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_1546534
_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_formula_moiety
'8(C40 H36 N20 O4), 13(C16 H36 N), 8(H2 O7 P2), 9(C6 H12 O2), C3 H6 O, H2 O'
_chemical_formula_sum            'C585 H888 N173 O108 P16'
_chemical_formula_weight         12568.15
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_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   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                76.0283(8)
_cell_angle_beta                 79.8139(8)
_cell_angle_gamma                73.4101(11)
_cell_formula_units_Z            2
_cell_length_a                   22.1903(3)
_cell_length_b                   31.9713(4)
_cell_length_c                   61.8821(4)
_cell_measurement_reflns_used    48002
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      70.8100
_cell_measurement_theta_min      3.6800
_cell_volume                     40554.3(8)
_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 2014/5 (Sheldrick, 2015)'
_diffrn_ambient_temperature      123(2)
_diffrn_detector_area_resol_mean 10.3953
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.958
_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  0.0446
_diffrn_reflns_av_unetI/netI     0.0554
_diffrn_reflns_Laue_measured_fraction_full 0.975
_diffrn_reflns_Laue_measured_fraction_max 0.958
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_l_max       53
_diffrn_reflns_limit_l_min       -75
_diffrn_reflns_number            238782
_diffrn_reflns_point_group_measured_fraction_full 0.975
_diffrn_reflns_point_group_measured_fraction_max 0.958
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         69.999
_diffrn_reflns_theta_min         3.511
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    0.878
_exptl_absorpt_correction_T_max  0.925
_exptl_absorpt_correction_T_min  0.806
_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    1.029
_exptl_crystal_description       plate
_exptl_crystal_F_000             13426
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.210
_exptl_crystal_size_min          0.080
_refine_diff_density_max         0.873
_refine_diff_density_min         -0.678
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     8199
_refine_ls_number_reflns         147346
_refine_ls_number_restraints     1968
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.1171
_refine_ls_R_factor_gt           0.0800
_refine_ls_shift/su_max          0.020
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1629P)^2^+7.1351P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2302
_refine_ls_wR_factor_ref         0.2710
_reflns_Friedel_coverage         0.000
_reflns_number_gt                91821
_reflns_number_total             147346
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7sc02700a2.cif
_cod_data_source_block           2-rac-2_DHPP-2
_cod_database_code               1546534
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_min   0.779
_shelx_estimated_absorpt_t_max   0.933
_shelx_res_checksum              70484
_shelx_fab_checksum              94883