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_1546535
_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
'3(C40 H36 N20 O4), 6(C16 H36 N), 3(H2 O7 P2), 4(C2 H6 O S), 1.61O'
_chemical_formula_sum            'C224 H354 N66 O38.61 P6 S4'
_chemical_formula_weight         4903.61
_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   geom
_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                72.4310(10)
_cell_angle_beta                 82.4440(10)
_cell_angle_gamma                60.3890(10)
_cell_formula_units_Z            4
_cell_length_a                   28.2322(3)
_cell_length_b                   28.4659(3)
_cell_length_c                   39.1611(5)
_cell_measurement_reflns_used    117645
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      68.9080
_cell_measurement_theta_min      3.5070
_cell_volume                     26079.5(6)
_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 0.994
_diffrn_measured_fraction_theta_max 0.993
_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  0.0656
_diffrn_reflns_av_unetI/netI     0.0377
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       47
_diffrn_reflns_limit_l_min       -46
_diffrn_reflns_number            453951
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         67.999
_diffrn_reflns_theta_min         3.365
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    1.330
_exptl_absorpt_correction_T_max  0.921
_exptl_absorpt_correction_T_min  0.762
_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    1.249
_exptl_crystal_description       plate
_exptl_crystal_F_000             10492
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.270
_exptl_crystal_size_min          0.090
_refine_diff_density_max         1.967
_refine_diff_density_min         -2.065
_refine_diff_density_rms         0.111
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.671
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     6486
_refine_ls_number_reflns         94326
_refine_ls_number_restraints     2100
_refine_ls_restrained_S_all      1.732
_refine_ls_R_factor_all          0.1375
_refine_ls_R_factor_gt           0.1161
_refine_ls_shift/su_max          0.014
_refine_ls_shift/su_mean         0.001
_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          0.3604
_refine_ls_wR_factor_ref         0.3926
_reflns_Friedel_coverage         0.000
_reflns_number_gt                72636
_reflns_number_total             94326
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7sc02700a2.cif
_cod_data_source_block           2-rac-2_DHPP-2_2
_cod_database_code               1546535
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_min   0.618
_shelx_estimated_absorpt_t_max   0.890
_shelx_res_checksum              53248
_shelx_fab_checksum              81354