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_7246189
_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         'C38 H47 N8 O6 S2, C4 H9 N O7'
_chemical_formula_sum            'C42 H56 N9 O7 S2'
_chemical_formula_weight         863.08
_chemical_name_systematic
; 
 cyclo(Val-Oxz-D-Val-Thz-Phg-Oxz-D-Val-Thz).dimethylacetamide
;
_space_group_IT_number           5
_space_group_name_Hall           'C 2y'
_space_group_name_H-M_alt        'C 1 2 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 1 2 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2022-07-20 deposited with the CCDC.	2023-01-04 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 123.754(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   18.269(6)
_cell_length_b                   12.967(4)
_cell_length_c                   11.641(4)
_cell_measurement_reflns_used    3354
_cell_measurement_temperature    240(2)
_cell_measurement_theta_max      27.82
_cell_measurement_theta_min      2.31
_cell_volume                     2292.8(13)
_computing_cell_refinement       'SAINT-PLUS (Bruker, 1998)'
_computing_data_collection       'SMART (Bruker, 1998)'
_computing_data_reduction        'SAINT-PLUS (Bruker, 1998)'
_computing_molecular_graphics    'PLATON (Spek, 2009)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      240(2)
_diffrn_detector_area_resol_mean 8.366
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0362
_diffrn_reflns_av_sigmaI/netI    0.0994
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            7239
_diffrn_reflns_theta_full        25.02
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         2.10
_diffrn_standards_decay_%        0.15
_diffrn_standards_interval_count 7239
_diffrn_standards_interval_time  840
_diffrn_standards_number         101
_exptl_absorpt_coefficient_mu    0.173
_exptl_absorpt_correction_T_max  1.352
_exptl_absorpt_correction_T_min  0.837
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.250
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             918
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: N,N-Dimethylacetamide'
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.660
_refine_diff_density_min         -0.691
_refine_diff_density_rms         0.088
_refine_ls_abs_structure_details 'Flack (1983), 1787 Friedel pairs'
_refine_ls_abs_structure_Flack   -0.3(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.141
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     330
_refine_ls_number_reflns         3907
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.141
_refine_ls_R_factor_all          0.1249
_refine_ls_R_factor_gt           0.1071
_refine_ls_shift/su_max          0.017
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0873P)^2^+6.8483P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2655
_refine_ls_wR_factor_ref         0.2780
_reflns_number_gt                3055
_reflns_number_total             3907
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            d2ra07063d2.cif
_cod_data_source_block           valphg
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_symmetry_cell_setting' value 'Monoclinic' was changed to
'monoclinic' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 
;
_cod_original_cell_volume        2292.9(13)
_cod_original_sg_symbol_H-M      'C2   '
_cod_database_code               7246189