Synthesis, crystallization, X-ray structural characterization and solid-state assembly of a cyclic hexapeptoid with propargyl and methoxyethyl side chains
Tedesco, Consiglia; Macedi, Eleonora; Meli, Alessandra; Pierri, Giovanni; Della Sala, Giorgio; Drathen, Christina; Fitch, Andrew N.; Vaughan, Gavin B. M.; Izzo, Irene; De Riccardis, Francesco; Acta Crystallographica Section B 73 (2017) 399–412; doi:10.1107/S2052520617002505

data_2108108
_publ_section_title
;
 Synthesis, crystallization, X-ray structural characterization and
 solid-state assembly of a cyclic hexapeptoid with propargyl and
 methoxyethyl side chains
;
_journal_coeditor_code           PS5059
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first              399
_journal_page_last               412
_journal_paper_doi               10.1107/S2052520617002505
_journal_volume                  73
_journal_year                    2017
_chemical_formula_moiety         'C30 H46 N6 O10, H2 O'
_chemical_formula_sum            'C30 H48 N6 O11'
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_space_group_name_Hall           '-P 1'
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_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                78.362(5)
_cell_angle_beta                 88.664(7)
_cell_angle_gamma                83.547(5)
_cell_formula_units_Z            2
_cell_length_a                   8.363(4)
_cell_length_b                   9.394(4)
_cell_length_c                   21.648(10)
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_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      12.303
_cell_measurement_theta_min      0.798
_cell_volume                     1655.2(13)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.801
_diffrn_measurement_device_type  'ID11 ESRF beamline goniometer'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.2952
_diffrn_reflns_av_R_equivalents  0.0386
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
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_diffrn_reflns_theta_full        10.202
_diffrn_reflns_theta_max         12.303
_diffrn_reflns_theta_min         0.798
_exptl_absorpt_coefficient_mu    0.031
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.342
_exptl_crystal_description       needle
_exptl_crystal_F_000             716
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.025
_exptl_crystal_size_min          0.010
_refine_diff_density_max         0.709
_refine_diff_density_min         -0.378
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.138
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     430
_refine_ls_number_reflns         8341
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.138
_refine_ls_R_factor_all          0.0814
_refine_ls_R_factor_gt           0.0731
_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^)+(0.1031P)^2^+1.1901P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
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_reflns_number_gt                7288
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_reflns_threshold_expression     'I > 2\s(I)'
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_cod_original_cell_volume        1655.1(13)
_cod_database_code               2108108
_cod_database_fobs_code          2108108
_shelx_hkl_checksum              71158
_shelx_res_checksum              8227