Self-assembling α,γ-cyclic peptides that generate cavities with tunable properties
Rodríguez-Vázquez, Nuria; García-Fandiño, Rebeca; Amorín, Manuel; Granja, Juan R.; Chem. Sci. 7 (2016) 183–; doi:10.1039/C5SC03187G

data_1531039
_publ_section_title
;
 Self-assembling \a,\g-cyclic peptides that generate cavities with tunable
 properties
;
_journal_issue                   1
_journal_name_full               'Chem. Sci.'
_journal_page_first              183
_journal_paper_doi               10.1039/C5SC03187G
_journal_volume                  7
_journal_year                    2016
_chemical_absolute_configuration rmad
_chemical_formula_moiety         'C66 H100 N8 O12, 4.462(C H Cl3), 0.053(O)'
_chemical_formula_sum            'C70.45 H104.45 Cl13.38 N8 O12.05'
_chemical_formula_weight         1730.54
_chemical_name_systematic        NR443-B
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_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   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4.3
_audit_creation_date             2015-05-11T09:35:12-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_update_record
;
2015-05-11 deposited with the CCDC.
2015-09-11 downloaded from the CCDC.
;
_cell_angle_alpha                90.131(2)
_cell_angle_beta                 93.427(3)
_cell_angle_gamma                91.090(3)
_cell_formula_units_Z            4
_cell_length_a                   14.3767(9)
_cell_length_b                   24.3477(16)
_cell_length_c                   24.5528(14)
_cell_measurement_reflns_used    9930
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      18.87
_cell_measurement_theta_min      2.29
_cell_measurement_wavelength     0.71073
_cell_volume                     8577.5(9)
_computing_cell_refinement       'SAINT V8.34A integration software'
_computing_data_collection       'Bruker APEX2 software'
_computing_data_reduction        'SORTAV (Blessing, 1995)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 2012)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT-2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'APEX-II CCD'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II'
_diffrn_measurement_method       '\f or \w oscillation scans'
_diffrn_orient_matrix_UB_11      0.018647
_diffrn_orient_matrix_UB_12      0.039468
_diffrn_orient_matrix_UB_13      0.005701
_diffrn_orient_matrix_UB_21      -0.062337
_diffrn_orient_matrix_UB_22      0.011343
_diffrn_orient_matrix_UB_23      -0.015904
_diffrn_orient_matrix_UB_31      -0.024975
_diffrn_orient_matrix_UB_32      -0.001046
_diffrn_orient_matrix_UB_33      0.03714
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0926
_diffrn_reflns_av_unetI/netI     0.118
_diffrn_reflns_laue_measured_fraction_full 0.999
_diffrn_reflns_laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            160890
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_reduction_process
;
        Scaled and merged with Sortav
        R.H. Blessing, (1987) Cryst. Rev. 1, 3-58
        R.H. Blessing, (1989) J. Appl. Cryst. 22, 396-397
;
_diffrn_reflns_theta_full        21.966
_diffrn_reflns_theta_max         21.966
_diffrn_reflns_theta_min         1.419
_diffrn_source                   'sealed x-ray tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.489
_exptl_absorpt_correction_T_max  0.958
_exptl_absorpt_correction_T_min  0.848
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 - Bruker AXS area detector scaling and absorption correction
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.34
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             3628
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: CHCl3'
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.551
_refine_diff_density_min         -0.434
_refine_diff_density_rms         0.078
_refine_ls_abs_structure_details
;
 Flack x determined using 9462 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.03(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     4670
_refine_ls_number_reflns         41489
_refine_ls_number_restraints     5300
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.1402
_refine_ls_R_factor_gt           0.0823
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1252P)^2^+15.5443P+1.0sin\q/\l] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1987
_refine_ls_wR_factor_ref         0.2339
_reflns_Friedel_coverage         0.984
_reflns_friedel_fraction_full    0.983
_reflns_friedel_fraction_max     0.983
_reflns_number_gt                26837
_reflns_number_total             41489
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5sc03187g2.cif
_cod_data_source_block           shelx
_cod_depositor_comments          'Adding full bibliography for 1531039.cif.'
_cod_database_code               1531039
_shelx_estimated_absorpt_t_min   0.887
_shelx_estimated_absorpt_t_max   0.944
_shelx_res_checksum              3442
_shelx_hkl_checksum              93309