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_7241202
_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         'C37 H54 N8 O6 S2, 2(C3 H7 N O)'
_chemical_formula_sum            'C43 H68 N10 O8 S2'
_chemical_formula_weight         917.20
_chemical_name_systematic        '[Tbu]ASC'
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2016/4
_audit_update_record
;
2020-06-02 deposited with the CCDC.	2020-09-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.703(5)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.9799(6)
_cell_length_b                   12.1900(7)
_cell_length_c                   15.9375(8)
_cell_measurement_reflns_used    5864
_cell_measurement_temperature    100
_cell_measurement_theta_max      74.0830
_cell_measurement_theta_min      5.4090
_cell_volume                     2460.0(2)
_computing_cell_refinement       'CrysAlisPro 1.171.39.7e (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.7e (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.7e (Rigaku OD, 2015)'
_computing_structure_refinement  'SHELXL-2016/4 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean 5.811
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Rigaku P200'
_diffrn_measurement_method       \w-scan
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0321
_diffrn_reflns_av_unetI/netI     0.0397
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            13264
_diffrn_reflns_point_group_measured_fraction_full 0.834
_diffrn_reflns_point_group_measured_fraction_max 0.834
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         67.729
_diffrn_reflns_theta_min         2.842
_diffrn_source                   'rotating anode'
_exptl_absorpt_coefficient_mu    1.464
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.75558
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   CryslisPro
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.238
_exptl_crystal_description       block
_exptl_crystal_F_000             984
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: N,N-dimethylformamide'
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.605
_refine_diff_density_min         -0.453
_refine_diff_density_rms         0.073
_refine_ls_abs_structure_details
;
 Flack x determined using 1546 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.38(2)
_refine_ls_extinction_coef       0.0017(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2016/4 (Sheldrick 2016)'
_refine_ls_goodness_of_fit_ref   0.858
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     760
_refine_ls_number_reflns         7422
_refine_ls_number_restraints     434
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.1108
_refine_ls_R_factor_gt           0.0993
_refine_ls_shift/su_max          0.064
_refine_ls_shift/su_mean         0.007
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1050P)^2^+8.2200P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2545
_refine_ls_wR_factor_ref         0.2599
_reflns_Friedel_coverage         0.589
_reflns_Friedel_fraction_full    0.652
_reflns_Friedel_fraction_max     0.652
_reflns_number_gt                5358
_reflns_number_total             7422
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0ra07396b2.cif
_cod_data_source_block           171108tbuasc
_cod_depositor_comments
'Adding full bibliography for 7241202--7241204.cif.'
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               7241202
_shelx_shelxl_version_number     2016/4
_shelx_res_checksum              36795