Spontaneous Self-Assembly of Fully Protected Ester 1:1 [α/α-N<sup>α</sup>-Bn-hydrazino] Pseudodipeptides into a Twisted Parallel β-Sheet in the Crystal State.
Romero, Eugénie; Moussodia, Ralph-Olivier; Kriznik, Alexandre; Wenger, Emmanuel; Acherar, Samir; Jamart-Grégoire, Brigitte; The Journal of organic chemistry 81 (2016) 9037–9045; doi:10.1021/acs.joc.6b01680

data_4037192
_publ_section_title
;
 Spontaneous Self-Assembly of Fully Protected Ester 1:1
 [\a/\a-N<sup>\a</sup>-Bn-hydrazino] Pseudodipeptides into a Twisted
 Parallel \b-Sheet in the Crystal State.
;
_journal_issue                   19
_journal_name_full               'The Journal of organic chemistry'
_journal_page_first              9037
_journal_page_last               9045
_journal_paper_doi               10.1021/acs.joc.6b01680
_journal_volume                  81
_journal_year                    2016
_chemical_formula_sum            'C22 H35 N3 O5'
_chemical_formula_weight         421.53
_chemical_melting_point          359
_chemical_name_systematic        '1:1[\a/\a-N\a-Bn-hydrazino] ester (S/S)'
_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'
_atom_sites_solution_hydrogens   geom
_audit_block_doi                 10.5517/cc1kl8yc
_audit_creation_method           SHELXL-2014
_audit_update_record
;
2016-01-14 deposited with the CCDC.
2016-04-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   12.284
_cell_length_b                   21.276
_cell_length_c                   38.207
_cell_measurement_reflns_used    23964
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      76.3550
_cell_measurement_theta_min      3.7290
_cell_volume                     9985.567
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.4508
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scan'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0439
_diffrn_reflns_av_unetI/netI     0.0302
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       46
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            82658
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.662
_diffrn_reflns_theta_min         1.741
_diffrn_source                   'sealed X-ray tube'
_exptl_absorpt_coefficient_mu    0.079
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.61705
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.122
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             3648
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Dichloromethane/petroleum ether'
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.581
_refine_diff_density_min         -0.965
_refine_diff_density_rms         0.125
_refine_ls_abs_structure_details
;
 Flack x determined using 7084 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -1.7(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.534
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1104
_refine_ls_number_reflns         20760
_refine_ls_number_restraints     1004
_refine_ls_restrained_S_all      1.518
_refine_ls_R_factor_all          0.1324
_refine_ls_R_factor_gt           0.1214
_refine_ls_shift/su_max          1.937
_refine_ls_shift/su_mean         0.013
_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          0.3325
_refine_ls_wR_factor_ref         0.3550
_reflns_Friedel_coverage         0.832
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.984
_reflns_number_gt                17535
_reflns_number_total             20760
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jo6b01680_si_004.cif
_cod_data_source_block           eug_er62h
_cod_depositor_comments
;

2020-08-12
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C88 H140 N12 O20'
_cod_original_formula_weight         1686.11
_cod_original_formula_units_Z            4
_cod_original_cell_volume        9985.6
_cod_database_code               4037192
_shelxl_version_number           2014-3
_shelx_res_checksum              2181
_shelx_hkl_checksum              65732