NMR-based quantitative studies of the conformational equilibrium between their square and folded forms of ascidiacyclamide and its analogues
Asano, Akiko; Minoura, Katsuhiko; Kojima, Yuki; Yoshii, Taishi; Ito, Ryoya; Yamada, Takeshi; Kato, Takuma; Doi, Mitsunobu; RSC Advances 10 (2020) 33317–33326; doi:10.1039/D0RA07396B

data_7241204
_publ_section_title
;
 NMR-based quantitative studies of the conformational equilibrium between
 their square and folded forms of ascidiacyclamide and its analogues
;
_journal_issue                   55
_journal_name_full               'RSC Advances'
_journal_page_first              33317
_journal_page_last               33326
_journal_paper_doi               10.1039/D0RA07396B
_journal_volume                  10
_journal_year                    2020
_chemical_absolute_configuration rm
_chemical_compound_source        synthesis
_chemical_formula_moiety         'C38 H54 N8 O6 S2, 2(C4 H9 N O), H2 O'
_chemical_formula_sum            'C46 H74 N10 O9 S2'
_chemical_formula_weight         975.27
_chemical_name_systematic
; 
 cyclo(Chg-Oxz-D-Val-Thz-Ile-Oxz-D-Val-Thz).H2O.2DMA
;
_space_group_IT_number           76
_space_group_name_Hall           'P 4w'
_space_group_name_H-M_alt        'P 41'
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_H-M   'P 41'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2020-06-02 deposited with the CCDC.	2020-09-03 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.9682(9)
_cell_length_b                   12.9682(9)
_cell_length_c                   30.798(3)
_cell_measurement_reflns_used    6185
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      23.52
_cell_measurement_theta_min      2.22
_cell_volume                     5179.4(7)
_computing_cell_refinement       'SAINTPLUS (Bruker, 1998)'
_computing_data_collection       'SMART (Bruker, 1998)'
_computing_data_reduction        'SAINTPLUS (Bruker, 1998)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      200(2)
_diffrn_detector_area_resol_mean 8.366
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'CCD (Bruker APEX)'
_diffrn_measurement_method       \w-scan
_diffrn_radiation_monochromator  'conforcal (Bruker Montel)'
_diffrn_radiation_source         'rotating anode (M18XCE)'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0370
_diffrn_reflns_av_sigmaI/netI    0.0397
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            47663
_diffrn_reflns_theta_full        27.87
_diffrn_reflns_theta_max         27.87
_diffrn_reflns_theta_min         1.57
_diffrn_standards_decay_%        0.0
_diffrn_standards_interval_count 47663
_diffrn_standards_interval_time  780
_diffrn_standards_number         365
_exptl_absorpt_coefficient_mu    0.164
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.9141
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.251
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       bipyrimidal
_exptl_crystal_F_000             2096
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: N,N-dimethykacetamide'
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.637
_refine_diff_density_min         -0.560
_refine_diff_density_rms         0.085
_refine_ls_abs_structure_details 'Flack (1983), 5918 Friedel pairs'
_refine_ls_abs_structure_Flack   0.09(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     604
_refine_ls_number_reflns         12202
_refine_ls_number_restraints     51
_refine_ls_restrained_S_all      1.098
_refine_ls_R_factor_all          0.0907
_refine_ls_R_factor_gt           0.0799
_refine_ls_shift/su_max          0.011
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1273P)^2^+6.6054P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2149
_refine_ls_wR_factor_ref         0.2243
_reflns_number_gt                10492
_reflns_number_total             12202
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            d0ra07396b2.cif
_cod_data_source_block           chg
_cod_depositor_comments
'Adding full bibliography for 7241202--7241204.cif.'
_cod_original_sg_symbol_H-M      P41
_cod_database_code               7241204