Efficient stabilisation of a dihydrogenphosphate tetramer and a dihydrogenpyrophosphate dimer by a cyclic pseudopeptide containing 1,4-disubstituted 1,2,3-triazole moieties
Mungalpara, Disha; Valkonen, Arto; Rissanen, Kari; Kubik, Stefan; Chem. Sci.  (2017) –; doi:10.1039/C7SC02700A

data_1546532
_publ_section_title
;
 Efficient stabilisation of a dihydrogenphosphate tetramer and a
 dihydrogenpyrophosphate dimer by a cyclic pseudopeptide containing
 1,4-disubstituted 1,2,3-triazole moieties
;
_journal_name_full               'Chem. Sci.'
_journal_paper_doi               10.1039/C7SC02700A
_journal_year                    2017
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C40 H36 N20 O4, C16 H36 N, H2 O7 P2'
_chemical_formula_sum            'C56 H74 N21 O11 P2'
_chemical_formula_weight         1279.30
_space_group_crystal_system      trigonal
_space_group_IT_number           150
_space_group_name_Hall           'P 3 2"'
_space_group_name_H-M_alt        'P 3 2 1'
_symmetry_space_group_name_Hall  'P 3 2"'
_symmetry_space_group_name_H-M   'P 3 2 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2016/6
_audit_update_record
;
2017-06-14 deposited with the CCDC.
2017-07-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   28.3369(4)
_cell_length_b                   28.3369(4)
_cell_length_c                   58.9056(13)
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_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      72.5210
_cell_measurement_theta_min      3.6470
_cell_volume                     40963.0(12)
_computing_cell_refinement       CrysAlisPro
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        CrysAlisPro
_computing_molecular_graphics    SHELXL-2016/6
_computing_publication_material  SHELXL-2016/6
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 10.3953
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0697
_diffrn_reflns_av_unetI/netI     0.0779
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       70
_diffrn_reflns_limit_l_min       -66
_diffrn_reflns_number            121482
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         67.994
_diffrn_reflns_theta_min         3.462
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    0.290
_exptl_absorpt_correction_T_max  0.951
_exptl_absorpt_correction_T_min  0.879
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    0.311
_exptl_crystal_description       prism
_exptl_crystal_F_000             4050
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.070
_refine_diff_density_max         0.563
_refine_diff_density_min         -0.544
_refine_diff_density_rms         0.073
_refine_ls_abs_structure_details
;
 Twinning involves inversion, so Flack parameter cannot be determined
;
_refine_ls_extinction_coef       0.00180(18)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2016/6 (Sheldrick 2016)'
_refine_ls_goodness_of_fit_ref   1.355
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     789
_refine_ls_number_reflns         49626
_refine_ls_number_restraints     561
_refine_ls_restrained_S_all      1.425
_refine_ls_R_factor_all          0.1571
_refine_ls_R_factor_gt           0.1378
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3698
_refine_ls_wR_factor_ref         0.3929
_reflns_Friedel_coverage         0.877
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                35387
_reflns_number_total             49626
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7sc02700a2.cif
_cod_data_source_block           2-2_DHPP-2
_cod_original_cell_volume        40963.0(15)
_cod_database_code               1546532
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_min   0.931
_shelx_estimated_absorpt_t_max   0.980
_shelx_res_checksum              79309
_shelx_fab_checksum              28797