Experimental evidence for CH⋯π interaction-mediated stabilization of the square form in phenylglycine-incorporated ascidiacyclamide
Asano, Akiko; Minoura, Katsuhiko; Yamada, Takeshi; Doi, Mitsunobu; RSC Advances 13 (2023) 2458–2466; doi:10.1039/D2RA07063D

data_7246188
_publ_section_title
;
 Experimental evidence for CH&#x22EF;\p interaction-mediated stabilization
 of the square form in phenylglycine-incorporated ascidiacyclamide
;
_journal_issue                   4
_journal_name_full               'RSC Advances'
_journal_page_first              2458
_journal_page_last               2466
_journal_paper_doi               10.1039/D2RA07063D
_journal_volume                  13
_journal_year                    2023
_chemical_absolute_configuration rm
_chemical_compound_source        synthesis
_chemical_formula_moiety         'C37 H52 N8 O6 S2, C4 H9 N O'
_chemical_formula_sum            'C41 H61 N9 O7 S2'
_chemical_formula_weight         856.11
_chemical_name_common            '[Val,Chg]ASC'
_chemical_name_systematic
; 
 c(Val-Oxz-dval-Thz-Chg-Oxz-dval-Thz)2.DMA 
;
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2022-07-19 deposited with the CCDC.	2023-01-04 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 97.85(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.012(2)
_cell_length_b                   12.909(3)
_cell_length_c                   14.885(3)
_cell_measurement_reflns_used    27513
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      74.9040
_cell_measurement_theta_min      3.0150
_cell_volume                     2286.5(8)
_computing_cell_refinement       CrysAlisPro
_computing_data_collection       CrysAlisPro
_computing_data_reduction        CrysAlisPro
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'XtaLAB Pro: Kappa single P200'
_diffrn_measurement_method       \w-scan
_diffrn_radiation_monochromator  conforcal
_diffrn_radiation_source         'rotated anode'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0818
_diffrn_reflns_av_sigmaI/netI    0.0366
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            39675
_diffrn_reflns_theta_full        70.07
_diffrn_reflns_theta_max         70.07
_diffrn_reflns_theta_min         3.00
_diffrn_standards_interval_count 39675
_diffrn_standards_interval_time  210
_exptl_absorpt_coefficient_mu    1.518
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.70036
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   CrysAlisPro
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.243
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             916
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: N,N-Dimethylacetamide'
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.959
_refine_diff_density_min         -0.334
_refine_diff_density_rms         0.075
_refine_ls_abs_structure_details 'Flack (1983), 4025 Friedel pairs'
_refine_ls_abs_structure_Flack   0.005(18)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.744
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     532
_refine_ls_number_reflns         8579
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.744
_refine_ls_R_factor_all          0.0657
_refine_ls_R_factor_gt           0.0644
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1676P)^2^+2.4145P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1733
_refine_ls_wR_factor_ref         0.1754
_reflns_number_gt                8214
_reflns_number_total             8579
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            d2ra07063d2.cif
_cod_data_source_block           valchg
_cod_original_sg_symbol_H-M      P21
_cod_database_code               7246188