.5) H40C(0.5)
 N501(0.25) C502(0.25) C503(0.25) H50A(0.25) H50B(0.25) H50C(0.25) N601(0.25)
 C602(0.25) C603(0.25) H60A(0.25) H60B(0.25) H60C(0.25) N701(0.25) C702(0.25)
 C703(0.25) H70A(0.25) H70B(0.25) H70C(0.25) N801(0.25) C802(0.25) C803(0.25)
 H80A(0.25) H80B(0.25) H80C(0.25) N901(0.25) C902(0.25) C903(0.25) H90A(0.25)
 H90B(0.25) H90C(0.25)
6.a Riding coordinates:
 C3(H3BC,H3BD,H3BE), N7(H6B,H7B), C203(H20A,H20B,H20C), C303(H30A,H30B,H30C),
 C403(H40A,H40B,H40C), C503(H50A,H50B,H50C), C603(H60A,H60B,H60C), C703(H70A,
 H70B,H70C), C803(H80A,H80B,H80C), C903(H90A,H90B,H90C)
6.b Ternary CH refined with riding coordinates:
 C6(H6A), C23(H23), C36(H36), C53(H53)
6.c Secondary CH2 refined with riding coordinates:
 C3(H3AA,H3AB), C5(H5A,H5B), C33(H33A,H33B), C35(H35A,H35B)
6.d Aromatic/amide H refined with riding coordinates:
 N7(H7A), C13(H13), C14(H14), C16(H16), C17(H17), N24(H24), N37(H37), C43(H43),
  C44(H44), C46(H46), C47(H47), N54(H54)
6.e Fitted hexagon refined as free rotating group:
 C12(C13,C14,C15,C16,C17), C42(C43,C44,C45,C46,C47)
6.f Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C25(H25A,H25B,H25C), C38(H38A,H38B,H38C), C55(H55A,H55B,H55C)
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_shelx_res_checksum              63652
_shelx_hkl_checksum              75335
_olex2_submission_special_instructions 'No special instructions were received'