Thermal fluctuation-induced selective CO2 uptake of seemingly nonporous N,C-protected dipeptide crystals as elucidated by in situ X-ray crystallographic analysis
Yamanaka, Kazuaki; Oketani, Ryusei; Mori, Yuya; Sato, Takashi; Tsuzuki, Seiji; Takahashi, Hiroki; Tsue, Hirohito; CrystEngComm 26 (2024) 2314–2321; doi:10.1039/D3CE01018J

data_7248342
_publ_section_title
;
 Thermal fluctuation-induced selective CO2 uptake of seemingly nonporous
 N,C-protected dipeptide crystals as elucidated by in situ X-ray
 crystallographic analysis
;
_journal_issue                   17
_journal_name_full               CrystEngComm
_journal_page_first              2314
_journal_page_last               2321
_journal_paper_doi               10.1039/D3CE01018J
_journal_volume                  26
_journal_year                    2024
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C14 H26 N2 O5 S'
_chemical_formula_sum            'C14 H26 N2 O5 S'
_chemical_formula_weight         334.439
_chemical_melting_point          398.2
_space_group_crystal_system      hexagonal
_space_group_IT_number           170
_space_group_name_Hall           'P 65'
_space_group_name_H-M_alt        'P 65'
_symmetry_Int_Tables_number      170
_audit_creation_date             2024-03-15
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2024-03-22 deposited with the CCDC.	2024-03-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   11.2333(9)
_cell_length_b                   11.2333(9)
_cell_length_c                   27.046(2)
_cell_measurement_reflns_used    6686
_cell_measurement_temperature    238
_cell_measurement_theta_max      30.4080
_cell_measurement_theta_min      2.2000
_cell_volume                     2955.6(4)
_computing_cell_refinement       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.3 (Bourhis et al., 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      238
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.9989
_diffrn_measured_fraction_theta_max 0.9592
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w   -110.00  70.00   0.50    8.00    --  -20.00  44.00 330.00  360
  2  \w   -110.00  70.00   0.50    8.00    --  -20.00  44.00 240.00  360
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type
'dtrek-CrysAlisPro-abstract goniometer imported rigaku-d*trek images'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0705785000
_diffrn_orient_matrix_UB_12      0.0225903000
_diffrn_orient_matrix_UB_13      0.0039531000
_diffrn_orient_matrix_UB_21      0.0170225000
_diffrn_orient_matrix_UB_22      0.0678632000
_diffrn_orient_matrix_UB_23      -0.0064796000
_diffrn_orient_matrix_UB_31      -0.0066845000
_diffrn_orient_matrix_UB_32      0.0140204000
_diffrn_orient_matrix_UB_33      0.0251089000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0677
_diffrn_reflns_av_unetI/netI     0.0851
_diffrn_reflns_Laue_measured_fraction_full 0.9989
_diffrn_reflns_Laue_measured_fraction_max 0.9592
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            28134
_diffrn_reflns_point_group_measured_fraction_full 0.9975
_diffrn_reflns_point_group_measured_fraction_max 0.9324
_diffrn_reflns_theta_full        25.2417
_diffrn_reflns_theta_max         31.20
_diffrn_reflns_theta_min         2.58
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.185
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.84728
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.49 (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.127
_exptl_crystal_description       needle
_exptl_crystal_F_000             1081.303
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: hexane'
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.0931
_refine_diff_density_min         -0.4943
_refine_diff_density_rms         0.1047
_refine_ls_abs_structure_details
'Flack, H. D. (1983). Acta Cryst. A39, 876-881.'
_refine_ls_abs_structure_Flack   -0.10(13)
_refine_ls_d_res_high            0.6861
_refine_ls_d_res_low             7.8972
_refine_ls_goodness_of_fit_ref   0.9909
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    38
_refine_ls_number_parameters     205
_refine_ls_number_reflns         5962
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.9909
_refine_ls_R_factor_all          0.2013
_refine_ls_R_factor_gt           0.0815
_refine_ls_shift/su_max          0.0002
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1245P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1848
_refine_ls_wR_factor_ref         0.2460
_reflns_Friedel_coverage         0.905
_reflns_limit_h_max              13
_reflns_limit_h_min              -13
_reflns_limit_k_max              14
_reflns_limit_k_min              -14
_reflns_limit_l_max              39
_reflns_limit_l_min              -38
_reflns_number_gt                2642
_reflns_number_total             5962
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d3ce01018j4.cif
_cod_data_source_block           cmpd_1_238K
_cod_depositor_comments
'Adding full bibliography for 7248340--7248345.cif.'
_cod_original_sg_symbol_Hall     ' P 65'
_cod_database_code               7248342
_reflns_odcompleteness_completeness 99.90
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C2(H2), C5(H5)
2.b Secondary CH2 refined with riding coordinates:
 C6(H6a,H6b), C7(H7a,H7b)
2.c Aromatic/amide H refined with riding coordinates:
 N1(H1), N2(H2a)
2.d Idealised Me refined as rotating group:
 C3(H3a,H3b,H3c), C8(H8a,H8b,H8c), C9(H9a,H9b,H9c), C12(H12a,H12b,H12c),
 C13(H13a,H13b,H13c), C14(H14a,H14b,H14c)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.101
_oxdiff_exptl_absorpt_empirical_full_min 0.921